# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ljb@sun.ac.za _publ_contact_author_name L.Barbour loop_ _publ_author_name 'Marike du Plessis' 'Leonard J. Barbour' data_twin4.CIF _database_code_depnum_ccdc_archive 'CCDC 840372' #TrackingRef '- Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H24 Br2 Cd N4, C H2 Cl2' _chemical_formula_sum 'C26 H26 Br2 Cd Cl2 N4' _chemical_formula_weight 737.63 _symmetry_space_group_name_Hall '-P 1 ' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.8233(16) _cell_length_b 15.163(2) _cell_length_c 18.137(3) _cell_angle_alpha 82.755(2) _cell_angle_beta 74.833(2) _cell_angle_gamma 71.208(2) _cell_volume 2716.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9377 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.6 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 3.965 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3294 _exptl_absorpt_correction_T_max 0.7167 _exptl_absorpt_process_details 'SAINT (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 24450 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.66 _reflns_number_total 12541 _reflns_number_gt 8720 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001; Atwood & Barbour,2003)' _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^)+(0.1100P)^2^] 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 12541 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.12647(4) 0.45417(3) 0.06873(3) 0.01666(13) Uani 1 1 d . . . Cd2 Cd -0.35876(5) 0.05284(3) 0.43342(3) 0.01958(13) Uani 1 1 d . . . Br1 Br -0.01913(6) 0.37515(4) 0.01996(4) 0.01919(16) Uani 1 1 d . . . Br4 Br -0.61870(6) 0.12487(4) 0.48196(4) 0.02058(16) Uani 1 1 d . . . Br3 Br -0.30214(7) -0.03024(5) 0.30597(4) 0.02241(17) Uani 1 1 d . . . Br2 Br -0.01020(7) 0.54047(5) 0.19350(4) 0.02295(17) Uani 1 1 d . . . N2 N 0.4102(5) 0.4227(4) -0.1548(3) 0.0193(12) Uani 1 1 d . . . N1 N 0.3084(5) 0.4267(4) -0.0310(3) 0.0178(11) Uani 1 1 d . . . N7 N 0.3024(5) -0.0713(4) 0.3397(3) 0.0192(12) Uani 1 1 d . . . C49 C 0.1748(7) 0.0857(5) 0.2326(4) 0.0199(14) Uani 1 1 d . . . N6 N -0.1210(5) 0.2245(4) 0.2863(3) 0.0205(12) Uani 1 1 d . . . C22 C 0.6656(6) 0.7491(4) -0.1184(4) 0.0202(14) Uani 1 1 d . . . C2 C 0.4463(6) 0.4032(4) -0.0380(4) 0.0146(12) Uani 1 1 d . . . C5 C 0.7211(7) 0.3647(4) -0.0852(4) 0.0203(14) Uani 1 1 d . . . H5 H 0.8158 0.3519 -0.0997 0.024 Uiso 1 1 calc R . . N3 N 0.6171(5) 0.7146(4) -0.2206(3) 0.0194(12) Uani 1 1 d . . . N4 N 0.7528(5) 0.6612(4) -0.1405(3) 0.0180(11) Uani 1 1 d . . . C9 C 0.5170(7) 0.4794(4) -0.2827(3) 0.0189(14) Uani 1 1 d . . . C37 C 0.1309(7) 0.0020(5) 0.1189(4) 0.0269(16) Uani 1 1 d . . . H37 H 0.1175 -0.0257 0.0787 0.032 Uiso 1 1 calc R . . N8 N 0.2920(5) -0.0753(4) 0.4642(3) 0.0199(12) Uani 1 1 d . . . C15 C 0.5827(7) 0.6207(5) -0.3098(4) 0.0232(15) Uani 1 1 d . . . N5 N -0.2769(6) 0.1703(4) 0.3665(3) 0.0216(12) Uani 1 1 d . . . C7 C 0.5118(6) 0.4018(4) -0.1156(4) 0.0185(13) Uani 1 1 d . . . C47 C 0.1810(6) -0.0955(4) 0.4553(4) 0.0156(13) Uani 1 1 d . . . C48 C 0.3610(7) -0.0623(5) 0.3941(4) 0.0217(14) Uani 1 1 d . . . H48 H 0.4434 -0.0481 0.3833 0.026 Uiso 1 1 calc R . . C12 C 0.7159(7) 0.4846(5) -0.3777(4) 0.0252(15) Uani 1 1 d . . . H12 H 0.7903 0.4543 -0.4165 0.030 Uiso 1 1 calc R . . C34 C 0.0728(6) 0.1328(5) 0.1944(4) 0.0201(14) Uani 1 1 d . . . C17 C 0.5811(6) 0.7818(4) -0.1689(4) 0.0201(14) Uani 1 1 d . . . C26 C -0.1769(7) 0.1538(5) 0.3049(4) 0.0201(14) Uani 1 1 d . . . H26 H -0.1476 0.0989 0.2769 0.024 Uiso 1 1 calc R . . C4 C 0.6564(7) 0.3632(5) -0.0068(4) 0.0219(14) Uani 1 1 d . . . H4 H 0.7090 0.3475 0.0301 0.026 Uiso 1 1 calc R . . C40 C 0.2534(6) -0.0063(5) 0.2135(4) 0.0202(14) Uani 1 1 d . . . C43 C 0.0839(6) -0.1079(4) 0.3502(4) 0.0200(14) Uani 1 1 d . . . H43 H 0.0867 -0.1045 0.2972 0.024 Uiso 1 1 calc R . . C23 C 0.7193(7) 0.6439(4) -0.2001(4) 0.0202(14) Uani 1 1 d . . . H23 H 0.7617 0.5877 -0.2265 0.024 Uiso 1 1 calc R . . C35 C 0.0489(7) 0.0906(5) 0.1396(4) 0.0239(15) Uani 1 1 d . . . C32 C -0.1902(7) 0.2921(5) 0.3389(4) 0.0242(15) Uani 1 1 d . . . C24 C 0.4929(7) 0.5738(5) -0.2695(4) 0.0214(14) Uani 1 1 d . . . C6 C 0.6506(7) 0.3840(5) -0.1406(4) 0.0209(14) Uani 1 1 d . . . H6 H 0.6936 0.3853 -0.1934 0.025 Uiso 1 1 calc R . . C1 C 0.2933(6) 0.4361(4) -0.1019(4) 0.0178(13) Uani 1 1 d . . . H1 H 0.2086 0.4508 -0.1142 0.021 Uiso 1 1 calc R . . C44 C -0.0201(7) -0.1283(5) 0.4049(4) 0.0254(15) Uani 1 1 d . . . H44 H -0.0917 -0.1381 0.3893 0.030 Uiso 1 1 calc R . . C25 C 0.3715(7) 0.6221(5) -0.2090(4) 0.0248(15) Uani 1 1 d . . . H25A H 0.3961 0.6147 -0.1597 0.037 Uiso 1 1 calc R . . H25B H 0.2996 0.5943 -0.2045 0.037 Uiso 1 1 calc R . . H25C H 0.3403 0.6886 -0.2235 0.037 Uiso 1 1 calc R . . C39 C 0.3158(9) -0.1455(5) 0.1306(5) 0.039(2) Uani 1 1 d . . . H39A H 0.4087 -0.1468 0.1070 0.059 Uiso 1 1 calc R . . H39B H 0.2779 -0.1635 0.0934 0.059 Uiso 1 1 calc R . . H39C H 0.3139 -0.1894 0.1752 0.059 Uiso 1 1 calc R . . C38 C 0.2333(7) -0.0478(5) 0.1557(4) 0.0277(16) Uani 1 1 d . . . C36 C -0.0702(9) 0.1356(6) 0.1021(5) 0.039(2) Uani 1 1 d . . . H36A H -0.1520 0.1600 0.1418 0.058 Uiso 1 1 calc R . . H36B H -0.0821 0.0888 0.0743 0.058 Uiso 1 1 calc R . . H36C H -0.0524 0.1868 0.0665 0.058 Uiso 1 1 calc R . . C45 C -0.0221(7) -0.1347(5) 0.4836(4) 0.0233(15) Uani 1 1 d . . . H45 H -0.0927 -0.1519 0.5197 0.028 Uiso 1 1 calc R . . C13 C 0.6988(7) 0.5747(5) -0.3646(4) 0.0248(15) Uani 1 1 d . . . C42 C 0.1851(6) -0.0927(4) 0.3771(4) 0.0187(14) Uani 1 1 d . . . C27 C -0.2885(7) 0.2568(5) 0.3895(4) 0.0223(14) Uani 1 1 d . . . C14 C 0.8019(8) 0.6219(6) -0.4077(5) 0.039(2) Uani 1 1 d . . . H14A H 0.8771 0.5769 -0.4397 0.058 Uiso 1 1 calc R . . H14B H 0.8349 0.6456 -0.3712 0.058 Uiso 1 1 calc R . . H14C H 0.7606 0.6739 -0.4401 0.058 Uiso 1 1 calc R . . C10 C 0.6291(7) 0.4337(5) -0.3366(4) 0.0231(15) Uani 1 1 d . . . C11 C 0.6659(8) 0.3300(5) -0.3505(5) 0.0335(18) Uani 1 1 d . . . H11A H 0.6805 0.2933 -0.3033 0.050 Uiso 1 1 calc R . . H11B H 0.7481 0.3121 -0.3911 0.050 Uiso 1 1 calc R . . H11C H 0.5925 0.3182 -0.3658 0.050 Uiso 1 1 calc R . . C50 C 0.1972(7) 0.1315(5) 0.2958(4) 0.0248(15) Uani 1 1 d . . . H50A H 0.1647 0.1994 0.2882 0.037 Uiso 1 1 calc R . . H50B H 0.2932 0.1121 0.2946 0.037 Uiso 1 1 calc R . . H50C H 0.1479 0.1125 0.3455 0.037 Uiso 1 1 calc R . . C28 C -0.3764(8) 0.3094(5) 0.4512(4) 0.0329(18) Uani 1 1 d . . . H28 H -0.4444 0.2873 0.4852 0.039 Uiso 1 1 calc R . . C31 C -0.1771(8) 0.3775(5) 0.3488(5) 0.0322(18) Uani 1 1 d . . . H31 H -0.1115 0.4016 0.3144 0.039 Uiso 1 1 calc R . . C46 C 0.0761(7) -0.1166(5) 0.5090(4) 0.0225(15) Uani 1 1 d . . . H46 H 0.0720 -0.1186 0.5621 0.027 Uiso 1 1 calc R . . C29 C -0.3618(9) 0.3926(5) 0.4609(5) 0.039(2) Uani 1 1 d . . . H29 H -0.4198 0.4288 0.5027 0.047 Uiso 1 1 calc R . . C30 C -0.2631(9) 0.4258(5) 0.4107(5) 0.041(2) Uani 1 1 d . . . H30 H -0.2552 0.4839 0.4197 0.049 Uiso 1 1 calc R . . Cl3 Cl 0.3175(2) 0.21381(17) -0.15293(16) 0.0547(6) Uani 1 1 d . . . Cl1 Cl 0.3487(3) 0.3139(3) -0.3785(2) 0.0853(10) Uani 1 1 d . . . Cl4 Cl 0.1384(3) 0.1125(2) -0.0755(2) 0.0958(13) Uani 1 1 d . . . C3 C 0.5196(6) 0.3840(4) 0.0173(4) 0.0181(13) Uani 1 1 d . . . H3 H 0.4766 0.3851 0.0701 0.022 Uiso 1 1 calc R . . C8 C 0.4225(7) 0.4270(5) -0.2382(4) 0.0214(14) Uani 1 1 d . . . H8A H 0.3326 0.4575 -0.2486 0.026 Uiso 1 1 calc R . . H8B H 0.4545 0.3627 -0.2561 0.026 Uiso 1 1 calc R . . C21 C 0.6569(7) 0.8004(5) -0.0578(4) 0.0262(16) Uani 1 1 d . . . H21 H 0.7139 0.7768 -0.0233 0.031 Uiso 1 1 calc R . . C18 C 0.4816(7) 0.8699(5) -0.1608(4) 0.0263(16) Uani 1 1 d . . . H18 H 0.4234 0.8929 -0.1947 0.032 Uiso 1 1 calc R . . C16 C 0.5674(7) 0.7183(5) -0.2887(4) 0.0262(16) Uani 1 1 d . . . H16A H 0.6180 0.7491 -0.3319 0.031 Uiso 1 1 calc R . . H16B H 0.4715 0.7557 -0.2792 0.031 Uiso 1 1 calc R . . C33 C -0.0163(7) 0.2290(5) 0.2179(4) 0.0265(16) Uani 1 1 d . . . H33A H 0.0388 0.2651 0.2278 0.032 Uiso 1 1 calc R . . H33B H -0.0581 0.2617 0.1756 0.032 Uiso 1 1 calc R . . C19 C 0.4744(8) 0.9201(5) -0.1009(5) 0.0354(19) Uani 1 1 d . . . H19 H 0.4084 0.9794 -0.0932 0.043 Uiso 1 1 calc R . . C20 C 0.5616(8) 0.8871(5) -0.0499(4) 0.0322(17) Uani 1 1 d . . . H20 H 0.5542 0.9250 -0.0101 0.039 Uiso 1 1 calc R . . Cl2 Cl 0.0711(4) 0.3601(3) -0.3881(2) 0.0933(11) Uani 1 1 d . . . C41 C 0.3587(7) -0.0606(5) 0.2569(4) 0.0223(14) Uani 1 1 d . . . H41A H 0.4035 -0.1232 0.2359 0.027 Uiso 1 1 calc R . . H41B H 0.4276 -0.0282 0.2489 0.027 Uiso 1 1 calc R . . C52 C 0.1607(10) 0.2003(6) -0.1436(5) 0.049(2) Uani 1 1 d . . . H52A H 0.0897 0.2594 -0.1282 0.059 Uiso 1 1 calc R . . H52B H 0.1535 0.1844 -0.1933 0.059 Uiso 1 1 calc R . . C51 C 0.1998(10) 0.2900(7) -0.3460(7) 0.065(3) Uani 1 1 d . . . H51A H 0.1703 0.2972 -0.2901 0.078 Uiso 1 1 calc R . . H51B H 0.2145 0.2240 -0.3553 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0147(3) 0.0204(2) 0.0144(2) 0.00947(18) -0.00533(18) -0.00690(18) Cd2 0.0178(3) 0.0269(3) 0.0158(2) 0.00981(19) -0.00537(19) -0.0121(2) Br1 0.0187(3) 0.0188(3) 0.0218(3) 0.0120(3) -0.0090(3) -0.0094(3) Br4 0.0175(4) 0.0208(3) 0.0224(3) 0.0129(3) -0.0063(3) -0.0083(3) Br3 0.0238(4) 0.0266(3) 0.0187(3) 0.0095(3) -0.0070(3) -0.0124(3) Br2 0.0218(4) 0.0268(4) 0.0173(3) 0.0056(3) -0.0046(3) -0.0058(3) N2 0.016(3) 0.027(3) 0.015(3) 0.004(2) -0.005(2) -0.008(2) N1 0.015(3) 0.019(3) 0.020(3) 0.010(2) -0.008(2) -0.007(2) N7 0.020(3) 0.022(3) 0.011(3) 0.010(2) 0.000(2) -0.008(2) C49 0.018(3) 0.024(3) 0.019(3) 0.010(3) -0.001(3) -0.014(3) N6 0.021(3) 0.018(3) 0.021(3) 0.012(2) -0.005(2) -0.009(2) C22 0.020(4) 0.020(3) 0.018(3) 0.015(3) -0.005(3) -0.008(3) C2 0.014(3) 0.012(3) 0.016(3) 0.004(2) -0.003(2) -0.004(2) C5 0.016(3) 0.021(3) 0.023(4) 0.010(3) -0.006(3) -0.007(3) N3 0.020(3) 0.017(3) 0.023(3) 0.013(2) -0.012(2) -0.009(2) N4 0.014(3) 0.021(3) 0.017(3) 0.012(2) -0.006(2) -0.006(2) C9 0.026(4) 0.021(3) 0.009(3) 0.012(2) -0.009(3) -0.007(3) C37 0.037(4) 0.035(4) 0.016(3) 0.008(3) -0.008(3) -0.024(3) N8 0.015(3) 0.024(3) 0.021(3) 0.008(2) -0.005(2) -0.008(2) C15 0.023(4) 0.026(4) 0.021(4) 0.010(3) -0.014(3) -0.005(3) N5 0.024(3) 0.023(3) 0.018(3) 0.011(2) -0.008(2) -0.010(2) C7 0.017(3) 0.014(3) 0.023(4) 0.007(3) -0.007(3) -0.004(2) C47 0.014(3) 0.014(3) 0.017(3) 0.007(2) -0.005(2) -0.005(2) C48 0.020(4) 0.027(4) 0.020(3) 0.007(3) -0.004(3) -0.011(3) C12 0.022(4) 0.032(4) 0.017(3) 0.003(3) -0.002(3) -0.005(3) C34 0.017(3) 0.023(3) 0.018(3) 0.015(3) 0.000(3) -0.012(3) C17 0.021(4) 0.016(3) 0.020(3) 0.016(3) -0.007(3) -0.006(3) C26 0.024(4) 0.019(3) 0.020(3) 0.013(3) -0.008(3) -0.012(3) C4 0.020(4) 0.021(3) 0.024(4) 0.009(3) -0.007(3) -0.009(3) C40 0.017(3) 0.026(3) 0.018(3) 0.008(3) -0.003(3) -0.011(3) C43 0.017(3) 0.020(3) 0.024(4) 0.004(3) -0.008(3) -0.006(3) C23 0.019(4) 0.017(3) 0.027(4) 0.013(3) -0.011(3) -0.010(3) C35 0.029(4) 0.026(4) 0.021(4) 0.019(3) -0.014(3) -0.016(3) C32 0.027(4) 0.024(3) 0.021(4) 0.010(3) -0.011(3) -0.007(3) C24 0.020(4) 0.024(3) 0.018(3) 0.008(3) -0.011(3) -0.002(3) C6 0.019(4) 0.024(3) 0.017(3) 0.005(3) 0.000(3) -0.008(3) C1 0.014(3) 0.019(3) 0.020(3) 0.005(3) -0.005(3) -0.006(3) C44 0.013(3) 0.029(4) 0.035(4) 0.010(3) -0.011(3) -0.009(3) C25 0.022(4) 0.027(4) 0.026(4) 0.005(3) -0.010(3) -0.007(3) C39 0.062(6) 0.028(4) 0.030(4) 0.005(3) -0.014(4) -0.014(4) C38 0.033(4) 0.028(4) 0.021(4) 0.004(3) 0.003(3) -0.018(3) C36 0.055(5) 0.036(4) 0.035(5) 0.022(4) -0.022(4) -0.026(4) C45 0.018(4) 0.022(3) 0.028(4) 0.015(3) -0.006(3) -0.008(3) C13 0.028(4) 0.029(4) 0.017(3) 0.018(3) -0.010(3) -0.011(3) C42 0.015(3) 0.015(3) 0.024(4) 0.008(3) -0.006(3) -0.003(2) C27 0.020(4) 0.025(3) 0.019(3) 0.011(3) -0.010(3) -0.004(3) C14 0.037(5) 0.037(5) 0.037(5) 0.021(4) -0.003(4) -0.016(4) C10 0.024(4) 0.028(4) 0.014(3) 0.006(3) -0.007(3) -0.004(3) C11 0.027(4) 0.032(4) 0.033(4) 0.004(3) 0.000(3) -0.005(3) C50 0.030(4) 0.028(4) 0.016(3) 0.004(3) -0.001(3) -0.014(3) C28 0.031(4) 0.033(4) 0.025(4) 0.010(3) -0.010(3) 0.002(3) C31 0.050(5) 0.019(3) 0.034(4) 0.013(3) -0.023(4) -0.014(3) C46 0.017(4) 0.029(4) 0.020(3) 0.011(3) -0.005(3) -0.009(3) C29 0.063(6) 0.027(4) 0.021(4) 0.002(3) -0.017(4) 0.001(4) C30 0.068(6) 0.019(4) 0.040(5) 0.007(3) -0.026(4) -0.010(4) Cl3 0.0373(13) 0.0525(14) 0.0688(17) -0.0084(13) -0.0020(11) -0.0125(10) Cl1 0.068(2) 0.102(3) 0.097(3) -0.038(2) -0.0024(17) -0.0432(18) Cl4 0.090(2) 0.0608(19) 0.106(3) 0.0071(18) 0.032(2) -0.0284(16) C3 0.019(4) 0.021(3) 0.013(3) 0.008(3) -0.005(3) -0.007(3) C8 0.023(4) 0.028(4) 0.014(3) 0.009(3) -0.008(3) -0.011(3) C21 0.030(4) 0.022(3) 0.026(4) 0.008(3) -0.009(3) -0.010(3) C18 0.030(4) 0.022(3) 0.023(4) 0.016(3) -0.008(3) -0.007(3) C16 0.030(4) 0.027(4) 0.027(4) 0.018(3) -0.015(3) -0.016(3) C33 0.030(4) 0.026(4) 0.024(4) 0.020(3) -0.007(3) -0.017(3) C19 0.048(5) 0.019(4) 0.031(4) 0.011(3) -0.004(4) -0.007(3) C20 0.039(5) 0.028(4) 0.024(4) 0.003(3) -0.008(3) -0.003(3) Cl2 0.090(2) 0.106(3) 0.078(2) -0.011(2) -0.048(2) 0.0021(19) C41 0.020(4) 0.026(4) 0.017(3) 0.004(3) -0.001(3) -0.007(3) C52 0.073(7) 0.025(4) 0.047(6) 0.012(4) -0.018(5) -0.012(4) C51 0.051(7) 0.042(6) 0.092(9) 0.011(6) -0.015(6) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.262(6) . ? Cd1 N4 2.303(5) 2_665 ? Cd1 Br2 2.6018(9) . ? Cd1 Br1 2.6295(8) . ? Cd1 Br1 2.9370(8) 2_565 ? Cd2 N8 2.259(6) 2_556 ? Cd2 N5 2.311(5) . ? Cd2 Br3 2.6080(9) . ? Cd2 Br4 2.6172(9) . ? Cd2 Br4 2.9766(8) 2_456 ? Br1 Cd1 2.9369(8) 2_565 ? Br4 Cd2 2.9766(8) 2_456 ? N2 C1 1.347(8) . ? N2 C7 1.394(8) . ? N2 C8 1.477(8) . ? N1 C1 1.322(8) . ? N1 C2 1.393(8) . ? N7 C48 1.346(9) . ? N7 C42 1.392(8) . ? N7 C41 1.475(8) . ? C49 C34 1.407(9) . ? C49 C40 1.411(9) . ? C49 C50 1.519(9) . ? N6 C26 1.360(8) . ? N6 C32 1.378(9) . ? N6 C33 1.456(8) . ? C22 C21 1.391(10) . ? C22 N4 1.398(8) . ? C22 C17 1.398(9) . ? C2 C3 1.383(8) . ? C2 C7 1.400(9) . ? C5 C6 1.363(9) . ? C5 C4 1.412(9) . ? C5 H5 0.9500 . ? N3 C17 1.364(9) . ? N3 C23 1.364(8) . ? N3 C16 1.460(8) . ? N4 C23 1.307(8) . ? N4 Cd1 2.303(5) 2_665 ? C9 C10 1.385(10) . ? C9 C24 1.411(9) . ? C9 C8 1.503(9) . ? C37 C35 1.385(10) . ? C37 C38 1.402(10) . ? C37 H37 0.9500 . ? N8 C48 1.322(8) . ? N8 C47 1.384(8) . ? N8 Cd2 2.259(6) 2_556 ? C15 C24 1.388(9) . ? C15 C13 1.417(10) . ? C15 C16 1.521(10) . ? N5 C26 1.321(9) . ? N5 C27 1.383(9) . ? C7 C6 1.395(9) . ? C47 C46 1.384(9) . ? C47 C42 1.402(9) . ? C48 H48 0.9500 . ? C12 C13 1.362(10) . ? C12 C10 1.409(10) . ? C12 H12 0.9500 . ? C34 C35 1.365(10) . ? C34 C33 1.508(10) . ? C17 C18 1.416(9) . ? C26 H26 0.9500 . ? C4 C3 1.370(9) . ? C4 H4 0.9500 . ? C40 C38 1.384(10) . ? C40 C41 1.516(9) . ? C43 C44 1.382(9) . ? C43 C42 1.401(9) . ? C43 H43 0.9500 . ? C23 H23 0.9500 . ? C35 C36 1.537(10) . ? C32 C31 1.387(10) . ? C32 C27 1.411(9) . ? C24 C25 1.515(10) . ? C6 H6 0.9500 . ? C1 H1 0.9500 . ? C44 C45 1.413(10) . ? C44 H44 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C39 C38 1.518(11) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C45 C46 1.375(9) . ? C45 H45 0.9500 . ? C13 C14 1.512(9) . ? C27 C28 1.404(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C10 C11 1.530(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C28 C29 1.360(11) . ? C28 H28 0.9500 . ? C31 C30 1.373(12) . ? C31 H31 0.9500 . ? C46 H46 0.9500 . ? C29 C30 1.394(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? Cl3 C52 1.737(10) . ? Cl1 C51 1.703(11) . ? Cl4 C52 1.729(9) . ? C3 H3 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C21 C20 1.381(10) . ? C21 H21 0.9500 . ? C18 C19 1.376(11) . ? C18 H18 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C19 C20 1.426(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? Cl2 C51 1.746(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N4 89.49(19) . 2_665 ? N1 Cd1 Br2 149.52(14) . . ? N4 Cd1 Br2 89.12(14) 2_665 . ? N1 Cd1 Br1 99.12(14) . . ? N4 Cd1 Br1 105.03(13) 2_665 . ? Br2 Cd1 Br1 110.63(3) . . ? N1 Cd1 Br1 85.20(13) . 2_565 ? N4 Cd1 Br1 165.91(13) 2_665 2_565 ? Br2 Cd1 Br1 88.88(3) . 2_565 ? Br1 Cd1 Br1 88.71(2) . 2_565 ? N8 Cd2 N5 89.20(19) 2_556 . ? N8 Cd2 Br3 148.73(14) 2_556 . ? N5 Cd2 Br3 89.64(14) . . ? N8 Cd2 Br4 99.63(14) 2_556 . ? N5 Cd2 Br4 107.22(14) . . ? Br3 Cd2 Br4 110.53(3) . . ? N8 Cd2 Br4 83.96(14) 2_556 2_456 ? N5 Cd2 Br4 163.56(14) . 2_456 ? Br3 Cd2 Br4 88.52(3) . 2_456 ? Br4 Cd2 Br4 88.70(2) . 2_456 ? Cd1 Br1 Cd1 91.28(2) . 2_565 ? Cd2 Br4 Cd2 91.30(2) . 2_456 ? C1 N2 C7 107.0(6) . . ? C1 N2 C8 124.3(5) . . ? C7 N2 C8 128.6(6) . . ? C1 N1 C2 105.2(5) . . ? C1 N1 Cd1 120.3(4) . . ? C2 N1 Cd1 134.5(4) . . ? C48 N7 C42 106.9(5) . . ? C48 N7 C41 124.1(5) . . ? C42 N7 C41 129.0(6) . . ? C34 C49 C40 119.1(6) . . ? C34 C49 C50 120.7(6) . . ? C40 C49 C50 120.2(6) . . ? C26 N6 C32 107.6(6) . . ? C26 N6 C33 124.3(6) . . ? C32 N6 C33 127.9(5) . . ? C21 C22 N4 129.3(6) . . ? C21 C22 C17 122.4(6) . . ? N4 C22 C17 108.3(6) . . ? C3 C2 N1 130.6(6) . . ? C3 C2 C7 120.1(6) . . ? N1 C2 C7 109.3(5) . . ? C6 C5 C4 121.5(6) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C17 N3 C23 106.4(5) . . ? C17 N3 C16 128.2(5) . . ? C23 N3 C16 125.2(6) . . ? C23 N4 C22 105.3(5) . . ? C23 N4 Cd1 122.7(4) . 2_665 ? C22 N4 Cd1 128.5(4) . 2_665 ? C10 C9 C24 120.1(6) . . ? C10 C9 C8 119.3(6) . . ? C24 C9 C8 120.6(6) . . ? C35 C37 C38 121.8(6) . . ? C35 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C48 N8 C47 105.5(5) . . ? C48 N8 Cd2 120.4(4) . 2_556 ? C47 N8 Cd2 133.9(4) . 2_556 ? C24 C15 C13 120.7(6) . . ? C24 C15 C16 120.3(6) . . ? C13 C15 C16 118.7(6) . . ? C26 N5 C27 106.1(5) . . ? C26 N5 Cd2 121.6(4) . . ? C27 N5 Cd2 129.9(4) . . ? N2 C7 C6 132.3(6) . . ? N2 C7 C2 105.3(5) . . ? C6 C7 C2 122.4(6) . . ? N8 C47 C46 130.8(6) . . ? N8 C47 C42 109.2(5) . . ? C46 C47 C42 120.0(6) . . ? N8 C48 N7 113.1(6) . . ? N8 C48 H48 123.5 . . ? N7 C48 H48 123.5 . . ? C13 C12 C10 123.5(7) . . ? C13 C12 H12 118.2 . . ? C10 C12 H12 118.2 . . ? C35 C34 C49 120.9(6) . . ? C35 C34 C33 119.8(6) . . ? C49 C34 C33 119.1(6) . . ? N3 C17 C22 106.7(6) . . ? N3 C17 C18 132.1(6) . . ? C22 C17 C18 121.2(7) . . ? N5 C26 N6 112.0(6) . . ? N5 C26 H26 124.0 . . ? N6 C26 H26 124.0 . . ? C3 C4 C5 121.6(6) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C38 C40 C49 120.1(6) . . ? C38 C40 C41 119.7(6) . . ? C49 C40 C41 120.2(6) . . ? C44 C43 C42 116.5(6) . . ? C44 C43 H43 121.8 . . ? C42 C43 H43 121.8 . . ? N4 C23 N3 113.2(6) . . ? N4 C23 H23 123.4 . . ? N3 C23 H23 123.4 . . ? C34 C35 C37 119.3(6) . . ? C34 C35 C36 122.6(7) . . ? C37 C35 C36 118.1(7) . . ? N6 C32 C31 133.1(7) . . ? N6 C32 C27 105.3(6) . . ? C31 C32 C27 121.6(7) . . ? C15 C24 C9 120.0(6) . . ? C15 C24 C25 120.5(6) . . ? C9 C24 C25 119.4(6) . . ? C5 C6 C7 116.5(6) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? N1 C1 N2 113.2(6) . . ? N1 C1 H1 123.4 . . ? N2 C1 H1 123.4 . . ? C43 C44 C45 121.3(6) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 C38 C37 118.7(7) . . ? C40 C38 C39 123.3(7) . . ? C37 C38 C39 118.1(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C46 C45 C44 121.3(6) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C12 C13 C15 117.6(6) . . ? C12 C13 C14 120.0(7) . . ? C15 C13 C14 122.5(7) . . ? N7 C42 C43 132.2(6) . . ? N7 C42 C47 105.3(5) . . ? C43 C42 C47 122.4(6) . . ? N5 C27 C28 131.3(7) . . ? N5 C27 C32 109.0(6) . . ? C28 C27 C32 119.7(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C10 C12 118.1(6) . . ? C9 C10 C11 122.8(6) . . ? C12 C10 C11 119.0(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C29 C28 C27 118.3(8) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C30 C31 C32 116.9(7) . . ? C30 C31 H31 121.6 . . ? C32 C31 H31 121.6 . . ? C45 C46 C47 118.5(6) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? C28 C29 C30 121.2(8) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 122.4(7) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C4 C3 C2 117.8(6) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? N2 C8 C9 113.1(5) . . ? N2 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C20 C21 C22 117.1(7) . . ? C20 C21 H21 121.5 . . ? C22 C21 H21 121.5 . . ? C19 C18 C17 116.0(7) . . ? C19 C18 H18 122.0 . . ? C17 C18 H18 122.0 . . ? N3 C16 C15 110.8(5) . . ? N3 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N6 C33 C34 111.2(5) . . ? N6 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? N6 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C18 C19 C20 122.8(7) . . ? C18 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C21 C20 C19 120.6(7) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N7 C41 C40 113.0(5) . . ? N7 C41 H41A 109.0 . . ? C40 C41 H41A 109.0 . . ? N7 C41 H41B 109.0 . . ? C40 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? Cl4 C52 Cl3 109.8(5) . . ? Cl4 C52 H52A 109.7 . . ? Cl3 C52 H52A 109.7 . . ? Cl4 C52 H52B 109.7 . . ? Cl3 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? Cl1 C51 Cl2 114.7(6) . . ? Cl1 C51 H51A 108.6 . . ? Cl2 C51 H51A 108.6 . . ? Cl1 C51 H51B 108.6 . . ? Cl2 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 Br1 Cd1 -84.93(13) . . . 2_565 ? N4 Cd1 Br1 Cd1 -176.87(14) 2_665 . . 2_565 ? Br2 Cd1 Br1 Cd1 88.31(3) . . . 2_565 ? Br1 Cd1 Br1 Cd1 0.0 2_565 . . 2_565 ? N8 Cd2 Br4 Cd2 -83.65(14) 2_556 . . 2_456 ? N5 Cd2 Br4 Cd2 -175.81(15) . . . 2_456 ? Br3 Cd2 Br4 Cd2 87.93(3) . . . 2_456 ? Br4 Cd2 Br4 Cd2 0.0 2_456 . . 2_456 ? N4 Cd1 N1 C1 146.2(5) 2_665 . . . ? Br2 Cd1 N1 C1 -126.5(4) . . . . ? Br1 Cd1 N1 C1 41.0(5) . . . . ? Br1 Cd1 N1 C1 -46.9(5) 2_565 . . . ? N4 Cd1 N1 C2 -36.9(6) 2_665 . . . ? Br2 Cd1 N1 C2 50.5(7) . . . . ? Br1 Cd1 N1 C2 -142.1(5) . . . . ? Br1 Cd1 N1 C2 130.0(5) 2_565 . . . ? C1 N1 C2 C3 -179.0(6) . . . . ? Cd1 N1 C2 C3 3.7(10) . . . . ? C1 N1 C2 C7 1.7(7) . . . . ? Cd1 N1 C2 C7 -175.5(4) . . . . ? C21 C22 N4 C23 179.3(7) . . . . ? C17 C22 N4 C23 -0.6(7) . . . . ? C21 C22 N4 Cd1 20.2(9) . . . 2_665 ? C17 C22 N4 Cd1 -159.6(4) . . . 2_665 ? N8 Cd2 N5 C26 116.5(5) 2_556 . . . ? Br3 Cd2 N5 C26 -32.3(5) . . . . ? Br4 Cd2 N5 C26 -143.7(5) . . . . ? Br4 Cd2 N5 C26 51.3(8) 2_456 . . . ? N8 Cd2 N5 C27 -43.7(5) 2_556 . . . ? Br3 Cd2 N5 C27 167.6(5) . . . . ? Br4 Cd2 N5 C27 56.2(5) . . . . ? Br4 Cd2 N5 C27 -108.9(6) 2_456 . . . ? C1 N2 C7 C6 -178.2(7) . . . . ? C8 N2 C7 C6 3.9(11) . . . . ? C1 N2 C7 C2 0.5(7) . . . . ? C8 N2 C7 C2 -177.4(6) . . . . ? C3 C2 C7 N2 179.3(5) . . . . ? N1 C2 C7 N2 -1.4(7) . . . . ? C3 C2 C7 C6 -1.8(9) . . . . ? N1 C2 C7 C6 177.5(6) . . . . ? C48 N8 C47 C46 178.8(7) . . . . ? Cd2 N8 C47 C46 -6.1(11) 2_556 . . . ? C48 N8 C47 C42 -1.0(7) . . . . ? Cd2 N8 C47 C42 174.1(4) 2_556 . . . ? C47 N8 C48 N7 0.9(8) . . . . ? Cd2 N8 C48 N7 -175.0(4) 2_556 . . . ? C42 N7 C48 N8 -0.5(8) . . . . ? C41 N7 C48 N8 -179.8(6) . . . . ? C40 C49 C34 C35 0.1(9) . . . . ? C50 C49 C34 C35 -177.5(6) . . . . ? C40 C49 C34 C33 176.6(5) . . . . ? C50 C49 C34 C33 -1.0(9) . . . . ? C23 N3 C17 C22 0.7(7) . . . . ? C16 N3 C17 C22 -174.3(6) . . . . ? C23 N3 C17 C18 -179.5(7) . . . . ? C16 N3 C17 C18 5.6(11) . . . . ? C21 C22 C17 N3 -179.9(6) . . . . ? N4 C22 C17 N3 -0.1(7) . . . . ? C21 C22 C17 C18 0.2(10) . . . . ? N4 C22 C17 C18 -179.9(6) . . . . ? C27 N5 C26 N6 0.6(7) . . . . ? Cd2 N5 C26 N6 -163.7(4) . . . . ? C32 N6 C26 N5 -0.7(8) . . . . ? C33 N6 C26 N5 -174.9(6) . . . . ? C6 C5 C4 C3 -2.0(10) . . . . ? C34 C49 C40 C38 2.6(9) . . . . ? C50 C49 C40 C38 -179.7(6) . . . . ? C34 C49 C40 C41 -176.5(6) . . . . ? C50 C49 C40 C41 1.1(9) . . . . ? C22 N4 C23 N3 1.0(7) . . . . ? Cd1 N4 C23 N3 161.6(4) 2_665 . . . ? C17 N3 C23 N4 -1.1(7) . . . . ? C16 N3 C23 N4 174.1(6) . . . . ? C49 C34 C35 C37 -3.2(10) . . . . ? C33 C34 C35 C37 -179.6(6) . . . . ? C49 C34 C35 C36 173.8(6) . . . . ? C33 C34 C35 C36 -2.6(10) . . . . ? C38 C37 C35 C34 3.6(10) . . . . ? C38 C37 C35 C36 -173.5(6) . . . . ? C26 N6 C32 C31 179.1(7) . . . . ? C33 N6 C32 C31 -7.0(12) . . . . ? C26 N6 C32 C27 0.5(7) . . . . ? C33 N6 C32 C27 174.5(6) . . . . ? C13 C15 C24 C9 0.3(9) . . . . ? C16 C15 C24 C9 -172.0(6) . . . . ? C13 C15 C24 C25 177.8(6) . . . . ? C16 C15 C24 C25 5.5(9) . . . . ? C10 C9 C24 C15 -1.0(9) . . . . ? C8 C9 C24 C15 178.5(6) . . . . ? C10 C9 C24 C25 -178.6(6) . . . . ? C8 C9 C24 C25 0.9(9) . . . . ? C4 C5 C6 C7 -0.2(10) . . . . ? N2 C7 C6 C5 -179.3(6) . . . . ? C2 C7 C6 C5 2.1(9) . . . . ? C2 N1 C1 N2 -1.4(7) . . . . ? Cd1 N1 C1 N2 176.3(4) . . . . ? C7 N2 C1 N1 0.6(7) . . . . ? C8 N2 C1 N1 178.6(6) . . . . ? C42 C43 C44 C45 -1.0(10) . . . . ? C49 C40 C38 C37 -2.3(10) . . . . ? C41 C40 C38 C37 176.9(6) . . . . ? C49 C40 C38 C39 178.6(6) . . . . ? C41 C40 C38 C39 -2.3(10) . . . . ? C35 C37 C38 C40 -0.9(10) . . . . ? C35 C37 C38 C39 178.3(7) . . . . ? C43 C44 C45 C46 3.1(11) . . . . ? C10 C12 C13 C15 -3.9(10) . . . . ? C10 C12 C13 C14 175.9(7) . . . . ? C24 C15 C13 C12 2.1(10) . . . . ? C16 C15 C13 C12 174.5(6) . . . . ? C24 C15 C13 C14 -177.7(6) . . . . ? C16 C15 C13 C14 -5.3(10) . . . . ? C48 N7 C42 C43 178.7(7) . . . . ? C41 N7 C42 C43 -2.0(11) . . . . ? C48 N7 C42 C47 -0.2(7) . . . . ? C41 N7 C42 C47 179.1(6) . . . . ? C44 C43 C42 N7 179.9(7) . . . . ? C44 C43 C42 C47 -1.4(9) . . . . ? N8 C47 C42 N7 0.7(7) . . . . ? C46 C47 C42 N7 -179.1(6) . . . . ? N8 C47 C42 C43 -178.3(6) . . . . ? C46 C47 C42 C43 1.8(10) . . . . ? C26 N5 C27 C28 -179.7(7) . . . . ? Cd2 N5 C27 C28 -17.3(10) . . . . ? C26 N5 C27 C32 -0.2(7) . . . . ? Cd2 N5 C27 C32 162.2(4) . . . . ? N6 C32 C27 N5 -0.2(7) . . . . ? C31 C32 C27 N5 -178.9(6) . . . . ? N6 C32 C27 C28 179.4(6) . . . . ? C31 C32 C27 C28 0.6(10) . . . . ? C24 C9 C10 C12 -0.6(9) . . . . ? C8 C9 C10 C12 179.8(6) . . . . ? C24 C9 C10 C11 176.3(6) . . . . ? C8 C9 C10 C11 -3.3(10) . . . . ? C13 C12 C10 C9 3.2(10) . . . . ? C13 C12 C10 C11 -173.8(7) . . . . ? N5 C27 C28 C29 178.2(7) . . . . ? C32 C27 C28 C29 -1.3(10) . . . . ? N6 C32 C31 C30 -177.7(7) . . . . ? C27 C32 C31 C30 0.7(10) . . . . ? C44 C45 C46 C47 -2.6(10) . . . . ? N8 C47 C46 C45 -179.6(6) . . . . ? C42 C47 C46 C45 0.2(10) . . . . ? C27 C28 C29 C30 0.6(11) . . . . ? C32 C31 C30 C29 -1.4(11) . . . . ? C28 C29 C30 C31 0.7(12) . . . . ? C5 C4 C3 C2 2.3(10) . . . . ? N1 C2 C3 C4 -179.6(6) . . . . ? C7 C2 C3 C4 -0.5(9) . . . . ? C1 N2 C8 C9 136.7(6) . . . . ? C7 N2 C8 C9 -45.7(9) . . . . ? C10 C9 C8 N2 119.5(7) . . . . ? C24 C9 C8 N2 -60.0(8) . . . . ? N4 C22 C21 C20 179.0(6) . . . . ? C17 C22 C21 C20 -1.2(10) . . . . ? N3 C17 C18 C19 -179.7(7) . . . . ? C22 C17 C18 C19 0.1(9) . . . . ? C17 N3 C16 C15 -154.8(6) . . . . ? C23 N3 C16 C15 31.2(9) . . . . ? C24 C15 C16 N3 77.7(8) . . . . ? C13 C15 C16 N3 -94.7(7) . . . . ? C26 N6 C33 C34 -31.0(9) . . . . ? C32 N6 C33 C34 156.0(6) . . . . ? C35 C34 C33 N6 96.5(7) . . . . ? C49 C34 C33 N6 -80.0(7) . . . . ? C17 C18 C19 C20 0.5(10) . . . . ? C22 C21 C20 C19 1.8(11) . . . . ? C18 C19 C20 C21 -1.6(12) . . . . ? C48 N7 C41 C40 -138.2(6) . . . . ? C42 N7 C41 C40 42.7(9) . . . . ? C38 C40 C41 N7 -120.4(7) . . . . ? C49 C40 C41 N7 58.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.422 _refine_diff_density_min -2.501 _refine_diff_density_rms 0.263 # Attachment '- Compound2.cif' data_mdpc55.CIF _database_code_depnum_ccdc_archive 'CCDC 840373' #TrackingRef '- Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H48 Br4 Cd2 N8, 2(C2 H3 N)' _chemical_formula_sum 'C27 H27 Br2 Cd N5' _chemical_formula_weight 693.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.7707(16) _cell_length_b 10.7210(12) _cell_length_c 18.482(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.3540(10) _cell_angle_gamma 90.00 _cell_volume 2725.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9929 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.7 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 3.757 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3220 _exptl_absorpt_correction_T_max 0.6827 _exptl_absorpt_process_details 'SAINT (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17139 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.82 _reflns_number_total 6433 _reflns_number_gt 5943 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001; Atwood & Barbour,2003)' _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^)+(0.0221P)^2^+1.5498P] 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 6433 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0454 _refine_ls_wR_factor_gt 0.0445 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.810779(8) 0.446533(11) 0.162273(7) 0.01481(4) Uani 1 1 d . . . Br1 Br 0.636084(12) 0.420150(16) 0.169670(9) 0.01806(4) Uani 1 1 d . . . Br2 Br 0.904962(13) 0.272691(16) 0.126989(10) 0.02088(4) Uani 1 1 d . . . C2 C 0.95755(12) 0.67340(16) 0.15235(9) 0.0182(3) Uani 1 1 d . . . N2 N 0.99348(11) 0.77836(13) 0.26286(8) 0.0187(3) Uani 1 1 d . . . C7 C 1.01404(13) 0.77155(16) 0.19554(9) 0.0186(3) Uani 1 1 d . . . C11 C 0.90173(15) 1.06140(17) 0.27122(10) 0.0268(4) Uani 1 1 d . . . H11A H 0.8536 1.1283 0.2619 0.040 Uiso 1 1 calc R . . H11B H 0.8817 1.0041 0.2269 0.040 Uiso 1 1 calc R . . H11C H 0.9652 1.0975 0.2777 0.040 Uiso 1 1 calc R . . C10 C 0.90903(13) 0.99099(16) 0.34401(9) 0.0196(3) Uani 1 1 d . . . C9 C 0.97635(13) 0.89414(15) 0.37281(9) 0.0177(3) Uani 1 1 d . . . C8 C 1.04231(13) 0.86035(16) 0.32985(10) 0.0209(4) Uani 1 1 d . . . H8A H 1.0638 0.9376 0.3114 0.025 Uiso 1 1 calc R . . H8B H 1.1008 0.8177 0.3659 0.025 Uiso 1 1 calc R . . C15 C 0.92018(12) 0.86512(15) 0.47982(9) 0.0155(3) Uani 1 1 d . . . C24 C 0.98187(12) 0.82968(15) 0.44070(9) 0.0159(3) Uani 1 1 d . . . C1 C 0.92868(13) 0.68735(16) 0.25848(10) 0.0200(3) Uani 1 1 d . . . H1 H 0.9034 0.6717 0.2981 0.024 Uiso 1 1 calc R . . C16 C 0.92569(12) 0.79772(15) 0.55310(9) 0.0161(3) Uani 1 1 d . . . H16A H 0.9939 0.7740 0.5830 0.019 Uiso 1 1 calc R . . H16B H 0.9035 0.8539 0.5858 0.019 Uiso 1 1 calc R . . C12 C 0.84741(13) 1.02136(16) 0.38274(10) 0.0201(3) Uani 1 1 d . . . H12 H 0.8014 1.0865 0.3629 0.024 Uiso 1 1 calc R . . C25 C 1.05157(13) 0.72134(16) 0.46983(10) 0.0205(3) Uani 1 1 d . . . H25A H 1.1158 0.7530 0.5024 0.031 Uiso 1 1 calc R . . H25B H 1.0567 0.6759 0.4255 0.031 Uiso 1 1 calc R . . H25C H 1.0274 0.6651 0.5005 0.031 Uiso 1 1 calc R . . C14 C 0.77819(13) 0.99248(18) 0.48660(11) 0.0242(4) Uani 1 1 d . . . H14A H 0.7343 1.0574 0.4557 0.036 Uiso 1 1 calc R . . H14B H 0.8126 1.0234 0.5395 0.036 Uiso 1 1 calc R . . H14C H 0.7404 0.9182 0.4885 0.036 Uiso 1 1 calc R . . N1 N 0.90392(11) 0.62203(13) 0.19342(8) 0.0187(3) Uani 1 1 d . . . C13 C 0.85102(12) 0.95933(15) 0.44977(10) 0.0178(3) Uani 1 1 d . . . N3 N 0.86434(10) 0.68484(13) 0.53390(8) 0.0158(3) Uani 1 1 d . . . C23 C 0.81174(12) 0.64251(15) 0.46211(9) 0.0176(3) Uani 1 1 d . . . H23 H 0.8093 0.6840 0.4160 0.021 Uiso 1 1 calc R . . C18 C 0.88672(12) 0.59673(17) 0.66678(10) 0.0194(3) Uani 1 1 d . . . H18 H 0.9311 0.6576 0.6972 0.023 Uiso 1 1 calc R . . C17 C 0.84999(12) 0.60092(15) 0.58582(9) 0.0156(3) Uani 1 1 d . . . C6 C 1.07651(13) 0.84159(18) 0.17031(10) 0.0236(4) Uani 1 1 d . . . H6 H 1.1144 0.9080 0.2003 0.028 Uiso 1 1 calc R . . C3 C 0.96312(13) 0.63997(18) 0.08103(10) 0.0222(4) Uani 1 1 d . . . H3 H 0.9262 0.5726 0.0513 0.027 Uiso 1 1 calc R . . C4 C 1.02477(14) 0.70936(19) 0.05563(10) 0.0271(4) Uani 1 1 d . . . H4 H 1.0299 0.6891 0.0072 0.033 Uiso 1 1 calc R . . C5 C 1.08005(14) 0.80873(19) 0.09918(11) 0.0268(4) Uani 1 1 d . . . H5 H 1.1209 0.8545 0.0792 0.032 Uiso 1 1 calc R . . N4 N 0.76397(10) 0.53842(13) 0.46162(8) 0.0172(3) Uani 1 1 d . . . C22 C 0.78634(11) 0.51056(15) 0.53989(9) 0.0157(3) Uani 1 1 d . . . C21 C 0.75496(13) 0.41213(16) 0.57466(10) 0.0197(3) Uani 1 1 d . . . H21 H 0.7118 0.3501 0.5444 0.024 Uiso 1 1 calc R . . C19 C 0.85494(13) 0.49903(18) 0.70036(10) 0.0232(4) Uani 1 1 d . . . H19 H 0.8779 0.4927 0.7554 0.028 Uiso 1 1 calc R . . N5 N 1.19544(15) 1.08717(19) 0.32007(12) 0.0426(5) Uani 1 1 d . . . C20 C 0.78958(14) 0.40894(18) 0.65517(10) 0.0238(4) Uani 1 1 d . . . H20 H 0.7686 0.3442 0.6804 0.029 Uiso 1 1 calc R . . C26 C 1.25939(16) 1.1535(2) 0.33990(11) 0.0321(4) Uani 1 1 d . . . C27 C 1.33980(18) 1.2409(3) 0.36403(16) 0.0546(7) Uani 1 1 d . . . H27A H 1.3856 1.2196 0.3387 0.082 Uiso 1 1 calc R . . H27B H 1.3730 1.2366 0.4205 0.082 Uiso 1 1 calc R . . H27C H 1.3151 1.3256 0.3492 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01695(6) 0.01567(6) 0.01260(6) 0.00005(4) 0.00633(5) 0.00106(4) Br1 0.01661(8) 0.02560(9) 0.01231(8) -0.00386(6) 0.00567(6) -0.00236(6) Br2 0.02724(9) 0.02101(9) 0.01913(8) 0.00411(6) 0.01406(7) 0.00761(7) C2 0.0187(8) 0.0223(8) 0.0138(8) 0.0018(6) 0.0063(6) 0.0019(7) N2 0.0261(8) 0.0197(7) 0.0135(7) -0.0009(5) 0.0111(6) -0.0058(6) C7 0.0225(8) 0.0219(8) 0.0126(8) 0.0013(6) 0.0077(7) 0.0009(7) C11 0.0379(11) 0.0249(9) 0.0144(8) 0.0040(7) 0.0057(8) -0.0047(8) C10 0.0253(9) 0.0183(8) 0.0113(7) 0.0000(6) 0.0022(6) -0.0069(7) C9 0.0218(8) 0.0171(8) 0.0143(8) -0.0033(6) 0.0064(7) -0.0065(6) C8 0.0282(9) 0.0216(8) 0.0144(8) -0.0039(6) 0.0097(7) -0.0098(7) C15 0.0179(8) 0.0158(7) 0.0111(7) -0.0012(6) 0.0030(6) -0.0041(6) C24 0.0195(8) 0.0145(7) 0.0124(7) -0.0008(6) 0.0043(6) -0.0035(6) C1 0.0261(9) 0.0214(8) 0.0135(8) -0.0004(6) 0.0085(7) -0.0058(7) C16 0.0185(8) 0.0171(8) 0.0123(7) -0.0010(6) 0.0050(6) -0.0029(6) C12 0.0230(9) 0.0163(8) 0.0160(8) 0.0008(6) 0.0010(7) -0.0010(7) C25 0.0239(9) 0.0192(8) 0.0197(8) 0.0008(6) 0.0097(7) 0.0011(7) C14 0.0217(9) 0.0271(9) 0.0235(9) -0.0003(7) 0.0077(7) 0.0031(7) N1 0.0236(7) 0.0220(7) 0.0116(6) -0.0010(5) 0.0078(6) -0.0029(6) C13 0.0175(8) 0.0187(8) 0.0149(8) -0.0035(6) 0.0032(6) -0.0031(6) N3 0.0180(7) 0.0182(7) 0.0115(6) 0.0000(5) 0.0056(5) -0.0028(5) C23 0.0208(8) 0.0193(8) 0.0123(7) -0.0001(6) 0.0055(6) -0.0020(6) C18 0.0181(8) 0.0256(8) 0.0137(8) 0.0005(6) 0.0048(6) -0.0004(7) C17 0.0143(7) 0.0191(8) 0.0143(8) 0.0024(6) 0.0063(6) 0.0010(6) C6 0.0249(9) 0.0269(9) 0.0216(9) 0.0013(7) 0.0117(7) -0.0035(7) C3 0.0213(9) 0.0325(10) 0.0131(8) -0.0017(7) 0.0063(7) 0.0011(7) C4 0.0255(9) 0.0439(11) 0.0149(8) -0.0001(8) 0.0108(7) 0.0036(8) C5 0.0241(9) 0.0382(11) 0.0227(9) 0.0042(8) 0.0139(8) -0.0018(8) N4 0.0197(7) 0.0192(7) 0.0130(7) 0.0011(5) 0.0061(6) -0.0017(6) C22 0.0138(7) 0.0204(8) 0.0132(7) 0.0005(6) 0.0055(6) 0.0019(6) C21 0.0198(8) 0.0205(8) 0.0202(8) 0.0016(6) 0.0088(7) -0.0015(7) C19 0.0244(9) 0.0320(10) 0.0134(8) 0.0053(7) 0.0071(7) 0.0001(8) N5 0.0500(12) 0.0498(12) 0.0385(11) -0.0080(9) 0.0287(10) -0.0186(10) C20 0.0272(9) 0.0263(9) 0.0208(9) 0.0070(7) 0.0123(7) -0.0016(7) C26 0.0327(11) 0.0453(12) 0.0232(10) -0.0016(8) 0.0160(8) -0.0012(10) C27 0.0310(12) 0.084(2) 0.0473(15) -0.0209(14) 0.0128(11) -0.0167(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.2775(15) . ? Cd1 N4 2.3646(14) 2_655 ? Cd1 Br2 2.5485(3) . ? Cd1 Br1 2.6484(4) . ? Cd1 Br1 2.9271(4) 2_655 ? Br1 Cd1 2.9271(4) 2_655 ? C2 N1 1.395(2) . ? C2 C3 1.397(2) . ? C2 C7 1.398(2) . ? N2 C1 1.348(2) . ? N2 C7 1.386(2) . ? N2 C8 1.475(2) . ? C7 C6 1.395(2) . ? C11 C10 1.512(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10 C12 1.386(3) . ? C10 C9 1.402(2) . ? C9 C24 1.409(2) . ? C9 C8 1.508(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C15 C13 1.400(2) . ? C15 C24 1.406(2) . ? C15 C16 1.511(2) . ? C24 C25 1.515(2) . ? C1 N1 1.323(2) . ? C1 H1 0.9500 . ? C16 N3 1.476(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C12 C13 1.390(2) . ? C12 H12 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C14 C13 1.510(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N3 C23 1.349(2) . ? N3 C17 1.387(2) . ? C23 N4 1.319(2) . ? C23 H23 0.9500 . ? C18 C19 1.384(2) . ? C18 C17 1.394(2) . ? C18 H18 0.9500 . ? C17 C22 1.401(2) . ? C6 C5 1.380(3) . ? C6 H6 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.404(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? N4 C22 1.394(2) . ? N4 Cd1 2.3647(14) 2_655 ? C22 C21 1.399(2) . ? C21 C20 1.387(2) . ? C21 H21 0.9500 . ? C19 C20 1.406(3) . ? C19 H19 0.9500 . ? N5 C26 1.132(3) . ? C20 H20 0.9500 . ? C26 C27 1.450(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N4 85.79(5) . 2_655 ? N1 Cd1 Br2 109.46(4) . . ? N4 Cd1 Br2 99.37(3) 2_655 . ? N1 Cd1 Br1 125.83(4) . . ? N4 Cd1 Br1 88.53(4) 2_655 . ? Br2 Cd1 Br1 124.611(9) . . ? N1 Cd1 Br1 84.70(3) . 2_655 ? N4 Cd1 Br1 156.64(3) 2_655 2_655 ? Br2 Cd1 Br1 103.911(7) . 2_655 ? Br1 Cd1 Br1 79.907(7) . 2_655 ? Cd1 Br1 Cd1 98.895(6) . 2_655 ? N1 C2 C3 130.73(16) . . ? N1 C2 C7 109.00(14) . . ? C3 C2 C7 120.24(16) . . ? C1 N2 C7 106.91(14) . . ? C1 N2 C8 126.94(14) . . ? C7 N2 C8 125.81(14) . . ? N2 C7 C6 131.27(16) . . ? N2 C7 C2 105.77(14) . . ? C6 C7 C2 122.96(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C10 C9 119.10(15) . . ? C12 C10 C11 119.66(16) . . ? C9 C10 C11 121.24(17) . . ? C10 C9 C24 120.31(16) . . ? C10 C9 C8 118.88(15) . . ? C24 C9 C8 120.81(16) . . ? N2 C8 C9 111.90(14) . . ? N2 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C13 C15 C24 120.46(15) . . ? C13 C15 C16 119.62(15) . . ? C24 C15 C16 119.88(15) . . ? C15 C24 C9 119.16(15) . . ? C15 C24 C25 120.54(14) . . ? C9 C24 C25 120.28(15) . . ? N1 C1 N2 113.14(15) . . ? N1 C1 H1 123.4 . . ? N2 C1 H1 123.4 . . ? N3 C16 C15 110.41(13) . . ? N3 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? N3 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C10 C12 C13 121.91(16) . . ? C10 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 N1 C2 105.18(14) . . ? C1 N1 Cd1 127.50(11) . . ? C2 N1 Cd1 126.81(11) . . ? C12 C13 C15 118.98(16) . . ? C12 C13 C14 119.13(16) . . ? C15 C13 C14 121.86(15) . . ? C23 N3 C17 106.49(13) . . ? C23 N3 C16 126.57(14) . . ? C17 N3 C16 126.93(13) . . ? N4 C23 N3 114.00(14) . . ? N4 C23 H23 123.0 . . ? N3 C23 H23 123.0 . . ? C19 C18 C17 116.28(16) . . ? C19 C18 H18 121.9 . . ? C17 C18 H18 121.9 . . ? N3 C17 C18 131.73(15) . . ? N3 C17 C22 105.51(14) . . ? C18 C17 C22 122.76(15) . . ? C5 C6 C7 116.11(17) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? C4 C3 C2 117.03(17) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 122.05(17) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.60(17) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C23 N4 C22 104.48(13) . . ? C23 N4 Cd1 114.79(11) . 2_655 ? C22 N4 Cd1 140.03(11) . 2_655 ? N4 C22 C21 130.17(15) . . ? N4 C22 C17 109.50(14) . . ? C21 C22 C17 120.32(15) . . ? C20 C21 C22 117.19(16) . . ? C20 C21 H21 121.4 . . ? C22 C21 H21 121.4 . . ? C18 C19 C20 121.70(16) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 121.73(16) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? N5 C26 C27 178.6(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 Br1 Cd1 -64.69(4) . . . 2_655 ? N4 Cd1 Br1 Cd1 -148.43(3) 2_655 . . 2_655 ? Br2 Cd1 Br1 Cd1 111.192(8) . . . 2_655 ? Br1 Cd1 Br1 Cd1 11.180(8) 2_655 . . 2_655 ? C1 N2 C7 C6 -179.12(19) . . . . ? C8 N2 C7 C6 -5.5(3) . . . . ? C1 N2 C7 C2 0.47(19) . . . . ? C8 N2 C7 C2 174.07(16) . . . . ? N1 C2 C7 N2 -0.07(19) . . . . ? C3 C2 C7 N2 -178.57(16) . . . . ? N1 C2 C7 C6 179.56(16) . . . . ? C3 C2 C7 C6 1.1(3) . . . . ? C12 C10 C9 C24 -0.7(2) . . . . ? C11 C10 C9 C24 -179.95(15) . . . . ? C12 C10 C9 C8 179.20(15) . . . . ? C11 C10 C9 C8 0.0(2) . . . . ? C1 N2 C8 C9 -36.1(2) . . . . ? C7 N2 C8 C9 151.59(16) . . . . ? C10 C9 C8 N2 -81.51(19) . . . . ? C24 C9 C8 N2 98.40(18) . . . . ? C13 C15 C24 C9 3.0(2) . . . . ? C16 C15 C24 C9 -179.49(14) . . . . ? C13 C15 C24 C25 -175.41(15) . . . . ? C16 C15 C24 C25 2.1(2) . . . . ? C10 C9 C24 C15 -1.0(2) . . . . ? C8 C9 C24 C15 179.04(14) . . . . ? C10 C9 C24 C25 177.32(15) . . . . ? C8 C9 C24 C25 -2.6(2) . . . . ? C7 N2 C1 N1 -0.8(2) . . . . ? C8 N2 C1 N1 -174.26(16) . . . . ? C13 C15 C16 N3 92.00(18) . . . . ? C24 C15 C16 N3 -85.57(18) . . . . ? C9 C10 C12 C13 0.6(3) . . . . ? C11 C10 C12 C13 179.86(16) . . . . ? N2 C1 N1 C2 0.7(2) . . . . ? N2 C1 N1 Cd1 172.90(11) . . . . ? C3 C2 N1 C1 177.92(18) . . . . ? C7 C2 N1 C1 -0.37(19) . . . . ? C3 C2 N1 Cd1 5.7(3) . . . . ? C7 C2 N1 Cd1 -172.64(11) . . . . ? N4 Cd1 N1 C1 137.29(16) 2_655 . . . ? Br2 Cd1 N1 C1 -124.25(14) . . . . ? Br1 Cd1 N1 C1 52.15(16) . . . . ? Br1 Cd1 N1 C1 -21.35(15) 2_655 . . . ? N4 Cd1 N1 C2 -52.13(14) 2_655 . . . ? Br2 Cd1 N1 C2 46.33(14) . . . . ? Br1 Cd1 N1 C2 -137.26(12) . . . . ? Br1 Cd1 N1 C2 149.24(14) 2_655 . . . ? C10 C12 C13 C15 1.3(3) . . . . ? C10 C12 C13 C14 -176.74(16) . . . . ? C24 C15 C13 C12 -3.1(2) . . . . ? C16 C15 C13 C12 179.38(14) . . . . ? C24 C15 C13 C14 174.89(15) . . . . ? C16 C15 C13 C14 -2.7(2) . . . . ? C15 C16 N3 C23 1.7(2) . . . . ? C15 C16 N3 C17 -178.93(15) . . . . ? C17 N3 C23 N4 0.0(2) . . . . ? C16 N3 C23 N4 179.45(15) . . . . ? C23 N3 C17 C18 179.21(18) . . . . ? C16 N3 C17 C18 -0.3(3) . . . . ? C23 N3 C17 C22 -0.56(18) . . . . ? C16 N3 C17 C22 179.95(15) . . . . ? C19 C18 C17 N3 178.71(18) . . . . ? C19 C18 C17 C22 -1.6(3) . . . . ? N2 C7 C6 C5 179.50(18) . . . . ? C2 C7 C6 C5 0.0(3) . . . . ? N1 C2 C3 C4 -179.30(17) . . . . ? C7 C2 C3 C4 -1.2(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C7 C6 C5 C4 -0.9(3) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? N3 C23 N4 C22 0.63(19) . . . . ? N3 C23 N4 Cd1 -171.75(11) . . . 2_655 ? C23 N4 C22 C21 178.66(18) . . . . ? Cd1 N4 C22 C21 -12.1(3) 2_655 . . . ? C23 N4 C22 C17 -0.97(18) . . . . ? Cd1 N4 C22 C17 168.23(13) 2_655 . . . ? N3 C17 C22 N4 0.96(18) . . . . ? C18 C17 C22 N4 -178.84(15) . . . . ? N3 C17 C22 C21 -178.71(15) . . . . ? C18 C17 C22 C21 1.5(3) . . . . ? N4 C22 C21 C20 -179.65(17) . . . . ? C17 C22 C21 C20 -0.1(2) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C22 C21 C20 C19 -1.2(3) . . . . ? C18 C19 C20 C21 1.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.666 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.063 # Attachment '- Compound3.cif' data_mdpc66.CIF _database_code_depnum_ccdc_archive 'CCDC 840374' #TrackingRef '- Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H48 Br4 Cd2 N8, 2(C3 H7 N O)' _chemical_formula_sum 'C28 H31 Br2 Cd N5 O' _chemical_formula_weight 725.80 _symmetry_space_group_name_Hall '-P 2yac' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 15.1378(11) _cell_length_b 10.9825(8) _cell_length_c 18.4356(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.6550(10) _cell_angle_gamma 90.00 _cell_volume 2828.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.6 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 3.628 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3320 _exptl_absorpt_correction_T_max 0.6910 _exptl_absorpt_process_details 'SAINT (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17862 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.80 _reflns_number_total 6823 _reflns_number_gt 6275 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour,2001; Atwood & Barbour,2003)' _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^)+(0.0195P)^2^+1.4424P] 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 6823 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0419 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.194041(7) 0.049746(9) 0.337525(6) 0.01207(3) Uani 1 1 d . . . Br1 Br 0.364616(11) 0.076452(15) 0.330906(9) 0.01721(4) Uani 1 1 d . . . Br2 Br 0.106644(11) 0.220609(14) 0.376838(9) 0.01792(4) Uani 1 1 d . . . N2 N 0.36827(9) -0.19228(12) 0.53252(7) 0.0139(2) Uani 1 1 d . . . N1 N 0.26909(9) -0.04730(12) 0.46085(7) 0.0150(3) Uani 1 1 d . . . C5 C 0.37100(11) -0.01020(16) 0.70257(9) 0.0192(3) Uani 1 1 d . . . H5 H 0.3960 -0.0045 0.7583 0.023 Uiso 1 1 calc R . . C9 C 0.42219(11) -0.36742(13) 0.47731(8) 0.0137(3) Uani 1 1 d . . . C1 C 0.31352(11) -0.14998(14) 0.46010(9) 0.0163(3) Uani 1 1 d . . . H1 H 0.3077 -0.1907 0.4130 0.020 Uiso 1 1 calc R . . C4 C 0.30687(12) 0.07945(16) 0.65787(9) 0.0199(3) Uani 1 1 d . . . H4 H 0.2890 0.1434 0.6842 0.024 Uiso 1 1 calc R . . C3 C 0.26898(11) 0.07695(14) 0.57641(9) 0.0168(3) Uani 1 1 d . . . H3 H 0.2265 0.1385 0.5465 0.020 Uiso 1 1 calc R . . C11 C 0.28339(12) -0.49492(16) 0.48057(10) 0.0225(3) Uani 1 1 d . . . H11A H 0.2398 -0.5571 0.4478 0.034 Uiso 1 1 calc R . . H11B H 0.2466 -0.4227 0.4831 0.034 Uiso 1 1 calc R . . H11C H 0.3173 -0.5272 0.5337 0.034 Uiso 1 1 calc R . . C8 C 0.42717(11) -0.30337(14) 0.55135(9) 0.0153(3) Uani 1 1 d . . . H8A H 0.4043 -0.3590 0.5827 0.018 Uiso 1 1 calc R . . H8B H 0.4945 -0.2818 0.5834 0.018 Uiso 1 1 calc R . . C15 C 0.47794(11) -0.39153(14) 0.37131(9) 0.0157(3) Uani 1 1 d . . . C12 C 0.35264(12) -0.51961(15) 0.37801(9) 0.0193(3) Uani 1 1 d . . . H12 H 0.3083 -0.5841 0.3570 0.023 Uiso 1 1 calc R . . C6 C 0.39867(11) -0.10647(15) 0.66770(9) 0.0166(3) Uani 1 1 d . . . H6 H 0.4423 -0.1669 0.6978 0.020 Uiso 1 1 calc R . . C10 C 0.35494(11) -0.46059(14) 0.44538(9) 0.0162(3) Uani 1 1 d . . . C24 C 0.48261(11) -0.33036(14) 0.43973(8) 0.0139(3) Uani 1 1 d . . . C7 C 0.35873(10) -0.10968(14) 0.58578(9) 0.0134(3) Uani 1 1 d . . . C14 C 0.40690(14) -0.55540(16) 0.26752(10) 0.0269(4) Uani 1 1 d . . . H14A H 0.3614 -0.6229 0.2579 0.040 Uiso 1 1 calc R . . H14B H 0.4702 -0.5876 0.2749 0.040 Uiso 1 1 calc R . . H14C H 0.3851 -0.4999 0.2224 0.040 Uiso 1 1 calc R . . C2 C 0.29582(10) -0.01981(14) 0.54013(9) 0.0137(3) Uani 1 1 d . . . C13 C 0.41305(12) -0.48742(15) 0.34039(9) 0.0187(3) Uani 1 1 d . . . N3 N 0.49299(10) -0.27095(12) 0.26365(7) 0.0161(3) Uani 1 1 d . . . C22 C 0.45860(11) -0.15831(14) 0.15603(8) 0.0140(3) Uani 1 1 d . . . C17 C 0.51805(11) -0.25248(14) 0.19960(8) 0.0144(3) Uani 1 1 d . . . C23 C 0.42391(12) -0.18928(15) 0.25734(9) 0.0179(3) Uani 1 1 d . . . H23 H 0.3954 -0.1821 0.2949 0.021 Uiso 1 1 calc R . . C18 C 0.58857(11) -0.30631(14) 0.17886(9) 0.0160(3) Uani 1 1 d . . . H18 H 0.6286 -0.3698 0.2091 0.019 Uiso 1 1 calc R . . C16 C 0.54194(12) -0.35428(15) 0.32947(9) 0.0190(3) Uani 1 1 d . . . H16A H 0.5998 -0.3139 0.3673 0.023 Uiso 1 1 calc R . . H16B H 0.5627 -0.4279 0.3093 0.023 Uiso 1 1 calc R . . C25 C 0.54997(12) -0.22378(14) 0.47094(10) 0.0188(3) Uani 1 1 d . . . H25A H 0.5273 -0.1726 0.5038 0.028 Uiso 1 1 calc R . . H25B H 0.5520 -0.1757 0.4268 0.028 Uiso 1 1 calc R . . H25C H 0.6143 -0.2540 0.5024 0.028 Uiso 1 1 calc R . . N4 N 0.39969(9) -0.12048(12) 0.19418(7) 0.0161(3) Uani 1 1 d . . . N5 N 0.17516(10) -0.33460(14) 0.62232(9) 0.0255(3) Uani 1 1 d . . . C20 C 0.53763(11) -0.16721(15) 0.06725(9) 0.0176(3) Uani 1 1 d . . . H20 H 0.5458 -0.1390 0.0215 0.021 Uiso 1 1 calc R . . C19 C 0.59653(11) -0.26134(14) 0.11151(9) 0.0176(3) Uani 1 1 d . . . H19 H 0.6433 -0.2952 0.0947 0.021 Uiso 1 1 calc R . . C21 C 0.46795(11) -0.11417(14) 0.08819(9) 0.0157(3) Uani 1 1 d . . . H21 H 0.4282 -0.0506 0.0578 0.019 Uiso 1 1 calc R . . C28 C 0.15635(13) -0.20635(17) 0.63000(12) 0.0297(4) Uani 1 1 d . . . H28A H 0.2108 -0.1704 0.6730 0.045 Uiso 1 1 calc R . . H28B H 0.0985 -0.1982 0.6414 0.045 Uiso 1 1 calc R . . H28C H 0.1471 -0.1640 0.5808 0.045 Uiso 1 1 calc R . . C26 C 0.25866(14) -0.3861(2) 0.66676(11) 0.0312(4) Uani 1 1 d . . . H26 H 0.3058 -0.3349 0.7029 0.037 Uiso 1 1 calc R . . C27 C 0.09841(14) -0.40563(18) 0.56575(13) 0.0356(5) Uani 1 1 d . . . H27A H 0.1203 -0.4894 0.5649 0.053 Uiso 1 1 calc R . . H27B H 0.0802 -0.3695 0.5134 0.053 Uiso 1 1 calc R . . H27C H 0.0430 -0.4059 0.5808 0.053 Uiso 1 1 calc R . . O1 O 0.27966(11) -0.49329(16) 0.66495(8) 0.0420(4) 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 Cd1 0.01310(6) 0.01253(5) 0.01177(5) -0.00015(4) 0.00610(4) -0.00008(4) Br1 0.01312(7) 0.02732(9) 0.01202(7) -0.00429(6) 0.00576(6) -0.00357(6) Br2 0.02338(8) 0.01585(8) 0.01886(8) 0.00220(6) 0.01293(6) 0.00486(6) N2 0.0151(6) 0.0156(6) 0.0113(6) -0.0001(5) 0.0053(5) 0.0025(5) N1 0.0165(6) 0.0170(6) 0.0120(6) -0.0004(5) 0.0061(5) 0.0016(5) C5 0.0176(8) 0.0275(9) 0.0125(7) -0.0055(6) 0.0057(6) -0.0022(6) C9 0.0162(7) 0.0132(7) 0.0106(7) 0.0022(5) 0.0038(6) 0.0035(6) C1 0.0200(8) 0.0178(8) 0.0112(7) 0.0005(6) 0.0061(6) 0.0022(6) C4 0.0193(8) 0.0231(8) 0.0190(8) -0.0069(6) 0.0091(7) -0.0013(6) C3 0.0149(7) 0.0182(8) 0.0183(8) -0.0026(6) 0.0075(6) -0.0009(6) C11 0.0203(8) 0.0234(8) 0.0240(8) 0.0034(7) 0.0087(7) -0.0027(7) C8 0.0177(7) 0.0166(7) 0.0114(7) 0.0023(6) 0.0055(6) 0.0038(6) C15 0.0193(8) 0.0159(7) 0.0115(7) 0.0036(6) 0.0053(6) 0.0068(6) C12 0.0217(8) 0.0148(7) 0.0163(7) 0.0003(6) 0.0015(6) 0.0004(6) C6 0.0124(7) 0.0234(8) 0.0131(7) 0.0001(6) 0.0040(6) 0.0000(6) C10 0.0163(7) 0.0152(7) 0.0152(7) 0.0039(6) 0.0041(6) 0.0025(6) C24 0.0160(7) 0.0127(7) 0.0122(7) 0.0029(5) 0.0043(6) 0.0036(6) C7 0.0120(7) 0.0166(7) 0.0135(7) -0.0022(6) 0.0069(6) -0.0018(6) C14 0.0387(11) 0.0237(9) 0.0154(8) -0.0045(7) 0.0071(7) 0.0057(8) C2 0.0120(7) 0.0169(7) 0.0131(7) -0.0023(6) 0.0058(5) -0.0032(6) C13 0.0249(8) 0.0154(7) 0.0118(7) 0.0000(6) 0.0027(6) 0.0065(6) N3 0.0213(7) 0.0177(7) 0.0117(6) 0.0028(5) 0.0089(5) 0.0056(5) C22 0.0155(7) 0.0147(7) 0.0118(7) -0.0014(5) 0.0052(6) 0.0005(6) C17 0.0185(7) 0.0150(7) 0.0104(7) -0.0003(6) 0.0063(6) -0.0003(6) C23 0.0228(8) 0.0195(8) 0.0141(7) 0.0013(6) 0.0099(6) 0.0050(6) C18 0.0166(7) 0.0151(7) 0.0161(7) -0.0016(6) 0.0062(6) 0.0011(6) C16 0.0229(8) 0.0223(8) 0.0134(7) 0.0058(6) 0.0089(6) 0.0099(6) C25 0.0215(8) 0.0179(8) 0.0181(8) -0.0006(6) 0.0087(6) -0.0019(6) N4 0.0196(7) 0.0178(6) 0.0122(6) 0.0005(5) 0.0074(5) 0.0033(5) N5 0.0192(7) 0.0309(8) 0.0271(8) 0.0056(6) 0.0096(6) 0.0041(6) C20 0.0196(8) 0.0199(8) 0.0159(7) -0.0005(6) 0.0097(6) -0.0040(6) C19 0.0178(8) 0.0174(7) 0.0205(8) -0.0042(6) 0.0108(6) -0.0026(6) C21 0.0182(7) 0.0167(7) 0.0118(7) 0.0011(6) 0.0055(6) -0.0002(6) C28 0.0201(9) 0.0320(10) 0.0344(10) 0.0006(8) 0.0077(8) -0.0016(7) C26 0.0238(9) 0.0525(13) 0.0220(9) 0.0092(8) 0.0139(7) 0.0128(9) C27 0.0289(10) 0.0260(10) 0.0448(12) 0.0023(9) 0.0064(9) 0.0013(8) O1 0.0402(8) 0.0571(10) 0.0330(8) 0.0138(7) 0.0188(7) 0.0273(8) _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 N4 2.2827(13) 2 ? Cd1 N1 2.3677(13) . ? Cd1 Br2 2.5565(2) . ? Cd1 Br1 2.6478(3) . ? Cd1 Br1 2.8970(3) 2 ? Br1 Cd1 2.8969(3) 2 ? N2 C1 1.3538(19) . ? N2 C7 1.3846(19) . ? N2 C8 1.4715(19) . ? N1 C1 1.316(2) . ? N1 C2 1.3913(19) . ? C5 C6 1.384(2) . ? C5 C4 1.405(2) . ? C5 H5 0.9500 . ? C9 C10 1.403(2) . ? C9 C24 1.404(2) . ? C9 C8 1.511(2) . ? C1 H1 0.9500 . ? C4 C3 1.386(2) . ? C4 H4 0.9500 . ? C3 C2 1.397(2) . ? C3 H3 0.9500 . ? C11 C10 1.509(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C15 C13 1.403(2) . ? C15 C24 1.407(2) . ? C15 C16 1.509(2) . ? C12 C10 1.389(2) . ? C12 C13 1.390(2) . ? C12 H12 0.9500 . ? C6 C7 1.394(2) . ? C6 H6 0.9500 . ? C24 C25 1.513(2) . ? C7 C2 1.404(2) . ? C14 C13 1.508(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N3 C23 1.348(2) . ? N3 C17 1.3872(19) . ? N3 C16 1.4719(19) . ? C22 N4 1.3950(19) . ? C22 C21 1.398(2) . ? C22 C17 1.403(2) . ? C17 C18 1.396(2) . ? C23 N4 1.316(2) . ? C23 H23 0.9500 . ? C18 C19 1.384(2) . ? C18 H18 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N4 Cd1 2.2827(13) 2 ? N5 C26 1.338(2) . ? N5 C27 1.453(2) . ? N5 C28 1.455(2) . ? C20 C21 1.384(2) . ? C20 C19 1.403(2) . ? C20 H20 0.9500 . ? C19 H19 0.9500 . ? C21 H21 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26 O1 1.223(3) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N1 84.16(5) 2 . ? N4 Cd1 Br2 109.59(3) 2 . ? N1 Cd1 Br2 99.64(3) . . ? N4 Cd1 Br1 126.86(3) 2 . ? N1 Cd1 Br1 88.76(3) . . ? Br2 Cd1 Br1 123.511(7) . . ? N4 Cd1 Br1 84.54(3) 2 2 ? N1 Cd1 Br1 155.57(3) . 2 ? Br2 Cd1 Br1 104.544(6) . 2 ? Br1 Cd1 Br1 80.857(6) . 2 ? Cd1 Br1 Cd1 97.842(6) . 2 ? C1 N2 C7 106.44(12) . . ? C1 N2 C8 127.04(13) . . ? C7 N2 C8 126.52(12) . . ? C1 N1 C2 104.72(13) . . ? C1 N1 Cd1 115.71(10) . . ? C2 N1 Cd1 138.50(10) . . ? C6 C5 C4 121.83(14) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C10 C9 C24 120.65(14) . . ? C10 C9 C8 119.61(14) . . ? C24 C9 C8 119.70(14) . . ? N1 C1 N2 113.89(13) . . ? N1 C1 H1 123.1 . . ? N2 C1 H1 123.1 . . ? C3 C4 C5 121.70(15) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C3 C2 117.29(15) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C8 C9 110.97(12) . . ? N2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C13 C15 C24 120.56(14) . . ? C13 C15 C16 118.87(14) . . ? C24 C15 C16 120.57(14) . . ? C10 C12 C13 122.18(15) . . ? C10 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C5 C6 C7 116.11(15) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? C12 C10 C9 118.66(15) . . ? C12 C10 C11 119.52(15) . . ? C9 C10 C11 121.79(14) . . ? C9 C24 C15 119.14(14) . . ? C9 C24 C25 120.56(13) . . ? C15 C24 C25 120.28(14) . . ? N2 C7 C6 131.64(14) . . ? N2 C7 C2 105.51(12) . . ? C6 C7 C2 122.84(14) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C2 C3 130.36(14) . . ? N1 C2 C7 109.43(13) . . ? C3 C2 C7 120.20(14) . . ? C12 C13 C15 118.74(14) . . ? C12 C13 C14 119.47(15) . . ? C15 C13 C14 121.80(15) . . ? C23 N3 C17 106.65(13) . . ? C23 N3 C16 127.75(13) . . ? C17 N3 C16 125.22(13) . . ? N4 C22 C21 130.72(14) . . ? N4 C22 C17 108.94(13) . . ? C21 C22 C17 120.27(14) . . ? N3 C17 C18 131.28(14) . . ? N3 C17 C22 105.65(13) . . ? C18 C17 C22 123.01(14) . . ? N4 C23 N3 113.63(13) . . ? N4 C23 H23 123.2 . . ? N3 C23 H23 123.2 . . ? C19 C18 C17 115.75(14) . . ? C19 C18 H18 122.1 . . ? C17 C18 H18 122.1 . . ? N3 C16 C15 111.81(13) . . ? N3 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? N3 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 N4 C22 105.11(13) . . ? C23 N4 Cd1 129.10(10) . 2 ? C22 N4 Cd1 124.74(10) . 2 ? C26 N5 C27 121.20(17) . . ? C26 N5 C28 121.57(17) . . ? C27 N5 C28 117.21(15) . . ? C21 C20 C19 122.00(14) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C18 C19 C20 121.95(14) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C20 C21 C22 117.01(14) . . ? C20 C21 H21 121.5 . . ? C22 C21 H21 121.5 . . ? N5 C28 H28A 109.5 . . ? N5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C26 N5 125.7(2) . . ? O1 C26 H26 117.1 . . ? N5 C26 H26 117.1 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd1 Br1 Cd1 64.36(4) 2 . . 2 ? N1 Cd1 Br1 Cd1 146.12(3) . . . 2 ? Br2 Cd1 Br1 Cd1 -113.128(7) . . . 2 ? Br1 Cd1 Br1 Cd1 -11.678(8) 2 . . 2 ? N4 Cd1 N1 C1 64.16(11) 2 . . . ? Br2 Cd1 N1 C1 173.10(11) . . . . ? Br1 Cd1 N1 C1 -63.09(11) . . . . ? Br1 Cd1 N1 C1 1.33(17) 2 . . . ? N4 Cd1 N1 C2 -129.98(15) 2 . . . ? Br2 Cd1 N1 C2 -21.05(15) . . . . ? Br1 Cd1 N1 C2 102.77(15) . . . . ? Br1 Cd1 N1 C2 167.18(10) 2 . . . ? C2 N1 C1 N2 -0.55(18) . . . . ? Cd1 N1 C1 N2 169.81(10) . . . . ? C7 N2 C1 N1 0.10(18) . . . . ? C8 N2 C1 N1 -179.37(14) . . . . ? C6 C5 C4 C3 -0.9(3) . . . . ? C5 C4 C3 C2 1.1(2) . . . . ? C1 N2 C8 C9 1.6(2) . . . . ? C7 N2 C8 C9 -177.74(13) . . . . ? C10 C9 C8 N2 -93.74(16) . . . . ? C24 C9 C8 N2 84.09(17) . . . . ? C4 C5 C6 C7 -0.4(2) . . . . ? C13 C12 C10 C9 -1.6(2) . . . . ? C13 C12 C10 C11 176.34(15) . . . . ? C24 C9 C10 C12 3.2(2) . . . . ? C8 C9 C10 C12 -178.97(14) . . . . ? C24 C9 C10 C11 -174.63(14) . . . . ? C8 C9 C10 C11 3.2(2) . . . . ? C10 C9 C24 C15 -2.8(2) . . . . ? C8 C9 C24 C15 179.37(13) . . . . ? C10 C9 C24 C25 175.48(14) . . . . ? C8 C9 C24 C25 -2.3(2) . . . . ? C13 C15 C24 C9 0.7(2) . . . . ? C16 C15 C24 C9 -179.88(13) . . . . ? C13 C15 C24 C25 -177.57(14) . . . . ? C16 C15 C24 C25 1.8(2) . . . . ? C1 N2 C7 C6 -179.74(16) . . . . ? C8 N2 C7 C6 -0.3(3) . . . . ? C1 N2 C7 C2 0.40(16) . . . . ? C8 N2 C7 C2 179.87(14) . . . . ? C5 C6 C7 N2 -178.31(15) . . . . ? C5 C6 C7 C2 1.5(2) . . . . ? C1 N1 C2 C3 -178.36(16) . . . . ? Cd1 N1 C2 C3 14.8(3) . . . . ? C1 N1 C2 C7 0.79(17) . . . . ? Cd1 N1 C2 C7 -166.05(11) . . . . ? C4 C3 C2 N1 179.10(15) . . . . ? C4 C3 C2 C7 0.0(2) . . . . ? N2 C7 C2 N1 -0.74(16) . . . . ? C6 C7 C2 N1 179.38(14) . . . . ? N2 C7 C2 C3 178.51(13) . . . . ? C6 C7 C2 C3 -1.4(2) . . . . ? C10 C12 C13 C15 -0.5(2) . . . . ? C10 C12 C13 C14 179.91(15) . . . . ? C24 C15 C13 C12 0.9(2) . . . . ? C16 C15 C13 C12 -178.50(14) . . . . ? C24 C15 C13 C14 -179.50(14) . . . . ? C16 C15 C13 C14 1.1(2) . . . . ? C23 N3 C17 C18 176.11(17) . . . . ? C16 N3 C17 C18 2.7(3) . . . . ? C23 N3 C17 C22 -1.15(17) . . . . ? C16 N3 C17 C22 -174.58(14) . . . . ? N4 C22 C17 N3 0.61(17) . . . . ? C21 C22 C17 N3 177.81(14) . . . . ? N4 C22 C17 C18 -176.93(14) . . . . ? C21 C22 C17 C18 0.3(2) . . . . ? C17 N3 C23 N4 1.38(19) . . . . ? C16 N3 C23 N4 174.59(15) . . . . ? N3 C17 C18 C19 -177.17(16) . . . . ? C22 C17 C18 C19 -0.3(2) . . . . ? C23 N3 C16 C15 30.5(2) . . . . ? C17 N3 C16 C15 -157.45(15) . . . . ? C13 C15 C16 N3 83.01(18) . . . . ? C24 C15 C16 N3 -96.38(17) . . . . ? N3 C23 N4 C22 -0.98(19) . . . . ? N3 C23 N4 Cd1 -169.48(11) . . . 2 ? C21 C22 N4 C23 -176.63(16) . . . . ? C17 C22 N4 C23 0.19(17) . . . . ? C21 C22 N4 Cd1 -7.5(2) . . . 2 ? C17 C22 N4 Cd1 169.34(10) . . . 2 ? C17 C18 C19 C20 0.3(2) . . . . ? C21 C20 C19 C18 -0.2(2) . . . . ? C19 C20 C21 C22 0.2(2) . . . . ? N4 C22 C21 C20 176.33(15) . . . . ? C17 C22 C21 C20 -0.2(2) . . . . ? C27 N5 C26 O1 0.5(3) . . . . ? C28 N5 C26 O1 178.75(18) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.396 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.060