Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_f _database_code_CSD 165005 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Cui, C.-P.' 'Dai, J.-C.' 'Fu, Z.-Y.' 'Hu, S.-M.' 'Wu, Xintao' 'Wu, L.-M.' _publ_contact_author_name 'Prof Xintao Wu' _publ_contact_author_address ; Prof Xintao Wu Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email 'WXT@MS.FJIRSM.AC.CN' _publ_section_title ; Interpenetration in [Cd(isonicotinate)2(1,2-bis(4-pyridyl)ethane)0.5H20]n, A Novel Octahedral Polymer Containing an Unusual Two-dimensional Bilayer Motif Generated by Self-assembly of Rectangle Building Blocks ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H16 Cd N3 O5' _chemical_formula_weight 466.74 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.6442(5) _cell_length_b 14.7052(6) _cell_length_c 11.1580(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.7730(10) _cell_angle_gamma 90.00 _cell_volume 1912.94(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method ? _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 1.000 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3472 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1717 _reflns_number_observed 1545 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+5.1213P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1717 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_obs 0.0302 _refine_ls_wR_factor_all 0.0767 _refine_ls_wR_factor_obs 0.0726 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd -0.22309(3) 0.0000 -0.32061(3) 0.02073(13) Uani 1 d S . O1 O -0.1551(3) 0.0000 -0.0911(3) 0.0285(8) Uani 1 d S . O2 O -0.3570(2) -0.1128(2) -0.3367(2) 0.0305(6) Uani 1 d . . N1 N -0.2856(3) 0.0000 -0.5483(4) 0.0290(9) Uani 1 d S . C8 C -0.4383(3) -0.2347(3) -0.2599(4) 0.0320(8) Uani 1 d . . O3 O -0.2872(3) -0.1434(2) -0.1232(3) 0.0577(9) Uani 1 d . . C7 C -0.3533(3) -0.1575(3) -0.2383(4) 0.0328(8) Uani 1 d . . C11 C -0.5378(3) -0.2412(3) -0.3713(4) 0.0362(9) Uani 1 d . . H11A H -0.5554(3) -0.1972(3) -0.4359(4) 0.043 Uiso 1 calc R . C9 C -0.4180(3) -0.3018(3) -0.1665(4) 0.0419(10) Uani 1 d . . H9A H -0.3529(3) -0.2993(3) -0.0900(4) 0.050 Uiso 1 calc R . C4 C -0.4510(4) 0.0000 -0.7470(5) 0.0343(12) Uani 1 d S . H4A H -0.5306(4) 0.0000 -0.7873(5) 0.041 Uiso 1 calc SR . C3 C -0.3995(4) 0.0000 -0.6137(5) 0.0353(12) Uani 1 d S . H3A H -0.4461(4) 0.0000 -0.5665(5) 0.042 Uiso 1 calc SR . C5 C -0.3861(5) 0.0000 -0.8216(5) 0.046(2) Uani 1 d S . C12 C -0.6105(3) -0.3142(3) -0.3847(4) 0.0372(9) Uani 1 d . . H12A H -0.6771(3) -0.3175(3) -0.4595(4) 0.045 Uiso 1 calc R . N2 N -0.5905(2) -0.3802(2) -0.2963(3) 0.0315(7) Uani 1 d . . C10 C -0.4944(3) -0.3721(3) -0.1873(4) 0.0422(10) Uani 1 d . . H10A H -0.4794(3) -0.4164(3) -0.1233(4) 0.051 Uiso 1 calc R . C1 C -0.2212(5) 0.0000 -0.6197(6) 0.056(2) Uani 1 d S . H1A H -0.1417(5) 0.0000 -0.5770(6) 0.067 Uiso 1 calc SR . C2 C -0.2680(6) 0.0000 -0.7539(6) 0.076(3) Uani 1 d S . H2A H -0.2199(6) 0.0000 -0.7994(6) 0.091 Uiso 1 calc SR . C6 C -0.4366(5) 0.0000 -0.9684(6) 0.070(2) Uani 1 d S . H6A H -0.4082(5) 0.0531 -0.9980(6) 0.085 Uiso 0.50 calc PR . H6B H -0.4082(5) -0.0531 -0.9980(6) 0.085 Uiso 0.50 calc PR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0200(2) 0.0183(2) 0.0215(2) 0.000 0.00538(14) 0.000 O1 0.028(2) 0.031(2) 0.023(2) 0.000 0.0048(14) 0.000 O2 0.0288(13) 0.0268(13) 0.0310(13) 0.0045(11) 0.0061(11) -0.0089(11) N1 0.024(2) 0.039(3) 0.022(2) 0.000 0.007(2) 0.000 C8 0.031(2) 0.030(2) 0.031(2) 0.004(2) 0.008(2) -0.007(2) O3 0.060(2) 0.057(2) 0.032(2) 0.0108(15) -0.0075(14) -0.036(2) C7 0.030(2) 0.029(2) 0.035(2) 0.003(2) 0.008(2) -0.008(2) C11 0.034(2) 0.034(2) 0.032(2) 0.009(2) 0.003(2) -0.007(2) C9 0.035(2) 0.041(2) 0.036(2) 0.013(2) -0.002(2) -0.013(2) C4 0.024(3) 0.052(3) 0.024(3) 0.000 0.006(2) 0.000 C3 0.030(3) 0.051(3) 0.027(3) 0.000 0.013(2) 0.000 C5 0.037(3) 0.075(5) 0.024(3) 0.000 0.009(2) 0.000 C12 0.030(2) 0.034(2) 0.034(2) 0.009(2) -0.002(2) -0.007(2) N2 0.0261(15) 0.027(2) 0.035(2) 0.0054(14) 0.0052(13) -0.0070(13) C10 0.040(2) 0.038(2) 0.035(2) 0.014(2) 0.000(2) -0.010(2) C1 0.027(3) 0.110(6) 0.028(3) 0.000 0.006(3) 0.000 C2 0.033(3) 0.167(9) 0.032(3) 0.000 0.018(3) 0.000 C6 0.039(4) 0.143(8) 0.027(3) 0.000 0.010(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.327(2) . ? Cd1 O2 2.327(2) 6 ? Cd1 N1 2.351(4) . ? Cd1 O1 2.365(3) . ? Cd1 N2 2.374(3) 8_545 ? Cd1 N2 2.374(3) 3 ? O2 C7 1.265(4) . ? N1 C3 1.340(6) . ? N1 C1 1.342(7) . ? C8 C9 1.385(5) . ? C8 C11 1.388(5) . ? C8 C7 1.517(5) . ? O3 C7 1.249(5) . ? C11 C12 1.382(5) . ? C9 C10 1.372(5) . ? C4 C3 1.373(7) . ? C4 C5 1.378(8) . ? C5 C2 1.388(9) . ? C5 C6 1.509(8) . ? C12 N2 1.337(5) . ? N2 C10 1.350(5) . ? N2 Cd1 2.374(3) 3_445 ? C1 C2 1.381(9) . ? C6 C6 1.481(12) 5_453 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 90.94(12) . 6 ? O2 Cd1 N1 89.23(9) . . ? O2 Cd1 N1 89.23(9) 6 . ? O2 Cd1 O1 91.84(8) . . ? O2 Cd1 O1 91.84(8) 6 . ? N1 Cd1 O1 178.47(12) . . ? O2 Cd1 N2 86.58(10) . 8_545 ? O2 Cd1 N2 176.70(10) 6 8_545 ? N1 Cd1 N2 92.90(10) . 8_545 ? O1 Cd1 N2 86.08(9) . 8_545 ? O2 Cd1 N2 176.70(10) . 3 ? O2 Cd1 N2 86.58(10) 6 3 ? N1 Cd1 N2 92.90(10) . 3 ? O1 Cd1 N2 86.08(9) . 3 ? N2 Cd1 N2 95.82(15) 8_545 3 ? C7 O2 Cd1 121.5(2) . . ? C3 N1 C1 116.7(4) . . ? C3 N1 Cd1 115.4(3) . . ? C1 N1 Cd1 127.9(3) . . ? C9 C8 C11 117.6(3) . . ? C9 C8 C7 120.1(3) . . ? C11 C8 C7 122.3(3) . . ? O3 C7 O2 126.2(3) . . ? O3 C7 C8 116.1(3) . . ? O2 C7 C8 117.7(3) . . ? C12 C11 C8 119.0(3) . . ? C10 C9 C8 119.8(4) . . ? C3 C4 C5 120.7(5) . . ? N1 C3 C4 123.3(5) . . ? C4 C5 C2 116.0(5) . . ? C4 C5 C6 123.7(5) . . ? C2 C5 C6 120.3(5) . . ? N2 C12 C11 123.7(3) . . ? C12 N2 C10 116.6(3) . . ? C12 N2 Cd1 122.1(2) . 3_445 ? C10 N2 Cd1 121.1(2) . 3_445 ? N2 C10 C9 123.2(4) . . ? N1 C1 C2 122.7(5) . . ? C1 C2 C5 120.6(6) . . ? C6 C6 C5 116.3(7) 5_453 . ? _refine_diff_density_max 0.587 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.090