# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name M.Hosseini _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg France ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Porphyrin based Metallamacrocycles ; loop_ _publ_author_name 'M. Hosseini' 'Veronique Bulach' 'Emmanuel Deiters' # Attachment 'compound 5.cif' data_e5 _database_code_depnum_ccdc_archive 'CCDC 245804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H62 I4 N12 O3 Zn4' _chemical_formula_weight 2080.56 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' 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' _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 9.6797(3) _cell_length_b 12.6462(4) _cell_length_c 17.6494(6) _cell_angle_alpha 87.281(2) _cell_angle_beta 75.648(2) _cell_angle_gamma 87.824(2) _cell_volume 2089.94(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6747 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 22.04 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 2.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6176 _exptl_absorpt_correction_T_max 0.7764 _exptl_absorpt_process_details sadabs _exptl_special_details ; Disordered solvent molecules have been refined isotropically. no Hydrogen atoms have been introduced on disordered molecules however the missing hydrogen have been introduced to the formula ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 99405 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 29.26 _reflns_number_total 11230 _reflns_number_gt 7421 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+0.5998P] 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 11230 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1961 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.67987(8) -0.01833(5) 0.86734(4) 0.03645(19) Uani 1 1 d . A 1 Zn2 Zn 0.84623(7) 0.45802(5) 0.40315(3) 0.02992(17) Uani 1 1 d . . 1 I1 I 1.10806(4) 0.43795(3) 0.32780(2) 0.04287(14) Uani 1 1 d . B 1 I2 I 0.72311(4) 0.64048(3) 0.42539(2) 0.04008(14) Uani 1 1 d . C 1 N1 N 0.6266(5) -0.0111(3) 0.7624(2) 0.0286(9) Uani 1 1 d . A 1 N2 N 0.5878(5) -0.1624(3) 0.8931(2) 0.0268(9) Uani 1 1 d . A 1 N3 N 0.7106(5) -0.0186(3) 0.9776(2) 0.0288(9) Uani 1 1 d . A 1 N4 N 0.7680(5) 0.1269(3) 0.8440(2) 0.0276(9) Uani 1 1 d . A 1 N5 N 0.2768(5) -0.3749(4) 0.6536(2) 0.0300(10) Uani 1 1 d . . 1 C45 C 0.5885(7) -0.4238(5) 1.2184(3) 0.0381(13) Uani 1 1 d . A 1 H45 H 0.5809 -0.4731 1.2614 0.046 Uiso 1 1 calc R A 1 C46 C 1.0026(8) 0.3790(6) 1.0935(4) 0.0503(18) Uani 1 1 d . A 1 H46 H 1.0438 0.4284 1.1197 0.060 Uiso 1 1 calc R A 1 N8 N 0.8167(5) 0.3730(4) 0.5078(3) 0.0314(10) Uani 1 1 d . A 1 C1 C 0.6538(6) 0.0717(4) 0.7063(3) 0.0336(12) Uani 1 1 d . A 1 C2 C 0.5894(8) 0.0499(5) 0.6436(4) 0.0520(18) Uani 1 1 d . A 1 H2 H 0.5895 0.0946 0.5987 0.062 Uiso 1 1 calc R A 1 C3 C 0.5289(8) -0.0453(5) 0.6601(4) 0.0493(17) Uani 1 1 d . A 1 H3 H 0.4792 -0.0804 0.6289 0.059 Uiso 1 1 calc R A 1 C4 C 0.5535(6) -0.0845(4) 0.7340(3) 0.0334(12) Uani 1 1 d . A 1 C5 C 0.5145(6) -0.1848(4) 0.7698(3) 0.0305(12) Uani 1 1 d . A 1 C6 C 0.5380(6) -0.2216(4) 0.8432(3) 0.0284(11) Uani 1 1 d . A 1 C7 C 0.5124(6) -0.3278(4) 0.8735(3) 0.0345(12) Uani 1 1 d . A 1 H7 H 0.4771 -0.3832 0.8497 0.041 Uiso 1 1 calc R A 1 C8 C 0.5494(7) -0.3336(4) 0.9447(3) 0.0352(13) Uani 1 1 d . A 1 H8 H 0.5484 -0.3946 0.9783 0.042 Uiso 1 1 calc R A 1 C9 C 0.5899(6) -0.2279(4) 0.9577(3) 0.0280(11) Uani 1 1 d . A 1 C10 C 0.6246(6) -0.1977(4) 1.0258(3) 0.0279(11) Uani 1 1 d . A 1 C11 C 0.6718(6) -0.0964(4) 1.0359(3) 0.0284(11) Uani 1 1 d . A 1 C12 C 0.6934(6) -0.0604(4) 1.1084(3) 0.0320(12) Uani 1 1 d . A 1 H12 H 0.6724 -0.0981 1.1575 0.038 Uiso 1 1 calc R A 1 C13 C 0.7497(6) 0.0383(4) 1.0932(3) 0.0303(11) Uani 1 1 d . A 1 H13 H 0.7750 0.0821 1.1296 0.036 Uiso 1 1 calc R A 1 C14 C 0.7630(6) 0.0630(4) 1.0108(3) 0.0280(11) Uani 1 1 d . A 1 C15 C 0.8233(6) 0.1567(4) 0.9702(3) 0.0284(11) Uani 1 1 d . A 1 C16 C 0.8308(6) 0.1817(4) 0.8907(3) 0.0282(11) Uani 1 1 d . A 1 C17 C 0.9013(6) 0.2720(5) 0.8469(3) 0.0344(12) Uani 1 1 d . A 1 H17 H 0.9544 0.3222 0.8655 0.041 Uiso 1 1 calc R A 1 C18 C 0.8780(6) 0.2720(4) 0.7748(3) 0.0340(12) Uani 1 1 d . A 1 H18 H 0.9123 0.3219 0.7330 0.041 Uiso 1 1 calc R A 1 C19 C 0.7926(6) 0.1834(4) 0.7726(3) 0.0286(11) Uani 1 1 d . A 1 C20 C 0.7349(6) 0.1596(4) 0.7107(3) 0.0289(11) Uani 1 1 d . A 1 C21 C 0.4353(6) -0.2540(4) 0.7301(3) 0.0266(11) Uani 1 1 d . A 1 C22 C 0.4977(6) -0.2952(5) 0.6570(3) 0.0365(13) Uani 1 1 d . A 1 H22 H 0.5950 -0.2832 0.6321 0.044 Uiso 1 1 calc R A 1 C23 C 0.4151(6) -0.3537(5) 0.6217(3) 0.0353(13) Uani 1 1 d . A 1 H23 H 0.4585 -0.3808 0.5718 0.042 Uiso 1 1 calc R A 1 C24 C 0.2204(6) -0.3379(5) 0.7263(3) 0.0343(12) Uani 1 1 d . A 1 H24 H 0.1242 -0.3532 0.7515 0.041 Uiso 1 1 calc R A 1 C25 C 0.2964(6) -0.2796(4) 0.7647(3) 0.0314(12) Uani 1 1 d . A 1 H25 H 0.2526 -0.2566 0.8158 0.038 Uiso 1 1 calc R A 1 C29 C 0.6100(6) -0.2768(4) 1.0929(3) 0.0281(11) Uani 1 1 d . A 1 C30 C 0.4839(6) -0.3271(4) 1.1257(3) 0.0331(12) Uani 1 1 d . A 1 H30 H 0.4033 -0.3108 1.1051 0.040 Uiso 1 1 calc R A 1 C31 C 0.4708(7) -0.4008(5) 1.1876(3) 0.0367(13) Uani 1 1 d . A 1 H31 H 0.3832 -0.4350 1.2088 0.044 Uiso 1 1 calc R A 1 C32 C 0.7155(7) -0.3750(5) 1.1864(3) 0.0400(14) Uani 1 1 d . A 1 H32 H 0.7956 -0.3913 1.2073 0.048 Uiso 1 1 calc R A 1 C33 C 0.7280(6) -0.3025(5) 1.1242(3) 0.0346(12) Uani 1 1 d . A 1 H33 H 0.8166 -0.2698 1.1024 0.042 Uiso 1 1 calc R A 1 C34 C 0.8852(6) 0.2331(4) 1.0144(3) 0.0325(12) Uani 1 1 d . A 1 C35 C 0.9924(7) 0.2025(5) 1.0520(3) 0.0405(14) Uani 1 1 d . A 1 H35 H 1.0263 0.1309 1.0509 0.049 Uiso 1 1 calc R A 1 C36 C 1.0497(7) 0.2761(7) 1.0909(4) 0.056(2) Uani 1 1 d . A 1 H36 H 1.1228 0.2543 1.1160 0.067 Uiso 1 1 calc R A 1 C37 C 0.8945(8) 0.4119(6) 1.0578(4) 0.0508(18) Uani 1 1 d . A 1 H37 H 0.8609 0.4835 1.0598 0.061 Uiso 1 1 calc R A 1 C38 C 0.8353(7) 0.3375(5) 1.0185(3) 0.0379(13) Uani 1 1 d . A 1 H38 H 0.7605 0.3592 0.9947 0.046 Uiso 1 1 calc R A 1 C39 C 0.7635(6) 0.2357(4) 0.6405(3) 0.0301(12) Uani 1 1 d . A 1 C40 C 0.8997(6) 0.2424(5) 0.5901(3) 0.0384(13) Uani 1 1 d . A 1 H40 H 0.9769 0.2000 0.6000 0.046 Uiso 1 1 calc R A 1 C41 C 0.9202(6) 0.3114(5) 0.5259(3) 0.0383(13) Uani 1 1 d . A 1 H41 H 1.0134 0.3156 0.4924 0.046 Uiso 1 1 calc R A 1 C42 C 0.6886(6) 0.3693(5) 0.5578(3) 0.0340(12) Uani 1 1 d . A 1 H42 H 0.6148 0.4153 0.5477 0.041 Uiso 1 1 calc R A 1 C43 C 0.6576(7) 0.3020(5) 0.6235(3) 0.0354(13) Uani 1 1 d . A 1 H43 H 0.5639 0.3014 0.6567 0.043 Uiso 1 1 calc R A 1 O1 O 0.9072(10) -0.0802(7) 0.7990(5) 0.048(2) Uiso 0.50 1 d P A 1 C44 C 1.0241(14) -0.0566(10) 0.7300(7) 0.042(3) Uiso 0.50 1 d P A 1 O4 O 0.2072(10) 0.8987(7) 0.5733(5) 0.050(2) Uiso 0.50 1 d P D 1 O2 O 0.9025(10) -0.0899(7) 0.5993(6) 0.050(2) Uiso 0.50 1 d P A 1 C48 C 0.9576(15) -0.1606(11) 0.6655(8) 0.047(3) Uiso 0.50 1 d P A 1 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 Zn1 0.0607(5) 0.0267(3) 0.0292(3) 0.0093(2) -0.0239(3) -0.0194(3) Zn2 0.0374(4) 0.0319(3) 0.0233(3) 0.0069(2) -0.0120(3) -0.0166(3) I1 0.0366(2) 0.0481(3) 0.0423(2) 0.01002(18) -0.00681(17) -0.01556(18) I2 0.0428(2) 0.0357(2) 0.0433(2) 0.00187(16) -0.01310(18) -0.00947(17) N1 0.035(2) 0.026(2) 0.026(2) 0.0072(17) -0.0107(18) -0.0145(18) N2 0.035(2) 0.025(2) 0.023(2) 0.0052(16) -0.0110(18) -0.0099(18) N3 0.037(2) 0.027(2) 0.024(2) 0.0062(17) -0.0088(19) -0.0127(18) N4 0.036(2) 0.029(2) 0.021(2) 0.0054(17) -0.0109(18) -0.0107(18) N5 0.039(3) 0.032(2) 0.021(2) 0.0047(17) -0.0099(19) -0.0160(19) C45 0.051(4) 0.033(3) 0.030(3) 0.009(2) -0.012(3) -0.003(3) C46 0.063(4) 0.054(4) 0.032(3) -0.007(3) -0.002(3) -0.037(3) N8 0.037(3) 0.035(2) 0.026(2) 0.0093(18) -0.0122(19) -0.020(2) C1 0.045(3) 0.034(3) 0.025(3) 0.008(2) -0.014(2) -0.018(2) C2 0.081(5) 0.055(4) 0.033(3) 0.021(3) -0.037(3) -0.037(4) C3 0.075(5) 0.051(4) 0.034(3) 0.014(3) -0.035(3) -0.036(3) C4 0.039(3) 0.036(3) 0.029(3) 0.009(2) -0.014(2) -0.018(2) C5 0.031(3) 0.036(3) 0.025(3) 0.006(2) -0.008(2) -0.015(2) C6 0.032(3) 0.032(3) 0.024(2) 0.004(2) -0.010(2) -0.013(2) C7 0.045(3) 0.032(3) 0.031(3) 0.001(2) -0.018(3) -0.010(2) C8 0.048(3) 0.029(3) 0.032(3) 0.007(2) -0.017(3) -0.015(2) C9 0.036(3) 0.023(2) 0.027(3) 0.0039(19) -0.010(2) -0.009(2) C10 0.036(3) 0.028(3) 0.023(2) 0.006(2) -0.012(2) -0.011(2) C11 0.033(3) 0.027(3) 0.027(3) 0.007(2) -0.011(2) -0.010(2) C12 0.041(3) 0.032(3) 0.022(2) 0.003(2) -0.006(2) -0.011(2) C13 0.039(3) 0.031(3) 0.023(3) -0.001(2) -0.009(2) -0.007(2) C14 0.035(3) 0.026(2) 0.025(2) 0.001(2) -0.010(2) -0.010(2) C15 0.029(3) 0.028(3) 0.029(3) 0.000(2) -0.008(2) -0.012(2) C16 0.033(3) 0.026(3) 0.027(3) 0.003(2) -0.010(2) -0.012(2) C17 0.036(3) 0.040(3) 0.029(3) 0.006(2) -0.011(2) -0.015(2) C18 0.037(3) 0.038(3) 0.029(3) 0.009(2) -0.010(2) -0.020(2) C19 0.029(3) 0.032(3) 0.024(2) 0.005(2) -0.005(2) -0.010(2) C20 0.035(3) 0.030(3) 0.021(2) 0.009(2) -0.005(2) -0.014(2) C21 0.035(3) 0.025(2) 0.022(2) 0.0057(19) -0.012(2) -0.011(2) C22 0.037(3) 0.041(3) 0.033(3) 0.006(2) -0.011(2) -0.015(3) C23 0.039(3) 0.044(3) 0.023(3) -0.005(2) -0.005(2) -0.012(3) C24 0.038(3) 0.039(3) 0.026(3) 0.001(2) -0.006(2) -0.015(2) C25 0.044(3) 0.033(3) 0.019(2) 0.000(2) -0.010(2) -0.014(2) C29 0.034(3) 0.028(3) 0.024(2) 0.003(2) -0.011(2) -0.004(2) C30 0.038(3) 0.030(3) 0.033(3) 0.004(2) -0.013(2) -0.004(2) C31 0.044(3) 0.035(3) 0.029(3) 0.007(2) -0.005(2) -0.011(3) C32 0.049(4) 0.043(3) 0.032(3) 0.006(2) -0.019(3) 0.003(3) C33 0.037(3) 0.038(3) 0.029(3) 0.005(2) -0.009(2) -0.009(2) C34 0.039(3) 0.038(3) 0.019(2) 0.001(2) -0.003(2) -0.019(2) C35 0.042(3) 0.053(4) 0.026(3) -0.001(2) -0.005(2) -0.015(3) C36 0.042(4) 0.102(6) 0.025(3) 0.001(3) -0.008(3) -0.034(4) C37 0.069(5) 0.045(4) 0.033(3) -0.001(3) 0.002(3) -0.032(3) C38 0.050(4) 0.033(3) 0.029(3) 0.000(2) -0.004(3) -0.017(3) C39 0.036(3) 0.033(3) 0.024(3) 0.010(2) -0.013(2) -0.016(2) C40 0.035(3) 0.043(3) 0.037(3) 0.013(3) -0.011(3) -0.007(3) C41 0.035(3) 0.048(3) 0.029(3) 0.012(2) -0.004(2) -0.011(3) C42 0.040(3) 0.037(3) 0.027(3) 0.002(2) -0.014(2) -0.005(2) C43 0.039(3) 0.040(3) 0.026(3) 0.005(2) -0.007(2) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.036(4) . ? Zn1 N3 2.039(4) . ? Zn1 N1 2.039(4) . ? Zn1 N2 2.041(4) . ? Zn1 O1 2.356(9) . ? Zn2 N8 2.056(4) . ? Zn2 N5 2.077(4) 2_656 ? Zn2 I2 2.5581(8) . ? Zn2 I1 2.5629(8) . ? N1 C4 1.373(7) . ? N1 C1 1.392(6) . ? N2 C6 1.366(6) . ? N2 C9 1.382(6) . ? N3 C11 1.382(6) . ? N3 C14 1.383(6) . ? N4 C16 1.364(6) . ? N4 C19 1.391(6) . ? N5 C23 1.349(7) . ? N5 C24 1.361(7) . ? N5 Zn2 2.077(4) 2_656 ? C45 C32 1.376(9) . ? C45 C31 1.393(9) . ? C45 H45 0.9500 . ? C46 C36 1.361(11) . ? C46 C37 1.390(11) . ? C46 H46 0.9500 . ? N8 C42 1.332(7) . ? N8 C41 1.336(8) . ? C1 C20 1.401(7) . ? C1 C2 1.441(7) . ? C2 C3 1.347(8) . ? C2 H2 0.9500 . ? C3 C4 1.444(7) . ? C3 H3 0.9500 . ? C4 C5 1.411(7) . ? C5 C6 1.424(7) . ? C5 C21 1.490(7) . ? C6 C7 1.428(7) . ? C7 C8 1.387(7) . ? C7 H7 0.9500 . ? C8 C9 1.451(7) . ? C8 H8 0.9500 . ? C9 C10 1.398(7) . ? C10 C11 1.410(7) . ? C10 C29 1.496(7) . ? C11 C12 1.444(7) . ? C12 C13 1.369(7) . ? C12 H12 0.9500 . ? C13 C14 1.448(7) . ? C13 H13 0.9500 . ? C14 C15 1.422(7) . ? C15 C16 1.408(7) . ? C15 C34 1.501(7) . ? C16 C17 1.444(7) . ? C17 C18 1.346(7) . ? C17 H17 0.9500 . ? C18 C19 1.425(7) . ? C18 H18 0.9500 . ? C19 C20 1.394(7) . ? C20 C39 1.509(7) . ? C21 C25 1.376(7) . ? C21 C22 1.398(8) . ? C22 C23 1.383(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.372(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C29 C30 1.380(8) . ? C29 C33 1.408(8) . ? C30 C31 1.387(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.381(8) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C38 1.387(9) . ? C34 C35 1.397(9) . ? C35 C36 1.392(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.412(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C43 1.381(8) . ? C39 C40 1.399(8) . ? C40 C41 1.376(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.382(7) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? O1 C44 1.470(16) . ? C44 C48 2.003(19) . ? O2 C48 1.620(16) . ? 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 N4 Zn1 N3 89.76(16) . . ? N4 Zn1 N1 90.62(16) . . ? N3 Zn1 N1 173.53(19) . . ? N4 Zn1 N2 178.55(18) . . ? N3 Zn1 N2 89.46(16) . . ? N1 Zn1 N2 90.02(16) . . ? N4 Zn1 O1 84.1(3) . . ? N3 Zn1 O1 99.6(3) . . ? N1 Zn1 O1 86.9(3) . . ? N2 Zn1 O1 97.3(3) . . ? N8 Zn2 N5 101.29(17) . 2_656 ? N8 Zn2 I2 109.82(14) . . ? N5 Zn2 I2 105.34(13) 2_656 . ? N8 Zn2 I1 108.93(14) . . ? N5 Zn2 I1 108.26(13) 2_656 . ? I2 Zn2 I1 121.30(3) . . ? C4 N1 C1 106.4(4) . . ? C4 N1 Zn1 127.2(3) . . ? C1 N1 Zn1 126.4(3) . . ? C6 N2 C9 106.2(4) . . ? C6 N2 Zn1 126.4(3) . . ? C9 N2 Zn1 126.3(3) . . ? C11 N3 C14 106.4(4) . . ? C11 N3 Zn1 126.8(3) . . ? C14 N3 Zn1 126.6(3) . . ? C16 N4 C19 106.2(4) . . ? C16 N4 Zn1 127.4(3) . . ? C19 N4 Zn1 125.9(3) . . ? C23 N5 C24 116.0(4) . . ? C23 N5 Zn2 123.0(4) . 2_656 ? C24 N5 Zn2 121.0(4) . 2_656 ? C32 C45 C31 120.0(5) . . ? C32 C45 H45 120.0 . . ? C31 C45 H45 120.0 . . ? C36 C46 C37 120.2(6) . . ? C36 C46 H46 119.9 . . ? C37 C46 H46 119.9 . . ? C42 N8 C41 116.8(5) . . ? C42 N8 Zn2 120.9(4) . . ? C41 N8 Zn2 122.1(4) . . ? N1 C1 C20 124.4(5) . . ? N1 C1 C2 109.1(5) . . ? C20 C1 C2 126.5(5) . . ? C3 C2 C1 107.4(5) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.5(5) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 125.1(5) . . ? N1 C4 C3 109.5(5) . . ? C5 C4 C3 125.4(5) . . ? C4 C5 C6 124.6(5) . . ? C4 C5 C21 117.4(5) . . ? C6 C5 C21 117.8(4) . . ? N2 C6 C5 125.4(5) . . ? N2 C6 C7 111.4(4) . . ? C5 C6 C7 123.1(5) . . ? C8 C7 C6 106.2(5) . . ? C8 C7 H7 126.9 . . ? C6 C7 H7 126.9 . . ? C7 C8 C9 106.4(5) . . ? C7 C8 H8 126.8 . . ? C9 C8 H8 126.8 . . ? N2 C9 C10 125.7(4) . . ? N2 C9 C8 109.6(4) . . ? C10 C9 C8 124.7(5) . . ? C9 C10 C11 124.1(5) . . ? C9 C10 C29 118.6(4) . . ? C11 C10 C29 117.3(4) . . ? N3 C11 C10 125.5(5) . . ? N3 C11 C12 109.7(4) . . ? C10 C11 C12 124.8(5) . . ? C13 C12 C11 107.3(5) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 106.7(4) . . ? C12 C13 H13 126.7 . . ? C14 C13 H13 126.7 . . ? N3 C14 C15 125.3(5) . . ? N3 C14 C13 109.9(4) . . ? C15 C14 C13 124.8(5) . . ? C16 C15 C14 124.3(5) . . ? C16 C15 C34 117.7(4) . . ? C14 C15 C34 118.0(5) . . ? N4 C16 C15 125.4(4) . . ? N4 C16 C17 109.5(4) . . ? C15 C16 C17 125.1(5) . . ? C18 C17 C16 107.3(5) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 107.5(5) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? C20 C19 N4 124.6(4) . . ? C20 C19 C18 125.8(5) . . ? N4 C19 C18 109.5(4) . . ? C19 C20 C1 126.9(5) . . ? C19 C20 C39 116.9(4) . . ? C1 C20 C39 116.3(4) . . ? C25 C21 C22 117.4(5) . . ? C25 C21 C5 120.6(5) . . ? C22 C21 C5 122.0(5) . . ? C23 C22 C21 118.7(5) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? N5 C23 C22 124.1(5) . . ? N5 C23 H23 117.9 . . ? C22 C23 H23 117.9 . . ? N5 C24 C25 122.9(5) . . ? N5 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C24 C25 C21 120.7(5) . . ? C24 C25 H25 119.6 . . ? C21 C25 H25 119.6 . . ? C30 C29 C33 117.9(5) . . ? C30 C29 C10 122.3(5) . . ? C33 C29 C10 119.8(5) . . ? C29 C30 C31 122.1(5) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C45 118.9(5) . . ? C30 C31 H31 120.5 . . ? C45 C31 H31 120.5 . . ? C45 C32 C33 120.8(6) . . ? C45 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C29 120.3(5) . . ? C32 C33 H33 119.9 . . ? C29 C33 H33 119.9 . . ? C38 C34 C35 118.5(5) . . ? C38 C34 C15 119.5(5) . . ? C35 C34 C15 121.9(5) . . ? C34 C35 C36 120.4(7) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C46 C36 C35 121.0(7) . . ? C46 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C46 C37 C38 119.1(7) . . ? C46 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C34 C38 C37 120.7(6) . . ? C34 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C43 C39 C40 117.2(5) . . ? C43 C39 C20 121.8(5) . . ? C40 C39 C20 120.9(5) . . ? C41 C40 C39 118.9(5) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? N8 C41 C40 123.9(5) . . ? N8 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? N8 C42 C43 123.4(5) . . ? N8 C42 H42 118.3 . . ? C43 C42 H42 118.3 . . ? C39 C43 C42 119.6(5) . . ? C39 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C44 O1 Zn1 142.3(7) . . ? O1 C44 C48 92.6(8) . . ? O2 C48 C44 105.4(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.739 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.190 # Attachment 'compound 3.cif' data_e407a _database_code_depnum_ccdc_archive 'CCDC 611786' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H58 Cd2 Cl6 I4 N12' _chemical_formula_weight 2204.54 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8032(3) _cell_length_b 12.5002(4) _cell_length_c 17.7426(5) _cell_angle_alpha 86.910(2) _cell_angle_beta 75.7380(10) _cell_angle_gamma 86.087(2) _cell_volume 2100.74(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7294 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 30.07 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 2.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6070 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 42891 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.07 _reflns_number_total 12098 _reflns_number_gt 9508 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+2.0000P] 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 12098 _refine_ls_number_parameters 490 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.85476(3) 0.47416(2) 0.398888(15) 0.02441(8) Uani 1 1 d . . 1 I1 I 0.70910(3) 0.66557(2) 0.423969(18) 0.03639(9) Uani 1 1 d . A 1 I2 I 1.12265(3) 0.42885(3) 0.317281(18) 0.03916(10) Uani 1 1 d . B 1 N1 N 0.4222(3) 0.1629(2) 0.10344(17) 0.0178(5) Uani 1 1 d . C 1 H1A H 0.3972 0.0961 0.1104 0.021 Uiso 1 1 calc R C 1 N2 N 0.3729(3) 0.0107(2) 0.23631(17) 0.0200(6) Uani 1 1 d . C 1 N3 N 0.2238(3) -0.1218(2) 0.15591(16) 0.0178(5) Uani 1 1 d . C 1 H3A H 0.2724 -0.0641 0.1433 0.021 Uiso 1 1 calc R C 1 N4 N 0.2934(3) 0.0209(2) 0.01921(17) 0.0178(5) Uani 1 1 d . C 1 C1 C 0.4205(4) 0.2285(3) 0.03902(19) 0.0175(6) Uani 1 1 d . C 1 C2 C 0.4614(4) 0.3326(3) 0.0526(2) 0.0225(7) Uani 1 1 d . C 1 H2 H 0.4653 0.3943 0.0187 0.027 Uiso 1 1 calc R C 1 C3 C 0.4935(4) 0.3265(3) 0.1232(2) 0.0231(7) Uani 1 1 d . C 1 H3 H 0.5258 0.3828 0.1470 0.028 Uiso 1 1 calc R C 1 C4 C 0.4696(4) 0.2196(3) 0.1551(2) 0.0189(6) Uani 1 1 d . C 1 C5 C 0.4898(4) 0.1801(3) 0.2281(2) 0.0193(6) Uani 1 1 d . C 1 C6 C 0.4488(4) 0.0820(3) 0.2640(2) 0.0224(7) Uani 1 1 d . C 1 C7 C 0.4752(5) 0.0391(3) 0.3365(2) 0.0312(9) Uani 1 1 d . C 1 H7 H 0.5281 0.0708 0.3667 0.037 Uiso 1 1 calc R C 1 C8 C 0.4103(5) -0.0554(4) 0.3537(2) 0.0318(9) Uani 1 1 d . C 1 H8 H 0.4082 -0.1011 0.3985 0.038 Uiso 1 1 calc R C 1 C9 C 0.3453(4) -0.0727(3) 0.2908(2) 0.0219(7) Uani 1 1 d . C 1 C10 C 0.2585(4) -0.1565(3) 0.2889(2) 0.0198(7) Uani 1 1 d . C 1 C11 C 0.1975(4) -0.1753(3) 0.2266(2) 0.0198(6) Uani 1 1 d . C 1 C12 C 0.1108(4) -0.2627(3) 0.2249(2) 0.0224(7) Uani 1 1 d . C 1 H12 H 0.0762 -0.3124 0.2666 0.027 Uiso 1 1 calc R C 1 C13 C 0.0875(4) -0.2612(3) 0.1522(2) 0.0216(7) Uani 1 1 d . C 1 H13 H 0.0326 -0.3091 0.1339 0.026 Uiso 1 1 calc R C 1 C14 C 0.1620(4) -0.1730(3) 0.1079(2) 0.0187(6) Uani 1 1 d . C 1 C15 C 0.1721(3) -0.1477(3) 0.02792(19) 0.0168(6) Uani 1 1 d . C 1 C16 C 0.2369(4) -0.0580(3) -0.01276(19) 0.0172(6) Uani 1 1 d . C 1 C17 C 0.2489(4) -0.0309(3) -0.0943(2) 0.0213(7) Uani 1 1 d . C 1 H17 H 0.2199 -0.0725 -0.1302 0.026 Uiso 1 1 calc R C 1 C18 C 0.3096(4) 0.0652(3) -0.1100(2) 0.0213(7) Uani 1 1 d . C 1 H18 H 0.3313 0.1031 -0.1590 0.026 Uiso 1 1 calc R C 1 C19 C 0.3345(4) 0.0984(3) -0.03831(19) 0.0181(6) Uani 1 1 d . C 1 C20 C 0.3856(4) 0.1986(3) -0.02838(19) 0.0165(6) Uani 1 1 d . C 1 C21 C 0.5670(4) 0.2492(3) 0.26758(19) 0.0195(7) Uani 1 1 d . C 1 C22 C 0.5067(4) 0.2882(3) 0.3419(2) 0.0234(7) Uani 1 1 d . C 1 H22 H 0.4130 0.2726 0.3681 0.028 Uiso 1 1 calc R C 1 C23 C 0.5846(4) 0.3493(3) 0.3766(2) 0.0273(8) Uani 1 1 d . C 1 H23 H 0.5417 0.3761 0.4265 0.033 Uiso 1 1 calc R C 1 N5 N 0.7189(3) 0.3728(3) 0.34288(17) 0.0213(6) Uani 1 1 d . C 1 C24 C 0.7772(4) 0.3362(3) 0.2714(2) 0.0224(7) Uani 1 1 d . C 1 H24 H 0.8713 0.3525 0.2466 0.027 Uiso 1 1 calc R C 1 C25 C 0.7040(4) 0.2749(3) 0.2324(2) 0.0224(7) Uani 1 1 d . C 1 H25 H 0.7481 0.2510 0.1818 0.027 Uiso 1 1 calc R C 1 C26 C 0.2284(4) -0.2323(3) 0.3573(2) 0.0211(7) Uani 1 1 d . C 1 C27 C 0.0945(4) -0.2377(3) 0.4063(2) 0.0269(8) Uani 1 1 d . C 1 H27 H 0.0183 -0.1928 0.3962 0.032 Uiso 1 1 calc R C 1 C28 C 0.0727(4) -0.3095(3) 0.4705(2) 0.0269(8) Uani 1 1 d . C 1 H28 H -0.0194 -0.3121 0.5037 0.032 Uiso 1 1 calc R C 1 N6 N 0.1764(4) -0.3752(3) 0.48742(18) 0.0244(6) Uani 1 1 d . . 1 C29 C 0.3044(4) -0.3723(3) 0.4394(2) 0.0254(7) Uani 1 1 d . C 1 H29 H 0.3774 -0.4206 0.4496 0.030 Uiso 1 1 calc R C 1 C30 C 0.3358(4) -0.3017(3) 0.3750(2) 0.0250(7) Uani 1 1 d . C 1 H30 H 0.4292 -0.3005 0.3433 0.030 Uiso 1 1 calc R C 1 C31 C 0.1072(4) -0.2220(3) -0.01489(19) 0.0191(6) Uani 1 1 d . C 1 C32 C 0.1509(4) -0.3307(3) -0.0183(2) 0.0262(8) Uani 1 1 d . C 1 H32 H 0.2231 -0.3575 0.0060 0.031 Uiso 1 1 calc R C 1 C33 C 0.0888(5) -0.4001(4) -0.0573(3) 0.0348(10) Uani 1 1 d . C 1 H33 H 0.1188 -0.4740 -0.0591 0.042 Uiso 1 1 calc R C 1 C34 C -0.0161(5) -0.3624(4) -0.0935(2) 0.0395(11) Uani 1 1 d . C 1 H34 H -0.0592 -0.4103 -0.1191 0.047 Uiso 1 1 calc R C 1 C35 C -0.0582(4) -0.2535(4) -0.0921(2) 0.0347(10) Uani 1 1 d . C 1 H35 H -0.1283 -0.2268 -0.1180 0.042 Uiso 1 1 calc R C 1 C36 C 0.0027(4) -0.1836(4) -0.0527(2) 0.0257(8) Uani 1 1 d . C 1 H36 H -0.0269 -0.1096 -0.0515 0.031 Uiso 1 1 calc R C 1 C37 C 0.3980(4) 0.2798(3) -0.09419(19) 0.0178(6) Uani 1 1 d . C 1 C38 C 0.2795(4) 0.3109(3) -0.1237(2) 0.0250(7) Uani 1 1 d . C 1 H38 H 0.1914 0.2812 -0.1011 0.030 Uiso 1 1 calc R C 1 C39 C 0.2920(5) 0.3853(3) -0.1860(2) 0.0305(9) Uani 1 1 d . C 1 H39 H 0.2124 0.4058 -0.2061 0.037 Uiso 1 1 calc R C 1 C40 C 0.4198(5) 0.4294(3) -0.2186(2) 0.0296(8) Uani 1 1 d . C 1 H40 H 0.4278 0.4795 -0.2615 0.035 Uiso 1 1 calc R C 1 C41 C 0.5354(4) 0.4011(3) -0.1894(2) 0.0278(8) Uani 1 1 d . C 1 H41 H 0.6226 0.4325 -0.2115 0.033 Uiso 1 1 calc R C 1 C42 C 0.5243(4) 0.3259(3) -0.1272(2) 0.0221(7) Uani 1 1 d . C 1 H42 H 0.6045 0.3063 -0.1074 0.027 Uiso 1 1 calc R C 1 C43A C 0.9507(9) 0.1243(8) 0.3646(5) 0.053(2) Uiso 0.657(4) 1 d PD D 1 H43A H 0.9589 0.2026 0.3507 0.063 Uiso 0.657(4) 1 calc PR D 1 Cl1A Cl 0.7885(3) 0.1128(3) 0.42719(16) 0.0649(7) Uiso 0.657(4) 1 d PD D 1 Cl2A Cl 0.9761(4) 0.0599(3) 0.2758(2) 0.0879(10) Uiso 0.657(4) 1 d PD D 1 Cl3A Cl 1.0927(3) 0.0849(2) 0.40582(16) 0.0677(8) Uiso 0.657(4) 1 d PD D 1 C43B C 0.946(2) 0.0361(19) 0.3596(11) 0.1188(19) Uiso 0.343(4) 1 d PD D 2 H43B H 1.0108 -0.0224 0.3742 0.143 Uiso 0.343(4) 1 calc PR D 2 Cl2B Cl 0.8908(10) -0.0002(8) 0.2843(6) 0.1188(19) Uiso 0.343(4) 1 d PD D 2 Cl1B Cl 0.8009(10) 0.0523(9) 0.4338(6) 0.1188(19) Uiso 0.343(4) 1 d PD D 2 Cl3B Cl 1.0334(11) 0.1503(8) 0.3369(6) 0.1188(19) Uiso 0.343(4) 1 d PD D 2 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 0.02916(15) 0.02554(15) 0.02097(13) 0.00530(10) -0.00934(10) -0.01175(11) I1 0.02973(15) 0.03544(17) 0.04478(17) -0.00117(12) -0.01058(12) -0.00198(12) I2 0.02844(15) 0.04465(19) 0.04185(17) 0.00598(13) -0.00369(12) -0.00825(13) N1 0.0209(14) 0.0150(13) 0.0192(13) 0.0048(10) -0.0081(11) -0.0052(11) N2 0.0227(15) 0.0195(14) 0.0190(13) 0.0047(11) -0.0063(11) -0.0096(12) N3 0.0214(14) 0.0158(13) 0.0176(13) 0.0050(10) -0.0070(11) -0.0063(11) N4 0.0198(13) 0.0145(13) 0.0198(13) 0.0033(10) -0.0060(11) -0.0042(11) C1 0.0153(14) 0.0176(16) 0.0196(15) 0.0043(12) -0.0046(12) -0.0037(12) C2 0.0276(18) 0.0188(17) 0.0223(16) 0.0028(13) -0.0084(14) -0.0047(14) C3 0.033(2) 0.0162(16) 0.0233(16) 0.0022(13) -0.0117(15) -0.0084(14) C4 0.0195(16) 0.0176(16) 0.0209(15) 0.0012(12) -0.0064(12) -0.0058(13) C5 0.0191(16) 0.0208(17) 0.0192(15) 0.0006(12) -0.0060(12) -0.0070(13) C6 0.0278(18) 0.0221(17) 0.0194(15) 0.0057(13) -0.0086(13) -0.0100(14) C7 0.044(2) 0.032(2) 0.0261(18) 0.0078(15) -0.0225(17) -0.0151(18) C8 0.044(2) 0.031(2) 0.0274(19) 0.0095(16) -0.0205(18) -0.0160(18) C9 0.0264(18) 0.0228(17) 0.0189(15) 0.0051(13) -0.0093(13) -0.0086(14) C10 0.0220(16) 0.0201(16) 0.0179(15) 0.0057(12) -0.0058(13) -0.0064(13) C11 0.0191(16) 0.0206(16) 0.0204(15) 0.0046(13) -0.0062(12) -0.0056(13) C12 0.0248(17) 0.0250(18) 0.0193(15) 0.0079(13) -0.0080(13) -0.0114(14) C13 0.0229(17) 0.0217(17) 0.0221(16) 0.0068(13) -0.0082(13) -0.0107(14) C14 0.0174(15) 0.0192(16) 0.0193(15) 0.0044(12) -0.0040(12) -0.0050(13) C15 0.0159(15) 0.0167(15) 0.0183(14) 0.0003(12) -0.0053(12) -0.0007(12) C16 0.0177(15) 0.0167(15) 0.0177(14) -0.0005(12) -0.0056(12) 0.0002(12) C17 0.0271(18) 0.0209(17) 0.0161(14) 0.0002(12) -0.0051(13) -0.0043(14) C18 0.0271(18) 0.0208(17) 0.0160(14) 0.0000(12) -0.0048(13) -0.0022(14) C19 0.0188(15) 0.0185(16) 0.0174(14) 0.0036(12) -0.0058(12) -0.0017(13) C20 0.0189(15) 0.0148(15) 0.0160(14) 0.0043(11) -0.0057(12) -0.0021(12) C21 0.0236(17) 0.0186(16) 0.0182(15) 0.0023(12) -0.0081(13) -0.0068(13) C22 0.0224(17) 0.0286(19) 0.0187(15) 0.0005(13) -0.0026(13) -0.0086(15) C23 0.031(2) 0.032(2) 0.0190(16) -0.0010(14) -0.0052(14) -0.0069(17) N5 0.0237(15) 0.0229(15) 0.0192(13) 0.0014(11) -0.0083(11) -0.0067(12) C24 0.0228(17) 0.0253(18) 0.0196(15) 0.0007(13) -0.0041(13) -0.0090(14) C25 0.0231(17) 0.0261(18) 0.0187(15) -0.0025(13) -0.0047(13) -0.0064(14) C26 0.0281(18) 0.0209(17) 0.0162(14) 0.0062(12) -0.0085(13) -0.0088(14) C27 0.0231(18) 0.033(2) 0.0245(17) 0.0085(15) -0.0078(14) -0.0015(16) C28 0.0227(18) 0.035(2) 0.0225(17) 0.0077(15) -0.0048(14) -0.0080(16) N6 0.0293(16) 0.0263(16) 0.0194(14) 0.0076(12) -0.0084(12) -0.0113(13) C29 0.0273(19) 0.0275(19) 0.0232(17) 0.0034(14) -0.0110(14) 0.0001(15) C30 0.0224(17) 0.030(2) 0.0210(16) 0.0037(14) -0.0029(13) -0.0029(15) C31 0.0183(15) 0.0217(17) 0.0174(14) 0.0003(12) -0.0035(12) -0.0059(13) C32 0.031(2) 0.0219(18) 0.0234(17) 0.0010(14) -0.0018(15) -0.0082(15) C33 0.043(2) 0.026(2) 0.030(2) -0.0053(16) 0.0065(17) -0.0172(18) C34 0.041(2) 0.053(3) 0.0247(19) -0.0079(18) 0.0012(17) -0.032(2) C35 0.0222(19) 0.061(3) 0.0220(18) -0.0055(18) -0.0032(14) -0.0147(19) C36 0.0171(16) 0.039(2) 0.0209(16) -0.0027(15) -0.0034(13) -0.0036(15) C37 0.0195(16) 0.0158(15) 0.0183(14) 0.0041(12) -0.0057(12) -0.0024(13) C38 0.0260(18) 0.0250(18) 0.0255(17) 0.0067(14) -0.0101(14) -0.0036(15) C39 0.035(2) 0.032(2) 0.0264(18) 0.0064(16) -0.0148(16) 0.0044(17) C40 0.044(2) 0.0214(18) 0.0213(17) 0.0087(14) -0.0059(16) -0.0012(17) C41 0.031(2) 0.0245(19) 0.0234(17) 0.0063(14) 0.0024(15) -0.0074(16) C42 0.0225(17) 0.0198(17) 0.0237(16) 0.0025(13) -0.0052(13) -0.0027(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 Cd1 N6 2.274(3) 2_656 ? Cd1 N5 2.321(3) . ? Cd1 I1 2.7013(4) . ? Cd1 I2 2.7066(4) . ? N1 C4 1.373(4) . ? N1 C1 1.373(4) . ? N1 H1A 0.8800 . ? N2 C9 1.376(5) . ? N2 C6 1.381(4) . ? N3 C11 1.365(4) . ? N3 C14 1.367(4) . ? N3 H3A 0.8800 . ? N4 C19 1.373(4) . ? N4 C16 1.376(4) . ? C1 C20 1.398(4) . ? C1 C2 1.437(5) . ? C2 C3 1.361(5) . ? C2 H2 0.9500 . ? C3 C4 1.435(5) . ? C3 H3 0.9500 . ? C4 C5 1.415(5) . ? C5 C6 1.388(5) . ? C5 C21 1.492(4) . ? C6 C7 1.442(5) . ? C7 C8 1.364(6) . ? C7 H7 0.9500 . ? C8 C9 1.448(5) . ? C8 H8 0.9500 . ? C9 C10 1.401(5) . ? C10 C11 1.416(5) . ? C10 C26 1.481(5) . ? C11 C12 1.435(5) . ? C12 C13 1.364(5) . ? C12 H12 0.9500 . ? C13 C14 1.449(5) . ? C13 H13 0.9500 . ? C14 C15 1.418(5) . ? C15 C16 1.402(5) . ? C15 C31 1.496(4) . ? C16 C17 1.445(5) . ? C17 C18 1.361(5) . ? C17 H17 0.9500 . ? C18 C19 1.441(4) . ? C18 H18 0.9500 . ? C19 C20 1.416(5) . ? C20 C37 1.492(5) . ? C21 C25 1.386(5) . ? C21 C22 1.403(5) . ? C22 C23 1.381(5) . ? C22 H22 0.9500 . ? C23 N5 1.350(5) . ? C23 H23 0.9500 . ? N5 C24 1.347(5) . ? C24 C25 1.399(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.388(5) . ? C26 C30 1.404(5) . ? C27 C28 1.394(5) . ? C27 H27 0.9500 . ? C28 N6 1.344(5) . ? C28 H28 0.9500 . ? N6 C29 1.334(5) . ? N6 Cd1 2.274(3) 2_656 ? C29 C30 1.390(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.396(5) . ? C31 C36 1.403(5) . ? C32 C33 1.395(5) . ? C32 H32 0.9500 . ? C33 C34 1.386(7) . ? C33 H33 0.9500 . ? C34 C35 1.394(7) . ? C34 H34 0.9500 . ? C35 C36 1.397(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.382(5) . ? C37 C38 1.411(5) . ? C38 C39 1.392(5) . ? C38 H38 0.9500 . ? C39 C40 1.382(6) . ? C39 H39 0.9500 . ? C40 C41 1.376(6) . ? C40 H40 0.9500 . ? C41 C42 1.399(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43A Cl1A 1.710(9) . ? C43A Cl3A 1.756(9) . ? C43A Cl2A 1.764(9) . ? C43A H43A 1.0000 . ? C43B Cl2B 1.656(17) . ? C43B Cl3B 1.692(17) . ? C43B Cl1B 1.695(17) . ? C43B H43B 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cd1 N5 95.98(11) 2_656 . ? N6 Cd1 I1 109.69(9) 2_656 . ? N5 Cd1 I1 105.00(8) . . ? N6 Cd1 I2 106.83(9) 2_656 . ? N5 Cd1 I2 104.33(8) . . ? I1 Cd1 I2 129.681(14) . . ? C4 N1 C1 108.1(3) . . ? C4 N1 H1A 125.9 . . ? C1 N1 H1A 125.9 . . ? C9 N2 C6 107.2(3) . . ? C11 N3 C14 108.5(3) . . ? C11 N3 H3A 125.8 . . ? C14 N3 H3A 125.8 . . ? C19 N4 C16 107.1(3) . . ? N1 C1 C20 125.7(3) . . ? N1 C1 C2 108.4(3) . . ? C20 C1 C2 125.9(3) . . ? C3 C2 C1 107.4(3) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.6(3) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 126.0(3) . . ? N1 C4 C3 108.4(3) . . ? C5 C4 C3 125.6(3) . . ? C6 C5 C4 125.7(3) . . ? C6 C5 C21 117.9(3) . . ? C4 C5 C21 116.3(3) . . ? N2 C6 C5 125.0(3) . . ? N2 C6 C7 109.0(3) . . ? C5 C6 C7 126.0(3) . . ? C8 C7 C6 107.5(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.9(3) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N2 C9 C10 125.4(3) . . ? N2 C9 C8 109.3(3) . . ? C10 C9 C8 125.1(3) . . ? C9 C10 C11 125.3(3) . . ? C9 C10 C26 117.6(3) . . ? C11 C10 C26 117.1(3) . . ? N3 C11 C10 125.9(3) . . ? N3 C11 C12 108.9(3) . . ? C10 C11 C12 124.7(3) . . ? C13 C12 C11 107.2(3) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 107.2(3) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N3 C14 C15 126.6(3) . . ? N3 C14 C13 108.1(3) . . ? C15 C14 C13 125.3(3) . . ? C16 C15 C14 124.5(3) . . ? C16 C15 C31 118.5(3) . . ? C14 C15 C31 117.0(3) . . ? N4 C16 C15 125.5(3) . . ? N4 C16 C17 109.0(3) . . ? C15 C16 C17 125.4(3) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 106.9(3) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? N4 C19 C20 125.7(3) . . ? N4 C19 C18 109.5(3) . . ? C20 C19 C18 124.7(3) . . ? C1 C20 C19 125.1(3) . . ? C1 C20 C37 117.7(3) . . ? C19 C20 C37 117.1(3) . . ? C25 C21 C22 117.4(3) . . ? C25 C21 C5 120.5(3) . . ? C22 C21 C5 122.0(3) . . ? C23 C22 C21 119.5(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N5 C23 C22 123.1(3) . . ? N5 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? C24 N5 C23 117.7(3) . . ? C24 N5 Cd1 117.8(2) . . ? C23 N5 Cd1 124.4(2) . . ? N5 C24 C25 122.3(3) . . ? N5 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C21 C25 C24 120.0(3) . . ? C21 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C30 117.3(3) . . ? C27 C26 C10 122.0(3) . . ? C30 C26 C10 120.7(3) . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N6 C28 C27 122.8(4) . . ? N6 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C29 N6 C28 118.0(3) . . ? C29 N6 Cd1 119.7(3) . 2_656 ? C28 N6 Cd1 121.9(3) . 2_656 ? N6 C29 C30 122.9(4) . . ? N6 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C29 C30 C26 119.4(4) . . ? C29 C30 H30 120.3 . . ? C26 C30 H30 120.3 . . ? C32 C31 C36 119.0(3) . . ? C32 C31 C15 120.4(3) . . ? C36 C31 C15 120.6(3) . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.7(4) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.3(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C37 C38 118.8(3) . . ? C42 C37 C20 121.2(3) . . ? C38 C37 C20 120.0(3) . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.2(4) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 120.4(4) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 119.8(4) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C37 C42 C41 120.8(3) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? Cl1A C43A Cl3A 114.2(5) . . ? Cl1A C43A Cl2A 115.5(5) . . ? Cl3A C43A Cl2A 108.4(5) . . ? Cl1A C43A H43A 106.0 . . ? Cl3A C43A H43A 106.0 . . ? Cl2A C43A H43A 106.0 . . ? Cl2B C43B Cl3B 110.3(13) . . ? Cl2B C43B Cl1B 106.4(12) . . ? Cl3B C43B Cl1B 111.9(14) . . ? Cl2B C43B H43B 109.4 . . ? Cl3B C43B H43B 109.4 . . ? Cl1B C43B H43B 109.4 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.997 _refine_diff_density_min -1.551 _refine_diff_density_rms 0.147 # Attachment 'compound 4.cif' data_e551a _database_code_depnum_ccdc_archive 'CCDC 611787' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H56 Hg2 I4 N12, 2(C H Cl3)' _chemical_formula_sum 'C86 H58 Cl6 Hg2 I4 N12' _chemical_formula_weight 2380.92 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.8204(3) _cell_length_b 12.4299(3) _cell_length_c 17.7025(5) _cell_angle_alpha 86.5920(10) _cell_angle_beta 75.9920(10) _cell_angle_gamma 85.8720(10) _cell_volume 2089.21(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9232 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 5.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3845 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 32404 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9545 _reflns_number_gt 7255 _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^)+(0.0615P)^2^+2.3753P] 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 9545 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.87178(3) 0.48754(2) 0.393373(15) 0.02759(9) Uani 1 1 d . . . I2 I 1.12794(5) 0.41908(4) 0.31507(3) 0.03585(13) Uani 1 1 d . . . I3 I 0.70505(5) 0.66568(4) 0.42301(3) 0.03727(13) Uani 1 1 d . . . N1 N 0.5764(5) -0.1617(4) 0.8954(3) 0.0188(10) Uani 1 1 d . . . H1A H 0.6007 -0.0944 0.8884 0.023 Uiso 1 1 calc R . . N2 N 0.6261(5) -0.0080(4) 0.7623(3) 0.0184(10) Uani 1 1 d . . . N3 N 0.7763(5) 0.1222(4) 0.8435(3) 0.0174(10) Uani 1 1 d . . . H3A H 0.7275 0.0645 0.8566 0.021 Uiso 1 1 calc R . . N4 N 0.7053(5) -0.0206(4) 0.9808(3) 0.0174(10) Uani 1 1 d . . . C1 C 0.5798(6) -0.2280(4) 0.9600(3) 0.0176(12) Uani 1 1 d . . . C2 C 0.5372(6) -0.3327(5) 0.9469(4) 0.0229(13) Uani 1 1 d . . . H2 H 0.5320 -0.3946 0.9814 0.027 Uiso 1 1 calc R . . C3 C 0.5060(6) -0.3263(5) 0.8761(4) 0.0215(13) Uani 1 1 d . . . H3 H 0.4747 -0.3829 0.8520 0.026 Uiso 1 1 calc R . . C4 C 0.5291(6) -0.2178(4) 0.8443(4) 0.0191(12) Uani 1 1 d . . . C5 C 0.5078(6) -0.1779(5) 0.7721(3) 0.0187(12) Uani 1 1 d . . . C6 C 0.5490(6) -0.0783(5) 0.7350(4) 0.0204(12) Uani 1 1 d . . . C7 C 0.5238(7) -0.0336(5) 0.6630(4) 0.0272(14) Uani 1 1 d . . . H7 H 0.4704 -0.0644 0.6325 0.033 Uiso 1 1 calc R . . C8 C 0.5876(7) 0.0584(5) 0.6459(4) 0.0282(15) Uani 1 1 d . . . H8 H 0.5887 0.1044 0.6009 0.034 Uiso 1 1 calc R . . C9 C 0.6554(6) 0.0766(5) 0.7077(3) 0.0207(12) Uani 1 1 d . . . C10 C 0.7428(6) 0.1593(5) 0.7102(3) 0.0194(12) Uani 1 1 d . . . C11 C 0.8019(6) 0.1762(4) 0.7723(3) 0.0184(12) Uani 1 1 d . . . C12 C 0.8899(6) 0.2644(5) 0.7755(4) 0.0217(13) Uani 1 1 d . . . H12 H 0.9243 0.3151 0.7341 0.026 Uiso 1 1 calc R . . C13 C 0.9135(6) 0.2614(5) 0.8463(3) 0.0217(13) Uani 1 1 d . . . H13 H 0.9690 0.3089 0.8643 0.026 Uiso 1 1 calc R . . C14 C 0.8400(6) 0.1737(4) 0.8909(3) 0.0174(12) Uani 1 1 d . . . C15 C 0.8286(6) 0.1474(4) 0.9712(3) 0.0162(11) Uani 1 1 d . . . C16 C 0.7639(6) 0.0588(4) 1.0121(3) 0.0175(12) Uani 1 1 d . . . C17 C 0.7526(6) 0.0297(5) 1.0935(3) 0.0200(12) Uani 1 1 d . . . H17 H 0.7825 0.0709 1.1293 0.024 Uiso 1 1 calc R . . C18 C 0.6925(6) -0.0661(4) 1.1102(3) 0.0198(12) Uani 1 1 d . . . H18 H 0.6721 -0.1043 1.1594 0.024 Uiso 1 1 calc R . . C19 C 0.6649(6) -0.0993(4) 1.0379(3) 0.0184(12) Uani 1 1 d . . . C20 C 0.6150(6) -0.1993(4) 1.0272(3) 0.0168(12) Uani 1 1 d . . . C21 C 0.4299(6) -0.2467(4) 0.7317(3) 0.0196(12) Uani 1 1 d . . . C22 C 0.2947(6) -0.2733(4) 0.7678(3) 0.0193(12) Uani 1 1 d . . . H22 H 0.2518 -0.2496 0.8185 0.023 Uiso 1 1 calc R . . C23 C 0.2221(7) -0.3342(5) 0.7301(3) 0.0219(13) Uani 1 1 d . . . H23 H 0.1295 -0.3518 0.7562 0.026 Uiso 1 1 calc R . . N5 N 0.2758(5) -0.3700(4) 0.6583(3) 0.0239(11) Uani 1 1 d . . . C24 C 0.4074(7) -0.3471(5) 0.6237(4) 0.0242(13) Uani 1 1 d . . . H24 H 0.4481 -0.3740 0.5736 0.029 Uiso 1 1 calc R . . C25 C 0.4887(7) -0.2854(5) 0.6574(4) 0.0238(13) Uani 1 1 d . . . H25 H 0.5818 -0.2701 0.6305 0.029 Uiso 1 1 calc R . . C26 C 0.7748(6) 0.2353(5) 0.6408(3) 0.0197(12) Uani 1 1 d . . . C27 C 0.6702(6) 0.3093(5) 0.6229(3) 0.0215(13) Uani 1 1 d . . . H27 H 0.5775 0.3113 0.6552 0.026 Uiso 1 1 calc R . . C28 C 0.7032(7) 0.3784(5) 0.5588(4) 0.0260(14) Uani 1 1 d . . . H28 H 0.6317 0.4279 0.5475 0.031 Uiso 1 1 calc R . . N6 N 0.8327(5) 0.3790(4) 0.5112(3) 0.0229(11) Uani 1 1 d . . . C29 C 0.9325(7) 0.3084(5) 0.5282(4) 0.0261(14) Uani 1 1 d . . . H29 H 1.0243 0.3075 0.4948 0.031 Uiso 1 1 calc R . . C30 C 0.9072(6) 0.2380(5) 0.5915(3) 0.0225(13) Uani 1 1 d . . . H30 H 0.9814 0.1905 0.6018 0.027 Uiso 1 1 calc R . . C31 C 0.8944(6) 0.2216(5) 1.0142(3) 0.0182(12) Uani 1 1 d . . . C32 C 0.8495(7) 0.3314(5) 1.0174(4) 0.0250(14) Uani 1 1 d . . . H32 H 0.7767 0.3585 0.9933 0.030 Uiso 1 1 calc R . . C33 C 0.9130(7) 0.4006(5) 1.0566(4) 0.0295(15) Uani 1 1 d . . . H33 H 0.8839 0.4752 1.0585 0.035 Uiso 1 1 calc R . . C34 C 1.0173(8) 0.3611(6) 1.0925(4) 0.0379(19) Uani 1 1 d . . . H34 H 1.0609 0.4087 1.1181 0.045 Uiso 1 1 calc R . . C35 C 1.0581(7) 0.2541(6) 1.0912(4) 0.0327(16) Uani 1 1 d . . . H35 H 1.1281 0.2273 1.1175 0.039 Uiso 1 1 calc R . . C36 C 0.9986(6) 0.1830(5) 1.0519(4) 0.0224(13) Uani 1 1 d . . . H36 H 1.0289 0.1087 1.0509 0.027 Uiso 1 1 calc R . . C37 C 0.6022(6) -0.2818(4) 1.0937(3) 0.0170(12) Uani 1 1 d . . . C38 C 0.4749(6) -0.3275(5) 1.1274(4) 0.0222(13) Uani 1 1 d . . . H38 H 0.3948 -0.3077 1.1074 0.027 Uiso 1 1 calc R . . C39 C 0.4640(7) -0.4020(5) 1.1905(4) 0.0265(14) Uani 1 1 d . . . H39 H 0.3766 -0.4321 1.2136 0.032 Uiso 1 1 calc R . . C40 C 0.5801(8) -0.4318(5) 1.2190(4) 0.0299(15) Uani 1 1 d . . . H40 H 0.5728 -0.4831 1.2616 0.036 Uiso 1 1 calc R . . C41 C 0.7061(7) -0.3883(5) 1.1868(4) 0.0278(14) Uani 1 1 d . . . H41 H 0.7851 -0.4082 1.2077 0.033 Uiso 1 1 calc R . . C42 C 0.7192(7) -0.3142(5) 1.1227(4) 0.0242(13) Uani 1 1 d . . . H42 H 0.8078 -0.2863 1.0992 0.029 Uiso 1 1 calc R . . C43 C 0.0416(12) 0.8785(8) 0.6381(6) 0.070(3) Uani 1 1 d . . . H43 H 0.0391 0.7993 0.6518 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.0337(5) 0.9455(4) 0.7222(2) 0.143(2) Uani 1 1 d . . . Cl2 Cl -0.0927(3) 0.9150(2) 0.59480(18) 0.0802(8) Uani 1 1 d . . . Cl3 Cl 0.2079(3) 0.9026(3) 0.57000(19) 0.0949(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 Hg1 0.03212(16) 0.03142(14) 0.01972(15) 0.00605(9) -0.00689(11) -0.00862(10) I2 0.0263(2) 0.0448(3) 0.0337(3) 0.0065(2) -0.0016(2) -0.00938(19) I3 0.0303(3) 0.0406(3) 0.0411(3) -0.0011(2) -0.0093(2) -0.00076(19) N1 0.023(3) 0.020(2) 0.015(3) 0.0041(19) -0.007(2) -0.0055(19) N2 0.016(3) 0.022(2) 0.017(3) 0.0069(19) -0.004(2) -0.0069(19) N3 0.020(3) 0.018(2) 0.014(3) 0.0068(18) -0.004(2) -0.0061(19) N4 0.015(2) 0.019(2) 0.018(3) 0.0044(19) -0.004(2) -0.0041(18) C1 0.016(3) 0.019(3) 0.017(3) 0.003(2) -0.002(2) -0.004(2) C2 0.026(3) 0.020(3) 0.023(3) 0.005(2) -0.006(3) -0.005(2) C3 0.023(3) 0.023(3) 0.020(3) 0.004(2) -0.007(3) -0.009(2) C4 0.016(3) 0.023(3) 0.018(3) 0.003(2) -0.003(3) -0.007(2) C5 0.016(3) 0.026(3) 0.014(3) 0.000(2) -0.003(2) -0.005(2) C6 0.019(3) 0.027(3) 0.017(3) 0.001(2) -0.006(3) -0.005(2) C7 0.033(4) 0.036(3) 0.018(3) 0.008(3) -0.014(3) -0.016(3) C8 0.038(4) 0.038(3) 0.014(3) 0.012(3) -0.017(3) -0.014(3) C9 0.020(3) 0.028(3) 0.013(3) 0.006(2) -0.004(3) -0.006(2) C10 0.017(3) 0.027(3) 0.013(3) 0.005(2) -0.002(2) -0.001(2) C11 0.017(3) 0.021(3) 0.017(3) 0.004(2) -0.002(2) -0.004(2) C12 0.018(3) 0.022(3) 0.024(3) 0.008(2) -0.002(3) -0.012(2) C13 0.022(3) 0.029(3) 0.015(3) 0.005(2) -0.006(3) -0.010(2) C14 0.014(3) 0.023(3) 0.015(3) 0.004(2) -0.003(2) -0.006(2) C15 0.014(3) 0.020(3) 0.014(3) 0.002(2) -0.002(2) -0.002(2) C16 0.017(3) 0.024(3) 0.010(3) 0.002(2) -0.001(2) -0.001(2) C17 0.021(3) 0.028(3) 0.009(3) -0.002(2) -0.002(2) -0.001(2) C18 0.023(3) 0.025(3) 0.010(3) 0.005(2) -0.002(3) -0.004(2) C19 0.017(3) 0.023(3) 0.015(3) 0.004(2) -0.004(2) -0.001(2) C20 0.019(3) 0.018(3) 0.014(3) 0.005(2) -0.004(2) -0.004(2) C21 0.023(3) 0.021(3) 0.018(3) 0.004(2) -0.010(3) -0.004(2) C22 0.018(3) 0.025(3) 0.011(3) 0.000(2) 0.003(2) -0.003(2) C23 0.023(3) 0.028(3) 0.014(3) 0.003(2) -0.002(3) -0.007(2) N5 0.025(3) 0.030(3) 0.018(3) 0.001(2) -0.007(2) -0.010(2) C24 0.028(4) 0.033(3) 0.013(3) -0.004(2) -0.004(3) -0.005(3) C25 0.022(3) 0.036(3) 0.013(3) 0.005(2) -0.004(3) -0.007(3) C26 0.022(3) 0.025(3) 0.014(3) 0.002(2) -0.007(3) -0.008(2) C27 0.021(3) 0.028(3) 0.014(3) 0.003(2) -0.002(3) -0.006(2) C28 0.033(4) 0.028(3) 0.017(3) 0.004(2) -0.009(3) 0.002(3) N6 0.026(3) 0.029(3) 0.015(3) 0.005(2) -0.007(2) -0.007(2) C29 0.021(3) 0.037(3) 0.020(3) 0.005(3) -0.004(3) -0.006(3) C30 0.021(3) 0.031(3) 0.015(3) 0.008(2) -0.006(3) -0.002(2) C31 0.017(3) 0.029(3) 0.007(3) 0.002(2) 0.002(2) -0.006(2) C32 0.030(4) 0.022(3) 0.017(3) 0.004(2) 0.006(3) -0.006(2) C33 0.043(4) 0.031(3) 0.013(3) 0.001(3) 0.003(3) -0.021(3) C34 0.039(4) 0.053(4) 0.021(4) -0.011(3) 0.006(3) -0.034(4) C35 0.014(3) 0.065(5) 0.018(4) 0.004(3) 0.003(3) -0.018(3) C36 0.015(3) 0.036(3) 0.016(3) 0.002(2) -0.002(3) -0.005(2) C37 0.020(3) 0.018(3) 0.014(3) 0.002(2) -0.006(2) -0.003(2) C38 0.021(3) 0.023(3) 0.021(3) 0.001(2) -0.003(3) 0.000(2) C39 0.025(3) 0.025(3) 0.025(4) 0.004(3) 0.003(3) -0.007(2) C40 0.047(4) 0.026(3) 0.014(3) 0.011(2) -0.006(3) -0.002(3) C41 0.030(4) 0.036(3) 0.018(3) 0.011(3) -0.011(3) 0.001(3) C42 0.026(3) 0.026(3) 0.021(3) 0.004(2) -0.007(3) -0.002(2) C43 0.104(8) 0.050(5) 0.062(7) -0.002(4) -0.039(6) 0.024(5) Cl1 0.198(4) 0.160(4) 0.072(2) -0.039(2) -0.058(3) 0.111(3) Cl2 0.0697(18) 0.0799(18) 0.086(2) -0.0084(15) -0.0155(15) 0.0216(14) Cl3 0.0633(19) 0.145(3) 0.080(2) -0.009(2) -0.0215(16) -0.0133(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N6 2.382(5) . ? Hg1 N5 2.485(5) 2_656 ? Hg1 I3 2.6570(5) . ? Hg1 I2 2.6679(5) . ? N1 C4 1.359(7) . ? N1 C1 1.375(7) . ? N1 H1A 0.8800 . ? N2 C6 1.377(7) . ? N2 C9 1.382(7) . ? N3 C11 1.369(7) . ? N3 C14 1.370(7) . ? N3 H3A 0.8800 . ? N4 C19 1.371(7) . ? N4 C16 1.383(7) . ? C1 C20 1.389(8) . ? C1 C2 1.444(8) . ? C2 C3 1.357(8) . ? C2 H2 0.9500 . ? C3 C4 1.443(8) . ? C3 H3 0.9500 . ? C4 C5 1.400(8) . ? C5 C6 1.406(8) . ? C5 C21 1.503(8) . ? C6 C7 1.430(8) . ? C7 C8 1.328(9) . ? C7 H7 0.9500 . ? C8 C9 1.447(8) . ? C8 H8 0.9500 . ? C9 C10 1.395(8) . ? C10 C11 1.393(8) . ? C10 C26 1.490(8) . ? C11 C12 1.456(8) . ? C12 C13 1.327(8) . ? C12 H12 0.9500 . ? C13 C14 1.438(8) . ? C13 H13 0.9500 . ? C14 C15 1.419(8) . ? C15 C16 1.387(8) . ? C15 C31 1.502(8) . ? C16 C17 1.443(8) . ? C17 C18 1.353(8) . ? C17 H17 0.9500 . ? C18 C19 1.460(8) . ? C18 H18 0.9500 . ? C19 C20 1.407(8) . ? C20 C37 1.502(8) . ? C21 C22 1.382(8) . ? C21 C25 1.401(8) . ? C22 C23 1.376(8) . ? C22 H22 0.9500 . ? C23 N5 1.341(8) . ? C23 H23 0.9500 . ? N5 C24 1.333(8) . ? N5 Hg1 2.485(5) 2_656 ? C24 C25 1.398(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.381(9) . ? C26 C27 1.410(8) . ? C27 C28 1.370(9) . ? C27 H27 0.9500 . ? C28 N6 1.345(8) . ? C28 H28 0.9500 . ? N6 C29 1.345(8) . ? C29 C30 1.365(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.395(8) . ? C31 C32 1.403(8) . ? C32 C33 1.403(9) . ? C32 H32 0.9500 . ? C33 C34 1.378(10) . ? C33 H33 0.9500 . ? C34 C35 1.361(10) . ? C34 H34 0.9500 . ? C35 C36 1.396(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.393(8) . ? C37 C38 1.394(8) . ? C38 C39 1.397(9) . ? C38 H38 0.9500 . ? C39 C40 1.374(9) . ? C39 H39 0.9500 . ? C40 C41 1.366(10) . ? C40 H40 0.9500 . ? C41 C42 1.404(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 Cl2 1.701(10) . ? C43 Cl1 1.731(10) . ? C43 Cl3 1.813(12) . ? C43 H43 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Hg1 N5 89.57(17) . 2_656 ? N6 Hg1 I3 106.61(13) . . ? N5 Hg1 I3 102.13(12) 2_656 . ? N6 Hg1 I2 103.90(13) . . ? N5 Hg1 I2 100.55(12) 2_656 . ? I3 Hg1 I2 141.784(18) . . ? C4 N1 C1 108.4(5) . . ? C4 N1 H1A 125.8 . . ? C1 N1 H1A 125.8 . . ? C6 N2 C9 107.8(5) . . ? C11 N3 C14 108.1(5) . . ? C11 N3 H3A 125.9 . . ? C14 N3 H3A 125.9 . . ? C19 N4 C16 108.1(5) . . ? N1 C1 C20 126.3(5) . . ? N1 C1 C2 108.2(5) . . ? C20 C1 C2 125.5(5) . . ? C3 C2 C1 107.3(5) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.4(5) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C5 126.0(5) . . ? N1 C4 C3 108.7(5) . . ? C5 C4 C3 125.3(5) . . ? C4 C5 C6 126.1(5) . . ? C4 C5 C21 116.9(5) . . ? C6 C5 C21 116.9(5) . . ? N2 C6 C5 124.3(5) . . ? N2 C6 C7 108.2(5) . . ? C5 C6 C7 127.4(5) . . ? C8 C7 C6 108.4(5) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 C9 108.1(5) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? N2 C9 C10 125.4(5) . . ? N2 C9 C8 107.4(5) . . ? C10 C9 C8 127.1(5) . . ? C11 C10 C9 125.3(5) . . ? C11 C10 C26 117.7(5) . . ? C9 C10 C26 117.0(5) . . ? N3 C11 C10 127.0(5) . . ? N3 C11 C12 107.6(5) . . ? C10 C11 C12 125.0(5) . . ? C13 C12 C11 107.9(5) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 108.0(5) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? N3 C14 C15 125.3(5) . . ? N3 C14 C13 108.4(5) . . ? C15 C14 C13 126.3(5) . . ? C16 C15 C14 125.4(5) . . ? C16 C15 C31 118.1(5) . . ? C14 C15 C31 116.5(5) . . ? N4 C16 C15 125.7(5) . . ? N4 C16 C17 107.8(5) . . ? C15 C16 C17 126.4(5) . . ? C18 C17 C16 108.7(5) . . ? C18 C17 H17 125.6 . . ? C16 C17 H17 125.6 . . ? C17 C18 C19 106.5(5) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? N4 C19 C20 125.7(5) . . ? N4 C19 C18 108.8(5) . . ? C20 C19 C18 125.4(5) . . ? C1 C20 C19 125.3(5) . . ? C1 C20 C37 117.9(5) . . ? C19 C20 C37 116.8(5) . . ? C22 C21 C25 117.5(5) . . ? C22 C21 C5 119.9(5) . . ? C25 C21 C5 122.5(5) . . ? C23 C22 C21 120.0(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N5 C23 C22 123.2(6) . . ? N5 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C24 N5 C23 117.3(5) . . ? C24 N5 Hg1 125.6(4) . 2_656 ? C23 N5 Hg1 116.8(4) . 2_656 ? N5 C24 C25 123.3(6) . . ? N5 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C24 C25 C21 118.6(6) . . ? C24 C25 H25 120.7 . . ? C21 C25 H25 120.7 . . ? C30 C26 C27 116.7(5) . . ? C30 C26 C10 122.2(5) . . ? C27 C26 C10 121.1(5) . . ? C28 C27 C26 119.6(6) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? N6 C28 C27 122.6(6) . . ? N6 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 N6 C29 117.8(5) . . ? C28 N6 Hg1 119.8(4) . . ? C29 N6 Hg1 122.0(4) . . ? N6 C29 C30 122.6(6) . . ? N6 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C29 C30 C26 120.6(6) . . ? C29 C30 H30 119.7 . . ? C26 C30 H30 119.7 . . ? C36 C31 C32 119.3(6) . . ? C36 C31 C15 121.0(5) . . ? C32 C31 C15 119.7(5) . . ? C31 C32 C33 119.4(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 120.4(6) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 121.0(7) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C31 C36 C35 119.7(6) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C42 C37 C38 118.7(5) . . ? C42 C37 C20 120.0(5) . . ? C38 C37 C20 121.3(5) . . ? C37 C38 C39 120.6(6) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 119.8(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.6(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.3(6) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.0(6) . . ? C37 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? Cl2 C43 Cl1 114.1(5) . . ? Cl2 C43 Cl3 109.6(6) . . ? Cl1 C43 Cl3 108.5(6) . . ? Cl2 C43 H43 108.2 . . ? Cl1 C43 H43 108.2 . . ? Cl3 C43 H43 108.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.344 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.175 # Attachment 'compound 6.cif' data_e504a _database_code_depnum_ccdc_archive 'CCDC 611788' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H54 Cd2 Cl6 Cu2 I4 N12' _chemical_formula_weight 2327.59 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' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 '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 9.7586(5) _cell_length_b 12.4722(5) _cell_length_c 17.6672(7) _cell_angle_alpha 87.060(2) _cell_angle_beta 75.477(2) _cell_angle_gamma 85.986(2) _cell_volume 2075.21(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3463 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 23.31 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 2.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8103 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 26518 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.55 _reflns_number_total 9382 _reflns_number_gt 5765 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.6867P] 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 9382 _refine_ls_number_parameters 499 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.018 _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 Cd1 Cd 0.85493(6) 0.47501(4) 0.39818(3) 0.02477(13) Uani 1 1 d . . . I1 I 0.71080(5) 0.66747(4) 0.42307(3) 0.03760(14) Uani 1 1 d . . . I2 I 1.12340(5) 0.42809(4) 0.31534(3) 0.03986(15) Uani 1 1 d . . . Cu1 Cu 0.66938(8) -0.01743(6) 0.87081(4) 0.01514(17) Uani 1 1 d . . . N1 N 0.7726(5) 0.1172(4) 0.8437(3) 0.0169(11) Uani 1 1 d . . . N2 N 0.6253(5) -0.0094(4) 0.7658(3) 0.0176(11) Uani 1 1 d . . . N3 N 0.5854(5) -0.1607(4) 0.8934(3) 0.0160(11) Uani 1 1 d . . . N4 N 0.7038(5) -0.0214(4) 0.9776(3) 0.0147(11) Uani 1 1 d . . . C1 C 0.8375(6) 0.1706(5) 0.8901(3) 0.0179(13) Uani 1 1 d . . . C2 C 0.9117(7) 0.2573(5) 0.8462(3) 0.0220(14) Uani 1 1 d . . . H2 H 0.9673 0.3048 0.8646 0.026 Uiso 1 1 calc R . . C3 C 0.8889(7) 0.2598(5) 0.7743(3) 0.0205(14) Uani 1 1 d . . . H3 H 0.9251 0.3092 0.7325 0.025 Uiso 1 1 calc R . . C4 C 0.7993(6) 0.1737(4) 0.7724(3) 0.0162(13) Uani 1 1 d . . . C5 C 0.7402(6) 0.1556(5) 0.7114(3) 0.0168(13) Uani 1 1 d . . . C6 C 0.6521(7) 0.0744(5) 0.7104(3) 0.0211(14) Uani 1 1 d . . . C7 C 0.5836(8) 0.0567(5) 0.6490(4) 0.0287(16) Uani 1 1 d . . . H7 H 0.5826 0.1029 0.6047 0.034 Uiso 1 1 calc R . . C8 C 0.5216(8) -0.0373(5) 0.6662(4) 0.0274(16) Uani 1 1 d . . . H8 H 0.4681 -0.0697 0.6364 0.033 Uiso 1 1 calc R . . C9 C 0.5509(7) -0.0794(5) 0.7374(3) 0.0211(14) Uani 1 1 d . . . C10 C 0.5103(7) -0.1800(5) 0.7724(3) 0.0193(14) Uani 1 1 d . . . C11 C 0.5348(7) -0.2190(5) 0.8434(3) 0.0191(14) Uani 1 1 d . . . C12 C 0.5103(7) -0.3254(5) 0.8755(4) 0.0257(15) Uani 1 1 d . . . H12 H 0.4771 -0.3816 0.8517 0.031 Uiso 1 1 calc R . . C13 C 0.5424(7) -0.3316(5) 0.9452(3) 0.0219(14) Uani 1 1 d . . . H13 H 0.5370 -0.3932 0.9796 0.026 Uiso 1 1 calc R C 4 C14 C 0.5864(6) -0.2281(4) 0.9583(3) 0.0175(13) Uani 1 1 d . . . C15 C 0.6171(6) -0.1998(5) 1.0271(3) 0.0159(13) Uani 1 1 d . . . C16 C 0.6654(7) -0.0999(5) 1.0361(3) 0.0193(14) Uani 1 1 d . . . C17 C 0.6895(7) -0.0655(5) 1.1076(3) 0.0201(14) Uani 1 1 d . . . H17 H 0.6689 -0.1036 1.1567 0.024 Uiso 1 1 calc R . . C18 C 0.7476(7) 0.0321(5) 1.0922(3) 0.0180(13) Uani 1 1 d . . . H18 H 0.7746 0.0749 1.1284 0.022 Uiso 1 1 calc R . . C19 C 0.7601(6) 0.0576(5) 1.0112(3) 0.0164(13) Uani 1 1 d . . . C20 C 0.8270(6) 0.1470(5) 0.9703(3) 0.0164(13) Uani 1 1 d . . . C21 C 0.7705(7) 0.2326(5) 0.6418(3) 0.0195(14) Uani 1 1 d . . . C22 C 0.6624(7) 0.3028(5) 0.6247(3) 0.0214(14) Uani 1 1 d . . . H22 H 0.5682 0.3021 0.6565 0.026 Uiso 1 1 calc R . . C23 C 0.6961(7) 0.3727(5) 0.5606(3) 0.0219(14) Uani 1 1 d . . . H23 H 0.6233 0.4219 0.5506 0.026 Uiso 1 1 calc R . . N5 N 0.8229(6) 0.3754(4) 0.5127(3) 0.0234(12) Uani 1 1 d . . . C24 C 0.9258(7) 0.3082(5) 0.5287(4) 0.0262(16) Uani 1 1 d . . . H24 H 1.0178 0.3088 0.4943 0.031 Uiso 1 1 calc R . . C25 C 0.9043(7) 0.2379(5) 0.5928(4) 0.0254(15) Uani 1 1 d . . . H25 H 0.9811 0.1936 0.6032 0.030 Uiso 1 1 calc R . . C26 C 0.4347(7) -0.2497(5) 0.7318(3) 0.0205(14) Uani 1 1 d . . . C27 C 0.2959(7) -0.2760(5) 0.7679(3) 0.0212(14) Uani 1 1 d . . . H28 H 0.2511 -0.2521 0.8188 0.025 Uiso 1 1 calc R . . C28 C 0.2250(7) -0.3364(5) 0.7292(3) 0.0214(14) Uani 1 1 d . . . H29 H 0.1308 -0.3531 0.7550 0.026 Uiso 1 1 calc R . . N6 N 0.2794(6) -0.3731(4) 0.6578(3) 0.0197(12) Uani 1 1 d . . . C29 C 0.4153(7) -0.3495(5) 0.6234(3) 0.0238(15) Uani 1 1 d . . . H30 H 0.4583 -0.3764 0.5731 0.029 Uiso 1 1 calc R . . C30 C 0.4941(7) -0.2881(5) 0.6579(3) 0.0239(15) Uani 1 1 d . . . H31 H 0.5882 -0.2724 0.6310 0.029 Uiso 1 1 calc R . . C31 C 0.6031(7) -0.2807(4) 1.0932(3) 0.0173(13) Uani 1 1 d . . . C32 C 0.4768(7) -0.3257(5) 1.1269(3) 0.0213(14) Uani 1 1 d . . . H33 H 0.3960 -0.3054 1.1074 0.026 Uiso 1 1 calc R . . C33 C 0.4647(7) -0.3997(5) 1.1884(4) 0.0257(15) Uani 1 1 d . . . H34 H 0.3764 -0.4302 1.2105 0.031 Uiso 1 1 calc R . . C34 C 0.5805(8) -0.4301(5) 1.2185(4) 0.0304(17) Uani 1 1 d . . . H35 H 0.5720 -0.4805 1.2613 0.036 Uiso 1 1 calc R . . C35 C 0.7087(7) -0.3857(5) 1.1849(4) 0.0264(16) Uani 1 1 d . . . H36 H 0.7888 -0.4055 1.2051 0.032 Uiso 1 1 calc R . . C36 C 0.7215(7) -0.3127(5) 1.1222(3) 0.0228(14) Uani 1 1 d . . . H37 H 0.8106 -0.2842 1.0987 0.027 Uiso 1 1 calc R . . C37 C 0.8898(6) 0.2222(5) 1.0137(3) 0.0176(13) Uani 1 1 d . . . C38 C 0.8465(7) 0.3317(5) 1.0166(3) 0.0237(15) Uani 1 1 d . . . H39 H 0.7756 0.3585 0.9911 0.028 Uiso 1 1 calc R . . C39 C 0.9051(8) 0.4008(5) 1.0559(4) 0.0302(17) Uani 1 1 d . . . H40 H 0.8724 0.4744 1.0584 0.036 Uiso 1 1 calc R . . C40 C 1.0111(8) 0.3645(6) 1.0917(4) 0.0363(19) Uani 1 1 d . . . H41 H 1.0540 0.4130 1.1172 0.044 Uiso 1 1 calc R . . C41 C 1.0534(7) 0.2571(6) 1.0898(4) 0.0293(16) Uani 1 1 d . . . H42 H 1.1244 0.2310 1.1155 0.035 Uiso 1 1 calc R . . C42 C 0.9941(7) 0.1860(6) 1.0509(3) 0.0251(15) Uani 1 1 d . . . H43 H 1.0254 0.1121 1.0499 0.030 Uiso 1 1 calc R . . C43 C 0.9479(12) 0.1227(11) 0.3651(6) 0.055(3) Uiso 0.688(5) 1 d PD D 1 H44 H 0.9548 0.2012 0.3513 0.065 Uiso 0.688(5) 1 calc PR D 1 Cl1 Cl 0.9729(5) 0.0595(3) 0.2759(2) 0.0789(14) Uiso 0.688(5) 1 d PD D 1 Cl2 Cl 0.7898(4) 0.1114(3) 0.4275(2) 0.0623(11) Uiso 0.688(5) 1 d PD D 1 Cl3 Cl 1.0936(4) 0.0850(3) 0.4037(2) 0.0626(12) Uiso 0.688(5) 1 d PD D 1 C43B C 0.949(3) 0.031(2) 0.3583(12) 0.115(3) Uiso 0.312(5) 1 d PD D 2 H44B H 1.0146 -0.0277 0.3716 0.138 Uiso 0.312(5) 1 calc PR D 2 Cl1B Cl 0.8883(14) 0.0003(9) 0.2818(6) 0.115(3) Uiso 0.312(5) 1 d PD D 2 Cl2B Cl 0.8047(13) 0.0518(11) 0.4337(7) 0.115(3) Uiso 0.312(5) 1 d PD D 2 Cl3B Cl 1.0325(13) 0.1467(9) 0.3318(7) 0.115(3) Uiso 0.312(5) 1 d PD D 2 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 0.0320(3) 0.0260(3) 0.0191(2) 0.0054(2) -0.0095(2) -0.0140(2) I1 0.0332(3) 0.0366(3) 0.0442(3) -0.0016(2) -0.0112(2) -0.0041(2) I2 0.0312(3) 0.0452(3) 0.0411(3) 0.0062(2) -0.0042(2) -0.0106(2) Cu1 0.0196(4) 0.0151(4) 0.0124(3) 0.0034(3) -0.0063(3) -0.0075(3) N1 0.023(3) 0.018(3) 0.012(2) 0.005(2) -0.007(2) -0.006(2) N2 0.019(3) 0.020(3) 0.014(2) 0.003(2) -0.003(2) -0.009(2) N3 0.018(3) 0.016(3) 0.014(2) 0.004(2) -0.005(2) -0.003(2) N4 0.019(3) 0.008(2) 0.019(2) -0.001(2) -0.006(2) -0.005(2) C1 0.018(3) 0.018(3) 0.021(3) 0.006(3) -0.011(3) -0.009(3) C2 0.024(4) 0.021(3) 0.024(3) 0.006(3) -0.009(3) -0.014(3) C3 0.027(4) 0.017(3) 0.018(3) 0.002(3) -0.005(3) -0.008(3) C4 0.018(3) 0.011(3) 0.020(3) 0.004(2) -0.005(3) -0.005(2) C5 0.021(4) 0.018(3) 0.013(3) 0.003(2) -0.005(3) -0.007(3) C6 0.028(4) 0.018(3) 0.021(3) 0.000(3) -0.013(3) -0.006(3) C7 0.046(5) 0.025(4) 0.023(3) 0.010(3) -0.020(3) -0.015(3) C8 0.041(5) 0.026(4) 0.023(3) 0.007(3) -0.019(3) -0.015(3) C9 0.027(4) 0.018(3) 0.022(3) 0.000(3) -0.010(3) -0.010(3) C10 0.021(4) 0.017(3) 0.022(3) -0.003(3) -0.007(3) -0.008(3) C11 0.022(4) 0.018(3) 0.017(3) 0.000(3) -0.004(3) -0.005(3) C12 0.035(4) 0.018(3) 0.025(3) 0.001(3) -0.007(3) -0.012(3) C13 0.031(4) 0.017(3) 0.017(3) 0.004(3) -0.005(3) -0.007(3) C14 0.021(4) 0.010(3) 0.023(3) 0.003(3) -0.007(3) -0.006(2) C15 0.015(3) 0.018(3) 0.015(3) 0.005(2) -0.005(2) -0.009(3) C16 0.018(3) 0.020(3) 0.018(3) 0.004(3) -0.003(3) 0.003(3) C17 0.029(4) 0.020(3) 0.013(3) 0.002(3) -0.007(3) -0.005(3) C18 0.023(4) 0.016(3) 0.016(3) -0.001(3) -0.005(3) -0.005(3) C19 0.017(3) 0.018(3) 0.015(3) 0.004(2) -0.004(2) -0.004(3) C20 0.015(3) 0.017(3) 0.018(3) 0.004(3) -0.005(3) -0.006(3) C21 0.032(4) 0.016(3) 0.014(3) 0.000(2) -0.011(3) -0.007(3) C22 0.027(4) 0.022(3) 0.016(3) 0.002(3) -0.005(3) -0.007(3) C23 0.031(4) 0.019(3) 0.016(3) -0.002(3) -0.007(3) 0.001(3) N5 0.030(3) 0.027(3) 0.017(3) 0.008(2) -0.011(2) -0.014(3) C24 0.028(4) 0.032(4) 0.020(3) 0.004(3) -0.005(3) -0.013(3) C25 0.024(4) 0.026(4) 0.027(3) 0.003(3) -0.008(3) -0.003(3) C26 0.024(4) 0.021(3) 0.019(3) 0.005(3) -0.010(3) -0.008(3) C27 0.023(4) 0.023(3) 0.017(3) -0.002(3) -0.001(3) -0.009(3) C28 0.023(4) 0.022(3) 0.018(3) 0.003(3) -0.001(3) -0.013(3) N6 0.027(3) 0.018(3) 0.017(2) 0.006(2) -0.009(2) -0.013(2) C29 0.034(4) 0.024(4) 0.014(3) 0.002(3) -0.005(3) -0.011(3) C30 0.023(4) 0.029(4) 0.021(3) 0.003(3) -0.004(3) -0.016(3) C31 0.023(4) 0.012(3) 0.015(3) 0.004(2) -0.002(3) -0.003(3) C32 0.021(4) 0.018(3) 0.025(3) 0.000(3) -0.007(3) 0.001(3) C33 0.026(4) 0.021(3) 0.025(3) 0.004(3) 0.004(3) -0.012(3) C34 0.052(5) 0.017(3) 0.020(3) 0.005(3) -0.007(3) -0.001(3) C35 0.031(4) 0.028(4) 0.024(3) 0.004(3) -0.015(3) 0.002(3) C36 0.023(4) 0.025(4) 0.021(3) 0.004(3) -0.005(3) -0.008(3) C37 0.019(3) 0.020(3) 0.015(3) 0.002(3) -0.004(2) -0.011(3) C38 0.026(4) 0.022(4) 0.021(3) 0.008(3) -0.002(3) -0.010(3) C39 0.046(5) 0.019(4) 0.021(3) 0.003(3) 0.002(3) -0.014(3) C40 0.041(5) 0.044(5) 0.024(3) -0.007(3) 0.000(3) -0.028(4) C41 0.025(4) 0.045(5) 0.020(3) 0.001(3) -0.005(3) -0.017(3) C42 0.028(4) 0.033(4) 0.014(3) -0.001(3) -0.003(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.283(5) . ? Cd1 N6 2.308(5) 2_656 ? Cd1 I1 2.6942(7) . ? Cd1 I2 2.7016(7) . ? Cu1 N1 1.993(5) . ? Cu1 N4 1.995(5) . ? Cu1 N3 1.998(5) . ? Cu1 N2 2.003(5) . ? N1 C1 1.376(7) . ? N1 C4 1.387(7) . ? N2 C9 1.363(8) . ? N2 C6 1.386(7) . ? N3 C11 1.375(7) . ? N3 C14 1.388(7) . ? N4 C16 1.386(7) . ? N4 C19 1.387(7) . ? C1 C20 1.412(8) . ? C1 C2 1.428(8) . ? C2 C3 1.342(8) . ? C2 H2 0.9500 . ? C3 C4 1.439(8) . ? C3 H3 0.9500 . ? C4 C5 1.378(8) . ? C5 C6 1.378(8) . ? C5 C21 1.503(8) . ? C6 C7 1.443(8) . ? C7 C8 1.343(9) . ? C7 H7 0.9500 . ? C8 C9 1.426(8) . ? C8 H8 0.9500 . ? C9 C10 1.407(8) . ? C10 C11 1.392(8) . ? C10 C26 1.495(8) . ? C11 C12 1.428(8) . ? C12 C13 1.342(8) . ? C12 H12 0.9500 . ? C13 C14 1.437(8) . ? C13 H13 0.9500 . ? C14 C15 1.389(8) . ? C15 C16 1.393(8) . ? C15 C31 1.489(8) . ? C16 C17 1.433(8) . ? C17 C18 1.365(8) . ? C17 H17 0.9500 . ? C18 C19 1.427(8) . ? C18 H18 0.9500 . ? C19 C20 1.404(8) . ? C20 C37 1.494(8) . ? C21 C25 1.377(9) . ? C21 C22 1.406(8) . ? C22 C23 1.379(8) . ? C22 H22 0.9500 . ? C23 N5 1.315(8) . ? C23 H23 0.9500 . ? N5 C24 1.339(8) . ? C24 C25 1.379(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.385(8) . ? C26 C27 1.398(9) . ? C27 C28 1.370(8) . ? C27 H28 0.9500 . ? C28 N6 1.331(7) . ? C28 H29 0.9500 . ? N6 C29 1.359(8) . ? N6 Cd1 2.308(5) 2_656 ? C29 C30 1.383(8) . ? C29 H30 0.9500 . ? C30 H31 0.9500 . ? C31 C32 1.373(9) . ? C31 C36 1.403(8) . ? C32 C33 1.377(8) . ? C32 H33 0.9500 . ? C33 C34 1.386(9) . ? C33 H34 0.9500 . ? C34 C35 1.384(10) . ? C34 H35 0.9500 . ? C35 C36 1.384(8) . ? C35 H36 0.9500 . ? C36 H37 0.9500 . ? C37 C42 1.383(8) . ? C37 C38 1.402(8) . ? C38 C39 1.370(9) . ? C38 H39 0.9500 . ? C39 C40 1.382(10) . ? C39 H40 0.9500 . ? C40 C41 1.374(10) . ? C40 H41 0.9500 . ? C41 C42 1.387(9) . ? C41 H42 0.9500 . ? C42 H43 0.9500 . ? C43 Cl2 1.667(12) . ? C43 Cl1 1.751(11) . ? C43 Cl3 1.752(11) . ? C43 H44 1.0000 . ? C43B Cl1B 1.676(18) . ? C43B Cl2B 1.691(19) . ? C43B Cl3B 1.693(19) . ? C43B H44B 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cd1 N6 95.73(17) . 2_656 ? N5 Cd1 I1 110.06(14) . . ? N6 Cd1 I1 105.72(13) 2_656 . ? N5 Cd1 I2 106.88(14) . . ? N6 Cd1 I2 103.59(13) 2_656 . ? I1 Cd1 I2 129.44(2) . . ? N1 Cu1 N4 90.19(19) . . ? N1 Cu1 N3 174.0(2) . . ? N4 Cu1 N3 90.00(19) . . ? N1 Cu1 N2 89.98(19) . . ? N4 Cu1 N2 177.1(2) . . ? N3 Cu1 N2 90.14(19) . . ? C1 N1 C4 105.7(5) . . ? C1 N1 Cu1 127.5(4) . . ? C4 N1 Cu1 126.8(4) . . ? C9 N2 C6 105.9(5) . . ? C9 N2 Cu1 127.2(4) . . ? C6 N2 Cu1 126.7(4) . . ? C11 N3 C14 106.0(5) . . ? C11 N3 Cu1 127.0(4) . . ? C14 N3 Cu1 126.3(4) . . ? C16 N4 C19 105.5(5) . . ? C16 N4 Cu1 127.0(4) . . ? C19 N4 Cu1 127.4(4) . . ? N1 C1 C20 125.3(5) . . ? N1 C1 C2 109.9(5) . . ? C20 C1 C2 124.7(6) . . ? C3 C2 C1 107.7(6) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? C2 C3 C4 107.2(5) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 125.3(5) . . ? C5 C4 C3 125.1(5) . . ? N1 C4 C3 109.4(5) . . ? C6 C5 C4 125.0(5) . . ? C6 C5 C21 117.6(5) . . ? C4 C5 C21 117.4(5) . . ? C5 C6 N2 124.7(5) . . ? C5 C6 C7 126.1(6) . . ? N2 C6 C7 109.0(5) . . ? C8 C7 C6 107.2(5) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 107.3(6) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 125.1(5) . . ? N2 C9 C8 110.5(5) . . ? C10 C9 C8 124.4(6) . . ? C11 C10 C9 124.1(6) . . ? C11 C10 C26 117.3(5) . . ? C9 C10 C26 118.6(5) . . ? N3 C11 C10 125.1(5) . . ? N3 C11 C12 109.7(5) . . ? C10 C11 C12 125.2(6) . . ? C13 C12 C11 107.7(6) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 107.4(5) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? N3 C14 C15 126.2(5) . . ? N3 C14 C13 109.0(5) . . ? C15 C14 C13 124.7(5) . . ? C14 C15 C16 122.8(5) . . ? C14 C15 C31 119.0(5) . . ? C16 C15 C31 118.2(5) . . ? N4 C16 C15 125.9(5) . . ? N4 C16 C17 109.7(5) . . ? C15 C16 C17 124.3(5) . . ? C18 C17 C16 107.4(5) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 106.8(5) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N4 C19 C20 124.8(5) . . ? N4 C19 C18 110.4(5) . . ? C20 C19 C18 124.7(6) . . ? C19 C20 C1 123.6(5) . . ? C19 C20 C37 118.7(5) . . ? C1 C20 C37 117.7(5) . . ? C25 C21 C22 117.4(5) . . ? C25 C21 C5 121.8(6) . . ? C22 C21 C5 120.8(6) . . ? C23 C22 C21 118.5(6) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? N5 C23 C22 123.9(6) . . ? N5 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? C23 N5 C24 117.6(5) . . ? C23 N5 Cd1 120.0(4) . . ? C24 N5 Cd1 121.9(4) . . ? N5 C24 C25 123.0(6) . . ? N5 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? C21 C25 C24 119.5(6) . . ? C21 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C30 C26 C27 117.2(6) . . ? C30 C26 C10 123.0(6) . . ? C27 C26 C10 119.7(5) . . ? C28 C27 C26 119.6(6) . . ? C28 C27 H28 120.2 . . ? C26 C27 H28 120.2 . . ? N6 C28 C27 124.2(6) . . ? N6 C28 H29 117.9 . . ? C27 C28 H29 117.9 . . ? C28 N6 C29 116.2(5) . . ? C28 N6 Cd1 119.6(4) . 2_656 ? C29 N6 Cd1 124.2(4) . 2_656 ? N6 C29 C30 123.3(6) . . ? N6 C29 H30 118.3 . . ? C30 C29 H30 118.3 . . ? C29 C30 C26 119.4(6) . . ? C29 C30 H31 120.3 . . ? C26 C30 H31 120.3 . . ? C32 C31 C36 118.5(5) . . ? C32 C31 C15 121.8(5) . . ? C36 C31 C15 119.7(6) . . ? C31 C32 C33 121.3(6) . . ? C31 C32 H33 119.3 . . ? C33 C32 H33 119.3 . . ? C32 C33 C34 120.6(6) . . ? C32 C33 H34 119.7 . . ? C34 C33 H34 119.7 . . ? C35 C34 C33 118.8(6) . . ? C35 C34 H35 120.6 . . ? C33 C34 H35 120.6 . . ? C34 C35 C36 120.6(6) . . ? C34 C35 H36 119.7 . . ? C36 C35 H36 119.7 . . ? C35 C36 C31 120.2(6) . . ? C35 C36 H37 119.9 . . ? C31 C36 H37 119.9 . . ? C42 C37 C38 118.1(6) . . ? C42 C37 C20 121.0(5) . . ? C38 C37 C20 120.9(5) . . ? C39 C38 C37 120.9(6) . . ? C39 C38 H39 119.6 . . ? C37 C38 H39 119.6 . . ? C38 C39 C40 120.8(6) . . ? C38 C39 H40 119.6 . . ? C40 C39 H40 119.6 . . ? C41 C40 C39 118.8(7) . . ? C41 C40 H41 120.6 . . ? C39 C40 H41 120.6 . . ? C40 C41 C42 121.1(7) . . ? C40 C41 H42 119.5 . . ? C42 C41 H42 119.5 . . ? C37 C42 C41 120.4(6) . . ? C37 C42 H43 119.8 . . ? C41 C42 H43 119.8 . . ? Cl2 C43 Cl1 115.9(7) . . ? Cl2 C43 Cl3 115.1(7) . . ? Cl1 C43 Cl3 108.1(6) . . ? Cl2 C43 H44 105.5 . . ? Cl1 C43 H44 105.5 . . ? Cl3 C43 H44 105.5 . . ? Cl1B C43B Cl2B 106.5(14) . . ? Cl1B C43B Cl3B 106.0(13) . . ? Cl2B C43B Cl3B 110.4(15) . . ? Cl1B C43B H44B 111.2 . . ? Cl2B C43B H44B 111.2 . . ? Cl3B C43B H44B 111.2 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.657 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.219 # Attachment 'compound 7.cif' data_e452 _database_code_depnum_ccdc_archive 'CCDC 611789' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H54 Br4 Cl6 Cu2 Hg2 N12' _chemical_formula_weight 2316.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5541(4) _cell_length_b 12.5202(5) _cell_length_c 17.6342(6) _cell_angle_alpha 86.332(2) _cell_angle_beta 76.009(2) _cell_angle_gamma 87.361(2) _cell_volume 2041.60(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4381 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 6.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4868 _exptl_absorpt_correction_T_max 0.8296 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 21296 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9317 _reflns_number_gt 6847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+4.7563P] 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 9317 _refine_ls_number_parameters 491 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.042 _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 Hg1 Hg 0.86571(3) 0.49197(2) 0.394647(16) 0.02965(10) Uani 1 1 d . . . Br1 Br 0.69914(9) 0.65032(7) 0.42586(5) 0.0411(2) Uani 1 1 d . . . Br2 Br 1.11119(9) 0.43553(7) 0.31920(5) 0.0434(2) Uani 1 1 d . . . N1 N 0.4098(6) 0.1585(4) 0.1057(3) 0.0197(11) Uani 1 1 d . . . N2 N 0.3667(6) 0.0065(4) 0.2344(3) 0.0208(11) Uani 1 1 d . . . N3 N 0.2213(5) -0.1231(4) 0.1547(3) 0.0158(10) Uani 1 1 d . . . N4 N 0.2918(5) 0.0172(4) 0.0201(3) 0.0160(10) Uani 1 1 d . . . C1 C 0.4110(7) 0.2257(5) 0.0404(3) 0.0183(13) Uani 1 1 d . . . C2 C 0.4507(8) 0.3312(5) 0.0538(4) 0.0267(15) Uani 1 1 d . . . H2 H 0.4544 0.3931 0.0194 0.032 Uiso 1 1 calc R . . C3 C 0.4818(7) 0.3251(5) 0.1250(4) 0.0249(14) Uani 1 1 d . . . H3 H 0.5144 0.3814 0.1494 0.030 Uiso 1 1 calc R . . C4 C 0.4561(7) 0.2180(5) 0.1564(4) 0.0212(13) Uani 1 1 d . . . C5 C 0.4803(7) 0.1796(5) 0.2287(4) 0.0219(14) Uani 1 1 d . . . C6 C 0.4421(7) 0.0785(5) 0.2636(4) 0.0228(14) Uani 1 1 d . . . C7 C 0.4681(8) 0.0373(6) 0.3371(4) 0.0311(17) Uani 1 1 d . . . H7 H 0.5206 0.0706 0.3680 0.037 Uiso 1 1 calc R . . C8 C 0.4032(9) -0.0584(6) 0.3538(4) 0.0330(17) Uani 1 1 d . . . H8 H 0.4010 -0.1046 0.3989 0.040 Uiso 1 1 calc R . . C9 C 0.3383(7) -0.0766(5) 0.2904(4) 0.0227(14) Uani 1 1 d . . . C10 C 0.2512(7) -0.1623(5) 0.2885(3) 0.0222(14) Uani 1 1 d . . . C11 C 0.1922(7) -0.1813(5) 0.2255(3) 0.0190(13) Uani 1 1 d . . . C12 C 0.1049(7) -0.2703(5) 0.2235(4) 0.0221(14) Uani 1 1 d . . . H12 H 0.0677 -0.3204 0.2655 0.027 Uiso 1 1 calc R . . C13 C 0.0857(7) -0.2690(5) 0.1500(4) 0.0234(14) Uani 1 1 d . . . H13 H 0.0331 -0.3190 0.1306 0.028 Uiso 1 1 calc R . . C14 C 0.1587(7) -0.1786(5) 0.1066(4) 0.0188(13) Uani 1 1 d . . . C15 C 0.1713(7) -0.1546(5) 0.0269(4) 0.0191(13) Uani 1 1 d . . . C16 C 0.2377(7) -0.0633(5) -0.0135(3) 0.0175(12) Uani 1 1 d . . . C17 C 0.2528(7) -0.0362(5) -0.0956(4) 0.0218(14) Uani 1 1 d . . . H17 H 0.2258 -0.0789 -0.1320 0.026 Uiso 1 1 calc R . . C18 C 0.3121(7) 0.0608(5) -0.1113(4) 0.0222(14) Uani 1 1 d . . . H18 H 0.3346 0.0993 -0.1607 0.027 Uiso 1 1 calc R . . C19 C 0.3344(7) 0.0945(5) -0.0391(3) 0.0189(13) Uani 1 1 d . . . C20 C 0.3825(6) 0.1975(5) -0.0287(3) 0.0169(12) Uani 1 1 d . . . C21 C 0.5581(7) 0.2501(5) 0.2701(4) 0.0219(14) Uani 1 1 d . . . C22 C 0.4960(8) 0.2907(6) 0.3428(4) 0.0300(16) Uani 1 1 d . . . H22 H 0.3988 0.2760 0.3684 0.036 Uiso 1 1 calc R . . C23 C 0.5767(8) 0.3526(6) 0.3774(4) 0.0287(16) Uani 1 1 d . . . H23 H 0.5325 0.3800 0.4268 0.034 Uiso 1 1 calc R . . N5 N 0.7137(6) 0.3756(5) 0.3445(3) 0.0253(12) Uani 1 1 d . . . C24 C 0.7722(8) 0.3378(5) 0.2747(4) 0.0250(14) Uani 1 1 d . . . H24 H 0.8697 0.3537 0.2506 0.030 Uiso 1 1 calc R . . C25 C 0.6999(8) 0.2773(5) 0.2356(4) 0.0260(15) Uani 1 1 d . . . H25 H 0.7462 0.2540 0.1852 0.031 Uiso 1 1 calc R . . C26 C 0.2207(7) -0.2395(5) 0.3583(3) 0.0203(13) Uani 1 1 d . . . C27 C 0.0833(7) -0.2477(5) 0.4075(4) 0.0237(14) Uani 1 1 d . . . H27 H 0.0052 -0.2043 0.3970 0.028 Uiso 1 1 calc R . . C28 C 0.0618(8) -0.3192(6) 0.4714(4) 0.0282(15) Uani 1 1 d . . . H28 H -0.0320 -0.3223 0.5053 0.034 Uiso 1 1 calc R . . N6 N 0.1648(6) -0.3840(4) 0.4883(3) 0.0240(12) Uani 1 1 d . . . C29 C 0.2973(8) -0.3783(5) 0.4405(4) 0.0253(15) Uani 1 1 d . . . H29 H 0.3721 -0.4251 0.4512 0.030 Uiso 1 1 calc R . . C30 C 0.3284(8) -0.3067(5) 0.3765(4) 0.0244(14) Uani 1 1 d . . . H30 H 0.4240 -0.3035 0.3447 0.029 Uiso 1 1 calc R . . C31 C 0.1090(7) -0.2311(5) -0.0174(3) 0.0182(13) Uani 1 1 d . . . C32 C 0.1578(7) -0.3375(5) -0.0205(4) 0.0245(14) Uani 1 1 d . . . H32 H 0.2315 -0.3617 0.0048 0.029 Uiso 1 1 calc R . . C33 C 0.0978(8) -0.4092(6) -0.0611(4) 0.0316(17) Uani 1 1 d . . . H33 H 0.1313 -0.4818 -0.0630 0.038 Uiso 1 1 calc R . . C34 C -0.0082(9) -0.3756(7) -0.0978(4) 0.0371(19) Uani 1 1 d . . . H34 H -0.0500 -0.4250 -0.1239 0.045 Uiso 1 1 calc R . . C35 C -0.0538(8) -0.2705(7) -0.0968(4) 0.0366(19) Uani 1 1 d . . . H35 H -0.1247 -0.2469 -0.1242 0.044 Uiso 1 1 calc R . . C36 C 0.0017(7) -0.1976(6) -0.0562(4) 0.0258(15) Uani 1 1 d . . . H36 H -0.0331 -0.1253 -0.0549 0.031 Uiso 1 1 calc R . . C37 C 0.3977(7) 0.2780(5) -0.0959(3) 0.0174(12) Uani 1 1 d . . . C38 C 0.2811(7) 0.3055(5) -0.1282(4) 0.0244(14) Uani 1 1 d . . . H38 H 0.1911 0.2726 -0.1077 0.029 Uiso 1 1 calc R . . C39 C 0.2960(8) 0.3814(6) -0.1908(4) 0.0322(17) Uani 1 1 d . . . H39 H 0.2159 0.4004 -0.2126 0.039 Uiso 1 1 calc R . . C40 C 0.4258(8) 0.4287(5) -0.2212(4) 0.0293(16) Uani 1 1 d . . . H40 H 0.4349 0.4799 -0.2641 0.035 Uiso 1 1 calc R . . C41 C 0.5432(8) 0.4030(6) -0.1903(4) 0.0303(16) Uani 1 1 d . . . H41 H 0.6328 0.4360 -0.2117 0.036 Uiso 1 1 calc R . . C42 C 0.5283(7) 0.3279(5) -0.1273(4) 0.0224(14) Uani 1 1 d . . . H42 H 0.6085 0.3103 -0.1053 0.027 Uiso 1 1 calc R . . C43A C 0.9517(15) 0.1287(17) 0.3628(8) 0.0703(12) Uiso 0.545(6) 1 d PD A 1 H43A H 0.9606 0.2069 0.3476 0.084 Uiso 0.545(6) 1 calc PR A 1 Cl1A Cl 0.7907(6) 0.1171(5) 0.4274(3) 0.0703(12) Uiso 0.545(6) 1 d PD A 1 Cl2A Cl 0.9716(6) 0.0662(5) 0.2761(3) 0.0703(12) Uiso 0.545(6) 1 d PD A 1 Cl3A Cl 1.0979(6) 0.0934(4) 0.4033(3) 0.0703(12) Uiso 0.545(6) 1 d PD A 1 C43B C 0.970(2) 0.0417(18) 0.3598(11) 0.113(2) Uiso 0.455(6) 1 d PD A 2 H43B H 1.0430 -0.0135 0.3709 0.136 Uiso 0.455(6) 1 calc PR A 2 Cl2B Cl 0.9026(11) 0.0105(8) 0.2811(5) 0.113(2) Uiso 0.455(6) 1 d PD A 2 Cl1B Cl 0.8178(10) 0.0481(9) 0.4373(5) 0.113(2) Uiso 0.455(6) 1 d PD A 2 Cl3B Cl 1.0432(10) 0.1671(7) 0.3384(5) 0.113(2) Uiso 0.455(6) 1 d PD A 2 Cu1 Cu 0.32453(8) 0.01371(6) 0.12831(4) 0.01608(16) Uiso 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 Hg1 0.03680(18) 0.02916(15) 0.02384(14) 0.00659(10) -0.00952(11) -0.00882(11) Br1 0.0325(4) 0.0407(4) 0.0506(5) -0.0010(4) -0.0115(4) -0.0001(4) Br2 0.0329(4) 0.0510(5) 0.0417(4) 0.0040(4) -0.0011(3) -0.0053(4) N1 0.021(3) 0.020(3) 0.020(3) 0.002(2) -0.009(2) -0.002(2) N2 0.026(3) 0.018(3) 0.018(2) 0.004(2) -0.005(2) -0.003(2) N3 0.014(3) 0.016(2) 0.018(2) 0.005(2) -0.006(2) -0.003(2) N4 0.015(3) 0.015(2) 0.017(2) 0.0022(19) -0.003(2) 0.000(2) C1 0.013(3) 0.020(3) 0.020(3) 0.008(2) -0.002(2) -0.003(2) C2 0.029(4) 0.020(3) 0.029(3) 0.008(3) -0.006(3) -0.005(3) C3 0.024(4) 0.020(3) 0.030(3) 0.002(3) -0.006(3) -0.006(3) C4 0.021(3) 0.018(3) 0.024(3) -0.001(2) -0.004(3) -0.004(3) C5 0.023(4) 0.020(3) 0.023(3) -0.001(3) -0.007(3) -0.003(3) C6 0.025(4) 0.022(3) 0.022(3) 0.004(3) -0.007(3) -0.011(3) C7 0.044(5) 0.028(4) 0.027(3) 0.007(3) -0.019(3) -0.015(3) C8 0.046(5) 0.036(4) 0.022(3) 0.010(3) -0.019(3) -0.011(4) C9 0.026(4) 0.021(3) 0.020(3) 0.008(3) -0.004(3) -0.006(3) C10 0.021(3) 0.024(3) 0.017(3) 0.012(3) 0.001(3) -0.004(3) C11 0.018(3) 0.022(3) 0.015(3) 0.004(2) -0.001(2) -0.001(3) C12 0.022(3) 0.021(3) 0.023(3) 0.009(3) -0.005(3) -0.010(3) C13 0.020(3) 0.027(3) 0.024(3) 0.010(3) -0.009(3) -0.009(3) C14 0.014(3) 0.020(3) 0.022(3) 0.005(2) -0.006(2) 0.000(3) C15 0.013(3) 0.023(3) 0.020(3) 0.001(2) -0.003(2) -0.001(3) C16 0.019(3) 0.016(3) 0.016(3) 0.000(2) -0.004(2) 0.004(2) C17 0.023(4) 0.023(3) 0.020(3) -0.001(3) -0.008(3) 0.001(3) C18 0.022(4) 0.027(3) 0.017(3) 0.007(3) -0.005(3) -0.001(3) C19 0.018(3) 0.021(3) 0.017(3) 0.004(2) -0.003(2) 0.001(3) C20 0.009(3) 0.021(3) 0.019(3) 0.003(2) -0.002(2) 0.001(2) C21 0.029(4) 0.019(3) 0.019(3) 0.005(2) -0.008(3) -0.011(3) C22 0.029(4) 0.033(4) 0.025(3) 0.003(3) -0.002(3) -0.007(3) C23 0.036(4) 0.033(4) 0.019(3) -0.006(3) -0.009(3) 0.003(3) N5 0.029(3) 0.028(3) 0.021(3) -0.001(2) -0.009(2) -0.006(3) C24 0.024(4) 0.024(3) 0.028(3) 0.003(3) -0.008(3) -0.007(3) C25 0.030(4) 0.026(4) 0.022(3) 0.000(3) -0.006(3) -0.004(3) C26 0.024(3) 0.019(3) 0.020(3) 0.000(2) -0.008(3) -0.009(3) C27 0.024(4) 0.026(3) 0.022(3) 0.004(3) -0.007(3) -0.003(3) C28 0.023(4) 0.033(4) 0.025(3) 0.003(3) 0.000(3) -0.008(3) N6 0.029(3) 0.025(3) 0.021(3) 0.007(2) -0.011(2) -0.008(2) C29 0.028(4) 0.024(3) 0.026(3) 0.003(3) -0.013(3) 0.001(3) C30 0.027(4) 0.030(4) 0.015(3) 0.002(3) -0.004(3) -0.005(3) C31 0.015(3) 0.024(3) 0.015(3) 0.002(2) -0.002(2) -0.008(3) C32 0.019(3) 0.028(4) 0.026(3) 0.002(3) -0.003(3) -0.008(3) C33 0.043(5) 0.025(4) 0.023(3) -0.001(3) 0.001(3) -0.016(3) C34 0.039(5) 0.048(5) 0.022(3) -0.007(3) 0.001(3) -0.027(4) C35 0.025(4) 0.063(6) 0.022(3) 0.001(3) -0.005(3) -0.016(4) C36 0.018(3) 0.035(4) 0.024(3) 0.001(3) -0.007(3) 0.001(3) C37 0.019(3) 0.012(3) 0.022(3) 0.004(2) -0.006(2) -0.003(2) C38 0.023(4) 0.023(3) 0.028(3) 0.006(3) -0.010(3) -0.002(3) C39 0.039(5) 0.033(4) 0.028(4) 0.007(3) -0.016(3) 0.004(3) C40 0.040(4) 0.023(3) 0.021(3) 0.013(3) -0.004(3) 0.000(3) C41 0.035(4) 0.023(3) 0.032(4) 0.008(3) -0.006(3) -0.007(3) C42 0.018(3) 0.024(3) 0.026(3) 0.005(3) -0.007(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N6 2.358(5) 2_656 ? Hg1 N5 2.448(5) . ? Hg1 Br1 2.4884(9) . ? Hg1 Br2 2.4957(9) . ? N1 C4 1.362(8) . ? N1 C1 1.379(7) . ? N1 Cu1 1.999(5) . ? N2 C6 1.377(8) . ? N2 C9 1.378(8) . ? N2 Cu1 2.002(5) . ? N3 C11 1.379(7) . ? N3 C14 1.385(8) . ? N3 Cu1 1.989(5) . ? N4 C19 1.375(7) . ? N4 C16 1.380(8) . ? N4 Cu1 2.005(5) . ? C1 C20 1.382(9) . ? C1 C2 1.440(9) . ? C2 C3 1.355(9) . ? C2 H2 0.9500 . ? C3 C4 1.427(9) . ? C3 H3 0.9500 . ? C4 C5 1.402(9) . ? C5 C6 1.395(9) . ? C5 C21 1.507(9) . ? C6 C7 1.436(9) . ? C7 C8 1.357(10) . ? C7 H7 0.9500 . ? C8 C9 1.437(9) . ? C8 H8 0.9500 . ? C9 C10 1.394(9) . ? C10 C11 1.400(9) . ? C10 C26 1.494(8) . ? C11 C12 1.430(9) . ? C12 C13 1.351(9) . ? C12 H12 0.9500 . ? C13 C14 1.434(9) . ? C13 H13 0.9500 . ? C14 C15 1.396(8) . ? C15 C16 1.400(8) . ? C15 C31 1.502(9) . ? C16 C17 1.439(8) . ? C17 C18 1.348(9) . ? C17 H17 0.9500 . ? C18 C19 1.434(8) . ? C18 H18 0.9500 . ? C19 C20 1.425(9) . ? C20 C37 1.490(8) . ? C21 C25 1.393(9) . ? C21 C22 1.393(9) . ? C22 C23 1.382(10) . ? C22 H22 0.9500 . ? C23 N5 1.333(9) . ? C23 H23 0.9500 . ? N5 C24 1.331(8) . ? C24 C25 1.368(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.384(9) . ? C26 C27 1.391(9) . ? C27 C28 1.376(9) . ? C27 H27 0.9500 . ? C28 N6 1.324(9) . ? C28 H28 0.9500 . ? N6 C29 1.343(9) . ? N6 Hg1 2.358(5) 2_656 ? C29 C30 1.378(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.391(9) . ? C31 C36 1.399(9) . ? C32 C33 1.405(9) . ? C32 H32 0.9500 . ? C33 C34 1.365(11) . ? C33 H33 0.9500 . ? C34 C35 1.366(12) . ? C34 H34 0.9500 . ? C35 C36 1.392(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.390(9) . ? C37 C42 1.396(9) . ? C38 C39 1.394(9) . ? C38 H38 0.9500 . ? C39 C40 1.372(10) . ? C39 H39 0.9500 . ? C40 C41 1.377(10) . ? C40 H40 0.9500 . ? C41 C42 1.394(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43A Cl1A 1.685(15) . ? C43A Cl3A 1.744(14) . ? C43A Cl2A 1.727(14) . ? C43A H43A 1.0000 . ? C43B Cl1B 1.744(18) . ? C43B Cl2B 1.739(18) . ? C43B Cl3B 1.729(18) . ? C43B H43B 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Hg1 N5 91.00(18) 2_656 . ? N6 Hg1 Br1 106.09(14) 2_656 . ? N5 Hg1 Br1 100.45(14) . . ? N6 Hg1 Br2 103.01(15) 2_656 . ? N5 Hg1 Br2 101.15(14) . . ? Br1 Hg1 Br2 143.15(3) . . ? C4 N1 C1 105.7(5) . . ? C4 N1 Cu1 126.9(4) . . ? C1 N1 Cu1 126.6(4) . . ? C6 N2 C9 105.6(5) . . ? C6 N2 Cu1 127.3(4) . . ? C9 N2 Cu1 126.9(4) . . ? C11 N3 C14 105.1(5) . . ? C11 N3 Cu1 127.5(4) . . ? C14 N3 Cu1 127.4(4) . . ? C19 N4 C16 105.5(5) . . ? C19 N4 Cu1 127.0(4) . . ? C16 N4 Cu1 127.0(4) . . ? N1 C1 C20 126.1(6) . . ? N1 C1 C2 109.7(5) . . ? C20 C1 C2 124.2(6) . . ? C3 C2 C1 106.8(6) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 106.9(6) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? N1 C4 C5 125.3(6) . . ? N1 C4 C3 110.9(5) . . ? C5 C4 C3 123.8(6) . . ? C6 C5 C4 124.3(6) . . ? C6 C5 C21 117.6(5) . . ? C4 C5 C21 118.0(6) . . ? N2 C6 C5 124.5(6) . . ? N2 C6 C7 110.4(5) . . ? C5 C6 C7 125.1(6) . . ? C8 C7 C6 106.7(6) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 107.1(6) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? C10 C9 N2 125.0(6) . . ? C10 C9 C8 124.8(6) . . ? N2 C9 C8 110.1(6) . . ? C9 C10 C11 124.4(5) . . ? C9 C10 C26 117.6(6) . . ? C11 C10 C26 118.0(6) . . ? N3 C11 C10 124.7(6) . . ? N3 C11 C12 110.9(5) . . ? C10 C11 C12 124.1(5) . . ? C13 C12 C11 106.4(5) . . ? C13 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? C12 C13 C14 107.9(6) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N3 C14 C15 125.5(6) . . ? N3 C14 C13 109.6(5) . . ? C15 C14 C13 124.8(6) . . ? C14 C15 C16 123.7(6) . . ? C14 C15 C31 117.7(5) . . ? C16 C15 C31 118.5(5) . . ? N4 C16 C15 125.2(5) . . ? N4 C16 C17 109.6(5) . . ? C15 C16 C17 125.2(6) . . ? C18 C17 C16 107.6(6) . . ? C18 C17 H17 126.2 . . ? C16 C17 H17 126.2 . . ? C17 C18 C19 106.7(5) . . ? C17 C18 H18 126.7 . . ? C19 C18 H18 126.7 . . ? N4 C19 C20 124.7(5) . . ? N4 C19 C18 110.6(5) . . ? C20 C19 C18 124.5(5) . . ? C1 C20 C19 123.3(5) . . ? C1 C20 C37 119.6(5) . . ? C19 C20 C37 117.2(5) . . ? C25 C21 C22 116.8(6) . . ? C25 C21 C5 119.7(6) . . ? C22 C21 C5 123.5(6) . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N5 C23 C22 123.0(6) . . ? N5 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? C23 N5 C24 117.3(6) . . ? C23 N5 Hg1 126.8(4) . . ? C24 N5 Hg1 115.7(4) . . ? N5 C24 C25 123.7(7) . . ? N5 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C24 C25 C21 119.6(6) . . ? C24 C25 H25 120.2 . . ? C21 C25 H25 120.2 . . ? C30 C26 C27 117.0(6) . . ? C30 C26 C10 121.2(6) . . ? C27 C26 C10 121.8(6) . . ? C28 C27 C26 119.3(6) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? N6 C28 C27 123.5(6) . . ? N6 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C28 N6 C29 117.8(6) . . ? C28 N6 Hg1 123.2(5) . 2_656 ? C29 N6 Hg1 118.5(4) . 2_656 ? N6 C29 C30 122.2(6) . . ? N6 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C26 120.1(6) . . ? C29 C30 H30 119.9 . . ? C26 C30 H30 119.9 . . ? C32 C31 C36 118.7(6) . . ? C32 C31 C15 120.0(6) . . ? C36 C31 C15 121.3(6) . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.7(7) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 119.6(7) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 121.2(7) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C31 119.8(7) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C38 C37 C42 118.6(6) . . ? C38 C37 C20 120.4(6) . . ? C42 C37 C20 121.0(5) . . ? C37 C38 C39 120.1(6) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.3(7) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.9(6) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 118.9(7) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C37 C42 C41 121.2(6) . . ? C37 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? Cl1A C43A Cl3A 113.4(9) . . ? Cl1A C43A Cl2A 116.3(10) . . ? Cl3A C43A Cl2A 109.6(9) . . ? Cl1A C43A H43A 105.5 . . ? Cl3A C43A H43A 105.5 . . ? Cl2A C43A H43A 105.5 . . ? Cl1B C43B Cl2B 103.8(11) . . ? Cl1B C43B Cl3B 109.6(13) . . ? Cl2B C43B Cl3B 107.4(12) . . ? Cl1B C43B H43B 111.9 . . ? Cl2B C43B H43B 111.9 . . ? Cl3B C43B H43B 111.9 . . ? N3 Cu1 N1 174.4(2) . . ? N3 Cu1 N2 90.1(2) . . ? N1 Cu1 N2 90.0(2) . . ? N3 Cu1 N4 90.0(2) . . ? N1 Cu1 N4 90.1(2) . . ? N2 Cu1 N4 177.1(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.984 _refine_diff_density_min -1.606 _refine_diff_density_rms 0.175