#------------------------------------------------------------------------------ #$Date: 2016-01-21 09:38:23 +0200 (Thu, 21 Jan 2016) $ #$Revision: 174676 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/39/7223948.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_7223948 loop_ _publ_author_name 'Tyagi, Adish' 'Kedarnath, G.' 'Wadawale, Amey' 'Shah, Alpa Y.' 'Jain, Vimal K.' 'Vishwanadh, B.' _publ_section_title ; Diorganotin(iv) 4,6-dimethyl-2-pyrimidyl selenolates: synthesis, structures and their utility as molecular precursors for the preparation of SnSe2nano-sheets and thin films ; _journal_issue 10 _journal_name_full 'RSC Adv.' _journal_page_first 8367 _journal_paper_doi 10.1039/C5RA20578F _journal_volume 6 _journal_year 2016 _chemical_formula_sum 'C20 H32 N4 Se2 Sn' _chemical_formula_weight 605.10 _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_method SHELXL-2014/6 _audit_update_record ; 2015-12-30 deposited with the CCDC. 2016-01-13 downloaded from the CCDC. ; _cell_angle_alpha 84.62(9) _cell_angle_beta 84.17(5) _cell_angle_gamma 70.44(7) _cell_formula_units_Z 8 _cell_length_a 11.659(6) _cell_length_b 16.166(17) _cell_length_c 29.13(3) _cell_measurement_reflns_used 16 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 9.1 _cell_measurement_theta_min 2.7 _cell_volume 5136(8) _computing_cell_refinement WinAFC _computing_data_collection WInAFC _computing_data_reduction 'Crystal Structure' _computing_molecular_graphics Ortep3 _computing_publication_material 'WinGX 2014.1' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution SIR-92 _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.1381 _diffrn_reflns_av_unetI/netI 0.6142 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 28407 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 27.559 _diffrn_reflns_theta_min 2.496 _exptl_absorpt_coefficient_mu 3.840 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.565 _exptl_crystal_description block _exptl_crystal_F_000 2384 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.139 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.172 _refine_ls_extinction_coef 0.00016(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 925 _refine_ls_number_reflns 23556 _refine_ls_number_restraints 624 _refine_ls_restrained_S_all 0.899 _refine_ls_R_factor_all 0.4531 _refine_ls_R_factor_gt 0.1132 _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^)+(0.1322P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2392 _refine_ls_wR_factor_ref 0.3834 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4580 _reflns_number_total 23556 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5ra20578f2.cif _cod_data_source_block shelx _cod_original_cell_volume 5137(8) _cod_database_code 7223948 _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_min 0.514 _shelx_estimated_absorpt_t_max 0.831 _shelxl_version_number 2014/6 _shelx_res_file ; TITL VK-35 CELL 0.71069 11.6594 16.1660 29.1321 84.618 84.169 70.440 ZERR 8.00 0.0057 0.0173 0.0250 0.092 0.052 0.069 LATT 1 SFAC C H N SE SN UNIT 160 256 32 16 8 MERG 2 DFIX 1.540 C15 C16 C17 C18 C18 C19 C19 C20 DFIX 1.540 C33 C34 C34 C35 C35 C36 C37 C38 c38 c39 c39 c40 DFIX 1.540 C55 C56 C57 C58 DFIX 1.540 C73 C74 C74 C75 C79 C80 DFIX 2.450 C53 C55 DFIX 2.450 C77 C79 DFIX 2.450 C54a C56 C54b C56 DFIX 2.450 0.020 C33 C35 DFIX 2.450 0.020 C34 C36 SIMU C1 N1 C2 C3 C4 N2 SIMU C7 N4 C8 C9 C10 N4 SIMU C21 N5 C22 C23 C4 N6 SIMU C27 N8 C28 C29 C30 N8 SIMU C41 N12 C42 C43 C44 N11 SIMU C47 N11 C48 C49 C50 N12 SIMU C61 N16 C62 C63 C64 N15 SIMU C67 N15 C68 C69 C70 N16 DELU C4 C6 DELU C8 C11 SIMU C13 C14a C15 C16 SIMU C17 C18 C19 C20 SIMU C33 C34 C35 C36 SIMU C37 C38 C39 C40 SIMU C53 C54a C54b C55 C56 SIMU C57 C58 C59a C59b C60 SIMU C73 C74 C75 C76a C76b SIMU C77 C78a C78b C79 C80 DELU C13 C14a C15 C16 DELU C17 C18 C19 C20 DELU C33 C34 C35 C36 DELU C37 C38 C39 C40 DELU C53 C54a C54b C55 C56 DELU C57 C58 C59a C59b C60 DELU C73 C74 C75 C76a C76b DELU C77 C78a C78b C79 C80 SIMU C77 SN4 BOND N1 Sn1 BOND N3 SN1 BIND N1 Sn1 BIND N3 SN1 BOND N5 Sn2 BOND N7 SN2 BIND N5 Sn2 BIND N7 SN2 BOND N9 Sn3 BOND N11 SN3 BIND N9 Sn3 BIND N11 SN3 BOND N13 Sn4 BOND N15 SN4 BIND N13 Sn4 BIND N15 SN4 DFIX 1.54 C13 C14a C14a C15 DFIX 1.54 C53 C54a C54a C55 DFIX 1.54 C58 C59a C59a C60 DFIX 1.54 C75 C76a C77 C78a C78a C79 DFIX 1.54 C13 C14b C14b C15 DFIX 1.54 C53 C54b C54b C55 DFIX 1.54 C58 C59b C59b C60 DFIX 1.54 C75 C76b C75 C76a C77 C78b C78b C79 DFIX 2.45 C74 C76b C74 C76a ISOR C14b C34 C48 C50 C54a C54b C55 C58 C59b C75 C76a C76b C78a C78b C79 SADI C13 C14A C13 C14B C14A C15 C14B C15 SADI C53 C54A C53 C54B C54A C55 C54B C55 SADI C58 C59A C58 C59B C59A C60 C59B C60 SADI C75 C76A C75 C76B SADI C77 C78a C77 C78b C78a C79 C78b C79 DELU C14A C14B SIMU C14A C14B FMAP 2 PLAN 20 SIZE 0.050 0.150 0.200 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 20 TEMP 25.00 WGHT 0.132200 EXTI 0.000158 FVAR 0.02307 0.61228 0.04000 PART 1 C14A 1 0.139141 0.118507 0.200386 21.00000 0.19410 0.23423 = 0.18218 0.04422 0.01491 -0.08703 AFIX 23 H14A 2 0.076019 0.091339 0.206359 21.00000 -1.20000 H14B 2 0.112149 0.174169 0.214852 21.00000 -1.20000 AFIX 0 C54A 1 0.908409 0.349274 0.667153 21.00000 0.19790 0.24638 = 0.22683 0.02952 -0.07640 -0.08449 AFIX 23 H54A 2 0.987446 0.303654 0.664293 21.00000 -1.20000 H54B 2 0.918622 0.405717 0.657764 21.00000 -1.20000 AFIX 0 C59A 1 0.822357 0.070661 0.488509 21.00000 0.28635 0.19319 = 0.13677 -0.04978 -0.02282 -0.08415 AFIX 23 H59A 2 0.792436 0.124227 0.468979 21.00000 -1.20000 H59B 2 0.906590 0.039356 0.478605 21.00000 -1.20000 AFIX 0 C76A 1 0.489552 0.517851 0.849246 21.00000 0.17329 0.08088 = 0.21114 -0.02984 -0.05664 -0.05730 AFIX 33 H76A 2 0.424797 0.569034 0.859237 21.00000 -1.50000 H76B 2 0.547048 0.535612 0.828150 21.00000 -1.50000 H76C 2 0.456357 0.481743 0.834033 21.00000 -1.50000 AFIX 0 C78A 1 1.010563 0.069558 0.821592 21.00000 0.18806 0.19372 = 0.12508 -0.07135 0.02323 -0.00073 AFIX 23 H78A 2 0.963830 0.029477 0.826787 21.00000 -1.20000 H78B 2 1.069045 0.055905 0.844923 21.00000 -1.20000 AFIX 0 PART 2 C14B 1 0.271778 0.125721 0.179118 -21.00000 0.15101 0.16988 = 0.16266 0.02623 0.03951 -0.10931 AFIX 23 H14C 2 0.351089 0.106277 0.162110 -21.00000 -1.20000 H14D 2 0.259784 0.182173 0.191192 -21.00000 -1.20000 AFIX 0 C54B 1 0.769847 0.319816 0.687793 -21.00000 0.19828 0.22908 = 0.18873 0.04815 -0.02686 -0.05497 AFIX 23 H54C 2 0.776576 0.258848 0.695809 -21.00000 -1.20000 H54D 2 0.685068 0.356156 0.692710 -21.00000 -1.20000 AFIX 0 C59B 1 0.772985 0.097386 0.489735 -21.00000 0.25976 0.20530 = 0.13936 -0.07173 -0.03085 -0.07759 AFIX 23 H59C 2 0.703512 0.149431 0.483593 -21.00000 -1.20000 H59D 2 0.841263 0.097700 0.467798 -21.00000 -1.20000 AFIX 0 C76B 1 0.615560 0.528085 0.905225 -21.00000 0.23605 0.15832 = 0.29233 -0.09203 -0.04856 -0.05770 AFIX 33 H76D 2 0.554611 0.579360 0.917119 -21.00000 -1.50000 H76E 2 0.670258 0.498941 0.928656 -21.00000 -1.50000 H76F 2 0.660585 0.545246 0.878773 -21.00000 -1.50000 AFIX 0 C78B 1 1.062984 0.112982 0.816455 -21.00000 0.13942 0.18586 = 0.12057 -0.04365 0.01895 -0.01309 AFIX 23 H78C 2 1.088942 0.072275 0.842989 -21.00000 -1.20000 H78D 2 1.111389 0.151989 0.812268 -21.00000 -1.20000 PART 0 AFIX 66 C1 1 0.338300 0.301394 0.095988 11.00000 0.10185 0.12412 = 0.06348 -0.02867 -0.02077 -0.04460 N1 3 0.320210 0.233262 0.075174 11.00000 0.06416 0.12373 = 0.04831 -0.01772 0.00760 -0.04378 C2 1 0.406647 0.187692 0.041978 11.00000 0.12240 0.09684 = 0.03526 0.02372 -0.00507 -0.02879 C3 1 0.511174 0.210253 0.029596 11.00000 0.10746 0.08790 = 0.05452 -0.00472 0.01669 -0.02630 AFIX 43 H3 2 0.569006 0.179763 0.007385 11.00000 -1.20000 AFIX 65 C4 1 0.529266 0.278385 0.050409 11.00000 0.08115 0.10880 = 0.07744 0.01649 0.02290 -0.02193 N2 3 0.442830 0.323956 0.083605 11.00000 0.08154 0.11098 = 0.07395 -0.01519 -0.01962 -0.02485 AFIX 0 C5 1 0.375412 0.117529 0.019179 11.00000 0.25664 0.08806 = 0.08032 -0.02891 -0.00233 -0.03396 AFIX 33 H5A 2 0.299378 0.112966 0.033136 11.00000 -1.50000 H5B 2 0.368382 0.133536 -0.013246 11.00000 -1.50000 H5C 2 0.438821 0.061935 0.023297 11.00000 -1.50000 AFIX 0 C6 1 0.627798 0.315158 0.039063 11.00000 0.17343 0.15099 = 0.11206 -0.01947 0.05650 -0.10391 AFIX 33 H6A 2 0.617766 0.361599 0.058938 11.00000 -1.50000 H6B 2 0.704763 0.269933 0.043337 11.00000 -1.50000 H6C 2 0.625743 0.338153 0.007442 11.00000 -1.50000 AFIX 66 C7 1 -0.161873 0.271412 0.167915 11.00000 0.06798 0.15155 = 0.10914 -0.04008 -0.02450 0.00341 N4 3 -0.274118 0.274117 0.190253 11.00000 0.09204 0.10698 = 0.09171 -0.01611 -0.01327 -0.02846 C8 1 -0.336650 0.222125 0.176478 11.00000 0.05712 0.10741 = 0.09507 0.00913 0.00213 -0.02303 C9 1 -0.286936 0.167428 0.140365 11.00000 0.07812 0.10771 = 0.10656 -0.01182 -0.00580 -0.00741 AFIX 43 H9 2 -0.328774 0.132642 0.131149 11.00000 -1.20000 AFIX 65 C10 1 -0.174691 0.164721 0.118027 11.00000 0.10959 0.06574 = 0.11839 -0.01092 -0.02184 0.00134 N3 3 -0.112158 0.216713 0.131801 11.00000 0.13741 0.08459 = 0.07700 -0.01136 -0.03087 -0.01724 AFIX 0 C11 1 -0.455274 0.232175 0.203044 11.00000 0.06372 0.19749 = 0.10276 0.04857 -0.00188 -0.05794 AFIX 33 H11A 2 -0.468483 0.273845 0.226066 11.00000 -1.50000 H11B 2 -0.519706 0.252810 0.182456 11.00000 -1.50000 H11C 2 -0.454517 0.176385 0.217830 11.00000 -1.50000 AFIX 0 C12 1 -0.115574 0.105810 0.080084 11.00000 0.12119 0.10032 = 0.13537 -0.04569 -0.02129 -0.02898 AFIX 33 H12A 2 -0.039135 0.113792 0.069346 11.00000 -1.50000 H12B 2 -0.101496 0.045746 0.091326 11.00000 -1.50000 H12C 2 -0.167890 0.119824 0.055062 11.00000 -1.50000 AFIX 0 C13 1 0.169036 0.131755 0.148063 11.00000 0.13457 0.21068 = 0.16576 0.01301 -0.00834 -0.14091 AFIX 23 H13A 2 0.138735 0.094336 0.131957 11.00000 -1.20000 H13B 2 0.256992 0.113109 0.141842 11.00000 -1.20000 AFIX 0 C15 1 0.260808 0.057285 0.218437 11.00000 0.25063 0.25589 = 0.20745 0.04395 -0.03860 -0.06941 AFIX 23 H15A 2 0.230785 0.015036 0.237273 11.00000 -1.20000 H15B 2 0.297029 0.027541 0.190471 11.00000 -1.20000 AFIX 0 C16 1 0.375681 0.043829 0.241949 11.00000 0.28869 0.19702 = 0.27008 0.12991 -0.09242 -0.09827 AFIX 33 H16A 2 0.380867 0.001632 0.267805 11.00000 -1.50000 H16B 2 0.445388 0.022582 0.220426 11.00000 -1.50000 H16C 2 0.373923 0.098708 0.252586 11.00000 -1.50000 AFIX 0 C17 1 0.037925 0.305194 0.051987 11.00000 0.04349 0.13831 = 0.07683 -0.02262 -0.03092 0.00087 AFIX 23 H17A 2 0.106196 0.314518 0.032873 11.00000 -1.20000 H17B 2 0.018418 0.258579 0.039278 11.00000 -1.20000 AFIX 0 C18 1 -0.070657 0.388472 0.048877 11.00000 0.07060 0.13039 = 0.09473 -0.01060 -0.03230 -0.00647 AFIX 23 H18A 2 -0.051050 0.436609 0.059860 11.00000 -1.20000 H18B 2 -0.139376 0.380693 0.068334 11.00000 -1.20000 AFIX 0 C19 1 -0.104681 0.410447 -0.000892 11.00000 0.11494 0.12372 = 0.09673 0.00173 -0.05072 0.00114 AFIX 23 H19A 2 -0.125099 0.362533 -0.011729 11.00000 -1.20000 H19B 2 -0.035542 0.417441 -0.020379 11.00000 -1.20000 AFIX 0 C20 1 -0.212863 0.494709 -0.004435 11.00000 0.11885 0.13733 = 0.13787 0.01672 -0.04714 0.00749 AFIX 33 H20A 2 -0.233311 0.507760 -0.036004 11.00000 -1.50000 H20B 2 -0.281522 0.487411 0.014547 11.00000 -1.50000 H20C 2 -0.192134 0.542215 0.005913 11.00000 -1.50000 AFIX 66 C21 1 0.805777 0.276272 0.405171 11.00000 0.07649 0.08336 = 0.12510 0.00473 -0.02290 -0.03140 N5 3 0.790304 0.241673 0.365223 11.00000 0.08990 0.09560 = 0.09441 -0.01095 -0.02692 -0.03967 C22 1 0.890396 0.184821 0.341222 11.00000 0.10169 0.10738 = 0.10551 0.00476 0.00562 -0.03260 C23 1 1.005963 0.162568 0.357168 11.00000 0.12159 0.13151 = 0.09072 -0.01134 -0.00542 -0.03291 AFIX 43 H23 2 1.072932 0.124530 0.341110 11.00000 -1.20000 AFIX 65 C24 1 1.021438 0.197166 0.397116 11.00000 0.04771 0.08934 = 0.11819 0.02096 0.03459 -0.00090 N6 3 0.921346 0.254018 0.421118 11.00000 0.10781 0.10787 = 0.09852 0.01216 -0.03326 -0.01844 AFIX 0 C25 1 0.868603 0.159889 0.295462 11.00000 0.15239 0.29379 = 0.11710 -0.12273 0.03107 -0.06170 AFIX 33 H25A 2 0.782743 0.181650 0.291287 11.00000 -1.50000 H25B 2 0.911122 0.185038 0.271168 11.00000 -1.50000 H25C 2 0.897973 0.096995 0.294593 11.00000 -1.50000 AFIX 0 C26 1 1.138620 0.185209 0.416307 11.00000 0.06263 0.12754 = 0.21931 -0.00258 -0.06201 0.01490 AFIX 33 H26A 2 1.123740 0.215952 0.444094 11.00000 -1.50000 H26B 2 1.179651 0.123701 0.423216 11.00000 -1.50000 H26C 2 1.188754 0.208189 0.394102 11.00000 -1.50000 AFIX 66 C27 1 0.237826 0.411457 0.391611 11.00000 0.06018 0.09144 = 0.11133 0.03179 0.00853 0.00443 N8 3 0.113993 0.449627 0.403816 11.00000 0.08970 0.07676 = 0.10035 -0.00255 -0.02425 -0.01864 C28 1 0.028166 0.440200 0.376735 11.00000 0.11302 0.07325 = 0.13161 0.02481 -0.05884 -0.02502 C29 1 0.066171 0.392602 0.337449 11.00000 0.10923 0.10443 = 0.10751 -0.00095 -0.02636 -0.02608 AFIX 43 H29 2 0.008747 0.386295 0.319331 11.00000 -1.20000 AFIX 65 C30 1 0.190004 0.354431 0.325244 11.00000 0.10344 0.08736 = 0.10246 0.01706 -0.00674 -0.01607 N7 3 0.275832 0.363858 0.352325 11.00000 0.07516 0.12767 = 0.08452 -0.01234 0.01413 -0.01542 AFIX 0 C31 1 -0.099382 0.486117 0.391914 11.00000 0.03819 0.17590 = 0.13992 0.00689 -0.02033 -0.03401 AFIX 33 H31A 2 -0.151957 0.476030 0.371337 11.00000 -1.50000 H31B 2 -0.117069 0.464349 0.422681 11.00000 -1.50000 H31C 2 -0.112689 0.548056 0.391668 11.00000 -1.50000 AFIX 0 C32 1 0.236147 0.299435 0.285007 11.00000 0.17396 0.18364 = 0.10003 -0.06491 -0.01315 -0.01739 AFIX 33 H32A 2 0.168488 0.298090 0.269212 11.00000 -1.50000 H32B 2 0.287527 0.323922 0.264247 11.00000 -1.50000 H32C 2 0.282282 0.240705 0.295524 11.00000 -1.50000 AFIX 0 C33 1 0.524775 0.188323 0.392667 11.00000 0.19174 0.19438 = 0.13951 0.05129 -0.02744 -0.04833 AFIX 23 H33A 2 0.592155 0.151973 0.410244 11.00000 -1.20000 H33B 2 0.449114 0.189790 0.410382 11.00000 -1.20000 AFIX 0 C34 1 0.531305 0.149917 0.346776 11.00000 0.22253 0.18062 = 0.17637 0.01558 -0.00732 -0.02536 AFIX 23 H34A 2 0.593324 0.163771 0.325751 11.00000 -1.20000 H34B 2 0.453525 0.175392 0.333191 11.00000 -1.20000 AFIX 0 C35 1 0.562267 0.050309 0.353910 11.00000 0.20454 0.17976 = 0.21566 0.02970 -0.00655 -0.01145 AFIX 23 H35A 2 0.574464 0.024940 0.324184 11.00000 -1.20000 H35B 2 0.637313 0.025276 0.369367 11.00000 -1.20000 AFIX 0 C36 1 0.461732 0.029207 0.382173 11.00000 0.21708 0.21434 = 0.26717 0.06067 -0.00279 -0.02983 AFIX 33 H36A 2 0.481564 -0.033479 0.386577 11.00000 -1.50000 H36B 2 0.450535 0.053869 0.411681 11.00000 -1.50000 H36C 2 0.387839 0.053533 0.366608 11.00000 -1.50000 AFIX 0 C37 1 0.551548 0.392377 0.313822 11.00000 0.11759 0.10913 = 0.09699 -0.00326 -0.04246 -0.02049 AFIX 23 H37A 2 0.585065 0.349086 0.290875 11.00000 -1.20000 H37B 2 0.471137 0.429236 0.305314 11.00000 -1.20000 AFIX 0 C38 1 0.632568 0.448882 0.313087 11.00000 0.17674 0.13462 = 0.12229 0.01359 -0.01873 -0.06580 AFIX 23 H38A 2 0.713880 0.411314 0.320168 11.00000 -1.20000 H38B 2 0.601349 0.489811 0.337275 11.00000 -1.20000 AFIX 0 C39 1 0.641722 0.500663 0.267392 11.00000 0.20706 0.18867 = 0.10968 0.02189 -0.02594 -0.07669 AFIX 23 H39A 2 0.662322 0.460473 0.242801 11.00000 -1.20000 H39B 2 0.561991 0.543333 0.262355 11.00000 -1.20000 AFIX 0 C40 1 0.733976 0.548844 0.263446 11.00000 0.15653 0.20642 = 0.18251 0.05992 0.01681 -0.05827 AFIX 33 H40A 2 0.733047 0.579434 0.233532 11.00000 -1.50000 H40B 2 0.713379 0.590342 0.286954 11.00000 -1.50000 H40C 2 0.813952 0.507281 0.267352 11.00000 -1.50000 AFIX 66 C41 1 0.603982 0.191954 0.661157 11.00000 0.10414 0.12639 = 0.06290 -0.00978 0.04243 -0.07160 N12 3 0.495633 0.183364 0.682091 11.00000 0.13322 0.14137 = 0.07946 -0.01399 -0.00220 -0.08402 C42 1 0.384404 0.238101 0.667019 11.00000 0.11518 0.15348 = 0.06318 -0.03708 -0.00212 -0.05839 C43 1 0.381521 0.301429 0.631014 11.00000 0.11546 0.16800 = 0.07859 -0.01958 0.01370 -0.03981 AFIX 43 H43 2 0.307101 0.338051 0.620930 11.00000 -1.20000 AFIX 65 C44 1 0.489869 0.310019 0.610080 11.00000 0.12245 0.16081 = 0.04275 -0.02473 -0.00097 -0.05092 N11 3 0.601099 0.255283 0.625151 11.00000 0.12177 0.12913 = 0.06543 -0.01896 -0.01314 -0.05938 AFIX 0 C45 1 0.283461 0.221702 0.693999 11.00000 0.10977 0.22256 = 0.20135 -0.02383 0.01234 -0.08252 AFIX 33 H45A 2 0.208371 0.260542 0.682662 11.00000 -1.50000 H45B 2 0.288096 0.161813 0.691646 11.00000 -1.50000 H45C 2 0.286320 0.231767 0.725756 11.00000 -1.50000 AFIX 0 C46 1 0.496898 0.379645 0.571765 11.00000 0.16471 0.12513 = 0.12915 0.03714 -0.00356 -0.00453 AFIX 33 H46A 2 0.580878 0.372897 0.562713 11.00000 -1.50000 H46B 2 0.457721 0.372731 0.545631 11.00000 -1.50000 H46C 2 0.456519 0.437124 0.582839 11.00000 -1.50000 AFIX 66 C47 1 1.133606 0.171538 0.588298 11.00000 0.15335 0.08282 = 0.04188 0.00066 0.00509 -0.02078 N9 3 1.047638 0.244152 0.568077 11.00000 0.12017 0.11826 = 0.06192 -0.00412 -0.01903 -0.04681 C48 1 1.085030 0.298540 0.534430 11.00000 0.17919 0.08505 = 0.03809 -0.01678 0.01261 -0.06158 C49 1 1.208391 0.280315 0.521005 11.00000 0.21029 0.12591 = 0.05330 -0.01929 0.04303 -0.07014 AFIX 43 H49 2 1.233408 0.316705 0.498493 11.00000 -1.20000 AFIX 65 C50 1 1.294360 0.207702 0.541225 11.00000 0.19966 0.08347 = 0.04768 -0.01453 0.03854 -0.07346 N10 3 1.256970 0.153313 0.574872 11.00000 0.09138 0.16213 = 0.08868 -0.04329 -0.00951 -0.04147 AFIX 0 C51 1 0.983195 0.375008 0.516624 11.00000 0.25763 0.07428 = 0.11710 0.02367 -0.01390 -0.05639 AFIX 33 H51A 2 1.015660 0.409456 0.493635 11.00000 -1.50000 H51B 2 0.927176 0.354044 0.503121 11.00000 -1.50000 H51C 2 0.941267 0.410692 0.541665 11.00000 -1.50000 AFIX 0 C52 1 1.426478 0.173397 0.527398 11.00000 0.11533 0.25747 = 0.16471 -0.04301 0.07592 -0.08208 AFIX 33 H52A 2 1.464485 0.122634 0.547180 11.00000 -1.50000 H52B 2 1.438218 0.157327 0.495938 11.00000 -1.50000 H52C 2 1.462504 0.217961 0.530101 11.00000 -1.50000 AFIX 0 C53 1 0.818126 0.331819 0.637460 11.00000 0.11122 0.17688 = 0.19570 0.03390 -0.01919 -0.06636 AFIX 23 H53A 2 0.809197 0.372630 0.610395 11.00000 -1.20000 H53B 2 0.739445 0.347249 0.655022 11.00000 -1.20000 AFIX 0 C55 1 0.851545 0.348842 0.716773 11.00000 0.27476 0.27005 = 0.21675 0.00694 -0.06758 -0.05206 AFIX 23 H55A 2 0.798780 0.312947 0.720154 11.00000 -1.20000 H55B 2 0.915010 0.324495 0.738097 11.00000 -1.20000 AFIX 0 C56 1 0.778496 0.442713 0.727229 11.00000 0.33572 0.25365 = 0.24562 0.00899 -0.09542 -0.03870 AFIX 33 H56A 2 0.741917 0.443913 0.758314 11.00000 -1.50000 H56B 2 0.831509 0.477643 0.723941 11.00000 -1.50000 H56C 2 0.715716 0.466139 0.706066 11.00000 -1.50000 AFIX 0 C57 1 0.818652 0.177205 0.546524 11.00000 0.06324 0.19543 = 0.08260 -0.01469 -0.00823 -0.07292 AFIX 23 H57A 2 0.743774 0.222083 0.537714 11.00000 -1.20000 H57B 2 0.883814 0.184342 0.524719 11.00000 -1.20000 AFIX 0 C58 1 0.806829 0.089092 0.540085 11.00000 0.24108 0.19730 = 0.12708 -0.03055 -0.01194 -0.09751 AFIX 23 H58A 2 0.727256 0.088075 0.553012 11.00000 -1.20000 H58B 2 0.868355 0.043293 0.556564 11.00000 -1.20000 AFIX 0 C60 1 0.741467 0.012858 0.489445 11.00000 0.28146 0.21394 = 0.18005 -0.06352 -0.03937 -0.08591 AFIX 33 H60A 2 0.741607 -0.004625 0.458837 11.00000 -1.50000 H60B 2 0.772473 -0.038486 0.509801 11.00000 -1.50000 H60C 2 0.659595 0.045436 0.500282 11.00000 -1.50000 AFIX 66 C61 1 0.644471 0.110664 0.895770 11.00000 0.09295 0.08035 = 0.09953 -0.02227 -0.02938 -0.01952 N16 3 0.556248 0.069821 0.905076 11.00000 0.07944 0.10129 = 0.09435 -0.01585 -0.00190 -0.05352 C62 1 0.460821 0.089199 0.876554 11.00000 0.08322 0.10239 = 0.07485 -0.04202 -0.01137 -0.00843 C63 1 0.453617 0.149421 0.838726 11.00000 0.11716 0.12462 = 0.09467 -0.01479 -0.02635 -0.01482 AFIX 43 H63 2 0.389770 0.162386 0.819643 11.00000 -1.20000 AFIX 65 C64 1 0.541840 0.190265 0.829419 11.00000 0.11501 0.10254 = 0.06894 -0.01978 -0.02454 -0.02858 N15 3 0.637267 0.170888 0.857941 11.00000 0.09189 0.07360 = 0.07585 0.00135 -0.01513 -0.01133 AFIX 0 C65 1 0.549790 0.246235 0.789796 11.00000 0.13178 0.17039 = 0.08380 0.00779 0.00351 -0.02812 AFIX 33 H65A 2 0.617979 0.266410 0.791055 11.00000 -1.50000 H65B 2 0.560746 0.214496 0.762549 11.00000 -1.50000 H65C 2 0.476043 0.295812 0.788876 11.00000 -1.50000 AFIX 0 C66 1 0.375027 0.038972 0.887862 11.00000 0.09266 0.15876 = 0.23452 0.00096 -0.04876 -0.07665 AFIX 33 H66A 2 0.397409 0.001504 0.915344 11.00000 -1.50000 H66B 2 0.293576 0.079130 0.892899 11.00000 -1.50000 H66C 2 0.378506 0.003738 0.862670 11.00000 -1.50000 AFIX 66 C67 1 1.086910 0.239352 0.916810 11.00000 0.08975 0.08639 = 0.04199 0.01054 -0.02068 -0.00399 N13 3 1.025185 0.296680 0.881975 11.00000 0.08469 0.06387 = 0.11543 -0.01418 -0.00500 -0.02226 C68 1 1.068618 0.362745 0.861579 11.00000 0.10785 0.08841 = 0.11152 -0.00554 -0.02899 -0.02369 C69 1 1.173776 0.371482 0.876018 11.00000 0.10898 0.09654 = 0.12263 -0.01011 -0.00867 -0.03943 AFIX 43 H69 2 1.202835 0.415685 0.862372 11.00000 -1.20000 AFIX 65 C70 1 1.235502 0.314155 0.910854 11.00000 0.08175 0.10590 = 0.08237 -0.02941 -0.00003 -0.03922 N14 3 1.192071 0.248090 0.931250 11.00000 0.11773 0.08452 = 0.12848 -0.00415 -0.04927 -0.03719 AFIX 0 C71 1 1.352217 0.314117 0.927177 11.00000 0.08970 0.16243 = 0.15030 -0.03716 0.01626 -0.07261 AFIX 33 H71A 2 1.377110 0.268761 0.951393 11.00000 -1.50000 H71B 2 1.413929 0.303371 0.901930 11.00000 -1.50000 H71C 2 1.341002 0.370193 0.938752 11.00000 -1.50000 AFIX 0 C72 1 0.997503 0.415530 0.825582 11.00000 0.10066 0.18325 = 0.17595 0.03914 -0.03888 -0.02751 AFIX 33 H72A 2 1.032460 0.459595 0.813092 11.00000 -1.50000 H72B 2 0.996981 0.378901 0.801556 11.00000 -1.50000 H72C 2 0.915392 0.443483 0.837964 11.00000 -1.50000 AFIX 0 C73 1 0.735914 0.324073 0.907014 11.00000 0.18043 0.07499 = 0.12054 -0.05506 -0.00240 -0.02310 AFIX 23 H73A 2 0.682758 0.314758 0.933381 11.00000 -1.20000 H73B 2 0.785131 0.355358 0.917647 11.00000 -1.20000 AFIX 0 C74 1 0.655530 0.385372 0.872484 11.00000 0.18431 0.11915 = 0.17106 -0.04208 -0.03348 -0.02181 AFIX 23 H74A 2 0.617986 0.351709 0.856876 11.00000 -1.20000 H74B 2 0.707074 0.406385 0.849389 11.00000 -1.20000 AFIX 0 C75 1 0.553911 0.465613 0.891116 11.00000 0.18375 0.09941 = 0.21510 -0.04795 -0.05484 -0.01652 AFIX 23 H75A 2 0.496948 0.447087 0.912754 11.00000 -1.20000 H75B 2 0.588113 0.501237 0.906841 11.00000 -1.20000 AFIX 0 C77 1 0.926119 0.165572 0.822778 11.00000 0.11621 0.17072 = 0.08348 -0.06861 0.00574 -0.04073 AFIX 23 H77A 2 0.859583 0.174201 0.803422 11.00000 -1.20000 H77B 2 0.971580 0.203848 0.809857 11.00000 -1.20000 AFIX 0 C79 1 1.075479 0.063214 0.772739 11.00000 0.20207 0.20726 = 0.12857 -0.06748 0.03094 0.02426 AFIX 23 H79A 2 1.039117 0.031062 0.755528 11.00000 -1.20000 H79B 2 1.053225 0.122645 0.758585 11.00000 -1.20000 AFIX 0 C80 1 1.212252 0.023031 0.763727 11.00000 0.19552 0.23753 = 0.15979 -0.06912 0.03853 0.00484 AFIX 33 H80A 2 1.233606 0.025687 0.731045 11.00000 -1.50000 H80B 2 1.252096 0.055117 0.778748 11.00000 -1.50000 H80C 2 1.237872 -0.037218 0.775666 11.00000 -1.50000 AFIX 0 SE1 4 -0.079197 0.337694 0.182848 11.00000 0.10334 0.14315 = 0.10020 -0.05719 0.02031 -0.05514 SE2 4 0.225293 0.354905 0.140429 11.00000 0.10133 0.14039 = 0.09807 -0.05427 0.01668 -0.05730 SE3 4 0.675608 0.348317 0.436847 11.00000 0.08430 0.12453 = 0.08176 -0.01815 -0.01466 -0.02261 SE4 4 0.346792 0.422256 0.428193 11.00000 0.08080 0.12234 = 0.09830 -0.01425 -0.01260 -0.03370 SE5 4 0.753384 0.117160 0.674815 11.00000 0.10393 0.14083 = 0.10358 0.02939 -0.01303 -0.04402 SE6 4 1.072600 0.105571 0.632357 11.00000 0.08757 0.13827 = 0.09493 0.02939 -0.01300 -0.02847 SN1 5 0.094605 0.261504 0.121645 11.00000 0.08048 0.09983 = 0.06551 -0.01898 -0.00374 -0.03007 SN2 5 0.534045 0.325679 0.380100 11.00000 0.08819 0.09841 = 0.07518 0.00255 -0.01534 -0.03147 SN3 5 0.854119 0.204948 0.613983 11.00000 0.09259 0.10080 = 0.06424 -0.00317 -0.01267 -0.03192 SE7 4 0.767102 0.086718 0.933679 11.00000 0.07781 0.10829 = 0.08978 -0.00299 -0.01442 -0.02940 SE8 4 1.029707 0.157366 0.943905 11.00000 0.09506 0.09969 = 0.09285 0.00010 -0.02272 -0.03813 SN4 5 0.852630 0.202298 0.890299 11.00000 0.07865 0.08956 = 0.06868 -0.01693 -0.00605 -0.02056 HKLF 4 REM VK-35 REM R1 = 0.1132 for 4580 Fo > 4sig(Fo) and 0.4531 for all 23556 data REM 925 parameters refined using 624 restraints END WGHT 0.1331 0.0000 REM Highest difference peak 1.139, deepest hole -1.402, 1-sigma level 0.172 Q1 1 0.2582 0.2641 0.1281 11.00000 0.05 1.14 Q2 1 0.5000 0.4365 0.4178 11.00000 0.05 1.09 Q3 1 0.0642 0.3499 0.1393 11.00000 0.05 0.98 Q4 1 0.8808 0.1292 0.6296 11.00000 0.05 0.90 Q5 1 1.0187 0.2179 0.6211 11.00000 0.05 0.89 Q6 1 -0.1930 0.2631 0.1650 11.00000 0.05 0.89 Q7 1 0.5599 0.2394 0.3741 11.00000 0.05 0.88 Q8 1 0.8638 0.1519 0.9163 11.00000 0.05 0.83 Q9 1 0.8808 0.1340 0.5972 11.00000 0.05 0.81 Q10 1 0.8781 0.1227 0.8855 11.00000 0.05 0.81 Q11 1 0.8430 0.2793 0.9069 11.00000 0.05 0.80 Q12 1 0.7595 0.1388 0.9121 11.00000 0.05 0.80 Q13 1 0.8763 0.0453 0.9320 11.00000 0.05 0.78 Q14 1 0.7425 0.2389 0.6139 11.00000 0.05 0.78 Q15 1 0.7429 0.1613 0.9421 11.00000 0.05 0.77 Q16 1 0.3865 0.3141 0.3945 11.00000 0.05 0.77 Q17 1 0.9058 0.4045 0.7146 11.00000 0.05 0.76 Q18 1 0.4455 0.3711 0.3935 11.00000 0.05 0.74 Q19 1 1.0763 0.0685 0.9270 11.00000 0.05 0.74 Q20 1 0.0193 0.2816 0.1413 11.00000 0.05 0.74 ; _shelx_res_checksum 82756 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 C14A C 0.139(4) 0.119(4) 0.2004(12) 0.205(16) Uani 0.612(19) 1 d D U P A 1 H14A H 0.0760 0.0913 0.2064 0.246 Uiso 0.612(19) 1 calc R U P A 1 H14B H 0.1121 0.1742 0.2149 0.246 Uiso 0.612(19) 1 calc R U P A 1 C54A C 0.908(3) 0.349(4) 0.6672(13) 0.219(14) Uani 0.612(19) 1 d D U P A 1 H54A H 0.9874 0.3037 0.6643 0.263 Uiso 0.612(19) 1 calc R U P A 1 H54B H 0.9186 0.4057 0.6578 0.263 Uiso 0.612(19) 1 calc R U P A 1 C59A C 0.822(6) 0.071(4) 0.4885(11) 0.201(14) Uani 0.612(19) 1 d D U P A 1 H59A H 0.7924 0.1242 0.4690 0.241 Uiso 0.612(19) 1 calc R U P A 1 H59B H 0.9066 0.0394 0.4786 0.241 Uiso 0.612(19) 1 calc R U P A 1 C76A C 0.490(4) 0.518(2) 0.8492(14) 0.147(18) Uani 0.612(19) 1 d D U P A 1 H76A H 0.4248 0.5690 0.8592 0.220 Uiso 0.612(19) 1 calc R U P A 1 H76B H 0.5470 0.5356 0.8282 0.220 Uiso 0.612(19) 1 calc R U P A 1 H76C H 0.4564 0.4817 0.8340 0.220 Uiso 0.612(19) 1 calc R U P A 1 C78A C 1.011(5) 0.070(2) 0.8216(12) 0.183(15) Uani 0.612(19) 1 d D U P A 1 H78A H 0.9638 0.0295 0.8268 0.220 Uiso 0.612(19) 1 calc R U P A 1 H78B H 1.0690 0.0559 0.8449 0.220 Uiso 0.612(19) 1 calc R U P A 1 C14B C 0.272(6) 0.126(5) 0.179(2) 0.15(2) Uani 0.388(19) 1 d D U P A 2 H14C H 0.3511 0.1063 0.1621 0.184 Uiso 0.388(19) 1 calc R U P A 2 H14D H 0.2598 0.1822 0.1912 0.184 Uiso 0.388(19) 1 calc R U P A 2 C54B C 0.770(6) 0.320(4) 0.6878(14) 0.212(15) Uani 0.388(19) 1 d D U P A 2 H54C H 0.7766 0.2588 0.6958 0.255 Uiso 0.388(19) 1 calc R U P A 2 H54D H 0.6851 0.3562 0.6927 0.255 Uiso 0.388(19) 1 calc R U P A 2 C59B C 0.773(11) 0.097(5) 0.4897(15) 0.196(14) Uani 0.388(19) 1 d D U P A 2 H59C H 0.7035 0.1494 0.4836 0.235 Uiso 0.388(19) 1 calc R U P A 2 H59D H 0.8413 0.0977 0.4678 0.235 Uiso 0.388(19) 1 calc R U P A 2 C76B C 0.616(6) 0.528(4) 0.905(4) 0.22(3) Uani 0.388(19) 1 d D U P A 2 H76D H 0.5546 0.5794 0.9171 0.335 Uiso 0.388(19) 1 calc R U P A 2 H76E H 0.6703 0.4989 0.9287 0.335 Uiso 0.388(19) 1 calc R U P A 2 H76F H 0.6606 0.5452 0.8788 0.335 Uiso 0.388(19) 1 calc R U P A 2 C78B C 1.063(3) 0.113(5) 0.816(2) 0.159(16) Uani 0.388(19) 1 d D U P A 2 H78C H 1.0889 0.0723 0.8430 0.190 Uiso 0.388(19) 1 calc R U P A 2 H78D H 1.1114 0.1520 0.8123 0.190 Uiso 0.388(19) 1 calc R U P A 2 C1 C 0.3383(13) 0.3014(10) 0.0960(4) 0.092(7) Uani 1 1 d G U . . . N1 N 0.3202(12) 0.2333(11) 0.0752(5) 0.076(5) Uani 1 1 d G U . . . C2 C 0.4066(17) 0.1877(8) 0.0420(5) 0.089(8) Uani 1 1 d G U . . . C3 C 0.5112(14) 0.2103(10) 0.0296(4) 0.086(7) Uani 1 1 d G U . . . H3 H 0.5690 0.1798 0.0074 0.104 Uiso 1 1 calc R U . . . C4 C 0.5293(12) 0.2784(12) 0.0504(6) 0.095(8) Uani 1 1 d G U . . . N2 N 0.4428(16) 0.3240(9) 0.0836(5) 0.089(6) Uani 1 1 d G U . . . C5 C 0.375(3) 0.1175(16) 0.0192(9) 0.147(14) Uani 1 1 d . . . . . H5A H 0.2994 0.1130 0.0331 0.220 Uiso 1 1 calc R U . . . H5B H 0.3684 0.1335 -0.0132 0.220 Uiso 1 1 calc R U . . . H5C H 0.4388 0.0619 0.0233 0.220 Uiso 1 1 calc R U . . . C6 C 0.628(3) 0.3152(18) 0.0391(9) 0.137(12) Uani 1 1 d . U . . . H6A H 0.6178 0.3616 0.0589 0.205 Uiso 1 1 calc R U . . . H6B H 0.7048 0.2699 0.0433 0.205 Uiso 1 1 calc R U . . . H6C H 0.6257 0.3382 0.0074 0.205 Uiso 1 1 calc R U . . . C7 C -0.1619(16) 0.2714(10) 0.1679(6) 0.116(10) Uani 1 1 d G U . . . N4 N -0.2741(17) 0.2741(10) 0.1903(5) 0.097(6) Uani 1 1 d G U . . . C8 C -0.3366(12) 0.2221(12) 0.1765(6) 0.089(7) Uani 1 1 d G U . . . C9 C -0.2869(18) 0.1674(10) 0.1404(7) 0.103(8) Uani 1 1 d G U . . . H9 H -0.3288 0.1326 0.1311 0.124 Uiso 1 1 calc R U . . . C10 C -0.1747(18) 0.1647(10) 0.1180(5) 0.104(9) Uani 1 1 d G U . . . N3 N -0.1122(12) 0.2167(12) 0.1318(6) 0.102(7) Uani 1 1 d G . . . . C11 C -0.455(2) 0.2322(19) 0.2030(9) 0.122(11) Uani 1 1 d . U . . . H11A H -0.4685 0.2738 0.2261 0.183 Uiso 1 1 calc R U . . . H11B H -0.5197 0.2528 0.1825 0.183 Uiso 1 1 calc R U . . . H11C H -0.4545 0.1764 0.2178 0.183 Uiso 1 1 calc R U . . . C12 C -0.116(3) 0.1058(16) 0.0801(9) 0.117(10) Uani 1 1 d . . . . . H12A H -0.0391 0.1138 0.0693 0.176 Uiso 1 1 calc R U . . . H12B H -0.1015 0.0457 0.0913 0.176 Uiso 1 1 calc R U . . . H12C H -0.1679 0.1198 0.0551 0.176 Uiso 1 1 calc R U . . . C13 C 0.169(3) 0.132(2) 0.1481(11) 0.151(11) Uani 1 1 d D U . . . H13A H 0.1387 0.0943 0.1320 0.181 Uiso 1 1 calc R U . A 1 H13B H 0.2570 0.1131 0.1418 0.181 Uiso 1 1 calc R U . A 1 C15 C 0.261(4) 0.057(3) 0.2184(16) 0.244(17) Uani 1 1 d D U . . . H15A H 0.2308 0.0150 0.2373 0.293 Uiso 1 1 calc R U . A 1 H15B H 0.2970 0.0275 0.1905 0.293 Uiso 1 1 calc R U . A 1 C16 C 0.376(4) 0.044(3) 0.2419(15) 0.25(2) Uani 1 1 d D U . . . H16A H 0.3809 0.0016 0.2678 0.378 Uiso 1 1 calc R U . . . H16B H 0.4454 0.0226 0.2204 0.378 Uiso 1 1 calc R U . . . H16C H 0.3739 0.0987 0.2526 0.378 Uiso 1 1 calc R U . . . C17 C 0.0379(18) 0.3052(14) 0.0520(7) 0.091(8) Uani 1 1 d D U . . . H17A H 0.1062 0.3145 0.0329 0.109 Uiso 1 1 calc R U . . . H17B H 0.0184 0.2586 0.0393 0.109 Uiso 1 1 calc R U . . . C18 C -0.071(2) 0.3885(14) 0.0489(7) 0.103(8) Uani 1 1 d D U . . . H18A H -0.0510 0.4366 0.0599 0.124 Uiso 1 1 calc R U . . . H18B H -0.1394 0.3807 0.0683 0.124 Uiso 1 1 calc R U . . . C19 C -0.105(2) 0.4104(16) -0.0009(8) 0.119(9) Uani 1 1 d D U . . . H19A H -0.1251 0.3625 -0.0117 0.143 Uiso 1 1 calc R U . . . H19B H -0.0355 0.4174 -0.0204 0.143 Uiso 1 1 calc R U . . . C20 C -0.213(2) 0.4947(16) -0.0044(10) 0.143(12) Uani 1 1 d D U . . . H20A H -0.2333 0.5078 -0.0360 0.214 Uiso 1 1 calc R U . . . H20B H -0.2815 0.4874 0.0145 0.214 Uiso 1 1 calc R U . . . H20C H -0.1921 0.5422 0.0059 0.214 Uiso 1 1 calc R U . . . C21 C 0.8058(14) 0.2763(9) 0.4052(6) 0.093(7) Uani 1 1 d G U . . . N5 N 0.7903(14) 0.2417(11) 0.3652(6) 0.089(6) Uani 1 1 d G U . . . C22 C 0.890(2) 0.1848(11) 0.3412(5) 0.107(9) Uani 1 1 d G U . . . C23 C 1.0060(16) 0.1626(10) 0.3572(7) 0.117(10) Uani 1 1 d G U . . . H23 H 1.0729 0.1245 0.3411 0.140 Uiso 1 1 calc R U . . . C24 C 1.0214(12) 0.1972(12) 0.3971(7) 0.095(9) Uani 1 1 d G . . . . N6 N 0.9213(18) 0.2540(11) 0.4211(5) 0.108(7) Uani 1 1 d G U . . . C25 C 0.869(3) 0.160(2) 0.2955(10) 0.186(17) Uani 1 1 d . . . . . H25A H 0.7827 0.1816 0.2913 0.279 Uiso 1 1 calc R U . . . H25B H 0.9111 0.1850 0.2712 0.279 Uiso 1 1 calc R U . . . H25C H 0.8980 0.0970 0.2946 0.279 Uiso 1 1 calc R U . . . C26 C 1.139(2) 0.1852(18) 0.4163(11) 0.145(13) Uani 1 1 d . . . . . H26A H 1.1237 0.2160 0.4441 0.217 Uiso 1 1 calc R U . . . H26B H 1.1797 0.1237 0.4232 0.217 Uiso 1 1 calc R U . . . H26C H 1.1888 0.2082 0.3941 0.217 Uiso 1 1 calc R U . . . C27 C 0.2378(15) 0.4115(11) 0.3916(6) 0.099(9) Uani 1 1 d G U . . . N8 N 0.1140(17) 0.4496(9) 0.4038(5) 0.090(6) Uani 1 1 d G U . . . C28 C 0.0282(12) 0.4402(10) 0.3767(7) 0.106(8) Uani 1 1 d G U . . . C29 C 0.0662(18) 0.3926(11) 0.3374(6) 0.108(9) Uani 1 1 d G U . . . H29 H 0.0087 0.3863 0.3193 0.130 Uiso 1 1 calc R U . . . C30 C 0.190(2) 0.3544(10) 0.3252(5) 0.103(9) Uani 1 1 d G U . . . N7 N 0.2758(13) 0.3639(10) 0.3523(7) 0.101(7) Uani 1 1 d G . . . . C31 C -0.099(2) 0.4861(18) 0.3919(9) 0.118(10) Uani 1 1 d . . . . . H31A H -0.1520 0.4760 0.3713 0.178 Uiso 1 1 calc R U . . . H31B H -0.1171 0.4643 0.4227 0.178 Uiso 1 1 calc R U . . . H31C H -0.1127 0.5481 0.3917 0.178 Uiso 1 1 calc R U . . . C32 C 0.236(3) 0.299(2) 0.2850(10) 0.159(14) Uani 1 1 d . . . . . H32A H 0.1685 0.2981 0.2692 0.239 Uiso 1 1 calc R U . . . H32B H 0.2875 0.3239 0.2642 0.239 Uiso 1 1 calc R U . . . H32C H 0.2823 0.2407 0.2955 0.239 Uiso 1 1 calc R U . . . C33 C 0.525(4) 0.1883(18) 0.3927(11) 0.182(13) Uani 1 1 d D U . . . H33A H 0.5922 0.1520 0.4102 0.218 Uiso 1 1 calc R U . . . H33B H 0.4491 0.1898 0.4104 0.218 Uiso 1 1 calc R U . . . C34 C 0.531(4) 0.150(2) 0.3468(10) 0.206(14) Uani 1 1 d D U . . . H34A H 0.5933 0.1638 0.3258 0.247 Uiso 1 1 calc R U . . . H34B H 0.4535 0.1754 0.3332 0.247 Uiso 1 1 calc R U . . . C35 C 0.562(3) 0.0503(18) 0.3539(13) 0.217(15) Uani 1 1 d D U . . . H35A H 0.5745 0.0249 0.3242 0.260 Uiso 1 1 calc R U . . . H35B H 0.6373 0.0253 0.3694 0.260 Uiso 1 1 calc R U . . . C36 C 0.462(4) 0.029(2) 0.3822(16) 0.25(2) Uani 1 1 d D U . . . H36A H 0.4816 -0.0335 0.3866 0.374 Uiso 1 1 calc R U . . . H36B H 0.4505 0.0539 0.4117 0.374 Uiso 1 1 calc R U . . . H36C H 0.3878 0.0535 0.3666 0.374 Uiso 1 1 calc R U . . . C37 C 0.552(2) 0.3924(16) 0.3138(8) 0.110(8) Uani 1 1 d D U . . . H37A H 0.5851 0.3491 0.2909 0.132 Uiso 1 1 calc R U . . . H37B H 0.4711 0.4292 0.3053 0.132 Uiso 1 1 calc R U . . . C38 C 0.633(3) 0.4489(19) 0.3131(9) 0.142(10) Uani 1 1 d D U . . . H38A H 0.7139 0.4113 0.3202 0.170 Uiso 1 1 calc R U . . . H38B H 0.6013 0.4898 0.3373 0.170 Uiso 1 1 calc R U . . . C39 C 0.642(3) 0.501(2) 0.2674(10) 0.167(11) Uani 1 1 d D U . . . H39A H 0.6623 0.4605 0.2428 0.200 Uiso 1 1 calc R U . . . H39B H 0.5620 0.5433 0.2624 0.200 Uiso 1 1 calc R U . . . C40 C 0.734(3) 0.549(2) 0.2634(12) 0.189(15) Uani 1 1 d D U . . . H40A H 0.7330 0.5794 0.2335 0.284 Uiso 1 1 calc R U . . . H40B H 0.7134 0.5903 0.2870 0.284 Uiso 1 1 calc R U . . . H40C H 0.8140 0.5073 0.2674 0.284 Uiso 1 1 calc R U . . . C41 C 0.6040(14) 0.1920(10) 0.6612(6) 0.093(8) Uani 1 1 d G U . . . N12 N 0.4956(19) 0.1834(10) 0.6821(5) 0.108(7) Uani 1 1 d G U . . . C42 C 0.3844(15) 0.2381(13) 0.6670(6) 0.105(9) Uani 1 1 d G U . . . C43 C 0.3815(15) 0.3014(12) 0.6310(7) 0.123(9) Uani 1 1 d G U . . . H43 H 0.3071 0.3381 0.6209 0.148 Uiso 1 1 calc R U . . . C44 C 0.490(2) 0.3100(10) 0.6101(5) 0.107(8) Uani 1 1 d G U . . . N11 N 0.6011(15) 0.2553(12) 0.6252(5) 0.100(7) Uani 1 1 d G U . . . C45 C 0.283(3) 0.222(2) 0.6940(12) 0.172(15) Uani 1 1 d . . . . . H45A H 0.2084 0.2605 0.6827 0.258 Uiso 1 1 calc R U . . . H45B H 0.2881 0.1618 0.6916 0.258 Uiso 1 1 calc R U . . . H45C H 0.2863 0.2318 0.7258 0.258 Uiso 1 1 calc R U . . . C46 C 0.497(3) 0.3796(18) 0.5718(10) 0.154(13) Uani 1 1 d . . . . . H46A H 0.5809 0.3729 0.5627 0.231 Uiso 1 1 calc R U . . . H46B H 0.4577 0.3727 0.5456 0.231 Uiso 1 1 calc R U . . . H46C H 0.4565 0.4371 0.5828 0.231 Uiso 1 1 calc R U . . . C47 C 1.134(2) 0.1715(12) 0.5883(5) 0.098(9) Uani 1 1 d G . . . . N9 N 1.0476(14) 0.2442(14) 0.5681(6) 0.097(7) Uani 1 1 d G . . . . C48 C 1.0850(19) 0.2985(10) 0.5344(6) 0.097(9) Uani 1 1 d G U . . . C49 C 1.208(2) 0.2803(12) 0.5210(5) 0.129(11) Uani 1 1 d G U . . . H49 H 1.2334 0.3167 0.4985 0.155 Uiso 1 1 calc R U . . . C50 C 1.2944(14) 0.2077(14) 0.5412(7) 0.106(10) Uani 1 1 d G U . . . N10 N 1.2570(18) 0.1533(10) 0.5749(6) 0.112(8) Uani 1 1 d G . . . . C51 C 0.983(3) 0.3750(17) 0.5166(10) 0.151(14) Uani 1 1 d . . . . . H51A H 1.0157 0.4095 0.4936 0.227 Uiso 1 1 calc R U . . . H51B H 0.9272 0.3540 0.5031 0.227 Uiso 1 1 calc R U . . . H51C H 0.9413 0.4107 0.5417 0.227 Uiso 1 1 calc R U . . . C52 C 1.426(3) 0.173(2) 0.5274(11) 0.178(16) Uani 1 1 d . . . . . H52A H 1.4645 0.1226 0.5472 0.267 Uiso 1 1 calc R U . . . H52B H 1.4382 0.1573 0.4959 0.267 Uiso 1 1 calc R U . . . H52C H 1.4625 0.2180 0.5301 0.267 Uiso 1 1 calc R U . . . C53 C 0.818(3) 0.332(2) 0.6375(11) 0.159(11) Uani 1 1 d D U . . . H53A H 0.8092 0.3726 0.6104 0.191 Uiso 1 1 calc R U . A 1 H53B H 0.7394 0.3472 0.6550 0.191 Uiso 1 1 calc R U . A 1 C55 C 0.852(4) 0.349(2) 0.7168(11) 0.261(16) Uani 1 1 d D U . . . H55A H 0.7988 0.3129 0.7202 0.313 Uiso 1 1 calc R U . A 1 H55B H 0.9150 0.3245 0.7381 0.313 Uiso 1 1 calc R U . A 1 C56 C 0.778(4) 0.443(2) 0.7272(13) 0.29(2) Uani 1 1 d D U . . . H56A H 0.7419 0.4439 0.7583 0.434 Uiso 1 1 calc R U . . . H56B H 0.8315 0.4776 0.7239 0.434 Uiso 1 1 calc R U . . . H56C H 0.7157 0.4661 0.7061 0.434 Uiso 1 1 calc R U . . . C57 C 0.819(2) 0.1772(18) 0.5465(8) 0.105(8) Uani 1 1 d D U . . . H57A H 0.7438 0.2221 0.5377 0.127 Uiso 1 1 calc R U . . . H57B H 0.8838 0.1843 0.5247 0.127 Uiso 1 1 calc R U . . . C58 C 0.807(4) 0.089(2) 0.5401(10) 0.181(11) Uani 1 1 d D U . . . H58A H 0.7273 0.0881 0.5530 0.217 Uiso 1 1 calc R U . A 1 H58B H 0.8684 0.0433 0.5566 0.217 Uiso 1 1 calc R U . A 1 C60 C 0.741(4) 0.013(2) 0.4894(13) 0.219(14) Uani 1 1 d D U . . . H60A H 0.7416 -0.0046 0.4588 0.328 Uiso 1 1 calc R U . A 1 H60B H 0.7725 -0.0385 0.5098 0.328 Uiso 1 1 calc R U . A 1 H60C H 0.6596 0.0454 0.5003 0.328 Uiso 1 1 calc R U . A 1 C61 C 0.6445(13) 0.1107(10) 0.8958(5) 0.090(7) Uani 1 1 d G U . . . N16 N 0.5562(16) 0.0698(9) 0.9051(5) 0.085(6) Uani 1 1 d G U . . . C62 C 0.4608(13) 0.0892(11) 0.8766(6) 0.090(8) Uani 1 1 d G U . . . C63 C 0.4536(14) 0.1494(12) 0.8387(6) 0.117(9) Uani 1 1 d G U . . . H63 H 0.3898 0.1624 0.8196 0.140 Uiso 1 1 calc R U . . . C64 C 0.5418(18) 0.1903(9) 0.8294(5) 0.095(8) Uani 1 1 d G U . . . N15 N 0.6373(14) 0.1709(10) 0.8579(6) 0.084(6) Uani 1 1 d G U . . . C65 C 0.550(3) 0.246(2) 0.7898(9) 0.136(11) Uani 1 1 d . . . . . H65A H 0.6180 0.2664 0.7911 0.204 Uiso 1 1 calc R U . . . H65B H 0.5607 0.2145 0.7625 0.204 Uiso 1 1 calc R U . . . H65C H 0.4760 0.2958 0.7889 0.204 Uiso 1 1 calc R U . . . C66 C 0.375(3) 0.0390(19) 0.8879(11) 0.151(14) Uani 1 1 d . . . . . H66A H 0.3974 0.0015 0.9153 0.227 Uiso 1 1 calc R U . . . H66B H 0.2936 0.0791 0.8929 0.227 Uiso 1 1 calc R U . . . H66C H 0.3785 0.0037 0.8627 0.227 Uiso 1 1 calc R U . . . C67 C 1.0869(18) 0.2394(9) 0.9168(6) 0.079(8) Uani 1 1 d G . . . . N13 N 1.0252(12) 0.2967(12) 0.8820(6) 0.088(6) Uani 1 1 d G . . . . C68 C 1.0686(17) 0.3627(10) 0.8616(5) 0.103(9) Uani 1 1 d G U . . . C69 C 1.1738(18) 0.3715(11) 0.8760(6) 0.108(9) Uani 1 1 d G U . . . H69 H 1.2028 0.4157 0.8624 0.129 Uiso 1 1 calc R U . . . C70 C 1.2355(13) 0.3142(13) 0.9109(7) 0.087(8) Uani 1 1 d G U . . . N14 N 1.1921(17) 0.2481(11) 0.9313(5) 0.107(8) Uani 1 1 d G . . . . C71 C 1.352(2) 0.3141(18) 0.9272(10) 0.126(11) Uani 1 1 d . . . . . H71A H 1.3771 0.2688 0.9514 0.189 Uiso 1 1 calc R U . . . H71B H 1.4139 0.3034 0.9019 0.189 Uiso 1 1 calc R U . . . H71C H 1.3410 0.3702 0.9388 0.189 Uiso 1 1 calc R U . . . C72 C 0.998(3) 0.416(2) 0.8256(11) 0.159(14) Uani 1 1 d . . . . . H72A H 1.0325 0.4596 0.8131 0.239 Uiso 1 1 calc R U . . . H72B H 0.9970 0.3789 0.8016 0.239 Uiso 1 1 calc R U . . . H72C H 0.9154 0.4435 0.8380 0.239 Uiso 1 1 calc R U . . . C73 C 0.736(3) 0.3241(15) 0.9070(9) 0.127(10) Uani 1 1 d D U . . . H73A H 0.6828 0.3148 0.9334 0.153 Uiso 1 1 calc R U . . . H73B H 0.7851 0.3554 0.9176 0.153 Uiso 1 1 calc R U . . . C74 C 0.656(3) 0.3854(17) 0.8725(10) 0.162(11) Uani 1 1 d D U . . . H74A H 0.6180 0.3517 0.8569 0.194 Uiso 1 1 calc R U . . . H74B H 0.7071 0.4064 0.8494 0.194 Uiso 1 1 calc R U . . . C75 C 0.554(3) 0.4656(19) 0.8911(10) 0.168(12) Uani 1 1 d D U . . . H75A H 0.4969 0.4471 0.9128 0.202 Uiso 1 1 calc R U . A 1 H75B H 0.5881 0.5012 0.9068 0.202 Uiso 1 1 calc R U . A 1 C77 C 0.926(2) 0.1656(17) 0.8228(8) 0.122(9) Uani 1 1 d D U . . . H77A H 0.8596 0.1742 0.8034 0.146 Uiso 1 1 calc R U . A 1 H77B H 0.9716 0.2038 0.8099 0.146 Uiso 1 1 calc R U . A 1 C79 C 1.075(3) 0.063(2) 0.7727(10) 0.202(14) Uani 1 1 d D U . . . H79A H 1.0391 0.0311 0.7555 0.242 Uiso 1 1 calc R U . A 1 H79B H 1.0532 0.1226 0.7586 0.242 Uiso 1 1 calc R U . A 1 C80 C 1.212(3) 0.023(2) 0.7637(12) 0.217(18) Uani 1 1 d D U . . . H80A H 1.2336 0.0257 0.7310 0.325 Uiso 1 1 calc R U . . . H80B H 1.2521 0.0551 0.7787 0.325 Uiso 1 1 calc R U . . . H80C H 1.2379 -0.0372 0.7757 0.325 Uiso 1 1 calc R U . . . Se1 Se -0.0792(3) 0.3377(2) 0.18285(10) 0.1106(11) Uani 1 1 d . . . . . Se2 Se 0.2253(3) 0.3549(2) 0.14043(10) 0.1074(11) Uani 1 1 d . . . . . Se3 Se 0.6756(3) 0.34832(19) 0.43685(9) 0.0984(10) Uani 1 1 d . . . . . Se4 Se 0.3468(3) 0.42226(19) 0.42819(10) 0.0995(10) Uani 1 1 d . . . . . Se5 Se 0.7534(3) 0.1172(2) 0.67481(11) 0.1173(11) Uani 1 1 d . . . . . Se6 Se 1.0726(3) 0.1056(2) 0.63236(10) 0.1111(11) Uani 1 1 d . . . . . Sn1 Sn 0.09461(16) 0.26150(12) 0.12164(6) 0.0810(6) Uani 1 1 d . . . . . Sn2 Sn 0.53404(17) 0.32568(12) 0.38010(6) 0.0869(6) Uani 1 1 d . . . . . Sn3 Sn 0.85412(17) 0.20495(12) 0.61398(6) 0.0855(6) Uani 1 1 d . . . . . Se7 Se 0.7671(2) 0.08672(18) 0.93368(9) 0.0919(9) Uani 1 1 d . . . . . Se8 Se 1.0297(3) 0.15737(18) 0.94391(10) 0.0936(9) Uani 1 1 d . . . . . Sn4 Sn 0.85263(16) 0.20230(11) 0.89030(6) 0.0799(6) Uani 1 1 d . . . . . 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 C14A 0.19(3) 0.23(3) 0.18(3) 0.04(3) 0.01(3) -0.09(3) C54A 0.20(3) 0.25(3) 0.23(3) 0.03(3) -0.08(2) -0.08(3) C59A 0.29(3) 0.19(3) 0.14(2) -0.05(2) -0.02(3) -0.08(2) C76A 0.17(4) 0.08(3) 0.21(4) -0.03(3) -0.06(3) -0.06(2) C78A 0.19(3) 0.19(3) 0.13(2) -0.07(2) 0.02(2) 0.00(2) C14B 0.15(4) 0.17(4) 0.16(4) 0.03(4) 0.04(4) -0.11(4) C54B 0.20(3) 0.23(3) 0.19(3) 0.05(3) -0.03(3) -0.05(3) C59B 0.26(3) 0.21(3) 0.14(2) -0.07(2) -0.03(2) -0.08(3) C76B 0.24(6) 0.16(5) 0.29(7) -0.09(5) -0.05(6) -0.06(4) C78B 0.14(2) 0.19(3) 0.12(2) -0.04(2) 0.02(2) -0.01(2) C1 0.102(18) 0.124(18) 0.063(15) -0.029(14) -0.021(14) -0.045(15) N1 0.064(12) 0.124(15) 0.048(11) -0.018(10) 0.008(9) -0.044(11) C2 0.12(2) 0.097(17) 0.035(13) 0.024(13) -0.005(14) -0.029(16) C3 0.107(19) 0.088(17) 0.055(14) -0.005(13) 0.017(14) -0.026(15) C4 0.081(16) 0.109(19) 0.077(17) 0.016(14) 0.023(14) -0.022(14) N2 0.082(14) 0.111(14) 0.074(14) -0.015(11) -0.020(12) -0.025(12) C5 0.26(4) 0.09(2) 0.08(2) -0.029(17) 0.00(2) -0.03(2) C6 0.17(3) 0.15(3) 0.11(2) -0.02(2) 0.06(2) -0.10(2) C7 0.068(19) 0.15(2) 0.11(2) -0.04(2) -0.024(16) 0.003(19) N4 0.092(16) 0.107(15) 0.092(15) -0.016(12) -0.013(13) -0.028(13) C8 0.057(14) 0.107(18) 0.095(18) 0.009(15) 0.002(12) -0.023(14) C9 0.078(18) 0.108(18) 0.11(2) -0.012(16) -0.006(15) -0.007(16) C10 0.11(2) 0.066(17) 0.12(2) -0.011(17) -0.022(19) 0.001(18) N3 0.14(2) 0.085(16) 0.077(16) -0.011(13) -0.031(15) -0.017(15) C11 0.064(16) 0.20(3) 0.10(2) 0.05(2) -0.002(14) -0.06(2) C12 0.12(2) 0.10(2) 0.14(3) -0.05(2) -0.02(2) -0.029(18) C13 0.13(3) 0.21(3) 0.17(3) 0.01(2) -0.01(2) -0.14(2) C15 0.25(4) 0.26(4) 0.21(3) 0.04(3) -0.04(3) -0.07(3) C16 0.29(5) 0.20(3) 0.27(5) 0.13(3) -0.09(4) -0.10(4) C17 0.043(14) 0.138(19) 0.077(15) -0.023(14) -0.031(12) 0.001(11) C18 0.071(15) 0.130(18) 0.095(14) -0.011(14) -0.032(13) -0.006(11) C19 0.115(19) 0.124(19) 0.097(16) 0.002(16) -0.051(16) 0.001(13) C20 0.12(2) 0.14(2) 0.14(2) 0.017(19) -0.047(19) 0.007(15) C21 0.076(17) 0.083(16) 0.13(2) 0.005(15) -0.023(16) -0.031(14) N5 0.090(15) 0.096(15) 0.094(15) -0.011(12) -0.027(12) -0.040(12) C22 0.10(2) 0.107(19) 0.11(2) 0.005(16) 0.006(18) -0.033(18) C23 0.12(3) 0.13(2) 0.09(2) -0.011(18) -0.005(19) -0.03(2) C24 0.048(18) 0.09(2) 0.12(2) 0.021(18) 0.035(18) -0.001(16) N6 0.108(18) 0.108(16) 0.099(16) 0.012(13) -0.033(15) -0.018(15) C25 0.15(3) 0.29(5) 0.12(3) -0.12(3) 0.03(2) -0.06(3) C26 0.06(2) 0.13(3) 0.22(4) 0.00(2) -0.06(2) 0.015(18) C27 0.060(17) 0.091(19) 0.11(2) 0.032(17) 0.009(17) 0.004(15) N8 0.090(15) 0.077(13) 0.100(15) -0.003(11) -0.024(13) -0.019(12) C28 0.11(2) 0.073(17) 0.13(2) 0.025(15) -0.059(18) -0.025(16) C29 0.109(19) 0.10(2) 0.11(2) -0.001(16) -0.026(18) -0.026(17) C30 0.10(2) 0.087(19) 0.10(2) 0.017(17) -0.01(2) -0.016(18) N7 0.075(16) 0.128(19) 0.085(17) -0.012(15) 0.014(14) -0.015(14) C31 0.038(16) 0.18(3) 0.14(3) 0.01(2) -0.020(17) -0.034(18) C32 0.17(3) 0.18(3) 0.10(2) -0.06(2) -0.01(2) -0.02(3) C33 0.19(3) 0.19(3) 0.14(3) 0.05(2) -0.03(3) -0.05(3) C34 0.22(3) 0.18(2) 0.18(3) 0.02(2) -0.01(3) -0.03(2) C35 0.20(3) 0.18(2) 0.22(3) 0.03(3) -0.01(3) -0.01(3) C36 0.22(4) 0.21(3) 0.27(5) 0.06(4) 0.00(3) -0.03(3) C37 0.12(2) 0.11(2) 0.097(18) -0.003(15) -0.042(16) -0.020(14) C38 0.18(3) 0.13(2) 0.12(2) 0.014(16) -0.02(2) -0.066(16) C39 0.21(3) 0.19(3) 0.11(2) 0.022(18) -0.03(2) -0.08(2) C40 0.16(3) 0.21(4) 0.18(3) 0.06(3) 0.02(3) -0.06(2) C41 0.104(18) 0.126(18) 0.063(15) -0.010(14) 0.042(14) -0.072(16) N12 0.133(18) 0.141(17) 0.079(14) -0.014(13) -0.002(14) -0.084(15) C42 0.12(2) 0.15(2) 0.063(17) -0.037(16) -0.002(17) -0.058(19) C43 0.12(2) 0.17(2) 0.079(19) -0.020(17) 0.014(17) -0.040(19) C44 0.12(2) 0.16(2) 0.043(15) -0.025(15) -0.001(15) -0.051(19) N11 0.122(17) 0.129(18) 0.065(13) -0.019(12) -0.013(13) -0.059(14) C45 0.11(3) 0.22(4) 0.20(4) -0.02(3) 0.01(3) -0.08(3) C46 0.16(3) 0.13(3) 0.13(3) 0.04(2) 0.00(2) 0.00(2) C47 0.15(3) 0.08(2) 0.042(16) 0.001(14) 0.005(19) -0.02(2) N9 0.12(2) 0.118(19) 0.062(15) -0.004(13) -0.019(14) -0.047(17) C48 0.18(3) 0.085(18) 0.038(15) -0.017(14) 0.013(17) -0.06(2) C49 0.21(3) 0.13(2) 0.053(16) -0.019(15) 0.043(19) -0.07(2) C50 0.20(3) 0.08(2) 0.048(16) -0.015(14) 0.039(18) -0.07(2) N10 0.091(18) 0.16(2) 0.089(18) -0.043(17) -0.010(14) -0.041(17) C51 0.26(4) 0.07(2) 0.12(3) 0.024(19) -0.01(3) -0.06(2) C52 0.12(3) 0.26(4) 0.16(3) -0.04(3) 0.08(2) -0.08(3) C53 0.11(2) 0.18(2) 0.20(3) 0.03(2) -0.02(2) -0.07(2) C55 0.27(3) 0.27(3) 0.22(3) 0.01(3) -0.07(2) -0.05(3) C56 0.34(5) 0.25(3) 0.25(4) 0.01(3) -0.10(3) -0.04(3) C57 0.063(16) 0.20(2) 0.083(16) -0.015(17) -0.008(14) -0.073(18) C58 0.24(3) 0.20(2) 0.127(17) -0.03(2) -0.012(19) -0.10(2) C60 0.28(3) 0.21(3) 0.18(2) -0.06(2) -0.04(3) -0.09(2) C61 0.093(17) 0.080(17) 0.100(18) -0.022(14) -0.029(15) -0.020(14) N16 0.079(14) 0.101(14) 0.094(14) -0.016(11) -0.002(12) -0.054(12) C62 0.083(17) 0.102(18) 0.075(17) -0.042(14) -0.011(15) -0.008(16) C63 0.12(2) 0.12(2) 0.095(19) -0.015(16) -0.026(18) -0.015(17) C64 0.12(2) 0.103(18) 0.069(16) -0.020(15) -0.025(16) -0.029(16) N15 0.092(14) 0.074(13) 0.076(14) 0.001(11) -0.015(12) -0.011(11) C65 0.13(3) 0.17(3) 0.08(2) 0.01(2) 0.00(2) -0.03(2) C66 0.09(2) 0.16(3) 0.23(4) 0.00(3) -0.05(3) -0.08(2) C67 0.09(2) 0.09(2) 0.042(15) 0.011(14) -0.021(14) -0.004(17) N13 0.085(16) 0.064(14) 0.115(19) -0.014(13) -0.005(14) -0.022(13) C68 0.11(2) 0.088(19) 0.11(2) -0.006(17) -0.029(19) -0.024(19) C69 0.11(2) 0.097(18) 0.12(2) -0.010(16) -0.009(17) -0.039(17) C70 0.08(2) 0.11(2) 0.082(19) -0.029(16) 0.000(15) -0.039(18) N14 0.12(2) 0.085(16) 0.13(2) -0.004(14) -0.049(17) -0.037(15) C71 0.09(2) 0.16(3) 0.15(3) -0.04(2) 0.02(2) -0.07(2) C72 0.10(3) 0.18(3) 0.18(3) 0.04(3) -0.04(2) -0.03(2) C73 0.18(3) 0.075(18) 0.12(2) -0.055(16) -0.002(18) -0.023(16) C74 0.18(3) 0.12(2) 0.17(3) -0.042(17) -0.033(19) -0.022(16) C75 0.18(3) 0.10(2) 0.22(3) -0.048(19) -0.05(2) -0.017(16) C77 0.116(19) 0.17(2) 0.083(17) -0.069(16) 0.006(15) -0.041(16) C79 0.20(2) 0.21(3) 0.129(19) -0.067(19) 0.03(2) 0.02(2) C80 0.20(3) 0.24(4) 0.16(3) -0.07(3) 0.04(2) 0.00(3) Se1 0.103(2) 0.143(3) 0.100(2) -0.057(2) 0.0203(18) -0.055(2) Se2 0.101(2) 0.140(3) 0.098(2) -0.054(2) 0.0167(18) -0.057(2) Se3 0.084(2) 0.125(2) 0.082(2) -0.0181(17) -0.0147(16) -0.0226(18) Se4 0.081(2) 0.122(2) 0.098(2) -0.0143(18) -0.0126(17) -0.0337(18) Se5 0.104(3) 0.141(3) 0.104(2) 0.029(2) -0.0130(19) -0.044(2) Se6 0.088(2) 0.138(3) 0.095(2) 0.029(2) -0.0130(18) -0.0285(19) Sn1 0.0805(13) 0.0998(14) 0.0655(12) -0.0190(10) -0.0037(10) -0.0301(11) Sn2 0.0882(14) 0.0984(14) 0.0752(13) 0.0026(11) -0.0153(11) -0.0315(11) Sn3 0.0926(14) 0.1008(14) 0.0642(12) -0.0032(10) -0.0127(10) -0.0319(11) Se7 0.078(2) 0.108(2) 0.090(2) -0.0030(17) -0.0144(16) -0.0294(17) Se8 0.095(2) 0.100(2) 0.093(2) 0.0001(17) -0.0227(17) -0.0381(18) Sn4 0.0787(13) 0.0896(13) 0.0687(12) -0.0169(10) -0.0060(10) -0.0206(10) 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 C13 C14A C15 104(3) C13 C14A H14A 110.9 C15 C14A H14A 110.9 C13 C14A H14B 110.9 C15 C14A H14B 110.9 H14A C14A H14B 108.9 C55 C54A C53 105.3(16) C55 C54A H54A 110.7 C53 C54A H54A 110.7 C55 C54A H54B 110.7 C53 C54A H54B 110.7 H54A C54A H54B 108.8 C60 C59A C58 99(3) C60 C59A H59A 111.9 C58 C59A H59A 111.9 C60 C59A H59B 111.9 C58 C59A H59B 111.9 H59A C59A H59B 109.6 C75 C76A H76A 109.5 C75 C76A H76B 109.5 H76A C76A H76B 109.5 C75 C76A H76C 109.5 H76A C76A H76C 109.5 H76B C76A H76C 109.5 C77 C78A C79 104.4(15) C77 C78A H78A 110.9 C79 C78A H78A 110.9 C77 C78A H78B 110.9 C79 C78A H78B 110.9 H78A C78A H78B 108.9 C15 C14B C13 104(3) C15 C14B H14C 111.0 C13 C14B H14C 111.0 C15 C14B H14D 111.0 C13 C14B H14D 111.0 H14C C14B H14D 109.0 C53 C54B C55 104.8(16) C53 C54B H54C 110.8 C55 C54B H54C 110.8 C53 C54B H54D 110.8 C55 C54B H54D 110.8 H54C C54B H54D 108.9 C60 C59B C58 99(3) C60 C59B H59C 111.9 C58 C59B H59C 111.9 C60 C59B H59D 111.9 C58 C59B H59D 111.9 H59C C59B H59D 109.6 C75 C76B H76D 109.5 C75 C76B H76E 109.5 H76D C76B H76E 109.5 C75 C76B H76F 109.5 H76D C76B H76F 109.5 H76E C76B H76F 109.5 C77 C78B C79 104.3(15) C77 C78B H78C 110.9 C79 C78B H78C 110.9 C77 C78B H78D 110.9 C79 C78B H78D 110.9 H78C C78B H78D 108.9 N1 C1 N2 120.0 N1 C1 Se2 117.6(11) N2 C1 Se2 122.3(11) C1 N1 C2 120.0 C1 N1 Sn1 92.0(9) C2 N1 Sn1 147.8(9) C3 C2 N1 120.0 C3 C2 C5 123.8(17) N1 C2 C5 116.2(17) C4 C3 C2 120.0 C4 C3 H3 120.0 C2 C3 H3 120.0 C3 C4 N2 120.0 C3 C4 C6 127.2(17) N2 C4 C6 112.6(17) C4 N2 C1 120.0 C2 C5 H5A 109.5 C2 C5 H5B 109.5 H5A C5 H5B 109.5 C2 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C4 C6 H6A 109.5 C4 C6 H6B 109.5 H6A C6 H6B 109.5 C4 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 N4 C7 N3 120.0 N4 C7 Se1 122.3(14) N3 C7 Se1 117.7(14) C7 N4 C8 120.0 C9 C8 N4 120.0 C9 C8 C11 125.8(19) N4 C8 C11 114.2(19) C8 C9 C10 120.0 C8 C9 H9 120.0 C10 C9 H9 120.0 C9 C10 N3 120.0 C9 C10 C12 122.4(18) N3 C10 C12 117.6(18) C10 N3 C7 120.0 C10 N3 Sn1 147.3(11) C7 N3 Sn1 92.6(11) C8 C11 H11A 109.5 C8 C11 H11B 109.5 H11A C11 H11B 109.5 C8 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C10 C12 H12A 109.5 C10 C12 H12B 109.5 H12A C12 H12B 109.5 C10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C14A C13 Sn1 114(3) C14B C13 Sn1 109(3) C14A C13 H13A 108.8 Sn1 C13 H13A 108.8 C14A C13 H13B 108.8 Sn1 C13 H13B 108.8 H13A C13 H13B 107.7 C16 C15 C14B 100(3) C16 C15 C14A 150(5) C16 C15 H15A 99.0 C14A C15 H15A 99.0 C16 C15 H15B 99.0 C14A C15 H15B 99.0 H15A C15 H15B 103.9 C15 C16 H16A 109.5 C15 C16 H16B 109.5 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C18 C17 Sn1 114.8(14) C18 C17 H17A 108.6 Sn1 C17 H17A 108.6 C18 C17 H17B 108.6 Sn1 C17 H17B 108.6 H17A C17 H17B 107.6 C17 C18 C19 110.0(18) C17 C18 H18A 109.7 C19 C18 H18A 109.7 C17 C18 H18B 109.7 C19 C18 H18B 109.7 H18A C18 H18B 108.2 C18 C19 C20 110(2) C18 C19 H19A 109.6 C20 C19 H19A 109.6 C18 C19 H19B 109.6 C20 C19 H19B 109.6 H19A C19 H19B 108.1 C19 C20 H20A 109.5 C19 C20 H20B 109.5 H20A C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 N5 C21 N6 120.0 N5 C21 Se3 120.0(12) N6 C21 Se3 120.0(12) C21 N5 C22 120.0 C21 N5 Sn2 88.9(10) C22 N5 Sn2 150.8(10) C23 C22 N5 120.0 C23 C22 C25 123(2) N5 C22 C25 116(2) C24 C23 C22 120.0 C24 C23 H23 120.0 C22 C23 H23 120.0 C23 C24 N6 120.0 C23 C24 C26 126.3(19) N6 C24 C26 113.6(19) C24 N6 C21 120.0 C22 C25 H25A 109.5 C22 C25 H25B 109.5 H25A C25 H25B 109.5 C22 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 H26A C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 N8 C27 N7 120.0 N8 C27 Se4 119.0(13) N7 C27 Se4 121.0(13) C28 N8 C27 120.0 N8 C28 C29 120.0 N8 C28 C31 115.2(17) C29 C28 C31 124.8(17) C30 C29 C28 120.0 C30 C29 H29 120.0 C28 C29 H29 120.0 N7 C30 C29 120.0 N7 C30 C32 117(2) C29 C30 C32 122(2) C30 N7 C27 120.0 C30 N7 Sn2 153.8(10) C27 N7 Sn2 86.1(10) C28 C31 H31A 109.5 C28 C31 H31B 109.5 H31A C31 H31B 109.5 C28 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C30 C32 H32A 109.5 C30 C32 H32B 109.5 H32A C32 H32B 109.5 C30 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C34 C33 Sn2 109(2) C34 C33 H33A 109.8 Sn2 C33 H33A 109.8 C34 C33 H33B 109.8 Sn2 C33 H33B 109.8 H33A C33 H33B 108.3 C33 C34 C35 109.7(17) C33 C34 H34A 109.7 C35 C34 H34A 109.7 C33 C34 H34B 109.7 C35 C34 H34B 109.7 H34A C34 H34B 108.2 C36 C35 C34 109.7(18) C36 C35 H35A 109.7 C34 C35 H35A 109.7 C36 C35 H35B 109.7 C34 C35 H35B 109.7 H35A C35 H35B 108.2 C35 C36 H36A 109.5 C35 C36 H36B 109.5 H36A C36 H36B 109.5 C35 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C38 C37 Sn2 113.0(16) C38 C37 H37A 109.0 Sn2 C37 H37A 109.0 C38 C37 H37B 109.0 Sn2 C37 H37B 109.0 H37A C37 H37B 107.8 C37 C38 C39 114(2) C37 C38 H38A 108.7 C39 C38 H38A 108.7 C37 C38 H38B 108.7 C39 C38 H38B 108.7 H38A C38 H38B 107.6 C40 C39 C38 116(3) C40 C39 H39A 108.4 C38 C39 H39A 108.4 C40 C39 H39B 108.4 C38 C39 H39B 108.4 H39A C39 H39B 107.4 C39 C40 H40A 109.5 C39 C40 H40B 109.5 H40A C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 N12 C41 N11 120.0 N12 C41 Se5 123.1(12) N11 C41 Se5 116.7(12) C42 N12 C41 120.0 N12 C42 C43 120.0 N12 C42 C45 112(2) C43 C42 C45 128(2) C44 C43 C42 120.0 C44 C43 H43 120.0 C42 C43 H43 120.0 C43 C44 N11 120.0 C43 C44 C46 124.2(19) N11 C44 C46 115.7(19) C44 N11 C41 120.0 C44 N11 Sn3 147.5(10) C41 N11 Sn3 92.4(10) C42 C45 H45A 109.5 C42 C45 H45B 109.5 H45A C45 H45B 109.5 C42 C45 H45C 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C44 C46 H46A 109.5 C44 C46 H46B 109.5 H46A C46 H46B 109.5 C44 C46 H46C 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 N9 C47 N10 120.0 N9 C47 Se6 115.7(15) N10 C47 Se6 124.3(15) C48 N9 C47 120.0 C48 N9 Sn3 146.2(12) C47 N9 Sn3 93.6(12) N9 C48 C49 120.0 N9 C48 C51 114(2) C49 C48 C51 126(2) C50 C49 C48 120.0 C50 C49 H49 120.0 C48 C49 H49 120.0 C49 C50 N10 120.0 C49 C50 C52 127(2) N10 C50 C52 113(2) C50 N10 C47 120.0 C48 C51 H51A 109.5 C48 C51 H51B 109.5 H51A C51 H51B 109.5 C48 C51 H51C 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 C50 C52 H52A 109.5 C50 C52 H52B 109.5 H52A C52 H52B 109.5 C50 C52 H52C 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 C54B C53 Sn3 102(3) C54A C53 Sn3 120(3) C54A C53 H53A 107.3 Sn3 C53 H53A 107.3 C54A C53 H53B 107.3 Sn3 C53 H53B 107.3 H53A C53 H53B 106.9 C56 C55 C54A 108.1(17) C56 C55 C54B 104.9(17) C56 C55 H55A 110.1 C54A C55 H55A 110.1 C56 C55 H55B 110.1 C54A C55 H55B 110.1 H55A C55 H55B 108.4 C55 C56 H56A 109.5 C55 C56 H56B 109.5 H56A C56 H56B 109.5 C55 C56 H56C 109.5 H56A C56 H56C 109.5 H56B C56 H56C 109.5 C58 C57 Sn3 119.1(19) C58 C57 H57A 107.5 Sn3 C57 H57A 107.5 C58 C57 H57B 107.5 Sn3 C57 H57B 107.5 H57A C57 H57B 107.0 C57 C58 C59B 104(3) C57 C58 C59A 111(3) C57 C58 H58A 109.4 C59A C58 H58A 109.4 C57 C58 H58B 109.4 C59A C58 H58B 109.4 H58A C58 H58B 108.0 C59A C60 H60A 109.5 C59A C60 H60B 109.5 H60A C60 H60B 109.5 C59A C60 H60C 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 N16 C61 N15 120.0 N16 C61 Se7 119.8(11) N15 C61 Se7 120.2(11) C62 N16 C61 120.0 C63 C62 N16 120.0 C63 C62 C66 123.9(18) N16 C62 C66 116.0(18) C64 C63 C62 120.0 C64 C63 H63 120.0 C62 C63 H63 120.0 C63 C64 N15 120.0 C63 C64 C65 124.8(19) N15 C64 C65 115.0(19) C64 N15 C61 120.0 C64 N15 Sn4 152.5(9) C61 N15 Sn4 87.1(9) C64 C65 H65A 109.5 C64 C65 H65B 109.5 H65A C65 H65B 109.5 C64 C65 H65C 109.5 H65A C65 H65C 109.5 H65B C65 H65C 109.5 C62 C66 H66A 109.5 C62 C66 H66B 109.5 H66A C66 H66B 109.5 C62 C66 H66C 109.5 H66A C66 H66C 109.5 H66B C66 H66C 109.5 N13 C67 N14 120.0 N13 C67 Se8 120.1(14) N14 C67 Se8 119.8(14) C67 N13 C68 120.0 C67 N13 Sn4 88.4(11) C68 N13 Sn4 151.6(11) N13 C68 C69 120.0 N13 C68 C72 113.9(19) C69 C68 C72 126.1(19) C70 C69 C68 120.0 C70 C69 H69 120.0 C68 C69 H69 120.0 C69 C70 N14 120.0 C69 C70 C71 124.6(19) N14 C70 C71 115.3(19) C70 N14 C67 120.0 C70 C71 H71A 109.5 C70 C71 H71B 109.5 H71A C71 H71B 109.5 C70 C71 H71C 109.5 H71A C71 H71C 109.5 H71B C71 H71C 109.5 C68 C72 H72A 109.5 C68 C72 H72B 109.5 H72A C72 H72B 109.5 C68 C72 H72C 109.5 H72A C72 H72C 109.5 H72B C72 H72C 109.5 C74 C73 Sn4 121.7(17) C74 C73 H73A 106.9 Sn4 C73 H73A 106.9 C74 C73 H73B 106.9 Sn4 C73 H73B 106.9 H73A C73 H73B 106.7 C73 C74 C75 117(2) C73 C74 H74A 108.0 C75 C74 H74A 108.0 C73 C74 H74B 108.0 C75 C74 H74B 108.0 H74A C74 H74B 107.3 C76B C75 C74 107.0(17) C76A C75 C74 106.4(16) C76A C75 H75A 110.4 C74 C75 H75A 110.4 C76A C75 H75B 110.4 C74 C75 H75B 110.4 H75A C75 H75B 108.6 C78A C77 Sn4 113.2(18) C78B C77 Sn4 118(2) C78A C77 H77A 108.9 Sn4 C77 H77A 108.9 C78A C77 H77B 108.9 Sn4 C77 H77B 108.9 H77A C77 H77B 107.8 C80 C79 C78A 123(3) C80 C79 C78B 103(3) C80 C79 H79A 106.6 C78A C79 H79A 106.6 C80 C79 H79B 106.6 C78A C79 H79B 106.6 H79A C79 H79B 106.5 C79 C80 H80A 109.5 C79 C80 H80B 109.5 H80A C80 H80B 109.5 C79 C80 H80C 109.5 H80A C80 H80C 109.5 H80B C80 H80C 109.5 C7 Se1 Sn1 88.4(7) C1 Se2 Sn1 88.3(6) C21 Se3 Sn2 89.8(6) C27 Se4 Sn2 94.3(7) C41 Se5 Sn3 89.6(6) C47 Se6 Sn3 88.7(8) C13 Sn1 C17 126.9(11) C13 Sn1 Se2 110.3(8) C17 Sn1 Se2 106.7(7) C13 Sn1 Se1 105.5(9) C17 Sn1 Se1 110.4(5) Se2 Sn1 Se1 91.43(12) C13 Sn1 N3 81.3(8) C17 Sn1 N3 83.2(7) Se2 Sn1 N3 152.4(4) Se1 Sn1 N3 61.1(4) C13 Sn1 N1 84.6(9) C17 Sn1 N1 80.8(6) Se2 Sn1 N1 61.6(4) Se1 Sn1 N1 153.0(4) N3 Sn1 N1 145.9(6) C37 Sn2 C33 126.0(10) C37 Sn2 Se3 111.5(6) C33 Sn2 Se3 109.2(9) C37 Sn2 Se4 109.3(7) C33 Sn2 Se4 104.8(10) Se3 Sn2 Se4 89.68(12) C37 Sn2 N5 84.6(8) C33 Sn2 N5 85.3(11) Se3 Sn2 N5 61.2(4) Se4 Sn2 N5 150.8(4) C37 Sn2 N7 81.6(7) C33 Sn2 N7 81.9(10) Se3 Sn2 N7 148.3(4) Se4 Sn2 N7 58.6(4) N5 Sn2 N7 150.5(5) C53 Sn3 C57 125.5(11) C53 Sn3 Se6 109.9(8) C57 Sn3 Se6 108.7(7) C53 Sn3 Se5 108.2(9) C57 Sn3 Se5 106.9(6) Se6 Sn3 Se5 92.43(13) C53 Sn3 N9 81.1(10) C57 Sn3 N9 84.9(7) Se6 Sn3 N9 61.8(5) Se5 Sn3 N9 154.2(5) C53 Sn3 N11 81.3(9) C57 Sn3 N11 80.8(7) Se6 Sn3 N11 153.5(4) Se5 Sn3 N11 61.1(4) N9 Sn3 N11 144.7(6) C61 Se7 Sn4 92.9(6) C67 Se8 Sn4 91.6(7) C73 Sn4 C77 125.6(11) C73 Sn4 Se7 107.5(9) C77 Sn4 Se7 111.3(8) C73 Sn4 Se8 108.1(8) C77 Sn4 Se8 108.3(7) Se7 Sn4 Se8 90.26(12) C73 Sn4 N13 80.9(10) C77 Sn4 N13 84.0(8) Se7 Sn4 N13 149.9(4) Se8 Sn4 N13 59.9(4) C73 Sn4 N15 86.8(9) C77 Sn4 N15 81.6(8) Se7 Sn4 N15 59.6(3) Se8 Sn4 N15 149.6(3) N13 Sn4 N15 150.5(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C14A C13 1.540(14) C14A C15 1.543(14) C14A H14A 0.9700 C14A H14B 0.9700 C54A C55 1.528(14) C54A C53 1.538(14) C54A H54A 0.9700 C54A H54B 0.9700 C59A C60 1.531(14) C59A C58 1.540(14) C59A H59A 0.9700 C59A H59B 0.9700 C76A C75 1.527(12) C76A H76A 0.9600 C76A H76B 0.9600 C76A H76C 0.9600 C78A C77 1.536(14) C78A C79 1.538(14) C78A H78A 0.9700 C78A H78B 0.9700 C14B C15 1.543(14) C14B C13 1.545(14) C14B H14C 0.9700 C14B H14D 0.9700 C54B C53 1.535(14) C54B C55 1.542(14) C54B H54C 0.9700 C54B H54D 0.9700 C59B C60 1.530(14) C59B C58 1.540(14) C59B H59C 0.9700 C59B H59D 0.9700 C76B C75 1.526(15) C76B H76D 0.9600 C76B H76E 0.9600 C76B H76F 0.9600 C78B C77 1.538(14) C78B C79 1.538(14) C78B H78C 0.9700 C78B H78D 0.9700 C1 N1 1.3900 C1 N2 1.3900 C1 Se2 1.806(11) N1 C2 1.3900 N1 Sn1 2.747(13) C2 C3 1.3900 C2 C5 1.53(3) C3 C4 1.3900 C3 H3 0.9300 C4 N2 1.3900 C4 C6 1.46(3) C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 C6 H6A 0.9600 C6 H6B 0.9600 C6 H6C 0.9600 C7 N4 1.3900 C7 N3 1.3900 C7 Se1 1.769(14) N4 C8 1.3900 C8 C9 1.3900 C8 C11 1.48(2) C9 C10 1.3900 C9 H9 0.9300 C10 N3 1.3900 C10 C12 1.49(3) N3 Sn1 2.722(16) C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C13 Sn1 2.09(3) C13 H13A 0.9700 C13 H13B 0.9700 C15 C16 1.508(19) C15 H15A 0.9700 C15 H15B 0.9700 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 C18 1.511(17) C17 Sn1 2.18(2) C17 H17A 0.9700 C17 H17B 0.9700 C18 C19 1.520(17) C18 H18A 0.9700 C18 H18B 0.9700 C19 C20 1.519(17) C19 H19A 0.9700 C19 H19B 0.9700 C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C21 N5 1.3900 C21 N6 1.3900 C21 Se3 1.801(13) N5 C22 1.3900 N5 Sn2 2.844(16) C22 C23 1.3900 C22 C25 1.50(3) C23 C24 1.3900 C23 H23 0.9300 C24 N6 1.3900 C24 C26 1.47(3) C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 C27 N8 1.3900 C27 N7 1.3900 C27 Se4 1.800(14) N8 C28 1.3900 C28 C29 1.3900 C28 C31 1.47(2) C29 C30 1.3900 C29 H29 0.9300 C30 N7 1.3900 C30 C32 1.48(3) N7 Sn2 3.042(18) C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 C34 1.511(18) C33 Sn2 2.25(3) C33 H33A 0.9700 C33 H33B 0.9700 C34 C35 1.526(18) C34 H34A 0.9700 C34 H34B 0.9700 C35 C36 1.479(19) C35 H35A 0.9700 C35 H35B 0.9700 C36 H36A 0.9600 C36 H36B 0.9600 C36 H36C 0.9600 C37 C38 1.516(17) C37 Sn2 2.15(2) C37 H37A 0.9700 C37 H37B 0.9700 C38 C39 1.519(18) C38 H38A 0.9700 C38 H38B 0.9700 C39 C40 1.515(18) C39 H39A 0.9700 C39 H39B 0.9700 C40 H40A 0.9600 C40 H40B 0.9600 C40 H40C 0.9600 C41 N12 1.3900 C41 N11 1.3900 C41 Se5 1.815(14) N12 C42 1.3900 C42 C43 1.3900 C42 C45 1.43(3) C43 C44 1.3900 C43 H43 0.9300 C44 N11 1.3900 C44 C46 1.53(3) N11 Sn3 2.778(16) C45 H45A 0.9600 C45 H45B 0.9600 C45 H45C 0.9600 C46 H46A 0.9600 C46 H46B 0.9600 C46 H46C 0.9600 C47 N9 1.3900 C47 N10 1.3900 C47 Se6 1.832(14) N9 C48 1.3900 N9 Sn3 2.732(17) C48 C49 1.3900 C48 C51 1.49(3) C49 C50 1.3900 C49 H49 0.9300 C50 N10 1.3900 C50 C52 1.48(3) C51 H51A 0.9600 C51 H51B 0.9600 C51 H51C 0.9600 C52 H52A 0.9600 C52 H52B 0.9600 C52 H52C 0.9600 C53 Sn3 2.12(3) C53 H53A 0.9700 C53 H53B 0.9700 C55 C56 1.513(19) C55 H55A 0.9700 C55 H55B 0.9700 C56 H56A 0.9600 C56 H56B 0.9600 C56 H56C 0.9600 C57 C58 1.507(18) C57 Sn3 2.17(2) C57 H57A 0.9700 C57 H57B 0.9700 C58 H58A 0.9700 C58 H58B 0.9700 C60 H60A 0.9600 C60 H60B 0.9600 C60 H60C 0.9600 C61 N16 1.3900 C61 N15 1.3900 C61 Se7 1.812(13) N16 C62 1.3900 C62 C63 1.3900 C62 C66 1.48(3) C63 C64 1.3900 C63 H63 0.9300 C64 N15 1.3900 C64 C65 1.41(3) N15 Sn4 2.979(16) C65 H65A 0.9600 C65 H65B 0.9600 C65 H65C 0.9600 C66 H66A 0.9600 C66 H66B 0.9600 C66 H66C 0.9600 C67 N13 1.3900 C67 N14 1.3900 C67 Se8 1.764(13) N13 C68 1.3900 N13 Sn4 2.885(16) C68 C69 1.3900 C68 C72 1.43(3) C69 C70 1.3900 C69 H69 0.9300 C70 N14 1.3900 C70 C71 1.49(3) C71 H71A 0.9600 C71 H71B 0.9600 C71 H71C 0.9600 C72 H72A 0.9600 C72 H72B 0.9600 C72 H72C 0.9600 C73 C74 1.502(17) C73 Sn4 2.05(2) C73 H73A 0.9700 C73 H73B 0.9700 C74 C75 1.534(18) C74 H74A 0.9700 C74 H74B 0.9700 C75 H75A 0.9700 C75 H75B 0.9700 C77 Sn4 2.12(2) C77 H77A 0.9700 C77 H77B 0.9700 C79 C80 1.512(19) C79 H79A 0.9700 C79 H79B 0.9700 C80 H80A 0.9600 C80 H80B 0.9600 C80 H80C 0.9600 Se1 Sn1 2.609(4) Se2 Sn1 2.601(4) Se3 Sn2 2.581(4) Se4 Sn2 2.583(4) Se5 Sn3 2.599(4) Se6 Sn3 2.595(4) Se7 Sn4 2.575(4) Se8 Sn4 2.582(4) 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 N2 C1 N1 C2 0.0 Se2 C1 N1 C2 -177.6(10) N2 C1 N1 Sn1 -176.7(7) Se2 C1 N1 Sn1 5.7(6) C1 N1 C2 C3 0.0 Sn1 N1 C2 C3 173.7(14) C1 N1 C2 C5 -176.7(15) Sn1 N1 C2 C5 -3.0(19) N1 C2 C3 C4 0.0 C5 C2 C3 C4 176.4(17) C2 C3 C4 N2 0.0 C2 C3 C4 C6 -175(2) C3 C4 N2 C1 0.0 C6 C4 N2 C1 175.4(17) N1 C1 N2 C4 0.0 Se2 C1 N2 C4 177.5(11) N3 C7 N4 C8 0.0 Se1 C7 N4 C8 178.5(12) C7 N4 C8 C9 0.0 C7 N4 C8 C11 -179.6(16) N4 C8 C9 C10 0.0 C11 C8 C9 C10 179.5(17) C8 C9 C10 N3 0.0 C8 C9 C10 C12 178.3(17) C9 C10 N3 C7 0.0 C12 C10 N3 C7 -178.4(17) C9 C10 N3 Sn1 175.3(14) C12 C10 N3 Sn1 -3(2) N4 C7 N3 C10 0.0 Se1 C7 N3 C10 -178.6(11) N4 C7 N3 Sn1 -177.4(8) Se1 C7 N3 Sn1 4.0(7) C15 C14A C13 Sn1 -137(4) C15 C14B C13 Sn1 144(4) C13 C14B C15 C16 171(5) C13 C14A C15 C16 100(9) Sn1 C17 C18 C19 -177.8(18) C17 C18 C19 C20 -179(2) N6 C21 N5 C22 0.0 Se3 C21 N5 C22 -178.8(11) N6 C21 N5 Sn2 175.9(7) Se3 C21 N5 Sn2 -3.0(7) C21 N5 C22 C23 0.0 Sn2 N5 C22 C23 -171.5(15) C21 N5 C22 C25 -172(2) Sn2 N5 C22 C25 16(2) N5 C22 C23 C24 0.0 C25 C22 C23 C24 172(2) C22 C23 C24 N6 0.0 C22 C23 C24 C26 -175(2) C23 C24 N6 C21 0.0 C26 C24 N6 C21 175.7(18) N5 C21 N6 C24 0.0 Se3 C21 N6 C24 178.8(11) N7 C27 N8 C28 0.0 Se4 C27 N8 C28 -178.3(11) C27 N8 C28 C29 0.0 C27 N8 C28 C31 -177.7(16) N8 C28 C29 C30 0.0 C31 C28 C29 C30 177.4(18) C28 C29 C30 N7 0.0 C28 C29 C30 C32 177(2) C29 C30 N7 C27 0.0 C32 C30 N7 C27 -177.2(19) C29 C30 N7 Sn2 172.9(17) C32 C30 N7 Sn2 -4(2) N8 C27 N7 C30 0.0 Se4 C27 N7 C30 178.3(11) N8 C27 N7 Sn2 -176.9(7) Se4 C27 N7 Sn2 1.4(7) Sn2 C33 C34 C35 164(2) C33 C34 C35 C36 65(5) Sn2 C37 C38 C39 -177(2) C37 C38 C39 C40 -173(3) N11 C41 N12 C42 0.0 Se5 C41 N12 C42 -174.2(12) C41 N12 C42 C43 0.0 C41 N12 C42 C45 -178(2) N12 C42 C43 C44 0.0 C45 C42 C43 C44 177(2) C42 C43 C44 N11 0.0 C42 C43 C44 C46 -177.3(19) C43 C44 N11 C41 0.0 C46 C44 N11 C41 177.6(17) C43 C44 N11 Sn3 177.7(14) C46 C44 N11 Sn3 -5(2) N12 C41 N11 C44 0.0 Se5 C41 N11 C44 174.5(11) N12 C41 N11 Sn3 -178.8(8) Se5 C41 N11 Sn3 -4.3(7) N10 C47 N9 C48 0.0 Se6 C47 N9 C48 179.7(10) N10 C47 N9 Sn3 175.9(8) Se6 C47 N9 Sn3 -4.4(6) C47 N9 C48 C49 0.0 Sn3 N9 C48 C49 -172.6(14) C47 N9 C48 C51 -178.6(17) Sn3 N9 C48 C51 9(2) N9 C48 C49 C50 0.0 C51 C48 C49 C50 178.5(19) C48 C49 C50 N10 0.0 C48 C49 C50 C52 173(2) C49 C50 N10 C47 0.0 C52 C50 N10 C47 -173.5(19) N9 C47 N10 C50 0.0 Se6 C47 N10 C50 -179.7(11) C55 C54B C53 Sn3 125(3) C55 C54A C53 Sn3 -102(3) C53 C54A C55 C56 -94(4) C53 C54B C55 C56 98(4) Sn3 C57 C58 C59B 176(5) Sn3 C57 C58 C59A -162(4) C60 C59B C58 C57 -171(5) C60 C59A C58 C57 -150(4) N15 C61 N16 C62 0.0 Se7 C61 N16 C62 178.8(11) C61 N16 C62 C63 0.0 C61 N16 C62 C66 176.9(18) N16 C62 C63 C64 0.0 C66 C62 C63 C64 -177(2) C62 C63 C64 N15 0.0 C62 C63 C64 C65 174.0(19) C63 C64 N15 C61 0.0 C65 C64 N15 C61 -174.6(18) C63 C64 N15 Sn4 -170.2(16) C65 C64 N15 Sn4 15(2) N16 C61 N15 C64 0.0 Se7 C61 N15 C64 -178.8(11) N16 C61 N15 Sn4 175.5(7) Se7 C61 N15 Sn4 -3.4(6) N14 C67 N13 C68 0.0 Se8 C67 N13 C68 178.2(11) N14 C67 N13 Sn4 179.3(7) Se8 C67 N13 Sn4 -2.5(7) C67 N13 C68 C69 0.0 Sn4 N13 C68 C69 -178.5(16) C67 N13 C68 C72 179(2) Sn4 N13 C68 C72 0(2) N13 C68 C69 C70 0.0 C72 C68 C69 C70 -179(2) C68 C69 C70 N14 0.0 C68 C69 C70 C71 176.4(19) C69 C70 N14 C67 0.0 C71 C70 N14 C67 -176.7(17) N13 C67 N14 C70 0.0 Se8 C67 N14 C70 -178.2(11) Sn4 C73 C74 C75 168(2) C73 C74 C75 C76B 71(6) C73 C74 C75 C76A 178(3) C79 C78A C77 Sn4 -167(3) C79 C78B C77 Sn4 156(4) C77 C78A C79 C80 131(4) C77 C78B C79 C80 172(5) N4 C7 Se1 Sn1 177.3(8) N3 C7 Se1 Sn1 -4.1(7) N1 C1 Se2 Sn1 -6.0(7) N2 C1 Se2 Sn1 176.4(7) N5 C21 Se3 Sn2 3.3(8) N6 C21 Se3 Sn2 -175.6(7) N8 C27 Se4 Sn2 176.6(7) N7 C27 Se4 Sn2 -1.7(8) N12 C41 Se5 Sn3 178.9(8) N11 C41 Se5 Sn3 4.6(7) N9 C47 Se6 Sn3 4.7(7) N10 C47 Se6 Sn3 -175.7(8) N16 C61 Se7 Sn4 -175.0(7) N15 C61 Se7 Sn4 3.9(7) N13 C67 Se8 Sn4 2.8(8) N14 C67 Se8 Sn4 -179.0(7)