Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_job _database_code_CSD 181534 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Louer, Daniel' 'Audebrand, Nathalie' 'Jeanneau, Erwann' _publ_contact_author_name 'Dr Daniel Louer' _publ_contact_author_address ; Laboratoire de Chimie du Solide et Inorganique Moleculaire UMR CNRS 6511, Inst de Chimie, Univ de Rennes I Avenue du General Leclerc Rennes 35042 cedex FRANCE ; _publ_contact_author_email 'DANIEL.LOUER@UNIV-RENNES1.FR' _publ_section_title ; Synthesis, crystal structure and thermal behaviour of CdZrK2(C2O4)5.8H2O ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Cd K2 O24 Zr' _chemical_formula_weight 778.03 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'tetragonal' _symmetry_space_group_name_H-M 'I-4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 11.216(5) _cell_length_b 11.216(5) _cell_length_c 8.954(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 1126.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 34.97 _exptl_crystal_description 'bipyramidal crystals' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.888 _exptl_absorpt_correction_type ? _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9787 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 34.96 _reflns_number_total 2482 _reflns_number_gt 2358 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0000P)^2^+0.4985P] 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 SHELXL _refine_ls_extinction_coef 0.0109(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(15) _refine_ls_number_reflns 2482 _refine_ls_number_parameters 94 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.5000 0.5000 0.5000 0.01385(7) Uani 1 4 d S . . Zr Zr 0.5000 1.0000 0.2500 0.00993(8) Uani 1 4 d S . . K1 K 0.5000 0.5000 0.0000 0.02395(18) Uani 1 4 d S . . K2 K 0.5000 1.0000 -0.2500 0.0274(3) Uani 1 4 d S . . O1 O 0.49630(11) 0.81210(10) 0.18908(15) 0.0209(3) Uani 1 1 d . . . O2 O 0.48843(12) 0.62189(11) 0.26682(14) 0.0244(3) Uani 1 1 d . . . C1 C 0.49471(14) 0.72934(13) 0.28841(17) 0.0154(3) Uani 1 1 d . . . O3 O 0.50183(13) 0.70404(11) 0.55358(14) 0.0232(3) Uani 1 1 d . . . O4 O 0.50433(11) 0.88886(10) 0.45828(12) 0.0192(2) Uani 1 1 d . . . C2 C 0.50044(14) 0.77625(14) 0.44890(17) 0.0155(3) Uani 1 1 d . . . OW1 O 0.70958(15) 0.6456(2) 0.0423(2) 0.0478(5) Uani 1 1 d . . . OW2 O 0.8587(2) 0.70657(15) 0.2921(2) 0.0472(5) Uani 1 1 d . . . H11 H 0.751(2) 0.595(2) -0.007(5) 0.050 Uiso 1 1 d D . . H12 H 0.743(2) 0.654(3) 0.120(3) 0.050 Uiso 1 1 d D . . H21 H 0.828(3) 0.743(2) 0.367(3) 0.050 Uiso 1 1 d D . . H22 H 0.911(2) 0.754(3) 0.248(4) 0.050 Uiso 1 1 d 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 Cd 0.01226(8) 0.01226(8) 0.01702(11) 0.000 0.000 0.000 Zr 0.00953(11) 0.00953(11) 0.01072(14) 0.000 0.000 0.000 K1 0.0280(3) 0.0280(3) 0.0159(3) 0.000 0.000 0.000 K2 0.0324(4) 0.0324(4) 0.0172(4) 0.000 0.000 0.000 O1 0.0339(7) 0.0140(5) 0.0149(5) 0.0007(4) -0.0008(5) -0.0008(5) O2 0.0412(7) 0.0113(5) 0.0207(6) -0.0021(4) 0.0008(5) -0.0005(5) C1 0.0184(7) 0.0116(6) 0.0162(6) -0.0023(5) 0.0011(6) 0.0004(5) O3 0.0397(7) 0.0138(5) 0.0159(5) 0.0014(4) -0.0021(5) 0.0001(5) O4 0.0316(6) 0.0111(4) 0.0147(5) -0.0007(4) 0.0001(4) -0.0006(4) C2 0.0175(7) 0.0132(6) 0.0157(6) 0.0020(5) -0.0018(6) 0.0000(5) OW1 0.0371(9) 0.0660(11) 0.0404(11) -0.0164(10) 0.0017(7) 0.0101(8) OW2 0.0666(12) 0.0361(9) 0.0387(9) 0.0022(8) 0.0160(10) -0.0080(8) _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 Cd O3 2.3384(16) ? ? Cd O3 2.3384(16) 4_656 ? Cd O3 2.3384(16) . ? Cd O3 2.3384(16) 3_566 ? Cd O3 2.3384(16) 2_665 ? Cd O2 2.4990(16) 3_566 ? Cd O2 2.4990(16) 2_665 ? Cd O2 2.4990(16) 4_656 ? Cd O2 2.4990(16) . ? Cd O2 2.4990(16) ? ? Zr O1 2.1774(15) . ? Zr O1 2.1774(15) 8_655 ? Zr O1 2.1774(15) 7_465 ? Zr O1 2.1774(15) 2_675 ? Zr O4 2.2437(14) 2_675 ? Zr O4 2.2437(14) 7_465 ? Zr O4 2.2437(14) 8_655 ? Zr O4 2.2437(14) . ? K1 O2 2.7556(17) ? ? K1 O2 2.7556(17) 4_655 ? K1 O2 2.7556(17) . ? K1 O2 2.7556(17) 2_665 ? K1 O2 2.7556(17) 3_565 ? K1 OW1 2.887(2) . ? K1 OW1 2.887(2) 2_665 ? K1 OW1 2.887(2) 3_565 ? K1 OW1 2.887(2) 4_655 ? K1 H11 3.01(3) . ? K2 OW2 2.832(2) 4_655 ? K2 OW2 2.832(2) 3_575 ? K2 OW2 2.832(2) 5_454 ? K2 OW2 2.832(2) 6_664 ? K2 O4 2.8947(17) 1_554 ? K2 O4 2.8947(17) 8_655 ? K2 O4 2.8947(17) 2_674 ? K2 O4 2.8947(17) 7_465 ? O1 C1 1.286(2) . ? O1 O4 2.561(2) . ? O1 O4 2.726(2) 7_465 ? O1 O4 2.837(2) 8_655 ? O1 O1 3.174(2) 8_655 ? O2 C1 1.2227(19) . ? O2 O3 2.732(2) . ? O2 O2 2.746(3) 2_665 ? O2 O3 3.010(2) 4_656 ? O2 OW1 3.204(2) . ? O2 O3 3.219(2) 3_566 ? O2 OW1 3.300(3) 4_655 ? C1 C2 1.5317(19) . ? O3 C2 1.239(2) . ? O3 O3 3.376(2) 4_656 ? O4 C2 1.267(2) . ? O4 O4 2.495(3) 2_675 ? O4 K2 2.8947(17) 1_556 ? O4 OW2 3.272(2) 4_656 ? O4 OW2 3.527(3) 6_665 ? O4 OW2 4.261(3) 3_576 ? OW1 OW1 4.118(3) 3_565 ? OW1 O2 4.239(3) 2_665 ? OW1 H11 0.86(3) . ? OW1 H12 0.80(2) . ? OW2 K2 2.832(2) 5_545 ? OW2 OW2 4.041(3) 7_565 ? OW2 H21 0.85(3) . ? OW2 H22 0.89(3) . ? 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 O3 Cd O3 180.0 ? 4_656 ? O3 Cd O3 87.587(13) ? . ? O3 Cd O3 92.413(13) 4_656 . ? O3 Cd O3 23.68(6) ? 3_566 ? O3 Cd O3 156.32(6) 4_656 3_566 ? O3 Cd O3 92.413(13) . 3_566 ? O3 Cd O3 87.587(13) ? 2_665 ? O3 Cd O3 92.413(13) 4_656 2_665 ? O3 Cd O3 156.32(6) . 2_665 ? O3 Cd O3 92.413(13) 3_566 2_665 ? O3 Cd O2 45.06(4) ? 3_566 ? O3 Cd O2 134.94(4) 4_656 3_566 ? O3 Cd O2 76.88(4) . 3_566 ? O3 Cd O2 68.68(5) 3_566 3_566 ? O3 Cd O2 83.35(5) 2_665 3_566 ? O3 Cd O2 96.65(5) ? 2_665 ? O3 Cd O2 83.35(5) 4_656 2_665 ? O3 Cd O2 134.94(4) . 2_665 ? O3 Cd O2 76.88(4) 3_566 2_665 ? O3 Cd O2 68.68(5) 2_665 2_665 ? O2 Cd O2 134.27(4) 3_566 2_665 ? O3 Cd O2 111.32(5) ? 4_656 ? O3 Cd O2 68.68(5) 4_656 4_656 ? O3 Cd O2 83.35(5) . 4_656 ? O3 Cd O2 134.94(4) 3_566 4_656 ? O3 Cd O2 76.88(4) 2_665 4_656 ? O2 Cd O2 66.67(7) 3_566 4_656 ? O2 Cd O2 134.27(4) 2_665 4_656 ? O3 Cd O2 103.12(4) ? . ? O3 Cd O2 76.88(4) 4_656 . ? O3 Cd O2 68.68(5) . . ? O3 Cd O2 83.35(5) 3_566 . ? O3 Cd O2 134.94(4) 2_665 . ? O2 Cd O2 134.27(4) 3_566 . ? O2 Cd O2 66.67(7) 2_665 . ? O2 Cd O2 134.27(4) 4_656 . ? O3 Cd O2 68.68(5) ? ? ? O3 Cd O2 111.32(5) 4_656 ? ? O3 Cd O2 96.65(5) . ? ? O3 Cd O2 45.06(4) 3_566 ? ? O3 Cd O2 103.12(4) 2_665 ? ? O2 Cd O2 113.33(7) 3_566 ? ? O2 Cd O2 45.73(4) 2_665 ? ? O2 Cd O2 180.0 4_656 ? ? O2 Cd O2 45.73(4) . ? ? O1 Zr O1 93.599(18) . 8_655 ? O1 Zr O1 93.599(18) . 7_465 ? O1 Zr O1 150.98(7) 8_655 7_465 ? O1 Zr O1 150.98(7) . 2_675 ? O1 Zr O1 93.599(18) 8_655 2_675 ? O1 Zr O1 93.599(18) 7_465 2_675 ? O1 Zr O4 138.21(5) . 2_675 ? O1 Zr O4 79.82(5) 8_655 2_675 ? O1 Zr O4 76.13(5) 7_465 2_675 ? O1 Zr O4 70.79(5) 2_675 2_675 ? O1 Zr O4 76.13(5) . 7_465 ? O1 Zr O4 138.21(5) 8_655 7_465 ? O1 Zr O4 70.79(5) 7_465 7_465 ? O1 Zr O4 79.82(5) 2_675 7_465 ? O4 Zr O4 133.70(4) 2_675 7_465 ? O1 Zr O4 79.82(5) . 8_655 ? O1 Zr O4 70.79(5) 8_655 8_655 ? O1 Zr O4 138.21(5) 7_465 8_655 ? O1 Zr O4 76.13(5) 2_675 8_655 ? O4 Zr O4 133.70(4) 2_675 8_655 ? O4 Zr O4 67.56(7) 7_465 8_655 ? O1 Zr O4 70.79(5) . . ? O1 Zr O4 76.13(5) 8_655 . ? O1 Zr O4 79.82(5) 7_465 . ? O1 Zr O4 138.21(5) 2_675 . ? O4 Zr O4 67.56(7) 2_675 . ? O4 Zr O4 133.70(4) 7_465 . ? O4 Zr O4 133.70(4) 8_655 . ? O2 K1 O2 180.0 ? 4_655 ? O2 K1 O2 41.27(4) ? . ? O2 K1 O2 138.73(4) 4_655 . ? O2 K1 O2 41.27(4) ? 2_665 ? O2 K1 O2 138.73(4) 4_655 2_665 ? O2 K1 O2 59.78(6) . 2_665 ? O2 K1 O2 120.22(6) ? 3_565 ? O2 K1 O2 59.78(6) 4_655 3_565 ? O2 K1 O2 138.73(4) . 3_565 ? O2 K1 O2 138.73(4) 2_665 3_565 ? O2 K1 OW1 57.02(5) ? . ? O2 K1 OW1 122.98(5) 4_655 . ? O2 K1 OW1 69.14(5) . . ? O2 K1 OW1 97.38(5) 2_665 . ? O2 K1 OW1 71.54(5) 3_565 . ? O2 K1 OW1 108.46(5) ? 2_665 ? O2 K1 OW1 71.54(5) 4_655 2_665 ? O2 K1 OW1 97.38(5) . 2_665 ? O2 K1 OW1 69.14(5) 2_665 2_665 ? O2 K1 OW1 122.98(5) 3_565 2_665 ? OW1 K1 OW1 164.91(7) . 2_665 ? O2 K1 OW1 82.62(5) ? 3_565 ? O2 K1 OW1 97.38(5) 4_655 3_565 ? O2 K1 OW1 122.98(5) . 3_565 ? O2 K1 OW1 71.54(5) 2_665 3_565 ? O2 K1 OW1 69.14(5) 3_565 3_565 ? OW1 K1 OW1 90.988(10) . 3_565 ? OW1 K1 OW1 90.988(10) 2_665 3_565 ? O2 K1 OW1 110.86(5) ? 4_655 ? O2 K1 OW1 69.14(5) 4_655 4_655 ? O2 K1 OW1 71.54(5) . 4_655 ? O2 K1 OW1 122.98(5) 2_665 4_655 ? O2 K1 OW1 97.38(5) 3_565 4_655 ? OW1 K1 OW1 90.988(10) . 4_655 ? OW1 K1 OW1 90.988(10) 2_665 4_655 ? OW1 K1 OW1 164.91(7) 3_565 4_655 ? O2 K1 H11 62.4(8) ? . ? O2 K1 H11 117.6(8) 4_655 . ? O2 K1 H11 83.5(8) . . ? O2 K1 H11 98.6(8) 2_665 . ? O2 K1 H11 60.1(9) 3_565 . ? OW1 K1 H11 16.5(6) . . ? OW1 K1 H11 164.6(5) 2_665 . ? OW1 K1 H11 75.9(5) 3_565 . ? OW1 K1 H11 103.8(5) 4_655 . ? OW2 K2 OW2 164.69(8) 4_655 3_575 ? OW2 K2 OW2 91.017(11) 4_655 5_454 ? OW2 K2 OW2 91.017(11) 3_575 5_454 ? OW2 K2 OW2 91.017(10) 4_655 6_664 ? OW2 K2 OW2 91.017(11) 3_575 6_664 ? OW2 K2 OW2 164.69(8) 5_454 6_664 ? OW2 K2 O4 69.67(4) 4_655 1_554 ? OW2 K2 O4 96.14(5) 3_575 1_554 ? OW2 K2 O4 118.81(5) 5_454 1_554 ? OW2 K2 O4 76.03(5) 6_664 1_554 ? OW2 K2 O4 118.81(5) 4_655 8_655 ? OW2 K2 O4 76.03(5) 3_575 8_655 ? OW2 K2 O4 96.14(5) 5_454 8_655 ? OW2 K2 O4 69.67(4) 6_664 8_655 ? O4 K2 O4 144.51(4) 1_554 8_655 ? OW2 K2 O4 96.14(5) 4_655 2_674 ? OW2 K2 O4 69.67(4) 3_575 2_674 ? OW2 K2 O4 76.03(5) 5_454 2_674 ? OW2 K2 O4 118.81(5) 6_664 2_674 ? O4 K2 O4 51.06(6) 1_554 2_674 ? O4 K2 O4 144.51(4) 8_655 2_674 ? OW2 K2 O4 76.03(5) 4_655 7_465 ? OW2 K2 O4 118.81(5) 3_575 7_465 ? OW2 K2 O4 69.67(4) 5_454 7_465 ? OW2 K2 O4 96.14(5) 6_664 7_465 ? O4 K2 O4 144.51(4) 1_554 7_465 ? O4 K2 O4 51.06(6) 8_655 7_465 ? O4 K2 O4 144.51(4) 2_674 7_465 ? C1 O1 Zr 121.72(11) . . ? C1 O1 O4 65.93(9) . . ? Zr O1 O4 55.82(4) . . ? C1 O1 O4 150.92(11) . 7_465 ? Zr O1 O4 53.03(4) . 7_465 ? O4 O1 O4 102.54(6) . 7_465 ? C1 O1 O4 151.25(11) . 8_655 ? Zr O1 O4 51.12(4) . 8_655 ? O4 O1 O4 99.57(6) . 8_655 ? O4 O1 O4 53.25(5) 7_465 8_655 ? C1 O1 O1 103.98(12) . 8_655 ? Zr O1 O1 43.201(9) . 8_655 ? O4 O1 O1 55.53(5) . 8_655 ? O4 O1 O1 88.51(4) 7_465 8_655 ? O4 O1 O1 50.05(4) 8_655 8_655 ? C1 O2 Cd 113.84(11) . . ? C1 O2 O3 61.04(9) . . ? Cd O2 O3 52.88(5) . . ? C1 O2 O2 167.39(12) . 2_665 ? Cd O2 O2 56.67(3) . 2_665 ? O3 O2 O2 109.30(4) . 2_665 ? C1 O2 K1 128.57(11) . . ? Cd O2 K1 116.78(6) . . ? O3 O2 K1 168.38(6) . . ? O2 O2 K1 60.11(3) 2_665 . ? C1 O2 O3 113.44(12) . 4_656 ? Cd O2 O3 49.17(4) . 4_656 ? O3 O2 O3 71.83(5) . 4_656 ? O2 O2 O3 67.82(5) 2_665 4_656 ? K1 O2 O3 105.96(6) . 4_656 ? C1 O2 OW1 88.44(11) . . ? Cd O2 OW1 121.96(6) . . ? O3 O2 OW1 121.27(7) . . ? O2 O2 OW1 90.54(6) 2_665 . ? K1 O2 OW1 57.37(5) . . ? O3 O2 OW1 158.07(6) 4_656 . ? C1 O2 O3 107.62(11) . 3_566 ? Cd O2 O3 46.19(3) . 3_566 ? O3 O2 O3 68.56(5) . 3_566 ? O2 O2 O3 59.99(5) 2_665 3_566 ? K1 O2 O3 100.60(5) . 3_566 ? O3 O2 O3 94.53(6) 4_656 3_566 ? OW1 O2 O3 76.56(6) . 3_566 ? C1 O2 OW1 82.25(10) . 4_655 ? Cd O2 OW1 152.57(6) . 4_655 ? O3 O2 OW1 135.47(6) . 4_655 ? O2 O2 OW1 109.86(5) 2_665 4_655 ? K1 O2 OW1 56.08(5) . 4_655 ? O3 O2 OW1 104.76(7) 4_656 4_655 ? OW1 O2 OW1 78.56(5) . 4_655 ? O3 O2 OW1 152.85(6) 3_566 4_655 ? O2 C1 O1 127.09(15) . . ? O2 C1 C2 119.30(13) . . ? O1 C1 C2 113.61(12) . . ? C2 O3 Cd 118.98(10) . . ? C2 O3 O2 60.57(9) . . ? Cd O3 O2 58.44(4) . . ? C2 O3 O3 102.44(12) . 4_656 ? Cd O3 O3 43.794(7) . 4_656 ? O2 O3 O3 57.90(4) . 4_656 ? C2 O4 Zr 119.88(10) . . ? C2 O4 O4 174.33(12) . 2_675 ? Zr O4 O4 56.22(3) . 2_675 ? C2 O4 O1 66.49(9) . . ? Zr O4 O1 53.40(5) . . ? O4 O4 O1 109.54(4) 2_675 . ? C2 O4 K2 119.26(10) . 1_556 ? Zr O4 K2 120.69(6) . 1_556 ? O4 O4 K2 64.47(3) 2_675 1_556 ? O1 O4 K2 173.43(5) . 1_556 ? C2 O4 OW2 85.26(10) . 4_656 ? Zr O4 OW2 127.55(6) . 4_656 ? O4 O4 OW2 94.31(6) 2_675 4_656 ? O1 O4 OW2 125.64(6) . 4_656 ? K2 O4 OW2 54.27(4) 1_556 4_656 ? C2 O4 OW2 76.62(9) . 6_665 ? Zr O4 OW2 151.94(6) . 6_665 ? O4 O4 OW2 108.67(4) 2_675 6_665 ? O1 O4 OW2 135.31(6) . 6_665 ? K2 O4 OW2 51.19(5) 1_556 6_665 ? OW2 O4 OW2 72.82(5) 4_656 6_665 ? C2 O4 OW2 135.70(10) . 3_576 ? Zr O4 OW2 94.49(5) . 3_576 ? O4 O4 OW2 49.97(4) 2_675 3_576 ? O1 O4 OW2 137.37(5) . 3_576 ? K2 O4 OW2 41.37(3) 1_556 3_576 ? OW2 O4 OW2 95.47(7) 4_656 3_576 ? OW2 O4 OW2 61.66(4) 6_665 3_576 ? O3 C2 O4 126.96(15) . . ? O3 C2 C1 119.07(12) . . ? O4 C2 C1 113.97(12) . . ? K1 OW1 O2 53.49(4) . . ? K1 OW1 OW1 44.506(5) . 3_565 ? O2 OW1 OW1 84.28(4) . 3_565 ? K1 OW1 O2 40.14(4) . 2_665 ? O2 OW1 O2 40.38(4) . 2_665 ? OW1 OW1 O2 46.49(4) 3_565 2_665 ? K1 OW1 H11 89.6(18) . . ? O2 OW1 H11 133.3(19) . . ? OW1 OW1 H11 49.8(18) 3_565 . ? O2 OW1 H11 93(2) 2_665 . ? K1 OW1 H12 124.5(19) . . ? O2 OW1 H12 79.9(19) . . ? OW1 OW1 H12 111(2) 3_565 . ? O2 OW1 H12 85(2) 2_665 . ? H11 OW1 H12 106(3) . . ? K2 OW2 OW2 44.492(5) 5_545 7_565 ? K2 OW2 H21 135.9(17) 5_545 . ? OW2 OW2 H21 128(2) 7_565 . ? K2 OW2 H22 93.5(19) 5_545 . ? OW2 OW2 H22 52.0(18) 7_565 . ? H21 OW2 H22 109(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 34.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.492 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.078