# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1413 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; Na3Co(O3PCH2PO3)(OH) ; _chemical_name_common 'sodium-cobalt methylene diphosphonate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H3 Co Na3 O7 P2' _chemical_formula_weight 316.87 _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 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.7890(10) _cell_length_b 7.3290(10) _cell_length_c 7.9570(10) _cell_angle_alpha 90.00 _cell_angle_beta 118.650(10) _cell_angle_gamma 90.00 _cell_volume 398.62(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'elongated plate' _exptl_crystal_colour 'colorless, transparent' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.640 _exptl_crystal_density_method ? _exptl_crystal_F_000 310 _exptl_absorpt_coefficient_mu 2.719 _exptl_absorpt_correction_type 'Xabs' _exptl_absorpt_correction_T_min 0.5425 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; Na3Co(O3PCH2PO3)(OH) ; _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% '0' _diffrn_reflns_number 760 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 24.95 _reflns_number_total 760 _reflns_number_observed 556 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-V5.0' _computing_publication_material 'SHELXTL-V5.0' _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^)+(0.0460P)^2^+0.2775P] 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 reall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 760 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_obs 0.0444 _refine_ls_wR_factor_all 0.1175 _refine_ls_wR_factor_obs 0.0978 _refine_ls_goodness_of_fit_all 1.182 _refine_ls_goodness_of_fit_obs 1.174 _refine_ls_restrained_S_all 1.182 _refine_ls_restrained_S_obs 1.174 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.0000 0.0000 0.0000 0.0109(4) Uani 1 d S . P1 P 0.6085(3) 0.2500 0.7533(3) 0.0084(5) Uani 1 d S . P2 P 0.7886(3) 0.2500 0.1960(3) 0.0091(5) Uani 1 d S . Na1 Na 0.3909(5) 0.2500 0.2745(5) 0.0162(8) Uani 1 d S . Na2 Na 0.2016(3) 0.0036(3) 0.4745(3) 0.0164(6) Uani 1 d . . O1 O 0.7102(8) 0.2500 0.3389(8) 0.0144(13) Uani 1 d S . O2 O 0.1074(9) 0.2500 0.0006(9) 0.0129(13) Uani 1 d S . O3 O 0.7202(5) 0.0755(5) 0.7630(5) 0.0130(9) Uani 1 d . . O4 O 0.9051(5) 0.0764(6) 0.2159(6) 0.0155(9) Uani 1 d . . O5 O 0.4051(8) 0.2500 0.5764(8) 0.0130(13) Uani 1 d S . C6 C 0.5719(12) 0.2500 -0.0373(12) 0.012(2) Uani 1 d S . H1 H 0.1330(135) 0.2500 -0.0827(137) 0.013(27) Uiso 1 d S . H2 H 0.4981(90) 0.1516(83) -0.0402(81) 0.012(16) Uiso 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 Co 0.0113(6) 0.0094(6) 0.0113(6) -0.0009(5) 0.0049(4) 0.0006(5) P1 0.0102(11) 0.0078(10) 0.0071(10) 0.000 0.0041(9) 0.000 P2 0.0104(11) 0.0091(10) 0.0098(10) 0.000 0.0064(9) 0.000 Na1 0.010(2) 0.022(2) 0.016(2) 0.000 0.007(2) 0.000 Na2 0.0168(13) 0.0182(12) 0.0152(13) 0.0012(11) 0.0084(11) 0.0004(12) O1 0.017(3) 0.020(3) 0.013(3) 0.000 0.012(3) 0.000 O2 0.014(3) 0.010(3) 0.020(3) 0.000 0.012(3) 0.000 O3 0.014(2) 0.013(2) 0.013(2) -0.004(2) 0.007(2) -0.002(2) O4 0.012(2) 0.016(2) 0.015(2) -0.001(2) 0.004(2) 0.004(2) O5 0.014(3) 0.012(3) 0.011(3) 0.000 0.004(3) 0.000 C6 0.010(4) 0.010(4) 0.015(4) 0.000 0.006(4) 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 Co O2 2.013(3) . ? Co O2 2.013(3) 3 ? Co O3 2.161(4) 1_454 ? Co O3 2.161(4) 3_656 ? Co O4 2.242(4) 3_655 ? Co O4 2.242(4) 1_455 ? Co Na1 3.320(3) . ? Co Na1 3.320(3) 3 ? Co Na2 3.322(2) 3 ? Co Na2 3.322(2) . ? P1 O3 1.528(4) 4_565 ? P1 O3 1.528(4) . ? P1 O5 1.534(6) . ? P1 C6 1.820(9) 1_556 ? P1 Na1 3.346(4) . ? P1 Na2 3.389(3) . ? P1 Na2 3.389(3) 4_565 ? P1 Na2 3.391(3) 3_656 ? P1 Na2 3.391(3) 2_656 ? P2 O4 1.526(4) . ? P2 O4 1.526(4) 4_565 ? P2 O1 1.527(6) . ? P2 C6 1.814(9) . ? P2 Na2 3.185(3) 2_656 ? P2 Na2 3.185(3) 3_656 ? P2 Na2 3.418(3) 4_665 ? P2 Na2 3.418(3) 1_655 ? P2 Na1 3.441(4) . ? Na1 O2 2.239(7) . ? Na1 O1 2.286(7) . ? Na1 O5 2.351(7) . ? Na1 O3 2.506(4) 3_656 ? Na1 O3 2.506(4) 2_656 ? Na1 Na2 3.196(4) . ? Na1 Na2 3.196(4) 4_565 ? Na1 Co 3.320(3) 2 ? Na1 Na2 3.383(4) 2_656 ? Na1 Na2 3.383(4) 3_656 ? Na1 H1 2.58(9) . ? Na2 O1 2.270(4) 3_656 ? Na2 O5 2.280(4) . ? Na2 O4 2.301(4) 1_455 ? Na2 O3 2.320(4) 3_656 ? Na2 O4 3.012(5) 3_656 ? Na2 P2 3.185(3) 3_656 ? Na2 Na2 3.354(4) 3_556 ? Na2 Na1 3.383(4) 3_656 ? Na2 P1 3.391(3) 3_656 ? O1 Na2 2.270(4) 2_656 ? O1 Na2 2.270(4) 3_656 ? O2 Co 2.013(3) 2 ? O2 H1 0.78(9) . ? O3 Co 2.161(4) 1_656 ? O3 Na2 2.320(4) 3_656 ? O3 Na1 2.506(4) 3_656 ? O4 Co 2.242(4) 1_655 ? O4 Na2 2.301(4) 1_655 ? O4 Na2 3.012(5) 3_656 ? O5 Na2 2.280(4) 4_565 ? C6 P1 1.820(9) 1_554 ? C6 H2 0.92(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co O2 180.0 . 3 ? O2 Co O3 90.8(2) . 1_454 ? O2 Co O3 89.2(2) 3 1_454 ? O2 Co O3 89.2(2) . 3_656 ? O2 Co O3 90.8(2) 3 3_656 ? O3 Co O3 180.0 1_454 3_656 ? O2 Co O4 86.6(2) . 3_655 ? O2 Co O4 93.4(2) 3 3_655 ? O3 Co O4 87.73(14) 1_454 3_655 ? O3 Co O4 92.27(14) 3_656 3_655 ? O2 Co O4 93.4(2) . 1_455 ? O2 Co O4 86.6(2) 3 1_455 ? O3 Co O4 92.27(14) 1_454 1_455 ? O3 Co O4 87.73(14) 3_656 1_455 ? O4 Co O4 180.0 3_655 1_455 ? O2 Co Na1 41.2(2) . . ? O2 Co Na1 138.8(2) 3 . ? O3 Co Na1 130.99(11) 1_454 . ? O3 Co Na1 49.01(11) 3_656 . ? O4 Co Na1 96.13(11) 3_655 . ? O4 Co Na1 83.87(11) 1_455 . ? O2 Co Na1 138.8(2) . 3 ? O2 Co Na1 41.2(2) 3 3 ? O3 Co Na1 49.01(11) 1_454 3 ? O3 Co Na1 130.99(11) 3_656 3 ? O4 Co Na1 83.87(11) 3_655 3 ? O4 Co Na1 96.13(11) 1_455 3 ? Na1 Co Na1 180.0 . 3 ? O2 Co Na2 88.8(2) . 3 ? O2 Co Na2 91.2(2) 3 3 ? O3 Co Na2 44.03(11) 1_454 3 ? O3 Co Na2 135.97(11) 3_656 3 ? O4 Co Na2 43.71(10) 3_655 3 ? O4 Co Na2 136.29(10) 1_455 3 ? Na1 Co Na2 122.47(7) . 3 ? Na1 Co Na2 57.53(7) 3 3 ? O2 Co Na2 91.2(2) . . ? O2 Co Na2 88.8(2) 3 . ? O3 Co Na2 135.97(11) 1_454 . ? O3 Co Na2 44.03(11) 3_656 . ? O4 Co Na2 136.29(10) 3_655 . ? O4 Co Na2 43.71(10) 1_455 . ? Na1 Co Na2 57.53(7) . . ? Na1 Co Na2 122.47(7) 3 . ? Na2 Co Na2 180.0 3 . ? O3 P1 O3 113.7(3) 4_565 . ? O3 P1 O5 111.0(2) 4_565 . ? O3 P1 O5 111.0(2) . . ? O3 P1 C6 106.8(2) 4_565 1_556 ? O3 P1 C6 106.8(2) . 1_556 ? O5 P1 C6 107.1(4) . 1_556 ? O3 P1 Na1 91.3(2) 4_565 . ? O3 P1 Na1 91.3(2) . . ? O5 P1 Na1 38.6(2) . . ? C6 P1 Na1 145.7(3) 1_556 . ? O3 P1 Na2 144.1(2) 4_565 . ? O3 P1 Na2 85.3(2) . . ? O5 P1 Na2 33.80(7) . . ? C6 P1 Na2 95.2(2) 1_556 . ? Na1 P1 Na2 56.66(6) . . ? O3 P1 Na2 85.3(2) 4_565 4_565 ? O3 P1 Na2 144.1(2) . 4_565 ? O5 P1 Na2 33.80(8) . 4_565 ? C6 P1 Na2 95.2(2) 1_556 4_565 ? Na1 P1 Na2 56.66(6) . 4_565 ? Na2 P1 Na2 64.38(9) . 4_565 ? O3 P1 Na2 95.9(2) 4_565 3_656 ? O3 P1 Na2 35.3(2) . 3_656 ? O5 P1 Na2 91.9(2) . 3_656 ? C6 P1 Na2 142.12(13) 1_556 3_656 ? Na1 P1 Na2 60.27(7) . 3_656 ? Na2 P1 Na2 82.46(6) . 3_656 ? Na2 P1 Na2 116.92(7) 4_565 3_656 ? O3 P1 Na2 35.3(2) 4_565 2_656 ? O3 P1 Na2 95.9(2) . 2_656 ? O5 P1 Na2 91.9(2) . 2_656 ? C6 P1 Na2 142.12(14) 1_556 2_656 ? Na1 P1 Na2 60.27(7) . 2_656 ? Na2 P1 Na2 116.92(7) . 2_656 ? Na2 P1 Na2 82.46(6) 4_565 2_656 ? Na2 P1 Na2 66.48(9) 3_656 2_656 ? O4 P2 O4 112.9(3) . 4_565 ? O4 P2 O1 110.7(2) . . ? O4 P2 O1 110.7(2) 4_565 . ? O4 P2 C6 108.7(2) . . ? O4 P2 C6 108.7(2) 4_565 . ? O1 P2 C6 104.7(4) . . ? O4 P2 Na2 128.5(2) . 2_656 ? O4 P2 Na2 69.5(2) 4_565 2_656 ? O1 P2 Na2 41.19(11) . 2_656 ? C6 P2 Na2 119.1(2) . 2_656 ? O4 P2 Na2 69.5(2) . 3_656 ? O4 P2 Na2 128.5(2) 4_565 3_656 ? O1 P2 Na2 41.19(11) . 3_656 ? C6 P2 Na2 119.1(2) . 3_656 ? Na2 P2 Na2 71.42(9) 2_656 3_656 ? O4 P2 Na2 92.6(2) . 4_665 ? O4 P2 Na2 33.3(2) 4_565 4_665 ? O1 P2 Na2 96.1(2) . 4_665 ? C6 P2 Na2 142.0(2) . 4_665 ? Na2 P2 Na2 60.94(7) 2_656 4_665 ? Na2 P2 Na2 97.53(7) 3_656 4_665 ? O4 P2 Na2 33.3(2) . 1_655 ? O4 P2 Na2 92.6(2) 4_565 1_655 ? O1 P2 Na2 96.1(2) . 1_655 ? C6 P2 Na2 142.0(2) . 1_655 ? Na2 P2 Na2 97.53(7) 2_656 1_655 ? Na2 P2 Na2 60.94(7) 3_656 1_655 ? Na2 P2 Na2 63.78(8) 4_665 1_655 ? O4 P2 Na1 121.6(2) . . ? O4 P2 Na1 121.6(2) 4_565 . ? O1 P2 Na1 31.6(2) . . ? C6 P2 Na1 73.1(3) . . ? Na2 P2 Na1 61.25(7) 2_656 . ? Na2 P2 Na1 61.25(7) 3_656 . ? Na2 P2 Na1 122.12(7) 4_665 . ? Na2 P2 Na1 122.12(7) 1_655 . ? O2 Na1 O1 132.7(3) . . ? O2 Na1 O5 122.4(3) . . ? O1 Na1 O5 104.9(2) . . ? O2 Na1 O3 76.16(12) . 3_656 ? O1 Na1 O3 107.65(11) . 3_656 ? O5 Na1 O3 88.06(12) . 3_656 ? O2 Na1 O3 76.16(12) . 2_656 ? O1 Na1 O3 107.65(11) . 2_656 ? O5 Na1 O3 88.06(12) . 2_656 ? O3 Na1 O3 144.3(2) 3_656 2_656 ? O2 Na1 Na2 90.5(2) . . ? O1 Na1 Na2 126.90(14) . . ? O5 Na1 Na2 45.44(10) . . ? O3 Na1 Na2 46.07(10) 3_656 . ? O3 Na1 Na2 112.43(14) 2_656 . ? O2 Na1 Na2 90.5(2) . 4_565 ? O1 Na1 Na2 126.90(14) . 4_565 ? O5 Na1 Na2 45.44(10) . 4_565 ? O3 Na1 Na2 112.43(14) 3_656 4_565 ? O3 Na1 Na2 46.07(10) 2_656 4_565 ? Na2 Na1 Na2 68.79(11) . 4_565 ? O2 Na1 Co 36.29(7) . 2 ? O1 Na1 Co 134.71(12) . 2 ? O5 Na1 Co 104.56(15) . 2 ? O3 Na1 Co 106.95(13) 3_656 2 ? O3 Na1 Co 40.61(10) 2_656 2 ? Na2 Na1 Co 98.21(9) . 2 ? Na2 Na1 Co 61.27(6) 4_565 2 ? O2 Na1 Co 36.29(7) . . ? O1 Na1 Co 134.71(12) . . ? O5 Na1 Co 104.56(15) . . ? O3 Na1 Co 40.61(10) 3_656 . ? O3 Na1 Co 106.95(13) 2_656 . ? Na2 Na1 Co 61.27(6) . . ? Na2 Na1 Co 98.21(9) 4_565 . ? Co Na1 Co 67.00(6) 2 . ? O2 Na1 P1 146.4(2) . . ? O1 Na1 P1 80.9(2) . . ? O5 Na1 P1 24.02(15) . . ? O3 Na1 P1 95.34(12) 3_656 . ? O3 Na1 P1 95.34(12) 2_656 . ? Na2 Na1 P1 62.35(7) . . ? Na2 Na1 P1 62.35(7) 4_565 . ? Co Na1 P1 123.59(8) 2 . ? Co Na1 P1 123.59(8) . . ? O2 Na1 Na2 141.56(11) . 2_656 ? O1 Na1 Na2 41.89(10) . 2_656 ? O5 Na1 Na2 79.95(15) . 2_656 ? O3 Na1 Na2 140.01(14) 3_656 2_656 ? O3 Na1 Na2 73.74(10) 2_656 2_656 ? Na2 Na1 Na2 122.88(11) . 2_656 ? Na2 Na1 Na2 85.52(7) 4_565 2_656 ? Co Na1 Na2 112.97(4) 2 2_656 ? Co Na1 Na2 175.42(12) . 2_656 ? P1 Na1 Na2 60.53(7) . 2_656 ? O2 Na1 Na2 141.56(11) . 3_656 ? O1 Na1 Na2 41.89(10) . 3_656 ? O5 Na1 Na2 79.95(15) . 3_656 ? O3 Na1 Na2 73.74(10) 3_656 3_656 ? O3 Na1 Na2 140.01(14) 2_656 3_656 ? Na2 Na1 Na2 85.52(7) . 3_656 ? Na2 Na1 Na2 122.87(11) 4_565 3_656 ? Co Na1 Na2 175.42(12) 2 3_656 ? Co Na1 Na2 112.97(4) . 3_656 ? P1 Na1 Na2 60.53(7) . 3_656 ? Na2 Na1 Na2 66.67(10) 2_656 3_656 ? O2 Na1 H1 16.8(21) . . ? O1 Na1 H1 115.9(21) . . ? O5 Na1 H1 139.2(21) . . ? O3 Na1 H1 80.0(6) 3_656 . ? O3 Na1 H1 80.0(6) 2_656 . ? Na2 Na1 H1 104.3(17) . . ? Na2 Na1 H1 104.3(17) 4_565 . ? Co Na1 H1 44.8(13) 2 . ? Co Na1 H1 44.8(13) . . ? P1 Na1 H1 163.2(21) . . ? Na2 Na1 H1 131.8(14) 2_656 . ? Na2 Na1 H1 131.8(14) 3_656 . ? O1 Na2 O5 118.3(2) 3_656 . ? O1 Na2 O4 129.4(2) 3_656 1_455 ? O5 Na2 O4 111.3(2) . 1_455 ? O1 Na2 O3 102.3(2) 3_656 3_656 ? O5 Na2 O3 94.5(2) . 3_656 ? O4 Na2 O3 82.7(2) 1_455 3_656 ? O1 Na2 O4 54.6(2) 3_656 3_656 ? O5 Na2 O4 106.3(2) . 3_656 ? O4 Na2 O4 102.98(14) 1_455 3_656 ? O3 Na2 O4 154.3(2) 3_656 3_656 ? O1 Na2 P2 26.28(13) 3_656 3_656 ? O5 Na2 P2 115.5(2) . 3_656 ? O4 Na2 P2 119.29(14) 1_455 3_656 ? O3 Na2 P2 127.78(14) 3_656 3_656 ? O4 Na2 P2 28.35(8) 3_656 3_656 ? O1 Na2 Na1 136.1(2) 3_656 . ? O5 Na2 Na1 47.3(2) . . ? O4 Na2 Na1 85.90(14) 1_455 . ? O3 Na2 Na1 51.07(11) 3_656 . ? O4 Na2 Na1 153.06(12) 3_656 . ? P2 Na2 Na1 154.80(10) 3_656 . ? O1 Na2 Co 124.52(15) 3_656 . ? O5 Na2 Co 106.2(2) . . ? O4 Na2 Co 42.32(11) 1_455 . ? O3 Na2 Co 40.34(10) 3_656 . ? O4 Na2 Co 139.71(10) 3_656 . ? P2 Na2 Co 137.96(8) 3_656 . ? Na1 Na2 Co 61.20(7) . . ? O1 Na2 Na2 85.1(2) 3_656 3_556 ? O5 Na2 Na2 120.1(2) . 3_556 ? O4 Na2 Na2 61.03(12) 1_455 3_556 ? O3 Na2 Na2 136.17(15) 3_656 3_556 ? O4 Na2 Na2 41.95(9) 3_656 3_556 ? P2 Na2 Na2 62.96(8) 3_656 3_556 ? Na1 Na2 Na2 138.71(12) . 3_556 ? Co Na2 Na2 100.24(8) . 3_556 ? O1 Na2 Na1 42.2(2) 3_656 3_656 ? O5 Na2 Na1 85.95(13) . 3_656 ? O4 Na2 Na1 155.61(15) 1_455 3_656 ? O3 Na2 Na1 78.76(12) 3_656 3_656 ? O4 Na2 Na1 87.64(11) 3_656 3_656 ? P2 Na2 Na1 63.11(8) 3_656 3_656 ? Na1 Na2 Na1 94.48(7) . 3_656 ? Co Na2 Na1 117.71(8) . 3_656 ? Na2 Na2 Na1 126.00(11) 3_556 3_656 ? O1 Na2 P1 96.49(15) 3_656 . ? O5 Na2 P1 21.97(12) . . ? O4 Na2 P1 133.20(14) 1_455 . ? O3 Na2 P1 97.93(12) 3_656 . ? O4 Na2 P1 96.11(10) 3_656 . ? P2 Na2 P1 97.25(7) 3_656 . ? Na1 Na2 P1 61.00(8) . . ? Co Na2 P1 122.17(7) . . ? Na2 Na2 P1 124.41(11) 3_556 . ? Na1 Na2 P1 65.66(5) 3_656 . ? O1 Na2 P1 80.09(14) 3_656 3_656 ? O5 Na2 P1 102.5(2) . 3_656 ? O4 Na2 P1 99.03(13) 1_455 3_656 ? O3 Na2 P1 22.40(11) 3_656 3_656 ? O4 Na2 P1 133.85(11) 3_656 3_656 ? P2 Na2 P1 106.00(7) 3_656 3_656 ? Na1 Na2 P1 67.66(6) . 3_656 ? Co Na2 P1 58.51(5) . 3_656 ? Na2 Na2 P1 136.85(11) 3_556 3_656 ? Na1 Na2 P1 59.21(7) 3_656 3_656 ? P1 Na2 P1 97.54(6) . 3_656 ? P2 O1 Na2 112.5(2) . 2_656 ? P2 O1 Na2 112.5(2) . 3_656 ? Na2 O1 Na2 109.9(3) 2_656 3_656 ? P2 O1 Na1 127.9(3) . . ? Na2 O1 Na1 95.9(2) 2_656 . ? Na2 O1 Na1 95.9(2) 3_656 . ? Co O2 Co 131.1(3) . 2 ? Co O2 Na1 102.5(2) . . ? Co O2 Na1 102.5(2) 2 . ? Co O2 H1 105.9(23) . . ? Co O2 H1 105.9(22) 2 . ? Na1 O2 H1 107.1(70) . . ? P1 O3 Co 124.7(2) . 1_656 ? P1 O3 Na2 122.3(2) . 3_656 ? Co O3 Na2 95.6(2) 1_656 3_656 ? P1 O3 Na1 129.4(2) . 3_656 ? Co O3 Na1 90.4(2) 1_656 3_656 ? Na2 O3 Na1 82.9(2) 3_656 3_656 ? P2 O4 Co 121.8(2) . 1_655 ? P2 O4 Na2 125.3(2) . 1_655 ? Co O4 Na2 94.0(2) 1_655 1_655 ? P2 O4 Na2 82.1(2) . 3_656 ? Co O4 Na2 154.1(2) 1_655 3_656 ? Na2 O4 Na2 77.02(14) 1_655 3_656 ? P1 O5 Na2 124.2(2) . 4_565 ? P1 O5 Na2 124.23(15) . . ? Na2 O5 Na2 104.7(2) 4_565 . ? P1 O5 Na1 117.4(3) . . ? Na2 O5 Na1 87.3(2) 4_565 . ? Na2 O5 Na1 87.3(2) . . ? P2 C6 P1 117.3(5) . 1_554 ? P2 C6 H2 106.9(37) . . ? P1 C6 H2 110.4(37) 1_554 . ? _refine_diff_density_max 1.335 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.152 #===END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; Na3Mg(O3PCH2PO3)(F)*2H2O ; _chemical_name_common 'sodium-magnesium methylene diphosphonate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H4 F Mg Na3 O7 P2' _chemical_formula_weight 302.26 _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 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 '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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.996(2) _cell_length_b 7.1516(7) _cell_length_c 8.100(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.730(10) _cell_angle_gamma 90.00 _cell_volume 406.17(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 12 _exptl_crystal_description bar _exptl_crystal_colour 'colorless, transparent' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.471 _exptl_crystal_density_method ? _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type 'Xabs' _exptl_absorpt_correction_T_min 0.8633 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; Na3Mg(O3PCH2PO3)(F)*2H2O ; _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% '0' _diffrn_reflns_number 778 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 24.92 _reflns_number_total 778 _reflns_number_observed 566 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-V5.0' _computing_publication_material 'SHELXTL-V5.0' _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^)+(0.0429P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 778 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.0998 _refine_ls_wR_factor_obs 0.0886 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.014 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.0000 0.0000 0.0000 0.0102(4) Uani 1 d S . P1 P 0.6254(2) 0.2500 0.7453(2) 0.0095(4) Uani 1 d S . P2 P 0.7780(2) 0.2500 0.1729(2) 0.0091(4) Uani 1 d S . Na1 Na 0.3887(3) 0.2500 0.2584(3) 0.0166(6) Uani 1 d S . Na2 Na 0.2046(2) 0.0115(3) 0.4809(2) 0.0196(5) Uani 1 d . . O1 O 0.6968(6) 0.2500 0.3086(5) 0.0146(10) Uani 1 d S . F F 0.1022(4) 0.2500 0.0163(4) 0.0139(8) Uani 1 d S . O3 O 0.7405(4) 0.0723(4) 0.7668(3) 0.0117(7) Uani 1 d . . O4 O 0.8956(4) 0.0750(4) 0.1909(4) 0.0125(7) Uani 1 d . . O5 O 0.4385(6) 0.2500 0.5619(5) 0.0154(10) Uani 1 d S . C C 0.5708(8) 0.2500 -0.0614(8) 0.0104(13) Uani 1 d S . O6 O 0.1012(7) 0.2500 0.6464(7) 0.0242(11) Uani 1 d S . H1 H 0.4987(55) 0.1311(58) -0.0756(53) 0.014(11) Uiso 1 d . . H2 H 0.1158(72) 0.1586(77) 0.7249(65) 0.045(17) Uiso 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 Mg 0.0117(9) 0.0063(10) 0.0115(9) 0.0008(8) 0.0046(8) 0.0005(8) P1 0.0086(7) 0.0100(8) 0.0093(8) 0.000 0.0039(6) 0.000 P2 0.0103(7) 0.0084(8) 0.0096(8) 0.000 0.0056(6) 0.000 Na1 0.0128(12) 0.0199(14) 0.0160(13) 0.000 0.0060(11) 0.000 Na2 0.0214(9) 0.0218(10) 0.0173(9) 0.0011(8) 0.0107(7) 0.0025(8) O1 0.016(2) 0.019(2) 0.012(2) 0.000 0.009(2) 0.000 F 0.013(2) 0.009(2) 0.018(2) 0.000 0.0068(15) 0.000 O3 0.0118(14) 0.010(2) 0.0103(14) 0.0009(12) 0.0034(12) 0.0020(13) O4 0.0127(14) 0.012(2) 0.0147(15) 0.0018(12) 0.0083(12) 0.0018(13) O5 0.011(2) 0.017(2) 0.015(2) 0.000 0.004(2) 0.000 C 0.011(3) 0.010(3) 0.010(3) 0.000 0.005(3) 0.000 O6 0.033(3) 0.021(3) 0.019(3) 0.000 0.012(2) 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 Mg F 1.9436(13) 3 ? Mg F 1.9436(13) . ? Mg O3 2.091(3) 3_656 ? Mg O3 2.091(3) 1_454 ? Mg O4 2.149(3) 1_455 ? Mg O4 2.149(3) 3_655 ? Mg Na1 3.314(2) 3 ? Mg Na1 3.314(2) . ? Mg Na2 3.425(2) 3 ? Mg Na2 3.425(2) . ? Mg Mg 3.5758(4) 2_545 ? Mg Mg 3.5758(4) 2 ? P1 O5 1.519(4) . ? P1 O3 1.529(3) . ? P1 O3 1.529(3) 4_565 ? P1 C 1.816(6) 1_556 ? P1 Na2 3.332(2) 3_656 ? P1 Na2 3.332(2) 2_656 ? P1 F 3.363(4) 1_656 ? P1 O4 3.430(3) 4_566 ? P1 O4 3.430(3) 1_556 ? P1 Na2 3.448(2) . ? P1 Na2 3.448(2) 4_565 ? P1 Na1 3.458(3) . ? P2 O1 1.522(4) . ? P2 O4 1.530(3) . ? P2 O4 1.530(3) 4_565 ? P2 C 1.823(6) . ? P2 Na2 3.317(2) 2_656 ? P2 Na2 3.317(2) 3_656 ? P2 F 3.389(4) 1_655 ? Na1 F 2.185(4) . ? Na1 O5 2.293(5) . ? Na1 O1 2.296(5) . ? Na1 O3 2.494(3) 3_656 ? Na1 O3 2.494(3) 2_656 ? Na1 Na2 3.298(3) . ? Na1 Na2 3.298(3) 4_565 ? Na1 Mg 3.314(2) 2 ? Na1 Na2 3.454(3) 2_656 ? Na1 Na2 3.454(3) 3_656 ? Na2 O3 2.329(3) 3_656 ? Na2 O5 2.379(3) . ? Na2 O1 2.394(3) 3_656 ? Na2 O4 2.500(3) 1_455 ? Na2 O6 2.540(4) . ? Na2 O6 2.849(4) 3_556 ? Na2 O4 3.184(3) 3_656 ? Na2 P2 3.317(2) 3_656 ? Na2 P1 3.332(2) 3_656 ? Na2 Na2 3.411(4) 4_565 ? Na2 H2 2.62(5) . ? O1 Na2 2.394(3) 2_656 ? O1 Na2 2.394(3) 3_656 ? O1 O4 2.542(4) . ? O1 O4 2.542(4) 4_565 ? F Mg 1.9436(13) 2 ? F H2 2.50(5) 1_554 ? F O3 2.803(3) 2_656 ? F O3 2.803(3) 3_656 ? F O4 2.872(3) 3_655 ? F O4 2.872(3) 2_655 ? F O3 2.906(4) 1_454 ? F O3 2.906(4) 4_464 ? O3 Mg 2.091(3) 1_656 ? O3 Na2 2.329(3) 3_656 ? O3 Na1 2.494(3) 3_656 ? O3 F 2.803(3) 3_656 ? O3 F 2.906(4) 1_656 ? O3 O4 2.955(4) 3_756 ? O3 O4 3.040(4) 1_556 ? O4 H2 1.82(5) 3_656 ? O4 Mg 2.149(3) 1_655 ? O4 Na2 2.500(3) 1_655 ? O4 O4 2.504(6) 4_565 ? O4 O6 2.666(4) 3_656 ? O5 Na2 2.379(3) 4_565 ? C P1 1.816(6) 1_554 ? C O4 2.718(6) 4_565 ? C H1 1.00(4) . ? O6 Na2 2.540(4) 4_565 ? O6 O4 2.666(4) 2_656 ? O6 O4 2.666(4) 3_656 ? O6 Na2 2.849(4) 3_556 ? O6 Na2 2.849(4) 2_556 ? O6 F 2.993(6) 1_556 ? O6 O4 3.472(5) 1_455 ? O6 O4 3.472(5) 4_465 ? O6 H2 0.88(5) . ? 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 F Mg F 180.0 3 . ? F Mg O3 92.06(12) 3 3_656 ? F Mg O3 87.94(12) . 3_656 ? F Mg O3 87.94(12) 3 1_454 ? F Mg O3 92.06(12) . 1_454 ? O3 Mg O3 180.0 3_656 1_454 ? F Mg O4 88.99(12) 3 1_455 ? F Mg O4 91.01(12) . 1_455 ? O3 Mg O4 88.38(10) 3_656 1_455 ? O3 Mg O4 91.62(10) 1_454 1_455 ? F Mg O4 91.01(12) 3 3_655 ? F Mg O4 88.99(12) . 3_655 ? O3 Mg O4 91.62(10) 3_656 3_655 ? O3 Mg O4 88.38(10) 1_454 3_655 ? O4 Mg O4 180.0 1_455 3_655 ? F Mg Na1 39.19(9) 3 3 ? F Mg Na1 140.81(9) . 3 ? O3 Mg Na1 131.23(8) 3_656 3 ? O3 Mg Na1 48.77(8) 1_454 3 ? O4 Mg Na1 91.05(8) 1_455 3 ? O4 Mg Na1 88.95(8) 3_655 3 ? F Mg Na1 140.81(9) 3 . ? F Mg Na1 39.19(9) . . ? O3 Mg Na1 48.77(8) 3_656 . ? O3 Mg Na1 131.23(8) 1_454 . ? O4 Mg Na1 88.95(8) 1_455 . ? O4 Mg Na1 91.05(8) 3_655 . ? Na1 Mg Na1 180.0 3 . ? F Mg Na2 86.86(10) 3 3 ? F Mg Na2 93.14(10) . 3 ? O3 Mg Na2 138.20(7) 3_656 3 ? O3 Mg Na2 41.80(7) 1_454 3 ? O4 Mg Na2 133.32(8) 1_455 3 ? O4 Mg Na2 46.68(8) 3_655 3 ? Na1 Mg Na2 58.57(5) 3 3 ? Na1 Mg Na2 121.44(5) . 3 ? F Mg Na2 93.14(10) 3 . ? F Mg Na2 86.86(10) . . ? O3 Mg Na2 41.80(7) 3_656 . ? O3 Mg Na2 138.20(8) 1_454 . ? O4 Mg Na2 46.68(8) 1_455 . ? O4 Mg Na2 133.32(8) 3_655 . ? Na1 Mg Na2 121.43(5) 3 . ? Na1 Mg Na2 58.56(5) . . ? Na2 Mg Na2 180.0 3 . ? F Mg Mg 23.09(9) 3 2_545 ? F Mg Mg 156.91(9) . 2_545 ? O3 Mg Mg 75.68(7) 3_656 2_545 ? O3 Mg Mg 104.32(7) 1_454 2_545 ? O4 Mg Mg 104.45(8) 1_455 2_545 ? O4 Mg Mg 75.55(8) 3_655 2_545 ? Na1 Mg Mg 57.35(2) 3 2_545 ? Na1 Mg Mg 122.65(2) . 2_545 ? Na2 Mg Mg 88.62(3) 3 2_545 ? Na2 Mg Mg 91.38(3) . 2_545 ? F Mg Mg 156.91(9) 3 2 ? F Mg Mg 23.09(9) . 2 ? O3 Mg Mg 104.32(7) 3_656 2 ? O3 Mg Mg 75.68(7) 1_454 2 ? O4 Mg Mg 75.55(8) 1_455 2 ? O4 Mg Mg 104.45(8) 3_655 2 ? Na1 Mg Mg 122.65(2) 3 2 ? Na1 Mg Mg 57.35(2) . 2 ? Na2 Mg Mg 91.37(3) 3 2 ? Na2 Mg Mg 88.62(3) . 2 ? Mg Mg Mg 180.0 2_545 2 ? O5 P1 O3 111.52(13) . . ? O5 P1 O3 111.52(13) . 4_565 ? O3 P1 O3 112.4(2) . 4_565 ? O5 P1 C 108.2(2) . 1_556 ? O3 P1 C 106.44(15) . 1_556 ? O3 P1 C 106.44(15) 4_565 1_556 ? O5 P1 Na2 86.08(14) . 3_656 ? O3 P1 Na2 38.15(11) . 3_656 ? O3 P1 Na2 98.41(12) 4_565 3_656 ? C P1 Na2 143.60(7) 1_556 3_656 ? O5 P1 Na2 86.08(14) . 2_656 ? O3 P1 Na2 98.41(12) . 2_656 ? O3 P1 Na2 38.14(11) 4_565 2_656 ? C P1 Na2 143.60(7) 1_556 2_656 ? Na2 P1 Na2 68.29(7) 3_656 2_656 ? O5 P1 F 155.8(2) . 1_656 ? O3 P1 F 59.60(11) . 1_656 ? O3 P1 F 59.60(11) 4_565 1_656 ? C P1 F 96.0(2) 1_556 1_656 ? Na2 P1 F 74.01(6) 3_656 1_656 ? Na2 P1 F 74.01(6) 2_656 1_656 ? O5 P1 O4 148.81(13) . 4_566 ? O3 P1 O4 98.23(12) . 4_566 ? O3 P1 O4 62.40(12) 4_565 4_566 ? C P1 O4 52.0(2) 1_556 4_566 ? Na2 P1 O4 124.50(7) 3_656 4_566 ? Na2 P1 O4 99.01(6) 2_656 4_566 ? F P1 O4 50.95(7) 1_656 4_566 ? O5 P1 O4 148.81(13) . 1_556 ? O3 P1 O4 62.40(12) . 1_556 ? O3 P1 O4 98.23(12) 4_565 1_556 ? C P1 O4 52.0(2) 1_556 1_556 ? Na2 P1 O4 99.01(6) 3_656 1_556 ? Na2 P1 O4 124.50(7) 2_656 1_556 ? F P1 O4 50.95(7) 1_656 1_556 ? O4 P1 O4 42.81(10) 4_566 1_556 ? O5 P1 Na2 35.39(9) . . ? O3 P1 Na2 90.81(11) . . ? O3 P1 Na2 146.73(12) 4_565 . ? C P1 Na2 88.2(2) 1_556 . ? Na2 P1 Na2 85.13(5) 3_656 . ? Na2 P1 Na2 118.07(5) 2_656 . ? F P1 Na2 150.12(3) 1_656 . ? O4 P1 Na2 140.10(7) 4_566 . ? O4 P1 Na2 113.96(6) 1_556 . ? O5 P1 Na2 35.39(9) . 4_565 ? O3 P1 Na2 146.74(12) . 4_565 ? O3 P1 Na2 90.81(11) 4_565 4_565 ? C P1 Na2 88.2(2) 1_556 4_565 ? Na2 P1 Na2 118.07(5) 3_656 4_565 ? Na2 P1 Na2 85.13(5) 2_656 4_565 ? F P1 Na2 150.12(3) 1_656 4_565 ? O4 P1 Na2 113.96(6) 4_566 4_565 ? O4 P1 Na2 140.10(7) 1_556 4_565 ? Na2 P1 Na2 59.30(6) . 4_565 ? O5 P1 Na1 31.0(2) . . ? O3 P1 Na1 95.70(11) . . ? O3 P1 Na1 95.70(11) 4_565 . ? C P1 Na1 139.2(2) 1_556 . ? Na2 P1 Na1 61.13(5) 3_656 . ? Na2 P1 Na1 61.13(5) 2_656 . ? F P1 Na1 124.87(8) 1_656 . ? O4 P1 Na1 157.31(5) 4_566 . ? O4 P1 Na1 157.31(5) 1_556 . ? Na2 P1 Na1 57.04(5) . . ? Na2 P1 Na1 57.04(5) 4_565 . ? O1 P2 O4 112.79(13) . . ? O1 P2 O4 112.79(13) . 4_565 ? O4 P2 O4 109.8(2) . 4_565 ? O1 P2 C 105.2(2) . . ? O4 P2 C 107.96(15) . . ? O4 P2 C 107.96(15) 4_565 . ? O1 P2 Na2 41.29(8) . 2_656 ? O4 P2 Na2 127.35(12) . 2_656 ? O4 P2 Na2 71.58(11) 4_565 2_656 ? C P2 Na2 121.9(2) . 2_656 ? O1 P2 Na2 41.29(8) . 3_656 ? O4 P2 Na2 71.58(11) . 3_656 ? O4 P2 Na2 127.35(12) 4_565 3_656 ? C P2 Na2 121.9(2) . 3_656 ? Na2 P2 Na2 68.64(7) 2_656 3_656 ? O1 P2 F 159.9(2) . 1_655 ? O4 P2 F 59.34(11) . 1_655 ? O4 P2 F 59.34(11) 4_565 1_655 ? C P2 F 94.9(2) . 1_655 ? Na2 P2 F 125.97(6) 2_656 1_655 ? Na2 P2 F 125.97(6) 3_656 1_655 ? F Na1 O5 121.9(2) . . ? F Na1 O1 137.0(2) . . ? O5 Na1 O1 101.0(2) . . ? F Na1 O3 73.27(8) . 3_656 ? O5 Na1 O3 86.53(9) . 3_656 ? O1 Na1 O3 112.42(8) . 3_656 ? F Na1 O3 73.27(8) . 2_656 ? O5 Na1 O3 86.53(9) . 2_656 ? O1 Na1 O3 112.42(8) . 2_656 ? O3 Na1 O3 135.1(2) 3_656 2_656 ? F Na1 Na2 86.55(10) . . ? O5 Na1 Na2 46.17(8) . . ? O1 Na1 Na2 128.76(10) . . ? O3 Na1 Na2 44.81(7) 3_656 . ? O3 Na1 Na2 104.29(10) 2_656 . ? F Na1 Na2 86.55(10) . 4_565 ? O5 Na1 Na2 46.17(8) . 4_565 ? O1 Na1 Na2 128.76(10) . 4_565 ? O3 Na1 Na2 104.29(10) 3_656 4_565 ? O3 Na1 Na2 44.81(7) 2_656 4_565 ? Na2 Na1 Na2 62.30(7) . 4_565 ? F Na1 Mg 34.19(3) . . ? O5 Na1 Mg 107.70(11) . . ? O1 Na1 Mg 135.43(9) . . ? O3 Na1 Mg 39.09(6) 3_656 . ? O3 Na1 Mg 102.78(9) 2_656 . ? Na2 Na1 Mg 62.40(5) . . ? Na2 Na1 Mg 95.44(7) 4_565 . ? F Na1 Mg 34.19(3) . 2 ? O5 Na1 Mg 107.70(11) . 2 ? O1 Na1 Mg 135.43(9) . 2 ? O3 Na1 Mg 102.78(9) 3_656 2 ? O3 Na1 Mg 39.09(6) 2_656 2 ? Na2 Na1 Mg 95.44(7) . 2 ? Na2 Na1 Mg 62.40(5) 4_565 2 ? Mg Na1 Mg 65.30(5) . 2 ? F Na1 Na2 145.23(5) . 2_656 ? O5 Na1 Na2 73.59(10) . 2_656 ? O1 Na1 Na2 43.68(7) . 2_656 ? O3 Na1 Na2 141.42(10) 3_656 2_656 ? O3 Na1 Na2 77.35(7) 2_656 2_656 ? Na2 Na1 Na2 118.85(7) . 2_656 ? Na2 Na1 Na2 85.55(6) 4_565 2_656 ? Mg Na1 Na2 178.70(8) . 2_656 ? Mg Na1 Na2 114.56(3) 2 2_656 ? F Na1 Na2 145.23(5) . 3_656 ? O5 Na1 Na2 73.59(10) . 3_656 ? O1 Na1 Na2 43.68(7) . 3_656 ? O3 Na1 Na2 77.35(7) 3_656 3_656 ? O3 Na1 Na2 141.42(10) 2_656 3_656 ? Na2 Na1 Na2 85.55(6) . 3_656 ? Na2 Na1 Na2 118.85(7) 4_565 3_656 ? Mg Na1 Na2 114.56(3) . 3_656 ? Mg Na1 Na2 178.70(8) 2 3_656 ? Na2 Na1 Na2 65.55(7) 2_656 3_656 ? F Na1 P1 141.86(12) . . ? O5 Na1 P1 19.92(11) . . ? O1 Na1 P1 81.12(12) . . ? O3 Na1 P1 94.10(8) 3_656 . ? O3 Na1 P1 94.10(8) 2_656 . ? Na2 Na1 P1 61.32(5) . . ? Na2 Na1 P1 61.32(5) 4_565 . ? Mg Na1 P1 123.60(6) . . ? Mg Na1 P1 123.60(6) 2 . ? Na2 Na1 P1 57.63(5) 2_656 . ? Na2 Na1 P1 57.63(5) 3_656 . ? O3 Na2 O5 88.47(12) 3_656 . ? O3 Na2 O1 106.16(12) 3_656 3_656 ? O5 Na2 O1 114.68(13) . 3_656 ? O3 Na2 O4 75.38(10) 3_656 1_455 ? O5 Na2 O4 114.82(12) . 1_455 ? O1 Na2 O4 130.50(13) 3_656 1_455 ? O3 Na2 O6 150.59(13) 3_656 . ? O5 Na2 O6 77.60(14) . . ? O1 Na2 O6 103.19(12) 3_656 . ? O4 Na2 O6 87.06(13) 1_455 . ? O3 Na2 O6 90.20(13) 3_656 3_556 ? O5 Na2 O6 174.17(13) . 3_556 ? O1 Na2 O6 71.14(12) 3_656 3_556 ? O4 Na2 O6 59.36(11) 1_455 3_556 ? O6 Na2 O6 101.04(9) . 3_556 ? O3 Na2 O4 153.70(12) 3_656 3_656 ? O5 Na2 O4 112.90(12) . 3_656 ? O1 Na2 O4 51.89(10) 3_656 3_656 ? O4 Na2 O4 106.76(9) 1_455 3_656 ? O6 Na2 O4 54.11(9) . 3_656 ? O6 Na2 O4 70.01(11) 3_556 3_656 ? O3 Na2 Na1 48.99(8) 3_656 . ? O5 Na2 Na1 44.06(10) . . ? O1 Na2 Na1 135.42(12) 3_656 . ? O4 Na2 Na1 83.78(9) 1_455 . ? O6 Na2 Na1 106.55(10) . . ? O6 Na2 Na1 132.27(12) 3_556 . ? O4 Na2 Na1 156.10(8) 3_656 . ? O3 Na2 P2 129.37(10) 3_656 3_656 ? O5 Na2 P2 117.60(11) . 3_656 ? O1 Na2 P2 24.80(9) 3_656 3_656 ? O4 Na2 P2 121.18(9) 1_455 3_656 ? O6 Na2 P2 79.90(9) . 3_656 ? O6 Na2 P2 67.41(10) 3_556 3_656 ? O4 Na2 P2 27.12(6) 3_656 3_656 ? Na1 Na2 P2 154.85(7) . 3_656 ? O3 Na2 P1 23.93(7) 3_656 3_656 ? O5 Na2 P1 94.55(10) . 3_656 ? O1 Na2 P1 82.61(10) 3_656 3_656 ? O4 Na2 P1 93.75(8) 1_455 3_656 ? O6 Na2 P1 171.64(11) . 3_656 ? O6 Na2 P1 86.48(10) 3_556 3_656 ? O4 Na2 P1 133.09(8) 3_656 3_656 ? Na1 Na2 P1 65.31(4) . 3_656 ? P2 Na2 P1 106.62(6) 3_656 3_656 ? O3 Na2 Na2 104.91(8) 3_656 4_565 ? O5 Na2 Na2 44.19(8) . 4_565 ? O1 Na2 Na2 141.36(8) 3_656 4_565 ? O4 Na2 Na2 79.54(8) 1_455 4_565 ? O6 Na2 Na2 47.82(8) . 4_565 ? O6 Na2 Na2 131.03(8) 3_556 4_565 ? O4 Na2 Na2 101.20(6) 3_656 4_565 ? Na1 Na2 Na2 58.85(4) . 4_565 ? P2 Na2 Na2 124.32(3) 3_656 4_565 ? P1 Na2 Na2 124.15(3) 3_656 4_565 ? O3 Na2 Mg 36.75(7) 3_656 . ? O5 Na2 Mg 102.30(10) . . ? O1 Na2 Mg 127.21(9) 3_656 . ? O4 Na2 Mg 38.70(6) 1_455 . ? O6 Na2 Mg 121.17(11) . . ? O6 Na2 Mg 73.44(10) 3_556 . ? O4 Na2 Mg 140.41(7) 3_656 . ? Na1 Na2 Mg 59.03(5) . . ? P2 Na2 Mg 138.67(6) 3_656 . ? P1 Na2 Mg 57.25(4) 3_656 . ? Na2 Na2 Mg 91.38(3) 4_565 . ? O3 Na2 H2 170.0(11) 3_656 . ? O5 Na2 H2 88.1(12) . . ? O1 Na2 H2 83.8(12) 3_656 . ? O4 Na2 H2 97.6(11) 1_455 . ? O6 Na2 H2 19.6(11) . . ? O6 Na2 H2 92.3(12) 3_556 . ? O4 Na2 H2 34.9(12) 3_656 . ? Na1 Na2 H2 124.0(12) . . ? P2 Na2 H2 60.4(12) 3_656 . ? P1 Na2 H2 166.0(11) 3_656 . ? Na2 Na2 H2 66.3(12) 4_565 . ? Mg Na2 H2 135.5(11) . . ? P2 O1 Na1 131.8(2) . . ? P2 O1 Na2 113.91(14) . 2_656 ? Na1 O1 Na2 94.84(12) . 2_656 ? P2 O1 Na2 113.91(14) . 3_656 ? Na1 O1 Na2 94.84(12) . 3_656 ? Na2 O1 Na2 102.7(2) 2_656 3_656 ? P2 O1 O4 33.70(9) . . ? Na1 O1 O4 138.15(14) . . ? Na2 O1 O4 126.9(2) 2_656 . ? Na2 O1 O4 80.27(10) 3_656 . ? P2 O1 O4 33.70(9) . 4_565 ? Na1 O1 O4 138.15(14) . 4_565 ? Na2 O1 O4 80.27(10) 2_656 4_565 ? Na2 O1 O4 126.9(2) 3_656 4_565 ? O4 O1 O4 59.0(2) . 4_565 ? Mg F Mg 133.8(2) 2 . ? Mg F Na1 106.62(9) 2 . ? Mg F Na1 106.62(9) . . ? Mg F H2 112.6(12) 2 1_554 ? Mg F H2 84.4(12) . 1_554 ? Na1 F H2 110.2(12) . 1_554 ? Mg F O3 48.20(6) 2 2_656 ? Mg F O3 147.8(2) . 2_656 ? Na1 F O3 58.43(8) . 2_656 ? H2 F O3 126.6(12) 1_554 2_656 ? Mg F O3 147.8(2) 2 3_656 ? Mg F O3 48.20(6) . 3_656 ? Na1 F O3 58.43(8) . 3_656 ? H2 F O3 99.6(12) 1_554 3_656 ? O3 F O3 110.6(2) 2_656 3_656 ? Mg F O4 145.6(2) 2 3_655 ? Mg F O4 48.42(7) . 3_655 ? Na1 F O4 103.07(10) . 3_655 ? H2 F O4 38.9(12) 1_554 3_655 ? O3 F O4 154.79(15) 2_656 3_655 ? O3 F O4 64.77(8) 3_656 3_655 ? Mg F O4 48.42(7) 2 2_655 ? Mg F O4 145.6(2) . 2_655 ? Na1 F O4 103.07(10) . 2_655 ? H2 F O4 69.2(13) 1_554 2_655 ? O3 F O4 64.77(8) 2_656 2_655 ? O3 F O4 154.79(15) 3_656 2_655 ? O4 F O4 108.05(15) 3_655 2_655 ? Mg F O3 96.30(13) 2 1_454 ? Mg F O3 45.99(8) . 1_454 ? Na1 F O3 152.59(8) . 1_454 ? H2 F O3 73.1(12) 1_554 1_454 ? O3 F O3 142.40(12) 2_656 1_454 ? O3 F O3 94.19(8) 3_656 1_454 ? O4 F O3 61.53(9) 3_655 1_454 ? O4 F O3 103.36(12) 2_655 1_454 ? Mg F O3 45.99(8) 2 4_464 ? Mg F O3 96.30(13) . 4_464 ? Na1 F O3 152.59(8) . 4_464 ? H2 F O3 86.4(12) 1_554 4_464 ? O3 F O3 94.19(8) 2_656 4_464 ? O3 F O3 142.40(12) 3_656 4_464 ? O4 F O3 103.36(12) 3_655 4_464 ? O4 F O3 61.53(9) 2_655 4_464 ? O3 F O3 51.87(12) 1_454 4_464 ? P1 O3 Mg 126.2(2) . 1_656 ? P1 O3 Na2 117.9(2) . 3_656 ? Mg O3 Na2 101.45(11) 1_656 3_656 ? P1 O3 Na1 123.75(15) . 3_656 ? Mg O3 Na1 92.14(11) 1_656 3_656 ? Na2 O3 Na1 86.20(11) 3_656 3_656 ? P1 O3 F 145.0(2) . 3_656 ? Mg O3 F 43.86(8) 1_656 3_656 ? Na2 O3 F 96.58(12) 3_656 3_656 ? Na1 O3 F 48.29(9) 3_656 3_656 ? P1 O3 F 93.40(13) . 1_656 ? Mg O3 F 41.95(6) 1_656 1_656 ? Na2 O3 F 100.09(12) 3_656 1_656 ? Na1 O3 F 134.09(12) 3_656 1_656 ? F O3 F 85.81(8) 3_656 1_656 ? P1 O3 O4 144.6(2) . 3_756 ? Mg O3 O4 46.61(7) 1_656 3_756 ? Na2 O3 O4 54.93(8) 3_656 3_756 ? Na1 O3 O4 91.49(11) 3_656 3_756 ? F O3 O4 60.93(10) 3_656 3_756 ? F O3 O4 58.67(9) 1_656 3_756 ? P1 O3 O4 91.12(13) . 1_556 ? Mg O3 O4 44.95(7) 1_656 1_556 ? Na2 O3 O4 146.26(12) 3_656 1_556 ? Na1 O3 O4 91.50(11) 3_656 1_556 ? F O3 O4 58.71(9) 3_656 1_556 ? F O3 O4 58.83(9) 1_656 1_556 ? O4 O3 O4 91.56(10) 3_756 1_556 ? P2 O4 H2 130.3(16) . 3_656 ? P2 O4 Mg 124.7(2) . 1_655 ? H2 O4 Mg 98.5(15) 3_656 1_655 ? P2 O4 Na2 121.5(2) . 1_655 ? H2 O4 Na2 71.7(16) 3_656 1_655 ? Mg O4 Na2 94.62(11) 1_655 1_655 ? P2 O4 O4 35.09(11) . 4_565 ? H2 O4 O4 156.4(15) 3_656 4_565 ? Mg O4 O4 104.45(8) 1_655 4_565 ? Na2 O4 O4 100.46(8) 1_655 4_565 ? P2 O4 O1 33.51(9) . . ? H2 O4 O1 99.1(15) 3_656 . ? Mg O4 O1 157.27(15) 1_655 . ? Na2 O4 O1 104.52(13) 1_655 . ? O4 O4 O1 60.50(8) 4_565 . ? P2 O4 O6 128.3(2) . 3_656 ? H2 O4 O6 6.6(15) 3_656 3_656 ? Mg O4 O6 102.92(14) 1_655 3_656 ? Na2 O4 O6 66.84(13) 1_655 3_656 ? O4 O4 O6 150.67(11) 4_565 3_656 ? O1 O4 O6 95.91(13) . 3_656 ? P1 O5 Na1 129.1(2) . . ? P1 O5 Na2 122.90(14) . . ? Na1 O5 Na2 89.78(13) . . ? P1 O5 Na2 122.90(14) . 4_565 ? Na1 O5 Na2 89.78(13) . 4_565 ? Na2 O5 Na2 91.6(2) . 4_565 ? P1 C P2 115.0(3) 1_554 . ? P1 C O4 96.3(2) 1_554 4_565 ? P2 C O4 32.38(10) . 4_565 ? P1 C O4 96.3(2) 1_554 . ? P2 C O4 32.38(10) . . ? O4 C O4 54.9(2) 4_565 . ? P1 C H1 105.3(23) 1_554 . ? P2 C H1 107.7(23) . . ? O4 C H1 140.0(23) 4_565 . ? O4 C H1 89.1(23) . . ? Na2 O6 Na2 84.4(2) 4_565 . ? Na2 O6 O4 75.36(7) 4_565 2_656 ? Na2 O6 O4 156.6(2) . 2_656 ? Na2 O6 O4 156.6(2) 4_565 3_656 ? Na2 O6 O4 75.36(7) . 3_656 ? O4 O6 O4 121.3(2) 2_656 3_656 ? Na2 O6 Na2 133.6(2) 4_565 3_556 ? Na2 O6 Na2 78.96(9) . 3_556 ? O4 O6 Na2 123.6(2) 2_656 3_556 ? O4 O6 Na2 53.79(8) 3_656 3_556 ? Na2 O6 Na2 78.96(9) 4_565 2_556 ? Na2 O6 Na2 133.6(2) . 2_556 ? O4 O6 Na2 53.79(8) 2_656 2_556 ? O4 O6 Na2 123.6(2) 3_656 2_556 ? Na2 O6 Na2 82.1(2) 3_556 2_556 ? Na2 O6 F 133.10(11) 4_565 1_556 ? Na2 O6 F 133.11(11) . 1_556 ? O4 O6 F 60.67(11) 2_656 1_556 ? O4 O6 F 60.67(11) 3_656 1_556 ? Na2 O6 F 87.20(13) 3_556 1_556 ? Na2 O6 F 87.20(13) 2_556 1_556 ? Na2 O6 O4 77.84(13) 4_565 1_455 ? Na2 O6 O4 45.98(9) . 1_455 ? O4 O6 O4 136.63(15) 2_656 1_455 ? O4 O6 O4 95.63(9) 3_656 1_455 ? Na2 O6 O4 59.53(9) 3_556 1_455 ? Na2 O6 O4 88.07(14) 2_556 1_455 ? F O6 O4 146.73(15) 1_556 1_455 ? Na2 O6 O4 45.98(9) 4_565 4_465 ? Na2 O6 O4 77.84(13) . 4_465 ? O4 O6 O4 95.63(9) 2_656 4_465 ? O4 O6 O4 136.6(2) 3_656 4_465 ? Na2 O6 O4 88.07(14) 3_556 4_465 ? Na2 O6 O4 59.53(9) 2_556 4_465 ? F O6 O4 146.73(15) 1_556 4_465 ? O4 O6 O4 42.27(11) 1_455 4_465 ? Na2 O6 H2 156.4(35) 4_565 . ? Na2 O6 H2 85.3(33) . . ? O4 O6 H2 108.9(33) 2_656 . ? O4 O6 H2 13.7(33) 3_656 . ? Na2 O6 H2 64.3(34) 3_556 . ? Na2 O6 H2 122.8(34) 2_556 . ? F O6 H2 48.8(33) 1_556 . ? O4 O6 H2 109.3(34) 1_455 . ? O4 O6 H2 150.1(34) 4_465 . ? _refine_diff_density_max 0.394 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.102 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; Na2Co(O3PCH2PO3)*(H2O) ; _chemical_name_common 'sodium-cobalt methylene diphosphonate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H4 Co Na2 O7 P2' _chemical_formula_weight 294.89 _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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 8.997(1) _cell_length_b 10.348(2) _cell_length_c 16.260(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1513.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'deep-purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.588 _exptl_crystal_density_method ? _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 2.803 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Na2Co(O3PCH2PO3)*(H2O) ; _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% '0' _diffrn_reflns_number 841 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 19.95 _reflns_number_total 841 _reflns_number_observed 793 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-V5.0' _computing_publication_material 'SHELXTL-V5.0' _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^)+(0.0432P)^2^+0.3961P] 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 0.0006(3) _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 0.03(3) _refine_ls_number_reflns 841 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_obs 0.0228 _refine_ls_wR_factor_all 0.0627 _refine_ls_wR_factor_obs 0.0593 _refine_ls_goodness_of_fit_all 1.077 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -2.714 _refine_ls_shift/esd_mean 0.013 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 Co1 Co 0.77532(13) 0.88886(11) 0.91723(7) 0.0136(4) Uani 1 d . . Co2 Co 0.79093(14) 1.37746(11) 0.94511(7) 0.0125(4) Uani 1 d . . P1 P 1.0718(3) 0.8791(3) 1.03543(15) 0.0125(7) Uani 1 d . . P2 P 0.7930(3) 1.6145(2) 0.82527(13) 0.0126(6) Uani 1 d . . P3 P 0.8034(3) 1.1529(2) 0.80823(14) 0.0120(6) Uani 1 d . . P4 P 0.5629(3) 1.1398(2) 0.93736(14) 0.0109(7) Uani 1 d . . Na1 Na 1.0035(4) 0.8857(4) 0.7504(2) 0.0323(10) Uani 1 d . . Na2 Na 0.3921(4) 0.8719(4) 0.9676(2) 0.0210(9) Uani 1 d . . Na3 Na 0.6077(4) 1.3653(4) 1.1086(2) 0.0246(9) Uani 1 d . . Na4 Na 0.8358(4) 1.0811(4) 0.5947(2) 0.0274(11) Uani 1 d . . O1 O 0.6206(9) 1.0088(6) 0.9655(4) 0.022(2) Uani 1 d . . O2 O 0.8640(7) 1.0230(6) 0.8375(4) 0.020(2) Uani 1 d . . O3 O 0.8128(7) 1.5624(6) 0.7398(3) 0.017(2) Uani 1 d . . O4 O 0.8775(7) 1.2629(6) 0.8567(4) 0.015(2) Uani 1 d . . O5 O 0.8244(7) 1.7598(5) 0.8299(4) 0.019(2) Uani 1 d . . O6 O 0.8222(7) 1.1765(6) 0.7175(4) 0.020(2) Uani 1 d . . O7 O 0.8853(7) 1.5396(6) 0.8887(3) 0.015(2) Uani 1 d . . O8 O 0.6369(9) 1.2487(7) 0.9826(4) 0.026(2) Uani 1 d . . O9 O 0.9049(6) 0.8784(6) 1.0191(3) 0.018(2) Uani 1 d . . O10 O 0.6389(9) 0.7512(6) 0.9846(4) 0.020(2) Uani 1 d . . O11 O 0.8936(7) 1.3567(6) 1.0545(4) 0.020(2) Uani 1 d . . O12 O 0.6553(8) 1.5147(6) 1.0087(4) 0.020(2) Uani 1 d . . O13 O 0.7378(12) 1.1351(11) 1.1505(8) 0.048(3) Uani 1 d . . H1 H 0.7884(135) 1.1551(129) 1.1333(72) 0.017(48) Uiso 1 d . . H2 H 0.8229(266) 1.1363(211) 1.1860(100) 0.176(93) Uiso 1 d . . O14 O 0.3752(9) 0.8737(9) 0.8269(4) 0.029(2) Uani 1 d . . H3 H 0.2991(113) 0.9297(83) 0.8106(51) 0.016(27) Uiso 1 d . . H4 H 0.3316(100) 0.8237(83) 0.8064(53) 0.000(32) Uiso 1 d . . C1 C 0.6064(11) 1.1547(12) 0.8296(6) 0.015(3) Uani 1 d . . H5 H 0.5684(88) 1.0791(82) 0.8035(48) 0.000(23) Uiso 1 d . . H6 H 0.5728(97) 1.2170(89) 0.8072(52) 0.009(31) Uiso 1 d . . C2 C 0.5995(11) 1.5981(12) 0.8555(6) 0.013(3) Uani 1 d . . H7 H 0.5534(141) 1.6704(121) 0.8146(71) 0.072(43) Uiso 1 d . . H8 H 0.5770(98) 1.5365(89) 0.8452(51) 0.000(31) Uiso 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 Co1 0.0175(7) 0.0107(7) 0.0126(7) -0.0002(6) 0.0022(6) 0.0009(7) Co2 0.0160(7) 0.0092(7) 0.0124(7) -0.0005(6) 0.0013(5) -0.0022(7) P1 0.0153(15) 0.0108(14) 0.0114(13) 0.0013(12) -0.0012(11) -0.0020(14) P2 0.0172(14) 0.0101(14) 0.0103(13) -0.0001(12) 0.0031(11) -0.0017(14) P3 0.0167(14) 0.0089(15) 0.0104(13) 0.0016(12) 0.0029(12) 0.0005(13) P4 0.0113(14) 0.0096(15) 0.0118(14) -0.0014(12) 0.0020(10) 0.0004(12) Na1 0.035(2) 0.025(2) 0.038(2) -0.011(2) 0.018(2) -0.005(2) Na2 0.019(2) 0.022(2) 0.021(2) -0.007(2) 0.004(2) -0.001(2) Na3 0.038(2) 0.018(2) 0.017(2) 0.001(2) 0.005(2) 0.000(2) Na4 0.035(2) 0.035(3) 0.012(2) -0.007(2) 0.001(2) 0.011(2) O1 0.030(4) 0.023(4) 0.013(4) 0.010(3) 0.005(4) 0.009(3) O2 0.020(4) 0.010(3) 0.030(4) 0.002(3) 0.008(3) 0.000(3) O3 0.025(4) 0.018(4) 0.009(3) -0.002(3) 0.001(3) 0.001(3) O4 0.014(3) 0.015(4) 0.017(3) -0.004(3) 0.003(3) -0.001(3) O5 0.026(4) 0.012(4) 0.017(4) -0.001(3) 0.007(3) -0.001(3) O6 0.023(4) 0.025(4) 0.013(3) 0.001(3) 0.005(3) 0.002(3) O7 0.019(4) 0.012(3) 0.014(4) 0.001(3) 0.002(3) 0.003(3) O8 0.029(4) 0.031(4) 0.017(4) -0.006(4) 0.012(4) -0.017(4) O9 0.012(4) 0.024(4) 0.017(3) -0.001(3) 0.000(3) -0.001(3) O10 0.028(4) 0.015(3) 0.016(4) -0.004(3) 0.007(3) -0.004(3) O11 0.015(4) 0.026(4) 0.021(4) 0.004(3) -0.001(3) -0.004(3) O12 0.021(5) 0.022(4) 0.016(4) 0.005(3) 0.003(3) 0.008(3) O13 0.052(7) 0.040(6) 0.052(6) 0.008(5) 0.020(6) -0.008(6) O14 0.041(5) 0.019(5) 0.025(4) -0.006(4) -0.012(4) 0.002(5) C1 0.024(6) 0.012(7) 0.008(6) 0.007(6) 0.004(5) -0.006(6) C2 0.020(6) 0.000(6) 0.020(6) -0.009(5) -0.006(5) -0.015(6) _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 Co1 O5 1.999(6) 1_545 ? Co1 O1 2.023(7) . ? Co1 O9 2.028(6) . ? Co1 O2 2.060(6) . ? Co1 O10 2.176(7) . ? Co1 Na4 3.070(4) 2_675 ? Co1 Na1 3.401(4) . ? Co1 Na2 3.449(4) 4_567 ? Co1 Na2 3.548(4) . ? Co2 O11 2.015(6) . ? Co2 O8 2.017(7) . ? Co2 O4 2.019(6) . ? Co2 O7 2.092(6) . ? Co2 O12 2.139(7) . ? Co2 Na2 3.093(4) 4_577 ? Co2 Na3 3.130(4) . ? P1 O12 1.512(7) 4_577 ? P1 O10 1.512(7) 4_567 ? P1 O9 1.525(7) . ? P1 C2 1.806(10) 4_577 ? P1 Na2 3.060(4) 4_567 ? P1 Na2 3.087(4) 1_655 ? P2 O3 1.501(6) . ? P2 O5 1.532(6) . ? P2 O7 1.534(6) . ? P2 C2 1.817(11) . ? P2 Na1 3.236(5) 3_756 ? P3 O6 1.504(6) . ? P3 O2 1.527(7) . ? P3 O4 1.537(7) . ? P3 C1 1.806(10) . ? P3 Na3 3.059(4) 4_577 ? P3 Na1 3.120(5) 3_756 ? P3 Na1 3.430(5) . ? P4 O8 1.502(8) . ? P4 O1 1.521(7) . ? P4 O11 1.530(7) 4_477 ? P4 C1 1.802(9) . ? P4 Na2 3.206(4) . ? Na1 O2 2.366(7) . ? Na1 O4 2.408(7) 3_746 ? Na1 O5 2.442(7) 1_545 ? Na1 O3 2.470(7) 3_746 ? Na1 O13 2.720(12) 2_674 ? Na1 O6 2.724(8) 3_746 ? Na1 O7 2.942(7) 3_746 ? Na1 P3 3.120(5) 3_746 ? Na1 P2 3.236(5) 3_746 ? Na1 Na3 3.574(5) 4_577 ? Na2 O14 2.294(7) . ? Na2 O12 2.462(8) 4_477 ? Na2 O1 2.497(9) . ? Na2 O7 2.510(7) 4_477 ? Na2 O10 2.563(8) . ? Na2 O9 2.602(8) 4_467 ? Na2 O10 2.724(9) 4_467 ? Na2 O11 2.831(8) 4_477 ? Na2 P1 3.060(4) 4_467 ? Na2 P1 3.087(4) 1_455 ? Na2 Co2 3.093(4) 4_477 ? Na3 O12 2.283(7) . ? Na3 O3 2.371(6) 2_685 ? Na3 O8 2.392(7) . ? Na3 O4 2.523(7) 4_477 ? Na3 O2 2.629(8) 4_477 ? Na3 O11 2.720(7) . ? Na3 O13 2.741(12) . ? Na3 P3 3.059(4) 4_477 ? Na3 Na1 3.574(5) 4_477 ? Na3 Na1 3.615(5) 2_675 ? Na3 Na2 3.934(5) 4_577 ? Na4 O6 2.231(7) . ? Na4 O1 2.332(7) 2_674 ? Na4 O13 2.503(12) 2_674 ? Na4 O10 2.504(7) 2_674 ? Na4 O9 2.525(7) 2_674 ? Na4 O7 2.560(7) 3_746 ? Na4 Co1 3.070(4) 2_674 ? Na4 Na2 3.240(5) 2_674 ? Na4 Na2 3.780(5) 3_656 ? O1 Na4 2.332(7) 2_675 ? O2 Na3 2.628(8) 4_577 ? O3 Na3 2.371(6) 2_684 ? O3 Na1 2.470(7) 3_756 ? O4 Na1 2.408(7) 3_756 ? O4 Na3 2.523(7) 4_577 ? O5 Co1 1.999(6) 1_565 ? O5 Na1 2.442(7) 1_565 ? O6 Na1 2.724(8) 3_756 ? O7 Na2 2.510(7) 4_577 ? O7 Na4 2.560(7) 3_756 ? O7 Na1 2.942(7) 3_756 ? O9 Na4 2.525(7) 2_675 ? O9 Na2 2.602(8) 4_567 ? O10 P1 1.512(7) 4_467 ? O10 Na4 2.504(7) 2_675 ? O10 Na2 2.724(8) 4_567 ? O11 P4 1.529(6) 4_577 ? O11 Na2 2.831(8) 4_577 ? O12 P1 1.512(7) 4_477 ? O12 Na2 2.462(8) 4_577 ? O13 Na4 2.503(12) 2_675 ? O13 Na1 2.720(12) 2_675 ? O13 H1 0.57(11) . ? O13 H2 0.96(21) . ? O14 H3 0.94(10) . ? O14 H4 0.73(9) . ? C1 H5 0.95(9) . ? C1 H6 0.80(9) . ? C2 P1 1.806(10) 4_477 ? C2 H7 1.08(13) . ? C2 H8 0.69(9) . ? 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 Co1 O1 146.9(3) 1_545 . ? O5 Co1 O9 114.7(3) 1_545 . ? O1 Co1 O9 96.4(3) . . ? O5 Co1 O2 85.3(2) 1_545 . ? O1 Co1 O2 95.6(3) . . ? O9 Co1 O2 109.1(3) . . ? O5 Co1 O10 92.5(2) 1_545 . ? O1 Co1 O10 79.6(2) . . ? O9 Co1 O10 83.0(3) . . ? O2 Co1 O10 167.5(3) . . ? O5 Co1 Na4 143.8(2) 1_545 2_675 ? O1 Co1 Na4 49.4(2) . 2_675 ? O9 Co1 Na4 54.9(2) . 2_675 ? O2 Co1 Na4 130.5(2) . 2_675 ? O10 Co1 Na4 53.8(2) . 2_675 ? O5 Co1 Na1 45.1(2) 1_545 . ? O1 Co1 Na1 136.9(2) . . ? O9 Co1 Na1 107.7(2) . . ? O2 Co1 Na1 43.2(2) . . ? O10 Co1 Na1 137.3(2) . . ? Na4 Co1 Na1 161.27(11) 2_675 . ? O5 Co1 Na2 78.2(2) 1_545 4_567 ? O1 Co1 Na2 118.6(2) . 4_567 ? O9 Co1 Na2 48.7(2) . 4_567 ? O2 Co1 Na2 138.7(2) . 4_567 ? O10 Co1 Na2 52.1(2) . 4_567 ? Na4 Co1 Na2 70.61(9) 2_675 4_567 ? Na1 Co1 Na2 103.97(10) . 4_567 ? O5 Co1 Na2 110.2(2) 1_545 . ? O1 Co1 Na2 43.3(2) . . ? O9 Co1 Na2 111.5(2) . . ? O2 Co1 Na2 123.7(2) . . ? O10 Co1 Na2 45.8(2) . . ? Na4 Co1 Na2 58.10(9) 2_675 . ? Na1 Co1 Na2 140.36(9) . . ? Na2 Co1 Na2 97.59(7) 4_567 . ? O11 Co2 O8 88.7(3) . . ? O11 Co2 O4 112.9(3) . . ? O8 Co2 O4 95.3(3) . . ? O11 Co2 O7 106.6(3) . . ? O8 Co2 O7 160.2(3) . . ? O4 Co2 O7 90.1(2) . . ? O11 Co2 O12 84.6(3) . . ? O8 Co2 O12 84.3(3) . . ? O4 Co2 O12 162.5(2) . . ? O7 Co2 O12 84.9(2) . . ? O11 Co2 Na2 63.2(2) . 4_577 ? O8 Co2 Na2 128.1(2) . 4_577 ? O4 Co2 Na2 134.8(2) . 4_577 ? O7 Co2 Na2 53.8(2) . 4_577 ? O12 Co2 Na2 52.4(2) . 4_577 ? O11 Co2 Na3 59.2(2) . . ? O8 Co2 Na3 49.8(2) . . ? O4 Co2 Na3 141.6(2) . . ? O7 Co2 Na3 128.2(2) . . ? O12 Co2 Na3 46.8(2) . . ? Na2 Co2 Na3 78.41(9) 4_577 . ? O12 P1 O10 110.3(4) 4_577 4_567 ? O12 P1 O9 114.2(4) 4_577 . ? O10 P1 O9 110.6(4) 4_567 . ? O12 P1 C2 107.6(5) 4_577 4_577 ? O10 P1 C2 105.8(5) 4_567 4_577 ? O9 P1 C2 107.9(4) . 4_577 ? O12 P1 Na2 150.7(3) 4_577 4_567 ? O10 P1 Na2 56.7(3) 4_567 4_567 ? O9 P1 Na2 58.2(3) . 4_567 ? C2 P1 Na2 101.5(4) 4_577 4_567 ? O12 P1 Na2 52.0(3) 4_577 1_655 ? O10 P1 Na2 61.9(3) 4_567 1_655 ? O9 P1 Na2 149.0(3) . 1_655 ? C2 P1 Na2 103.0(3) 4_577 1_655 ? Na2 P1 Na2 117.85(10) 4_567 1_655 ? O3 P2 O5 112.1(3) . . ? O3 P2 O7 112.2(4) . . ? O5 P2 O7 111.2(4) . . ? O3 P2 C2 109.3(4) . . ? O5 P2 C2 104.8(5) . . ? O7 P2 C2 106.8(4) . . ? O3 P2 Na1 47.0(3) . 3_756 ? O5 P2 Na1 129.2(3) . 3_756 ? O7 P2 Na1 65.2(2) . 3_756 ? C2 P2 Na1 125.3(4) . 3_756 ? O6 P3 O2 114.1(4) . . ? O6 P3 O4 109.5(4) . . ? O2 P3 O4 109.7(4) . . ? O6 P3 C1 107.3(5) . . ? O2 P3 C1 107.4(5) . . ? O4 P3 C1 108.6(5) . . ? O6 P3 Na3 110.1(3) . 4_577 ? O2 P3 Na3 59.2(3) . 4_577 ? O4 P3 Na3 55.3(3) . 4_577 ? C1 P3 Na3 142.5(3) . 4_577 ? O6 P3 Na1 60.8(3) . 3_756 ? O2 P3 Na1 125.2(3) . 3_756 ? O4 P3 Na1 48.9(2) . 3_756 ? C1 P3 Na1 126.7(4) . 3_756 ? Na3 P3 Na1 71.60(11) 4_577 3_756 ? O6 P3 Na1 78.7(3) . . ? O2 P3 Na1 35.8(3) . . ? O4 P3 Na1 120.7(3) . . ? C1 P3 Na1 125.2(4) . . ? Na3 P3 Na1 66.54(11) 4_577 . ? Na1 P3 Na1 104.27(7) 3_756 . ? O8 P4 O1 111.7(4) . . ? O8 P4 O11 112.4(4) . 4_477 ? O1 P4 O11 109.6(4) . 4_477 ? O8 P4 C1 108.4(5) . . ? O1 P4 C1 107.1(5) . . ? O11 P4 C1 107.4(4) 4_477 . ? O8 P4 Na2 141.8(3) . . ? O1 P4 Na2 49.3(3) . . ? O11 P4 Na2 62.0(3) 4_477 . ? C1 P4 Na2 109.1(4) . . ? O2 Na1 O4 170.4(3) . 3_746 ? O2 Na1 O5 69.7(2) . 1_545 ? O4 Na1 O5 113.3(3) 3_746 1_545 ? O2 Na1 O3 82.6(2) . 3_746 ? O4 Na1 O3 98.0(2) 3_746 3_746 ? O5 Na1 O3 143.3(3) 1_545 3_746 ? O2 Na1 O13 89.0(3) . 2_674 ? O4 Na1 O13 83.2(3) 3_746 2_674 ? O5 Na1 O13 75.4(3) 1_545 2_674 ? O3 Na1 O13 129.1(3) 3_746 2_674 ? O2 Na1 O6 131.9(3) . 3_746 ? O4 Na1 O6 57.5(2) 3_746 3_746 ? O5 Na1 O6 81.6(2) 1_545 3_746 ? O3 Na1 O6 101.0(2) 3_746 3_746 ? O13 Na1 O6 120.7(3) 2_674 3_746 ? O2 Na1 O7 108.4(2) . 3_746 ? O4 Na1 O7 65.0(2) 3_746 3_746 ? O5 Na1 O7 157.0(3) 1_545 3_746 ? O3 Na1 O7 54.6(2) 3_746 3_746 ? O13 Na1 O7 81.7(3) 2_674 3_746 ? O6 Na1 O7 112.4(2) 3_746 3_746 ? O2 Na1 P3 160.4(2) . 3_746 ? O4 Na1 P3 28.8(2) 3_746 3_746 ? O5 Na1 P3 96.7(2) 1_545 3_746 ? O3 Na1 P3 102.6(2) 3_746 3_746 ? O13 Na1 P3 101.6(3) 2_674 3_746 ? O6 Na1 P3 28.83(14) 3_746 3_746 ? O7 Na1 P3 89.6(2) 3_746 3_746 ? O2 Na1 P2 95.1(2) . 3_746 ? O4 Na1 P2 81.9(2) 3_746 3_746 ? O5 Na1 P2 164.8(2) 1_545 3_746 ? O3 Na1 P2 26.41(14) 3_746 3_746 ? O13 Na1 P2 106.4(3) 2_674 3_746 ? O6 Na1 P2 109.2(2) 3_746 3_746 ? O7 Na1 P2 28.24(13) 3_746 3_746 ? P3 Na1 P2 97.66(12) 3_746 3_746 ? O2 Na1 Co1 36.6(2) . . ? O4 Na1 Co1 148.3(2) 3_746 . ? O5 Na1 Co1 35.42(14) 1_545 . ? O3 Na1 Co1 110.2(2) 3_746 . ? O13 Na1 Co1 89.7(3) 2_674 . ? O6 Na1 Co1 101.7(2) 3_746 . ? O7 Na1 Co1 144.4(2) 3_746 . ? P3 Na1 Co1 125.96(14) 3_746 . ? P2 Na1 Co1 129.63(13) 3_746 . ? O2 Na1 P3 22.2(2) . . ? O4 Na1 P3 149.0(2) 3_746 . ? O5 Na1 P3 86.5(2) 1_545 . ? O3 Na1 P3 74.7(2) 3_746 . ? O13 Na1 P3 79.0(3) 2_674 . ? O6 Na1 P3 152.9(2) 3_746 . ? O7 Na1 P3 87.3(2) 3_746 . ? P3 Na1 P3 176.8(2) 3_746 . ? P2 Na1 P3 79.14(11) 3_746 . ? Co1 Na1 P3 57.13(7) . . ? O2 Na1 Na3 47.3(2) . 4_577 ? O4 Na1 Na3 136.7(2) 3_746 4_577 ? O5 Na1 Na3 102.6(2) 1_545 4_577 ? O3 Na1 Na3 41.36(15) 3_746 4_577 ? O13 Na1 Na3 130.5(3) 2_674 4_577 ? O6 Na1 Na3 107.4(2) 3_746 4_577 ? O7 Na1 Na3 90.8(2) 3_746 4_577 ? P3 Na1 Na3 127.35(14) 3_746 4_577 ? P2 Na1 Na3 64.42(10) 3_746 4_577 ? Co1 Na1 Na3 68.89(9) . 4_577 ? P3 Na1 Na3 51.75(9) . 4_577 ? O14 Na2 O12 95.4(3) . 4_477 ? O14 Na2 O1 92.1(3) . . ? O12 Na2 O1 116.4(2) 4_477 . ? O14 Na2 O7 157.5(3) . 4_477 ? O12 Na2 O7 70.1(2) 4_477 4_477 ? O1 Na2 O7 80.0(2) . 4_477 ? O14 Na2 O10 99.7(3) . . ? O12 Na2 O10 164.8(3) 4_477 . ? O1 Na2 O10 64.2(2) . . ? O7 Na2 O10 95.7(2) 4_477 . ? O14 Na2 O9 95.4(3) . 4_467 ? O12 Na2 O9 120.0(2) 4_477 4_467 ? O1 Na2 O9 122.0(3) . 4_467 ? O7 Na2 O9 106.7(2) 4_477 4_467 ? O10 Na2 O9 57.8(2) . 4_467 ? O14 Na2 O10 103.5(3) . 4_467 ? O12 Na2 O10 56.9(2) 4_477 4_467 ? O1 Na2 O10 163.4(2) . 4_467 ? O7 Na2 O10 83.4(2) 4_477 4_467 ? O10 Na2 O10 117.77(14) . 4_467 ? O9 Na2 O10 63.1(2) 4_467 4_467 ? O14 Na2 O11 82.3(3) . 4_477 ? O12 Na2 O11 63.3(2) 4_477 4_477 ? O1 Na2 O11 55.4(2) . 4_477 ? O7 Na2 O11 75.9(2) 4_477 4_477 ? O10 Na2 O11 119.6(2) . 4_477 ? O9 Na2 O11 176.2(2) 4_467 4_477 ? O10 Na2 O11 120.3(2) 4_467 4_477 ? O14 Na2 P1 91.5(2) . 4_467 ? O12 Na2 P1 149.8(2) 4_477 4_467 ? O1 Na2 P1 92.7(2) . 4_467 ? O7 Na2 P1 109.7(2) 4_477 4_467 ? O10 Na2 P1 29.6(2) . 4_467 ? O9 Na2 P1 29.87(15) 4_467 4_467 ? O10 Na2 P1 92.8(2) 4_467 4_467 ? O11 Na2 P1 146.9(2) 4_477 4_467 ? O14 Na2 P1 107.1(2) . 1_455 ? O12 Na2 P1 28.9(2) 4_477 1_455 ? O1 Na2 P1 139.5(2) . 1_455 ? O7 Na2 P1 68.6(2) 4_477 1_455 ? O10 Na2 P1 141.5(2) . 1_455 ? O9 Na2 P1 92.0(2) 4_467 1_455 ? O10 Na2 P1 29.3(2) 4_467 1_455 ? O11 Na2 P1 91.5(2) 4_477 1_455 ? P1 Na2 P1 121.29(13) 4_467 1_455 ? O14 Na2 Co2 115.6(3) . 4_477 ? O12 Na2 Co2 43.5(2) 4_477 4_477 ? O1 Na2 Co2 76.9(2) . 4_477 ? O7 Na2 Co2 42.28(14) 4_477 4_477 ? O10 Na2 Co2 127.9(2) . 4_477 ? O9 Na2 Co2 144.1(2) 4_467 4_477 ? O10 Na2 Co2 90.9(2) 4_467 4_477 ? O11 Na2 Co2 39.46(13) 4_477 4_477 ? P1 Na2 Co2 151.01(13) 4_467 4_477 ? P1 Na2 Co2 62.69(8) 1_455 4_477 ? O14 Na2 P4 82.6(3) . . ? O12 Na2 P4 91.5(2) 4_477 . ? O1 Na2 P4 27.5(2) . . ? O7 Na2 P4 80.8(2) 4_477 . ? O10 Na2 P4 91.3(2) . . ? O9 Na2 P4 148.4(2) 4_467 . ? O10 Na2 P4 148.1(2) 4_467 . ? O11 Na2 P4 28.49(13) 4_477 . ? P1 Na2 P4 118.57(12) 4_467 . ? P1 Na2 P4 118.78(13) 1_455 . ? Co2 Na2 P4 59.12(8) 4_477 . ? O12 Na3 O3 111.7(3) . 2_685 ? O12 Na3 O8 73.2(2) . . ? O3 Na3 O8 153.7(3) 2_685 . ? O12 Na3 O4 132.0(3) . 4_477 ? O3 Na3 O4 102.3(2) 2_685 4_477 ? O8 Na3 O4 90.9(3) . 4_477 ? O12 Na3 O2 95.5(2) . 4_477 ? O3 Na3 O2 79.2(2) 2_685 4_477 ? O8 Na3 O2 126.8(3) . 4_477 ? O4 Na3 O2 58.2(2) 4_477 4_477 ? O12 Na3 O11 67.3(2) . . ? O3 Na3 O11 90.9(2) 2_685 . ? O8 Na3 O11 66.6(2) . . ? O4 Na3 O11 146.2(3) 4_477 . ? O2 Na3 O11 155.6(3) 4_477 . ? O12 Na3 O13 133.3(3) . . ? O3 Na3 O13 85.5(3) 2_685 . ? O8 Na3 O13 74.2(3) . . ? O4 Na3 O13 80.7(3) 4_477 . ? O2 Na3 O13 131.0(3) 4_477 . ? O11 Na3 O13 69.4(3) . . ? O12 Na3 P3 121.6(2) . 4_477 ? O3 Na3 P3 83.8(2) 2_685 4_477 ? O8 Na3 P3 116.5(2) . 4_477 ? O4 Na3 P3 30.1(2) 4_477 4_477 ? O2 Na3 P3 29.9(2) 4_477 4_477 ? O11 Na3 P3 170.8(2) . 4_477 ? O13 Na3 P3 102.6(3) . 4_477 ? O12 Na3 Co2 43.1(2) . . ? O3 Na3 Co2 126.3(2) 2_685 . ? O8 Na3 Co2 40.1(2) . . ? O4 Na3 Co2 130.0(2) 4_477 . ? O2 Na3 Co2 134.8(2) 4_477 . ? O11 Na3 Co2 39.52(13) . . ? O13 Na3 Co2 91.2(3) . . ? P3 Na3 Co2 148.13(13) 4_477 . ? O12 Na3 Na1 91.0(2) . 4_477 ? O3 Na3 Na1 43.5(2) 2_685 4_477 ? O8 Na3 Na1 160.4(2) . 4_477 ? O4 Na3 Na1 91.2(2) 4_477 4_477 ? O2 Na3 Na1 41.4(2) 4_477 4_477 ? O11 Na3 Na1 118.6(2) . 4_477 ? O13 Na3 Na1 125.4(3) . 4_477 ? P3 Na3 Na1 61.71(10) 4_477 4_477 ? Co2 Na3 Na1 130.84(14) . 4_477 ? O12 Na3 Na1 173.0(2) . 2_675 ? O3 Na3 Na1 74.7(2) 2_685 2_675 ? O8 Na3 Na1 102.4(2) . 2_675 ? O4 Na3 Na1 41.6(2) 4_477 2_675 ? O2 Na3 Na1 82.7(2) 4_477 2_675 ? O11 Na3 Na1 116.4(2) . 2_675 ? O13 Na3 Na1 48.3(3) . 2_675 ? P3 Na3 Na1 54.98(10) 4_477 2_675 ? Co2 Na3 Na1 135.74(14) . 2_675 ? Na1 Na3 Na1 92.07(8) 4_477 2_675 ? O12 Na3 Na2 35.5(2) . 4_577 ? O3 Na3 Na2 82.5(2) 2_685 4_577 ? O8 Na3 Na2 90.4(2) . 4_577 ? O4 Na3 Na2 165.4(2) 4_477 4_577 ? O2 Na3 Na2 110.1(2) 4_477 4_577 ? O11 Na3 Na2 46.0(2) . 4_577 ? O13 Na3 Na2 113.6(3) . 4_577 ? P3 Na3 Na2 139.82(12) 4_477 4_577 ? Co2 Na3 Na2 50.37(7) . 4_577 ? Na1 Na3 Na2 82.79(11) 4_477 4_577 ? Na1 Na3 Na2 151.34(13) 2_675 4_577 ? O6 Na4 O1 173.0(3) . 2_674 ? O6 Na4 O13 93.3(3) . 2_674 ? O1 Na4 O13 90.8(4) 2_674 2_674 ? O6 Na4 O10 109.8(3) . 2_674 ? O1 Na4 O10 67.5(2) 2_674 2_674 ? O13 Na4 O10 154.5(4) 2_674 2_674 ? O6 Na4 O9 108.4(3) . 2_674 ? O1 Na4 O9 76.8(3) 2_674 2_674 ? O13 Na4 O9 95.6(3) 2_674 2_674 ? O10 Na4 O9 67.3(2) 2_674 2_674 ? O6 Na4 O7 91.9(2) . 3_746 ? O1 Na4 O7 82.1(3) 2_674 3_746 ? O13 Na4 O7 94.1(3) 2_674 3_746 ? O10 Na4 O7 95.9(3) 2_674 3_746 ? O9 Na4 O7 156.9(2) 2_674 3_746 ? O6 Na4 Co1 141.2(2) . 2_674 ? O1 Na4 Co1 41.2(2) 2_674 2_674 ? O13 Na4 Co1 110.2(3) 2_674 2_674 ? O10 Na4 Co1 44.5(2) 2_674 2_674 ? O9 Na4 Co1 41.08(14) 2_674 2_674 ? O7 Na4 Co1 115.8(2) 3_746 2_674 ? O6 Na4 Na2 123.1(2) . 2_674 ? O1 Na4 Na2 50.1(2) 2_674 2_674 ? O13 Na4 Na2 124.4(3) 2_674 2_674 ? O10 Na4 Na2 51.0(2) 2_674 2_674 ? O9 Na4 Na2 108.2(2) 2_674 2_674 ? O7 Na4 Na2 49.6(2) 3_746 2_674 ? Co1 Na4 Na2 68.36(9) 2_674 2_674 ? O6 Na4 Na1 68.9(2) . . ? O1 Na4 Na1 110.0(2) 2_674 . ? O13 Na4 Na1 49.4(3) 2_674 . ? O10 Na4 Na1 149.3(2) 2_674 . ? O9 Na4 Na1 143.2(2) 2_674 . ? O7 Na4 Na1 54.3(2) 3_746 . ? Co1 Na4 Na1 149.38(14) 2_674 . ? Na2 Na4 Na1 102.57(13) 2_674 . ? O6 Na4 Na2 81.8(2) . 3_656 ? O1 Na4 Na2 99.6(2) 2_674 3_656 ? O13 Na4 Na2 131.7(3) 2_674 3_656 ? O10 Na4 Na2 46.0(2) 2_674 3_656 ? O9 Na4 Na2 43.3(2) 2_674 3_656 ? O7 Na4 Na2 133.9(2) 3_746 3_656 ? Co1 Na4 Na2 59.39(8) 2_674 3_656 ? Na2 Na4 Na2 96.86(10) 2_674 3_656 ? Na1 Na4 Na2 150.39(13) . 3_656 ? P4 O1 Co1 131.7(4) . . ? P4 O1 Na4 133.1(4) . 2_675 ? Co1 O1 Na4 89.4(3) . 2_675 ? P4 O1 Na2 103.2(4) . . ? Co1 O1 Na2 102.9(3) . . ? Na4 O1 Na2 84.2(2) 2_675 . ? P3 O2 Co1 130.6(4) . . ? P3 O2 Na1 122.1(4) . . ? Co1 O2 Na1 100.2(3) . . ? P3 O2 Na3 90.8(3) . 4_577 ? Co1 O2 Na3 114.2(3) . 4_577 ? Na1 O2 Na3 91.2(3) . 4_577 ? P2 O3 Na3 139.1(4) . 2_684 ? P2 O3 Na1 106.6(3) . 3_756 ? Na3 O3 Na1 95.1(2) 2_684 3_756 ? P3 O4 Co2 129.2(4) . . ? P3 O4 Na1 102.3(3) . 3_756 ? Co2 O4 Na1 112.1(3) . 3_756 ? P3 O4 Na3 94.7(3) . 4_577 ? Co2 O4 Na3 117.8(3) . 4_577 ? Na1 O4 Na3 94.3(3) 3_756 4_577 ? P2 O5 Co1 130.6(4) . 1_565 ? P2 O5 Na1 128.3(3) . 1_565 ? Co1 O5 Na1 99.5(2) 1_565 1_565 ? P3 O6 Na4 144.3(4) . . ? P3 O6 Na1 90.4(3) . 3_756 ? Na4 O6 Na1 119.4(3) . 3_756 ? P2 O7 Co2 118.7(4) . . ? P2 O7 Na2 117.1(3) . 4_577 ? Co2 O7 Na2 83.9(2) . 4_577 ? P2 O7 Na4 121.1(3) . 3_756 ? Co2 O7 Na4 119.1(3) . 3_756 ? Na2 O7 Na4 79.4(2) 4_577 3_756 ? P2 O7 Na1 86.6(3) . 3_756 ? Co2 O7 Na1 92.4(2) . 3_756 ? Na2 O7 Na1 154.8(3) 4_577 3_756 ? Na4 O7 Na1 80.7(2) 3_756 3_756 ? P4 O8 Co2 130.8(4) . . ? P4 O8 Na3 138.5(4) . . ? Co2 O8 Na3 90.1(3) . . ? P1 O9 Co1 135.1(4) . . ? P1 O9 Na4 139.4(4) . 2_675 ? Co1 O9 Na4 84.0(2) . 2_675 ? P1 O9 Na2 91.9(3) . 4_567 ? Co1 O9 Na2 95.5(3) . 4_567 ? Na4 O9 Na2 95.0(2) 2_675 4_567 ? P1 O10 Co1 134.4(4) 4_467 . ? P1 O10 Na4 143.9(4) 4_467 2_675 ? Co1 O10 Na4 81.7(2) . 2_675 ? P1 O10 Na2 93.8(4) 4_467 . ? Co1 O10 Na2 96.6(3) . . ? Na4 O10 Na2 79.5(2) 2_675 . ? P1 O10 Na2 88.8(3) 4_467 4_567 ? Co1 O10 Na2 88.7(3) . 4_567 ? Na4 O10 Na2 92.5(3) 2_675 4_567 ? Na2 O10 Na2 169.6(3) . 4_567 ? P4 O11 Co2 122.0(4) 4_577 . ? P4 O11 Na3 155.9(4) 4_577 . ? Co2 O11 Na3 81.3(2) . . ? P4 O11 Na2 89.5(3) 4_577 4_577 ? Co2 O11 Na2 77.3(2) . 4_577 ? Na3 O11 Na2 90.2(2) . 4_577 ? P1 O12 Co2 122.5(4) 4_477 . ? P1 O12 Na3 137.4(4) 4_477 . ? Co2 O12 Na3 90.1(2) . . ? P1 O12 Na2 99.1(3) 4_477 4_577 ? Co2 O12 Na2 84.2(3) . 4_577 ? Na3 O12 Na2 111.9(3) . 4_577 ? Na4 O13 Na1 86.2(4) 2_675 2_675 ? Na4 O13 Na3 125.0(5) 2_675 . ? Na1 O13 Na3 82.9(3) 2_675 . ? Na4 O13 H1 111.0(100) 2_675 . ? Na1 O13 H1 162.5(100) 2_675 . ? Na3 O13 H1 84.5(100) . . ? Na4 O13 H2 116.1(100) 2_675 . ? Na1 O13 H2 106.1(100) 2_675 . ? Na3 O13 H2 118.7(100) . . ? H1 O13 H2 69.8(100) . . ? Na2 O14 H3 109.6(52) . . ? Na2 O14 H4 119.0(70) . . ? H3 O14 H4 85.3(81) . . ? P4 C1 P3 113.6(6) . . ? P4 C1 H5 106.5(46) . . ? P3 C1 H5 104.9(48) . . ? P4 C1 H6 115.5(64) . . ? P3 C1 H6 107.0(65) . . ? H5 C1 H6 108.8(80) . . ? P1 C2 P2 112.7(6) 4_477 . ? P1 C2 H7 117.4(60) 4_477 . ? P2 C2 H7 97.8(65) . . ? P1 C2 H8 108.5(73) 4_477 . ? P2 C2 H8 107.5(78) . . ? H7 C2 H8 112.2(100) . . ? _refine_diff_density_max 0.312 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.072 #===END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; NaCo2(O3PCH2CH2CH2PO3)(OH) ; _chemical_name_common 'sodium-cobalt propylene diphosphonate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H7 Co2 Na O7 P2' _chemical_formula_weight 357.88 _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' 'Co' 'Co' 0.3494 0.9721 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 6.123(1) _cell_length_b 16.634(3) _cell_length_c 18.780(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1912.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pink' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.486 _exptl_crystal_density_method ? _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 3.857 _exptl_absorpt_correction_type 'Xabs' _exptl_absorpt_correction_T_min 0.4656 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; NaCo2(O3PCH2CH2CH2PO3)(OH) ; _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% '0' _diffrn_reflns_number 962 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 24.96 _reflns_number_total 962 _reflns_number_observed 607 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-V5.0' _computing_publication_material 'SHELXTL-V5.0' _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^)+(0.0244P)^2^+26.0684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 962 _refine_ls_number_parameters 87 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_obs 0.0608 _refine_ls_wR_factor_all 0.1467 _refine_ls_wR_factor_obs 0.1121 _refine_ls_goodness_of_fit_all 1.097 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.096 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.0000 0.43124(11) 0.55967(10) 0.0111(5) Uani 1 d S . Co2 Co 0.2500 0.2500 0.5000 0.0113(5) Uani 1 d S . P1 P 0.0000 0.3714(2) 0.4013(2) 0.0128(9) Uani 1 d S . P2 P 0.5000 0.3908(2) 0.5997(2) 0.0099(8) Uani 1 d S . O1 O 0.5000 0.3316(6) 0.5372(5) 0.014(2) Uani 1 d S . O2 O 0.2980(13) 0.4448(4) 0.5970(3) 0.023(2) Uani 1 d . . O3 O 0.2104(12) 0.3226(3) 0.4104(3) 0.014(2) Uani 1 d . . O4 O 0.0000 0.3062(5) 0.5534(5) 0.008(2) Uani 1 d SD . H H 0.0000 0.2977(189) 0.6060(30) 0.198(169) Uiso 1 d SD . O5 O 0.0000 0.4428(5) 0.4537(5) 0.013(2) Uiso 1 d S . C1 C 0.0000 0.4186(8) 0.3160(7) 0.018(4) Uani 1 d S . H1A H -0.1273 0.4533(8) 0.3138(7) 0.022 Uiso 0.50 calc PR . H1B H 0.1273 0.4533(8) 0.3138(7) 0.022 Uiso 0.50 calc PR . C2 C 0.5000 0.3356(9) 0.6829(7) 0.022(4) Uani 1 d S . H2A H 0.3724 0.3011(9) 0.6836(7) 0.026 Uiso 0.50 calc PR . H2B H 0.6276 0.3011(9) 0.6836(7) 0.026 Uiso 0.50 calc PR . C3 C 0.5000 0.3848(14) 0.7500 0.033(7) Uani 1 d S . H3A H 0.3721 0.4192(14) 0.7500 0.039 Uiso 0.50 calc SPR . H3B H 0.6279 0.4192(14) 0.7500 0.039 Uiso 0.50 calc SPR . C4 C 0.0000 0.3674(13) 0.2500 0.033(7) Uani 1 d S . H4A H 0.1282 0.3332(13) 0.2500 0.040 Uiso 0.50 calc SPR . H4B H -0.1282 0.3332(13) 0.2500 0.040 Uiso 0.50 calc SPR . Na Na 0.5000 0.4191(3) 0.4289(3) 0.031(2) Uani 1 d S . 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 Co1 0.0103(10) 0.0122(9) 0.0108(9) -0.0008(8) 0.000 0.000 Co2 0.0100(10) 0.0113(7) 0.0127(8) 0.0002(7) -0.0012(8) 0.0013(9) P1 0.019(2) 0.011(2) 0.009(2) 0.0020(14) 0.000 0.000 P2 0.007(2) 0.014(2) 0.009(2) 0.0000(14) 0.000 0.000 O1 0.015(6) 0.015(4) 0.013(5) 0.000(4) 0.000 0.000 O2 0.028(5) 0.019(3) 0.023(4) -0.011(3) -0.008(4) 0.007(4) O3 0.010(4) 0.017(3) 0.015(3) 0.004(3) 0.004(3) 0.002(3) O4 0.012(5) 0.003(4) 0.009(5) -0.004(4) 0.000 0.000 C1 0.027(10) 0.012(6) 0.015(7) -0.003(5) 0.000 0.000 C2 0.032(11) 0.021(7) 0.013(8) 0.005(6) 0.000 0.000 C3 0.047(19) 0.028(12) 0.024(12) 0.000 0.000 0.000 C4 0.071(23) 0.020(10) 0.009(10) 0.000 0.000 0.000 Na 0.032(4) 0.019(3) 0.041(4) 0.004(3) 0.000 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 Co1 O2 1.968(8) . ? Co1 O2 1.968(8) 12 ? Co1 O5 1.999(9) . ? Co1 O4 2.083(8) . ? Co1 O5 2.110(9) 9_566 ? Co2 O4 2.055(6) . ? Co2 O4 2.056(6) 13_556 ? Co2 O3 2.086(6) . ? Co2 O3 2.086(6) 13_556 ? Co2 O1 2.162(6) . ? Co2 O1 2.162(6) 13_556 ? Co2 Na 3.470(5) 13_556 ? Co2 Na 3.470(5) . ? P1 O3 1.533(7) 12 ? P1 O3 1.533(7) . ? P1 O5 1.542(9) . ? P1 C1 1.784(13) . ? P1 Na 3.205(2) 1_455 ? P1 Na 3.205(2) . ? P2 O2 1.529(7) . ? P2 O2 1.529(8) 12_655 ? P2 O1 1.533(10) . ? P2 C2 1.812(14) . ? P2 Na 3.206(7) 9_666 ? P2 Na 3.242(8) . ? O1 Co2 2.162(6) 8_556 ? O1 Na 2.500(11) . ? O2 Na 2.624(9) 9_666 ? O3 Na 2.417(8) . ? O4 Co2 2.055(6) 8_456 ? O4 H 1.00(3) . ? O5 Co1 2.110(9) 9_566 ? C1 C4 1.50(2) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 C3 1.50(2) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C2 1.50(2) 10_557 ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C1 1.50(2) 10_556 ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? Na O3 2.417(8) 12_655 ? Na O2 2.624(9) 9_666 ? Na O2 2.624(8) 4_566 ? Na P1 3.205(2) 1_655 ? Na P2 3.206(7) 9_666 ? Na Co2 3.470(5) 8_556 ? Na Na 3.790(13) 9_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 O2 Co1 O2 136.1(4) . 12 ? O2 Co1 O5 110.1(2) . . ? O2 Co1 O5 110.1(2) 12 . ? O2 Co1 O4 97.7(2) . . ? O2 Co1 O4 97.7(2) 12 . ? O5 Co1 O4 92.3(4) . . ? O2 Co1 O5 85.9(2) . 9_566 ? O2 Co1 O5 85.9(2) 12 9_566 ? O5 Co1 O5 77.6(4) . 9_566 ? O4 Co1 O5 169.9(4) . 9_566 ? O4 Co2 O4 179.998(1) . 13_556 ? O4 Co2 O3 92.5(3) . . ? O4 Co2 O3 87.5(3) 13_556 . ? O4 Co2 O3 87.5(3) . 13_556 ? O4 Co2 O3 92.5(3) 13_556 13_556 ? O3 Co2 O3 179.999(2) . 13_556 ? O4 Co2 O1 94.8(2) . . ? O4 Co2 O1 85.2(2) 13_556 . ? O3 Co2 O1 88.8(3) . . ? O3 Co2 O1 91.2(3) 13_556 . ? O4 Co2 O1 85.2(2) . 13_556 ? O4 Co2 O1 94.8(2) 13_556 13_556 ? O3 Co2 O1 91.2(3) . 13_556 ? O3 Co2 O1 88.8(3) 13_556 13_556 ? O1 Co2 O1 180.0 . 13_556 ? O4 Co2 Na 81.5(2) . 13_556 ? O4 Co2 Na 98.5(2) 13_556 13_556 ? O3 Co2 Na 136.8(2) . 13_556 ? O3 Co2 Na 43.2(2) 13_556 13_556 ? O1 Co2 Na 134.2(3) . 13_556 ? O1 Co2 Na 45.8(3) 13_556 13_556 ? O4 Co2 Na 98.5(2) . . ? O4 Co2 Na 81.5(2) 13_556 . ? O3 Co2 Na 43.2(2) . . ? O3 Co2 Na 136.8(2) 13_556 . ? O1 Co2 Na 45.8(3) . . ? O1 Co2 Na 134.2(3) 13_556 . ? Na Co2 Na 180.0 13_556 . ? O3 P1 O3 114.4(5) 12 . ? O3 P1 O5 109.7(3) 12 . ? O3 P1 O5 109.7(3) . . ? O3 P1 C1 109.5(3) 12 . ? O3 P1 C1 109.5(3) . . ? O5 P1 C1 103.5(5) . . ? O3 P1 Na 46.4(3) 12 1_455 ? O3 P1 Na 156.4(3) . 1_455 ? O5 P1 Na 72.91(12) . 1_455 ? C1 P1 Na 92.1(2) . 1_455 ? O3 P1 Na 156.4(3) 12 . ? O3 P1 Na 46.4(3) . . ? O5 P1 Na 72.91(12) . . ? C1 P1 Na 92.1(2) . . ? Na P1 Na 145.6(2) 1_455 . ? O2 P2 O2 107.9(6) . 12_655 ? O2 P2 O1 110.6(3) . . ? O2 P2 O1 110.6(3) 12_655 . ? O2 P2 C2 109.1(4) . . ? O2 P2 C2 109.1(4) 12_655 . ? O1 P2 C2 109.6(6) . . ? O2 P2 Na 54.2(3) . 9_666 ? O2 P2 Na 54.2(3) 12_655 9_666 ? O1 P2 Na 120.3(4) . 9_666 ? C2 P2 Na 130.1(5) . 9_666 ? O2 P2 Na 83.2(3) . . ? O2 P2 Na 83.2(3) 12_655 . ? O1 P2 Na 48.3(4) . . ? C2 P2 Na 157.9(5) . . ? Na P2 Na 72.0(2) 9_666 . ? P2 O1 Co2 130.6(3) . . ? P2 O1 Co2 130.6(3) . 8_556 ? Co2 O1 Co2 90.1(3) . 8_556 ? P2 O1 Na 104.4(5) . . ? Co2 O1 Na 95.9(3) . . ? Co2 O1 Na 95.9(3) 8_556 . ? P2 O2 Co1 134.0(4) . . ? P2 O2 Na 97.6(4) . 9_666 ? Co1 O2 Na 118.0(3) . 9_666 ? P1 O3 Co2 119.6(4) . . ? P1 O3 Na 106.3(3) . . ? Co2 O3 Na 100.5(3) . . ? Co2 O4 Co2 96.3(3) 8_456 . ? Co2 O4 Co1 118.8(3) 8_456 . ? Co2 O4 Co1 118.8(3) . . ? Co2 O4 H 114.7(100) 8_456 . ? Co2 O4 H 114.7(100) . . ? Co1 O4 H 94.9(100) . . ? P1 O5 Co1 124.1(5) . . ? P1 O5 Co1 133.5(5) . 9_566 ? Co1 O5 Co1 102.4(4) . 9_566 ? C4 C1 P1 119.4(10) . . ? C4 C1 H1A 107.5(4) . . ? P1 C1 H1A 107.5(2) . . ? C4 C1 H1B 107.5(4) . . ? P1 C1 H1B 107.5(2) . . ? H1A C1 H1B 107.0 . . ? C3 C2 P2 116.6(11) . . ? C3 C2 H2A 108.2(5) . . ? P2 C2 H2A 108.2(2) . . ? C3 C2 H2B 108.2(5) . . ? P2 C2 H2B 108.2(2) . . ? H2A C2 H2B 107.3 . . ? C2 C3 C2 114.0(17) . 10_557 ? C2 C3 H3A 108.7(5) . . ? C2 C3 H3A 108.7(5) 10_557 . ? C2 C3 H3B 108.7(4) . . ? C2 C3 H3B 108.7(4) 10_557 . ? H3A C3 H3B 107.6 . . ? C1 C4 C1 111.0(17) 10_556 . ? C1 C4 H4A 109.4(4) 10_556 . ? C1 C4 H4A 109.4(4) . . ? C1 C4 H4B 109.4(4) 10_556 . ? C1 C4 H4B 109.4(4) . . ? H4A C4 H4B 108.0 . . ? O3 Na O3 94.4(4) 12_655 . ? O3 Na O1 74.4(2) 12_655 . ? O3 Na O1 74.4(2) . . ? O3 Na O2 101.6(2) 12_655 9_666 ? O3 Na O2 153.1(3) . 9_666 ? O1 Na O2 130.7(3) . 9_666 ? O3 Na O2 153.1(3) 12_655 4_566 ? O3 Na O2 101.6(2) . 4_566 ? O1 Na O2 130.7(3) . 4_566 ? O2 Na O2 56.2(3) 9_666 4_566 ? O3 Na P1 120.9(3) 12_655 . ? O3 Na P1 27.3(2) . . ? O1 Na P1 89.29(14) . . ? O2 Na P1 129.3(2) 9_666 . ? O2 Na P1 74.5(2) 4_566 . ? O3 Na P1 27.3(2) 12_655 1_655 ? O3 Na P1 120.9(3) . 1_655 ? O1 Na P1 89.29(14) . 1_655 ? O2 Na P1 74.5(2) 9_666 1_655 ? O2 Na P1 129.3(2) 4_566 1_655 ? P1 Na P1 145.6(2) . 1_655 ? O3 Na P2 129.1(2) 12_655 9_666 ? O3 Na P2 129.1(2) . 9_666 ? O1 Na P2 135.3(3) . 9_666 ? O2 Na P2 28.2(2) 9_666 9_666 ? O2 Na P2 28.2(2) 4_566 9_666 ? P1 Na P2 102.52(11) . 9_666 ? P1 Na P2 102.52(11) 1_655 9_666 ? O3 Na P2 92.6(2) 12_655 . ? O3 Na P2 92.6(2) . . ? O1 Na P2 27.2(2) . . ? O2 Na P2 108.0(2) 9_666 . ? O2 Na P2 108.0(2) 4_566 . ? P1 Na P2 97.14(13) . . ? P1 Na P2 97.14(13) 1_655 . ? P2 Na P2 108.0(2) 9_666 . ? O3 Na Co2 80.8(2) 12_655 . ? O3 Na Co2 36.2(2) . . ? O1 Na Co2 38.3(2) . . ? O2 Na Co2 168.1(3) 9_666 . ? O2 Na Co2 124.2(2) 4_566 . ? P1 Na Co2 55.95(8) . . ? P1 Na Co2 106.44(15) 1_655 . ? P2 Na Co2 149.76(11) 9_666 . ? P2 Na Co2 60.12(11) . . ? O3 Na Co2 36.2(2) 12_655 8_556 ? O3 Na Co2 80.8(2) . 8_556 ? O1 Na Co2 38.3(2) . 8_556 ? O2 Na Co2 124.2(2) 9_666 8_556 ? O2 Na Co2 168.1(3) 4_566 8_556 ? P1 Na Co2 106.44(15) . 8_556 ? P1 Na Co2 55.95(8) 1_655 8_556 ? P2 Na Co2 149.76(12) 9_666 8_556 ? P2 Na Co2 60.12(11) . 8_556 ? Co2 Na Co2 52.36(8) . 8_556 ? O3 Na Na 125.0(2) 12_655 9_666 ? O3 Na Na 125.0(2) . 9_666 ? O1 Na Na 80.8(3) . 9_666 ? O2 Na Na 61.2(2) 9_666 9_666 ? O2 Na Na 61.2(2) 4_566 9_666 ? P1 Na Na 106.84(12) . 9_666 ? P1 Na Na 106.84(12) 1_655 9_666 ? P2 Na Na 54.4(2) 9_666 9_666 ? P2 Na Na 53.6(2) . 9_666 ? Co2 Na Na 107.7(2) . 9_666 ? Co2 Na Na 107.7(2) 8_556 9_666 ? _refine_diff_density_max 1.708 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.243 #===END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; Co2(O3P-CH2-PO3).H2O ; _chemical_name_common 'Cobalt Methylene Diphosphonate Monohydrate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H4 Co2 O7 P2' _chemical_formula_weight 307.84 _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' 'Co' 'Co' 0.3494 0.9721 '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 18.820(4) _cell_length_b 8.246(2) _cell_length_c 8.916(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.68(3) _cell_angle_gamma 90.00 _cell_volume 1325.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.085 _exptl_crystal_density_method ? _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 5.481 _exptl_absorpt_correction_type 'Xabs-Empirical Absorption Correction' _exptl_absorpt_correction_T_min 0.6418 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; Co2(O3P-CH2-PO3).H2O ; _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 Enraf_Nonius_CAD4 _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -1.2% _diffrn_reflns_number 2322 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1164 _reflns_number_observed 906 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction SDP_Package_(Enraf-Nonius,_1985) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _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^)+(0.0509P)^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 'fixed distance model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1164 _refine_ls_number_parameters 122 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_obs 0.0456 _refine_ls_wR_factor_all 0.1158 _refine_ls_wR_factor_obs 0.1028 _refine_ls_goodness_of_fit_all 1.110 _refine_ls_goodness_of_fit_obs 1.134 _refine_ls_restrained_S_all 1.114 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.0000 0.0274(2) 0.7500 0.0100(4) Uani 1 d S . Co2 Co -0.18535(6) -0.11187(12) 0.56574(11) 0.0078(3) Uani 1 d . . Co3 Co -0.2500 0.2500 0.5000 0.0078(4) Uani 1 d S . P1 P -0.30560(11) 0.0446(2) 0.7430(2) 0.0068(4) Uani 1 d . . P2 P -0.09390(11) -0.1774(2) 0.9242(2) 0.0071(5) Uani 1 d . . O1 O -0.2536(3) 0.0447(6) 0.6376(6) 0.0102(11) Uani 1 d . . O2 O -0.2791(3) 0.1703(6) 0.8717(6) 0.0094(11) Uani 1 d . . O3 O -0.1598(3) -0.1173(6) 0.9738(6) 0.0093(11) Uani 1 d . . O4 O -0.0880(3) -0.0942(6) 0.7718(6) 0.0090(11) Uani 1 d . . O5 O -0.3163(3) -0.1220(6) 0.8043(6) 0.0098(11) Uani 1 d . . O6 O -0.1168(3) -0.2252(7) 0.4596(7) 0.0149(13) Uani 1 d D . H1 H -0.0647(51) -0.2289(158) 0.4769(179) 0.084(48) Uiso 1 d D . H2 H -0.1382(81) -0.2764(148) 0.3478(116) 0.086(48) Uiso 1 d D . O7 O -0.0217(3) -0.1557(6) 1.0567(6) 0.0138(12) Uani 1 d . . C C -0.1040(4) -0.3901(9) 0.8800(9) 0.008(2) Uiso 1 d D . H3 H -0.0986(51) -0.4549(91) 0.9628(92) 0.018(23) Uiso 1 d D . H4 H -0.0686(57) -0.4204(118) 0.7993(118) 0.050(32) Uiso 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 Co1 0.0086(8) 0.0126(8) 0.0087(7) 0.000 0.0023(6) 0.000 Co2 0.0083(6) 0.0070(5) 0.0080(5) 0.0003(4) 0.0022(4) 0.0000(4) Co3 0.0096(8) 0.0064(7) 0.0078(7) 0.0001(6) 0.0033(6) 0.0010(6) P1 0.0085(10) 0.0056(9) 0.0064(9) 0.0004(7) 0.0025(8) 0.0007(8) P2 0.0066(10) 0.0086(10) 0.0064(9) -0.0014(7) 0.0022(8) -0.0012(8) O1 0.017(3) 0.005(2) 0.011(3) 0.000(2) 0.008(2) 0.000(2) O2 0.012(3) 0.006(2) 0.010(3) -0.002(2) 0.004(2) 0.002(2) O3 0.011(3) 0.005(3) 0.013(3) -0.002(2) 0.005(2) -0.001(2) O4 0.013(3) 0.008(3) 0.006(3) 0.001(2) 0.003(2) -0.004(2) O5 0.012(3) 0.008(3) 0.011(3) -0.001(2) 0.006(2) -0.003(2) O6 0.014(3) 0.018(3) 0.016(3) -0.009(2) 0.008(3) -0.002(2) O7 0.010(3) 0.016(3) 0.016(3) -0.005(2) 0.005(2) -0.001(2) _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 Co1 O7 1.963(5) 6 ? Co1 O7 1.963(5) 5_557 ? Co1 O4 1.992(5) 2_556 ? Co1 O4 1.992(5) . ? Co2 O6 2.033(6) . ? Co2 O2 2.049(5) 4_446 ? Co2 O1 2.050(5) . ? Co2 O2 2.142(5) 6 ? Co2 O3 2.169(5) 6 ? Co2 O4 2.196(5) . ? Co3 O3 2.089(5) 6 ? Co3 O3 2.089(5) 4_456 ? Co3 O1 2.103(5) 7_456 ? Co3 O1 2.104(5) . ? Co3 O5 2.113(5) 4_456 ? Co3 O5 2.113(5) 6 ? P1 O5 1.513(5) . ? P1 O2 1.520(5) . ? P1 O1 1.539(6) . ? P1 C 1.821(8) 4_456 ? P2 O3 1.514(6) . ? P2 O7 1.534(6) . ? P2 O4 1.554(5) . ? P2 C 1.796(8) . ? O2 Co2 2.049(5) 4_456 ? O2 Co2 2.142(5) 6_556 ? O3 Co3 2.089(5) 4_446 ? O3 Co2 2.169(5) 6_556 ? O5 Co3 2.113(5) 4_446 ? O6 H1 0.95(9) . ? O6 H2 1.05(9) . ? O7 Co1 1.963(5) 5_557 ? C P1 1.821(8) 4_446 ? C H3 0.89(7) . ? C H4 1.14(8) . ? 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 Co1 O7 114.7(3) 6 5_557 ? O7 Co1 O4 98.9(2) 6 2_556 ? O7 Co1 O4 112.8(2) 5_557 2_556 ? O7 Co1 O4 112.8(2) 6 . ? O7 Co1 O4 98.9(2) 5_557 . ? O4 Co1 O4 119.6(3) 2_556 . ? O6 Co2 O2 91.4(2) . 4_446 ? O6 Co2 O1 166.8(2) . . ? O2 Co2 O1 100.6(2) 4_446 . ? O6 Co2 O2 90.3(2) . 6 ? O2 Co2 O2 76.4(2) 4_446 6 ? O1 Co2 O2 87.1(2) . 6 ? O6 Co2 O3 89.2(2) . 6 ? O2 Co2 O3 172.8(2) 4_446 6 ? O1 Co2 O3 78.3(2) . 6 ? O2 Co2 O3 96.4(2) 6 6 ? O6 Co2 O4 86.1(2) . . ? O2 Co2 O4 95.1(2) 4_446 . ? O1 Co2 O4 98.3(2) . . ? O2 Co2 O4 170.7(2) 6 . ? O3 Co2 O4 92.1(2) 6 . ? O3 Co3 O3 179.997(1) 6 4_456 ? O3 Co3 O1 101.1(2) 6 7_456 ? O3 Co3 O1 78.9(2) 4_456 7_456 ? O3 Co3 O1 78.9(2) 6 . ? O3 Co3 O1 101.1(2) 4_456 . ? O1 Co3 O1 179.998(1) 7_456 . ? O3 Co3 O5 92.8(2) 6 4_456 ? O3 Co3 O5 87.3(2) 4_456 4_456 ? O1 Co3 O5 88.2(2) 7_456 4_456 ? O1 Co3 O5 91.8(2) . 4_456 ? O3 Co3 O5 87.3(2) 6 6 ? O3 Co3 O5 92.7(2) 4_456 6 ? O1 Co3 O5 91.8(2) 7_456 6 ? O1 Co3 O5 88.2(2) . 6 ? O5 Co3 O5 179.997(1) 4_456 6 ? O5 P1 O2 113.3(3) . . ? O5 P1 O1 113.2(3) . . ? O2 P1 O1 109.4(3) . . ? O5 P1 C 106.8(3) . 4_456 ? O2 P1 C 107.5(3) . 4_456 ? O1 P1 C 106.2(3) . 4_456 ? O3 P2 O7 110.8(3) . . ? O3 P2 O4 112.4(3) . . ? O7 P2 O4 110.6(3) . . ? O3 P2 C 109.9(3) . . ? O7 P2 C 107.3(3) . . ? O4 P2 C 105.6(3) . . ? P1 O1 Co2 139.1(3) . . ? P1 O1 Co3 119.3(3) . . ? Co2 O1 Co3 101.3(2) . . ? P1 O2 Co2 137.8(3) . 4_456 ? P1 O2 Co2 118.1(3) . 6_556 ? Co2 O2 Co2 103.6(2) 4_456 6_556 ? P2 O3 Co3 128.4(3) . 4_446 ? P2 O3 Co2 133.2(3) . 6_556 ? Co3 O3 Co2 97.9(2) 4_446 6_556 ? P2 O4 Co1 125.3(3) . . ? P2 O4 Co2 116.8(3) . . ? Co1 O4 Co2 118.0(2) . . ? P1 O5 Co3 130.1(3) . 4_446 ? Co2 O6 H1 134.6(89) . . ? Co2 O6 H2 120.4(83) . . ? H1 O6 H2 103.8(100) . . ? P2 O7 Co1 130.8(3) . 5_557 ? P2 C P1 116.3(4) . 4_446 ? P2 C H3 115.0(55) . . ? P1 C H3 100.7(59) 4_446 . ? P2 C H4 107.9(51) . . ? P1 C H4 99.8(56) 4_446 . ? H3 C H4 116.3(77) . . ? _refine_diff_density_max 0.853 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.212