data_5 _audit_creation_date 2022-08-21 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common 5 _chemical_name_systematic ? _chemical_formula_moiety 'C32 H72 Cl Si8 U, C24 H48 Cl3 Mg2 O6' _chemical_formula_sum 'C56 H120 Cl4 Mg2 O6 Si8 U' _chemical_formula_weight 1542.68 _chemical_melting_point ? _chemical_oxdiff_formula 'C56 H120 Si8 O6 Mg2 Cl4 U' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3309(2) _cell_length_b 17.7676(2) _cell_length_c 33.4350(5) _cell_angle_alpha 90 _cell_angle_beta 90.6810(10) _cell_angle_gamma 90 _cell_volume 7918.79(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 19082 _cell_measurement_temperature 99.9(2) _cell_measurement_theta_max 71.4790 _cell_measurement_theta_min 4.2580 _shelx_estimated_absorpt_T_max 0.658 _shelx_estimated_absorpt_T_min 0.307 _exptl_absorpt_coefficient_mu 8.631 _exptl_absorpt_correction_T_max 0.661 _exptl_absorpt_correction_T_min 0.357 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'dark bronze' _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 3200 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 -10 -10 0.0597 5 1 17 0.0673 -7 -1 13 0.0279 1 11 7 0.0610 -5 3 -17 0.0659 7 1 -14 0.0230 3 -10 7 0.0927 _exptl_crystal_size_max 0.179 _exptl_crystal_size_mid 0.129 _exptl_crystal_size_min 0.053 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.9769 -10.0028 -9.9851 -0.0117 -0.3606 -0.9450 4.9876 1.0125 17.0257 -0.0092 -0.5448 0.8185 -7.0117 -0.9971 13.0003 -1.0040 0.0459 0.0087 0.9771 11.0000 6.9768 0.0155 0.5418 0.8585 -4.9941 2.9858 -17.0375 0.0526 0.8128 -0.6022 7.0124 0.9965 -14.0014 1.0317 -0.0257 -0.0395 3.0123 -9.9898 7.0435 -0.0318 -0.9724 -0.1806 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 21288 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.062 _diffrn_reflns_theta_min 3.315 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.9(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1033 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -32.00 -7.00 1.00 15.00 -- -30.00 69.00 -33.00 25 2 \w -77.00 -52.00 1.00 15.00 -- -30.00 -69.00-165.00 25 3 \w -29.00 36.00 1.00 15.00 -- 37.29 -69.00-165.00 65 4 \w 26.00 104.00 1.00 15.00 -- 37.29 69.00 -33.00 78 5 \w 87.00 121.00 1.00 75.00 -- 107.00 -69.00-165.00 34 6 \w 86.00 171.00 1.00 75.00 -- 107.00 69.00 -33.00 85 7 \w -96.00 -53.00 1.00 15.00 -- -30.00 -57.00 0.00 43 8 \w 25.00 104.00 1.00 15.00 -- 37.29 38.00 -60.00 79 9 \w 18.00 93.00 1.00 15.00 -- 37.29 38.00 90.00 75 10 \w 50.00 101.00 1.00 75.00 -- 107.00 -30.00 0.00 51 11 \w 82.00 109.00 1.00 75.00 -- 107.00 -45.00-150.00 27 12 \w 44.00 74.00 1.00 75.00 -- 107.00-111.00-150.00 30 13 \w 50.00 80.00 1.00 75.00 -- 107.00 -45.00-150.00 30 14 \w 90.00 164.00 1.00 75.00 -- 107.00 61.00-120.00 74 15 \w 89.00 173.00 1.00 75.00 -- 107.00 61.00 -60.00 84 16 \w 43.00 70.00 1.00 75.00 -- 107.00-111.00 90.00 27 17 \w 90.00 159.00 1.00 75.00 -- 107.00 45.00 60.00 69 18 \w 104.00 162.00 1.00 75.00 -- 107.00 45.00 30.00 58 19 \w 102.00 167.00 1.00 75.00 -- 107.00 61.00 -90.00 65 20 \w 40.00 95.00 1.00 75.00 -- 107.00 -61.00-180.00 55 21 \w 128.00 153.00 1.00 75.00 -- 107.00 111.00-120.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0903518000 _diffrn_orient_matrix_UB_12 0.0109246000 _diffrn_orient_matrix_UB_13 -0.0276571000 _diffrn_orient_matrix_UB_21 -0.0536337000 _diffrn_orient_matrix_UB_22 0.0668753000 _diffrn_orient_matrix_UB_23 -0.0202635000 _diffrn_orient_matrix_UB_31 0.0480809000 _diffrn_orient_matrix_UB_32 0.0542616000 _diffrn_orient_matrix_UB_33 0.0307629000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 15631 _reflns_number_total 21288 _reflns_special_details ; Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 4.428 _refine_diff_density_min -4.477 _refine_diff_density_rms 0.249 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 738 _refine_ls_number_reflns 21288 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0828 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1865P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2325 _refine_ls_wR_factor_ref 0.2452 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.906(3) 0.094(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C35-C36 \\sim C35-C36A with sigma of 0.02 O4-C36 \\sim O4-C36A with sigma of 0.02 O6-C43 \\sim O6A-C43A with sigma of 0.04 Mg2-O6 \\sim Mg2-O6A with sigma of 0.02 O6-C41 \\sim O6A-C41 with sigma of 0.02 O6-C44 \\sim O6A-C44A with sigma of 0.02 C44-C41 \\sim C44A-C41 with sigma of 0.04 C42-C44 \\sim C42-C44A with sigma of 0.04 C43-C44 \\sim C43A-C44A with sigma of 0.02 C42-C43 \\sim C42-C43A with sigma of 0.02 Mg2-C44 \\sim Mg2-C44A with sigma of 0.04 4. Uiso/Uaniso restraints and constraints Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(O6) = Uanis(O6A) Uanis(C43) = Uanis(C43A) Uanis(C44) = Uanis(C44A) 5. Others Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(1) Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1) Sof(H42C)=Sof(H42D)=Sof(H41C)=Sof(H41D)=Sof(O6A)=Sof(C44A)=Sof(H44C)= Sof(H44D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(2) Sof(O6)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)= Sof(H44B)=Sof(H41A)=Sof(H41B)=FVAR(2) 6.a Ternary CH refined with riding coordinates: C2(H2) 6.b Secondary CH2 refined with riding coordinates: C45(H45A,H45B), C54(H54A,H54B), C52(H52A,H52B), C34(H34A,H34B), C53(H53A, H53B), C35(H35A,H35B), C35(H35C,H35D), C48(H48A,H48B), C50(H50A,H50B), C46(H46A,H46B), C56(H56A,H56B), C49(H49A,H49B), C55(H55A,H55B), C42(H42A,H42B), C42(H42C,H42D), C40(H40A,H40B), C47(H47A,H47B), C51(H51A,H51B), C38(H38A, H38B), C37(H37A,H37B), C43(H43A,H43B), C39(H39A,H39B), C44(H44A,H44B), C41(H41A,H41B), C41(H41C,H41D), C36(H36A,H36B), C36A(H36C,H36D), C33(H33A, H33B), C1(H1A,H1B), C44A(H44C,H44D), C43A(H43C,H43D) 6.c Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C21(H21A,H21B, H21C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C13(H13A,H13B,H13C), C23(H23A, H23B,H23C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C14(H14A,H14B, H14C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A, H18B,H18C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.46829(2) 0.78402(2) 0.36898(2) 0.01938(13) Uani 1 1 d . . . . . Cl3 Cl 0.92192(18) 0.83563(14) 0.10465(8) 0.0300(5) Uani 1 1 d . . . . . Cl4 Cl 1.07325(19) 0.68627(15) 0.11847(9) 0.0353(6) Uani 1 1 d . . . . . Cl2 Cl 0.9226(2) 0.73947(14) 0.19317(8) 0.0326(6) Uani 1 1 d . . . . . Cl1 Cl 0.3499(2) 0.89490(15) 0.34394(9) 0.0384(6) Uani 1 1 d . . . . . Si5 Si 0.5680(2) 0.66362(14) 0.46619(8) 0.0241(5) Uani 1 1 d . . . . . Si4 Si 0.5643(2) 0.90444(16) 0.26989(9) 0.0282(6) Uani 1 1 d . . . . . Si7 Si 0.1933(2) 0.77313(16) 0.41216(9) 0.0265(6) Uani 1 1 d . . . . . Si6 Si 0.4083(2) 0.85064(15) 0.48194(8) 0.0252(5) Uani 1 1 d . . . . . Si3 Si 0.6591(3) 0.96196(16) 0.38114(9) 0.0319(6) Uani 1 1 d . . . . . Si8 Si 0.3429(2) 0.58027(15) 0.40021(10) 0.0299(6) Uani 1 1 d . . . . . Si2 Si 0.8110(2) 0.78031(19) 0.36019(11) 0.0359(7) Uani 1 1 d . . . . . Mg1 Mg 0.8874(3) 0.70097(19) 0.12217(11) 0.0251(7) Uani 1 1 d . . . . . Si1 Si 0.5729(3) 0.68568(17) 0.29598(10) 0.0381(7) Uani 1 1 d . . . . . Mg2 Mg 1.0553(3) 0.8089(2) 0.15555(12) 0.0317(8) Uani 1 1 d D . . . . O3 O 0.7368(5) 0.7251(4) 0.1253(2) 0.0274(16) Uani 1 1 d . . . . . O1 O 0.8589(6) 0.5919(4) 0.1423(3) 0.0344(18) Uani 1 1 d . . . . . O2 O 0.8710(6) 0.6654(4) 0.0632(2) 0.0297(16) Uani 1 1 d . . . . . O4 O 1.0252(6) 0.9097(4) 0.1858(3) 0.0333(17) Uani 1 1 d D . . . . O5 O 1.1648(7) 0.7837(5) 0.1990(3) 0.047(2) Uani 1 1 d . . . . . C5 C 0.6239(7) 0.7725(6) 0.3212(4) 0.025(2) Uani 1 1 d . . . . . C3 C 0.6244(8) 0.8714(6) 0.3569(3) 0.027(2) Uani 1 1 d . . . . . C4 C 0.5990(8) 0.8505(6) 0.3163(3) 0.024(2) Uani 1 1 d . . . . . C9 C 0.3839(8) 0.6778(5) 0.4121(3) 0.023(2) Uani 1 1 d . . . . . O6 O 1.1683(8) 0.8576(6) 0.1203(3) 0.047(3) Uani 0.93(2) 1 d D U P A 1 C45 C 0.9323(9) 0.6938(7) 0.0304(3) 0.034(2) Uani 1 1 d . . . . . H45A H 0.982246 0.730721 0.040379 0.040 Uiso 1 1 calc R U . . . H45B H 0.889637 0.718397 0.009732 0.040 Uiso 1 1 calc R U . . . C8 C 0.4700(8) 0.7089(5) 0.4346(3) 0.023(2) Uani 1 1 d . . . . . C30 C 0.1481(9) 0.7599(7) 0.3592(3) 0.034(2) Uani 1 1 d . . . . . H30A H 0.180325 0.797022 0.341878 0.051 Uiso 1 1 calc R U . . . H30B H 0.075142 0.766608 0.357849 0.051 Uiso 1 1 calc R U . . . H30C H 0.165183 0.709047 0.350109 0.051 Uiso 1 1 calc R U . . . C54 C 0.5600(9) 0.7201(6) 0.1199(4) 0.033(3) Uani 1 1 d . . . . . H54A H 0.541551 0.687826 0.142821 0.039 Uiso 1 1 calc R U . . . H54B H 0.503646 0.721645 0.100377 0.039 Uiso 1 1 calc R U . . . C52 C 0.7803(9) 0.5766(7) 0.1711(4) 0.036(3) Uani 1 1 d . . . . . H52A H 0.722340 0.551641 0.157887 0.044 Uiso 1 1 calc R U . . . H52B H 0.757015 0.623816 0.183645 0.044 Uiso 1 1 calc R U . . . C6 C 0.3261(8) 0.7465(6) 0.4189(3) 0.025(2) Uani 1 1 d . . . . . C7 C 0.4106(7) 0.7793(5) 0.4416(3) 0.0205(19) Uani 1 1 d . . . . . C34 C 0.9342(10) 1.0022(6) 0.2211(4) 0.037(3) Uani 1 1 d . . . . . H34A H 0.959532 0.999905 0.249046 0.045 Uiso 1 1 calc R U . . . H34B H 0.868330 1.027872 0.220589 0.045 Uiso 1 1 calc R U . . . C22 C 0.5267(9) 0.8543(6) 0.5132(4) 0.037(3) Uani 1 1 d . . . . . H22A H 0.541288 0.804104 0.523907 0.056 Uiso 1 1 calc R U . . . H22B H 0.517840 0.889745 0.535301 0.056 Uiso 1 1 calc R U . . . H22C H 0.582543 0.870933 0.496549 0.056 Uiso 1 1 calc R U . . . C53 C 0.6560(8) 0.6942(6) 0.1008(4) 0.031(2) Uani 1 1 d . . . . . H53A H 0.659519 0.638513 0.100393 0.037 Uiso 1 1 calc R U . . . H53B H 0.660221 0.713009 0.073028 0.037 Uiso 1 1 calc R U . . . C27 C 0.3145(10) 0.5309(6) 0.4483(4) 0.044(3) Uani 1 1 d . . . . . H27A H 0.377258 0.520131 0.462717 0.067 Uiso 1 1 calc R U . . . H27B H 0.279209 0.483700 0.442552 0.067 Uiso 1 1 calc R U . . . H27C H 0.272034 0.563221 0.464812 0.067 Uiso 1 1 calc R U . . . C35 C 1.0089(9) 1.0418(6) 0.1940(4) 0.042(3) Uani 1 1 d D . . . . H35A H 1.071823 1.054754 0.208456 0.050 Uiso 0.30(4) 1 calc R U P B 1 H35B H 0.979899 1.087737 0.181729 0.050 Uiso 0.30(4) 1 calc R U P B 1 H35C H 1.042949 1.083904 0.208048 0.050 Uiso 0.70(4) 1 calc R U P B 2 H35D H 0.975854 1.061014 0.169389 0.050 Uiso 0.70(4) 1 calc R U P B 2 C21 C 0.3852(10) 0.9483(6) 0.4629(4) 0.038(3) Uani 1 1 d . . . . . H21A H 0.449397 0.972482 0.457101 0.057 Uiso 1 1 calc R U . . . H21B H 0.349816 0.977440 0.483234 0.057 Uiso 1 1 calc R U . . . H21C H 0.344122 0.945940 0.438423 0.057 Uiso 1 1 calc R U . . . C31 C 0.1679(8) 0.8744(6) 0.4244(4) 0.031(2) Uani 1 1 d . . . . . H31A H 0.206927 0.906801 0.406724 0.047 Uiso 1 1 calc R U . . . H31B H 0.187386 0.884235 0.452309 0.047 Uiso 1 1 calc R U . . . H31C H 0.096290 0.884938 0.420704 0.047 Uiso 1 1 calc R U . . . C32 C 0.1156(9) 0.7151(7) 0.4471(4) 0.038(3) Uani 1 1 d . . . . . H32A H 0.044465 0.726825 0.442912 0.058 Uiso 1 1 calc R U . . . H32B H 0.134902 0.726591 0.474819 0.058 Uiso 1 1 calc R U . . . H32C H 0.127059 0.661516 0.441839 0.058 Uiso 1 1 calc R U . . . C13 C 0.6757(9) 0.9022(6) 0.2363(3) 0.032(2) Uani 1 1 d . . . . . H13A H 0.731663 0.929121 0.249138 0.048 Uiso 1 1 calc R U . . . H13B H 0.658587 0.926469 0.210842 0.048 Uiso 1 1 calc R U . . . H13C H 0.695238 0.849843 0.231494 0.048 Uiso 1 1 calc R U . . . C23 C 0.3095(10) 0.8268(7) 0.5193(3) 0.039(3) Uani 1 1 d . . . . . H23A H 0.245215 0.819094 0.505350 0.059 Uiso 1 1 calc R U . . . H23B H 0.303176 0.868129 0.538457 0.059 Uiso 1 1 calc R U . . . H23C H 0.328509 0.780608 0.533492 0.059 Uiso 1 1 calc R U . . . C48 C 0.8282(9) 0.5957(7) 0.0477(4) 0.039(3) Uani 1 1 d . . . . . H48A H 0.768813 0.606081 0.030548 0.047 Uiso 1 1 calc R U . . . H48B H 0.807959 0.562164 0.069880 0.047 Uiso 1 1 calc R U . . . C50 C 0.8989(11) 0.4784(7) 0.1773(4) 0.049(3) Uani 1 1 d . . . . . H50A H 0.862737 0.438118 0.162626 0.059 Uiso 1 1 calc R U . . . H50B H 0.952560 0.455567 0.194068 0.059 Uiso 1 1 calc R U . . . C46 C 0.9832(11) 0.6260(7) 0.0136(4) 0.044(3) Uani 1 1 d . . . . . H46A H 1.049935 0.618535 0.026297 0.053 Uiso 1 1 calc R U . . . H46B H 0.991598 0.630910 -0.015675 0.053 Uiso 1 1 calc R U . . . C25 C 0.5186(9) 0.6409(7) 0.5175(3) 0.033(2) Uani 1 1 d . . . . . H25A H 0.489680 0.686344 0.529349 0.050 Uiso 1 1 calc R U . . . H25B H 0.573667 0.622639 0.534617 0.050 Uiso 1 1 calc R U . . . H25C H 0.466828 0.601927 0.515256 0.050 Uiso 1 1 calc R U . . . C28 C 0.2249(11) 0.5753(7) 0.3695(5) 0.048(3) Uani 1 1 d . . . . . H28A H 0.171174 0.602182 0.383282 0.073 Uiso 1 1 calc R U . . . H28B H 0.205536 0.522547 0.365769 0.073 Uiso 1 1 calc R U . . . H28C H 0.236096 0.598624 0.343372 0.073 Uiso 1 1 calc R U . . . C56 C 0.6967(9) 0.7882(6) 0.1482(4) 0.037(3) Uani 1 1 d . . . . . H56A H 0.736952 0.834175 0.143666 0.045 Uiso 1 1 calc R U . . . H56B H 0.697909 0.776559 0.177174 0.045 Uiso 1 1 calc R U . . . C24 C 0.6852(9) 0.7216(6) 0.4731(4) 0.035(3) Uani 1 1 d . . . . . H24A H 0.731367 0.711388 0.451214 0.053 Uiso 1 1 calc R U . . . H24B H 0.717557 0.708528 0.498671 0.053 Uiso 1 1 calc R U . . . H24C H 0.667585 0.775192 0.473155 0.053 Uiso 1 1 calc R U . . . C49 C 0.9409(10) 0.5366(7) 0.1489(5) 0.048(3) Uani 1 1 d . . . . . H49A H 1.000627 0.561458 0.160877 0.058 Uiso 1 1 calc R U . . . H49B H 0.960312 0.512915 0.123356 0.058 Uiso 1 1 calc R U . . . C2 C 0.6681(8) 0.7901(5) 0.3633(3) 0.025(2) Uani 1 1 d . . . . . H2 H 0.636907 0.761281 0.385618 0.030 Uiso 1 1 calc R U . . . C55 C 0.5908(10) 0.7993(6) 0.1336(4) 0.036(3) Uani 1 1 d . . . . . H55A H 0.587910 0.835453 0.111053 0.043 Uiso 1 1 calc R U . . . H55B H 0.547242 0.817546 0.155291 0.043 Uiso 1 1 calc R U . . . C11 C 0.6352(12) 0.5989(7) 0.3154(4) 0.048(3) Uani 1 1 d . . . . . H11A H 0.644538 0.603111 0.344448 0.071 Uiso 1 1 calc R U . . . H11B H 0.700562 0.592949 0.302727 0.071 Uiso 1 1 calc R U . . . H11C H 0.593104 0.555060 0.309298 0.071 Uiso 1 1 calc R U . . . C10 C 0.6008(14) 0.6885(7) 0.2419(4) 0.056(4) Uani 1 1 d . . . . . H10A H 0.566059 0.731362 0.229518 0.085 Uiso 1 1 calc R U . . . H10B H 0.577790 0.641725 0.229220 0.085 Uiso 1 1 calc R U . . . H10C H 0.673266 0.693892 0.238249 0.085 Uiso 1 1 calc R U . . . C42 C 1.2594(11) 0.8816(9) 0.0613(5) 0.056(4) Uani 1 1 d D . . . . H42A H 1.250452 0.935600 0.054774 0.067 Uiso 0.93(2) 1 calc R U P A 1 H42B H 1.283064 0.854464 0.037348 0.067 Uiso 0.93(2) 1 calc R U P A 1 H42C H 1.245121 0.920939 0.041018 0.067 Uiso 0.07(2) 1 calc R U P A 2 H42D H 1.304292 0.843073 0.049854 0.067 Uiso 0.07(2) 1 calc R U P A 2 C40 C 1.2399(12) 0.7271(9) 0.1944(6) 0.065(5) Uani 1 1 d . . . . . H40A H 1.306902 0.747096 0.201746 0.078 Uiso 1 1 calc R U . . . H40B H 1.241485 0.709237 0.166333 0.078 Uiso 1 1 calc R U . . . C20 C 0.5544(12) 1.0319(6) 0.3807(4) 0.047(3) Uani 1 1 d . . . . . H20A H 0.559029 1.063496 0.356709 0.070 Uiso 1 1 calc R U . . . H20B H 0.559240 1.063650 0.404574 0.070 Uiso 1 1 calc R U . . . H20C H 0.489984 1.005324 0.380415 0.070 Uiso 1 1 calc R U . . . C47 C 0.9119(11) 0.5602(8) 0.0236(4) 0.048(3) Uani 1 1 d . . . . . H47A H 0.884820 0.536940 -0.001162 0.058 Uiso 1 1 calc R U . . . H47B H 0.947391 0.521227 0.039477 0.058 Uiso 1 1 calc R U . . . C14 C 0.5353(11) 1.0053(7) 0.2792(4) 0.043(3) Uani 1 1 d . . . . . H14A H 0.476331 1.009075 0.296300 0.064 Uiso 1 1 calc R U . . . H14B H 0.521436 1.030558 0.253650 0.064 Uiso 1 1 calc R U . . . H14C H 0.592787 1.029358 0.292477 0.064 Uiso 1 1 calc R U . . . C26 C 0.6140(10) 0.5705(6) 0.4459(4) 0.038(3) Uani 1 1 d . . . . . H26A H 0.557576 0.535230 0.443747 0.057 Uiso 1 1 calc R U . . . H26B H 0.665253 0.549704 0.463978 0.057 Uiso 1 1 calc R U . . . H26C H 0.642801 0.578223 0.419362 0.057 Uiso 1 1 calc R U . . . C51 C 0.8279(12) 0.5248(8) 0.2023(4) 0.050(3) Uani 1 1 d . . . . . H51A H 0.864602 0.553859 0.223065 0.060 Uiso 1 1 calc R U . . . H51B H 0.776953 0.492746 0.215228 0.060 Uiso 1 1 calc R U . . . C15 C 0.8460(11) 0.6784(8) 0.3648(5) 0.056(4) Uani 1 1 d . . . . . H15A H 0.806530 0.655050 0.385957 0.083 Uiso 1 1 calc R U . . . H15B H 0.917570 0.674212 0.371401 0.083 Uiso 1 1 calc R U . . . H15C H 0.832165 0.652838 0.339333 0.083 Uiso 1 1 calc R U . . . C17 C 0.8768(9) 0.8287(9) 0.4026(4) 0.047(3) Uani 1 1 d . . . . . H17A H 0.868087 0.883254 0.400051 0.071 Uiso 1 1 calc R U . . . H17B H 0.948486 0.816440 0.402130 0.071 Uiso 1 1 calc R U . . . H17C H 0.848461 0.811776 0.428010 0.071 Uiso 1 1 calc R U . . . C18 C 0.7685(11) 1.0072(7) 0.3569(4) 0.049(3) Uani 1 1 d . . . . . H18A H 0.828536 0.976344 0.361395 0.074 Uiso 1 1 calc R U . . . H18B H 0.779256 1.057360 0.368334 0.074 Uiso 1 1 calc R U . . . H18C H 0.755492 1.011749 0.328050 0.074 Uiso 1 1 calc R U . . . C12 C 0.4507(10) 0.8664(7) 0.2431(4) 0.043(3) Uani 1 1 d . . . . . H12A H 0.456138 0.811591 0.241009 0.064 Uiso 1 1 calc R U . . . H12B H 0.446284 0.888425 0.216296 0.064 Uiso 1 1 calc R U . . . H12C H 0.390449 0.879466 0.258136 0.064 Uiso 1 1 calc R U . . . C38 C 1.1560(18) 0.7027(10) 0.2548(6) 0.078(6) Uani 1 1 d . . . . . H38A H 1.194828 0.700191 0.280201 0.093 Uiso 1 1 calc R U . . . H38B H 1.089454 0.679430 0.258852 0.093 Uiso 1 1 calc R U . . . C37 C 1.1453(13) 0.7830(8) 0.2408(5) 0.057(4) Uani 1 1 d . . . . . H37A H 1.076620 0.801635 0.245902 0.068 Uiso 1 1 calc R U . . . H37B H 1.193673 0.815829 0.255203 0.068 Uiso 1 1 calc R U . . . C16 C 0.8589(11) 0.8206(10) 0.3121(4) 0.054(4) Uani 1 1 d . . . . . H16A H 0.831887 0.791536 0.289529 0.081 Uiso 1 1 calc R U . . . H16B H 0.932340 0.818076 0.312099 0.081 Uiso 1 1 calc R U . . . H16C H 0.837487 0.873163 0.309665 0.081 Uiso 1 1 calc R U . . . C43 C 1.3282(13) 0.8708(11) 0.0960(6) 0.061(5) Uani 0.93(2) 1 d D U P A 1 H43A H 1.386466 0.905261 0.094565 0.073 Uiso 0.93(2) 1 calc R U P A 1 H43B H 1.352805 0.818289 0.097391 0.073 Uiso 0.93(2) 1 calc R U P A 1 C19 C 0.6919(11) 0.9469(7) 0.4356(4) 0.045(3) Uani 1 1 d . . . . . H19A H 0.632189 0.955006 0.451856 0.068 Uiso 1 1 calc R U . . . H19B H 0.744400 0.982608 0.443759 0.068 Uiso 1 1 calc R U . . . H19C H 0.716305 0.895381 0.439512 0.068 Uiso 1 1 calc R U . . . C39 C 1.2106(17) 0.6643(10) 0.2220(6) 0.078(6) Uani 1 1 d . . . . . H39A H 1.166659 0.627522 0.208109 0.093 Uiso 1 1 calc R U . . . H39B H 1.270675 0.637779 0.232545 0.093 Uiso 1 1 calc R U . . . C29 C 0.4356(11) 0.5201(6) 0.3720(4) 0.042(3) Uani 1 1 d . . . . . H29A H 0.435593 0.535173 0.343768 0.063 Uiso 1 1 calc R U . . . H29B H 0.416182 0.467072 0.374030 0.063 Uiso 1 1 calc R U . . . H29C H 0.502881 0.527005 0.383488 0.063 Uiso 1 1 calc R U . . . C44 C 1.2629(13) 0.8895(11) 0.1320(6) 0.068(5) Uani 0.93(2) 1 d D U P A 1 H44A H 1.289311 0.865740 0.156799 0.081 Uiso 0.93(2) 1 calc R U P A 1 H44B H 1.257632 0.944514 0.136159 0.081 Uiso 0.93(2) 1 calc R U P A 1 C41 C 1.1673(12) 0.8485(11) 0.0769(5) 0.065(4) Uani 1 1 d D . . . . H41A H 1.107995 0.874052 0.065081 0.078 Uiso 0.93(2) 1 calc R U P A 1 H41B H 1.163881 0.794436 0.069884 0.078 Uiso 0.93(2) 1 calc R U P A 1 H41C H 1.110817 0.860837 0.058565 0.078 Uiso 0.07(2) 1 calc R U P A 2 H41D H 1.174559 0.793072 0.077485 0.078 Uiso 0.07(2) 1 calc R U P A 2 C36 C 1.025(4) 0.9795(14) 0.1631(9) 0.049(14) Uani 0.30(4) 1 d D U P B 1 H36A H 0.969899 0.979409 0.142955 0.059 Uiso 0.30(4) 1 calc R U P B 1 H36B H 1.089417 0.986418 0.149319 0.059 Uiso 0.30(4) 1 calc R U P B 1 C36A C 1.0819(13) 0.9780(9) 0.1848(6) 0.041(5) Uani 0.70(4) 1 d D U P B 2 H36C H 1.111656 0.985169 0.158128 0.049 Uiso 0.70(4) 1 calc R U P B 2 H36D H 1.136667 0.976502 0.205069 0.049 Uiso 0.70(4) 1 calc R U P B 2 C33 C 0.9272(14) 0.9250(8) 0.2030(6) 0.066(5) Uani 1 1 d . . . . . H33A H 0.911127 0.887246 0.223723 0.079 Uiso 1 1 calc R U . . . H33B H 0.874178 0.923608 0.182016 0.079 Uiso 1 1 calc R U . . . C1 C 0.4361(11) 0.6946(7) 0.3126(4) 0.041(3) Uani 1 1 d . U . . . H1A H 0.408118 0.646062 0.321795 0.049 Uiso 1 1 calc R U . . . H1B H 0.392277 0.716492 0.291524 0.049 Uiso 1 1 calc R U . . . O6A O 1.144(9) 0.875(5) 0.1170(17) 0.047(3) Uani 0.07(2) 1 d D . P A 2 C44A C 1.211(11) 0.937(6) 0.124(3) 0.068(5) Uani 0.07(2) 1 d D . P A 2 H44C H 1.229379 0.940495 0.153004 0.081 Uiso 0.07(2) 1 calc R U P A 2 H44D H 1.181746 0.984947 0.115180 0.081 Uiso 0.07(2) 1 calc R U P A 2 C43A C 1.301(8) 0.914(11) 0.099(2) 0.061(5) Uani 0.07(2) 1 d D . P A 2 H43C H 1.343251 0.958768 0.093232 0.073 Uiso 0.07(2) 1 calc R U P A 2 H43D H 1.343058 0.876553 0.113386 0.073 Uiso 0.07(2) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01790(19) 0.02185(18) 0.0184(2) 0.00007(11) 0.00031(12) 0.00195(11) Cl3 0.0260(11) 0.0333(11) 0.0306(13) 0.0020(10) 0.0007(10) -0.0037(10) Cl4 0.0244(12) 0.0360(12) 0.0453(16) -0.0089(11) -0.0054(11) -0.0001(10) Cl2 0.0378(14) 0.0321(11) 0.0276(13) -0.0031(10) -0.0053(11) -0.0106(11) Cl1 0.0314(13) 0.0388(13) 0.0452(16) 0.0131(12) 0.0066(12) 0.0098(11) Si5 0.0247(13) 0.0237(12) 0.0238(14) 0.0025(10) -0.0017(11) 0.0054(10) Si4 0.0307(14) 0.0309(13) 0.0230(14) 0.0040(11) -0.0001(11) -0.0018(12) Si7 0.0202(13) 0.0303(13) 0.0291(15) 0.0014(11) 0.0022(11) -0.0002(11) Si6 0.0304(14) 0.0237(11) 0.0215(13) -0.0020(10) 0.0005(11) 0.0020(11) Si3 0.0408(17) 0.0251(12) 0.0298(16) -0.0037(11) -0.0023(13) -0.0071(12) Si8 0.0333(15) 0.0200(12) 0.0363(16) 0.0021(11) -0.0040(13) -0.0056(11) Si2 0.0241(15) 0.0458(17) 0.0378(18) 0.0031(14) -0.0010(13) 0.0029(13) Mg1 0.0191(16) 0.0292(15) 0.0271(18) -0.0068(14) 0.0010(13) -0.0051(13) Si1 0.050(2) 0.0306(14) 0.0341(18) -0.0075(13) 0.0063(15) -0.0062(14) Mg2 0.0233(17) 0.0327(17) 0.039(2) -0.0065(16) -0.0038(16) -0.0063(15) O3 0.019(3) 0.033(4) 0.030(4) -0.017(3) 0.000(3) -0.004(3) O1 0.031(4) 0.030(4) 0.043(5) -0.007(3) 0.004(3) -0.002(3) O2 0.028(4) 0.036(4) 0.025(4) -0.010(3) 0.004(3) -0.006(3) O4 0.027(4) 0.030(4) 0.043(5) -0.002(3) 0.003(3) -0.006(3) O5 0.034(5) 0.049(5) 0.058(6) -0.017(4) -0.017(4) 0.004(4) C5 0.006(4) 0.028(5) 0.041(6) -0.007(4) 0.008(4) -0.003(4) C3 0.029(5) 0.025(5) 0.025(5) 0.000(4) -0.001(4) 0.002(4) C4 0.029(5) 0.025(4) 0.018(5) 0.003(4) 0.008(4) -0.008(4) C9 0.028(5) 0.021(4) 0.021(5) 0.005(4) -0.002(4) 0.002(4) O6 0.028(5) 0.046(5) 0.066(6) -0.013(4) 0.006(4) -0.012(4) C45 0.032(6) 0.044(6) 0.025(6) -0.001(5) 0.005(5) -0.004(5) C8 0.018(5) 0.018(4) 0.032(6) 0.006(4) -0.003(4) 0.008(4) C30 0.034(6) 0.040(6) 0.028(6) 0.001(5) -0.005(5) -0.005(5) C54 0.022(5) 0.038(6) 0.039(7) -0.009(5) -0.008(5) -0.002(4) C52 0.041(6) 0.035(5) 0.033(6) 0.000(5) 0.002(5) -0.003(5) C6 0.020(5) 0.029(5) 0.027(5) 0.002(4) 0.004(4) -0.010(4) C7 0.020(5) 0.019(4) 0.022(5) 0.006(4) 0.004(4) 0.002(4) C34 0.049(7) 0.030(5) 0.034(6) 0.003(5) 0.002(5) -0.005(5) C22 0.041(6) 0.032(5) 0.038(6) -0.001(5) -0.013(5) 0.006(5) C53 0.025(5) 0.038(5) 0.030(6) -0.010(5) -0.006(4) -0.004(5) C27 0.048(7) 0.027(5) 0.058(9) 0.014(5) 0.000(6) -0.018(5) C35 0.037(6) 0.030(5) 0.058(8) -0.001(5) 0.004(6) -0.006(5) C21 0.048(7) 0.023(5) 0.043(7) -0.002(5) -0.006(6) 0.010(5) C31 0.019(5) 0.035(5) 0.040(6) 0.003(5) 0.002(4) 0.005(4) C32 0.029(6) 0.044(6) 0.042(7) 0.011(5) 0.007(5) -0.002(5) C13 0.038(6) 0.035(5) 0.023(5) 0.004(4) 0.004(5) -0.006(5) C23 0.047(7) 0.047(6) 0.023(6) -0.001(5) 0.012(5) 0.011(6) C48 0.039(6) 0.040(6) 0.038(7) -0.017(5) 0.008(5) -0.011(5) C50 0.052(8) 0.043(6) 0.052(8) 0.004(6) -0.022(7) -0.004(6) C46 0.046(7) 0.047(7) 0.040(7) -0.002(6) 0.015(6) 0.001(6) C25 0.035(6) 0.040(6) 0.026(6) 0.014(5) 0.004(5) 0.006(5) C28 0.055(8) 0.027(5) 0.063(9) -0.002(6) -0.019(7) -0.012(5) C56 0.031(6) 0.042(6) 0.040(7) -0.019(5) 0.009(5) -0.007(5) C24 0.028(6) 0.039(6) 0.039(7) 0.001(5) 0.002(5) 0.008(5) C49 0.039(7) 0.031(6) 0.075(10) -0.005(6) -0.004(7) 0.007(5) C2 0.027(5) 0.025(5) 0.024(5) 0.000(4) -0.007(4) 0.000(4) C55 0.040(7) 0.033(5) 0.036(7) -0.008(5) -0.004(5) 0.008(5) C11 0.065(9) 0.028(5) 0.051(8) -0.002(5) 0.004(7) -0.003(6) C10 0.096(13) 0.038(6) 0.036(7) -0.016(6) 0.017(8) -0.020(7) C42 0.040(7) 0.053(8) 0.075(11) 0.012(8) 0.001(7) -0.013(6) C40 0.048(9) 0.073(10) 0.073(12) -0.038(9) -0.033(8) 0.022(8) C20 0.074(10) 0.026(5) 0.040(7) -0.008(5) 0.002(7) 0.003(6) C47 0.047(7) 0.046(7) 0.051(8) -0.024(6) 0.020(6) 0.001(6) C14 0.055(8) 0.037(6) 0.037(7) 0.009(5) -0.003(6) 0.005(6) C26 0.044(7) 0.031(5) 0.039(7) 0.004(5) -0.001(5) 0.016(5) C51 0.070(10) 0.045(7) 0.035(7) 0.002(6) -0.011(7) -0.003(7) C15 0.034(7) 0.056(8) 0.077(11) -0.001(8) 0.007(7) 0.019(6) C17 0.027(6) 0.070(9) 0.045(8) 0.006(7) -0.006(5) -0.006(6) C18 0.055(8) 0.035(6) 0.058(9) 0.012(6) -0.001(7) -0.022(6) C12 0.043(7) 0.049(7) 0.035(7) 0.001(5) -0.011(6) -0.010(6) C38 0.098(16) 0.072(11) 0.062(12) -0.010(9) -0.019(11) 0.014(11) C37 0.057(9) 0.064(9) 0.048(9) -0.022(7) -0.020(7) 0.003(7) C16 0.038(7) 0.079(10) 0.045(8) 0.014(7) 0.008(6) -0.005(7) C43 0.043(7) 0.067(9) 0.074(9) -0.002(7) 0.015(7) -0.011(7) C19 0.061(9) 0.040(6) 0.034(7) -0.009(5) -0.006(6) -0.001(6) C39 0.097(15) 0.060(10) 0.075(13) -0.021(9) -0.018(11) 0.025(10) C29 0.060(8) 0.019(5) 0.048(8) -0.002(5) 0.007(6) -0.003(5) C44 0.047(8) 0.071(9) 0.084(10) -0.016(8) 0.002(7) -0.018(7) C41 0.043(8) 0.083(11) 0.071(11) 0.003(9) 0.017(8) -0.019(8) C36 0.051(15) 0.048(14) 0.048(15) 0.000(6) 0.003(6) 0.000(6) C36A 0.040(7) 0.039(6) 0.045(7) -0.007(5) 0.004(5) -0.007(5) C33 0.075(11) 0.039(7) 0.085(12) -0.009(8) 0.040(10) 0.000(7) C1 0.069(7) 0.032(5) 0.021(5) -0.007(4) 0.001(5) -0.006(5) O6A 0.028(5) 0.046(5) 0.066(6) -0.013(4) 0.006(4) -0.012(4) C44A 0.047(8) 0.071(9) 0.084(10) -0.016(8) 0.002(7) -0.018(7) C43A 0.043(7) 0.067(9) 0.074(9) -0.002(7) 0.015(7) -0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 Cl1 2.654(3) . ? U1 Si1 3.322(3) . ? U1 C5 2.641(10) . ? U1 C3 2.631(11) . ? U1 C4 2.759(9) . ? U1 C9 2.636(10) . ? U1 C8 2.569(10) . ? U1 C6 2.626(10) . ? U1 C7 2.556(10) . ? U1 C1 2.499(11) . ? Cl3 Mg1 2.507(4) . ? Cl3 Mg2 2.492(5) . ? Cl4 Mg1 2.495(4) . ? Cl4 Mg2 2.520(4) . ? Cl2 Mg1 2.509(4) . ? Cl2 Mg2 2.508(5) . ? Si5 C8 1.854(10) . ? Si5 C25 1.890(11) . ? Si5 C24 1.883(12) . ? Si5 C26 1.894(11) . ? Si4 C4 1.876(10) . ? Si4 C13 1.873(12) . ? Si4 C14 1.860(12) . ? Si4 C12 1.874(12) . ? Si7 C30 1.880(12) . ? Si7 C6 1.844(11) . ? Si7 C31 1.877(11) . ? Si7 C32 1.879(12) . ? Si6 C7 1.852(10) . ? Si6 C22 1.883(12) . ? Si6 C21 1.872(11) . ? Si6 C23 1.874(12) . ? Si3 C3 1.858(10) . ? Si3 C20 1.869(14) . ? Si3 C18 1.861(13) . ? Si3 C19 1.887(13) . ? Si8 C9 1.858(10) . ? Si8 C27 1.874(13) . ? Si8 C28 1.870(13) . ? Si8 C29 1.895(13) . ? Si2 C2 1.917(12) . ? Si2 C15 1.875(14) . ? Si2 C17 1.870(14) . ? Si2 C16 1.878(14) . ? Mg1 Mg2 3.142(5) . ? Mg1 O3 2.057(8) . ? Mg1 O1 2.087(9) . ? Mg1 O2 2.079(8) . ? Si1 C5 1.881(10) . ? Si1 C11 1.864(13) . ? Si1 C10 1.852(14) . ? Si1 C1 1.918(15) . ? Mg2 O4 2.098(9) . ? Mg2 O5 2.096(10) . ? Mg2 O6 2.109(10) . ? Mg2 O6A 2.11(2) . ? O3 C53 1.454(12) . ? O3 C56 1.461(13) . ? O1 C52 1.458(14) . ? O1 C49 1.485(14) . ? O2 C45 1.467(13) . ? O2 C48 1.456(12) . ? O4 C36 1.45(3) . ? O4 C36A 1.429(17) . ? O4 C33 1.459(17) . ? O5 C40 1.427(17) . ? O5 C37 1.42(2) . ? C5 C4 1.436(14) . ? C5 C2 1.551(15) . ? C3 C4 1.444(14) . ? C3 C2 1.570(13) . ? C9 C8 1.473(14) . ? C9 C6 1.462(14) . ? O6 C44 1.433(18) . ? O6 C41 1.46(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.495(17) . ? C8 C7 1.500(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C53 1.510(16) . ? C54 C55 1.534(14) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 C51 1.523(17) . ? C6 C7 1.472(14) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.525(17) . ? C34 C33 1.501(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 H35C 0.9900 . ? C35 H35D 0.9900 . ? C35 C36 1.53(3) . ? C35 C36A 1.53(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 C47 1.522(16) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 C49 1.517(19) . ? C50 C51 1.51(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.546(18) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56 C55 1.502(17) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C2 H2 1.0000 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 H42C 0.9900 . ? C42 H42D 0.9900 . ? C42 C43 1.48(2) . ? C42 C41 1.463(19) . ? C42 C43A 1.49(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C39 1.50(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C37 1.51(2) . ? C38 C39 1.49(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.53(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 H41C 0.9900 . ? C41 H41D 0.9900 . ? C41 O6A 1.46(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O6A C44A 1.43(3) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C44A C43A 1.53(4) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 U1 Si1 114.33(9) . . ? Cl1 U1 C4 81.9(2) . . ? C5 U1 Cl1 109.6(3) . . ? C5 U1 Si1 34.4(2) . . ? C5 U1 C4 30.7(3) . . ? C3 U1 Cl1 89.0(2) . . ? C3 U1 Si1 81.8(2) . . ? C3 U1 C5 47.5(3) . . ? C3 U1 C4 31.0(3) . . ? C3 U1 C9 148.2(3) . . ? C4 U1 Si1 58.8(2) . . ? C9 U1 Cl1 116.6(2) . . ? C9 U1 Si1 102.2(2) . . ? C9 U1 C5 128.2(3) . . ? C9 U1 C4 158.9(3) . . ? C8 U1 Cl1 130.9(2) . . ? C8 U1 Si1 110.8(2) . . ? C8 U1 C5 118.5(3) . . ? C8 U1 C3 116.0(3) . . ? C8 U1 C4 140.3(3) . . ? C8 U1 C9 32.8(3) . . ? C8 U1 C6 47.5(3) . . ? C6 U1 Cl1 87.6(2) . . ? C6 U1 Si1 130.2(2) . . ? C6 U1 C5 160.5(3) . . ? C6 U1 C3 145.7(3) . . ? C6 U1 C4 168.7(3) . . ? C6 U1 C9 32.3(3) . . ? C7 U1 Cl1 98.0(2) . . ? C7 U1 Si1 144.5(2) . . ? C7 U1 C5 145.0(3) . . ? C7 U1 C3 114.4(3) . . ? C7 U1 C4 145.1(3) . . ? C7 U1 C9 47.3(3) . . ? C7 U1 C8 34.0(3) . . ? C7 U1 C6 33.0(3) . . ? C1 U1 Cl1 97.9(3) . . ? C1 U1 Si1 35.0(4) . . ? C1 U1 C5 67.9(4) . . ? C1 U1 C3 112.9(4) . . ? C1 U1 C4 83.9(4) . . ? C1 U1 C9 83.5(4) . . ? C1 U1 C8 108.3(4) . . ? C1 U1 C6 101.5(4) . . ? C1 U1 C7 130.1(4) . . ? Mg2 Cl3 Mg1 77.88(13) . . ? Mg1 Cl4 Mg2 77.59(13) . . ? Mg2 Cl2 Mg1 77.55(14) . . ? C8 Si5 C25 111.0(5) . . ? C8 Si5 C24 114.3(5) . . ? C8 Si5 C26 113.8(5) . . ? C25 Si5 C26 104.9(5) . . ? C24 Si5 C25 107.6(6) . . ? C24 Si5 C26 104.6(6) . . ? C13 Si4 C4 107.1(5) . . ? C13 Si4 C12 110.4(6) . . ? C14 Si4 C4 113.8(5) . . ? C14 Si4 C13 106.8(6) . . ? C14 Si4 C12 105.0(6) . . ? C12 Si4 C4 113.6(5) . . ? C6 Si7 C30 112.3(5) . . ? C6 Si7 C31 113.2(5) . . ? C6 Si7 C32 108.6(5) . . ? C31 Si7 C30 105.7(5) . . ? C31 Si7 C32 106.8(5) . . ? C32 Si7 C30 110.2(6) . . ? C7 Si6 C22 114.0(5) . . ? C7 Si6 C21 113.0(5) . . ? C7 Si6 C23 110.4(5) . . ? C21 Si6 C22 106.9(5) . . ? C21 Si6 C23 108.8(6) . . ? C23 Si6 C22 103.3(6) . . ? C3 Si3 C20 113.0(6) . . ? C3 Si3 C18 112.1(6) . . ? C3 Si3 C19 110.6(5) . . ? C20 Si3 C19 105.5(6) . . ? C18 Si3 C20 107.4(6) . . ? C18 Si3 C19 107.9(7) . . ? C9 Si8 C27 108.3(5) . . ? C9 Si8 C28 113.9(5) . . ? C9 Si8 C29 116.1(5) . . ? C27 Si8 C29 107.7(6) . . ? C28 Si8 C27 105.8(7) . . ? C28 Si8 C29 104.4(7) . . ? C15 Si2 C2 109.3(6) . . ? C15 Si2 C16 110.5(8) . . ? C17 Si2 C2 112.0(6) . . ? C17 Si2 C15 105.5(7) . . ? C17 Si2 C16 108.2(7) . . ? C16 Si2 C2 111.1(6) . . ? Cl3 Mg1 Cl2 85.88(13) . . ? Cl3 Mg1 Mg2 50.84(11) . . ? Cl4 Mg1 Cl3 84.46(14) . . ? Cl4 Mg1 Cl2 84.33(14) . . ? Cl4 Mg1 Mg2 51.56(11) . . ? Cl2 Mg1 Mg2 51.21(11) . . ? O3 Mg1 Cl3 89.7(2) . . ? O3 Mg1 Cl4 174.0(3) . . ? O3 Mg1 Cl2 93.8(2) . . ? O3 Mg1 Mg2 123.1(2) . . ? O3 Mg1 O1 89.7(3) . . ? O3 Mg1 O2 91.2(3) . . ? O1 Mg1 Cl3 174.7(3) . . ? O1 Mg1 Cl4 96.0(3) . . ? O1 Mg1 Cl2 88.9(3) . . ? O1 Mg1 Mg2 125.7(3) . . ? O2 Mg1 Cl3 95.0(3) . . ? O2 Mg1 Cl4 90.8(3) . . ? O2 Mg1 Cl2 175.0(3) . . ? O2 Mg1 Mg2 126.1(3) . . ? O2 Mg1 O1 90.3(3) . . ? C5 Si1 U1 52.5(3) . . ? C5 Si1 C1 98.2(5) . . ? C11 Si1 U1 111.6(5) . . ? C11 Si1 C5 111.3(6) . . ? C11 Si1 C1 112.8(6) . . ? C10 Si1 U1 142.6(5) . . ? C10 Si1 C5 109.9(6) . . ? C10 Si1 C11 105.6(7) . . ? C10 Si1 C1 118.9(7) . . ? C1 Si1 U1 48.3(3) . . ? Cl3 Mg2 Cl4 84.25(14) . . ? Cl3 Mg2 Cl2 86.23(14) . . ? Cl3 Mg2 Mg1 51.27(11) . . ? Cl4 Mg2 Mg1 50.85(10) . . ? Cl2 Mg2 Cl4 83.84(14) . . ? Cl2 Mg2 Mg1 51.24(11) . . ? O4 Mg2 Cl3 91.6(3) . . ? O4 Mg2 Cl4 174.4(3) . . ? O4 Mg2 Cl2 92.2(3) . . ? O4 Mg2 Mg1 123.6(3) . . ? O4 Mg2 O6 93.5(4) . . ? O4 Mg2 O6A 86.0(19) . . ? O5 Mg2 Cl3 178.2(3) . . ? O5 Mg2 Cl4 95.0(3) . . ? O5 Mg2 Cl2 92.1(3) . . ? O5 Mg2 Mg1 127.1(3) . . ? O5 Mg2 O4 89.1(4) . . ? O5 Mg2 O6 88.8(5) . . ? O5 Mg2 O6A 99(4) . . ? O6 Mg2 Cl3 92.8(4) . . ? O6 Mg2 Cl4 90.4(3) . . ? O6 Mg2 Cl2 174.2(3) . . ? O6 Mg2 Mg1 124.2(3) . . ? O6A Mg2 Cl3 83(4) . . ? O6A Mg2 Cl4 97.2(16) . . ? O6A Mg2 Cl2 169(4) . . ? O6A Mg2 Mg1 122(2) . . ? C53 O3 Mg1 127.5(6) . . ? C53 O3 C56 108.2(8) . . ? C56 O3 Mg1 123.4(6) . . ? C52 O1 Mg1 121.5(7) . . ? C52 O1 C49 108.1(9) . . ? C49 O1 Mg1 121.7(7) . . ? C45 O2 Mg1 123.5(6) . . ? C48 O2 Mg1 129.2(7) . . ? C48 O2 C45 104.3(8) . . ? C36 O4 Mg2 118.4(12) . . ? C36 O4 C33 93(2) . . ? C36A O4 Mg2 127.5(9) . . ? C36A O4 C33 109.1(11) . . ? C33 O4 Mg2 121.8(8) . . ? C40 O5 Mg2 123.9(9) . . ? C37 O5 Mg2 123.2(9) . . ? C37 O5 C40 103.7(12) . . ? Si1 C5 U1 93.0(4) . . ? C4 C5 U1 79.2(6) . . ? C4 C5 Si1 131.2(8) . . ? C4 C5 C2 89.6(8) . . ? C2 C5 U1 74.3(6) . . ? C2 C5 Si1 134.8(8) . . ? Si3 C3 U1 129.6(5) . . ? C4 C3 U1 79.4(6) . . ? C4 C3 Si3 133.4(8) . . ? C4 C3 C2 88.5(8) . . ? C2 C3 U1 74.3(6) . . ? C2 C3 Si3 130.3(7) . . ? Si4 C4 U1 126.5(5) . . ? C5 C4 U1 70.1(5) . . ? C5 C4 Si4 130.0(8) . . ? C5 C4 C3 95.1(9) . . ? C3 C4 U1 69.6(6) . . ? C3 C4 Si4 134.4(8) . . ? Si8 C9 U1 132.6(5) . . ? C8 C9 U1 71.1(6) . . ? C8 C9 Si8 133.2(7) . . ? C6 C9 U1 73.5(5) . . ? C6 C9 Si8 131.1(8) . . ? C6 C9 C8 91.0(8) . . ? C44 O6 Mg2 129.8(11) . . ? C44 O6 C41 108.3(12) . . ? C41 O6 Mg2 120.8(8) . . ? O2 C45 H45A 110.7 . . ? O2 C45 H45B 110.7 . . ? O2 C45 C46 105.2(9) . . ? H45A C45 H45B 108.8 . . ? C46 C45 H45A 110.7 . . ? C46 C45 H45B 110.7 . . ? Si5 C8 U1 135.3(5) . . ? C9 C8 U1 76.1(6) . . ? C9 C8 Si5 132.0(7) . . ? C9 C8 C7 89.0(8) . . ? C7 C8 U1 72.5(5) . . ? C7 C8 Si5 130.1(8) . . ? Si7 C30 H30A 109.5 . . ? Si7 C30 H30B 109.5 . . ? Si7 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54A 111.7 . . ? C53 C54 H54B 111.7 . . ? C53 C54 C55 100.4(9) . . ? C55 C54 H54A 111.7 . . ? C55 C54 H54B 111.7 . . ? O1 C52 H52A 110.6 . . ? O1 C52 H52B 110.6 . . ? O1 C52 C51 105.6(11) . . ? H52A C52 H52B 108.8 . . ? C51 C52 H52A 110.6 . . ? C51 C52 H52B 110.6 . . ? Si7 C6 U1 123.8(5) . . ? C9 C6 U1 74.2(6) . . ? C9 C6 Si7 134.6(8) . . ? C9 C6 C7 90.5(8) . . ? C7 C6 U1 70.9(5) . . ? C7 C6 Si7 133.6(8) . . ? Si6 C7 U1 132.6(4) . . ? C8 C7 U1 73.5(6) . . ? C8 C7 Si6 134.2(8) . . ? C6 C7 U1 76.1(6) . . ? C6 C7 Si6 128.9(8) . . ? C6 C7 C8 89.5(8) . . ? H34A C34 H34B 109.1 . . ? C35 C34 H34A 111.2 . . ? C35 C34 H34B 111.2 . . ? C33 C34 H34A 111.2 . . ? C33 C34 H34B 111.2 . . ? C33 C34 C35 102.7(11) . . ? Si6 C22 H22A 109.5 . . ? Si6 C22 H22B 109.5 . . ? Si6 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C53 C54 105.8(8) . . ? O3 C53 H53A 110.6 . . ? O3 C53 H53B 110.6 . . ? C54 C53 H53A 110.6 . . ? C54 C53 H53B 110.6 . . ? H53A C53 H53B 108.7 . . ? Si8 C27 H27A 109.5 . . ? Si8 C27 H27B 109.5 . . ? Si8 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C34 C35 H35A 111.9 . . ? C34 C35 H35B 111.9 . . ? C34 C35 H35C 111.5 . . ? C34 C35 H35D 111.5 . . ? C34 C35 C36 99.4(17) . . ? C34 C35 C36A 101.4(11) . . ? H35A C35 H35B 109.6 . . ? H35C C35 H35D 109.3 . . ? C36 C35 H35A 111.9 . . ? C36 C35 H35B 111.9 . . ? C36A C35 H35C 111.5 . . ? C36A C35 H35D 111.5 . . ? Si6 C21 H21A 109.5 . . ? Si6 C21 H21B 109.5 . . ? Si6 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si7 C31 H31A 109.5 . . ? Si7 C31 H31B 109.5 . . ? Si7 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si7 C32 H32A 109.5 . . ? Si7 C32 H32B 109.5 . . ? Si7 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si6 C23 H23A 109.5 . . ? Si6 C23 H23B 109.5 . . ? Si6 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C48 H48A 110.8 . . ? O2 C48 H48B 110.8 . . ? O2 C48 C47 104.7(9) . . ? H48A C48 H48B 108.9 . . ? C47 C48 H48A 110.8 . . ? C47 C48 H48B 110.8 . . ? H50A C50 H50B 109.2 . . ? C49 C50 H50A 111.3 . . ? C49 C50 H50B 111.3 . . ? C51 C50 H50A 111.3 . . ? C51 C50 H50B 111.3 . . ? C51 C50 C49 102.2(11) . . ? C45 C46 H46A 110.9 . . ? C45 C46 H46B 110.9 . . ? C45 C46 C47 104.2(10) . . ? H46A C46 H46B 108.9 . . ? C47 C46 H46A 110.9 . . ? C47 C46 H46B 110.9 . . ? Si5 C25 H25A 109.5 . . ? Si5 C25 H25B 109.5 . . ? Si5 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si8 C28 H28A 109.5 . . ? Si8 C28 H28B 109.5 . . ? Si8 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C56 H56A 110.5 . . ? O3 C56 H56B 110.5 . . ? O3 C56 C55 106.2(9) . . ? H56A C56 H56B 108.7 . . ? C55 C56 H56A 110.5 . . ? C55 C56 H56B 110.5 . . ? Si5 C24 H24A 109.5 . . ? Si5 C24 H24B 109.5 . . ? Si5 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C49 C50 105.5(11) . . ? O1 C49 H49A 110.6 . . ? O1 C49 H49B 110.6 . . ? C50 C49 H49A 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.8 . . ? Si2 C2 H2 114.6 . . ? C5 C2 Si2 107.4(7) . . ? C5 C2 C3 85.8(7) . . ? C5 C2 H2 114.6 . . ? C3 C2 Si2 116.3(7) . . ? C3 C2 H2 114.6 . . ? C54 C55 H55A 111.2 . . ? C54 C55 H55B 111.2 . . ? C56 C55 C54 102.9(9) . . ? C56 C55 H55A 111.2 . . ? C56 C55 H55B 111.2 . . ? H55A C55 H55B 109.1 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H42A C42 H42B 109.4 . . ? H42C C42 H42D 109.6 . . ? C43 C42 H42A 111.7 . . ? C43 C42 H42B 111.7 . . ? C41 C42 H42A 111.7 . . ? C41 C42 H42B 111.7 . . ? C41 C42 H42C 111.9 . . ? C41 C42 H42D 111.9 . . ? C41 C42 C43 100.5(14) . . ? C41 C42 C43A 99(4) . . ? C43A C42 H42C 111.9 . . ? C43A C42 H42D 111.9 . . ? O5 C40 H40A 110.6 . . ? O5 C40 H40B 110.6 . . ? O5 C40 C39 105.6(15) . . ? H40A C40 H40B 108.8 . . ? C39 C40 H40A 110.6 . . ? C39 C40 H40B 110.6 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C48 C47 C46 105.0(10) . . ? C48 C47 H47A 110.7 . . ? C48 C47 H47B 110.7 . . ? C46 C47 H47A 110.7 . . ? C46 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C52 C51 H51A 111.3 . . ? C52 C51 H51B 111.3 . . ? C50 C51 C52 102.1(11) . . ? C50 C51 H51A 111.3 . . ? C50 C51 H51B 111.3 . . ? H51A C51 H51B 109.2 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H38A C38 H38B 108.9 . . ? C37 C38 H38A 110.8 . . ? C37 C38 H38B 110.8 . . ? C39 C38 H38A 110.8 . . ? C39 C38 H38B 110.8 . . ? C39 C38 C37 104.5(17) . . ? O5 C37 C38 107.1(13) . . ? O5 C37 H37A 110.3 . . ? O5 C37 H37B 110.3 . . ? C38 C37 H37A 110.3 . . ? C38 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C42 C43 H43A 111.0 . . ? C42 C43 H43B 111.0 . . ? C42 C43 C44 103.6(15) . . ? H43A C43 H43B 109.0 . . ? C44 C43 H43A 111.0 . . ? C44 C43 H43B 111.0 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C40 C39 H39A 110.9 . . ? C40 C39 H39B 110.9 . . ? C38 C39 C40 104.2(15) . . ? C38 C39 H39A 110.9 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? Si8 C29 H29A 109.5 . . ? Si8 C29 H29B 109.5 . . ? Si8 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C44 C43 101.9(14) . . ? O6 C44 H44A 111.4 . . ? O6 C44 H44B 111.4 . . ? C43 C44 H44A 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.3 . . ? O6 C41 C42 108.2(13) . . ? O6 C41 H41A 110.1 . . ? O6 C41 H41B 110.1 . . ? C42 C41 H41A 110.1 . . ? C42 C41 H41B 110.1 . . ? C42 C41 H41C 109.0 . . ? C42 C41 H41D 109.0 . . ? H41A C41 H41B 108.4 . . ? H41C C41 H41D 107.8 . . ? O6A C41 C42 113(3) . . ? O6A C41 H41C 109.0 . . ? O6A C41 H41D 109.0 . . ? O4 C36 C35 105.4(18) . . ? O4 C36 H36A 110.7 . . ? O4 C36 H36B 110.7 . . ? C35 C36 H36A 110.7 . . ? C35 C36 H36B 110.7 . . ? H36A C36 H36B 108.8 . . ? O4 C36A C35 106.7(12) . . ? O4 C36A H36C 110.4 . . ? O4 C36A H36D 110.4 . . ? C35 C36A H36C 110.4 . . ? C35 C36A H36D 110.4 . . ? H36C C36A H36D 108.6 . . ? O4 C33 C34 106.1(12) . . ? O4 C33 H33A 110.5 . . ? O4 C33 H33B 110.5 . . ? C34 C33 H33A 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? U1 C1 H1A 112.4 . . ? U1 C1 H1B 112.4 . . ? Si1 C1 U1 96.7(5) . . ? Si1 C1 H1A 112.4 . . ? Si1 C1 H1B 112.4 . . ? H1A C1 H1B 110.0 . . ? C41 O6A Mg2 120.5(19) . . ? C44A O6A Mg2 132(4) . . ? C44A O6A C41 105(3) . . ? O6A C44A H44C 111.4 . . ? O6A C44A H44D 111.4 . . ? O6A C44A C43A 102(3) . . ? H44C C44A H44D 109.3 . . ? C43A C44A H44C 111.4 . . ? C43A C44A H44D 111.4 . . ? C42 C43A C44A 106(3) . . ? C42 C43A H43C 110.5 . . ? C42 C43A H43D 110.5 . . ? C44A C43A H43C 110.5 . . ? C44A C43A H43D 110.5 . . ? H43C C43A H43D 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 Si1 C5 C4 -78.2(9) . . . . ? U1 Si1 C5 C2 70.7(10) . . . . ? U1 C5 C4 Si4 -121.5(8) . . . . ? U1 C5 C4 C3 66.2(6) . . . . ? U1 C5 C2 Si2 172.0(5) . . . . ? U1 C5 C2 C3 -71.7(6) . . . . ? U1 C3 C4 Si4 121.7(9) . . . . ? U1 C3 C4 C5 -66.6(6) . . . . ? U1 C3 C2 Si2 179.6(7) . . . . ? U1 C3 C2 C5 72.2(5) . . . . ? U1 C9 C8 Si5 -139.6(10) . . . . ? U1 C9 C8 C7 72.2(5) . . . . ? U1 C9 C6 Si7 122.3(10) . . . . ? U1 C9 C6 C7 -70.0(6) . . . . ? U1 C8 C7 Si6 -134.2(9) . . . . ? U1 C8 C7 C6 75.7(6) . . . . ? U1 C6 C7 Si6 134.2(8) . . . . ? U1 C6 C7 C8 -73.1(6) . . . . ? Si5 C8 C7 U1 135.1(9) . . . . ? Si5 C8 C7 Si6 0.9(16) . . . . ? Si5 C8 C7 C6 -149.2(9) . . . . ? Si7 C6 C7 U1 -118.9(10) . . . . ? Si7 C6 C7 Si6 15.2(15) . . . . ? Si7 C6 C7 C8 168.0(9) . . . . ? Si3 C3 C4 U1 -135.7(10) . . . . ? Si3 C3 C4 Si4 -14.0(18) . . . . ? Si3 C3 C4 C5 157.8(9) . . . . ? Si3 C3 C2 Si2 -51.3(13) . . . . ? Si3 C3 C2 C5 -158.7(9) . . . . ? Si8 C9 C8 U1 131.3(10) . . . . ? Si8 C9 C8 Si5 -8.3(18) . . . . ? Si8 C9 C8 C7 -156.5(9) . . . . ? Si8 C9 C6 U1 -132.7(9) . . . . ? Si8 C9 C6 Si7 -10.4(17) . . . . ? Si8 C9 C6 C7 157.3(8) . . . . ? Mg1 O3 C53 C54 170.6(7) . . . . ? Mg1 O3 C56 C55 164.2(8) . . . . ? Mg1 O1 C52 C51 -133.4(8) . . . . ? Mg1 O1 C49 C50 158.9(8) . . . . ? Mg1 O2 C45 C46 120.8(9) . . . . ? Mg1 O2 C48 C47 -122.2(10) . . . . ? Si1 C5 C4 U1 84.5(8) . . . . ? Si1 C5 C4 Si4 -37.0(14) . . . . ? Si1 C5 C4 C3 150.7(9) . . . . ? Si1 C5 C2 Si2 93.8(10) . . . . ? Si1 C5 C2 C3 -149.9(9) . . . . ? Mg2 O4 C36 C35 -175.8(16) . . . . ? Mg2 O4 C36A C35 153.8(9) . . . . ? Mg2 O4 C33 C34 -178.9(8) . . . . ? Mg2 O5 C40 C39 -108.3(13) . . . . ? Mg2 O5 C37 C38 113.5(14) . . . . ? Mg2 O6 C44 C43 147.8(12) . . . . ? Mg2 O6 C41 C42 -174.4(11) . . . . ? Mg2 O6A C44A C43A 134(13) . . . . ? O3 C56 C55 C54 28.5(13) . . . . ? O1 C52 C51 C50 -34.4(12) . . . . ? O2 C45 C46 C47 26.6(13) . . . . ? O2 C48 C47 C46 -21.2(14) . . . . ? O5 C40 C39 C38 -28.9(18) . . . . ? C4 C5 C2 Si2 -109.1(7) . . . . ? C4 C5 C2 C3 7.2(8) . . . . ? C4 C3 C2 Si2 100.2(8) . . . . ? C4 C3 C2 C5 -7.2(8) . . . . ? C9 C8 C7 U1 -75.7(6) . . . . ? C9 C8 C7 Si6 150.2(9) . . . . ? C9 C8 C7 C6 0.0(8) . . . . ? C9 C6 C7 U1 73.1(6) . . . . ? C9 C6 C7 Si6 -152.7(8) . . . . ? C9 C6 C7 C8 0.0(8) . . . . ? C45 O2 C48 C47 38.3(13) . . . . ? C45 C46 C47 C48 -3.3(15) . . . . ? C8 C9 C6 U1 69.9(6) . . . . ? C8 C9 C6 Si7 -167.7(10) . . . . ? C8 C9 C6 C7 0.0(8) . . . . ? C30 Si7 C6 U1 44.1(7) . . . . ? C30 Si7 C6 C9 -57.6(12) . . . . ? C30 Si7 C6 C7 139.5(10) . . . . ? C52 O1 C49 C50 10.8(13) . . . . ? C6 C9 C8 U1 -72.2(6) . . . . ? C6 C9 C8 Si5 148.2(10) . . . . ? C6 C9 C8 C7 0.0(8) . . . . ? C34 C35 C36 O4 -38(3) . . . . ? C34 C35 C36A O4 30.3(16) . . . . ? C22 Si6 C7 U1 -89.2(7) . . . . ? C22 Si6 C7 C8 21.6(12) . . . . ? C22 Si6 C7 C6 161.9(9) . . . . ? C53 O3 C56 C55 -5.5(13) . . . . ? C53 C54 C55 C56 -39.3(12) . . . . ? C27 Si8 C9 U1 168.0(7) . . . . ? C27 Si8 C9 C8 63.0(12) . . . . ? C27 Si8 C9 C6 -85.1(11) . . . . ? C35 C34 C33 O4 31.2(16) . . . . ? C21 Si6 C7 U1 33.1(9) . . . . ? C21 Si6 C7 C8 143.9(10) . . . . ? C21 Si6 C7 C6 -75.8(10) . . . . ? C31 Si7 C6 U1 -75.5(7) . . . . ? C31 Si7 C6 C9 -177.1(10) . . . . ? C31 Si7 C6 C7 19.9(12) . . . . ? C32 Si7 C6 U1 166.1(6) . . . . ? C32 Si7 C6 C9 64.5(12) . . . . ? C32 Si7 C6 C7 -98.5(11) . . . . ? C13 Si4 C4 U1 -157.6(5) . . . . ? C13 Si4 C4 C5 -63.6(10) . . . . ? C13 Si4 C4 C3 105.6(11) . . . . ? C23 Si6 C7 U1 155.1(6) . . . . ? C23 Si6 C7 C8 -94.1(11) . . . . ? C23 Si6 C7 C6 46.2(10) . . . . ? C48 O2 C45 C46 -41.0(12) . . . . ? C25 Si5 C8 U1 164.5(7) . . . . ? C25 Si5 C8 C9 -78.9(12) . . . . ? C25 Si5 C8 C7 57.6(11) . . . . ? C28 Si8 C9 U1 -74.6(9) . . . . ? C28 Si8 C9 C8 -179.7(11) . . . . ? C28 Si8 C9 C6 32.3(12) . . . . ? C56 O3 C53 C54 -20.2(12) . . . . ? C24 Si5 C8 U1 42.6(9) . . . . ? C24 Si5 C8 C9 159.1(10) . . . . ? C24 Si5 C8 C7 -64.3(11) . . . . ? C49 O1 C52 C51 14.7(12) . . . . ? C49 C50 C51 C52 40.1(13) . . . . ? C2 C5 C4 U1 -74.0(6) . . . . ? C2 C5 C4 Si4 164.5(9) . . . . ? C2 C5 C4 C3 -7.8(8) . . . . ? C2 C3 C4 U1 74.3(6) . . . . ? C2 C3 C4 Si4 -164.0(9) . . . . ? C2 C3 C4 C5 7.7(8) . . . . ? C55 C54 C53 O3 36.8(12) . . . . ? C11 Si1 C5 U1 -101.4(6) . . . . ? C11 Si1 C5 C4 -179.7(10) . . . . ? C11 Si1 C5 C2 -30.7(12) . . . . ? C10 Si1 C5 U1 141.9(7) . . . . ? C10 Si1 C5 C4 63.7(12) . . . . ? C10 Si1 C5 C2 -147.4(11) . . . . ? C42 C43 C44 O6 38.3(18) . . . . ? C42 C41 O6A Mg2 -155(6) . . . . ? C42 C41 O6A C44A 11(10) . . . . ? C40 O5 C37 C38 -34.4(17) . . . . ? C20 Si3 C3 U1 -50.9(8) . . . . ? C20 Si3 C3 C4 66.0(12) . . . . ? C20 Si3 C3 C2 -154.9(10) . . . . ? C14 Si4 C4 U1 84.7(7) . . . . ? C14 Si4 C4 C5 178.6(9) . . . . ? C14 Si4 C4 C3 -12.1(13) . . . . ? C26 Si5 C8 U1 -77.5(8) . . . . ? C26 Si5 C8 C9 39.1(13) . . . . ? C26 Si5 C8 C7 175.6(9) . . . . ? C51 C50 C49 O1 -31.9(13) . . . . ? C18 Si3 C3 U1 -172.4(7) . . . . ? C18 Si3 C3 C4 -55.5(13) . . . . ? C18 Si3 C3 C2 83.6(11) . . . . ? C12 Si4 C4 U1 -35.4(8) . . . . ? C12 Si4 C4 C5 58.5(11) . . . . ? C12 Si4 C4 C3 -132.2(11) . . . . ? C37 O5 C40 C39 39.2(14) . . . . ? C37 C38 C39 C40 8(2) . . . . ? C43 C42 C41 O6 28.8(18) . . . . ? C19 Si3 C3 U1 67.1(8) . . . . ? C19 Si3 C3 C4 -176.0(11) . . . . ? C19 Si3 C3 C2 -36.9(12) . . . . ? C39 C38 C37 O5 16(2) . . . . ? C29 Si8 C9 U1 46.8(9) . . . . ? C29 Si8 C9 C8 -58.3(13) . . . . ? C29 Si8 C9 C6 153.6(10) . . . . ? C44 O6 C41 C42 -5.2(19) . . . . ? C41 O6 C44 C43 -20.2(19) . . . . ? C41 C42 C43 C44 -40.8(18) . . . . ? C41 C42 C43A C44A -32(10) . . . . ? C41 O6A C44A C43A -29(8) . . . . ? C36 O4 C33 C34 -53(2) . . . . ? C36A O4 C33 C34 -12.5(18) . . . . ? C33 O4 C36 C35 55(3) . . . . ? C33 O4 C36A C35 -11.6(18) . . . . ? C33 C34 C35 C36 4(2) . . . . ? C33 C34 C35 C36A -36.8(15) . . . . ? C1 Si1 C5 U1 17.1(5) . . . . ? C1 Si1 C5 C4 -61.2(11) . . . . ? C1 Si1 C5 C2 87.7(10) . . . . ? O6A C44A C43A C42 40(9) . . . . ? C43A C42 C41 O6A 14(11) . . . . ? _smtbx_masks_special_details ; A solvent mask was calculated and 78 electrons were found in a volume of 490\%A^3^ in 3 voids per unit cell. This is consistent with the presence of 0.5[C4H8O] per Asymmetric Unit which account for 80 electrons per unit cell. ; loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 213.1 38.7 '1 C4H8O' 2 0.000 0.500 0.500 213.1 38.7 '1 C4H8O' 3 0.167 0.167 0.233 7.3 0.4 ? 4 0.167 0.333 0.733 7.3 0.2 ? 5 0.329 0.683 0.107 9.4 0.2 ? 6 0.329 0.817 0.607 9.4 0.3 ? 7 0.671 0.183 0.393 9.4 0.0 ? 8 0.671 0.317 0.893 9.4 0.0 ? 9 0.833 0.667 0.267 7.3 0.3 ? 10 0.833 0.833 0.767 7.3 0.2 ? _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 2021ntl15p49b_pc_twin1_hklf4_a.res in P2(1)/c 2021ntl15p49b_pc_twin1_hklf4.res created by SHELXL-2018/3 at 19:05:38 on 21-Aug-2022 REM Old TITL 2021NTL15p49b_pc_twin1_hklf4 in Pc REM SHELXT solution in P2(1)/c: R1 0.195, Rweak 0.006, Alpha 0.041 REM 0.194 for 9 systematic absences, Orientation as input REM Formula found by SHELXT: C64 O9 Mg2 Si8 Cl4 CELL 1.54184 13.3309 17.7676 33.435 90 90.681 90 ZERR 4 0.0002 0.0002 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Mg O Si U UNIT 224 480 16 8 24 32 4 SADI C35 C36 C35 C36A SADI O4 C36 O4 C36A ISOR 0.005 0.005 C36 C36A ISOR 0.01 0.01 C1 SADI 0.04 O6 C43 O6A C43A SADI Mg2 O6 Mg2 O6A SADI O6 C41 O6A C41 SADI O6 C44 O6A C44A SADI 0.04 C44 C41 C44A C41 SADI 0.04 C42 C44 C42 C44A SADI C43 C44 C43A C44A SADI C42 C43 C42 C43A SADI 0.04 Mg2 C44 Mg2 C44A ISOR 0.01 0.01 C43 C44 O6 EADP O6 O6A EADP C43 C43A EADP C44 C44A L.S. 32 PLAN 5 SIZE 0.053 0.129 0.179 TEMP -173 CONF FREE U1 C2 BOND list 4 fmap 2 MORE -1 BOND $H ABIN ACTA OMIT 6 7 15 REM REM REM WGHT 0.186500 BASF 0.09358 FVAR 1.25194 0.29975 0.93202 U1 7 0.468290 0.784024 0.368982 11.00000 0.01790 0.02185 = 0.01840 0.00007 0.00031 0.00195 CL3 3 0.921924 0.835634 0.104650 11.00000 0.02603 0.03331 = 0.03060 0.00195 0.00070 -0.00374 CL4 3 1.073253 0.686269 0.118473 11.00000 0.02438 0.03602 = 0.04530 -0.00892 -0.00543 -0.00011 CL2 3 0.922559 0.739466 0.193171 11.00000 0.03782 0.03212 = 0.02764 -0.00308 -0.00530 -0.01058 CL1 3 0.349870 0.894901 0.343942 11.00000 0.03136 0.03881 = 0.04523 0.01312 0.00660 0.00982 SI5 6 0.568041 0.663624 0.466188 11.00000 0.02468 0.02371 = 0.02383 0.00251 -0.00165 0.00536 SI4 6 0.564251 0.904437 0.269888 11.00000 0.03071 0.03092 = 0.02304 0.00399 -0.00008 -0.00178 SI7 6 0.193256 0.773127 0.412158 11.00000 0.02019 0.03032 = 0.02908 0.00136 0.00219 -0.00024 SI6 6 0.408322 0.850642 0.481937 11.00000 0.03043 0.02365 = 0.02147 -0.00196 0.00051 0.00198 SI3 6 0.659096 0.961960 0.381137 11.00000 0.04078 0.02511 = 0.02981 -0.00370 -0.00231 -0.00707 SI8 6 0.342859 0.580275 0.400213 11.00000 0.03334 0.02001 = 0.03633 0.00209 -0.00399 -0.00557 SI2 6 0.810989 0.780307 0.360188 11.00000 0.02411 0.04583 = 0.03783 0.00310 -0.00103 0.00289 MG1 4 0.887444 0.700966 0.122167 11.00000 0.01911 0.02917 = 0.02713 -0.00682 0.00102 -0.00506 SI1 6 0.572860 0.685682 0.295982 11.00000 0.04982 0.03063 = 0.03406 -0.00750 0.00632 -0.00623 MG2 4 1.055303 0.808935 0.155547 11.00000 0.02325 0.03270 = 0.03892 -0.00649 -0.00376 -0.00633 O3 5 0.736822 0.725134 0.125339 11.00000 0.01936 0.03338 = 0.02959 -0.01676 -0.00005 -0.00399 O1 5 0.858909 0.591942 0.142300 11.00000 0.03052 0.02966 = 0.04295 -0.00714 0.00360 -0.00209 O2 5 0.871003 0.665366 0.063212 11.00000 0.02750 0.03633 = 0.02530 -0.01002 0.00426 -0.00616 O4 5 1.025168 0.909706 0.185816 11.00000 0.02693 0.03018 = 0.04295 -0.00186 0.00272 -0.00594 O5 5 1.164842 0.783690 0.199001 11.00000 0.03448 0.04855 = 0.05765 -0.01698 -0.01689 0.00362 C5 1 0.623901 0.772457 0.321232 11.00000 0.00596 0.02810 = 0.04058 -0.00716 0.00751 -0.00324 C3 1 0.624393 0.871390 0.356915 11.00000 0.02871 0.02549 = 0.02545 -0.00039 -0.00086 0.00157 C4 1 0.598986 0.850539 0.316285 11.00000 0.02925 0.02470 = 0.01798 0.00291 0.00821 -0.00778 C9 1 0.383875 0.677792 0.412100 11.00000 0.02837 0.02083 = 0.02059 0.00523 -0.00153 0.00173 PART 1 O6 5 1.168264 0.857641 0.120281 31.00000 0.02824 0.04593 = 0.06638 -0.01288 0.00607 -0.01183 PART 0 C45 1 0.932281 0.693833 0.030362 11.00000 0.03169 0.04379 = 0.02530 -0.00066 0.00540 -0.00396 AFIX 23 H45A 2 0.982246 0.730721 0.040379 11.00000 -1.20000 H45B 2 0.889637 0.718397 0.009732 11.00000 -1.20000 AFIX 0 C8 1 0.469957 0.708878 0.434632 11.00000 0.01780 0.01821 = 0.03206 0.00553 -0.00321 0.00753 C30 1 0.148069 0.759864 0.359156 11.00000 0.03363 0.03955 = 0.02827 0.00107 -0.00478 -0.00500 AFIX 137 H30A 2 0.180325 0.797022 0.341878 11.00000 -1.50000 H30B 2 0.075142 0.766608 0.357849 11.00000 -1.50000 H30C 2 0.165183 0.709047 0.350109 11.00000 -1.50000 AFIX 0 C54 1 0.559980 0.720114 0.119922 11.00000 0.02208 0.03759 = 0.03863 -0.00940 -0.00803 -0.00224 AFIX 23 H54A 2 0.541551 0.687826 0.142821 11.00000 -1.20000 H54B 2 0.503646 0.721645 0.100377 11.00000 -1.20000 AFIX 0 C52 1 0.780291 0.576561 0.171106 11.00000 0.04102 0.03496 = 0.03321 0.00013 0.00201 -0.00265 AFIX 23 H52A 2 0.722340 0.551641 0.157887 11.00000 -1.20000 H52B 2 0.757015 0.623816 0.183645 11.00000 -1.20000 AFIX 0 C6 1 0.326093 0.746453 0.418859 11.00000 0.02020 0.02917 = 0.02693 0.00152 0.00401 -0.00980 C7 1 0.410626 0.779285 0.441566 11.00000 0.02034 0.01880 = 0.02244 0.00615 0.00445 0.00220 C34 1 0.934246 1.002203 0.221112 11.00000 0.04865 0.02977 = 0.03401 0.00260 0.00233 -0.00504 AFIX 23 H34A 2 0.959532 0.999905 0.249046 11.00000 -1.20000 H34B 2 0.868330 1.027872 0.220589 11.00000 -1.20000 AFIX 0 C22 1 0.526688 0.854294 0.513167 11.00000 0.04088 0.03206 = 0.03780 -0.00053 -0.01339 0.00584 AFIX 137 H22A 2 0.541288 0.804104 0.523907 11.00000 -1.50000 H22B 2 0.517840 0.889745 0.535301 11.00000 -1.50000 H22C 2 0.582543 0.870933 0.496549 11.00000 -1.50000 AFIX 0 C53 1 0.656023 0.694164 0.100822 11.00000 0.02504 0.03803 = 0.03002 -0.01011 -0.00595 -0.00377 AFIX 23 H53A 2 0.659519 0.638513 0.100393 11.00000 -1.20000 H53B 2 0.660221 0.713009 0.073028 11.00000 -1.20000 AFIX 0 C27 1 0.314452 0.530948 0.448310 11.00000 0.04813 0.02721 = 0.05801 0.01361 0.00031 -0.01757 AFIX 137 H27A 2 0.377258 0.520131 0.462717 11.00000 -1.50000 H27B 2 0.279209 0.483700 0.442552 11.00000 -1.50000 H27C 2 0.272034 0.563221 0.464812 11.00000 -1.50000 AFIX 0 C35 1 1.008873 1.041821 0.194029 11.00000 0.03674 0.02983 = 0.05846 -0.00060 0.00355 -0.00623 PART 1 AFIX 23 H35A 2 1.071823 1.054754 0.208456 21.00000 -1.20000 H35B 2 0.979899 1.087737 0.181729 21.00000 -1.20000 AFIX 23 PART 2 H35C 2 1.042949 1.083904 0.208048 -21.00000 -1.20000 H35D 2 0.975854 1.061014 0.169389 -21.00000 -1.20000 AFIX 0 PART 0 C21 1 0.385155 0.948252 0.462907 11.00000 0.04848 0.02340 = 0.04288 -0.00175 -0.00594 0.01036 AFIX 137 H21A 2 0.449397 0.972482 0.457101 11.00000 -1.50000 H21B 2 0.349816 0.977440 0.483234 11.00000 -1.50000 H21C 2 0.344122 0.945940 0.438423 11.00000 -1.50000 AFIX 0 C31 1 0.167941 0.874368 0.424441 11.00000 0.01878 0.03499 = 0.04003 0.00309 0.00153 0.00538 AFIX 137 H31A 2 0.206927 0.906801 0.406724 11.00000 -1.50000 H31B 2 0.187386 0.884235 0.452309 11.00000 -1.50000 H31C 2 0.096290 0.884938 0.420704 11.00000 -1.50000 AFIX 0 C32 1 0.115638 0.715072 0.447112 11.00000 0.02880 0.04442 = 0.04200 0.01096 0.00674 -0.00200 AFIX 137 H32A 2 0.044465 0.726825 0.442912 11.00000 -1.50000 H32B 2 0.134902 0.726591 0.474819 11.00000 -1.50000 H32C 2 0.127059 0.661516 0.441839 11.00000 -1.50000 AFIX 0 C13 1 0.675719 0.902201 0.236343 11.00000 0.03827 0.03535 = 0.02316 0.00406 0.00427 -0.00597 AFIX 137 H13A 2 0.731663 0.929121 0.249138 11.00000 -1.50000 H13B 2 0.658587 0.926469 0.210842 11.00000 -1.50000 H13C 2 0.695238 0.849843 0.231494 11.00000 -1.50000 AFIX 0 C23 1 0.309525 0.826772 0.519259 11.00000 0.04676 0.04733 = 0.02346 -0.00069 0.01236 0.01108 AFIX 137 H23A 2 0.245215 0.819094 0.505350 11.00000 -1.50000 H23B 2 0.303176 0.868129 0.538457 11.00000 -1.50000 H23C 2 0.328509 0.780608 0.533492 11.00000 -1.50000 AFIX 0 C48 1 0.828176 0.595697 0.047745 11.00000 0.03851 0.04003 = 0.03798 -0.01746 0.00753 -0.01102 AFIX 23 H48A 2 0.768813 0.606081 0.030548 11.00000 -1.20000 H48B 2 0.807959 0.562164 0.069880 11.00000 -1.20000 AFIX 0 C50 1 0.898893 0.478387 0.177325 11.00000 0.05188 0.04274 = 0.05167 0.00374 -0.02208 -0.00409 AFIX 23 H50A 2 0.862737 0.438118 0.162626 11.00000 -1.20000 H50B 2 0.952560 0.455567 0.194068 11.00000 -1.20000 AFIX 0 C46 1 0.983223 0.626028 0.013592 11.00000 0.04597 0.04663 = 0.04022 -0.00183 0.01530 0.00060 AFIX 23 H46A 2 1.049935 0.618535 0.026297 11.00000 -1.20000 H46B 2 0.991598 0.630910 -0.015675 11.00000 -1.20000 AFIX 0 C25 1 0.518604 0.640898 0.517532 11.00000 0.03487 0.04002 = 0.02559 0.01384 0.00428 0.00620 AFIX 137 H25A 2 0.489680 0.686344 0.529349 11.00000 -1.50000 H25B 2 0.573667 0.622639 0.534617 11.00000 -1.50000 H25C 2 0.466828 0.601927 0.515256 11.00000 -1.50000 AFIX 0 C28 1 0.224878 0.575317 0.369505 11.00000 0.05451 0.02708 = 0.06341 -0.00153 -0.01859 -0.01215 AFIX 137 H28A 2 0.171174 0.602182 0.383282 11.00000 -1.50000 H28B 2 0.205536 0.522547 0.365769 11.00000 -1.50000 H28C 2 0.236096 0.598624 0.343372 11.00000 -1.50000 AFIX 0 C56 1 0.696733 0.788190 0.148215 11.00000 0.03089 0.04156 = 0.03959 -0.01900 0.00858 -0.00686 AFIX 23 H56A 2 0.736952 0.834175 0.143666 11.00000 -1.20000 H56B 2 0.697909 0.776559 0.177174 11.00000 -1.20000 AFIX 0 C24 1 0.685184 0.721639 0.473141 11.00000 0.02764 0.03881 = 0.03896 0.00059 0.00164 0.00775 AFIX 137 H24A 2 0.731367 0.711388 0.451214 11.00000 -1.50000 H24B 2 0.717557 0.708528 0.498671 11.00000 -1.50000 H24C 2 0.667585 0.775192 0.473155 11.00000 -1.50000 AFIX 0 C49 1 0.940933 0.536634 0.148918 11.00000 0.03861 0.03089 = 0.07471 -0.00455 -0.00420 0.00738 AFIX 23 H49A 2 1.000627 0.561458 0.160877 11.00000 -1.20000 H49B 2 0.960312 0.512915 0.123356 11.00000 -1.20000 AFIX 0 C2 1 0.668097 0.790144 0.363301 11.00000 0.02662 0.02538 = 0.02395 0.00011 -0.00748 -0.00039 AFIX 13 H2 2 0.636907 0.761281 0.385618 11.00000 -1.20000 AFIX 0 C55 1 0.590810 0.799297 0.133566 11.00000 0.03988 0.03263 = 0.03560 -0.00803 -0.00408 0.00841 AFIX 23 H55A 2 0.587910 0.835453 0.111053 11.00000 -1.20000 H55B 2 0.547242 0.817546 0.155291 11.00000 -1.20000 AFIX 0 C11 1 0.635154 0.598910 0.315419 11.00000 0.06472 0.02753 = 0.05069 -0.00172 0.00363 -0.00279 AFIX 137 H11A 2 0.644538 0.603111 0.344448 11.00000 -1.50000 H11B 2 0.700562 0.592949 0.302727 11.00000 -1.50000 H11C 2 0.593104 0.555060 0.309298 11.00000 -1.50000 AFIX 0 C10 1 0.600780 0.688497 0.241873 11.00000 0.09581 0.03795 = 0.03607 -0.01571 0.01714 -0.02024 AFIX 137 H10A 2 0.566059 0.731362 0.229518 11.00000 -1.50000 H10B 2 0.577790 0.641725 0.229220 11.00000 -1.50000 H10C 2 0.673266 0.693892 0.238249 11.00000 -1.50000 AFIX 0 C42 1 1.259366 0.881643 0.061295 11.00000 0.03985 0.05324 = 0.07498 0.01208 0.00133 -0.01322 PART 1 AFIX 23 H42A 2 1.250452 0.935600 0.054774 31.00000 -1.20000 H42B 2 1.283064 0.854464 0.037348 31.00000 -1.20000 AFIX 23 PART 2 H42C 2 1.245121 0.920939 0.041018 -31.00000 -1.20000 H42D 2 1.304292 0.843073 0.049854 -31.00000 -1.20000 AFIX 0 PART 0 C40 1 1.239867 0.727139 0.194358 11.00000 0.04797 0.07308 = 0.07341 -0.03815 -0.03256 0.02151 AFIX 23 H40A 2 1.306902 0.747096 0.201746 11.00000 -1.20000 H40B 2 1.241485 0.709237 0.166333 11.00000 -1.20000 AFIX 0 C20 1 0.554385 1.031928 0.380651 11.00000 0.07393 0.02581 = 0.04033 -0.00791 0.00241 0.00258 AFIX 137 H20A 2 0.559029 1.063496 0.356709 11.00000 -1.50000 H20B 2 0.559240 1.063650 0.404574 11.00000 -1.50000 H20C 2 0.489984 1.005324 0.380415 11.00000 -1.50000 AFIX 0 C47 1 0.911903 0.560241 0.023601 11.00000 0.04703 0.04641 = 0.05131 -0.02375 0.01979 0.00077 AFIX 23 H47A 2 0.884820 0.536940 -0.001162 11.00000 -1.20000 H47B 2 0.947391 0.521227 0.039477 11.00000 -1.20000 AFIX 0 C14 1 0.535274 1.005284 0.279177 11.00000 0.05474 0.03678 = 0.03684 0.00892 -0.00276 0.00543 AFIX 137 H14A 2 0.476331 1.009075 0.296300 11.00000 -1.50000 H14B 2 0.521436 1.030558 0.253650 11.00000 -1.50000 H14C 2 0.592787 1.029358 0.292477 11.00000 -1.50000 AFIX 0 C26 1 0.613957 0.570457 0.445868 11.00000 0.04364 0.03129 = 0.03925 0.00445 -0.00113 0.01557 AFIX 137 H26A 2 0.557576 0.535230 0.443747 11.00000 -1.50000 H26B 2 0.665253 0.549704 0.463978 11.00000 -1.50000 H26C 2 0.642801 0.578223 0.419362 11.00000 -1.50000 AFIX 0 C51 1 0.827906 0.524811 0.202289 11.00000 0.06985 0.04487 = 0.03478 0.00211 -0.01144 -0.00309 AFIX 23 H51A 2 0.864602 0.553859 0.223065 11.00000 -1.20000 H51B 2 0.776953 0.492746 0.215228 11.00000 -1.20000 AFIX 0 C15 1 0.845990 0.678448 0.364766 11.00000 0.03402 0.05573 = 0.07694 -0.00051 0.00655 0.01882 AFIX 137 H15A 2 0.806530 0.655050 0.385957 11.00000 -1.50000 H15B 2 0.917570 0.674212 0.371401 11.00000 -1.50000 H15C 2 0.832165 0.652838 0.339333 11.00000 -1.50000 AFIX 0 C17 1 0.876839 0.828701 0.402645 11.00000 0.02661 0.06993 = 0.04534 0.00616 -0.00603 -0.00568 AFIX 137 H17A 2 0.868087 0.883254 0.400051 11.00000 -1.50000 H17B 2 0.948486 0.816440 0.402130 11.00000 -1.50000 H17C 2 0.848461 0.811776 0.428010 11.00000 -1.50000 AFIX 0 C18 1 0.768547 1.007208 0.356856 11.00000 0.05467 0.03494 = 0.05758 0.01183 -0.00128 -0.02198 AFIX 137 H18A 2 0.828536 0.976344 0.361395 11.00000 -1.50000 H18B 2 0.779256 1.057360 0.368334 11.00000 -1.50000 H18C 2 0.755492 1.011749 0.328050 11.00000 -1.50000 AFIX 0 C12 1 0.450741 0.866448 0.243142 11.00000 0.04336 0.04930 = 0.03473 0.00114 -0.01051 -0.01043 AFIX 137 H12A 2 0.456138 0.811591 0.241009 11.00000 -1.50000 H12B 2 0.446284 0.888425 0.216296 11.00000 -1.50000 H12C 2 0.390449 0.879466 0.258136 11.00000 -1.50000 AFIX 0 C38 1 1.156034 0.702713 0.254804 11.00000 0.09817 0.07198 = 0.06222 -0.00980 -0.01901 0.01400 AFIX 23 H38A 2 1.194828 0.700191 0.280201 11.00000 -1.20000 H38B 2 1.089454 0.679430 0.258852 11.00000 -1.20000 AFIX 0 C37 1 1.145291 0.783039 0.240795 11.00000 0.05705 0.06423 = 0.04803 -0.02209 -0.02019 0.00347 AFIX 23 H37A 2 1.076620 0.801635 0.245902 11.00000 -1.20000 H37B 2 1.193673 0.815829 0.255203 11.00000 -1.20000 AFIX 0 C16 1 0.858904 0.820585 0.312125 11.00000 0.03780 0.07853 = 0.04531 0.01431 0.00766 -0.00547 AFIX 137 H16A 2 0.831887 0.791536 0.289529 11.00000 -1.50000 H16B 2 0.932340 0.818076 0.312099 11.00000 -1.50000 H16C 2 0.837487 0.873163 0.309665 11.00000 -1.50000 AFIX 0 PART 1 C43 1 1.328246 0.870822 0.096034 31.00000 0.04289 0.06679 = 0.07437 -0.00228 0.01491 -0.01104 AFIX 23 H43A 2 1.386466 0.905261 0.094565 31.00000 -1.20000 H43B 2 1.352805 0.818289 0.097391 31.00000 -1.20000 AFIX 0 PART 0 C19 1 0.691945 0.946933 0.435613 11.00000 0.06147 0.03973 = 0.03425 -0.00900 -0.00578 -0.00128 AFIX 137 H19A 2 0.632189 0.955006 0.451856 11.00000 -1.50000 H19B 2 0.744400 0.982608 0.443759 11.00000 -1.50000 H19C 2 0.716305 0.895381 0.439512 11.00000 -1.50000 AFIX 0 C39 1 1.210607 0.664291 0.222027 11.00000 0.09726 0.05972 = 0.07519 -0.02146 -0.01822 0.02459 AFIX 23 H39A 2 1.166659 0.627522 0.208109 11.00000 -1.20000 H39B 2 1.270675 0.637779 0.232545 11.00000 -1.20000 AFIX 0 C29 1 0.435567 0.520122 0.371966 11.00000 0.05984 0.01927 = 0.04757 -0.00243 0.00722 -0.00282 AFIX 137 H29A 2 0.435593 0.535173 0.343768 11.00000 -1.50000 H29B 2 0.416182 0.467072 0.374030 11.00000 -1.50000 H29C 2 0.502881 0.527005 0.383488 11.00000 -1.50000 AFIX 0 PART 1 C44 1 1.262867 0.889480 0.132048 31.00000 0.04701 0.07146 = 0.08424 -0.01646 0.00244 -0.01831 AFIX 23 H44A 2 1.289311 0.865740 0.156799 31.00000 -1.20000 H44B 2 1.257632 0.944514 0.136159 31.00000 -1.20000 AFIX 0 PART 0 C41 1 1.167331 0.848517 0.076895 11.00000 0.04303 0.08252 = 0.07095 0.00328 0.01651 -0.01930 PART 1 AFIX 23 H41A 2 1.107995 0.874052 0.065081 31.00000 -1.20000 H41B 2 1.163881 0.794436 0.069884 31.00000 -1.20000 AFIX 23 PART 2 H41C 2 1.110817 0.860837 0.058565 -31.00000 -1.20000 H41D 2 1.174559 0.793072 0.077485 -31.00000 -1.20000 AFIX 0 PART 1 C36 1 1.024820 0.979451 0.163147 21.00000 0.05118 0.04752 = 0.04774 -0.00024 0.00349 -0.00019 AFIX 23 H36A 2 0.969899 0.979409 0.142955 21.00000 -1.20000 H36B 2 1.089417 0.986418 0.149319 21.00000 -1.20000 AFIX 0 PART 2 C36A 1 1.081867 0.977953 0.184838 -21.00000 0.04003 0.03862 = 0.04510 -0.00668 0.00399 -0.00654 AFIX 23 H36C 2 1.111656 0.985169 0.158128 -21.00000 -1.20000 H36D 2 1.136667 0.976502 0.205069 -21.00000 -1.20000 AFIX 0 PART 0 C33 1 0.927153 0.925049 0.203006 11.00000 0.07476 0.03916 = 0.08530 -0.00937 0.04045 0.00011 AFIX 23 H33A 2 0.911127 0.887246 0.223723 11.00000 -1.20000 H33B 2 0.874178 0.923608 0.182016 11.00000 -1.20000 AFIX 0 C1 1 0.436140 0.694585 0.312598 11.00000 0.06858 0.03244 = 0.02133 -0.00658 0.00119 -0.00558 AFIX 23 H1A 2 0.408118 0.646062 0.321795 11.00000 -1.20000 H1B 2 0.392277 0.716492 0.291524 11.00000 -1.20000 AFIX 0 PART 2 O6A 5 1.143619 0.875109 0.117020 -31.00000 0.02824 0.04593 = 0.06638 -0.01288 0.00607 -0.01183 C44A 1 1.211002 0.936604 0.124303 -31.00000 0.04701 0.07146 = 0.08424 -0.01646 0.00244 -0.01831 AFIX 23 H44C 2 1.229379 0.940495 0.153004 -31.00000 -1.20000 H44D 2 1.181746 0.984947 0.115180 -31.00000 -1.20000 AFIX 0 C43A 1 1.301315 0.914204 0.099065 -31.00000 0.04289 0.06679 = 0.07437 -0.00228 0.01491 -0.01104 AFIX 23 H43C 2 1.343251 0.958768 0.093232 -31.00000 -1.20000 H43D 2 1.343058 0.876553 0.113386 -31.00000 -1.20000 AFIX 0 HKLF 5 REM 2021ntl15p49b_pc_twin1_hklf4_a.res in P2(1)/c REM wR2 = 0.2452, GooF = S = 1.014, Restrained GooF = 1.014 for all data REM R1 = 0.0828 for 15631 Fo > 4sig(Fo) and 0.1008 for all 21288 data REM 738 parameters refined using 47 restraints END WGHT 0.1866 0.0000 REM Highest difference peak 4.428, deepest hole -4.477, 1-sigma level 0.249 Q1 1 0.5398 0.7844 0.3857 11.00000 0.05 3.75 Q2 1 0.3961 0.7843 0.3506 11.00000 0.05 3.74 Q3 1 0.5602 0.8174 0.3698 11.00000 0.05 3.43 Q4 1 0.3769 0.8164 0.3656 11.00000 0.05 3.42 Q5 1 0.5620 0.7565 0.3716 11.00000 0.05 3.31 ; _shelx_res_checksum 82554 _shelx_hkl_file ; 16 0 6 683.639 429.878 -2 -16 0 -6 683.639 429.878 1 16 0 4 13202.5 647.178 -2 -16 0 -4 13202.5 647.178 1 16 0 2 500.542 436.492 -2 -16 0 -2 500.542 436.492 1 16 0 0 8121.08 595.505 -2 -16 0 0 8121.08 595.505 1 16 0 -2-54.8054 471.990 -2 -16 0 2-54.8054 471.990 1 16 0 -4 13088.6 611.660 -2 -16 0 4 13088.6 611.660 1 16 0 -6 3708.87 475.974 -2 -16 0 6 3708.87 475.974 1 16 -1 6 21382.2 507.448 -2 -16 -1 -6 21382.2 507.448 1 16 1 5 352.725 314.323 -2 -16 1 -5 352.725 314.323 1 16 -1 4 491.031 312.997 -2 -16 -1 -4 491.031 312.997 1 16 -1 3 14.8039 321.805 -2 -16 -1 -3 14.8039 321.805 1 16 1 2 16084.3 490.890 -2 -16 1 -2 16084.3 490.890 1 16 -1 1 3734.44 367.625 -2 -16 -1 -1 3734.44 367.625 1 16 1 0 31.3024 293.091 -2 -16 1 0 31.3024 293.091 1 16 1 -1 2051.78 339.795 -2 -16 1 1 2051.78 339.795 1 16 -1 -2 10264.9 405.643 -2 -16 -1 2 10264.9 405.643 1 16 -1 -3 1495.24 338.052 -2 -16 -1 3 1495.24 338.052 1 16 1 -4 51.3177 280.309 -2 -16 1 4 51.3177 280.309 1 16 1 -5 946.383 274.121 -2 -16 1 5 946.383 274.121 1 16 -1 -6 10911.6 390.644 -2 -16 -1 6 10911.6 390.644 1 16 -1 -7 2449.22 296.107 -2 -16 -1 7 2449.22 296.107 1 16 -2 5 4894.54 344.194 -2 -16 -2 -5 4894.54 344.194 1 16 2 4 3448.26 328.758 -2 -16 2 -4 3448.26 328.758 1 16 2 3 1098.19 308.172 -2 -16 2 -3 1098.19 308.172 1 16 -2 2 1041.66 318.078 -2 -16 -2 -2 1041.66 318.078 1 16 -2 1 1412.96 332.772 -2 -16 -2 -1 1412.96 332.772 1 16 2 0 3490.62 329.323 -2 -16 2 0 3490.62 329.323 1 16 -2 -1 1598.35 321.238 -2 -16 -2 1 1598.35 321.238 1 16 2 -2 261.293 285.369 -2 -16 2 2 261.293 285.369 1 16 -2 -3 2766.10 327.552 -2 -16 -2 3 2766.10 327.552 1 16 2 -4 6392.11 340.225 -2 -16 2 4 6392.11 340.225 1 16 -2 -5 559.555 164.406 -2 -16 -2 5 559.555 164.406 1 16 -2 -6 457.768 260.715 -2 -16 -2 6 457.768 260.715 1 16 -3 3 319.147 259.218 -2 -16 -3 -3 319.147 259.218 1 16 -3 2 5659.65 320.329 -2 -16 -3 -2 5659.65 320.329 1 16 3 1 5468.59 326.726 -2 -16 3 -1 5468.59 326.726 1 16 3 0 208.160 165.201 -2 -16 3 0 208.160 165.201 1 16 3 -1 405.449 256.082 -2 -16 3 1 405.449 256.082 1 16 -3 -2 3611.12 305.854 -2 -16 -3 2 3611.12 305.854 1 16 -3 -3 3417.02 290.292 -2 -16 -3 3 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3544.93 -2 -2 -8 7 112959. 3544.93 1 2 -8 -8 3320.41 1149.16 -2 -2 -8 8 3320.41 1149.16 1 2 -8 -9 82853.4 3264.41 -2 -2 -8 9 82853.4 3264.41 1 2 -8 -10 6098.34 1412.37 -2 -2 -8 10 6098.34 1412.37 1 2 -8 -11 104356. 3786.53 -2 -2 -8 11 104356. 3786.53 1 2 -8 -12 1416.10 1194.32 -2 -2 -8 12 1416.10 1194.32 1 2 -8 -13 40692.4 2737.93 -2 -2 -8 13 40692.4 2737.93 1 2 -8 -14 1684.27 1272.92 -2 -2 -8 14 1684.27 1272.92 1 2 -8 -15 77142.9 3685.05 -2 -2 -8 15 77142.9 3685.05 1 2 -8 -16 91.6840 625.695 -2 -2 -8 16 91.6840 625.695 1 2 -8 -17 18100.3 2246.27 -2 -2 -8 17 18100.3 2246.27 1 2 -8 -18 2505.09 1508.66 -2 -2 -8 18 2505.09 1508.66 1 2 -8 -19 13216.9 950.191 -2 -2 -8 19 13216.9 950.191 1 2 -8 -20 14703.9 989.705 -2 -2 -8 20 14703.9 989.705 1 2 -8 -21 108331. 1715.31 -2 -2 -8 21 108331. 1715.31 1 2 -8 -22 1151.13 617.110 -2 -2 -8 22 1151.13 617.110 1 2 -8 -23 7760.95 681.178 -2 -2 -8 23 7760.95 681.178 1 2 -8 -24 8834.51 660.158 -2 -2 -8 24 8834.51 660.158 1 2 8 -25 27778.2 1145.96 -2 -2 8 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1582.99 -2 -2 9 -29 13965.2 1582.99 1 2 9 28 11.1978 512.509 -2 -2 9 -28 11.1978 512.509 1 2 9 27 10741.3 1568.90 -2 -2 9 -27 10741.3 1568.90 1 2 9 26 552.785 1041.69 -2 -2 9 -26 552.785 1041.69 1 2 9 25 10726.0 1593.14 -2 -2 9 -25 10726.0 1593.14 1 2 9 24 7312.45 1188.43 -2 -2 9 -24 7312.45 1188.43 1 2 9 23 18285.1 1593.32 -2 -2 9 -23 18285.1 1593.32 1 2 9 22 2635.48 1457.67 -2 -2 9 -22 2635.48 1457.67 1 2 9 21 1925.06 1480.35 -2 -2 9 -21 1925.06 1480.35 1 2 9 20 17573.0 1684.95 -2 -2 9 -20 17573.0 1684.95 1 2 9 19 62458.3 1700.37 -2 -2 9 -19 62458.3 1700.37 1 2 9 18 7498.63 847.560 -2 -2 9 -18 7498.63 847.560 1 2 9 17 279.165 1078.23 -2 -2 9 -17 279.165 1078.23 1 2 9 16 5581.12 1162.89 -2 -2 9 -16 5581.12 1162.89 1 2 9 15 22695.3 1815.37 -2 -2 9 -15 22695.3 1815.37 1 2 9 14 2790.77 1111.85 -2 -2 9 -14 2790.77 1111.85 1 2 9 13 1348.16 1024.53 -2 -2 9 -13 1348.16 1024.53 1 2 9 12 5205.29 1106.13 -2 -2 9 -12 5205.29 1106.13 1 2 9 11 14714.0 1508.76 -2 -2 9 -11 14714.0 1508.76 1 2 9 10 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0.8354 15 6 5 2.1579 0.7352 15 6 6 -1.2265 0.5104 15 6 7 1.8238 0.5075 15 6 8 -1.6135 0.0899 15 6 9 1.5184 -0.0713 15 6 10 -0.9048 -0.2907 15 7 0 0.2200 0.3991 15 7 1 0.8675 0.0494 15 7 2 0.2706 0.9525 15 7 3 2.3609 0.1388 15 7 4 0.0363 0.9616 15 7 5 1.0954 0.8061 15 7 6 1.0830 0.8575 15 7 7 -1.1951 -0.0187 15 7 8 0.7684 0.5667 15 8 0 -0.1220 -0.2475 15 8 1 0.3023 0.7326 15 8 2 1.7852 0.4522 15 8 3 -0.7062 1.8533 15 8 4 2.4532 0.3982 16 0 0 1.6789 0.6468 16 0 2 1.7178 0.2463 16 0 4 -0.0055 -1.0112 16 0 6 -0.6851 -1.4677 16 1 0 -1.3892 0.2852 16 1 1 1.7572 0.0939 16 1 2 0.3921 0.1313 16 1 3 1.8760 0.3348 16 1 4 -1.6926 0.7579 16 1 5 -0.7521 0.9130 16 1 6 -0.4307 1.4229 16 2 0 2.6704 0.0886 16 2 1 -0.9388 0.2691 16 2 2 1.7717 0.3033 16 2 3 -1.0012 0.2778 16 2 4 0.2557 1.4266 16 2 5 -0.6691 0.6180 16 3 0 -0.6788 0.3318 16 3 1 2.7117 0.3422 16 3 2 -0.5416 0.6845 16 3 3 -0.5716 0.8420 0 0 0 0.0 0.0 ; _shelx_fab_checksum 93838 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.684 _oxdiff_exptl_absorpt_empirical_full_min 0.266 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.906(3) 406 41983 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.094(3) 434 41983 nmt -0.9996 0.0002 0.0025 0.0007 1.0001 -0.0013 -0.0144 -0.0091 -1.0008 _twin_special_details ; Component 2 rotated by 179.6709\% around [-0.00 1.00 -0.00] (reciprocal) or [0.00 1.00 -0.00] (direct) ;