# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email lutongbu@mail.sysu.edu.cn loop_ _publ_author_name 'Di-Chang Zhong' 'Xiao-Long Feng' 'Tong-Bu Lu' data_1 _database_code_depnum_ccdc_archive 'CCDC 795026' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H5 Cd Cl N8' _chemical_formula_weight 361.05 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.253(6) _cell_length_b 7.6111(19) _cell_length_c 14.573(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2579.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1356 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7266 _exptl_absorpt_correction_T_max 0.8479 _exptl_absorpt_process_details 'SADABS (SHELDRICK, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4959 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1257 _reflns_number_gt 1008 _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^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1257 _refine_ls_number_parameters 48 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.5000 0.0000 0.5000 0.0121(3) Uani 1 4 d SU . . N1 N 0.42903(13) 0.1633(4) 0.4250(2) 0.0193(8) Uani 1 1 d . . . N2 N 0.38265(15) 0.1046(4) 0.3807(3) 0.0258(9) Uani 0.75 1 d P . . N2' N 0.38265(15) 0.1046(4) 0.3807(3) 0.0258(9) Uani 0.25 1 d P . . H2' H 0.3721 -0.0050 0.3716 0.031 Uiso 0.25 1 calc PR . . C1 C 0.3562(3) 0.2500 0.3534(5) 0.0343(16) Uani 1 2 d S . . C2 C 0.3016(3) 0.2500 0.2987(5) 0.0331(17) Uani 1 2 d S . . C3 C 0.2754(3) 0.0941(7) 0.2742(5) 0.061(2) Uani 1 1 d . . . H3 H 0.2927 -0.0144 0.2908 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.5000 0.2500 0.62345(19) 0.0367(6) Uani 1 4 d SU . . 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 0.0066(4) 0.0070(4) 0.0229(4) 0.00269(18) 0.000 0.000 N1 0.0123(17) 0.0111(14) 0.034(2) 0.0036(14) -0.0079(15) -0.0019(14) N2 0.0201(19) 0.0099(16) 0.047(2) -0.0004(16) -0.0175(18) 0.0012(14) N2' 0.0201(19) 0.0099(16) 0.047(2) -0.0004(16) -0.0175(18) 0.0012(14) C1 0.036(4) 0.020(3) 0.047(5) 0.000 -0.014(3) 0.000 C2 0.024(3) 0.019(3) 0.055(5) 0.000 -0.019(3) 0.000 C3 0.052(3) 0.019(3) 0.114(5) 0.002(3) -0.056(4) 0.000(2) Cl1 0.0409(14) 0.0216(11) 0.0477(16) 0.000 0.000 0.000 _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 N1 2.337(3) 9_656 ? Cd1 N1 2.337(3) 12_655 ? Cd1 N1 2.337(3) . ? Cd1 N1 2.337(3) 4_556 ? Cd1 Cl1 2.6186(19) . ? Cd1 Cl1 2.6186(19) 9_656 ? N1 N1 1.320(6) 11_565 ? N1 N2 1.334(5) . ? N2 C1 1.326(5) . ? C1 N2' 1.326(5) 11_565 ? C1 N2 1.326(5) 11_565 ? C1 C2 1.500(9) . ? C2 C3 1.381(6) . ? C2 C3 1.381(6) 11_565 ? C3 C3 1.377(10) 7_545 ? C3 H3 0.9500 . ? Cl1 Cd1 2.6186(19) 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 Cd1 N1 90.16(16) 9_656 12_655 ? N1 Cd1 N1 180.00(17) 9_656 . ? N1 Cd1 N1 89.84(16) 12_655 . ? N1 Cd1 N1 89.84(16) 9_656 4_556 ? N1 Cd1 N1 180.00(11) 12_655 4_556 ? N1 Cd1 N1 90.16(16) . 4_556 ? N1 Cd1 Cl1 93.74(9) 9_656 . ? N1 Cd1 Cl1 86.26(9) 12_655 . ? N1 Cd1 Cl1 86.26(9) . . ? N1 Cd1 Cl1 93.74(9) 4_556 . ? N1 Cd1 Cl1 86.26(9) 9_656 9_656 ? N1 Cd1 Cl1 93.74(9) 12_655 9_656 ? N1 Cd1 Cl1 93.74(9) . 9_656 ? N1 Cd1 Cl1 86.26(9) 4_556 9_656 ? Cl1 Cd1 Cl1 180.0 . 9_656 ? N1 N1 N2 109.6(2) 11_565 . ? N1 N1 Cd1 122.13(8) 11_565 . ? N2 N1 Cd1 128.3(2) . . ? C1 N2 N1 103.9(3) . . ? N2' C1 N2 0.0(4) 11_565 11_565 ? N2' C1 N2 113.1(5) 11_565 . ? N2 C1 N2 113.1(5) 11_565 . ? N2' C1 C2 123.5(3) 11_565 . ? N2 C1 C2 123.5(3) 11_565 . ? N2 C1 C2 123.5(3) . . ? C3 C2 C3 118.5(6) . 11_565 ? C3 C2 C1 120.7(3) . . ? C3 C2 C1 120.7(3) 11_565 . ? C3 C3 C2 120.7(3) 7_545 . ? C3 C3 H3 119.6 7_545 . ? C2 C3 H3 119.6 . . ? Cd1 Cl1 Cd1 93.21(9) . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.042 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.180 #start Validation Reply Form _vrf_PLAT602_1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure RESPONSE: All of the disordered electron density of solvent molecules was treated as a diffuse contribution using the program SQUEEZE. ; # end Validation Reply Form # Attachment '2.cif' data_l05022m _database_code_depnum_ccdc_archive 'CCDC 795027' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 Cd5 Cl6 N16 O2' _chemical_formula_sum 'C18 H16 Cd5 Cl6 N16 O2' _chemical_formula_weight 1263.17 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7396(14) _cell_length_b 9.1057(15) _cell_length_c 10.0556(16) _cell_angle_alpha 74.388(2) _cell_angle_beta 82.547(2) _cell_angle_gamma 77.733(2) _cell_volume 750.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4297 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.07 _exptl_crystal_description BLOCK _exptl_crystal_colour 'LIGHT YELLOW' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 4.070 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4417 _exptl_absorpt_correction_T_max 0.6408 _exptl_absorpt_process_details 'SADABS (SHELDRICK, 1996)' _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_% 0 _diffrn_reflns_number 5416 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2614 _reflns_number_gt 2315 _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^)+(0.0266P)^2^+0.4384P] 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 2614 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.18514(3) -0.06022(3) 0.37189(3) 0.00985(8) Uani 1 1 d . . . Cd2 Cd 0.42108(3) -0.11892(3) 0.70775(3) 0.01048(8) Uani 1 1 d . . . Cd3 Cd 0.5000 0.5000 0.0000 0.00979(10) Uani 1 2 d S . . Cl1 Cl 0.13161(10) -0.00465(10) 0.62394(9) 0.01197(19) Uani 1 1 d . . . Cl2 Cl 0.48511(10) -0.13535(10) 0.41996(9) 0.01180(19) Uani 1 1 d . . . Cl3 Cl 0.38295(10) -0.39732(10) 0.76130(9) 0.01279(19) Uani 1 1 d . . . C1 C 0.1265(4) 0.4357(4) 0.1867(3) 0.0100(7) Uani 1 1 d . . . C2 C 0.0269(4) 0.5867(4) 0.1352(4) 0.0096(7) Uani 1 1 d . . . C3 C -0.1136(4) 0.6300(4) 0.2075(4) 0.0156(8) Uani 1 1 d . . . H3 H -0.1430 0.5638 0.2904 0.019 Uiso 1 1 calc R . . C4 C -0.2114(4) 0.7708(4) 0.1583(4) 0.0136(8) Uani 1 1 d . . . H4 H -0.3064 0.7976 0.2073 0.016 Uiso 1 1 calc R . . C5 C -0.1675(4) 0.8717(4) 0.0360(4) 0.0103(8) Uani 1 1 d . . . C6 C -0.2636(4) 1.0248(4) -0.0175(4) 0.0101(8) Uani 1 1 d . . . C7 C -0.0279(4) 0.8277(4) -0.0380(4) 0.0108(8) Uani 1 1 d . . . H7 H 0.0015 0.8943 -0.1207 0.013 Uiso 1 1 calc R . . C8 C 0.0684(4) 0.6857(4) 0.0097(4) 0.0113(8) Uani 1 1 d . . . H8 H 0.1607 0.6565 -0.0419 0.014 Uiso 1 1 calc R . . C9 C 0.2501(5) -0.4488(5) 0.4586(4) 0.0216(9) Uani 1 1 d . . . H9A H 0.3047 -0.4331 0.3682 0.032 Uiso 1 1 calc R . . H9B H 0.1894 -0.5285 0.4710 0.032 Uiso 1 1 calc R . . H9C H 0.3248 -0.4797 0.5276 0.032 Uiso 1 1 calc R . . N1 N 0.0763(3) 0.3186(3) 0.2836(3) 0.0112(6) Uani 1 1 d . . . N2 N 0.2002(3) 0.2021(3) 0.2976(3) 0.0107(6) Uani 1 1 d . . . N3 N 0.3199(3) 0.2443(3) 0.2147(3) 0.0108(6) Uani 1 1 d . . . N4 N 0.2779(3) 0.3924(3) 0.1422(3) 0.0106(6) Uani 1 1 d . . . N5 N -0.2647(3) 1.1012(3) -0.1525(3) 0.0107(6) Uani 1 1 d . . . N6 N -0.3580(3) 1.2398(4) -0.1572(3) 0.0129(7) Uani 1 1 d . . . N7 N -0.4113(3) 1.2471(3) -0.0313(3) 0.0103(6) Uani 1 1 d . . . N8 N -0.3542(3) 1.1129(3) 0.0608(3) 0.0109(6) Uani 1 1 d . . . O1 O 0.1473(3) -0.3064(3) 0.4722(3) 0.0179(6) Uani 1 1 d . . . H1 H 0.1216 -0.2543 0.3955 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.00976(14) 0.00861(15) 0.00992(14) -0.00189(11) 0.00094(10) -0.00051(11) Cd2 0.00930(14) 0.00982(15) 0.01039(14) -0.00073(11) -0.00014(10) -0.00025(11) Cd3 0.01051(19) 0.0070(2) 0.00984(19) -0.00143(15) 0.00114(14) 0.00077(15) Cl1 0.0090(4) 0.0152(5) 0.0106(4) -0.0034(4) 0.0003(3) -0.0005(4) Cl2 0.0105(4) 0.0111(5) 0.0129(4) -0.0030(4) 0.0006(3) -0.0009(3) Cl3 0.0149(4) 0.0106(5) 0.0122(4) -0.0021(4) -0.0018(3) -0.0015(4) C1 0.0103(18) 0.0119(19) 0.0091(18) -0.0041(15) -0.0008(14) -0.0032(15) C2 0.0096(18) 0.0089(19) 0.0113(18) -0.0035(14) -0.0021(14) -0.0019(15) C3 0.015(2) 0.016(2) 0.0124(19) 0.0014(16) 0.0024(15) -0.0029(16) C4 0.0118(18) 0.013(2) 0.0147(19) -0.0075(16) 0.0040(15) 0.0015(16) C5 0.0130(18) 0.0070(18) 0.0116(18) -0.0033(15) -0.0029(15) -0.0011(15) C6 0.0084(17) 0.013(2) 0.0113(18) -0.0048(15) 0.0004(14) -0.0043(15) C7 0.0122(18) 0.012(2) 0.0087(18) -0.0003(15) -0.0002(14) -0.0061(15) C8 0.0070(18) 0.0129(19) 0.0139(19) -0.0057(15) 0.0010(15) 0.0003(15) C9 0.033(2) 0.017(2) 0.016(2) -0.0077(17) 0.0050(18) -0.0047(19) N1 0.0103(16) 0.0094(16) 0.0127(16) -0.0026(13) -0.0003(12) 0.0001(13) N2 0.0127(16) 0.0073(16) 0.0101(15) -0.0009(12) 0.0007(12) -0.0005(13) N3 0.0095(15) 0.0093(16) 0.0113(15) -0.0015(13) -0.0005(12) 0.0018(13) N4 0.0105(16) 0.0075(16) 0.0121(16) -0.0003(13) -0.0008(12) -0.0009(13) N5 0.0142(16) 0.0063(16) 0.0117(16) -0.0038(13) -0.0022(13) 0.0004(13) N6 0.0140(16) 0.0095(16) 0.0129(16) -0.0020(13) -0.0017(13) 0.0021(13) N7 0.0092(15) 0.0084(16) 0.0111(15) -0.0022(12) -0.0010(12) 0.0031(12) N8 0.0084(15) 0.0094(16) 0.0128(16) -0.0007(13) -0.0011(12) 0.0005(13) O1 0.0210(15) 0.0088(14) 0.0177(14) 0.0023(11) 0.0028(11) 0.0005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.273(3) . ? Cd1 N5 2.329(3) 2_565 ? Cd1 N2 2.330(3) . ? Cd1 Cl2 2.6388(9) . ? Cd1 Cl1 2.6797(10) . ? Cd1 Cl1 2.7023(10) 2_556 ? Cd2 N8 2.337(3) 2_566 ? Cd2 N3 2.433(3) 2_656 ? Cd2 Cl3 2.5308(10) . ? Cd2 Cl2 2.5720(10) 2_656 ? Cd2 Cl1 2.6750(9) . ? Cd2 Cl2 2.9134(10) . ? Cd3 N7 2.361(3) 2_575 ? Cd3 N7 2.361(3) 1_645 ? Cd3 N4 2.471(3) 2_665 ? Cd3 N4 2.471(3) . ? Cd3 Cl3 2.5894(9) 1_564 ? Cd3 Cl3 2.5894(9) 2_656 ? Cl1 Cd1 2.7023(10) 2_556 ? Cl2 Cd2 2.5720(10) 2_656 ? Cl3 Cd3 2.5894(9) 1_546 ? C1 N1 1.344(5) . ? C1 N4 1.351(4) . ? C1 C2 1.463(5) . ? C2 C3 1.382(5) . ? C2 C8 1.394(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.387(5) . ? C4 H4 0.9300 . ? C5 C7 1.386(5) . ? C5 C6 1.468(5) . ? C6 N8 1.341(5) . ? C6 N5 1.349(4) . ? C7 C8 1.385(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O1 1.441(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N1 N2 1.338(4) . ? N2 N3 1.307(4) . ? N3 N4 1.347(4) . ? N3 Cd2 2.433(3) 2_656 ? N5 N6 1.343(4) . ? N5 Cd1 2.329(3) 2_565 ? N6 N7 1.305(4) . ? N7 N8 1.361(4) . ? N7 Cd3 2.361(3) 1_465 ? N8 Cd2 2.337(3) 2_566 ? O1 H1 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N5 95.52(10) . 2_565 ? O1 Cd1 N2 171.33(10) . . ? N5 Cd1 N2 92.71(10) 2_565 . ? O1 Cd1 Cl2 91.93(7) . . ? N5 Cd1 Cl2 86.71(7) 2_565 . ? N2 Cd1 Cl2 91.27(7) . . ? O1 Cd1 Cl1 88.10(7) . . ? N5 Cd1 Cl1 172.39(7) 2_565 . ? N2 Cd1 Cl1 84.06(7) . . ? Cl2 Cd1 Cl1 86.48(3) . . ? O1 Cd1 Cl1 83.62(7) . 2_556 ? N5 Cd1 Cl1 103.69(7) 2_565 2_556 ? N2 Cd1 Cl1 91.78(7) . 2_556 ? Cl2 Cd1 Cl1 169.01(3) . 2_556 ? Cl1 Cd1 Cl1 83.34(3) . 2_556 ? N8 Cd2 N3 84.78(10) 2_566 2_656 ? N8 Cd2 Cl3 90.99(8) 2_566 . ? N3 Cd2 Cl3 82.08(7) 2_656 . ? N8 Cd2 Cl2 107.84(8) 2_566 2_656 ? N3 Cd2 Cl2 92.63(7) 2_656 2_656 ? Cl3 Cd2 Cl2 159.96(3) . 2_656 ? N8 Cd2 Cl1 95.92(7) 2_566 . ? N3 Cd2 Cl1 175.22(7) 2_656 . ? Cl3 Cd2 Cl1 93.17(3) . . ? Cl2 Cd2 Cl1 91.66(3) 2_656 . ? N8 Cd2 Cl2 176.05(7) 2_566 . ? N3 Cd2 Cl2 97.80(7) 2_656 . ? Cl3 Cd2 Cl2 86.42(3) . . ? Cl2 Cd2 Cl2 75.11(3) 2_656 . ? Cl1 Cd2 Cl2 81.26(3) . . ? N7 Cd3 N7 180.0 2_575 1_645 ? N7 Cd3 N4 84.98(10) 2_575 2_665 ? N7 Cd3 N4 95.02(10) 1_645 2_665 ? N7 Cd3 N4 95.02(10) 2_575 . ? N7 Cd3 N4 84.98(10) 1_645 . ? N4 Cd3 N4 180.0 2_665 . ? N7 Cd3 Cl3 86.92(7) 2_575 1_564 ? N7 Cd3 Cl3 93.08(7) 1_645 1_564 ? N4 Cd3 Cl3 79.85(7) 2_665 1_564 ? N4 Cd3 Cl3 100.15(7) . 1_564 ? N7 Cd3 Cl3 93.08(7) 2_575 2_656 ? N7 Cd3 Cl3 86.92(7) 1_645 2_656 ? N4 Cd3 Cl3 100.15(7) 2_665 2_656 ? N4 Cd3 Cl3 79.85(7) . 2_656 ? Cl3 Cd3 Cl3 180.0 1_564 2_656 ? Cd2 Cl1 Cd1 97.91(3) . . ? Cd2 Cl1 Cd1 160.64(4) . 2_556 ? Cd1 Cl1 Cd1 96.66(3) . 2_556 ? Cd2 Cl2 Cd1 100.76(3) 2_656 . ? Cd2 Cl2 Cd2 104.89(3) 2_656 . ? Cd1 Cl2 Cd2 93.21(3) . . ? Cd2 Cl3 Cd3 99.06(3) . 1_546 ? N1 C1 N4 110.7(3) . . ? N1 C1 C2 123.7(3) . . ? N4 C1 C2 125.6(3) . . ? C3 C2 C8 119.0(3) . . ? C3 C2 C1 120.2(3) . . ? C8 C2 C1 120.7(3) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C7 119.2(3) . . ? C4 C5 C6 122.1(3) . . ? C7 C5 C6 118.7(3) . . ? N8 C6 N5 110.4(3) . . ? N8 C6 C5 125.0(3) . . ? N5 C6 C5 124.4(3) . . ? C8 C7 C5 120.8(3) . . ? C8 C7 H7 119.6 . . ? C5 C7 H7 119.6 . . ? C7 C8 C2 120.0(3) . . ? C7 C8 H8 120.0 . . ? C2 C8 H8 120.0 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 N1 C1 104.7(3) . . ? N3 N2 N1 110.6(3) . . ? N3 N2 Cd1 119.3(2) . . ? N1 N2 Cd1 124.7(2) . . ? N2 N3 N4 109.1(3) . . ? N2 N3 Cd2 116.3(2) . 2_656 ? N4 N3 Cd2 126.4(2) . 2_656 ? N3 N4 C1 105.0(3) . . ? N3 N4 Cd3 113.1(2) . . ? C1 N4 Cd3 141.4(2) . . ? N6 N5 C6 106.0(3) . . ? N6 N5 Cd1 112.5(2) . 2_565 ? C6 N5 Cd1 140.9(2) . 2_565 ? N7 N6 N5 108.8(3) . . ? N6 N7 N8 110.2(3) . . ? N6 N7 Cd3 115.3(2) . 1_465 ? N8 N7 Cd3 130.1(2) . 1_465 ? C6 N8 N7 104.5(3) . . ? C6 N8 Cd2 141.3(2) . 2_566 ? N7 N8 Cd2 113.8(2) . 2_566 ? C9 O1 Cd1 127.4(2) . . ? C9 O1 H1 109.5 . . ? Cd1 O1 H1 54.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.851 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.123