#------------------------------------------------------------------------------
#$Date: 2023-03-13 08:35:08 +0100 (Mon 13 de Mar de 2023) $
#$Revision: 281832 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/38/2003882.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003882
loop_
_publ_author_name
'Sarraute, S.'
'Ravez, J.'
'Bravic, G.'
'Chasseau, D.'
'Abrahams, S. C.'
_publ_section_title
;
 Paraelastic Pb₅Al₃F₁₉ at 370 K
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1731
_journal_page_last               1732
_journal_paper_doi               10.1107/S0108270195001879
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'melting and slow cooling'
_chemical_formula_analytical     'Pb5 Al3 F19'
_chemical_formula_moiety         'Pb5 Al3 F19'
_chemical_formula_sum            'Al3 F19 Pb5'
_chemical_formula_weight         1477.89
_chemical_name_systematic        ' ?'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.285(7)
_cell_length_b                   14.285(7)
_cell_length_c                   7.227(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    370
_cell_measurement_theta_max      26
_cell_measurement_theta_min      10
_cell_volume                     1474.8(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'local program (unpublished)'
_computing_molecular_graphics
'   CRYSTALS (Watkin, Carruthers & Betteridge, 1985)'
_computing_structure_refinement
'   CRYSTALS (Watkin, Carruthers & Betteridge, 1985)'
_diffrn_ambient_temperature      370
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       ω/θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Xray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .065
_diffrn_reflns_av_sigmaI/netI    3
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -020
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -020
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5787
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         0
_diffrn_standards_decay_%        <4
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    56.4
_exptl_absorpt_correction_T_max  .0185
_exptl_absorpt_correction_T_min  .0009
_exptl_absorpt_correction_type   'by spherical model'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.66
_exptl_crystal_density_meas      6.66
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2480
_exptl_crystal_size_rad          .3
_refine_diff_density_max         5
_refine_diff_density_min         -06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.12
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_obs      1.12
_refine_ls_R_factor_obs          .053
_refine_ls_shift/esd_max         .01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      '[w][1-(\DF/6\sF)^2^]^2^'
_refine_ls_wR_factor_obs         .058
_reflns_number_observed          1314
_reflns_number_total             1715
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            du1109.cif
_cod_data_source_block           Pb5Al3F19
_cod_original_cell_volume        1475(3)
_cod_database_code               2003882
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text

1 'Steef Boerrigter' 2023-02-22T10:07:00+02:00
;Corrected space group symmetry operator:
added missing minus symbol
y,x,-z  -->  -y,x,-z
;

2 'Saulius Gra\<zulis' 2023-02-23T21:02:48+02:00
;Changing the '..._site_symmetry_...' data item values to
question marks, indicating that they are not know. This is
necessary since the symmetry operators have been updated
and we do not know what operators were meant by the original
CIF.
;

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
-y,x,z
y,-x,z
-x,-y,-z
x,y,-z
y,-x,-z
-y,x,-z
x+0.5,y+0.5,z+0.5
0.5-x,0.5-y,z+0.5
0.5-y,x+0.5,z+0.5
y+0.5,0.5-x,z+0.5
0.5-x,0.5-y,0.5-z
x+0.5,y+0.5,0.5-z
y+0.5,0.5-x,0.5-z
0.5-y,x-0.5,0.5-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Pb1 0.030(2) 0.0200(10) 0.011(5) 0.0000 0.0000 0.006(2) Pb
Pb2 0.021(3) 0.013(2) 0.010(6) 0.0000 0.0000 -0.005(5) Pb
Pb3 0.122(2) 0.122(2) 0.025(4) 0.0000 0.0000 0.000 Pb
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_type_symbol
Pb1 .08474(7) -0.23970(6) .0000 .0180(10) Uani Pb
Pb2 -.06116(6) -0.21768(5) .5000 .013(2) Uani Pb
Pb3 .0000 .5000 .2500 .072(2) Uani Pb
Al1 .1581(4) .3255(4) .0000 .012(4) Uiso Al
Al2 .0000 .0000 .24600(10) .012(4) Uiso Al
F1 .0000 .0000 .0000 .038(5) Uiso F
F2 .0000 .0000 .5000 .038(5) Uiso F
F3 .3854(9) .4500(8) .2460(2) .038(5) Uiso F
F4 .2001(9) .4076(9) .1730(2) .038(5) Uiso F
F5 .3921(9) .2494(9) .6700(2) .038(5) Uiso F
F6 .2630(10) .2610(10) .0000 .038(5) Uiso F
F7 .4530(10) .1120(10) .5000 .038(5) Uiso F
F8 .4170(10) .1250(10) .0000 .038(5) Uiso F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
Pb *DS 'Cromer \& Waber (1974)' '21.7886 1.33660 19.5682 0.488383'
'19.1406 6.77270 7.01107 23.8132 12.4734'
Al HF 'Cromer \& Waber (1974)' '4.17448 1.93816 3.38760 4.14553 1.20296'
'0.228753 0.528137 8.28524 0.706786'
F HF 'Cromer \& Waber (1974)' '3.63220 5.27756 3.51057 14.7353'
'1.26064 0.442258 0.940706 47.3437 0.653396'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
10 5 5
-5 10 5
10 -1 1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F4 Pb1 F4 ? ? ? 139.7(6) yes
F4 Pb1 F6 ? ? ? 85.0(3) yes
F5 Pb2 F5 ? ? ? 142.2(6) yes
F5 Pb2 F6 ? ? ? 73.4(3) yes
F5 Pb2 F8 ? ? ? 77.2(6) yes
F6 Pb2 F8 ? ? ? 75.2(6) yes
F7 Pb3 F7 ? ? ? 87.9(6) yes
F7 Pb3 F7 ? ? ? 121.2(3) yes
F4 Al1 F4 ? ? ? 87.0(8) yes
F4 Al1 F5 ? ? ? 175.1(7) yes
F4 Al1 F5 ? ? ? 92.7(6) yes
F5 Al1 F5 ? ? ? 87.2(9) yes
F4 Al1 F6 ? ? ? 93.3(6) yes
F4 Al1 F7 ? ? ? 88.4(6) yes
F5 Al1 F7 ? ? ? 86.8(6) yes
F6 Al1 F7 ? ? ? 177.7(9) yes
F1 Al2 F2 ? ? ? 179.99 yes
F1 Al2 F3 ? ? ? 92.0(5) yes
F3 Al2 F3 ? ? ? 89.93(3) yes
F3 Al2 F3 ? ? ? 176.1(10) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 F4 ? 2.520(10) yes
Pb1 F4 ? 2.520(10) yes
Pb1 F6 ? 2.54(2) yes
Pb2 F5 ? 2.520(10) yes
Pb2 F5 ? 2.520(10) yes
Pb2 F6 ? 2.54(2) yes
Pb2 F8 ? 2.27(2) yes
Pb3 F7 ? 2.510(10) yes
Pb3 F7 ? 2.510(10) yes
Pb3 F7 ? 2.510(10) yes
Pb3 F7 ? 2.510(10) yes
Al1 F4 ? 1.820(10) yes
Al1 F4 ? 1.820(10) yes
Al1 F5 ? 1.780(10) yes
Al1 F5 ? 1.780(10) yes
Al1 F6 ? 1.75(2) yes
Al1 F7 ? 1.81(2) yes
Al2 F1 ? 1.777(8) yes
Al2 F2 ? 1.836(8) yes
Al2 F3 ? 1.790(10) yes
Al2 F3 ? 1.790(10) yes
Al2 F3 ? 1.790(10) yes
Al2 F3 ? 1.790(10) yes
