#------------------------------------------------------------------------------ #$Date: 2024-06-29 01:09:46 +0300 (Sat, 29 Jun 2024) $ #$Revision: 292647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572015.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_1572015 loop_ _publ_author_name 'Doyle, Michael P.' 'Bao, Ming' 'Boh\'orquez, Arnold R. R.' 'Arman, Hadi' _publ_section_title ; Photoinduced [4+2]-Cycloaddition Reactions of Vinyldiazo Compounds for the Construction of Heterocyclic and Bicyclic Rings ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03558E _journal_year 2024 _chemical_formula_moiety 'C35 H41 N3 O4 Si' _chemical_formula_sum 'C35 H41 N3 O4 Si' _chemical_formula_weight 595.80 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-04-03 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2024-04-05 deposited with the CCDC. 2024-06-27 downloaded from the CCDC. ; _cell_angle_alpha 90.5720(10) _cell_angle_beta 92.7850(10) _cell_angle_gamma 107.3760(10) _cell_formula_units_Z 4 _cell_length_a 14.0714(2) _cell_length_b 14.8588(2) _cell_length_c 16.3784(2) _cell_measurement_reflns_used 23130 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 75.9960 _cell_measurement_theta_min 4.1390 _cell_volume 3263.25(8) _computing_cell_refinement 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.959 _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 -122.00 -30.00 0.50 0.42 -- -46.65 -16.00 72.00 184 2 \w 30.00 123.00 0.50 0.42 -- 46.65 16.00-118.00 186 3 \w -28.00 29.00 0.50 0.42 -- 46.65 -16.00 72.00 114 4 \w -167.00 -75.00 0.50 1.66 -- -91.75 -16.00 72.00 184 5 \w 90.00 178.00 0.50 1.66 -- 106.91 16.00-118.00 176 6 \w -118.00 -83.00 0.50 0.42 -- -46.65 -57.00 120.00 70 7 \w -29.00 30.00 0.50 0.42 -- -46.65 16.00-118.00 118 8 \w -118.00 -83.00 0.50 0.42 -- -46.65 -57.00 0.00 70 9 \w -30.00 29.00 0.50 0.42 -- -46.65 19.00 -60.00 118 10 \w -86.00 -13.00 0.50 0.42 -- -46.65 125.00-120.00 146 11 \w 83.00 120.00 0.50 0.42 -- 46.65 57.00 0.00 74 12 \w -25.00 63.00 0.50 0.42 -- 46.65 -57.00 60.00 176 13 \w 34.00 93.00 0.50 0.42 -- 46.65-125.00 120.00 118 14 \w -51.00 -19.00 0.50 1.66 -- -91.75 45.00-150.00 64 15 \w -51.00 -19.00 0.50 1.66 -- -91.75 45.00 60.00 64 16 \w -164.00-100.00 0.50 1.66 -- -91.75 -94.00 150.00 128 17 \w -51.00 -19.00 0.50 1.66 -- -91.75 45.00-180.00 64 18 \w -51.00 -19.00 0.50 1.66 -- -91.75 45.00-120.00 64 19 \w -164.00 -90.00 0.50 1.66 -- -91.75 -60.00-110.28 148 20 \w -164.00-101.00 0.50 1.66 -- -91.75 -77.00-180.00 126 21 \w -162.00 -87.00 0.50 1.66 -- -91.75-125.00-180.00 150 22 \w -101.00 -19.00 0.50 1.66 -- -91.75 77.00 30.00 164 23 \w -164.00-101.00 0.50 1.66 -- -91.75 -77.00-150.00 126 24 \w -164.00-100.00 0.50 1.66 -- -91.75 -94.00 60.00 128 25 \w -85.00 -22.00 0.50 1.66 -- -91.75 125.00 -60.00 126 26 \w -71.00 -19.00 0.50 1.66 -- -91.75 61.00 120.00 104 27 \w 34.00 71.00 0.50 1.66 -- 106.91 -61.00 120.00 74 28 \w 37.00 112.00 0.50 1.66 -- 106.91-125.00 60.00 150 29 \w 37.00 112.00 0.50 1.66 -- 106.91-125.00 120.00 150 30 \w 37.00 112.00 0.50 1.66 -- 106.91-125.00 30.00 150 31 \w 34.00 106.00 0.50 1.66 -- 106.91 -94.00-120.00 144 32 \w 34.00 106.00 0.50 1.66 -- 106.91 -94.00 150.00 144 33 \w 34.00 71.00 0.50 1.66 -- 106.91 -61.00 60.00 74 34 \w 37.00 112.00 0.50 1.66 -- 106.91-125.00-180.00 150 35 \w 38.00 108.00 0.50 1.66 -- 106.91-111.00 -62.55 140 36 \w 34.00 106.00 0.50 1.66 -- 106.91 -94.00-180.00 144 37 \w 37.00 112.00 0.50 1.66 -- 106.91-125.00 -30.00 150 38 \w 34.00 71.00 0.50 1.66 -- 106.91 -61.00-120.00 74 39 \w 34.00 106.00 0.50 1.66 -- 106.91 -94.00 30.00 144 40 \w 34.00 71.00 0.50 1.66 -- 106.91 -61.00-150.00 74 41 \w 39.00 119.00 0.50 1.66 -- 106.91-134.00 -95.97 160 42 \w 92.00 178.00 0.50 1.66 -- 106.91 30.00 -30.00 172 43 \w 34.00 71.00 0.50 1.66 -- 106.91 -61.00 30.00 74 44 \w 34.00 106.00 0.50 1.66 -- 106.91 -94.00 90.00 144 45 \w -118.00 -31.00 0.50 0.42 -- -46.65 -55.00 26.88 174 46 \w 31.00 120.00 0.50 0.42 -- 46.65 55.00 158.42 178 47 \w 31.00 120.00 0.50 0.42 -- 46.65 54.00 -6.07 178 48 \w 31.00 120.00 0.50 0.42 -- 46.65 55.00-134.99 178 49 \w 31.00 120.00 0.50 0.42 -- 46.65 55.00 115.64 178 50 \w 31.00 120.00 0.50 0.42 -- 46.65 53.00 -74.43 178 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0591211000 _diffrn_orient_matrix_UB_12 -0.1024211000 _diffrn_orient_matrix_UB_13 0.0181468000 _diffrn_orient_matrix_UB_21 0.0950006000 _diffrn_orient_matrix_UB_22 -0.0299968000 _diffrn_orient_matrix_UB_23 -0.0077993000 _diffrn_orient_matrix_UB_31 0.0260408000 _diffrn_orient_matrix_UB_32 0.0204948000 _diffrn_orient_matrix_UB_33 0.0921092000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0143 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 23211 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.829 _diffrn_reflns_theta_min 2.702 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_T_max 0.117 _exptl_absorpt_correction_T_min 0.007 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.213 _exptl_crystal_description plate _exptl_crystal_F_000 1272 _exptl_crystal_size_max 0.139 _exptl_crystal_size_mid 0.093 _exptl_crystal_size_min 0.062 _refine_diff_density_max 0.900 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 788 _refine_ls_number_reflns 23211 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0669 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1395 _refine_ls_wR_factor_ref 0.1432 _reflns_Friedel_coverage 0.000 _reflns_number_gt 20241 _reflns_number_total 23211 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 179.5296\% around [-0.00 -0.00 1.00] (reciprocal) or [0.06 0.03 1.00] (direct) ; _cod_data_source_file d4sc03558e2.cif _cod_data_source_block hpd873_twin1_hklf4 _cod_database_code 1572015 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H O N Si' _chemical_oxdiff_usercomment 627 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.5668(7) 0.4332(7) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3.a Ternary CH refined with riding coordinates: C4(H4), C39(H39) 3.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B), C2(H2A,H2B), C55(H55A,H55B), C56(H56A,H56B), C20(H20A,H20B), C21(H21A,H21B) 3.c Aromatic/amide H refined with riding coordinates: C14(H14), C64(H64), C18(H18), C53(H53), C43(H43), C29(H29), C47(H47), C8(H8), C44(H44), C12(H12), C16(H16), C45(H45), C23(H23), C17(H17), C50(H50), C9(H9), C27(H27), C62(H62), C49(H49), C58(H58), C15(H15), C10(H10), C46(H46), C61(H61), C60(H60), C51(H51), C52(H52), C24(H24), C26(H26), C11(H11), C25(H25), C59(H59) 3.d Idealised Me refined as rotating group: C63(H63A,H63B,H63C), C68(H68A,H68B,H68C), C28(H28A,H28B,H28C), C33(H33A,H33B, H33C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C34(H34A,H34B,H34C), C31(H31A, H31B,H31C), C66(H66A,H66B,H66C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C65(H65A,H65B,H65C) ; _shelx_res_file ; TITL hpd873_twin1_hklf4_a.res in P-1 hpd873_twin1_hklf4.res created by SHELXL-2018/3 at 13:12:21 on 03-Apr-2024 REM Old TITL hpd873_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.144, Rweak 0.007, Alpha 0.029 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C70 N6 O8 Si2 CELL 1.54184 14.0714 14.8588 16.3784 90.572 92.785 107.376 ZERR 4 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N O Si UNIT 140 164 12 16 4 L.S. 4 0 0 PLAN 10 TEMP -173 BOND list 4 fmap 2 53 ACTA OMIT -1 0 4 OMIT 1 1 -2 OMIT 1 1 -1 OMIT 1 0 4 OMIT -2 2 1 OMIT -1 -1 0 OMIT 1 1 0 OMIT -1 -1 -1 OMIT 2 -2 1 OMIT 1 1 1 OMIT -1 -1 -2 REM REM REM WGHT 0.030000 3.000000 BASF 0.43324 FVAR 3.63377 SI1 5 0.225059 0.826340 0.416499 11.00000 0.05620 0.05575 = 0.05246 0.00694 -0.00529 0.01840 SI2 5 0.754965 0.801295 1.107853 11.00000 0.05150 0.05728 = 0.05414 -0.00594 0.00228 0.01868 O3 4 0.155548 0.324252 0.562185 11.00000 0.05148 0.04925 = 0.04594 -0.00122 -0.00393 0.02162 O6 4 0.595561 0.439892 1.006191 11.00000 0.05355 0.05505 = 0.04561 0.00282 0.00775 0.02521 O7 4 0.639409 0.321132 0.949613 11.00000 0.05028 0.04667 = 0.04811 0.00504 0.00553 0.02095 O5 4 0.702393 0.725749 0.795594 11.00000 0.04882 0.05414 = 0.05340 0.00635 0.00181 0.02564 O2 4 0.097996 0.431061 0.497029 11.00000 0.05380 0.05726 = 0.04612 0.00163 -0.00578 0.02551 O4 4 0.170240 0.715761 0.443481 11.00000 0.06094 0.05723 = 0.04843 0.00687 -0.00518 0.02837 O8 4 0.674269 0.727223 1.041322 11.00000 0.05084 0.05717 = 0.05012 -0.00764 0.00061 0.02536 O1 4 0.225397 0.745359 0.692920 11.00000 0.05423 0.06486 = 0.05864 -0.01008 -0.00160 0.03089 N2 3 0.393814 0.626134 0.635131 11.00000 0.04403 0.05346 = 0.04072 -0.00138 0.00146 0.02130 N1 3 0.302034 0.639905 0.654192 11.00000 0.04649 0.05231 = 0.04317 -0.00181 0.00043 0.02361 N4 3 0.779374 0.621067 0.839197 11.00000 0.04318 0.04872 = 0.04432 0.00367 0.00245 0.02203 N5 3 0.871795 0.606368 0.860260 11.00000 0.04077 0.05056 = 0.04126 0.00342 -0.00016 0.02021 N6 3 0.721063 0.681662 0.985301 11.00000 0.04843 0.05424 = 0.04566 -0.00272 0.00195 0.02488 N3 3 0.223900 0.687349 0.509402 11.00000 0.05591 0.05331 = 0.04721 0.00541 -0.00395 0.02418 C54 1 0.636098 0.410349 0.953192 11.00000 0.03949 0.04821 = 0.04476 0.00036 -0.00244 0.01765 C1 1 0.391633 0.538359 0.633224 11.00000 0.04962 0.05235 = 0.03496 -0.00046 -0.00308 0.02178 C36 1 0.867824 0.518483 0.866443 11.00000 0.04655 0.05014 = 0.03755 0.00058 0.00327 0.02170 C38 1 0.683203 0.464019 0.881778 11.00000 0.04293 0.04525 = 0.04273 0.00003 0.00190 0.01786 C3 1 0.204326 0.476489 0.619543 11.00000 0.04656 0.05030 = 0.04018 0.00266 -0.00009 0.02056 C41 1 0.780062 0.704510 0.803003 11.00000 0.04904 0.04817 = 0.04098 -0.00020 -0.00024 0.02139 C6 1 0.303388 0.725662 0.688180 11.00000 0.05565 0.05455 = 0.04257 0.00103 0.00230 0.02676 C19 1 0.148059 0.411763 0.552304 11.00000 0.04132 0.05132 = 0.04429 0.00206 0.00490 0.01834 C57 1 0.710813 0.166430 1.016166 11.00000 0.05125 0.04220 = 0.04883 0.00466 0.00085 0.01867 C42 1 0.874447 0.764192 0.769432 11.00000 0.04645 0.05175 = 0.04021 0.00387 -0.00405 0.02098 C13 1 0.486418 0.519228 0.616375 11.00000 0.05096 0.05372 = 0.03421 0.00254 -0.00010 0.02418 C7 1 0.399353 0.789725 0.724840 11.00000 0.05174 0.05241 = 0.04291 -0.00434 0.00646 0.02103 C40 1 0.689377 0.567907 0.876744 11.00000 0.04235 0.04725 = 0.04113 0.00260 0.00187 0.01924 C5 1 0.208362 0.580791 0.617847 11.00000 0.04761 0.05098 = 0.04201 0.00019 0.00050 0.02141 C4 1 0.141482 0.516098 0.675238 11.00000 0.05136 0.05458 = 0.04038 -0.00071 0.00097 0.02311 AFIX 13 H4 2 0.168120 0.525152 0.733444 11.00000 -1.20000 AFIX 0 C48 1 0.964511 0.500116 0.885997 11.00000 0.04983 0.05163 = 0.03781 -0.00156 0.00071 0.02468 C37 1 0.772576 0.440801 0.848448 11.00000 0.05040 0.05069 = 0.04576 0.00001 0.00394 0.02199 AFIX 23 H37A 2 0.778418 0.381960 0.873037 11.00000 -1.20000 H37B 2 0.761647 0.429752 0.788549 11.00000 -1.20000 AFIX 0 C14 1 0.487928 0.429424 0.590774 11.00000 0.05363 0.05157 = 0.04471 0.00078 0.00047 0.01956 AFIX 43 H14 2 0.427306 0.379466 0.583746 11.00000 -1.20000 AFIX 0 C64 1 0.656539 0.619622 0.942461 11.00000 0.04466 0.04736 = 0.04214 0.00262 0.00106 0.02121 AFIX 43 H64 2 0.587723 0.606131 0.952125 11.00000 -1.20000 AFIX 0 C18 1 0.576602 0.590785 0.626509 11.00000 0.05625 0.05380 = 0.04145 0.00132 0.00074 0.02423 AFIX 43 H18 2 0.576880 0.651979 0.644117 11.00000 -1.20000 AFIX 0 C2 1 0.300438 0.461609 0.654856 11.00000 0.05014 0.05231 = 0.04523 0.00221 -0.00296 0.02274 AFIX 23 H2A 2 0.298229 0.458747 0.715122 11.00000 -1.20000 H2B 2 0.305121 0.400319 0.634195 11.00000 -1.20000 AFIX 0 C53 1 0.968113 0.412958 0.915430 11.00000 0.05199 0.04999 = 0.04225 0.00000 0.00152 0.02043 AFIX 43 H53 2 0.908009 0.364051 0.922794 11.00000 -1.20000 AFIX 0 C43 1 0.934603 0.728358 0.722092 11.00000 0.05106 0.05547 = 0.04210 0.00408 -0.00181 0.02300 AFIX 43 H43 2 0.920370 0.662059 0.714753 11.00000 -1.20000 AFIX 0 C22 1 0.222729 0.164989 0.499351 11.00000 0.05373 0.04465 = 0.04961 -0.00072 0.00126 0.01923 C55 1 0.588476 0.261016 1.013008 11.00000 0.04962 0.05270 = 0.05363 0.00723 0.00763 0.01919 AFIX 23 H55A 2 0.516486 0.255370 1.009193 11.00000 -1.20000 H55B 2 0.616459 0.287814 1.067671 11.00000 -1.20000 AFIX 0 C29 1 0.166296 0.620817 0.547727 11.00000 0.04892 0.05036 = 0.04364 -0.00116 -0.00211 0.02317 AFIX 43 H29 2 0.097413 0.597216 0.531600 11.00000 -1.20000 AFIX 0 C47 1 0.895994 0.861811 0.779832 11.00000 0.05039 0.05295 = 0.04732 0.00379 -0.00130 0.01978 AFIX 43 H47 2 0.854880 0.887179 0.811567 11.00000 -1.20000 AFIX 0 C56 1 0.603709 0.164962 1.000175 11.00000 0.05041 0.04969 = 0.05517 0.00617 0.00352 0.01835 AFIX 23 H56A 2 0.561140 0.119584 1.037043 11.00000 -1.20000 H56B 2 0.581997 0.142548 0.943209 11.00000 -1.20000 AFIX 0 C8 1 0.464570 0.758427 0.775375 11.00000 0.05367 0.05483 = 0.04619 -0.00494 0.00454 0.02418 AFIX 43 H8 2 0.454666 0.692717 0.780856 11.00000 -1.20000 AFIX 0 C44 1 1.015057 0.788429 0.685553 11.00000 0.04567 0.07113 = 0.04317 0.00514 -0.00215 0.02324 AFIX 43 H44 2 1.055739 0.763336 0.653093 11.00000 -1.20000 AFIX 0 C12 1 0.415537 0.885782 0.715815 11.00000 0.05632 0.05932 = 0.05653 -0.00172 0.00748 0.02461 AFIX 43 H12 2 0.370948 0.907814 0.681862 11.00000 -1.20000 AFIX 0 C16 1 0.666240 0.484741 0.586314 11.00000 0.05512 0.06924 = 0.04175 0.00656 0.00723 0.03108 AFIX 43 H16 2 0.727461 0.472859 0.576555 11.00000 -1.20000 AFIX 0 C20 1 0.096608 0.254528 0.503166 11.00000 0.04834 0.05612 = 0.05009 -0.00352 -0.00230 0.01958 AFIX 23 H20A 2 0.114146 0.274686 0.447005 11.00000 -1.20000 H20B 2 0.024775 0.246619 0.508299 11.00000 -1.20000 AFIX 0 C45 1 1.036467 0.885101 0.696171 11.00000 0.04612 0.07166 = 0.04603 0.00905 -0.00431 0.01296 AFIX 43 H45 2 1.091573 0.926465 0.670863 11.00000 -1.20000 AFIX 0 C39 1 0.613626 0.496649 0.822373 11.00000 0.04933 0.05083 = 0.03849 0.00239 0.00180 0.02176 AFIX 13 H39 2 0.632013 0.497020 0.764136 11.00000 -1.20000 AFIX 0 C23 1 0.246473 0.161666 0.418166 11.00000 0.05929 0.04987 = 0.05016 -0.00086 -0.00289 0.02282 AFIX 43 H23 2 0.196618 0.158053 0.375960 11.00000 -1.20000 AFIX 0 C17 1 0.665836 0.574107 0.611318 11.00000 0.05041 0.06241 = 0.04342 0.00287 0.00106 0.01953 AFIX 43 H17 2 0.726732 0.623779 0.618001 11.00000 -1.20000 AFIX 0 C50 1 1.144492 0.554789 0.893958 11.00000 0.04551 0.05740 = 0.04655 -0.00277 -0.00124 0.01994 AFIX 43 H50 2 1.204881 0.603465 0.886934 11.00000 -1.20000 AFIX 0 C63 1 0.502884 0.474006 0.832037 11.00000 0.04795 0.05329 = 0.04527 -0.00093 -0.00339 0.01990 AFIX 137 H63A 2 0.467914 0.415085 0.802055 11.00000 -1.50000 H63B 2 0.479568 0.525327 0.810212 11.00000 -1.50000 H63C 2 0.489271 0.466907 0.890118 11.00000 -1.50000 AFIX 0 C9 1 0.544263 0.823078 0.817916 11.00000 0.04978 0.06839 = 0.04918 -0.00888 0.00431 0.02423 AFIX 43 H9 2 0.587916 0.801506 0.853293 11.00000 -1.20000 AFIX 0 C27 1 0.296677 0.170056 0.560030 11.00000 0.06297 0.05924 = 0.04687 0.00240 0.00307 0.02333 AFIX 43 H27 2 0.282050 0.172259 0.615900 11.00000 -1.20000 AFIX 0 C21 1 0.118607 0.162338 0.520030 11.00000 0.05360 0.05060 = 0.06060 -0.00257 0.00249 0.01825 AFIX 23 H21A 2 0.109980 0.147990 0.578591 11.00000 -1.20000 H21B 2 0.069892 0.110896 0.487582 11.00000 -1.20000 AFIX 0 C62 1 0.753652 0.179853 1.095287 11.00000 0.06445 0.05050 = 0.04512 0.00301 0.00300 0.02301 AFIX 43 H62 2 0.715672 0.189621 1.139073 11.00000 -1.20000 AFIX 0 C49 1 1.053466 0.570125 0.875417 11.00000 0.05374 0.05315 = 0.04464 0.00141 0.00150 0.02439 AFIX 43 H49 2 1.051975 0.629410 0.855181 11.00000 -1.20000 AFIX 0 C68 1 0.586157 0.811292 1.187679 11.00000 0.06417 0.05655 = 0.06062 -0.00019 0.01224 0.02301 AFIX 137 H68A 2 0.545957 0.766393 1.145936 11.00000 -1.50000 H68B 2 0.547136 0.850719 1.207910 11.00000 -1.50000 H68C 2 0.605217 0.776701 1.233112 11.00000 -1.50000 AFIX 0 C58 1 0.767458 0.152260 0.953748 11.00000 0.05677 0.06440 = 0.04258 0.00238 -0.00182 0.02434 AFIX 43 H58 2 0.739443 0.142996 0.899233 11.00000 -1.20000 AFIX 0 C15 1 0.577560 0.413266 0.575681 11.00000 0.06825 0.05831 = 0.04556 0.00084 0.00436 0.03355 AFIX 43 H15 2 0.577889 0.352335 0.557831 11.00000 -1.20000 AFIX 0 C10 1 0.559982 0.918545 0.808781 11.00000 0.05011 0.06476 = 0.05694 -0.01124 0.00709 0.01377 AFIX 43 H10 2 0.613914 0.962807 0.838328 11.00000 -1.20000 AFIX 0 C46 1 0.977094 0.921244 0.743916 11.00000 0.05657 0.05233 = 0.05320 0.00352 -0.00820 0.01516 AFIX 43 H46 2 0.992403 0.987555 0.751973 11.00000 -1.20000 AFIX 0 C61 1 0.850870 0.179183 1.111151 11.00000 0.06730 0.05368 = 0.04961 0.00298 -0.00987 0.02290 AFIX 43 H61 2 0.879078 0.188458 1.165607 11.00000 -1.20000 AFIX 0 C28 1 0.029273 0.489261 0.666377 11.00000 0.05133 0.05958 = 0.05017 0.00098 0.00631 0.02326 AFIX 137 H28A 2 0.007289 0.473410 0.608924 11.00000 -1.50000 H28B 2 0.007106 0.542388 0.684546 11.00000 -1.50000 H28C 2 0.000497 0.434542 0.699903 11.00000 -1.50000 AFIX 0 C60 1 0.906633 0.165227 1.048793 11.00000 0.05184 0.06946 = 0.06363 0.00615 -0.00529 0.02392 AFIX 43 H60 2 0.973491 0.165057 1.059793 11.00000 -1.20000 AFIX 0 C51 1 1.146942 0.467330 0.923040 11.00000 0.05372 0.06421 = 0.04397 -0.00576 -0.00576 0.03136 AFIX 43 H51 2 1.209024 0.456042 0.935253 11.00000 -1.20000 AFIX 0 C67 1 0.679911 0.873727 1.150403 11.00000 0.05601 0.05867 = 0.05391 -0.00629 0.00279 0.01765 C52 1 1.059449 0.397995 0.933845 11.00000 0.06346 0.05381 = 0.04611 -0.00053 -0.00503 0.03129 AFIX 43 H52 2 1.061298 0.338869 0.954217 11.00000 -1.20000 AFIX 0 C24 1 0.341139 0.163513 0.397647 11.00000 0.06993 0.06021 = 0.04768 0.00104 0.00766 0.02819 AFIX 43 H24 2 0.356099 0.161182 0.341869 11.00000 -1.20000 AFIX 0 C32 1 0.163690 0.833498 0.313913 11.00000 0.05770 0.05877 = 0.05345 0.00867 0.00461 0.02248 C26 1 0.391226 0.171915 0.539770 11.00000 0.05475 0.07427 = 0.05765 0.00342 -0.00377 0.02776 AFIX 43 H26 2 0.441166 0.175386 0.581869 11.00000 -1.20000 AFIX 0 C33 1 0.208593 0.931210 0.278716 11.00000 0.06820 0.05746 = 0.04891 0.00645 0.00086 0.02498 AFIX 137 H33A 2 0.194188 0.978994 0.313581 11.00000 -1.50000 H33B 2 0.179392 0.932790 0.223394 11.00000 -1.50000 H33C 2 0.280945 0.944396 0.276642 11.00000 -1.50000 AFIX 0 C70 1 0.744150 0.944098 1.214849 11.00000 0.06932 0.05604 = 0.05467 -0.00819 0.00122 0.02233 AFIX 137 H70A 2 0.764788 0.909663 1.259663 11.00000 -1.50000 H70B 2 0.705416 0.983182 1.236221 11.00000 -1.50000 H70C 2 0.803354 0.984482 1.189904 11.00000 -1.50000 AFIX 0 C11 1 0.497061 0.949487 0.756559 11.00000 0.06759 0.05188 = 0.06635 -0.00383 0.01352 0.01714 AFIX 43 H11 2 0.509749 1.015156 0.748441 11.00000 -1.20000 AFIX 0 C69 1 0.649383 0.929549 1.079989 11.00000 0.06317 0.05853 = 0.07097 -0.00123 -0.00107 0.02522 AFIX 137 H69A 2 0.709361 0.971370 1.057153 11.00000 -1.50000 H69B 2 0.608986 0.967261 1.100952 11.00000 -1.50000 H69C 2 0.610435 0.885427 1.037191 11.00000 -1.50000 AFIX 0 C25 1 0.414068 0.168788 0.459015 11.00000 0.05469 0.06697 = 0.06540 0.00368 0.00984 0.02532 AFIX 43 H25 2 0.479420 0.170243 0.445571 11.00000 -1.20000 AFIX 0 C59 1 0.865095 0.151369 0.969654 11.00000 0.05556 0.08057 = 0.05584 0.00345 0.00633 0.02966 AFIX 43 H59 2 0.903308 0.141241 0.926166 11.00000 -1.20000 AFIX 0 C34 1 0.051972 0.810522 0.315812 11.00000 0.06139 0.08125 = 0.05466 0.00677 -0.00454 0.02326 AFIX 137 H34A 2 0.024362 0.747598 0.337976 11.00000 -1.50000 H34B 2 0.023421 0.811733 0.260202 11.00000 -1.50000 H34C 2 0.035518 0.857300 0.350494 11.00000 -1.50000 AFIX 0 C31 1 0.198249 0.907759 0.494806 11.00000 0.08752 0.06659 = 0.05655 -0.00090 -0.00070 0.02714 AFIX 137 H31A 2 0.126930 0.901941 0.491210 11.00000 -1.50000 H31B 2 0.236803 0.972962 0.484394 11.00000 -1.50000 H31C 2 0.217048 0.890787 0.549605 11.00000 -1.50000 AFIX 0 C66 1 0.866294 0.870602 1.058105 11.00000 0.06217 0.07203 = 0.09470 -0.02211 0.01884 0.01567 AFIX 137 H66A 2 0.897625 0.827953 1.031872 11.00000 -1.50000 H66B 2 0.913530 0.910770 1.099094 11.00000 -1.50000 H66C 2 0.847287 0.910161 1.016735 11.00000 -1.50000 AFIX 0 C30 1 0.360008 0.853112 0.413626 11.00000 0.05205 0.09554 = 0.08801 0.02653 0.00077 0.02181 AFIX 137 H30A 2 0.388166 0.846105 0.468254 11.00000 -1.50000 H30B 2 0.388613 0.918064 0.396118 11.00000 -1.50000 H30C 2 0.375781 0.809556 0.374961 11.00000 -1.50000 AFIX 0 C35 1 0.183986 0.757516 0.256318 11.00000 0.09026 0.07235 = 0.05386 -0.00109 0.00815 0.03195 AFIX 137 H35A 2 0.256033 0.770761 0.251804 11.00000 -1.50000 H35B 2 0.152205 0.759282 0.202020 11.00000 -1.50000 H35C 2 0.156443 0.694871 0.279024 11.00000 -1.50000 AFIX 0 C65 1 0.791925 0.730221 1.190615 11.00000 0.07917 0.08654 = 0.06517 0.00136 -0.00690 0.04349 AFIX 137 H65A 2 0.732545 0.694572 1.218226 11.00000 -1.50000 H65B 2 0.839153 0.772579 1.230307 11.00000 -1.50000 H65C 2 0.823407 0.686343 1.166597 11.00000 -1.50000 AFIX 0 HKLF 5 REM hpd873_twin1_hklf4_a.res in P-1 REM wR2 = 0.1432, GooF = S = 1.002, Restrained GooF = 1.002 for all data REM R1 = 0.0669 for 20241 Fo > 4sig(Fo) and 0.0737 for all 23211 data REM 788 parameters refined using 0 restraints END WGHT 0.1043 1.2372 REM Highest difference peak 0.900, deepest hole -0.567, 1-sigma level 0.054 Q1 1 0.7353 0.8431 1.0702 11.00000 0.05 0.90 Q2 1 0.2601 0.8026 0.3826 11.00000 0.05 0.84 Q3 1 0.3179 0.7607 0.3204 11.00000 0.05 0.48 Q4 1 0.1216 0.9190 0.4063 11.00000 0.05 0.43 Q5 1 0.3426 0.9001 0.4630 11.00000 0.05 0.41 Q6 1 0.7104 0.9191 1.0046 11.00000 0.05 0.39 Q7 1 0.7213 0.7616 1.2338 11.00000 0.05 0.36 Q8 1 0.7021 0.8174 1.1478 11.00000 0.05 0.34 Q9 1 0.3004 0.8731 0.4307 11.00000 0.05 0.33 Q10 1 0.7654 0.8810 1.1209 11.00000 0.05 0.30 ; _shelx_res_checksum 80279 _olex2_exptl_crystal_mounting_method 'nylon loop' _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 2.083 _oxdiff_exptl_absorpt_empirical_full_min 0.472 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.22506(7) 0.82634(7) 0.41650(6) 0.0547(2) Uani 1 1 d . . . . . Si2 Si 0.75497(7) 0.80130(7) 1.10785(6) 0.0539(2) Uani 1 1 d . . . . . O3 O 0.15555(15) 0.32425(14) 0.56219(12) 0.0477(5) Uani 1 1 d . . . . . O6 O 0.59556(16) 0.43989(15) 1.00619(12) 0.0493(5) Uani 1 1 d . . . . . O7 O 0.63941(15) 0.32113(14) 0.94961(12) 0.0468(5) Uani 1 1 d . . . . . O5 O 0.70239(15) 0.72575(15) 0.79559(13) 0.0499(5) Uani 1 1 d . . . . . O2 O 0.09800(16) 0.43106(15) 0.49703(12) 0.0507(5) Uani 1 1 d . . . . . O4 O 0.17024(16) 0.71576(15) 0.44348(13) 0.0534(5) Uani 1 1 d . . . . . O8 O 0.67427(16) 0.72722(15) 1.04132(13) 0.0508(5) Uani 1 1 d . . . . . O1 O 0.22540(16) 0.74536(16) 0.69292(14) 0.0566(5) Uani 1 1 d . . . . . N2 N 0.39381(18) 0.62613(18) 0.63513(14) 0.0447(5) Uani 1 1 d . . . . . N1 N 0.30203(18) 0.63991(18) 0.65419(14) 0.0455(6) Uani 1 1 d . . . . . N4 N 0.77937(18) 0.62107(17) 0.83920(14) 0.0436(5) Uani 1 1 d . . . . . N5 N 0.87179(17) 0.60637(17) 0.86026(14) 0.0428(5) Uani 1 1 d . . . . . N6 N 0.72106(19) 0.68166(18) 0.98530(15) 0.0474(6) Uani 1 1 d . . . . . N3 N 0.2239(2) 0.68735(19) 0.50940(15) 0.0506(6) Uani 1 1 d . . . . . C54 C 0.6361(2) 0.4103(2) 0.95319(18) 0.0433(6) Uani 1 1 d . . . . . C1 C 0.3916(2) 0.5384(2) 0.63322(17) 0.0444(6) Uani 1 1 d . . . . . C36 C 0.8678(2) 0.5185(2) 0.86644(17) 0.0431(6) Uani 1 1 d . . . . . C38 C 0.6832(2) 0.4640(2) 0.88178(17) 0.0426(6) Uani 1 1 d . . . . . C3 C 0.2043(2) 0.4765(2) 0.61954(17) 0.0444(6) Uani 1 1 d . . . . . C41 C 0.7801(2) 0.7045(2) 0.80300(17) 0.0447(6) Uani 1 1 d . . . . . C6 C 0.3034(2) 0.7257(2) 0.68818(18) 0.0487(7) Uani 1 1 d . . . . . C19 C 0.1481(2) 0.4118(2) 0.55230(18) 0.0446(6) Uani 1 1 d . . . . . C57 C 0.7108(2) 0.1664(2) 1.01617(18) 0.0464(7) Uani 1 1 d . . . . . C42 C 0.8744(2) 0.7642(2) 0.76943(17) 0.0450(6) Uani 1 1 d . . . . . C13 C 0.4864(2) 0.5192(2) 0.61637(17) 0.0445(7) Uani 1 1 d . . . . . C7 C 0.3994(2) 0.7897(2) 0.72484(18) 0.0477(7) Uani 1 1 d . . . . . C40 C 0.6894(2) 0.5679(2) 0.87674(17) 0.0423(6) Uani 1 1 d . . . . . C5 C 0.2084(2) 0.5808(2) 0.61785(18) 0.0455(7) Uani 1 1 d . . . . . C4 C 0.1415(2) 0.5161(2) 0.67524(18) 0.0472(7) Uani 1 1 d . . . . . H4 H 0.168120 0.525152 0.733444 0.057 Uiso 1 1 calc R U . . . C48 C 0.9645(2) 0.5001(2) 0.88600(17) 0.0444(6) Uani 1 1 d . . . . . C37 C 0.7726(2) 0.4408(2) 0.84845(19) 0.0474(7) Uani 1 1 d . . . . . H37A H 0.778418 0.381960 0.873037 0.057 Uiso 1 1 calc R U . . . H37B H 0.761647 0.429752 0.788549 0.057 Uiso 1 1 calc R U . . . C14 C 0.4879(2) 0.4294(2) 0.59077(18) 0.0492(7) Uani 1 1 d . . . . . H14 H 0.427306 0.379466 0.583746 0.059 Uiso 1 1 calc R U . . . C64 C 0.6565(2) 0.6196(2) 0.94246(17) 0.0431(6) Uani 1 1 d . . . . . H64 H 0.587723 0.606131 0.952125 0.052 Uiso 1 1 calc R U . . . C18 C 0.5766(2) 0.5908(2) 0.62651(18) 0.0489(7) Uani 1 1 d . . . . . H18 H 0.576880 0.651979 0.644117 0.059 Uiso 1 1 calc R U . . . C2 C 0.3004(2) 0.4616(2) 0.65486(19) 0.0478(7) Uani 1 1 d . . . . . H2A H 0.298229 0.458747 0.715122 0.057 Uiso 1 1 calc R U . . . H2B H 0.305121 0.400319 0.634195 0.057 Uiso 1 1 calc R U . . . C53 C 0.9681(2) 0.4130(2) 0.91543(18) 0.0470(7) Uani 1 1 d . . . . . H53 H 0.908009 0.364051 0.922794 0.056 Uiso 1 1 calc R U . . . C43 C 0.9346(2) 0.7284(2) 0.72209(18) 0.0481(7) Uani 1 1 d . . . . . H43 H 0.920370 0.662059 0.714753 0.058 Uiso 1 1 calc R U . . . C22 C 0.2227(2) 0.1650(2) 0.49935(19) 0.0484(7) Uani 1 1 d . . . . . C55 C 0.5885(2) 0.2610(2) 1.0130(2) 0.0509(7) Uani 1 1 d . . . . . H55A H 0.516486 0.255370 1.009193 0.061 Uiso 1 1 calc R U . . . H55B H 0.616459 0.287814 1.067671 0.061 Uiso 1 1 calc R U . . . C29 C 0.1663(2) 0.6208(2) 0.54773(18) 0.0460(7) Uani 1 1 d . . . . . H29 H 0.097413 0.597216 0.531600 0.055 Uiso 1 1 calc R U . . . C47 C 0.8960(2) 0.8618(2) 0.77983(19) 0.0494(7) Uani 1 1 d . . . . . H47 H 0.854880 0.887179 0.811567 0.059 Uiso 1 1 calc R U . . . C56 C 0.6037(2) 0.1650(2) 1.0002(2) 0.0510(7) Uani 1 1 d . . . . . H56A H 0.561140 0.119584 1.037043 0.061 Uiso 1 1 calc R U . . . H56B H 0.581997 0.142548 0.943209 0.061 Uiso 1 1 calc R U . . . C8 C 0.4646(2) 0.7584(2) 0.77537(18) 0.0498(7) Uani 1 1 d . . . . . H8 H 0.454666 0.692717 0.780856 0.060 Uiso 1 1 calc R U . . . C44 C 1.0151(2) 0.7884(2) 0.68555(18) 0.0522(7) Uani 1 1 d . . . . . H44 H 1.055739 0.763336 0.653093 0.063 Uiso 1 1 calc R U . . . C12 C 0.4155(3) 0.8858(2) 0.7158(2) 0.0557(8) Uani 1 1 d . . . . . H12 H 0.370948 0.907814 0.681862 0.067 Uiso 1 1 calc R U . . . C16 C 0.6662(2) 0.4847(2) 0.58631(18) 0.0525(7) Uani 1 1 d . . . . . H16 H 0.727461 0.472859 0.576555 0.063 Uiso 1 1 calc R U . . . C20 C 0.0966(2) 0.2545(2) 0.50317(19) 0.0509(7) Uani 1 1 d . . . . . H20A H 0.114146 0.274686 0.447005 0.061 Uiso 1 1 calc R U . . . H20B H 0.024775 0.246619 0.508299 0.061 Uiso 1 1 calc R U . . . C45 C 1.0365(2) 0.8851(3) 0.69617(19) 0.0558(8) Uani 1 1 d . . . . . H45 H 1.091573 0.926465 0.670863 0.067 Uiso 1 1 calc R U . . . C39 C 0.6136(2) 0.4966(2) 0.82237(17) 0.0447(6) Uani 1 1 d . . . . . H39 H 0.632013 0.497020 0.764136 0.054 Uiso 1 1 calc R U . . . C23 C 0.2465(2) 0.1617(2) 0.41817(19) 0.0519(7) Uani 1 1 d . . . . . H23 H 0.196618 0.158053 0.375960 0.062 Uiso 1 1 calc R U . . . C17 C 0.6658(2) 0.5741(2) 0.61132(18) 0.0515(7) Uani 1 1 d . . . . . H17 H 0.726732 0.623779 0.618001 0.062 Uiso 1 1 calc R U . . . C50 C 1.1445(2) 0.5548(2) 0.89396(18) 0.0490(7) Uani 1 1 d . . . . . H50 H 1.204881 0.603465 0.886934 0.059 Uiso 1 1 calc R U . . . C63 C 0.5029(2) 0.4740(2) 0.83204(18) 0.0480(7) Uani 1 1 d . . . . . H63A H 0.467914 0.415085 0.802055 0.072 Uiso 1 1 calc R U . . . H63B H 0.479568 0.525327 0.810212 0.072 Uiso 1 1 calc R U . . . H63C H 0.489271 0.466907 0.890118 0.072 Uiso 1 1 calc R U . . . C9 C 0.5443(2) 0.8231(2) 0.81792(19) 0.0544(8) Uani 1 1 d . . . . . H9 H 0.587916 0.801506 0.853293 0.065 Uiso 1 1 calc R U . . . C27 C 0.2967(3) 0.1701(2) 0.5600(2) 0.0552(8) Uani 1 1 d . . . . . H27 H 0.282050 0.172259 0.615900 0.066 Uiso 1 1 calc R U . . . C21 C 0.1186(2) 0.1623(2) 0.5200(2) 0.0544(8) Uani 1 1 d . . . . . H21A H 0.109980 0.147990 0.578591 0.065 Uiso 1 1 calc R U . . . H21B H 0.069892 0.110896 0.487582 0.065 Uiso 1 1 calc R U . . . C62 C 0.7537(3) 0.1799(2) 1.09529(19) 0.0521(7) Uani 1 1 d . . . . . H62 H 0.715672 0.189621 1.139073 0.062 Uiso 1 1 calc R U . . . C49 C 1.0535(2) 0.5701(2) 0.87542(18) 0.0487(7) Uani 1 1 d . . . . . H49 H 1.051975 0.629410 0.855181 0.058 Uiso 1 1 calc R U . . . C68 C 0.5862(3) 0.8113(2) 1.1877(2) 0.0591(8) Uani 1 1 d . . . . . H68A H 0.545957 0.766393 1.145936 0.089 Uiso 1 1 calc R U . . . H68B H 0.547136 0.850719 1.207910 0.089 Uiso 1 1 calc R U . . . H68C H 0.605217 0.776701 1.233112 0.089 Uiso 1 1 calc R U . . . C58 C 0.7675(2) 0.1523(2) 0.95375(19) 0.0534(8) Uani 1 1 d . . . . . H58 H 0.739443 0.142996 0.899233 0.064 Uiso 1 1 calc R U . . . C15 C 0.5776(3) 0.4133(2) 0.57568(19) 0.0541(8) Uani 1 1 d . . . . . H15 H 0.577889 0.352335 0.557831 0.065 Uiso 1 1 calc R U . . . C10 C 0.5600(3) 0.9185(3) 0.8088(2) 0.0580(8) Uani 1 1 d . . . . . H10 H 0.613914 0.962807 0.838328 0.070 Uiso 1 1 calc R U . . . C46 C 0.9771(2) 0.9212(2) 0.7439(2) 0.0547(8) Uani 1 1 d . . . . . H46 H 0.992403 0.987555 0.751973 0.066 Uiso 1 1 calc R U . . . C61 C 0.8509(3) 0.1792(2) 1.1112(2) 0.0562(8) Uani 1 1 d . . . . . H61 H 0.879078 0.188458 1.165607 0.067 Uiso 1 1 calc R U . . . C28 C 0.0293(2) 0.4893(2) 0.6664(2) 0.0521(7) Uani 1 1 d . . . . . H28A H 0.007289 0.473410 0.608924 0.078 Uiso 1 1 calc R U . . . H28B H 0.007106 0.542388 0.684546 0.078 Uiso 1 1 calc R U . . . H28C H 0.000497 0.434542 0.699903 0.078 Uiso 1 1 calc R U . . . C60 C 0.9066(3) 0.1652(3) 1.0488(2) 0.0606(8) Uani 1 1 d . . . . . H60 H 0.973491 0.165057 1.059793 0.073 Uiso 1 1 calc R U . . . C51 C 1.1469(2) 0.4673(2) 0.92304(18) 0.0513(7) Uani 1 1 d . . . . . H51 H 1.209024 0.456042 0.935253 0.062 Uiso 1 1 calc R U . . . C67 C 0.6799(3) 0.8737(2) 1.1504(2) 0.0562(8) Uani 1 1 d . . . . . C52 C 1.0594(3) 0.3980(2) 0.93385(19) 0.0517(7) Uani 1 1 d . . . . . H52 H 1.061298 0.338869 0.954217 0.062 Uiso 1 1 calc R U . . . C24 C 0.3411(3) 0.1635(2) 0.3976(2) 0.0572(8) Uani 1 1 d . . . . . H24 H 0.356099 0.161182 0.341869 0.069 Uiso 1 1 calc R U . . . C32 C 0.1637(3) 0.8335(2) 0.3139(2) 0.0554(8) Uani 1 1 d . . . . . C26 C 0.3912(3) 0.1719(3) 0.5398(2) 0.0606(8) Uani 1 1 d . . . . . H26 H 0.441166 0.175386 0.581869 0.073 Uiso 1 1 calc R U . . . C33 C 0.2086(3) 0.9312(2) 0.2787(2) 0.0569(8) Uani 1 1 d . . . . . H33A H 0.194188 0.978994 0.313581 0.085 Uiso 1 1 calc R U . . . H33B H 0.179392 0.932790 0.223394 0.085 Uiso 1 1 calc R U . . . H33C H 0.280945 0.944396 0.276642 0.085 Uiso 1 1 calc R U . . . C70 C 0.7441(3) 0.9441(2) 1.2148(2) 0.0594(8) Uani 1 1 d . . . . . H70A H 0.764788 0.909663 1.259663 0.089 Uiso 1 1 calc R U . . . H70B H 0.705416 0.983182 1.236221 0.089 Uiso 1 1 calc R U . . . H70C H 0.803354 0.984482 1.189904 0.089 Uiso 1 1 calc R U . . . C11 C 0.4971(3) 0.9495(3) 0.7566(2) 0.0618(9) Uani 1 1 d . . . . . H11 H 0.509749 1.015156 0.748441 0.074 Uiso 1 1 calc R U . . . C69 C 0.6494(3) 0.9295(3) 1.0800(2) 0.0629(9) Uani 1 1 d . . . . . H69A H 0.709361 0.971370 1.057153 0.094 Uiso 1 1 calc R U . . . H69B H 0.608986 0.967261 1.100952 0.094 Uiso 1 1 calc R U . . . H69C H 0.610435 0.885427 1.037191 0.094 Uiso 1 1 calc R U . . . C25 C 0.4141(3) 0.1688(3) 0.4590(2) 0.0606(8) Uani 1 1 d . . . . . H25 H 0.479420 0.170243 0.445571 0.073 Uiso 1 1 calc R U . . . C59 C 0.8651(3) 0.1514(3) 0.9697(2) 0.0618(9) Uani 1 1 d . . . . . H59 H 0.903308 0.141241 0.926166 0.074 Uiso 1 1 calc R U . . . C34 C 0.0520(3) 0.8105(3) 0.3158(2) 0.0656(9) Uani 1 1 d . . . . . H34A H 0.024362 0.747598 0.337976 0.098 Uiso 1 1 calc R U . . . H34B H 0.023421 0.811733 0.260202 0.098 Uiso 1 1 calc R U . . . H34C H 0.035518 0.857300 0.350494 0.098 Uiso 1 1 calc R U . . . C31 C 0.1982(3) 0.9078(3) 0.4948(2) 0.0695(10) Uani 1 1 d . . . . . H31A H 0.126930 0.901941 0.491210 0.104 Uiso 1 1 calc R U . . . H31B H 0.236803 0.972962 0.484394 0.104 Uiso 1 1 calc R U . . . H31C H 0.217048 0.890787 0.549605 0.104 Uiso 1 1 calc R U . . . C66 C 0.8663(3) 0.8706(3) 1.0581(3) 0.0769(11) Uani 1 1 d . . . . . H66A H 0.897625 0.827953 1.031872 0.115 Uiso 1 1 calc R U . . . H66B H 0.913530 0.910770 1.099094 0.115 Uiso 1 1 calc R U . . . H66C H 0.847287 0.910161 1.016735 0.115 Uiso 1 1 calc R U . . . C30 C 0.3600(3) 0.8531(3) 0.4136(3) 0.0785(12) Uani 1 1 d . . . . . H30A H 0.388166 0.846105 0.468254 0.118 Uiso 1 1 calc R U . . . H30B H 0.388613 0.918064 0.396118 0.118 Uiso 1 1 calc R U . . . H30C H 0.375781 0.809556 0.374961 0.118 Uiso 1 1 calc R U . . . C35 C 0.1840(3) 0.7575(3) 0.2563(2) 0.0704(10) Uani 1 1 d . . . . . H35A H 0.256033 0.770761 0.251804 0.106 Uiso 1 1 calc R U . . . H35B H 0.152205 0.759282 0.202020 0.106 Uiso 1 1 calc R U . . . H35C H 0.156443 0.694871 0.279024 0.106 Uiso 1 1 calc R U . . . C65 C 0.7919(3) 0.7302(3) 1.1906(2) 0.0732(11) Uani 1 1 d . . . . . H65A H 0.732545 0.694572 1.218226 0.110 Uiso 1 1 calc R U . . . H65B H 0.839153 0.772579 1.230307 0.110 Uiso 1 1 calc R U . . . H65C H 0.823407 0.686343 1.166597 0.110 Uiso 1 1 calc R 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 Si1 0.0562(5) 0.0558(5) 0.0525(5) 0.0069(4) -0.0053(4) 0.0184(4) Si2 0.0515(5) 0.0573(5) 0.0541(5) -0.0059(4) 0.0023(4) 0.0187(4) O3 0.0515(12) 0.0492(12) 0.0459(11) -0.0012(9) -0.0039(9) 0.0216(10) O6 0.0536(12) 0.0551(12) 0.0456(11) 0.0028(9) 0.0078(9) 0.0252(10) O7 0.0503(12) 0.0467(11) 0.0481(11) 0.0050(9) 0.0055(9) 0.0210(9) O5 0.0488(12) 0.0541(12) 0.0534(12) 0.0064(9) 0.0018(9) 0.0256(10) O2 0.0538(12) 0.0573(13) 0.0461(11) 0.0016(9) -0.0058(9) 0.0255(10) O4 0.0609(14) 0.0572(13) 0.0484(12) 0.0069(10) -0.0052(10) 0.0284(11) O8 0.0508(12) 0.0572(13) 0.0501(12) -0.0076(9) 0.0006(9) 0.0254(10) O1 0.0542(13) 0.0649(14) 0.0586(13) -0.0101(11) -0.0016(10) 0.0309(11) N2 0.0440(13) 0.0535(15) 0.0407(13) -0.0014(10) 0.0015(10) 0.0213(11) N1 0.0465(14) 0.0523(14) 0.0432(13) -0.0018(11) 0.0004(10) 0.0236(12) N4 0.0432(13) 0.0487(14) 0.0443(13) 0.0037(10) 0.0024(10) 0.0220(11) N5 0.0408(13) 0.0506(14) 0.0413(12) 0.0034(10) -0.0002(10) 0.0202(11) N6 0.0484(14) 0.0542(15) 0.0457(13) -0.0027(11) 0.0020(11) 0.0249(12) N3 0.0559(16) 0.0533(15) 0.0472(14) 0.0054(12) -0.0039(12) 0.0242(13) C54 0.0395(15) 0.0482(16) 0.0448(15) 0.0004(12) -0.0024(12) 0.0177(13) C1 0.0496(17) 0.0523(17) 0.0350(14) -0.0005(12) -0.0031(12) 0.0218(14) C36 0.0466(16) 0.0501(17) 0.0375(14) 0.0006(12) 0.0033(12) 0.0217(13) C38 0.0429(15) 0.0452(16) 0.0427(15) 0.0000(12) 0.0019(12) 0.0179(13) C3 0.0466(16) 0.0503(17) 0.0402(15) 0.0027(12) -0.0001(12) 0.0206(13) C41 0.0490(17) 0.0482(16) 0.0410(15) -0.0002(12) -0.0002(12) 0.0214(14) C6 0.0556(18) 0.0545(18) 0.0426(15) 0.0010(13) 0.0023(13) 0.0268(15) C19 0.0413(15) 0.0513(17) 0.0443(15) 0.0021(12) 0.0049(12) 0.0183(13) C57 0.0512(17) 0.0422(16) 0.0488(16) 0.0047(12) 0.0008(13) 0.0187(13) C42 0.0464(16) 0.0517(17) 0.0402(15) 0.0039(12) -0.0041(12) 0.0210(14) C13 0.0510(17) 0.0537(17) 0.0342(14) 0.0025(12) -0.0001(12) 0.0242(14) C7 0.0517(17) 0.0524(17) 0.0429(15) -0.0043(13) 0.0065(13) 0.0210(14) C40 0.0424(15) 0.0473(16) 0.0411(15) 0.0026(12) 0.0019(12) 0.0192(13) C5 0.0476(16) 0.0510(17) 0.0420(15) 0.0002(12) 0.0005(12) 0.0214(14) C4 0.0514(17) 0.0546(18) 0.0404(15) -0.0007(13) 0.0010(13) 0.0231(14) C48 0.0498(17) 0.0516(17) 0.0378(14) -0.0016(12) 0.0007(12) 0.0247(14) C37 0.0504(17) 0.0507(17) 0.0458(16) 0.0000(13) 0.0039(13) 0.0220(14) C14 0.0536(18) 0.0516(17) 0.0447(16) 0.0008(13) 0.0005(13) 0.0196(14) C64 0.0447(16) 0.0474(16) 0.0421(15) 0.0026(12) 0.0011(12) 0.0212(13) C18 0.0563(19) 0.0538(18) 0.0414(15) 0.0013(13) 0.0007(13) 0.0242(15) C2 0.0501(17) 0.0523(17) 0.0452(16) 0.0022(13) -0.0030(13) 0.0227(14) C53 0.0520(17) 0.0500(17) 0.0422(15) 0.0000(12) 0.0015(13) 0.0204(14) C43 0.0511(17) 0.0555(18) 0.0421(15) 0.0041(13) -0.0018(13) 0.0230(14) C22 0.0537(18) 0.0447(16) 0.0496(17) -0.0007(13) 0.0013(13) 0.0192(14) C55 0.0496(17) 0.0527(18) 0.0536(18) 0.0072(14) 0.0076(14) 0.0192(14) C29 0.0489(17) 0.0504(17) 0.0436(15) -0.0012(13) -0.0021(13) 0.0232(14) C47 0.0504(18) 0.0530(18) 0.0473(16) 0.0038(13) -0.0013(13) 0.0198(14) C56 0.0504(18) 0.0497(17) 0.0552(18) 0.0062(14) 0.0035(14) 0.0183(14) C8 0.0537(18) 0.0548(18) 0.0462(16) -0.0049(13) 0.0045(13) 0.0242(15) C44 0.0457(17) 0.071(2) 0.0432(16) 0.0051(14) -0.0021(13) 0.0232(15) C12 0.0563(19) 0.059(2) 0.0565(19) -0.0017(15) 0.0075(15) 0.0246(16) C16 0.0551(19) 0.069(2) 0.0418(16) 0.0066(14) 0.0072(14) 0.0311(16) C20 0.0483(17) 0.0561(18) 0.0501(17) -0.0035(14) -0.0023(13) 0.0196(15) C45 0.0461(17) 0.072(2) 0.0460(17) 0.0091(15) -0.0043(13) 0.0130(16) C39 0.0493(17) 0.0508(17) 0.0385(14) 0.0024(12) 0.0018(12) 0.0218(14) C23 0.0593(19) 0.0499(17) 0.0502(17) -0.0009(14) -0.0029(14) 0.0228(15) C17 0.0504(18) 0.062(2) 0.0434(16) 0.0029(14) 0.0011(13) 0.0195(15) C50 0.0455(16) 0.0574(18) 0.0466(16) -0.0028(14) -0.0012(13) 0.0199(14) C63 0.0480(17) 0.0533(18) 0.0453(16) -0.0009(13) -0.0034(13) 0.0199(14) C9 0.0498(18) 0.068(2) 0.0492(17) -0.0089(15) 0.0043(14) 0.0242(16) C27 0.063(2) 0.0592(19) 0.0469(17) 0.0024(14) 0.0031(15) 0.0233(16) C21 0.0536(19) 0.0506(18) 0.0606(19) -0.0026(15) 0.0025(15) 0.0183(15) C62 0.064(2) 0.0505(18) 0.0451(16) 0.0030(13) 0.0030(14) 0.0230(15) C49 0.0537(18) 0.0532(18) 0.0446(16) 0.0014(13) 0.0015(13) 0.0244(15) C68 0.064(2) 0.057(2) 0.061(2) -0.0002(16) 0.0122(16) 0.0230(17) C58 0.0568(19) 0.064(2) 0.0426(16) 0.0024(14) -0.0018(14) 0.0243(16) C15 0.068(2) 0.0583(19) 0.0456(17) 0.0008(14) 0.0044(15) 0.0336(17) C10 0.0501(18) 0.065(2) 0.0569(19) -0.0112(16) 0.0071(15) 0.0138(16) C46 0.0566(19) 0.0523(18) 0.0532(18) 0.0035(14) -0.0082(15) 0.0152(15) C61 0.067(2) 0.0537(18) 0.0496(18) 0.0030(14) -0.0099(15) 0.0229(16) C28 0.0513(18) 0.060(2) 0.0502(17) 0.0010(14) 0.0063(14) 0.0233(15) C60 0.0518(19) 0.069(2) 0.064(2) 0.0062(17) -0.0053(16) 0.0239(17) C51 0.0537(19) 0.064(2) 0.0440(16) -0.0058(14) -0.0058(13) 0.0314(16) C67 0.0560(19) 0.059(2) 0.0539(19) -0.0063(15) 0.0028(15) 0.0176(16) C52 0.063(2) 0.0538(18) 0.0461(16) -0.0005(13) -0.0050(14) 0.0313(16) C24 0.070(2) 0.060(2) 0.0477(17) 0.0010(15) 0.0077(15) 0.0282(17) C32 0.0577(19) 0.059(2) 0.0534(18) 0.0087(15) 0.0046(15) 0.0225(16) C26 0.055(2) 0.074(2) 0.058(2) 0.0034(17) -0.0038(15) 0.0278(17) C33 0.068(2) 0.0575(19) 0.0489(17) 0.0065(14) 0.0009(15) 0.0250(17) C70 0.069(2) 0.056(2) 0.0547(19) -0.0082(15) 0.0012(16) 0.0223(17) C11 0.068(2) 0.0519(19) 0.066(2) -0.0038(16) 0.0135(17) 0.0171(17) C69 0.063(2) 0.059(2) 0.071(2) -0.0012(17) -0.0011(17) 0.0252(17) C25 0.055(2) 0.067(2) 0.065(2) 0.0037(17) 0.0098(16) 0.0253(17) C59 0.056(2) 0.081(2) 0.056(2) 0.0034(17) 0.0063(16) 0.0297(18) C34 0.061(2) 0.081(3) 0.055(2) 0.0068(18) -0.0045(16) 0.0233(19) C31 0.088(3) 0.067(2) 0.057(2) -0.0009(17) -0.0007(19) 0.027(2) C66 0.062(2) 0.072(3) 0.095(3) -0.022(2) 0.019(2) 0.0157(19) C30 0.052(2) 0.096(3) 0.088(3) 0.027(2) 0.0008(19) 0.022(2) C35 0.090(3) 0.072(2) 0.054(2) -0.0011(17) 0.0082(19) 0.032(2) C65 0.079(3) 0.087(3) 0.065(2) 0.001(2) -0.0069(19) 0.043(2) 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' N N 0.0311 0.0180 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 2 10 0.0585 8 -7 -1 0.0543 -1 -2 -10 0.0694 -8 7 1 0.0374 -1 -2 10 0.0594 -4 -7 -1 0.0177 2 3 -10 0.0628 4 7 1 0.0432 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 O4 Si1 C32 103.40(14) . . ? O4 Si1 C31 107.91(15) . . ? O4 Si1 C30 112.45(16) . . ? C32 Si1 C31 112.29(16) . . ? C30 Si1 C32 112.71(18) . . ? C30 Si1 C31 108.0(2) . . ? O8 Si2 C67 103.41(13) . . ? O8 Si2 C66 111.44(16) . . ? O8 Si2 C65 108.35(16) . . ? C67 Si2 C65 109.98(17) . . ? C66 Si2 C67 113.87(17) . . ? C66 Si2 C65 109.5(2) . . ? C19 O3 C20 114.8(2) . . ? C54 O7 C55 115.2(2) . . ? N3 O4 Si1 112.38(18) . . ? N6 O8 Si2 113.42(17) . . ? C1 N2 N1 113.7(3) . . ? N2 N1 C5 121.4(2) . . ? C6 N1 N2 118.4(3) . . ? C6 N1 C5 117.5(2) . . ? N5 N4 C40 121.0(2) . . ? C41 N4 N5 118.0(2) . . ? C41 N4 C40 117.9(2) . . ? C36 N5 N4 114.3(2) . . ? C64 N6 O8 110.7(2) . . ? C29 N3 O4 110.6(3) . . ? O6 C54 O7 123.0(3) . . ? O6 C54 C38 125.9(3) . . ? O7 C54 C38 111.0(2) . . ? N2 C1 C13 116.4(3) . . ? N2 C1 C2 121.2(3) . . ? C13 C1 C2 122.1(3) . . ? N5 C36 C48 115.8(3) . . ? N5 C36 C37 121.5(3) . . ? C48 C36 C37 122.6(3) . . ? C54 C38 C40 118.5(2) . . ? C54 C38 C37 117.7(2) . . ? C54 C38 C39 116.1(2) . . ? C40 C38 C37 113.7(2) . . ? C40 C38 C39 59.07(18) . . ? C37 C38 C39 118.7(2) . . ? C19 C3 C5 119.0(2) . . ? C19 C3 C4 115.6(2) . . ? C19 C3 C2 118.0(2) . . ? C4 C3 C5 58.73(19) . . ? C2 C3 C5 113.0(2) . . ? C2 C3 C4 119.1(2) . . ? O5 C41 N4 119.4(3) . . ? O5 C41 C42 121.6(3) . . ? N4 C41 C42 118.9(2) . . ? O1 C6 N1 119.8(3) . . ? O1 C6 C7 120.9(3) . . ? N1 C6 C7 119.1(3) . . ? O3 C19 C3 110.8(2) . . ? O2 C19 O3 122.7(3) . . ? O2 C19 C3 126.4(3) . . ? C62 C57 C56 120.2(3) . . ? C58 C57 C56 121.4(3) . . ? C58 C57 C62 118.4(3) . . ? C43 C42 C41 123.4(3) . . ? C43 C42 C47 119.3(3) . . ? C47 C42 C41 116.9(3) . . ? C14 C13 C1 121.3(3) . . ? C18 C13 C1 120.2(3) . . ? C18 C13 C14 118.5(3) . . ? C8 C7 C6 123.1(3) . . ? C12 C7 C6 116.8(3) . . ? C12 C7 C8 119.6(3) . . ? N4 C40 C38 111.1(2) . . ? N4 C40 C64 114.9(2) . . ? N4 C40 C39 116.3(2) . . ? C64 C40 C38 122.9(2) . . ? C64 C40 C39 120.3(3) . . ? C39 C40 C38 60.69(19) . . ? N1 C5 C3 110.8(2) . . ? N1 C5 C4 115.5(2) . . ? N1 C5 C29 115.7(3) . . ? C4 C5 C3 60.47(19) . . ? C29 C5 C3 122.1(3) . . ? C29 C5 C4 120.9(3) . . ? C5 C4 C3 60.80(19) . . ? C5 C4 C28 123.0(3) . . ? C28 C4 C3 123.4(3) . . ? C53 C48 C36 121.3(3) . . ? C49 C48 C36 120.0(3) . . ? C49 C48 C53 118.8(3) . . ? C36 C37 C38 112.0(3) . . ? C15 C14 C13 120.2(3) . . ? N6 C64 C40 119.3(3) . . ? C17 C18 C13 121.0(3) . . ? C1 C2 C3 112.7(3) . . ? C52 C53 C48 120.0(3) . . ? C44 C43 C42 120.5(3) . . ? C23 C22 C21 120.2(3) . . ? C27 C22 C23 118.4(3) . . ? C27 C22 C21 121.4(3) . . ? O7 C55 C56 107.2(2) . . ? N3 C29 C5 118.8(3) . . ? C46 C47 C42 119.8(3) . . ? C57 C56 C55 112.9(3) . . ? C7 C8 C9 120.1(3) . . ? C43 C44 C45 120.1(3) . . ? C11 C12 C7 119.7(3) . . ? C15 C16 C17 119.8(3) . . ? O3 C20 C21 107.7(2) . . ? C44 C45 C46 119.7(3) . . ? C40 C39 C38 60.25(18) . . ? C40 C39 C63 122.4(3) . . ? C63 C39 C38 123.2(3) . . ? C24 C23 C22 121.3(3) . . ? C18 C17 C16 119.9(3) . . ? C49 C50 C51 119.7(3) . . ? C10 C9 C8 120.0(3) . . ? C26 C27 C22 120.5(3) . . ? C22 C21 C20 112.7(3) . . ? C61 C62 C57 120.9(3) . . ? C50 C49 C48 121.0(3) . . ? C57 C58 C59 120.8(3) . . ? C16 C15 C14 120.6(3) . . ? C9 C10 C11 119.7(3) . . ? C47 C46 C45 120.6(3) . . ? C60 C61 C62 120.3(3) . . ? C61 C60 C59 119.6(3) . . ? C52 C51 C50 119.7(3) . . ? C68 C67 Si2 111.1(2) . . ? C68 C67 C70 110.3(3) . . ? C68 C67 C69 109.2(3) . . ? C70 C67 Si2 109.4(2) . . ? C70 C67 C69 108.5(3) . . ? C69 C67 Si2 108.2(2) . . ? C51 C52 C53 120.9(3) . . ? C23 C24 C25 119.5(3) . . ? C33 C32 Si1 110.1(2) . . ? C33 C32 C35 109.1(3) . . ? C34 C32 Si1 112.9(2) . . ? C34 C32 C33 110.5(3) . . ? C34 C32 C35 106.5(3) . . ? C35 C32 Si1 107.6(2) . . ? C27 C26 C25 120.7(3) . . ? C10 C11 C12 120.7(3) . . ? C26 C25 C24 119.6(3) . . ? C60 C59 C58 120.0(3) . . ? 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 Si1 O4 1.668(2) . ? Si1 C32 1.870(3) . ? Si1 C31 1.881(4) . ? Si1 C30 1.823(4) . ? Si2 O8 1.673(2) . ? Si2 C67 1.869(3) . ? Si2 C66 1.832(4) . ? Si2 C65 1.874(4) . ? O3 C19 1.346(3) . ? O3 C20 1.444(4) . ? O6 C54 1.209(3) . ? O7 C54 1.341(3) . ? O7 C55 1.448(3) . ? O5 C41 1.226(3) . ? O2 C19 1.209(3) . ? O4 N3 1.426(3) . ? O8 N6 1.430(3) . ? O1 C6 1.223(4) . ? N2 N1 1.415(3) . ? N2 C1 1.295(4) . ? N1 C6 1.380(4) . ? N1 C5 1.444(4) . ? N4 N5 1.409(3) . ? N4 C41 1.377(4) . ? N4 C40 1.447(4) . ? N5 C36 1.295(4) . ? N6 C64 1.262(4) . ? N3 C29 1.269(4) . ? C54 C38 1.491(4) . ? C1 C13 1.482(4) . ? C1 C2 1.500(4) . ? C36 C48 1.486(4) . ? C36 C37 1.499(4) . ? C38 C40 1.523(4) . ? C38 C37 1.523(4) . ? C38 C39 1.530(4) . ? C3 C19 1.485(4) . ? C3 C5 1.534(4) . ? C3 C4 1.529(4) . ? C3 C2 1.522(4) . ? C41 C42 1.493(4) . ? C6 C7 1.494(4) . ? C57 C56 1.511(4) . ? C57 C62 1.389(4) . ? C57 C58 1.378(4) . ? C42 C43 1.388(4) . ? C42 C47 1.397(4) . ? C13 C14 1.401(4) . ? C13 C18 1.392(4) . ? C7 C8 1.390(4) . ? C7 C12 1.387(4) . ? C40 C64 1.485(4) . ? C40 C39 1.505(4) . ? C5 C4 1.502(4) . ? C5 C29 1.477(4) . ? C4 C28 1.508(4) . ? C48 C53 1.401(4) . ? C48 C49 1.388(4) . ? C14 C15 1.385(4) . ? C18 C17 1.384(4) . ? C53 C52 1.388(4) . ? C43 C44 1.382(4) . ? C22 C23 1.391(4) . ? C22 C27 1.388(4) . ? C22 C21 1.509(4) . ? C55 C56 1.519(4) . ? C47 C46 1.379(4) . ? C8 C9 1.390(4) . ? C44 C45 1.384(5) . ? C12 C11 1.386(5) . ? C16 C17 1.387(4) . ? C16 C15 1.378(5) . ? C20 C21 1.517(4) . ? C45 C46 1.386(5) . ? C39 C63 1.509(4) . ? C23 C24 1.382(4) . ? C50 C49 1.387(4) . ? C50 C51 1.398(4) . ? C9 C10 1.380(5) . ? C27 C26 1.379(5) . ? C62 C61 1.383(5) . ? C68 C67 1.527(5) . ? C58 C59 1.390(4) . ? C10 C11 1.380(5) . ? C61 C60 1.368(5) . ? C60 C59 1.383(5) . ? C51 C52 1.370(5) . ? C67 C70 1.531(5) . ? C67 C69 1.545(5) . ? C24 C25 1.386(5) . ? C32 C33 1.531(5) . ? C32 C34 1.508(5) . ? C32 C35 1.563(5) . ? C26 C25 1.380(5) . ? 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 0.5668(7) 39929 32442 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4332(7) 39727 32442 nmt -1.0033 -0.0082 -0.0015 0.0090 -0.9975 -0.0013 0.1288 0.0578 0.9998 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 0.2322 1.9393 10.2822 -0.0258 -0.1163 0.9929 7.9065 -7.0463 -1.1386 0.2336 0.9714 -0.0434 -0.6136 -1.6137 -10.2960 0.0147 0.0704 -0.9974 -7.8818 7.0579 1.2969 -0.2334 -0.9706 0.0589 -0.7228 -1.6874 10.4466 0.4051 -0.0995 0.9088 -4.4561 -6.5510 -0.8074 0.9198 -0.2205 -0.3247 1.6509 3.0238 -9.8056 -0.5852 0.1426 -0.7982 4.4595 6.5646 0.6624 -0.9240 0.2216 0.3117