# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Miao Du' _publ_contact_author_email DUMIAO@PUBLIC.TPT.TJ.CN _publ_section_title ; Structural diversification and metal-directed assembly of coordination architectures based on tetrabromoterephthalic acid and a bent dipyridyl tecton 2,5-bis(4-pyridyl)-1,3,4-oxadiazole ; loop_ _publ_author_name 'Miao Du' 'Jing Chen' 'Cheng-Peng L' # Attachment 'C003738A.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 763365' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H24 Br8 Co N10 O10' _chemical_formula_weight 1550.94 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.701(3) _cell_length_b 8.7379(14) _cell_length_c 15.466(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.585(3) _cell_angle_gamma 90.00 _cell_volume 2392.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4645 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.63 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1490 _exptl_absorpt_coefficient_mu 7.111 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.487382 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 11729 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4190 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0420P)^2^+4.1654P] 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 4190 _refine_ls_number_parameters 333 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.079 _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 Co1 Co 0.5000 1.0000 1.0000 0.0250(2) Uani 1 2 d S . . Br1 Br 0.79787(3) 1.04932(5) 0.96097(3) 0.03643(14) Uani 1 1 d . . . Br2 Br 0.92179(2) 1.33477(5) 0.93636(3) 0.03487(14) Uani 1 1 d . . . Br3 Br 0.72469(3) 1.73975(5) 1.10462(3) 0.03543(14) Uani 1 1 d . . . Br4 Br 0.60855(3) 1.45076(5) 1.14762(3) 0.03662(14) Uani 1 1 d . . . O1 O 0.59534(16) 1.1492(3) 1.0069(2) 0.0302(7) Uani 1 1 d . . . O2 O 0.66154(17) 1.0550(3) 1.1196(2) 0.0338(7) Uani 1 1 d . . . O3 O 0.91090(18) 1.6807(4) 1.0684(2) 0.0442(9) Uani 1 1 d . . . O4 O 0.86728(19) 1.7001(4) 0.9317(2) 0.0419(8) Uani 1 1 d . . . H4 H 0.9062 1.7482 0.9228 0.063 Uiso 1 1 calc R . . O5 O 0.77036(17) 0.5187(4) 0.7762(2) 0.0330(7) Uani 1 1 d . . . N1 N 0.5710(2) 0.8328(4) 0.9348(3) 0.0309(9) Uani 1 1 d . . . N2 N 0.6893(2) 0.3414(5) 0.8180(3) 0.0388(10) Uani 1 1 d . . . N3 N 0.7489(2) 0.2696(5) 0.7748(3) 0.0382(10) Uani 1 1 d . . . N4 N 1.0058(2) 0.3161(5) 0.6285(3) 0.0456(11) Uani 1 1 d . . . C1 C 0.6013(2) 0.5685(5) 0.9115(3) 0.0317(10) Uani 1 1 d . . . H1 H 0.5907 0.4662 0.9227 0.038 Uiso 1 1 calc R . . C2 C 0.5590(3) 0.6827(5) 0.9485(3) 0.0337(11) Uani 1 1 d . . . H2 H 0.5200 0.6547 0.9850 0.040 Uiso 1 1 calc R . . C3 C 0.6282(3) 0.8702(6) 0.8822(3) 0.0353(11) Uani 1 1 d . . . H3 H 0.6373 0.9732 0.8716 0.042 Uiso 1 1 calc R . . C4 C 0.6737(3) 0.7633(6) 0.8434(3) 0.0354(11) Uani 1 1 d . . . H4A H 0.7133 0.7942 0.8084 0.043 Uiso 1 1 calc R . . C5 C 0.6599(2) 0.6084(5) 0.8570(3) 0.0307(10) Uani 1 1 d . . . C6 C 0.7041(2) 0.4857(5) 0.8175(3) 0.0299(10) Uani 1 1 d . . . C7 C 0.7944(2) 0.3767(5) 0.7511(3) 0.0306(10) Uani 1 1 d . . . C8 C 0.8671(3) 0.3599(5) 0.7071(3) 0.0320(10) Uani 1 1 d . . . C9 C 0.9065(3) 0.4817(6) 0.6728(4) 0.0426(13) Uani 1 1 d . . . H9 H 0.8869 0.5803 0.6759 0.051 Uiso 1 1 calc R . . C10 C 0.9748(3) 0.4557(6) 0.6341(4) 0.0523(15) Uani 1 1 d . . . H10 H 1.0006 0.5384 0.6108 0.063 Uiso 1 1 calc R . . C11 C 0.9666(3) 0.1972(6) 0.6606(4) 0.0469(13) Uani 1 1 d . . . H11 H 0.9870 0.0995 0.6558 0.056 Uiso 1 1 calc R . . C12 C 0.8980(3) 0.2133(6) 0.7002(4) 0.0423(12) Uani 1 1 d . . . H12 H 0.8727 0.1286 0.7219 0.051 Uiso 1 1 calc R . . C13 C 0.7088(2) 1.2730(4) 1.0468(3) 0.0239(9) Uani 1 1 d . . . C14 C 0.6957(2) 1.4178(5) 1.0807(3) 0.0240(9) Uani 1 1 d . . . C15 C 0.7463(2) 1.5385(5) 1.0673(3) 0.0247(9) Uani 1 1 d . . . C16 C 0.8125(2) 1.5133(5) 1.0214(3) 0.0251(9) Uani 1 1 d . . . C17 C 0.8277(2) 1.3673(5) 0.9898(3) 0.0254(9) Uani 1 1 d . . . C18 C 0.7763(2) 1.2486(4) 1.0026(3) 0.0253(9) Uani 1 1 d . . . C19 C 0.6504(2) 1.1455(4) 1.0596(3) 0.0249(9) Uani 1 1 d . . . C20 C 0.8697(2) 1.6427(5) 1.0094(3) 0.0314(11) Uani 1 1 d . . . N5 N 0.5327(2) 0.9060(5) 1.1193(3) 0.0384(10) Uani 1 1 d DU . . C21 C 0.5072(5) 0.8252(7) 1.1715(4) 0.111(3) Uani 1 1 d DU . . C22 C 0.4760(6) 0.6985(8) 1.2208(6) 0.125(4) Uani 1 1 d D . . H22A H 0.4572 0.6217 1.1818 0.187 Uiso 1 1 calc R . . H22B H 0.4355 0.7351 1.2560 0.187 Uiso 1 1 calc R . . H22C H 0.5148 0.6552 1.2571 0.187 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0174(4) 0.0255(4) 0.0321(5) -0.0012(3) 0.0035(3) -0.0026(3) Br1 0.0333(3) 0.0218(2) 0.0544(3) -0.0059(2) 0.0083(2) -0.00092(18) Br2 0.0228(2) 0.0320(2) 0.0501(3) -0.0039(2) 0.0120(2) -0.00079(18) Br3 0.0317(3) 0.0213(2) 0.0535(3) -0.0066(2) 0.0120(2) -0.00313(18) Br4 0.0275(2) 0.0348(3) 0.0478(3) -0.0060(2) 0.0162(2) -0.00589(19) O1 0.0205(15) 0.0307(16) 0.0394(18) 0.0008(14) 0.0012(14) -0.0042(13) O2 0.0304(17) 0.0267(16) 0.044(2) 0.0072(15) -0.0031(15) -0.0068(13) O3 0.0271(18) 0.046(2) 0.059(2) -0.0123(18) 0.0012(17) -0.0135(16) O4 0.0364(19) 0.0363(19) 0.053(2) 0.0087(17) 0.0122(17) -0.0105(15) O5 0.0278(17) 0.0338(17) 0.0376(19) -0.0042(14) 0.0049(14) 0.0059(14) N1 0.0232(19) 0.033(2) 0.037(2) -0.0055(17) 0.0006(16) 0.0015(16) N2 0.034(2) 0.039(2) 0.044(3) -0.0046(19) 0.0058(19) 0.0037(18) N3 0.032(2) 0.038(2) 0.045(3) -0.0042(19) 0.0065(19) 0.0074(18) N4 0.038(2) 0.050(3) 0.049(3) -0.007(2) 0.011(2) 0.010(2) C1 0.027(2) 0.035(2) 0.033(3) -0.002(2) 0.000(2) 0.0017(19) C2 0.025(2) 0.038(3) 0.038(3) -0.004(2) 0.003(2) -0.002(2) C3 0.030(3) 0.035(3) 0.041(3) 0.000(2) 0.005(2) 0.001(2) C4 0.027(2) 0.046(3) 0.033(3) -0.002(2) 0.006(2) 0.001(2) C5 0.020(2) 0.038(3) 0.033(3) -0.002(2) -0.0027(19) 0.0049(19) C6 0.024(2) 0.038(3) 0.028(2) -0.001(2) -0.0009(19) 0.0051(19) C7 0.030(2) 0.031(2) 0.030(2) -0.002(2) 0.000(2) 0.009(2) C8 0.031(2) 0.035(2) 0.030(3) -0.004(2) -0.003(2) 0.007(2) C9 0.042(3) 0.032(3) 0.054(3) -0.001(2) 0.009(3) 0.010(2) C10 0.048(3) 0.042(3) 0.067(4) -0.004(3) 0.017(3) 0.000(3) C11 0.049(3) 0.040(3) 0.052(3) -0.005(3) 0.013(3) 0.013(3) C12 0.044(3) 0.037(3) 0.047(3) -0.002(2) 0.008(2) 0.008(2) C13 0.022(2) 0.020(2) 0.029(2) 0.0013(18) -0.0015(18) -0.0029(17) C14 0.018(2) 0.026(2) 0.028(2) 0.0012(18) 0.0036(17) -0.0002(17) C15 0.022(2) 0.020(2) 0.032(2) -0.0005(18) 0.0003(18) 0.0003(16) C16 0.023(2) 0.024(2) 0.028(2) 0.0001(18) 0.0014(18) -0.0048(17) C17 0.018(2) 0.026(2) 0.033(2) -0.0013(19) 0.0030(18) -0.0012(17) C18 0.024(2) 0.020(2) 0.032(2) -0.0034(18) -0.0002(18) -0.0006(17) C19 0.020(2) 0.017(2) 0.038(3) -0.0040(19) 0.0024(19) -0.0017(16) C20 0.021(2) 0.023(2) 0.050(3) -0.006(2) 0.010(2) -0.0013(18) N5 0.0232(19) 0.048(2) 0.043(2) 0.033(2) -0.0092(17) -0.0222(18) C21 0.088(5) 0.125(7) 0.120(7) 0.024(6) -0.015(5) -0.015(5) C22 0.104(8) 0.152(10) 0.118(9) -0.027(8) 0.013(6) 0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 2.096(4) . ? Co1 N5 2.096(4) 3_677 ? Co1 O1 2.134(3) . ? Co1 O1 2.134(3) 3_677 ? Co1 N1 2.181(4) . ? Co1 N1 2.181(4) 3_677 ? Br1 C18 1.897(4) . ? Br2 C17 1.889(4) . ? Br3 C15 1.891(4) . ? Br4 C14 1.889(4) . ? O1 C19 1.264(5) . ? O2 C19 1.233(5) . ? O3 C20 1.208(6) . ? O4 C20 1.302(6) . ? O4 H4 0.8200 . ? O5 C7 1.369(5) . ? O5 C6 1.372(5) . ? N1 C3 1.345(6) . ? N1 C2 1.345(6) . ? N2 C6 1.287(6) . ? N2 N3 1.403(5) . ? N3 C7 1.290(6) . ? N4 C10 1.341(7) . ? N4 C11 1.348(7) . ? C1 C2 1.376(6) . ? C1 C5 1.389(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.376(6) . ? C3 H3 0.9300 . ? C4 C5 1.391(7) . ? C4 H4A 0.9300 . ? C5 C6 1.465(6) . ? C7 C8 1.469(6) . ? C8 C9 1.380(7) . ? C8 C12 1.397(7) . ? C9 C10 1.374(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.372(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 C18 1.400(6) . ? C13 C19 1.534(5) . ? C14 C15 1.400(6) . ? C15 C16 1.395(6) . ? C16 C17 1.393(6) . ? C16 C20 1.530(6) . ? C17 C18 1.394(6) . ? N5 C21 1.167(8) . ? C21 C22 1.456(11) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 Co1 N5 180 . 3_677 ? N5 Co1 O1 89.09(13) . . ? N5 Co1 O1 90.91(13) 3_677 . ? N5 Co1 O1 90.91(13) . 3_677 ? N5 Co1 O1 89.09(13) 3_677 3_677 ? O1 Co1 O1 180 . 3_677 ? N5 Co1 N1 89.41(16) . . ? N5 Co1 N1 90.59(16) 3_677 . ? O1 Co1 N1 88.47(13) . . ? O1 Co1 N1 91.53(13) 3_677 . ? N5 Co1 N1 90.59(16) . 3_677 ? N5 Co1 N1 89.41(16) 3_677 3_677 ? O1 Co1 N1 91.53(13) . 3_677 ? O1 Co1 N1 88.47(13) 3_677 3_677 ? N1 Co1 N1 180 . 3_677 ? C19 O1 Co1 128.4(3) . . ? C20 O4 H4 109.5 . . ? C7 O5 C6 102.2(3) . . ? C3 N1 C2 116.9(4) . . ? C3 N1 Co1 123.9(3) . . ? C2 N1 Co1 119.2(3) . . ? C6 N2 N3 106.3(4) . . ? C7 N3 N2 106.6(4) . . ? C10 N4 C11 117.7(4) . . ? C2 C1 C5 118.9(4) . . ? C2 C1 H1 120.6 . . ? C5 C1 H1 120.6 . . ? N1 C2 C1 123.7(4) . . ? N1 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? N1 C3 C4 123.1(4) . . ? N1 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C1 C5 C4 118.0(4) . . ? C1 C5 C6 118.3(4) . . ? C4 C5 C6 123.7(4) . . ? N2 C6 O5 112.6(4) . . ? N2 C6 C5 127.2(4) . . ? O5 C6 C5 120.2(4) . . ? N3 C7 O5 112.3(4) . . ? N3 C7 C8 127.7(4) . . ? O5 C7 C8 119.8(4) . . ? C9 C8 C12 118.5(4) . . ? C9 C8 C7 123.3(4) . . ? C12 C8 C7 118.2(4) . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N4 C10 C9 122.8(5) . . ? N4 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N4 C11 C12 123.1(5) . . ? N4 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C8 118.5(5) . . ? C11 C12 H12 120.7 . . ? C8 C12 H12 120.7 . . ? C14 C13 C18 118.0(4) . . ? C14 C13 C19 119.9(4) . . ? C18 C13 C19 122.2(4) . . ? C13 C14 C15 121.4(4) . . ? C13 C14 Br4 119.0(3) . . ? C15 C14 Br4 119.5(3) . . ? C16 C15 C14 119.9(4) . . ? C16 C15 Br3 118.4(3) . . ? C14 C15 Br3 121.6(3) . . ? C17 C16 C15 119.3(4) . . ? C17 C16 C20 120.3(4) . . ? C15 C16 C20 120.4(4) . . ? C16 C17 C18 120.2(4) . . ? C16 C17 Br2 117.7(3) . . ? C18 C17 Br2 121.9(3) . . ? C17 C18 C13 121.1(4) . . ? C17 C18 Br1 120.1(3) . . ? C13 C18 Br1 118.8(3) . . ? O2 C19 O1 128.1(4) . . ? O2 C19 C13 117.4(4) . . ? O1 C19 C13 114.5(4) . . ? O3 C20 O4 127.2(4) . . ? O3 C20 C16 120.4(4) . . ? O4 C20 C16 112.4(4) . . ? C21 N5 Co1 137.9(5) . . ? N5 C21 C22 166.9(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 N5 Co1 O1 C19 10.2(4) . . . . ? N5 Co1 O1 C19 -169.8(4) 3_677 . . . ? N1 Co1 O1 C19 -79.2(4) . . . . ? N1 Co1 O1 C19 100.8(4) 3_677 . . . ? N5 Co1 N1 C3 -121.3(4) . . . . ? N5 Co1 N1 C3 58.7(4) 3_677 . . . ? O1 Co1 N1 C3 -32.2(4) . . . . ? O1 Co1 N1 C3 147.8(4) 3_677 . . . ? N5 Co1 N1 C2 57.2(4) . . . . ? N5 Co1 N1 C2 -122.8(4) 3_677 . . . ? O1 Co1 N1 C2 146.3(4) . . . . ? O1 Co1 N1 C2 -33.7(4) 3_677 . . . ? C6 N2 N3 C7 -0.5(5) . . . . ? C3 N1 C2 C1 -0.5(7) . . . . ? Co1 N1 C2 C1 -179.1(4) . . . . ? C5 C1 C2 N1 0.2(7) . . . . ? C2 N1 C3 C4 -0.3(7) . . . . ? Co1 N1 C3 C4 178.2(4) . . . . ? N1 C3 C4 C5 1.3(8) . . . . ? C2 C1 C5 C4 0.8(7) . . . . ? C2 C1 C5 C6 -179.6(4) . . . . ? C3 C4 C5 C1 -1.6(7) . . . . ? C3 C4 C5 C6 178.9(4) . . . . ? N3 N2 C6 O5 0.2(5) . . . . ? N3 N2 C6 C5 -178.0(4) . . . . ? C7 O5 C6 N2 0.2(5) . . . . ? C7 O5 C6 C5 178.5(4) . . . . ? C1 C5 C6 N2 9.8(7) . . . . ? C4 C5 C6 N2 -170.6(5) . . . . ? C1 C5 C6 O5 -168.3(4) . . . . ? C4 C5 C6 O5 11.3(7) . . . . ? N2 N3 C7 O5 0.7(5) . . . . ? N2 N3 C7 C8 177.0(4) . . . . ? C6 O5 C7 N3 -0.5(5) . . . . ? C6 O5 C7 C8 -177.1(4) . . . . ? N3 C7 C8 C9 170.0(5) . . . . ? O5 C7 C8 C9 -14.0(7) . . . . ? N3 C7 C8 C12 -10.5(7) . . . . ? O5 C7 C8 C12 165.6(4) . . . . ? C12 C8 C9 C10 -0.7(8) . . . . ? C7 C8 C9 C10 178.8(5) . . . . ? C11 N4 C10 C9 1.7(9) . . . . ? C8 C9 C10 N4 -0.5(9) . . . . ? C10 N4 C11 C12 -1.6(9) . . . . ? N4 C11 C12 C8 0.4(9) . . . . ? C9 C8 C12 C11 0.8(8) . . . . ? C7 C8 C12 C11 -178.7(5) . . . . ? C18 C13 C14 C15 3.3(6) . . . . ? C19 C13 C14 C15 -177.4(4) . . . . ? C18 C13 C14 Br4 -175.6(3) . . . . ? C19 C13 C14 Br4 3.6(6) . . . . ? C13 C14 C15 C16 -1.9(7) . . . . ? Br4 C14 C15 C16 177.0(3) . . . . ? C13 C14 C15 Br3 174.5(3) . . . . ? Br4 C14 C15 Br3 -6.6(5) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? Br3 C15 C16 C17 -177.0(3) . . . . ? C14 C15 C16 C20 -177.6(4) . . . . ? Br3 C15 C16 C20 5.9(6) . . . . ? C15 C16 C17 C18 1.3(7) . . . . ? C20 C16 C17 C18 178.4(4) . . . . ? C15 C16 C17 Br2 -174.9(3) . . . . ? C20 C16 C17 Br2 2.3(6) . . . . ? C16 C17 C18 C13 0.2(7) . . . . ? Br2 C17 C18 C13 176.2(3) . . . . ? C16 C17 C18 Br1 -179.0(3) . . . . ? Br2 C17 C18 Br1 -3.1(5) . . . . ? C14 C13 C18 C17 -2.5(7) . . . . ? C19 C13 C18 C17 178.3(4) . . . . ? C14 C13 C18 Br1 176.8(3) . . . . ? C19 C13 C18 Br1 -2.4(6) . . . . ? Co1 O1 C19 O2 -0.4(7) . . . . ? Co1 O1 C19 C13 -179.0(2) . . . . ? C14 C13 C19 O2 -97.3(5) . . . . ? C18 C13 C19 O2 81.9(5) . . . . ? C14 C13 C19 O1 81.5(5) . . . . ? C18 C13 C19 O1 -99.3(5) . . . . ? C17 C16 C20 O3 -101.1(5) . . . . ? C15 C16 C20 O3 76.0(6) . . . . ? C17 C16 C20 O4 78.6(5) . . . . ? C15 C16 C20 O4 -104.3(5) . . . . ? O1 Co1 N5 C21 168.6(7) . . . . ? O1 Co1 N5 C21 -11.4(7) 3_677 . . . ? N1 Co1 N5 C21 -103.0(7) . . . . ? N1 Co1 N5 C21 77.0(7) 3_677 . . . ? Co1 N5 C21 C22 64(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.935 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.094 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 763366' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Br4 N8 Ni O13' _chemical_formula_weight 1141.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ni Ni 0.3393 1.1124 '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 7.9351(4) _cell_length_b 11.3444(5) _cell_length_c 12.9490(6) _cell_angle_alpha 100.7740(10) _cell_angle_beta 107.3420(10) _cell_angle_gamma 101.2400(10) _cell_volume 1053.28(9) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2830 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.90 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 566 _exptl_absorpt_coefficient_mu 4.326 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.548663 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 5446 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3711 _reflns_number_gt 3009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0351P)^2^+1.2924P] 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 3711 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Ni1 Ni 0.0000 0.5000 0.0000 0.02583(16) Uani 1 2 d S . . Br1 Br 0.38650(6) 0.95454(4) 0.14501(4) 0.05036(15) Uani 1 1 d . . . Br2 Br 0.37887(6) 1.22257(4) 0.07648(4) 0.04937(14) Uani 1 1 d . . . O1 O 0.9180(4) 0.6767(3) 0.3752(2) 0.0441(7) Uani 1 1 d . . . O2 O 0.0285(3) 0.6834(2) -0.0003(2) 0.0333(6) Uani 1 1 d . . . O3 O -0.0288(4) 0.7620(2) 0.1545(2) 0.0461(7) Uani 1 1 d . . . O4 O 0.1472(3) 0.4876(2) -0.1071(2) 0.0376(6) Uani 1 1 d . . . H4A H 0.1111 0.4090 -0.1339 0.056 Uiso 1 1 d R . . H4B H 0.1417 0.5318 -0.1537 0.056 Uiso 1 1 d R . . N1 N 0.2488(4) 0.5447(3) 0.1348(3) 0.0321(7) Uani 1 1 d . . . N2 N 0.7981(5) 0.5931(4) 0.4869(3) 0.0523(9) Uani 1 1 d . . . N3 N 0.9889(5) 0.6353(4) 0.5391(3) 0.0527(10) Uani 1 1 d . . . N4 N 1.6065(5) 0.8500(4) 0.5201(4) 0.0578(10) Uani 1 1 d . . . C1 C 0.5868(5) 0.5951(4) 0.3032(3) 0.0371(9) Uani 1 1 d . . . C2 C 0.5704(5) 0.6454(4) 0.2123(3) 0.0407(9) Uani 1 1 d . . . H2 H 0.6721 0.6963 0.2062 0.049 Uiso 1 1 calc R . . C3 C 0.4002(5) 0.6183(4) 0.1315(3) 0.0385(9) Uani 1 1 d . . . H3 H 0.3895 0.6531 0.0711 0.046 Uiso 1 1 calc R . . C4 C 0.2674(5) 0.4982(4) 0.2243(3) 0.0370(9) Uani 1 1 d . . . H4 H 0.1637 0.4478 0.2288 0.044 Uiso 1 1 calc R . . C5 C 0.4307(5) 0.5210(4) 0.3092(3) 0.0429(10) Uani 1 1 d . . . H5 H 0.4370 0.4874 0.3701 0.051 Uiso 1 1 calc R . . C6 C 0.7646(5) 0.6191(4) 0.3913(3) 0.0409(9) Uani 1 1 d . . . C7 C 1.0535(6) 0.6844(4) 0.4721(3) 0.0443(10) Uani 1 1 d . . . C8 C 1.2422(6) 0.7419(4) 0.4873(3) 0.0434(10) Uani 1 1 d . . . C9 C 1.3821(6) 0.7420(5) 0.5830(4) 0.0549(12) Uani 1 1 d . . . H9 H 1.3561 0.7061 0.6374 0.066 Uiso 1 1 calc R . . C10 C 1.5596(6) 0.7968(5) 0.5943(4) 0.0599(13) Uani 1 1 d . . . H10 H 1.6529 0.7966 0.6580 0.072 Uiso 1 1 calc R . . C11 C 1.4715(7) 0.8490(4) 0.4299(4) 0.0587(12) Uani 1 1 d . . . H11 H 1.5018 0.8857 0.3771 0.070 Uiso 1 1 calc R . . C12 C 1.2890(6) 0.7971(4) 0.4098(4) 0.0530(12) Uani 1 1 d . . . H12 H 1.1992 0.7992 0.3453 0.064 Uiso 1 1 calc R . . C13 C 0.0014(5) 0.7668(3) 0.0663(3) 0.0330(8) Uani 1 1 d . . . C14 C 0.0019(5) 0.8890(3) 0.0317(3) 0.0306(8) Uani 1 1 d . . . C15 C 0.1632(5) 0.9825(3) 0.0632(3) 0.0307(8) Uani 1 1 d . . . C16 C 0.1606(5) 1.0925(3) 0.0312(3) 0.0321(8) Uani 1 1 d . . . O5 O 0.1566(5) 0.6501(3) 0.7652(3) 0.0629(9) Uani 1 1 d D . . H5A H 0.1138 0.6277 0.6965 0.094 Uiso 1 1 calc R . . C17 C 0.1473(10) 0.7773(6) 0.8039(6) 0.101(2) Uani 1 1 d D . . H17A H 0.2057 0.8057 0.8838 0.151 Uiso 1 1 calc R . . H17B H 0.0214 0.7792 0.7839 0.151 Uiso 1 1 calc R . . H17C H 0.2087 0.8307 0.7692 0.151 Uiso 1 1 calc R . . O6 O 0.7978(12) 0.9379(8) 0.2556(8) 0.093(3) Uani 0.50 1 d P A 1 O6' O 0.957(3) 0.9894(13) 0.3274(15) 0.195(7) Uani 0.50 1 d P . 2 O7 O 0.9688(11) 0.9307(9) 0.5407(9) 0.120(4) Uani 0.50 1 d P . . 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 Ni1 0.0268(3) 0.0211(3) 0.0317(4) 0.0129(3) 0.0089(3) 0.0074(2) Br1 0.0389(2) 0.0367(2) 0.0643(3) 0.0188(2) -0.0023(2) 0.01160(18) Br2 0.0364(2) 0.0317(2) 0.0720(3) 0.0184(2) 0.0097(2) 0.00088(17) O1 0.0353(15) 0.0499(17) 0.0376(15) 0.0104(13) 0.0007(12) 0.0098(13) O2 0.0397(14) 0.0216(12) 0.0406(15) 0.0126(11) 0.0137(12) 0.0087(11) O3 0.070(2) 0.0340(15) 0.0393(16) 0.0152(13) 0.0220(15) 0.0144(14) O4 0.0404(15) 0.0332(14) 0.0446(16) 0.0156(12) 0.0183(13) 0.0111(12) N1 0.0276(16) 0.0293(16) 0.0389(18) 0.0124(14) 0.0084(14) 0.0078(13) N2 0.039(2) 0.062(2) 0.049(2) 0.023(2) 0.0033(17) 0.0097(17) N3 0.038(2) 0.065(2) 0.046(2) 0.019(2) 0.0001(17) 0.0097(18) N4 0.045(2) 0.057(2) 0.068(3) 0.016(2) 0.019(2) 0.0093(18) C1 0.032(2) 0.038(2) 0.038(2) 0.0072(18) 0.0052(17) 0.0144(17) C2 0.031(2) 0.042(2) 0.046(2) 0.0141(19) 0.0094(18) 0.0061(17) C3 0.038(2) 0.035(2) 0.043(2) 0.0169(18) 0.0116(18) 0.0089(17) C4 0.034(2) 0.038(2) 0.040(2) 0.0196(18) 0.0097(18) 0.0073(17) C5 0.043(2) 0.045(2) 0.040(2) 0.0196(19) 0.0079(19) 0.0114(19) C6 0.034(2) 0.038(2) 0.045(2) 0.0084(19) 0.0089(19) 0.0083(17) C7 0.040(2) 0.046(2) 0.036(2) 0.007(2) -0.0007(19) 0.0136(19) C8 0.039(2) 0.040(2) 0.042(2) 0.0057(19) 0.0043(19) 0.0095(18) C9 0.040(2) 0.069(3) 0.048(3) 0.019(2) 0.004(2) 0.012(2) C10 0.037(2) 0.074(3) 0.058(3) 0.017(3) 0.003(2) 0.012(2) C11 0.063(3) 0.053(3) 0.059(3) 0.019(2) 0.020(3) 0.011(2) C12 0.049(3) 0.051(3) 0.048(3) 0.012(2) 0.004(2) 0.010(2) C13 0.0312(19) 0.0232(19) 0.038(2) 0.0093(17) 0.0034(17) 0.0057(15) C14 0.039(2) 0.0214(17) 0.033(2) 0.0089(15) 0.0114(17) 0.0098(15) C15 0.0325(19) 0.0229(17) 0.032(2) 0.0037(15) 0.0046(16) 0.0102(15) C16 0.034(2) 0.0211(17) 0.037(2) 0.0073(16) 0.0084(17) 0.0042(15) O5 0.070(2) 0.061(2) 0.056(2) 0.0318(17) 0.0160(19) 0.0081(17) C17 0.101(5) 0.112(6) 0.086(5) 0.032(4) 0.037(4) 0.008(4) O6 0.073(5) 0.065(5) 0.116(7) 0.007(5) 0.011(5) 0.014(4) O6' 0.239(19) 0.099(10) 0.205(16) 0.026(10) 0.044(14) 0.022(11) O7 0.054(5) 0.097(7) 0.168(10) -0.040(7) 0.040(6) -0.001(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 Ni1 O2 2.050(2) . ? Ni1 O2 2.050(2) 2_565 ? Ni1 O4 2.066(2) . ? Ni1 O4 2.066(2) 2_565 ? Ni1 N1 2.104(3) 2_565 ? Ni1 N1 2.104(3) . ? Br1 C15 1.894(3) . ? Br2 C16 1.896(3) . ? O1 C6 1.359(5) . ? O1 C7 1.363(5) . ? O2 C13 1.254(4) . ? O3 C13 1.243(5) . ? O4 H4A 0.8501 . ? O4 H4B 0.8499 . ? N1 C3 1.340(5) . ? N1 C4 1.342(5) . ? N2 C6 1.288(5) . ? N2 N3 1.401(5) . ? N3 C7 1.289(6) . ? N4 C11 1.325(6) . ? N4 C10 1.330(6) . ? C1 C2 1.384(6) . ? C1 C5 1.387(6) . ? C1 C6 1.463(5) . ? C2 C3 1.374(5) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.367(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.450(6) . ? C8 C12 1.380(6) . ? C8 C9 1.395(6) . ? C9 C10 1.376(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.377(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.535(5) . ? C14 C16 1.384(5) 2_575 ? C14 C15 1.389(5) . ? C15 C16 1.388(5) . ? C16 C14 1.384(5) 2_575 ? O5 C17 1.460(6) . ? O5 H5A 0.8200 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? O6' O7 1.643(18) 2_776 ? O7 O6' 1.643(18) 2_776 ? 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 O2 Ni1 O2 180 . 2_565 ? O2 Ni1 O4 88.05(10) . . ? O2 Ni1 O4 91.95(10) 2_565 . ? O2 Ni1 O4 91.95(10) . 2_565 ? O2 Ni1 O4 88.05(10) 2_565 2_565 ? O4 Ni1 O4 180 . 2_565 ? O2 Ni1 N1 88.36(10) . 2_565 ? O2 Ni1 N1 91.64(10) 2_565 2_565 ? O4 Ni1 N1 91.83(11) . 2_565 ? O4 Ni1 N1 88.17(11) 2_565 2_565 ? O2 Ni1 N1 91.64(10) . . ? O2 Ni1 N1 88.36(10) 2_565 . ? O4 Ni1 N1 88.17(11) . . ? O4 Ni1 N1 91.83(11) 2_565 . ? N1 Ni1 N1 180 2_565 . ? C6 O1 C7 102.7(3) . . ? C13 O2 Ni1 127.6(2) . . ? Ni1 O4 H4A 97.5 . . ? Ni1 O4 H4B 121.0 . . ? H4A O4 H4B 117.1 . . ? C3 N1 C4 116.8(3) . . ? C3 N1 Ni1 120.1(3) . . ? C4 N1 Ni1 123.0(2) . . ? C6 N2 N3 105.2(4) . . ? C7 N3 N2 107.4(3) . . ? C11 N4 C10 116.9(4) . . ? C2 C1 C5 118.6(3) . . ? C2 C1 C6 121.0(4) . . ? C5 C1 C6 120.4(4) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? N1 C3 C2 123.8(4) . . ? N1 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? N1 C4 C5 123.5(4) . . ? N1 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C4 C5 C1 118.9(4) . . ? C4 C5 H5 120.5 . . ? C1 C5 H5 120.5 . . ? N2 C6 O1 113.1(3) . . ? N2 C6 C1 128.1(4) . . ? O1 C6 C1 118.8(4) . . ? N3 C7 O1 111.6(4) . . ? N3 C7 C8 129.0(4) . . ? O1 C7 C8 119.4(4) . . ? C12 C8 C9 118.4(4) . . ? C12 C8 C7 122.1(4) . . ? C9 C8 C7 119.5(4) . . ? C10 C9 C8 117.9(5) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N4 C10 C9 124.2(4) . . ? N4 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N4 C11 C12 124.0(5) . . ? N4 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C8 118.6(4) . . ? C11 C12 H12 120.7 . . ? C8 C12 H12 120.7 . . ? O3 C13 O2 128.4(3) . . ? O3 C13 C14 116.7(3) . . ? O2 C13 C14 114.8(3) . . ? C16 C14 C15 119.1(3) 2_575 . ? C16 C14 C13 119.9(3) 2_575 . ? C15 C14 C13 121.1(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 Br1 120.9(3) . . ? C14 C15 Br1 118.9(3) . . ? C14 C16 C15 120.8(3) 2_575 . ? C14 C16 Br2 118.5(3) 2_575 . ? C15 C16 Br2 120.7(3) . . ? C17 O5 H5A 109.5 . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 O4 Ni1 O2 C13 -164.9(3) . . . . ? O4 Ni1 O2 C13 15.1(3) 2_565 . . . ? N1 Ni1 O2 C13 103.2(3) 2_565 . . . ? N1 Ni1 O2 C13 -76.8(3) . . . . ? O2 Ni1 N1 C3 -49.4(3) . . . . ? O2 Ni1 N1 C3 130.6(3) 2_565 . . . ? O4 Ni1 N1 C3 38.6(3) . . . . ? O4 Ni1 N1 C3 -141.4(3) 2_565 . . . ? O2 Ni1 N1 C4 133.7(3) . . . . ? O2 Ni1 N1 C4 -46.3(3) 2_565 . . . ? O4 Ni1 N1 C4 -138.3(3) . . . . ? O4 Ni1 N1 C4 41.7(3) 2_565 . . . ? C6 N2 N3 C7 0.9(5) . . . . ? C5 C1 C2 C3 -0.8(6) . . . . ? C6 C1 C2 C3 179.3(4) . . . . ? C4 N1 C3 C2 1.6(6) . . . . ? Ni1 N1 C3 C2 -175.6(3) . . . . ? C1 C2 C3 N1 -0.7(6) . . . . ? C3 N1 C4 C5 -0.9(6) . . . . ? Ni1 N1 C4 C5 176.1(3) . . . . ? N1 C4 C5 C1 -0.6(6) . . . . ? C2 C1 C5 C4 1.4(6) . . . . ? C6 C1 C5 C4 -178.6(4) . . . . ? N3 N2 C6 O1 -0.5(5) . . . . ? N3 N2 C6 C1 180.0(4) . . . . ? C7 O1 C6 N2 -0.1(5) . . . . ? C7 O1 C6 C1 179.5(3) . . . . ? C2 C1 C6 N2 170.1(4) . . . . ? C5 C1 C6 N2 -9.9(7) . . . . ? C2 C1 C6 O1 -9.5(6) . . . . ? C5 C1 C6 O1 170.6(4) . . . . ? N2 N3 C7 O1 -1.0(5) . . . . ? N2 N3 C7 C8 179.6(4) . . . . ? C6 O1 C7 N3 0.7(5) . . . . ? C6 O1 C7 C8 -179.8(4) . . . . ? N3 C7 C8 C12 -176.2(5) . . . . ? O1 C7 C8 C12 4.5(6) . . . . ? N3 C7 C8 C9 3.8(7) . . . . ? O1 C7 C8 C9 -175.5(4) . . . . ? C12 C8 C9 C10 -0.3(7) . . . . ? C7 C8 C9 C10 179.6(4) . . . . ? C11 N4 C10 C9 -0.1(8) . . . . ? C8 C9 C10 N4 0.2(8) . . . . ? C10 N4 C11 C12 0.2(7) . . . . ? N4 C11 C12 C8 -0.3(7) . . . . ? C9 C8 C12 C11 0.4(7) . . . . ? C7 C8 C12 C11 -179.6(4) . . . . ? Ni1 O2 C13 O3 8.8(6) . . . . ? Ni1 O2 C13 C14 -169.7(2) . . . . ? O3 C13 C14 C16 -86.8(4) . . . 2_575 ? O2 C13 C14 C16 91.9(4) . . . 2_575 ? O3 C13 C14 C15 92.8(4) . . . . ? O2 C13 C14 C15 -88.5(4) . . . . ? C16 C14 C15 C16 -0.3(6) 2_575 . . . ? C13 C14 C15 C16 -179.9(3) . . . . ? C16 C14 C15 Br1 -177.9(3) 2_575 . . . ? C13 C14 C15 Br1 2.6(5) . . . . ? C14 C15 C16 C14 0.3(6) . . . 2_575 ? Br1 C15 C16 C14 177.8(3) . . . 2_575 ? C14 C15 C16 Br2 178.5(3) . . . . ? Br1 C15 C16 Br2 -3.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.539 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.076 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 763367' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Br4 N8 O10 Zn' _chemical_formula_weight 1065.60 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' Br Br -0.2901 2.4595 '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 8.1293(9) _cell_length_b 10.9582(11) _cell_length_c 11.4728(12) _cell_angle_alpha 63.567(2) _cell_angle_beta 76.532(2) _cell_angle_gamma 86.0070(10) _cell_volume 889.33(16) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3651 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.90 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 5.254 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.587688 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 4560 _diffrn_reflns_av_R_equivalents 0.0098 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3098 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0248P)^2^+0.7441P] 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 3098 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Br1 Br 0.32122(3) 0.15002(3) 0.01723(3) 0.04524(10) Uani 1 1 d . . . Br2 Br 0.35048(3) 0.05638(3) -0.22872(3) 0.03666(9) Uani 1 1 d . . . Zn1 Zn 0.0000 0.0000 0.5000 0.02239(10) Uani 1 2 d S . . N1 N 0.1865(2) 0.1661(2) 0.4183(2) 0.0270(4) Uani 1 1 d . . . N2 N 0.5757(3) 0.5569(2) 0.3370(2) 0.0400(6) Uani 1 1 d . . . N3 N 0.7409(3) 0.6133(2) 0.2934(3) 0.0404(6) Uani 1 1 d . . . N4 N 1.3551(3) 0.6165(3) 0.0571(3) 0.0457(6) Uani 1 1 d . . . O1 O 0.7410(2) 0.43851(17) 0.24737(17) 0.0297(4) Uani 1 1 d . . . O2 O 0.0343(2) -0.00764(17) 0.31484(16) 0.0287(4) Uani 1 1 d . . . O3 O -0.0909(3) 0.18512(18) 0.20322(18) 0.0398(5) Uani 1 1 d . . . O4 O -0.1986(2) 0.13475(18) 0.45709(18) 0.0350(4) Uani 1 1 d . . . H4A H -0.2285 0.1871 0.4944 0.052 Uiso 1 1 d R . . H4B H -0.1745 0.1717 0.3722 0.052 Uiso 1 1 d R . . C1 C 0.4467(3) 0.3571(2) 0.3412(2) 0.0277(5) Uani 1 1 d . . . C2 C 0.2911(3) 0.3636(3) 0.4200(3) 0.0347(6) Uani 1 1 d . . . H2 H 0.2717 0.4321 0.4479 0.042 Uiso 1 1 calc R . . C3 C 0.1665(3) 0.2666(3) 0.4557(3) 0.0328(6) Uani 1 1 d . . . H3 H 0.0628 0.2712 0.5086 0.039 Uiso 1 1 calc R . . C4 C 0.3358(3) 0.1625(3) 0.3410(3) 0.0306(6) Uani 1 1 d . . . H4 H 0.3510 0.0940 0.3131 0.037 Uiso 1 1 calc R . . C5 C 0.4686(3) 0.2547(3) 0.3001(3) 0.0307(6) Uani 1 1 d . . . H5 H 0.5705 0.2483 0.2463 0.037 Uiso 1 1 calc R . . C6 C 0.5821(3) 0.4551(3) 0.3089(2) 0.0289(5) Uani 1 1 d . . . C7 C 0.8321(3) 0.5415(2) 0.2417(3) 0.0288(5) Uani 1 1 d . . . C8 C 1.0127(3) 0.5628(2) 0.1789(2) 0.0292(5) Uani 1 1 d . . . C9 C 1.0987(3) 0.6726(3) 0.1710(3) 0.0367(6) Uani 1 1 d . . . H9 H 1.0431 0.7299 0.2064 0.044 Uiso 1 1 calc R . . C10 C 1.2671(4) 0.6944(3) 0.1097(3) 0.0438(7) Uani 1 1 d . . . H10 H 1.3238 0.7682 0.1044 0.053 Uiso 1 1 calc R . . C11 C 1.2707(4) 0.5114(3) 0.0659(3) 0.0417(7) Uani 1 1 d . . . H11 H 1.3300 0.4557 0.0299 0.050 Uiso 1 1 calc R . . C12 C 1.1008(3) 0.4801(3) 0.1252(3) 0.0358(6) Uani 1 1 d . . . H12 H 1.0472 0.4057 0.1289 0.043 Uiso 1 1 calc R . . C13 C -0.0105(3) 0.0363(2) 0.1041(2) 0.0233(5) Uani 1 1 d . . . C14 C 0.1379(3) 0.0608(2) 0.0068(2) 0.0251(5) Uani 1 1 d . . . C15 C 0.1488(3) 0.0249(2) -0.0962(2) 0.0238(5) Uani 1 1 d . . . C16 C -0.0242(3) 0.0762(2) 0.2176(2) 0.0254(5) Uani 1 1 d . . . O5 O 0.7126(3) 0.2902(3) 0.5928(3) 0.0694(7) Uani 1 1 d . . . H5A H 0.6242 0.3282 0.6150 0.104 Uiso 1 1 d R . . H5B H 0.7480 0.2249 0.6556 0.104 Uiso 1 1 d 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 Br1 0.03113(15) 0.0758(2) 0.04012(17) -0.03535(16) -0.00276(12) -0.01774(13) Br2 0.02715(14) 0.05020(17) 0.03445(15) -0.02519(13) 0.00463(11) -0.00345(11) Zn1 0.0222(2) 0.0267(2) 0.0214(2) -0.01368(16) -0.00368(15) -0.00062(15) N1 0.0259(11) 0.0306(11) 0.0264(11) -0.0149(9) -0.0036(9) -0.0021(8) N2 0.0298(12) 0.0406(13) 0.0532(15) -0.0295(12) 0.0048(11) -0.0086(10) N3 0.0287(12) 0.0418(13) 0.0546(15) -0.0291(12) 0.0027(11) -0.0093(10) N4 0.0283(12) 0.0536(15) 0.0466(15) -0.0171(13) -0.0018(11) -0.0023(11) O1 0.0232(9) 0.0305(9) 0.0372(10) -0.0183(8) -0.0020(7) -0.0032(7) O2 0.0339(9) 0.0354(9) 0.0212(9) -0.0164(8) -0.0060(7) 0.0004(7) O3 0.0613(13) 0.0324(10) 0.0317(10) -0.0194(8) -0.0121(9) 0.0080(9) O4 0.0375(10) 0.0393(10) 0.0313(10) -0.0193(8) -0.0087(8) 0.0110(8) C1 0.0241(12) 0.0324(13) 0.0274(13) -0.0142(11) -0.0040(10) -0.0025(10) C2 0.0335(14) 0.0368(14) 0.0386(15) -0.0246(13) 0.0008(12) -0.0039(11) C3 0.0254(13) 0.0386(15) 0.0362(14) -0.0222(12) 0.0030(11) -0.0042(11) C4 0.0299(14) 0.0338(14) 0.0326(14) -0.0205(12) -0.0021(11) -0.0014(10) C5 0.0233(12) 0.0374(14) 0.0331(14) -0.0202(12) 0.0002(11) -0.0007(10) C6 0.0259(13) 0.0318(13) 0.0288(13) -0.0144(11) -0.0029(10) -0.0012(10) C7 0.0279(13) 0.0269(13) 0.0323(14) -0.0140(11) -0.0051(11) -0.0029(10) C8 0.0254(13) 0.0290(13) 0.0286(13) -0.0088(11) -0.0053(10) -0.0009(10) C9 0.0295(14) 0.0325(14) 0.0473(16) -0.0178(13) -0.0066(12) -0.0001(11) C10 0.0320(15) 0.0397(16) 0.0542(19) -0.0161(14) -0.0067(13) -0.0083(12) C11 0.0334(15) 0.0518(18) 0.0399(16) -0.0224(14) -0.0055(13) 0.0075(13) C12 0.0345(15) 0.0356(15) 0.0375(15) -0.0165(13) -0.0079(12) 0.0011(11) C13 0.0294(13) 0.0249(12) 0.0185(11) -0.0112(10) -0.0077(10) 0.0023(10) C14 0.0240(12) 0.0305(13) 0.0244(12) -0.0141(11) -0.0072(10) -0.0020(10) C15 0.0218(12) 0.0296(12) 0.0210(12) -0.0131(10) -0.0024(9) 0.0006(9) C16 0.0288(13) 0.0279(13) 0.0212(12) -0.0133(10) -0.0019(10) -0.0049(10) O5 0.0612(15) 0.0899(19) 0.0786(18) -0.0634(16) -0.0020(13) 0.0075(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 Br1 C14 1.892(2) . ? Br2 C15 1.889(2) . ? Zn1 O4 2.1027(17) 2_556 ? Zn1 O4 2.1027(17) . ? Zn1 O2 2.1157(16) . ? Zn1 O2 2.1157(16) 2_556 ? Zn1 N1 2.167(2) 2_556 ? Zn1 N1 2.167(2) . ? N1 C4 1.336(3) . ? N1 C3 1.336(3) . ? N2 C6 1.286(3) . ? N2 N3 1.401(3) . ? N3 C7 1.284(3) . ? N4 C10 1.332(4) . ? N4 C11 1.335(4) . ? O1 C6 1.362(3) . ? O1 C7 1.363(3) . ? O2 C16 1.260(3) . ? O3 C16 1.234(3) . ? O4 H4A 0.8501 . ? O4 H4B 0.8501 . ? C1 C5 1.385(3) . ? C1 C2 1.391(3) . ? C1 C6 1.457(3) . ? C2 C3 1.376(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.379(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.460(3) . ? C8 C12 1.384(4) . ? C8 C9 1.391(4) . ? C9 C10 1.369(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.387(3) . ? C13 C15 1.388(3) 2 ? C13 C16 1.528(3) . ? C14 C15 1.387(3) . ? C15 C13 1.388(3) 2 ? O5 H5A 0.8500 . ? O5 H5B 0.8500 . ? 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 O4 Zn1 O4 180.0 2_556 . ? O4 Zn1 O2 88.70(7) 2_556 . ? O4 Zn1 O2 91.30(7) . . ? O4 Zn1 O2 91.30(7) 2_556 2_556 ? O4 Zn1 O2 88.70(7) . 2_556 ? O2 Zn1 O2 180.0 . 2_556 ? O4 Zn1 N1 92.32(7) 2_556 2_556 ? O4 Zn1 N1 87.68(7) . 2_556 ? O2 Zn1 N1 87.38(7) . 2_556 ? O2 Zn1 N1 92.62(7) 2_556 2_556 ? O4 Zn1 N1 87.68(7) 2_556 . ? O4 Zn1 N1 92.32(7) . . ? O2 Zn1 N1 92.62(7) . . ? O2 Zn1 N1 87.38(7) 2_556 . ? N1 Zn1 N1 180.00(8) 2_556 . ? C4 N1 C3 117.2(2) . . ? C4 N1 Zn1 120.50(16) . . ? C3 N1 Zn1 121.80(16) . . ? C6 N2 N3 106.3(2) . . ? C7 N3 N2 106.4(2) . . ? C10 N4 C11 116.7(2) . . ? C6 O1 C7 102.39(18) . . ? C16 O2 Zn1 124.64(15) . . ? Zn1 O4 H4A 122.5 . . ? Zn1 O4 H4B 101.3 . . ? H4A O4 H4B 117.0 . . ? C5 C1 C2 118.6(2) . . ? C5 C1 C6 122.5(2) . . ? C2 C1 C6 118.9(2) . . ? C3 C2 C1 118.6(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? N1 C3 C2 123.5(2) . . ? N1 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? N1 C4 C5 123.7(2) . . ? N1 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C1 118.4(2) . . ? C4 C5 H5 120.8 . . ? C1 C5 H5 120.8 . . ? N2 C6 O1 112.4(2) . . ? N2 C6 C1 128.2(2) . . ? O1 C6 C1 119.3(2) . . ? N3 C7 O1 112.5(2) . . ? N3 C7 C8 127.0(2) . . ? O1 C7 C8 120.5(2) . . ? C12 C8 C9 118.8(2) . . ? C12 C8 C7 122.9(2) . . ? C9 C8 C7 118.3(2) . . ? C10 C9 C8 118.4(3) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? N4 C10 C9 124.2(3) . . ? N4 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N4 C11 C12 124.0(3) . . ? N4 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C8 118.0(3) . . ? C11 C12 H12 121.0 . . ? C8 C12 H12 121.0 . . ? C14 C13 C15 118.7(2) . 2 ? C14 C13 C16 121.3(2) . . ? C15 C13 C16 120.0(2) 2 . ? C15 C14 C13 120.9(2) . . ? C15 C14 Br1 121.57(18) . . ? C13 C14 Br1 117.51(17) . . ? C14 C15 C13 120.4(2) . 2 ? C14 C15 Br2 121.40(17) . . ? C13 C15 Br2 118.16(17) 2 . ? O3 C16 O2 128.3(2) . . ? O3 C16 C13 116.5(2) . . ? O2 C16 C13 115.2(2) . . ? H5A O5 H5B 117.1 . . ? 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 O4 Zn1 N1 C4 42.82(19) 2_556 . . . ? O4 Zn1 N1 C4 -137.18(19) . . . . ? O2 Zn1 N1 C4 -45.77(19) . . . . ? O2 Zn1 N1 C4 134.23(19) 2_556 . . . ? O4 Zn1 N1 C3 -128.8(2) 2_556 . . . ? O4 Zn1 N1 C3 51.2(2) . . . . ? O2 Zn1 N1 C3 142.6(2) . . . . ? O2 Zn1 N1 C3 -37.4(2) 2_556 . . . ? C6 N2 N3 C7 0.6(3) . . . . ? O4 Zn1 O2 C16 -164.03(18) 2_556 . . . ? O4 Zn1 O2 C16 15.97(18) . . . . ? N1 Zn1 O2 C16 103.59(18) 2_556 . . . ? N1 Zn1 O2 C16 -76.41(18) . . . . ? C5 C1 C2 C3 1.1(4) . . . . ? C6 C1 C2 C3 -176.8(2) . . . . ? C4 N1 C3 C2 -0.8(4) . . . . ? Zn1 N1 C3 C2 171.1(2) . . . . ? C1 C2 C3 N1 -0.2(4) . . . . ? C3 N1 C4 C5 0.9(4) . . . . ? Zn1 N1 C4 C5 -171.1(2) . . . . ? N1 C4 C5 C1 -0.1(4) . . . . ? C2 C1 C5 C4 -1.0(4) . . . . ? C6 C1 C5 C4 176.9(2) . . . . ? N3 N2 C6 O1 -0.6(3) . . . . ? N3 N2 C6 C1 175.7(3) . . . . ? C7 O1 C6 N2 0.4(3) . . . . ? C7 O1 C6 C1 -176.3(2) . . . . ? C5 C1 C6 N2 177.3(3) . . . . ? C2 C1 C6 N2 -4.9(4) . . . . ? C5 C1 C6 O1 -6.6(4) . . . . ? C2 C1 C6 O1 171.2(2) . . . . ? N2 N3 C7 O1 -0.3(3) . . . . ? N2 N3 C7 C8 178.1(2) . . . . ? C6 O1 C7 N3 0.0(3) . . . . ? C6 O1 C7 C8 -178.6(2) . . . . ? N3 C7 C8 C12 -179.7(3) . . . . ? O1 C7 C8 C12 -1.4(4) . . . . ? N3 C7 C8 C9 -0.8(4) . . . . ? O1 C7 C8 C9 177.5(2) . . . . ? C12 C8 C9 C10 0.3(4) . . . . ? C7 C8 C9 C10 -178.7(3) . . . . ? C11 N4 C10 C9 0.1(4) . . . . ? C8 C9 C10 N4 -0.3(5) . . . . ? C10 N4 C11 C12 0.1(4) . . . . ? N4 C11 C12 C8 -0.1(4) . . . . ? C9 C8 C12 C11 -0.1(4) . . . . ? C7 C8 C12 C11 178.8(2) . . . . ? C15 C13 C14 C15 -0.1(4) 2 . . . ? C16 C13 C14 C15 -179.6(2) . . . . ? C15 C13 C14 Br1 177.90(17) 2 . . . ? C16 C13 C14 Br1 -1.6(3) . . . . ? C13 C14 C15 C13 0.1(4) . . . 2 ? Br1 C14 C15 C13 -177.82(17) . . . 2 ? C13 C14 C15 Br2 -179.53(18) . . . . ? Br1 C14 C15 Br2 2.5(3) . . . . ? Zn1 O2 C16 O3 10.2(4) . . . . ? Zn1 O2 C16 C13 -169.55(14) . . . . ? C14 C13 C16 O3 97.9(3) . . . . ? C15 C13 C16 O3 -81.6(3) 2 . . . ? C14 C13 C16 O2 -82.3(3) . . . . ? C15 C13 C16 O2 98.2(3) 2 . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.682 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.070 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 763368' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H19 Ag Br4 N8 O7' _chemical_formula_weight 1055.06 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' Ag Ag -0.8971 1.1015 '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 10.891(2) _cell_length_b 12.402(3) _cell_length_c 15.103(3) _cell_angle_alpha 78.950(4) _cell_angle_beta 71.012(4) _cell_angle_gamma 64.975(4) _cell_volume 1744.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2144 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 23.95 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 5.219 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.730658 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 9004 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6111 _reflns_number_gt 4284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6111 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ag1 Ag 0.44576(5) 0.82025(4) 0.67794(3) 0.02773(14) Uani 1 1 d . . . Br1 Br 0.70670(8) 0.21824(6) 0.97260(5) 0.0436(2) Uani 1 1 d . . . Br2 Br 0.67691(8) 0.40942(7) 0.78916(5) 0.0494(2) Uani 1 1 d . . . Br3 Br -0.00600(8) 1.11028(7) 0.68186(5) 0.0473(2) Uani 1 1 d . . . Br4 Br -0.29724(8) 1.19496(7) 0.61784(6) 0.0497(2) Uani 1 1 d . . . O1 O -0.0316(5) 1.3820(4) 0.9013(4) 0.0481(13) Uani 1 1 d . . . O2 O 0.8949(4) 0.3336(4) 0.3517(3) 0.0373(11) Uani 1 1 d . . . O3 O 0.3697(5) 0.6964(4) 0.8068(3) 0.0496(14) Uani 1 1 d . . . O4 O 0.5625(5) 0.7163(4) 0.8030(3) 0.0475(13) Uani 1 1 d . . . O5 O 0.2590(5) 0.8325(4) 0.6298(3) 0.0434(13) Uani 1 1 d . . . O6 O 0.3487(5) 0.9538(4) 0.5301(3) 0.0467(13) Uani 1 1 d . . . O7 O 0.6226(5) 0.8896(4) 0.6156(4) 0.0571(16) Uani 1 1 d . . . H7A H 0.7045 0.8565 0.6238 0.086 Uiso 1 1 d R . . H7B H 0.6117 0.9423 0.5705 0.086 Uiso 1 1 d R . . N1 N 0.3237(6) 1.0099(5) 0.7367(4) 0.0379(14) Uani 1 1 d . . . N2 N 0.0237(7) 1.4570(6) 0.7552(5) 0.061(2) Uani 1 1 d . . . N3 N -0.0752(7) 1.5505(5) 0.8122(5) 0.0598(19) Uani 1 1 d . . . N4 N -0.3628(8) 1.6753(9) 1.1469(7) 0.087(3) Uani 1 1 d . . . H4A H -0.4144 1.7106 1.1978 0.104 Uiso 1 1 calc R . . N5 N 0.5978(6) 0.6573(5) 0.5870(4) 0.0389(14) Uani 1 1 d . . . N6 N 1.0291(6) 0.3021(5) 0.4447(4) 0.0431(15) Uani 1 1 d . . . N7 N 1.1021(6) 0.2213(5) 0.3743(4) 0.0435(15) Uani 1 1 d . . . N8 N 1.1329(8) 0.0542(6) 0.0815(5) 0.0611(19) Uani 1 1 d . . . C1 C 0.1406(8) 1.1416(6) 0.8487(5) 0.0462(19) Uani 1 1 d . . . H1 H 0.0777 1.1513 0.9083 0.055 Uiso 1 1 calc R . . C2 C 0.2330(8) 1.0294(6) 0.8207(5) 0.0440(18) Uani 1 1 d . . . H2 H 0.2316 0.9643 0.8628 0.053 Uiso 1 1 calc R . . C3 C 0.3290(7) 1.1058(6) 0.6780(5) 0.0457(19) Uani 1 1 d . . . H3 H 0.3964 1.0934 0.6201 0.055 Uiso 1 1 calc R . . C4 C 0.2398(8) 1.2203(6) 0.6999(6) 0.049(2) Uani 1 1 d . . . H4 H 0.2445 1.2840 0.6568 0.059 Uiso 1 1 calc R . . C5 C 0.1420(7) 1.2400(6) 0.7875(5) 0.0390(17) Uani 1 1 d . . . C6 C 0.0450(8) 1.3615(6) 0.8105(6) 0.0446(19) Uani 1 1 d . . . C7 C -0.1032(8) 1.5025(6) 0.8965(6) 0.046(2) Uani 1 1 d . . . C8 C -0.1956(8) 1.5624(7) 0.9841(6) 0.052(2) Uani 1 1 d . . . C9 C -0.2088(9) 1.4979(8) 1.0678(7) 0.065(2) Uani 1 1 d . . . H9 H -0.1629 1.4153 1.0715 0.078 Uiso 1 1 calc R . . C10 C -0.2928(10) 1.5598(10) 1.1471(7) 0.076(3) Uani 1 1 d . . . H10 H -0.3001 1.5163 1.2046 0.091 Uiso 1 1 calc R . . C11 C -0.3502(10) 1.7341(10) 1.0655(9) 0.082(3) Uani 1 1 d . . . H11 H -0.3974 1.8165 1.0639 0.099 Uiso 1 1 calc R . . C12 C -0.2712(9) 1.6818(8) 0.9813(7) 0.071(3) Uani 1 1 d . . . H12 H -0.2698 1.7270 0.9245 0.085 Uiso 1 1 calc R . . C13 C 0.6681(7) 0.5299(6) 0.4631(5) 0.0445(19) Uani 1 1 d . . . H13 H 0.6463 0.5106 0.4151 0.053 Uiso 1 1 calc R . . C14 C 0.5724(7) 0.6240(6) 0.5183(5) 0.0450(19) Uani 1 1 d . . . H14 H 0.4849 0.6666 0.5066 0.054 Uiso 1 1 calc R . . C15 C 0.7228(7) 0.5964(6) 0.6026(5) 0.0392(17) Uani 1 1 d . . . H15 H 0.7430 0.6198 0.6494 0.047 Uiso 1 1 calc R . . C16 C 0.8246(7) 0.5003(6) 0.5533(5) 0.0384(17) Uani 1 1 d . . . H16 H 0.9103 0.4591 0.5676 0.046 Uiso 1 1 calc R . . C17 C 0.7977(7) 0.4654(6) 0.4819(5) 0.0345(16) Uani 1 1 d . . . C18 C 0.9078(7) 0.3666(6) 0.4278(5) 0.0353(16) Uani 1 1 d . . . C19 C 1.0219(7) 0.2421(6) 0.3214(5) 0.0350(16) Uani 1 1 d . . . C20 C 1.0567(7) 0.1807(6) 0.2393(5) 0.0388(17) Uani 1 1 d . . . C21 C 1.1920(8) 0.0952(7) 0.2070(6) 0.052(2) Uani 1 1 d . . . H21 H 1.2606 0.0783 0.2373 0.063 Uiso 1 1 calc R . . C22 C 1.2223(9) 0.0363(8) 0.1296(6) 0.063(2) Uani 1 1 d . . . H22 H 1.3130 -0.0207 0.1094 0.076 Uiso 1 1 calc R . . C23 C 1.0045(9) 0.1372(7) 0.1133(5) 0.054(2) Uani 1 1 d . . . H23 H 0.9389 0.1528 0.0806 0.064 Uiso 1 1 calc R . . C24 C 0.9611(7) 0.2015(6) 0.1904(5) 0.0440(19) Uani 1 1 d . . . H24 H 0.8694 0.2577 0.2090 0.053 Uiso 1 1 calc R . . C25 C 0.4710(7) 0.6720(6) 0.8375(5) 0.0344(16) Uani 1 1 d . . . C26 C 0.4872(6) 0.5826(5) 0.9219(4) 0.0288(15) Uani 1 1 d . . . C27 C 0.5758(7) 0.4613(5) 0.9117(4) 0.0319(15) Uani 1 1 d . . . C28 C 0.5872(6) 0.3807(5) 0.9878(4) 0.0299(15) Uani 1 1 d . . . C29 C 0.2540(7) 0.9127(6) 0.5657(5) 0.0319(15) Uani 1 1 d . . . C30 C 0.1241(6) 0.9618(6) 0.5296(4) 0.0304(15) Uani 1 1 d . . . C31 C -0.0035(7) 1.0454(6) 0.5778(4) 0.0318(15) Uani 1 1 d . . . C32 C -0.1249(7) 1.0825(6) 0.5488(5) 0.0324(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0272(3) 0.0250(3) 0.0261(3) 0.0007(2) -0.0088(2) -0.0056(2) Br1 0.0537(5) 0.0256(4) 0.0378(4) -0.0032(3) -0.0153(3) -0.0002(3) Br2 0.0641(5) 0.0391(4) 0.0271(4) -0.0058(3) -0.0057(4) -0.0068(4) Br3 0.0446(4) 0.0545(5) 0.0436(5) -0.0171(4) -0.0198(4) -0.0082(4) Br4 0.0377(4) 0.0519(5) 0.0489(5) -0.0171(4) -0.0172(4) 0.0023(4) O1 0.053(3) 0.028(3) 0.056(4) -0.008(2) -0.010(3) -0.011(2) O2 0.030(2) 0.028(3) 0.050(3) -0.011(2) -0.009(2) -0.005(2) O3 0.049(3) 0.055(3) 0.042(3) 0.013(3) -0.025(3) -0.015(3) O4 0.060(3) 0.043(3) 0.039(3) 0.011(2) -0.017(3) -0.024(3) O5 0.041(3) 0.046(3) 0.039(3) 0.013(3) -0.019(2) -0.015(2) O6 0.040(3) 0.063(3) 0.043(3) 0.011(3) -0.016(2) -0.027(3) O7 0.029(3) 0.057(3) 0.075(4) 0.025(3) -0.020(3) -0.015(3) N1 0.037(3) 0.032(3) 0.039(4) -0.003(3) -0.010(3) -0.009(3) N2 0.067(5) 0.033(4) 0.066(5) 0.002(4) -0.006(4) -0.014(4) N3 0.058(4) 0.031(4) 0.074(5) -0.004(4) -0.008(4) -0.009(3) N4 0.068(6) 0.099(8) 0.095(7) -0.064(6) -0.001(5) -0.026(6) N5 0.031(3) 0.039(4) 0.039(4) -0.005(3) -0.005(3) -0.009(3) N6 0.040(3) 0.042(4) 0.040(4) -0.011(3) -0.011(3) -0.006(3) N7 0.039(3) 0.037(4) 0.045(4) -0.013(3) -0.009(3) -0.004(3) N8 0.066(5) 0.058(5) 0.048(4) -0.019(4) -0.007(4) -0.014(4) C1 0.054(5) 0.035(4) 0.037(4) -0.001(4) -0.006(4) -0.010(4) C2 0.057(5) 0.031(4) 0.033(4) -0.003(3) -0.010(4) -0.008(4) C3 0.043(4) 0.035(4) 0.047(5) 0.002(4) 0.001(4) -0.016(4) C4 0.055(5) 0.035(4) 0.052(5) 0.003(4) -0.006(4) -0.022(4) C5 0.046(4) 0.034(4) 0.040(4) -0.001(3) -0.015(4) -0.016(3) C6 0.042(4) 0.032(4) 0.057(5) -0.008(4) -0.009(4) -0.012(4) C7 0.048(5) 0.021(4) 0.068(6) -0.009(4) -0.015(4) -0.010(3) C8 0.043(4) 0.041(5) 0.072(6) -0.013(4) -0.013(4) -0.015(4) C9 0.077(6) 0.052(6) 0.068(7) -0.011(5) -0.016(5) -0.026(5) C10 0.082(7) 0.089(8) 0.059(6) -0.024(6) -0.008(5) -0.036(6) C11 0.069(7) 0.062(7) 0.113(10) -0.039(7) -0.017(7) -0.014(6) C12 0.065(6) 0.041(5) 0.092(8) -0.024(5) -0.012(5) -0.004(5) C13 0.037(4) 0.044(5) 0.047(5) -0.012(4) -0.016(4) -0.004(4) C14 0.034(4) 0.041(4) 0.050(5) -0.008(4) -0.012(4) -0.002(3) C15 0.036(4) 0.041(4) 0.040(4) -0.012(3) -0.006(3) -0.015(4) C16 0.032(4) 0.038(4) 0.044(4) -0.005(3) -0.011(3) -0.011(3) C17 0.034(4) 0.029(4) 0.037(4) -0.001(3) -0.002(3) -0.015(3) C18 0.039(4) 0.023(4) 0.042(4) -0.004(3) -0.010(3) -0.011(3) C19 0.028(4) 0.029(4) 0.043(4) -0.002(3) -0.010(3) -0.006(3) C20 0.041(4) 0.029(4) 0.041(4) -0.002(3) -0.007(3) -0.013(3) C21 0.041(4) 0.049(5) 0.060(5) -0.026(4) -0.011(4) -0.004(4) C22 0.059(5) 0.054(6) 0.062(6) -0.029(5) -0.001(5) -0.009(5) C23 0.066(6) 0.062(6) 0.041(5) -0.001(4) -0.021(4) -0.029(5) C24 0.035(4) 0.043(5) 0.044(5) 0.001(4) -0.009(4) -0.009(3) C25 0.037(4) 0.028(4) 0.027(4) -0.002(3) -0.004(3) -0.006(3) C26 0.035(4) 0.029(4) 0.028(4) 0.001(3) -0.014(3) -0.013(3) C27 0.042(4) 0.025(4) 0.027(4) -0.003(3) -0.013(3) -0.008(3) C28 0.034(4) 0.025(3) 0.027(4) -0.004(3) -0.011(3) -0.005(3) C29 0.029(4) 0.029(4) 0.030(4) -0.011(3) -0.009(3) 0.002(3) C30 0.026(3) 0.033(4) 0.028(4) 0.005(3) -0.009(3) -0.008(3) C31 0.035(4) 0.030(4) 0.031(4) 0.000(3) -0.013(3) -0.011(3) C32 0.034(4) 0.032(4) 0.030(4) 0.003(3) -0.012(3) -0.011(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 Ag1 O7 2.290(4) . ? Ag1 O5 2.312(4) . ? Ag1 N5 2.337(6) . ? Ag1 N1 2.340(6) . ? Ag1 O3 2.391(5) . ? Ag1 O4 2.468(5) . ? Br1 C28 1.889(6) . ? Br2 C27 1.893(6) . ? Br3 C31 1.887(7) . ? Br4 C32 1.904(7) . ? O1 C6 1.360(9) . ? O1 C7 1.362(8) . ? O2 C18 1.357(8) . ? O2 C19 1.368(7) . ? O3 C25 1.233(8) . ? O4 C25 1.258(8) . ? O5 C29 1.245(7) . ? O6 C29 1.262(8) . ? O7 H7A 0.8500 . ? O7 H7B 0.8501 . ? N1 C2 1.320(8) . ? N1 C3 1.350(8) . ? N2 C6 1.292(9) . ? N2 N3 1.403(9) . ? N3 C7 1.296(9) . ? N4 C11 1.300(12) . ? N4 C10 1.307(12) . ? N4 H4A 0.8600 . ? N5 C15 1.323(8) . ? N5 C14 1.332(9) . ? N6 C18 1.302(8) . ? N6 N7 1.398(8) . ? N7 C19 1.285(8) . ? N8 C22 1.319(10) . ? N8 C23 1.334(10) . ? C1 C2 1.375(9) . ? C1 C5 1.385(9) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.369(10) . ? C3 H3 0.9300 . ? C4 C5 1.390(10) . ? C4 H4 0.9300 . ? C5 C6 1.457(10) . ? C7 C8 1.480(11) . ? C8 C12 1.356(11) . ? C8 C9 1.360(11) . ? C9 C10 1.380(12) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.383(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.387(10) . ? C13 C17 1.390(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.375(9) . ? C15 H15 0.9300 . ? C16 C17 1.388(9) . ? C16 H16 0.9300 . ? C17 C18 1.452(9) . ? C19 C20 1.439(10) . ? C20 C24 1.378(10) . ? C20 C21 1.394(9) . ? C21 C22 1.371(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.377(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.524(9) . ? C26 C28 1.391(8) 2_667 ? C26 C27 1.407(8) . ? C27 C28 1.372(8) . ? C28 C26 1.391(8) 2_667 ? C29 C30 1.521(8) . ? C30 C32 1.393(9) 2_576 ? C30 C31 1.396(8) . ? C31 C32 1.391(8) . ? C32 C30 1.393(9) 2_576 ? 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 O7 Ag1 O5 134.29(17) . . ? O7 Ag1 N5 85.0(2) . . ? O5 Ag1 N5 90.80(19) . . ? O7 Ag1 N1 82.02(19) . . ? O5 Ag1 N1 92.81(18) . . ? N5 Ag1 N1 164.87(19) . . ? O7 Ag1 O3 140.58(17) . . ? O5 Ag1 O3 84.98(16) . . ? N5 Ag1 O3 92.45(19) . . ? N1 Ag1 O3 102.50(19) . . ? O7 Ag1 O4 86.83(17) . . ? O5 Ag1 O4 138.60(16) . . ? N5 Ag1 O4 88.16(19) . . ? N1 Ag1 O4 98.72(18) . . ? O3 Ag1 O4 53.76(16) . . ? C6 O1 C7 101.9(6) . . ? C18 O2 C19 102.9(5) . . ? C25 O3 Ag1 93.2(4) . . ? C25 O4 Ag1 89.0(4) . . ? C29 O5 Ag1 101.9(4) . . ? Ag1 O7 H7A 125.8 . . ? Ag1 O7 H7B 115.7 . . ? H7A O7 H7B 116.7 . . ? C2 N1 C3 117.7(6) . . ? C2 N1 Ag1 122.7(5) . . ? C3 N1 Ag1 118.9(5) . . ? C6 N2 N3 105.6(7) . . ? C7 N3 N2 106.3(6) . . ? C11 N4 C10 116.5(9) . . ? C11 N4 H4A 121.8 . . ? C10 N4 H4A 121.8 . . ? C15 N5 C14 117.3(6) . . ? C15 N5 Ag1 116.8(5) . . ? C14 N5 Ag1 125.8(5) . . ? C18 N6 N7 105.1(6) . . ? C19 N7 N6 107.8(5) . . ? C22 N8 C23 114.9(7) . . ? C2 C1 C5 119.5(7) . . ? C2 C1 H1 120.3 . . ? C5 C1 H1 120.3 . . ? N1 C2 C1 123.0(7) . . ? N1 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? N1 C3 C4 123.0(7) . . ? N1 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 118.9(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C1 C5 C4 117.8(7) . . ? C1 C5 C6 123.0(7) . . ? C4 C5 C6 119.2(6) . . ? N2 C6 O1 113.4(7) . . ? N2 C6 C5 128.1(8) . . ? O1 C6 C5 118.4(6) . . ? N3 C7 O1 112.7(7) . . ? N3 C7 C8 128.3(7) . . ? O1 C7 C8 118.9(7) . . ? C12 C8 C9 119.3(9) . . ? C12 C8 C7 120.3(8) . . ? C9 C8 C7 120.4(7) . . ? C8 C9 C10 117.4(9) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? N4 C10 C9 124.6(10) . . ? N4 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? N4 C11 C12 124.2(10) . . ? N4 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C8 C12 C11 117.9(10) . . ? C8 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C14 C13 C17 117.7(7) . . ? C14 C13 H13 121.1 . . ? C17 C13 H13 121.1 . . ? N5 C14 C13 124.1(7) . . ? N5 C14 H14 118.0 . . ? C13 C14 H14 118.0 . . ? N5 C15 C16 123.5(7) . . ? N5 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 119.2(6) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C13 118.2(6) . . ? C16 C17 C18 118.8(6) . . ? C13 C17 C18 122.9(7) . . ? N6 C18 O2 112.7(6) . . ? N6 C18 C17 124.8(7) . . ? O2 C18 C17 122.5(6) . . ? N7 C19 O2 111.4(6) . . ? N7 C19 C20 126.2(6) . . ? O2 C19 C20 122.3(6) . . ? C24 C20 C21 117.3(7) . . ? C24 C20 C19 122.9(6) . . ? C21 C20 C19 119.8(7) . . ? C22 C21 C20 118.8(8) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N8 C22 C21 125.2(8) . . ? N8 C22 H22 117.4 . . ? C21 C22 H22 117.4 . . ? N8 C23 C24 125.3(8) . . ? N8 C23 H23 117.3 . . ? C24 C23 H23 117.3 . . ? C23 C24 C20 118.4(7) . . ? C23 C24 H24 120.8 . . ? C20 C24 H24 120.8 . . ? O3 C25 O4 123.8(6) . . ? O3 C25 C26 118.3(6) . . ? O4 C25 C26 117.9(6) . . ? C28 C26 C27 117.8(6) 2_667 . ? C28 C26 C25 120.3(6) 2_667 . ? C27 C26 C25 121.9(6) . . ? C28 C27 C26 121.6(6) . . ? C28 C27 Br2 119.9(5) . . ? C26 C27 Br2 118.4(5) . . ? C27 C28 C26 120.5(6) . 2_667 ? C27 C28 Br1 121.0(5) . . ? C26 C28 Br1 118.5(5) 2_667 . ? O5 C29 O6 124.1(6) . . ? O5 C29 C30 116.4(6) . . ? O6 C29 C30 119.5(6) . . ? C32 C30 C31 117.2(6) 2_576 . ? C32 C30 C29 121.0(6) 2_576 . ? C31 C30 C29 121.6(6) . . ? C32 C31 C30 121.3(6) . . ? C32 C31 Br3 120.7(5) . . ? C30 C31 Br3 118.0(5) . . ? C31 C32 C30 121.5(6) . 2_576 ? C31 C32 Br4 119.7(5) . . ? C30 C32 Br4 118.8(5) 2_576 . ? 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 O7 Ag1 O3 C25 -1.2(6) . . . . ? O5 Ag1 O3 C25 174.4(4) . . . . ? N5 Ag1 O3 C25 83.8(4) . . . . ? N1 Ag1 O3 C25 -93.8(4) . . . . ? O4 Ag1 O3 C25 -2.1(4) . . . . ? O7 Ag1 O4 C25 -177.4(4) . . . . ? O5 Ag1 O4 C25 -3.2(5) . . . . ? N5 Ag1 O4 C25 -92.3(4) . . . . ? N1 Ag1 O4 C25 101.2(4) . . . . ? O3 Ag1 O4 C25 2.1(4) . . . . ? O7 Ag1 O5 C29 -14.4(5) . . . . ? N5 Ag1 O5 C29 -98.1(4) . . . . ? N1 Ag1 O5 C29 67.2(4) . . . . ? O3 Ag1 O5 C29 169.5(4) . . . . ? O4 Ag1 O5 C29 173.8(4) . . . . ? O7 Ag1 N1 C2 -143.0(6) . . . . ? O5 Ag1 N1 C2 82.6(5) . . . . ? N5 Ag1 N1 C2 -173.8(7) . . . . ? O3 Ag1 N1 C2 -2.9(6) . . . . ? O4 Ag1 N1 C2 -57.5(6) . . . . ? O7 Ag1 N1 C3 47.3(5) . . . . ? O5 Ag1 N1 C3 -87.0(5) . . . . ? N5 Ag1 N1 C3 16.6(10) . . . . ? O3 Ag1 N1 C3 -172.5(5) . . . . ? O4 Ag1 N1 C3 132.9(5) . . . . ? C6 N2 N3 C7 0.5(9) . . . . ? O7 Ag1 N5 C15 58.3(5) . . . . ? O5 Ag1 N5 C15 -167.3(5) . . . . ? N1 Ag1 N5 C15 88.9(9) . . . . ? O3 Ag1 N5 C15 -82.3(5) . . . . ? O4 Ag1 N5 C15 -28.7(5) . . . . ? O7 Ag1 N5 C14 -118.3(6) . . . . ? O5 Ag1 N5 C14 16.1(6) . . . . ? N1 Ag1 N5 C14 -87.8(9) . . . . ? O3 Ag1 N5 C14 101.1(6) . . . . ? O4 Ag1 N5 C14 154.7(6) . . . . ? C18 N6 N7 C19 -0.1(7) . . . . ? C3 N1 C2 C1 3.1(11) . . . . ? Ag1 N1 C2 C1 -166.6(6) . . . . ? C5 C1 C2 N1 -0.7(12) . . . . ? C2 N1 C3 C4 -3.9(11) . . . . ? Ag1 N1 C3 C4 166.3(6) . . . . ? N1 C3 C4 C5 2.2(12) . . . . ? C2 C1 C5 C4 -1.0(11) . . . . ? C2 C1 C5 C6 178.1(7) . . . . ? C3 C4 C5 C1 0.3(11) . . . . ? C3 C4 C5 C6 -178.8(7) . . . . ? N3 N2 C6 O1 0.0(9) . . . . ? N3 N2 C6 C5 -177.7(7) . . . . ? C7 O1 C6 N2 -0.4(8) . . . . ? C7 O1 C6 C5 177.5(6) . . . . ? C1 C5 C6 N2 -169.5(8) . . . . ? C4 C5 C6 N2 9.6(12) . . . . ? C1 C5 C6 O1 12.9(11) . . . . ? C4 C5 C6 O1 -168.0(7) . . . . ? N2 N3 C7 O1 -0.8(9) . . . . ? N2 N3 C7 C8 176.7(7) . . . . ? C6 O1 C7 N3 0.7(8) . . . . ? C6 O1 C7 C8 -177.0(7) . . . . ? N3 C7 C8 C12 4.5(13) . . . . ? O1 C7 C8 C12 -178.2(7) . . . . ? N3 C7 C8 C9 -177.4(8) . . . . ? O1 C7 C8 C9 -0.1(11) . . . . ? C12 C8 C9 C10 -4.0(13) . . . . ? C7 C8 C9 C10 177.8(8) . . . . ? C11 N4 C10 C9 -0.3(15) . . . . ? C8 C9 C10 N4 1.7(15) . . . . ? C10 N4 C11 C12 1.4(16) . . . . ? C9 C8 C12 C11 5.1(13) . . . . ? C7 C8 C12 C11 -176.8(8) . . . . ? N4 C11 C12 C8 -3.9(16) . . . . ? C15 N5 C14 C13 0.3(11) . . . . ? Ag1 N5 C14 C13 176.9(5) . . . . ? C17 C13 C14 N5 1.0(11) . . . . ? C14 N5 C15 C16 -1.5(10) . . . . ? Ag1 N5 C15 C16 -178.4(5) . . . . ? N5 C15 C16 C17 1.3(10) . . . . ? C15 C16 C17 C13 0.1(10) . . . . ? C15 C16 C17 C18 177.7(6) . . . . ? C14 C13 C17 C16 -1.2(10) . . . . ? C14 C13 C17 C18 -178.6(6) . . . . ? N7 N6 C18 O2 0.5(7) . . . . ? N7 N6 C18 C17 -178.1(6) . . . . ? C19 O2 C18 N6 -0.8(7) . . . . ? C19 O2 C18 C17 177.9(6) . . . . ? C16 C17 C18 N6 4.4(10) . . . . ? C13 C17 C18 N6 -178.1(7) . . . . ? C16 C17 C18 O2 -174.1(6) . . . . ? C13 C17 C18 O2 3.4(10) . . . . ? N6 N7 C19 O2 -0.4(8) . . . . ? N6 N7 C19 C20 178.8(6) . . . . ? C18 O2 C19 N7 0.7(7) . . . . ? C18 O2 C19 C20 -178.6(6) . . . . ? N7 C19 C20 C24 174.6(7) . . . . ? O2 C19 C20 C24 -6.2(10) . . . . ? N7 C19 C20 C21 -4.8(11) . . . . ? O2 C19 C20 C21 174.4(6) . . . . ? C24 C20 C21 C22 -0.5(11) . . . . ? C19 C20 C21 C22 178.9(7) . . . . ? C23 N8 C22 C21 0.2(13) . . . . ? C20 C21 C22 N8 0.4(14) . . . . ? C22 N8 C23 C24 -0.7(12) . . . . ? N8 C23 C24 C20 0.6(12) . . . . ? C21 C20 C24 C23 0.0(10) . . . . ? C19 C20 C24 C23 -179.3(7) . . . . ? Ag1 O3 C25 O4 4.0(7) . . . . ? Ag1 O3 C25 C26 -175.6(5) . . . . ? Ag1 O4 C25 O3 -3.9(7) . . . . ? Ag1 O4 C25 C26 175.7(5) . . . . ? O3 C25 C26 C28 -82.8(8) . . . 2_667 ? O4 C25 C26 C28 97.5(8) . . . 2_667 ? O3 C25 C26 C27 96.8(8) . . . . ? O4 C25 C26 C27 -82.8(8) . . . . ? C28 C26 C27 C28 1.3(11) 2_667 . . . ? C25 C26 C27 C28 -178.4(6) . . . . ? C28 C26 C27 Br2 179.6(5) 2_667 . . . ? C25 C26 C27 Br2 -0.1(8) . . . . ? C26 C27 C28 C26 -1.3(11) . . . 2_667 ? Br2 C27 C28 C26 -179.6(5) . . . 2_667 ? C26 C27 C28 Br1 179.9(5) . . . . ? Br2 C27 C28 Br1 1.7(8) . . . . ? Ag1 O5 C29 O6 11.5(8) . . . . ? Ag1 O5 C29 C30 -168.5(5) . . . . ? O5 C29 C30 C32 -95.0(7) . . . 2_576 ? O6 C29 C30 C32 85.0(8) . . . 2_576 ? O5 C29 C30 C31 79.6(8) . . . . ? O6 C29 C30 C31 -100.4(8) . . . . ? C32 C30 C31 C32 0.2(10) 2_576 . . . ? C29 C30 C31 C32 -174.5(6) . . . . ? C32 C30 C31 Br3 -178.1(5) 2_576 . . . ? C29 C30 C31 Br3 7.1(8) . . . . ? C30 C31 C32 C30 -0.2(11) . . . 2_576 ? Br3 C31 C32 C30 178.1(5) . . . 2_576 ? C30 C31 C32 Br4 179.1(5) . . . . ? Br3 C31 C32 Br4 -2.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.659 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.144 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 763369' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H18 Br4 Cd N8 O7' _chemical_formula_weight 1058.58 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8691(8) _cell_length_b 12.3897(9) _cell_length_c 15.1065(10) _cell_angle_alpha 78.9610(10) _cell_angle_beta 71.0450(10) _cell_angle_gamma 64.9900(10) _cell_volume 1740.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3289 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.66 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 2.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 5.281 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.767397 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 8819 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6086 _reflns_number_gt 4705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0145P)^2^+2.7975P] 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 6086 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.44560(3) 0.82029(3) 0.67795(2) 0.02871(9) Uani 1 1 d . . . Br1 Br 0.70680(5) 0.21820(4) 0.97258(3) 0.04169(13) Uani 1 1 d . . . Br2 Br 0.67691(5) 0.40953(4) 0.78917(3) 0.04709(14) Uani 1 1 d . . . Br3 Br -0.00575(5) 1.11030(4) 0.68178(3) 0.04553(13) Uani 1 1 d . . . Br4 Br -0.29712(5) 1.19497(4) 0.61785(3) 0.04794(14) Uani 1 1 d . . . O1 O -0.0315(3) 1.3826(3) 0.9010(2) 0.0447(8) Uani 1 1 d . . . O2 O 0.8953(3) 0.3334(2) 0.3521(2) 0.0341(7) Uani 1 1 d . . . O3 O 0.3699(3) 0.6962(3) 0.8068(2) 0.0499(9) Uani 1 1 d . . . O4 O 0.5628(3) 0.7164(3) 0.8028(2) 0.0462(8) Uani 1 1 d . . . O5 O 0.2578(3) 0.8330(3) 0.6302(2) 0.0390(7) Uani 1 1 d . . . O6 O 0.3477(3) 0.9541(3) 0.5303(2) 0.0442(8) Uani 1 1 d . . . O7 O 0.6221(3) 0.8898(3) 0.6149(2) 0.0555(10) Uani 1 1 d . . . H7A H 0.7045 0.8565 0.6238 0.083 Uiso 1 1 d R . . H7B H 0.6117 0.9423 0.5705 0.083 Uiso 1 1 d R . . N1 N 0.3241(4) 1.0099(3) 0.7364(3) 0.0362(9) Uani 1 1 d . . . N2 N 0.0226(4) 1.4567(3) 0.7561(3) 0.0560(12) Uani 1 1 d . . . N3 N -0.0760(5) 1.5510(4) 0.8126(3) 0.0605(12) Uani 1 1 d . . . N4 N -0.3626(5) 1.6762(5) 1.1476(4) 0.0812(17) Uani 1 1 d . . . N5 N 0.5984(4) 0.6576(3) 0.5867(2) 0.0369(9) Uani 1 1 d . . . N6 N 1.0287(4) 0.3021(3) 0.4452(3) 0.0417(10) Uani 1 1 d . . . N7 N 1.1029(4) 0.2213(3) 0.3749(3) 0.0409(9) Uani 1 1 d . . . N8 N 1.1325(5) 0.0548(4) 0.0825(3) 0.0566(12) Uani 1 1 d . . . C1 C 0.1400(5) 1.1425(4) 0.8484(3) 0.0438(12) Uani 1 1 d . . . H1 H 0.0774 1.1529 0.9081 0.053 Uiso 1 1 calc R . . C2 C 0.2312(5) 1.0302(4) 0.8206(3) 0.0431(12) Uani 1 1 d . . . H2 H 0.2281 0.9652 0.8626 0.052 Uiso 1 1 calc R . . C3 C 0.3287(5) 1.1045(4) 0.6783(3) 0.0436(12) Uani 1 1 d . . . H3 H 0.3950 1.0919 0.6200 0.052 Uiso 1 1 calc R . . C4 C 0.2400(5) 1.2201(4) 0.7003(4) 0.0475(13) Uani 1 1 d . . . H4 H 0.2459 1.2838 0.6576 0.057 Uiso 1 1 calc R . . C5 C 0.1423(5) 1.2394(4) 0.7869(3) 0.0394(11) Uani 1 1 d . . . C6 C 0.0464(5) 1.3605(4) 0.8107(3) 0.0421(12) Uani 1 1 d . . . C7 C -0.1038(5) 1.5034(4) 0.8963(4) 0.0450(12) Uani 1 1 d . . . C8 C -0.1957(5) 1.5611(4) 0.9834(4) 0.0479(13) Uani 1 1 d . . . C9 C -0.2066(6) 1.4980(5) 1.0677(4) 0.0613(15) Uani 1 1 d . . . H9 H -0.1576 1.4157 1.0718 0.074 Uiso 1 1 calc R . . C10 C -0.2924(7) 1.5594(6) 1.1474(4) 0.0780(19) Uani 1 1 d . . . H10 H -0.3013 1.5153 1.2046 0.094 Uiso 1 1 calc R . . C11 C -0.3496(7) 1.7341(6) 1.0650(6) 0.084(2) Uani 1 1 d . . . H11 H -0.3977 1.8166 1.0629 0.101 Uiso 1 1 calc R . . C12 C -0.2705(6) 1.6825(5) 0.9814(4) 0.0678(17) Uani 1 1 d . . . H12 H -0.2675 1.7284 0.9249 0.081 Uiso 1 1 calc R . . C13 C 0.6672(4) 0.5298(4) 0.4638(3) 0.0415(11) Uani 1 1 d . . . H13 H 0.6449 0.5099 0.4164 0.050 Uiso 1 1 calc R . . C14 C 0.5718(5) 0.6239(4) 0.5186(3) 0.0429(12) Uani 1 1 d . . . H14 H 0.4840 0.6662 0.5073 0.052 Uiso 1 1 calc R . . C15 C 0.7237(4) 0.5953(4) 0.6028(3) 0.0356(10) Uani 1 1 d . . . H15 H 0.7440 0.6181 0.6499 0.043 Uiso 1 1 calc R . . C16 C 0.8250(4) 0.4990(4) 0.5533(3) 0.0359(11) Uani 1 1 d . . . H16 H 0.9108 0.4569 0.5676 0.043 Uiso 1 1 calc R . . C17 C 0.7972(4) 0.4661(3) 0.4820(3) 0.0325(10) Uani 1 1 d . . . C18 C 0.9078(4) 0.3661(4) 0.4286(3) 0.0325(10) Uani 1 1 d . . . C19 C 1.0220(4) 0.2423(4) 0.3223(3) 0.0347(10) Uani 1 1 d . . . C20 C 1.0564(4) 0.1810(4) 0.2390(3) 0.0345(10) Uani 1 1 d . . . C21 C 1.1927(5) 0.0958(4) 0.2076(4) 0.0497(13) Uani 1 1 d . . . H21 H 1.2607 0.0795 0.2384 0.060 Uiso 1 1 calc R . . C22 C 1.2236(6) 0.0366(5) 0.1301(4) 0.0593(15) Uani 1 1 d . . . H22 H 1.3146 -0.0202 0.1096 0.071 Uiso 1 1 calc R . . C23 C 1.0041(6) 0.1378(5) 0.1129(3) 0.0515(13) Uani 1 1 d . . . H23 H 0.9390 0.1539 0.0797 0.062 Uiso 1 1 calc R . . C24 C 0.9609(5) 0.2017(4) 0.1905(3) 0.0409(11) Uani 1 1 d . . . H24 H 0.8689 0.2576 0.2094 0.049 Uiso 1 1 calc R . . C25 C 0.4731(5) 0.6722(4) 0.8370(3) 0.0344(11) Uani 1 1 d . . . C26 C 0.4878(4) 0.5824(3) 0.9212(3) 0.0275(9) Uani 1 1 d . . . C27 C 0.5753(4) 0.4621(3) 0.9111(3) 0.0284(9) Uani 1 1 d . . . C28 C 0.5876(4) 0.3817(3) 0.9884(3) 0.0273(9) Uani 1 1 d . . . C29 C 0.2546(4) 0.9127(4) 0.5655(3) 0.0295(10) Uani 1 1 d . . . C30 C 0.1233(4) 0.9609(3) 0.5296(3) 0.0275(9) Uani 1 1 d . . . C31 C -0.0033(4) 1.0458(4) 0.5781(3) 0.0305(10) Uani 1 1 d . . . C32 C -0.1248(4) 1.0834(3) 0.5486(3) 0.0310(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 Cd1 0.02621(16) 0.02668(16) 0.02643(17) -0.00146(13) -0.00625(13) -0.00475(13) Br1 0.0503(3) 0.0249(2) 0.0350(3) -0.00473(19) -0.0121(2) 0.0007(2) Br2 0.0597(3) 0.0382(3) 0.0242(2) -0.0075(2) -0.0022(2) -0.0057(2) Br3 0.0412(3) 0.0538(3) 0.0408(3) -0.0182(2) -0.0167(2) -0.0074(2) Br4 0.0346(3) 0.0514(3) 0.0463(3) -0.0186(2) -0.0142(2) 0.0029(2) O1 0.0472(19) 0.0306(17) 0.049(2) -0.0084(15) -0.0083(17) -0.0099(15) O2 0.0234(15) 0.0297(16) 0.0422(18) -0.0126(14) -0.0059(13) -0.0017(13) O3 0.049(2) 0.058(2) 0.0377(19) 0.0163(16) -0.0216(17) -0.0177(17) O4 0.056(2) 0.0442(19) 0.039(2) 0.0090(16) -0.0128(17) -0.0244(17) O5 0.0383(18) 0.0421(18) 0.0359(18) 0.0119(15) -0.0182(15) -0.0150(15) O6 0.0341(18) 0.059(2) 0.042(2) 0.0093(16) -0.0150(15) -0.0216(17) O7 0.0309(18) 0.057(2) 0.070(2) 0.0244(19) -0.0201(17) -0.0163(16) N1 0.038(2) 0.034(2) 0.034(2) -0.0024(18) -0.0072(18) -0.0140(17) N2 0.057(3) 0.034(2) 0.057(3) -0.004(2) -0.001(2) -0.010(2) N3 0.057(3) 0.034(2) 0.073(3) -0.005(2) -0.005(3) -0.010(2) N4 0.063(3) 0.085(4) 0.098(5) -0.051(4) -0.002(3) -0.027(3) N5 0.034(2) 0.037(2) 0.030(2) -0.0067(17) -0.0041(17) -0.0064(17) N6 0.035(2) 0.039(2) 0.044(2) -0.0148(19) -0.0086(19) -0.0050(18) N7 0.031(2) 0.037(2) 0.045(2) -0.0130(18) -0.0090(19) -0.0009(17) N8 0.062(3) 0.055(3) 0.049(3) -0.020(2) -0.006(2) -0.019(2) C1 0.053(3) 0.034(3) 0.033(3) -0.006(2) -0.003(2) -0.010(2) C2 0.053(3) 0.035(3) 0.033(3) 0.003(2) -0.010(2) -0.013(2) C3 0.044(3) 0.041(3) 0.039(3) -0.004(2) 0.001(2) -0.019(2) C4 0.052(3) 0.031(3) 0.056(3) 0.001(2) -0.008(3) -0.018(2) C5 0.043(3) 0.036(3) 0.041(3) -0.006(2) -0.011(2) -0.016(2) C6 0.045(3) 0.033(3) 0.047(3) -0.004(2) -0.008(2) -0.017(2) C7 0.039(3) 0.027(3) 0.067(4) -0.010(2) -0.010(3) -0.010(2) C8 0.040(3) 0.037(3) 0.066(4) -0.015(3) -0.008(3) -0.015(2) C9 0.059(4) 0.052(3) 0.068(4) -0.017(3) -0.010(3) -0.016(3) C10 0.079(4) 0.092(5) 0.067(4) -0.029(4) -0.003(4) -0.040(4) C11 0.068(4) 0.057(4) 0.117(6) -0.037(4) -0.014(5) -0.010(3) C12 0.064(4) 0.043(3) 0.082(4) -0.017(3) -0.012(3) -0.009(3) C13 0.036(3) 0.042(3) 0.045(3) -0.012(2) -0.013(2) -0.008(2) C14 0.028(2) 0.044(3) 0.047(3) -0.008(2) -0.011(2) -0.002(2) C15 0.032(2) 0.036(2) 0.034(3) -0.007(2) -0.003(2) -0.011(2) C16 0.026(2) 0.041(3) 0.034(3) -0.007(2) -0.003(2) -0.008(2) C17 0.032(2) 0.025(2) 0.033(3) -0.0022(19) 0.000(2) -0.0102(19) C18 0.032(2) 0.028(2) 0.037(3) -0.003(2) -0.008(2) -0.011(2) C19 0.028(2) 0.028(2) 0.039(3) -0.006(2) -0.004(2) -0.0053(19) C20 0.036(2) 0.028(2) 0.035(3) -0.006(2) -0.005(2) -0.009(2) C21 0.038(3) 0.043(3) 0.059(3) -0.021(3) -0.011(2) -0.002(2) C22 0.046(3) 0.054(3) 0.065(4) -0.027(3) -0.005(3) -0.006(3) C23 0.059(3) 0.060(3) 0.039(3) -0.001(3) -0.016(3) -0.025(3) C24 0.037(3) 0.041(3) 0.035(3) -0.001(2) -0.003(2) -0.011(2) C25 0.040(3) 0.024(2) 0.027(3) -0.0043(19) -0.007(2) -0.002(2) C26 0.030(2) 0.028(2) 0.022(2) -0.0005(18) -0.0095(18) -0.0077(18) C27 0.031(2) 0.029(2) 0.021(2) -0.0047(18) -0.0060(18) -0.0075(18) C28 0.029(2) 0.023(2) 0.027(2) -0.0027(18) -0.0104(19) -0.0045(18) C29 0.025(2) 0.034(2) 0.025(2) -0.008(2) -0.0059(19) -0.0056(19) C30 0.027(2) 0.027(2) 0.023(2) 0.0033(18) -0.0085(18) -0.0065(18) C31 0.032(2) 0.034(2) 0.026(2) -0.0028(19) -0.0114(19) -0.0109(19) C32 0.027(2) 0.030(2) 0.030(2) -0.0010(19) -0.0065(19) -0.0057(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 Cd1 O7 2.286(3) . ? Cd1 O5 2.314(3) . ? Cd1 N1 2.335(3) . ? Cd1 N5 2.339(3) . ? Cd1 O3 2.390(3) . ? Cd1 O4 2.467(3) . ? Cd1 C25 2.746(4) . ? Br1 C28 1.899(4) . ? Br2 C27 1.888(4) . ? Br3 C31 1.878(4) . ? Br4 C32 1.899(4) . ? O1 C6 1.359(5) . ? O1 C7 1.365(5) . ? O2 C18 1.359(5) . ? O2 C19 1.361(4) . ? O3 C25 1.247(5) . ? O4 C25 1.238(5) . ? O5 C29 1.248(5) . ? O6 C29 1.246(5) . ? O7 H7A 0.8569 . ? O7 H7B 0.8406 . ? N1 C3 1.332(5) . ? N1 C2 1.332(5) . ? N2 C6 1.293(6) . ? N2 N3 1.403(5) . ? N3 C7 1.286(6) . ? N4 C11 1.313(8) . ? N4 C10 1.321(8) . ? N5 C15 1.328(5) . ? N5 C14 1.332(5) . ? N6 C18 1.294(5) . ? N6 N7 1.397(5) . ? N7 C19 1.286(5) . ? N8 C22 1.327(6) . ? N8 C23 1.330(6) . ? C1 C2 1.372(6) . ? C1 C5 1.374(6) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.378(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(6) . ? C4 H4 0.9300 . ? C5 C6 1.452(6) . ? C7 C8 1.465(7) . ? C8 C9 1.359(7) . ? C8 C12 1.374(7) . ? C9 C10 1.384(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.371(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.382(6) . ? C13 C17 1.386(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 C17 1.380(6) . ? C16 H16 0.9300 . ? C17 C18 1.457(5) . ? C19 C20 1.456(6) . ? C20 C24 1.370(6) . ? C20 C21 1.395(6) . ? C21 C22 1.373(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.380(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.524(6) . ? C26 C28 1.389(5) 2_667 ? C26 C27 1.395(5) . ? C27 C28 1.385(5) . ? C28 C26 1.389(5) 2_667 ? C29 C30 1.531(5) . ? C30 C32 1.387(5) 2_576 ? C30 C31 1.398(5) . ? C31 C32 1.394(5) . ? C32 C30 1.387(5) 2_576 ? 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 O7 Cd1 O5 134.03(11) . . ? O7 Cd1 N1 81.95(12) . . ? O5 Cd1 N1 92.76(11) . . ? O7 Cd1 N5 84.63(13) . . ? O5 Cd1 N5 91.06(12) . . ? N1 Cd1 N5 164.54(13) . . ? O7 Cd1 O3 140.81(11) . . ? O5 Cd1 O3 85.01(11) . . ? N1 Cd1 O3 102.62(12) . . ? N5 Cd1 O3 92.62(12) . . ? O7 Cd1 O4 87.09(11) . . ? O5 Cd1 O4 138.62(11) . . ? N1 Cd1 O4 98.69(11) . . ? N5 Cd1 O4 88.22(11) . . ? O3 Cd1 O4 53.72(11) . . ? O7 Cd1 C25 113.84(13) . . ? O5 Cd1 C25 111.86(13) . . ? N1 Cd1 C25 102.93(12) . . ? N5 Cd1 C25 89.49(12) . . ? O3 Cd1 C25 26.97(12) . . ? O4 Cd1 C25 26.78(11) . . ? C6 O1 C7 102.8(4) . . ? C18 O2 C19 102.7(3) . . ? C25 O3 Cd1 92.6(3) . . ? C25 O4 Cd1 89.3(3) . . ? C29 O5 Cd1 101.3(3) . . ? Cd1 O7 H7A 125.2 . . ? Cd1 O7 H7B 116.4 . . ? H7A O7 H7B 116.8 . . ? C3 N1 C2 117.4(4) . . ? C3 N1 Cd1 118.9(3) . . ? C2 N1 Cd1 122.8(3) . . ? C6 N2 N3 106.8(4) . . ? C7 N3 N2 105.9(4) . . ? C11 N4 C10 115.5(6) . . ? C15 N5 C14 117.4(4) . . ? C15 N5 Cd1 117.0(3) . . ? C14 N5 Cd1 125.6(3) . . ? C18 N6 N7 105.6(3) . . ? C19 N7 N6 107.1(3) . . ? C22 N8 C23 116.1(4) . . ? C2 C1 C5 119.2(4) . . ? C2 C1 H1 120.4 . . ? C5 C1 H1 120.4 . . ? N1 C2 C1 123.1(4) . . ? N1 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? N1 C3 C4 123.2(4) . . ? N1 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C1 C5 C4 118.5(4) . . ? C1 C5 C6 122.1(4) . . ? C4 C5 C6 119.4(4) . . ? N2 C6 O1 111.9(4) . . ? N2 C6 C5 128.4(5) . . ? O1 C6 C5 119.7(4) . . ? N3 C7 O1 112.6(4) . . ? N3 C7 C8 129.1(4) . . ? O1 C7 C8 118.3(5) . . ? C9 C8 C12 118.4(5) . . ? C9 C8 C7 121.6(5) . . ? C12 C8 C7 119.9(5) . . ? C8 C9 C10 118.3(6) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N4 C10 C9 124.5(7) . . ? N4 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? N4 C11 C12 125.1(6) . . ? N4 C11 H11 117.5 . . ? C12 C11 H11 117.5 . . ? C11 C12 C8 118.2(6) . . ? C11 C12 H12 120.9 . . ? C8 C12 H12 120.9 . . ? C14 C13 C17 117.8(4) . . ? C14 C13 H13 121.1 . . ? C17 C13 H13 121.1 . . ? N5 C14 C13 123.8(4) . . ? N5 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? N5 C15 C16 123.3(4) . . ? N5 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 118.8(4) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C13 118.9(4) . . ? C16 C17 C18 117.8(4) . . ? C13 C17 C18 123.3(4) . . ? N6 C18 O2 112.6(4) . . ? N6 C18 C17 125.1(4) . . ? O2 C18 C17 122.2(4) . . ? N7 C19 O2 111.9(4) . . ? N7 C19 C20 126.5(4) . . ? O2 C19 C20 121.6(4) . . ? C24 C20 C21 118.2(4) . . ? C24 C20 C19 123.2(4) . . ? C21 C20 C19 118.5(4) . . ? C22 C21 C20 118.2(5) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? N8 C22 C21 124.5(5) . . ? N8 C22 H22 117.8 . . ? C21 C22 H22 117.8 . . ? N8 C23 C24 124.4(5) . . ? N8 C23 H23 117.8 . . ? C24 C23 H23 117.8 . . ? C20 C24 C23 118.6(4) . . ? C20 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? O4 C25 O3 124.2(4) . . ? O4 C25 C26 118.9(4) . . ? O3 C25 C26 116.9(4) . . ? O4 C25 Cd1 63.9(2) . . ? O3 C25 Cd1 60.4(2) . . ? C26 C25 Cd1 175.3(3) . . ? C28 C26 C27 117.5(4) 2_667 . ? C28 C26 C25 120.6(3) 2_667 . ? C27 C26 C25 121.9(3) . . ? C28 C27 C26 121.1(3) . . ? C28 C27 Br2 120.1(3) . . ? C26 C27 Br2 118.8(3) . . ? C27 C28 C26 121.3(3) . 2_667 ? C27 C28 Br1 120.3(3) . . ? C26 C28 Br1 118.4(3) 2_667 . ? O6 C29 O5 125.1(4) . . ? O6 C29 C30 119.9(4) . . ? O5 C29 C30 115.1(4) . . ? C32 C30 C31 118.4(4) 2_576 . ? C32 C30 C29 120.9(3) 2_576 . ? C31 C30 C29 120.6(3) . . ? C32 C31 C30 120.3(4) . . ? C32 C31 Br3 120.7(3) . . ? C30 C31 Br3 118.9(3) . . ? C30 C32 C31 121.3(4) 2_576 . ? C30 C32 Br4 119.1(3) 2_576 . ? C31 C32 Br4 119.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cd1 O3 C25 -1.0(4) . . . . ? O5 Cd1 O3 C25 174.5(3) . . . . ? N1 Cd1 O3 C25 -93.7(3) . . . . ? N5 Cd1 O3 C25 83.7(3) . . . . ? O4 Cd1 O3 C25 -2.2(2) . . . . ? O7 Cd1 O4 C25 -177.1(3) . . . . ? O5 Cd1 O4 C25 -2.8(3) . . . . ? N1 Cd1 O4 C25 101.5(3) . . . . ? N5 Cd1 O4 C25 -92.4(3) . . . . ? O3 Cd1 O4 C25 2.2(2) . . . . ? O7 Cd1 O5 C29 -13.7(3) . . . . ? N1 Cd1 O5 C29 67.7(3) . . . . ? N5 Cd1 O5 C29 -97.3(3) . . . . ? O3 Cd1 O5 C29 170.2(3) . . . . ? O4 Cd1 O5 C29 174.2(2) . . . . ? C25 Cd1 O5 C29 172.8(2) . . . . ? O7 Cd1 N1 C3 47.5(3) . . . . ? O5 Cd1 N1 C3 -86.6(3) . . . . ? N5 Cd1 N1 C3 17.5(7) . . . . ? O3 Cd1 N1 C3 -172.1(3) . . . . ? O4 Cd1 N1 C3 133.3(3) . . . . ? C25 Cd1 N1 C3 160.2(3) . . . . ? O7 Cd1 N1 C2 -144.2(4) . . . . ? O5 Cd1 N1 C2 81.7(3) . . . . ? N5 Cd1 N1 C2 -174.2(4) . . . . ? O3 Cd1 N1 C2 -3.8(4) . . . . ? O4 Cd1 N1 C2 -58.4(4) . . . . ? C25 Cd1 N1 C2 -31.5(4) . . . . ? C6 N2 N3 C7 -0.3(6) . . . . ? O7 Cd1 N5 C15 59.4(3) . . . . ? O5 Cd1 N5 C15 -166.4(3) . . . . ? N1 Cd1 N5 C15 89.2(5) . . . . ? O3 Cd1 N5 C15 -81.4(3) . . . . ? O4 Cd1 N5 C15 -27.8(3) . . . . ? C25 Cd1 N5 C15 -54.6(3) . . . . ? O7 Cd1 N5 C14 -118.8(4) . . . . ? O5 Cd1 N5 C14 15.3(4) . . . . ? N1 Cd1 N5 C14 -89.0(6) . . . . ? O3 Cd1 N5 C14 100.4(4) . . . . ? O4 Cd1 N5 C14 153.9(4) . . . . ? C25 Cd1 N5 C14 127.2(4) . . . . ? C18 N6 N7 C19 -0.2(5) . . . . ? C3 N1 C2 C1 1.4(7) . . . . ? Cd1 N1 C2 C1 -167.0(4) . . . . ? C5 C1 C2 N1 0.7(7) . . . . ? C2 N1 C3 C4 -2.0(7) . . . . ? Cd1 N1 C3 C4 166.9(4) . . . . ? N1 C3 C4 C5 0.6(7) . . . . ? C2 C1 C5 C4 -2.2(7) . . . . ? C2 C1 C5 C6 178.4(4) . . . . ? C3 C4 C5 C1 1.6(7) . . . . ? C3 C4 C5 C6 -179.0(4) . . . . ? N3 N2 C6 O1 1.0(6) . . . . ? N3 N2 C6 C5 -178.6(5) . . . . ? C7 O1 C6 N2 -1.2(5) . . . . ? C7 O1 C6 C5 178.4(4) . . . . ? C1 C5 C6 N2 -168.7(5) . . . . ? C4 C5 C6 N2 11.8(8) . . . . ? C1 C5 C6 O1 11.7(7) . . . . ? C4 C5 C6 O1 -167.7(4) . . . . ? N2 N3 C7 O1 -0.5(6) . . . . ? N2 N3 C7 C8 177.5(5) . . . . ? C6 O1 C7 N3 1.0(5) . . . . ? C6 O1 C7 C8 -177.2(4) . . . . ? N3 C7 C8 C9 -175.7(5) . . . . ? O1 C7 C8 C9 2.1(7) . . . . ? N3 C7 C8 C12 2.4(8) . . . . ? O1 C7 C8 C12 -179.8(5) . . . . ? C12 C8 C9 C10 -0.1(8) . . . . ? C7 C8 C9 C10 178.1(5) . . . . ? C11 N4 C10 C9 1.7(10) . . . . ? C8 C9 C10 N4 -1.7(9) . . . . ? C10 N4 C11 C12 0.0(10) . . . . ? N4 C11 C12 C8 -1.7(10) . . . . ? C9 C8 C12 C11 1.6(8) . . . . ? C7 C8 C12 C11 -176.6(5) . . . . ? C15 N5 C14 C13 -0.8(7) . . . . ? Cd1 N5 C14 C13 177.4(3) . . . . ? C17 C13 C14 N5 0.9(7) . . . . ? C14 N5 C15 C16 -0.3(7) . . . . ? Cd1 N5 C15 C16 -178.7(3) . . . . ? N5 C15 C16 C17 1.3(7) . . . . ? C15 C16 C17 C13 -1.1(6) . . . . ? C15 C16 C17 C18 178.1(4) . . . . ? C14 C13 C17 C16 0.1(7) . . . . ? C14 C13 C17 C18 -179.1(4) . . . . ? N7 N6 C18 O2 0.3(5) . . . . ? N7 N6 C18 C17 -177.1(4) . . . . ? C19 O2 C18 N6 -0.3(5) . . . . ? C19 O2 C18 C17 177.2(4) . . . . ? C16 C17 C18 N6 3.0(7) . . . . ? C13 C17 C18 N6 -177.8(4) . . . . ? C16 C17 C18 O2 -174.2(4) . . . . ? C13 C17 C18 O2 5.0(7) . . . . ? N6 N7 C19 O2 0.0(5) . . . . ? N6 N7 C19 C20 178.8(4) . . . . ? C18 O2 C19 N7 0.2(5) . . . . ? C18 O2 C19 C20 -178.7(4) . . . . ? N7 C19 C20 C24 174.7(5) . . . . ? O2 C19 C20 C24 -6.7(7) . . . . ? N7 C19 C20 C21 -4.4(7) . . . . ? O2 C19 C20 C21 174.3(4) . . . . ? C24 C20 C21 C22 -0.4(7) . . . . ? C19 C20 C21 C22 178.7(5) . . . . ? C23 N8 C22 C21 1.0(8) . . . . ? C20 C21 C22 N8 0.0(8) . . . . ? C22 N8 C23 C24 -1.7(8) . . . . ? C21 C20 C24 C23 -0.3(7) . . . . ? C19 C20 C24 C23 -179.3(4) . . . . ? N8 C23 C24 C20 1.5(8) . . . . ? Cd1 O4 C25 O3 -4.1(4) . . . . ? Cd1 O4 C25 C26 175.7(3) . . . . ? Cd1 O3 C25 O4 4.2(4) . . . . ? Cd1 O3 C25 C26 -175.6(3) . . . . ? O7 Cd1 C25 O4 3.2(3) . . . . ? O5 Cd1 C25 O4 178.0(2) . . . . ? N1 Cd1 C25 O4 -83.6(3) . . . . ? N5 Cd1 C25 O4 87.1(3) . . . . ? O3 Cd1 C25 O4 -176.1(4) . . . . ? O7 Cd1 C25 O3 179.3(2) . . . . ? O5 Cd1 C25 O3 -5.9(3) . . . . ? N1 Cd1 C25 O3 92.5(3) . . . . ? N5 Cd1 C25 O3 -96.8(3) . . . . ? O4 Cd1 C25 O3 176.1(4) . . . . ? O4 C25 C26 C28 97.8(5) . . . 2_667 ? O3 C25 C26 C28 -82.4(5) . . . 2_667 ? O4 C25 C26 C27 -82.8(5) . . . . ? O3 C25 C26 C27 97.0(5) . . . . ? C28 C26 C27 C28 -0.7(7) 2_667 . . . ? C25 C26 C27 C28 179.9(4) . . . . ? C28 C26 C27 Br2 178.9(3) 2_667 . . . ? C25 C26 C27 Br2 -0.5(6) . . . . ? C26 C27 C28 C26 0.7(7) . . . 2_667 ? Br2 C27 C28 C26 -178.9(3) . . . 2_667 ? C26 C27 C28 Br1 179.7(3) . . . . ? Br2 C27 C28 Br1 0.1(5) . . . . ? Cd1 O5 C29 O6 10.6(5) . . . . ? Cd1 O5 C29 C30 -168.9(3) . . . . ? O6 C29 C30 C32 84.6(5) . . . 2_576 ? O5 C29 C30 C32 -95.9(5) . . . 2_576 ? O6 C29 C30 C31 -99.1(5) . . . . ? O5 C29 C30 C31 80.4(5) . . . . ? C32 C30 C31 C32 0.6(7) 2_576 . . . ? C29 C30 C31 C32 -175.8(4) . . . . ? C32 C30 C31 Br3 -178.1(3) 2_576 . . . ? C29 C30 C31 Br3 5.5(5) . . . . ? C30 C31 C32 C30 -0.6(7) . . . 2_576 ? Br3 C31 C32 C30 178.0(3) . . . 2_576 ? C30 C31 C32 Br4 178.0(3) . . . . ? Br3 C31 C32 Br4 -3.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.452 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.088 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 763370' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Br4 Cu N4 O7' _chemical_formula_weight 817.54 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2722(4) _cell_length_b 27.6453(11) _cell_length_c 11.1959(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.5610(10) _cell_angle_gamma 90.00 _cell_volume 2555.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6166 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.85 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 7.159 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.456552 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 13010 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4506 _reflns_number_gt 3674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0285P)^2^+2.1380P] 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 4506 _refine_ls_number_parameters 336 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.052 _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 Cu1 Cu 0.59434(5) 0.343785(14) 0.26867(3) 0.02412(11) Uani 1 1 d D . . Br1 Br 0.51253(5) 0.243927(13) -0.10044(3) 0.03704(11) Uani 1 1 d . . . Br2 Br 0.65722(5) 0.244217(13) -0.37184(3) 0.03730(11) Uani 1 1 d . . . Br3 Br 0.69148(5) 0.447614(13) -0.36082(3) 0.04354(12) Uani 1 1 d . . . Br4 Br 0.56872(5) 0.446627(14) -0.08082(3) 0.04394(12) Uani 1 1 d . . . O1 O 0.6435(3) 0.08747(8) 0.2693(2) 0.0317(5) Uani 1 1 d . . . O2 O 0.6052(3) 0.33965(8) 0.09249(18) 0.0277(5) Uani 1 1 d . . . O3 O 0.3454(3) 0.34997(11) 0.0251(2) 0.0490(7) Uani 1 1 d . . . O4 O 0.8490(3) 0.34527(10) -0.4928(2) 0.0466(7) Uani 1 1 d . . . O5 O 0.5863(3) 0.34732(8) -0.55544(19) 0.0310(5) Uani 1 1 d . . . O6 O 0.3456(3) 0.37134(11) 0.2580(2) 0.0490(7) Uani 1 1 d . . . H6A H 0.2944 0.3652 0.1916 0.074 Uiso 1 1 d RD . . H6B H 0.2927 0.3696 0.3206 0.074 Uiso 1 1 d RD . . N1 N 0.5728(3) 0.27140(9) 0.2746(2) 0.0242(6) Uani 1 1 d . . . N2 N 0.4700(4) 0.10073(10) 0.4080(3) 0.0449(8) Uani 1 1 d . . . N3 N 0.4982(4) 0.05075(11) 0.4013(3) 0.0491(9) Uani 1 1 d . . . N4 N 0.7952(3) -0.09171(10) 0.2404(2) 0.0281(6) Uani 1 1 d . . . C1 C 0.5638(4) 0.17192(12) 0.3052(3) 0.0269(7) Uani 1 1 d . . . C2 C 0.6599(4) 0.19230(12) 0.2208(3) 0.0311(8) Uani 1 1 d . . . H2 H 0.7216 0.1729 0.1733 0.037 Uiso 1 1 calc R . . C3 C 0.6613(4) 0.24186(12) 0.2093(3) 0.0294(8) Uani 1 1 d . . . H3 H 0.7266 0.2555 0.1536 0.035 Uiso 1 1 calc R . . C4 C 0.4756(4) 0.25135(11) 0.3524(3) 0.0275(7) Uani 1 1 d . . . H4 H 0.4111 0.2714 0.3961 0.033 Uiso 1 1 calc R . . C5 C 0.4679(4) 0.20237(12) 0.3698(3) 0.0277(7) Uani 1 1 d . . . H5 H 0.3991 0.1896 0.4244 0.033 Uiso 1 1 calc R . . C6 C 0.5563(4) 0.12044(12) 0.3296(3) 0.0302(8) Uani 1 1 d . . . C7 C 0.5991(4) 0.04492(12) 0.3199(3) 0.0336(8) Uani 1 1 d . . . C8 C 0.6649(4) -0.00161(12) 0.2837(3) 0.0310(8) Uani 1 1 d . . . C9 C 0.7948(4) -0.00639(13) 0.2125(3) 0.0342(8) Uani 1 1 d . . . H9 H 0.8399 0.0207 0.1782 0.041 Uiso 1 1 calc R . . C10 C 0.8562(4) -0.05172(12) 0.1932(3) 0.0329(8) Uani 1 1 d . . . H10 H 0.9437 -0.0547 0.1454 0.040 Uiso 1 1 calc R . . C11 C 0.6672(4) -0.08712(12) 0.3056(3) 0.0345(8) Uani 1 1 d . . . H11 H 0.6225 -0.1149 0.3370 0.041 Uiso 1 1 calc R . . C12 C 0.5975(5) -0.04295(13) 0.3287(3) 0.0380(9) Uani 1 1 d . . . H12 H 0.5069 -0.0411 0.3736 0.046 Uiso 1 1 calc R . . C13 C 0.4916(4) 0.34523(12) 0.0130(3) 0.0290(8) Uani 1 1 d . . . C14 C 0.5465(4) 0.34548(12) -0.1148(3) 0.0249(7) Uani 1 1 d . . . C15 C 0.5636(4) 0.30252(12) -0.1771(3) 0.0247(7) Uani 1 1 d . . . C16 C 0.6172(4) 0.30277(12) -0.2923(3) 0.0252(7) Uani 1 1 d . . . C17 C 0.6504(4) 0.34616(11) -0.3485(3) 0.0233(7) Uani 1 1 d . . . C18 C 0.6348(4) 0.38898(12) -0.2858(3) 0.0270(7) Uani 1 1 d . . . C19 C 0.5843(4) 0.38901(12) -0.1694(3) 0.0269(7) Uani 1 1 d . . . C20 C 0.7042(4) 0.34629(11) -0.4776(3) 0.0261(7) Uani 1 1 d . . . O7 O 0.1197(5) 0.38190(14) 0.4206(4) 0.1013(15) Uani 1 1 d D . . H7 H 0.0330 0.3708 0.4397 0.152 Uiso 1 1 calc R . . C21 C 0.1370(8) 0.4286(2) 0.4629(5) 0.095(2) Uani 1 1 d D . . H21A H 0.0659 0.4336 0.5263 0.143 Uiso 1 1 calc R . . H21B H 0.1102 0.4510 0.3991 0.143 Uiso 1 1 calc R . . H21C H 0.2471 0.4337 0.4927 0.143 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 Cu1 0.0388(2) 0.0237(2) 0.01033(19) 0.00084(15) 0.00511(16) -0.00270(17) Br1 0.0546(2) 0.0363(2) 0.02084(19) 0.00652(15) 0.00684(16) -0.00771(16) Br2 0.0620(3) 0.0309(2) 0.01939(19) -0.00325(14) 0.00590(17) 0.00459(16) Br3 0.0735(3) 0.0311(2) 0.0277(2) 0.00442(15) 0.01665(18) -0.00315(18) Br4 0.0745(3) 0.0351(2) 0.02300(19) -0.00627(15) 0.00902(18) 0.01159(19) O1 0.0404(14) 0.0246(13) 0.0309(14) 0.0011(10) 0.0092(11) 0.0030(10) O2 0.0398(14) 0.0335(13) 0.0100(11) 0.0006(9) 0.0043(10) 0.0001(10) O3 0.0361(16) 0.089(2) 0.0233(14) -0.0033(13) 0.0094(12) 0.0042(14) O4 0.0411(17) 0.0608(19) 0.0402(16) 0.0034(13) 0.0212(13) 0.0017(13) O5 0.0487(15) 0.0330(14) 0.0115(11) 0.0013(9) 0.0040(11) -0.0031(11) O6 0.0422(16) 0.080(2) 0.0254(14) -0.0088(14) 0.0101(12) 0.0079(14) N1 0.0326(16) 0.0261(15) 0.0139(13) 0.0021(11) 0.0022(12) -0.0005(12) N2 0.060(2) 0.0234(16) 0.055(2) 0.0038(15) 0.0301(17) 0.0082(15) N3 0.069(2) 0.0258(17) 0.057(2) 0.0048(15) 0.0325(19) 0.0091(15) N4 0.0394(17) 0.0271(16) 0.0180(14) -0.0017(12) 0.0046(12) 0.0035(12) C1 0.0315(18) 0.0275(18) 0.0212(17) -0.0011(14) -0.0036(14) 0.0002(14) C2 0.038(2) 0.0308(19) 0.0249(18) -0.0043(15) 0.0066(15) 0.0035(15) C3 0.038(2) 0.033(2) 0.0182(17) 0.0010(14) 0.0065(15) -0.0006(15) C4 0.0323(19) 0.0275(19) 0.0230(18) -0.0032(14) 0.0037(14) 0.0013(14) C5 0.0311(19) 0.0296(19) 0.0227(18) -0.0011(14) 0.0048(14) -0.0036(14) C6 0.036(2) 0.0268(18) 0.0277(19) -0.0027(15) 0.0021(16) 0.0036(15) C7 0.041(2) 0.0240(19) 0.036(2) 0.0023(15) 0.0049(17) 0.0029(15) C8 0.042(2) 0.0254(18) 0.0250(18) -0.0013(14) -0.0002(16) 0.0044(15) C9 0.046(2) 0.0289(19) 0.0288(19) 0.0043(15) 0.0089(16) -0.0002(16) C10 0.047(2) 0.030(2) 0.0232(18) 0.0021(15) 0.0138(16) 0.0033(16) C11 0.047(2) 0.0268(19) 0.031(2) 0.0039(15) 0.0143(17) 0.0007(16) C12 0.047(2) 0.032(2) 0.038(2) 0.0041(17) 0.0177(18) 0.0052(16) C13 0.040(2) 0.034(2) 0.0135(17) 0.0023(14) 0.0069(15) -0.0033(15) C14 0.0259(17) 0.0352(19) 0.0138(16) 0.0011(14) 0.0027(13) 0.0009(14) C15 0.0269(17) 0.0327(19) 0.0147(16) 0.0064(14) 0.0031(13) -0.0010(14) C16 0.0302(18) 0.0298(18) 0.0156(16) -0.0029(14) 0.0014(13) 0.0038(14) C17 0.0253(17) 0.0307(18) 0.0142(16) 0.0022(13) 0.0054(13) 0.0013(13) C18 0.0370(19) 0.0294(19) 0.0151(16) 0.0023(14) 0.0046(14) 0.0004(15) C19 0.0342(19) 0.0332(19) 0.0137(16) -0.0016(14) 0.0042(14) 0.0058(15) C20 0.041(2) 0.0221(17) 0.0168(17) 0.0011(13) 0.0110(15) -0.0010(14) O7 0.095(3) 0.092(3) 0.126(4) -0.036(3) 0.079(3) -0.036(2) C21 0.124(5) 0.099(5) 0.066(4) -0.026(3) 0.036(4) -0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.977(2) 1_556 ? Cu1 O2 1.983(2) . ? Cu1 N4 2.009(3) 2_655 ? Cu1 N1 2.010(3) . ? Cu1 O6 2.190(3) . ? Br1 C15 1.893(3) . ? Br2 C16 1.887(3) . ? Br3 C18 1.898(3) . ? Br4 C19 1.885(3) . ? O1 C7 1.366(4) . ? O1 C6 1.366(4) . ? O2 C13 1.263(4) . ? O3 C13 1.232(4) . ? O4 C20 1.221(4) . ? O5 C20 1.267(4) . ? O5 Cu1 1.977(2) 1_554 ? O6 H6A 0.8500 . ? O6 H6B 0.8497 . ? N1 C4 1.341(4) . ? N1 C3 1.343(4) . ? N2 C6 1.286(5) . ? N2 N3 1.404(4) . ? N3 C7 1.283(5) . ? N4 C11 1.329(4) . ? N4 C10 1.338(4) . ? N4 Cu1 2.009(3) 2_645 ? C1 C5 1.390(5) . ? C1 C2 1.391(5) . ? C1 C6 1.451(5) . ? C2 C3 1.376(5) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.370(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.464(5) . ? C8 C12 1.381(5) . ? C8 C9 1.383(5) . ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.382(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.527(4) . ? C14 C15 1.389(5) . ? C14 C19 1.394(4) . ? C15 C16 1.389(4) . ? C16 C17 1.390(4) . ? C17 C18 1.386(4) . ? C17 C20 1.538(4) . ? C18 C19 1.393(4) . ? O7 C21 1.380(5) . ? O7 H7 0.8200 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 O5 Cu1 O2 179.18(10) 1_556 . ? O5 Cu1 N4 92.87(10) 1_556 2_655 ? O2 Cu1 N4 87.25(10) . 2_655 ? O5 Cu1 N1 90.45(10) 1_556 . ? O2 Cu1 N1 89.14(10) . . ? N4 Cu1 N1 157.90(11) 2_655 . ? O5 Cu1 O6 86.98(10) 1_556 . ? O2 Cu1 O6 93.81(9) . . ? N4 Cu1 O6 96.73(11) 2_655 . ? N1 Cu1 O6 105.26(11) . . ? C7 O1 C6 101.9(3) . . ? C13 O2 Cu1 128.0(2) . . ? C20 O5 Cu1 127.8(2) . 1_554 ? Cu1 O6 H6A 113.2 . . ? Cu1 O6 H6B 117.7 . . ? H6A O6 H6B 117.0 . . ? C4 N1 C3 118.1(3) . . ? C4 N1 Cu1 119.4(2) . . ? C3 N1 Cu1 122.3(2) . . ? C6 N2 N3 106.2(3) . . ? C7 N3 N2 106.2(3) . . ? C11 N4 C10 118.1(3) . . ? C11 N4 Cu1 119.5(2) . 2_645 ? C10 N4 Cu1 122.0(2) . 2_645 ? C5 C1 C2 118.5(3) . . ? C5 C1 C6 117.6(3) . . ? C2 C1 C6 123.9(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? N1 C3 C2 123.1(3) . . ? N1 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? N1 C4 C5 122.4(3) . . ? N1 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C1 119.4(3) . . ? C4 C5 H5 120.3 . . ? C1 C5 H5 120.3 . . ? N2 C6 O1 112.8(3) . . ? N2 C6 C1 125.2(3) . . ? O1 C6 C1 122.1(3) . . ? N3 C7 O1 112.9(3) . . ? N3 C7 C8 125.2(3) . . ? O1 C7 C8 121.9(3) . . ? C12 C8 C9 118.5(3) . . ? C12 C8 C7 117.4(3) . . ? C9 C8 C7 124.0(3) . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N4 C10 C9 122.6(3) . . ? N4 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N4 C11 C12 122.9(3) . . ? N4 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C8 C12 C11 118.7(3) . . ? C8 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? O3 C13 O2 128.9(3) . . ? O3 C13 C14 116.9(3) . . ? O2 C13 C14 114.2(3) . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C13 120.8(3) . . ? C19 C14 C13 120.2(3) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 Br1 121.2(2) . . ? C14 C15 Br1 118.1(2) . . ? C15 C16 C17 120.6(3) . . ? C15 C16 Br2 120.6(2) . . ? C17 C16 Br2 118.8(2) . . ? C18 C17 C16 118.7(3) . . ? C18 C17 C20 121.0(3) . . ? C16 C17 C20 120.3(3) . . ? C17 C18 C19 121.1(3) . . ? C17 C18 Br3 118.1(2) . . ? C19 C18 Br3 120.7(2) . . ? C18 C19 C14 119.9(3) . . ? C18 C19 Br4 121.8(2) . . ? C14 C19 Br4 118.3(2) . . ? O4 C20 O5 128.6(3) . . ? O4 C20 C17 118.3(3) . . ? O5 C20 C17 113.1(3) . . ? C21 O7 H7 109.5 . . ? O7 C21 H21A 109.5 . . ? O7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 Cu1 O2 C13 -105.2(3) 2_655 . . . ? N1 Cu1 O2 C13 96.6(3) . . . . ? O6 Cu1 O2 C13 -8.6(3) . . . . ? O5 Cu1 N1 C4 37.8(2) 1_556 . . . ? O2 Cu1 N1 C4 -142.9(2) . . . . ? N4 Cu1 N1 C4 136.5(3) 2_655 . . . ? O6 Cu1 N1 C4 -49.2(2) . . . . ? O5 Cu1 N1 C3 -137.4(3) 1_556 . . . ? O2 Cu1 N1 C3 41.9(2) . . . . ? N4 Cu1 N1 C3 -38.6(4) 2_655 . . . ? O6 Cu1 N1 C3 135.6(2) . . . . ? C6 N2 N3 C7 0.2(4) . . . . ? C5 C1 C2 C3 3.0(5) . . . . ? C6 C1 C2 C3 -177.4(3) . . . . ? C4 N1 C3 C2 -1.8(5) . . . . ? Cu1 N1 C3 C2 173.4(3) . . . . ? C1 C2 C3 N1 -0.8(5) . . . . ? C3 N1 C4 C5 2.2(5) . . . . ? Cu1 N1 C4 C5 -173.2(2) . . . . ? N1 C4 C5 C1 0.0(5) . . . . ? C2 C1 C5 C4 -2.7(5) . . . . ? C6 C1 C5 C4 177.8(3) . . . . ? N3 N2 C6 O1 -0.4(4) . . . . ? N3 N2 C6 C1 179.6(3) . . . . ? C7 O1 C6 N2 0.4(4) . . . . ? C7 O1 C6 C1 -179.6(3) . . . . ? C5 C1 C6 N2 -1.3(5) . . . . ? C2 C1 C6 N2 179.1(4) . . . . ? C5 C1 C6 O1 178.7(3) . . . . ? C2 C1 C6 O1 -0.8(5) . . . . ? N2 N3 C7 O1 0.0(4) . . . . ? N2 N3 C7 C8 179.1(3) . . . . ? C6 O1 C7 N3 -0.2(4) . . . . ? C6 O1 C7 C8 -179.3(3) . . . . ? N3 C7 C8 C12 9.2(6) . . . . ? O1 C7 C8 C12 -171.9(3) . . . . ? N3 C7 C8 C9 -167.5(4) . . . . ? O1 C7 C8 C9 11.5(5) . . . . ? C12 C8 C9 C10 -2.7(5) . . . . ? C7 C8 C9 C10 174.0(3) . . . . ? C11 N4 C10 C9 2.0(5) . . . . ? Cu1 N4 C10 C9 -170.9(3) 2_645 . . . ? C8 C9 C10 N4 0.1(5) . . . . ? C10 N4 C11 C12 -1.6(5) . . . . ? Cu1 N4 C11 C12 171.5(3) 2_645 . . . ? C9 C8 C12 C11 3.1(5) . . . . ? C7 C8 C12 C11 -173.8(3) . . . . ? N4 C11 C12 C8 -1.0(6) . . . . ? Cu1 O2 C13 O3 -7.6(5) . . . . ? Cu1 O2 C13 C14 173.09(19) . . . . ? O3 C13 C14 C15 -93.4(4) . . . . ? O2 C13 C14 C15 86.0(4) . . . . ? O3 C13 C14 C19 88.3(4) . . . . ? O2 C13 C14 C19 -92.3(4) . . . . ? C19 C14 C15 C16 -0.1(5) . . . . ? C13 C14 C15 C16 -178.5(3) . . . . ? C19 C14 C15 Br1 179.7(2) . . . . ? C13 C14 C15 Br1 1.3(4) . . . . ? C14 C15 C16 C17 -1.8(5) . . . . ? Br1 C15 C16 C17 178.4(2) . . . . ? C14 C15 C16 Br2 174.8(2) . . . . ? Br1 C15 C16 Br2 -5.0(4) . . . . ? C15 C16 C17 C18 2.3(5) . . . . ? Br2 C16 C17 C18 -174.3(2) . . . . ? C15 C16 C17 C20 -177.9(3) . . . . ? Br2 C16 C17 C20 5.5(4) . . . . ? C16 C17 C18 C19 -1.0(5) . . . . ? C20 C17 C18 C19 179.2(3) . . . . ? C16 C17 C18 Br3 176.8(2) . . . . ? C20 C17 C18 Br3 -3.0(4) . . . . ? C17 C18 C19 C14 -0.9(5) . . . . ? Br3 C18 C19 C14 -178.6(2) . . . . ? C17 C18 C19 Br4 178.0(2) . . . . ? Br3 C18 C19 Br4 0.3(4) . . . . ? C15 C14 C19 C18 1.4(5) . . . . ? C13 C14 C19 C18 179.8(3) . . . . ? C15 C14 C19 Br4 -177.4(2) . . . . ? C13 C14 C19 Br4 0.9(4) . . . . ? Cu1 O5 C20 O4 3.9(5) 1_554 . . . ? Cu1 O5 C20 C17 -175.83(19) 1_554 . . . ? C18 C17 C20 O4 87.7(4) . . . . ? C16 C17 C20 O4 -92.1(4) . . . . ? C18 C17 C20 O5 -92.6(4) . . . . ? C16 C17 C20 O5 87.7(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.491 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.112 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 763371' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H19 Br4 N5 O8 Zn' _chemical_formula_weight 878.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.398(4) _cell_length_b 12.337(4) _cell_length_c 12.667(4) _cell_angle_alpha 65.774(5) _cell_angle_beta 75.569(5) _cell_angle_gamma 75.861(4) _cell_volume 1552.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2787 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.93 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 5.989 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.677199 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 8038 _diffrn_reflns_av_R_equivalents 0.0884 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5451 _reflns_number_gt 3592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.1038P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5451 _refine_ls_number_parameters 396 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.003 _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 0.53489(6) 0.35076(6) 0.31487(6) 0.0337(2) Uani 1 1 d . . . Br1 Br 1.18776(7) 0.54055(8) 0.09442(7) 0.0614(3) Uani 1 1 d . . . Br2 Br 1.16920(7) 0.12094(7) 0.50232(8) 0.0650(3) Uani 1 1 d . . . Br3 Br 0.86492(7) 0.16489(7) 0.52892(9) 0.0684(3) Uani 1 1 d . . . Br4 Br 0.88280(7) 0.59320(8) 0.12916(8) 0.0672(3) Uani 1 1 d . . . O1 O 0.4566(4) 0.9318(4) -0.1060(4) 0.0425(11) Uani 1 1 d . . . O2 O 0.7200(4) 0.3423(4) 0.2899(4) 0.0457(12) Uani 1 1 d . . . O3 O 0.6963(4) 0.4508(5) 0.3989(6) 0.0655(16) Uani 1 1 d . . . O4 O 1.3415(4) 0.3541(4) 0.3250(4) 0.0422(11) Uani 1 1 d . . . O5 O 1.3446(4) 0.2367(5) 0.2273(5) 0.0564(14) Uani 1 1 d . . . O6 O 0.5697(4) 0.2540(5) 0.2143(6) 0.0755(19) Uani 1 1 d . . . H6A H 0.6387 0.2662 0.1704 0.113 Uiso 1 1 d R . . H6B H 0.5194 0.2339 0.1888 0.113 Uiso 1 1 d R . . O7 O 0.2381(6) 0.9008(8) 0.8073(11) 0.153(4) Uani 1 1 d . . . N1 N 0.4925(5) 0.5326(4) 0.2282(5) 0.0395(13) Uani 1 1 d . . . N2 N 0.3249(6) 0.9817(5) 0.0345(5) 0.0543(17) Uani 1 1 d . . . N3 N 0.3267(6) 1.0821(5) -0.0696(6) 0.0566(17) Uani 1 1 d . . . N4 N 0.5045(5) 1.2574(4) -0.5078(5) 0.0363(13) Uani 1 1 d . . . N5 N 0.0302(7) 0.9225(7) 0.8279(8) 0.081(2) Uani 1 1 d . . . C1 C 0.3651(7) 0.7237(6) 0.1929(7) 0.055(2) Uani 1 1 d . . . H1 H 0.2981 0.7710 0.2208 0.066 Uiso 1 1 calc R . . C2 C 0.3978(7) 0.6035(6) 0.2600(7) 0.058(2) Uani 1 1 d . . . H2 H 0.3491 0.5711 0.3325 0.069 Uiso 1 1 calc R . . C3 C 0.5587(6) 0.5801(6) 0.1232(6) 0.0488(18) Uani 1 1 d . . . H3 H 0.6263 0.5310 0.0986 0.059 Uiso 1 1 calc R . . C4 C 0.5337(6) 0.6965(6) 0.0492(6) 0.0466(18) Uani 1 1 d . . . H4 H 0.5828 0.7256 -0.0238 0.056 Uiso 1 1 calc R . . C5 C 0.4334(6) 0.7708(6) 0.0850(6) 0.0402(16) Uani 1 1 d . . . C6 C 0.4009(6) 0.8960(6) 0.0073(6) 0.0441(17) Uani 1 1 d . . . C7 C 0.4033(7) 1.0493(6) -0.1476(6) 0.0448(17) Uani 1 1 d . . . C8 C 0.4416(6) 1.1197(6) -0.2733(6) 0.0413(16) Uani 1 1 d . . . C9 C 0.5226(7) 1.0700(6) -0.3472(7) 0.0508(19) Uani 1 1 d . . . H9 H 0.5581 0.9894 -0.3193 0.061 Uiso 1 1 calc R . . C10 C 0.5502(6) 1.1405(6) -0.4621(6) 0.0478(18) Uani 1 1 d . . . H10 H 0.6042 1.1054 -0.5119 0.057 Uiso 1 1 calc R . . C11 C 0.4316(7) 1.3029(6) -0.4349(6) 0.0513(19) Uani 1 1 d . . . H11 H 0.4023 1.3851 -0.4642 0.062 Uiso 1 1 calc R . . C12 C 0.3942(7) 1.2404(6) -0.3187(7) 0.0516(19) Uani 1 1 d . . . H12 H 0.3386 1.2779 -0.2717 0.062 Uiso 1 1 calc R . . C13 C 0.8979(6) 0.3740(6) 0.3253(6) 0.0396(16) Uani 1 1 d . . . C14 C 0.9665(6) 0.4536(6) 0.2343(6) 0.0408(16) Uani 1 1 d . . . C15 C 1.0931(6) 0.4327(6) 0.2190(6) 0.0411(16) Uani 1 1 d . . . C16 C 1.1536(5) 0.3316(6) 0.2985(6) 0.0391(16) Uani 1 1 d . . . C17 C 1.0866(5) 0.2526(6) 0.3899(6) 0.0393(16) Uani 1 1 d . . . C18 C 0.9591(6) 0.2737(6) 0.4039(7) 0.0437(17) Uani 1 1 d . . . C19 C 0.7563(6) 0.3936(6) 0.3412(7) 0.0446(17) Uani 1 1 d . . . C20 C 1.2939(6) 0.3054(6) 0.2823(6) 0.0414(17) Uani 1 1 d . . . C21 C 0.0056(11) 1.0414(11) 0.8309(11) 0.115(4) Uani 1 1 d . . . H21A H 0.0795 1.0610 0.8372 0.172 Uiso 1 1 calc R . . H21B H -0.0561 1.0439 0.8974 0.172 Uiso 1 1 calc R . . H21C H -0.0228 1.0988 0.7601 0.172 Uiso 1 1 calc R . . C22 C -0.0750(9) 0.8756(10) 0.8301(11) 0.097(3) Uani 1 1 d . . . H22A H -0.1042 0.9186 0.7566 0.146 Uiso 1 1 calc R . . H22B H -0.1388 0.8853 0.8928 0.146 Uiso 1 1 calc R . . H22C H -0.0519 0.7917 0.8422 0.146 Uiso 1 1 calc R . . C23 C 0.1432(9) 0.8624(11) 0.8138(12) 0.103(4) Uani 1 1 d . . . H23 H 0.1525 0.7877 0.8085 0.124 Uiso 1 1 calc R . . O8 O 0.0000 0.5000 0.5000 0.041(3) Uani 0.50 2 d SPU A 1 O9 O 0.094(2) 0.621(2) 0.368(2) 0.061(6) Uani 0.25 1 d PU B 2 O10 O 0.072(3) 0.552(3) 0.435(3) 0.087(8) Uani 0.25 1 d PU C 3 O11 O -0.102(3) 0.568(2) 0.461(2) 0.088(8) Uani 0.25 1 d PU D 4 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 0.0168(4) 0.0356(4) 0.0450(5) -0.0115(3) -0.0072(3) -0.0017(3) Br1 0.0332(4) 0.0769(6) 0.0580(5) -0.0088(4) -0.0041(4) -0.0135(4) Br2 0.0332(4) 0.0522(5) 0.0879(6) -0.0051(4) -0.0174(4) 0.0011(3) Br3 0.0338(4) 0.0604(5) 0.0934(7) -0.0086(5) -0.0049(4) -0.0185(4) Br4 0.0351(4) 0.0730(6) 0.0747(6) -0.0072(5) -0.0232(4) 0.0026(4) O1 0.033(2) 0.036(2) 0.048(3) -0.008(2) -0.009(2) 0.002(2) O2 0.016(2) 0.058(3) 0.073(3) -0.032(3) -0.013(2) -0.005(2) O3 0.028(3) 0.079(4) 0.112(5) -0.070(4) -0.002(3) 0.003(3) O4 0.019(2) 0.058(3) 0.057(3) -0.028(2) -0.009(2) -0.007(2) O5 0.018(2) 0.081(4) 0.081(4) -0.045(3) -0.009(2) -0.001(2) O6 0.020(2) 0.122(5) 0.130(5) -0.100(4) -0.011(3) 0.001(3) O7 0.046(4) 0.170(8) 0.316(14) -0.178(9) -0.059(6) 0.037(5) N1 0.021(3) 0.039(3) 0.048(3) -0.009(3) -0.003(3) -0.002(2) N2 0.055(4) 0.042(3) 0.048(4) -0.012(3) 0.000(3) 0.006(3) N3 0.059(4) 0.037(3) 0.054(4) -0.012(3) 0.000(3) 0.008(3) N4 0.022(3) 0.030(3) 0.052(3) -0.012(3) -0.009(2) 0.002(2) N5 0.050(4) 0.089(6) 0.105(6) -0.053(5) -0.016(4) 0.019(4) C1 0.041(4) 0.039(4) 0.058(5) -0.007(4) 0.008(4) 0.007(3) C2 0.040(4) 0.050(4) 0.054(5) -0.005(4) 0.009(4) 0.003(3) C3 0.033(4) 0.045(4) 0.054(5) -0.010(4) -0.006(3) 0.004(3) C4 0.037(4) 0.053(4) 0.033(4) -0.007(3) -0.004(3) 0.003(3) C5 0.032(4) 0.040(4) 0.045(4) -0.010(3) -0.012(3) -0.003(3) C6 0.038(4) 0.044(4) 0.044(4) -0.009(3) -0.007(3) -0.008(3) C7 0.046(4) 0.033(4) 0.051(4) -0.006(3) -0.020(4) -0.003(3) C8 0.037(4) 0.039(4) 0.047(4) -0.012(3) -0.015(3) -0.005(3) C9 0.042(4) 0.029(3) 0.061(5) -0.004(3) -0.005(4) 0.005(3) C10 0.036(4) 0.042(4) 0.048(4) -0.010(3) 0.003(3) 0.002(3) C11 0.057(5) 0.038(4) 0.051(5) -0.010(4) -0.020(4) 0.006(3) C12 0.060(5) 0.040(4) 0.050(5) -0.018(3) -0.015(4) 0.010(3) C13 0.018(3) 0.044(4) 0.061(4) -0.023(3) -0.010(3) -0.001(3) C14 0.021(3) 0.049(4) 0.054(4) -0.019(3) -0.015(3) 0.000(3) C15 0.026(3) 0.051(4) 0.052(4) -0.023(3) -0.007(3) -0.007(3) C16 0.014(3) 0.047(4) 0.061(4) -0.026(3) -0.010(3) 0.000(3) C17 0.018(3) 0.041(4) 0.060(4) -0.021(3) -0.010(3) 0.002(3) C18 0.018(3) 0.049(4) 0.067(5) -0.023(4) -0.003(3) -0.012(3) C19 0.016(3) 0.045(4) 0.069(5) -0.020(4) -0.009(3) 0.002(3) C20 0.017(3) 0.043(4) 0.060(5) -0.018(4) -0.005(3) -0.001(3) C21 0.090(9) 0.128(10) 0.116(10) -0.063(8) -0.010(7) 0.027(7) C22 0.051(6) 0.111(8) 0.120(9) -0.037(7) -0.010(6) -0.011(6) C23 0.047(6) 0.116(9) 0.164(12) -0.084(9) -0.025(7) 0.018(6) O8 0.017(5) 0.061(7) 0.063(7) -0.043(6) 0.004(5) -0.015(5) O9 0.058(9) 0.063(9) 0.060(9) -0.029(8) 0.002(7) -0.007(7) O10 0.124(13) 0.078(11) 0.085(11) -0.062(9) 0.000(9) -0.025(9) O11 0.106(12) 0.097(11) 0.097(11) -0.071(9) -0.019(8) -0.015(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 Zn1 O6 1.992(5) . ? Zn1 O2 2.037(4) . ? Zn1 N4 2.044(5) 1_546 ? Zn1 N1 2.046(5) . ? Zn1 O4 2.167(4) 1_455 ? Br1 C15 1.885(7) . ? Br2 C17 1.891(7) . ? Br3 C18 1.891(7) . ? Br4 C14 1.897(7) . ? O1 C6 1.349(8) . ? O1 C7 1.361(8) . ? O2 C19 1.262(8) . ? O3 C19 1.199(8) . ? O4 C20 1.234(8) . ? O4 Zn1 2.167(4) 1_655 ? O5 C20 1.258(8) . ? O6 H6A 0.8500 . ? O6 H6B 0.8498 . ? O7 C23 1.254(13) . ? N1 C2 1.306(9) . ? N1 C3 1.326(8) . ? N2 C6 1.299(9) . ? N2 N3 1.390(8) . ? N3 C7 1.276(9) . ? N4 C11 1.294(9) . ? N4 C10 1.336(8) . ? N4 Zn1 2.044(5) 1_564 ? N5 C23 1.330(11) . ? N5 C21 1.440(13) . ? N5 C22 1.443(12) . ? C1 C5 1.360(9) . ? C1 C2 1.383(10) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.360(9) . ? C3 H3 0.9300 . ? C4 C5 1.387(9) . ? C4 H4 0.9300 . ? C5 C6 1.465(9) . ? C7 C8 1.477(10) . ? C8 C9 1.367(10) . ? C8 C12 1.378(9) . ? C9 C10 1.356(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.364(10) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.379(9) . ? C13 C18 1.387(9) . ? C13 C19 1.546(8) . ? C14 C15 1.381(9) . ? C15 C16 1.394(9) . ? C16 C17 1.368(9) . ? C16 C20 1.530(8) . ? C17 C18 1.391(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O2 86.53(19) . . ? O6 Zn1 N4 116.2(2) . 1_546 ? O2 Zn1 N4 98.9(2) . 1_546 ? O6 Zn1 N1 114.7(3) . . ? O2 Zn1 N1 97.17(19) . . ? N4 Zn1 N1 127.2(2) 1_546 . ? O6 Zn1 O4 87.52(18) . 1_455 ? O2 Zn1 O4 173.77(18) . 1_455 ? N4 Zn1 O4 85.41(19) 1_546 1_455 ? N1 Zn1 O4 83.64(19) . 1_455 ? C6 O1 C7 101.2(5) . . ? C19 O2 Zn1 115.8(4) . . ? C20 O4 Zn1 128.4(4) . 1_655 ? Zn1 O6 H6A 107.7 . . ? Zn1 O6 H6B 128.9 . . ? H6A O6 H6B 116.7 . . ? C2 N1 C3 116.7(6) . . ? C2 N1 Zn1 126.0(5) . . ? C3 N1 Zn1 116.8(4) . . ? C6 N2 N3 105.1(6) . . ? C7 N3 N2 106.6(6) . . ? C11 N4 C10 116.0(6) . . ? C11 N4 Zn1 122.9(4) . 1_564 ? C10 N4 Zn1 120.7(5) . 1_564 ? C23 N5 C21 122.8(9) . . ? C23 N5 C22 121.0(9) . . ? C21 N5 C22 115.9(8) . . ? C5 C1 C2 118.2(7) . . ? C5 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? N1 C2 C1 124.3(7) . . ? N1 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? N1 C3 C4 123.9(6) . . ? N1 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C3 C4 C5 118.6(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C1 C5 C4 118.3(6) . . ? C1 C5 C6 121.1(6) . . ? C4 C5 C6 120.6(6) . . ? N2 C6 O1 113.6(6) . . ? N2 C6 C5 127.7(7) . . ? O1 C6 C5 118.7(6) . . ? N3 C7 O1 113.5(6) . . ? N3 C7 C8 129.7(6) . . ? O1 C7 C8 116.8(6) . . ? C9 C8 C12 118.2(6) . . ? C9 C8 C7 122.7(6) . . ? C12 C8 C7 119.1(6) . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N4 C10 C9 123.8(7) . . ? N4 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N4 C11 C12 125.4(7) . . ? N4 C11 H11 117.3 . . ? C12 C11 H11 117.3 . . ? C11 C12 C8 117.7(7) . . ? C11 C12 H12 121.1 . . ? C8 C12 H12 121.1 . . ? C14 C13 C18 118.3(6) . . ? C14 C13 C19 121.9(6) . . ? C18 C13 C19 119.8(6) . . ? C13 C14 C15 121.3(6) . . ? C13 C14 Br4 118.4(5) . . ? C15 C14 Br4 120.3(5) . . ? C14 C15 C16 119.9(6) . . ? C14 C15 Br1 121.6(5) . . ? C16 C15 Br1 118.5(5) . . ? C17 C16 C15 119.4(6) . . ? C17 C16 C20 119.7(6) . . ? C15 C16 C20 120.9(6) . . ? C16 C17 C18 120.3(6) . . ? C16 C17 Br2 118.9(4) . . ? C18 C17 Br2 120.7(5) . . ? C13 C18 C17 120.9(6) . . ? C13 C18 Br3 118.2(5) . . ? C17 C18 Br3 120.9(5) . . ? O3 C19 O2 128.7(6) . . ? O3 C19 C13 119.2(7) . . ? O2 C19 C13 112.1(6) . . ? O4 C20 O5 129.0(6) . . ? O4 C20 C16 115.7(6) . . ? O5 C20 C16 115.3(6) . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O7 C23 N5 123.7(10) . . ? O7 C23 H23 118.1 . . ? N5 C23 H23 118.1 . . ? 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 O6 Zn1 O2 C19 -179.0(5) . . . . ? N4 Zn1 O2 C19 -63.0(5) 1_546 . . . ? N1 Zn1 O2 C19 66.5(5) . . . . ? O6 Zn1 N1 C2 129.6(7) . . . . ? O2 Zn1 N1 C2 -140.9(7) . . . . ? N4 Zn1 N1 C2 -34.0(8) 1_546 . . . ? O4 Zn1 N1 C2 45.3(7) 1_455 . . . ? O6 Zn1 N1 C3 -41.7(6) . . . . ? O2 Zn1 N1 C3 47.8(5) . . . . ? N4 Zn1 N1 C3 154.7(5) 1_546 . . . ? O4 Zn1 N1 C3 -126.0(5) 1_455 . . . ? C6 N2 N3 C7 -1.1(9) . . . . ? C3 N1 C2 C1 -1.6(12) . . . . ? Zn1 N1 C2 C1 -172.9(6) . . . . ? C5 C1 C2 N1 2.1(13) . . . . ? C2 N1 C3 C4 0.4(11) . . . . ? Zn1 N1 C3 C4 172.6(6) . . . . ? N1 C3 C4 C5 0.2(12) . . . . ? C2 C1 C5 C4 -1.4(12) . . . . ? C2 C1 C5 C6 177.5(7) . . . . ? C3 C4 C5 C1 0.3(11) . . . . ? C3 C4 C5 C6 -178.5(7) . . . . ? N3 N2 C6 O1 1.9(9) . . . . ? N3 N2 C6 C5 -179.9(7) . . . . ? C7 O1 C6 N2 -1.9(8) . . . . ? C7 O1 C6 C5 179.7(6) . . . . ? C1 C5 C6 N2 14.3(12) . . . . ? C4 C5 C6 N2 -166.9(8) . . . . ? C1 C5 C6 O1 -167.6(7) . . . . ? C4 C5 C6 O1 11.3(10) . . . . ? N2 N3 C7 O1 0.0(9) . . . . ? N2 N3 C7 C8 -179.6(7) . . . . ? C6 O1 C7 N3 1.1(8) . . . . ? C6 O1 C7 C8 -179.3(6) . . . . ? N3 C7 C8 C9 -177.7(8) . . . . ? O1 C7 C8 C9 2.8(10) . . . . ? N3 C7 C8 C12 2.2(12) . . . . ? O1 C7 C8 C12 -177.3(6) . . . . ? C12 C8 C9 C10 -1.6(11) . . . . ? C7 C8 C9 C10 178.2(7) . . . . ? C11 N4 C10 C9 1.2(11) . . . . ? Zn1 N4 C10 C9 -172.4(6) 1_564 . . . ? C8 C9 C10 N4 1.2(12) . . . . ? C10 N4 C11 C12 -3.4(11) . . . . ? Zn1 N4 C11 C12 170.1(6) 1_564 . . . ? N4 C11 C12 C8 2.9(12) . . . . ? C9 C8 C12 C11 -0.2(11) . . . . ? C7 C8 C12 C11 179.9(7) . . . . ? C18 C13 C14 C15 2.0(11) . . . . ? C19 C13 C14 C15 -177.8(7) . . . . ? C18 C13 C14 Br4 -178.3(5) . . . . ? C19 C13 C14 Br4 1.9(9) . . . . ? C13 C14 C15 C16 -2.0(11) . . . . ? Br4 C14 C15 C16 178.3(5) . . . . ? C13 C14 C15 Br1 179.7(5) . . . . ? Br4 C14 C15 Br1 0.0(9) . . . . ? C14 C15 C16 C17 1.3(10) . . . . ? Br1 C15 C16 C17 179.6(5) . . . . ? C14 C15 C16 C20 178.9(7) . . . . ? Br1 C15 C16 C20 -2.7(9) . . . . ? C15 C16 C17 C18 -0.6(11) . . . . ? C20 C16 C17 C18 -178.3(6) . . . . ? C15 C16 C17 Br2 -176.3(5) . . . . ? C20 C16 C17 Br2 6.0(9) . . . . ? C14 C13 C18 C17 -1.3(11) . . . . ? C19 C13 C18 C17 178.5(7) . . . . ? C14 C13 C18 Br3 179.8(5) . . . . ? C19 C13 C18 Br3 -0.4(9) . . . . ? C16 C17 C18 C13 0.6(11) . . . . ? Br2 C17 C18 C13 176.2(5) . . . . ? C16 C17 C18 Br3 179.5(5) . . . . ? Br2 C17 C18 Br3 -4.9(9) . . . . ? Zn1 O2 C19 O3 -3.4(10) . . . . ? Zn1 O2 C19 C13 175.5(4) . . . . ? C14 C13 C19 O3 -89.3(9) . . . . ? C18 C13 C19 O3 90.9(9) . . . . ? C14 C13 C19 O2 91.7(8) . . . . ? C18 C13 C19 O2 -88.1(8) . . . . ? Zn1 O4 C20 O5 4.0(11) 1_655 . . . ? Zn1 O4 C20 C16 -176.2(4) 1_655 . . . ? C17 C16 C20 O4 -95.7(8) . . . . ? C15 C16 C20 O4 86.7(8) . . . . ? C17 C16 C20 O5 84.1(9) . . . . ? C15 C16 C20 O5 -93.5(8) . . . . ? C21 N5 C23 O7 3(2) . . . . ? C22 N5 C23 O7 177.4(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.213 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.173 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 763372' #TrackingRef 'C003738A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H8 Br4 N4 O5 Pb' _chemical_formula_weight 911.10 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.691(2) _cell_length_b 13.201(2) _cell_length_c 16.250(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.032(3) _cell_angle_gamma 90.00 _cell_volume 2483.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3324 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.42 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 13.269 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.218238 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'APEX II 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 5985 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2200 _reflns_number_gt 1881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0491P)^2^+13.4134P] 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 2200 _refine_ls_number_parameters 231 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.036 _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 Pb1 Pb 1.0000 1.01323(3) 0.7500 0.03344(17) Uani 1 2 d S . . Br1 Br 1.36658(8) 0.82386(8) 0.83824(5) 0.0505(3) Uani 1 1 d . . . Br2 Br 1.48762(7) 0.63993(8) 0.96105(5) 0.0464(3) Uani 1 1 d . . . O1 O 1.0643(5) 0.8766(4) 0.8319(3) 0.0442(14) Uani 1 1 d . . . O2 O 1.1691(6) 0.9968(5) 0.9022(4) 0.0493(16) Uani 1 1 d . . . C1 C 1.1399(7) 0.9095(7) 0.8897(5) 0.0370(19) Uani 1 1 d . . . C2 C 1.1969(6) 0.8249(6) 0.9477(5) 0.0333(18) Uani 1 1 d . . . C3 C 1.3009(6) 0.7803(7) 0.9316(5) 0.0359(19) Uani 1 1 d . . . C4 C 1.3529(6) 0.7053(6) 0.9837(4) 0.0303(17) Uani 1 1 d . . . C5 C 0.6110(18) 1.0445(18) 0.8731(11) 0.052(7) Uani 0.50 1 d PD . . C6 C 0.6812(16) 0.963(2) 0.8990(15) 0.086(14) Uani 0.50 1 d PD . . H6A H 0.6623 0.9220 0.9440 0.103 Uiso 0.50 1 d PR . . C7 C 0.7773(16) 0.9390(19) 0.8624(11) 0.054(6) Uani 0.50 1 d PD . . H7A H 0.8238 0.8816 0.8819 0.065 Uiso 0.50 1 d PR . . N1 N 0.806(2) 0.9951(14) 0.8000(13) 0.052(8) Uani 0.50 1 d PD . . C8 C 0.7397(12) 1.0742(14) 0.7732(11) 0.052(5) Uani 0.50 1 d PD . . H8A H 0.7604 1.1136 0.7278 0.062 Uiso 0.50 1 d PR . . C9 C 0.6429(11) 1.1010(12) 0.8083(9) 0.043(4) Uani 0.50 1 d PD . . H9A H 0.5979 1.1587 0.7876 0.052 Uiso 0.50 1 d PR . . O5 O 0.4860(12) 1.0331(12) 0.9802(8) 0.077(7) Uani 0.50 1 d PD . . C10 C 0.5042(16) 1.0828(13) 0.9089(8) 0.081(9) Uani 0.50 1 d PD . . N2 N 0.4383(14) 1.1571(12) 0.8815(10) 0.067(6) Uani 0.50 1 d PD . . N3 N 0.3647(12) 1.1596(13) 0.9417(10) 0.074(6) Uani 0.50 1 d PD . . C11 C 0.3935(11) 1.0894(12) 0.9959(11) 0.049(5) Uani 0.50 1 d PD . . C12 C 0.3300(13) 1.0643(17) 1.0743(14) 0.064(10) Uani 0.50 1 d PD . . C13 C 0.3373(16) 0.968(2) 1.1086(11) 0.062(10) Uani 0.50 1 d PD . . H13A H 0.3882 0.9160 1.0943 0.075 Uiso 0.50 1 d PR . . C14 C 0.2613(13) 0.9580(16) 1.1661(11) 0.061(6) Uani 0.50 1 d PD . . H14A H 0.2590 0.8940 1.1939 0.073 Uiso 0.50 1 d PR . . N4 N 0.1906(15) 1.0307(18) 1.1858(14) 0.054(8) Uani 0.50 1 d PD . . C15 C 0.1877(16) 1.122(2) 1.1506(10) 0.068(8) Uani 0.50 1 d PD . . H15A H 0.1360 1.1733 1.1659 0.081 Uiso 0.50 1 d PR . . C16 C 0.2596(12) 1.1427(16) 1.0919(9) 0.060(6) Uani 0.50 1 d PD . . H16A H 0.2606 1.2075 1.0651 0.072 Uiso 0.50 1 d PR . . 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 Pb1 0.0356(3) 0.0393(3) 0.0259(2) 0.000 0.00595(16) 0.000 Br1 0.0510(5) 0.0597(7) 0.0431(5) 0.0115(4) 0.0143(4) 0.0097(4) Br2 0.0433(5) 0.0578(7) 0.0382(5) -0.0009(4) 0.0063(3) 0.0195(4) O1 0.051(3) 0.038(4) 0.039(3) 0.008(3) -0.008(3) 0.004(3) O2 0.062(4) 0.030(4) 0.053(4) 0.001(3) 0.000(3) 0.003(3) C1 0.037(4) 0.044(6) 0.029(4) 0.004(4) 0.002(3) 0.013(4) C2 0.035(4) 0.030(5) 0.033(4) -0.004(3) -0.001(3) -0.002(3) C3 0.039(4) 0.037(5) 0.032(4) -0.001(4) 0.005(3) 0.013(4) C4 0.031(4) 0.033(5) 0.027(4) -0.004(3) 0.004(3) 0.007(3) C5 0.063(17) 0.062(16) 0.033(11) -0.016(11) 0.019(11) -0.032(14) C6 0.13(3) 0.07(2) 0.062(19) -0.009(19) 0.008(18) -0.04(2) C7 0.038(11) 0.10(2) 0.024(10) 0.004(12) 0.012(8) -0.023(13) N1 0.078(18) 0.033(11) 0.050(15) -0.012(10) 0.025(12) -0.021(10) C8 0.053(11) 0.058(15) 0.050(11) -0.005(10) 0.028(9) -0.006(10) C9 0.045(9) 0.036(11) 0.055(11) -0.006(9) 0.028(8) -0.007(8) O5 0.060(10) 0.13(2) 0.051(12) -0.042(10) 0.034(9) -0.046(12) C10 0.106(18) 0.09(2) 0.058(13) -0.052(14) 0.065(13) -0.079(16) N2 0.099(14) 0.029(10) 0.085(13) -0.027(10) 0.060(12) -0.017(9) N3 0.065(11) 0.062(13) 0.106(15) -0.036(12) 0.051(11) -0.022(10) C11 0.036(9) 0.059(14) 0.053(11) -0.022(10) 0.015(8) -0.021(9) C12 0.010(8) 0.11(3) 0.077(18) -0.054(18) 0.005(9) -0.013(10) C13 0.06(2) 0.08(2) 0.049(16) -0.043(16) 0.034(14) -0.033(17) C14 0.049(12) 0.084(18) 0.052(13) -0.009(13) 0.010(10) -0.014(12) N4 0.028(10) 0.11(2) 0.027(11) -0.004(12) 0.019(9) -0.001(12) C15 0.039(12) 0.13(3) 0.035(11) -0.012(15) 0.016(9) -0.011(14) C16 0.046(10) 0.096(18) 0.042(10) -0.020(11) 0.018(8) -0.005(11) _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 Pb1 O1 2.304(5) 2_756 ? Pb1 O1 2.304(5) . ? Pb1 N1 2.53(3) . ? Pb1 N1 2.53(3) 2_756 ? Pb1 N4 2.65(2) 5_677 ? Pb1 N4 2.65(2) 6_675 ? Br1 C3 1.884(8) . ? Br2 C4 1.877(7) . ? O1 C1 1.272(10) . ? O2 C1 1.212(10) . ? C1 C2 1.550(11) . ? C2 C4 1.387(10) 7_767 ? C2 C3 1.407(10) . ? C3 C4 1.386(11) . ? C4 C2 1.387(10) 7_767 ? C5 C13 0.66(3) 5_677 ? C5 C6 1.384(10) . ? C5 C9 1.384(10) . ? C5 C10 1.53(3) . ? C5 C14 1.70(3) 5_677 ? C6 C12 0.59(4) 5_677 ? C6 C13 0.94(4) 5_677 ? C6 C7 1.379(10) . ? C6 C16 1.55(3) 5_677 ? C6 C14 1.69(3) 5_677 ? C6 H6A 0.9600 . ? C7 C15 0.95(3) 5_677 ? C7 N4 1.00(4) 5_677 ? C7 N1 1.336(10) . ? C7 C16 1.41(3) 5_677 ? C7 C14 1.49(3) 5_677 ? C7 H7A 0.9599 . ? N1 N4 0.41(3) 5_677 ? N1 C14 1.19(3) 5_677 ? N1 C8 1.336(10) . ? N1 C15 1.74(3) 5_677 ? C8 C14 1.08(3) 5_677 ? C8 C9 1.383(10) . ? C8 N4 1.70(3) 5_677 ? C8 H8A 0.9599 . ? C9 C14 1.38(2) 5_677 ? C9 C13 1.62(3) 5_677 ? C9 H9A 0.9600 . ? O5 O5 1.11(3) 5_677 ? O5 C11 1.366(10) . ? O5 C10 1.374(10) . ? C10 N2 1.288(10) . ? N2 N3 1.392(9) . ? N3 C11 1.290(10) . ? C11 C12 1.60(3) . ? C12 C6 0.59(4) 5_677 ? C12 C16 1.377(10) . ? C12 C13 1.383(10) . ? C13 C5 0.66(3) 5_677 ? C13 C6 0.94(4) 5_677 ? C13 C14 1.383(10) . ? C13 C9 1.62(3) 5_677 ? C13 H13A 0.9600 . ? C14 C8 1.08(3) 5_677 ? C14 N1 1.19(3) 5_677 ? C14 N4 1.334(10) . ? C14 C9 1.38(2) 5_677 ? C14 C7 1.49(3) 5_677 ? C14 C6 1.69(3) 5_677 ? C14 C5 1.70(3) 5_677 ? C14 H14A 0.9600 . ? N4 N1 0.41(3) 5_677 ? N4 C7 1.00(4) 5_677 ? N4 C15 1.337(10) . ? N4 C8 1.70(3) 5_677 ? N4 Pb1 2.65(2) 5_677 ? C15 C7 0.95(3) 5_677 ? C15 C16 1.383(10) . ? C15 N1 1.74(3) 5_677 ? C15 H15A 0.9601 . ? C16 C7 1.41(3) 5_677 ? C16 C6 1.55(3) 5_677 ? C16 H16A 0.9600 . ? 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 O1 Pb1 O1 77.0(3) 2_756 . ? O1 Pb1 N1 82.9(4) 2_756 . ? O1 Pb1 N1 88.6(5) . . ? O1 Pb1 N1 88.6(5) 2_756 2_756 ? O1 Pb1 N1 82.9(4) . 2_756 ? N1 Pb1 N1 169.1(8) . 2_756 ? O1 Pb1 N4 80.3(4) 2_756 5_677 ? O1 Pb1 N4 80.0(5) . 5_677 ? N1 Pb1 N4 8.6(7) . 5_677 ? N1 Pb1 N4 161.3(6) 2_756 5_677 ? O1 Pb1 N4 80.0(5) 2_756 6_675 ? O1 Pb1 N4 80.3(4) . 6_675 ? N1 Pb1 N4 161.3(6) . 6_675 ? N1 Pb1 N4 8.6(7) 2_756 6_675 ? N4 Pb1 N4 154.7(9) 5_677 6_675 ? C1 O1 Pb1 107.2(5) . . ? O2 C1 O1 126.8(8) . . ? O2 C1 C2 119.7(7) . . ? O1 C1 C2 113.5(8) . . ? C4 C2 C3 119.9(7) 7_767 . ? C4 C2 C1 120.2(7) 7_767 . ? C3 C2 C1 119.9(7) . . ? C4 C3 C2 120.2(7) . . ? C4 C3 Br1 121.1(5) . . ? C2 C3 Br1 118.7(6) . . ? C3 C4 C2 119.9(7) . 7_767 ? C3 C4 Br2 121.1(5) . . ? C2 C4 Br2 118.9(6) 7_767 . ? C13 C5 C9 99(3) 5_677 . ? C6 C5 C9 116(2) . . ? C13 C5 C10 131(3) 5_677 . ? C6 C5 C10 128.4(16) . . ? C9 C5 C10 115.5(17) . . ? C13 C5 C14 51(2) 5_677 5_677 ? C6 C5 C14 65.4(18) . 5_677 ? C9 C5 C14 51.8(13) . 5_677 ? C10 C5 C14 161.8(17) . 5_677 ? C13 C5 C12 46(2) 5_677 5_677 ? C9 C5 C12 132.8(19) . 5_677 ? C10 C5 C12 111.7(14) . 5_677 ? C14 C5 C12 82.0(14) 5_677 5_677 ? C12 C6 C13 128(4) 5_677 5_677 ? C12 C6 C7 117(3) 5_677 . ? C13 C6 C7 111(3) 5_677 . ? C12 C6 C5 121(3) 5_677 . ? C7 C6 C5 122(3) . . ? C12 C6 C16 62(3) 5_677 5_677 ? C13 C6 C16 167(2) 5_677 5_677 ? C7 C6 C16 57.1(14) . 5_677 ? C5 C6 C16 164.7(13) . 5_677 ? C12 C6 C14 169(3) 5_677 5_677 ? C13 C6 C14 54.9(18) 5_677 5_677 ? C7 C6 C14 56.8(15) . 5_677 ? C5 C6 C14 66.5(17) . 5_677 ? C16 C6 C14 113.8(14) 5_677 5_677 ? C13 C6 H6A 124.9 5_677 . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 118.6 . . ? C16 C6 H6A 64.5 5_677 . ? C14 C6 H6A 168.0 5_677 . ? C15 C7 N4 86.9(19) 5_677 5_677 ? C15 C7 N1 98.2(19) 5_677 . ? C15 C7 C6 134(3) 5_677 . ? N4 C7 C6 132(3) 5_677 . ? N1 C7 C6 120(3) . . ? C15 C7 C16 69(2) 5_677 5_677 ? N4 C7 C16 154(2) 5_677 5_677 ? N1 C7 C16 161.9(16) . 5_677 ? C6 C7 C16 67.7(16) . 5_677 ? C15 C7 C14 147(2) 5_677 5_677 ? N4 C7 C14 61.3(16) 5_677 5_677 ? N1 C7 C14 49.7(17) . 5_677 ? C6 C7 C14 72.2(18) . 5_677 ? C16 C7 C14 139.6(17) 5_677 5_677 ? C15 C7 C12 119(2) 5_677 5_677 ? N4 C7 C12 149(2) 5_677 5_677 ? N1 C7 C12 138(2) . 5_677 ? C16 C7 C12 50.8(8) 5_677 5_677 ? C14 C7 C12 89.7(15) 5_677 5_677 ? C15 C7 C13 160(2) 5_677 5_677 ? N4 C7 C13 107(2) 5_677 5_677 ? N1 C7 C13 95(2) . 5_677 ? C16 C7 C13 94.8(11) 5_677 5_677 ? C14 C7 C13 45.7(9) 5_677 5_677 ? N4 C7 H7A 108.5 5_677 . ? N1 C7 H7A 119.9 . . ? C6 C7 H7A 119.7 . . ? C16 C7 H7A 54.8 5_677 . ? C14 C7 H7A 163.4 5_677 . ? C12 C7 H7A 102.0 5_677 . ? C13 C7 H7A 143.5 5_677 . ? N4 N1 C14 101(6) 5_677 5_677 ? C14 N1 C7 72(2) 5_677 . ? N4 N1 C8 147(7) 5_677 . ? C14 N1 C8 49.9(16) 5_677 . ? C7 N1 C8 119(3) . . ? C14 N1 C15 103.7(19) 5_677 5_677 ? C8 N1 C15 146(2) . 5_677 ? N4 N1 Pb1 104(6) 5_677 . ? C14 N1 Pb1 141.1(17) 5_677 . ? C7 N1 Pb1 128.9(16) . . ? C8 N1 Pb1 109.1(14) . . ? C15 N1 Pb1 104.5(13) 5_677 . ? C14 C8 N1 58(2) 5_677 . ? C14 C8 C9 67.0(13) 5_677 . ? N1 C8 C9 122(2) . . ? C14 C8 N4 51.9(13) 5_677 5_677 ? C9 C8 N4 115.0(16) . 5_677 ? C14 C8 H8A 162.6 5_677 . ? N1 C8 H8A 118.5 . . ? C9 C8 H8A 119.1 . . ? N4 C8 H8A 125.9 5_677 . ? C14 C9 C8 45.8(11) 5_677 . ? C14 C9 C5 76.1(17) 5_677 . ? C8 C9 C5 120.0(19) . . ? C14 C9 C13 54.2(10) 5_677 5_677 ? C8 C9 C13 99.7(15) . 5_677 ? C14 C9 H9A 159.4 5_677 . ? C8 C9 H9A 120.0 . . ? C5 C9 H9A 120.1 . . ? C13 C9 H9A 138.3 5_677 . ? O5 O5 C11 119.9(18) 5_677 . ? O5 O5 C10 143(2) 5_677 . ? C11 O5 C10 96.7(14) . . ? N2 C10 O5 120.1(17) . . ? N2 C10 C5 126.8(13) . . ? O5 C10 C5 113.1(16) . . ? N2 C10 C13 135.9(12) . 5_677 ? O5 C10 C13 102.2(14) . 5_677 ? C10 N2 N3 99.9(16) . . ? C11 N3 N2 109.6(16) . . ? N3 C11 O5 113.7(15) . . ? N3 C11 C12 126.0(14) . . ? O5 C11 C12 120.3(15) . . ? C6 C12 C16 96(3) 5_677 . ? C16 C12 C13 128(2) . . ? C6 C12 C11 152(3) 5_677 . ? C16 C12 C11 111.5(18) . . ? C13 C12 C11 120.2(15) . . ? C6 C12 C7 45(2) 5_677 5_677 ? C16 C12 C7 52.5(16) . 5_677 ? C13 C12 C7 75.3(19) . 5_677 ? C11 C12 C7 159.4(16) . 5_677 ? C16 C12 C5 136(2) . 5_677 ? C11 C12 C5 111.2(13) . 5_677 ? C7 C12 C5 87.7(16) 5_677 5_677 ? C5 C13 C6 119(4) 5_677 5_677 ? C5 C13 C14 108(3) 5_677 . ? C6 C13 C14 91(3) 5_677 . ? C5 C13 C12 115(3) 5_677 . ? C14 C13 C12 111(2) . . ? C5 C13 C9 58(2) 5_677 5_677 ? C6 C13 C9 131(3) 5_677 5_677 ? C14 C13 C9 54.0(10) . 5_677 ? C12 C13 C9 147.8(16) . 5_677 ? C5 C13 C7 133(4) 5_677 5_677 ? C14 C13 C7 50.3(14) . 5_677 ? C12 C13 C7 60.6(16) . 5_677 ? C9 C13 C7 100.3(12) 5_677 5_677 ? C6 C13 C10 120.1(19) 5_677 5_677 ? C14 C13 C10 138.4(17) . 5_677 ? C12 C13 C10 104.7(12) . 5_677 ? C9 C13 C10 84.4(12) 5_677 5_677 ? C7 C13 C10 158.1(14) 5_677 5_677 ? C5 C13 H13A 50.5 5_677 . ? C6 C13 H13A 143.3 5_677 . ? C14 C13 H13A 125.0 . . ? C12 C13 H13A 124.4 . . ? C9 C13 H13A 77.1 5_677 . ? C7 C13 H13A 173.7 5_677 . ? C8 C14 N1 71.9(14) 5_677 5_677 ? C8 C14 N4 88.7(17) 5_677 . ? C8 C14 C9 67.2(14) 5_677 5_677 ? N1 C14 C9 135.4(19) 5_677 5_677 ? N4 C14 C9 146.9(14) . 5_677 ? C8 C14 C13 138.5(19) 5_677 . ? N1 C14 C13 142(2) 5_677 . ? N4 C14 C13 125(2) . . ? C9 C14 C13 71.8(14) 5_677 . ? C8 C14 C7 127.3(19) 5_677 5_677 ? N1 C14 C7 58.6(12) 5_677 5_677 ? C9 C14 C7 144.0(17) 5_677 5_677 ? C13 C14 C7 84.1(19) . 5_677 ? C8 C14 C6 150.9(18) 5_677 5_677 ? N1 C14 C6 108.3(18) 5_677 5_677 ? N4 C14 C6 91.1(18) . 5_677 ? C9 C14 C6 99.2(12) 5_677 5_677 ? C7 C14 C6 51.0(9) 5_677 5_677 ? C8 C14 C5 117.2(16) 5_677 5_677 ? N1 C14 C5 148(2) 5_677 5_677 ? N4 C14 C5 135(2) . 5_677 ? C9 C14 C5 52.0(8) 5_677 5_677 ? C7 C14 C5 98.4(15) 5_677 5_677 ? C6 C14 C5 48.1(7) 5_677 5_677 ? N1 C14 H14A 100.1 5_677 . ? N4 C14 H14A 117.5 . . ? C9 C14 H14A 55.7 5_677 . ? C13 C14 H14A 117.8 . . ? C7 C14 H14A 157.6 5_677 . ? C6 C14 H14A 151.3 5_677 . ? C5 C14 H14A 104.0 5_677 . ? N1 N4 C7 139(6) 5_677 5_677 ? N1 N4 C14 62(5) 5_677 . ? C7 N4 C14 78(2) 5_677 . ? N1 N4 C15 171(5) 5_677 . ? C7 N4 C15 45(2) 5_677 . ? C14 N4 C15 122(3) . . ? C7 N4 C8 115.1(18) 5_677 5_677 ? C15 N4 C8 152.8(18) . 5_677 ? N1 N4 Pb1 68(6) 5_677 5_677 ? C7 N4 Pb1 145.5(18) 5_677 5_677 ? C14 N4 Pb1 121.3(17) . 5_677 ? C15 N4 Pb1 113.2(12) . 5_677 ? C8 N4 Pb1 92.9(12) 5_677 5_677 ? C7 C15 N4 48(2) 5_677 . ? C7 C15 C16 72(2) 5_677 . ? N4 C15 C16 119(2) . . ? C7 C15 N1 49.3(15) 5_677 5_677 ? C16 C15 N1 120(2) . 5_677 ? C7 C15 H15A 165.1 5_677 . ? N4 C15 H15A 120.2 . . ? C16 C15 H15A 120.6 . . ? N1 C15 H15A 119.4 5_677 . ? C12 C16 C15 116(2) . . ? C12 C16 C7 76.7(18) . 5_677 ? C15 C16 C6 93.7(18) . 5_677 ? C7 C16 C6 55.2(12) 5_677 5_677 ? C12 C16 H16A 122.0 . . ? C15 C16 H16A 122.2 . . ? C7 C16 H16A 160.6 5_677 . ? C6 C16 H16A 144.0 5_677 . ? 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 O1 Pb1 O1 C1 164.4(6) 2_756 . . . ? N1 Pb1 O1 C1 -112.5(6) . . . . ? N1 Pb1 O1 C1 74.3(6) 2_756 . . . ? N4 Pb1 O1 C1 -113.3(6) 5_677 . . . ? N4 Pb1 O1 C1 82.6(7) 6_675 . . . ? Pb1 O1 C1 O2 3.4(10) . . . . ? Pb1 O1 C1 C2 -176.7(5) . . . . ? O2 C1 C2 C4 92.2(10) . . . 7_767 ? O1 C1 C2 C4 -87.7(9) . . . 7_767 ? O2 C1 C2 C3 -86.4(10) . . . . ? O1 C1 C2 C3 93.7(9) . . . . ? C4 C2 C3 C4 0.8(13) 7_767 . . . ? C1 C2 C3 C4 179.4(7) . . . . ? C4 C2 C3 Br1 -179.6(6) 7_767 . . . ? C1 C2 C3 Br1 -1.0(10) . . . . ? C2 C3 C4 C2 -0.8(13) . . . 7_767 ? Br1 C3 C4 C2 179.6(6) . . . 7_767 ? C2 C3 C4 Br2 177.0(6) . . . . ? Br1 C3 C4 Br2 -2.6(10) . . . . ? C13 C5 C6 C12 114(7) 5_677 . . 5_677 ? C9 C5 C6 C12 -178(4) . . . 5_677 ? C10 C5 C6 C12 5(3) . . . 5_677 ? C14 C5 C6 C12 171(4) 5_677 . . 5_677 ? C9 C5 C6 C13 68(4) . . . 5_677 ? C10 C5 C6 C13 -110(5) . . . 5_677 ? C14 C5 C6 C13 56(4) 5_677 . . 5_677 ? C12 C5 C6 C13 -114(7) 5_677 . . 5_677 ? C13 C5 C6 C7 -68(4) 5_677 . . . ? C9 C5 C6 C7 -0.1(3) . . . . ? C10 C5 C6 C7 -177.8(18) . . . . ? C14 C5 C6 C7 -11.8(8) 5_677 . . . ? C12 C5 C6 C7 178(4) 5_677 . . . ? C13 C5 C6 C16 -150(9) 5_677 . . 5_677 ? C9 C5 C6 C16 -83(8) . . . 5_677 ? C10 C5 C6 C16 100(8) . . . 5_677 ? C14 C5 C6 C16 -94(8) 5_677 . . 5_677 ? C12 C5 C6 C16 95(9) 5_677 . . 5_677 ? C13 C5 C6 C14 -56(4) 5_677 . . 5_677 ? C9 C5 C6 C14 11.7(8) . . . 5_677 ? C10 C5 C6 C14 -166.0(19) . . . 5_677 ? C12 C5 C6 C14 -171(4) 5_677 . . 5_677 ? C12 C6 C7 C15 35(5) 5_677 . . 5_677 ? C13 C6 C7 C15 -167(3) 5_677 . . 5_677 ? C5 C6 C7 C15 -143(3) . . . 5_677 ? C16 C6 C7 C15 19(3) 5_677 . . 5_677 ? C14 C6 C7 C15 -156(4) 5_677 . . 5_677 ? C12 C6 C7 N4 174(4) 5_677 . . 5_677 ? C13 C6 C7 N4 -28(3) 5_677 . . 5_677 ? C5 C6 C7 N4 -3(2) . . . 5_677 ? C16 C6 C7 N4 158(3) 5_677 . . 5_677 ? C14 C6 C7 N4 -16(2) 5_677 . . 5_677 ? C12 C6 C7 N1 178(4) 5_677 . . . ? C13 C6 C7 N1 -24.1(19) 5_677 . . . ? C5 C6 C7 N1 0.1(3) . . . . ? C16 C6 C7 N1 162.0(15) 5_677 . . . ? C14 C6 C7 N1 -12.8(9) 5_677 . . . ? C12 C6 C7 C16 16(3) 5_677 . . 5_677 ? C13 C6 C7 C16 174(3) 5_677 . . 5_677 ? C5 C6 C7 C16 -161.8(15) . . . 5_677 ? C14 C6 C7 C16 -174.7(18) 5_677 . . 5_677 ? C12 C6 C7 C14 -169(4) 5_677 . . 5_677 ? C13 C6 C7 C14 -11.4(18) 5_677 . . 5_677 ? C5 C6 C7 C14 12.9(9) . . . 5_677 ? C16 C6 C7 C14 174.7(18) 5_677 . . 5_677 ? C13 C6 C7 C12 158(5) 5_677 . . 5_677 ? C5 C6 C7 C12 -178(4) . . . 5_677 ? C16 C6 C7 C12 -16(3) 5_677 . . 5_677 ? C14 C6 C7 C12 169(4) 5_677 . . 5_677 ? C12 C6 C7 C13 -158(5) 5_677 . . 5_677 ? C5 C6 C7 C13 24.3(19) . . . 5_677 ? C16 C6 C7 C13 -174(3) 5_677 . . 5_677 ? C14 C6 C7 C13 11.4(18) 5_677 . . 5_677 ? C15 C7 N1 N4 -13(8) 5_677 . . 5_677 ? C6 C7 N1 N4 -167(9) . . . 5_677 ? C16 C7 N1 N4 -54(11) 5_677 . . 5_677 ? C14 C7 N1 N4 177(10) 5_677 . . 5_677 ? C12 C7 N1 N4 -166(9) 5_677 . . 5_677 ? C13 C7 N1 N4 -178(9) 5_677 . . 5_677 ? C15 C7 N1 C14 170(3) 5_677 . . 5_677 ? N4 C7 N1 C14 -177(10) 5_677 . . 5_677 ? C6 C7 N1 C14 16.0(12) . . . 5_677 ? C16 C7 N1 C14 128(7) 5_677 . . 5_677 ? C12 C7 N1 C14 17(2) 5_677 . . 5_677 ? C13 C7 N1 C14 5.2(11) 5_677 . . 5_677 ? C15 C7 N1 C8 154(2) 5_677 . . . ? N4 C7 N1 C8 166(9) 5_677 . . . ? C6 C7 N1 C8 -0.4(7) . . . . ? C16 C7 N1 C8 112(7) 5_677 . . . ? C14 C7 N1 C8 -16.4(11) 5_677 . . . ? C12 C7 N1 C8 1(2) 5_677 . . . ? C13 C7 N1 C8 -11.2(10) 5_677 . . . ? N4 C7 N1 C15 13(8) 5_677 . . 5_677 ? C6 C7 N1 C15 -154(2) . . . 5_677 ? C16 C7 N1 C15 -42(6) 5_677 . . 5_677 ? C14 C7 N1 C15 -170(3) 5_677 . . 5_677 ? C12 C7 N1 C15 -153(3) 5_677 . . 5_677 ? C13 C7 N1 C15 -165(2) 5_677 . . 5_677 ? C15 C7 N1 Pb1 -47.9(18) 5_677 . . . ? N4 C7 N1 Pb1 -35(9) 5_677 . . . ? C6 C7 N1 Pb1 157.8(14) . . . . ? C16 C7 N1 Pb1 -90(7) 5_677 . . . ? C14 C7 N1 Pb1 142(2) 5_677 . . . ? C12 C7 N1 Pb1 158.8(16) 5_677 . . . ? C13 C7 N1 Pb1 147.0(13) 5_677 . . . ? O1 Pb1 N1 N4 72(5) 2_756 . . 5_677 ? O1 Pb1 N1 N4 -5(5) . . . 5_677 ? N1 Pb1 N1 N4 33(5) 2_756 . . 5_677 ? N4 Pb1 N1 N4 48(7) 6_675 . . 5_677 ? O1 Pb1 N1 C14 -160(3) 2_756 . . 5_677 ? O1 Pb1 N1 C14 123(3) . . . 5_677 ? N1 Pb1 N1 C14 161(3) 2_756 . . 5_677 ? N4 Pb1 N1 C14 128(6) 5_677 . . 5_677 ? N4 Pb1 N1 C14 176.2(17) 6_675 . . 5_677 ? O1 Pb1 N1 C7 89.0(14) 2_756 . . . ? O1 Pb1 N1 C7 12.0(14) . . . . ? N1 Pb1 N1 C7 50.3(14) 2_756 . . . ? N4 Pb1 N1 C7 17(4) 5_677 . . . ? N4 Pb1 N1 C7 65(3) 6_675 . . . ? O1 Pb1 N1 C8 -111.0(8) 2_756 . . . ? O1 Pb1 N1 C8 171.9(8) . . . . ? N1 Pb1 N1 C8 -149.7(8) 2_756 . . . ? N4 Pb1 N1 C8 177(5) 5_677 . . . ? N4 Pb1 N1 C8 -134.8(18) 6_675 . . . ? O1 Pb1 N1 C15 64.8(11) 2_756 . . 5_677 ? O1 Pb1 N1 C15 -12.3(12) . . . 5_677 ? N1 Pb1 N1 C15 26.1(11) 2_756 . . 5_677 ? N4 Pb1 N1 C15 -7(4) 5_677 . . 5_677 ? N4 Pb1 N1 C15 41(3) 6_675 . . 5_677 ? N4 N1 C8 C14 33(8) 5_677 . . 5_677 ? C7 N1 C8 C14 20.5(14) . . . 5_677 ? C15 N1 C8 C14 46(3) 5_677 . . 5_677 ? Pb1 N1 C8 C14 -142(2) . . . 5_677 ? N4 N1 C8 C9 13(9) 5_677 . . . ? C14 N1 C8 C9 -19.9(15) 5_677 . . . ? C7 N1 C8 C9 0.6(9) . . . . ? C15 N1 C8 C9 26(3) 5_677 . . . ? Pb1 N1 C8 C9 -161.6(11) . . . . ? C14 N1 C8 N4 -33(8) 5_677 . . 5_677 ? C7 N1 C8 N4 -12(8) . . . 5_677 ? C15 N1 C8 N4 13(7) 5_677 . . 5_677 ? Pb1 N1 C8 N4 -174(9) . . . 5_677 ? N1 C8 C9 C14 18.3(15) . . . 5_677 ? N4 C8 C9 C14 20.2(11) 5_677 . . 5_677 ? C14 C8 C9 C5 -18.9(15) 5_677 . . . ? N1 C8 C9 C5 -0.5(9) . . . . ? N4 C8 C9 C5 1.3(13) 5_677 . . . ? C14 C8 C9 C13 -5.7(15) 5_677 . . 5_677 ? N1 C8 C9 C13 12.6(13) . . . 5_677 ? N4 C8 C9 C13 14.5(18) 5_677 . . 5_677 ? C13 C5 C9 C14 20(3) 5_677 . . 5_677 ? C6 C5 C9 C14 -13.6(10) . . . 5_677 ? C10 C5 C9 C14 164.5(18) . . . 5_677 ? C12 C5 C9 C14 -14.5(19) 5_677 . . 5_677 ? C13 C5 C9 C8 34(4) 5_677 . . . ? C6 C5 C9 C8 0.2(7) . . . . ? C10 C5 C9 C8 178.3(16) . . . . ? C14 C5 C9 C8 13.8(10) 5_677 . . . ? C12 C5 C9 C8 -0.7(18) 5_677 . . . ? C6 C5 C9 C13 -34(3) . . . 5_677 ? C10 C5 C9 C13 144(5) . . . 5_677 ? C14 C5 C9 C13 -20(3) 5_677 . . 5_677 ? C12 C5 C9 C13 -35(3) 5_677 . . 5_677 ? O5 O5 C10 N2 173(3) 5_677 . . . ? C11 O5 C10 N2 -0.1(3) . . . . ? O5 O5 C10 C5 -11(3) 5_677 . . . ? C11 O5 C10 C5 176.3(14) . . . . ? O5 O5 C10 C13 -20(3) 5_677 . . 5_677 ? C11 O5 C10 C13 166.8(11) . . . 5_677 ? C13 C5 C10 N2 135(4) 5_677 . . . ? C6 C5 C10 N2 -177.4(10) . . . . ? C9 C5 C10 N2 5(2) . . . . ? C14 C5 C10 N2 47(5) 5_677 . . . ? C12 C5 C10 N2 -176.0(12) 5_677 . . . ? C13 C5 C10 O5 -41(5) 5_677 . . . ? C6 C5 C10 O5 6.4(16) . . . . ? C9 C5 C10 O5 -171.3(10) . . . . ? C14 C5 C10 O5 -129(5) 5_677 . . . ? C12 C5 C10 O5 7.9(18) 5_677 . . . ? C6 C5 C10 C13 48(4) . . . 5_677 ? C9 C5 C10 C13 -130(5) . . . 5_677 ? C14 C5 C10 C13 -88(7) 5_677 . . 5_677 ? C12 C5 C10 C13 49(4) 5_677 . . 5_677 ? O5 C10 N2 N3 0.2(5) . . . . ? C5 C10 N2 N3 -175.7(16) . . . . ? C13 C10 N2 N3 -161.3(16) 5_677 . . . ? C10 N2 N3 C11 -0.2(5) . . . . ? N2 N3 C11 O5 0.1(5) . . . . ? N2 N3 C11 C12 -178.7(14) . . . . ? O5 O5 C11 N3 -175(2) 5_677 . . . ? C10 O5 C11 N3 0.0(3) . . . . ? O5 O5 C11 C12 4(2) 5_677 . . . ? C10 O5 C11 C12 178.8(13) . . . . ? N3 C11 C12 C6 160(7) . . . 5_677 ? O5 C11 C12 C6 -19(7) . . . 5_677 ? N3 C11 C12 C16 -16.6(15) . . . . ? O5 C11 C12 C16 164.7(10) . . . . ? N3 C11 C12 C13 154.9(10) . . . . ? O5 C11 C12 C13 -23.8(15) . . . . ? N3 C11 C12 C7 20(5) . . . 5_677 ? O5 C11 C12 C7 -159(4) . . . 5_677 ? N3 C11 C12 C5 174.7(12) . . . 5_677 ? O5 C11 C12 C5 -4.0(18) . . . 5_677 ? C6 C12 C13 C5 -108(7) 5_677 . . 5_677 ? C16 C12 C13 C5 -122(4) . . . 5_677 ? C11 C12 C13 C5 68(4) . . . 5_677 ? C7 C12 C13 C5 -127(4) 5_677 . . 5_677 ? C16 C12 C13 C6 -14(4) . . . 5_677 ? C11 C12 C13 C6 176(5) . . . 5_677 ? C7 C12 C13 C6 -19(4) 5_677 . . 5_677 ? C5 C12 C13 C6 108(7) 5_677 . . 5_677 ? C6 C12 C13 C14 14(4) 5_677 . . . ? C16 C12 C13 C14 0.1(3) . . . . ? C11 C12 C13 C14 -169.9(13) . . . . ? C7 C12 C13 C14 -4.7(8) 5_677 . . . ? C5 C12 C13 C14 122(4) 5_677 . . . ? C6 C12 C13 C9 -40(5) 5_677 . . 5_677 ? C16 C12 C13 C9 -54(3) . . . 5_677 ? C11 C12 C13 C9 136(3) . . . 5_677 ? C7 C12 C13 C9 -59(3) 5_677 . . 5_677 ? C5 C12 C13 C9 68(3) 5_677 . . 5_677 ? C6 C12 C13 C7 19(4) 5_677 . . 5_677 ? C16 C12 C13 C7 4.9(8) . . . 5_677 ? C11 C12 C13 C7 -165.2(15) . . . 5_677 ? C5 C12 C13 C7 127(4) 5_677 . . 5_677 ? C6 C12 C13 C10 -143(5) 5_677 . . 5_677 ? C16 C12 C13 C10 -157.5(12) . . . 5_677 ? C11 C12 C13 C10 32.4(11) . . . 5_677 ? C7 C12 C13 C10 -162.4(13) 5_677 . . 5_677 ? C5 C12 C13 C10 -35(3) 5_677 . . 5_677 ? C5 C13 C14 C8 -12(6) 5_677 . . 5_677 ? C6 C13 C14 C8 -133(3) 5_677 . . 5_677 ? C12 C13 C14 C8 -138(3) . . . 5_677 ? C9 C13 C14 C8 10(3) 5_677 . . 5_677 ? C7 C13 C14 C8 -143(4) 5_677 . . 5_677 ? C10 C13 C14 C8 8(5) 5_677 . . 5_677 ? C5 C13 C14 N1 121(4) 5_677 . . 5_677 ? C6 C13 C14 N1 0(3) 5_677 . . 5_677 ? C12 C13 C14 N1 -5(3) . . . 5_677 ? C9 C13 C14 N1 143(3) 5_677 . . 5_677 ? C7 C13 C14 N1 -10(2) 5_677 . . 5_677 ? C10 C13 C14 N1 142(3) 5_677 . . 5_677 ? C5 C13 C14 N4 126(4) 5_677 . . . ? C6 C13 C14 N4 4.9(16) 5_677 . . . ? C12 C13 C14 N4 0.1(3) . . . . ? C9 C13 C14 N4 147.7(13) 5_677 . . . ? C7 C13 C14 N4 -5.2(10) 5_677 . . . ? C10 C13 C14 N4 146(2) 5_677 . . . ? C5 C13 C14 C9 -21(4) 5_677 . . 5_677 ? C6 C13 C14 C9 -143(2) 5_677 . . 5_677 ? C12 C13 C14 C9 -147.5(13) . . . 5_677 ? C7 C13 C14 C9 -152.9(16) 5_677 . . 5_677 ? C10 C13 C14 C9 -1(2) 5_677 . . 5_677 ? C5 C13 C14 C7 131(4) 5_677 . . 5_677 ? C6 C13 C14 C7 10.1(15) 5_677 . . 5_677 ? C12 C13 C14 C7 5.4(9) . . . 5_677 ? C9 C13 C14 C7 152.9(16) 5_677 . . 5_677 ? C10 C13 C14 C7 152(2) 5_677 . . 5_677 ? C5 C13 C14 C6 121(5) 5_677 . . 5_677 ? C12 C13 C14 C6 -4.8(16) . . . 5_677 ? C9 C13 C14 C6 143(2) 5_677 . . 5_677 ? C7 C13 C14 C6 -10.1(15) 5_677 . . 5_677 ? C10 C13 C14 C6 142(3) 5_677 . . 5_677 ? C6 C13 C14 C5 -121(5) 5_677 . . 5_677 ? C12 C13 C14 C5 -126(4) . . . 5_677 ? C9 C13 C14 C5 21(4) 5_677 . . 5_677 ? C7 C13 C14 C5 -131(4) 5_677 . . 5_677 ? C10 C13 C14 C5 20(3) 5_677 . . 5_677 ? C8 C14 N4 N1 -17(4) 5_677 . . 5_677 ? C9 C14 N4 N1 -59(6) 5_677 . . 5_677 ? C13 C14 N4 N1 -170(5) . . . 5_677 ? C7 C14 N4 N1 -178(7) 5_677 . . 5_677 ? C6 C14 N4 N1 -167(5) 5_677 . . 5_677 ? C5 C14 N4 N1 -145(5) 5_677 . . 5_677 ? C8 C14 N4 C7 162(3) 5_677 . . 5_677 ? N1 C14 N4 C7 178(7) 5_677 . . 5_677 ? C9 C14 N4 C7 120(4) 5_677 . . 5_677 ? C13 C14 N4 C7 8.0(15) . . . 5_677 ? C6 C14 N4 C7 10.7(13) 5_677 . . 5_677 ? C5 C14 N4 C7 33(2) 5_677 . . 5_677 ? C8 C14 N4 C15 153.4(18) 5_677 . . . ? N1 C14 N4 C15 170(6) 5_677 . . . ? C9 C14 N4 C15 111(4) 5_677 . . . ? C13 C14 N4 C15 -0.3(7) . . . . ? C7 C14 N4 C15 -8.3(14) 5_677 . . . ? C6 C14 N4 C15 2.4(11) 5_677 . . . ? C5 C14 N4 C15 25(2) 5_677 . . . ? N1 C14 N4 C8 17(4) 5_677 . . 5_677 ? C9 C14 N4 C8 -42(3) 5_677 . . 5_677 ? C13 C14 N4 C8 -153.6(18) . . . 5_677 ? C7 C14 N4 C8 -162(3) 5_677 . . 5_677 ? C6 C14 N4 C8 -150.9(18) 5_677 . . 5_677 ? C5 C14 N4 C8 -129(2) 5_677 . . 5_677 ? C8 C14 N4 Pb1 -49.6(13) 5_677 . . 5_677 ? N1 C14 N4 Pb1 -33(5) 5_677 . . 5_677 ? C9 C14 N4 Pb1 -92(3) 5_677 . . 5_677 ? C13 C14 N4 Pb1 156.7(12) . . . 5_677 ? C7 C14 N4 Pb1 149(2) 5_677 . . 5_677 ? C6 C14 N4 Pb1 159.4(12) 5_677 . . 5_677 ? C5 C14 N4 Pb1 -178.5(15) 5_677 . . 5_677 ? C14 N4 C15 C7 11.5(19) . . . 5_677 ? C8 N4 C15 C7 50(3) 5_677 . . 5_677 ? Pb1 N4 C15 C7 -147(3) 5_677 . . 5_677 ? C7 N4 C15 C16 -11.3(19) 5_677 . . . ? C14 N4 C15 C16 0.2(9) . . . . ? C8 N4 C15 C16 39(3) 5_677 . . . ? Pb1 N4 C15 C16 -158.5(11) 5_677 . . . ? C6 C12 C16 C15 -8(3) 5_677 . . . ? C13 C12 C16 C15 -0.2(6) . . . . ? C11 C12 C16 C15 170.6(13) . . . . ? C7 C12 C16 C15 5.7(11) 5_677 . . . ? C5 C12 C16 C15 -24.6(18) 5_677 . . . ? C6 C12 C16 C7 -13(2) 5_677 . . 5_677 ? C13 C12 C16 C7 -5.9(10) . . . 5_677 ? C11 C12 C16 C7 164.8(15) . . . 5_677 ? C5 C12 C16 C7 -30(2) 5_677 . . 5_677 ? C13 C12 C16 C6 8(3) . . . 5_677 ? C11 C12 C16 C6 178(3) . . . 5_677 ? C7 C12 C16 C6 13(2) 5_677 . . 5_677 ? C5 C12 C16 C6 -16.8(19) 5_677 . . 5_677 ? C7 C15 C16 C12 -8.8(16) 5_677 . . . ? N4 C15 C16 C12 0.0(8) . . . . ? N1 C15 C16 C12 2.4(14) 5_677 . . . ? N4 C15 C16 C7 8.8(15) . . . 5_677 ? N1 C15 C16 C7 11.2(12) 5_677 . . 5_677 ? C7 C15 C16 C6 -11.7(15) 5_677 . . 5_677 ? N4 C15 C16 C6 -2.9(11) . . . 5_677 ? N1 C15 C16 C6 -0.5(18) 5_677 . . 5_677 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.625 _refine_diff_density_min -1.499 _refine_diff_density_rms 0.170 #===END