# 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 _publ_contact_author_name 'Yun-Qi Tian' _publ_contact_author_address ; Institute of Chemistry for Functionalized Materials Liaoning Normal University Huang-He-Road 850 Dalian 116029 CHINA ; _publ_contact_author_email yqtian@lnnu.edu.cn _publ_section_title ; Acentric and Chiral Four-connected Metal-Organic Frameworks Based on Racemic Binaphthol-like Chiral Ligand of 4-(1-H(or Methyl)-imidaozol-1-yl)benzoic Acid ; loop_ _publ_author_name 'Ke-Hui Cui' 'Shi-Yan Yao' 'Hai-Qin Li' 'Yan-Tao Li' 'Hai-Ping Zhao' ; Chun-Jie Jiang ; 'Yun-Qi Tian' data_HIBA _database_code_depnum_ccdc_archive 'CCDC 795326' #TrackingRef '- Crystal structures .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4-(1-H-imidaozol-1-yl)benzoic Acid' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H11 Cl N2 O3' _chemical_formula_weight 242.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2013(16) _cell_length_b 7.3815(16) _cell_length_c 11.328(2) _cell_angle_alpha 77.121(3) _cell_angle_beta 77.612(2) _cell_angle_gamma 75.969(3) _cell_volume 561.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 69 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 248 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10 Sec' _diffrn_standards_decay_% ? _diffrn_reflns_number 3495 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 29.06 _reflns_number_total 2574 _reflns_number_gt 1968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One restraint for O-H bond on carboxyl grouphas been made ; _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^)+(0.1688P)^2^+0.1381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.22(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2574 _refine_ls_number_parameters 150 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2427 _refine_ls_wR_factor_gt 0.2171 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Cl1 Cl 0.46060(11) 0.24848(11) 0.17520(7) 0.0457(3) Uani 1 1 d . . . O1 O 0.2847(5) 0.4701(5) 0.3852(3) 0.0866(11) Uani 1 1 d D . . O2 O 0.4921(5) 0.6607(5) 0.2987(3) 0.0785(9) Uani 1 1 d . . . N1 N 0.0267(6) 1.2408(5) 0.8794(4) 0.0721(10) Uani 1 1 d . . . H1B H 0.0559 1.3206 0.9137 0.087 Uiso 1 1 calc R . . N2 N 0.0450(5) 1.0452(5) 0.7608(3) 0.0625(9) Uani 1 1 d . . . C1 C 0.1403(7) 1.1576(6) 0.7919(4) 0.0659(10) Uani 1 1 d . . . H1A H 0.2658 1.1736 0.7572 0.079 Uiso 1 1 calc R . . C2 C -0.1479(8) 1.1804(7) 0.9082(5) 0.0764(12) Uani 1 1 d . . . H2A H -0.2535 1.2183 0.9672 0.092 Uiso 1 1 calc R . . C3 C -0.1356(6) 1.0577(6) 0.8353(4) 0.0649(10) Uani 1 1 d . . . H3A H -0.2307 0.9925 0.8345 0.078 Uiso 1 1 calc R . . C4 C 0.1189(6) 0.9362(6) 0.6656(4) 0.0589(9) Uani 1 1 d . . . C5 C 0.2304(6) 1.0132(6) 0.5577(4) 0.0608(10) Uani 1 1 d . . . H5A H 0.2536 1.1346 0.5482 0.073 Uiso 1 1 calc R . . C6 C 0.3050(6) 0.9091(6) 0.4664(4) 0.0606(9) Uani 1 1 d . . . H6A H 0.3809 0.9594 0.3950 0.073 Uiso 1 1 calc R . . C7 C 0.2682(5) 0.7267(5) 0.4791(4) 0.0568(9) Uani 1 1 d . . . C8 C 0.1518(6) 0.6557(6) 0.5853(4) 0.0603(9) Uani 1 1 d . . . H8A H 0.1232 0.5367 0.5937 0.072 Uiso 1 1 calc R . . C9 C 0.0781(6) 0.7587(6) 0.6782(4) 0.0617(9) Uani 1 1 d . . . H9A H 0.0010 0.7092 0.7492 0.074 Uiso 1 1 calc R . . C10 C 0.3596(5) 0.6176(6) 0.3795(4) 0.0589(9) Uani 1 1 d . . . O1W O 0.2310(5) 1.4552(6) 0.9516(4) 0.0882(10) Uani 1 1 d . . . H1O H 0.337(7) 0.455(8) 0.2992(19) 0.093(17) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0465(5) 0.0502(5) 0.0426(5) -0.0102(3) -0.0003(3) -0.0187(3) O1 0.089(2) 0.091(2) 0.088(2) -0.0344(19) 0.0148(18) -0.0429(19) O2 0.070(2) 0.081(2) 0.083(2) -0.0143(16) 0.0043(16) -0.0283(16) N1 0.086(3) 0.066(2) 0.070(2) -0.0136(17) -0.0169(19) -0.0219(19) N2 0.0599(19) 0.061(2) 0.067(2) -0.0076(15) -0.0125(16) -0.0168(15) C1 0.065(2) 0.066(2) 0.072(3) -0.0107(19) -0.016(2) -0.0218(19) C2 0.077(3) 0.076(3) 0.071(3) -0.009(2) -0.011(2) -0.014(2) C3 0.056(2) 0.065(2) 0.073(3) -0.0091(19) -0.0109(19) -0.0153(18) C4 0.054(2) 0.060(2) 0.064(2) -0.0085(17) -0.0134(17) -0.0135(16) C5 0.062(2) 0.053(2) 0.070(2) -0.0021(17) -0.0141(19) -0.0223(17) C6 0.060(2) 0.060(2) 0.060(2) -0.0001(17) -0.0097(17) -0.0193(17) C7 0.0481(19) 0.058(2) 0.065(2) -0.0023(17) -0.0169(16) -0.0151(16) C8 0.056(2) 0.053(2) 0.071(2) -0.0055(17) -0.0100(17) -0.0142(16) C9 0.059(2) 0.059(2) 0.065(2) -0.0022(17) -0.0071(17) -0.0198(17) C10 0.050(2) 0.058(2) 0.067(2) -0.0043(17) -0.0102(17) -0.0142(16) O1W 0.075(2) 0.101(3) 0.096(2) -0.021(2) -0.0058(18) -0.0362(19) _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 O1 C10 1.311(5) . ? O2 C10 1.222(5) . ? N1 C1 1.307(7) . ? N1 C2 1.385(6) . ? N2 C1 1.339(5) . ? N2 C3 1.385(6) . ? N2 C4 1.424(5) . ? C2 C3 1.332(7) . ? C4 C9 1.381(6) . ? C4 C5 1.397(6) . ? C5 C6 1.366(6) . ? C6 C7 1.405(5) . ? C7 C8 1.387(6) . ? C7 C10 1.478(6) . ? C8 C9 1.375(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 109.4(4) . . ? C1 N2 C3 108.1(4) . . ? C1 N2 C4 124.9(4) . . ? C3 N2 C4 127.0(3) . . ? N1 C1 N2 108.4(4) . . ? C3 C2 N1 106.9(4) . . ? C2 C3 N2 107.3(4) . . ? C9 C4 C5 120.3(4) . . ? C9 C4 N2 120.7(4) . . ? C5 C4 N2 118.9(3) . . ? C6 C5 C4 119.6(4) . . ? C5 C6 C7 120.6(4) . . ? C8 C7 C6 118.8(4) . . ? C8 C7 C10 123.0(4) . . ? C6 C7 C10 118.2(4) . . ? C9 C8 C7 120.9(4) . . ? C8 C9 C4 119.7(4) . . ? O2 C10 O1 122.8(4) . . ? O2 C10 C7 123.4(4) . . ? O1 C10 C7 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 29.06 _diffrn_measured_fraction_theta_full 0.859 _refine_diff_density_max 0.922 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.135 data_HMIBA _database_code_depnum_ccdc_archive 'CCDC 795327' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4-(1-Methyl-imidaozol-1-yl)benzoic Acid' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H13 Cl N2 O3' _chemical_formula_weight 256.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.465(8) _cell_length_b 7.830(4) _cell_length_c 11.406(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.139(6) _cell_angle_gamma 90.00 _cell_volume 1205.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 72 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7083 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.87 _reflns_number_total 2826 _reflns_number_gt 1744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2826 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.11235(19) 0.6104(4) -0.1768(3) 0.0458(7) Uani 1 1 d . . . C2 C 0.00581(18) 0.6099(4) -0.2599(2) 0.0413(6) Uani 1 1 d . . . C3 C -0.01909(18) 0.6430(4) -0.3869(2) 0.0467(7) Uani 1 1 d . . . H3A H 0.0304 0.6690 -0.4182 0.056 Uiso 1 1 calc R . . C4 C -0.06871(19) 0.5727(4) -0.2139(3) 0.0456(7) Uani 1 1 d . . . H10A H -0.0526 0.5530 -0.1285 0.055 Uiso 1 1 calc R . . C5 C -0.11676(19) 0.6378(4) -0.4673(3) 0.0470(7) Uani 1 1 d . . . H4A H -0.1334 0.6605 -0.5525 0.056 Uiso 1 1 calc R . . C6 C -0.16626(18) 0.5648(4) -0.2936(2) 0.0446(7) Uani 1 1 d . . . H5A H -0.2158 0.5373 -0.2628 0.053 Uiso 1 1 calc R . . C7 C -0.18963(18) 0.5982(3) -0.4196(2) 0.0384(6) Uani 1 1 d . . . C8 C -0.32077(19) 0.4914(4) -0.6149(2) 0.0439(7) Uani 1 1 d . . . H1A H -0.2805 0.4279 -0.6462 0.053 Uiso 1 1 calc R . . C9 C -0.36987(17) 0.6582(3) -0.4915(2) 0.0381(6) Uani 1 1 d . . . N1 N -0.44748(15) 0.6129(3) -0.5906(2) 0.0415(6) Uani 1 1 d . . . H22A H -0.5074 0.6444 -0.6043 0.050 Uiso 1 1 calc R . . C11 C -0.3724(2) 0.7715(4) -0.3897(3) 0.0503(7) Uani 1 1 d . . . H2A H -0.4396 0.8044 -0.4046 0.076 Uiso 1 1 calc R . . H2B H -0.3333 0.8715 -0.3872 0.076 Uiso 1 1 calc R . . H2C H -0.3458 0.7124 -0.3108 0.076 Uiso 1 1 calc R . . O1 O 0.17868(13) 0.6151(3) -0.21793(19) 0.0665(7) Uani 1 1 d . . . O2 O 0.12672(14) 0.5992(3) -0.05662(19) 0.0646(7) Uani 1 1 d . . . C10 C -0.41946(19) 0.5095(4) -0.6678(3) 0.0451(7) Uani 1 1 d . . . H1B H -0.4607 0.4608 -0.7428 0.054 Uiso 1 1 calc R . . N2 N -0.29032(14) 0.5858(3) -0.50441(19) 0.0373(5) Uani 1 1 d . . . Cl1 Cl 0.33244(5) 0.53609(10) 0.12193(6) 0.0501(3) Uani 1 1 d . . . O1W O -0.62137(14) 0.7566(3) -0.59078(19) 0.0627(6) Uani 1 1 d . . . H1O H 0.195(3) 0.583(5) -0.004(3) 0.092(12) Uiso 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 0.0375(14) 0.0558(19) 0.0435(16) -0.0030(12) 0.0137(13) -0.0007(13) C2 0.0301(13) 0.0476(17) 0.0462(16) -0.0027(12) 0.0138(11) 0.0002(12) C3 0.0314(13) 0.065(2) 0.0465(16) 0.0040(13) 0.0174(12) -0.0042(13) C4 0.0359(14) 0.0619(19) 0.0375(15) 0.0047(13) 0.0116(12) 0.0024(13) C5 0.0421(15) 0.062(2) 0.0380(14) 0.0029(13) 0.0159(12) -0.0025(14) C6 0.0336(13) 0.0578(19) 0.0449(15) 0.0055(13) 0.0173(12) -0.0013(13) C7 0.0298(12) 0.0451(16) 0.0399(14) -0.0007(11) 0.0120(11) -0.0020(11) C8 0.0412(15) 0.0523(18) 0.0407(15) -0.0034(12) 0.0180(13) 0.0007(13) C9 0.0339(13) 0.0416(15) 0.0408(14) 0.0053(11) 0.0157(11) 0.0018(12) N1 0.0266(10) 0.0523(14) 0.0436(13) 0.0075(10) 0.0102(9) 0.0023(10) C11 0.0457(15) 0.0553(19) 0.0501(17) -0.0056(13) 0.0173(13) 0.0068(13) O1 0.0326(10) 0.113(2) 0.0551(13) -0.0017(12) 0.0170(10) -0.0021(11) O2 0.0342(11) 0.113(2) 0.0434(12) 0.0014(11) 0.0098(9) 0.0012(12) C10 0.0376(14) 0.0576(19) 0.0373(15) -0.0032(12) 0.0102(12) -0.0036(13) N2 0.0308(10) 0.0443(13) 0.0373(12) -0.0004(9) 0.0128(9) -0.0011(10) Cl1 0.0387(4) 0.0647(5) 0.0431(4) 0.0058(3) 0.0101(3) 0.0014(3) O1W 0.0432(11) 0.0835(18) 0.0588(13) 0.0058(11) 0.0151(10) 0.0189(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 C1 O1 1.211(3) . ? C1 O2 1.313(3) . ? C1 C2 1.490(4) . ? C2 C3 1.385(4) . ? C2 C4 1.389(3) . ? C3 C5 1.380(4) . ? C4 C6 1.377(3) . ? C5 C7 1.385(3) . ? C6 C7 1.377(4) . ? C7 N2 1.432(3) . ? C8 C10 1.342(3) . ? C8 N2 1.389(3) . ? C9 N1 1.322(3) . ? C9 N2 1.338(3) . ? C9 C11 1.472(4) . ? N1 C10 1.362(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 123.8(2) . . ? O1 C1 C2 122.4(2) . . ? O2 C1 C2 113.7(2) . . ? C3 C2 C4 119.3(2) . . ? C3 C2 C1 118.9(2) . . ? C4 C2 C1 121.8(2) . . ? C5 C3 C2 120.5(2) . . ? C6 C4 C2 120.7(3) . . ? C3 C5 C7 119.1(3) . . ? C4 C6 C7 119.2(2) . . ? C6 C7 C5 121.2(2) . . ? C6 C7 N2 120.0(2) . . ? C5 C7 N2 118.8(2) . . ? C10 C8 N2 106.9(2) . . ? N1 C9 N2 106.9(2) . . ? N1 C9 C11 125.5(2) . . ? N2 C9 C11 127.5(2) . . ? C9 N1 C10 110.7(2) . . ? C8 C10 N1 106.7(2) . . ? C9 N2 C8 108.8(2) . . ? C9 N2 C7 127.1(2) . . ? C8 N2 C7 124.2(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.382 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.057 data_2 _database_code_depnum_ccdc_archive 'CCDC 795328' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 N4 O4 Zn' _chemical_formula_sum 'C20 H14 N4 O4 Zn' _chemical_formula_weight 439.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' '-x, y, -z' 'x, -y, -z+1/2' 'y, x, -z+1/4' '-y, -x, -z+3/4' _cell_length_a 8.0674(4) _cell_length_b 8.0674(4) _cell_length_c 28.0367(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1824.71(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 79 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9881 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.88 _reflns_number_total 1771 _reflns_number_gt 1273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 1771 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.01115(8) 0.0000 0.0338(2) Uani 1 2 d S . . C1 C 0.0165(6) 0.2529(6) 0.08260(17) 0.0477(12) Uani 1 1 d . . . H1A H -0.0846 0.2188 0.0951 0.057 Uiso 1 1 calc R . . C2 C 0.2360(5) 0.2583(5) 0.04027(16) 0.0373(10) Uani 1 1 d . . . H2A H 0.3176 0.2320 0.0181 0.045 Uiso 1 1 calc R . . C3 C 0.1003(6) 0.3888(6) 0.09659(17) 0.0477(13) Uani 1 1 d . . . H3A H 0.0693 0.4654 0.1197 0.057 Uiso 1 1 calc R . . C4 C 0.3626(5) 0.5186(5) 0.06779(14) 0.0331(10) Uani 1 1 d . . . C5 C 0.5283(5) 0.4794(5) 0.06379(15) 0.0374(10) Uani 1 1 d . . . H5A H 0.5626 0.3694 0.0647 0.045 Uiso 1 1 calc R . . C6 C 0.3094(6) 0.6824(5) 0.06867(15) 0.0388(10) Uani 1 1 d . . . H6A H 0.1977 0.7079 0.0723 0.047 Uiso 1 1 calc R . . C7 C 0.6435(5) 0.6062(5) 0.05836(14) 0.0382(11) Uani 1 1 d . . . H7A H 0.7553 0.5810 0.0548 0.046 Uiso 1 1 calc R . . C8 C 0.4260(6) 0.8061(6) 0.06408(15) 0.0381(11) Uani 1 1 d . . . H8A H 0.3922 0.9163 0.0649 0.046 Uiso 1 1 calc R . . C9 C 0.5920(6) 0.7695(6) 0.05824(15) 0.0353(11) Uani 1 1 d . . . C10 C 0.7120(7) 0.9110(6) 0.04844(16) 0.0433(12) Uani 1 1 d . . . N1 N 0.1021(4) 0.1713(4) 0.04696(13) 0.0408(10) Uani 1 1 d . . . N2 N 0.2418(4) 0.3897(4) 0.06912(12) 0.0369(9) Uani 1 1 d . . . O1 O 0.8523(4) 0.8613(4) 0.03273(12) 0.0526(9) Uani 1 1 d . . . O2 O 0.6678(4) 1.0549(4) 0.05373(12) 0.0577(10) 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 0.0292(4) 0.0265(4) 0.0458(4) 0.000 0.0027(3) 0.000 C1 0.040(3) 0.045(3) 0.058(3) -0.007(2) 0.016(3) -0.015(2) C2 0.037(3) 0.034(3) 0.041(3) -0.005(2) 0.002(2) -0.004(2) C3 0.045(3) 0.045(3) 0.053(3) -0.007(2) 0.013(2) -0.010(2) C4 0.037(2) 0.034(2) 0.028(2) 0.000(2) 0.0039(19) -0.008(2) C5 0.043(3) 0.032(2) 0.037(2) -0.0018(18) 0.0046(19) -0.0020(19) C6 0.034(3) 0.039(3) 0.043(3) -0.002(2) 0.004(2) -0.0052(19) C7 0.033(3) 0.041(3) 0.041(3) -0.001(2) 0.005(2) -0.006(2) C8 0.049(3) 0.027(2) 0.038(3) -0.003(2) 0.001(2) -0.002(2) C9 0.037(3) 0.035(3) 0.034(3) 0.001(2) 0.001(2) -0.007(2) C10 0.045(3) 0.042(3) 0.042(3) 0.001(2) -0.001(2) -0.011(2) N1 0.037(2) 0.038(2) 0.048(2) -0.0005(18) 0.0033(18) -0.0102(18) N2 0.041(2) 0.029(2) 0.041(2) -0.0067(18) 0.0108(19) -0.0073(17) O1 0.046(2) 0.046(2) 0.066(2) 0.0027(18) 0.0066(18) -0.0127(16) O2 0.059(2) 0.0343(19) 0.079(3) 0.0021(18) 0.011(2) -0.0171(17) _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 O1 1.929(3) 5_645 ? Zn1 O1 1.929(3) 1_445 ? Zn1 N1 2.020(4) . ? Zn1 N1 2.020(4) 5 ? C1 C3 1.346(6) . ? C1 N1 1.381(5) . ? C1 H1A 0.9300 . ? C2 N1 1.301(5) . ? C2 N2 1.335(5) . ? C2 H2A 0.9300 . ? C3 N2 1.377(5) . ? C3 H3A 0.9300 . ? C4 C5 1.378(5) . ? C4 C6 1.389(6) . ? C4 N2 1.426(5) . ? C5 C7 1.391(5) . ? C5 H5A 0.9300 . ? C6 C8 1.377(6) . ? C6 H6A 0.9300 . ? C7 C9 1.381(6) . ? C7 H7A 0.9300 . ? C8 C9 1.382(6) . ? C8 H8A 0.9300 . ? C9 C10 1.522(6) . ? C10 O2 1.223(5) . ? C10 O1 1.279(5) . ? O1 Zn1 1.929(3) 1_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 O1 Zn1 O1 102.4(2) 5_645 1_445 ? O1 Zn1 N1 117.31(14) 5_645 . ? O1 Zn1 N1 110.02(15) 1_445 . ? O1 Zn1 N1 110.02(15) 5_645 5 ? O1 Zn1 N1 117.31(14) 1_445 5 ? N1 Zn1 N1 100.5(2) . 5 ? C3 C1 N1 110.4(4) . . ? C3 C1 H1A 124.8 . . ? N1 C1 H1A 124.8 . . ? N1 C2 N2 111.7(4) . . ? N1 C2 H2A 124.1 . . ? N2 C2 H2A 124.1 . . ? C1 C3 N2 104.9(4) . . ? C1 C3 H3A 127.5 . . ? N2 C3 H3A 127.5 . . ? C5 C4 C6 121.3(4) . . ? C5 C4 N2 119.8(4) . . ? C6 C4 N2 118.8(4) . . ? C4 C5 C7 119.2(4) . . ? C4 C5 H5A 120.4 . . ? C7 C5 H5A 120.4 . . ? C8 C6 C4 118.5(4) . . ? C8 C6 H6A 120.8 . . ? C4 C6 H6A 120.8 . . ? C9 C7 C5 120.1(4) . . ? C9 C7 H7A 120.0 . . ? C5 C7 H7A 120.0 . . ? C6 C8 C9 121.2(4) . . ? C6 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C7 C9 C8 119.7(4) . . ? C7 C9 C10 121.7(4) . . ? C8 C9 C10 118.5(4) . . ? O2 C10 O1 126.7(5) . . ? O2 C10 C9 120.3(5) . . ? O1 C10 C9 112.9(4) . . ? C2 N1 C1 105.2(4) . . ? C2 N1 Zn1 126.1(3) . . ? C1 N1 Zn1 124.9(3) . . ? C2 N2 C3 107.8(4) . . ? C2 N2 C4 126.0(4) . . ? C3 N2 C4 125.8(4) . . ? C10 O1 Zn1 120.9(3) . 1_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C3 N2 -0.6(6) . . . . ? C6 C4 C5 C7 -2.9(6) . . . . ? N2 C4 C5 C7 174.5(4) . . . . ? C5 C4 C6 C8 1.8(6) . . . . ? N2 C4 C6 C8 -175.6(4) . . . . ? C4 C5 C7 C9 1.6(6) . . . . ? C4 C6 C8 C9 0.6(7) . . . . ? C5 C7 C9 C8 0.7(7) . . . . ? C5 C7 C9 C10 -175.0(4) . . . . ? C6 C8 C9 C7 -1.9(7) . . . . ? C6 C8 C9 C10 174.0(4) . . . . ? C7 C9 C10 O2 -171.9(5) . . . . ? C8 C9 C10 O2 12.3(7) . . . . ? C7 C9 C10 O1 11.3(6) . . . . ? C8 C9 C10 O1 -164.5(4) . . . . ? N2 C2 N1 C1 0.0(5) . . . . ? N2 C2 N1 Zn1 158.7(3) . . . . ? C3 C1 N1 C2 0.4(6) . . . . ? C3 C1 N1 Zn1 -158.7(3) . . . . ? O1 Zn1 N1 C2 44.3(4) 5_645 . . . ? O1 Zn1 N1 C2 160.8(4) 1_445 . . . ? N1 Zn1 N1 C2 -74.9(3) 5 . . . ? O1 Zn1 N1 C1 -160.9(4) 5_645 . . . ? O1 Zn1 N1 C1 -44.4(4) 1_445 . . . ? N1 Zn1 N1 C1 79.9(4) 5 . . . ? N1 C2 N2 C3 -0.3(5) . . . . ? N1 C2 N2 C4 -173.5(4) . . . . ? C1 C3 N2 C2 0.5(5) . . . . ? C1 C3 N2 C4 173.7(4) . . . . ? C5 C4 N2 C2 -45.7(6) . . . . ? C6 C4 N2 C2 131.8(5) . . . . ? C5 C4 N2 C3 142.4(4) . . . . ? C6 C4 N2 C3 -40.2(6) . . . . ? O2 C10 O1 Zn1 -15.3(7) . . . 1_665 ? C9 C10 O1 Zn1 161.3(3) . . . 1_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.264 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.071 data_1 _database_code_depnum_ccdc_archive 'CCDC 795329' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Co N4 O4' _chemical_formula_sum 'C20 H14 Co N4 O4' _chemical_formula_weight 433.28 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' '-x, y, -z' 'x, -y, -z+1/2' 'y, x, -z+3/4' '-y, -x, -z+1/4' _cell_length_a 8.0814(3) _cell_length_b 8.0814(3) _cell_length_c 28.0836(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1834.11(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 82 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8679 _exptl_absorpt_correction_T_max 0.9091 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11555 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 29.19 _reflns_number_total 2343 _reflns_number_gt 1920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.7648P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 2343 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 Co1 Co 0.0000 0.01301(5) 0.0000 0.03033(11) Uani 1 2 d S . . C1 C -0.0152(3) 0.2543(3) 0.08253(9) 0.0451(6) Uani 1 1 d . . . H1A H 0.0858 0.2206 0.0950 0.054 Uiso 1 1 calc R . . C2 C -0.2363(3) 0.2600(3) 0.03996(8) 0.0359(5) Uani 1 1 d . . . H2A H -0.3175 0.2335 0.0178 0.043 Uiso 1 1 calc R . . C3 C -0.1004(3) 0.3897(3) 0.09651(8) 0.0434(6) Uani 1 1 d . . . H3A H -0.0698 0.4658 0.1198 0.052 Uiso 1 1 calc R . . C4 C -0.3633(3) 0.5209(3) 0.06773(7) 0.0320(5) Uani 1 1 d . . . C5 C -0.5288(3) 0.4797(3) 0.06368(7) 0.0361(5) Uani 1 1 d . . . H5A H -0.5625 0.3697 0.0645 0.043 Uiso 1 1 calc R . . C6 C -0.3104(3) 0.6834(3) 0.06863(7) 0.0374(5) Uani 1 1 d . . . H6A H -0.1989 0.7087 0.0722 0.045 Uiso 1 1 calc R . . C7 C -0.6438(3) 0.6062(3) 0.05831(7) 0.0377(5) Uani 1 1 d . . . H7A H -0.7554 0.5807 0.0547 0.045 Uiso 1 1 calc R . . C8 C -0.4273(3) 0.8078(3) 0.06410(8) 0.0380(5) Uani 1 1 d . . . H8A H -0.3938 0.9178 0.0650 0.046 Uiso 1 1 calc R . . C9 C -0.5928(3) 0.7708(3) 0.05827(8) 0.0360(5) Uani 1 1 d . . . C10 C -0.7142(3) 0.9088(3) 0.04767(9) 0.0441(6) Uani 1 1 d . . . N1 N -0.1008(2) 0.1737(2) 0.04686(7) 0.0371(5) Uani 1 1 d . . . N2 N -0.2421(2) 0.3918(2) 0.06917(6) 0.0349(4) Uani 1 1 d . . . O1 O -0.8544(2) 0.8597(2) 0.03212(6) 0.0545(5) Uani 1 1 d . . . O2 O -0.6715(3) 1.0543(2) 0.05302(7) 0.0625(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 Co1 0.0258(2) 0.0236(2) 0.0416(2) 0.000 -0.00224(16) 0.000 C1 0.0376(13) 0.0463(13) 0.0515(13) -0.0062(11) -0.0134(12) 0.0140(13) C2 0.0373(13) 0.0324(12) 0.0380(11) -0.0049(10) -0.0058(10) 0.0053(10) C3 0.0405(13) 0.0433(14) 0.0464(14) -0.0104(11) -0.0153(11) 0.0105(12) C4 0.0370(12) 0.0313(11) 0.0277(10) -0.0027(9) -0.0040(9) 0.0104(10) C5 0.0391(12) 0.0304(11) 0.0389(10) -0.0021(9) -0.0055(9) 0.0027(9) C6 0.0365(14) 0.0361(14) 0.0394(11) -0.0015(10) -0.0040(10) 0.0037(9) C7 0.0305(12) 0.0427(13) 0.0400(12) -0.0017(10) -0.0059(9) 0.0071(11) C8 0.0478(14) 0.0294(12) 0.0367(12) -0.0010(10) -0.0023(11) 0.0070(11) C9 0.0403(14) 0.0364(13) 0.0315(11) 0.0006(10) -0.0027(10) 0.0134(11) C10 0.0462(16) 0.0473(15) 0.0388(13) 0.0022(12) 0.0011(11) 0.0200(13) N1 0.0358(10) 0.0334(10) 0.0421(10) -0.0024(9) -0.0044(9) 0.0093(9) N2 0.0354(11) 0.0307(10) 0.0385(10) -0.0038(8) -0.0075(9) 0.0092(9) O1 0.0451(12) 0.0572(13) 0.0613(10) 0.0060(10) -0.0080(9) 0.0237(9) O2 0.0698(14) 0.0387(11) 0.0788(14) 0.0044(10) -0.0010(11) 0.0233(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 Co1 O1 1.9322(15) 5_445 ? Co1 O1 1.9322(15) 1_645 ? Co1 N1 2.0202(19) 5 ? Co1 N1 2.0202(19) . ? C1 C3 1.351(3) . ? C1 N1 1.381(3) . ? C1 H1A 0.9300 . ? C2 N1 1.313(3) . ? C2 N2 1.345(3) . ? C2 H2A 0.9300 . ? C3 N2 1.379(3) . ? C3 H3A 0.9300 . ? C4 C5 1.383(3) . ? C4 C6 1.381(3) . ? C4 N2 1.431(3) . ? C5 C7 1.389(3) . ? C5 H5A 0.9300 . ? C6 C8 1.385(3) . ? C6 H6A 0.9300 . ? C7 C9 1.393(3) . ? C7 H7A 0.9300 . ? C8 C9 1.380(3) . ? C8 H8A 0.9300 . ? C9 C10 1.514(3) . ? C10 O2 1.235(3) . ? C10 O1 1.277(3) . ? O1 Co1 1.9322(15) 1_465 ? 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 Co1 O1 100.24(12) 5_445 1_645 ? O1 Co1 N1 110.70(8) 5_445 5 ? O1 Co1 N1 118.08(8) 1_645 5 ? O1 Co1 N1 118.08(8) 5_445 . ? O1 Co1 N1 110.70(8) 1_645 . ? N1 Co1 N1 100.01(11) 5 . ? C3 C1 N1 109.8(2) . . ? C3 C1 H1A 125.1 . . ? N1 C1 H1A 125.1 . . ? N1 C2 N2 111.1(2) . . ? N1 C2 H2A 124.4 . . ? N2 C2 H2A 124.4 . . ? C1 C3 N2 105.7(2) . . ? C1 C3 H3A 127.1 . . ? N2 C3 H3A 127.1 . . ? C5 C4 C6 121.9(2) . . ? C5 C4 N2 119.3(2) . . ? C6 C4 N2 118.7(2) . . ? C4 C5 C7 118.6(2) . . ? C4 C5 H5A 120.7 . . ? C7 C5 H5A 120.7 . . ? C8 C6 C4 118.5(2) . . ? C8 C6 H6A 120.7 . . ? C4 C6 H6A 120.7 . . ? C5 C7 C9 120.3(2) . . ? C5 C7 H7A 119.8 . . ? C9 C7 H7A 119.9 . . ? C9 C8 C6 121.0(2) . . ? C9 C8 H8A 119.5 . . ? C6 C8 H8A 119.5 . . ? C8 C9 C7 119.6(2) . . ? C8 C9 C10 119.4(2) . . ? C7 C9 C10 120.8(2) . . ? O2 C10 O1 125.8(3) . . ? O2 C10 C9 119.8(2) . . ? O1 C10 C9 114.4(2) . . ? C2 N1 C1 105.89(19) . . ? C2 N1 Co1 125.56(15) . . ? C1 N1 Co1 125.05(15) . . ? C2 N2 C3 107.47(19) . . ? C2 N2 C4 125.73(18) . . ? C3 N2 C4 126.37(19) . . ? C10 O1 Co1 120.06(18) . 1_465 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 29.19 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.270 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.047 data_3 _database_code_depnum_ccdc_archive 'CCDC 795330' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22.85 H20.65 Cd N4.95 O6.70' _chemical_formula_sum 'C22.85 H20.65 Cd N4.95 O6.70' _chemical_formula_weight 584.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 19.0367(16) _cell_length_b 8.2300(7) _cell_length_c 18.2963(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2866.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 88 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas MULTI-SCAN _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1281 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10 Sec.' _diffrn_standards_decay_% ? _diffrn_reflns_number 11412 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4623 _reflns_number_gt 3658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Except the watter molecules discovered in the structure, there are still solvent accessible void of 18.4% of the crystal volume, which are occupied by the highly disordered molecules of DMF that were used as solvent in the synthesis ; _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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.63(3) _refine_ls_number_reflns 4623 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.475830(10) 1.00444(3) 0.31786(5) 0.03771(8) Uani 1 1 d . . . C1 C 0.61752(17) 1.2295(4) 0.3279(2) 0.0422(9) Uani 1 1 d . . . H1A H 0.5943 1.3140 0.3514 0.051 Uiso 1 1 calc R . . C2 C 0.6386(2) 1.0026(5) 0.2717(3) 0.0724(15) Uani 1 1 d . . . H2A H 0.6324 0.9022 0.2493 0.087 Uiso 1 1 calc R . . C3 C 0.6977(2) 1.0904(6) 0.2734(3) 0.0717(14) Uani 1 1 d . . . H3A H 0.7407 1.0581 0.2541 0.086 Uiso 1 1 calc R . . C4 C 0.73278(16) 1.3653(4) 0.3148(4) 0.0445(9) Uani 1 1 d . . . C5 C 0.80286(19) 1.3306(4) 0.3267(4) 0.0508(11) Uani 1 1 d . . . H5A H 0.8179 1.2237 0.3318 0.061 Uiso 1 1 calc R . . C6 C 0.8506(2) 1.4586(4) 0.3310(3) 0.0486(14) Uani 1 1 d . . . H6A H 0.8974 1.4381 0.3421 0.058 Uiso 1 1 calc R . . C7 C 0.82788(18) 1.6191(4) 0.3184(3) 0.0469(8) Uani 1 1 d . . . C8 C 0.75838(19) 1.6489(4) 0.3077(4) 0.0525(13) Uani 1 1 d . . . H8A H 0.7432 1.7558 0.3026 0.063 Uiso 1 1 calc R . . C9 C 0.7094(2) 1.5238(4) 0.3041(3) 0.0495(16) Uani 1 1 d . . . H9A H 0.6623 1.5455 0.2948 0.059 Uiso 1 1 calc R . . C10 C 0.88133(18) 1.7558(4) 0.3205(3) 0.0455(8) Uani 1 1 d . . . C11 C 0.4681(2) 0.7730(5) 0.4586(2) 0.0459(10) Uani 1 1 d . . . H11A H 0.4952 0.6949 0.4351 0.055 Uiso 1 1 calc R . . C12 C 0.4103(2) 0.9899(5) 0.4800(2) 0.0552(11) Uani 1 1 d . . . H12A H 0.3890 1.0905 0.4732 0.066 Uiso 1 1 calc R . . C13 C 0.4072(2) 0.9018(5) 0.5416(2) 0.0517(10) Uani 1 1 d . . . H13A H 0.3852 0.9308 0.5851 0.062 Uiso 1 1 calc R . . C14 C 0.4546(2) 0.6281(5) 0.5771(2) 0.0462(10) Uani 1 1 d . . . C15 C 0.4681(2) 0.6617(6) 0.6501(2) 0.0516(11) Uani 1 1 d . . . H15A H 0.4693 0.7687 0.6664 0.062 Uiso 1 1 calc R . . C16 C 0.4797(2) 0.5349(5) 0.6985(3) 0.0519(11) Uani 1 1 d . . . H16A H 0.4860 0.5569 0.7479 0.062 Uiso 1 1 calc R . . C17 C 0.48215(19) 0.3771(6) 0.6743(2) 0.0447(10) Uani 1 1 d . . . C18 C 0.4711(2) 0.3457(5) 0.6004(3) 0.0542(11) Uani 1 1 d . . . H18A H 0.4732 0.2391 0.5837 0.065 Uiso 1 1 calc R . . C19 C 0.4568(2) 0.4711(5) 0.5504(3) 0.0524(11) Uani 1 1 d . . . H19A H 0.4492 0.4492 0.5012 0.063 Uiso 1 1 calc R . . C20 C 0.4976(2) 0.2431(5) 0.7254(2) 0.0490(10) Uani 1 1 d . . . N1 N 0.58836(13) 1.0907(3) 0.3098(2) 0.0497(8) Uani 1 1 d . . . N2 N 0.68547(14) 1.2332(3) 0.3077(2) 0.0482(8) Uani 1 1 d . . . N3 N 0.44888(17) 0.9113(5) 0.42952(17) 0.0457(8) Uani 1 1 d . . . N4 N 0.44317(17) 0.7590(4) 0.52735(17) 0.0463(8) Uani 1 1 d . . . O1 O 0.86356(13) 1.8936(4) 0.29802(15) 0.0618(8) Uani 1 1 d . . . O2 O 0.94198(14) 1.7254(3) 0.34441(16) 0.0613(9) Uani 1 1 d . . . O3 O 0.49370(16) 0.2699(4) 0.79208(16) 0.0625(8) Uani 1 1 d . . . O4 O 0.51451(15) 0.1049(4) 0.70060(17) 0.0619(9) 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 Cd1 0.03773(13) 0.03164(13) 0.04377(14) 0.00216(15) -0.0001(2) -0.00001(11) C1 0.0370(18) 0.0357(18) 0.054(3) 0.002(2) 0.007(2) 0.0039(15) C2 0.043(3) 0.045(3) 0.130(5) -0.023(3) 0.013(3) 0.004(2) C3 0.051(3) 0.052(3) 0.112(4) -0.018(3) 0.014(2) 0.005(2) C4 0.0396(18) 0.0357(19) 0.058(2) -0.007(3) 0.005(3) -0.0049(15) C5 0.044(2) 0.039(2) 0.069(3) 0.007(3) -0.005(3) -0.0006(16) C6 0.0386(18) 0.045(2) 0.062(4) -0.003(2) -0.002(2) 0.0008(15) C7 0.055(2) 0.0374(19) 0.048(2) 0.000(3) 0.002(3) -0.0041(16) C8 0.044(2) 0.034(2) 0.080(4) 0.001(3) -0.001(3) 0.0008(16) C9 0.0344(18) 0.043(2) 0.071(5) 0.005(2) -0.004(2) -0.0038(16) C10 0.046(2) 0.045(2) 0.046(2) -0.011(3) 0.001(2) -0.0081(16) C11 0.053(2) 0.042(3) 0.043(3) 0.0007(19) 0.0019(19) 0.0028(19) C12 0.065(3) 0.045(3) 0.056(3) 0.009(2) 0.002(2) 0.021(2) C13 0.060(3) 0.049(3) 0.046(2) -0.003(2) 0.0150(19) 0.009(2) C14 0.052(2) 0.040(3) 0.046(3) 0.0003(19) 0.0073(19) -0.0051(19) C15 0.074(3) 0.049(3) 0.032(2) -0.0024(19) 0.001(2) 0.001(2) C16 0.057(3) 0.058(3) 0.041(3) 0.006(2) -0.0010(19) 0.0009(19) C17 0.044(2) 0.050(3) 0.040(2) 0.002(2) -0.0066(17) -0.0039(18) C18 0.065(3) 0.037(3) 0.061(3) 0.001(2) -0.004(2) -0.006(2) C19 0.060(3) 0.053(3) 0.043(2) 0.001(2) -0.009(2) 0.001(2) C20 0.046(2) 0.052(3) 0.049(3) 0.009(2) -0.001(2) -0.010(2) N1 0.0355(14) 0.0348(16) 0.079(2) 0.002(2) 0.000(2) -0.0017(13) N2 0.0400(16) 0.0341(16) 0.070(2) 0.0032(18) 0.0086(17) 0.0001(13) N3 0.054(2) 0.041(2) 0.0413(19) 0.0030(16) 0.0003(16) 0.0044(18) N4 0.058(2) 0.042(2) 0.0395(19) 0.0041(15) 0.0000(15) 0.0049(16) O1 0.0574(16) 0.0492(18) 0.079(2) 0.0118(15) -0.0167(15) -0.0151(14) O2 0.0413(16) 0.0450(17) 0.097(3) -0.0142(15) 0.0005(15) -0.0076(13) O3 0.087(2) 0.0483(19) 0.052(2) 0.0078(13) -0.0130(16) -0.0151(16) O4 0.073(2) 0.060(2) 0.0526(18) 0.0146(17) 0.0101(16) 0.0175(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.242(3) . ? Cd1 N1 2.262(3) . ? Cd1 O1 2.325(2) 3_485 ? Cd1 O4 2.334(3) 2_664 ? Cd1 O2 2.365(3) 3_485 ? Cd1 O3 2.379(3) 2_664 ? Cd1 C10 2.670(3) 3_485 ? Cd1 C20 2.695(4) 2_664 ? C1 N1 1.313(4) . ? C1 N2 1.345(4) . ? C1 H1A 0.9300 . ? C2 C3 1.338(6) . ? C2 N1 1.387(5) . ? C2 H2A 0.9300 . ? C3 N2 1.353(5) . ? C3 H3A 0.9300 . ? C4 C5 1.382(5) . ? C4 C9 1.393(5) . ? C4 N2 1.417(4) . ? C5 C6 1.393(5) . ? C5 H5A 0.9300 . ? C6 C7 1.409(5) . ? C6 H6A 0.9300 . ? C7 C8 1.360(5) . ? C7 C10 1.517(4) . ? C8 C9 1.391(5) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 O1 1.253(4) . ? C10 O2 1.260(4) . ? C10 Cd1 2.670(3) 3_585 ? C11 N3 1.308(5) . ? C11 N4 1.349(5) . ? C11 H11A 0.9300 . ? C12 C13 1.342(6) . ? C12 N3 1.346(5) . ? C12 H12A 0.9300 . ? C13 N4 1.386(5) . ? C13 H13A 0.9300 . ? C14 C19 1.382(6) . ? C14 C15 1.388(5) . ? C14 N4 1.426(5) . ? C15 C16 1.387(6) . ? C15 H15A 0.9300 . ? C16 C17 1.372(6) . ? C16 H16A 0.9300 . ? C17 C18 1.392(6) . ? C17 C20 1.477(6) . ? C18 C19 1.405(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 O3 1.241(4) . ? C20 O4 1.267(5) . ? C20 Cd1 2.695(4) 2_665 ? O1 Cd1 2.325(2) 3_585 ? O2 Cd1 2.365(3) 3_585 ? O3 Cd1 2.379(3) 2_665 ? O4 Cd1 2.334(3) 2_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 N3 Cd1 N1 112.54(14) . . ? N3 Cd1 O1 93.17(11) . 3_485 ? N1 Cd1 O1 138.38(11) . 3_485 ? N3 Cd1 O4 136.39(12) . 2_664 ? N1 Cd1 O4 89.22(13) . 2_664 ? O1 Cd1 O4 93.90(10) 3_485 2_664 ? N3 Cd1 O2 94.13(12) . 3_485 ? N1 Cd1 O2 88.65(10) . 3_485 ? O1 Cd1 O2 56.10(10) 3_485 3_485 ? O4 Cd1 O2 124.93(12) 2_664 3_485 ? N3 Cd1 O3 84.94(12) . 2_664 ? N1 Cd1 O3 93.09(10) . 2_664 ? O1 Cd1 O3 122.41(10) 3_485 2_664 ? O4 Cd1 O3 55.43(12) 2_664 2_664 ? O2 Cd1 O3 178.23(9) 3_485 2_664 ? N3 Cd1 C10 94.72(13) . 3_485 ? N1 Cd1 C10 114.04(11) . 3_485 ? O1 Cd1 C10 27.96(10) 3_485 3_485 ? O4 Cd1 C10 110.75(14) 2_664 3_485 ? O2 Cd1 C10 28.15(10) 3_485 3_485 ? O3 Cd1 C10 150.37(12) 2_664 3_485 ? N3 Cd1 C20 110.87(14) . 2_664 ? N1 Cd1 C20 91.06(12) . 2_664 ? O1 Cd1 C20 110.33(12) 3_485 2_664 ? O4 Cd1 C20 28.01(12) 2_664 2_664 ? O2 Cd1 C20 152.93(13) 3_485 2_664 ? O3 Cd1 C20 27.42(11) 2_664 2_664 ? C10 Cd1 C20 134.12(15) 3_485 2_664 ? N1 C1 N2 110.9(3) . . ? N1 C1 H1A 124.5 . . ? N2 C1 H1A 124.5 . . ? C3 C2 N1 106.6(4) . . ? C3 C2 H2A 126.7 . . ? N1 C2 H2A 126.7 . . ? C2 C3 N2 109.6(4) . . ? C2 C3 H3A 125.2 . . ? N2 C3 H3A 125.2 . . ? C5 C4 C9 121.6(3) . . ? C5 C4 N2 118.0(3) . . ? C9 C4 N2 120.2(3) . . ? C4 C5 C6 118.8(3) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 119.4(3) . . ? C8 C7 C10 121.5(3) . . ? C6 C7 C10 119.1(3) . . ? C7 C8 C9 121.7(3) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C9 C4 118.2(4) . . ? C8 C9 H9A 120.9 . . ? C4 C9 H9A 120.9 . . ? O1 C10 O2 122.8(3) . . ? O1 C10 C7 118.8(3) . . ? O2 C10 C7 118.4(3) . . ? O1 C10 Cd1 60.48(18) . 3_585 ? O2 C10 Cd1 62.34(18) . 3_585 ? C7 C10 Cd1 177.6(4) . 3_585 ? N3 C11 N4 110.8(4) . . ? N3 C11 H11A 124.6 . . ? N4 C11 H11A 124.6 . . ? C13 C12 N3 109.9(4) . . ? C13 C12 H12A 125.0 . . ? N3 C12 H12A 125.0 . . ? C12 C13 N4 106.2(3) . . ? C12 C13 H13A 126.9 . . ? N4 C13 H13A 126.9 . . ? C19 C14 C15 121.3(4) . . ? C19 C14 N4 119.1(4) . . ? C15 C14 N4 119.4(4) . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 118.9(4) . . ? C16 C17 C20 120.6(4) . . ? C18 C17 C20 120.5(4) . . ? C17 C18 C19 121.6(4) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C14 C19 C18 117.6(4) . . ? C14 C19 H19A 121.2 . . ? C18 C19 H19A 121.2 . . ? O3 C20 O4 121.8(4) . . ? O3 C20 C17 118.6(4) . . ? O4 C20 C17 119.6(4) . . ? O3 C20 Cd1 61.9(2) . 2_665 ? O4 C20 Cd1 59.9(2) . 2_665 ? C17 C20 Cd1 179.1(3) . 2_665 ? C1 N1 C2 106.8(3) . . ? C1 N1 Cd1 131.1(2) . . ? C2 N1 Cd1 121.4(3) . . ? C1 N2 C3 105.9(3) . . ? C1 N2 C4 127.1(3) . . ? C3 N2 C4 126.8(3) . . ? C11 N3 C12 106.9(3) . . ? C11 N3 Cd1 127.2(3) . . ? C12 N3 Cd1 125.9(3) . . ? C11 N4 C13 106.1(3) . . ? C11 N4 C14 127.3(3) . . ? C13 N4 C14 126.6(3) . . ? C10 O1 Cd1 91.6(2) . 3_585 ? C10 O2 Cd1 89.5(2) . 3_585 ? C20 O3 Cd1 90.6(3) . 2_665 ? C20 O4 Cd1 92.1(3) . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.252 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.044 data_4 _database_code_depnum_ccdc_archive 'CCDC 795331' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25.9 H27.85 Cd N5.30 O6.05' _chemical_formula_sum 'C25.9 H27.85 Cd N5.30 O6.05' _chemical_formula_weight 622.58 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 Tetragonal _symmetry_space_group_name_H-M P42(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z' 'y+1/2, -x+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 18.8725(15) _cell_length_b 18.8725(15) _cell_length_c 8.0221(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2857.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 66 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1281 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14296 _diffrn_reflns_av_R_equivalents 0.1077 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2503 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Except the watter molecules discovered in the structure, there are still solvent accessible void of 20.9% of the crystalvolume, which are occupied by the highly disordered molecules of DMF that were used as solvent in the synthesis ; _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^)+(0.0083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.36(6) _refine_ls_number_reflns 2503 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.715599(18) 0.715599(18) 0.5000 0.04510(16) Uani 1 2 d S . . C1 C 0.8352(3) 0.8012(3) 0.2251(8) 0.095(3) Uani 1 1 d . . . H1A H 0.7904 0.8137 0.2739 0.143 Uiso 1 1 calc R . . H1B H 0.8291 0.7932 0.1078 0.143 Uiso 1 1 calc R . . H1C H 0.8683 0.8391 0.2419 0.143 Uiso 1 1 calc R . . C2 C 0.8622(3) 0.7364(3) 0.3042(7) 0.0515(17) Uani 1 1 d . . . C3 C 0.8758(3) 0.6476(3) 0.4730(9) 0.0607(17) Uani 1 1 d . . . H3A H 0.8672 0.6149 0.5573 0.073 Uiso 1 1 calc R . . C4 C 0.9347(3) 0.6499(4) 0.3769(8) 0.0655(19) Uani 1 1 d . . . H4A H 0.9741 0.6205 0.3839 0.079 Uiso 1 1 calc R . . C5 C 0.9715(4) 0.7233(5) 0.1311(10) 0.063(2) Uani 1 1 d . . . C6 C 1.0419(4) 0.7365(4) 0.1642(9) 0.059(2) Uani 1 1 d . . . H6A H 1.0580 0.7355 0.2737 0.071 Uiso 1 1 calc R . . C7 C 0.9477(3) 0.7232(4) -0.0303(8) 0.075(2) Uani 1 1 d . . . H7A H 0.9008 0.7118 -0.0536 0.090 Uiso 1 1 calc R . . C8 C 1.0878(3) 0.7510(3) 0.0395(7) 0.057(2) Uani 1 1 d . . . H8A H 1.1351 0.7596 0.0643 0.068 Uiso 1 1 calc R . . C9 C 0.9933(4) 0.7401(4) -0.1574(8) 0.064(3) Uani 1 1 d . . . H9A H 0.9762 0.7427 -0.2659 0.077 Uiso 1 1 calc R . . C10 C 1.0649(4) 0.7533(4) -0.1271(9) 0.056(2) Uani 1 1 d . . . C11 C 1.1151(4) 0.7699(4) -0.2663(8) 0.0592(19) Uani 1 1 d . . . N1 N 0.8299(2) 0.7022(3) 0.4255(5) 0.0544(14) Uani 1 1 d . . . N2 N 0.9243(3) 0.7052(3) 0.2660(6) 0.0531(13) Uani 1 1 d . . . O1 O 1.1796(2) 0.7715(3) -0.2295(5) 0.0762(14) Uani 1 1 d . . . O2 O 1.0928(2) 0.7795(3) -0.4095(5) 0.0722(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0504(2) 0.0504(2) 0.0346(3) 0.0017(4) -0.0017(4) 0.0035(3) C1 0.096(6) 0.091(6) 0.099(5) 0.054(5) 0.050(4) 0.029(5) C2 0.049(4) 0.062(5) 0.044(4) 0.013(3) 0.011(3) 0.008(3) C3 0.060(4) 0.061(4) 0.061(5) 0.011(4) 0.010(4) 0.003(3) C4 0.060(5) 0.085(6) 0.052(4) 0.002(4) 0.005(4) 0.016(4) C5 0.054(5) 0.087(6) 0.047(5) 0.004(5) 0.007(4) -0.011(5) C6 0.047(5) 0.085(6) 0.046(5) -0.009(4) -0.003(4) -0.005(5) C7 0.057(4) 0.130(6) 0.038(6) 0.012(5) 0.000(4) -0.026(4) C8 0.047(4) 0.085(5) 0.039(5) -0.014(3) -0.003(3) -0.008(3) C9 0.062(5) 0.101(7) 0.029(4) 0.004(4) -0.004(4) -0.011(5) C10 0.051(5) 0.068(6) 0.049(5) 0.005(4) 0.015(4) -0.006(4) C11 0.065(5) 0.064(5) 0.049(4) -0.006(4) 0.020(4) 0.002(4) N1 0.052(3) 0.058(4) 0.054(3) 0.013(3) 0.000(2) 0.008(3) N2 0.053(3) 0.065(4) 0.042(3) 0.009(3) 0.014(3) 0.006(3) O1 0.063(3) 0.119(4) 0.047(2) -0.024(3) 0.016(2) -0.024(3) O2 0.081(3) 0.091(3) 0.045(3) 0.006(3) 0.018(2) 0.015(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 Cd1 N1 2.253(4) 7_556 ? Cd1 N1 2.253(4) . ? Cd1 O1 2.287(4) 6_465 ? Cd1 O1 2.287(4) 3_646 ? Cd1 O2 2.431(4) 6_465 ? Cd1 O2 2.431(4) 3_646 ? Cd1 C11 2.681(6) 6_465 ? Cd1 C11 2.681(6) 3_646 ? C1 C2 1.470(7) . ? C2 N1 1.316(6) . ? C2 N2 1.346(6) . ? C3 C4 1.353(7) . ? C3 N1 1.400(6) . ? C4 N2 1.385(7) . ? C5 C7 1.370(10) . ? C5 C6 1.377(8) . ? C5 N2 1.443(8) . ? C6 C8 1.351(8) . ? C7 C9 1.373(9) . ? C8 C10 1.405(9) . ? C9 C10 1.394(9) . ? C10 C11 1.498(8) . ? C11 O2 1.237(7) . ? C11 O1 1.253(6) . ? C11 Cd1 2.681(6) 4_564 ? O1 Cd1 2.287(4) 4_564 ? O2 Cd1 2.431(4) 4_564 ? 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 106.5(3) 7_556 . ? N1 Cd1 O1 96.68(16) 7_556 6_465 ? N1 Cd1 O1 92.54(16) . 6_465 ? N1 Cd1 O1 92.54(15) 7_556 3_646 ? N1 Cd1 O1 96.68(16) . 3_646 ? O1 Cd1 O1 164.6(3) 6_465 3_646 ? N1 Cd1 O2 86.33(19) 7_556 6_465 ? N1 Cd1 O2 146.95(14) . 6_465 ? O1 Cd1 O2 55.22(13) 6_465 6_465 ? O1 Cd1 O2 113.36(16) 3_646 6_465 ? N1 Cd1 O2 146.95(14) 7_556 3_646 ? N1 Cd1 O2 86.33(19) . 3_646 ? O1 Cd1 O2 113.36(16) 6_465 3_646 ? O1 Cd1 O2 55.22(13) 3_646 3_646 ? O2 Cd1 O2 99.3(2) 6_465 3_646 ? N1 Cd1 C11 90.49(19) 7_556 6_465 ? N1 Cd1 C11 120.2(2) . 6_465 ? O1 Cd1 C11 27.81(14) 6_465 6_465 ? O1 Cd1 C11 140.3(2) 3_646 6_465 ? O2 Cd1 C11 27.46(15) 6_465 6_465 ? O2 Cd1 C11 109.47(18) 3_646 6_465 ? N1 Cd1 C11 120.2(2) 7_556 3_646 ? N1 Cd1 C11 90.49(19) . 3_646 ? O1 Cd1 C11 140.3(2) 6_465 3_646 ? O1 Cd1 C11 27.80(14) 3_646 3_646 ? O2 Cd1 C11 109.47(18) 6_465 3_646 ? O2 Cd1 C11 27.46(15) 3_646 3_646 ? C11 Cd1 C11 129.3(3) 6_465 3_646 ? N1 C2 N2 110.9(5) . . ? N1 C2 C1 124.4(6) . . ? N2 C2 C1 124.6(5) . . ? C4 C3 N1 109.2(6) . . ? C3 C4 N2 105.9(6) . . ? C7 C5 C6 119.9(7) . . ? C7 C5 N2 120.4(6) . . ? C6 C5 N2 119.6(7) . . ? C8 C6 C5 120.8(7) . . ? C9 C7 C5 119.7(6) . . ? C6 C8 C10 120.9(6) . . ? C7 C9 C10 121.3(6) . . ? C9 C10 C8 117.3(6) . . ? C9 C10 C11 121.4(6) . . ? C8 C10 C11 121.4(7) . . ? O2 C11 O1 123.1(6) . . ? O2 C11 C10 120.5(7) . . ? O1 C11 C10 116.4(6) . . ? O2 C11 Cd1 65.0(3) . 4_564 ? O1 C11 Cd1 58.3(3) . 4_564 ? C10 C11 Cd1 172.1(5) . 4_564 ? C2 N1 C3 105.9(5) . . ? C2 N1 Cd1 125.8(4) . . ? C3 N1 Cd1 127.1(4) . . ? C2 N2 C4 107.8(5) . . ? C2 N2 C5 127.2(6) . . ? C4 N2 C5 124.9(6) . . ? C11 O1 Cd1 93.8(4) . 4_564 ? C11 O2 Cd1 87.6(4) . 4_564 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 N2 -1.6(7) . . . . ? C7 C5 C6 C8 1.4(12) . . . . ? N2 C5 C6 C8 177.5(7) . . . . ? C6 C5 C7 C9 -3.5(13) . . . . ? N2 C5 C7 C9 -179.6(8) . . . . ? C5 C6 C8 C10 0.4(11) . . . . ? C5 C7 C9 C10 3.9(12) . . . . ? C7 C9 C10 C8 -2.1(12) . . . . ? C7 C9 C10 C11 178.4(7) . . . . ? C6 C8 C10 C9 0.0(10) . . . . ? C6 C8 C10 C11 179.5(7) . . . . ? C9 C10 C11 O2 7.6(11) . . . . ? C8 C10 C11 O2 -171.9(7) . . . . ? C9 C10 C11 O1 -170.6(7) . . . . ? C8 C10 C11 O1 9.8(10) . . . . ? C9 C10 C11 Cd1 -124(4) . . . 4_564 ? C8 C10 C11 Cd1 56(4) . . . 4_564 ? N2 C2 N1 C3 2.9(7) . . . . ? C1 C2 N1 C3 -175.3(6) . . . . ? N2 C2 N1 Cd1 -165.5(4) . . . . ? C1 C2 N1 Cd1 16.3(8) . . . . ? C4 C3 N1 C2 -0.7(7) . . . . ? C4 C3 N1 Cd1 167.5(4) . . . . ? N1 Cd1 N1 C2 -60.1(5) 7_556 . . . ? O1 Cd1 N1 C2 37.6(5) 6_465 . . . ? O1 Cd1 N1 C2 -154.8(5) 3_646 . . . ? O2 Cd1 N1 C2 49.4(6) 6_465 . . . ? O2 Cd1 N1 C2 150.9(5) 3_646 . . . ? C11 Cd1 N1 C2 40.4(5) 6_465 . . . ? C11 Cd1 N1 C2 178.0(5) 3_646 . . . ? N1 Cd1 N1 C3 133.9(5) 7_556 . . . ? O1 Cd1 N1 C3 -128.3(5) 6_465 . . . ? O1 Cd1 N1 C3 39.3(5) 3_646 . . . ? O2 Cd1 N1 C3 -116.5(5) 6_465 . . . ? O2 Cd1 N1 C3 -15.1(5) 3_646 . . . ? C11 Cd1 N1 C3 -125.5(5) 6_465 . . . ? C11 Cd1 N1 C3 12.1(5) 3_646 . . . ? N1 C2 N2 C4 -4.0(7) . . . . ? C1 C2 N2 C4 174.2(6) . . . . ? N1 C2 N2 C5 174.1(6) . . . . ? C1 C2 N2 C5 -7.7(10) . . . . ? C3 C4 N2 C2 3.3(7) . . . . ? C3 C4 N2 C5 -174.8(6) . . . . ? C7 C5 N2 C2 -56.9(11) . . . . ? C6 C5 N2 C2 127.0(8) . . . . ? C7 C5 N2 C4 120.9(8) . . . . ? C6 C5 N2 C4 -55.2(11) . . . . ? O2 C11 O1 Cd1 -4.9(8) . . . 4_564 ? C10 C11 O1 Cd1 173.3(5) . . . 4_564 ? O1 C11 O2 Cd1 4.6(7) . . . 4_564 ? C10 C11 O2 Cd1 -173.5(6) . . . 4_564 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.369 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.056 data_5 _database_code_depnum_ccdc_archive 'CCDC 795332' #TrackingRef '- Crystal structures (revised).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H29.5 Co N5 O6.25' _chemical_formula_sum 'C26 H29.5 Co N5 O6.3' _chemical_formula_weight 573.97 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z' 'y+1/2, -x+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 18.5718(9) _cell_length_b 18.5718(9) _cell_length_c 7.7776(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2682.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 79 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1195 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10 Sec.' _diffrn_standards_decay_% ? _diffrn_reflns_number 12408 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.06 _reflns_number_total 2128 _reflns_number_gt 1839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. except the watter molecules discovered in the structure, there are still solvent accessible void of 16.1% of the crystal volume, which are occupied by the highly disordered molecules of DMF that were used as solvent in the synthesis ; _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^)+(0.0880P)^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 SHELXL _refine_ls_extinction_coef 0.0100(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(3) _refine_ls_number_reflns 2128 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Co1 Co 0.27655(2) 0.27655(2) 0.5000 0.0363(3) Uani 1 2 d S . . C1 C -0.1223(3) 0.2314(2) -0.2832(6) 0.0544(12) Uani 1 1 d . . . C2 C -0.0704(2) 0.2459(2) -0.1385(5) 0.0471(12) Uani 1 1 d . . . C3 C -0.0942(2) 0.2484(2) 0.0308(6) 0.0537(12) Uani 1 1 d . . . H3A H -0.1427 0.2405 0.0541 0.064 Uiso 1 1 calc R . . C4 C 0.0017(3) 0.2567(3) -0.1688(6) 0.0595(13) Uani 1 1 d . . . H4A H 0.0189 0.2535 -0.2809 0.071 Uiso 1 1 calc R . . C5 C -0.0479(2) 0.2622(3) 0.1648(6) 0.0527(12) Uani 1 1 d . . . H5A H -0.0647 0.2635 0.2774 0.063 Uiso 1 1 calc R . . C6 C 0.0492(2) 0.2720(3) -0.0376(6) 0.0621(13) Uani 1 1 d . . . H6A H 0.0975 0.2808 -0.0619 0.075 Uiso 1 1 calc R . . C7 C 0.0251(2) 0.2743(3) 0.1290(6) 0.0503(11) Uani 1 1 d . . . C8 C 0.0645(2) 0.3475(2) 0.3807(6) 0.0521(11) Uani 1 1 d . . . H8A H 0.0256 0.3789 0.3872 0.063 Uiso 1 1 calc R . . C9 C 0.1347(2) 0.2561(2) 0.3055(5) 0.0486(10) Uani 1 1 d . . . C10 C 0.1607(3) 0.1895(3) 0.2285(7) 0.089(2) Uani 1 1 d . . . H10A H 0.1278 0.1741 0.1408 0.134 Uiso 1 1 calc R . . H10B H 0.1643 0.1529 0.3155 0.134 Uiso 1 1 calc R . . H10C H 0.2073 0.1975 0.1786 0.134 Uiso 1 1 calc R . . C11 C 0.1239(2) 0.3486(2) 0.4795(6) 0.0522(11) Uani 1 1 d . . . H11A H 0.1336 0.3823 0.5650 0.063 Uiso 1 1 calc R . . N1 N 0.07237(18) 0.2903(2) 0.2670(4) 0.0469(9) Uani 1 1 d . . . N2 N 0.16909(16) 0.29086(16) 0.4331(4) 0.0416(8) Uani 1 1 d . . . O1 O -0.10164(18) 0.22058(18) -0.4322(4) 0.0657(9) Uani 1 1 d . . . O2 O -0.18908(19) 0.23509(18) -0.2484(4) 0.0646(9) 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 Co1 0.0410(3) 0.0410(3) 0.0269(4) 0.0003(3) -0.0003(3) 0.0037(3) C1 0.072(3) 0.045(3) 0.046(3) 0.013(2) -0.014(2) -0.010(2) C2 0.049(2) 0.062(3) 0.031(2) 0.0060(19) -0.008(2) -0.008(2) C3 0.048(2) 0.071(3) 0.042(3) 0.003(2) -0.0004(19) -0.008(2) C4 0.065(3) 0.084(4) 0.030(2) 0.002(2) 0.010(2) -0.001(3) C5 0.040(2) 0.086(3) 0.033(2) -0.001(2) -0.0044(18) -0.001(2) C6 0.036(2) 0.107(4) 0.043(3) -0.005(3) -0.0011(18) -0.008(2) C7 0.041(2) 0.067(3) 0.042(2) -0.006(3) -0.0051(18) -0.003(2) C8 0.039(2) 0.068(3) 0.049(3) -0.011(2) -0.002(2) 0.003(2) C9 0.049(2) 0.053(3) 0.044(2) -0.0106(19) -0.0058(19) 0.007(2) C10 0.098(4) 0.089(4) 0.080(4) -0.046(3) -0.043(3) 0.031(3) C11 0.042(2) 0.060(2) 0.054(3) -0.016(2) 0.000(2) 0.0038(18) N1 0.0391(18) 0.063(2) 0.0382(19) -0.0055(18) -0.0031(15) -0.0009(16) N2 0.0443(17) 0.0461(19) 0.0343(17) -0.0064(14) -0.0033(14) 0.0055(15) O1 0.083(2) 0.075(2) 0.0395(18) -0.0062(16) -0.0134(16) 0.0072(19) O2 0.060(2) 0.082(2) 0.0517(19) 0.0189(17) -0.0176(16) -0.0218(17) _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 Co1 O2 2.070(3) 3_556 ? Co1 O2 2.070(3) 6 ? Co1 N2 2.080(3) . ? Co1 N2 2.080(3) 7_556 ? Co1 O1 2.323(3) 3_556 ? Co1 O1 2.323(3) 6 ? C1 O1 1.237(5) . ? C1 O2 1.272(6) . ? C1 C2 1.506(6) . ? C2 C4 1.374(7) . ? C2 C3 1.389(6) . ? C3 C5 1.376(6) . ? C3 H3A 0.9300 . ? C4 C6 1.379(7) . ? C4 H4A 0.9300 . ? C5 C7 1.401(6) . ? C5 H5A 0.9300 . ? C6 C7 1.372(7) . ? C6 H6A 0.9300 . ? C7 N1 1.419(5) . ? C8 C11 1.344(6) . ? C8 N1 1.390(5) . ? C8 H8A 0.9300 . ? C9 N2 1.346(5) . ? C9 N1 1.353(5) . ? C9 C10 1.457(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.409(5) . ? C11 H11A 0.9300 . ? O1 Co1 2.323(3) 4_454 ? O2 Co1 2.070(3) 4_454 ? 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 O2 Co1 O2 163.4(2) 3_556 6 ? O2 Co1 N2 95.55(13) 3_556 . ? O2 Co1 N2 94.18(13) 6 . ? O2 Co1 N2 94.18(13) 3_556 7_556 ? O2 Co1 N2 95.55(13) 6 7_556 ? N2 Co1 N2 107.93(18) . 7_556 ? O2 Co1 O1 59.17(13) 3_556 3_556 ? O2 Co1 O1 108.02(13) 6 3_556 ? N2 Co1 O1 87.39(12) . 3_556 ? N2 Co1 O1 151.01(12) 7_556 3_556 ? O2 Co1 O1 108.02(13) 3_556 6 ? O2 Co1 O1 59.17(13) 6 6 ? N2 Co1 O1 151.01(12) . 6 ? N2 Co1 O1 87.39(12) 7_556 6 ? O1 Co1 O1 90.39(17) 3_556 6 ? O1 C1 O2 120.7(4) . . ? O1 C1 C2 122.1(4) . . ? O2 C1 C2 117.1(4) . . ? C4 C2 C3 117.9(4) . . ? C4 C2 C1 121.4(4) . . ? C3 C2 C1 120.7(4) . . ? C5 C3 C2 121.7(4) . . ? C5 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C2 C4 C6 121.8(4) . . ? C2 C4 H4A 119.1 . . ? C6 C4 H4A 119.1 . . ? C3 C5 C7 118.9(4) . . ? C3 C5 H5A 120.5 . . ? C7 C5 H5A 120.5 . . ? C7 C6 C4 119.7(4) . . ? C7 C6 H6A 120.1 . . ? C4 C6 H6A 120.1 . . ? C6 C7 C5 119.9(4) . . ? C6 C7 N1 121.2(4) . . ? C5 C7 N1 118.8(4) . . ? C11 C8 N1 106.8(4) . . ? C11 C8 H8A 126.6 . . ? N1 C8 H8A 126.6 . . ? N2 C9 N1 110.1(4) . . ? N2 C9 C10 123.6(4) . . ? N1 C9 C10 126.3(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 N2 109.3(4) . . ? C8 C11 H11A 125.4 . . ? N2 C11 H11A 125.4 . . ? C9 N1 C8 107.9(3) . . ? C9 N1 C7 126.8(4) . . ? C8 N1 C7 125.2(4) . . ? C9 N2 C11 105.7(3) . . ? C9 N2 Co1 125.4(3) . . ? C11 N2 Co1 127.2(2) . . ? C1 O1 Co1 84.7(3) . 4_454 ? C1 O2 Co1 95.4(3) . 4_454 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C4 8.2(7) . . . . ? O2 C1 C2 C4 -167.6(4) . . . . ? O1 C1 C2 C3 -171.3(4) . . . . ? O2 C1 C2 C3 12.8(6) . . . . ? C4 C2 C3 C5 1.0(7) . . . . ? C1 C2 C3 C5 -179.4(4) . . . . ? C3 C2 C4 C6 -2.3(8) . . . . ? C1 C2 C4 C6 178.1(5) . . . . ? C2 C3 C5 C7 0.2(8) . . . . ? C2 C4 C6 C7 2.3(9) . . . . ? C4 C6 C7 C5 -1.0(9) . . . . ? C4 C6 C7 N1 -179.7(5) . . . . ? C3 C5 C7 C6 -0.3(8) . . . . ? C3 C5 C7 N1 178.5(4) . . . . ? N1 C8 C11 N2 -1.8(5) . . . . ? N2 C9 N1 C8 -3.1(5) . . . . ? C10 C9 N1 C8 174.2(5) . . . . ? N2 C9 N1 C7 173.2(4) . . . . ? C10 C9 N1 C7 -9.5(8) . . . . ? C11 C8 N1 C9 3.0(5) . . . . ? C11 C8 N1 C7 -173.4(4) . . . . ? C6 C7 N1 C9 -54.6(7) . . . . ? C5 C7 N1 C9 126.6(5) . . . . ? C6 C7 N1 C8 121.0(6) . . . . ? C5 C7 N1 C8 -57.7(7) . . . . ? N1 C9 N2 C11 2.0(5) . . . . ? C10 C9 N2 C11 -175.4(5) . . . . ? N1 C9 N2 Co1 -164.2(3) . . . . ? C10 C9 N2 Co1 18.4(7) . . . . ? C8 C11 N2 C9 -0.1(5) . . . . ? C8 C11 N2 Co1 165.8(3) . . . . ? O2 Co1 N2 C9 -155.7(3) 3_556 . . . ? O2 Co1 N2 C9 37.7(4) 6 . . . ? N2 Co1 N2 C9 -59.5(3) 7_556 . . . ? O1 Co1 N2 C9 145.6(3) 3_556 . . . ? O1 Co1 N2 C9 59.5(5) 6 . . . ? O2 Co1 N2 C11 41.1(4) 3_556 . . . ? O2 Co1 N2 C11 -125.5(3) 6 . . . ? N2 Co1 N2 C11 137.3(4) 7_556 . . . ? O1 Co1 N2 C11 -17.6(3) 3_556 . . . ? O1 Co1 N2 C11 -103.7(4) 6 . . . ? O2 C1 O1 Co1 2.5(4) . . . 4_454 ? C2 C1 O1 Co1 -173.2(4) . . . 4_454 ? O1 C1 O2 Co1 -2.8(5) . . . 4_454 ? C2 C1 O2 Co1 173.1(3) . . . 4_454 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.105 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.169 data_6 _database_code_depnum_ccdc_archive 'CCDC 795333' #TrackingRef '- Crystal structures .CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30.80 H37.8 Cd N6.20 O6.20' _chemical_formula_sum 'C30.80 H37.8 Cd N6.20 O6.20' _chemical_formula_weight 706.47 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 orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 15.573(2) _cell_length_b 19.416(3) _cell_length_c 19.664(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5945.8(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 30.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11183 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 22.24 _reflns_number_total 3653 _reflns_number_gt 2501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are still solvent accessible void of 37.7% of the crystal, which are occupied by the highly disordered molecules of DMA that were used as solvent in the synthesis ; _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^)+(0.0206P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(4) _refine_ls_number_reflns 3653 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 1.00612(4) 0.77264(2) 0.55798(6) 0.04078(17) Uani 1 1 d . . . C1 C 0.8966(6) 0.8795(4) 0.5547(8) 0.052(2) Uani 1 1 d . . . C2 C 0.8267(6) 0.9321(4) 0.5463(7) 0.054(3) Uani 1 1 d . . . C3 C 0.7425(5) 0.9125(4) 0.5406(5) 0.053(3) Uani 1 1 d . . . H3A H 0.7279 0.8662 0.5430 0.064 Uiso 1 1 calc R . . C4 C 0.6793(6) 0.9614(4) 0.5313(5) 0.058(3) Uani 1 1 d . . . H4A H 0.6221 0.9481 0.5287 0.070 Uiso 1 1 calc R . . C5 C 0.7013(7) 1.0314(5) 0.5258(4) 0.052(3) Uani 1 1 d . . . C6 C 0.7868(7) 1.0509(5) 0.5300(5) 0.072(4) Uani 1 1 d . . . H6A H 0.8020 1.0970 0.5263 0.086 Uiso 1 1 calc R . . C7 C 0.8492(5) 1.0013(5) 0.5397(5) 0.061(4) Uani 1 1 d . . . H7A H 0.9066 1.0141 0.5419 0.074 Uiso 1 1 calc R . . C8 C 0.8383(6) 0.6577(4) 0.6144(4) 0.057(3) Uani 1 1 d . . . H8A H 0.8606 0.7007 0.6308 0.086 Uiso 1 1 calc R . . H8B H 0.8447 0.6231 0.6489 0.086 Uiso 1 1 calc R . . H8C H 0.7786 0.6629 0.6034 0.086 Uiso 1 1 calc R . . C9 C 0.8876(6) 0.6360(4) 0.5510(7) 0.047(2) Uani 1 1 d . . . C10 C 0.9301(6) 0.5761(5) 0.4654(5) 0.056(3) Uani 1 1 d . . . H10A H 0.9330 0.5426 0.4316 0.067 Uiso 1 1 calc R . . C11 C 0.9844(6) 0.6267(5) 0.4736(4) 0.051(2) Uani 1 1 d . . . H11A H 1.0333 0.6354 0.4477 0.062 Uiso 1 1 calc R . . C21 C 1.1296(6) 0.7741(5) 0.4623(6) 0.051(3) Uani 1 1 d . . . C22 C 1.1998(6) 0.7737(5) 0.4070(4) 0.045(2) Uani 1 1 d . . . C23 C 1.1842(7) 0.7874(6) 0.3422(5) 0.072(4) Uani 1 1 d . . . H23A H 1.1282 0.7957 0.3278 0.086 Uiso 1 1 calc R . . C24 C 1.2490(10) 0.7893(5) 0.2974(7) 0.070(3) Uani 1 1 d . . . H24A H 1.2373 0.8031 0.2531 0.084 Uiso 1 1 calc R . . C25 C 1.3307(6) 0.7719(5) 0.3137(5) 0.051(3) Uani 1 1 d . . . C26 C 1.3497(6) 0.7554(4) 0.3785(5) 0.050(3) Uani 1 1 d . . . H26A H 1.4056 0.7443 0.3910 0.061 Uiso 1 1 calc R . . C27 C 1.2827(6) 0.7554(4) 0.4272(5) 0.053(3) Uani 1 1 d . . . H27A H 1.2937 0.7433 0.4722 0.063 Uiso 1 1 calc R . . C28 C 1.1624(7) 0.6993(5) 0.6764(5) 0.081(3) Uani 1 1 d . . . H28A H 1.1476 0.6888 0.6301 0.122 Uiso 1 1 calc R . . H28B H 1.1620 0.6577 0.7028 0.122 Uiso 1 1 calc R . . H28C H 1.2187 0.7195 0.6778 0.122 Uiso 1 1 calc R . . C29 C 1.0988(6) 0.7487(5) 0.7048(6) 0.056(3) Uani 1 1 d . . . C30 C 0.9850(7) 0.8080(5) 0.7162(5) 0.075(3) Uani 1 1 d . . . H30A H 0.9331 0.8301 0.7074 0.090 Uiso 1 1 calc R . . C31 C 1.0263(7) 0.8094(6) 0.7762(5) 0.089(4) Uani 1 1 d . . . H31A H 1.0073 0.8301 0.8161 0.107 Uiso 1 1 calc R . . N1 N 0.9547(4) 0.6655(3) 0.5290(4) 0.048(2) Uani 1 1 d . . . N2 N 0.8679(5) 0.5803(4) 0.5150(4) 0.047(2) Uani 1 1 d . . . N3 N 1.0305(6) 0.7691(4) 0.6694(5) 0.048(3) Uani 1 1 d . . . N4 N 1.0999(5) 0.7756(5) 0.7673(3) 0.059(2) Uani 1 1 d . . . O1 O 0.8713(3) 0.8187(3) 0.5664(4) 0.0513(17) Uani 1 1 d . . . O2 O 0.9731(3) 0.8951(3) 0.5501(6) 0.065(2) Uani 1 1 d . . . O3 O 1.1481(4) 0.7652(3) 0.5246(3) 0.0577(18) Uani 1 1 d . . . O4 O 1.0548(6) 0.7837(4) 0.4401(4) 0.058(2) 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 Cd1 0.0333(3) 0.0483(3) 0.0408(3) -0.0002(7) -0.0013(6) -0.0005(4) C1 0.051(6) 0.048(5) 0.058(6) -0.021(9) -0.023(10) -0.003(5) C2 0.052(6) 0.025(5) 0.086(9) 0.010(6) 0.020(7) 0.006(5) C3 0.032(5) 0.045(5) 0.082(10) 0.007(5) 0.001(6) 0.003(5) C4 0.044(6) 0.035(5) 0.097(10) 0.005(6) 0.002(5) -0.006(5) C5 0.051(7) 0.052(6) 0.052(6) -0.010(5) 0.002(5) 0.002(6) C6 0.044(6) 0.040(6) 0.131(12) 0.004(6) 0.004(7) -0.005(6) C7 0.037(5) 0.065(6) 0.083(12) -0.016(7) 0.001(5) 0.012(6) C8 0.060(7) 0.048(6) 0.064(6) -0.008(5) 0.004(6) -0.010(5) C9 0.059(6) 0.035(5) 0.048(6) 0.029(7) 0.005(8) 0.008(5) C10 0.056(7) 0.052(7) 0.058(7) -0.020(5) -0.002(6) 0.011(6) C11 0.061(7) 0.049(5) 0.044(5) 0.002(5) 0.007(6) -0.007(6) C21 0.025(6) 0.046(6) 0.082(8) -0.010(6) 0.003(6) -0.011(6) C22 0.029(5) 0.060(6) 0.046(6) -0.012(6) 0.007(4) -0.003(6) C23 0.049(8) 0.148(12) 0.019(6) -0.011(7) 0.002(6) -0.008(7) C24 0.051(6) 0.112(9) 0.047(8) 0.001(7) -0.002(7) 0.010(10) C25 0.051(7) 0.066(8) 0.037(7) 0.015(6) 0.010(6) -0.008(6) C26 0.029(6) 0.065(7) 0.057(7) 0.009(5) 0.017(5) 0.002(5) C27 0.055(7) 0.059(7) 0.045(6) -0.005(5) -0.010(5) 0.002(6) C28 0.093(9) 0.087(8) 0.063(7) 0.004(6) 0.003(7) 0.034(8) C29 0.032(6) 0.073(8) 0.064(8) 0.013(6) 0.003(6) 0.010(6) C30 0.054(7) 0.099(8) 0.072(7) -0.021(6) -0.011(6) 0.024(7) C31 0.065(8) 0.163(12) 0.039(6) -0.023(6) -0.010(6) 0.027(8) N1 0.024(4) 0.055(5) 0.064(6) 0.005(4) -0.001(4) -0.007(4) N2 0.046(5) 0.034(5) 0.061(5) -0.011(4) 0.010(4) -0.010(4) N3 0.042(7) 0.056(5) 0.047(5) -0.012(4) -0.007(4) -0.002(5) N4 0.044(6) 0.104(6) 0.030(5) -0.015(5) 0.001(4) 0.021(6) O1 0.035(3) 0.058(4) 0.061(4) -0.017(5) -0.013(4) 0.002(3) O2 0.039(4) 0.057(3) 0.098(6) 0.012(5) -0.010(6) 0.000(3) O3 0.049(4) 0.087(5) 0.037(4) 0.001(4) 0.002(3) 0.007(4) O4 0.037(6) 0.084(6) 0.053(5) 0.020(4) 0.006(4) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.225(10) . ? Cd1 O1 2.289(5) . ? Cd1 N1 2.300(7) . ? Cd1 O3 2.311(6) . ? Cd1 O2 2.437(5) . ? Cd1 O4 2.448(7) . ? Cd1 C1 2.686(8) . ? Cd1 C21 2.691(9) . ? C1 O2 1.232(9) . ? C1 O1 1.266(9) . ? C1 C2 1.502(10) . ? C2 C3 1.371(10) . ? C2 C7 1.393(10) . ? C3 C4 1.379(10) . ? C3 H3A 0.9300 . ? C4 C5 1.404(10) . ? C4 H4A 0.9300 . ? C5 C6 1.387(11) . ? C5 N2 1.452(10) 4_655 ? C6 C7 1.381(11) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.524(13) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N1 1.268(9) . ? C9 N2 1.329(11) . ? C10 C11 1.307(10) . ? C10 N2 1.378(10) . ? C10 H10A 0.9300 . ? C11 N1 1.404(9) . ? C11 H11A 0.9300 . ? C21 O4 1.258(11) . ? C21 O3 1.272(10) . ? C21 C22 1.542(11) . ? C22 C23 1.324(12) . ? C22 C27 1.396(12) . ? C23 C24 1.340(16) . ? C23 H23A 0.9300 . ? C24 C25 1.355(15) . ? C24 H24A 0.9300 . ? C25 C26 1.347(12) . ? C25 N4 1.417(11) 8_744 ? C26 C27 1.417(11) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.488(12) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N3 1.332(12) . ? C29 N4 1.335(11) . ? C30 C31 1.344(12) . ? C30 N3 1.386(12) . ? C30 H30A 0.9300 . ? C31 N4 1.332(11) . ? C31 H31A 0.9300 . ? N2 C5 1.452(11) 4_645 ? N4 C25 1.417(11) 8_745 ? 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 Cd1 O1 95.6(3) . . ? N3 Cd1 N1 106.0(3) . . ? O1 Cd1 N1 93.0(2) . . ? N3 Cd1 O3 96.5(3) . . ? O1 Cd1 O3 157.3(2) . . ? N1 Cd1 O3 101.9(2) . . ? N3 Cd1 O2 97.4(3) . . ? O1 Cd1 O2 55.23(19) . . ? N1 Cd1 O2 142.4(2) . . ? O3 Cd1 O2 104.2(2) . . ? N3 Cd1 O4 151.9(3) . . ? O1 Cd1 O4 108.6(3) . . ? N1 Cd1 O4 87.3(3) . . ? O3 Cd1 O4 56.0(2) . . ? O2 Cd1 O4 85.4(3) . . ? N3 Cd1 C1 99.0(4) . . ? O1 Cd1 C1 28.0(2) . . ? N1 Cd1 C1 118.1(2) . . ? O3 Cd1 C1 130.4(3) . . ? O2 Cd1 C1 27.28(19) . . ? O4 Cd1 C1 96.1(4) . . ? N3 Cd1 C21 124.6(3) . . ? O1 Cd1 C21 134.6(3) . . ? N1 Cd1 C21 94.9(3) . . ? O3 Cd1 C21 28.2(2) . . ? O2 Cd1 C21 95.5(3) . . ? O4 Cd1 C21 27.8(3) . . ? C1 Cd1 C21 115.4(4) . . ? O2 C1 O1 122.9(8) . . ? O2 C1 C2 121.7(8) . . ? O1 C1 C2 115.4(8) . . ? O2 C1 Cd1 65.0(4) . . ? O1 C1 Cd1 58.2(4) . . ? C2 C1 Cd1 171.2(7) . . ? C3 C2 C7 120.0(8) . . ? C3 C2 C1 120.9(8) . . ? C7 C2 C1 119.0(8) . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C5 120.1(8) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C6 C5 C4 119.5(9) . . ? C6 C5 N2 122.8(9) . 4_655 ? C4 C5 N2 117.6(9) . 4_655 ? C7 C6 C5 119.6(9) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C2 120.5(8) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 N2 112.2(10) . . ? N1 C9 C8 124.7(10) . . ? N2 C9 C8 123.0(8) . . ? C11 C10 N2 108.9(8) . . ? C11 C10 H10A 125.6 . . ? N2 C10 H10A 125.6 . . ? C10 C11 N1 106.6(8) . . ? C10 C11 H11A 126.7 . . ? N1 C11 H11A 126.7 . . ? O4 C21 O3 124.4(9) . . ? O4 C21 C22 114.4(9) . . ? O3 C21 C22 121.2(8) . . ? O4 C21 Cd1 65.3(5) . . ? O3 C21 Cd1 59.1(4) . . ? C22 C21 Cd1 179.0(7) . . ? C23 C22 C27 119.7(9) . . ? C23 C22 C21 123.2(9) . . ? C27 C22 C21 117.1(8) . . ? C22 C23 C24 119.9(11) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 123.1(11) . . ? C23 C24 H24A 118.5 . . ? C25 C24 H24A 118.5 . . ? C26 C25 C24 119.3(11) . . ? C26 C25 N4 117.0(9) . 8_744 ? C24 C25 N4 123.5(11) . 8_744 ? C25 C26 C27 118.5(9) . . ? C25 C26 H26A 120.7 . . ? C27 C26 H26A 120.7 . . ? C22 C27 C26 119.2(8) . . ? C22 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 N4 112.0(9) . . ? N3 C29 C28 121.8(10) . . ? N4 C29 C28 126.1(10) . . ? C31 C30 N3 110.4(9) . . ? C31 C30 H30A 124.8 . . ? N3 C30 H30A 124.8 . . ? N4 C31 C30 106.7(9) . . ? N4 C31 H31A 126.7 . . ? C30 C31 H31A 126.7 . . ? C9 N1 C11 107.1(8) . . ? C9 N1 Cd1 127.7(7) . . ? C11 N1 Cd1 124.2(6) . . ? C9 N2 C10 105.2(8) . . ? C9 N2 C5 128.8(9) . 4_645 ? C10 N2 C5 125.9(8) . 4_645 ? C29 N3 C30 102.9(9) . . ? C29 N3 Cd1 131.4(8) . . ? C30 N3 Cd1 123.4(7) . . ? C31 N4 C29 107.6(8) . . ? C31 N4 C25 126.6(8) . 8_745 ? C29 N4 C25 125.7(9) . 8_745 ? C1 O1 Cd1 93.7(5) . . ? C1 O2 Cd1 87.7(5) . . ? C21 O3 Cd1 92.8(5) . . ? C21 O4 Cd1 86.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cd1 C1 O2 88.7(10) . . . . ? O1 Cd1 C1 O2 173.8(15) . . . . ? N1 Cd1 C1 O2 -157.7(8) . . . . ? O3 Cd1 C1 O2 -17.9(12) . . . . ? O4 Cd1 C1 O2 -67.5(10) . . . . ? C21 Cd1 C1 O2 -46.5(10) . . . . ? N3 Cd1 C1 O1 -85.1(8) . . . . ? N1 Cd1 C1 O1 28.5(9) . . . . ? O3 Cd1 C1 O1 168.3(6) . . . . ? O2 Cd1 C1 O1 -173.8(15) . . . . ? O4 Cd1 C1 O1 118.7(8) . . . . ? C21 Cd1 C1 O1 139.6(7) . . . . ? N3 Cd1 C1 C2 -131(7) . . . . ? O1 Cd1 C1 C2 -45(6) . . . . ? N1 Cd1 C1 C2 -17(7) . . . . ? O3 Cd1 C1 C2 123(6) . . . . ? O2 Cd1 C1 C2 141(7) . . . . ? O4 Cd1 C1 C2 73(7) . . . . ? C21 Cd1 C1 C2 94(7) . . . . ? O2 C1 C2 C3 169.4(13) . . . . ? O1 C1 C2 C3 -10(2) . . . . ? Cd1 C1 C2 C3 32(7) . . . . ? O2 C1 C2 C7 -6(2) . . . . ? O1 C1 C2 C7 174.0(11) . . . . ? Cd1 C1 C2 C7 -144(6) . . . . ? C7 C2 C3 C4 -2.9(17) . . . . ? C1 C2 C3 C4 -178.5(11) . . . . ? C2 C3 C4 C5 1.8(16) . . . . ? C3 C4 C5 C6 -0.2(15) . . . . ? C3 C4 C5 N2 179.0(8) . . . 4_655 ? C4 C5 C6 C7 -0.2(15) . . . . ? N2 C5 C6 C7 -179.4(8) 4_655 . . . ? C5 C6 C7 C2 -0.9(16) . . . . ? C3 C2 C7 C6 2.5(18) . . . . ? C1 C2 C7 C6 178.1(11) . . . . ? N2 C10 C11 N1 -1.6(10) . . . . ? N3 Cd1 C21 O4 -172.0(5) . . . . ? O1 Cd1 C21 O4 -24.3(8) . . . . ? N1 Cd1 C21 O4 74.7(6) . . . . ? O3 Cd1 C21 O4 -179.0(10) . . . . ? O2 Cd1 C21 O4 -69.1(6) . . . . ? C1 Cd1 C21 O4 -49.6(7) . . . . ? N3 Cd1 C21 O3 7.0(7) . . . . ? O1 Cd1 C21 O3 154.7(5) . . . . ? N1 Cd1 C21 O3 -106.3(6) . . . . ? O2 Cd1 C21 O3 109.9(6) . . . . ? O4 Cd1 C21 O3 179.0(10) . . . . ? C1 Cd1 C21 O3 129.4(6) . . . . ? N3 Cd1 C21 C22 116(50) . . . . ? O1 Cd1 C21 C22 -96(50) . . . . ? N1 Cd1 C21 C22 3(50) . . . . ? O3 Cd1 C21 C22 109(50) . . . . ? O2 Cd1 C21 C22 -141(50) . . . . ? O4 Cd1 C21 C22 -72(50) . . . . ? C1 Cd1 C21 C22 -122(50) . . . . ? O4 C21 C22 C23 4.8(15) . . . . ? O3 C21 C22 C23 -175.2(10) . . . . ? Cd1 C21 C22 C23 76(50) . . . . ? O4 C21 C22 C27 -172.8(9) . . . . ? O3 C21 C22 C27 7.2(14) . . . . ? Cd1 C21 C22 C27 -101(50) . . . . ? C27 C22 C23 C24 -5.6(16) . . . . ? C21 C22 C23 C24 176.9(10) . . . . ? C22 C23 C24 C25 5.8(18) . . . . ? C23 C24 C25 C26 -3.6(17) . . . . ? C23 C24 C25 N4 -178.2(11) . . . 8_744 ? C24 C25 C26 C27 1.3(14) . . . . ? N4 C25 C26 C27 176.2(8) 8_744 . . . ? C23 C22 C27 C26 3.4(14) . . . . ? C21 C22 C27 C26 -179.0(8) . . . . ? C25 C26 C27 C22 -1.2(14) . . . . ? N3 C30 C31 N4 3.6(13) . . . . ? N2 C9 N1 C11 -0.6(10) . . . . ? C8 C9 N1 C11 175.0(8) . . . . ? N2 C9 N1 Cd1 168.4(5) . . . . ? C8 C9 N1 Cd1 -16.0(13) . . . . ? C10 C11 N1 C9 1.4(10) . . . . ? C10 C11 N1 Cd1 -168.1(6) . . . . ? N3 Cd1 N1 C9 60.2(8) . . . . ? O1 Cd1 N1 C9 -36.5(8) . . . . ? O3 Cd1 N1 C9 160.7(8) . . . . ? O2 Cd1 N1 C9 -66.1(10) . . . . ? O4 Cd1 N1 C9 -144.9(8) . . . . ? C1 Cd1 N1 C9 -49.5(9) . . . . ? C21 Cd1 N1 C9 -171.7(8) . . . . ? N3 Cd1 N1 C11 -132.5(6) . . . . ? O1 Cd1 N1 C11 130.8(6) . . . . ? O3 Cd1 N1 C11 -32.0(6) . . . . ? O2 Cd1 N1 C11 101.2(8) . . . . ? O4 Cd1 N1 C11 22.4(6) . . . . ? C1 Cd1 N1 C11 117.8(7) . . . . ? C21 Cd1 N1 C11 -4.4(7) . . . . ? N1 C9 N2 C10 -0.3(10) . . . . ? C8 C9 N2 C10 -176.0(8) . . . . ? N1 C9 N2 C5 177.0(8) . . . 4_645 ? C8 C9 N2 C5 1.3(15) . . . 4_645 ? C11 C10 N2 C9 1.2(10) . . . . ? C11 C10 N2 C5 -176.2(8) . . . 4_645 ? N4 C29 N3 C30 -3.6(11) . . . . ? C28 C29 N3 C30 174.0(9) . . . . ? N4 C29 N3 Cd1 158.8(7) . . . . ? C28 C29 N3 Cd1 -23.6(15) . . . . ? C31 C30 N3 C29 -0.1(12) . . . . ? C31 C30 N3 Cd1 -164.3(7) . . . . ? O1 Cd1 N3 C29 -178.7(9) . . . . ? N1 Cd1 N3 C29 86.5(9) . . . . ? O3 Cd1 N3 C29 -17.9(9) . . . . ? O2 Cd1 N3 C29 -123.2(9) . . . . ? O4 Cd1 N3 C29 -29.1(12) . . . . ? C1 Cd1 N3 C29 -150.7(9) . . . . ? C21 Cd1 N3 C29 -21.2(10) . . . . ? O1 Cd1 N3 C30 -19.4(8) . . . . ? N1 Cd1 N3 C30 -114.1(8) . . . . ? O3 Cd1 N3 C30 141.5(8) . . . . ? O2 Cd1 N3 C30 36.2(8) . . . . ? O4 Cd1 N3 C30 130.3(8) . . . . ? C1 Cd1 N3 C30 8.7(8) . . . . ? C21 Cd1 N3 C30 138.2(8) . . . . ? C30 C31 N4 C29 -5.7(13) . . . . ? C30 C31 N4 C25 170.7(10) . . . 8_745 ? N3 C29 N4 C31 6.0(13) . . . . ? C28 C29 N4 C31 -171.5(10) . . . . ? N3 C29 N4 C25 -170.4(9) . . . 8_745 ? C28 C29 N4 C25 12.1(17) . . . 8_745 ? O2 C1 O1 Cd1 -6.7(16) . . . . ? C2 C1 O1 Cd1 173.0(11) . . . . ? N3 Cd1 O1 C1 98.6(8) . . . . ? N1 Cd1 O1 C1 -155.0(8) . . . . ? O3 Cd1 O1 C1 -23.6(11) . . . . ? O2 Cd1 O1 C1 3.4(8) . . . . ? O4 Cd1 O1 C1 -66.9(8) . . . . ? C21 Cd1 O1 C1 -55.2(9) . . . . ? O1 C1 O2 Cd1 6.3(15) . . . . ? C2 C1 O2 Cd1 -173.4(13) . . . . ? N3 Cd1 O2 C1 -95.3(10) . . . . ? O1 Cd1 O2 C1 -3.5(9) . . . . ? N1 Cd1 O2 C1 33.4(12) . . . . ? O3 Cd1 O2 C1 166.0(9) . . . . ? O4 Cd1 O2 C1 112.8(10) . . . . ? C21 Cd1 O2 C1 138.8(10) . . . . ? O4 C21 O3 Cd1 1.1(11) . . . . ? C22 C21 O3 Cd1 -178.9(8) . . . . ? N3 Cd1 O3 C21 -174.2(6) . . . . ? O1 Cd1 O3 C21 -52.2(9) . . . . ? N1 Cd1 O3 C21 77.8(6) . . . . ? O2 Cd1 O3 C21 -74.9(6) . . . . ? O4 Cd1 O3 C21 -0.6(6) . . . . ? C1 Cd1 O3 C21 -66.5(7) . . . . ? O3 C21 O4 Cd1 -1.0(10) . . . . ? C22 C21 O4 Cd1 179.0(7) . . . . ? N3 Cd1 O4 C21 14.0(9) . . . . ? O1 Cd1 O4 C21 162.0(6) . . . . ? N1 Cd1 O4 C21 -105.8(6) . . . . ? O3 Cd1 O4 C21 0.6(6) . . . . ? O2 Cd1 O4 C21 111.1(6) . . . . ? C1 Cd1 O4 C21 136.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.24 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.509 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.071