Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shilun Qiu' _publ_contact_author_address ; Preparative Chemisty Jilin University Qianjin Avenue 2699 Changchun 130012 CHINA ; _publ_contact_author_email SQIU@MAIL.JLU.EDU.CN _publ_section_title ; Porous coordination polymers with zeolite topologies constructed from 4-connected building units ; loop_ _publ_author_name 'Shilun Qiu' 'Qian-Rong Fang' 'Jin-Yu Sun' 'Ming Xue' 'Guang-Shan Zhu' # Attachment 'the polymer 1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 274238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H19 Cd Cl0 N O8' _chemical_formula_sum 'C11 H19 Cd Cl0 N O8' _chemical_formula_weight 405.67 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1355(6) _cell_length_b 15.4673(9) _cell_length_c 9.1740(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.9300(10) _cell_angle_gamma 90.00 _cell_volume 1368.35(14) _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 colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.636 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6940 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2406 _reflns_number_gt 2382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0948P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2406 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.762714(15) 1.210804(10) -0.105863(16) 0.02133(15) Uani 1 1 d . . . O1 O 0.7238(2) 1.05928(13) -0.1404(2) 0.0395(5) Uani 1 1 d . . . O2 O 0.8501(2) 1.09772(12) 0.0898(2) 0.0402(5) Uani 1 1 d . . . O3 O 1.17124(19) 0.80259(12) 0.3219(2) 0.0288(4) Uani 1 1 d . . . O4 O 1.0472(2) 0.78660(10) 0.4792(2) 0.0309(5) Uani 1 1 d . . . O5 O 0.51792(18) 0.81984(15) 0.27693(19) 0.0367(4) Uani 1 1 d . . . O6 O 0.4309(2) 0.78047(11) 0.0361(2) 0.0320(4) Uani 1 1 d . . . O7 O 0.66916(18) 1.34348(12) -0.23968(19) 0.0334(4) Uani 1 1 d . . . H1O7 H 0.6304 1.3931 -0.2418 0.040 Uiso 1 1 d . . . H2O7 H 0.7005 1.3422 -0.3159 0.040 Uiso 1 1 d . . . O8 O 0.0944(2) 0.11179(17) 0.3498(3) 0.0539(6) Uani 1 1 d . . . H1O8 H 0.0394 0.1221 0.2607 0.065 Uiso 1 1 d . . . H2O8 H 0.0510 0.1256 0.4137 0.065 Uiso 1 1 d . . . C1 C 0.7927(2) 1.04048(14) -0.0054(3) 0.0258(5) Uani 1 1 d . . . C2 C 0.8025(2) 0.94586(15) 0.0411(3) 0.0251(5) Uani 1 1 d . . . H2A H 0.8125 0.9114 -0.0445 0.030 Uiso 1 1 calc R . . C3 C 0.9258(2) 0.92607(17) 0.1825(3) 0.0261(5) Uani 1 1 d . . . H3A H 0.9191 0.9601 0.2688 0.031 Uiso 1 1 calc R . . H3B H 1.0116 0.9412 0.1628 0.031 Uiso 1 1 calc R . . C4 C 0.9257(2) 0.82947(14) 0.2202(2) 0.0243(5) Uani 1 1 d . . . H4A H 0.9264 0.7973 0.1284 0.029 Uiso 1 1 calc R . . C5 C 0.7918(2) 0.80587(17) 0.2548(3) 0.0264(5) Uani 1 1 d . . . H5A H 0.7932 0.7450 0.2807 0.032 Uiso 1 1 calc R . . H5B H 0.7854 0.8390 0.3422 0.032 Uiso 1 1 calc R . . C6 C 0.6664(2) 0.82465(15) 0.1169(2) 0.0248(5) Uani 1 1 d . . . H6A H 0.6712 0.7880 0.0315 0.030 Uiso 1 1 calc R . . C7 C 0.6654(2) 0.92017(15) 0.0684(3) 0.0259(5) Uani 1 1 d . . . H7A H 0.5894 0.9295 -0.0248 0.031 Uiso 1 1 calc R . . H7B H 0.6503 0.9567 0.1477 0.031 Uiso 1 1 calc R . . C8 C 1.0560(3) 0.80505(15) 0.3474(3) 0.0229(5) Uani 1 1 d . . . C9 C 0.5298(2) 0.80751(15) 0.1476(3) 0.0231(5) Uani 1 1 d . . . C10 C 0.4166(3) 0.0707(2) 0.4216(4) 0.0434(7) Uani 1 1 d . . . H10A H 0.4106 0.0608 0.3154 0.052 Uiso 1 1 calc R . . H10B H 0.3641 0.1225 0.4265 0.052 Uiso 1 1 calc R . . C11 C 0.6443(3) 0.00568(18) 0.5183(3) 0.0365(6) Uani 1 1 d . . . H11A H 0.7388 0.0151 0.5831 0.044 Uiso 1 1 calc R . . H11B H 0.6470 -0.0071 0.4158 0.044 Uiso 1 1 calc R . . N1 N 0.5646(2) 0.08325(15) 0.5147(3) 0.0363(5) Uani 1 1 d . . . H1A H 0.6013 0.1267 0.4744 0.044 Uiso 1 1 calc R . . H1B H 0.5691 0.0981 0.6109 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 0.0171(2) 0.0220(2) 0.0246(2) 0.00108(4) 0.00594(13) -0.00115(4) O1 0.0517(11) 0.0307(11) 0.0307(10) 0.0081(8) 0.0046(9) 0.0045(8) O2 0.0406(11) 0.0248(9) 0.0457(10) -0.0033(7) -0.0009(8) 0.0001(7) O3 0.0171(9) 0.0415(10) 0.0262(9) 0.0041(7) 0.0042(7) 0.0030(7) O4 0.0231(11) 0.0458(12) 0.0240(10) 0.0070(6) 0.0076(8) 0.0085(6) O5 0.0251(9) 0.0565(12) 0.0297(10) 0.0003(8) 0.0104(7) -0.0016(9) O6 0.0181(9) 0.0415(10) 0.0347(10) -0.0037(7) 0.0057(8) -0.0033(6) O7 0.0372(10) 0.0326(10) 0.0313(9) 0.0050(7) 0.0120(7) 0.0072(7) O8 0.0396(12) 0.0568(14) 0.0574(13) -0.0130(11) 0.0031(10) 0.0100(10) C1 0.0219(12) 0.0245(12) 0.0337(13) 0.0049(9) 0.0125(10) 0.0031(9) C2 0.0229(11) 0.0246(12) 0.0277(11) 0.0036(8) 0.0078(9) 0.0006(8) C3 0.0185(11) 0.0262(13) 0.0330(12) 0.0023(9) 0.0069(9) -0.0019(9) C4 0.0189(11) 0.0273(13) 0.0251(11) 0.0022(8) 0.0047(8) 0.0003(8) C5 0.0200(13) 0.0320(11) 0.0267(12) 0.0071(9) 0.0064(10) 0.0003(9) C6 0.0192(11) 0.0269(13) 0.0278(11) 0.0012(9) 0.0065(9) -0.0013(9) C7 0.0187(11) 0.0263(11) 0.0306(11) 0.0067(9) 0.0048(9) 0.0007(9) C8 0.0210(12) 0.0208(10) 0.0255(12) 0.0021(9) 0.0052(9) 0.0013(9) C9 0.0190(12) 0.0215(10) 0.0277(12) 0.0050(9) 0.0054(9) 0.0040(9) C10 0.0372(16) 0.0316(15) 0.0519(18) 0.0046(13) 0.0000(13) 0.0038(12) C11 0.0269(13) 0.0406(15) 0.0446(15) -0.0100(11) 0.0150(11) -0.0039(11) N1 0.0358(12) 0.0339(12) 0.0393(12) -0.0008(9) 0.0118(9) -0.0087(9) _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 O6 2.248(2) 3_675 ? Cd1 O4 2.2492(18) 2_755 ? Cd1 O3 2.2880(18) 3_775 ? Cd1 O1 2.382(2) . ? Cd1 O7 2.4291(17) . ? Cd1 O2 2.4669(18) . ? O1 C1 1.255(3) . ? O2 C1 1.254(3) . ? O3 C8 1.261(3) . ? O3 Cd1 2.2880(18) 3_775 ? O4 C8 1.272(3) . ? O4 Cd1 2.2492(18) 2_745 ? O5 C9 1.244(3) . ? O6 C9 1.262(3) . ? O6 Cd1 2.248(2) 3_675 ? O7 H1O7 0.86 . ? O7 H2O7 0.85 . ? O8 H1O8 0.85 . ? O8 H2O8 0.86 . ? C1 C2 1.519(3) . ? C2 C3 1.530(3) . ? C2 C7 1.538(3) . ? C2 H2A 0.9800 . ? C3 C4 1.534(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C8 1.517(3) . ? C4 C5 1.530(3) . ? C4 H4A 0.9800 . ? C5 C6 1.520(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C9 1.518(3) . ? C6 C7 1.542(3) . ? C6 H6A 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 N1 1.493(4) . ? C10 C11 1.514(4) 3_656 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.441(4) . ? C11 C10 1.513(4) 3_656 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? 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 O6 Cd1 O4 120.39(7) 3_675 2_755 ? O6 Cd1 O3 139.99(7) 3_675 3_775 ? O4 Cd1 O3 93.56(7) 2_755 3_775 ? O6 Cd1 O1 88.49(7) 3_675 . ? O4 Cd1 O1 131.47(7) 2_755 . ? O3 Cd1 O1 82.88(7) 3_775 . ? O6 Cd1 O7 81.60(6) 3_675 . ? O4 Cd1 O7 87.69(6) 2_755 . ? O3 Cd1 O7 79.14(6) 3_775 . ? O1 Cd1 O7 137.83(7) . . ? O6 Cd1 O2 89.13(7) 3_675 . ? O4 Cd1 O2 86.28(7) 2_755 . ? O3 Cd1 O2 115.51(7) 3_775 . ? O1 Cd1 O2 53.62(6) . . ? O7 Cd1 O2 164.47(6) . . ? C1 O1 Cd1 94.44(16) . . ? C1 O2 Cd1 90.49(15) . . ? C8 O3 Cd1 134.32(16) . 3_775 ? C8 O4 Cd1 107.96(16) . 2_745 ? C9 O6 Cd1 107.11(16) . 3_675 ? Cd1 O7 H1O7 150.5 . . ? Cd1 O7 H2O7 102.1 . . ? H1O7 O7 H2O7 106.6 . . ? H1O8 O8 H2O8 106.6 . . ? O2 C1 O1 121.4(2) . . ? O2 C1 C2 120.6(2) . . ? O1 C1 C2 118.0(2) . . ? C1 C2 C3 113.36(19) . . ? C1 C2 C7 108.10(18) . . ? C3 C2 C7 110.70(19) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C7 C2 H2A 108.2 . . ? C2 C3 C4 109.20(19) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C8 C4 C5 113.49(19) . . ? C8 C4 C3 110.79(18) . . ? C5 C4 C3 109.97(19) . . ? C8 C4 H4A 107.4 . . ? C5 C4 H4A 107.4 . . ? C3 C4 H4A 107.4 . . ? C6 C5 C4 110.47(19) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C9 C6 C5 112.92(18) . . ? C9 C6 C7 107.20(18) . . ? C5 C6 C7 110.64(19) . . ? C9 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C2 C7 C6 111.65(19) . . ? C2 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C2 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O3 C8 O4 120.7(2) . . ? O3 C8 C4 120.1(2) . . ? O4 C8 C4 119.2(2) . . ? O5 C9 O6 122.6(2) . . ? O5 C9 C6 120.7(2) . . ? O6 C9 C6 116.7(2) . . ? N1 C10 C11 110.1(2) . 3_656 ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 3_656 . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 3_656 . ? H10A C10 H10B 108.2 . . ? N1 C11 C10 111.7(2) . 3_656 ? N1 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 3_656 . ? N1 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 3_656 . ? H11A C11 H11B 107.9 . . ? C11 N1 C10 111.3(2) . . ? C11 N1 H1A 109.4 . . ? C10 N1 H1A 109.4 . . ? C11 N1 H1B 109.4 . . ? C10 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? 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 O7 H2O7 O2 0.85 2.17 2.899(3) 143.0 4_585 O7 H2O7 O6 0.85 2.26 2.771(3) 118.5 2_654 O7 H2O7 O3 0.85 2.60 3.007(3) 110.6 3_775 O8 H1O8 O2 0.85 2.11 2.869(3) 149.3 1_445 O8 H2O8 O4 0.86 2.10 2.894(3) 153.4 3_666 N1 H1A O7 0.90 2.32 3.061(3) 139.8 4_576 N1 H1A O6 0.90 2.40 3.088(3) 133.5 2_645 N1 H1A O3 0.90 2.71 3.172(3) 112.9 3_766 N1 H1B O5 0.90 2.00 2.755(3) 140.3 3_666 N1 H1B O1 0.90 2.41 3.100(3) 133.3 1_546 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.465 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.116 # Attachment 'the polymer 2.cif' data_squeez _database_code_depnum_ccdc_archive 'CCDC 274239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C9 H9 Cd O6' _chemical_formula_sum 'C9 H9 Cd O6' _chemical_formula_weight 325.56 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2484(18) _cell_length_b 15.569(3) _cell_length_c 8.6385(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.42(3) _cell_angle_gamma 90.00 _cell_volume 1238.3(4) _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 colorless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 1.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2771 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1382 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2771 _reflns_number_gt 1427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2771 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.72864(5) -0.16290(4) 0.23069(7) 0.03402(18) Uani 1 1 d . . . O1 O 0.7080(5) -0.0141(4) 0.2379(7) 0.0535(15) Uani 1 1 d . . . O2 O 0.7749(5) -0.0652(3) 0.0255(6) 0.0483(15) Uani 1 1 d . . . O3 O 0.4803(4) 0.3241(4) 0.1577(5) 0.0395(14) Uani 1 1 d . . . O4 O 0.3567(5) 0.2565(4) -0.0382(7) 0.0538(17) Uani 1 1 d . . . O5 O 1.1022(5) 0.2365(4) 0.2160(7) 0.0560(18) Uani 1 1 d . . . O6 O 1.0535(5) 0.3450(4) 0.0667(7) 0.0597(18) Uani 1 1 d . . . C1 C 0.7423(6) -0.0038(6) 0.1070(10) 0.038(2) Uani 1 1 d . . . C2 C 0.7434(7) 0.0882(5) 0.0403(8) 0.0327(19) Uani 1 1 d . . . H2 H 0.7420 0.0837 -0.0730 0.039 Uiso 1 1 calc R . . C3 C 0.6109(6) 0.1385(5) 0.0760(9) 0.038(2) Uani 1 1 d . . . H3A H 0.6089 0.1429 0.1877 0.046 Uiso 1 1 calc R . . H3B H 0.5241 0.1083 0.0344 0.046 Uiso 1 1 calc R . . C4 C 0.6117(6) 0.2292(5) 0.0051(9) 0.0327(19) Uani 1 1 d . . . H4 H 0.6086 0.2237 -0.1082 0.039 Uiso 1 1 calc R . . C5 C 0.7518(6) 0.2765(5) 0.0638(9) 0.0330(19) Uani 1 1 d . . . H5A H 0.7502 0.2880 0.1740 0.040 Uiso 1 1 calc R . . H5B H 0.7541 0.3314 0.0109 0.040 Uiso 1 1 calc R . . C6 C 0.8909(6) 0.2264(5) 0.0385(9) 0.033(2) Uani 1 1 d . . . H6 H 0.8999 0.2234 -0.0735 0.040 Uiso 1 1 calc R . . C7 C 0.8849(7) 0.1348(5) 0.1015(10) 0.043(2) Uani 1 1 d . . . H7A H 0.8916 0.1366 0.2142 0.052 Uiso 1 1 calc R . . H7B H 0.9676 0.1027 0.0714 0.052 Uiso 1 1 calc R . . C8 C 0.4744(7) 0.2730(5) 0.0440(10) 0.035(2) Uani 1 1 d . . . C9 C 1.0241(7) 0.2715(6) 0.1157(10) 0.039(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0213(2) 0.0324(3) 0.0483(4) 0.0022(4) 0.00282(19) 0.0010(3) O1 0.059(3) 0.041(4) 0.064(4) 0.004(4) 0.027(3) 0.004(3) O2 0.057(3) 0.031(4) 0.057(4) 0.006(3) 0.006(3) 0.007(3) O3 0.035(3) 0.052(4) 0.032(3) -0.011(3) 0.011(2) 0.005(3) O4 0.019(3) 0.058(4) 0.082(5) -0.024(4) -0.011(3) 0.006(3) O5 0.033(3) 0.067(5) 0.063(4) 0.016(4) -0.022(3) -0.024(3) O6 0.028(3) 0.045(4) 0.103(5) 0.004(4) -0.008(3) -0.008(3) C1 0.004(3) 0.042(6) 0.069(6) 0.001(5) 0.013(3) -0.003(3) C2 0.023(4) 0.045(5) 0.031(5) -0.001(4) 0.007(3) 0.000(3) C3 0.021(4) 0.029(5) 0.067(6) 0.004(4) 0.011(3) -0.002(3) C4 0.017(3) 0.035(5) 0.046(5) -0.004(4) 0.003(3) -0.003(3) C5 0.019(3) 0.029(5) 0.052(5) 0.003(4) 0.009(3) 0.001(3) C6 0.018(3) 0.032(5) 0.050(5) -0.006(4) 0.001(3) 0.002(3) C7 0.018(3) 0.030(5) 0.082(6) -0.005(5) 0.003(4) -0.005(3) C8 0.021(4) 0.029(5) 0.058(6) 0.004(5) 0.012(3) 0.003(3) C9 0.013(3) 0.043(6) 0.060(6) 0.007(5) 0.001(4) 0.003(4) _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 O5 2.231(5) 2_745 ? Cd1 O3 2.249(4) 2_645 ? Cd1 O4 2.295(5) 3_655 ? Cd1 O1 2.326(6) . ? Cd1 O2 2.405(5) . ? Cd1 O6 2.544(5) 2_745 ? Cd1 C9 2.732(7) 2_745 ? O1 C1 1.213(9) . ? O2 C1 1.242(9) . ? O3 C8 1.261(8) . ? O3 Cd1 2.249(4) 2_655 ? O4 C8 1.268(8) . ? O4 Cd1 2.295(5) 3_655 ? O5 C9 1.204(8) . ? O5 Cd1 2.231(5) 2_755 ? O6 C9 1.259(9) . ? O6 Cd1 2.544(5) 2_755 ? C1 C2 1.545(10) . ? C2 C3 1.510(8) . ? C2 C7 1.545(9) . ? C3 C4 1.539(9) . ? C4 C8 1.507(9) . ? C4 C5 1.534(8) . ? C5 C6 1.538(8) . ? C6 C9 1.516(9) . ? C6 C7 1.530(10) . ? C9 Cd1 2.732(7) 2_755 ? 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 O5 Cd1 O3 117.5(2) 2_745 2_645 ? O5 Cd1 O4 83.71(19) 2_745 3_655 ? O3 Cd1 O4 90.17(18) 2_645 3_655 ? O5 Cd1 O1 138.72(19) 2_745 . ? O3 Cd1 O1 90.13(19) 2_645 . ? O4 Cd1 O1 128.9(2) 3_655 . ? O5 Cd1 O2 115.2(2) 2_745 . ? O3 Cd1 O2 126.38(18) 2_645 . ? O4 Cd1 O2 86.6(2) 3_655 . ? O1 Cd1 O2 53.87(18) . . ? O5 Cd1 O6 52.94(19) 2_745 2_745 ? O3 Cd1 O6 111.47(17) 2_645 2_745 ? O4 Cd1 O6 136.49(18) 3_655 2_745 ? O1 Cd1 O6 89.7(2) . 2_745 ? O2 Cd1 O6 106.98(18) . 2_745 ? O5 Cd1 C9 25.6(2) 2_745 2_745 ? O3 Cd1 C9 118.1(2) 2_645 2_745 ? O4 Cd1 C9 109.2(2) 3_655 2_745 ? O1 Cd1 C9 115.3(2) . 2_745 ? O2 Cd1 C9 113.3(2) . 2_745 ? O6 Cd1 C9 27.31(19) 2_745 2_745 ? C1 O1 Cd1 94.4(5) . . ? C1 O2 Cd1 90.0(5) . . ? C8 O3 Cd1 114.5(4) . 2_655 ? C8 O4 Cd1 138.8(5) . 3_655 ? C9 O5 Cd1 101.1(5) . 2_755 ? C9 O6 Cd1 84.7(4) . 2_755 ? O1 C1 O2 121.7(8) . . ? O1 C1 C2 118.8(8) . . ? O2 C1 C2 119.5(7) . . ? C3 C2 C7 111.3(6) . . ? C3 C2 C1 111.7(6) . . ? C7 C2 C1 110.0(6) . . ? C2 C3 C4 111.1(6) . . ? C8 C4 C5 114.3(6) . . ? C8 C4 C3 106.9(6) . . ? C5 C4 C3 110.2(6) . . ? C4 C5 C6 113.6(6) . . ? C9 C6 C7 109.3(6) . . ? C9 C6 C5 111.0(6) . . ? C7 C6 C5 111.3(6) . . ? C6 C7 C2 111.9(6) . . ? O4 C8 O3 122.4(6) . . ? O4 C8 C4 118.7(7) . . ? O3 C8 C4 118.9(6) . . ? O5 C9 O6 121.2(7) . . ? O5 C9 C6 120.9(7) . . ? O6 C9 C6 117.7(7) . . ? O5 C9 Cd1 53.3(4) . 2_755 ? O6 C9 Cd1 68.0(4) . 2_755 ? C6 C9 Cd1 174.1(6) . 2_755 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.678 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.147