# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wubiao@lzb.ac.cn _publ_contact_author_name 'Wu, Biao' loop_ _publ_author_name 'Zaiwen Yang' 'Xiaojuan Huang' 'Qilong Zhao' 'Li Shaoguang' 'Biao Wu' data_ZnCl2 _database_code_depnum_ccdc_archive 'CCDC 874345' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Cl2 N6 O3 Zn' _chemical_formula_weight 680.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 7.143(3) _cell_length_b 14.458(6) _cell_length_c 29.544(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3051(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7285 _exptl_absorpt_correction_T_max 0.7985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16042 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.64 _reflns_number_total 5709 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(16) _refine_ls_number_reflns 5709 _refine_ls_number_parameters 403 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Zn Zn 0.68389(8) 1.12455(4) 0.846784(18) 0.05104(17) Uani 1 1 d . . . Cl1 Cl 0.8661(2) 1.24693(9) 0.84594(6) 0.0784(4) Uani 1 1 d . . . Cl2 Cl 0.3901(2) 1.14694(10) 0.82208(5) 0.0680(4) Uani 1 1 d . . . N1 N 0.7817(6) 1.0266(2) 0.80340(12) 0.0451(9) Uani 1 1 d . . . N2 N 0.6145(8) 0.8084(3) 0.75782(13) 0.0692(14) Uani 1 1 d . . . H2A H 0.6197 0.7831 0.7315 0.083 Uiso 1 1 calc R . . N3 N 0.4093(9) 0.6957(3) 0.77631(15) 0.098(2) Uani 1 1 d . . . H3B H 0.4402 0.6709 0.7509 0.117 Uiso 1 1 calc R . . N4 N 0.6729(6) 1.0724(3) 0.91077(12) 0.0555(10) Uani 1 1 d . . . N5 N 0.5928(6) 0.8576(2) 0.97014(12) 0.0497(10) Uani 1 1 d . . . H5B H 0.5467 0.8288 0.9472 0.060 Uiso 1 1 calc R . . N6 N 0.5841(6) 0.7162(3) 1.00293(13) 0.0532(11) Uani 1 1 d . . . H6A H 0.5501 0.6993 0.9763 0.064 Uiso 1 1 calc R . . O1 O 0.4760(8) 0.8042(3) 0.82649(13) 0.1004(17) Uani 1 1 d . . . O2 O 0.6710(6) 0.8413(2) 1.04407(11) 0.0675(10) Uani 1 1 d . . . O3 O 0.4818(6) 0.7154(3) 0.90689(12) 0.0751(12) Uani 1 1 d D . . C1 C 0.6753(8) 0.9547(3) 0.79343(15) 0.0509(12) Uani 1 1 d . . . H1A H 0.5561 0.9523 0.8060 0.061 Uiso 1 1 calc R . . C2 C 0.7283(8) 0.8839(3) 0.76599(14) 0.0527(13) Uani 1 1 d . . . C3 C 0.9048(9) 0.8901(4) 0.74601(16) 0.0651(15) Uani 1 1 d . . . H3A H 0.9469 0.8438 0.7267 0.078 Uiso 1 1 calc R . . C4 C 1.0138(9) 0.9642(4) 0.75517(18) 0.0666(16) Uani 1 1 d . . . H4A H 1.1305 0.9699 0.7415 0.080 Uiso 1 1 calc R . . C5 C 0.9523(7) 1.0315(3) 0.78481(17) 0.0552(14) Uani 1 1 d . . . H5A H 1.0304 1.0808 0.7920 0.066 Uiso 1 1 calc R . . C6 C 0.4933(9) 0.7711(4) 0.78916(18) 0.0690(16) Uani 1 1 d . . . C7 C 0.2628(11) 0.6517(4) 0.80405(19) 0.0772(18) Uani 1 1 d . . . C8 C 0.0942(12) 0.6913(4) 0.8112(2) 0.0764(18) Uani 1 1 d . . . H8A H 0.0719 0.7485 0.7979 0.092 Uiso 1 1 calc R . . C9 C -0.0493(11) 0.6524(6) 0.8372(3) 0.095(2) Uani 1 1 d . . . H9A H -0.1641 0.6817 0.8411 0.114 Uiso 1 1 calc R . . C10 C -0.0087(11) 0.5662(6) 0.8570(2) 0.095(2) Uani 1 1 d . . . H10A H -0.0980 0.5366 0.8747 0.114 Uiso 1 1 calc R . . C11 C 0.2106(15) 0.4393(5) 0.8683(2) 0.108(3) Uani 1 1 d . . . H11A H 0.1213 0.4105 0.8864 0.129 Uiso 1 1 calc R . . C12 C 0.3725(19) 0.3957(6) 0.8619(3) 0.132(4) Uani 1 1 d . . . H12A H 0.3948 0.3370 0.8736 0.158 Uiso 1 1 calc R . . C13 C 0.5027(12) 0.4413(6) 0.8374(3) 0.096(2) Uani 1 1 d . . . H13A H 0.6183 0.4125 0.8342 0.115 Uiso 1 1 calc R . . C14 C 0.4832(9) 0.5227(4) 0.8174(2) 0.0745(17) Uani 1 1 d . . . H14A H 0.5794 0.5489 0.8005 0.089 Uiso 1 1 calc R . . C15 C 0.3023(9) 0.5693(4) 0.82308(16) 0.0618(14) Uani 1 1 d . . . C16 C 0.1660(8) 0.5251(3) 0.84996(17) 0.0578(12) Uani 1 1 d . . . C17 C 0.6362(7) 0.9850(3) 0.92088(15) 0.0478(12) Uani 1 1 d . . . H17A H 0.6107 0.9445 0.8972 0.057 Uiso 1 1 calc R . . C18 C 0.6334(7) 0.9506(3) 0.96433(15) 0.0526(13) Uani 1 1 d . . . C19 C 0.6710(10) 1.0114(3) 0.99912(17) 0.0749(18) Uani 1 1 d . . . H19A H 0.6687 0.9918 1.0291 0.090 Uiso 1 1 calc R . . C20 C 0.7118(12) 1.1011(4) 0.9884(2) 0.103(3) Uani 1 1 d . . . H20A H 0.7411 1.1429 1.0113 0.124 Uiso 1 1 calc R . . C21 C 0.7097(10) 1.1298(4) 0.94429(17) 0.090(2) Uani 1 1 d . . . H21A H 0.7349 1.1915 0.9377 0.108 Uiso 1 1 calc R . . C22 C 0.6190(7) 0.8067(3) 1.00899(16) 0.0495(12) Uani 1 1 d . . . C23 C 0.5976(7) 0.6466(3) 1.03581(16) 0.0509(12) Uani 1 1 d . . . C24 C 0.5693(8) 0.6649(4) 1.08119(17) 0.0595(14) Uani 1 1 d . . . H24A H 0.5387 0.7245 1.0904 0.071 Uiso 1 1 calc R . . C25 C 0.5863(9) 0.5944(4) 1.11336(17) 0.0686(16) Uani 1 1 d . . . H25A H 0.5698 0.6079 1.1439 0.082 Uiso 1 1 calc R . . C26 C 0.6261(8) 0.5079(4) 1.10067(17) 0.0654(15) Uani 1 1 d . . . H26A H 0.6371 0.4620 1.1225 0.078 Uiso 1 1 calc R . . C27 C 0.6918(11) 0.3948(4) 1.0417(2) 0.097(2) Uani 1 1 d . . . H27A H 0.7039 0.3489 1.0636 0.116 Uiso 1 1 calc R . . C28 C 0.7135(13) 0.3729(4) 0.9979(2) 0.122(3) Uani 1 1 d . . . H28A H 0.7377 0.3119 0.9897 0.147 Uiso 1 1 calc R . . C29 C 0.7000(11) 0.4405(4) 0.9647(2) 0.101(2) Uani 1 1 d . . . H29A H 0.7170 0.4248 0.9344 0.121 Uiso 1 1 calc R . . C30 C 0.6622(10) 0.5296(4) 0.97620(18) 0.0769(17) Uani 1 1 d . . . H30A H 0.6530 0.5743 0.9537 0.092 Uiso 1 1 calc R . . C31 C 0.6366(8) 0.5550(3) 1.02187(15) 0.0539(13) Uani 1 1 d . . . C32 C 0.6514(8) 0.4856(3) 1.05529(17) 0.0616(14) Uani 1 1 d . . . H3C H 0.379(5) 0.696(4) 0.9174(19) 0.080 Uiso 1 1 d D . . H3D H 0.479(9) 0.740(4) 0.8814(11) 0.080 Uiso 1 1 d 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 Zn 0.0665(4) 0.0415(3) 0.0451(3) 0.0073(3) 0.0020(3) -0.0015(3) Cl1 0.0859(11) 0.0551(7) 0.0942(10) 0.0062(8) 0.0054(9) -0.0198(7) Cl2 0.0578(9) 0.0733(9) 0.0729(9) 0.0256(7) 0.0027(7) 0.0002(7) N1 0.047(3) 0.047(2) 0.041(2) 0.0085(17) -0.0001(18) -0.0007(19) N2 0.124(4) 0.046(2) 0.037(2) -0.0035(19) 0.014(3) -0.019(3) N3 0.181(6) 0.069(3) 0.043(3) -0.011(2) 0.013(3) -0.059(4) N4 0.076(3) 0.046(2) 0.045(2) 0.0022(18) -0.001(2) 0.004(2) N5 0.075(3) 0.038(2) 0.036(2) 0.0043(17) 0.0000(19) 0.0015(19) N6 0.082(3) 0.044(2) 0.033(2) 0.0039(18) -0.011(2) -0.008(2) O1 0.171(5) 0.094(3) 0.036(2) -0.013(2) 0.020(2) -0.062(3) O2 0.113(3) 0.0504(18) 0.0394(19) 0.0042(15) -0.015(2) -0.004(2) O3 0.095(3) 0.093(3) 0.038(2) 0.002(2) 0.001(2) -0.016(3) C1 0.057(3) 0.048(3) 0.047(3) 0.010(2) 0.002(3) 0.003(3) C2 0.080(4) 0.045(3) 0.033(2) 0.008(2) 0.001(2) 0.007(3) C3 0.103(5) 0.050(3) 0.043(3) 0.010(3) 0.015(3) 0.019(3) C4 0.079(4) 0.070(4) 0.051(3) 0.013(3) 0.020(3) 0.021(3) C5 0.058(4) 0.057(3) 0.050(3) 0.021(3) 0.001(3) 0.001(3) C6 0.112(5) 0.053(3) 0.041(3) 0.004(3) 0.000(3) -0.014(3) C7 0.109(6) 0.067(4) 0.055(3) -0.023(3) -0.015(3) -0.007(4) C8 0.108(6) 0.056(4) 0.066(4) -0.013(3) -0.025(4) 0.015(4) C9 0.078(5) 0.108(6) 0.100(6) -0.041(5) -0.017(4) 0.012(4) C10 0.096(6) 0.128(6) 0.062(4) -0.031(4) -0.004(4) -0.034(5) C11 0.171(9) 0.082(5) 0.070(4) 0.003(4) -0.029(5) -0.023(6) C12 0.220(13) 0.072(6) 0.105(7) -0.008(5) -0.063(7) 0.002(7) C13 0.106(6) 0.076(5) 0.106(6) -0.011(4) -0.032(5) 0.008(4) C14 0.078(5) 0.076(4) 0.069(4) -0.021(3) -0.006(3) -0.001(4) C15 0.087(4) 0.051(3) 0.047(3) -0.008(2) -0.013(3) -0.007(3) C16 0.073(4) 0.054(3) 0.046(3) -0.009(3) -0.004(3) -0.011(3) C17 0.065(4) 0.037(2) 0.042(3) 0.000(2) 0.002(2) 0.001(2) C18 0.074(4) 0.045(3) 0.039(3) 0.006(2) 0.001(2) 0.008(2) C19 0.137(6) 0.047(3) 0.041(3) -0.001(2) 0.005(3) 0.018(3) C20 0.212(8) 0.041(3) 0.056(3) -0.010(3) 0.004(5) 0.001(4) C21 0.181(7) 0.039(3) 0.050(3) -0.005(3) -0.002(4) 0.008(4) C22 0.062(3) 0.047(3) 0.040(3) 0.007(2) -0.005(2) 0.003(2) C23 0.064(3) 0.046(3) 0.043(3) 0.007(2) -0.007(2) -0.011(2) C24 0.085(4) 0.051(3) 0.043(3) 0.005(2) 0.002(3) -0.011(3) C25 0.095(4) 0.072(4) 0.039(3) 0.010(3) -0.008(3) -0.016(3) C26 0.078(4) 0.067(4) 0.051(3) 0.022(3) -0.008(3) 0.001(3) C27 0.155(7) 0.053(4) 0.083(4) 0.015(3) 0.002(5) 0.015(4) C28 0.233(9) 0.045(3) 0.088(5) 0.003(4) 0.031(6) 0.023(5) C29 0.177(8) 0.062(4) 0.064(4) -0.013(3) 0.016(5) 0.017(4) C30 0.125(5) 0.055(3) 0.051(3) 0.004(2) 0.003(3) -0.008(4) C31 0.078(4) 0.044(3) 0.040(3) 0.006(2) -0.003(3) -0.001(2) C32 0.075(4) 0.051(3) 0.058(3) 0.011(2) -0.002(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N1 2.034(4) . ? Zn N4 2.037(4) . ? Zn Cl1 2.1969(15) . ? Zn Cl2 2.2451(18) . ? N1 C1 1.321(6) . ? N1 C5 1.338(6) . ? N2 C6 1.378(7) . ? N2 C2 1.383(6) . ? N2 H2A 0.8600 . ? N3 C6 1.300(7) . ? N3 C7 1.474(9) . ? N3 H3B 0.8600 . ? N4 C21 1.319(6) . ? N4 C17 1.325(6) . ? N5 C22 1.376(5) . ? N5 C18 1.387(6) . ? N5 H5B 0.8600 . ? N6 C22 1.344(6) . ? N6 C23 1.402(5) . ? N6 H6A 0.8600 . ? O1 C6 1.209(6) . ? O2 C22 1.209(5) . ? O3 H3C 0.85(2) . ? O3 H3D 0.83(2) . ? C1 C2 1.359(6) . ? C1 H1A 0.9300 . ? C2 C3 1.395(7) . ? C3 C4 1.352(8) . ? C3 H3A 0.9300 . ? C4 C5 1.380(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C15 1.347(8) . ? C7 C8 1.350(9) . ? C8 C9 1.398(10) . ? C8 H8A 0.9300 . ? C9 C10 1.407(10) . ? C9 H9A 0.9300 . ? C10 C16 1.398(9) . ? C10 H10A 0.9300 . ? C11 C12 1.331(12) . ? C11 C16 1.391(9) . ? C11 H11A 0.9300 . ? C12 C13 1.350(12) . ? C12 H12A 0.9300 . ? C13 C14 1.323(9) . ? C13 H13A 0.9300 . ? C14 C15 1.467(8) . ? C14 H14A 0.9300 . ? C15 C16 1.410(8) . ? C17 C18 1.377(6) . ? C17 H17A 0.9300 . ? C18 C19 1.378(7) . ? C19 C20 1.367(7) . ? C19 H19A 0.9300 . ? C20 C21 1.369(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C23 C24 1.381(7) . ? C23 C31 1.414(7) . ? C24 C25 1.399(7) . ? C24 H24A 0.9300 . ? C25 C26 1.336(8) . ? C25 H25A 0.9300 . ? C26 C32 1.391(7) . ? C26 H26A 0.9300 . ? C27 C28 1.342(9) . ? C27 C32 1.402(7) . ? C27 H27A 0.9300 . ? C28 C29 1.389(9) . ? C28 H28A 0.9300 . ? C29 C30 1.359(8) . ? C29 H29A 0.9300 . ? C30 C31 1.411(7) . ? C30 H30A 0.9300 . ? C31 C32 1.413(6) . ? 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 Zn N4 109.90(15) . . ? N1 Zn Cl1 110.48(12) . . ? N4 Zn Cl1 109.37(13) . . ? N1 Zn Cl2 102.52(12) . . ? N4 Zn Cl2 108.61(14) . . ? Cl1 Zn Cl2 115.72(6) . . ? C1 N1 C5 118.3(4) . . ? C1 N1 Zn 119.4(3) . . ? C5 N1 Zn 122.3(3) . . ? C6 N2 C2 124.2(4) . . ? C6 N2 H2A 117.9 . . ? C2 N2 H2A 117.9 . . ? C6 N3 C7 121.8(5) . . ? C6 N3 H3B 119.1 . . ? C7 N3 H3B 119.1 . . ? C21 N4 C17 118.1(4) . . ? C21 N4 Zn 117.1(3) . . ? C17 N4 Zn 124.8(3) . . ? C22 N5 C18 126.4(4) . . ? C22 N5 H5B 116.8 . . ? C18 N5 H5B 116.8 . . ? C22 N6 C23 126.4(4) . . ? C22 N6 H6A 116.8 . . ? C23 N6 H6A 116.8 . . ? H3C O3 H3D 117(6) . . ? N1 C1 C2 124.4(5) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 N2 122.4(5) . . ? C1 C2 C3 117.1(5) . . ? N2 C2 C3 120.5(5) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 120.9(5) . . ? N1 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? O1 C6 N3 123.5(6) . . ? O1 C6 N2 121.5(5) . . ? N3 C6 N2 114.9(5) . . ? C15 C7 C8 119.8(7) . . ? C15 C7 N3 117.7(7) . . ? C8 C7 N3 122.5(6) . . ? C7 C8 C9 124.7(6) . . ? C7 C8 H8A 117.6 . . ? C9 C8 H8A 117.6 . . ? C8 C9 C10 115.6(7) . . ? C8 C9 H9A 122.2 . . ? C10 C9 H9A 122.2 . . ? C16 C10 C9 120.0(7) . . ? C16 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C16 124.4(9) . . ? C12 C11 H11A 117.8 . . ? C16 C11 H11A 117.8 . . ? C11 C12 C13 116.3(9) . . ? C11 C12 H12A 121.8 . . ? C13 C12 H12A 121.8 . . ? C14 C13 C12 127.0(9) . . ? C14 C13 H13A 116.5 . . ? C12 C13 H13A 116.5 . . ? C13 C14 C15 116.7(7) . . ? C13 C14 H14A 121.6 . . ? C15 C14 H14A 121.6 . . ? C7 C15 C16 119.4(6) . . ? C7 C15 C14 122.9(6) . . ? C16 C15 C14 117.7(5) . . ? C11 C16 C10 121.7(7) . . ? C11 C16 C15 117.8(7) . . ? C10 C16 C15 120.5(6) . . ? N4 C17 C18 123.9(4) . . ? N4 C17 H17A 118.1 . . ? C18 C17 H17A 118.1 . . ? C17 C18 C19 117.6(4) . . ? C17 C18 N5 117.9(4) . . ? C19 C18 N5 124.5(4) . . ? C20 C19 C18 118.3(5) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C19 C20 C21 120.4(5) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? N4 C21 C20 121.8(5) . . ? N4 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? O2 C22 N6 125.0(4) . . ? O2 C22 N5 122.4(4) . . ? N6 C22 N5 112.6(4) . . ? C24 C23 N6 121.6(4) . . ? C24 C23 C31 119.4(4) . . ? N6 C23 C31 118.9(4) . . ? C23 C24 C25 120.5(5) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 120.6(5) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C32 121.1(5) . . ? C25 C26 H26A 119.5 . . ? C32 C26 H26A 119.5 . . ? C28 C27 C32 121.4(6) . . ? C28 C27 H27A 119.3 . . ? C32 C27 H27A 119.3 . . ? C27 C28 C29 120.5(6) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 120.3(6) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 120.8(5) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C32 118.3(5) . . ? C30 C31 C23 123.3(4) . . ? C32 C31 C23 118.5(4) . . ? C26 C32 C27 121.3(5) . . ? C26 C32 C31 119.9(5) . . ? C27 C32 C31 118.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn N1 C1 70.5(3) . . . . ? Cl1 Zn N1 C1 -168.7(3) . . . . ? Cl2 Zn N1 C1 -44.9(3) . . . . ? N4 Zn N1 C5 -108.6(3) . . . . ? Cl1 Zn N1 C5 12.2(4) . . . . ? Cl2 Zn N1 C5 136.1(3) . . . . ? N1 Zn N4 C21 145.3(4) . . . . ? Cl1 Zn N4 C21 23.9(5) . . . . ? Cl2 Zn N4 C21 -103.3(5) . . . . ? N1 Zn N4 C17 -33.0(5) . . . . ? Cl1 Zn N4 C17 -154.4(4) . . . . ? Cl2 Zn N4 C17 78.4(4) . . . . ? C5 N1 C1 C2 1.1(6) . . . . ? Zn N1 C1 C2 -178.0(3) . . . . ? N1 C1 C2 N2 177.6(4) . . . . ? N1 C1 C2 C3 -2.3(7) . . . . ? C6 N2 C2 C1 -33.7(8) . . . . ? C6 N2 C2 C3 146.2(5) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? N2 C2 C3 C4 -179.1(5) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? C1 N1 C5 C4 1.5(6) . . . . ? Zn N1 C5 C4 -179.4(4) . . . . ? C3 C4 C5 N1 -2.9(8) . . . . ? C7 N3 C6 O1 9.5(11) . . . . ? C7 N3 C6 N2 -174.4(6) . . . . ? C2 N2 C6 O1 1.5(9) . . . . ? C2 N2 C6 N3 -174.7(5) . . . . ? C6 N3 C7 C15 -111.6(7) . . . . ? C6 N3 C7 C8 67.6(9) . . . . ? C15 C7 C8 C9 -0.8(9) . . . . ? N3 C7 C8 C9 180.0(5) . . . . ? C7 C8 C9 C10 0.6(9) . . . . ? C8 C9 C10 C16 -0.1(9) . . . . ? C16 C11 C12 C13 3.1(12) . . . . ? C11 C12 C13 C14 -3.5(13) . . . . ? C12 C13 C14 C15 1.3(11) . . . . ? C8 C7 C15 C16 0.6(8) . . . . ? N3 C7 C15 C16 179.8(4) . . . . ? C8 C7 C15 C14 -179.1(5) . . . . ? N3 C7 C15 C14 0.1(7) . . . . ? C13 C14 C15 C7 -179.0(5) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C12 C11 C16 C10 178.2(7) . . . . ? C12 C11 C16 C15 -0.8(10) . . . . ? C9 C10 C16 C11 -179.0(6) . . . . ? C9 C10 C16 C15 -0.1(8) . . . . ? C7 C15 C16 C11 178.8(5) . . . . ? C14 C15 C16 C11 -1.5(7) . . . . ? C7 C15 C16 C10 -0.1(8) . . . . ? C14 C15 C16 C10 179.6(5) . . . . ? C21 N4 C17 C18 0.2(8) . . . . ? Zn N4 C17 C18 178.5(4) . . . . ? N4 C17 C18 C19 0.1(8) . . . . ? N4 C17 C18 N5 180.0(5) . . . . ? C22 N5 C18 C17 166.3(5) . . . . ? C22 N5 C18 C19 -13.9(8) . . . . ? C17 C18 C19 C20 -1.1(9) . . . . ? N5 C18 C19 C20 179.0(6) . . . . ? C18 C19 C20 C21 1.8(11) . . . . ? C17 N4 C21 C20 0.5(10) . . . . ? Zn N4 C21 C20 -177.9(6) . . . . ? C19 C20 C21 N4 -1.5(12) . . . . ? C23 N6 C22 O2 1.4(9) . . . . ? C23 N6 C22 N5 -179.9(4) . . . . ? C18 N5 C22 O2 5.1(8) . . . . ? C18 N5 C22 N6 -173.7(5) . . . . ? C22 N6 C23 C24 28.8(8) . . . . ? C22 N6 C23 C31 -152.8(5) . . . . ? N6 C23 C24 C25 -179.1(5) . . . . ? C31 C23 C24 C25 2.6(8) . . . . ? C23 C24 C25 C26 -1.5(9) . . . . ? C24 C25 C26 C32 -0.1(9) . . . . ? C32 C27 C28 C29 1.3(14) . . . . ? C27 C28 C29 C30 -0.9(14) . . . . ? C28 C29 C30 C31 0.2(12) . . . . ? C29 C30 C31 C32 0.0(10) . . . . ? C29 C30 C31 C23 179.8(7) . . . . ? C24 C23 C31 C30 178.2(5) . . . . ? N6 C23 C31 C30 -0.2(8) . . . . ? C24 C23 C31 C32 -2.1(8) . . . . ? N6 C23 C31 C32 179.5(5) . . . . ? C25 C26 C32 C27 -179.5(6) . . . . ? C25 C26 C32 C31 0.5(9) . . . . ? C28 C27 C32 C26 179.0(7) . . . . ? C28 C27 C32 C31 -1.1(11) . . . . ? C30 C31 C32 C26 -179.7(5) . . . . ? C23 C31 C32 C26 0.6(8) . . . . ? C30 C31 C32 C27 0.4(9) . . . . ? C23 C31 C32 C27 -179.4(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5B O3 0.86 2.08 2.889(6) 156.5 . N6 H6A O3 0.86 2.12 2.930(5) 156.9 . O3 H3D O1 0.83(2) 1.87(2) 2.701(6) 175(6) . O3 H3C O2 0.85(2) 1.95(3) 2.775(6) 166(6) 4_467 C1 H1A O1 0.93 2.30 2.777(6) 111.6 . C19 H19A O2 0.93 2.22 2.795(6) 119.2 . C24 H24A O2 0.93 2.37 2.870(6) 113.4 . N2 H2A Cl2 0.86 2.53 3.320(4) 153.7 3_646 N3 H3B Cl2 0.86 2.50 3.317(5) 159.2 3_646 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.525 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.060 ##################### data_ZnBr2C2H5OH _database_code_depnum_ccdc_archive 'CCDC 874346' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.50 H30.50 Br2 N6 O2.75 Zn' _chemical_formula_weight 786.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.274(4) _cell_length_b 16.062(3) _cell_length_c 8.8413(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3447.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1582 _exptl_absorpt_coefficient_mu 3.072 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4593 _exptl_absorpt_correction_T_max 0.7487 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22831 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.27 _reflns_number_total 5273 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.1578P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(12) _refine_ls_number_reflns 5273 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Zn Zn 1.16355(2) 1.15317(3) 0.36042(9) 0.04942(17) Uani 1 1 d . . . Br1 Br 1.11546(3) 1.11391(5) 0.14217(10) 0.0803(2) Uani 1 1 d . . . Br2 Br 1.25189(2) 1.21369(4) 0.35033(10) 0.0720(2) Uani 1 1 d . . . N1 N 1.17070(18) 1.0530(3) 0.5058(6) 0.0497(12) Uani 1 1 d . . . N2 N 1.11579(18) 0.8435(3) 0.5508(6) 0.0545(12) Uani 1 1 d . . . H2A H 1.1070 0.8345 0.4580 0.065 Uiso 1 1 calc R . . N3 N 1.0753(2) 0.7180(3) 0.5988(6) 0.0567(14) Uani 1 1 d . . . H3B H 1.0704 0.7145 0.5027 0.068 Uiso 1 1 calc R . . N4 N 1.11357(18) 1.2311(3) 0.4837(6) 0.0509(12) Uani 1 1 d . . . N5 N 0.96619(18) 1.2643(3) 0.5417(6) 0.0567(13) Uani 1 1 d . . . H5B H 0.9543 1.2526 0.4527 0.068 Uiso 1 1 calc R . . N6 N 0.87553(18) 1.2640(3) 0.6101(6) 0.0608(14) Uani 1 1 d . . . H6A H 0.8683 1.2593 0.5153 0.073 Uiso 1 1 calc R . . C1 C 1.1421(2) 0.9830(3) 0.4863(7) 0.0477(14) Uani 1 1 d . . . H1A H 1.1181 0.9792 0.4046 0.057 Uiso 1 1 calc R . . C2 C 1.1469(2) 0.9160(3) 0.5826(7) 0.0434(13) Uani 1 1 d . . . C3 C 1.1836(3) 0.9206(4) 0.7008(8) 0.0630(18) Uani 1 1 d . . . H3A H 1.1886 0.8761 0.7667 0.076 Uiso 1 1 calc R . . C4 C 1.2125(3) 0.9928(4) 0.7177(8) 0.076(2) Uani 1 1 d . . . H4A H 1.2379 0.9973 0.7960 0.091 Uiso 1 1 calc R . . C5 C 1.2050(3) 1.0588(4) 0.6223(9) 0.0692(18) Uani 1 1 d . . . H5A H 1.2240 1.1082 0.6392 0.083 Uiso 1 1 calc R . . C6 C 1.0985(2) 0.7864(3) 0.6563(8) 0.0454(13) Uani 1 1 d . . . C7 C 1.0584(2) 0.6508(3) 0.6928(7) 0.0504(15) Uani 1 1 d . . . C8 C 1.0973(3) 0.6079(4) 0.7729(9) 0.0639(17) Uani 1 1 d . . . H8A H 1.1344 0.6212 0.7614 0.077 Uiso 1 1 calc R . . C9 C 1.0820(3) 0.5449(4) 0.8709(11) 0.085(2) Uani 1 1 d . . . H9A H 1.1087 0.5178 0.9281 0.102 Uiso 1 1 calc R . . C10 C 1.0288(4) 0.5224(4) 0.8843(10) 0.084(2) Uani 1 1 d . . . H10A H 1.0191 0.4791 0.9489 0.100 Uiso 1 1 calc R . . C11 C 0.9312(4) 0.5444(6) 0.8163(12) 0.116(4) Uani 1 1 d . . . H11A H 0.9200 0.5030 0.8832 0.139 Uiso 1 1 calc R . . C12 C 0.8926(4) 0.5864(7) 0.7321(15) 0.115(4) Uani 1 1 d . . . H12A H 0.8559 0.5701 0.7375 0.137 Uiso 1 1 calc R . . C13 C 0.9070(3) 0.6520(5) 0.6398(13) 0.097(3) Uani 1 1 d . . . H13A H 0.8798 0.6816 0.5889 0.116 Uiso 1 1 calc R . . C14 C 0.9613(2) 0.6741(4) 0.6226(9) 0.0635(18) Uani 1 1 d . . . H14A H 0.9708 0.7178 0.5588 0.076 Uiso 1 1 calc R . . C15 C 1.0026(3) 0.6303(3) 0.7017(7) 0.0519(15) Uani 1 1 d . . . C16 C 0.9879(3) 0.5636(4) 0.8021(9) 0.073(2) Uani 1 1 d . . . C17 C 1.0584(2) 1.2266(3) 0.4762(7) 0.0464(14) Uani 1 1 d . . . H17A H 1.0431 1.1895 0.4072 0.056 Uiso 1 1 calc R . . C18 C 1.0236(2) 1.2724(3) 0.5624(7) 0.0487(14) Uani 1 1 d . . . C19 C 1.0461(3) 1.3284(5) 0.6635(9) 0.080(2) Uani 1 1 d . . . H19A H 1.0237 1.3616 0.7238 0.096 Uiso 1 1 calc R . . C20 C 1.1024(3) 1.3336(5) 0.6727(11) 0.096(3) Uani 1 1 d . . . H20A H 1.1185 1.3706 0.7406 0.115 Uiso 1 1 calc R . . C21 C 1.1350(3) 1.2850(4) 0.5828(9) 0.074(2) Uani 1 1 d . . . H21A H 1.1731 1.2894 0.5908 0.089 Uiso 1 1 calc R . . C22 C 0.9287(2) 1.2741(4) 0.6541(8) 0.0603(17) Uani 1 1 d . . . C23 C 0.8315(2) 1.2609(4) 0.7159(7) 0.0562(16) Uani 1 1 d . . . C24 C 0.8222(3) 1.3268(4) 0.8084(8) 0.0651(18) Uani 1 1 d . . . H24A H 0.8437 1.3744 0.7987 0.078 Uiso 1 1 calc R . . C25 C 0.7796(3) 1.3241(5) 0.9209(9) 0.087(2) Uani 1 1 d . . . H25A H 0.7729 1.3699 0.9825 0.105 Uiso 1 1 calc R . . C26 C 0.7489(3) 1.2532(6) 0.9362(9) 0.079(2) Uani 1 1 d . . . H26A H 0.7221 1.2504 1.0111 0.094 Uiso 1 1 calc R . . C27 C 0.7268(2) 1.1099(5) 0.8555(12) 0.083(2) Uani 1 1 d . . . H27A H 0.6998 1.1064 0.9299 0.100 Uiso 1 1 calc R . . C28 C 0.7359(3) 1.0435(5) 0.7640(13) 0.096(3) Uani 1 1 d . . . H28A H 0.7149 0.9954 0.7751 0.115 Uiso 1 1 calc R . . C29 C 0.7770(3) 1.0474(5) 0.6525(12) 0.088(2) Uani 1 1 d . . . H29A H 0.7824 1.0022 0.5886 0.106 Uiso 1 1 calc R . . C30 C 0.8085(2) 1.1156(4) 0.6370(10) 0.0655(17) Uani 1 1 d . . . H30A H 0.8366 1.1158 0.5655 0.079 Uiso 1 1 calc R . . C31 C 0.7999(2) 1.1871(4) 0.7273(7) 0.0538(15) Uani 1 1 d . . . C32 C 0.7574(2) 1.1839(4) 0.8400(10) 0.0657(18) Uani 1 1 d . . . C33 C 0.0143(8) 0.0720(12) 0.814(2) 0.196(11) Uani 0.75 1 d P . . H33A H 0.0381 0.0852 0.7292 0.235 Uiso 0.75 1 calc PR . . H33B H 0.0247 0.1090 0.8959 0.235 Uiso 0.75 1 calc PR . . C34 C 0.0270(8) -0.0049(12) 0.858(4) 0.252(15) Uani 0.75 1 d P . . H34A H 0.0652 -0.0070 0.8860 0.378 Uiso 0.75 1 calc PR . . H34B H 0.0204 -0.0430 0.7763 0.378 Uiso 0.75 1 calc PR . . H34C H 0.0047 -0.0201 0.9431 0.378 Uiso 0.75 1 calc PR . . O1 O 1.10376(16) 0.7985(2) 0.7933(5) 0.0560(11) Uani 1 1 d . . . O2 O 0.9415(2) 1.2899(5) 0.7846(6) 0.117(3) Uani 1 1 d . . . O3 O -0.0456(4) 0.0969(6) 0.7660(15) 0.143(4) Uani 0.75 1 d P . . H3 H -0.0584 0.0609 0.7105 0.215 Uiso 0.75 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0524(3) 0.0493(3) 0.0466(4) 0.0057(4) 0.0023(4) -0.0011(3) Br1 0.0932(5) 0.0865(5) 0.0612(5) -0.0100(4) -0.0224(4) 0.0147(4) Br2 0.0628(3) 0.0872(4) 0.0661(5) 0.0114(5) 0.0087(4) -0.0214(3) N1 0.051(3) 0.055(3) 0.043(3) 0.008(2) -0.006(2) -0.009(2) N2 0.065(3) 0.064(3) 0.034(3) 0.005(2) 0.001(2) -0.016(3) N3 0.090(4) 0.046(3) 0.034(3) -0.002(2) 0.005(3) -0.021(3) N4 0.047(3) 0.056(3) 0.050(3) -0.009(2) -0.003(2) -0.005(2) N5 0.052(3) 0.087(4) 0.031(3) -0.007(3) 0.001(2) -0.005(3) N6 0.051(3) 0.098(4) 0.033(3) -0.008(3) 0.000(2) -0.005(3) C1 0.048(3) 0.057(3) 0.038(4) 0.010(3) -0.003(3) -0.008(3) C2 0.045(3) 0.046(3) 0.040(4) 0.001(3) 0.006(3) -0.007(2) C3 0.070(4) 0.061(4) 0.059(5) 0.017(3) -0.010(4) -0.005(3) C4 0.082(5) 0.084(5) 0.061(5) 0.018(4) -0.031(4) -0.027(4) C5 0.087(4) 0.061(4) 0.060(5) 0.014(4) -0.015(4) -0.026(3) C6 0.048(3) 0.047(3) 0.041(4) 0.003(3) 0.002(3) 0.003(2) C7 0.068(4) 0.044(3) 0.039(4) -0.009(3) 0.005(3) -0.004(3) C8 0.074(4) 0.049(3) 0.069(5) -0.001(3) 0.007(4) 0.005(3) C9 0.123(6) 0.053(4) 0.080(6) 0.006(5) -0.005(6) 0.012(4) C10 0.135(7) 0.046(3) 0.070(6) 0.014(4) 0.002(5) -0.010(4) C11 0.133(8) 0.104(6) 0.110(10) -0.024(6) 0.037(7) -0.059(6) C12 0.080(6) 0.124(8) 0.140(11) -0.044(8) 0.005(6) -0.039(6) C13 0.077(5) 0.083(5) 0.130(9) -0.039(6) -0.012(6) -0.006(4) C14 0.059(4) 0.051(3) 0.081(5) -0.020(4) -0.005(4) -0.005(3) C15 0.074(4) 0.038(3) 0.044(4) -0.012(3) 0.003(3) -0.010(3) C16 0.092(5) 0.048(4) 0.078(6) -0.015(3) 0.019(4) -0.027(4) C17 0.051(3) 0.046(3) 0.042(4) 0.001(3) -0.007(3) -0.008(3) C18 0.045(3) 0.060(4) 0.041(4) -0.006(3) -0.001(3) -0.001(3) C19 0.064(4) 0.106(5) 0.070(6) -0.050(5) -0.003(4) 0.007(4) C20 0.066(5) 0.122(6) 0.101(7) -0.067(6) -0.015(4) -0.001(4) C21 0.054(4) 0.089(5) 0.080(6) -0.019(4) -0.008(4) -0.007(3) C22 0.054(4) 0.097(5) 0.030(4) -0.011(3) -0.005(3) 0.002(3) C23 0.053(3) 0.078(4) 0.038(4) -0.001(3) -0.007(3) 0.019(3) C24 0.071(4) 0.075(4) 0.049(5) -0.010(3) -0.006(3) 0.017(3) C25 0.093(5) 0.108(6) 0.061(5) -0.022(4) -0.005(4) 0.048(5) C26 0.056(4) 0.116(6) 0.064(5) 0.004(5) 0.007(4) 0.030(4) C27 0.046(3) 0.111(6) 0.092(6) 0.039(6) 0.008(5) -0.002(4) C28 0.065(5) 0.098(6) 0.125(9) 0.033(6) -0.020(5) -0.006(4) C29 0.070(4) 0.085(5) 0.110(7) 0.009(5) -0.027(5) -0.001(4) C30 0.050(3) 0.075(4) 0.072(5) 0.004(4) -0.012(4) 0.008(3) C31 0.040(3) 0.077(4) 0.044(4) 0.014(3) -0.008(3) 0.014(3) C32 0.039(3) 0.098(4) 0.059(5) 0.022(5) -0.003(4) 0.019(3) C33 0.178(16) 0.224(18) 0.19(2) 0.084(18) -0.121(17) -0.092(15) C34 0.197(18) 0.175(14) 0.38(4) -0.19(2) 0.06(2) -0.026(15) O1 0.076(3) 0.054(2) 0.038(3) 0.0016(18) 0.001(2) -0.013(2) O2 0.064(3) 0.249(8) 0.039(3) -0.036(4) -0.001(2) -0.002(4) O3 0.167(9) 0.143(8) 0.121(9) -0.003(6) 0.032(7) -0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N4 2.056(5) . ? Zn N1 2.067(5) . ? Zn Br1 2.3418(11) . ? Zn Br2 2.3560(8) . ? N1 C5 1.327(8) . ? N1 C1 1.332(6) . ? N2 C6 1.374(7) . ? N2 C2 1.415(7) . ? N2 H2A 0.8600 . ? N3 C6 1.335(7) . ? N3 C7 1.422(7) . ? N3 H3B 0.8600 . ? N4 C21 1.337(8) . ? N4 C17 1.343(7) . ? N5 C22 1.356(8) . ? N5 C18 1.411(7) . ? N5 H5B 0.8600 . ? N6 C22 1.359(7) . ? N6 C23 1.421(8) . ? N6 H6A 0.8600 . ? C1 C2 1.377(7) . ? C1 H1A 0.9300 . ? C2 C3 1.376(9) . ? C3 C4 1.364(8) . ? C3 H3A 0.9300 . ? C4 C5 1.367(9) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O1 1.233(7) . ? C7 C8 1.367(9) . ? C7 C15 1.397(8) . ? C8 C9 1.383(10) . ? C8 H8A 0.9300 . ? C9 C10 1.348(10) . ? C9 H9A 0.9300 . ? C10 C16 1.397(10) . ? C10 H10A 0.9300 . ? C11 C12 1.374(14) . ? C11 C16 1.415(11) . ? C11 H11A 0.9300 . ? C12 C13 1.378(14) . ? C12 H12A 0.9300 . ? C13 C14 1.373(10) . ? C13 H13A 0.9300 . ? C14 C15 1.411(9) . ? C14 H14A 0.9300 . ? C15 C16 1.436(9) . ? C17 C18 1.355(8) . ? C17 H17A 0.9300 . ? C18 C19 1.381(9) . ? C19 C20 1.371(10) . ? C19 H19A 0.9300 . ? C20 C21 1.368(10) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 O2 1.221(8) . ? C23 C24 1.356(9) . ? C23 C31 1.416(8) . ? C24 C25 1.436(10) . ? C24 H24A 0.9300 . ? C25 C26 1.367(11) . ? C25 H25A 0.9300 . ? C26 C32 1.415(11) . ? C26 H26A 0.9300 . ? C27 C28 1.356(12) . ? C27 C32 1.408(9) . ? C27 H27A 0.9300 . ? C28 C29 1.404(13) . ? C28 H28A 0.9300 . ? C29 C30 1.344(9) . ? C29 H29A 0.9300 . ? C30 C31 1.414(10) . ? C30 H30A 0.9300 . ? C31 C32 1.436(9) . ? C33 C34 1.33(2) . ? C33 O3 1.566(18) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? O3 H3 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn N1 101.2(2) . . ? N4 Zn Br1 107.86(14) . . ? N1 Zn Br1 110.15(13) . . ? N4 Zn Br2 107.81(13) . . ? N1 Zn Br2 105.57(12) . . ? Br1 Zn Br2 122.25(4) . . ? C5 N1 C1 119.1(5) . . ? C5 N1 Zn 118.7(4) . . ? C1 N1 Zn 122.2(4) . . ? C6 N2 C2 125.3(5) . . ? C6 N2 H2A 117.4 . . ? C2 N2 H2A 117.4 . . ? C6 N3 C7 121.6(5) . . ? C6 N3 H3B 119.2 . . ? C7 N3 H3B 119.2 . . ? C21 N4 C17 117.2(5) . . ? C21 N4 Zn 120.7(4) . . ? C17 N4 Zn 121.9(4) . . ? C22 N5 C18 123.8(5) . . ? C22 N5 H5B 118.1 . . ? C18 N5 H5B 118.1 . . ? C22 N6 C23 122.0(5) . . ? C22 N6 H6A 119.0 . . ? C23 N6 H6A 119.0 . . ? N1 C1 C2 122.4(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 118.8(5) . . ? C3 C2 N2 122.7(5) . . ? C1 C2 N2 118.4(5) . . ? C4 C3 C2 117.5(6) . . ? C4 C3 H3A 121.2 . . ? C2 C3 H3A 121.2 . . ? C3 C4 C5 121.6(6) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? N1 C5 C4 120.5(5) . . ? N1 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? O1 C6 N3 123.2(5) . . ? O1 C6 N2 121.9(5) . . ? N3 C6 N2 114.8(6) . . ? C8 C7 C15 121.5(6) . . ? C8 C7 N3 119.1(5) . . ? C15 C7 N3 119.4(5) . . ? C7 C8 C9 120.5(6) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C10 C9 C8 120.5(7) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C16 120.6(7) . . ? C9 C10 H10A 119.7 . . ? C16 C10 H10A 119.7 . . ? C12 C11 C16 120.5(9) . . ? C12 C11 H11A 119.7 . . ? C16 C11 H11A 119.7 . . ? C11 C12 C13 121.5(8) . . ? C11 C12 H12A 119.2 . . ? C13 C12 H12A 119.2 . . ? C14 C13 C12 120.4(9) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C7 C15 C14 122.9(6) . . ? C7 C15 C16 116.9(6) . . ? C14 C15 C16 120.1(6) . . ? C10 C16 C11 122.8(8) . . ? C10 C16 C15 119.9(6) . . ? C11 C16 C15 117.3(8) . . ? N4 C17 C18 124.4(5) . . ? N4 C17 H17A 117.8 . . ? C18 C17 H17A 117.8 . . ? C17 C18 C19 118.1(5) . . ? C17 C18 N5 119.6(5) . . ? C19 C18 N5 122.3(5) . . ? C20 C19 C18 118.2(6) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? C21 C20 C19 120.5(7) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? N4 C21 C20 121.6(6) . . ? N4 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? O2 C22 N5 123.2(6) . . ? O2 C22 N6 122.4(6) . . ? N5 C22 N6 114.4(6) . . ? C24 C23 C31 121.3(6) . . ? C24 C23 N6 119.7(6) . . ? C31 C23 N6 118.9(6) . . ? C23 C24 C25 121.0(7) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C26 C25 C24 119.1(7) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C32 121.1(7) . . ? C25 C26 H26A 119.4 . . ? C32 C26 H26A 119.4 . . ? C28 C27 C32 121.3(8) . . ? C28 C27 H27A 119.3 . . ? C32 C27 H27A 119.3 . . ? C27 C28 C29 120.0(8) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.9(8) . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C29 C30 C31 121.3(7) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C30 C31 C23 124.0(6) . . ? C30 C31 C32 118.0(6) . . ? C23 C31 C32 118.0(6) . . ? C27 C32 C26 122.0(8) . . ? C27 C32 C31 118.4(7) . . ? C26 C32 C31 119.5(6) . . ? C34 C33 O3 122.1(14) . . ? C34 C33 H33A 106.8 . . ? O3 C33 H33A 106.8 . . ? C34 C33 H33B 106.8 . . ? O3 C33 H33B 106.8 . . ? H33A C33 H33B 106.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 O3 H3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn N1 C5 -78.1(5) . . . . ? Br1 Zn N1 C5 168.0(5) . . . . ? Br2 Zn N1 C5 34.2(5) . . . . ? N4 Zn N1 C1 101.9(4) . . . . ? Br1 Zn N1 C1 -12.0(5) . . . . ? Br2 Zn N1 C1 -145.8(4) . . . . ? N1 Zn N4 C21 87.6(5) . . . . ? Br1 Zn N4 C21 -156.8(5) . . . . ? Br2 Zn N4 C21 -23.0(5) . . . . ? N1 Zn N4 C17 -87.9(5) . . . . ? Br1 Zn N4 C17 27.7(5) . . . . ? Br2 Zn N4 C17 161.6(4) . . . . ? C5 N1 C1 C2 -0.2(9) . . . . ? Zn N1 C1 C2 179.8(4) . . . . ? N1 C1 C2 C3 -1.9(9) . . . . ? N1 C1 C2 N2 -178.6(5) . . . . ? C6 N2 C2 C3 30.2(8) . . . . ? C6 N2 C2 C1 -153.2(5) . . . . ? C1 C2 C3 C4 1.6(9) . . . . ? N2 C2 C3 C4 178.1(6) . . . . ? C2 C3 C4 C5 0.7(11) . . . . ? C1 N1 C5 C4 2.5(10) . . . . ? Zn N1 C5 C4 -177.5(6) . . . . ? C3 C4 C5 N1 -2.9(12) . . . . ? C7 N3 C6 O1 -4.7(9) . . . . ? C7 N3 C6 N2 176.0(5) . . . . ? C2 N2 C6 O1 8.1(8) . . . . ? C2 N2 C6 N3 -172.6(5) . . . . ? C6 N3 C7 C8 -63.8(8) . . . . ? C6 N3 C7 C15 116.0(6) . . . . ? C15 C7 C8 C9 -2.9(10) . . . . ? N3 C7 C8 C9 176.8(6) . . . . ? C7 C8 C9 C10 2.8(12) . . . . ? C8 C9 C10 C16 -1.5(12) . . . . ? C16 C11 C12 C13 -4.7(15) . . . . ? C11 C12 C13 C14 4.0(15) . . . . ? C12 C13 C14 C15 -1.1(12) . . . . ? C8 C7 C15 C14 179.0(6) . . . . ? N3 C7 C15 C14 -0.8(8) . . . . ? C8 C7 C15 C16 1.7(8) . . . . ? N3 C7 C15 C16 -178.1(5) . . . . ? C13 C14 C15 C7 -178.2(6) . . . . ? C13 C14 C15 C16 -1.0(9) . . . . ? C9 C10 C16 C11 -177.6(8) . . . . ? C9 C10 C16 C15 0.3(11) . . . . ? C12 C11 C16 C10 -179.6(8) . . . . ? C12 C11 C16 C15 2.5(12) . . . . ? C7 C15 C16 C10 -0.3(9) . . . . ? C14 C15 C16 C10 -177.7(6) . . . . ? C7 C15 C16 C11 177.7(6) . . . . ? C14 C15 C16 C11 0.3(9) . . . . ? C21 N4 C17 C18 -0.3(9) . . . . ? Zn N4 C17 C18 175.3(4) . . . . ? N4 C17 C18 C19 0.9(9) . . . . ? N4 C17 C18 N5 178.1(5) . . . . ? C22 N5 C18 C17 148.8(6) . . . . ? C22 N5 C18 C19 -34.1(10) . . . . ? C17 C18 C19 C20 -0.9(11) . . . . ? N5 C18 C19 C20 -178.1(7) . . . . ? C18 C19 C20 C21 0.5(14) . . . . ? C17 N4 C21 C20 -0.1(11) . . . . ? Zn N4 C21 C20 -175.8(7) . . . . ? C19 C20 C21 N4 0.0(14) . . . . ? C18 N5 C22 O2 -0.9(11) . . . . ? C18 N5 C22 N6 179.8(5) . . . . ? C23 N6 C22 O2 -7.9(11) . . . . ? C23 N6 C22 N5 171.4(6) . . . . ? C22 N6 C23 C24 59.9(8) . . . . ? C22 N6 C23 C31 -117.1(7) . . . . ? C31 C23 C24 C25 -0.3(9) . . . . ? N6 C23 C24 C25 -177.3(6) . . . . ? C23 C24 C25 C26 1.3(10) . . . . ? C24 C25 C26 C32 -2.1(11) . . . . ? C32 C27 C28 C29 0.9(13) . . . . ? C27 C28 C29 C30 1.5(12) . . . . ? C28 C29 C30 C31 -3.0(11) . . . . ? C29 C30 C31 C23 -179.7(6) . . . . ? C29 C30 C31 C32 1.9(9) . . . . ? C24 C23 C31 C30 -178.3(6) . . . . ? N6 C23 C31 C30 -1.3(9) . . . . ? C24 C23 C31 C32 0.1(8) . . . . ? N6 C23 C31 C32 177.0(5) . . . . ? C28 C27 C32 C26 -178.9(7) . . . . ? C28 C27 C32 C31 -1.8(11) . . . . ? C25 C26 C32 C27 179.0(7) . . . . ? C25 C26 C32 C31 1.9(10) . . . . ? C30 C31 C32 C27 0.4(9) . . . . ? C23 C31 C32 C27 -178.1(6) . . . . ? C30 C31 C32 C26 177.6(6) . . . . ? C23 C31 C32 C26 -0.8(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O3 0.86 2.51 3.187(12) 135.8 2_664 N3 H3B O2 0.86 1.95 2.810(8) 178.2 2_774 N5 H5B O1 0.86 2.15 2.954(6) 154.5 2_774 N6 H6A O1 0.86 2.27 3.018(7) 144.6 2_774 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.495 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.060 ##################### data_ZnBr2H2O _database_code_depnum_ccdc_archive 'CCDC 874347' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H27.60 Br2 N6 O2.80 Zn' _chemical_formula_weight 766.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.058(9) _cell_length_b 15.927(7) _cell_length_c 8.730(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3345(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 3.163 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3643 _exptl_absorpt_correction_T_max 0.7427 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17075 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.1287 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.28 _reflns_number_total 5977 _reflns_number_gt 3192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.039(18) _refine_ls_number_reflns 5977 _refine_ls_number_parameters 397 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Zn Zn -0.16087(4) -0.15116(6) 0.63623(15) 0.0504(3) Uani 1 1 d . . . Br1 Br -0.10961(6) -0.10967(9) 0.84899(18) 0.0913(5) Uani 1 1 d . . . Br2 Br -0.24889(4) -0.21266(7) 0.64964(17) 0.0720(4) Uani 1 1 d . . . N1 N -0.1712(3) -0.0502(5) 0.4922(9) 0.045(2) Uani 1 1 d . . . N2 N -0.1183(3) 0.1603(5) 0.4455(9) 0.051(2) Uani 1 1 d . . . H2A H -0.1098 0.1702 0.5395 0.061 Uiso 1 1 calc R . . N3 N -0.0776(4) 0.2841(6) 0.3968(10) 0.060(3) Uani 1 1 d . . . H3B H -0.0737 0.2882 0.4945 0.072 Uiso 1 1 calc R . . N4 N -0.1112(4) -0.2280(5) 0.5094(10) 0.052(2) Uani 1 1 d . . . N5 N 0.0355(4) -0.2665(5) 0.4524(10) 0.051(2) Uani 1 1 d . . . H5B H 0.0474 -0.2522 0.5416 0.061 Uiso 1 1 calc R . . N6 N 0.1254(4) -0.2655(6) 0.3866(9) 0.059(2) Uani 1 1 d . . . H6A H 0.1323 -0.2577 0.4822 0.071 Uiso 1 1 calc R . . C1 C -0.1443(4) 0.0197(7) 0.5097(10) 0.041(2) Uani 1 1 d . . . H1A H -0.1200 0.0239 0.5921 0.049 Uiso 1 1 calc R . . C2 C -0.1494(4) 0.0873(6) 0.4156(11) 0.040(2) Uani 1 1 d . . . C3 C -0.1864(4) 0.0816(7) 0.2961(11) 0.052(3) Uani 1 1 d . . . H3A H -0.1922 0.1262 0.2293 0.062 Uiso 1 1 calc R . . C4 C -0.2140(4) 0.0081(8) 0.2802(13) 0.064(3) Uani 1 1 d . . . H4A H -0.2394 0.0023 0.2006 0.077 Uiso 1 1 calc R . . C5 C -0.2057(4) -0.0568(7) 0.3757(13) 0.057(3) Uani 1 1 d . . . H5A H -0.2247 -0.1069 0.3595 0.069 Uiso 1 1 calc R . . C6 C -0.1004(4) 0.2169(6) 0.3385(14) 0.046(2) Uani 1 1 d . . . C7 C -0.0591(5) 0.3512(7) 0.3003(11) 0.051(3) Uani 1 1 d . . . C8 C -0.0963(5) 0.3952(7) 0.2177(13) 0.060(3) Uani 1 1 d . . . H8A H -0.1338 0.3824 0.2287 0.071 Uiso 1 1 calc R . . C9 C -0.0820(6) 0.4568(7) 0.1202(16) 0.080(4) Uani 1 1 d . . . H9A H -0.1090 0.4853 0.0645 0.096 Uiso 1 1 calc R . . C10 C -0.0263(8) 0.4771(8) 0.1042(16) 0.094(5) Uani 1 1 d . . . H10A H -0.0155 0.5181 0.0346 0.113 Uiso 1 1 calc R . . C11 C 0.0694(8) 0.4531(10) 0.179(2) 0.115(6) Uani 1 1 d . . . H11A H 0.0818 0.4947 0.1125 0.139 Uiso 1 1 calc R . . C12 C 0.1066(7) 0.4055(15) 0.269(3) 0.122(8) Uani 1 1 d . . . H12A H 0.1444 0.4181 0.2659 0.146 Uiso 1 1 calc R . . C13 C 0.0889(8) 0.3431(10) 0.358(2) 0.109(6) Uani 1 1 d . . . H13A H 0.1150 0.3110 0.4108 0.131 Uiso 1 1 calc R . . C14 C 0.0368(5) 0.3257(8) 0.3737(15) 0.062(3) Uani 1 1 d . . . H14A H 0.0261 0.2825 0.4392 0.075 Uiso 1 1 calc R . . C15 C -0.0035(5) 0.3704(6) 0.2943(12) 0.050(3) Uani 1 1 d . . . C16 C 0.0144(6) 0.4348(7) 0.1949(14) 0.067(3) Uani 1 1 d . . . C17 C -0.0563(4) -0.2260(6) 0.5169(13) 0.047(3) Uani 1 1 d . . . H17A H -0.0403 -0.1896 0.5875 0.057 Uiso 1 1 calc R . . C18 C -0.0216(4) -0.2732(7) 0.4289(11) 0.046(3) Uani 1 1 d . . . C19 C -0.0452(5) -0.3273(8) 0.3265(15) 0.069(3) Uani 1 1 d . . . H19A H -0.0235 -0.3614 0.2641 0.083 Uiso 1 1 calc R . . C20 C -0.1014(5) -0.3295(9) 0.3193(16) 0.090(4) Uani 1 1 d . . . H20A H -0.1180 -0.3656 0.2492 0.108 Uiso 1 1 calc R . . C21 C -0.1348(5) -0.2812(8) 0.4103(14) 0.076(4) Uani 1 1 d . . . H21A H -0.1733 -0.2853 0.4033 0.091 Uiso 1 1 calc R . . C22 C 0.0722(5) -0.2812(7) 0.3420(15) 0.063(3) Uani 1 1 d . . . C23 C 0.1700(4) -0.2616(7) 0.2796(12) 0.052(3) Uani 1 1 d . . . C24 C 0.1814(5) -0.3280(7) 0.1877(13) 0.062(3) Uani 1 1 d . . . H24A H 0.1610 -0.3774 0.1966 0.074 Uiso 1 1 calc R . . C25 C 0.2245(6) -0.3216(9) 0.0778(14) 0.078(4) Uani 1 1 d . . . H25A H 0.2326 -0.3672 0.0152 0.093 Uiso 1 1 calc R . . C26 C 0.2534(5) -0.2510(10) 0.0635(15) 0.074(4) Uani 1 1 d . . . H26A H 0.2805 -0.2471 -0.0122 0.088 Uiso 1 1 calc R . . C27 C 0.2727(4) -0.1078(9) 0.1454(19) 0.075(4) Uani 1 1 d . . . H27A H 0.3000 -0.1023 0.0708 0.090 Uiso 1 1 calc R . . C28 C 0.2611(6) -0.0430(9) 0.2391(19) 0.081(4) Uani 1 1 d . . . H28A H 0.2812 0.0066 0.2292 0.098 Uiso 1 1 calc R . . C29 C 0.2216(5) -0.0480(8) 0.3459(17) 0.074(4) Uani 1 1 d . . . H29A H 0.2153 -0.0023 0.4100 0.089 Uiso 1 1 calc R . . C30 C 0.1913(4) -0.1157(8) 0.3624(15) 0.058(3) Uani 1 1 d . . . H30A H 0.1632 -0.1163 0.4353 0.069 Uiso 1 1 calc R . . C31 C 0.2005(4) -0.1879(8) 0.2722(12) 0.052(3) Uani 1 1 d . . . C32 C 0.2438(4) -0.1827(8) 0.1600(16) 0.058(3) Uani 1 1 d . . . O1 O -0.1053(3) 0.2036(4) 0.2009(8) 0.0545(19) Uani 1 1 d . . . O2 O 0.0609(3) -0.3018(6) 0.2123(9) 0.087(3) Uani 1 1 d . . . O3 O -0.0057(14) 0.072(2) 0.695(2) 0.43(3) Uani 0.80 1 d P . . H3C H -0.0091 0.0881 0.6019 0.522 Uiso 0.80 1 d PR . . H3D H 0.0166 0.0975 0.7562 0.522 Uiso 0.80 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0572(6) 0.0477(6) 0.0464(7) 0.0062(7) 0.0004(8) -0.0002(5) Br1 0.1174(11) 0.0844(9) 0.0720(9) -0.0112(8) -0.0327(9) 0.0206(8) Br2 0.0697(7) 0.0821(8) 0.0641(7) 0.0103(9) 0.0108(7) -0.0215(6) N1 0.047(5) 0.040(5) 0.048(5) 0.005(4) -0.015(4) -0.002(4) N2 0.060(6) 0.062(6) 0.031(5) 0.009(5) 0.002(4) -0.007(5) N3 0.080(7) 0.060(7) 0.040(6) 0.000(5) 0.001(5) -0.033(5) N4 0.048(6) 0.056(6) 0.051(6) 0.004(5) -0.006(4) 0.002(4) N5 0.055(6) 0.067(6) 0.032(5) -0.004(5) -0.006(4) -0.003(5) N6 0.069(7) 0.086(7) 0.022(5) 0.001(5) 0.002(5) -0.004(5) C1 0.037(6) 0.057(7) 0.030(6) 0.013(5) -0.011(4) 0.006(5) C2 0.039(6) 0.044(6) 0.039(6) -0.006(5) 0.009(5) -0.007(5) C3 0.053(7) 0.059(7) 0.043(7) 0.007(5) -0.005(6) -0.011(6) C4 0.061(8) 0.077(9) 0.054(8) 0.014(7) -0.021(6) -0.006(7) C5 0.057(7) 0.060(7) 0.054(7) 0.006(6) -0.017(6) -0.020(5) C6 0.052(6) 0.045(6) 0.041(7) 0.000(6) 0.002(6) 0.006(5) C7 0.070(8) 0.047(7) 0.035(6) -0.005(5) -0.003(5) -0.004(6) C8 0.079(8) 0.046(7) 0.054(7) 0.012(6) 0.005(6) 0.016(6) C9 0.125(11) 0.051(8) 0.064(9) 0.000(8) 0.000(9) 0.029(7) C10 0.166(15) 0.054(8) 0.063(11) 0.006(7) 0.003(11) -0.017(9) C11 0.126(14) 0.106(13) 0.114(16) -0.040(12) 0.046(13) -0.069(11) C12 0.074(12) 0.138(19) 0.15(2) -0.084(16) 0.020(12) -0.029(13) C13 0.119(16) 0.067(10) 0.141(16) -0.050(12) -0.030(13) -0.027(9) C14 0.054(8) 0.061(8) 0.071(9) -0.021(7) -0.016(7) -0.012(7) C15 0.075(9) 0.036(6) 0.038(7) -0.016(5) 0.001(6) -0.020(6) C16 0.099(10) 0.049(7) 0.055(8) -0.016(6) 0.009(7) -0.022(7) C17 0.053(7) 0.045(7) 0.044(6) 0.001(5) -0.003(5) -0.010(5) C18 0.050(7) 0.057(7) 0.031(6) -0.001(5) 0.003(5) -0.009(5) C19 0.059(8) 0.087(9) 0.061(8) -0.018(8) 0.003(7) -0.003(6) C20 0.071(10) 0.119(11) 0.079(11) -0.055(10) -0.016(8) -0.014(8) C21 0.053(7) 0.105(10) 0.070(9) -0.035(8) -0.013(7) 0.009(7) C22 0.065(8) 0.079(9) 0.046(8) -0.019(7) -0.005(7) 0.010(6) C23 0.062(7) 0.059(8) 0.036(6) 0.003(6) -0.002(5) 0.007(6) C24 0.072(8) 0.060(7) 0.054(8) -0.001(6) 0.009(6) 0.005(6) C25 0.077(9) 0.097(11) 0.059(9) -0.016(7) -0.007(7) 0.038(8) C26 0.046(7) 0.122(12) 0.053(8) 0.008(8) 0.018(6) 0.009(8) C27 0.045(6) 0.100(10) 0.081(9) 0.037(12) -0.008(8) -0.004(7) C28 0.065(9) 0.079(11) 0.100(12) 0.025(9) -0.025(9) -0.009(7) C29 0.053(8) 0.092(11) 0.077(10) -0.005(9) -0.021(8) 0.006(7) C30 0.043(7) 0.069(8) 0.062(8) 0.004(7) -0.008(6) 0.002(6) C31 0.047(7) 0.078(9) 0.032(6) 0.003(6) -0.013(5) 0.012(6) C32 0.041(6) 0.081(8) 0.051(7) 0.014(8) -0.005(6) 0.013(6) O1 0.076(5) 0.057(5) 0.031(4) 0.001(3) 0.000(3) -0.003(3) O2 0.064(5) 0.161(9) 0.036(5) -0.017(5) -0.006(4) -0.021(5) O3 0.62(6) 0.59(6) 0.089(18) 0.01(2) -0.04(2) -0.40(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N4 2.038(8) . ? Zn N1 2.056(8) . ? Zn Br1 2.325(2) . ? Zn Br2 2.3361(16) . ? N1 C1 1.298(11) . ? N1 C5 1.317(12) . ? N2 C6 1.367(12) . ? N2 C2 1.406(11) . ? N2 H2A 0.8600 . ? N3 C6 1.307(12) . ? N3 C7 1.431(13) . ? N3 H3B 0.8600 . ? N4 C17 1.323(12) . ? N4 C21 1.337(13) . ? N5 C22 1.327(14) . ? N5 C18 1.393(13) . ? N5 H5B 0.8600 . ? N6 C22 1.363(13) . ? N6 C23 1.423(13) . ? N6 H6A 0.8600 . ? C1 C2 1.359(12) . ? C1 H1A 0.9300 . ? C2 C3 1.375(13) . ? C3 C4 1.353(14) . ? C3 H3A 0.9300 . ? C4 C5 1.342(14) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O1 1.226(12) . ? C7 C8 1.345(14) . ? C7 C15 1.374(14) . ? C8 C9 1.343(16) . ? C8 H8A 0.9300 . ? C9 C10 1.384(17) . ? C9 H9A 0.9300 . ? C10 C16 1.428(16) . ? C10 H10A 0.9300 . ? C11 C16 1.362(18) . ? C11 C12 1.41(2) . ? C11 H11A 0.9300 . ? C12 C13 1.33(2) . ? C12 H12A 0.9300 . ? C13 C14 1.292(18) . ? C13 H13A 0.9300 . ? C14 C15 1.389(15) . ? C14 H14A 0.9300 . ? C15 C16 1.411(15) . ? C17 C18 1.362(13) . ? C17 H17A 0.9300 . ? C18 C19 1.365(14) . ? C19 C20 1.353(15) . ? C19 H19A 0.9300 . ? C20 C21 1.367(16) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 O2 1.209(13) . ? C23 C24 1.355(14) . ? C23 C31 1.386(15) . ? C24 C25 1.417(15) . ? C24 H24A 0.9300 . ? C25 C26 1.328(17) . ? C25 H25A 0.9300 . ? C26 C32 1.396(17) . ? C26 H26A 0.9300 . ? C27 C28 1.346(18) . ? C27 C32 1.386(15) . ? C27 H27A 0.9300 . ? C28 C29 1.335(17) . ? C28 H28A 0.9300 . ? C29 C30 1.309(15) . ? C29 H29A 0.9300 . ? C30 C31 1.411(15) . ? C30 H30A 0.9300 . ? C31 C32 1.432(15) . ? O3 H3C 0.8600 . ? O3 H3D 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn N1 102.0(3) . . ? N4 Zn Br1 107.1(3) . . ? N1 Zn Br1 109.3(2) . . ? N4 Zn Br2 107.8(3) . . ? N1 Zn Br2 104.4(2) . . ? Br1 Zn Br2 124.05(8) . . ? C1 N1 C5 118.3(9) . . ? C1 N1 Zn 122.6(6) . . ? C5 N1 Zn 119.1(7) . . ? C6 N2 C2 125.8(9) . . ? C6 N2 H2A 117.1 . . ? C2 N2 H2A 117.1 . . ? C6 N3 C7 120.8(9) . . ? C6 N3 H3B 119.6 . . ? C7 N3 H3B 119.6 . . ? C17 N4 C21 118.1(9) . . ? C17 N4 Zn 122.9(7) . . ? C21 N4 Zn 119.0(7) . . ? C22 N5 C18 122.3(9) . . ? C22 N5 H5B 118.9 . . ? C18 N5 H5B 118.9 . . ? C22 N6 C23 121.9(9) . . ? C22 N6 H6A 119.0 . . ? C23 N6 H6A 119.0 . . ? N1 C1 C2 124.3(9) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 117.6(9) . . ? C1 C2 N2 119.7(9) . . ? C3 C2 N2 122.7(9) . . ? C4 C3 C2 116.9(10) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? C5 C4 C3 122.0(10) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? N1 C5 C4 120.8(10) . . ? N1 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? O1 C6 N3 124.3(10) . . ? O1 C6 N2 121.7(10) . . ? N3 C6 N2 114.0(10) . . ? C8 C7 C15 120.7(11) . . ? C8 C7 N3 119.9(11) . . ? C15 C7 N3 119.4(10) . . ? C9 C8 C7 123.4(12) . . ? C9 C8 H8A 118.3 . . ? C7 C8 H8A 118.3 . . ? C8 C9 C10 118.8(12) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C9 C10 C16 119.9(12) . . ? C9 C10 H10A 120.1 . . ? C16 C10 H10A 120.1 . . ? C16 C11 C12 116.5(17) . . ? C16 C11 H11A 121.8 . . ? C12 C11 H11A 121.8 . . ? C13 C12 C11 121.5(17) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C14 C13 C12 122.1(18) . . ? C14 C13 H13A 118.9 . . ? C12 C13 H13A 118.9 . . ? C13 C14 C15 121.0(14) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C7 C15 C14 123.2(11) . . ? C7 C15 C16 118.9(11) . . ? C14 C15 C16 117.8(11) . . ? C11 C16 C15 121.0(14) . . ? C11 C16 C10 120.6(15) . . ? C15 C16 C10 118.3(12) . . ? N4 C17 C18 124.8(10) . . ? N4 C17 H17A 117.6 . . ? C18 C17 H17A 117.6 . . ? C17 C18 C19 117.5(10) . . ? C17 C18 N5 118.6(9) . . ? C19 C18 N5 123.8(10) . . ? C20 C19 C18 117.6(11) . . ? C20 C19 H19A 121.2 . . ? C18 C19 H19A 121.2 . . ? C19 C20 C21 123.1(11) . . ? C19 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? N4 C21 C20 118.9(11) . . ? N4 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? O2 C22 N5 125.4(11) . . ? O2 C22 N6 121.8(11) . . ? N5 C22 N6 112.6(10) . . ? C24 C23 C31 121.7(11) . . ? C24 C23 N6 120.5(10) . . ? C31 C23 N6 117.8(10) . . ? C23 C24 C25 119.5(11) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C26 C25 C24 120.5(12) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C32 121.1(11) . . ? C25 C26 H26A 119.4 . . ? C32 C26 H26A 119.4 . . ? C28 C27 C32 120.1(13) . . ? C28 C27 H27A 120.0 . . ? C32 C27 H27A 120.0 . . ? C29 C28 C27 121.7(13) . . ? C29 C28 H28A 119.1 . . ? C27 C28 H28A 119.1 . . ? C30 C29 C28 121.5(14) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 121.6(12) . . ? C29 C30 H30A 119.2 . . ? C31 C30 H30A 119.2 . . ? C23 C31 C30 125.5(11) . . ? C23 C31 C32 117.8(11) . . ? C30 C31 C32 116.6(11) . . ? C27 C32 C26 122.2(13) . . ? C27 C32 C31 118.5(13) . . ? C26 C32 C31 119.2(11) . . ? H3C O3 H3D 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn N1 C1 -102.3(8) . . . . ? Br1 Zn N1 C1 10.8(8) . . . . ? Br2 Zn N1 C1 145.4(7) . . . . ? N4 Zn N1 C5 76.6(8) . . . . ? Br1 Zn N1 C5 -170.3(7) . . . . ? Br2 Zn N1 C5 -35.6(8) . . . . ? N1 Zn N4 C17 91.3(8) . . . . ? Br1 Zn N4 C17 -23.5(8) . . . . ? Br2 Zn N4 C17 -159.1(7) . . . . ? N1 Zn N4 C21 -86.5(9) . . . . ? Br1 Zn N4 C21 158.7(8) . . . . ? Br2 Zn N4 C21 23.1(9) . . . . ? C5 N1 C1 C2 0.0(14) . . . . ? Zn N1 C1 C2 179.0(7) . . . . ? N1 C1 C2 C3 1.6(14) . . . . ? N1 C1 C2 N2 179.8(9) . . . . ? C6 N2 C2 C1 151.1(9) . . . . ? C6 N2 C2 C3 -30.7(14) . . . . ? C1 C2 C3 C4 -1.4(14) . . . . ? N2 C2 C3 C4 -179.6(9) . . . . ? C2 C3 C4 C5 -0.2(17) . . . . ? C1 N1 C5 C4 -1.7(15) . . . . ? Zn N1 C5 C4 179.3(8) . . . . ? C3 C4 C5 N1 1.8(18) . . . . ? C7 N3 C6 O1 3.7(16) . . . . ? C7 N3 C6 N2 -177.0(9) . . . . ? C2 N2 C6 O1 -7.9(15) . . . . ? C2 N2 C6 N3 172.8(9) . . . . ? C6 N3 C7 C8 65.0(14) . . . . ? C6 N3 C7 C15 -115.7(11) . . . . ? C15 C7 C8 C9 3.3(17) . . . . ? N3 C7 C8 C9 -177.4(11) . . . . ? C7 C8 C9 C10 -0.7(18) . . . . ? C8 C9 C10 C16 -2.3(18) . . . . ? C16 C11 C12 C13 4(2) . . . . ? C11 C12 C13 C14 -4(3) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C8 C7 C15 C14 -178.2(10) . . . . ? N3 C7 C15 C14 2.5(15) . . . . ? C8 C7 C15 C16 -2.7(15) . . . . ? N3 C7 C15 C16 178.0(9) . . . . ? C13 C14 C15 C7 176.2(12) . . . . ? C13 C14 C15 C16 0.6(17) . . . . ? C12 C11 C16 C15 -1(2) . . . . ? C12 C11 C16 C10 -177.4(13) . . . . ? C7 C15 C16 C11 -176.5(11) . . . . ? C14 C15 C16 C11 -0.7(16) . . . . ? C7 C15 C16 C10 -0.3(14) . . . . ? C14 C15 C16 C10 175.5(10) . . . . ? C9 C10 C16 C11 179.0(12) . . . . ? C9 C10 C16 C15 2.8(17) . . . . ? C21 N4 C17 C18 1.2(15) . . . . ? Zn N4 C17 C18 -176.6(8) . . . . ? N4 C17 C18 C19 -0.7(16) . . . . ? N4 C17 C18 N5 -178.1(9) . . . . ? C22 N5 C18 C17 -152.6(10) . . . . ? C22 N5 C18 C19 30.2(16) . . . . ? C17 C18 C19 C20 0.5(17) . . . . ? N5 C18 C19 C20 177.7(11) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C17 N4 C21 C20 -1.4(17) . . . . ? Zn N4 C21 C20 176.5(10) . . . . ? C19 C20 C21 N4 1(2) . . . . ? C18 N5 C22 O2 -0.2(19) . . . . ? C18 N5 C22 N6 175.9(9) . . . . ? C23 N6 C22 O2 8.4(18) . . . . ? C23 N6 C22 N5 -167.9(10) . . . . ? C22 N6 C23 C24 -57.7(14) . . . . ? C22 N6 C23 C31 121.6(11) . . . . ? C31 C23 C24 C25 -1.8(16) . . . . ? N6 C23 C24 C25 177.5(9) . . . . ? C23 C24 C25 C26 -0.6(17) . . . . ? C24 C25 C26 C32 2.7(19) . . . . ? C32 C27 C28 C29 -1(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 2.5(18) . . . . ? C24 C23 C31 C30 179.5(10) . . . . ? N6 C23 C31 C30 0.1(15) . . . . ? C24 C23 C31 C32 2.0(15) . . . . ? N6 C23 C31 C32 -177.4(9) . . . . ? C29 C30 C31 C23 -178.7(11) . . . . ? C29 C30 C31 C32 -1.1(15) . . . . ? C28 C27 C32 C26 178.5(11) . . . . ? C28 C27 C32 C31 2.3(17) . . . . ? C25 C26 C32 C27 -178.7(12) . . . . ? C25 C26 C32 C31 -2.5(18) . . . . ? C23 C31 C32 C27 176.5(10) . . . . ? C30 C31 C32 C27 -1.2(15) . . . . ? C23 C31 C32 C26 0.2(15) . . . . ? C30 C31 C32 C26 -177.6(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O2 0.86 1.94 2.797(13) 176.5 2 N5 H5B O1 0.86 2.11 2.920(10) 155.7 2 N6 H6A O1 0.86 2.19 2.955(11) 147.6 2 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.837 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.095 ##################### data_ZnI2 _database_code_depnum_ccdc_archive 'CCDC 874348' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 I2 N6 O2 Zn' _chemical_formula_weight 845.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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 25.815(2) _cell_length_b 8.8838(8) _cell_length_c 28.137(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6452.9(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 2.713 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30905 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5679 _reflns_number_gt 3180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^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 5679 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Zn Zn 0.62204(3) 0.66327(8) 0.10119(3) 0.0455(2) Uani 1 1 d . . . I1 I 0.534632(18) 0.79819(5) 0.103062(16) 0.06389(17) Uani 1 1 d . . . I2 I 0.70392(2) 0.81607(6) 0.111662(19) 0.0786(2) Uani 1 1 d . . . N1 N 0.62184(19) 0.5248(5) 0.04185(16) 0.0399(12) Uani 1 1 d . . . N2 N 0.71041(18) 0.2547(5) -0.01365(17) 0.0444(13) Uani 1 1 d . . . H2A H 0.7094 0.1580 -0.0138 0.053 Uiso 1 1 calc R . . N3 N 0.79485(18) 0.2254(5) -0.03385(16) 0.0398(12) Uani 1 1 d . . . H3B H 0.7875 0.1312 -0.0320 0.048 Uiso 1 1 calc R . . N4 N 0.62627(19) 0.4784(6) 0.14633(18) 0.0474(13) Uani 1 1 d . . . N5 N 0.71120(19) 0.3409(5) 0.23826(18) 0.0520(15) Uani 1 1 d . . . H5B H 0.7224 0.4289 0.2458 0.062 Uiso 1 1 calc R . . N6 N 0.7765(2) 0.2637(5) 0.28614(19) 0.0580(16) Uani 1 1 d . . . H6A H 0.7819 0.3580 0.2910 0.070 Uiso 1 1 calc R . . O1 O 0.76092(14) 0.4601(4) -0.02625(15) 0.0524(12) Uani 1 1 d . . . O2 O 0.72070(15) 0.0926(4) 0.25584(15) 0.0510(11) Uani 1 1 d . . . C1 C 0.6643(2) 0.4472(6) 0.0309(2) 0.0403(15) Uani 1 1 d . . . H1A H 0.6951 0.4707 0.0463 0.048 Uiso 1 1 calc R . . C2 C 0.6644(2) 0.3329(6) -0.0026(2) 0.0384(15) Uani 1 1 d . . . C3 C 0.6195(2) 0.2953(7) -0.0246(2) 0.0530(18) Uani 1 1 d . . . H3A H 0.6187 0.2175 -0.0467 0.064 Uiso 1 1 calc R . . C4 C 0.5750(2) 0.3745(8) -0.0136(2) 0.061(2) Uani 1 1 d . . . H4A H 0.5436 0.3503 -0.0279 0.074 Uiso 1 1 calc R . . C5 C 0.5779(2) 0.4892(7) 0.0189(2) 0.0531(18) Uani 1 1 d . . . H5A H 0.5482 0.5449 0.0252 0.064 Uiso 1 1 calc R . . C6 C 0.7564(2) 0.3226(6) -0.0242(2) 0.0375(15) Uani 1 1 d . . . C7 C 0.8460(2) 0.2620(6) -0.0467(2) 0.0392(15) Uani 1 1 d . . . C8 C 0.8743(2) 0.3682(7) -0.0228(2) 0.0499(17) Uani 1 1 d . . . H8A H 0.8593 0.4221 0.0020 0.060 Uiso 1 1 calc R . . C9 C 0.9260(3) 0.3953(8) -0.0358(3) 0.063(2) Uani 1 1 d . . . H9A H 0.9449 0.4695 -0.0202 0.076 Uiso 1 1 calc R . . C10 C 0.9484(3) 0.3138(9) -0.0710(3) 0.071(2) Uani 1 1 d . . . H10A H 0.9829 0.3314 -0.0788 0.086 Uiso 1 1 calc R . . C11 C 0.9438(3) 0.1161(11) -0.1323(3) 0.083(3) Uani 1 1 d . . . H11A H 0.9783 0.1331 -0.1402 0.100 Uiso 1 1 calc R . . C12 C 0.9170(4) 0.0098(10) -0.1554(3) 0.086(3) Uani 1 1 d . . . H12A H 0.9331 -0.0466 -0.1790 0.103 Uiso 1 1 calc R . . C13 C 0.8656(3) -0.0167(8) -0.1446(3) 0.069(2) Uani 1 1 d . . . H13A H 0.8471 -0.0901 -0.1609 0.083 Uiso 1 1 calc R . . C14 C 0.8422(3) 0.0651(7) -0.1098(2) 0.0536(18) Uani 1 1 d . . . H14A H 0.8074 0.0472 -0.1032 0.064 Uiso 1 1 calc R . . C15 C 0.8685(2) 0.1758(7) -0.0835(2) 0.0406(15) Uani 1 1 d . . . C16 C 0.9204(3) 0.2033(8) -0.0958(3) 0.0588(19) Uani 1 1 d . . . C17 C 0.6641(2) 0.4645(7) 0.1784(2) 0.0445(16) Uani 1 1 d . . . H17A H 0.6871 0.5440 0.1823 0.053 Uiso 1 1 calc R . . C18 C 0.6706(2) 0.3375(6) 0.2062(2) 0.0455(16) Uani 1 1 d . . . C19 C 0.6381(3) 0.2181(8) 0.1992(3) 0.081(3) Uani 1 1 d . . . H19A H 0.6419 0.1297 0.2165 0.098 Uiso 1 1 calc R . . C20 C 0.5996(3) 0.2327(9) 0.1658(3) 0.089(3) Uani 1 1 d . . . H20A H 0.5770 0.1530 0.1604 0.107 Uiso 1 1 calc R . . C21 C 0.5940(3) 0.3636(9) 0.1401(3) 0.075(2) Uani 1 1 d . . . H21A H 0.5673 0.3717 0.1180 0.090 Uiso 1 1 calc R . . C22 C 0.7356(2) 0.2228(7) 0.2594(2) 0.0438(16) Uani 1 1 d . . . C23 C 0.8112(3) 0.1575(6) 0.3067(2) 0.0439(16) Uani 1 1 d . . . C24 C 0.7946(2) 0.0674(7) 0.3418(2) 0.0532(18) Uani 1 1 d . . . H24A H 0.7610 0.0773 0.3532 0.064 Uiso 1 1 calc R . . C25 C 0.8278(3) -0.0422(8) 0.3616(3) 0.069(2) Uani 1 1 d . . . H25A H 0.8158 -0.1066 0.3852 0.083 Uiso 1 1 calc R . . C26 C 0.8766(3) -0.0528(8) 0.3461(3) 0.071(2) Uani 1 1 d . . . H26A H 0.8984 -0.1243 0.3596 0.085 Uiso 1 1 calc R . . C27 C 0.9463(4) 0.0295(12) 0.2938(4) 0.109(3) Uani 1 1 d . . . H27A H 0.9684 -0.0418 0.3070 0.130 Uiso 1 1 calc R . . C28 C 0.9641(4) 0.1194(16) 0.2593(4) 0.130(4) Uani 1 1 d . . . H28A H 0.9982 0.1110 0.2492 0.156 Uiso 1 1 calc R . . C29 C 0.9311(4) 0.2268(13) 0.2383(3) 0.103(3) Uani 1 1 d . . . H29A H 0.9437 0.2872 0.2139 0.123 Uiso 1 1 calc R . . C30 C 0.8815(3) 0.2440(9) 0.2528(2) 0.070(2) Uani 1 1 d . . . H30A H 0.8604 0.3172 0.2392 0.084 Uiso 1 1 calc R . . C31 C 0.8619(3) 0.1478(7) 0.2895(2) 0.0492(17) Uani 1 1 d . . . C32 C 0.8958(3) 0.0400(8) 0.3104(2) 0.0573(19) 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 Zn 0.0466(5) 0.0422(4) 0.0477(5) -0.0029(4) -0.0030(4) 0.0062(3) I1 0.0608(3) 0.0723(3) 0.0586(3) -0.0137(3) -0.0052(2) 0.0284(3) I2 0.0741(4) 0.0848(4) 0.0768(4) 0.0032(3) -0.0135(3) -0.0287(3) N1 0.036(3) 0.039(3) 0.044(3) 0.000(2) -0.003(3) 0.013(3) N2 0.039(3) 0.020(3) 0.074(4) -0.007(3) 0.013(3) -0.001(2) N3 0.039(3) 0.018(3) 0.062(3) -0.005(2) 0.010(3) -0.002(2) N4 0.043(4) 0.051(3) 0.048(3) 0.006(3) -0.011(3) -0.001(3) N5 0.062(4) 0.025(3) 0.069(4) 0.006(3) -0.020(3) -0.001(3) N6 0.063(4) 0.032(3) 0.079(4) 0.008(3) -0.026(3) 0.001(3) O1 0.043(3) 0.021(2) 0.093(4) -0.003(2) 0.004(2) 0.001(2) O2 0.054(3) 0.026(2) 0.072(3) 0.005(2) -0.013(2) -0.006(2) C1 0.033(4) 0.036(4) 0.052(4) 0.003(3) -0.002(3) 0.002(3) C2 0.035(4) 0.029(4) 0.051(4) -0.001(3) 0.004(3) -0.001(3) C3 0.051(4) 0.040(4) 0.068(5) -0.021(4) 0.004(4) -0.003(4) C4 0.036(4) 0.066(5) 0.081(5) -0.027(4) -0.009(4) 0.003(4) C5 0.037(4) 0.055(4) 0.067(5) -0.015(4) -0.007(3) 0.018(3) C6 0.042(4) 0.023(3) 0.048(4) 0.000(3) 0.001(3) 0.004(3) C7 0.032(4) 0.028(3) 0.058(4) 0.009(3) 0.000(3) 0.008(3) C8 0.053(5) 0.036(4) 0.060(5) 0.007(3) -0.005(4) -0.006(3) C9 0.050(5) 0.053(5) 0.086(6) 0.012(4) -0.015(4) -0.020(4) C10 0.035(4) 0.084(6) 0.096(6) 0.022(5) 0.008(4) 0.004(4) C11 0.055(6) 0.105(7) 0.090(7) 0.016(6) 0.022(5) 0.013(5) C12 0.078(7) 0.098(7) 0.080(6) -0.007(5) 0.030(5) 0.031(6) C13 0.082(6) 0.064(5) 0.062(5) -0.012(4) 0.006(4) 0.019(4) C14 0.048(4) 0.050(4) 0.063(5) 0.004(4) 0.003(4) 0.005(4) C15 0.029(4) 0.039(4) 0.053(4) 0.009(3) 0.005(3) 0.005(3) C16 0.043(5) 0.065(5) 0.068(5) 0.015(4) 0.005(4) 0.007(4) C17 0.049(4) 0.038(4) 0.046(4) -0.004(3) -0.002(3) -0.002(3) C18 0.045(4) 0.032(4) 0.059(4) 0.003(3) -0.006(3) -0.001(3) C19 0.075(6) 0.070(5) 0.099(6) 0.038(5) -0.032(5) -0.028(5) C20 0.065(5) 0.082(6) 0.121(7) 0.038(5) -0.041(5) -0.034(5) C21 0.046(5) 0.089(6) 0.091(6) 0.034(5) -0.024(4) -0.019(5) C22 0.042(4) 0.042(4) 0.048(4) 0.006(3) -0.003(3) 0.012(3) C23 0.055(5) 0.031(4) 0.045(4) 0.002(3) -0.011(3) -0.001(3) C24 0.051(5) 0.045(4) 0.063(5) 0.001(4) -0.002(4) -0.005(4) C25 0.090(7) 0.051(5) 0.067(5) 0.016(4) -0.020(5) -0.008(5) C26 0.083(6) 0.057(5) 0.073(6) 0.017(4) -0.023(5) 0.024(5) C27 0.067(7) 0.159(10) 0.100(8) -0.026(7) -0.003(6) 0.040(7) C28 0.068(8) 0.215(14) 0.107(10) -0.026(9) 0.027(7) 0.000(8) C29 0.091(8) 0.163(10) 0.054(6) -0.015(6) 0.021(5) -0.031(7) C30 0.081(6) 0.082(6) 0.047(5) 0.005(4) 0.000(4) -0.022(5) C31 0.054(5) 0.052(4) 0.042(4) -0.001(3) -0.007(3) -0.006(4) C32 0.052(5) 0.068(5) 0.052(5) -0.004(4) -0.013(4) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N1 2.074(5) . ? Zn N4 2.079(5) . ? Zn I2 2.5293(9) . ? Zn I1 2.5556(8) . ? N1 C1 1.331(6) . ? N1 C5 1.343(7) . ? N2 C6 1.364(7) . ? N2 C2 1.410(7) . ? N2 H2A 0.8600 . ? N3 C6 1.343(6) . ? N3 C7 1.409(7) . ? N3 H3B 0.8600 . ? N4 C21 1.329(8) . ? N4 C17 1.335(7) . ? N5 C22 1.361(7) . ? N5 C18 1.384(7) . ? N5 H5B 0.8600 . ? N6 C22 1.347(7) . ? N6 C23 1.423(7) . ? N6 H6A 0.8600 . ? O1 C6 1.229(6) . ? O2 C22 1.223(7) . ? C1 C2 1.384(7) . ? C1 H1A 0.9300 . ? C2 C3 1.356(8) . ? C3 C4 1.384(8) . ? C3 H3A 0.9300 . ? C4 C5 1.371(8) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.369(8) . ? C7 C15 1.411(8) . ? C8 C9 1.404(8) . ? C8 H8A 0.9300 . ? C9 C10 1.356(9) . ? C9 H9A 0.9300 . ? C10 C16 1.404(9) . ? C10 H10A 0.9300 . ? C11 C12 1.340(10) . ? C11 C16 1.422(10) . ? C11 H11A 0.9300 . ? C12 C13 1.382(10) . ? C12 H12A 0.9300 . ? C13 C14 1.359(8) . ? C13 H13A 0.9300 . ? C14 C15 1.407(8) . ? C14 H14A 0.9300 . ? C15 C16 1.405(8) . ? C17 C18 1.383(7) . ? C17 H17A 0.9300 . ? C18 C19 1.367(8) . ? C19 C20 1.374(9) . ? C19 H19A 0.9300 . ? C20 C21 1.376(9) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C23 C24 1.343(8) . ? C23 C31 1.397(8) . ? C24 C25 1.412(8) . ? C24 H24A 0.9300 . ? C25 C26 1.336(9) . ? C25 H25A 0.9300 . ? C26 C32 1.390(9) . ? C26 H26A 0.9300 . ? C27 C28 1.339(13) . ? C27 C32 1.389(10) . ? C27 H27A 0.9300 . ? C28 C29 1.408(13) . ? C28 H28A 0.9300 . ? C29 C30 1.354(10) . ? C29 H29A 0.9300 . ? C30 C31 1.433(9) . ? C30 H30A 0.9300 . ? C31 C32 1.425(8) . ? 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 Zn N4 91.35(19) . . ? N1 Zn I2 114.47(14) . . ? N4 Zn I2 107.99(14) . . ? N1 Zn I1 107.01(14) . . ? N4 Zn I1 113.84(14) . . ? I2 Zn I1 118.93(3) . . ? C1 N1 C5 117.4(5) . . ? C1 N1 Zn 119.5(4) . . ? C5 N1 Zn 122.0(4) . . ? C6 N2 C2 124.3(5) . . ? C6 N2 H2A 117.9 . . ? C2 N2 H2A 117.9 . . ? C6 N3 C7 126.7(5) . . ? C6 N3 H3B 116.7 . . ? C7 N3 H3B 116.7 . . ? C21 N4 C17 118.4(6) . . ? C21 N4 Zn 119.5(4) . . ? C17 N4 Zn 121.6(4) . . ? C22 N5 C18 128.3(5) . . ? C22 N5 H5B 115.9 . . ? C18 N5 H5B 115.9 . . ? C22 N6 C23 122.7(5) . . ? C22 N6 H6A 118.6 . . ? C23 N6 H6A 118.6 . . ? N1 C1 C2 122.8(5) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 N2 119.8(5) . . ? C1 C2 N2 121.0(5) . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 118.8(6) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 122.9(6) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O1 C6 N3 124.0(6) . . ? O1 C6 N2 122.2(5) . . ? N3 C6 N2 113.8(5) . . ? C8 C7 N3 122.1(6) . . ? C8 C7 C15 121.0(6) . . ? N3 C7 C15 116.7(5) . . ? C7 C8 C9 119.7(6) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 120.3(7) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C16 121.1(7) . . ? C9 C10 H10A 119.4 . . ? C16 C10 H10A 119.4 . . ? C12 C11 C16 121.0(8) . . ? C12 C11 H11A 119.5 . . ? C16 C11 H11A 119.5 . . ? C11 C12 C13 120.6(8) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 119.7(7) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 122.5(6) . . ? C13 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C16 C15 C14 117.0(6) . . ? C16 C15 C7 118.5(6) . . ? C14 C15 C7 124.5(6) . . ? C10 C16 C15 119.3(7) . . ? C10 C16 C11 121.5(7) . . ? C15 C16 C11 119.2(7) . . ? N4 C17 C18 123.1(6) . . ? N4 C17 H17A 118.5 . . ? C18 C17 H17A 118.5 . . ? C19 C18 C17 118.5(6) . . ? C19 C18 N5 125.2(6) . . ? C17 C18 N5 116.2(5) . . ? C18 C19 C20 118.0(7) . . ? C18 C19 H19A 121.0 . . ? C20 C19 H19A 121.0 . . ? C19 C20 C21 121.0(7) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? N4 C21 C20 120.9(6) . . ? N4 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? O2 C22 N6 123.2(6) . . ? O2 C22 N5 123.2(6) . . ? N6 C22 N5 113.5(6) . . ? C24 C23 C31 121.1(6) . . ? C24 C23 N6 119.6(6) . . ? C31 C23 N6 119.3(6) . . ? C23 C24 C25 120.5(7) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 119.5(7) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C32 122.0(7) . . ? C25 C26 H26A 119.0 . . ? C32 C26 H26A 119.0 . . ? C28 C27 C32 121.7(10) . . ? C28 C27 H27A 119.1 . . ? C32 C27 H27A 119.1 . . ? C27 C28 C29 120.1(10) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 121.5(10) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 119.0(8) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? C23 C31 C32 118.3(6) . . ? C23 C31 C30 122.8(7) . . ? C32 C31 C30 118.8(7) . . ? C27 C32 C26 122.5(8) . . ? C27 C32 C31 118.9(8) . . ? C26 C32 C31 118.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zn N1 C1 -68.2(4) . . . . ? I2 Zn N1 C1 42.3(4) . . . . ? I1 Zn N1 C1 176.3(4) . . . . ? N4 Zn N1 C5 99.5(5) . . . . ? I2 Zn N1 C5 -150.0(4) . . . . ? I1 Zn N1 C5 -16.0(5) . . . . ? N1 Zn N4 C21 -48.6(5) . . . . ? I2 Zn N4 C21 -164.9(5) . . . . ? I1 Zn N4 C21 60.7(5) . . . . ? N1 Zn N4 C17 124.2(5) . . . . ? I2 Zn N4 C17 7.9(5) . . . . ? I1 Zn N4 C17 -126.5(4) . . . . ? C5 N1 C1 C2 -0.4(8) . . . . ? Zn N1 C1 C2 167.9(4) . . . . ? N1 C1 C2 C3 -1.4(9) . . . . ? N1 C1 C2 N2 179.1(5) . . . . ? C6 N2 C2 C3 131.3(6) . . . . ? C6 N2 C2 C1 -49.2(8) . . . . ? C1 C2 C3 C4 1.2(9) . . . . ? N2 C2 C3 C4 -179.3(6) . . . . ? C2 C3 C4 C5 0.6(10) . . . . ? C1 N1 C5 C4 2.4(9) . . . . ? Zn N1 C5 C4 -165.6(5) . . . . ? C3 C4 C5 N1 -2.6(10) . . . . ? C7 N3 C6 O1 1.3(10) . . . . ? C7 N3 C6 N2 178.7(5) . . . . ? C2 N2 C6 O1 -2.3(9) . . . . ? C2 N2 C6 N3 -179.7(5) . . . . ? C6 N3 C7 C8 46.7(8) . . . . ? C6 N3 C7 C15 -138.0(6) . . . . ? N3 C7 C8 C9 177.1(5) . . . . ? C15 C7 C8 C9 2.0(9) . . . . ? C7 C8 C9 C10 -2.0(10) . . . . ? C8 C9 C10 C16 1.4(11) . . . . ? C16 C11 C12 C13 0.5(13) . . . . ? C11 C12 C13 C14 -0.5(12) . . . . ? C12 C13 C14 C15 -1.0(10) . . . . ? C13 C14 C15 C16 2.4(9) . . . . ? C13 C14 C15 C7 -179.2(6) . . . . ? C8 C7 C15 C16 -1.4(9) . . . . ? N3 C7 C15 C16 -176.7(5) . . . . ? C8 C7 C15 C14 -179.8(6) . . . . ? N3 C7 C15 C14 4.9(8) . . . . ? C9 C10 C16 C15 -0.8(10) . . . . ? C9 C10 C16 C11 -179.2(7) . . . . ? C14 C15 C16 C10 179.3(6) . . . . ? C7 C15 C16 C10 0.7(9) . . . . ? C14 C15 C16 C11 -2.2(9) . . . . ? C7 C15 C16 C11 179.2(6) . . . . ? C12 C11 C16 C10 179.3(8) . . . . ? C12 C11 C16 C15 0.9(11) . . . . ? C21 N4 C17 C18 -1.4(9) . . . . ? Zn N4 C17 C18 -174.3(4) . . . . ? N4 C17 C18 C19 2.6(10) . . . . ? N4 C17 C18 N5 -179.2(5) . . . . ? C22 N5 C18 C19 18.8(11) . . . . ? C22 N5 C18 C17 -159.2(6) . . . . ? C17 C18 C19 C20 -1.9(12) . . . . ? N5 C18 C19 C20 -179.9(7) . . . . ? C18 C19 C20 C21 0.1(14) . . . . ? C17 N4 C21 C20 -0.5(11) . . . . ? Zn N4 C21 C20 172.6(6) . . . . ? C19 C20 C21 N4 1.2(14) . . . . ? C23 N6 C22 O2 10.4(10) . . . . ? C23 N6 C22 N5 -172.2(5) . . . . ? C18 N5 C22 O2 -7.5(10) . . . . ? C18 N5 C22 N6 175.1(6) . . . . ? C22 N6 C23 C24 -68.6(8) . . . . ? C22 N6 C23 C31 110.7(7) . . . . ? C31 C23 C24 C25 -1.5(9) . . . . ? N6 C23 C24 C25 177.8(5) . . . . ? C23 C24 C25 C26 2.1(10) . . . . ? C24 C25 C26 C32 -0.9(11) . . . . ? C32 C27 C28 C29 -0.9(17) . . . . ? C27 C28 C29 C30 1.3(17) . . . . ? C28 C29 C30 C31 -1.7(13) . . . . ? C24 C23 C31 C32 -0.2(9) . . . . ? N6 C23 C31 C32 -179.6(5) . . . . ? C24 C23 C31 C30 -178.6(6) . . . . ? N6 C23 C31 C30 2.1(9) . . . . ? C29 C30 C31 C23 -180.0(7) . . . . ? C29 C30 C31 C32 1.7(10) . . . . ? C28 C27 C32 C26 179.8(9) . . . . ? C28 C27 C32 C31 1.0(13) . . . . ? C25 C26 C32 C27 -179.6(8) . . . . ? C25 C26 C32 C31 -0.8(11) . . . . ? C23 C31 C32 C27 -179.8(7) . . . . ? C30 C31 C32 C27 -1.4(10) . . . . ? C23 C31 C32 C26 1.4(9) . . . . ? C30 C31 C32 C26 179.8(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1A O1 0.93 2.66 2.970(7) 100.4 . C19 H19A O2 0.93 2.34 2.888(8) 117.3 . N2 H2A O1 0.86 1.95 2.743(6) 152.9 8_755 N3 H3B O1 0.86 1.97 2.770(6) 153.5 8_755 N5 H5B O2 0.86 2.09 2.887(6) 154.7 8_765 N6 H6A O2 0.86 2.31 3.044(6) 143.7 8_765 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.916 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.093 ##################### data_HgCl2 _database_code_depnum_ccdc_archive 'CCDC 874349' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Cl2 Hg N6 O2' _chemical_formula_weight 798.08 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.713(3) _cell_length_b 20.677(6) _cell_length_c 15.911(3) _cell_angle_alpha 90.00 _cell_angle_beta 125.323(14) _cell_angle_gamma 90.00 _cell_volume 3144.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 5.105 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3096 _exptl_absorpt_correction_T_max 0.3618 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15604 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5523 _reflns_number_gt 4339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^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 5523 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg -0.269653(18) 0.121924(9) -0.198094(14) 0.05379(9) Uani 1 1 d . . . Cl1 Cl -0.44497(13) 0.04158(6) -0.24951(12) 0.0706(4) Uani 1 1 d . . . Cl2 Cl -0.06779(14) 0.18400(9) -0.08065(11) 0.0850(5) Uani 1 1 d . . . O1 O -0.8405(3) 0.13478(13) -0.5036(2) 0.0426(7) Uani 1 1 d . . . O2 O 0.1020(4) 0.20766(18) -0.2489(3) 0.0760(12) Uani 1 1 d . . . N1 N -0.4281(4) 0.20501(18) -0.3198(3) 0.0487(9) Uani 1 1 d . . . N2 N -0.7749(4) 0.21435(17) -0.5694(3) 0.0479(9) Uani 1 1 d . . . H2B H -0.8007 0.2367 -0.6244 0.057 Uiso 1 1 d R . . N3 N -0.9729(4) 0.15569(19) -0.6782(3) 0.0530(10) Uani 1 1 d . . . H3B H -0.9782 0.1801 -0.7251 0.064 Uiso 1 1 d R . . N4 N -0.1968(4) 0.07700(18) -0.3053(3) 0.0484(9) Uani 1 1 d . . . N5 N 0.0595(4) 0.12427(17) -0.3600(3) 0.0488(9) Uani 1 1 d . . . H5B H 0.0824 0.1086 -0.3991 0.059 Uiso 1 1 d R . . N6 N 0.2193(4) 0.2035(2) -0.3229(3) 0.0560(11) Uani 1 1 d . . . H6B H 0.2314 0.1836 -0.3655 0.067 Uiso 1 1 d R . . C1 C -0.5515(4) 0.1874(2) -0.4054(3) 0.0429(10) Uani 1 1 d . . . H1A H -0.5743 0.1437 -0.4174 0.052 Uiso 1 1 calc R . . C2 C -0.6473(4) 0.2330(2) -0.4772(3) 0.0420(10) Uani 1 1 d . . . C3 C -0.6099(6) 0.2978(2) -0.4579(4) 0.0620(13) Uani 1 1 d . . . H3A H -0.6706 0.3293 -0.5040 0.074 Uiso 1 1 calc R . . C4 C -0.4818(6) 0.3155(3) -0.3695(4) 0.0727(16) Uani 1 1 d . . . H4A H -0.4558 0.3588 -0.3560 0.087 Uiso 1 1 calc R . . C5 C -0.3934(6) 0.2682(2) -0.3017(4) 0.0642(14) Uani 1 1 d . . . H5A H -0.3079 0.2802 -0.2422 0.077 Uiso 1 1 calc R . . C6 C -0.8628(4) 0.1658(2) -0.5782(3) 0.0406(10) Uani 1 1 d . . . C7 C -1.0806(4) 0.1078(2) -0.7113(3) 0.0426(10) Uani 1 1 d . . . C8 C -1.1466(4) 0.1013(2) -0.6630(3) 0.0501(11) Uani 1 1 d . . . H8A H -1.1214 0.1278 -0.6076 0.060 Uiso 1 1 calc R . . C9 C -1.2531(4) 0.0539(3) -0.6977(4) 0.0594(13) Uani 1 1 d . . . H9A H -1.2959 0.0492 -0.6637 0.071 Uiso 1 1 calc R . . C10 C -1.2935(5) 0.0154(2) -0.7803(4) 0.0610(13) Uani 1 1 d . . . H10A H -1.3646 -0.0147 -0.8026 0.073 Uiso 1 1 calc R . . C11 C -1.2684(7) -0.0189(3) -0.9181(5) 0.0799(17) Uani 1 1 d . . . H11A H -1.3406 -0.0485 -0.9418 0.096 Uiso 1 1 calc R . . C12 C -1.2043(8) -0.0149(3) -0.9668(5) 0.095(2) Uani 1 1 d . . . H12A H -1.2328 -0.0412 -1.0231 0.114 Uiso 1 1 calc R . . C13 C -1.0954(7) 0.0291(3) -0.9315(5) 0.0870(18) Uani 1 1 d . . . H13A H -1.0502 0.0312 -0.9639 0.104 Uiso 1 1 calc R . . C14 C -1.0531(5) 0.0696(3) -0.8492(4) 0.0634(13) Uani 1 1 d . . . H14A H -0.9812 0.0991 -0.8279 0.076 Uiso 1 1 calc R . . C15 C -1.1181(4) 0.0668(2) -0.7969(3) 0.0449(10) Uani 1 1 d . . . C16 C -1.2289(5) 0.0205(2) -0.8324(4) 0.0522(11) Uani 1 1 d . . . C17 C -0.0893(4) 0.1077(2) -0.2973(3) 0.0445(10) Uani 1 1 d . . . H17A H -0.0425 0.1405 -0.2489 0.053 Uiso 1 1 calc R . . C18 C -0.0467(4) 0.09104(19) -0.3608(3) 0.0380(9) Uani 1 1 d . . . C19 C -0.1127(4) 0.0386(2) -0.4284(3) 0.0453(10) Uani 1 1 d . . . H19A H -0.0827 0.0245 -0.4682 0.054 Uiso 1 1 calc R . . C20 C -0.2238(5) 0.0079(2) -0.4351(4) 0.0546(12) Uani 1 1 d . . . H20A H -0.2712 -0.0259 -0.4813 0.066 Uiso 1 1 calc R . . C21 C -0.2625(5) 0.0284(2) -0.3723(4) 0.0540(12) Uani 1 1 d . . . H21A H -0.3363 0.0078 -0.3766 0.065 Uiso 1 1 calc R . . C22 C 0.1257(4) 0.1806(2) -0.3067(3) 0.0472(11) Uani 1 1 d . . . C23 C 0.3050(5) 0.2597(2) -0.2655(4) 0.0458(11) Uani 1 1 d . . . C24 C 0.2542(5) 0.3209(3) -0.3034(4) 0.0630(14) Uani 1 1 d . . . H24A H 0.1666 0.3256 -0.3655 0.076 Uiso 1 1 calc R . . C25 C 0.3318(7) 0.3762(2) -0.2504(5) 0.0721(15) Uani 1 1 d . . . H25A H 0.2967 0.4172 -0.2767 0.086 Uiso 1 1 calc R . . C26 C 0.4608(6) 0.3688(2) -0.1588(5) 0.0691(16) Uani 1 1 d . . . H26A H 0.5121 0.4053 -0.1225 0.083 Uiso 1 1 calc R . . C27 C 0.6522(6) 0.2964(4) -0.0237(5) 0.090(2) Uani 1 1 d . . . H27A H 0.7054 0.3322 0.0141 0.108 Uiso 1 1 calc R . . C28 C 0.7046(7) 0.2361(5) 0.0127(5) 0.106(3) Uani 1 1 d . . . H28A H 0.7930 0.2314 0.0739 0.127 Uiso 1 1 calc R . . C29 C 0.6259(7) 0.1811(4) -0.0417(5) 0.0911(19) Uani 1 1 d . . . H29A H 0.6625 0.1401 -0.0163 0.109 Uiso 1 1 calc R . . C30 C 0.4955(5) 0.1873(3) -0.1321(4) 0.0612(13) Uani 1 1 d . . . H30A H 0.4441 0.1505 -0.1673 0.073 Uiso 1 1 calc R . . C31 C 0.4382(4) 0.2493(2) -0.1722(3) 0.0454(11) Uani 1 1 d . . . C32 C 0.5181(5) 0.3063(3) -0.1180(4) 0.0600(13) 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 Hg 0.04619(13) 0.05998(15) 0.05342(13) -0.00269(8) 0.02777(10) -0.01173(8) Cl1 0.0740(8) 0.0535(8) 0.1054(10) -0.0091(7) 0.0641(9) -0.0192(6) Cl2 0.0589(8) 0.1175(14) 0.0611(8) -0.0248(8) 0.0248(7) -0.0330(8) O1 0.0521(17) 0.0384(17) 0.0368(16) -0.0014(12) 0.0254(14) -0.0060(12) O2 0.087(3) 0.089(3) 0.094(3) -0.059(2) 0.076(2) -0.051(2) N1 0.044(2) 0.051(2) 0.046(2) -0.0034(17) 0.0235(19) -0.0114(16) N2 0.053(2) 0.039(2) 0.045(2) 0.0108(16) 0.0244(19) -0.0055(16) N3 0.051(2) 0.054(3) 0.042(2) 0.0094(18) 0.0197(19) -0.0094(18) N4 0.048(2) 0.047(2) 0.054(2) -0.0054(17) 0.0313(19) -0.0104(17) N5 0.052(2) 0.052(2) 0.057(2) -0.0238(17) 0.040(2) -0.0171(16) N6 0.054(2) 0.067(3) 0.061(2) -0.033(2) 0.041(2) -0.0270(19) C1 0.046(2) 0.037(2) 0.046(2) -0.0042(19) 0.027(2) -0.0095(18) C2 0.048(2) 0.036(2) 0.047(2) 0.0005(18) 0.030(2) -0.0064(18) C3 0.079(4) 0.035(3) 0.072(3) 0.008(2) 0.043(3) -0.004(2) C4 0.086(4) 0.038(3) 0.080(4) -0.007(3) 0.039(3) -0.023(3) C5 0.072(3) 0.052(3) 0.065(3) -0.012(3) 0.038(3) -0.029(3) C6 0.045(2) 0.035(2) 0.046(2) 0.0010(19) 0.028(2) 0.0038(18) C7 0.038(2) 0.043(3) 0.039(2) 0.0110(18) 0.018(2) 0.0054(17) C8 0.047(3) 0.057(3) 0.042(2) 0.003(2) 0.023(2) 0.008(2) C9 0.049(3) 0.072(4) 0.066(3) 0.014(3) 0.039(3) 0.004(2) C10 0.055(3) 0.053(3) 0.068(3) 0.003(3) 0.032(3) -0.012(2) C11 0.097(4) 0.051(4) 0.078(4) -0.014(3) 0.043(4) -0.011(3) C12 0.133(6) 0.076(5) 0.077(4) -0.025(3) 0.061(5) -0.005(4) C13 0.112(5) 0.094(5) 0.084(4) -0.006(4) 0.073(4) 0.012(4) C14 0.063(3) 0.074(4) 0.063(3) 0.003(3) 0.042(3) -0.001(3) C15 0.046(2) 0.043(3) 0.043(2) 0.0098(19) 0.024(2) 0.0078(19) C16 0.053(3) 0.045(3) 0.052(3) 0.003(2) 0.026(2) -0.001(2) C17 0.044(2) 0.047(3) 0.043(2) -0.0096(19) 0.025(2) -0.0099(18) C18 0.034(2) 0.031(2) 0.043(2) 0.0000(17) 0.0195(19) -0.0006(16) C19 0.050(3) 0.035(2) 0.053(3) -0.0068(19) 0.031(2) 0.0026(18) C20 0.057(3) 0.034(3) 0.059(3) -0.011(2) 0.026(3) -0.010(2) C21 0.049(3) 0.046(3) 0.067(3) -0.001(2) 0.033(3) -0.012(2) C22 0.041(2) 0.056(3) 0.048(3) -0.019(2) 0.028(2) -0.012(2) C23 0.048(2) 0.049(3) 0.050(3) -0.018(2) 0.034(2) -0.015(2) C24 0.059(3) 0.066(4) 0.063(3) -0.008(3) 0.035(3) -0.002(3) C25 0.088(4) 0.044(3) 0.093(4) -0.009(3) 0.057(4) -0.004(3) C26 0.084(4) 0.042(3) 0.098(4) -0.031(3) 0.062(4) -0.029(3) C27 0.057(4) 0.112(6) 0.089(5) -0.039(4) 0.035(4) -0.023(3) C28 0.064(4) 0.158(8) 0.065(4) -0.017(5) 0.020(4) 0.008(5) C29 0.090(5) 0.101(6) 0.079(4) 0.019(4) 0.047(4) 0.027(4) C30 0.074(3) 0.058(3) 0.068(3) -0.007(2) 0.050(3) 0.002(3) C31 0.049(3) 0.048(3) 0.051(3) -0.015(2) 0.036(2) -0.011(2) C32 0.049(3) 0.073(4) 0.068(3) -0.027(3) 0.039(3) -0.022(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 Hg Cl2 2.3708(14) . ? Hg Cl1 2.3881(13) . ? Hg N1 2.448(4) . ? Hg N4 2.487(4) . ? O1 C6 1.237(5) . ? O2 C22 1.238(5) . ? N1 C1 1.342(5) . ? N1 C5 1.349(6) . ? N2 C6 1.386(5) . ? N2 C2 1.414(5) . ? N2 H2B 0.8734 . ? N3 C6 1.366(5) . ? N3 C7 1.443(6) . ? N3 H3B 0.8736 . ? N4 C21 1.338(6) . ? N4 C17 1.349(5) . ? N5 C22 1.384(5) . ? N5 C18 1.415(5) . ? N5 H5B 0.8697 . ? N6 C22 1.348(5) . ? N6 C23 1.460(5) . ? N6 H6B 0.8719 . ? C1 C2 1.405(6) . ? C1 H1A 0.9300 . ? C2 C3 1.388(6) . ? C3 C4 1.387(7) . ? C3 H3A 0.9300 . ? C4 C5 1.377(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.376(6) . ? C7 C15 1.440(6) . ? C8 C9 1.422(7) . ? C8 H8A 0.9300 . ? C9 C10 1.368(7) . ? C9 H9A 0.9300 . ? C10 C16 1.412(7) . ? C10 H10A 0.9300 . ? C11 C12 1.357(9) . ? C11 C16 1.418(7) . ? C11 H11A 0.9300 . ? C12 C13 1.393(9) . ? C12 H12A 0.9300 . ? C13 C14 1.383(7) . ? C13 H13A 0.9300 . ? C14 C15 1.418(6) . ? C14 H14A 0.9300 . ? C15 C16 1.439(6) . ? C17 C18 1.404(6) . ? C17 H17A 0.9300 . ? C18 C19 1.403(6) . ? C19 C20 1.396(6) . ? C19 H19A 0.9300 . ? C20 C21 1.381(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C23 C24 1.381(7) . ? C23 C31 1.416(6) . ? C24 C25 1.398(8) . ? C24 H24A 0.9300 . ? C25 C26 1.373(9) . ? C25 H25A 0.9300 . ? C26 C32 1.427(7) . ? C26 H26A 0.9300 . ? C27 C28 1.361(10) . ? C27 C32 1.427(8) . ? C27 H27A 0.9300 . ? C28 C29 1.404(10) . ? C28 H28A 0.9300 . ? C29 C30 1.370(7) . ? C29 H29A 0.9300 . ? C30 C31 1.416(7) . ? C30 H30A 0.9300 . ? C31 C32 1.440(6) . ? 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 Cl2 Hg Cl1 156.18(6) . . ? Cl2 Hg N1 101.42(10) . . ? Cl1 Hg N1 96.25(9) . . ? Cl2 Hg N4 99.29(9) . . ? Cl1 Hg N4 94.21(9) . . ? N1 Hg N4 97.07(12) . . ? C1 N1 C5 119.7(4) . . ? C1 N1 Hg 119.4(3) . . ? C5 N1 Hg 120.9(3) . . ? C6 N2 C2 125.4(3) . . ? C6 N2 H2B 118.3 . . ? C2 N2 H2B 116.2 . . ? C6 N3 C7 124.6(4) . . ? C6 N3 H3B 117.3 . . ? C7 N3 H3B 118.1 . . ? C21 N4 C17 120.4(4) . . ? C21 N4 Hg 124.0(3) . . ? C17 N4 Hg 115.5(3) . . ? C22 N5 C18 126.3(4) . . ? C22 N5 H5B 117.1 . . ? C18 N5 H5B 116.5 . . ? C22 N6 C23 120.1(3) . . ? C22 N6 H6B 119.9 . . ? C23 N6 H6B 120.0 . . ? N1 C1 C2 121.8(4) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 N2 120.2(4) . . ? C1 C2 N2 121.9(4) . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 121.5(5) . . ? N1 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? O1 C6 N3 124.9(4) . . ? O1 C6 N2 123.1(4) . . ? N3 C6 N2 112.0(4) . . ? C8 C7 C15 120.5(4) . . ? C8 C7 N3 121.2(4) . . ? C15 C7 N3 118.3(4) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C16 121.0(4) . . ? C9 C10 H10A 119.5 . . ? C16 C10 H10A 119.5 . . ? C12 C11 C16 122.3(6) . . ? C12 C11 H11A 118.9 . . ? C16 C11 H11A 118.9 . . ? C11 C12 C13 119.2(6) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 121.4(6) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C16 117.8(4) . . ? C14 C15 C7 123.8(4) . . ? C16 C15 C7 118.4(4) . . ? C10 C16 C11 122.3(5) . . ? C10 C16 C15 119.2(4) . . ? C11 C16 C15 118.6(5) . . ? N4 C17 C18 121.1(4) . . ? N4 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 118.3(4) . . ? C19 C18 N5 118.3(4) . . ? C17 C18 N5 123.4(4) . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C21 C20 C19 119.1(4) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? N4 C21 C20 121.9(4) . . ? N4 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? O2 C22 N6 122.6(4) . . ? O2 C22 N5 123.3(4) . . ? N6 C22 N5 114.1(4) . . ? C24 C23 C31 122.2(4) . . ? C24 C23 N6 119.4(4) . . ? C31 C23 N6 118.5(4) . . ? C23 C24 C25 121.3(5) . . ? C23 C24 H24A 119.3 . . ? C25 C24 H24A 119.3 . . ? C26 C25 C24 118.8(5) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C25 C26 C32 121.5(4) . . ? C25 C26 H26A 119.2 . . ? C32 C26 H26A 119.2 . . ? C28 C27 C32 122.0(6) . . ? C28 C27 H27A 119.0 . . ? C32 C27 H27A 119.0 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.6(5) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C30 C31 C23 123.9(4) . . ? C30 C31 C32 119.7(5) . . ? C23 C31 C32 116.4(4) . . ? C27 C32 C26 123.4(5) . . ? C27 C32 C31 116.8(5) . . ? C26 C32 C31 119.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Hg N1 C1 173.4(3) . . . . ? Cl1 Hg N1 C1 -22.7(3) . . . . ? N4 Hg N1 C1 72.4(3) . . . . ? Cl2 Hg N1 C5 -7.1(4) . . . . ? Cl1 Hg N1 C5 156.9(3) . . . . ? N4 Hg N1 C5 -108.1(4) . . . . ? Cl2 Hg N4 C21 166.8(4) . . . . ? Cl1 Hg N4 C21 6.5(4) . . . . ? N1 Hg N4 C21 -90.3(4) . . . . ? Cl2 Hg N4 C17 -17.3(3) . . . . ? Cl1 Hg N4 C17 -177.6(3) . . . . ? N1 Hg N4 C17 85.6(3) . . . . ? C5 N1 C1 C2 -0.4(6) . . . . ? Hg N1 C1 C2 179.1(3) . . . . ? N1 C1 C2 C3 0.8(6) . . . . ? N1 C1 C2 N2 177.4(4) . . . . ? C6 N2 C2 C3 -141.5(5) . . . . ? C6 N2 C2 C1 42.0(6) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? N2 C2 C3 C4 -177.1(5) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? C1 N1 C5 C4 -0.3(7) . . . . ? Hg N1 C5 C4 -179.8(4) . . . . ? C3 C4 C5 N1 0.6(8) . . . . ? C7 N3 C6 O1 0.8(7) . . . . ? C7 N3 C6 N2 179.2(4) . . . . ? C2 N2 C6 O1 3.0(7) . . . . ? C2 N2 C6 N3 -175.5(4) . . . . ? C6 N3 C7 C8 47.9(6) . . . . ? C6 N3 C7 C15 -132.4(4) . . . . ? C15 C7 C8 C9 -0.2(6) . . . . ? N3 C7 C8 C9 179.5(4) . . . . ? C7 C8 C9 C10 -1.4(7) . . . . ? C8 C9 C10 C16 1.2(8) . . . . ? C16 C11 C12 C13 0.4(10) . . . . ? C11 C12 C13 C14 -1.3(11) . . . . ? C12 C13 C14 C15 1.2(10) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C13 C14 C15 C7 -179.4(5) . . . . ? C8 C7 C15 C14 -178.7(4) . . . . ? N3 C7 C15 C14 1.6(6) . . . . ? C8 C7 C15 C16 2.0(6) . . . . ? N3 C7 C15 C16 -177.8(4) . . . . ? C9 C10 C16 C11 179.9(5) . . . . ? C9 C10 C16 C15 0.6(7) . . . . ? C12 C11 C16 C10 -178.6(6) . . . . ? C12 C11 C16 C15 0.7(9) . . . . ? C14 C15 C16 C10 178.5(4) . . . . ? C7 C15 C16 C10 -2.1(6) . . . . ? C14 C15 C16 C11 -0.8(7) . . . . ? C7 C15 C16 C11 178.6(4) . . . . ? C21 N4 C17 C18 2.1(7) . . . . ? Hg N4 C17 C18 -173.9(3) . . . . ? N4 C17 C18 C19 -4.2(6) . . . . ? N4 C17 C18 N5 176.0(4) . . . . ? C22 N5 C18 C19 173.0(4) . . . . ? C22 N5 C18 C17 -7.1(7) . . . . ? C17 C18 C19 C20 4.3(6) . . . . ? N5 C18 C19 C20 -175.9(4) . . . . ? C18 C19 C20 C21 -2.4(7) . . . . ? C17 N4 C21 C20 -0.1(7) . . . . ? Hg N4 C21 C20 175.6(3) . . . . ? C19 C20 C21 N4 0.3(7) . . . . ? C23 N6 C22 O2 4.6(8) . . . . ? C23 N6 C22 N5 -175.2(4) . . . . ? C18 N5 C22 O2 2.8(8) . . . . ? C18 N5 C22 N6 -177.4(4) . . . . ? C22 N6 C23 C24 -87.6(6) . . . . ? C22 N6 C23 C31 92.4(5) . . . . ? C31 C23 C24 C25 -0.8(7) . . . . ? N6 C23 C24 C25 179.2(5) . . . . ? C23 C24 C25 C26 -0.1(8) . . . . ? C24 C25 C26 C32 1.3(8) . . . . ? C32 C27 C28 C29 -1.1(11) . . . . ? C27 C28 C29 C30 0.0(10) . . . . ? C28 C29 C30 C31 0.2(9) . . . . ? C29 C30 C31 C23 179.3(5) . . . . ? C29 C30 C31 C32 0.5(7) . . . . ? C24 C23 C31 C30 -178.4(4) . . . . ? N6 C23 C31 C30 1.7(6) . . . . ? C24 C23 C31 C32 0.5(6) . . . . ? N6 C23 C31 C32 -179.5(4) . . . . ? C28 C27 C32 C26 -179.3(6) . . . . ? C28 C27 C32 C31 1.7(9) . . . . ? C25 C26 C32 C27 179.4(5) . . . . ? C25 C26 C32 C31 -1.6(8) . . . . ? C30 C31 C32 C27 -1.4(6) . . . . ? C23 C31 C32 C27 179.7(4) . . . . ? C30 C31 C32 C26 179.6(4) . . . . ? C23 C31 C32 C26 0.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.87 1.98 2.841(5) 166.5 4_465 N3 H3B O2 0.87 2.61 3.340(5) 141.7 4_465 N5 H5B O1 0.87 2.37 3.120(5) 144.8 1_655 N6 H6B O1 0.87 2.10 2.907(4) 153.2 1_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.166 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.089 ##################### data_HgBr2 _database_code_depnum_ccdc_archive 'CCDC 874350' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Br2 Hg N6 O2' _chemical_formula_weight 887.00 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' 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.860(3) _cell_length_b 20.465(5) _cell_length_c 15.636(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.868(12) _cell_angle_gamma 90.00 _cell_volume 3113.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 7.549 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2104 _exptl_absorpt_correction_T_max 0.2541 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23217 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6415 _reflns_number_gt 4816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+1.4536P] 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 6415 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Hg Hg 0.729817(15) 0.121813(8) 0.803465(13) 0.05387(7) Uani 1 1 d . . . Br1 Br 0.55935(5) 0.03423(2) 0.75882(5) 0.07467(15) Uani 1 1 d . . . Br2 Br 0.93669(5) 0.18654(3) 0.92949(4) 0.07617(16) Uani 1 1 d . . . O1 O 0.1670(2) 0.13405(12) 0.50481(19) 0.0425(6) Uani 1 1 d . . . O2 O 1.1046(3) 0.20564(16) 0.7599(2) 0.0726(10) Uani 1 1 d . . . N1 N 0.5705(3) 0.20457(15) 0.6877(2) 0.0486(8) Uani 1 1 d . . . N2 N 0.2302(3) 0.21623(15) 0.4417(2) 0.0476(8) Uani 1 1 d . . . H2B H 0.2044 0.2385 0.3867 0.057 Uiso 1 1 d R . . N3 N 0.0374(3) 0.15765(16) 0.3313(2) 0.0518(9) Uani 1 1 d . . . H3B H 0.0321 0.1821 0.2844 0.062 Uiso 1 1 d R . . N4 N 0.7990(3) 0.08052(16) 0.6923(2) 0.0476(8) Uani 1 1 d . . . N5 N 1.0580(3) 0.12496(15) 0.6438(2) 0.0476(8) Uani 1 1 d . . . H5B H 1.0809 0.1093 0.6047 0.057 Uiso 1 1 d R . . N6 N 1.2276(3) 0.19902(17) 0.6917(3) 0.0552(9) Uani 1 1 d . . . H6B H 1.2397 0.1791 0.6490 0.066 Uiso 1 1 d R . . C1 C 0.4493(4) 0.18861(18) 0.6029(3) 0.0436(9) Uani 1 1 d . . . H1A H 0.4265 0.1445 0.5897 0.052 Uiso 1 1 calc R . . C2 C 0.3547(4) 0.23392(18) 0.5330(3) 0.0419(9) Uani 1 1 d . . . C3 C 0.3911(5) 0.2989(2) 0.5538(4) 0.0634(12) Uani 1 1 d . . . H3A H 0.3310 0.3311 0.5085 0.076 Uiso 1 1 calc R . . C4 C 0.5158(5) 0.3159(2) 0.6411(4) 0.0744(14) Uani 1 1 d . . . H4A H 0.5409 0.3596 0.6559 0.089 Uiso 1 1 calc R . . C5 C 0.6039(5) 0.2677(2) 0.7071(4) 0.0652(13) Uani 1 1 d . . . H5A H 0.6887 0.2795 0.7666 0.078 Uiso 1 1 calc R . . C6 C 0.1454(3) 0.16698(17) 0.4312(3) 0.0377(8) Uani 1 1 d . . . C7 C -0.0688(4) 0.11033(18) 0.2977(3) 0.0436(9) Uani 1 1 d . . . C8 C -0.1368(4) 0.1061(2) 0.3434(3) 0.0516(10) Uani 1 1 d . . . H8A H -0.1145 0.1343 0.3977 0.062 Uiso 1 1 calc R . . C9 C -0.2417(4) 0.0591(2) 0.3090(3) 0.0613(12) Uani 1 1 d . . . H9A H -0.2874 0.0560 0.3413 0.074 Uiso 1 1 calc R . . C10 C -0.2756(4) 0.0187(2) 0.2293(4) 0.0639(12) Uani 1 1 d . . . H10A H -0.3450 -0.0119 0.2073 0.077 Uiso 1 1 calc R . . C11 C -0.2416(6) -0.0200(2) 0.0963(4) 0.0780(15) Uani 1 1 d . . . H11A H -0.3124 -0.0502 0.0720 0.094 Uiso 1 1 calc R . . C12 C -0.1733(6) -0.0174(3) 0.0520(4) 0.0912(17) Uani 1 1 d . . . H12A H -0.1959 -0.0459 -0.0020 0.109 Uiso 1 1 calc R . . C13 C -0.0687(6) 0.0279(3) 0.0864(5) 0.0906(17) Uani 1 1 d . . . H13A H -0.0224 0.0298 0.0545 0.109 Uiso 1 1 calc R . . C14 C -0.0325(5) 0.0696(2) 0.1660(4) 0.0654(12) Uani 1 1 d . . . H14A H 0.0385 0.0993 0.1883 0.078 Uiso 1 1 calc R . . C15 C -0.1016(4) 0.06804(19) 0.2146(3) 0.0457(9) Uani 1 1 d . . . C16 C -0.2088(4) 0.0219(2) 0.1793(3) 0.0524(10) Uani 1 1 d . . . C17 C 0.9051(4) 0.11047(18) 0.7011(3) 0.0440(9) Uani 1 1 d . . . H17A H 0.9494 0.1441 0.7493 0.053 Uiso 1 1 calc R . . C18 C 0.9514(3) 0.09276(17) 0.6404(3) 0.0391(8) Uani 1 1 d . . . C19 C 0.8880(4) 0.04054(18) 0.5731(3) 0.0462(9) Uani 1 1 d . . . H19A H 0.9189 0.0260 0.5335 0.055 Uiso 1 1 calc R . . C20 C 0.7790(4) 0.01028(19) 0.5652(3) 0.0534(11) Uani 1 1 d . . . H20A H 0.7346 -0.0245 0.5194 0.064 Uiso 1 1 calc R . . C21 C 0.7366(4) 0.03162(19) 0.6249(3) 0.0533(10) Uani 1 1 d . . . H21A H 0.6618 0.0114 0.6185 0.064 Uiso 1 1 calc R . . C22 C 1.1290(4) 0.1783(2) 0.7024(3) 0.0481(10) Uani 1 1 d . . . C23 C 1.3129(4) 0.2536(2) 0.7495(3) 0.0467(9) Uani 1 1 d . . . C24 C 1.2640(4) 0.3147(2) 0.7147(4) 0.0661(13) Uani 1 1 d . . . H24A H 1.1772 0.3203 0.6532 0.079 Uiso 1 1 calc R . . C25 C 1.3423(6) 0.3692(2) 0.7699(5) 0.0830(16) Uani 1 1 d . . . H25A H 1.3075 0.4109 0.7457 0.100 Uiso 1 1 calc R . . C26 C 1.4682(5) 0.3615(2) 0.8580(5) 0.0784(16) Uani 1 1 d . . . H26A H 1.5199 0.3982 0.8944 0.094 Uiso 1 1 calc R . . C27 C 1.6536(6) 0.2886(4) 0.9873(5) 0.100(2) Uani 1 1 d . . . H27A H 1.7064 0.3248 1.0247 0.120 Uiso 1 1 calc R . . C28 C 1.7048(6) 0.2290(5) 1.0222(5) 0.115(3) Uani 1 1 d . . . H28A H 1.7929 0.2243 1.0826 0.138 Uiso 1 1 calc R . . C29 C 1.6275(6) 0.1734(3) 0.9689(4) 0.0925(18) Uani 1 1 d . . . H29A H 1.6636 0.1320 0.9943 0.111 Uiso 1 1 calc R . . C30 C 1.4990(5) 0.1801(2) 0.8796(4) 0.0668(12) Uani 1 1 d . . . H30A H 1.4479 0.1431 0.8439 0.080 Uiso 1 1 calc R . . C31 C 1.4432(4) 0.2424(2) 0.8411(3) 0.0482(10) Uani 1 1 d . . . C32 C 1.5239(4) 0.2982(3) 0.8968(4) 0.0631(13) 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 Hg 0.04675(9) 0.05906(12) 0.05515(11) -0.00431(8) 0.02874(8) -0.01169(7) Br1 0.0797(3) 0.0563(3) 0.1139(4) -0.0144(3) 0.0705(3) -0.0218(2) Br2 0.0572(3) 0.1006(4) 0.0583(3) -0.0191(3) 0.0257(2) -0.0278(2) O1 0.0529(14) 0.0426(15) 0.0353(14) 0.0010(12) 0.0271(12) -0.0033(11) O2 0.083(2) 0.087(2) 0.085(2) -0.0519(19) 0.0700(19) -0.0443(17) N1 0.0473(18) 0.048(2) 0.048(2) -0.0037(16) 0.0263(16) -0.0099(15) N2 0.0527(19) 0.0431(19) 0.0418(19) 0.0107(15) 0.0240(16) -0.0029(15) N3 0.0545(19) 0.053(2) 0.0372(18) 0.0103(15) 0.0199(16) -0.0097(16) N4 0.0465(18) 0.048(2) 0.050(2) -0.0046(16) 0.0288(16) -0.0088(15) N5 0.0496(17) 0.055(2) 0.0494(19) -0.0210(16) 0.0349(16) -0.0111(15) N6 0.0528(18) 0.070(2) 0.060(2) -0.0309(18) 0.0418(18) -0.0234(17) C1 0.048(2) 0.037(2) 0.051(2) -0.0046(18) 0.031(2) -0.0081(17) C2 0.048(2) 0.042(2) 0.042(2) 0.0013(17) 0.0295(19) -0.0049(17) C3 0.073(3) 0.040(3) 0.072(3) 0.007(2) 0.039(3) -0.005(2) C4 0.087(3) 0.041(3) 0.080(3) -0.004(2) 0.039(3) -0.021(2) C5 0.063(3) 0.062(3) 0.065(3) -0.011(2) 0.033(2) -0.025(2) C6 0.0410(19) 0.035(2) 0.038(2) -0.0002(17) 0.0230(17) 0.0039(15) C7 0.044(2) 0.042(2) 0.036(2) 0.0117(17) 0.0179(17) 0.0065(16) C8 0.046(2) 0.062(3) 0.041(2) 0.0056(19) 0.0214(19) 0.0067(18) C9 0.049(2) 0.082(3) 0.059(3) 0.010(3) 0.035(2) 0.001(2) C10 0.052(2) 0.066(3) 0.063(3) 0.006(2) 0.027(2) -0.011(2) C11 0.091(4) 0.063(3) 0.067(3) -0.013(3) 0.037(3) -0.014(3) C12 0.125(5) 0.077(4) 0.075(4) -0.020(3) 0.059(4) -0.005(3) C13 0.113(4) 0.094(4) 0.093(4) -0.013(3) 0.076(4) -0.003(4) C14 0.071(3) 0.070(3) 0.061(3) -0.002(2) 0.042(3) -0.003(2) C15 0.045(2) 0.047(2) 0.041(2) 0.0105(18) 0.0220(18) 0.0068(17) C16 0.051(2) 0.045(2) 0.049(2) 0.0068(19) 0.022(2) 0.0018(18) C17 0.043(2) 0.045(2) 0.042(2) -0.0088(17) 0.0234(18) -0.0083(16) C18 0.0375(18) 0.037(2) 0.040(2) -0.0038(17) 0.0206(17) -0.0008(15) C19 0.051(2) 0.040(2) 0.045(2) -0.0072(18) 0.0262(19) 0.0033(17) C20 0.056(2) 0.038(2) 0.055(3) -0.0115(19) 0.025(2) -0.0112(18) C21 0.051(2) 0.046(2) 0.059(3) -0.004(2) 0.029(2) -0.0129(18) C22 0.047(2) 0.058(3) 0.047(2) -0.019(2) 0.031(2) -0.0134(18) C23 0.053(2) 0.051(3) 0.049(2) -0.0131(19) 0.037(2) -0.0108(19) C24 0.065(3) 0.068(3) 0.069(3) -0.007(3) 0.040(3) -0.005(2) C25 0.094(4) 0.050(3) 0.118(5) -0.007(3) 0.068(4) -0.003(3) C26 0.080(3) 0.062(3) 0.113(5) -0.040(3) 0.067(4) -0.033(3) C27 0.063(3) 0.140(6) 0.079(4) -0.049(4) 0.030(3) -0.018(3) C28 0.063(4) 0.190(8) 0.065(4) -0.026(5) 0.021(3) 0.009(5) C29 0.090(4) 0.115(5) 0.071(4) 0.018(4) 0.045(3) 0.034(4) C30 0.077(3) 0.073(3) 0.065(3) -0.009(2) 0.049(3) 0.003(2) C31 0.049(2) 0.059(3) 0.047(2) -0.014(2) 0.033(2) -0.0101(19) C32 0.048(2) 0.086(4) 0.061(3) -0.032(3) 0.035(2) -0.019(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 Hg N1 2.409(3) . ? Hg N4 2.458(3) . ? Hg Br2 2.4758(7) . ? Hg Br1 2.4847(6) . ? O1 C6 1.227(4) . ? O2 C22 1.225(4) . ? N1 C1 1.323(4) . ? N1 C5 1.335(5) . ? N2 C6 1.366(4) . ? N2 C2 1.392(4) . ? N2 H2B 0.8600 . ? N3 C6 1.353(4) . ? N3 C7 1.430(5) . ? N3 H3B 0.8601 . ? N4 C21 1.329(5) . ? N4 C17 1.334(4) . ? N5 C22 1.363(5) . ? N5 C18 1.400(5) . ? N5 H5B 0.8600 . ? N6 C22 1.342(5) . ? N6 C23 1.430(5) . ? N6 H6B 0.8600 . ? C1 C2 1.383(5) . ? C1 H1A 0.9300 . ? C2 C3 1.379(5) . ? C3 C4 1.365(6) . ? C3 H3A 0.9300 . ? C4 C5 1.377(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.352(6) . ? C7 C15 1.418(5) . ? C8 C9 1.413(6) . ? C8 H8A 0.9300 . ? C9 C10 1.351(6) . ? C9 H9A 0.9300 . ? C10 C16 1.396(6) . ? C10 H10A 0.9300 . ? C11 C12 1.335(7) . ? C11 C16 1.413(6) . ? C11 H11A 0.9300 . ? C12 C13 1.388(8) . ? C12 H12A 0.9300 . ? C13 C14 1.360(7) . ? C13 H13A 0.9300 . ? C14 C15 1.400(6) . ? C14 H14A 0.9300 . ? C15 C16 1.418(5) . ? C17 C18 1.389(5) . ? C17 H17A 0.9300 . ? C18 C19 1.382(5) . ? C19 C20 1.374(5) . ? C19 H19A 0.9300 . ? C20 C21 1.362(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C23 C24 1.355(6) . ? C23 C31 1.401(5) . ? C24 C25 1.390(7) . ? C24 H24A 0.9300 . ? C25 C26 1.341(7) . ? C25 H25A 0.9300 . ? C26 C32 1.425(7) . ? C26 H26A 0.9300 . ? C27 C28 1.333(9) . ? C27 C32 1.384(7) . ? C27 H27A 0.9300 . ? C28 C29 1.398(9) . ? C28 H28A 0.9300 . ? C29 C30 1.363(6) . ? C29 H29A 0.9300 . ? C30 C31 1.405(6) . ? C30 H30A 0.9300 . ? C31 C32 1.422(6) . ? 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 Hg N4 98.37(11) . . ? N1 Hg Br2 102.51(8) . . ? N4 Hg Br2 99.63(7) . . ? N1 Hg Br1 97.67(7) . . ? N4 Hg Br1 95.76(7) . . ? Br2 Hg Br1 152.44(2) . . ? C1 N1 C5 118.6(3) . . ? C1 N1 Hg 121.0(2) . . ? C5 N1 Hg 120.4(3) . . ? C6 N2 C2 126.2(3) . . ? C6 N2 H2B 117.1 . . ? C2 N2 H2B 116.7 . . ? C6 N3 C7 125.0(3) . . ? C6 N3 H3B 117.5 . . ? C7 N3 H3B 117.5 . . ? C21 N4 C17 119.6(4) . . ? C21 N4 Hg 124.0(3) . . ? C17 N4 Hg 116.4(2) . . ? C22 N5 C18 126.8(3) . . ? C22 N5 H5B 116.9 . . ? C18 N5 H5B 116.3 . . ? C22 N6 C23 121.3(3) . . ? C22 N6 H6B 119.4 . . ? C23 N6 H6B 119.3 . . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 117.2(4) . . ? C3 C2 N2 119.9(3) . . ? C1 C2 N2 122.8(3) . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? N1 C5 C4 121.5(4) . . ? N1 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? O1 C6 N3 123.9(3) . . ? O1 C6 N2 123.2(3) . . ? N3 C6 N2 112.9(3) . . ? C8 C7 C15 120.8(4) . . ? C8 C7 N3 121.0(4) . . ? C15 C7 N3 118.2(4) . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C16 121.5(4) . . ? C9 C10 H10A 119.2 . . ? C16 C10 H10A 119.2 . . ? C12 C11 C16 121.5(5) . . ? C12 C11 H11A 119.2 . . ? C16 C11 H11A 119.2 . . ? C11 C12 C13 120.0(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C7 123.0(4) . . ? C14 C15 C16 118.5(4) . . ? C7 C15 C16 118.5(4) . . ? C10 C16 C11 122.7(4) . . ? C10 C16 C15 118.9(4) . . ? C11 C16 C15 118.4(4) . . ? N4 C17 C18 121.8(3) . . ? N4 C17 H17A 119.1 . . ? C18 C17 H17A 119.1 . . ? C19 C18 C17 117.8(3) . . ? C19 C18 N5 118.7(3) . . ? C17 C18 N5 123.5(3) . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? N4 C21 C20 121.8(4) . . ? N4 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? O2 C22 N6 122.4(3) . . ? O2 C22 N5 123.0(3) . . ? N6 C22 N5 114.6(3) . . ? C24 C23 C31 122.1(4) . . ? C24 C23 N6 118.8(4) . . ? C31 C23 N6 119.1(4) . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 120.1(5) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C32 121.1(4) . . ? C25 C26 H26A 119.5 . . ? C32 C26 H26A 119.5 . . ? C28 C27 C32 121.8(6) . . ? C28 C27 H27A 119.1 . . ? C32 C27 H27A 119.1 . . ? C27 C28 C29 120.7(6) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C30 C29 C28 119.8(6) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 120.4(5) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C23 C31 C30 124.1(4) . . ? C23 C31 C32 117.2(4) . . ? C30 C31 C32 118.6(4) . . ? C27 C32 C31 118.6(5) . . ? C27 C32 C26 122.5(5) . . ? C31 C32 C26 118.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Hg N1 C1 72.3(3) . . . . ? Br2 Hg N1 C1 174.2(3) . . . . ? Br1 Hg N1 C1 -24.7(3) . . . . ? N4 Hg N1 C5 -106.7(3) . . . . ? Br2 Hg N1 C5 -4.8(3) . . . . ? Br1 Hg N1 C5 156.3(3) . . . . ? N1 Hg N4 C21 -90.7(3) . . . . ? Br2 Hg N4 C21 165.0(3) . . . . ? Br1 Hg N4 C21 7.9(3) . . . . ? N1 Hg N4 C17 88.6(3) . . . . ? Br2 Hg N4 C17 -15.7(3) . . . . ? Br1 Hg N4 C17 -172.8(3) . . . . ? C5 N1 C1 C2 0.0(6) . . . . ? Hg N1 C1 C2 -179.1(3) . . . . ? N1 C1 C2 C3 0.5(6) . . . . ? N1 C1 C2 N2 177.0(3) . . . . ? C6 N2 C2 C3 -142.6(4) . . . . ? C6 N2 C2 C1 41.0(6) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? N2 C2 C3 C4 -177.2(4) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C1 N1 C5 C4 -0.3(7) . . . . ? Hg N1 C5 C4 178.8(4) . . . . ? C3 C4 C5 N1 0.1(8) . . . . ? C7 N3 C6 O1 2.5(6) . . . . ? C7 N3 C6 N2 -178.9(3) . . . . ? C2 N2 C6 O1 4.0(6) . . . . ? C2 N2 C6 N3 -174.7(3) . . . . ? C6 N3 C7 C8 51.2(5) . . . . ? C6 N3 C7 C15 -129.2(4) . . . . ? C15 C7 C8 C9 0.2(6) . . . . ? N3 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C10 -0.9(6) . . . . ? C8 C9 C10 C16 0.2(7) . . . . ? C16 C11 C12 C13 -0.9(9) . . . . ? C11 C12 C13 C14 0.8(9) . . . . ? C12 C13 C14 C15 -0.6(8) . . . . ? C13 C14 C15 C7 -179.8(4) . . . . ? C13 C14 C15 C16 0.4(7) . . . . ? C8 C7 C15 C14 -178.7(4) . . . . ? N3 C7 C15 C14 1.6(5) . . . . ? C8 C7 C15 C16 1.0(5) . . . . ? N3 C7 C15 C16 -178.7(3) . . . . ? C9 C10 C16 C11 179.5(4) . . . . ? C9 C10 C16 C15 1.0(6) . . . . ? C12 C11 C16 C10 -177.9(5) . . . . ? C12 C11 C16 C15 0.7(7) . . . . ? C14 C15 C16 C10 178.1(4) . . . . ? C7 C15 C16 C10 -1.6(5) . . . . ? C14 C15 C16 C11 -0.4(6) . . . . ? C7 C15 C16 C11 179.8(4) . . . . ? C21 N4 C17 C18 1.2(6) . . . . ? Hg N4 C17 C18 -178.2(3) . . . . ? N4 C17 C18 C19 -3.1(5) . . . . ? N4 C17 C18 N5 176.9(3) . . . . ? C22 N5 C18 C19 177.8(4) . . . . ? C22 N5 C18 C17 -2.2(6) . . . . ? C17 C18 C19 C20 2.9(5) . . . . ? N5 C18 C19 C20 -177.0(3) . . . . ? C18 C19 C20 C21 -1.0(6) . . . . ? C17 N4 C21 C20 1.0(6) . . . . ? Hg N4 C21 C20 -179.8(3) . . . . ? C19 C20 C21 N4 -1.0(6) . . . . ? C23 N6 C22 O2 1.7(7) . . . . ? C23 N6 C22 N5 -178.7(4) . . . . ? C18 N5 C22 O2 -1.2(7) . . . . ? C18 N5 C22 N6 179.3(4) . . . . ? C22 N6 C23 C24 -81.4(5) . . . . ? C22 N6 C23 C31 97.6(5) . . . . ? C31 C23 C24 C25 -0.5(7) . . . . ? N6 C23 C24 C25 178.5(4) . . . . ? C23 C24 C25 C26 0.7(8) . . . . ? C24 C25 C26 C32 -0.1(8) . . . . ? C32 C27 C28 C29 -1.1(10) . . . . ? C27 C28 C29 C30 0.9(10) . . . . ? C28 C29 C30 C31 -0.5(8) . . . . ? C24 C23 C31 C30 -179.2(4) . . . . ? N6 C23 C31 C30 1.8(6) . . . . ? C24 C23 C31 C32 -0.2(6) . . . . ? N6 C23 C31 C32 -179.2(3) . . . . ? C29 C30 C31 C23 179.3(4) . . . . ? C29 C30 C31 C32 0.4(6) . . . . ? C28 C27 C32 C31 1.0(9) . . . . ? C28 C27 C32 C26 -179.4(6) . . . . ? C23 C31 C32 C27 -179.6(4) . . . . ? C30 C31 C32 C27 -0.6(6) . . . . ? C23 C31 C32 C26 0.8(6) . . . . ? C30 C31 C32 C26 179.8(4) . . . . ? C25 C26 C32 C27 179.7(5) . . . . ? C25 C26 C32 C31 -0.7(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6B O1 0.86 2.11 2.902(4) 152.6 1_655 N5 H5B O1 0.86 2.36 3.105(4) 145.4 1_655 N3 H3B O2 0.86 2.56 3.275(4) 141.6 4_465 N2 H2B O2 0.86 1.99 2.831(4) 166.0 4_465 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.022 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.078 ##################### data_HgI2 _database_code_depnum_ccdc_archive 'CCDC 874351' #TrackingRef '- LZnHgX2_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Hg I2 N3 O' _chemical_formula_weight 717.68 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6281(8) _cell_length_b 28.162(3) _cell_length_c 9.1674(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.6430(10) _cell_angle_gamma 90.00 _cell_volume 1804.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 11.960 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0867 _exptl_absorpt_correction_T_max 0.3809 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12895 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3529 _reflns_number_gt 3162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+5.2537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00270(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3529 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Hg Hg 1.13846(4) 0.120157(7) 1.29195(3) 0.04184(10) Uani 1 1 d . . . I1 I 1.18412(7) 0.031735(14) 1.38432(6) 0.05672(15) Uani 1 1 d . . . I2 I 1.21344(7) 0.209579(15) 1.36457(7) 0.06437(16) Uani 1 1 d . . . N1 N 0.9250(7) 0.12221(14) 1.0204(5) 0.0317(10) Uani 1 1 d . . . N2 N 0.7168(7) 0.21061(14) 0.7039(4) 0.0310(10) Uani 1 1 d . . . H2B H 0.7106 0.2107 0.6081 0.037 Uiso 1 1 calc R . . N3 N 0.6473(6) 0.28927(14) 0.6618(4) 0.0281(9) Uani 1 1 d . . . H3B H 0.6334 0.2827 0.5662 0.034 Uiso 1 1 calc R . . O O 0.7041(6) 0.25623(12) 0.9046(4) 0.0348(9) Uani 1 1 d . . . C1 C 0.8885(7) 0.16346(17) 0.9427(5) 0.0277(10) Uani 1 1 d . . . H1A H 0.9544 0.1905 0.9941 0.033 Uiso 1 1 calc R . . C2 C 0.7537(7) 0.16704(16) 0.7860(5) 0.0252(10) Uani 1 1 d . . . C3 C 0.6572(9) 0.12641(18) 0.7113(6) 0.0355(12) Uani 1 1 d . . . H3A H 0.5655 0.1280 0.6074 0.043 Uiso 1 1 calc R . . C4 C 0.6973(9) 0.08368(19) 0.7912(7) 0.0381(13) Uani 1 1 d . . . H4A H 0.6358 0.0559 0.7418 0.046 Uiso 1 1 calc R . . C5 C 0.8319(9) 0.08322(18) 0.9474(6) 0.0363(12) Uani 1 1 d . . . H5A H 0.8581 0.0547 1.0031 0.044 Uiso 1 1 calc R . . C6 C 0.6903(7) 0.25266(16) 0.7663(5) 0.0243(10) Uani 1 1 d . . . C7 C 0.6231(7) 0.33711(16) 0.6946(5) 0.0253(10) Uani 1 1 d . . . C8 C 0.7304(8) 0.35760(18) 0.8379(6) 0.0334(12) Uani 1 1 d . . . H8A H 0.8174 0.3394 0.9194 0.040 Uiso 1 1 calc R . . C9 C 0.7094(10) 0.4064(2) 0.8624(7) 0.0449(15) Uani 1 1 d . . . H9A H 0.7820 0.4200 0.9607 0.054 Uiso 1 1 calc R . . C10 C 0.5857(11) 0.4335(2) 0.7455(9) 0.0511(17) Uani 1 1 d . . . H10A H 0.5760 0.4657 0.7636 0.061 Uiso 1 1 calc R . . C11 C 0.3348(11) 0.4411(2) 0.4691(9) 0.0581(19) Uani 1 1 d . . . H11A H 0.3219 0.4733 0.4848 0.070 Uiso 1 1 calc R . . C12 C 0.2251(11) 0.4218(3) 0.3281(9) 0.0588(19) Uani 1 1 d . . . H12A H 0.1391 0.4406 0.2478 0.071 Uiso 1 1 calc R . . C13 C 0.2403(10) 0.3733(3) 0.3021(8) 0.0521(17) Uani 1 1 d . . . H13A H 0.1632 0.3598 0.2048 0.062 Uiso 1 1 calc R . . C14 C 0.3686(9) 0.3455(2) 0.4196(6) 0.0379(12) Uani 1 1 d . . . H14A H 0.3778 0.3134 0.4002 0.045 Uiso 1 1 calc R . . C15 C 0.4861(8) 0.36456(18) 0.5683(6) 0.0283(10) Uani 1 1 d . . . C16 C 0.4709(9) 0.41406(19) 0.5963(7) 0.0389(13) 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 Hg 0.04853(17) 0.03041(14) 0.03714(14) 0.00892(9) 0.00731(10) 0.00226(9) I1 0.0754(3) 0.0331(2) 0.0638(3) 0.01878(19) 0.0301(2) 0.01479(19) I2 0.0496(3) 0.0361(2) 0.0828(3) -0.0037(2) 0.0008(2) -0.01084(19) N1 0.042(3) 0.027(2) 0.024(2) 0.0045(17) 0.0112(19) 0.0041(18) N2 0.057(3) 0.019(2) 0.0159(18) 0.0035(16) 0.0138(19) 0.0066(19) N3 0.049(3) 0.024(2) 0.0126(17) 0.0004(15) 0.0141(18) 0.0040(18) O 0.066(3) 0.0270(18) 0.0159(15) 0.0034(14) 0.0208(16) 0.0069(17) C1 0.038(3) 0.020(2) 0.024(2) 0.0007(19) 0.011(2) 0.000(2) C2 0.036(3) 0.021(2) 0.021(2) 0.0041(18) 0.014(2) 0.0054(19) C3 0.046(3) 0.031(3) 0.026(2) -0.005(2) 0.010(2) 0.005(2) C4 0.049(4) 0.021(2) 0.043(3) -0.009(2) 0.018(3) -0.006(2) C5 0.052(4) 0.018(2) 0.039(3) 0.008(2) 0.018(3) 0.005(2) C6 0.036(3) 0.020(2) 0.016(2) 0.0028(18) 0.0097(19) 0.0039(19) C7 0.036(3) 0.022(2) 0.023(2) 0.0015(19) 0.017(2) 0.001(2) C8 0.045(3) 0.029(3) 0.029(2) -0.002(2) 0.017(2) -0.003(2) C9 0.065(4) 0.037(3) 0.040(3) -0.018(3) 0.028(3) -0.013(3) C10 0.078(5) 0.021(3) 0.072(4) -0.009(3) 0.049(4) 0.001(3) C11 0.068(5) 0.037(3) 0.081(5) 0.024(3) 0.042(4) 0.027(3) C12 0.055(4) 0.064(5) 0.059(4) 0.030(4) 0.025(4) 0.023(4) C13 0.040(4) 0.069(5) 0.040(3) 0.021(3) 0.009(3) 0.008(3) C14 0.046(3) 0.033(3) 0.035(3) 0.008(2) 0.016(2) 0.003(2) C15 0.033(3) 0.025(2) 0.032(2) 0.006(2) 0.020(2) 0.001(2) C16 0.046(4) 0.027(3) 0.054(3) 0.005(3) 0.031(3) 0.009(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 Hg N1 2.366(4) . ? Hg I1 2.6082(5) . ? Hg I2 2.6090(5) . ? N1 C1 1.333(6) . ? N1 C5 1.333(7) . ? N2 C6 1.365(6) . ? N2 C2 1.408(6) . ? N2 H2B 0.8600 . ? N3 C6 1.355(6) . ? N3 C7 1.408(6) . ? N3 H3B 0.8600 . ? O C6 1.233(5) . ? C1 C2 1.395(7) . ? C1 H1A 0.9300 . ? C2 C3 1.384(7) . ? C3 C4 1.378(7) . ? C3 H3A 0.9300 . ? C4 C5 1.387(8) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.366(7) . ? C7 C15 1.435(7) . ? C8 C9 1.413(8) . ? C8 H8A 0.9300 . ? C9 C10 1.346(10) . ? C9 H9A 0.9300 . ? C10 C16 1.406(9) . ? C10 H10A 0.9300 . ? C11 C12 1.341(11) . ? C11 C16 1.430(9) . ? C11 H11A 0.9300 . ? C12 C13 1.398(10) . ? C12 H12A 0.9300 . ? C13 C14 1.373(8) . ? C13 H13A 0.9300 . ? C14 C15 1.403(8) . ? C14 H14A 0.9300 . ? C15 C16 1.431(7) . ? 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 Hg I1 108.11(10) . . ? N1 Hg I2 103.46(10) . . ? I1 Hg I2 148.391(19) . . ? C1 N1 C5 119.6(4) . . ? C1 N1 Hg 119.5(3) . . ? C5 N1 Hg 120.8(3) . . ? C6 N2 C2 124.3(4) . . ? C6 N2 H2B 117.9 . . ? C2 N2 H2B 117.9 . . ? C6 N3 C7 126.3(4) . . ? C6 N3 H3B 116.8 . . ? C7 N3 H3B 116.8 . . ? N1 C1 C2 121.5(5) . . ? N1 C1 H1A 119.2 . . ? C2 C1 H1A 119.2 . . ? C3 C2 C1 118.4(4) . . ? C3 C2 N2 120.2(4) . . ? C1 C2 N2 121.3(4) . . ? C4 C3 C2 119.9(5) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 118.1(5) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? N1 C5 C4 122.4(5) . . ? N1 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? O C6 N3 124.1(4) . . ? O C6 N2 122.4(4) . . ? N3 C6 N2 113.5(4) . . ? C8 C7 N3 122.0(5) . . ? C8 C7 C15 120.6(5) . . ? N3 C7 C15 117.3(4) . . ? C7 C8 C9 120.1(5) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C10 C9 C8 120.8(5) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C16 121.2(5) . . ? C9 C10 H10A 119.4 . . ? C16 C10 H10A 119.4 . . ? C12 C11 C16 122.6(6) . . ? C12 C11 H11A 118.7 . . ? C16 C11 H11A 118.7 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 120.3(7) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 121.4(6) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C14 C15 C16 118.7(5) . . ? C14 C15 C7 123.5(5) . . ? C16 C15 C7 117.7(5) . . ? C10 C16 C11 123.5(6) . . ? C10 C16 C15 119.4(5) . . ? C11 C16 C15 117.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Hg N1 C1 -175.6(4) . . . . ? I2 Hg N1 C1 6.0(4) . . . . ? I1 Hg N1 C5 8.7(4) . . . . ? I2 Hg N1 C5 -169.7(4) . . . . ? C5 N1 C1 C2 0.4(8) . . . . ? Hg N1 C1 C2 -175.4(4) . . . . ? N1 C1 C2 C3 -0.1(8) . . . . ? N1 C1 C2 N2 -179.4(5) . . . . ? C6 N2 C2 C3 134.7(5) . . . . ? C6 N2 C2 C1 -46.0(8) . . . . ? C1 C2 C3 C4 -0.8(8) . . . . ? N2 C2 C3 C4 178.5(5) . . . . ? C2 C3 C4 C5 1.5(9) . . . . ? C1 N1 C5 C4 0.4(9) . . . . ? Hg N1 C5 C4 176.1(4) . . . . ? C3 C4 C5 N1 -1.3(9) . . . . ? C7 N3 C6 O 4.1(9) . . . . ? C7 N3 C6 N2 -176.1(5) . . . . ? C2 N2 C6 O 2.9(8) . . . . ? C2 N2 C6 N3 -176.8(5) . . . . ? C6 N3 C7 C8 35.8(8) . . . . ? C6 N3 C7 C15 -146.9(5) . . . . ? N3 C7 C8 C9 176.2(5) . . . . ? C15 C7 C8 C9 -0.9(8) . . . . ? C7 C8 C9 C10 -0.7(9) . . . . ? C8 C9 C10 C16 1.2(10) . . . . ? C16 C11 C12 C13 0.7(11) . . . . ? C11 C12 C13 C14 -0.7(11) . . . . ? C12 C13 C14 C15 0.5(10) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C13 C14 C15 C7 -179.6(5) . . . . ? C8 C7 C15 C14 -178.6(5) . . . . ? N3 C7 C15 C14 4.1(7) . . . . ? C8 C7 C15 C16 1.9(7) . . . . ? N3 C7 C15 C16 -175.3(4) . . . . ? C9 C10 C16 C11 178.8(6) . . . . ? C9 C10 C16 C15 -0.1(9) . . . . ? C12 C11 C16 C10 -179.3(7) . . . . ? C12 C11 C16 C15 -0.3(10) . . . . ? C14 C15 C16 C10 179.1(5) . . . . ? C7 C15 C16 C10 -1.4(7) . . . . ? C14 C15 C16 C11 0.1(8) . . . . ? C7 C15 C16 C11 179.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O 0.86 2.07 2.863(5) 153.5 4_565 N3 H3B O 0.86 2.08 2.866(5) 151.5 4_565 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.346 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.129 ###############END