# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[Cd(1,3-BDC)(bimb)] _database_code_depnum_ccdc_archive 'CCDC 874180' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd N4 O4' _chemical_formula_sum 'C26 H18 Cd N4 O4' _chemical_formula_weight 562.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.762(2) _cell_length_b 13.486(3) _cell_length_c 16.804(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.04(3) _cell_angle_gamma 90.00 _cell_volume 2178.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7143 _cell_measurement_theta_min 3.0222 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 0.9026 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23311 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4973 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0397P)^2^+4.7444P] 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_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4973 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1099(6) 0.3590(4) 0.9510(3) 0.0449(14) Uani 1 1 d . . . H1A H 0.0860 0.3655 1.0020 0.054 Uiso 1 1 calc R . . C2 C 0.0189(6) 0.3610(4) 0.8807(3) 0.0444(14) Uani 1 1 d . . . H2A H -0.0771 0.3688 0.8743 0.053 Uiso 1 1 calc R . . C3 C 0.2303(5) 0.3418(4) 0.8574(3) 0.0368(12) Uani 1 1 d . . . H3A H 0.3053 0.3346 0.8305 0.044 Uiso 1 1 calc R . . C4 C 0.0508(5) 0.3475(4) 0.7342(3) 0.0335(11) Uani 1 1 d . . . C5 C -0.0876(5) 0.3608(4) 0.7013(3) 0.0357(12) Uani 1 1 d . . . H5A H -0.1536 0.3684 0.7346 0.043 Uiso 1 1 calc R . . C6 C -0.1273(5) 0.3625(4) 0.6177(3) 0.0365(12) Uani 1 1 d . . . H6A H -0.2209 0.3700 0.5957 0.044 Uiso 1 1 calc R . . C7 C -0.0316(5) 0.3533(4) 0.5666(3) 0.0343(11) Uani 1 1 d . . . C8 C 0.1051(6) 0.3368(5) 0.6012(3) 0.0531(17) Uani 1 1 d . . . H8A H 0.1711 0.3282 0.5680 0.064 Uiso 1 1 calc R . . C9 C 0.1464(6) 0.3329(5) 0.6844(3) 0.0532(17) Uani 1 1 d . . . H9A H 0.2389 0.3203 0.7064 0.064 Uiso 1 1 calc R . . C10 C -0.0734(5) 0.3595(4) 0.4772(3) 0.0343(12) Uani 1 1 d . . . C11 C -0.2081(6) 0.3342(5) 0.4390(3) 0.0464(15) Uani 1 1 d . . . H11A H -0.2730 0.3135 0.4700 0.056 Uiso 1 1 calc R . . C12 C -0.2458(6) 0.3396(5) 0.3559(3) 0.0511(16) Uani 1 1 d . . . H12A H -0.3356 0.3222 0.3317 0.061 Uiso 1 1 calc R . . C13 C -0.1526(5) 0.3704(4) 0.3088(3) 0.0332(12) Uani 1 1 d . . . C14 C -0.0186(5) 0.3952(4) 0.3449(3) 0.0406(13) Uani 1 1 d . . . H14A H 0.0458 0.4157 0.3135 0.049 Uiso 1 1 calc R . . C15 C 0.0188(5) 0.3894(4) 0.4282(3) 0.0391(13) Uani 1 1 d . . . H15A H 0.1091 0.4063 0.4519 0.047 Uiso 1 1 calc R . . C16 C -0.1138(6) 0.4007(5) 0.1656(3) 0.0448(14) Uani 1 1 d . . . H16A H -0.0190 0.4147 0.1748 0.054 Uiso 1 1 calc R . . C17 C -0.1994(6) 0.3991(5) 0.0936(3) 0.0459(14) Uani 1 1 d . . . H17A H -0.1729 0.4129 0.0442 0.055 Uiso 1 1 calc R . . C18 C -0.3234(5) 0.3625(4) 0.1817(3) 0.0377(13) Uani 1 1 d . . . H18A H -0.3990 0.3458 0.2058 0.045 Uiso 1 1 calc R . . C19 C 0.4784(5) 0.1716(4) 1.0967(3) 0.0316(11) Uani 1 1 d . . . C20 C 0.5867(5) 0.0542(4) 1.3824(3) 0.0367(12) Uani 1 1 d . . . C21 C 0.5267(5) 0.0895(4) 1.1546(3) 0.0314(11) Uani 1 1 d . . . C22 C 0.5358(5) 0.1063(4) 1.2369(3) 0.0293(11) Uani 1 1 d . . . H22A H 0.5052 0.1666 1.2541 0.035 Uiso 1 1 calc R . . C23 C 0.5887(5) 0.0367(4) 1.2937(3) 0.0317(11) Uani 1 1 d . . . C24 C 0.6355(6) -0.0536(4) 1.2677(3) 0.0405(13) Uani 1 1 d . . . H24A H 0.6735 -0.1010 1.3054 0.049 Uiso 1 1 calc R . . C25 C 0.6255(6) -0.0723(4) 1.1863(3) 0.0466(14) Uani 1 1 d . . . H25A H 0.6549 -0.1330 1.1691 0.056 Uiso 1 1 calc R . . C26 C 0.5718(6) -0.0010(4) 1.1297(3) 0.0392(13) Uani 1 1 d . . . H26A H 0.5660 -0.0140 1.0749 0.047 Uiso 1 1 calc R . . N1 N 0.2415(5) 0.3462(3) 0.9366(2) 0.0387(10) Uani 1 1 d . . . N2 N 0.0967(4) 0.3489(3) 0.8202(2) 0.0335(9) Uani 1 1 d . . . N3 N -0.3309(5) 0.3743(3) 0.1036(2) 0.0387(11) Uani 1 1 d . . . N4 N -0.1936(4) 0.3776(3) 0.2230(2) 0.0335(10) Uani 1 1 d . . . O1 O 0.4203(3) 0.2460(3) 1.12263(19) 0.0346(8) Uani 1 1 d . . . O2 O 0.5035(4) 0.1674(3) 1.0261(2) 0.0458(10) Uani 1 1 d . . . O3 O 0.5411(4) 0.1375(3) 1.4002(2) 0.0428(9) Uani 1 1 d . . . O4 O 0.6290(4) -0.0123(3) 1.4324(2) 0.0504(10) Uani 1 1 d . . . Cd1 Cd 0.45987(4) 0.34864(3) 1.01673(2) 0.03198(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.051(4) 0.062(4) 0.021(2) -0.001(3) 0.007(2) -0.002(3) C2 0.038(3) 0.066(4) 0.028(3) 0.003(3) 0.002(2) -0.007(3) C3 0.037(3) 0.047(3) 0.023(2) -0.003(2) -0.005(2) 0.005(3) C4 0.037(3) 0.039(3) 0.022(2) -0.001(2) -0.005(2) 0.003(2) C5 0.034(3) 0.046(3) 0.027(3) 0.000(2) 0.004(2) 0.001(2) C6 0.027(3) 0.050(3) 0.028(3) 0.000(2) -0.005(2) -0.001(2) C7 0.037(3) 0.042(3) 0.021(2) -0.002(2) -0.001(2) 0.006(2) C8 0.033(3) 0.093(5) 0.030(3) -0.006(3) -0.004(2) 0.015(3) C9 0.027(3) 0.102(5) 0.029(3) -0.003(3) -0.002(2) 0.012(3) C10 0.033(3) 0.043(3) 0.023(2) 0.000(2) -0.005(2) 0.002(2) C11 0.033(3) 0.080(5) 0.025(3) -0.002(3) 0.000(2) -0.005(3) C12 0.030(3) 0.091(5) 0.028(3) 0.002(3) -0.007(2) -0.004(3) C13 0.035(3) 0.039(3) 0.022(2) 0.000(2) -0.004(2) 0.003(2) C14 0.035(3) 0.054(4) 0.029(3) 0.002(3) -0.004(2) -0.011(3) C15 0.028(3) 0.051(3) 0.034(3) -0.003(3) -0.006(2) -0.005(2) C16 0.033(3) 0.065(4) 0.034(3) 0.005(3) 0.002(2) -0.008(3) C17 0.048(4) 0.066(4) 0.024(3) 0.003(3) 0.006(2) -0.014(3) C18 0.036(3) 0.054(4) 0.021(2) 0.000(2) 0.000(2) -0.004(3) C19 0.030(3) 0.041(3) 0.024(2) 0.002(2) 0.003(2) -0.002(2) C20 0.033(3) 0.047(3) 0.030(3) 0.002(3) 0.003(2) -0.008(2) C21 0.036(3) 0.035(3) 0.022(2) 0.001(2) 0.004(2) -0.003(2) C22 0.033(3) 0.032(3) 0.024(2) 0.001(2) 0.006(2) -0.004(2) C23 0.034(3) 0.041(3) 0.020(2) 0.001(2) 0.005(2) -0.005(2) C24 0.050(3) 0.037(3) 0.035(3) 0.007(2) 0.008(2) 0.006(3) C25 0.064(4) 0.036(3) 0.042(3) -0.002(3) 0.014(3) 0.006(3) C26 0.053(3) 0.039(3) 0.026(3) -0.005(2) 0.008(2) -0.004(3) N1 0.048(3) 0.041(3) 0.024(2) -0.004(2) -0.0031(19) -0.001(2) N2 0.035(2) 0.043(2) 0.020(2) -0.0049(19) -0.0008(16) -0.003(2) N3 0.041(3) 0.050(3) 0.024(2) 0.0021(19) 0.0012(18) -0.006(2) N4 0.031(2) 0.045(3) 0.021(2) 0.0027(18) -0.0049(17) -0.0030(19) O1 0.037(2) 0.039(2) 0.0269(18) 0.0068(16) 0.0040(14) 0.0043(16) O2 0.066(3) 0.051(2) 0.0222(18) 0.0072(17) 0.0116(17) 0.0051(19) O3 0.053(2) 0.056(3) 0.0186(17) 0.0003(17) 0.0056(16) 0.0061(19) O4 0.069(3) 0.048(2) 0.029(2) 0.0139(18) -0.0063(18) -0.013(2) Cd1 0.0404(2) 0.0357(2) 0.01740(19) 0.00097(16) -0.00172(14) -0.00018(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 C1 C2 1.349(7) . ? C1 N1 1.360(7) . ? C1 H1A 0.9300 . ? C2 N2 1.381(7) . ? C2 H2A 0.9300 . ? C3 N1 1.318(6) . ? C3 N2 1.348(6) . ? C3 H3A 0.9300 . ? C4 C9 1.372(7) . ? C4 C5 1.379(7) . ? C4 N2 1.437(6) . ? C5 C6 1.390(7) . ? C5 H5A 0.9300 . ? C6 C7 1.381(7) . ? C6 H6A 0.9300 . ? C7 C8 1.377(7) . ? C7 C10 1.488(7) . ? C8 C9 1.387(7) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.382(7) . ? C10 C11 1.400(7) . ? C11 C12 1.383(7) . ? C11 H11A 0.9300 . ? C12 C13 1.370(8) . ? C12 H12A 0.9300 . ? C13 C14 1.383(7) . ? C13 N4 1.430(6) . ? C14 C15 1.386(7) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.346(7) . ? C16 N4 1.378(7) . ? C16 H16A 0.9300 . ? C17 N3 1.365(7) . ? C17 H17A 0.9300 . ? C18 N3 1.310(6) . ? C18 N4 1.350(6) . ? C18 H18A 0.9300 . ? C19 O2 1.254(6) . ? C19 O1 1.266(6) . ? C19 C21 1.495(7) . ? C19 Cd1 2.730(5) . ? C20 O4 1.249(6) . ? C20 O3 1.263(6) . ? C20 C23 1.514(7) . ? C21 C26 1.387(7) . ? C21 C22 1.388(6) . ? C22 C23 1.374(7) . ? C22 H22A 0.9300 . ? C23 C24 1.396(7) . ? C24 C25 1.378(7) . ? C24 H24A 0.9300 . ? C25 C26 1.389(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? N1 Cd1 2.314(4) . ? N3 Cd1 2.320(4) 1_454 ? O1 Cd1 2.339(3) . ? O2 Cd1 2.482(4) . ? O3 Cd1 2.245(3) 4_566 ? O4 Cd1 2.293(4) 2_647 ? Cd1 O3 2.245(3) 4_565 ? Cd1 O4 2.293(4) 2_657 ? Cd1 N3 2.320(4) 1_656 ? 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 C2 C1 N1 110.2(5) . . ? C2 C1 H1A 124.9 . . ? N1 C1 H1A 124.9 . . ? C1 C2 N2 106.3(5) . . ? C1 C2 H2A 126.9 . . ? N2 C2 H2A 126.9 . . ? N1 C3 N2 111.7(5) . . ? N1 C3 H3A 124.2 . . ? N2 C3 H3A 124.2 . . ? C9 C4 C5 119.8(5) . . ? C9 C4 N2 119.3(4) . . ? C5 C4 N2 120.9(4) . . ? C4 C5 C6 119.2(5) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C7 C6 C5 121.8(5) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C8 C7 C6 117.5(5) . . ? C8 C7 C10 120.7(5) . . ? C6 C7 C10 121.8(4) . . ? C7 C8 C9 121.5(5) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C4 C9 C8 120.0(5) . . ? C4 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C15 C10 C11 117.1(5) . . ? C15 C10 C7 121.7(5) . . ? C11 C10 C7 121.3(5) . . ? C12 C11 C10 120.9(5) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C13 C12 C11 120.8(5) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 119.5(5) . . ? C12 C13 N4 120.4(4) . . ? C14 C13 N4 120.1(5) . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C10 C15 C14 122.3(5) . . ? C10 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C17 C16 N4 106.7(5) . . ? C17 C16 H16A 126.6 . . ? N4 C16 H16A 126.6 . . ? C16 C17 N3 110.0(5) . . ? C16 C17 H17A 125.0 . . ? N3 C17 H17A 125.0 . . ? N3 C18 N4 112.4(5) . . ? N3 C18 H18A 123.8 . . ? N4 C18 H18A 123.8 . . ? O2 C19 O1 122.3(5) . . ? O2 C19 C21 119.4(5) . . ? O1 C19 C21 118.2(4) . . ? O2 C19 Cd1 65.2(3) . . ? O1 C19 Cd1 58.8(2) . . ? C21 C19 Cd1 162.7(3) . . ? O4 C20 O3 124.6(5) . . ? O4 C20 C23 119.4(5) . . ? O3 C20 C23 116.0(5) . . ? C26 C21 C22 118.4(5) . . ? C26 C21 C19 122.4(4) . . ? C22 C21 C19 119.0(5) . . ? C23 C22 C21 122.1(5) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C22 C23 C24 118.9(4) . . ? C22 C23 C20 120.6(5) . . ? C24 C23 C20 120.3(5) . . ? C25 C24 C23 119.9(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.4(5) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C21 C26 C25 120.3(5) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C3 N1 C1 105.7(4) . . ? C3 N1 Cd1 119.6(4) . . ? C1 N1 Cd1 134.3(3) . . ? C3 N2 C2 106.2(4) . . ? C3 N2 C4 125.0(4) . . ? C2 N2 C4 128.9(4) . . ? C18 N3 C17 105.3(4) . . ? C18 N3 Cd1 120.1(4) . 1_454 ? C17 N3 Cd1 134.6(3) . 1_454 ? C18 N4 C16 105.5(4) . . ? C18 N4 C13 125.6(4) . . ? C16 N4 C13 128.9(4) . . ? C19 O1 Cd1 93.7(3) . . ? C19 O2 Cd1 87.4(3) . . ? C20 O3 Cd1 118.2(3) . 4_566 ? C20 O4 Cd1 137.4(4) . 2_647 ? O3 Cd1 O4 118.09(14) 4_565 2_657 ? O3 Cd1 N1 85.62(15) 4_565 . ? O4 Cd1 N1 81.84(15) 2_657 . ? O3 Cd1 N3 97.49(15) 4_565 1_656 ? O4 Cd1 N3 89.57(15) 2_657 1_656 ? N1 Cd1 N3 171.33(16) . 1_656 ? O3 Cd1 O1 147.48(13) 4_565 . ? O4 Cd1 O1 94.42(13) 2_657 . ? N1 Cd1 O1 100.17(14) . . ? N3 Cd1 O1 81.58(14) 1_656 . ? O3 Cd1 O2 93.14(13) 4_565 . ? O4 Cd1 O2 148.63(13) 2_657 . ? N1 Cd1 O2 98.83(15) . . ? N3 Cd1 O2 89.11(15) 1_656 . ? O1 Cd1 O2 54.42(12) . . ? O3 Cd1 C19 119.95(15) 4_565 . ? O4 Cd1 C19 121.91(15) 2_657 . ? N1 Cd1 C19 104.44(15) . . ? N3 Cd1 C19 81.08(15) 1_656 . ? O1 Cd1 C19 27.57(13) . . ? O2 Cd1 C19 27.32(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.064 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.110 data_[Cd(5-Me-1,3-BDC)(bimb)]n _database_code_depnum_ccdc_archive 'CCDC 874181' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H20 Cd N4 O4' _chemical_formula_sum 'C27 H20 Cd N4 O4' _chemical_formula_weight 576.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.857(2) _cell_length_b 14.011(3) _cell_length_c 16.884(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.93(3) _cell_angle_gamma 90.00 _cell_volume 2289.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10477 _cell_measurement_theta_min 2.9994 _cell_measurement_theta_max 27.5243 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7814 _exptl_absorpt_correction_T_max 0.8408 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ?0 _diffrn_reflns_number 20898 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5192 _reflns_number_gt 4442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0073P)^2^+11.6809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5192 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.3972(7) 0.1402(5) 0.0446(3) 0.0441(17) Uani 1 1 d . . . H1A H 0.4208 0.1384 -0.0062 0.053 Uiso 1 1 calc R . . C2 C 0.4890(7) 0.1425(6) 0.1152(3) 0.0469(18) Uani 1 1 d . . . H2A H 0.5848 0.1428 0.1220 0.056 Uiso 1 1 calc R . . C3 C 0.2780(6) 0.1420(4) 0.1373(3) 0.0260(11) Uani 1 1 d . . . H3A H 0.2040 0.1412 0.1642 0.031 Uiso 1 1 calc R . . C4 C 0.4593(5) 0.1472(4) 0.2602(3) 0.0247(11) Uani 1 1 d . . . C5 C 0.5974(5) 0.1373(4) 0.2937(3) 0.0261(11) Uani 1 1 d . . . H5A H 0.6623 0.1293 0.2608 0.031 Uiso 1 1 calc R . . C6 C 0.6389(6) 0.1394(4) 0.3774(3) 0.0278(12) Uani 1 1 d . . . H6A H 0.7323 0.1348 0.4001 0.033 Uiso 1 1 calc R . . C7 C 0.5433(5) 0.1482(4) 0.4272(3) 0.0247(11) Uani 1 1 d . . . C8 C 0.4060(6) 0.1613(5) 0.3920(3) 0.0420(17) Uani 1 1 d . . . H8A H 0.3409 0.1698 0.4247 0.050 Uiso 1 1 calc R . . C9 C 0.3639(6) 0.1622(5) 0.3094(3) 0.0380(15) Uani 1 1 d . . . H9A H 0.2715 0.1728 0.2867 0.046 Uiso 1 1 calc R . . C10 C 0.5863(6) 0.1429(4) 0.5166(3) 0.0267(11) Uani 1 1 d . . . C11 C 0.7137(6) 0.1773(4) 0.5560(3) 0.0286(12) Uani 1 1 d . . . H11A H 0.7743 0.2041 0.5262 0.034 Uiso 1 1 calc R . . C12 C 0.7508(6) 0.1719(4) 0.6389(3) 0.0320(13) Uani 1 1 d . . . H12A H 0.8357 0.1960 0.6647 0.038 Uiso 1 1 calc R . . C13 C 0.6630(5) 0.1312(4) 0.6837(3) 0.0234(11) Uani 1 1 d . . . C14 C 0.5360(6) 0.0960(4) 0.6454(3) 0.0334(14) Uani 1 1 d . . . H14A H 0.4764 0.0680 0.6752 0.040 Uiso 1 1 calc R . . C15 C 0.4993(6) 0.1033(4) 0.5626(3) 0.0326(14) Uani 1 1 d . . . H15A H 0.4133 0.0808 0.5371 0.039 Uiso 1 1 calc R . . C16 C 0.6216(6) 0.1037(4) 0.8246(3) 0.0316(13) Uani 1 1 d . . . H16A H 0.5266 0.0938 0.8144 0.038 Uiso 1 1 calc R . . C17 C 0.7078(6) 0.1017(4) 0.8973(3) 0.0294(13) Uani 1 1 d . . . H17A H 0.6805 0.0897 0.9461 0.035 Uiso 1 1 calc R . . C18 C 0.8341(6) 0.1321(4) 0.8110(3) 0.0285(12) Uani 1 1 d . . . H18A H 0.9102 0.1451 0.7877 0.034 Uiso 1 1 calc R . . C19 C 0.0352(6) 0.3099(4) -0.1050(3) 0.0240(11) Uani 1 1 d . . . C20 C -0.0135(5) 0.3908(3) -0.1618(3) 0.0191(10) Uani 1 1 d . . . C21 C -0.0563(5) 0.4762(3) -0.1347(3) 0.0214(11) Uani 1 1 d . . . H21A H -0.0469 0.4860 -0.0795 0.026 Uiso 1 1 calc R . . C22 C -0.1133(6) 0.5485(4) -0.1874(3) 0.0242(11) Uani 1 1 d . . . C23 C -0.1249(5) 0.5324(4) -0.2696(3) 0.0235(11) Uani 1 1 d . . . H23A H -0.1640 0.5792 -0.3058 0.028 Uiso 1 1 calc R . . C24 C -0.0794(5) 0.4482(3) -0.2988(3) 0.0189(10) Uani 1 1 d . . . C25 C -0.0227(5) 0.3772(3) -0.2444(3) 0.0192(10) Uani 1 1 d . . . H25A H 0.0089 0.3207 -0.2634 0.023 Uiso 1 1 calc R . . C26 C -0.0802(5) 0.4347(4) -0.3871(3) 0.0216(11) Uani 1 1 d . . . C27 C -0.1600(6) 0.6413(4) -0.1576(3) 0.0340(13) Uani 1 1 d . . . H27A H -0.1957 0.6816 -0.2028 0.051 Uiso 1 1 calc R . . H27B H -0.0832 0.6723 -0.1239 0.051 Uiso 1 1 calc R . . H27C H -0.2311 0.6295 -0.1270 0.051 Uiso 1 1 calc R . . N1 N 0.2650(5) 0.1411(3) 0.0582(2) 0.0274(10) Uani 1 1 d . . . N2 N 0.4118(4) 0.1442(3) 0.1746(2) 0.0237(9) Uani 1 1 d . . . N3 N 0.8406(5) 0.1200(3) 0.8889(2) 0.0274(10) Uani 1 1 d . . . N4 N 0.7036(4) 0.1234(3) 0.7690(2) 0.0225(9) Uani 1 1 d . . . O1 O 0.0047(4) 0.3125(3) -0.0362(2) 0.0326(9) Uani 1 1 d . . . O2 O 0.0952(4) 0.2400(2) -0.1303(2) 0.0241(8) Uani 1 1 d . . . O3 O -0.0323(4) 0.3564(3) -0.40764(19) 0.0298(9) Uani 1 1 d . . . O4 O -0.1240(4) 0.5006(3) -0.4347(2) 0.0325(9) Uani 1 1 d . . . Cd1 Cd 0.04865(4) 0.14284(3) -0.02292(2) 0.02133(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(4) 0.066(4) 0.016(2) 0.005(3) 0.003(3) -0.019(4) C2 0.031(4) 0.088(5) 0.022(3) 0.004(3) 0.003(2) -0.021(4) C3 0.028(3) 0.028(3) 0.019(2) -0.008(2) -0.004(2) 0.004(2) C4 0.026(3) 0.032(3) 0.014(2) -0.001(2) -0.001(2) 0.001(2) C5 0.024(3) 0.035(3) 0.019(2) 0.004(2) 0.001(2) 0.006(2) C6 0.021(3) 0.039(3) 0.019(2) -0.005(2) -0.006(2) -0.001(3) C7 0.023(3) 0.034(3) 0.015(2) 0.001(2) -0.002(2) 0.000(2) C8 0.024(3) 0.080(5) 0.021(3) -0.001(3) 0.003(2) 0.003(3) C9 0.016(3) 0.075(5) 0.021(3) 0.000(3) -0.003(2) 0.005(3) C10 0.027(3) 0.037(3) 0.014(2) 0.000(2) -0.002(2) -0.001(3) C11 0.021(3) 0.046(3) 0.018(2) -0.001(2) 0.002(2) -0.004(2) C12 0.025(3) 0.048(4) 0.019(2) -0.002(2) -0.004(2) -0.010(3) C13 0.022(3) 0.035(3) 0.011(2) -0.001(2) -0.0037(19) 0.001(2) C14 0.031(3) 0.049(4) 0.019(3) -0.003(2) 0.002(2) -0.011(3) C15 0.025(3) 0.054(4) 0.015(2) 0.000(2) -0.006(2) -0.009(3) C16 0.020(3) 0.049(4) 0.024(3) 0.005(3) -0.001(2) -0.005(3) C17 0.034(4) 0.036(3) 0.018(2) 0.003(2) 0.002(2) -0.004(3) C18 0.025(3) 0.043(3) 0.015(2) 0.000(2) -0.002(2) -0.001(3) C19 0.024(3) 0.025(3) 0.021(2) 0.002(2) 0.001(2) -0.004(2) C20 0.019(3) 0.025(3) 0.012(2) 0.0001(19) 0.0008(19) -0.003(2) C21 0.030(3) 0.024(3) 0.010(2) -0.0014(19) 0.001(2) -0.004(2) C22 0.030(3) 0.021(3) 0.022(2) -0.002(2) 0.005(2) -0.003(2) C23 0.026(3) 0.021(3) 0.021(2) 0.002(2) -0.001(2) -0.002(2) C24 0.020(3) 0.023(3) 0.013(2) 0.0002(19) 0.0008(19) -0.004(2) C25 0.022(3) 0.018(2) 0.018(2) 0.0008(19) 0.004(2) -0.003(2) C26 0.023(3) 0.026(3) 0.014(2) 0.001(2) -0.001(2) -0.009(2) C27 0.044(4) 0.030(3) 0.030(3) -0.006(3) 0.011(3) 0.003(3) N1 0.036(3) 0.027(2) 0.0151(19) 0.0015(19) -0.0057(18) 0.001(2) N2 0.027(3) 0.029(2) 0.0132(18) 0.0026(18) -0.0009(17) -0.003(2) N3 0.025(3) 0.041(3) 0.0139(19) 0.0013(19) -0.0021(18) 0.001(2) N4 0.021(2) 0.031(2) 0.0138(19) 0.0025(17) -0.0028(17) -0.0026(18) O1 0.051(3) 0.032(2) 0.0154(17) 0.0059(16) 0.0080(17) 0.0060(19) O2 0.030(2) 0.0219(18) 0.0195(17) 0.0036(15) 0.0014(16) 0.0018(16) O3 0.041(2) 0.035(2) 0.0125(15) -0.0023(16) 0.0040(15) 0.0083(19) O4 0.050(3) 0.028(2) 0.0144(16) 0.0073(15) -0.0062(17) -0.0062(18) Cd1 0.0299(2) 0.02178(19) 0.00984(15) 0.00087(15) -0.00247(13) 0.00103(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 C1 C2 1.354(8) . ? C1 N1 1.365(8) . ? C1 H1A 0.9300 . ? C2 N2 1.369(7) . ? C2 H2A 0.9300 . ? C3 N1 1.317(6) . ? C3 N2 1.350(6) . ? C3 H3A 0.9300 . ? C4 C5 1.379(7) . ? C4 C9 1.383(7) . ? C4 N2 1.433(6) . ? C5 C6 1.396(6) . ? C5 H5A 0.9300 . ? C6 C7 1.382(7) . ? C6 H6A 0.9300 . ? C7 C8 1.383(8) . ? C7 C10 1.491(6) . ? C8 C9 1.378(7) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.378(7) . ? C10 C11 1.391(7) . ? C11 C12 1.380(7) . ? C11 H11A 0.9300 . ? C12 C13 1.377(7) . ? C12 H12A 0.9300 . ? C13 C14 1.386(7) . ? C13 N4 1.424(6) . ? C14 C15 1.380(7) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.354(7) . ? C16 N4 1.378(7) . ? C16 H16A 0.9300 . ? C17 N3 1.368(7) . ? C17 H17A 0.9300 . ? C18 N3 1.314(6) . ? C18 N4 1.351(7) . ? C18 H18A 0.9300 . ? C19 O1 1.255(6) . ? C19 O2 1.260(6) . ? C19 C20 1.503(7) . ? C19 Cd1 2.711(5) . ? C20 C21 1.376(7) . ? C20 C25 1.393(6) . ? C21 C22 1.395(7) . ? C21 H21A 0.9300 . ? C22 C23 1.388(7) . ? C22 C27 1.499(7) . ? C23 C24 1.386(7) . ? C23 H23A 0.9300 . ? C24 C25 1.396(7) . ? C24 C26 1.502(6) . ? C25 H25A 0.9300 . ? C26 O4 1.246(6) . ? C26 O3 1.269(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 Cd1 2.306(4) . ? N3 Cd1 2.317(4) 1_656 ? O1 Cd1 2.419(4) . ? O2 Cd1 2.380(3) . ? O3 Cd1 2.239(3) 4_565 ? O4 Cd1 2.288(4) 2_554 ? Cd1 O3 2.239(3) 4_566 ? Cd1 O4 2.288(4) 2_544 ? Cd1 N3 2.317(4) 1_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 C2 C1 N1 110.5(5) . . ? C2 C1 H1A 124.7 . . ? N1 C1 H1A 124.7 . . ? C1 C2 N2 105.9(5) . . ? C1 C2 H2A 127.0 . . ? N2 C2 H2A 127.0 . . ? N1 C3 N2 111.8(5) . . ? N1 C3 H3A 124.1 . . ? N2 C3 H3A 124.1 . . ? C5 C4 C9 120.0(5) . . ? C5 C4 N2 121.3(4) . . ? C9 C4 N2 118.7(5) . . ? C4 C5 C6 119.3(5) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C7 C6 C5 121.0(5) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 118.4(5) . . ? C6 C7 C10 121.0(5) . . ? C8 C7 C10 120.6(5) . . ? C9 C8 C7 121.2(5) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C4 119.9(5) . . ? C8 C9 H9A 120.1 . . ? C4 C9 H9A 120.1 . . ? C15 C10 C11 118.2(4) . . ? C15 C10 C7 120.2(5) . . ? C11 C10 C7 121.6(5) . . ? C12 C11 C10 120.5(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 119.8(4) . . ? C12 C13 N4 120.1(5) . . ? C14 C13 N4 120.0(5) . . ? C15 C14 C13 119.1(5) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C10 C15 C14 121.9(5) . . ? C10 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C17 C16 N4 105.9(5) . . ? C17 C16 H16A 127.1 . . ? N4 C16 H16A 127.1 . . ? C16 C17 N3 110.5(5) . . ? C16 C17 H17A 124.7 . . ? N3 C17 H17A 124.7 . . ? N3 C18 N4 112.0(5) . . ? N3 C18 H18A 124.0 . . ? N4 C18 H18A 124.0 . . ? O1 C19 O2 123.1(5) . . ? O1 C19 C20 117.7(5) . . ? O2 C19 C20 118.9(4) . . ? O1 C19 Cd1 63.2(3) . . ? O2 C19 Cd1 61.4(3) . . ? C20 C19 Cd1 162.9(4) . . ? C21 C20 C25 119.1(4) . . ? C21 C20 C19 121.6(4) . . ? C25 C20 C19 119.2(4) . . ? C20 C21 C22 122.1(4) . . ? C20 C21 H21A 119.0 . . ? C22 C21 H21A 119.0 . . ? C23 C22 C21 117.8(5) . . ? C23 C22 C27 120.3(5) . . ? C21 C22 C27 121.9(4) . . ? C24 C23 C22 121.5(5) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 C26 121.3(4) . . ? C25 C24 C26 119.3(4) . . ? C20 C25 C24 120.2(5) . . ? C20 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? O4 C26 O3 124.5(4) . . ? O4 C26 C24 118.9(5) . . ? O3 C26 C24 116.6(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C3 N1 C1 105.0(4) . . ? C3 N1 Cd1 120.2(4) . . ? C1 N1 Cd1 134.8(3) . . ? C3 N2 C2 106.7(4) . . ? C3 N2 C4 125.1(4) . . ? C2 N2 C4 128.2(5) . . ? C18 N3 C17 105.2(4) . . ? C18 N3 Cd1 119.6(4) . 1_656 ? C17 N3 Cd1 135.0(3) . 1_656 ? C18 N4 C16 106.4(4) . . ? C18 N4 C13 125.5(4) . . ? C16 N4 C13 128.0(4) . . ? C19 O1 Cd1 89.3(3) . . ? C19 O2 Cd1 90.9(3) . . ? C26 O3 Cd1 116.5(3) . 4_565 ? C26 O4 Cd1 138.9(4) . 2_554 ? O3 Cd1 O4 117.79(14) 4_566 2_544 ? O3 Cd1 N1 85.72(14) 4_566 . ? O4 Cd1 N1 81.84(15) 2_544 . ? O3 Cd1 N3 98.15(14) 4_566 1_454 ? O4 Cd1 N3 88.77(15) 2_544 1_454 ? N1 Cd1 N3 170.58(16) . 1_454 ? O3 Cd1 O2 144.23(13) 4_566 . ? O4 Cd1 O2 97.97(13) 2_544 . ? N1 Cd1 O2 99.70(14) . . ? N3 Cd1 O2 82.21(14) 1_454 . ? O3 Cd1 O1 89.36(13) 4_566 . ? O4 Cd1 O1 152.85(12) 2_544 . ? N1 Cd1 O1 101.23(15) . . ? N3 Cd1 O1 87.45(15) 1_454 . ? O2 Cd1 O1 54.87(12) . . ? O3 Cd1 C19 116.71(15) 4_566 . ? O4 Cd1 C19 125.40(14) 2_544 . ? N1 Cd1 C19 105.26(16) . . ? N3 Cd1 C19 80.75(16) 1_454 . ? O2 Cd1 C19 27.70(13) . . ? O1 Cd1 C19 27.57(13) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.563 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.134 data_[Cd(5-NH2-1,3-BDC)(bimb)] _database_code_depnum_ccdc_archive 'CCDC 874182' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H19 Cd N5 O4' _chemical_formula_sum 'C26 H19 Cd N5 O4' _chemical_formula_weight 577.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5702(19) _cell_length_b 14.329(3) _cell_length_c 16.631(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.75(3) _cell_angle_gamma 90.00 _cell_volume 2254.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7965 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5811 _exptl_absorpt_correction_T_max 0.8228 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21176 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4119 _reflns_number_gt 3735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0328P)^2^+5.6649P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4119 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1192(6) 0.3578(4) 0.4599(3) 0.0645(15) Uani 1 1 d . . . H1A H 0.0941 0.3574 0.5118 0.077 Uiso 1 1 calc R . . C2 C 0.0258(6) 0.3589(5) 0.3898(3) 0.0748(18) Uani 1 1 d . . . H2A H -0.0723 0.3599 0.3845 0.090 Uiso 1 1 calc R . . C3 C 0.2436(5) 0.3578(3) 0.3640(2) 0.0415(10) Uani 1 1 d . . . H3A H 0.3204 0.3578 0.3358 0.050 Uiso 1 1 calc R . . C4 C 0.0623(5) 0.3582(4) 0.2416(3) 0.0502(12) Uani 1 1 d . . . C5 C -0.0734(5) 0.3609(4) 0.2083(3) 0.0581(13) Uani 1 1 d . A . H5A H -0.1431 0.3621 0.2416 0.070 Uiso 1 1 calc R . . C6 C -0.1114(5) 0.3619(4) 0.1242(3) 0.0590(14) Uani 1 1 d . . . H6A H -0.2069 0.3630 0.1026 0.071 Uiso 1 1 calc R A . C7 C -0.0149(5) 0.3613(4) 0.0728(3) 0.0536(13) Uani 1 1 d . A . C8 C 0.1246(16) 0.4046(17) 0.1100(8) 0.045(5) Uani 0.330(19) 1 d P A 1 H8A H 0.1849 0.4317 0.0778 0.054 Uiso 0.330(19) 1 calc PR A 1 C8A C 0.1194(8) 0.3345(12) 0.1076(4) 0.067(4) Uani 0.670(19) 1 d P A 2 H8AA H 0.1848 0.3181 0.0739 0.080 Uiso 0.670(19) 1 calc PR A 2 C9 C 0.1583(15) 0.4022(16) 0.1939(8) 0.043(5) Uani 0.330(19) 1 d P A 1 H9A H 0.2422 0.4286 0.2195 0.052 Uiso 0.330(19) 1 calc PR A 1 C9A C 0.1594(8) 0.3314(12) 0.1910(4) 0.066(4) Uani 0.670(19) 1 d P A 2 H9AA H 0.2497 0.3117 0.2132 0.080 Uiso 0.670(19) 1 calc PR A 2 C10 C -0.0548(5) 0.3651(4) -0.0174(3) 0.0548(13) Uani 1 1 d . . . C11 C -0.1917(5) 0.3453(6) -0.0539(3) 0.094(3) Uani 1 1 d . A . H11A H -0.2594 0.3297 -0.0216 0.113 Uiso 1 1 calc R . . C12 C -0.2296(6) 0.3485(6) -0.1375(3) 0.096(3) Uani 1 1 d . . . H12A H -0.3215 0.3340 -0.1610 0.115 Uiso 1 1 calc R A . C13 C -0.1308(5) 0.3733(4) -0.1859(3) 0.0530(12) Uani 1 1 d . A . C14 C 0.0071(5) 0.3865(4) -0.1518(3) 0.0591(14) Uani 1 1 d . . . H14A H 0.0758 0.3982 -0.1845 0.071 Uiso 1 1 calc R A . C15 C 0.0431(5) 0.3822(4) -0.0681(3) 0.0601(14) Uani 1 1 d . A . H15A H 0.1370 0.3912 -0.0452 0.072 Uiso 1 1 calc R . . C16 C -0.0940(6) 0.4033(5) -0.3316(3) 0.0758(18) Uani 1 1 d . A . H16A H 0.0019 0.4175 -0.3237 0.091 Uiso 1 1 calc R . . C17 C -0.1810(6) 0.4020(4) -0.4030(3) 0.0641(15) Uani 1 1 d . . . H17A H -0.1544 0.4151 -0.4533 0.077 Uiso 1 1 calc R . . C18 C -0.3041(5) 0.3671(4) -0.3121(3) 0.0525(12) Uani 1 1 d . A . H18A H -0.3809 0.3515 -0.2866 0.063 Uiso 1 1 calc R . . C19 C 0.5900(4) 0.4375(3) 0.3838(2) 0.0401(10) Uani 1 1 d . . . C20 C 0.4822(4) 0.3114(3) 0.1010(2) 0.0394(9) Uani 1 1 d . . . C21 C 0.5860(4) 0.4515(3) 0.2933(2) 0.0339(9) Uani 1 1 d . . . C22 C 0.5425(4) 0.3781(3) 0.2405(2) 0.0347(9) Uani 1 1 d . . . H22A H 0.5246 0.3197 0.2610 0.042 Uiso 1 1 calc R . . C23 C 0.5260(4) 0.3925(3) 0.1571(2) 0.0344(9) Uani 1 1 d . . . C24 C 0.5521(4) 0.4792(3) 0.1265(2) 0.0382(9) Uani 1 1 d . . . H24A H 0.5404 0.4882 0.0705 0.046 Uiso 1 1 calc R . . C25 C 0.5956(4) 0.5536(3) 0.1784(2) 0.0379(9) Uani 1 1 d . . . C26 C 0.6136(4) 0.5381(3) 0.2626(2) 0.0391(9) Uani 1 1 d . . . H26A H 0.6445 0.5865 0.2982 0.047 Uiso 1 1 calc R . . N1 N 0.2547(4) 0.3575(2) 0.4440(2) 0.0458(9) Uani 1 1 d . . . N2 N 0.1072(4) 0.3582(3) 0.3281(2) 0.0478(9) Uani 1 1 d . A . N3 N -0.3119(4) 0.3792(3) -0.3909(2) 0.0485(9) Uani 1 1 d . . . N4 N -0.1730(4) 0.3797(3) -0.2729(2) 0.0505(10) Uani 1 1 d . . . N5 N 0.6185(5) 0.6412(3) 0.1482(3) 0.0584(11) Uani 1 1 d . . . H5B H 0.6059 0.6507 0.0966 0.070 Uiso 1 1 calc R . . H5C H 0.6453 0.6863 0.1811 0.070 Uiso 1 1 calc R . . O1 O 0.5628(4) 0.3568(2) 0.40717(17) 0.0538(8) Uani 1 1 d . . . O2 O 0.6147(4) 0.5053(2) 0.43013(17) 0.0604(9) Uani 1 1 d . . . O3 O 0.4328(3) 0.2397(2) 0.13024(17) 0.0454(7) Uani 1 1 d . . . O4 O 0.5013(4) 0.1836(2) 0.52817(16) 0.0533(8) Uani 1 1 d U . . Cd1 Cd 0.47403(3) 0.35920(2) 0.524549(15) 0.03784(12) Uani 1 1 d U . . 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 0.064(3) 0.098(4) 0.031(2) 0.004(3) 0.007(2) -0.010(3) C2 0.056(3) 0.134(6) 0.033(3) 0.001(3) 0.003(2) -0.006(3) C3 0.047(2) 0.047(2) 0.028(2) -0.0040(18) -0.0048(17) 0.006(2) C4 0.041(2) 0.081(3) 0.025(2) -0.002(2) -0.0063(18) 0.005(2) C5 0.042(3) 0.097(4) 0.034(2) -0.002(2) 0.0011(19) 0.000(3) C6 0.036(2) 0.100(4) 0.036(2) -0.002(2) -0.0102(19) 0.001(3) C7 0.038(2) 0.090(4) 0.029(2) -0.002(2) -0.0069(18) 0.013(2) C8 0.043(8) 0.063(13) 0.027(7) -0.002(7) 0.002(5) -0.011(8) C8A 0.034(4) 0.135(13) 0.030(4) -0.012(5) -0.003(3) 0.008(5) C9 0.034(7) 0.063(13) 0.027(7) -0.013(7) -0.013(5) 0.000(7) C9A 0.037(4) 0.127(13) 0.031(4) -0.013(5) -0.007(3) 0.025(5) C10 0.041(3) 0.090(4) 0.029(2) -0.002(2) -0.0050(18) 0.011(2) C11 0.037(3) 0.212(9) 0.031(3) 0.001(4) -0.001(2) 0.002(4) C12 0.040(3) 0.212(9) 0.031(3) -0.003(4) -0.011(2) 0.003(4) C13 0.044(3) 0.087(4) 0.026(2) -0.002(2) -0.0036(18) 0.007(2) C14 0.046(3) 0.096(4) 0.033(2) 0.000(2) -0.003(2) -0.013(3) C15 0.040(3) 0.099(4) 0.036(2) -0.001(3) -0.010(2) -0.012(3) C16 0.047(3) 0.141(6) 0.038(3) 0.006(3) 0.001(2) -0.007(3) C17 0.064(3) 0.099(4) 0.029(2) 0.006(3) 0.004(2) -0.009(3) C18 0.047(3) 0.079(3) 0.028(2) -0.001(2) -0.0050(19) 0.000(2) C19 0.041(2) 0.056(3) 0.0211(19) -0.0028(19) -0.0024(16) 0.008(2) C20 0.043(2) 0.045(2) 0.028(2) -0.0082(18) -0.0019(17) 0.0027(19) C21 0.040(2) 0.039(2) 0.0223(18) -0.0026(16) 0.0032(15) 0.0043(17) C22 0.046(2) 0.034(2) 0.0234(19) -0.0004(15) 0.0049(16) 0.0013(17) C23 0.044(2) 0.037(2) 0.0220(18) -0.0030(16) 0.0028(16) 0.0013(17) C24 0.044(2) 0.049(2) 0.0216(18) 0.0037(17) 0.0051(16) 0.0035(19) C25 0.039(2) 0.038(2) 0.037(2) 0.0031(17) 0.0074(17) -0.0026(18) C26 0.049(2) 0.034(2) 0.032(2) -0.0063(17) 0.0005(17) -0.0006(18) N1 0.061(2) 0.046(2) 0.0263(17) 0.0005(15) -0.0063(16) 0.0040(18) N2 0.049(2) 0.066(3) 0.0255(18) -0.0023(17) -0.0021(15) 0.0025(19) N3 0.053(2) 0.064(2) 0.0254(18) 0.0049(16) -0.0052(16) -0.0008(19) N4 0.046(2) 0.074(3) 0.0269(18) -0.0006(17) -0.0075(16) 0.0020(19) N5 0.083(3) 0.042(2) 0.050(2) 0.0093(18) 0.008(2) -0.014(2) O1 0.093(3) 0.0439(18) 0.0238(15) 0.0053(13) 0.0060(15) -0.0070(17) O2 0.094(3) 0.056(2) 0.0263(15) -0.0128(15) -0.0046(15) 0.0179(18) O3 0.0604(19) 0.0394(16) 0.0349(15) -0.0066(13) 0.0029(13) -0.0041(14) O4 0.090(2) 0.0442(10) 0.0256(15) 0.0115(13) 0.0097(15) 0.0109(16) Cd1 0.0586(2) 0.03592(18) 0.01591(15) 0.00160(11) -0.00424(12) 0.00179(14) _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 C2 1.357(7) . ? C1 N1 1.363(6) . ? C1 H1A 0.9300 . ? C2 N2 1.379(6) . ? C2 H2A 0.9300 . ? C3 N1 1.317(5) . ? C3 N2 1.351(6) . ? C3 H3A 0.9300 . ? C4 C5 1.332(6) . ? C4 C9A 1.400(9) . ? C4 N2 1.438(5) . ? C4 C9 1.446(16) . ? C5 C6 1.391(6) . ? C5 H5A 0.9300 . ? C6 C7 1.351(7) . ? C6 H6A 0.9300 . ? C7 C8A 1.382(9) . ? C7 C10 1.493(6) . ? C7 C8 1.516(17) . ? C8 C9 1.384(19) . ? C8 H8A 0.9300 . ? C8A C9A 1.383(10) . ? C8A H8AA 0.9300 . ? C9 H9A 0.9300 . ? C9A H9AA 0.9300 . ? C10 C15 1.373(7) . ? C10 C11 1.387(7) . ? C11 C12 1.383(7) . ? C11 H11A 0.9300 . ? C12 C13 1.378(7) . ? C12 H12A 0.9300 . ? C13 C14 1.368(6) . ? C13 N4 1.445(5) . ? C14 C15 1.385(6) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.342(7) . ? C16 N4 1.365(6) . ? C16 H16A 0.9300 . ? C17 N3 1.339(6) . ? C17 H17A 0.9300 . ? C18 N3 1.312(5) . ? C18 N4 1.335(6) . ? C18 H18A 0.9300 . ? C19 O2 1.240(5) . ? C19 O1 1.260(5) . ? C19 C21 1.513(5) . ? C20 O4 1.254(5) 4_565 ? C20 O3 1.259(5) . ? C20 C23 1.510(5) . ? C20 Cd1 2.750(4) 4_565 ? C21 C26 1.382(6) . ? C21 C22 1.393(5) . ? C22 C23 1.388(5) . ? C22 H22A 0.9300 . ? C23 C24 1.379(6) . ? C24 C25 1.395(6) . ? C24 H24A 0.9300 . ? C25 N5 1.382(5) . ? C25 C26 1.402(5) . ? C26 H26A 0.9300 . ? N1 Cd1 2.312(4) . ? N3 Cd1 2.320(4) 1_454 ? N5 H5B 0.8600 . ? N5 H5C 0.8600 . ? O1 Cd1 2.245(3) . ? O2 Cd1 2.293(3) 3_666 ? O3 Cd1 2.337(3) 4_565 ? O4 C20 1.254(5) 4_566 ? O4 Cd1 2.529(3) . ? Cd1 O2 2.293(3) 3_666 ? Cd1 N3 2.320(4) 1_656 ? Cd1 O3 2.337(3) 4_566 ? Cd1 C20 2.750(4) 4_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 110.8(4) . . ? C2 C1 H1A 124.6 . . ? N1 C1 H1A 124.6 . . ? C1 C2 N2 105.5(5) . . ? C1 C2 H2A 127.3 . . ? N2 C2 H2A 127.3 . . ? N1 C3 N2 111.7(4) . . ? N1 C3 H3A 124.1 . . ? N2 C3 H3A 124.1 . . ? C5 C4 C9A 116.9(5) . . ? C5 C4 N2 122.7(4) . . ? C9A C4 N2 118.5(4) . . ? C5 C4 C9 114.8(7) . . ? C9A C4 C9 41.8(7) . . ? N2 C4 C9 115.5(6) . . ? C4 C5 C6 120.5(5) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C7 C6 C5 122.5(4) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C8A 114.8(5) . . ? C6 C7 C10 122.8(4) . . ? C8A C7 C10 120.7(5) . . ? C6 C7 C8 112.5(7) . . ? C8A C7 C8 40.3(7) . . ? C10 C7 C8 118.0(7) . . ? C9 C8 C7 117.2(12) . . ? C9 C8 H8A 121.4 . . ? C7 C8 H8A 121.4 . . ? C7 C8A C9A 121.8(7) . . ? C7 C8A H8AA 119.1 . . ? C9A C8A H8AA 119.1 . . ? C8 C9 C4 119.6(11) . . ? C8 C9 H9A 120.2 . . ? C4 C9 H9A 120.2 . . ? C8A C9A C4 119.1(7) . . ? C8A C9A H9AA 120.4 . . ? C4 C9A H9AA 120.4 . . ? C15 C10 C11 117.1(4) . . ? C15 C10 C7 122.0(4) . . ? C11 C10 C7 120.8(5) . . ? C12 C11 C10 121.2(5) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 N4 120.8(4) . . ? C12 C13 N4 119.2(4) . . ? C13 C14 C15 119.2(5) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C10 C15 C14 122.4(4) . . ? C10 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? C17 C16 N4 107.0(5) . . ? C17 C16 H16A 126.5 . . ? N4 C16 H16A 126.5 . . ? N3 C17 C16 109.8(4) . . ? N3 C17 H17A 125.1 . . ? C16 C17 H17A 125.1 . . ? N3 C18 N4 112.1(4) . . ? N3 C18 H18A 123.9 . . ? N4 C18 H18A 123.9 . . ? O2 C19 O1 123.8(4) . . ? O2 C19 C21 119.2(4) . . ? O1 C19 C21 117.0(4) . . ? O4 C20 O3 122.6(4) 4_565 . ? O4 C20 C23 119.0(4) 4_565 . ? O3 C20 C23 118.4(3) . . ? O4 C20 Cd1 66.6(2) 4_565 4_565 ? O3 C20 Cd1 57.8(2) . 4_565 ? C23 C20 Cd1 162.9(3) . 4_565 ? C26 C21 C22 120.0(3) . . ? C26 C21 C19 120.6(3) . . ? C22 C21 C19 119.1(4) . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 C20 121.0(3) . . ? C22 C23 C20 118.8(4) . . ? C23 C24 C25 120.9(3) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? N5 C25 C24 121.2(4) . . ? N5 C25 C26 120.3(4) . . ? C24 C25 C26 118.5(4) . . ? C21 C26 C25 120.6(4) . . ? C21 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C3 N1 C1 105.3(4) . . ? C3 N1 Cd1 120.8(3) . . ? C1 N1 Cd1 134.0(3) . . ? C3 N2 C2 106.8(4) . . ? C3 N2 C4 124.3(4) . . ? C2 N2 C4 128.9(4) . . ? C18 N3 C17 105.7(4) . . ? C18 N3 Cd1 120.0(3) . 1_454 ? C17 N3 Cd1 134.4(3) . 1_454 ? C18 N4 C16 105.4(4) . . ? C18 N4 C13 125.4(4) . . ? C16 N4 C13 129.1(4) . . ? C25 N5 H5B 120.0 . . ? C25 N5 H5C 120.0 . . ? H5B N5 H5C 120.0 . . ? C19 O1 Cd1 112.2(3) . . ? C19 O2 Cd1 145.3(3) . 3_666 ? C20 O3 Cd1 95.0(2) . 4_565 ? C20 O4 Cd1 86.3(3) 4_566 . ? O1 Cd1 O2 120.47(11) . 3_666 ? O1 Cd1 N1 85.76(13) . . ? O2 Cd1 N1 81.39(12) 3_666 . ? O1 Cd1 N3 96.47(13) . 1_656 ? O2 Cd1 N3 91.93(13) 3_666 1_656 ? N1 Cd1 N3 173.16(13) . 1_656 ? O1 Cd1 O3 140.74(11) . 4_566 ? O2 Cd1 O3 98.79(11) 3_666 4_566 ? N1 Cd1 O3 100.79(12) . 4_566 ? N3 Cd1 O3 81.58(12) 1_656 4_566 ? O1 Cd1 O4 87.37(10) . . ? O2 Cd1 O4 151.27(12) 3_666 . ? N1 Cd1 O4 94.86(12) . . ? N3 Cd1 O4 91.71(12) 1_656 . ? O3 Cd1 O4 53.68(10) 4_566 . ? O1 Cd1 C20 113.61(12) . 4_566 ? O2 Cd1 C20 125.92(12) 3_666 4_566 ? N1 Cd1 C20 102.59(12) . 4_566 ? N3 Cd1 C20 82.48(13) 1_656 4_566 ? O3 Cd1 C20 27.13(11) 4_566 4_566 ? O4 Cd1 C20 27.07(11) . 4_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5B O4 0.86 2.22 3.044(5) 160.3 2_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.889 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.072 data_[Cd(5-HO-1,3-BDC)(bimb)]n _database_code_depnum_ccdc_archive 'CCDC 874183' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd N4 O5' _chemical_formula_sum 'C26 H18 Cd N4 O5' _chemical_formula_weight 578.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6647(19) _cell_length_b 14.032(3) _cell_length_c 16.543(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.79(3) _cell_angle_gamma 90.00 _cell_volume 2217.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8049 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6825 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21086 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.36 _reflns_number_total 4049 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics "'ORTEPII (Johnson, 1976)" _computing_publication_material SHELXL97 _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^)+(0.0440P)^2^+3.6394P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4049 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1072(5) 0.6325(3) 0.4588(2) 0.0542(11) Uani 1 1 d . . . H1A H 0.0832 0.6247 0.5108 0.065 Uiso 1 1 calc R . . C2 C 0.0159(5) 0.6333(4) 0.3882(3) 0.0623(13) Uani 1 1 d . . . H2A H -0.0809 0.6265 0.3826 0.075 Uiso 1 1 calc R . . C3 C 0.2282(4) 0.6524(3) 0.3621(2) 0.0386(8) Uani 1 1 d . . . H3A H 0.3032 0.6609 0.3337 0.046 Uiso 1 1 calc R . . C4 C 0.0483(4) 0.6488(3) 0.2396(2) 0.0422(9) Uani 1 1 d . . . C5 C -0.0874(4) 0.6336(3) 0.2067(2) 0.0465(10) Uani 1 1 d . . . H5A H -0.1542 0.6235 0.2407 0.056 Uiso 1 1 calc R . . C6 C -0.1265(4) 0.6332(3) 0.1224(2) 0.0471(10) Uani 1 1 d . . . H6A H -0.2200 0.6231 0.1008 0.057 Uiso 1 1 calc R . . C7 C -0.0321(4) 0.6469(3) 0.0704(2) 0.0462(10) Uani 1 1 d . . . C8 C 0.1015(5) 0.6708(5) 0.1048(3) 0.0835(19) Uani 1 1 d . . . H8A H 0.1666 0.6858 0.0709 0.100 Uiso 1 1 calc R . . C9 C 0.1422(5) 0.6732(5) 0.1887(3) 0.085(2) Uani 1 1 d . . . H9A H 0.2329 0.6912 0.2105 0.103 Uiso 1 1 calc R . . C10 C -0.0724(4) 0.6426(3) -0.0203(2) 0.0451(10) Uani 1 1 d . . . C11 C -0.2067(4) 0.6679(4) -0.0572(3) 0.0595(12) Uani 1 1 d . . . H11A H -0.2720 0.6875 -0.0248 0.071 Uiso 1 1 calc R . . C12 C -0.2444(4) 0.6644(4) -0.1410(2) 0.0557(12) Uani 1 1 d . . . H12A H -0.3343 0.6820 -0.1646 0.067 Uiso 1 1 calc R . . C13 C -0.1484(4) 0.6346(3) -0.1899(2) 0.0403(9) Uani 1 1 d . . . C14 C -0.0131(5) 0.6145(4) -0.1551(2) 0.0549(11) Uani 1 1 d . . . H14A H 0.0534 0.5982 -0.1879 0.066 Uiso 1 1 calc R . . C15 C 0.0234(4) 0.6186(4) -0.0712(3) 0.0564(12) Uani 1 1 d . . . H15A H 0.1151 0.6048 -0.0481 0.068 Uiso 1 1 calc R . . C16 C -0.1119(4) 0.5995(4) -0.3355(3) 0.0586(12) Uani 1 1 d . . . H16A H -0.0177 0.5827 -0.3269 0.070 Uiso 1 1 calc R . . C17 C -0.1982(4) 0.6007(3) -0.4079(2) 0.0524(11) Uani 1 1 d . . . H17A H -0.1726 0.5848 -0.4581 0.063 Uiso 1 1 calc R . . C18 C -0.3190(4) 0.6438(3) -0.3171(2) 0.0455(10) Uani 1 1 d . . . H18A H -0.3938 0.6633 -0.2918 0.055 Uiso 1 1 calc R . . C19 C 0.5816(4) 0.5587(2) 0.37912(19) 0.0321(7) Uani 1 1 d . . . C20 C 0.4642(4) 0.6776(2) 0.09096(19) 0.0319(7) Uani 1 1 d . . . C21 C 0.5765(3) 0.5423(2) 0.28847(18) 0.0286(7) Uani 1 1 d . . . C22 C 0.5262(3) 0.6138(2) 0.23385(19) 0.0297(7) Uani 1 1 d . . . H22A H 0.5022 0.6728 0.2534 0.036 Uiso 1 1 calc R . . C23 C 0.5114(3) 0.5976(2) 0.14990(18) 0.0280(7) Uani 1 1 d . . . C24 C 0.5462(4) 0.5094(2) 0.12125(19) 0.0342(7) Uani 1 1 d . . . H24A H 0.5361 0.4983 0.0652 0.041 Uiso 1 1 calc R . . C25 C 0.5960(4) 0.4380(2) 0.1753(2) 0.0336(7) Uani 1 1 d . . . C26 C 0.6141(4) 0.4541(2) 0.2591(2) 0.0332(7) Uani 1 1 d . . . H26A H 0.6510 0.4066 0.2954 0.040 Uiso 1 1 calc R . . N1 N 0.2408(3) 0.6451(2) 0.44202(18) 0.0394(7) Uani 1 1 d . . . N2 N 0.0942(3) 0.6461(2) 0.32634(18) 0.0387(7) Uani 1 1 d . . . N3 N -0.3282(3) 0.6289(2) -0.39612(18) 0.0422(7) Uani 1 1 d . . . N4 N -0.1900(3) 0.6278(2) -0.27711(18) 0.0405(7) Uani 1 1 d . . . O1 O 0.5440(3) 0.63887(18) 0.40070(15) 0.0435(6) Uani 1 1 d . . . O2 O 0.6213(3) 0.49233(18) 0.42731(14) 0.0488(7) Uani 1 1 d . . . O3 O 0.4197(3) 0.75283(16) 0.12045(14) 0.0355(5) Uani 1 1 d . . . O4 O 0.4768(3) 0.6691(2) 0.01760(14) 0.0481(7) Uani 1 1 d . . . O5 O 0.6288(3) 0.34944(18) 0.14965(17) 0.0531(8) Uani 1 1 d . . . H5B H 0.5984 0.3435 0.1009 0.080 Uiso 1 1 calc R . . Cd1 Cd 0.45956(3) 0.642579(17) 0.519665(13) 0.03090(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 C1 0.056(3) 0.083(3) 0.0237(19) 0.0018(19) 0.0070(18) 0.005(2) C2 0.047(2) 0.111(4) 0.028(2) 0.006(2) 0.0052(18) 0.006(2) C3 0.043(2) 0.046(2) 0.0228(17) 0.0044(15) -0.0059(15) -0.0079(16) C4 0.041(2) 0.060(3) 0.0226(18) 0.0061(16) -0.0046(15) -0.0016(17) C5 0.038(2) 0.072(3) 0.0289(19) 0.0025(18) 0.0028(16) -0.0036(18) C6 0.0338(19) 0.073(3) 0.032(2) 0.0001(18) -0.0056(16) -0.0056(18) C7 0.037(2) 0.073(3) 0.0253(19) 0.0053(17) -0.0069(15) -0.0068(18) C8 0.040(2) 0.178(6) 0.030(2) 0.011(3) -0.0026(18) -0.015(3) C9 0.043(2) 0.180(6) 0.030(2) 0.009(3) -0.0072(19) -0.020(3) C10 0.040(2) 0.067(3) 0.0263(19) 0.0027(17) -0.0044(16) -0.0048(18) C11 0.040(2) 0.106(4) 0.031(2) -0.001(2) -0.0014(17) -0.001(2) C12 0.036(2) 0.094(4) 0.033(2) -0.002(2) -0.0083(16) 0.006(2) C13 0.040(2) 0.054(2) 0.0234(18) 0.0016(15) -0.0063(15) -0.0036(17) C14 0.049(2) 0.083(3) 0.030(2) -0.002(2) -0.0032(17) 0.018(2) C15 0.041(2) 0.090(3) 0.034(2) 0.000(2) -0.0088(17) 0.015(2) C16 0.044(2) 0.093(4) 0.036(2) -0.004(2) -0.0007(18) 0.011(2) C17 0.056(3) 0.072(3) 0.028(2) -0.0071(19) 0.0013(17) 0.008(2) C18 0.043(2) 0.068(3) 0.0219(18) -0.0014(17) -0.0044(15) 0.0026(18) C19 0.0401(18) 0.0362(19) 0.0186(15) 0.0039(14) -0.0004(13) -0.0059(15) C20 0.0388(18) 0.0339(18) 0.0215(16) 0.0036(14) 0.0002(13) -0.0012(15) C21 0.0366(17) 0.0284(16) 0.0189(15) 0.0032(12) -0.0016(13) -0.0026(13) C22 0.0403(18) 0.0278(16) 0.0206(16) -0.0002(13) 0.0037(13) -0.0017(14) C23 0.0368(17) 0.0279(17) 0.0184(15) 0.0042(13) 0.0012(13) -0.0013(13) C24 0.052(2) 0.0335(18) 0.0167(15) -0.0013(13) 0.0026(14) -0.0009(16) C25 0.0467(19) 0.0272(17) 0.0256(17) -0.0036(14) 0.0016(14) 0.0025(15) C26 0.0442(19) 0.0306(18) 0.0232(16) 0.0053(13) -0.0006(14) 0.0018(14) N1 0.0528(19) 0.0381(17) 0.0227(15) 0.0040(12) -0.0083(13) -0.0026(14) N2 0.0410(17) 0.0510(19) 0.0218(15) 0.0042(13) -0.0023(12) -0.0025(14) N3 0.0465(18) 0.054(2) 0.0236(15) -0.0017(13) -0.0031(13) 0.0013(15) N4 0.0413(17) 0.054(2) 0.0234(15) 0.0017(13) -0.0035(13) -0.0010(14) O1 0.0667(18) 0.0441(16) 0.0186(12) -0.0020(10) 0.0034(12) 0.0105(13) O2 0.0848(19) 0.0347(14) 0.0220(12) 0.0081(11) -0.0075(12) -0.0101(13) O3 0.0504(14) 0.0294(13) 0.0255(12) 0.0049(10) 0.0019(10) 0.0036(10) O4 0.0771(19) 0.0499(16) 0.0175(13) 0.0078(11) 0.0077(12) 0.0111(14) O5 0.090(2) 0.0352(15) 0.0305(14) -0.0067(11) -0.0013(14) 0.0199(14) Cd1 0.04869(18) 0.02781(15) 0.01378(14) -0.00167(9) -0.00298(10) -0.00020(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 C2 1.353(6) . ? C1 N1 1.373(6) . ? C1 H1A 0.9300 . ? C2 N2 1.374(5) . ? C2 H2A 0.9300 . ? C3 N1 1.312(5) . ? C3 N2 1.343(5) . ? C3 H3A 0.9300 . ? C4 C5 1.357(5) . ? C4 C9 1.373(6) . ? C4 N2 1.436(4) . ? C5 C6 1.389(5) . ? C5 H5A 0.9300 . ? C6 C7 1.360(6) . ? C6 H6A 0.9300 . ? C7 C8 1.371(6) . ? C7 C10 1.492(5) . ? C8 C9 1.383(6) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.385(6) . ? C10 C11 1.394(6) . ? C11 C12 1.379(6) . ? C11 H11A 0.9300 . ? C12 C13 1.386(6) . ? C12 H12A 0.9300 . ? C13 C14 1.375(6) . ? C13 N4 1.440(4) . ? C14 C15 1.381(6) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.351(6) . ? C16 N4 1.373(5) . ? C16 H16A 0.9300 . ? C17 N3 1.359(5) . ? C17 H17A 0.9300 . ? C18 N3 1.314(5) . ? C18 N4 1.338(5) . ? C18 H18A 0.9300 . ? C19 O2 1.247(4) . ? C19 O1 1.251(4) . ? C19 C21 1.510(4) . ? C20 O4 1.244(4) . ? C20 O3 1.266(4) . ? C20 C23 1.511(4) . ? C21 C22 1.388(4) . ? C21 C26 1.397(5) . ? C22 C23 1.393(4) . ? C22 H22A 0.9300 . ? C23 C24 1.385(5) . ? C24 C25 1.380(5) . ? C24 H24A 0.9300 . ? C25 O5 1.366(4) . ? C25 C26 1.389(5) . ? C26 H26A 0.9300 . ? N1 Cd1 2.301(3) . ? N3 Cd1 2.305(3) 1_454 ? O1 Cd1 2.243(3) . ? O2 Cd1 2.274(2) 3_666 ? O3 Cd1 2.298(2) 4_575 ? O4 Cd1 2.649(3) 4_575 ? O5 H5B 0.8200 . ? Cd1 O2 2.274(2) 3_666 ? Cd1 O3 2.298(2) 4_576 ? Cd1 N3 2.305(3) 1_656 ? Cd1 O4 2.649(3) 4_576 ? 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 C2 C1 N1 109.5(4) . . ? C2 C1 H1A 125.3 . . ? N1 C1 H1A 125.3 . . ? C1 C2 N2 106.5(4) . . ? C1 C2 H2A 126.8 . . ? N2 C2 H2A 126.8 . . ? N1 C3 N2 111.9(3) . . ? N1 C3 H3A 124.0 . . ? N2 C3 H3A 124.0 . . ? C5 C4 C9 118.8(4) . . ? C5 C4 N2 121.9(3) . . ? C9 C4 N2 119.2(3) . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 121.9(4) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 116.9(4) . . ? C6 C7 C10 122.2(4) . . ? C8 C7 C10 120.8(4) . . ? C7 C8 C9 121.9(4) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C4 C9 C8 119.7(4) . . ? C4 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C15 C10 C11 117.4(4) . . ? C15 C10 C7 121.7(4) . . ? C11 C10 C7 120.8(4) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 N4 120.5(4) . . ? C12 C13 N4 119.7(3) . . ? C13 C14 C15 119.5(4) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C14 C15 C10 122.0(4) . . ? C14 C15 H15A 119.0 . . ? C10 C15 H15A 119.0 . . ? C17 C16 N4 106.8(4) . . ? C17 C16 H16A 126.6 . . ? N4 C16 H16A 126.6 . . ? C16 C17 N3 109.6(4) . . ? C16 C17 H17A 125.2 . . ? N3 C17 H17A 125.2 . . ? N3 C18 N4 112.4(4) . . ? N3 C18 H18A 123.8 . . ? N4 C18 H18A 123.8 . . ? O2 C19 O1 124.3(3) . . ? O2 C19 C21 118.8(3) . . ? O1 C19 C21 117.0(3) . . ? O4 C20 O3 123.1(3) . . ? O4 C20 C23 119.6(3) . . ? O3 C20 C23 117.2(3) . . ? C22 C21 C26 119.9(3) . . ? C22 C21 C19 119.4(3) . . ? C26 C21 C19 120.6(3) . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 C20 120.5(3) . . ? C22 C23 C20 119.8(3) . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? O5 C25 C24 122.2(3) . . ? O5 C25 C26 117.3(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 119.4(3) . . ? C25 C26 H26A 120.3 . . ? C21 C26 H26A 120.3 . . ? C3 N1 C1 105.6(3) . . ? C3 N1 Cd1 119.9(3) . . ? C1 N1 Cd1 134.2(2) . . ? C3 N2 C2 106.5(3) . . ? C3 N2 C4 124.7(3) . . ? C2 N2 C4 128.8(3) . . ? C18 N3 C17 105.4(3) . . ? C18 N3 Cd1 120.4(3) . 1_454 ? C17 N3 Cd1 134.0(2) . 1_454 ? C18 N4 C16 105.8(3) . . ? C18 N4 C13 125.5(3) . . ? C16 N4 C13 128.6(3) . . ? C19 O1 Cd1 115.6(2) . . ? C19 O2 Cd1 141.0(2) . 3_666 ? C20 O3 Cd1 98.56(19) . 4_575 ? C20 O4 Cd1 82.9(2) . 4_575 ? C25 O5 H5B 109.5 . . ? O1 Cd1 O2 120.76(9) . 3_666 ? O1 Cd1 O3 140.83(9) . 4_576 ? O2 Cd1 O3 98.41(9) 3_666 4_576 ? O1 Cd1 N1 86.39(11) . . ? O2 Cd1 N1 83.54(10) 3_666 . ? O3 Cd1 N1 98.84(10) 4_576 . ? O1 Cd1 N3 96.82(11) . 1_656 ? O2 Cd1 N3 91.38(11) 3_666 1_656 ? O3 Cd1 N3 81.20(10) 4_576 1_656 ? N1 Cd1 N3 174.88(11) . 1_656 ? O1 Cd1 O4 88.84(8) . 4_576 ? O2 Cd1 O4 149.48(9) 3_666 4_576 ? O3 Cd1 O4 52.40(8) 4_576 4_576 ? N1 Cd1 O4 91.82(9) . 4_576 ? N3 Cd1 O4 92.23(10) 1_656 4_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5B O4 0.82 1.99 2.811(4) 179.2 3_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.932 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.074 data_{[Cd2(OH2)(5-NO2-1,3-BDC)2(bimb)]*2(H2O)}n _database_code_depnum_ccdc_archive 'CCDC 874184' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H28 Cd2 N6 O16' _chemical_formula_sum 'C34 H28 Cd2 N6 O16' _chemical_formula_weight 1001.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.967(2) _cell_length_b 12.179(2) _cell_length_c 15.859(3) _cell_angle_alpha 96.41(3) _cell_angle_beta 96.96(3) _cell_angle_gamma 104.19(3) _cell_volume 1832.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5669 _cell_measurement_theta_min 3.0910 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7064 _exptl_absorpt_correction_T_max 0.8856 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ?0 _diffrn_standards_decay_% ?0 _diffrn_reflns_number 17804 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6640 _reflns_number_gt 5269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0487P)^2^+1.3397P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6640 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5656(5) 0.7924(4) 0.1676(3) 0.0372(12) Uani 1 1 d . . . H1A H 0.6400 0.7608 0.1599 0.045 Uiso 1 1 calc R . . C2 C 0.5007(5) 0.8408(5) 0.1084(3) 0.0393(12) Uani 1 1 d . . . H2A H 0.5210 0.8483 0.0533 0.047 Uiso 1 1 calc R . . C3 C 0.4059(4) 0.8482(4) 0.2256(3) 0.0293(10) Uani 1 1 d . . . H3A H 0.3480 0.8628 0.2649 0.035 Uiso 1 1 calc R . . C4 C 0.2904(5) 0.9215(4) 0.1050(3) 0.0327(11) Uani 1 1 d . . . C5 C 0.2648(7) 0.9102(7) 0.0170(3) 0.070(2) Uani 1 1 d . . . H5A H 0.3227 0.8805 -0.0156 0.084 Uiso 1 1 calc R . . C6 C 0.1519(7) 0.9435(7) -0.0235(4) 0.074(2) Uani 1 1 d . . . H6A H 0.1368 0.9367 -0.0831 0.089 Uiso 1 1 calc R . . C7 C 0.0629(5) 0.9858(4) 0.0221(3) 0.0376(11) Uani 1 1 d . . . C8 C 0.0927(6) 0.9988(5) 0.1099(3) 0.0506(15) Uani 1 1 d . . . H8A H 0.0351 1.0286 0.1427 0.061 Uiso 1 1 calc R . . C9 C 0.2065(6) 0.9687(5) 0.1515(3) 0.0520(15) Uani 1 1 d . . . H9A H 0.2255 0.9808 0.2112 0.062 Uiso 1 1 calc R . . C10 C 1.4397(5) 0.5171(4) 0.0159(3) 0.0345(11) Uani 1 1 d . . . C11 C 1.3603(6) 0.5735(5) -0.0326(3) 0.0472(13) Uani 1 1 d . . . H11A H 1.3813 0.5880 -0.0865 0.057 Uiso 1 1 calc R . . C12 C 1.2511(5) 0.6086(5) -0.0026(3) 0.0481(14) Uani 1 1 d . . . H12A H 1.2002 0.6467 -0.0362 0.058 Uiso 1 1 calc R . . C13 C 1.2166(5) 0.5877(4) 0.0767(3) 0.0316(10) Uani 1 1 d . . . C14 C 1.2902(6) 0.5292(5) 0.1247(3) 0.0495(14) Uani 1 1 d . . . H14A H 1.2669 0.5130 0.1778 0.059 Uiso 1 1 calc R . . C15 C 1.4007(6) 0.4939(5) 0.0938(3) 0.0509(15) Uani 1 1 d . . . H15A H 1.4494 0.4536 0.1268 0.061 Uiso 1 1 calc R . . C16 C 1.0013(5) 0.6625(5) 0.0634(3) 0.0460(13) Uani 1 1 d . . . H16C H 0.9808 0.6560 0.0040 0.055 Uiso 1 1 calc R . . C17 C 0.9319(5) 0.7050(5) 0.1213(3) 0.0451(13) Uani 1 1 d . . . H17A H 0.8541 0.7328 0.1081 0.054 Uiso 1 1 calc R . . C18 C 1.0989(5) 0.6565(4) 0.1929(3) 0.0321(10) Uani 1 1 d . . . H18A H 1.1597 0.6443 0.2381 0.039 Uiso 1 1 calc R . . C19 C 0.7109(5) 0.5666(4) 0.3626(3) 0.0352(11) Uani 1 1 d . . . C20 C 0.9324(4) 0.3152(4) 0.5330(3) 0.0320(10) Uani 1 1 d . . . C21 C 0.7923(4) 0.4793(4) 0.3678(3) 0.0292(10) Uani 1 1 d . . . C22 C 0.8158(4) 0.4334(4) 0.4433(3) 0.0300(10) Uani 1 1 d . . . H22A H 0.7753 0.4543 0.4904 0.036 Uiso 1 1 calc R . . C23 C 0.8991(4) 0.3568(4) 0.4496(3) 0.0303(10) Uani 1 1 d . . . C24 C 0.9546(5) 0.3218(4) 0.3785(3) 0.0339(11) Uani 1 1 d . . . H24A H 1.0079 0.2691 0.3808 0.041 Uiso 1 1 calc R . . C25 C 0.9290(5) 0.3671(4) 0.3042(3) 0.0338(11) Uani 1 1 d . . . C26 C 0.8498(4) 0.4458(4) 0.2965(3) 0.0323(10) Uani 1 1 d . . . H26A H 0.8356 0.4752 0.2455 0.039 Uiso 1 1 calc R . . C27 C 0.8057(4) 0.9440(4) 0.3212(3) 0.0326(11) Uani 1 1 d . . . C28 C 0.5466(4) 1.1569(4) 0.5038(3) 0.0303(10) Uani 1 1 d . . . C29 C 0.7226(4) 1.0319(4) 0.3316(3) 0.0271(10) Uani 1 1 d . . . C30 C 0.6772(4) 1.0556(4) 0.4096(3) 0.0284(10) Uani 1 1 d . . . H30A H 0.7029 1.0205 0.4559 0.034 Uiso 1 1 calc R . . C31 C 0.5936(4) 1.1314(4) 0.4191(3) 0.0259(9) Uani 1 1 d . . . C32 C 0.5548(5) 1.1827(4) 0.3503(3) 0.0320(10) Uani 1 1 d . . . H32A H 0.4976 1.2323 0.3551 0.038 Uiso 1 1 calc R . . C33 C 0.6028(5) 1.1586(4) 0.2739(3) 0.0315(10) Uani 1 1 d . . . C34 C 0.6881(5) 1.0861(4) 0.2634(3) 0.0327(10) Uani 1 1 d . . . H34A H 0.7214 1.0740 0.2118 0.039 Uiso 1 1 calc R . . N1 N 0.5064(4) 0.7967(3) 0.2408(2) 0.0304(8) Uani 1 1 d . . . N2 N 0.3979(4) 0.8770(3) 0.1457(2) 0.0306(8) Uani 1 1 d . . . N3 N 0.9933(4) 0.7011(3) 0.2028(2) 0.0355(9) Uani 1 1 d . . . N4 N 1.1085(4) 0.6303(3) 0.1089(2) 0.0332(9) Uani 1 1 d . . . N5 N 0.9881(5) 0.3291(4) 0.2287(3) 0.0502(11) Uani 1 1 d . . . N6 N 0.5615(5) 1.2147(4) 0.2012(3) 0.0520(12) Uani 1 1 d . . . O1 O 0.6398(4) 0.5826(3) 0.4206(2) 0.0506(9) Uani 1 1 d . . . O2 O 0.7212(3) 0.6263(3) 0.3025(2) 0.0382(8) Uani 1 1 d . . . O3 O 1.0197(3) 0.2544(3) 0.5359(2) 0.0443(9) Uani 1 1 d . . . O4 O 0.8789(4) 0.3412(3) 0.5973(2) 0.0422(8) Uani 1 1 d . . . O5 O 1.0538(7) 0.2593(5) 0.2340(3) 0.115(2) Uani 1 1 d . . . O6 O 0.9730(5) 0.3725(4) 0.1644(3) 0.0761(14) Uani 1 1 d . . . O7 O 0.7942(3) 0.8717(3) 0.3745(2) 0.0342(7) Uani 1 1 d . . . O8 O 0.8784(4) 0.9421(3) 0.2640(2) 0.0455(9) Uani 1 1 d U . . O9 O 0.4481(3) 1.2071(3) 0.5031(2) 0.0401(8) Uani 1 1 d . . . O10 O 0.6035(3) 1.1327(3) 0.5703(2) 0.0381(8) Uani 1 1 d . . . O11 O 0.4980(6) 1.2849(5) 0.2118(3) 0.0920(18) Uani 1 1 d . . . O12 O 0.5933(8) 1.1875(6) 0.1327(3) 0.125(3) Uani 1 1 d . . . O13 O 0.3426(3) 0.5993(3) 0.3447(2) 0.0408(8) Uani 1 1 d . . . H13A H 0.3201 0.6262 0.3855 0.061 Uiso 1 1 d R . . H13B H 0.3621 0.5351 0.3545 0.061 Uiso 1 1 d R . . O14 O 1.1642(3) 0.9210(3) 0.3557(2) 0.0411(8) Uani 1 1 d . . . H14C H 1.2319 0.9103 0.4004 0.062 Uiso 1 1 d R . . H14B H 1.1066 0.9015 0.3787 0.062 Uiso 1 1 d R . . O15 O 0.8276(4) 0.8578(3) 0.5797(2) 0.0563(10) Uani 1 1 d . . . H15C H 0.8839 0.8666 0.5458 0.084 Uiso 1 1 d R . . H15B H 0.7533 0.8680 0.5583 0.084 Uiso 1 1 d R . . O16 O 0.3379(5) 0.3899(4) 0.3912(3) 0.0820(14) Uani 1 1 d . . . H16A H 0.2676 0.3582 0.3527 0.123 Uiso 1 1 d R . . H16B H 0.3725 0.3892 0.4407 0.123 Uiso 1 1 d R . . Cd1 Cd 0.95377(3) 0.77996(3) 0.32727(2) 0.03105(12) Uani 1 1 d U . . Cd2 Cd 0.56300(3) 0.73022(3) 0.36186(2) 0.03118(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(2) 0.056(3) 0.034(3) 0.007(2) 0.009(2) 0.025(2) C2 0.037(3) 0.063(4) 0.027(3) 0.015(2) 0.013(2) 0.023(2) C3 0.030(2) 0.033(3) 0.027(2) 0.0081(19) 0.0027(19) 0.0099(19) C4 0.037(3) 0.039(3) 0.031(3) 0.013(2) 0.005(2) 0.023(2) C5 0.081(4) 0.135(6) 0.028(3) 0.024(3) 0.019(3) 0.079(4) C6 0.079(4) 0.147(7) 0.029(3) 0.026(4) 0.017(3) 0.083(5) C7 0.049(3) 0.043(3) 0.030(3) 0.011(2) 0.007(2) 0.026(2) C8 0.059(3) 0.076(4) 0.030(3) 0.006(3) 0.006(2) 0.046(3) C9 0.063(3) 0.078(4) 0.026(3) 0.005(3) 0.001(2) 0.042(3) C10 0.045(3) 0.038(3) 0.030(3) 0.009(2) 0.014(2) 0.023(2) C11 0.061(3) 0.063(4) 0.033(3) 0.017(3) 0.025(3) 0.032(3) C12 0.052(3) 0.070(4) 0.042(3) 0.021(3) 0.018(3) 0.042(3) C13 0.037(3) 0.034(3) 0.029(2) 0.000(2) 0.012(2) 0.016(2) C14 0.066(4) 0.068(4) 0.038(3) 0.026(3) 0.031(3) 0.042(3) C15 0.061(3) 0.072(4) 0.047(3) 0.032(3) 0.026(3) 0.050(3) C16 0.043(3) 0.068(4) 0.029(3) 0.001(3) -0.002(2) 0.024(3) C17 0.037(3) 0.071(4) 0.036(3) 0.005(3) 0.005(2) 0.032(3) C18 0.030(2) 0.038(3) 0.031(3) 0.001(2) 0.008(2) 0.016(2) C19 0.030(2) 0.030(3) 0.048(3) 0.010(2) 0.000(2) 0.014(2) C20 0.028(2) 0.028(3) 0.041(3) 0.012(2) 0.001(2) 0.0095(19) C21 0.023(2) 0.025(2) 0.042(3) 0.005(2) 0.0031(19) 0.0128(18) C22 0.030(2) 0.028(3) 0.034(3) 0.007(2) 0.0058(19) 0.0111(19) C23 0.029(2) 0.027(2) 0.035(3) 0.006(2) 0.002(2) 0.0080(18) C24 0.034(2) 0.029(3) 0.044(3) 0.007(2) 0.005(2) 0.019(2) C25 0.042(3) 0.032(3) 0.030(3) 0.005(2) 0.003(2) 0.015(2) C26 0.033(2) 0.029(3) 0.035(3) 0.006(2) 0.001(2) 0.0112(19) C27 0.029(2) 0.030(3) 0.039(3) -0.003(2) 0.002(2) 0.0112(19) C28 0.028(2) 0.028(3) 0.036(3) 0.000(2) 0.011(2) 0.0089(19) C29 0.026(2) 0.023(2) 0.034(3) 0.0028(19) 0.0053(19) 0.0090(18) C30 0.031(2) 0.027(2) 0.032(2) 0.0065(19) 0.0086(19) 0.0145(19) C31 0.026(2) 0.025(2) 0.028(2) 0.0020(18) 0.0049(18) 0.0102(18) C32 0.035(2) 0.029(3) 0.040(3) 0.008(2) 0.007(2) 0.019(2) C33 0.041(3) 0.032(3) 0.031(3) 0.015(2) 0.012(2) 0.021(2) C34 0.040(3) 0.032(3) 0.031(3) 0.010(2) 0.012(2) 0.014(2) N1 0.0298(19) 0.038(2) 0.026(2) 0.0049(17) 0.0023(16) 0.0158(17) N2 0.034(2) 0.037(2) 0.026(2) 0.0091(17) 0.0055(16) 0.0172(17) N3 0.036(2) 0.042(2) 0.033(2) 0.0057(18) 0.0114(18) 0.0174(18) N4 0.035(2) 0.041(2) 0.028(2) 0.0045(17) 0.0110(17) 0.0158(18) N5 0.071(3) 0.051(3) 0.039(3) 0.004(2) 0.016(2) 0.036(2) N6 0.078(3) 0.056(3) 0.043(3) 0.026(2) 0.021(2) 0.042(3) O1 0.054(2) 0.057(2) 0.058(2) 0.0197(19) 0.0201(19) 0.0364(19) O2 0.0443(19) 0.0346(19) 0.043(2) 0.0154(16) 0.0050(15) 0.0207(15) O3 0.051(2) 0.053(2) 0.042(2) 0.0210(17) 0.0068(16) 0.0323(18) O4 0.051(2) 0.051(2) 0.0351(19) 0.0157(16) 0.0142(16) 0.0258(17) O5 0.197(6) 0.145(5) 0.072(3) 0.038(3) 0.065(4) 0.144(5) O6 0.108(4) 0.105(4) 0.041(2) 0.020(2) 0.025(2) 0.066(3) O7 0.0352(17) 0.0301(18) 0.044(2) 0.0080(15) 0.0056(15) 0.0200(14) O8 0.048(2) 0.054(2) 0.048(2) 0.0075(17) 0.0224(17) 0.0294(17) O9 0.0439(19) 0.054(2) 0.0333(18) 0.0046(16) 0.0118(15) 0.0323(17) O10 0.0421(19) 0.050(2) 0.0277(18) 0.0095(15) 0.0053(15) 0.0202(16) O11 0.143(4) 0.120(4) 0.067(3) 0.050(3) 0.039(3) 0.107(4) O12 0.240(7) 0.161(6) 0.057(3) 0.068(3) 0.083(4) 0.157(6) O13 0.0461(19) 0.042(2) 0.042(2) 0.0111(16) 0.0113(16) 0.0219(16) O14 0.0334(17) 0.053(2) 0.0392(19) 0.0144(16) 0.0054(15) 0.0134(15) O15 0.058(2) 0.062(3) 0.052(2) 0.004(2) -0.0015(19) 0.029(2) O16 0.109(4) 0.065(3) 0.074(3) 0.027(2) 0.003(3) 0.025(3) Cd1 0.0353(2) 0.0366(2) 0.0300(2) 0.00739(15) 0.01085(15) 0.02191(15) Cd2 0.0374(2) 0.0382(2) 0.02717(19) 0.00992(15) 0.00742(14) 0.02368(16) _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 C2 1.346(6) . ? C1 N1 1.365(6) . ? C1 H1A 0.9300 . ? C2 N2 1.380(6) . ? C2 H2A 0.9300 . ? C3 N1 1.318(5) . ? C3 N2 1.351(5) . ? C3 H3A 0.9300 . ? C4 C9 1.365(7) . ? C4 C5 1.373(7) . ? C4 N2 1.433(5) . ? C5 C6 1.396(7) . ? C5 H5A 0.9300 . ? C6 C7 1.369(7) . ? C6 H6A 0.9300 . ? C7 C8 1.371(7) . ? C7 C7 1.495(9) 2_575 ? C8 C9 1.389(7) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.377(7) . ? C10 C11 1.388(7) . ? C10 C10 1.489(8) 2_865 ? C11 C12 1.379(7) . ? C11 H11A 0.9300 . ? C12 C13 1.377(7) . ? C12 H12A 0.9300 . ? C13 C14 1.366(7) . ? C13 N4 1.428(5) . ? C14 C15 1.398(7) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.347(7) . ? C16 N4 1.377(6) . ? C16 H16C 0.9300 . ? C17 N3 1.372(6) . ? C17 H17A 0.9300 . ? C18 N3 1.315(5) . ? C18 N4 1.355(6) . ? C18 H18A 0.9300 . ? C19 O1 1.254(6) . ? C19 O2 1.260(6) . ? C19 C21 1.491(6) . ? C19 Cd2 2.754(5) . ? C20 O4 1.251(6) . ? C20 O3 1.273(5) . ? C20 C23 1.497(6) . ? C21 C26 1.394(6) . ? C21 C22 1.395(6) . ? C22 C23 1.397(6) . ? C22 H22A 0.9300 . ? C23 C24 1.386(6) . ? C24 C25 1.378(6) . ? C24 H24A 0.9300 . ? C25 C26 1.389(6) . ? C25 N5 1.474(6) . ? C26 H26A 0.9300 . ? C27 O8 1.230(6) . ? C27 O7 1.283(6) . ? C27 C29 1.513(6) . ? C28 O10 1.237(5) . ? C28 O9 1.277(5) . ? C28 C31 1.499(6) . ? C29 C34 1.380(6) . ? C29 C30 1.392(6) . ? C30 C31 1.395(6) . ? C30 H30A 0.9300 . ? C31 C32 1.378(6) . ? C32 C33 1.383(6) . ? C32 H32A 0.9300 . ? C33 C34 1.378(6) . ? C33 N6 1.471(6) . ? C34 H34A 0.9300 . ? N1 Cd2 2.230(4) . ? N3 Cd1 2.220(4) . ? N5 O5 1.198(6) . ? N5 O6 1.210(6) . ? N6 O11 1.191(6) . ? N6 O12 1.202(6) . ? O1 Cd2 2.358(3) . ? O2 Cd2 2.459(3) . ? O2 Cd1 2.553(3) . ? O3 Cd1 2.253(3) 2_766 ? O7 Cd1 2.305(3) . ? O7 Cd2 2.486(3) . ? O8 Cd1 2.541(3) . ? O9 Cd2 2.216(3) 2_676 ? O13 Cd2 2.342(3) . ? O13 H13A 0.7746 . ? O13 H13B 0.8755 . ? O14 Cd1 2.320(3) . ? O14 H14C 0.9604 . ? O14 H14B 0.7229 . ? O15 H15C 0.8200 . ? O15 H15B 0.8201 . ? O16 H16A 0.8509 . ? O16 H16B 0.8201 . ? Cd1 O3 2.253(3) 2_766 ? Cd1 H14B 1.8707 . ? Cd2 O9 2.216(3) 2_676 ? 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 C2 C1 N1 110.0(4) . . ? C2 C1 H1A 125.0 . . ? N1 C1 H1A 125.0 . . ? C1 C2 N2 106.4(4) . . ? C1 C2 H2A 126.8 . . ? N2 C2 H2A 126.8 . . ? N1 C3 N2 111.3(4) . . ? N1 C3 H3A 124.4 . . ? N2 C3 H3A 124.4 . . ? C9 C4 C5 118.9(4) . . ? C9 C4 N2 121.5(4) . . ? C5 C4 N2 119.5(4) . . ? C4 C5 C6 120.0(5) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 121.8(5) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 117.0(4) . . ? C6 C7 C7 121.3(5) . 2_575 ? C8 C7 C7 121.7(5) . 2_575 ? C7 C8 C9 122.0(5) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C4 C9 C8 120.2(5) . . ? C4 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C15 C10 C11 116.8(4) . . ? C15 C10 C10 122.1(5) . 2_865 ? C11 C10 C10 121.1(5) . 2_865 ? C12 C11 C10 121.5(4) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C13 C12 C11 120.8(5) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C14 C13 C12 119.0(4) . . ? C14 C13 N4 120.9(4) . . ? C12 C13 N4 120.0(4) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C10 C15 C14 122.1(5) . . ? C10 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C17 C16 N4 107.0(4) . . ? C17 C16 H16C 126.5 . . ? N4 C16 H16C 126.5 . . ? C16 C17 N3 109.6(4) . . ? C16 C17 H17A 125.2 . . ? N3 C17 H17A 125.2 . . ? N3 C18 N4 111.8(4) . . ? N3 C18 H18A 124.1 . . ? N4 C18 H18A 124.1 . . ? O1 C19 O2 121.8(4) . . ? O1 C19 C21 119.0(4) . . ? O2 C19 C21 119.1(4) . . ? O1 C19 Cd2 58.6(2) . . ? O2 C19 Cd2 63.2(2) . . ? C21 C19 Cd2 177.1(4) . . ? O4 C20 O3 121.8(4) . . ? O4 C20 C23 121.4(4) . . ? O3 C20 C23 116.8(4) . . ? C26 C21 C22 119.5(4) . . ? C26 C21 C19 119.0(4) . . ? C22 C21 C19 121.4(4) . . ? C21 C22 C23 121.2(4) . . ? C21 C22 H22A 119.4 . . ? C23 C22 H22A 119.4 . . ? C24 C23 C22 119.4(4) . . ? C24 C23 C20 119.9(4) . . ? C22 C23 C20 120.6(4) . . ? C25 C24 C23 118.5(4) . . ? C25 C24 H24A 120.8 . . ? C23 C24 H24A 120.8 . . ? C24 C25 C26 123.5(4) . . ? C24 C25 N5 118.0(4) . . ? C26 C25 N5 118.4(4) . . ? C25 C26 C21 117.8(4) . . ? C25 C26 H26A 121.1 . . ? C21 C26 H26A 121.1 . . ? O8 C27 O7 122.5(4) . . ? O8 C27 C29 121.4(4) . . ? O7 C27 C29 116.1(4) . . ? O10 C28 O9 122.5(4) . . ? O10 C28 C31 121.1(4) . . ? O9 C28 C31 116.3(4) . . ? C34 C29 C30 119.9(4) . . ? C34 C29 C27 120.3(4) . . ? C30 C29 C27 119.8(4) . . ? C29 C30 C31 120.7(4) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C32 C31 C30 119.5(4) . . ? C32 C31 C28 120.4(4) . . ? C30 C31 C28 120.1(4) . . ? C31 C32 C33 118.5(4) . . ? C31 C32 H32A 120.8 . . ? C33 C32 H32A 120.8 . . ? C34 C33 C32 123.1(4) . . ? C34 C33 N6 119.1(4) . . ? C32 C33 N6 117.8(4) . . ? C33 C34 C29 118.2(4) . . ? C33 C34 H34A 120.9 . . ? C29 C34 H34A 120.9 . . ? C3 N1 C1 105.9(4) . . ? C3 N1 Cd2 126.0(3) . . ? C1 N1 Cd2 128.1(3) . . ? C3 N2 C2 106.4(4) . . ? C3 N2 C4 125.6(4) . . ? C2 N2 C4 127.4(4) . . ? C18 N3 C17 105.7(4) . . ? C18 N3 Cd1 124.9(3) . . ? C17 N3 Cd1 128.6(3) . . ? C18 N4 C16 105.9(4) . . ? C18 N4 C13 125.7(4) . . ? C16 N4 C13 128.2(4) . . ? O5 N5 O6 122.0(5) . . ? O5 N5 C25 119.1(5) . . ? O6 N5 C25 118.9(4) . . ? O11 N6 O12 122.3(5) . . ? O11 N6 C33 119.4(4) . . ? O12 N6 C33 118.3(4) . . ? C19 O1 Cd2 94.4(3) . . ? C19 O2 Cd2 89.6(3) . . ? C19 O2 Cd1 111.8(3) . . ? Cd2 O2 Cd1 102.46(12) . . ? C20 O3 Cd1 104.7(3) . 2_766 ? C27 O7 Cd1 96.6(3) . . ? C27 O7 Cd2 116.9(3) . . ? Cd1 O7 Cd2 109.26(12) . . ? C27 O8 Cd1 86.9(3) . . ? C28 O9 Cd2 107.8(3) . 2_676 ? Cd2 O13 H13A 95.5 . . ? Cd2 O13 H13B 103.6 . . ? H13A O13 H13B 108.8 . . ? Cd1 O14 H14C 115.1 . . ? Cd1 O14 H14B 44.1 . . ? H14C O14 H14B 92.8 . . ? H15C O15 H15B 110.0 . . ? H16A O16 H16B 143.6 . . ? N3 Cd1 O3 135.65(13) . 2_766 ? N3 Cd1 O7 137.16(13) . . ? O3 Cd1 O7 82.69(12) 2_766 . ? N3 Cd1 O14 95.33(13) . . ? O3 Cd1 O14 90.47(13) 2_766 . ? O7 Cd1 O14 103.93(12) . . ? N3 Cd1 O8 93.88(13) . . ? O3 Cd1 O8 130.35(12) 2_766 . ? O7 Cd1 O8 53.82(11) . . ? O14 Cd1 O8 79.70(12) . . ? N3 Cd1 O2 86.94(13) . . ? O3 Cd1 O2 87.40(12) 2_766 . ? O7 Cd1 O2 74.74(11) . . ? O14 Cd1 O2 177.62(11) . . ? O8 Cd1 O2 100.88(11) . . ? N3 Cd1 H14B 110.8 . . ? O3 Cd1 H14B 78.1 2_766 . ? O7 Cd1 H14B 92.7 . . ? O14 Cd1 H14B 15.6 . . ? O8 Cd1 H14B 81.0 . . ? O2 Cd1 H14B 162.0 . . ? O9 Cd2 N1 130.55(12) 2_676 . ? O9 Cd2 O13 92.38(13) 2_676 . ? N1 Cd2 O13 91.79(13) . . ? O9 Cd2 O1 84.41(13) 2_676 . ? N1 Cd2 O1 144.96(13) . . ? O13 Cd2 O1 83.26(12) . . ? O9 Cd2 O2 130.28(11) 2_676 . ? N1 Cd2 O2 95.02(12) . . ? O13 Cd2 O2 106.76(11) . . ? O1 Cd2 O2 54.21(11) . . ? O9 Cd2 O7 89.17(12) 2_676 . ? N1 Cd2 O7 85.94(12) . . ? O13 Cd2 O7 177.73(10) . . ? O1 Cd2 O7 98.55(12) . . ? O2 Cd2 O7 73.39(11) . . ? O9 Cd2 C19 108.10(14) 2_676 . ? N1 Cd2 C19 120.54(14) . . ? O13 Cd2 C19 95.05(12) . . ? O1 Cd2 C19 26.99(13) . . ? O2 Cd2 C19 27.22(13) . . ? O7 Cd2 C19 86.04(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13B O16 0.88 1.89 2.724(5) 158.0 . O13 H13A O4 0.77 2.16 2.715(5) 129.2 2_666 O14 H14C O10 0.96 1.86 2.724(4) 147.8 2_776 O15 H15B O9 0.82 2.06 2.780(5) 146.4 2_676 O16 H16A O5 0.85 2.61 3.458(9) 179.3 1_455 O16 H16B O1 0.82 2.21 2.941(6) 148.4 2_666 O14 H14B O3 0.72 2.62 3.248(5) 147.3 2_766 O15 H15C O3 0.82 2.31 2.946(5) 134.7 2_766 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.918 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.097 data_[Cd(5-SO3-1,3-BDC)(bimb)]n _database_code_depnum_ccdc_archive 'CCDC 874185' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd N4 O7 S' _chemical_formula_sum 'C26 H18 Cd N4 O7 S' _chemical_formula_weight 642.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.425(6) _cell_length_b 9.4342(19) _cell_length_c 20.233(4) _cell_angle_alpha 90.00 _cell_angle_beta 123.71(3) _cell_angle_gamma 90.00 _cell_volume 4672.2(23) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7268 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5625 _exptl_absorpt_correction_T_max 0.7370 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21883 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4274 _reflns_number_gt 3749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0396P)^2^+13.0301P] 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 4274 _refine_ls_number_parameters 356 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.14805(17) 0.5724(4) 0.1773(2) 0.0344(9) Uani 1 1 d . . . H1A H 0.1689 0.5191 0.2234 0.041 Uiso 1 1 calc R . . C2 C 0.10803(17) 0.5204(4) 0.1061(2) 0.0365(10) Uani 1 1 d . . . H2A H 0.0966 0.4265 0.0941 0.044 Uiso 1 1 calc R . . C3 C 0.11602(15) 0.7484(4) 0.0969(2) 0.0296(9) Uani 1 1 d . . . H3A H 0.1101 0.8393 0.0759 0.035 Uiso 1 1 calc R . . C4 C 0.04429(15) 0.6317(4) -0.0283(2) 0.0278(8) Uani 1 1 d . . . C5 C 0.03769(16) 0.5136(4) -0.0732(2) 0.0348(9) Uani 1 1 d . . . H5A H 0.0602 0.4350 -0.0498 0.042 Uiso 1 1 calc R . . C6 C -0.00324(17) 0.5139(4) -0.1541(2) 0.0368(10) Uani 1 1 d . . . H6A H -0.0081 0.4343 -0.1845 0.044 Uiso 1 1 calc R . . C7 C -0.03686(15) 0.6308(4) -0.1902(2) 0.0298(9) Uani 1 1 d . . . C8 C -0.02955(16) 0.7467(4) -0.1433(2) 0.0318(9) Uani 1 1 d . . . H8A H -0.0519 0.8256 -0.1664 0.038 Uiso 1 1 calc R . . C9 C 0.01067(16) 0.7472(4) -0.0620(2) 0.0319(9) Uani 1 1 d . . . H9A H 0.0147 0.8251 -0.0310 0.038 Uiso 1 1 calc R . . C10 C -0.07946(16) 0.6339(4) -0.2773(2) 0.0306(9) Uani 1 1 d . . . C11 C -0.11256(17) 0.5167(4) -0.3151(2) 0.0352(10) Uani 1 1 d . . . H11A H -0.1080 0.4356 -0.2858 0.042 Uiso 1 1 calc R . . C12 C -0.15233(16) 0.5193(4) -0.3960(2) 0.0317(9) Uani 1 1 d . . . H12A H -0.1751 0.4415 -0.4206 0.038 Uiso 1 1 calc R . . C13 C -0.15791(15) 0.6383(4) -0.4400(2) 0.0267(8) Uani 1 1 d . . . C14 C -0.12551(16) 0.7556(4) -0.4039(2) 0.0325(9) Uani 1 1 d . . . H14A H -0.1294 0.8354 -0.4336 0.039 Uiso 1 1 calc R . . C15 C -0.08689(17) 0.7529(4) -0.3222(2) 0.0362(10) Uani 1 1 d . . . H15A H -0.0656 0.8328 -0.2973 0.043 Uiso 1 1 calc R . . C16 C -0.23055(16) 0.7460(4) -0.5710(2) 0.0327(9) Uani 1 1 d . . . H16A H -0.2299 0.8391 -0.5554 0.039 Uiso 1 1 calc R . . C17 C -0.26385(16) 0.6916(4) -0.6449(2) 0.0313(9) Uani 1 1 d . . . H17A H -0.2905 0.7422 -0.6891 0.038 Uiso 1 1 calc R . . C18 C -0.21241(16) 0.5213(4) -0.5709(2) 0.0313(9) Uani 1 1 d . . . H18A H -0.1962 0.4326 -0.5535 0.038 Uiso 1 1 calc R . . C19 C 0.50164(15) 0.6091(4) 0.6171(2) 0.0281(8) Uani 1 1 d . . . C20 C 0.33968(15) 0.6582(4) 0.6363(2) 0.0257(8) Uani 1 1 d . . . C21 C 0.35088(15) 0.6272(4) 0.45919(19) 0.0247(8) Uani 1 1 d . . . C22 C 0.32878(14) 0.6440(4) 0.5041(2) 0.0255(8) Uani 1 1 d . . . H22A H 0.2912 0.6537 0.4791 0.031 Uiso 1 1 calc R . . C23 C 0.36319(14) 0.6462(4) 0.5868(2) 0.0233(8) Uani 1 1 d . . . C24 C 0.41911(15) 0.6357(4) 0.6226(2) 0.0256(8) Uani 1 1 d . . . H24A H 0.4423 0.6382 0.6777 0.031 Uiso 1 1 calc R . . C25 C 0.44122(14) 0.6214(4) 0.5775(2) 0.0241(8) Uani 1 1 d . . . C26 C 0.40648(15) 0.6153(4) 0.4948(2) 0.0255(8) Uani 1 1 d . . . H26A H 0.4207 0.6032 0.4641 0.031 Uiso 1 1 calc R . . N1 N 0.15339(12) 0.7160(3) 0.17148(17) 0.0261(7) Uani 1 1 d . . . N2 N 0.08748(12) 0.6338(3) 0.05482(17) 0.0264(7) Uani 1 1 d . . . N3 N -0.25233(12) 0.5506(3) -0.64464(17) 0.0268(7) Uani 1 1 d . . . N4 N -0.19799(12) 0.6365(3) -0.52385(17) 0.0265(7) Uani 1 1 d . . . O1 O 0.52804(13) 0.6284(5) 0.69396(18) 0.0708(14) Uani 1 1 d . . . H1B H 0.558(3) 0.620(6) 0.716(4) 0.08(2) Uiso 1 1 d . . . O2 O 0.52333(11) 0.5819(3) 0.58335(16) 0.0373(7) Uani 1 1 d . . . O3 O 0.36809(10) 0.6115(3) 0.70754(14) 0.0326(6) Uani 1 1 d . . . O4 O 0.29361(11) 0.7098(3) 0.60723(16) 0.0352(7) Uani 1 1 d . . . O5 O 0.28668(10) 0.7613(3) 0.32756(14) 0.0298(6) Uani 1 1 d . . . O6 O 0.26280(15) 0.5219(4) 0.33645(19) 0.0784(13) Uani 1 1 d . . . O7 O 0.16106(14) 1.0654(4) 0.17341(16) 0.0631(11) Uani 1 1 d U . . S1 S 0.30613(4) 0.61837(10) 0.35374(5) 0.0314(2) Uani 1 1 d . . . Cd1 Cd 0.202008(10) 0.87338(3) 0.268947(14) 0.02391(11) Uani 1 1 d U . . 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 0.036(2) 0.037(2) 0.0183(19) 0.0048(17) 0.0077(18) 0.0029(19) C2 0.040(2) 0.030(2) 0.026(2) 0.0002(18) 0.0096(18) -0.0075(19) C3 0.026(2) 0.031(2) 0.0196(18) -0.0049(16) 0.0053(16) -0.0034(17) C4 0.028(2) 0.031(2) 0.0167(17) -0.0040(16) 0.0079(16) -0.0041(17) C5 0.038(2) 0.028(2) 0.024(2) -0.0014(17) 0.0081(18) 0.0031(18) C6 0.041(2) 0.032(2) 0.024(2) -0.0079(18) 0.0098(19) -0.0029(19) C7 0.029(2) 0.036(2) 0.0143(17) -0.0033(16) 0.0056(16) -0.0045(17) C8 0.031(2) 0.031(2) 0.0219(19) -0.0010(17) 0.0074(17) 0.0033(17) C9 0.033(2) 0.034(2) 0.0218(19) -0.0090(17) 0.0103(17) -0.0003(18) C10 0.036(2) 0.032(2) 0.0190(18) -0.0028(17) 0.0130(17) -0.0003(18) C11 0.045(2) 0.031(2) 0.0192(19) -0.0009(17) 0.0106(18) -0.0073(19) C12 0.036(2) 0.029(2) 0.0192(18) -0.0044(17) 0.0091(17) -0.0104(18) C13 0.028(2) 0.030(2) 0.0158(17) -0.0052(16) 0.0083(16) -0.0025(16) C14 0.037(2) 0.027(2) 0.0220(19) 0.0009(17) 0.0087(17) -0.0053(18) C15 0.040(2) 0.030(2) 0.024(2) -0.0090(17) 0.0087(18) -0.0113(19) C16 0.042(2) 0.025(2) 0.023(2) 0.0004(16) 0.0128(18) 0.0010(18) C17 0.031(2) 0.031(2) 0.0228(19) 0.0021(16) 0.0092(17) 0.0060(18) C18 0.035(2) 0.0257(19) 0.0202(19) -0.0035(16) 0.0074(17) 0.0015(17) C19 0.0254(19) 0.038(2) 0.0177(18) -0.0010(17) 0.0100(16) -0.0027(17) C20 0.0229(19) 0.029(2) 0.0238(19) -0.0027(16) 0.0119(16) -0.0052(16) C21 0.0271(19) 0.0248(18) 0.0114(16) -0.0012(15) 0.0041(15) 0.0020(16) C22 0.0172(17) 0.028(2) 0.0208(18) 0.0039(16) 0.0041(15) 0.0037(15) C23 0.0217(18) 0.0267(19) 0.0190(17) 0.0026(15) 0.0098(15) -0.0005(15) C24 0.0233(18) 0.033(2) 0.0141(16) 0.0000(16) 0.0062(15) 0.0009(16) C25 0.0204(18) 0.032(2) 0.0152(17) -0.0025(16) 0.0073(15) -0.0012(16) C26 0.0261(19) 0.031(2) 0.0159(17) -0.0038(16) 0.0093(15) -0.0005(16) N1 0.0229(16) 0.0331(17) 0.0178(15) -0.0045(13) 0.0085(13) 0.0001(14) N2 0.0250(16) 0.0291(17) 0.0163(15) -0.0013(13) 0.0059(13) -0.0005(14) N3 0.0276(16) 0.0290(17) 0.0149(15) -0.0031(13) 0.0062(13) -0.0019(14) N4 0.0272(16) 0.0287(17) 0.0146(14) -0.0030(13) 0.0058(13) -0.0038(14) O1 0.0195(16) 0.165(5) 0.0163(15) -0.018(2) 0.0027(13) 0.011(2) O2 0.0305(15) 0.0577(19) 0.0275(14) 0.0003(14) 0.0183(13) 0.0006(14) O3 0.0218(13) 0.0556(18) 0.0180(13) 0.0044(12) 0.0095(11) -0.0007(13) O4 0.0271(15) 0.0458(17) 0.0381(16) 0.0102(14) 0.0215(13) 0.0079(13) O5 0.0315(14) 0.0280(14) 0.0194(13) 0.0041(11) 0.0077(11) 0.0093(12) O6 0.071(2) 0.055(2) 0.0355(18) 0.0088(16) -0.0162(17) -0.034(2) O7 0.060(2) 0.087(2) 0.0137(14) 0.0138(14) 0.0024(14) -0.0431(18) S1 0.0335(5) 0.0291(5) 0.0125(4) -0.0017(4) 0.0009(4) 0.0071(4) Cd1 0.02074(16) 0.03120(17) 0.01522(15) -0.00375(11) 0.00713(12) -0.00325(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.349(5) . ? C1 N1 1.377(5) . ? C1 H1A 0.9300 . ? C2 N2 1.375(5) . ? C2 H2A 0.9300 . ? C3 N1 1.319(5) . ? C3 N2 1.343(5) . ? C3 H3A 0.9300 . ? C4 C9 1.372(5) . ? C4 C5 1.382(5) . ? C4 N2 1.439(4) . ? C5 C6 1.393(5) . ? C5 H5A 0.9300 . ? C6 C7 1.388(6) . ? C6 H6A 0.9300 . ? C7 C8 1.384(5) . ? C7 C10 1.492(5) . ? C8 C9 1.394(5) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.383(6) . ? C10 C11 1.389(5) . ? C11 C12 1.387(5) . ? C11 H11A 0.9300 . ? C12 C13 1.384(5) . ? C12 H12A 0.9300 . ? C13 C14 1.376(5) . ? C13 N4 1.432(4) . ? C14 C15 1.392(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.353(5) . ? C16 N4 1.372(5) . ? C16 H16A 0.9300 . ? C17 N3 1.372(5) . ? C17 H17A 0.9300 . ? C18 N3 1.318(5) . ? C18 N4 1.349(5) . ? C18 H18A 0.9300 . ? C19 O2 1.193(4) . ? C19 O1 1.310(5) . ? C19 C25 1.495(5) . ? C20 O4 1.239(4) . ? C20 O3 1.279(4) . ? C20 C23 1.503(5) . ? C21 C26 1.378(5) . ? C21 C22 1.389(5) . ? C21 S1 1.782(3) . ? C22 C23 1.395(5) . ? C22 H22A 0.9300 . ? C23 C24 1.386(5) . ? C24 C25 1.391(5) . ? C24 H24A 0.9300 . ? C25 C26 1.395(5) . ? C26 H26A 0.9300 . ? N1 Cd1 2.238(3) . ? N3 Cd1 2.247(3) 3_444 ? O1 H1B 0.73(6) . ? O3 Cd1 2.364(3) 7_566 ? O4 Cd1 2.559(3) 7_566 ? O5 S1 1.446(3) . ? O5 Cd1 2.335(3) . ? O6 S1 1.442(4) . ? O7 S1 1.439(3) 4 ? O7 Cd1 2.426(3) . ? S1 O7 1.439(3) 4_545 ? Cd1 N3 2.247(3) 3_556 ? Cd1 O3 2.364(3) 7_566 ? Cd1 O4 2.559(3) 7_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 109.9(3) . . ? C2 C1 H1A 125.1 . . ? N1 C1 H1A 125.1 . . ? C1 C2 N2 106.3(3) . . ? C1 C2 H2A 126.9 . . ? N2 C2 H2A 126.9 . . ? N1 C3 N2 111.7(3) . . ? N1 C3 H3A 124.2 . . ? N2 C3 H3A 124.2 . . ? C9 C4 C5 120.9(3) . . ? C9 C4 N2 119.8(3) . . ? C5 C4 N2 119.3(3) . . ? C4 C5 C6 119.0(4) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C10 120.3(4) . . ? C6 C7 C10 121.6(3) . . ? C7 C8 C9 121.3(4) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C4 C9 C8 119.3(4) . . ? C4 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C15 C10 C11 118.6(3) . . ? C15 C10 C7 121.0(4) . . ? C11 C10 C7 120.5(4) . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 N4 120.7(3) . . ? C12 C13 N4 118.5(3) . . ? C13 C14 C15 118.9(4) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C10 C15 C14 121.5(4) . . ? C10 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C17 C16 N4 106.3(3) . . ? C17 C16 H16A 126.8 . . ? N4 C16 H16A 126.8 . . ? C16 C17 N3 109.7(3) . . ? C16 C17 H17A 125.1 . . ? N3 C17 H17A 125.1 . . ? N3 C18 N4 111.3(3) . . ? N3 C18 H18A 124.3 . . ? N4 C18 H18A 124.3 . . ? O2 C19 O1 123.8(4) . . ? O2 C19 C25 124.4(3) . . ? O1 C19 C25 111.8(3) . . ? O4 C20 O3 121.9(3) . . ? O4 C20 C23 120.1(3) . . ? O3 C20 C23 118.0(3) . . ? C26 C21 C22 121.2(3) . . ? C26 C21 S1 119.7(3) . . ? C22 C21 S1 119.0(3) . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 C20 120.7(3) . . ? C22 C23 C20 120.3(3) . . ? C23 C24 C25 121.1(3) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C24 C25 C26 119.5(3) . . ? C24 C25 C19 120.4(3) . . ? C26 C25 C19 120.1(3) . . ? C21 C26 C25 119.4(3) . . ? C21 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C3 N1 C1 105.3(3) . . ? C3 N1 Cd1 125.1(3) . . ? C1 N1 Cd1 128.7(2) . . ? C3 N2 C2 106.8(3) . . ? C3 N2 C4 126.0(3) . . ? C2 N2 C4 127.2(3) . . ? C18 N3 C17 105.7(3) . . ? C18 N3 Cd1 119.8(3) . 3_444 ? C17 N3 Cd1 132.7(2) . 3_444 ? C18 N4 C16 106.9(3) . . ? C18 N4 C13 125.1(3) . . ? C16 N4 C13 127.9(3) . . ? C19 O1 H1B 115(5) . . ? C20 O3 Cd1 96.3(2) . 7_566 ? C20 O4 Cd1 88.2(2) . 7_566 ? S1 O5 Cd1 134.59(16) . . ? S1 O7 Cd1 114.9(2) 4 . ? O7 S1 O6 112.2(3) 4_545 . ? O7 S1 O5 113.4(2) 4_545 . ? O6 S1 O5 112.5(2) . . ? O7 S1 C21 105.48(17) 4_545 . ? O6 S1 C21 106.64(19) . . ? O5 S1 C21 105.91(16) . . ? N1 Cd1 N3 173.19(11) . 3_556 ? N1 Cd1 O5 97.31(10) . . ? N3 Cd1 O5 86.16(10) 3_556 . ? N1 Cd1 O3 90.85(10) . 7_566 ? N3 Cd1 O3 90.59(11) 3_556 7_566 ? O5 Cd1 O3 136.82(9) . 7_566 ? N1 Cd1 O7 90.08(11) . . ? N3 Cd1 O7 83.25(11) 3_556 . ? O5 Cd1 O7 131.36(11) . . ? O3 Cd1 O7 90.71(11) 7_566 . ? N1 Cd1 O4 108.63(10) . 7_566 ? N3 Cd1 O4 77.46(10) 3_556 7_566 ? O5 Cd1 O4 84.51(9) . 7_566 ? O3 Cd1 O4 52.92(9) 7_566 7_566 ? O7 Cd1 O4 137.88(11) . 7_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O3 0.73(6) 1.85(6) 2.565(4) 165(7) 2_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.725 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.081