# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 804241' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H12 Cd N10' _chemical_formula_sum 'C20 H12 Cd N10' _chemical_formula_weight 504.81 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd _symmetry_space_group_name_Hall -F2uv2vw loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 15.1007(10) _cell_length_b 17.2538(11) _cell_length_c 31.509(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8209.5(9) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2448 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 28.06 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000.0 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.008 _exptl_absorpt_correction_T_max 0.014 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 11883 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.06 _reflns_number_total 2448 _reflns_number_gt 2177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0323P)^2^+14.5608P] 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 2448 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 C1 C 0.21906(13) 0.33944(11) 0.05576(6) 0.0292(4) Uani 1 1 d . . . H1 H 0.1946 0.2999 0.0394 0.035 Uiso 1 1 calc R . . C2 C 0.25949(13) 0.40208(11) 0.03455(6) 0.0279(4) Uani 1 1 d . . . C3 C 0.29665(14) 0.45971(12) 0.05837(6) 0.0356(4) Uani 1 1 d . . . H3 H 0.3244 0.5013 0.0452 0.043 Uiso 1 1 calc R . . C4 C 0.29273(14) 0.45589(12) 0.10313(6) 0.0334(4) Uani 1 1 d . . . C5 C 0.25065(13) 0.39136(11) 0.12208(6) 0.0285(4) Uani 1 1 d . . . C6 C 0.24703(15) 0.38605(12) 0.16679(7) 0.0369(5) Uani 1 1 d . . . H6 H 0.2207 0.3434 0.1797 0.044 Uiso 1 1 calc R . . C7 C 0.28235(17) 0.44391(15) 0.19095(7) 0.0462(5) Uani 1 1 d . . . H7 H 0.2786 0.4407 0.2204 0.055 Uiso 1 1 calc R . . C8 C 0.32401(19) 0.50794(15) 0.17256(8) 0.0517(6) Uani 1 1 d . . . H8 H 0.3473 0.5468 0.1897 0.062 Uiso 1 1 calc R . . C9 C 0.33062(19) 0.51355(13) 0.12959(7) 0.0460(6) Uani 1 1 d . . . H9 H 0.3601 0.5554 0.1175 0.055 Uiso 1 1 calc R . . C10 C 0.26390(12) 0.40150(11) -0.01199(6) 0.0279(4) Uani 1 1 d . . . Cd1 Cd 0.1250 0.237189(10) 0.1250 0.02701(8) Uani 1 2 d S . . N1 N 0.21392(11) 0.33370(9) 0.09742(5) 0.0286(3) Uani 1 1 d . . . N2 N 0.23399(12) 0.34384(10) -0.03638(5) 0.0363(4) Uani 1 1 d . . . N3 N 0.30393(11) 0.45687(9) -0.03452(5) 0.0315(3) Uani 1 1 d . . . N4 N 0.29748(11) 0.43081(9) -0.07440(5) 0.0312(3) Uani 1 1 d . . . N5 N 0.25646(13) 0.36336(10) -0.07586(5) 0.0369(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 C1 0.0373(10) 0.0252(9) 0.0251(9) -0.0008(7) 0.0020(7) -0.0020(7) C2 0.0337(9) 0.0276(9) 0.0223(8) 0.0019(7) 0.0049(7) 0.0012(7) C3 0.0477(12) 0.0285(10) 0.0307(10) 0.0035(8) 0.0059(8) -0.0074(8) C4 0.0417(11) 0.0287(10) 0.0298(10) -0.0011(8) 0.0033(8) -0.0050(8) C5 0.0358(10) 0.0249(9) 0.0247(9) -0.0006(7) 0.0000(7) -0.0019(7) C6 0.0465(12) 0.0373(11) 0.0268(10) 0.0011(8) 0.0001(9) -0.0084(9) C7 0.0606(14) 0.0523(14) 0.0257(10) -0.0056(9) -0.0021(10) -0.0117(11) C8 0.0677(17) 0.0479(14) 0.0396(12) -0.0117(10) -0.0022(12) -0.0192(12) C9 0.0607(15) 0.0358(12) 0.0414(12) -0.0043(9) 0.0029(10) -0.0174(10) C10 0.0344(9) 0.0257(9) 0.0237(8) 0.0039(7) 0.0027(7) 0.0008(7) Cd1 0.04097(12) 0.02239(11) 0.01767(10) 0.000 -0.00334(7) 0.000 N1 0.0393(9) 0.0241(8) 0.0223(7) 0.0007(6) -0.0002(6) -0.0026(6) N2 0.0507(10) 0.0330(9) 0.0254(8) 0.0031(7) 0.0021(7) -0.0093(8) N3 0.0433(9) 0.0284(8) 0.0227(7) 0.0000(6) 0.0049(7) -0.0034(7) N4 0.0423(9) 0.0286(8) 0.0226(7) 0.0011(6) 0.0022(7) -0.0013(7) N5 0.0525(11) 0.0330(9) 0.0251(8) 0.0016(7) 0.0021(7) -0.0079(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 C1 N1 1.319(2) . ? C1 C2 1.410(3) . ? C1 H1 0.9300 . ? C2 C3 1.366(3) . ? C2 C10 1.468(2) . ? C3 C4 1.413(3) . ? C3 H3 0.9300 . ? C4 C5 1.414(3) . ? C4 C9 1.419(3) . ? C5 N1 1.379(2) . ? C5 C6 1.413(3) . ? C6 C7 1.364(3) . ? C6 H6 0.9300 . ? C7 C8 1.397(3) . ? C7 H7 0.9300 . ? C8 C9 1.361(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N3 1.335(2) . ? C10 N2 1.336(3) . ? Cd1 N4 2.2041(16) 30 ? Cd1 N4 2.2041(16) 32_556 ? Cd1 N1 2.3088(16) . ? Cd1 N1 2.3088(16) 11_454 ? N2 N5 1.333(2) . ? N3 N4 1.338(2) . ? N4 N5 1.319(2) . ? N4 Cd1 2.2041(16) 18_665 ? 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 C1 C2 123.72(17) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.38(17) . . ? C3 C2 C10 122.35(17) . . ? C1 C2 C10 119.21(17) . . ? C2 C3 C4 119.81(18) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.48(18) . . ? C3 C4 C9 122.48(19) . . ? C5 C4 C9 119.03(18) . . ? N1 C5 C6 119.96(17) . . ? N1 C5 C4 120.73(17) . . ? C6 C5 C4 119.31(18) . . ? C7 C6 C5 119.6(2) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 121.6(2) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C4 120.3(2) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? N3 C10 N2 112.34(16) . . ? N3 C10 C2 123.15(17) . . ? N2 C10 C2 124.36(17) . . ? N4 Cd1 N4 127.63(8) 30 32_556 ? N4 Cd1 N1 110.79(6) 30 . ? N4 Cd1 N1 106.36(6) 32_556 . ? N4 Cd1 N1 106.36(6) 30 11_454 ? N4 Cd1 N1 110.79(6) 32_556 11_454 ? N1 Cd1 N1 87.69(8) . 11_454 ? C1 N1 C5 118.88(16) . . ? C1 N1 Cd1 117.58(12) . . ? C5 N1 Cd1 122.84(12) . . ? N5 N2 C10 105.23(16) . . ? C10 N3 N4 103.06(15) . . ? N5 N4 N3 111.30(15) . . ? N5 N4 Cd1 127.85(12) . 18_665 ? N3 N4 Cd1 119.49(12) . 18_665 ? N4 N5 N2 108.07(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.370 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.065 data_2 _database_code_depnum_ccdc_archive 'CCDC 804242' #TrackingRef '15239_web_deposit_cif_file_0_HongDeng_1352260642.cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cd N8 O' _chemical_formula_sum 'C10 H8 Cd N8 O' _chemical_formula_weight 368.65 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.5230(13) _cell_length_b 16.510(2) _cell_length_c 7.4998(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.9080(10) _cell_angle_gamma 90.00 _cell_volume 1225.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5423 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.539 _exptl_absorpt_correction_T_max 0.605 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6113 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.20 _reflns_number_total 2189 _reflns_number_gt 2100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0333P)^2^+4.8864P] 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 0.0494(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2189 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 C1 C 0.1908(4) 0.0381(3) 0.7936(6) 0.0236(9) Uani 1 1 d . A 1 H1 H 0.1035 0.0277 0.7918 0.028 Uiso 1 1 calc R A 1 C2 C 0.2503(4) -0.0179(2) 0.7031(6) 0.0213(9) Uani 1 1 d . A 1 C3 C 0.3783(4) -0.0029(3) 0.7050(6) 0.0227(9) Uani 1 1 d . A 1 H3 H 0.4197 -0.0382 0.6452 0.027 Uiso 1 1 calc R A 1 C4 C 0.4471(4) 0.0664(3) 0.7981(6) 0.0208(9) Uani 1 1 d . A 1 C5 C 0.3817(4) 0.1185(3) 0.8883(6) 0.0229(9) Uani 1 1 d . A 1 C6 C 0.4502(5) 0.1880(3) 0.9860(7) 0.0295(10) Uani 1 1 d . A 1 H6 H 0.4093 0.2211 1.0510 0.035 Uiso 1 1 calc R A 1 C7 C 0.5745(5) 0.2059(3) 0.9845(8) 0.0362(12) Uani 1 1 d . A 1 H7 H 0.6185 0.2519 1.0476 0.043 Uiso 1 1 calc R A 1 C8 C 0.6396(5) 0.1561(3) 0.8884(7) 0.0338(11) Uani 1 1 d . A 1 H8 H 0.7244 0.1704 0.8857 0.041 Uiso 1 1 calc R A 1 C9 C 0.5789(4) 0.0872(3) 0.7999(7) 0.0295(10) Uani 1 1 d . A 1 H9 H 0.6234 0.0538 0.7406 0.035 Uiso 1 1 calc R A 1 C10 C 0.1673(4) -0.0872(2) 0.6071(6) 0.0201(8) Uani 1 1 d . A 1 Cd1 Cd 0.10150(3) 0.208239(17) 0.90300(4) 0.01889(18) Uani 1 1 d . . 1 N1 N 0.2510(4) 0.1040(2) 0.8799(5) 0.0232(8) Uani 1 1 d . A 1 N2 N 0.1497(4) -0.1120(2) 0.4313(5) 0.0260(8) Uani 1 1 d . A 1 N3 N 0.0613(4) -0.1733(2) 0.4021(5) 0.0248(8) Uani 1 1 d . . 1 N4 N 0.0287(4) -0.1840(2) 0.5547(5) 0.0248(8) Uani 1 1 d . . 1 N5 N 0.0937(4) -0.1304(2) 0.6867(5) 0.0277(8) Uani 1 1 d . A 1 N6 N 0.1954(5) 0.2127(3) 1.2286(6) 0.0410(7) Uani 1 1 d . . 1 N7 N 0.2673(5) 0.1557(3) 1.2935(6) 0.0410(7) Uani 1 1 d . . 1 N8 N 0.3414(5) 0.1042(3) 1.3516(6) 0.0410(7) Uani 1 1 d . . 1 O1 O -0.0261(3) 0.1037(2) 0.9795(5) 0.0334(8) Uani 1 1 d . B 1 H1A H -0.0848 0.0789 0.8973 0.050 Uiso 1 1 d R B 1 H1B H -0.0509 0.1136 1.0699 0.050 Uiso 1 1 d R B 1 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 0.023(2) 0.022(2) 0.030(2) 0.0007(18) 0.0156(18) -0.0003(17) C2 0.027(2) 0.019(2) 0.020(2) -0.0006(16) 0.0108(17) 0.0010(17) C3 0.025(2) 0.022(2) 0.025(2) -0.0010(17) 0.0138(18) 0.0022(17) C4 0.0182(19) 0.023(2) 0.021(2) 0.0031(16) 0.0073(16) 0.0007(16) C5 0.023(2) 0.022(2) 0.024(2) 0.0036(17) 0.0077(17) 0.0001(17) C6 0.028(2) 0.025(2) 0.035(3) -0.004(2) 0.010(2) 0.0006(19) C7 0.029(3) 0.031(3) 0.046(3) -0.009(2) 0.008(2) -0.009(2) C8 0.021(2) 0.037(3) 0.044(3) 0.000(2) 0.011(2) -0.006(2) C9 0.022(2) 0.035(3) 0.034(3) 0.001(2) 0.0130(19) 0.0019(19) C10 0.023(2) 0.018(2) 0.022(2) 0.0017(16) 0.0108(17) 0.0010(16) Cd1 0.0241(2) 0.0175(2) 0.0185(2) 0.00009(10) 0.01164(14) 0.00143(11) N1 0.0237(18) 0.0199(18) 0.029(2) -0.0034(15) 0.0135(15) -0.0014(14) N2 0.0287(19) 0.027(2) 0.027(2) -0.0046(16) 0.0152(16) -0.0080(16) N3 0.032(2) 0.0220(19) 0.0242(19) -0.0037(15) 0.0140(16) -0.0068(16) N4 0.032(2) 0.0253(19) 0.0197(18) -0.0040(15) 0.0125(16) -0.0096(16) N5 0.038(2) 0.027(2) 0.0229(19) -0.0060(16) 0.0162(17) -0.0112(17) N6 0.0573(17) 0.0400(14) 0.0271(13) 0.0053(10) 0.0161(12) 0.0224(11) N7 0.0573(17) 0.0400(14) 0.0271(13) 0.0053(10) 0.0161(12) 0.0224(11) N8 0.0573(17) 0.0400(14) 0.0271(13) 0.0053(10) 0.0161(12) 0.0224(11) O1 0.0376(19) 0.040(2) 0.0294(18) -0.0070(15) 0.0204(15) -0.0116(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 C1 N1 1.313(6) . ? C1 C2 1.413(6) . ? C1 H1 0.9300 . ? C2 C3 1.365(6) . ? C2 C10 1.470(6) . ? C3 C4 1.405(6) . ? C3 H3 0.9300 . ? C4 C5 1.411(6) . ? C4 C9 1.424(6) . ? C5 N1 1.376(6) . ? C5 C6 1.418(6) . ? C6 C7 1.345(7) . ? C6 H6 0.9300 . ? C7 C8 1.415(8) . ? C7 H7 0.9300 . ? C8 C9 1.361(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N2 1.332(6) . ? C10 N5 1.335(6) . ? Cd1 N6 2.296(4) 4_565 ? Cd1 N6 2.302(5) . ? Cd1 N4 2.332(4) 2_556 ? Cd1 O1 2.373(3) . ? Cd1 N1 2.378(4) . ? Cd1 N3 2.415(4) 3_556 ? N2 N3 1.341(5) . ? N3 N4 1.314(5) . ? N3 Cd1 2.415(4) 3_556 ? N4 N5 1.331(5) . ? N4 Cd1 2.332(4) 2_546 ? N6 N7 1.202(6) . ? N6 Cd1 2.296(4) 4_566 ? N7 N8 1.135(6) . ? O1 H1A 0.8192 . ? O1 H1B 0.8217 . ? 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 C1 C2 124.0(4) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.3(4) . . ? C3 C2 C10 124.5(4) . . ? C1 C2 C10 117.2(4) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 C9 122.5(4) . . ? C5 C4 C9 118.7(4) . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 119.3(4) . . ? C4 C5 C6 119.8(4) . . ? C7 C6 C5 119.9(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 121.1(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 120.4(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C4 120.1(4) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N2 C10 N5 111.9(4) . . ? N2 C10 C2 125.7(4) . . ? N5 C10 C2 122.4(4) . . ? N6 Cd1 N6 118.27(19) 4_565 . ? N6 Cd1 N4 91.75(16) 4_565 2_556 ? N6 Cd1 N4 83.75(14) . 2_556 ? N6 Cd1 O1 159.99(14) 4_565 . ? N6 Cd1 O1 80.82(16) . . ? N4 Cd1 O1 96.58(14) 2_556 . ? N6 Cd1 N1 86.92(16) 4_565 . ? N6 Cd1 N1 92.57(14) . . ? N4 Cd1 N1 174.94(13) 2_556 . ? O1 Cd1 N1 86.23(12) . . ? N6 Cd1 N3 84.27(14) 4_565 3_556 ? N6 Cd1 N3 157.23(16) . 3_556 ? N4 Cd1 N3 92.92(13) 2_556 3_556 ? O1 Cd1 N3 77.18(12) . 3_556 ? N1 Cd1 N3 91.80(13) . 3_556 ? C1 N1 C5 118.3(4) . . ? C1 N1 Cd1 114.5(3) . . ? C5 N1 Cd1 123.1(3) . . ? C10 N2 N3 104.4(3) . . ? N4 N3 N2 109.4(3) . . ? N4 N3 Cd1 118.8(3) . 3_556 ? N2 N3 Cd1 124.3(3) . 3_556 ? N3 N4 N5 109.8(3) . . ? N3 N4 Cd1 124.1(3) . 2_546 ? N5 N4 Cd1 125.7(3) . 2_546 ? N4 N5 C10 104.6(3) . . ? N7 N6 Cd1 123.3(4) . 4_566 ? N7 N6 Cd1 112.8(3) . . ? Cd1 N6 Cd1 120.66(19) 4_566 . ? N8 N7 N6 175.7(6) . . ? Cd1 O1 H1A 121.7 . . ? Cd1 O1 H1B 114.9 . . ? H1A O1 H1B 110.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.782 _refine_diff_density_min -2.084 _refine_diff_density_rms 0.112 data_3 _database_code_depnum_ccdc_archive 'CCDC 804243' #TrackingRef '15239_web_deposit_cif_file_0_HongDeng_1352260642.cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H6 Cl N5 Zn ' _chemical_formula_sum 'C10 H6 Cl N5 Zn' _chemical_formula_weight 297.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 8.0261(10) _cell_length_b 8.7696(11) _cell_length_c 15.719(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.000(2) _cell_angle_gamma 90.00 _cell_volume 1092.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1971 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592.0 _exptl_absorpt_coefficient_mu 2.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.099 _exptl_absorpt_correction_T_max 0.121 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 5370 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.18 _reflns_number_total 1972 _reflns_number_gt 1637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0798P)^2^+2.0141P] 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 1971 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Zn1 Zn 0.28377(7) 0.82266(6) 1.18138(3) 0.0323(2) Uani 1 1 d . . . N1 N 0.2841(5) 0.7048(4) 1.0689(2) 0.0323(9) Uani 1 1 d . . . C9 C 0.2041(8) 0.3256(5) 0.9659(3) 0.0421(13) Uani 1 1 d . . . H9 H 0.2145 0.2758 0.9147 0.051 Uiso 1 1 calc R . . C1 C 0.3362(7) 0.7787(5) 1.0056(3) 0.0336(11) Uani 1 1 d . . . H1 H 0.3652 0.8808 1.0145 0.040 Uiso 1 1 calc R . . C7 C 0.1310(7) 0.3226(6) 1.1086(4) 0.0435(13) Uani 1 1 d . . . H7 H 0.0912 0.2688 1.1523 0.052 Uiso 1 1 calc R . . C2 C 0.3515(7) 0.7153(6) 0.9255(3) 0.0348(11) Uani 1 1 d . . . C4 C 0.2502(6) 0.4813(5) 0.9769(3) 0.0333(11) Uani 1 1 d . . . C6 C 0.1753(7) 0.4709(6) 1.1207(3) 0.0400(12) Uani 1 1 d . . . H6 H 0.1645 0.5185 1.1724 0.048 Uiso 1 1 calc R . . C5 C 0.2373(6) 0.5532(5) 1.0561(3) 0.0295(10) Uani 1 1 d . . . C3 C 0.3102(7) 0.5652(5) 0.9117(3) 0.0348(11) Uani 1 1 d . . . H3 H 0.3216 0.5190 0.8597 0.042 Uiso 1 1 calc R . . C8 C 0.1448(7) 0.2492(6) 1.0301(3) 0.0451(13) Uani 1 1 d . . . H8 H 0.1130 0.1476 1.0223 0.054 Uiso 1 1 calc R . . C10 C 0.4233(7) 0.8146(5) 0.8650(3) 0.0331(11) Uani 1 1 d . . . N2 N 0.5137(6) 0.9342(5) 0.8921(2) 0.0388(10) Uani 1 1 d . . . N3 N 0.4124(6) 0.7987(4) 0.7794(2) 0.0345(9) Uani 1 1 d . . . N4 N 0.5015(6) 0.9145(5) 0.7533(2) 0.0390(10) Uani 1 1 d . . . N5 N 0.5612(6) 0.9934(5) 0.8219(2) 0.0372(10) Uani 1 1 d . . . Cl1 Cl 0.0277(3) 0.9197(2) 1.19326(12) 0.0794(6) 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 0.0517(4) 0.0298(4) 0.0174(3) 0.00092(19) 0.0112(2) -0.0017(2) N1 0.046(2) 0.033(2) 0.0197(18) 0.0014(15) 0.0094(16) -0.0031(18) C9 0.059(4) 0.029(3) 0.039(3) -0.005(2) 0.010(3) -0.007(2) C1 0.052(3) 0.028(2) 0.021(2) -0.0014(18) 0.008(2) -0.005(2) C7 0.053(3) 0.038(3) 0.040(3) 0.011(2) 0.009(2) -0.010(2) C2 0.053(3) 0.035(3) 0.017(2) 0.0009(18) 0.008(2) -0.004(2) C4 0.044(3) 0.030(2) 0.026(2) -0.0005(19) 0.005(2) -0.003(2) C6 0.055(3) 0.038(3) 0.029(2) 0.004(2) 0.013(2) -0.003(2) C5 0.040(3) 0.026(2) 0.023(2) 0.0008(18) 0.0056(18) 0.0001(19) C3 0.054(3) 0.030(2) 0.021(2) -0.0057(19) 0.008(2) -0.005(2) C8 0.059(4) 0.028(3) 0.048(3) 0.002(2) 0.006(3) -0.008(2) C10 0.052(3) 0.032(2) 0.016(2) -0.0027(17) 0.008(2) -0.004(2) N2 0.060(3) 0.038(2) 0.0196(18) -0.0021(17) 0.0120(18) -0.012(2) N3 0.057(3) 0.029(2) 0.0201(19) -0.0022(15) 0.0133(18) -0.0052(18) N4 0.059(3) 0.038(2) 0.0208(19) -0.0001(17) 0.0108(18) -0.006(2) N5 0.060(3) 0.033(2) 0.0207(19) 0.0007(16) 0.0112(17) -0.0067(19) Cl1 0.0901(14) 0.0819(13) 0.0739(12) -0.0231(10) 0.0372(10) -0.0128(10) _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 N3 2.019(4) 4_576 ? Zn1 N5 2.043(4) 3_677 ? Zn1 N1 2.049(4) . ? Zn1 Cl1 2.259(2) . ? N1 C1 1.310(6) . ? N1 C5 1.388(6) . ? C9 C8 1.359(7) . ? C9 C4 1.418(7) . ? C9 H9 0.9300 . ? C1 C2 1.398(6) . ? C1 H1 0.9300 . ? C7 C6 1.354(7) . ? C7 C8 1.411(8) . ? C7 H7 0.9300 . ? C2 C3 1.367(7) . ? C2 C10 1.472(7) . ? C4 C3 1.406(7) . ? C4 C5 1.413(6) . ? C6 C5 1.399(6) . ? C6 H6 0.9300 . ? C3 H3 0.9300 . ? C8 H8 0.9300 . ? C10 N2 1.308(6) . ? C10 N3 1.342(6) . ? N2 N5 1.328(5) . ? N3 N4 1.343(6) . ? N3 Zn1 2.019(4) 4_575 ? N4 N5 1.307(5) . ? N5 Zn1 2.043(4) 3_677 ? 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 N3 Zn1 N5 101.25(17) 4_576 3_677 ? N3 Zn1 N1 108.87(16) 4_576 . ? N5 Zn1 N1 107.06(16) 3_677 . ? N3 Zn1 Cl1 119.90(13) 4_576 . ? N5 Zn1 Cl1 105.68(13) 3_677 . ? N1 Zn1 Cl1 112.67(14) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 Zn1 116.8(3) . . ? C5 N1 Zn1 124.9(3) . . ? C8 C9 C4 119.9(5) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N1 C1 C2 124.8(4) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C6 C7 C8 120.4(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C2 C1 118.2(4) . . ? C3 C2 C10 125.3(4) . . ? C1 C2 C10 116.4(4) . . ? C3 C4 C5 119.3(4) . . ? C3 C4 C9 121.8(4) . . ? C5 C4 C9 118.9(4) . . ? C7 C6 C5 120.6(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? N1 C5 C6 120.5(4) . . ? N1 C5 C4 120.0(4) . . ? C6 C5 C4 119.5(4) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N2 C10 N3 110.8(4) . . ? N2 C10 C2 121.2(4) . . ? N3 C10 C2 128.0(4) . . ? C10 N2 N5 105.0(4) . . ? C10 N3 N4 105.9(4) . . ? C10 N3 Zn1 140.0(4) . 4_575 ? N4 N3 Zn1 113.5(3) . 4_575 ? N5 N4 N3 107.0(3) . . ? N4 N5 N2 111.3(4) . . ? N4 N5 Zn1 122.9(3) . 3_677 ? N2 N5 Zn1 125.8(3) . 3_677 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.732 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.113 data_4 _database_code_depnum_ccdc_archive 'CCDC 804244' #TrackingRef '15239_web_deposit_cif_file_0_HongDeng_1352260642.cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Cd2 N12 O4,0.25(H2O)' _chemical_formula_sum 'C32 H20.5 Cd2 N12 O4.25' _chemical_formula_weight 865.92 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' Cd Cd -0.8075 1.2024 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3824(13) _cell_length_b 13.4516(19) _cell_length_c 14.717(2) _cell_angle_alpha 112.547(2) _cell_angle_beta 96.925(2) _cell_angle_gamma 101.903(2) _cell_volume 1637.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5790 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 853.0 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8448 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5790 _reflns_number_gt 4847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0356P)^2^+0.5591P] 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 5790 _refine_ls_number_parameters 460 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.7095(4) 0.7220(3) 0.2692(3) 0.0322(8) Uani 1 1 d . . . C2 C 0.7408(4) 0.6788(3) 0.3474(3) 0.0392(9) Uani 1 1 d . . . C3 C 0.8856(5) 0.6870(4) 0.3881(3) 0.0556(12) Uani 1 1 d . . . H3 H 0.9652 0.7181 0.3665 0.067 Uiso 1 1 calc R . . C4 C 0.9104(7) 0.6485(5) 0.4611(4) 0.0840(18) Uani 1 1 d . . . H4 H 1.0085 0.6543 0.4875 0.101 Uiso 1 1 calc R . . C5 C 0.6661(7) 0.5946(6) 0.4553(5) 0.106(2) Uani 1 1 d U . . H5 H 0.5884 0.5625 0.4778 0.128 Uiso 1 1 calc R . . C6 C 0.6299(6) 0.6299(5) 0.3813(4) 0.0799(18) Uani 1 1 d . . . H6 H 0.5305 0.6203 0.3546 0.096 Uiso 1 1 calc R . . C7 C 0.3056(5) 0.8026(3) 0.3855(3) 0.0417(10) Uani 1 1 d . . . C8 C 0.3013(4) 0.8771(3) 0.4915(3) 0.0372(9) Uani 1 1 d . . . C9 C 0.3871(6) 0.8817(4) 0.5746(3) 0.0692(15) Uani 1 1 d . . . H9 H 0.4513 0.8363 0.5681 0.083 Uiso 1 1 calc R . . C10 C 0.3788(6) 0.9542(4) 0.6691(3) 0.0665(15) Uani 1 1 d . . . H10 H 0.4414 0.9576 0.7249 0.080 Uiso 1 1 calc R . . C11 C 0.2019(6) 1.0099(4) 0.6031(3) 0.0636(14) Uani 1 1 d . . . H11 H 0.1343 1.0528 0.6117 0.076 Uiso 1 1 calc R . . C12 C 0.2052(6) 0.9424(4) 0.5067(3) 0.0613(13) Uani 1 1 d . . . H12 H 0.1425 0.9411 0.4520 0.074 Uiso 1 1 calc R . . C13 C 0.2740(4) 0.4168(3) 0.0103(2) 0.0252(7) Uani 1 1 d . . . C14 C 0.1899(4) 0.4470(3) -0.0617(2) 0.0262(7) Uani 1 1 d . . . C15 C 0.0356(4) 0.3969(3) -0.0982(2) 0.0291(8) Uani 1 1 d . . . H15 H -0.0088 0.3421 -0.0786 0.035 Uiso 1 1 calc R . . C16 C 0.0153(4) 0.5009(3) -0.1911(3) 0.0305(8) Uani 1 1 d . . . C17 C -0.0718(5) 0.5286(3) -0.2571(3) 0.0425(9) Uani 1 1 d . . . H17 H -0.1747 0.4970 -0.2763 0.051 Uiso 1 1 calc R . . C18 C -0.0061(5) 0.6021(4) -0.2934(3) 0.0543(12) Uani 1 1 d . . . H18 H -0.0647 0.6196 -0.3375 0.065 Uiso 1 1 calc R . . C19 C 0.1480(5) 0.6508(4) -0.2647(3) 0.0579(12) Uani 1 1 d . . . H19 H 0.1911 0.7001 -0.2904 0.069 Uiso 1 1 calc R . . C20 C 0.2358(5) 0.6273(3) -0.2000(3) 0.0464(10) Uani 1 1 d . . . H20 H 0.3384 0.6603 -0.1814 0.056 Uiso 1 1 calc R . . C21 C 0.1703(4) 0.5518(3) -0.1607(3) 0.0319(8) Uani 1 1 d . . . C22 C 0.2568(4) 0.5246(3) -0.0934(3) 0.0305(8) Uani 1 1 d . . . H22 H 0.3589 0.5591 -0.0706 0.037 Uiso 1 1 calc R . . C23 C 0.7330(4) 1.1452(3) -0.0218(3) 0.0299(8) Uani 1 1 d . . . C24 C 0.8235(4) 1.1041(3) 0.0374(3) 0.0298(8) Uani 1 1 d . . . C25 C 0.7562(4) 1.0112(3) 0.0539(3) 0.0315(8) Uani 1 1 d . . . H25 H 0.6557 0.9753 0.0241 0.038 Uiso 1 1 calc R . . C26 C 0.9765(4) 1.0223(3) 0.1532(3) 0.0307(8) Uani 1 1 d . . . C27 C 1.0563(4) 0.9807(3) 0.2115(3) 0.0395(9) Uani 1 1 d . . . H27 H 1.0083 0.9174 0.2189 0.047 Uiso 1 1 calc R . . C28 C 1.2020(5) 1.0322(4) 0.2565(3) 0.0520(11) Uani 1 1 d . . . H28 H 1.2537 1.0036 0.2940 0.062 Uiso 1 1 calc R . . C29 C 1.2759(5) 1.1283(4) 0.2471(4) 0.0606(13) Uani 1 1 d . . . H29 H 1.3752 1.1643 0.2806 0.073 Uiso 1 1 calc R . . C30 C 1.2045(4) 1.1702(4) 0.1896(4) 0.0531(12) Uani 1 1 d . . . H30 H 1.2557 1.2329 0.1825 0.064 Uiso 1 1 calc R . . C31 C 1.0526(4) 1.1176(3) 0.1409(3) 0.0365(9) Uani 1 1 d . . . C32 C 0.9718(4) 1.1561(3) 0.0802(3) 0.0366(9) Uani 1 1 d . . . H32 H 1.0196 1.2171 0.0693 0.044 Uiso 1 1 calc R . . Cd1 Cd 0.31330(3) 0.662517(19) 0.198439(17) 0.02640(8) Uani 1 1 d . . . Cd2 Cd 0.69411(3) 0.835970(19) 0.150074(18) 0.02739(8) Uani 1 1 d . . . N1 N 0.8031(6) 0.6036(5) 0.4962(4) 0.1070(19) Uani 1 1 d . . . N2 N 0.2891(4) 1.0180(3) 0.6850(2) 0.0401(8) Uani 1 1 d . . . N3 N -0.0506(3) 0.4228(2) -0.1590(2) 0.0308(7) Uani 1 1 d . . . N4 N 0.3299(3) 0.4866(2) 0.1069(2) 0.0295(6) Uani 1 1 d . . . N5 N 0.3937(3) 0.4284(2) 0.1495(2) 0.0352(7) Uani 1 1 d . . . N6 N 0.3765(3) 0.3292(2) 0.0815(2) 0.0329(7) Uani 1 1 d . . . N7 N 0.3014(3) 0.3185(2) -0.0078(2) 0.0301(7) Uani 1 1 d . . . N8 N 0.8280(3) 0.9714(2) 0.1096(2) 0.0295(6) Uani 1 1 d . . . N9 N 0.5851(3) 1.1119(2) -0.0477(2) 0.0350(7) Uani 1 1 d . . . N10 N 0.5483(3) 1.1708(2) -0.0972(2) 0.0322(7) Uani 1 1 d . . . N11 N 0.6712(3) 1.2377(2) -0.1002(2) 0.0305(7) Uani 1 1 d . . . N12 N 0.7898(3) 1.2229(2) -0.0531(2) 0.0338(7) Uani 1 1 d . . . O1 O 0.8202(3) 0.7694(2) 0.24631(18) 0.0350(6) Uani 1 1 d . . . O2 O 0.5778(3) 0.7125(2) 0.2303(2) 0.0429(7) Uani 1 1 d . . . O3 O 0.2759(5) 0.8313(3) 0.3172(2) 0.0696(10) Uani 1 1 d . . . O4 O 0.3361(4) 0.7120(2) 0.3708(2) 0.0551(8) Uani 1 1 d . . . O1W O 0.2995(13) 0.6335(9) 0.5256(8) 0.051(3) Uani 0.25 1 d P . . H1WA H 0.3078 0.6441 0.4729 0.076 Uiso 0.25 1 d PR . . H1WB H 0.2528 0.5652 0.5069 0.076 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(2) 0.0275(18) 0.0299(19) 0.0112(16) 0.0051(17) 0.0101(16) C2 0.038(2) 0.047(2) 0.041(2) 0.0257(19) 0.0073(18) 0.0147(19) C3 0.047(3) 0.076(3) 0.053(3) 0.040(3) 0.004(2) 0.017(2) C4 0.066(4) 0.129(5) 0.083(4) 0.074(4) -0.001(3) 0.033(4) C5 0.089(4) 0.171(6) 0.123(5) 0.122(5) 0.034(4) 0.042(4) C6 0.053(3) 0.135(5) 0.102(4) 0.098(4) 0.024(3) 0.031(3) C7 0.043(2) 0.041(2) 0.032(2) 0.0075(18) 0.0069(18) 0.0076(19) C8 0.043(2) 0.034(2) 0.0302(19) 0.0093(16) 0.0064(17) 0.0105(17) C9 0.088(4) 0.083(4) 0.039(2) 0.010(2) 0.006(3) 0.063(3) C10 0.092(4) 0.078(3) 0.028(2) 0.008(2) -0.001(2) 0.055(3) C11 0.070(3) 0.065(3) 0.042(3) 0.001(2) -0.003(2) 0.042(3) C12 0.080(4) 0.062(3) 0.033(2) 0.006(2) -0.003(2) 0.038(3) C13 0.0227(18) 0.0258(18) 0.0291(18) 0.0131(15) 0.0079(14) 0.0064(14) C14 0.0288(19) 0.0266(17) 0.0241(17) 0.0098(14) 0.0074(15) 0.0102(15) C15 0.0288(19) 0.0293(18) 0.0301(18) 0.0135(15) 0.0066(15) 0.0080(15) C16 0.034(2) 0.0330(19) 0.0287(18) 0.0152(16) 0.0081(16) 0.0119(16) C17 0.042(2) 0.045(2) 0.042(2) 0.0234(19) 0.0006(19) 0.0105(19) C18 0.061(3) 0.066(3) 0.050(3) 0.041(2) 0.003(2) 0.019(2) C19 0.067(3) 0.065(3) 0.058(3) 0.048(3) 0.011(2) 0.009(2) C20 0.041(2) 0.053(3) 0.049(2) 0.032(2) 0.007(2) 0.004(2) C21 0.036(2) 0.0329(19) 0.0295(18) 0.0161(16) 0.0082(16) 0.0088(16) C22 0.0263(19) 0.0298(19) 0.0311(19) 0.0116(16) 0.0032(15) 0.0030(15) C23 0.032(2) 0.0309(19) 0.0325(19) 0.0185(16) 0.0068(16) 0.0101(16) C24 0.029(2) 0.0347(19) 0.0339(19) 0.0214(16) 0.0089(16) 0.0103(16) C25 0.029(2) 0.0352(19) 0.0336(19) 0.0189(16) 0.0056(16) 0.0068(16) C26 0.030(2) 0.0342(19) 0.035(2) 0.0209(16) 0.0092(16) 0.0096(16) C27 0.038(2) 0.039(2) 0.051(2) 0.0295(19) 0.0092(19) 0.0110(18) C28 0.037(2) 0.066(3) 0.070(3) 0.049(3) 0.003(2) 0.015(2) C29 0.031(2) 0.076(3) 0.084(3) 0.054(3) -0.009(2) 0.004(2) C30 0.029(2) 0.059(3) 0.081(3) 0.050(3) 0.000(2) 0.000(2) C31 0.028(2) 0.042(2) 0.048(2) 0.0305(19) 0.0058(17) 0.0066(17) C32 0.036(2) 0.039(2) 0.046(2) 0.0306(19) 0.0083(18) 0.0071(17) Cd1 0.02953(15) 0.02598(14) 0.02408(14) 0.01106(11) 0.00435(11) 0.00830(11) Cd2 0.03084(16) 0.02577(14) 0.02781(14) 0.01359(11) 0.00552(11) 0.00833(11) N1 0.091(4) 0.185(6) 0.108(4) 0.120(4) 0.023(3) 0.051(4) N2 0.048(2) 0.0405(18) 0.0307(17) 0.0108(14) 0.0077(15) 0.0182(16) N3 0.0315(17) 0.0305(16) 0.0332(16) 0.0155(14) 0.0068(14) 0.0104(13) N4 0.0306(16) 0.0308(16) 0.0286(15) 0.0130(13) 0.0044(13) 0.0116(13) N5 0.0396(18) 0.0369(17) 0.0316(16) 0.0155(14) 0.0059(14) 0.0149(14) N6 0.0385(18) 0.0331(17) 0.0324(16) 0.0174(14) 0.0081(14) 0.0133(14) N7 0.0343(17) 0.0264(15) 0.0328(16) 0.0146(13) 0.0088(14) 0.0104(13) N8 0.0327(17) 0.0283(15) 0.0326(16) 0.0189(13) 0.0074(13) 0.0069(13) N9 0.0296(17) 0.0412(18) 0.0462(19) 0.0309(16) 0.0071(14) 0.0103(14) N10 0.0321(17) 0.0361(17) 0.0354(17) 0.0226(14) 0.0059(14) 0.0097(14) N11 0.0305(17) 0.0327(16) 0.0321(16) 0.0177(13) 0.0066(13) 0.0087(13) N12 0.0282(17) 0.0407(17) 0.0417(18) 0.0279(15) 0.0077(14) 0.0076(14) O1 0.0341(15) 0.0379(14) 0.0379(14) 0.0198(12) 0.0093(12) 0.0116(12) O2 0.0316(15) 0.0546(17) 0.0491(16) 0.0330(14) 0.0002(13) 0.0081(13) O3 0.130(3) 0.0519(19) 0.0330(16) 0.0179(15) 0.0213(19) 0.035(2) O4 0.074(2) 0.0527(18) 0.0354(15) 0.0089(14) 0.0109(15) 0.0309(16) O1W 0.073(8) 0.053(7) 0.037(6) 0.036(6) 0.007(6) 0.007(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 C1 O1 1.255(4) . ? C1 O2 1.256(4) . ? C1 C2 1.500(5) . ? C2 C6 1.363(6) . ? C2 C3 1.382(6) . ? C3 C4 1.376(6) . ? C3 H3 0.9300 . ? C4 N1 1.326(7) . ? C4 H4 0.9300 . ? C5 N1 1.313(7) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O3 1.229(5) . ? C7 O4 1.253(5) . ? C7 C8 1.507(5) . ? C8 C9 1.354(6) . ? C8 C12 1.364(6) . ? C9 C10 1.382(6) . ? C9 H9 0.9300 . ? C10 N2 1.300(5) . ? C10 H10 0.9300 . ? C11 N2 1.327(5) . ? C11 C12 1.368(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N4 1.331(4) . ? C13 N7 1.331(4) . ? C13 C14 1.473(5) . ? C14 C22 1.369(5) . ? C14 C15 1.404(5) . ? C15 N3 1.325(4) . ? C15 H15 0.9300 . ? C16 N3 1.376(4) . ? C16 C17 1.401(5) . ? C16 C21 1.408(5) . ? C17 C18 1.369(6) . ? C17 H17 0.9300 . ? C18 C19 1.396(6) . ? C18 H18 0.9300 . ? C19 C20 1.355(6) . ? C19 H19 0.9300 . ? C20 C21 1.421(5) . ? C20 H20 0.9300 . ? C21 C22 1.408(5) . ? C22 H22 0.9300 . ? C23 N9 1.326(4) . ? C23 N12 1.338(4) . ? C23 C24 1.473(5) . ? C24 C32 1.368(5) . ? C24 C25 1.402(5) . ? C25 N8 1.329(4) . ? C25 H25 0.9300 . ? C26 N8 1.369(4) . ? C26 C27 1.414(5) . ? C26 C31 1.420(5) . ? C27 C28 1.351(5) . ? C27 H27 0.9300 . ? C28 C29 1.400(6) . ? C28 H28 0.9300 . ? C29 C30 1.367(6) . ? C29 H29 0.9300 . ? C30 C31 1.413(5) . ? C30 H30 0.9300 . ? C31 C32 1.411(5) . ? C32 H32 0.9300 . ? Cd1 N4 2.280(3) . ? Cd1 N11 2.317(3) 2_675 ? Cd1 O4 2.332(3) . ? Cd1 O2 2.371(3) . ? Cd1 N3 2.388(3) 2_565 ? Cd1 O3 2.401(3) . ? Cd2 O1 2.284(2) . ? Cd2 N10 2.285(3) 2_675 ? Cd2 N8 2.306(3) . ? Cd2 N7 2.329(3) 2_665 ? Cd2 N2 2.429(3) 2_676 ? Cd2 O2 2.533(3) . ? N2 Cd2 2.429(3) 2_676 ? N3 Cd1 2.388(3) 2_565 ? N4 N5 1.358(4) . ? N5 N6 1.287(4) . ? N6 N7 1.355(4) . ? N7 Cd2 2.329(3) 2_665 ? N9 N10 1.332(4) . ? N10 N11 1.325(4) . ? N10 Cd2 2.285(3) 2_675 ? N11 N12 1.330(4) . ? N11 Cd1 2.317(3) 2_675 ? O1W H1WA 0.8499 . ? O1W H1WB 0.8501 . ? 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 C1 O2 122.1(3) . . ? O1 C1 C2 117.0(3) . . ? O2 C1 C2 120.9(3) . . ? C6 C2 C3 117.0(4) . . ? C6 C2 C1 122.4(4) . . ? C3 C2 C1 120.6(4) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? N1 C4 C3 124.0(5) . . ? N1 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? N1 C5 C6 124.2(5) . . ? N1 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C2 C6 C5 119.6(5) . . ? C2 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? O3 C7 O4 122.8(4) . . ? O3 C7 C8 119.2(4) . . ? O4 C7 C8 117.9(4) . . ? C9 C8 C12 117.0(4) . . ? C9 C8 C7 123.2(4) . . ? C12 C8 C7 119.8(4) . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 124.2(4) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? N2 C11 C12 124.0(4) . . ? N2 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C8 C12 C11 119.5(4) . . ? C8 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N4 C13 N7 109.9(3) . . ? N4 C13 C14 123.0(3) . . ? N7 C13 C14 127.1(3) . . ? C22 C14 C15 118.2(3) . . ? C22 C14 C13 122.1(3) . . ? C15 C14 C13 119.6(3) . . ? N3 C15 C14 124.0(3) . . ? N3 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? N3 C16 C17 119.9(3) . . ? N3 C16 C21 121.0(3) . . ? C17 C16 C21 119.1(3) . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C16 118.7(3) . . ? C22 C21 C20 121.7(3) . . ? C16 C21 C20 119.5(3) . . ? C14 C22 C21 119.7(3) . . ? C14 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N9 C23 N12 111.9(3) . . ? N9 C23 C24 123.9(3) . . ? N12 C23 C24 124.1(3) . . ? C32 C24 C25 118.2(3) . . ? C32 C24 C23 122.0(3) . . ? C25 C24 C23 119.7(3) . . ? N8 C25 C24 123.6(3) . . ? N8 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N8 C26 C27 120.2(3) . . ? N8 C26 C31 120.8(3) . . ? C27 C26 C31 119.0(3) . . ? C28 C27 C26 120.4(4) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.7(4) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 122.7(3) . . ? C32 C31 C26 118.1(3) . . ? C30 C31 C26 119.2(3) . . ? C24 C32 C31 120.2(3) . . ? C24 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? N4 Cd1 N11 109.27(10) . 2_675 ? N4 Cd1 O4 114.97(10) . . ? N11 Cd1 O4 134.17(10) 2_675 . ? N4 Cd1 O2 84.46(10) . . ? N11 Cd1 O2 85.50(9) 2_675 . ? O4 Cd1 O2 87.36(10) . . ? N4 Cd1 N3 85.38(10) . 2_565 ? N11 Cd1 N3 101.44(10) 2_675 2_565 ? O4 Cd1 N3 93.53(10) . 2_565 ? O2 Cd1 N3 169.16(9) . 2_565 ? N4 Cd1 O3 168.14(10) . . ? N11 Cd1 O3 82.12(10) 2_675 . ? O4 Cd1 O3 54.82(10) . . ? O2 Cd1 O3 100.13(12) . . ? N3 Cd1 O3 89.14(12) 2_565 . ? O1 Cd2 N10 137.19(9) . 2_675 ? O1 Cd2 N8 118.63(9) . . ? N10 Cd2 N8 103.23(10) 2_675 . ? O1 Cd2 N7 88.27(9) . 2_665 ? N10 Cd2 N7 95.55(10) 2_675 2_665 ? N8 Cd2 N7 96.99(10) . 2_665 ? O1 Cd2 N2 81.63(10) . 2_676 ? N10 Cd2 N2 91.55(11) 2_675 2_676 ? N8 Cd2 N2 88.36(10) . 2_676 ? N7 Cd2 N2 169.89(10) 2_665 2_676 ? O1 Cd2 O2 53.99(8) . . ? N10 Cd2 O2 83.24(9) 2_675 . ? N8 Cd2 O2 168.39(9) . . ? N7 Cd2 O2 91.91(9) 2_665 . ? N2 Cd2 O2 81.76(10) 2_676 . ? C5 N1 C4 116.0(5) . . ? C10 N2 C11 115.7(4) . . ? C10 N2 Cd2 122.6(3) . 2_676 ? C11 N2 Cd2 121.0(3) . 2_676 ? C15 N3 C16 118.3(3) . . ? C15 N3 Cd1 117.5(2) . 2_565 ? C16 N3 Cd1 124.2(2) . 2_565 ? C13 N4 N5 106.0(3) . . ? C13 N4 Cd1 131.2(2) . . ? N5 N4 Cd1 122.6(2) . . ? N6 N5 N4 108.8(3) . . ? N5 N6 N7 109.6(3) . . ? C13 N7 N6 105.7(3) . . ? C13 N7 Cd2 136.0(2) . 2_665 ? N6 N7 Cd2 116.1(2) . 2_665 ? C25 N8 C26 119.0(3) . . ? C25 N8 Cd2 119.3(2) . . ? C26 N8 Cd2 121.0(2) . . ? C23 N9 N10 104.7(3) . . ? N11 N10 N9 109.4(3) . . ? N11 N10 Cd2 128.0(2) . 2_675 ? N9 N10 Cd2 122.2(2) . 2_675 ? N10 N11 N12 109.3(3) . . ? N10 N11 Cd1 126.3(2) . 2_675 ? N12 N11 Cd1 123.3(2) . 2_675 ? N11 N12 C23 104.6(3) . . ? C1 O1 Cd2 97.5(2) . . ? C1 O2 Cd1 158.6(2) . . ? C1 O2 Cd2 85.9(2) . . ? Cd1 O2 Cd2 115.28(10) . . ? C7 O3 Cd1 89.8(2) . . ? C7 O4 Cd1 92.5(2) . . ? H1WA O1W H1WB 107.7 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.554 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.081 data_5 _database_code_depnum_ccdc_archive 'CCDC 804245' #TrackingRef '15239_web_deposit_cif_file_0_HongDeng_1352260642.cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H4 Cd2 N5 O8, 1.67(H2 O)' _chemical_formula_sum 'C19 H7.34 Cd2 N5 O9.67' _chemical_formula_weight 685.17 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' H H 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.0822(11) _cell_length_b 10.2910(12) _cell_length_c 11.6096(13) _cell_angle_alpha 102.7390(10) _cell_angle_beta 107.2230(10) _cell_angle_gamma 90.8240(10) _cell_volume 1118.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4206 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.200 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 659.1 _exptl_absorpt_coefficient_mu 1.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.569 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5756 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3951 _reflns_number_gt 3571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0505P)^2^+1.5420P] 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 4033 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 C1 C 0.6555(4) 0.2864(4) 0.5013(4) 0.0261(9) Uani 1 1 d . . . C2 C 0.5904(4) 0.2511(4) 0.5880(4) 0.0257(8) Uani 1 1 d . . . C3 C 0.5072(5) 0.3456(4) 0.6354(4) 0.0300(9) Uani 1 1 d . . . C4 C 0.4502(4) 0.2064(4) 0.7498(4) 0.0264(9) Uani 1 1 d . . . C5 C 0.3783(5) 0.1846(5) 0.8328(4) 0.0374(11) Uani 1 1 d . . . C6 C 0.3854(5) 0.0658(5) 0.8685(4) 0.0419(12) Uani 1 1 d . . . C7 C 0.4628(6) -0.0356(5) 0.8232(5) 0.0458(12) Uani 1 1 d . . . C8 C 0.5340(5) -0.0168(5) 0.7435(4) 0.0376(11) Uani 1 1 d . . . C9 C 0.5290(4) 0.1071(4) 0.7053(4) 0.0267(9) Uani 1 1 d . . . C10 C 0.6014(4) 0.1315(4) 0.6239(4) 0.0280(9) Uani 1 1 d . . . C11 C 0.7650(4) 0.3498(4) 0.0330(4) 0.0271(9) Uani 1 1 d . . . C12 C 0.8367(4) 0.3034(4) -0.0629(3) 0.0219(8) Uani 1 1 d . . . C13 C 0.8717(4) 0.1727(4) -0.0890(4) 0.0243(8) Uani 1 1 d . . . C14 C 0.9469(4) 0.1348(4) -0.1725(4) 0.0239(8) Uani 1 1 d . . . C15 C 0.9834(4) -0.0071(4) -0.2044(4) 0.0284(9) Uani 1 1 d . . . C16 C 0.9890(4) 0.2285(4) -0.2279(4) 0.0242(8) Uani 1 1 d . . . C17 C 0.9528(4) 0.3588(4) -0.2031(4) 0.0222(8) Uani 1 1 d . . . C18 C 1.0044(4) 0.4612(4) -0.2579(4) 0.0254(9) Uani 1 1 d . . . C19 C 0.8750(4) 0.3968(4) -0.1216(3) 0.0217(8) Uani 1 1 d . . . Cd1 Cd 0.66157(3) 0.49035(3) 0.21613(3) 0.02620(11) Uani 1 1 d . . . Cd2 Cd 1.05196(3) -0.25632(3) -0.28539(3) 0.02407(11) Uani 1 1 d . . . N1 N 0.6099(4) 0.3781(4) 0.4381(3) 0.0329(8) Uani 1 1 d . . . N2 N 0.6934(4) 0.3794(4) 0.3684(3) 0.0289(8) Uani 1 1 d . . . N3 N 0.7861(4) 0.2920(4) 0.3894(3) 0.0294(8) Uani 1 1 d . . . N4 N 0.7656(4) 0.2310(4) 0.4736(3) 0.0317(8) Uani 1 1 d . . . N5 N 0.4399(4) 0.3253(4) 0.7127(3) 0.0287(8) Uani 1 1 d . . . O1 O 0.7631(3) 0.2812(3) 0.1099(3) 0.0305(7) Uani 1 1 d . . . O2 O 0.7119(3) 0.4611(3) 0.0370(3) 0.0327(7) Uani 1 1 d . . . O3 O 0.9301(4) -0.0974(3) -0.1715(3) 0.0450(9) Uani 1 1 d . . . O4 O 1.0681(3) -0.0322(3) -0.2655(3) 0.0403(8) Uani 1 1 d . . . O5 O 1.1001(3) 0.4347(3) -0.3065(3) 0.0325(7) Uani 1 1 d . . . O6 O 0.95149(17) 0.57170(17) -0.24744(16) 0.0370(7) Uani 1 1 d . . . O1W O 0.44228(17) 0.39011(17) 0.11698(16) 0.0474(9) Uani 1 1 d R . . H1B H 0.3893 0.4325 0.0698 0.071 Uiso 1 1 d R . . H1A H 0.3895 0.3464 0.1424 0.071 Uiso 1 1 d R . . O2W O 0.87508(17) -0.28103(17) -0.46956(16) 0.0443(8) Uani 1 1 d R . . H2B H 0.8603 -0.2064 -0.4886 0.066 Uiso 1 1 d R . . H2A H 0.8999 -0.3288 -0.5280 0.066 Uiso 1 1 d R . . O3W O 0.83937(17) 0.95511(17) 0.45929(16) 0.0667(12) Uani 1 1 d R . . H3A H 0.8826 1.0319 0.4932 0.100 Uiso 1 1 d R . . H3B H 0.7597 0.9621 0.4703 0.100 Uiso 1 1 d R . . O4W O 0.29466(17) 0.29052(17) 0.23832(16) 0.081(2) Uani 0.67 1 d PR . . H4A H 0.2459 0.2775 0.1626 0.122 Uiso 0.67 1 d PR . . H4B H 0.2819 0.3695 0.2719 0.122 Uiso 0.67 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(2) 0.026(2) 0.028(2) 0.0079(17) 0.0170(17) 0.0097(17) C2 0.030(2) 0.026(2) 0.025(2) 0.0075(16) 0.0147(17) 0.0054(17) C3 0.037(2) 0.030(2) 0.034(2) 0.0120(18) 0.0234(19) 0.0112(19) C4 0.027(2) 0.030(2) 0.025(2) 0.0079(17) 0.0102(16) -0.0009(17) C5 0.036(2) 0.047(3) 0.035(2) 0.015(2) 0.016(2) -0.002(2) C6 0.046(3) 0.051(3) 0.032(2) 0.018(2) 0.012(2) -0.007(2) C7 0.057(3) 0.040(3) 0.042(3) 0.018(2) 0.010(2) -0.006(2) C8 0.046(3) 0.031(2) 0.040(3) 0.015(2) 0.014(2) 0.000(2) C9 0.029(2) 0.024(2) 0.027(2) 0.0072(16) 0.0080(17) 0.0011(17) C10 0.034(2) 0.026(2) 0.028(2) 0.0091(17) 0.0135(18) 0.0081(18) C11 0.027(2) 0.033(2) 0.024(2) 0.0076(17) 0.0125(17) 0.0020(18) C12 0.026(2) 0.0212(19) 0.0217(19) 0.0052(15) 0.0113(15) 0.0034(16) C13 0.027(2) 0.024(2) 0.026(2) 0.0093(16) 0.0130(16) 0.0045(16) C14 0.028(2) 0.018(2) 0.027(2) 0.0035(15) 0.0122(16) 0.0034(16) C15 0.032(2) 0.022(2) 0.030(2) 0.0057(17) 0.0078(18) 0.0071(17) C16 0.028(2) 0.021(2) 0.025(2) 0.0032(16) 0.0125(16) 0.0019(16) C17 0.025(2) 0.0181(19) 0.028(2) 0.0061(15) 0.0129(16) 0.0016(15) C18 0.030(2) 0.024(2) 0.025(2) 0.0058(16) 0.0124(17) -0.0015(17) C19 0.025(2) 0.0202(19) 0.0208(19) 0.0035(15) 0.0100(16) 0.0027(16) Cd1 0.03022(18) 0.03058(19) 0.02788(18) 0.01206(13) 0.01978(13) 0.01163(13) Cd2 0.03112(18) 0.01846(17) 0.03193(18) 0.00993(12) 0.02038(13) 0.00786(12) N1 0.039(2) 0.038(2) 0.039(2) 0.0208(17) 0.0276(17) 0.0186(17) N2 0.0339(19) 0.0320(19) 0.0339(19) 0.0169(15) 0.0227(16) 0.0139(16) N3 0.0334(19) 0.035(2) 0.0319(19) 0.0138(16) 0.0228(16) 0.0132(16) N4 0.041(2) 0.036(2) 0.034(2) 0.0193(16) 0.0251(17) 0.0172(17) N5 0.0352(19) 0.0296(19) 0.0311(19) 0.0124(15) 0.0207(16) 0.0096(16) O1 0.0356(16) 0.0357(17) 0.0288(15) 0.0133(13) 0.0185(13) 0.0051(13) O2 0.0449(18) 0.0322(17) 0.0312(16) 0.0093(13) 0.0250(14) 0.0156(14) O3 0.070(2) 0.0207(16) 0.061(2) 0.0154(15) 0.041(2) 0.0081(16) O4 0.050(2) 0.0230(16) 0.062(2) 0.0089(14) 0.0384(18) 0.0112(14) O5 0.0356(16) 0.0341(17) 0.0334(16) 0.0035(13) 0.0224(13) -0.0043(13) O6 0.0431(18) 0.0255(16) 0.057(2) 0.0182(14) 0.0302(16) 0.0100(14) O1W 0.0336(18) 0.048(2) 0.058(2) 0.0142(17) 0.0098(16) 0.0049(15) O2W 0.0442(19) 0.050(2) 0.0353(18) 0.0031(15) 0.0115(15) 0.0097(16) O3W 0.071(3) 0.050(2) 0.081(3) 0.016(2) 0.027(2) 0.017(2) O4W 0.050(4) 0.051(4) 0.183(8) 0.052(4) 0.076(5) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(5) . ? C1 N4 1.345(5) . ? C1 C2 1.457(5) . ? C2 C10 1.380(6) . ? C2 C3 1.419(6) . ? C3 N5 1.323(5) . ? C4 N5 1.380(5) . ? C4 C9 1.406(6) . ? C4 C5 1.418(6) . ? C5 C6 1.372(7) . ? C6 C7 1.414(8) . ? C7 C8 1.370(7) . ? C8 C9 1.436(6) . ? C9 C10 1.413(6) . ? C11 O1 1.259(5) . ? C11 O2 1.269(5) . ? C11 C12 1.497(5) . ? C12 C13 1.387(5) . ? C12 C19 1.404(5) . ? C13 C14 1.394(5) . ? C14 C16 1.395(6) . ? C14 C15 1.505(5) . ? C15 O3 1.249(5) . ? C15 O4 1.259(5) . ? C16 C17 1.386(5) . ? C17 C19 1.396(5) . ? C17 C18 1.503(5) . ? C18 O5 1.259(5) . ? C18 O6 1.260(4) . ? Cd1 O2 2.242(3) . ? Cd1 N2 2.257(3) . ? Cd1 O1W 2.2761(17) . ? Cd1 N5 2.279(3) 2_666 ? Cd1 O5 2.360(3) 2_765 ? Cd1 O1 2.616(3) . ? Cd2 O6 2.2156(18) 1_545 ? Cd2 O4 2.265(3) . ? Cd2 N3 2.291(3) 2_755 ? Cd2 O2W 2.3034(18) . ? Cd2 O1 2.385(3) 2_755 ? Cd2 O3 2.449(3) . ? N1 N2 1.332(5) . ? N2 N3 1.314(5) . ? N3 N4 1.334(5) . ? N3 Cd2 2.291(3) 2_755 ? N5 Cd1 2.279(3) 2_666 ? O1 Cd2 2.385(3) 2_755 ? O5 Cd1 2.360(3) 2_765 ? O6 Cd2 2.2156(18) 1_565 ? O1W H1B 0.8448 . ? O1W H1A 0.8471 . ? O2W H2B 0.8483 . ? O2W H2A 0.8496 . ? O3W H3A 0.8490 . ? O3W H3B 0.8515 . ? O4W H4A 0.8504 . ? O4W H4B 0.8493 . ? 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 C1 N4 111.7(4) . . ? N1 C1 C2 122.8(3) . . ? N4 C1 C2 125.5(4) . . ? C10 C2 C3 118.5(4) . . ? C10 C2 C1 124.4(4) . . ? C3 C2 C1 117.1(4) . . ? N5 C3 C2 123.4(4) . . ? N5 C4 C9 121.0(4) . . ? N5 C4 C5 118.9(4) . . ? C9 C4 C5 120.1(4) . . ? C6 C5 C4 119.5(5) . . ? C5 C6 C7 120.9(4) . . ? C8 C7 C6 120.7(4) . . ? C7 C8 C9 119.5(4) . . ? C4 C9 C10 119.2(4) . . ? C4 C9 C8 119.2(4) . . ? C10 C9 C8 121.6(4) . . ? C2 C10 C9 119.1(4) . . ? O1 C11 O2 121.7(4) . . ? O1 C11 C12 120.0(4) . . ? O2 C11 C12 118.3(3) . . ? C13 C12 C19 120.2(3) . . ? C13 C12 C11 121.0(3) . . ? C19 C12 C11 118.7(3) . . ? C12 C13 C14 119.7(4) . . ? C13 C14 C16 120.2(4) . . ? C13 C14 C15 120.7(4) . . ? C16 C14 C15 119.1(4) . . ? O3 C15 O4 121.1(4) . . ? O3 C15 C14 120.7(4) . . ? O4 C15 C14 118.2(4) . . ? C17 C16 C14 120.2(4) . . ? C16 C17 C19 119.9(4) . . ? C16 C17 C18 120.0(3) . . ? C19 C17 C18 120.0(3) . . ? O5 C18 O6 124.0(4) . . ? O5 C18 C17 119.2(4) . . ? O6 C18 C17 116.8(3) . . ? C17 C19 C12 119.7(3) . . ? O2 Cd1 N2 135.88(11) . . ? O2 Cd1 O1W 91.78(9) . . ? N2 Cd1 O1W 92.44(11) . . ? O2 Cd1 N5 121.33(11) . 2_666 ? N2 Cd1 N5 102.75(12) . 2_666 ? O1W Cd1 N5 87.10(10) . 2_666 ? O2 Cd1 O5 83.95(11) . 2_765 ? N2 Cd1 O5 85.85(12) . 2_765 ? O1W Cd1 O5 171.82(8) . 2_765 ? N5 Cd1 O5 101.08(12) 2_666 2_765 ? O2 Cd1 O1 53.38(10) . . ? N2 Cd1 O1 82.75(11) . . ? O1W Cd1 O1 89.63(8) . . ? N5 Cd1 O1 173.71(11) 2_666 . ? O5 Cd1 O1 82.22(10) 2_765 . ? O6 Cd2 O4 146.66(9) 1_545 . ? O6 Cd2 N3 119.63(10) 1_545 2_755 ? O4 Cd2 N3 93.70(12) . 2_755 ? O6 Cd2 O2W 89.47(6) 1_545 . ? O4 Cd2 O2W 89.84(10) . . ? N3 Cd2 O2W 90.91(10) 2_755 . ? O6 Cd2 O1 82.47(9) 1_545 2_755 ? O4 Cd2 O1 102.03(12) . 2_755 ? N3 Cd2 O1 85.03(11) 2_755 2_755 ? O2W Cd2 O1 167.66(8) . 2_755 ? O6 Cd2 O3 91.71(9) 1_545 . ? O4 Cd2 O3 55.03(11) . . ? N3 Cd2 O3 148.50(12) 2_755 . ? O2W Cd2 O3 92.53(10) . . ? O1 Cd2 O3 97.01(12) 2_755 . ? C1 N1 N2 104.8(3) . . ? N3 N2 N1 109.7(3) . . ? N3 N2 Cd1 124.5(2) . . ? N1 N2 Cd1 125.3(3) . . ? N2 N3 N4 109.6(3) . . ? N2 N3 Cd2 121.7(3) . 2_755 ? N4 N3 Cd2 128.6(3) . 2_755 ? N3 N4 C1 104.2(3) . . ? C3 N5 C4 118.9(3) . . ? C3 N5 Cd1 112.5(3) . 2_666 ? C4 N5 Cd1 128.2(3) . 2_666 ? C11 O1 Cd2 128.5(3) . 2_755 ? C11 O1 Cd1 83.7(2) . . ? Cd2 O1 Cd1 98.95(10) 2_755 . ? C11 O2 Cd1 100.8(2) . . ? C15 O3 Cd2 87.7(3) . . ? C15 O4 Cd2 96.0(3) . . ? C18 O5 Cd1 126.7(3) . 2_765 ? C18 O6 Cd2 119.5(2) . 1_565 ? Cd1 O1W H1B 115.0 . . ? Cd1 O1W H1A 130.2 . . ? H1B O1W H1A 105.9 . . ? Cd2 O2W H2B 111.0 . . ? Cd2 O2W H2A 109.4 . . ? H2B O2W H2A 105.4 . . ? H3A O3W H3B 104.9 . . ? H4A O4W H4B 105.2 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.852 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.130 data_6 _database_code_depnum_ccdc_archive 'CCDC 804246' #TrackingRef '15239_web_deposit_cif_file_0_HongDeng_1352260642.cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H18 Cd3 N10 O10), 4(H O0.5), 2(H O0.5)' _chemical_formula_sum 'C60 H42 Cd6 N20 O23' _chemical_formula_weight 2085.60 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' 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 C2/c _symmetry_space_group_name_Hall -C2yc 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 8.7590(7) _cell_length_b 25.993(2) _cell_length_c 15.0096(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.5280(10) _cell_angle_gamma 90.00 _cell_volume 3322.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3007 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.200 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 1.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.646 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 8483 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3007 _reflns_number_gt 2673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0451P)^2^+5.3772P] 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 3007 _refine_ls_number_parameters 269 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.038 _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 Cd1 Cd 0.5000 0.186678(15) 0.2500 0.03883(13) Uani 1 2 d S . . Cd2 Cd 0.25564(3) 0.136203(9) 0.001836(16) 0.03078(11) Uani 1 1 d . . . C1 C 0.7017(4) 0.06212(13) 0.1169(2) 0.0307(7) Uani 1 1 d . A . C2 C 0.8202(4) 0.02321(13) 0.1102(2) 0.0302(7) Uani 1 1 d . . . C3 C 0.7681(4) -0.02509(13) 0.0722(2) 0.0336(8) Uani 1 1 d . . . H3 H 0.6606 -0.0306 0.0520 0.040 Uiso 1 1 calc R . . C4 C 1.0239(4) -0.05533(14) 0.0944(2) 0.0350(8) Uani 1 1 d . . . C5 C 1.1288(5) -0.09541(17) 0.0881(3) 0.0472(10) Uani 1 1 d . . . H5 H 1.0902 -0.1275 0.0666 0.057 Uiso 1 1 calc R . . C6 C 1.2872(5) -0.0874(2) 0.1136(3) 0.0559(12) Uani 1 1 d . . . H6 H 1.3558 -0.1139 0.1084 0.067 Uiso 1 1 calc R . . C7 C 1.3467(5) -0.0398(2) 0.1473(3) 0.0585(12) Uani 1 1 d . . . H7 H 1.4548 -0.0347 0.1636 0.070 Uiso 1 1 calc R . . C8 C 1.2498(5) -0.00071(18) 0.1566(3) 0.0477(10) Uani 1 1 d . . . H8 H 1.2917 0.0307 0.1802 0.057 Uiso 1 1 calc R . . C9 C 1.0844(4) -0.00728(15) 0.1305(2) 0.0347(8) Uani 1 1 d . . . C10 C 0.9784(4) 0.03206(14) 0.1381(2) 0.0349(8) Uani 1 1 d . . . H10 H 1.0153 0.0639 0.1620 0.042 Uiso 1 1 calc R . . C11 C 0.3591(4) 0.19089(13) -0.1250(3) 0.0336(8) Uani 1 1 d D . . C12 C 0.4300(4) 0.22112(13) -0.1888(2) 0.0316(7) Uani 1 1 d . A . C13 C 0.5000 0.19572(18) -0.2500 0.0333(11) Uani 1 2 d S . . H13 H 0.5000 0.1599 -0.2500 0.040 Uiso 1 2 calc SR A . C14 C 0.4320(4) 0.27531(13) -0.1886(2) 0.0310(7) Uani 1 1 d . . . C15 C 0.5000 0.30137(19) -0.2500 0.0373(11) Uani 1 2 d S . . H15 H 0.5000 0.3372 -0.2500 0.045 Uiso 1 2 calc SR . . C16 C 0.3664(5) 0.30653(13) -0.1229(3) 0.0361(8) Uani 1 1 d D . . N1 N 0.7203(4) 0.09927(11) 0.1795(2) 0.0383(7) Uani 1 1 d . A . N2 N 0.5822(4) 0.12407(11) 0.1607(2) 0.0368(7) Uani 1 1 d . . . N3 N 0.4871(4) 0.10230(11) 0.0902(2) 0.0382(7) Uani 1 1 d . A . N4 N 0.5592(4) 0.06271(12) 0.0612(2) 0.0419(8) Uani 1 1 d . . . N5 N 0.8646(3) -0.06302(11) 0.06392(19) 0.0330(6) Uani 1 1 d . . . O1 O 0.241(3) 0.1672(9) -0.1594(16) 0.101(2) Uani 0.134(5) 1 d PDU A 1 O2 O 0.419(3) 0.1998(10) -0.0465(13) 0.0901(17) Uani 0.134(5) 1 d PDU A 1 O3 O 0.2343(6) 0.3259(2) -0.1425(4) 0.0403(13) Uani 0.736(10) 1 d PDU . 1 O4 O 0.4558(6) 0.3144(3) -0.0421(4) 0.0661(17) Uani 0.736(10) 1 d PDU . 1 O1' O 0.2784(7) 0.21033(15) -0.0779(3) 0.101(2) Uani 0.866(5) 1 d PDU A 2 O2' O 0.3764(6) 0.14381(14) -0.1204(4) 0.0901(17) Uani 0.866(5) 1 d PDU A 2 O3' O 0.2189(16) 0.3059(6) -0.1383(13) 0.0403(13) Uani 0.264(10) 1 d PDU . 2 O4' O 0.4451(17) 0.3395(6) -0.0780(11) 0.0661(17) Uani 0.264(10) 1 d PDU . 2 O1W O 0.5538(5) 0.24966(12) 0.1574(3) 0.0820(12) Uani 1 1 d . . . H1B H 0.4649 0.2560 0.1263 0.123 Uiso 1 1 d R A . H1A H 0.6159 0.2472 0.1236 0.123 Uiso 1 1 d R . . O2W O 0.7128(7) 0.2056(3) 0.0338(4) 0.074(2) Uani 0.50 1 d P . . H2B H 0.7297 0.2384 0.0242 0.112 Uiso 0.50 1 d PR . . H2A H 0.6325 0.1977 -0.0111 0.112 Uiso 0.50 1 d PR . . O3W O 0.5000 0.3439(7) 0.2500 0.173(8) Uani 0.50 2 d SP . . H3A H 0.5667 0.3224 0.2735 0.260 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0444(2) 0.0384(2) 0.0370(2) 0.000 0.01632(17) 0.000 Cd2 0.03551(17) 0.02504(16) 0.03532(17) 0.00113(9) 0.01540(12) 0.00482(9) C1 0.0313(18) 0.0261(17) 0.0356(18) -0.0006(14) 0.0095(14) 0.0010(14) C2 0.0299(18) 0.0290(17) 0.0320(17) 0.0002(13) 0.0079(14) 0.0023(14) C3 0.0268(18) 0.0329(18) 0.0412(19) -0.0016(15) 0.0079(15) 0.0036(14) C4 0.0312(19) 0.043(2) 0.0321(17) 0.0042(15) 0.0095(14) 0.0068(15) C5 0.041(2) 0.049(2) 0.051(2) 0.0024(18) 0.0093(18) 0.0173(18) C6 0.038(2) 0.078(3) 0.052(2) 0.007(2) 0.0122(19) 0.025(2) C7 0.029(2) 0.100(4) 0.046(2) 0.001(2) 0.0057(17) 0.011(2) C8 0.032(2) 0.072(3) 0.040(2) -0.0059(19) 0.0097(16) -0.0016(19) C9 0.0258(18) 0.049(2) 0.0294(17) 0.0030(15) 0.0069(14) 0.0035(15) C10 0.0338(19) 0.0383(19) 0.0329(18) -0.0007(15) 0.0086(15) -0.0028(15) C11 0.0335(19) 0.0283(19) 0.043(2) -0.0031(15) 0.0164(16) -0.0008(15) C12 0.0281(18) 0.0322(19) 0.0375(18) -0.0002(14) 0.0135(14) 0.0014(14) C13 0.038(3) 0.024(2) 0.043(3) 0.000 0.019(2) 0.000 C14 0.0315(19) 0.0303(18) 0.0318(17) -0.0014(14) 0.0088(14) 0.0009(14) C15 0.050(3) 0.024(2) 0.042(3) 0.000 0.018(2) 0.000 C16 0.043(2) 0.0277(18) 0.041(2) -0.0032(15) 0.0165(17) -0.0004(16) N1 0.0364(17) 0.0359(17) 0.0413(17) -0.0058(13) 0.0066(13) 0.0079(13) N2 0.0380(17) 0.0342(16) 0.0389(17) -0.0035(13) 0.0104(14) 0.0048(13) N3 0.0345(17) 0.0311(15) 0.0482(18) -0.0031(13) 0.0080(14) 0.0066(13) N4 0.0336(17) 0.0367(17) 0.0524(19) -0.0095(14) 0.0039(14) 0.0053(13) N5 0.0318(16) 0.0301(15) 0.0381(15) 0.0024(12) 0.0104(12) 0.0042(12) O1 0.190(6) 0.047(2) 0.109(3) 0.034(2) 0.124(4) 0.043(3) O2 0.127(4) 0.042(2) 0.140(4) 0.021(2) 0.108(4) 0.014(2) O3 0.0417(19) 0.047(4) 0.0364(16) -0.001(3) 0.0177(14) 0.011(2) O4 0.060(2) 0.083(4) 0.049(3) -0.026(3) 0.000(2) 0.029(3) O1' 0.190(6) 0.047(2) 0.109(3) 0.034(2) 0.124(4) 0.043(3) O2' 0.127(4) 0.042(2) 0.140(4) 0.021(2) 0.108(4) 0.014(2) O3' 0.0417(19) 0.047(4) 0.0364(16) -0.001(3) 0.0177(14) 0.011(2) O4' 0.060(2) 0.083(4) 0.049(3) -0.026(3) 0.000(2) 0.029(3) O1W 0.082(3) 0.072(3) 0.100(3) 0.034(2) 0.038(2) 0.0080(18) O2W 0.038(3) 0.129(6) 0.057(4) 0.004(4) 0.013(3) 0.002(4) O3W 0.133(15) 0.110(13) 0.26(2) 0.000 0.017(15) 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 O3' 2.241(16) 8_556 ? Cd1 O3' 2.241(16) 7 ? Cd1 O1W 2.267(3) 2_655 ? Cd1 O1W 2.267(3) . ? Cd1 O3 2.318(5) 7 ? Cd1 O3 2.318(5) 8_556 ? Cd1 N2 2.326(3) . ? Cd1 N2 2.326(3) 2_655 ? Cd2 N5 2.284(3) 5_655 ? Cd2 O1' 2.302(3) . ? Cd2 O3 2.313(6) 7 ? Cd2 N3 2.322(3) . ? Cd2 O2' 2.330(4) . ? Cd2 O4' 2.395(15) 7 ? Cd2 O2 2.40(2) . ? Cd2 O4 2.443(5) 7 ? Cd2 O3' 2.510(19) 7 ? Cd2 O1 2.52(2) . ? Cd2 C16 2.751(4) 7 ? C1 N4 1.330(4) . ? C1 N1 1.331(4) . ? C1 C2 1.470(5) . ? C2 C10 1.370(5) . ? C2 C3 1.410(5) . ? C3 N5 1.323(4) . ? C3 H3 0.9300 . ? C4 N5 1.377(4) . ? C4 C5 1.407(5) . ? C4 C9 1.414(5) . ? C5 C6 1.366(6) . ? C5 H5 0.9300 . ? C6 C7 1.391(7) . ? C6 H6 0.9300 . ? C7 C8 1.352(6) . ? C7 H7 0.9300 . ? C8 C9 1.420(5) . ? C8 H8 0.9300 . ? C9 C10 1.404(5) . ? C10 H10 0.9300 . ? C11 O2 1.193(19) . ? C11 O1 1.214(19) . ? C11 O1' 1.220(5) . ? C11 O2' 1.233(5) . ? C11 C12 1.482(5) . ? C12 C13 1.385(4) . ? C12 C14 1.409(5) . ? C13 C12 1.385(4) 2_654 ? C13 H13 0.9300 . ? C14 C15 1.386(4) . ? C14 C16 1.492(5) . ? C15 C14 1.386(4) 2_654 ? C15 H15 0.9300 . ? C16 O4' 1.203(13) . ? C16 O3 1.232(6) . ? C16 O3' 1.258(14) . ? C16 O4 1.297(6) . ? C16 Cd2 2.751(4) 7 ? N1 N2 1.341(4) . ? N2 N3 1.312(4) . ? N3 N4 1.332(4) . ? N5 Cd2 2.284(3) 5_655 ? O3 Cd2 2.313(6) 7 ? O3 Cd1 2.318(5) 7 ? O4 Cd2 2.443(5) 7 ? O3' Cd1 2.241(16) 7 ? O3' Cd2 2.510(19) 7 ? O4' Cd2 2.395(15) 7 ? O1W H1B 0.8251 . ? O1W H1A 0.8282 . ? O2W H2B 0.8819 . ? O2W H2A 0.8771 . ? O3W H3A 0.8249 . ? 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 O3' Cd1 O3' 170.1(8) 8_556 7 ? O3' Cd1 O1W 75.1(4) 8_556 2_655 ? O3' Cd1 O1W 97.6(5) 7 2_655 ? O3' Cd1 O1W 97.6(5) 8_556 . ? O3' Cd1 O1W 75.1(4) 7 . ? O1W Cd1 O1W 87.6(2) 2_655 . ? O3' Cd1 O3 175.1(5) 8_556 7 ? O3' Cd1 O3 13.6(4) 7 7 ? O1W Cd1 O3 104.55(17) 2_655 7 ? O1W Cd1 O3 87.24(19) . 7 ? O3' Cd1 O3 13.6(4) 8_556 8_556 ? O3' Cd1 O3 175.1(5) 7 8_556 ? O1W Cd1 O3 87.24(19) 2_655 8_556 ? O1W Cd1 O3 104.55(17) . 8_556 ? O3 Cd1 O3 163.8(3) 7 8_556 ? O3' Cd1 N2 99.5(4) 8_556 . ? O3' Cd1 N2 87.5(5) 7 . ? O1W Cd1 N2 174.14(14) 2_655 . ? O1W Cd1 N2 90.88(13) . . ? O3 Cd1 N2 81.00(15) 7 . ? O3 Cd1 N2 87.69(17) 8_556 . ? O3' Cd1 N2 87.5(5) 8_556 2_655 ? O3' Cd1 N2 99.5(4) 7 2_655 ? O1W Cd1 N2 90.88(13) 2_655 2_655 ? O1W Cd1 N2 174.14(14) . 2_655 ? O3 Cd1 N2 87.69(17) 7 2_655 ? O3 Cd1 N2 81.00(15) 8_556 2_655 ? N2 Cd1 N2 91.23(15) . 2_655 ? N5 Cd2 O1' 124.04(17) 5_655 . ? N5 Cd2 O3 131.66(16) 5_655 7 ? O1' Cd2 O3 97.38(18) . 7 ? N5 Cd2 N3 100.59(10) 5_655 . ? O1' Cd2 N3 116.41(18) . . ? O3 Cd2 N3 78.38(14) 7 . ? N5 Cd2 O2' 88.79(14) 5_655 . ? O1' Cd2 O2' 53.77(13) . . ? O3 Cd2 O2' 139.02(19) 7 . ? N3 Cd2 O2' 89.16(16) . . ? N5 Cd2 O4' 96.3(3) 5_655 7 ? O1' Cd2 O4' 101.0(5) . 7 ? O3 Cd2 O4' 47.7(3) 7 7 ? N3 Cd2 O4' 117.9(4) . 7 ? O2' Cd2 O4' 150.8(5) . 7 ? N5 Cd2 O2 133.5(5) 5_655 . ? O1' Cd2 O2 30.4(6) . . ? O3 Cd2 O2 94.8(5) 7 . ? N3 Cd2 O2 86.1(7) . . ? O2' Cd2 O2 45.0(5) . . ? O4' Cd2 O2 121.2(8) 7 . ? N5 Cd2 O4 104.17(15) 5_655 7 ? O1' Cd2 O4 81.5(2) . 7 ? O3 Cd2 O4 54.51(16) 7 7 ? N3 Cd2 O4 132.03(14) . 7 ? O2' Cd2 O4 131.3(2) . 7 ? O4' Cd2 O4 19.9(4) 7 7 ? O2 Cd2 O4 104.6(7) . 7 ? N5 Cd2 O3' 142.8(4) 5_655 7 ? O1' Cd2 O3' 85.4(4) . 7 ? O3 Cd2 O3' 12.1(4) 7 7 ? N3 Cd2 O3' 82.1(3) . 7 ? O2' Cd2 O3' 128.4(4) . 7 ? O4' Cd2 O3' 52.2(4) 7 7 ? O2 Cd2 O3' 83.6(6) . 7 ? O4 Cd2 O3' 53.9(3) 7 7 ? N5 Cd2 O1 86.3(5) 5_655 . ? O1' Cd2 O1 39.3(5) . . ? O3 Cd2 O1 136.2(5) 7 . ? N3 Cd2 O1 120.8(6) . . ? O2' Cd2 O1 31.8(6) . . ? O4' Cd2 O1 119.6(7) 7 . ? O2 Cd2 O1 52.6(6) . . ? O4 Cd2 O1 101.4(6) 7 . ? O3' Cd2 O1 124.4(6) 7 . ? N5 Cd2 C16 121.66(11) 5_655 7 ? O1' Cd2 C16 89.13(12) . 7 ? O3 Cd2 C16 26.40(14) 7 7 ? N3 Cd2 C16 104.50(11) . 7 ? O2' Cd2 C16 142.37(12) . 7 ? O4' Cd2 C16 25.9(3) 7 7 ? O2 Cd2 C16 100.2(6) . 7 ? O4 Cd2 C16 28.12(13) 7 7 ? O3' Cd2 C16 27.2(3) 7 7 ? O1 Cd2 C16 121.3(6) . 7 ? N4 C1 N1 112.2(3) . . ? N4 C1 C2 122.6(3) . . ? N1 C1 C2 125.2(3) . . ? C10 C2 C3 118.8(3) . . ? C10 C2 C1 122.9(3) . . ? C3 C2 C1 118.3(3) . . ? N5 C3 C2 123.2(3) . . ? N5 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? N5 C4 C5 119.8(3) . . ? N5 C4 C9 121.0(3) . . ? C5 C4 C9 119.2(3) . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C4 118.6(3) . . ? C10 C9 C8 122.8(4) . . ? C4 C9 C8 118.6(3) . . ? C2 C10 C9 119.6(3) . . ? C2 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? O2 C11 O1 130.5(17) . . ? O2 C11 O1' 61.8(14) . . ? O1 C11 O1' 84.4(12) . . ? O2 C11 O2' 96.7(13) . . ? O1 C11 O2' 66.5(13) . . ? O1' C11 O2' 117.3(4) . . ? O2 C11 C12 112.5(12) . . ? O1 C11 C12 116.1(12) . . ? O1' C11 C12 122.8(3) . . ? O2' C11 C12 119.9(3) . . ? C13 C12 C14 118.1(3) . . ? C13 C12 C11 119.5(3) . . ? C14 C12 C11 122.4(3) . . ? C12 C13 C12 123.1(4) 2_654 . ? C12 C13 H13 118.5 2_654 . ? C12 C13 H13 118.5 . . ? C15 C14 C12 119.6(3) . . ? C15 C14 C16 117.8(3) . . ? C12 C14 C16 122.6(3) . . ? C14 C15 C14 121.5(5) . 2_654 ? C14 C15 H15 119.3 . . ? C14 C15 H15 119.3 2_654 . ? O4' C16 O3 103.1(8) . . ? O4' C16 O3' 122.8(11) . . ? O3 C16 O3' 25.2(7) . . ? O4' C16 O4 39.0(8) . . ? O3 C16 O4 119.1(4) . . ? O3' C16 O4 122.9(10) . . ? O4' C16 C14 119.9(8) . . ? O3 C16 C14 123.3(4) . . ? O3' C16 C14 114.1(9) . . ? O4 C16 C14 117.5(4) . . ? O4' C16 Cd2 60.3(8) . 7 ? O3 C16 Cd2 56.6(3) . 7 ? O3' C16 Cd2 65.7(9) . 7 ? O4 C16 Cd2 62.6(3) . 7 ? C14 C16 Cd2 179.8(3) . 7 ? C1 N1 N2 104.2(3) . . ? N3 N2 N1 109.4(3) . . ? N3 N2 Cd1 122.9(2) . . ? N1 N2 Cd1 126.9(2) . . ? N2 N3 N4 109.7(3) . . ? N2 N3 Cd2 127.0(2) . . ? N4 N3 Cd2 121.6(2) . . ? C1 N4 N3 104.5(3) . . ? C3 N5 C4 118.7(3) . . ? C3 N5 Cd2 114.9(2) . 5_655 ? C4 N5 Cd2 126.4(2) . 5_655 ? C11 O1 Cd2 84.7(12) . . ? C11 O2 Cd2 90.7(14) . . ? C16 O3 Cd2 97.0(4) . 7 ? C16 O3 Cd1 137.5(4) . 7 ? Cd2 O3 Cd1 122.3(2) 7 7 ? C16 O4 Cd2 89.3(3) . 7 ? C11 O1' Cd2 95.0(3) . . ? C11 O2' Cd2 93.2(3) . . ? C16 O3' Cd1 143.0(13) . 7 ? C16 O3' Cd2 87.2(9) . 7 ? Cd1 O3' Cd2 117.1(6) 7 7 ? C16 O4' Cd2 93.8(9) . 7 ? Cd1 O1W H1B 100.7 . . ? Cd1 O1W H1A 125.5 . . ? H1B O1W H1A 109.6 . . ? H2B O2W H2A 103.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.059 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.090