Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Molecular tectonics: generation and packing of 1- D coordination networks formed between dibromofluorene based tectons bearing two pyridines and metal halides ; _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR loop_ _publ_author_name 'Mir Wais Hosseini' 'Abdelaziz Jouaiti' 'Nathalie Krytsakas' 'Jean-March Planeix' # Attachment 'New CIF for 4-CdBr2.cif' data_e460a _database_code_depnum_ccdc_archive 'CCDC 617743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br4 Cd N2 O4, 3(C H Cl3)' _chemical_formula_sum 'C40 H25 Br4 Cd Cl9 N2 O4' _chemical_formula_weight 1348.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1433(4) _cell_length_b 16.1077(6) _cell_length_c 17.4365(7) _cell_angle_alpha 114.815(2) _cell_angle_beta 91.345(2) _cell_angle_gamma 92.087(2) _cell_volume 2327.22(16) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5397 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.34 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 4.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8417 _exptl_absorpt_correction_T_max 0.9567 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24597 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.1114 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.43 _reflns_number_total 10522 _reflns_number_gt 6563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^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 10522 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 -0.43451(4) 0.72936(3) 0.97850(2) 0.02199(11) Uani 1 1 d . . . Br4 Br -0.54329(7) 0.65207(4) 1.06550(4) 0.03561(17) Uani 1 1 d . . . Br3 Br -0.56636(7) 0.79245(4) 0.88766(4) 0.03471(17) Uani 1 1 d . . . N1 N -0.2917(5) 0.6198(3) 0.8896(3) 0.0218(7) Uani 1 1 d . . . C1 C -0.2928(6) 0.5386(3) 0.8938(3) 0.0218(7) Uani 1 1 d . . . H1 H -0.3469 0.5312 0.9351 0.026 Uiso 1 1 calc R . . C2 C -0.2183(7) 0.4660(4) 0.8402(4) 0.0377(16) Uani 1 1 d . . . H2 H -0.2214 0.4109 0.8455 0.045 Uiso 1 1 calc R . . C3 C -0.1382(7) 0.4762(4) 0.7780(4) 0.0290(14) Uani 1 1 d . . . H3 H -0.0883 0.4276 0.7400 0.035 Uiso 1 1 calc R . . C4 C -0.1342(6) 0.5589(3) 0.7739(3) 0.0190(12) Uani 1 1 d . . . C5 C -0.2136(6) 0.6287(4) 0.8300(3) 0.0218(7) Uani 1 1 d . . . H5 H -0.2121 0.6844 0.8257 0.026 Uiso 1 1 calc R . . C6 C -0.0448(6) 0.5704(4) 0.7073(3) 0.0249(13) Uani 1 1 d . . . O1 O 0.0042(5) 0.5080(3) 0.6494(2) 0.0335(10) Uani 1 1 d . . . O2 O -0.0274(4) 0.6595(2) 0.7224(2) 0.0261(9) Uani 1 1 d . . . C7 C 0.0534(6) 0.6828(3) 0.6651(3) 0.0220(12) Uani 1 1 d . . . C8 C 0.0084(6) 0.6507(4) 0.5811(3) 0.0255(13) Uani 1 1 d . . . H8 H -0.0721 0.6096 0.5594 0.031 Uiso 1 1 calc R . . C9 C 0.0857(6) 0.6811(3) 0.5303(3) 0.0185(6) Uani 1 1 d . . . H9 H 0.0567 0.6598 0.4735 0.022 Uiso 1 1 calc R . . C10 C 0.2069(6) 0.7433(3) 0.5618(3) 0.0185(6) Uani 1 1 d . . . C11 C 0.2499(6) 0.7728(3) 0.6461(3) 0.0185(6) Uani 1 1 d . . . H11 H 0.3313 0.8131 0.6681 0.022 Uiso 1 1 calc R . . C12 C 0.1726(6) 0.7430(3) 0.6980(3) 0.0228(13) Uani 1 1 d . . . H12 H 0.2013 0.7636 0.7548 0.027 Uiso 1 1 calc R . . C13 C 0.2977(6) 0.7678(3) 0.5016(3) 0.0185(6) Uani 1 1 d . . . C14 C 0.4138(6) 0.6956(3) 0.4647(3) 0.0189(12) Uani 1 1 d . . . C15 C 0.3901(6) 0.6009(4) 0.4252(3) 0.0251(13) Uani 1 1 d . . . H15 H 0.2959 0.5737 0.4136 0.030 Uiso 1 1 calc R . . C16 C 0.5125(7) 0.5487(4) 0.4037(3) 0.0290(14) Uani 1 1 d . . . Br1 Br 0.48497(8) 0.41905(4) 0.35144(4) 0.0481(2) Uani 1 1 d . . . C17 C 0.6547(7) 0.5875(4) 0.4189(3) 0.0324(15) Uani 1 1 d . . . H17 H 0.7343 0.5505 0.4026 0.039 Uiso 1 1 calc R . . C18 C 0.6759(6) 0.6818(4) 0.4587(3) 0.0290(14) Uani 1 1 d . . . H18 H 0.7700 0.7090 0.4698 0.035 Uiso 1 1 calc R . . C19 C 0.5542(6) 0.7354(4) 0.4819(3) 0.0212(12) Uani 1 1 d . . . C20 C 0.5456(6) 0.8357(4) 0.5288(3) 0.0212(12) Uani 1 1 d . . . C21 C 0.6542(6) 0.9060(3) 0.5578(3) 0.0206(5) Uani 1 1 d . . . H21 H 0.7520 0.8926 0.5480 0.025 Uiso 1 1 calc R . . C22 C 0.6161(6) 0.9959(4) 0.6013(3) 0.0259(13) Uani 1 1 d . . . H22 H 0.6876 1.0434 0.6198 0.031 Uiso 1 1 calc R . . C23 C 0.4699(6) 1.0140(4) 0.6169(3) 0.0235(13) Uani 1 1 d . . . C24 C 0.3589(6) 0.9440(3) 0.5874(3) 0.0206(5) Uani 1 1 d . . . H24 H 0.2611 0.9573 0.5973 0.025 Uiso 1 1 calc R . . Br2 Br 0.41879(7) 1.13654(4) 0.67962(4) 0.03407(17) Uani 1 1 d . . . C25 C 0.3987(6) 0.8550(3) 0.5434(3) 0.0179(12) Uani 1 1 d . . . C26 C 0.2029(6) 0.7812(3) 1.4334(3) 0.0206(5) Uani 1 1 d . . . C27 C 0.2452(6) 0.7533(3) 1.3515(3) 0.0206(5) Uani 1 1 d . . . H27 H 0.3284 0.7198 1.3345 0.025 Uiso 1 1 calc R . . C28 C 0.1653(6) 0.7744(3) 1.2939(3) 0.0206(5) Uani 1 1 d . . . H28 H 0.1960 0.7567 1.2390 0.025 Uiso 1 1 calc R . . C29 C 0.0404(6) 0.8218(4) 1.3190(3) 0.0222(12) Uani 1 1 d . . . C30 C -0.0054(6) 0.8499(4) 1.3998(4) 0.0268(13) Uani 1 1 d . . . H30 H -0.0902 0.8821 1.4159 0.032 Uiso 1 1 calc R . . C31 C 0.0754(6) 0.8301(4) 1.4570(3) 0.0249(13) Uani 1 1 d . . . H31 H 0.0450 0.8495 1.5121 0.030 Uiso 1 1 calc R . . O3 O -0.0449(4) 0.8369(2) 1.2574(2) 0.0248(9) Uani 1 1 d . . . C32 C -0.0483(6) 0.9234(4) 1.2650(3) 0.0247(13) Uani 1 1 d . . . O4 O 0.0176(5) 0.9884(3) 1.3185(3) 0.0425(12) Uani 1 1 d . . . C33 C -0.1417(6) 0.9273(4) 1.1949(3) 0.0238(7) Uani 1 1 d . . . C34 C -0.2241(6) 0.8520(4) 1.1374(3) 0.0238(7) Uani 1 1 d . . . H34 H -0.2237 0.7974 1.1436 0.029 Uiso 1 1 calc R . . N2 N -0.3041(5) 0.8547(3) 1.0732(3) 0.0197(10) Uani 1 1 d . . . C35 C -0.3058(6) 0.9339(4) 1.0658(4) 0.0275(14) Uani 1 1 d . . . H35 H -0.3610 0.9362 1.0213 0.033 Uiso 1 1 calc R . . C36 C -0.2290(6) 1.0128(4) 1.1214(3) 0.0238(7) Uani 1 1 d . . . H36 H -0.2337 1.0669 1.1146 0.029 Uiso 1 1 calc R . . C37 C -0.1444(6) 1.0097(4) 1.1877(4) 0.0271(13) Uani 1 1 d . . . H37 H -0.0913 1.0615 1.2260 0.032 Uiso 1 1 calc R . . C38 C 0.8636(7) 0.2317(4) 0.9858(4) 0.0439(18) Uani 1 1 d . . . H38 H 0.7877 0.2655 1.0236 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.9713(2) 0.30865(13) 0.96224(13) 0.0573(5) Uani 1 1 d . . . Cl2 Cl 0.7775(2) 0.14707(12) 0.89365(12) 0.0565(5) Uani 1 1 d . . . Cl3 Cl 0.9706(2) 0.18094(17) 1.03823(15) 0.0711(6) Uani 1 1 d . . . C39 C 0.2767(8) 0.1053(6) 0.2358(5) 0.066(2) Uani 1 1 d . . . H39 H 0.2120 0.0728 0.2593 0.079 Uiso 1 1 calc R . . Cl4 Cl 0.2944(3) 0.21389(15) 0.31103(14) 0.0859(8) Uani 1 1 d . . . Cl5 Cl 0.1846(2) 0.09554(15) 0.14274(13) 0.0611(6) Uani 1 1 d . . . Cl6 Cl 0.4359(2) 0.04753(12) 0.21623(11) 0.0511(5) Uani 1 1 d . . . C40 C 0.7116(8) 0.5455(4) 0.1534(4) 0.0443(18) Uani 1 1 d . . . H40 H 0.6186 0.5475 0.1253 0.053 Uiso 1 1 calc R . . Cl7 Cl 0.7044(2) 0.44965(12) 0.17616(12) 0.0594(6) Uani 1 1 d . . . Cl8 Cl 0.8542(3) 0.5384(2) 0.08580(16) 0.0881(8) Uani 1 1 d . . . Cl9 Cl 0.7383(4) 0.64516(15) 0.24553(15) 0.1203(12) 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 0.0244(3) 0.0238(2) 0.0226(2) 0.01447(16) 0.00129(16) 0.00242(17) Br4 0.0369(4) 0.0393(4) 0.0454(4) 0.0313(3) 0.0147(3) 0.0065(3) Br3 0.0337(4) 0.0416(4) 0.0398(3) 0.0283(3) -0.0081(3) 0.0023(3) N1 0.0211(17) 0.0249(14) 0.0254(15) 0.0166(12) 0.0013(12) -0.0010(13) C1 0.0211(17) 0.0249(14) 0.0254(15) 0.0166(12) 0.0013(12) -0.0010(13) C2 0.051(4) 0.020(3) 0.048(4) 0.018(3) 0.015(3) 0.005(3) C3 0.035(4) 0.024(3) 0.031(3) 0.013(3) 0.014(3) 0.008(3) C4 0.021(3) 0.022(3) 0.018(3) 0.012(2) 0.001(2) 0.000(2) C5 0.0211(17) 0.0249(14) 0.0254(15) 0.0166(12) 0.0013(12) -0.0010(13) C6 0.019(3) 0.031(3) 0.026(3) 0.014(3) -0.004(2) -0.003(3) O1 0.043(3) 0.027(2) 0.031(2) 0.0119(19) 0.0150(19) 0.0052(19) O2 0.035(2) 0.023(2) 0.024(2) 0.0139(16) 0.0087(17) -0.0005(18) C7 0.027(3) 0.019(3) 0.020(3) 0.008(2) 0.003(2) 0.000(2) C8 0.020(3) 0.028(3) 0.027(3) 0.012(2) -0.004(2) -0.005(2) C9 0.0152(15) 0.0225(14) 0.0200(13) 0.0112(11) -0.0008(11) 0.0025(11) C10 0.0152(15) 0.0225(14) 0.0200(13) 0.0112(11) -0.0008(11) 0.0025(11) C11 0.0152(15) 0.0225(14) 0.0200(13) 0.0112(11) -0.0008(11) 0.0025(11) C12 0.028(3) 0.026(3) 0.015(2) 0.009(2) -0.002(2) 0.000(2) C13 0.0152(15) 0.0225(14) 0.0200(13) 0.0112(11) -0.0008(11) 0.0025(11) C14 0.018(3) 0.023(3) 0.017(2) 0.010(2) 0.002(2) 0.003(2) C15 0.021(3) 0.030(3) 0.025(3) 0.012(2) -0.002(2) 0.003(3) C16 0.037(4) 0.025(3) 0.026(3) 0.011(2) 0.005(3) 0.008(3) Br1 0.0594(5) 0.0267(3) 0.0508(4) 0.0083(3) -0.0022(3) 0.0133(3) C17 0.026(4) 0.038(3) 0.030(3) 0.010(3) 0.008(3) 0.018(3) C18 0.016(3) 0.041(3) 0.031(3) 0.017(3) 0.005(2) 0.005(3) C19 0.021(3) 0.027(3) 0.019(3) 0.012(2) 0.003(2) 0.004(2) C20 0.016(3) 0.030(3) 0.020(3) 0.012(2) 0.001(2) 0.006(2) C21 0.0179(14) 0.0242(12) 0.0227(12) 0.0130(10) 0.0015(10) -0.0007(10) C22 0.021(3) 0.029(3) 0.030(3) 0.015(2) 0.002(2) -0.007(2) C23 0.029(3) 0.020(3) 0.022(3) 0.010(2) 0.003(2) 0.001(2) C24 0.0179(14) 0.0242(12) 0.0227(12) 0.0130(10) 0.0015(10) -0.0007(10) Br2 0.0331(4) 0.0232(3) 0.0421(4) 0.0099(3) 0.0103(3) -0.0020(3) C25 0.019(3) 0.024(3) 0.015(2) 0.012(2) -0.001(2) -0.003(2) C26 0.0179(14) 0.0242(12) 0.0227(12) 0.0130(10) 0.0015(10) -0.0007(10) C27 0.0179(14) 0.0242(12) 0.0227(12) 0.0130(10) 0.0015(10) -0.0007(10) C28 0.0179(14) 0.0242(12) 0.0227(12) 0.0130(10) 0.0015(10) -0.0007(10) C29 0.021(3) 0.023(3) 0.027(3) 0.017(2) -0.006(2) -0.007(2) C30 0.018(3) 0.036(3) 0.034(3) 0.021(3) 0.003(2) 0.008(3) C31 0.020(3) 0.037(3) 0.020(3) 0.014(2) 0.002(2) 0.005(3) O3 0.026(2) 0.025(2) 0.026(2) 0.0145(17) -0.0089(16) -0.0025(17) C32 0.021(3) 0.028(3) 0.032(3) 0.020(3) 0.003(2) 0.002(3) O4 0.044(3) 0.030(2) 0.047(3) 0.013(2) -0.025(2) -0.009(2) C33 0.0201(19) 0.0239(16) 0.0347(18) 0.0191(14) 0.0028(14) 0.0048(14) C34 0.0201(19) 0.0239(16) 0.0347(18) 0.0191(14) 0.0028(14) 0.0048(14) N2 0.018(3) 0.023(2) 0.022(2) 0.0130(19) -0.0012(18) 0.0029(19) C35 0.027(4) 0.034(3) 0.031(3) 0.022(3) -0.005(3) 0.006(3) C36 0.0201(19) 0.0239(16) 0.0347(18) 0.0191(14) 0.0028(14) 0.0048(14) C37 0.025(3) 0.024(3) 0.033(3) 0.013(2) 0.001(3) 0.000(2) C38 0.034(4) 0.046(4) 0.048(4) 0.016(3) 0.003(3) 0.004(3) Cl1 0.0452(12) 0.0485(11) 0.0809(14) 0.0297(10) 0.0089(10) 0.0013(9) Cl2 0.0519(12) 0.0441(10) 0.0631(12) 0.0125(9) -0.0013(9) 0.0022(9) Cl3 0.0452(13) 0.1057(18) 0.0938(16) 0.0730(15) -0.0025(11) 0.0024(12) C39 0.042(5) 0.095(6) 0.060(5) 0.031(5) -0.012(4) 0.020(5) Cl4 0.131(2) 0.0634(13) 0.0559(13) 0.0154(11) -0.0038(13) 0.0444(14) Cl5 0.0511(12) 0.0806(14) 0.0647(12) 0.0451(11) -0.0160(10) -0.0062(11) Cl6 0.0446(11) 0.0487(10) 0.0574(11) 0.0198(9) -0.0052(9) 0.0068(8) C40 0.054(5) 0.047(4) 0.034(4) 0.020(3) -0.006(3) 0.003(4) Cl7 0.0858(15) 0.0446(10) 0.0549(11) 0.0305(9) -0.0165(10) -0.0162(10) Cl8 0.0593(15) 0.139(2) 0.0955(18) 0.0801(18) 0.0002(13) -0.0106(15) Cl9 0.251(4) 0.0391(12) 0.0595(14) 0.0103(11) -0.0120(19) 0.0184(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.271(4) . ? Cd1 N1 2.277(4) . ? Cd1 Br3 2.5191(7) . ? Cd1 Br4 2.5311(7) . ? N1 C5 1.329(7) . ? N1 C1 1.340(7) . ? C1 C2 1.370(7) . ? C1 H1 0.9300 . ? C2 C3 1.383(8) . ? C2 H2 0.9300 . ? C3 C4 1.364(7) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 C6 1.506(8) . ? C5 H5 0.9300 . ? C6 O1 1.197(6) . ? C6 O2 1.348(6) . ? O2 C7 1.419(6) . ? C7 C12 1.372(7) . ? C7 C8 1.380(7) . ? C8 C9 1.376(8) . ? C8 H8 0.9300 . ? C9 C10 1.400(7) . ? C9 H9 0.9300 . ? C10 C11 1.383(7) . ? C10 C13 1.520(7) . ? C11 C12 1.386(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C25 1.540(7) . ? C13 C26 1.546(7) 1_554 ? C13 C14 1.545(7) . ? C14 C19 1.382(7) . ? C14 C15 1.391(7) . ? C15 C16 1.387(8) . ? C15 H15 0.9300 . ? C16 C17 1.392(8) . ? C16 Br1 1.900(5) . ? C17 C18 1.383(8) . ? C17 H17 0.9300 . ? C18 C19 1.395(7) . ? C18 H18 0.9300 . ? C19 C20 1.479(7) . ? C20 C21 1.392(7) . ? C20 C25 1.395(7) . ? C21 C22 1.386(7) . ? C21 H21 0.9300 . ? C22 C23 1.387(8) . ? C22 H22 0.9300 . ? C23 C24 1.403(7) . ? C23 Br2 1.895(5) . ? C24 C25 1.381(7) . ? C24 H24 0.9300 . ? C26 C27 1.375(7) . ? C26 C31 1.403(7) . ? C26 C13 1.546(7) 1_556 ? C27 C28 1.390(7) . ? C27 H27 0.9300 . ? C28 C29 1.373(7) . ? C28 H28 0.9300 . ? C29 C30 1.368(8) . ? C29 O3 1.421(6) . ? C30 C31 1.374(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? O3 C32 1.345(6) . ? C32 O4 1.199(6) . ? C32 C33 1.500(8) . ? C33 C37 1.385(7) . ? C33 C34 1.386(7) . ? C34 N2 1.339(6) . ? C34 H34 0.9300 . ? N2 C35 1.337(7) . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 C37 1.396(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 Cl1 1.741(7) . ? C38 Cl2 1.756(6) . ? C38 Cl3 1.762(7) . ? C38 H38 0.9800 . ? C39 Cl4 1.688(8) . ? C39 Cl6 1.720(8) . ? C39 Cl5 1.755(7) . ? C39 H39 0.9800 . ? C40 Cl9 1.734(6) . ? C40 Cl7 1.747(7) . ? C40 Cl8 1.754(7) . ? C40 H40 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 113.42(15) . . ? N2 Cd1 Br3 102.41(11) . . ? N1 Cd1 Br3 105.62(11) . . ? N2 Cd1 Br4 105.04(11) . . ? N1 Cd1 Br4 102.30(11) . . ? Br3 Cd1 Br4 128.34(3) . . ? C5 N1 C1 117.2(5) . . ? C5 N1 Cd1 124.5(4) . . ? C1 N1 Cd1 118.3(4) . . ? N1 C1 C2 123.3(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 C6 118.5(5) . . ? C5 C4 C6 122.3(5) . . ? N1 C5 C4 123.0(5) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O1 C6 O2 125.4(5) . . ? O1 C6 C4 123.7(5) . . ? O2 C6 C4 110.9(5) . . ? C6 O2 C7 118.4(4) . . ? C12 C7 C8 121.5(5) . . ? C12 C7 O2 117.1(4) . . ? C8 C7 O2 121.2(5) . . ? C9 C8 C7 118.3(5) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 C10 121.8(5) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 118.2(5) . . ? C11 C10 C13 121.6(4) . . ? C9 C10 C13 119.9(4) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 119.6(5) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C10 C13 C25 115.5(4) . . ? C10 C13 C26 112.9(4) . 1_554 ? C25 C13 C26 105.9(4) . 1_554 ? C10 C13 C14 108.6(4) . . ? C25 C13 C14 99.8(4) . . ? C26 C13 C14 113.6(4) 1_554 . ? C19 C14 C15 120.9(5) . . ? C19 C14 C13 111.6(4) . . ? C15 C14 C13 127.3(5) . . ? C16 C15 C14 117.4(5) . . ? C16 C15 H15 121.3 . . ? C14 C15 H15 121.3 . . ? C15 C16 C17 122.7(5) . . ? C15 C16 Br1 118.7(4) . . ? C17 C16 Br1 118.7(4) . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.1(5) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C14 C19 C18 120.9(5) . . ? C14 C19 C20 108.8(5) . . ? C18 C19 C20 130.2(5) . . ? C21 C20 C25 120.5(5) . . ? C21 C20 C19 131.3(5) . . ? C25 C20 C19 108.2(5) . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 121.8(5) . . ? C22 C23 Br2 119.1(4) . . ? C24 C23 Br2 119.1(4) . . ? C25 C24 C23 118.2(5) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C20 120.5(5) . . ? C24 C25 C13 127.9(5) . . ? C20 C25 C13 111.5(4) . . ? C27 C26 C31 118.3(5) . . ? C27 C26 C13 122.3(5) . 1_556 ? C31 C26 C13 119.2(4) . 1_556 ? C26 C27 C28 120.9(5) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.1(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C30 C29 C28 121.5(5) . . ? C30 C29 O3 120.5(5) . . ? C28 C29 O3 118.0(5) . . ? C29 C30 C31 119.2(5) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C26 121.0(5) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C32 O3 C29 117.3(4) . . ? O4 C32 O3 125.2(5) . . ? O4 C32 C33 124.2(5) . . ? O3 C32 C33 110.5(4) . . ? C37 C33 C34 119.3(5) . . ? C37 C33 C32 118.1(5) . . ? C34 C33 C32 122.6(5) . . ? N2 C34 C33 122.6(5) . . ? N2 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C34 N2 C35 118.1(5) . . ? C34 N2 Cd1 121.9(4) . . ? C35 N2 Cd1 120.1(4) . . ? N2 C35 C36 123.0(5) . . ? N2 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C37 118.9(5) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C33 C37 C36 118.1(5) . . ? C33 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? Cl1 C38 Cl2 110.9(4) . . ? Cl1 C38 Cl3 110.4(4) . . ? Cl2 C38 Cl3 110.3(4) . . ? Cl1 C38 H38 108.4 . . ? Cl2 C38 H38 108.4 . . ? Cl3 C38 H38 108.4 . . ? Cl4 C39 Cl6 114.6(4) . . ? Cl4 C39 Cl5 113.4(5) . . ? Cl6 C39 Cl5 112.4(5) . . ? Cl4 C39 H39 105.1 . . ? Cl6 C39 H39 105.1 . . ? Cl5 C39 H39 105.1 . . ? Cl9 C40 Cl7 110.6(4) . . ? Cl9 C40 Cl8 109.3(4) . . ? Cl7 C40 Cl8 110.3(4) . . ? Cl9 C40 H40 108.8 . . ? Cl7 C40 H40 108.8 . . ? Cl8 C40 H40 108.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.530 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.149 # Attachment 'CIF For 4-CoCl2.cif' data_e459a _database_code_depnum_ccdc_archive 'CCDC 617744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br2 Cl2 Co N2 O4, 3(C H Cl3)' _chemical_formula_sum 'C40 H25 Br2 Cl11 Co N2 O4' _chemical_formula_weight 1206.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0994(7) _cell_length_b 15.7338(13) _cell_length_c 17.0478(14) _cell_angle_alpha 112.465(2) _cell_angle_beta 92.386(2) _cell_angle_gamma 90.890(2) _cell_volume 2252.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1190 _exptl_absorpt_coefficient_mu 2.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6278 _exptl_absorpt_correction_T_max 0.8040 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24746 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.40 _reflns_number_total 10127 _reflns_number_gt 7266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+7.5065P] 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 10127 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _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 -0.42477(7) 0.22376(4) 0.47444(4) 0.01894(15) Uani 1 1 d . . . Cl1 Cl -0.52625(15) 0.16230(9) 0.55965(9) 0.0331(3) Uani 1 1 d . . . Cl2 Cl -0.55860(14) 0.27146(9) 0.38730(8) 0.0301(3) Uani 1 1 d . . . N1 N -0.3139(4) 0.3408(3) 0.5541(2) 0.0190(8) Uani 1 1 d . . . C1 C -0.2314(5) 0.3431(3) 0.6216(3) 0.0200(9) Uani 1 1 d . . . H1 H -0.2224 0.2877 0.6312 0.024 Uiso 1 1 calc R . . C2 C -0.1576(5) 0.4227(3) 0.6789(3) 0.0218(10) Uani 1 1 d . . . C3 C -0.1755(6) 0.5050(3) 0.6662(3) 0.0268(11) Uani 1 1 d . . . H3 H -0.1289 0.5609 0.7043 0.032 Uiso 1 1 calc R . . C4 C -0.2623(6) 0.5030(4) 0.5971(3) 0.0316(12) Uani 1 1 d . . . H4 H -0.2766 0.5577 0.5870 0.038 Uiso 1 1 calc R . . C5 C -0.3281(5) 0.4205(3) 0.5428(3) 0.0257(10) Uani 1 1 d . . . H5 H -0.3864 0.4200 0.4950 0.031 Uiso 1 1 calc R . . C6 C -0.0626(5) 0.4234(3) 0.7514(3) 0.0227(10) Uani 1 1 d . . . O1 O -0.0011(5) 0.4903(3) 0.8029(2) 0.0380(9) Uani 1 1 d . . . O2 O -0.0538(4) 0.3380(2) 0.7518(2) 0.0248(7) Uani 1 1 d . . . C7 C 0.0367(6) 0.3256(3) 0.8161(3) 0.0238(10) Uani 1 1 d . . . C8 C -0.0071(6) 0.3562(4) 0.8980(3) 0.0291(11) Uani 1 1 d . . . H8 H -0.0937 0.3905 0.9132 0.035 Uiso 1 1 calc R . . C9 C 0.0760(5) 0.3366(4) 0.9579(3) 0.0257(10) Uani 1 1 d . . . H9 H 0.0464 0.3576 1.0148 0.031 Uiso 1 1 calc R . . C10 C 0.2047(5) 0.2857(3) 0.9357(3) 0.0189(9) Uani 1 1 d . . . C11 C 0.2456(5) 0.2570(3) 0.8525(3) 0.0208(9) Uani 1 1 d . . . H11 H 0.3320 0.2227 0.8363 0.025 Uiso 1 1 calc R . . C12 C 0.1619(5) 0.2776(3) 0.7921(3) 0.0228(10) Uani 1 1 d . . . H12 H 0.1914 0.2586 0.7353 0.027 Uiso 1 1 calc R . . C13 C 0.3031(5) 0.2703(3) 1.0048(3) 0.0179(9) Uani 1 1 d . . . C14 C 0.4020(5) 0.3567(3) 1.0465(3) 0.0184(9) Uani 1 1 d . . . C15 C 0.3621(5) 0.4462(3) 1.0916(3) 0.0199(9) Uani 1 1 d . . . H15 H 0.2622 0.4606 1.1029 0.024 Uiso 1 1 calc R . . C16 C 0.4741(6) 0.5149(3) 1.1200(3) 0.0245(10) Uani 1 1 d . . . Br1 Br 0.42186(6) 0.63704(4) 1.18492(4) 0.03412(15) Uani 1 1 d . . . C17 C 0.6198(6) 0.4956(4) 1.1027(3) 0.0262(11) Uani 1 1 d . . . H17 H 0.6930 0.5439 1.1212 0.031 Uiso 1 1 calc R . . C18 C 0.6585(5) 0.4063(4) 1.0586(3) 0.0274(11) Uani 1 1 d . . . H18 H 0.7586 0.3925 1.0475 0.033 Uiso 1 1 calc R . . C19 C 0.5504(5) 0.3365(3) 1.0302(3) 0.0213(10) Uani 1 1 d . . . C20 C 0.5595(5) 0.2369(3) 0.9844(3) 0.0216(10) Uani 1 1 d . . . C21 C 0.6815(6) 0.1822(4) 0.9597(3) 0.0307(12) Uani 1 1 d . . . H21 H 0.7780 0.2093 0.9699 0.037 Uiso 1 1 calc R . . C22 C 0.6604(6) 0.0876(4) 0.9200(3) 0.0333(12) Uani 1 1 d . . . H22 H 0.7423 0.0491 0.9031 0.040 Uiso 1 1 calc R . . C23 C 0.5179(6) 0.0495(4) 0.9051(3) 0.0291(11) Uani 1 1 d . . . C24 C 0.3948(6) 0.1019(3) 0.9290(3) 0.0239(10) Uani 1 1 d . . . H24 H 0.2987 0.0742 0.9187 0.029 Uiso 1 1 calc R . . Br2 Br 0.49089(8) -0.08059(4) 0.85208(4) 0.04332(17) Uani 1 1 d . . . C25 C 0.4170(5) 0.1970(3) 0.9686(3) 0.0192(9) Uani 1 1 d . . . C26 C 0.2110(5) 0.2434(3) 1.0663(3) 0.0172(9) Uani 1 1 d . . . C27 C 0.0896(5) 0.1816(3) 1.0343(3) 0.0220(10) Uani 1 1 d . . . H27 H 0.0600 0.1610 0.9757 0.026 Uiso 1 1 calc R . . C28 C 0.0129(5) 0.1506(3) 1.0866(3) 0.0254(10) Uani 1 1 d . . . H28 H -0.0691 0.1088 1.0646 0.030 Uiso 1 1 calc R . . C29 C 0.0573(5) 0.1815(3) 1.1718(3) 0.0209(10) Uani 1 1 d . . . C30 C 0.1757(5) 0.2411(3) 1.2050(3) 0.0221(10) Uani 1 1 d . . . H30 H 0.2045 0.2614 1.2637 0.027 Uiso 1 1 calc R . . C31 C 0.2539(5) 0.2719(3) 1.1513(3) 0.0208(9) Uani 1 1 d . . . H31 H 0.3370 0.3126 1.1735 0.025 Uiso 1 1 calc R . . O3 O -0.0244(4) 0.1579(2) 1.2297(2) 0.0247(7) Uani 1 1 d . . . C32 C -0.0522(5) 0.0682(3) 1.2140(3) 0.0223(10) Uani 1 1 d . . . O4 O -0.0100(4) 0.0047(3) 1.1552(2) 0.0337(9) Uani 1 1 d . . . C33 C -0.1449(5) 0.0579(3) 0.2805(3) 0.0215(10) Uani 1 1 d . . . C34 C -0.2172(5) 0.1304(3) 0.3378(3) 0.0214(10) Uani 1 1 d . . . H34 H -0.2067 0.1895 0.3352 0.026 Uiso 1 1 calc R . . N2 N -0.3013(4) 0.1209(3) 0.3968(2) 0.0197(8) Uani 1 1 d . . . C35 C -0.3140(6) 0.0359(3) 0.3992(3) 0.0260(10) Uani 1 1 d . . . H35 H -0.3717 0.0283 0.4413 0.031 Uiso 1 1 calc R . . C36 C -0.2482(7) -0.0389(4) 0.3440(4) 0.0350(13) Uani 1 1 d . . . H36 H -0.2612 -0.0974 0.3472 0.042 Uiso 1 1 calc R . . C37 C -0.1610(6) -0.0283(3) 0.2824(3) 0.0288(11) Uani 1 1 d . . . H37 H -0.1141 -0.0794 0.2429 0.035 Uiso 1 1 calc R . . C38 C 0.8448(7) 0.7321(5) 0.4844(4) 0.0422(14) Uani 1 1 d . . . H38 H 0.7644 0.7671 0.5200 0.051 Uiso 1 1 calc R . . Cl3 Cl 0.7649(2) 0.64406(13) 0.39424(13) 0.0623(5) Uani 1 1 d . . . Cl4 Cl 0.95059(19) 0.80774(12) 0.45484(12) 0.0537(4) Uani 1 1 d . . . Cl5 Cl 0.9545(2) 0.68636(18) 0.54498(15) 0.0731(6) Uani 1 1 d . . . C39 C 0.7299(7) 0.3942(4) 0.2619(4) 0.0408(14) Uani 1 1 d . . . H39 H 0.7854 0.4274 0.2323 0.049 Uiso 1 1 calc R . . Cl6 Cl 0.56235(18) 0.44770(11) 0.29096(11) 0.0494(4) Uani 1 1 d . . . Cl7 Cl 0.6992(2) 0.27982(13) 0.19188(12) 0.0596(5) Uani 1 1 d . . . Cl8 Cl 0.8360(2) 0.39974(14) 0.35219(12) 0.0572(5) Uani 1 1 d . . . C40 C 0.2814(8) 0.9475(4) 0.3454(4) 0.0444(15) Uani 1 1 d . . . H40 H 0.3757 0.9375 0.3724 0.053 Uiso 1 1 calc R . . Cl9 Cl 0.2372(3) 0.85043(13) 0.25351(14) 0.0782(5) Uani 1 1 d . . . Cl10 Cl 0.3030(3) 1.04517(13) 0.32120(14) 0.0782(5) Uani 1 1 d . . . Cl11 Cl 0.1424(3) 0.9621(2) 0.41550(15) 0.0859(7) 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 Co1 0.0198(3) 0.0195(3) 0.0189(3) 0.0089(3) 0.0014(2) 0.0000(2) Cl1 0.0353(7) 0.0361(7) 0.0389(7) 0.0250(6) 0.0145(6) 0.0057(5) Cl2 0.0318(7) 0.0302(7) 0.0309(6) 0.0159(5) -0.0078(5) -0.0009(5) N1 0.0164(19) 0.021(2) 0.0216(19) 0.0104(16) 0.0008(15) 0.0017(15) C1 0.021(2) 0.019(2) 0.021(2) 0.0096(19) 0.0056(18) 0.0024(18) C2 0.021(2) 0.020(2) 0.023(2) 0.0062(19) 0.0048(19) 0.0022(18) C3 0.028(3) 0.019(2) 0.033(3) 0.010(2) -0.001(2) 0.000(2) C4 0.039(3) 0.021(3) 0.039(3) 0.016(2) -0.004(2) 0.001(2) C5 0.024(3) 0.029(3) 0.028(3) 0.016(2) -0.004(2) -0.001(2) C6 0.020(2) 0.024(3) 0.024(2) 0.010(2) 0.0003(19) 0.0015(19) O1 0.047(2) 0.025(2) 0.037(2) 0.0083(17) -0.0162(19) -0.0071(17) O2 0.0265(18) 0.0246(18) 0.0235(17) 0.0107(15) -0.0088(14) -0.0024(14) C7 0.028(3) 0.022(2) 0.022(2) 0.010(2) -0.007(2) -0.0026(19) C8 0.024(3) 0.037(3) 0.027(3) 0.013(2) 0.005(2) 0.008(2) C9 0.022(2) 0.034(3) 0.022(2) 0.011(2) 0.0048(19) 0.003(2) C10 0.017(2) 0.020(2) 0.019(2) 0.0081(19) -0.0015(17) -0.0005(17) C11 0.021(2) 0.020(2) 0.022(2) 0.0087(19) 0.0036(18) 0.0012(18) C12 0.026(3) 0.021(2) 0.021(2) 0.008(2) 0.0004(19) -0.0028(19) C13 0.018(2) 0.020(2) 0.016(2) 0.0068(18) 0.0004(17) -0.0009(17) C14 0.017(2) 0.025(2) 0.016(2) 0.0108(19) -0.0001(17) -0.0021(18) C15 0.018(2) 0.022(2) 0.022(2) 0.0096(19) 0.0014(18) -0.0014(18) C16 0.031(3) 0.020(2) 0.022(2) 0.007(2) 0.004(2) -0.001(2) Br1 0.0341(3) 0.0220(3) 0.0408(3) 0.0052(2) 0.0108(2) -0.0035(2) C17 0.024(2) 0.027(3) 0.028(3) 0.010(2) 0.001(2) -0.009(2) C18 0.015(2) 0.037(3) 0.028(3) 0.011(2) 0.0042(19) -0.003(2) C19 0.020(2) 0.025(2) 0.019(2) 0.009(2) 0.0030(18) 0.0015(19) C20 0.019(2) 0.025(3) 0.020(2) 0.008(2) 0.0033(18) 0.0015(18) C21 0.019(2) 0.036(3) 0.032(3) 0.007(2) 0.000(2) 0.004(2) C22 0.030(3) 0.039(3) 0.030(3) 0.011(2) 0.004(2) 0.017(2) C23 0.037(3) 0.026(3) 0.022(2) 0.007(2) 0.001(2) 0.006(2) C24 0.026(2) 0.025(3) 0.020(2) 0.008(2) 0.0002(19) -0.0002(19) Br2 0.0554(4) 0.0234(3) 0.0447(4) 0.0055(3) 0.0015(3) 0.0105(3) C25 0.020(2) 0.021(2) 0.016(2) 0.0064(19) 0.0008(17) 0.0038(18) C26 0.017(2) 0.017(2) 0.020(2) 0.0088(18) 0.0022(17) 0.0012(17) C27 0.022(2) 0.024(2) 0.017(2) 0.0055(19) -0.0019(18) -0.0045(19) C28 0.023(2) 0.028(3) 0.026(3) 0.012(2) -0.001(2) -0.008(2) C29 0.025(2) 0.019(2) 0.021(2) 0.0089(19) 0.0054(19) 0.0009(18) C30 0.027(2) 0.022(2) 0.015(2) 0.0049(19) 0.0014(18) -0.0010(19) C31 0.022(2) 0.021(2) 0.019(2) 0.0067(19) -0.0011(18) -0.0052(18) O3 0.0316(19) 0.0202(17) 0.0234(17) 0.0090(14) 0.0084(14) -0.0030(14) C32 0.022(2) 0.024(2) 0.021(2) 0.009(2) 0.0019(19) -0.0009(19) O4 0.045(2) 0.027(2) 0.0287(19) 0.0080(16) 0.0156(17) 0.0035(16) C33 0.021(2) 0.021(2) 0.021(2) 0.0067(19) -0.0004(19) -0.0035(18) C34 0.024(2) 0.018(2) 0.023(2) 0.0084(19) 0.0004(19) -0.0014(18) N2 0.021(2) 0.019(2) 0.0193(19) 0.0078(16) 0.0003(15) -0.0009(15) C35 0.029(3) 0.025(3) 0.027(3) 0.014(2) 0.005(2) -0.003(2) C36 0.045(3) 0.020(3) 0.042(3) 0.014(2) 0.017(3) -0.001(2) C37 0.035(3) 0.020(3) 0.031(3) 0.009(2) 0.009(2) 0.001(2) C38 0.029(3) 0.053(4) 0.045(3) 0.018(3) 0.003(3) 0.004(3) Cl3 0.0607(11) 0.0433(10) 0.0678(12) 0.0055(9) -0.0063(9) 0.0009(8) Cl4 0.0459(9) 0.0514(10) 0.0692(11) 0.0282(9) 0.0114(8) 0.0050(7) Cl5 0.0437(10) 0.1166(18) 0.0903(15) 0.0758(14) -0.0065(10) -0.0023(10) C39 0.036(3) 0.050(4) 0.041(3) 0.024(3) -0.001(3) 0.001(3) Cl6 0.0410(8) 0.0450(9) 0.0572(10) 0.0145(8) -0.0040(7) 0.0044(7) Cl7 0.0752(13) 0.0461(10) 0.0527(10) 0.0139(8) -0.0037(9) 0.0146(9) Cl8 0.0466(10) 0.0725(12) 0.0585(10) 0.0338(9) -0.0153(8) -0.0030(8) C40 0.049(4) 0.039(3) 0.053(4) 0.027(3) -0.003(3) -0.003(3) Cl9 0.1252(14) 0.0411(7) 0.0666(9) 0.0215(7) -0.0132(9) -0.0151(8) Cl10 0.1252(14) 0.0411(7) 0.0666(9) 0.0215(7) -0.0132(9) -0.0151(8) Cl11 0.0618(13) 0.135(2) 0.0777(15) 0.0591(15) 0.0109(11) -0.0011(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 Co1 N1 2.042(4) . ? Co1 N2 2.044(4) . ? Co1 Cl2 2.2323(13) . ? Co1 Cl1 2.2484(13) . ? N1 C1 1.335(6) . ? N1 C5 1.348(6) . ? C1 C2 1.399(7) . ? C1 H1 0.9500 . ? C2 C3 1.404(7) . ? C2 C6 1.475(7) . ? C3 C4 1.380(7) . ? C3 H3 0.9500 . ? C4 C5 1.383(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.194(6) . ? C6 O2 1.349(6) . ? O2 C7 1.418(6) . ? C7 C12 1.366(7) . ? C7 C8 1.370(7) . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.411(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(6) . ? C10 C13 1.544(6) . ? C11 C12 1.394(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C25 1.527(6) . ? C13 C14 1.527(6) . ? C13 C26 1.543(6) . ? C14 C15 1.385(7) . ? C14 C19 1.406(6) . ? C15 C16 1.402(7) . ? C15 H15 0.9500 . ? C16 C17 1.383(7) . ? C16 Br1 1.895(5) . ? C17 C18 1.376(7) . ? C17 H17 0.9500 . ? C18 C19 1.389(7) . ? C18 H18 0.9500 . ? C19 C20 1.465(7) . ? C20 C21 1.394(7) . ? C20 C25 1.402(7) . ? C21 C22 1.386(8) . ? C21 H21 0.9500 . ? C22 C23 1.392(8) . ? C22 H22 0.9500 . ? C23 C24 1.382(7) . ? C23 Br2 1.902(5) . ? C24 C25 1.394(7) . ? C24 H24 0.9500 . ? C26 C31 1.380(6) . ? C26 C27 1.405(6) . ? C27 C28 1.376(7) . ? C27 H27 0.9500 . ? C28 C29 1.385(7) . ? C28 H28 0.9500 . ? C29 C30 1.369(7) . ? C29 O3 1.414(5) . ? C30 C31 1.400(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O3 C32 1.349(6) . ? C32 O4 1.196(6) . ? C32 C33 1.498(6) 1_556 ? C33 C37 1.374(7) . ? C33 C34 1.384(7) . ? C33 C32 1.498(6) 1_554 ? C34 N2 1.339(6) . ? C34 H34 0.9500 . ? N2 C35 1.357(6) . ? C35 C36 1.361(7) . ? C35 H35 0.9500 . ? C36 C37 1.398(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 Cl3 1.749(7) . ? C38 Cl4 1.749(7) . ? C38 Cl5 1.757(6) . ? C38 H38 1.0000 . ? C39 Cl7 1.748(7) . ? C39 Cl6 1.750(6) . ? C39 Cl8 1.755(6) . ? C39 H39 1.0000 . ? C40 Cl11 1.734(7) . ? C40 Cl9 1.746(7) . ? C40 Cl10 1.746(6) . ? C40 H40 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 116.89(15) . . ? N1 Co1 Cl2 103.37(11) . . ? N2 Co1 Cl2 105.19(11) . . ? N1 Co1 Cl1 105.49(11) . . ? N2 Co1 Cl1 104.02(11) . . ? Cl2 Co1 Cl1 122.76(6) . . ? C1 N1 C5 117.3(4) . . ? C1 N1 Co1 122.0(3) . . ? C5 N1 Co1 120.6(3) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.1(4) . . ? C1 C2 C6 122.9(4) . . ? C3 C2 C6 119.0(4) . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.3(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 123.3(4) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? O1 C6 O2 124.3(4) . . ? O1 C6 C2 124.9(5) . . ? O2 C6 C2 110.9(4) . . ? C6 O2 C7 118.5(4) . . ? C12 C7 C8 122.1(4) . . ? C12 C7 O2 117.7(4) . . ? C8 C7 O2 120.1(4) . . ? C7 C8 C9 119.2(5) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 120.7(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 118.2(4) . . ? C11 C10 C13 121.4(4) . . ? C9 C10 C13 120.2(4) . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C7 C12 C11 118.9(4) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C25 C13 C14 101.2(4) . . ? C25 C13 C26 108.3(4) . . ? C14 C13 C26 115.2(4) . . ? C25 C13 C10 113.4(4) . . ? C14 C13 C10 106.8(4) . . ? C26 C13 C10 111.6(4) . . ? C15 C14 C19 120.5(4) . . ? C15 C14 C13 128.6(4) . . ? C19 C14 C13 110.8(4) . . ? C14 C15 C16 117.7(4) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 122.0(5) . . ? C17 C16 Br1 119.8(4) . . ? C15 C16 Br1 118.2(4) . . ? C18 C17 C16 119.8(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C14 120.3(4) . . ? C18 C19 C20 131.5(4) . . ? C14 C19 C20 108.2(4) . . ? C21 C20 C25 120.5(5) . . ? C21 C20 C19 130.6(5) . . ? C25 C20 C19 108.9(4) . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.3(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 122.8(5) . . ? C24 C23 Br2 118.4(4) . . ? C22 C23 Br2 118.8(4) . . ? C23 C24 C25 117.5(5) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C24 C25 C20 120.7(4) . . ? C24 C25 C13 128.6(4) . . ? C20 C25 C13 110.7(4) . . ? C31 C26 C27 118.9(4) . . ? C31 C26 C13 121.1(4) . . ? C27 C26 C13 119.7(4) . . ? C28 C27 C26 121.0(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 118.8(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 121.8(4) . . ? C30 C29 O3 116.9(4) . . ? C28 C29 O3 121.2(4) . . ? C29 C30 C31 119.1(4) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C26 C31 C30 120.5(4) . . ? C26 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C32 O3 C29 119.0(4) . . ? O4 C32 O3 125.6(4) . . ? O4 C32 C33 123.7(4) . 1_556 ? O3 C32 C33 110.7(4) . 1_556 ? C37 C33 C34 119.4(4) . . ? C37 C33 C32 117.8(4) . 1_554 ? C34 C33 C32 122.7(4) . 1_554 ? N2 C34 C33 122.7(4) . . ? N2 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 N2 C35 117.4(4) . . ? C34 N2 Co1 123.5(3) . . ? C35 N2 Co1 118.9(3) . . ? N2 C35 C36 123.1(5) . . ? N2 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C37 119.1(5) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C33 C37 C36 118.3(5) . . ? C33 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? Cl3 C38 Cl4 110.3(3) . . ? Cl3 C38 Cl5 110.6(4) . . ? Cl4 C38 Cl5 110.0(3) . . ? Cl3 C38 H38 108.6 . . ? Cl4 C38 H38 108.6 . . ? Cl5 C38 H38 108.6 . . ? Cl7 C39 Cl6 110.4(3) . . ? Cl7 C39 Cl8 110.5(3) . . ? Cl6 C39 Cl8 110.6(3) . . ? Cl7 C39 H39 108.4 . . ? Cl6 C39 H39 108.4 . . ? Cl8 C39 H39 108.4 . . ? Cl11 C40 Cl9 108.7(4) . . ? Cl11 C40 Cl10 110.4(4) . . ? Cl9 C40 Cl10 110.8(4) . . ? Cl11 C40 H40 109.0 . . ? Cl9 C40 H40 109.0 . . ? Cl10 C40 H40 109.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.938 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.128 # Attachment 'CIF For 4-HgCl2.cif' data_e446a _database_code_depnum_ccdc_archive 'CCDC 617745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br2 Cl2 Hg N2 O4, 3(C H Cl3)' _chemical_formula_sum 'C40 H25 Br2 Cl11 Hg N2 O4' _chemical_formula_weight 1347.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0953(18) _cell_length_b 15.939(3) _cell_length_c 17.300(4) _cell_angle_alpha 113.92(3) _cell_angle_beta 91.97(3) _cell_angle_gamma 91.79(3) _cell_volume 2288.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 5.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6236 _exptl_absorpt_correction_T_max 0.7225 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35088 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 30.15 _reflns_number_total 13400 _reflns_number_gt 10763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+3.2178P] 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 13400 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.04631(2) 0.226620(12) 0.477061(11) 0.02535(7) Uani 1 1 d . . . Cl1 Cl -0.03298(17) 0.14907(11) 0.56261(10) 0.0428(3) Uani 1 1 d . . . Cl2 Cl -0.06328(17) 0.29079(10) 0.38766(9) 0.0398(3) Uani 1 1 d . . . N1 N 0.1874(4) 0.3558(3) 0.5715(2) 0.0227(8) Uani 1 1 d . . . C1 C 0.1849(6) 0.4351(4) 0.5618(3) 0.0286(10) Uani 1 1 d . . . H1 H 0.1265 0.4367 0.5160 0.034 Uiso 1 1 calc R . . C2 C 0.2626(6) 0.5141(4) 0.6149(4) 0.0309(11) Uani 1 1 d . . . H2 H 0.2586 0.5689 0.6059 0.037 Uiso 1 1 calc R . . C3 C 0.3467(6) 0.5113(4) 0.6819(3) 0.0279(10) Uani 1 1 d . . . H3 H 0.3999 0.5649 0.7207 0.033 Uiso 1 1 calc R . . C4 C 0.3524(5) 0.4292(3) 0.6919(3) 0.0206(8) Uani 1 1 d . . . C5 C 0.2696(5) 0.3529(3) 0.6361(3) 0.0213(9) Uani 1 1 d . . . H5 H 0.2711 0.2972 0.6438 0.026 Uiso 1 1 calc R . . C6 C 0.4468(5) 0.4258(3) 0.7623(3) 0.0239(9) Uani 1 1 d . . . O1 O 0.5147(5) 0.4913(3) 0.8154(3) 0.0417(10) Uani 1 1 d . . . O2 O 0.4504(4) 0.3395(2) 0.7577(2) 0.0258(7) Uani 1 1 d . . . C7 C 0.5368(5) 0.3254(3) 0.8201(3) 0.0230(9) Uani 1 1 d . . . C8 C 0.4922(5) 0.3548(4) 0.9019(3) 0.0263(10) Uani 1 1 d . . . H8 H 0.4063 0.3888 0.9183 0.032 Uiso 1 1 calc R . . C9 C 0.5759(5) 0.3336(4) 0.9600(3) 0.0259(10) Uani 1 1 d . . . H9 H 0.5467 0.3538 1.0166 0.031 Uiso 1 1 calc R . . C10 C 0.7018(5) 0.2832(3) 0.9364(3) 0.0198(8) Uani 1 1 d . . . C11 C 0.7432(5) 0.2556(3) 0.8536(3) 0.0194(8) Uani 1 1 d . . . H11 H 0.8291 0.2218 0.8367 0.023 Uiso 1 1 calc R . . C12 C 0.6622(5) 0.2764(3) 0.7952(3) 0.0229(9) Uani 1 1 d . . . H12 H 0.6922 0.2572 0.7388 0.028 Uiso 1 1 calc R . . C13 C 0.7996(5) 0.2691(3) 1.0037(3) 0.0179(8) Uani 1 1 d . . . C14 C 0.8998(5) 0.3557(3) 1.0457(3) 0.0194(8) Uani 1 1 d . . . C15 C 0.8610(5) 0.4452(3) 1.0900(3) 0.0220(9) Uani 1 1 d . . . H15 H 0.7611 0.4591 1.1013 0.026 Uiso 1 1 calc R . . C16 C 0.9720(5) 0.5144(3) 1.1174(3) 0.0237(9) Uani 1 1 d . . . C17 C 1.1195(5) 0.4957(4) 1.1017(3) 0.0275(10) Uani 1 1 d . . . H17 H 1.1931 0.5443 1.1205 0.033 Uiso 1 1 calc R . . C18 C 1.1577(5) 0.4057(4) 1.0583(3) 0.0277(10) Uani 1 1 d . . . H18 H 1.2578 0.3917 1.0477 0.033 Uiso 1 1 calc R . . C19 C 1.0473(5) 0.3360(3) 1.0305(3) 0.0204(8) Uani 1 1 d . . . Br1 Br 0.92152(6) 0.63740(3) 1.18042(4) 0.03393(12) Uani 1 1 d . . . C20 C 1.0557(5) 0.2360(3) 0.9840(3) 0.0227(9) Uani 1 1 d . . . C21 C 1.1774(6) 0.1815(4) 0.9601(3) 0.0307(11) Uani 1 1 d . . . H21 H 1.2744 0.2090 0.9706 0.037 Uiso 1 1 calc R . . C22 C 1.1552(6) 0.0873(4) 0.9210(3) 0.0337(12) Uani 1 1 d . . . H22 H 1.2368 0.0492 0.9049 0.040 Uiso 1 1 calc R . . C23 C 1.0137(6) 0.0490(4) 0.9055(3) 0.0295(10) Uani 1 1 d . . . C24 C 0.8905(5) 0.1018(3) 0.9280(3) 0.0244(9) Uani 1 1 d . . . H24 H 0.7938 0.0739 0.9165 0.029 Uiso 1 1 calc R . . C25 C 0.9133(5) 0.1957(3) 0.9673(3) 0.0201(8) Uani 1 1 d . . . Br2 Br 0.98435(8) -0.08125(4) 0.85340(4) 0.04479(15) Uani 1 1 d . . . C26 C 0.7085(5) 0.2420(3) 1.0641(3) 0.0175(8) Uani 1 1 d . . . C27 C 0.7532(5) 0.2710(3) 1.1496(3) 0.0222(9) Uani 1 1 d . . . H27 H 0.8368 0.3122 1.1721 0.027 Uiso 1 1 calc R . . C28 C 0.6766(5) 0.2402(3) 1.2020(3) 0.0234(9) Uani 1 1 d . . . H28 H 0.7072 0.2600 1.2600 0.028 Uiso 1 1 calc R . . C29 C 0.5566(5) 0.1808(3) 1.1688(3) 0.0213(8) Uani 1 1 d . . . C30 C 0.5093(5) 0.1498(3) 1.0846(3) 0.0244(9) Uani 1 1 d . . . H30 H 0.4262 0.1081 1.0627 0.029 Uiso 1 1 calc R . . C31 C 0.5866(5) 0.1813(3) 1.0328(3) 0.0233(9) Uani 1 1 d . . . H31 H 0.5553 0.1608 0.9749 0.028 Uiso 1 1 calc R . . O3 O 0.4748(4) 0.1568(2) 1.2258(2) 0.0249(7) Uani 1 1 d . . . C32 C 0.4525(5) 0.0673(3) 1.2099(3) 0.0224(9) Uani 1 1 d . . . O4 O 0.4988(5) 0.0046(3) 1.1518(2) 0.0350(9) Uani 1 1 d . . . C33 C 0.3612(5) 0.0557(3) 1.2755(3) 0.0213(8) Uani 1 1 d . . . C34 C 0.3541(6) -0.0289(4) 1.2799(3) 0.0313(11) Uani 1 1 d . . . H34 H 0.4051 -0.0788 1.2417 0.038 Uiso 1 1 calc R . . C35 C 0.2825(5) 0.1268(3) 0.3310(3) 0.0215(8) Uani 1 1 d . . . H35 H 0.2859 0.1844 0.3267 0.026 Uiso 1 1 calc R . . N2 N 0.2023(4) 0.1165(3) 0.3899(2) 0.0212(7) Uani 1 1 d . . . C36 C 0.1981(6) 0.0338(3) 0.3954(3) 0.0261(10) Uani 1 1 d . . . H36 H 0.1428 0.0266 0.4382 0.031 Uiso 1 1 calc R . . C37 C 0.2702(7) -0.0393(4) 0.3419(4) 0.0363(13) Uani 1 1 d . . . H37 H 0.2634 -0.0966 0.3467 0.044 Uiso 1 1 calc R . . C38 C 0.7887(8) 0.9551(4) 0.3459(4) 0.0439(14) Uani 1 1 d . . . H38 H 0.8848 0.9497 0.3730 0.053 Uiso 1 1 calc R . . Cl3 Cl 0.6494(3) 0.9702(3) 0.41659(18) 0.0982(10) Uani 1 1 d . . . Cl4 Cl 0.7449(3) 0.85338(15) 0.25686(15) 0.0814(5) Uani 1 1 d . . . Cl5 Cl 0.8009(3) 1.04888(15) 0.31846(15) 0.0814(5) Uani 1 1 d . . . C39 C 0.7721(8) 0.6024(6) 0.7345(5) 0.0538(17) Uani 1 1 d . . . H39 H 0.7076 0.5687 0.7591 0.065 Uiso 1 1 calc R . . Cl6 Cl 0.7924(3) 0.71409(15) 0.80723(13) 0.0750(7) Uani 1 1 d . . . Cl7 Cl 0.93631(19) 0.54807(12) 0.71398(11) 0.0504(4) Uani 1 1 d . . . Cl8 Cl 0.6811(2) 0.59478(16) 0.63984(13) 0.0635(5) Uani 1 1 d . . . C40 C 0.3618(7) 0.7358(5) 0.4849(4) 0.0444(14) Uani 1 1 d . . . H40 H 0.2870 0.7731 0.5238 0.053 Uiso 1 1 calc R . . Cl9 Cl 0.4715(2) 0.80872(14) 0.45580(16) 0.0643(5) Uani 1 1 d . . . Cl10 Cl 0.4687(2) 0.6845(2) 0.53881(17) 0.0811(7) Uani 1 1 d . . . Cl11 Cl 0.2693(2) 0.65191(13) 0.39588(13) 0.0582(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02910(11) 0.02454(10) 0.02608(10) 0.01394(7) 0.00237(7) 0.00202(7) Cl1 0.0459(8) 0.0454(8) 0.0556(9) 0.0373(7) 0.0233(7) 0.0116(6) Cl2 0.0445(8) 0.0409(7) 0.0420(7) 0.0262(6) -0.0125(6) 0.0019(6) N1 0.0214(19) 0.0249(19) 0.0247(18) 0.0128(16) 0.0005(15) 0.0044(15) C1 0.035(3) 0.028(2) 0.029(2) 0.018(2) 0.000(2) 0.004(2) C2 0.035(3) 0.023(2) 0.040(3) 0.018(2) -0.003(2) 0.003(2) C3 0.026(2) 0.024(2) 0.034(3) 0.012(2) 0.001(2) 0.0032(19) C4 0.019(2) 0.023(2) 0.024(2) 0.0133(18) 0.0018(16) 0.0034(16) C5 0.024(2) 0.019(2) 0.026(2) 0.0144(18) 0.0032(17) 0.0026(17) C6 0.022(2) 0.026(2) 0.025(2) 0.0110(19) 0.0005(18) 0.0033(18) O1 0.047(2) 0.031(2) 0.045(2) 0.0160(18) -0.019(2) -0.0052(18) O2 0.0285(18) 0.0251(17) 0.0267(16) 0.0143(14) -0.0071(14) -0.0011(13) C7 0.023(2) 0.024(2) 0.024(2) 0.0126(18) -0.0045(17) -0.0001(17) C8 0.018(2) 0.037(3) 0.027(2) 0.017(2) 0.0038(18) 0.0086(19) C9 0.018(2) 0.038(3) 0.025(2) 0.017(2) 0.0066(17) 0.0055(19) C10 0.0162(19) 0.022(2) 0.021(2) 0.0092(17) -0.0032(16) 0.0012(16) C11 0.019(2) 0.022(2) 0.0190(19) 0.0101(17) 0.0017(16) 0.0014(16) C12 0.025(2) 0.026(2) 0.019(2) 0.0105(18) 0.0027(17) 0.0009(18) C13 0.0141(19) 0.023(2) 0.0176(18) 0.0087(16) 0.0003(15) 0.0024(15) C14 0.017(2) 0.026(2) 0.0183(19) 0.0120(17) 0.0011(15) -0.0006(16) C15 0.019(2) 0.026(2) 0.024(2) 0.0122(18) 0.0067(17) 0.0029(17) C16 0.024(2) 0.025(2) 0.024(2) 0.0115(18) 0.0039(18) -0.0007(18) C17 0.019(2) 0.029(2) 0.032(2) 0.010(2) 0.0035(19) -0.0027(18) C18 0.014(2) 0.038(3) 0.031(2) 0.014(2) 0.0047(18) -0.0041(19) C19 0.0148(19) 0.024(2) 0.024(2) 0.0116(18) 0.0030(16) -0.0002(16) Br1 0.0321(3) 0.0230(2) 0.0422(3) 0.0081(2) 0.0114(2) -0.0014(2) C20 0.019(2) 0.027(2) 0.021(2) 0.0076(18) 0.0028(17) 0.0043(18) C21 0.018(2) 0.038(3) 0.031(2) 0.008(2) 0.0031(19) 0.007(2) C22 0.030(3) 0.037(3) 0.032(3) 0.011(2) 0.006(2) 0.016(2) C23 0.036(3) 0.026(2) 0.024(2) 0.0061(19) 0.004(2) 0.010(2) C24 0.022(2) 0.028(2) 0.025(2) 0.0125(19) 0.0027(18) 0.0027(18) C25 0.019(2) 0.025(2) 0.0174(19) 0.0099(17) 0.0004(16) 0.0031(17) Br2 0.0566(4) 0.0252(3) 0.0465(3) 0.0077(2) 0.0005(3) 0.0128(3) C26 0.0171(19) 0.0187(19) 0.0178(18) 0.0085(16) 0.0017(15) 0.0008(15) C27 0.022(2) 0.022(2) 0.020(2) 0.0065(17) -0.0027(17) -0.0026(17) C28 0.027(2) 0.026(2) 0.0182(19) 0.0095(18) 0.0013(17) -0.0009(18) C29 0.022(2) 0.023(2) 0.020(2) 0.0095(17) 0.0068(17) 0.0007(17) C30 0.021(2) 0.030(2) 0.023(2) 0.0116(19) 0.0004(17) -0.0072(18) C31 0.023(2) 0.027(2) 0.0170(19) 0.0073(18) -0.0017(17) -0.0041(18) O3 0.0303(18) 0.0245(16) 0.0211(15) 0.0102(13) 0.0079(13) -0.0026(14) C32 0.023(2) 0.023(2) 0.023(2) 0.0109(18) 0.0039(17) -0.0022(17) O4 0.045(2) 0.0264(18) 0.034(2) 0.0115(16) 0.0190(17) 0.0048(16) C33 0.021(2) 0.021(2) 0.023(2) 0.0108(17) 0.0005(17) -0.0022(16) C34 0.039(3) 0.025(2) 0.034(3) 0.015(2) 0.015(2) 0.007(2) C35 0.023(2) 0.022(2) 0.021(2) 0.0104(17) 0.0037(17) 0.0000(17) N2 0.0214(19) 0.0217(18) 0.0245(18) 0.0132(15) 0.0043(15) 0.0017(15) C36 0.026(2) 0.026(2) 0.029(2) 0.015(2) 0.0099(19) -0.0015(18) C37 0.048(3) 0.022(2) 0.047(3) 0.021(2) 0.021(3) 0.004(2) C38 0.055(4) 0.038(3) 0.043(3) 0.021(3) -0.008(3) -0.004(3) Cl3 0.0645(14) 0.169(3) 0.0820(16) 0.073(2) 0.0059(12) -0.0048(17) Cl4 0.1255(15) 0.0465(8) 0.0697(10) 0.0243(7) -0.0206(10) -0.0134(8) Cl5 0.1255(15) 0.0465(8) 0.0697(10) 0.0243(7) -0.0206(10) -0.0134(8) C39 0.050(4) 0.067(5) 0.050(4) 0.030(4) -0.002(3) 0.007(4) Cl6 0.1121(19) 0.0537(11) 0.0549(11) 0.0160(9) -0.0003(11) 0.0358(12) Cl7 0.0432(9) 0.0480(9) 0.0553(9) 0.0162(8) -0.0025(7) 0.0080(7) Cl8 0.0497(10) 0.0903(15) 0.0609(11) 0.0435(11) -0.0163(8) -0.0050(10) C40 0.031(3) 0.050(4) 0.051(4) 0.018(3) 0.006(3) 0.006(3) Cl9 0.0516(10) 0.0529(11) 0.0915(15) 0.0323(11) 0.0068(10) 0.0039(8) Cl10 0.0496(11) 0.127(2) 0.1010(18) 0.0836(17) -0.0093(11) -0.0062(12) Cl11 0.0529(10) 0.0459(9) 0.0627(11) 0.0088(8) -0.0004(8) 0.0038(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 Hg1 N1 2.349(4) . ? Hg1 N2 2.351(4) . ? Hg1 Cl2 2.3816(13) . ? Hg1 Cl1 2.3956(14) . ? N1 C1 1.341(6) . ? N1 C5 1.341(6) . ? C1 C2 1.375(8) . ? C1 H1 0.9500 . ? C2 C3 1.383(7) . ? C2 H2 0.9500 . ? C3 C4 1.390(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 C6 1.485(6) . ? C5 H5 0.9500 . ? C6 O1 1.207(6) . ? C6 O2 1.347(6) . ? O2 C7 1.409(5) . ? C7 C8 1.378(7) . ? C7 C12 1.384(7) . ? C8 C9 1.394(6) . ? C8 H8 0.9500 . ? C9 C10 1.395(6) . ? C9 H9 0.9500 . ? C10 C11 1.387(6) . ? C10 C13 1.533(6) . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.526(6) . ? C13 C25 1.536(6) . ? C13 C26 1.539(6) . ? C14 C15 1.382(6) . ? C14 C19 1.396(6) . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C17 1.395(7) . ? C16 Br1 1.898(5) . ? C17 C18 1.385(7) . ? C17 H17 0.9500 . ? C18 C19 1.392(7) . ? C18 H18 0.9500 . ? C19 C20 1.471(6) . ? C20 C25 1.395(6) . ? C20 C21 1.398(6) . ? C21 C22 1.378(8) . ? C21 H21 0.9500 . ? C22 C23 1.377(8) . ? C22 H22 0.9500 . ? C23 C24 1.392(7) . ? C23 Br2 1.904(5) . ? C24 C25 1.375(7) . ? C24 H24 0.9500 . ? C26 C31 1.388(6) . ? C26 C27 1.399(6) . ? C27 C28 1.389(6) . ? C27 H27 0.9500 . ? C28 C29 1.367(7) . ? C28 H28 0.9500 . ? C29 C30 1.382(6) . ? C29 O3 1.419(5) . ? C30 C31 1.391(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O3 C32 1.345(6) . ? C32 O4 1.195(6) . ? C32 C33 1.495(6) . ? C33 C34 1.381(6) . ? C33 C35 1.390(6) 1_556 ? C34 C37 1.398(7) 1_556 ? C34 H34 0.9500 . ? C35 N2 1.334(6) . ? C35 C33 1.390(6) 1_554 ? C35 H35 0.9500 . ? N2 C36 1.358(6) . ? C36 C37 1.364(7) . ? C36 H36 0.9500 . ? C37 C34 1.398(7) 1_554 ? C37 H37 0.9500 . ? C38 Cl5 1.744(6) . ? C38 Cl3 1.745(7) . ? C38 Cl4 1.746(7) . ? C38 H38 1.0000 . ? C39 Cl6 1.712(8) . ? C39 Cl7 1.725(7) . ? C39 Cl8 1.766(7) . ? C39 H39 1.0000 . ? C40 Cl11 1.744(7) . ? C40 Cl9 1.743(7) . ? C40 Cl10 1.758(7) . ? C40 H40 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N2 109.78(14) . . ? N1 Hg1 Cl2 99.66(10) . . ? N2 Hg1 Cl2 104.81(10) . . ? N1 Hg1 Cl1 104.39(10) . . ? N2 Hg1 Cl1 98.99(10) . . ? Cl2 Hg1 Cl1 137.79(6) . . ? C1 N1 C5 118.7(4) . . ? C1 N1 Hg1 119.7(3) . . ? C5 N1 Hg1 121.6(3) . . ? N1 C1 C2 123.4(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 118.0(5) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 119.3(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 C6 121.9(4) . . ? C3 C4 C6 119.0(4) . . ? N1 C5 C4 121.6(4) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? O1 C6 O2 124.3(4) . . ? O1 C6 C4 124.6(5) . . ? O2 C6 C4 111.1(4) . . ? C6 O2 C7 117.6(4) . . ? C8 C7 C12 121.5(4) . . ? C8 C7 O2 120.6(4) . . ? C12 C7 O2 117.7(4) . . ? C7 C8 C9 118.6(4) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 118.2(4) . . ? C11 C10 C13 121.6(4) . . ? C9 C10 C13 119.8(4) . . ? C12 C11 C10 121.5(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 119.0(4) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? C14 C13 C10 106.7(3) . . ? C14 C13 C25 101.1(3) . . ? C10 C13 C25 114.1(3) . . ? C14 C13 C26 115.6(4) . . ? C10 C13 C26 112.0(3) . . ? C25 C13 C26 107.1(3) . . ? C15 C14 C19 120.4(4) . . ? C15 C14 C13 128.6(4) . . ? C19 C14 C13 111.0(4) . . ? C14 C15 C16 118.2(4) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C15 C16 C17 122.0(4) . . ? C15 C16 Br1 118.8(3) . . ? C17 C16 Br1 119.2(4) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 119.0(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C14 C19 C18 121.0(4) . . ? C14 C19 C20 108.4(4) . . ? C18 C19 C20 130.6(4) . . ? C25 C20 C21 120.4(5) . . ? C25 C20 C19 108.8(4) . . ? C21 C20 C19 130.7(5) . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 122.5(5) . . ? C22 C23 Br2 119.1(4) . . ? C24 C23 Br2 118.4(4) . . ? C25 C24 C23 117.9(5) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C20 120.6(4) . . ? C24 C25 C13 128.7(4) . . ? C20 C25 C13 110.5(4) . . ? C31 C26 C27 118.4(4) . . ? C31 C26 C13 120.1(4) . . ? C27 C26 C13 121.2(4) . . ? C28 C27 C26 120.7(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.0(4) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 122.2(4) . . ? C28 C29 O3 117.2(4) . . ? C30 C29 O3 120.5(4) . . ? C29 C30 C31 118.3(4) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C30 C31 C26 121.3(4) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? C32 O3 C29 118.7(4) . . ? O4 C32 O3 125.5(4) . . ? O4 C32 C33 123.6(4) . . ? O3 C32 C33 110.9(4) . . ? C34 C33 C35 119.4(4) . 1_556 ? C34 C33 C32 118.5(4) . . ? C35 C33 C32 122.1(4) 1_556 . ? C33 C34 C37 118.4(5) . 1_556 ? C33 C34 H34 120.8 . . ? C37 C34 H34 120.8 1_556 . ? N2 C35 C33 122.0(4) . 1_554 ? N2 C35 H35 119.0 . . ? C33 C35 H35 119.0 1_554 . ? C35 N2 C36 118.6(4) . . ? C35 N2 Hg1 124.6(3) . . ? C36 N2 Hg1 116.5(3) . . ? C37 C36 N2 122.5(4) . . ? C37 C36 H36 118.8 . . ? N2 C36 H36 118.8 . . ? C36 C37 C34 119.2(5) . 1_554 ? C36 C37 H37 120.4 . . ? C34 C37 H37 120.4 1_554 . ? Cl5 C38 Cl3 109.6(4) . . ? Cl5 C38 Cl4 111.0(4) . . ? Cl3 C38 Cl4 107.7(4) . . ? Cl5 C38 H38 109.5 . . ? Cl3 C38 H38 109.5 . . ? Cl4 C38 H38 109.5 . . ? Cl6 C39 Cl7 113.0(4) . . ? Cl6 C39 Cl8 111.2(4) . . ? Cl7 C39 Cl8 110.9(4) . . ? Cl6 C39 H39 107.1 . . ? Cl7 C39 H39 107.1 . . ? Cl8 C39 H39 107.1 . . ? Cl11 C40 Cl9 110.3(4) . . ? Cl11 C40 Cl10 110.4(4) . . ? Cl9 C40 Cl10 110.6(4) . . ? Cl11 C40 H40 108.5 . . ? Cl9 C40 H40 108.5 . . ? Cl10 C40 H40 108.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.797 _refine_diff_density_min -1.720 _refine_diff_density_rms 0.221 # Attachment 'CIF For 5-HgBr2.cif' data_e674a _database_code_depnum_ccdc_archive 'CCDC 617746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br4 Hg N2 O4, C H Cl3' _chemical_formula_sum 'C38 H23 Br4 Cl3 Hg N2 O4' _chemical_formula_weight 1198.16 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.7500(11) _cell_length_b 16.1881(14) _cell_length_c 37.508(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7741.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3106 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 21.09 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 8.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4887 _exptl_absorpt_correction_T_max 0.6801 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39854 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8921 _reflns_number_gt 5214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^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 8921 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.54665(2) 0.14409(2) -0.003717(9) 0.03525(11) Uani 1 1 d . . . Br1 Br 0.72067(6) 0.08807(6) 0.01301(3) 0.0471(3) Uani 1 1 d . . . Br2 Br 0.40970(8) 0.16704(7) -0.04896(3) 0.0576(3) Uani 1 1 d . . . N1 N 0.5556(5) 0.2821(4) 0.02068(19) 0.0371(17) Uani 1 1 d . . . C1 C 0.4864(6) 0.3428(5) 0.0166(2) 0.038(2) Uani 1 1 d . . . H1 H 0.4269 0.3326 0.0020 0.046 Uiso 1 1 calc R . . C2 C 0.4952(6) 0.4184(5) 0.0321(2) 0.037(2) Uani 1 1 d . . . H2 H 0.4457 0.4605 0.0269 0.044 Uiso 1 1 calc R . . C3 C 0.5770(6) 0.4335(5) 0.0555(2) 0.0305(18) Uani 1 1 d . . . C4 C 0.6487(6) 0.3715(5) 0.0606(3) 0.048(2) Uani 1 1 d . . . H4 H 0.7072 0.3799 0.0758 0.058 Uiso 1 1 calc R . . C5 C 0.6356(7) 0.2971(6) 0.0435(3) 0.051(3) Uani 1 1 d . . . H5 H 0.6849 0.2543 0.0478 0.061 Uiso 1 1 calc R . . C6 C 0.5867(6) 0.5140(5) 0.0744(2) 0.035(2) Uani 1 1 d . . . O2 O 0.5312(4) 0.5731(3) 0.07108(16) 0.0409(14) Uani 1 1 d . . . O1 O 0.6686(4) 0.5076(3) 0.09732(14) 0.0336(13) Uani 1 1 d . . . C7 C 0.7073(5) 0.5722(5) 0.1186(2) 0.0309(18) Uani 1 1 d . . . C8 C 0.7078(6) 0.6549(5) 0.1094(2) 0.0317(19) Uani 1 1 d . . . H8 H 0.6724 0.6738 0.0886 0.038 Uiso 1 1 calc R . . C9 C 0.7614(6) 0.7095(5) 0.1313(2) 0.0308(18) Uani 1 1 d . . . H9 H 0.7616 0.7667 0.1255 0.037 Uiso 1 1 calc R . . C10 C 0.8154(5) 0.6828(4) 0.1617(2) 0.0255(17) Uani 1 1 d . . . C11 C 0.8090(6) 0.6003(5) 0.1710(2) 0.0292(18) Uani 1 1 d . . . H11 H 0.8409 0.5817 0.1925 0.035 Uiso 1 1 calc R . . C12 C 0.7569(6) 0.5447(5) 0.1496(2) 0.0336(19) Uani 1 1 d . . . H12 H 0.7547 0.4878 0.1559 0.040 Uiso 1 1 calc R . . C13 C 0.8722(5) 0.7454(4) 0.1857(2) 0.0263(17) Uani 1 1 d . . . C14 C 0.7951(5) 0.7883(4) 0.2113(2) 0.0252(17) Uani 1 1 d . . . C15 C 0.7063(6) 0.8330(4) 0.2021(2) 0.0296(18) Uani 1 1 d . . . H15 H 0.6855 0.8402 0.1780 0.036 Uiso 1 1 calc R . . C16 C 0.6495(6) 0.8669(5) 0.2303(3) 0.041(2) Uani 1 1 d . . . Br3 Br 0.52589(6) 0.92876(5) 0.21910(3) 0.0530(3) Uani 1 1 d . . . C17 C 0.6773(6) 0.8559(5) 0.2652(3) 0.042(2) Uani 1 1 d . . . H17 H 0.6359 0.8798 0.2835 0.050 Uiso 1 1 calc R . . C18 C 0.7653(6) 0.8103(5) 0.2739(2) 0.039(2) Uani 1 1 d . . . H18 H 0.7855 0.8025 0.2980 0.047 Uiso 1 1 calc R . . C19 C 0.8237(6) 0.7761(5) 0.2460(2) 0.0273(17) Uani 1 1 d . . . C20 C 0.9173(6) 0.7249(5) 0.2473(2) 0.0307(18) Uani 1 1 d . . . C21 C 0.9780(6) 0.6969(5) 0.2763(2) 0.037(2) Uani 1 1 d . . . H21 H 0.9589 0.7103 0.3001 0.044 Uiso 1 1 calc R . . C22 C 1.0655(6) 0.6498(5) 0.2694(3) 0.040(2) Uani 1 1 d . . . H22 H 1.1069 0.6304 0.2887 0.048 Uiso 1 1 calc R . . C23 C 1.0944(6) 0.6302(5) 0.2348(3) 0.038(2) Uani 1 1 d . . . Br4 Br 1.21299(6) 0.56250(6) 0.22673(3) 0.0510(3) Uani 1 1 d . . . C24 C 1.0363(6) 0.6587(5) 0.2055(2) 0.0335(19) Uani 1 1 d . . . H24 H 1.0572 0.6469 0.1817 0.040 Uiso 1 1 calc R . . C25 C 0.9468(5) 0.7051(4) 0.2128(2) 0.0266(17) Uani 1 1 d . . . C26 C 0.9392(5) 0.8062(5) 0.1635(2) 0.0259(17) Uani 1 1 d . . . C27 C 0.9509(6) 0.8878(5) 0.1730(2) 0.0323(18) Uani 1 1 d . . . H27 H 0.9097 0.9091 0.1920 0.039 Uiso 1 1 calc R . . C28 C 1.0216(6) 0.9408(5) 0.1555(2) 0.039(2) Uani 1 1 d . . . H28 H 1.0290 0.9970 0.1623 0.047 Uiso 1 1 calc R . . C29 C 1.0796(6) 0.9071(5) 0.1281(2) 0.038(2) Uani 1 1 d . . . C30 C 1.0686(6) 0.8267(6) 0.1176(2) 0.042(2) Uani 1 1 d . . . H30 H 1.1093 0.8058 0.0984 0.050 Uiso 1 1 calc R . . C31 C 0.9988(5) 0.7766(5) 0.1349(2) 0.0339(19) Uani 1 1 d . . . H31 H 0.9907 0.7210 0.1274 0.041 Uiso 1 1 calc R . . O3 O 1.1486(4) 0.9587(4) 0.10833(15) 0.0472(16) Uani 1 1 d . . . C32 C 0.2479(6) -0.0346(5) 0.1209(3) 0.035(2) Uani 1 1 d . . . O4 O 0.2770(4) -0.0627(4) 0.14868(19) 0.0574(18) Uani 1 1 d . . . C33 C 0.3118(6) 0.0129(5) 0.0944(2) 0.0321(18) Uani 1 1 d . . . C34 C 0.2708(6) 0.0527(5) 0.0654(2) 0.041(2) Uani 1 1 d . . . H34 H 0.1971 0.0533 0.0618 0.049 Uiso 1 1 calc R . . C35 C 0.3361(6) 0.0922(5) 0.0413(2) 0.040(2) Uani 1 1 d . . . H35 H 0.3059 0.1194 0.0214 0.048 Uiso 1 1 calc R . . N2 N 0.4421(5) 0.0932(4) 0.0453(2) 0.0407(18) Uani 1 1 d . . . C36 C 0.4814(6) 0.0547(6) 0.0738(2) 0.045(2) Uani 1 1 d . . . H36 H 0.5554 0.0546 0.0768 0.054 Uiso 1 1 calc R . . C37 C 0.4221(6) 0.0154(5) 0.0992(3) 0.045(2) Uani 1 1 d . . . H37 H 0.4540 -0.0095 0.1194 0.054 Uiso 1 1 calc R . . C38 C 0.3981(8) 0.7256(6) 0.1117(3) 0.057(3) Uani 1 1 d . . . H38 H 0.4507 0.6882 0.1002 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.4678(2) 0.80021(18) 0.13572(8) 0.0720(8) Uani 1 1 d . . . Cl2 Cl 0.32159(19) 0.76861(19) 0.07755(7) 0.0684(8) Uani 1 1 d . . . Cl3 Cl 0.3223(3) 0.6656(2) 0.14030(8) 0.0930(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02598(16) 0.03905(19) 0.0407(2) -0.00133(15) 0.00285(14) -0.00473(14) Br1 0.0284(4) 0.0529(6) 0.0600(7) -0.0067(5) 0.0017(4) 0.0067(4) Br2 0.0419(5) 0.0749(7) 0.0561(7) 0.0007(5) -0.0122(5) -0.0031(5) N1 0.027(4) 0.043(4) 0.042(5) -0.011(3) 0.003(3) -0.005(3) C1 0.033(4) 0.039(5) 0.043(5) 0.006(4) -0.014(4) -0.006(4) C2 0.030(4) 0.038(5) 0.043(6) 0.000(4) -0.009(4) 0.003(4) C3 0.023(4) 0.035(5) 0.033(5) -0.002(4) 0.004(3) -0.001(3) C4 0.020(4) 0.056(6) 0.068(7) -0.016(5) -0.014(4) 0.008(4) C5 0.034(5) 0.043(6) 0.075(8) -0.012(5) -0.021(5) 0.011(4) C6 0.021(4) 0.043(5) 0.042(6) 0.003(4) 0.005(4) -0.007(4) O2 0.027(3) 0.041(4) 0.055(4) -0.005(3) -0.004(3) -0.002(3) O1 0.028(3) 0.034(3) 0.039(4) -0.003(3) -0.010(2) 0.004(2) C7 0.021(4) 0.030(5) 0.042(5) -0.001(4) 0.000(3) -0.002(3) C8 0.027(4) 0.029(5) 0.039(5) 0.007(4) -0.002(3) -0.001(3) C9 0.031(4) 0.023(4) 0.038(5) 0.003(3) -0.003(4) 0.001(3) C10 0.017(4) 0.027(4) 0.032(5) -0.004(3) 0.003(3) -0.004(3) C11 0.030(4) 0.028(4) 0.030(5) 0.005(3) -0.003(3) -0.004(3) C12 0.034(4) 0.024(4) 0.043(6) 0.000(4) -0.004(4) 0.000(3) C13 0.022(4) 0.029(4) 0.028(5) -0.003(3) 0.002(3) -0.002(3) C14 0.023(4) 0.018(4) 0.035(5) -0.006(3) 0.003(3) -0.007(3) C15 0.024(4) 0.025(4) 0.039(5) 0.003(3) 0.005(3) 0.003(3) C16 0.015(4) 0.027(5) 0.081(8) -0.002(4) 0.009(4) 0.000(3) Br3 0.0278(4) 0.0380(5) 0.0931(8) 0.0087(5) 0.0169(5) 0.0093(4) C17 0.031(4) 0.039(5) 0.055(7) -0.015(5) 0.021(4) -0.011(4) C18 0.034(5) 0.038(5) 0.046(6) -0.004(4) 0.009(4) -0.008(4) C19 0.023(4) 0.028(4) 0.031(5) -0.002(3) 0.009(3) -0.005(3) C20 0.024(4) 0.027(4) 0.041(5) 0.002(4) 0.003(3) -0.007(3) C21 0.035(5) 0.043(5) 0.032(5) -0.003(4) -0.002(4) -0.006(4) C22 0.029(4) 0.043(5) 0.047(6) 0.018(4) -0.017(4) -0.008(4) C23 0.022(4) 0.028(5) 0.063(7) 0.003(4) -0.009(4) -0.002(3) Br4 0.0296(5) 0.0458(6) 0.0777(8) -0.0041(5) -0.0119(4) 0.0107(4) C24 0.023(4) 0.030(5) 0.047(5) 0.002(4) -0.003(4) -0.004(3) C25 0.020(4) 0.027(4) 0.033(5) 0.004(3) 0.000(3) -0.009(3) C26 0.017(4) 0.029(4) 0.031(5) 0.006(3) -0.009(3) -0.004(3) C27 0.025(4) 0.033(4) 0.039(5) 0.007(4) 0.000(4) 0.001(3) C28 0.028(4) 0.036(5) 0.053(6) 0.007(4) -0.009(4) -0.006(4) C29 0.017(4) 0.050(6) 0.045(6) 0.020(4) -0.007(4) -0.012(4) C30 0.025(4) 0.054(6) 0.046(6) 0.014(5) 0.007(4) 0.005(4) C31 0.022(4) 0.040(5) 0.039(5) 0.004(4) 0.005(4) 0.001(4) O3 0.023(3) 0.068(4) 0.050(4) 0.025(3) -0.003(3) -0.016(3) C32 0.017(4) 0.040(5) 0.047(6) 0.001(4) 0.007(4) -0.002(3) O4 0.032(3) 0.083(5) 0.058(5) 0.017(4) -0.005(3) -0.021(3) C33 0.022(4) 0.033(4) 0.041(5) -0.002(4) 0.009(3) -0.006(3) C34 0.026(4) 0.058(6) 0.038(6) 0.014(4) 0.000(4) -0.009(4) C35 0.031(5) 0.059(6) 0.032(5) 0.013(4) 0.004(4) 0.000(4) N2 0.021(4) 0.052(5) 0.049(5) 0.001(4) 0.011(3) -0.007(3) C36 0.020(4) 0.066(6) 0.048(6) 0.016(5) 0.008(4) -0.006(4) C37 0.024(4) 0.054(6) 0.056(7) 0.017(5) 0.000(4) -0.005(4) C38 0.068(7) 0.066(7) 0.036(6) -0.004(5) -0.003(5) -0.001(5) Cl1 0.0728(19) 0.079(2) 0.065(2) 0.0090(15) -0.0040(14) -0.0152(15) Cl2 0.0382(13) 0.106(2) 0.0607(18) 0.0178(16) 0.0056(12) 0.0044(14) Cl3 0.142(3) 0.083(2) 0.054(2) 0.0080(16) -0.0149(19) -0.052(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N2 2.417(7) . ? Hg1 N1 2.418(7) . ? Hg1 Br2 2.4631(10) . ? Hg1 Br1 2.4777(9) . ? N1 C1 1.329(10) . ? N1 C5 1.352(10) . ? C1 C2 1.360(11) . ? C1 H1 0.9500 . ? C2 C3 1.385(10) . ? C2 H2 0.9500 . ? C3 C4 1.370(10) . ? C3 C6 1.489(11) . ? C4 C5 1.375(11) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O2 1.197(9) . ? C6 O1 1.356(9) . ? O1 C7 1.404(9) . ? C7 C8 1.383(10) . ? C7 C12 1.399(11) . ? C8 C9 1.388(10) . ? C8 H8 0.9500 . ? C9 C10 1.401(10) . ? C9 H9 0.9500 . ? C10 C11 1.383(10) . ? C10 C13 1.537(10) . ? C11 C12 1.376(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C25 1.536(10) . ? C13 C14 1.540(10) . ? C13 C26 1.547(10) . ? C14 C19 1.366(10) . ? C14 C15 1.386(10) . ? C15 C16 1.393(11) . ? C15 H15 0.9500 . ? C16 C17 1.368(12) . ? C16 Br3 1.913(8) . ? C17 C18 1.382(12) . ? C17 H17 0.9500 . ? C18 C19 1.399(10) . ? C18 H18 0.9500 . ? C19 C20 1.454(10) . ? C20 C25 1.386(11) . ? C20 C21 1.408(11) . ? C21 C22 1.375(11) . ? C21 H21 0.9500 . ? C22 C23 1.385(12) . ? C22 H22 0.9500 . ? C23 C24 1.405(11) . ? C23 Br4 1.892(8) . ? C24 C25 1.394(10) . ? C24 H24 0.9500 . ? C26 C27 1.375(11) . ? C26 C31 1.399(10) . ? C27 C28 1.405(10) . ? C27 H27 0.9500 . ? C28 C29 1.379(12) . ? C28 H28 0.9500 . ? C29 C30 1.366(12) . ? C29 O3 1.423(9) . ? C30 C31 1.368(10) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O3 C32 1.355(9) 1_665 ? C32 O4 1.195(10) . ? C32 O3 1.355(9) 1_445 ? C32 C33 1.500(11) . ? C33 C34 1.366(11) . ? C33 C37 1.418(10) . ? C34 C35 1.385(10) . ? C34 H34 0.9500 . ? C35 N2 1.360(9) . ? C35 H35 0.9500 . ? N2 C36 1.334(11) . ? C36 C37 1.370(11) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 Cl3 1.741(10) . ? C38 Cl1 1.750(10) . ? C38 Cl2 1.753(10) . ? C38 H38 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Hg1 N1 93.1(2) . . ? N2 Hg1 Br2 100.66(17) . . ? N1 Hg1 Br2 98.91(17) . . ? N2 Hg1 Br1 100.15(17) . . ? N1 Hg1 Br1 101.55(16) . . ? Br2 Hg1 Br1 149.83(4) . . ? C1 N1 C5 116.2(7) . . ? C1 N1 Hg1 127.4(5) . . ? C5 N1 Hg1 116.1(5) . . ? N1 C1 C2 124.1(8) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 C2 C3 119.4(7) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 117.5(7) . . ? C4 C3 C6 121.3(7) . . ? C2 C3 C6 121.2(7) . . ? C3 C4 C5 119.7(8) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 122.9(8) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? O2 C6 O1 125.6(8) . . ? O2 C6 C3 126.9(8) . . ? O1 C6 C3 107.4(7) . . ? C6 O1 C7 125.0(6) . . ? C8 C7 C12 120.9(7) . . ? C8 C7 O1 125.5(7) . . ? C12 C7 O1 113.3(7) . . ? C7 C8 C9 118.1(7) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C8 C9 C10 121.8(7) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 118.4(7) . . ? C11 C10 C13 121.1(7) . . ? C9 C10 C13 120.3(7) . . ? C12 C11 C10 120.9(7) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C7 119.7(7) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C25 C13 C10 113.5(6) . . ? C25 C13 C14 100.1(6) . . ? C10 C13 C14 111.2(6) . . ? C25 C13 C26 106.5(5) . . ? C10 C13 C26 111.4(6) . . ? C14 C13 C26 113.6(6) . . ? C19 C14 C15 122.0(7) . . ? C19 C14 C13 110.9(6) . . ? C15 C14 C13 127.1(7) . . ? C14 C15 C16 116.3(8) . . ? C14 C15 H15 121.9 . . ? C16 C15 H15 121.9 . . ? C17 C16 C15 122.6(7) . . ? C17 C16 Br3 119.4(6) . . ? C15 C16 Br3 117.9(7) . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 117.8(8) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C14 C19 C18 120.9(7) . . ? C14 C19 C20 109.6(7) . . ? C18 C19 C20 129.5(8) . . ? C25 C20 C21 119.8(7) . . ? C25 C20 C19 108.8(7) . . ? C21 C20 C19 131.4(8) . . ? C22 C21 C20 118.7(8) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 121.2(8) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 121.3(7) . . ? C22 C23 Br4 119.7(6) . . ? C24 C23 Br4 119.0(7) . . ? C25 C24 C23 117.0(8) . . ? C25 C24 H24 121.5 . . ? C23 C24 H24 121.5 . . ? C20 C25 C24 122.1(7) . . ? C20 C25 C13 110.6(6) . . ? C24 C25 C13 127.2(7) . . ? C27 C26 C31 117.8(7) . . ? C27 C26 C13 122.2(7) . . ? C31 C26 C13 119.6(7) . . ? C26 C27 C28 122.4(8) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 116.7(8) . . ? C29 C28 H28 121.7 . . ? C27 C28 H28 121.7 . . ? C30 C29 C28 122.5(8) . . ? C30 C29 O3 118.2(8) . . ? C28 C29 O3 119.2(8) . . ? C29 C30 C31 119.7(8) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C26 120.9(8) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C32 O3 C29 116.2(6) 1_665 . ? O4 C32 O3 124.4(7) . 1_445 ? O4 C32 C33 127.2(7) . . ? O3 C32 C33 108.5(7) 1_445 . ? C34 C33 C37 117.8(7) . . ? C34 C33 C32 124.2(7) . . ? C37 C33 C32 118.0(8) . . ? C33 C34 C35 120.4(7) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? N2 C35 C34 122.1(8) . . ? N2 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C36 N2 C35 117.1(7) . . ? C36 N2 Hg1 124.2(5) . . ? C35 N2 Hg1 117.9(6) . . ? N2 C36 C37 124.4(8) . . ? N2 C36 H36 117.8 . . ? C37 C36 H36 117.8 . . ? C36 C37 C33 118.2(8) . . ? C36 C37 H37 120.9 . . ? C33 C37 H37 120.9 . . ? Cl3 C38 Cl1 110.4(5) . . ? Cl3 C38 Cl2 111.2(6) . . ? Cl1 C38 Cl2 112.6(6) . . ? Cl3 C38 H38 107.5 . . ? Cl1 C38 H38 107.5 . . ? Cl2 C38 H38 107.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.897 _refine_diff_density_min -3.177 _refine_diff_density_rms 0.195 # Attachment 'CIF For 5-HgCl2.cif' data_e480a _database_code_depnum_ccdc_archive 'CCDC 617747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br2 Cl2 Hg N2 O4, C H Cl3' _chemical_formula_sum 'C38 H23 Br2 Cl5 Hg N2 O4' _chemical_formula_weight 1109.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.6080(9) _cell_length_b 16.2385(13) _cell_length_c 37.085(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7592.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8453 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 23.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 6.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6569 _exptl_absorpt_correction_T_max 0.7352 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61869 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8745 _reflns_number_gt 5395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+19.8504P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8745 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.943521(19) 1.355464(15) 1.006643(7) 0.03242(8) Uani 1 1 d . . . Cl1 Cl 1.07994(14) 1.33167(13) 1.04856(5) 0.0526(5) Uani 1 1 d . . . Cl2 Cl 0.77599(13) 1.40458(11) 0.98901(5) 0.0438(4) Uani 1 1 d . . . N1 N 0.9360(4) 1.2173(3) 0.98231(13) 0.0303(12) Uani 1 1 d . . . C1 C 0.8516(5) 1.1985(4) 0.96251(18) 0.0374(17) Uani 1 1 d . . . H1 H 0.7972 1.2385 0.9600 0.045 Uiso 1 1 calc R . . C2 C 0.8390(5) 1.1239(4) 0.94545(17) 0.0352(16) Uani 1 1 d . . . H2 H 0.7766 1.1125 0.9320 0.042 Uiso 1 1 calc R . . C3 C 0.9181(5) 1.0663(4) 0.94820(15) 0.0258(13) Uani 1 1 d . . . C4 C 1.0056(5) 1.0839(4) 0.96895(16) 0.0294(15) Uani 1 1 d . . . H4 H 1.0609 1.0448 0.9718 0.035 Uiso 1 1 calc R . . C5 C 1.0108(5) 1.1598(4) 0.98549(16) 0.0333(16) Uani 1 1 d . . . H5 H 1.0711 1.1718 0.9999 0.040 Uiso 1 1 calc R . . C6 C 0.9099(5) 0.9863(4) 0.92826(16) 0.0262(14) Uani 1 1 d . . . O1 O 0.9698(3) 0.9285(3) 0.93104(12) 0.0365(11) Uani 1 1 d . . . O2 O 0.8259(3) 0.9900(2) 0.90574(11) 0.0310(10) Uani 1 1 d . . . C7 C 0.7903(4) 0.9257(4) 0.88350(16) 0.0253(13) Uani 1 1 d . . . C8 C 0.7907(5) 0.8440(4) 0.89342(15) 0.0285(14) Uani 1 1 d . . . H8 H 0.8252 0.8261 0.9148 0.034 Uiso 1 1 calc R . . C9 C 0.7383(5) 0.7885(4) 0.87079(15) 0.0275(14) Uani 1 1 d . . . H9 H 0.7386 0.7317 0.8769 0.033 Uiso 1 1 calc R . . C10 C 0.6861(4) 0.8133(4) 0.83978(15) 0.0228(13) Uani 1 1 d . . . C11 C 0.6920(5) 0.8960(4) 0.83041(16) 0.0269(14) Uani 1 1 d . . . H11 H 0.6606 0.9142 0.8085 0.032 Uiso 1 1 calc R . . C12 C 0.7424(5) 0.9516(4) 0.85224(16) 0.0287(14) Uani 1 1 d . . . H12 H 0.7442 1.0082 0.8458 0.034 Uiso 1 1 calc R . . C13 C 0.6286(4) 0.7506(3) 0.81602(14) 0.0205(12) Uani 1 1 d . . . C14 C 0.5540(4) 0.7900(3) 0.78836(15) 0.0236(13) Uani 1 1 d . . . C15 C 0.4640(4) 0.8372(3) 0.79482(16) 0.0268(14) Uani 1 1 d . . . H15 H 0.4423 0.8501 0.8187 0.032 Uiso 1 1 calc R . . C16 C 0.4067(5) 0.8648(4) 0.76495(18) 0.0328(15) Uani 1 1 d . . . Br1 Br 0.28610(5) 0.93253(5) 0.77281(2) 0.0486(2) Uani 1 1 d . . . C17 C 0.4361(5) 0.8449(4) 0.73013(17) 0.0354(16) Uani 1 1 d . . . H17 H 0.3950 0.8641 0.7104 0.043 Uiso 1 1 calc R . . C18 C 0.5242(5) 0.7974(4) 0.72399(18) 0.0378(17) Uani 1 1 d . . . H18 H 0.5447 0.7838 0.7001 0.045 Uiso 1 1 calc R . . C19 C 0.5831(5) 0.7693(3) 0.75322(15) 0.0259(14) Uani 1 1 d . . . C20 C 0.6782(5) 0.7184(4) 0.75483(16) 0.0271(14) Uani 1 1 d . . . C21 C 0.7392(5) 0.6826(4) 0.72758(18) 0.0392(17) Uani 1 1 d . . . H21 H 0.7199 0.6891 0.7030 0.047 Uiso 1 1 calc R . . C22 C 0.8269(5) 0.6379(4) 0.73675(19) 0.0400(17) Uani 1 1 d . . . H22 H 0.8691 0.6138 0.7183 0.048 Uiso 1 1 calc R . . C23 C 0.8547(5) 0.6274(4) 0.7720(2) 0.0359(17) Uani 1 1 d . . . C24 C 0.7959(5) 0.6623(3) 0.80019(17) 0.0286(14) Uani 1 1 d . . . H24 H 0.8164 0.6555 0.8247 0.034 Uiso 1 1 calc R . . Br2 Br 0.97900(6) 0.56676(5) 0.78394(2) 0.0560(2) Uani 1 1 d . . . C25 C 0.7076(4) 0.7065(3) 0.79098(16) 0.0233(13) Uani 1 1 d . . . C26 C 0.5614(4) 0.6902(4) 0.83827(14) 0.0227(12) Uani 1 1 d . . . C27 C 0.5482(5) 0.6088(4) 0.82836(16) 0.0289(14) Uani 1 1 d . . . H27 H 0.5885 0.5873 0.8089 0.035 Uiso 1 1 calc R . . C28 C 0.4763(5) 0.5572(4) 0.84661(17) 0.0326(15) Uani 1 1 d . . . H28 H 0.4686 0.5009 0.8402 0.039 Uiso 1 1 calc R . . C29 C 0.4179(5) 0.5910(4) 0.87387(17) 0.0355(17) Uani 1 1 d . . . C30 C 0.4303(5) 0.6707(4) 0.88483(18) 0.0404(17) Uani 1 1 d . . . H30 H 0.3899 0.6918 0.9044 0.048 Uiso 1 1 calc R . . C31 C 0.5023(5) 0.7202(4) 0.86705(17) 0.0351(16) Uani 1 1 d . . . H31 H 0.5116 0.7756 0.8746 0.042 Uiso 1 1 calc R . . O3 O 0.3471(3) 0.5410(3) 0.89407(12) 0.0452(13) Uani 1 1 d . . . C32 C 0.2483(5) 0.5320(4) 0.88128(18) 0.0349(16) Uani 1 1 d . . . O4 O 0.2197(4) 0.5577(3) 0.85279(13) 0.0564(15) Uani 1 1 d . . . C33 C 0.1803(5) 0.4872(4) 0.90785(17) 0.0310(15) Uani 1 1 d . . . C34 C 0.0715(5) 0.4829(4) 0.9024(2) 0.0442(18) Uani 1 1 d . . . H34 H 0.0402 0.5066 0.8815 0.053 Uiso 1 1 calc R . . C35 C 0.0100(5) 0.4439(4) 0.92771(19) 0.0422(18) Uani 1 1 d . . . H35 H -0.0643 0.4406 0.9238 0.051 Uiso 1 1 calc R . . N2 N 0.0500(4) 0.4104(3) 0.95761(14) 0.0353(13) Uani 1 1 d . . . C36 C 0.1545(6) 0.4137(4) 0.96217(18) 0.0432(18) Uani 1 1 d . . . H36 H 0.1839 0.3893 0.9832 0.052 Uiso 1 1 calc R . . C37 C 0.2223(5) 0.4508(4) 0.93785(18) 0.0412(18) Uani 1 1 d . . . H37 H 0.2967 0.4510 0.9419 0.049 Uiso 1 1 calc R . . C38 C 0.8980(7) 0.2202(5) 0.1096(2) 0.059(2) Uani 1 1 d . . . H38 H 0.9533 0.1838 0.0985 0.070 Uiso 1 1 calc R . . Cl3 Cl 0.9622(2) 0.30027(16) 0.13349(6) 0.0840(8) Uani 1 1 d . . . Cl4 Cl 0.81773(16) 0.25887(16) 0.07532(6) 0.0752(7) Uani 1 1 d . . . Cl5 Cl 0.8229(3) 0.16186(15) 0.13996(6) 0.0935(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02778(13) 0.03335(14) 0.03613(13) -0.00210(12) 0.00513(11) -0.00606(12) Cl1 0.0382(10) 0.0715(14) 0.0481(11) -0.0013(9) -0.0070(8) -0.0090(9) Cl2 0.0311(9) 0.0457(11) 0.0545(11) -0.0074(9) 0.0038(8) 0.0050(8) N1 0.028(3) 0.032(3) 0.031(3) -0.004(2) 0.002(2) -0.002(2) C1 0.028(4) 0.031(4) 0.053(4) -0.010(3) -0.007(3) 0.008(3) C2 0.026(4) 0.037(4) 0.043(4) -0.012(3) -0.008(3) 0.000(3) C3 0.026(3) 0.026(3) 0.025(3) 0.000(3) 0.004(3) 0.000(3) C4 0.027(3) 0.032(4) 0.030(4) -0.005(3) -0.004(3) 0.001(3) C5 0.032(4) 0.041(4) 0.027(4) -0.004(3) -0.007(3) -0.004(3) C6 0.023(3) 0.028(4) 0.027(3) -0.002(3) 0.002(3) -0.005(3) O1 0.034(3) 0.033(3) 0.042(3) -0.006(2) -0.005(2) 0.004(2) O2 0.033(2) 0.025(2) 0.035(2) -0.0033(19) -0.009(2) 0.0028(19) C7 0.025(3) 0.022(3) 0.028(3) -0.004(3) -0.005(3) -0.001(3) C8 0.032(3) 0.030(4) 0.023(3) 0.000(3) -0.004(3) -0.001(3) C9 0.030(3) 0.022(3) 0.030(3) 0.005(3) -0.001(3) 0.001(3) C10 0.017(3) 0.022(3) 0.029(3) -0.003(3) 0.001(2) 0.001(2) C11 0.027(3) 0.024(3) 0.029(3) 0.006(3) -0.004(3) -0.001(3) C12 0.034(4) 0.020(3) 0.031(4) 0.002(3) -0.001(3) -0.006(3) C13 0.018(3) 0.023(3) 0.021(3) -0.002(2) 0.004(2) 0.001(2) C14 0.024(3) 0.017(3) 0.029(3) -0.003(2) 0.000(3) -0.007(3) C15 0.027(3) 0.023(3) 0.031(3) 0.001(3) -0.005(3) 0.000(3) C16 0.031(3) 0.020(3) 0.048(4) 0.001(3) -0.004(3) -0.006(3) Br1 0.0356(4) 0.0396(4) 0.0705(5) -0.0008(4) -0.0150(3) 0.0083(3) C17 0.044(4) 0.028(4) 0.034(4) 0.009(3) -0.017(3) -0.006(3) C18 0.045(4) 0.039(4) 0.030(4) 0.003(3) -0.002(3) -0.008(3) C19 0.029(3) 0.025(3) 0.024(3) -0.001(3) -0.001(3) -0.010(3) C20 0.028(3) 0.024(3) 0.030(4) 0.002(3) 0.007(3) -0.009(3) C21 0.039(4) 0.036(4) 0.043(4) -0.008(3) 0.010(3) -0.007(3) C22 0.037(4) 0.031(4) 0.052(4) -0.015(3) 0.022(3) -0.008(3) C23 0.025(3) 0.017(3) 0.066(5) 0.001(3) 0.011(3) -0.001(3) C24 0.026(3) 0.019(3) 0.041(4) 0.001(3) 0.010(3) -0.006(3) Br2 0.0357(4) 0.0323(4) 0.1001(7) 0.0085(4) 0.0235(4) 0.0098(3) C25 0.023(3) 0.013(3) 0.034(3) -0.001(2) 0.005(3) -0.005(2) C26 0.018(3) 0.030(3) 0.021(3) 0.004(2) 0.000(3) -0.002(3) C27 0.032(4) 0.028(3) 0.027(3) 0.006(3) -0.001(3) -0.005(3) C28 0.026(3) 0.035(4) 0.037(4) 0.014(3) -0.005(3) -0.011(3) C29 0.025(4) 0.046(5) 0.036(4) 0.018(3) -0.003(3) -0.011(3) C30 0.032(4) 0.055(5) 0.034(4) 0.013(3) 0.009(3) 0.008(3) C31 0.034(4) 0.036(4) 0.036(4) 0.004(3) 0.003(3) -0.005(3) O3 0.026(3) 0.059(3) 0.051(3) 0.031(2) -0.001(2) -0.015(2) C32 0.029(4) 0.036(4) 0.039(4) 0.011(3) 0.001(3) -0.005(3) O4 0.036(3) 0.088(4) 0.045(3) 0.027(3) -0.001(2) -0.014(3) C33 0.024(3) 0.032(4) 0.037(4) 0.003(3) 0.002(3) -0.006(3) C34 0.029(4) 0.046(4) 0.057(5) 0.020(4) -0.003(3) -0.003(3) C35 0.029(4) 0.047(5) 0.051(5) 0.012(4) 0.010(3) 0.001(3) N2 0.028(3) 0.038(3) 0.040(3) 0.004(3) 0.010(3) -0.009(3) C36 0.041(4) 0.054(5) 0.034(4) 0.012(3) -0.001(3) -0.015(4) C37 0.035(4) 0.048(5) 0.041(4) 0.006(3) 0.003(3) -0.016(3) C38 0.067(5) 0.062(6) 0.047(5) -0.004(4) -0.001(4) 0.009(4) Cl3 0.116(2) 0.0829(18) 0.0532(13) 0.0103(12) 0.0021(13) -0.0246(15) Cl4 0.0439(12) 0.124(2) 0.0581(13) 0.0325(13) 0.0064(10) 0.0051(13) Cl5 0.152(3) 0.0777(18) 0.0504(13) 0.0128(12) -0.0187(15) -0.0498(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl1 2.3504(18) . ? Hg1 Cl2 2.3505(17) . ? Hg1 N1 2.421(5) . ? Hg1 N2 2.431(5) 1_665 ? N1 C1 1.329(8) . ? N1 C5 1.332(8) . ? C1 C2 1.375(8) . ? C1 H1 0.9500 . ? C2 C3 1.371(8) . ? C2 H2 0.9500 . ? C3 C4 1.374(8) . ? C3 C6 1.499(8) . ? C4 C5 1.378(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.208(7) . ? C6 O2 1.351(7) . ? O2 C7 1.405(7) . ? C7 C12 1.373(8) . ? C7 C8 1.376(8) . ? C8 C9 1.397(8) . ? C8 H8 0.9500 . ? C9 C10 1.385(8) . ? C9 H9 0.9500 . ? C10 C11 1.389(8) . ? C10 C13 1.529(8) . ? C11 C12 1.369(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.531(8) . ? C13 C26 1.536(7) . ? C13 C25 1.539(7) . ? C14 C15 1.390(8) . ? C14 C19 1.395(8) . ? C15 C16 1.396(8) . ? C15 H15 0.9500 . ? C16 C17 1.382(9) . ? C16 Br1 1.899(6) . ? C17 C18 1.372(9) . ? C17 H17 0.9500 . ? C18 C19 1.391(8) . ? C18 H18 0.9500 . ? C19 C20 1.457(8) . ? C20 C21 1.397(8) . ? C20 C25 1.404(8) . ? C21 C22 1.365(10) . ? C21 H21 0.9500 . ? C22 C23 1.365(9) . ? C22 H22 0.9500 . ? C23 C24 1.400(9) . ? C23 Br2 1.903(6) . ? C24 C25 1.368(8) . ? C24 H24 0.9500 . ? C26 C27 1.382(8) . ? C26 C31 1.389(8) . ? C27 C28 1.409(8) . ? C27 H27 0.9500 . ? C28 C29 1.365(9) . ? C28 H28 0.9500 . ? C29 C30 1.367(10) . ? C29 O3 1.421(7) . ? C30 C31 1.380(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O3 C32 1.341(7) . ? C32 O4 1.192(7) . ? C32 C33 1.494(8) . ? C33 C37 1.367(9) . ? C33 C34 1.388(8) . ? C34 C35 1.372(9) . ? C34 H34 0.9500 . ? C35 N2 1.334(8) . ? C35 H35 0.9500 . ? N2 C36 1.329(8) . ? N2 Hg1 2.431(5) 1_445 ? C36 C37 1.381(9) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 Cl4 1.741(8) . ? C38 Cl5 1.751(8) . ? C38 Cl3 1.770(8) . ? C38 H38 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 Cl2 153.81(7) . . ? Cl1 Hg1 N1 97.05(13) . . ? Cl2 Hg1 N1 100.13(13) . . ? Cl1 Hg1 N2 98.68(14) . 1_665 ? Cl2 Hg1 N2 99.43(14) . 1_665 ? N1 Hg1 N2 94.76(17) . 1_665 ? C1 N1 C5 117.1(5) . . ? C1 N1 Hg1 116.7(4) . . ? C5 N1 Hg1 126.1(4) . . ? N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.8(6) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 C6 120.3(5) . . ? C4 C3 C6 120.8(5) . . ? C3 C4 C5 118.3(6) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 123.6(6) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? O1 C6 O2 125.3(5) . . ? O1 C6 C3 126.0(6) . . ? O2 C6 C3 108.7(5) . . ? C6 O2 C7 125.5(5) . . ? C12 C7 C8 121.5(5) . . ? C12 C7 O2 114.1(5) . . ? C8 C7 O2 123.9(5) . . ? C7 C8 C9 117.3(5) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 122.4(6) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 117.6(5) . . ? C9 C10 C13 120.7(5) . . ? C11 C10 C13 121.6(5) . . ? C12 C11 C10 121.0(6) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 120.1(6) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C10 C13 C14 113.5(5) . . ? C10 C13 C26 112.1(5) . . ? C14 C13 C26 106.7(4) . . ? C10 C13 C25 110.5(4) . . ? C14 C13 C25 100.8(4) . . ? C26 C13 C25 112.6(5) . . ? C15 C14 C19 120.5(5) . . ? C15 C14 C13 128.0(5) . . ? C19 C14 C13 111.3(5) . . ? C14 C15 C16 117.6(6) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? C17 C16 C15 121.8(6) . . ? C17 C16 Br1 119.6(5) . . ? C15 C16 Br1 118.6(5) . . ? C18 C17 C16 120.2(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.2(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C14 120.6(6) . . ? C18 C19 C20 131.1(6) . . ? C14 C19 C20 108.3(5) . . ? C21 C20 C25 119.2(6) . . ? C21 C20 C19 131.3(6) . . ? C25 C20 C19 109.6(5) . . ? C22 C21 C20 119.1(6) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.9(6) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C24 121.9(6) . . ? C22 C23 Br2 119.9(5) . . ? C24 C23 Br2 118.2(5) . . ? C25 C24 C23 117.2(6) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.4 . . ? C24 C25 C20 121.7(5) . . ? C24 C25 C13 128.4(5) . . ? C20 C25 C13 109.9(5) . . ? C27 C26 C31 118.4(5) . . ? C27 C26 C13 122.2(5) . . ? C31 C26 C13 119.0(5) . . ? C26 C27 C28 121.2(6) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 117.7(6) . . ? C29 C28 H28 121.2 . . ? C27 C28 H28 121.2 . . ? C28 C29 C30 122.6(6) . . ? C28 C29 O3 120.0(6) . . ? C30 C29 O3 117.2(6) . . ? C29 C30 C31 119.0(6) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C26 121.1(6) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? C32 O3 C29 117.4(5) . . ? O4 C32 O3 123.8(6) . . ? O4 C32 C33 125.6(6) . . ? O3 C32 C33 110.6(5) . . ? C37 C33 C34 118.6(6) . . ? C37 C33 C32 121.7(6) . . ? C34 C33 C32 119.7(6) . . ? C35 C34 C33 118.8(6) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N2 C35 C34 122.9(6) . . ? N2 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C36 N2 C35 117.7(6) . . ? C36 N2 Hg1 117.8(4) . 1_445 ? C35 N2 Hg1 124.2(4) . 1_445 ? N2 C36 C37 123.2(6) . . ? N2 C36 H36 118.4 . . ? C37 C36 H36 118.4 . . ? C33 C37 C36 118.7(6) . . ? C33 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? Cl4 C38 Cl5 110.5(5) . . ? Cl4 C38 Cl3 111.5(5) . . ? Cl5 C38 Cl3 108.8(4) . . ? Cl4 C38 H38 108.7 . . ? Cl5 C38 H38 108.7 . . ? Cl3 C38 H38 108.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.615 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.147 # Attachment 'CIF For 5-HgI2.cif' data_e670a _database_code_depnum_ccdc_archive 'CCDC 617748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br2 Hg I2 N2 O4, C H Cl3' _chemical_formula_sum 'C38 H23 Br2 Cl3 Hg I2 N2 O4' _chemical_formula_weight 1292.14 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.741(3) _cell_length_b 15.790(3) _cell_length_c 40.525(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8153(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4832 _exptl_absorpt_coefficient_mu 7.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4669 _exptl_absorpt_correction_T_max 0.5214 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82893 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9304 _reflns_number_gt 6185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^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 9304 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.672409(16) 1.168270(12) -0.007463(5) 0.02883(7) Uani 1 1 d . . 1 I1 I 0.56140(3) 1.28810(2) -0.036182(10) 0.04357(12) Uani 1 1 d . . 1 I2 I 0.81470(3) 1.04711(2) -0.010628(10) 0.04152(11) Uani 1 1 d . . 1 N1 N 0.5351(3) 1.1027(2) 0.02854(10) 0.0279(10) Uani 1 1 d . . 1 C1 C 0.5448(4) 1.0216(3) 0.03819(13) 0.0322(13) Uani 1 1 d . . 1 H1 H 0.6013 0.9892 0.0296 0.039 Uiso 1 1 calc R . 1 C2 C 0.4761(4) 0.9829(3) 0.06025(13) 0.0269(12) Uani 1 1 d . . 1 H2 H 0.4858 0.9257 0.0669 0.032 Uiso 1 1 calc R . 1 C3 C 0.3927(4) 1.0306(3) 0.07229(12) 0.0246(12) Uani 1 1 d . . 1 C4 C 0.3803(4) 1.1138(3) 0.06161(13) 0.0315(13) Uani 1 1 d . . 1 H4 H 0.3231 1.1472 0.0692 0.038 Uiso 1 1 calc R . 1 C5 C 0.4532(4) 1.1469(3) 0.03973(14) 0.0364(14) Uani 1 1 d . . 1 H5 H 0.4444 1.2036 0.0324 0.044 Uiso 1 1 calc R . 1 C6 C 0.3145(4) 0.9947(3) 0.09678(13) 0.0276(12) Uani 1 1 d . . 1 O1 O 0.2385(3) 1.0311(2) 0.10607(9) 0.0353(9) Uani 1 1 d . . 1 O2 O 0.3442(2) 0.9154(2) 0.10595(8) 0.0276(8) Uani 1 1 d . . 1 C7 C 0.2816(4) 0.8672(3) 0.12795(14) 0.0251(12) Uani 1 1 d . . 1 C8 C 0.2351(3) 0.9007(3) 0.15606(12) 0.0214(11) Uani 1 1 d . . 1 H8 H 0.2413 0.9593 0.1611 0.026 Uiso 1 1 calc R . 1 C9 C 0.1790(3) 0.8463(3) 0.17682(13) 0.0236(12) Uani 1 1 d . . 1 H9 H 0.1476 0.8682 0.1963 0.028 Uiso 1 1 calc R . 1 C10 C 0.1683(3) 0.7603(3) 0.16943(12) 0.0194(11) Uani 1 1 d . . 1 C11 C 0.2196(4) 0.7291(3) 0.14153(13) 0.0269(12) Uani 1 1 d . . 1 H11 H 0.2158 0.6703 0.1368 0.032 Uiso 1 1 calc R . 1 C12 C 0.2752(4) 0.7810(3) 0.12074(13) 0.0298(13) Uani 1 1 d . . 1 H12 H 0.3088 0.7585 0.1017 0.036 Uiso 1 1 calc R . 1 C13 C 0.1131(3) 0.6994(3) 0.19330(11) 0.0168(10) Uani 1 1 d . . 1 C14 C 0.0371(3) 0.7445(3) 0.21732(13) 0.0220(12) Uani 1 1 d . . 1 C15 C -0.0509(3) 0.7919(3) 0.20988(13) 0.0247(12) Uani 1 1 d . . 1 H15 H -0.0713 0.8013 0.1876 0.030 Uiso 1 1 calc R . 1 C16 C -0.1085(4) 0.8254(3) 0.23567(15) 0.0274(13) Uani 1 1 d . . 1 Br1 Br -0.22782(4) 0.89398(4) 0.226421(18) 0.05068(19) Uani 1 1 d . . 1 C17 C -0.0814(4) 0.8110(3) 0.26856(15) 0.0325(14) Uani 1 1 d . . 1 H17 H -0.1238 0.8332 0.2858 0.039 Uiso 1 1 calc R . 1 C18 C 0.0079(4) 0.7640(3) 0.27610(14) 0.0304(13) Uani 1 1 d . . 1 H18 H 0.0282 0.7549 0.2984 0.036 Uiso 1 1 calc R . 1 C19 C 0.0669(4) 0.7304(3) 0.25020(13) 0.0226(12) Uani 1 1 d . . 1 C20 C 0.1631(4) 0.6810(3) 0.25067(13) 0.0229(12) Uani 1 1 d . . 1 C21 C 0.2246(4) 0.6519(3) 0.27702(14) 0.0285(13) Uani 1 1 d . . 1 H21 H 0.2049 0.6636 0.2992 0.034 Uiso 1 1 calc R . 1 C22 C 0.3145(4) 0.6057(3) 0.27019(14) 0.0279(13) Uani 1 1 d . . 1 H22 H 0.3575 0.5859 0.2877 0.033 Uiso 1 1 calc R . 1 C23 C 0.3414(3) 0.5887(3) 0.23775(14) 0.0269(13) Uani 1 1 d . . 1 Br2 Br 0.46282(4) 0.52067(3) 0.228955(16) 0.03962(16) Uani 1 1 d . . 1 C24 C 0.2826(4) 0.6164(3) 0.21120(14) 0.0241(12) Uani 1 1 d . . 1 H24 H 0.3028 0.6042 0.1891 0.029 Uiso 1 1 calc R . 1 C25 C 0.1928(3) 0.6629(3) 0.21816(13) 0.0201(11) Uani 1 1 d . . 1 C26 C 0.0520(3) 0.6293(3) 0.17496(12) 0.0165(10) Uani 1 1 d . . 1 C27 C 0.0547(3) 0.5452(3) 0.18508(12) 0.0218(11) Uani 1 1 d . . 1 H27 H 0.0981 0.5300 0.2032 0.026 Uiso 1 1 calc R . 1 C28 C -0.0046(4) 0.4821(3) 0.16943(13) 0.0268(12) Uani 1 1 d . . 1 H28 H -0.0017 0.4249 0.1766 0.032 Uiso 1 1 calc R . 1 C29 C -0.0673(4) 0.5057(3) 0.14319(13) 0.0251(12) Uani 1 1 d . . 1 C30 C -0.0746(4) 0.5894(3) 0.13333(13) 0.0295(13) Uani 1 1 d . . 1 H30 H -0.1208 0.6051 0.1160 0.035 Uiso 1 1 calc R . 1 C31 C -0.0139(4) 0.6502(3) 0.14894(13) 0.0261(12) Uani 1 1 d . . 1 H31 H -0.0175 0.7073 0.1417 0.031 Uiso 1 1 calc R . 1 O3 O -0.1286(2) 0.44929(19) 0.12384(8) 0.0292(8) Uani 1 1 d . . 1 C32 C -0.1290(5) 0.3638(3) 0.12720(16) 0.0393(15) Uani 1 1 d . . 1 O4 O -0.0906(5) 0.3256(3) 0.14890(13) 0.095(2) Uani 1 1 d . . 1 C33 C -0.1858(4) 0.3234(3) 0.09801(14) 0.0304(13) Uani 1 1 d . . 1 C34 C -0.2314(4) 0.3694(3) 0.07313(15) 0.0355(14) Uani 1 1 d . . 1 H34 H -0.2333 0.4295 0.0740 0.043 Uiso 1 1 calc R . 1 C35 C 0.7259(4) 1.3263(3) 0.04694(15) 0.0380(14) Uani 1 1 d . . 1 H35 H 0.6933 1.3582 0.0299 0.046 Uiso 1 1 calc R . 1 N2 N 0.7275(3) 1.2423(2) 0.04410(11) 0.0308(11) Uani 1 1 d . . 1 C36 C 0.7712(4) 1.1990(3) 0.06869(14) 0.0377(14) Uani 1 1 d . . 1 H36 H 0.7725 1.1390 0.0672 0.045 Uiso 1 1 calc R . 1 C37 C -0.1856(4) 0.2364(3) 0.09597(15) 0.0400(15) Uani 1 1 d . . 1 H37 H -0.1562 0.2030 0.1131 0.048 Uiso 1 1 calc R . 1 C38 C 0.5008(8) 0.4574(7) 0.1055(3) 0.0858(7) Uani 0.735(3) 1 d P A 1 H38 H 0.4298 0.4802 0.1112 0.103 Uiso 0.735(3) 1 calc PR A 1 Cl1 Cl 0.5516(3) 0.5132(3) 0.07283(10) 0.0858(7) Uani 0.735(3) 1 d P A 1 Cl2 Cl 0.4904(2) 0.34767(16) 0.09590(8) 0.0858(7) Uani 0.735(3) 1 d P A 1 Cl3 Cl 0.5961(3) 0.4734(2) 0.14333(10) 0.0858(7) Uani 0.735(3) 1 d P A 1 C39 C 0.517(2) 0.5123(15) 0.1315(7) 0.0613(16) Uani 0.265(3) 1 d P A 2 H39 H 0.4456 0.4858 0.1327 0.074 Uiso 0.265(3) 1 calc PR A 2 Cl4 Cl 0.4792(5) 0.6210(4) 0.13876(17) 0.0613(16) Uani 0.265(3) 1 d P A 2 Cl5 Cl 0.5303(8) 0.5180(7) 0.0829(2) 0.0613(16) Uani 0.265(3) 1 d P A 2 Cl6 Cl 0.5823(6) 0.4357(4) 0.1434(2) 0.0613(16) Uani 0.265(3) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03334(13) 0.02664(11) 0.02650(13) -0.00062(9) -0.00150(10) -0.00366(9) I1 0.0531(3) 0.0421(2) 0.0354(3) 0.00751(18) -0.00080(19) 0.01209(19) I2 0.0388(2) 0.0399(2) 0.0459(3) -0.00945(18) -0.00260(19) 0.00631(17) N1 0.032(2) 0.026(2) 0.026(3) 0.003(2) 0.001(2) -0.008(2) C1 0.029(3) 0.036(3) 0.032(4) -0.005(3) 0.001(3) -0.005(3) C2 0.028(3) 0.023(3) 0.030(3) 0.001(2) 0.000(3) -0.005(2) C3 0.029(3) 0.026(3) 0.018(3) -0.001(2) -0.001(2) -0.006(2) C4 0.035(3) 0.027(3) 0.032(4) 0.003(2) 0.010(3) 0.003(2) C5 0.049(4) 0.024(3) 0.037(4) 0.004(2) 0.011(3) -0.002(3) C6 0.036(3) 0.024(3) 0.023(3) 0.000(2) -0.007(3) -0.009(3) O1 0.035(2) 0.026(2) 0.045(3) 0.0035(18) 0.0071(19) 0.0016(18) O2 0.029(2) 0.0249(19) 0.029(2) 0.0040(16) 0.0042(16) -0.0038(15) C7 0.022(3) 0.023(3) 0.031(3) 0.001(2) 0.001(2) -0.003(2) C8 0.022(3) 0.020(3) 0.022(3) 0.000(2) -0.004(2) -0.002(2) C9 0.024(3) 0.022(3) 0.025(3) -0.005(2) 0.001(2) 0.001(2) C10 0.019(3) 0.017(2) 0.022(3) -0.002(2) 0.001(2) 0.001(2) C11 0.035(3) 0.018(3) 0.027(3) -0.005(2) 0.007(3) -0.004(2) C12 0.035(3) 0.021(3) 0.033(4) -0.006(2) 0.009(3) -0.002(2) C13 0.015(2) 0.013(2) 0.022(3) -0.002(2) 0.003(2) 0.0003(19) C14 0.018(3) 0.017(2) 0.031(3) -0.006(2) 0.007(2) -0.005(2) C15 0.024(3) 0.017(3) 0.033(3) -0.004(2) -0.002(2) -0.001(2) C16 0.020(3) 0.015(2) 0.047(4) -0.005(2) 0.009(3) -0.006(2) Br1 0.0348(3) 0.0329(3) 0.0843(6) 0.0064(3) 0.0195(3) 0.0141(3) C17 0.025(3) 0.029(3) 0.044(4) -0.016(3) 0.017(3) -0.007(2) C18 0.032(3) 0.029(3) 0.030(4) -0.007(2) 0.006(3) -0.006(2) C19 0.022(3) 0.019(2) 0.026(3) -0.005(2) 0.008(2) -0.005(2) C20 0.021(3) 0.022(3) 0.026(3) 0.000(2) -0.001(2) -0.008(2) C21 0.034(3) 0.024(3) 0.027(3) -0.002(2) -0.003(3) -0.009(2) C22 0.027(3) 0.019(3) 0.038(4) 0.000(2) -0.016(3) -0.005(2) C23 0.018(3) 0.017(2) 0.046(4) -0.003(2) -0.006(3) -0.004(2) Br2 0.0288(3) 0.0293(3) 0.0608(5) -0.0100(3) -0.0114(3) 0.0077(2) C24 0.025(3) 0.017(2) 0.030(3) -0.007(2) 0.000(2) -0.003(2) C25 0.023(3) 0.013(2) 0.023(3) -0.002(2) -0.001(2) -0.007(2) C26 0.016(2) 0.016(2) 0.018(3) -0.005(2) 0.003(2) -0.0009(19) C27 0.019(3) 0.023(3) 0.023(3) -0.003(2) -0.003(2) 0.001(2) C28 0.025(3) 0.018(3) 0.038(4) -0.003(2) -0.002(3) -0.002(2) C29 0.020(3) 0.024(3) 0.032(4) -0.013(2) -0.005(2) 0.001(2) C30 0.037(3) 0.027(3) 0.024(3) 0.000(2) -0.010(2) 0.001(2) C31 0.035(3) 0.015(2) 0.029(3) 0.000(2) -0.002(3) -0.005(2) O3 0.0286(19) 0.0227(19) 0.036(2) -0.0060(16) -0.0099(17) -0.0049(15) C32 0.054(4) 0.027(3) 0.037(4) -0.009(3) -0.013(3) -0.014(3) O4 0.186(6) 0.042(3) 0.059(4) 0.018(2) -0.076(4) -0.043(3) C33 0.033(3) 0.030(3) 0.028(3) -0.004(2) -0.001(3) -0.007(2) C34 0.035(3) 0.024(3) 0.047(4) -0.005(3) -0.009(3) 0.000(2) C35 0.048(4) 0.026(3) 0.040(4) -0.005(3) -0.017(3) -0.002(3) N2 0.037(3) 0.025(2) 0.030(3) -0.001(2) -0.002(2) -0.001(2) C36 0.053(4) 0.025(3) 0.035(4) -0.008(3) -0.004(3) -0.006(3) C37 0.054(4) 0.030(3) 0.035(4) 0.003(3) -0.013(3) -0.009(3) C38 0.0797(13) 0.0729(11) 0.1048(17) 0.0348(12) 0.0166(10) 0.0000(9) Cl1 0.0797(13) 0.0729(11) 0.1048(17) 0.0348(12) 0.0166(10) 0.0000(9) Cl2 0.0797(13) 0.0729(11) 0.1048(17) 0.0348(12) 0.0166(10) 0.0000(9) Cl3 0.0797(13) 0.0729(11) 0.1048(17) 0.0348(12) 0.0166(10) 0.0000(9) C39 0.073(3) 0.047(2) 0.063(3) 0.020(2) -0.002(2) -0.002(2) Cl4 0.073(3) 0.047(2) 0.063(3) 0.020(2) -0.002(2) -0.002(2) Cl5 0.073(3) 0.047(2) 0.063(3) 0.020(2) -0.002(2) -0.002(2) Cl6 0.073(3) 0.047(2) 0.063(3) 0.020(2) -0.002(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N2 2.495(4) . ? Hg1 N1 2.503(4) . ? Hg1 I1 2.6334(5) . ? Hg1 I2 2.6388(6) . ? N1 C1 1.344(6) . ? N1 C5 1.336(6) . ? C1 C2 1.393(7) . ? C1 H1 0.9500 . ? C2 C3 1.391(6) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 C6 1.516(7) . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.188(6) . ? C6 O2 1.359(6) . ? O2 C7 1.418(6) . ? C7 C8 1.388(7) . ? C7 C12 1.395(6) . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C9 C10 1.396(6) . ? C9 H9 0.9500 . ? C10 C11 1.396(6) . ? C10 C13 1.535(6) . ? C11 C12 1.372(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C25 1.542(6) . ? C13 C26 1.543(6) . ? C13 C14 1.546(6) . ? C14 C15 1.382(6) . ? C14 C19 1.403(7) . ? C15 C16 1.381(7) . ? C15 H15 0.9500 . ? C16 C17 1.396(7) . ? C16 Br1 1.904(5) . ? C17 C18 1.392(7) . ? C17 H17 0.9500 . ? C18 C19 1.395(6) . ? C18 H18 0.9500 . ? C19 C20 1.454(6) . ? C20 C25 1.400(7) . ? C20 C21 1.401(7) . ? C21 C22 1.385(7) . ? C21 H21 0.9500 . ? C22 C23 1.385(7) . ? C22 H22 0.9500 . ? C23 C24 1.382(7) . ? C23 Br2 1.917(5) . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C26 C31 1.388(7) . ? C26 C27 1.391(6) . ? C27 C28 1.402(6) . ? C27 H27 0.9500 . ? C28 C29 1.381(7) . ? C28 H28 0.9500 . ? C29 C30 1.383(6) . ? C29 O3 1.421(5) . ? C30 C31 1.385(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? O3 C32 1.357(6) . ? C32 O4 1.173(7) . ? C32 C33 1.527(8) . ? C33 C34 1.372(7) . ? C33 C37 1.376(7) . ? C34 C35 1.373(7) 1_445 ? C34 H34 0.9500 . ? C35 N2 1.331(6) . ? C35 C34 1.373(7) 1_665 ? C35 H35 0.9500 . ? N2 C36 1.330(6) . ? C36 C37 1.368(7) 1_665 ? C36 H36 0.9500 . ? C37 C36 1.368(7) 1_445 ? C37 H37 0.9500 . ? C38 Cl1 1.718(11) . ? C38 Cl2 1.781(11) . ? C38 Cl3 1.970(13) . ? C38 H38 1.0000 . ? C39 Cl6 1.55(2) . ? C39 Cl4 1.81(2) . ? C39 Cl5 1.98(3) . ? C39 H39 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Hg1 N1 84.40(13) . . ? N2 Hg1 I1 100.64(10) . . ? N1 Hg1 I1 100.35(10) . . ? N2 Hg1 I2 100.78(9) . . ? N1 Hg1 I2 102.03(10) . . ? I1 Hg1 I2 150.275(16) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Hg1 120.0(3) . . ? C5 N1 Hg1 121.8(3) . . ? N1 C1 C2 123.1(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 117.9(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.3(5) . . ? C2 C3 C6 121.9(4) . . ? C4 C3 C6 118.8(4) . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.9(5) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? O1 C6 O2 125.9(5) . . ? O1 C6 C3 124.2(5) . . ? O2 C6 C3 109.9(4) . . ? C6 O2 C7 120.6(4) . . ? C8 C7 C12 121.2(5) . . ? C8 C7 O2 123.5(4) . . ? C12 C7 O2 115.1(4) . . ? C7 C8 C9 118.5(4) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 121.2(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 118.1(4) . . ? C11 C10 C13 120.3(4) . . ? C9 C10 C13 121.2(4) . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 119.0(5) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? C25 C13 C10 110.2(3) . . ? C25 C13 C26 112.2(3) . . ? C10 C13 C26 112.1(4) . . ? C25 C13 C14 100.0(4) . . ? C10 C13 C14 113.3(4) . . ? C26 C13 C14 108.5(3) . . ? C15 C14 C19 120.8(4) . . ? C15 C14 C13 128.3(5) . . ? C19 C14 C13 110.8(4) . . ? C14 C15 C16 118.2(5) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C17 C16 C15 121.9(5) . . ? C17 C16 Br1 118.6(4) . . ? C15 C16 Br1 119.5(4) . . ? C16 C17 C18 119.9(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 118.5(5) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C14 C19 C18 120.6(5) . . ? C14 C19 C20 109.0(4) . . ? C18 C19 C20 130.4(5) . . ? C25 C20 C21 119.9(5) . . ? C25 C20 C19 109.0(4) . . ? C21 C20 C19 131.1(5) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 119.8(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 122.9(5) . . ? C24 C23 Br2 118.0(4) . . ? C22 C23 Br2 119.0(4) . . ? C25 C24 C23 117.1(5) . . ? C25 C24 H24 121.4 . . ? C23 C24 H24 121.4 . . ? C24 C25 C20 121.4(5) . . ? C24 C25 C13 127.4(5) . . ? C20 C25 C13 111.1(4) . . ? C31 C26 C27 117.8(4) . . ? C31 C26 C13 120.0(4) . . ? C27 C26 C13 122.0(4) . . ? C26 C27 C28 122.2(4) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C29 C28 C27 117.9(4) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? C28 C29 C30 121.3(4) . . ? C28 C29 O3 124.9(4) . . ? C30 C29 O3 113.8(4) . . ? C29 C30 C31 119.5(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C26 C31 C30 121.3(4) . . ? C26 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C32 O3 C29 124.8(4) . . ? O4 C32 O3 125.8(5) . . ? O4 C32 C33 124.3(5) . . ? O3 C32 C33 109.9(5) . . ? C34 C33 C37 119.0(5) . . ? C34 C33 C32 123.3(5) . . ? C37 C33 C32 117.6(5) . . ? C33 C34 C35 118.3(5) . 1_445 ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 1_445 . ? N2 C35 C34 123.6(5) . 1_665 ? N2 C35 H35 118.2 . . ? C34 C35 H35 118.2 1_665 . ? C36 N2 C35 117.0(5) . . ? C36 N2 Hg1 120.3(3) . . ? C35 N2 Hg1 122.3(4) . . ? N2 C36 C37 123.5(5) . 1_665 ? N2 C36 H36 118.2 . . ? C37 C36 H36 118.2 1_665 . ? C36 C37 C33 118.5(5) 1_445 . ? C36 C37 H37 120.7 1_445 . ? C33 C37 H37 120.7 . . ? Cl1 C38 Cl2 111.0(7) . . ? Cl1 C38 Cl3 107.6(6) . . ? Cl2 C38 Cl3 109.9(5) . . ? Cl1 C38 H38 109.5 . . ? Cl2 C38 H38 109.5 . . ? Cl3 C38 H38 109.5 . . ? Cl6 C39 Cl4 146.5(19) . . ? Cl6 C39 Cl5 107.6(15) . . ? Cl4 C39 Cl5 98.2(11) . . ? Cl6 C39 H39 98.5 . . ? Cl4 C39 H39 98.5 . . ? Cl5 C39 H39 98.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.552 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.149 # Attachment 'CIF for 4-ZnBr2.cif' data_e465a _database_code_depnum_ccdc_archive 'CCDC 617749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Br4 N2 O4 Zn, 3(C H Cl3)' _chemical_formula_sum 'C40 H25 Br4 Cl9 N2 O4 Zn' _chemical_formula_weight 1301.68 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1378(14) _cell_length_b 15.927(3) _cell_length_c 17.210(3) _cell_angle_alpha 114.132(6) _cell_angle_beta 91.838(7) _cell_angle_gamma 91.495(7) _cell_volume 2282.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2073 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 22.18 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 4.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5447 _exptl_absorpt_correction_T_max 0.7694 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18457 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.2079 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.43 _reflns_number_total 10272 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^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 10272 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1958 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2293 _refine_ls_wR_factor_gt 0.1911 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.92408(13) 0.27410(8) 0.02527(8) 0.0242(3) Uani 1 1 d . . . Br1 Br 1.05686(12) 0.22268(8) 0.11616(7) 0.0327(3) Uani 1 1 d . . . Br2 Br 1.03849(13) 0.33975(9) -0.06012(8) 0.0363(3) Uani 1 1 d . . . N1 N 0.7945(9) 0.3760(6) 0.1046(5) 0.024(2) Uani 1 1 d . . . C1 C 0.7187(11) 0.3670(7) 0.1643(6) 0.025(2) Uani 1 1 d . . . H1 H 0.7180 0.3107 0.1688 0.029 Uiso 1 1 calc R . . C2 C 0.6391(11) 0.4374(7) 0.2213(6) 0.024(2) Uani 1 1 d . . . C3 C 0.6460(12) 0.5209(8) 0.2169(8) 0.035(3) Uani 1 1 d . . . H3 H 0.5968 0.5701 0.2552 0.042 Uiso 1 1 calc R . . C4 C 0.7272(14) 0.5316(8) 0.1546(8) 0.041(3) Uani 1 1 d . . . H4 H 0.7343 0.5880 0.1505 0.050 Uiso 1 1 calc R . . C5 C 0.7951(12) 0.4587(8) 0.1006(8) 0.033(3) Uani 1 1 d . . . H5 H 0.8461 0.4657 0.0575 0.040 Uiso 1 1 calc R . . C6 C 0.5530(12) 0.4256(8) 0.2873(8) 0.029(3) Uani 1 1 d . . . O1 O 0.5068(9) 0.4908(6) 0.3471(5) 0.042(2) Uani 1 1 d . . . O2 O 0.5314(8) 0.3381(5) 0.2744(4) 0.0284(18) Uani 1 1 d . . . C7 C 0.4493(12) 0.3145(7) 0.3316(6) 0.025(2) Uani 1 1 d . . . C8 C 0.3311(11) 0.2553(7) 0.2996(7) 0.027(3) Uani 1 1 d . . . H8 H 0.3026 0.2352 0.2423 0.033 Uiso 1 1 calc R . . C9 C 0.2517(12) 0.2238(7) 0.3511(7) 0.028(3) Uani 1 1 d . . . H9 H 0.1738 0.1810 0.3277 0.034 Uiso 1 1 calc R . . C10 C 0.2898(11) 0.2570(7) 0.4377(6) 0.021(2) Uani 1 1 d . . . C11 C 0.4115(12) 0.3185(8) 0.4697(7) 0.031(3) Uani 1 1 d . . . H11 H 0.4392 0.3400 0.5272 0.038 Uiso 1 1 calc R . . C12 C 0.4924(12) 0.3486(8) 0.4179(7) 0.032(3) Uani 1 1 d . . . H12 H 0.5722 0.3901 0.4401 0.039 Uiso 1 1 calc R . . C13 C 0.1995(10) 0.2308(7) 0.4979(7) 0.022(2) Uani 1 1 d . . . C14 C 0.1005(11) 0.1426(8) 0.4553(7) 0.026(3) Uani 1 1 d . . . C15 C 0.1394(11) 0.0545(8) 0.4100(7) 0.027(3) Uani 1 1 d . . . H15 H 0.2369 0.0410 0.3990 0.032 Uiso 1 1 calc R . . C16 C 0.0306(14) -0.0142(7) 0.3809(7) 0.031(3) Uani 1 1 d . . . Br3 Br 0.07984(14) -0.13717(8) 0.31684(8) 0.0400(3) Uani 1 1 d . . . C17 C -0.1177(12) 0.0041(7) 0.3970(7) 0.029(3) Uani 1 1 d . . . H17 H -0.1897 -0.0431 0.3781 0.034 Uiso 1 1 calc R . . C18 C -0.1529(12) 0.0942(9) 0.4416(7) 0.035(3) Uani 1 1 d . . . H18 H -0.2507 0.1075 0.4522 0.042 Uiso 1 1 calc R . . C19 C -0.0491(12) 0.1651(7) 0.4710(7) 0.026(3) Uani 1 1 d . . . C20 C -0.0558(11) 0.2631(7) 0.5164(6) 0.024(2) Uani 1 1 d . . . C21 C -0.1797(13) 0.3174(8) 0.5403(7) 0.035(3) Uani 1 1 d . . . H21 H -0.2736 0.2901 0.5300 0.042 Uiso 1 1 calc R . . C22 C -0.1588(13) 0.4109(9) 0.5791(7) 0.039(3) Uani 1 1 d . . . H22 H -0.2388 0.4483 0.5940 0.046 Uiso 1 1 calc R . . C23 C -0.0163(12) 0.4499(7) 0.5961(7) 0.029(3) Uani 1 1 d . . . Br4 Br 0.01123(16) 0.58087(9) 0.64839(9) 0.0502(4) Uani 1 1 d . . . C24 C 0.1090(12) 0.3979(7) 0.5737(7) 0.029(3) Uani 1 1 d . . . H24 H 0.2027 0.4256 0.5846 0.035 Uiso 1 1 calc R . . C25 C 0.0866(12) 0.3044(8) 0.5352(7) 0.027(3) Uani 1 1 d . . . C26 C 0.2957(10) 0.2181(7) 0.5681(6) 0.019(2) Uani 1 1 d . . . C27 C 0.2544(11) 0.2455(7) 0.6485(6) 0.022(2) Uani 1 1 d . . . H27 H 0.1684 0.2771 0.6640 0.027 Uiso 1 1 calc R . . C28 C 0.3371(11) 0.2280(7) 0.7101(7) 0.026(2) Uani 1 1 d . . . H28 H 0.3072 0.2478 0.7657 0.031 Uiso 1 1 calc R . . C29 C 0.4620(12) 0.1814(7) -0.3137(6) 0.027(3) Uani 1 1 d . . . C30 C 0.5070(13) 0.1487(8) 0.6033(7) 0.036(3) Uani 1 1 d . . . H30 H 0.5905 0.1146 0.5874 0.043 Uiso 1 1 calc R . . C31 C 0.4232(11) 0.1685(8) 0.5450(7) 0.029(3) Uani 1 1 d . . . H31 H 0.4523 0.1485 0.4892 0.035 Uiso 1 1 calc R . . O3 O 0.5501(8) 0.1676(5) -0.2505(4) 0.0301(18) Uani 1 1 d . . . C32 C 0.5562(12) 0.0831(8) -0.2539(7) 0.029(3) Uani 1 1 d . . . O4 O 0.4923(9) 0.0152(6) -0.3073(5) 0.046(2) Uani 1 1 d . . . C33 C 0.6507(12) 0.0798(8) -0.1835(7) 0.026(3) Uani 1 1 d . . . C34 C 0.7264(10) 0.1576(7) -0.1254(6) 0.021(2) Uani 1 1 d . . . H34 H 0.7218 0.2120 -0.1331 0.025 Uiso 1 1 calc R . . N2 N 0.8059(9) 0.1580(6) -0.0589(5) 0.026(2) Uani 1 1 d . . . C35 C 0.8125(12) 0.0771(7) -0.0503(7) 0.030(3) Uani 1 1 d . . . H35 H 0.8648 0.0761 -0.0035 0.036 Uiso 1 1 calc R . . C36 C 0.7462(12) -0.0016(8) -0.1070(7) 0.032(3) Uani 1 1 d . . . H36 H 0.7561 -0.0562 -0.1001 0.039 Uiso 1 1 calc R . . C37 C 0.6651(12) -0.0011(8) -0.1739(7) 0.031(3) Uani 1 1 d . . . H37 H 0.6192 -0.0553 -0.2132 0.037 Uiso 1 1 calc R . . C38 C 0.2113(14) 0.5506(8) 0.1553(8) 0.044(3) Uani 1 1 d . . . H38 H 0.1192 0.5520 0.1252 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.3554(5) 0.5492(4) 0.0931(4) 0.1082(19) Uani 1 1 d . . . Cl2 Cl 0.2065(7) 0.4538(3) 0.1795(3) 0.0996(13) Uani 1 1 d . . . Cl3 Cl 0.2319(7) 0.6496(3) 0.2492(3) 0.0996(13) Uani 1 1 d . . . C39 C 0.2301(15) 0.8961(9) 0.7625(8) 0.050(4) Uani 1 1 d . . . H39 H 0.2885 0.9284 0.7357 0.059 Uiso 1 1 calc R . . Cl4 Cl 0.1989(5) 0.7826(3) 0.6889(2) 0.0656(11) Uani 1 1 d . . . Cl5 Cl 0.3278(4) 0.9030(3) 0.8534(2) 0.0553(10) Uani 1 1 d . . . Cl6 Cl 0.0616(3) 0.9509(2) 0.7888(2) 0.0499(9) Uani 1 1 d . . . C40 C 0.3539(12) 0.2307(8) 0.9882(8) 0.039(3) Uani 1 1 d . . . H40 H 0.2736 0.2623 1.0236 0.047 Uiso 1 1 calc R . . Cl7 Cl 0.4598(4) 0.3119(2) 0.9660(2) 0.0550(10) Uani 1 1 d . . . Cl8 Cl 0.2785(4) 0.1451(2) 0.8927(2) 0.0592(10) Uani 1 1 d . . . Cl9 Cl 0.4598(4) 0.1828(3) 1.0439(3) 0.0698(12) 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 Zn1 0.0202(7) 0.0289(7) 0.0251(7) 0.0133(6) -0.0056(5) -0.0026(5) Br1 0.0307(6) 0.0392(7) 0.0328(7) 0.0205(6) -0.0120(5) -0.0024(5) Br2 0.0318(7) 0.0461(8) 0.0425(8) 0.0295(7) 0.0037(6) 0.0028(6) N1 0.021(5) 0.029(5) 0.021(5) 0.010(4) -0.004(4) -0.007(4) C1 0.021(6) 0.026(6) 0.023(6) 0.007(5) -0.003(5) -0.008(5) C2 0.027(6) 0.028(6) 0.020(6) 0.014(5) -0.007(5) -0.007(5) C3 0.022(6) 0.042(7) 0.044(8) 0.020(6) 0.008(6) 0.008(5) C4 0.059(9) 0.029(7) 0.044(8) 0.023(7) 0.007(7) 0.004(6) C5 0.036(7) 0.030(7) 0.041(8) 0.022(6) 0.003(6) -0.005(5) C6 0.021(6) 0.037(7) 0.031(7) 0.016(6) -0.006(5) -0.007(5) O1 0.044(5) 0.045(5) 0.037(5) 0.018(5) 0.004(4) -0.005(4) O2 0.033(4) 0.025(4) 0.026(4) 0.011(4) 0.002(3) -0.004(3) C7 0.034(7) 0.026(6) 0.018(6) 0.011(5) 0.003(5) -0.001(5) C8 0.027(6) 0.031(7) 0.016(6) 0.003(5) -0.006(5) -0.013(5) C9 0.028(6) 0.025(6) 0.028(7) 0.008(5) -0.012(5) -0.012(5) C10 0.025(6) 0.021(6) 0.017(6) 0.007(5) -0.004(4) 0.005(5) C11 0.037(7) 0.040(7) 0.015(6) 0.009(5) -0.008(5) -0.007(6) C12 0.025(6) 0.050(8) 0.021(6) 0.014(6) -0.011(5) -0.010(5) C13 0.010(5) 0.031(6) 0.027(6) 0.016(5) -0.006(4) -0.003(4) C14 0.020(6) 0.041(7) 0.020(6) 0.019(6) -0.008(5) -0.007(5) C15 0.017(6) 0.037(7) 0.038(7) 0.026(6) 0.005(5) 0.001(5) C16 0.051(8) 0.018(6) 0.022(6) 0.007(5) -0.002(5) 0.007(5) Br3 0.0387(7) 0.0315(7) 0.0451(8) 0.0112(6) 0.0031(6) -0.0046(6) C17 0.023(6) 0.027(7) 0.035(7) 0.013(6) -0.009(5) -0.011(5) C18 0.023(6) 0.057(9) 0.032(7) 0.025(7) -0.001(5) -0.005(6) C19 0.027(6) 0.024(6) 0.027(7) 0.012(5) 0.000(5) 0.003(5) C20 0.016(5) 0.036(7) 0.020(6) 0.013(5) -0.007(4) -0.007(5) C21 0.029(7) 0.036(7) 0.033(7) 0.008(6) -0.005(5) 0.000(6) C22 0.037(7) 0.044(8) 0.035(8) 0.015(7) -0.007(6) 0.006(6) C23 0.029(7) 0.030(6) 0.027(7) 0.011(5) -0.004(5) 0.004(5) Br4 0.0597(9) 0.0335(8) 0.0506(9) 0.0107(7) -0.0071(7) 0.0069(6) C24 0.030(6) 0.028(7) 0.028(7) 0.013(6) -0.008(5) -0.009(5) C25 0.026(6) 0.042(7) 0.019(6) 0.020(6) -0.008(5) 0.004(5) C26 0.015(5) 0.018(5) 0.024(6) 0.012(5) -0.013(4) -0.011(4) C27 0.015(5) 0.031(6) 0.022(6) 0.013(5) -0.005(4) -0.002(5) C28 0.021(6) 0.030(6) 0.025(6) 0.011(5) -0.008(5) -0.005(5) C29 0.039(7) 0.025(6) 0.017(6) 0.010(5) -0.016(5) -0.009(5) C30 0.031(7) 0.054(8) 0.024(7) 0.017(6) -0.004(5) 0.013(6) C31 0.024(6) 0.038(7) 0.019(6) 0.005(5) -0.007(5) 0.005(5) O3 0.039(5) 0.030(5) 0.021(4) 0.010(4) -0.011(3) -0.002(4) C32 0.021(6) 0.037(7) 0.031(7) 0.017(6) 0.002(5) 0.005(5) O4 0.048(6) 0.043(6) 0.038(5) 0.010(5) -0.021(4) -0.002(4) C33 0.028(6) 0.034(7) 0.018(6) 0.011(5) 0.000(5) 0.003(5) C34 0.016(5) 0.033(6) 0.019(6) 0.015(5) -0.002(4) 0.005(5) N2 0.026(5) 0.029(5) 0.026(5) 0.014(4) -0.006(4) -0.002(4) C35 0.033(7) 0.028(7) 0.031(7) 0.014(6) -0.002(5) 0.003(5) C36 0.033(7) 0.034(7) 0.032(7) 0.017(6) -0.009(5) -0.001(5) C37 0.037(7) 0.028(7) 0.023(6) 0.007(5) -0.003(5) -0.006(5) C38 0.044(8) 0.047(8) 0.039(8) 0.017(7) -0.008(6) 0.000(6) Cl1 0.065(3) 0.172(5) 0.139(5) 0.118(5) -0.009(3) -0.017(3) Cl2 0.185(4) 0.0502(19) 0.063(2) 0.0253(17) -0.017(2) -0.011(2) Cl3 0.185(4) 0.0502(19) 0.063(2) 0.0253(17) -0.017(2) -0.011(2) C39 0.050(9) 0.059(9) 0.044(9) 0.025(8) -0.002(7) 0.000(7) Cl4 0.082(3) 0.055(2) 0.057(3) 0.021(2) -0.012(2) 0.014(2) Cl5 0.041(2) 0.074(3) 0.061(2) 0.040(2) -0.0201(17) -0.0067(17) Cl6 0.0389(19) 0.054(2) 0.054(2) 0.0195(18) -0.0113(16) 0.0027(16) C40 0.023(6) 0.043(8) 0.049(8) 0.017(7) -0.001(6) 0.004(6) Cl7 0.0387(19) 0.058(2) 0.076(3) 0.037(2) -0.0013(18) -0.0023(16) Cl8 0.053(2) 0.050(2) 0.060(2) 0.0092(19) -0.0092(18) 0.0049(17) Cl9 0.040(2) 0.113(3) 0.088(3) 0.074(3) -0.007(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.071(9) . ? Zn1 N1 2.072(8) . ? Zn1 Br1 2.3594(16) . ? Zn1 Br2 2.3758(16) . ? N1 C1 1.310(12) . ? N1 C5 1.347(13) . ? C1 C2 1.392(14) . ? C1 H1 0.9300 . ? C2 C3 1.362(14) . ? C2 C6 1.473(14) . ? C3 C4 1.387(15) . ? C3 H3 0.9300 . ? C4 C5 1.337(15) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.221(13) . ? C6 O2 1.327(13) . ? O2 C7 1.416(11) . ? C7 C8 1.358(14) . ? C7 C12 1.395(14) . ? C8 C9 1.396(14) . ? C8 H8 0.9300 . ? C9 C10 1.391(14) . ? C9 H9 0.9300 . ? C10 C11 1.401(15) . ? C10 C13 1.523(13) . ? C11 C12 1.394(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C25 1.531(14) . ? C13 C14 1.542(14) . ? C13 C26 1.554(13) . ? C14 C15 1.361(14) . ? C14 C19 1.428(14) . ? C15 C16 1.378(15) . ? C15 H15 0.9300 . ? C16 C17 1.406(15) . ? C16 Br3 1.888(10) . ? C17 C18 1.374(15) . ? C17 H17 0.9300 . ? C18 C19 1.370(15) . ? C18 H18 0.9300 . ? C19 C20 1.437(14) . ? C20 C25 1.409(14) . ? C20 C21 1.410(14) . ? C21 C22 1.365(16) . ? C21 H21 0.9300 . ? C22 C23 1.398(16) . ? C22 H22 0.9300 . ? C23 C24 1.400(14) . ? C23 Br4 1.911(11) . ? C24 C25 1.366(15) . ? C24 H24 0.9300 . ? C26 C27 1.340(13) . ? C26 C31 1.400(14) . ? C27 C28 1.405(14) . ? C27 H27 0.9300 . ? C28 C29 1.359(14) 1_556 ? C28 H28 0.9300 . ? C29 C28 1.359(14) 1_554 ? C29 C30 1.387(14) 1_554 ? C29 O3 1.424(12) . ? C30 C31 1.384(15) . ? C30 C29 1.387(14) 1_556 ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? O3 C32 1.325(13) . ? C32 O4 1.215(14) . ? C32 C33 1.484(15) . ? C33 C37 1.374(14) . ? C33 C34 1.383(15) . ? C34 N2 1.334(12) . ? C34 H34 0.9300 . ? N2 C35 1.358(13) . ? C35 C36 1.347(15) . ? C35 H35 0.9300 . ? C36 C37 1.352(15) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 Cl1 1.719(13) . ? C38 Cl3 1.736(13) . ? C38 Cl2 1.754(13) . ? C38 H38 0.9800 . ? C39 Cl5 1.737(13) . ? C39 Cl4 1.741(14) . ? C39 Cl6 1.769(13) . ? C39 H39 0.9800 . ? C40 Cl9 1.735(12) . ? C40 Cl8 1.754(13) . ? C40 Cl7 1.765(12) . ? C40 H40 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N1 113.7(3) . . ? N2 Zn1 Br1 104.4(2) . . ? N1 Zn1 Br1 105.2(2) . . ? N2 Zn1 Br2 105.9(2) . . ? N1 Zn1 Br2 104.9(2) . . ? Br1 Zn1 Br2 123.00(6) . . ? C1 N1 C5 117.0(9) . . ? C1 N1 Zn1 123.1(7) . . ? C5 N1 Zn1 119.8(7) . . ? N1 C1 C2 123.2(10) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.1(9) . . ? C3 C2 C6 119.4(10) . . ? C1 C2 C6 122.4(10) . . ? C2 C3 C4 119.1(11) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.3(11) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 N1 124.2(10) . . ? C4 C5 H5 117.9 . . ? N1 C5 H5 117.9 . . ? O1 C6 O2 124.5(10) . . ? O1 C6 C2 122.3(10) . . ? O2 C6 C2 113.2(10) . . ? C6 O2 C7 120.4(8) . . ? C8 C7 C12 121.0(9) . . ? C8 C7 O2 118.2(9) . . ? C12 C7 O2 120.7(10) . . ? C7 C8 C9 121.3(10) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.5(10) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 118.4(9) . . ? C9 C10 C13 121.6(9) . . ? C11 C10 C13 120.0(9) . . ? C12 C11 C10 122.1(10) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C7 117.7(10) . . ? C11 C12 H12 121.1 . . ? C7 C12 H12 121.1 . . ? C10 C13 C25 107.6(8) . . ? C10 C13 C14 115.6(9) . . ? C25 C13 C14 101.7(8) . . ? C10 C13 C26 112.6(8) . . ? C25 C13 C26 112.4(8) . . ? C14 C13 C26 106.5(8) . . ? C15 C14 C19 121.6(10) . . ? C15 C14 C13 128.9(9) . . ? C19 C14 C13 109.4(9) . . ? C14 C15 C16 118.4(10) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C15 C16 C17 122.0(10) . . ? C15 C16 Br3 119.7(9) . . ? C17 C16 Br3 118.3(9) . . ? C18 C17 C16 117.9(10) . . ? C18 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? C19 C18 C17 122.3(10) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C14 117.7(10) . . ? C18 C19 C20 133.5(10) . . ? C14 C19 C20 108.7(9) . . ? C25 C20 C21 120.6(10) . . ? C25 C20 C19 110.2(9) . . ? C21 C20 C19 129.2(10) . . ? C22 C21 C20 118.6(11) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C23 119.4(11) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 123.4(11) . . ? C22 C23 Br4 119.0(8) . . ? C24 C23 Br4 117.6(8) . . ? C25 C24 C23 116.6(10) . . ? C25 C24 H24 121.7 . . ? C23 C24 H24 121.7 . . ? C24 C25 C20 121.4(10) . . ? C24 C25 C13 128.5(10) . . ? C20 C25 C13 109.8(10) . . ? C27 C26 C31 118.5(9) . . ? C27 C26 C13 122.3(9) . . ? C31 C26 C13 118.9(9) . . ? C26 C27 C28 121.9(9) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C29 C28 C27 118.4(10) 1_556 . ? C29 C28 H28 120.8 1_556 . ? C27 C28 H28 120.8 . . ? C28 C29 C30 122.0(10) 1_554 1_554 ? C28 C29 O3 118.5(9) 1_554 . ? C30 C29 O3 119.4(10) 1_554 . ? C31 C30 C29 117.6(10) . 1_556 ? C31 C30 H30 121.2 . . ? C29 C30 H30 121.2 1_556 . ? C30 C31 C26 121.5(10) . . ? C30 C31 H31 119.2 . . ? C26 C31 H31 119.2 . . ? C32 O3 C29 118.4(9) . . ? O4 C32 O3 125.1(11) . . ? O4 C32 C33 122.7(11) . . ? O3 C32 C33 112.2(10) . . ? C37 C33 C34 117.8(10) . . ? C37 C33 C32 120.8(11) . . ? C34 C33 C32 121.4(10) . . ? N2 C34 C33 122.8(10) . . ? N2 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 N2 C35 117.2(10) . . ? C34 N2 Zn1 122.3(7) . . ? C35 N2 Zn1 120.5(7) . . ? C36 C35 N2 122.5(11) . . ? C36 C35 H35 118.7 . . ? N2 C35 H35 118.7 . . ? C35 C36 C37 119.8(11) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C33 119.8(11) . . ? C36 C37 H37 120.1 . . ? C33 C37 H37 120.1 . . ? Cl1 C38 Cl3 108.1(8) . . ? Cl1 C38 Cl2 111.5(7) . . ? Cl3 C38 Cl2 109.4(7) . . ? Cl1 C38 H38 109.3 . . ? Cl3 C38 H38 109.3 . . ? Cl2 C38 H38 109.3 . . ? Cl5 C39 Cl4 111.9(7) . . ? Cl5 C39 Cl6 111.0(7) . . ? Cl4 C39 Cl6 109.9(8) . . ? Cl5 C39 H39 107.9 . . ? Cl4 C39 H39 107.9 . . ? Cl6 C39 H39 107.9 . . ? Cl9 C40 Cl8 110.9(7) . . ? Cl9 C40 Cl7 110.4(6) . . ? Cl8 C40 Cl7 109.7(7) . . ? Cl9 C40 H40 108.6 . . ? Cl8 C40 H40 108.6 . . ? Cl7 C40 H40 108.6 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.421 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.203