 
data_fluorphosphohedyphane
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Ca4.71 F2 O24 P6 Pb5.29' 
_chemical_formula_weight          1892.63 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Pb'  'Pb'  -3.3944  10.1111 
 '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' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'F'  'F'   0.0171   0.0103 
 '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, x, z+1/2' 
 '-y, x-y, z' 
 '-x, -y, z+1/2' 
 '-x+y, -x, z' 
 'y, -x+y, z+1/2' 
 '-x, -y, -z' 
 '-x+y, -x, -z-1/2' 
 'y, -x+y, -z' 
 'x, y, -z-1/2' 
 'x-y, x, -z' 
 '-y, x-y, -z-1/2' 
 
_cell_length_a                    9.6402(12) 
_cell_length_b                    9.6402(12) 
_cell_length_c                    7.0121(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      564.35(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           0.10 
_exptl_crystal_size_mid           0.03 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.569 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              828 
_exptl_absorpt_coefficient_mu     40.945 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.1122 
_exptl_absorpt_correction_T_max   0.4276 
_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_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             13324 
_diffrn_reflns_av_R_equivalents   0.0419 
_diffrn_reflns_av_sigmaI/netI     0.0124 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          3.79 
_diffrn_reflns_theta_max          27.41 
_reflns_number_total              459 
_reflns_number_gt                 444 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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^)+(0.0000P)^2^+5.6001P] 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        0.00036(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          459 
_refine_ls_number_parameters      41 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0186 
_refine_ls_R_factor_gt            0.0175 
_refine_ls_wR_factor_ref          0.0338 
_refine_ls_wR_factor_gt           0.0334 
_refine_ls_goodness_of_fit_ref    1.229 
_refine_ls_restrained_S_all       1.229 
_refine_ls_shift/su_max           0.000 
_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 0.3333 0.6667 0.0046(3) 0.0085(4) Uani 1 3 d S . . 
Pb2 Pb 0.23960(3) 0.00873(3) 0.2500 0.01181(12) Uani 0.882(7) 2 d SP . . 
Ca2 Ca 0.23960(3) 0.00873(3) 0.2500 0.01181(12) Uani 0.118(7) 2 d SP . . 
P P 0.4183(2) 0.3880(2) 0.2500 0.0099(5) Uani 1 2 d S . . 
O1 O 0.3592(6) 0.5078(6) 0.2500 0.0155(11) Uani 1 2 d S . . 
O2 O 0.6047(6) 0.4731(6) 0.2500 0.0163(12) Uani 1 2 d S . . 
O3 O 0.3610(5) 0.2780(4) 0.0733(6) 0.0188(9) Uani 1 1 d . . . 
F F 0.0000 0.0000 0.0000 0.057(3) Uani 1 6 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 
Ca1 0.0093(5) 0.0093(5) 0.0068(8) 0.000 0.000 0.0047(3) 
Pb2 0.00986(17) 0.00937(17) 0.01485(17) 0.000 0.000 0.00379(12) 
Ca2 0.00986(17) 0.00937(17) 0.01485(17) 0.000 0.000 0.00379(12) 
P 0.0101(9) 0.0076(8) 0.0120(10) 0.000 0.000 0.0043(7) 
O1 0.020(3) 0.014(3) 0.016(3) 0.000 0.000 0.011(2) 
O2 0.011(2) 0.016(3) 0.024(3) 0.000 0.000 0.007(2) 
O3 0.029(2) 0.0155(18) 0.017(2) -0.0051(16) -0.0074(17) 0.0144(16) 
F 0.048(4) 0.048(4) 0.076(9) 0.000 0.000 0.024(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 O1 2.398(4) 8_566 ? 
Ca1 O1 2.398(4) 3_665 ? 
Ca1 O1 2.398(4) . ? 
Ca1 O2 2.483(4) 2_554 ? 
Ca1 O2 2.483(4) 9_565 ? 
Ca1 O2 2.483(4) 7_665 ? 
Ca1 O3 2.774(4) 9_565 ? 
Ca1 O3 2.774(4) 11 ? 
Ca1 O3 2.774(4) 7_665 ? 
Ca1 P 3.2335(18) 2_554 ? 
Ca1 P 3.2335(18) 9_565 ? 
Ca1 P 3.2335(18) 7_665 ? 
Pb2 O2 2.407(5) 3_655 ? 
Pb2 O3 2.527(4) 9 ? 
Pb2 O3 2.527(4) 6 ? 
Pb2 O3 2.570(4) 10_556 ? 
Pb2 O3 2.570(4) . ? 
Pb2 F 2.8672(3) . ? 
Pb2 F 2.8672(3) 2 ? 
Pb2 P 3.1679(18) . ? 
Pb2 O1 3.200(5) 8_556 ? 
Pb2 O1 3.453(5) 3_655 ? 
Pb2 P 3.4906(19) 3_655 ? 
Pb2 O3 3.581(4) 5 ? 
Pb2 O3 3.581(4) 8_556 ? 
Pb2 P 3.6067(19) 8_556 ? 
Pb2 P 3.8755(9) 9_556 ? 
Pb2 P 3.8755(9) 9 ? 
P O1 1.523(5) . ? 
P O3 1.542(4) 10_556 ? 
P O3 1.542(4) . ? 
P O2 1.558(5) . ? 
P Ca1 3.2335(18) 2_655 ? 
P Ca1 3.2335(18) 7_665 ? 
P Ca2 3.4907(19) 8_666 ? 
P Pb2 3.4907(19) 8_666 ? 
P Pb2 3.6067(19) 3 ? 
P Pb2 3.8755(9) 2_554 ? 
O1 Ca1 2.398(4) 8_566 ? 
O1 Pb2 3.200(5) 3 ? 
O1 Pb2 3.453(5) 8_666 ? 
O2 Ca2 2.407(5) 8_666 ? 
O2 Pb2 2.407(5) 8_666 ? 
O2 Ca1 2.483(4) 7_665 ? 
O2 Ca1 2.483(4) 2_655 ? 
O3 Ca2 2.527(4) 2_554 ? 
O3 Pb2 2.527(4) 2_554 ? 
O3 Ca1 2.774(4) 7_665 ? 
O3 Pb2 3.581(4) 3 ? 
F Ca2 2.8672(3) 7 ? 
F Pb2 2.8672(3) 7 ? 
F Ca2 2.8672(3) 9 ? 
F Ca2 2.8672(3) 3 ? 
F Pb2 2.8672(3) 9 ? 
F Pb2 2.8672(3) 3 ? 
F Pb2 2.8672(3) 2_554 ? 
F Pb2 2.8672(3) 8_556 ? 
F Ca2 2.8672(3) 8_556 ? 
F Ca2 2.8672(3) 2_554 ? 
 
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 74.17(14) 8_566 3_665 ? 
O1 Ca1 O1 74.17(14) 8_566 . ? 
O1 Ca1 O1 74.17(14) 3_665 . ? 
O1 Ca1 O2 92.26(12) 8_566 2_554 ? 
O1 Ca1 O2 145.83(17) 3_665 2_554 ? 
O1 Ca1 O2 132.94(17) . 2_554 ? 
O1 Ca1 O2 132.95(17) 8_566 9_565 ? 
O1 Ca1 O2 92.26(12) 3_665 9_565 ? 
O1 Ca1 O2 145.82(17) . 9_565 ? 
O2 Ca1 O2 74.02(14) 2_554 9_565 ? 
O1 Ca1 O2 145.82(17) 8_566 7_665 ? 
O1 Ca1 O2 132.94(17) 3_665 7_665 ? 
O1 Ca1 O2 92.26(12) . 7_665 ? 
O2 Ca1 O2 74.02(14) 2_554 7_665 ? 
O2 Ca1 O2 74.02(14) 9_565 7_665 ? 
O1 Ca1 O3 77.05(14) 8_566 9_565 ? 
O1 Ca1 O3 79.89(15) 3_665 9_565 ? 
O1 Ca1 O3 145.42(13) . 9_565 ? 
O2 Ca1 O3 66.40(14) 2_554 9_565 ? 
O2 Ca1 O3 56.08(14) 9_565 9_565 ? 
O2 Ca1 O3 122.27(13) 7_665 9_565 ? 
O1 Ca1 O3 79.89(15) 8_566 11 ? 
O1 Ca1 O3 145.42(14) 3_665 11 ? 
O1 Ca1 O3 77.05(14) . 11 ? 
O2 Ca1 O3 56.08(14) 2_554 11 ? 
O2 Ca1 O3 122.27(13) 9_565 11 ? 
O2 Ca1 O3 66.40(14) 7_665 11 ? 
O3 Ca1 O3 116.23(6) 9_565 11 ? 
O1 Ca1 O3 145.42(14) 8_566 7_665 ? 
O1 Ca1 O3 77.05(14) 3_665 7_665 ? 
O1 Ca1 O3 79.89(15) . 7_665 ? 
O2 Ca1 O3 122.27(13) 2_554 7_665 ? 
O2 Ca1 O3 66.40(14) 9_565 7_665 ? 
O2 Ca1 O3 56.08(14) 7_665 7_665 ? 
O3 Ca1 O3 116.23(6) 9_565 7_665 ? 
O3 Ca1 O3 116.23(6) 11 7_665 ? 
O1 Ca1 P 88.31(10) 8_566 2_554 ? 
O1 Ca1 P 161.98(12) 3_665 2_554 ? 
O1 Ca1 P 105.50(12) . 2_554 ? 
O2 Ca1 P 27.87(12) 2_554 2_554 ? 
O2 Ca1 P 96.81(11) 9_565 2_554 ? 
O2 Ca1 P 64.83(12) 7_665 2_554 ? 
O3 Ca1 P 92.30(9) 9_565 2_554 ? 
O3 Ca1 P 28.45(8) 11 2_554 ? 
O3 Ca1 P 120.88(9) 7_665 2_554 ? 
O1 Ca1 P 105.50(12) 8_566 9_565 ? 
O1 Ca1 P 88.31(10) 3_665 9_565 ? 
O1 Ca1 P 161.98(12) . 9_565 ? 
O2 Ca1 P 64.83(12) 2_554 9_565 ? 
O2 Ca1 P 27.87(12) 9_565 9_565 ? 
O2 Ca1 P 96.82(11) 7_665 9_565 ? 
O3 Ca1 P 28.45(8) 9_565 9_565 ? 
O3 Ca1 P 120.88(9) 11 9_565 ? 
O3 Ca1 P 92.30(9) 7_665 9_565 ? 
P Ca1 P 92.46(4) 2_554 9_565 ? 
O1 Ca1 P 161.98(12) 8_566 7_665 ? 
O1 Ca1 P 105.50(12) 3_665 7_665 ? 
O1 Ca1 P 88.31(10) . 7_665 ? 
O2 Ca1 P 96.81(11) 2_554 7_665 ? 
O2 Ca1 P 64.83(12) 9_565 7_665 ? 
O2 Ca1 P 27.87(12) 7_665 7_665 ? 
O3 Ca1 P 120.88(9) 9_565 7_665 ? 
O3 Ca1 P 92.30(9) 11 7_665 ? 
O3 Ca1 P 28.45(8) 7_665 7_665 ? 
P Ca1 P 92.46(4) 2_554 7_665 ? 
P Ca1 P 92.46(4) 9_565 7_665 ? 
O2 Pb2 O3 80.69(10) 3_655 9 ? 
O2 Pb2 O3 80.69(10) 3_655 6 ? 
O3 Pb2 O3 127.58(18) 9 6 ? 
O2 Pb2 O3 70.88(13) 3_655 10_556 ? 
O3 Pb2 O3 135.52(13) 9 10_556 ? 
O3 Pb2 O3 81.28(6) 6 10_556 ? 
O2 Pb2 O3 70.88(13) 3_655 . ? 
O3 Pb2 O3 81.28(6) 9 . ? 
O3 Pb2 O3 135.52(13) 6 . ? 
O3 Pb2 O3 57.64(17) 10_556 . ? 
O2 Pb2 F 136.58(5) 3_655 . ? 
O3 Pb2 F 72.42(9) 9 . ? 
O3 Pb2 F 142.66(9) 6 . ? 
O3 Pb2 F 106.11(9) 10_556 . ? 
O3 Pb2 F 71.82(9) . . ? 
O2 Pb2 F 136.58(5) 3_655 2 ? 
O3 Pb2 F 142.66(9) 9 2 ? 
O3 Pb2 F 72.42(9) 6 2 ? 
O3 Pb2 F 71.82(9) 10_556 2 ? 
O3 Pb2 F 106.11(9) . 2 ? 
F Pb2 F 75.382(11) . 2 ? 
O2 Pb2 P 66.68(13) 3_655 . ? 
O3 Pb2 P 108.26(8) 9 . ? 
O3 Pb2 P 108.26(8) 6 . ? 
O3 Pb2 P 28.85(8) 10_556 . ? 
O3 Pb2 P 28.85(8) . . ? 
F Pb2 P 89.95(3) . . ? 
F Pb2 P 89.95(3) 2 . ? 
O2 Pb2 O1 98.95(15) 3_655 8_556 ? 
O3 Pb2 O1 67.62(9) 9 8_556 ? 
O3 Pb2 O1 67.62(9) 6 8_556 ? 
O3 Pb2 O1 148.61(9) 10_556 8_556 ? 
O3 Pb2 O1 148.61(9) . 8_556 ? 
F Pb2 O1 101.37(7) . 8_556 ? 
F Pb2 O1 101.37(7) 2 8_556 ? 
P Pb2 O1 165.63(9) . 8_556 ? 
O2 Pb2 O1 47.59(14) 3_655 3_655 ? 
O3 Pb2 O1 65.64(9) 9 3_655 ? 
O3 Pb2 O1 65.64(9) 6 3_655 ? 
O3 Pb2 O1 112.27(11) 10_556 3_655 ? 
O3 Pb2 O1 112.27(11) . 3_655 ? 
F Pb2 O1 136.20(4) . 3_655 ? 
F Pb2 O1 136.20(4) 2 3_655 ? 
P Pb2 O1 114.27(9) . 3_655 ? 
O1 Pb2 O1 51.36(17) 8_556 3_655 ? 
O2 Pb2 P 22.26(12) 3_655 3_655 ? 
O3 Pb2 P 72.22(9) 9 3_655 ? 
O3 Pb2 P 72.22(9) 6 3_655 ? 
O3 Pb2 P 90.26(9) 10_556 3_655 ? 
O3 Pb2 P 90.26(9) . 3_655 ? 
F Pb2 P 142.295(6) . 3_655 ? 
F Pb2 P 142.295(6) 2 3_655 ? 
P Pb2 P 88.94(6) . 3_655 ? 
O1 Pb2 P 76.69(10) 8_556 3_655 ? 
O1 Pb2 P 25.33(9) 3_655 3_655 ? 
O2 Pb2 O3 134.64(12) 3_655 5 ? 
O3 Pb2 O3 63.11(8) 9 5 ? 
O3 Pb2 O3 99.70(8) 6 5 ? 
O3 Pb2 O3 154.45(10) 10_556 5 ? 
O3 Pb2 O3 124.66(14) . 5 ? 
F Pb2 O3 58.22(6) . 5 ? 
F Pb2 O3 84.06(6) 2 5 ? 
P Pb2 O3 148.12(6) . 5 ? 
O1 Pb2 O3 43.66(10) 8_556 5 ? 
O1 Pb2 O3 90.85(10) 3_655 5 ? 
P Pb2 O3 114.50(7) 3_655 5 ? 
O2 Pb2 O3 134.64(12) 3_655 8_556 ? 
O3 Pb2 O3 99.70(8) 9 8_556 ? 
O3 Pb2 O3 63.11(8) 6 8_556 ? 
O3 Pb2 O3 124.66(14) 10_556 8_556 ? 
O3 Pb2 O3 154.45(10) . 8_556 ? 
F Pb2 O3 84.06(6) . 8_556 ? 
F Pb2 O3 58.22(6) 2 8_556 ? 
P Pb2 O3 148.12(6) . 8_556 ? 
O1 Pb2 O3 43.66(10) 8_556 8_556 ? 
O1 Pb2 O3 90.85(10) 3_655 8_556 ? 
P Pb2 O3 114.50(7) 3_655 8_556 ? 
O3 Pb2 O3 40.49(12) 5 8_556 ? 
O2 Pb2 P 123.89(12) 3_655 8_556 ? 
O3 Pb2 P 75.47(8) 9 8_556 ? 
O3 Pb2 P 75.47(8) 6 8_556 ? 
O3 Pb2 P 149.00(9) 10_556 8_556 ? 
O3 Pb2 P 149.00(9) . 8_556 ? 
F Pb2 P 81.70(2) . 8_556 ? 
F Pb2 P 81.70(2) 2 8_556 ? 
P Pb2 P 169.43(4) . 8_556 ? 
O1 Pb2 P 24.95(9) 8_556 8_556 ? 
O1 Pb2 P 76.31(9) 3_655 8_556 ? 
P Pb2 P 101.64(5) 3_655 8_556 ? 
O3 Pb2 P 24.78(6) 5 8_556 ? 
O3 Pb2 P 24.78(6) 8_556 8_556 ? 
O2 Pb2 P 70.00(4) 3_655 9_556 ? 
O3 Pb2 P 130.68(10) 9 9_556 ? 
O3 Pb2 P 13.73(8) 6 9_556 ? 
O3 Pb2 P 70.02(9) 10_556 9_556 ? 
O3 Pb2 P 122.05(9) . 9_556 ? 
F Pb2 P 151.80(3) . 9_556 ? 
F Pb2 P 77.00(3) 2 9_556 ? 
P Pb2 P 95.625(17) . 9_556 ? 
O1 Pb2 P 78.59(4) 8_556 9_556 ? 
O1 Pb2 P 65.27(3) 3_655 9_556 ? 
P Pb2 P 65.62(3) 3_655 9_556 ? 
O3 Pb2 P 113.28(7) 5 9_556 ? 
O3 Pb2 P 76.66(7) 8_556 9_556 ? 
P Pb2 P 88.840(18) 8_556 9_556 ? 
O2 Pb2 P 70.00(4) 3_655 9 ? 
O3 Pb2 P 13.73(8) 9 9 ? 
O3 Pb2 P 130.68(10) 6 9 ? 
O3 Pb2 P 122.05(9) 10_556 9 ? 
O3 Pb2 P 70.02(9) . 9 ? 
F Pb2 P 77.00(3) . 9 ? 
F Pb2 P 151.80(3) 2 9 ? 
P Pb2 P 95.625(17) . 9 ? 
O1 Pb2 P 78.59(4) 8_556 9 ? 
O1 Pb2 P 65.27(3) 3_655 9 ? 
P Pb2 P 65.62(2) 3_655 9 ? 
O3 Pb2 P 76.66(7) 5 9 ? 
O3 Pb2 P 113.28(7) 8_556 9 ? 
P Pb2 P 88.839(18) 8_556 9 ? 
P Pb2 P 129.56(5) 9_556 9 ? 
O1 P O3 112.32(18) . 10_556 ? 
O1 P O3 112.32(18) . . ? 
O3 P O3 106.9(3) 10_556 . ? 
O1 P O2 111.8(3) . . ? 
O3 P O2 106.6(2) 10_556 . ? 
O3 P O2 106.6(2) . . ? 
O1 P Pb2 133.0(2) . . ? 
O3 P Pb2 53.53(15) 10_556 . ? 
O3 P Pb2 53.53(15) . . ? 
O2 P Pb2 115.2(2) . . ? 
O1 P Ca1 135.42(14) . 2_655 ? 
O3 P Ca1 58.99(16) 10_556 2_655 ? 
O3 P Ca1 111.83(16) . 2_655 ? 
O2 P Ca1 48.17(13) . 2_655 ? 
Pb2 P Ca1 80.31(4) . 2_655 ? 
O1 P Ca1 135.42(14) . 7_665 ? 
O3 P Ca1 111.83(16) 10_556 7_665 ? 
O3 P Ca1 58.99(16) . 7_665 ? 
O2 P Ca1 48.17(13) . 7_665 ? 
Pb2 P Ca1 80.31(4) . 7_665 ? 
Ca1 P Ca1 67.01(6) 2_655 7_665 ? 
O1 P Ca2 76.0(2) . 8_666 ? 
O3 P Ca2 122.48(17) 10_556 8_666 ? 
O3 P Ca2 122.48(17) . 8_666 ? 
O2 P Ca2 35.82(19) . 8_666 ? 
Pb2 P Ca2 151.06(6) . 8_666 ? 
Ca1 P Ca2 75.65(4) 2_655 8_666 ? 
Ca1 P Ca2 75.65(4) 7_665 8_666 ? 
O1 P Pb2 76.0(2) . 8_666 ? 
O3 P Pb2 122.48(17) 10_556 8_666 ? 
O3 P Pb2 122.48(17) . 8_666 ? 
O2 P Pb2 35.82(19) . 8_666 ? 
Pb2 P Pb2 151.06(6) . 8_666 ? 
Ca1 P Pb2 75.65(4) 2_655 8_666 ? 
Ca1 P Pb2 75.65(4) 7_665 8_666 ? 
Ca2 P Pb2 0.000(10) 8_666 8_666 ? 
O1 P Pb2 62.4(2) . 3 ? 
O3 P Pb2 76.68(16) 10_556 3 ? 
O3 P Pb2 76.68(16) . 3 ? 
O2 P Pb2 174.2(2) . 3 ? 
Pb2 P Pb2 70.57(4) . 3 ? 
Ca1 P Pb2 135.58(4) 2_655 3 ? 
Ca1 P Pb2 135.58(4) 7_665 3 ? 
Ca2 P Pb2 138.36(5) 8_666 3 ? 
Pb2 P Pb2 138.36(5) 8_666 3 ? 
O1 P Pb2 89.86(9) . 2_554 ? 
O3 P Pb2 122.16(17) 10_556 2_554 ? 
O3 P Pb2 22.88(14) . 2_554 ? 
O2 P Pb2 113.36(4) . 2_554 ? 
Pb2 P Pb2 71.93(3) . 2_554 ? 
Ca1 P Pb2 133.30(5) 2_655 2_554 ? 
Ca1 P Pb2 71.76(3) 7_665 2_554 ? 
Ca2 P Pb2 114.38(3) 8_666 2_554 ? 
Pb2 P Pb2 114.38(3) 8_666 2_554 ? 
Pb2 P Pb2 67.75(3) 3 2_554 ? 
P O1 Ca1 133.02(11) . 8_566 ? 
P O1 Ca1 133.03(11) . . ? 
Ca1 O1 Ca1 91.74(18) 8_566 . ? 
P O1 Pb2 92.7(2) . 3 ? 
Ca1 O1 Pb2 96.15(15) 8_566 3 ? 
Ca1 O1 Pb2 96.15(15) . 3 ? 
P O1 Pb2 78.7(2) . 8_666 ? 
Ca1 O1 Pb2 89.85(14) 8_566 8_666 ? 
Ca1 O1 Pb2 89.85(14) . 8_666 ? 
Pb2 O1 Pb2 171.36(17) 3 8_666 ? 
P O2 Ca2 121.9(3) . 8_666 ? 
P O2 Pb2 121.9(3) . 8_666 ? 
Ca2 O2 Pb2 0.000(14) 8_666 8_666 ? 
P O2 Ca1 103.96(19) . 7_665 ? 
Ca2 O2 Ca1 115.19(15) 8_666 7_665 ? 
Pb2 O2 Ca1 115.19(15) 8_666 7_665 ? 
P O2 Ca1 103.96(19) . 2_655 ? 
Ca2 O2 Ca1 115.19(15) 8_666 2_655 ? 
Pb2 O2 Ca1 115.19(15) 8_666 2_655 ? 
Ca1 O2 Ca1 91.94(18) 7_665 2_655 ? 
P O2 Pb2 44.57(16) . . ? 
Ca2 O2 Pb2 166.50(19) 8_666 . ? 
Pb2 O2 Pb2 166.50(19) 8_666 . ? 
Ca1 O2 Pb2 73.40(12) 7_665 . ? 
Ca1 O2 Pb2 73.40(12) 2_655 . ? 
P O3 Ca2 143.4(2) . 2_554 ? 
P O3 Pb2 143.4(2) . 2_554 ? 
Ca2 O3 Pb2 0.000(14) 2_554 2_554 ? 
P O3 Pb2 97.62(19) . . ? 
Ca2 O3 Pb2 110.03(14) 2_554 . ? 
Pb2 O3 Pb2 110.03(14) 2_554 . ? 
P O3 Ca1 92.55(19) . 7_665 ? 
Ca2 O3 Ca1 104.67(14) 2_554 7_665 ? 
Pb2 O3 Ca1 104.67(14) 2_554 7_665 ? 
Pb2 O3 Ca1 101.09(12) . 7_665 ? 
P O3 Pb2 78.55(16) . 3 ? 
Ca2 O3 Pb2 84.39(10) 2_554 3 ? 
Pb2 O3 Pb2 84.39(10) 2_554 3 ? 
Pb2 O3 Pb2 77.50(10) . 3 ? 
Ca1 O3 Pb2 170.64(14) 7_665 3 ? 
Ca2 F Pb2 0.000(8) 7 7 ? 
Ca2 F Ca2 86.518(9) 7 9 ? 
Pb2 F Ca2 86.518(9) 7 9 ? 
Ca2 F Ca2 93.482(9) 7 3 ? 
Pb2 F Ca2 93.482(9) 7 3 ? 
Ca2 F Ca2 180.000(12) 9 3 ? 
Ca2 F Pb2 86.518(9) 7 9 ? 
Pb2 F Pb2 86.518(9) 7 9 ? 
Ca2 F Pb2 0.0 9 9 ? 
Ca2 F Pb2 180.0 3 9 ? 
Ca2 F Pb2 93.482(9) 7 3 ? 
Pb2 F Pb2 93.482(9) 7 3 ? 
Ca2 F Pb2 180.000(12) 9 3 ? 
Ca2 F Pb2 0.000(12) 3 3 ? 
Pb2 F Pb2 180.000(12) 9 3 ? 
Ca2 F Pb2 86.518(8) 7 2_554 ? 
Pb2 F Pb2 86.518(8) 7 2_554 ? 
Ca2 F Pb2 86.518(8) 9 2_554 ? 
Ca2 F Pb2 93.482(8) 3 2_554 ? 
Pb2 F Pb2 86.518(8) 9 2_554 ? 
Pb2 F Pb2 93.482(8) 3 2_554 ? 
Ca2 F Pb2 93.482(8) 7 8_556 ? 
Pb2 F Pb2 93.482(8) 7 8_556 ? 
Ca2 F Pb2 93.482(8) 9 8_556 ? 
Ca2 F Pb2 86.518(8) 3 8_556 ? 
Pb2 F Pb2 93.482(8) 9 8_556 ? 
Pb2 F Pb2 86.518(8) 3 8_556 ? 
Pb2 F Pb2 180.000(12) 2_554 8_556 ? 
Ca2 F Ca2 93.482(8) 7 8_556 ? 
Pb2 F Ca2 93.482(8) 7 8_556 ? 
Ca2 F Ca2 93.482(8) 9 8_556 ? 
Ca2 F Ca2 86.518(8) 3 8_556 ? 
Pb2 F Ca2 93.482(8) 9 8_556 ? 
Pb2 F Ca2 86.518(8) 3 8_556 ? 
Pb2 F Ca2 180.000(12) 2_554 8_556 ? 
Pb2 F Ca2 0.00(2) 8_556 8_556 ? 
Ca2 F Ca2 86.518(8) 7 2_554 ? 
Pb2 F Ca2 86.518(8) 7 2_554 ? 
Ca2 F Ca2 86.518(8) 9 2_554 ? 
Ca2 F Ca2 93.482(8) 3 2_554 ? 
Pb2 F Ca2 86.518(8) 9 2_554 ? 
Pb2 F Ca2 93.482(8) 3 2_554 ? 
Pb2 F Ca2 0.000(12) 2_554 2_554 ? 
Pb2 F Ca2 180.0 8_556 2_554 ? 
Ca2 F Ca2 180.0 8_556 2_554 ? 
Ca2 F Pb2 180.0 7 . ? 
Pb2 F Pb2 180.0 7 . ? 
Ca2 F Pb2 93.481(9) 9 . ? 
Ca2 F Pb2 86.519(8) 3 . ? 
Pb2 F Pb2 93.481(9) 9 . ? 
Pb2 F Pb2 86.519(8) 3 . ? 
Pb2 F Pb2 93.481(9) 2_554 . ? 
Pb2 F Pb2 86.519(9) 8_556 . ? 
Ca2 F Pb2 86.519(9) 8_556 . ? 
Ca2 F Pb2 93.481(9) 2_554 . ? 
 
_diffrn_measured_fraction_theta_max    0.981 
_diffrn_reflns_theta_full              27.41 
_diffrn_measured_fraction_theta_full   0.981 
_refine_diff_density_max    0.700 
_refine_diff_density_min   -1.452 
_refine_diff_density_rms    0.191 
