 
data_calcioaravaipaite 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Al Ca2 F9 Pb' 
_chemical_formula_weight          485.33 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Al'  'Al'   0.0645   0.0514 
 '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' 
 'Pb'  'Pb'  -3.3944  10.1111 
 '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                    5.3815(3) 
_cell_length_b                    5.3846(3) 
_cell_length_c                    12.2034(6) 
_cell_angle_alpha                 91.364(2) 
_cell_angle_beta                  101.110(3) 
_cell_angle_gamma                 91.525(3) 
_cell_volume                      346.72(3) 
_cell_formula_units_Z             2 
_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           0.04 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     4.649 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              432 
_exptl_absorpt_coefficient_mu     26.057 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.4221 
_exptl_absorpt_correction_T_max   0.4221 
_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_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8559 
_diffrn_reflns_av_R_equivalents   0.0211 
_diffrn_reflns_av_sigmaI/netI     0.0228 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.40 
_diffrn_reflns_theta_max          32.60 
_reflns_number_total              2427 
_reflns_number_gt                 2257 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0203P)²+0.3468P] where P=(Fo²+2Fc²)/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(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2427 
_refine_ls_number_parameters      119 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0227 
_refine_ls_R_factor_gt            0.0195 
_refine_ls_wR_factor_ref          0.0419 
_refine_ls_wR_factor_gt           0.0412 
_refine_ls_goodness_of_fit_ref    1.082 
_refine_ls_restrained_S_all       1.082 
_refine_ls_shift/su_max           0.995 
_refine_ls_shift/su_mean          0.008 
 
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 
Pb Pb 0.27238(3) 0.28211(2) 0.107209(10) 0.01678(5) Uani 1 1 d . . . 
Ca1 Ca 0.04213(11) 0.75777(10) 0.61450(5) 0.00876(11) Uani 1 1 d . . . 
Ca2 Ca 0.44851(11) 0.73503(10) 0.38616(5) 0.00891(11) Uani 1 1 d . . . 
Al Al 0.20387(18) 0.20662(16) 0.81864(8) 0.00910(16) Uani 1 1 d . . . 
F1 F 0.8481(5) 0.0489(4) 0.09603(19) 0.0234(5) Uani 1 1 d . . . 
F2 F 0.7419(4) 0.5504(3) 0.27419(17) 0.0165(4) Uani 1 1 d . . . 
F3 F 0.3698(4) 0.0017(3) 0.73490(16) 0.0141(4) Uani 1 1 d . . . 
F4 F 0.0419(4) 0.4057(4) 0.90021(17) 0.0180(4) Uani 1 1 d . . . 
F5 F 0.9168(4) 0.1103(4) 0.72148(18) 0.0169(4) Uani 1 1 d . . . 
F6 F 0.5004(4) 0.2955(4) 0.90746(19) 0.0226(4) Uani 1 1 d . . . 
F7 F 0.2517(4) 0.0076(3) 0.50112(16) 0.0118(3) Uani 1 1 d . . . 
F8 F 0.2503(4) 0.5117(3) 0.50560(16) 0.0116(3) Uani 1 1 d . . . 
F9 F 0.2567(4) 0.3857(3) 0.29105(17) 0.0154(4) Uani 1 1 d . . . 
 
 
_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 
Pb F9 2.3169(19) . ? 
Pb F4 2.407(2) 2_566 ? 
Pb F1 2.555(2) 1_455 ? 
Pb F6 2.580(2) 2_666 ? 
Pb F4 2.698(2) 1_554 ? 
Pb F6 2.934(2) 1_554 ? 
Pb F3 2.936(2) 2_656 ? 
Pb F1 2.976(2) 2_655 ? 
Pb F2 3.210(2) . ? 
Pb F5 3.285(2) 2_656 ? 
Pb F6 3.386(2) 2_656 ? 
Pb F1 3.399(2) . ? 
Pb Al 3.4821(9) 1_554 ? 
Pb Al 3.8506(9) 2_666 ? 
Pb Al 3.8679(9) 2_556 ? 
Pb Al 3.9005(10) 2_656 ? 
Ca1 F9 2.281(2) 2_566 ? 
Ca1 F8 2.3118(19) . ? 
Ca1 F7 2.328(2) 2_566 ? 
Ca1 F2 2.356(2) 2_666 ? 
Ca1 F7 2.3676(19) 1_565 ? 
Ca1 F8 2.370(2) 2_566 ? 
Ca1 F3 2.404(2) 1_565 ? 
Ca1 F5 2.460(2) 1_465 ? 
Ca1 Al 3.4017(11) 1_565 ? 
Ca1 Ca2 3.6920(8) 2_566 ? 
Ca1 Ca2 3.8101(9) 1_455 ? 
Ca1 Ca2 3.8189(8) 2_676 ? 
Ca2 F9 2.298(2) . ? 
Ca2 F8 2.3071(19) . ? 
Ca2 F7 2.313(2) 2_666 ? 
Ca2 F5 2.330(2) 2_666 ? 
Ca2 F8 2.348(2) 2_666 ? 
Ca2 F3 2.394(2) 2_666 ? 
Ca2 F7 2.4085(19) 1_565 ? 
Ca2 F2 2.490(2) . ? 
Ca2 Al 3.4137(11) 2_666 ? 
Ca2 Ca1 3.6920(8) 2_566 ? 
Ca2 Ca2 3.7749(12) 2_666 ? 
Ca2 Ca1 3.8101(9) 1_655 ? 
Al F1 1.793(2) 2_656 ? 
Al F6 1.794(2) . ? 
Al F4 1.798(2) . ? 
Al F2 1.805(2) 2_666 ? 
Al F5 1.812(2) 1_455 ? 
Al F3 1.847(2) . ? 
Al Ca1 3.4016(11) 1_545 ? 
Al Ca2 3.4136(11) 2_666 ? 
Al Pb 3.4822(9) 1_556 ? 
Al Pb 3.8506(9) 2_666 ? 
Al Pb 3.8679(9) 2_556 ? 
Al Pb 3.9005(10) 2_656 ? 
F1 Al 1.793(2) 2_656 ? 
F1 Pb 2.555(2) 1_655 ? 
F1 Pb 2.976(2) 2_655 ? 
F2 Al 1.805(2) 2_666 ? 
F2 Ca1 2.356(2) 2_666 ? 
F2 Pb 4.088(2) 1_655 ? 
F3 Ca2 2.394(2) 2_666 ? 
F3 Ca1 2.404(2) 1_545 ? 
F3 Pb 2.9364(19) 2_656 ? 
F4 Pb 2.407(2) 2_566 ? 
F4 Pb 2.698(2) 1_556 ? 
F4 Pb 4.022(2) 2_556 ? 
F4 Pb 4.032(2) 2_666 ? 
F5 Al 1.812(2) 1_655 ? 
F5 Ca2 2.330(2) 2_666 ? 
F5 Ca1 2.460(2) 1_645 ? 
F5 Pb 3.285(2) 2_656 ? 
F5 Pb 4.097(2) 2_666 ? 
F6 Pb 2.580(2) 2_666 ? 
F6 Pb 2.934(2) 1_556 ? 
F6 Pb 3.386(2) 2_656 ? 
F7 Ca2 2.313(2) 2_666 ? 
F7 Ca1 2.328(2) 2_566 ? 
F7 Ca1 2.3675(19) 1_545 ? 
F7 Ca2 2.4085(19) 1_545 ? 
F8 Ca2 2.348(2) 2_666 ? 
F8 Ca1 2.370(2) 2_566 ? 
F9 Ca1 2.281(2) 2_566 ? 
 
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 
F9 Pb F4 73.88(7) . 2_566 ? 
F9 Pb F1 87.37(7) . 1_455 ? 
F4 Pb F1 73.68(7) 2_566 1_455 ? 
F9 Pb F6 89.04(7) . 2_666 ? 
F4 Pb F6 73.21(7) 2_566 2_666 ? 
F1 Pb F6 146.38(7) 1_455 2_666 ? 
F9 Pb F4 138.45(7) . 1_554 ? 
F4 Pb F4 64.58(8) 2_566 1_554 ? 
F1 Pb F4 80.63(7) 1_455 1_554 ? 
F6 Pb F4 80.12(7) 2_666 1_554 ? 
F9 Pb F6 153.66(6) . 1_554 ? 
F4 Pb F6 110.39(7) 2_566 1_554 ? 
F1 Pb F6 118.93(7) 1_455 1_554 ? 
F6 Pb F6 68.51(8) 2_666 1_554 ? 
F4 Pb F6 53.38(6) 1_554 1_554 ? 
F9 Pb F3 68.16(6) . 2_656 ? 
F4 Pb F3 142.05(6) 2_566 2_656 ? 
F1 Pb F3 104.03(6) 1_455 2_656 ? 
F6 Pb F3 105.54(6) 2_666 2_656 ? 
F4 Pb F3 153.37(6) 1_554 2_656 ? 
F6 Pb F3 103.71(6) 1_554 2_656 ? 
F9 Pb F1 152.76(6) . 2_655 ? 
F4 Pb F1 110.01(7) 2_566 2_655 ? 
F1 Pb F1 68.89(8) 1_455 2_655 ? 
F6 Pb F1 118.10(7) 2_666 2_655 ? 
F4 Pb F1 52.76(6) 1_554 2_655 ? 
F6 Pb F1 52.10(6) 1_554 2_655 ? 
F3 Pb F1 103.81(6) 2_656 2_655 ? 
F9 Pb F2 57.77(6) . . ? 
F4 Pb F2 100.80(6) 2_566 . ? 
F1 Pb F2 144.30(6) 1_455 . ? 
F6 Pb F2 50.09(6) 2_666 . ? 
F4 Pb F2 129.81(6) 1_554 . ? 
F6 Pb F2 96.28(5) 1_554 . ? 
F3 Pb F2 58.49(5) 2_656 . ? 
F1 Pb F2 141.61(6) 2_655 . ? 
F9 Pb F5 56.80(6) . 2_656 ? 
F4 Pb F5 100.89(6) 2_566 2_656 ? 
F1 Pb F5 49.24(6) 1_455 2_656 ? 
F6 Pb F5 145.04(6) 2_666 2_656 ? 
F4 Pb F5 129.46(6) 1_554 2_656 ? 
F6 Pb F5 141.34(6) 1_554 2_656 ? 
F3 Pb F5 57.81(5) 2_656 2_656 ? 
F1 Pb F5 96.49(5) 2_655 2_656 ? 
F2 Pb F5 99.67(5) . 2_656 ? 
F9 Pb F6 109.58(6) . 2_656 ? 
F4 Pb F6 157.19(6) 2_566 2_656 ? 
F1 Pb F6 83.85(6) 1_455 2_656 ? 
F6 Pb F6 128.50(8) 2_666 2_656 ? 
F4 Pb F6 108.45(6) 1_554 2_656 ? 
F6 Pb F6 76.92(6) 1_554 2_656 ? 
F3 Pb F6 47.47(5) 2_656 2_656 ? 
F1 Pb F6 56.44(6) 2_655 2_656 ? 
F2 Pb F6 99.76(5) . 2_656 ? 
F5 Pb F6 65.82(5) 2_656 2_656 ? 
F9 Pb F1 109.20(7) . . ? 
F4 Pb F1 156.81(6) 2_566 . ? 
F1 Pb F1 128.77(8) 1_455 . ? 
F6 Pb F1 83.77(6) 2_666 . ? 
F4 Pb F1 109.28(6) 1_554 . ? 
F6 Pb F1 56.58(6) 1_554 . ? 
F3 Pb F1 47.33(5) 2_656 . ? 
F1 Pb F1 78.15(7) 2_655 . ? 
F2 Pb F1 64.97(5) . . ? 
F5 Pb F1 99.62(5) 2_656 . ? 
F6 Pb F1 44.99(5) 2_656 . ? 
F9 Pb Al 169.06(5) . 1_554 ? 
F4 Pb Al 95.18(5) 2_566 1_554 ? 
F1 Pb Al 89.16(5) 1_455 1_554 ? 
F6 Pb Al 88.11(5) 2_666 1_554 ? 
F4 Pb Al 30.61(4) 1_554 1_554 ? 
F6 Pb Al 30.99(4) 1_554 1_554 ? 
F3 Pb Al 122.77(4) 2_656 1_554 ? 
F1 Pb Al 31.00(4) 2_655 1_554 ? 
F2 Pb Al 126.53(4) . 1_554 ? 
F5 Pb Al 126.84(4) 2_656 1_554 ? 
F6 Pb Al 80.32(4) 2_656 1_554 ? 
F1 Pb Al 80.98(4) . 1_554 ? 
F9 Pb Al 77.51(5) . 2_666 ? 
F4 Pb Al 89.44(5) 2_566 2_666 ? 
F1 Pb Al 160.02(5) 1_455 2_666 ? 
F6 Pb Al 23.17(5) 2_666 2_666 ? 
F4 Pb Al 102.05(5) 1_554 2_666 ? 
F6 Pb Al 76.57(4) 1_554 2_666 ? 
F3 Pb Al 82.57(4) 2_656 2_666 ? 
F1 Pb Al 128.51(4) 2_655 2_666 ? 
F2 Pb Al 27.77(4) . 2_666 ? 
F5 Pb Al 127.00(4) 2_656 2_666 ? 
F6 Pb Al 113.37(4) 2_656 2_666 ? 
F1 Pb Al 69.48(4) . 2_666 ? 
Al Pb Al 103.239(18) 1_554 2_666 ? 
F9 Pb Al 76.70(5) . 2_556 ? 
F4 Pb Al 89.79(5) 2_566 2_556 ? 
F1 Pb Al 22.40(5) 1_455 2_556 ? 
F6 Pb Al 160.43(5) 2_666 2_556 ? 
F4 Pb Al 101.63(5) 1_554 2_556 ? 
F6 Pb Al 128.22(4) 1_554 2_556 ? 
F3 Pb Al 81.75(4) 2_656 2_556 ? 
F1 Pb Al 76.37(4) 2_655 2_556 ? 
F2 Pb Al 127.14(4) . 2_556 ? 
F5 Pb Al 27.85(4) 2_656 2_556 ? 
F6 Pb Al 69.83(4) 2_656 2_556 ? 
F1 Pb Al 113.38(4) . 2_556 ? 
Al Pb Al 103.358(18) 1_554 2_556 ? 
Al Pb Al 153.35(3) 2_666 2_556 ? 
F9 Pb Al 95.08(5) . 2_656 ? 
F4 Pb Al 168.96(5) 2_566 2_656 ? 
F1 Pb Al 106.50(5) 1_455 2_656 ? 
F6 Pb Al 107.11(5) 2_666 2_656 ? 
F4 Pb Al 126.46(4) 1_554 2_656 ? 
F6 Pb Al 79.43(5) 1_554 2_656 ? 
F3 Pb Al 26.91(4) 2_656 2_656 ? 
F1 Pb Al 79.82(5) 2_655 2_656 ? 
F2 Pb Al 72.42(4) . 2_656 ? 
F5 Pb Al 72.33(4) 2_656 2_656 ? 
F6 Pb Al 27.35(4) 2_656 2_656 ? 
F1 Pb Al 27.35(4) . 2_656 ? 
Al Pb Al 95.86(2) 1_554 2_656 ? 
Al Pb Al 88.00(2) 2_666 2_656 ? 
Al Pb Al 87.694(19) 2_556 2_656 ? 
F9 Ca1 F8 124.56(7) 2_566 . ? 
F9 Ca1 F7 92.00(7) 2_566 2_566 ? 
F8 Ca1 F7 109.18(7) . 2_566 ? 
F9 Ca1 F2 77.48(7) 2_566 2_666 ? 
F8 Ca1 F2 70.92(7) . 2_666 ? 
F7 Ca1 F2 166.21(7) 2_566 2_666 ? 
F9 Ca1 F7 161.10(8) 2_566 1_565 ? 
F8 Ca1 F7 69.62(6) . 1_565 ? 
F7 Ca1 F7 70.29(8) 2_566 1_565 ? 
F2 Ca1 F7 121.03(7) 2_666 1_565 ? 
F9 Ca1 F8 70.82(7) 2_566 2_566 ? 
F8 Ca1 F8 69.52(8) . 2_566 ? 
F7 Ca1 F8 70.57(7) 2_566 2_566 ? 
F2 Ca1 F8 97.27(7) 2_666 2_566 ? 
F7 Ca1 F8 107.65(7) 1_565 2_566 ? 
F9 Ca1 F3 111.50(7) 2_566 1_565 ? 
F8 Ca1 F3 105.36(7) . 1_565 ? 
F7 Ca1 F3 114.04(7) 2_566 1_565 ? 
F2 Ca1 F3 78.51(7) 2_666 1_565 ? 
F7 Ca1 F3 71.91(7) 1_565 1_565 ? 
F8 Ca1 F3 174.36(7) 2_566 1_565 ? 
F9 Ca1 F5 72.20(7) 2_566 1_465 ? 
F8 Ca1 F5 162.99(7) . 1_465 ? 
F7 Ca1 F5 69.94(7) 2_566 1_465 ? 
F2 Ca1 F5 114.18(7) 2_666 1_465 ? 
F7 Ca1 F5 94.81(7) 1_565 1_465 ? 
F8 Ca1 F5 123.72(7) 2_566 1_465 ? 
F3 Ca1 F5 61.77(7) 1_565 1_465 ? 
F9 Ca1 Al 87.90(5) 2_566 1_565 ? 
F8 Ca1 Al 136.87(5) . 1_565 ? 
F7 Ca1 Al 95.53(5) 2_566 1_565 ? 
F2 Ca1 Al 92.98(6) 2_666 1_565 ? 
F7 Ca1 Al 87.35(5) 1_565 1_565 ? 
F8 Ca1 Al 153.60(5) 2_566 1_565 ? 
F3 Ca1 Al 31.53(5) 1_565 1_565 ? 
F5 Ca1 Al 31.04(5) 1_465 1_565 ? 
F9 Ca1 Ca2 36.42(5) 2_566 2_566 ? 
F8 Ca1 Ca2 91.37(5) . 2_566 ? 
F7 Ca1 Ca2 89.99(5) 2_566 2_566 ? 
F2 Ca1 Ca2 76.25(5) 2_666 2_566 ? 
F7 Ca1 Ca2 144.90(5) 1_565 2_566 ? 
F8 Ca1 Ca2 37.28(5) 2_566 2_566 ? 
F3 Ca1 Ca2 143.04(5) 1_565 2_566 ? 
F5 Ca1 Ca2 105.56(5) 1_465 2_566 ? 
Al Ca1 Ca2 124.28(3) 1_565 2_566 ? 
F9 Ca1 Ca2 78.40(6) 2_566 1_455 ? 
F8 Ca1 Ca2 90.85(5) . 1_455 ? 
F7 Ca1 Ca2 34.69(5) 2_566 1_455 ? 
F2 Ca1 Ca2 132.62(6) 2_666 1_455 ? 
F7 Ca1 Ca2 89.72(5) 1_565 1_455 ? 
F8 Ca1 Ca2 35.94(5) 2_566 1_455 ? 
F3 Ca1 Ca2 148.72(5) 1_565 1_455 ? 
F5 Ca1 Ca2 96.04(5) 1_465 1_455 ? 
Al Ca1 Ca2 126.13(2) 1_565 1_455 ? 
Ca2 Ca1 Ca2 60.397(18) 2_566 1_455 ? 
F9 Ca1 Ca2 143.93(5) 2_566 2_676 ? 
F8 Ca1 Ca2 88.26(5) . 2_676 ? 
F7 Ca1 Ca2 90.10(5) 2_566 2_676 ? 
F2 Ca1 Ca2 103.66(5) 2_666 2_676 ? 
F7 Ca1 Ca2 34.85(5) 1_565 2_676 ? 
F8 Ca1 Ca2 142.46(5) 2_566 2_676 ? 
F3 Ca1 Ca2 37.17(5) 1_565 2_676 ? 
F5 Ca1 Ca2 74.81(5) 1_465 2_676 ? 
Al Ca1 Ca2 56.07(2) 1_565 2_676 ? 
Ca2 Ca1 Ca2 179.63(3) 2_566 2_676 ? 
Ca2 Ca1 Ca2 119.567(17) 1_455 2_676 ? 
F9 Ca2 F8 71.66(7) . . ? 
F9 Ca2 F7 160.65(8) . 2_666 ? 
F8 Ca2 F7 105.99(7) . 2_666 ? 
F9 Ca2 F5 77.31(7) . 2_666 ? 
F8 Ca2 F5 96.86(8) . 2_666 ? 
F7 Ca2 F5 121.83(7) 2_666 2_666 ? 
F9 Ca2 F8 90.16(7) . 2_666 ? 
F8 Ca2 F8 71.62(8) . 2_666 ? 
F7 Ca2 F8 71.23(7) 2_666 2_666 ? 
F5 Ca2 F8 165.32(7) 2_666 2_666 ? 
F9 Ca2 F3 111.05(7) . 2_666 ? 
F8 Ca2 F3 174.67(7) . 2_666 ? 
F7 Ca2 F3 73.04(7) 2_666 2_666 ? 
F5 Ca2 F3 79.54(7) 2_666 2_666 ? 
F8 Ca2 F3 112.55(7) 2_666 2_666 ? 
F9 Ca2 F7 124.84(7) . 1_565 ? 
F8 Ca2 F7 68.98(6) . 1_565 ? 
F7 Ca2 F7 69.16(8) 2_666 1_565 ? 
F5 Ca2 F7 70.83(7) 2_666 1_565 ? 
F8 Ca2 F7 111.64(7) 2_666 1_565 ? 
F3 Ca2 F7 105.97(6) 2_666 1_565 ? 
F9 Ca2 F2 70.92(7) . . ? 
F8 Ca2 F2 123.71(7) . . ? 
F7 Ca2 F2 96.40(7) 2_666 . ? 
F5 Ca2 F2 113.86(8) 2_666 . ? 
F8 Ca2 F2 68.02(7) 2_666 . ? 
F3 Ca2 F2 61.57(6) 2_666 . ? 
F7 Ca2 F2 163.94(7) 1_565 . ? 
F9 Ca2 Al 87.82(5) . 2_666 ? 
F8 Ca2 Al 153.85(5) . 2_666 ? 
F7 Ca2 Al 87.92(5) 2_666 2_666 ? 
F5 Ca2 Al 94.13(6) 2_666 2_666 ? 
F8 Ca2 Al 92.99(5) 2_666 2_666 ? 
F3 Ca2 Al 31.24(5) 2_666 2_666 ? 
F7 Ca2 Al 137.17(5) 1_565 2_666 ? 
F2 Ca2 Al 30.85(4) . 2_666 ? 
F9 Ca2 Ca1 36.10(5) . 2_566 ? 
F8 Ca2 Ca1 38.48(5) . 2_566 ? 
F7 Ca2 Ca1 144.44(5) 2_666 2_566 ? 
F5 Ca2 Ca1 75.47(5) 2_666 2_566 ? 
F8 Ca2 Ca1 89.91(5) 2_666 2_566 ? 
F3 Ca2 Ca1 142.44(5) 2_666 2_566 ? 
F7 Ca2 Ca1 91.81(5) 1_565 2_566 ? 
F2 Ca2 Ca1 104.22(5) . 2_566 ? 
Al Ca2 Ca1 123.88(2) 2_666 2_566 ? 
F9 Ca2 Ca2 79.02(5) . 2_666 ? 
F8 Ca2 Ca2 36.17(5) . 2_666 ? 
F7 Ca2 Ca2 88.18(5) 2_666 2_666 ? 
F5 Ca2 Ca2 132.42(6) 2_666 2_666 ? 
F8 Ca2 Ca2 35.45(5) 2_666 2_666 ? 
F3 Ca2 Ca2 147.89(6) 2_666 2_666 ? 
F7 Ca2 Ca2 90.58(5) 1_565 2_666 ? 
F2 Ca2 Ca2 96.11(5) . 2_666 ? 
Al Ca2 Ca2 125.52(3) 2_666 2_666 ? 
Ca1 Ca2 Ca2 61.352(18) 2_566 2_666 ? 
F9 Ca2 Ca1 126.45(6) . 1_655 ? 
F8 Ca2 Ca1 87.63(5) . 1_655 ? 
F7 Ca2 Ca1 34.94(5) 2_666 1_655 ? 
F5 Ca2 Ca1 155.70(5) 2_666 1_655 ? 
F8 Ca2 Ca1 36.34(5) 2_666 1_655 ? 
F3 Ca2 Ca1 94.07(5) 2_666 1_655 ? 
F7 Ca2 Ca1 88.83(5) 1_565 1_655 ? 
F2 Ca2 Ca1 82.38(5) . 1_655 ? 
Al Ca2 Ca1 92.04(2) 2_666 1_655 ? 
Ca1 Ca2 Ca1 119.604(18) 2_566 1_655 ? 
Ca2 Ca2 Ca1 58.252(18) 2_666 1_655 ? 
F1 Al F6 92.71(12) 2_656 . ? 
F1 Al F4 89.72(11) 2_656 . ? 
F6 Al F4 89.93(11) . . ? 
F1 Al F2 176.35(11) 2_656 2_666 ? 
F6 Al F2 88.74(11) . 2_666 ? 
F4 Al F2 93.64(10) . 2_666 ? 
F1 Al F5 88.76(11) 2_656 1_455 ? 
F6 Al F5 175.96(12) . 1_455 ? 
F4 Al F5 93.84(11) . 1_455 ? 
F2 Al F5 89.57(11) 2_666 1_455 ? 
F1 Al F3 90.19(10) 2_656 . ? 
F6 Al F3 90.14(11) . . ? 
F4 Al F3 179.89(11) . . ? 
F2 Al F3 86.45(9) 2_666 . ? 
F5 Al F3 86.09(10) 1_455 . ? 
F1 Al Ca1 81.10(8) 2_656 1_545 ? 
F6 Al Ca1 132.13(9) . 1_545 ? 
F4 Al Ca1 137.01(8) . 1_545 ? 
F2 Al Ca1 95.44(8) 2_666 1_545 ? 
F5 Al Ca1 44.44(7) 1_455 1_545 ? 
F3 Al Ca1 42.91(7) . 1_545 ? 
F1 Al Ca2 131.88(8) 2_656 2_666 ? 
F6 Al Ca2 82.61(8) . 2_666 ? 
F4 Al Ca2 137.84(8) . 2_666 ? 
F2 Al Ca2 45.01(7) 2_666 2_666 ? 
F5 Al Ca2 93.60(8) 1_455 2_666 ? 
F3 Al Ca2 42.26(6) . 2_666 ? 
Ca1 Al Ca2 68.16(2) 1_545 2_666 ? 
F1 Al Pb 58.72(8) 2_656 1_556 ? 
F6 Al Pb 57.38(8) . 1_556 ? 
F4 Al Pb 49.82(7) . 1_556 ? 
F2 Al Pb 124.75(8) 2_666 1_556 ? 
F5 Al Pb 126.43(8) 1_455 1_556 ? 
F3 Al Pb 130.17(7) . 1_556 ? 
Ca1 Al Pb 139.81(3) 1_545 1_556 ? 
Ca2 Al Pb 139.96(3) 2_666 1_556 ? 
F1 Al Pb 126.07(9) 2_656 2_666 ? 
F6 Al Pb 34.47(7) . 2_666 ? 
F4 Al Pb 82.52(8) . 2_666 ? 
F2 Al Pb 55.96(7) 2_666 2_666 ? 
F5 Al Pb 144.78(8) 1_455 2_666 ? 
F3 Al Pb 97.59(7) . 2_666 ? 
Ca1 Al Pb 135.83(3) 1_545 2_666 ? 
Ca2 Al Pb 68.095(19) 2_666 2_666 ? 
Pb Al Pb 76.761(18) 1_556 2_666 ? 
F1 Al Pb 32.89(8) 2_656 2_556 ? 
F6 Al Pb 124.29(8) . 2_556 ? 
F4 Al Pb 81.66(8) . 2_556 ? 
F2 Al Pb 146.41(8) 2_666 2_556 ? 
F5 Al Pb 57.87(7) 1_455 2_556 ? 
F3 Al Pb 98.23(7) . 2_556 ? 
Ca1 Al Pb 68.002(19) 1_545 2_556 ? 
Ca2 Al Pb 135.73(3) 2_666 2_556 ? 
Pb Al Pb 76.642(18) 1_556 2_556 ? 
Pb Al Pb 153.35(3) 2_666 2_556 ? 
F1 Al Pb 60.57(8) 2_656 2_656 ? 
F6 Al Pb 60.13(8) . 2_656 ? 
F4 Al Pb 133.96(8) . 2_656 ? 
F2 Al Pb 117.56(8) 2_666 2_656 ? 
F5 Al Pb 117.66(7) 1_455 2_656 ? 
F3 Al Pb 46.03(7) . 2_656 ? 
Ca1 Al Pb 76.16(2) 1_545 2_656 ? 
Ca2 Al Pb 76.27(2) 2_666 2_656 ? 
Pb Al Pb 84.14(2) 1_556 2_656 ? 
Pb Al Pb 88.00(2) 2_666 2_656 ? 
Pb Al Pb 87.694(19) 2_556 2_656 ? 
Al F1 Pb 124.70(12) 2_656 1_655 ? 
Al F1 Pb 90.28(9) 2_656 2_655 ? 
Pb F1 Pb 111.11(8) 1_655 2_655 ? 
Al F1 Pb 92.08(9) 2_656 . ? 
Pb F1 Pb 128.77(8) 1_655 . ? 
Pb F1 Pb 101.85(7) 2_655 . ? 
Al F2 Ca1 141.06(11) 2_666 2_666 ? 
Al F2 Ca2 104.15(9) 2_666 . ? 
Ca1 F2 Ca2 105.83(8) 2_666 . ? 
Al F2 Pb 96.26(9) 2_666 . ? 
Ca1 F2 Pb 107.63(7) 2_666 . ? 
Ca2 F2 Pb 90.61(6) . . ? 
Al F2 Pb 74.87(7) 2_666 1_655 ? 
Ca1 F2 Pb 73.14(5) 2_666 1_655 ? 
Ca2 F2 Pb 175.12(8) . 1_655 ? 
Pb F2 Pb 94.25(5) . 1_655 ? 
Al F3 Ca2 106.50(9) . 2_666 ? 
Al F3 Ca1 105.56(9) . 1_545 ? 
Ca2 F3 Ca1 105.49(8) 2_666 1_545 ? 
Al F3 Pb 107.06(9) . 2_656 ? 
Ca2 F3 Pb 116.13(7) 2_666 2_656 ? 
Ca1 F3 Pb 115.31(7) 1_545 2_656 ? 
Al F4 Pb 144.99(12) . 2_566 ? 
Al F4 Pb 99.57(9) . 1_556 ? 
Pb F4 Pb 115.42(8) 2_566 1_556 ? 
Al F4 Pb 72.08(7) . 2_556 ? 
Pb F4 Pb 111.26(7) 2_566 2_556 ? 
Pb F4 Pb 83.14(5) 1_556 2_556 ? 
Al F4 Pb 71.24(7) . 2_666 ? 
Pb F4 Pb 110.85(7) 2_566 2_666 ? 
Pb F4 Pb 82.81(5) 1_556 2_666 ? 
Pb F4 Pb 137.67(5) 2_556 2_666 ? 
Al F5 Ca2 142.23(11) 1_655 2_666 ? 
Al F5 Ca1 104.53(9) 1_655 1_645 ? 
Ca2 F5 Ca1 106.86(8) 2_666 1_645 ? 
Al F5 Pb 94.28(8) 1_655 2_656 ? 
Ca2 F5 Pb 106.43(7) 2_666 2_656 ? 
Ca1 F5 Pb 89.41(6) 1_645 2_656 ? 
Al F5 Pb 74.58(7) 1_655 2_666 ? 
Ca2 F5 Pb 73.14(5) 2_666 2_666 ? 
Ca1 F5 Pb 177.45(8) 1_645 2_666 ? 
Pb F5 Pb 93.03(5) 2_656 2_666 ? 
Al F6 Pb 122.35(11) . 2_666 ? 
Al F6 Pb 91.63(9) . 1_556 ? 
Pb F6 Pb 111.49(8) 2_666 1_556 ? 
Al F6 Pb 92.52(9) . 2_656 ? 
Pb F6 Pb 128.50(8) 2_666 2_656 ? 
Pb F6 Pb 103.08(6) 1_556 2_656 ? 
Ca2 F7 Ca1 110.37(7) 2_666 2_566 ? 
Ca2 F7 Ca1 109.35(8) 2_666 1_545 ? 
Ca1 F7 Ca1 109.71(8) 2_566 1_545 ? 
Ca2 F7 Ca2 110.84(8) 2_666 1_545 ? 
Ca1 F7 Ca2 108.65(8) 2_566 1_545 ? 
Ca1 F7 Ca2 107.89(7) 1_545 1_545 ? 
Ca2 F8 Ca1 113.43(7) . . ? 
Ca2 F8 Ca2 108.38(8) . 2_666 ? 
Ca1 F8 Ca2 112.16(8) . 2_666 ? 
Ca2 F8 Ca1 104.24(8) . 2_566 ? 
Ca1 F8 Ca1 110.48(8) . 2_566 ? 
Ca2 F8 Ca1 107.72(7) 2_666 2_566 ? 
Ca1 F9 Ca2 107.47(8) 2_566 . ? 
Ca1 F9 Pb 125.29(9) 2_566 . ? 
Ca2 F9 Pb 124.45(9) . . ? 
 
_diffrn_measured_fraction_theta_max    0.959 
_diffrn_reflns_theta_full              32.60 
_diffrn_measured_fraction_theta_full   0.959 
_refine_diff_density_max    2.198 
_refine_diff_density_min   -0.949 
_refine_diff_density_rms    0.183 
