# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ffj _database_code_depnum_ccdc_archive 'CCDC 850218' #TrackingRef 'jf2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H36 Cd N10 S2' _chemical_formula_weight 977.43 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' 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fdd2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 32.440(5) _cell_length_b 38.700(5) _cell_length_c 14.781(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 18556(7) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.81 _exptl_crystal_description neddle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7968 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8385 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28930 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8001 _reflns_number_gt 7243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 8001 _refine_ls_number_parameters 586 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Cd1 Cd 0.182539(9) 1.081874(7) 0.16633(3) 0.04069(11) Uani 1 1 d . . . S1 S 0.18497(5) 1.15106(6) 0.43855(14) 0.0824(5) Uani 1 1 d . . . S2 S 0.17171(6) 1.16828(6) -0.0756(2) 0.1168(10) Uani 1 1 d . . . N3 N 0.23725(11) 1.05056(10) 0.0925(2) 0.0406(8) Uani 1 1 d . . . N2 N 0.18309(10) 1.03093(10) 0.2657(3) 0.0378(8) Uani 1 1 d . . . N1 N 0.11690(10) 1.05710(9) 0.1753(3) 0.0420(8) Uani 1 1 d . . . C10 C 0.21735(13) 1.01532(11) 0.2999(3) 0.0371(9) Uani 1 1 d . . . C9 C 0.21853(14) 0.98090(11) 0.3246(3) 0.0416(10) Uani 1 1 d . . . H9 H 0.2431 0.9712 0.3450 0.050 Uiso 1 1 calc R . . N4 N 0.24222(11) 1.11570(9) 0.1580(3) 0.0483(9) Uani 1 1 d . . . C17 C 0.18322(14) 0.92432(12) 0.3486(4) 0.0452(11) Uani 1 1 d . . . C20 C 0.18194(14) 0.85574(12) 0.4085(4) 0.0505(12) Uani 1 1 d . . . C35 C 0.23506(14) 1.01802(12) 0.0611(3) 0.0426(10) Uani 1 1 d . . . C16 C 0.25400(13) 1.03797(11) 0.3164(3) 0.0393(10) Uani 1 1 d . . . C26 C 0.27775(15) 1.10113(12) 0.1315(3) 0.0434(10) Uani 1 1 d . . . C51 C 0.17046(16) 1.13299(14) 0.3454(4) 0.0508(12) Uani 1 1 d . . . C34 C 0.27012(15) 0.99862(13) 0.0401(3) 0.0470(11) Uani 1 1 d . . . H34 H 0.2673 0.9760 0.0197 0.056 Uiso 1 1 calc R . . C11 C 0.24806(14) 1.07062(12) 0.3552(3) 0.0442(10) Uani 1 1 d . . . H11 H 0.2215 1.0787 0.3655 0.053 Uiso 1 1 calc R . . C5 C 0.11152(14) 1.02901(12) 0.2265(3) 0.0413(10) Uani 1 1 d . . . C4 C 0.07190(16) 1.01769(16) 0.2464(5) 0.0636(16) Uani 1 1 d . . . H4 H 0.0680 0.9982 0.2822 0.076 Uiso 1 1 calc R . . C6 C 0.14901(14) 1.01137(11) 0.2616(3) 0.0398(10) Uani 1 1 d . . . C31 C 0.27618(14) 1.06467(12) 0.1007(3) 0.0412(10) Uani 1 1 d . . . N7 N 0.18128(15) 0.82093(11) 0.4393(4) 0.0606(14) Uani 1 1 d . . . C15 C 0.29387(15) 1.02669(13) 0.3009(4) 0.0487(11) Uani 1 1 d . . . H15 H 0.2984 1.0048 0.2766 0.058 Uiso 1 1 calc R . . N5 N 0.16043(15) 1.11321(13) 0.0410(4) 0.0667(14) Uani 1 1 d . . . C1 C 0.08445(16) 1.07387(13) 0.1417(4) 0.0534(14) Uani 1 1 d . . . H1 H 0.0890 1.0933 0.1061 0.064 Uiso 1 1 calc R . . C30 C 0.24198(17) 1.14879(13) 0.1778(5) 0.0640(15) Uani 1 1 d . . . H30 H 0.2169 1.1590 0.1924 0.077 Uiso 1 1 calc R . . C7 C 0.14765(14) 0.97684(11) 0.2866(3) 0.0427(10) Uani 1 1 d . . . H7 H 0.1232 0.9645 0.2817 0.051 Uiso 1 1 calc R . . C32 C 0.31152(15) 1.04592(14) 0.0806(3) 0.0471(11) Uani 1 1 d . . . H32 H 0.3373 1.0560 0.0884 0.056 Uiso 1 1 calc R . . C33 C 0.30883(15) 1.01279(13) 0.0495(3) 0.0452(11) Uani 1 1 d . . . N6 N 0.16125(15) 1.11948(12) 0.2795(4) 0.0613(12) Uani 1 1 d . . . C36 C 0.19366(15) 1.00302(13) 0.0468(4) 0.0483(11) Uani 1 1 d . . . C18 C 0.14574(18) 0.90747(15) 0.3697(5) 0.0694(18) Uani 1 1 d . . . H18 H 0.1209 0.9192 0.3633 0.083 Uiso 1 1 calc R . . C41 C 0.16264(17) 1.02195(16) 0.0054(4) 0.0603(14) Uani 1 1 d . . . H41 H 0.1674 1.0445 -0.0136 0.072 Uiso 1 1 calc R . . C14 C 0.32700(16) 1.04766(14) 0.3211(4) 0.0577(14) Uani 1 1 d . . . H14 H 0.3537 1.0403 0.3087 0.069 Uiso 1 1 calc R . . N9 N 0.45025(17) 0.93460(16) -0.0610(4) 0.0787(16) Uani 1 1 d . . . C29 C 0.2771(2) 1.16956(12) 0.1783(5) 0.0673(16) Uani 1 1 d . . . H29 H 0.2759 1.1928 0.1940 0.081 Uiso 1 1 calc R . . C8 C 0.18319(14) 0.96082(11) 0.3192(3) 0.0420(10) Uani 1 1 d . . . C12 C 0.28128(16) 1.09062(13) 0.3780(4) 0.0541(13) Uani 1 1 d . . . H12 H 0.2773 1.1119 0.4059 0.065 Uiso 1 1 calc R . . C22 C 0.21829(18) 0.90544(14) 0.3585(5) 0.0683(17) Uani 1 1 d . . . H22 H 0.2433 0.9158 0.3440 0.082 Uiso 1 1 calc R . . C52 C 0.16541(16) 1.13565(16) -0.0068(4) 0.0588(14) Uani 1 1 d . . . C23 C 0.14634(17) 0.80605(13) 0.4677(4) 0.0601(14) Uani 1 1 d . . . H23 H 0.1203 0.8160 0.4705 0.072 Uiso 1 1 calc R . . C45 C 0.41484(19) 0.95420(17) -0.0321(4) 0.0643(14) Uani 1 1 d . . . C27 C 0.31431(16) 1.12032(15) 0.1305(4) 0.0573(14) Uani 1 1 d . . . H27 H 0.3390 1.1100 0.1135 0.069 Uiso 1 1 calc R . . C43 C 0.34395(17) 0.95686(16) 0.0018(4) 0.0640(15) Uani 1 1 d . . . H43 H 0.3187 0.9457 0.0074 0.077 Uiso 1 1 calc R . . C42 C 0.34653(15) 0.99293(13) 0.0220(4) 0.0505(12) Uani 1 1 d . . . C2 C 0.04431(15) 1.06358(13) 0.1577(5) 0.0630(15) Uani 1 1 d . . . H2 H 0.0222 1.0754 0.1319 0.076 Uiso 1 1 calc R . . C46 C 0.41936(18) 0.98919(18) -0.0091(4) 0.0687(16) Uani 1 1 d . . . H46 H 0.4450 0.9998 -0.0123 0.082 Uiso 1 1 calc R . . C44 C 0.37737(18) 0.93843(17) -0.0252(5) 0.0691(16) Uani 1 1 d . . . H44 H 0.3747 0.9151 -0.0390 0.083 Uiso 1 1 calc R . . C28 C 0.31336(18) 1.15407(14) 0.1546(6) 0.0654(16) Uani 1 1 d . . . H28 H 0.3377 1.1668 0.1549 0.078 Uiso 1 1 calc R . . N8 N 0.2144(2) 0.79881(15) 0.4439(6) 0.105(2) Uani 1 1 d . . . C25 C 0.1967(3) 0.76816(17) 0.4786(6) 0.091(2) Uani 1 1 d . . . H25 H 0.2104 0.7476 0.4907 0.109 Uiso 1 1 calc R . . C3 C 0.03797(17) 1.03574(16) 0.2121(5) 0.0713(18) Uani 1 1 d . . . H3 H 0.0113 1.0288 0.2264 0.086 Uiso 1 1 calc R . . C37 C 0.18545(18) 0.96864(15) 0.0744(4) 0.0598(14) Uani 1 1 d . . . H37 H 0.2062 0.9553 0.1003 0.072 Uiso 1 1 calc R . . C19 C 0.14578(18) 0.87346(14) 0.3999(6) 0.078(2) Uani 1 1 d . . . H19 H 0.1210 0.8627 0.4143 0.093 Uiso 1 1 calc R . . C21 C 0.21878(18) 0.87130(14) 0.3892(5) 0.0656(17) Uani 1 1 d . . . H21 H 0.2435 0.8595 0.3963 0.079 Uiso 1 1 calc R . . C47 C 0.38516(17) 1.00749(16) 0.0181(4) 0.0643(15) Uani 1 1 d . . . H47 H 0.3883 1.0305 0.0345 0.077 Uiso 1 1 calc R . . C40 C 0.12440(18) 1.00666(19) -0.0070(5) 0.078(2) Uani 1 1 d . . . H40 H 0.1036 1.0190 -0.0360 0.093 Uiso 1 1 calc R . . C38 C 0.1468(2) 0.95532(19) 0.0626(5) 0.080(2) Uani 1 1 d . . . H38 H 0.1414 0.9330 0.0827 0.096 Uiso 1 1 calc R . . C13 C 0.32032(18) 1.07937(14) 0.3597(5) 0.0625(17) Uani 1 1 d . . . H13 H 0.3427 1.0934 0.3737 0.075 Uiso 1 1 calc R . . C49 C 0.5131(3) 0.9248(3) -0.0855(11) 0.139(4) Uani 1 1 d . . . H49 H 0.5414 0.9281 -0.0913 0.166 Uiso 1 1 calc R . . C48 C 0.48939(18) 0.9463(2) -0.0469(6) 0.093(3) Uani 1 1 d . . . H48 H 0.4971 0.9661 -0.0154 0.112 Uiso 1 1 calc R . . C39 C 0.1164(2) 0.9733(2) 0.0232(6) 0.088(2) Uani 1 1 d . . . H39 H 0.0904 0.9636 0.0160 0.106 Uiso 1 1 calc R . . C24 C 0.1568(2) 0.77442(16) 0.4908(6) 0.082(2) Uani 1 1 d . . . H24 H 0.1382 0.7582 0.5131 0.098 Uiso 1 1 calc R . . N10 N 0.4490(3) 0.9034(2) -0.1057(6) 0.119(3) Uani 1 1 d . . . C50 C 0.4945(4) 0.8989(3) -0.1148(7) 0.130(4) Uani 1 1 d . . . H50 H 0.5072 0.8794 -0.1389 0.156 Uiso 1 1 calc R . . 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 Cd1 0.03929(16) 0.03156(16) 0.05120(18) 0.00429(14) 0.00075(15) -0.00029(12) S1 0.0720(10) 0.0943(13) 0.0809(12) -0.0281(10) -0.0093(8) 0.0142(8) S2 0.0620(9) 0.1170(16) 0.171(2) 0.0964(18) 0.0058(14) 0.0006(10) N3 0.0405(19) 0.045(2) 0.0366(19) 0.0041(16) 0.0004(15) -0.0081(16) N2 0.0387(19) 0.0334(19) 0.041(2) -0.0003(16) -0.0007(15) 0.0020(14) N1 0.0439(19) 0.0308(16) 0.051(2) -0.0015(18) -0.0070(19) 0.0024(14) C10 0.042(2) 0.031(2) 0.039(2) 0.0037(18) 0.0012(19) 0.0033(18) C9 0.043(2) 0.037(2) 0.044(2) 0.0028(19) -0.0018(19) 0.0021(18) N4 0.044(2) 0.040(2) 0.061(3) 0.001(2) 0.003(2) -0.0046(15) C17 0.055(3) 0.033(2) 0.048(3) 0.004(2) -0.005(2) -0.0015(19) C20 0.066(3) 0.033(2) 0.053(3) 0.004(2) -0.008(3) -0.0071(18) C35 0.045(2) 0.045(3) 0.038(2) -0.003(2) 0.000(2) -0.004(2) C16 0.042(2) 0.035(2) 0.041(2) 0.0086(18) -0.0020(19) -0.0006(17) C26 0.051(3) 0.040(2) 0.040(2) 0.0039(19) -0.0012(19) -0.011(2) C51 0.039(2) 0.046(3) 0.067(4) -0.007(3) 0.008(2) 0.006(2) C34 0.052(3) 0.045(3) 0.044(3) -0.008(2) 0.000(2) 0.001(2) C11 0.044(2) 0.034(2) 0.054(3) 0.008(2) -0.002(2) 0.0015(19) C5 0.039(2) 0.038(2) 0.048(3) 0.0000(19) -0.0014(19) -0.0063(18) C4 0.050(3) 0.052(3) 0.089(4) 0.022(3) 0.002(3) -0.004(2) C6 0.044(2) 0.034(2) 0.041(2) 0.0033(18) 0.0027(19) -0.0040(18) C31 0.046(2) 0.043(2) 0.035(2) 0.0024(19) -0.0015(19) -0.007(2) N7 0.083(4) 0.031(2) 0.068(3) 0.010(2) -0.011(2) -0.0023(19) C15 0.050(3) 0.040(3) 0.056(3) 0.003(2) 0.002(2) 0.005(2) N5 0.064(3) 0.059(3) 0.077(3) 0.033(3) -0.004(2) -0.003(2) C1 0.049(3) 0.041(3) 0.070(4) 0.006(2) -0.007(2) 0.006(2) C30 0.062(3) 0.042(3) 0.088(4) -0.004(3) 0.009(3) -0.004(2) C7 0.042(2) 0.032(2) 0.055(3) 0.002(2) -0.003(2) -0.0005(18) C32 0.045(2) 0.056(3) 0.040(3) -0.002(2) 0.001(2) -0.007(2) C33 0.048(3) 0.053(3) 0.034(2) -0.003(2) -0.0010(19) 0.000(2) N6 0.059(3) 0.047(3) 0.079(4) -0.009(3) 0.008(2) 0.006(2) C36 0.049(3) 0.046(3) 0.050(3) -0.014(2) 0.004(2) -0.011(2) C18 0.053(3) 0.045(3) 0.110(5) 0.029(3) -0.017(3) -0.004(2) C41 0.056(3) 0.063(3) 0.063(3) -0.014(3) -0.008(3) 0.007(3) C14 0.039(2) 0.053(3) 0.081(4) 0.006(3) -0.001(2) 0.001(2) N9 0.072(3) 0.094(4) 0.070(4) -0.012(3) 0.005(3) 0.025(3) C29 0.076(4) 0.038(3) 0.088(5) -0.004(3) 0.008(4) -0.017(2) C8 0.053(3) 0.030(2) 0.043(3) 0.0023(19) -0.005(2) -0.0031(18) C12 0.054(3) 0.034(2) 0.074(4) 0.000(2) -0.004(2) -0.001(2) C22 0.056(3) 0.039(3) 0.110(5) 0.019(3) 0.019(3) 0.001(2) C52 0.036(3) 0.063(4) 0.078(4) 0.011(3) -0.008(3) 0.009(2) C23 0.052(3) 0.040(3) 0.089(4) 0.021(3) -0.006(3) -0.015(2) C45 0.063(3) 0.076(4) 0.054(3) -0.013(3) -0.001(3) 0.013(3) C27 0.048(3) 0.059(3) 0.065(3) -0.004(3) 0.004(2) -0.012(2) C43 0.053(3) 0.062(3) 0.077(4) -0.015(3) -0.005(3) 0.003(3) C42 0.048(3) 0.057(3) 0.046(3) -0.009(2) 0.000(2) 0.007(2) C2 0.041(2) 0.048(3) 0.100(5) 0.008(3) -0.011(3) 0.004(2) C46 0.044(3) 0.096(5) 0.067(4) -0.011(3) 0.007(3) 0.010(3) C44 0.062(3) 0.066(4) 0.080(4) -0.017(3) -0.009(3) 0.018(3) C28 0.068(3) 0.052(3) 0.076(4) -0.001(3) 0.002(3) -0.029(3) N8 0.125(5) 0.058(3) 0.132(7) 0.022(4) -0.005(4) 0.021(3) C25 0.117(6) 0.037(3) 0.120(6) 0.016(4) -0.023(5) -0.003(3) C3 0.041(3) 0.061(3) 0.113(5) 0.011(3) -0.001(3) -0.005(2) C37 0.067(3) 0.052(3) 0.060(3) -0.003(3) 0.003(3) -0.014(3) C19 0.060(3) 0.049(3) 0.125(6) 0.037(4) -0.015(4) -0.014(3) C21 0.058(3) 0.044(3) 0.096(5) 0.022(3) 0.014(3) 0.011(2) C47 0.060(3) 0.068(4) 0.065(3) -0.013(3) 0.006(3) 0.004(3) C40 0.051(3) 0.090(5) 0.093(5) -0.037(4) -0.009(3) -0.002(3) C38 0.078(5) 0.075(4) 0.087(5) -0.017(4) 0.024(4) -0.036(4) C13 0.058(4) 0.052(3) 0.078(4) 0.014(3) -0.017(3) -0.015(2) C49 0.073(5) 0.158(9) 0.185(12) -0.072(10) 0.013(7) 0.021(6) C48 0.042(3) 0.106(5) 0.132(7) -0.038(5) 0.001(3) 0.021(3) C39 0.049(3) 0.099(6) 0.116(6) -0.050(5) 0.009(4) -0.017(4) C24 0.077(4) 0.054(4) 0.114(6) 0.027(4) -0.017(4) -0.022(3) N10 0.136(6) 0.104(5) 0.118(7) -0.014(5) 0.032(5) 0.052(5) C50 0.136(8) 0.145(9) 0.108(7) 0.003(6) 0.047(6) 0.078(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N6 2.322(5) . ? Cd1 N5 2.327(5) . ? Cd1 N1 2.339(3) . ? Cd1 N4 2.340(4) . ? Cd1 N3 2.410(4) . ? Cd1 N2 2.459(4) . ? S1 C51 1.614(6) . ? S2 C52 1.634(7) . ? N3 C35 1.344(6) . ? N3 C31 1.381(6) . ? N2 C6 1.341(6) . ? N2 C10 1.362(6) . ? N1 C1 1.333(6) . ? N1 C5 1.336(6) . ? C10 C9 1.382(6) . ? C10 C16 1.497(6) . ? C9 C8 1.387(6) . ? C9 H9 0.9300 . ? N4 C30 1.314(6) . ? N4 C26 1.342(6) . ? C17 C22 1.360(7) . ? C17 C18 1.415(8) . ? C17 C8 1.478(7) . ? C20 C19 1.365(8) . ? C20 C21 1.368(7) . ? C20 N7 1.422(6) . ? C35 C34 1.398(7) . ? C35 C36 1.478(7) . ? C16 C15 1.384(7) . ? C16 C11 1.401(7) . ? C26 C27 1.400(7) . ? C26 C31 1.484(7) . ? C51 N6 1.146(7) . ? C34 C33 1.377(7) . ? C34 H34 0.9300 . ? C11 C12 1.369(7) . ? C11 H11 0.9300 . ? C5 C4 1.389(7) . ? C5 C6 1.488(7) . ? C4 C3 1.398(8) . ? C4 H4 0.9300 . ? C6 C7 1.387(6) . ? C31 C32 1.389(7) . ? N7 C23 1.339(7) . ? N7 N8 1.375(8) . ? C15 C14 1.379(7) . ? C15 H15 0.9300 . ? N5 C52 1.131(8) . ? C1 C2 1.382(8) . ? C1 H1 0.9300 . ? C30 C29 1.395(8) . ? C30 H30 0.9300 . ? C7 C8 1.395(6) . ? C7 H7 0.9300 . ? C32 C33 1.365(7) . ? C32 H32 0.9300 . ? C33 C42 1.500(7) . ? C36 C41 1.387(8) . ? C36 C37 1.417(8) . ? C18 C19 1.390(8) . ? C18 H18 0.9300 . ? C41 C40 1.387(8) . ? C41 H41 0.9300 . ? C14 C13 1.371(9) . ? C14 H14 0.9300 . ? N9 C48 1.364(9) . ? N9 N10 1.376(11) . ? N9 C45 1.441(8) . ? C29 C28 1.366(9) . ? C29 H29 0.9300 . ? C12 C13 1.366(8) . ? C12 H12 0.9300 . ? C22 C21 1.397(7) . ? C22 H22 0.9300 . ? C23 C24 1.315(8) . ? C23 H23 0.9300 . ? C45 C44 1.364(9) . ? C45 C46 1.404(9) . ? C27 C28 1.354(8) . ? C27 H27 0.9300 . ? C43 C44 1.358(8) . ? C43 C42 1.430(8) . ? C43 H43 0.9300 . ? C42 C47 1.375(7) . ? C2 C3 1.360(9) . ? C2 H2 0.9300 . ? C46 C47 1.376(8) . ? C46 H46 0.9300 . ? C44 H44 0.9300 . ? C28 H28 0.9300 . ? N8 C25 1.414(10) . ? C25 C24 1.330(11) . ? C25 H25 0.9300 . ? C3 H3 0.9300 . ? C37 C38 1.367(8) . ? C37 H37 0.9300 . ? C19 H19 0.9300 . ? C21 H21 0.9300 . ? C47 H47 0.9300 . ? C40 C39 1.391(12) . ? C40 H40 0.9300 . ? C38 C39 1.339(11) . ? C38 H38 0.9300 . ? C13 H13 0.9300 . ? C49 C50 1.250(15) . ? C49 C48 1.268(11) . ? C49 H49 0.9300 . ? C48 H48 0.9300 . ? C39 H39 0.9300 . ? C24 H24 0.9300 . ? N10 C50 1.490(13) . ? C50 H50 0.9300 . ? 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 N6 Cd1 N5 98.93(18) . . ? N6 Cd1 N1 86.85(15) . . ? N5 Cd1 N1 88.76(16) . . ? N6 Cd1 N4 86.19(16) . . ? N5 Cd1 N4 85.51(17) . . ? N1 Cd1 N4 170.19(12) . . ? N6 Cd1 N3 149.34(16) . . ? N5 Cd1 N3 97.38(17) . . ? N1 Cd1 N3 119.34(12) . . ? N4 Cd1 N3 69.40(13) . . ? N6 Cd1 N2 94.25(15) . . ? N5 Cd1 N2 153.59(16) . . ? N1 Cd1 N2 69.14(12) . . ? N4 Cd1 N2 118.29(13) . . ? N3 Cd1 N2 82.07(12) . . ? C35 N3 C31 116.7(4) . . ? C35 N3 Cd1 126.1(3) . . ? C31 N3 Cd1 115.8(3) . . ? C6 N2 C10 116.1(4) . . ? C6 N2 Cd1 114.8(3) . . ? C10 N2 Cd1 125.7(3) . . ? C1 N1 C5 120.3(4) . . ? C1 N1 Cd1 119.9(3) . . ? C5 N1 Cd1 119.0(3) . . ? N2 C10 C9 123.2(4) . . ? N2 C10 C16 116.7(4) . . ? C9 C10 C16 120.0(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C30 N4 C26 118.7(4) . . ? C30 N4 Cd1 121.9(3) . . ? C26 N4 Cd1 119.4(3) . . ? C22 C17 C18 116.6(5) . . ? C22 C17 C8 123.1(4) . . ? C18 C17 C8 120.3(4) . . ? C19 C20 C21 120.7(5) . . ? C19 C20 N7 119.5(4) . . ? C21 C20 N7 119.8(4) . . ? N3 C35 C34 122.5(4) . . ? N3 C35 C36 117.8(4) . . ? C34 C35 C36 119.8(4) . . ? C15 C16 C11 118.8(4) . . ? C15 C16 C10 122.0(4) . . ? C11 C16 C10 119.1(4) . . ? N4 C26 C27 120.5(4) . . ? N4 C26 C31 117.4(4) . . ? C27 C26 C31 122.1(4) . . ? N6 C51 S1 177.8(5) . . ? C33 C34 C35 120.4(4) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C12 C11 C16 120.1(5) . . ? C12 C11 H11 119.9 . . ? C16 C11 H11 119.9 . . ? N1 C5 C4 119.8(4) . . ? N1 C5 C6 117.6(4) . . ? C4 C5 C6 122.6(4) . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N2 C6 C7 123.9(4) . . ? N2 C6 C5 115.5(4) . . ? C7 C6 C5 120.6(4) . . ? N3 C31 C32 122.0(4) . . ? N3 C31 C26 115.7(4) . . ? C32 C31 C26 122.3(4) . . ? C23 N7 N8 112.2(5) . . ? C23 N7 C20 121.4(5) . . ? N8 N7 C20 126.5(5) . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C52 N5 Cd1 148.6(5) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? N4 C30 C29 123.9(5) . . ? N4 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? C6 C7 C8 119.6(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 117.8(5) . . ? C32 C33 C42 121.3(4) . . ? C34 C33 C42 120.8(4) . . ? C51 N6 Cd1 145.2(4) . . ? C41 C36 C37 119.1(5) . . ? C41 C36 C35 121.0(5) . . ? C37 C36 C35 119.9(5) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C40 C41 C36 118.8(6) . . ? C40 C41 H41 120.6 . . ? C36 C41 H41 120.6 . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C48 N9 N10 113.0(6) . . ? C48 N9 C45 121.4(6) . . ? N10 N9 C45 125.5(6) . . ? C28 C29 C30 116.7(5) . . ? C28 C29 H29 121.7 . . ? C30 C29 H29 121.7 . . ? C9 C8 C7 117.0(4) . . ? C9 C8 C17 121.2(4) . . ? C7 C8 C17 121.8(4) . . ? C13 C12 C11 120.1(5) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C17 C22 C21 123.6(5) . . ? C17 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N5 C52 S2 178.9(6) . . ? C24 C23 N7 105.3(6) . . ? C24 C23 H23 127.3 . . ? N7 C23 H23 127.3 . . ? C44 C45 C46 120.4(5) . . ? C44 C45 N9 119.8(6) . . ? C46 C45 N9 119.7(6) . . ? C28 C27 C26 119.3(5) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C44 C43 C42 121.8(5) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C47 C42 C43 116.4(5) . . ? C47 C42 C33 123.0(5) . . ? C43 C42 C33 120.6(5) . . ? C3 C2 C1 118.1(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C47 C46 C45 118.9(6) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C43 C44 C45 119.9(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? N7 N8 C25 103.0(7) . . ? C24 C25 N8 106.9(6) . . ? C24 C25 H25 126.5 . . ? N8 C25 H25 126.5 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C38 C37 C36 119.3(6) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C20 C21 C22 118.3(5) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C42 C47 C46 122.4(6) . . ? C42 C47 H47 118.8 . . ? C46 C47 H47 118.8 . . ? C41 C40 C39 121.3(7) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C39 C38 C37 122.3(7) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C12 C13 C14 120.9(5) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C50 C49 C48 112.8(9) . . ? C50 C49 H49 123.6 . . ? C48 C49 H49 123.6 . . ? C49 C48 N9 106.2(8) . . ? C49 C48 H48 126.9 . . ? N9 C48 H48 126.9 . . ? C38 C39 C40 119.0(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C23 C24 C25 112.7(6) . . ? C23 C24 H24 123.7 . . ? C25 C24 H24 123.7 . . ? N9 N10 C50 96.8(8) . . ? C49 C50 N10 110.7(8) . . ? C49 C50 H50 124.7 . . ? N10 C50 H50 124.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cd1 N3 C35 139.6(4) . . . . ? N5 Cd1 N3 C35 -98.7(4) . . . . ? N1 Cd1 N3 C35 -6.0(4) . . . . ? N4 Cd1 N3 C35 178.9(4) . . . . ? N2 Cd1 N3 C35 54.6(4) . . . . ? N6 Cd1 N3 C31 -26.0(5) . . . . ? N5 Cd1 N3 C31 95.7(3) . . . . ? N1 Cd1 N3 C31 -171.5(3) . . . . ? N4 Cd1 N3 C31 13.4(3) . . . . ? N2 Cd1 N3 C31 -110.9(3) . . . . ? N6 Cd1 N2 C6 97.0(3) . . . . ? N5 Cd1 N2 C6 -23.0(5) . . . . ? N1 Cd1 N2 C6 12.0(3) . . . . ? N4 Cd1 N2 C6 -175.0(3) . . . . ? N3 Cd1 N2 C6 -113.6(3) . . . . ? N6 Cd1 N2 C10 -105.1(4) . . . . ? N5 Cd1 N2 C10 135.0(4) . . . . ? N1 Cd1 N2 C10 169.9(4) . . . . ? N4 Cd1 N2 C10 -17.1(4) . . . . ? N3 Cd1 N2 C10 44.3(3) . . . . ? N6 Cd1 N1 C1 73.6(4) . . . . ? N5 Cd1 N1 C1 -25.4(4) . . . . ? N4 Cd1 N1 C1 28.8(12) . . . . ? N3 Cd1 N1 C1 -123.2(4) . . . . ? N2 Cd1 N1 C1 169.4(4) . . . . ? N6 Cd1 N1 C5 -95.9(4) . . . . ? N5 Cd1 N1 C5 165.1(4) . . . . ? N4 Cd1 N1 C5 -140.7(9) . . . . ? N3 Cd1 N1 C5 67.3(4) . . . . ? N2 Cd1 N1 C5 -0.1(3) . . . . ? C6 N2 C10 C9 3.5(6) . . . . ? Cd1 N2 C10 C9 -154.2(4) . . . . ? C6 N2 C10 C16 -172.1(4) . . . . ? Cd1 N2 C10 C16 30.2(5) . . . . ? N2 C10 C9 C8 -3.0(7) . . . . ? C16 C10 C9 C8 172.5(4) . . . . ? N6 Cd1 N4 C30 -29.4(5) . . . . ? N5 Cd1 N4 C30 69.9(5) . . . . ? N1 Cd1 N4 C30 15.5(13) . . . . ? N3 Cd1 N4 C30 169.5(5) . . . . ? N2 Cd1 N4 C30 -122.2(5) . . . . ? N6 Cd1 N4 C26 151.2(4) . . . . ? N5 Cd1 N4 C26 -109.5(4) . . . . ? N1 Cd1 N4 C26 -163.9(8) . . . . ? N3 Cd1 N4 C26 -9.8(4) . . . . ? N2 Cd1 N4 C26 58.5(4) . . . . ? C31 N3 C35 C34 2.0(7) . . . . ? Cd1 N3 C35 C34 -163.4(4) . . . . ? C31 N3 C35 C36 -176.6(4) . . . . ? Cd1 N3 C35 C36 18.0(6) . . . . ? N2 C10 C16 C15 -142.7(4) . . . . ? C9 C10 C16 C15 41.5(7) . . . . ? N2 C10 C16 C11 42.2(6) . . . . ? C9 C10 C16 C11 -133.6(5) . . . . ? C30 N4 C26 C27 4.0(8) . . . . ? Cd1 N4 C26 C27 -176.6(4) . . . . ? C30 N4 C26 C31 -173.9(5) . . . . ? Cd1 N4 C26 C31 5.5(6) . . . . ? N3 C35 C34 C33 -1.3(8) . . . . ? C36 C35 C34 C33 177.2(5) . . . . ? C15 C16 C11 C12 -0.8(7) . . . . ? C10 C16 C11 C12 174.5(4) . . . . ? C1 N1 C5 C4 -1.4(8) . . . . ? Cd1 N1 C5 C4 168.1(4) . . . . ? C1 N1 C5 C6 179.7(4) . . . . ? Cd1 N1 C5 C6 -10.9(6) . . . . ? N1 C5 C4 C3 0.3(10) . . . . ? C6 C5 C4 C3 179.2(6) . . . . ? C10 N2 C6 C7 -2.4(7) . . . . ? Cd1 N2 C6 C7 157.8(4) . . . . ? C10 N2 C6 C5 178.4(4) . . . . ? Cd1 N2 C6 C5 -21.5(5) . . . . ? N1 C5 C6 N2 22.1(6) . . . . ? C4 C5 C6 N2 -156.8(5) . . . . ? N1 C5 C6 C7 -157.2(5) . . . . ? C4 C5 C6 C7 23.9(8) . . . . ? C35 N3 C31 C32 -2.2(6) . . . . ? Cd1 N3 C31 C32 164.7(4) . . . . ? C35 N3 C31 C26 177.3(4) . . . . ? Cd1 N3 C31 C26 -15.7(5) . . . . ? N4 C26 C31 N3 7.2(6) . . . . ? C27 C26 C31 N3 -170.7(5) . . . . ? N4 C26 C31 C32 -173.2(5) . . . . ? C27 C26 C31 C32 8.9(7) . . . . ? C19 C20 N7 C23 -5.9(9) . . . . ? C21 C20 N7 C23 173.0(6) . . . . ? C19 C20 N7 N8 173.8(7) . . . . ? C21 C20 N7 N8 -7.2(10) . . . . ? C11 C16 C15 C14 -1.6(7) . . . . ? C10 C16 C15 C14 -176.8(5) . . . . ? N6 Cd1 N5 C52 76.4(10) . . . . ? N1 Cd1 N5 C52 163.0(10) . . . . ? N4 Cd1 N5 C52 -9.0(10) . . . . ? N3 Cd1 N5 C52 -77.5(10) . . . . ? N2 Cd1 N5 C52 -164.6(8) . . . . ? C5 N1 C1 C2 0.3(8) . . . . ? Cd1 N1 C1 C2 -169.1(5) . . . . ? C26 N4 C30 C29 -4.1(10) . . . . ? Cd1 N4 C30 C29 176.6(6) . . . . ? N2 C6 C7 C8 0.7(8) . . . . ? C5 C6 C7 C8 179.9(4) . . . . ? N3 C31 C32 C33 1.8(7) . . . . ? C26 C31 C32 C33 -177.8(4) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C31 C32 C33 C42 176.1(5) . . . . ? C35 C34 C33 C32 0.7(7) . . . . ? C35 C34 C33 C42 -176.4(5) . . . . ? S1 C51 N6 Cd1 -12(17) . . . . ? N5 Cd1 N6 C51 -134.1(8) . . . . ? N1 Cd1 N6 C51 137.7(8) . . . . ? N4 Cd1 N6 C51 -49.2(8) . . . . ? N3 Cd1 N6 C51 -12.7(10) . . . . ? N2 Cd1 N6 C51 68.9(8) . . . . ? N3 C35 C36 C41 44.2(7) . . . . ? C34 C35 C36 C41 -134.5(5) . . . . ? N3 C35 C36 C37 -136.7(5) . . . . ? C34 C35 C36 C37 44.7(7) . . . . ? C22 C17 C18 C19 0.8(10) . . . . ? C8 C17 C18 C19 -178.2(6) . . . . ? C37 C36 C41 C40 0.4(8) . . . . ? C35 C36 C41 C40 179.6(5) . . . . ? C16 C15 C14 C13 2.2(9) . . . . ? N4 C30 C29 C28 1.5(11) . . . . ? C10 C9 C8 C7 1.1(7) . . . . ? C10 C9 C8 C17 -177.5(5) . . . . ? C6 C7 C8 C9 0.0(7) . . . . ? C6 C7 C8 C17 178.6(5) . . . . ? C22 C17 C8 C9 -18.8(8) . . . . ? C18 C17 C8 C9 160.1(6) . . . . ? C22 C17 C8 C7 162.7(6) . . . . ? C18 C17 C8 C7 -18.5(8) . . . . ? C16 C11 C12 C13 2.6(8) . . . . ? C18 C17 C22 C21 -1.1(11) . . . . ? C8 C17 C22 C21 177.8(6) . . . . ? Cd1 N5 C52 S2 -130(39) . . . . ? N8 N7 C23 C24 0.1(8) . . . . ? C20 N7 C23 C24 179.9(6) . . . . ? C48 N9 C45 C44 -162.9(7) . . . . ? N10 N9 C45 C44 18.2(10) . . . . ? C48 N9 C45 C46 15.6(10) . . . . ? N10 N9 C45 C46 -163.3(7) . . . . ? N4 C26 C27 C28 -1.6(9) . . . . ? C31 C26 C27 C28 176.3(6) . . . . ? C44 C43 C42 C47 -4.0(9) . . . . ? C44 C43 C42 C33 178.4(6) . . . . ? C32 C33 C42 C47 -6.3(8) . . . . ? C34 C33 C42 C47 170.7(5) . . . . ? C32 C33 C42 C43 171.1(5) . . . . ? C34 C33 C42 C43 -11.9(8) . . . . ? N1 C1 C2 C3 1.9(10) . . . . ? C44 C45 C46 C47 -1.7(10) . . . . ? N9 C45 C46 C47 179.8(6) . . . . ? C42 C43 C44 C45 1.3(10) . . . . ? C46 C45 C44 C43 1.6(10) . . . . ? N9 C45 C44 C43 -179.9(6) . . . . ? C26 C27 C28 C29 -1.0(11) . . . . ? C30 C29 C28 C27 1.1(12) . . . . ? C23 N7 N8 C25 -0.2(9) . . . . ? C20 N7 N8 C25 -180.0(6) . . . . ? N7 N8 C25 C24 0.1(9) . . . . ? C1 C2 C3 C4 -2.9(11) . . . . ? C5 C4 C3 C2 1.9(11) . . . . ? C41 C36 C37 C38 -2.3(9) . . . . ? C35 C36 C37 C38 178.6(6) . . . . ? C21 C20 C19 C18 1.2(11) . . . . ? N7 C20 C19 C18 -179.9(7) . . . . ? C17 C18 C19 C20 -0.8(12) . . . . ? C19 C20 C21 C22 -1.5(10) . . . . ? N7 C20 C21 C22 179.6(6) . . . . ? C17 C22 C21 C20 1.5(11) . . . . ? C43 C42 C47 C46 4.0(9) . . . . ? C33 C42 C47 C46 -178.5(5) . . . . ? C45 C46 C47 C42 -1.3(10) . . . . ? C36 C41 C40 C39 1.7(10) . . . . ? C36 C37 C38 C39 2.1(10) . . . . ? C11 C12 C13 C14 -2.0(10) . . . . ? C15 C14 C13 C12 -0.4(10) . . . . ? C50 C49 C48 N9 -6.8(16) . . . . ? N10 N9 C48 C49 3.7(13) . . . . ? C45 N9 C48 C49 -175.3(9) . . . . ? C37 C38 C39 C40 0.0(11) . . . . ? C41 C40 C39 C38 -1.9(11) . . . . ? N7 C23 C24 C25 0.0(9) . . . . ? N8 C25 C24 C23 -0.1(10) . . . . ? C48 N9 N10 C50 0.3(9) . . . . ? C45 N9 N10 C50 179.2(7) . . . . ? C48 C49 C50 N10 7.3(17) . . . . ? N9 N10 C50 C49 -4.3(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.384 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.083 data_jf _database_code_depnum_ccdc_archive 'CCDC 854147' #TrackingRef 'jf.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H18 Hg N6 S2' _chemical_formula_weight 691.18 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' 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' Hg Hg -2.3894 9.2266 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 13.460(5) _cell_length_b 25.921(5) _cell_length_c 7.340(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 95.017(5) _cell_angle_gamma 90.000(5) _cell_volume 2551(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 6.225 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2567 _exptl_absorpt_correction_T_max 0.3690 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17956 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4497 _reflns_number_gt 3873 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0346P)^2^+0.7745P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00040(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4497 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 Hg1 Hg 0.739625(12) 0.953664(6) 0.23186(2) 0.04978(9) Uani 1 1 d . . . S1 S 0.67534(8) 0.92029(4) 0.51183(15) 0.0571(3) Uani 1 1 d . . . S2 S 0.63786(10) 1.00980(5) 0.0225(2) 0.0789(4) Uani 1 1 d . . . C2 C 1.0251(3) 1.05142(14) 0.2954(5) 0.0460(9) Uani 1 1 d . . . H2 H 1.0404 1.0853 0.3284 0.055 Uiso 1 1 calc R . . N2 N 0.8447(2) 0.88852(11) 0.1328(4) 0.0378(7) Uani 1 1 d . . . C7 C 1.0132(3) 0.86002(13) 0.1326(5) 0.0398(8) Uani 1 1 d . . . H7 H 1.0808 0.8680 0.1475 0.048 Uiso 1 1 calc R . . N1 N 0.9049(2) 0.98386(11) 0.2592(4) 0.0379(7) Uani 1 1 d . . . C27 C 0.7521(3) 0.87073(18) 0.5536(6) 0.0545(10) Uani 1 1 d . . . C26 C 0.7036(3) 1.06390(18) 0.0497(6) 0.0557(11) Uani 1 1 d . . . C9 C 0.8811(3) 0.80031(14) 0.0706(5) 0.0423(9) Uani 1 1 d . . . H9 H 0.8577 0.7673 0.0420 0.051 Uiso 1 1 calc R . . N6 N 0.8043(4) 0.83657(19) 0.5897(7) 0.0914(14) Uani 1 1 d . . . C1 C 0.9305(3) 1.03225(14) 0.3056(5) 0.0440(9) Uani 1 1 d . . . H1 H 0.8822 1.0539 0.3467 0.053 Uiso 1 1 calc R . . C5 C 0.9748(3) 0.95200(12) 0.2013(5) 0.0368(8) Uani 1 1 d . . . C11 C 0.7039(3) 0.83082(14) 0.0745(5) 0.0431(9) Uani 1 1 d . . . C4 C 1.0722(3) 0.96903(14) 0.1886(5) 0.0409(8) Uani 1 1 d . . . H4 H 1.1201 0.9468 0.1492 0.049 Uiso 1 1 calc R . . C3 C 1.0965(3) 1.01923(14) 0.2354(5) 0.0457(9) Uani 1 1 d . . . H3 H 1.1610 1.0313 0.2264 0.055 Uiso 1 1 calc R . . C10 C 0.8137(3) 0.83977(13) 0.0933(5) 0.0382(8) Uani 1 1 d . . . C17 C 1.0581(3) 0.76845(13) 0.0669(5) 0.0376(8) Uani 1 1 d . . . C22 C 1.0335(3) 0.71661(13) 0.0872(5) 0.0417(9) Uani 1 1 d . . . H22 H 0.9702 0.7076 0.1177 0.050 Uiso 1 1 calc R . . N5 N 0.7466(4) 1.10201(16) 0.0639(6) 0.0837(13) Uani 1 1 d . . . C6 C 0.9435(3) 0.89816(12) 0.1527(4) 0.0350(8) Uani 1 1 d . . . C8 C 0.9834(3) 0.80951(13) 0.0900(5) 0.0381(8) Uani 1 1 d . . . C19 C 1.2222(3) 0.74228(14) -0.0040(5) 0.0464(10) Uani 1 1 d . . . H19 H 1.2855 0.7510 -0.0356 0.056 Uiso 1 1 calc R . . C18 C 1.1536(3) 0.78050(14) 0.0229(5) 0.0444(9) Uani 1 1 d . . . H18 H 1.1717 0.8149 0.0113 0.053 Uiso 1 1 calc R . . C16 C 0.6401(3) 0.86462(16) -0.0260(5) 0.0509(10) Uani 1 1 d . . . H16 H 0.6669 0.8922 -0.0865 0.061 Uiso 1 1 calc R . . C12 C 0.6633(3) 0.78914(17) 0.1600(6) 0.0616(12) Uani 1 1 d . . . H12 H 0.7046 0.7655 0.2249 0.074 Uiso 1 1 calc R . . C15 C 0.5384(3) 0.85806(19) -0.0375(7) 0.0675(13) Uani 1 1 d . . . H15 H 0.4969 0.8808 -0.1060 0.081 Uiso 1 1 calc R . . C14 C 0.4986(4) 0.8176(2) 0.0530(8) 0.0813(16) Uani 1 1 d . . . H14 H 0.4298 0.8138 0.0497 0.098 Uiso 1 1 calc R . . C13 C 0.5601(4) 0.7830(2) 0.1479(8) 0.0828(16) Uani 1 1 d . . . H13 H 0.5327 0.7550 0.2050 0.099 Uiso 1 1 calc R . . C20 C 1.1969(3) 0.69106(13) 0.0158(5) 0.0389(8) Uani 1 1 d . . . C21 C 1.1024(3) 0.67881(14) 0.0625(5) 0.0438(9) Uani 1 1 d . . . H21 H 1.0852 0.6444 0.0772 0.053 Uiso 1 1 calc R . . C23 C 1.3652(4) 0.6540(2) -0.0153(8) 0.0823(16) Uani 1 1 d . . . H23 H 1.4040 0.6836 0.0043 0.099 Uiso 1 1 calc R . . N3 N 1.2663(2) 0.65147(12) -0.0139(4) 0.0453(7) Uani 1 1 d . . . N4 N 1.2338(3) 0.60278(12) -0.0483(5) 0.0556(9) Uani 1 1 d . . . C25 C 1.3160(4) 0.57626(18) -0.0688(6) 0.0638(12) Uani 1 1 d . . . H25 H 1.3169 0.5411 -0.0933 0.077 Uiso 1 1 calc R . . C24 C 1.3993(4) 0.6064(2) -0.0499(8) 0.0859(17) Uani 1 1 d . . . H24 H 1.4650 0.5963 -0.0589 0.103 Uiso 1 1 calc R . . 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 Hg1 0.04359(12) 0.03990(12) 0.06713(13) 0.00282(7) 0.01210(8) 0.00087(7) S1 0.0461(6) 0.0612(7) 0.0663(7) 0.0058(5) 0.0187(5) 0.0035(5) S2 0.0590(8) 0.0516(7) 0.1203(11) 0.0191(7) -0.0251(7) -0.0070(6) C2 0.048(2) 0.033(2) 0.056(2) -0.0085(17) 0.0026(19) -0.0068(17) N2 0.0390(17) 0.0314(16) 0.0430(16) 0.0014(13) 0.0032(14) -0.0004(13) C7 0.038(2) 0.034(2) 0.047(2) -0.0016(16) -0.0003(16) -0.0013(16) N1 0.0358(17) 0.0312(16) 0.0472(16) -0.0020(13) 0.0069(13) 0.0013(13) C27 0.049(3) 0.058(3) 0.057(2) 0.000(2) 0.013(2) -0.007(2) C26 0.047(3) 0.049(3) 0.071(3) 0.012(2) 0.007(2) 0.006(2) C9 0.045(2) 0.0316(19) 0.050(2) -0.0008(16) 0.0014(17) -0.0036(17) N6 0.085(3) 0.086(3) 0.104(4) 0.022(3) 0.019(3) 0.025(3) C1 0.045(2) 0.035(2) 0.052(2) -0.0081(16) 0.0062(18) 0.0017(17) C5 0.040(2) 0.0335(19) 0.0360(17) 0.0010(15) 0.0006(16) -0.0015(16) C11 0.042(2) 0.039(2) 0.049(2) -0.0072(17) 0.0050(18) -0.0038(17) C4 0.035(2) 0.037(2) 0.051(2) -0.0042(16) 0.0046(17) -0.0008(16) C3 0.040(2) 0.040(2) 0.056(2) -0.0023(18) 0.0004(18) -0.0067(18) C10 0.042(2) 0.0336(19) 0.0386(18) -0.0003(15) 0.0012(16) -0.0044(16) C17 0.039(2) 0.0329(19) 0.0405(19) -0.0022(15) 0.0015(16) 0.0011(16) C22 0.039(2) 0.034(2) 0.053(2) 0.0008(16) 0.0120(17) -0.0016(16) N5 0.090(3) 0.055(3) 0.105(3) 0.014(2) 0.001(3) -0.017(2) C6 0.040(2) 0.0285(18) 0.0363(18) 0.0018(14) 0.0005(16) -0.0021(15) C8 0.041(2) 0.0327(19) 0.0401(19) 0.0008(15) 0.0017(16) 0.0001(16) C19 0.040(2) 0.043(2) 0.057(2) 0.0007(18) 0.0118(19) -0.0067(18) C18 0.052(2) 0.0273(19) 0.054(2) -0.0005(16) 0.0037(19) -0.0054(17) C16 0.049(2) 0.047(2) 0.057(2) -0.0058(19) 0.003(2) 0.000(2) C12 0.057(3) 0.049(3) 0.078(3) 0.003(2) 0.003(2) -0.014(2) C15 0.041(3) 0.074(3) 0.086(3) -0.018(3) -0.006(2) 0.007(2) C14 0.037(3) 0.098(4) 0.109(4) -0.023(3) 0.007(3) -0.012(3) C13 0.065(3) 0.081(4) 0.104(4) -0.002(3) 0.017(3) -0.033(3) C20 0.038(2) 0.035(2) 0.0436(19) -0.0025(15) 0.0005(16) 0.0003(16) C21 0.046(2) 0.0302(19) 0.056(2) 0.0003(16) 0.0073(19) -0.0059(17) C23 0.041(3) 0.065(3) 0.141(5) -0.021(3) 0.007(3) 0.000(2) N3 0.0424(19) 0.0392(18) 0.0544(18) -0.0016(14) 0.0059(15) 0.0018(15) N4 0.056(2) 0.0354(18) 0.077(2) -0.0081(17) 0.0140(19) 0.0053(16) C25 0.064(3) 0.050(3) 0.078(3) -0.007(2) 0.014(2) 0.019(2) C24 0.044(3) 0.080(4) 0.134(5) -0.013(3) 0.007(3) 0.020(3) _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 Hg1 N1 2.350(3) . ? Hg1 N2 2.358(3) . ? Hg1 S2 2.4466(14) . ? Hg1 S1 2.4559(16) . ? S1 C27 1.660(5) . ? S2 C26 1.661(5) . ? C2 C3 1.374(5) . ? C2 C1 1.375(6) . ? C2 H2 0.9300 . ? N2 C6 1.349(4) . ? N2 C10 1.354(4) . ? C7 C6 1.380(5) . ? C7 C8 1.396(5) . ? C7 H7 0.9300 . ? N1 C1 1.337(4) . ? N1 C5 1.348(4) . ? C27 N6 1.147(6) . ? C26 N5 1.145(6) . ? C9 C10 1.387(5) . ? C9 C8 1.393(5) . ? C9 H9 0.9300 . ? C1 H1 0.9300 . ? C5 C4 1.395(5) . ? C5 C6 1.492(4) . ? C11 C12 1.386(5) . ? C11 C16 1.392(6) . ? C11 C10 1.490(5) . ? C4 C3 1.378(5) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C17 C18 1.388(5) . ? C17 C22 1.395(5) . ? C17 C8 1.484(5) . ? C22 C21 1.371(5) . ? C22 H22 0.9300 . ? C19 C18 1.380(5) . ? C19 C20 1.382(5) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C16 C15 1.375(6) . ? C16 H16 0.9300 . ? C12 C13 1.393(7) . ? C12 H12 0.9300 . ? C15 C14 1.374(7) . ? C15 H15 0.9300 . ? C14 C13 1.370(8) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C20 C21 1.383(5) . ? C20 N3 1.418(4) . ? C21 H21 0.9300 . ? C23 N3 1.334(5) . ? C23 C24 1.349(6) . ? C23 H23 0.9300 . ? N3 N4 1.352(4) . ? N4 C25 1.322(5) . ? C25 C24 1.364(7) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? 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 N1 Hg1 N2 71.10(10) . . ? N1 Hg1 S2 109.22(8) . . ? N2 Hg1 S2 123.38(9) . . ? N1 Hg1 S1 116.49(8) . . ? N2 Hg1 S1 105.70(7) . . ? S2 Hg1 S1 121.07(5) . . ? C27 S1 Hg1 99.68(14) . . ? C26 S2 Hg1 99.41(17) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C6 N2 C10 118.6(3) . . ? C6 N2 Hg1 116.5(2) . . ? C10 N2 Hg1 123.5(2) . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Hg1 123.8(2) . . ? C5 N1 Hg1 116.8(2) . . ? N6 C27 S1 177.2(4) . . ? N5 C26 S2 177.5(5) . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? N1 C5 C4 120.9(3) . . ? N1 C5 C6 117.3(3) . . ? C4 C5 C6 121.8(3) . . ? C12 C11 C16 118.8(4) . . ? C12 C11 C10 120.4(4) . . ? C16 C11 C10 120.8(3) . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? N2 C10 C9 121.4(3) . . ? N2 C10 C11 116.7(3) . . ? C9 C10 C11 121.9(3) . . ? C18 C17 C22 118.3(3) . . ? C18 C17 C8 121.0(3) . . ? C22 C17 C8 120.6(3) . . ? C21 C22 C17 120.3(3) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? N2 C6 C7 121.9(3) . . ? N2 C6 C5 117.0(3) . . ? C7 C6 C5 121.1(3) . . ? C9 C8 C7 116.4(3) . . ? C9 C8 C17 122.6(3) . . ? C7 C8 C17 120.9(3) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C18 C17 121.1(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C15 C16 C11 121.3(4) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C13 C12 120.8(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C19 C20 C21 119.2(3) . . ? C19 C20 N3 120.5(3) . . ? C21 C20 N3 120.3(3) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? N3 C23 C24 108.2(4) . . ? N3 C23 H23 125.9 . . ? C24 C23 H23 125.9 . . ? C23 N3 N4 110.6(3) . . ? C23 N3 C20 129.5(4) . . ? N4 N3 C20 119.9(3) . . ? C25 N4 N3 104.3(4) . . ? N4 C25 C24 112.3(4) . . ? N4 C25 H25 123.9 . . ? C24 C25 H25 123.9 . . ? C23 C24 C25 104.7(4) . . ? C23 C24 H24 127.7 . . ? C25 C24 H24 127.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Hg1 S1 C27 -62.88(18) . . . . ? N2 Hg1 S1 C27 13.48(18) . . . . ? S2 Hg1 S1 C27 160.26(16) . . . . ? N1 Hg1 S2 C26 -26.21(18) . . . . ? N2 Hg1 S2 C26 -105.79(18) . . . . ? S1 Hg1 S2 C26 113.39(17) . . . . ? N1 Hg1 N2 C6 4.9(2) . . . . ? S2 Hg1 N2 C6 105.9(2) . . . . ? S1 Hg1 N2 C6 -108.3(2) . . . . ? N1 Hg1 N2 C10 171.3(3) . . . . ? S2 Hg1 N2 C10 -87.7(3) . . . . ? S1 Hg1 N2 C10 58.1(3) . . . . ? N2 Hg1 N1 C1 173.6(3) . . . . ? S2 Hg1 N1 C1 53.9(3) . . . . ? S1 Hg1 N1 C1 -87.8(3) . . . . ? N2 Hg1 N1 C5 2.5(2) . . . . ? S2 Hg1 N1 C5 -117.2(2) . . . . ? S1 Hg1 N1 C5 101.1(2) . . . . ? Hg1 S1 C27 N6 158(10) . . . . ? Hg1 S2 C26 N5 177(100) . . . . ? C5 N1 C1 C2 0.7(6) . . . . ? Hg1 N1 C1 C2 -170.3(3) . . . . ? C3 C2 C1 N1 -0.3(6) . . . . ? C1 N1 C5 C4 -0.4(5) . . . . ? Hg1 N1 C5 C4 171.2(3) . . . . ? C1 N1 C5 C6 179.4(3) . . . . ? Hg1 N1 C5 C6 -9.1(4) . . . . ? N1 C5 C4 C3 -0.3(5) . . . . ? C6 C5 C4 C3 180.0(3) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C5 C4 C3 C2 0.7(6) . . . . ? C6 N2 C10 C9 -1.0(5) . . . . ? Hg1 N2 C10 C9 -167.1(3) . . . . ? C6 N2 C10 C11 179.4(3) . . . . ? Hg1 N2 C10 C11 13.3(4) . . . . ? C8 C9 C10 N2 0.8(5) . . . . ? C8 C9 C10 C11 -179.6(3) . . . . ? C12 C11 C10 N2 -133.4(4) . . . . ? C16 C11 C10 N2 45.2(5) . . . . ? C12 C11 C10 C9 47.0(5) . . . . ? C16 C11 C10 C9 -134.3(4) . . . . ? C18 C17 C22 C21 -0.5(5) . . . . ? C8 C17 C22 C21 178.8(3) . . . . ? C10 N2 C6 C7 0.6(5) . . . . ? Hg1 N2 C6 C7 167.6(2) . . . . ? C10 N2 C6 C5 -178.3(3) . . . . ? Hg1 N2 C6 C5 -11.2(4) . . . . ? C8 C7 C6 N2 0.1(5) . . . . ? C8 C7 C6 C5 178.9(3) . . . . ? N1 C5 C6 N2 13.7(4) . . . . ? C4 C5 C6 N2 -166.6(3) . . . . ? N1 C5 C6 C7 -165.2(3) . . . . ? C4 C5 C6 C7 14.6(5) . . . . ? C10 C9 C8 C7 -0.2(5) . . . . ? C10 C9 C8 C17 -180.0(3) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C6 C7 C8 C17 179.5(3) . . . . ? C18 C17 C8 C9 157.0(4) . . . . ? C22 C17 C8 C9 -22.4(5) . . . . ? C18 C17 C8 C7 -22.8(5) . . . . ? C22 C17 C8 C7 157.8(3) . . . . ? C20 C19 C18 C17 -1.1(6) . . . . ? C22 C17 C18 C19 1.3(5) . . . . ? C8 C17 C18 C19 -178.0(3) . . . . ? C12 C11 C16 C15 1.7(6) . . . . ? C10 C11 C16 C15 -177.0(4) . . . . ? C16 C11 C12 C13 -1.9(6) . . . . ? C10 C11 C12 C13 176.8(4) . . . . ? C11 C16 C15 C14 0.5(7) . . . . ? C16 C15 C14 C13 -2.6(8) . . . . ? C15 C14 C13 C12 2.4(8) . . . . ? C11 C12 C13 C14 -0.1(8) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C18 C19 C20 N3 179.1(3) . . . . ? C17 C22 C21 C20 -0.5(6) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? N3 C20 C21 C22 -178.4(3) . . . . ? C24 C23 N3 N4 -0.4(6) . . . . ? C24 C23 N3 C20 -179.9(4) . . . . ? C19 C20 N3 C23 19.2(6) . . . . ? C21 C20 N3 C23 -161.8(5) . . . . ? C19 C20 N3 N4 -160.2(3) . . . . ? C21 C20 N3 N4 18.8(5) . . . . ? C23 N3 N4 C25 0.5(5) . . . . ? C20 N3 N4 C25 -180.0(3) . . . . ? N3 N4 C25 C24 -0.4(5) . . . . ? N3 C23 C24 C25 0.1(7) . . . . ? N4 C25 C24 C23 0.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.867 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.088 data_jf _database_code_depnum_ccdc_archive 'CCDC 854404' #TrackingRef 'jf.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Br2 Hg N4' _chemical_formula_weight 734.84 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 ' 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 17.794(5) _cell_length_b 18.670(5) _cell_length_c 14.665(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 96.751(5) _cell_angle_gamma 90.000(5) _cell_volume 4838(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4265 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 18.72 _exptl_crystal_description Neddle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 9.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1592 _exptl_absorpt_correction_T_max 0.4442 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34120 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8517 _reflns_number_gt 4838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0355P)^2^+11.7377P] 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 SHELXL _refine_ls_extinction_coef 0.00004(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8517 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.000 _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 Hg1 Hg 0.44434(2) 0.16774(2) 0.61484(3) 0.06273(15) Uani 1 1 d . . . Hg2 Hg 0.03716(2) 0.45419(2) 0.72308(3) 0.07343(17) Uani 1 1 d . . . Br3 Br -0.03720(7) 0.53230(6) 0.81914(10) 0.0955(4) Uani 1 1 d . . . Br4 Br 0.10738(8) 0.48493(6) 0.59140(9) 0.0927(4) Uani 1 1 d . . . Br1 Br 0.52902(6) 0.15353(7) 0.76279(8) 0.0848(4) Uani 1 1 d . . . Br2 Br 0.46236(9) 0.20825(8) 0.45951(9) 0.1062(5) Uani 1 1 d . . . C10 C 0.1780(5) 0.3549(5) 0.8335(6) 0.048(2) Uani 1 1 d . . . N6 N 0.3095(4) 0.1993(3) 0.6253(4) 0.0415(17) Uani 1 1 d . . . C31 C 0.2620(5) 0.1423(4) 0.6083(6) 0.041(2) Uani 1 1 d . . . N7 N -0.1543(4) 0.2672(4) 0.4130(6) 0.063(2) Uani 1 1 d . . . C41 C 0.3161(5) 0.3957(5) 0.6048(6) 0.053(2) Uani 1 1 d . . . H41 H 0.2742 0.4021 0.5612 0.063 Uiso 1 1 calc R . . C11 C 0.2094(5) 0.4264(4) 0.8596(6) 0.051(2) Uani 1 1 d . . . N2 N 0.1053(4) 0.3520(4) 0.7929(5) 0.0497(19) Uani 1 1 d . . . C48 C -0.2060(5) 0.2156(5) 0.4068(9) 0.087(4) Uani 1 1 d . . . H48 H -0.1980 0.1677 0.4227 0.104 Uiso 1 1 calc R . . C38 C 0.4404(5) 0.3790(5) 0.7345(7) 0.064(3) Uani 1 1 d . . . H38 H 0.4824 0.3734 0.7780 0.077 Uiso 1 1 calc R . . C12 C 0.2832(6) 0.4441(5) 0.8488(7) 0.071(3) Uani 1 1 d . . . H12 H 0.3136 0.4101 0.8247 0.085 Uiso 1 1 calc R . . C7 C 0.1135(5) 0.2242(5) 0.7888(6) 0.052(2) Uani 1 1 d . . . H7 H 0.0905 0.1805 0.7731 0.062 Uiso 1 1 calc R . . C4 C -0.0526(6) 0.2257(5) 0.7160(7) 0.062(3) Uani 1 1 d . . . H4 H -0.0310 0.1813 0.7311 0.075 Uiso 1 1 calc R . . C35 C 0.2799(5) 0.2657(4) 0.6166(5) 0.040(2) Uani 1 1 d . . . C3 C -0.1280(6) 0.2299(6) 0.6802(8) 0.079(3) Uani 1 1 d . . . H3 H -0.1570 0.1885 0.6714 0.095 Uiso 1 1 calc R . . C36 C 0.3317(5) 0.3278(4) 0.6425(6) 0.040(2) Uani 1 1 d . . . C42 C 0.0749(5) 0.2319(4) 0.5232(5) 0.039(2) Uani 1 1 d . . . C32 C 0.1862(5) 0.1516(4) 0.5779(5) 0.044(2) Uani 1 1 d . . . H32 H 0.1554 0.1115 0.5676 0.053 Uiso 1 1 calc R . . N8 N -0.1882(6) 0.3312(5) 0.3836(8) 0.115(4) Uani 1 1 d . . . C46 C -0.0292(5) 0.3121(5) 0.4723(7) 0.056(3) Uani 1 1 d . . . H46 H -0.0465 0.3589 0.4640 0.068 Uiso 1 1 calc R . . C33 C 0.1544(4) 0.2201(4) 0.5620(5) 0.0360(19) Uani 1 1 d . . . C28 C 0.2862(7) -0.0538(5) 0.6648(8) 0.082(4) Uani 1 1 d . . . H28 H 0.2583 -0.0927 0.6821 0.098 Uiso 1 1 calc R . . C16 C 0.1657(6) 0.4782(5) 0.8972(6) 0.058(3) Uani 1 1 d . . . H16 H 0.1160 0.4681 0.9065 0.070 Uiso 1 1 calc R . . N1 N -0.0410(5) 0.3514(4) 0.7047(6) 0.068(2) Uani 1 1 d . . . C45 C -0.0781(5) 0.2557(4) 0.4484(6) 0.048(2) Uani 1 1 d . . . C26 C 0.4013(6) -0.0029(6) 0.6351(8) 0.083(4) Uani 1 1 d . . . H26 H 0.4530 -0.0076 0.6326 0.100 Uiso 1 1 calc R . . C39 C 0.4235(6) 0.4450(5) 0.6963(7) 0.060(3) Uani 1 1 d . . . H39 H 0.4539 0.4841 0.7145 0.072 Uiso 1 1 calc R . . C34 C 0.2040(5) 0.2768(4) 0.5863(6) 0.043(2) Uani 1 1 d . . . H34 H 0.1856 0.3234 0.5821 0.051 Uiso 1 1 calc R . . C30 C 0.2953(5) 0.0703(4) 0.6250(6) 0.045(2) Uani 1 1 d . . . N5 N 0.3691(4) 0.0619(4) 0.6185(5) 0.055(2) Uani 1 1 d . . . C37 C 0.3950(5) 0.3209(5) 0.7083(6) 0.052(2) Uani 1 1 d . . . H37 H 0.4067 0.2764 0.7347 0.062 Uiso 1 1 calc R . . C5 C -0.0088(5) 0.2876(5) 0.7295(6) 0.048(2) Uani 1 1 d . . . C40 C 0.3620(6) 0.4536(5) 0.6315(7) 0.063(3) Uani 1 1 d . . . H40 H 0.3511 0.4984 0.6055 0.075 Uiso 1 1 calc R . . C44 C -0.0495(5) 0.1862(5) 0.4602(6) 0.051(2) Uani 1 1 d . . . H44 H -0.0809 0.1473 0.4436 0.061 Uiso 1 1 calc R . . C6 C 0.0723(5) 0.2880(5) 0.7707(6) 0.051(2) Uani 1 1 d . . . C14 C 0.2700(7) 0.5618(7) 0.9092(8) 0.087(4) Uani 1 1 d . . . H14 H 0.2900 0.6066 0.9257 0.104 Uiso 1 1 calc R . . C47 C 0.0440(5) 0.3000(5) 0.5080(6) 0.054(2) Uani 1 1 d . . . H47 H 0.0750 0.3394 0.5229 0.065 Uiso 1 1 calc R . . C29 C 0.2522(5) 0.0116(5) 0.6486(6) 0.056(3) Uani 1 1 d . . . H29 H 0.2009 0.0171 0.6532 0.067 Uiso 1 1 calc R . . C2 C -0.1593(7) 0.2940(7) 0.6582(9) 0.094(4) Uani 1 1 d . . . H2 H -0.2100 0.2974 0.6346 0.113 Uiso 1 1 calc R . . C15 C 0.1970(7) 0.5459(5) 0.9209(7) 0.075(3) Uani 1 1 d . . . H15 H 0.1673 0.5804 0.9451 0.091 Uiso 1 1 calc R . . C43 C 0.0246(5) 0.1744(4) 0.4962(6) 0.048(2) Uani 1 1 d . . . H43 H 0.0422 0.1276 0.5029 0.058 Uiso 1 1 calc R . . C50 C -0.2634(6) 0.3155(7) 0.3574(11) 0.121(6) Uani 1 1 d . . . H50 H -0.3014 0.3468 0.3334 0.145 Uiso 1 1 calc R . . C49 C -0.2697(7) 0.2448(7) 0.3742(13) 0.153(8) Uani 1 1 d . . . H49 H -0.3150 0.2197 0.3636 0.184 Uiso 1 1 calc R . . C27 C 0.3614(6) -0.0616(5) 0.6554(9) 0.091(4) Uani 1 1 d . . . H27 H 0.3846 -0.1062 0.6628 0.109 Uiso 1 1 calc R . . C8 C 0.1889(5) 0.2255(5) 0.8300(6) 0.051(2) Uani 1 1 d . . . C13 C 0.3136(7) 0.5109(6) 0.8729(8) 0.089(4) Uani 1 1 d . . . H13 H 0.3634 0.5212 0.8643 0.107 Uiso 1 1 calc R . . C1 C -0.1153(7) 0.3543(7) 0.6710(9) 0.098(4) Uani 1 1 d . . . H1 H -0.1370 0.3987 0.6560 0.117 Uiso 1 1 calc R . . C9 C 0.2196(5) 0.2924(5) 0.8516(6) 0.050(2) Uani 1 1 d . . . H9 H 0.2693 0.2956 0.8790 0.060 Uiso 1 1 calc R . . C17 C 0.2312(5) 0.1575(4) 0.8499(6) 0.047(2) Uani 1 1 d . . . C18 C 0.3094(5) 0.1552(5) 0.8507(6) 0.056(3) Uani 1 1 d . . . H18 H 0.3358 0.1965 0.8388 0.067 Uiso 1 1 calc R . . C22 C 0.1944(5) 0.0951(5) 0.8695(6) 0.058(3) Uani 1 1 d . . . H22 H 0.1421 0.0958 0.8695 0.069 Uiso 1 1 calc R . . C20 C 0.3109(6) 0.0297(5) 0.8895(6) 0.053(2) Uani 1 1 d . . . C19 C 0.3481(5) 0.0915(5) 0.8690(6) 0.055(2) Uani 1 1 d . . . H19 H 0.4002 0.0904 0.8676 0.066 Uiso 1 1 calc R . . C21 C 0.2332(6) 0.0316(5) 0.8893(6) 0.058(3) Uani 1 1 d . . . H21 H 0.2071 -0.0096 0.9023 0.069 Uiso 1 1 calc R . . N3 N 0.3498(5) -0.0356(5) 0.9089(6) 0.066(2) Uani 1 1 d . . . N4 N 0.4262(7) -0.0440(6) 0.9241(8) 0.122(4) Uani 1 1 d . . . C23 C 0.3166(6) -0.0960(6) 0.9190(10) 0.100(5) Uani 1 1 d . . . H23 H 0.2648 -0.1046 0.9104 0.120 Uiso 1 1 calc R . . C24 C 0.3693(9) -0.1421(7) 0.9432(11) 0.121(5) Uani 1 1 d . . . H24 H 0.3598 -0.1895 0.9579 0.146 Uiso 1 1 calc R . . C25 C 0.4390(7) -0.1145(6) 0.9451(9) 0.089(4) Uani 1 1 d . . . H25 H 0.4852 -0.1379 0.9577 0.107 Uiso 1 1 calc R . . 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 Hg1 0.0514(3) 0.0675(3) 0.0683(3) 0.0060(2) 0.0031(2) 0.0017(2) Hg2 0.0696(3) 0.0581(3) 0.0921(4) -0.0027(2) 0.0075(2) 0.0155(2) Br3 0.0735(8) 0.0831(8) 0.1305(11) -0.0294(8) 0.0140(8) 0.0230(6) Br4 0.1282(11) 0.0515(6) 0.1019(9) 0.0033(6) 0.0290(8) -0.0070(7) Br1 0.0576(7) 0.1006(9) 0.0892(8) 0.0069(7) -0.0204(6) 0.0076(6) Br2 0.1344(12) 0.1193(11) 0.0669(8) 0.0068(8) 0.0202(8) -0.0174(9) C10 0.057(6) 0.058(6) 0.030(5) -0.003(4) 0.012(5) 0.002(5) N6 0.039(4) 0.042(4) 0.043(4) 0.007(3) 0.003(3) 0.003(3) C31 0.034(5) 0.036(5) 0.052(6) -0.005(4) 0.008(4) -0.008(4) N7 0.035(5) 0.048(5) 0.102(7) -0.009(4) -0.008(4) 0.010(4) C41 0.054(6) 0.053(6) 0.046(6) 0.007(5) -0.011(5) -0.006(5) C11 0.059(7) 0.041(5) 0.053(6) -0.008(5) 0.008(5) 0.003(5) N2 0.050(5) 0.047(4) 0.054(5) -0.004(4) 0.013(4) 0.000(4) C48 0.018(5) 0.022(5) 0.214(14) -0.002(6) -0.015(7) -0.010(4) C38 0.046(6) 0.064(7) 0.079(8) 0.008(6) -0.008(5) -0.013(5) C12 0.058(7) 0.064(7) 0.092(8) -0.020(6) 0.012(6) -0.009(6) C7 0.056(7) 0.046(5) 0.057(6) -0.005(5) 0.018(5) 0.003(5) C4 0.053(7) 0.057(6) 0.077(7) -0.011(5) 0.007(6) -0.005(5) C35 0.038(5) 0.047(5) 0.034(5) 0.007(4) 0.007(4) -0.002(4) C3 0.054(8) 0.080(8) 0.102(9) -0.021(7) 0.005(7) -0.012(6) C36 0.038(5) 0.035(5) 0.046(5) 0.003(4) 0.005(4) -0.011(4) C42 0.041(5) 0.039(5) 0.038(5) -0.006(4) 0.006(4) -0.003(4) C32 0.045(6) 0.039(5) 0.047(5) 0.001(4) 0.004(4) -0.008(4) N8 0.091(8) 0.086(7) 0.161(11) -0.017(7) -0.022(7) 0.025(6) C46 0.035(6) 0.040(5) 0.089(8) -0.004(5) -0.013(5) -0.001(4) C33 0.034(5) 0.036(5) 0.037(5) -0.003(4) 0.002(4) -0.003(4) C28 0.083(9) 0.038(6) 0.114(10) 0.017(6) -0.032(7) -0.018(6) C16 0.063(7) 0.060(6) 0.051(6) 0.002(5) 0.005(5) 0.004(5) N1 0.062(6) 0.056(5) 0.085(6) -0.010(5) 0.002(5) 0.015(4) C45 0.045(6) 0.043(5) 0.055(6) -0.001(4) 0.003(5) 0.004(5) C26 0.055(7) 0.060(7) 0.126(10) 0.004(7) -0.022(7) 0.009(6) C39 0.063(7) 0.056(6) 0.061(7) 0.000(5) 0.004(6) -0.033(5) C34 0.048(6) 0.032(5) 0.050(6) 0.002(4) 0.010(5) 0.001(4) C30 0.047(6) 0.036(5) 0.049(6) -0.002(4) 0.001(5) 0.002(4) N5 0.038(5) 0.045(5) 0.077(6) 0.004(4) -0.007(4) 0.002(4) C37 0.043(6) 0.047(5) 0.065(6) 0.006(5) -0.001(5) -0.012(4) C5 0.036(6) 0.060(6) 0.050(6) -0.010(5) 0.011(5) -0.001(5) C40 0.075(8) 0.045(6) 0.066(7) 0.010(5) 0.001(6) -0.014(5) C44 0.040(6) 0.048(6) 0.064(6) -0.006(5) 0.000(5) -0.011(4) C6 0.049(6) 0.057(6) 0.047(6) -0.018(5) 0.012(5) -0.001(5) C14 0.083(9) 0.085(9) 0.093(9) -0.008(7) 0.009(8) -0.025(8) C47 0.047(6) 0.042(5) 0.072(7) -0.007(5) 0.000(5) -0.006(4) C29 0.045(6) 0.044(5) 0.075(7) 0.005(5) -0.008(5) -0.004(5) C2 0.058(8) 0.086(9) 0.135(12) -0.021(9) -0.003(7) 0.005(7) C15 0.111(10) 0.041(6) 0.073(8) -0.011(5) 0.008(7) 0.005(6) C43 0.045(6) 0.036(5) 0.062(6) 0.000(4) 0.000(5) 0.000(4) C50 0.023(6) 0.086(10) 0.241(18) -0.046(10) -0.037(8) 0.010(6) C49 0.042(8) 0.062(9) 0.34(3) -0.033(11) -0.031(11) 0.000(7) C27 0.052(8) 0.046(7) 0.161(12) -0.006(7) -0.039(8) 0.006(6) C8 0.052(6) 0.063(6) 0.039(6) 0.009(5) 0.010(5) -0.001(5) C13 0.096(10) 0.073(8) 0.101(9) -0.029(7) 0.025(8) -0.028(7) C1 0.056(8) 0.084(9) 0.149(12) 0.005(8) -0.005(8) 0.031(7) C9 0.049(6) 0.057(6) 0.044(6) -0.004(5) 0.009(5) 0.002(5) C17 0.057(7) 0.043(5) 0.039(5) 0.003(4) 0.001(5) -0.005(5) C18 0.051(6) 0.055(6) 0.065(7) 0.010(5) 0.015(5) 0.003(5) C22 0.042(6) 0.066(7) 0.064(7) -0.009(5) -0.002(5) 0.005(5) C20 0.056(7) 0.056(6) 0.047(6) -0.007(5) 0.006(5) 0.003(5) C19 0.040(6) 0.076(7) 0.048(6) 0.010(5) 0.007(5) 0.007(5) C21 0.063(7) 0.045(6) 0.064(7) -0.003(5) 0.004(5) -0.006(5) N3 0.052(6) 0.071(6) 0.071(6) 0.000(5) 0.001(5) 0.025(5) N4 0.095(9) 0.122(10) 0.149(11) 0.003(8) 0.015(8) 0.038(7) C23 0.038(7) 0.054(7) 0.200(15) 0.045(8) -0.013(8) 0.002(6) C24 0.092(11) 0.066(8) 0.205(17) 0.037(9) 0.011(11) 0.004(8) C25 0.078(9) 0.068(8) 0.125(11) 0.027(7) 0.026(8) 0.039(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N5 2.391(7) . ? Hg1 Br2 2.4568(15) . ? Hg1 N6 2.493(6) . ? Hg1 Br1 2.5060(13) . ? Hg2 N1 2.367(8) . ? Hg2 N2 2.422(7) . ? Hg2 Br4 2.4873(15) . ? Hg2 Br3 2.5099(13) . ? C10 N2 1.359(10) . ? C10 C9 1.392(11) . ? C10 C11 1.481(12) . ? N6 C35 1.348(9) . ? N6 C31 1.363(9) . ? C31 C32 1.381(11) . ? C31 C30 1.477(11) . ? N7 C48 1.328(10) . ? N7 N8 1.385(11) . ? N7 C45 1.410(10) . ? C41 C40 1.383(12) . ? C41 C36 1.398(11) . ? C41 H41 0.9300 . ? C11 C12 1.381(12) . ? C11 C16 1.393(12) . ? N2 C6 1.355(10) . ? C48 C49 1.298(14) . ? C48 H48 0.9300 . ? C38 C39 1.371(12) . ? C38 C37 1.378(11) . ? C38 H38 0.9300 . ? C12 C13 1.388(13) . ? C12 H12 0.9300 . ? C7 C6 1.407(12) . ? C7 C8 1.407(12) . ? C7 H7 0.9300 . ? C4 C3 1.385(13) . ? C4 C5 1.394(12) . ? C4 H4 0.9300 . ? C35 C34 1.386(11) . ? C35 C36 1.502(10) . ? C3 C2 1.342(14) . ? C3 H3 0.9300 . ? C36 C37 1.401(11) . ? C42 C47 1.393(11) . ? C42 C43 1.424(10) . ? C42 C33 1.478(11) . ? C32 C33 1.407(10) . ? C32 H32 0.9300 . ? N8 C50 1.380(13) . ? C46 C47 1.365(11) . ? C46 C45 1.385(11) . ? C46 H46 0.9300 . ? C33 C34 1.398(10) . ? C28 C27 1.368(14) . ? C28 C29 1.372(12) . ? C28 H28 0.9300 . ? C16 C15 1.408(12) . ? C16 H16 0.9300 . ? N1 C1 1.356(12) . ? N1 C5 1.354(11) . ? C45 C44 1.397(11) . ? C26 C27 1.359(14) . ? C26 N5 1.348(11) . ? C26 H26 0.9300 . ? C39 C40 1.372(12) . ? C39 H39 0.9300 . ? C34 H34 0.9300 . ? C30 N5 1.338(10) . ? C30 C29 1.403(11) . ? C37 H37 0.9300 . ? C5 C6 1.497(12) . ? C40 H40 0.9300 . ? C44 C43 1.379(11) . ? C44 H44 0.9300 . ? C14 C15 1.362(14) . ? C14 C13 1.373(15) . ? C14 H14 0.9300 . ? C47 H47 0.9300 . ? C29 H29 0.9300 . ? C2 C1 1.372(15) . ? C2 H2 0.9300 . ? C15 H15 0.9300 . ? C43 H43 0.9300 . ? C50 C49 1.350(16) . ? C50 H50 0.9300 . ? C49 H49 0.9300 . ? C27 H27 0.9300 . ? C8 C9 1.384(12) . ? C8 C17 1.487(12) . ? C13 H13 0.9300 . ? C1 H1 0.9300 . ? C9 H9 0.9300 . ? C17 C22 1.383(12) . ? C17 C18 1.392(12) . ? C18 C19 1.383(11) . ? C18 H18 0.9300 . ? C22 C21 1.386(12) . ? C22 H22 0.9300 . ? C20 C21 1.382(12) . ? C20 C19 1.381(12) . ? C20 N3 1.414(11) . ? C19 H19 0.9300 . ? C21 H21 0.9300 . ? N3 C23 1.289(12) . ? N3 N4 1.360(12) . ? N4 C25 1.365(13) . ? C23 C24 1.292(14) . ? C23 H23 0.9300 . ? C24 C25 1.342(15) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 N5 Hg1 Br2 114.17(19) . . ? N5 Hg1 N6 69.4(2) . . ? Br2 Hg1 N6 102.45(15) . . ? N5 Hg1 Br1 100.05(18) . . ? Br2 Hg1 Br1 134.80(5) . . ? N6 Hg1 Br1 117.21(15) . . ? N1 Hg2 N2 70.6(3) . . ? N1 Hg2 Br4 116.2(2) . . ? N2 Hg2 Br4 103.76(16) . . ? N1 Hg2 Br3 101.2(2) . . ? N2 Hg2 Br3 119.40(17) . . ? Br4 Hg2 Br3 130.37(5) . . ? N2 C10 C9 120.5(8) . . ? N2 C10 C11 117.4(8) . . ? C9 C10 C11 122.1(9) . . ? C35 N6 C31 118.3(7) . . ? C35 N6 Hg1 125.4(5) . . ? C31 N6 Hg1 112.6(5) . . ? N6 C31 C32 121.4(7) . . ? N6 C31 C30 116.9(7) . . ? C32 C31 C30 121.7(7) . . ? C48 N7 N8 109.4(8) . . ? C48 N7 C45 122.9(8) . . ? N8 N7 C45 127.7(8) . . ? C40 C41 C36 120.9(8) . . ? C40 C41 H41 119.5 . . ? C36 C41 H41 119.5 . . ? C12 C11 C16 117.5(9) . . ? C12 C11 C10 121.4(8) . . ? C16 C11 C10 121.1(9) . . ? C10 N2 C6 120.2(7) . . ? C10 N2 Hg2 123.8(6) . . ? C6 N2 Hg2 114.3(6) . . ? C49 C48 N7 106.7(9) . . ? C49 C48 H48 126.6 . . ? N7 C48 H48 126.6 . . ? C39 C38 C37 120.0(9) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C13 C12 C11 122.2(10) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C6 C7 C8 121.1(8) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C3 C4 C5 120.5(10) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N6 C35 C34 121.5(7) . . ? N6 C35 C36 117.8(7) . . ? C34 C35 C36 120.7(7) . . ? C2 C3 C4 119.9(10) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C41 C36 C37 117.5(7) . . ? C41 C36 C35 120.9(7) . . ? C37 C36 C35 121.6(7) . . ? C47 C42 C43 114.9(8) . . ? C47 C42 C33 122.6(7) . . ? C43 C42 C33 122.5(7) . . ? C31 C32 C33 121.8(7) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? N7 N8 C50 106.1(10) . . ? C47 C46 C45 121.0(8) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C34 C33 C32 114.6(7) . . ? C34 C33 C42 122.2(7) . . ? C32 C33 C42 123.2(7) . . ? C27 C28 C29 119.6(10) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C11 C16 C15 119.9(10) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C1 N1 C5 119.8(9) . . ? C1 N1 Hg2 122.9(7) . . ? C5 N1 Hg2 117.3(6) . . ? C46 C45 N7 121.7(8) . . ? C46 C45 C44 117.8(8) . . ? N7 C45 C44 120.5(8) . . ? C27 C26 N5 122.8(10) . . ? C27 C26 H26 118.6 . . ? N5 C26 H26 118.6 . . ? C38 C39 C40 120.5(8) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C35 C34 C33 122.1(7) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? N5 C30 C29 119.7(7) . . ? N5 C30 C31 118.2(7) . . ? C29 C30 C31 122.1(8) . . ? C30 N5 C26 119.5(8) . . ? C30 N5 Hg1 117.5(5) . . ? C26 N5 Hg1 121.2(6) . . ? C38 C37 C36 121.1(8) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? N1 C5 C4 118.6(8) . . ? N1 C5 C6 117.5(8) . . ? C4 C5 C6 123.9(9) . . ? C41 C40 C39 120.0(9) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C43 C44 C45 120.8(8) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? N2 C6 C7 120.0(8) . . ? N2 C6 C5 118.2(8) . . ? C7 C6 C5 121.9(8) . . ? C15 C14 C13 119.3(11) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C46 C47 C42 123.6(8) . . ? C46 C47 H47 118.2 . . ? C42 C47 H47 118.2 . . ? C28 C29 C30 119.8(9) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C3 C2 C1 119.0(11) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C14 C15 C16 121.3(10) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C44 C43 C42 121.9(8) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C49 C50 N8 104.8(10) . . ? C49 C50 H50 127.6 . . ? N8 C50 H50 127.6 . . ? C48 C49 C50 113.0(10) . . ? C48 C49 H49 123.5 . . ? C50 C49 H49 123.5 . . ? C26 C27 C28 118.6(10) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C9 C8 C7 116.4(8) . . ? C9 C8 C17 123.3(8) . . ? C7 C8 C17 120.3(8) . . ? C12 C13 C14 119.9(11) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N1 C1 C2 122.2(11) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C8 C9 C10 121.7(9) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C22 C17 C18 118.0(8) . . ? C22 C17 C8 121.3(8) . . ? C18 C17 C8 120.7(8) . . ? C19 C18 C17 120.2(9) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C17 C22 C21 121.8(9) . . ? C17 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C21 C20 C19 118.8(9) . . ? C21 C20 N3 119.3(9) . . ? C19 C20 N3 121.9(9) . . ? C18 C19 C20 121.4(9) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C20 C21 C22 119.8(9) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 N3 N4 110.1(9) . . ? C23 N3 C20 123.8(9) . . ? N4 N3 C20 126.1(10) . . ? N3 N4 C25 106.6(11) . . ? N3 C23 C24 106.7(10) . . ? N3 C23 H23 126.7 . . ? C24 C23 H23 126.7 . . ? C23 C24 C25 112.9(12) . . ? C23 C24 H24 123.5 . . ? C25 C24 H24 123.5 . . ? N4 C25 C24 103.6(11) . . ? N4 C25 H25 128.2 . . ? C24 C25 H25 128.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Hg1 N6 C35 -170.9(7) . . . . ? Br2 Hg1 N6 C35 -59.5(6) . . . . ? Br1 Hg1 N6 C35 98.1(6) . . . . ? N5 Hg1 N6 C31 -12.9(5) . . . . ? Br2 Hg1 N6 C31 98.5(5) . . . . ? Br1 Hg1 N6 C31 -103.8(5) . . . . ? C35 N6 C31 C32 3.7(12) . . . . ? Hg1 N6 C31 C32 -156.1(6) . . . . ? C35 N6 C31 C30 -175.6(7) . . . . ? Hg1 N6 C31 C30 24.6(9) . . . . ? N2 C10 C11 C12 -140.9(9) . . . . ? C9 C10 C11 C12 40.9(13) . . . . ? N2 C10 C11 C16 39.9(12) . . . . ? C9 C10 C11 C16 -138.2(9) . . . . ? C9 C10 N2 C6 0.8(12) . . . . ? C11 C10 N2 C6 -177.4(7) . . . . ? C9 C10 N2 Hg2 -164.0(6) . . . . ? C11 C10 N2 Hg2 17.9(10) . . . . ? N1 Hg2 N2 C10 178.3(7) . . . . ? Br4 Hg2 N2 C10 65.0(6) . . . . ? Br3 Hg2 N2 C10 -89.6(6) . . . . ? N1 Hg2 N2 C6 12.7(6) . . . . ? Br4 Hg2 N2 C6 -100.6(6) . . . . ? Br3 Hg2 N2 C6 104.8(5) . . . . ? N8 N7 C48 C49 0.6(16) . . . . ? C45 N7 C48 C49 178.1(12) . . . . ? C16 C11 C12 C13 -0.9(15) . . . . ? C10 C11 C12 C13 179.9(10) . . . . ? C31 N6 C35 C34 -3.6(12) . . . . ? Hg1 N6 C35 C34 153.4(6) . . . . ? C31 N6 C35 C36 175.4(7) . . . . ? Hg1 N6 C35 C36 -27.7(10) . . . . ? C5 C4 C3 C2 0.1(16) . . . . ? C40 C41 C36 C37 0.3(13) . . . . ? C40 C41 C36 C35 177.3(8) . . . . ? N6 C35 C36 C41 155.4(8) . . . . ? C34 C35 C36 C41 -25.7(12) . . . . ? N6 C35 C36 C37 -27.8(12) . . . . ? C34 C35 C36 C37 151.1(8) . . . . ? N6 C31 C32 C33 0.7(13) . . . . ? C30 C31 C32 C33 179.9(8) . . . . ? C48 N7 N8 C50 -1.1(14) . . . . ? C45 N7 N8 C50 -178.5(11) . . . . ? C31 C32 C33 C34 -4.8(12) . . . . ? C31 C32 C33 C42 175.5(8) . . . . ? C47 C42 C33 C34 0.3(12) . . . . ? C43 C42 C33 C34 178.4(8) . . . . ? C47 C42 C33 C32 179.9(8) . . . . ? C43 C42 C33 C32 -2.0(12) . . . . ? C12 C11 C16 C15 1.1(14) . . . . ? C10 C11 C16 C15 -179.7(8) . . . . ? N2 Hg2 N1 C1 171.9(9) . . . . ? Br4 Hg2 N1 C1 -91.9(9) . . . . ? Br3 Hg2 N1 C1 54.5(9) . . . . ? N2 Hg2 N1 C5 -8.1(6) . . . . ? Br4 Hg2 N1 C5 88.1(7) . . . . ? Br3 Hg2 N1 C5 -125.5(6) . . . . ? C47 C46 C45 N7 178.9(9) . . . . ? C47 C46 C45 C44 -1.3(14) . . . . ? C48 N7 C45 C46 -166.1(10) . . . . ? N8 N7 C45 C46 10.9(16) . . . . ? C48 N7 C45 C44 14.1(15) . . . . ? N8 N7 C45 C44 -168.8(10) . . . . ? C37 C38 C39 C40 -0.5(15) . . . . ? N6 C35 C34 C33 -0.9(12) . . . . ? C36 C35 C34 C33 -179.8(7) . . . . ? C32 C33 C34 C35 5.0(11) . . . . ? C42 C33 C34 C35 -175.4(7) . . . . ? N6 C31 C30 N5 -26.8(12) . . . . ? C32 C31 C30 N5 153.9(8) . . . . ? N6 C31 C30 C29 152.2(8) . . . . ? C32 C31 C30 C29 -27.1(13) . . . . ? C29 C30 N5 C26 -0.4(13) . . . . ? C31 C30 N5 C26 178.7(9) . . . . ? C29 C30 N5 Hg1 -165.3(6) . . . . ? C31 C30 N5 Hg1 13.8(10) . . . . ? C27 C26 N5 C30 2.4(17) . . . . ? C27 C26 N5 Hg1 166.8(9) . . . . ? Br2 Hg1 N5 C30 -95.5(6) . . . . ? N6 Hg1 N5 C30 -0.7(6) . . . . ? Br1 Hg1 N5 C30 114.7(6) . . . . ? Br2 Hg1 N5 C26 99.8(8) . . . . ? N6 Hg1 N5 C26 -165.4(9) . . . . ? Br1 Hg1 N5 C26 -49.9(8) . . . . ? C39 C38 C37 C36 0.4(14) . . . . ? C41 C36 C37 C38 -0.3(13) . . . . ? C35 C36 C37 C38 -177.2(8) . . . . ? C1 N1 C5 C4 2.6(14) . . . . ? Hg2 N1 C5 C4 -177.4(6) . . . . ? C1 N1 C5 C6 -177.0(9) . . . . ? Hg2 N1 C5 C6 3.0(10) . . . . ? C3 C4 C5 N1 -1.7(14) . . . . ? C3 C4 C5 C6 177.8(9) . . . . ? C36 C41 C40 C39 -0.5(14) . . . . ? C38 C39 C40 C41 0.6(15) . . . . ? C46 C45 C44 C43 1.2(14) . . . . ? N7 C45 C44 C43 -179.0(8) . . . . ? C10 N2 C6 C7 -0.7(12) . . . . ? Hg2 N2 C6 C7 165.5(6) . . . . ? C10 N2 C6 C5 177.7(7) . . . . ? Hg2 N2 C6 C5 -16.1(9) . . . . ? C8 C7 C6 N2 0.2(13) . . . . ? C8 C7 C6 C5 -178.1(8) . . . . ? N1 C5 C6 N2 9.3(12) . . . . ? C4 C5 C6 N2 -170.3(8) . . . . ? N1 C5 C6 C7 -172.4(8) . . . . ? C4 C5 C6 C7 8.1(13) . . . . ? C45 C46 C47 C42 -0.2(15) . . . . ? C43 C42 C47 C46 1.8(13) . . . . ? C33 C42 C47 C46 -180.0(9) . . . . ? C27 C28 C29 C30 -1.7(16) . . . . ? N5 C30 C29 C28 0.1(14) . . . . ? C31 C30 C29 C28 -179.0(9) . . . . ? C4 C3 C2 C1 0.6(19) . . . . ? C13 C14 C15 C16 0.5(18) . . . . ? C11 C16 C15 C14 -1.0(15) . . . . ? C45 C44 C43 C42 0.4(14) . . . . ? C47 C42 C43 C44 -1.8(12) . . . . ? C33 C42 C43 C44 179.9(8) . . . . ? N7 N8 C50 C49 1.2(17) . . . . ? N7 C48 C49 C50 0(2) . . . . ? N8 C50 C49 C48 -1(2) . . . . ? N5 C26 C27 C28 -4.1(19) . . . . ? C29 C28 C27 C26 3.7(18) . . . . ? C6 C7 C8 C9 0.1(12) . . . . ? C6 C7 C8 C17 179.0(8) . . . . ? C11 C12 C13 C14 0.5(18) . . . . ? C15 C14 C13 C12 -0.3(19) . . . . ? C5 N1 C1 C2 -2.0(18) . . . . ? Hg2 N1 C1 C2 178.0(10) . . . . ? C3 C2 C1 N1 0(2) . . . . ? C7 C8 C9 C10 0.0(12) . . . . ? C17 C8 C9 C10 -178.8(8) . . . . ? N2 C10 C9 C8 -0.5(13) . . . . ? C11 C10 C9 C8 177.6(8) . . . . ? C9 C8 C17 C22 148.7(9) . . . . ? C7 C8 C17 C22 -30.1(12) . . . . ? C9 C8 C17 C18 -30.3(13) . . . . ? C7 C8 C17 C18 150.9(9) . . . . ? C22 C17 C18 C19 1.1(13) . . . . ? C8 C17 C18 C19 -179.8(8) . . . . ? C18 C17 C22 C21 -0.2(14) . . . . ? C8 C17 C22 C21 -179.2(8) . . . . ? C17 C18 C19 C20 -1.9(14) . . . . ? C21 C20 C19 C18 1.6(14) . . . . ? N3 C20 C19 C18 -179.7(8) . . . . ? C19 C20 C21 C22 -0.7(14) . . . . ? N3 C20 C21 C22 -179.4(8) . . . . ? C17 C22 C21 C20 -0.1(14) . . . . ? C21 C20 N3 C23 6.2(15) . . . . ? C19 C20 N3 C23 -172.5(11) . . . . ? C21 C20 N3 N4 -170.3(10) . . . . ? C19 C20 N3 N4 11.0(15) . . . . ? C23 N3 N4 C25 -0.2(14) . . . . ? C20 N3 N4 C25 176.7(10) . . . . ? N4 N3 C23 C24 2.2(16) . . . . ? C20 N3 C23 C24 -174.8(11) . . . . ? N3 C23 C24 C25 -3.4(19) . . . . ? N3 N4 C25 C24 -1.7(15) . . . . ? C23 C24 C25 N4 3.2(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.946 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.128 data_jf _database_code_depnum_ccdc_archive 'CCDC 857231' #TrackingRef 'jf.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Hg I2 N4' _chemical_formula_weight 828.82 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' 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 13.334(5) _cell_length_b 26.776(5) _cell_length_c 7.767(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 100.081(5) _cell_angle_gamma 90.000(5) _cell_volume 2730(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 26.82 _exptl_crystal_description neddle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 7.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1998 _exptl_absorpt_correction_T_max 0.3004 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19252 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4809 _reflns_number_gt 4344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0934P)^2^+11.8135P] 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 4809 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _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 Hg1 Hg 0.30427(2) 0.118080(12) 1.05349(5) 0.04598(16) Uani 1 1 d . . . I2 I 0.21960(5) 0.08663(2) 1.32139(8) 0.0556(2) Uani 1 1 d . . . I1 I 0.41020(6) 0.06789(3) 0.85517(11) 0.0740(3) Uani 1 1 d . . . N1 N 0.1729(5) 0.1800(2) 0.9426(8) 0.0355(14) Uani 1 1 d . . . N3 N -0.2952(5) 0.3929(3) 0.9642(10) 0.0419(16) Uani 1 1 d . . . C11 C 0.1957(6) 0.2275(3) 0.9904(10) 0.0356(16) Uani 1 1 d . . . C20 C -0.2165(6) 0.3573(3) 0.9512(11) 0.0419(18) Uani 1 1 d . . . C9 C 0.0189(6) 0.2511(3) 0.9325(10) 0.0383(17) Uani 1 1 d . . . C13 C 0.3443(7) 0.2870(3) 1.0725(14) 0.055(2) Uani 1 1 d . . . H13 H 0.3007 0.3139 1.0414 0.066 Uiso 1 1 calc R . . C16 C 0.4680(6) 0.2086(4) 1.1578(14) 0.055(2) Uani 1 1 d . . . H16 H 0.5110 0.1814 1.1870 0.066 Uiso 1 1 calc R . . C18 C -0.1604(6) 0.2732(3) 0.9611(13) 0.048(2) Uani 1 1 d . . . H18 H -0.1735 0.2394 0.9733 0.057 Uiso 1 1 calc R . . C5 C -0.0304(6) 0.0903(3) 0.8842(12) 0.046(2) Uani 1 1 d . . . H5 H -0.0735 0.1075 0.9455 0.055 Uiso 1 1 calc R . . C14 C 0.4432(8) 0.2960(4) 1.1342(15) 0.062(3) Uani 1 1 d . . . H14 H 0.4676 0.3285 1.1464 0.075 Uiso 1 1 calc R . . C4 C -0.0498(7) 0.0411(4) 0.8381(13) 0.054(2) Uani 1 1 d . . . H4 H -0.1051 0.0249 0.8715 0.064 Uiso 1 1 calc R . . C6 C 0.0525(6) 0.1138(3) 0.8396(11) 0.0381(17) Uani 1 1 d . . . C7 C 0.0748(6) 0.1670(3) 0.8906(10) 0.0367(16) Uani 1 1 d . . . N2 N 0.3690(5) 0.2002(3) 1.0963(9) 0.0432(15) Uani 1 1 d . . . C23 C -0.3941(6) 0.3797(3) 0.9239(14) 0.047(2) Uani 1 1 d . . . H23 H -0.4207 0.3487 0.8861 0.056 Uiso 1 1 calc R . . C12 C 0.3056(5) 0.2392(3) 1.0540(9) 0.0363(17) Uani 1 1 d . . . C15 C 0.5079(7) 0.2561(4) 1.1791(13) 0.057(2) Uani 1 1 d . . . H15 H 0.5767 0.2612 1.2226 0.068 Uiso 1 1 calc R . . C21 C -0.1238(6) 0.3740(3) 0.9219(13) 0.045(2) Uani 1 1 d . . . H21 H -0.1122 0.4079 0.9082 0.054 Uiso 1 1 calc R . . C17 C -0.0638(6) 0.2879(3) 0.9342(11) 0.0393(17) Uani 1 1 d . . . C22 C -0.0463(6) 0.3388(3) 0.9129(12) 0.0437(18) Uani 1 1 d . . . H22 H 0.0170 0.3495 0.8926 0.052 Uiso 1 1 calc R . . C25 C -0.3803(7) 0.4597(4) 1.0085(15) 0.058(2) Uani 1 1 d . . . H25 H -0.3988 0.4917 1.0367 0.070 Uiso 1 1 calc R . . C10 C 0.1216(6) 0.2634(3) 0.9861(11) 0.0407(17) Uani 1 1 d . . . H10 H 0.1398 0.2960 1.0189 0.049 Uiso 1 1 calc R . . C8 C -0.0032(6) 0.2012(3) 0.8829(11) 0.0385(17) Uani 1 1 d . . . H8 H -0.0703 0.1913 0.8451 0.046 Uiso 1 1 calc R . . C3 C 0.0116(8) 0.0156(4) 0.7435(13) 0.054(2) Uani 1 1 d . . . H3 H -0.0027 -0.0174 0.7109 0.065 Uiso 1 1 calc R . . C2 C 0.0938(7) 0.0392(3) 0.6975(12) 0.051(2) Uani 1 1 d . . . H2 H 0.1360 0.0219 0.6347 0.061 Uiso 1 1 calc R . . C24 C -0.4441(7) 0.4201(4) 0.9500(16) 0.062(3) Uani 1 1 d . . . H24 H -0.5148 0.4221 0.9313 0.075 Uiso 1 1 calc R . . N4 N -0.2843(7) 0.4410(3) 1.0158(13) 0.064(2) Uani 1 1 d . . . C1 C 0.1150(7) 0.0885(3) 0.7434(11) 0.0425(18) Uani 1 1 d . . . H1 H 0.1705 0.1045 0.7103 0.051 Uiso 1 1 calc R . . C19 C -0.2358(6) 0.3067(3) 0.9700(13) 0.049(2) Uani 1 1 d . . . H19 H -0.2994 0.2960 0.9884 0.059 Uiso 1 1 calc R . . 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 Hg1 0.0424(2) 0.0415(2) 0.0547(2) 0.00306(13) 0.01055(16) 0.00471(13) I2 0.0606(4) 0.0538(4) 0.0547(4) 0.0064(3) 0.0167(3) -0.0070(3) I1 0.0634(4) 0.0768(5) 0.0861(5) -0.0134(4) 0.0254(4) 0.0177(4) N1 0.031(3) 0.037(3) 0.037(3) 0.001(3) 0.003(3) 0.003(3) N3 0.029(3) 0.033(3) 0.063(5) -0.006(3) 0.005(3) 0.002(3) C11 0.037(4) 0.035(4) 0.035(4) 0.001(3) 0.005(3) -0.001(3) C20 0.034(4) 0.040(4) 0.050(5) -0.002(4) 0.003(3) 0.002(3) C9 0.032(4) 0.039(4) 0.043(4) -0.004(3) 0.004(3) 0.005(3) C13 0.040(5) 0.039(5) 0.084(7) 0.006(4) 0.004(4) 0.001(4) C16 0.030(4) 0.054(5) 0.077(7) 0.010(5) -0.002(4) 0.002(4) C18 0.044(5) 0.030(4) 0.070(6) 0.000(4) 0.012(4) -0.002(3) C5 0.035(4) 0.045(5) 0.057(5) -0.004(4) 0.005(4) 0.000(3) C14 0.049(5) 0.047(5) 0.088(7) 0.003(5) 0.003(5) -0.011(4) C4 0.040(5) 0.048(5) 0.071(6) -0.001(4) 0.004(4) -0.011(4) C6 0.033(4) 0.043(5) 0.036(4) -0.003(3) 0.000(3) 0.000(3) C7 0.038(4) 0.032(4) 0.039(4) -0.001(3) 0.004(3) 0.001(3) N2 0.034(3) 0.041(4) 0.052(4) 0.003(3) 0.001(3) -0.002(3) C23 0.022(4) 0.036(4) 0.081(7) -0.012(4) 0.006(4) 0.000(3) C12 0.035(4) 0.037(4) 0.036(4) 0.006(3) 0.002(3) 0.002(3) C15 0.037(5) 0.062(6) 0.068(6) 0.006(5) 0.001(4) -0.012(4) C21 0.032(4) 0.031(4) 0.070(6) -0.002(4) 0.005(4) 0.001(3) C17 0.033(4) 0.036(4) 0.048(4) -0.004(3) 0.004(3) 0.002(3) C22 0.028(4) 0.041(4) 0.061(5) 0.002(4) 0.003(3) 0.002(3) C25 0.051(5) 0.042(5) 0.083(7) -0.005(5) 0.014(5) 0.012(4) C10 0.039(4) 0.033(4) 0.047(4) 0.000(3) 0.002(3) 0.001(3) C8 0.028(4) 0.040(4) 0.046(4) -0.003(3) 0.004(3) 0.003(3) C3 0.060(6) 0.041(5) 0.060(6) -0.005(4) 0.002(4) -0.003(4) C2 0.058(5) 0.042(5) 0.055(5) -0.011(4) 0.015(4) 0.006(4) C24 0.033(5) 0.058(6) 0.096(8) -0.005(5) 0.014(5) 0.007(4) N4 0.057(5) 0.050(5) 0.083(6) -0.005(4) 0.003(4) 0.004(4) C1 0.044(4) 0.043(5) 0.040(4) -0.004(3) 0.006(3) -0.003(3) C19 0.034(4) 0.041(5) 0.072(6) -0.003(4) 0.010(4) -0.002(3) _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 Hg1 N2 2.365(7) . ? Hg1 N1 2.456(6) . ? Hg1 I1 2.6336(11) . ? Hg1 I2 2.6712(13) . ? N1 C7 1.346(10) . ? N1 C11 1.346(10) . ? N3 N4 1.349(11) . ? N3 C23 1.348(10) . ? N3 C20 1.434(10) . ? C11 C10 1.374(11) . ? C11 C12 1.495(10) . ? C20 C21 1.370(12) . ? C20 C19 1.392(12) . ? C9 C10 1.399(11) . ? C9 C8 1.407(11) . ? C9 C17 1.480(11) . ? C13 C14 1.344(14) . ? C13 C12 1.378(12) . ? C13 H13 0.9300 . ? C16 N2 1.341(11) . ? C16 C15 1.378(14) . ? C16 H16 0.9300 . ? C18 C19 1.359(12) . ? C18 C17 1.396(12) . ? C18 H18 0.9300 . ? C5 C6 1.367(12) . ? C5 C4 1.380(13) . ? C5 H5 0.9300 . ? C14 C15 1.378(14) . ? C14 H14 0.9300 . ? C4 C3 1.374(14) . ? C4 H4 0.9300 . ? C6 C1 1.390(12) . ? C6 C7 1.494(11) . ? C7 C8 1.379(11) . ? N2 C12 1.348(10) . ? C23 C24 1.305(13) . ? C23 H23 0.9300 . ? C15 H15 0.9300 . ? C21 C22 1.410(11) . ? C21 H21 0.9300 . ? C17 C22 1.398(12) . ? C22 H22 0.9300 . ? C25 N4 1.367(13) . ? C25 C24 1.384(14) . ? C25 H25 0.9300 . ? C10 H10 0.9300 . ? C8 H8 0.9300 . ? C3 C2 1.364(14) . ? C3 H3 0.9300 . ? C2 C1 1.384(12) . ? C2 H2 0.9300 . ? C24 H24 0.9300 . ? C1 H1 0.9300 . ? C19 H19 0.9300 . ? 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 N2 Hg1 N1 69.0(2) . . ? N2 Hg1 I1 109.69(18) . . ? N1 Hg1 I1 124.19(15) . . ? N2 Hg1 I2 112.16(18) . . ? N1 Hg1 I2 96.52(15) . . ? I1 Hg1 I2 129.63(3) . . ? C7 N1 C11 119.2(7) . . ? C7 N1 Hg1 121.8(5) . . ? C11 N1 Hg1 115.4(5) . . ? N4 N3 C23 111.7(7) . . ? N4 N3 C20 127.8(7) . . ? C23 N3 C20 120.5(7) . . ? N1 C11 C10 121.9(7) . . ? N1 C11 C12 116.7(7) . . ? C10 C11 C12 121.4(7) . . ? C21 C20 C19 121.5(8) . . ? C21 C20 N3 119.2(7) . . ? C19 C20 N3 119.3(7) . . ? C10 C9 C8 116.9(7) . . ? C10 C9 C17 122.2(7) . . ? C8 C9 C17 120.9(7) . . ? C14 C13 C12 121.9(9) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? N2 C16 C15 122.2(8) . . ? N2 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C19 C18 C17 122.2(8) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C6 C5 C4 119.8(8) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C13 C14 C15 119.0(9) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C5 C4 C3 120.7(9) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C5 C6 C1 119.9(8) . . ? C5 C6 C7 120.2(7) . . ? C1 C6 C7 119.9(7) . . ? N1 C7 C8 121.8(7) . . ? N1 C7 C6 117.6(7) . . ? C8 C7 C6 120.6(7) . . ? C16 N2 C12 119.6(7) . . ? C16 N2 Hg1 121.2(6) . . ? C12 N2 Hg1 119.2(5) . . ? C24 C23 N3 104.6(8) . . ? C24 C23 H23 127.7 . . ? N3 C23 H23 127.7 . . ? N2 C12 C13 119.1(7) . . ? N2 C12 C11 117.1(7) . . ? C13 C12 C11 123.8(7) . . ? C16 C15 C14 118.2(8) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C20 C21 C22 118.8(8) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C18 C17 C22 118.0(7) . . ? C18 C17 C9 121.5(7) . . ? C22 C17 C9 120.5(7) . . ? C17 C22 C21 120.5(8) . . ? C17 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? N4 C25 C24 104.5(8) . . ? N4 C25 H25 127.7 . . ? C24 C25 H25 127.7 . . ? C11 C10 C9 120.3(7) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C7 C8 C9 119.9(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C2 C3 C4 119.5(9) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C2 C1 120.7(8) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C23 C24 C25 112.6(8) . . ? C23 C24 H24 123.7 . . ? C25 C24 H24 123.7 . . ? N3 N4 C25 106.6(8) . . ? C2 C1 C6 119.3(8) . . ? C2 C1 H1 120.3 . . ? C6 C1 H1 120.3 . . ? C18 C19 C20 119.1(8) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Hg1 N1 C7 -170.7(6) . . . . ? I1 Hg1 N1 C7 89.1(6) . . . . ? I2 Hg1 N1 C7 -59.5(6) . . . . ? N2 Hg1 N1 C11 -12.3(5) . . . . ? I1 Hg1 N1 C11 -112.4(5) . . . . ? I2 Hg1 N1 C11 99.0(5) . . . . ? C7 N1 C11 C10 -0.7(11) . . . . ? Hg1 N1 C11 C10 -159.7(6) . . . . ? C7 N1 C11 C12 177.5(7) . . . . ? Hg1 N1 C11 C12 18.4(8) . . . . ? N4 N3 C20 C21 -27.0(14) . . . . ? C23 N3 C20 C21 153.6(9) . . . . ? N4 N3 C20 C19 152.4(10) . . . . ? C23 N3 C20 C19 -26.9(13) . . . . ? C12 C13 C14 C15 0.5(17) . . . . ? C6 C5 C4 C3 -1.8(14) . . . . ? C4 C5 C6 C1 1.9(13) . . . . ? C4 C5 C6 C7 -179.3(8) . . . . ? C11 N1 C7 C8 0.8(11) . . . . ? Hg1 N1 C7 C8 158.5(6) . . . . ? C11 N1 C7 C6 -179.6(7) . . . . ? Hg1 N1 C7 C6 -22.0(9) . . . . ? C5 C6 C7 N1 141.1(8) . . . . ? C1 C6 C7 N1 -40.2(11) . . . . ? C5 C6 C7 C8 -39.4(12) . . . . ? C1 C6 C7 C8 139.4(8) . . . . ? C15 C16 N2 C12 -0.2(15) . . . . ? C15 C16 N2 Hg1 178.1(8) . . . . ? N1 Hg1 N2 C16 -173.9(8) . . . . ? I1 Hg1 N2 C16 -53.8(8) . . . . ? I2 Hg1 N2 C16 97.5(7) . . . . ? N1 Hg1 N2 C12 4.4(5) . . . . ? I1 Hg1 N2 C12 124.6(6) . . . . ? I2 Hg1 N2 C12 -84.1(6) . . . . ? N4 N3 C23 C24 0.4(12) . . . . ? C20 N3 C23 C24 179.9(9) . . . . ? C16 N2 C12 C13 1.0(12) . . . . ? Hg1 N2 C12 C13 -177.4(7) . . . . ? C16 N2 C12 C11 -178.5(8) . . . . ? Hg1 N2 C12 C11 3.1(9) . . . . ? C14 C13 C12 N2 -1.1(15) . . . . ? C14 C13 C12 C11 178.4(9) . . . . ? N1 C11 C12 N2 -14.8(10) . . . . ? C10 C11 C12 N2 163.4(8) . . . . ? N1 C11 C12 C13 165.7(8) . . . . ? C10 C11 C12 C13 -16.1(12) . . . . ? N2 C16 C15 C14 -0.4(16) . . . . ? C13 C14 C15 C16 0.3(17) . . . . ? C19 C20 C21 C22 -0.8(14) . . . . ? N3 C20 C21 C22 178.7(8) . . . . ? C19 C18 C17 C22 -1.2(14) . . . . ? C19 C18 C17 C9 177.3(9) . . . . ? C10 C9 C17 C18 -149.8(9) . . . . ? C8 C9 C17 C18 27.6(12) . . . . ? C10 C9 C17 C22 28.7(12) . . . . ? C8 C9 C17 C22 -154.0(8) . . . . ? C18 C17 C22 C21 1.2(13) . . . . ? C9 C17 C22 C21 -177.3(8) . . . . ? C20 C21 C22 C17 -0.2(14) . . . . ? N1 C11 C10 C9 0.6(12) . . . . ? C12 C11 C10 C9 -177.5(7) . . . . ? C8 C9 C10 C11 -0.6(12) . . . . ? C17 C9 C10 C11 176.9(8) . . . . ? N1 C7 C8 C9 -0.8(12) . . . . ? C6 C7 C8 C9 179.6(7) . . . . ? C10 C9 C8 C7 0.7(12) . . . . ? C17 C9 C8 C7 -176.8(8) . . . . ? C5 C4 C3 C2 1.2(15) . . . . ? C4 C3 C2 C1 -0.8(15) . . . . ? N3 C23 C24 C25 -0.7(14) . . . . ? N4 C25 C24 C23 0.7(14) . . . . ? C23 N3 N4 C25 0.0(12) . . . . ? C20 N3 N4 C25 -179.4(9) . . . . ? C24 C25 N4 N3 -0.4(12) . . . . ? C3 C2 C1 C6 1.0(14) . . . . ? C5 C6 C1 C2 -1.5(13) . . . . ? C7 C6 C1 C2 179.7(8) . . . . ? C17 C18 C19 C20 0.2(15) . . . . ? C21 C20 C19 C18 0.8(15) . . . . ? N3 C20 C19 C18 -178.7(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.382 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.225 data_jf _database_code_depnum_ccdc_archive 'CCDC 872923' #TrackingRef 'jf.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H40 Co N10 O S2' _chemical_formula_weight 956.00 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.194(5) _cell_length_b 12.533(5) _cell_length_c 15.864(5) _cell_angle_alpha 86.325(5) _cell_angle_beta 71.489(5) _cell_angle_gamma 87.781(5) _cell_volume 2293.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7054 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.04 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8602 _exptl_absorpt_correction_T_max 0.9035 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16421 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7994 _reflns_number_gt 6690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] 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 7994 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1442 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.42922(2) 1.06028(2) 0.264223(19) 0.03379(13) Uani 1 1 d . . . S1 S 0.07436(7) 1.02650(7) 0.19916(7) 0.0757(3) Uani 1 1 d . . . S2 S 0.50416(9) 1.38265(6) 0.38288(6) 0.0743(3) Uani 1 1 d . . . N2 N 0.49566(15) 0.91800(14) 0.17541(12) 0.0317(4) Uani 1 1 d . . . N6 N 0.56795(15) 0.98482(14) 0.32075(12) 0.0310(4) Uani 1 1 d . . . N1 N 0.51550(16) 1.12737(14) 0.13610(12) 0.0355(4) Uani 1 1 d . . . C11 C 0.3926(2) 0.77311(17) 0.27791(15) 0.0345(5) Uani 1 1 d . . . N9 N 0.27599(19) 1.07789(17) 0.23275(15) 0.0477(5) Uani 1 1 d . . . N5 N 0.33884(16) 0.99880(14) 0.39508(12) 0.0355(4) Uani 1 1 d . . . C7 C 0.65205(19) 0.87582(17) 0.04304(15) 0.0374(5) Uani 1 1 d . . . H7 H 0.7059 0.9002 -0.0100 0.045 Uiso 1 1 calc R . . C35 C 0.68288(19) 0.97350(17) 0.27820(15) 0.0335(5) Uani 1 1 d . . . C30 C 0.39503(19) 0.93415(17) 0.43842(14) 0.0334(5) Uani 1 1 d . . . C32 C 0.5802(2) 0.82763(18) 0.41329(16) 0.0391(5) Uani 1 1 d . . . H32 H 0.5431 0.7808 0.4608 0.047 Uiso 1 1 calc R . . N3 N 0.9500(2) 0.44127(19) -0.11761(15) 0.0542(6) Uani 1 1 d . . . C6 C 0.57639(19) 0.94780(17) 0.09745(14) 0.0324(5) Uani 1 1 d . . . N7 N 0.96910(19) 0.43478(16) 0.37012(15) 0.0505(6) Uani 1 1 d . . . C45 C 0.8975(2) 0.52875(19) 0.37675(16) 0.0423(6) Uani 1 1 d . . . C36 C 0.74102(18) 1.05701(18) 0.20975(15) 0.0363(5) Uani 1 1 d . . . C51 C 0.1914(2) 1.05695(19) 0.21955(17) 0.0430(6) Uani 1 1 d . . . C31 C 0.52041(19) 0.91426(17) 0.38930(14) 0.0330(5) Uani 1 1 d . . . C8 C 0.64672(19) 0.76666(17) 0.06853(16) 0.0365(5) Uani 1 1 d . . . C10 C 0.48767(19) 0.81151(17) 0.19863(15) 0.0328(5) Uani 1 1 d . . . C17 C 0.7250(2) 0.68452(18) 0.01432(16) 0.0404(5) Uani 1 1 d . . . C34 C 0.7469(2) 0.88839(18) 0.29988(16) 0.0383(5) Uani 1 1 d . . . H34 H 0.8257 0.8831 0.2695 0.046 Uiso 1 1 calc R . . C42 C 0.7630(2) 0.71357(19) 0.37933(16) 0.0417(6) Uani 1 1 d . . . C4 C 0.6385(2) 1.10628(19) -0.01290(16) 0.0420(6) Uani 1 1 d . . . H4 H 0.6829 1.0617 -0.0560 0.050 Uiso 1 1 calc R . . C20 C 0.8731(2) 0.5255(2) -0.07578(17) 0.0462(6) Uani 1 1 d . . . C33 C 0.6965(2) 0.81125(18) 0.36555(16) 0.0385(5) Uani 1 1 d . . . C9 C 0.5625(2) 0.73669(18) 0.14795(15) 0.0379(5) Uani 1 1 d . . . H9 H 0.5562 0.6650 0.1675 0.045 Uiso 1 1 calc R . . C5 C 0.57857(19) 1.06426(17) 0.07196(15) 0.0334(5) Uani 1 1 d . . . C52 C 0.4562(2) 1.27951(19) 0.34873(16) 0.0433(6) Uani 1 1 d . . . C21 C 0.9026(2) 0.6310(2) -0.09580(18) 0.0533(7) Uani 1 1 d . . . H21 H 0.9716 0.6493 -0.1394 0.064 Uiso 1 1 calc R . . C16 C 0.2812(2) 0.81490(19) 0.29401(17) 0.0447(6) Uani 1 1 d . . . H16 H 0.2661 0.8683 0.2555 0.054 Uiso 1 1 calc R . . C26 C 0.2274(2) 1.0249(2) 0.43785(17) 0.0442(6) Uani 1 1 d . . . H26 H 0.1885 1.0718 0.4089 0.053 Uiso 1 1 calc R . . C41 C 0.7176(2) 1.16401(19) 0.22504(18) 0.0445(6) Uani 1 1 d . . . H41 H 0.6627 1.1837 0.2777 0.053 Uiso 1 1 calc R . . C28 C 0.2268(2) 0.9167(2) 0.56588(17) 0.0493(6) Uani 1 1 d . . . H28 H 0.1892 0.8884 0.6230 0.059 Uiso 1 1 calc R . . C29 C 0.3413(2) 0.8909(2) 0.52355(16) 0.0443(6) Uani 1 1 d . . . H29 H 0.3819 0.8449 0.5518 0.053 Uiso 1 1 calc R . . C19 C 0.7700(2) 0.4982(2) -0.01373(19) 0.0520(7) Uani 1 1 d . . . H19 H 0.7500 0.4267 -0.0016 0.062 Uiso 1 1 calc R . . C44 C 0.9451(2) 0.6270(2) 0.3730(2) 0.0546(7) Uani 1 1 d . . . H44 H 1.0223 0.6318 0.3698 0.065 Uiso 1 1 calc R . . C37 C 0.8244(2) 1.0289(2) 0.13045(17) 0.0473(6) Uani 1 1 d . . . H37 H 0.8428 0.9574 0.1195 0.057 Uiso 1 1 calc R . . C27 C 0.1689(2) 0.9850(2) 0.52243(18) 0.0499(6) Uani 1 1 d . . . H27 H 0.0918 1.0038 0.5497 0.060 Uiso 1 1 calc R . . C18 C 0.6957(2) 0.57648(19) 0.03077(18) 0.0489(6) Uani 1 1 d . . . H18 H 0.6253 0.5574 0.0722 0.059 Uiso 1 1 calc R . . C22 C 0.8284(2) 0.7100(2) -0.05028(18) 0.0496(6) Uani 1 1 d . . . H22 H 0.8486 0.7814 -0.0635 0.059 Uiso 1 1 calc R . . C43 C 0.8784(2) 0.7189(2) 0.3739(2) 0.0532(7) Uani 1 1 d . . . H43 H 0.9114 0.7853 0.3708 0.064 Uiso 1 1 calc R . . C12 C 0.4122(2) 0.69018(19) 0.33475(16) 0.0451(6) Uani 1 1 d . . . H12 H 0.4860 0.6599 0.3237 0.054 Uiso 1 1 calc R . . N4 N 0.9042(3) 0.3459(2) -0.12653(19) 0.0746(8) Uani 1 1 d . . . O1 O 0.4610(2) 0.4828(2) 0.19200(17) 0.0843(7) Uani 1 1 d . . . H54 H 0.4715 0.4657 0.2397 0.126 Uiso 1 1 calc R . . C2 C 0.5623(2) 1.27840(19) 0.03221(17) 0.0457(6) Uani 1 1 d . . . H2 H 0.5533 1.3512 0.0200 0.055 Uiso 1 1 calc R . . C53 C 0.3426(4) 0.4929(4) 0.2048(3) 0.1049(14) Uani 1 1 d . . . H53A H 0.3011 0.4896 0.2674 0.157 Uiso 1 1 calc R . . H53B H 0.3188 0.4359 0.1773 0.157 Uiso 1 1 calc R . . H53C H 0.3264 0.5603 0.1784 0.157 Uiso 1 1 calc R . . N10 N 0.42555(19) 1.20528(16) 0.32307(14) 0.0474(5) Uani 1 1 d . . . N8 N 0.9418(2) 0.3439(2) 0.33942(18) 0.0693(7) Uani 1 1 d . . . C47 C 0.7152(2) 0.6131(2) 0.38728(18) 0.0488(6) Uani 1 1 d . . . H47 H 0.6369 0.6080 0.3942 0.059 Uiso 1 1 calc R . . C3 C 0.6313(2) 1.2151(2) -0.03255(18) 0.0472(6) Uani 1 1 d . . . H3 H 0.6723 1.2448 -0.0884 0.057 Uiso 1 1 calc R . . C1 C 0.5072(2) 1.23218(18) 0.11504(17) 0.0443(6) Uani 1 1 d . . . H1 H 0.4618 1.2757 0.1587 0.053 Uiso 1 1 calc R . . C46 C 0.7817(2) 0.5204(2) 0.38516(18) 0.0500(7) Uani 1 1 d . . . H46 H 0.7490 0.4537 0.3893 0.060 Uiso 1 1 calc R . . C40 C 0.7750(3) 1.2423(2) 0.1628(2) 0.0600(8) Uani 1 1 d . . . H40 H 0.7588 1.3140 0.1741 0.072 Uiso 1 1 calc R . . C15 C 0.1927(2) 0.7772(2) 0.3675(2) 0.0572(7) Uani 1 1 d . . . H15 H 0.1183 0.8059 0.3785 0.069 Uiso 1 1 calc R . . C24 C 1.0969(4) 0.3325(3) -0.1601(2) 0.0812(11) Uani 1 1 d . . . H24 H 1.1713 0.3029 -0.1762 0.097 Uiso 1 1 calc R . . C23 C 1.0645(3) 0.4348(3) -0.1376(2) 0.0776(10) Uani 1 1 d . . . H23 H 1.1132 0.4896 -0.1364 0.093 Uiso 1 1 calc R . . C38 C 0.8795(2) 1.1084(3) 0.06837(19) 0.0604(8) Uani 1 1 d . . . H38 H 0.9333 1.0897 0.0149 0.072 Uiso 1 1 calc R . . C50 C 1.0280(3) 0.2758(3) 0.3413(2) 0.0770(10) Uani 1 1 d . . . H50 H 1.0332 0.2056 0.3245 0.092 Uiso 1 1 calc R . . C13 C 0.3229(3) 0.6529(2) 0.40723(18) 0.0607(8) Uani 1 1 d . . . H13 H 0.3365 0.5975 0.4447 0.073 Uiso 1 1 calc R . . C39 C 0.8554(3) 1.2147(3) 0.0849(2) 0.0656(9) Uani 1 1 d . . . H39 H 0.8936 1.2675 0.0432 0.079 Uiso 1 1 calc R . . C14 C 0.2141(3) 0.6972(2) 0.4242(2) 0.0644(8) Uani 1 1 d . . . H14 H 0.1547 0.6733 0.4742 0.077 Uiso 1 1 calc R . . C48 C 1.0668(3) 0.4226(3) 0.3915(3) 0.0734(9) Uani 1 1 d . . . H48 H 1.1007 0.4727 0.4157 0.088 Uiso 1 1 calc R . . C49 C 1.1061(3) 0.3211(3) 0.3704(3) 0.0880(12) Uani 1 1 d . . . H49 H 1.1742 0.2895 0.3753 0.106 Uiso 1 1 calc R . . C25 C 0.9955(4) 0.2822(3) -0.1540(2) 0.0879(13) Uani 1 1 d . . . H25 H 0.9923 0.2116 -0.1677 0.106 Uiso 1 1 calc R . . 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 Co1 0.0371(2) 0.02966(19) 0.0352(2) -0.00036(13) -0.01275(14) 0.00158(13) S1 0.0617(5) 0.0677(5) 0.1145(8) -0.0117(5) -0.0496(5) -0.0051(4) S2 0.1081(7) 0.0467(4) 0.0790(6) -0.0090(4) -0.0424(5) -0.0130(4) N2 0.0360(10) 0.0311(9) 0.0305(10) -0.0018(7) -0.0139(8) -0.0018(7) N6 0.0343(10) 0.0308(9) 0.0294(9) -0.0046(7) -0.0118(8) -0.0002(7) N1 0.0432(11) 0.0283(9) 0.0383(11) 0.0006(8) -0.0179(9) -0.0011(8) C11 0.0431(13) 0.0283(11) 0.0321(12) -0.0060(9) -0.0106(10) -0.0053(9) N9 0.0440(12) 0.0477(12) 0.0532(13) 0.0000(10) -0.0191(10) 0.0039(10) N5 0.0339(10) 0.0356(10) 0.0367(11) -0.0039(8) -0.0106(8) 0.0021(8) C7 0.0377(13) 0.0363(12) 0.0348(12) -0.0012(10) -0.0065(10) -0.0034(10) C35 0.0359(12) 0.0348(11) 0.0321(12) -0.0045(9) -0.0137(10) -0.0010(9) C30 0.0390(12) 0.0322(11) 0.0306(11) -0.0052(9) -0.0125(10) -0.0017(9) C32 0.0444(14) 0.0368(12) 0.0376(13) 0.0033(10) -0.0160(11) -0.0006(10) N3 0.0567(15) 0.0567(14) 0.0429(13) -0.0095(10) -0.0074(11) 0.0153(11) C6 0.0353(12) 0.0309(11) 0.0333(12) -0.0007(9) -0.0141(10) -0.0033(9) N7 0.0553(14) 0.0377(12) 0.0532(13) 0.0043(10) -0.0125(11) 0.0101(10) C45 0.0483(15) 0.0361(13) 0.0410(13) 0.0052(10) -0.0138(11) 0.0048(10) C36 0.0271(11) 0.0436(13) 0.0387(13) 0.0043(10) -0.0124(10) -0.0020(9) C51 0.0444(14) 0.0385(13) 0.0461(14) -0.0017(11) -0.0155(12) 0.0076(11) C31 0.0386(12) 0.0317(11) 0.0312(11) -0.0034(9) -0.0140(10) -0.0031(9) C8 0.0364(12) 0.0343(12) 0.0403(13) -0.0049(10) -0.0137(10) -0.0016(9) C10 0.0377(12) 0.0299(11) 0.0334(12) -0.0019(9) -0.0146(10) -0.0013(9) C17 0.0395(13) 0.0365(12) 0.0432(13) -0.0036(10) -0.0104(11) 0.0015(10) C34 0.0334(12) 0.0406(13) 0.0408(13) -0.0026(10) -0.0121(10) 0.0043(10) C42 0.0466(14) 0.0396(13) 0.0400(13) 0.0024(10) -0.0167(11) 0.0045(11) C4 0.0469(14) 0.0397(13) 0.0389(13) 0.0016(10) -0.0132(11) -0.0050(10) C20 0.0492(15) 0.0462(14) 0.0417(14) -0.0114(11) -0.0120(12) 0.0116(11) C33 0.0449(14) 0.0347(12) 0.0402(13) -0.0025(10) -0.0199(11) 0.0028(10) C9 0.0457(13) 0.0304(11) 0.0374(13) -0.0018(9) -0.0126(11) -0.0023(10) C5 0.0374(12) 0.0323(11) 0.0345(12) 0.0006(9) -0.0174(10) -0.0022(9) C52 0.0514(15) 0.0363(13) 0.0402(14) 0.0007(11) -0.0131(12) 0.0067(11) C21 0.0449(15) 0.0544(16) 0.0488(16) -0.0028(12) 0.0016(12) 0.0016(12) C16 0.0461(14) 0.0354(12) 0.0513(15) 0.0000(11) -0.0134(12) -0.0073(10) C26 0.0386(13) 0.0498(14) 0.0432(14) -0.0074(11) -0.0114(11) 0.0069(11) C41 0.0434(14) 0.0426(14) 0.0475(15) 0.0038(11) -0.0157(12) -0.0018(11) C28 0.0486(15) 0.0595(16) 0.0359(14) -0.0044(12) -0.0062(12) -0.0107(12) C29 0.0476(15) 0.0510(14) 0.0340(13) 0.0007(11) -0.0127(11) -0.0014(11) C19 0.0555(16) 0.0357(13) 0.0576(17) -0.0078(12) -0.0069(13) 0.0015(11) C44 0.0487(15) 0.0457(15) 0.077(2) 0.0021(13) -0.0329(15) 0.0034(12) C37 0.0374(13) 0.0570(16) 0.0464(15) -0.0006(12) -0.0126(11) 0.0028(11) C27 0.0388(14) 0.0594(16) 0.0468(15) -0.0138(12) -0.0050(12) 0.0010(12) C18 0.0438(14) 0.0395(14) 0.0546(16) -0.0116(11) -0.0014(12) -0.0020(11) C22 0.0529(16) 0.0379(13) 0.0503(16) -0.0020(11) -0.0052(13) -0.0040(11) C43 0.0554(16) 0.0391(14) 0.0745(19) -0.0020(13) -0.0343(15) 0.0030(12) C12 0.0561(15) 0.0404(13) 0.0376(13) -0.0005(10) -0.0135(12) -0.0020(11) N4 0.085(2) 0.0456(14) 0.0697(18) -0.0117(12) 0.0097(15) 0.0078(13) O1 0.108(2) 0.0630(15) 0.0709(15) 0.0058(12) -0.0135(14) -0.0158(13) C2 0.0590(16) 0.0313(12) 0.0532(16) 0.0076(11) -0.0282(13) -0.0053(11) C53 0.108(3) 0.109(3) 0.108(3) -0.020(3) -0.044(3) -0.009(3) N10 0.0566(13) 0.0356(11) 0.0488(13) -0.0038(9) -0.0150(10) 0.0002(10) N8 0.0799(18) 0.0476(14) 0.0734(18) -0.0103(12) -0.0143(15) 0.0110(13) C47 0.0399(14) 0.0425(14) 0.0606(17) 0.0105(12) -0.0137(12) -0.0005(11) C3 0.0524(15) 0.0469(14) 0.0435(14) 0.0140(12) -0.0187(12) -0.0126(12) C1 0.0588(16) 0.0307(12) 0.0455(14) -0.0015(10) -0.0196(12) -0.0007(11) C46 0.0486(15) 0.0398(14) 0.0565(16) 0.0087(12) -0.0118(13) 0.0003(11) C40 0.0630(19) 0.0452(15) 0.071(2) 0.0138(14) -0.0228(16) -0.0110(13) C15 0.0431(15) 0.0526(16) 0.0682(19) -0.0147(14) -0.0034(13) -0.0092(12) C24 0.082(3) 0.103(3) 0.060(2) -0.0279(19) -0.0257(19) 0.053(2) C23 0.062(2) 0.111(3) 0.063(2) -0.0363(19) -0.0228(17) 0.0294(19) C38 0.0388(15) 0.088(2) 0.0453(16) 0.0125(15) -0.0044(12) 0.0006(14) C50 0.075(2) 0.0492(18) 0.088(3) -0.0060(16) -0.002(2) 0.0199(17) C13 0.085(2) 0.0509(16) 0.0411(15) 0.0101(12) -0.0139(15) -0.0157(15) C39 0.0543(18) 0.072(2) 0.068(2) 0.0309(16) -0.0195(16) -0.0170(15) C14 0.072(2) 0.0597(18) 0.0476(17) -0.0024(14) 0.0030(15) -0.0237(16) C48 0.063(2) 0.0582(19) 0.105(3) 0.0109(18) -0.0390(19) 0.0086(15) C49 0.058(2) 0.062(2) 0.130(3) 0.018(2) -0.016(2) 0.0222(17) C25 0.118(3) 0.058(2) 0.062(2) -0.0105(16) 0.005(2) 0.028(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 Co1 N9 2.082(2) . ? Co1 N10 2.088(2) . ? Co1 N1 2.1064(19) . ? Co1 N5 2.1274(19) . ? Co1 N6 2.3002(18) . ? Co1 N2 2.3037(19) . ? S1 C51 1.624(3) . ? S2 C52 1.630(3) . ? N2 C6 1.354(3) . ? N2 C10 1.360(3) . ? N6 C31 1.348(3) . ? N6 C35 1.355(3) . ? N1 C1 1.343(3) . ? N1 C5 1.346(3) . ? C11 C16 1.388(3) . ? C11 C12 1.396(3) . ? C11 C10 1.482(3) . ? N9 C51 1.158(3) . ? N5 C30 1.335(3) . ? N5 C26 1.350(3) . ? C7 C6 1.393(3) . ? C7 C8 1.399(3) . ? C7 H7 0.9300 . ? C35 C34 1.388(3) . ? C35 C36 1.483(3) . ? C30 C29 1.385(3) . ? C30 C31 1.499(3) . ? C32 C31 1.385(3) . ? C32 C33 1.394(3) . ? C32 H32 0.9300 . ? N3 C23 1.330(4) . ? N3 N4 1.373(4) . ? N3 C20 1.433(3) . ? C6 C5 1.488(3) . ? N7 C48 1.339(4) . ? N7 N8 1.360(3) . ? N7 C45 1.428(3) . ? C45 C44 1.372(4) . ? C45 C46 1.383(4) . ? C36 C41 1.381(3) . ? C36 C37 1.399(3) . ? C8 C9 1.389(3) . ? C8 C17 1.492(3) . ? C10 C9 1.387(3) . ? C17 C22 1.382(3) . ? C17 C18 1.401(3) . ? C34 C33 1.381(3) . ? C34 H34 0.9300 . ? C42 C43 1.386(4) . ? C42 C47 1.389(4) . ? C42 C33 1.485(3) . ? C4 C3 1.385(3) . ? C4 C5 1.392(3) . ? C4 H4 0.9300 . ? C20 C19 1.367(4) . ? C20 C21 1.375(4) . ? C9 H9 0.9300 . ? C52 N10 1.159(3) . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C16 C15 1.385(4) . ? C16 H16 0.9300 . ? C26 C27 1.376(4) . ? C26 H26 0.9300 . ? C41 C40 1.384(4) . ? C41 H41 0.9300 . ? C28 C27 1.375(4) . ? C28 C29 1.380(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C19 C18 1.377(3) . ? C19 H19 0.9300 . ? C44 C43 1.383(3) . ? C44 H44 0.9300 . ? C37 C38 1.385(4) . ? C37 H37 0.9300 . ? C27 H27 0.9300 . ? C18 H18 0.9300 . ? C22 H22 0.9300 . ? C43 H43 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? N4 C25 1.318(4) . ? O1 C53 1.394(5) . ? O1 H54 0.8200 . ? C2 C1 1.373(4) . ? C2 C3 1.377(4) . ? C2 H2 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? N8 C50 1.335(4) . ? C47 C46 1.387(3) . ? C47 H47 0.9300 . ? C3 H3 0.9300 . ? C1 H1 0.9300 . ? C46 H46 0.9300 . ? C40 C39 1.367(4) . ? C40 H40 0.9300 . ? C15 C14 1.377(5) . ? C15 H15 0.9300 . ? C24 C23 1.362(5) . ? C24 C25 1.382(6) . ? C24 H24 0.9300 . ? C23 H23 0.9300 . ? C38 C39 1.376(4) . ? C38 H38 0.9300 . ? C50 C49 1.341(5) . ? C50 H50 0.9300 . ? C13 C14 1.369(4) . ? C13 H13 0.9300 . ? C39 H39 0.9300 . ? C14 H14 0.9300 . ? C48 C49 1.365(5) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C25 H25 0.9300 . ? 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 N9 Co1 N10 99.33(9) . . ? N9 Co1 N1 87.83(8) . . ? N10 Co1 N1 92.47(8) . . ? N9 Co1 N5 91.34(8) . . ? N10 Co1 N5 85.48(8) . . ? N1 Co1 N5 177.64(7) . . ? N9 Co1 N6 159.69(8) . . ? N10 Co1 N6 93.58(8) . . ? N1 Co1 N6 107.32(7) . . ? N5 Co1 N6 74.02(7) . . ? N9 Co1 N2 93.87(8) . . ? N10 Co1 N2 160.79(8) . . ? N1 Co1 N2 74.05(7) . . ? N5 Co1 N2 108.22(7) . . ? N6 Co1 N2 77.97(6) . . ? C6 N2 C10 116.92(18) . . ? C6 N2 Co1 111.96(13) . . ? C10 N2 Co1 128.80(14) . . ? C31 N6 C35 117.01(18) . . ? C31 N6 Co1 110.71(14) . . ? C35 N6 Co1 127.75(14) . . ? C1 N1 C5 118.1(2) . . ? C1 N1 Co1 121.84(16) . . ? C5 N1 Co1 119.99(14) . . ? C16 C11 C12 118.9(2) . . ? C16 C11 C10 120.5(2) . . ? C12 C11 C10 120.5(2) . . ? C51 N9 Co1 160.8(2) . . ? C30 N5 C26 118.1(2) . . ? C30 N5 Co1 119.06(15) . . ? C26 N5 Co1 122.85(16) . . ? C6 C7 C8 119.8(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N6 C35 C34 121.4(2) . . ? N6 C35 C36 118.55(19) . . ? C34 C35 C36 120.0(2) . . ? N5 C30 C29 122.1(2) . . ? N5 C30 C31 115.22(19) . . ? C29 C30 C31 122.7(2) . . ? C31 C32 C33 119.4(2) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C23 N3 N4 111.9(3) . . ? C23 N3 C20 128.4(3) . . ? N4 N3 C20 118.8(2) . . ? N2 C6 C7 123.33(19) . . ? N2 C6 C5 115.42(18) . . ? C7 C6 C5 121.2(2) . . ? C48 N7 N8 111.9(2) . . ? C48 N7 C45 127.2(3) . . ? N8 N7 C45 121.0(2) . . ? C44 C45 C46 120.5(2) . . ? C44 C45 N7 119.4(2) . . ? C46 C45 N7 120.0(2) . . ? C41 C36 C37 118.8(2) . . ? C41 C36 C35 120.5(2) . . ? C37 C36 C35 120.6(2) . . ? N9 C51 S1 178.8(3) . . ? N6 C31 C32 123.7(2) . . ? N6 C31 C30 115.27(18) . . ? C32 C31 C30 121.0(2) . . ? C9 C8 C7 116.5(2) . . ? C9 C8 C17 120.4(2) . . ? C7 C8 C17 123.1(2) . . ? N2 C10 C9 122.0(2) . . ? N2 C10 C11 119.30(19) . . ? C9 C10 C11 118.6(2) . . ? C22 C17 C18 117.9(2) . . ? C22 C17 C8 122.6(2) . . ? C18 C17 C8 119.4(2) . . ? C33 C34 C35 121.6(2) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C43 C42 C47 118.1(2) . . ? C43 C42 C33 121.0(2) . . ? C47 C42 C33 120.5(2) . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C19 C20 C21 120.6(2) . . ? C19 C20 N3 118.2(2) . . ? C21 C20 N3 121.2(2) . . ? C34 C33 C32 116.6(2) . . ? C34 C33 C42 120.5(2) . . ? C32 C33 C42 122.8(2) . . ? C10 C9 C8 121.4(2) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.48(19) . . ? C4 C5 C6 123.0(2) . . ? N10 C52 S2 177.9(2) . . ? C20 C21 C22 119.4(2) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C15 C16 C11 120.0(2) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? N5 C26 C27 122.8(2) . . ? N5 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C36 C41 C40 120.7(3) . . ? C36 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C27 C28 C29 119.1(2) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 119.2(2) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C45 C44 C43 120.0(3) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C28 C27 C26 118.7(2) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C19 C18 C17 120.8(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C17 C22 C21 121.2(2) . . ? C17 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C44 C43 C42 121.0(3) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C25 N4 N3 103.7(3) . . ? C53 O1 H54 109.5 . . ? C1 C2 C3 118.8(2) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? O1 C53 H53A 109.5 . . ? O1 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O1 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 N10 Co1 160.9(2) . . ? C50 N8 N7 103.7(3) . . ? C46 C47 C42 121.4(2) . . ? C46 C47 H47 119.3 . . ? C42 C47 H47 119.3 . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C45 C46 C47 119.0(2) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C23 C24 C25 105.3(3) . . ? C23 C24 H24 127.3 . . ? C25 C24 H24 127.3 . . ? N3 C23 C24 106.9(4) . . ? N3 C23 H23 126.5 . . ? C24 C23 H23 126.5 . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? N8 C50 C49 111.7(3) . . ? N8 C50 H50 124.2 . . ? C49 C50 H50 124.2 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C40 C39 C38 119.7(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N7 C48 C49 105.6(3) . . ? N7 C48 H48 127.2 . . ? C49 C48 H48 127.2 . . ? C50 C49 C48 107.1(3) . . ? C50 C49 H49 126.5 . . ? C48 C49 H49 126.5 . . ? N4 C25 C24 112.1(3) . . ? N4 C25 H25 123.9 . . ? C24 C25 H25 123.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N9 Co1 N2 C6 101.92(15) . . . . ? N10 Co1 N2 C6 -31.5(3) . . . . ? N1 Co1 N2 C6 15.29(14) . . . . ? N5 Co1 N2 C6 -165.39(14) . . . . ? N6 Co1 N2 C6 -96.88(14) . . . . ? N9 Co1 N2 C10 -96.16(18) . . . . ? N10 Co1 N2 C10 130.4(2) . . . . ? N1 Co1 N2 C10 177.21(19) . . . . ? N5 Co1 N2 C10 -3.47(19) . . . . ? N6 Co1 N2 C10 65.04(18) . . . . ? N9 Co1 N6 C31 -25.1(3) . . . . ? N10 Co1 N6 C31 104.47(15) . . . . ? N1 Co1 N6 C31 -161.82(14) . . . . ? N5 Co1 N6 C31 20.22(14) . . . . ? N2 Co1 N6 C31 -92.96(15) . . . . ? N9 Co1 N6 C35 130.0(2) . . . . ? N10 Co1 N6 C35 -100.46(18) . . . . ? N1 Co1 N6 C35 -6.75(18) . . . . ? N5 Co1 N6 C35 175.28(18) . . . . ? N2 Co1 N6 C35 62.10(17) . . . . ? N9 Co1 N1 C1 73.82(19) . . . . ? N10 Co1 N1 C1 -25.43(19) . . . . ? N5 Co1 N1 C1 4.2(18) . . . . ? N6 Co1 N1 C1 -119.96(18) . . . . ? N2 Co1 N1 C1 168.46(19) . . . . ? N9 Co1 N1 C5 -104.33(17) . . . . ? N10 Co1 N1 C5 156.42(17) . . . . ? N5 Co1 N1 C5 -173.9(16) . . . . ? N6 Co1 N1 C5 61.89(17) . . . . ? N2 Co1 N1 C5 -9.68(16) . . . . ? N10 Co1 N9 C51 -148.5(6) . . . . ? N1 Co1 N9 C51 119.3(6) . . . . ? N5 Co1 N9 C51 -62.9(6) . . . . ? N6 Co1 N9 C51 -19.8(8) . . . . ? N2 Co1 N9 C51 45.5(6) . . . . ? N9 Co1 N5 C30 154.16(17) . . . . ? N10 Co1 N5 C30 -106.59(17) . . . . ? N1 Co1 N5 C30 -136.3(16) . . . . ? N6 Co1 N5 C30 -11.55(16) . . . . ? N2 Co1 N5 C30 59.64(18) . . . . ? N9 Co1 N5 C26 -27.96(19) . . . . ? N10 Co1 N5 C26 71.29(19) . . . . ? N1 Co1 N5 C26 41.5(18) . . . . ? N6 Co1 N5 C26 166.33(19) . . . . ? N2 Co1 N5 C26 -122.48(18) . . . . ? C31 N6 C35 C34 4.7(3) . . . . ? Co1 N6 C35 C34 -149.02(18) . . . . ? C31 N6 C35 C36 -172.7(2) . . . . ? Co1 N6 C35 C36 33.5(3) . . . . ? C26 N5 C30 C29 2.4(3) . . . . ? Co1 N5 C30 C29 -179.65(17) . . . . ? C26 N5 C30 C31 -176.19(19) . . . . ? Co1 N5 C30 C31 1.8(3) . . . . ? C10 N2 C6 C7 -2.1(3) . . . . ? Co1 N2 C6 C7 162.15(18) . . . . ? C10 N2 C6 C5 176.98(18) . . . . ? Co1 N2 C6 C5 -18.8(2) . . . . ? C8 C7 C6 N2 -0.2(3) . . . . ? C8 C7 C6 C5 -179.2(2) . . . . ? C48 N7 C45 C44 25.8(4) . . . . ? N8 N7 C45 C44 -154.2(3) . . . . ? C48 N7 C45 C46 -155.5(3) . . . . ? N8 N7 C45 C46 24.5(4) . . . . ? N6 C35 C36 C41 43.7(3) . . . . ? C34 C35 C36 C41 -133.8(2) . . . . ? N6 C35 C36 C37 -139.4(2) . . . . ? C34 C35 C36 C37 43.1(3) . . . . ? Co1 N9 C51 S1 -71(13) . . . . ? C35 N6 C31 C32 -5.2(3) . . . . ? Co1 N6 C31 C32 152.84(19) . . . . ? C35 N6 C31 C30 175.97(18) . . . . ? Co1 N6 C31 C30 -26.0(2) . . . . ? C33 C32 C31 N6 0.7(4) . . . . ? C33 C32 C31 C30 179.5(2) . . . . ? N5 C30 C31 N6 17.6(3) . . . . ? C29 C30 C31 N6 -160.9(2) . . . . ? N5 C30 C31 C32 -161.3(2) . . . . ? C29 C30 C31 C32 20.2(3) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C6 C7 C8 C17 -179.7(2) . . . . ? C6 N2 C10 C9 3.6(3) . . . . ? Co1 N2 C10 C9 -157.61(17) . . . . ? C6 N2 C10 C11 -173.24(19) . . . . ? Co1 N2 C10 C11 25.6(3) . . . . ? C16 C11 C10 N2 42.3(3) . . . . ? C12 C11 C10 N2 -141.3(2) . . . . ? C16 C11 C10 C9 -134.6(2) . . . . ? C12 C11 C10 C9 41.7(3) . . . . ? C9 C8 C17 C22 -161.6(2) . . . . ? C7 C8 C17 C22 19.2(4) . . . . ? C9 C8 C17 C18 16.2(3) . . . . ? C7 C8 C17 C18 -163.1(2) . . . . ? N6 C35 C34 C33 0.2(4) . . . . ? C36 C35 C34 C33 177.6(2) . . . . ? C23 N3 C20 C19 -139.4(3) . . . . ? N4 N3 C20 C19 28.5(4) . . . . ? C23 N3 C20 C21 39.2(4) . . . . ? N4 N3 C20 C21 -152.9(3) . . . . ? C35 C34 C33 C32 -4.7(4) . . . . ? C35 C34 C33 C42 171.8(2) . . . . ? C31 C32 C33 C34 4.2(3) . . . . ? C31 C32 C33 C42 -172.2(2) . . . . ? C43 C42 C33 C34 40.1(4) . . . . ? C47 C42 C33 C34 -132.1(3) . . . . ? C43 C42 C33 C32 -143.7(3) . . . . ? C47 C42 C33 C32 44.2(4) . . . . ? N2 C10 C9 C8 -2.8(4) . . . . ? C11 C10 C9 C8 174.1(2) . . . . ? C7 C8 C9 C10 0.3(3) . . . . ? C17 C8 C9 C10 -178.9(2) . . . . ? C1 N1 C5 C4 3.0(3) . . . . ? Co1 N1 C5 C4 -178.74(17) . . . . ? C1 N1 C5 C6 -175.1(2) . . . . ? Co1 N1 C5 C6 3.1(3) . . . . ? C3 C4 C5 N1 -1.3(3) . . . . ? C3 C4 C5 C6 176.7(2) . . . . ? N2 C6 C5 N1 11.6(3) . . . . ? C7 C6 C5 N1 -169.3(2) . . . . ? N2 C6 C5 C4 -166.6(2) . . . . ? C7 C6 C5 C4 12.5(3) . . . . ? C19 C20 C21 C22 2.1(4) . . . . ? N3 C20 C21 C22 -176.5(3) . . . . ? C12 C11 C16 C15 2.5(4) . . . . ? C10 C11 C16 C15 178.9(2) . . . . ? C30 N5 C26 C27 -2.2(4) . . . . ? Co1 N5 C26 C27 179.90(19) . . . . ? C37 C36 C41 C40 0.4(4) . . . . ? C35 C36 C41 C40 177.4(2) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? N5 C30 C29 C28 -1.3(4) . . . . ? C31 C30 C29 C28 177.2(2) . . . . ? C21 C20 C19 C18 -1.4(4) . . . . ? N3 C20 C19 C18 177.2(3) . . . . ? C46 C45 C44 C43 -2.7(4) . . . . ? N7 C45 C44 C43 176.1(3) . . . . ? C41 C36 C37 C38 -1.5(4) . . . . ? C35 C36 C37 C38 -178.5(2) . . . . ? C29 C28 C27 C26 0.2(4) . . . . ? N5 C26 C27 C28 0.9(4) . . . . ? C20 C19 C18 C17 -0.9(4) . . . . ? C22 C17 C18 C19 2.5(4) . . . . ? C8 C17 C18 C19 -175.4(2) . . . . ? C18 C17 C22 C21 -1.8(4) . . . . ? C8 C17 C22 C21 176.0(2) . . . . ? C20 C21 C22 C17 -0.5(4) . . . . ? C45 C44 C43 C42 0.5(4) . . . . ? C47 C42 C43 C44 2.4(4) . . . . ? C33 C42 C43 C44 -169.9(3) . . . . ? C16 C11 C12 C13 -2.0(4) . . . . ? C10 C11 C12 C13 -178.4(2) . . . . ? C23 N3 N4 C25 -1.0(4) . . . . ? C20 N3 N4 C25 -170.8(3) . . . . ? S2 C52 N10 Co1 10(7) . . . . ? N9 Co1 N10 C52 -156.7(6) . . . . ? N1 Co1 N10 C52 -68.5(6) . . . . ? N5 Co1 N10 C52 112.7(6) . . . . ? N6 Co1 N10 C52 39.1(6) . . . . ? N2 Co1 N10 C52 -23.9(8) . . . . ? C48 N7 N8 C50 -1.1(3) . . . . ? C45 N7 N8 C50 178.9(2) . . . . ? C43 C42 C47 C46 -3.4(4) . . . . ? C33 C42 C47 C46 169.0(2) . . . . ? C1 C2 C3 C4 2.8(4) . . . . ? C5 C4 C3 C2 -1.6(4) . . . . ? C5 N1 C1 C2 -1.8(4) . . . . ? Co1 N1 C1 C2 179.98(19) . . . . ? C3 C2 C1 N1 -1.1(4) . . . . ? C44 C45 C46 C47 1.7(4) . . . . ? N7 C45 C46 C47 -177.0(2) . . . . ? C42 C47 C46 C45 1.3(4) . . . . ? C36 C41 C40 C39 0.4(4) . . . . ? C11 C16 C15 C14 -0.8(4) . . . . ? N4 N3 C23 C24 -0.3(4) . . . . ? C20 N3 C23 C24 168.3(3) . . . . ? C25 C24 C23 N3 1.4(4) . . . . ? C36 C37 C38 C39 1.8(4) . . . . ? N7 N8 C50 C49 -0.7(4) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C41 C40 C39 C38 -0.2(5) . . . . ? C37 C38 C39 C40 -1.0(5) . . . . ? C12 C13 C14 C15 2.0(5) . . . . ? C16 C15 C14 C13 -1.4(5) . . . . ? N8 N7 C48 C49 2.4(4) . . . . ? C45 N7 C48 C49 -177.6(3) . . . . ? N8 C50 C49 C48 2.2(5) . . . . ? N7 C48 C49 C50 -2.7(4) . . . . ? N3 N4 C25 C24 1.9(4) . . . . ? C23 C24 C25 N4 -2.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.530 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.048