# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Junfeng Bai' _publ_contact_author_email BJUNFENG@NJU.EDU.CN _publ_section_title ; pH-Controlled Change of the Coordination Modes of the Highly Symmetrical Multitopic Ligand and Metal-Oxygen Arrays to Construct Coordination Assemblies ; loop_ _publ_author_name 'Junfeng Bai' 'Zhuxiu Zhang' 'Bo Zheng' # Attachment '732255.cif' data_260304g _database_code_depnum_ccdc_archive 'CCDC 732255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H2 Cd3 O10' _chemical_formula_sum 'C8 H2 Cd3 O10' _chemical_formula_weight 595.33 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' 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 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' 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 13.2366(13) _cell_length_b 7.1753(6) _cell_length_c 12.7690(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.344(2) _cell_angle_gamma 90.00 _cell_volume 1077.25(17) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2364 _cell_measurement_theta_min 3.084 _cell_measurement_theta_max 28.258 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 5.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.216 _exptl_absorpt_correction_T_max 0.315 _exptl_absorpt_process_details 'SADABS(Brucker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2915 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1139 _reflns_number_gt 1094 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _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^)+(0.0335P)^2^+2.3520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1139 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.5262(4) 0.5000 0.3865(4) 0.0134(10) Uani 1 2 d S . . C2 C 0.4446(3) 0.3559(5) 0.3155(3) 0.0128(7) Uani 1 1 d . . . C3 C 0.3693(4) 0.5000 0.2334(4) 0.0132(10) Uani 1 2 d S . . C4 C 0.8764(3) 0.6010(5) 0.7644(3) 0.0135(7) Uani 1 1 d . . . C5 C 0.9916(3) 0.6032(5) 0.8635(3) 0.0153(8) Uani 1 1 d . . . Cd1 Cd 0.7500 0.7500 0.5000 0.01431(15) Uani 1 2 d S . . Cd2 Cd 0.70920(3) 1.0000 0.71437(3) 0.01312(15) Uani 1 2 d S . . Cd3 Cd 0.7500 1.2500 1.0000 0.01409(15) Uani 1 2 d S . . O1 O 0.6230(3) 0.5000 0.4699(3) 0.0156(7) Uani 1 2 d S . . O2 O 0.4437(2) 0.1841(4) 0.3255(3) 0.0206(6) Uani 1 1 d . . . O3 O 0.2831(3) 0.5000 0.1370(3) 0.0151(7) Uani 1 2 d S . . O4 O 0.8095(2) 0.7275(4) 0.7012(2) 0.0180(6) Uani 1 1 d . . . O5 O 1.0594(2) 0.7282(4) 0.9191(3) 0.0220(6) Uani 1 1 d . . . O6 O 0.6629(3) 1.0000 0.5205(3) 0.0129(7) Uani 1 2 d S . . H6 H 0.5916 1.0000 0.4756 0.016 Uiso 1 2 d SR . . O7 O 0.7810(3) 1.0000 0.9067(3) 0.0151(7) Uani 1 2 d S . . H7 H 0.8518 1.0000 0.9390 0.018 Uiso 1 2 d SR . . 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 0.013(2) 0.014(2) 0.015(3) 0.000 0.008(2) 0.000 C2 0.0130(15) 0.0143(17) 0.0103(17) -0.0016(14) 0.0048(13) 0.0005(13) C3 0.015(2) 0.013(2) 0.011(2) 0.000 0.006(2) 0.000 C4 0.0145(16) 0.0166(19) 0.0120(17) -0.0008(15) 0.0082(14) 0.0015(14) C5 0.0117(16) 0.024(2) 0.0119(17) 0.0019(15) 0.0069(14) 0.0019(14) Cd1 0.0210(2) 0.0096(2) 0.0124(2) -0.00195(13) 0.00773(18) -0.00055(12) Cd2 0.0171(2) 0.0120(2) 0.0111(2) 0.000 0.00728(17) 0.000 Cd3 0.0152(2) 0.0105(2) 0.0138(2) -0.00086(13) 0.00429(17) -0.00055(12) O1 0.0128(16) 0.0128(18) 0.0176(19) 0.000 0.0038(15) 0.000 O2 0.0196(12) 0.0084(13) 0.0324(16) 0.0011(12) 0.0108(12) -0.0008(10) O3 0.0163(17) 0.0154(18) 0.0113(18) 0.000 0.0043(14) 0.000 O4 0.0199(13) 0.0181(14) 0.0140(14) 0.0012(11) 0.0060(11) 0.0062(10) O5 0.0178(13) 0.0215(15) 0.0218(15) -0.0074(11) 0.0048(12) -0.0072(10) O6 0.0106(16) 0.0176(18) 0.0086(17) 0.000 0.0027(13) 0.000 O7 0.0179(17) 0.0136(18) 0.0123(18) 0.000 0.0058(14) 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 C1 O1 1.233(6) . ? C1 C2 1.469(5) . ? C1 C2 1.469(5) 6_565 ? C2 O2 1.241(5) . ? C2 C3 1.483(5) . ? C3 O3 1.236(6) . ? C3 C2 1.483(5) 6_565 ? C4 O4 1.266(4) . ? C4 C4 1.449(7) 6_565 ? C4 C5 1.468(5) . ? C5 O5 1.236(5) . ? C5 C5 1.481(8) 6_565 ? Cd1 O6 2.2116(19) 7_666 ? Cd1 O6 2.2116(19) . ? Cd1 O4 2.321(3) 7_666 ? Cd1 O4 2.321(3) . ? Cd1 O1 2.366(2) . ? Cd1 O1 2.366(2) 7_666 ? Cd2 O7 2.189(3) . ? Cd2 O6 2.261(3) . ? Cd2 O2 2.270(3) 5_666 ? Cd2 O2 2.270(3) 2_666 ? Cd2 O4 2.412(3) 6_575 ? Cd2 O4 2.412(2) . ? Cd3 O5 2.250(3) 3_455 ? Cd3 O5 2.250(3) 5_777 ? Cd3 O7 2.292(2) . ? Cd3 O7 2.292(2) 7_677 ? Cd3 O3 2.401(2) 3_556 ? Cd3 O3 2.401(2) 5_676 ? O1 Cd1 2.366(2) 4_646 ? O2 Cd2 2.270(3) 5_666 ? O3 Cd3 2.401(2) 2_646 ? O3 Cd3 2.401(2) 3_444 ? O5 Cd3 2.250(3) 3_545 ? O6 Cd1 2.2116(19) 4_656 ? O6 H6 0.8500 . ? O7 Cd3 2.292(2) 4_647 ? O7 H7 0.8330 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 135.3(2) . . ? O1 C1 C2 135.3(2) . 6_565 ? C2 C1 C2 89.5(4) . 6_565 ? O2 C2 C1 132.5(3) . . ? O2 C2 C3 136.9(3) . . ? C1 C2 C3 90.6(3) . . ? O3 C3 C2 135.82(19) . 6_565 ? O3 C3 C2 135.82(19) . . ? C2 C3 C2 88.3(4) 6_565 . ? O4 C4 C4 135.8(2) . 6_565 ? O4 C4 C5 133.4(3) . . ? C4 C4 C5 90.6(2) 6_565 . ? O5 C5 C4 134.1(4) . . ? O5 C5 C5 136.5(2) . 6_565 ? C4 C5 C5 89.4(2) . 6_565 ? O6 Cd1 O6 180.000(1) 7_666 . ? O6 Cd1 O4 81.72(10) 7_666 7_666 ? O6 Cd1 O4 98.28(10) . 7_666 ? O6 Cd1 O4 98.28(10) 7_666 . ? O6 Cd1 O4 81.72(10) . . ? O4 Cd1 O4 180.000(1) 7_666 . ? O6 Cd1 O1 74.69(10) 7_666 . ? O6 Cd1 O1 105.31(10) . . ? O4 Cd1 O1 91.04(11) 7_666 . ? O4 Cd1 O1 88.96(11) . . ? O6 Cd1 O1 105.31(10) 7_666 7_666 ? O6 Cd1 O1 74.69(10) . 7_666 ? O4 Cd1 O1 88.96(11) 7_666 7_666 ? O4 Cd1 O1 91.04(11) . 7_666 ? O1 Cd1 O1 180.000(1) . 7_666 ? O7 Cd2 O6 171.24(12) . . ? O7 Cd2 O2 97.72(10) . 5_666 ? O6 Cd2 O2 89.39(10) . 5_666 ? O7 Cd2 O2 97.72(10) . 2_666 ? O6 Cd2 O2 89.39(10) . 2_666 ? O2 Cd2 O2 71.16(13) 5_666 2_666 ? O7 Cd2 O4 96.26(9) . 6_575 ? O6 Cd2 O4 78.73(8) . 6_575 ? O2 Cd2 O4 156.72(10) 5_666 6_575 ? O2 Cd2 O4 88.59(9) 2_666 6_575 ? O7 Cd2 O4 96.26(8) . . ? O6 Cd2 O4 78.73(8) . . ? O2 Cd2 O4 88.59(9) 5_666 . ? O2 Cd2 O4 156.72(10) 2_666 . ? O4 Cd2 O4 108.30(13) 6_575 . ? O5 Cd3 O5 180.00(6) 3_455 5_777 ? O5 Cd3 O7 97.91(11) 3_455 . ? O5 Cd3 O7 82.09(11) 5_777 . ? O5 Cd3 O7 82.09(11) 3_455 7_677 ? O5 Cd3 O7 97.91(11) 5_777 7_677 ? O7 Cd3 O7 180.000(1) . 7_677 ? O5 Cd3 O3 94.22(11) 3_455 3_556 ? O5 Cd3 O3 85.78(11) 5_777 3_556 ? O7 Cd3 O3 77.15(10) . 3_556 ? O7 Cd3 O3 102.85(10) 7_677 3_556 ? O5 Cd3 O3 85.78(11) 3_455 5_676 ? O5 Cd3 O3 94.22(11) 5_777 5_676 ? O7 Cd3 O3 102.85(10) . 5_676 ? O7 Cd3 O3 77.15(10) 7_677 5_676 ? O3 Cd3 O3 180.000(1) 3_556 5_676 ? C1 O1 Cd1 121.28(17) . . ? C1 O1 Cd1 121.28(17) . 4_646 ? Cd1 O1 Cd1 98.59(12) . 4_646 ? C2 O2 Cd2 127.3(2) . 5_666 ? C3 O3 Cd3 120.11(16) . 2_646 ? C3 O3 Cd3 120.11(16) . 3_444 ? Cd3 O3 Cd3 96.66(12) 2_646 3_444 ? C4 O4 Cd1 122.5(2) . . ? C4 O4 Cd2 141.6(2) . . ? Cd1 O4 Cd2 95.91(9) . . ? C5 O5 Cd3 132.7(3) . 3_545 ? Cd1 O6 Cd1 108.41(14) . 4_656 ? Cd1 O6 Cd2 103.63(10) . . ? Cd1 O6 Cd2 103.63(10) 4_656 . ? Cd1 O6 H6 113.5 . . ? Cd1 O6 H6 113.5 4_656 . ? Cd2 O6 H6 113.3 . . ? Cd2 O7 Cd3 119.61(10) . 4_647 ? Cd2 O7 Cd3 119.61(10) . . ? Cd3 O7 Cd3 103.00(13) 4_647 . ? Cd2 O7 H7 111.4 . . ? Cd3 O7 H7 99.9 4_647 . ? Cd3 O7 H7 99.9 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.330 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.172 # Attachment '732256.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 732256' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H Cd O3' _chemical_formula_sum 'C2 H Cd O3' _chemical_formula_weight 185.43 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 6.8958(3) _cell_length_b 5.8147(3) _cell_length_c 15.8331(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 634.86(5) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2350 _cell_measurement_theta_min 2.573 _cell_measurement_theta_max 28.288 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 6.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.159 _exptl_absorpt_correction_T_max 0.251 _exptl_absorpt_process_details 'SADABS(Brucker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3062 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.99 _reflns_number_total 625 _reflns_number_gt 597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _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^)+(0.0219P)^2^+0.5382P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0160(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 625 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 O2 O 0.3502(3) 0.3085(4) 0.39203(14) 0.0173(5) Uani 1 1 d . . . C2 C 0.4331(4) 0.4142(6) 0.4516(2) 0.0132(6) Uani 1 1 d . . . Cd1 Cd 0.39710(3) 0.96733(4) 0.309487(13) 0.01213(15) Uani 1 1 d . . . O1 O 0.5895(3) 0.7881(5) 0.40924(15) 0.0203(6) Uani 1 1 d . . . O3 O 0.3368(3) 0.6480(4) 0.23362(13) 0.0129(4) Uani 1 1 d . . . H3A H 0.2726 0.7014 0.1820 0.016 Uiso 1 1 calc R . . C1 C 0.5391(4) 0.6303(5) 0.45871(18) 0.0138(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0195(11) 0.0151(13) 0.0174(11) -0.0051(9) -0.0076(9) 0.0028(10) C2 0.0123(14) 0.0126(15) 0.0146(14) -0.0007(12) -0.0003(11) 0.0031(12) Cd1 0.01101(19) 0.0107(2) 0.01472(18) 0.00048(8) 0.00029(7) -0.00050(8) O1 0.0187(12) 0.0211(14) 0.0211(12) 0.0101(10) -0.0041(9) -0.0047(9) O3 0.0131(10) 0.0108(11) 0.0150(10) -0.0010(8) 0.0017(8) 0.0001(8) C1 0.0096(14) 0.0174(17) 0.0144(14) 0.0001(11) -0.0008(12) 0.0028(12) _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 O2 C2 1.263(4) . ? O2 Cd1 2.339(2) 8_655 ? O2 Cd1 2.397(2) 1_545 ? C2 C1 1.456(4) 5_666 ? C2 C1 1.458(5) . ? Cd1 O3 2.222(2) 3_655 ? Cd1 O3 2.250(2) . ? Cd1 O3 2.269(2) 8_665 ? Cd1 O1 2.311(2) . ? Cd1 O2 2.339(2) 8_665 ? Cd1 O2 2.397(2) 1_565 ? O1 C1 1.255(4) . ? O3 Cd1 2.222(2) 3_645 ? O3 Cd1 2.269(2) 8_655 ? O3 H3A 0.9800 . ? C1 C2 1.456(4) 5_666 ? 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 O2 Cd1 123.7(2) . 8_655 ? C2 O2 Cd1 138.5(2) . 1_545 ? Cd1 O2 Cd1 96.92(8) 8_655 1_545 ? O2 C2 C1 134.6(3) . 5_666 ? O2 C2 C1 134.7(3) . . ? C1 C2 C1 90.7(3) 5_666 . ? O3 Cd1 O3 112.26(5) 3_655 . ? O3 Cd1 O3 101.87(7) 3_655 8_665 ? O3 Cd1 O3 88.17(7) . 8_665 ? O3 Cd1 O1 87.07(8) 3_655 . ? O3 Cd1 O1 95.66(9) . . ? O3 Cd1 O1 168.16(8) 8_665 . ? O3 Cd1 O2 163.87(8) 3_655 8_665 ? O3 Cd1 O2 80.66(7) . 8_665 ? O3 Cd1 O2 87.72(8) 8_665 8_665 ? O1 Cd1 O2 81.88(8) . 8_665 ? O3 Cd1 O2 83.55(8) 3_655 1_565 ? O3 Cd1 O2 161.59(8) . 1_565 ? O3 Cd1 O2 79.03(8) 8_665 1_565 ? O1 Cd1 O2 94.48(9) . 1_565 ? O2 Cd1 O2 85.63(7) 8_665 1_565 ? C1 O1 Cd1 126.65(19) . . ? Cd1 O3 Cd1 113.67(9) 3_645 . ? Cd1 O3 Cd1 122.07(10) 3_645 8_655 ? Cd1 O3 Cd1 103.34(8) . 8_655 ? Cd1 O3 H3A 105.5 3_645 . ? Cd1 O3 H3A 105.5 . . ? Cd1 O3 H3A 105.5 8_655 . ? O1 C1 C2 134.6(3) . 5_666 ? O1 C1 C2 136.1(3) . . ? C2 C1 C2 89.3(3) 5_666 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.951 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.267 # Attachment '732257.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 732257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H2 Cd2 O6' _chemical_formula_sum 'C4 H2 Cd2 O6' _chemical_formula_weight 370.86 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' 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 3.5793(3) _cell_length_b 10.4878(9) _cell_length_c 8.5834(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.5510(10) _cell_angle_gamma 90.00 _cell_volume 317.75(5) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1275 _cell_measurement_theta_min 3.093 _cell_measurement_theta_max 28.220 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 6.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.272 _exptl_absorpt_process_details 'SADABS(Brucker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1675 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 619 _reflns_number_gt 559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.022(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 619 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 0.5743(9) 0.5552(3) 0.6000(4) 0.0149(8) Uani 1 1 d . . . C2 C 0.3533(10) 0.5762(4) 0.4425(5) 0.0149(8) Uani 1 1 d . . . Cd1 Cd 1.21353(7) 0.62225(2) 0.92213(3) 0.01602(19) Uani 1 1 d . . . O1 O 0.6586(8) 0.6226(2) 0.7216(4) 0.0190(7) Uani 1 1 d . . . O2 O 0.1729(7) 0.6681(3) 0.3738(4) 0.0209(6) Uani 1 1 d . . . O3 O 1.7695(7) 0.5947(3) 1.0733(3) 0.0161(6) Uani 1 1 d . . . H3 H 1.8072 0.6393 1.1746 0.019 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0122(17) 0.019(2) 0.0134(17) -0.0004(15) 0.0008(15) -0.0018(14) C2 0.0129(17) 0.0154(19) 0.0170(18) -0.0002(15) 0.0045(15) -0.0041(15) Cd1 0.0122(2) 0.0149(3) 0.0204(2) 0.00309(10) 0.00085(14) 0.00015(9) O1 0.0176(14) 0.0210(17) 0.0174(14) -0.0043(11) -0.0006(12) 0.0005(9) O2 0.0232(14) 0.0135(15) 0.0226(14) 0.0027(14) -0.0065(12) 0.0019(11) O3 0.0152(13) 0.0195(15) 0.0124(14) -0.0026(11) -0.0007(12) 0.0007(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 C1 O1 1.255(5) . ? C1 C2 1.460(5) 3_666 ? C1 C2 1.465(5) . ? C2 O2 1.252(5) . ? C2 C1 1.460(5) 3_666 ? Cd1 O3 2.207(2) . ? Cd1 O3 2.231(3) 1_455 ? Cd1 O2 2.238(3) 4_676 ? Cd1 O3 2.277(4) 3_867 ? Cd1 O1 2.403(3) . ? Cd1 O1 2.532(3) 1_655 ? Cd1 Cd1 3.3730(5) 3_767 ? Cd1 Cd1 3.4144(5) 3_867 ? O1 Cd1 2.532(3) 1_455 ? O2 Cd1 2.238(3) 4_475 ? O3 Cd1 2.231(3) 1_655 ? O3 Cd1 2.277(4) 3_867 ? O3 H3 0.9766 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 135.3(3) . 3_666 ? O1 C1 C2 134.5(4) . . ? C2 C1 C2 90.1(3) 3_666 . ? O2 C2 C1 135.1(4) . 3_666 ? O2 C2 C1 135.0(4) . . ? C1 C2 C1 89.9(3) 3_666 . ? O3 Cd1 O3 107.52(11) . 1_455 ? O3 Cd1 O2 105.18(12) . 4_676 ? O3 Cd1 O2 101.78(12) 1_455 4_676 ? O3 Cd1 O3 80.81(12) . 3_867 ? O3 Cd1 O3 83.12(11) 1_455 3_867 ? O2 Cd1 O3 170.43(11) 4_676 3_867 ? O3 Cd1 O1 168.24(10) . . ? O3 Cd1 O1 80.37(10) 1_455 . ? O2 Cd1 O1 81.09(9) 4_676 . ? O3 Cd1 O1 91.75(8) 3_867 . ? O3 Cd1 O1 78.00(9) . 1_655 ? O3 Cd1 O1 170.04(10) 1_455 1_655 ? O2 Cd1 O1 84.34(9) 4_676 1_655 ? O3 Cd1 O1 89.73(8) 3_867 1_655 ? O1 Cd1 O1 92.97(11) . 1_655 ? O3 Cd1 Cd1 95.24(9) . 3_767 ? O3 Cd1 Cd1 42.08(9) 1_455 3_767 ? O2 Cd1 Cd1 143.19(8) 4_676 3_767 ? O3 Cd1 Cd1 41.04(6) 3_867 3_767 ? O1 Cd1 Cd1 84.83(7) . 3_767 ? O1 Cd1 Cd1 130.41(5) 1_655 3_767 ? O3 Cd1 Cd1 41.17(9) . 3_867 ? O3 Cd1 Cd1 96.59(8) 1_455 3_867 ? O2 Cd1 Cd1 145.77(7) 4_676 3_867 ? O3 Cd1 Cd1 39.65(6) 3_867 3_867 ? O1 Cd1 Cd1 130.78(6) . 3_867 ? O1 Cd1 Cd1 82.10(6) 1_655 3_867 ? Cd1 Cd1 Cd1 63.649(11) 3_767 3_867 ? C1 O1 Cd1 130.6(2) . . ? C1 O1 Cd1 118.2(2) . 1_455 ? Cd1 O1 Cd1 92.97(11) . 1_455 ? C2 O2 Cd1 131.1(3) . 4_475 ? Cd1 O3 Cd1 107.52(11) . 1_655 ? Cd1 O3 Cd1 99.19(12) . 3_867 ? Cd1 O3 Cd1 96.88(11) 1_655 3_867 ? Cd1 O3 H3 116.0 . . ? Cd1 O3 H3 116.7 1_655 . ? Cd1 O3 H3 117.6 3_867 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.038 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.237