# Supplementary Material (ESI) for Polymer Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1478 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Qiwei Wang' 'Wai-Yeung Wong' _publ_contact_author_name 'Qi-Wei Wang' _publ_contact_author_email w_qiwei@yahoo.com.cn _publ_section_title ; New low-bandgap polymetallaynes of platinum functionalized with triphenylamine-benzothiadiazole donor-acceptor unit for solar cell applications ; # Attachment 'wy2040wm.cif' data_wy2040wm _database_code_depnum_ccdc_archive 'CCDC 801106' #TrackingRef 'wy2040wm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H38 N4 S3' _chemical_formula_sum 'C52 H38 N4 S3' _chemical_formula_weight 815.04 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2608(7) _cell_length_b 17.8234(11) _cell_length_c 20.1891(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.7050(10) _cell_angle_gamma 90.00 _cell_volume 4005.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24702 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6857 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24702 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9673 _reflns_number_gt 6788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+2.2200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9673 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.4784(3) 0.1928(2) 0.15588(15) 0.0491(7) Uani 1 1 d . . . H1A H 1.4533 0.1658 0.1157 0.059 Uiso 1 1 calc R . . C2 C 1.5993(3) 0.2115(2) 0.17508(17) 0.0556(9) Uani 1 1 d . . . H2A H 1.6567 0.1970 0.1475 0.067 Uiso 1 1 calc R . . C3 C 1.6368(3) 0.25087(19) 0.23384(16) 0.0464(7) Uani 1 1 d . . . H3A H 1.7193 0.2627 0.2467 0.056 Uiso 1 1 calc R . . C4 C 1.5547(3) 0.27228(17) 0.27279(16) 0.0448(7) Uani 1 1 d . . . H4A H 1.5801 0.3002 0.3125 0.054 Uiso 1 1 calc R . . C5 C 1.4336(2) 0.25392(16) 0.25548(15) 0.0403(6) Uani 1 1 d . . . H5A H 1.3773 0.2683 0.2837 0.048 Uiso 1 1 calc R . . C6 C 1.3957(2) 0.21451(16) 0.19661(14) 0.0377(6) Uani 1 1 d . . . C7 C 1.2382(2) 0.12018(16) 0.16397(14) 0.0386(6) Uani 1 1 d . . . C8 C 1.1472(3) 0.10026(17) 0.11266(15) 0.0424(6) Uani 1 1 d . . . H8A H 1.1075 0.1380 0.0843 0.051 Uiso 1 1 calc R . . C9 C 1.1139(3) 0.02646(18) 0.10253(16) 0.0476(7) Uani 1 1 d . . . H9A H 1.0507 0.0139 0.0676 0.057 Uiso 1 1 calc R . . C10 C 1.1728(3) -0.03132(17) 0.14365(17) 0.0497(8) Uani 1 1 d . . . C11 C 1.2665(3) -0.01029(19) 0.19149(16) 0.0516(8) Uani 1 1 d . . . H11A H 1.3103 -0.0480 0.2180 0.062 Uiso 1 1 calc R . . C12 C 1.2993(3) 0.06330(17) 0.20248(15) 0.0462(7) Uani 1 1 d . . . H12A H 1.3642 0.0756 0.2366 0.055 Uiso 1 1 calc R . . C13 C 1.1339(4) -0.11121(19) 0.1366(2) 0.0650(10) Uani 1 1 d . . . H13A H 1.1855 -0.1419 0.1694 0.098 Uiso 1 1 calc R . . H13B H 1.1402 -0.1288 0.0912 0.098 Uiso 1 1 calc R . . H13C H 1.0504 -0.1154 0.1444 0.098 Uiso 1 1 calc R . . C14 C 1.1836(2) 0.25327(16) 0.17675(13) 0.0350(6) Uani 1 1 d . . . C15 C 1.2130(2) 0.32802(16) 0.16767(13) 0.0351(6) Uani 1 1 d . . . H15A H 1.2938 0.3409 0.1644 0.042 Uiso 1 1 calc R . . C16 C 1.1275(2) 0.38377(16) 0.16329(13) 0.0343(6) Uani 1 1 d . . . H16A H 1.1504 0.4342 0.1568 0.041 Uiso 1 1 calc R . . C17 C 1.0070(2) 0.36762(15) 0.16817(12) 0.0329(5) Uani 1 1 d . . . C18 C 0.9794(2) 0.29293(16) 0.17948(13) 0.0355(6) Uani 1 1 d . . . H18A H 0.8991 0.2802 0.1840 0.043 Uiso 1 1 calc R . . C19 C 1.0644(2) 0.23680(15) 0.18440(14) 0.0370(6) Uani 1 1 d . . . H19A H 1.0424 0.1867 0.1930 0.044 Uiso 1 1 calc R . . C20 C 0.9152(2) 0.42644(15) 0.15769(13) 0.0337(6) Uani 1 1 d . . . C21 C 0.9293(2) 0.50303(16) 0.15690(14) 0.0382(6) Uani 1 1 d . . . H21A H 1.0045 0.5281 0.1656 0.046 Uiso 1 1 calc R . . C22 C 0.8154(2) 0.53998(16) 0.14122(13) 0.0368(6) Uani 1 1 d . . . H22A H 0.8074 0.5930 0.1397 0.044 Uiso 1 1 calc R . . C23 C 0.7249(2) 0.49532(14) 0.12940(12) 0.0315(5) Uani 1 1 d . . . C24 C 0.5941(2) 0.51736(14) 0.11374(13) 0.0300(5) Uani 1 1 d . . . C25 C 0.5555(2) 0.58896(14) 0.12801(13) 0.0332(5) Uani 1 1 d . . . H25A H 0.6132 0.6239 0.1486 0.040 Uiso 1 1 calc R . . C26 C 0.4349(2) 0.61179(14) 0.11329(13) 0.0310(5) Uani 1 1 d . . . H26A H 0.4151 0.6614 0.1250 0.037 Uiso 1 1 calc R . . C27 C 0.3436(2) 0.56623(13) 0.08278(12) 0.0273(5) Uani 1 1 d . . . C28 C 0.3792(2) 0.49144(14) 0.06794(11) 0.0274(5) Uani 1 1 d . . . C29 C 0.5032(2) 0.46856(14) 0.08397(12) 0.0283(5) Uani 1 1 d . . . C30 C 0.2156(2) 0.59196(13) 0.06539(11) 0.0274(5) Uani 1 1 d . . . C31 C 0.1310(2) 0.56684(15) 0.01841(13) 0.0357(6) Uani 1 1 d . . . H31A H 0.1412 0.5250 -0.0094 0.043 Uiso 1 1 calc R . . C32 C 0.0233(2) 0.60880(15) 0.01369(13) 0.0344(6) Uani 1 1 d . . . H32A H -0.0462 0.5982 -0.0178 0.041 Uiso 1 1 calc R . . C33 C 0.0297(2) 0.66618(14) 0.05915(12) 0.0273(5) Uani 1 1 d . . . C34 C -0.06365(19) 0.72009(13) 0.07031(12) 0.0253(5) Uani 1 1 d . . . C35 C -0.0747(2) 0.74592(14) 0.13439(12) 0.0293(5) Uani 1 1 d . . . H35A H -0.0195 0.7290 0.1717 0.035 Uiso 1 1 calc R . . C36 C -0.1644(2) 0.79561(15) 0.14451(12) 0.0303(5) Uani 1 1 d . . . H36A H -0.1704 0.8124 0.1885 0.036 Uiso 1 1 calc R . . C37 C -0.2465(2) 0.82129(14) 0.09037(12) 0.0286(5) Uani 1 1 d . . . C38 C -0.2355(2) 0.79674(15) 0.02607(12) 0.0320(5) Uani 1 1 d . . . H38A H -0.2897 0.8145 -0.0113 0.038 Uiso 1 1 calc R . . C39 C -0.1456(2) 0.74649(14) 0.01648(12) 0.0299(5) Uani 1 1 d . . . H39A H -0.1396 0.7297 -0.0276 0.036 Uiso 1 1 calc R . . C40 C -0.4570(2) 0.86249(14) 0.06627(12) 0.0296(5) Uani 1 1 d . . . C41 C -0.5017(2) 0.79141(15) 0.04941(13) 0.0329(5) Uani 1 1 d . . . H41A H -0.4528 0.7488 0.0618 0.040 Uiso 1 1 calc R . . C42 C -0.6163(2) 0.78164(17) 0.01479(13) 0.0376(6) Uani 1 1 d . . . H42A H -0.6438 0.7323 0.0029 0.045 Uiso 1 1 calc R . . C43 C -0.6922(2) 0.84188(18) -0.00300(14) 0.0415(7) Uani 1 1 d . . . C44 C -0.6479(3) 0.91296(18) 0.01473(15) 0.0443(7) Uani 1 1 d . . . H44A H -0.6981 0.9553 0.0034 0.053 Uiso 1 1 calc R . . C45 C -0.5321(2) 0.92398(16) 0.04866(14) 0.0389(6) Uani 1 1 d . . . H45A H -0.5041 0.9733 0.0598 0.047 Uiso 1 1 calc R . . C46 C -0.8183(3) 0.8299(2) -0.03994(17) 0.0598(9) Uani 1 1 d . . . H46A H -0.8586 0.8785 -0.0482 0.090 Uiso 1 1 calc R . . H46B H -0.8637 0.7985 -0.0127 0.090 Uiso 1 1 calc R . . H46C H -0.8143 0.8050 -0.0828 0.090 Uiso 1 1 calc R . . C47 C -0.3097(2) 0.93254(14) 0.14636(13) 0.0343(6) Uani 1 1 d . . . C48 C -0.3868(3) 0.95331(19) 0.19097(15) 0.0477(7) Uani 1 1 d . . . H48A H -0.4607 0.9276 0.1909 0.057 Uiso 1 1 calc R . . C49 C -0.3550(4) 1.0117(2) 0.23548(17) 0.0666(11) Uani 1 1 d . . . H49A H -0.4078 1.0260 0.2658 0.080 Uiso 1 1 calc R . . C50 C -0.2486(4) 1.0488(2) 0.23629(19) 0.0702(12) Uani 1 1 d . . . H50A H -0.2282 1.0890 0.2667 0.084 Uiso 1 1 calc R . . C51 C -0.1713(3) 1.02811(18) 0.19332(18) 0.0561(9) Uani 1 1 d . . . H51A H -0.0965 1.0532 0.1949 0.067 Uiso 1 1 calc R . . C52 C -0.2014(3) 0.97074(16) 0.14748(15) 0.0437(7) Uani 1 1 d . . . H52A H -0.1485 0.9575 0.1169 0.052 Uiso 1 1 calc R . . N1 N 1.2710(2) 0.19663(13) 0.17748(12) 0.0418(6) Uani 1 1 d . . . N2 N 0.51930(19) 0.39589(12) 0.06680(11) 0.0351(5) Uani 1 1 d . . . N3 N 0.30563(19) 0.43668(12) 0.03997(11) 0.0341(5) Uani 1 1 d . . . N4 N -0.33880(18) 0.87222(12) 0.10127(11) 0.0336(5) Uani 1 1 d . . . S1 S 0.76502(5) 0.40224(4) 0.13635(4) 0.03507(17) Uani 1 1 d . . . S2 S 0.38953(6) 0.36415(4) 0.03493(4) 0.04035(18) Uani 1 1 d . . . S3 S 0.17054(5) 0.66931(4) 0.10704(3) 0.02999(15) 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 C1 0.0472(16) 0.061(2) 0.0392(15) 0.0001(14) 0.0070(13) 0.0170(15) C2 0.0392(16) 0.075(2) 0.056(2) 0.0082(17) 0.0193(14) 0.0125(16) C3 0.0331(14) 0.0573(18) 0.0484(17) 0.0167(15) 0.0049(12) 0.0006(13) C4 0.0388(15) 0.0438(16) 0.0500(17) 0.0045(13) 0.0012(13) 0.0003(13) C5 0.0345(13) 0.0440(16) 0.0427(15) 0.0013(13) 0.0072(11) 0.0059(12) C6 0.0321(13) 0.0377(14) 0.0425(15) 0.0031(12) 0.0034(11) 0.0081(11) C7 0.0400(14) 0.0368(14) 0.0394(14) -0.0015(12) 0.0077(11) 0.0091(11) C8 0.0403(14) 0.0431(16) 0.0435(16) -0.0013(13) 0.0051(12) 0.0048(13) C9 0.0454(16) 0.0482(17) 0.0499(17) -0.0044(14) 0.0093(13) 0.0004(14) C10 0.0535(18) 0.0374(15) 0.064(2) -0.0042(14) 0.0268(16) 0.0012(14) C11 0.063(2) 0.0440(17) 0.0491(18) 0.0052(14) 0.0116(15) 0.0131(15) C12 0.0512(17) 0.0409(16) 0.0450(16) -0.0006(13) 0.0026(13) 0.0101(13) C13 0.070(2) 0.0414(18) 0.087(3) -0.0036(18) 0.023(2) -0.0112(17) C14 0.0333(13) 0.0415(15) 0.0288(12) -0.0036(11) 0.0004(10) 0.0094(11) C15 0.0309(12) 0.0434(15) 0.0314(13) -0.0004(11) 0.0056(10) 0.0049(11) C16 0.0326(12) 0.0377(14) 0.0325(13) 0.0004(11) 0.0043(10) 0.0036(11) C17 0.0303(12) 0.0381(14) 0.0295(12) 0.0010(11) 0.0020(10) 0.0086(11) C18 0.0290(12) 0.0410(14) 0.0366(14) -0.0002(12) 0.0051(10) 0.0051(11) C19 0.0362(13) 0.0321(13) 0.0424(15) 0.0001(11) 0.0048(11) 0.0047(11) C20 0.0283(12) 0.0394(14) 0.0336(13) -0.0004(11) 0.0054(10) 0.0061(11) C21 0.0306(13) 0.0373(14) 0.0461(15) 0.0004(12) 0.0033(11) 0.0024(11) C22 0.0362(13) 0.0351(14) 0.0390(14) 0.0009(11) 0.0059(11) 0.0175(11) C23 0.0447(14) 0.0244(11) 0.0277(12) 0.0041(10) 0.0131(10) 0.0088(10) C24 0.0258(11) 0.0311(12) 0.0345(13) 0.0047(10) 0.0090(10) 0.0051(10) C25 0.0290(12) 0.0282(12) 0.0426(14) 0.0028(11) 0.0060(10) 0.0013(10) C26 0.0305(12) 0.0248(11) 0.0386(13) 0.0038(10) 0.0081(10) 0.0057(9) C27 0.0285(11) 0.0286(12) 0.0264(11) 0.0041(9) 0.0094(9) 0.0056(9) C28 0.0285(11) 0.0300(12) 0.0255(11) 0.0010(10) 0.0097(9) 0.0045(9) C29 0.0301(11) 0.0283(12) 0.0287(12) 0.0024(10) 0.0117(9) 0.0063(9) C30 0.0418(13) 0.0209(10) 0.0224(11) 0.0032(9) 0.0144(10) 0.0081(10) C31 0.0375(13) 0.0361(14) 0.0353(14) -0.0051(11) 0.0111(11) 0.0087(11) C32 0.0298(12) 0.0405(14) 0.0324(13) -0.0077(11) 0.0028(10) 0.0052(11) C33 0.0254(10) 0.0306(12) 0.0264(11) 0.0008(10) 0.0056(9) 0.0029(9) C34 0.0221(10) 0.0261(11) 0.0285(11) -0.0017(9) 0.0066(9) 0.0017(9) C35 0.0285(11) 0.0331(12) 0.0257(12) 0.0001(10) 0.0021(9) 0.0023(10) C36 0.0296(12) 0.0374(13) 0.0249(11) -0.0044(10) 0.0073(9) 0.0024(10) C37 0.0230(10) 0.0292(12) 0.0342(13) -0.0035(10) 0.0065(9) 0.0011(9) C38 0.0284(12) 0.0387(14) 0.0281(12) -0.0004(11) 0.0018(9) 0.0063(10) C39 0.0283(11) 0.0367(13) 0.0247(11) -0.0035(10) 0.0034(9) 0.0040(10) C40 0.0267(11) 0.0336(13) 0.0296(12) -0.0013(10) 0.0078(9) 0.0030(10) C41 0.0331(12) 0.0323(13) 0.0346(13) -0.0016(11) 0.0091(10) 0.0031(10) C42 0.0329(13) 0.0446(15) 0.0363(14) -0.0016(12) 0.0085(11) -0.0048(12) C43 0.0301(13) 0.0602(19) 0.0346(14) 0.0037(13) 0.0063(11) 0.0000(13) C44 0.0351(14) 0.0490(17) 0.0478(16) 0.0087(14) 0.0031(12) 0.0121(13) C45 0.0372(14) 0.0341(14) 0.0455(16) 0.0032(12) 0.0064(12) 0.0046(11) C46 0.0343(15) 0.092(3) 0.0503(18) 0.0026(19) -0.0022(13) -0.0008(17) C47 0.0385(13) 0.0303(13) 0.0329(13) -0.0020(11) 0.0022(11) 0.0089(11) C48 0.0428(15) 0.0547(18) 0.0457(16) -0.0096(14) 0.0069(13) 0.0181(14) C49 0.072(2) 0.074(2) 0.0487(19) -0.0271(18) -0.0060(17) 0.040(2) C50 0.092(3) 0.0419(18) 0.065(2) -0.0250(17) -0.026(2) 0.0234(19) C51 0.065(2) 0.0356(16) 0.060(2) -0.0062(15) -0.0141(17) -0.0036(15) C52 0.0460(15) 0.0359(15) 0.0477(17) -0.0030(13) 0.0025(13) -0.0022(12) N1 0.0332(11) 0.0374(13) 0.0527(14) -0.0077(11) 0.0000(10) 0.0078(10) N2 0.0333(11) 0.0335(11) 0.0396(12) -0.0038(10) 0.0093(9) 0.0070(9) N3 0.0319(11) 0.0333(11) 0.0377(12) -0.0057(9) 0.0078(9) 0.0049(9) N4 0.0277(10) 0.0335(11) 0.0393(12) -0.0091(9) 0.0048(9) 0.0048(9) S1 0.0278(3) 0.0301(3) 0.0474(4) 0.0027(3) 0.0061(3) 0.0050(2) S2 0.0346(3) 0.0341(3) 0.0528(4) -0.0125(3) 0.0079(3) 0.0044(3) S3 0.0264(3) 0.0301(3) 0.0329(3) -0.0044(2) 0.0026(2) 0.0053(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.387(4) . ? C1 C2 1.398(4) . ? C1 H1A 0.9500 . ? C2 C3 1.388(5) . ? C2 H2A 0.9500 . ? C3 C4 1.356(4) . ? C3 H3A 0.9500 . ? C4 C5 1.394(4) . ? C4 H4A 0.9500 . ? C5 C6 1.391(4) . ? C5 H5A 0.9500 . ? C6 N1 1.434(3) . ? C7 C8 1.389(4) . ? C7 C12 1.394(4) . ? C7 N1 1.427(4) . ? C8 C9 1.374(4) . ? C8 H8A 0.9500 . ? C9 C10 1.422(5) . ? C9 H9A 0.9500 . ? C10 C11 1.371(5) . ? C10 C13 1.490(4) . ? C11 C12 1.372(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.391(4) . ? C14 C19 1.405(4) . ? C14 N1 1.409(3) . ? C15 C16 1.377(4) . ? C15 H15A 0.9500 . ? C16 C17 1.405(4) . ? C16 H16A 0.9500 . ? C17 C18 1.394(4) . ? C17 C20 1.465(3) . ? C18 C19 1.378(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.375(4) . ? C20 S1 1.735(3) . ? C21 C22 1.434(3) . ? C21 H21A 0.9500 . ? C22 C23 1.287(4) . ? C22 H22A 0.9500 . ? C23 C24 1.511(3) . ? C23 S1 1.719(2) . ? C24 C25 1.392(3) . ? C24 C29 1.407(4) . ? C25 C26 1.406(3) . ? C25 H25A 0.9500 . ? C26 C27 1.380(3) . ? C26 H26A 0.9500 . ? C27 C28 1.437(3) . ? C27 C30 1.503(3) . ? C28 N3 1.348(3) . ? C28 C29 1.443(3) . ? C29 N2 1.360(3) . ? C30 C31 1.317(4) . ? C30 S3 1.730(2) . ? C31 C32 1.416(3) . ? C31 H31A 0.9500 . ? C32 C33 1.369(3) . ? C32 H32A 0.9500 . ? C33 C34 1.467(3) . ? C33 S3 1.729(2) . ? C34 C39 1.396(3) . ? C34 C35 1.396(3) . ? C35 C36 1.382(3) . ? C35 H35A 0.9500 . ? C36 C37 1.397(3) . ? C36 H36A 0.9500 . ? C37 C38 1.393(3) . ? C37 N4 1.422(3) . ? C38 C39 1.387(3) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.386(4) . ? C40 C45 1.397(4) . ? C40 N4 1.420(3) . ? C41 C42 1.383(4) . ? C41 H41A 0.9500 . ? C42 C43 1.385(4) . ? C42 H42A 0.9500 . ? C43 C44 1.388(4) . ? C43 C46 1.516(4) . ? C44 C45 1.392(4) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.392(4) . ? C47 C52 1.393(4) . ? C47 N4 1.415(3) . ? C48 C49 1.386(5) . ? C48 H48A 0.9500 . ? C49 C50 1.367(6) . ? C49 H49A 0.9500 . ? C50 C51 1.369(6) . ? C50 H50A 0.9500 . ? C51 C52 1.387(4) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? N2 S2 1.608(2) . ? N3 S2 1.613(2) . ? 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 C6 C1 C2 118.8(3) . . ? C6 C1 H1A 120.6 . . ? C2 C1 H1A 120.6 . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C1 C6 C5 120.0(3) . . ? C1 C6 N1 119.7(3) . . ? C5 C6 N1 120.2(2) . . ? C8 C7 C12 118.5(3) . . ? C8 C7 N1 121.8(3) . . ? C12 C7 N1 119.7(3) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.9(3) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 117.0(3) . . ? C11 C10 C13 120.8(3) . . ? C9 C10 C13 122.1(3) . . ? C10 C11 C12 122.4(3) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.7(2) . . ? C15 C14 N1 120.5(2) . . ? C19 C14 N1 121.8(3) . . ? C16 C15 C14 121.4(2) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C17 121.4(3) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C18 C17 C16 116.7(2) . . ? C18 C17 C20 122.5(2) . . ? C16 C17 C20 120.7(2) . . ? C19 C18 C17 122.4(2) . . ? C19 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? C18 C19 C14 120.4(3) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? C21 C20 C17 129.2(2) . . ? C21 C20 S1 110.75(19) . . ? C17 C20 S1 119.9(2) . . ? C20 C21 C22 110.9(2) . . ? C20 C21 H21A 124.5 . . ? C22 C21 H21A 124.5 . . ? C23 C22 C21 114.4(3) . . ? C23 C22 H22A 122.8 . . ? C21 C22 H22A 122.8 . . ? C22 C23 C24 126.7(2) . . ? C22 C23 S1 113.0(2) . . ? C24 C23 S1 120.24(19) . . ? C25 C24 C29 115.1(2) . . ? C25 C24 C23 121.3(2) . . ? C29 C24 C23 123.5(2) . . ? C24 C25 C26 122.9(2) . . ? C24 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C27 C26 C25 123.7(2) . . ? C27 C26 H26A 118.2 . . ? C25 C26 H26A 118.2 . . ? C26 C27 C28 115.3(2) . . ? C26 C27 C30 123.2(2) . . ? C28 C27 C30 121.5(2) . . ? N3 C28 C27 125.9(2) . . ? N3 C28 C29 113.7(2) . . ? C27 C28 C29 120.4(2) . . ? N2 C29 C24 125.5(2) . . ? N2 C29 C28 111.9(2) . . ? C24 C29 C28 122.5(2) . . ? C31 C30 C27 128.9(2) . . ? C31 C30 S3 112.82(19) . . ? C27 C30 S3 118.09(18) . . ? C30 C31 C32 112.8(2) . . ? C30 C31 H31A 123.6 . . ? C32 C31 H31A 123.6 . . ? C33 C32 C31 113.1(2) . . ? C33 C32 H32A 123.5 . . ? C31 C32 H32A 123.5 . . ? C32 C33 C34 128.8(2) . . ? C32 C33 S3 110.48(18) . . ? C34 C33 S3 120.75(18) . . ? C39 C34 C35 118.0(2) . . ? C39 C34 C33 120.4(2) . . ? C35 C34 C33 121.6(2) . . ? C36 C35 C34 121.2(2) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C35 C36 C37 120.4(2) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 119.0(2) . . ? C38 C37 N4 121.0(2) . . ? C36 C37 N4 120.0(2) . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C38 C39 C34 121.3(2) . . ? C38 C39 H39A 119.4 . . ? C34 C39 H39A 119.4 . . ? C41 C40 C45 118.1(2) . . ? C41 C40 N4 120.8(2) . . ? C45 C40 N4 121.1(2) . . ? C42 C41 C40 121.0(2) . . ? C42 C41 H41A 119.5 . . ? C40 C41 H41A 119.5 . . ? C41 C42 C43 121.7(3) . . ? C41 C42 H42A 119.1 . . ? C43 C42 H42A 119.1 . . ? C42 C43 C44 117.2(3) . . ? C42 C43 C46 120.9(3) . . ? C44 C43 C46 121.9(3) . . ? C43 C44 C45 121.9(3) . . ? C43 C44 H44A 119.0 . . ? C45 C44 H44A 119.0 . . ? C44 C45 C40 120.0(3) . . ? C44 C45 H45A 120.0 . . ? C40 C45 H45A 120.0 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 119.3(3) . . ? C48 C47 N4 120.8(3) . . ? C52 C47 N4 119.9(2) . . ? C49 C48 C47 119.6(3) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C50 C49 C48 120.7(3) . . ? C50 C49 H49A 119.6 . . ? C48 C49 H49A 119.6 . . ? C49 C50 C51 120.2(3) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C50 C51 C52 120.4(3) . . ? C50 C51 H51A 119.8 . . ? C52 C51 H51A 119.8 . . ? C51 C52 C47 119.8(3) . . ? C51 C52 H52A 120.1 . . ? C47 C52 H52A 120.1 . . ? C14 N1 C7 121.5(2) . . ? C14 N1 C6 119.8(2) . . ? C7 N1 C6 118.6(2) . . ? C29 N2 S2 106.78(17) . . ? C28 N3 S2 106.14(17) . . ? C47 N4 C40 121.4(2) . . ? C47 N4 C37 118.7(2) . . ? C40 N4 C37 119.8(2) . . ? C23 S1 C20 90.83(13) . . ? N2 S2 N3 101.44(11) . . ? C33 S3 C30 90.80(12) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.722 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.069