data_33 _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Cd(2,2'-biim)(4,4'-bipy)(H2O)(ClO4)]nn(ClO4)' ; _chemical_name_common '[Cd(2,2'-biim)(4,4'-bipy)(H2O)(ClO4)]nn(ClO4)' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Cd(2,2'-biim)(4,4'-bipy)(H2O)(ClO4)]nn(ClO4)' _chemical_formula_sum 'C16 H16 Cd Cl2 N6 O9' _chemical_formula_weight 619.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 2(1)' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 17.7584(5) _cell_length_b 9.8785(3) _cell_length_c 12.3847(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2172.60(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4159 _cell_measurement_theta_min 3.9960 _cell_measurement_theta_max 28.4420 _exptl_crystal_description block _exptl_crystal_colour 'light-yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'micro-focus sealed X-ray tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova (Mo) X-ray Source' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.0894 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6691 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3304 _reflns_number_gt 3118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.0257P] 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 theo _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 3304 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.011831(12) 0.21793(2) 0.87890(4) 0.03008(9) Uani 1 1 d . . . Cl1 Cl -0.21641(6) 0.43998(10) 0.34828(10) 0.0417(3) Uani 1 1 d . . . Cl2 Cl 0.05075(7) 0.37759(12) 0.62752(11) 0.0484(3) Uani 1 1 d . . . O1 O -0.2219(2) 0.5584(3) 0.4120(3) 0.0688(12) Uani 1 1 d . . . O2 O -0.13943(17) 0.3958(4) 0.3482(4) 0.0679(12) Uani 1 1 d . . . O3 O -0.2604(2) 0.3340(4) 0.3925(5) 0.0854(14) Uani 1 1 d . . . O4 O -0.2395(2) 0.4660(4) 0.2406(3) 0.0748(12) Uani 1 1 d . . . O5 O 0.0218(2) 0.5090(5) 0.6496(4) 0.0803(16) Uani 1 1 d . . . O6 O -0.0033(3) 0.3050(7) 0.5706(6) 0.112(2) Uani 1 1 d . . . O7 O 0.0659(2) 0.3099(4) 0.7276(3) 0.0567(10) Uani 1 1 d . . . O8 O 0.1181(3) 0.3871(4) 0.5673(4) 0.0821(14) Uani 1 1 d . . . O1W O 0.0450(2) 0.4017(3) 0.9569(3) 0.0624(11) Uani 1 1 d . . . H1WA H 0.0225 0.4221 1.0124 0.094 Uiso 1 1 calc R . . N1 N 0.15572(18) -0.0930(4) 0.9294(3) 0.0404(9) Uani 1 1 d . . . H1B H 0.1661 -0.1771 0.9192 0.049 Uiso 1 1 calc R . . N2 N 0.09597(17) 0.1000(3) 0.9214(3) 0.0319(8) Uani 1 1 d . . . N3 N 0.0269(2) -0.2001(4) 0.7794(4) 0.0381(9) Uani 1 1 d . . . H3A H 0.0573 -0.2673 0.7870 0.046 Uiso 1 1 calc R . . N4 N -0.02179(17) 0.0024(4) 0.7960(3) 0.0331(8) Uani 1 1 d . . . N5 N -0.38882(18) -0.1632(4) 1.3088(3) 0.0357(9) Uani 1 1 d . . . N6 N -0.08998(17) 0.1489(3) 1.0222(3) 0.0302(8) Uani 1 1 d . . . C1 C 0.1978(2) -0.0023(5) 0.9865(4) 0.0450(12) Uani 1 1 d . . . H1A H 0.2428 -0.0192 1.0224 0.054 Uiso 1 1 calc R . . C2 C 0.1609(2) 0.1169(5) 0.9807(4) 0.0405(11) Uani 1 1 d . . . H2A H 0.1767 0.1976 1.0118 0.049 Uiso 1 1 calc R . . C3 C 0.09485(18) -0.0264(4) 0.8918(4) 0.0311(9) Uani 1 1 d . . . C4 C 0.0344(2) -0.0765(4) 0.8243(4) 0.0318(10) Uani 1 1 d . . . C5 C -0.0380(3) -0.1992(5) 0.7194(5) 0.0434(12) Uani 1 1 d . . . H5A H -0.0577 -0.2703 0.6792 0.052 Uiso 1 1 calc R . . C6 C -0.0670(2) -0.0747(5) 0.7309(4) 0.0453(12) Uani 1 1 d . . . H6A H -0.1115 -0.0449 0.6991 0.054 Uiso 1 1 calc R . . C7 C -0.0900(2) 0.0182(5) 1.0477(4) 0.0405(12) Uani 1 1 d . . . H7A H -0.0505 -0.0349 1.0225 0.049 Uiso 1 1 calc R . . C8 C -0.1445(2) -0.0433(4) 1.1089(4) 0.0393(11) Uani 1 1 d . . . H8A H -0.1417 -0.1356 1.1231 0.047 Uiso 1 1 calc R . . C9 C -0.2039(2) 0.0325(4) 1.1497(3) 0.0267(9) Uani 1 1 d . . . C10 C -0.2015(2) 0.1705(4) 1.1297(3) 0.0296(9) Uani 1 1 d . . . H10A H -0.2379 0.2275 1.1588 0.036 Uiso 1 1 calc R . . C11 C -0.1445(3) 0.2226(4) 1.0659(4) 0.0341(11) Uani 1 1 d . . . H11A H -0.1445 0.3153 1.0528 0.041 Uiso 1 1 calc R . . C12 C -0.3357(3) -0.2318(5) 1.2564(7) 0.068(2) Uani 1 1 d . . . H12A H -0.3398 -0.3255 1.2536 0.081 Uiso 1 1 calc R . . C13 C -0.2749(3) -0.1725(5) 1.2063(5) 0.0611(18) Uani 1 1 d . . . H13A H -0.2396 -0.2259 1.1709 0.073 Uiso 1 1 calc R . . C14 C -0.2666(2) -0.0347(4) 1.2084(4) 0.0297(9) Uani 1 1 d . . . C15 C -0.3205(2) 0.0363(4) 1.2663(4) 0.0377(11) Uani 1 1 d . . . H15A H -0.3164 0.1298 1.2730 0.045 Uiso 1 1 calc R . . C16 C -0.3800(2) -0.0301(4) 1.3140(4) 0.0365(11) Uani 1 1 d . . . H16A H -0.4155 0.0206 1.3515 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02799(13) 0.02701(15) 0.03525(16) 0.0040(2) 0.0010(2) 0.00381(10) Cl1 0.0395(5) 0.0324(5) 0.0531(8) -0.0090(6) 0.0005(5) 0.0067(4) Cl2 0.0617(7) 0.0447(7) 0.0386(6) 0.0085(6) 0.0067(6) 0.0195(6) O1 0.089(2) 0.0474(19) 0.070(3) -0.028(2) 0.011(2) 0.0150(18) O2 0.0474(16) 0.065(2) 0.091(4) -0.012(2) 0.000(2) 0.0217(16) O3 0.082(2) 0.060(2) 0.114(4) 0.006(3) 0.032(3) -0.0246(19) O4 0.100(3) 0.071(3) 0.054(3) -0.010(2) -0.027(2) 0.025(2) O5 0.115(4) 0.054(2) 0.072(4) 0.010(3) 0.013(3) 0.045(3) O6 0.101(4) 0.119(5) 0.114(5) -0.023(4) -0.032(4) 0.010(3) O7 0.068(2) 0.058(2) 0.044(2) 0.0234(19) 0.0203(19) 0.0247(19) O8 0.091(3) 0.086(3) 0.069(3) 0.030(3) 0.045(3) 0.023(2) O1W 0.064(2) 0.051(2) 0.072(3) -0.029(2) 0.027(2) -0.0182(18) N1 0.0375(18) 0.041(2) 0.043(2) 0.003(2) -0.0054(18) 0.0136(17) N2 0.0307(16) 0.0345(19) 0.0306(19) 0.0031(17) -0.0007(15) 0.0005(15) N3 0.0391(19) 0.029(2) 0.046(3) -0.005(2) 0.004(2) 0.0043(15) N4 0.0287(16) 0.0328(19) 0.038(2) -0.0044(19) -0.0032(17) 0.0042(15) N5 0.0324(18) 0.0312(19) 0.044(2) 0.007(2) 0.0006(17) -0.0045(16) N6 0.0287(17) 0.0317(19) 0.0303(19) 0.0026(18) 0.0036(15) 0.0021(15) C1 0.037(2) 0.062(3) 0.036(3) 0.002(3) -0.006(2) 0.013(2) C2 0.034(2) 0.049(3) 0.038(3) -0.005(2) -0.005(2) 0.000(2) C3 0.0298(16) 0.0311(19) 0.032(3) 0.006(2) 0.005(2) 0.0080(15) C4 0.0322(19) 0.032(2) 0.032(2) -0.004(2) 0.0032(19) 0.0046(18) C5 0.037(2) 0.039(3) 0.054(3) -0.016(3) 0.001(2) 0.000(2) C6 0.033(2) 0.051(3) 0.052(3) -0.015(3) -0.007(2) 0.004(2) C7 0.037(2) 0.038(3) 0.047(3) 0.011(3) 0.010(2) 0.009(2) C8 0.042(2) 0.027(2) 0.048(3) 0.008(2) 0.013(2) 0.012(2) C9 0.0253(18) 0.026(2) 0.028(2) 0.000(2) -0.0021(17) -0.0016(17) C10 0.029(2) 0.026(2) 0.034(2) 0.000(2) 0.0042(19) 0.0057(17) C11 0.035(2) 0.031(2) 0.036(3) 0.004(2) -0.001(2) -0.0064(19) C12 0.047(3) 0.029(3) 0.127(6) -0.001(4) 0.036(4) -0.003(2) C13 0.055(3) 0.028(2) 0.100(5) -0.009(3) 0.034(3) -0.001(2) C14 0.0263(19) 0.031(2) 0.032(2) 0.000(2) -0.0053(19) -0.0009(18) C15 0.033(2) 0.026(2) 0.055(3) -0.004(2) 0.007(2) -0.0009(18) C16 0.037(2) 0.032(2) 0.040(3) -0.008(2) 0.007(2) -0.0011(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.290(3) 4_454 ? Cd1 O1W 2.291(3) . ? Cd1 N2 2.302(3) . ? Cd1 N6 2.354(3) . ? Cd1 N4 2.370(4) . ? Cd1 O7 2.499(3) . ? Cl1 O1 1.415(3) . ? Cl1 O3 1.417(4) . ? Cl1 O4 1.418(4) . ? Cl1 O2 1.435(3) . ? Cl2 O6 1.390(6) . ? Cl2 O8 1.412(4) . ? Cl2 O5 1.423(5) . ? Cl2 O7 1.433(4) . ? O1W H1WA 0.8200 . ? N1 C3 1.348(5) . ? N1 C1 1.364(6) . ? N1 H1B 0.8600 . ? N2 C3 1.301(5) . ? N2 C2 1.376(5) . ? N3 C4 1.349(5) . ? N3 C5 1.371(7) . ? N3 H3A 0.8600 . ? N4 C4 1.315(5) . ? N4 C6 1.369(6) . ? N5 C16 1.326(5) . ? N5 C12 1.330(6) . ? N5 Cd1 2.290(3) 4_445 ? N6 C11 1.328(6) . ? N6 C7 1.329(6) . ? C1 C2 1.349(6) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.447(6) . ? C5 C6 1.342(7) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.372(6) . ? C7 H7A 0.9300 . ? C8 C9 1.389(5) . ? C8 H8A 0.9300 . ? C9 C10 1.386(5) . ? C9 C14 1.487(6) . ? C10 C11 1.383(6) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.375(7) . ? C12 H12A 0.9300 . ? C13 C14 1.369(6) . ? C13 H13A 0.9300 . ? C14 C15 1.385(6) . ? C15 C16 1.377(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? 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 N5 Cd1 O1W 95.35(14) 4_454 . ? N5 Cd1 N2 170.66(13) 4_454 . ? O1W Cd1 N2 86.46(13) . . ? N5 Cd1 N6 88.87(12) 4_454 . ? O1W Cd1 N6 99.87(13) . . ? N2 Cd1 N6 99.87(12) . . ? N5 Cd1 N4 103.79(12) 4_454 . ? O1W Cd1 N4 158.03(12) . . ? N2 Cd1 N4 72.94(11) . . ? N6 Cd1 N4 91.28(13) . . ? N5 Cd1 O7 87.39(12) 4_454 . ? O1W Cd1 O7 77.58(14) . . ? N2 Cd1 O7 84.04(11) . . ? N6 Cd1 O7 175.25(11) . . ? N4 Cd1 O7 92.45(13) . . ? O1 Cl1 O3 111.0(3) . . ? O1 Cl1 O4 110.8(2) . . ? O3 Cl1 O4 109.7(3) . . ? O1 Cl1 O2 108.5(2) . . ? O3 Cl1 O2 107.5(2) . . ? O4 Cl1 O2 109.2(3) . . ? O6 Cl2 O8 110.5(4) . . ? O6 Cl2 O5 108.6(3) . . ? O8 Cl2 O5 110.3(3) . . ? O6 Cl2 O7 109.1(4) . . ? O8 Cl2 O7 109.2(2) . . ? O5 Cl2 O7 109.1(3) . . ? Cl2 O7 Cd1 135.6(2) . . ? Cd1 O1W H1WA 109.5 . . ? C3 N1 C1 107.3(4) . . ? C3 N1 H1B 126.4 . . ? C1 N1 H1B 126.4 . . ? C3 N2 C2 106.2(3) . . ? C3 N2 Cd1 114.1(2) . . ? C2 N2 Cd1 139.2(3) . . ? C4 N3 C5 107.5(4) . . ? C4 N3 H3A 126.2 . . ? C5 N3 H3A 126.2 . . ? C4 N4 C6 105.8(4) . . ? C4 N4 Cd1 111.1(3) . . ? C6 N4 Cd1 143.0(3) . . ? C16 N5 C12 116.4(4) . . ? C16 N5 Cd1 125.5(3) . 4_445 ? C12 N5 Cd1 118.1(3) . 4_445 ? C11 N6 C7 115.9(4) . . ? C11 N6 Cd1 125.4(3) . . ? C7 N6 Cd1 117.4(3) . . ? C2 C1 N1 106.2(4) . . ? C2 C1 H1A 126.9 . . ? N1 C1 H1A 126.9 . . ? C1 C2 N2 109.2(4) . . ? C1 C2 H2A 125.4 . . ? N2 C2 H2A 125.4 . . ? N2 C3 N1 111.1(4) . . ? N2 C3 C4 120.1(3) . . ? N1 C3 C4 128.8(4) . . ? N4 C4 N3 110.6(4) . . ? N4 C4 C3 121.0(4) . . ? N3 C4 C3 128.4(4) . . ? C6 C5 N3 105.8(4) . . ? C6 C5 H5A 127.1 . . ? N3 C5 H5A 127.1 . . ? C5 C6 N4 110.3(4) . . ? C5 C6 H6A 124.9 . . ? N4 C6 H6A 124.9 . . ? N6 C7 C8 124.2(4) . . ? N6 C7 H7A 117.9 . . ? C8 C7 H7A 117.9 . . ? C7 C8 C9 119.9(4) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 116.2(4) . . ? C10 C9 C14 123.4(3) . . ? C8 C9 C14 120.4(4) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? N6 C11 C10 124.2(4) . . ? N6 C11 H11A 117.9 . . ? C10 C11 H11A 117.9 . . ? N5 C12 C13 124.0(4) . . ? N5 C12 H12A 118.0 . . ? C13 C12 H12A 118.0 . . ? C14 C13 C12 119.9(5) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 116.1(4) . . ? C13 C14 C9 121.0(4) . . ? C15 C14 C9 123.0(4) . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? N5 C16 C15 122.8(4) . . ? N5 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.380 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.057