data_11945 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H38 Ca2 O46 V10' _chemical_formula_weight 1363.86 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' '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 9.7212(6) _cell_length_b 10.2598(8) _cell_length_c 10.5928(8) _cell_angle_alpha 89.999(6) _cell_angle_beta 77.083(7) _cell_angle_gamma 69.887(8) _cell_volume 963.55(12) _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 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 2.709 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5872 _exptl_absorpt_correction_T_max 0.8994 _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 18571 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4396 _reflns_number_gt 3440 _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^)+(0.0485P)^2^+0.1073P] 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 4396 _refine_ls_number_parameters 319 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.65439(5) 0.03563(4) 0.94782(4) 0.01912(12) Uani 1 1 d . . . V2 V 0.34785(5) 0.27089(5) 1.09318(5) 0.02374(13) Uani 1 1 d . . . V3 V 0.51790(5) 0.04014(5) 1.24712(4) 0.02206(12) Uani 1 1 d . . . V4 V 0.81413(5) -0.19828(5) 1.10355(5) 0.02525(13) Uani 1 1 d . . . V5 V 0.47686(5) 0.26110(5) 0.79393(5) 0.02551(13) Uani 1 1 d . . . Ca Ca 0.83962(7) 0.26607(6) 1.41299(6) 0.02816(15) Uani 1 1 d . . . O1 O 0.4263(2) 0.09869(17) 0.93156(16) 0.0205(4) Uani 1 1 d . . . O2 O 0.5596(2) 0.15842(18) 1.10244(17) 0.0217(4) Uani 1 1 d . . . O3 O 0.6720(2) -0.10466(18) 0.81782(17) 0.0213(4) Uani 1 1 d . . . O4 O 0.6755(2) 0.15763(18) 0.84533(18) 0.0246(4) Uani 1 1 d . . . O5 O 0.7195(2) -0.04444(19) 1.23251(18) 0.0254(4) Uani 1 1 d . . . O6 O 0.8241(2) -0.04398(19) 0.98196(18) 0.0253(4) Uani 1 1 d . . . O7 O 0.4664(2) -0.10244(19) 1.31933(18) 0.0253(4) Uani 1 1 d . . . O8 O 0.2763(2) 0.30383(19) 0.79403(19) 0.0280(4) Uani 1 1 d . . . O9 O 0.1693(2) 0.29926(19) 1.04793(19) 0.0265(4) Uani 1 1 d . . . O10 O 0.4241(2) 0.35638(18) 0.95846(19) 0.0270(4) Uani 1 1 d . . . O11 O 0.4653(2) 0.1539(2) 1.36944(19) 0.0314(5) Uani 1 1 d . . . O12 O 0.2999(3) 0.3837(2) 1.2148(2) 0.0360(5) Uani 1 1 d . . . O13 O 0.9835(2) -0.2523(2) 1.1212(2) 0.0365(5) Uani 1 1 d . . . O14 O 0.5284(3) 0.3660(2) 0.6995(2) 0.0379(5) Uani 1 1 d . . . OW1 O 0.7548(2) 0.0726(2) 1.4654(2) 0.0306(5) Uani 1 1 d D . . H1A H 0.742(3) 0.030(3) 1.398(2) 0.037 Uiso 1 1 d D . . H1B H 0.673(3) 0.088(3) 1.529(2) 0.037 Uiso 1 1 d D . . OW2 O 0.8885(3) 0.1343(2) 1.2015(2) 0.0380(5) Uani 1 1 d D . . H2A H 0.829(3) 0.091(3) 1.185(3) 0.046 Uiso 1 1 d D . . H2B H 0.975(2) 0.100(3) 1.147(3) 0.046 Uiso 1 1 d D . . OW3 O 1.0958(3) 0.1416(3) 1.3823(2) 0.0490(7) Uani 1 1 d D . . H3A H 1.133(4) 0.062(3) 1.420(3) 0.059 Uiso 1 1 d D . . H3B H 1.158(4) 0.137(4) 1.308(2) 0.059 Uiso 1 1 d D . . OW4 O 0.8363(4) -0.2909(3) 1.4248(3) 0.0689(9) Uani 1 1 d D . . H4A H 0.802(4) -0.236(4) 1.503(3) 0.083 Uiso 1 1 d D . . H4B H 0.759(4) -0.254(4) 1.384(3) 0.083 Uiso 1 1 d D . . OW5 O 0.9033(3) 0.4104(2) 1.2396(2) 0.0418(6) Uani 1 1 d D . . H5A H 0.981(3) 0.380(3) 1.174(3) 0.050 Uiso 1 1 d D . . H5B H 0.863(3) 0.5009(19) 1.243(3) 0.050 Uiso 1 1 d D . . OW6 O 0.5957(3) 0.3612(2) 1.3717(3) 0.0457(6) Uani 1 1 d D . . H6A H 0.529(3) 0.318(3) 1.389(4) 0.055 Uiso 1 1 d D . . H6B H 0.540(3) 0.4513(19) 1.373(4) 0.055 Uiso 1 1 d D . . OW7 O 0.8894(3) 0.2086(3) 1.6283(2) 0.0509(7) Uani 1 1 d D . . H7A H 0.951(3) 0.251(4) 1.637(3) 0.061 Uiso 1 1 d D . . H7B H 0.826(3) 0.216(4) 1.704(2) 0.061 Uiso 1 1 d D . . OW8 O 0.7847(4) 0.4827(3) 1.5249(2) 0.0649(8) Uani 1 1 d D . . H8A H 0.769(5) 0.494(4) 1.6093(18) 0.078 Uiso 1 1 d D . . H8B H 0.809(5) 0.551(3) 1.487(3) 0.078 Uiso 1 1 d D . . OW9 O 0.2864(3) 0.6429(3) 0.9472(3) 0.0537(7) Uani 1 1 d D . . H9A H 0.340(3) 0.554(2) 0.965(3) 0.064 Uiso 1 1 d D . . H9B H 0.353(3) 0.691(3) 0.938(3) 0.064 Uiso 1 1 d D . . H9C H 0.213(3) 0.684(3) 1.025(3) 0.064 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 0.0192(2) 0.0179(2) 0.0201(2) 0.00144(17) -0.00144(19) -0.00831(19) V2 0.0266(3) 0.0171(2) 0.0250(3) -0.00075(18) -0.0038(2) -0.00607(19) V3 0.0234(3) 0.0228(2) 0.0197(2) 0.00043(18) -0.0034(2) -0.0089(2) V4 0.0214(3) 0.0249(2) 0.0277(3) 0.00370(19) -0.0049(2) -0.0065(2) V5 0.0273(3) 0.0216(2) 0.0278(3) 0.00767(19) -0.0045(2) -0.0102(2) Ca 0.0265(3) 0.0278(3) 0.0294(3) 0.0016(2) -0.0036(3) -0.0105(2) O1 0.0221(10) 0.0200(9) 0.0194(10) 0.0014(7) -0.0030(8) -0.0088(8) O2 0.0228(10) 0.0196(9) 0.0233(10) -0.0003(7) -0.0024(8) -0.0100(8) O3 0.0198(10) 0.0223(9) 0.0204(10) 0.0007(7) -0.0010(8) -0.0079(8) O4 0.0252(11) 0.0234(10) 0.0265(10) 0.0042(8) -0.0024(8) -0.0123(8) O5 0.0244(10) 0.0298(10) 0.0228(10) 0.0014(8) -0.0055(8) -0.0107(8) O6 0.0207(10) 0.0277(10) 0.0264(10) 0.0024(8) -0.0016(8) -0.0097(8) O7 0.0277(11) 0.0269(10) 0.0207(10) 0.0050(8) -0.0024(8) -0.0107(8) O8 0.0281(11) 0.0240(10) 0.0298(11) 0.0066(8) -0.0065(9) -0.0068(8) O9 0.0226(10) 0.0234(10) 0.0283(10) -0.0004(8) -0.0011(8) -0.0045(8) O10 0.0313(11) 0.0190(9) 0.0306(11) 0.0035(8) -0.0044(9) -0.0107(8) O11 0.0324(12) 0.0331(11) 0.0264(11) -0.0046(9) -0.0033(9) -0.0111(9) O12 0.0403(13) 0.0280(11) 0.0353(12) -0.0066(9) -0.0051(10) -0.0090(10) O13 0.0259(12) 0.0409(12) 0.0377(12) 0.0015(10) -0.0060(10) -0.0063(10) O14 0.0439(14) 0.0334(11) 0.0418(13) 0.0172(10) -0.0124(11) -0.0190(10) OW1 0.0326(12) 0.0342(11) 0.0254(11) 0.0020(9) -0.0011(9) -0.0159(10) OW2 0.0371(13) 0.0383(12) 0.0367(13) -0.0082(10) 0.0059(10) -0.0202(11) OW3 0.0285(13) 0.0644(17) 0.0388(14) 0.0179(12) 0.0032(11) -0.0045(12) OW4 0.098(3) 0.084(2) 0.0487(18) 0.0154(15) -0.0301(17) -0.054(2) OW5 0.0427(14) 0.0267(11) 0.0438(14) 0.0030(10) 0.0108(11) -0.0101(10) OW6 0.0349(13) 0.0290(12) 0.0769(18) 0.0132(12) -0.0198(13) -0.0117(10) OW7 0.0453(16) 0.084(2) 0.0341(13) 0.0096(13) -0.0089(12) -0.0363(15) OW8 0.112(3) 0.0461(15) 0.0370(15) -0.0069(12) -0.0033(16) -0.0376(16) OW9 0.0514(17) 0.0380(14) 0.0708(19) 0.0027(13) -0.0111(14) -0.0166(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O6 1.691(2) . ? V1 O4 1.6925(18) . ? V1 O2 1.9094(18) . ? V1 O3 1.9294(18) . ? V1 O1 2.1078(17) 2_657 ? V1 O1 2.1326(18) . ? V1 V4 3.0780(7) . ? V1 V5 3.0821(7) . ? V2 O12 1.605(2) . ? V2 O10 1.8246(19) . ? V2 O9 1.831(2) . ? V2 O3 1.9948(18) 2_657 ? V2 O2 2.0091(19) . ? V2 O1 2.2636(17) . ? V2 V3 3.0837(7) . ? V2 V4 3.1066(7) 2_657 ? V3 O11 1.6114(19) . ? V3 O7 1.8189(18) . ? V3 O5 1.820(2) . ? V3 O3 2.0114(19) 2_657 ? V3 O2 2.0116(18) . ? V3 O1 2.2170(17) 2_657 ? V3 V5 3.1026(7) 2_657 ? V4 O13 1.601(2) . ? V4 O8 1.8306(19) 2_657 ? V4 O9 1.856(2) 2_657 ? V4 O5 1.9088(19) . ? V4 O6 2.0552(19) . ? V4 O1 2.3221(18) 2_657 ? V4 V5 3.0785(7) 2_657 ? V4 V2 3.1067(7) 2_657 ? V5 O14 1.5989(19) . ? V5 O8 1.845(2) . ? V5 O7 1.8655(19) 2_657 ? V5 O10 1.874(2) . ? V5 O4 2.053(2) . ? V5 O1 2.3207(17) . ? V5 V4 3.0785(7) 2_657 ? V5 V3 3.1026(7) 2_657 ? Ca OW3 2.321(2) . ? Ca OW8 2.352(2) . ? Ca OW6 2.374(2) . ? Ca OW1 2.419(2) . ? Ca OW5 2.464(2) . ? Ca OW7 2.466(3) . ? Ca OW2 2.481(2) . ? O1 V1 2.1079(17) 2_657 ? O1 V3 2.2170(17) 2_657 ? O1 V4 2.3221(18) 2_657 ? O3 V2 1.9948(18) 2_657 ? O3 V3 2.0114(19) 2_657 ? O7 V5 1.8655(19) 2_657 ? O8 V4 1.8307(19) 2_657 ? O9 V4 1.856(2) 2_657 ? OW1 H1A 0.888(17) . ? OW1 H1B 0.888(17) . ? OW2 H2A 0.879(17) . ? OW2 H2B 0.862(17) . ? OW3 H3A 0.905(18) . ? OW3 H3B 0.864(17) . ? OW4 H4A 0.929(18) . ? OW4 H4B 0.920(18) . ? OW5 H5A 0.870(17) . ? OW5 H5B 0.872(17) . ? OW6 H6A 0.894(18) . ? OW6 H6B 0.896(18) . ? OW7 H7A 0.872(18) . ? OW7 H7B 0.883(18) . ? OW8 H8A 0.873(18) . ? OW8 H8B 0.881(18) . ? OW9 H9A 0.923(17) . ? OW9 H9B 0.927(17) . ? OW9 H9C 0.942(17) . ? 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 O6 V1 O4 106.40(9) . . ? O6 V1 O2 98.07(9) . . ? O4 V1 O2 97.09(8) . . ? O6 V1 O3 97.02(9) . . ? O4 V1 O3 97.11(8) . . ? O2 V1 O3 155.42(8) . . ? O6 V1 O1 87.75(8) . 2_657 ? O4 V1 O1 165.84(8) . 2_657 ? O2 V1 O1 81.06(7) . 2_657 ? O3 V1 O1 80.27(7) . 2_657 ? O6 V1 O1 166.14(8) . . ? O4 V1 O1 87.41(8) . . ? O2 V1 O1 81.05(7) . . ? O3 V1 O1 79.67(7) . . ? O1 V1 O1 78.44(7) 2_657 . ? O6 V1 V4 38.82(6) . . ? O4 V1 V4 145.21(7) . . ? O2 V1 V4 90.88(6) . . ? O3 V1 V4 88.81(6) . . ? O1 V1 V4 48.93(5) 2_657 . ? O1 V1 V4 127.35(5) . . ? O6 V1 V5 145.01(6) . . ? O4 V1 V5 38.62(6) . . ? O2 V1 V5 89.44(6) . . ? O3 V1 V5 89.24(6) . . ? O1 V1 V5 127.22(5) 2_657 . ? O1 V1 V5 48.79(5) . . ? V4 V1 V5 175.984(19) . . ? O12 V2 O10 102.85(10) . . ? O12 V2 O9 102.97(10) . . ? O10 V2 O9 95.53(9) . . ? O12 V2 O3 101.30(9) . 2_657 ? O10 V2 O3 153.56(8) . 2_657 ? O9 V2 O3 89.37(8) . 2_657 ? O12 V2 O2 100.38(10) . . ? O10 V2 O2 89.07(8) . . ? O9 V2 O2 154.52(8) . . ? O3 V2 O2 76.11(7) 2_657 . ? O12 V2 O1 175.24(10) . . ? O10 V2 O1 80.07(7) . . ? O9 V2 O1 80.33(8) . . ? O3 V2 O1 75.16(7) 2_657 . ? O2 V2 O1 75.79(7) . . ? O12 V2 V3 90.77(8) . . ? O10 V2 V3 129.00(7) . . ? O9 V2 V3 129.24(6) . . ? O3 V2 V3 39.87(5) 2_657 . ? O2 V2 V3 39.95(5) . . ? O1 V2 V3 84.48(5) . . ? O12 V2 V4 135.50(8) . 2_657 ? O10 V2 V4 83.45(7) . 2_657 ? O9 V2 V4 32.82(6) . 2_657 ? O3 V2 V4 86.85(6) 2_657 2_657 ? O2 V2 V4 123.92(5) . 2_657 ? O1 V2 V4 48.15(5) . 2_657 ? V3 V2 V4 119.538(18) . 2_657 ? O11 V3 O7 102.54(9) . . ? O11 V3 O5 103.65(10) . . ? O7 V3 O5 95.44(9) . . ? O11 V3 O3 98.65(9) . 2_657 ? O7 V3 O3 89.91(8) . 2_657 ? O5 V3 O3 155.30(8) . 2_657 ? O11 V3 O2 99.49(9) . . ? O7 V3 O2 155.25(8) . . ? O5 V3 O2 90.15(8) . . ? O3 V3 O2 75.69(7) 2_657 . ? O11 V3 O1 173.72(9) . 2_657 ? O7 V3 O1 80.85(7) . 2_657 ? O5 V3 O1 81.13(8) . 2_657 ? O3 V3 O1 75.94(7) 2_657 2_657 ? O2 V3 O1 76.22(7) . 2_657 ? O11 V3 V2 88.56(8) . . ? O7 V3 V2 129.39(7) . . ? O5 V3 V2 130.03(6) . . ? O3 V3 V2 39.47(5) 2_657 . ? O2 V3 V2 39.89(5) . . ? O1 V3 V2 85.21(5) 2_657 . ? O11 V3 V5 135.55(7) . 2_657 ? O7 V3 V5 33.11(6) . 2_657 ? O5 V3 V5 84.32(6) . 2_657 ? O3 V3 V5 87.21(5) 2_657 2_657 ? O2 V3 V5 124.45(5) . 2_657 ? O1 V3 V5 48.28(4) 2_657 2_657 ? V2 V3 V5 119.779(19) . 2_657 ? O13 V4 O8 104.38(10) . 2_657 ? O13 V4 O9 102.87(10) . 2_657 ? O8 V4 O9 92.58(9) 2_657 2_657 ? O13 V4 O5 101.34(10) . . ? O8 V4 O5 90.73(9) 2_657 . ? O9 V4 O5 153.90(9) 2_657 . ? O13 V4 O6 99.64(9) . . ? O8 V4 O6 155.91(9) 2_657 . ? O9 V4 O6 83.76(8) 2_657 . ? O5 V4 O6 82.73(8) . . ? O13 V4 O1 173.68(9) . 2_657 ? O8 V4 O1 81.71(7) 2_657 2_657 ? O9 V4 O1 78.28(7) 2_657 2_657 ? O5 V4 O1 76.61(7) . 2_657 ? O6 V4 O1 74.23(7) . 2_657 ? O13 V4 V1 130.68(8) . . ? O8 V4 V1 124.89(6) 2_657 . ? O9 V4 V1 78.96(6) 2_657 . ? O5 V4 V1 77.95(6) . . ? O6 V4 V1 31.05(5) . . ? O1 V4 V1 43.18(4) 2_657 . ? O13 V4 V5 137.64(8) . 2_657 ? O8 V4 V5 33.26(6) 2_657 2_657 ? O9 V4 V5 85.03(6) 2_657 2_657 ? O5 V4 V5 83.64(6) . 2_657 ? O6 V4 V5 122.67(6) . 2_657 ? O1 V4 V5 48.45(4) 2_657 2_657 ? V1 V4 V5 91.631(18) . 2_657 ? O13 V4 V2 135.13(8) . 2_657 ? O8 V4 V2 82.22(7) 2_657 2_657 ? O9 V4 V2 32.33(6) 2_657 2_657 ? O5 V4 V2 123.17(6) . 2_657 ? O6 V4 V2 82.09(6) . 2_657 ? O1 V4 V2 46.56(4) 2_657 2_657 ? V1 V4 V2 61.944(15) . 2_657 ? V5 V4 V2 60.699(16) 2_657 2_657 ? O14 V5 O8 104.03(10) . . ? O14 V5 O7 101.78(10) . 2_657 ? O8 V5 O7 91.55(9) . 2_657 ? O14 V5 O10 102.73(10) . . ? O8 V5 O10 91.02(9) . . ? O7 V5 O10 153.93(8) 2_657 . ? O14 V5 O4 99.81(10) . . ? O8 V5 O4 156.15(8) . . ? O7 V5 O4 83.90(8) 2_657 . ? O10 V5 O4 83.33(8) . . ? O14 V5 O1 174.47(10) . . ? O8 V5 O1 81.45(7) . . ? O7 V5 O1 77.15(7) 2_657 . ? O10 V5 O1 77.59(7) . . ? O4 V5 O1 74.71(7) . . ? O14 V5 V4 137.01(8) . 2_657 ? O8 V5 V4 32.97(6) . 2_657 ? O7 V5 V4 84.61(6) 2_657 2_657 ? O10 V5 V4 83.52(6) . 2_657 ? O4 V5 V4 123.18(5) . 2_657 ? O1 V5 V4 48.49(5) . 2_657 ? O14 V5 V1 130.79(8) . . ? O8 V5 V1 125.18(6) . . ? O7 V5 V1 79.02(6) 2_657 . ? O10 V5 V1 78.34(6) . . ? O4 V5 V1 30.98(5) . . ? O1 V5 V1 43.73(5) . . ? V4 V5 V1 92.204(18) 2_657 . ? O14 V5 V3 133.89(9) . 2_657 ? O8 V5 V3 81.82(6) . 2_657 ? O7 V5 V3 32.18(5) 2_657 2_657 ? O10 V5 V3 123.08(6) . 2_657 ? O4 V5 V3 81.96(5) . 2_657 ? O1 V5 V3 45.48(4) . 2_657 ? V4 V5 V3 60.812(17) 2_657 2_657 ? V1 V5 V3 61.893(15) . 2_657 ? OW3 Ca OW8 108.34(12) . . ? OW3 Ca OW6 160.70(10) . . ? OW8 Ca OW6 86.42(11) . . ? OW3 Ca OW1 96.84(9) . . ? OW8 Ca OW1 132.79(9) . . ? OW6 Ca OW1 80.95(8) . . ? OW3 Ca OW5 88.22(9) . . ? OW8 Ca OW5 76.34(9) . . ? OW6 Ca OW5 83.18(9) . . ? OW1 Ca OW5 145.25(8) . . ? OW3 Ca OW7 72.37(9) . . ? OW8 Ca OW7 75.34(10) . . ? OW6 Ca OW7 124.72(9) . . ? OW1 Ca OW7 75.30(8) . . ? OW5 Ca OW7 138.13(9) . . ? OW3 Ca OW2 80.09(9) . . ? OW8 Ca OW2 147.28(9) . . ? OW6 Ca OW2 80.84(9) . . ? OW1 Ca OW2 74.75(7) . . ? OW5 Ca OW2 72.33(8) . . ? OW7 Ca OW2 136.04(10) . . ? V1 O1 V1 101.56(7) 2_657 . ? V1 O1 V3 93.27(6) 2_657 2_657 ? V1 O1 V3 93.95(7) . 2_657 ? V1 O1 V2 93.39(7) 2_657 . ? V1 O1 V2 92.42(7) . . ? V3 O1 V2 169.69(9) 2_657 . ? V1 O1 V5 170.95(9) 2_657 . ? V1 O1 V5 87.48(6) . . ? V3 O1 V5 86.24(6) 2_657 . ? V2 O1 V5 85.95(6) . . ? V1 O1 V4 87.89(6) 2_657 2_657 ? V1 O1 V4 170.41(9) . 2_657 ? V3 O1 V4 87.10(6) 2_657 2_657 ? V2 O1 V4 85.28(6) . 2_657 ? V5 O1 V4 83.07(6) . 2_657 ? V1 O2 V2 108.20(9) . . ? V1 O2 V3 106.63(8) . . ? V2 O2 V3 100.16(8) . . ? V1 O3 V2 108.39(8) . 2_657 ? V1 O3 V3 107.60(9) . 2_657 ? V2 O3 V3 100.66(8) 2_657 2_657 ? V1 O4 V5 110.40(9) . . ? V3 O5 V4 114.06(10) . . ? V1 O6 V4 110.13(9) . . ? V3 O7 V5 114.71(10) . 2_657 ? V4 O8 V5 113.76(10) 2_657 . ? V2 O9 V4 114.85(10) . 2_657 ? V2 O10 V5 115.34(9) . . ? Ca OW1 H1A 115(2) . . ? Ca OW1 H1B 118(2) . . ? H1A OW1 H1B 107(2) . . ? Ca OW2 H2A 123(2) . . ? Ca OW2 H2B 125(2) . . ? H2A OW2 H2B 109(2) . . ? Ca OW3 H3A 123(2) . . ? Ca OW3 H3B 121(2) . . ? H3A OW3 H3B 108(2) . . ? H4A OW4 H4B 103(2) . . ? Ca OW5 H5A 124(2) . . ? Ca OW5 H5B 125(2) . . ? H5A OW5 H5B 110(2) . . ? Ca OW6 H6A 122(2) . . ? Ca OW6 H6B 128(2) . . ? H6A OW6 H6B 105(2) . . ? Ca OW7 H7A 104(2) . . ? Ca OW7 H7B 130(3) . . ? H7A OW7 H7B 109(2) . . ? Ca OW8 H8A 123(3) . . ? Ca OW8 H8B 122(3) . . ? H8A OW8 H8B 112(3) . . ? H9A OW9 H9B 106(2) . . ? H9A OW9 H9C 106(2) . . ? H9B OW9 H9C 105(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.574 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.104