#------------------------------------------------------------------------------
#$Date: 2015-03-02 10:37:44 +0000 (Mon, 02 Mar 2015) $
#$Revision: 132591 $
#$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500022.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_3500022
loop_
_publ_author_name
'Armel Le Bail'
_publ_section_title
;
 Crystal structure of Pb3FeF9.H2O
;
_journal_name_full               'Personal communication to COD'
_journal_year                    2015
_chemical_formula_sum            'F9 Fe H2 O Pb3'
_chemical_formula_weight         866.50
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.28(3)
_cell_angle_beta                 94.04(3)
_cell_angle_gamma                90.83(3)
_cell_formula_units_Z            2
_cell_length_a                   5.754(3)
_cell_length_b                   5.939(3)
_cell_length_c                   12.786(6)
_cell_measurement_temperature    293(2)
_cell_volume                     431.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.662
_diffrn_measured_fraction_theta_max 0.662
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1237
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2995
_diffrn_reflns_theta_full        37.49
_diffrn_reflns_theta_max         37.49
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    60.609
_exptl_crystal_density_diffrn    6.674
_exptl_crystal_F_000             730
_exptl_special_details
;
This fluorite-related Pb3FeF9(H2O) crystal structure is solved from a twinned 
crystal. It is found to be isostructural with one (MDO2) of the polytypes of 
the mineral aravaipaite Pb3AlF9(H2O). 

Synthesized during investigations of the PbF2/FeF3/HFaq systems (HF 5M) by 
hydrothermal synthesis (473 K). 

Extremely thin pale-pink platelet-shaped single crystals. 
;
_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. 
;
_refine_diff_density_max         4.796
_refine_diff_density_min         -4.614
_refine_diff_density_rms         0.801
_refine_ls_extinction_coef       0.0012(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1944
_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. 
;
_reflns_number_gt                1968
_reflns_number_total             2995
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    Pb3FrF9-H2O.cif
_[local]_cod_data_source_block   Pb3FeF9-H2O
_[local]_cod_chemical_formula_sum_orig 'H2 F9 Fe O Pb3'
_cod_database_code               3500022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pb1 Pb 0.30347(12) 0.11129(11) 0.36130(5) 0.01020(16) Uani 1 1 d .
Pb2 Pb 0.7701(3) 0.04982(14) 0.11554(7) 0.0327(3) Uani 1 1 d .
Pb3 Pb 0.27697(14) 0.50794(12) 0.11342(6) 0.01481(18) Uani 1 1 d .
Fe Fe 0.7892(5) 0.6126(4) 0.3107(2) 0.0087(4) Uani 1 1 d .
F1 F 0.058(3) 0.773(2) 0.2689(13) 0.023(3) Uiso 1 1 d .
F2 F 0.723(3) 0.488(2) 0.1599(12) 0.023(3) Uiso 1 1 d .
F3 F 0.855(4) 0.723(3) 0.4567(17) 0.040(4) Uiso 1 1 d .
F4 F 0.497(3) 0.476(2) 0.3317(12) 0.020(2) Uiso 1 1 d .
F5 F 0.606(3) 0.874(2) 0.2789(13) 0.026(3) Uiso 1 1 d .
F6 F 0.946(3) 0.339(3) 0.3219(14) 0.028(3) Uiso 1 1 d .
F7 F 0.502(3) 0.241(2) 0.9919(10) 0.017(2) Uiso 1 1 d .
F8 F -0.001(3) 0.250(2) 0.9940(11) 0.018(2) Uiso 1 1 d .
F9 F 0.281(4) 0.137(3) 0.1706(16) 0.035(4) Uiso 1 1 d .
OW O 0.669(3) 0.216(3) 0.5099(14) 0.019(3) Uiso 1 1 d D
H1 H 0.65(5) 0.29(6) 0.575(13) 0.050 Uiso 1 1 d D
H2 H 0.81(3) 0.23(6) 0.49(3) 0.050 Uiso 1 1 d D
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0069(3) 0.0126(3) 0.0111(2) 0.0020(2) -0.00005(18) 0.00119(19)
Pb2 0.0699(9) 0.0145(3) 0.0131(3) 0.0017(3) 0.0005(4) -0.0068(4)
Pb3 0.0141(4) 0.0169(3) 0.0132(3) 0.0010(2) 0.0024(2) 0.0000(2)
Fe 0.0040(10) 0.0114(8) 0.0096(9) -0.0010(8) -0.0022(7) 0.0024(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -4.1330 10.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3010 0.8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
F5 Pb1 F9 71.2(6) 1_545 .
F5 Pb1 F4 93.4(5) 1_545 .
F9 Pb1 F4 70.5(5) . .
F5 Pb1 F1 79.5(6) 1_545 1_545
F9 Pb1 F1 73.0(6) . 1_545
F4 Pb1 F1 143.1(5) . 1_545
F5 Pb1 F6 143.7(5) 1_545 1_455
F9 Pb1 F6 73.0(6) . 1_455
F4 Pb1 F6 80.2(5) . 1_455
F1 Pb1 F6 84.5(5) 1_545 1_455
F5 Pb1 F3 143.8(7) 1_545 2_666
F9 Pb1 F3 144.5(7) . 2_666
F4 Pb1 F3 95.5(5) . 2_666
F1 Pb1 F3 111.6(6) 1_545 2_666
F6 Pb1 F3 72.5(7) 1_455 2_666
F5 Pb1 OW 79.8(5) 1_545 2_656
F9 Pb1 OW 138.4(5) . 2_656
F4 Pb1 OW 141.8(5) . 2_656
F1 Pb1 OW 73.0(5) 1_545 2_656
F6 Pb1 OW 126.0(5) 1_455 2_656
F3 Pb1 OW 71.6(6) 2_666 2_656
F5 Pb1 OW 79.6(6) 1_545 .
F9 Pb1 OW 129.3(6) . .
F4 Pb1 OW 71.0(5) . .
F1 Pb1 OW 140.7(5) 1_545 .
F6 Pb1 OW 129.8(5) 1_455 .
F3 Pb1 OW 70.5(7) 2_666 .
OW Pb1 OW 70.9(6) 2_656 .
F7 Pb2 F8 109.7(4) 2_656 1_654
F7 Pb2 F7 70.4(4) 2_656 1_554
F8 Pb2 F7 69.0(5) 1_654 1_554
F7 Pb2 F8 70.0(5) 2_656 2_656
F8 Pb2 F8 72.4(4) 1_654 2_656
F7 Pb2 F8 108.9(4) 1_554 2_656
F7 Pb2 F2 129.0(5) 2_656 .
F8 Pb2 F2 70.3(5) 1_654 .
F7 Pb2 F2 62.2(5) 1_554 .
F8 Pb2 F2 142.3(5) 2_656 .
F7 Pb2 F5 83.0(5) 2_656 1_545
F8 Pb2 F5 166.6(5) 1_654 1_545
F7 Pb2 F5 121.0(5) 1_554 1_545
F8 Pb2 F5 109.5(4) 2_656 1_545
F2 Pb2 F5 105.4(5) . 1_545
F7 Pb2 F9 69.8(5) 2_656 .
F8 Pb2 F9 127.1(5) 1_654 .
F7 Pb2 F9 61.2(5) 1_554 .
F8 Pb2 F9 139.4(5) 2_656 .
F2 Pb2 F9 71.8(5) . .
F5 Pb2 F9 60.4(5) 1_545 .
F7 Pb2 F9 140.0(5) 2_656 1_655
F8 Pb2 F9 61.6(5) 1_654 1_655
F7 Pb2 F9 128.3(5) 1_554 1_655
F8 Pb2 F9 70.3(5) 2_656 1_655
F2 Pb2 F9 86.9(5) . 1_655
F5 Pb2 F9 106.0(5) 1_545 1_655
F9 Pb2 F9 148.6(7) . 1_655
F9 Pb3 F8 71.2(6) . 1_554
F9 Pb3 F7 70.3(6) . 1_554
F8 Pb3 F7 71.2(5) 1_554 1_554
F9 Pb3 F7 142.3(6) . 2_666
F8 Pb3 F7 110.3(4) 1_554 2_666
F7 Pb3 F7 74.7(4) 1_554 2_666
F9 Pb3 F2 81.7(6) . .
F8 Pb3 F2 132.1(5) 1_554 .
F7 Pb3 F2 62.6(5) 1_554 .
F7 Pb3 F2 69.9(5) 2_666 .
F9 Pb3 F8 139.0(6) . 2_566
F8 Pb3 F8 70.9(5) 1_554 2_566
F7 Pb3 F8 110.8(4) 1_554 2_566
F7 Pb3 F8 67.5(5) 2_666 2_566
F2 Pb3 F8 136.9(4) . 2_566
F9 Pb3 F1 103.6(6) . .
F8 Pb3 F1 112.1(5) 1_554 .
F7 Pb3 F1 172.1(4) 1_554 .
F7 Pb3 F1 109.8(4) 2_666 .
F2 Pb3 F1 112.3(5) . .
F8 Pb3 F1 77.1(4) 2_566 .
F9 Pb3 F4 62.6(5) . .
F8 Pb3 F4 131.5(4) 1_554 .
F7 Pb3 F4 104.5(4) 1_554 .
F7 Pb3 F4 114.9(4) 2_666 .
F2 Pb3 F4 55.5(5) . .
F8 Pb3 F4 143.5(4) 2_566 .
F1 Pb3 F4 67.8(4) . .
F6 Fe F3 92.6(8) . .
F6 Fe F4 91.8(7) . .
F3 Fe F4 93.8(8) . .
F6 Fe F1 95.2(7) . 1_655
F3 Fe F1 93.1(8) . 1_655
F4 Fe F1 170.0(7) . 1_655
F6 Fe F5 171.5(7) . .
F3 Fe F5 95.6(8) . .
F4 Fe F5 85.5(7) . .
F1 Fe F5 86.6(7) 1_655 .
F6 Fe F2 85.8(7) . .
F3 Fe F2 178.2(7) . .
F4 Fe F2 85.7(7) . .
F1 Fe F2 87.7(7) 1_655 .
F5 Fe F2 86.1(7) . .
Fe F1 Pb1 132.1(8) 1_455 1_565
Fe F1 F5 46.9(5) 1_455 1_455
Pb1 F1 F5 108.7(6) 1_565 1_455
Fe F1 F2 46.5(5) 1_455 1_455
Pb1 F1 F2 166.3(8) 1_565 1_455
F5 F1 F2 59.6(6) 1_455 1_455
Fe F1 Pb3 111.3(6) 1_455 .
Pb1 F1 Pb3 113.8(6) 1_565 .
F5 F1 Pb3 129.8(7) 1_455 .
F2 F1 Pb3 74.1(5) 1_455 .
Fe F1 F3 42.7(6) 1_455 1_455
Pb1 F1 F3 91.3(7) 1_565 1_455
F5 F1 F3 62.9(7) 1_455 1_455
F2 F1 F3 89.1(7) 1_455 1_455
Pb3 F1 F3 138.3(7) . 1_455
Fe F1 F6 41.6(5) 1_455 1_455
Pb1 F1 F6 134.0(7) 1_565 1_455
F5 F1 F6 88.2(7) 1_455 1_455
F2 F1 F6 56.5(6) 1_455 1_455
Pb3 F1 F6 81.2(5) . 1_455
F3 F1 F6 58.1(6) 1_455 1_455
Fe F1 F9 153.2(9) 1_455 1_565
Pb1 F1 F9 52.3(5) 1_565 1_565
F5 F1 F9 106.8(7) 1_455 1_565
F2 F1 F9 121.4(8) 1_455 1_565
Pb3 F1 F9 80.6(6) . 1_565
F3 F1 F9 138.7(8) 1_455 1_565
F6 F1 F9 161.3(8) 1_455 1_565
Fe F1 OW 93.1(6) 1_455 2_666
Pb1 F1 OW 56.3(4) 1_565 2_666
F5 F1 OW 114.2(8) 1_455 2_666
F2 F1 OW 133.1(7) 1_455 2_666
Pb3 F1 OW 111.1(6) . 2_666
F3 F1 OW 55.1(7) 1_455 2_666
F6 F1 OW 77.8(6) 1_455 2_666
F9 F1 OW 105.2(7) 1_565 2_666
Fe F2 Pb3 108.4(7) . .
Fe F2 Pb2 114.7(6) . .
Pb3 F2 Pb2 99.1(5) . .
Fe F2 F6 45.8(5) . .
Pb3 F2 F6 129.5(7) . .
Pb2 F2 F6 70.9(5) . .
Fe F2 F4 46.1(5) . .
Pb3 F2 F4 70.3(5) . .
Pb2 F2 F4 96.2(5) . .
F6 F2 F4 62.3(6) . .
Fe F2 F7 157.4(8) . 1_554
Pb3 F2 F7 56.8(5) . 1_554
Pb2 F2 F7 57.5(4) . 1_554
F6 F2 F7 127.3(7) . 1_554
F4 F2 F7 111.5(7) . 1_554
Fe F2 F5 46.8(5) . .
Pb3 F2 F5 76.8(6) . .
Pb2 F2 F5 155.2(7) . .
F6 F2 F5 92.6(7) . .
F4 F2 F5 59.2(6) . .
F7 F2 F5 131.2(9) 1_554 .
Fe F2 F1 45.9(5) . 1_655
Pb3 F2 F1 135.8(7) . 1_655
Pb2 F2 F1 123.4(7) . 1_655
F6 F2 F1 64.1(6) . 1_655
F4 F2 F1 91.7(7) . 1_655
F7 F2 F1 156.8(8) 1_554 1_655
F5 F2 F1 59.6(6) . 1_655
Fe F2 F7 121.7(7) . 2_666
Pb3 F2 F7 54.0(4) . 2_666
Pb2 F2 F7 122.5(6) . 2_666
F6 F2 F7 166.6(7) . 2_666
F4 F2 F7 114.1(7) . 2_666
F7 F2 F7 66.0(6) 1_554 2_666
F5 F2 F7 75.3(6) . 2_666
F1 F2 F7 104.1(6) 1_655 2_666
Fe F2 F8 134.5(8) . 1_654
Pb3 F2 F8 116.7(6) . 1_654
Pb2 F2 F8 53.5(4) . 1_654
F6 F2 F8 97.0(7) . 1_654
F4 F2 F8 149.0(7) . 1_654
F7 F2 F8 61.1(5) 1_554 1_654
F5 F2 F8 150.0(7) . 1_654
F1 F2 F8 99.6(7) 1_655 1_654
F7 F2 F8 91.1(6) 2_666 1_654
Fe F3 Pb1 148.1(13) . 2_666
Fe F3 F6 43.6(6) . .
Pb1 F3 F6 146.1(8) 2_666 .
Fe F3 OW 107.1(10) . 2_766
Pb1 F3 OW 104.3(9) 2_666 2_766
F6 F3 OW 86.1(8) . 2_766
Fe F3 F4 43.3(6) . .
Pb1 F3 F4 108.6(9) 2_666 .
F6 F3 F4 59.3(7) . .
OW F3 F4 144.7(9) 2_766 .
Fe F3 F1 44.2(6) . 1_655
Pb1 F3 F1 152.2(8) 2_666 1_655
F6 F3 F1 61.7(6) . 1_655
OW F3 F1 68.6(7) 2_766 1_655
F4 F3 F1 87.3(8) . 1_655
Fe F3 F5 43.1(6) . .
Pb1 F3 F5 113.3(9) 2_666 .
F6 F3 F5 86.7(8) . .
OW F3 F5 120.9(9) 2_766 .
F4 F3 F5 55.6(6) . .
F1 F3 F5 56.7(7) 1_655 .
Fe F3 F6 151.1(10) . 2_766
Pb1 F3 F6 52.5(5) 2_666 2_766
F6 F3 F6 107.6(8) . 2_766
OW F3 F6 65.2(7) 2_766 2_766
F4 F3 F6 128.5(8) . 2_766
F1 F3 F6 133.3(10) 1_655 2_766
F5 F3 F6 165.3(9) . 2_766
Fe F3 OW 91.7(10) . 2_666
Pb1 F3 OW 56.4(5) 2_666 2_666
F6 F3 OW 113.7(9) . 2_666
OW F3 OW 159.5(10) 2_766 2_666
F4 F3 OW 55.8(6) . 2_666
F1 F3 OW 124.4(9) 1_655 2_666
F5 F3 OW 67.9(7) . 2_666
F6 F3 OW 102.0(8) 2_766 2_666
Fe F3 OW 110.3(9) . 1_565
Pb1 F3 OW 55.6(5) 2_666 1_565
F6 F3 OW 153.8(10) . 1_565
OW F3 OW 103.5(8) 2_766 1_565
F4 F3 OW 105.4(9) . 1_565
F1 F3 OW 98.7(7) 1_655 1_565
F5 F3 OW 67.3(6) . 1_565
F6 F3 OW 98.6(7) 2_766 1_565
OW F3 OW 61.1(7) 2_666 1_565
Fe F4 Pb1 143.6(7) . .
Fe F4 F5 48.1(5) . .
Pb1 F4 F5 166.8(8) . .
Fe F4 F2 48.2(5) . .
Pb1 F4 F2 119.7(6) . .
F5 F4 F2 61.3(6) . .
Fe F4 F6 43.9(5) . .
Pb1 F4 F6 99.7(6) . .
F5 F4 F6 91.7(7) . .
F2 F4 F6 58.7(6) . .
Fe F4 OW 102.3(7) . 2_666
Pb1 F4 OW 101.8(6) . 2_666
F5 F4 OW 76.2(6) . 2_666
F2 F4 OW 137.6(7) . 2_666
F6 F4 OW 125.8(8) . 2_666
Fe F4 F3 42.9(5) . .
Pb1 F4 F3 127.9(7) . .
F5 F4 F3 63.8(6) . .
F2 F4 F3 91.1(7) . .
F6 F4 F3 59.6(7) . .
OW F4 F3 67.9(7) 2_666 .
Fe F4 F9 119.8(8) . .
Pb1 F4 F9 53.9(5) . .
F5 F4 F9 118.2(7) . .
F2 F4 F9 73.2(6) . .
F6 F4 F9 98.5(7) . .
OW F4 F9 134.0(8) 2_666 .
F3 F4 F9 157.9(9) . .
Fe F4 Pb3 95.8(5) . .
Pb1 F4 Pb3 98.8(5) . .
F5 F4 Pb3 70.8(5) . .
F2 F4 Pb3 54.3(5) . .
F6 F4 Pb3 110.9(6) . .
OW F4 Pb3 114.1(6) 2_666 .
F3 F4 Pb3 132.7(6) . .
F9 F4 Pb3 48.5(4) . .
Fe F4 OW 97.5(7) . .
Pb1 F4 OW 57.9(4) . .
F5 F4 OW 134.0(7) . .
F2 F4 OW 122.9(7) . .
F6 F4 OW 65.6(6) . .
OW F4 OW 85.5(6) 2_666 .
F3 F4 OW 70.3(6) . .
F9 F4 OW 104.9(6) . .
Pb3 F4 OW 153.3(6) . .
Fe F5 Pb1 137.0(8) . 1_565
Fe F5 F4 46.3(5) . .
Pb1 F5 F4 100.9(7) 1_565 .
Fe F5 Pb2 110.8(7) . 1_565
Pb1 F5 Pb2 111.6(6) 1_565 1_565
F4 F5 Pb2 139.6(7) . 1_565
Fe F5 F1 46.5(5) . 1_655
Pb1 F5 F1 149.3(8) 1_565 1_655
F4 F5 F1 92.7(7) . 1_655
Pb2 F5 F1 71.5(6) 1_565 1_655
Fe F5 F2 47.1(5) . .
Pb1 F5 F2 149.0(8) 1_565 .
F4 F5 F2 59.5(5) . .
Pb2 F5 F2 80.6(6) 1_565 .
F1 F5 F2 60.8(6) 1_655 .
Fe F5 F9 159.5(9) . 1_565
Pb1 F5 F9 54.5(5) 1_565 1_565
F4 F5 F9 122.9(9) . 1_565
Pb2 F5 F9 64.9(5) 1_565 1_565
F1 F5 F9 136.3(8) 1_655 1_565
F2 F5 F9 113.4(8) . 1_565
Fe F5 F3 41.3(5) . .
Pb1 F5 F3 102.8(8) 1_565 .
F4 F5 F3 60.6(6) . .
Pb2 F5 F3 129.6(9) 1_565 .
F1 F5 F3 60.4(7) 1_655 .
F2 F5 F3 88.4(7) . .
F9 F5 F3 156.9(9) 1_565 .
Fe F6 Pb1 153.3(9) . 1_655
Fe F6 F2 48.4(5) . .
Pb1 F6 F2 139.2(8) 1_655 .
Fe F6 F4 44.4(5) . .
Pb1 F6 F4 157.5(8) 1_655 .
F2 F6 F4 59.0(6) . .
Fe F6 F3 43.8(6) . .
Pb1 F6 F3 119.7(9) 1_655 .
F2 F6 F3 92.3(8) . .
F4 F6 F3 61.1(7) . .
Fe F6 F1 43.3(5) . 1_655
Pb1 F6 F1 112.9(7) 1_655 1_655
F2 F6 F1 59.5(6) . 1_655
F4 F6 F1 87.4(6) . 1_655
F3 F6 F1 60.2(6) . 1_655
Fe F6 F9 124.1(8) . 1_655
Pb1 F6 F9 52.3(5) 1_655 1_655
F2 F6 F9 86.9(7) . 1_655
F4 F6 F9 142.1(9) . 1_655
F3 F6 F9 143.4(9) . 1_655
F1 F6 F9 88.8(7) 1_655 1_655
Fe F6 F3 116.2(8) . 2_766
Pb1 F6 F3 55.0(5) 1_655 2_766
F2 F6 F3 164.5(8) . 2_766
F4 F6 F3 109.4(8) . 2_766
F3 F6 F3 72.4(8) . 2_766
F1 F6 F3 112.6(7) 1_655 2_766
F9 F6 F3 106.9(8) 1_655 2_766
Pb3 F7 Pb2 109.5(6) 1_556 2_656
Pb3 F7 Pb2 104.0(5) 1_556 1_556
Pb2 F7 Pb2 109.6(4) 2_656 1_556
Pb3 F7 Pb3 105.3(4) 1_556 2_666
Pb2 F7 Pb3 115.4(5) 2_656 2_666
Pb2 F7 Pb3 112.3(6) 1_556 2_666
Pb3 F7 F2 60.6(5) 1_556 1_556
Pb2 F7 F2 159.7(7) 2_656 1_556
Pb2 F7 F2 60.3(4) 1_556 1_556
Pb3 F7 F2 84.9(5) 2_666 1_556
Pb3 F7 F9 53.6(4) 1_556 1_556
Pb2 F7 F9 86.3(6) 2_656 1_556
Pb2 F7 F9 67.3(5) 1_556 1_556
Pb3 F7 F9 155.3(6) 2_666 1_556
F2 F7 F9 73.6(6) 1_556 1_556
Pb3 F7 F8 123.8(6) 1_556 1_655
Pb2 F7 F8 126.4(6) 2_656 1_655
Pb2 F7 F8 55.4(4) 1_556 1_655
Pb3 F7 F8 57.5(4) 2_666 1_655
F2 F7 F8 64.6(6) 1_556 1_655
F9 F7 F8 120.1(7) 1_556 1_655
Pb3 F7 F8 54.1(4) 1_556 .
Pb2 F7 F8 55.8(4) 2_656 .
Pb2 F7 F8 125.1(6) 1_556 .
Pb3 F7 F8 121.6(6) 2_666 .
F2 F7 F8 113.5(7) 1_556 .
F9 F7 F8 59.7(6) 1_556 .
F8 F7 F8 177.8(8) 1_655 .
Pb3 F7 F7 120.0(7) 1_556 2_657
Pb2 F7 F7 55.2(4) 2_656 2_657
Pb2 F7 F7 54.4(4) 1_556 2_657
Pb3 F7 F7 134.5(8) 2_666 2_657
F2 F7 F7 112.2(8) 1_556 2_657
F9 F7 F7 66.9(6) 1_556 2_657
F8 F7 F7 90.9(7) 1_655 2_657
F8 F7 F7 90.9(7) . 2_657
Pb3 F7 F2 79.6(5) 1_556 2_666
Pb2 F7 F2 78.9(5) 2_656 2_666
Pb2 F7 F2 168.4(7) 1_556 2_666
Pb3 F7 F2 56.2(4) 2_666 2_666
F2 F7 F2 114.0(6) 1_556 2_666
F9 F7 F2 122.2(7) 1_556 2_666
F8 F7 F2 113.4(6) 1_655 2_666
F8 F7 F2 66.0(5) . 2_666
F7 F7 F2 133.5(8) 2_657 2_666
Pb3 F7 F7 53.1(4) 1_556 2_667
Pb2 F7 F7 129.0(8) 2_656 2_667
Pb2 F7 F7 120.9(7) 1_556 2_667
Pb3 F7 F7 52.1(4) 2_666 2_667
F2 F7 F7 61.6(5) 1_556 2_667
F9 F7 F7 105.5(7) 1_556 2_667
F8 F7 F7 90.6(7) 1_655 2_667
F8 F7 F7 87.4(7) . 2_667
F7 F7 F7 171.9(10) 2_657 2_667
F2 F7 F7 52.5(5) 2_666 2_667
Pb3 F8 Pb2 105.0(5) 1_556 1_456
Pb3 F8 Pb2 108.7(6) 1_556 2_656
Pb2 F8 Pb2 107.6(4) 1_456 2_656
Pb3 F8 Pb3 109.1(5) 1_556 2_566
Pb2 F8 Pb3 110.1(6) 1_456 2_566
Pb2 F8 Pb3 115.9(5) 2_656 2_566
Pb3 F8 F9 53.5(5) 1_556 1_556
Pb2 F8 F9 67.5(5) 1_456 1_556
Pb2 F8 F9 85.0(6) 2_656 1_556
Pb3 F8 F9 157.8(7) 2_566 1_556
Pb3 F8 F7 127.4(6) 1_556 1_455
Pb2 F8 F7 55.6(4) 1_456 1_455
Pb2 F8 F7 123.6(6) 2_656 1_455
Pb3 F8 F7 54.9(4) 2_566 1_455
F9 F8 F7 121.1(7) 1_556 1_455
Pb3 F8 F7 54.7(4) 1_556 .
Pb2 F8 F7 123.8(6) 1_456 .
Pb2 F8 F7 54.2(4) 2_656 .
Pb3 F8 F7 125.9(6) 2_566 .
F9 F8 F7 59.0(6) 1_556 .
F7 F8 F7 177.8(7) 1_455 .
Pb3 F8 F2 74.0(5) 1_556 1_456
Pb2 F8 F2 56.2(4) 1_456 1_456
Pb2 F8 F2 162.9(6) 2_656 1_456
Pb3 F8 F2 77.7(5) 2_566 1_456
F9 F8 F2 83.4(7) 1_556 1_456
F7 F8 F2 54.3(5) 1_455 1_456
F7 F8 F2 127.6(7) . 1_456
Pb3 F8 F8 56.7(5) 1_556 2_567
Pb2 F8 F8 121.4(8) 1_456 2_567
Pb2 F8 F8 130.9(8) 2_656 2_567
Pb3 F8 F8 52.5(4) 2_566 2_567
F9 F8 F8 108.6(8) 1_556 2_567
F7 F8 F8 90.1(7) 1_455 2_567
F7 F8 F8 91.9(7) . 2_567
F2 F8 F8 65.2(6) 1_456 2_567
Pb3 F8 F8 119.3(8) 1_556 2_557
Pb2 F8 F8 54.3(4) 1_456 2_557
Pb2 F8 F8 53.3(4) 2_656 2_557
Pb3 F8 F8 131.3(8) 2_566 2_557
F9 F8 F8 66.6(6) 1_556 2_557
F7 F8 F8 89.8(7) 1_455 2_557
F7 F8 F8 88.3(7) . 2_557
F2 F8 F8 110.2(7) 1_456 2_557
F8 F8 F8 174.2(11) 2_567 2_557
Pb3 F9 Pb1 119.1(7) . .
Pb3 F9 F7 56.1(5) . 1_554
Pb1 F9 F7 149.0(10) . 1_554
Pb3 F9 F8 55.3(5) . 1_554
Pb1 F9 F8 145.9(10) . 1_554
F7 F9 F8 61.3(6) 1_554 1_554
Pb3 F9 F5 136.9(9) . 1_545
Pb1 F9 F5 54.4(5) . 1_545
F7 F9 F5 105.8(8) 1_554 1_545
F8 F9 F5 155.9(9) 1_554 1_545
Pb3 F9 F4 68.9(5) . .
Pb1 F9 F4 55.6(5) . .
F7 F9 F4 100.1(7) 1_554 .
F8 F9 F4 122.4(7) 1_554 .
F5 F9 F4 78.3(7) 1_545 .
Pb3 F9 F1 151.2(10) . 1_545
Pb1 F9 F1 54.7(5) . 1_545
F7 F9 F1 145.6(8) 1_554 1_545
F8 F9 F1 111.7(8) 1_554 1_545
F5 F9 F1 66.4(6) 1_545 1_545
F4 F9 F1 110.2(8) . 1_545
Pb3 F9 F6 83.9(6) . 1_455
Pb1 F9 F6 54.7(5) . 1_455
F7 F9 F6 139.5(8) 1_554 1_455
F8 F9 F6 91.8(7) 1_554 1_455
F5 F9 F6 108.9(8) 1_545 1_455
F4 F9 F6 67.7(6) . 1_455
F1 F9 F6 70.1(6) 1_545 1_455
Pb3 F9 Pb2 93.7(6) . .
Pb1 F9 Pb2 102.5(7) . .
F7 F9 Pb2 51.5(5) 1_554 .
F8 F9 Pb2 111.3(7) 1_554 .
F5 F9 Pb2 54.7(5) 1_545 .
F4 F9 Pb2 83.7(7) . .
F1 F9 Pb2 115.0(7) 1_545 .
F6 F9 Pb2 150.1(9) 1_455 .
Pb3 F9 Pb2 93.5(7) . 1_455
Pb1 F9 Pb2 100.5(7) . 1_455
F7 F9 Pb2 110.2(7) 1_554 1_455
F8 F9 Pb2 51.0(5) 1_554 1_455
F5 F9 Pb2 129.1(7) 1_545 1_455
F4 F9 Pb2 127.3(8) . 1_455
F1 F9 Pb2 63.5(5) 1_545 1_455
F6 F9 Pb2 61.1(6) 1_455 1_455
Pb2 F9 Pb2 148.6(7) . 1_455
Pb1 OW Pb1 109.1(6) 2_656 .
Pb1 OW F3 88.3(7) 2_656 2_766
Pb1 OW F3 145.3(8) . 2_766
Pb1 OW F4 91.4(6) 2_656 2_666
Pb1 OW F4 106.0(7) . 2_666
F3 OW F4 103.2(8) 2_766 2_666
Pb1 OW F4 160.3(7) 2_656 .
Pb1 OW F4 51.1(4) . .
F3 OW F4 108.6(7) 2_766 .
F4 OW F4 94.5(6) 2_666 .
Pb1 OW F3 91.3(6) 2_656 2_666
Pb1 OW F3 53.1(5) . 2_666
F3 OW F3 159.5(10) 2_766 2_666
F4 OW F3 56.3(6) 2_666 2_666
F4 OW F3 76.5(7) . 2_666
Pb1 OW F3 52.7(5) 2_656 1_545
Pb1 OW F3 90.3(6) . 1_545
F3 OW F3 76.5(8) 2_766 1_545
F4 OW F3 144.0(8) 2_666 1_545
F4 OW F3 120.1(7) . 1_545
F3 OW F3 118.9(7) 2_666 1_545
Pb1 OW F1 50.8(4) 2_656 2_666
Pb1 OW F1 155.8(7) . 2_666
F3 OW F1 56.3(7) 2_766 2_666
F4 OW F1 66.0(6) 2_666 2_666
F4 OW F1 147.9(7) . 2_666
F3 OW F1 108.7(7) 2_666 2_666
F3 OW F1 86.0(6) 1_545 2_666
Pb1 OW OW 54.8(5) 2_656 2_656
Pb1 OW OW 54.4(5) . 2_656
F3 OW OW 133.3(10) 2_766 2_656
F4 OW OW 105.0(9) 2_666 2_656
F4 OW OW 105.5(9) . 2_656
F3 OW OW 60.0(7) 2_666 2_656
F3 OW OW 58.9(7) 1_545 2_656
F1 OW OW 104.2(8) 2_666 2_656
Pb1 OW H1 74(10) 2_656 .
Pb1 OW H1 122(10) . .
F3 OW H1 91(10) 2_766 .
F4 OW H1 21(10) 2_666 .
F4 OW H1 114(10) . .
F3 OW H1 70(10) 2_666 .
F3 OW H1 125(10) 1_545 .
F1 OW H1 46(10) 2_666 .
OW OW H1 104(10) 2_656 .
Pb1 OW H2 106(10) 2_656 .
Pb1 OW H2 121(10) . .
F3 OW H2 25(10) 2_766 .
F4 OW H2 119(10) 2_666 .
F4 OW H2 88(10) . .
F3 OW H2 163(10) 2_666 .
F3 OW H2 75(10) 1_545 .
F1 OW H2 81(10) 2_666 .
OW OW H2 133(10) 2_656 .
H1 OW H2 111.7(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 F5 2.456(17) 1_545
Pb1 F9 2.46(2) .
Pb1 F4 2.513(13) .
Pb1 F1 2.534(15) 1_545
Pb1 F6 2.538(18) 1_455
Pb1 F3 2.62(2) 2_666
Pb1 OW 2.721(16) 2_656
Pb1 OW 2.734(18) .
Pb2 F7 2.502(13) 2_656
Pb2 F8 2.519(13) 1_654
Pb2 F7 2.527(14) 1_554
Pb2 F8 2.550(14) 2_656
Pb2 F2 2.604(14) .
Pb2 F5 2.686(16) 1_545
Pb2 F9 2.98(2) .
Pb2 F9 3.00(2) 1_655
Pb3 F9 2.422(17) .
Pb3 F8 2.478(14) 1_554
Pb3 F7 2.499(14) 1_554
Pb3 F7 2.532(13) 2_666
Pb3 F2 2.600(17) .
Pb3 F8 2.610(14) 2_566
Pb3 F1 2.742(16) .
Pb3 F4 3.015(15) .
Fe F6 1.890(16) .
Fe F3 1.90(2) .
Fe F4 1.908(15) .
Fe F1 1.952(16) 1_655
Fe F5 1.964(16) .
Fe F2 1.973(16) .
F1 Fe 1.952(16) 1_455
F1 Pb1 2.534(15) 1_565
F1 F5 2.69(3) 1_455
F1 F2 2.72(2) 1_455
F1 F3 2.79(3) 1_455
F1 F6 2.84(2) 1_455
F1 F9 2.97(2) 1_565
F1 OW 3.13(2) 2_666
F2 F6 2.63(2) .
F2 F4 2.64(2) .
F2 F7 2.65(2) 1_554
F2 F5 2.69(2) .
F2 F1 2.72(2) 1_655
F2 F7 2.94(2) 2_666
F2 F8 2.95(2) 1_654
F3 Pb1 2.62(2) 2_666
F3 F6 2.74(3) .
F3 OW 2.76(3) 2_766
F3 F4 2.78(3) .
F3 F1 2.79(3) 1_655
F3 F5 2.86(3) .
F3 F6 3.05(3) 2_766
F3 OW 3.09(3) 2_666
F3 OW 3.13(3) 1_565
F4 F5 2.629(19) .
F4 F6 2.73(3) .
F4 OW 2.76(2) 2_666
F4 F9 2.87(2) .
F4 OW 3.05(2) .
F5 Pb1 2.456(17) 1_565
F5 Pb2 2.686(16) 1_565
F5 F1 2.69(3) 1_655
F5 F9 2.86(3) 1_565
F6 Pb1 2.538(18) 1_655
F6 F1 2.84(2) 1_655
F6 F9 2.97(3) 1_655
F6 F3 3.05(3) 2_766
F7 Pb3 2.499(14) 1_556
F7 Pb2 2.502(13) 2_656
F7 Pb2 2.527(14) 1_556
F7 Pb3 2.532(13) 2_666
F7 F2 2.65(2) 1_556
F7 F9 2.83(2) 1_556
F7 F8 2.86(2) 1_655
F7 F8 2.90(2) .
F7 F7 2.90(2) 2_657
F7 F2 2.94(2) 2_666
F7 F7 3.05(2) 2_667
F8 Pb3 2.478(14) 1_556
F8 Pb2 2.519(13) 1_456
F8 Pb2 2.550(14) 2_656
F8 Pb3 2.610(14) 2_566
F8 F9 2.85(3) 1_556
F8 F7 2.86(2) 1_455
F8 F2 2.95(2) 1_456
F8 F8 2.95(2) 2_567
F8 F8 3.00(2) 2_557
F9 F7 2.83(2) 1_554
F9 F8 2.85(3) 1_554
F9 F5 2.86(3) 1_545
F9 F1 2.97(2) 1_545
F9 F6 2.97(3) 1_455
F9 Pb2 3.00(2) 1_455
OW Pb1 2.721(16) 2_656
OW F3 2.76(3) 2_766
OW F4 2.76(2) 2_666
OW F3 3.09(3) 2_666
OW F3 3.13(3) 1_545
OW F1 3.13(2) 2_666
OW OW 3.16(3) 2_656
OW H1 0.900(10) .
OW H2 0.900(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
OW H1 F4 0.9(2) 1.9(3) 2.76(2) 151.00 2_666 yes
OW H2 F6 0.9(2) 2.5(4) 3.14(2) 130.00 . yes
OW H2 F3 0.9(2) 2.00(19) 2.75(3) 144.00 2_766 yes

_cod_database_fobs_code 3500022