#------------------------------------------------------------------------------ #$Date: 2015-10-09 16:07:17 +0300 (Fri, 09 Oct 2015) $ #$Revision: 162082 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/48/7054813.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7054813 loop_ _publ_author_name 'Kahan, Rachel J.' 'Cloke, F. Geoffrey N.' 'Roe, S. Mark' 'Nief, Fran\,cois' _publ_section_title ; Activation of carbon dioxide by new mixed sandwich uranium(iii) complexes incorporating cyclooctatetraenyl and pyrrolide, phospholide, or arsolide ligands ; _journal_issue 10 _journal_name_full 'New J. Chem.' _journal_page_first 7602 _journal_paper_doi 10.1039/C5NJ00590F _journal_volume 39 _journal_year 2015 _chemical_formula_moiety 'C70 H120 N2 O5 Si4 U2' _chemical_formula_sum 'C70 H120 N2 O5 Si4 U2' _chemical_formula_weight 1658.09 _chemical_name_common 4 _chemical_name_systematic 4 _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-03-02 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2015-04-16 deposited with the CCDC. 2015-04-22 downloaded from the CCDC. ; _cell_angle_alpha 97.035(6) _cell_angle_beta 97.053(6) _cell_angle_gamma 102.983(7) _cell_formula_units_Z 2 _cell_length_a 12.9610(9) _cell_length_b 14.6337(10) _cell_length_c 22.2106(16) _cell_measurement_reflns_used 39042 _cell_measurement_temperature 173.15 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.4 _cell_volume 4024.5(5) _computing_cell_refinement ; CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112) ; _computing_data_collection ; CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112) ; _computing_data_reduction ; CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXL (Sheldrick, 2008)' _diffrn_ambient_temperature 173.15 _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_unetI/netI 0.0952 _diffrn_reflns_laue_measured_fraction_full 0.984 _diffrn_reflns_laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 47825 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.562 _diffrn_reflns_theta_min 2.430 _diffrn_source 'Sealed Tube' _diffrn_standards_interval_count 120 _diffrn_standards_interval_time 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.121 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_crystal_colour 'clear yellowish orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description plate _exptl_crystal_F_000 1668 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: hexane' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _refine_diff_density_max 4.017 _refine_diff_density_min -2.642 _refine_diff_density_rms 0.194 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 750 _refine_ls_number_reflns 18150 _refine_ls_number_restraints 1119 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0703 _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^)+(0.1107P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1751 _refine_ls_wR_factor_ref 0.1944 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11223 _reflns_number_total 18150 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5nj00590f2.cif _cod_data_source_block 4 _cod_depositor_comments 'Adding full bibliography for 7054809--7054814.cif.' _cod_database_code 7054813 _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. ; _shelx_estimated_absorpt_t_max 0.960 _shelx_estimated_absorpt_t_min 0.761 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C27) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1 Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C40) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1 Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C53) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1 Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C58) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1 3. Rigid body (RIGU) restrains U2, C1, N1, O2, O3, C2, C5, U1, C3, C6, C4, C9, O1, O4, C47, C49, C50, C46, C48, C52, C51, C45, O5, C25, C20, C26, C24, C23, C21, C19, C22, C7, H6A, H6B, H6C, C8, H9A, H9B, H9C, C10, H47, H49, H50, H46, Si4, H52, H51, Si3, H25, H20, H26, H24, H23, H21, Si1, Si2, H7A, H7B, H7C, H8A, H8B, H8C, N2, C62, C65, C68, C53, C56, C59, C27, C30, C33, C36, C39, C42, C11, C14, H62, C63, C64, H65, C66, C67, H68, C69, C70, H53, C54, C55, H56, C57, C58, H59, C60, C61, H27, C28, C29, H30, C31, C32, H33, C34, C35, H36, C37, C38, H39, C40, C41, H42, C43, C44, C12, C15, C13, C18, H63A, H63B, H63C, H64A, H64B, H64C, H66A, H66B, H66C, H67A, H67B, H67C, H69A, H69B, H69C, H70A, H70B, H70C, H54A, H54B, H54C, H55A, H55B, H55C, H57A, H57B, H57C, H58A, H58B, H58C, H60A, H60B, H60C, H61A, H61B, H61C, H28A, H28B, H28C, H29A, H29B, H29C, H31A, H31B, H31C, H32A, H32B, H32C, H34A, H34B, H34C, H35A, H35B, H35C, H37A, H37B, H37C, H38A, H38B, H38C, H40A, H40B, H40C, H41A, H41B, H41C, H43A, H43B, H43C, H44A, H44B, H44C, C16, H15A, H15B, H15C, C17, H18A, H18B, H18C, H16A, H16B, H16C, H17A, H17B, H17C with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Ternary CH refined with riding coordinates: C27(H27), C30(H30), C33(H33), C36(H36), C39(H39), C42(H42), C53(H53), C56(H56), C59(H59), C62(H62), C65(H65), C68(H68) 4.b Me refined with riding coordinates: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C28(H28A,H28B, H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A, H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C54(H54A,H54B, H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A, H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B, H70C) 4.c Aromatic/amide H refined with riding coordinates: C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52) 4.d Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C43(H43A,H43B,H43C) ; _shelx_res_file ; rjk363.res created by SHELXL-2014/7 TITL 2013ncs0533 in P -1 CELL 0.71073 12.961 14.6337 22.2106 97.035 97.053 102.983 ZERR 2 0.0009 0.001 0.0016 0.006 0.006 0.007 LATT 1 SFAC C H N O Si U UNIT 140 240 4 10 8 4 RIGU U2 C1 N1 O2 O3 C2 C5 U1 C3 C6 C4 C9 O1 O4 C47 C49 C50 C46 C48 C52 C51 = C45 O5 C25 C20 C26 C24 C23 C21 C19 C22 C7 H6A H6B H6C C8 H9A H9B H9C C10 H47 = H49 H50 H46 SI4 H52 H51 SI3 H25 H20 H26 H24 H23 H21 SI1 SI2 H7A H7B H7C H8A = H8B H8C N2 C62 C65 C68 C53 C56 C59 C27 C30 C33 C36 C39 C42 C11 C14 H62 C63 = C64 H65 C66 C67 H68 C69 C70 H53 C54 C55 H56 C57 C58 H59 C60 C61 H27 C28 C29 = H30 C31 C32 H33 C34 C35 H36 C37 C38 H39 C40 C41 H42 C43 C44 C12 C15 C13 C18 = H63A H63B H63C H64A H64B H64C H66A H66B H66C H67A H67B H67C H69A H69B H69C = H70A H70B H70C H54A H54B H54C H55A H55B H55C H57A H57B H57C H58A H58B H58C = H60A H60B H60C H61A H61B H61C H28A H28B H28C H29A H29B H29C H31A H31B H31C = H32A H32B H32C H34A H34B H34C H35A H35B H35C H37A H37B H37C H38A H38B H38C = H40A H40B H40C H41A H41B H41C H43A H43B H43C H44A H44B H44C C16 H15A H15B = H15C C17 H18A H18B H18C H16A H16B H16C H17A H17B H17C ISOR 0.01 0.02 C12 ISOR 0.01 0.02 C13 ISOR 0.01 0.02 C16 ISOR 0.01 0.02 C17 ISOR 0.01 0.02 C18 ISOR 0.05 0.1 C27 ISOR 0.01 0.02 C28 ISOR 0.01 0.02 C29 ISOR 0.01 0.02 C31 ISOR 0.01 0.02 C32 ISOR 0.01 0.02 C35 ISOR 0.01 0.02 C37 ISOR 0.01 0.02 C39 ISOR 0.05 0.1 C40 ISOR 0.01 0.02 C41 ISOR 0.01 0.02 C42 ISOR 0.01 0.02 C43 ISOR 0.01 0.02 C44 ISOR 0.05 0.1 C53 ISOR 0.01 0.02 C54 ISOR 0.01 0.02 C57 ISOR 0.05 0.1 C58 L.S. 50 PLAN 5 SIZE 0.01 0.06 0.07 TEMP -100 HTAB 2.00000 BOND $H CONF fmap 2 MORE -1 acta MERG 2 OMIT 1 2 0 OMIT -3 -4 4 OMIT 1 -1 3 OMIT -1 -1 1 REM REM REM WGHT 0.110700 FVAR 0.33242 C1 1 0.044957 0.904743 0.765490 11.00000 0.02083 0.03773 = 0.04339 0.00844 -0.00046 0.00603 C2 1 0.214315 0.899304 0.828058 11.00000 0.02538 0.05389 = 0.05862 0.00362 -0.00272 0.01233 C3 1 0.309708 0.964083 0.848831 11.00000 0.02232 0.07039 = 0.04243 -0.00150 0.00294 0.00454 C4 1 0.304658 1.048802 0.828057 11.00000 0.02196 0.06904 = 0.06341 0.01018 0.00074 -0.00321 C5 1 0.203878 1.039633 0.795116 11.00000 0.02695 0.04773 = 0.05276 0.00058 0.00679 0.00038 C6 1 0.176197 0.801370 0.840909 11.00000 0.05524 0.05910 = 0.08921 0.01584 -0.02496 0.01370 AFIX 137 H6A 2 0.233741 0.784228 0.866645 11.00000 -1.50000 H6B 2 0.155510 0.757176 0.802145 11.00000 -1.50000 H6C 2 0.114132 0.797942 0.862435 11.00000 -1.50000 AFIX 0 C7 1 0.405099 0.944532 0.888354 11.00000 0.03258 0.11566 = 0.05973 0.00403 -0.01308 0.02060 AFIX 33 H7A 2 0.464006 1.001865 0.897329 11.00000 -1.50000 H7B 2 0.383748 0.926444 0.926900 11.00000 -1.50000 H7C 2 0.428722 0.892749 0.866179 11.00000 -1.50000 AFIX 0 C8 1 0.396289 1.134936 0.837815 11.00000 0.04891 0.09188 = 0.12229 0.02583 -0.00848 -0.02681 AFIX 33 H8A 2 0.458309 1.122905 0.862673 11.00000 -1.50000 H8B 2 0.415052 1.149207 0.797990 11.00000 -1.50000 H8C 2 0.375460 1.189052 0.859165 11.00000 -1.50000 AFIX 0 C9 1 0.163235 1.105845 0.759018 11.00000 0.03929 0.05018 = 0.08800 0.01712 0.00170 -0.00932 AFIX 33 H9A 2 0.087984 1.077894 0.741309 11.00000 -1.50000 H9B 2 0.169041 1.165774 0.785811 11.00000 -1.50000 H9C 2 0.205672 1.117865 0.725947 11.00000 -1.50000 AFIX 0 C10 1 -0.202740 0.768858 0.830607 11.00000 0.03478 0.04979 = 0.05848 0.02176 0.00157 -0.00121 C11 1 -0.194934 0.658090 0.905105 11.00000 0.06491 0.05312 = 0.04796 0.02015 -0.01447 -0.01078 C12 1 -0.251300 0.635972 0.952075 11.00000 0.07417 0.09797 = 0.06916 0.03991 0.00095 -0.00694 C13 1 -0.311379 0.703361 0.961414 11.00000 0.10205 0.12542 = 0.09013 0.05628 0.02901 0.01784 C14 1 -0.296472 0.768605 0.921840 11.00000 0.06466 0.12561 = 0.07817 0.05154 0.02811 0.02919 C15 1 -0.112351 0.616556 0.884580 11.00000 0.09685 0.06134 = 0.04395 0.02068 -0.01201 0.00967 AFIX 33 H15A 2 -0.086498 0.646253 0.850266 11.00000 -1.50000 H15B 2 -0.052823 0.626842 0.918415 11.00000 -1.50000 H15C 2 -0.141441 0.548264 0.871069 11.00000 -1.50000 AFIX 0 C16 1 -0.243134 0.560298 0.990915 11.00000 0.09468 0.11715 = 0.09572 0.06307 -0.00591 -0.01489 AFIX 33 H16A 2 -0.292748 0.560583 1.020829 11.00000 -1.50000 H16B 2 -0.261628 0.498227 0.964674 11.00000 -1.50000 H16C 2 -0.169686 0.572600 1.012642 11.00000 -1.50000 AFIX 0 C17 1 -0.380451 0.712043 1.013361 11.00000 0.14610 0.21848 = 0.12094 0.08493 0.06527 0.05694 AFIX 33 H17A 2 -0.381333 0.659033 1.036473 11.00000 -1.50000 H17B 2 -0.349715 0.772130 1.041067 11.00000 -1.50000 H17C 2 -0.453840 0.710438 0.995283 11.00000 -1.50000 AFIX 0 C18 1 -0.343738 0.847221 0.911612 11.00000 0.10263 0.16074 = 0.09622 0.07038 0.05843 0.06749 AFIX 33 H18A 2 -0.312817 0.878340 0.879063 11.00000 -1.50000 H18B 2 -0.421391 0.823550 0.899277 11.00000 -1.50000 H18C 2 -0.328993 0.892977 0.949573 11.00000 -1.50000 AFIX 0 C19 1 -0.397750 0.959372 0.689964 11.00000 0.03754 0.07858 = 0.04002 0.01456 0.00585 0.03736 C20 1 -0.385797 0.990840 0.753383 11.00000 0.03584 0.08879 = 0.04102 0.01316 0.00683 0.02970 AFIX 43 H20 2 -0.450255 0.966154 0.768421 11.00000 -1.20000 AFIX 0 C21 1 -0.307488 1.048179 0.802451 11.00000 0.02981 0.09266 = 0.03932 0.01265 0.00379 0.02676 AFIX 43 H21 2 -0.330246 1.045291 0.841383 11.00000 -1.20000 AFIX 0 C22 1 -0.203332 1.108598 0.806527 11.00000 0.03989 0.07814 = 0.04651 0.01998 0.00855 0.03212 C23 1 -0.138213 1.128312 0.761391 11.00000 0.04055 0.06262 = 0.05354 0.02176 0.01240 0.02743 AFIX 43 H23 2 -0.071112 1.170444 0.778621 11.00000 -1.20000 AFIX 0 C24 1 -0.145146 1.102784 0.697745 11.00000 0.05490 0.05549 = 0.05181 0.02250 0.02043 0.03023 AFIX 43 H24 2 -0.082661 1.133196 0.682887 11.00000 -1.20000 AFIX 0 C25 1 -0.221954 1.043194 0.650559 11.00000 0.06054 0.06166 = 0.04552 0.02110 0.01878 0.03666 AFIX 43 H25 2 -0.198798 1.043103 0.611600 11.00000 -1.20000 AFIX 0 C26 1 -0.327375 0.982235 0.647150 11.00000 0.04884 0.07023 = 0.04304 0.01350 0.00921 0.04012 AFIX 43 H26 2 -0.356311 0.949904 0.606773 11.00000 -1.20000 AFIX 0 C27 1 -0.522854 0.791372 0.585875 11.00000 0.04086 0.13741 = 0.06402 -0.01817 -0.00448 0.04297 AFIX 13 H27 2 -0.480233 0.830840 0.559527 11.00000 -1.20000 AFIX 0 C28 1 -0.458706 0.720915 0.601031 11.00000 0.04367 0.10503 = 0.09607 -0.03618 -0.00858 0.02522 AFIX 33 H28A 2 -0.390460 0.754417 0.626686 11.00000 -1.50000 H28B 2 -0.499130 0.674841 0.623303 11.00000 -1.50000 H28C 2 -0.444796 0.687648 0.562964 11.00000 -1.50000 AFIX 0 C29 1 -0.632913 0.748977 0.545523 11.00000 0.06835 0.20318 = 0.11324 -0.06806 -0.02998 0.06199 AFIX 33 H29A 2 -0.668355 0.800001 0.538212 11.00000 -1.50000 H29B 2 -0.623018 0.716388 0.506180 11.00000 -1.50000 H29C 2 -0.677351 0.703582 0.566518 11.00000 -1.50000 AFIX 0 C30 1 -0.603421 0.822980 0.712704 11.00000 0.08908 0.09538 = 0.04544 0.00034 0.00779 0.00039 AFIX 13 H30 2 -0.600166 0.876621 0.745996 11.00000 -1.20000 AFIX 0 C31 1 -0.726899 0.779760 0.688622 11.00000 0.10056 0.14124 = 0.08216 0.01334 0.00644 -0.00852 AFIX 33 H31A 2 -0.756904 0.826199 0.668635 11.00000 -1.50000 H31B 2 -0.736288 0.721964 0.659016 11.00000 -1.50000 H31C 2 -0.764045 0.764326 0.723288 11.00000 -1.50000 AFIX 0 C32 1 -0.553820 0.754279 0.743742 11.00000 0.16057 0.12367 = 0.07328 0.01667 0.00004 0.03185 AFIX 33 H32A 2 -0.477487 0.783063 0.758116 11.00000 -1.50000 H32B 2 -0.589664 0.738629 0.778829 11.00000 -1.50000 H32C 2 -0.561907 0.696267 0.714557 11.00000 -1.50000 AFIX 0 C33 1 -0.617838 0.954549 0.620724 11.00000 0.03145 0.10443 = 0.09350 0.03686 0.00388 0.02784 AFIX 13 H33 2 -0.688852 0.912307 0.601016 11.00000 -1.20000 AFIX 0 C34 1 -0.637350 1.027909 0.672475 11.00000 0.04016 0.09690 = 0.12928 0.02403 -0.00003 0.03437 AFIX 33 H34A 2 -0.667694 0.994553 0.704335 11.00000 -1.50000 H34B 2 -0.569186 1.072801 0.690510 11.00000 -1.50000 H34C 2 -0.687441 1.062506 0.655121 11.00000 -1.50000 AFIX 0 C35 1 -0.570491 1.011606 0.572661 11.00000 0.06625 0.14666 = 0.12268 0.07232 0.00825 0.03857 AFIX 33 H35A 2 -0.556830 0.968144 0.539034 11.00000 -1.50000 H35B 2 -0.621353 1.046381 0.556457 11.00000 -1.50000 H35C 2 -0.503099 1.056675 0.591846 11.00000 -1.50000 AFIX 0 C36 1 -0.071011 1.295810 0.884370 11.00000 0.11358 0.08519 = 0.05835 0.00243 0.00020 0.03345 AFIX 13 H36 2 -0.003835 1.294529 0.866786 11.00000 -1.20000 AFIX 0 C37 1 -0.135178 1.344837 0.840810 11.00000 0.23242 0.12224 = 0.09715 -0.00230 -0.04182 0.08654 AFIX 33 H37A 2 -0.159349 1.303812 0.800925 11.00000 -1.50000 H37B 2 -0.197524 1.356431 0.858549 11.00000 -1.50000 H37C 2 -0.089396 1.405391 0.835304 11.00000 -1.50000 AFIX 0 C38 1 -0.033910 1.363227 0.947347 11.00000 0.12605 0.11337 = 0.07137 -0.01568 -0.00941 0.05902 AFIX 33 H38A 2 0.007106 1.333542 0.975844 11.00000 -1.50000 H38B 2 0.011273 1.423677 0.941212 11.00000 -1.50000 H38C 2 -0.096855 1.374717 0.964457 11.00000 -1.50000 AFIX 0 C39 1 -0.011521 1.106064 0.901852 11.00000 0.10232 0.09008 = 0.10546 0.02743 -0.01787 0.01593 AFIX 13 H39 2 0.012345 1.097824 0.860816 11.00000 -1.20000 AFIX 0 C40 1 -0.043859 1.006621 0.915481 11.00000 0.16652 0.11355 = 0.14400 0.04011 -0.02859 0.01774 AFIX 33 H40A 2 -0.108567 0.971597 0.887145 11.00000 -1.50000 H40B 2 0.014288 0.974961 0.910386 11.00000 -1.50000 H40C 2 -0.058424 1.008334 0.957817 11.00000 -1.50000 AFIX 0 C41 1 0.079989 1.160136 0.940384 11.00000 0.10042 0.13089 = 0.16002 0.01963 -0.02646 0.03743 AFIX 33 H41A 2 0.097630 1.224202 0.929620 11.00000 -1.50000 H41B 2 0.067102 1.163869 0.983079 11.00000 -1.50000 H41C 2 0.139814 1.130496 0.935647 11.00000 -1.50000 AFIX 0 C42 1 -0.228159 1.139019 0.941404 11.00000 0.12264 0.15343 = 0.10074 0.00444 0.03595 0.01974 AFIX 13 H42 2 -0.260571 1.069489 0.928672 11.00000 -1.20000 AFIX 0 C43 1 -0.160202 1.146891 1.010258 11.00000 0.14022 0.19002 = 0.09644 0.01475 0.03010 -0.01027 AFIX 137 H43A 2 -0.194401 1.094577 1.030309 11.00000 -1.50000 H43B 2 -0.159144 1.207560 1.034837 11.00000 -1.50000 H43C 2 -0.086593 1.143225 1.006630 11.00000 -1.50000 AFIX 0 C44 1 -0.311467 1.176693 0.942667 11.00000 0.12691 0.19958 = 0.10250 -0.07805 0.01610 0.04753 AFIX 33 H44A 2 -0.349264 1.170333 0.900784 11.00000 -1.50000 H44B 2 -0.360118 1.143660 0.967863 11.00000 -1.50000 H44C 2 -0.286883 1.244063 0.960293 11.00000 -1.50000 AFIX 0 C45 1 -0.249811 0.518286 0.664510 11.00000 0.06416 0.03436 = 0.04690 0.00850 -0.00812 -0.00546 C46 1 -0.267039 0.565981 0.613776 11.00000 0.04958 0.04393 = 0.05153 0.01070 -0.00627 -0.00478 AFIX 43 H46 2 -0.341370 0.556047 0.599265 11.00000 -1.20000 AFIX 0 C47 1 -0.204412 0.624195 0.578777 11.00000 0.04449 0.03906 = 0.04544 0.01098 -0.00663 0.00030 AFIX 43 H47 2 -0.247527 0.640524 0.545986 11.00000 -1.20000 AFIX 0 C48 1 -0.092682 0.664981 0.579945 11.00000 0.04015 0.03057 = 0.04628 0.00942 -0.00575 -0.00106 C49 1 -0.000755 0.654446 0.619175 11.00000 0.04296 0.02917 = 0.04642 0.01039 -0.00965 0.00696 AFIX 43 H49 2 0.064254 0.686961 0.607759 11.00000 -1.20000 AFIX 0 C50 1 0.018365 0.608552 0.670153 11.00000 0.04877 0.03082 = 0.04614 0.00945 -0.00964 0.00982 AFIX 43 H50 2 0.092553 0.619569 0.685427 11.00000 -1.20000 AFIX 0 C51 1 -0.045637 0.551079 0.703282 11.00000 0.06394 0.03793 = 0.04521 0.01317 -0.00853 0.00334 AFIX 43 H51 2 -0.004418 0.530245 0.734815 11.00000 -1.20000 AFIX 0 C52 1 -0.155534 0.516277 0.701783 11.00000 0.07066 0.03460 = 0.04843 0.00710 -0.00718 0.00491 AFIX 43 H52 2 -0.170092 0.482254 0.734801 11.00000 -1.20000 AFIX 0 C53 1 -0.496721 0.441405 0.638174 11.00000 0.06937 0.08765 = 0.06827 0.02531 -0.00266 -0.02680 AFIX 13 H53 2 -0.496618 0.509289 0.636044 11.00000 -1.20000 AFIX 0 C54 1 -0.597800 0.396777 0.663501 11.00000 0.08256 0.11655 = 0.08869 0.03893 0.00076 -0.02843 AFIX 33 H54A 2 -0.594304 0.427949 0.705604 11.00000 -1.50000 H54B 2 -0.661107 0.404875 0.637707 11.00000 -1.50000 H54C 2 -0.602665 0.328952 0.663398 11.00000 -1.50000 AFIX 0 C55 1 -0.504801 0.390556 0.571612 11.00000 0.10367 0.10353 = 0.07758 0.01547 -0.00320 -0.04211 AFIX 33 H55A 2 -0.440754 0.418110 0.554515 11.00000 -1.50000 H55B 2 -0.510155 0.322760 0.571986 11.00000 -1.50000 H55C 2 -0.568597 0.398683 0.546296 11.00000 -1.50000 AFIX 0 C56 1 -0.373780 0.484374 0.769548 11.00000 0.08247 0.12789 = 0.06769 0.02740 -0.00389 0.03673 AFIX 13 H56 2 -0.296454 0.506801 0.788134 11.00000 -1.20000 AFIX 0 C57 1 -0.414594 0.575300 0.772663 11.00000 0.06277 0.11193 = 0.08843 -0.00281 -0.01158 0.01084 AFIX 33 H57A 2 -0.381132 0.615441 0.744685 11.00000 -1.50000 H57B 2 -0.492608 0.558613 0.760581 11.00000 -1.50000 H57C 2 -0.396090 0.609877 0.814709 11.00000 -1.50000 AFIX 0 C58 1 -0.420512 0.422092 0.809999 11.00000 0.11052 0.18498 = 0.13901 0.09309 0.02502 0.06166 AFIX 33 H58A 2 -0.392499 0.365100 0.806660 11.00000 -1.50000 H58B 2 -0.402096 0.455115 0.852440 11.00000 -1.50000 H58C 2 -0.498613 0.403851 0.798312 11.00000 -1.50000 AFIX 0 C59 1 -0.330329 0.314422 0.687199 11.00000 0.11971 0.05536 = 0.13078 0.02817 0.01529 -0.00043 AFIX 13 H59 2 -0.273942 0.322121 0.723726 11.00000 -1.20000 AFIX 0 C60 1 -0.423985 0.239845 0.695574 11.00000 0.15932 0.06912 = 0.21324 0.05354 0.04393 -0.00211 AFIX 33 H60A 2 -0.452730 0.261309 0.732112 11.00000 -1.50000 H60B 2 -0.479491 0.227761 0.659401 11.00000 -1.50000 H60C 2 -0.401488 0.181294 0.700733 11.00000 -1.50000 AFIX 0 C61 1 -0.287828 0.286638 0.636202 11.00000 0.16364 0.05182 = 0.15489 0.02740 0.03120 0.01128 AFIX 33 H61A 2 -0.226340 0.336909 0.631706 11.00000 -1.50000 H61B 2 -0.264434 0.228372 0.640952 11.00000 -1.50000 H61C 2 -0.342436 0.274839 0.599621 11.00000 -1.50000 AFIX 0 C62 1 -0.025017 0.653117 0.451444 11.00000 0.06313 0.04546 = 0.03954 0.01129 -0.00751 0.02178 AFIX 13 H62 2 -0.010699 0.689495 0.416824 11.00000 -1.20000 AFIX 0 C63 1 -0.122607 0.569643 0.427669 11.00000 0.06428 0.04204 = 0.07580 -0.00527 -0.01959 0.02236 AFIX 33 H63A 2 -0.185313 0.594011 0.415523 11.00000 -1.50000 H63B 2 -0.108099 0.530566 0.392106 11.00000 -1.50000 H63C 2 -0.136735 0.531042 0.460193 11.00000 -1.50000 AFIX 0 C64 1 0.075613 0.617795 0.471087 11.00000 0.06216 0.05142 = 0.06925 0.00779 -0.00230 0.02254 AFIX 33 H64A 2 0.136612 0.672390 0.486045 11.00000 -1.50000 H64B 2 0.062777 0.579509 0.503894 11.00000 -1.50000 H64C 2 0.091412 0.579033 0.435807 11.00000 -1.50000 AFIX 0 C65 1 -0.181025 0.773332 0.480135 11.00000 0.03888 0.03912 = 0.05091 0.01508 0.00032 0.00821 AFIX 13 H65 2 -0.240272 0.714295 0.469074 11.00000 -1.20000 AFIX 0 C66 1 -0.220784 0.842554 0.524578 11.00000 0.04318 0.06284 = 0.04995 0.01887 0.00186 0.02206 AFIX 33 H66A 2 -0.229813 0.816606 0.562762 11.00000 -1.50000 H66B 2 -0.168168 0.903993 0.533675 11.00000 -1.50000 H66C 2 -0.289624 0.851030 0.505526 11.00000 -1.50000 AFIX 0 C67 1 -0.166943 0.813812 0.420577 11.00000 0.05113 0.04140 = 0.05528 0.01712 -0.00383 0.01422 AFIX 33 H67A 2 -0.141689 0.769848 0.392346 11.00000 -1.50000 H67B 2 -0.235784 0.822289 0.401527 11.00000 -1.50000 H67C 2 -0.114327 0.875252 0.429676 11.00000 -1.50000 AFIX 0 C68 1 0.065325 0.836228 0.544906 11.00000 0.03432 0.03507 = 0.04610 0.00950 0.00480 0.01131 AFIX 13 H68 2 0.122912 0.806012 0.560868 11.00000 -1.20000 AFIX 0 C69 1 0.108687 0.891218 0.495248 11.00000 0.04895 0.05376 = 0.04764 0.01732 -0.00114 0.00478 AFIX 33 H69A 2 0.117190 0.846498 0.460667 11.00000 -1.50000 H69B 2 0.058307 0.927762 0.480978 11.00000 -1.50000 H69C 2 0.178305 0.934576 0.512328 11.00000 -1.50000 AFIX 0 C70 1 0.051813 0.906659 0.599575 11.00000 0.04455 0.03495 = 0.05313 0.00275 0.00816 0.00379 AFIX 33 H70A 2 0.024070 0.871353 0.631292 11.00000 -1.50000 H70B 2 0.121404 0.950024 0.616703 11.00000 -1.50000 H70C 2 0.001407 0.943210 0.585354 11.00000 -1.50000 AFIX 0 N1 3 0.148346 0.945263 0.794862 11.00000 0.01949 0.04362 = 0.05196 -0.00073 0.00088 0.00833 N2 3 -0.224590 0.737663 0.884955 11.00000 0.03577 0.06135 = 0.05936 0.02717 -0.00141 -0.00856 O1 4 -0.201694 0.811911 0.687547 11.00000 0.02673 0.04786 = 0.05309 0.01350 -0.00286 0.00551 O2 4 0.019992 0.816618 0.746499 11.00000 0.02961 0.03125 = 0.06336 0.00395 -0.00901 0.00820 O3 4 -0.018863 0.958627 0.760041 11.00000 0.02110 0.03893 = 0.04813 0.00817 0.00047 0.00921 O4 4 -0.163456 0.717151 0.795143 11.00000 0.05433 0.03898 = 0.05204 0.01637 -0.00363 0.00174 O5 4 -0.222265 0.844902 0.819312 11.00000 0.06263 0.08059 = 0.07300 0.04273 0.03562 0.03830 SI1 5 -0.533175 0.879186 0.652770 11.00000 0.03790 0.09425 = 0.03964 0.01238 0.00309 0.03530 SI2 5 -0.135761 1.168942 0.886957 11.00000 0.03529 0.11572 = 0.04825 0.01889 -0.00411 0.00893 SI3 5 -0.371090 0.439660 0.687220 11.00000 0.08841 0.04093 = 0.06792 0.01832 0.01187 -0.01496 SI4 5 -0.057601 0.735552 0.515106 11.00000 0.03721 0.03171 = 0.04356 0.00965 -0.00250 0.00893 U1 6 -0.205292 0.939985 0.739845 11.00000 0.02189 0.05484 = 0.04793 0.02122 0.00793 0.01615 U2 6 -0.130195 0.699394 0.694205 11.00000 0.03332 0.03354 = 0.04579 0.01339 -0.00759 -0.00036 HKLF 4 REM 2013ncs0533 in P -1 REM R1 = 0.0703 for 11223 Fo > 4sig(Fo) and 0.1155 for all 18150 data REM 750 parameters refined using 1119 restraints END WGHT 0.1107 0.0000 REM Instructions for potential hydrogen bonds HTAB C9 O3 HTAB C15 O4 HTAB C18 O5 REM Highest difference peak 4.017, deepest hole -2.642, 1-sigma level 0.194 Q1 1 -0.1189 0.7050 0.7398 11.00000 0.05 4.02 Q2 1 -0.1487 0.6942 0.6479 11.00000 0.05 3.63 Q3 1 -0.2218 0.9387 0.6963 11.00000 0.05 3.50 Q4 1 -0.1942 0.9491 0.7879 11.00000 0.05 3.35 Q5 1 -0.0565 1.1189 0.9361 11.00000 0.05 2.25 ; _shelx_res_checksum 90934 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C1 C 0.0450(6) 0.9047(6) 0.7655(4) 0.0345(18) Uani 1 1 d . U C2 C 0.2143(7) 0.8993(7) 0.8281(5) 0.047(2) Uani 1 1 d . U C3 C 0.3097(7) 0.9641(8) 0.8488(5) 0.047(2) Uani 1 1 d . U C4 C 0.3047(7) 1.0488(8) 0.8281(5) 0.054(2) Uani 1 1 d . U C5 C 0.2039(7) 1.0396(7) 0.7951(5) 0.044(2) Uani 1 1 d . U C6 C 0.1762(10) 0.8014(8) 0.8409(6) 0.071(3) Uani 1 1 d . U H6A H 0.2337 0.7842 0.8666 0.106 Uiso 1 1 calc GR U H6B H 0.1555 0.7572 0.8021 0.106 Uiso 1 1 calc GR U H6C H 0.1141 0.7979 0.8624 0.106 Uiso 1 1 calc GR U C7 C 0.4051(9) 0.9445(10) 0.8884(6) 0.071(3) Uani 1 1 d . U H7A H 0.4640 1.0019 0.8973 0.107 Uiso 1 1 calc R U H7B H 0.3837 0.9264 0.9269 0.107 Uiso 1 1 calc R U H7C H 0.4287 0.8927 0.8662 0.107 Uiso 1 1 calc R U C8 C 0.3963(11) 1.1349(11) 0.8378(8) 0.096(5) Uani 1 1 d . U H8A H 0.4583 1.1229 0.8627 0.144 Uiso 1 1 calc R U H8B H 0.4151 1.1492 0.7980 0.144 Uiso 1 1 calc R U H8C H 0.3755 1.1891 0.8592 0.144 Uiso 1 1 calc R U C9 C 0.1632(9) 1.1058(8) 0.7590(6) 0.063(3) Uani 1 1 d . U H9A H 0.0880 1.0779 0.7413 0.094 Uiso 1 1 calc R U H9B H 0.1690 1.1658 0.7858 0.094 Uiso 1 1 calc R U H9C H 0.2057 1.1179 0.7259 0.094 Uiso 1 1 calc R U C10 C -0.2027(8) 0.7689(8) 0.8306(5) 0.049(2) Uani 1 1 d . U C11 C -0.1949(10) 0.6581(8) 0.9051(5) 0.060(2) Uani 1 1 d . U C12 C -0.2513(12) 0.6360(11) 0.9521(7) 0.083(3) Uani 1 1 d . U C13 C -0.3114(14) 0.7034(13) 0.9614(8) 0.103(4) Uani 1 1 d . U C14 C -0.2965(11) 0.7686(12) 0.9218(7) 0.084(4) Uani 1 1 d . U C15 C -0.1124(11) 0.6166(9) 0.8846(5) 0.070(3) Uani 1 1 d . U H15A H -0.0865 0.6463 0.8503 0.105 Uiso 1 1 calc R U H15B H -0.0528 0.6268 0.9184 0.105 Uiso 1 1 calc R U H15C H -0.1414 0.5483 0.8711 0.105 Uiso 1 1 calc R U C16 C -0.2431(14) 0.5603(12) 0.9909(8) 0.107(5) Uani 1 1 d . U H16A H -0.2927 0.5606 1.0208 0.160 Uiso 1 1 calc R U H16B H -0.2616 0.4982 0.9647 0.160 Uiso 1 1 calc R U H16C H -0.1697 0.5726 1.0126 0.160 Uiso 1 1 calc R U C17 C -0.3805(18) 0.7120(18) 1.0134(9) 0.151(7) Uani 1 1 d . U H17A H -0.3813 0.6590 1.0365 0.226 Uiso 1 1 calc R U H17B H -0.3497 0.7721 1.0411 0.226 Uiso 1 1 calc R U H17C H -0.4538 0.7104 0.9953 0.226 Uiso 1 1 calc R U C18 C -0.3437(14) 0.8472(14) 0.9116(8) 0.106(5) Uani 1 1 d . U H18A H -0.3128 0.8783 0.8791 0.159 Uiso 1 1 calc R U H18B H -0.4214 0.8235 0.8993 0.159 Uiso 1 1 calc R U H18C H -0.3290 0.8930 0.9496 0.159 Uiso 1 1 calc R U C19 C -0.3977(8) 0.9594(8) 0.6900(5) 0.048(2) Uani 1 1 d . U C20 C -0.3858(8) 0.9908(8) 0.7534(5) 0.053(2) Uani 1 1 d . U H20 H -0.4503 0.9662 0.7684 0.063 Uiso 1 1 calc R U C21 C -0.3075(8) 1.0482(8) 0.8025(5) 0.052(2) Uani 1 1 d . U H21 H -0.3302 1.0453 0.8414 0.062 Uiso 1 1 calc R U C22 C -0.2033(8) 1.1086(8) 0.8065(5) 0.051(2) Uani 1 1 d . U C23 C -0.1382(8) 1.1283(8) 0.7614(5) 0.048(2) Uani 1 1 d . U H23 H -0.0711 1.1704 0.7786 0.058 Uiso 1 1 calc R U C24 C -0.1451(9) 1.1028(7) 0.6977(5) 0.049(2) Uani 1 1 d . U H24 H -0.0827 1.1332 0.6829 0.059 Uiso 1 1 calc R U C25 C -0.2220(9) 1.0432(8) 0.6506(5) 0.050(2) Uani 1 1 d . U H25 H -0.1988 1.0431 0.6116 0.060 Uiso 1 1 calc R U C26 C -0.3274(8) 0.9822(8) 0.6472(5) 0.049(2) Uani 1 1 d . U H26 H -0.3563 0.9499 0.6068 0.059 Uiso 1 1 calc R U C27 C -0.5229(10) 0.7914(12) 0.5859(6) 0.081(4) Uani 1 1 d . U H27 H -0.4802 0.8308 0.5595 0.098 Uiso 1 1 calc R U C28 C -0.4587(10) 0.7209(11) 0.6010(7) 0.087(4) Uani 1 1 d . U H28A H -0.3905 0.7544 0.6267 0.130 Uiso 1 1 calc R U H28B H -0.4991 0.6748 0.6233 0.130 Uiso 1 1 calc R U H28C H -0.4448 0.6876 0.5630 0.130 Uiso 1 1 calc R U C29 C -0.6329(13) 0.7490(16) 0.5455(9) 0.135(7) Uani 1 1 d . U H29A H -0.6684 0.8000 0.5382 0.203 Uiso 1 1 calc R U H29B H -0.6230 0.7164 0.5062 0.203 Uiso 1 1 calc R U H29C H -0.6774 0.7036 0.5665 0.203 Uiso 1 1 calc R U C30 C -0.6034(12) 0.8230(11) 0.7127(6) 0.081(3) Uani 1 1 d . U H30 H -0.6002 0.8766 0.7460 0.098 Uiso 1 1 calc R U C31 C -0.7269(14) 0.7798(14) 0.6886(8) 0.115(5) Uani 1 1 d . U H31A H -0.7569 0.8262 0.6686 0.173 Uiso 1 1 calc R U H31B H -0.7363 0.7220 0.6590 0.173 Uiso 1 1 calc R U H31C H -0.7640 0.7643 0.7233 0.173 Uiso 1 1 calc R U C32 C -0.5538(17) 0.7543(14) 0.7437(8) 0.121(6) Uani 1 1 d . U H32A H -0.4775 0.7831 0.7581 0.182 Uiso 1 1 calc R U H32B H -0.5897 0.7386 0.7788 0.182 Uiso 1 1 calc R U H32C H -0.5619 0.6963 0.7146 0.182 Uiso 1 1 calc R U C33 C -0.6178(9) 0.9545(10) 0.6207(6) 0.073(3) Uani 1 1 d . U H33 H -0.6889 0.9123 0.6010 0.088 Uiso 1 1 calc R U C34 C -0.6374(10) 1.0279(10) 0.6725(7) 0.087(4) Uani 1 1 d . U H34A H -0.6677 0.9946 0.7043 0.130 Uiso 1 1 calc R U H34B H -0.5692 1.0728 0.6905 0.130 Uiso 1 1 calc R U H34C H -0.6874 1.0625 0.6551 0.130 Uiso 1 1 calc R U C35 C -0.5705(12) 1.0116(13) 0.5727(8) 0.106(5) Uani 1 1 d . U H35A H -0.5568 0.9681 0.5390 0.159 Uiso 1 1 calc R U H35B H -0.6214 1.0464 0.5565 0.159 Uiso 1 1 calc R U H35C H -0.5031 1.0567 0.5918 0.159 Uiso 1 1 calc R U C36 C -0.0710(14) 1.2958(10) 0.8844(6) 0.086(4) Uani 1 1 d . U H36 H -0.0038 1.2945 0.8668 0.103 Uiso 1 1 calc R U C37 C -0.135(2) 1.3448(14) 0.8408(9) 0.151(7) Uani 1 1 d . U H37A H -0.1593 1.3038 0.8009 0.227 Uiso 1 1 calc R U H37B H -0.1975 1.3564 0.8585 0.227 Uiso 1 1 calc R U H37C H -0.0894 1.4054 0.8353 0.227 Uiso 1 1 calc R U C38 C -0.0339(15) 1.3632(12) 0.9473(7) 0.104(5) Uani 1 1 d . U H38A H 0.0071 1.3335 0.9758 0.155 Uiso 1 1 calc R U H38B H 0.0113 1.4237 0.9412 0.155 Uiso 1 1 calc R U H38C H -0.0969 1.3747 0.9645 0.155 Uiso 1 1 calc R U C39 C -0.0115(15) 1.1061(12) 0.9019(9) 0.102(4) Uani 1 1 d . U H39 H 0.0123 1.0978 0.8608 0.123 Uiso 1 1 calc R U C40 C -0.0439(19) 1.0066(14) 0.9155(10) 0.147(8) Uani 1 1 d . U H40A H -0.1086 0.9716 0.8871 0.220 Uiso 1 1 calc R U H40B H 0.0143 0.9750 0.9104 0.220 Uiso 1 1 calc R U H40C H -0.0584 1.0083 0.9578 0.220 Uiso 1 1 calc R U C41 C 0.0800(16) 1.1601(15) 0.9404(10) 0.133(7) Uani 1 1 d . U H41A H 0.0976 1.2242 0.9296 0.200 Uiso 1 1 calc R U H41B H 0.0671 1.1639 0.9831 0.200 Uiso 1 1 calc R U H41C H 0.1398 1.1305 0.9356 0.200 Uiso 1 1 calc R U C42 C -0.2282(17) 1.1390(17) 0.9414(9) 0.128(5) Uani 1 1 d . U H42 H -0.2606 1.0695 0.9287 0.153 Uiso 1 1 calc R U C43 C -0.1602(18) 1.1469(17) 1.0103(9) 0.150(7) Uani 1 1 d . U H43A H -0.1944 1.0946 1.0303 0.225 Uiso 1 1 calc GR U H43B H -0.1591 1.2076 1.0348 0.225 Uiso 1 1 calc GR U H43C H -0.0866 1.1432 1.0066 0.225 Uiso 1 1 calc GR U C44 C -0.3115(17) 1.1767(17) 0.9427(9) 0.151(7) Uani 1 1 d . U H44A H -0.3493 1.1703 0.9008 0.226 Uiso 1 1 calc R U H44B H -0.3601 1.1437 0.9679 0.226 Uiso 1 1 calc R U H44C H -0.2869 1.2441 0.9603 0.226 Uiso 1 1 calc R U C45 C -0.2498(9) 0.5183(7) 0.6645(5) 0.053(2) Uani 1 1 d . U C46 C -0.2670(9) 0.5660(7) 0.6138(5) 0.052(2) Uani 1 1 d . U H46 H -0.3414 0.5560 0.5993 0.062 Uiso 1 1 calc R U C47 C -0.2044(8) 0.6242(7) 0.5788(5) 0.045(2) Uani 1 1 d . U H47 H -0.2475 0.6405 0.5460 0.054 Uiso 1 1 calc R U C48 C -0.0927(8) 0.6650(6) 0.5799(5) 0.0413(18) Uani 1 1 d . U C49 C -0.0008(8) 0.6544(6) 0.6192(4) 0.0409(19) Uani 1 1 d . U H49 H 0.0643 0.6870 0.6078 0.049 Uiso 1 1 calc R U C50 C 0.0184(8) 0.6086(6) 0.6702(4) 0.0431(19) Uani 1 1 d . U H50 H 0.0926 0.6196 0.6854 0.052 Uiso 1 1 calc R U C51 C -0.0456(9) 0.5511(7) 0.7033(5) 0.051(2) Uani 1 1 d . U H51 H -0.0044 0.5302 0.7348 0.062 Uiso 1 1 calc R U C52 C -0.1555(9) 0.5163(7) 0.7018(5) 0.054(2) Uani 1 1 d . U H52 H -0.1701 0.4823 0.7348 0.065 Uiso 1 1 calc R U C53 C -0.4967(11) 0.4414(11) 0.6382(6) 0.083(4) Uani 1 1 d . U H53 H -0.4966 0.5093 0.6360 0.099 Uiso 1 1 calc R U C54 C -0.5978(13) 0.3968(12) 0.6635(7) 0.104(5) Uani 1 1 d . U H54A H -0.5943 0.4279 0.7056 0.155 Uiso 1 1 calc R U H54B H -0.6611 0.4049 0.6377 0.155 Uiso 1 1 calc R U H54C H -0.6027 0.3290 0.6634 0.155 Uiso 1 1 calc R U C55 C -0.5048(14) 0.3906(12) 0.5716(7) 0.107(5) Uani 1 1 d . U H55A H -0.4408 0.4181 0.5545 0.161 Uiso 1 1 calc R U H55B H -0.5102 0.3228 0.5720 0.161 Uiso 1 1 calc R U H55C H -0.5686 0.3987 0.5463 0.161 Uiso 1 1 calc R U C56 C -0.3738(13) 0.4844(13) 0.7695(7) 0.091(4) Uani 1 1 d . U H56 H -0.2965 0.5068 0.7881 0.109 Uiso 1 1 calc R U C57 C -0.4146(12) 0.5753(12) 0.7727(7) 0.093(4) Uani 1 1 d . U H57A H -0.3811 0.6154 0.7447 0.140 Uiso 1 1 calc R U H57B H -0.4926 0.5586 0.7606 0.140 Uiso 1 1 calc R U H57C H -0.3961 0.6099 0.8147 0.140 Uiso 1 1 calc R U C58 C -0.4205(16) 0.4221(16) 0.8100(9) 0.134(6) Uani 1 1 d . U H58A H -0.3925 0.3651 0.8067 0.201 Uiso 1 1 calc R U H58B H -0.4021 0.4551 0.8524 0.201 Uiso 1 1 calc R U H58C H -0.4986 0.4039 0.7983 0.201 Uiso 1 1 calc R U C59 C -0.3303(16) 0.3144(10) 0.6872(9) 0.105(5) Uani 1 1 d . U H59 H -0.2739 0.3221 0.7237 0.126 Uiso 1 1 calc R U C60 C -0.4240(18) 0.2398(12) 0.6956(11) 0.148(8) Uani 1 1 d . U H60A H -0.4527 0.2613 0.7321 0.222 Uiso 1 1 calc R U H60B H -0.4795 0.2278 0.6594 0.222 Uiso 1 1 calc R U H60C H -0.4015 0.1813 0.7007 0.222 Uiso 1 1 calc R U C61 C -0.2878(18) 0.2866(11) 0.6362(10) 0.124(6) Uani 1 1 d . U H61A H -0.2263 0.3369 0.6317 0.186 Uiso 1 1 calc R U H61B H -0.2644 0.2284 0.6410 0.186 Uiso 1 1 calc R U H61C H -0.3424 0.2748 0.5996 0.186 Uiso 1 1 calc R U C62 C -0.0250(9) 0.6531(7) 0.4514(5) 0.049(2) Uani 1 1 d . U H62 H -0.0107 0.6895 0.4168 0.059 Uiso 1 1 calc R U C63 C -0.1226(10) 0.5696(7) 0.4277(6) 0.063(3) Uani 1 1 d . U H63A H -0.1853 0.5940 0.4155 0.095 Uiso 1 1 calc R U H63B H -0.1081 0.5306 0.3921 0.095 Uiso 1 1 calc R U H63C H -0.1367 0.5310 0.4602 0.095 Uiso 1 1 calc R U C64 C 0.0756(10) 0.6178(8) 0.4711(6) 0.061(3) Uani 1 1 d . U H64A H 0.1366 0.6724 0.4860 0.091 Uiso 1 1 calc R U H64B H 0.0628 0.5795 0.5039 0.091 Uiso 1 1 calc R U H64C H 0.0914 0.5790 0.4358 0.091 Uiso 1 1 calc R U C65 C -0.1810(8) 0.7733(7) 0.4801(5) 0.043(2) Uani 1 1 d . U H65 H -0.2403 0.7143 0.4691 0.052 Uiso 1 1 calc R U C66 C -0.2208(8) 0.8426(8) 0.5246(5) 0.050(2) Uani 1 1 d . U H66A H -0.2298 0.8166 0.5628 0.075 Uiso 1 1 calc R U H66B H -0.1682 0.9040 0.5337 0.075 Uiso 1 1 calc R U H66C H -0.2896 0.8510 0.5055 0.075 Uiso 1 1 calc R U C67 C -0.1669(9) 0.8138(7) 0.4206(5) 0.049(2) Uani 1 1 d . U H67A H -0.1417 0.7698 0.3923 0.074 Uiso 1 1 calc R U H67B H -0.2358 0.8223 0.4015 0.074 Uiso 1 1 calc R U H67C H -0.1143 0.8753 0.4297 0.074 Uiso 1 1 calc R U C68 C 0.0653(7) 0.8362(6) 0.5449(4) 0.0379(19) Uani 1 1 d . U H68 H 0.1229 0.8060 0.5609 0.045 Uiso 1 1 calc R U C69 C 0.1087(9) 0.8912(8) 0.4952(5) 0.051(2) Uani 1 1 d . U H69A H 0.1172 0.8465 0.4607 0.077 Uiso 1 1 calc R U H69B H 0.0583 0.9278 0.4810 0.077 Uiso 1 1 calc R U H69C H 0.1783 0.9346 0.5123 0.077 Uiso 1 1 calc R U C70 C 0.0518(8) 0.9067(7) 0.5996(5) 0.045(2) Uani 1 1 d . U H70A H 0.0241 0.8714 0.6313 0.068 Uiso 1 1 calc R U H70B H 0.1214 0.9500 0.6167 0.068 Uiso 1 1 calc R U H70C H 0.0014 0.9432 0.5854 0.068 Uiso 1 1 calc R U N1 N 0.1483(5) 0.9453(5) 0.7949(4) 0.0394(16) Uani 1 1 d . U N2 N -0.2246(7) 0.7377(6) 0.8850(4) 0.0547(19) Uani 1 1 d . U O1 O -0.2017(5) 0.8119(5) 0.6875(3) 0.0434(14) Uani 1 1 d . U O2 O 0.0200(5) 0.8166(4) 0.7465(3) 0.0430(15) Uani 1 1 d . U O3 O -0.0189(4) 0.9586(4) 0.7600(3) 0.0361(13) Uani 1 1 d . U O4 O -0.1635(6) 0.7172(5) 0.7951(3) 0.0502(16) Uani 1 1 d . U O5 O -0.2223(6) 0.8449(6) 0.8193(4) 0.064(2) Uani 1 1 d . U Si1 Si -0.5332(2) 0.8792(3) 0.65277(13) 0.0542(8) Uani 1 1 d . U Si2 Si -0.1358(3) 1.1689(3) 0.88696(15) 0.0683(10) Uani 1 1 d . U Si3 Si -0.3711(3) 0.4397(2) 0.68722(17) 0.0699(10) Uani 1 1 d . U Si4 Si -0.0576(2) 0.73555(17) 0.51511(12) 0.0378(6) Uani 1 1 d . U U1 U -0.20529(3) 0.93998(3) 0.73985(2) 0.03909(12) Uani 1 1 d . U U2 U -0.13019(3) 0.69939(2) 0.69420(2) 0.03949(12) Uani 1 1 d . U 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 C1 0.021(3) 0.038(3) 0.043(5) 0.008(3) 0.000(3) 0.006(3) C2 0.025(4) 0.054(4) 0.059(6) 0.004(4) -0.003(3) 0.012(3) C3 0.022(3) 0.070(5) 0.042(5) -0.001(4) 0.003(3) 0.005(3) C4 0.022(4) 0.069(5) 0.063(6) 0.010(4) 0.001(4) -0.003(3) C5 0.027(4) 0.048(4) 0.053(5) 0.001(3) 0.007(3) 0.000(3) C6 0.055(7) 0.059(5) 0.089(9) 0.016(5) -0.025(6) 0.014(4) C7 0.033(5) 0.116(9) 0.060(7) 0.004(6) -0.013(5) 0.021(5) C8 0.049(6) 0.092(8) 0.122(12) 0.026(8) -0.008(7) -0.027(6) C9 0.039(5) 0.050(5) 0.088(8) 0.017(5) 0.002(5) -0.009(4) C10 0.035(5) 0.050(4) 0.058(5) 0.022(3) 0.002(4) -0.001(4) C11 0.065(6) 0.053(5) 0.048(5) 0.020(4) -0.014(4) -0.011(4) C12 0.074(6) 0.098(6) 0.069(6) 0.040(5) 0.001(5) -0.007(5) C13 0.102(7) 0.125(7) 0.090(7) 0.056(5) 0.029(6) 0.018(6) C14 0.065(7) 0.126(8) 0.078(7) 0.052(6) 0.028(6) 0.029(6) C15 0.097(7) 0.061(7) 0.044(6) 0.021(5) -0.012(5) 0.010(6) C16 0.095(10) 0.117(9) 0.096(9) 0.063(8) -0.006(7) -0.015(7) C17 0.146(13) 0.218(15) 0.121(10) 0.085(10) 0.065(10) 0.057(11) C18 0.103(10) 0.161(10) 0.096(10) 0.070(8) 0.058(8) 0.067(9) C19 0.038(4) 0.079(5) 0.040(4) 0.015(3) 0.006(3) 0.037(3) C20 0.036(4) 0.089(6) 0.041(4) 0.013(4) 0.007(3) 0.030(4) C21 0.030(4) 0.093(6) 0.039(4) 0.013(4) 0.004(3) 0.027(4) C22 0.040(4) 0.078(5) 0.047(4) 0.020(3) 0.009(3) 0.032(3) C23 0.041(4) 0.063(5) 0.054(4) 0.022(3) 0.012(3) 0.027(4) C24 0.055(5) 0.055(5) 0.052(4) 0.022(3) 0.020(3) 0.030(4) C25 0.061(5) 0.062(5) 0.046(4) 0.021(4) 0.019(3) 0.037(4) C26 0.049(4) 0.070(5) 0.043(4) 0.013(4) 0.009(3) 0.040(4) C27 0.041(5) 0.137(8) 0.064(6) -0.018(6) -0.004(5) 0.043(6) C28 0.044(6) 0.105(8) 0.096(9) -0.036(6) -0.009(6) 0.025(6) C29 0.068(7) 0.203(13) 0.113(10) -0.068(10) -0.030(7) 0.062(8) C30 0.089(7) 0.095(8) 0.045(6) 0.000(5) 0.008(5) 0.000(6) C31 0.101(8) 0.141(12) 0.082(9) 0.013(9) 0.006(6) -0.009(7) C32 0.161(12) 0.124(10) 0.073(9) 0.017(8) 0.000(8) 0.032(9) C33 0.031(5) 0.104(7) 0.094(7) 0.037(6) 0.004(5) 0.028(5) C34 0.040(6) 0.097(9) 0.129(9) 0.024(7) 0.000(6) 0.034(6) C35 0.066(8) 0.147(11) 0.123(9) 0.072(8) 0.008(7) 0.039(8) C36 0.114(10) 0.085(6) 0.058(7) 0.002(5) 0.000(6) 0.033(6) C37 0.232(16) 0.122(10) 0.097(10) -0.002(8) -0.042(10) 0.087(10) C38 0.126(13) 0.113(10) 0.071(8) -0.016(7) -0.009(8) 0.059(9) C39 0.102(7) 0.090(7) 0.105(8) 0.027(6) -0.018(5) 0.016(5) C40 0.167(16) 0.114(9) 0.144(17) 0.040(9) -0.029(13) 0.018(8) C41 0.100(8) 0.131(10) 0.160(13) 0.020(9) -0.026(8) 0.037(7) C42 0.123(7) 0.153(9) 0.101(7) 0.004(6) 0.036(6) 0.020(6) C43 0.140(11) 0.190(16) 0.096(8) 0.015(8) 0.030(7) -0.010(10) C44 0.127(9) 0.200(14) 0.103(10) -0.078(9) 0.016(7) 0.048(9) C45 0.064(4) 0.034(4) 0.047(5) 0.009(3) -0.008(3) -0.005(3) C46 0.050(5) 0.044(4) 0.052(5) 0.011(4) -0.006(3) -0.005(4) C47 0.044(4) 0.039(4) 0.045(4) 0.011(3) -0.007(3) 0.000(3) C48 0.040(4) 0.031(4) 0.046(4) 0.009(3) -0.006(3) -0.001(3) C49 0.043(4) 0.029(4) 0.046(4) 0.010(3) -0.010(3) 0.007(3) C50 0.049(4) 0.031(4) 0.046(4) 0.009(3) -0.010(3) 0.010(3) C51 0.064(5) 0.038(4) 0.045(5) 0.013(4) -0.009(4) 0.003(3) C52 0.071(5) 0.035(4) 0.048(5) 0.007(4) -0.007(4) 0.005(3) C53 0.069(6) 0.088(8) 0.068(6) 0.025(6) -0.003(5) -0.027(5) C54 0.083(7) 0.117(11) 0.089(9) 0.039(8) 0.001(6) -0.028(7) C55 0.104(11) 0.104(11) 0.078(7) 0.015(7) -0.003(6) -0.042(8) C56 0.082(9) 0.128(9) 0.068(6) 0.027(5) -0.004(5) 0.037(7) C57 0.063(8) 0.112(8) 0.088(9) -0.003(6) -0.012(7) 0.011(6) C58 0.111(13) 0.185(14) 0.139(12) 0.093(11) 0.025(10) 0.062(11) C59 0.120(10) 0.055(6) 0.131(12) 0.028(6) 0.015(8) 0.000(6) C60 0.159(14) 0.069(9) 0.21(2) 0.054(10) 0.044(14) -0.002(8) C61 0.164(15) 0.052(8) 0.155(13) 0.027(8) 0.031(12) 0.011(8) C62 0.063(5) 0.045(5) 0.040(5) 0.011(4) -0.008(4) 0.022(4) C63 0.064(6) 0.042(5) 0.076(8) -0.005(5) -0.020(5) 0.022(4) C64 0.062(6) 0.051(6) 0.069(7) 0.008(5) -0.002(5) 0.023(5) C65 0.039(4) 0.039(4) 0.051(5) 0.015(4) 0.000(3) 0.008(4) C66 0.043(5) 0.063(6) 0.050(5) 0.019(4) 0.002(4) 0.022(5) C67 0.051(6) 0.041(5) 0.055(5) 0.017(4) -0.004(4) 0.014(4) C68 0.034(4) 0.035(4) 0.046(5) 0.010(3) 0.005(3) 0.011(3) C69 0.049(6) 0.054(6) 0.048(5) 0.017(4) -0.001(4) 0.005(4) C70 0.045(5) 0.035(4) 0.053(5) 0.003(4) 0.008(4) 0.004(4) N1 0.019(3) 0.044(3) 0.052(4) -0.001(3) 0.001(3) 0.008(2) N2 0.036(4) 0.061(4) 0.059(4) 0.027(3) -0.001(3) -0.009(3) O1 0.027(3) 0.048(3) 0.053(4) 0.013(3) -0.003(3) 0.006(2) O2 0.030(3) 0.031(3) 0.063(4) 0.004(2) -0.009(3) 0.008(2) O3 0.021(2) 0.039(3) 0.048(4) 0.008(3) 0.000(2) 0.009(2) O4 0.054(4) 0.039(3) 0.052(3) 0.016(3) -0.004(3) 0.002(3) O5 0.063(5) 0.081(4) 0.073(5) 0.043(4) 0.036(4) 0.038(4) Si1 0.0379(15) 0.094(2) 0.0396(16) 0.0124(15) 0.0031(12) 0.0353(15) Si2 0.0353(16) 0.116(3) 0.0483(18) 0.0189(18) -0.0041(13) 0.0089(17) Si3 0.088(2) 0.0409(16) 0.068(2) 0.0183(15) 0.0119(18) -0.0150(16) Si4 0.0372(13) 0.0317(12) 0.0436(15) 0.0097(11) -0.0025(11) 0.0089(10) U1 0.02189(16) 0.0548(2) 0.0479(2) 0.02122(17) 0.00793(14) 0.01615(14) U2 0.03332(19) 0.03354(19) 0.0458(2) 0.01339(15) -0.00759(15) -0.00036(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 C1 N1 117.8(7) O2 C1 O3 124.5(8) O3 C1 N1 117.7(8) C3 C2 C6 130.0(10) C3 C2 N1 107.0(9) N1 C2 C6 122.8(9) C2 C3 C4 108.7(9) C2 C3 C7 124.7(11) C4 C3 C7 126.5(10) C3 C4 C8 124.6(11) C5 C4 C3 109.5(9) C5 C4 C8 125.8(12) C4 C5 C9 129.9(9) C4 C5 N1 105.3(9) N1 C5 C9 124.3(9) C2 C6 H6A 109.5 C2 C6 H6B 109.5 C2 C6 H6C 109.5 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C3 C7 H7A 109.5 C3 C7 H7B 109.5 C3 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C4 C8 H8A 109.5 C4 C8 H8B 109.5 C4 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C5 C9 H9A 109.5 C5 C9 H9B 109.5 C5 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 O4 C10 N2 116.7(10) O5 C10 N2 119.5(10) O5 C10 O4 123.8(10) C12 C11 C15 127.4(12) C12 C11 N2 106.7(13) N2 C11 C15 125.5(10) C11 C12 C13 107.3(13) C11 C12 C16 127.2(16) C13 C12 C16 125.2(15) C12 C13 C17 125.8(16) C14 C13 C12 112.2(15) C14 C13 C17 121.8(17) C13 C14 C18 132.8(14) C13 C14 N2 103.4(14) N2 C14 C18 123.6(12) C11 C15 H15A 109.5 C11 C15 H15B 109.5 C11 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C12 C16 H16A 109.5 C12 C16 H16B 109.5 C12 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C13 C17 H17A 109.5 C13 C17 H17B 109.5 C13 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C14 C18 H18A 109.5 C14 C18 H18B 109.5 C14 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C20 C19 C26 130.6(11) C20 C19 Si1 116.3(8) C20 C19 U1 73.1(5) C26 C19 Si1 113.0(8) C26 C19 U1 73.4(5) Si1 C19 U1 137.8(5) C19 C20 H20 109.9 C19 C20 C21 140.1(10) C19 C20 U1 76.4(5) C21 C20 H20 109.9 C21 C20 U1 74.6(5) U1 C20 H20 137.2 C20 C21 H21 112.6 C20 C21 U1 74.1(6) C22 C21 C20 134.9(10) C22 C21 H21 112.6 C22 C21 U1 76.8(6) U1 C21 H21 130.8 C21 C22 Si2 115.7(8) C21 C22 U1 72.5(6) C23 C22 C21 131.0(10) C23 C22 Si2 113.2(8) C23 C22 U1 72.9(6) Si2 C22 U1 132.6(5) C22 C23 H23 111.3 C22 C23 C24 137.4(11) C22 C23 U1 76.9(7) C24 C23 H23 111.3 C24 C23 U1 74.5(6) U1 C23 H23 133.0 C23 C24 H24 112.2 C23 C24 C25 135.7(10) C23 C24 U1 74.9(6) C25 C24 H24 112.2 C25 C24 U1 74.5(6) U1 C24 H24 134.3 C24 C25 H25 112.3 C24 C25 C26 135.3(10) C24 C25 U1 74.7(6) C26 C25 H25 112.3 C26 C25 U1 74.5(6) U1 C25 H25 134.2 C19 C26 C25 134.9(10) C19 C26 H26 112.6 C19 C26 U1 75.9(6) C25 C26 H26 112.6 C25 C26 U1 74.0(6) U1 C26 H26 132.6 C28 C27 H27 104.4 C28 C27 C29 115.5(14) C28 C27 Si1 115.5(9) C29 C27 H27 104.4 C29 C27 Si1 111.1(9) Si1 C27 H27 104.4 C27 C28 H28A 109.5 C27 C28 H28B 109.5 C27 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C27 C29 H29A 109.5 C27 C29 H29B 109.5 C27 C29 H29C 109.5 H29A C29 H29B 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C31 C30 H30 105.2 C31 C30 Si1 111.6(10) C32 C30 H30 105.2 C32 C30 C31 111.4(15) C32 C30 Si1 117.1(13) Si1 C30 H30 105.2 C30 C31 H31A 109.5 C30 C31 H31B 109.5 C30 C31 H31C 109.5 H31A C31 H31B 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C30 C32 H32A 109.5 C30 C32 H32B 109.5 C30 C32 H32C 109.5 H32A C32 H32B 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C34 C33 H33 108.2 C34 C33 Si1 111.0(9) C35 C33 H33 108.2 C35 C33 C34 106.6(13) C35 C33 Si1 114.5(9) Si1 C33 H33 108.2 C33 C34 H34A 109.5 C33 C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34B 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C33 C35 H35A 109.5 C33 C35 H35B 109.5 C33 C35 H35C 109.5 H35A C35 H35B 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C37 C36 H36 105.3 C37 C36 C38 108.0(13) C37 C36 Si2 115.0(13) C38 C36 H36 105.3 C38 C36 Si2 116.8(11) Si2 C36 H36 105.3 C36 C37 H37A 109.5 C36 C37 H37B 109.5 C36 C37 H37C 109.5 H37A C37 H37B 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C36 C38 H38A 109.5 C36 C38 H38B 109.5 C36 C38 H38C 109.5 H38A C38 H38B 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C40 C39 H39 103.8 C40 C39 Si2 114.2(15) C41 C39 H39 103.8 C41 C39 C40 112.7(16) C41 C39 Si2 116.7(13) Si2 C39 H39 103.8 C39 C40 H40A 109.5 C39 C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40B 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C39 C41 H41A 109.5 C39 C41 H41B 109.5 C39 C41 H41C 109.5 H41A C41 H41B 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C43 C42 H42 104.2 C43 C42 Si2 109.8(14) C44 C42 H42 104.2 C44 C42 C43 112.5(17) C44 C42 Si2 120.2(19) Si2 C42 H42 104.2 C42 C43 H43A 109.5 C42 C43 H43B 109.5 C42 C43 H43C 109.5 H43A C43 H43B 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C42 C44 H44A 109.5 C42 C44 H44B 109.5 C42 C44 H44C 109.5 H44A C44 H44B 109.5 H44A C44 H44C 109.5 H44B C44 H44C 109.5 C46 C45 Si3 117.5(8) C46 C45 U2 71.9(6) C52 C45 C46 131.1(11) C52 C45 Si3 111.3(8) C52 C45 U2 72.8(6) Si3 C45 U2 138.9(6) C45 C46 H46 111.2 C45 C46 U2 77.4(6) C47 C46 C45 137.7(10) C47 C46 H46 111.2 C47 C46 U2 74.3(5) U2 C46 H46 132.6 C46 C47 H47 111.8 C46 C47 C48 136.5(10) C46 C47 U2 74.6(6) C48 C47 H47 111.8 C48 C47 U2 75.0(6) U2 C47 H47 135.0 C47 C48 C49 130.1(9) C47 C48 Si4 115.9(7) C47 C48 U2 73.6(6) C49 C48 Si4 113.8(7) C49 C48 U2 73.6(6) Si4 C48 U2 137.7(4) C48 C49 H49 111.6 C48 C49 U2 74.9(6) C50 C49 C48 136.8(10) C50 C49 H49 111.6 C50 C49 U2 74.9(6) U2 C49 H49 135.0 C49 C50 H50 112.5 C49 C50 U2 74.1(6) C51 C50 C49 135.1(10) C51 C50 H50 112.5 C51 C50 U2 75.5(6) U2 C50 H50 133.3 C50 C51 H51 112.1 C50 C51 C52 135.8(10) C50 C51 U2 74.2(6) C52 C51 H51 112.1 C52 C51 U2 74.6(6) U2 C51 H51 135.8 C45 C52 H52 111.6 C45 C52 U2 77.1(6) C51 C52 C45 136.8(11) C51 C52 H52 111.6 C51 C52 U2 75.0(6) U2 C52 H52 131.0 C54 C53 H53 107.7 C54 C53 C55 108.2(11) C54 C53 Si3 113.3(10) C55 C53 H53 107.7 C55 C53 Si3 112.2(12) Si3 C53 H53 107.7 C53 C54 H54A 109.5 C53 C54 H54B 109.5 C53 C54 H54C 109.5 H54A C54 H54B 109.5 H54A C54 H54C 109.5 H54B C54 H54C 109.5 C53 C55 H55A 109.5 C53 C55 H55B 109.5 C53 C55 H55C 109.5 H55A C55 H55B 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 C57 C56 H56 104.2 C57 C56 Si3 108.6(10) C58 C56 H56 104.2 C58 C56 C57 112.0(15) C58 C56 Si3 121.7(15) Si3 C56 H56 104.2 C56 C57 H57A 109.5 C56 C57 H57B 109.5 C56 C57 H57C 109.5 H57A C57 H57B 109.5 H57A C57 H57C 109.5 H57B C57 H57C 109.5 C56 C58 H58A 109.5 C56 C58 H58B 109.5 C56 C58 H58C 109.5 H58A C58 H58B 109.5 H58A C58 H58C 109.5 H58B C58 H58C 109.5 C60 C59 H59 107.2 C60 C59 Si3 109.8(14) C61 C59 H59 107.2 C61 C59 C60 111.1(17) C61 C59 Si3 114.0(13) Si3 C59 H59 107.2 C59 C60 H60A 109.5 C59 C60 H60B 109.5 C59 C60 H60C 109.5 H60A C60 H60B 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 C59 C61 H61A 109.5 C59 C61 H61B 109.5 C59 C61 H61C 109.5 H61A C61 H61B 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C63 C62 H62 107.6 C63 C62 C64 111.1(8) C63 C62 Si4 109.6(8) C64 C62 H62 107.6 C64 C62 Si4 112.9(7) Si4 C62 H62 107.6 C62 C63 H63A 109.5 C62 C63 H63B 109.5 C62 C63 H63C 109.5 H63A C63 H63B 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 C62 C64 H64A 109.5 C62 C64 H64B 109.5 C62 C64 H64C 109.5 H64A C64 H64B 109.5 H64A C64 H64C 109.5 H64B C64 H64C 109.5 C66 C65 H65 106.4 C66 C65 Si4 114.4(7) C67 C65 H65 106.4 C67 C65 C66 109.5(8) C67 C65 Si4 113.3(7) Si4 C65 H65 106.4 C65 C66 H66A 109.5 C65 C66 H66B 109.5 C65 C66 H66C 109.5 H66A C66 H66B 109.5 H66A C66 H66C 109.5 H66B C66 H66C 109.5 C65 C67 H67A 109.5 C65 C67 H67B 109.5 C65 C67 H67C 109.5 H67A C67 H67B 109.5 H67A C67 H67C 109.5 H67B C67 H67C 109.5 C69 C68 H68 106.1 C69 C68 C70 109.6(8) C69 C68 Si4 114.0(7) C70 C68 H68 106.1 C70 C68 Si4 114.3(6) Si4 C68 H68 106.1 C68 C69 H69A 109.5 C68 C69 H69B 109.5 C68 C69 H69C 109.5 H69A C69 H69B 109.5 H69A C69 H69C 109.5 H69B C69 H69C 109.5 C68 C70 H70A 109.5 C68 C70 H70B 109.5 C68 C70 H70C 109.5 H70A C70 H70B 109.5 H70A C70 H70C 109.5 H70B C70 H70C 109.5 C1 N1 C2 125.7(8) C1 N1 C5 124.7(8) C2 N1 C5 109.5(8) C10 N2 C11 123.8(10) C10 N2 C14 124.9(10) C11 N2 C14 110.3(10) U2 O1 U1 139.4(3) C1 O2 U2 138.5(5) C1 O3 U1 136.7(5) C10 O4 U2 139.8(7) C10 O5 U1 137.9(7) C27 Si1 C19 112.7(5) C30 Si1 C19 109.7(6) C30 Si1 C27 113.6(7) C33 Si1 C19 108.2(6) C33 Si1 C27 105.8(7) C33 Si1 C30 106.4(7) C22 Si2 C39 102.3(6) C36 Si2 C22 109.1(6) C36 Si2 C39 104.9(7) C42 Si2 C22 109.3(8) C42 Si2 C36 120.2(9) C42 Si2 C39 109.6(10) C45 Si3 C59 102.8(7) C53 Si3 C45 111.9(6) C53 Si3 C56 110.9(7) C53 Si3 C59 118.0(8) C56 Si3 C45 106.7(7) C56 Si3 C59 105.6(8) C48 Si4 C65 109.7(4) C62 Si4 C48 108.1(4) C62 Si4 C65 105.8(4) C62 Si4 C68 108.7(5) C68 Si4 C48 109.2(4) C68 Si4 C65 115.1(4) C19 U1 C22 81.2(3) C19 U1 U2 118.1(2) C20 U1 C19 30.5(3) C20 U1 C21 31.3(3) C20 U1 C22 58.9(3) C20 U1 C23 78.3(3) C20 U1 C24 86.0(3) C20 U1 C25 78.3(3) C20 U1 C26 57.7(3) C20 U1 U2 135.0(3) C21 U1 C19 59.8(3) C21 U1 C22 30.7(3) C21 U1 C23 57.9(3) C21 U1 C26 80.3(3) C21 U1 U2 152.5(3) C22 U1 U2 159.3(2) C23 U1 C19 88.4(3) C23 U1 C22 30.3(3) C23 U1 U2 146.4(2) C24 U1 C19 80.1(3) C24 U1 C21 78.9(3) C24 U1 C22 58.3(3) C24 U1 C23 30.6(3) C24 U1 C26 59.4(4) C24 U1 U2 128.7(2) C25 U1 C19 59.1(3) C25 U1 C21 87.7(3) C25 U1 C22 79.9(3) C25 U1 C23 58.7(3) C25 U1 C24 30.7(3) C25 U1 C26 31.5(3) C25 U1 U2 115.6(2) C26 U1 C19 30.7(3) C26 U1 C22 89.1(3) C26 U1 C23 80.5(3) C26 U1 U2 111.3(2) O1 U1 C19 100.0(3) O1 U1 C20 122.8(3) O1 U1 C21 151.2(3) O1 U1 C22 178.0(3) O1 U1 C23 147.9(3) O1 U1 C24 120.2(3) O1 U1 C25 99.4(3) O1 U1 C26 91.2(3) O1 U1 O3 83.2(2) O1 U1 O5 82.7(3) O1 U1 U2 20.22(17) O3 U1 C19 160.4(3) O3 U1 C20 153.8(3) O3 U1 C21 123.0(3) O3 U1 C22 95.1(3) O3 U1 C23 79.3(3) O3 U1 C24 81.6(3) O3 U1 C25 101.3(3) O3 U1 C26 130.8(3) O3 U1 O5 88.4(2) O3 U1 U2 69.19(14) O5 U1 C19 111.1(3) O5 U1 C20 92.5(3) O5 U1 C21 86.1(3) O5 U1 C22 98.4(3) O5 U1 C23 123.2(3) O5 U1 C24 153.3(3) O5 U1 C25 170.2(3) O5 U1 C26 139.4(3) O5 U1 U2 68.71(18) C45 U2 U1 132.2(3) C46 U2 C45 30.7(3) C46 U2 C48 59.9(3) C46 U2 C50 87.2(3) C46 U2 C51 78.4(3) C46 U2 C52 57.9(3) C46 U2 U1 118.8(2) C47 U2 C45 59.2(3) C47 U2 C46 31.1(3) C47 U2 C48 31.5(3) C47 U2 C49 59.2(3) C47 U2 C50 79.9(3) C47 U2 C51 87.3(3) C47 U2 C52 79.5(3) C47 U2 U1 112.6(2) C48 U2 C45 81.5(3) C48 U2 C51 80.7(3) C48 U2 C52 89.3(3) C48 U2 U1 115.9(2) C49 U2 C45 88.1(3) C49 U2 C46 79.9(3) C49 U2 C48 31.5(3) C49 U2 C50 31.0(3) C49 U2 C51 58.4(3) C49 U2 C52 79.6(3) C49 U2 U1 130.72(19) C50 U2 C45 79.2(3) C50 U2 C48 59.9(3) C50 U2 C51 30.3(3) C50 U2 C52 58.3(3) C50 U2 U1 148.6(2) C51 U2 C45 57.8(3) C51 U2 U1 160.1(2) C52 U2 C45 30.2(3) C52 U2 C51 30.5(3) C52 U2 U1 149.6(3) O1 U2 C45 120.2(3) O1 U2 C46 100.2(3) O1 U2 C47 92.4(3) O1 U2 C48 100.1(3) O1 U2 C49 123.1(3) O1 U2 C50 151.6(3) O1 U2 C51 177.8(3) O1 U2 C52 147.4(3) O1 U2 O2 84.7(2) O1 U2 O4 83.9(3) O1 U2 U1 20.42(18) O2 U2 C45 153.0(3) O2 U2 C46 165.3(3) O2 U2 C47 135.8(3) O2 U2 C48 105.7(3) O2 U2 C49 85.9(3) O2 U2 C50 82.2(2) O2 U2 C51 97.0(3) O2 U2 C52 122.9(3) O2 U2 U1 68.70(14) O4 U2 C45 94.8(3) O4 U2 C46 117.6(3) O4 U2 C47 147.2(3) O4 U2 C48 175.5(2) O4 U2 C49 146.4(3) O4 U2 C50 117.0(3) O4 U2 C51 95.2(3) O4 U2 C52 86.2(3) O4 U2 O2 76.5(2) O4 U2 U1 68.56(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.381(10) C1 O2 1.262(10) C1 O3 1.270(10) C2 C3 1.366(13) C2 C6 1.482(16) C2 N1 1.397(12) C3 C4 1.387(16) C3 C7 1.528(14) C4 C5 1.386(13) C4 C8 1.498(15) C5 C9 1.475(15) C5 N1 1.406(12) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 N2 1.381(14) C10 O4 1.256(12) C10 O5 1.243(12) C11 C12 1.375(18) C11 C15 1.438(18) C11 N2 1.411(15) C12 C13 1.40(2) C12 C16 1.50(2) C13 C14 1.37(2) C13 C17 1.55(2) C14 C18 1.45(2) C14 N2 1.425(16) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 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 C19 C20 1.406(13) C19 C26 1.415(14) C19 Si1 1.903(11) C19 U1 2.692(9) C20 H20 0.9500 C20 C21 1.430(14) C20 U1 2.649(9) C21 H21 0.9500 C21 C22 1.424(15) C21 U1 2.655(10) C22 C23 1.404(14) C22 Si2 1.903(12) C22 U1 2.711(11) C23 H23 0.9500 C23 C24 1.404(14) C23 U1 2.660(11) C24 H24 0.9500 C24 C25 1.407(15) C24 U1 2.655(10) C25 H25 0.9500 C25 C26 1.442(16) C25 U1 2.652(10) C26 H26 0.9500 C26 U1 2.660(10) C27 H27 1.0000 C27 C28 1.506(19) C27 C29 1.541(18) C27 Si1 1.880(12) C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 H30 1.0000 C30 C31 1.58(2) C30 C32 1.50(2) C30 Si1 1.873(14) C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 H33 1.0000 C33 C34 1.558(19) C33 C35 1.54(2) C33 Si1 1.863(12) C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 H36 1.0000 C36 C37 1.54(2) C36 C38 1.564(18) C36 Si2 1.869(16) C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 C39 H39 1.0000 C39 C40 1.50(2) C39 C41 1.39(2) C39 Si2 2.039(18) C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 C41 H41A 0.9800 C41 H41B 0.9800 C41 H41C 0.9800 C42 H42 1.0000 C42 C43 1.65(3) C42 C44 1.32(3) C42 Si2 1.827(19) C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C44 H44A 0.9800 C44 H44B 0.9800 C44 H44C 0.9800 C45 C46 1.417(15) C45 C52 1.397(15) C45 Si3 1.890(12) C45 U2 2.709(9) C46 H46 0.9500 C46 C47 1.413(14) C46 U2 2.638(10) C47 H47 0.9500 C47 C48 1.433(13) C47 U2 2.634(10) C48 C49 1.436(13) C48 Si4 1.913(10) C48 U2 2.651(10) C49 H49 0.9500 C49 C50 1.409(13) C49 U2 2.634(10) C50 H50 0.9500 C50 C51 1.387(14) C50 U2 2.644(10) C51 H51 0.9500 C51 C52 1.396(15) C51 U2 2.660(10) C52 H52 0.9500 C52 U2 2.654(10) C53 H53 1.0000 C53 C54 1.532(19) C53 C55 1.552(19) C53 Si3 1.852(15) C54 H54A 0.9800 C54 H54B 0.9800 C54 H54C 0.9800 C55 H55A 0.9800 C55 H55B 0.9800 C55 H55C 0.9800 C56 H56 1.0000 C56 C57 1.54(2) C56 C58 1.45(2) C56 Si3 1.872(15) C57 H57A 0.9800 C57 H57B 0.9800 C57 H57C 0.9800 C58 H58A 0.9800 C58 H58B 0.9800 C58 H58C 0.9800 C59 H59 1.0000 C59 C60 1.49(2) C59 C61 1.38(2) C59 Si3 2.018(17) C60 H60A 0.9800 C60 H60B 0.9800 C60 H60C 0.9800 C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C62 H62 1.0000 C62 C63 1.534(15) C62 C64 1.542(14) C62 Si4 1.895(10) C63 H63A 0.9800 C63 H63B 0.9800 C63 H63C 0.9800 C64 H64A 0.9800 C64 H64B 0.9800 C64 H64C 0.9800 C65 H65 1.0000 C65 C66 1.543(14) C65 C67 1.529(14) C65 Si4 1.915(10) C66 H66A 0.9800 C66 H66B 0.9800 C66 H66C 0.9800 C67 H67A 0.9800 C67 H67B 0.9800 C67 H67C 0.9800 C68 H68 1.0000 C68 C69 1.532(14) C68 C70 1.547(12) C68 Si4 1.896(9) C69 H69A 0.9800 C69 H69B 0.9800 C69 H69C 0.9800 C70 H70A 0.9800 C70 H70B 0.9800 C70 H70C 0.9800 O1 U1 2.094(7) O1 U2 2.074(6) O2 U2 2.353(6) O3 U1 2.350(5) O4 U2 2.329(7) O5 U1 2.379(7) U1 U2 3.9087(5) 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 C2 C3 C4 C5 1.8(13) C2 C3 C4 C8 -175.7(12) C3 C2 N1 C1 179.3(9) C3 C2 N1 C5 0.1(11) C3 C4 C5 C9 -173.1(10) C3 C4 C5 N1 -1.7(12) C4 C5 N1 C1 -178.2(9) C4 C5 N1 C2 1.0(11) C6 C2 C3 C4 -175.2(12) C6 C2 C3 C7 4.9(19) C6 C2 N1 C1 -6.1(16) C6 C2 N1 C5 174.6(10) C7 C3 C4 C5 -178.2(10) C7 C3 C4 C8 4.2(19) C8 C4 C5 C9 4(2) C8 C4 C5 N1 175.8(12) C9 C5 N1 C1 -6.2(15) C9 C5 N1 C2 173.0(10) C11 C12 C13 C14 0(2) C11 C12 C13 C17 -174.7(18) C12 C11 N2 C10 -165.9(10) C12 C11 N2 C14 2.9(14) C12 C13 C14 C18 176.4(18) C12 C13 C14 N2 1(2) C13 C14 N2 C10 166.1(12) C13 C14 N2 C11 -2.6(16) C15 C11 C12 C13 171.4(13) C15 C11 C12 C16 -3(2) C15 C11 N2 C10 20.6(17) C15 C11 N2 C14 -170.6(12) C16 C12 C13 C14 174.8(15) C16 C12 C13 C17 0(3) C17 C13 C14 C18 -8(3) C17 C13 C14 N2 176.6(17) C18 C14 N2 C10 -10(2) C18 C14 N2 C11 -178.2(14) C19 C20 C21 C22 7(2) C19 C20 C21 U1 -44.8(14) C20 C19 C26 C25 -0.3(19) C20 C19 C26 U1 49.1(10) C20 C21 C22 C23 -4(2) C20 C21 C22 Si2 179.6(10) C20 C21 C22 U1 -51.0(12) C21 C22 C23 C24 2(2) C21 C22 C23 U1 -46.7(11) C22 C23 C24 C25 -2(2) C22 C23 C24 U1 -49.4(12) C23 C24 C25 C26 0(2) C23 C24 C25 U1 -48.0(11) C24 C25 C26 C19 2(2) C24 C25 C26 U1 -48.0(11) C26 C19 C20 C21 -5(2) C26 C19 C20 U1 -49.2(10) C28 C27 Si1 C19 62.9(13) C28 C27 Si1 C30 -62.7(13) C28 C27 Si1 C33 -179.0(11) C29 C27 Si1 C19 -163.0(13) C29 C27 Si1 C30 71.4(15) C29 C27 Si1 C33 -44.9(15) C31 C30 Si1 C19 163.9(11) C31 C30 Si1 C27 -69.0(13) C31 C30 Si1 C33 47.0(13) C32 C30 Si1 C19 -66.0(13) C32 C30 Si1 C27 61.1(13) C32 C30 Si1 C33 177.1(12) C34 C33 Si1 C19 -61.7(10) C34 C33 Si1 C27 177.3(10) C34 C33 Si1 C30 56.1(11) C35 C33 Si1 C19 59.0(13) C35 C33 Si1 C27 -62.0(13) C35 C33 Si1 C30 176.9(12) C37 C36 Si2 C22 38.4(15) C37 C36 Si2 C39 147.4(14) C37 C36 Si2 C42 -88.8(16) C38 C36 Si2 C22 166.5(11) C38 C36 Si2 C39 -84.5(13) C38 C36 Si2 C42 39.3(16) C43 C42 Si2 C22 154.5(13) C43 C42 Si2 C36 -78.4(17) C43 C42 Si2 C39 43.1(17) C44 C42 Si2 C22 -73(2) C44 C42 Si2 C36 54(2) C44 C42 Si2 C39 175.9(17) C45 C46 C47 C48 -3(2) C45 C46 C47 U2 -49.8(13) C46 C45 C52 C51 -5(2) C46 C45 C52 U2 45.3(12) C46 C45 Si3 C53 -1.5(11) C46 C45 Si3 C56 -123.0(9) C46 C45 Si3 C59 126.1(10) C46 C47 C48 C49 4(2) C46 C47 C48 Si4 177.4(10) C46 C47 C48 U2 -47.0(12) C47 C48 C49 C50 -3.7(19) C47 C48 C49 U2 -50.7(10) C48 C49 C50 C51 2(2) C48 C49 C50 U2 -47.1(11) C49 C50 C51 C52 -2(2) C49 C50 C51 U2 -48.8(11) C50 C51 C52 C45 5(2) C50 C51 C52 U2 -46.4(12) C52 C45 C46 C47 3(2) C52 C45 C46 U2 -45.6(12) C52 C45 Si3 C53 -179.9(9) C52 C45 Si3 C56 58.6(10) C52 C45 Si3 C59 -52.3(10) C54 C53 Si3 C45 -167.4(11) C54 C53 Si3 C56 -48.3(14) C54 C53 Si3 C59 73.7(14) C55 C53 Si3 C45 69.8(11) C55 C53 Si3 C56 -171.1(10) C55 C53 Si3 C59 -49.2(12) C57 C56 Si3 C45 76.3(12) C57 C56 Si3 C53 -45.8(13) C57 C56 Si3 C59 -174.8(11) C58 C56 Si3 C45 -151.4(13) C58 C56 Si3 C53 86.5(15) C58 C56 Si3 C59 -42.4(16) C63 C62 Si4 C48 60.2(8) C63 C62 Si4 C65 -57.3(8) C63 C62 Si4 C68 178.6(7) C64 C62 Si4 C48 -64.4(9) C64 C62 Si4 C65 178.2(8) C64 C62 Si4 C68 54.1(9) C69 C68 Si4 C48 173.5(7) C69 C68 Si4 C62 55.8(8) C69 C68 Si4 C65 -62.6(8) C70 C68 Si4 C48 -59.3(8) C70 C68 Si4 C62 -177.1(7) C70 C68 Si4 C65 64.5(8) N1 C1 O2 U2 -179.4(6) N1 C1 O3 U1 -161.6(6) N1 C2 C3 C4 -1.2(12) N1 C2 C3 C7 178.9(9) N2 C10 O4 U2 166.9(6) N2 C10 O5 U1 179.2(7) N2 C11 C12 C13 -1.9(16) N2 C11 C12 C16 -176.3(13) O2 C1 N1 C2 -28.2(14) O2 C1 N1 C5 150.9(9) O2 C1 O3 U1 17.6(15) O3 C1 N1 C2 151.0(9) O3 C1 N1 C5 -29.9(13) O3 C1 O2 U2 1.4(16) O4 C10 N2 C11 7.1(15) O4 C10 N2 C14 -160.2(11) O4 C10 O5 U1 -0.7(18) O5 C10 N2 C11 -172.9(10) O5 C10 N2 C14 19.9(17) O5 C10 O4 U2 -13.2(17) Si1 C19 C20 C21 179.8(12) Si1 C19 C20 U1 135.5(6) Si1 C19 C26 C25 175.2(9) Si1 C19 C26 U1 -135.5(6) Si2 C22 C23 C24 178.4(10) Si2 C22 C23 U1 129.7(6) Si3 C45 C46 C47 -174.8(11) Si3 C45 C46 U2 136.3(7) Si3 C45 C52 C51 172.7(11) Si3 C45 C52 U2 -136.5(6) Si4 C48 C49 C50 -177.4(9) Si4 C48 C49 U2 135.5(6) U1 C19 C20 C21 44.4(14) U1 C19 C26 C25 -49.3(11) U1 C20 C21 C22 51.8(12) U1 C21 C22 C23 46.8(11) U1 C21 C22 Si2 -129.5(6) U1 C22 C23 C24 48.7(12) U1 C23 C24 C25 47.9(11) U1 C24 C25 C26 48.0(11) U1 C25 C26 C19 50.0(11) U2 C45 C46 C47 48.9(13) U2 C45 C52 C51 -50.7(13) U2 C45 Si3 C53 92.2(9) U2 C45 Si3 C56 -29.3(10) U2 C45 Si3 C59 -140.2(9) U2 C46 C47 C48 47.1(12) U2 C47 C48 C49 50.7(10) U2 C47 C48 Si4 -135.6(6) U2 C48 C49 C50 47.1(11) U2 C49 C50 C51 49.2(11) U2 C50 C51 C52 46.5(13) U2 C51 C52 C45 51.4(13) 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 1 0.500 0.500 0.000 635.6 10.2 2 0.333 0.888 0.450 7.2 0.5 3 0.667 0.113 0.550 7.2 0.0