data_c69929_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca10 Cl0.25 F1.89 O24 P6' _chemical_formula_weight 1015.39 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 9.4446(3) _cell_length_b 9.4446(3) _cell_length_c 6.8728(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 530.92(3) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 503 _exptl_absorpt_coefficient_mu 3.090 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11581 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0052 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 33.06 _reflns_number_total 711 _reflns_number_gt 708 _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^)+(0.0224P)^2^+0.2746P] 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 0.0092(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 711 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0146 _refine_ls_R_factor_gt 0.0145 _refine_ls_wR_factor_ref 0.0427 _refine_ls_wR_factor_gt 0.0427 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _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 Ca1 Ca 0.6667 0.3333 0.00132(5) 0.01174(9) Uani 1 3 d S . . Ca2 Ca -0.00641(9) 0.2408(4) 0.2500 0.0104(2) Uani 0.885(19) 2 d SP . . Ca2' Ca -0.0085(5) 0.2687(11) 0.2500 0.0104(2) Uani 0.176(19) 2 d SP . . P P 0.36951(4) 0.39953(4) 0.2500 0.00760(9) Uani 1 2 d S . . O1 O 0.48520(13) 0.32929(13) 0.2500 0.01286(18) Uani 1 2 d S . . O2 O 0.46602(13) 0.58799(13) 0.2500 0.0161(2) Uani 1 2 d S . . O3 O 0.25857(9) 0.34381(11) 0.07013(11) 0.01924(17) Uani 1 1 d . . . F F 0.0000 0.0000 0.2500 0.0123(10) Uiso 0.578(17) 6 d SP . . FB F 0.0000 0.0000 0.1783(18) 0.0072(19) Uiso 0.183(10) 3 d SP . . ClB Cl 0.0000 0.0000 0.1012(18) 0.008(3) Uiso 0.050(4) 3 d SP . . Cl Cl 0.0000 0.0000 0.0000 0.06(2) Uiso 0.024(7) 6 d SP . . 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 0.01401(11) 0.01401(11) 0.00722(14) 0.000 0.000 0.00700(5) Ca2 0.01067(12) 0.0132(5) 0.00859(12) 0.000 0.000 0.00677(16) Ca2' 0.01067(12) 0.0132(5) 0.00859(12) 0.000 0.000 0.00677(16) P 0.00812(14) 0.00925(14) 0.00662(14) 0.000 0.000 0.00524(11) O1 0.0135(4) 0.0178(4) 0.0127(4) 0.000 0.000 0.0118(4) O2 0.0155(4) 0.0097(4) 0.0226(5) 0.000 0.000 0.0059(3) O3 0.0170(3) 0.0347(4) 0.0117(3) -0.0098(3) -0.0063(3) 0.0172(3) _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 O1 2.4071(7) 3_665 ? Ca1 O1 2.4071(7) . ? Ca1 O1 2.4071(7) 2_655 ? Ca1 O2 2.4571(8) 8 ? Ca1 O2 2.4571(8) 9_655 ? Ca1 O2 2.4571(8) 7_665 ? Ca1 O3 2.8079(9) 9_655 ? Ca1 O3 2.8079(9) 8 ? Ca1 O3 2.8080(9) 7_665 ? Ca1 P 3.2137(3) 8 ? Ca1 P 3.2137(3) 9_655 ? Ca1 P 3.2137(3) 7_665 ? Ca2 F 2.306(4) . ? Ca2 O3 2.3554(13) 9 ? Ca2 O3 2.3554(13) 6 ? Ca2 FB 2.358(5) 10_556 ? Ca2 FB 2.358(5) . ? Ca2 O2 2.404(4) 3_565 ? Ca2 O3 2.5107(12) . ? Ca2 O3 2.5107(12) 10_556 ? Ca2 ClB 2.522(6) . ? Ca2 ClB 2.522(6) 10_556 ? Ca2 O1 2.7379(18) 2 ? Ca2 Cl 2.875(3) . ? Ca2' O2 2.170(9) 3_565 ? Ca2' O3 2.3033(19) 9 ? Ca2' O3 2.3033(19) 6 ? Ca2' O3 2.570(5) . ? Ca2' O3 2.570(5) 10_556 ? Ca2' F 2.579(10) . ? Ca2' FB 2.626(11) 10_556 ? Ca2' FB 2.626(11) . ? Ca2' O1 2.662(5) 2 ? Ca2' ClB 2.775(11) . ? Ca2' ClB 2.775(11) 10_556 ? Ca2' Cl 3.099(9) . ? P O3 1.5335(7) 10_556 ? P O3 1.5335(7) . ? P O1 1.5359(10) . ? P O2 1.5416(11) . ? P Ca1 3.2137(3) 4_665 ? P Ca1 3.2137(3) 7_665 ? P Ca2' 3.250(10) 2_665 ? P Ca2 3.2911(10) 3 ? P Ca2' 3.343(5) 3 ? P Ca2 3.521(4) 2_665 ? O1 Ca1 2.4071(7) 10_556 ? O1 Ca2' 2.662(5) 3 ? O1 Ca2 2.7379(18) 3 ? O2 Ca2' 2.170(9) 2_665 ? O2 Ca2 2.404(4) 2_665 ? O2 Ca1 2.4571(8) 7_665 ? O2 Ca1 2.4571(8) 4_665 ? O3 Ca2' 2.3033(19) 8 ? O3 Ca2 2.3554(13) 8 ? O3 Ca1 2.8079(9) 7_665 ? F FB 0.493(13) 10_556 ? F ClB 1.023(12) . ? F ClB 1.023(12) 10_556 ? F Cl 1.7182 4 ? F Cl 1.7182 . ? F Ca2 2.306(4) 3 ? F Ca2 2.306(4) 2 ? F Ca2' 2.579(10) 2 ? F Ca2' 2.579(10) 3 ? FB ClB 0.530(9) . ? FB FB 0.99(3) 10_556 ? FB Cl 1.225(13) . ? FB ClB 1.52(2) 10_556 ? FB ClB 1.92(2) 7 ? FB Ca2 2.358(5) 3 ? FB Ca2 2.358(5) 2 ? FB Ca2' 2.626(11) 2 ? FB Ca2' 2.626(11) 3 ? ClB Cl 0.696(12) . ? ClB ClB 1.39(2) 7 ? ClB FB 1.52(2) 10_556 ? ClB FB 1.92(2) 7 ? ClB ClB 2.05(2) 10_556 ? ClB Ca2 2.522(6) 3 ? ClB Ca2 2.522(6) 2 ? ClB Ca2' 2.775(11) 3 ? Cl ClB 0.696(12) 7 ? Cl FB 1.225(13) 7 ? Cl F 1.7182 7 ? Cl Ca2 2.875(3) 9 ? Cl Ca2 2.875(3) 3 ? Cl Ca2 2.875(3) 8 ? Cl Ca2 2.875(3) 2 ? Cl Ca2 2.875(3) 7 ? 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 O1 Ca1 O1 75.16(3) 3_665 . ? O1 Ca1 O1 75.16(3) 3_665 2_655 ? O1 Ca1 O1 75.16(3) . 2_655 ? O1 Ca1 O2 153.85(3) 3_665 8 ? O1 Ca1 O2 124.23(3) . 8 ? O1 Ca1 O2 92.13(3) 2_655 8 ? O1 Ca1 O2 92.13(3) 3_665 9_655 ? O1 Ca1 O2 153.85(3) . 9_655 ? O1 Ca1 O2 124.23(3) 2_655 9_655 ? O2 Ca1 O2 76.04(3) 8 9_655 ? O1 Ca1 O2 124.23(3) 3_665 7_665 ? O1 Ca1 O2 92.13(3) . 7_665 ? O1 Ca1 O2 153.85(3) 2_655 7_665 ? O2 Ca1 O2 76.04(3) 8 7_665 ? O2 Ca1 O2 76.04(3) 9_655 7_665 ? O1 Ca1 O3 86.09(3) 3_665 9_655 ? O1 Ca1 O3 142.87(3) . 9_655 ? O1 Ca1 O3 69.11(3) 2_655 9_655 ? O2 Ca1 O3 67.92(3) 8 9_655 ? O2 Ca1 O3 55.81(3) 9_655 9_655 ? O2 Ca1 O3 124.68(3) 7_665 9_655 ? O1 Ca1 O3 142.86(3) 3_665 8 ? O1 Ca1 O3 69.11(3) . 8 ? O1 Ca1 O3 86.09(3) 2_655 8 ? O2 Ca1 O3 55.81(3) 8 8 ? O2 Ca1 O3 124.68(3) 9_655 8 ? O2 Ca1 O3 67.92(3) 7_665 8 ? O3 Ca1 O3 117.009(10) 9_655 8 ? O1 Ca1 O3 69.11(3) 3_665 7_665 ? O1 Ca1 O3 86.09(3) . 7_665 ? O1 Ca1 O3 142.87(3) 2_655 7_665 ? O2 Ca1 O3 124.68(3) 8 7_665 ? O2 Ca1 O3 67.92(3) 9_655 7_665 ? O2 Ca1 O3 55.81(3) 7_665 7_665 ? O3 Ca1 O3 117.009(10) 9_655 7_665 ? O3 Ca1 O3 117.007(10) 8 7_665 ? O1 Ca1 P 166.67(2) 3_665 8 ? O1 Ca1 P 97.59(2) . 8 ? O1 Ca1 P 92.28(2) 2_655 8 ? O2 Ca1 P 27.65(2) 8 8 ? O2 Ca1 P 98.76(2) 9_655 8 ? O2 Ca1 P 66.42(2) 7_665 8 ? O3 Ca1 P 93.655(17) 9_655 8 ? O3 Ca1 P 28.500(15) 8 8 ? O3 Ca1 P 122.213(17) 7_665 8 ? O1 Ca1 P 92.28(2) 3_665 9_655 ? O1 Ca1 P 166.67(2) . 9_655 ? O1 Ca1 P 97.59(2) 2_655 9_655 ? O2 Ca1 P 66.42(2) 8 9_655 ? O2 Ca1 P 27.66(2) 9_655 9_655 ? O2 Ca1 P 98.76(2) 7_665 9_655 ? O3 Ca1 P 28.499(15) 9_655 9_655 ? O3 Ca1 P 122.214(17) 8 9_655 ? O3 Ca1 P 93.656(17) 7_665 9_655 ? P Ca1 P 93.824(8) 8 9_655 ? O1 Ca1 P 97.59(2) 3_665 7_665 ? O1 Ca1 P 92.28(2) . 7_665 ? O1 Ca1 P 166.67(2) 2_655 7_665 ? O2 Ca1 P 98.76(2) 8 7_665 ? O2 Ca1 P 66.42(2) 9_655 7_665 ? O2 Ca1 P 27.65(2) 7_665 7_665 ? O3 Ca1 P 122.213(17) 9_655 7_665 ? O3 Ca1 P 93.654(17) 8 7_665 ? O3 Ca1 P 28.499(15) 7_665 7_665 ? P Ca1 P 93.824(8) 8 7_665 ? P Ca1 P 93.824(8) 9_655 7_665 ? F Ca2 O3 103.61(9) . 9 ? F Ca2 O3 103.61(9) . 6 ? O3 Ca2 O3 138.17(13) 9 6 ? F Ca2 FB 12.1(3) . 10_556 ? O3 Ca2 FB 115.2(3) 9 10_556 ? O3 Ca2 FB 92.0(3) 6 10_556 ? F Ca2 FB 12.1(3) . . ? O3 Ca2 FB 92.0(3) 9 . ? O3 Ca2 FB 115.2(3) 6 . ? FB Ca2 FB 24.1(6) 10_556 . ? F Ca2 O2 152.79(6) . 3_565 ? O3 Ca2 O2 85.04(10) 9 3_565 ? O3 Ca2 O2 85.04(10) 6 3_565 ? FB Ca2 O2 150.42(13) 10_556 3_565 ? FB Ca2 O2 150.42(13) . 3_565 ? F Ca2 O3 82.49(10) . . ? O3 Ca2 O3 78.569(19) 9 . ? O3 Ca2 O3 136.20(4) 6 . ? FB Ca2 O3 88.57(18) 10_556 . ? FB Ca2 O3 76.66(17) . . ? O2 Ca2 O3 73.91(6) 3_565 . ? F Ca2 O3 82.49(10) . 10_556 ? O3 Ca2 O3 136.19(4) 9 10_556 ? O3 Ca2 O3 78.570(19) 6 10_556 ? FB Ca2 O3 76.66(17) 10_556 10_556 ? FB Ca2 O3 88.57(18) . 10_556 ? O2 Ca2 O3 73.91(6) 3_565 10_556 ? O3 Ca2 O3 58.99(4) . 10_556 ? F Ca2 ClB 23.9(3) . . ? O3 Ca2 ClB 80.6(3) 9 . ? O3 Ca2 ClB 126.4(3) 6 . ? FB Ca2 ClB 36.0(5) 10_556 . ? FB Ca2 ClB 11.9(2) . . ? O2 Ca2 ClB 144.39(16) 3_565 . ? O3 Ca2 ClB 71.39(13) . . ? O3 Ca2 ClB 94.60(17) 10_556 . ? F Ca2 ClB 23.9(3) . 10_556 ? O3 Ca2 ClB 126.4(3) 9 10_556 ? O3 Ca2 ClB 80.6(3) 6 10_556 ? FB Ca2 ClB 11.9(2) 10_556 10_556 ? FB Ca2 ClB 36.0(5) . 10_556 ? O2 Ca2 ClB 144.39(16) 3_565 10_556 ? O3 Ca2 ClB 94.60(17) . 10_556 ? O3 Ca2 ClB 71.39(13) 10_556 10_556 ? ClB Ca2 ClB 47.8(5) . 10_556 ? F Ca2 O1 106.61(8) . 2 ? O3 Ca2 O1 71.06(5) 9 2 ? O3 Ca2 O1 71.06(5) 6 2 ? FB Ca2 O1 106.23(8) 10_556 2 ? FB Ca2 O1 106.23(8) . 2 ? O2 Ca2 O1 100.60(13) 3_565 2 ? O3 Ca2 O1 149.54(5) . 2 ? O3 Ca2 O1 149.54(5) 10_556 2 ? ClB Ca2 O1 105.14(8) . 2 ? ClB Ca2 O1 105.14(8) 10_556 2 ? F Ca2 Cl 36.69(5) . . ? O3 Ca2 Cl 68.31(5) 9 . ? O3 Ca2 Cl 138.32(13) 6 . ? FB Ca2 Cl 48.8(3) 10_556 . ? FB Ca2 Cl 24.6(3) . . ? O2 Ca2 Cl 135.49(2) 3_565 . ? O3 Ca2 Cl 66.48(6) . . ? O3 Ca2 Cl 100.92(10) 10_556 . ? ClB Ca2 Cl 12.8(3) . . ? ClB Ca2 Cl 60.6(3) 10_556 . ? O1 Ca2 Cl 103.25(6) 2 . ? O2 Ca2' O3 91.9(3) 3_565 9 ? O2 Ca2' O3 91.9(3) 3_565 6 ? O3 Ca2' O3 145.6(3) 9 6 ? O2 Ca2' O3 76.64(15) 3_565 . ? O3 Ca2' O3 78.28(7) 9 . ? O3 Ca2' O3 135.71(17) 6 . ? O2 Ca2' O3 76.64(15) 3_565 10_556 ? O3 Ca2' O3 135.71(17) 9 10_556 ? O3 Ca2' O3 78.29(7) 6 10_556 ? O3 Ca2' O3 57.50(11) . 10_556 ? O2 Ca2' F 149.0(2) 3_565 . ? O3 Ca2' F 97.1(3) 9 . ? O3 Ca2' F 97.1(3) 6 . ? O3 Ca2' F 76.2(2) . . ? O3 Ca2' F 76.2(2) 10_556 . ? O2 Ca2' FB 147.3(2) 3_565 10_556 ? O3 Ca2' FB 107.5(4) 9 10_556 ? O3 Ca2' FB 86.6(3) 6 10_556 ? O3 Ca2' FB 81.8(3) . 10_556 ? O3 Ca2' FB 71.1(3) 10_556 10_556 ? F Ca2' FB 10.8(3) . 10_556 ? O2 Ca2' FB 147.3(2) 3_565 . ? O3 Ca2' FB 86.6(3) 9 . ? O3 Ca2' FB 107.5(4) 6 . ? O3 Ca2' FB 71.1(3) . . ? O3 Ca2' FB 81.8(3) 10_556 . ? F Ca2' FB 10.8(3) . . ? FB Ca2' FB 21.6(5) 10_556 . ? O2 Ca2' O1 109.8(4) 3_565 2 ? O3 Ca2' O1 73.26(12) 9 2 ? O3 Ca2' O1 73.26(12) 6 2 ? O3 Ca2' O1 150.93(6) . 2 ? O3 Ca2' O1 150.93(6) 10_556 2 ? F Ca2' O1 101.3(2) . 2 ? FB Ca2' O1 101.1(2) 10_556 2 ? FB Ca2' O1 101.1(2) . 2 ? O2 Ca2' ClB 142.8(2) 3_565 . ? O3 Ca2' ClB 76.2(3) 9 . ? O3 Ca2' ClB 117.8(4) 6 . ? O3 Ca2' ClB 66.5(2) . . ? O3 Ca2' ClB 87.5(3) 10_556 . ? F Ca2' ClB 21.6(2) . . ? FB Ca2' ClB 32.4(5) 10_556 . ? FB Ca2' ClB 10.81(19) . . ? O1 Ca2' ClB 100.5(2) 2 . ? O2 Ca2' ClB 142.8(2) 3_565 10_556 ? O3 Ca2' ClB 117.8(4) 9 10_556 ? O3 Ca2' ClB 76.2(3) 6 10_556 ? O3 Ca2' ClB 87.5(3) . 10_556 ? O3 Ca2' ClB 66.5(2) 10_556 10_556 ? F Ca2' ClB 21.6(2) . 10_556 ? FB Ca2' ClB 10.81(19) 10_556 10_556 ? FB Ca2' ClB 32.4(5) . 10_556 ? O1 Ca2' ClB 100.5(2) 2 10_556 ? ClB Ca2' ClB 43.3(5) . 10_556 ? O2 Ca2' Cl 135.50(12) 3_565 . ? O3 Ca2' Cl 64.71(15) 9 . ? O3 Ca2' Cl 129.2(4) 6 . ? O3 Ca2' Cl 62.32(16) . . ? O3 Ca2' Cl 93.9(3) 10_556 . ? F Ca2' Cl 33.67(11) . . ? FB Ca2' Cl 44.5(3) 10_556 . ? FB Ca2' Cl 22.9(3) . . ? O1 Ca2' Cl 99.36(19) 2 . ? ClB Ca2' Cl 12.0(2) . . ? ClB Ca2' Cl 55.3(3) 10_556 . ? O3 P O3 107.44(6) 10_556 . ? O3 P O1 111.31(4) 10_556 . ? O3 P O1 111.31(4) . . ? O3 P O2 107.71(4) 10_556 . ? O3 P O2 107.71(4) . . ? O1 P O2 111.17(6) . . ? O3 P Ca2 53.90(3) 10_556 . ? O3 P Ca2 53.90(3) . . ? O1 P Ca2 133.17(8) . . ? O2 P Ca2 115.66(8) . . ? O3 P Ca2' 54.39(4) 10_556 . ? O3 P Ca2' 54.39(4) . . ? O1 P Ca2' 138.12(19) . . ? O2 P Ca2' 110.71(19) . . ? Ca2 P Ca2' 4.95(12) . . ? O3 P Ca1 60.89(4) 10_556 4_665 ? O3 P Ca1 112.34(3) . 4_665 ? O1 P Ca1 135.80(3) . 4_665 ? O2 P Ca1 47.71(3) . 4_665 ? Ca2 P Ca1 80.40(6) . 4_665 ? Ca2' P Ca1 76.26(16) . 4_665 ? O3 P Ca1 112.34(3) 10_556 7_665 ? O3 P Ca1 60.89(4) . 7_665 ? O1 P Ca1 135.80(3) . 7_665 ? O2 P Ca1 47.71(3) . 7_665 ? Ca2 P Ca1 80.40(6) . 7_665 ? Ca2' P Ca1 76.26(16) . 7_665 ? Ca1 P Ca1 65.025(11) 4_665 7_665 ? O3 P Ca2' 122.64(4) 10_556 2_665 ? O3 P Ca2' 122.64(4) . 2_665 ? O1 P Ca2' 76.40(9) . 2_665 ? O2 P Ca2' 34.77(9) . 2_665 ? Ca2 P Ca2' 150.43(9) . 2_665 ? Ca2' P Ca2' 145.48(19) . 2_665 ? Ca1 P Ca2' 74.76(7) 4_665 2_665 ? Ca1 P Ca2' 74.76(7) 7_665 2_665 ? O3 P Ca2 79.56(5) 10_556 3 ? O3 P Ca2 79.56(5) . 3 ? O1 P Ca2 55.72(8) . 3 ? O2 P Ca2 166.89(8) . 3 ? Ca2 P Ca2 77.45(14) . 3 ? Ca2' P Ca2 82.4(3) . 3 ? Ca1 P Ca2 140.41(4) 4_665 3 ? Ca1 P Ca2 140.41(4) 7_665 3 ? Ca2' P Ca2 132.12(12) 2_665 3 ? O3 P Ca2' 82.24(11) 10_556 3 ? O3 P Ca2' 82.24(11) . 3 ? O1 P Ca2' 51.07(18) . 3 ? O2 P Ca2' 162.24(18) . 3 ? Ca2 P Ca2' 82.1(2) . 3 ? Ca2' P Ca2' 87.0(4) . 3 ? Ca1 P Ca2' 142.73(8) 4_665 3 ? Ca1 P Ca2' 142.73(8) 7_665 3 ? Ca2' P Ca2' 127.5(2) 2_665 3 ? Ca2 P Ca2' 4.65(11) 3 3 ? O3 P Ca2 122.43(4) 10_556 2_665 ? O3 P Ca2 122.43(4) . 2_665 ? O1 P Ca2 77.11(4) . 2_665 ? O2 P Ca2 34.06(4) . 2_665 ? Ca2 P Ca2 149.71(6) . 2_665 ? Ca2' P Ca2 144.77(18) . 2_665 ? Ca1 P Ca2 74.167(13) 4_665 2_665 ? Ca1 P Ca2 74.167(13) 7_665 2_665 ? Ca2' P Ca2 0.71(9) 2_665 2_665 ? Ca2 P Ca2 132.83(8) 3 2_665 ? Ca2' P Ca2 128.19(18) 3 2_665 ? P O1 Ca1 130.38(3) . 10_556 ? P O1 Ca1 130.38(3) . . ? Ca1 O1 Ca1 90.47(3) 10_556 . ? P O1 Ca2' 102.3(2) . 3 ? Ca1 O1 Ca2' 97.61(16) 10_556 3 ? Ca1 O1 Ca2' 97.60(16) . 3 ? P O1 Ca2 96.66(9) . 3 ? Ca1 O1 Ca2 101.48(6) 10_556 3 ? Ca1 O1 Ca2 101.48(6) . 3 ? Ca2' O1 Ca2 5.59(15) 3 3 ? P O2 Ca2' 121.33(19) . 2_665 ? P O2 Ca2 124.89(8) . 2_665 ? Ca2' O2 Ca2 3.57(15) 2_665 2_665 ? P O2 Ca1 104.64(4) . 7_665 ? Ca2' O2 Ca1 115.88(11) 2_665 7_665 ? Ca2 O2 Ca1 113.62(4) 2_665 7_665 ? P O2 Ca1 104.64(4) . 4_665 ? Ca2' O2 Ca1 115.88(11) 2_665 4_665 ? Ca2 O2 Ca1 113.62(4) 2_665 4_665 ? Ca1 O2 Ca1 89.34(4) 7_665 4_665 ? P O3 Ca2' 138.51(18) . 8 ? P O3 Ca2 142.18(7) . 8 ? Ca2' O3 Ca2 6.62(18) 8 8 ? P O3 Ca2 96.53(4) . . ? Ca2' O3 Ca2 122.3(3) 8 . ? Ca2 O3 Ca2 116.48(12) 8 . ? P O3 Ca2' 96.60(6) . . ? Ca2' O3 Ca2' 123.6(3) 8 . ? Ca2 O3 Ca2' 118.20(14) 8 . ? Ca2 O3 Ca2' 6.03(15) . . ? P O3 Ca1 90.61(4) . 7_665 ? Ca2' O3 Ca1 96.1(2) 8 7_665 ? Ca2 O3 Ca1 100.82(7) 8 7_665 ? Ca2 O3 Ca1 99.64(9) . 7_665 ? Ca2' O3 Ca1 93.6(2) . 7_665 ? FB F ClB 180.000(2) 10_556 . ? FB F ClB 0.000(4) 10_556 10_556 ? ClB F ClB 180.000(2) . 10_556 ? FB F Cl 0.000(3) 10_556 4 ? ClB F Cl 180.0 . 4 ? ClB F Cl 0.000(2) 10_556 4 ? FB F Cl 180.000(3) 10_556 . ? ClB F Cl 0.0 . . ? ClB F Cl 180.000(2) 10_556 . ? Cl F Cl 180.0 4 . ? FB F Ca2 90.000(1) 10_556 3 ? ClB F Ca2 90.0 . 3 ? ClB F Ca2 90.000(1) 10_556 3 ? Cl F Ca2 90.0 4 3 ? Cl F Ca2 90.0 . 3 ? FB F Ca2 90.000(3) 10_556 2 ? ClB F Ca2 90.000(1) . 2 ? ClB F Ca2 90.000(1) 10_556 2 ? Cl F Ca2 90.0 4 2 ? Cl F Ca2 90.0 . 2 ? Ca2 F Ca2 120.0 3 2 ? FB F Ca2 90.000(1) 10_556 . ? ClB F Ca2 90.0 . . ? ClB F Ca2 90.000(1) 10_556 . ? Cl F Ca2 90.0 4 . ? Cl F Ca2 90.0 . . ? Ca2 F Ca2 120.0 3 . ? Ca2 F Ca2 120.0 2 . ? FB F Ca2' 90.000(1) 10_556 . ? ClB F Ca2' 90.000(1) . . ? ClB F Ca2' 90.000(1) 10_556 . ? Cl F Ca2' 90.0 4 . ? Cl F Ca2' 90.0 . . ? Ca2 F Ca2' 120.25(11) 3 . ? Ca2 F Ca2' 119.75(11) 2 . ? Ca2 F Ca2' 0.25(11) . . ? FB F Ca2' 90.000(4) 10_556 2 ? ClB F Ca2' 90.000(2) . 2 ? ClB F Ca2' 90.000(2) 10_556 2 ? Cl F Ca2' 90.000(1) 4 2 ? Cl F Ca2' 90.000(1) . 2 ? Ca2 F Ca2' 119.75(11) 3 2 ? Ca2 F Ca2' 0.25(11) 2 2 ? Ca2 F Ca2' 120.25(11) . 2 ? Ca2' F Ca2' 120.0 . 2 ? FB F Ca2' 90.000(2) 10_556 3 ? ClB F Ca2' 90.000(1) . 3 ? ClB F Ca2' 90.000(1) 10_556 3 ? Cl F Ca2' 90.0 4 3 ? Cl F Ca2' 90.0 . 3 ? Ca2 F Ca2' 0.25(11) 3 3 ? Ca2 F Ca2' 120.25(11) 2 3 ? Ca2 F Ca2' 119.75(11) . 3 ? Ca2' F Ca2' 120.0 . 3 ? Ca2' F Ca2' 120.0 2 3 ? ClB FB FB 180.000(2) . 10_556 ? ClB FB Cl 0.000(1) . . ? FB FB Cl 180.000(2) 10_556 . ? ClB FB ClB 180.000(1) . 10_556 ? FB FB ClB 0.000(2) 10_556 10_556 ? Cl FB ClB 180.000(1) . 10_556 ? ClB FB ClB 0.000(2) . 7 ? FB FB ClB 180.000(3) 10_556 7 ? Cl FB ClB 0.0 . 7 ? ClB FB ClB 180.000(2) 10_556 7 ? ClB FB Ca2 102.1(3) . 3 ? FB FB Ca2 77.9(3) 10_556 3 ? Cl FB Ca2 102.1(3) . 3 ? ClB FB Ca2 77.9(3) 10_556 3 ? ClB FB Ca2 102.1(3) 7 3 ? ClB FB Ca2 102.1(3) . . ? FB FB Ca2 77.9(3) 10_556 . ? Cl FB Ca2 102.1(3) . . ? ClB FB Ca2 77.9(3) 10_556 . ? ClB FB Ca2 102.1(3) 7 . ? Ca2 FB Ca2 115.8(2) 3 . ? ClB FB Ca2 102.1(3) . 2 ? FB FB Ca2 77.9(3) 10_556 2 ? Cl FB Ca2 102.1(3) . 2 ? ClB FB Ca2 77.9(3) 10_556 2 ? ClB FB Ca2 102.1(3) 7 2 ? Ca2 FB Ca2 115.8(2) 3 2 ? Ca2 FB Ca2 115.8(2) . 2 ? ClB FB Ca2' 100.8(3) . . ? FB FB Ca2' 79.2(3) 10_556 . ? Cl FB Ca2' 100.8(3) . . ? ClB FB Ca2' 79.2(3) 10_556 . ? ClB FB Ca2' 100.8(3) 7 . ? Ca2 FB Ca2' 116.4(2) 3 . ? Ca2 FB Ca2' 1.27(4) . . ? Ca2 FB Ca2' 115.9(2) 2 . ? ClB FB Ca2' 100.8(3) . 2 ? FB FB Ca2' 79.2(3) 10_556 2 ? Cl FB Ca2' 100.8(3) . 2 ? ClB FB Ca2' 79.2(3) 10_556 2 ? ClB FB Ca2' 100.8(3) 7 2 ? Ca2 FB Ca2' 115.9(2) 3 2 ? Ca2 FB Ca2' 116.4(2) . 2 ? Ca2 FB Ca2' 1.27(4) 2 2 ? Ca2' FB Ca2' 116.56(17) . 2 ? ClB FB Ca2' 100.8(3) . 3 ? FB FB Ca2' 79.2(3) 10_556 3 ? Cl FB Ca2' 100.8(3) . 3 ? ClB FB Ca2' 79.2(3) 10_556 3 ? ClB FB Ca2' 100.8(3) 7 3 ? Ca2 FB Ca2' 1.27(4) 3 3 ? Ca2 FB Ca2' 115.9(2) . 3 ? Ca2 FB Ca2' 116.4(2) 2 3 ? Ca2' FB Ca2' 116.56(17) . 3 ? Ca2' FB Ca2' 116.56(17) 2 3 ? FB ClB Cl 180.000(2) . . ? FB ClB F 0.000(2) . . ? Cl ClB F 180.0 . . ? FB ClB ClB 180.000(1) . 7 ? Cl ClB ClB 0.0 . 7 ? F ClB ClB 180.000(1) . 7 ? FB ClB FB 0.000(2) . 10_556 ? Cl ClB FB 180.000(1) . 10_556 ? F ClB FB 0.0 . 10_556 ? ClB ClB FB 180.000(1) 7 10_556 ? FB ClB FB 180.000(1) . 7 ? Cl ClB FB 0.0 . 7 ? F ClB FB 180.000(1) . 7 ? ClB ClB FB 0.0 7 7 ? FB ClB FB 180.000(2) 10_556 7 ? FB ClB ClB 0.000(2) . 10_556 ? Cl ClB ClB 180.000(1) . 10_556 ? F ClB ClB 0.0 . 10_556 ? ClB ClB ClB 180.000(1) 7 10_556 ? FB ClB ClB 0.000(1) 10_556 10_556 ? FB ClB ClB 180.000(1) 7 10_556 ? FB ClB Ca2 66.1(3) . 3 ? Cl ClB Ca2 113.9(3) . 3 ? F ClB Ca2 66.1(3) . 3 ? ClB ClB Ca2 113.9(3) 7 3 ? FB ClB Ca2 66.1(3) 10_556 3 ? FB ClB Ca2 113.9(3) 7 3 ? ClB ClB Ca2 66.1(3) 10_556 3 ? FB ClB Ca2 66.1(3) . . ? Cl ClB Ca2 113.9(3) . . ? F ClB Ca2 66.1(3) . . ? ClB ClB Ca2 113.9(3) 7 . ? FB ClB Ca2 66.1(3) 10_556 . ? FB ClB Ca2 113.9(3) 7 . ? ClB ClB Ca2 66.1(3) 10_556 . ? Ca2 ClB Ca2 104.7(3) 3 . ? FB ClB Ca2 66.1(3) . 2 ? Cl ClB Ca2 113.9(3) . 2 ? F ClB Ca2 66.1(3) . 2 ? ClB ClB Ca2 113.9(3) 7 2 ? FB ClB Ca2 66.1(3) 10_556 2 ? FB ClB Ca2 113.9(3) 7 2 ? ClB ClB Ca2 66.1(3) 10_556 2 ? Ca2 ClB Ca2 104.7(3) 3 2 ? Ca2 ClB Ca2 104.7(3) . 2 ? FB ClB Ca2' 68.4(2) . . ? Cl ClB Ca2' 111.6(2) . . ? F ClB Ca2' 68.4(2) . . ? ClB ClB Ca2' 111.6(2) 7 . ? FB ClB Ca2' 68.4(2) 10_556 . ? FB ClB Ca2' 111.6(2) 7 . ? ClB ClB Ca2' 68.4(2) 10_556 . ? Ca2 ClB Ca2' 106.2(3) 3 . ? Ca2 ClB Ca2' 2.30(5) . . ? Ca2 ClB Ca2' 105.8(3) 2 . ? FB ClB Ca2' 68.4(2) . 3 ? Cl ClB Ca2' 111.6(2) . 3 ? F ClB Ca2' 68.4(2) . 3 ? ClB ClB Ca2' 111.6(2) 7 3 ? FB ClB Ca2' 68.4(2) 10_556 3 ? FB ClB Ca2' 111.6(2) 7 3 ? ClB ClB Ca2' 68.4(2) 10_556 3 ? Ca2 ClB Ca2' 2.30(5) 3 3 ? Ca2 ClB Ca2' 105.8(3) . 3 ? Ca2 ClB Ca2' 106.2(3) 2 3 ? Ca2' ClB Ca2' 107.2(3) . 3 ? ClB Cl ClB 180.000(1) 7 . ? ClB Cl FB 180.000(1) 7 . ? ClB Cl FB 0.000(1) . . ? ClB Cl FB 0.000(1) 7 7 ? ClB Cl FB 180.000(1) . 7 ? FB Cl FB 180.000(1) . 7 ? ClB Cl F 180.000(1) 7 . ? ClB Cl F 0.000(1) . . ? FB Cl F 0.000(1) . . ? FB Cl F 180.000(1) 7 . ? ClB Cl F 0.000(1) 7 7 ? ClB Cl F 180.000(1) . 7 ? FB Cl F 180.000(1) . 7 ? FB Cl F 0.000(1) 7 7 ? F Cl F 180.0 . 7 ? ClB Cl Ca2 53.31(5) 7 9 ? ClB Cl Ca2 126.69(5) . 9 ? FB Cl Ca2 126.69(5) . 9 ? FB Cl Ca2 53.31(5) 7 9 ? F Cl Ca2 126.69(5) . 9 ? F Cl Ca2 53.31(5) 7 9 ? ClB Cl Ca2 126.69(5) 7 3 ? ClB Cl Ca2 53.31(5) . 3 ? FB Cl Ca2 53.31(5) . 3 ? FB Cl Ca2 126.69(5) 7 3 ? F Cl Ca2 53.31(5) . 3 ? F Cl Ca2 126.69(5) 7 3 ? Ca2 Cl Ca2 180.00(9) 9 3 ? ClB Cl Ca2 126.69(5) 7 . ? ClB Cl Ca2 53.31(5) . . ? FB Cl Ca2 53.31(5) . . ? FB Cl Ca2 126.69(5) 7 . ? F Cl Ca2 53.31(5) . . ? F Cl Ca2 126.69(5) 7 . ? Ca2 Cl Ca2 92.04(7) 9 . ? Ca2 Cl Ca2 87.96(7) 3 . ? ClB Cl Ca2 53.31(5) 7 8 ? ClB Cl Ca2 126.69(5) . 8 ? FB Cl Ca2 126.69(5) . 8 ? FB Cl Ca2 53.31(5) 7 8 ? F Cl Ca2 126.69(5) . 8 ? F Cl Ca2 53.31(5) 7 8 ? Ca2 Cl Ca2 87.96(7) 9 8 ? Ca2 Cl Ca2 92.04(7) 3 8 ? Ca2 Cl Ca2 92.04(7) . 8 ? ClB Cl Ca2 126.69(5) 7 2 ? ClB Cl Ca2 53.31(5) . 2 ? FB Cl Ca2 53.31(5) . 2 ? FB Cl Ca2 126.69(5) 7 2 ? F Cl Ca2 53.31(5) . 2 ? F Cl Ca2 126.69(5) 7 2 ? Ca2 Cl Ca2 92.04(7) 9 2 ? Ca2 Cl Ca2 87.96(7) 3 2 ? Ca2 Cl Ca2 87.96(7) . 2 ? Ca2 Cl Ca2 180.00(15) 8 2 ? ClB Cl Ca2 53.31(5) 7 7 ? ClB Cl Ca2 126.69(5) . 7 ? FB Cl Ca2 126.69(5) . 7 ? FB Cl Ca2 53.31(5) 7 7 ? F Cl Ca2 126.69(5) . 7 ? F Cl Ca2 53.31(5) 7 7 ? Ca2 Cl Ca2 87.96(7) 9 7 ? Ca2 Cl Ca2 92.04(7) 3 7 ? Ca2 Cl Ca2 180.0 . 7 ? Ca2 Cl Ca2 87.96(7) 8 7 ? Ca2 Cl Ca2 92.04(7) 2 7 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 33.06 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.422 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.069