data_11207 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H48 Ca2 Na2 O52 V10' _chemical_formula_weight 1515.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.74899(19) _cell_length_b 10.9746(3) _cell_length_c 12.8216(9) _cell_angle_alpha 114.492(8) _cell_angle_beta 105.093(7) _cell_angle_gamma 91.111(6) _cell_volume 1070.25(8) _cell_formula_units_Z 1 _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 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 2.479 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7552 _exptl_absorpt_correction_T_max 0.9293 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20535 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4885 _reflns_number_gt 3806 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.9223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4885 _refine_ls_number_parameters 371 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.80250(6) 0.47931(5) 0.46000(4) 0.01906(13) Uani 1 1 d . . . V2 V 0.99343(6) 0.24235(5) 0.47322(4) 0.02104(13) Uani 1 1 d . . . V3 V 0.99148(6) 0.51228(5) 0.29221(4) 0.02221(13) Uani 1 1 d . . . V4 V 0.82947(7) 0.72650(6) 0.69749(5) 0.02664(14) Uani 1 1 d . . . V5 V 0.80443(7) 0.23481(5) 0.22879(5) 0.02638(14) Uani 1 1 d . . . Na Na 0.52096(17) 0.13866(14) 0.63539(13) 0.0385(3) Uani 1 1 d . . . Ca Ca 0.32122(9) 0.32248(7) 0.93686(6) 0.03122(17) Uani 1 1 d . . . O1 O 0.0075(2) 0.60774(19) 0.60314(17) 0.0187(4) Uani 1 1 d . . . O2 O 0.8517(2) 0.6002(2) 0.39478(17) 0.0200(4) Uani 1 1 d . . . O3 O 0.8527(2) 0.3721(2) 0.54700(18) 0.0205(4) Uani 1 1 d . . . O4 O 0.6901(3) 0.5781(2) 0.5410(2) 0.0261(5) Uani 1 1 d . . . O5 O 0.1481(3) 0.4111(2) 0.25020(19) 0.0270(5) Uani 1 1 d . . . O6 O 0.1475(3) 0.1888(2) 0.39888(19) 0.0258(5) Uani 1 1 d . . . O7 O 0.6752(3) 0.3604(2) 0.33217(19) 0.0260(5) Uani 1 1 d . . . O8 O 0.8277(3) 0.1560(2) 0.33586(19) 0.0260(5) Uani 1 1 d . . . O9 O 0.8269(3) 0.3793(2) 0.18775(18) 0.0265(5) Uani 1 1 d . . . O10 O 1.0175(3) 0.8267(2) 0.81227(19) 0.0291(5) Uani 1 1 d . . . O11 O 0.9925(3) 0.1471(2) 0.5410(2) 0.0295(5) Uani 1 1 d . . . O12 O 0.6942(3) 0.7998(3) 0.7534(2) 0.0385(6) Uani 1 1 d . . . O13 O 0.6594(3) 0.1333(2) 0.1177(2) 0.0405(6) Uani 1 1 d . . . O14 O 0.0128(3) 0.3894(2) 0.7732(2) 0.0327(5) Uani 1 1 d . . . OW1 O 0.5575(4) 0.3016(4) 0.5709(3) 0.0622(10) Uani 1 1 d D . . H1A H 0.482(4) 0.343(5) 0.545(5) 0.075 Uiso 1 1 d D . . H1B H 0.649(3) 0.324(5) 0.566(5) 0.075 Uiso 1 1 d D . . OW2 O 0.4723(4) 0.9660(3) 0.6947(3) 0.0577(8) Uani 1 1 d D . . H2A H 0.377(3) 0.908(4) 0.661(4) 0.069 Uiso 1 1 d D . . H2B H 0.550(4) 0.911(4) 0.695(4) 0.069 Uiso 1 1 d D . . OW3 O 0.6999(3) 0.9971(3) 0.5364(2) 0.0386(6) Uani 1 1 d D . . H3A H 0.790(4) 1.038(4) 0.532(4) 0.046 Uiso 1 1 d D . . H3B H 0.745(4) 0.937(3) 0.562(4) 0.046 Uiso 1 1 d D . . OW4 O 0.7456(3) 0.2575(3) 0.8106(3) 0.0445(7) Uani 1 1 d D . . H4A H 0.787(5) 0.201(4) 0.840(4) 0.053 Uiso 1 1 d D . . H4B H 0.819(4) 0.295(4) 0.795(4) 0.053 Uiso 1 1 d D . . OW5 O 0.3774(3) 0.3281(3) 0.7602(2) 0.0322(5) Uani 1 1 d D . . H5A H 0.450(4) 0.394(3) 0.781(3) 0.039 Uiso 1 1 d D . . H5B H 0.300(3) 0.326(4) 0.699(3) 0.039 Uiso 1 1 d D . . OW6 O 0.4855(6) 0.1541(4) 0.9129(3) 0.0908(15) Uani 1 1 d D . . H6A H 0.560(6) 0.151(6) 0.972(3) 0.109 Uiso 1 1 d D . . H6B H 0.480(7) 0.082(5) 0.840(3) 0.109 Uiso 1 1 d D . . OW7 O 0.0909(4) 0.3804(4) 0.0099(3) 0.0698(11) Uani 1 1 d D . . H7A H 0.100(7) 0.293(3) -0.012(4) 0.084 Uiso 1 1 d D . . H7B H 0.086(7) 0.407(5) 0.086(3) 0.084 Uiso 1 1 d D . . OW8 O 0.1337(4) 0.1336(3) 0.7663(2) 0.0445(7) Uani 1 1 d D . . H8A H 0.137(5) 0.048(3) 0.743(4) 0.053 Uiso 1 1 d D . . H8B H 0.092(5) 0.145(4) 0.701(3) 0.053 Uiso 1 1 d D . . OW9 O 0.3551(3) 0.5686(3) 0.9940(2) 0.0376(6) Uani 1 1 d D . . H9A H 0.310(5) 0.614(4) 1.052(3) 0.045 Uiso 1 1 d D . . H9B H 0.294(4) 0.579(4) 0.930(3) 0.045 Uiso 1 1 d D . . OW10 O 0.4256(3) 0.4199(3) 0.1656(2) 0.0370(6) Uani 1 1 d D . . H10A H 0.513(3) 0.409(4) 0.210(3) 0.044 Uiso 1 1 d D . . H10B H 0.348(3) 0.423(4) 0.199(3) 0.044 Uiso 1 1 d D . . OW11 O 0.2414(8) 0.1424(5) 0.0012(4) 0.069(2) Uani 0.650(10) 1 d PD . . H11A H 0.270(10) 0.057(5) -0.033(6) 0.083 Uiso 0.650(10) 1 d PD . . H11B H 0.261(10) 0.156(7) 0.079(3) 0.083 Uiso 0.650(10) 1 d PD . . OW12 O 0.8861(5) 0.0970(4) 0.9242(3) 0.0718(10) Uani 1 1 d D . . H12A H 0.930(6) 0.029(4) 0.885(4) 0.086 Uiso 1 1 d D . . H12B H 0.948(6) 0.174(3) 0.965(5) 0.086 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0178(2) 0.0203(3) 0.0209(3) 0.0116(2) 0.00411(19) 0.00305(19) V2 0.0266(3) 0.0174(3) 0.0199(3) 0.0105(2) 0.0042(2) 0.0034(2) V3 0.0305(3) 0.0215(3) 0.0191(3) 0.0122(2) 0.0085(2) 0.0063(2) V4 0.0324(3) 0.0263(3) 0.0257(3) 0.0128(2) 0.0126(2) 0.0120(2) V5 0.0314(3) 0.0212(3) 0.0200(3) 0.0079(2) -0.0010(2) 0.0015(2) Na 0.0377(8) 0.0349(8) 0.0420(8) 0.0176(7) 0.0092(6) 0.0045(6) Ca 0.0447(4) 0.0260(3) 0.0213(3) 0.0063(3) 0.0141(3) 0.0035(3) O1 0.0207(10) 0.0188(10) 0.0174(10) 0.0094(8) 0.0042(8) 0.0027(8) O2 0.0213(10) 0.0204(10) 0.0197(10) 0.0110(8) 0.0041(8) 0.0044(8) O3 0.0214(10) 0.0209(10) 0.0228(10) 0.0125(9) 0.0073(8) 0.0035(8) O4 0.0218(11) 0.0293(12) 0.0316(12) 0.0162(10) 0.0097(9) 0.0079(9) O5 0.0357(13) 0.0272(12) 0.0246(11) 0.0141(10) 0.0140(10) 0.0106(10) O6 0.0321(12) 0.0236(11) 0.0255(11) 0.0138(9) 0.0086(9) 0.0109(9) O7 0.0232(11) 0.0252(11) 0.0273(11) 0.0131(10) 0.0008(9) 0.0010(9) O8 0.0272(11) 0.0211(11) 0.0258(11) 0.0108(9) 0.0011(9) -0.0005(9) O9 0.0330(12) 0.0256(11) 0.0193(10) 0.0117(9) 0.0019(9) 0.0056(9) O10 0.0404(13) 0.0248(11) 0.0213(11) 0.0096(9) 0.0082(10) 0.0095(10) O11 0.0387(13) 0.0232(11) 0.0288(12) 0.0154(10) 0.0066(10) 0.0043(10) O12 0.0438(15) 0.0415(14) 0.0411(14) 0.0217(12) 0.0225(12) 0.0204(12) O13 0.0452(15) 0.0298(13) 0.0306(13) 0.0104(11) -0.0088(11) -0.0024(11) O14 0.0494(15) 0.0293(12) 0.0290(12) 0.0185(10) 0.0168(11) 0.0101(11) OW1 0.0345(16) 0.092(3) 0.106(3) 0.082(2) 0.0271(17) 0.0186(16) OW2 0.0458(17) 0.059(2) 0.087(2) 0.049(2) 0.0197(17) 0.0113(15) OW3 0.0328(14) 0.0360(14) 0.0543(17) 0.0271(13) 0.0114(12) 0.0091(11) OW4 0.0389(15) 0.0513(17) 0.0428(16) 0.0218(14) 0.0095(12) 0.0007(13) OW5 0.0291(13) 0.0394(14) 0.0292(13) 0.0180(11) 0.0049(10) 0.0042(11) OW6 0.122(3) 0.050(2) 0.064(2) 0.0251(19) -0.032(2) 0.015(2) OW7 0.0468(19) 0.123(3) 0.0310(16) 0.026(2) 0.0110(14) 0.006(2) OW8 0.0619(18) 0.0328(14) 0.0338(14) 0.0177(12) 0.0008(13) 0.0057(13) OW9 0.0469(16) 0.0406(15) 0.0267(13) 0.0165(12) 0.0092(11) 0.0156(12) OW10 0.0347(14) 0.0485(15) 0.0357(14) 0.0249(13) 0.0118(11) 0.0091(12) OW11 0.131(6) 0.040(3) 0.035(3) 0.014(2) 0.028(3) -0.001(3) OW12 0.101(3) 0.052(2) 0.061(2) 0.0200(18) 0.029(2) 0.019(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 V1 O7 1.688(2) . ? V1 O4 1.692(2) . ? V1 O3 1.917(2) . ? V1 O2 1.931(2) . ? V1 O1 2.110(2) 2_666 ? V1 O1 2.148(2) 1_655 ? V1 V5 3.0694(8) . ? V1 V4 3.0723(8) . ? V2 O11 1.614(2) . ? V2 O6 1.818(2) 1_655 ? V2 O8 1.826(2) . ? V2 O2 1.994(2) 2_766 ? V2 O3 1.999(2) . ? V2 O1 2.2354(19) 2_666 ? V2 V3 3.0624(8) 2_766 ? V2 V5 3.1055(7) . ? V2 V4 3.1105(8) 2_766 ? V3 O14 1.614(2) 2_666 ? V3 O9 1.814(2) . ? V3 O5 1.829(2) 1_655 ? V3 O2 1.997(2) . ? V3 O3 2.005(2) 2_766 ? V3 O1 2.2350(19) 2_666 ? V3 V2 3.0624(8) 2_766 ? V3 V5 3.1101(8) . ? V3 V4 3.1108(7) 2_766 ? V4 O12 1.601(2) . ? V4 O10 1.846(2) . ? V4 O6 1.873(2) 2_666 ? V4 O5 1.885(2) 2_666 ? V4 O4 2.026(2) . ? V4 O1 2.311(2) 1_655 ? V4 V5 3.0612(8) 2_766 ? V4 V2 3.1105(8) 2_766 ? V4 V3 3.1108(7) 2_766 ? V5 O13 1.603(2) . ? V5 O10 1.826(2) 2_766 ? V5 O8 1.876(2) . ? V5 O9 1.887(2) . ? V5 O7 2.064(2) . ? V5 O1 2.300(2) 2_666 ? V5 V4 3.0612(8) 2_766 ? Na OW1 2.308(3) . ? Na OW2 2.384(3) 1_545 ? Na OW3 2.399(3) 2_666 ? Na OW4 2.405(3) . ? Na OW3 2.443(3) 1_545 ? Na OW5 2.617(3) . ? Na Na 3.462(3) 2_656 ? Ca OW6 2.332(4) . ? Ca OW7 2.425(3) 1_556 ? Ca OW8 2.452(3) . ? Ca OW5 2.464(2) . ? Ca OW9 2.476(3) . ? Ca OW10 2.559(3) 1_556 ? Ca OW11 2.583(5) 1_556 ? Ca OW9 2.814(3) 2_667 ? Ca Ca 4.3873(14) 2_667 ? O1 V1 2.110(2) 2_666 ? O1 V1 2.1484(19) 1_455 ? O1 V3 2.2350(19) 2_666 ? O1 V2 2.2355(19) 2_666 ? O1 V5 2.300(2) 2_666 ? O1 V4 2.311(2) 1_455 ? O2 V2 1.994(2) 2_766 ? O3 V3 2.005(2) 2_766 ? O5 V3 1.829(2) 1_455 ? O5 V4 1.885(2) 2_666 ? O6 V2 1.818(2) 1_455 ? O6 V4 1.873(2) 2_666 ? O10 V5 1.826(2) 2_766 ? O14 V3 1.614(2) 2_666 ? OW1 H1A 0.89(3) . ? OW1 H1B 0.86(3) . ? OW2 Na 2.384(3) 1_565 ? OW2 H2A 0.92(3) . ? OW2 H2B 0.91(3) . ? OW3 Na 2.399(3) 2_666 ? OW3 Na 2.443(3) 1_565 ? OW3 H3A 0.92(2) . ? OW3 H3B 0.91(2) . ? OW4 H4A 0.89(2) . ? OW4 H4B 0.86(2) . ? OW5 H5A 0.86(2) . ? OW5 H5B 0.89(2) . ? OW6 H6A 0.88(3) . ? OW6 H6B 0.93(3) . ? OW7 Ca 2.425(3) 1_554 ? OW7 H7A 0.89(3) . ? OW7 H7B 0.91(3) . ? OW8 H8A 0.87(2) . ? OW8 H8B 0.88(2) . ? OW9 Ca 2.814(3) 2_667 ? OW9 H9A 0.90(2) . ? OW9 H9B 0.91(2) . ? OW10 Ca 2.559(3) 1_554 ? OW10 H10A 0.87(2) . ? OW10 H10B 0.88(2) . ? OW11 Ca 2.583(5) 1_554 ? OW11 H11A 0.93(3) . ? OW11 H11B 0.92(3) . ? OW12 H12A 0.87(3) . ? OW12 H12B 0.87(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 V1 O4 107.18(11) . . ? O7 V1 O3 98.56(10) . . ? O4 V1 O3 97.24(10) . . ? O7 V1 O2 97.24(10) . . ? O4 V1 O2 96.39(10) . . ? O3 V1 O2 155.05(9) . . ? O7 V1 O1 87.89(9) . 2_666 ? O4 V1 O1 164.92(9) . 2_666 ? O3 V1 O1 80.69(8) . 2_666 ? O2 V1 O1 80.72(8) . 2_666 ? O7 V1 O1 166.16(10) . 1_655 ? O4 V1 O1 86.65(9) . 1_655 ? O3 V1 O1 79.95(8) . 1_655 ? O2 V1 O1 80.09(8) . 1_655 ? O1 V1 O1 78.28(8) 2_666 1_655 ? O7 V1 V5 39.39(8) . . ? O4 V1 V5 146.56(8) . . ? O3 V1 V5 89.91(6) . . ? O2 V1 V5 90.15(6) . . ? O1 V1 V5 48.51(5) 2_666 . ? O1 V1 V5 126.79(6) 1_655 . ? O7 V1 V4 145.13(8) . . ? O4 V1 V4 37.95(8) . . ? O3 V1 V4 88.98(6) . . ? O2 V1 V4 89.02(6) . . ? O1 V1 V4 126.98(6) 2_666 . ? O1 V1 V4 48.70(5) 1_655 . ? V5 V1 V4 175.49(2) . . ? O11 V2 O6 103.92(11) . 1_655 ? O11 V2 O8 102.84(11) . . ? O6 V2 O8 94.43(10) 1_655 . ? O11 V2 O2 99.12(10) . 2_766 ? O6 V2 O2 89.92(9) 1_655 2_766 ? O8 V2 O2 155.84(9) . 2_766 ? O11 V2 O3 98.99(10) . . ? O6 V2 O3 154.97(9) 1_655 . ? O8 V2 O3 90.14(9) . . ? O2 V2 O3 76.51(8) 2_766 . ? O11 V2 O1 173.95(10) . 2_666 ? O6 V2 O1 80.59(8) 1_655 2_666 ? O8 V2 O1 80.61(8) . 2_666 ? O2 V2 O1 76.67(8) 2_766 2_666 ? O3 V2 O1 75.90(8) . 2_666 ? O11 V2 V3 88.71(8) . 2_766 ? O6 V2 V3 129.82(7) 1_655 2_766 ? O8 V2 V3 130.31(8) . 2_766 ? O2 V2 V3 39.91(6) 2_766 2_766 ? O3 V2 V3 40.17(6) . 2_766 ? O1 V2 V3 85.29(5) 2_666 2_766 ? O11 V2 V5 136.22(9) . . ? O6 V2 V5 83.05(7) 1_655 . ? O8 V2 V5 33.51(7) . . ? O2 V2 V5 124.33(6) 2_766 . ? O3 V2 V5 87.39(6) . . ? O1 V2 V5 47.67(5) 2_666 . ? V3 V2 V5 120.14(2) 2_766 . ? O11 V2 V4 136.94(9) . 2_766 ? O6 V2 V4 33.11(7) 1_655 2_766 ? O8 V2 V4 83.99(7) . 2_766 ? O2 V2 V4 86.84(6) 2_766 2_766 ? O3 V2 V4 123.71(6) . 2_766 ? O1 V2 V4 47.86(5) 2_666 2_766 ? V3 V2 V4 119.29(2) 2_766 2_766 ? V5 V2 V4 59.006(18) . 2_766 ? O14 V3 O9 101.92(11) 2_666 . ? O14 V3 O5 103.26(11) 2_666 1_655 ? O9 V3 O5 95.01(10) . 1_655 ? O14 V3 O2 98.88(10) 2_666 . ? O9 V3 O2 90.29(9) . . ? O5 V3 O2 155.60(9) 1_655 . ? O14 V3 O3 100.73(11) 2_666 2_766 ? O9 V3 O3 155.19(9) . 2_766 ? O5 V3 O3 89.50(9) 1_655 2_766 ? O2 V3 O3 76.32(8) . 2_766 ? O14 V3 O1 174.66(10) 2_666 2_666 ? O9 V3 O1 80.58(8) . 2_666 ? O5 V3 O1 81.10(8) 1_655 2_666 ? O2 V3 O1 76.30(8) . 2_666 ? O3 V3 O1 76.04(8) 2_766 2_666 ? O14 V3 V2 89.70(9) 2_666 2_766 ? O9 V3 V2 130.13(8) . 2_766 ? O5 V3 V2 129.53(7) 1_655 2_766 ? O2 V3 V2 39.84(6) . 2_766 ? O3 V3 V2 40.03(6) 2_766 2_766 ? O1 V3 V2 85.11(5) 2_666 2_766 ? O14 V3 V5 135.35(9) 2_666 . ? O9 V3 V5 33.58(7) . . ? O5 V3 V5 83.66(7) 1_655 . ? O2 V3 V5 87.80(6) . . ? O3 V3 V5 123.62(6) 2_766 . ? O1 V3 V5 47.59(5) 2_666 . ? V2 V3 V5 119.95(2) 2_766 . ? O14 V3 V4 136.76(9) 2_666 2_766 ? O9 V3 V4 84.06(7) . 2_766 ? O5 V3 V4 33.68(7) 1_655 2_766 ? O2 V3 V4 124.08(6) . 2_766 ? O3 V3 V4 86.35(6) 2_766 2_766 ? O1 V3 V4 47.86(5) 2_666 2_766 ? V2 V3 V4 119.14(2) 2_766 2_766 ? V5 V3 V4 58.955(17) . 2_766 ? O12 V4 O10 103.28(12) . . ? O12 V4 O6 102.35(11) . 2_666 ? O10 V4 O6 90.83(10) . 2_666 ? O12 V4 O5 101.66(12) . 2_666 ? O10 V4 O5 90.89(10) . 2_666 ? O6 V4 O5 154.85(10) 2_666 2_666 ? O12 V4 O4 99.95(12) . . ? O10 V4 O4 156.77(10) . . ? O6 V4 O4 83.96(9) 2_666 . ? O5 V4 O4 84.63(10) 2_666 . ? O12 V4 O1 175.15(11) . 1_655 ? O10 V4 O1 81.57(9) . 1_655 ? O6 V4 O1 77.49(8) 2_666 1_655 ? O5 V4 O1 77.96(8) 2_666 1_655 ? O4 V4 O1 75.20(8) . 1_655 ? O12 V4 V5 136.59(10) . 2_766 ? O10 V4 V5 33.31(7) . 2_766 ? O6 V4 V5 83.52(7) 2_666 2_766 ? O5 V4 V5 84.23(7) 2_666 2_766 ? O4 V4 V5 123.45(6) . 2_766 ? O1 V4 V5 48.26(5) 1_655 2_766 ? O12 V4 V1 130.86(10) . . ? O10 V4 V1 125.86(7) . . ? O6 V4 V1 79.22(7) 2_666 . ? O5 V4 V1 79.48(7) 2_666 . ? O4 V4 V1 30.91(6) . . ? O1 V4 V1 44.29(5) 1_655 . ? V5 V4 V1 92.55(2) 2_766 . ? O12 V4 V2 134.34(9) . 2_766 ? O10 V4 V2 82.06(7) . 2_766 ? O6 V4 V2 32.04(7) 2_666 2_766 ? O5 V4 V2 123.78(7) 2_666 2_766 ? O4 V4 V2 81.58(6) . 2_766 ? O1 V4 V2 45.82(5) 1_655 2_766 ? V5 V4 V2 60.415(18) 2_766 2_766 ? V1 V4 V2 61.778(17) . 2_766 ? O12 V4 V3 134.16(9) . 2_766 ? O10 V4 V3 81.78(7) . 2_766 ? O6 V4 V3 123.29(7) 2_666 2_766 ? O5 V4 V3 32.56(7) 2_666 2_766 ? O4 V4 V3 82.26(6) . 2_766 ? O1 V4 V3 45.81(5) 1_655 2_766 ? V5 V4 V3 60.512(18) 2_766 2_766 ? V1 V4 V3 61.921(17) . 2_766 ? V2 V4 V3 91.46(2) 2_766 2_766 ? O13 V5 O10 103.75(13) . 2_766 ? O13 V5 O8 101.77(12) . . ? O10 V5 O8 92.12(10) 2_766 . ? O13 V5 O9 102.04(11) . . ? O10 V5 O9 91.57(10) 2_766 . ? O8 V5 O9 154.27(9) . . ? O13 V5 O7 99.30(12) . . ? O10 V5 O7 156.93(9) 2_766 . ? O8 V5 O7 84.09(9) . . ? O9 V5 O7 82.60(9) . . ? O13 V5 O1 173.95(12) . 2_666 ? O10 V5 O1 82.30(9) 2_766 2_666 ? O8 V5 O1 77.89(8) . 2_666 ? O9 V5 O1 77.40(8) . 2_666 ? O7 V5 O1 74.65(8) . 2_666 ? O13 V5 V4 137.49(11) . 2_766 ? O10 V5 V4 33.74(7) 2_766 2_766 ? O8 V5 V4 84.65(7) . 2_766 ? O9 V5 V4 84.38(7) . 2_766 ? O7 V5 V4 123.21(6) . 2_766 ? O1 V5 V4 48.56(5) 2_666 2_766 ? O13 V5 V1 130.55(11) . . ? O10 V5 V1 125.69(7) 2_766 . ? O8 V5 V1 78.79(7) . . ? O9 V5 V1 78.41(7) . . ? O7 V5 V1 31.26(6) . . ? O1 V5 V1 43.39(5) 2_666 . ? V4 V5 V1 91.96(2) 2_766 . ? O13 V5 V2 134.22(10) . . ? O10 V5 V2 82.50(7) 2_766 . ? O8 V5 V2 32.50(6) . . ? O9 V5 V2 123.32(7) . . ? O7 V5 V2 82.18(6) . . ? O1 V5 V2 45.92(5) 2_666 . ? V4 V5 V2 60.578(18) 2_766 . ? V1 V5 V2 61.499(17) . . ? O13 V5 V3 134.10(9) . . ? O10 V5 V3 82.09(7) 2_766 . ? O8 V5 V3 123.72(7) . . ? O9 V5 V3 32.12(6) . . ? O7 V5 V3 81.19(6) . . ? O1 V5 V3 45.84(5) 2_666 . ? V4 V5 V3 60.534(18) 2_766 . ? V1 V5 V3 61.444(17) . . ? V2 V5 V3 91.56(2) . . ? OW1 Na OW2 177.40(13) . 1_545 ? OW1 Na OW3 95.11(12) . 2_666 ? OW2 Na OW3 82.33(11) 1_545 2_666 ? OW1 Na OW4 89.56(12) . . ? OW2 Na OW4 93.01(12) 1_545 . ? OW3 Na OW4 175.01(11) 2_666 . ? OW1 Na OW3 94.30(12) . 1_545 ? OW2 Na OW3 86.05(11) 1_545 1_545 ? OW3 Na OW3 88.73(10) 2_666 1_545 ? OW4 Na OW3 89.17(10) . 1_545 ? OW1 Na OW5 79.06(11) . . ? OW2 Na OW5 100.99(11) 1_545 . ? OW3 Na OW5 100.86(10) 2_666 . ? OW4 Na OW5 81.73(10) . . ? OW3 Na OW5 168.72(10) 1_545 . ? OW1 Na Na 96.59(12) . 2_656 ? OW2 Na Na 81.89(11) 1_545 2_656 ? OW3 Na Na 44.87(7) 2_666 2_656 ? OW4 Na Na 132.86(10) . 2_656 ? OW3 Na Na 43.86(7) 1_545 2_656 ? OW5 Na Na 145.35(9) . 2_656 ? OW6 Ca OW7 137.38(16) . 1_556 ? OW6 Ca OW8 81.04(12) . . ? OW7 Ca OW8 85.05(12) 1_556 . ? OW6 Ca OW5 85.37(13) . . ? OW7 Ca OW5 129.65(10) 1_556 . ? OW8 Ca OW5 75.98(9) . . ? OW6 Ca OW9 136.65(14) . . ? OW7 Ca OW9 80.63(12) 1_556 . ? OW8 Ca OW9 131.55(9) . . ? OW5 Ca OW9 78.42(9) . . ? OW6 Ca OW10 91.94(12) . 1_556 ? OW7 Ca OW10 73.66(10) 1_556 1_556 ? OW8 Ca OW10 139.87(9) . 1_556 ? OW5 Ca OW10 143.19(9) . 1_556 ? OW9 Ca OW10 78.67(9) . 1_556 ? OW6 Ca OW11 66.09(19) . 1_556 ? OW7 Ca OW11 71.30(17) 1_556 1_556 ? OW8 Ca OW11 69.50(14) . 1_556 ? OW5 Ca OW11 137.71(13) . 1_556 ? OW9 Ca OW11 143.55(13) . 1_556 ? OW10 Ca OW11 71.55(13) 1_556 1_556 ? OW6 Ca OW9 68.71(13) . 2_667 ? OW7 Ca OW9 137.46(11) 1_556 2_667 ? OW8 Ca OW9 137.34(9) . 2_667 ? OW5 Ca OW9 72.36(8) . 2_667 ? OW9 Ca OW9 68.10(9) . 2_667 ? OW10 Ca OW9 72.51(8) 1_556 2_667 ? OW11 Ca OW9 119.83(16) 1_556 2_667 ? OW6 Ca Ca 100.23(12) . 2_667 ? OW7 Ca Ca 112.38(10) 1_556 2_667 ? OW8 Ca Ca 147.79(7) . 2_667 ? OW5 Ca Ca 72.09(6) . 2_667 ? OW9 Ca Ca 36.52(6) . 2_667 ? OW10 Ca Ca 72.32(6) 1_556 2_667 ? OW11 Ca Ca 140.63(13) 1_556 2_667 ? OW9 Ca Ca 31.58(5) 2_667 2_667 ? V1 O1 V1 101.72(8) 2_666 1_455 ? V1 O1 V3 93.17(7) 2_666 2_666 ? V1 O1 V3 93.04(7) 1_455 2_666 ? V1 O1 V2 93.16(7) 2_666 2_666 ? V1 O1 V2 92.76(7) 1_455 2_666 ? V3 O1 V2 170.39(10) 2_666 2_666 ? V1 O1 V5 88.10(7) 2_666 2_666 ? V1 O1 V5 170.18(10) 1_455 2_666 ? V3 O1 V5 86.58(7) 2_666 2_666 ? V2 O1 V5 86.40(7) 2_666 2_666 ? V1 O1 V4 171.27(10) 2_666 1_455 ? V1 O1 V4 87.01(7) 1_455 1_455 ? V3 O1 V4 86.34(7) 2_666 1_455 ? V2 O1 V4 86.31(7) 2_666 1_455 ? V5 O1 V4 83.18(7) 2_666 1_455 ? V1 O2 V2 107.92(9) . 2_766 ? V1 O2 V3 106.96(9) . . ? V2 O2 V3 100.24(9) 2_766 . ? V1 O3 V2 107.46(9) . . ? V1 O3 V3 108.42(10) . 2_766 ? V2 O3 V3 99.80(9) . 2_766 ? V1 O4 V4 111.14(11) . . ? V3 O5 V4 113.75(11) 1_455 2_666 ? V2 O6 V4 114.85(11) 1_455 2_666 ? V1 O7 V5 109.36(11) . . ? V2 O8 V5 113.99(11) . . ? V3 O9 V5 114.30(11) . . ? V5 O10 V4 112.95(11) 2_766 . ? Na OW1 H1A 126(3) . . ? Na OW1 H1B 121(3) . . ? H1A OW1 H1B 113(4) . . ? Na OW2 H2A 122(3) 1_565 . ? Na OW2 H2B 115(3) 1_565 . ? H2A OW2 H2B 105(3) . . ? Na OW3 Na 91.27(10) 2_666 1_565 ? Na OW3 H3A 124(3) 2_666 . ? Na OW3 H3A 119(3) 1_565 . ? Na OW3 H3B 104(3) 2_666 . ? Na OW3 H3B 120(3) 1_565 . ? H3A OW3 H3B 100(3) . . ? Na OW4 H4A 110(3) . . ? Na OW4 H4B 112(3) . . ? H4A OW4 H4B 109(3) . . ? Ca OW5 Na 119.41(10) . . ? Ca OW5 H5A 111(3) . . ? Na OW5 H5A 96(3) . . ? Ca OW5 H5B 122(2) . . ? Na OW5 H5B 97(3) . . ? H5A OW5 H5B 108(3) . . ? Ca OW6 H6A 124(4) . . ? Ca OW6 H6B 125(4) . . ? H6A OW6 H6B 111(4) . . ? Ca OW7 H7A 68(4) 1_554 . ? Ca OW7 H7B 128(3) 1_554 . ? H7A OW7 H7B 102(3) . . ? Ca OW8 H8A 128(3) . . ? Ca OW8 H8B 117(3) . . ? H8A OW8 H8B 107(3) . . ? Ca OW9 Ca 111.90(9) . 2_667 ? Ca OW9 H9A 112(3) . . ? Ca OW9 H9A 111(3) 2_667 . ? Ca OW9 H9B 106(3) . . ? Ca OW9 H9B 113(3) 2_667 . ? H9A OW9 H9B 103(3) . . ? Ca OW10 H10A 129(3) 1_554 . ? Ca OW10 H10B 112(3) 1_554 . ? H10A OW10 H10B 109(3) . . ? Ca OW11 H11A 119(5) 1_554 . ? Ca OW11 H11B 125(5) 1_554 . ? H11A OW11 H11B 101(4) . . ? H12A OW12 H12B 116(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 H1A O4 0.89(3) 2.05(3) 2.925(4) 171(5) 2_666 OW1 H1B O3 0.86(3) 1.96(3) 2.810(3) 178(5) . OW2 H2A O8 0.92(3) 1.93(3) 2.779(4) 153(4) 2_666 OW2 H2B O12 0.91(3) 2.00(3) 2.859(4) 156(5) . OW3 H3A O11 0.92(2) 2.07(3) 2.991(3) 174(4) 1_565 OW3 H3B O6 0.91(2) 1.84(3) 2.750(3) 172(4) 2_666 OW4 H4A OW12 0.89(2) 1.95(3) 2.830(5) 173(4) . OW4 H4B O14 0.86(2) 2.11(3) 2.970(4) 174(4) 1_655 OW5 H5A OW10 0.86(2) 2.04(3) 2.881(4) 165(4) 2_666 OW5 H5B O2 0.89(2) 1.97(3) 2.805(3) 157(3) 2_666 OW6 H6A O13 0.88(3) 1.93(3) 2.773(4) 160(6) 1_556 OW6 H6B OW2 0.93(3) 1.75(3) 2.672(6) 171(6) 1_545 OW7 H7A OW11 0.89(3) 2.12(4) 2.921(7) 149(5) . OW7 H7A OW12 0.89(3) 2.53(5) 3.165(5) 129(5) 1_454 OW7 H7B O5 0.91(3) 2.02(3) 2.861(4) 155(4) . OW7 H7B O14 0.91(3) 2.56(4) 3.243(4) 133(4) 2_566 OW8 H8A O8 0.87(2) 2.10(3) 2.958(3) 168(4) 2_656 OW8 H8B O11 0.88(2) 2.02(3) 2.897(3) 173(4) 1_455 OW9 H9A OW4 0.90(2) 1.94(3) 2.818(4) 167(4) 2_667 OW9 H9B O9 0.91(2) 1.84(3) 2.739(3) 173(4) 2_666 OW10 H10A O7 0.87(2) 2.08(3) 2.922(3) 164(4) . OW10 H10B O5 0.88(2) 2.05(2) 2.921(3) 172(4) . OW11 H11A O13 0.93(3) 2.11(3) 3.032(6) 176(7) 2_655 OW11 H11B O12 0.92(3) 1.92(3) 2.834(5) 175(7) 2_666 OW12 H12A O10 0.87(3) 2.26(3) 3.105(4) 164(5) 1_545 OW12 H12B OW7 0.87(3) 2.34(3) 3.165(5) 160(5) 1_656 OW12 H12B OW11 0.87(3) 2.55(5) 2.970(8) 111(4) 1_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.154 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.116