Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; New d10 Metal-Organic Coordination Polymers with 9,10-Bis(triazol-1- ylmethyl)anthracene (L): Synthesis, Crystal Structures, and Luminescent Properties ; loop_ _publ_author_name 'Xian-He Bu.' 'Jian-Rong Li.' 'Lei Li.' 'Chun-Sen Liu.' 'Duo-Zhi Wang.' ; Fei-Zhang Yong ; # Attachment 'complexes_1-6.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 630074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Cu I N6' _chemical_formula_weight 530.84 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' Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.877(10) _cell_length_b 8.045(3) _cell_length_c 10.222(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1881.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1520 _cell_measurement_theta_min 3.3428 _cell_measurement_theta_max 23.1755 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.821 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 4561 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1652 _reflns_number_gt 1295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+68.2606P] 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 1652 _refine_ls_number_parameters 128 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2246 _refine_ls_wR_factor_gt 0.2102 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.053 _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 I1 I 0.0000 -0.01692(14) 0.7500 0.0486(5) Uani 1 2 d S . . Cu1 Cu 0.0000 0.2968(2) 0.7500 0.0361(6) Uani 1 2 d S . . N1 N 0.0479(6) 0.4060(13) 0.6210(11) 0.062(3) Uani 1 1 d D . . N2 N 0.0954(5) 0.5959(15) 0.5146(11) 0.067(4) Uani 1 1 d D . . N3 N 0.1009(6) 0.4558(16) 0.4410(14) 0.071(4) Uani 1 1 d D . . C1 C 0.0630(7) 0.5677(15) 0.6197(13) 0.068(4) Uani 1 1 d D . . H1A H 0.0525 0.6463 0.6821 0.081 Uiso 1 1 calc R . . C2 C 0.0721(8) 0.345(2) 0.5107(12) 0.075(5) Uani 1 1 d D . . H2A H 0.0687 0.2341 0.4859 0.090 Uiso 1 1 calc R . . C3 C 0.1228(7) 0.754(2) 0.4709(17) 0.065(4) Uani 1 1 d . . . H3A H 0.1068 0.8455 0.5213 0.077 Uiso 1 1 calc R . . H3B H 0.1134 0.7731 0.3796 0.077 Uiso 1 1 calc R . . C4 C 0.1884(7) 0.751(2) 0.4873(15) 0.062(4) Uani 1 1 d . . . C6 C 0.1995(6) 0.6697(16) 0.2518(13) 0.047(3) Uani 1 1 d . . . H6A H 0.1590 0.6660 0.2444 0.056 Uiso 1 1 calc R . . C7 C 0.2328(8) 0.647(3) 0.1436(16) 0.086(7) Uani 1 1 d . . . H7A H 0.2157 0.6304 0.0621 0.103 Uiso 1 1 calc R . . C8 C 0.2937(10) 0.648(3) 0.158(2) 0.104(8) Uani 1 1 d . . . H8A H 0.3170 0.6336 0.0840 0.125 Uiso 1 1 calc R . . C9 C 0.3187(7) 0.6689(19) 0.272(2) 0.071(5) Uani 1 1 d . . . H9A H 0.3592 0.6616 0.2776 0.085 Uiso 1 1 calc R . . C5 C 0.2245(7) 0.699(2) 0.3726(15) 0.067(5) Uani 1 1 d . . . C10 C 0.2131(6) 0.798(2) 0.6112(16) 0.060(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0511(8) 0.0256(6) 0.0690(9) 0.000 -0.0010(6) 0.000 Cu1 0.0320(11) 0.0351(11) 0.0413(12) 0.000 0.0016(8) 0.000 N1 0.072(8) 0.051(7) 0.062(8) -0.001(6) 0.000(6) -0.005(6) N2 0.062(8) 0.086(10) 0.053(7) -0.040(7) 0.018(6) -0.041(7) N3 0.064(8) 0.078(10) 0.072(9) -0.036(8) 0.013(7) 0.005(7) C1 0.085(12) 0.053(9) 0.064(10) 0.007(8) 0.000(9) -0.011(8) C2 0.097(14) 0.079(12) 0.048(9) -0.022(9) -0.007(9) 0.041(11) C3 0.064(9) 0.058(9) 0.072(10) 0.019(8) -0.014(8) -0.004(8) C4 0.058(9) 0.065(10) 0.062(9) 0.014(8) -0.012(7) -0.008(8) C6 0.042(7) 0.045(7) 0.054(8) 0.007(6) -0.009(6) -0.022(6) C7 0.067(10) 0.142(19) 0.048(9) -0.023(10) 0.000(8) -0.058(12) C8 0.091(15) 0.112(17) 0.109(16) -0.062(14) 0.056(13) -0.026(13) C9 0.046(9) 0.050(9) 0.117(15) -0.014(9) -0.017(9) 0.001(7) C5 0.056(9) 0.096(13) 0.049(8) 0.029(8) -0.013(7) -0.033(8) C10 0.039(7) 0.070(10) 0.071(10) 0.034(8) -0.013(7) -0.017(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 I1 Cu1 2.524(2) . ? Cu1 N1 1.927(11) . ? Cu1 N1 1.927(11) 2_556 ? N1 C1 1.346(9) . ? N1 C2 1.348(9) . ? N2 C1 1.325(9) . ? N2 N3 1.360(9) . ? N2 C3 1.487(19) . ? N3 C2 1.318(10) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.51(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C10 1.44(2) . ? C4 C5 1.49(2) . ? C6 C7 1.36(2) . ? C6 C5 1.38(2) . ? C6 H6A 0.9300 . ? C7 C8 1.40(3) . ? C7 H7A 0.9300 . ? C8 C9 1.32(3) . ? C8 H8A 0.9300 . ? C9 C10 1.42(2) 7_566 ? C9 H9A 0.9300 . ? C5 C10 1.44(2) 7_566 ? C10 C9 1.42(2) 7_566 ? C10 C5 1.44(2) 7_566 ? 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 Cu1 N1 125.8(6) . 2_556 ? N1 Cu1 I1 117.1(3) . . ? N1 Cu1 I1 117.1(3) 2_556 . ? C1 N1 C2 103.8(12) . . ? C1 N1 Cu1 126.4(8) . . ? C2 N1 Cu1 129.7(10) . . ? C1 N2 N3 111.0(12) . . ? C1 N2 C3 128.7(12) . . ? N3 N2 C3 120.3(12) . . ? C2 N3 N2 102.5(12) . . ? N2 C1 N1 108.5(12) . . ? N2 C1 H1A 125.8 . . ? N1 C1 H1A 125.8 . . ? N3 C2 N1 114.2(13) . . ? N3 C2 H2A 122.9 . . ? N1 C2 H2A 122.9 . . ? N2 C3 C4 111.8(13) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C10 C4 C5 123.2(14) . . ? C10 C4 C3 118.9(15) . . ? C5 C4 C3 117.8(13) . . ? C7 C6 C5 121.3(14) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 118.3(15) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? C9 C8 C7 121.7(17) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 123.2(15) . 7_566 ? C8 C9 H9A 118.4 . . ? C10 C9 H9A 118.4 7_566 . ? C6 C5 C10 121.2(15) . 7_566 ? C6 C5 C4 121.3(14) . . ? C10 C5 C4 116.9(14) 7_566 . ? C9 C10 C5 114.2(14) 7_566 7_566 ? C9 C10 C4 125.9(14) 7_566 . ? C5 C10 C4 119.8(15) 7_566 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 N1 C1 13.7(12) 2_556 . . . ? I1 Cu1 N1 C1 -166.3(12) . . . . ? N1 Cu1 N1 C2 -163.4(16) 2_556 . . . ? I1 Cu1 N1 C2 16.6(16) . . . . ? C1 N2 N3 C2 -2.1(19) . . . . ? C3 N2 N3 C2 179.4(14) . . . . ? N3 N2 C1 N1 2(2) . . . . ? C3 N2 C1 N1 -179.4(14) . . . . ? C2 N1 C1 N2 -1.3(18) . . . . ? Cu1 N1 C1 N2 -179.0(11) . . . . ? N2 N3 C2 N1 1(2) . . . . ? C1 N1 C2 N3 0(2) . . . . ? Cu1 N1 C2 N3 177.5(12) . . . . ? C1 N2 C3 C4 109(2) . . . . ? N3 N2 C3 C4 -73.2(19) . . . . ? N2 C3 C4 C10 -86.2(18) . . . . ? N2 C3 C4 C5 93.8(16) . . . . ? C5 C6 C7 C8 2(3) . . . . ? C6 C7 C8 C9 1(3) . . . . ? C7 C8 C9 C10 -4(3) . . . 7_566 ? C7 C6 C5 C10 -1(3) . . . 7_566 ? C7 C6 C5 C4 170.1(17) . . . . ? C10 C4 C5 C6 -173.7(15) . . . . ? C3 C4 C5 C6 6(2) . . . . ? C10 C4 C5 C10 -2(3) . . . 7_566 ? C3 C4 C5 C10 177.9(14) . . . 7_566 ? C5 C4 C10 C9 -172.7(16) . . . 7_566 ? C3 C4 C10 C9 7(2) . . . 7_566 ? C5 C4 C10 C5 2(3) . . . 7_566 ? C3 C4 C10 C5 -177.8(15) . . . 7_566 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.436 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.223 #END data_2 _database_code_depnum_ccdc_archive 'CCDC 630075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Ag B F4 N6 O0' _chemical_formula_weight 535.07 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pccn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 23.858(5) _cell_length_b 5.2642(10) _cell_length_c 15.317(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1923.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1893 _cell_measurement_theta_min 3.1614 _cell_measurement_theta_max 23.9622 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9926 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.35 _reflns_number_total 1959 _reflns_number_gt 1204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.9075P] 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 1959 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.7500 0.2500 1.15515(3) 0.03776(19) Uani 1 2 d S . . N1 N 0.69570(15) -0.0730(7) 1.1382(2) 0.0318(9) Uani 1 1 d . . . N2 N 0.63882(17) -0.4005(8) 1.1661(2) 0.0406(10) Uani 1 1 d . . . N3 N 0.64793(15) -0.3761(7) 1.0787(2) 0.0303(8) Uani 1 1 d . . . C1 C 0.68172(19) -0.1827(8) 1.0636(3) 0.0315(10) Uani 1 1 d . . . H1A H 0.6939 -0.1312 1.0087 0.038 Uiso 1 1 calc R . . C2 C 0.6688(2) -0.2135(9) 1.1989(3) 0.0409(12) Uani 1 1 d . . . H2A H 0.6713 -0.1812 1.2584 0.049 Uiso 1 1 calc R . . C3 C 0.62140(18) -0.5515(8) 1.0164(3) 0.0320(10) Uani 1 1 d . . . H3A H 0.6300 -0.7245 1.0337 0.038 Uiso 1 1 calc R . . H3B H 0.6376 -0.5241 0.9591 0.038 Uiso 1 1 calc R . . C4 C 0.55888(17) -0.5231(7) 1.0098(3) 0.0248(9) Uani 1 1 d . . . C5 C 0.53684(18) -0.3411(8) 0.9516(3) 0.0263(10) Uani 1 1 d . . . C6 C 0.5715(2) -0.1744(8) 0.9020(3) 0.0343(11) Uani 1 1 d . . . H6A H 0.6102 -0.1861 0.9075 0.041 Uiso 1 1 calc R . . C7 C 0.5494(2) 0.0008(8) 0.8468(3) 0.0385(12) Uani 1 1 d . . . H7A H 0.5732 0.1099 0.8165 0.046 Uiso 1 1 calc R . . C8 C 0.4912(2) 0.0195(9) 0.8350(3) 0.0393(12) Uani 1 1 d . . . H8A H 0.4764 0.1376 0.7961 0.047 Uiso 1 1 calc R . . C9 C 0.4565(2) -0.1363(9) 0.8807(3) 0.0337(11) Uani 1 1 d . . . H9A H 0.4180 -0.1223 0.8724 0.040 Uiso 1 1 calc R . . C10 C 0.47705(18) -0.3203(7) 0.9409(3) 0.0268(10) Uani 1 1 d . . . B1 B 0.7500 0.2500 0.8805(6) 0.057(3) Uani 1 2 d S . . F1 F 0.7500 0.2500 0.9651(3) 0.095(2) Uani 1 2 d S A 1 F1' F 0.7569(5) -0.038(2) 0.8818(8) 0.150(5) Uani 0.50 1 d P A 2 F2 F 0.7038(2) 0.2360(12) 0.8375(3) 0.144(3) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0362(3) 0.0335(3) 0.0436(3) 0.000 0.000 -0.0056(3) N1 0.029(2) 0.033(2) 0.034(2) 0.0024(18) -0.0022(16) 0.0014(17) N2 0.044(3) 0.043(3) 0.034(2) 0.0028(19) -0.0004(19) -0.009(2) N3 0.028(2) 0.031(2) 0.032(2) 0.0018(17) 0.0002(16) 0.0001(17) C1 0.030(2) 0.030(3) 0.034(2) 0.0027(19) 0.004(2) 0.0009(18) C2 0.046(3) 0.046(3) 0.031(2) 0.001(2) -0.002(2) -0.008(2) C3 0.028(2) 0.030(2) 0.037(3) -0.003(2) -0.001(2) 0.0032(19) C4 0.025(2) 0.021(2) 0.028(2) -0.0059(17) -0.0010(18) -0.0012(17) C5 0.031(2) 0.021(2) 0.027(2) -0.0078(18) 0.0031(19) -0.0018(18) C6 0.036(3) 0.035(3) 0.032(2) -0.002(2) 0.005(2) -0.0029(19) C7 0.054(3) 0.034(3) 0.027(2) 0.004(2) 0.011(2) -0.011(2) C8 0.056(3) 0.030(3) 0.031(3) 0.006(2) 0.000(2) 0.005(2) C9 0.036(3) 0.031(2) 0.034(2) -0.003(2) -0.002(2) 0.005(2) C10 0.036(3) 0.019(2) 0.025(2) -0.0058(17) -0.0015(19) 0.0015(17) B1 0.043(5) 0.096(8) 0.033(4) 0.000 0.000 -0.008(6) F1 0.075(3) 0.171(6) 0.038(3) 0.000 0.000 -0.036(4) F1' 0.247(15) 0.089(8) 0.116(8) -0.034(6) 0.001(9) 0.038(8) F2 0.093(3) 0.245(8) 0.094(3) -0.042(4) -0.047(3) 0.014(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 Ag1 N1 2.153(4) 2_655 ? Ag1 N1 2.153(4) . ? N1 C1 1.322(6) . ? N1 C2 1.350(6) . ? N2 C2 1.317(6) . ? N2 N3 1.362(5) . ? N3 C1 1.319(6) . ? N3 C3 1.471(6) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.502(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C10 1.409(6) 5_647 ? C4 C5 1.410(6) . ? C5 C6 1.425(6) . ? C5 C10 1.440(6) . ? C6 C7 1.357(6) . ? C6 H6A 0.9300 . ? C7 C8 1.405(7) . ? C7 H7A 0.9300 . ? C8 C9 1.360(7) . ? C8 H8A 0.9300 . ? C9 C10 1.425(6) . ? C9 H9A 0.9300 . ? C10 C4 1.409(6) 5_647 ? B1 F2 1.286(6) 2_655 ? B1 F2 1.286(6) . ? B1 F1 1.295(10) . ? B1 F1' 1.527(11) . ? B1 F1' 1.527(11) 2_655 ? 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 Ag1 N1 166.12(19) 2_655 . ? C1 N1 C2 103.6(4) . . ? C1 N1 Ag1 126.9(3) . . ? C2 N1 Ag1 129.4(3) . . ? C2 N2 N3 102.5(4) . . ? C1 N3 N2 110.0(4) . . ? C1 N3 C3 129.4(4) . . ? N2 N3 C3 120.6(4) . . ? N3 C1 N1 109.9(4) . . ? N3 C1 H1A 125.1 . . ? N1 C1 H1A 125.1 . . ? N2 C2 N1 113.9(4) . . ? N2 C2 H2A 123.0 . . ? N1 C2 H2A 123.0 . . ? N3 C3 C4 114.1(3) . . ? N3 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N3 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C10 C4 C5 120.6(4) 5_647 . ? C10 C4 C3 120.7(4) 5_647 . ? C5 C4 C3 118.7(4) . . ? C4 C5 C6 122.6(4) . . ? C4 C5 C10 119.6(4) . . ? C6 C5 C10 117.8(4) . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 120.8(4) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C10 122.2(4) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? C4 C10 C9 122.3(4) 5_647 . ? C4 C10 C5 119.8(4) 5_647 . ? C9 C10 C5 117.9(4) . . ? F2 B1 F2 118.3(9) 2_655 . ? F2 B1 F1 120.8(4) 2_655 . ? F2 B1 F1 120.8(4) . . ? F2 B1 F1' 88.4(6) 2_655 . ? F2 B1 F1' 92.4(6) . . ? F1 B1 F1' 89.3(6) . . ? F2 B1 F1' 92.4(6) 2_655 2_655 ? F2 B1 F1' 88.4(6) . 2_655 ? F1 B1 F1' 89.3(6) . 2_655 ? F1' B1 F1' 178.5(11) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C1 4.6(3) 2_655 . . . ? N1 Ag1 N1 C2 -176.6(4) 2_655 . . . ? C2 N2 N3 C1 0.0(5) . . . . ? C2 N2 N3 C3 -179.9(4) . . . . ? N2 N3 C1 N1 -0.4(5) . . . . ? C3 N3 C1 N1 179.4(4) . . . . ? C2 N1 C1 N3 0.7(5) . . . . ? Ag1 N1 C1 N3 179.7(3) . . . . ? N3 N2 C2 N1 0.4(5) . . . . ? C1 N1 C2 N2 -0.7(6) . . . . ? Ag1 N1 C2 N2 -179.7(3) . . . . ? C1 N3 C3 C4 -111.6(5) . . . . ? N2 N3 C3 C4 68.3(5) . . . . ? N3 C3 C4 C10 -95.4(5) . . . 5_647 ? N3 C3 C4 C5 86.2(5) . . . . ? C10 C4 C5 C6 178.5(4) 5_647 . . . ? C3 C4 C5 C6 -3.2(6) . . . . ? C10 C4 C5 C10 -1.7(6) 5_647 . . . ? C3 C4 C5 C10 176.7(4) . . . . ? C4 C5 C6 C7 -179.5(4) . . . . ? C10 C5 C6 C7 0.6(6) . . . . ? C5 C6 C7 C8 -1.7(7) . . . . ? C6 C7 C8 C9 1.4(7) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C8 C9 C10 C4 178.1(4) . . . 5_647 ? C8 C9 C10 C5 -1.0(7) . . . . ? C4 C5 C10 C4 1.6(6) . . . 5_647 ? C6 C5 C10 C4 -178.5(4) . . . 5_647 ? C4 C5 C10 C9 -179.2(4) . . . . ? C6 C5 C10 C9 0.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.511 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.094 #END data_3 _database_code_depnum_ccdc_archive 'CCDC 630076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 N8 O6 Zn' _chemical_formula_weight 529.78 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.142(5) _cell_length_b 5.1544(10) _cell_length_c 15.608(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.98(3) _cell_angle_gamma 90.00 _cell_volume 2003.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3192 _cell_measurement_theta_min 1.6357 _cell_measurement_theta_max 28.6732 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8012 _exptl_absorpt_correction_T_max 0.8204 _exptl_absorpt_process_details ? _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12491 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.68 _reflns_number_total 2569 _reflns_number_gt 2337 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+3.0437P] 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 0.0039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2569 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Zn1 Zn 0.0000 0.32262(6) 0.7500 0.01277(11) Uani 1 2 d S . . N1 N -0.06144(6) 0.1046(3) 0.69797(10) 0.0134(3) Uani 1 1 d . . . N2 N -0.11038(6) -0.1706(3) 0.61664(9) 0.0117(3) Uani 1 1 d . . . N3 N -0.12902(6) -0.1809(3) 0.69472(10) 0.0169(3) Uani 1 1 d . . . N4 N -0.03633(6) 0.5158(3) 0.89563(10) 0.0152(3) Uani 1 1 d . . . C1 C -0.09831(7) -0.0131(4) 0.74130(12) 0.0169(4) Uani 1 1 d . . . H1A H -0.1014 0.0225 0.7988 0.020 Uiso 1 1 calc R . . C2 C -0.07024(7) -0.0021(3) 0.61920(11) 0.0128(3) Uani 1 1 d . . . H2A H -0.0513 0.0356 0.5736 0.015 Uiso 1 1 calc R . . C3 C -0.13450(7) -0.3366(3) 0.54497(11) 0.0123(3) Uani 1 1 d . . . H3A H -0.1283 -0.5172 0.5608 0.015 Uiso 1 1 calc R . . H3B H -0.1172 -0.3025 0.4943 0.015 Uiso 1 1 calc R . . C4 C -0.19422(7) -0.2902(3) 0.52284(11) 0.0108(3) Uani 1 1 d . . . C5 C -0.23085(7) -0.4448(3) 0.56115(11) 0.0113(3) Uani 1 1 d . . . C6 C -0.21397(8) -0.6420(4) 0.62386(11) 0.0141(4) Uani 1 1 d . . . H6A H -0.1774 -0.6666 0.6414 0.017 Uiso 1 1 calc R . . C7 C -0.24964(8) -0.7941(4) 0.65854(12) 0.0163(4) Uani 1 1 d . . . H7A H -0.2374 -0.9214 0.6987 0.020 Uiso 1 1 calc R . . C8 C -0.30545(8) -0.7586(4) 0.63336(12) 0.0168(4) Uani 1 1 d . . . H8A H -0.3298 -0.8641 0.6566 0.020 Uiso 1 1 calc R . . C9 C -0.17639(7) 0.0707(4) 0.42481(11) 0.0140(4) Uani 1 1 d . . . H9A H -0.1396 0.0492 0.4402 0.017 Uiso 1 1 calc R . . C10 C -0.21256(7) -0.0952(3) 0.46297(11) 0.0116(3) Uani 1 1 d . . . O1 O -0.01375(6) 0.6052(3) 0.83220(9) 0.0188(3) Uani 1 1 d . . . O2 O -0.04415(6) 0.2779(3) 0.89887(9) 0.0211(3) Uani 1 1 d . . . O3 O -0.04912(6) 0.6691(3) 0.94970(10) 0.0236(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01060(17) 0.01272(17) 0.01444(17) 0.000 -0.00017(11) 0.000 N1 0.0109(7) 0.0149(7) 0.0137(7) 0.0012(6) -0.0006(6) -0.0005(6) N2 0.0091(7) 0.0149(7) 0.0108(7) -0.0002(6) 0.0003(5) 0.0001(6) N3 0.0159(8) 0.0231(9) 0.0121(7) -0.0012(6) 0.0034(6) -0.0060(6) N4 0.0106(7) 0.0173(8) 0.0176(7) -0.0030(6) 0.0013(6) 0.0001(6) C1 0.0148(9) 0.0227(10) 0.0134(8) -0.0021(7) 0.0018(7) -0.0054(7) C2 0.0101(8) 0.0144(8) 0.0138(8) 0.0008(7) 0.0009(6) 0.0004(7) C3 0.0108(8) 0.0135(8) 0.0124(8) -0.0032(7) 0.0009(6) 0.0001(7) C4 0.0100(8) 0.0124(8) 0.0095(8) -0.0044(6) 0.0001(6) 0.0002(6) C5 0.0130(8) 0.0111(8) 0.0096(7) -0.0039(6) 0.0012(6) 0.0004(7) C6 0.0149(9) 0.0141(8) 0.0129(8) -0.0017(7) 0.0004(7) 0.0014(7) C7 0.0223(10) 0.0130(9) 0.0137(8) 0.0010(7) 0.0035(7) 0.0017(7) C8 0.0204(10) 0.0150(9) 0.0163(9) -0.0018(7) 0.0068(7) -0.0037(7) C9 0.0126(8) 0.0154(9) 0.0143(8) -0.0036(7) 0.0032(7) -0.0019(7) C10 0.0126(8) 0.0113(8) 0.0111(8) -0.0038(6) 0.0018(6) -0.0006(6) O1 0.0213(7) 0.0187(7) 0.0181(7) -0.0001(5) 0.0082(6) -0.0020(6) O2 0.0248(8) 0.0151(7) 0.0238(7) -0.0031(6) 0.0050(6) -0.0042(6) O3 0.0255(8) 0.0226(7) 0.0246(7) -0.0094(6) 0.0106(6) 0.0006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.9898(16) . ? Zn1 N1 1.9898(16) 2_556 ? Zn1 O1 2.0026(14) . ? Zn1 O1 2.0026(14) 2_556 ? N1 C2 1.337(2) . ? N1 C1 1.364(2) . ? N2 C2 1.328(2) . ? N2 N3 1.366(2) . ? N2 C3 1.471(2) . ? N3 C1 1.310(2) . ? N4 O3 1.231(2) . ? N4 O2 1.244(2) . ? N4 O1 1.293(2) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.512(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C10 1.406(2) . ? C4 C5 1.412(2) . ? C5 C6 1.434(2) . ? C5 C10 1.435(2) 7_446 ? C6 C7 1.359(3) . ? C6 H6A 0.9300 . ? C7 C8 1.415(3) . ? C7 H7A 0.9300 . ? C8 C9 1.363(3) 7_446 ? C8 H8A 0.9300 . ? C9 C8 1.363(3) 7_446 ? C9 C10 1.436(2) . ? C9 H9A 0.9300 . ? C10 C5 1.435(2) 7_446 ? 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 Zn1 N1 111.24(9) . 2_556 ? N1 Zn1 O1 118.62(6) . . ? N1 Zn1 O1 110.03(6) 2_556 . ? N1 Zn1 O1 110.03(6) . 2_556 ? N1 Zn1 O1 118.62(6) 2_556 2_556 ? O1 Zn1 O1 86.66(8) . 2_556 ? C2 N1 C1 103.64(15) . . ? C2 N1 Zn1 128.88(13) . . ? C1 N1 Zn1 126.27(13) . . ? C2 N2 N3 110.61(15) . . ? C2 N2 C3 129.41(15) . . ? N3 N2 C3 119.97(14) . . ? C1 N3 N2 102.76(15) . . ? O3 N4 O2 123.18(16) . . ? O3 N4 O1 118.69(16) . . ? O2 N4 O1 118.13(15) . . ? N3 C1 N1 114.03(16) . . ? N3 C1 H1A 123.0 . . ? N1 C1 H1A 123.0 . . ? N2 C2 N1 108.96(16) . . ? N2 C2 H2A 125.5 . . ? N1 C2 H2A 125.5 . . ? N2 C3 C4 111.90(14) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C10 C4 C5 120.79(16) . . ? C10 C4 C3 119.25(16) . . ? C5 C4 C3 119.95(16) . . ? C4 C5 C6 122.72(16) . . ? C4 C5 C10 119.29(16) . 7_446 ? C6 C5 C10 118.00(16) . 7_446 ? C7 C6 C5 122.13(17) . . ? C7 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C6 C7 C8 119.89(17) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.30(17) 7_446 . ? C9 C8 H8A 119.8 7_446 . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 121.77(17) 7_446 . ? C8 C9 H9A 119.1 7_446 . ? C10 C9 H9A 119.1 . . ? C4 C10 C5 119.91(16) . 7_446 ? C4 C10 C9 122.20(16) . . ? C5 C10 C9 117.88(16) 7_446 . ? N4 O1 Zn1 111.37(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 N1 C2 -84.91(16) 2_556 . . . ? O1 Zn1 N1 C2 145.99(15) . . . . ? O1 Zn1 N1 C2 48.61(17) 2_556 . . . ? N1 Zn1 N1 C1 80.39(15) 2_556 . . . ? O1 Zn1 N1 C1 -48.71(18) . . . . ? O1 Zn1 N1 C1 -146.08(15) 2_556 . . . ? C2 N2 N3 C1 0.1(2) . . . . ? C3 N2 N3 C1 179.31(16) . . . . ? N2 N3 C1 N1 0.3(2) . . . . ? C2 N1 C1 N3 -0.6(2) . . . . ? Zn1 N1 C1 N3 -168.84(13) . . . . ? N3 N2 C2 N1 -0.5(2) . . . . ? C3 N2 C2 N1 -179.57(16) . . . . ? C1 N1 C2 N2 0.6(2) . . . . ? Zn1 N1 C2 N2 168.45(12) . . . . ? C2 N2 C3 C4 -123.23(19) . . . . ? N3 N2 C3 C4 57.7(2) . . . . ? N2 C3 C4 C10 87.86(19) . . . . ? N2 C3 C4 C5 -93.17(19) . . . . ? C10 C4 C5 C6 -178.63(16) . . . . ? C3 C4 C5 C6 2.4(3) . . . . ? C10 C4 C5 C10 1.3(3) . . . 7_446 ? C3 C4 C5 C10 -177.67(15) . . . 7_446 ? C4 C5 C6 C7 -178.21(17) . . . . ? C10 C5 C6 C7 1.9(3) 7_446 . . . ? C5 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 -0.7(3) . . . 7_446 ? C5 C4 C10 C5 -1.3(3) . . . 7_446 ? C3 C4 C10 C5 177.67(15) . . . 7_446 ? C5 C4 C10 C9 178.06(16) . . . . ? C3 C4 C10 C9 -3.0(3) . . . . ? C8 C9 C10 C4 179.80(17) 7_446 . . . ? C8 C9 C10 C5 -0.8(3) 7_446 . . 7_446 ? O3 N4 O1 Zn1 -177.24(13) . . . . ? O2 N4 O1 Zn1 2.65(19) . . . . ? N1 Zn1 O1 N4 55.59(13) . . . . ? N1 Zn1 O1 N4 -74.06(12) 2_556 . . . ? O1 Zn1 O1 N4 166.63(14) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.782 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.082 data_4 _database_code_depnum_ccdc_archive 'CCDC 630077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Cl2 N12 O11 Zn' _chemical_formula_weight 1027.15 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 13.678(2) _cell_length_b 34.456(5) _cell_length_c 10.2430(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.382(2) _cell_angle_gamma 90.00 _cell_volume 4525.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4703 _cell_measurement_theta_min 2.3644 _cell_measurement_theta_max 25.8076 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8669 _exptl_absorpt_correction_T_max 0.9077 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 19500 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8400 _reflns_number_gt 4909 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+1.0300P] 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_number_reflns 8400 _refine_ls_number_parameters 656 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.080 _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 Zn2 Zn -0.03236(4) 0.126983(18) 0.04142(6) 0.0387(2) Uani 1 1 d . . . N1 N 0.0477(3) 0.16466(13) -0.0517(4) 0.0379(10) Uani 1 1 d . . . N2 N 0.1216(3) 0.21646(13) -0.1141(5) 0.0528(12) Uani 1 1 d . . . N3 N 0.1463(3) 0.18250(13) -0.1657(4) 0.0381(10) Uani 1 1 d . . . N4 N 0.7194(3) 0.20283(13) 0.0240(4) 0.0428(11) Uani 1 1 d . . . N5 N 0.7123(3) 0.20771(13) -0.1102(4) 0.0466(11) Uani 1 1 d . . . N6 N 0.8462(3) 0.16793(12) 0.0024(4) 0.0415(11) Uani 1 1 d . . . N7 N 0.0965(3) 0.08774(12) 0.1127(4) 0.0375(10) Uani 1 1 d . . . N8 N 0.2114(3) 0.04078(13) 0.1178(4) 0.0476(12) Uani 1 1 d . . . N9 N 0.2289(3) 0.05491(12) 0.2476(4) 0.0354(10) Uani 1 1 d . . . N10 N 0.8046(3) 0.08028(12) 0.6408(4) 0.0355(10) Uani 1 1 d . . . N11 N 0.8028(3) 0.04758(13) 0.7125(5) 0.0535(13) Uani 1 1 d . . . N12 N 0.8994(3) 0.09416(12) 0.8555(4) 0.0374(10) Uani 1 1 d . . . C1 C 0.1015(4) 0.15292(15) -0.1290(5) 0.0400(12) Uani 1 1 d . . . H1A H 0.1068 0.1273 -0.1541 0.048 Uiso 1 1 calc R . . C2 C 0.0619(4) 0.20322(17) -0.0476(6) 0.0507(15) Uani 1 1 d . . . H2A H 0.0314 0.2196 -0.0006 0.061 Uiso 1 1 calc R . . C3 C 0.2123(4) 0.18286(16) -0.2519(5) 0.0418(13) Uani 1 1 d . . . H3A H 0.1849 0.2016 -0.3263 0.050 Uiso 1 1 calc R . . H3B H 0.2099 0.1575 -0.2941 0.050 Uiso 1 1 calc R . . C4 C 0.3243(3) 0.19291(15) -0.1690(5) 0.0349(12) Uani 1 1 d . . . C5 C 0.3628(4) 0.23017(15) -0.1797(5) 0.0389(12) Uani 1 1 d . . . C6 C 0.3001(4) 0.25973(18) -0.2661(6) 0.0589(16) Uani 1 1 d . . . H6A H 0.2306 0.2544 -0.3173 0.071 Uiso 1 1 calc R . . C7 C 0.3387(5) 0.2952(2) -0.2757(7) 0.074(2) Uani 1 1 d . . . H7A H 0.2953 0.3140 -0.3321 0.089 Uiso 1 1 calc R . . C8 C 0.4435(5) 0.3041(2) -0.2016(7) 0.0680(18) Uani 1 1 d . . . H8A H 0.4690 0.3287 -0.2089 0.082 Uiso 1 1 calc R . . C9 C 0.5071(4) 0.27746(18) -0.1207(6) 0.0533(15) Uani 1 1 d . . . H9A H 0.5769 0.2837 -0.0753 0.064 Uiso 1 1 calc R . . C10 C 0.4712(4) 0.23980(15) -0.1018(5) 0.0373(12) Uani 1 1 d . . . C11 C 0.5333(4) 0.21180(17) -0.0099(5) 0.0432(14) Uani 1 1 d . . . C12 C 0.4939(4) 0.17477(16) 0.0013(5) 0.0415(13) Uani 1 1 d . . . C13 C 0.5561(5) 0.1459(2) 0.0933(6) 0.0567(16) Uani 1 1 d . . . H13A H 0.6243 0.1518 0.1485 0.068 Uiso 1 1 calc R . . C14 C 0.5178(5) 0.1100(2) 0.1021(6) 0.0700(19) Uani 1 1 d . . . H14A H 0.5594 0.0918 0.1639 0.084 Uiso 1 1 calc R . . C15 C 0.4160(5) 0.10024(18) 0.0183(7) 0.0618(17) Uani 1 1 d . . . H15A H 0.3907 0.0755 0.0235 0.074 Uiso 1 1 calc R . . C16 C 0.3538(4) 0.12663(17) -0.0704(6) 0.0530(15) Uani 1 1 d . . . H16A H 0.2866 0.1194 -0.1256 0.064 Uiso 1 1 calc R . . C17 C 0.3885(4) 0.16499(16) -0.0815(5) 0.0388(12) Uani 1 1 d . . . C18 C 0.6454(4) 0.22139(18) 0.0791(5) 0.0508(15) Uani 1 1 d . . . H18A H 0.6552 0.2493 0.0813 0.061 Uiso 1 1 calc R . . H18B H 0.6588 0.2126 0.1737 0.061 Uiso 1 1 calc R . . C19 C 0.7900(4) 0.18674(16) -0.1167(5) 0.0470(14) Uani 1 1 d . . . H19A H 0.8059 0.1848 -0.1976 0.056 Uiso 1 1 calc R . . C20 C 0.7984(4) 0.17948(17) 0.0891(5) 0.0498(14) Uani 1 1 d . . . H20A H 0.8178 0.1722 0.1820 0.060 Uiso 1 1 calc R . . C21 C 0.1310(4) 0.06155(16) 0.0425(5) 0.0450(14) Uani 1 1 d . . . H21A H 0.1001 0.0583 -0.0533 0.054 Uiso 1 1 calc R . . C22 C 0.1617(4) 0.08257(15) 0.2436(5) 0.0404(13) Uani 1 1 d . . . H22A H 0.1599 0.0965 0.3204 0.048 Uiso 1 1 calc R . . C23 C 0.3101(3) 0.03763(15) 0.3698(5) 0.0383(12) Uani 1 1 d . . . H23A H 0.3068 0.0096 0.3599 0.046 Uiso 1 1 calc R . . H23B H 0.2943 0.0440 0.4526 0.046 Uiso 1 1 calc R . . C24 C 0.4206(3) 0.05071(14) 0.3915(4) 0.0330(11) Uani 1 1 d . . . C25 C 0.4599(3) 0.08455(14) 0.4718(4) 0.0336(11) Uani 1 1 d . . . C26 C 0.3974(4) 0.10808(17) 0.5246(5) 0.0498(14) Uani 1 1 d . . . H26A H 0.3284 0.1011 0.5070 0.060 Uiso 1 1 calc R . . C27 C 0.4352(4) 0.14055(18) 0.6001(6) 0.0607(17) Uani 1 1 d . . . H27A H 0.3926 0.1554 0.6342 0.073 Uiso 1 1 calc R . . C28 C 0.5390(5) 0.15162(18) 0.6262(6) 0.0599(16) Uani 1 1 d . . . H28A H 0.5649 0.1739 0.6777 0.072 Uiso 1 1 calc R . . C29 C 0.6024(4) 0.13001(16) 0.5770(5) 0.0505(14) Uani 1 1 d . . . H29A H 0.6704 0.1382 0.5937 0.061 Uiso 1 1 calc R . . C30 C 0.5664(4) 0.09536(14) 0.5008(4) 0.0338(11) Uani 1 1 d . . . C31 C 0.6322(3) 0.07110(14) 0.4554(4) 0.0322(11) Uani 1 1 d . . . C32 C 0.5929(3) 0.03799(14) 0.3759(4) 0.0339(12) Uani 1 1 d . . . C33 C 0.6557(4) 0.01266(15) 0.3271(5) 0.0434(13) Uani 1 1 d . . . H33A H 0.7268 0.0177 0.3527 0.052 Uiso 1 1 calc R . . C34 C 0.6153(5) -0.01811(19) 0.2454(6) 0.0640(17) Uani 1 1 d . . . H34A H 0.6577 -0.0334 0.2125 0.077 Uiso 1 1 calc R . . C35 C 0.5092(5) -0.02721(18) 0.2097(6) 0.0673(19) Uani 1 1 d . . . H35A H 0.4820 -0.0488 0.1547 0.081 Uiso 1 1 calc R . . C36 C 0.4460(4) -0.00480(16) 0.2546(5) 0.0513(15) Uani 1 1 d . . . H36A H 0.3757 -0.0112 0.2284 0.062 Uiso 1 1 calc R . . C37 C 0.4838(3) 0.02816(14) 0.3405(4) 0.0337(12) Uani 1 1 d . . . C38 C 0.7454(4) 0.08288(17) 0.4911(5) 0.0438(13) Uani 1 1 d . . . H38A H 0.7776 0.0662 0.4413 0.053 Uiso 1 1 calc R . . H38B H 0.7483 0.1093 0.4603 0.053 Uiso 1 1 calc R . . C39 C 0.8625(3) 0.10693(15) 0.7260(5) 0.0344(11) Uani 1 1 d . . . H39A H 0.8755 0.1315 0.6982 0.041 Uiso 1 1 calc R . . C40 C 0.8610(4) 0.05766(16) 0.8412(5) 0.0495(15) Uani 1 1 d . . . H40A H 0.8744 0.0408 0.9162 0.059 Uiso 1 1 calc R . . C41 C 0.0849(9) 0.1858(3) 0.3170(11) 0.162(5) Uani 1 1 d . . . H41A H 0.0972 0.1872 0.4150 0.242 Uiso 1 1 calc R . . H41B H 0.0457 0.2081 0.2713 0.242 Uiso 1 1 calc R . . H41C H 0.1504 0.1852 0.3021 0.242 Uiso 1 1 calc R . . C42 C -0.2250(6) 0.0807(3) 0.1044(10) 0.118(3) Uani 1 1 d . . . H42A H -0.2355 0.0616 0.1666 0.177 Uiso 1 1 calc R . . H42B H -0.2546 0.0715 0.0103 0.177 Uiso 1 1 calc R . . H42C H -0.2584 0.1045 0.1137 0.177 Uiso 1 1 calc R . . Cl1 Cl 0.87066(12) 0.19561(5) 0.49563(15) 0.0594(4) Uani 1 1 d D . . Cl2 Cl 0.08778(11) 0.06911(5) 0.57510(15) 0.0587(4) Uani 1 1 d D . . O5 O -0.0135(4) 0.0784(2) 0.4912(8) 0.164(3) Uani 1 1 d . . . O6 O 0.1161(4) 0.03488(14) 0.5234(5) 0.0924(16) Uani 1 1 d . . . O7 O 0.1534(5) 0.09936(19) 0.5638(6) 0.129(2) Uani 1 1 d . . . O8 O 0.1268(14) 0.0639(7) 0.7240(8) 0.111(5) Uani 0.548(14) 1 d PD . . O8' O 0.0647(14) 0.0684(8) 0.6969(17) 0.092(5) Uani 0.452(14) 1 d P . . O9 O 0.0249(3) 0.14992(12) 0.2588(4) 0.0575(10) Uani 1 1 d . . . H9B H 0.0086 0.1346 0.3233 0.069 Uiso 1 1 calc R . . O10 O -0.1163(3) 0.08722(13) 0.1378(4) 0.0708(12) Uani 1 1 d . . . H10A H -0.0734 0.0725 0.2118 0.085 Uiso 1 1 calc R . . O1W O -0.0317(6) 0.01703(17) 0.2381(6) 0.117(2) Uani 1 1 d D . . H1WA H -0.053(8) -0.0064(10) 0.234(10) 0.175 Uiso 1 1 d D . . H1WB H -0.058(8) 0.026(2) 0.296(9) 0.175 Uiso 1 1 d D . . O1 O 0.8825(6) 0.22517(17) 0.4140(7) 0.150(3) Uani 1 1 d D A . O2 O 0.9546(7) 0.1718(4) 0.5592(19) 0.130(7) Uani 0.548(14) 1 d PD A 1 O3 O 0.939(3) 0.2190(8) 0.603(2) 0.39(2) Uani 0.548(14) 1 d PD A 1 O4 O 0.7793(10) 0.1787(4) 0.4022(11) 0.132(6) Uani 0.548(14) 1 d PD A 1 O2' O 0.887(2) 0.1591(3) 0.435(2) 0.133(10) Uani 0.452(14) 1 d PD A 2 O3' O 0.845(2) 0.2047(5) 0.6115(17) 0.162(12) Uani 0.452(14) 1 d PD A 2 O4' O 0.7821(13) 0.1926(4) 0.536(3) 0.123(10) Uani 0.452(14) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn2 0.0207(3) 0.0525(4) 0.0373(3) -0.0007(3) 0.0032(2) 0.0032(3) N1 0.020(2) 0.044(3) 0.048(3) 0.001(2) 0.0110(18) -0.0010(19) N2 0.040(3) 0.046(3) 0.073(3) -0.008(2) 0.020(2) -0.009(2) N3 0.017(2) 0.044(3) 0.046(2) -0.002(2) 0.0014(17) -0.0044(19) N4 0.022(2) 0.061(3) 0.041(3) -0.013(2) 0.0061(18) 0.003(2) N5 0.029(2) 0.058(3) 0.051(3) -0.004(2) 0.0111(19) 0.008(2) N6 0.023(2) 0.057(3) 0.040(2) -0.002(2) 0.0046(18) 0.004(2) N7 0.026(2) 0.051(3) 0.028(2) -0.0015(19) -0.0014(17) 0.0014(19) N8 0.036(2) 0.065(3) 0.034(2) -0.002(2) 0.0028(19) 0.018(2) N9 0.020(2) 0.048(3) 0.032(2) 0.0012(19) 0.0000(16) -0.0002(19) N10 0.0191(19) 0.043(3) 0.035(2) -0.001(2) -0.0027(16) -0.0039(18) N11 0.045(3) 0.042(3) 0.054(3) 0.000(2) -0.007(2) -0.014(2) N12 0.021(2) 0.043(3) 0.038(2) -0.0007(19) -0.0019(17) -0.0067(19) C1 0.031(3) 0.028(3) 0.059(3) -0.002(2) 0.015(2) -0.004(2) C2 0.035(3) 0.047(4) 0.067(4) -0.012(3) 0.014(3) 0.001(3) C3 0.036(3) 0.048(3) 0.036(3) 0.002(2) 0.006(2) -0.006(2) C4 0.027(3) 0.044(3) 0.034(3) -0.003(2) 0.012(2) -0.003(2) C5 0.030(3) 0.052(4) 0.037(3) 0.006(2) 0.015(2) 0.002(2) C6 0.043(3) 0.067(4) 0.056(4) 0.020(3) 0.003(3) -0.009(3) C7 0.066(5) 0.067(5) 0.078(5) 0.037(4) 0.010(4) 0.004(4) C8 0.066(4) 0.065(5) 0.075(4) 0.017(4) 0.027(4) -0.016(4) C9 0.037(3) 0.067(4) 0.058(4) -0.008(3) 0.019(3) -0.018(3) C10 0.026(3) 0.050(3) 0.040(3) -0.005(2) 0.016(2) -0.002(2) C11 0.025(3) 0.066(4) 0.039(3) -0.008(3) 0.013(2) 0.006(3) C12 0.035(3) 0.059(4) 0.038(3) 0.002(3) 0.022(2) 0.011(3) C13 0.043(3) 0.080(5) 0.049(3) 0.017(3) 0.018(3) 0.022(3) C14 0.067(5) 0.085(5) 0.060(4) 0.035(4) 0.025(3) 0.032(4) C15 0.076(5) 0.044(4) 0.079(5) 0.017(3) 0.045(4) 0.019(3) C16 0.044(3) 0.059(4) 0.064(4) 0.001(3) 0.029(3) 0.001(3) C17 0.033(3) 0.049(4) 0.040(3) 0.002(2) 0.021(2) 0.006(2) C18 0.023(3) 0.079(4) 0.047(3) -0.016(3) 0.008(2) 0.002(3) C19 0.037(3) 0.067(4) 0.034(3) 0.003(3) 0.008(2) 0.009(3) C20 0.026(3) 0.079(4) 0.036(3) 0.003(3) 0.000(2) 0.010(3) C21 0.040(3) 0.058(4) 0.029(3) -0.010(3) 0.002(2) 0.008(3) C22 0.031(3) 0.053(4) 0.029(3) -0.002(2) 0.001(2) 0.004(3) C23 0.022(2) 0.045(3) 0.037(3) 0.011(2) -0.004(2) -0.002(2) C24 0.023(2) 0.044(3) 0.023(2) 0.007(2) -0.0029(18) -0.002(2) C25 0.025(2) 0.042(3) 0.024(2) 0.001(2) -0.0028(19) 0.000(2) C26 0.028(3) 0.074(4) 0.043(3) -0.015(3) 0.007(2) 0.002(3) C27 0.044(3) 0.079(5) 0.056(4) -0.027(3) 0.014(3) 0.006(3) C28 0.055(4) 0.058(4) 0.054(4) -0.025(3) 0.002(3) -0.004(3) C29 0.030(3) 0.054(4) 0.055(3) -0.006(3) -0.001(2) -0.007(3) C30 0.030(3) 0.040(3) 0.024(2) 0.000(2) -0.0006(19) -0.004(2) C31 0.020(2) 0.044(3) 0.026(2) 0.007(2) -0.0013(18) 0.000(2) C32 0.024(2) 0.043(3) 0.025(2) 0.005(2) -0.0039(19) 0.001(2) C33 0.031(3) 0.050(4) 0.041(3) -0.001(3) 0.001(2) 0.008(2) C34 0.050(4) 0.075(5) 0.059(4) -0.011(3) 0.010(3) 0.018(3) C35 0.049(4) 0.061(4) 0.068(4) -0.026(3) -0.009(3) 0.004(3) C36 0.032(3) 0.054(4) 0.052(3) -0.015(3) -0.005(2) 0.001(3) C37 0.026(2) 0.039(3) 0.026(2) 0.000(2) -0.0039(19) 0.001(2) C38 0.030(3) 0.063(4) 0.034(3) -0.001(2) 0.005(2) -0.005(3) C39 0.023(2) 0.036(3) 0.038(3) -0.001(2) 0.003(2) -0.002(2) C40 0.048(3) 0.043(4) 0.040(3) 0.012(3) -0.006(2) -0.008(3) C41 0.188(12) 0.190(12) 0.121(8) -0.027(8) 0.073(8) -0.049(10) C42 0.076(6) 0.118(7) 0.183(9) 0.042(6) 0.073(6) 0.010(5) Cl1 0.0554(9) 0.0621(11) 0.0564(9) 0.0157(8) 0.0141(7) 0.0040(8) Cl2 0.0468(8) 0.0731(11) 0.0608(10) -0.0145(8) 0.0246(7) -0.0030(8) O5 0.059(4) 0.193(7) 0.209(7) -0.046(5) 0.009(4) 0.052(4) O6 0.081(3) 0.082(4) 0.104(4) -0.029(3) 0.019(3) 0.027(3) O7 0.151(6) 0.138(5) 0.130(5) -0.058(4) 0.088(4) -0.078(5) O8 0.137(14) 0.147(12) 0.059(7) -0.001(7) 0.044(8) -0.003(14) O8' 0.099(12) 0.134(13) 0.062(8) 0.001(8) 0.054(8) -0.011(13) O9 0.047(2) 0.071(3) 0.046(2) -0.004(2) 0.0056(17) 0.006(2) O10 0.050(3) 0.089(3) 0.074(3) 0.032(2) 0.022(2) 0.006(2) O1W 0.153(6) 0.084(4) 0.088(4) 0.021(3) 0.011(4) -0.001(4) O1 0.204(7) 0.094(5) 0.186(7) 0.062(5) 0.112(6) 0.017(5) O2 0.061(7) 0.113(11) 0.188(15) 0.080(11) 0.008(8) 0.038(7) O3 0.28(3) 0.61(6) 0.140(18) -0.10(3) -0.09(2) -0.06(4) O4 0.118(10) 0.167(13) 0.070(8) -0.012(8) -0.020(7) -0.052(10) O2' 0.27(3) 0.042(8) 0.162(17) 0.000(8) 0.17(2) 0.006(10) O3' 0.26(3) 0.201(19) 0.076(10) -0.079(10) 0.121(15) -0.145(18) O4' 0.098(12) 0.063(9) 0.25(3) 0.013(11) 0.117(16) 0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn2 N6 2.109(4) 1_455 ? Zn2 N1 2.126(4) . ? Zn2 N12 2.131(4) 1_454 ? Zn2 N7 2.138(4) . ? Zn2 O10 2.227(4) . ? Zn2 O9 2.232(4) . ? N1 C1 1.319(6) . ? N1 C2 1.341(6) . ? N2 C2 1.313(7) . ? N2 N3 1.373(6) . ? N3 C1 1.310(6) . ? N3 C3 1.468(6) . ? N4 C20 1.326(6) . ? N4 N5 1.354(5) . ? N4 C18 1.466(6) . ? N5 C19 1.306(6) . ? N6 C20 1.333(6) . ? N6 C19 1.358(6) . ? N6 Zn2 2.109(4) 1_655 ? N7 C21 1.339(6) . ? N7 C22 1.339(5) . ? N8 C21 1.313(6) . ? N8 N9 1.357(5) . ? N9 C22 1.314(6) . ? N9 C23 1.479(5) . ? N10 C39 1.323(6) . ? N10 N11 1.350(6) . ? N10 C38 1.466(6) . ? N11 C40 1.326(6) . ? N12 C39 1.319(6) . ? N12 C40 1.351(6) . ? N12 Zn2 2.131(4) 1_656 ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.510(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C17 1.397(7) . ? C4 C5 1.407(7) . ? C5 C6 1.424(7) . ? C5 C10 1.455(6) . ? C6 C7 1.349(8) . ? C6 H6A 0.9300 . ? C7 C8 1.403(8) . ? C7 H7A 0.9300 . ? C8 C9 1.335(8) . ? C8 H8A 0.9300 . ? C9 C10 1.424(7) . ? C9 H9A 0.9300 . ? C10 C11 1.408(7) . ? C11 C12 1.405(7) . ? C11 C18 1.522(6) . ? C12 C13 1.430(7) . ? C12 C17 1.435(7) . ? C13 C14 1.358(9) . ? C13 H13A 0.9300 . ? C14 C15 1.398(9) . ? C14 H14A 0.9300 . ? C15 C16 1.356(8) . ? C15 H15A 0.9300 . ? C16 C17 1.422(7) . ? C16 H16A 0.9300 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.518(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C37 1.392(6) . ? C24 C25 1.420(6) . ? C25 C26 1.415(7) . ? C25 C30 1.431(6) . ? C26 C27 1.356(8) . ? C26 H26A 0.9300 . ? C27 C28 1.403(8) . ? C27 H27A 0.9300 . ? C28 C29 1.366(8) . ? C28 H28A 0.9300 . ? C29 C30 1.417(7) . ? C29 H29A 0.9300 . ? C30 C31 1.420(6) . ? C31 C32 1.396(6) . ? C31 C38 1.517(6) . ? C32 C33 1.431(7) . ? C32 C37 1.448(6) . ? C33 C34 1.345(7) . ? C33 H33A 0.9300 . ? C34 C35 1.403(8) . ? C34 H34A 0.9300 . ? C35 C36 1.354(7) . ? C35 H35A 0.9300 . ? C36 C37 1.419(7) . ? C36 H36A 0.9300 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 O9 1.489(11) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 O10 1.424(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cl1 O1 1.363(5) . ? Cl1 O2 1.376(7) . ? Cl1 O3' 1.386(8) . ? Cl1 O4 1.409(7) . ? Cl1 O4' 1.412(8) . ? Cl1 O3 1.416(10) . ? Cl1 O2' 1.456(8) . ? Cl2 O5 1.390(6) . ? Cl2 O8' 1.389(13) . ? Cl2 O6 1.401(4) . ? Cl2 O7 1.406(5) . ? Cl2 O8 1.441(7) . ? O8 O8' 0.811(17) . ? O9 H9B 0.9300 . ? O10 H10A 0.9300 . ? O1W H1WA 0.853(10) . ? O1W H1WB 0.856(10) . ? O2 O3 1.72(3) . ? O3' O4' 1.03(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Zn2 N1 90.07(16) 1_455 . ? N6 Zn2 N12 96.59(15) 1_455 1_454 ? N1 Zn2 N12 93.26(15) . 1_454 ? N6 Zn2 N7 171.51(15) 1_455 . ? N1 Zn2 N7 92.73(15) . . ? N12 Zn2 N7 91.26(15) 1_454 . ? N6 Zn2 O10 90.12(16) 1_455 . ? N1 Zn2 O10 179.61(17) . . ? N12 Zn2 O10 86.38(16) 1_454 . ? N7 Zn2 O10 87.13(15) . . ? N6 Zn2 O9 86.09(14) 1_455 . ? N1 Zn2 O9 100.06(15) . . ? N12 Zn2 O9 166.42(16) 1_454 . ? N7 Zn2 O9 85.54(14) . . ? O10 Zn2 O9 80.29(16) . . ? C1 N1 C2 102.5(4) . . ? C1 N1 Zn2 124.4(4) . . ? C2 N1 Zn2 133.1(4) . . ? C2 N2 N3 100.6(4) . . ? C1 N3 N2 110.5(4) . . ? C1 N3 C3 128.8(5) . . ? N2 N3 C3 120.7(4) . . ? C20 N4 N5 110.1(4) . . ? C20 N4 C18 128.5(5) . . ? N5 N4 C18 121.4(4) . . ? C19 N5 N4 102.2(4) . . ? C20 N6 C19 101.6(4) . . ? C20 N6 Zn2 127.6(3) . 1_655 ? C19 N6 Zn2 130.7(4) . 1_655 ? C21 N7 C22 102.2(4) . . ? C21 N7 Zn2 130.2(3) . . ? C22 N7 Zn2 127.5(3) . . ? C21 N8 N9 101.9(4) . . ? C22 N9 N8 110.3(4) . . ? C22 N9 C23 129.0(4) . . ? N8 N9 C23 120.6(4) . . ? C39 N10 N11 109.9(4) . . ? C39 N10 C38 129.3(4) . . ? N11 N10 C38 120.8(4) . . ? C40 N11 N10 101.8(4) . . ? C39 N12 C40 101.7(4) . . ? C39 N12 Zn2 128.1(3) . 1_656 ? C40 N12 Zn2 128.6(3) . 1_656 ? N3 C1 N1 110.4(4) . . ? N3 C1 H1A 124.8 . . ? N1 C1 H1A 124.8 . . ? N2 C2 N1 116.0(5) . . ? N2 C2 H2A 122.0 . . ? N1 C2 H2A 122.0 . . ? N3 C3 C4 112.3(4) . . ? N3 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N3 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C17 C4 C5 120.6(4) . . ? C17 C4 C3 119.4(5) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 122.7(5) . . ? C4 C5 C10 120.2(4) . . ? C6 C5 C10 117.1(5) . . ? C7 C6 C5 121.9(5) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 120.6(6) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 122.0(5) . . ? C8 C9 H9A 119.0 . . ? C10 C9 H9A 119.0 . . ? C11 C10 C9 124.0(5) . . ? C11 C10 C5 118.2(5) . . ? C9 C10 C5 117.8(5) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 C18 118.9(5) . . ? C10 C11 C18 120.0(5) . . ? C11 C12 C13 121.9(5) . . ? C11 C12 C17 120.0(5) . . ? C13 C12 C17 118.1(5) . . ? C14 C13 C12 121.6(6) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 121.9(6) . . ? C15 C16 H16A 119.1 . . ? C17 C16 H16A 119.1 . . ? C4 C17 C16 122.6(5) . . ? C4 C17 C12 119.7(5) . . ? C16 C17 C12 117.7(5) . . ? N4 C18 C11 111.2(4) . . ? N4 C18 H18A 109.4 . . ? C11 C18 H18A 109.4 . . ? N4 C18 H18B 109.4 . . ? C11 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N5 C19 N6 115.7(5) . . ? N5 C19 H19A 122.1 . . ? N6 C19 H19A 122.1 . . ? N4 C20 N6 110.4(4) . . ? N4 C20 H20A 124.8 . . ? N6 C20 H20A 124.8 . . ? N8 C21 N7 115.6(4) . . ? N8 C21 H21A 122.2 . . ? N7 C21 H21A 122.2 . . ? N9 C22 N7 110.0(4) . . ? N9 C22 H22A 125.0 . . ? N7 C22 H22A 125.0 . . ? N9 C23 C24 114.9(4) . . ? N9 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? N9 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C37 C24 C25 121.1(4) . . ? C37 C24 C23 119.7(4) . . ? C25 C24 C23 119.0(4) . . ? C26 C25 C24 122.3(4) . . ? C26 C25 C30 118.6(4) . . ? C24 C25 C30 119.1(4) . . ? C27 C26 C25 122.0(5) . . ? C27 C26 H26A 119.0 . . ? C25 C26 H26A 119.0 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C28 C29 C30 121.3(5) . . ? C28 C29 H29A 119.3 . . ? C30 C29 H29A 119.3 . . ? C29 C30 C31 122.6(4) . . ? C29 C30 C25 117.8(5) . . ? C31 C30 C25 119.6(4) . . ? C32 C31 C30 120.9(4) . . ? C32 C31 C38 120.9(4) . . ? C30 C31 C38 118.2(4) . . ? C31 C32 C33 123.1(4) . . ? C31 C32 C37 119.4(4) . . ? C33 C32 C37 117.5(4) . . ? C34 C33 C32 122.1(5) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C35 120.1(6) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C36 C35 C34 120.6(5) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 121.9(5) . . ? C35 C36 H36A 119.0 . . ? C37 C36 H36A 119.0 . . ? C24 C37 C36 122.7(4) . . ? C24 C37 C32 119.7(4) . . ? C36 C37 C32 117.6(4) . . ? N10 C38 C31 112.4(4) . . ? N10 C38 H38A 109.1 . . ? C31 C38 H38A 109.1 . . ? N10 C38 H38B 109.1 . . ? C31 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? N12 C39 N10 111.3(4) . . ? N12 C39 H39A 124.4 . . ? N10 C39 H39A 124.4 . . ? N11 C40 N12 115.3(4) . . ? N11 C40 H40A 122.3 . . ? N12 C40 H40A 122.3 . . ? O9 C41 H41A 109.5 . . ? O9 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O9 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O10 C42 H42A 109.5 . . ? O10 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O10 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 Cl1 O2 118.5(6) . . ? O1 Cl1 O3' 118.4(8) . . ? O2 Cl1 O3' 98.5(14) . . ? O1 Cl1 O4 99.2(6) . . ? O2 Cl1 O4 118.1(9) . . ? O3' Cl1 O4 104.3(12) . . ? O1 Cl1 O4' 122.0(7) . . ? O2 Cl1 O4' 118.5(9) . . ? O3' Cl1 O4' 43.0(12) . . ? O4 Cl1 O4' 61.3(9) . . ? O1 Cl1 O3 82.1(14) . . ? O2 Cl1 O3 75.9(14) . . ? O3' Cl1 O3 60.3(14) . . ? O4 Cl1 O3 161.9(19) . . ? O4' Cl1 O3 103(2) . . ? O1 Cl1 O2' 108.5(6) . . ? O2 Cl1 O2' 57.0(9) . . ? O3' Cl1 O2' 133.1(9) . . ? O4 Cl1 O2' 65.6(10) . . ? O4' Cl1 O2' 109.8(9) . . ? O3 Cl1 O2' 131.3(18) . . ? O5 Cl2 O8' 94.0(9) . . ? O5 Cl2 O6 107.9(4) . . ? O8' Cl2 O6 120.2(11) . . ? O5 Cl2 O7 107.8(5) . . ? O8' Cl2 O7 116.0(10) . . ? O6 Cl2 O7 108.9(3) . . ? O5 Cl2 O8 127.2(8) . . ? O8' Cl2 O8 33.2(7) . . ? O6 Cl2 O8 104.2(9) . . ? O7 Cl2 O8 99.7(9) . . ? O8' O8 Cl2 69.9(12) . . ? O8 O8' Cl2 76.9(13) . . ? C41 O9 Zn2 130.3(5) . . ? C41 O9 H9B 114.9 . . ? Zn2 O9 H9B 114.9 . . ? C42 O10 Zn2 130.4(4) . . ? C42 O10 H10A 114.8 . . ? Zn2 O10 H10A 114.8 . . ? H1WA O1W H1WB 99(2) . . ? Cl1 O2 O3 53.1(8) . . ? Cl1 O3 O2 51.0(8) . . ? O4' O3' Cl1 69.9(9) . . ? O3' O4' Cl1 67.2(9) . . ? 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 N6 Zn2 N1 C1 -142.8(4) 1_455 . . . ? N12 Zn2 N1 C1 -46.2(4) 1_454 . . . ? N7 Zn2 N1 C1 45.2(4) . . . . ? O10 Zn2 N1 C1 -24(25) . . . . ? O9 Zn2 N1 C1 131.1(4) . . . . ? N6 Zn2 N1 C2 39.8(4) 1_455 . . . ? N12 Zn2 N1 C2 136.4(4) 1_454 . . . ? N7 Zn2 N1 C2 -132.2(4) . . . . ? O10 Zn2 N1 C2 159(25) . . . . ? O9 Zn2 N1 C2 -46.2(4) . . . . ? C2 N2 N3 C1 0.4(5) . . . . ? C2 N2 N3 C3 178.9(4) . . . . ? C20 N4 N5 C19 -0.6(6) . . . . ? C18 N4 N5 C19 -179.6(5) . . . . ? N6 Zn2 N7 C21 175.6(9) 1_455 . . . ? N1 Zn2 N7 C21 -75.3(5) . . . . ? N12 Zn2 N7 C21 18.0(5) 1_454 . . . ? O10 Zn2 N7 C21 104.4(5) . . . . ? O9 Zn2 N7 C21 -175.2(5) . . . . ? N6 Zn2 N7 C22 -2.0(13) 1_455 . . . ? N1 Zn2 N7 C22 107.1(4) . . . . ? N12 Zn2 N7 C22 -159.6(4) 1_454 . . . ? O10 Zn2 N7 C22 -73.3(4) . . . . ? O9 Zn2 N7 C22 7.2(4) . . . . ? C21 N8 N9 C22 -0.7(5) . . . . ? C21 N8 N9 C23 175.9(4) . . . . ? C39 N10 N11 C40 1.0(5) . . . . ? C38 N10 N11 C40 -177.5(4) . . . . ? N2 N3 C1 N1 -1.1(5) . . . . ? C3 N3 C1 N1 -179.5(4) . . . . ? C2 N1 C1 N3 1.3(5) . . . . ? Zn2 N1 C1 N3 -176.7(3) . . . . ? N3 N2 C2 N1 0.5(6) . . . . ? C1 N1 C2 N2 -1.1(6) . . . . ? Zn2 N1 C2 N2 176.6(3) . . . . ? C1 N3 C3 C4 -111.4(5) . . . . ? N2 N3 C3 C4 70.3(5) . . . . ? N3 C3 C4 C17 75.9(6) . . . . ? N3 C3 C4 C5 -103.8(5) . . . . ? C17 C4 C5 C6 -179.2(5) . . . . ? C3 C4 C5 C6 0.4(7) . . . . ? C17 C4 C5 C10 1.4(7) . . . . ? C3 C4 C5 C10 -178.9(4) . . . . ? C4 C5 C6 C7 -179.5(6) . . . . ? C10 C5 C6 C7 -0.2(9) . . . . ? C5 C6 C7 C8 1.0(10) . . . . ? C6 C7 C8 C9 0.3(11) . . . . ? C7 C8 C9 C10 -2.4(10) . . . . ? C8 C9 C10 C11 -175.2(5) . . . . ? C8 C9 C10 C5 3.1(8) . . . . ? C4 C5 C10 C11 -4.0(7) . . . . ? C6 C5 C10 C11 176.6(5) . . . . ? C4 C5 C10 C9 177.6(4) . . . . ? C6 C5 C10 C9 -1.8(7) . . . . ? C9 C10 C11 C12 -178.4(5) . . . . ? C5 C10 C11 C12 3.4(7) . . . . ? C9 C10 C11 C18 1.4(7) . . . . ? C5 C10 C11 C18 -176.9(4) . . . . ? C10 C11 C12 C13 179.5(5) . . . . ? C18 C11 C12 C13 -0.3(7) . . . . ? C10 C11 C12 C17 -0.2(7) . . . . ? C18 C11 C12 C17 -179.9(4) . . . . ? C11 C12 C13 C14 -179.1(5) . . . . ? C17 C12 C13 C14 0.6(8) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C13 C14 C15 C16 -1.2(9) . . . . ? C14 C15 C16 C17 -0.5(9) . . . . ? C5 C4 C17 C16 -178.2(5) . . . . ? C3 C4 C17 C16 2.2(7) . . . . ? C5 C4 C17 C12 1.8(7) . . . . ? C3 C4 C17 C12 -177.8(4) . . . . ? C15 C16 C17 C4 -177.8(5) . . . . ? C15 C16 C17 C12 2.2(7) . . . . ? C11 C12 C17 C4 -2.5(7) . . . . ? C13 C12 C17 C4 177.8(4) . . . . ? C11 C12 C17 C16 177.5(4) . . . . ? C13 C12 C17 C16 -2.2(7) . . . . ? C20 N4 C18 C11 -125.0(6) . . . . ? N5 N4 C18 C11 53.8(7) . . . . ? C12 C11 C18 N4 75.6(6) . . . . ? C10 C11 C18 N4 -104.2(6) . . . . ? N4 N5 C19 N6 1.2(6) . . . . ? C20 N6 C19 N5 -1.3(6) . . . . ? Zn2 N6 C19 N5 173.4(4) 1_655 . . . ? N5 N4 C20 N6 -0.2(6) . . . . ? C18 N4 C20 N6 178.7(5) . . . . ? C19 N6 C20 N4 0.9(6) . . . . ? Zn2 N6 C20 N4 -174.1(3) 1_655 . . . ? N9 N8 C21 N7 0.4(6) . . . . ? C22 N7 C21 N8 0.0(6) . . . . ? Zn2 N7 C21 N8 -178.1(4) . . . . ? N8 N9 C22 N7 0.8(6) . . . . ? C23 N9 C22 N7 -175.5(4) . . . . ? C21 N7 C22 N9 -0.5(5) . . . . ? Zn2 N7 C22 N9 177.7(3) . . . . ? C22 N9 C23 C24 -104.2(6) . . . . ? N8 N9 C23 C24 79.8(5) . . . . ? N9 C23 C24 C37 -95.8(5) . . . . ? N9 C23 C24 C25 88.3(5) . . . . ? C37 C24 C25 C26 179.8(4) . . . . ? C23 C24 C25 C26 -4.4(7) . . . . ? C37 C24 C25 C30 -0.3(7) . . . . ? C23 C24 C25 C30 175.5(4) . . . . ? C24 C25 C26 C27 -179.4(5) . . . . ? C30 C25 C26 C27 0.7(8) . . . . ? C25 C26 C27 C28 0.6(9) . . . . ? C26 C27 C28 C29 -0.2(9) . . . . ? C27 C28 C29 C30 -1.4(9) . . . . ? C28 C29 C30 C31 -176.2(5) . . . . ? C28 C29 C30 C25 2.6(7) . . . . ? C26 C25 C30 C29 -2.3(7) . . . . ? C24 C25 C30 C29 177.8(4) . . . . ? C26 C25 C30 C31 176.6(4) . . . . ? C24 C25 C30 C31 -3.3(6) . . . . ? C29 C30 C31 C32 -177.5(4) . . . . ? C25 C30 C31 C32 3.7(6) . . . . ? C29 C30 C31 C38 0.4(7) . . . . ? C25 C30 C31 C38 -178.5(4) . . . . ? C30 C31 C32 C33 179.8(4) . . . . ? C38 C31 C32 C33 2.0(7) . . . . ? C30 C31 C32 C37 -0.5(7) . . . . ? C38 C31 C32 C37 -178.3(4) . . . . ? C31 C32 C33 C34 -177.0(5) . . . . ? C37 C32 C33 C34 3.4(7) . . . . ? C32 C33 C34 C35 -2.5(9) . . . . ? C33 C34 C35 C36 1.3(9) . . . . ? C34 C35 C36 C37 -1.0(9) . . . . ? C25 C24 C37 C36 -177.0(4) . . . . ? C23 C24 C37 C36 7.2(7) . . . . ? C25 C24 C37 C32 3.4(6) . . . . ? C23 C24 C37 C32 -172.3(4) . . . . ? C35 C36 C37 C24 -177.7(5) . . . . ? C35 C36 C37 C32 1.8(8) . . . . ? C31 C32 C37 C24 -3.0(6) . . . . ? C33 C32 C37 C24 176.7(4) . . . . ? C31 C32 C37 C36 177.4(4) . . . . ? C33 C32 C37 C36 -2.9(6) . . . . ? C39 N10 C38 C31 -126.9(5) . . . . ? N11 N10 C38 C31 51.2(6) . . . . ? C32 C31 C38 N10 -114.2(5) . . . . ? C30 C31 C38 N10 68.0(6) . . . . ? C40 N12 C39 N10 1.1(5) . . . . ? Zn2 N12 C39 N10 -165.2(3) 1_656 . . . ? N11 N10 C39 N12 -1.4(6) . . . . ? C38 N10 C39 N12 176.9(4) . . . . ? N10 N11 C40 N12 -0.3(6) . . . . ? C39 N12 C40 N11 -0.5(6) . . . . ? Zn2 N12 C40 N11 165.7(4) 1_656 . . . ? O5 Cl2 O8 O8' 2(4) . . . . ? O6 Cl2 O8 O8' -124(3) . . . . ? O7 Cl2 O8 O8' 123(3) . . . . ? O5 Cl2 O8' O8 -178(3) . . . . ? O6 Cl2 O8' O8 68(3) . . . . ? O7 Cl2 O8' O8 -66(3) . . . . ? N6 Zn2 O9 C41 -78.8(7) 1_455 . . . ? N1 Zn2 O9 C41 10.5(7) . . . . ? N12 Zn2 O9 C41 179.2(8) 1_454 . . . ? N7 Zn2 O9 C41 102.5(7) . . . . ? O10 Zn2 O9 C41 -169.6(7) . . . . ? N6 Zn2 O10 C42 34.4(6) 1_455 . . . ? N1 Zn2 O10 C42 -84(25) . . . . ? N12 Zn2 O10 C42 -62.2(6) 1_454 . . . ? N7 Zn2 O10 C42 -153.7(6) . . . . ? O9 Zn2 O10 C42 120.4(6) . . . . ? O1 Cl1 O2 O3 72.6(19) . . . . ? O3' Cl1 O2 O3 -56.3(15) . . . . ? O4 Cl1 O2 O3 -167.6(19) . . . . ? O4' Cl1 O2 O3 -97(2) . . . . ? O2' Cl1 O2 O3 167(2) . . . . ? O1 Cl1 O3 O2 -122.2(10) . . . . ? O3' Cl1 O3 O2 108.6(19) . . . . ? O4 Cl1 O3 O2 142(4) . . . . ? O4' Cl1 O3 O2 116.7(9) . . . . ? O2' Cl1 O3 O2 -15(2) . . . . ? O1 Cl1 O3' O4' 107.7(13) . . . . ? O2 Cl1 O3' O4' -123.2(16) . . . . ? O4 Cl1 O3' O4' -1.3(18) . . . . ? O3 Cl1 O3' O4' 168(3) . . . . ? O2' Cl1 O3' O4' -71(3) . . . . ? O1 Cl1 O4' O3' -98.7(19) . . . . ? O2 Cl1 O4' O3' 70.4(19) . . . . ? O4 Cl1 O4' O3' 179(2) . . . . ? O3 Cl1 O4' O3' -10(2) . . . . ? O2' Cl1 O4' O3' 132.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.549 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.076 #--end--- data_5 _database_code_depnum_ccdc_archive 'CCDC 630078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Cd Cl2 N12 O11' _chemical_formula_weight 1074.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.675(3) _cell_length_b 33.935(7) _cell_length_c 10.178(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.05(3) _cell_angle_gamma 90.00 _cell_volume 4437.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9913 _cell_measurement_theta_min 1.2000 _cell_measurement_theta_max 27.8764 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8633 _exptl_absorpt_correction_T_max 0.8746 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 32321 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.87 _reflns_number_total 10348 _reflns_number_gt 8439 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1925P)^2^+7.5285P] 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_number_reflns 10348 _refine_ls_number_parameters 647 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.2874 _refine_ls_wR_factor_gt 0.2696 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.03199(3) 0.127301(14) 0.45607(5) 0.0355(2) Uani 1 1 d . . . N1 N -0.0964(3) 0.08780(11) 0.3826(4) 0.0112(6) Uani 1 1 d . . . N2 N -0.2125(3) 0.04025(12) 0.3813(4) 0.0169(8) Uani 1 1 d . . . N3 N -0.2310(3) 0.05475(10) 0.2498(3) 0.0106(6) Uani 1 1 d . . . N4 N -0.8062(3) 0.08034(10) -0.1411(4) 0.0126(7) Uani 1 1 d . . . N5 N -0.8040(3) 0.04718(12) -0.2133(4) 0.0234(9) Uani 1 1 d . . . N6 N -0.9020(3) 0.09417(11) -0.3565(4) 0.0143(7) Uani 1 1 d . . . N7 N -0.0486(3) 0.16553(11) 0.5486(4) 0.0129(7) Uani 1 1 d . . . N8 N -0.1214(3) 0.21785(11) 0.6147(4) 0.0197(8) Uani 1 1 d . . . N9 N -0.1481(3) 0.18373(11) 0.6647(4) 0.0141(7) Uani 1 1 d . . . N10 N -0.7205(3) 0.20536(12) 0.4765(4) 0.0166(8) Uani 1 1 d . . . N11 N -0.7145(3) 0.21001(11) 0.6114(4) 0.0172(7) Uani 1 1 d . . . N12 N -0.8471(3) 0.16952(12) 0.4977(4) 0.0173(7) Uani 1 1 d . . . C1 C -0.1308(3) 0.06140(14) 0.4579(4) 0.0166(8) Uani 1 1 d . . . H1A H -0.1000 0.0584 0.5542 0.020 Uiso 1 1 calc R . . C2 C -0.1623(3) 0.08280(12) 0.2520(4) 0.0136(8) Uani 1 1 d . . . H2A H -0.1605 0.0968 0.1743 0.016 Uiso 1 1 calc R . . C3 C -0.3117(3) 0.03745(12) 0.1279(4) 0.0114(7) Uani 1 1 d . . . H3A H -0.3082 0.0090 0.1372 0.014 Uiso 1 1 calc R . . H3B H -0.2961 0.0442 0.0446 0.014 Uiso 1 1 calc R . . C4 C -0.4218(3) 0.05045(11) 0.1072(4) 0.0090(7) Uani 1 1 d . . . C5 C -0.4859(3) 0.02736(12) 0.1603(4) 0.0103(7) Uani 1 1 d . . . C6 C -0.4468(3) -0.00592(13) 0.2464(5) 0.0168(8) Uani 1 1 d . . . H6A H -0.3766 -0.0123 0.2713 0.020 Uiso 1 1 calc R . . C7 C -0.5103(4) -0.02900(14) 0.2940(5) 0.0235(10) Uani 1 1 d . . . H7A H -0.4828 -0.0506 0.3508 0.028 Uiso 1 1 calc R . . C8 C -0.6160(4) -0.02001(15) 0.2569(5) 0.0212(9) Uani 1 1 d . . . H8A H -0.6587 -0.0361 0.2880 0.025 Uiso 1 1 calc R . . C9 C -0.6578(3) 0.01205(13) 0.1756(5) 0.0160(8) Uani 1 1 d . . . H9A H -0.7284 0.0174 0.1525 0.019 Uiso 1 1 calc R . . C10 C -0.5948(3) 0.03766(12) 0.1252(4) 0.0096(7) Uani 1 1 d . . . C11 C -0.6346(3) 0.07151(12) 0.0438(4) 0.0106(7) Uani 1 1 d . . . C12 C -0.5691(3) 0.09555(12) -0.0036(4) 0.0107(7) Uani 1 1 d . . . C13 C -0.6060(3) 0.13027(13) -0.0827(5) 0.0160(9) Uani 1 1 d . . . H13A H -0.6745 0.1381 -0.1004 0.019 Uiso 1 1 calc R . . C14 C -0.5432(4) 0.15267(15) -0.1342(5) 0.0213(9) Uani 1 1 d . . . H14A H -0.5697 0.1750 -0.1877 0.026 Uiso 1 1 calc R . . C15 C -0.4380(4) 0.14149(15) -0.1053(5) 0.0211(9) Uani 1 1 d . . . H15A H -0.3950 0.1567 -0.1388 0.025 Uiso 1 1 calc R . . C16 C -0.3995(3) 0.10837(14) -0.0280(5) 0.0162(8) Uani 1 1 d . . . H16A H -0.3305 0.1014 -0.0105 0.019 Uiso 1 1 calc R . . C17 C -0.4615(3) 0.08456(12) 0.0258(4) 0.0105(7) Uani 1 1 d . . . C18 C -0.7473(3) 0.08331(14) 0.0095(4) 0.0163(8) Uani 1 1 d . . . H18A H -0.7792 0.0664 0.0602 0.020 Uiso 1 1 calc R . . H18B H -0.7505 0.1102 0.0400 0.020 Uiso 1 1 calc R . . C19 C -0.8630(4) 0.05665(14) -0.3424(5) 0.0237(10) Uani 1 1 d . . . H19A H -0.8767 0.0393 -0.4173 0.028 Uiso 1 1 calc R . . C20 C -0.8658(3) 0.10737(12) -0.2258(4) 0.0112(7) Uani 1 1 d . . . H20A H -0.8801 0.1321 -0.1975 0.013 Uiso 1 1 calc R . . C21 C -0.0610(3) 0.20585(13) 0.5480(5) 0.0180(9) Uani 1 1 d . . . H21A H -0.0290 0.2230 0.5039 0.022 Uiso 1 1 calc R . . C22 C -0.1037(3) 0.15303(13) 0.6255(5) 0.0159(8) Uani 1 1 d . . . H22A H -0.1104 0.1269 0.6484 0.019 Uiso 1 1 calc R . . C23 C -0.2153(3) 0.18332(15) 0.7504(5) 0.0188(9) Uani 1 1 d . . . H23A H -0.1876 0.2015 0.8277 0.023 Uiso 1 1 calc R . . H23B H -0.2143 0.1571 0.7892 0.023 Uiso 1 1 calc R . . C24 C -0.3257(3) 0.19447(13) 0.6689(4) 0.0135(8) Uani 1 1 d . . . C25 C -0.3628(3) 0.23253(13) 0.6782(4) 0.0131(8) Uani 1 1 d . . . C26 C -0.2983(4) 0.26252(14) 0.7635(5) 0.0197(9) Uani 1 1 d . . . H26A H -0.2287 0.2569 0.8122 0.024 Uiso 1 1 calc R . . C27 C -0.3357(4) 0.29925(15) 0.7758(5) 0.0235(10) Uani 1 1 d . . . H27A H -0.2918 0.3182 0.8319 0.028 Uiso 1 1 calc R . . C28 C -0.4416(4) 0.30828(15) 0.7028(5) 0.0231(10) Uani 1 1 d . . . H28A H -0.4667 0.3333 0.7103 0.028 Uiso 1 1 calc R . . C29 C -0.5072(4) 0.28046(15) 0.6212(5) 0.0223(9) Uani 1 1 d . . . H29A H -0.5772 0.2865 0.5779 0.027 Uiso 1 1 calc R . . C30 C -0.4703(3) 0.24219(13) 0.6012(4) 0.0142(8) Uani 1 1 d . . . C31 C -0.5353(3) 0.21434(14) 0.5097(5) 0.0170(8) Uani 1 1 d . . . C32 C -0.4970(3) 0.17637(14) 0.4987(5) 0.0167(8) Uani 1 1 d . . . C33 C -0.5600(4) 0.14706(16) 0.4061(5) 0.0242(10) Uani 1 1 d . . . H33A H -0.6281 0.1531 0.3513 0.029 Uiso 1 1 calc R . . C34 C -0.5214(5) 0.11033(17) 0.3973(6) 0.0316(12) Uani 1 1 d . . . H34A H -0.5639 0.0920 0.3362 0.038 Uiso 1 1 calc R . . C35 C -0.4200(5) 0.09975(15) 0.4776(6) 0.0261(11) Uani 1 1 d . . . H35A H -0.3955 0.0746 0.4699 0.031 Uiso 1 1 calc R . . C36 C -0.3559(4) 0.12682(13) 0.5688(5) 0.0199(9) Uani 1 1 d . . . H36A H -0.2887 0.1196 0.6235 0.024 Uiso 1 1 calc R . . C37 C -0.3921(3) 0.16588(13) 0.5799(4) 0.0134(8) Uani 1 1 d . . . C38 C -0.6461(4) 0.22460(17) 0.4221(5) 0.0239(10) Uani 1 1 d . . . H38A H -0.6554 0.2529 0.4223 0.029 Uiso 1 1 calc R . . H38B H -0.6596 0.2163 0.3263 0.029 Uiso 1 1 calc R . . C39 C -0.7990(4) 0.18127(16) 0.4094(5) 0.0222(10) Uani 1 1 d . . . H39A H -0.8175 0.1738 0.3161 0.027 Uiso 1 1 calc R . . C40 C -0.7924(3) 0.18830(14) 0.6191(5) 0.0175(8) Uani 1 1 d . . . H40A H -0.8086 0.1860 0.7004 0.021 Uiso 1 1 calc R . . C41 C 0.2261(5) 0.0822(2) 0.3966(10) 0.0499(19) Uani 1 1 d . . . H41A H 0.2387 0.0625 0.3366 0.075 Uiso 1 1 calc R . . H41B H 0.2561 0.0739 0.4922 0.075 Uiso 1 1 calc R . . H41C H 0.2572 0.1066 0.3841 0.075 Uiso 1 1 calc R . . C42 C -0.0789(6) 0.1852(2) 0.1866(7) 0.0423(16) Uani 1 1 d . . . H42A H -0.0920 0.1874 0.0880 0.063 Uiso 1 1 calc R . . H42B H -0.0387 0.2074 0.2342 0.063 Uiso 1 1 calc R . . H42C H -0.1439 0.1845 0.2032 0.063 Uiso 1 1 calc R . . Cl1 Cl -0.09162(9) 0.06938(4) 0.92458(13) 0.0260(3) Uani 1 1 d D . . Cl2 Cl 0.12943(9) 0.19406(3) 1.00951(12) 0.0208(3) Uani 1 1 d D . . O1 O -0.0224(2) 0.14954(10) 0.2381(3) 0.0180(6) Uani 1 1 d . . . H1B H -0.0067 0.1340 0.1727 0.022 Uiso 1 1 calc R . . O1W O 0.0303(4) 0.01657(12) 0.2611(5) 0.0390(10) Uani 1 1 d D . . H1WA H -0.022(4) 0.028(2) 0.200(7) 0.058 Uiso 1 1 d D . . H1WB H -0.003(5) 0.000(2) 0.293(8) 0.058 Uiso 1 1 d D . . O2 O 0.1165(3) 0.08753(11) 0.3621(4) 0.0242(7) Uani 1 1 d . . . H2B H 0.0749 0.0719 0.2894 0.029 Uiso 1 1 calc R . . O3 O -0.1084(7) 0.0625(2) 0.7801(5) 0.090(3) Uani 1 1 d D A 1 O4 O 0.0154(4) 0.0780(2) 0.9978(9) 0.094(3) Uani 1 1 d D A 2 O5 O -0.1186(3) 0.03444(12) 0.9827(4) 0.0318(9) Uani 1 1 d D A 1 O6 O -0.1569(4) 0.10110(15) 0.9368(5) 0.0484(13) Uani 1 1 d D A 1 O7 O 0.1151(5) 0.22612(13) 1.0893(6) 0.0522(14) Uani 1 1 d D B 1 O8 O 0.0356(7) 0.1855(6) 0.8981(13) 0.076(5) Uani 0.545(17) 1 d PD B 1 O8' O 0.0525(11) 0.1641(4) 0.985(2) 0.067(6) Uani 0.455(17) 1 d PD B 2 O9 O 0.1245(13) 0.1578(2) 1.0862(13) 0.062(5) Uani 0.545(17) 1 d PD B 1 O9' O 0.2272(9) 0.1785(5) 1.0967(13) 0.078(7) Uani 0.455(17) 1 d PD B 2 O10 O 0.2165(7) 0.1934(3) 0.9656(14) 0.050(4) Uani 0.545(17) 1 d PD B 1 O10' O 0.141(2) 0.2059(5) 0.8805(16) 0.118(10) Uani 0.455(17) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0284(3) 0.0410(3) 0.0364(3) 0.00009(17) 0.0102(2) -0.00114(16) N1 0.0059(14) 0.0165(17) 0.0101(15) -0.0005(13) 0.0014(12) -0.0002(12) N2 0.0121(16) 0.0250(19) 0.0099(16) 0.0047(14) -0.0010(13) -0.0066(14) N3 0.0053(14) 0.0154(16) 0.0083(15) 0.0005(12) -0.0012(12) 0.0004(12) N4 0.0093(15) 0.0131(16) 0.0129(16) 0.0020(13) 0.0006(13) 0.0026(12) N5 0.0204(19) 0.0177(19) 0.021(2) -0.0026(15) -0.0071(16) 0.0085(15) N6 0.0066(14) 0.0156(17) 0.0157(17) -0.0005(13) -0.0027(13) 0.0039(13) N7 0.0079(14) 0.0112(16) 0.0201(18) -0.0005(13) 0.0054(14) 0.0003(12) N8 0.0185(18) 0.0134(17) 0.029(2) 0.0037(15) 0.0101(16) 0.0010(14) N9 0.0106(15) 0.0104(16) 0.0216(18) -0.0018(13) 0.0057(14) 0.0000(12) N10 0.0091(16) 0.0236(19) 0.0160(17) 0.0077(14) 0.0028(14) -0.0054(14) N11 0.0139(17) 0.0186(18) 0.0179(18) 0.0037(14) 0.0041(14) -0.0001(14) N12 0.0117(16) 0.0231(19) 0.0169(18) 0.0016(14) 0.0046(14) -0.0034(14) C1 0.0104(18) 0.026(2) 0.0112(18) 0.0011(16) 0.0006(15) -0.0058(16) C2 0.0124(18) 0.0132(19) 0.0146(19) 0.0013(15) 0.0040(15) -0.0014(14) C3 0.0060(16) 0.0139(18) 0.0104(17) -0.0046(14) -0.0021(14) -0.0003(14) C4 0.0056(16) 0.0112(17) 0.0078(16) -0.0020(13) -0.0008(13) 0.0002(13) C5 0.0077(16) 0.0107(17) 0.0099(17) -0.0006(14) -0.0006(14) 0.0008(13) C6 0.0123(18) 0.0144(19) 0.018(2) 0.0058(16) -0.0021(16) 0.0007(15) C7 0.018(2) 0.019(2) 0.026(2) 0.0101(18) -0.0018(18) -0.0008(17) C8 0.019(2) 0.024(2) 0.019(2) 0.0029(18) 0.0050(17) -0.0098(18) C9 0.0120(18) 0.018(2) 0.017(2) -0.0019(16) 0.0038(16) -0.0037(15) C10 0.0054(16) 0.0134(18) 0.0082(16) -0.0017(14) -0.0002(13) -0.0037(13) C11 0.0040(16) 0.0163(19) 0.0102(17) -0.0006(14) 0.0007(14) 0.0031(13) C12 0.0071(16) 0.0130(18) 0.0086(17) -0.0003(14) -0.0018(14) 0.0004(14) C13 0.0112(19) 0.016(2) 0.016(2) 0.0036(16) -0.0010(16) 0.0035(14) C14 0.018(2) 0.022(2) 0.019(2) 0.0065(17) 0.0001(17) -0.0005(17) C15 0.015(2) 0.027(2) 0.020(2) 0.0110(18) 0.0042(17) 0.0010(17) C16 0.0153(19) 0.020(2) 0.0151(19) 0.0040(16) 0.0071(16) 0.0000(16) C17 0.0080(17) 0.0146(18) 0.0069(16) -0.0007(14) -0.0001(14) 0.0035(14) C18 0.0080(17) 0.030(2) 0.0097(18) -0.0006(16) 0.0009(15) 0.0024(16) C19 0.021(2) 0.021(2) 0.018(2) -0.0086(18) -0.0072(18) 0.0069(18) C20 0.0043(15) 0.0136(18) 0.0138(18) 0.0001(14) 0.0006(14) 0.0037(13) C21 0.0132(19) 0.014(2) 0.028(2) 0.0036(17) 0.0090(17) 0.0039(15) C22 0.0109(18) 0.015(2) 0.022(2) 0.0014(16) 0.0053(16) 0.0026(15) C23 0.014(2) 0.025(2) 0.016(2) 0.0009(17) 0.0041(17) 0.0078(17) C24 0.0118(18) 0.017(2) 0.0148(19) -0.0018(15) 0.0085(16) -0.0014(15) C25 0.0121(18) 0.017(2) 0.0115(18) -0.0027(15) 0.0055(15) 0.0003(15) C26 0.017(2) 0.021(2) 0.020(2) -0.0071(17) 0.0043(17) 0.0038(17) C27 0.025(2) 0.021(2) 0.025(2) -0.0090(18) 0.010(2) 0.0001(18) C28 0.026(2) 0.022(2) 0.025(2) -0.0011(18) 0.014(2) 0.0079(18) C29 0.017(2) 0.026(2) 0.026(2) 0.0036(19) 0.0110(19) 0.0044(18) C30 0.0110(18) 0.020(2) 0.0146(19) 0.0012(15) 0.0079(16) 0.0009(15) C31 0.0135(19) 0.025(2) 0.0145(19) 0.0043(17) 0.0072(16) -0.0044(16) C32 0.0135(19) 0.023(2) 0.016(2) -0.0036(16) 0.0084(16) -0.0075(16) C33 0.025(2) 0.029(3) 0.022(2) -0.0101(19) 0.013(2) -0.0123(19) C34 0.046(3) 0.029(3) 0.028(3) -0.014(2) 0.022(2) -0.018(2) C35 0.041(3) 0.018(2) 0.031(3) -0.0099(19) 0.027(2) -0.011(2) C36 0.024(2) 0.017(2) 0.024(2) -0.0048(17) 0.016(2) -0.0043(16) C37 0.0153(19) 0.0148(19) 0.0130(18) -0.0022(15) 0.0086(16) -0.0027(15) C38 0.014(2) 0.036(3) 0.020(2) 0.013(2) 0.0040(18) -0.0051(18) C39 0.013(2) 0.038(3) 0.015(2) 0.0014(18) 0.0035(17) -0.0091(18) C40 0.0110(18) 0.021(2) 0.018(2) 0.0021(17) 0.0026(16) -0.0013(15) C41 0.027(3) 0.050(4) 0.088(5) -0.027(4) 0.039(3) -0.003(3) C42 0.045(4) 0.050(4) 0.036(3) 0.023(3) 0.018(3) 0.026(3) Cl1 0.0205(6) 0.0363(7) 0.0277(6) 0.0105(5) 0.0168(5) 0.0048(5) Cl2 0.0184(5) 0.0212(5) 0.0219(5) -0.0075(4) 0.0057(4) 0.0000(4) O1 0.0143(14) 0.0215(16) 0.0176(15) 0.0051(12) 0.0048(12) 0.0001(12) O1W 0.053(3) 0.026(2) 0.028(2) -0.0062(16) -0.0003(19) 0.0021(18) O2 0.0191(16) 0.0262(18) 0.0296(18) -0.0057(14) 0.0113(14) 0.0018(13) O3 0.170(8) 0.084(5) 0.039(3) 0.023(3) 0.068(4) 0.052(5) O4 0.012(2) 0.108(6) 0.146(7) 0.065(5) 0.009(3) -0.019(3) O5 0.0305(19) 0.032(2) 0.029(2) 0.0079(16) 0.0049(16) -0.0109(16) O6 0.064(3) 0.047(3) 0.047(3) 0.022(2) 0.035(2) 0.032(2) O7 0.078(4) 0.023(2) 0.073(3) -0.027(2) 0.049(3) -0.003(2) O8 0.026(5) 0.148(15) 0.043(6) -0.037(8) -0.002(5) -0.019(6) O8' 0.040(7) 0.064(9) 0.103(17) -0.050(11) 0.034(10) -0.033(7) O9 0.131(14) 0.014(4) 0.077(8) 0.004(4) 0.082(10) 0.009(5) O9' 0.048(8) 0.102(12) 0.048(8) -0.027(7) -0.031(6) 0.063(8) O10 0.033(5) 0.042(5) 0.101(11) -0.030(6) 0.054(6) -0.011(4) O10' 0.25(3) 0.094(12) 0.043(8) 0.031(8) 0.095(14) 0.063(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N12 2.118(4) 1_655 ? Cd1 N7 2.120(4) . ? Cd1 N1 2.130(3) . ? Cd1 N6 2.130(4) 1_656 ? Cd1 O2 2.197(4) . ? Cd1 O1 2.216(3) . ? N1 C2 1.336(5) . ? N1 C1 1.364(6) . ? N2 C1 1.332(5) . ? N2 N3 1.365(5) . ? N3 C2 1.332(5) . ? N3 C3 1.471(5) . ? N4 C20 1.329(5) . ? N4 N5 1.350(5) . ? N4 C18 1.470(5) . ? N5 C19 1.325(6) . ? N6 C20 1.328(6) . ? N6 C19 1.369(6) . ? N6 Cd1 2.130(4) 1_454 ? N7 C22 1.329(6) . ? N7 C21 1.378(6) . ? N8 C21 1.301(6) . ? N8 N9 1.364(5) . ? N9 C22 1.334(6) . ? N9 C23 1.468(6) . ? N10 C39 1.336(6) . ? N10 N11 1.357(5) . ? N10 C38 1.468(6) . ? N11 C40 1.319(6) . ? N12 C39 1.343(6) . ? N12 C40 1.363(6) . ? N12 Cd1 2.118(4) 1_455 ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.513(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.413(6) . ? C4 C17 1.419(5) . ? C5 C6 1.417(6) . ? C5 C10 1.450(5) . ? C6 C7 1.374(7) . ? C6 H6A 0.9300 . ? C7 C8 1.398(7) . ? C7 H7A 0.9300 . ? C8 C9 1.367(7) . ? C8 H8A 0.9300 . ? C9 C10 1.437(6) . ? C9 H9A 0.9300 . ? C10 C11 1.412(6) . ? C11 C12 1.413(6) . ? C11 C18 1.513(5) . ? C12 C13 1.419(6) . ? C12 C17 1.446(5) . ? C13 C14 1.378(7) . ? C13 H13A 0.9300 . ? C14 C15 1.418(7) . ? C14 H14A 0.9300 . ? C15 C16 1.369(6) . ? C15 H15A 0.9300 . ? C16 C17 1.410(6) . ? C16 H16A 0.9300 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.501(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.402(6) . ? C24 C37 1.422(6) . ? C25 C26 1.429(6) . ? C25 C30 1.447(6) . ? C26 C27 1.369(7) . ? C26 H26A 0.9300 . ? C27 C28 1.415(7) . ? C27 H27A 0.9300 . ? C28 C29 1.369(7) . ? C28 H28A 0.9300 . ? C29 C30 1.433(7) . ? C29 H29A 0.9300 . ? C30 C31 1.408(6) . ? C31 C32 1.410(7) . ? C31 C38 1.512(6) . ? C32 C37 1.434(6) . ? C32 C33 1.436(6) . ? C33 C34 1.369(9) . ? C33 H33A 0.9300 . ? C34 C35 1.394(9) . ? C34 H34A 0.9300 . ? C35 C36 1.384(7) . ? C35 H35A 0.9300 . ? C36 C37 1.433(6) . ? C36 H36A 0.9300 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 O2 1.429(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 O1 1.434(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cl1 O4 1.427(5) . ? Cl1 O3 1.428(5) . ? Cl1 O5 1.429(4) . ? Cl1 O6 1.431(4) . ? Cl2 O10 1.409(6) . ? Cl2 O7 1.411(4) . ? Cl2 O8 1.421(7) . ? Cl2 O8' 1.421(8) . ? Cl2 O9' 1.429(7) . ? Cl2 O10' 1.434(8) . ? Cl2 O9 1.472(7) . ? O1 H1B 0.9300 . ? O1W H1WA 0.854(10) . ? O1W H1WB 0.853(10) . ? O2 H2B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Cd1 N7 89.21(15) 1_655 . ? N12 Cd1 N1 171.42(14) 1_655 . ? N7 Cd1 N1 92.85(14) . . ? N12 Cd1 N6 96.64(14) 1_655 1_656 ? N7 Cd1 N6 92.89(14) . 1_656 ? N1 Cd1 N6 91.58(14) . 1_656 ? N12 Cd1 O2 90.67(15) 1_655 . ? N7 Cd1 O2 179.47(14) . . ? N1 Cd1 O2 87.35(13) . . ? N6 Cd1 O2 86.61(14) 1_656 . ? N12 Cd1 O1 86.61(13) 1_655 . ? N7 Cd1 O1 100.89(13) . . ? N1 Cd1 O1 84.82(13) . . ? N6 Cd1 O1 165.89(14) 1_656 . ? O2 Cd1 O1 79.61(13) . . ? C2 N1 C1 103.3(3) . . ? C2 N1 Cd1 128.5(3) . . ? C1 N1 Cd1 128.2(3) . . ? C1 N2 N3 102.5(3) . . ? C2 N3 N2 110.4(3) . . ? C2 N3 C3 128.3(4) . . ? N2 N3 C3 121.1(3) . . ? C20 N4 N5 110.2(3) . . ? C20 N4 C18 128.6(4) . . ? N5 N4 C18 121.2(3) . . ? C19 N5 N4 102.6(4) . . ? C20 N6 C19 102.2(4) . . ? C20 N6 Cd1 128.1(3) . 1_454 ? C19 N6 Cd1 127.9(3) . 1_454 ? C22 N7 C21 103.0(4) . . ? C22 N7 Cd1 123.5(3) . . ? C21 N7 Cd1 133.4(3) . . ? C21 N8 N9 103.2(4) . . ? C22 N9 N8 110.1(4) . . ? C22 N9 C23 127.8(4) . . ? N8 N9 C23 122.2(4) . . ? C39 N10 N11 110.4(4) . . ? C39 N10 C38 128.2(4) . . ? N11 N10 C38 121.4(4) . . ? C40 N11 N10 103.0(4) . . ? C39 N12 C40 103.0(4) . . ? C39 N12 Cd1 126.5(3) . 1_455 ? C40 N12 Cd1 130.2(3) . 1_455 ? N2 C1 N1 114.0(4) . . ? N2 C1 H1A 123.0 . . ? N1 C1 H1A 123.0 . . ? N3 C2 N1 109.8(4) . . ? N3 C2 H2A 125.1 . . ? N1 C2 H2A 125.1 . . ? N3 C3 C4 115.1(3) . . ? N3 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N3 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C17 120.8(4) . . ? C5 C4 C3 120.2(3) . . ? C17 C4 C3 118.8(4) . . ? C4 C5 C6 121.8(4) . . ? C4 C5 C10 119.4(4) . . ? C6 C5 C10 118.8(4) . . ? C7 C6 C5 121.5(4) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 120.0(4) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 121.3(4) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 122.9(4) . . ? C11 C10 C5 119.9(4) . . ? C9 C10 C5 117.2(4) . . ? C10 C11 C12 120.5(3) . . ? C10 C11 C18 120.6(4) . . ? C12 C11 C18 118.9(4) . . ? C11 C12 C13 122.0(4) . . ? C11 C12 C17 120.0(4) . . ? C13 C12 C17 118.0(4) . . ? C14 C13 C12 121.9(4) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 119.6(4) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 122.0(4) . . ? C15 C16 H16A 119.0 . . ? C17 C16 H16A 119.0 . . ? C16 C17 C4 122.2(4) . . ? C16 C17 C12 118.4(4) . . ? C4 C17 C12 119.3(4) . . ? N4 C18 C11 111.9(3) . . ? N4 C18 H18A 109.2 . . ? C11 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C11 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N5 C19 N6 114.3(4) . . ? N5 C19 H19A 122.8 . . ? N6 C19 H19A 122.8 . . ? N6 C20 N4 110.6(4) . . ? N6 C20 H20A 124.7 . . ? N4 C20 H20A 124.7 . . ? N8 C21 N7 114.1(4) . . ? N8 C21 H21A 123.0 . . ? N7 C21 H21A 123.0 . . ? N7 C22 N9 109.6(4) . . ? N7 C22 H22A 125.2 . . ? N9 C22 H22A 125.2 . . ? N9 C23 C24 112.7(4) . . ? N9 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N9 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C37 120.3(4) . . ? C25 C24 C23 120.9(4) . . ? C37 C24 C23 118.8(4) . . ? C24 C25 C26 122.3(4) . . ? C24 C25 C30 119.7(4) . . ? C26 C25 C30 117.9(4) . . ? C27 C26 C25 122.1(4) . . ? C27 C26 H26A 118.9 . . ? C25 C26 H26A 118.9 . . ? C26 C27 C28 119.7(5) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 121.4(4) . . ? C28 C29 H29A 119.3 . . ? C30 C29 H29A 119.3 . . ? C31 C30 C29 121.9(4) . . ? C31 C30 C25 120.0(4) . . ? C29 C30 C25 118.1(4) . . ? C30 C31 C32 119.9(4) . . ? C30 C31 C38 120.9(4) . . ? C32 C31 C38 119.2(4) . . ? C31 C32 C37 120.4(4) . . ? C31 C32 C33 122.0(4) . . ? C37 C32 C33 117.6(4) . . ? C34 C33 C32 121.0(5) . . ? C34 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C33 C34 C35 121.7(5) . . ? C33 C34 H34A 119.2 . . ? C35 C34 H34A 119.2 . . ? C36 C35 C34 119.8(5) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C35 C36 C37 120.7(5) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? C24 C37 C36 121.3(4) . . ? C24 C37 C32 119.5(4) . . ? C36 C37 C32 119.2(4) . . ? N10 C38 C31 111.0(4) . . ? N10 C38 H38A 109.4 . . ? C31 C38 H38A 109.4 . . ? N10 C38 H38B 109.4 . . ? C31 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? N10 C39 N12 109.4(4) . . ? N10 C39 H39A 125.3 . . ? N12 C39 H39A 125.3 . . ? N11 C40 N12 114.3(4) . . ? N11 C40 H40A 122.9 . . ? N12 C40 H40A 122.9 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O1 C42 H42A 109.5 . . ? O1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 Cl1 O3 110.2(6) . . ? O4 Cl1 O5 108.5(3) . . ? O3 Cl1 O5 108.5(4) . . ? O4 Cl1 O6 111.1(5) . . ? O3 Cl1 O6 109.1(3) . . ? O5 Cl1 O6 109.4(3) . . ? O10 Cl2 O7 119.7(4) . . ? O10 Cl2 O8 112.0(7) . . ? O7 Cl2 O8 110.6(7) . . ? O10 Cl2 O8' 126.0(6) . . ? O7 Cl2 O8' 114.3(6) . . ? O8 Cl2 O8' 45.7(10) . . ? O10 Cl2 O9' 58.6(9) . . ? O7 Cl2 O9' 102.3(6) . . ? O8 Cl2 O9' 144.7(10) . . ? O8' Cl2 O9' 108.9(12) . . ? O10 Cl2 O10' 48.7(11) . . ? O7 Cl2 O10' 113.2(8) . . ? O8 Cl2 O10' 71.4(13) . . ? O8' Cl2 O10' 110.3(14) . . ? O9' Cl2 O10' 107.3(14) . . ? O10 Cl2 O9 110.6(7) . . ? O7 Cl2 O9 107.4(4) . . ? O8 Cl2 O9 93.3(12) . . ? O8' Cl2 O9 48.0(10) . . ? O9' Cl2 O9 64.2(10) . . ? O10' Cl2 O9 139.4(8) . . ? C42 O1 Cd1 127.4(3) . . ? C42 O1 H1B 116.3 . . ? Cd1 O1 H1B 116.3 . . ? H1WA O1W H1WB 98(2) . . ? C41 O2 Cd1 129.4(4) . . ? C41 O2 H2B 115.3 . . ? Cd1 O2 H2B 115.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Cd1 N1 C2 2.1(12) 1_655 . . . ? N7 Cd1 N1 C2 105.8(4) . . . . ? N6 Cd1 N1 C2 -161.3(4) 1_656 . . . ? O2 Cd1 N1 C2 -74.7(4) . . . . ? O1 Cd1 N1 C2 5.1(4) . . . . ? N12 Cd1 N1 C1 -178(20) 1_655 . . . ? N7 Cd1 N1 C1 -74.4(4) . . . . ? N6 Cd1 N1 C1 18.5(4) 1_656 . . . ? O2 Cd1 N1 C1 105.1(4) . . . . ? O1 Cd1 N1 C1 -175.1(4) . . . . ? C1 N2 N3 C2 0.3(5) . . . . ? C1 N2 N3 C3 175.5(4) . . . . ? C20 N4 N5 C19 1.1(5) . . . . ? C18 N4 N5 C19 -178.3(4) . . . . ? N12 Cd1 N7 C22 -143.2(3) 1_655 . . . ? N1 Cd1 N7 C22 45.1(3) . . . . ? N6 Cd1 N7 C22 -46.6(3) 1_656 . . . ? O2 Cd1 N7 C22 -67(15) . . . . ? O1 Cd1 N7 C22 130.4(3) . . . . ? N12 Cd1 N7 C21 37.7(4) 1_655 . . . ? N1 Cd1 N7 C21 -134.0(4) . . . . ? N6 Cd1 N7 C21 134.3(4) 1_656 . . . ? O2 Cd1 N7 C21 114(15) . . . . ? O1 Cd1 N7 C21 -48.7(4) . . . . ? C21 N8 N9 C22 -0.5(5) . . . . ? C21 N8 N9 C23 178.8(4) . . . . ? C39 N10 N11 C40 -0.7(5) . . . . ? C38 N10 N11 C40 -179.4(4) . . . . ? N3 N2 C1 N1 -0.8(5) . . . . ? C2 N1 C1 N2 0.9(5) . . . . ? Cd1 N1 C1 N2 -178.9(3) . . . . ? N2 N3 C2 N1 0.3(5) . . . . ? C3 N3 C2 N1 -174.5(4) . . . . ? C1 N1 C2 N3 -0.7(5) . . . . ? Cd1 N1 C2 N3 179.1(3) . . . . ? C2 N3 C3 C4 -105.8(5) . . . . ? N2 N3 C3 C4 79.8(5) . . . . ? N3 C3 C4 C5 -95.1(4) . . . . ? N3 C3 C4 C17 89.2(5) . . . . ? C17 C4 C5 C6 -177.5(4) . . . . ? C3 C4 C5 C6 6.9(6) . . . . ? C17 C4 C5 C10 3.0(6) . . . . ? C3 C4 C5 C10 -172.6(3) . . . . ? C4 C5 C6 C7 -177.9(4) . . . . ? C10 C5 C6 C7 1.6(7) . . . . ? C5 C6 C7 C8 0.4(8) . . . . ? C6 C7 C8 C9 -1.3(8) . . . . ? C7 C8 C9 C10 0.1(7) . . . . ? C8 C9 C10 C11 -178.5(4) . . . . ? C8 C9 C10 C5 1.9(6) . . . . ? C4 C5 C10 C11 -2.8(6) . . . . ? C6 C5 C10 C11 177.7(4) . . . . ? C4 C5 C10 C9 176.8(4) . . . . ? C6 C5 C10 C9 -2.7(6) . . . . ? C9 C10 C11 C12 -179.7(4) . . . . ? C5 C10 C11 C12 -0.2(6) . . . . ? C9 C10 C11 C18 2.1(6) . . . . ? C5 C10 C11 C18 -178.3(4) . . . . ? C10 C11 C12 C13 -178.5(4) . . . . ? C18 C11 C12 C13 -0.3(6) . . . . ? C10 C11 C12 C17 2.9(6) . . . . ? C18 C11 C12 C17 -178.9(4) . . . . ? C11 C12 C13 C14 -177.0(4) . . . . ? C17 C12 C13 C14 1.7(6) . . . . ? C12 C13 C14 C15 -1.5(7) . . . . ? C13 C14 C15 C16 0.8(8) . . . . ? C14 C15 C16 C17 -0.4(8) . . . . ? C15 C16 C17 C4 -179.3(4) . . . . ? C15 C16 C17 C12 0.7(7) . . . . ? C5 C4 C17 C16 179.6(4) . . . . ? C3 C4 C17 C16 -4.7(6) . . . . ? C5 C4 C17 C12 -0.4(6) . . . . ? C3 C4 C17 C12 175.3(3) . . . . ? C11 C12 C17 C16 177.4(4) . . . . ? C13 C12 C17 C16 -1.3(6) . . . . ? C11 C12 C17 C4 -2.6(6) . . . . ? C13 C12 C17 C4 178.7(4) . . . . ? C20 N4 C18 C11 -128.3(5) . . . . ? N5 N4 C18 C11 51.0(6) . . . . ? C10 C11 C18 N4 -114.4(4) . . . . ? C12 C11 C18 N4 67.4(5) . . . . ? N4 N5 C19 N6 0.4(6) . . . . ? C20 N6 C19 N5 -1.7(6) . . . . ? Cd1 N6 C19 N5 163.9(4) 1_454 . . . ? C19 N6 C20 N4 2.3(5) . . . . ? Cd1 N6 C20 N4 -163.2(3) 1_454 . . . ? N5 N4 C20 N6 -2.3(5) . . . . ? C18 N4 C20 N6 177.1(4) . . . . ? N9 N8 C21 N7 1.5(5) . . . . ? C22 N7 C21 N8 -2.0(5) . . . . ? Cd1 N7 C21 N8 177.3(3) . . . . ? C21 N7 C22 N9 1.6(5) . . . . ? Cd1 N7 C22 N9 -177.8(3) . . . . ? N8 N9 C22 N7 -0.7(5) . . . . ? C23 N9 C22 N7 -180.0(4) . . . . ? C22 N9 C23 C24 -111.7(5) . . . . ? N8 N9 C23 C24 69.1(5) . . . . ? N9 C23 C24 C25 -100.7(5) . . . . ? N9 C23 C24 C37 78.2(5) . . . . ? C37 C24 C25 C26 -178.4(4) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C37 C24 C25 C30 2.6(6) . . . . ? C23 C24 C25 C30 -178.5(4) . . . . ? C24 C25 C26 C27 -177.8(5) . . . . ? C30 C25 C26 C27 1.2(7) . . . . ? C25 C26 C27 C28 0.2(8) . . . . ? C26 C27 C28 C29 0.8(8) . . . . ? C27 C28 C29 C30 -3.2(8) . . . . ? C28 C29 C30 C31 -175.4(5) . . . . ? C28 C29 C30 C25 4.6(7) . . . . ? C24 C25 C30 C31 -4.5(6) . . . . ? C26 C25 C30 C31 176.5(4) . . . . ? C24 C25 C30 C29 175.6(4) . . . . ? C26 C25 C30 C29 -3.5(6) . . . . ? C29 C30 C31 C32 -176.9(4) . . . . ? C25 C30 C31 C32 3.2(6) . . . . ? C29 C30 C31 C38 3.4(7) . . . . ? C25 C30 C31 C38 -176.5(4) . . . . ? C30 C31 C32 C37 0.0(6) . . . . ? C38 C31 C32 C37 179.7(4) . . . . ? C30 C31 C32 C33 -179.5(4) . . . . ? C38 C31 C32 C33 0.2(7) . . . . ? C31 C32 C33 C34 -179.8(5) . . . . ? C37 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 C35 0.3(8) . . . . ? C33 C34 C35 C36 -0.1(8) . . . . ? C34 C35 C36 C37 -1.1(7) . . . . ? C25 C24 C37 C36 -180.0(4) . . . . ? C23 C24 C37 C36 1.1(6) . . . . ? C25 C24 C37 C32 0.5(6) . . . . ? C23 C24 C37 C32 -178.4(4) . . . . ? C35 C36 C37 C24 -177.4(4) . . . . ? C35 C36 C37 C32 2.1(7) . . . . ? C31 C32 C37 C24 -1.9(6) . . . . ? C33 C32 C37 C24 177.6(4) . . . . ? C31 C32 C37 C36 178.6(4) . . . . ? C33 C32 C37 C36 -1.9(6) . . . . ? C39 N10 C38 C31 -123.6(5) . . . . ? N11 N10 C38 C31 54.9(6) . . . . ? C30 C31 C38 N10 -106.5(5) . . . . ? C32 C31 C38 N10 73.8(6) . . . . ? N11 N10 C39 N12 0.2(6) . . . . ? C38 N10 C39 N12 178.9(4) . . . . ? C40 N12 C39 N10 0.3(5) . . . . ? Cd1 N12 C39 N10 -174.1(3) 1_455 . . . ? N10 N11 C40 N12 0.9(5) . . . . ? C39 N12 C40 N11 -0.8(5) . . . . ? Cd1 N12 C40 N11 173.3(3) 1_455 . . . ? N12 Cd1 O1 C42 -77.3(5) 1_655 . . . ? N7 Cd1 O1 C42 11.3(5) . . . . ? N1 Cd1 O1 C42 103.2(5) . . . . ? N6 Cd1 O1 C42 178.9(6) 1_656 . . . ? O2 Cd1 O1 C42 -168.6(5) . . . . ? N12 Cd1 O2 C41 32.4(6) 1_655 . . . ? N7 Cd1 O2 C41 -44(16) . . . . ? N1 Cd1 O2 C41 -155.9(6) . . . . ? N6 Cd1 O2 C41 -64.2(6) 1_656 . . . ? O1 Cd1 O2 C41 118.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.844 _refine_diff_density_min -2.687 _refine_diff_density_rms 0.212 #--end--- ##END data_6 _database_code_depnum_ccdc_archive 'CCDC 630079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Br2 Hg N6' _chemical_formula_weight 700.78 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.236(5) _cell_length_b 5.1343(10) _cell_length_c 15.771(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.68(3) _cell_angle_gamma 90.00 _cell_volume 1955.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8688 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 30.00 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 11.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.242 _exptl_absorpt_correction_T_max 0.305 _exptl_absorpt_process_details ? _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3053 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1702 _reflns_number_gt 1648 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+6.3883P] 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 0.00282(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1702 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.0000 1.47685(5) 0.2500 0.01109(14) Uani 1 2 d S . . Br1 Br -0.034157(19) 1.59044(11) 0.38960(3) 0.01782(17) Uani 1 1 d . . . N1 N 0.06546(15) 1.1607(8) 0.3066(2) 0.0127(8) Uani 1 1 d . . . N2 N 0.11043(14) 0.8677(8) 0.3840(2) 0.0108(8) Uani 1 1 d . . . N3 N 0.13081(15) 0.8511(8) 0.3059(2) 0.0136(8) Uani 1 1 d . . . C1 C 0.07175(19) 1.0545(10) 0.3829(3) 0.0126(9) Uani 1 1 d . . . H1A H 0.0523 1.1019 0.4290 0.015 Uiso 1 1 calc R . . C2 C 0.1023(2) 1.0330(10) 0.2625(3) 0.0158(10) Uani 1 1 d . . . H2A H 0.1073 1.0702 0.2059 0.019 Uiso 1 1 calc R . . C3 C 0.13121(17) 0.6949(9) 0.4523(3) 0.0114(9) Uani 1 1 d . . . H3A H 0.1237 0.5161 0.4351 0.014 Uiso 1 1 calc R . . H3B H 0.1114 0.7292 0.5021 0.014 Uiso 1 1 calc R . . C4 C 0.19284(17) 0.7258(9) 0.4757(3) 0.0083(8) Uani 1 1 d . . . C5 C 0.23070(19) 0.5629(9) 0.4385(3) 0.0103(9) Uani 1 1 d . . . C6 C 0.21350(18) 0.3759(9) 0.3751(3) 0.0117(9) Uani 1 1 d . . . H6A H 0.1762 0.3636 0.3564 0.014 Uiso 1 1 calc R . . C7 C 0.25063(19) 0.2142(9) 0.3413(3) 0.0128(9) Uani 1 1 d . . . H7A H 0.2384 0.0924 0.3004 0.015 Uiso 1 1 calc R . . C8 C 0.30723(19) 0.2312(9) 0.3680(3) 0.0146(9) Uani 1 1 d . . . H8A H 0.3323 0.1183 0.3456 0.018 Uiso 1 1 calc R . . C9 C 0.32547(18) 0.4118(9) 0.4266(3) 0.0105(9) Uani 1 1 d . . . H9A H 0.3631 0.4222 0.4429 0.013 Uiso 1 1 calc R . . C10 C 0.21151(18) 0.9140(9) 0.5363(3) 0.0087(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.00737(18) 0.01460(19) 0.01108(18) 0.000 -0.00062(10) 0.000 Br1 0.0142(3) 0.0255(3) 0.0142(3) -0.0006(2) 0.00396(17) 0.0023(2) N1 0.0063(17) 0.017(2) 0.0137(17) -0.0018(16) -0.0047(14) 0.0014(16) N2 0.0040(17) 0.018(2) 0.0101(17) -0.0024(16) 0.0007(13) -0.0008(16) N3 0.0094(18) 0.021(2) 0.0102(17) -0.0024(16) 0.0006(14) 0.0022(17) C1 0.005(2) 0.016(2) 0.016(2) -0.001(2) -0.0001(17) -0.0003(18) C2 0.015(3) 0.021(3) 0.011(2) -0.0025(19) -0.0006(19) 0.004(2) C3 0.006(2) 0.016(2) 0.012(2) -0.0010(18) 0.0013(16) -0.0008(17) C4 0.0046(19) 0.008(2) 0.0130(19) 0.0047(17) 0.0023(15) -0.0012(16) C5 0.011(2) 0.011(2) 0.009(2) 0.0068(18) 0.0017(16) 0.0001(18) C6 0.012(2) 0.011(2) 0.012(2) -0.0015(18) 0.0023(16) -0.0029(18) C7 0.016(2) 0.011(2) 0.012(2) 0.0005(18) 0.0005(17) -0.0037(18) C8 0.016(2) 0.013(2) 0.016(2) 0.0019(19) 0.0081(17) 0.0055(19) C9 0.009(2) 0.012(2) 0.011(2) 0.0056(18) 0.0032(16) 0.0011(18) C10 0.008(2) 0.009(2) 0.0092(19) 0.0039(18) 0.0024(15) -0.0014(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.391(4) 2 ? Hg1 N1 2.391(4) . ? Hg1 Br1 2.4839(7) . ? Hg1 Br1 2.4839(7) 2 ? N1 C1 1.319(6) . ? N1 C2 1.347(7) . ? N2 C1 1.340(6) . ? N2 N3 1.367(5) . ? N2 C3 1.453(6) . ? N3 C2 1.319(7) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.517(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.405(6) . ? C4 C10 1.407(6) . ? C5 C6 1.424(7) . ? C5 C10 1.429(6) 7_566 ? C6 C7 1.364(6) . ? C6 H6A 0.9300 . ? C7 C8 1.405(6) . ? C7 H7A 0.9300 . ? C8 C9 1.357(7) . ? C8 H8A 0.9300 . ? C9 C10 1.426(7) 7_566 ? C9 H9A 0.9300 . ? C10 C9 1.426(7) 7_566 ? C10 C5 1.429(6) 7_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N1 94.51(19) 2 . ? N1 Hg1 Br1 103.38(9) 2 . ? N1 Hg1 Br1 95.01(9) . . ? N1 Hg1 Br1 95.01(9) 2 2 ? N1 Hg1 Br1 103.38(9) . 2 ? Br1 Hg1 Br1 152.84(3) . 2 ? C1 N1 C2 103.8(4) . . ? C1 N1 Hg1 130.2(3) . . ? C2 N1 Hg1 125.8(3) . . ? C1 N2 N3 109.7(4) . . ? C1 N2 C3 130.3(4) . . ? N3 N2 C3 120.0(4) . . ? C2 N3 N2 102.2(4) . . ? N1 C1 N2 109.7(4) . . ? N1 C1 H1A 125.2 . . ? N2 C1 H1A 125.2 . . ? N3 C2 N1 114.7(4) . . ? N3 C2 H2A 122.6 . . ? N1 C2 H2A 122.6 . . ? N2 C3 C4 113.0(4) . . ? N2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C10 120.5(4) . . ? C5 C4 C3 120.0(4) . . ? C10 C4 C3 119.5(4) . . ? C4 C5 C6 122.1(4) . . ? C4 C5 C10 119.5(4) . 7_566 ? C6 C5 C10 118.4(4) . 7_566 ? C7 C6 C5 121.3(4) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 121.9(4) . 7_566 ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 7_566 . ? C4 C10 C9 122.1(4) . 7_566 ? C4 C10 C5 120.0(4) . 7_566 ? C9 C10 C5 117.9(4) 7_566 7_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Hg1 N1 C1 -92.5(4) 2 . . . ? Br1 Hg1 N1 C1 11.4(4) . . . . ? Br1 Hg1 N1 C1 171.3(4) 2 . . . ? N1 Hg1 N1 C2 81.3(4) 2 . . . ? Br1 Hg1 N1 C2 -174.8(4) . . . . ? Br1 Hg1 N1 C2 -14.9(4) 2 . . . ? C1 N2 N3 C2 0.0(5) . . . . ? C3 N2 N3 C2 179.7(4) . . . . ? C2 N1 C1 N2 -0.8(5) . . . . ? Hg1 N1 C1 N2 174.1(3) . . . . ? N3 N2 C1 N1 0.5(5) . . . . ? C3 N2 C1 N1 -179.1(4) . . . . ? N2 N3 C2 N1 -0.5(5) . . . . ? C1 N1 C2 N3 0.9(6) . . . . ? Hg1 N1 C2 N3 -174.3(3) . . . . ? C1 N2 C3 C4 -119.8(5) . . . . ? N3 N2 C3 C4 60.6(5) . . . . ? N2 C3 C4 C5 -94.2(5) . . . . ? N2 C3 C4 C10 87.4(5) . . . . ? C10 C4 C5 C6 -178.1(4) . . . . ? C3 C4 C5 C6 3.5(6) . . . . ? C10 C4 C5 C10 1.2(7) . . . 7_566 ? C3 C4 C5 C10 -177.3(4) . . . 7_566 ? C4 C5 C6 C7 -178.2(4) . . . . ? C10 C5 C6 C7 2.6(7) 7_566 . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? C6 C7 C8 C9 -1.2(7) . . . . ? C7 C8 C9 C10 1.0(7) . . . 7_566 ? C5 C4 C10 C9 178.0(4) . . . 7_566 ? C3 C4 C10 C9 -3.6(6) . . . 7_566 ? C5 C4 C10 C5 -1.2(7) . . . 7_566 ? C3 C4 C10 C5 177.3(4) . . . 7_566 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.230 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.180