# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_z1 _database_code_depnum_ccdc_archive 'CCDC 805571' #TrackingRef 'z1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H22 N6' _chemical_formula_weight 478.55 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' _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 9.5127(19) _cell_length_b 46.843(9) _cell_length_c 11.521(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.441(3) _cell_angle_gamma 90.00 _cell_volume 4710.3(16) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1505 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 20.42 _exptl_crystal_description CUBOID _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9918 _exptl_absorpt_correction_T_max 0.9926 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 33351 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8292 _reflns_number_gt 3111 _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_number_reflns 8292 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2022 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 N4 N 0.6996(4) 0.18382(7) 0.4337(3) 0.0496(10) Uani 1 1 d . . . N1 N 1.2054(4) 0.18572(7) 0.3832(3) 0.0507(10) Uani 1 1 d . . . N7 N 0.3078(4) -0.05754(8) -0.4346(3) 0.0524(10) Uani 1 1 d . . . C17 C 0.4378(5) 0.12134(9) 0.1588(4) 0.0444(11) Uani 1 1 d . . . C22 C 0.6163(5) 0.16403(10) 0.4616(4) 0.0502(12) Uani 1 1 d . . . N10 N -0.1870(4) -0.05224(8) -0.4474(3) 0.0486(9) Uani 1 1 d . . . C24 C 0.6968(5) 0.18353(9) 0.3167(4) 0.0468(11) Uani 1 1 d . . . C51 C 1.0290(5) 0.14444(9) 0.2101(4) 0.0487(12) Uani 1 1 d . . . C59 C 0.9385(5) 0.12241(9) 0.1201(4) 0.0474(12) Uani 1 1 d . . . N5 N 0.7795(4) 0.20692(8) 0.1691(4) 0.0631(11) Uani 1 1 d . . . C20 C 0.5261(5) 0.14335(9) 0.2529(4) 0.0458(11) Uani 1 1 d . . . C72 C 0.3870(5) -0.03483(10) -0.3539(4) 0.0483(11) Uani 1 1 d . . . C47 C 1.1254(5) 0.16590(10) 0.4159(4) 0.0494(12) Uani 1 1 d . . . C14 C 0.2777(5) 0.07865(9) -0.0157(4) 0.0463(11) Uani 1 1 d . . . C21 C 0.5274(5) 0.14379(9) 0.3747(4) 0.0520(12) Uani 1 1 d . . . H21 H 0.4695 0.1307 0.3975 0.062 Uiso 1 1 calc R . . C6 C -0.1086(4) -0.03071(9) -0.3579(4) 0.0423(11) Uani 1 1 d . . . C69 C 0.3397(5) -0.02569(10) -0.2610(4) 0.0536(12) Uani 1 1 d . . . H69 H 0.2589 -0.0348 -0.2500 0.064 Uiso 1 1 calc R . . C62 C 0.7723(5) 0.07879(10) -0.0480(4) 0.0506(12) Uani 1 1 d . . . C8 C 0.0334(5) -0.01634(9) -0.1455(4) 0.0500(12) Uani 1 1 d . . . H8 H 0.0765 -0.0209 -0.0600 0.060 Uiso 1 1 calc R . . C50 C 1.1107(5) 0.16518(9) 0.1765(4) 0.0504(12) Uani 1 1 d . . . H50 H 1.1067 0.1656 0.0945 0.060 Uiso 1 1 calc R . . C52 C 1.2884(5) 0.20737(9) 0.2324(4) 0.0517(12) Uani 1 1 d . . . C46 C 1.0384(5) 0.14544(9) 0.3331(4) 0.0511(12) Uani 1 1 d . . . H46 H 0.9852 0.1321 0.3600 0.061 Uiso 1 1 calc R . . C7 C -0.0428(5) -0.03732(9) -0.2312(4) 0.0492(12) Uani 1 1 d . . . H7 H -0.0497 -0.0557 -0.2038 0.059 Uiso 1 1 calc R . . C42 C 1.1335(5) 0.16804(10) 0.5471(4) 0.0529(12) Uani 1 1 d . . . C64 C 0.8215(5) 0.10793(9) 0.1373(4) 0.0559(13) Uani 1 1 d . . . H64 H 0.7977 0.1127 0.2057 0.067 Uiso 1 1 calc R . . C32 C 0.7879(5) 0.20585(9) 0.2874(5) 0.0510(12) Uani 1 1 d . . . C70 C 0.5081(5) -0.02148(10) -0.3677(4) 0.0553(12) Uani 1 1 d . . . H70 H 0.5419 -0.0278 -0.4288 0.066 Uiso 1 1 calc R . . C13 C 0.1889(5) 0.05743(9) -0.1095(4) 0.0529(12) Uani 1 1 d . . . H13 H 0.1654 0.0620 -0.1937 0.064 Uiso 1 1 calc R . . C11 C -0.1004(5) -0.00326(9) -0.3982(4) 0.0517(12) Uani 1 1 d . . . H11 H -0.1470 0.0013 -0.4837 0.062 Uiso 1 1 calc R . . N6 N 0.5404(5) 0.14457(8) 0.6223(4) 0.0663(11) Uani 1 1 d . . . C67 C 0.5321(5) 0.01145(9) -0.1988(4) 0.0495(12) Uani 1 1 d . . . C60 C 0.9672(5) 0.11501(10) 0.0153(4) 0.0600(13) Uani 1 1 d . . . H60 H 1.0432 0.1247 -0.0005 0.072 Uiso 1 1 calc R . . N8 N 0.1845(5) -0.06999(9) -0.4235(4) 0.0721(12) Uani 1 1 d . . . C26 C 0.6220(5) 0.16458(10) 0.5936(4) 0.0526(12) Uani 1 1 d . . . C25 C 0.6138(5) 0.16381(9) 0.2259(4) 0.0516(12) Uani 1 1 d . . . H25 H 0.6169 0.1643 0.1463 0.062 Uiso 1 1 calc R . . N3 N 1.0523(5) 0.14928(8) 0.5808(4) 0.0653(12) Uani 1 1 d . . . C61 C 0.8864(5) 0.09372(10) -0.0664(4) 0.0590(13) Uani 1 1 d . . . H61 H 0.9094 0.0893 -0.1356 0.071 Uiso 1 1 calc R . . C18 C 0.3968(5) 0.12481(10) 0.0311(4) 0.0598(13) Uani 1 1 d . . . H18 H 0.4228 0.1417 0.0019 0.072 Uiso 1 1 calc R . . C9 C 0.0485(5) 0.01142(9) -0.1815(4) 0.0452(11) Uani 1 1 d . . . C66 C 0.6002(5) 0.03660(10) -0.1197(4) 0.0557(13) Uani 1 1 d . . . H66 H 0.5689 0.0400 -0.0541 0.067 Uiso 1 1 calc R . . C63 C 0.7387(5) 0.08656(9) 0.0559(4) 0.0555(13) Uani 1 1 d . . . H63 H 0.6605 0.0773 0.0701 0.067 Uiso 1 1 calc R . . C65 C 0.6984(5) 0.05456(10) -0.1300(4) 0.0561(13) Uani 1 1 d . . . H65 H 0.7253 0.0517 -0.1984 0.067 Uiso 1 1 calc R . . C49 C 1.1979(5) 0.18515(9) 0.2643(4) 0.0483(12) Uani 1 1 d . . . C36 C 0.9493(6) 0.24692(10) 0.2281(6) 0.0699(15) Uani 1 1 d . . . H36 H 1.0025 0.2608 0.2044 0.084 Uiso 1 1 calc R . . C12 C 0.1385(5) 0.03257(9) -0.0885(4) 0.0530(12) Uani 1 1 d . . . H12 H 0.1632 0.0279 -0.0042 0.064 Uiso 1 1 calc R . . C16 C 0.3967(5) 0.09568(10) 0.1978(4) 0.0579(13) Uani 1 1 d . . . H16 H 0.4225 0.0926 0.2835 0.069 Uiso 1 1 calc R . . C19 C 0.3190(5) 0.10419(10) -0.0546(4) 0.0593(13) Uani 1 1 d . . . H19 H 0.2933 0.1073 -0.1403 0.071 Uiso 1 1 calc R . . C68 C 0.4137(5) -0.00299(10) -0.1848(4) 0.0563(13) Uani 1 1 d . . . H68 H 0.3824 0.0028 -0.1216 0.068 Uiso 1 1 calc R . . N11 N -0.2166(5) -0.07824(9) -0.4123(4) 0.0736(13) Uani 1 1 d . . . C33 C 0.8762(5) 0.22488(10) 0.3787(4) 0.0584(13) Uani 1 1 d . . . H33 H 0.8800 0.2236 0.4605 0.070 Uiso 1 1 calc R . . C54 C 1.4728(6) 0.24460(10) 0.2936(5) 0.0653(14) Uani 1 1 d . . . H54 H 1.5399 0.2566 0.3551 0.078 Uiso 1 1 calc R . . C10 C -0.0223(5) 0.01745(9) -0.3105(4) 0.0524(12) Uani 1 1 d . . . H10 H -0.0168 0.0359 -0.3384 0.063 Uiso 1 1 calc R . . C75 C 0.3269(6) -0.06946(11) -0.5332(5) 0.0644(14) Uani 1 1 d . . . H75 H 0.4034 -0.0643 -0.5603 0.077 Uiso 1 1 calc R . . C38 C 1.0535(6) 0.15111(11) 0.6954(5) 0.0783(16) Uani 1 1 d . . . H38 H 0.9959 0.1380 0.7184 0.094 Uiso 1 1 calc R . . C15 C 0.3187(5) 0.07481(10) 0.1121(4) 0.0575(13) Uani 1 1 d . . . H15 H 0.2932 0.0579 0.1411 0.069 Uiso 1 1 calc R . . N12 N -0.3019(5) -0.07617(10) -0.6233(4) 0.0773(13) Uani 1 1 d . . . N9 N 0.2233(5) -0.08937(9) -0.5866(4) 0.0742(13) Uani 1 1 d . . . C4 C -0.2384(6) -0.05169(11) -0.5724(5) 0.0744(16) Uani 1 1 d . . . H4 H -0.2307 -0.0360 -0.6187 0.089 Uiso 1 1 calc R . . C53 C 1.3880(5) 0.22477(10) 0.3253(4) 0.0589(13) Uani 1 1 d . . . H53 H 1.3975 0.2231 0.4086 0.071 Uiso 1 1 calc R . . N2 N 1.2706(5) 0.20925(9) 0.1116(4) 0.0731(13) Uani 1 1 d . . . C27 C 0.7110(6) 0.18424(11) 0.6809(5) 0.0737(15) Uani 1 1 d . . . H27 H 0.7647 0.1982 0.6582 0.088 Uiso 1 1 calc R . . C40 C 1.2192(6) 0.19019(12) 0.7495(5) 0.0815(17) Uani 1 1 d . . . H40 H 1.2772 0.2039 0.8068 0.098 Uiso 1 1 calc R . . C1 C -0.2837(6) -0.09146(11) -0.5206(5) 0.0694(15) Uani 1 1 d . . . H1 H -0.3165 -0.1103 -0.5256 0.083 Uiso 1 1 calc R . . C35 C 0.8596(6) 0.22720(11) 0.1421(5) 0.0758(16) Uani 1 1 d . . . H35 H 0.8547 0.2281 0.0599 0.091 Uiso 1 1 calc R . . C55 C 1.4581(6) 0.24666(10) 0.1710(5) 0.0681(15) Uani 1 1 d . . . H55 H 1.5149 0.2598 0.1472 0.082 Uiso 1 1 calc R . . C71 C 0.5794(5) 0.00120(10) -0.2910(4) 0.0559(12) Uani 1 1 d . . . H71 H 0.6616 0.0100 -0.3010 0.067 Uiso 1 1 calc R . . C37 C 0.9582(6) 0.24560(11) 0.3496(6) 0.0716(15) Uani 1 1 d . . . H37 H 1.0184 0.2585 0.4107 0.086 Uiso 1 1 calc R . . C41 C 1.2185(6) 0.18889(10) 0.6296(5) 0.0711(15) Uani 1 1 d . . . H41 H 1.2749 0.2019 0.6048 0.085 Uiso 1 1 calc R . . C74 C 0.1392(7) -0.08876(12) -0.5168(5) 0.0822(17) Uani 1 1 d . . . H74 H 0.0553 -0.1007 -0.5328 0.099 Uiso 1 1 calc R . . C30 C 0.5510(6) 0.14388(12) 0.7413(5) 0.0803(17) Uani 1 1 d . . . H30 H 0.4947 0.1301 0.7623 0.096 Uiso 1 1 calc R . . C56 C 1.3577(7) 0.22882(12) 0.0857(5) 0.0843(17) Uani 1 1 d . . . H56 H 1.3481 0.2302 0.0024 0.101 Uiso 1 1 calc R . . C28 C 0.7186(7) 0.18277(12) 0.8031(5) 0.0867(18) Uani 1 1 d . . . H28 H 0.7777 0.1959 0.8634 0.104 Uiso 1 1 calc R . . C39 C 1.1346(6) 0.17122(12) 0.7824(5) 0.0746(16) Uani 1 1 d . . . H39 H 1.1315 0.1718 0.8621 0.090 Uiso 1 1 calc R . . C29 C 0.6401(7) 0.16225(13) 0.8352(5) 0.0831(18) Uani 1 1 d . . . H29 H 0.6461 0.1606 0.9175 0.100 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 N4 0.058(2) 0.043(2) 0.050(2) -0.0030(19) 0.024(2) -0.0012(19) N1 0.057(2) 0.046(2) 0.051(3) 0.0012(19) 0.023(2) 0.008(2) N7 0.056(3) 0.053(3) 0.049(2) -0.001(2) 0.023(2) -0.004(2) C17 0.049(3) 0.042(3) 0.045(3) 0.000(2) 0.021(2) 0.000(2) C22 0.058(3) 0.048(3) 0.043(3) 0.000(2) 0.019(2) 0.009(3) N10 0.051(2) 0.049(3) 0.044(2) -0.001(2) 0.0167(19) -0.0043(19) C24 0.052(3) 0.039(3) 0.051(3) 0.001(2) 0.022(2) 0.003(2) C51 0.053(3) 0.040(3) 0.053(3) -0.003(2) 0.020(2) 0.008(2) C59 0.055(3) 0.043(3) 0.048(3) -0.002(2) 0.024(2) 0.004(2) N5 0.076(3) 0.055(3) 0.067(3) -0.002(2) 0.036(2) -0.011(2) C20 0.052(3) 0.044(3) 0.042(3) 0.000(2) 0.020(2) 0.001(2) C72 0.047(3) 0.055(3) 0.043(3) 0.002(2) 0.018(2) 0.002(2) C47 0.061(3) 0.045(3) 0.046(3) -0.001(2) 0.025(2) 0.004(2) C14 0.054(3) 0.041(3) 0.046(3) -0.003(2) 0.022(2) -0.002(2) C21 0.059(3) 0.043(3) 0.053(3) 0.004(2) 0.020(2) 0.001(2) C6 0.039(2) 0.043(3) 0.045(3) 0.000(2) 0.018(2) 0.000(2) C69 0.049(3) 0.063(3) 0.053(3) 0.002(3) 0.024(2) -0.002(3) C62 0.050(3) 0.054(3) 0.041(3) 0.000(2) 0.011(2) 0.004(2) C8 0.055(3) 0.054(3) 0.042(3) 0.006(2) 0.020(2) 0.002(2) C50 0.055(3) 0.052(3) 0.045(3) -0.001(2) 0.020(2) 0.007(2) C52 0.053(3) 0.046(3) 0.054(3) 0.001(2) 0.020(2) 0.005(2) C46 0.060(3) 0.044(3) 0.048(3) -0.002(2) 0.019(2) 0.004(2) C7 0.056(3) 0.046(3) 0.047(3) 0.006(2) 0.023(2) 0.003(2) C42 0.062(3) 0.042(3) 0.052(3) 0.000(2) 0.021(3) 0.004(3) C64 0.067(3) 0.052(3) 0.055(3) -0.012(2) 0.030(3) -0.003(3) C32 0.057(3) 0.036(3) 0.061(3) -0.002(3) 0.026(3) 0.001(2) C70 0.057(3) 0.059(3) 0.059(3) -0.006(3) 0.032(3) -0.004(3) C13 0.067(3) 0.045(3) 0.049(3) -0.003(2) 0.025(2) -0.004(3) C11 0.058(3) 0.049(3) 0.045(3) 0.005(2) 0.016(2) 0.000(2) N6 0.082(3) 0.068(3) 0.054(3) -0.002(2) 0.033(2) -0.011(2) C67 0.042(3) 0.053(3) 0.048(3) -0.006(2) 0.012(2) 0.000(2) C60 0.067(3) 0.061(3) 0.058(3) -0.015(3) 0.031(3) -0.013(3) N8 0.084(3) 0.073(3) 0.069(3) -0.011(2) 0.040(3) -0.027(3) C26 0.058(3) 0.047(3) 0.051(3) 0.002(3) 0.020(3) 0.006(3) C25 0.064(3) 0.048(3) 0.048(3) 0.000(2) 0.029(2) 0.000(3) N3 0.089(3) 0.057(3) 0.057(3) -0.005(2) 0.037(2) -0.014(2) C61 0.066(3) 0.065(3) 0.052(3) -0.006(3) 0.031(3) 0.000(3) C18 0.071(3) 0.058(3) 0.051(3) 0.002(3) 0.025(3) -0.016(3) C9 0.050(3) 0.038(3) 0.050(3) 0.001(2) 0.023(2) -0.001(2) C66 0.054(3) 0.061(3) 0.054(3) -0.005(3) 0.022(2) -0.001(3) C63 0.051(3) 0.055(3) 0.063(3) -0.003(3) 0.024(3) -0.007(2) C65 0.059(3) 0.064(3) 0.041(3) 0.000(2) 0.015(2) -0.003(3) C49 0.053(3) 0.044(3) 0.047(3) -0.002(2) 0.020(2) 0.004(2) C36 0.067(4) 0.052(3) 0.098(5) 0.008(3) 0.039(3) -0.008(3) C12 0.064(3) 0.048(3) 0.050(3) 0.000(2) 0.025(2) 0.003(3) C16 0.077(3) 0.052(3) 0.045(3) 0.002(2) 0.024(3) -0.005(3) C19 0.072(3) 0.064(3) 0.042(3) -0.003(3) 0.023(3) -0.016(3) C68 0.053(3) 0.062(3) 0.054(3) -0.009(3) 0.021(2) -0.009(3) N11 0.110(4) 0.048(3) 0.065(3) 0.001(2) 0.037(3) -0.016(2) C33 0.062(3) 0.050(3) 0.063(3) -0.005(3) 0.025(3) -0.006(3) C54 0.067(4) 0.055(3) 0.076(4) -0.006(3) 0.030(3) -0.003(3) C10 0.056(3) 0.043(3) 0.058(3) 0.003(2) 0.022(2) 0.001(2) C75 0.066(3) 0.073(4) 0.057(3) -0.010(3) 0.027(3) 0.002(3) C38 0.101(4) 0.072(4) 0.070(4) -0.008(3) 0.044(3) -0.016(3) C15 0.071(3) 0.051(3) 0.050(3) 0.004(3) 0.024(3) -0.009(3) N12 0.089(3) 0.070(3) 0.059(3) -0.007(3) 0.015(2) -0.015(3) N9 0.079(3) 0.062(3) 0.075(3) -0.013(2) 0.023(3) -0.001(3) C4 0.095(4) 0.065(4) 0.050(3) 0.005(3) 0.015(3) -0.015(3) C53 0.060(3) 0.058(3) 0.059(3) -0.003(3) 0.024(3) -0.005(3) N2 0.094(3) 0.072(3) 0.051(3) 0.001(2) 0.026(2) -0.017(3) C27 0.091(4) 0.075(4) 0.057(3) -0.014(3) 0.032(3) -0.016(3) C40 0.108(5) 0.083(4) 0.048(3) -0.022(3) 0.026(3) -0.015(4) C1 0.091(4) 0.050(3) 0.066(4) -0.012(3) 0.030(3) -0.016(3) C35 0.096(4) 0.063(4) 0.079(4) -0.002(3) 0.046(3) -0.019(3) C55 0.068(4) 0.055(3) 0.083(4) 0.008(3) 0.032(3) -0.007(3) C71 0.050(3) 0.063(3) 0.060(3) -0.003(3) 0.028(3) -0.008(3) C37 0.067(4) 0.059(4) 0.082(4) -0.009(3) 0.022(3) -0.008(3) C41 0.090(4) 0.060(4) 0.067(4) -0.011(3) 0.035(3) -0.015(3) C74 0.096(5) 0.074(4) 0.078(4) -0.013(3) 0.036(4) -0.027(4) C30 0.094(4) 0.095(5) 0.059(4) 0.004(3) 0.038(3) -0.006(4) C56 0.108(5) 0.084(4) 0.065(4) 0.013(3) 0.040(4) -0.028(4) C28 0.109(5) 0.098(5) 0.058(4) -0.021(3) 0.039(4) -0.017(4) C39 0.104(5) 0.068(4) 0.059(4) 0.009(3) 0.040(3) 0.008(3) C29 0.096(5) 0.109(5) 0.046(3) 0.003(3) 0.030(3) 0.002(4) _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 N4 C24 1.337(5) . ? N4 C22 1.340(5) . ? N1 C49 1.343(5) . ? N1 C47 1.346(5) . ? N7 C75 1.342(5) . ? N7 N8 1.360(5) . ? N7 C72 1.416(5) . ? C17 C18 1.374(5) . ? C17 C16 1.392(5) . ? C17 C20 1.489(5) . ? C22 C21 1.394(5) . ? C22 C26 1.500(6) . ? N10 C4 1.324(5) . ? N10 N11 1.348(5) . ? N10 C6 1.423(5) . ? C24 C25 1.383(5) . ? C24 C32 1.480(6) . ? C51 C46 1.385(5) . ? C51 C50 1.393(5) . ? C51 C59 1.473(6) . ? C59 C64 1.383(6) . ? C59 C60 1.384(5) . ? N5 C35 1.330(6) . ? N5 C32 1.334(5) . ? C20 C25 1.384(5) . ? C20 C21 1.399(5) . ? C72 C70 1.374(6) . ? C72 C69 1.384(5) . ? C47 C46 1.373(5) . ? C47 C42 1.486(6) . ? C14 C15 1.377(5) . ? C14 C19 1.388(5) . ? C14 C13 1.464(5) . ? C21 H21 0.9300 . ? C6 C7 1.375(5) . ? C6 C11 1.380(5) . ? C69 C68 1.381(5) . ? C69 H69 0.9300 . ? C62 C61 1.376(6) . ? C62 C63 1.404(6) . ? C62 C65 1.465(6) . ? C8 C7 1.377(5) . ? C8 C9 1.390(5) . ? C8 H8 0.9300 . ? C50 C49 1.385(5) . ? C50 H50 0.9300 . ? C52 N2 1.336(5) . ? C52 C53 1.379(6) . ? C52 C49 1.487(6) . ? C46 H46 0.9300 . ? C7 H7 0.9300 . ? C42 N3 1.326(5) . ? C42 C41 1.378(6) . ? C64 C63 1.383(5) . ? C64 H64 0.9300 . ? C32 C33 1.380(6) . ? C70 C71 1.375(6) . ? C70 H70 0.9300 . ? C13 C12 1.318(5) . ? C13 H13 0.9300 . ? C11 C10 1.384(5) . ? C11 H11 0.9300 . ? N6 C30 1.335(6) . ? N6 C26 1.340(5) . ? C67 C68 1.376(6) . ? C67 C71 1.394(6) . ? C67 C66 1.473(6) . ? C60 C61 1.377(6) . ? C60 H60 0.9300 . ? N8 C74 1.321(6) . ? C26 C27 1.378(6) . ? C25 H25 0.9300 . ? N3 C38 1.318(6) . ? C61 H61 0.9300 . ? C18 C19 1.369(6) . ? C18 H18 0.9300 . ? C9 C10 1.396(5) . ? C9 C12 1.460(5) . ? C66 C65 1.298(5) . ? C66 H66 0.9300 . ? C63 H63 0.9300 . ? C65 H65 0.9300 . ? C36 C37 1.370(6) . ? C36 C35 1.375(6) . ? C36 H36 0.9300 . ? C12 H12 0.9300 . ? C16 C15 1.377(6) . ? C16 H16 0.9300 . ? C19 H19 0.9300 . ? C68 H68 0.9300 . ? N11 C1 1.309(5) . ? C33 C37 1.368(6) . ? C33 H33 0.9300 . ? C54 C55 1.365(6) . ? C54 C53 1.373(6) . ? C54 H54 0.9300 . ? C10 H10 0.9300 . ? C75 N9 1.318(5) . ? C75 H75 0.9300 . ? C38 C39 1.368(6) . ? C38 H38 0.9300 . ? C15 H15 0.9300 . ? N12 C4 1.320(5) . ? N12 C1 1.335(6) . ? N9 C74 1.342(6) . ? C4 H4 0.9300 . ? C53 H53 0.9300 . ? N2 C56 1.346(6) . ? C27 C28 1.382(6) . ? C27 H27 0.9300 . ? C40 C39 1.351(6) . ? C40 C41 1.380(6) . ? C40 H40 0.9300 . ? C1 H1 0.9300 . ? C35 H35 0.9300 . ? C55 C56 1.352(6) . ? C55 H55 0.9300 . ? C71 H71 0.9300 . ? C37 H37 0.9300 . ? C41 H41 0.9300 . ? C74 H74 0.9300 . ? C30 C29 1.378(7) . ? C30 H30 0.9300 . ? C56 H56 0.9300 . ? C28 C29 1.356(7) . ? C28 H28 0.9300 . ? C39 H39 0.9300 . ? C29 H29 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 C24 N4 C22 117.3(4) . . ? C49 N1 C47 117.8(4) . . ? C75 N7 N8 108.2(4) . . ? C75 N7 C72 130.7(4) . . ? N8 N7 C72 121.0(4) . . ? C18 C17 C16 116.8(4) . . ? C18 C17 C20 122.3(4) . . ? C16 C17 C20 120.8(4) . . ? N4 C22 C21 123.1(4) . . ? N4 C22 C26 116.4(4) . . ? C21 C22 C26 120.5(5) . . ? C4 N10 N11 108.2(4) . . ? C4 N10 C6 129.4(4) . . ? N11 N10 C6 122.3(4) . . ? N4 C24 C25 123.0(4) . . ? N4 C24 C32 116.3(4) . . ? C25 C24 C32 120.6(4) . . ? C46 C51 C50 116.5(4) . . ? C46 C51 C59 121.7(4) . . ? C50 C51 C59 121.8(4) . . ? C64 C59 C60 116.8(4) . . ? C64 C59 C51 121.4(4) . . ? C60 C59 C51 121.8(4) . . ? C35 N5 C32 117.3(4) . . ? C25 C20 C21 116.7(4) . . ? C25 C20 C17 122.1(4) . . ? C21 C20 C17 121.2(4) . . ? C70 C72 C69 119.6(4) . . ? C70 C72 N7 121.2(4) . . ? C69 C72 N7 119.2(4) . . ? N1 C47 C46 122.6(4) . . ? N1 C47 C42 115.6(4) . . ? C46 C47 C42 121.8(4) . . ? C15 C14 C19 117.5(4) . . ? C15 C14 C13 122.4(4) . . ? C19 C14 C13 120.1(4) . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C7 C6 C11 120.3(4) . . ? C7 C6 N10 119.7(4) . . ? C11 C6 N10 120.0(4) . . ? C68 C69 C72 119.3(4) . . ? C68 C69 H69 120.3 . . ? C72 C69 H69 120.3 . . ? C61 C62 C63 117.4(4) . . ? C61 C62 C65 120.0(4) . . ? C63 C62 C65 122.5(4) . . ? C7 C8 C9 122.8(4) . . ? C7 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C49 C50 C51 120.4(4) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? N2 C52 C53 122.2(5) . . ? N2 C52 C49 117.3(4) . . ? C53 C52 C49 120.5(4) . . ? C47 C46 C51 120.7(4) . . ? C47 C46 H46 119.7 . . ? C51 C46 H46 119.7 . . ? C6 C7 C8 119.2(4) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? N3 C42 C41 121.2(5) . . ? N3 C42 C47 116.9(4) . . ? C41 C42 C47 121.9(5) . . ? C59 C64 C63 122.1(4) . . ? C59 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? N5 C32 C33 121.7(4) . . ? N5 C32 C24 117.2(4) . . ? C33 C32 C24 121.1(5) . . ? C72 C70 C71 119.9(4) . . ? C72 C70 H70 120.0 . . ? C71 C70 H70 120.0 . . ? C12 C13 C14 127.6(4) . . ? C12 C13 H13 116.2 . . ? C14 C13 H13 116.2 . . ? C6 C11 C10 119.6(4) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C30 N6 C26 117.1(4) . . ? C68 C67 C71 116.6(4) . . ? C68 C67 C66 120.0(4) . . ? C71 C67 C66 123.5(4) . . ? C61 C60 C59 121.8(5) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C74 N8 N7 102.9(4) . . ? N6 C26 C27 122.3(5) . . ? N6 C26 C22 116.5(4) . . ? C27 C26 C22 121.1(5) . . ? C24 C25 C20 120.5(4) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C38 N3 C42 118.4(4) . . ? C62 C61 C60 121.5(4) . . ? C62 C61 H61 119.2 . . ? C60 C61 H61 119.2 . . ? C19 C18 C17 122.0(4) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C8 C9 C10 116.3(4) . . ? C8 C9 C12 121.1(4) . . ? C10 C9 C12 122.5(4) . . ? C65 C66 C67 128.1(5) . . ? C65 C66 H66 115.9 . . ? C67 C66 H66 115.9 . . ? C64 C63 C62 120.3(4) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C66 C65 C62 128.4(5) . . ? C66 C65 H65 115.8 . . ? C62 C65 H65 115.8 . . ? N1 C49 C50 122.1(4) . . ? N1 C49 C52 115.9(4) . . ? C50 C49 C52 121.9(4) . . ? C37 C36 C35 118.4(5) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C13 C12 C9 128.0(4) . . ? C13 C12 H12 116.0 . . ? C9 C12 H12 116.0 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C19 C14 121.2(4) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? C67 C68 C69 122.6(4) . . ? C67 C68 H68 118.7 . . ? C69 C68 H68 118.7 . . ? C1 N11 N10 102.9(4) . . ? C37 C33 C32 120.3(5) . . ? C37 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C55 C54 C53 119.6(5) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C11 C10 C9 121.8(4) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N9 C75 N7 111.2(5) . . ? N9 C75 H75 124.4 . . ? N7 C75 H75 124.4 . . ? N3 C38 C39 123.8(5) . . ? N3 C38 H38 118.1 . . ? C39 C38 H38 118.1 . . ? C14 C15 C16 121.1(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C4 N12 C1 101.3(4) . . ? C75 N9 C74 102.6(4) . . ? N12 C4 N10 111.9(5) . . ? N12 C4 H4 124.1 . . ? N10 C4 H4 124.1 . . ? C54 C53 C52 119.2(5) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C52 N2 C56 116.2(5) . . ? C26 C27 C28 118.6(5) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C39 C40 C41 119.1(5) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? N11 C1 N12 115.7(5) . . ? N11 C1 H1 122.2 . . ? N12 C1 H1 122.2 . . ? N5 C35 C36 124.1(5) . . ? N5 C35 H35 118.0 . . ? C36 C35 H35 118.0 . . ? C56 C55 C54 117.4(5) . . ? C56 C55 H55 121.3 . . ? C54 C55 H55 121.3 . . ? C70 C71 C67 122.0(4) . . ? C70 C71 H71 119.0 . . ? C67 C71 H71 119.0 . . ? C33 C37 C36 118.2(5) . . ? C33 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C42 C41 C40 119.3(5) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? N8 C74 N9 115.0(5) . . ? N8 C74 H74 122.5 . . ? N9 C74 H74 122.5 . . ? N6 C30 C29 124.2(5) . . ? N6 C30 H30 117.9 . . ? C29 C30 H30 117.9 . . ? N2 C56 C55 125.3(5) . . ? N2 C56 H56 117.3 . . ? C55 C56 H56 117.3 . . ? C29 C28 C27 120.1(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C40 C39 C38 118.2(5) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C28 C29 C30 117.6(5) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? 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 C24 N4 C22 C21 -0.7(6) . . . . ? C24 N4 C22 C26 179.5(4) . . . . ? C22 N4 C24 C25 -0.5(6) . . . . ? C22 N4 C24 C32 179.1(4) . . . . ? C46 C51 C59 C64 21.5(6) . . . . ? C50 C51 C59 C64 -159.1(4) . . . . ? C46 C51 C59 C60 -157.8(4) . . . . ? C50 C51 C59 C60 21.5(6) . . . . ? C18 C17 C20 C25 -21.3(6) . . . . ? C16 C17 C20 C25 156.9(4) . . . . ? C18 C17 C20 C21 160.6(4) . . . . ? C16 C17 C20 C21 -21.3(6) . . . . ? C75 N7 C72 C70 -1.7(7) . . . . ? N8 N7 C72 C70 -177.6(4) . . . . ? C75 N7 C72 C69 177.3(4) . . . . ? N8 N7 C72 C69 1.4(6) . . . . ? C49 N1 C47 C46 0.2(6) . . . . ? C49 N1 C47 C42 -178.1(4) . . . . ? N4 C22 C21 C20 1.4(6) . . . . ? C26 C22 C21 C20 -178.8(4) . . . . ? C25 C20 C21 C22 -0.8(6) . . . . ? C17 C20 C21 C22 177.5(4) . . . . ? C4 N10 C6 C7 -169.2(5) . . . . ? N11 N10 C6 C7 8.6(6) . . . . ? C4 N10 C6 C11 11.5(7) . . . . ? N11 N10 C6 C11 -170.7(4) . . . . ? C70 C72 C69 C68 1.0(6) . . . . ? N7 C72 C69 C68 -178.0(4) . . . . ? C46 C51 C50 C49 1.1(6) . . . . ? C59 C51 C50 C49 -178.3(4) . . . . ? N1 C47 C46 C51 -0.2(7) . . . . ? C42 C47 C46 C51 178.0(4) . . . . ? C50 C51 C46 C47 -0.4(6) . . . . ? C59 C51 C46 C47 179.0(4) . . . . ? C11 C6 C7 C8 -1.0(6) . . . . ? N10 C6 C7 C8 179.7(4) . . . . ? C9 C8 C7 C6 -0.7(7) . . . . ? N1 C47 C42 N3 178.2(4) . . . . ? C46 C47 C42 N3 -0.2(6) . . . . ? N1 C47 C42 C41 -0.5(6) . . . . ? C46 C47 C42 C41 -178.8(4) . . . . ? C60 C59 C64 C63 1.5(7) . . . . ? C51 C59 C64 C63 -177.9(4) . . . . ? C35 N5 C32 C33 -0.2(7) . . . . ? C35 N5 C32 C24 179.1(4) . . . . ? N4 C24 C32 N5 -176.2(4) . . . . ? C25 C24 C32 N5 3.4(6) . . . . ? N4 C24 C32 C33 3.1(6) . . . . ? C25 C24 C32 C33 -177.3(4) . . . . ? C69 C72 C70 C71 -1.3(7) . . . . ? N7 C72 C70 C71 177.6(4) . . . . ? C15 C14 C13 C12 -0.9(7) . . . . ? C19 C14 C13 C12 -178.6(5) . . . . ? C7 C6 C11 C10 1.5(6) . . . . ? N10 C6 C11 C10 -179.2(4) . . . . ? C64 C59 C60 C61 -1.8(7) . . . . ? C51 C59 C60 C61 177.6(4) . . . . ? C75 N7 N8 C74 0.4(5) . . . . ? C72 N7 N8 C74 177.1(4) . . . . ? C30 N6 C26 C27 -1.5(7) . . . . ? C30 N6 C26 C22 176.5(4) . . . . ? N4 C22 C26 N6 -179.1(4) . . . . ? C21 C22 C26 N6 1.1(6) . . . . ? N4 C22 C26 C27 -1.1(6) . . . . ? C21 C22 C26 C27 179.1(4) . . . . ? N4 C24 C25 C20 1.1(6) . . . . ? C32 C24 C25 C20 -178.6(4) . . . . ? C21 C20 C25 C24 -0.3(6) . . . . ? C17 C20 C25 C24 -178.6(4) . . . . ? C41 C42 N3 C38 0.6(7) . . . . ? C47 C42 N3 C38 -178.1(4) . . . . ? C63 C62 C61 C60 1.5(7) . . . . ? C65 C62 C61 C60 -174.4(4) . . . . ? C59 C60 C61 C62 0.3(7) . . . . ? C16 C17 C18 C19 0.2(7) . . . . ? C20 C17 C18 C19 178.4(4) . . . . ? C7 C8 C9 C10 1.9(6) . . . . ? C7 C8 C9 C12 -176.0(4) . . . . ? C68 C67 C66 C65 -171.0(5) . . . . ? C71 C67 C66 C65 8.0(7) . . . . ? C59 C64 C63 C62 0.2(7) . . . . ? C61 C62 C63 C64 -1.7(6) . . . . ? C65 C62 C63 C64 174.1(4) . . . . ? C67 C66 C65 C62 -176.7(4) . . . . ? C61 C62 C65 C66 173.0(5) . . . . ? C63 C62 C65 C66 -2.6(7) . . . . ? C47 N1 C49 C50 0.5(6) . . . . ? C47 N1 C49 C52 -179.8(4) . . . . ? C51 C50 C49 N1 -1.2(6) . . . . ? C51 C50 C49 C52 179.2(4) . . . . ? N2 C52 C49 N1 -173.2(4) . . . . ? C53 C52 C49 N1 8.0(6) . . . . ? N2 C52 C49 C50 6.5(6) . . . . ? C53 C52 C49 C50 -172.3(4) . . . . ? C14 C13 C12 C9 179.3(4) . . . . ? C8 C9 C12 C13 165.1(4) . . . . ? C10 C9 C12 C13 -12.8(7) . . . . ? C18 C17 C16 C15 0.0(7) . . . . ? C20 C17 C16 C15 -178.2(4) . . . . ? C17 C18 C19 C14 0.0(7) . . . . ? C15 C14 C19 C18 -0.3(7) . . . . ? C13 C14 C19 C18 177.5(4) . . . . ? C71 C67 C68 C69 -2.8(6) . . . . ? C66 C67 C68 C69 176.3(4) . . . . ? C72 C69 C68 C67 1.2(7) . . . . ? C4 N10 N11 C1 0.3(5) . . . . ? C6 N10 N11 C1 -177.9(4) . . . . ? N5 C32 C33 C37 0.1(7) . . . . ? C24 C32 C33 C37 -179.2(4) . . . . ? C6 C11 C10 C9 -0.3(7) . . . . ? C8 C9 C10 C11 -1.4(6) . . . . ? C12 C9 C10 C11 176.5(4) . . . . ? N8 N7 C75 N9 -0.7(5) . . . . ? C72 N7 C75 N9 -177.0(4) . . . . ? C42 N3 C38 C39 -0.4(8) . . . . ? C19 C14 C15 C16 0.5(7) . . . . ? C13 C14 C15 C16 -177.3(4) . . . . ? C17 C16 C15 C14 -0.3(7) . . . . ? N7 C75 N9 C74 0.7(6) . . . . ? C1 N12 C4 N10 -0.6(6) . . . . ? N11 N10 C4 N12 0.2(6) . . . . ? C6 N10 C4 N12 178.2(4) . . . . ? C55 C54 C53 C52 -0.4(7) . . . . ? N2 C52 C53 C54 -0.4(7) . . . . ? C49 C52 C53 C54 178.4(4) . . . . ? C53 C52 N2 C56 1.1(7) . . . . ? C49 C52 N2 C56 -177.7(4) . . . . ? N6 C26 C27 C28 1.5(7) . . . . ? C22 C26 C27 C28 -176.5(4) . . . . ? N10 N11 C1 N12 -0.7(6) . . . . ? C4 N12 C1 N11 0.8(6) . . . . ? C32 N5 C35 C36 -0.2(8) . . . . ? C37 C36 C35 N5 0.6(8) . . . . ? C53 C54 C55 C56 0.5(7) . . . . ? C72 C70 C71 C67 -0.4(7) . . . . ? C68 C67 C71 C70 2.4(6) . . . . ? C66 C67 C71 C70 -176.6(4) . . . . ? C32 C33 C37 C36 0.3(7) . . . . ? C35 C36 C37 C33 -0.6(7) . . . . ? N3 C42 C41 C40 0.1(7) . . . . ? C47 C42 C41 C40 178.7(4) . . . . ? C39 C40 C41 C42 -0.9(8) . . . . ? N7 N8 C74 N9 0.0(6) . . . . ? C75 N9 C74 N8 -0.4(6) . . . . ? C26 N6 C30 C29 -0.2(8) . . . . ? C52 N2 C56 C55 -1.0(8) . . . . ? C54 C55 C56 N2 0.2(9) . . . . ? C26 C27 C28 C29 0.2(8) . . . . ? C41 C40 C39 C38 1.1(8) . . . . ? N3 C38 C39 C40 -0.5(9) . . . . ? C27 C28 C29 C30 -1.8(9) . . . . ? N6 C30 C29 C28 1.8(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.168 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.043 data_3939 _database_code_depnum_ccdc_archive 'CCDC 831609' #TrackingRef 'zfx3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H22 I2 N6 Zn' _chemical_formula_weight 797.77 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' Zn Zn 0.2839 1.4301 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.682(5) _cell_length_b 26.740(5) _cell_length_c 17.568(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 112.864(5) _cell_angle_gamma 90.000(5) _cell_volume 6355(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2405 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 19.35 _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 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 2.751 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4925 _exptl_absorpt_correction_T_max 0.6092 _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 '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 17809 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5596 _reflns_number_gt 2416 _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^+0.0716P] 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(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5596 _refine_ls_number_parameters 362 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1942 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.033 _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 I2 I -0.07313(9) 0.65052(3) -0.11600(5) 0.1218(5) Uani 1 1 d . . . Zn1 Zn -0.11737(10) 0.62611(4) 0.00972(7) 0.0843(5) Uani 1 1 d . . . I1 I -0.28560(7) 0.65309(3) 0.01208(8) 0.1397(5) Uani 1 1 d . . . N2 N -0.0193(6) 0.5836(3) 0.1068(5) 0.069(2) Uani 1 1 d . . . N4 N 0.6938(7) 0.2890(3) 0.8220(5) 0.089(3) Uani 1 1 d . . . C24 C -0.1922(8) 0.4457(4) -0.0517(7) 0.082(3) Uani 1 1 d . . . H24 H -0.2075 0.4118 -0.0595 0.098 Uiso 1 1 calc R . . N1 N -0.0255(8) 0.6801(3) 0.0968(6) 0.098(3) Uani 1 1 d . . . N3 N -0.1535(6) 0.5469(3) -0.0248(5) 0.078(2) Uani 1 1 d . . . C22 C -0.0989(7) 0.5124(3) 0.0300(6) 0.071(3) Uani 1 1 d . . . C27 C 0.0459(9) 0.6628(4) 0.1687(7) 0.084(3) Uani 1 1 d . . . C1 C 0.8016(10) 0.2776(6) 0.9363(8) 0.114(4) Uani 1 1 d . . . H1 H 0.8511 0.2832 0.9881 0.137 Uiso 1 1 calc R . . C28 C 0.1074(9) 0.6939(4) 0.2284(8) 0.103(4) Uani 1 1 d . . . H28 H 0.1544 0.6804 0.2763 0.123 Uiso 1 1 calc R . . N6 N 0.7717(9) 0.2305(4) 0.9091(8) 0.126(4) Uani 1 1 d . . . C3 C 0.6296(8) 0.3137(4) 0.7481(7) 0.084(3) Uani 1 1 d . . . C21 C 0.0464(7) 0.5058(3) 0.1682(6) 0.073(3) Uani 1 1 d . . . H21 H 0.0442 0.4712 0.1631 0.087 Uiso 1 1 calc R . . N5 N 0.7587(7) 0.3143(3) 0.8876(6) 0.093(3) Uani 1 1 d . . . C5 C 0.5658(14) 0.3901(5) 0.6798(12) 0.157(6) Uani 1 1 d . . . H5 H 0.5663 0.4248 0.6777 0.188 Uiso 1 1 calc R . . C13 C 0.2629(9) 0.5217(5) 0.3714(8) 0.117(4) Uani 1 1 d . . . H13 H 0.2658 0.5565 0.3750 0.141 Uiso 1 1 calc R . . C8 C 0.5707(9) 0.2885(4) 0.6831(7) 0.111(4) Uani 1 1 d . . . H8 H 0.5729 0.2537 0.6818 0.133 Uiso 1 1 calc R . . C17 C 0.1183(8) 0.5280(4) 0.2383(6) 0.081(3) Uani 1 1 d . . . C31 C -0.0354(10) 0.7329(4) 0.0868(8) 0.114(4) Uani 1 1 d . . . H31 H -0.0841 0.7460 0.0393 0.136 Uiso 1 1 calc R . . C14 C 0.1913(9) 0.5000(4) 0.3039(6) 0.087(3) Uani 1 1 d . . . C15 C 0.1863(10) 0.4471(4) 0.3021(7) 0.114(4) Uani 1 1 d . . . H15 H 0.1381 0.4299 0.2591 0.137 Uiso 1 1 calc R . . C25 C -0.2490(8) 0.4811(4) -0.1118(7) 0.089(3) Uani 1 1 d . . . H25 H -0.2988 0.4714 -0.1613 0.107 Uiso 1 1 calc R . . C2 C 0.7055(9) 0.2392(4) 0.8385(8) 0.103(4) Uani 1 1 d . . . H2 H 0.6692 0.2145 0.8021 0.124 Uiso 1 1 calc R . . C4 C 0.6312(9) 0.3654(4) 0.7529(7) 0.114(5) Uani 1 1 d . . . H4 H 0.6715 0.3827 0.7998 0.137 Uiso 1 1 calc R . . C19 C 0.0484(8) 0.6074(3) 0.1724(6) 0.071(3) Uani 1 1 d . . . C12 C 0.3307(10) 0.4941(7) 0.4340(8) 0.144(6) Uani 1 1 d . . . H12 H 0.3783 0.5116 0.4768 0.172 Uiso 1 1 calc R . . C18 C 0.1169(8) 0.5815(4) 0.2388(6) 0.085(3) Uani 1 1 d . . . H18 H 0.1617 0.5990 0.2835 0.102 Uiso 1 1 calc R . . C23 C -0.1170(8) 0.4609(4) 0.0158(7) 0.080(3) Uani 1 1 d . . . H23 H -0.0769 0.4377 0.0532 0.096 Uiso 1 1 calc R . . C20 C -0.0207(7) 0.5343(3) 0.1071(6) 0.069(3) Uani 1 1 d . . . C30 C 0.0255(11) 0.7651(5) 0.1460(10) 0.122(5) Uani 1 1 d . . . H30 H 0.0179 0.7995 0.1387 0.146 Uiso 1 1 calc R . . C10 C 0.4071(12) 0.4233(7) 0.5068(10) 0.188(6) Uani 1 1 d DU . . H10 H 0.4494 0.4480 0.5386 0.226 Uiso 1 1 calc R . . C26 C -0.2263(8) 0.5302(4) -0.0928(7) 0.094(4) Uani 1 1 d . . . H26 H -0.2646 0.5539 -0.1303 0.113 Uiso 1 1 calc R . . C16 C 0.2578(13) 0.4219(5) 0.3686(10) 0.154(7) Uani 1 1 d . . . H16 H 0.2559 0.3872 0.3674 0.185 Uiso 1 1 calc R . . C6 C 0.5017(11) 0.3640(8) 0.6120(8) 0.125(6) Uani 1 1 d D . . C7 C 0.5056(11) 0.3153(7) 0.6168(8) 0.124(5) Uani 1 1 d . . . H7 H 0.4614 0.2972 0.5726 0.149 Uiso 1 1 calc R . . C9 C 0.4338(13) 0.3823(7) 0.5388(11) 0.197(6) Uani 1 1 d DU . . H9 H 0.3986 0.3566 0.5042 0.236 Uiso 1 1 calc R . . C29 C 0.1002(10) 0.7451(5) 0.2183(9) 0.115(4) Uani 1 1 d . . . H29 H 0.1435 0.7662 0.2581 0.138 Uiso 1 1 calc R . . C11 C 0.3334(13) 0.4447(9) 0.4380(11) 0.171(6) Uani 1 1 d DU . . 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 I2 0.1961(11) 0.0719(5) 0.0806(6) 0.0140(4) 0.0353(6) 0.0040(5) Zn1 0.0915(10) 0.0621(7) 0.0746(8) 0.0103(6) 0.0053(7) 0.0163(6) I1 0.1043(8) 0.0952(7) 0.2015(12) 0.0078(6) 0.0397(7) 0.0307(5) N2 0.078(6) 0.055(4) 0.061(5) 0.001(4) 0.013(5) 0.017(4) N4 0.092(7) 0.065(5) 0.079(6) 0.010(5) -0.001(5) 0.012(5) C24 0.076(8) 0.071(7) 0.090(8) 0.002(6) 0.025(7) -0.002(6) N1 0.129(8) 0.058(5) 0.100(7) 0.007(5) 0.035(7) 0.018(5) N3 0.079(6) 0.060(5) 0.074(5) 0.007(4) 0.005(5) 0.008(4) C22 0.073(7) 0.063(6) 0.065(6) -0.002(5) 0.013(6) 0.017(5) C27 0.095(9) 0.067(6) 0.085(8) -0.004(6) 0.030(7) 0.010(6) C1 0.101(10) 0.128(12) 0.081(9) -0.009(9) 0.000(8) 0.002(9) C28 0.119(10) 0.067(7) 0.096(9) -0.007(6) 0.014(8) 0.008(7) N6 0.125(9) 0.106(9) 0.098(8) 0.033(7) -0.010(7) 0.015(7) C3 0.096(8) 0.056(6) 0.081(8) 0.024(6) 0.015(7) 0.025(6) C21 0.085(7) 0.054(5) 0.055(6) 0.008(5) 0.001(6) 0.012(5) N5 0.084(7) 0.087(6) 0.067(6) 0.002(5) -0.014(5) -0.001(5) C5 0.195(17) 0.084(9) 0.161(16) 0.054(10) 0.035(14) 0.061(10) C13 0.085(9) 0.122(10) 0.097(10) 0.013(8) -0.016(8) 0.006(8) C8 0.130(11) 0.072(7) 0.071(8) -0.014(6) -0.026(7) 0.003(7) C17 0.104(9) 0.064(6) 0.070(7) 0.008(5) 0.027(7) 0.017(6) C31 0.150(12) 0.078(8) 0.097(9) 0.008(7) 0.031(9) 0.013(8) C14 0.104(9) 0.083(7) 0.064(7) 0.022(6) 0.022(7) 0.038(7) C15 0.144(12) 0.090(8) 0.079(8) 0.016(6) 0.010(8) 0.050(8) C25 0.077(8) 0.088(8) 0.088(8) -0.006(7) 0.016(7) 0.003(6) C2 0.107(10) 0.070(7) 0.108(10) 0.007(7) 0.015(9) 0.007(7) C4 0.119(10) 0.083(8) 0.086(8) 0.005(6) -0.020(7) -0.001(7) C19 0.083(7) 0.057(5) 0.070(7) 0.016(5) 0.027(6) 0.017(5) C12 0.097(10) 0.215(18) 0.089(10) 0.076(11) 0.003(8) 0.050(11) C18 0.090(8) 0.077(7) 0.074(7) 0.003(6) 0.015(6) 0.016(6) C23 0.083(8) 0.072(7) 0.066(7) 0.008(5) 0.009(6) 0.006(6) C20 0.075(7) 0.050(5) 0.077(7) -0.003(5) 0.024(6) 0.011(5) C30 0.142(13) 0.080(8) 0.142(13) -0.039(9) 0.053(11) -0.019(9) C10 0.141(10) 0.270(16) 0.155(10) 0.095(10) 0.060(8) 0.111(10) C26 0.086(8) 0.073(7) 0.082(8) 0.000(6) -0.011(7) 0.008(6) C16 0.205(17) 0.101(10) 0.123(12) 0.032(9) 0.027(12) 0.088(11) C6 0.087(10) 0.191(16) 0.072(9) 0.028(11) 0.004(7) 0.076(11) C7 0.127(12) 0.148(13) 0.068(8) -0.002(9) 0.005(8) 0.031(11) C9 0.151(11) 0.280(17) 0.165(11) 0.091(11) 0.066(10) 0.107(11) C29 0.124(11) 0.083(9) 0.101(10) -0.022(7) 0.004(9) -0.005(8) C11 0.138(11) 0.251(16) 0.117(10) 0.113(10) 0.043(9) 0.111(10) _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 I2 Zn1 2.6155(17) . ? Zn1 N2 2.088(7) . ? Zn1 N1 2.153(9) . ? Zn1 N3 2.210(8) . ? Zn1 I1 2.5890(19) . ? N2 C20 1.319(10) . ? N2 C19 1.353(11) . ? N4 C2 1.359(12) . ? N4 N5 1.355(11) . ? N4 C3 1.435(12) . ? C24 C23 1.331(12) . ? C24 C25 1.424(14) . ? C24 H24 0.9300 . ? N1 C27 1.371(13) . ? N1 C31 1.424(13) . ? N3 C22 1.350(11) . ? N3 C26 1.334(12) . ? C22 C23 1.406(13) . ? C22 C20 1.513(13) . ? C27 C28 1.367(14) . ? C27 C19 1.485(13) . ? C1 N5 1.294(14) . ? C1 N6 1.357(16) . ? C1 H1 0.9300 . ? C28 C29 1.379(14) . ? C28 H28 0.9300 . ? N6 C2 1.266(14) . ? C3 C8 1.319(13) . ? C3 C4 1.384(14) . ? C21 C20 1.372(12) . ? C21 C17 1.405(13) . ? C21 H21 0.9300 . ? C5 C6 1.38(2) . ? C5 C4 1.432(18) . ? C5 H5 0.9300 . ? C13 C14 1.373(14) . ? C13 C12 1.376(16) . ? C13 H13 0.9300 . ? C8 C7 1.385(16) . ? C8 H8 0.9300 . ? C17 C14 1.441(13) . ? C17 C18 1.433(14) . ? C31 C30 1.378(16) . ? C31 H31 0.9300 . ? C14 C15 1.416(14) . ? C15 C16 1.403(17) . ? C15 H15 0.9300 . ? C25 C26 1.362(13) . ? C25 H25 0.9300 . ? C2 H2 0.9300 . ? C4 H4 0.9300 . ? C19 C18 1.392(13) . ? C12 C11 1.32(3) . ? C12 H12 0.9300 . ? C18 H18 0.9300 . ? C23 H23 0.9300 . ? C30 C29 1.420(19) . ? C30 H30 0.9300 . ? C10 C9 1.224(9) . ? C10 C11 1.394(14) . ? C10 H10 0.9300 . ? C26 H26 0.9300 . ? C16 C11 1.43(2) . ? C16 H16 0.9300 . ? C6 C7 1.31(2) . ? C6 C9 1.375(15) . ? C7 H7 0.9300 . ? C9 H9 0.9300 . ? C29 H29 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 Zn1 N1 75.0(3) . . ? N2 Zn1 N3 73.6(3) . . ? N1 Zn1 N3 148.7(3) . . ? N2 Zn1 I1 119.8(2) . . ? N1 Zn1 I1 98.1(3) . . ? N3 Zn1 I1 98.2(2) . . ? N2 Zn1 I2 120.4(2) . . ? N1 Zn1 I2 98.1(3) . . ? N3 Zn1 I2 96.8(2) . . ? I1 Zn1 I2 119.70(5) . . ? C20 N2 C19 118.2(8) . . ? C20 N2 Zn1 122.7(7) . . ? C19 N2 Zn1 119.1(6) . . ? C2 N4 N5 108.5(9) . . ? C2 N4 C3 128.9(10) . . ? N5 N4 C3 122.5(8) . . ? C23 C24 C25 120.0(10) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C27 N1 C31 116.9(10) . . ? C27 N1 Zn1 118.3(7) . . ? C31 N1 Zn1 124.8(8) . . ? C22 N3 C26 117.2(8) . . ? C22 N3 Zn1 116.6(6) . . ? C26 N3 Zn1 126.2(7) . . ? N3 C22 C23 121.6(9) . . ? N3 C22 C20 114.0(8) . . ? C23 C22 C20 124.3(9) . . ? C28 C27 N1 122.9(10) . . ? C28 C27 C19 125.2(10) . . ? N1 C27 C19 111.9(9) . . ? N5 C1 N6 117.6(11) . . ? N5 C1 H1 121.2 . . ? N6 C1 H1 121.2 . . ? C29 C28 C27 120.6(11) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C2 N6 C1 101.2(11) . . ? C8 C3 C4 123.6(10) . . ? C8 C3 N4 121.9(9) . . ? C4 C3 N4 114.5(10) . . ? C20 C21 C17 121.3(9) . . ? C20 C21 H21 119.4 . . ? C17 C21 H21 119.4 . . ? C1 N5 N4 100.7(9) . . ? C6 C5 C4 122.2(13) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C14 C13 C12 122.4(14) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C3 C8 C7 118.0(11) . . ? C3 C8 H8 121.0 . . ? C7 C8 H8 121.0 . . ? C14 C17 C21 123.6(9) . . ? C14 C17 C18 121.5(10) . . ? C21 C17 C18 114.8(9) . . ? C30 C31 N1 121.4(12) . . ? C30 C31 H31 119.3 . . ? N1 C31 H31 119.3 . . ? C13 C14 C17 123.5(11) . . ? C13 C14 C15 117.3(10) . . ? C17 C14 C15 119.0(11) . . ? C14 C15 C16 116.4(12) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C26 C25 C24 116.2(10) . . ? C26 C25 H25 121.9 . . ? C24 C25 H25 121.9 . . ? N6 C2 N4 112.0(11) . . ? N6 C2 H2 124.0 . . ? N4 C2 H2 124.0 . . ? C3 C4 C5 114.6(11) . . ? C3 C4 H4 122.7 . . ? C5 C4 H4 122.7 . . ? N2 C19 C18 122.3(9) . . ? N2 C19 C27 115.7(8) . . ? C18 C19 C27 122.0(10) . . ? C13 C12 C11 125.2(17) . . ? C13 C12 H12 117.4 . . ? C11 C12 H12 117.4 . . ? C19 C18 C17 119.9(10) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C23 C22 119.5(10) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? N2 C20 C21 123.5(9) . . ? N2 C20 C22 113.0(8) . . ? C21 C20 C22 123.4(8) . . ? C31 C30 C29 119.3(12) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C9 C10 C11 140(2) . . ? C9 C10 H10 109.9 . . ? C11 C10 H10 109.9 . . ? N3 C26 C25 125.3(10) . . ? N3 C26 H26 117.4 . . ? C25 C26 H26 117.4 . . ? C11 C16 C15 126.1(14) . . ? C11 C16 H16 117.0 . . ? C15 C16 H16 117.0 . . ? C5 C6 C7 116.7(12) . . ? C5 C6 C9 129(2) . . ? C7 C6 C9 114.4(19) . . ? C6 C7 C8 124.6(13) . . ? C6 C7 H7 117.7 . . ? C8 C7 H7 117.7 . . ? C10 C9 C6 137(2) . . ? C10 C9 H9 111.4 . . ? C6 C9 H9 111.4 . . ? C28 C29 C30 118.8(12) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C16 C11 C10 130(2) . . ? C16 C11 C12 112.6(12) . . ? C10 C11 C12 117(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 N1 Zn1 N2 C20 -179.7(8) . . . . ? N3 Zn1 N2 C20 -0.7(7) . . . . ? I1 Zn1 N2 C20 89.5(7) . . . . ? I2 Zn1 N2 C20 -89.1(8) . . . . ? N1 Zn1 N2 C19 0.5(7) . . . . ? N3 Zn1 N2 C19 179.5(8) . . . . ? I1 Zn1 N2 C19 -90.3(7) . . . . ? I2 Zn1 N2 C19 91.1(7) . . . . ? N2 Zn1 N1 C27 -1.1(8) . . . . ? N3 Zn1 N1 C27 -2.9(12) . . . . ? I1 Zn1 N1 C27 117.7(8) . . . . ? I2 Zn1 N1 C27 -120.6(8) . . . . ? N2 Zn1 N1 C31 -178.8(10) . . . . ? N3 Zn1 N1 C31 179.4(8) . . . . ? I1 Zn1 N1 C31 -60.0(9) . . . . ? I2 Zn1 N1 C31 61.7(9) . . . . ? N2 Zn1 N3 C22 0.4(7) . . . . ? N1 Zn1 N3 C22 2.2(11) . . . . ? I1 Zn1 N3 C22 -118.4(7) . . . . ? I2 Zn1 N3 C22 120.2(7) . . . . ? N2 Zn1 N3 C26 177.6(10) . . . . ? N1 Zn1 N3 C26 179.4(9) . . . . ? I1 Zn1 N3 C26 58.8(9) . . . . ? I2 Zn1 N3 C26 -62.7(9) . . . . ? C26 N3 C22 C23 0.7(15) . . . . ? Zn1 N3 C22 C23 178.2(8) . . . . ? C26 N3 C22 C20 -177.6(9) . . . . ? Zn1 N3 C22 C20 -0.1(11) . . . . ? C31 N1 C27 C28 -1.4(17) . . . . ? Zn1 N1 C27 C28 -179.2(9) . . . . ? C31 N1 C27 C19 179.4(10) . . . . ? Zn1 N1 C27 C19 1.5(12) . . . . ? N1 C27 C28 C29 -0.4(19) . . . . ? C19 C27 C28 C29 178.7(11) . . . . ? N5 C1 N6 C2 0.0(18) . . . . ? C2 N4 C3 C8 -0.3(19) . . . . ? N5 N4 C3 C8 176.2(12) . . . . ? C2 N4 C3 C4 176.4(12) . . . . ? N5 N4 C3 C4 -7.1(16) . . . . ? N6 C1 N5 N4 0.3(16) . . . . ? C2 N4 N5 C1 -0.5(13) . . . . ? C3 N4 N5 C1 -177.6(11) . . . . ? C4 C3 C8 C7 -1(2) . . . . ? N4 C3 C8 C7 175.0(12) . . . . ? C20 C21 C17 C14 -179.2(10) . . . . ? C20 C21 C17 C18 -1.7(15) . . . . ? C27 N1 C31 C30 1.4(18) . . . . ? Zn1 N1 C31 C30 179.1(10) . . . . ? C12 C13 C14 C17 178.8(12) . . . . ? C12 C13 C14 C15 3(2) . . . . ? C21 C17 C14 C13 178.4(12) . . . . ? C18 C17 C14 C13 1.1(18) . . . . ? C21 C17 C14 C15 -5.6(17) . . . . ? C18 C17 C14 C15 177.1(11) . . . . ? C13 C14 C15 C16 -2.2(19) . . . . ? C17 C14 C15 C16 -178.4(12) . . . . ? C23 C24 C25 C26 -4.6(16) . . . . ? C1 N6 C2 N4 -0.3(16) . . . . ? N5 N4 C2 N6 0.5(15) . . . . ? C3 N4 C2 N6 177.4(12) . . . . ? C8 C3 C4 C5 -2(2) . . . . ? N4 C3 C4 C5 -178.9(13) . . . . ? C6 C5 C4 C3 4(2) . . . . ? C20 N2 C19 C18 1.0(15) . . . . ? Zn1 N2 C19 C18 -179.2(8) . . . . ? C20 N2 C19 C27 -179.6(9) . . . . ? Zn1 N2 C19 C27 0.1(11) . . . . ? C28 C27 C19 N2 179.7(11) . . . . ? N1 C27 C19 N2 -1.1(13) . . . . ? C28 C27 C19 C18 -1.0(17) . . . . ? N1 C27 C19 C18 178.3(10) . . . . ? C14 C13 C12 C11 -2(2) . . . . ? N2 C19 C18 C17 1.2(16) . . . . ? C27 C19 C18 C17 -178.1(10) . . . . ? C14 C17 C18 C19 176.7(10) . . . . ? C21 C17 C18 C19 -0.8(15) . . . . ? C25 C24 C23 C22 4.6(16) . . . . ? N3 C22 C23 C24 -2.7(16) . . . . ? C20 C22 C23 C24 175.4(9) . . . . ? C19 N2 C20 C21 -3.8(15) . . . . ? Zn1 N2 C20 C21 176.4(8) . . . . ? C19 N2 C20 C22 -179.4(8) . . . . ? Zn1 N2 C20 C22 0.8(11) . . . . ? C17 C21 C20 N2 4.2(16) . . . . ? C17 C21 C20 C22 179.4(10) . . . . ? N3 C22 C20 N2 -0.4(13) . . . . ? C23 C22 C20 N2 -178.6(9) . . . . ? N3 C22 C20 C21 -176.0(10) . . . . ? C23 C22 C20 C21 5.7(16) . . . . ? N1 C31 C30 C29 0(2) . . . . ? C22 N3 C26 C25 -0.9(17) . . . . ? Zn1 N3 C26 C25 -178.1(9) . . . . ? C24 C25 C26 N3 2.8(18) . . . . ? C14 C15 C16 C11 1(2) . . . . ? C4 C5 C6 C7 -2(3) . . . . ? C4 C5 C6 C9 178.6(16) . . . . ? C5 C6 C7 C8 -2(3) . . . . ? C9 C6 C7 C8 177.4(14) . . . . ? C3 C8 C7 C6 4(2) . . . . ? C11 C10 C9 C6 -171(2) . . . . ? C5 C6 C9 C10 2(4) . . . . ? C7 C6 C9 C10 -178(2) . . . . ? C27 C28 C29 C30 2(2) . . . . ? C31 C30 C29 C28 -2(2) . . . . ? C15 C16 C11 C10 179.7(16) . . . . ? C15 C16 C11 C12 0(3) . . . . ? C9 C10 C11 C16 -6(4) . . . . ? C9 C10 C11 C12 174(2) . . . . ? C13 C12 C11 C16 1(3) . . . . ? C13 C12 C11 C10 -179.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.472 _refine_diff_density_min -1.315 _refine_diff_density_rms 0.109 data_40 _database_code_depnum_ccdc_archive 'CCDC 833135' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 Cl3 N8 S2 Zn' _chemical_formula_weight 778.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.4590(14) _cell_length_b 26.123(2) _cell_length_c 17.6798(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.5360(10) _cell_angle_gamma 90.00 _cell_volume 6859.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4446 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 18.77 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 40976 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11889 _reflns_number_gt 4762 _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0010(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11889 _refine_ls_number_parameters 866 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2210 _refine_ls_R_factor_gt 0.1086 _refine_ls_wR_factor_ref 0.3857 _refine_ls_wR_factor_gt 0.3013 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8874(8) -0.0119(5) 1.4768(8) 0.104(4) Uani 1 1 d . . . H1 H 0.8788 -0.0087 1.5252 0.125 Uiso 1 1 calc R . . C2 C 0.9064(8) -0.0460(4) 1.3814(8) 0.100(4) Uani 1 1 d . . . H2 H 0.9150 -0.0696 1.3462 0.121 Uiso 1 1 calc R . . C3 C 0.9124(8) 0.0339(4) 1.3048(6) 0.085(3) Uani 1 1 d . . . C4 C 0.8917(8) 0.0132(4) 1.2287(6) 0.093(3) Uani 1 1 d . . . H4 H 0.8700 -0.0201 1.2184 0.112 Uiso 1 1 calc R . . C5 C 0.9405(10) 0.0849(4) 1.3203(8) 0.112(4) Uani 1 1 d . . . H5 H 0.9516 0.1005 1.3711 0.135 Uiso 1 1 calc R . . C6 C 0.9515(11) 0.1121(5) 1.2557(11) 0.141(6) Uani 1 1 d . . . H6 H 0.9730 0.1455 1.2655 0.169 Uiso 1 1 calc R . . C7 C 0.9309(9) 0.0898(6) 1.1779(7) 0.108(4) Uani 1 1 d . . . C8 C 0.9013(9) 0.0393(5) 1.1667(8) 0.105(4) Uani 1 1 d . . . H8 H 0.8878 0.0231 1.1158 0.126 Uiso 1 1 calc R . . C9 C 0.9405(11) 0.1153(6) 1.1080(10) 0.138(6) Uani 1 1 d . . . H9 H 0.9345 0.0938 1.0639 0.166 Uiso 1 1 calc R . . C10 C 0.9538(11) 0.1562(7) 1.0995(12) 0.148(6) Uani 1 1 d . . . H10 H 0.9619 0.1771 1.1447 0.178 Uiso 1 1 calc R . . C11 C 0.9611(11) 0.1840(8) 1.0270(9) 0.130(5) Uani 1 1 d . . . C12 C 0.9822(13) 0.1596(6) 0.9706(11) 0.162(7) Uani 1 1 d . . . H12 H 0.9990 0.1253 0.9798 0.195 Uiso 1 1 calc R . . C13 C 0.9801(14) 0.1839(6) 0.8975(10) 0.169(7) Uani 1 1 d . . . H13 H 0.9904 0.1651 0.8578 0.203 Uiso 1 1 calc R . . C14 C 0.9631(8) 0.2344(4) 0.8870(8) 0.094(3) Uani 1 1 d . . . C15 C 0.9520(9) 0.2580(5) 0.9489(8) 0.107(4) Uani 1 1 d . . . H15 H 0.9434 0.2933 0.9459 0.128 Uiso 1 1 calc R . . C16 C 0.9529(10) 0.2321(7) 1.0175(9) 0.137(6) Uani 1 1 d . . . H16 H 0.9471 0.2512 1.0592 0.165 Uiso 1 1 calc R . . C17 C 0.9574(8) 0.2622(4) 0.8114(7) 0.085(3) Uani 1 1 d . . . C18 C 0.9593(7) 0.2371(4) 0.7442(7) 0.081(3) Uani 1 1 d . . . H18 H 0.9639 0.2016 0.7464 0.097 Uiso 1 1 calc R . . C19 C 0.9544(7) 0.2619(4) 0.6728(6) 0.076(3) Uani 1 1 d . . . C20 C 0.9533(7) 0.3155(4) 0.8079(7) 0.085(3) Uani 1 1 d . . . H20 H 0.9551 0.3344 0.8531 0.102 Uiso 1 1 calc R . . C21 C 0.9466(7) 0.3396(4) 0.7360(7) 0.079(3) Uani 1 1 d . . . C22 C 0.9390(7) 0.3971(4) 0.7231(7) 0.084(3) Uani 1 1 d . . . C23 C 0.9314(9) 0.4298(4) 0.7789(8) 0.111(4) Uani 1 1 d . . . H23 H 0.9316 0.4185 0.8288 0.133 Uiso 1 1 calc R . . C24 C 0.9234(11) 0.4804(5) 0.7576(10) 0.144(6) Uani 1 1 d . . . H24 H 0.9171 0.5044 0.7936 0.172 Uiso 1 1 calc R . . C25 C 0.9243(11) 0.4959(6) 0.6864(11) 0.141(6) Uani 1 1 d . . . H25 H 0.9199 0.5306 0.6737 0.169 Uiso 1 1 calc R . . C26 C 0.9316(9) 0.4614(5) 0.6315(9) 0.114(4) Uani 1 1 d . . . H26 H 0.9316 0.4725 0.5815 0.137 Uiso 1 1 calc R . . C27 C 0.9512(7) 0.2392(4) 0.5963(7) 0.081(3) Uani 1 1 d . . . C28 C 0.9468(8) 0.1863(4) 0.5811(7) 0.096(3) Uani 1 1 d . . . H28 H 0.9455 0.1634 0.6209 0.115 Uiso 1 1 calc R . . C29 C 0.9445(10) 0.1689(4) 0.5078(8) 0.110(4) Uani 1 1 d . . . H29 H 0.9429 0.1340 0.4973 0.132 Uiso 1 1 calc R . . C30 C 0.9444(10) 0.2037(5) 0.4491(8) 0.119(4) Uani 1 1 d . . . H30 H 0.9417 0.1927 0.3980 0.143 Uiso 1 1 calc R . . C31 C 0.9484(9) 0.2533(5) 0.4672(8) 0.107(4) Uani 1 1 d . . . H31 H 0.9489 0.2765 0.4274 0.129 Uiso 1 1 calc R . . C32 C 0.7661(9) 0.3701(3) 0.4022(7) 0.082(3) Uani 1 1 d . . . C33 C 1.0907(9) 0.4074(5) 0.5376(7) 0.098(4) Uani 1 1 d . . . C39 C 0.6795(11) 0.4476(5) -0.4692(9) 0.122(5) Uani 1 1 d . . . H39 H 0.6980 0.4440 -0.5117 0.146 Uiso 1 1 calc R . . C40 C 0.6207(11) 0.4796(5) -0.3963(9) 0.134(5) Uani 1 1 d . . . H40 H 0.5895 0.5013 -0.3765 0.161 Uiso 1 1 calc R . . C41 C 0.6833(7) 0.4176(4) -0.2786(7) 0.081(3) Uani 1 1 d . . . C42 C 0.7117(9) 0.3661(4) -0.2628(8) 0.103(4) Uani 1 1 d . . . H42 H 0.7280 0.3479 -0.2992 0.124 Uiso 1 1 calc R . . C43 C 0.7140(9) 0.3440(4) -0.1904(7) 0.104(4) Uani 1 1 d . . . H43 H 0.7281 0.3094 -0.1808 0.124 Uiso 1 1 calc R . . C44 C 0.6962(7) 0.3713(4) -0.1318(6) 0.077(3) Uani 1 1 d . . . C45 C 0.6763(10) 0.4194(5) -0.1494(8) 0.119(5) Uani 1 1 d . . . H45 H 0.6673 0.4389 -0.1096 0.143 Uiso 1 1 calc R . . C46 C 0.6674(10) 0.4443(4) -0.2214(7) 0.112(4) Uani 1 1 d . . . H46 H 0.6508 0.4786 -0.2301 0.134 Uiso 1 1 calc R . . C47 C 0.6970(7) 0.3477(5) -0.0541(7) 0.089(3) Uani 1 1 d . . . H47 H 0.6816 0.3685 -0.0196 0.107 Uiso 1 1 calc R . . C48 C 0.7177(8) 0.2998(5) -0.0311(7) 0.094(3) Uani 1 1 d . . . H48 H 0.7353 0.2803 -0.0654 0.113 Uiso 1 1 calc R . . C49 C 0.7167(8) 0.2731(5) 0.0412(7) 0.087(3) Uani 1 1 d . . . C50 C 0.7405(8) 0.2232(5) 0.0559(7) 0.097(4) Uani 1 1 d . . . H50 H 0.7600 0.2065 0.0202 0.117 Uiso 1 1 calc R . . C51 C 0.7370(7) 0.1960(5) 0.1210(7) 0.092(3) Uani 1 1 d . . . H51 H 0.7532 0.1616 0.1282 0.110 Uiso 1 1 calc R . . C52 C 0.7086(7) 0.2206(4) 0.1775(6) 0.079(3) Uani 1 1 d . . . C53 C 0.6853(8) 0.2729(4) 0.1633(7) 0.090(3) Uani 1 1 d . . . H53 H 0.6675 0.2904 0.1995 0.107 Uiso 1 1 calc R . . C54 C 0.6884(9) 0.2980(5) 0.0970(7) 0.105(4) Uani 1 1 d . . . H54 H 0.6716 0.3323 0.0882 0.125 Uiso 1 1 calc R . . C55 C 0.7042(7) 0.1921(4) 0.2484(6) 0.074(3) Uani 1 1 d . . . C56 C 0.6959(7) 0.1380(4) 0.2466(6) 0.080(3) Uani 1 1 d . . . H56 H 0.6950 0.1195 0.2012 0.096 Uiso 1 1 calc R . . C57 C 0.6892(6) 0.1127(4) 0.3123(6) 0.072(3) Uani 1 1 d . . . C58 C 0.7038(7) 0.2174(4) 0.3182(6) 0.079(3) Uani 1 1 d . . . H58 H 0.7075 0.2529 0.3219 0.095 Uiso 1 1 calc R . . C59 C 0.6979(6) 0.1887(4) 0.3813(6) 0.073(3) Uani 1 1 d . . . C60 C 0.6774(7) 0.0557(4) 0.3129(7) 0.075(3) Uani 1 1 d . . . C61 C 0.6777(8) 0.0244(4) 0.2515(7) 0.096(3) Uani 1 1 d . . . H61 H 0.6821 0.0372 0.2043 0.115 Uiso 1 1 calc R . . C62 C 0.6707(10) -0.0301(5) 0.2637(10) 0.124(5) Uani 1 1 d . . . H62 H 0.6738 -0.0538 0.2256 0.148 Uiso 1 1 calc R . . C63 C 0.6594(11) -0.0461(5) 0.3331(10) 0.125(5) Uani 1 1 d . . . H63 H 0.6512 -0.0806 0.3410 0.151 Uiso 1 1 calc R . . C64 C 0.6605(8) -0.0105(5) 0.3898(8) 0.101(4) Uani 1 1 d . . . H64 H 0.6534 -0.0219 0.4365 0.121 Uiso 1 1 calc R . . C65 C 0.7009(7) 0.2125(4) 0.4598(6) 0.084(3) Uani 1 1 d . . . C66 C 0.7036(8) 0.2643(4) 0.4746(6) 0.090(3) Uani 1 1 d . . . H66 H 0.7028 0.2875 0.4343 0.107 Uiso 1 1 calc R . . C67 C 0.7075(9) 0.2811(5) 0.5480(8) 0.107(4) Uani 1 1 d . . . H67 H 0.7112 0.3160 0.5590 0.128 Uiso 1 1 calc R . . C68 C 0.7059(9) 0.2476(5) 0.6065(7) 0.109(4) Uani 1 1 d . . . H68 H 0.7081 0.2586 0.6574 0.130 Uiso 1 1 calc R . . C69 C 0.7011(10) 0.1967(5) 0.5861(8) 0.122(5) Uani 1 1 d . . . H69 H 0.7011 0.1734 0.6258 0.146 Uiso 1 1 calc R . . C70 C 0.5177(10) 0.0923(5) 0.5053(8) 0.107(4) Uani 1 1 d . . . C71 C 0.8508(9) 0.0771(4) 0.6387(8) 0.079(3) Uani 1 1 d . . . C90 C 0.770(2) 0.1204(8) 0.8112(12) 0.250(14) Uani 1 1 d . . . H90 H 0.8313 0.1132 0.8177 0.300 Uiso 1 1 calc R . . C104 C 0.0236(10) 0.3240(3) 0.2543(7) 0.64(6) Uani 1 1 d D . . H104 H 0.0262 0.3414 0.2063 0.763 Uiso 1 1 d R . . Cl1 Cl 0.7473(6) 0.1872(2) 0.8084(4) 0.253(3) Uani 1 1 d . . . Cl2 Cl 0.6897(6) 0.0917(3) 0.7256(5) 0.265(4) Uani 1 1 d . . . Cl3 Cl 0.7520(7) 0.0993(3) 0.9012(5) 0.299(4) Uani 1 1 d . . . Cl4 Cl 0.0216(12) 0.3557(3) 0.3401(6) 0.416(9) Uani 1 1 d D . . Cl5 Cl 0.0426(8) 0.2604(3) 0.2862(6) 0.341(6) Uani 1 1 d D . . Cl6 Cl -0.0866(10) 0.3062(6) 0.2310(10) 0.479(10) Uani 1 1 d D . . N1 N 0.9031(6) 0.0048(3) 1.3693(5) 0.080(2) Uani 1 1 d . . . N2 N 0.8918(6) 0.0285(3) 1.4331(6) 0.087(2) Uani 1 1 d . . . N3 N 0.8965(7) -0.0583(4) 1.4463(6) 0.100(3) Uani 1 1 d . . . N4 N 0.9483(5) 0.3147(3) 0.6702(5) 0.076(2) Uani 1 1 d . . . N5 N 0.9517(6) 0.2720(3) 0.5387(6) 0.088(3) Uani 1 1 d . . . N6 N 0.9384(6) 0.4130(3) 0.6500(6) 0.091(3) Uani 1 1 d . . . N7 N 0.8274(7) 0.3667(4) 0.4641(6) 0.098(3) Uani 1 1 d . . . N8 N 1.0402(8) 0.3820(4) 0.5455(6) 0.105(3) Uani 1 1 d . . . N9 N 0.6693(7) 0.4401(3) -0.3561(6) 0.091(3) Uani 1 1 d . . . N10 N 0.7063(8) 0.4178(4) -0.4043(6) 0.109(3) Uani 1 1 d . . . N11 N 0.6234(11) 0.4834(5) -0.4689(8) 0.156(5) Uani 1 1 d . . . N12 N 0.6916(5) 0.1378(3) 0.3783(5) 0.073(2) Uani 1 1 d . . . N13 N 0.6709(6) 0.0391(3) 0.3831(5) 0.081(2) Uani 1 1 d . . . N14 N 0.6964(7) 0.1778(3) 0.5149(6) 0.092(3) Uani 1 1 d . . . N15 N 0.5764(9) 0.0850(5) 0.4931(7) 0.117(4) Uani 1 1 d . . . N16 N 0.7931(8) 0.0743(4) 0.5726(7) 0.101(3) Uani 1 1 d . . . S1 S 0.6752(3) 0.37289(14) 0.3180(2) 0.1333(15) Uani 1 1 d . . . S2 S 1.1711(3) 0.44294(19) 0.5350(3) 0.1569(18) Uani 1 1 d . . . S3 S 0.4351(5) 0.1062(3) 0.5244(7) 0.281(5) Uani 1 1 d . . . S4 S 0.9334(2) 0.08027(13) 0.7307(2) 0.1162(12) Uani 1 1 d . . . Zn1 Zn 0.94265(9) 0.35362(5) 0.56552(8) 0.0850(5) Uani 1 1 d . . . Zn2 Zn 0.68544(9) 0.09684(5) 0.47577(7) 0.0862(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.127(10) 0.110(10) 0.087(8) 0.015(8) 0.055(7) -0.001(8) C2 0.145(11) 0.075(8) 0.086(8) 0.014(6) 0.054(8) 0.012(7) C3 0.118(8) 0.069(7) 0.063(7) 0.012(5) 0.036(6) 0.005(6) C4 0.143(10) 0.076(7) 0.057(6) 0.006(6) 0.040(6) 0.003(6) C5 0.184(13) 0.072(8) 0.086(8) 0.020(6) 0.062(8) -0.002(8) C6 0.174(14) 0.083(9) 0.151(14) 0.042(9) 0.057(11) -0.010(9) C7 0.137(11) 0.145(13) 0.052(7) 0.029(8) 0.049(7) 0.035(9) C8 0.147(11) 0.099(10) 0.074(8) 0.011(7) 0.052(8) 0.016(8) C9 0.171(14) 0.090(10) 0.129(13) 0.041(9) 0.042(10) -0.008(10) C10 0.136(13) 0.140(15) 0.165(16) 0.021(13) 0.061(11) 0.009(11) C11 0.171(14) 0.162(16) 0.080(9) 0.034(11) 0.074(9) 0.017(12) C12 0.233(19) 0.123(13) 0.141(15) 0.065(11) 0.089(14) 0.030(12) C13 0.29(2) 0.099(11) 0.125(12) 0.047(9) 0.095(14) 0.020(12) C14 0.124(9) 0.067(7) 0.090(8) 0.021(6) 0.045(7) 0.002(6) C15 0.128(10) 0.123(10) 0.085(8) 0.025(8) 0.059(8) 0.027(8) C16 0.163(14) 0.161(15) 0.099(10) 0.059(11) 0.066(9) 0.019(12) C17 0.107(8) 0.075(7) 0.084(8) 0.014(6) 0.051(6) 0.010(6) C18 0.107(8) 0.057(6) 0.090(7) 0.023(6) 0.054(6) -0.008(5) C19 0.087(7) 0.064(6) 0.077(7) 0.020(5) 0.035(5) 0.004(5) C20 0.117(8) 0.067(7) 0.080(7) 0.017(5) 0.051(6) 0.004(6) C21 0.085(7) 0.063(6) 0.080(7) 0.001(6) 0.027(6) 0.004(5) C22 0.108(8) 0.070(7) 0.082(7) 0.014(6) 0.049(7) 0.014(6) C23 0.145(11) 0.072(8) 0.092(9) 0.002(7) 0.028(8) 0.019(7) C24 0.211(16) 0.068(9) 0.125(12) -0.001(8) 0.047(11) 0.027(9) C25 0.210(16) 0.076(9) 0.136(13) 0.034(9) 0.074(12) 0.023(9) C26 0.165(12) 0.067(8) 0.119(10) 0.014(8) 0.068(9) 0.011(8) C27 0.093(7) 0.072(7) 0.074(7) 0.013(6) 0.032(6) 0.006(5) C28 0.134(10) 0.076(8) 0.092(8) 0.000(6) 0.062(7) -0.003(7) C29 0.183(13) 0.067(7) 0.098(9) -0.012(7) 0.078(9) -0.012(8) C30 0.177(13) 0.102(10) 0.103(10) 0.009(8) 0.084(10) 0.004(9) C31 0.177(13) 0.078(8) 0.092(9) 0.013(7) 0.081(9) 0.006(8) C32 0.128(10) 0.052(6) 0.059(6) 0.006(5) 0.035(7) 0.009(6) C33 0.110(10) 0.113(10) 0.070(7) 0.036(7) 0.039(7) 0.008(8) C39 0.192(15) 0.086(9) 0.119(11) 0.016(8) 0.096(11) 0.022(9) C40 0.212(16) 0.110(10) 0.124(11) 0.047(9) 0.114(11) 0.053(11) C41 0.113(8) 0.060(6) 0.074(7) 0.007(5) 0.044(6) 0.000(5) C42 0.170(12) 0.073(7) 0.099(9) 0.005(6) 0.088(9) 0.012(7) C43 0.174(12) 0.073(7) 0.083(8) 0.018(6) 0.072(8) 0.028(7) C44 0.112(8) 0.067(7) 0.066(6) 0.007(5) 0.050(6) 0.009(6) C45 0.204(15) 0.087(9) 0.105(10) -0.008(7) 0.103(10) 0.010(9) C46 0.222(14) 0.069(7) 0.084(8) 0.005(6) 0.103(9) 0.021(8) C47 0.102(8) 0.099(9) 0.077(7) -0.007(6) 0.049(6) 0.004(7) C48 0.116(9) 0.099(9) 0.073(7) 0.013(6) 0.045(7) 0.008(7) C49 0.116(9) 0.092(8) 0.070(7) -0.005(6) 0.056(6) -0.012(7) C50 0.148(11) 0.091(8) 0.078(7) 0.019(6) 0.072(7) 0.021(7) C51 0.108(9) 0.094(8) 0.082(7) 0.007(6) 0.048(7) 0.002(7) C52 0.086(7) 0.092(8) 0.066(6) 0.011(6) 0.040(6) -0.005(6) C53 0.127(9) 0.083(8) 0.086(8) 0.002(6) 0.072(7) 0.009(7) C54 0.156(11) 0.079(7) 0.088(8) 0.023(6) 0.062(8) 0.001(7) C55 0.086(7) 0.083(7) 0.061(6) -0.004(5) 0.039(5) -0.007(5) C56 0.100(8) 0.074(7) 0.065(6) -0.007(5) 0.035(6) -0.003(6) C57 0.073(6) 0.090(7) 0.057(6) 0.005(5) 0.031(5) -0.005(5) C58 0.094(7) 0.074(6) 0.074(7) -0.002(5) 0.041(6) -0.001(5) C59 0.087(7) 0.086(7) 0.060(6) -0.004(5) 0.045(5) -0.016(6) C60 0.094(7) 0.060(6) 0.084(7) -0.011(5) 0.052(6) -0.012(5) C61 0.132(10) 0.088(8) 0.077(7) -0.007(6) 0.055(7) 0.000(7) C62 0.160(12) 0.076(9) 0.130(12) -0.024(8) 0.057(10) -0.007(8) C63 0.188(14) 0.063(8) 0.138(12) 0.008(8) 0.082(11) -0.007(8) C64 0.135(10) 0.079(8) 0.096(8) 0.004(7) 0.056(8) -0.018(7) C65 0.113(8) 0.080(7) 0.065(6) 0.005(6) 0.045(6) -0.006(6) C66 0.138(10) 0.067(7) 0.071(7) -0.008(5) 0.052(7) -0.005(6) C67 0.149(11) 0.069(7) 0.104(9) -0.012(7) 0.057(8) 0.002(7) C68 0.172(12) 0.087(9) 0.076(8) -0.010(7) 0.063(8) -0.001(8) C69 0.189(14) 0.097(10) 0.094(9) 0.020(8) 0.075(9) 0.012(9) C70 0.124(11) 0.126(11) 0.098(9) 0.023(8) 0.072(9) -0.015(9) C71 0.116(9) 0.052(6) 0.091(8) 0.001(5) 0.065(8) -0.001(6) C90 0.43(4) 0.19(2) 0.131(15) -0.048(14) 0.12(2) -0.17(2) C104 0.56(6) 0.40(5) 1.32(15) -0.62(8) 0.76(9) -0.31(5) Cl1 0.356(9) 0.165(5) 0.196(6) -0.007(4) 0.078(6) -0.020(6) Cl2 0.342(9) 0.270(8) 0.205(6) -0.050(6) 0.138(7) -0.133(7) Cl3 0.372(11) 0.282(9) 0.185(6) 0.024(6) 0.065(7) -0.066(8) Cl4 0.88(3) 0.135(5) 0.220(8) -0.016(5) 0.219(12) -0.053(9) Cl5 0.434(13) 0.130(5) 0.351(11) 0.021(6) 0.068(10) 0.016(6) Cl6 0.50(2) 0.367(16) 0.49(2) 0.147(16) 0.136(18) -0.032(15) N1 0.107(6) 0.065(5) 0.062(5) 0.010(4) 0.031(5) 0.003(4) N2 0.123(7) 0.080(6) 0.081(6) 0.015(5) 0.065(5) 0.015(5) N3 0.137(8) 0.085(7) 0.084(7) 0.018(6) 0.053(6) 0.002(6) N4 0.094(6) 0.058(5) 0.073(5) 0.009(4) 0.032(4) 0.001(4) N5 0.125(7) 0.075(6) 0.079(6) 0.012(5) 0.059(5) 0.007(5) N6 0.119(7) 0.062(6) 0.093(7) 0.018(5) 0.047(6) 0.006(5) N7 0.111(8) 0.095(7) 0.084(7) 0.020(5) 0.038(6) -0.001(5) N8 0.127(8) 0.105(8) 0.091(7) 0.011(6) 0.056(6) -0.022(6) N9 0.135(8) 0.061(5) 0.090(6) 0.010(5) 0.060(6) 0.010(5) N10 0.177(10) 0.095(7) 0.084(7) 0.018(6) 0.083(7) 0.026(7) N11 0.259(16) 0.137(10) 0.116(9) 0.068(8) 0.123(10) 0.055(11) N12 0.093(6) 0.061(5) 0.071(5) -0.011(4) 0.041(4) -0.007(4) N13 0.100(6) 0.068(6) 0.079(6) 0.004(4) 0.042(5) -0.005(4) N14 0.144(8) 0.084(6) 0.069(6) -0.004(5) 0.066(6) -0.004(5) N15 0.145(10) 0.133(9) 0.105(8) -0.021(6) 0.084(8) -0.027(8) N16 0.139(9) 0.085(6) 0.075(6) -0.002(5) 0.041(6) -0.004(6) S1 0.180(4) 0.096(2) 0.079(2) 0.0199(18) 0.014(2) 0.003(2) S2 0.160(4) 0.172(4) 0.143(3) 0.057(3) 0.069(3) -0.036(3) S3 0.210(6) 0.247(7) 0.491(14) 0.171(8) 0.250(8) 0.063(5) S4 0.129(3) 0.102(2) 0.097(2) 0.0170(19) 0.030(2) -0.010(2) Zn1 0.1065(10) 0.0745(8) 0.0782(9) 0.0222(6) 0.0437(7) 0.0016(7) Zn2 0.1186(11) 0.0782(8) 0.0720(8) 0.0050(6) 0.0508(7) -0.0095(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 C1 N2 1.328(13) . ? C1 N3 1.360(15) . ? C1 H1 0.9300 . ? C2 N3 1.268(13) . ? C2 N1 1.341(13) . ? C2 H2 0.9300 . ? C3 C4 1.350(14) . ? C3 C5 1.397(15) . ? C3 N1 1.433(12) . ? C4 C8 1.356(15) . ? C4 H4 0.9300 . ? C5 C6 1.422(18) . ? C5 H5 0.9300 . ? C6 C7 1.392(19) . ? C6 H6 0.9300 . ? C7 C8 1.392(17) . ? C7 C9 1.470(19) . ? C8 H8 0.9300 . ? C9 C10 1.114(18) . ? C9 H9 0.9300 . ? C10 C11 1.52(2) . ? C10 H10 0.9300 . ? C11 C16 1.27(2) . ? C11 C12 1.35(2) . ? C12 C13 1.43(2) . ? C12 H12 0.9300 . ? C13 C14 1.346(17) . ? C13 H13 0.9300 . ? C14 C15 1.335(16) . ? C14 C17 1.487(15) . ? C15 C16 1.382(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.369(14) . ? C17 C20 1.396(14) . ? C18 C19 1.392(13) . ? C18 H18 0.9300 . ? C19 N4 1.383(12) . ? C19 C27 1.455(14) . ? C20 C21 1.379(14) . ? C20 H20 0.9300 . ? C21 N4 1.344(12) . ? C21 C22 1.516(14) . ? C22 C23 1.351(15) . ? C22 N6 1.353(13) . ? C23 C24 1.364(17) . ? C23 H23 0.9300 . ? C24 C25 1.33(2) . ? C24 H24 0.9300 . ? C25 C26 1.367(18) . ? C25 H25 0.9300 . ? C26 N6 1.299(13) . ? C26 H26 0.9300 . ? C27 N5 1.335(12) . ? C27 C28 1.404(14) . ? C28 C29 1.359(15) . ? C28 H28 0.9300 . ? C29 C30 1.378(16) . ? C29 H29 0.9300 . ? C30 C31 1.331(16) . ? C30 H30 0.9300 . ? C31 N5 1.334(13) . ? C31 H31 0.9300 . ? C32 N7 1.128(12) . ? C32 S1 1.593(13) . ? C33 N8 1.119(13) . ? C33 S2 1.634(15) . ? C39 N10 1.295(15) . ? C39 N11 1.315(16) . ? C39 H39 0.9300 . ? C40 N9 1.310(14) . ? C40 N11 1.307(15) . ? C40 H40 0.9300 . ? C41 C46 1.344(14) . ? C41 C42 1.411(14) . ? C41 N9 1.416(13) . ? C42 C43 1.390(15) . ? C42 H42 0.9300 . ? C43 C44 1.390(14) . ? C43 H43 0.9300 . ? C44 C45 1.302(14) . ? C44 C47 1.502(14) . ? C45 C46 1.380(15) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.314(14) . ? C47 H47 0.9300 . ? C48 C49 1.462(15) . ? C48 H48 0.9300 . ? C49 C50 1.353(15) . ? C49 C54 1.419(15) . ? C50 C51 1.375(14) . ? C50 H50 0.9300 . ? C51 C52 1.425(14) . ? C51 H51 0.9300 . ? C52 C53 1.412(14) . ? C52 C55 1.487(13) . ? C53 C54 1.363(14) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C58 1.401(13) . ? C55 C56 1.419(13) . ? C56 C57 1.380(13) . ? C56 H56 0.9300 . ? C57 N12 1.324(12) . ? C57 C60 1.504(13) . ? C58 C59 1.382(13) . ? C58 H58 0.9300 . ? C59 N12 1.332(12) . ? C59 C65 1.502(13) . ? C60 N13 1.361(12) . ? C60 C61 1.361(13) . ? C61 C62 1.452(16) . ? C61 H61 0.9300 . ? C62 C63 1.384(18) . ? C62 H62 0.9300 . ? C63 C64 1.362(17) . ? C63 H63 0.9300 . ? C64 N13 1.318(13) . ? C64 H64 0.9300 . ? C65 N14 1.358(12) . ? C65 C66 1.375(14) . ? C66 C67 1.346(15) . ? C66 H66 0.9300 . ? C67 C68 1.363(15) . ? C67 H67 0.9300 . ? C68 C69 1.371(16) . ? C68 H68 0.9300 . ? C69 N14 1.322(14) . ? C69 H69 0.9300 . ? C70 N15 1.094(14) . ? C70 S3 1.578(17) . ? C71 N16 1.148(13) . ? C71 S4 1.611(14) . ? C90 Cl2 1.70(2) . ? C90 Cl1 1.78(3) . ? C90 Cl3 1.83(2) . ? C90 H90 0.9800 . ? C104 Cl6 1.7400(10) . ? C104 Cl4 1.7401(10) . ? C104 Cl5 1.7402(10) . ? C104 H104 0.9800 . ? N1 N2 1.371(11) . ? N4 Zn1 2.078(8) . ? N5 Zn1 2.203(9) . ? N6 Zn1 2.174(9) . ? N7 Zn1 1.999(10) . ? N8 Zn1 1.934(11) . ? N9 N10 1.372(12) . ? N12 Zn2 2.068(8) . ? N13 Zn2 2.163(8) . ? N14 Zn2 2.208(9) . ? N15 Zn2 1.971(13) . ? N16 Zn2 1.950(11) . ? 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 C1 N3 115.9(11) . . ? N2 C1 H1 122.1 . . ? N3 C1 H1 122.1 . . ? N3 C2 N1 112.5(11) . . ? N3 C2 H2 123.7 . . ? N1 C2 H2 123.7 . . ? C4 C3 C5 119.8(10) . . ? C4 C3 N1 120.8(10) . . ? C5 C3 N1 119.4(10) . . ? C3 C4 C8 122.5(11) . . ? C3 C4 H4 118.8 . . ? C8 C4 H4 118.8 . . ? C3 C5 C6 117.6(12) . . ? C3 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C7 C6 C5 121.6(13) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 117.3(12) . . ? C8 C7 C9 117.8(13) . . ? C6 C7 C9 124.9(15) . . ? C4 C8 C7 121.1(12) . . ? C4 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C7 130(2) . . ? C10 C9 H9 114.9 . . ? C7 C9 H9 114.9 . . ? C9 C10 C11 132(2) . . ? C9 C10 H10 114.2 . . ? C11 C10 H10 114.2 . . ? C16 C11 C12 114.7(15) . . ? C16 C11 C10 122.8(17) . . ? C12 C11 C10 122.4(18) . . ? C11 C12 C13 123.1(16) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 119.0(16) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 115.7(13) . . ? C15 C14 C17 122.3(11) . . ? C13 C14 C17 122.0(13) . . ? C14 C15 C16 122.7(14) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C11 C16 C15 124.2(17) . . ? C11 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? C18 C17 C20 117.3(10) . . ? C18 C17 C14 122.1(10) . . ? C20 C17 C14 120.6(11) . . ? C17 C18 C19 123.4(10) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? N4 C19 C18 118.0(10) . . ? N4 C19 C27 113.8(9) . . ? C18 C19 C27 128.1(10) . . ? C21 C20 C17 118.8(11) . . ? C21 C20 H20 120.6 . . ? C17 C20 H20 120.6 . . ? N4 C21 C20 123.5(9) . . ? N4 C21 C22 112.3(9) . . ? C20 C21 C22 124.1(10) . . ? C23 C22 N6 122.7(10) . . ? C23 C22 C21 122.9(10) . . ? N6 C22 C21 114.4(10) . . ? C22 C23 C24 116.1(13) . . ? C22 C23 H23 122.0 . . ? C24 C23 H23 122.0 . . ? C25 C24 C23 121.1(15) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.8(13) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? N6 C26 C25 119.2(13) . . ? N6 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? N5 C27 C28 120.2(10) . . ? N5 C27 C19 116.0(9) . . ? C28 C27 C19 123.8(10) . . ? C29 C28 C27 119.3(11) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 119.3(11) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 118.5(12) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C30 C31 N5 124.2(11) . . ? C30 C31 H31 117.9 . . ? N5 C31 H31 117.9 . . ? N7 C32 S1 175.6(12) . . ? N8 C33 S2 174.5(11) . . ? N10 C39 N11 113.3(12) . . ? N10 C39 H39 123.3 . . ? N11 C39 H39 123.3 . . ? N9 C40 N11 108.8(13) . . ? N9 C40 H40 125.6 . . ? N11 C40 H40 125.6 . . ? C46 C41 C42 120.0(10) . . ? C46 C41 N9 120.6(9) . . ? C42 C41 N9 119.3(10) . . ? C43 C42 C41 117.1(11) . . ? C43 C42 H42 121.5 . . ? C41 C42 H42 121.5 . . ? C42 C43 C44 122.8(10) . . ? C42 C43 H43 118.6 . . ? C44 C43 H43 118.6 . . ? C45 C44 C43 115.5(10) . . ? C45 C44 C47 121.1(10) . . ? C43 C44 C47 123.4(9) . . ? C44 C45 C46 126.2(11) . . ? C44 C45 H45 116.9 . . ? C46 C45 H45 116.9 . . ? C41 C46 C45 118.2(10) . . ? C41 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C48 C47 C44 125.0(11) . . ? C48 C47 H47 117.5 . . ? C44 C47 H47 117.5 . . ? C47 C48 C49 128.7(12) . . ? C47 C48 H48 115.6 . . ? C49 C48 H48 115.6 . . ? C50 C49 C54 117.6(10) . . ? C50 C49 C48 121.1(11) . . ? C54 C49 C48 121.3(11) . . ? C49 C50 C51 123.0(11) . . ? C49 C50 H50 118.5 . . ? C51 C50 H50 118.5 . . ? C50 C51 C52 119.9(11) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.1 . . ? C53 C52 C51 117.3(9) . . ? C53 C52 C55 121.7(10) . . ? C51 C52 C55 121.0(10) . . ? C54 C53 C52 120.7(10) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.6 . . ? C53 C54 C49 121.5(11) . . ? C53 C54 H54 119.3 . . ? C49 C54 H54 119.3 . . ? C58 C55 C56 116.9(9) . . ? C58 C55 C52 121.8(10) . . ? C56 C55 C52 121.3(9) . . ? C57 C56 C55 119.9(9) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? N12 C57 C56 121.5(9) . . ? N12 C57 C60 116.0(9) . . ? C56 C57 C60 122.5(10) . . ? C59 C58 C55 118.9(9) . . ? C59 C58 H58 120.6 . . ? C55 C58 H58 120.6 . . ? N12 C59 C58 122.7(9) . . ? N12 C59 C65 114.9(9) . . ? C58 C59 C65 122.3(10) . . ? N13 C60 C61 124.4(9) . . ? N13 C60 C57 112.6(9) . . ? C61 C60 C57 123.0(10) . . ? C60 C61 C62 116.3(11) . . ? C60 C61 H61 121.9 . . ? C62 C61 H61 121.8 . . ? C63 C62 C61 118.5(12) . . ? C63 C62 H62 120.8 . . ? C61 C62 H62 120.8 . . ? C64 C63 C62 118.9(12) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? N13 C64 C63 124.5(12) . . ? N13 C64 H64 117.8 . . ? C63 C64 H64 117.8 . . ? N14 C65 C66 121.9(10) . . ? N14 C65 C59 113.3(9) . . ? C66 C65 C59 124.7(10) . . ? C67 C66 C65 119.2(10) . . ? C67 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? C66 C67 C68 121.0(11) . . ? C66 C67 H67 119.5 . . ? C68 C67 H67 119.5 . . ? C67 C68 C69 116.1(11) . . ? C67 C68 H68 122.0 . . ? C69 C68 H68 122.0 . . ? N14 C69 C68 125.9(12) . . ? N14 C69 H69 117.0 . . ? C68 C69 H69 117.0 . . ? N15 C70 S3 176.6(15) . . ? N16 C71 S4 178.6(12) . . ? Cl2 C90 Cl1 109.4(17) . . ? Cl2 C90 Cl3 106.5(12) . . ? Cl1 C90 Cl3 102.0(13) . . ? Cl2 C90 H90 112.7 . . ? Cl1 C90 H90 112.7 . . ? Cl3 C90 H90 112.7 . . ? Cl6 C104 Cl4 85.7(8) . . ? Cl6 C104 Cl5 81.1(8) . . ? Cl4 C104 Cl5 103.9(6) . . ? Cl6 C104 H104 110.4 . . ? Cl4 C104 H104 124.0 . . ? Cl5 C104 H104 130.9 . . ? C2 N1 N2 109.1(9) . . ? C2 N1 C3 130.0(10) . . ? N2 N1 C3 120.9(8) . . ? C1 N2 N1 100.3(9) . . ? C2 N3 C1 102.2(10) . . ? C21 N4 C19 118.9(9) . . ? C21 N4 Zn1 121.6(6) . . ? C19 N4 Zn1 119.5(7) . . ? C27 N5 C31 118.6(10) . . ? C27 N5 Zn1 115.7(7) . . ? C31 N5 Zn1 125.4(7) . . ? C26 N6 C22 120.1(11) . . ? C26 N6 Zn1 123.1(9) . . ? C22 N6 Zn1 116.7(7) . . ? C32 N7 Zn1 171.9(10) . . ? C33 N8 Zn1 166.0(12) . . ? C40 N9 N10 109.1(10) . . ? C40 N9 C41 131.2(11) . . ? N10 N9 C41 119.6(9) . . ? C39 N10 N9 102.8(10) . . ? C40 N11 C39 105.7(12) . . ? C57 N12 C59 120.1(9) . . ? C57 N12 Zn2 119.0(6) . . ? C59 N12 Zn2 120.9(6) . . ? C64 N13 C60 117.3(9) . . ? C64 N13 Zn2 126.4(8) . . ? C60 N13 Zn2 116.2(6) . . ? C69 N14 C65 115.8(10) . . ? C69 N14 Zn2 128.3(8) . . ? C65 N14 Zn2 115.9(7) . . ? C70 N15 Zn2 160.7(13) . . ? C71 N16 Zn2 156.2(9) . . ? N8 Zn1 N7 108.2(4) . . ? N8 Zn1 N4 128.9(4) . . ? N7 Zn1 N4 122.9(4) . . ? N8 Zn1 N6 97.3(4) . . ? N7 Zn1 N6 101.3(4) . . ? N4 Zn1 N6 74.9(3) . . ? N8 Zn1 N5 101.1(4) . . ? N7 Zn1 N5 95.6(4) . . ? N4 Zn1 N5 74.8(3) . . ? N6 Zn1 N5 149.7(3) . . ? N16 Zn2 N15 111.1(5) . . ? N16 Zn2 N12 122.3(4) . . ? N15 Zn2 N12 125.9(4) . . ? N16 Zn2 N13 102.5(4) . . ? N15 Zn2 N13 101.4(4) . . ? N12 Zn2 N13 76.1(3) . . ? N16 Zn2 N14 95.4(4) . . ? N15 Zn2 N14 93.4(4) . . ? N12 Zn2 N14 74.9(3) . . ? N13 Zn2 N14 150.8(3) . . ? 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 C5 C3 C4 C8 3.4(19) . . . . ? N1 C3 C4 C8 -178.7(11) . . . . ? C4 C3 C5 C6 -3.9(19) . . . . ? N1 C3 C5 C6 178.1(11) . . . . ? C3 C5 C6 C7 3(2) . . . . ? C5 C6 C7 C8 -2(2) . . . . ? C5 C6 C7 C9 -180.0(14) . . . . ? C3 C4 C8 C7 -2(2) . . . . ? C6 C7 C8 C4 1(2) . . . . ? C9 C7 C8 C4 179.4(12) . . . . ? C8 C7 C9 C10 171(2) . . . . ? C6 C7 C9 C10 -11(3) . . . . ? C7 C9 C10 C11 -177.8(15) . . . . ? C9 C10 C11 C16 161(2) . . . . ? C9 C10 C11 C12 -23(3) . . . . ? C16 C11 C12 C13 -11(3) . . . . ? C10 C11 C12 C13 173.2(16) . . . . ? C11 C12 C13 C14 5(3) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C12 C13 C14 C17 -178.4(15) . . . . ? C13 C14 C15 C16 -3(2) . . . . ? C17 C14 C15 C16 176.8(12) . . . . ? C12 C11 C16 C15 9(3) . . . . ? C10 C11 C16 C15 -174.7(14) . . . . ? C14 C15 C16 C11 -2(3) . . . . ? C15 C14 C17 C18 -172.9(12) . . . . ? C13 C14 C17 C18 7(2) . . . . ? C15 C14 C17 C20 9.5(19) . . . . ? C13 C14 C17 C20 -170.2(15) . . . . ? C20 C17 C18 C19 -2.0(17) . . . . ? C14 C17 C18 C19 -179.7(10) . . . . ? C17 C18 C19 N4 0.6(16) . . . . ? C17 C18 C19 C27 -176.6(11) . . . . ? C18 C17 C20 C21 3.3(16) . . . . ? C14 C17 C20 C21 -178.9(10) . . . . ? C17 C20 C21 N4 -3.5(17) . . . . ? C17 C20 C21 C22 178.3(10) . . . . ? N4 C21 C22 C23 176.4(11) . . . . ? C20 C21 C22 C23 -5.1(18) . . . . ? N4 C21 C22 N6 -2.1(14) . . . . ? C20 C21 C22 N6 176.3(10) . . . . ? N6 C22 C23 C24 0(2) . . . . ? C21 C22 C23 C24 -178.7(12) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C23 C24 C25 C26 1(3) . . . . ? C24 C25 C26 N6 -1(3) . . . . ? N4 C19 C27 N5 6.3(14) . . . . ? C18 C19 C27 N5 -176.5(10) . . . . ? N4 C19 C27 C28 -173.1(10) . . . . ? C18 C19 C27 C28 4.2(18) . . . . ? N5 C27 C28 C29 1.0(18) . . . . ? C19 C27 C28 C29 -179.7(11) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 1(2) . . . . ? C29 C30 C31 N5 -1(2) . . . . ? C46 C41 C42 C43 5.6(19) . . . . ? N9 C41 C42 C43 -172.5(11) . . . . ? C41 C42 C43 C44 -5(2) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C42 C43 C44 C47 178.9(12) . . . . ? C43 C44 C45 C46 3(2) . . . . ? C47 C44 C45 C46 -175.2(13) . . . . ? C42 C41 C46 C45 -2(2) . . . . ? N9 C41 C46 C45 175.7(12) . . . . ? C44 C45 C46 C41 -2(2) . . . . ? C45 C44 C47 C48 -178.8(13) . . . . ? C43 C44 C47 C48 2.8(19) . . . . ? C44 C47 C48 C49 -177.3(11) . . . . ? C47 C48 C49 C50 -179.8(13) . . . . ? C47 C48 C49 C54 2(2) . . . . ? C54 C49 C50 C51 1.0(19) . . . . ? C48 C49 C50 C51 -177.2(11) . . . . ? C49 C50 C51 C52 -0.9(19) . . . . ? C50 C51 C52 C53 -0.2(16) . . . . ? C50 C51 C52 C55 180.0(10) . . . . ? C51 C52 C53 C54 1.3(17) . . . . ? C55 C52 C53 C54 -178.9(10) . . . . ? C52 C53 C54 C49 -1.2(19) . . . . ? C50 C49 C54 C53 0.1(18) . . . . ? C48 C49 C54 C53 178.3(11) . . . . ? C53 C52 C55 C58 -19.7(15) . . . . ? C51 C52 C55 C58 160.1(10) . . . . ? C53 C52 C55 C56 157.3(10) . . . . ? C51 C52 C55 C56 -22.9(15) . . . . ? C58 C55 C56 C57 -0.9(15) . . . . ? C52 C55 C56 C57 -178.0(9) . . . . ? C55 C56 C57 N12 -1.0(15) . . . . ? C55 C56 C57 C60 178.1(9) . . . . ? C56 C55 C58 C59 1.6(14) . . . . ? C52 C55 C58 C59 178.7(9) . . . . ? C55 C58 C59 N12 -0.6(15) . . . . ? C55 C58 C59 C65 177.4(9) . . . . ? N12 C57 C60 N13 0.1(13) . . . . ? C56 C57 C60 N13 -179.0(9) . . . . ? N12 C57 C60 C61 -177.0(10) . . . . ? C56 C57 C60 C61 4.0(16) . . . . ? N13 C60 C61 C62 -0.2(17) . . . . ? C57 C60 C61 C62 176.5(10) . . . . ? C60 C61 C62 C63 3.5(19) . . . . ? C61 C62 C63 C64 -4(2) . . . . ? C62 C63 C64 N13 1(2) . . . . ? N12 C59 C65 N14 -0.2(14) . . . . ? C58 C59 C65 N14 -178.4(10) . . . . ? N12 C59 C65 C66 -177.2(10) . . . . ? C58 C59 C65 C66 4.6(17) . . . . ? N14 C65 C66 C67 4.1(18) . . . . ? C59 C65 C66 C67 -179.1(11) . . . . ? C65 C66 C67 C68 -2(2) . . . . ? C66 C67 C68 C69 1(2) . . . . ? C67 C68 C69 N14 -1(2) . . . . ? N3 C2 N1 N2 1.3(14) . . . . ? N3 C2 N1 C3 179.1(10) . . . . ? C4 C3 N1 C2 26.3(18) . . . . ? C5 C3 N1 C2 -155.8(12) . . . . ? C4 C3 N1 N2 -156.1(11) . . . . ? C5 C3 N1 N2 21.8(15) . . . . ? N3 C1 N2 N1 0.9(13) . . . . ? C2 N1 N2 C1 -1.3(12) . . . . ? C3 N1 N2 C1 -179.3(9) . . . . ? N1 C2 N3 C1 -0.7(14) . . . . ? N2 C1 N3 C2 -0.2(15) . . . . ? C20 C21 N4 C19 2.0(15) . . . . ? C22 C21 N4 C19 -179.6(9) . . . . ? C20 C21 N4 Zn1 -177.7(8) . . . . ? C22 C21 N4 Zn1 0.8(12) . . . . ? C18 C19 N4 C21 -0.5(14) . . . . ? C27 C19 N4 C21 177.1(9) . . . . ? C18 C19 N4 Zn1 179.2(7) . . . . ? C27 C19 N4 Zn1 -3.2(12) . . . . ? C28 C27 N5 C31 -0.3(17) . . . . ? C19 C27 N5 C31 -179.7(10) . . . . ? C28 C27 N5 Zn1 173.0(8) . . . . ? C19 C27 N5 Zn1 -6.3(12) . . . . ? C30 C31 N5 C27 0(2) . . . . ? C30 C31 N5 Zn1 -172.5(11) . . . . ? C25 C26 N6 C22 -1(2) . . . . ? C25 C26 N6 Zn1 176.3(11) . . . . ? C23 C22 N6 C26 1.0(18) . . . . ? C21 C22 N6 C26 179.5(11) . . . . ? C23 C22 N6 Zn1 -176.1(10) . . . . ? C21 C22 N6 Zn1 2.5(12) . . . . ? S1 C32 N7 Zn1 112(14) . . . . ? S2 C33 N8 Zn1 98(15) . . . . ? N11 C40 N9 N10 0.9(17) . . . . ? N11 C40 N9 C41 -175.1(13) . . . . ? C46 C41 N9 C40 -20(2) . . . . ? C42 C41 N9 C40 157.6(14) . . . . ? C46 C41 N9 N10 163.8(12) . . . . ? C42 C41 N9 N10 -18.1(16) . . . . ? N11 C39 N10 N9 -5.5(17) . . . . ? C40 N9 N10 C39 2.7(15) . . . . ? C41 N9 N10 C39 179.3(11) . . . . ? N9 C40 N11 C39 -4.1(19) . . . . ? N10 C39 N11 C40 6(2) . . . . ? C56 C57 N12 C59 2.1(15) . . . . ? C60 C57 N12 C59 -177.0(8) . . . . ? C56 C57 N12 Zn2 -177.9(7) . . . . ? C60 C57 N12 Zn2 3.0(11) . . . . ? C58 C59 N12 C57 -1.3(15) . . . . ? C65 C59 N12 C57 -179.4(9) . . . . ? C58 C59 N12 Zn2 178.7(7) . . . . ? C65 C59 N12 Zn2 0.6(12) . . . . ? C63 C64 N13 C60 2.7(19) . . . . ? C63 C64 N13 Zn2 -174.0(11) . . . . ? C61 C60 N13 C64 -2.9(16) . . . . ? C57 C60 N13 C64 -179.9(9) . . . . ? C61 C60 N13 Zn2 174.1(9) . . . . ? C57 C60 N13 Zn2 -2.9(11) . . . . ? C68 C69 N14 C65 3(2) . . . . ? C68 C69 N14 Zn2 -178.5(11) . . . . ? C66 C65 N14 C69 -4.5(17) . . . . ? C59 C65 N14 C69 178.4(11) . . . . ? C66 C65 N14 Zn2 176.9(9) . . . . ? C59 C65 N14 Zn2 -0.2(12) . . . . ? S3 C70 N15 Zn2 -10(27) . . . . ? S4 C71 N16 Zn2 -145(45) . . . . ? C33 N8 Zn1 N7 78(4) . . . . ? C33 N8 Zn1 N4 -103(4) . . . . ? C33 N8 Zn1 N6 -26(4) . . . . ? C33 N8 Zn1 N5 178(4) . . . . ? C32 N7 Zn1 N8 68(7) . . . . ? C32 N7 Zn1 N4 -111(7) . . . . ? C32 N7 Zn1 N6 169(7) . . . . ? C32 N7 Zn1 N5 -36(7) . . . . ? C21 N4 Zn1 N8 87.6(9) . . . . ? C19 N4 Zn1 N8 -92.1(8) . . . . ? C21 N4 Zn1 N7 -93.4(8) . . . . ? C19 N4 Zn1 N7 86.9(8) . . . . ? C21 N4 Zn1 N6 0.4(8) . . . . ? C19 N4 Zn1 N6 -179.3(8) . . . . ? C21 N4 Zn1 N5 179.7(8) . . . . ? C19 N4 Zn1 N5 0.0(7) . . . . ? C26 N6 Zn1 N8 53.1(11) . . . . ? C22 N6 Zn1 N8 -130.0(8) . . . . ? C26 N6 Zn1 N7 -57.2(11) . . . . ? C22 N6 Zn1 N7 119.7(8) . . . . ? C26 N6 Zn1 N4 -178.5(11) . . . . ? C22 N6 Zn1 N4 -1.6(8) . . . . ? C26 N6 Zn1 N5 -179.8(9) . . . . ? C22 N6 Zn1 N5 -2.9(13) . . . . ? C27 N5 Zn1 N8 131.1(8) . . . . ? C31 N5 Zn1 N8 -56.1(11) . . . . ? C27 N5 Zn1 N7 -119.1(8) . . . . ? C31 N5 Zn1 N7 53.7(11) . . . . ? C27 N5 Zn1 N4 3.5(7) . . . . ? C31 N5 Zn1 N4 176.3(11) . . . . ? C27 N5 Zn1 N6 4.8(12) . . . . ? C31 N5 Zn1 N6 177.7(9) . . . . ? C71 N16 Zn2 N15 -79(2) . . . . ? C71 N16 Zn2 N12 92(2) . . . . ? C71 N16 Zn2 N13 173(2) . . . . ? C71 N16 Zn2 N14 16(2) . . . . ? C70 N15 Zn2 N16 106(4) . . . . ? C70 N15 Zn2 N12 -65(4) . . . . ? C70 N15 Zn2 N13 -146(4) . . . . ? C70 N15 Zn2 N14 9(4) . . . . ? C57 N12 Zn2 N16 92.7(8) . . . . ? C59 N12 Zn2 N16 -87.3(8) . . . . ? C57 N12 Zn2 N15 -97.5(8) . . . . ? C59 N12 Zn2 N15 82.5(9) . . . . ? C57 N12 Zn2 N13 -3.4(7) . . . . ? C59 N12 Zn2 N13 176.6(8) . . . . ? C57 N12 Zn2 N14 179.5(8) . . . . ? C59 N12 Zn2 N14 -0.5(7) . . . . ? C64 N13 Zn2 N16 59.4(10) . . . . ? C60 N13 Zn2 N16 -117.3(8) . . . . ? C64 N13 Zn2 N15 -55.5(10) . . . . ? C60 N13 Zn2 N15 127.8(8) . . . . ? C64 N13 Zn2 N12 -179.9(10) . . . . ? C60 N13 Zn2 N12 3.4(7) . . . . ? C64 N13 Zn2 N14 -174.3(9) . . . . ? C60 N13 Zn2 N14 9.0(12) . . . . ? C69 N14 Zn2 N16 -55.9(12) . . . . ? C65 N14 Zn2 N16 122.5(8) . . . . ? C69 N14 Zn2 N15 55.7(12) . . . . ? C65 N14 Zn2 N15 -126.0(9) . . . . ? C69 N14 Zn2 N12 -178.0(12) . . . . ? C65 N14 Zn2 N12 0.4(8) . . . . ? C69 N14 Zn2 N13 176.3(10) . . . . ? C65 N14 Zn2 N13 -5.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.509 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.128 data_2 _database_code_depnum_ccdc_archive 'CCDC 835528' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H48 Cd Cl2 N12 O9' _chemical_formula_weight 1300.43 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 18.938(5) _cell_length_b 10.356(5) _cell_length_c 29.755(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 101.461(5) _cell_angle_gamma 90.000(5) _cell_volume 5719(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.252 _cell_measurement_theta_max 24.056 _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 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8531 _exptl_absorpt_correction_T_max 0.8985 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76972 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10066 _reflns_number_gt 8259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0697P)^2^+6.5001P] 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 10066 _refine_ls_number_parameters 786 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.007 _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 0.237208(15) 1.05533(3) 0.015759(10) 0.05337(12) Uani 1 1 d . . . N5 N 0.33037(15) 1.0674(3) -0.02358(10) 0.0455(7) Uani 1 1 d . . . N2 N 0.14401(15) 1.0091(3) 0.05205(10) 0.0469(7) Uani 1 1 d . . . N6 N 0.23250(18) 1.2522(3) -0.02305(11) 0.0555(8) Uani 1 1 d . . . N3 N 0.25296(17) 1.1681(3) 0.08530(11) 0.0551(8) Uani 1 1 d . . . N1 N 0.14962(18) 0.9245(3) -0.03184(11) 0.0578(8) Uani 1 1 d . . . N4 N 0.30276(16) 0.8618(3) 0.02445(10) 0.0513(7) Uani 1 1 d . . . C38 C 0.3909(2) 1.1817(3) -0.07380(13) 0.0496(8) Uani 1 1 d . . . H38 H 0.3958 1.2567 -0.0902 0.060 Uiso 1 1 calc R . . C40 C 0.4270(2) 0.9682(3) -0.05006(13) 0.0495(8) Uani 1 1 d . . . H40 H 0.4568 0.8969 -0.0501 0.059 Uiso 1 1 calc R . . C11 C 0.09773(19) 0.8739(4) -0.01275(12) 0.0490(8) Uani 1 1 d . . . N10 N 0.95719(18) 1.1829(3) -0.26258(11) 0.0560(8) Uani 1 1 d . . . N7 N -0.50703(19) 0.6478(3) 0.23386(12) 0.0623(9) Uani 1 1 d . . . C42 C 0.35664(18) 0.8490(3) 0.00113(12) 0.0454(8) Uani 1 1 d . . . C50 C 0.6051(2) 1.0820(4) -0.15350(13) 0.0526(9) Uani 1 1 d . . . C41 C 0.37349(19) 0.9654(3) -0.02471(12) 0.0466(8) Uani 1 1 d . . . C6 C 0.14468(18) 1.0574(3) 0.09405(12) 0.0461(8) Uani 1 1 d . . . C19 C -0.1310(2) 0.8277(4) 0.16842(13) 0.0581(10) Uani 1 1 d . . . C39 C 0.4367(2) 1.0769(3) -0.07563(13) 0.0481(8) Uani 1 1 d . . . C46 C 0.2828(2) 0.7576(4) 0.04539(14) 0.0601(10) Uani 1 1 d . . . H46 H 0.2457 0.7662 0.0615 0.072 Uiso 1 1 calc R . . C5 C 0.20276(19) 1.1536(3) 0.11102(12) 0.0484(8) Uani 1 1 d . . . C49 C 0.5822(2) 1.1957(4) -0.13508(12) 0.0511(9) Uani 1 1 d . . . H49 H 0.6048 1.2734 -0.1391 0.061 Uiso 1 1 calc R . . C36 C 0.2860(2) 1.2800(3) -0.04493(12) 0.0492(8) Uani 1 1 d . . . C8 C 0.04136(19) 0.9308(3) 0.10096(13) 0.0482(8) Uani 1 1 d . . . C7 C 0.09447(19) 1.0207(4) 0.11909(13) 0.0491(8) Uani 1 1 d . . . H7 H 0.0958 1.0556 0.1480 0.059 Uiso 1 1 calc R . . C37 C 0.33836(19) 1.1738(3) -0.04758(12) 0.0466(8) Uani 1 1 d . . . C48 C 0.5271(2) 1.1950(4) -0.11121(13) 0.0507(8) Uani 1 1 d . . . H48 H 0.5127 1.2721 -0.0998 0.061 Uiso 1 1 calc R . . C16 C -0.01516(19) 0.8920(4) 0.12638(13) 0.0512(8) Uani 1 1 d . . . C59 C 0.8970(2) 1.1761(4) -0.24033(13) 0.0539(9) Uani 1 1 d . . . N11 N 0.9704(2) 1.0872(4) -0.29131(14) 0.0754(10) Uani 1 1 d . . . C47 C 0.4927(2) 1.0801(3) -0.10395(13) 0.0491(8) Uani 1 1 d . . . C44 C 0.3702(2) 0.6262(4) 0.02163(14) 0.0627(10) Uani 1 1 d . . . H44 H 0.3932 0.5472 0.0209 0.075 Uiso 1 1 calc R . . C27 C -0.4395(2) 0.6601(4) 0.22100(13) 0.0550(9) Uani 1 1 d . . . C35 C 0.2916(2) 1.4009(4) -0.06374(14) 0.0599(10) Uani 1 1 d . . . H35 H 0.3295 1.4196 -0.0783 0.072 Uiso 1 1 calc R . . C18 C -0.0935(2) 0.9429(4) 0.17824(14) 0.0595(10) Uani 1 1 d . . . H18 H -0.1073 1.0003 0.1990 0.071 Uiso 1 1 calc R . . C17 C -0.0364(2) 0.9739(4) 0.15790(14) 0.0563(9) Uani 1 1 d . . . H17 H -0.0117 1.0510 0.1655 0.068 Uiso 1 1 calc R . . C57 C 0.7932(2) 1.0669(4) -0.22548(15) 0.0637(10) Uani 1 1 d . . . H57 H 0.7628 0.9955 -0.2300 0.076 Uiso 1 1 calc R . . C51 C 0.5673(2) 0.9703(4) -0.14856(15) 0.0617(10) Uani 1 1 d . . . H51 H 0.5790 0.8945 -0.1622 0.074 Uiso 1 1 calc R . . C60 C 0.8837(2) 1.2755(5) -0.21257(17) 0.0741(13) Uani 1 1 d . . . H60 H 0.9146 1.3463 -0.2077 0.089 Uiso 1 1 calc R . . C21 C -0.0502(2) 0.7734(4) 0.11807(15) 0.0655(11) Uani 1 1 d . . . H21 H -0.0354 0.7147 0.0982 0.079 Uiso 1 1 calc R . . C53 C 0.6666(2) 1.0775(4) -0.17645(14) 0.0585(10) Uani 1 1 d . . . H53 H 0.6713 1.0039 -0.1935 0.070 Uiso 1 1 calc R . . C1 C 0.3050(2) 1.2564(5) 0.09839(16) 0.0699(12) Uani 1 1 d . . . H1 H 0.3401 1.2667 0.0808 0.084 Uiso 1 1 calc R . . N12 N 1.0529(2) 1.2454(4) -0.28712(13) 0.0736(10) Uani 1 1 d . . . C45 C 0.3142(2) 0.6392(4) 0.04430(14) 0.0641(11) Uani 1 1 d . . . H45 H 0.2980 0.5687 0.0587 0.077 Uiso 1 1 calc R . . C26 C -0.4081(2) 0.5572(4) 0.20365(16) 0.0653(11) Uani 1 1 d . . . H26 H -0.4303 0.4767 0.2013 0.078 Uiso 1 1 calc R . . C52 C 0.5128(2) 0.9682(4) -0.12397(15) 0.0602(10) Uani 1 1 d . . . H52 H 0.4892 0.8910 -0.1207 0.072 Uiso 1 1 calc R . . C12 C 0.0520(2) 0.7787(4) -0.03474(14) 0.0624(10) Uani 1 1 d . . . H12 H 0.0157 0.7452 -0.0213 0.075 Uiso 1 1 calc R . . C55 C 0.7781(2) 1.1672(4) -0.19785(13) 0.0556(9) Uani 1 1 d . . . C54 C 0.7161(2) 1.1681(4) -0.17522(14) 0.0606(10) Uani 1 1 d . . . H54 H 0.7110 1.2411 -0.1579 0.073 Uiso 1 1 calc R . . C9 C 0.0410(2) 0.8836(4) 0.05722(13) 0.0527(9) Uani 1 1 d . . . H9 H 0.0056 0.8255 0.0438 0.063 Uiso 1 1 calc R . . C24 C -0.3083(2) 0.6912(4) 0.19386(13) 0.0578(10) Uani 1 1 d . . . C58 C 0.8524(2) 1.0706(4) -0.24653(15) 0.0617(10) Uani 1 1 d . . . H58 H 0.8618 1.0020 -0.2647 0.074 Uiso 1 1 calc R . . C4 C 0.2039(2) 1.2258(4) 0.15007(15) 0.0652(11) Uani 1 1 d . . . H4 H 0.1689 1.2139 0.1677 0.078 Uiso 1 1 calc R . . N8 N -0.5302(2) 0.7363(4) 0.26118(15) 0.0824(12) Uani 1 1 d . . . C20 C -0.1065(2) 0.7425(4) 0.13910(16) 0.0693(12) Uani 1 1 d . . . H20 H -0.1287 0.6624 0.1334 0.083 Uiso 1 1 calc R . . C43 C 0.3918(2) 0.7332(4) -0.00005(14) 0.0569(9) Uani 1 1 d . . . H43 H 0.4299 0.7268 -0.0154 0.068 Uiso 1 1 calc R . . C22 C -0.1956(2) 0.8048(4) 0.18706(15) 0.0660(11) Uani 1 1 d . . . H22 H -0.2069 0.8674 0.2069 0.079 Uiso 1 1 calc R . . C10 C 0.09344(19) 0.9232(3) 0.03354(12) 0.0473(8) Uani 1 1 d . . . C34 C 0.2402(3) 1.4937(4) -0.06055(16) 0.0676(11) Uani 1 1 d . . . H34 H 0.2426 1.5751 -0.0734 0.081 Uiso 1 1 calc R . . C30 C -0.5586(3) 0.5611(5) 0.2207(2) 0.0790(14) Uani 1 1 d . . . H30 H -0.5551 0.4921 0.2013 0.095 Uiso 1 1 calc R . . C14 C 0.1152(3) 0.7841(5) -0.09554(15) 0.0730(12) Uani 1 1 d . . . H14 H 0.1232 0.7538 -0.1235 0.088 Uiso 1 1 calc R . . C15 C 0.1575(3) 0.8793(5) -0.07255(14) 0.0739(13) Uani 1 1 d . . . H15 H 0.1936 0.9143 -0.0859 0.089 Uiso 1 1 calc R . . C3 C 0.2576(3) 1.3158(5) 0.16257(18) 0.0815(14) Uani 1 1 d . . . H3 H 0.2593 1.3657 0.1887 0.098 Uiso 1 1 calc R . . C25 C -0.3433(2) 0.5739(4) 0.18972(16) 0.0649(11) Uani 1 1 d . . . H25 H -0.3229 0.5043 0.1772 0.078 Uiso 1 1 calc R . . C62 C 1.0277(3) 1.1314(5) -0.30470(16) 0.0720(12) Uani 1 1 d . . . H62 H 1.0497 1.0862 -0.3252 0.086 Uiso 1 1 calc R . . C28 C -0.4075(3) 0.7790(5) 0.22370(18) 0.0820(15) Uani 1 1 d . . . H28 H -0.4300 0.8495 0.2342 0.098 Uiso 1 1 calc R . . C56 C 0.8250(3) 1.2705(5) -0.19197(17) 0.0750(13) Uani 1 1 d . . . H56 H 0.8165 1.3389 -0.1735 0.090 Uiso 1 1 calc R . . C61 C 1.0077(2) 1.2739(4) -0.26076(16) 0.0655(11) Uani 1 1 d . . . H61 H 1.0102 1.3482 -0.2430 0.079 Uiso 1 1 calc R . . N9 N -0.6156(2) 0.5855(5) 0.2388(2) 0.0965(15) Uani 1 1 d . . . C13 C 0.0613(3) 0.7344(5) -0.07682(15) 0.0708(12) Uani 1 1 d . . . H13 H 0.0310 0.6711 -0.0922 0.085 Uiso 1 1 calc R . . C33 C 0.1861(3) 1.4638(4) -0.03827(17) 0.0741(13) Uani 1 1 d . . . H33 H 0.1512 1.5248 -0.0354 0.089 Uiso 1 1 calc R . . C2 C 0.3084(3) 1.3315(5) 0.13636(18) 0.0834(14) Uani 1 1 d . . . H2 H 0.3448 1.3924 0.1443 0.100 Uiso 1 1 calc R . . C29 C -0.3419(3) 0.7942(5) 0.21093(19) 0.0811(14) Uani 1 1 d . . . H29 H -0.3197 0.8748 0.2138 0.097 Uiso 1 1 calc R . . C32 C 0.1838(2) 1.3432(4) -0.02018(15) 0.0682(11) Uani 1 1 d . . . H32 H 0.1465 1.3236 -0.0051 0.082 Uiso 1 1 calc R . . C23 C -0.2398(2) 0.7055(4) 0.17887(14) 0.0625(10) Uani 1 1 d . . . H23 H -0.2261 0.6379 0.1619 0.075 Uiso 1 1 calc R . . C31 C -0.5947(3) 0.6926(6) 0.2625(2) 0.0964(18) Uani 1 1 d . . . H31 H -0.6245 0.7344 0.2792 0.116 Uiso 1 1 calc R . . Cl1 Cl 0.49189(6) 0.59563(9) 0.90931(4) 0.0630(3) Uani 1 1 d . . . Cl2 Cl 0.90210(8) 0.48676(12) 0.92473(4) 0.0810(4) Uani 1 1 d . . . O1 O 0.53311(19) 0.6752(3) 0.94393(13) 0.0849(10) Uani 1 1 d . . . O2 O 0.5381(2) 0.5430(4) 0.88181(14) 0.0983(12) Uani 1 1 d . . . O3 O 0.4611(2) 0.4924(4) 0.92940(15) 0.1000(12) Uani 1 1 d . . . O4 O 0.4355(2) 0.6692(3) 0.88270(16) 0.1087(13) Uani 1 1 d . . . O5 O 0.8996(2) 0.6181(4) 0.93722(16) 0.1120(13) Uani 1 1 d . . . O6 O 0.9139(4) 0.4745(6) 0.88233(18) 0.164(3) Uani 1 1 d . . . O7 O 0.8507(6) 0.4181(7) 0.9327(4) 0.290(6) Uani 1 1 d . . . O8 O 0.9667(6) 0.4365(6) 0.9507(3) 0.251(5) Uani 1 1 d . . . C66 C 0.2904(3) 0.7532(8) 0.8756(3) 0.120(2) Uani 1 1 d . . . H66A H 0.3404 0.7292 0.8808 0.180 Uiso 1 1 calc R . . H66B H 0.2611 0.6777 0.8679 0.180 Uiso 1 1 calc R . . H66C H 0.2799 0.7916 0.9029 0.180 Uiso 1 1 calc R . . O10 O 0.2766(6) 0.8362(14) 0.8419(3) 0.314(7) Uani 1 1 d . . . H10 H 0.2805 0.9098 0.8522 0.471 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 0.04972(18) 0.05625(19) 0.05930(19) 0.00536(13) 0.02327(13) -0.00194(12) N5 0.0442(16) 0.0424(16) 0.0521(16) 0.0040(13) 0.0152(13) -0.0019(12) N2 0.0426(16) 0.0475(16) 0.0524(17) 0.0016(14) 0.0139(13) -0.0003(13) N6 0.0587(18) 0.0548(18) 0.0579(18) 0.0039(15) 0.0237(15) 0.0086(15) N3 0.0475(17) 0.0612(19) 0.0575(18) 0.0010(15) 0.0125(14) -0.0083(15) N1 0.0557(19) 0.069(2) 0.0496(18) 0.0012(15) 0.0127(15) -0.0030(16) N4 0.0498(17) 0.0498(17) 0.0557(18) 0.0101(14) 0.0141(14) -0.0030(14) C38 0.054(2) 0.0418(19) 0.057(2) 0.0068(16) 0.0194(17) -0.0019(16) C40 0.051(2) 0.0405(18) 0.060(2) 0.0029(16) 0.0180(17) -0.0001(15) C11 0.0451(19) 0.050(2) 0.053(2) 0.0042(16) 0.0121(16) 0.0031(16) N10 0.0583(19) 0.0578(19) 0.0573(18) 0.0067(15) 0.0245(15) 0.0038(16) N7 0.062(2) 0.063(2) 0.067(2) 0.0098(17) 0.0258(17) -0.0055(17) C42 0.0441(18) 0.0438(18) 0.0476(19) 0.0056(15) 0.0076(15) -0.0051(15) C50 0.051(2) 0.059(2) 0.049(2) 0.0035(17) 0.0148(16) -0.0001(17) C41 0.0455(19) 0.0433(19) 0.051(2) 0.0023(15) 0.0102(15) -0.0046(15) C6 0.0410(18) 0.0473(19) 0.051(2) 0.0019(15) 0.0100(15) -0.0001(15) C19 0.054(2) 0.067(2) 0.055(2) 0.0018(19) 0.0160(18) -0.0103(19) C39 0.0475(19) 0.0455(19) 0.054(2) -0.0019(16) 0.0169(16) -0.0064(15) C46 0.058(2) 0.065(3) 0.061(2) 0.0121(19) 0.0192(19) -0.0086(19) C5 0.0436(19) 0.0492(19) 0.053(2) 0.0024(16) 0.0106(16) -0.0033(16) C49 0.049(2) 0.053(2) 0.053(2) 0.0045(17) 0.0153(16) -0.0087(17) C36 0.052(2) 0.0462(19) 0.051(2) 0.0002(16) 0.0131(16) 0.0017(16) C8 0.0419(18) 0.049(2) 0.055(2) 0.0055(16) 0.0133(16) 0.0015(15) C7 0.0450(19) 0.054(2) 0.0491(19) -0.0007(16) 0.0114(16) -0.0033(16) C37 0.0488(19) 0.0405(18) 0.053(2) -0.0002(15) 0.0153(16) -0.0031(15) C48 0.051(2) 0.0460(19) 0.059(2) 0.0007(16) 0.0186(17) -0.0030(16) C16 0.0427(19) 0.054(2) 0.058(2) 0.0048(17) 0.0128(16) -0.0021(16) C59 0.048(2) 0.063(2) 0.053(2) 0.0036(18) 0.0152(17) 0.0020(18) N11 0.086(3) 0.072(2) 0.079(2) -0.010(2) 0.042(2) -0.004(2) C47 0.048(2) 0.049(2) 0.052(2) 0.0018(16) 0.0160(16) -0.0032(16) C44 0.074(3) 0.043(2) 0.070(3) 0.0058(18) 0.011(2) -0.0017(19) C27 0.052(2) 0.062(2) 0.054(2) 0.0043(18) 0.0178(17) -0.0063(18) C35 0.072(3) 0.043(2) 0.068(2) 0.0043(18) 0.023(2) 0.0017(19) C18 0.058(2) 0.065(2) 0.061(2) -0.0024(19) 0.0243(19) -0.0052(19) C17 0.052(2) 0.056(2) 0.064(2) -0.0030(18) 0.0165(18) -0.0077(18) C57 0.059(2) 0.066(3) 0.068(3) -0.001(2) 0.018(2) -0.013(2) C51 0.068(3) 0.050(2) 0.074(3) -0.0071(19) 0.031(2) -0.0047(19) C60 0.061(3) 0.071(3) 0.099(3) -0.024(3) 0.039(2) -0.019(2) C21 0.065(3) 0.060(2) 0.079(3) -0.012(2) 0.032(2) -0.008(2) C53 0.056(2) 0.063(2) 0.058(2) 0.0010(19) 0.0179(18) -0.0026(19) C1 0.056(2) 0.079(3) 0.078(3) -0.005(2) 0.021(2) -0.023(2) N12 0.070(2) 0.076(3) 0.083(3) 0.024(2) 0.035(2) 0.011(2) C45 0.076(3) 0.050(2) 0.066(3) 0.0105(19) 0.014(2) -0.016(2) C26 0.057(2) 0.057(2) 0.085(3) 0.002(2) 0.021(2) -0.0121(19) C52 0.066(3) 0.045(2) 0.077(3) -0.0034(18) 0.034(2) -0.0066(18) C12 0.070(3) 0.059(2) 0.059(2) -0.0016(19) 0.017(2) -0.011(2) C55 0.054(2) 0.066(2) 0.049(2) -0.0022(18) 0.0153(17) -0.0004(19) C54 0.058(2) 0.069(3) 0.058(2) -0.0056(19) 0.0208(19) -0.003(2) C9 0.0445(19) 0.050(2) 0.064(2) -0.0026(18) 0.0119(17) -0.0063(16) C24 0.058(2) 0.063(2) 0.055(2) 0.0008(18) 0.0180(18) -0.0106(19) C58 0.062(2) 0.064(3) 0.063(2) -0.0090(19) 0.021(2) -0.003(2) C4 0.059(2) 0.067(3) 0.072(3) -0.009(2) 0.020(2) -0.011(2) N8 0.083(3) 0.081(3) 0.096(3) 0.004(2) 0.050(2) 0.009(2) C20 0.070(3) 0.060(2) 0.086(3) -0.010(2) 0.036(2) -0.019(2) C43 0.061(2) 0.050(2) 0.063(2) 0.0037(18) 0.0181(19) -0.0004(18) C22 0.064(3) 0.074(3) 0.065(3) -0.004(2) 0.025(2) -0.011(2) C10 0.0416(18) 0.0471(19) 0.053(2) 0.0017(15) 0.0081(15) 0.0024(15) C34 0.081(3) 0.043(2) 0.081(3) 0.002(2) 0.020(2) 0.009(2) C30 0.070(3) 0.070(3) 0.103(4) 0.010(3) 0.033(3) -0.010(2) C14 0.085(3) 0.084(3) 0.051(2) -0.005(2) 0.015(2) 0.002(3) C15 0.071(3) 0.104(4) 0.051(2) 0.002(2) 0.021(2) -0.009(3) C3 0.077(3) 0.088(3) 0.080(3) -0.027(3) 0.017(3) -0.023(3) C25 0.059(2) 0.059(2) 0.080(3) -0.005(2) 0.022(2) -0.0069(19) C62 0.080(3) 0.077(3) 0.069(3) 0.014(2) 0.039(2) 0.018(3) C28 0.085(3) 0.067(3) 0.107(4) -0.024(3) 0.051(3) -0.021(3) C56 0.071(3) 0.070(3) 0.093(3) -0.024(2) 0.038(3) -0.011(2) C61 0.063(3) 0.061(3) 0.077(3) 0.012(2) 0.028(2) 0.004(2) N9 0.071(3) 0.082(3) 0.150(4) 0.035(3) 0.053(3) 0.002(2) C13 0.082(3) 0.068(3) 0.059(2) -0.007(2) 0.006(2) -0.006(2) C33 0.083(3) 0.064(3) 0.078(3) -0.001(2) 0.023(3) 0.026(2) C2 0.068(3) 0.089(4) 0.092(3) -0.018(3) 0.016(3) -0.032(3) C29 0.078(3) 0.065(3) 0.112(4) -0.020(3) 0.046(3) -0.028(2) C32 0.069(3) 0.067(3) 0.075(3) 0.003(2) 0.032(2) 0.017(2) C23 0.062(2) 0.068(3) 0.061(2) 0.000(2) 0.020(2) -0.008(2) C31 0.092(4) 0.082(4) 0.133(5) 0.034(4) 0.066(4) 0.013(3) Cl1 0.0611(6) 0.0432(5) 0.0910(7) -0.0013(5) 0.0303(5) -0.0021(4) Cl2 0.1139(10) 0.0649(7) 0.0763(7) 0.0012(6) 0.0476(7) -0.0041(7) O1 0.082(2) 0.071(2) 0.104(3) -0.0172(18) 0.0244(19) -0.0100(17) O2 0.085(2) 0.115(3) 0.109(3) -0.017(2) 0.052(2) -0.004(2) O3 0.101(3) 0.064(2) 0.151(4) 0.008(2) 0.063(3) -0.0176(19) O4 0.090(3) 0.066(2) 0.158(4) 0.002(2) -0.005(3) 0.0120(19) O5 0.124(3) 0.079(3) 0.143(4) -0.024(2) 0.051(3) 0.010(2) O6 0.256(7) 0.151(5) 0.114(4) -0.041(3) 0.110(4) -0.064(5) O7 0.320(11) 0.180(6) 0.470(15) -0.127(8) 0.319(12) -0.144(7) O8 0.376(13) 0.118(5) 0.201(7) -0.012(4) -0.087(8) 0.059(6) C66 0.075(4) 0.161(7) 0.132(6) 0.042(5) 0.043(4) 0.019(4) O10 0.225(9) 0.56(2) 0.193(8) 0.111(11) 0.127(7) 0.156(13) _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 N2 2.295(3) . ? Cd1 N5 2.306(3) . ? Cd1 N6 2.336(3) . ? Cd1 N3 2.343(3) . ? Cd1 N4 2.345(3) . ? Cd1 N1 2.379(3) . ? N5 C37 1.337(4) . ? N5 C41 1.340(5) . ? N2 C10 1.343(5) . ? N2 C6 1.344(5) . ? N6 C36 1.340(5) . ? N6 C32 1.334(5) . ? N3 C5 1.342(5) . ? N3 C1 1.344(5) . ? N1 C15 1.335(5) . ? N1 C11 1.336(5) . ? N4 C46 1.337(5) . ? N4 C42 1.350(5) . ? C38 C37 1.384(5) . ? C38 C39 1.397(5) . ? C38 H38 0.9300 . ? C40 C41 1.378(5) . ? C40 C39 1.391(5) . ? C40 H40 0.9300 . ? C11 C12 1.388(5) . ? C11 C10 1.486(5) . ? N10 C61 1.336(5) . ? N10 N11 1.363(5) . ? N10 C59 1.429(5) . ? N7 C30 1.327(6) . ? N7 N8 1.355(5) . ? N7 C27 1.412(5) . ? C42 C43 1.375(5) . ? C42 C41 1.498(5) . ? C50 C51 1.383(5) . ? C50 C49 1.404(5) . ? C50 C53 1.464(5) . ? C6 C7 1.373(5) . ? C6 C5 1.496(5) . ? C19 C20 1.383(6) . ? C19 C18 1.389(6) . ? C19 C22 1.461(5) . ? C39 C47 1.480(5) . ? C46 C45 1.366(6) . ? C46 H46 0.9300 . ? C5 C4 1.378(6) . ? C49 C48 1.373(5) . ? C49 H49 0.9300 . ? C36 C35 1.384(5) . ? C36 C37 1.494(5) . ? C8 C9 1.389(5) . ? C8 C7 1.398(5) . ? C8 C16 1.483(5) . ? C7 H7 0.9300 . ? C48 C47 1.394(5) . ? C48 H48 0.9300 . ? C16 C17 1.382(6) . ? C16 C21 1.394(6) . ? C59 C58 1.371(6) . ? C59 C60 1.374(6) . ? N11 C62 1.311(6) . ? C47 C52 1.390(5) . ? C44 C45 1.372(6) . ? C44 C43 1.383(5) . ? C44 H44 0.9300 . ? C27 C28 1.367(6) . ? C27 C26 1.369(6) . ? C35 C34 1.385(6) . ? C35 H35 0.9300 . ? C18 C17 1.379(5) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? C57 C58 1.390(6) . ? C57 C55 1.389(6) . ? C57 H57 0.9300 . ? C51 C52 1.380(6) . ? C51 H51 0.9300 . ? C60 C56 1.375(6) . ? C60 H60 0.9300 . ? C21 C20 1.378(6) . ? C21 H21 0.9300 . ? C53 C54 1.322(6) . ? C53 H53 0.9300 . ? C1 C2 1.362(7) . ? C1 H1 0.9300 . ? N12 C61 1.306(5) . ? N12 C62 1.341(6) . ? C45 H45 0.9300 . ? C26 C25 1.381(6) . ? C26 H26 0.9300 . ? C52 H52 0.9300 . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C55 C56 1.379(6) . ? C55 C54 1.465(5) . ? C54 H54 0.9300 . ? C9 C10 1.389(5) . ? C9 H9 0.9300 . ? C24 C25 1.378(6) . ? C24 C29 1.389(6) . ? C24 C23 1.461(6) . ? C58 H58 0.9300 . ? C4 C3 1.376(6) . ? C4 H4 0.9300 . ? N8 C31 1.310(7) . ? C20 H20 0.9300 . ? C43 H43 0.9300 . ? C22 C23 1.318(6) . ? C22 H22 0.9300 . ? C34 C33 1.362(7) . ? C34 H34 0.9300 . ? C30 N9 1.322(6) . ? C30 H30 0.9300 . ? C14 C13 1.358(6) . ? C14 C15 1.365(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C3 C2 1.363(7) . ? C3 H3 0.9300 . ? C25 H25 0.9300 . ? C62 H62 0.9300 . ? C28 C29 1.379(6) . ? C28 H28 0.9300 . ? C56 H56 0.9300 . ? C61 H61 0.9300 . ? N9 C31 1.331(8) . ? C13 H13 0.9300 . ? C33 C32 1.364(6) . ? C33 H33 0.9300 . ? C2 H2 0.9300 . ? C29 H29 0.9300 . ? C32 H32 0.9300 . ? C23 H23 0.9300 . ? C31 H31 0.9300 . ? Cl1 O3 1.407(4) . ? Cl1 O4 1.418(4) . ? Cl1 O1 1.425(4) . ? Cl1 O2 1.420(4) . ? Cl2 O7 1.266(6) . ? Cl2 O6 1.331(4) . ? Cl2 O8 1.411(9) . ? Cl2 O5 1.413(4) . ? C66 O10 1.308(10) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? O10 H10 0.8200 . ? 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 Cd1 N5 170.91(10) . . ? N2 Cd1 N6 117.21(11) . . ? N5 Cd1 N6 70.10(10) . . ? N2 Cd1 N3 70.32(11) . . ? N5 Cd1 N3 116.43(10) . . ? N6 Cd1 N3 89.27(11) . . ? N2 Cd1 N4 102.10(10) . . ? N5 Cd1 N4 70.17(10) . . ? N6 Cd1 N4 140.17(11) . . ? N3 Cd1 N4 110.92(11) . . ? N2 Cd1 N1 69.57(11) . . ? N5 Cd1 N1 104.01(11) . . ? N6 Cd1 N1 104.43(12) . . ? N3 Cd1 N1 139.55(11) . . ? N4 Cd1 N1 82.53(11) . . ? C37 N5 C41 120.1(3) . . ? C37 N5 Cd1 119.7(2) . . ? C41 N5 Cd1 120.1(2) . . ? C10 N2 C6 120.1(3) . . ? C10 N2 Cd1 119.8(2) . . ? C6 N2 Cd1 119.6(2) . . ? C36 N6 C32 118.6(3) . . ? C36 N6 Cd1 118.0(2) . . ? C32 N6 Cd1 123.0(3) . . ? C5 N3 C1 118.2(3) . . ? C5 N3 Cd1 117.9(2) . . ? C1 N3 Cd1 123.5(3) . . ? C15 N1 C11 118.2(4) . . ? C15 N1 Cd1 123.3(3) . . ? C11 N1 Cd1 117.1(2) . . ? C46 N4 C42 118.2(3) . . ? C46 N4 Cd1 123.3(3) . . ? C42 N4 Cd1 117.7(2) . . ? C37 C38 C39 119.8(3) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C41 C40 C39 120.5(3) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? N1 C11 C12 121.4(4) . . ? N1 C11 C10 116.1(3) . . ? C12 C11 C10 122.5(3) . . ? C61 N10 N11 108.6(3) . . ? C61 N10 C59 130.2(4) . . ? N11 N10 C59 121.2(3) . . ? C30 N7 N8 109.1(4) . . ? C30 N7 C27 129.4(4) . . ? N8 N7 C27 121.4(4) . . ? N4 C42 C43 121.2(3) . . ? N4 C42 C41 116.4(3) . . ? C43 C42 C41 122.4(3) . . ? C51 C50 C49 117.0(3) . . ? C51 C50 C53 120.0(4) . . ? C49 C50 C53 123.0(3) . . ? N5 C41 C40 121.0(3) . . ? N5 C41 C42 115.4(3) . . ? C40 C41 C42 123.5(3) . . ? N2 C6 C7 121.5(3) . . ? N2 C6 C5 115.6(3) . . ? C7 C6 C5 122.9(3) . . ? C20 C19 C18 117.4(4) . . ? C20 C19 C22 123.2(4) . . ? C18 C19 C22 119.4(4) . . ? C40 C39 C38 117.2(3) . . ? C40 C39 C47 121.2(3) . . ? C38 C39 C47 121.7(3) . . ? N4 C46 C45 123.2(4) . . ? N4 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? N3 C5 C4 121.7(3) . . ? N3 C5 C6 116.0(3) . . ? C4 C5 C6 122.2(3) . . ? C48 C49 C50 121.5(3) . . ? C48 C49 H49 119.2 . . ? C50 C49 H49 119.2 . . ? N6 C36 C35 121.2(3) . . ? N6 C36 C37 116.2(3) . . ? C35 C36 C37 122.6(3) . . ? C9 C8 C7 117.7(3) . . ? C9 C8 C16 120.9(3) . . ? C7 C8 C16 121.3(3) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N5 C37 C38 121.4(3) . . ? N5 C37 C36 115.6(3) . . ? C38 C37 C36 123.1(3) . . ? C49 C48 C47 120.7(4) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C17 C16 C21 118.0(3) . . ? C17 C16 C8 121.1(3) . . ? C21 C16 C8 120.9(3) . . ? C58 C59 C60 119.8(4) . . ? C58 C59 N10 120.2(4) . . ? C60 C59 N10 120.0(4) . . ? C62 N11 N10 101.7(4) . . ? C48 C47 C52 118.0(3) . . ? C48 C47 C39 121.2(3) . . ? C52 C47 C39 120.9(3) . . ? C45 C44 C43 118.7(4) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C28 C27 C26 120.2(4) . . ? C28 C27 N7 118.6(4) . . ? C26 C27 N7 121.1(4) . . ? C36 C35 C34 119.2(4) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C17 C18 C19 121.3(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C58 C57 C55 121.7(4) . . ? C58 C57 H57 119.2 . . ? C55 C57 H57 119.2 . . ? C50 C51 C52 121.8(4) . . ? C50 C51 H51 119.1 . . ? C52 C51 H51 119.1 . . ? C56 C60 C59 120.0(4) . . ? C56 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C20 C21 C16 120.5(4) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C54 C53 C50 126.2(4) . . ? C54 C53 H53 116.9 . . ? C50 C53 H53 116.9 . . ? N3 C1 C2 122.7(4) . . ? N3 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C61 N12 C62 102.0(4) . . ? C46 C45 C44 118.9(4) . . ? C46 C45 H45 120.6 . . ? C44 C45 H45 120.6 . . ? C25 C26 C27 119.6(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C51 C52 C47 120.8(4) . . ? C51 C52 H52 119.6 . . ? C47 C52 H52 119.6 . . ? C13 C12 C11 119.1(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C56 C55 C57 116.9(4) . . ? C56 C55 C54 119.4(4) . . ? C57 C55 C54 123.7(4) . . ? C53 C54 C55 127.7(4) . . ? C53 C54 H54 116.1 . . ? C55 C54 H54 116.1 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C25 C24 C29 117.6(4) . . ? C25 C24 C23 120.2(4) . . ? C29 C24 C23 122.2(4) . . ? C59 C58 C57 119.5(4) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C31 N8 N7 101.5(5) . . ? C19 C20 C21 121.6(4) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C42 C43 C44 119.8(4) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C23 C22 C19 127.3(4) . . ? C23 C22 H22 116.4 . . ? C19 C22 H22 116.4 . . ? N2 C10 C9 120.7(3) . . ? N2 C10 C11 116.2(3) . . ? C9 C10 C11 123.1(3) . . ? C33 C34 C35 118.9(4) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? N9 C30 N7 111.3(5) . . ? N9 C30 H30 124.4 . . ? N7 C30 H30 124.4 . . ? C13 C14 C15 118.9(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N1 C15 C14 123.2(4) . . ? N1 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C26 C25 C24 121.6(4) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? N11 C62 N12 116.2(4) . . ? N11 C62 H62 121.9 . . ? N12 C62 H62 121.9 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C60 C56 C55 122.1(4) . . ? C60 C56 H56 119.0 . . ? C55 C56 H56 119.0 . . ? N12 C61 N10 111.5(4) . . ? N12 C61 H61 124.3 . . ? N10 C61 H61 124.3 . . ? C30 N9 C31 101.2(4) . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C28 C29 C24 121.0(4) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? N6 C32 C33 123.0(4) . . ? N6 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C22 C23 C24 126.3(4) . . ? C22 C23 H23 116.8 . . ? C24 C23 H23 116.8 . . ? N8 C31 N9 116.9(5) . . ? N8 C31 H31 121.5 . . ? N9 C31 H31 121.5 . . ? O3 Cl1 O4 108.4(3) . . ? O3 Cl1 O1 110.2(3) . . ? O4 Cl1 O1 109.7(2) . . ? O3 Cl1 O2 107.9(2) . . ? O4 Cl1 O2 111.5(3) . . ? O1 Cl1 O2 109.1(2) . . ? O7 Cl2 O6 113.9(5) . . ? O7 Cl2 O8 107.8(7) . . ? O6 Cl2 O8 101.1(6) . . ? O7 Cl2 O5 115.1(4) . . ? O6 Cl2 O5 111.2(3) . . ? O8 Cl2 O5 106.4(4) . . ? O10 C66 H66A 109.5 . . ? O10 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O10 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C66 O10 H10 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.691 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.061 data_zhou00006 _database_code_depnum_ccdc_archive 'CCDC 837604' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H45 Br4 Cd2 Cl3 N12' _chemical_formula_weight 1620.90 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 15.643(5) _cell_length_b 51.938(5) _cell_length_c 16.613(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.008(5) _cell_angle_gamma 90.000(5) _cell_volume 12232(5) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 19.45 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6352 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4206 _exptl_absorpt_correction_T_max 0.7216 _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 72453 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -61 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21542 _reflns_number_gt 10137 _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_number_reflns 21542 _refine_ls_number_parameters 1513 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1906 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2479 _refine_ls_wR_factor_gt 0.2143 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.249 _refine_ls_shift/su_max 0.020 _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 N6 N 0.2344(7) 0.1000(2) -0.5006(8) 0.089(3) Uani 1 1 d . . . C30 C 0.3108(9) 0.1037(2) -0.4258(9) 0.079(4) Uani 1 1 d . . . H30 H 0.3478 0.0908 -0.3887 0.095 Uiso 1 1 calc R . . Cd1 Cd 1.16691(6) 0.304305(16) 0.45891(6) 0.0732(3) Uani 1 1 d . . . Cd2 Cd 0.36208(6) 0.561637(16) 0.00871(6) 0.0731(3) Uani 1 1 d . . . Cd3 Cd 0.58189(6) 0.573012(17) 0.54384(6) 0.0807(3) Uani 1 1 d . . . Cd4 Cd -0.06905(6) 0.328712(17) -0.06838(6) 0.0792(3) Uani 1 1 d . . . Br1 Br 1.10636(10) 0.31203(2) 0.58468(9) 0.0862(4) Uani 1 1 d . . . Br6 Br 0.54945(12) 0.56600(3) 0.68947(10) 0.1088(5) Uani 1 1 d . . . Br2 Br 1.32518(11) 0.32231(3) 0.51817(17) 0.1598(9) Uani 1 1 d . . . Br4 Br 0.20183(13) 0.57737(4) -0.0478(2) 0.2021(13) Uani 1 1 d . . . Br7 Br -0.03088(14) 0.33418(3) -0.21047(10) 0.1216(6) Uani 1 1 d . . . Br8 Br -0.21379(11) 0.34253(4) -0.06572(15) 0.1722(11) Uani 1 1 d . . . N8 N 0.4720(6) 0.53802(16) 0.1302(5) 0.055(2) Uani 1 1 d . . . N20 N 0.0425(6) 0.30632(16) 0.0519(6) 0.056(2) Uani 1 1 d . . . N14 N 0.4797(6) 0.55257(17) 0.4098(6) 0.057(2) Uani 1 1 d . . . N2 N 1.0617(6) 0.28288(15) 0.3264(6) 0.053(2) Uani 1 1 d . . . C68 C 0.4893(6) 0.5281(2) 0.3947(7) 0.055(3) Uani 1 1 d . . . N4 N 0.3266(6) 0.12898(17) -0.4117(6) 0.066(3) Uani 1 1 d . . . C37 C 0.5360(8) 0.5510(2) 0.2030(8) 0.058(3) Uani 1 1 d . . . N9 N 0.3436(6) 0.51656(17) -0.0197(6) 0.062(2) Uani 1 1 d . . . C47 C 0.7061(7) 0.4990(2) 0.3171(7) 0.056(3) Uani 1 1 d . . . N1 N 1.0772(7) 0.33412(16) 0.3458(6) 0.070(3) Uani 1 1 d . . . C42 C 0.4088(6) 0.5008(2) 0.0372(7) 0.052(3) Uani 1 1 d . . . C41 C 0.4816(7) 0.51289(18) 0.1191(7) 0.055(3) Uani 1 1 d . . . C98 C -0.0360(7) 0.2678(2) -0.0236(7) 0.050(3) Uani 1 1 d . . . C91 C -0.1234(8) 0.4151(2) -0.3232(8) 0.078(3) Uani 1 1 d U . . C44 C 0.3313(8) 0.4646(2) -0.0532(8) 0.073(3) Uani 1 1 d . . . H44 H 0.3277 0.4470 -0.0637 0.088 Uiso 1 1 calc R . . C39 C 0.6238(7) 0.5126(2) 0.2532(7) 0.057(3) Uani 1 1 d . . . N13 N 0.6288(6) 0.53092(17) 0.5319(6) 0.065(3) Uani 1 1 d . . . C69 C 0.4255(7) 0.5146(2) 0.3179(7) 0.056(3) Uani 1 1 d . . . H69 H 0.4371 0.4975 0.3088 0.067 Uiso 1 1 calc R . . N5 N 0.2568(7) 0.1424(2) -0.4788(7) 0.081(3) Uani 1 1 d . . . N21 N 0.0299(6) 0.35774(17) 0.0424(6) 0.064(2) Uani 1 1 d . . . C11 C 1.1402(7) 0.2444(2) 0.3975(7) 0.058(3) Uani 1 1 d . . . C103 C 0.1097(7) 0.31906(19) 0.1183(8) 0.055(3) Uani 1 1 d . . . N10 N 1.2650(7) 0.3836(2) 0.7760(7) 0.080(3) Uani 1 1 d . . . C38 C 0.6116(7) 0.5389(2) 0.2633(7) 0.058(3) Uani 1 1 d . . . H38 H 0.6556 0.5479 0.3114 0.069 Uiso 1 1 calc R . . N3 N 1.1975(6) 0.25966(16) 0.4633(6) 0.066(3) Uani 1 1 d . . . C6 C 0.9958(8) 0.2962(2) 0.2596(8) 0.060(3) Uani 1 1 d . . . C43 C 0.4025(7) 0.4744(2) 0.0209(7) 0.066(3) Uani 1 1 d . . . H43 H 0.4472 0.4634 0.0609 0.079 Uiso 1 1 calc R . . C100 C 0.1093(7) 0.2668(2) 0.1170(7) 0.059(3) Uani 1 1 d . . . H100 H 0.1066 0.2489 0.1152 0.071 Uiso 1 1 calc R . . C71 C 0.3411(7) 0.5532(2) 0.2758(7) 0.061(3) Uani 1 1 d . . . H71 H 0.2915 0.5629 0.2356 0.073 Uiso 1 1 calc R . . C16 C 0.8438(8) 0.2431(2) 0.1136(7) 0.063(3) Uani 1 1 d . . . N16 N -0.1869(6) 0.40255(19) -0.4076(7) 0.076(3) Uani 1 1 d . . . C117 C 0.5731(7) 0.1871(2) 0.5490(8) 0.068(3) Uani 1 1 d . . . C110 C 0.2687(7) 0.2385(2) 0.2524(8) 0.072(3) Uani 1 1 d . . . H110 H 0.2269 0.2298 0.2024 0.087 Uiso 1 1 calc R . . C29 C 0.3992(7) 0.1417(2) -0.3400(7) 0.061(3) Uani 1 1 d . . . C46 C 0.2747(7) 0.5058(2) -0.0929(8) 0.068(3) Uani 1 1 d . . . H46 H 0.2305 0.5168 -0.1332 0.082 Uiso 1 1 calc R . . C21 C 0.6958(8) 0.2174(2) -0.0243(8) 0.071(3) Uani 1 1 d . . . C60 C 1.1404(9) 0.3868(3) 0.6241(10) 0.109(5) Uani 1 1 d . . . H60 H 1.1559 0.3704 0.6124 0.130 Uiso 1 1 calc R . . C79 C 0.2052(7) 0.5260(2) 0.1140(7) 0.073(3) Uani 1 1 d . . . H79 H 0.2006 0.5437 0.1182 0.088 Uiso 1 1 calc R . . C70 C 0.3484(7) 0.5267(2) 0.2586(7) 0.060(3) Uani 1 1 d . . . C122 C 0.7111(7) 0.1614(2) 0.6970(8) 0.062(3) Uani 1 1 d U . . C10 C 1.0604(7) 0.25711(19) 0.3225(7) 0.055(3) Uani 1 1 d . . . C26 C 0.4555(8) 0.1801(2) -0.2474(9) 0.096(4) Uani 1 1 d . . . H26 H 0.4458 0.1969 -0.2343 0.115 Uiso 1 1 calc R . . C48 C 0.7759(8) 0.5119(2) 0.3878(8) 0.077(4) Uani 1 1 d . . . H48 H 0.7708 0.5296 0.3935 0.092 Uiso 1 1 calc R . . C86 C 0.0030(8) 0.4390(2) -0.1641(7) 0.068(3) Uani 1 1 d . . . C96 C -0.1235(7) 0.2319(2) -0.1045(8) 0.067(3) Uani 1 1 d . . . H96 H -0.1322 0.2142 -0.1109 0.081 Uiso 1 1 calc R . . C50 C 0.8505(8) 0.4994(3) 0.4478(8) 0.076(4) Uani 1 1 d . . . H50 H 0.8964 0.5086 0.4937 0.091 Uiso 1 1 calc R . . C52 C 0.8607(7) 0.4733(2) 0.4430(8) 0.064(3) Uani 1 1 d . . . N19 N -0.0974(6) 0.28387(17) -0.0840(6) 0.069(3) Uani 1 1 d . . . C7 C 0.9260(7) 0.2839(2) 0.1912(7) 0.061(3) Uani 1 1 d . . . H7 H 0.8805 0.2936 0.1463 0.073 Uiso 1 1 calc R . . C40 C 0.5562(7) 0.50003(19) 0.1787(7) 0.054(3) Uani 1 1 d . . . H40 H 0.5630 0.4826 0.1704 0.065 Uiso 1 1 calc R . . C85 C 0.0723(7) 0.4513(3) -0.0793(7) 0.076(4) Uani 1 1 d . . . H85 H 0.1220 0.4410 -0.0424 0.091 Uiso 1 1 calc R . . C5 C 1.0048(8) 0.3244(2) 0.2696(8) 0.067(3) Uani 1 1 d . . . N15 N 0.4722(7) 0.60178(19) 0.4506(7) 0.082(3) Uani 1 1 d . . . C59 C 1.1924(8) 0.3983(2) 0.7097(8) 0.078(4) Uani 1 1 d . . . C78 C 0.2782(7) 0.5128(2) 0.1813(7) 0.056(3) Uani 1 1 d . . . C109 C 0.2596(7) 0.2650(2) 0.2600(7) 0.064(3) Uani 1 1 d . . . C67 C 0.5738(7) 0.5156(2) 0.4627(7) 0.056(3) Uani 1 1 d . . . C82 C 0.2150(7) 0.4736(2) 0.0957(7) 0.072(3) Uani 1 1 d . . . H82 H 0.2205 0.4558 0.0918 0.087 Uiso 1 1 calc R . . C114 C 0.4036(8) 0.2375(2) 0.3929(8) 0.069(3) Uani 1 1 d . . . C51 C 0.7929(8) 0.4600(2) 0.3748(8) 0.072(3) Uani 1 1 d . . . H51 H 0.7990 0.4423 0.3703 0.087 Uiso 1 1 calc R . . C116 C 0.4997(8) 0.2004(2) 0.4755(8) 0.073(3) Uani 1 1 d . . . H116 H 0.4618 0.1901 0.4281 0.088 Uiso 1 1 calc R . . C8 C 0.9212(7) 0.25697(19) 0.1873(7) 0.053(3) Uani 1 1 d . . . C27 C 0.4780(8) 0.1305(2) -0.2908(8) 0.083(4) Uani 1 1 d . . . H27 H 0.4884 0.1136 -0.3029 0.100 Uiso 1 1 calc R . . C36 C 0.5139(9) 0.5787(2) 0.2083(9) 0.068(3) Uani 1 1 d . . . C99 C 0.0427(7) 0.28063(19) 0.0511(7) 0.053(3) Uani 1 1 d . . . N22 N 0.7783(6) 0.14808(19) 0.7719(7) 0.071(3) Uani 1 1 d . . . N11 N 1.3292(7) 0.3963(2) 0.8525(7) 0.079(3) Uani 1 1 d . . . C119 C 0.6280(9) 0.1998(2) 0.6310(9) 0.098(5) Uani 1 1 d . . . H119 H 0.6176 0.2173 0.6358 0.118 Uiso 1 1 calc R . . C74 C 0.3368(8) 0.6098(2) 0.3150(9) 0.081(4) Uani 1 1 d . . . H74 H 0.2902 0.6038 0.2617 0.097 Uiso 1 1 calc R . . C53 C 0.9419(8) 0.4611(2) 0.5116(8) 0.076(4) Uani 1 1 d . . . H53 H 0.9804 0.4709 0.5604 0.091 Uiso 1 1 calc R . . C73 C 0.4024(8) 0.5936(2) 0.3715(8) 0.065(3) Uani 1 1 d . . . C83 C 0.1418(7) 0.4866(2) 0.0286(7) 0.065(3) Uani 1 1 d . . . C63 C 0.7074(8) 0.5210(3) 0.5925(8) 0.082(4) Uani 1 1 d . . . H63 H 0.7465 0.5314 0.6391 0.099 Uiso 1 1 calc R . . N23 N 0.8389(7) 0.1617(2) 0.8456(7) 0.082(3) Uani 1 1 d . . . C55 C 1.0483(8) 0.4242(2) 0.5784(8) 0.073(3) Uani 1 1 d . . . C97 C -0.0472(7) 0.2420(2) -0.0318(8) 0.066(3) Uani 1 1 d . . . H97 H -0.0045 0.2312 0.0106 0.079 Uiso 1 1 calc R . . C66 C 0.5955(7) 0.4896(2) 0.4536(7) 0.058(3) Uani 1 1 d . . . H66 H 0.5576 0.4795 0.4057 0.069 Uiso 1 1 calc R . . C104 C 0.1039(8) 0.3480(2) 0.1139(8) 0.063(3) Uani 1 1 d . . . C72 C 0.4075(8) 0.5648(2) 0.3526(8) 0.059(3) Uani 1 1 d . . . C45 C 0.2651(7) 0.4807(2) -0.1122(8) 0.067(3) Uani 1 1 d . . . H45 H 0.2158 0.4745 -0.1631 0.080 Uiso 1 1 calc R . . C81 C 0.1397(9) 0.5132(3) 0.0411(8) 0.083(4) Uani 1 1 d . . . H81 H 0.0918 0.5227 -0.0019 0.100 Uiso 1 1 calc R . . C89 C -0.1356(8) 0.4396(3) -0.3074(9) 0.100(5) Uani 1 1 d . . . H89 H -0.1847 0.4491 -0.3493 0.119 Uiso 1 1 calc R . . C58 C 1.1767(9) 0.4213(2) 0.7287(9) 0.097(5) Uani 1 1 d . . . H58 H 1.2130 0.4286 0.7838 0.116 Uiso 1 1 calc R . . C9 C 0.9924(7) 0.2439(2) 0.2569(7) 0.060(3) Uani 1 1 d . . . H9 H 0.9928 0.2260 0.2579 0.072 Uiso 1 1 calc R . . C105 C 0.1669(9) 0.3638(2) 0.1811(9) 0.085(4) Uani 1 1 d . . . H105 H 0.2155 0.3568 0.2311 0.102 Uiso 1 1 calc R . . C101 C 0.1826(7) 0.2793(2) 0.1883(7) 0.059(3) Uani 1 1 d . . . C65 C 0.6756(8) 0.4808(2) 0.5199(8) 0.072(3) Uani 1 1 d . . . H65 H 0.6929 0.4637 0.5190 0.087 Uiso 1 1 calc R . . C49 C 0.7149(8) 0.4727(2) 0.3121(7) 0.075(4) Uani 1 1 d . . . H49 H 0.6685 0.4634 0.2667 0.090 Uiso 1 1 calc R . . C115 C 0.4801(8) 0.2244(3) 0.4667(8) 0.080(4) Uani 1 1 d . . . H115 H 0.5192 0.2349 0.5130 0.096 Uiso 1 1 calc R . . C34 C 0.5458(12) 0.6192(3) 0.2860(12) 0.101(5) Uani 1 1 d . . . H34 H 0.5780 0.6296 0.3353 0.121 Uiso 1 1 calc R . . N7 N 0.4412(7) 0.58834(17) 0.1376(7) 0.074(3) Uani 1 1 d . . . N18 N -0.2642(8) 0.3754(3) -0.5182(8) 0.112(4) Uani 1 1 d . . . C1 C 1.0905(10) 0.3592(2) 0.3564(9) 0.087(4) Uani 1 1 d . . . H1 H 1.1414 0.3654 0.4062 0.104 Uiso 1 1 calc R . . C90 C -0.0495(9) 0.4015(3) -0.2644(9) 0.106(4) Uani 1 1 d U . . H90 H -0.0389 0.3845 -0.2756 0.128 Uiso 1 1 calc R . . C25 C 0.5469(9) 0.1433(2) -0.2208(9) 0.091(4) Uani 1 1 d . . . H25 H 0.6027 0.1346 -0.1875 0.109 Uiso 1 1 calc R . . C121 C 0.6986(9) 0.1869(2) 0.7061(9) 0.093(4) Uani 1 1 d . . . H121 H 0.7341 0.1956 0.7586 0.111 Uiso 1 1 calc R . . C19 C 0.7726(9) 0.2042(2) 0.0377(8) 0.090(4) Uani 1 1 d . . . H19 H 0.7760 0.1864 0.0345 0.109 Uiso 1 1 calc R . . C12 C 1.1534(8) 0.2183(2) 0.3991(9) 0.086(4) Uani 1 1 d . . . H12 H 1.1106 0.2079 0.3545 0.103 Uiso 1 1 calc R . . C113 C 0.3962(8) 0.2643(3) 0.3991(9) 0.095(4) Uani 1 1 d . . . H113 H 0.4403 0.2731 0.4475 0.115 Uiso 1 1 calc R . . C54 C 0.9634(8) 0.4372(2) 0.5078(8) 0.073(3) Uani 1 1 d . . . H54 H 0.9244 0.4275 0.4589 0.088 Uiso 1 1 calc R . . C77 C 0.4714(11) 0.6276(3) 0.4717(10) 0.098(4) Uani 1 1 d . . . H77 H 0.5158 0.6335 0.5263 0.118 Uiso 1 1 calc R . . C94 C -0.1696(8) 0.2740(2) -0.1523(9) 0.083(4) Uani 1 1 d . . . H94 H -0.2125 0.2851 -0.1936 0.099 Uiso 1 1 calc R . . C76 C 0.4100(11) 0.6440(3) 0.4172(11) 0.101(5) Uani 1 1 d . . . H76 H 0.4132 0.6614 0.4318 0.121 Uiso 1 1 calc R . . C17 C 0.8436(8) 0.2175(2) 0.1038(8) 0.092(5) Uani 1 1 d . . . H17 H 0.8945 0.2082 0.1441 0.111 Uiso 1 1 calc R . . C80 C 0.2807(7) 0.4870(2) 0.1692(7) 0.065(3) Uani 1 1 d . . . H80 H 0.3291 0.4776 0.2123 0.077 Uiso 1 1 calc R . . C84 C 0.0706(8) 0.4744(3) -0.0520(9) 0.082(4) Uani 1 1 d . . . H84 H 0.0190 0.4844 -0.0868 0.098 Uiso 1 1 calc R . . C4 C 0.9446(8) 0.3408(2) 0.2033(9) 0.078(4) Uani 1 1 d . . . H4 H 0.8973 0.3345 0.1511 0.094 Uiso 1 1 calc R . . C102 C 0.1800(7) 0.3068(2) 0.1874(7) 0.063(3) Uani 1 1 d . . . H102 H 0.2254 0.3162 0.2333 0.076 Uiso 1 1 calc R . . C32 C 0.4198(11) 0.6131(3) 0.1414(11) 0.098(5) Uani 1 1 d . . . H32 H 0.3682 0.6202 0.0943 0.118 Uiso 1 1 calc R . . C15 C 1.2723(8) 0.2492(2) 0.5309(8) 0.076(4) Uani 1 1 d . . . H15 H 1.3125 0.2597 0.5764 0.091 Uiso 1 1 calc R . . N17 N -0.2571(7) 0.4165(2) -0.4722(7) 0.087(3) Uani 1 1 d . . . C118 C 0.5899(8) 0.1616(2) 0.5460(9) 0.092(4) Uani 1 1 d U . . H118 H 0.5552 0.1526 0.4939 0.110 Uiso 1 1 calc R . . C112 C 0.3394(8) 0.2255(2) 0.3189(8) 0.078(4) Uani 1 1 d . . . H112 H 0.3441 0.2078 0.3135 0.093 Uiso 1 1 calc R . . C106 C 0.1540(11) 0.3899(3) 0.1701(10) 0.097(4) Uani 1 1 d . . . H106 H 0.1962 0.4011 0.2119 0.117 Uiso 1 1 calc R . . C57 C 1.0686(9) 0.4000(2) 0.5601(9) 0.098(5) Uani 1 1 d . . . H57 H 1.0339 0.3926 0.5048 0.118 Uiso 1 1 calc R . . C18 C 0.7676(8) 0.2567(2) 0.0527(8) 0.085(4) Uani 1 1 d . . . H18 H 0.7652 0.2745 0.0568 0.101 Uiso 1 1 calc R . . C111 C 0.3255(9) 0.2772(2) 0.3353(8) 0.089(4) Uani 1 1 d . . . H111 H 0.3204 0.2948 0.3415 0.107 Uiso 1 1 calc R . . C64 C 0.7330(8) 0.4966(2) 0.5895(8) 0.073(3) Uani 1 1 d . . . H64 H 0.7887 0.4903 0.6336 0.087 Uiso 1 1 calc R . . C20 C 0.6952(8) 0.2437(2) -0.0143(8) 0.088(4) Uani 1 1 d . . . H20 H 0.6442 0.2530 -0.0542 0.105 Uiso 1 1 calc R . . C123 C 0.7941(8) 0.1234(2) 0.7858(9) 0.079(4) Uani 1 1 d . . . H123 H 0.7618 0.1106 0.7450 0.095 Uiso 1 1 calc R . . N24 N 0.8643(9) 0.1189(2) 0.8682(9) 0.101(4) Uani 1 1 d . . . C88 C 0.0109(9) 0.4142(3) -0.1850(9) 0.104(4) Uani 1 1 d U . . H88 H 0.0602 0.4046 -0.1437 0.125 Uiso 1 1 calc R . . C28 C 0.3876(8) 0.1670(2) -0.3170(8) 0.084(4) Uani 1 1 d . . . H28 H 0.3311 0.1754 -0.3506 0.101 Uiso 1 1 calc R . . C95 C -0.1841(8) 0.2478(3) -0.1648(8) 0.074(3) Uani 1 1 d . . . H95 H -0.2350 0.2413 -0.2142 0.089 Uiso 1 1 calc R . . C75 C 0.3410(10) 0.6351(3) 0.3386(10) 0.095(4) Uani 1 1 d . . . H75 H 0.2964 0.6466 0.3007 0.114 Uiso 1 1 calc R . . C93 C -0.2970(9) 0.3993(3) -0.5334(10) 0.103(5) Uani 1 1 d . . . H93 H -0.3474 0.4036 -0.5867 0.124 Uiso 1 1 calc R . . C56 C 1.1018(9) 0.4351(2) 0.6623(9) 0.100(5) Uani 1 1 d . . . H56 H 1.0878 0.4517 0.6744 0.120 Uiso 1 1 calc R . . C92 C -0.1924(9) 0.3783(2) -0.4362(9) 0.086(4) Uani 1 1 d . . . H92 H -0.1522 0.3651 -0.4041 0.103 Uiso 1 1 calc R . . Br3 Br 0.42176(9) 0.57673(2) -0.11042(9) 0.0800(4) Uani 1 1 d . . . C124 C 0.8860(9) 0.1433(3) 0.8988(10) 0.099(5) Uani 1 1 d . . . H124 H 0.9325 0.1467 0.9553 0.119 Uiso 1 1 calc R . . C22 C 0.6199(9) 0.2047(2) -0.0966(8) 0.091(4) Uani 1 1 d . . . H22 H 0.5683 0.2150 -0.1293 0.109 Uiso 1 1 calc R . . C87 C -0.0732(9) 0.4515(3) -0.2256(9) 0.098(5) Uani 1 1 d . . . H87 H -0.0851 0.4683 -0.2142 0.117 Uiso 1 1 calc R . . Br5 Br 0.72158(12) 0.59497(4) 0.55597(16) 0.1843(12) Uani 1 1 d . . . C23 C 0.6134(7) 0.1818(3) -0.1219(7) 0.073(3) Uani 1 1 d . . . H23 H 0.6648 0.1716 -0.0872 0.088 Uiso 1 1 calc R . . C31 C 0.2069(10) 0.1242(3) -0.5297(10) 0.096(4) Uani 1 1 d . . . H31 H 0.1553 0.1275 -0.5832 0.115 Uiso 1 1 calc R . . C24 C 0.5378(8) 0.1674(2) -0.1982(8) 0.070(3) Uani 1 1 d . . . C2 C 1.0318(11) 0.3762(2) 0.2962(11) 0.097(5) Uani 1 1 d . . . H2 H 1.0406 0.3938 0.3067 0.117 Uiso 1 1 calc R . . C14 C 1.2901(8) 0.2238(3) 0.5339(9) 0.085(4) Uani 1 1 d . . . H14 H 1.3427 0.2171 0.5809 0.102 Uiso 1 1 calc R . . C13 C 1.2306(9) 0.2075(2) 0.4673(9) 0.087(4) Uani 1 1 d . . . H13 H 1.2425 0.1899 0.4689 0.105 Uiso 1 1 calc R . . C3 C 0.9592(11) 0.3673(2) 0.2195(11) 0.097(4) Uani 1 1 d . . . H3 H 0.9195 0.3790 0.1783 0.116 Uiso 1 1 calc R . . C35 C 0.5707(9) 0.5944(2) 0.2846(9) 0.082(4) Uani 1 1 d . . . H35 H 0.6231 0.5875 0.3314 0.098 Uiso 1 1 calc R . . C33 C 0.4725(14) 0.6286(3) 0.2137(15) 0.124(7) Uani 1 1 d . . . H33 H 0.4568 0.6459 0.2123 0.149 Uiso 1 1 calc R . . N12 N 1.3569(9) 0.3536(3) 0.8588(9) 0.113(4) Uani 1 1 d . . . C62 C 1.3802(9) 0.3764(4) 0.8984(10) 0.097(5) Uani 1 1 d . . . H62 H 1.4290 0.3784 0.9548 0.117 Uiso 1 1 calc R . . C61 C 1.2850(9) 0.3585(3) 0.7803(10) 0.092(4) Uani 1 1 d . . . H61 H 1.2542 0.3464 0.7360 0.110 Uiso 1 1 calc R . . C107 C 0.0781(12) 0.3997(3) 0.0967(11) 0.109(5) Uani 1 1 d . . . H107 H 0.0674 0.4173 0.0886 0.131 Uiso 1 1 calc R . . C108 C 0.0208(10) 0.3825(3) 0.0378(9) 0.092(4) Uani 1 1 d . . . H108 H -0.0304 0.3891 -0.0109 0.110 Uiso 1 1 calc R . . C120 C 0.6556(8) 0.1488(2) 0.6159(9) 0.093(4) Uani 1 1 d U . . H120 H 0.6645 0.1313 0.6105 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.6038(3) 0.21637(8) 0.1335(3) 0.1163(13) Uani 1 1 d . . . Cl2 Cl 0.5075(3) 0.24512(9) 0.2140(3) 0.1503(18) Uani 1 1 d . . . Cl3 Cl 0.5958(4) 0.19814(9) 0.3007(4) 0.161(2) Uani 1 1 d . . . C125 C 0.5327(11) 0.2130(3) 0.1938(11) 0.127(6) Uani 1 1 d . . . H125 H 0.4744 0.2036 0.1586 0.153 Uiso 1 1 calc R . . Cl4 Cl 1.0688(3) 0.46698(10) 0.1954(3) 0.1374(16) Uani 1 1 d U . . Cl5 Cl 0.9636(3) 0.48954(10) 0.2779(3) 0.1444(18) Uani 1 1 d U . . Cl6 Cl 1.0745(4) 0.44512(10) 0.3579(4) 0.174(2) Uani 1 1 d . . . C126 C 0.9710(15) 0.4538(3) 0.2369(13) 0.196(8) Uani 1 1 d U . . H126 H 0.9170 0.4428 0.2023 0.235 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 N6 0.071(7) 0.072(8) 0.104(9) -0.014(7) 0.019(7) -0.026(6) C30 0.067(8) 0.053(8) 0.101(10) -0.012(7) 0.021(8) -0.008(6) Cd1 0.0602(5) 0.0517(5) 0.0910(7) -0.0145(5) 0.0156(5) -0.0131(4) Cd2 0.0657(6) 0.0517(5) 0.1013(7) 0.0200(5) 0.0347(5) 0.0216(4) Cd3 0.0724(6) 0.0596(6) 0.0808(6) 0.0002(5) 0.0039(5) -0.0108(5) Cd4 0.0779(6) 0.0591(6) 0.0764(6) -0.0028(5) 0.0092(5) 0.0224(5) Br1 0.0920(9) 0.0643(8) 0.0916(10) -0.0134(7) 0.0284(8) -0.0040(7) Br6 0.1379(14) 0.0896(11) 0.0849(10) -0.0015(8) 0.0334(10) 0.0274(10) Br2 0.0782(11) 0.0946(12) 0.285(3) -0.0649(15) 0.0560(14) -0.0370(9) Br4 0.1041(13) 0.1219(15) 0.400(4) 0.123(2) 0.1261(19) 0.0725(12) Br7 0.2080(19) 0.0607(9) 0.0951(11) 0.0036(8) 0.0630(12) 0.0059(10) Br8 0.0745(11) 0.181(2) 0.198(2) -0.0820(17) -0.0039(12) 0.0546(12) N8 0.051(5) 0.045(5) 0.060(6) 0.004(5) 0.014(5) 0.008(4) N20 0.048(5) 0.051(6) 0.068(6) -0.003(5) 0.022(5) 0.008(5) N14 0.040(5) 0.050(6) 0.070(6) 0.006(5) 0.011(5) -0.005(4) N2 0.050(5) 0.036(5) 0.065(6) -0.004(5) 0.015(5) -0.010(4) C68 0.030(6) 0.057(7) 0.075(8) 0.011(7) 0.019(6) -0.002(5) N4 0.043(5) 0.054(6) 0.085(7) -0.009(6) 0.011(5) -0.005(5) C37 0.063(7) 0.050(7) 0.075(8) 0.004(6) 0.044(7) 0.010(6) N9 0.040(5) 0.061(6) 0.081(7) 0.011(5) 0.021(5) 0.010(5) C47 0.051(7) 0.054(7) 0.061(7) -0.005(6) 0.021(6) 0.001(6) N1 0.075(7) 0.043(6) 0.078(7) 0.001(5) 0.020(6) -0.012(5) C42 0.038(6) 0.048(7) 0.060(7) -0.002(6) 0.011(5) 0.002(5) C41 0.055(7) 0.031(6) 0.077(8) 0.008(6) 0.026(6) 0.016(5) C98 0.038(6) 0.050(7) 0.054(7) -0.014(6) 0.011(5) -0.006(5) C91 0.069(7) 0.065(7) 0.084(8) 0.012(6) 0.018(6) -0.003(6) C44 0.059(7) 0.058(8) 0.090(9) 0.003(7) 0.020(7) 0.001(7) C39 0.060(7) 0.050(7) 0.065(7) -0.001(6) 0.031(6) 0.005(6) N13 0.046(5) 0.061(6) 0.071(6) -0.002(5) 0.008(5) -0.016(5) C69 0.045(6) 0.064(7) 0.061(7) -0.009(6) 0.025(6) 0.006(6) N5 0.062(6) 0.076(7) 0.081(7) 0.000(6) 0.007(6) 0.000(6) N21 0.072(6) 0.045(6) 0.072(6) 0.003(5) 0.027(6) 0.018(5) C11 0.050(7) 0.042(7) 0.077(8) -0.004(6) 0.024(6) -0.018(6) C103 0.053(7) 0.037(6) 0.080(8) -0.007(6) 0.032(7) 0.001(5) N10 0.058(6) 0.076(8) 0.089(8) 0.000(7) 0.013(6) 0.011(6) C38 0.045(6) 0.063(8) 0.061(7) -0.009(6) 0.020(6) 0.005(6) N3 0.050(6) 0.046(5) 0.091(7) -0.009(5) 0.020(5) -0.001(5) C6 0.054(7) 0.052(7) 0.073(8) -0.002(7) 0.028(7) -0.017(6) C43 0.045(7) 0.055(8) 0.078(8) 0.010(6) 0.008(6) 0.004(6) C100 0.061(7) 0.048(7) 0.074(8) -0.011(6) 0.033(7) 0.001(6) C71 0.054(7) 0.051(7) 0.073(8) 0.015(6) 0.021(6) 0.007(6) C16 0.064(8) 0.061(8) 0.056(7) 0.004(6) 0.019(6) -0.013(6) N16 0.045(6) 0.064(7) 0.097(8) -0.005(6) 0.007(6) -0.005(5) C117 0.032(6) 0.071(8) 0.083(9) -0.005(7) 0.006(6) 0.008(6) C110 0.054(7) 0.046(7) 0.090(9) -0.004(7) 0.004(7) 0.002(6) C29 0.052(7) 0.053(7) 0.073(8) 0.000(6) 0.021(6) -0.003(6) C46 0.040(7) 0.077(9) 0.080(9) 0.020(7) 0.017(7) 0.009(6) C21 0.059(7) 0.063(8) 0.065(8) 0.004(7) 0.000(6) -0.003(6) C60 0.089(10) 0.084(10) 0.113(12) -0.020(9) 0.004(9) 0.033(8) C79 0.062(7) 0.059(7) 0.067(8) -0.005(7) -0.005(7) 0.001(6) C70 0.047(7) 0.074(8) 0.056(7) 0.009(6) 0.018(6) 0.004(6) C122 0.043(6) 0.052(6) 0.081(7) 0.013(5) 0.018(5) -0.002(5) C10 0.049(6) 0.038(6) 0.071(8) 0.005(6) 0.018(6) -0.001(5) C26 0.059(8) 0.071(9) 0.120(11) -0.030(9) 0.003(8) -0.014(7) C48 0.050(7) 0.070(8) 0.107(10) 0.013(8) 0.031(8) -0.002(7) C86 0.056(7) 0.060(8) 0.062(8) 0.001(6) -0.001(6) -0.005(6) C96 0.040(6) 0.056(7) 0.097(9) -0.017(7) 0.020(7) -0.003(6) C50 0.055(8) 0.075(9) 0.080(9) 0.005(8) 0.012(7) -0.005(7) C52 0.031(6) 0.071(9) 0.078(8) -0.002(7) 0.010(6) -0.001(6) N19 0.044(5) 0.063(6) 0.082(7) -0.003(6) 0.009(5) 0.009(5) C7 0.044(6) 0.051(7) 0.078(8) 0.009(6) 0.017(6) -0.003(5) C40 0.068(7) 0.036(6) 0.064(7) -0.011(6) 0.033(6) -0.003(6) C85 0.042(7) 0.094(10) 0.065(8) 0.008(8) -0.003(6) -0.001(7) C5 0.060(7) 0.059(8) 0.094(9) 0.023(7) 0.042(7) 0.007(6) N15 0.074(7) 0.063(7) 0.085(7) -0.011(6) 0.012(6) -0.014(5) C59 0.051(7) 0.062(8) 0.082(9) -0.007(7) -0.010(7) 0.001(6) C78 0.042(6) 0.068(8) 0.050(7) -0.007(6) 0.012(6) -0.001(6) C109 0.053(7) 0.064(8) 0.064(8) 0.005(6) 0.016(6) 0.003(6) C67 0.051(7) 0.059(7) 0.062(7) 0.014(6) 0.027(6) -0.003(6) C82 0.063(8) 0.066(8) 0.067(8) 0.017(7) 0.007(7) -0.005(6) C114 0.060(8) 0.062(8) 0.074(8) 0.013(7) 0.016(7) 0.002(6) C51 0.074(8) 0.054(7) 0.078(8) 0.010(7) 0.021(7) 0.012(7) C116 0.060(8) 0.067(9) 0.081(9) -0.021(7) 0.019(7) 0.003(7) C8 0.053(7) 0.041(6) 0.060(7) 0.005(6) 0.020(6) -0.012(5) C27 0.061(8) 0.052(7) 0.108(10) 0.006(7) 0.007(8) 0.013(7) C36 0.082(9) 0.034(6) 0.116(11) -0.002(7) 0.067(9) 0.004(6) C99 0.049(6) 0.041(7) 0.073(8) 0.013(6) 0.030(6) 0.013(5) N22 0.051(6) 0.057(7) 0.096(8) 0.009(6) 0.021(6) 0.002(5) N11 0.050(6) 0.077(7) 0.085(7) -0.007(6) 0.006(6) 0.002(6) C119 0.083(9) 0.057(8) 0.111(11) -0.014(8) -0.001(8) 0.018(7) C74 0.063(8) 0.063(9) 0.103(10) 0.002(8) 0.022(8) 0.009(7) C53 0.074(9) 0.063(8) 0.076(9) -0.015(7) 0.016(7) -0.008(7) C73 0.060(7) 0.049(7) 0.079(8) -0.001(7) 0.024(7) 0.007(6) C83 0.046(7) 0.082(9) 0.044(7) -0.002(7) -0.001(6) 0.004(6) C63 0.048(7) 0.090(11) 0.079(9) 0.009(8) -0.003(7) -0.016(7) N23 0.062(6) 0.085(8) 0.079(7) 0.014(7) 0.011(6) 0.001(6) C55 0.049(7) 0.067(8) 0.085(9) -0.004(7) 0.011(7) 0.008(6) C97 0.054(7) 0.054(8) 0.083(8) -0.008(7) 0.022(7) 0.001(6) C66 0.051(7) 0.052(7) 0.059(7) 0.008(6) 0.012(6) 0.000(5) C104 0.065(8) 0.063(8) 0.069(8) -0.012(7) 0.035(7) -0.001(7) C72 0.049(7) 0.051(7) 0.074(8) 0.003(6) 0.022(6) -0.007(6) C45 0.051(7) 0.054(8) 0.083(9) 0.000(7) 0.016(6) 0.011(6) C81 0.077(9) 0.087(10) 0.064(8) -0.003(8) 0.010(7) 0.003(8) C89 0.052(8) 0.080(10) 0.113(11) -0.016(9) -0.018(7) 0.017(7) C58 0.102(11) 0.062(9) 0.094(10) -0.040(8) 0.009(8) 0.006(8) C9 0.056(7) 0.045(6) 0.072(8) -0.009(6) 0.021(6) -0.022(6) C105 0.083(9) 0.060(9) 0.105(10) -0.023(8) 0.034(8) -0.017(7) C101 0.046(6) 0.070(8) 0.051(7) -0.009(6) 0.012(6) 0.003(6) C65 0.056(7) 0.074(8) 0.078(9) 0.010(7) 0.020(7) 0.015(7) C49 0.067(8) 0.074(9) 0.059(8) 0.000(7) 0.002(6) 0.003(7) C115 0.050(7) 0.080(10) 0.087(9) -0.001(8) 0.007(7) -0.005(7) C34 0.135(14) 0.053(9) 0.159(16) -0.035(10) 0.106(13) -0.009(9) N7 0.083(7) 0.052(6) 0.098(8) 0.019(6) 0.050(6) 0.035(5) N18 0.069(8) 0.111(11) 0.120(10) -0.044(9) 0.004(8) -0.012(7) C1 0.103(10) 0.037(7) 0.117(11) -0.006(8) 0.043(9) -0.016(7) C90 0.089(7) 0.068(7) 0.109(8) 0.018(6) -0.010(6) 0.007(6) C25 0.071(9) 0.063(9) 0.095(10) 0.007(8) -0.007(8) -0.007(7) C121 0.099(10) 0.050(8) 0.092(10) -0.010(7) 0.006(8) -0.023(7) C19 0.101(10) 0.054(8) 0.091(10) 0.010(7) 0.016(9) -0.015(8) C12 0.064(8) 0.067(9) 0.110(11) -0.011(8) 0.021(8) -0.016(7) C113 0.059(8) 0.084(10) 0.095(10) -0.008(8) -0.015(7) 0.007(7) C54 0.060(8) 0.070(9) 0.083(9) -0.009(7) 0.023(7) -0.007(7) C77 0.118(12) 0.064(10) 0.107(11) -0.010(9) 0.042(10) -0.015(9) C94 0.046(7) 0.072(9) 0.104(10) 0.016(8) 0.007(7) 0.010(7) C76 0.107(12) 0.072(10) 0.125(13) 0.014(10) 0.049(11) 0.024(9) C17 0.073(9) 0.061(9) 0.082(9) 0.008(7) -0.027(7) -0.019(7) C80 0.049(7) 0.056(8) 0.068(8) 0.004(6) 0.004(6) -0.003(6) C84 0.055(8) 0.076(9) 0.099(10) 0.006(8) 0.019(7) 0.000(7) C4 0.071(8) 0.061(8) 0.107(10) 0.003(8) 0.042(8) 0.005(7) C102 0.056(7) 0.061(8) 0.058(7) -0.011(6) 0.011(6) 0.009(6) C32 0.120(12) 0.050(8) 0.141(14) 0.002(9) 0.070(11) 0.031(8) C15 0.047(7) 0.060(8) 0.101(10) -0.002(7) 0.011(7) -0.017(6) N17 0.059(6) 0.090(8) 0.079(7) -0.014(7) -0.003(6) -0.006(6) C118 0.059(7) 0.064(7) 0.108(8) -0.003(6) -0.008(6) 0.003(6) C112 0.072(8) 0.050(7) 0.083(9) -0.012(7) 0.006(7) 0.002(7) C106 0.121(13) 0.071(10) 0.104(12) -0.012(9) 0.051(10) -0.022(9) C57 0.080(9) 0.069(9) 0.095(10) -0.022(8) -0.012(8) 0.030(7) C18 0.077(9) 0.061(8) 0.087(9) -0.006(7) 0.007(8) -0.001(7) C111 0.085(9) 0.066(9) 0.090(10) -0.007(8) 0.011(8) 0.006(8) C64 0.050(7) 0.064(8) 0.076(9) 0.014(7) 0.000(6) 0.005(7) C20 0.066(8) 0.059(9) 0.098(10) 0.001(8) -0.004(7) -0.005(7) C123 0.063(8) 0.057(9) 0.094(10) 0.013(7) 0.010(8) 0.004(7) N24 0.094(9) 0.074(8) 0.121(10) 0.028(8) 0.032(8) 0.020(7) C88 0.086(8) 0.066(8) 0.106(9) 0.020(7) -0.011(7) 0.009(6) C28 0.065(8) 0.050(8) 0.105(10) 0.007(7) 0.005(8) 0.014(6) C95 0.049(7) 0.076(9) 0.077(9) -0.005(8) 0.008(6) -0.003(7) C75 0.101(11) 0.063(10) 0.114(12) 0.013(9) 0.038(10) 0.014(8) C93 0.071(9) 0.072(10) 0.113(12) 0.002(9) -0.012(8) 0.001(8) C56 0.090(10) 0.046(7) 0.112(11) -0.002(8) -0.008(9) 0.029(7) C92 0.063(8) 0.063(9) 0.118(12) -0.024(8) 0.025(9) 0.000(7) Br3 0.0902(9) 0.0562(8) 0.0969(10) 0.0135(7) 0.0426(8) 0.0103(7) C124 0.051(8) 0.118(13) 0.103(11) 0.032(11) 0.008(8) -0.002(9) C22 0.087(10) 0.054(8) 0.091(10) -0.013(8) -0.002(8) -0.012(7) C87 0.074(9) 0.073(9) 0.109(11) -0.021(8) 0.004(9) -0.001(8) Br5 0.0893(12) 0.1404(17) 0.233(2) 0.0599(16) -0.0190(13) -0.0621(12) C23 0.046(7) 0.086(10) 0.062(8) 0.006(7) -0.002(6) -0.008(7) C31 0.078(9) 0.087(11) 0.097(11) -0.019(10) 0.011(8) -0.021(9) C24 0.057(8) 0.051(8) 0.086(9) 0.002(7) 0.016(7) 0.000(6) C2 0.112(12) 0.036(7) 0.135(13) -0.004(9) 0.043(10) 0.002(8) C14 0.041(7) 0.081(10) 0.116(11) 0.010(9) 0.017(7) -0.001(7) C13 0.070(9) 0.049(7) 0.120(11) 0.001(8) 0.018(8) 0.005(7) C3 0.110(12) 0.049(8) 0.130(13) 0.020(9) 0.049(10) 0.013(8) C35 0.088(9) 0.062(9) 0.098(10) 0.000(8) 0.043(8) -0.006(7) C33 0.160(18) 0.056(10) 0.20(2) 0.020(13) 0.118(16) 0.033(11) N12 0.075(9) 0.139(13) 0.118(11) 0.022(10) 0.035(8) 0.045(9) C62 0.062(9) 0.130(14) 0.087(11) -0.004(11) 0.018(8) 0.028(10) C61 0.067(9) 0.064(9) 0.116(12) 0.021(8) 0.011(9) 0.015(7) C107 0.144(15) 0.051(9) 0.130(14) 0.002(10) 0.054(12) 0.009(10) C108 0.120(12) 0.051(9) 0.091(10) 0.003(8) 0.031(9) 0.004(8) C120 0.064(6) 0.063(6) 0.109(7) -0.002(5) -0.005(5) 0.002(5) Cl1 0.101(3) 0.115(3) 0.120(3) 0.003(3) 0.035(2) 0.007(2) Cl2 0.125(4) 0.125(4) 0.183(5) -0.015(3) 0.047(3) 0.021(3) Cl3 0.207(5) 0.102(3) 0.162(4) 0.018(3) 0.066(4) -0.031(3) C125 0.116(12) 0.119(13) 0.146(14) 0.020(11) 0.053(12) 0.055(11) Cl4 0.110(3) 0.148(4) 0.148(4) -0.014(3) 0.049(3) 0.012(3) Cl5 0.121(3) 0.150(4) 0.145(4) -0.027(3) 0.039(3) 0.039(3) Cl6 0.223(6) 0.109(4) 0.197(5) 0.001(4) 0.096(5) -0.006(4) C126 0.30(2) 0.167(11) 0.24(2) 0.117(12) 0.22(2) 0.192(12) _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 N6 C30 1.325(13) . ? N6 C31 1.351(16) . ? C30 N4 1.337(13) . ? C30 H30 0.9300 . ? Cd1 N3 2.363(8) . ? Cd1 N1 2.381(9) . ? Cd1 N2 2.394(8) . ? Cd1 Br2 2.4317(18) . ? Cd1 Br1 2.6640(18) . ? Cd2 N8 2.366(8) . ? Cd2 N9 2.382(9) . ? Cd2 N7 2.408(10) . ? Cd2 Br4 2.4172(19) . ? Cd2 Br3 2.6392(17) . ? Cd3 N15 2.309(10) . ? Cd3 N13 2.341(9) . ? Cd3 N14 2.374(8) . ? Cd3 Br5 2.397(2) . ? Cd3 Br6 2.698(2) . ? Cd4 N20 2.332(8) . ? Cd4 N19 2.365(9) . ? Cd4 N21 2.376(9) . ? Cd4 Br8 2.393(2) . ? Cd4 Br7 2.683(2) . ? N8 C41 1.335(12) . ? N8 C37 1.376(13) . ? N20 C99 1.334(12) . ? N20 C103 1.335(12) . ? N14 C72 1.293(12) . ? N14 C68 1.316(12) . ? N2 C10 1.340(12) . ? N2 C6 1.343(12) . ? C68 C69 1.428(14) . ? C68 C67 1.478(13) . ? N4 N5 1.375(11) . ? N4 C29 1.413(13) . ? C37 C38 1.340(13) . ? C37 C36 1.492(14) . ? N9 C42 1.337(12) . ? N9 C46 1.359(13) . ? C47 C49 1.384(15) . ? C47 C48 1.391(14) . ? C47 C39 1.457(14) . ? N1 C1 1.318(13) . ? N1 C5 1.389(13) . ? C42 C43 1.392(14) . ? C42 C41 1.493(13) . ? C41 C40 1.346(13) . ? C98 C97 1.346(13) . ? C98 N19 1.347(12) . ? C98 C99 1.487(13) . ? C91 C89 1.329(16) . ? C91 C90 1.355(15) . ? C91 N16 1.483(15) . ? C44 C43 1.362(14) . ? C44 C45 1.368(14) . ? C44 H44 0.9300 . ? C39 C38 1.399(14) . ? C39 C40 1.403(13) . ? N13 C63 1.320(13) . ? N13 C67 1.364(12) . ? C69 C70 1.347(13) . ? C69 H69 0.9300 . ? N5 C31 1.289(15) . ? N21 C108 1.292(14) . ? N21 C104 1.358(13) . ? C11 N3 1.342(12) . ? C11 C12 1.370(15) . ? C11 C10 1.495(14) . ? C103 C102 1.366(13) . ? C103 C104 1.507(14) . ? N10 C61 1.335(14) . ? N10 N11 1.408(12) . ? N10 C59 1.424(14) . ? C38 H38 0.9300 . ? N3 C15 1.348(13) . ? C6 C7 1.356(13) . ? C6 C5 1.474(15) . ? C43 H43 0.9300 . ? C100 C99 1.354(13) . ? C100 C101 1.411(13) . ? C100 H100 0.9300 . ? C71 C72 1.395(14) . ? C71 C70 1.418(14) . ? C71 H71 0.9300 . ? C16 C17 1.337(15) . ? C16 C18 1.388(14) . ? C16 C8 1.493(14) . ? N16 C92 1.335(14) . ? N16 N17 1.375(12) . ? C117 C118 1.352(15) . ? C117 C119 1.429(15) . ? C117 C116 1.451(15) . ? C110 C112 1.366(14) . ? C110 C109 1.392(14) . ? C110 H110 0.9300 . ? C29 C27 1.294(13) . ? C29 C28 1.403(15) . ? C46 C45 1.333(15) . ? C46 H46 0.9300 . ? C21 C20 1.373(15) . ? C21 C19 1.389(15) . ? C21 C22 1.445(15) . ? C60 C57 1.361(16) . ? C60 C59 1.435(16) . ? C60 H60 0.9300 . ? C79 C81 1.381(14) . ? C79 C78 1.394(13) . ? C79 H79 0.9300 . ? C70 C78 1.479(14) . ? C122 C121 1.356(15) . ? C122 C120 1.418(15) . ? C122 N22 1.424(13) . ? C10 C9 1.345(13) . ? C26 C24 1.368(15) . ? C26 C28 1.374(15) . ? C26 H26 0.9300 . ? C48 C50 1.339(14) . ? C48 H48 0.9300 . ? C86 C88 1.354(16) . ? C86 C87 1.363(15) . ? C86 C85 1.509(15) . ? C96 C95 1.333(14) . ? C96 C97 1.393(14) . ? C96 H96 0.9300 . ? C50 C52 1.373(15) . ? C50 H50 0.9300 . ? C52 C51 1.368(14) . ? C52 C53 1.444(15) . ? N19 C94 1.321(13) . ? C7 C8 1.403(13) . ? C7 H7 0.9300 . ? C40 H40 0.9300 . ? C85 C84 1.286(15) . ? C85 H85 0.9300 . ? C5 C4 1.397(15) . ? N15 C73 1.372(13) . ? N15 C77 1.386(15) . ? C59 C58 1.289(15) . ? C78 C80 1.359(14) . ? C109 C111 1.392(15) . ? C109 C101 1.488(14) . ? C67 C66 1.412(14) . ? C82 C83 1.389(14) . ? C82 C80 1.405(14) . ? C82 H82 0.9300 . ? C114 C112 1.365(14) . ? C114 C113 1.401(16) . ? C114 C115 1.471(15) . ? C51 C49 1.390(14) . ? C51 H51 0.9300 . ? C116 C115 1.275(15) . ? C116 H116 0.9300 . ? C8 C9 1.395(13) . ? C27 C25 1.375(15) . ? C27 H27 0.9300 . ? C36 N7 1.339(14) . ? C36 C35 1.453(16) . ? N22 C123 1.310(13) . ? N22 N23 1.385(12) . ? N11 C62 1.330(16) . ? C119 C121 1.436(16) . ? C119 H119 0.9300 . ? C74 C73 1.350(14) . ? C74 C75 1.368(17) . ? C74 H74 0.9300 . ? C53 C54 1.298(15) . ? C53 H53 0.9300 . ? C73 C72 1.541(14) . ? C83 C81 1.400(16) . ? C83 C84 1.475(15) . ? C63 C64 1.336(16) . ? C63 H63 0.9300 . ? N23 C124 1.300(15) . ? C55 C57 1.363(15) . ? C55 C56 1.407(16) . ? C55 C54 1.509(15) . ? C97 H97 0.9300 . ? C66 C65 1.352(13) . ? C66 H66 0.9300 . ? C104 C105 1.398(15) . ? C45 H45 0.9300 . ? C81 H81 0.9300 . ? C89 C87 1.434(16) . ? C89 H89 0.9300 . ? C58 C56 1.417(16) . ? C58 H58 0.9300 . ? C9 H9 0.9300 . ? C105 C106 1.375(17) . ? C105 H105 0.9300 . ? C101 C102 1.428(14) . ? C65 C64 1.394(15) . ? C65 H65 0.9300 . ? C49 H49 0.9300 . ? C115 H115 0.9300 . ? C34 C35 1.349(16) . ? C34 C33 1.35(2) . ? C34 H34 0.9300 . ? N7 C32 1.338(14) . ? N18 C93 1.324(15) . ? N18 C92 1.359(15) . ? C1 C2 1.359(16) . ? C1 H1 0.9300 . ? C90 C88 1.418(17) . ? C90 H90 0.9300 . ? C25 C24 1.332(15) . ? C25 H25 0.9300 . ? C121 H121 0.9300 . ? C19 C17 1.373(15) . ? C19 H19 0.9300 . ? C12 C13 1.378(15) . ? C12 H12 0.9300 . ? C113 C111 1.343(15) . ? C113 H113 0.9300 . ? C54 H54 0.9300 . ? C77 C76 1.318(17) . ? C77 H77 0.9300 . ? C94 C95 1.380(15) . ? C94 H94 0.9300 . ? C76 C75 1.375(17) . ? C76 H76 0.9300 . ? C17 H17 0.9300 . ? C80 H80 0.9300 . ? C84 H84 0.9300 . ? C4 C3 1.403(16) . ? C4 H4 0.9300 . ? C102 H102 0.9300 . ? C32 C33 1.39(2) . ? C32 H32 0.9300 . ? C15 C14 1.342(15) . ? C15 H15 0.9300 . ? N17 C93 1.300(15) . ? C118 C120 1.357(15) . ? C118 H118 0.9300 . ? C112 H112 0.9300 . ? C106 C107 1.389(18) . ? C106 H106 0.9300 . ? C57 H57 0.9300 . ? C18 C20 1.384(15) . ? C18 H18 0.9300 . ? C111 H111 0.9300 . ? C64 H64 0.9300 . ? C20 H20 0.9300 . ? C123 N24 1.365(15) . ? C123 H123 0.9300 . ? N24 C124 1.353(17) . ? C88 H88 0.9300 . ? C28 H28 0.9300 . ? C95 H95 0.9300 . ? C75 H75 0.9300 . ? C93 H93 0.9300 . ? C56 H56 0.9300 . ? C92 H92 0.9300 . ? C124 H124 0.9300 . ? C22 C23 1.250(15) . ? C22 H22 0.9300 . ? C87 H87 0.9300 . ? C23 C24 1.516(15) . ? C23 H23 0.9300 . ? C31 H31 0.9300 . ? C2 C3 1.378(18) . ? C2 H2 0.9300 . ? C14 C13 1.392(16) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C3 H3 0.9300 . ? C35 H35 0.9300 . ? C33 H33 0.9300 . ? N12 C62 1.331(17) . ? N12 C61 1.338(15) . ? C62 H62 0.9300 . ? C61 H61 0.9300 . ? C107 C108 1.348(17) . ? C107 H107 0.9300 . ? C108 H108 0.9300 . ? C120 H120 0.9300 . ? Cl1 C125 1.792(16) . ? Cl2 C125 1.777(16) . ? Cl3 C125 1.802(15) . ? C125 H125 0.9800 . ? Cl4 C126 2.044(19) . ? Cl5 C126 1.998(18) . ? Cl6 C126 2.03(2) . ? C126 H126 0.9800 . ? 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 C30 N6 C31 102.9(10) . . ? N6 C30 N4 109.6(11) . . ? N6 C30 H30 125.2 . . ? N4 C30 H30 125.2 . . ? N3 Cd1 N1 135.0(3) . . ? N3 Cd1 N2 67.9(3) . . ? N1 Cd1 N2 68.3(3) . . ? N3 Cd1 Br2 101.9(2) . . ? N1 Cd1 Br2 103.2(2) . . ? N2 Cd1 Br2 137.5(2) . . ? N3 Cd1 Br1 104.9(2) . . ? N1 Cd1 Br1 103.6(2) . . ? N2 Cd1 Br1 117.2(2) . . ? Br2 Cd1 Br1 105.26(7) . . ? N8 Cd2 N9 69.1(3) . . ? N8 Cd2 N7 68.0(3) . . ? N9 Cd2 N7 135.7(3) . . ? N8 Cd2 Br4 140.1(2) . . ? N9 Cd2 Br4 103.7(2) . . ? N7 Cd2 Br4 102.1(2) . . ? N8 Cd2 Br3 115.7(2) . . ? N9 Cd2 Br3 101.3(2) . . ? N7 Cd2 Br3 106.5(2) . . ? Br4 Cd2 Br3 104.25(8) . . ? N15 Cd3 N13 135.9(3) . . ? N15 Cd3 N14 69.2(3) . . ? N13 Cd3 N14 67.3(3) . . ? N15 Cd3 Br5 98.1(3) . . ? N13 Cd3 Br5 98.3(2) . . ? N14 Cd3 Br5 121.3(2) . . ? N15 Cd3 Br6 108.7(3) . . ? N13 Cd3 Br6 97.7(2) . . ? N14 Cd3 Br6 118.3(2) . . ? Br5 Cd3 Br6 119.95(8) . . ? N20 Cd4 N19 68.9(3) . . ? N20 Cd4 N21 69.3(3) . . ? N19 Cd4 N21 137.8(3) . . ? N20 Cd4 Br8 120.3(2) . . ? N19 Cd4 Br8 99.3(2) . . ? N21 Cd4 Br8 96.1(2) . . ? N20 Cd4 Br7 116.2(2) . . ? N19 Cd4 Br7 96.3(2) . . ? N21 Cd4 Br7 107.5(2) . . ? Br8 Cd4 Br7 123.26(8) . . ? C41 N8 C37 121.1(8) . . ? C41 N8 Cd2 118.2(7) . . ? C37 N8 Cd2 119.5(6) . . ? C99 N20 C103 119.9(9) . . ? C99 N20 Cd4 119.7(7) . . ? C103 N20 Cd4 120.3(7) . . ? C72 N14 C68 117.9(9) . . ? C72 N14 Cd3 120.2(7) . . ? C68 N14 Cd3 121.7(7) . . ? C10 N2 C6 118.9(8) . . ? C10 N2 Cd1 120.0(7) . . ? C6 N2 Cd1 120.7(6) . . ? N14 C68 C69 123.4(9) . . ? N14 C68 C67 114.6(10) . . ? C69 C68 C67 121.9(10) . . ? C30 N4 N5 109.3(9) . . ? C30 N4 C29 128.9(10) . . ? N5 N4 C29 121.8(9) . . ? C38 C37 N8 120.9(9) . . ? C38 C37 C36 124.1(11) . . ? N8 C37 C36 115.0(10) . . ? C42 N9 C46 117.4(9) . . ? C42 N9 Cd2 117.9(7) . . ? C46 N9 Cd2 124.6(7) . . ? C49 C47 C48 117.7(10) . . ? C49 C47 C39 121.0(10) . . ? C48 C47 C39 121.3(10) . . ? C1 N1 C5 120.3(10) . . ? C1 N1 Cd1 122.0(9) . . ? C5 N1 Cd1 117.6(7) . . ? N9 C42 C43 119.6(9) . . ? N9 C42 C41 116.6(9) . . ? C43 C42 C41 123.7(9) . . ? N8 C41 C40 119.8(10) . . ? N8 C41 C42 116.7(9) . . ? C40 C41 C42 123.5(9) . . ? C97 C98 N19 121.3(9) . . ? C97 C98 C99 123.9(10) . . ? N19 C98 C99 114.9(9) . . ? C89 C91 C90 120.5(12) . . ? C89 C91 N16 120.9(11) . . ? C90 C91 N16 118.6(12) . . ? C43 C44 C45 120.0(11) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C38 C39 C40 118.0(10) . . ? C38 C39 C47 120.5(10) . . ? C40 C39 C47 121.5(10) . . ? C63 N13 C67 117.9(10) . . ? C63 N13 Cd3 121.5(8) . . ? C67 N13 Cd3 120.6(7) . . ? C70 C69 C68 119.7(10) . . ? C70 C69 H69 120.2 . . ? C68 C69 H69 120.2 . . ? C31 N5 N4 102.3(10) . . ? C108 N21 C104 116.9(11) . . ? C108 N21 Cd4 124.5(9) . . ? C104 N21 Cd4 118.5(7) . . ? N3 C11 C12 121.8(10) . . ? N3 C11 C10 116.8(9) . . ? C12 C11 C10 121.3(10) . . ? N20 C103 C102 122.4(9) . . ? N20 C103 C104 116.4(10) . . ? C102 C103 C104 121.2(10) . . ? C61 N10 N11 110.4(10) . . ? C61 N10 C59 131.1(11) . . ? N11 N10 C59 118.5(10) . . ? C37 C38 C39 119.3(10) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C11 N3 C15 119.0(9) . . ? C11 N3 Cd1 120.0(7) . . ? C15 N3 Cd1 121.1(7) . . ? N2 C6 C7 121.1(10) . . ? N2 C6 C5 114.5(9) . . ? C7 C6 C5 124.4(11) . . ? C44 C43 C42 120.5(10) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C99 C100 C101 120.6(10) . . ? C99 C100 H100 119.7 . . ? C101 C100 H100 119.7 . . ? C72 C71 C70 120.6(10) . . ? C72 C71 H71 119.7 . . ? C70 C71 H71 119.7 . . ? C17 C16 C18 117.4(10) . . ? C17 C16 C8 122.6(10) . . ? C18 C16 C8 120.0(10) . . ? C92 N16 N17 108.0(10) . . ? C92 N16 C91 131.9(11) . . ? N17 N16 C91 120.0(10) . . ? C118 C117 C119 116.2(11) . . ? C118 C117 C116 122.2(11) . . ? C119 C117 C116 121.6(11) . . ? C112 C110 C109 119.5(11) . . ? C112 C110 H110 120.2 . . ? C109 C110 H110 120.2 . . ? C27 C29 C28 116.5(11) . . ? C27 C29 N4 122.4(11) . . ? C28 C29 N4 121.1(10) . . ? C45 C46 N9 125.7(10) . . ? C45 C46 H46 117.1 . . ? N9 C46 H46 117.1 . . ? C20 C21 C19 116.7(11) . . ? C20 C21 C22 120.7(11) . . ? C19 C21 C22 122.6(11) . . ? C57 C60 C59 120.0(12) . . ? C57 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C81 C79 C78 121.4(11) . . ? C81 C79 H79 119.3 . . ? C78 C79 H79 119.3 . . ? C69 C70 C71 115.4(10) . . ? C69 C70 C78 120.8(11) . . ? C71 C70 C78 123.7(10) . . ? C121 C122 C120 119.9(11) . . ? C121 C122 N22 117.8(11) . . ? C120 C122 N22 122.3(10) . . ? N2 C10 C9 122.6(10) . . ? N2 C10 C11 114.3(9) . . ? C9 C10 C11 123.1(9) . . ? C24 C26 C28 117.5(12) . . ? C24 C26 H26 121.3 . . ? C28 C26 H26 121.3 . . ? C50 C48 C47 121.4(12) . . ? C50 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C88 C86 C87 114.0(11) . . ? C88 C86 C85 122.3(11) . . ? C87 C86 C85 123.6(11) . . ? C95 C96 C97 119.7(11) . . ? C95 C96 H96 120.2 . . ? C97 C96 H96 120.2 . . ? C48 C50 C52 121.5(12) . . ? C48 C50 H50 119.2 . . ? C52 C50 H50 119.2 . . ? C51 C52 C50 118.6(10) . . ? C51 C52 C53 123.3(11) . . ? C50 C52 C53 118.2(11) . . ? C94 N19 C98 118.7(10) . . ? C94 N19 Cd4 122.1(8) . . ? C98 N19 Cd4 119.2(7) . . ? C6 C7 C8 121.0(10) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C41 C40 C39 120.9(9) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C84 C85 C86 127.6(12) . . ? C84 C85 H85 116.2 . . ? C86 C85 H85 116.2 . . ? N1 C5 C4 120.9(11) . . ? N1 C5 C6 117.8(10) . . ? C4 C5 C6 121.3(11) . . ? C73 N15 C77 116.9(11) . . ? C73 N15 Cd3 120.5(7) . . ? C77 N15 Cd3 122.6(9) . . ? C58 C59 N10 118.7(12) . . ? C58 C59 C60 122.8(12) . . ? N10 C59 C60 118.5(11) . . ? C80 C78 C79 115.5(10) . . ? C80 C78 C70 123.6(10) . . ? C79 C78 C70 120.8(10) . . ? C110 C109 C111 117.7(10) . . ? C110 C109 C101 120.0(10) . . ? C111 C109 C101 122.2(11) . . ? N13 C67 C66 123.5(9) . . ? N13 C67 C68 115.4(10) . . ? C66 C67 C68 121.1(10) . . ? C83 C82 C80 120.6(11) . . ? C83 C82 H82 119.7 . . ? C80 C82 H82 119.7 . . ? C112 C114 C113 117.8(11) . . ? C112 C114 C115 124.6(12) . . ? C113 C114 C115 117.6(11) . . ? C52 C51 C49 120.6(11) . . ? C52 C51 H51 119.7 . . ? C49 C51 H51 119.7 . . ? C115 C116 C117 129.0(12) . . ? C115 C116 H116 115.5 . . ? C117 C116 H116 115.5 . . ? C9 C8 C7 116.0(9) . . ? C9 C8 C16 122.1(9) . . ? C7 C8 C16 121.9(10) . . ? C29 C27 C25 121.0(12) . . ? C29 C27 H27 119.5 . . ? C25 C27 H27 119.5 . . ? N7 C36 C35 122.3(10) . . ? N7 C36 C37 116.2(11) . . ? C35 C36 C37 121.5(12) . . ? N20 C99 C100 121.8(10) . . ? N20 C99 C98 116.9(9) . . ? C100 C99 C98 121.2(9) . . ? C123 N22 N23 109.7(10) . . ? C123 N22 C122 130.3(11) . . ? N23 N22 C122 120.0(10) . . ? C62 N11 N10 100.4(10) . . ? C117 C119 C121 122.9(11) . . ? C117 C119 H119 118.5 . . ? C121 C119 H119 118.5 . . ? C73 C74 C75 117.9(12) . . ? C73 C74 H74 121.0 . . ? C75 C74 H74 121.0 . . ? C54 C53 C52 122.7(11) . . ? C54 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? C74 C73 N15 122.5(11) . . ? C74 C73 C72 123.5(11) . . ? N15 C73 C72 114.0(10) . . ? C82 C83 C81 115.1(10) . . ? C82 C83 C84 124.7(12) . . ? C81 C83 C84 120.2(10) . . ? N13 C63 C64 122.5(12) . . ? N13 C63 H63 118.8 . . ? C64 C63 H63 118.8 . . ? C124 N23 N22 101.8(11) . . ? C57 C55 C56 119.7(11) . . ? C57 C55 C54 116.7(11) . . ? C56 C55 C54 123.4(11) . . ? C98 C97 C96 119.3(11) . . ? C98 C97 H97 120.4 . . ? C96 C97 H97 120.4 . . ? C65 C66 C67 114.8(10) . . ? C65 C66 H66 122.6 . . ? C67 C66 H66 122.6 . . ? N21 C104 C105 122.3(11) . . ? N21 C104 C103 115.1(10) . . ? C105 C104 C103 122.5(11) . . ? N14 C72 C71 122.9(10) . . ? N14 C72 C73 115.5(10) . . ? C71 C72 C73 121.5(10) . . ? C46 C45 C44 116.7(11) . . ? C46 C45 H45 121.6 . . ? C44 C45 H45 121.6 . . ? C79 C81 C83 123.2(11) . . ? C79 C81 H81 118.4 . . ? C83 C81 H81 118.4 . . ? C91 C89 C87 120.1(12) . . ? C91 C89 H89 119.9 . . ? C87 C89 H89 119.9 . . ? C59 C58 C56 117.3(12) . . ? C59 C58 H58 121.3 . . ? C56 C58 H58 121.3 . . ? C10 C9 C8 120.3(10) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C106 C105 C104 117.3(13) . . ? C106 C105 H105 121.4 . . ? C104 C105 H105 121.4 . . ? C100 C101 C102 116.2(9) . . ? C100 C101 C109 122.6(10) . . ? C102 C101 C109 121.2(9) . . ? C66 C65 C64 121.6(11) . . ? C66 C65 H65 119.2 . . ? C64 C65 H65 119.2 . . ? C47 C49 C51 120.2(11) . . ? C47 C49 H49 119.9 . . ? C51 C49 H49 119.9 . . ? C116 C115 C114 128.3(12) . . ? C116 C115 H115 115.8 . . ? C114 C115 H115 115.8 . . ? C35 C34 C33 118.0(15) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? C32 N7 C36 117.1(12) . . ? C32 N7 Cd2 123.4(10) . . ? C36 N7 Cd2 119.4(7) . . ? C93 N18 C92 100.1(11) . . ? N1 C1 C2 121.5(12) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C91 C90 C88 117.3(13) . . ? C91 C90 H90 121.3 . . ? C88 C90 H90 121.3 . . ? C24 C25 C27 123.6(12) . . ? C24 C25 H25 118.2 . . ? C27 C25 H25 118.2 . . ? C122 C121 C119 116.9(11) . . ? C122 C121 H121 121.5 . . ? C119 C121 H121 121.5 . . ? C17 C19 C21 119.8(11) . . ? C17 C19 H19 120.1 . . ? C21 C19 H19 120.1 . . ? C11 C12 C13 119.3(11) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C111 C113 C114 120.2(12) . . ? C111 C113 H113 119.9 . . ? C114 C113 H113 119.9 . . ? C53 C54 C55 123.4(11) . . ? C53 C54 H54 118.3 . . ? C55 C54 H54 118.3 . . ? C76 C77 N15 122.2(14) . . ? C76 C77 H77 118.9 . . ? N15 C77 H77 118.9 . . ? N19 C94 C95 122.7(11) . . ? N19 C94 H94 118.7 . . ? C95 C94 H94 118.7 . . ? C77 C76 C75 119.2(14) . . ? C77 C76 H76 120.4 . . ? C75 C76 H76 120.4 . . ? C16 C17 C19 123.9(11) . . ? C16 C17 H17 118.1 . . ? C19 C17 H17 118.1 . . ? C78 C80 C82 124.2(10) . . ? C78 C80 H80 117.9 . . ? C82 C80 H80 117.9 . . ? C85 C84 C83 126.9(12) . . ? C85 C84 H84 116.5 . . ? C83 C84 H84 116.5 . . ? C5 C4 C3 116.7(12) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C103 C102 C101 119.0(10) . . ? C103 C102 H102 120.5 . . ? C101 C102 H102 120.5 . . ? N7 C32 C33 121.9(14) . . ? N7 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C14 C15 N3 121.4(11) . . ? C14 C15 H15 119.3 . . ? N3 C15 H15 119.3 . . ? C93 N17 N16 102.0(10) . . ? C117 C118 C120 122.4(12) . . ? C117 C118 H118 118.8 . . ? C120 C118 H118 118.8 . . ? C110 C112 C114 122.6(11) . . ? C110 C112 H112 118.7 . . ? C114 C112 H112 118.7 . . ? C105 C106 C107 120.0(14) . . ? C105 C106 H106 120.0 . . ? C107 C106 H106 120.0 . . ? C60 C57 C55 118.9(12) . . ? C60 C57 H57 120.6 . . ? C55 C57 H57 120.6 . . ? C20 C18 C16 119.7(11) . . ? C20 C18 H18 120.2 . . ? C16 C18 H18 120.2 . . ? C113 C111 C109 122.1(12) . . ? C113 C111 H111 118.9 . . ? C109 C111 H111 118.9 . . ? C63 C64 C65 119.6(11) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C21 C20 C18 122.5(11) . . ? C21 C20 H20 118.7 . . ? C18 C20 H20 118.7 . . ? N22 C123 N24 110.8(12) . . ? N22 C123 H123 124.6 . . ? N24 C123 H123 124.6 . . ? C124 N24 C123 100.7(11) . . ? C86 C88 C90 125.6(12) . . ? C86 C88 H88 117.2 . . ? C90 C88 H88 117.2 . . ? C26 C28 C29 123.4(11) . . ? C26 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C96 C95 C94 118.4(11) . . ? C96 C95 H95 120.8 . . ? C94 C95 H95 120.8 . . ? C74 C75 C76 121.2(13) . . ? C74 C75 H75 119.4 . . ? C76 C75 H75 119.4 . . ? N17 C93 N18 118.5(12) . . ? N17 C93 H93 120.8 . . ? N18 C93 H93 120.8 . . ? C55 C56 C58 121.2(11) . . ? C55 C56 H56 119.4 . . ? C58 C56 H56 119.4 . . ? N16 C92 N18 111.3(12) . . ? N16 C92 H92 124.3 . . ? N18 C92 H92 124.3 . . ? N23 C124 N24 117.0(13) . . ? N23 C124 H124 121.5 . . ? N24 C124 H124 121.5 . . ? C23 C22 C21 129.6(12) . . ? C23 C22 H22 115.2 . . ? C21 C22 H22 115.2 . . ? C86 C87 C89 122.3(12) . . ? C86 C87 H87 118.8 . . ? C89 C87 H87 118.8 . . ? C22 C23 C24 132.4(12) . . ? C22 C23 H23 113.8 . . ? C24 C23 H23 113.8 . . ? N5 C31 N6 115.8(13) . . ? N5 C31 H31 122.1 . . ? N6 C31 H31 122.1 . . ? C25 C24 C26 118.1(11) . . ? C25 C24 C23 124.2(11) . . ? C26 C24 C23 117.8(11) . . ? C1 C2 C3 120.1(12) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C15 C14 C13 120.6(12) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C12 C13 C14 117.8(11) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C2 C3 C4 120.5(13) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C34 C35 C36 118.5(13) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C34 C33 C32 122.0(14) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C62 N12 C61 104.7(13) . . ? N11 C62 N12 115.8(13) . . ? N11 C62 H62 122.1 . . ? N12 C62 H62 122.1 . . ? N10 C61 N12 108.6(13) . . ? N10 C61 H61 125.7 . . ? N12 C61 H61 125.7 . . ? C108 C107 C106 117.1(13) . . ? C108 C107 H107 121.4 . . ? C106 C107 H107 121.4 . . ? N21 C108 C107 126.4(13) . . ? N21 C108 H108 116.8 . . ? C107 C108 H108 116.8 . . ? C118 C120 C122 121.6(12) . . ? C118 C120 H120 119.2 . . ? C122 C120 H120 119.2 . . ? Cl2 C125 Cl1 104.8(9) . . ? Cl2 C125 Cl3 106.8(9) . . ? Cl1 C125 Cl3 112.4(8) . . ? Cl2 C125 H125 110.9 . . ? Cl1 C125 H125 110.9 . . ? Cl3 C125 H125 110.9 . . ? Cl5 C126 Cl6 90.3(10) . . ? Cl5 C126 Cl4 87.9(9) . . ? Cl6 C126 Cl4 90.7(9) . . ? Cl5 C126 H126 125.5 . . ? Cl6 C126 H126 125.5 . . ? Cl4 C126 H126 125.5 . . ? 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 C31 N6 C30 N4 0.5(15) . . . . ? N9 Cd2 N8 C41 11.0(7) . . . . ? N7 Cd2 N8 C41 179.9(8) . . . . ? Br4 Cd2 N8 C41 97.4(8) . . . . ? Br3 Cd2 N8 C41 -81.7(8) . . . . ? N9 Cd2 N8 C37 178.7(8) . . . . ? N7 Cd2 N8 C37 -12.4(7) . . . . ? Br4 Cd2 N8 C37 -94.9(7) . . . . ? Br3 Cd2 N8 C37 85.9(7) . . . . ? N19 Cd4 N20 C99 5.7(7) . . . . ? N21 Cd4 N20 C99 179.2(8) . . . . ? Br8 Cd4 N20 C99 94.3(7) . . . . ? Br7 Cd4 N20 C99 -80.9(8) . . . . ? N19 Cd4 N20 C103 -178.8(8) . . . . ? N21 Cd4 N20 C103 -5.2(7) . . . . ? Br8 Cd4 N20 C103 -90.2(7) . . . . ? Br7 Cd4 N20 C103 94.6(7) . . . . ? N15 Cd3 N14 C72 -7.0(8) . . . . ? N13 Cd3 N14 C72 -179.7(9) . . . . ? Br5 Cd3 N14 C72 -93.8(8) . . . . ? Br6 Cd3 N14 C72 93.7(8) . . . . ? N15 Cd3 N14 C68 179.2(9) . . . . ? N13 Cd3 N14 C68 6.5(8) . . . . ? Br5 Cd3 N14 C68 92.3(8) . . . . ? Br6 Cd3 N14 C68 -80.1(8) . . . . ? N3 Cd1 N2 C10 9.2(7) . . . . ? N1 Cd1 N2 C10 178.7(8) . . . . ? Br2 Cd1 N2 C10 92.7(8) . . . . ? Br1 Cd1 N2 C10 -86.8(8) . . . . ? N3 Cd1 N2 C6 -179.0(8) . . . . ? N1 Cd1 N2 C6 -9.5(7) . . . . ? Br2 Cd1 N2 C6 -95.5(8) . . . . ? Br1 Cd1 N2 C6 85.0(8) . . . . ? C72 N14 C68 C69 1.5(15) . . . . ? Cd3 N14 C68 C69 175.4(7) . . . . ? C72 N14 C68 C67 179.7(9) . . . . ? Cd3 N14 C68 C67 -6.3(12) . . . . ? N6 C30 N4 N5 1.3(14) . . . . ? N6 C30 N4 C29 179.2(11) . . . . ? C41 N8 C37 C38 2.4(16) . . . . ? Cd2 N8 C37 C38 -164.9(8) . . . . ? C41 N8 C37 C36 -177.6(9) . . . . ? Cd2 N8 C37 C36 15.1(11) . . . . ? N8 Cd2 N9 C42 -9.0(7) . . . . ? N7 Cd2 N9 C42 -23.8(9) . . . . ? Br4 Cd2 N9 C42 -147.8(7) . . . . ? Br3 Cd2 N9 C42 104.4(7) . . . . ? N8 Cd2 N9 C46 175.5(9) . . . . ? N7 Cd2 N9 C46 160.7(8) . . . . ? Br4 Cd2 N9 C46 36.7(9) . . . . ? Br3 Cd2 N9 C46 -71.1(8) . . . . ? N3 Cd1 N1 C1 -162.5(9) . . . . ? N2 Cd1 N1 C1 -176.3(10) . . . . ? Br2 Cd1 N1 C1 -40.1(10) . . . . ? Br1 Cd1 N1 C1 69.5(10) . . . . ? N3 Cd1 N1 C5 22.0(10) . . . . ? N2 Cd1 N1 C5 8.2(7) . . . . ? Br2 Cd1 N1 C5 144.4(7) . . . . ? Br1 Cd1 N1 C5 -106.0(8) . . . . ? C46 N9 C42 C43 -1.6(15) . . . . ? Cd2 N9 C42 C43 -177.4(8) . . . . ? C46 N9 C42 C41 -177.6(9) . . . . ? Cd2 N9 C42 C41 6.6(12) . . . . ? C37 N8 C41 C40 -1.7(15) . . . . ? Cd2 N8 C41 C40 165.8(8) . . . . ? C37 N8 C41 C42 -179.4(9) . . . . ? Cd2 N8 C41 C42 -11.9(12) . . . . ? N9 C42 C41 N8 3.5(14) . . . . ? C43 C42 C41 N8 -172.4(10) . . . . ? N9 C42 C41 C40 -174.1(10) . . . . ? C43 C42 C41 C40 10.0(17) . . . . ? C49 C47 C39 C38 174.5(11) . . . . ? C48 C47 C39 C38 -2.1(16) . . . . ? C49 C47 C39 C40 -7.5(16) . . . . ? C48 C47 C39 C40 175.9(10) . . . . ? N15 Cd3 N13 C63 166.4(8) . . . . ? N14 Cd3 N13 C63 176.2(10) . . . . ? Br5 Cd3 N13 C63 55.6(9) . . . . ? Br6 Cd3 N13 C63 -66.3(9) . . . . ? N15 Cd3 N13 C67 -15.5(10) . . . . ? N14 Cd3 N13 C67 -5.7(7) . . . . ? Br5 Cd3 N13 C67 -126.3(7) . . . . ? Br6 Cd3 N13 C67 111.8(7) . . . . ? N14 C68 C69 C70 -3.2(16) . . . . ? C67 C68 C69 C70 178.7(10) . . . . ? C30 N4 N5 C31 -2.5(13) . . . . ? C29 N4 N5 C31 179.4(11) . . . . ? N20 Cd4 N21 C108 -177.7(11) . . . . ? N19 Cd4 N21 C108 -168.7(9) . . . . ? Br8 Cd4 N21 C108 -57.6(10) . . . . ? Br7 Cd4 N21 C108 70.2(10) . . . . ? N20 Cd4 N21 C104 5.4(7) . . . . ? N19 Cd4 N21 C104 14.4(10) . . . . ? Br8 Cd4 N21 C104 125.6(8) . . . . ? Br7 Cd4 N21 C104 -106.7(8) . . . . ? C99 N20 C103 C102 -0.3(16) . . . . ? Cd4 N20 C103 C102 -175.9(8) . . . . ? C99 N20 C103 C104 -179.9(9) . . . . ? Cd4 N20 C103 C104 4.6(12) . . . . ? N8 C37 C38 C39 -2.0(16) . . . . ? C36 C37 C38 C39 178.0(10) . . . . ? C40 C39 C38 C37 1.0(15) . . . . ? C47 C39 C38 C37 179.1(10) . . . . ? C12 C11 N3 C15 2.9(17) . . . . ? C10 C11 N3 C15 -177.7(10) . . . . ? C12 C11 N3 Cd1 -177.6(9) . . . . ? C10 C11 N3 Cd1 1.9(12) . . . . ? N1 Cd1 N3 C11 -19.3(10) . . . . ? N2 Cd1 N3 C11 -5.4(7) . . . . ? Br2 Cd1 N3 C11 -142.1(8) . . . . ? Br1 Cd1 N3 C11 108.3(8) . . . . ? N1 Cd1 N3 C15 160.2(8) . . . . ? N2 Cd1 N3 C15 174.1(9) . . . . ? Br2 Cd1 N3 C15 37.4(9) . . . . ? Br1 Cd1 N3 C15 -72.2(9) . . . . ? C10 N2 C6 C7 3.3(16) . . . . ? Cd1 N2 C6 C7 -168.6(8) . . . . ? C10 N2 C6 C5 -178.8(9) . . . . ? Cd1 N2 C6 C5 9.3(12) . . . . ? C45 C44 C43 C42 -0.2(18) . . . . ? N9 C42 C43 C44 1.0(17) . . . . ? C41 C42 C43 C44 176.7(10) . . . . ? C89 C91 N16 C92 -175.5(14) . . . . ? C90 C91 N16 C92 8(2) . . . . ? C89 C91 N16 N17 2.7(18) . . . . ? C90 C91 N16 N17 -174.0(12) . . . . ? C30 N4 C29 C27 22.2(19) . . . . ? N5 N4 C29 C27 -160.2(12) . . . . ? C30 N4 C29 C28 -155.8(13) . . . . ? N5 N4 C29 C28 21.8(16) . . . . ? C42 N9 C46 C45 1.6(17) . . . . ? Cd2 N9 C46 C45 177.1(9) . . . . ? C68 C69 C70 C71 4.2(15) . . . . ? C68 C69 C70 C78 -176.3(9) . . . . ? C72 C71 C70 C69 -3.8(16) . . . . ? C72 C71 C70 C78 176.6(10) . . . . ? C6 N2 C10 C9 -4.0(16) . . . . ? Cd1 N2 C10 C9 167.9(8) . . . . ? C6 N2 C10 C11 176.6(9) . . . . ? Cd1 N2 C10 C11 -11.4(12) . . . . ? N3 C11 C10 N2 6.3(14) . . . . ? C12 C11 C10 N2 -174.3(11) . . . . ? N3 C11 C10 C9 -173.1(10) . . . . ? C12 C11 C10 C9 6.3(17) . . . . ? C49 C47 C48 C50 1.7(17) . . . . ? C39 C47 C48 C50 178.3(11) . . . . ? C47 C48 C50 C52 -1.0(19) . . . . ? C48 C50 C52 C51 0.4(19) . . . . ? C48 C50 C52 C53 -178.5(11) . . . . ? C97 C98 N19 C94 -0.1(16) . . . . ? C99 C98 N19 C94 -179.7(10) . . . . ? C97 C98 N19 Cd4 -177.2(8) . . . . ? C99 C98 N19 Cd4 3.1(12) . . . . ? N20 Cd4 N19 C94 178.4(10) . . . . ? N21 Cd4 N19 C94 169.4(8) . . . . ? Br8 Cd4 N19 C94 59.4(9) . . . . ? Br7 Cd4 N19 C94 -65.8(9) . . . . ? N20 Cd4 N19 C98 -4.5(7) . . . . ? N21 Cd4 N19 C98 -13.5(10) . . . . ? Br8 Cd4 N19 C98 -123.5(7) . . . . ? Br7 Cd4 N19 C98 111.2(8) . . . . ? N2 C6 C7 C8 -1.0(17) . . . . ? C5 C6 C7 C8 -178.8(10) . . . . ? N8 C41 C40 C39 0.7(16) . . . . ? C42 C41 C40 C39 178.2(9) . . . . ? C38 C39 C40 C41 -0.4(15) . . . . ? C47 C39 C40 C41 -178.5(10) . . . . ? C88 C86 C85 C84 -178.5(15) . . . . ? C87 C86 C85 C84 1(2) . . . . ? C1 N1 C5 C4 -0.5(17) . . . . ? Cd1 N1 C5 C4 175.1(8) . . . . ? C1 N1 C5 C6 177.4(11) . . . . ? Cd1 N1 C5 C6 -6.9(13) . . . . ? N2 C6 C5 N1 -1.4(14) . . . . ? C7 C6 C5 N1 176.5(10) . . . . ? N2 C6 C5 C4 176.5(10) . . . . ? C7 C6 C5 C4 -5.6(17) . . . . ? N13 Cd3 N15 C73 13.7(11) . . . . ? N14 Cd3 N15 C73 4.0(8) . . . . ? Br5 Cd3 N15 C73 124.6(9) . . . . ? Br6 Cd3 N15 C73 -109.9(9) . . . . ? N13 Cd3 N15 C77 -168.1(9) . . . . ? N14 Cd3 N15 C77 -177.8(11) . . . . ? Br5 Cd3 N15 C77 -57.2(10) . . . . ? Br6 Cd3 N15 C77 68.3(10) . . . . ? C61 N10 C59 C58 166.6(15) . . . . ? N11 N10 C59 C58 -13.1(18) . . . . ? C61 N10 C59 C60 -14(2) . . . . ? N11 N10 C59 C60 166.4(12) . . . . ? C57 C60 C59 C58 -3(2) . . . . ? C57 C60 C59 N10 177.8(13) . . . . ? C81 C79 C78 C80 1.0(17) . . . . ? C81 C79 C78 C70 179.4(11) . . . . ? C69 C70 C78 C80 6.7(17) . . . . ? C71 C70 C78 C80 -173.8(11) . . . . ? C69 C70 C78 C79 -171.5(10) . . . . ? C71 C70 C78 C79 8.0(17) . . . . ? C112 C110 C109 C111 1.5(18) . . . . ? C112 C110 C109 C101 -179.7(11) . . . . ? C63 N13 C67 C66 1.2(16) . . . . ? Cd3 N13 C67 C66 -176.9(8) . . . . ? C63 N13 C67 C68 -177.0(10) . . . . ? Cd3 N13 C67 C68 4.8(12) . . . . ? N14 C68 C67 N13 1.0(13) . . . . ? C69 C68 C67 N13 179.2(9) . . . . ? N14 C68 C67 C66 -177.3(10) . . . . ? C69 C68 C67 C66 0.9(15) . . . . ? C50 C52 C51 C49 -0.6(18) . . . . ? C53 C52 C51 C49 178.2(11) . . . . ? C118 C117 C116 C115 -174.9(14) . . . . ? C119 C117 C116 C115 9(2) . . . . ? C6 C7 C8 C9 -0.5(16) . . . . ? C6 C7 C8 C16 178.8(10) . . . . ? C17 C16 C8 C9 -7.9(18) . . . . ? C18 C16 C8 C9 171.0(11) . . . . ? C17 C16 C8 C7 172.8(12) . . . . ? C18 C16 C8 C7 -8.2(16) . . . . ? C28 C29 C27 C25 -1.1(19) . . . . ? N4 C29 C27 C25 -179.2(11) . . . . ? C38 C37 C36 N7 172.9(10) . . . . ? N8 C37 C36 N7 -7.1(14) . . . . ? C38 C37 C36 C35 -4.8(17) . . . . ? N8 C37 C36 C35 175.2(10) . . . . ? C103 N20 C99 C100 0.6(15) . . . . ? Cd4 N20 C99 C100 176.2(7) . . . . ? C103 N20 C99 C98 178.2(9) . . . . ? Cd4 N20 C99 C98 -6.2(12) . . . . ? C101 C100 C99 N20 -1.4(16) . . . . ? C101 C100 C99 C98 -178.9(9) . . . . ? C97 C98 C99 N20 -177.7(10) . . . . ? N19 C98 C99 N20 2.0(14) . . . . ? C97 C98 C99 C100 -0.1(16) . . . . ? N19 C98 C99 C100 179.5(10) . . . . ? C121 C122 N22 C123 168.6(13) . . . . ? C120 C122 N22 C123 -9.1(19) . . . . ? C121 C122 N22 N23 -10.4(16) . . . . ? C120 C122 N22 N23 171.9(11) . . . . ? C61 N10 N11 C62 -3.1(14) . . . . ? C59 N10 N11 C62 176.6(11) . . . . ? C118 C117 C119 C121 1(2) . . . . ? C116 C117 C119 C121 177.6(13) . . . . ? C51 C52 C53 C54 9(2) . . . . ? C50 C52 C53 C54 -172.2(13) . . . . ? C75 C74 C73 N15 -0.1(19) . . . . ? C75 C74 C73 C72 -178.6(12) . . . . ? C77 N15 C73 C74 1.6(18) . . . . ? Cd3 N15 C73 C74 179.9(9) . . . . ? C77 N15 C73 C72 -179.8(11) . . . . ? Cd3 N15 C73 C72 -1.4(13) . . . . ? C80 C82 C83 C81 -0.3(17) . . . . ? C80 C82 C83 C84 178.6(11) . . . . ? C67 N13 C63 C64 -1.8(18) . . . . ? Cd3 N13 C63 C64 176.3(10) . . . . ? C123 N22 N23 C124 -0.7(13) . . . . ? C122 N22 N23 C124 178.5(10) . . . . ? N19 C98 C97 C96 0.4(17) . . . . ? C99 C98 C97 C96 180.0(10) . . . . ? C95 C96 C97 C98 0.1(17) . . . . ? N13 C67 C66 C65 0.7(15) . . . . ? C68 C67 C66 C65 178.9(9) . . . . ? C108 N21 C104 C105 1.4(17) . . . . ? Cd4 N21 C104 C105 178.5(9) . . . . ? C108 N21 C104 C103 177.7(11) . . . . ? Cd4 N21 C104 C103 -5.1(12) . . . . ? N20 C103 C104 N21 0.5(14) . . . . ? C102 C103 C104 N21 -179.1(10) . . . . ? N20 C103 C104 C105 176.8(10) . . . . ? C102 C103 C104 C105 -2.7(16) . . . . ? C68 N14 C72 C71 -1.0(16) . . . . ? Cd3 N14 C72 C71 -175.1(8) . . . . ? C68 N14 C72 C73 -177.3(9) . . . . ? Cd3 N14 C72 C73 8.6(12) . . . . ? C70 C71 C72 N14 2.3(17) . . . . ? C70 C71 C72 C73 178.4(10) . . . . ? C74 C73 C72 N14 173.9(11) . . . . ? N15 C73 C72 N14 -4.7(15) . . . . ? C74 C73 C72 C71 -2.5(17) . . . . ? N15 C73 C72 C71 178.9(10) . . . . ? N9 C46 C45 C44 -0.9(18) . . . . ? C43 C44 C45 C46 0.1(18) . . . . ? C78 C79 C81 C83 -1(2) . . . . ? C82 C83 C81 C79 0.3(19) . . . . ? C84 C83 C81 C79 -178.6(11) . . . . ? C90 C91 C89 C87 -3(2) . . . . ? N16 C91 C89 C87 -179.7(12) . . . . ? N10 C59 C58 C56 -177.8(13) . . . . ? C60 C59 C58 C56 3(2) . . . . ? N2 C10 C9 C8 2.5(17) . . . . ? C11 C10 C9 C8 -178.2(10) . . . . ? C7 C8 C9 C10 -0.1(16) . . . . ? C16 C8 C9 C10 -179.5(10) . . . . ? N21 C104 C105 C106 -3.2(18) . . . . ? C103 C104 C105 C106 -179.3(11) . . . . ? C99 C100 C101 C102 1.8(15) . . . . ? C99 C100 C101 C109 -177.2(10) . . . . ? C110 C109 C101 C100 8.7(17) . . . . ? C111 C109 C101 C100 -172.5(11) . . . . ? C110 C109 C101 C102 -170.3(11) . . . . ? C111 C109 C101 C102 8.5(17) . . . . ? C67 C66 C65 C64 -2.2(16) . . . . ? C48 C47 C49 C51 -1.9(17) . . . . ? C39 C47 C49 C51 -178.5(10) . . . . ? C52 C51 C49 C47 1.4(18) . . . . ? C117 C116 C115 C114 -177.9(12) . . . . ? C112 C114 C115 C116 0(2) . . . . ? C113 C114 C115 C116 179.6(14) . . . . ? C35 C36 N7 C32 -2.9(17) . . . . ? C37 C36 N7 C32 179.4(10) . . . . ? C35 C36 N7 Cd2 173.8(8) . . . . ? C37 C36 N7 Cd2 -4.0(13) . . . . ? N8 Cd2 N7 C32 -175.2(11) . . . . ? N9 Cd2 N7 C32 -160.3(9) . . . . ? Br4 Cd2 N7 C32 -35.8(10) . . . . ? Br3 Cd2 N7 C32 73.2(10) . . . . ? N8 Cd2 N7 C36 8.4(8) . . . . ? N9 Cd2 N7 C36 23.3(10) . . . . ? Br4 Cd2 N7 C36 147.7(8) . . . . ? Br3 Cd2 N7 C36 -103.2(8) . . . . ? C5 N1 C1 C2 3.5(19) . . . . ? Cd1 N1 C1 C2 -172.0(10) . . . . ? C89 C91 C90 C88 2(2) . . . . ? N16 C91 C90 C88 179.0(12) . . . . ? C29 C27 C25 C24 1(2) . . . . ? C120 C122 C121 C119 0.0(19) . . . . ? N22 C122 C121 C119 -177.7(11) . . . . ? C117 C119 C121 C122 -1(2) . . . . ? C20 C21 C19 C17 -1(2) . . . . ? C22 C21 C19 C17 178.5(13) . . . . ? N3 C11 C12 C13 -3.8(19) . . . . ? C10 C11 C12 C13 176.8(11) . . . . ? C112 C114 C113 C111 3(2) . . . . ? C115 C114 C113 C111 -177.4(12) . . . . ? C52 C53 C54 C55 179.6(11) . . . . ? C57 C55 C54 C53 -171.9(14) . . . . ? C56 C55 C54 C53 12(2) . . . . ? C73 N15 C77 C76 -3(2) . . . . ? Cd3 N15 C77 C76 178.4(11) . . . . ? C98 N19 C94 C95 -0.7(18) . . . . ? Cd4 N19 C94 C95 176.3(10) . . . . ? N15 C77 C76 C75 3(2) . . . . ? C18 C16 C17 C19 0(2) . . . . ? C8 C16 C17 C19 178.7(12) . . . . ? C21 C19 C17 C16 1(2) . . . . ? C79 C78 C80 C82 -1.0(17) . . . . ? C70 C78 C80 C82 -179.4(10) . . . . ? C83 C82 C80 C78 0.7(18) . . . . ? C86 C85 C84 C83 -176.2(11) . . . . ? C82 C83 C84 C85 -11(2) . . . . ? C81 C83 C84 C85 168.0(14) . . . . ? N1 C5 C4 C3 -2.2(17) . . . . ? C6 C5 C4 C3 179.9(11) . . . . ? N20 C103 C102 C101 0.8(16) . . . . ? C104 C103 C102 C101 -179.6(10) . . . . ? C100 C101 C102 C103 -1.5(16) . . . . ? C109 C101 C102 C103 177.5(10) . . . . ? C36 N7 C32 C33 2(2) . . . . ? Cd2 N7 C32 C33 -174.0(11) . . . . ? C11 N3 C15 C14 -0.5(18) . . . . ? Cd1 N3 C15 C14 179.9(10) . . . . ? C92 N16 N17 C93 -0.7(14) . . . . ? C91 N16 N17 C93 -179.2(11) . . . . ? C119 C117 C118 C120 -1(2) . . . . ? C116 C117 C118 C120 -177.1(12) . . . . ? C109 C110 C112 C114 -1(2) . . . . ? C113 C114 C112 C110 -0.9(19) . . . . ? C115 C114 C112 C110 179.1(12) . . . . ? C104 C105 C106 C107 3(2) . . . . ? C59 C60 C57 C55 1(2) . . . . ? C56 C55 C57 C60 0(2) . . . . ? C54 C55 C57 C60 -175.5(13) . . . . ? C17 C16 C18 C20 0.5(19) . . . . ? C8 C16 C18 C20 -178.6(11) . . . . ? C114 C113 C111 C109 -2(2) . . . . ? C110 C109 C111 C113 0(2) . . . . ? C101 C109 C111 C113 -178.6(12) . . . . ? N13 C63 C64 C65 0(2) . . . . ? C66 C65 C64 C63 1.7(19) . . . . ? C19 C21 C20 C18 1(2) . . . . ? C22 C21 C20 C18 -178.3(13) . . . . ? C16 C18 C20 C21 -1(2) . . . . ? N23 N22 C123 N24 0.4(15) . . . . ? C122 N22 C123 N24 -178.6(11) . . . . ? N22 C123 N24 C124 0.1(15) . . . . ? C87 C86 C88 C90 3(2) . . . . ? C85 C86 C88 C90 -178.0(13) . . . . ? C91 C90 C88 C86 -2(2) . . . . ? C24 C26 C28 C29 -1(2) . . . . ? C27 C29 C28 C26 1(2) . . . . ? N4 C29 C28 C26 179.3(12) . . . . ? C97 C96 C95 C94 -0.9(18) . . . . ? N19 C94 C95 C96 1(2) . . . . ? C73 C74 C75 C76 0(2) . . . . ? C77 C76 C75 C74 -2(2) . . . . ? N16 N17 C93 N18 1.2(19) . . . . ? C92 N18 C93 N17 -1.2(19) . . . . ? C57 C55 C56 C58 0(2) . . . . ? C54 C55 C56 C58 175.3(13) . . . . ? C59 C58 C56 C55 -1(2) . . . . ? N17 N16 C92 N18 0.0(15) . . . . ? C91 N16 C92 N18 178.3(12) . . . . ? C93 N18 C92 N16 0.7(16) . . . . ? N22 N23 C124 N24 0.8(16) . . . . ? C123 N24 C124 N23 -0.6(17) . . . . ? C20 C21 C22 C23 171.2(15) . . . . ? C19 C21 C22 C23 -8(2) . . . . ? C88 C86 C87 C89 -4(2) . . . . ? C85 C86 C87 C89 177.4(13) . . . . ? C91 C89 C87 C86 4(2) . . . . ? C21 C22 C23 C24 -177.9(12) . . . . ? N4 N5 C31 N6 3.0(16) . . . . ? C30 N6 C31 N5 -2.3(17) . . . . ? C27 C25 C24 C26 0(2) . . . . ? C27 C25 C24 C23 -179.4(12) . . . . ? C28 C26 C24 C25 0(2) . . . . ? C28 C26 C24 C23 179.4(12) . . . . ? C22 C23 C24 C25 172.9(16) . . . . ? C22 C23 C24 C26 -6(2) . . . . ? N1 C1 C2 C3 -4(2) . . . . ? N3 C15 C14 C13 -1(2) . . . . ? C11 C12 C13 C14 2(2) . . . . ? C15 C14 C13 C12 0(2) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C5 C4 C3 C2 2(2) . . . . ? C33 C34 C35 C36 -4(2) . . . . ? N7 C36 C35 C34 3.8(18) . . . . ? C37 C36 C35 C34 -178.6(11) . . . . ? C35 C34 C33 C32 4(2) . . . . ? N7 C32 C33 C34 -3(3) . . . . ? N10 N11 C62 N12 1.8(16) . . . . ? C61 N12 C62 N11 0.1(18) . . . . ? N11 N10 C61 N12 3.4(15) . . . . ? C59 N10 C61 N12 -176.3(13) . . . . ? C62 N12 C61 N10 -2.1(16) . . . . ? C105 C106 C107 C108 -1(2) . . . . ? C104 N21 C108 C107 1(2) . . . . ? Cd4 N21 C108 C107 -176.3(12) . . . . ? C106 C107 C108 N21 -1(2) . . . . ? C117 C118 C120 C122 0(2) . . . . ? C121 C122 C120 C118 0(2) . . . . ? N22 C122 C120 C118 178.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.259 _refine_diff_density_min -2.225 _refine_diff_density_rms 0.115 data_zhou0009_0m _database_code_depnum_ccdc_archive 'CCDC 837605' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H102 Cl4 N24 O23 Zn2' _chemical_formula_sum 'C124 H102 Cl4 N24 O23 Zn2' _chemical_formula_weight 2568.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 18.095(5) _cell_length_b 18.724(5) _cell_length_c 20.836(5) _cell_angle_alpha 109.899(5) _cell_angle_beta 102.332(5) _cell_angle_gamma 107.921(5) _cell_volume 5903(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80164 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.05 _reflns_number_total 20885 _reflns_number_gt 12404 _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 '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_number_reflns 20885 _refine_ls_number_parameters 1595 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1392 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2480 _refine_ls_wR_factor_gt 0.2185 _refine_ls_goodness_of_fit_ref 1.458 _refine_ls_restrained_S_all 1.472 _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 C122 C 1.6619(4) 1.1719(5) 0.6425(4) 0.0696(17) Uani 1 1 d . . . C117 C 1.4978(4) 1.1306(7) 0.5679(4) 0.097(3) Uani 1 1 d . . . C62 C 1.8859(4) 0.8756(5) 0.7257(4) 0.080(2) Uani 1 1 d . . . H62 H 1.9352 0.8686 0.7330 0.097 Uiso 1 1 calc R . . N12 N 1.8857(3) 0.9528(3) 0.7550(3) 0.0760(16) Uani 1 1 d . . . N11 N 1.8147(3) 0.8126(3) 0.6874(3) 0.0762(16) Uani 1 1 d . . . C61 C 1.8060(4) 0.9327(4) 0.7309(4) 0.0735(18) Uani 1 1 d . . . H61 H 1.7826 0.9712 0.7409 0.088 Uiso 1 1 calc R . . N10 N 1.7616(3) 0.8508(3) 0.6902(3) 0.0644(13) Uani 1 1 d . . . C59 C 1.6267(4) 0.8479(6) 0.6420(4) 0.094(2) Uani 1 1 d . . . H59 H 1.6499 0.9056 0.6594 0.113 Uiso 1 1 calc R . . C60 C 1.6738(3) 0.8034(5) 0.6529(3) 0.0737(19) Uani 1 1 d . . . C58 C 1.6389(4) 0.7180(5) 0.6283(4) 0.089(2) Uani 1 1 d . . . H58 H 1.6727 0.6909 0.6365 0.106 Uiso 1 1 calc R . . C57 C 1.5372(4) 0.7959(6) 0.6007(4) 0.099(2) Uani 1 1 d U . . H57 H 1.5016 0.8203 0.5900 0.119 Uiso 1 1 calc R . . C56 C 1.5550(5) 0.6725(6) 0.5918(4) 0.106(3) Uani 1 1 d . . . H56 H 1.5326 0.6152 0.5771 0.128 Uiso 1 1 calc R . . C55 C 1.5058(5) 0.7082(7) 0.5772(5) 0.103(3) Uani 1 1 d U . . Zn1 Zn 0.70338(3) 0.39764(3) 0.27816(3) 0.04228(19) Uani 1 1 d . . . Zn2 Zn 0.71113(3) 0.88497(4) 0.26461(4) 0.0465(2) Uani 1 1 d . . . Cl2 Cl 0.33259(10) 0.95667(9) 0.16378(10) 0.0671(5) Uani 1 1 d . . . Cl1 Cl 0.93963(10) 0.73539(12) 0.35932(13) 0.0860(6) Uani 1 1 d . . . C83 C 0.1431(3) 0.6405(3) 0.1042(4) 0.0594(16) Uani 1 1 d . . . N3 N 0.6683(2) 0.4704(2) 0.2239(2) 0.0430(10) Uani 1 1 d . . . C33 C 0.7209(4) 0.2220(4) 0.0804(4) 0.0706(18) Uani 1 1 d . . . H33 H 0.6842 0.1775 0.0359 0.085 Uiso 1 1 calc R . . N9 N 0.7311(2) 0.4945(3) 0.3850(2) 0.0477(11) Uani 1 1 d . . . N1 N 0.6710(2) 0.2897(3) 0.3022(2) 0.0474(11) Uani 1 1 d . . . N2 N 0.5752(2) 0.3408(2) 0.2346(2) 0.0394(10) Uani 1 1 d . . . N20 N 0.8390(2) 0.9382(2) 0.3063(2) 0.0458(11) Uani 1 1 d . . . N15 N 0.6723(2) 0.9503(2) 0.2040(2) 0.0457(11) Uani 1 1 d . . . N8 N 0.8316(2) 0.4523(2) 0.3225(2) 0.0407(10) Uani 1 1 d . . . N7 N 0.7432(2) 0.3271(2) 0.1944(2) 0.0458(10) Uani 1 1 d . . . N21 N 0.7436(2) 0.9915(2) 0.3682(2) 0.0468(11) Uani 1 1 d . . . N16 N -0.3485(3) 0.4208(3) 0.0040(3) 0.0545(12) Uani 1 1 d . . . N4 N -0.3547(3) -0.0941(3) -0.0074(3) 0.0527(12) Uani 1 1 d . . . N19 N 0.7460(3) 0.8090(2) 0.1812(3) 0.0496(11) Uani 1 1 d . . . N13 N 0.6824(3) 0.7879(2) 0.3032(2) 0.0483(11) Uani 1 1 d . . . N14 N 0.5826(2) 0.8284(2) 0.2270(2) 0.0438(10) Uani 1 1 d . . . C38 C 0.9604(3) 0.4523(3) 0.3166(3) 0.0492(14) Uani 1 1 d . . . H38 H 0.9900 0.4301 0.2904 0.059 Uiso 1 1 calc R . . O7 O 0.3413(3) 0.9126(3) 0.0974(3) 0.0947(15) Uani 1 1 d . . . N17 N -0.3907(3) 0.3647(3) 0.0251(3) 0.0685(14) Uani 1 1 d . . . N18 N -0.4795(3) 0.3877(3) -0.0503(3) 0.0746(15) Uani 1 1 d . . . C8 C 0.4492(3) 0.2391(3) 0.2211(3) 0.0449(13) Uani 1 1 d . . . H8 H 0.4224 0.1940 0.2296 0.054 Uiso 1 1 calc R . . C42 C 0.8125(3) 0.5431(3) 0.4237(3) 0.0457(13) Uani 1 1 d . . . C24 C -0.0938(3) 0.0195(4) 0.0654(3) 0.0562(15) Uani 1 1 d . . . C10 C 0.4471(3) 0.3399(3) 0.1754(3) 0.0475(13) Uani 1 1 d . . . H10 H 0.4187 0.3625 0.1513 0.057 Uiso 1 1 calc R . . C5 C 0.5596(3) 0.1644(3) 0.2779(3) 0.0555(15) Uani 1 1 d . . . H5 H 0.5028 0.1316 0.2604 0.067 Uiso 1 1 calc R . . C4 C 0.6984(4) 0.1863(4) 0.3312(4) 0.0667(17) Uani 1 1 d . . . H4 H 0.7370 0.1685 0.3498 0.080 Uiso 1 1 calc R . . C16 C 0.3108(3) 0.2342(3) 0.1615(3) 0.0537(15) Uani 1 1 d . . . C12 C 0.5856(3) 0.4459(3) 0.1935(3) 0.0414(12) Uani 1 1 d . . . C78 C 0.3186(3) 0.7132(3) 0.1503(3) 0.0507(14) Uani 1 1 d . . . C70 C 0.4106(3) 0.7528(3) 0.1763(3) 0.0468(13) Uani 1 1 d . . . C72 C 0.5379(3) 0.8538(3) 0.1871(3) 0.0425(12) Uani 1 1 d . . . C85 C 0.0048(4) 0.5663(4) 0.1043(4) 0.0721(18) Uani 1 1 d . . . H85 H 0.0314 0.5590 0.1434 0.086 Uiso 1 1 calc R . . C100 C 0.9648(3) 1.0349(3) 0.4039(3) 0.0547(14) Uani 1 1 d . . . H100 H 0.9920 1.0804 0.4497 0.066 Uiso 1 1 calc R . . C37 C 0.8758(3) 0.4211(3) 0.2868(3) 0.0438(13) Uani 1 1 d . . . C91 C -0.2597(3) 0.4578(3) 0.0292(3) 0.0521(14) Uani 1 1 d . . . C41 C 0.8697(3) 0.5143(3) 0.3897(3) 0.0438(12) Uani 1 1 d . . . C47 C 1.0934(3) 0.5547(3) 0.4208(3) 0.0533(14) Uani 1 1 d . . . C40 C 0.9546(3) 0.5487(3) 0.4230(3) 0.0506(14) Uani 1 1 d . . . H40 H 0.9802 0.5925 0.4697 0.061 Uiso 1 1 calc R . . N6 N -0.4863(3) -0.1243(3) -0.0571(3) 0.0731(15) Uani 1 1 d . . . C69 C 0.4588(3) 0.7280(3) 0.2177(3) 0.0532(14) Uani 1 1 d . . . H69 H 0.4332 0.6848 0.2289 0.064 Uiso 1 1 calc R . . C39 C 1.0019(3) 0.5179(3) 0.3869(3) 0.0479(13) Uani 1 1 d . . . C112 C 1.2337(5) 1.1438(6) 0.4728(4) 0.105(3) Uani 1 1 d . . . H112 H 1.2653 1.2011 0.4983 0.126 Uiso 1 1 calc R . . C20 C 0.1817(3) 0.1184(4) 0.1281(3) 0.0604(16) Uani 1 1 d . . . H20 H 0.1547 0.0644 0.1223 0.072 Uiso 1 1 calc R . . C104 C 0.8264(3) 0.8295(3) 0.1977(3) 0.0500(14) Uani 1 1 d . . . C6 C 0.5891(3) 0.2415(3) 0.2765(3) 0.0460(13) Uani 1 1 d . . . N5 N -0.3959(3) -0.1595(3) 0.0053(3) 0.0664(14) Uani 1 1 d . . . C71 C 0.4526(3) 0.8172(3) 0.1609(3) 0.0484(13) Uani 1 1 d . . . H71 H 0.4229 0.8354 0.1327 0.058 Uiso 1 1 calc R . . C74 C 0.5557(3) 0.9647(4) 0.1392(3) 0.0566(15) Uani 1 1 d . . . H74 H 0.4985 0.9464 0.1190 0.068 Uiso 1 1 calc R . . C86 C -0.0861(3) 0.5314(4) 0.0794(4) 0.0637(16) Uani 1 1 d . . . C124 C 1.8754(5) 1.2420(6) 0.7192(5) 0.111(3) Uani 1 1 d . . . H124 H 1.9302 1.2724 0.7260 0.133 Uiso 1 1 calc R . . C11 C 0.5325(3) 0.3732(3) 0.2003(3) 0.0402(12) Uani 1 1 d . . . C9 C 0.4025(3) 0.2713(3) 0.1863(3) 0.0470(13) Uani 1 1 d . . . C102 C 0.9667(3) 0.9323(3) 0.3003(3) 0.0530(14) Uani 1 1 d . . . H102 H 0.9948 0.9067 0.2748 0.064 Uiso 1 1 calc R . . C36 C 0.8239(3) 0.3511(3) 0.2119(3) 0.0451(13) Uani 1 1 d . . . C107 C 0.7197(4) 0.7007(4) 0.0677(4) 0.0726(19) Uani 1 1 d . . . H107 H 0.6818 0.6571 0.0232 0.087 Uiso 1 1 calc R . . C54 C 1.4134(4) 0.6519(6) 0.5348(5) 0.114(3) Uani 1 1 d DU . . H54 H 1.3981 0.5948 0.5180 0.137 Uiso 1 1 calc R . . C23 C -0.0028(3) 0.0559(4) 0.0885(3) 0.0637(16) Uani 1 1 d . . . H23 H 0.0237 0.0262 0.1041 0.076 Uiso 1 1 calc R . . C7 C 0.5347(3) 0.2736(3) 0.2430(3) 0.0393(12) Uani 1 1 d . . . C68 C 0.5446(3) 0.7668(3) 0.2426(3) 0.0450(13) Uani 1 1 d . . . C29 C -0.2666(3) -0.0557(3) 0.0181(3) 0.0497(14) Uani 1 1 d . . . C32 C 0.6920(3) 0.2629(3) 0.1298(3) 0.0571(15) Uani 1 1 d . . . H32 H 0.6350 0.2456 0.1184 0.069 Uiso 1 1 calc R . . C88 C -0.1343(4) 0.5383(4) 0.0211(4) 0.0711(18) Uani 1 1 d . . . H88 H -0.1078 0.5682 -0.0011 0.085 Uiso 1 1 calc R . . C13 C 0.5551(3) 0.4873(3) 0.1588(3) 0.0579(15) Uani 1 1 d . . . H13 H 0.4980 0.4703 0.1389 0.069 Uiso 1 1 calc R . . C109 C 1.1008(3) 1.0313(4) 0.4029(3) 0.0587(15) Uani 1 1 d . . . C077 C 0.7201(3) 0.5350(3) 0.2197(3) 0.0548(14) Uani 1 1 d . . . H077 H 0.7769 0.5523 0.2416 0.066 Uiso 1 1 calc R . . C82 C 0.1851(3) 0.6853(4) 0.0718(4) 0.0700(18) Uani 1 1 d . . . H82 H 0.1545 0.6916 0.0337 0.084 Uiso 1 1 calc R . . C25 C -0.1422(3) 0.0548(4) 0.0394(4) 0.075(2) Uani 1 1 d . . . H25 H -0.1164 0.1054 0.0382 0.090 Uiso 1 1 calc R . . C77 C 0.7224(3) 1.0147(3) 0.1979(3) 0.0569(15) Uani 1 1 d . . . H77 H 0.7795 1.0325 0.2182 0.068 Uiso 1 1 calc R . . C94 C 0.6907(4) 1.0176(4) 0.3945(3) 0.0572(15) Uani 1 1 d . . . H94 H 0.6339 0.9860 0.3693 0.069 Uiso 1 1 calc R . . C73 C 0.5893(3) 0.9251(3) 0.1755(3) 0.0454(13) Uani 1 1 d . . . C98 C 0.8253(3) 1.0371(3) 0.4052(3) 0.0465(13) Uani 1 1 d . . . C103 C 0.8816(3) 0.9028(3) 0.2702(3) 0.0470(13) Uani 1 1 d . . . C35 C 0.8573(4) 0.3133(4) 0.1638(3) 0.0660(17) Uani 1 1 d . . . H35 H 0.9146 0.3318 0.1761 0.079 Uiso 1 1 calc R . . O8 O 0.3608(4) 1.0404(3) 0.1789(3) 0.131(2) Uani 1 1 d . . . C67 C 0.6013(3) 0.7435(3) 0.2860(3) 0.0503(14) Uani 1 1 d . . . C101 C 1.0106(3) 0.9997(3) 0.3681(3) 0.0525(14) Uani 1 1 d . . . C84 C 0.0519(3) 0.6055(3) 0.0787(4) 0.0669(17) Uani 1 1 d . . . H84 H 0.0255 0.6127 0.0394 0.080 Uiso 1 1 calc R . . C50 C 1.2251(3) 0.5439(4) 0.4442(4) 0.0682(18) Uani 1 1 d . . . H50 H 1.2540 0.5102 0.4378 0.082 Uiso 1 1 calc R . . C99 C 0.8801(3) 1.0032(3) 0.3723(3) 0.0464(13) Uani 1 1 d . . . C21 C 0.1357(3) 0.1607(4) 0.1137(4) 0.0662(17) Uani 1 1 d U . . C108 C 0.6927(4) 0.7442(3) 0.1177(3) 0.0586(16) Uani 1 1 d . . . H108 H 0.6359 0.7285 0.1072 0.070 Uiso 1 1 calc R . . O6 O 0.3805(4) 0.9471(4) 0.2210(3) 0.119(2) Uani 1 1 d . . . C48 C 1.1389(3) 0.5074(4) 0.4136(4) 0.0656(17) Uani 1 1 d . . . H48 H 1.1112 0.4496 0.3876 0.079 Uiso 1 1 calc R . . C90 C -0.2197(3) 0.5021(4) -0.0038(4) 0.0661(17) Uani 1 1 d . . . H90 H -0.2504 0.5073 -0.0425 0.079 Uiso 1 1 calc R . . O11 O 0.1028(7) 0.7758(7) 0.7280(6) 0.241(5) Uani 1 1 d . . . C63 C 0.7369(4) 0.7680(4) 0.3402(3) 0.0607(16) Uani 1 1 d . . . H63 H 0.7933 0.7991 0.3532 0.073 Uiso 1 1 calc R . . N22 N 1.7459(3) 1.1907(4) 0.6821(3) 0.0789(16) Uani 1 1 d . . . C95 C 0.7166(4) 1.0882(4) 0.4564(4) 0.0630(16) Uani 1 1 d . . . H95 H 0.6784 1.1052 0.4730 0.076 Uiso 1 1 calc R . . C106 C 0.8017(4) 0.7216(4) 0.0838(4) 0.081(2) Uani 1 1 d . . . H106 H 0.8208 0.6918 0.0507 0.098 Uiso 1 1 calc R . . C76 C 0.6929(4) 1.0559(3) 0.1629(3) 0.0606(16) Uani 1 1 d . . . H76 H 0.7294 1.1002 0.1588 0.073 Uiso 1 1 calc R . . C79 C 0.2774(3) 0.6658(4) 0.1819(4) 0.0657(17) Uani 1 1 d . . . H79 H 0.3085 0.6579 0.2185 0.079 Uiso 1 1 calc R . . C3 C 0.7247(4) 0.2621(4) 0.3291(4) 0.0612(16) Uani 1 1 d . . . H3 H 0.7813 0.2954 0.3468 0.073 Uiso 1 1 calc R . . C97 C 0.8553(4) 1.1081(3) 0.4682(3) 0.0607(16) Uani 1 1 d . . . H97 H 0.9123 1.1385 0.4929 0.073 Uiso 1 1 calc R . . C75 C 0.6081(4) 1.0303(4) 0.1337(4) 0.0657(17) Uani 1 1 d . . . H75 H 0.5868 1.0580 0.1105 0.079 Uiso 1 1 calc R . . C30 C -0.4110(3) -0.0758(4) -0.0444(4) 0.0670(17) Uani 1 1 d . . . H30 H -0.3973 -0.0332 -0.0590 0.080 Uiso 1 1 calc R . . C45 C 0.6989(4) 0.5839(4) 0.4763(4) 0.0646(16) Uani 1 1 d . . . H45 H 0.6591 0.5962 0.4940 0.078 Uiso 1 1 calc R . . C15 C 0.6928(4) 0.5779(4) 0.1840(4) 0.0670(17) Uani 1 1 d . . . H15 H 0.7305 0.6220 0.1807 0.080 Uiso 1 1 calc R . . C43 C 0.8401(4) 0.6133(3) 0.4886(3) 0.0574(15) Uani 1 1 d . . . H43 H 0.8966 0.6458 0.5142 0.069 Uiso 1 1 calc R . . C18 C 0.2670(3) 0.1538(3) 0.1509(3) 0.0587(16) Uani 1 1 d . . . H18 H 0.2960 0.1227 0.1594 0.070 Uiso 1 1 calc R . . C92 C -0.4031(4) 0.4325(4) -0.0416(4) 0.0670(17) Uani 1 1 d . . . H92 H -0.3888 0.4675 -0.0639 0.080 Uiso 1 1 calc R . . C44 C 0.7823(4) 0.6342(4) 0.5146(3) 0.0664(17) Uani 1 1 d . . . H44 H 0.7994 0.6819 0.5577 0.080 Uiso 1 1 calc R . . C26 C -0.1340(4) -0.0542(5) 0.0685(4) 0.083(2) Uani 1 1 d . . . H26 H -0.1032 -0.0789 0.0871 0.099 Uiso 1 1 calc R . . C46 C 0.6759(3) 0.5167(4) 0.4129(3) 0.0551(15) Uani 1 1 d . . . H46 H 0.6195 0.4838 0.3869 0.066 Uiso 1 1 calc R . . C31 C -0.4742(3) -0.1729(4) -0.0263(4) 0.075(2) Uani 1 1 d . . . H31 H -0.5186 -0.2147 -0.0266 0.090 Uiso 1 1 calc R . . N23 N 1.8122(4) 1.2435(4) 0.6747(4) 0.101(2) Uani 1 1 d . . . C66 C 0.5737(4) 0.6790(4) 0.3050(4) 0.0666(17) Uani 1 1 d . . . H66 H 0.5172 0.6488 0.2927 0.080 Uiso 1 1 calc R . . C14 C 0.6085(4) 0.5532(4) 0.1535(4) 0.0643(17) Uani 1 1 d . . . H14 H 0.5882 0.5809 0.1297 0.077 Uiso 1 1 calc R . . C111 C 1.1388(4) 0.9770(5) 0.3964(4) 0.078(2) Uani 1 1 d . . . H111 H 1.1073 0.9198 0.3697 0.093 Uiso 1 1 calc R . . C96 C 0.8007(4) 1.1343(4) 0.4945(4) 0.0679(17) Uani 1 1 d . . . H96 H 0.8199 1.1827 0.5375 0.081 Uiso 1 1 calc R . . C93 C -0.4680(4) 0.3484(4) -0.0086(4) 0.0717(18) Uani 1 1 d . . . H93 H -0.5122 0.3117 -0.0038 0.086 Uiso 1 1 calc R . . C105 C 0.8575(4) 0.7871(4) 0.1495(4) 0.0726(19) Uani 1 1 d . . . H105 H 0.9144 0.8025 0.1612 0.087 Uiso 1 1 calc R . . C81 C 0.1916(3) 0.6308(4) 0.1599(4) 0.0678(17) Uani 1 1 d . . . H81 H 0.1660 0.6006 0.1824 0.081 Uiso 1 1 calc R . . C120 C 1.6440(4) 1.2268(6) 0.6224(4) 0.088(2) Uani 1 1 d . . . H120 H 1.6859 1.2772 0.6327 0.105 Uiso 1 1 calc R . . C34 C 0.8043(4) 0.2476(4) 0.0973(4) 0.0732(19) Uani 1 1 d . . . H34 H 0.8254 0.2210 0.0642 0.088 Uiso 1 1 calc R . . N24 N 1.8557(4) 1.1937(5) 0.7543(4) 0.102(2) Uani 1 1 d . . . C131 C 0.6157(4) 0.1374(4) 0.3058(4) 0.0675(17) Uani 1 1 d . . . H131 H 0.5972 0.0860 0.3072 0.081 Uiso 1 1 calc R . . C118 C 1.5599(5) 1.2067(7) 0.5850(4) 0.104(3) Uani 1 1 d . . . H118 H 1.5463 1.2450 0.5717 0.125 Uiso 1 1 calc R . . C80 C 0.2706(3) 0.7204(4) 0.0945(4) 0.0646(17) Uani 1 1 d . . . H80 H 0.2963 0.7496 0.0714 0.078 Uiso 1 1 calc R . . C110 C 1.1505(4) 1.1151(4) 0.4412(4) 0.080(2) Uani 1 1 d . . . H110 H 1.1264 1.1530 0.4454 0.096 Uiso 1 1 calc R . . C114 C 1.2722(4) 1.0922(7) 0.4686(4) 0.097(3) Uani 1 1 d . . . C51 C 1.2226(4) 0.6762(4) 0.4888(4) 0.078(2) Uani 1 1 d . . . H51 H 1.2507 0.7340 0.5132 0.094 Uiso 1 1 calc R . . C52 C 1.2683(3) 0.6282(4) 0.4833(3) 0.0637(17) Uani 1 1 d . . . C22 C 0.0453(3) 0.1248(4) 0.0898(4) 0.0708(19) Uani 1 1 d . . . H22 H 0.0190 0.1544 0.0738 0.085 Uiso 1 1 calc R . . C28 C -0.2206(3) -0.0920(4) 0.0440(4) 0.0721(19) Uani 1 1 d . . . H28 H -0.2471 -0.1423 0.0455 0.087 Uiso 1 1 calc R . . C27 C -0.2273(3) 0.0176(4) 0.0153(4) 0.074(2) Uani 1 1 d . . . H27 H -0.2584 0.0423 -0.0030 0.089 Uiso 1 1 calc R . . C87 C -0.1278(4) 0.4867(4) 0.1105(4) 0.077(2) Uani 1 1 d . . . H87 H -0.0977 0.4804 0.1488 0.092 Uiso 1 1 calc R . . C65 C 0.6317(4) 0.6604(4) 0.3425(4) 0.0740(19) Uani 1 1 d . . . H65 H 0.6145 0.6173 0.3561 0.089 Uiso 1 1 calc R . . O5 O 0.2497(4) 0.9278(4) 0.1577(4) 0.158(3) Uani 1 1 d . . . C113 C 1.2247(4) 1.0084(6) 0.4301(5) 0.091(2) Uani 1 1 d . . . H113 H 1.2501 0.9716 0.4262 0.110 Uiso 1 1 calc R . . C64 C 0.7133(4) 0.7043(4) 0.3596(4) 0.0705(18) Uani 1 1 d . . . H64 H 0.7529 0.6915 0.3843 0.085 Uiso 1 1 calc R . . C123 C 1.7740(5) 1.1647(5) 0.7309(4) 0.087(2) Uani 1 1 d . . . H123 H 1.7402 1.1306 0.7462 0.104 Uiso 1 1 calc R . . C89 C -0.2151(3) 0.4502(4) 0.0856(4) 0.0731(19) Uani 1 1 d . . . H89 H -0.2422 0.4208 0.1079 0.088 Uiso 1 1 calc R . . C53 C 1.3587(4) 0.6736(6) 0.5208(4) 0.095(2) Uani 1 1 d DU . . H53 H 1.3774 0.7310 0.5371 0.115 Uiso 1 1 calc R . . C17 C 0.2658(4) 0.2771(4) 0.1476(5) 0.098(2) Uani 1 1 d U . . H17 H 0.2934 0.3312 0.1538 0.118 Uiso 1 1 calc R . . C49 C 1.1371(3) 0.6409(3) 0.4594(4) 0.074(2) Uani 1 1 d . . . H49 H 1.1085 0.6748 0.4653 0.088 Uiso 1 1 calc R . . O1 O 1.0172(4) 0.7372(5) 0.3814(4) 0.167(3) Uani 1 1 d U . . O2 O 0.8843(5) 0.6753(6) 0.3665(6) 0.203(4) Uani 1 1 d U . . O3 O 0.9072(6) 0.7314(6) 0.2926(5) 0.203(4) Uani 1 1 d U . . O4 O 0.9392(5) 0.8092(6) 0.4132(5) 0.207(4) Uani 1 1 d U . . Cl3 Cl 0.05984(11) 0.77151(13) 0.66330(13) 0.0855(6) Uani 1 1 d . . . O9 O 0.0633(6) 0.7081(7) 0.6090(6) 0.242(5) Uani 1 1 d . . . O10 O -0.0167(5) 0.7564(7) 0.6489(7) 0.313(9) Uani 1 1 d . . . C19 C 0.1791(4) 0.2417(4) 0.1242(5) 0.100(2) Uani 1 1 d U . . H19 H 0.1500 0.2728 0.1156 0.120 Uiso 1 1 calc R . . C119 C 1.5212(5) 1.0778(6) 0.5886(5) 0.109(3) Uani 1 1 d . . . H119 H 1.4808 1.0257 0.5767 0.131 Uiso 1 1 calc R . . C121 C 1.6012(4) 1.0976(5) 0.6260(4) 0.093(2) Uani 1 1 d . . . H121 H 1.6146 1.0599 0.6404 0.112 Uiso 1 1 calc R . . Cl4 Cl 0.42525(18) 0.52005(19) 0.35048(18) 0.1428(11) Uani 1 1 d . . . O12 O 0.4510(7) 0.4843(6) 0.2991(7) 0.305(8) Uani 1 1 d . . . O13 O 0.4934(6) 0.5648(10) 0.4128(6) 0.394(12) Uani 1 1 d . . . O15 O 0.3638(6) 0.4710(5) 0.3622(8) 0.278(7) Uani 1 1 d . . . O14 O 0.3798(12) 0.5599(13) 0.309(2) 0.63(3) Uani 1 1 d . . . O17 O 0.0984(8) 0.8408(7) 0.6685(8) 0.330(9) Uani 1 1 d . . . C115 C 1.3636(5) 1.1294(7) 0.5084(5) 0.140(4) Uani 1 1 d D . . H115 H 1.3897 1.1861 0.5214 0.168 Uiso 1 1 calc R . . C116 C 1.4098(6) 1.1003(8) 0.5269(5) 0.136(4) Uani 1 1 d D . . H116 H 1.3822 1.0431 0.5107 0.164 Uiso 1 1 calc R . . O1W O 0.9509(3) 0.1381(4) 0.8416(4) 0.133(2) Uani 1 1 d . . . O3W O 0.3514(4) 0.4764(5) 0.1479(5) 0.156(3) Uani 1 1 d . . . O5W O 0.9557(6) 0.6866(6) 0.7795(5) 0.215(4) Uani 1 1 d . . . O2W O 0.9194(8) 0.1893(7) 0.9612(6) 0.260(5) Uani 1 1 d . . . O6W O 0.1932(7) 0.4382(8) 0.1477(10) 0.346(10) Uani 1 1 d . . . O7W O 0.8157(10) 0.6545(7) 0.6996(7) 0.320(7) Uani 1 1 d . . . O4W O 0.0309(8) 0.3422(10) 0.0908(11) 0.351(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C122 0.050(4) 0.094(5) 0.058(4) 0.031(4) 0.016(3) 0.026(4) C117 0.045(4) 0.166(8) 0.070(5) 0.053(6) 0.019(4) 0.033(5) C62 0.042(4) 0.097(5) 0.094(6) 0.038(4) 0.012(4) 0.030(4) N12 0.037(3) 0.079(4) 0.091(4) 0.034(3) 0.006(3) 0.013(3) N11 0.036(3) 0.082(4) 0.086(4) 0.019(3) 0.010(3) 0.022(3) C61 0.052(4) 0.085(5) 0.083(5) 0.035(4) 0.018(4) 0.034(4) N10 0.033(3) 0.073(3) 0.068(4) 0.021(3) 0.010(2) 0.013(2) C59 0.047(4) 0.155(7) 0.090(6) 0.065(5) 0.025(4) 0.042(4) C60 0.030(3) 0.119(6) 0.056(4) 0.033(4) 0.011(3) 0.021(4) C58 0.043(4) 0.089(5) 0.082(5) 0.004(4) 0.018(4) 0.004(3) C57 0.056(4) 0.188(7) 0.089(5) 0.090(6) 0.032(4) 0.057(5) C56 0.050(5) 0.131(7) 0.078(6) 0.010(5) 0.011(4) 0.011(5) C55 0.059(5) 0.165(7) 0.076(5) 0.058(6) 0.029(4) 0.024(5) Zn1 0.0235(3) 0.0458(3) 0.0488(4) 0.0197(3) 0.0046(3) 0.0102(2) Zn2 0.0296(3) 0.0476(4) 0.0555(4) 0.0231(3) 0.0077(3) 0.0122(3) Cl2 0.0616(10) 0.0537(8) 0.0896(13) 0.0323(8) 0.0263(9) 0.0275(7) Cl1 0.0440(9) 0.0938(13) 0.1040(16) 0.0491(12) 0.0112(10) 0.0122(9) C83 0.042(3) 0.051(3) 0.078(5) 0.024(3) 0.017(3) 0.017(3) N3 0.031(2) 0.044(2) 0.048(3) 0.023(2) 0.007(2) 0.0100(18) C33 0.066(4) 0.063(4) 0.048(4) 0.007(3) 0.004(3) 0.014(3) N9 0.037(2) 0.054(3) 0.051(3) 0.023(2) 0.011(2) 0.021(2) N1 0.033(2) 0.057(3) 0.060(3) 0.032(2) 0.016(2) 0.020(2) N2 0.032(2) 0.038(2) 0.044(3) 0.0158(19) 0.0100(19) 0.0160(18) N20 0.040(2) 0.042(2) 0.052(3) 0.021(2) 0.011(2) 0.017(2) N15 0.035(2) 0.043(2) 0.057(3) 0.025(2) 0.015(2) 0.0117(19) N8 0.031(2) 0.038(2) 0.043(3) 0.015(2) 0.005(2) 0.0108(18) N7 0.030(2) 0.045(2) 0.046(3) 0.012(2) 0.005(2) 0.0100(18) N21 0.037(2) 0.049(2) 0.050(3) 0.021(2) 0.011(2) 0.016(2) N16 0.032(2) 0.054(3) 0.061(3) 0.017(2) 0.005(2) 0.014(2) N4 0.033(2) 0.054(3) 0.057(3) 0.022(2) 0.007(2) 0.009(2) N19 0.035(2) 0.046(2) 0.060(3) 0.023(2) 0.009(2) 0.013(2) N13 0.038(2) 0.048(2) 0.057(3) 0.027(2) 0.011(2) 0.015(2) N14 0.035(2) 0.041(2) 0.051(3) 0.018(2) 0.011(2) 0.0156(19) C38 0.034(3) 0.051(3) 0.057(4) 0.019(3) 0.011(3) 0.018(2) O7 0.127(4) 0.108(4) 0.077(3) 0.039(3) 0.045(3) 0.078(3) N17 0.038(3) 0.089(4) 0.081(4) 0.051(3) 0.018(3) 0.015(3) N18 0.037(3) 0.086(4) 0.090(4) 0.038(3) 0.010(3) 0.019(3) C8 0.034(3) 0.041(3) 0.053(3) 0.019(2) 0.013(3) 0.011(2) C42 0.036(3) 0.046(3) 0.048(3) 0.020(3) 0.008(3) 0.013(2) C24 0.033(3) 0.068(4) 0.054(4) 0.023(3) 0.009(3) 0.014(3) C10 0.034(3) 0.044(3) 0.057(4) 0.018(3) 0.007(3) 0.017(2) C5 0.047(3) 0.046(3) 0.069(4) 0.026(3) 0.016(3) 0.017(3) C4 0.073(5) 0.085(4) 0.075(5) 0.048(4) 0.029(4) 0.055(4) C16 0.031(3) 0.045(3) 0.071(4) 0.017(3) 0.011(3) 0.014(2) C12 0.033(3) 0.046(3) 0.044(3) 0.021(2) 0.009(2) 0.017(2) C78 0.038(3) 0.041(3) 0.063(4) 0.016(3) 0.012(3) 0.014(2) C70 0.034(3) 0.041(3) 0.056(4) 0.014(3) 0.013(3) 0.013(2) C72 0.033(3) 0.042(3) 0.044(3) 0.016(2) 0.007(2) 0.013(2) C85 0.041(3) 0.073(4) 0.075(5) 0.020(4) 0.011(3) 0.012(3) C100 0.043(3) 0.055(3) 0.050(4) 0.020(3) 0.003(3) 0.012(3) C37 0.031(3) 0.041(3) 0.050(3) 0.017(2) 0.006(2) 0.012(2) C91 0.036(3) 0.051(3) 0.060(4) 0.018(3) 0.011(3) 0.017(2) C41 0.034(3) 0.044(3) 0.048(3) 0.020(3) 0.007(3) 0.013(2) C47 0.029(3) 0.053(3) 0.065(4) 0.023(3) 0.005(3) 0.012(2) C40 0.036(3) 0.042(3) 0.051(4) 0.012(3) 0.002(3) 0.007(2) N6 0.036(3) 0.084(4) 0.081(4) 0.042(3) -0.001(3) 0.010(3) C69 0.040(3) 0.043(3) 0.070(4) 0.024(3) 0.017(3) 0.011(2) C39 0.031(3) 0.042(3) 0.062(4) 0.023(3) 0.006(3) 0.012(2) C112 0.049(5) 0.135(7) 0.074(6) 0.011(5) 0.013(4) 0.012(5) C20 0.036(3) 0.062(3) 0.076(4) 0.034(3) 0.017(3) 0.010(3) C104 0.040(3) 0.049(3) 0.056(4) 0.020(3) 0.012(3) 0.018(2) C6 0.041(3) 0.050(3) 0.053(3) 0.024(3) 0.022(3) 0.021(2) N5 0.041(3) 0.066(3) 0.082(4) 0.036(3) 0.011(3) 0.014(2) C71 0.039(3) 0.050(3) 0.053(4) 0.019(3) 0.010(3) 0.021(2) C74 0.048(3) 0.068(4) 0.062(4) 0.037(3) 0.016(3) 0.028(3) C86 0.039(3) 0.068(4) 0.067(4) 0.023(3) 0.011(3) 0.015(3) C124 0.041(4) 0.163(9) 0.089(6) 0.026(6) 0.015(4) 0.032(5) C11 0.028(3) 0.037(3) 0.046(3) 0.014(2) 0.007(2) 0.011(2) C9 0.028(3) 0.040(3) 0.057(4) 0.010(3) 0.010(3) 0.010(2) C102 0.039(3) 0.054(3) 0.064(4) 0.024(3) 0.019(3) 0.020(3) C36 0.035(3) 0.044(3) 0.048(3) 0.016(3) 0.009(3) 0.016(2) C107 0.071(5) 0.048(3) 0.067(5) 0.009(3) 0.009(4) 0.013(3) C54 0.063(5) 0.182(7) 0.090(5) 0.063(5) 0.028(4) 0.038(5) C23 0.039(3) 0.075(4) 0.062(4) 0.026(3) 0.006(3) 0.015(3) C7 0.034(3) 0.036(3) 0.045(3) 0.016(2) 0.012(2) 0.014(2) C68 0.034(3) 0.041(3) 0.057(4) 0.022(3) 0.015(3) 0.013(2) C29 0.032(3) 0.054(3) 0.052(4) 0.021(3) 0.009(3) 0.011(2) C32 0.044(3) 0.058(3) 0.043(4) 0.012(3) 0.002(3) 0.010(3) C88 0.045(4) 0.075(4) 0.093(5) 0.042(4) 0.022(4) 0.020(3) C13 0.038(3) 0.060(3) 0.072(4) 0.034(3) 0.010(3) 0.017(3) C109 0.037(3) 0.074(4) 0.061(4) 0.034(3) 0.013(3) 0.016(3) C077 0.042(3) 0.059(3) 0.059(4) 0.030(3) 0.011(3) 0.015(3) C82 0.042(3) 0.066(4) 0.092(5) 0.036(4) 0.007(3) 0.020(3) C25 0.037(3) 0.056(4) 0.116(6) 0.037(4) 0.016(4) 0.010(3) C77 0.048(3) 0.062(3) 0.066(4) 0.034(3) 0.021(3) 0.023(3) C94 0.055(4) 0.062(4) 0.060(4) 0.030(3) 0.019(3) 0.029(3) C73 0.040(3) 0.049(3) 0.046(3) 0.020(3) 0.011(3) 0.021(2) C98 0.046(3) 0.043(3) 0.052(4) 0.023(3) 0.016(3) 0.019(2) C103 0.036(3) 0.042(3) 0.059(4) 0.022(3) 0.010(3) 0.015(2) C35 0.048(3) 0.067(4) 0.066(4) 0.011(3) 0.017(3) 0.024(3) O8 0.141(5) 0.054(3) 0.143(5) 0.029(3) -0.005(4) 0.024(3) C67 0.043(3) 0.045(3) 0.060(4) 0.022(3) 0.016(3) 0.017(2) C101 0.033(3) 0.056(3) 0.062(4) 0.029(3) 0.006(3) 0.014(3) C84 0.037(3) 0.060(4) 0.087(5) 0.027(3) 0.013(3) 0.013(3) C50 0.036(3) 0.081(4) 0.090(5) 0.043(4) 0.013(3) 0.028(3) C99 0.036(3) 0.044(3) 0.050(3) 0.020(3) 0.007(3) 0.012(2) C21 0.029(3) 0.059(3) 0.102(5) 0.031(3) 0.021(3) 0.016(3) C108 0.045(3) 0.046(3) 0.064(4) 0.018(3) 0.007(3) 0.009(3) O6 0.188(6) 0.149(5) 0.088(4) 0.077(4) 0.063(4) 0.115(5) C48 0.038(3) 0.057(3) 0.088(5) 0.031(3) 0.004(3) 0.017(3) C90 0.044(3) 0.066(4) 0.081(5) 0.033(4) 0.013(3) 0.019(3) O11 0.252(11) 0.243(10) 0.158(9) 0.109(8) 0.004(8) 0.037(8) C63 0.051(3) 0.066(4) 0.069(4) 0.037(3) 0.015(3) 0.025(3) N22 0.045(3) 0.111(4) 0.070(4) 0.038(4) 0.016(3) 0.025(3) C95 0.060(4) 0.064(4) 0.072(5) 0.031(4) 0.025(4) 0.032(3) C106 0.077(5) 0.059(4) 0.083(5) 0.007(4) 0.026(4) 0.026(4) C76 0.064(4) 0.058(3) 0.069(4) 0.037(3) 0.028(3) 0.023(3) C79 0.041(3) 0.078(4) 0.072(4) 0.029(4) 0.018(3) 0.022(3) C3 0.046(3) 0.076(4) 0.077(4) 0.047(4) 0.020(3) 0.031(3) C97 0.054(4) 0.057(3) 0.056(4) 0.019(3) 0.010(3) 0.017(3) C75 0.074(4) 0.072(4) 0.070(4) 0.044(4) 0.026(4) 0.039(4) C30 0.035(3) 0.083(4) 0.075(5) 0.047(4) 0.004(3) 0.011(3) C45 0.066(4) 0.075(4) 0.062(4) 0.027(4) 0.031(4) 0.040(3) C15 0.062(4) 0.055(3) 0.085(5) 0.040(3) 0.025(4) 0.015(3) C43 0.053(3) 0.055(3) 0.052(4) 0.016(3) 0.012(3) 0.021(3) C18 0.031(3) 0.063(3) 0.079(4) 0.034(3) 0.015(3) 0.014(3) C92 0.044(4) 0.069(4) 0.085(5) 0.039(4) 0.011(3) 0.021(3) C44 0.082(5) 0.065(4) 0.052(4) 0.016(3) 0.023(4) 0.041(4) C26 0.042(4) 0.111(5) 0.110(6) 0.076(5) 0.018(4) 0.025(4) C46 0.040(3) 0.068(4) 0.063(4) 0.032(3) 0.016(3) 0.026(3) C31 0.031(3) 0.072(4) 0.095(5) 0.035(4) 0.007(3) 0.002(3) N23 0.050(4) 0.152(6) 0.081(5) 0.043(4) 0.026(3) 0.026(4) C66 0.052(4) 0.059(4) 0.093(5) 0.044(4) 0.025(4) 0.016(3) C14 0.059(4) 0.066(4) 0.076(5) 0.045(3) 0.014(3) 0.029(3) C111 0.044(4) 0.100(5) 0.093(5) 0.056(4) 0.017(4) 0.024(4) C96 0.084(5) 0.054(3) 0.060(4) 0.020(3) 0.025(4) 0.028(3) C93 0.037(4) 0.084(4) 0.090(5) 0.046(4) 0.014(3) 0.018(3) C105 0.049(4) 0.061(4) 0.086(5) 0.011(4) 0.021(4) 0.022(3) C81 0.043(3) 0.073(4) 0.079(5) 0.032(4) 0.018(3) 0.016(3) C120 0.065(5) 0.129(6) 0.074(5) 0.049(5) 0.027(4) 0.040(5) C34 0.075(5) 0.072(4) 0.058(4) 0.010(3) 0.032(4) 0.028(4) N24 0.059(4) 0.139(6) 0.086(5) 0.027(4) 0.016(4) 0.045(4) C131 0.073(5) 0.059(4) 0.079(5) 0.036(3) 0.022(4) 0.035(3) C118 0.087(6) 0.179(9) 0.074(5) 0.070(6) 0.028(5) 0.072(6) C80 0.039(3) 0.066(4) 0.092(5) 0.044(4) 0.017(3) 0.020(3) C110 0.037(3) 0.092(5) 0.072(5) 0.013(4) 0.013(3) 0.007(3) C114 0.037(4) 0.164(9) 0.061(5) 0.048(5) 0.008(4) 0.012(5) C51 0.039(3) 0.058(4) 0.090(5) 0.012(3) 0.001(3) -0.001(3) C52 0.032(3) 0.084(4) 0.062(4) 0.036(4) 0.003(3) 0.013(3) C22 0.030(3) 0.065(4) 0.100(5) 0.033(4) 0.007(3) 0.013(3) C28 0.037(3) 0.085(4) 0.101(5) 0.061(4) 0.019(3) 0.014(3) C27 0.039(3) 0.062(4) 0.107(6) 0.034(4) 0.010(4) 0.016(3) C87 0.041(4) 0.096(5) 0.077(5) 0.042(4) 0.004(3) 0.015(3) C65 0.065(4) 0.073(4) 0.102(6) 0.058(4) 0.025(4) 0.032(4) O5 0.078(4) 0.180(6) 0.203(8) 0.067(6) 0.080(5) 0.034(4) C113 0.057(5) 0.152(8) 0.100(6) 0.079(6) 0.032(5) 0.056(5) C64 0.069(4) 0.079(4) 0.084(5) 0.048(4) 0.024(4) 0.045(4) C123 0.065(5) 0.115(6) 0.083(6) 0.043(5) 0.022(4) 0.041(4) C89 0.037(3) 0.095(5) 0.083(5) 0.043(4) 0.016(3) 0.021(3) C53 0.052(4) 0.173(6) 0.086(5) 0.076(5) 0.027(4) 0.053(4) C17 0.039(3) 0.060(4) 0.180(7) 0.056(4) 0.019(4) 0.012(3) C49 0.037(3) 0.052(3) 0.100(5) 0.015(3) 0.003(3) 0.013(3) O1 0.092(4) 0.206(6) 0.153(6) 0.023(4) 0.038(4) 0.062(4) O2 0.173(6) 0.189(6) 0.249(8) 0.143(6) 0.065(5) 0.031(5) O3 0.246(8) 0.210(7) 0.164(7) 0.115(6) 0.043(5) 0.090(6) O4 0.178(7) 0.180(6) 0.193(7) 0.008(5) 0.015(5) 0.101(5) Cl3 0.0560(11) 0.0792(12) 0.0986(16) 0.0327(11) 0.0143(11) 0.0158(9) O9 0.196(9) 0.239(10) 0.201(10) -0.003(8) 0.025(8) 0.121(8) O10 0.073(5) 0.320(13) 0.295(14) -0.095(10) 0.031(7) 0.051(6) C19 0.043(3) 0.071(4) 0.169(6) 0.051(4) 0.014(4) 0.021(3) C119 0.053(5) 0.163(8) 0.101(7) 0.064(6) 0.011(4) 0.035(5) C121 0.057(4) 0.110(6) 0.104(6) 0.054(5) 0.022(4) 0.020(4) Cl4 0.106(2) 0.138(2) 0.141(2) 0.0249(18) 0.0650(19) 0.0234(17) O12 0.286(12) 0.194(8) 0.306(14) -0.050(8) 0.222(12) 0.037(8) O13 0.109(7) 0.58(2) 0.147(9) -0.062(12) 0.031(7) -0.024(11) O15 0.224(10) 0.163(7) 0.465(19) 0.126(10) 0.244(12) 0.033(7) O14 0.44(2) 0.52(3) 1.53(8) 0.76(5) 0.64(4) 0.40(2) O17 0.342(16) 0.182(9) 0.331(17) 0.176(11) -0.035(12) -0.024(10) C115 0.078(6) 0.265(13) 0.081(7) 0.086(8) 0.041(5) 0.058(8) C116 0.087(6) 0.287(14) 0.098(7) 0.111(8) 0.054(6) 0.109(8) O1W 0.066(3) 0.142(5) 0.140(6) 0.037(4) 0.012(4) 0.023(3) O3W 0.125(5) 0.197(7) 0.234(9) 0.168(7) 0.073(6) 0.085(5) O5W 0.213(9) 0.259(10) 0.192(9) 0.077(8) 0.096(8) 0.130(8) O2W 0.338(15) 0.288(12) 0.207(11) 0.134(10) 0.099(10) 0.164(12) O6W 0.257(12) 0.336(15) 0.72(3) 0.40(2) 0.282(17) 0.201(11) O7W 0.55(2) 0.246(12) 0.245(13) 0.112(10) 0.183(15) 0.232(14) O4W 0.267(13) 0.45(2) 0.62(3) 0.41(2) 0.268(17) 0.239(14) _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 C122 C120 1.333(9) . ? C122 C121 1.353(9) . ? C122 N22 1.433(8) . ? C117 C119 1.347(11) . ? C117 C118 1.385(11) . ? C117 C116 1.456(11) . ? C62 N11 1.293(7) . ? C62 N12 1.366(8) . ? C62 H62 0.9300 . ? N12 C61 1.304(7) . ? N11 N10 1.362(6) . ? C61 N10 1.334(7) . ? C61 H61 0.9300 . ? N10 C60 1.432(7) . ? C59 C60 1.399(9) . ? C59 C57 1.474(10) . ? C59 H59 0.9300 . ? C60 C58 1.379(9) . ? C58 C56 1.370(9) . ? C58 H58 0.9300 . ? C57 C55 1.421(12) . ? C57 H57 0.9300 . ? C56 C55 1.313(12) . ? C56 H56 0.9300 . ? C55 C54 1.528(11) . ? Zn1 N8 2.064(4) . ? Zn1 N2 2.065(4) . ? Zn1 N9 2.170(4) . ? Zn1 N1 2.183(4) . ? Zn1 N3 2.194(4) . ? Zn1 N7 2.206(4) . ? Zn2 N20 2.057(4) . ? Zn2 N14 2.071(4) . ? Zn2 N19 2.186(5) . ? Zn2 N15 2.187(4) . ? Zn2 N21 2.189(4) . ? Zn2 N13 2.194(4) . ? Cl2 O8 1.385(5) . ? Cl2 O5 1.390(5) . ? Cl2 O6 1.415(5) . ? Cl2 O7 1.420(5) . ? Cl1 O2 1.332(7) . ? Cl1 O3 1.355(9) . ? Cl1 O1 1.366(7) . ? Cl1 O4 1.457(8) . ? C83 C82 1.398(8) . ? C83 C81 1.399(8) . ? C83 C84 1.469(7) . ? N3 C077 1.324(6) . ? N3 C12 1.351(6) . ? C33 C34 1.357(8) . ? C33 C32 1.364(8) . ? C33 H33 0.9300 . ? N9 C42 1.348(6) . ? N9 C46 1.358(6) . ? N1 C3 1.341(6) . ? N1 C6 1.344(6) . ? N2 C7 1.336(6) . ? N2 C11 1.351(6) . ? N20 C99 1.338(6) . ? N20 C103 1.351(6) . ? N15 C77 1.332(6) . ? N15 C73 1.350(6) . ? N8 C41 1.332(6) . ? N8 C37 1.336(6) . ? N7 C36 1.313(6) . ? N7 C32 1.339(7) . ? N21 C94 1.335(7) . ? N21 C98 1.340(6) . ? N16 C92 1.342(7) . ? N16 N17 1.359(6) . ? N16 C91 1.430(6) . ? N4 C30 1.345(7) . ? N4 N5 1.367(6) . ? N4 C29 1.419(6) . ? N19 C104 1.317(6) . ? N19 C108 1.340(7) . ? N13 C67 1.339(6) . ? N13 C63 1.342(7) . ? N14 C68 1.331(6) . ? N14 C72 1.337(6) . ? C38 C37 1.365(6) . ? C38 C39 1.400(7) . ? C38 H38 0.9300 . ? N17 C93 1.310(7) . ? N18 C92 1.314(7) . ? N18 C93 1.338(8) . ? C8 C7 1.378(6) . ? C8 C9 1.397(7) . ? C8 H8 0.9300 . ? C42 C43 1.379(7) . ? C42 C41 1.504(7) . ? C24 C25 1.376(8) . ? C24 C26 1.378(8) . ? C24 C23 1.468(7) . ? C10 C11 1.374(6) . ? C10 C9 1.411(7) . ? C10 H10 0.9300 . ? C5 C131 1.374(8) . ? C5 C6 1.390(7) . ? C5 H5 0.9300 . ? C4 C131 1.359(8) . ? C4 C3 1.370(8) . ? C4 H4 0.9300 . ? C16 C17 1.362(8) . ? C16 C18 1.381(7) . ? C16 C9 1.477(6) . ? C12 C13 1.379(7) . ? C12 C11 1.478(7) . ? C78 C80 1.368(8) . ? C78 C79 1.406(8) . ? C78 C70 1.481(7) . ? C70 C69 1.387(7) . ? C70 C71 1.392(7) . ? C72 C71 1.373(6) . ? C72 C73 1.502(7) . ? C85 C84 1.273(8) . ? C85 C86 1.465(8) . ? C85 H85 0.9300 . ? C100 C99 1.371(7) . ? C100 C101 1.395(8) . ? C100 H100 0.9300 . ? C37 C36 1.502(7) . ? C91 C89 1.355(8) . ? C91 C90 1.382(8) . ? C41 C40 1.374(6) . ? C47 C48 1.376(7) . ? C47 C49 1.392(7) . ? C47 C39 1.477(7) . ? C40 C39 1.383(7) . ? C40 H40 0.9300 . ? N6 C30 1.293(7) . ? N6 C31 1.321(8) . ? C69 C68 1.383(7) . ? C69 H69 0.9300 . ? C112 C114 1.344(12) . ? C112 C110 1.352(9) . ? C112 H112 0.9300 . ? C20 C21 1.368(8) . ? C20 C18 1.374(7) . ? C20 H20 0.9300 . ? C104 C105 1.390(8) . ? C104 C103 1.504(7) . ? C6 C7 1.474(7) . ? N5 C31 1.332(7) . ? C71 H71 0.9300 . ? C74 C75 1.357(8) . ? C74 C73 1.398(7) . ? C74 H74 0.9300 . ? C86 C87 1.371(8) . ? C86 C88 1.406(8) . ? C124 N23 1.324(10) . ? C124 N24 1.360(11) . ? C124 H124 0.9300 . ? C102 C103 1.377(7) . ? C102 C101 1.382(8) . ? C102 H102 0.9300 . ? C36 C35 1.384(8) . ? C107 C106 1.345(9) . ? C107 C108 1.368(9) . ? C107 H107 0.9300 . ? C54 C53 1.198(2) . ? C54 H54 0.9300 . ? C23 C22 1.303(8) . ? C23 H23 0.9300 . ? C68 C67 1.486(7) . ? C29 C28 1.362(8) . ? C29 C27 1.364(8) . ? C32 H32 0.9300 . ? C88 C90 1.374(8) . ? C88 H88 0.9300 . ? C13 C14 1.369(7) . ? C13 H13 0.9300 . ? C109 C110 1.370(8) . ? C109 C111 1.379(8) . ? C109 C101 1.465(7) . ? C077 C15 1.393(8) . ? C077 H077 0.9300 . ? C82 C80 1.378(7) . ? C82 H82 0.9300 . ? C25 C27 1.372(7) . ? C25 H25 0.9300 . ? C77 C76 1.371(8) . ? C77 H77 0.9300 . ? C94 C95 1.353(8) . ? C94 H94 0.9300 . ? C98 C97 1.359(8) . ? C98 C99 1.497(7) . ? C35 C34 1.379(8) . ? C35 H35 0.9300 . ? C67 C66 1.380(7) . ? C84 H84 0.9300 . ? C50 C52 1.364(8) . ? C50 C48 1.390(7) . ? C50 H50 0.9300 . ? C21 C19 1.390(8) . ? C21 C22 1.457(7) . ? C108 H108 0.9300 . ? C48 H48 0.9300 . ? C90 H90 0.9300 . ? O11 Cl3 1.368(9) . ? C63 C64 1.363(8) . ? C63 H63 0.9300 . ? N22 C123 1.340(9) . ? N22 N23 1.376(7) . ? C95 C96 1.378(8) . ? C95 H95 0.9300 . ? C106 C105 1.379(9) . ? C106 H106 0.9300 . ? C76 C75 1.381(8) . ? C76 H76 0.9300 . ? C79 C81 1.383(7) . ? C79 H79 0.9300 . ? C3 H3 0.9300 . ? C97 C96 1.366(8) . ? C97 H97 0.9300 . ? C75 H75 0.9300 . ? C30 C31 2.032(9) . ? C30 H30 0.9300 . ? C45 C46 1.347(8) . ? C45 C44 1.379(8) . ? C45 H45 0.9300 . ? C15 C14 1.376(8) . ? C15 H15 0.9300 . ? C43 C44 1.374(8) . ? C43 H43 0.9300 . ? C18 H18 0.9300 . ? C92 H92 0.9300 . ? C44 H44 0.9300 . ? C26 C28 1.395(7) . ? C26 H26 0.9300 . ? C46 H46 0.9300 . ? C31 H31 0.9300 . ? C66 C65 1.378(8) . ? C66 H66 0.9300 . ? C14 H14 0.9300 . ? C111 C113 1.395(9) . ? C111 H111 0.9300 . ? C96 H96 0.9300 . ? C93 H93 0.9300 . ? C105 H105 0.9300 . ? C81 H81 0.9300 . ? C120 C118 1.417(10) . ? C120 H120 0.9300 . ? C34 H34 0.9300 . ? N24 C123 1.317(8) . ? C131 H131 0.9300 . ? C118 H118 0.9300 . ? C80 H80 0.9300 . ? C110 H110 0.9300 . ? C114 C113 1.366(11) . ? C114 C115 1.490(11) . ? C51 C49 1.377(8) . ? C51 C52 1.389(8) . ? C51 H51 0.9300 . ? C52 C53 1.468(9) . ? C22 H22 0.9300 . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C87 C89 1.405(8) . ? C87 H87 0.9300 . ? C65 C64 1.347(8) . ? C65 H65 0.9300 . ? C113 H113 0.9300 . ? C64 H64 0.9300 . ? C123 H123 0.9300 . ? C89 H89 0.9300 . ? C53 H53 0.9300 . ? C17 C19 1.397(8) . ? C17 H17 0.9300 . ? C49 H49 0.9300 . ? Cl3 O17 1.223(9) . ? Cl3 O10 1.269(7) . ? Cl3 O9 1.361(10) . ? C19 H19 0.9300 . ? C119 C121 1.354(9) . ? C119 H119 0.9300 . ? C121 H121 0.9300 . ? Cl4 O12 1.316(8) . ? Cl4 O15 1.333(7) . ? Cl4 O13 1.360(10) . ? Cl4 O14 1.58(2) . ? C115 C116 1.196(2) . ? C115 H115 0.9300 . ? C116 H116 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 C120 C122 C121 120.7(7) . . ? C120 C122 N22 120.4(6) . . ? C121 C122 N22 118.9(7) . . ? C119 C117 C118 117.1(8) . . ? C119 C117 C116 116.5(9) . . ? C118 C117 C116 126.4(9) . . ? N11 C62 N12 117.3(6) . . ? N11 C62 H62 121.3 . . ? N12 C62 H62 121.3 . . ? C61 N12 C62 100.0(5) . . ? C62 N11 N10 101.5(5) . . ? N12 C61 N10 112.6(6) . . ? N12 C61 H61 123.7 . . ? N10 C61 H61 123.7 . . ? C61 N10 N11 108.6(5) . . ? C61 N10 C60 130.6(5) . . ? N11 N10 C60 120.8(5) . . ? C60 C59 C57 114.6(8) . . ? C60 C59 H59 122.7 . . ? C57 C59 H59 122.7 . . ? C58 C60 C59 122.5(6) . . ? C58 C60 N10 120.8(6) . . ? C59 C60 N10 116.7(7) . . ? C56 C58 C60 120.8(8) . . ? C56 C58 H58 119.6 . . ? C60 C58 H58 119.6 . . ? C55 C57 C59 119.7(7) . . ? C55 C57 H57 120.2 . . ? C59 C57 H57 120.2 . . ? C55 C56 C58 121.3(9) . . ? C55 C56 H56 119.3 . . ? C58 C56 H56 119.3 . . ? C56 C55 C57 121.1(8) . . ? C56 C55 C54 117.4(9) . . ? C57 C55 C54 121.5(8) . . ? N8 Zn1 N2 178.67(15) . . ? N8 Zn1 N9 76.11(16) . . ? N2 Zn1 N9 104.04(15) . . ? N8 Zn1 N1 102.99(15) . . ? N2 Zn1 N1 75.68(15) . . ? N9 Zn1 N1 99.23(16) . . ? N8 Zn1 N3 105.91(15) . . ? N2 Zn1 N3 75.41(15) . . ? N9 Zn1 N3 91.59(15) . . ? N1 Zn1 N3 150.81(15) . . ? N8 Zn1 N7 75.13(15) . . ? N2 Zn1 N7 104.69(15) . . ? N9 Zn1 N7 151.22(15) . . ? N1 Zn1 N7 86.30(16) . . ? N3 Zn1 N7 97.16(16) . . ? N20 Zn2 N14 176.62(17) . . ? N20 Zn2 N19 75.82(16) . . ? N14 Zn2 N19 105.05(16) . . ? N20 Zn2 N15 107.34(15) . . ? N14 Zn2 N15 75.89(16) . . ? N19 Zn2 N15 96.15(16) . . ? N20 Zn2 N21 75.52(16) . . ? N14 Zn2 N21 103.66(16) . . ? N19 Zn2 N21 151.29(16) . . ? N15 Zn2 N21 90.55(16) . . ? N20 Zn2 N13 101.46(16) . . ? N14 Zn2 N13 75.34(16) . . ? N19 Zn2 N13 90.00(16) . . ? N15 Zn2 N13 151.20(15) . . ? N21 Zn2 N13 97.46(16) . . ? O8 Cl2 O5 108.3(4) . . ? O8 Cl2 O6 109.6(4) . . ? O5 Cl2 O6 110.1(4) . . ? O8 Cl2 O7 108.7(4) . . ? O5 Cl2 O7 110.8(4) . . ? O6 Cl2 O7 109.4(3) . . ? O2 Cl1 O3 108.4(6) . . ? O2 Cl1 O1 111.0(6) . . ? O3 Cl1 O1 119.9(6) . . ? O2 Cl1 O4 100.5(7) . . ? O3 Cl1 O4 107.4(6) . . ? O1 Cl1 O4 107.8(5) . . ? C82 C83 C81 117.0(5) . . ? C82 C83 C84 119.7(6) . . ? C81 C83 C84 123.3(6) . . ? C077 N3 C12 119.0(4) . . ? C077 N3 Zn1 126.1(3) . . ? C12 N3 Zn1 114.9(3) . . ? C34 C33 C32 118.7(6) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C42 N9 C46 117.2(5) . . ? C42 N9 Zn1 115.3(3) . . ? C46 N9 Zn1 127.1(4) . . ? C3 N1 C6 119.0(5) . . ? C3 N1 Zn1 125.6(4) . . ? C6 N1 Zn1 114.5(3) . . ? C7 N2 C11 120.2(4) . . ? C7 N2 Zn1 119.6(3) . . ? C11 N2 Zn1 120.1(3) . . ? C99 N20 C103 119.5(4) . . ? C99 N20 Zn2 120.4(4) . . ? C103 N20 Zn2 119.9(3) . . ? C77 N15 C73 118.8(4) . . ? C77 N15 Zn2 126.1(4) . . ? C73 N15 Zn2 114.9(3) . . ? C41 N8 C37 120.0(4) . . ? C41 N8 Zn1 119.5(3) . . ? C37 N8 Zn1 120.3(3) . . ? C36 N7 C32 119.6(5) . . ? C36 N7 Zn1 115.2(3) . . ? C32 N7 Zn1 125.2(4) . . ? C94 N21 C98 118.3(5) . . ? C94 N21 Zn2 126.4(4) . . ? C98 N21 Zn2 115.2(3) . . ? C92 N16 N17 109.1(4) . . ? C92 N16 C91 129.1(5) . . ? N17 N16 C91 121.8(5) . . ? C30 N4 N5 108.6(4) . . ? C30 N4 C29 129.9(5) . . ? N5 N4 C29 121.5(4) . . ? C104 N19 C108 119.5(5) . . ? C104 N19 Zn2 115.1(4) . . ? C108 N19 Zn2 125.3(4) . . ? C67 N13 C63 117.8(5) . . ? C67 N13 Zn2 115.1(3) . . ? C63 N13 Zn2 127.0(4) . . ? C68 N14 C72 120.2(4) . . ? C68 N14 Zn2 119.8(3) . . ? C72 N14 Zn2 120.0(3) . . ? C37 C38 C39 119.2(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C93 N17 N16 101.8(5) . . ? C92 N18 C93 102.4(5) . . ? C7 C8 C9 120.5(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? N9 C42 C43 122.4(5) . . ? N9 C42 C41 114.1(4) . . ? C43 C42 C41 123.5(5) . . ? C25 C24 C26 117.4(5) . . ? C25 C24 C23 123.2(5) . . ? C26 C24 C23 119.4(5) . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C131 C5 C6 118.9(5) . . ? C131 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C131 C4 C3 119.6(5) . . ? C131 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C17 C16 C18 117.0(5) . . ? C17 C16 C9 121.8(5) . . ? C18 C16 C9 121.2(5) . . ? N3 C12 C13 120.9(4) . . ? N3 C12 C11 115.4(4) . . ? C13 C12 C11 123.8(4) . . ? C80 C78 C79 117.5(5) . . ? C80 C78 C70 121.6(5) . . ? C79 C78 C70 120.9(5) . . ? C69 C70 C71 116.9(5) . . ? C69 C70 C78 121.5(5) . . ? C71 C70 C78 121.6(5) . . ? N14 C72 C71 121.4(5) . . ? N14 C72 C73 114.1(4) . . ? C71 C72 C73 124.4(5) . . ? C84 C85 C86 127.8(7) . . ? C84 C85 H85 116.1 . . ? C86 C85 H85 116.1 . . ? C99 C100 C101 120.6(5) . . ? C99 C100 H100 119.7 . . ? C101 C100 H100 119.7 . . ? N8 C37 C38 121.8(5) . . ? N8 C37 C36 113.5(4) . . ? C38 C37 C36 124.6(5) . . ? C89 C91 C90 120.3(5) . . ? C89 C91 N16 120.0(5) . . ? C90 C91 N16 119.7(5) . . ? N8 C41 C40 121.3(5) . . ? N8 C41 C42 114.4(4) . . ? C40 C41 C42 124.3(5) . . ? C48 C47 C49 117.4(5) . . ? C48 C47 C39 122.8(5) . . ? C49 C47 C39 119.7(5) . . ? C41 C40 C39 119.9(5) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C30 N6 C31 102.0(5) . . ? C68 C69 C70 120.6(5) . . ? C68 C69 H69 119.7 . . ? C70 C69 H69 119.7 . . ? C40 C39 C38 117.8(5) . . ? C40 C39 C47 121.1(5) . . ? C38 C39 C47 121.1(5) . . ? C114 C112 C110 122.2(8) . . ? C114 C112 H112 118.9 . . ? C110 C112 H112 118.9 . . ? C21 C20 C18 121.6(5) . . ? C21 C20 H20 119.2 . . ? C18 C20 H20 119.2 . . ? N19 C104 C105 121.3(5) . . ? N19 C104 C103 116.0(5) . . ? C105 C104 C103 122.6(5) . . ? N1 C6 C5 121.1(5) . . ? N1 C6 C7 115.5(4) . . ? C5 C6 C7 123.3(5) . . ? C31 N5 N4 100.2(5) . . ? C72 C71 C70 120.2(5) . . ? C72 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C75 C74 C73 118.9(5) . . ? C75 C74 H74 120.5 . . ? C73 C74 H74 120.5 . . ? C87 C86 C88 117.2(5) . . ? C87 C86 C85 120.4(6) . . ? C88 C86 C85 122.3(6) . . ? N23 C124 N24 116.2(7) . . ? N23 C124 H124 121.9 . . ? N24 C124 H124 121.9 . . ? N2 C11 C10 121.2(4) . . ? N2 C11 C12 114.0(4) . . ? C10 C11 C12 124.8(4) . . ? C8 C9 C10 116.8(4) . . ? C8 C9 C16 121.2(5) . . ? C10 C9 C16 122.0(5) . . ? C103 C102 C101 120.6(5) . . ? C103 C102 H102 119.7 . . ? C101 C102 H102 119.7 . . ? N7 C36 C35 121.2(5) . . ? N7 C36 C37 115.6(4) . . ? C35 C36 C37 123.2(5) . . ? C106 C107 C108 119.1(6) . . ? C106 C107 H107 120.4 . . ? C108 C107 H107 120.4 . . ? C53 C54 C55 126.9(9) . . ? C53 C54 H54 116.6 . . ? C55 C54 H54 116.6 . . ? C22 C23 C24 127.8(6) . . ? C22 C23 H23 116.1 . . ? C24 C23 H23 116.1 . . ? N2 C7 C8 121.1(4) . . ? N2 C7 C6 114.2(4) . . ? C8 C7 C6 124.6(4) . . ? N14 C68 C69 120.7(5) . . ? N14 C68 C67 114.8(4) . . ? C69 C68 C67 124.5(5) . . ? C28 C29 C27 119.5(5) . . ? C28 C29 N4 120.6(5) . . ? C27 C29 N4 119.9(5) . . ? N7 C32 C33 122.1(5) . . ? N7 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C90 C88 C86 121.6(6) . . ? C90 C88 H88 119.2 . . ? C86 C88 H88 119.2 . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C110 C109 C111 117.7(6) . . ? C110 C109 C101 121.8(6) . . ? C111 C109 C101 120.5(5) . . ? N3 C077 C15 122.6(5) . . ? N3 C077 H077 118.7 . . ? C15 C077 H077 118.7 . . ? C80 C82 C83 121.8(6) . . ? C80 C82 H82 119.1 . . ? C83 C82 H82 119.1 . . ? C27 C25 C24 122.0(6) . . ? C27 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? N15 C77 C76 122.6(5) . . ? N15 C77 H77 118.7 . . ? C76 C77 H77 118.7 . . ? N21 C94 C95 122.4(6) . . ? N21 C94 H94 118.8 . . ? C95 C94 H94 118.8 . . ? N15 C73 C74 121.1(5) . . ? N15 C73 C72 115.0(4) . . ? C74 C73 C72 123.9(5) . . ? N21 C98 C97 122.2(5) . . ? N21 C98 C99 114.8(4) . . ? C97 C98 C99 123.0(5) . . ? N20 C103 C102 121.0(5) . . ? N20 C103 C104 113.0(4) . . ? C102 C103 C104 126.0(5) . . ? C34 C35 C36 118.8(5) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? N13 C67 C66 121.7(5) . . ? N13 C67 C68 114.9(5) . . ? C66 C67 C68 123.3(5) . . ? C102 C101 C100 117.0(5) . . ? C102 C101 C109 122.2(5) . . ? C100 C101 C109 120.8(5) . . ? C85 C84 C83 127.4(7) . . ? C85 C84 H84 116.3 . . ? C83 C84 H84 116.3 . . ? C52 C50 C48 121.4(6) . . ? C52 C50 H50 119.3 . . ? C48 C50 H50 119.3 . . ? N20 C99 C100 121.3(5) . . ? N20 C99 C98 113.7(4) . . ? C100 C99 C98 124.9(5) . . ? C20 C21 C19 117.0(5) . . ? C20 C21 C22 122.7(5) . . ? C19 C21 C22 120.2(5) . . ? N19 C108 C107 121.7(6) . . ? N19 C108 H108 119.1 . . ? C107 C108 H108 119.1 . . ? C47 C48 C50 121.5(5) . . ? C47 C48 H48 119.2 . . ? C50 C48 H48 119.2 . . ? C88 C90 C91 119.6(6) . . ? C88 C90 H90 120.2 . . ? C91 C90 H90 120.2 . . ? N13 C63 C64 123.1(5) . . ? N13 C63 H63 118.4 . . ? C64 C63 H63 118.4 . . ? C123 N22 N23 109.5(6) . . ? C123 N22 C122 129.0(6) . . ? N23 N22 C122 121.5(6) . . ? C94 C95 C96 118.9(6) . . ? C94 C95 H95 120.5 . . ? C96 C95 H95 120.5 . . ? C107 C106 C105 120.0(6) . . ? C107 C106 H106 120.0 . . ? C105 C106 H106 120.0 . . ? C77 C76 C75 118.7(5) . . ? C77 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C81 C79 C78 121.5(6) . . ? C81 C79 H79 119.2 . . ? C78 C79 H79 119.2 . . ? N1 C3 C4 121.9(5) . . ? N1 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C98 C97 C96 119.1(6) . . ? C98 C97 H97 120.5 . . ? C96 C97 H97 120.5 . . ? C74 C75 C76 119.8(6) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? N6 C30 N4 111.9(5) . . ? N6 C30 C31 39.5(3) . . ? N4 C30 C31 72.4(4) . . ? N6 C30 H30 124.0 . . ? N4 C30 H30 124.0 . . ? C31 C30 H30 163.5 . . ? C46 C45 C44 118.9(5) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C14 C15 C077 118.3(5) . . ? C14 C15 H15 120.8 . . ? C077 C15 H15 120.8 . . ? C44 C43 C42 118.6(5) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C20 C18 C16 121.9(5) . . ? C20 C18 H18 119.0 . . ? C16 C18 H18 119.0 . . ? N18 C92 N16 110.4(6) . . ? N18 C92 H92 124.8 . . ? N16 C92 H92 124.8 . . ? C43 C44 C45 119.5(6) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C24 C26 C28 120.7(6) . . ? C24 C26 H26 119.7 . . ? C28 C26 H26 119.7 . . ? C45 C46 N9 123.3(5) . . ? C45 C46 H46 118.4 . . ? N9 C46 H46 118.4 . . ? N6 C31 N5 117.3(5) . . ? N6 C31 C30 38.5(3) . . ? N5 C31 C30 78.8(4) . . ? N6 C31 H31 121.4 . . ? N5 C31 H31 121.4 . . ? C30 C31 H31 159.9 . . ? C124 N23 N22 101.1(7) . . ? C65 C66 C67 118.5(5) . . ? C65 C66 H66 120.8 . . ? C67 C66 H66 120.8 . . ? C13 C14 C15 119.0(5) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C109 C111 C113 119.6(7) . . ? C109 C111 H111 120.2 . . ? C113 C111 H111 120.2 . . ? C97 C96 C95 119.1(6) . . ? C97 C96 H96 120.4 . . ? C95 C96 H96 120.4 . . ? N17 C93 N18 116.1(6) . . ? N17 C93 H93 121.9 . . ? N18 C93 H93 121.9 . . ? C106 C105 C104 118.2(6) . . ? C106 C105 H105 120.9 . . ? C104 C105 H105 120.9 . . ? C79 C81 C83 120.6(6) . . ? C79 C81 H81 119.7 . . ? C83 C81 H81 119.7 . . ? C122 C120 C118 118.7(8) . . ? C122 C120 H120 120.7 . . ? C118 C120 H120 120.7 . . ? C33 C34 C35 119.5(6) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C123 N24 C124 101.9(7) . . ? C4 C131 C5 119.5(6) . . ? C4 C131 H131 120.2 . . ? C5 C131 H131 120.2 . . ? C117 C118 C120 120.6(8) . . ? C117 C118 H118 119.7 . . ? C120 C118 H118 119.7 . . ? C78 C80 C82 121.5(6) . . ? C78 C80 H80 119.3 . . ? C82 C80 H80 119.3 . . ? C112 C110 C109 121.5(7) . . ? C112 C110 H110 119.3 . . ? C109 C110 H110 119.3 . . ? C112 C114 C113 118.0(7) . . ? C112 C114 C115 118.3(9) . . ? C113 C114 C115 123.6(9) . . ? C49 C51 C52 122.1(6) . . ? C49 C51 H51 118.9 . . ? C52 C51 H51 118.9 . . ? C50 C52 C51 117.1(5) . . ? C50 C52 C53 126.4(6) . . ? C51 C52 C53 116.5(6) . . ? C23 C22 C21 127.2(6) . . ? C23 C22 H22 116.4 . . ? C21 C22 H22 116.4 . . ? C29 C28 C26 120.3(6) . . ? C29 C28 H28 119.9 . . ? C26 C28 H28 119.9 . . ? C29 C27 C25 120.1(6) . . ? C29 C27 H27 119.9 . . ? C25 C27 H27 119.9 . . ? C86 C87 C89 121.2(6) . . ? C86 C87 H87 119.4 . . ? C89 C87 H87 119.4 . . ? C64 C65 C66 120.1(6) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C114 C113 C111 121.1(7) . . ? C114 C113 H113 119.5 . . ? C111 C113 H113 119.5 . . ? C65 C64 C63 118.7(6) . . ? C65 C64 H64 120.7 . . ? C63 C64 H64 120.7 . . ? N24 C123 N22 111.2(7) . . ? N24 C123 H123 124.4 . . ? N22 C123 H123 124.4 . . ? C91 C89 C87 120.0(6) . . ? C91 C89 H89 120.0 . . ? C87 C89 H89 120.0 . . ? C54 C53 C52 133.2(9) . . ? C54 C53 H53 113.4 . . ? C52 C53 H53 113.4 . . ? C16 C17 C19 121.6(6) . . ? C16 C17 H17 119.2 . . ? C19 C17 H17 119.2 . . ? C51 C49 C47 120.4(5) . . ? C51 C49 H49 119.8 . . ? C47 C49 H49 119.8 . . ? O17 Cl3 O10 110.0(10) . . ? O17 Cl3 O9 114.0(10) . . ? O10 Cl3 O9 105.8(6) . . ? O17 Cl3 O11 102.1(7) . . ? O10 Cl3 O11 118.1(9) . . ? O9 Cl3 O11 107.0(7) . . ? C21 C19 C17 120.8(6) . . ? C21 C19 H19 119.6 . . ? C17 C19 H19 119.6 . . ? C117 C119 C121 122.5(9) . . ? C117 C119 H119 118.8 . . ? C121 C119 H119 118.8 . . ? C122 C121 C119 120.4(8) . . ? C122 C121 H121 119.8 . . ? C119 C121 H121 119.8 . . ? O12 Cl4 O15 117.8(7) . . ? O12 Cl4 O13 105.9(8) . . ? O15 Cl4 O13 109.6(9) . . ? O12 Cl4 O14 97.5(12) . . ? O15 Cl4 O14 102.3(8) . . ? O13 Cl4 O14 124.2(13) . . ? C116 C115 C114 132.3(11) . . ? C116 C115 H115 113.8 . . ? C114 C115 H115 113.8 . . ? C115 C116 C117 137.0(12) . . ? C115 C116 H116 111.5 . . ? C117 C116 H116 111.5 . . ? 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 N11 C62 N12 C61 -0.4(9) . . . . ? N12 C62 N11 N10 0.8(8) . . . . ? C62 N12 C61 N10 -0.3(8) . . . . ? N12 C61 N10 N11 0.9(8) . . . . ? N12 C61 N10 C60 -178.9(6) . . . . ? C62 N11 N10 C61 -1.0(7) . . . . ? C62 N11 N10 C60 178.8(6) . . . . ? C57 C59 C60 C58 -1.4(10) . . . . ? C57 C59 C60 N10 177.6(5) . . . . ? C61 N10 C60 C58 -164.5(7) . . . . ? N11 N10 C60 C58 15.8(9) . . . . ? C61 N10 C60 C59 16.5(10) . . . . ? N11 N10 C60 C59 -163.2(6) . . . . ? C59 C60 C58 C56 -0.4(11) . . . . ? N10 C60 C58 C56 -179.2(6) . . . . ? C60 C59 C57 C55 1.5(10) . . . . ? C60 C58 C56 C55 2.1(12) . . . . ? C58 C56 C55 C57 -2.0(13) . . . . ? C58 C56 C55 C54 178.6(7) . . . . ? C59 C57 C55 C56 0.1(12) . . . . ? C59 C57 C55 C54 179.5(6) . . . . ? N8 Zn1 N3 C077 1.3(5) . . . . ? N2 Zn1 N3 C077 -178.6(5) . . . . ? N9 Zn1 N3 C077 77.3(4) . . . . ? N1 Zn1 N3 C077 -170.5(4) . . . . ? N7 Zn1 N3 C077 -75.2(4) . . . . ? N8 Zn1 N3 C12 -177.6(3) . . . . ? N2 Zn1 N3 C12 2.6(3) . . . . ? N9 Zn1 N3 C12 -101.5(3) . . . . ? N1 Zn1 N3 C12 10.7(5) . . . . ? N7 Zn1 N3 C12 105.9(3) . . . . ? N8 Zn1 N9 C42 3.7(3) . . . . ? N2 Zn1 N9 C42 -177.7(3) . . . . ? N1 Zn1 N9 C42 104.9(4) . . . . ? N3 Zn1 N9 C42 -102.3(4) . . . . ? N7 Zn1 N9 C42 5.7(6) . . . . ? N8 Zn1 N9 C46 175.8(5) . . . . ? N2 Zn1 N9 C46 -5.5(5) . . . . ? N1 Zn1 N9 C46 -82.9(4) . . . . ? N3 Zn1 N9 C46 69.8(4) . . . . ? N7 Zn1 N9 C46 177.9(4) . . . . ? N8 Zn1 N1 C3 -9.1(5) . . . . ? N2 Zn1 N1 C3 170.9(5) . . . . ? N9 Zn1 N1 C3 -86.8(5) . . . . ? N3 Zn1 N1 C3 162.8(4) . . . . ? N7 Zn1 N1 C3 64.7(5) . . . . ? N8 Zn1 N1 C6 -178.2(4) . . . . ? N2 Zn1 N1 C6 1.8(3) . . . . ? N9 Zn1 N1 C6 104.0(4) . . . . ? N3 Zn1 N1 C6 -6.3(6) . . . . ? N7 Zn1 N1 C6 -104.4(4) . . . . ? N8 Zn1 N2 C7 3(8) . . . . ? N9 Zn1 N2 C7 -93.2(4) . . . . ? N1 Zn1 N2 C7 2.9(3) . . . . ? N3 Zn1 N2 C7 178.8(4) . . . . ? N7 Zn1 N2 C7 85.1(4) . . . . ? N8 Zn1 N2 C11 -179(100) . . . . ? N9 Zn1 N2 C11 84.4(4) . . . . ? N1 Zn1 N2 C11 -179.5(4) . . . . ? N3 Zn1 N2 C11 -3.6(4) . . . . ? N7 Zn1 N2 C11 -97.3(4) . . . . ? N14 Zn2 N20 C99 -73(3) . . . . ? N19 Zn2 N20 C99 -178.2(4) . . . . ? N15 Zn2 N20 C99 89.7(4) . . . . ? N21 Zn2 N20 C99 3.7(4) . . . . ? N13 Zn2 N20 C99 -91.1(4) . . . . ? N14 Zn2 N20 C103 101(3) . . . . ? N19 Zn2 N20 C103 -4.3(4) . . . . ? N15 Zn2 N20 C103 -96.4(4) . . . . ? N21 Zn2 N20 C103 177.6(4) . . . . ? N13 Zn2 N20 C103 82.8(4) . . . . ? N20 Zn2 N15 C77 -2.4(5) . . . . ? N14 Zn2 N15 C77 176.5(5) . . . . ? N19 Zn2 N15 C77 -79.5(4) . . . . ? N21 Zn2 N15 C77 72.6(4) . . . . ? N13 Zn2 N15 C77 179.3(4) . . . . ? N20 Zn2 N15 C73 -177.3(3) . . . . ? N14 Zn2 N15 C73 1.7(3) . . . . ? N19 Zn2 N15 C73 105.7(4) . . . . ? N21 Zn2 N15 C73 -102.3(4) . . . . ? N13 Zn2 N15 C73 4.4(6) . . . . ? N2 Zn1 N8 C41 -95(7) . . . . ? N9 Zn1 N8 C41 1.3(4) . . . . ? N1 Zn1 N8 C41 -95.1(4) . . . . ? N3 Zn1 N8 C41 89.0(4) . . . . ? N7 Zn1 N8 C41 -177.7(4) . . . . ? N2 Zn1 N8 C37 79(7) . . . . ? N9 Zn1 N8 C37 175.3(4) . . . . ? N1 Zn1 N8 C37 78.9(4) . . . . ? N3 Zn1 N8 C37 -97.0(4) . . . . ? N7 Zn1 N8 C37 -3.7(4) . . . . ? N8 Zn1 N7 C36 0.9(3) . . . . ? N2 Zn1 N7 C36 -177.7(4) . . . . ? N9 Zn1 N7 C36 -1.1(6) . . . . ? N1 Zn1 N7 C36 -103.5(4) . . . . ? N3 Zn1 N7 C36 105.6(4) . . . . ? N8 Zn1 N7 C32 179.7(5) . . . . ? N2 Zn1 N7 C32 1.0(5) . . . . ? N9 Zn1 N7 C32 177.7(4) . . . . ? N1 Zn1 N7 C32 75.2(4) . . . . ? N3 Zn1 N7 C32 -75.7(4) . . . . ? N20 Zn2 N21 C94 176.2(5) . . . . ? N14 Zn2 N21 C94 -7.2(5) . . . . ? N19 Zn2 N21 C94 172.3(4) . . . . ? N15 Zn2 N21 C94 68.4(4) . . . . ? N13 Zn2 N21 C94 -83.9(4) . . . . ? N20 Zn2 N21 C98 0.9(3) . . . . ? N14 Zn2 N21 C98 177.6(3) . . . . ? N19 Zn2 N21 C98 -2.9(6) . . . . ? N15 Zn2 N21 C98 -106.8(4) . . . . ? N13 Zn2 N21 C98 100.9(4) . . . . ? N20 Zn2 N19 C104 2.9(4) . . . . ? N14 Zn2 N19 C104 -173.7(4) . . . . ? N15 Zn2 N19 C104 109.3(4) . . . . ? N21 Zn2 N19 C104 6.7(6) . . . . ? N13 Zn2 N19 C104 -98.9(4) . . . . ? N20 Zn2 N19 C108 -178.8(5) . . . . ? N14 Zn2 N19 C108 4.6(5) . . . . ? N15 Zn2 N19 C108 -72.4(4) . . . . ? N21 Zn2 N19 C108 -174.9(4) . . . . ? N13 Zn2 N19 C108 79.4(4) . . . . ? N20 Zn2 N13 C67 177.7(4) . . . . ? N14 Zn2 N13 C67 -1.2(4) . . . . ? N19 Zn2 N13 C67 -106.8(4) . . . . ? N15 Zn2 N13 C67 -4.0(6) . . . . ? N21 Zn2 N13 C67 101.0(4) . . . . ? N20 Zn2 N13 C63 -3.6(5) . . . . ? N14 Zn2 N13 C63 177.5(5) . . . . ? N19 Zn2 N13 C63 71.9(5) . . . . ? N15 Zn2 N13 C63 174.7(4) . . . . ? N21 Zn2 N13 C63 -80.3(5) . . . . ? N20 Zn2 N14 C68 -17(3) . . . . ? N19 Zn2 N14 C68 87.3(4) . . . . ? N15 Zn2 N14 C68 179.9(4) . . . . ? N21 Zn2 N14 C68 -93.0(4) . . . . ? N13 Zn2 N14 C68 1.3(4) . . . . ? N20 Zn2 N14 C72 163(3) . . . . ? N19 Zn2 N14 C72 -92.8(4) . . . . ? N15 Zn2 N14 C72 -0.1(4) . . . . ? N21 Zn2 N14 C72 87.0(4) . . . . ? N13 Zn2 N14 C72 -178.7(4) . . . . ? C92 N16 N17 C93 -1.3(7) . . . . ? C91 N16 N17 C93 179.0(5) . . . . ? C46 N9 C42 C43 -0.8(8) . . . . ? Zn1 N9 C42 C43 172.2(4) . . . . ? C46 N9 C42 C41 179.6(4) . . . . ? Zn1 N9 C42 C41 -7.5(5) . . . . ? C077 N3 C12 C13 -0.1(8) . . . . ? Zn1 N3 C12 C13 178.9(4) . . . . ? C077 N3 C12 C11 179.7(5) . . . . ? Zn1 N3 C12 C11 -1.4(5) . . . . ? C80 C78 C70 C69 -162.2(6) . . . . ? C79 C78 C70 C69 17.1(8) . . . . ? C80 C78 C70 C71 18.5(8) . . . . ? C79 C78 C70 C71 -162.2(5) . . . . ? C68 N14 C72 C71 -0.6(7) . . . . ? Zn2 N14 C72 C71 179.4(4) . . . . ? C68 N14 C72 C73 178.6(4) . . . . ? Zn2 N14 C72 C73 -1.4(6) . . . . ? C41 N8 C37 C38 -1.7(7) . . . . ? Zn1 N8 C37 C38 -175.6(4) . . . . ? C41 N8 C37 C36 179.5(4) . . . . ? Zn1 N8 C37 C36 5.5(6) . . . . ? C39 C38 C37 N8 1.0(8) . . . . ? C39 C38 C37 C36 179.8(5) . . . . ? C92 N16 C91 C89 167.5(6) . . . . ? N17 N16 C91 C89 -12.8(8) . . . . ? C92 N16 C91 C90 -11.8(9) . . . . ? N17 N16 C91 C90 167.9(5) . . . . ? C37 N8 C41 C40 1.6(7) . . . . ? Zn1 N8 C41 C40 175.7(4) . . . . ? C37 N8 C41 C42 -179.6(4) . . . . ? Zn1 N8 C41 C42 -5.6(6) . . . . ? N9 C42 C41 N8 8.5(6) . . . . ? C43 C42 C41 N8 -171.1(5) . . . . ? N9 C42 C41 C40 -172.7(5) . . . . ? C43 C42 C41 C40 7.6(8) . . . . ? N8 C41 C40 C39 -1.0(8) . . . . ? C42 C41 C40 C39 -179.6(5) . . . . ? C71 C70 C69 C68 0.6(8) . . . . ? C78 C70 C69 C68 -178.7(5) . . . . ? C41 C40 C39 C38 0.4(8) . . . . ? C41 C40 C39 C47 178.9(5) . . . . ? C37 C38 C39 C40 -0.4(8) . . . . ? C37 C38 C39 C47 -178.9(5) . . . . ? C48 C47 C39 C40 141.8(6) . . . . ? C49 C47 C39 C40 -41.0(8) . . . . ? C48 C47 C39 C38 -39.7(9) . . . . ? C49 C47 C39 C38 137.5(6) . . . . ? C108 N19 C104 C105 2.2(8) . . . . ? Zn2 N19 C104 C105 -179.4(5) . . . . ? C108 N19 C104 C103 -179.8(5) . . . . ? Zn2 N19 C104 C103 -1.3(6) . . . . ? C3 N1 C6 C5 0.5(8) . . . . ? Zn1 N1 C6 C5 170.4(4) . . . . ? C3 N1 C6 C7 -175.6(5) . . . . ? Zn1 N1 C6 C7 -5.7(6) . . . . ? C131 C5 C6 N1 -0.5(8) . . . . ? C131 C5 C6 C7 175.4(5) . . . . ? C30 N4 N5 C31 -0.1(7) . . . . ? C29 N4 N5 C31 178.7(5) . . . . ? N14 C72 C71 C70 0.8(8) . . . . ? C73 C72 C71 C70 -178.3(5) . . . . ? C69 C70 C71 C72 -0.8(8) . . . . ? C78 C70 C71 C72 178.5(5) . . . . ? C84 C85 C86 C87 176.4(7) . . . . ? C84 C85 C86 C88 -0.5(11) . . . . ? C7 N2 C11 C10 2.2(7) . . . . ? Zn1 N2 C11 C10 -175.4(4) . . . . ? C7 N2 C11 C12 -178.5(4) . . . . ? Zn1 N2 C11 C12 3.9(6) . . . . ? C9 C10 C11 N2 0.8(8) . . . . ? C9 C10 C11 C12 -178.5(5) . . . . ? N3 C12 C11 N2 -1.5(6) . . . . ? C13 C12 C11 N2 178.3(5) . . . . ? N3 C12 C11 C10 177.8(5) . . . . ? C13 C12 C11 C10 -2.4(8) . . . . ? C7 C8 C9 C10 -0.2(8) . . . . ? C7 C8 C9 C16 179.0(5) . . . . ? C11 C10 C9 C8 -1.7(7) . . . . ? C11 C10 C9 C16 179.1(5) . . . . ? C17 C16 C9 C8 160.4(7) . . . . ? C18 C16 C9 C8 -20.1(8) . . . . ? C17 C16 C9 C10 -20.4(9) . . . . ? C18 C16 C9 C10 159.0(6) . . . . ? C32 N7 C36 C35 2.5(8) . . . . ? Zn1 N7 C36 C35 -178.7(4) . . . . ? C32 N7 C36 C37 -177.3(5) . . . . ? Zn1 N7 C36 C37 1.5(6) . . . . ? N8 C37 C36 N7 -4.4(7) . . . . ? C38 C37 C36 N7 176.8(5) . . . . ? N8 C37 C36 C35 175.8(5) . . . . ? C38 C37 C36 C35 -3.0(8) . . . . ? C56 C55 C54 C53 174.7(9) . . . . ? C57 C55 C54 C53 -4.7(13) . . . . ? C25 C24 C23 C22 1.5(11) . . . . ? C26 C24 C23 C22 -179.4(7) . . . . ? C11 N2 C7 C8 -4.2(7) . . . . ? Zn1 N2 C7 C8 173.4(4) . . . . ? C11 N2 C7 C6 175.7(4) . . . . ? Zn1 N2 C7 C6 -6.7(6) . . . . ? C9 C8 C7 N2 3.2(8) . . . . ? C9 C8 C7 C6 -176.7(5) . . . . ? N1 C6 C7 N2 8.1(7) . . . . ? C5 C6 C7 N2 -168.0(5) . . . . ? N1 C6 C7 C8 -172.1(5) . . . . ? C5 C6 C7 C8 11.9(8) . . . . ? C72 N14 C68 C69 0.3(7) . . . . ? Zn2 N14 C68 C69 -179.7(4) . . . . ? C72 N14 C68 C67 178.8(5) . . . . ? Zn2 N14 C68 C67 -1.2(6) . . . . ? C70 C69 C68 N14 -0.4(8) . . . . ? C70 C69 C68 C67 -178.7(5) . . . . ? C30 N4 C29 C28 -169.2(7) . . . . ? N5 N4 C29 C28 12.3(8) . . . . ? C30 N4 C29 C27 9.5(9) . . . . ? N5 N4 C29 C27 -169.0(6) . . . . ? C36 N7 C32 C33 -1.4(9) . . . . ? Zn1 N7 C32 C33 179.9(4) . . . . ? C34 C33 C32 N7 -0.1(10) . . . . ? C87 C86 C88 C90 0.1(10) . . . . ? C85 C86 C88 C90 177.1(6) . . . . ? N3 C12 C13 C14 1.1(8) . . . . ? C11 C12 C13 C14 -178.6(5) . . . . ? C12 N3 C077 C15 -1.4(8) . . . . ? Zn1 N3 C077 C15 179.8(4) . . . . ? C81 C83 C82 C80 -1.6(9) . . . . ? C84 C83 C82 C80 179.0(6) . . . . ? C26 C24 C25 C27 -1.9(10) . . . . ? C23 C24 C25 C27 177.2(6) . . . . ? C73 N15 C77 C76 -0.9(8) . . . . ? Zn2 N15 C77 C76 -175.6(4) . . . . ? C98 N21 C94 C95 0.5(8) . . . . ? Zn2 N21 C94 C95 -174.6(4) . . . . ? C77 N15 C73 C74 0.9(8) . . . . ? Zn2 N15 C73 C74 176.1(4) . . . . ? C77 N15 C73 C72 -178.1(5) . . . . ? Zn2 N15 C73 C72 -2.9(5) . . . . ? C75 C74 C73 N15 -1.0(8) . . . . ? C75 C74 C73 C72 177.9(5) . . . . ? N14 C72 C73 N15 2.8(6) . . . . ? C71 C72 C73 N15 -178.0(5) . . . . ? N14 C72 C73 C74 -176.2(5) . . . . ? C71 C72 C73 C74 3.0(8) . . . . ? C94 N21 C98 C97 0.2(8) . . . . ? Zn2 N21 C98 C97 175.8(4) . . . . ? C94 N21 C98 C99 179.6(4) . . . . ? Zn2 N21 C98 C99 -4.8(6) . . . . ? C99 N20 C103 C102 0.3(7) . . . . ? Zn2 N20 C103 C102 -173.6(4) . . . . ? C99 N20 C103 C104 178.8(4) . . . . ? Zn2 N20 C103 C104 4.9(6) . . . . ? C101 C102 C103 N20 -0.7(8) . . . . ? C101 C102 C103 C104 -179.0(5) . . . . ? N19 C104 C103 N20 -2.1(7) . . . . ? C105 C104 C103 N20 175.9(5) . . . . ? N19 C104 C103 C102 176.3(5) . . . . ? C105 C104 C103 C102 -5.7(9) . . . . ? N7 C36 C35 C34 -2.0(9) . . . . ? C37 C36 C35 C34 177.8(6) . . . . ? C63 N13 C67 C66 -0.4(8) . . . . ? Zn2 N13 C67 C66 178.4(5) . . . . ? C63 N13 C67 C68 -177.8(5) . . . . ? Zn2 N13 C67 C68 1.0(6) . . . . ? N14 C68 C67 N13 0.0(7) . . . . ? C69 C68 C67 N13 178.5(5) . . . . ? N14 C68 C67 C66 -177.3(5) . . . . ? C69 C68 C67 C66 1.2(9) . . . . ? C103 C102 C101 C100 0.6(8) . . . . ? C103 C102 C101 C109 178.1(5) . . . . ? C99 C100 C101 C102 0.0(8) . . . . ? C99 C100 C101 C109 -177.6(5) . . . . ? C110 C109 C101 C102 140.6(6) . . . . ? C111 C109 C101 C102 -37.7(9) . . . . ? C110 C109 C101 C100 -42.0(9) . . . . ? C111 C109 C101 C100 139.7(6) . . . . ? C86 C85 C84 C83 179.8(6) . . . . ? C82 C83 C84 C85 -177.0(7) . . . . ? C81 C83 C84 C85 3.7(10) . . . . ? C103 N20 C99 C100 0.2(8) . . . . ? Zn2 N20 C99 C100 174.1(4) . . . . ? C103 N20 C99 C98 178.8(4) . . . . ? Zn2 N20 C99 C98 -7.3(6) . . . . ? C101 C100 C99 N20 -0.4(8) . . . . ? C101 C100 C99 C98 -178.8(5) . . . . ? N21 C98 C99 N20 7.7(7) . . . . ? C97 C98 C99 N20 -172.9(5) . . . . ? N21 C98 C99 C100 -173.7(5) . . . . ? C97 C98 C99 C100 5.6(9) . . . . ? C18 C20 C21 C19 -1.0(11) . . . . ? C18 C20 C21 C22 -179.7(6) . . . . ? C104 N19 C108 C107 -2.8(8) . . . . ? Zn2 N19 C108 C107 178.9(4) . . . . ? C106 C107 C108 N19 2.3(10) . . . . ? C49 C47 C48 C50 0.6(10) . . . . ? C39 C47 C48 C50 177.9(6) . . . . ? C52 C50 C48 C47 0.7(10) . . . . ? C86 C88 C90 C91 0.3(9) . . . . ? C89 C91 C90 C88 0.0(9) . . . . ? N16 C91 C90 C88 179.3(5) . . . . ? C67 N13 C63 C64 1.2(9) . . . . ? Zn2 N13 C63 C64 -177.4(5) . . . . ? C120 C122 N22 C123 150.3(8) . . . . ? C121 C122 N22 C123 -29.7(11) . . . . ? C120 C122 N22 N23 -28.1(10) . . . . ? C121 C122 N22 N23 152.0(7) . . . . ? N21 C94 C95 C96 -1.0(9) . . . . ? C108 C107 C106 C105 -1.1(10) . . . . ? N15 C77 C76 C75 1.0(9) . . . . ? C80 C78 C79 C81 -2.8(9) . . . . ? C70 C78 C79 C81 177.8(5) . . . . ? C6 N1 C3 C4 -0.1(9) . . . . ? Zn1 N1 C3 C4 -168.8(5) . . . . ? C131 C4 C3 N1 -0.4(10) . . . . ? N21 C98 C97 C96 -0.4(9) . . . . ? C99 C98 C97 C96 -179.6(5) . . . . ? C73 C74 C75 C76 1.1(9) . . . . ? C77 C76 C75 C74 -1.0(9) . . . . ? C31 N6 C30 N4 0.4(8) . . . . ? N5 N4 C30 N6 -0.2(8) . . . . ? C29 N4 C30 N6 -178.9(5) . . . . ? N5 N4 C30 C31 0.0(4) . . . . ? C29 N4 C30 C31 -178.6(6) . . . . ? N3 C077 C15 C14 1.8(9) . . . . ? N9 C42 C43 C44 0.1(8) . . . . ? C41 C42 C43 C44 179.7(5) . . . . ? C21 C20 C18 C16 1.0(10) . . . . ? C17 C16 C18 C20 -0.8(10) . . . . ? C9 C16 C18 C20 179.7(6) . . . . ? C93 N18 C92 N16 -0.6(7) . . . . ? N17 N16 C92 N18 1.2(7) . . . . ? C91 N16 C92 N18 -179.1(5) . . . . ? C42 C43 C44 C45 1.4(9) . . . . ? C46 C45 C44 C43 -2.1(9) . . . . ? C25 C24 C26 C28 1.8(10) . . . . ? C23 C24 C26 C28 -177.3(6) . . . . ? C44 C45 C46 N9 1.4(9) . . . . ? C42 N9 C46 C45 0.0(8) . . . . ? Zn1 N9 C46 C45 -172.0(4) . . . . ? C30 N6 C31 N5 -0.5(8) . . . . ? N4 N5 C31 N6 0.4(8) . . . . ? N4 N5 C31 C30 0.0(4) . . . . ? N4 C30 C31 N6 -179.6(7) . . . . ? N6 C30 C31 N5 179.6(8) . . . . ? N4 C30 C31 N5 0.0(4) . . . . ? N24 C124 N23 N22 -0.3(10) . . . . ? C123 N22 N23 C124 2.0(8) . . . . ? C122 N22 N23 C124 -179.4(6) . . . . ? N13 C67 C66 C65 0.0(9) . . . . ? C68 C67 C66 C65 177.1(6) . . . . ? C12 C13 C14 C15 -0.6(9) . . . . ? C077 C15 C14 C13 -0.8(9) . . . . ? C110 C109 C111 C113 1.7(10) . . . . ? C101 C109 C111 C113 -179.9(6) . . . . ? C98 C97 C96 C95 -0.2(9) . . . . ? C94 C95 C96 C97 0.9(9) . . . . ? N16 N17 C93 N18 1.0(8) . . . . ? C92 N18 C93 N17 -0.3(8) . . . . ? C107 C106 C105 C104 0.5(11) . . . . ? N19 C104 C105 C106 -1.0(9) . . . . ? C103 C104 C105 C106 -178.9(6) . . . . ? C78 C79 C81 C83 1.1(9) . . . . ? C82 C83 C81 C79 1.1(9) . . . . ? C84 C83 C81 C79 -179.5(5) . . . . ? C121 C122 C120 C118 1.6(11) . . . . ? N22 C122 C120 C118 -178.4(6) . . . . ? C32 C33 C34 C35 0.6(10) . . . . ? C36 C35 C34 C33 0.4(10) . . . . ? N23 C124 N24 C123 -1.5(10) . . . . ? C3 C4 C131 C5 0.4(10) . . . . ? C6 C5 C131 C4 0.0(9) . . . . ? C119 C117 C118 C120 0.2(12) . . . . ? C116 C117 C118 C120 -177.0(8) . . . . ? C122 C120 C118 C117 -1.7(11) . . . . ? C79 C78 C80 C82 2.4(9) . . . . ? C70 C78 C80 C82 -178.3(5) . . . . ? C83 C82 C80 C78 -0.2(9) . . . . ? C114 C112 C110 C109 0.0(12) . . . . ? C111 C109 C110 C112 -1.3(10) . . . . ? C101 C109 C110 C112 -179.7(7) . . . . ? C110 C112 C114 C113 0.9(13) . . . . ? C110 C112 C114 C115 -176.9(7) . . . . ? C48 C50 C52 C51 -2.5(10) . . . . ? C48 C50 C52 C53 177.1(6) . . . . ? C49 C51 C52 C50 3.1(11) . . . . ? C49 C51 C52 C53 -176.5(7) . . . . ? C24 C23 C22 C21 179.3(6) . . . . ? C20 C21 C22 C23 10.2(12) . . . . ? C19 C21 C22 C23 -168.5(8) . . . . ? C27 C29 C28 C26 0.8(10) . . . . ? N4 C29 C28 C26 179.5(6) . . . . ? C24 C26 C28 C29 -1.3(11) . . . . ? C28 C29 C27 C25 -0.9(10) . . . . ? N4 C29 C27 C25 -179.6(6) . . . . ? C24 C25 C27 C29 1.5(11) . . . . ? C88 C86 C87 C89 -0.7(10) . . . . ? C85 C86 C87 C89 -177.7(6) . . . . ? C67 C66 C65 C64 -0.3(10) . . . . ? C112 C114 C113 C111 -0.4(12) . . . . ? C115 C114 C113 C111 177.3(7) . . . . ? C109 C111 C113 C114 -0.9(11) . . . . ? C66 C65 C64 C63 1.1(10) . . . . ? N13 C63 C64 C65 -1.6(10) . . . . ? C124 N24 C123 N22 2.7(9) . . . . ? N23 N22 C123 N24 -3.1(9) . . . . ? C122 N22 C123 N24 178.4(6) . . . . ? C90 C91 C89 C87 -0.6(9) . . . . ? N16 C91 C89 C87 -179.9(5) . . . . ? C86 C87 C89 C91 1.0(10) . . . . ? C55 C54 C53 C52 -177.7(7) . . . . ? C50 C52 C53 C54 -10.9(14) . . . . ? C51 C52 C53 C54 168.7(9) . . . . ? C18 C16 C17 C19 0.6(12) . . . . ? C9 C16 C17 C19 -179.9(7) . . . . ? C52 C51 C49 C47 -1.8(11) . . . . ? C48 C47 C49 C51 -0.1(10) . . . . ? C39 C47 C49 C51 -177.4(6) . . . . ? C20 C21 C19 C17 0.8(12) . . . . ? C22 C21 C19 C17 179.6(8) . . . . ? C16 C17 C19 C21 -0.6(14) . . . . ? C118 C117 C119 C121 1.5(13) . . . . ? C116 C117 C119 C121 178.9(8) . . . . ? C120 C122 C121 C119 0.1(12) . . . . ? N22 C122 C121 C119 -180.0(7) . . . . ? C117 C119 C121 C122 -1.7(13) . . . . ? C112 C114 C115 C116 162.1(11) . . . . ? C113 C114 C115 C116 -15.6(15) . . . . ? C114 C115 C116 C117 -176.7(8) . . . . ? C119 C117 C116 C115 166.7(11) . . . . ? C118 C117 C116 C115 -16.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.319 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.107 data_wpp1 _database_code_depnum_ccdc_archive 'CCDC 843213' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H46 Cd2 Cl2 I4 N12' _chemical_formula_sum 'C63 H46 Cd2 Cl2 I4 N12' _chemical_formula_weight 1774.42 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' Cl Cl 0.1484 0.1585 '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' I I -0.4742 1.8119 '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 16.3236(3) _cell_length_b 26.8610(5) _cell_length_c 15.7429(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.5660(10) _cell_angle_gamma 90.00 _cell_volume 6226.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 22.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3400 _exptl_absorpt_coefficient_mu 2.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4869 _exptl_absorpt_correction_T_max 0.6041 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51489 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11026 _reflns_number_gt 7381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR92 _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1000P)^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 11026 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.006 _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 0.60240(4) 0.360677(19) 0.51494(4) 0.05594(17) Uani 1 1 d . . . Cd2 Cd 0.83976(4) 0.09615(2) 0.53398(4) 0.05786(18) Uani 1 1 d . . . I3 I 0.78917(4) 0.07819(2) 0.67697(4) 0.07220(19) Uani 1 1 d . . . I2 I 0.64562(4) 0.37179(2) 0.36418(4) 0.0771(2) Uani 1 1 d . . . I1 I 0.44761(4) 0.41044(2) 0.49011(4) 0.0824(2) Uani 1 1 d . . . I4 I 1.01020(4) 0.08251(2) 0.54516(5) 0.0879(2) Uani 1 1 d . . . C24 C 1.2478(5) 0.0885(3) 1.1487(5) 0.0527(17) Uani 1 1 d . . . Cl2 Cl 0.1534(3) 0.3378(3) 0.3347(3) 0.218(2) Uani 1 1 d . . . C56 C 0.1990(6) 0.4146(3) -0.1131(6) 0.092(3) Uani 1 1 d . . . H56 H 0.2488 0.4319 -0.0698 0.111 Uiso 1 1 calc R . . N2 N 0.7101(3) 0.31852(19) 0.6449(3) 0.0430(13) Uani 1 1 d . . . N1 N 0.5648(4) 0.2747(2) 0.5105(4) 0.0503(14) Uani 1 1 d . . . C55 C 0.1924(5) 0.3648(3) -0.0992(5) 0.0578(19) Uani 1 1 d . . . N7 N 0.8567(4) 0.1832(2) 0.5580(4) 0.0510(14) Uani 1 1 d . . . N8 N 0.7262(4) 0.1378(2) 0.4096(4) 0.0471(13) Uani 1 1 d . . . N3 N 0.7138(4) 0.4164(2) 0.6192(4) 0.0561(15) Uani 1 1 d . . . C8 C 0.8480(4) 0.2661(2) 0.7899(4) 0.0455(16) Uani 1 1 d . . . C40 C 0.6453(4) 0.2128(3) 0.3515(4) 0.0502(17) Uani 1 1 d . . . H40 H 0.6421 0.2472 0.3561 0.060 Uiso 1 1 calc R . . N9 N 0.7514(4) 0.0407(2) 0.4108(4) 0.0555(15) Uani 1 1 d . . . N5 N 1.5365(4) 0.0324(2) 1.4244(4) 0.0615(16) Uani 1 1 d . . . C39 C 0.5738(4) 0.1866(3) 0.2785(4) 0.0459(16) Uani 1 1 d . . . C29 C 1.3945(5) 0.0356(3) 1.2831(5) 0.0542(17) Uani 1 1 d . . . N4 N 1.4676(4) 0.0082(2) 1.3521(4) 0.0563(15) Uani 1 1 d . . . C47 C 0.4936(4) 0.2145(3) 0.2090(4) 0.0470(16) Uani 1 1 d . . . C6 C 0.7061(4) 0.2683(2) 0.6511(4) 0.0416(15) Uani 1 1 d . . . C17 C 0.9928(5) 0.2644(3) 0.9395(5) 0.0552(18) Uani 1 1 d . . . H17 H 0.9909 0.2989 0.9431 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.2494(4) 0.2883(3) 0.2517(4) 0.318(5) Uani 1 1 d . . . N10 N 0.0022(4) 0.4406(2) -0.3396(4) 0.0658(17) Uani 1 1 d . . . C52 C 0.3452(5) 0.2671(3) 0.0743(5) 0.0568(18) Uani 1 1 d . . . C20 C 0.9990(5) 0.1614(3) 0.9317(5) 0.063(2) Uani 1 1 d . . . H20 H 0.9992 0.1269 0.9282 0.076 Uiso 1 1 calc R . . C2 C 0.4732(5) 0.2049(3) 0.4351(5) 0.064(2) Uani 1 1 d . . . H2 H 0.4198 0.1925 0.3878 0.077 Uiso 1 1 calc R . . C37 C 0.6613(4) 0.1123(3) 0.3403(4) 0.0486(16) Uani 1 1 d . . . C12 C 0.8476(5) 0.4297(3) 0.7578(5) 0.063(2) Uani 1 1 d . . . H12 H 0.8939 0.4168 0.8122 0.075 Uiso 1 1 calc R . . C18 C 0.9288(5) 0.1884(3) 0.8634(5) 0.0595(19) Uani 1 1 d . . . H18 H 0.8833 0.1711 0.8146 0.071 Uiso 1 1 calc R . . N6 N 1.5592(5) -0.0501(3) 1.4369(5) 0.0756(19) Uani 1 1 d . . . C16 C 0.9235(4) 0.2387(2) 0.8646(4) 0.0453(16) Uani 1 1 d . . . C45 C 0.9416(5) 0.2528(3) 0.6377(5) 0.0596(19) Uani 1 1 d . . . H45 H 0.9926 0.2656 0.6878 0.071 Uiso 1 1 calc R . . C9 C 0.8499(4) 0.3184(2) 0.7819(4) 0.0480(16) Uani 1 1 d . . . H9 H 0.8982 0.3364 0.8261 0.058 Uiso 1 1 calc R . . C7 C 0.7732(4) 0.2423(2) 0.7232(4) 0.0468(16) Uani 1 1 d . . . H7 H 0.7678 0.2080 0.7269 0.056 Uiso 1 1 calc R . . C41 C 0.7185(4) 0.1875(3) 0.4146(4) 0.0479(16) Uani 1 1 d . . . C5 C 0.6249(4) 0.2442(2) 0.5750(4) 0.0425(15) Uani 1 1 d . . . C46 C 0.9271(5) 0.2036(3) 0.6287(5) 0.0601(19) Uani 1 1 d . . . H46 H 0.9683 0.1828 0.6743 0.072 Uiso 1 1 calc R . . C35 C 0.6213(6) 0.0271(3) 0.2680(5) 0.066(2) Uani 1 1 d . . . H35 H 0.5703 0.0400 0.2182 0.079 Uiso 1 1 calc R . . C10 C 0.7811(4) 0.3431(2) 0.7093(5) 0.0462(16) Uani 1 1 d . . . C51 C 0.3449(5) 0.2158(3) 0.0789(5) 0.066(2) Uani 1 1 d . . . H51 H 0.2952 0.1984 0.0353 0.079 Uiso 1 1 calc R . . C42 C 0.7961(4) 0.2135(3) 0.4933(4) 0.0470(16) Uani 1 1 d . . . C36 C 0.6767(5) 0.0576(3) 0.3380(5) 0.0508(17) Uani 1 1 d . . . C26 C 1.2736(6) 0.0415(3) 1.1298(5) 0.079(3) Uani 1 1 d . . . H26 H 1.2404 0.0272 1.0711 0.095 Uiso 1 1 calc R . . C25 C 1.2998(6) 0.1070(3) 1.2390(5) 0.078(2) Uani 1 1 d . . . H25 H 1.2848 0.1377 1.2558 0.094 Uiso 1 1 calc R . . C19 C 1.0630(5) 0.2381(3) 1.0071(5) 0.0569(19) Uani 1 1 d . . . H19 H 1.1083 0.2554 1.0559 0.068 Uiso 1 1 calc R . . C43 C 0.8059(5) 0.2634(3) 0.4983(5) 0.0523(17) Uani 1 1 d . . . H43 H 0.7630 0.2836 0.4528 0.063 Uiso 1 1 calc R . . C21 C 1.0688(5) 0.1859(3) 1.0051(4) 0.0554(18) Uani 1 1 d . . . C1 C 0.4916(5) 0.2550(3) 0.4425(5) 0.062(2) Uani 1 1 d . . . H1 H 0.4506 0.2762 0.3974 0.075 Uiso 1 1 calc R . . N11 N -0.0649(5) 0.4152(3) -0.4079(5) 0.076(2) Uani 1 1 d . . . C54 C 0.2635(5) 0.3402(3) -0.0215(5) 0.0612(19) Uani 1 1 d . . . H54 H 0.3105 0.3601 0.0195 0.073 Uiso 1 1 calc R . . C59 C 0.0536(5) 0.3661(3) -0.2450(6) 0.082(3) Uani 1 1 d . . . H59 H 0.0039 0.3490 -0.2888 0.098 Uiso 1 1 calc R . . C23 C 1.1701(5) 0.1139(3) 1.0776(5) 0.0593(19) Uani 1 1 d . . . H23 H 1.1337 0.0952 1.0249 0.071 Uiso 1 1 calc R . . C15 C 0.7118(6) 0.4643(3) 0.5996(5) 0.065(2) Uani 1 1 d . . . H15 H 0.6651 0.4763 0.5446 0.078 Uiso 1 1 calc R . . C50 C 0.4222(6) 0.2915(3) 0.1370(6) 0.078(2) Uani 1 1 d . . . H50 H 0.4255 0.3260 0.1342 0.093 Uiso 1 1 calc R . . C60 C 0.0639(5) 0.4154(3) -0.2581(5) 0.0548(18) Uani 1 1 d . . . C14 C 0.7769(7) 0.4972(3) 0.6581(6) 0.076(2) Uani 1 1 d . . . H14 H 0.7744 0.5308 0.6430 0.091 Uiso 1 1 calc R . . C22 C 1.1453(5) 0.1604(3) 1.0792(5) 0.0555(18) Uani 1 1 d . . . H22 H 1.1800 0.1788 1.1328 0.067 Uiso 1 1 calc R . . C44 C 0.8802(5) 0.2845(3) 0.5716(5) 0.0572(18) Uani 1 1 d . . . H44 H 0.8885 0.3188 0.5763 0.069 Uiso 1 1 calc R . . N12 N -0.0705(5) 0.4960(3) -0.4461(6) 0.095(2) Uani 1 1 d . . . C11 C 0.7808(4) 0.3984(2) 0.6955(5) 0.0461(16) Uani 1 1 d . . . C53 C 0.2689(5) 0.2930(3) -0.0026(5) 0.067(2) Uani 1 1 d . . . H53 H 0.2199 0.2734 -0.0411 0.080 Uiso 1 1 calc R . . C49 C 0.4168(5) 0.1891(3) 0.1468(5) 0.064(2) Uani 1 1 d . . . H49 H 0.4133 0.1547 0.1505 0.077 Uiso 1 1 calc R . . C3 C 0.5349(5) 0.1740(3) 0.4988(6) 0.072(2) Uani 1 1 d . . . H3 H 0.5253 0.1398 0.4947 0.086 Uiso 1 1 calc R . . C4 C 0.6114(5) 0.1935(3) 0.5691(5) 0.065(2) Uani 1 1 d . . . H4 H 0.6543 0.1726 0.6129 0.078 Uiso 1 1 calc R . . C63 C 0.2139(10) 0.3465(5) 0.2797(10) 0.163(6) Uani 1 1 d . . . H63A H 0.2668 0.3662 0.3183 0.195 Uiso 1 1 calc R . . H63B H 0.1792 0.3649 0.2222 0.195 Uiso 1 1 calc R . . C13 C 0.8449(6) 0.4791(3) 0.7388(6) 0.067(2) Uani 1 1 d . . . H13 H 0.8889 0.5004 0.7803 0.080 Uiso 1 1 calc R . . C48 C 0.4946(5) 0.2654(3) 0.2041(5) 0.074(2) Uani 1 1 d . . . H48 H 0.5448 0.2828 0.2465 0.089 Uiso 1 1 calc R . . C27 C 1.3729(6) 0.0812(3) 1.3041(6) 0.080(3) Uani 1 1 d . . . H27 H 1.4076 0.0951 1.3628 0.096 Uiso 1 1 calc R . . C28 C 1.3457(6) 0.0164(3) 1.1947(6) 0.078(3) Uani 1 1 d . . . H28 H 1.3621 -0.0142 1.1790 0.093 Uiso 1 1 calc R . . C30 C 1.5879(5) -0.0060(4) 1.4691(6) 0.071(2) Uani 1 1 d . . . H30 H 1.6427 -0.0014 1.5219 0.085 Uiso 1 1 calc R . . C31 C 1.4828(5) -0.0405(3) 1.3609(6) 0.072(2) Uani 1 1 d . . . H31 H 1.4453 -0.0644 1.3198 0.086 Uiso 1 1 calc R . . C38 C 0.5839(4) 0.1363(3) 0.2727(5) 0.0498(17) Uani 1 1 d . . . H38 H 0.5397 0.1180 0.2244 0.060 Uiso 1 1 calc R . . C33 C 0.7165(6) -0.0408(3) 0.3457(6) 0.075(2) Uani 1 1 d . . . H33 H 0.7312 -0.0745 0.3500 0.090 Uiso 1 1 calc R . . C34 C 0.6408(6) -0.0233(3) 0.2710(6) 0.073(2) Uani 1 1 d . . . H34 H 0.6035 -0.0446 0.2235 0.088 Uiso 1 1 calc R . . C32 C 0.7708(6) -0.0079(3) 0.4146(6) 0.065(2) Uani 1 1 d . . . H32 H 0.8223 -0.0199 0.4650 0.078 Uiso 1 1 calc R . . C57 C 0.1159(6) 0.3415(3) -0.1675(6) 0.092(3) Uani 1 1 d . . . H57 H 0.1067 0.3079 -0.1603 0.110 Uiso 1 1 calc R . . C58 C 0.1345(6) 0.4407(3) -0.1893(7) 0.096(3) Uani 1 1 d . . . H58 H 0.1392 0.4750 -0.1934 0.115 Uiso 1 1 calc R . . C62 C -0.1055(7) 0.4505(4) -0.4702(7) 0.091(3) Uani 1 1 d . . . H62 H -0.1553 0.4441 -0.5272 0.109 Uiso 1 1 calc R . . C61 C -0.0006(6) 0.4887(4) -0.3615(7) 0.095(3) Uani 1 1 d . . . H61 H 0.0391 0.5131 -0.3245 0.114 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 0.0576(3) 0.0426(3) 0.0494(3) 0.0053(2) 0.0059(3) 0.0092(2) Cd2 0.0552(3) 0.0509(3) 0.0544(3) 0.0039(3) 0.0113(3) 0.0097(3) I3 0.0925(4) 0.0544(3) 0.0655(4) 0.0040(2) 0.0302(3) 0.0041(3) I2 0.1073(5) 0.0548(4) 0.0589(3) 0.0078(2) 0.0261(3) 0.0014(3) I1 0.0700(4) 0.0760(4) 0.0871(4) 0.0194(3) 0.0206(3) 0.0284(3) I4 0.0575(4) 0.0910(5) 0.0971(5) -0.0100(3) 0.0164(3) 0.0217(3) C24 0.048(4) 0.050(5) 0.046(4) 0.005(3) 0.007(3) 0.004(3) Cl2 0.126(3) 0.403(8) 0.116(3) 0.022(4) 0.044(3) 0.012(4) C56 0.089(7) 0.053(6) 0.071(6) -0.002(4) -0.027(5) -0.008(5) N2 0.047(3) 0.040(3) 0.035(3) -0.002(2) 0.012(3) 0.005(3) N1 0.044(3) 0.047(4) 0.049(3) 0.001(3) 0.010(3) 0.007(3) C55 0.046(4) 0.062(5) 0.050(4) -0.002(4) 0.007(4) 0.002(4) N7 0.045(3) 0.052(4) 0.046(3) -0.001(3) 0.010(3) 0.002(3) N8 0.045(3) 0.046(4) 0.042(3) 0.001(3) 0.012(3) 0.004(3) N3 0.059(4) 0.035(3) 0.060(4) 0.002(3) 0.012(3) 0.009(3) C8 0.046(4) 0.046(4) 0.037(4) -0.001(3) 0.011(3) 0.003(3) C40 0.050(4) 0.053(4) 0.046(4) -0.002(3) 0.019(4) 0.003(3) N9 0.060(4) 0.047(4) 0.061(4) 0.003(3) 0.028(3) 0.012(3) N5 0.035(3) 0.082(5) 0.050(4) 0.007(3) 0.002(3) -0.004(3) C39 0.039(4) 0.053(4) 0.044(4) -0.001(3) 0.016(3) 0.000(3) C29 0.051(4) 0.050(4) 0.047(4) 0.008(3) 0.007(4) 0.006(4) N4 0.041(3) 0.059(4) 0.049(3) 0.006(3) 0.001(3) 0.004(3) C47 0.040(4) 0.052(5) 0.039(4) 0.000(3) 0.007(3) -0.001(3) C6 0.042(4) 0.037(4) 0.043(4) 0.007(3) 0.015(3) 0.009(3) C17 0.054(4) 0.047(4) 0.047(4) 0.001(3) 0.004(4) 0.001(3) Cl1 0.177(4) 0.484(11) 0.181(5) -0.175(6) -0.031(4) 0.109(6) N10 0.046(4) 0.058(4) 0.071(4) 0.007(3) 0.003(3) 0.001(3) C52 0.045(4) 0.067(5) 0.049(4) -0.001(4) 0.012(4) 0.002(4) C20 0.062(5) 0.044(4) 0.061(5) 0.007(4) 0.005(4) 0.013(4) C2 0.046(4) 0.061(5) 0.063(5) 0.002(4) 0.002(4) -0.012(4) C37 0.043(4) 0.055(5) 0.042(4) -0.002(3) 0.012(3) 0.000(3) C12 0.070(5) 0.054(5) 0.050(4) -0.007(4) 0.013(4) 0.010(4) C18 0.050(4) 0.053(5) 0.049(4) -0.004(3) -0.004(4) 0.004(4) N6 0.063(4) 0.071(5) 0.075(5) 0.014(4) 0.013(4) 0.022(4) C16 0.046(4) 0.043(4) 0.040(4) 0.008(3) 0.012(3) 0.008(3) C45 0.052(4) 0.056(5) 0.054(4) -0.008(4) 0.007(4) -0.002(4) C9 0.046(4) 0.045(4) 0.039(4) -0.006(3) 0.005(3) 0.000(3) C7 0.054(4) 0.037(4) 0.043(4) 0.001(3) 0.016(4) 0.006(3) C41 0.035(4) 0.062(5) 0.039(4) 0.001(3) 0.008(3) 0.003(3) C5 0.042(4) 0.033(4) 0.044(4) -0.001(3) 0.010(3) 0.003(3) C46 0.053(5) 0.063(5) 0.047(4) 0.005(4) 0.005(4) 0.005(4) C35 0.077(6) 0.066(6) 0.051(5) -0.006(4) 0.023(4) 0.003(4) C10 0.048(4) 0.043(4) 0.043(4) -0.006(3) 0.016(3) 0.005(3) C51 0.042(4) 0.070(6) 0.064(5) 0.000(4) 0.004(4) -0.001(4) C42 0.046(4) 0.049(4) 0.044(4) -0.004(3) 0.017(3) 0.000(3) C36 0.051(4) 0.055(5) 0.047(4) 0.001(3) 0.022(4) -0.001(4) C26 0.079(6) 0.054(5) 0.053(5) -0.007(4) -0.020(4) 0.004(4) C25 0.088(6) 0.055(5) 0.064(5) 0.004(4) 0.006(5) 0.026(5) C19 0.048(4) 0.060(5) 0.043(4) 0.003(3) 0.001(3) 0.001(4) C43 0.051(4) 0.050(5) 0.052(4) 0.006(3) 0.018(4) 0.011(3) C21 0.048(4) 0.066(5) 0.036(4) 0.005(3) 0.003(3) 0.003(4) C1 0.050(4) 0.066(5) 0.049(4) 0.005(4) 0.000(4) 0.011(4) N11 0.064(4) 0.067(5) 0.066(4) -0.007(4) -0.001(4) 0.006(4) C54 0.054(5) 0.046(5) 0.064(5) 0.000(4) 0.008(4) -0.001(4) C59 0.053(5) 0.061(6) 0.077(6) 0.005(4) -0.023(4) -0.008(4) C23 0.055(5) 0.053(5) 0.053(4) 0.005(4) 0.007(4) 0.007(4) C15 0.076(5) 0.047(5) 0.058(5) 0.003(4) 0.014(4) 0.011(4) C50 0.083(6) 0.041(5) 0.074(5) 0.002(4) 0.001(5) 0.009(4) C60 0.043(4) 0.054(5) 0.053(4) 0.009(4) 0.006(4) 0.005(3) C14 0.101(7) 0.037(5) 0.087(6) -0.003(4) 0.038(6) -0.002(5) C22 0.056(4) 0.044(4) 0.050(4) 0.002(3) 0.008(4) 0.003(4) C44 0.055(5) 0.052(5) 0.054(4) -0.006(4) 0.013(4) 0.003(4) N12 0.076(5) 0.085(6) 0.100(6) 0.037(5) 0.016(5) 0.013(5) C11 0.045(4) 0.039(4) 0.045(4) 0.000(3) 0.011(3) 0.006(3) C53 0.044(4) 0.082(6) 0.058(5) 0.001(4) 0.007(4) -0.003(4) C49 0.055(5) 0.054(5) 0.068(5) 0.001(4) 0.013(4) -0.005(4) C3 0.065(5) 0.050(5) 0.074(6) -0.004(4) 0.005(5) -0.016(4) C4 0.052(5) 0.060(5) 0.060(5) 0.016(4) 0.003(4) 0.003(4) C63 0.207(16) 0.143(13) 0.160(13) -0.005(10) 0.100(13) -0.042(12) C13 0.069(5) 0.046(5) 0.076(6) -0.024(4) 0.023(5) -0.011(4) C48 0.048(5) 0.083(7) 0.054(5) -0.008(4) -0.013(4) 0.004(4) C27 0.082(6) 0.053(5) 0.054(5) -0.003(4) -0.020(4) 0.013(4) C28 0.078(6) 0.047(5) 0.063(5) -0.005(4) -0.013(4) 0.013(4) C30 0.047(5) 0.086(7) 0.057(5) 0.016(5) 0.002(4) 0.007(5) C31 0.064(5) 0.059(5) 0.067(5) 0.012(4) 0.004(4) 0.018(4) C38 0.042(4) 0.056(5) 0.041(4) 0.001(3) 0.008(3) -0.002(3) C33 0.097(7) 0.054(5) 0.078(6) 0.008(5) 0.041(5) 0.024(5) C34 0.092(7) 0.059(6) 0.069(6) -0.016(4) 0.036(5) -0.003(5) C32 0.066(5) 0.058(5) 0.067(5) -0.007(4) 0.024(4) 0.008(4) C57 0.074(6) 0.055(6) 0.089(6) 0.016(5) -0.018(5) -0.020(4) C58 0.098(7) 0.034(5) 0.101(7) 0.003(5) -0.009(6) -0.008(5) C62 0.077(7) 0.095(8) 0.071(6) 0.006(6) 0.004(5) 0.028(6) C61 0.073(6) 0.068(7) 0.108(8) 0.039(6) 0.005(6) 0.007(5) _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 N2 2.336(5) . ? Cd1 N3 2.380(6) . ? Cd1 N1 2.383(6) . ? Cd1 I1 2.7333(7) . ? Cd1 I2 2.7686(8) . ? Cd2 N8 2.322(5) . ? Cd2 N7 2.366(6) . ? Cd2 N9 2.375(6) . ? Cd2 I4 2.7355(8) . ? Cd2 I3 2.7542(7) . ? C24 C25 1.396(10) . ? C24 C26 1.402(10) . ? C24 C23 1.449(9) . ? Cl2 C63 1.588(14) . ? C56 C55 1.367(10) . ? C56 C58 1.396(11) . ? C56 H56 0.9300 . ? N2 C10 1.339(8) . ? N2 C6 1.355(8) . ? N1 C1 1.322(8) . ? N1 C5 1.344(8) . ? C55 C57 1.395(10) . ? C55 C54 1.433(9) . ? N7 C46 1.325(8) . ? N7 C42 1.345(8) . ? N8 C37 1.336(8) . ? N8 C41 1.347(8) . ? N3 C11 1.319(8) . ? N3 C15 1.322(9) . ? C8 C7 1.377(8) . ? C8 C9 1.413(9) . ? C8 C16 1.481(9) . ? C40 C41 1.360(9) . ? C40 C39 1.421(9) . ? C40 H40 0.9300 . ? N9 C32 1.340(9) . ? N9 C36 1.341(8) . ? N5 C30 1.324(10) . ? N5 N4 1.371(8) . ? C39 C38 1.370(9) . ? C39 C47 1.494(9) . ? C29 C27 1.354(10) . ? C29 C28 1.371(10) . ? C29 N4 1.422(8) . ? N4 C31 1.327(10) . ? C47 C48 1.371(10) . ? C47 C49 1.391(9) . ? C6 C7 1.380(8) . ? C6 C5 1.498(8) . ? C17 C19 1.377(9) . ? C17 C16 1.413(9) . ? C17 H17 0.9300 . ? Cl1 C63 1.787(16) . ? N10 C61 1.334(10) . ? N10 N11 1.343(8) . ? N10 C60 1.416(9) . ? C52 C51 1.380(10) . ? C52 C50 1.383(10) . ? C52 C53 1.483(10) . ? C20 C18 1.389(9) . ? C20 C21 1.390(10) . ? C20 H20 0.9300 . ? C2 C3 1.355(10) . ? C2 C1 1.374(10) . ? C2 H2 0.9300 . ? C37 C38 1.409(9) . ? C37 C36 1.493(10) . ? C12 C13 1.359(11) . ? C12 C11 1.391(10) . ? C12 H12 0.9300 . ? C18 C16 1.353(9) . ? C18 H18 0.9300 . ? N6 C30 1.294(11) . ? N6 C31 1.330(9) . ? C45 C46 1.340(10) . ? C45 C44 1.382(10) . ? C45 H45 0.9300 . ? C9 C10 1.378(9) . ? C9 H9 0.9300 . ? C7 H7 0.9300 . ? C41 C42 1.507(9) . ? C5 C4 1.376(9) . ? C46 H46 0.9300 . ? C35 C36 1.358(10) . ? C35 C34 1.387(11) . ? C35 H35 0.9300 . ? C10 C11 1.501(9) . ? C51 C49 1.398(10) . ? C51 H51 0.9300 . ? C42 C43 1.348(9) . ? C26 C28 1.359(10) . ? C26 H26 0.9300 . ? C25 C27 1.379(10) . ? C25 H25 0.9300 . ? C19 C21 1.406(10) . ? C19 H19 0.9300 . ? C43 C44 1.384(9) . ? C43 H43 0.9300 . ? C21 C22 1.459(9) . ? C1 H1 0.9300 . ? N11 C62 1.319(11) . ? C54 C53 1.296(10) . ? C54 H54 0.9300 . ? C59 C60 1.360(10) . ? C59 C57 1.373(10) . ? C59 H59 0.9300 . ? C23 C22 1.318(10) . ? C23 H23 0.9300 . ? C15 C14 1.383(11) . ? C15 H15 0.9300 . ? C50 C48 1.387(10) . ? C50 H50 0.9300 . ? C60 C58 1.373(10) . ? C14 C13 1.365(11) . ? C14 H14 0.9300 . ? C22 H22 0.9300 . ? C44 H44 0.9300 . ? N12 C62 1.333(12) . ? N12 C61 1.342(11) . ? C53 H53 0.9300 . ? C49 H49 0.9300 . ? C3 C4 1.366(10) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C13 H13 0.9300 . ? C48 H48 0.9300 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C38 H38 0.9300 . ? C33 C34 1.371(11) . ? C33 C32 1.383(11) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C32 H32 0.9300 . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C62 H62 0.9300 . ? C61 H61 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 Cd1 N3 68.78(19) . . ? N2 Cd1 N1 69.08(18) . . ? N3 Cd1 N1 137.72(19) . . ? N2 Cd1 I1 131.47(12) . . ? N3 Cd1 I1 100.11(14) . . ? N1 Cd1 I1 105.03(13) . . ? N2 Cd1 I2 115.43(12) . . ? N3 Cd1 I2 97.00(15) . . ? N1 Cd1 I2 103.70(13) . . ? I1 Cd1 I2 112.74(2) . . ? N8 Cd2 N7 69.74(19) . . ? N8 Cd2 N9 68.4(2) . . ? N7 Cd2 N9 137.54(19) . . ? N8 Cd2 I4 122.60(13) . . ? N7 Cd2 I4 94.38(13) . . ? N9 Cd2 I4 102.20(13) . . ? N8 Cd2 I3 111.19(13) . . ? N7 Cd2 I3 95.64(13) . . ? N9 Cd2 I3 105.46(13) . . ? I4 Cd2 I3 125.40(3) . . ? C25 C24 C26 115.5(6) . . ? C25 C24 C23 124.4(7) . . ? C26 C24 C23 120.1(6) . . ? C55 C56 C58 123.2(8) . . ? C55 C56 H56 118.4 . . ? C58 C56 H56 118.4 . . ? C10 N2 C6 119.2(5) . . ? C10 N2 Cd1 120.2(4) . . ? C6 N2 Cd1 120.3(4) . . ? C1 N1 C5 118.6(6) . . ? C1 N1 Cd1 122.8(5) . . ? C5 N1 Cd1 118.3(4) . . ? C56 C55 C57 114.8(7) . . ? C56 C55 C54 119.8(7) . . ? C57 C55 C54 125.3(7) . . ? C46 N7 C42 118.2(6) . . ? C46 N7 Cd2 122.9(5) . . ? C42 N7 Cd2 118.7(4) . . ? C37 N8 C41 119.7(5) . . ? C37 N8 Cd2 120.3(4) . . ? C41 N8 Cd2 119.3(4) . . ? C11 N3 C15 119.8(6) . . ? C11 N3 Cd1 119.0(4) . . ? C15 N3 Cd1 121.1(5) . . ? C7 C8 C9 116.1(6) . . ? C7 C8 C16 122.3(6) . . ? C9 C8 C16 121.5(6) . . ? C41 C40 C39 120.0(7) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C32 N9 C36 118.6(7) . . ? C32 N9 Cd2 121.8(5) . . ? C36 N9 Cd2 119.6(5) . . ? C30 N5 N4 100.2(7) . . ? C38 C39 C40 117.4(6) . . ? C38 C39 C47 122.6(6) . . ? C40 C39 C47 119.9(6) . . ? C27 C29 C28 119.3(7) . . ? C27 C29 N4 120.1(6) . . ? C28 C29 N4 120.6(7) . . ? C31 N4 N5 109.3(6) . . ? C31 N4 C29 130.2(6) . . ? N5 N4 C29 120.5(6) . . ? C48 C47 C49 118.6(6) . . ? C48 C47 C39 120.8(6) . . ? C49 C47 C39 120.6(6) . . ? N2 C6 C7 121.2(6) . . ? N2 C6 C5 115.3(5) . . ? C7 C6 C5 123.6(6) . . ? C19 C17 C16 119.5(7) . . ? C19 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C61 N10 N11 111.1(7) . . ? C61 N10 C60 129.0(7) . . ? N11 N10 C60 119.9(6) . . ? C51 C52 C50 117.2(7) . . ? C51 C52 C53 119.4(7) . . ? C50 C52 C53 123.1(8) . . ? C18 C20 C21 120.2(7) . . ? C18 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C3 C2 C1 118.2(7) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? N8 C37 C38 121.2(6) . . ? N8 C37 C36 116.3(6) . . ? C38 C37 C36 122.5(6) . . ? C13 C12 C11 119.7(7) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C16 C18 C20 123.1(7) . . ? C16 C18 H18 118.5 . . ? C20 C18 H18 118.5 . . ? C30 N6 C31 102.4(7) . . ? C18 C16 C17 117.8(6) . . ? C18 C16 C8 121.5(6) . . ? C17 C16 C8 120.7(6) . . ? C46 C45 C44 119.3(7) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C8 C7 C6 121.3(6) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N8 C41 C40 121.7(6) . . ? N8 C41 C42 116.1(6) . . ? C40 C41 C42 122.1(6) . . ? N1 C5 C4 120.6(6) . . ? N1 C5 C6 116.5(6) . . ? C4 C5 C6 122.9(6) . . ? N7 C46 C45 123.2(7) . . ? N7 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? C36 C35 C34 119.9(8) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? N2 C10 C9 121.4(6) . . ? N2 C10 C11 115.5(5) . . ? C9 C10 C11 123.1(6) . . ? C52 C51 C49 122.1(7) . . ? C52 C51 H51 119.0 . . ? C49 C51 H51 119.0 . . ? N7 C42 C43 121.8(6) . . ? N7 C42 C41 115.1(6) . . ? C43 C42 C41 123.0(6) . . ? N9 C36 C35 122.1(7) . . ? N9 C36 C37 114.4(6) . . ? C35 C36 C37 123.6(7) . . ? C28 C26 C24 122.0(7) . . ? C28 C26 H26 119.0 . . ? C24 C26 H26 119.0 . . ? C27 C25 C24 121.9(7) . . ? C27 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C17 C19 C21 122.5(7) . . ? C17 C19 H19 118.7 . . ? C21 C19 H19 118.7 . . ? C42 C43 C44 119.7(7) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C20 C21 C19 116.8(6) . . ? C20 C21 C22 123.7(7) . . ? C19 C21 C22 119.5(6) . . ? N1 C1 C2 123.3(7) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C62 N11 N10 101.8(7) . . ? C53 C54 C55 126.6(7) . . ? C53 C54 H54 116.7 . . ? C55 C54 H54 116.7 . . ? C60 C59 C57 120.7(7) . . ? C60 C59 H59 119.7 . . ? C57 C59 H59 119.7 . . ? C22 C23 C24 127.2(7) . . ? C22 C23 H23 116.4 . . ? C24 C23 H23 116.4 . . ? N3 C15 C14 122.2(7) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C52 C50 C48 121.2(8) . . ? C52 C50 H50 119.4 . . ? C48 C50 H50 119.4 . . ? C59 C60 C58 118.6(7) . . ? C59 C60 N10 121.1(7) . . ? C58 C60 N10 120.3(7) . . ? C13 C14 C15 118.3(8) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C23 C22 C21 126.4(7) . . ? C23 C22 H22 116.8 . . ? C21 C22 H22 116.8 . . ? C45 C44 C43 117.7(7) . . ? C45 C44 H44 121.1 . . ? C43 C44 H44 121.1 . . ? C62 N12 C61 103.0(8) . . ? N3 C11 C12 120.7(6) . . ? N3 C11 C10 116.4(6) . . ? C12 C11 C10 122.9(6) . . ? C54 C53 C52 126.6(7) . . ? C54 C53 H53 116.7 . . ? C52 C53 H53 116.7 . . ? C47 C49 C51 119.4(7) . . ? C47 C49 H49 120.3 . . ? C51 C49 H49 120.3 . . ? C2 C3 C4 119.5(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.9(7) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? Cl2 C63 Cl1 110.5(9) . . ? Cl2 C63 H63A 109.6 . . ? Cl1 C63 H63A 109.6 . . ? Cl2 C63 H63B 109.6 . . ? Cl1 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? C12 C13 C14 119.3(7) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C47 C48 C50 121.3(7) . . ? C47 C48 H48 119.4 . . ? C50 C48 H48 119.4 . . ? C29 C27 C25 120.5(7) . . ? C29 C27 H27 119.7 . . ? C25 C27 H27 119.7 . . ? C26 C28 C29 120.7(7) . . ? C26 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? N6 C30 N5 117.8(7) . . ? N6 C30 H30 121.1 . . ? N5 C30 H30 121.1 . . ? N4 C31 N6 110.3(8) . . ? N4 C31 H31 124.9 . . ? N6 C31 H31 124.9 . . ? C39 C38 C37 119.8(6) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C34 C33 C32 119.2(8) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 118.3(8) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? N9 C32 C33 122.0(8) . . ? N9 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C59 C57 C55 122.9(8) . . ? C59 C57 H57 118.6 . . ? C55 C57 H57 118.6 . . ? C60 C58 C56 119.6(8) . . ? C60 C58 H58 120.2 . . ? C56 C58 H58 120.2 . . ? N11 C62 N12 115.6(8) . . ? N11 C62 H62 122.2 . . ? N12 C62 H62 122.2 . . ? N10 C61 N12 108.5(9) . . ? N10 C61 H61 125.7 . . ? N12 C61 H61 125.7 . . ? 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 N3 Cd1 N2 C10 -3.4(4) . . . . ? N1 Cd1 N2 C10 180.0(5) . . . . ? I1 Cd1 N2 C10 -88.2(4) . . . . ? I2 Cd1 N2 C10 84.3(4) . . . . ? N3 Cd1 N2 C6 -177.1(5) . . . . ? N1 Cd1 N2 C6 6.3(4) . . . . ? I1 Cd1 N2 C6 98.2(4) . . . . ? I2 Cd1 N2 C6 -89.3(4) . . . . ? N2 Cd1 N1 C1 179.5(6) . . . . ? N3 Cd1 N1 C1 174.8(5) . . . . ? I1 Cd1 N1 C1 50.4(5) . . . . ? I2 Cd1 N1 C1 -68.1(5) . . . . ? N2 Cd1 N1 C5 -6.8(4) . . . . ? N3 Cd1 N1 C5 -11.6(6) . . . . ? I1 Cd1 N1 C5 -136.0(4) . . . . ? I2 Cd1 N1 C5 105.5(4) . . . . ? C58 C56 C55 C57 0.2(15) . . . . ? C58 C56 C55 C54 177.3(9) . . . . ? N8 Cd2 N7 C46 -174.1(6) . . . . ? N9 Cd2 N7 C46 -164.3(5) . . . . ? I4 Cd2 N7 C46 -50.9(5) . . . . ? I3 Cd2 N7 C46 75.4(5) . . . . ? N8 Cd2 N7 C42 0.7(4) . . . . ? N9 Cd2 N7 C42 10.5(6) . . . . ? I4 Cd2 N7 C42 123.9(4) . . . . ? I3 Cd2 N7 C42 -109.8(4) . . . . ? N7 Cd2 N8 C37 -177.1(5) . . . . ? N9 Cd2 N8 C37 10.0(4) . . . . ? I4 Cd2 N8 C37 100.9(5) . . . . ? I3 Cd2 N8 C37 -88.9(5) . . . . ? N7 Cd2 N8 C41 -6.7(4) . . . . ? N9 Cd2 N8 C41 -179.6(5) . . . . ? I4 Cd2 N8 C41 -88.7(5) . . . . ? I3 Cd2 N8 C41 81.5(5) . . . . ? N2 Cd1 N3 C11 1.3(5) . . . . ? N1 Cd1 N3 C11 6.1(7) . . . . ? I1 Cd1 N3 C11 132.1(5) . . . . ? I2 Cd1 N3 C11 -113.3(5) . . . . ? N2 Cd1 N3 C15 178.1(6) . . . . ? N1 Cd1 N3 C15 -177.1(5) . . . . ? I1 Cd1 N3 C15 -51.1(6) . . . . ? I2 Cd1 N3 C15 63.5(6) . . . . ? N8 Cd2 N9 C32 176.9(6) . . . . ? N7 Cd2 N9 C32 167.1(5) . . . . ? I4 Cd2 N9 C32 56.5(5) . . . . ? I3 Cd2 N9 C32 -76.0(5) . . . . ? N8 Cd2 N9 C36 -7.2(4) . . . . ? N7 Cd2 N9 C36 -17.1(6) . . . . ? I4 Cd2 N9 C36 -127.7(4) . . . . ? I3 Cd2 N9 C36 99.8(5) . . . . ? C41 C40 C39 C38 -2.6(9) . . . . ? C41 C40 C39 C47 -179.8(6) . . . . ? C30 N5 N4 C31 1.1(8) . . . . ? C30 N5 N4 C29 -179.4(6) . . . . ? C27 C29 N4 C31 154.9(9) . . . . ? C28 C29 N4 C31 -25.6(12) . . . . ? C27 C29 N4 N5 -24.5(10) . . . . ? C28 C29 N4 N5 155.0(7) . . . . ? C38 C39 C47 C48 -165.6(7) . . . . ? C40 C39 C47 C48 11.4(10) . . . . ? C38 C39 C47 C49 13.5(10) . . . . ? C40 C39 C47 C49 -169.6(6) . . . . ? C10 N2 C6 C7 0.8(9) . . . . ? Cd1 N2 C6 C7 174.5(4) . . . . ? C10 N2 C6 C5 -179.0(5) . . . . ? Cd1 N2 C6 C5 -5.3(7) . . . . ? C41 N8 C37 C38 -1.0(9) . . . . ? Cd2 N8 C37 C38 169.4(5) . . . . ? C41 N8 C37 C36 178.0(6) . . . . ? Cd2 N8 C37 C36 -11.6(7) . . . . ? C21 C20 C18 C16 -0.8(12) . . . . ? C20 C18 C16 C17 -0.4(11) . . . . ? C20 C18 C16 C8 179.4(7) . . . . ? C19 C17 C16 C18 0.9(10) . . . . ? C19 C17 C16 C8 -178.9(6) . . . . ? C7 C8 C16 C18 9.3(10) . . . . ? C9 C8 C16 C18 -169.2(7) . . . . ? C7 C8 C16 C17 -171.0(6) . . . . ? C9 C8 C16 C17 10.5(9) . . . . ? C7 C8 C9 C10 -1.7(9) . . . . ? C16 C8 C9 C10 176.9(6) . . . . ? C9 C8 C7 C6 2.3(9) . . . . ? C16 C8 C7 C6 -176.3(6) . . . . ? N2 C6 C7 C8 -1.9(9) . . . . ? C5 C6 C7 C8 177.9(6) . . . . ? C37 N8 C41 C40 1.0(9) . . . . ? Cd2 N8 C41 C40 -169.5(5) . . . . ? C37 N8 C41 C42 -178.1(5) . . . . ? Cd2 N8 C41 C42 11.4(7) . . . . ? C39 C40 C41 N8 0.9(10) . . . . ? C39 C40 C41 C42 179.9(5) . . . . ? C1 N1 C5 C4 1.4(9) . . . . ? Cd1 N1 C5 C4 -172.5(5) . . . . ? C1 N1 C5 C6 -179.3(6) . . . . ? Cd1 N1 C5 C6 6.8(7) . . . . ? N2 C6 C5 N1 -1.1(8) . . . . ? C7 C6 C5 N1 179.1(6) . . . . ? N2 C6 C5 C4 178.1(6) . . . . ? C7 C6 C5 C4 -1.7(10) . . . . ? C42 N7 C46 C45 -1.5(10) . . . . ? Cd2 N7 C46 C45 173.4(6) . . . . ? C44 C45 C46 N7 1.3(12) . . . . ? C6 N2 C10 C9 -0.3(9) . . . . ? Cd1 N2 C10 C9 -174.0(5) . . . . ? C6 N2 C10 C11 178.6(5) . . . . ? Cd1 N2 C10 C11 4.9(7) . . . . ? C8 C9 C10 N2 0.7(9) . . . . ? C8 C9 C10 C11 -178.1(6) . . . . ? C50 C52 C51 C49 3.3(12) . . . . ? C53 C52 C51 C49 176.9(7) . . . . ? C46 N7 C42 C43 0.7(9) . . . . ? Cd2 N7 C42 C43 -174.3(5) . . . . ? C46 N7 C42 C41 179.6(6) . . . . ? Cd2 N7 C42 C41 4.5(7) . . . . ? N8 C41 C42 N7 -10.3(8) . . . . ? C40 C41 C42 N7 170.5(6) . . . . ? N8 C41 C42 C43 168.5(6) . . . . ? C40 C41 C42 C43 -10.7(10) . . . . ? C32 N9 C36 C35 -0.8(10) . . . . ? Cd2 N9 C36 C35 -176.8(5) . . . . ? C32 N9 C36 C37 -179.8(6) . . . . ? Cd2 N9 C36 C37 4.2(7) . . . . ? C34 C35 C36 N9 0.6(11) . . . . ? C34 C35 C36 C37 179.5(7) . . . . ? N8 C37 C36 N9 4.6(8) . . . . ? C38 C37 C36 N9 -176.4(6) . . . . ? N8 C37 C36 C35 -174.4(6) . . . . ? C38 C37 C36 C35 4.6(10) . . . . ? C25 C24 C26 C28 -1.3(13) . . . . ? C23 C24 C26 C28 -179.7(8) . . . . ? C26 C24 C25 C27 1.4(13) . . . . ? C23 C24 C25 C27 179.7(8) . . . . ? C16 C17 C19 C21 -0.2(11) . . . . ? N7 C42 C43 C44 0.2(10) . . . . ? C41 C42 C43 C44 -178.6(6) . . . . ? C18 C20 C21 C19 1.4(11) . . . . ? C18 C20 C21 C22 -179.5(7) . . . . ? C17 C19 C21 C20 -0.9(11) . . . . ? C17 C19 C21 C22 180.0(6) . . . . ? C5 N1 C1 C2 0.9(11) . . . . ? Cd1 N1 C1 C2 174.5(6) . . . . ? C3 C2 C1 N1 -2.6(12) . . . . ? C61 N10 N11 C62 0.8(9) . . . . ? C60 N10 N11 C62 -179.2(7) . . . . ? C56 C55 C54 C53 -176.0(9) . . . . ? C57 C55 C54 C53 0.7(13) . . . . ? C25 C24 C23 C22 12.3(12) . . . . ? C26 C24 C23 C22 -169.4(8) . . . . ? C11 N3 C15 C14 -1.9(11) . . . . ? Cd1 N3 C15 C14 -178.6(6) . . . . ? C51 C52 C50 C48 -2.4(12) . . . . ? C53 C52 C50 C48 -175.7(7) . . . . ? C57 C59 C60 C58 -4.3(14) . . . . ? C57 C59 C60 N10 177.4(8) . . . . ? C61 N10 C60 C59 176.3(9) . . . . ? N11 N10 C60 C59 -3.7(11) . . . . ? C61 N10 C60 C58 -2.0(13) . . . . ? N11 N10 C60 C58 177.9(8) . . . . ? N3 C15 C14 C13 -0.2(12) . . . . ? C24 C23 C22 C21 177.5(7) . . . . ? C20 C21 C22 C23 15.4(12) . . . . ? C19 C21 C22 C23 -165.5(8) . . . . ? C46 C45 C44 C43 -0.3(10) . . . . ? C42 C43 C44 C45 -0.4(10) . . . . ? C15 N3 C11 C12 2.7(10) . . . . ? Cd1 N3 C11 C12 179.5(5) . . . . ? C15 N3 C11 C10 -176.3(6) . . . . ? Cd1 N3 C11 C10 0.6(8) . . . . ? C13 C12 C11 N3 -1.5(11) . . . . ? C13 C12 C11 C10 177.4(7) . . . . ? N2 C10 C11 N3 -3.6(8) . . . . ? C9 C10 C11 N3 175.3(6) . . . . ? N2 C10 C11 C12 177.5(6) . . . . ? C9 C10 C11 C12 -3.6(10) . . . . ? C55 C54 C53 C52 175.8(7) . . . . ? C51 C52 C53 C54 -173.0(8) . . . . ? C50 C52 C53 C54 0.2(13) . . . . ? C48 C47 C49 C51 2.8(11) . . . . ? C39 C47 C49 C51 -176.3(6) . . . . ? C52 C51 C49 C47 -3.6(11) . . . . ? C1 C2 C3 C4 1.9(12) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? N1 C5 C4 C3 -2.0(11) . . . . ? C6 C5 C4 C3 178.7(7) . . . . ? C11 C12 C13 C14 -0.6(12) . . . . ? C15 C14 C13 C12 1.4(12) . . . . ? C49 C47 C48 C50 -2.0(12) . . . . ? C39 C47 C48 C50 177.1(7) . . . . ? C52 C50 C48 C47 1.8(13) . . . . ? C28 C29 C27 C25 3.2(14) . . . . ? N4 C29 C27 C25 -177.3(8) . . . . ? C24 C25 C27 C29 -2.5(14) . . . . ? C24 C26 C28 C29 2.2(14) . . . . ? C27 C29 C28 C26 -3.1(13) . . . . ? N4 C29 C28 C26 177.4(8) . . . . ? C31 N6 C30 N5 2.6(10) . . . . ? N4 N5 C30 N6 -2.3(9) . . . . ? N5 N4 C31 N6 0.3(9) . . . . ? C29 N4 C31 N6 -179.1(7) . . . . ? C30 N6 C31 N4 -1.6(9) . . . . ? C40 C39 C38 C37 2.6(9) . . . . ? C47 C39 C38 C37 179.7(6) . . . . ? N8 C37 C38 C39 -0.9(10) . . . . ? C36 C37 C38 C39 -179.8(6) . . . . ? C32 C33 C34 C35 -0.5(12) . . . . ? C36 C35 C34 C33 0.1(12) . . . . ? C36 N9 C32 C33 0.3(11) . . . . ? Cd2 N9 C32 C33 176.2(6) . . . . ? C34 C33 C32 N9 0.3(12) . . . . ? C60 C59 C57 C55 -0.5(15) . . . . ? C56 C55 C57 C59 2.5(14) . . . . ? C54 C55 C57 C59 -174.3(9) . . . . ? C59 C60 C58 C56 6.8(15) . . . . ? N10 C60 C58 C56 -174.8(9) . . . . ? C55 C56 C58 C60 -4.9(17) . . . . ? N10 N11 C62 N12 -1.1(11) . . . . ? C61 N12 C62 N11 1.0(12) . . . . ? N11 N10 C61 N12 -0.2(11) . . . . ? C60 N10 C61 N12 179.7(7) . . . . ? C62 N12 C61 N10 -0.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.270 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.106