 
data_Sr4V3O5F13 
  
_audit_creation_method            SHELXL-2014/6 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'F13 O5 Sr4 V3' 
_chemical_formula_sum 
 'F13 O5 Sr4 V3' 
_chemical_formula_weight          830.30 
  
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' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Sr'  'Sr'  -1.5307   3.2498 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            14 
_space_group_name_H-M_alt         'P 21/n' 
_space_group_name_Hall            '-P 2yn' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    9.7805(7) 
_cell_length_b                    7.2405(5) 
_cell_length_c                    10.0361(7) 
_cell_angle_alpha                 90 
_cell_angle_beta                  108.917(2) 
_cell_angle_gamma                 90 
_cell_volume                      672.33(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     6098 
_cell_measurement_theta_min       2.527 
_cell_measurement_theta_max       32.640 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             'yellow-green' 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     4.101 
_exptl_crystal_F_000              756 
_exptl_crystal_size_max           0.150 
_exptl_crystal_size_mid           0.080 
_exptl_crystal_size_min           0.020 
_exptl_absorpt_coefficient_mu     17.917 
_shelx_estimated_absorpt_T_min    0.174 
_shelx_estimated_absorpt_T_max    0.716 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.3943 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'SADABS Version 2.05 (Bruker, 2001)' 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'sealed ceramic tube' 
_diffrn_measurement_device_type   'Bruker SMART APEX CCD diffractometer' 
_diffrn_measurement_method        'omega and phi scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             12587 
_diffrn_reflns_av_unetI/netI      0.0411 
_diffrn_reflns_av_R_equivalents   0.0472 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.527 
_diffrn_reflns_theta_max          32.654 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.989 
_diffrn_measured_fraction_theta_full  1.000 
_diffrn_reflns_Laue_measured_fraction_max    0.989 
_diffrn_reflns_Laue_measured_fraction_full   1.000 
_diffrn_reflns_point_group_measured_fraction_max   0.989 
_diffrn_reflns_point_group_measured_fraction_full  1.000 
_reflns_number_total              2435 
_reflns_number_gt                 2073 
_reflns_threshold_expression      'I > 2σ(I)' 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'SMART Version 5.631 (Bruker, 2001)' 
_computing_cell_refinement        'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_data_reduction         'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)' 
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' 
_computing_molecular_graphics     various 
_computing_publication_material   various 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0265P)²+0.0578P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    . 
_refine_ls_hydrogen_treatment     undef 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          2435 
_refine_ls_number_parameters      118 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0398 
_refine_ls_R_factor_gt            0.0298 
_refine_ls_wR_factor_ref          0.0606 
_refine_ls_wR_factor_gt           0.0576 
_refine_ls_goodness_of_fit_ref    1.030 
_refine_ls_restrained_S_all       1.030 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Sr1 Sr 0.05359(3) 0.11606(4) 0.34806(3) 0.00708(7) Uani 1 1 d . . . . . 
Sr2 Sr 0.63671(3) 0.09699(4) 0.21230(3) 0.00668(7) Uani 1 1 d . . . . . 
V1 V 0.23644(5) 0.12988(7) 0.02895(5) 0.00812(10) Uani 1 1 d . . . . . 
V2 V 0.52496(12) -0.03148(16) 0.50805(14) 0.0116(2) Uani 0.5 1 d . . P . . 
F1 F 0.13664(17) 0.0928(2) 0.60519(17) 0.0095(3) Uani 1 1 d . . . . . 
F2 F 0.83803(17) 0.2845(2) 0.36956(17) 0.0083(3) Uani 1 1 d . . . . . 
F3 F 0.38780(18) 0.2689(2) 0.15304(18) 0.0129(4) Uani 1 1 d . . . . . 
F4 F 0.38995(17) -0.0550(2) 0.05060(17) 0.0083(3) Uani 1 1 d . . . . . 
F5 F 0.14278(17) -0.0297(2) -0.12428(17) 0.0104(3) Uani 1 1 d . . . . . 
F6 F 0.50783(18) 0.1091(2) 0.66827(18) 0.0126(4) Uani 1 1 d . . . . . 
F7 F 0.3336(2) 0.1571(3) 0.4131(2) 0.0186(4) Uani 0.5 1 d . . P . . 
O7 O 0.3336(2) 0.1571(3) 0.4131(2) 0.0186(4) Uani 0.5 1 d . . P . . 
O1 O 0.1258(2) 0.3165(3) -0.0372(2) 0.0101(4) Uani 1 1 d . . . . . 
O2 O 0.1685(2) 0.0499(3) 0.1423(2) 0.0094(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 
Sr1 F1 2.4472(17) . ? 
Sr1 F2 2.5049(16) 1_455 ? 
Sr1 F5 2.5153(16) 3 ? 
Sr1 F1 2.5563(17) 3_556 ? 
Sr1 F4 2.5780(16) 2 ? 
Sr1 F3 2.5787(17) 2_545 ? 
Sr1 F7 2.618(2) . ? 
Sr1 F6 2.6254(17) 4_565 ? 
Sr1 O2 2.695(2) . ? 
Sr1 Sr2 3.8598(4) 1_455 ? 
Sr1 Sr2 3.9020(4) 2 ? 
Sr2 F2 2.4467(16) 2_645 ? 
Sr2 F2 2.4893(16) . ? 
Sr2 F1 2.4901(16) 4_665 ? 
Sr2 F4 2.5838(17) 3_655 ? 
Sr2 F6 2.6000(18) 3_656 ? 
Sr2 F3 2.6252(17) . ? 
Sr2 O1 2.626(2) 4_666 ? 
Sr2 F5 2.6277(17) 3_655 ? 
Sr2 F4 2.6703(16) . ? 
Sr2 F1 2.7430(16) 3_656 ? 
Sr2 V1 3.4709(6) 3_655 ? 
Sr2 V1 3.5988(6) 4_666 ? 
V1 O2 1.600(2) . ? 
V1 O1 1.724(2) . ? 
V1 F3 1.8870(17) . ? 
V1 F5 1.9041(17) . ? 
V1 F4 1.9704(17) . ? 
V1 F2 2.2273(17) 4_565 ? 
V1 Sr2 3.4709(6) 3_655 ? 
V1 Sr2 3.5988(6) 4_565 ? 
V2 V2 0.6490(17) 3_656 ? 
V2 O7 1.631(2) 3_656 ? 
V2 F7 1.631(2) 3_656 ? 
V2 F6 1.784(2) 3_656 ? 
V2 O1 1.937(2) 2_545 ? 
V2 F6 1.956(2) . ? 
V2 O1 1.973(2) 4_666 ? 
V2 F7 2.263(2) . ? 
V2 Sr2 3.6714(14) 3_656 ? 
V2 Sr1 3.9486(11) 3_656 ? 
F1 Sr2 2.4901(16) 4_566 ? 
F1 Sr1 2.5562(16) 3_556 ? 
F1 Sr2 2.7430(16) 3_656 ? 
F2 V1 2.2272(17) 4_666 ? 
F2 Sr2 2.4467(16) 2_655 ? 
F2 Sr1 2.5048(16) 1_655 ? 
F3 Sr1 2.5787(17) 2 ? 
F4 Sr1 2.5780(16) 2_545 ? 
F4 Sr2 2.5838(17) 3_655 ? 
F5 Sr1 2.5154(16) 3 ? 
F5 Sr2 2.6277(17) 3_655 ? 
F6 V2 1.784(2) 3_656 ? 
F6 Sr2 2.6000(18) 3_656 ? 
F6 Sr1 2.6254(17) 4_666 ? 
F7 V2 1.631(2) 3_656 ? 
O1 V2 1.937(2) 2 ? 
O1 V2 1.973(2) 4_565 ? 
O1 Sr2 2.626(2) 4_565 ? 
  
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 
F1 Sr1 F2 86.76(5) . 1_455 ? 
F1 Sr1 F5 145.16(6) . 3 ? 
F2 Sr1 F5 77.15(5) 1_455 3 ? 
F1 Sr1 F1 77.19(6) . 3_556 ? 
F2 Sr1 F1 65.74(5) 1_455 3_556 ? 
F5 Sr1 F1 68.06(5) 3 3_556 ? 
F1 Sr1 F4 72.07(5) . 2 ? 
F2 Sr1 F4 66.10(5) 1_455 2 ? 
F5 Sr1 F4 125.86(5) 3 2 ? 
F1 Sr1 F4 123.34(5) 3_556 2 ? 
F1 Sr1 F3 86.51(5) . 2_545 ? 
F2 Sr1 F3 132.02(5) 1_455 2_545 ? 
F5 Sr1 F3 81.97(5) 3 2_545 ? 
F1 Sr1 F3 66.44(5) 3_556 2_545 ? 
F4 Sr1 F3 151.95(5) 2 2_545 ? 
F1 Sr1 F7 77.43(6) . . ? 
F2 Sr1 F7 139.89(6) 1_455 . ? 
F5 Sr1 F7 133.23(6) 3 . ? 
F1 Sr1 F7 141.83(6) 3_556 . ? 
F4 Sr1 F7 73.96(6) 2 . ? 
F3 Sr1 F7 84.02(6) 2_545 . ? 
F1 Sr1 F6 134.53(5) . 4_565 ? 
F2 Sr1 F6 74.30(5) 1_455 4_565 ? 
F5 Sr1 F6 70.37(5) 3 4_565 ? 
F1 Sr1 F6 127.05(5) 3_556 4_565 ? 
F4 Sr1 F6 62.48(5) 2 4_565 ? 
F3 Sr1 F6 136.42(6) 2_545 4_565 ? 
F7 Sr1 F6 90.95(6) . 4_565 ? 
F1 Sr1 O2 135.85(6) . . ? 
F2 Sr1 O2 136.42(6) 1_455 . ? 
F5 Sr1 O2 70.07(6) 3 . ? 
F1 Sr1 O2 123.01(6) 3_556 . ? 
F4 Sr1 O2 112.16(6) 2 . ? 
F3 Sr1 O2 71.04(6) 2_545 . ? 
F7 Sr1 O2 63.17(6) . . ? 
F6 Sr1 O2 68.20(6) 4_565 . ? 
F1 Sr1 Sr2 108.74(4) . 1_455 ? 
F2 Sr1 Sr2 39.24(4) 1_455 1_455 ? 
F5 Sr1 Sr2 42.48(4) 3 1_455 ? 
F1 Sr1 Sr2 45.19(4) 3_556 1_455 ? 
F4 Sr1 Sr2 103.83(4) 2 1_455 ? 
F3 Sr1 Sr2 100.05(4) 2_545 1_455 ? 
F7 Sr1 Sr2 172.69(5) . 1_455 ? 
F6 Sr1 Sr2 81.91(4) 4_565 1_455 ? 
O2 Sr1 Sr2 112.24(4) . 1_455 ? 
F1 Sr1 Sr2 101.75(4) . 2 ? 
F2 Sr1 Sr2 37.47(4) 1_455 2 ? 
F5 Sr1 Sr2 84.00(4) 3 2 ? 
F1 Sr1 Sr2 102.56(4) 3_556 2 ? 
F4 Sr1 Sr2 42.89(4) 2 2 ? 
F3 Sr1 Sr2 164.72(4) 2_545 2 ? 
F7 Sr1 Sr2 110.18(5) . 2 ? 
F6 Sr1 Sr2 41.44(4) 4_565 2 ? 
O2 Sr1 Sr2 109.64(4) . 2 ? 
Sr2 Sr1 Sr2 65.228(6) 1_455 2 ? 
F2 Sr2 F2 124.89(3) 2_645 . ? 
F2 Sr2 F1 132.46(6) 2_645 4_665 ? 
F2 Sr2 F1 70.80(5) . 4_665 ? 
F2 Sr2 F4 62.36(5) 2_645 3_655 ? 
F2 Sr2 F4 120.58(5) . 3_655 ? 
F1 Sr2 F4 71.30(5) 4_665 3_655 ? 
F2 Sr2 F6 75.72(5) 2_645 3_656 ? 
F2 Sr2 F6 117.21(5) . 3_656 ? 
F1 Sr2 F6 142.43(5) 4_665 3_656 ? 
F4 Sr2 F6 120.89(5) 3_655 3_656 ? 
F2 Sr2 F3 123.34(5) 2_645 . ? 
F2 Sr2 F3 111.70(5) . . ? 
F1 Sr2 F3 66.67(5) 4_665 . ? 
F4 Sr2 F3 92.59(5) 3_655 . ? 
F6 Sr2 F3 76.92(5) 3_656 . ? 
F2 Sr2 O1 125.58(6) 2_645 4_666 ? 
F2 Sr2 O1 62.12(6) . 4_666 ? 
F1 Sr2 O1 101.75(6) 4_665 4_666 ? 
F4 Sr2 O1 169.59(6) 3_655 4_666 ? 
F6 Sr2 O1 59.91(6) 3_656 4_666 ? 
F3 Sr2 O1 77.36(6) . 4_666 ? 
F2 Sr2 F5 62.12(5) 2_645 3_655 ? 
F2 Sr2 F5 75.38(5) . 3_655 ? 
F1 Sr2 F5 84.69(5) 4_665 3_655 ? 
F4 Sr2 F5 57.11(5) 3_655 3_655 ? 
F6 Sr2 F5 132.59(5) 3_656 3_655 ? 
F3 Sr2 F5 144.46(5) . 3_655 ? 
O1 Sr2 F5 131.20(6) 4_666 3_655 ? 
F2 Sr2 F4 65.45(5) 2_645 . ? 
F2 Sr2 F4 169.56(5) . . ? 
F1 Sr2 F4 103.64(5) 4_665 . ? 
F4 Sr2 F4 63.82(6) 3_655 . ? 
F6 Sr2 F4 61.59(5) 3_656 . ? 
F3 Sr2 F4 57.91(5) . . ? 
O1 Sr2 F4 111.76(6) 4_666 . ? 
F5 Sr2 F4 113.44(5) 3_655 . ? 
F2 Sr2 F1 67.25(5) 2_645 3_656 ? 
F2 Sr2 F1 63.13(5) . 3_656 ? 
F1 Sr2 F1 128.84(4) 4_665 3_656 ? 
F4 Sr2 F1 114.53(5) 3_655 3_656 ? 
F6 Sr2 F1 81.21(5) 3_656 3_656 ? 
F3 Sr2 F1 151.42(5) . 3_656 ? 
O1 Sr2 F1 75.84(6) 4_666 3_656 ? 
F5 Sr2 F1 63.76(5) 3_655 3_656 ? 
F4 Sr2 F1 125.09(5) . 3_656 ? 
F2 Sr2 V1 39.67(4) 2_645 3_655 ? 
F2 Sr2 V1 108.20(4) . 3_655 ? 
F1 Sr2 V1 94.35(4) 4_665 3_655 ? 
F4 Sr2 V1 34.17(4) 3_655 3_655 ? 
F6 Sr2 V1 114.88(4) 3_656 3_655 ? 
F3 Sr2 V1 125.55(4) . 3_655 ? 
O1 Sr2 V1 156.25(5) 4_666 3_655 ? 
F5 Sr2 V1 32.84(4) 3_655 3_655 ? 
F4 Sr2 V1 80.68(4) . 3_655 ? 
F1 Sr2 V1 80.47(4) 3_656 3_655 ? 
F2 Sr2 V1 140.96(4) 2_645 4_666 ? 
F2 Sr2 V1 37.64(4) . 4_666 ? 
F1 Sr2 V1 81.23(4) 4_665 4_666 ? 
F4 Sr2 V1 151.05(4) 3_655 4_666 ? 
F6 Sr2 V1 86.59(4) 3_656 4_666 ? 
F3 Sr2 V1 84.57(4) . 4_666 ? 
O1 Sr2 V1 26.77(4) 4_666 4_666 ? 
F5 Sr2 V1 112.44(4) 3_655 4_666 ? 
F4 Sr2 V1 134.11(4) . 4_666 ? 
F1 Sr2 V1 75.91(4) 3_656 4_666 ? 
V1 Sr2 V1 145.103(9) 3_655 4_666 ? 
O2 V1 O1 101.76(10) . . ? 
O2 V1 F3 98.13(9) . . ? 
O1 V1 F3 95.53(9) . . ? 
O2 V1 F5 98.79(9) . . ? 
O1 V1 F5 94.98(9) . . ? 
F3 V1 F5 157.80(8) . . ? 
O2 V1 F4 98.79(9) . . ? 
O1 V1 F4 159.37(9) . . ? 
F3 V1 F4 83.29(7) . . ? 
F5 V1 F4 80.01(7) . . ? 
O2 V1 F2 174.83(9) . 4_565 ? 
O1 V1 F2 82.87(8) . 4_565 ? 
F3 V1 F2 83.59(7) . 4_565 ? 
F5 V1 F2 78.38(7) . 4_565 ? 
F4 V1 F2 76.52(7) . 4_565 ? 
O2 V1 Sr2 130.49(8) . 3_655 ? 
O1 V1 Sr2 115.09(7) . 3_655 ? 
F3 V1 Sr2 109.36(6) . 3_655 ? 
F5 V1 Sr2 48.44(5) . 3_655 ? 
F4 V1 Sr2 47.43(5) . 3_655 ? 
F2 V1 Sr2 44.53(4) 4_565 3_655 ? 
O2 V1 Sr2 140.40(7) . 4_565 ? 
O1 V1 Sr2 43.33(7) . 4_565 ? 
F3 V1 Sr2 102.69(6) . 4_565 ? 
F5 V1 Sr2 72.46(5) . 4_565 ? 
F4 V1 Sr2 116.71(5) . 4_565 ? 
F2 V1 Sr2 43.05(4) 4_565 4_565 ? 
Sr2 V1 Sr2 72.538(11) 3_655 4_565 ? 
O2 V1 Sr2 103.63(7) . . ? 
O1 V1 Sr2 131.55(7) . . ? 
F3 V1 Sr2 40.55(5) . . ? 
F5 V1 Sr2 120.63(5) . . ? 
F4 V1 Sr2 42.84(5) . . ? 
F2 V1 Sr2 74.49(4) 4_565 . ? 
Sr2 V1 Sr2 76.124(12) 3_655 . ? 
Sr2 V1 Sr2 114.122(14) 4_565 . ? 
V2 V2 O7 164.7(3) 3_656 3_656 ? 
V2 V2 F7 164.7(3) 3_656 3_656 ? 
O7 V2 F7 0.0 3_656 3_656 ? 
V2 V2 F6 95.5(3) 3_656 3_656 ? 
O7 V2 F6 99.05(11) 3_656 3_656 ? 
F7 V2 F6 99.05(11) 3_656 3_656 ? 
V2 V2 O1 83.6(2) 3_656 2_545 ? 
O7 V2 O1 100.20(11) 3_656 2_545 ? 
F7 V2 O1 100.20(11) 3_656 2_545 ? 
F6 V2 O1 94.01(10) 3_656 2_545 ? 
V2 V2 F6 65.2(2) 3_656 . ? 
O7 V2 F6 100.17(11) 3_656 . ? 
F7 V2 F6 100.17(11) 3_656 . ? 
F6 V2 F6 160.71(6) 3_656 . ? 
O1 V2 F6 84.22(9) 2_545 . ? 
V2 V2 O1 77.3(2) 3_656 4_666 ? 
O7 V2 O1 98.25(11) 3_656 4_666 ? 
F7 V2 O1 98.25(11) 3_656 4_666 ? 
F6 V2 O1 87.86(10) 3_656 4_666 ? 
O1 V2 O1 160.92(5) 2_545 4_666 ? 
F6 V2 O1 87.77(9) . 4_666 ? 
V2 V2 F7 11.0(2) 3_656 . ? 
O7 V2 F7 175.6 3_656 . ? 
F7 V2 F7 175.65(9) 3_656 . ? 
F6 V2 F7 85.07(9) 3_656 . ? 
O1 V2 F7 80.82(9) 2_545 . ? 
F6 V2 F7 75.68(8) . . ? 
O1 V2 F7 80.42(9) 4_666 . ? 
V2 V2 Sr2 91.0(2) 3_656 . ? 
O7 V2 Sr2 96.19(9) 3_656 . ? 
F7 V2 Sr2 96.19(9) 3_656 . ? 
F6 V2 Sr2 43.02(6) 3_656 . ? 
O1 V2 Sr2 136.10(8) 2_545 . ? 
F6 V2 Sr2 132.30(7) . . ? 
O1 V2 Sr2 45.47(7) 4_666 . ? 
F7 V2 Sr2 85.84(6) . . ? 
V2 V2 Sr2 78.8(2) 3_656 3_656 ? 
O7 V2 Sr2 93.71(9) 3_656 3_656 ? 
F7 V2 Sr2 93.71(9) 3_656 3_656 ? 
F6 V2 Sr2 137.24(8) 3_656 3_656 ? 
O1 V2 Sr2 43.40(7) 2_545 3_656 ? 
F6 V2 Sr2 42.75(6) . 3_656 ? 
O1 V2 Sr2 130.48(8) 4_666 3_656 ? 
F7 V2 Sr2 84.12(6) . 3_656 ? 
Sr2 V2 Sr2 169.82(3) . 3_656 ? 
V2 V2 Sr1 144.3(3) 3_656 3_656 ? 
O7 V2 Sr1 27.75(8) 3_656 3_656 ? 
F7 V2 Sr1 27.75(8) 3_656 3_656 ? 
F6 V2 Sr1 98.31(7) 3_656 3_656 ? 
O1 V2 Sr1 127.74(7) 2_545 3_656 ? 
F6 V2 Sr1 97.91(7) . 3_656 ? 
O1 V2 Sr1 70.51(7) 4_666 3_656 ? 
F7 V2 Sr1 150.52(7) . 3_656 ? 
Sr2 V2 Sr1 77.39(2) . 3_656 ? 
Sr2 V2 Sr1 110.96(3) 3_656 3_656 ? 
Sr1 F1 Sr2 110.29(6) . 4_566 ? 
Sr1 F1 Sr1 102.81(6) . 3_556 ? 
Sr2 F1 Sr1 110.66(6) 4_566 3_556 ? 
Sr1 F1 Sr2 131.20(7) . 3_656 ? 
Sr2 F1 Sr2 106.05(6) 4_566 3_656 ? 
Sr1 F1 Sr2 93.43(5) 3_556 3_656 ? 
V1 F2 Sr2 95.79(6) 4_666 2_655 ? 
V1 F2 Sr2 99.31(6) 4_666 . ? 
Sr2 F2 Sr2 115.89(6) 2_655 . ? 
V1 F2 Sr1 141.38(7) 4_666 1_655 ? 
Sr2 F2 Sr1 104.00(6) 2_655 1_655 ? 
Sr2 F2 Sr1 101.22(6) . 1_655 ? 
V1 F3 Sr1 130.17(8) . 2 ? 
V1 F3 Sr2 111.59(8) . . ? 
Sr1 F3 Sr2 105.79(6) 2 . ? 
V1 F4 Sr1 136.83(8) . 2_545 ? 
V1 F4 Sr2 98.41(6) . 3_655 ? 
Sr1 F4 Sr2 103.42(6) 2_545 3_655 ? 
V1 F4 Sr2 107.04(7) . . ? 
Sr1 F4 Sr2 96.04(5) 2_545 . ? 
Sr2 F4 Sr2 116.18(6) 3_655 . ? 
V1 F5 Sr1 154.18(9) . 3 ? 
V1 F5 Sr2 98.72(6) . 3_655 ? 
Sr1 F5 Sr2 97.24(6) 3 3_655 ? 
V2 F6 V2 19.29(6) 3_656 . ? 
V2 F6 Sr2 109.07(9) 3_656 3_656 ? 
V2 F6 Sr2 106.54(8) . 3_656 ? 
V2 F6 Sr1 148.91(10) 3_656 4_666 ? 
V2 F6 Sr1 156.73(10) . 4_666 ? 
Sr2 F6 Sr1 96.61(6) 3_656 4_666 ? 
V2 F7 V2 4.35(9) 3_656 . ? 
V2 F7 Sr1 135.39(12) 3_656 . ? 
V2 F7 Sr1 133.78(10) . . ? 
V1 O1 V2 143.22(13) . 2 ? 
V1 O1 V2 145.89(13) . 4_565 ? 
V2 O1 V2 19.08(5) 2 4_565 ? 
V1 O1 Sr2 109.89(9) . 4_565 ? 
V2 O1 Sr2 106.16(9) 2 4_565 ? 
V2 O1 Sr2 102.16(9) 4_565 4_565 ? 
V1 O2 Sr1 148.53(11) . . ? 
  
_refine_diff_density_max    1.083 
_refine_diff_density_min   -0.766 
_refine_diff_density_rms    0.200

#===END
 
 
data_Pb7V4O8F18 
  
_audit_creation_method            SHELXL-2014/6 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'F18 O8 Pb7 V4' 
_chemical_formula_sum 
 'F18 O8 Pb7 V4' 
_chemical_formula_weight          2124.09 
  
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' 
 'V'  'V'   0.3005   0.5294 
 '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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            14 
_space_group_name_H-M_alt         'P 21/n' 
_space_group_name_Hall            '-P 2yn' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    10.1963(7) 
_cell_length_b                    7.3172(5) 
_cell_length_c                    13.9271(10) 
_cell_angle_alpha                 90 
_cell_angle_beta                  99.057(2) 
_cell_angle_gamma                 90 
_cell_volume                      1026.12(12) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     6152 
_cell_measurement_theta_min       2.688 
_cell_measurement_theta_max       35.152 
  
_exptl_crystal_description        polyhedron 
_exptl_crystal_colour             yellow 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     6.875 
_exptl_crystal_F_000              1784 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.100 
_exptl_crystal_size_mid           0.070 
_exptl_crystal_size_min           0.050 
_exptl_absorpt_coefficient_mu     59.113 
_shelx_estimated_absorpt_T_min    0.067 
_shelx_estimated_absorpt_T_max    0.156 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.1603 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'SADABS Version 2.05 (Bruker, 2001)' 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'sealed tube' 
_diffrn_measurement_device_type   'Bruker SMART APEX CCD diffractometer' 
_diffrn_measurement_method        'omega and phi scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             27943 
_diffrn_reflns_av_unetI/netI      0.0352 
_diffrn_reflns_av_R_equivalents   0.0589 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.311 
_diffrn_reflns_theta_max          32.506 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   1.000 
_diffrn_measured_fraction_theta_full  1.000 
_diffrn_reflns_Laue_measured_fraction_max    1.000 
_diffrn_reflns_Laue_measured_fraction_full   1.000 
_diffrn_reflns_point_group_measured_fraction_max   1.000 
_diffrn_reflns_point_group_measured_fraction_full  1.000 
_reflns_number_total              3702 
_reflns_number_gt                 3298 
_reflns_threshold_expression      'I > 2σ(I)' 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'SMART Version 5.631 (Bruker, 2001)' 
_computing_cell_refinement        'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_data_reduction         'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)' 
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' 
_computing_molecular_graphics     various 
_computing_publication_material   various 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0264P)²+7.3420P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    . 
_refine_ls_hydrogen_treatment     undef 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00201(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          3702 
_refine_ls_number_parameters      170 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0368 
_refine_ls_R_factor_gt            0.0306 
_refine_ls_wR_factor_ref          0.0703 
_refine_ls_wR_factor_gt           0.0678 
_refine_ls_goodness_of_fit_ref    1.101 
_refine_ls_restrained_S_all       1.101 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pb1 Pb 0.79001(3) 0.66238(4) 0.31716(2) 0.01241(7) Uani 1 1 d . . . . . 
Pb2 Pb 0.82165(3) 0.15371(3) 0.46917(2) 0.01036(7) Uani 1 1 d . . . . . 
Pb3 Pb 0.44894(3) -0.01319(4) 0.35596(2) 0.01124(7) Uani 1 1 d . . . . . 
Pb4 Pb 0.5000 0.5000 0.5000 0.01250(8) Uani 1 2 d S . P . . 
V1 V 0.42979(13) 0.48879(17) 0.23279(9) 0.0133(2) Uani 1 1 d . . . . . 
V2 V 0.16756(13) 0.36491(18) 0.40560(9) 0.0133(2) Uani 1 1 d . . . . . 
F1 F 0.5545(4) 0.6412(6) 0.3393(3) 0.0117(8) Uani 1 1 d . . . . . 
F2 F 0.3149(4) 0.5110(6) 0.3437(3) 0.0133(8) Uani 1 1 d . . . . . 
F3 F 0.5067(4) 0.2928(6) 0.3069(3) 0.0150(8) Uani 1 1 d . . . . . 
F4 F 0.2474(5) 0.5274(6) 0.5134(3) 0.0152(8) Uani 1 1 d . . . . . 
F5 F 0.3252(4) 0.2196(6) 0.4511(3) 0.0122(8) Uani 1 1 d . . . . . 
F6 F 0.0563(5) 0.5515(6) 0.3638(3) 0.0188(9) Uani 1 1 d . . . . . 
F7 F 0.5871(4) 0.1590(6) 0.4948(3) 0.0108(8) Uani 1 1 d . . . . . 
F8 F 0.6863(4) -0.0190(6) 0.3453(3) 0.0137(8) Uani 1 1 d . . . . . 
F9 F 0.7988(5) 0.3178(6) 0.3250(3) 0.0130(8) Uani 1 1 d . . . . . 
O1 O 0.3033(5) 0.3927(7) 0.1630(4) 0.0124(9) Uani 1 1 d . . . . . 
O2 O 0.5458(5) 0.4842(7) 0.1589(4) 0.0153(10) Uani 1 1 d . . . . . 
O3 O 0.3682(5) 0.7397(7) 0.1993(3) 0.0113(9) Uani 1 1 d . . . . . 
O4 O 0.0817(5) 0.2533(7) 0.4789(4) 0.0108(9) 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 
Pb1 F9 2.339(4) 2_655 ? 
Pb1 F1 2.474(4) . ? 
Pb1 F9 2.525(4) . ? 
Pb1 F8 2.615(4) 1_565 ? 
Pb1 F8 2.666(4) 2_655 ? 
Pb1 F6 2.810(5) 1_655 ? 
Pb1 F4 2.816(4) 3_666 ? 
Pb1 O2 2.878(5) 2_655 ? 
Pb1 Pb2 3.9715(4) 2_655 ? 
Pb1 Pb3 4.0705(4) 2_655 ? 
Pb2 F9 2.319(4) . ? 
Pb2 F8 2.394(4) . ? 
Pb2 F4 2.461(4) 3_666 ? 
Pb2 F7 2.473(4) . ? 
Pb2 O2 2.703(5) 2_645 ? 
Pb2 O4 2.732(5) 1_655 ? 
Pb2 O1 2.756(5) 4_666 ? 
Pb2 Pb1 3.9715(4) 2_645 ? 
Pb2 Pb3 4.0661(4) . ? 
Pb2 Pb3 4.0886(4) 3_656 ? 
Pb3 F7 2.416(4) 3_656 ? 
Pb3 F3 2.440(4) . ? 
Pb3 F8 2.448(4) . ? 
Pb3 F7 2.540(4) . ? 
Pb3 F5 2.602(4) . ? 
Pb3 O1 2.636(5) 2_545 ? 
Pb3 F1 2.772(4) 1_545 ? 
Pb3 O3 2.853(5) 1_545 ? 
Pb3 Pb3 3.9878(6) 3_656 ? 
Pb3 Pb1 4.0705(4) 2_645 ? 
Pb3 Pb4 4.0810(3) 1_545 ? 
Pb4 F1 2.603(4) . ? 
Pb4 F1 2.603(4) 3_666 ? 
Pb4 F4 2.619(5) 3_666 ? 
Pb4 F4 2.619(5) . ? 
Pb4 F2 2.649(4) 3_666 ? 
Pb4 F2 2.649(4) . ? 
Pb4 F7 2.653(4) . ? 
Pb4 F7 2.653(4) 3_666 ? 
Pb4 F5 2.733(4) 3_666 ? 
Pb4 F5 2.733(4) . ? 
Pb4 V2 3.5766(13) . ? 
Pb4 V2 3.5766(13) 3_666 ? 
V1 O1 1.645(5) . ? 
V1 O2 1.685(5) . ? 
V1 F3 1.866(4) . ? 
V1 O3 1.972(5) . ? 
V1 F2 2.086(4) . ? 
V1 F1 2.114(4) . ? 
V2 O4 1.661(5) . ? 
V2 O3 1.715(5) 2_545 ? 
V2 F6 1.812(5) . ? 
V2 F5 1.948(4) . ? 
V2 F4 1.986(5) . ? 
V2 F2 2.133(4) . ? 
F1 Pb3 2.772(4) 1_565 ? 
F4 Pb2 2.461(4) 3_666 ? 
F4 Pb1 2.816(4) 3_666 ? 
F6 Pb1 2.810(5) 1_455 ? 
F7 Pb3 2.416(4) 3_656 ? 
F8 Pb1 2.615(4) 1_545 ? 
F8 Pb1 2.666(4) 2_645 ? 
F9 Pb1 2.339(4) 2_645 ? 
O1 Pb3 2.636(5) 2 ? 
O1 Pb2 2.756(5) 4_565 ? 
O2 Pb2 2.703(5) 2_655 ? 
O2 Pb1 2.878(5) 2_645 ? 
O3 V2 1.715(5) 2 ? 
O3 Pb3 2.853(5) 1_565 ? 
O4 Pb2 2.732(5) 1_455 ? 
  
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 Pb1 F1 83.22(15) 2_655 . ? 
F9 Pb1 F9 121.92(11) 2_655 . ? 
F1 Pb1 F9 87.75(14) . . ? 
F9 Pb1 F8 65.25(14) 2_655 1_565 ? 
F1 Pb1 F8 67.27(14) . 1_565 ? 
F9 Pb1 F8 153.69(14) . 1_565 ? 
F9 Pb1 F8 66.33(14) 2_655 2_655 ? 
F1 Pb1 F8 107.11(14) . 2_655 ? 
F9 Pb1 F8 62.12(13) . 2_655 ? 
F8 Pb1 F8 131.58(10) 1_565 2_655 ? 
F9 Pb1 F6 124.58(15) 2_655 1_655 ? 
F1 Pb1 F6 151.00(14) . 1_655 ? 
F9 Pb1 F6 71.04(14) . 1_655 ? 
F8 Pb1 F6 128.43(14) 1_565 1_655 ? 
F8 Pb1 F6 80.75(14) 2_655 1_655 ? 
F9 Pb1 F4 149.76(15) 2_655 3_666 ? 
F1 Pb1 F4 66.55(13) . 3_666 ? 
F9 Pb1 F4 58.65(13) . 3_666 ? 
F8 Pb1 F4 101.69(13) 1_565 3_666 ? 
F8 Pb1 F4 120.53(13) 2_655 3_666 ? 
F6 Pb1 F4 85.26(13) 1_655 3_666 ? 
F9 Pb1 O2 80.85(16) 2_655 2_655 ? 
F1 Pb1 O2 126.53(14) . 2_655 ? 
F9 Pb1 O2 142.74(15) . 2_655 ? 
F8 Pb1 O2 59.66(14) 1_565 2_655 ? 
F8 Pb1 O2 112.13(14) 2_655 2_655 ? 
F6 Pb1 O2 71.71(15) 1_655 2_655 ? 
F4 Pb1 O2 117.36(14) 3_666 2_655 ? 
F9 Pb1 Pb2 31.35(10) 2_655 2_655 ? 
F1 Pb1 Pb2 89.65(9) . 2_655 ? 
F9 Pb1 Pb2 91.74(9) . 2_655 ? 
F8 Pb1 Pb2 96.07(10) 1_565 2_655 ? 
F8 Pb1 Pb2 35.92(9) 2_655 2_655 ? 
F6 Pb1 Pb2 109.97(10) 1_655 2_655 ? 
F4 Pb1 Pb2 141.13(9) 3_666 2_655 ? 
O2 Pb1 Pb2 101.47(11) 2_655 2_655 ? 
F9 Pb1 Pb3 81.61(11) 2_655 2_655 ? 
F1 Pb1 Pb3 142.41(10) . 2_655 ? 
F9 Pb1 Pb3 71.84(10) . 2_655 ? 
F8 Pb1 Pb3 133.45(10) 1_565 2_655 ? 
F8 Pb1 Pb3 35.45(10) 2_655 2_655 ? 
F6 Pb1 Pb3 49.30(10) 1_655 2_655 ? 
F4 Pb1 Pb3 121.91(9) 3_666 2_655 ? 
O2 Pb1 Pb3 84.49(11) 2_655 2_655 ? 
Pb2 Pb1 Pb3 60.728(7) 2_655 2_655 ? 
F9 Pb2 F8 71.43(15) . . ? 
F9 Pb2 F4 66.63(14) . 3_666 ? 
F8 Pb2 F4 115.50(15) . 3_666 ? 
F9 Pb2 F7 98.57(15) . . ? 
F8 Pb2 F7 69.59(14) . . ? 
F4 Pb2 F7 70.88(14) 3_666 . ? 
F9 Pb2 O2 70.05(16) . 2_645 ? 
F8 Pb2 O2 64.75(15) . 2_645 ? 
F4 Pb2 O2 132.92(15) 3_666 2_645 ? 
F7 Pb2 O2 134.24(15) . 2_645 ? 
F9 Pb2 O4 82.48(15) . 1_655 ? 
F8 Pb2 O4 128.43(15) . 1_655 ? 
F4 Pb2 O4 91.87(15) 3_666 1_655 ? 
F7 Pb2 O4 160.29(14) . 1_655 ? 
O2 Pb2 O4 64.73(15) 2_645 1_655 ? 
F9 Pb2 O1 153.97(15) . 4_666 ? 
F8 Pb2 O1 121.38(16) . 4_666 ? 
F4 Pb2 O1 87.45(15) 3_666 4_666 ? 
F7 Pb2 O1 69.19(14) . 4_666 ? 
O2 Pb2 O1 135.06(16) 2_645 4_666 ? 
O4 Pb2 O1 101.48(15) 1_655 4_666 ? 
F9 Pb2 Pb1 31.66(10) . 2_645 ? 
F8 Pb2 Pb1 40.80(11) . 2_645 ? 
F4 Pb2 Pb1 92.45(10) 3_666 2_645 ? 
F7 Pb2 Pb1 90.78(9) . 2_645 ? 
O2 Pb2 Pb1 55.86(12) 2_645 2_645 ? 
O4 Pb2 Pb1 99.69(10) 1_655 2_645 ? 
O1 Pb2 Pb1 158.83(11) 4_666 2_645 ? 
F9 Pb2 Pb3 81.93(11) . . ? 
F8 Pb2 Pb3 33.31(10) . . ? 
F4 Pb2 Pb3 93.36(11) 3_666 . ? 
F7 Pb2 Pb3 36.35(9) . . ? 
O2 Pb2 Pb3 98.06(11) 2_645 . ? 
O4 Pb2 Pb3 160.01(10) 1_655 . ? 
O1 Pb2 Pb3 98.02(11) 4_666 . ? 
Pb1 Pb2 Pb3 60.839(7) 2_645 . ? 
F9 Pb2 Pb3 131.35(12) . 3_656 ? 
F8 Pb2 Pb3 85.99(11) . 3_656 ? 
F4 Pb2 Pb3 87.08(10) 3_666 3_656 ? 
F7 Pb2 Pb3 32.81(9) . 3_656 ? 
O2 Pb2 Pb3 137.07(11) 2_645 3_656 ? 
O4 Pb2 Pb3 141.08(10) 1_655 3_656 ? 
O1 Pb2 Pb3 39.60(11) 4_666 3_656 ? 
Pb1 Pb2 Pb3 119.237(9) 2_645 3_656 ? 
Pb3 Pb2 Pb3 58.552(8) . 3_656 ? 
F7 Pb3 F3 136.25(14) 3_656 . ? 
F7 Pb3 F8 109.29(14) 3_656 . ? 
F3 Pb3 F8 73.40(15) . . ? 
F7 Pb3 F7 72.87(16) 3_656 . ? 
F3 Pb3 F7 68.18(14) . . ? 
F8 Pb3 F7 67.66(14) . . ? 
F7 Pb3 F5 72.51(13) 3_656 . ? 
F3 Pb3 F5 72.53(14) . . ? 
F8 Pb3 F5 127.25(14) . . ? 
F7 Pb3 F5 62.82(13) . . ? 
F7 Pb3 O1 72.09(14) 3_656 2_545 ? 
F3 Pb3 O1 119.12(15) . 2_545 ? 
F8 Pb3 O1 161.41(15) . 2_545 ? 
F7 Pb3 O1 128.42(14) . 2_545 ? 
F5 Pb3 O1 71.24(15) . 2_545 ? 
F7 Pb3 F1 77.45(13) 3_656 1_545 ? 
F3 Pb3 F1 134.39(14) . 1_545 ? 
F8 Pb3 F1 65.06(13) . 1_545 ? 
F7 Pb3 F1 109.87(13) . 1_545 ? 
F5 Pb3 F1 149.91(13) . 1_545 ? 
O1 Pb3 F1 98.00(14) 2_545 1_545 ? 
F7 Pb3 O3 108.26(14) 3_656 1_545 ? 
F3 Pb3 O3 114.89(14) . 1_545 ? 
F8 Pb3 O3 96.40(14) . 1_545 ? 
F7 Pb3 O3 162.74(14) . 1_545 ? 
F5 Pb3 O3 134.37(14) . 1_545 ? 
O1 Pb3 O3 66.32(15) 2_545 1_545 ? 
F1 Pb3 O3 55.05(13) 1_545 1_545 ? 
F7 Pb3 Pb3 37.49(10) 3_656 3_656 ? 
F3 Pb3 Pb3 101.59(10) . 3_656 ? 
F8 Pb3 Pb3 87.59(10) . 3_656 ? 
F7 Pb3 Pb3 35.38(9) . 3_656 ? 
F5 Pb3 Pb3 61.77(9) . 3_656 ? 
O1 Pb3 Pb3 102.09(11) 2_545 3_656 ? 
F1 Pb3 Pb3 94.87(8) 1_545 3_656 ? 
O3 Pb3 Pb3 142.95(10) 1_545 3_656 ? 
F7 Pb3 Pb2 93.35(10) 3_656 . ? 
F3 Pb3 Pb2 65.21(10) . . ? 
F8 Pb3 Pb2 32.48(10) . . ? 
F7 Pb3 Pb2 35.25(9) . . ? 
F5 Pb3 Pb2 95.99(9) . . ? 
O1 Pb3 Pb2 162.77(11) 2_545 . ? 
F1 Pb3 Pb2 87.41(9) 1_545 . ? 
O3 Pb3 Pb2 128.78(10) 1_545 . ? 
Pb3 Pb3 Pb2 61.006(7) 3_656 . ? 
F7 Pb3 Pb1 148.36(10) 3_656 2_645 ? 
F3 Pb3 Pb1 48.34(11) . 2_645 ? 
F8 Pb3 Pb1 39.17(10) . 2_645 ? 
F7 Pb3 Pb1 87.60(10) . 2_645 ? 
F5 Pb3 Pb1 120.63(9) . 2_645 ? 
O1 Pb3 Pb1 137.90(11) 2_545 2_645 ? 
F1 Pb3 Pb1 86.54(9) 1_545 2_645 ? 
O3 Pb3 Pb1 83.34(10) 1_545 2_645 ? 
Pb3 Pb3 Pb1 119.285(11) 3_656 2_645 ? 
Pb2 Pb3 Pb1 58.433(7) . 2_645 ? 
F7 Pb3 Pb4 38.41(10) 3_656 1_545 ? 
F3 Pb3 Pb4 157.04(10) . 1_545 ? 
F8 Pb3 Pb4 87.93(10) . 1_545 ? 
F7 Pb3 Pb4 92.66(9) . 1_545 ? 
F5 Pb3 Pb4 110.83(9) . 1_545 ? 
O1 Pb3 Pb4 82.43(11) 2_545 1_545 ? 
F1 Pb3 Pb4 39.08(9) 1_545 1_545 ? 
O3 Pb3 Pb4 79.73(10) 1_545 1_545 ? 
Pb3 Pb3 Pb4 63.565(7) 3_656 1_545 ? 
Pb2 Pb3 Pb4 91.859(7) . 1_545 ? 
Pb1 Pb3 Pb4 121.461(8) 2_645 1_545 ? 
F1 Pb4 F1 180.0 . 3_666 ? 
F1 Pb4 F4 67.90(13) . 3_666 ? 
F1 Pb4 F4 112.10(13) 3_666 3_666 ? 
F1 Pb4 F4 112.10(13) . . ? 
F1 Pb4 F4 67.90(13) 3_666 . ? 
F4 Pb4 F4 180.0 3_666 . ? 
F1 Pb4 F2 119.85(13) . 3_666 ? 
F1 Pb4 F2 60.15(13) 3_666 3_666 ? 
F4 Pb4 F2 58.31(13) 3_666 3_666 ? 
F4 Pb4 F2 121.69(13) . 3_666 ? 
F1 Pb4 F2 60.15(13) . . ? 
F1 Pb4 F2 119.85(13) 3_666 . ? 
F4 Pb4 F2 121.69(13) 3_666 . ? 
F4 Pb4 F2 58.31(13) . . ? 
F2 Pb4 F2 180.0 3_666 . ? 
F1 Pb4 F7 103.41(13) . . ? 
F1 Pb4 F7 76.59(13) 3_666 . ? 
F4 Pb4 F7 65.73(13) 3_666 . ? 
F4 Pb4 F7 114.27(14) . . ? 
F2 Pb4 F7 78.21(13) 3_666 . ? 
F2 Pb4 F7 101.79(13) . . ? 
F1 Pb4 F7 76.59(13) . 3_666 ? 
F1 Pb4 F7 103.41(13) 3_666 3_666 ? 
F4 Pb4 F7 114.27(13) 3_666 3_666 ? 
F4 Pb4 F7 65.73(13) . 3_666 ? 
F2 Pb4 F7 101.79(13) 3_666 3_666 ? 
F2 Pb4 F7 78.21(13) . 3_666 ? 
F7 Pb4 F7 180.0 . 3_666 ? 
F1 Pb4 F5 72.37(13) . 3_666 ? 
F1 Pb4 F5 107.63(13) 3_666 3_666 ? 
F4 Pb4 F5 57.67(13) 3_666 3_666 ? 
F4 Pb4 F5 122.33(13) . 3_666 ? 
F2 Pb4 F5 57.69(12) 3_666 3_666 ? 
F2 Pb4 F5 122.31(12) . 3_666 ? 
F7 Pb4 F5 120.33(12) . 3_666 ? 
F7 Pb4 F5 59.67(12) 3_666 3_666 ? 
F1 Pb4 F5 107.63(13) . . ? 
F1 Pb4 F5 72.37(13) 3_666 . ? 
F4 Pb4 F5 122.33(13) 3_666 . ? 
F4 Pb4 F5 57.67(13) . . ? 
F2 Pb4 F5 122.31(12) 3_666 . ? 
F2 Pb4 F5 57.69(12) . . ? 
F7 Pb4 F5 59.67(12) . . ? 
F7 Pb4 F5 120.33(12) 3_666 . ? 
F5 Pb4 F5 180.0 3_666 . ? 
F1 Pb4 V2 96.43(10) . . ? 
F1 Pb4 V2 83.57(10) 3_666 . ? 
F4 Pb4 V2 146.98(10) 3_666 . ? 
F4 Pb4 V2 33.02(10) . . ? 
F2 Pb4 V2 143.63(9) 3_666 . ? 
F2 Pb4 V2 36.37(9) . . ? 
F7 Pb4 V2 91.83(9) . . ? 
F7 Pb4 V2 88.17(9) 3_666 . ? 
F5 Pb4 V2 147.37(9) 3_666 . ? 
F5 Pb4 V2 32.63(9) . . ? 
F1 Pb4 V2 83.57(10) . 3_666 ? 
F1 Pb4 V2 96.43(10) 3_666 3_666 ? 
F4 Pb4 V2 33.02(10) 3_666 3_666 ? 
F4 Pb4 V2 146.98(10) . 3_666 ? 
F2 Pb4 V2 36.37(9) 3_666 3_666 ? 
F2 Pb4 V2 143.63(9) . 3_666 ? 
F7 Pb4 V2 88.17(9) . 3_666 ? 
F7 Pb4 V2 91.83(9) 3_666 3_666 ? 
F5 Pb4 V2 32.63(9) 3_666 3_666 ? 
F5 Pb4 V2 147.37(9) . 3_666 ? 
V2 Pb4 V2 180.0 . 3_666 ? 
O1 V1 O2 101.0(3) . . ? 
O1 V1 F3 102.7(2) . . ? 
O2 V1 F3 92.7(2) . . ? 
O1 V1 O3 93.9(2) . . ? 
O2 V1 O3 95.9(2) . . ? 
F3 V1 O3 159.5(2) . . ? 
O1 V1 F2 89.5(2) . . ? 
O2 V1 F2 169.4(2) . . ? 
F3 V1 F2 83.50(19) . . ? 
O3 V1 F2 84.68(19) . . ? 
O1 V1 F1 165.7(2) . . ? 
O2 V1 F1 92.1(2) . . ? 
F3 V1 F1 82.13(18) . . ? 
O3 V1 F1 78.98(19) . . ? 
F2 V1 F1 77.61(17) . . ? 
O4 V2 O3 101.5(2) . 2_545 ? 
O4 V2 F6 101.8(2) . . ? 
O3 V2 F6 95.2(2) 2_545 . ? 
O4 V2 F5 91.1(2) . . ? 
O3 V2 F5 92.2(2) 2_545 . ? 
F6 V2 F5 163.5(2) . . ? 
O4 V2 F4 91.3(2) . . ? 
O3 V2 F4 166.1(2) 2_545 . ? 
F6 V2 F4 87.3(2) . . ? 
F5 V2 F4 82.06(19) . . ? 
O4 V2 F2 165.5(2) . . ? 
O3 V2 F2 89.5(2) 2_545 . ? 
F6 V2 F2 86.4(2) . . ? 
F5 V2 F2 78.90(18) . . ? 
F4 V2 F2 76.98(18) . . ? 
O4 V2 Pb4 118.08(18) . . ? 
O3 V2 Pb4 121.53(18) 2_545 . ? 
F6 V2 Pb4 114.78(17) . . ? 
F5 V2 Pb4 49.12(13) . . ? 
F4 V2 Pb4 45.94(13) . . ? 
F2 V2 Pb4 47.41(12) . . ? 
V1 F1 Pb1 115.72(18) . . ? 
V1 F1 Pb4 101.98(17) . . ? 
Pb1 F1 Pb4 118.36(16) . . ? 
V1 F1 Pb3 109.95(17) . 1_565 ? 
Pb1 F1 Pb3 110.53(15) . 1_565 ? 
Pb4 F1 Pb3 98.74(14) . 1_565 ? 
V1 F2 V2 140.7(2) . . ? 
V1 F2 Pb4 101.27(17) . . ? 
V2 F2 Pb4 96.22(16) . . ? 
V1 F3 Pb3 139.5(2) . . ? 
V2 F4 Pb2 123.5(2) . 3_666 ? 
V2 F4 Pb4 101.03(18) . . ? 
Pb2 F4 Pb4 112.31(17) 3_666 . ? 
V2 F4 Pb1 104.17(18) . 3_666 ? 
Pb2 F4 Pb1 107.82(15) 3_666 3_666 ? 
Pb4 F4 Pb1 106.65(15) . 3_666 ? 
V2 F5 Pb3 129.3(2) . . ? 
V2 F5 Pb4 98.25(16) . . ? 
Pb3 F5 Pb4 105.61(15) . . ? 
V2 F6 Pb1 145.6(2) . 1_455 ? 
Pb3 F7 Pb2 113.49(16) 3_656 . ? 
Pb3 F7 Pb3 107.13(16) 3_656 . ? 
Pb2 F7 Pb3 108.40(15) . . ? 
Pb3 F7 Pb4 107.14(15) 3_656 . ? 
Pb2 F7 Pb4 110.75(16) . . ? 
Pb3 F7 Pb4 109.85(14) . . ? 
Pb2 F8 Pb3 114.21(17) . . ? 
Pb2 F8 Pb1 112.20(17) . 1_545 ? 
Pb3 F8 Pb1 116.85(17) . 1_545 ? 
Pb2 F8 Pb1 103.28(16) . 2_645 ? 
Pb3 F8 Pb1 105.39(16) . 2_645 ? 
Pb1 F8 Pb1 102.95(15) 1_545 2_645 ? 
Pb2 F9 Pb1 116.99(18) . 2_645 ? 
Pb2 F9 Pb1 123.55(17) . . ? 
Pb1 F9 Pb1 116.25(17) 2_645 . ? 
V1 O1 Pb3 127.5(3) . 2 ? 
V1 O1 Pb2 117.6(3) . 4_565 ? 
Pb3 O1 Pb2 98.60(16) 2 4_565 ? 
V1 O2 Pb2 149.9(3) . 2_655 ? 
V1 O2 Pb1 113.4(2) . 2_645 ? 
Pb2 O2 Pb1 96.29(16) 2_655 2_645 ? 
V2 O3 V1 135.7(3) 2 . ? 
V2 O3 Pb3 108.1(2) 2 1_565 ? 
V1 O3 Pb3 111.5(2) . 1_565 ? 
V2 O4 Pb2 134.6(3) . 1_455 ? 
  
_refine_diff_density_max    2.951 
_refine_diff_density_min   -2.079 
_refine_diff_density_rms    0.458

#===END

data_Pb2VO2F5 
  
_audit_creation_method            SHELXL-2014/6 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 'F5 O2 Pb2 V' 
_chemical_formula_sum 
 'F5 O2 Pb2 V' 
_chemical_formula_weight          592.32 
  
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' 
 'V'  'V'   0.3005   0.5294 
 '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' 
  
_space_group_crystal_system       triclinic 
_space_group_IT_number            2 
_space_group_name_H-M_alt         'P -1' 
_space_group_name_Hall            '-P 1' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    5.6675(5) 
_cell_length_b                    7.3492(6) 
_cell_length_c                    8.3152(7) 
_cell_angle_alpha                 101.2337(12) 
_cell_angle_beta                  108.9953(13) 
_cell_angle_gamma                 110.6249(12) 
_cell_volume                      287.14(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     7922 
_cell_measurement_theta_min       2.765 
_cell_measurement_theta_max       36.323 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     6.851 
_exptl_crystal_F_000              496 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.100 
_exptl_crystal_size_mid           0.060 
_exptl_crystal_size_min           0.050 
_exptl_absorpt_coefficient_mu     60.126 
_shelx_estimated_absorpt_T_min    0.065 
_shelx_estimated_absorpt_T_max    0.153 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.0231 
_exptl_absorpt_correction_T_max   0.0789 
_exptl_absorpt_process_details    'SADABS Version 2014/4 (Bruker, 2014)' 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'microfocus sealed X-ray tube' 
_diffrn_measurement_device_type   'Bruker D8 QUEST' 
_diffrn_measurement_method        'ω and φ scans'

_diffrn_standards_number          'n/a' 
_diffrn_standards_interval_count  'n/a' 
_diffrn_standards_interval_time   'n/a' 
_diffrn_standards_decay_%         'n/a'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             10075 
_diffrn_reflns_av_unetI/netI      0.0347 
_diffrn_reflns_av_R_equivalents   0.0407 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.765 
_diffrn_reflns_theta_max          36.346 
_diffrn_reflns_theta_full         36.300 
_diffrn_measured_fraction_theta_max   0.996 
_diffrn_measured_fraction_theta_full  0.998 
_diffrn_reflns_Laue_measured_fraction_max    0.996 
_diffrn_reflns_Laue_measured_fraction_full   0.998 
_diffrn_reflns_point_group_measured_fraction_max   0.996 
_diffrn_reflns_point_group_measured_fraction_full  0.998 
_reflns_number_total              2785 
_reflns_number_gt                 2649 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'Bruker APEXII v2014.9-0 (Bruker, 2014)' 
_computing_cell_refinement        'SAINT Version 8.34a (Bruker, 2014)' 
_computing_data_reduction         'SAINT Version 8.34a (Bruker, 2014)' 
_computing_structure_solution     'SHELXS (Sheldrick, 2008)' 
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' 
_computing_molecular_graphics     various 
_computing_publication_material   various 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0099P)²+7.9546P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    . 
_refine_ls_hydrogen_treatment     undef 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0150(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2785 
_refine_ls_number_parameters      92 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0322 
_refine_ls_R_factor_gt            0.0305 
_refine_ls_wR_factor_ref          0.0771 
_refine_ls_wR_factor_gt           0.0765 
_refine_ls_goodness_of_fit_ref    1.270 
_refine_ls_restrained_S_all       1.270 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pb1 Pb 0.02648(5) 0.24285(3) 0.39525(3) 0.00685(7) Uani 1 1 d . . . . . 
Pb2 Pb 0.29425(5) 0.78314(4) 0.24132(3) 0.00727(7) Uani 1 1 d . . . . . 
V1 V 0.3957(2) 0.31137(18) 0.08933(16) 0.00772(18) Uani 1 1 d . . . . . 
F1 F 0.1400(10) 0.6006(7) 0.4135(6) 0.0096(7) Uani 1 1 d . . . . . 
F2 F 0.2646(9) 0.0123(7) 0.4960(6) 0.0090(7) Uani 1 1 d . . . . . 
F3 F 0.2666(10) 0.1405(7) -0.1518(6) 0.0118(8) Uani 1 1 d . . . . . 
F4 F 0.5410(10) 0.5541(7) 0.2988(6) 0.0101(7) Uani 1 1 d . . . . . 
F5 F 0.7220(9) 0.4823(7) 0.0462(6) 0.0093(7) Uani 1 1 d . . . . . 
O1 O 0.0716(11) 0.2299(9) 0.0865(7) 0.0109(9) Uani 1 1 d . . . . . 
O2 O 0.5338(11) 0.1811(8) 0.1991(7) 0.0103(9) 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 
Pb1 F1 2.403(4) 2_566 ? 
Pb1 F1 2.437(4) . ? 
Pb1 F2 2.551(5) 2_556 ? 
Pb1 O2 2.553(6) 1_455 ? 
Pb1 F4 2.567(5) 2_666 ? 
Pb1 F2 2.612(4) . ? 
Pb1 O1 2.649(5) . ? 
Pb1 F3 2.662(4) 2 ? 
Pb2 F1 2.313(4) . ? 
Pb2 F2 2.408(5) 2_666 ? 
Pb2 F2 2.528(4) 1_565 ? 
Pb2 F4 2.560(5) . ? 
Pb2 F5 2.728(4) 2_665 ? 
Pb2 F3 2.729(5) 2_665 ? 
V1 O2 1.663(6) . ? 
V1 O1 1.710(5) . ? 
V1 F3 1.884(5) . ? 
V1 F4 1.927(5) . ? 
V1 F5 2.024(5) . ? 
V1 F5 2.214(5) 2_665 ? 
F1 Pb1 2.403(4) 2_566 ? 
F2 Pb2 2.408(5) 2_666 ? 
F2 Pb2 2.528(4) 1_545 ? 
F2 Pb1 2.551(4) 2_556 ? 
F3 Pb1 2.662(4) 2 ? 
F3 Pb2 2.729(5) 2_665 ? 
F4 Pb1 2.568(5) 2_666 ? 
F5 V1 2.214(5) 2_665 ? 
F5 Pb2 2.728(4) 2_665 ? 
O2 Pb1 2.553(6) 1_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 
F1 Pb1 F1 68.60(17) 2_566 . ? 
F1 Pb1 F2 67.02(14) 2_566 2_556 ? 
F1 Pb1 F2 135.28(14) . 2_556 ? 
F1 Pb1 O2 71.46(17) 2_566 1_455 ? 
F1 Pb1 O2 82.81(16) . 1_455 ? 
F2 Pb1 O2 78.43(16) 2_556 1_455 ? 
F1 Pb1 F4 76.57(15) 2_566 2_666 ? 
F1 Pb1 F4 78.21(15) . 2_666 ? 
F2 Pb1 F4 96.53(15) 2_556 2_666 ? 
O2 Pb1 F4 147.03(16) 1_455 2_666 ? 
F1 Pb1 F2 119.65(15) 2_566 . ? 
F1 Pb1 F2 140.99(15) . . ? 
F2 Pb1 F2 70.06(16) 2_556 . ? 
O2 Pb1 F2 136.08(15) 1_455 . ? 
F4 Pb1 F2 68.34(14) 2_666 . ? 
F1 Pb1 O1 140.15(17) 2_566 . ? 
F1 Pb1 O1 79.71(16) . . ? 
F2 Pb1 O1 135.58(16) 2_556 . ? 
O2 Pb1 O1 81.43(18) 1_455 . ? 
F4 Pb1 O1 120.67(16) 2_666 . ? 
F2 Pb1 O1 100.17(16) . . ? 
F1 Pb1 F3 124.16(15) 2_566 2 ? 
F1 Pb1 F3 140.15(15) . 2 ? 
F2 Pb1 F3 67.33(14) 2_556 2 ? 
O2 Pb1 F3 69.44(16) 1_455 2 ? 
F4 Pb1 F3 138.83(15) 2_666 2 ? 
F2 Pb1 F3 70.53(15) . 2 ? 
O1 Pb1 F3 68.61(15) . 2 ? 
F1 Pb2 F2 88.18(16) . 2_666 ? 
F1 Pb2 F2 68.71(15) . 1_565 ? 
F2 Pb2 F2 66.75(17) 2_666 1_565 ? 
F1 Pb2 F4 70.86(15) . . ? 
F2 Pb2 F4 71.62(15) 2_666 . ? 
F2 Pb2 F4 121.55(15) 1_565 . ? 
F1 Pb2 F5 109.31(14) . 2_665 ? 
F2 Pb2 F5 117.93(14) 2_666 2_665 ? 
F2 Pb2 F5 175.13(14) 1_565 2_665 ? 
F4 Pb2 F5 60.69(14) . 2_665 ? 
F1 Pb2 F3 133.78(15) . 2_665 ? 
F2 Pb2 F3 68.16(15) 2_666 2_665 ? 
F2 Pb2 F3 127.87(14) 1_565 2_665 ? 
F4 Pb2 F3 64.26(15) . 2_665 ? 
F5 Pb2 F3 56.81(13) 2_665 2_665 ? 
O2 V1 O1 104.0(3) . . ? 
O2 V1 F3 99.6(2) . . ? 
O1 V1 F3 94.8(2) . . ? 
O2 V1 F4 96.6(2) . . ? 
O1 V1 F4 90.6(2) . . ? 
F3 V1 F4 161.1(2) . . ? 
O2 V1 F5 99.5(2) . . ? 
O1 V1 F5 156.5(2) . . ? 
F3 V1 F5 83.2(2) . . ? 
F4 V1 F5 84.73(19) . . ? 
O2 V1 F5 171.3(2) . 2_665 ? 
O1 V1 F5 84.2(2) . 2_665 ? 
F3 V1 F5 82.39(19) . 2_665 ? 
F4 V1 F5 80.17(18) . 2_665 ? 
F5 V1 F5 72.3(2) . 2_665 ? 
Pb2 F1 Pb1 116.20(18) . 2_566 ? 
Pb2 F1 Pb1 131.15(19) . . ? 
Pb1 F1 Pb1 111.40(17) 2_566 . ? 
Pb2 F2 Pb2 113.25(17) 2_666 1_545 ? 
Pb2 F2 Pb1 103.89(17) 2_666 2_556 ? 
Pb2 F2 Pb1 104.05(15) 1_545 2_556 ? 
Pb2 F2 Pb1 111.14(16) 2_666 . ? 
Pb2 F2 Pb1 113.81(17) 1_545 . ? 
Pb1 F2 Pb1 109.94(16) 2_556 . ? 
V1 F3 Pb1 146.7(2) . 2 ? 
V1 F3 Pb2 109.3(2) . 2_665 ? 
Pb1 F3 Pb2 92.85(15) 2 2_665 ? 
V1 F4 Pb2 113.0(2) . . ? 
V1 F4 Pb1 138.0(2) . 2_666 ? 
Pb2 F4 Pb1 107.76(16) . 2_666 ? 
V1 F5 V1 107.7(2) . 2_665 ? 
V1 F5 Pb2 104.94(17) . 2_665 ? 
V1 F5 Pb2 98.44(17) 2_665 2_665 ? 
V1 O1 Pb1 119.0(3) . . ? 
V1 O2 Pb1 135.6(3) . 1_655 ? 
  
_refine_diff_density_max    5.627 
_refine_diff_density_min   -3.972 
_refine_diff_density_rms    0.565 

#===END

data_Pb2VOF6 
  
_audit_creation_method            SHELXL-2014/6 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'F6 O Pb2 V' 
_chemical_formula_sum 
 'F6 O Pb2 V' 
_chemical_formula_weight          595.32 
  
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' 
 'V'  'V'   0.3005   0.5294 
 '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' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            15 
_space_group_name_H-M_alt         'C 2/c' 
_space_group_name_Hall            '-C 2yc' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_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                    5.6675(4) 
_cell_length_b                    15.7931(12) 
_cell_length_c                    12.9995(9) 
_cell_angle_alpha                 90 
_cell_angle_beta                  92.019(2) 
_cell_angle_gamma                 90 
_cell_volume                      1162.83(15) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     7192 
_cell_measurement_theta_min       2.580 
_cell_measurement_theta_max       32.578 
  
_exptl_crystal_description        tablet 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     6.801 
_exptl_crystal_F_000              1992 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.100 
_exptl_crystal_size_mid           0.050 
_exptl_crystal_size_min           0.040 
_exptl_absorpt_coefficient_mu     59.401 
_shelx_estimated_absorpt_T_min    0.066 
_shelx_estimated_absorpt_T_max    0.200 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.1914 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'SADABS Version 2.05 (Bruker, 2001)' 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_source                    'sealed tube' 
_diffrn_measurement_device_type   'Bruker SMART APEX CCD diffractometer' 
_diffrn_measurement_method        'omega and phi scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             11443 
_diffrn_reflns_av_unetI/netI      0.0326 
_diffrn_reflns_av_R_equivalents   0.0423 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -23 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.579 
_diffrn_reflns_theta_max          32.578 
_diffrn_reflns_theta_full         25.242 
_diffrn_measured_fraction_theta_max   0.994 
_diffrn_measured_fraction_theta_full  0.999 
_diffrn_reflns_Laue_measured_fraction_max    0.994 
_diffrn_reflns_Laue_measured_fraction_full   0.999 
_diffrn_reflns_point_group_measured_fraction_max   0.994 
_diffrn_reflns_point_group_measured_fraction_full  0.999 
_reflns_number_total              2120 
_reflns_number_gt                 1963 
_reflns_threshold_expression      'I > 2σ(I)' 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'SMART Version 5.631 (Bruker, 2001)' 
_computing_cell_refinement        'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_data_reduction         'SAINT-Plus Version 6.45 (Bruker, 2001)' 
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)' 
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' 
_computing_molecular_graphics     various 
_computing_publication_material   various 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0242P)²+9.5236P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    . 
_refine_ls_hydrogen_treatment     undef 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00108(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2120 
_refine_ls_number_parameters      93 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0293 
_refine_ls_R_factor_gt            0.0260 
_refine_ls_wR_factor_ref          0.0577 
_refine_ls_wR_factor_gt           0.0564 
_refine_ls_goodness_of_fit_ref    1.096 
_refine_ls_restrained_S_all       1.096 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pb1 Pb 0.21077(4) 0.01143(2) 0.62502(2) 0.00942(7) Uani 1 1 d . . . . . 
Pb2 Pb 0.27257(4) 0.17245(2) 0.35773(2) 0.00933(7) Uani 1 1 d . . . . . 
V1 V 0.20791(18) 0.32501(6) 0.08999(8) 0.00929(19) Uani 1 1 d . . . . . 
F1 F 0.2520(7) 0.2288(2) 0.1785(3) 0.0152(7) Uani 1 1 d . . . . . 
F2 F -0.1078(7) 0.3339(2) 0.1311(3) 0.0142(7) Uani 1 1 d . . . . . 
F3 F 0.1095(6) 0.3952(2) -0.0271(3) 0.0127(7) Uani 1 1 d . . . . . 
F4 F 0.4590(6) 0.2755(2) 0.0098(3) 0.0119(7) Uani 1 1 d . . . . . 
F5 F 0.1209(6) 0.0568(2) 0.4514(3) 0.0124(7) Uani 1 1 d . . . . . 
F6 F 0.0000 0.0820(3) 0.2500 0.0122(9) Uani 1 2 d S T P . . 
F7 F 0.5000 0.0789(3) 0.2500 0.0127(10) Uani 1 2 d S T P . . 
O1 O 0.3447(8) 0.3972(3) 0.1574(3) 0.0122(8) 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 
Pb1 F5 2.356(4) 5_556 ? 
Pb1 F5 2.406(3) . ? 
Pb1 F3 2.474(3) 4_545 ? 
Pb1 F6 2.526(3) 5_556 ? 
Pb1 O1 2.574(4) 8_456 ? 
Pb1 F2 2.651(3) 8_556 ? 
Pb1 F7 2.679(3) 5_656 ? 
Pb1 Pb1 3.9820(5) 5_556 ? 
Pb1 Pb2 4.0039(4) 5_556 ? 
Pb2 F5 2.373(3) . ? 
Pb2 F7 2.435(3) . ? 
Pb2 F1 2.493(4) . ? 
Pb2 F6 2.497(3) . ? 
Pb2 F3 2.613(4) 8_556 ? 
Pb2 F2 2.720(3) 2 ? 
Pb2 F4 2.783(4) 2_655 ? 
Pb2 F4 2.826(3) 8_456 ? 
Pb2 F1 2.892(4) 2_655 ? 
Pb2 Pb2 3.8729(5) 2_655 ? 
V1 O1 1.619(4) . ? 
V1 F2 1.890(4) . ? 
V1 F1 1.917(4) . ? 
V1 F3 1.949(4) . ? 
V1 F4 1.957(4) . ? 
V1 F4 2.238(4) 7 ? 
F1 Pb2 2.892(4) 2_655 ? 
F2 Pb1 2.651(3) 8_455 ? 
F2 Pb2 2.721(3) 2 ? 
F3 Pb1 2.474(3) 4 ? 
F3 Pb2 2.613(4) 8_455 ? 
F4 V1 2.238(4) 7 ? 
F4 Pb2 2.783(4) 2_655 ? 
F4 Pb2 2.826(3) 8 ? 
F5 Pb1 2.356(3) 5_556 ? 
F6 Pb2 2.497(3) 2 ? 
F6 Pb1 2.526(3) 6 ? 
F6 Pb1 2.526(3) 5_556 ? 
F7 Pb2 2.435(3) 2_655 ? 
F7 Pb1 2.679(3) 6 ? 
F7 Pb1 2.679(3) 5_656 ? 
O1 Pb1 2.574(4) 8 ? 
  
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 
F5 Pb1 F5 66.50(14) 5_556 . ? 
F5 Pb1 F3 77.33(12) 5_556 4_545 ? 
F5 Pb1 F3 79.38(12) . 4_545 ? 
F5 Pb1 F6 67.39(9) 5_556 5_556 ? 
F5 Pb1 F6 133.49(8) . 5_556 ? 
F3 Pb1 F6 96.30(12) 4_545 5_556 ? 
F5 Pb1 O1 71.91(13) 5_556 8_456 ? 
F5 Pb1 O1 80.87(13) . 8_456 ? 
F3 Pb1 O1 148.12(13) 4_545 8_456 ? 
F6 Pb1 O1 79.66(12) 5_556 8_456 ? 
F5 Pb1 F2 137.48(12) 5_556 8_556 ? 
F5 Pb1 F2 79.79(12) . 8_556 ? 
F3 Pb1 F2 122.22(12) 4_545 8_556 ? 
F6 Pb1 F2 135.32(12) 5_556 8_556 ? 
O1 Pb1 F2 78.02(13) 8_456 8_556 ? 
F5 Pb1 F7 118.31(12) 5_556 5_656 ? 
F5 Pb1 F7 146.36(9) . 5_656 ? 
F3 Pb1 F7 70.26(11) 4_545 5_656 ? 
F6 Pb1 F7 65.91(5) 5_556 5_656 ? 
O1 Pb1 F7 132.78(10) 8_456 5_656 ? 
F2 Pb1 F7 104.15(12) 8_556 5_656 ? 
F5 Pb1 Pb1 33.64(8) 5_556 5_556 ? 
F5 Pb1 Pb1 32.85(8) . 5_556 ? 
F3 Pb1 Pb1 76.05(9) 4_545 5_556 ? 
F6 Pb1 Pb1 100.85(2) 5_556 5_556 ? 
O1 Pb1 Pb1 73.76(10) 8_456 5_556 ? 
F2 Pb1 Pb1 109.20(9) 8_556 5_556 ? 
F7 Pb1 Pb1 141.58(9) 5_656 5_556 ? 
F5 Pb1 Pb2 32.28(8) 5_556 5_556 ? 
F5 Pb1 Pb2 98.39(8) . 5_556 ? 
F3 Pb1 Pb2 77.61(8) 4_545 5_556 ? 
F6 Pb1 Pb2 36.90(5) 5_556 5_556 ? 
O1 Pb1 Pb2 80.83(10) 8_456 5_556 ? 
F2 Pb1 Pb2 158.79(8) 8_556 5_556 ? 
F7 Pb1 Pb2 89.13(8) 5_656 5_556 ? 
Pb1 Pb1 Pb2 65.667(7) 5_556 5_556 ? 
F5 Pb2 F7 92.10(13) . . ? 
F5 Pb2 F1 138.44(12) . . ? 
F7 Pb2 F1 71.77(11) . . ? 
F5 Pb2 F6 67.63(11) . . ? 
F7 Pb2 F6 70.13(6) . . ? 
F1 Pb2 F6 70.86(11) . . ? 
F5 Pb2 F3 70.25(11) . 8_556 ? 
F7 Pb2 F3 71.97(8) . 8_556 ? 
F1 Pb2 F3 133.67(12) . 8_556 ? 
F6 Pb2 F3 120.85(12) . 8_556 ? 
F5 Pb2 F2 124.25(12) . 2 ? 
F7 Pb2 F2 142.05(12) . 2 ? 
F1 Pb2 F2 73.18(12) . 2 ? 
F6 Pb2 F2 111.04(12) . 2 ? 
F3 Pb2 F2 126.72(12) 8_556 2 ? 
F5 Pb2 F4 109.43(11) . 2_655 ? 
F7 Pb2 F4 114.95(8) . 2_655 ? 
F1 Pb2 F4 112.11(12) . 2_655 ? 
F6 Pb2 F4 174.55(7) . 2_655 ? 
F3 Pb2 F4 60.79(10) 8_556 2_655 ? 
F2 Pb2 F4 66.44(11) 2 2_655 ? 
F5 Pb2 F4 67.49(11) . 8_456 ? 
F7 Pb2 F4 159.57(12) . 8_456 ? 
F1 Pb2 F4 122.68(11) . 8_456 ? 
F6 Pb2 F4 99.59(8) . 8_456 ? 
F3 Pb2 F4 100.56(10) 8_556 8_456 ? 
F2 Pb2 F4 57.64(11) 2 8_456 ? 
F4 Pb2 F4 74.97(11) 2_655 8_456 ? 
F5 Pb2 F1 132.58(12) . 2_655 ? 
F7 Pb2 F1 65.02(10) . 2_655 ? 
F1 Pb2 F1 75.60(14) . 2_655 ? 
F6 Pb2 F1 130.25(7) . 2_655 ? 
F3 Pb2 F1 63.42(11) 8_556 2_655 ? 
F2 Pb2 F1 92.53(11) 2 2_655 ? 
F4 Pb2 F1 55.17(10) 2_655 2_655 ? 
F4 Pb2 F1 129.57(10) 8_456 2_655 ? 
F5 Pb2 Pb2 129.29(9) . 2_655 ? 
F7 Pb2 Pb2 37.33(9) . 2_655 ? 
F1 Pb2 Pb2 48.28(9) . 2_655 ? 
F6 Pb2 Pb2 90.503(8) . 2_655 ? 
F3 Pb2 Pb2 85.56(8) 8_556 2_655 ? 
F2 Pb2 Pb2 106.08(8) 2 2_655 ? 
F4 Pb2 Pb2 94.84(7) 2_655 2_655 ? 
F4 Pb2 Pb2 163.08(7) 8_456 2_655 ? 
F1 Pb2 Pb2 40.04(7) 2_655 2_655 ? 
O1 V1 F2 103.6(2) . . ? 
O1 V1 F1 100.6(2) . . ? 
F2 V1 F1 89.63(16) . . ? 
O1 V1 F3 98.10(19) . . ? 
F2 V1 F3 86.06(16) . . ? 
F1 V1 F3 161.32(17) . . ? 
O1 V1 F4 103.1(2) . . ? 
F2 V1 F4 153.33(16) . . ? 
F1 V1 F4 85.49(16) . . ? 
F3 V1 F4 90.23(16) . . ? 
O1 V1 F4 176.02(19) . 7 ? 
F2 V1 F4 80.29(15) . 7 ? 
F1 V1 F4 80.15(15) . 7 ? 
F3 V1 F4 81.21(14) . 7 ? 
F4 V1 F4 73.04(16) . 7 ? 
V1 F1 Pb2 147.62(19) . . ? 
V1 F1 Pb2 104.38(15) . 2_655 ? 
Pb2 F1 Pb2 91.68(11) . 2_655 ? 
V1 F2 Pb1 115.45(16) . 8_455 ? 
V1 F2 Pb2 106.02(15) . 2 ? 
Pb1 F2 Pb2 137.02(16) 8_455 2 ? 
V1 F3 Pb1 135.42(18) . 4 ? 
V1 F3 Pb2 113.48(15) . 8_455 ? 
Pb1 F3 Pb2 108.34(13) 4 8_455 ? 
V1 F4 V1 106.96(16) . 7 ? 
V1 F4 Pb2 107.19(14) . 2_655 ? 
V1 F4 Pb2 98.89(13) 7 2_655 ? 
V1 F4 Pb2 138.04(17) . 8 ? 
V1 F4 Pb2 93.70(12) 7 8 ? 
Pb2 F4 Pb2 105.03(11) 2_655 8 ? 
Pb1 F5 Pb2 115.71(14) 5_556 . ? 
Pb1 F5 Pb1 113.50(14) 5_556 . ? 
Pb2 F5 Pb1 129.95(15) . . ? 
Pb2 F6 Pb2 110.23(19) . 2 ? 
Pb2 F6 Pb1 113.432(8) . 6 ? 
Pb2 F6 Pb1 105.705(9) 2 6 ? 
Pb2 F6 Pb1 105.705(9) . 5_556 ? 
Pb2 F6 Pb1 113.431(9) 2 5_556 ? 
Pb1 F6 Pb1 108.49(18) 6 5_556 ? 
Pb2 F7 Pb2 105.34(19) 2_655 . ? 
Pb2 F7 Pb1 107.415(11) 2_655 6 ? 
Pb2 F7 Pb1 110.298(11) . 6 ? 
Pb2 F7 Pb1 110.298(11) 2_655 5_656 ? 
Pb2 F7 Pb1 107.415(11) . 5_656 ? 
Pb1 F7 Pb1 115.61(18) 6 5_656 ? 
V1 O1 Pb1 132.8(2) . 8 ? 
  
_refine_diff_density_max    3.405 
_refine_diff_density_min   -1.646 
_refine_diff_density_rms    0.406 
