Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Riou, D.' 'Barthelet, K.' 'Ferey, G.' 'Merlier, C.' 'Riou-Cavellee, M.' 'Serre, C.' _publ_contact_author_name 'Dr D Riou' _publ_contact_author_address ; Institut Lavoisier UMR 8637 Universite de Versailles 45 Avenue des Etats-Unis Versailles 78035 FRANCE ; _publ_contact_author_email 'RIOU@CHIMIE.UVSQ.FR' _publ_section_title ; Microporous Hybrid Compounds: Hydrothermal Synthesis and Characterization of two zincomethylendiphosphonates with 3D Structures ; data_VSB3(Zn) _database_code_CSD 174227 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H2 O7 P2 Zn2' _chemical_formula_weight 318.71 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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/c 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' '-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 18.7573(3) _cell_length_b 8.2803(2) _cell_length_c 8.92250(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.8150(10) _cell_angle_gamma 90.00 _cell_volume 1326.56(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 3.269(2) _exptl_crystal_density_diffrn 3.192 _exptl_crystal_density_method ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 7.707 _exptl_absorpt_correction_type 'Semi empirical' _exptl_absorpt_correction_T_min 0.495376 _exptl_absorpt_correction_T_max 0.276218 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 4564 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 29.80 _reflns_number_total 1735 _reflns_number_observed 1598 _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^)+(0.0393P)^2^+3.3028P] 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 SHELXL _refine_ls_extinction_coef 0.0064(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1735 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_obs 0.0269 _refine_ls_wR_factor_all 0.0719 _refine_ls_wR_factor_obs 0.0704 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -0.001 _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 Zn1 Zn 0.0000 0.02716(5) 0.7500 0.00927(13) Uani 1 d S . Zn2 Zn -0.2500 -0.7500 0.5000 0.00905(13) Uani 1 d S . Zn3 Zn -0.18627(2) -0.11156(4) 0.56647(4) 0.00942(12) Uani 1 d . . P4 P -0.19372(4) -0.45556(8) 0.75833(7) 0.0069(2) Uani 1 d . . P5 P -0.09348(4) -0.17796(8) 0.92493(7) 0.0075(2) Uani 1 d . . O1 O -0.11660(12) -0.2250(3) 0.4612(2) 0.0158(4) Uani 1 d . . O2 O -0.22070(11) -0.3300(2) 0.6283(2) 0.0101(4) Uani 1 d . . O3 O -0.18295(11) -0.6217(2) 0.6970(2) 0.0100(4) Uani 1 d . . O4 O -0.25393(11) -0.9544(2) 0.6373(2) 0.0109(4) Uani 1 d . . O5 O -0.16093(11) -0.8815(2) 0.4716(2) 0.0105(4) Uani 1 d . . O6 O -0.08764(11) -0.0951(2) 0.7732(2) 0.0109(4) Uani 1 d . . O7 O 0.02181(11) 0.1551(3) 0.9414(2) 0.0116(4) Uani 1 d . . C C -0.1034(2) -0.3902(3) 0.8820(3) 0.0111(5) Uani 1 d . . H0A H -0.0928(2) -0.4486(3) 0.9803(3) 0.013 Uiso 1 calc R . H0B H -0.0660(2) -0.4212(3) 0.8318(3) 0.013 Uiso 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 Zn1 0.0077(2) 0.0123(2) 0.0079(2) 0.000 0.0024(2) 0.000 Zn2 0.0087(2) 0.0093(2) 0.0098(2) 0.0001(2) 0.0036(2) 0.00121(15) Zn3 0.0082(2) 0.0099(2) 0.0103(2) 0.00022(11) 0.00296(12) 0.00023(11) P4 0.0066(3) 0.0078(3) 0.0060(3) -0.0002(2) 0.0015(2) -0.0004(2) P5 0.0056(3) 0.0095(3) 0.0073(3) -0.0007(2) 0.0017(2) -0.0008(2) O1 0.0125(10) 0.0194(11) 0.0175(10) -0.0064(8) 0.0073(8) -0.0024(8) O2 0.0102(9) 0.0108(9) 0.0082(8) 0.0025(7) 0.0012(7) -0.0016(7) O3 0.0103(9) 0.0100(9) 0.0086(8) -0.0011(7) 0.0008(7) 0.0011(7) O4 0.0104(10) 0.0123(10) 0.0114(9) 0.0005(7) 0.0052(7) 0.0014(7) O5 0.0084(9) 0.0114(9) 0.0133(9) 0.0011(7) 0.0055(7) 0.0002(7) O6 0.0091(9) 0.0149(10) 0.0086(8) 0.0007(7) 0.0023(7) -0.0030(7) O7 0.0073(9) 0.0169(10) 0.0095(8) -0.0030(7) 0.0006(7) -0.0013(7) C 0.0092(12) 0.0091(12) 0.0133(12) 0.0001(10) 0.0006(10) 0.0011(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 Zn1 O7 1.950(2) . ? Zn1 O7 1.950(2) 2_556 ? Zn1 O6 1.992(2) 2_556 ? Zn1 O6 1.992(2) . ? Zn2 O5 2.070(2) . ? Zn2 O5 2.070(2) 7_436 ? Zn2 O4 2.103(2) . ? Zn2 O4 2.103(2) 7_436 ? Zn2 O3 2.126(2) 7_436 ? Zn2 O3 2.126(2) . ? Zn3 O4 2.041(2) 1_565 ? Zn3 O1 2.045(2) . ? Zn3 O2 2.049(2) . ? Zn3 O2 2.132(2) 7_446 ? Zn3 O5 2.192(2) 1_565 ? Zn3 O6 2.207(2) . ? P4 O3 1.516(2) . ? P4 O2 1.531(2) . ? P4 O4 1.536(2) 4_456 ? P4 C 1.816(3) . ? P5 O5 1.523(2) 6_546 ? P5 O7 1.529(2) 5_557 ? P5 O6 1.550(2) . ? P5 C 1.797(3) . ? O2 Zn3 2.132(2) 7_446 ? O4 P4 1.536(2) 4_446 ? O4 Zn3 2.041(2) 1_545 ? O5 P5 1.523(2) 6_545 ? O5 Zn3 2.192(2) 1_545 ? O7 P5 1.529(2) 5_557 ? C H0A 0.97 . ? C H0B 0.97 . ? 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 O7 Zn1 O7 114.20(13) . 2_556 ? O7 Zn1 O6 113.38(8) . 2_556 ? O7 Zn1 O6 98.94(8) 2_556 2_556 ? O7 Zn1 O6 98.94(8) . . ? O7 Zn1 O6 113.38(8) 2_556 . ? O6 Zn1 O6 118.89(12) 2_556 . ? O5 Zn2 O5 180.0 . 7_436 ? O5 Zn2 O4 79.27(8) . . ? O5 Zn2 O4 100.73(8) 7_436 . ? O5 Zn2 O4 100.73(8) . 7_436 ? O5 Zn2 O4 79.27(8) 7_436 7_436 ? O4 Zn2 O4 179.999(1) . 7_436 ? O5 Zn2 O3 86.63(8) . 7_436 ? O5 Zn2 O3 93.37(8) 7_436 7_436 ? O4 Zn2 O3 88.14(8) . 7_436 ? O4 Zn2 O3 91.86(7) 7_436 7_436 ? O5 Zn2 O3 93.37(7) . . ? O5 Zn2 O3 86.63(8) 7_436 . ? O4 Zn2 O3 91.86(8) . . ? O4 Zn2 O3 88.14(8) 7_436 . ? O3 Zn2 O3 180.0 7_436 . ? O4 Zn3 O1 166.43(9) 1_565 . ? O4 Zn3 O2 101.92(8) 1_565 . ? O1 Zn3 O2 90.65(9) . . ? O4 Zn3 O2 87.80(8) 1_565 7_446 ? O1 Zn3 O2 90.13(8) . 7_446 ? O2 Zn3 O2 76.81(8) . 7_446 ? O4 Zn3 O5 77.85(8) 1_565 1_565 ? O1 Zn3 O5 89.03(8) . 1_565 ? O2 Zn3 O5 172.55(7) . 1_565 ? O2 Zn3 O5 95.75(7) 7_446 1_565 ? O4 Zn3 O6 98.50(8) 1_565 . ? O1 Zn3 O6 85.39(8) . . ? O2 Zn3 O6 94.74(7) . . ? O2 Zn3 O6 170.41(8) 7_446 . ? O5 Zn3 O6 92.65(7) 1_565 . ? O3 P4 O2 113.12(11) . . ? O3 P4 O4 113.55(12) . 4_456 ? O2 P4 O4 109.02(11) . 4_456 ? O3 P4 C 106.94(12) . . ? O2 P4 C 107.69(12) . . ? O4 P4 C 106.10(12) 4_456 . ? O5 P5 O7 111.06(11) 6_546 5_557 ? O5 P5 O6 111.70(11) 6_546 . ? O7 P5 O6 110.98(11) 5_557 . ? O5 P5 C 109.34(13) 6_546 . ? O7 P5 C 107.52(12) 5_557 . ? O6 P5 C 106.02(12) . . ? P4 O2 Zn3 137.97(12) . . ? P4 O2 Zn3 118.47(11) . 7_446 ? Zn3 O2 Zn3 103.19(8) . 7_446 ? P4 O3 Zn2 130.02(12) . . ? P4 O4 Zn3 138.37(13) 4_446 1_545 ? P4 O4 Zn2 119.62(11) 4_446 . ? Zn3 O4 Zn2 101.70(8) 1_545 . ? P5 O5 Zn2 128.83(12) 6_545 . ? P5 O5 Zn3 132.56(12) 6_545 1_545 ? Zn2 O5 Zn3 97.86(8) . 1_545 ? P5 O6 Zn1 125.79(12) . . ? P5 O6 Zn3 116.67(11) . . ? Zn1 O6 Zn3 117.53(9) . . ? P5 O7 Zn1 131.67(13) 5_557 . ? P5 C P4 116.22(15) . . ? P5 C H0A 108.23(9) . . ? P4 C H0A 108.23(9) . . ? P5 C H0B 108.23(10) . . ? P4 C H0B 108.23(9) . . ? H0A C H0B 107.4 . . ? _refine_diff_density_max 0.889 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.161 data_MIL48 _database_code_CSD 174228 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H2 Na O8.50 P2 Zn2' _chemical_formula_weight 365.70 _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' 'O' 'O' 0.0106 0.0060 '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.9929(9) _cell_length_b 5.5093(6) _cell_length_c 18.025(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.376(2) _cell_angle_gamma 90.00 _cell_volume 892.3(2) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 2.74(5) _exptl_crystal_density_diffrn 2.722 _exptl_crystal_density_method ? _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 5.803 _exptl_absorpt_correction_type 'Semi empirical' _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.707244 _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 5898 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.1633 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 29.91 _reflns_number_total 2358 _reflns_number_observed 1283 _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^)+(0.0382P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2358 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1620 _refine_ls_R_factor_obs 0.0700 _refine_ls_wR_factor_all 0.1379 _refine_ls_wR_factor_obs 0.1078 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.145 _refine_ls_shift/esd_max 0.066 _refine_ls_shift/esd_mean 0.004 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 Zn1 Zn 0.09324(12) 0.7526(2) 0.06564(5) 0.0162(3) Uani 1 d . . Zn2 Zn 0.38968(12) 0.0227(2) -0.22814(6) 0.0162(3) Uani 1 d . . P1 P 0.1472(2) 0.2395(5) 0.15465(12) 0.0135(5) Uani 1 d . . P2 P 0.1687(3) -0.0964(5) -0.09835(12) 0.0143(5) Uani 1 d . . Na Na 0.3177(4) 0.3564(8) -0.0035(2) 0.0280(10) Uani 1 d . . O1 O 0.2008(6) 0.9950(12) 0.1253(3) 0.023(2) Uani 1 d . . O2 O 0.3243(6) -0.0784(12) -0.1302(3) 0.020(2) Uani 1 d . . O3 O -0.1141(7) 0.8445(12) 0.0749(3) 0.0195(15) Uani 1 d . . O4 O 0.1619(7) 0.4348(11) 0.0960(3) 0.024(2) Uani 1 d . . O5 O 0.5625(7) 0.2344(12) -0.2140(3) 0.0202(15) Uani 1 d . . O6 O 0.1720(7) 0.7250(12) -0.0338(3) 0.0183(14) Uani 1 d . . O7 O 0.2251(7) 0.1989(12) -0.2720(3) 0.024(2) Uani 1 d . . C C -0.0468(9) 0.2098(17) 0.1716(4) 0.015(2) Uani 1 d . . HA H -0.0558(9) 0.1039(17) 0.2142(4) 0.019 Uiso 1 calc R . HB H -0.0831(9) 0.3683(17) 0.1857(4) 0.019 Uiso 1 calc R . OW1 O 0.5126(7) 0.4926(13) 0.0880(3) 0.028(2) Uani 1 d . . OW2 O 0.4784(104) -0.0117(231) 0.0132(49) 0.075(18) Uani 0.50 d P . 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 Zn1 0.0193(6) 0.0143(6) 0.0149(5) 0.0004(5) 0.0005(4) 0.0024(5) Zn2 0.0170(6) 0.0166(6) 0.0149(5) 0.0005(5) 0.0006(4) 0.0012(5) P1 0.0154(12) 0.0123(12) 0.0128(11) 0.0019(11) -0.0007(9) -0.0001(10) P2 0.0139(12) 0.0173(14) 0.0116(12) -0.0002(10) -0.0006(9) 0.0004(10) Na 0.026(2) 0.031(2) 0.027(2) -0.006(2) 0.005(2) 0.004(2) O1 0.017(3) 0.018(4) 0.034(4) -0.009(3) -0.003(3) -0.005(3) O2 0.013(3) 0.033(5) 0.014(3) 0.006(3) 0.004(3) -0.001(3) O3 0.018(3) 0.015(4) 0.025(4) -0.002(3) -0.005(3) 0.000(3) O4 0.023(4) 0.019(4) 0.030(4) 0.017(3) 0.008(3) 0.003(3) O5 0.020(4) 0.019(4) 0.022(3) 0.003(3) -0.004(3) -0.005(3) O6 0.022(4) 0.021(4) 0.012(3) 0.005(3) 0.006(3) 0.011(3) O7 0.019(4) 0.031(5) 0.021(3) 0.003(3) -0.004(3) 0.005(3) C 0.023(5) 0.018(6) 0.006(4) 0.001(4) 0.005(4) -0.003(4) OW1 0.030(4) 0.032(5) 0.022(4) 0.002(3) 0.000(3) 0.002(3) OW2 0.076(48) 0.054(21) 0.089(54) 0.005(37) -0.043(29) 0.019(33) _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 Zn1 O4 1.929(6) . ? Zn1 O1 1.947(6) . ? Zn1 O3 1.946(6) . ? Zn1 O6 1.961(5) . ? Zn1 Na 3.256(4) . ? Zn2 O7 1.913(6) . ? Zn2 O5 1.951(6) . ? Zn2 O5 1.957(6) 2_644 ? Zn2 O2 1.964(6) . ? P1 O7 1.509(6) 4_566 ? P1 O4 1.518(6) . ? P1 O1 1.532(7) 1_545 ? P1 C 1.791(9) . ? P1 Na 3.355(4) . ? P2 O6 1.523(6) 1_545 ? P2 O3 1.537(7) 3_565 ? P2 O2 1.537(6) . ? P2 C 1.794(8) 3 ? P2 Na 3.279(5) . ? Na OW1 2.352(7) 3_665 ? Na O4 2.362(7) . ? Na O3 2.457(7) 3_565 ? Na O6 2.466(7) . ? Na OW2 2.50(12) . ? Na OW1 2.472(7) . ? Na OW2 2.65(11) 3_655 ? Na Na 3.637(8) 3_665 ? O1 P1 1.532(7) 1_565 ? O3 P2 1.537(7) 3_565 ? O3 Na 2.457(7) 3_565 ? O5 Zn2 1.957(6) 2_654 ? O6 P2 1.523(6) 1_565 ? O7 P1 1.509(6) 4_565 ? C P2 1.794(8) 3 ? C HA 0.97 . ? C HB 0.97 . ? OW1 Na 2.351(7) 3_665 ? OW2 OW2 0.64(12) 3_655 ? OW2 Na 2.65(11) 3_655 ? 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 O4 Zn1 O1 108.7(3) . . ? O4 Zn1 O3 120.6(3) . . ? O1 Zn1 O3 103.3(3) . . ? O4 Zn1 O6 93.8(3) . . ? O1 Zn1 O6 111.6(3) . . ? O3 Zn1 O6 118.8(2) . . ? O4 Zn1 Na 45.9(2) . . ? O1 Zn1 Na 111.7(2) . . ? O3 Zn1 Na 145.0(2) . . ? O6 Zn1 Na 49.1(2) . . ? O7 Zn2 O5 110.4(3) . . ? O7 Zn2 O5 112.0(3) . 2_644 ? O5 Zn2 O5 111.28(13) . 2_644 ? O7 Zn2 O2 105.1(3) . . ? O5 Zn2 O2 108.6(2) . . ? O5 Zn2 O2 109.2(3) 2_644 . ? O7 P1 O4 113.6(4) 4_566 . ? O7 P1 O1 111.0(4) 4_566 1_545 ? O4 P1 O1 110.2(4) . 1_545 ? O7 P1 C 106.9(4) 4_566 . ? O4 P1 C 107.3(4) . . ? O1 P1 C 107.5(4) 1_545 . ? O7 P1 Na 119.3(3) 4_566 . ? O4 P1 Na 38.4(2) . . ? O1 P1 Na 73.4(3) 1_545 . ? C P1 Na 130.2(3) . . ? O6 P2 O3 111.7(3) 1_545 3_565 ? O6 P2 O2 109.8(3) 1_545 . ? O3 P2 O2 110.5(4) 3_565 . ? O6 P2 C 109.2(4) 1_545 3 ? O3 P2 C 108.9(4) 3_565 3 ? O2 P2 C 106.6(4) . 3 ? O6 P2 Na 95.7(3) 1_545 . ? O3 P2 Na 45.4(2) 3_565 . ? O2 P2 Na 77.7(3) . . ? C P2 Na 150.8(3) 3 . ? OW1 Na O4 148.1(3) 3_665 . ? OW1 Na O3 108.0(3) 3_665 3_565 ? O4 Na O3 91.6(2) . 3_565 ? OW1 Na O6 85.3(3) 3_665 . ? O4 Na O6 72.0(2) . . ? O3 Na O6 82.9(2) 3_565 . ? OW1 Na OW2 88.7(15) 3_665 . ? O4 Na OW2 114.5(15) . . ? O3 Na OW2 96.4(28) 3_565 . ? O6 Na OW2 173.5(15) . . ? OW1 Na OW1 82.1(2) 3_665 . ? O4 Na OW1 82.2(2) . . ? O3 Na OW1 168.0(3) 3_565 . ? O6 Na OW1 104.7(3) . . ? OW2 Na OW1 77.0(28) . . ? OW1 Na OW2 75.0(16) 3_665 3_655 ? O4 Na OW2 128.0(16) . 3_655 ? O3 Na OW2 98.3(26) 3_565 3_655 ? O6 Na OW2 159.8(15) . 3_655 ? OW2 Na OW2 13.9(28) . 3_655 ? OW1 Na OW2 77.8(26) . 3_655 ? OW1 Na Zn1 116.1(2) 3_665 . ? O4 Na Zn1 35.9(2) . . ? O3 Na Zn1 92.4(2) 3_565 . ? O6 Na Zn1 36.91(14) . . ? OW2 Na Zn1 149.5(17) . . ? OW1 Na Zn1 88.6(2) . . ? OW2 Na Zn1 161.3(20) 3_655 . ? OW1 Na P2 101.2(2) 3_665 . ? O4 Na P2 107.0(2) . . ? O3 Na P2 26.5(2) 3_565 . ? O6 Na P2 108.0(2) . . ? OW2 Na P2 70.6(28) . . ? OW1 Na P2 147.3(2) . . ? OW2 Na P2 71.9(26) 3_655 . ? Zn1 Na P2 117.59(12) . . ? OW1 Na P1 161.8(2) 3_665 . ? O4 Na P1 23.5(2) . . ? O3 Na P1 90.1(2) 3_565 . ? O6 Na P1 95.1(2) . . ? OW2 Na P1 91.4(14) . . ? OW1 Na P1 80.1(2) . . ? OW2 Na P1 105.1(15) 3_655 . ? Zn1 Na P1 59.40(8) . . ? P2 Na P1 96.07(12) . . ? OW1 Na Na 42.3(2) 3_665 3_665 ? O4 Na Na 117.2(2) . 3_665 ? O3 Na Na 149.9(2) 3_565 3_665 ? O6 Na Na 96.9(2) . 3_665 ? OW2 Na Na 80.4(24) . 3_665 ? OW1 Na Na 39.8(2) . 3_665 ? OW2 Na Na 71.9(24) 3_655 3_665 ? Zn1 Na Na 105.5(2) . 3_665 ? P2 Na Na 134.2(2) . 3_665 ? P1 Na Na 119.8(2) . 3_665 ? P1 O1 Zn1 129.6(4) 1_565 . ? P2 O2 Zn2 131.7(4) . . ? P2 O3 Zn1 125.2(4) 3_565 . ? P2 O3 Na 108.1(3) 3_565 3_565 ? Zn1 O3 Na 122.3(3) . 3_565 ? P1 O4 Zn1 143.6(4) . . ? P1 O4 Na 118.1(4) . . ? Zn1 O4 Na 98.2(3) . . ? Zn2 O5 Zn2 127.4(3) . 2_654 ? P2 O6 Zn1 130.7(4) 1_565 . ? P2 O6 Na 134.0(3) 1_565 . ? Zn1 O6 Na 94.0(2) . . ? P1 O7 Zn2 143.1(4) 4_565 . ? P2 C P1 118.5(5) 3 . ? P2 C HA 107.7(3) 3 . ? P1 C HA 107.7(3) . . ? P2 C HB 107.7(3) 3 . ? P1 C HB 107.7(3) . . ? HA C HB 107.1 . . ? Na OW1 Na 97.9(2) 3_665 . ? OW2 OW2 Na 96.4(100) 3_655 . ? OW2 OW2 Na 69.7(100) 3_655 3_655 ? Na OW2 Na 166.1(28) . 3_655 ? _refine_diff_density_max 0.935 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.258