data_gt1028wb_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H24 Ca2 O18 P0' _chemical_formula_weight 416.37 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' 'Ca' 'Ca' 0.2262 0.3064 '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+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 8.8407(16) _cell_length_b 8.3333(15) _cell_length_c 11.072(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.683(3) _cell_angle_gamma 90.00 _cell_volume 763.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3798 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0111 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1108 _reflns_number_gt 1074 _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^)+(0.0198P)^2^+0.2335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1108 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0164 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 1.472 _refine_ls_shift/su_mean 0.021 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 Ca1 Ca 0.5000 0.64714(2) 0.2500 0.01516(8) Uani 1 2 d S . . C C 0.5000 0.30567(12) 0.2500 0.01695(19) Uani 1 2 d S . . O1 O 0.5000 0.15237(10) 0.2500 0.0293(2) Uani 1 2 d S . . O2 O 0.52639(7) 0.38534(7) 0.15943(6) 0.02078(13) Uani 1 1 d . . . OW3 O 0.61282(8) 0.72232(8) 0.09065(6) 0.02612(14) Uani 1 1 d . . . HW3A H 0.5770(19) 0.6887(18) 0.0144(15) 0.047(4) Uiso 1 1 d . . . HW3B H 0.6493(19) 0.813(2) 0.0917(15) 0.050(4) Uiso 1 1 d . . . OW4 O 0.78709(8) 0.55874(8) 0.38343(6) 0.02340(14) Uani 1 1 d . . . HW4A H 0.8078(17) 0.5863(16) 0.4574(15) 0.041(5) Uiso 1.00(4) 1 d . . . HW4B H 0.858(2) 0.6007(19) 0.3636(16) 0.052(4) Uiso 1 1 d . . . OW5 O 0.67063(8) 0.88549(7) 0.35805(6) 0.02107(13) Uani 1 1 d . . . HW5A H 0.7613(18) 0.8838(16) 0.3530(13) 0.037(3) Uiso 1 1 d . . . HW5B H 0.6323(17) 0.9714(18) 0.3356(13) 0.041(4) Uiso 1 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 Ca1 0.01830(12) 0.01243(10) 0.01569(11) 0.000 0.00717(7) 0.000 C 0.0123(4) 0.0148(4) 0.0222(5) 0.000 0.0041(4) 0.000 O1 0.0267(5) 0.0126(4) 0.0431(5) 0.000 0.0056(4) 0.000 O2 0.0245(3) 0.0206(3) 0.0200(3) -0.0026(2) 0.0112(2) -0.0020(2) OW3 0.0354(4) 0.0246(3) 0.0215(3) -0.0009(2) 0.0139(3) -0.0052(3) OW4 0.0256(3) 0.0231(3) 0.0212(3) -0.0016(2) 0.0079(2) -0.0011(2) OW5 0.0212(3) 0.0177(3) 0.0254(3) 0.0015(2) 0.0095(2) 0.0002(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 Ca1 OW3 2.3965(7) . ? Ca1 OW3 2.3965(7) 2_655 ? Ca1 O2 2.4464(7) . ? Ca1 O2 2.4464(7) 2_655 ? Ca1 OW5 2.5253(7) . ? Ca1 OW5 2.5253(7) 2_655 ? Ca1 OW4 2.5531(7) . ? Ca1 OW4 2.5531(7) 2_655 ? Ca1 C 2.8456(12) . ? C O1 1.2775(13) . ? C O2 1.2908(8) . ? C O2 1.2908(8) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OW3 Ca1 OW3 149.69(3) . 2_655 ? OW3 Ca1 O2 78.85(2) . . ? OW3 Ca1 O2 131.27(2) 2_655 . ? OW3 Ca1 O2 131.28(2) . 2_655 ? OW3 Ca1 O2 78.85(2) 2_655 2_655 ? O2 Ca1 O2 53.81(3) . 2_655 ? OW3 Ca1 OW5 78.98(2) . . ? OW3 Ca1 OW5 77.28(2) 2_655 . ? O2 Ca1 OW5 140.19(2) . . ? O2 Ca1 OW5 129.40(2) 2_655 . ? OW3 Ca1 OW5 77.28(2) . 2_655 ? OW3 Ca1 OW5 78.98(2) 2_655 2_655 ? O2 Ca1 OW5 129.40(2) . 2_655 ? O2 Ca1 OW5 140.19(2) 2_655 2_655 ? OW5 Ca1 OW5 76.27(3) . 2_655 ? OW3 Ca1 OW4 85.08(3) . . ? OW3 Ca1 OW4 103.69(3) 2_655 . ? O2 Ca1 OW4 76.15(2) . . ? O2 Ca1 OW4 74.02(2) 2_655 . ? OW5 Ca1 OW4 69.35(2) . . ? OW5 Ca1 OW4 143.75(2) 2_655 . ? OW3 Ca1 OW4 103.69(3) . 2_655 ? OW3 Ca1 OW4 85.08(3) 2_655 2_655 ? O2 Ca1 OW4 74.02(2) . 2_655 ? O2 Ca1 OW4 76.15(2) 2_655 2_655 ? OW5 Ca1 OW4 143.75(2) . 2_655 ? OW5 Ca1 OW4 69.36(2) 2_655 2_655 ? OW4 Ca1 OW4 146.46(3) . 2_655 ? OW3 Ca1 C 105.155(17) . . ? OW3 Ca1 C 105.155(17) 2_655 . ? O2 Ca1 C 26.903(14) . . ? O2 Ca1 C 26.904(14) 2_655 . ? OW5 Ca1 C 141.864(16) . . ? OW5 Ca1 C 141.865(16) 2_655 . ? OW4 Ca1 C 73.230(15) . . ? OW4 Ca1 C 73.230(15) 2_655 . ? O1 C O2 120.95(5) . . ? O1 C O2 120.95(5) . 2_655 ? O2 C O2 118.09(9) . 2_655 ? O1 C Ca1 180.0 . . ? O2 C Ca1 59.05(5) . . ? O2 C Ca1 59.05(5) 2_655 . ? C O2 Ca1 94.05(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.265 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.042