#------------------------------------------------------------------------------ #$Date: 2016-03-21 17:08:22 +0200 (Mon, 21 Mar 2016) $ #$Revision: 178770 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/10/24/4102440.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4102440 loop_ _publ_author_name 'Qi-Kui Liu' 'Jian-Ping Ma' 'Yu-Bin Dong' _publ_section_title ; Adsorption and Separation of Reactive Aromatic Isomers and Generation and Stabilization of Their Radicals within Cadmium(II)-Triazole Metal-Organic Confined Space in a Single-Crystal-to-Single-Crystal Fashion ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7005 _journal_page_last 7017 _journal_paper_doi 10.1021/ja101807c _journal_volume 132 _journal_year 2010 _chemical_formula_sum 'C58 H44 Cd Cl2 N12 O10 S2' _chemical_formula_weight 1316.47 _chemical_name_systematic ; ? ; _space_group_IT_number 92 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_space_group_name_H-M 'P 41 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.8440(10) _cell_length_b 15.8440(10) _cell_length_c 21.837(3) _cell_measurement_reflns_used 3743 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 20.235 _cell_measurement_theta_min 2.265 _cell_volume 5481.8(9) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 28655 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 1.59 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_correction_T_min 0.9037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2680 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.190 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.102 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 390 _refine_ls_number_reflns 5110 _refine_ls_number_restraints 27 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0584 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+6.8100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1425 _refine_ls_wR_factor_ref 0.1512 _reflns_number_gt 4351 _reflns_number_total 5110 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja101807c_si_003_07.cif _cod_data_source_block 4' _cod_original_cell_volume 5481.7(9) _cod_database_code 4102440 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' 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 C1 C 0.9151(4) 0.1405(4) 0.8896(3) 0.0295(14) Uani 1 1 d . H1 H 0.9639 0.1114 0.9003 0.035 Uiso 1 1 calc R C2 C 0.8863(4) 0.2015(4) 0.9287(3) 0.0300(14) Uani 1 1 d . H2 H 0.9160 0.2135 0.9644 0.036 Uiso 1 1 calc R C3 C 0.8116(4) 0.2463(4) 0.9151(3) 0.0286(14) Uani 1 1 d . C4 C 0.7681(4) 0.2179(4) 0.8636(3) 0.0363(15) Uani 1 1 d . H4 H 0.7153 0.2403 0.8544 0.044 Uiso 1 1 calc R C5 C 0.8024(4) 0.1572(4) 0.8261(3) 0.0373(17) Uani 1 1 d . H5 H 0.7725 0.1408 0.7914 0.045 Uiso 1 1 calc R C6 C 0.7808(4) 0.3187(4) 0.9527(3) 0.0281(14) Uani 1 1 d . C7 C 0.8079(4) 0.3327(4) 1.0118(3) 0.0342(16) Uani 1 1 d . H7 H 0.8475 0.2967 1.0294 0.041 Uiso 1 1 calc R C8 C 0.7769(5) 0.3993(5) 1.0448(3) 0.0402(18) Uani 1 1 d . H8 H 0.7952 0.4074 1.0848 0.048 Uiso 1 1 calc R C9 C 0.7189(4) 0.4548(5) 1.0199(3) 0.0344(16) Uani 1 1 d . H9 H 0.6993 0.5005 1.0425 0.041 Uiso 1 1 calc R C10 C 0.6900(4) 0.4406(4) 0.9599(3) 0.0281(13) Uani 1 1 d . C11 C 0.7221(4) 0.3733(4) 0.9271(3) 0.0296(14) Uani 1 1 d . H11 H 0.7041 0.3645 0.8871 0.036 Uiso 1 1 calc R C12 C 0.6275(4) 0.4962(4) 0.9303(3) 0.0264(13) Uani 1 1 d . C13 C 0.5763(3) 0.5916(4) 0.8678(2) 0.0239(12) Uani 1 1 d . C14 C 0.5685(4) 0.6607(4) 0.8240(3) 0.0304(14) Uani 1 1 d . C15 C 0.4970(5) 0.6617(5) 0.7872(3) 0.0405(17) Uani 1 1 d . H15 H 0.4569 0.6191 0.7903 0.049 Uiso 1 1 calc R C16 C 0.4861(4) 0.7277(5) 0.7453(4) 0.0479(18) Uani 1 1 d . H16 H 0.4385 0.7288 0.7204 0.058 Uiso 1 1 calc R C17 C 0.5454(4) 0.7906(5) 0.7407(3) 0.0444(18) Uani 1 1 d . H17 H 0.5384 0.8335 0.7121 0.053 Uiso 1 1 calc R C18 C 0.6156(4) 0.7905(4) 0.7787(3) 0.0317(15) Uani 1 1 d . C19 C 0.6267(4) 0.7249(4) 0.8196(3) 0.0279(14) Uani 1 1 d . H19 H 0.6742 0.7241 0.8446 0.033 Uiso 1 1 calc R C20 C 0.6823(4) 0.8580(4) 0.7723(3) 0.0275(14) Uani 1 1 d . C21 C 0.6927(5) 0.9032(4) 0.7189(3) 0.0373(16) Uani 1 1 d . H21 H 0.6552 0.8958 0.6865 0.045 Uiso 1 1 calc R C22 C 0.7591(5) 0.9595(5) 0.7137(3) 0.0378(17) Uani 1 1 d . H22 H 0.7660 0.9878 0.6767 0.045 Uiso 1 1 calc R C23 C 0.8011(4) 0.9335(5) 0.8112(3) 0.0355(15) Uani 1 1 d . H23 H 0.8373 0.9445 0.8437 0.043 Uiso 1 1 calc R C24 C 0.7383(4) 0.8758(4) 0.8197(3) 0.0351(16) Uani 1 1 d . H24 H 0.7330 0.8483 0.8572 0.042 Uiso 1 1 calc R C25 C 0.5853(7) 0.1296(9) 0.7309(7) 0.296(12) Uani 1 1 d DU H25 H 0.6241 0.1735 0.7331 0.355 Uiso 1 1 calc R C26 C 0.5692(9) 0.0948(9) 0.6760(8) 0.278(12) Uani 1 1 d DU H26 H 0.5929 0.1099 0.6386 0.333 Uiso 1 1 calc R C27 C 0.5047(9) 0.0261(8) 0.6872(7) 0.213(7) Uani 1 1 d DU H27 H 0.4808 -0.0097 0.6583 0.255 Uiso 1 1 calc R C28 C 0.4891(6) 0.0275(6) 0.7475(7) 0.160(6) Uani 1 1 d DU C29 C 0.4279(8) -0.0329(7) 0.7734(7) 0.121(5) Uani 1 1 d DU H29 H 0.4035 -0.0692 0.7449 0.146 Uiso 1 1 calc R Cd1 Cd 0.44228(2) 0.44228(2) 1.0000 0.02207(17) Uani 1 2 d S Cl1 Cl 0.12078(15) 0.12078(15) 1.0000 0.0698(9) Uani 1 2 d S Cl2 Cl 0.73122(13) 0.73122(13) 1.0000 0.0619(8) Uani 1 2 d S N1 N 0.8775(3) 0.1204(4) 0.8374(2) 0.0347(12) Uani 1 1 d . N2 N 0.5457(3) 0.4940(3) 0.9342(2) 0.0282(11) Uani 1 1 d . N3 N 0.5128(3) 0.5552(3) 0.8950(2) 0.0277(11) Uani 1 1 d . N4 N 0.6498(3) 0.5562(4) 0.8889(2) 0.0292(11) Uani 1 1 d . N5 N 0.7310(3) 0.5738(4) 0.8671(3) 0.0469(17) Uani 1 1 d . H5A H 0.7568 0.5252 0.8588 0.070 Uiso 1 1 d R H5B H 0.7599 0.6015 0.8956 0.070 Uiso 1 1 d R N6 N 0.8137(3) 0.9755(3) 0.7587(2) 0.0293(12) Uani 1 1 d . O1 O 0.7659(8) 0.7631(8) 0.9489(3) 0.139(4) Uani 1 1 d . O2 O 0.6719(6) 0.6719(6) 1.0000 0.169(8) Uani 1 2 d S O3 O 0.1139(13) 0.1764(10) 0.9566(8) 0.317(14) Uani 1 1 d . O5 O 0.7881(15) 0.6653(13) 1.008(2) 0.223(15) Uani 0.50 1 d P O7 O 0.4038(10) -0.0431(12) 0.8268(8) 0.281(10) Uani 1 1 d DU O4 O 0.1371(15) 0.0575(9) 0.9675(5) 0.284(12) Uani 1 1 d . S1 S 0.5379(5) 0.0968(5) 0.7960(5) 0.266(4) Uani 1 1 d DU 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 C1 0.025(3) 0.030(3) 0.034(4) 0.010(3) 0.001(3) 0.007(3) C2 0.032(3) 0.029(3) 0.029(3) 0.005(3) -0.002(3) 0.002(3) C3 0.029(3) 0.026(3) 0.031(3) 0.001(3) 0.004(3) 0.005(3) C4 0.033(4) 0.038(4) 0.038(3) -0.001(3) -0.005(3) 0.012(3) C5 0.031(4) 0.041(4) 0.040(4) -0.006(3) -0.004(3) 0.011(3) C6 0.020(3) 0.034(4) 0.030(3) 0.003(3) 0.007(3) 0.003(3) C7 0.034(4) 0.045(4) 0.024(4) 0.002(3) 0.001(3) 0.001(3) C8 0.032(4) 0.061(5) 0.027(3) -0.007(3) 0.000(3) 0.014(4) C9 0.033(4) 0.040(4) 0.030(3) -0.009(3) -0.002(3) 0.011(3) C10 0.023(3) 0.028(3) 0.033(3) 0.009(3) 0.001(2) -0.002(3) C11 0.034(4) 0.031(4) 0.024(3) 0.002(3) 0.002(3) 0.004(3) C12 0.024(3) 0.026(3) 0.029(3) -0.008(3) 0.005(3) 0.003(2) C13 0.020(3) 0.023(3) 0.028(3) -0.004(2) -0.001(2) -0.001(2) C14 0.027(3) 0.032(3) 0.033(3) -0.002(3) 0.004(3) 0.002(3) C15 0.038(4) 0.039(4) 0.045(4) 0.012(3) -0.008(3) -0.006(3) C16 0.038(4) 0.053(4) 0.053(5) 0.012(4) -0.018(4) -0.013(3) C17 0.034(4) 0.049(4) 0.050(4) 0.019(4) -0.002(4) -0.002(3) C18 0.023(3) 0.028(3) 0.044(4) 0.002(3) 0.000(3) -0.009(3) C19 0.022(3) 0.033(4) 0.029(3) 0.004(3) 0.003(3) -0.002(3) C20 0.028(3) 0.023(3) 0.032(3) 0.001(3) 0.002(3) 0.003(3) C21 0.039(4) 0.035(4) 0.037(4) 0.003(3) -0.007(3) -0.008(3) C22 0.043(4) 0.042(4) 0.028(3) 0.001(3) 0.002(3) -0.008(3) C23 0.033(3) 0.039(4) 0.034(3) 0.009(3) -0.008(3) -0.005(3) C24 0.037(4) 0.037(4) 0.031(3) 0.012(3) -0.004(3) -0.006(3) C25 0.111(14) 0.155(15) 0.62(3) 0.03(2) 0.19(2) 0.025(10) C26 0.19(2) 0.183(18) 0.456(17) 0.230(18) 0.09(2) 0.110(14) C27 0.184(19) 0.158(16) 0.296(15) 0.084(12) 0.091(14) 0.089(12) C28 0.092(9) 0.105(10) 0.283(16) 0.008(11) 0.049(12) 0.049(6) C29 0.130(11) 0.070(7) 0.164(13) -0.010(7) 0.000(9) 0.040(6) Cd1 0.01920(19) 0.01920(19) 0.0278(3) 0.0005(2) -0.0005(2) -0.0018(3) Cl1 0.0749(13) 0.0749(13) 0.0597(18) 0.0036(15) -0.0036(15) -0.0127(18) Cl2 0.0639(11) 0.0639(11) 0.0580(17) 0.0132(13) -0.0132(13) -0.0170(15) N1 0.027(3) 0.033(3) 0.044(3) -0.003(3) 0.000(3) 0.002(2) N2 0.026(3) 0.025(2) 0.034(3) 0.000(2) 0.001(2) -0.003(2) N3 0.023(2) 0.026(3) 0.035(3) -0.002(3) 0.001(2) 0.000(2) N4 0.023(2) 0.033(3) 0.032(3) 0.003(3) 0.005(2) 0.004(3) N5 0.026(3) 0.047(4) 0.068(4) 0.022(3) 0.015(3) 0.004(3) N6 0.026(3) 0.028(3) 0.034(3) -0.001(2) 0.002(2) 0.001(2) O1 0.171(11) 0.188(11) 0.059(4) 0.040(6) -0.026(6) -0.082(8) O2 0.196(12) 0.196(12) 0.114(10) -0.032(11) 0.032(11) -0.120(14) O3 0.39(2) 0.204(15) 0.36(2) 0.171(16) 0.28(2) 0.104(16) O5 0.117(17) 0.096(15) 0.45(5) 0.05(3) 0.00(3) 0.040(13) O7 0.250(18) 0.34(2) 0.252(18) 0.014(17) 0.122(16) 0.035(18) O4 0.63(4) 0.132(10) 0.094(7) -0.066(8) -0.044(13) 0.096(16) S1 0.181(6) 0.178(7) 0.438(13) -0.046(8) 0.065(8) -0.032(5) 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' S S 0.1246 0.1234 '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' 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 N1 C1 C2 123.8(6) . . N1 C1 H1 118.1 . . C2 C1 H1 118.1 . . C1 C2 C3 120.3(6) . . C1 C2 H2 119.9 . . C3 C2 H2 119.9 . . C4 C3 C2 115.0(6) . . C4 C3 C6 122.1(6) . . C2 C3 C6 123.0(6) . . C5 C4 C3 120.7(6) . . C5 C4 H4 119.6 . . C3 C4 H4 119.6 . . N1 C5 C4 122.8(6) . . N1 C5 H5 118.6 . . C4 C5 H5 118.6 . . C7 C6 C11 119.1(6) . . C7 C6 C3 122.5(6) . . C11 C6 C3 118.4(6) . . C8 C7 C6 120.3(6) . . C8 C7 H7 119.9 . . C6 C7 H7 119.9 . . C7 C8 C9 121.6(6) . . C7 C8 H8 119.2 . . C9 C8 H8 119.2 . . C8 C9 C10 118.7(7) . . C8 C9 H9 120.7 . . C10 C9 H9 120.7 . . C11 C10 C9 119.1(6) . . C11 C10 C12 118.7(5) . . C9 C10 C12 122.1(6) . . C10 C11 C6 121.3(6) . . C10 C11 H11 119.4 . . C6 C11 H11 119.4 . . N2 C12 N4 108.9(5) . . N2 C12 C10 128.7(6) . . N4 C12 C10 122.3(5) . . N3 C13 N4 108.7(5) . . N3 C13 C14 124.5(5) . . N4 C13 C14 126.7(5) . . C19 C14 C15 119.8(6) . . C19 C14 C13 122.9(6) . . C15 C14 C13 117.2(6) . . C14 C15 C16 119.2(6) . . C14 C15 H15 120.4 . . C16 C15 H15 120.4 . . C17 C16 C15 120.4(7) . . C17 C16 H16 119.8 . . C15 C16 H16 119.8 . . C16 C17 C18 120.2(6) . . C16 C17 H17 119.9 . . C18 C17 H17 119.9 . . C19 C18 C17 119.3(6) . . C19 C18 C20 120.2(6) . . C17 C18 C20 120.3(6) . . C14 C19 C18 121.0(6) . . C14 C19 H19 119.5 . . C18 C19 H19 119.5 . . C21 C20 C24 116.6(6) . . C21 C20 C18 121.9(6) . . C24 C20 C18 121.4(6) . . C20 C21 C22 119.7(6) . . C20 C21 H21 120.2 . . C22 C21 H21 120.2 . . N6 C22 C21 123.7(6) . . N6 C22 H22 118.1 . . C21 C22 H22 118.1 . . N6 C23 C24 124.0(6) . . N6 C23 H23 118.0 . . C24 C23 H23 118.0 . . C23 C24 C20 119.9(6) . . C23 C24 H24 120.0 . . C20 C24 H24 120.0 . . C26 C25 S1 122.8(11) . . C26 C25 H25 118.6 . . S1 C25 H25 118.6 . . C25 C26 C27 106.1(8) . . C25 C26 H26 126.9 . . C27 C26 H26 126.9 . . C28 C27 C26 105.8(8) . . C28 C27 H27 127.1 . . C26 C27 H27 127.1 . . C27 C28 C29 119.1(12) . . C27 C28 S1 122.4(11) . . C29 C28 S1 118.4(11) . . O7 C29 C28 130.4(18) . . O7 C29 H29 114.8 . . C28 C29 H29 114.8 . . N2 Cd1 N2 83.4(2) 7_557 . N2 Cd1 N1 159.86(19) 7_557 6_456 N2 Cd1 N1 87.46(17) . 6_456 N2 Cd1 N1 87.46(17) 7_557 3_545 N2 Cd1 N1 159.85(19) . 3_545 N1 Cd1 N1 106.4(3) 6_456 3_545 N2 Cd1 N6 88.03(17) 7_557 6_466 N2 Cd1 N6 110.74(17) . 6_466 N1 Cd1 N6 78.46(19) 6_456 6_466 N1 Cd1 N6 86.8(2) 3_545 6_466 N2 Cd1 N6 110.74(17) 7_557 3_645 N2 Cd1 N6 88.03(17) . 3_645 N1 Cd1 N6 86.8(2) 6_456 3_645 N1 Cd1 N6 78.46(19) 3_545 3_645 N6 Cd1 N6 155.3(2) 6_466 3_645 O4 Cl1 O4 130(2) . 7_557 O4 Cl1 O3 101.9(11) . 7_557 O4 Cl1 O3 98.4(9) 7_557 7_557 O4 Cl1 O3 98.4(9) . . O4 Cl1 O3 101.9(11) 7_557 . O3 Cl1 O3 130(2) 7_557 . O2 Cl2 O1 123.7(4) . 7_557 O2 Cl2 O1 123.7(4) . . O1 Cl2 O1 112.6(8) 7_557 . O2 Cl2 O5 85.8(11) . 7_557 O1 Cl2 O5 96.9(17) 7_557 7_557 O1 Cl2 O5 87.7(17) . 7_557 O2 Cl2 O5 85.8(10) . . O1 Cl2 O5 87.7(17) 7_557 . O1 Cl2 O5 96.9(17) . . O5 Cl2 O5 172(2) 7_557 . C1 N1 C5 116.8(6) . . C1 N1 Cd1 126.6(4) . 4_554 C5 N1 Cd1 114.4(4) . 4_554 C12 N2 N3 108.2(5) . . C12 N2 Cd1 138.8(4) . . N3 N2 Cd1 111.1(3) . . C13 N3 N2 107.4(5) . . C12 N4 C13 106.7(5) . . C12 N4 N5 127.3(5) . . C13 N4 N5 125.7(5) . . N4 N5 H5A 108.6 . . N4 N5 H5B 109.5 . . H5A N5 H5B 109.4 . . C22 N6 C23 116.0(5) . . C22 N6 Cd1 126.2(4) . 4_564 C23 N6 Cd1 117.3(4) . 4_564 C25 S1 C28 82.9(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.326(8) . C1 C2 1.368(9) . C1 H1 0.9300 . C2 C3 1.411(9) . C2 H2 0.9300 . C3 C4 1.393(9) . C3 C6 1.493(9) . C4 C5 1.375(9) . C4 H4 0.9300 . C5 N1 1.348(8) . C5 H5 0.9300 . C6 C7 1.378(9) . C6 C11 1.388(9) . C7 C8 1.368(10) . C7 H7 0.9300 . C8 C9 1.383(10) . C8 H8 0.9300 . C9 C10 1.406(9) . C9 H9 0.9300 . C10 C11 1.381(9) . C10 C12 1.475(8) . C11 H11 0.9300 . C12 N2 1.299(8) . C12 N4 1.358(8) . C13 N3 1.303(7) . C13 N4 1.374(7) . C13 C14 1.460(8) . C14 C19 1.376(9) . C14 C15 1.389(9) . C15 C16 1.399(10) . C15 H15 0.9300 . C16 C17 1.374(10) . C16 H16 0.9300 . C17 C18 1.388(10) . C17 H17 0.9300 . C18 C19 1.382(9) . C18 C20 1.509(9) . C19 H19 0.9300 . C20 C21 1.379(9) . C20 C24 1.393(9) . C21 C22 1.385(9) . C21 H21 0.9300 . C22 N6 1.333(8) . C22 H22 0.9300 . C23 N6 1.341(8) . C23 C24 1.365(9) . C23 H23 0.9300 . C24 H24 0.9300 . C25 C26 1.344(10) . C25 S1 1.690(10) . C25 H25 0.9300 . C26 C27 1.513(10) . C26 H26 0.9300 . C27 C28 1.339(10) . C27 H27 0.9300 . C28 C29 1.475(9) . C28 S1 1.711(9) . C29 O7 1.239(9) . C29 H29 0.9300 . Cd1 N2 2.328(5) 7_557 Cd1 N2 2.328(5) . Cd1 N1 2.383(5) 6_456 Cd1 N1 2.383(5) 3_545 Cd1 N6 2.425(5) 6_466 Cd1 N6 2.425(5) 3_645 Cl1 O4 1.255(11) . Cl1 O4 1.255(11) 7_557 Cl1 O3 1.299(13) 7_557 Cl1 O3 1.299(13) . Cl2 O2 1.329(13) . Cl2 O1 1.342(8) 7_557 Cl2 O1 1.342(8) . Cl2 O5 1.390(19) 7_557 Cl2 O5 1.39(2) . N1 Cd1 2.383(5) 4_554 N2 N3 1.395(7) . N4 N5 1.399(7) . N5 H5A 0.8904 . N5 H5B 0.8880 . N6 Cd1 2.425(5) 4_564 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_4 N1 C1 C2 C3 1.2(10) . . C1 C2 C3 C4 5.6(9) . . C1 C2 C3 C6 -174.4(6) . . C2 C3 C4 C5 -7.0(10) . . C6 C3 C4 C5 173.0(6) . . C3 C4 C5 N1 1.8(11) . . C4 C3 C6 C7 161.3(7) . . C2 C3 C6 C7 -18.7(10) . . C4 C3 C6 C11 -18.3(9) . . C2 C3 C6 C11 161.7(6) . . C11 C6 C7 C8 0.5(10) . . C3 C6 C7 C8 -179.1(7) . . C6 C7 C8 C9 -0.9(11) . . C7 C8 C9 C10 1.6(11) . . C8 C9 C10 C11 -1.7(10) . . C8 C9 C10 C12 179.3(7) . . C9 C10 C11 C6 1.3(10) . . C12 C10 C11 C6 -179.6(6) . . C7 C6 C11 C10 -0.7(10) . . C3 C6 C11 C10 178.9(6) . . C11 C10 C12 N2 96.8(8) . . C9 C10 C12 N2 -84.2(9) . . C11 C10 C12 N4 -77.8(8) . . C9 C10 C12 N4 101.2(7) . . N3 C13 C14 C19 145.3(6) . . N4 C13 C14 C19 -32.3(9) . . N3 C13 C14 C15 -32.3(9) . . N4 C13 C14 C15 150.1(6) . . C19 C14 C15 C16 1.1(10) . . C13 C14 C15 C16 178.8(6) . . C14 C15 C16 C17 -0.1(12) . . C15 C16 C17 C18 -1.5(12) . . C16 C17 C18 C19 2.1(11) . . C16 C17 C18 C20 177.9(7) . . C15 C14 C19 C18 -0.5(10) . . C13 C14 C19 C18 -178.1(6) . . C17 C18 C19 C14 -1.1(10) . . C20 C18 C19 C14 -177.0(6) . . C19 C18 C20 C21 153.6(7) . . C17 C18 C20 C21 -22.2(10) . . C19 C18 C20 C24 -24.3(10) . . C17 C18 C20 C24 159.9(7) . . C24 C20 C21 C22 3.2(10) . . C18 C20 C21 C22 -174.7(7) . . C20 C21 C22 N6 -2.2(11) . . N6 C23 C24 C20 -0.5(11) . . C21 C20 C24 C23 -2.0(10) . . C18 C20 C24 C23 176.0(6) . . C25 C26 C27 C28 0.2(4) . . C26 C27 C28 C29 180.0(4) . . C26 C27 C28 S1 -0.2(6) . . C27 C28 C29 O7 -180.0(6) . . S1 C28 C29 O7 0.2(8) . . C2 C1 N1 C5 -6.7(10) . . C2 C1 N1 Cd1 155.3(5) . 4_554 C4 C5 N1 C1 5.2(11) . . C4 C5 N1 Cd1 -159.0(6) . 4_554 N4 C12 N2 N3 -0.8(6) . . C10 C12 N2 N3 -176.0(6) . . N4 C12 N2 Cd1 -163.3(4) . . C10 C12 N2 Cd1 21.5(10) . . N2 Cd1 N2 C12 68.3(6) 7_557 . N1 Cd1 N2 C12 -129.7(6) 6_456 . N1 Cd1 N2 C12 4.7(10) 3_545 . N6 Cd1 N2 C12 153.6(6) 6_466 . N6 Cd1 N2 C12 -42.9(6) 3_645 . N2 Cd1 N2 N3 -93.9(4) 7_557 . N1 Cd1 N2 N3 68.1(4) 6_456 . N1 Cd1 N2 N3 -157.5(5) 3_545 . N6 Cd1 N2 N3 -8.5(4) 6_466 . N6 Cd1 N2 N3 155.0(4) 3_645 . N4 C13 N3 N2 -0.6(6) . . C14 C13 N3 N2 -178.6(5) . . C12 N2 N3 C13 0.9(6) . . Cd1 N2 N3 C13 168.7(4) . . N2 C12 N4 C13 0.4(6) . . C10 C12 N4 C13 176.0(5) . . N2 C12 N4 N5 -173.9(6) . . C10 C12 N4 N5 1.6(10) . . N3 C13 N4 C12 0.1(6) . . C14 C13 N4 C12 178.0(5) . . N3 C13 N4 N5 174.6(6) . . C14 C13 N4 N5 -7.5(10) . . C21 C22 N6 C23 -0.3(10) . . C21 C22 N6 Cd1 171.1(5) . 4_564 C24 C23 N6 C22 1.6(10) . . C24 C23 N6 Cd1 -170.5(6) . 4_564 C26 C25 S1 C28 -0.01(17) . . C27 C28 S1 C25 0.1(4) . . C29 C28 S1 C25 180.0(4) . .