#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/38/2013840.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_2013840
loop_
_publ_author_name
'Besma Hamdi'
'Jean-Michel Savariault'
'Hafed El Feki'
'Abdelhamid Ben Salah'
_publ_section_title
;
 Lead bismuth calcium sodium phosphate:
 Pb~4.6~Bi~0.4~Ca~2.6~Na~2.4~(PO₄)₆
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i1
_journal_page_last               i2
_journal_paper_doi               10.1107/S0108270103024971
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'Pb4.6 Bi0.4 Ca2.6 Na2.4 (PO4)6'
_chemical_formula_sum            'Bi0.4 Ca2.59 Na2.39 O24 P6 Pb4.61'
_chemical_formula_weight         1768.64
_chemical_melting_point          1373
_chemical_name_common            'lead bismuth calcium sodium phosphate'
_chemical_name_systematic
;
Pb~4.6~Bi~0.4~Ca~2.6~Na~2.4~(PO₄)₆.
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   9.5953(6)
_cell_length_b                   9.5953(6)
_cell_length_c                   7.0418(4)
_cell_measurement_reflns_used    KappaCCD
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      48.0
_cell_measurement_theta_min      5.0
_cell_volume                     561.48(6)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker Software, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Nonis KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'vertically mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17792
_diffrn_reflns_theta_full        47.95
_diffrn_reflns_theta_max         47.96
_diffrn_reflns_theta_min         3.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    38.789
_exptl_absorpt_correction_T_max  0.37183
_exptl_absorpt_correction_T_min  0.06602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    5.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_F_000             771.8
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.053
_refine_diff_density_min         -2.446
_refine_ls_extinction_coef       0.0019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1863
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0119P)²+3.2549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                1199
_reflns_number_total             1863
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk1662.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '1373K' was changed to '1373' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '1373K' was changed to '1373' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'Bi0.40 Ca2.59 Na2.39 O24 P6 Pb4.61'
_cod_database_code               2013840
_cod_database_fobs_code          2013840
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ca1 0.6667 0.3333 -0.0052(2) 0.0143(4) Uani d SP 0.648(5) . . Ca
Na1 0.6667 0.3333 -0.0052(2) 0.0143(4) Uani d SP 0.324(12) . . Na
Pb1 0.6667 0.3333 -0.0052(2) 0.0143(4) Uani d SP 0.030(2) . . Pb
Bi2 0.74931(3) 0.00171(3) 0.2500 0.01689(7) Uani d SP 0.067(12) . . Bi
Pb2 0.74931(3) 0.00171(3) 0.2500 0.01689(7) Uani d SP 0.749(15) . . Pb
Na2 0.74931(3) 0.00171(3) 0.2500 0.01689(7) Uani d SP 0.182(13) . . Na
P 0.40658(14) 0.02788(13) 0.2500 0.0103(3) Uani d S 1 . . P
O1 0.5932(5) 0.1229(5) 0.2500 0.0238(9) Uani d S 1 . . O
O2 0.3432(5) -0.1518(4) 0.2500 0.0181(7) Uani d S 1 . . O
O3 0.3512(4) 0.0836(4) 0.4240(5) 0.0262(7) Uani d . 1 . . O
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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Pb1 O2 9_665 7_655 74.81(10) ?
O2 Pb1 O2 9_665 10 74.81(10) ?
O2 Pb1 O2 7_655 10 74.81(10) ?
O2 Pb1 O1 9_665 . 150.41(12) ?
O2 Pb1 O1 7_655 . 92.10(9) ?
O2 Pb1 O1 10 . 127.97(12) ?
O2 Pb1 O1 9_665 3_655 92.10(9) ?
O2 Pb1 O1 7_655 3_655 127.97(12) ?
O2 Pb1 O1 10 3_655 150.41(12) ?
O1 Pb1 O1 . 3_655 74.96(11) ?
O2 Pb1 O1 9_665 4_665 127.97(12) ?
O2 Pb1 O1 7_655 4_665 150.41(12) ?
O2 Pb1 O1 10 4_665 92.10(9) ?
O1 Pb1 O1 . 4_665 74.96(11) ?
O1 Pb1 O1 3_655 4_665 74.96(11) ?
O2 Pb1 O3 9_665 12_656 83.90(11) ?
O2 Pb1 O3 7_655 12_656 73.48(10) ?
O2 Pb1 O3 10 12_656 145.43(10) ?
O1 Pb1 O3 . 12_656 66.82(11) ?
O1 Pb1 O3 3_655 12_656 54.94(11) ?
O1 Pb1 O3 4_665 12_656 122.42(11) ?
O2 Pb1 O3 9_665 11_666 73.48(10) ?
O2 Pb1 O3 7_655 11_666 145.43(10) ?
O2 Pb1 O3 10 11_666 83.90(11) ?
O1 Pb1 O3 . 11_666 122.42(11) ?
O1 Pb1 O3 3_655 11_666 66.82(11) ?
O1 Pb1 O3 4_665 11_666 54.94(11) ?
O3 Pb1 O3 12_656 11_666 116.01(5) ?
O2 Pb1 O3 9_665 8_556 145.43(10) ?
O2 Pb1 O3 7_655 8_556 83.90(11) ?
O2 Pb1 O3 10 8_556 73.48(10) ?
O1 Pb1 O3 . 8_556 54.94(11) ?
O1 Pb1 O3 3_655 8_556 122.42(11) ?
O1 Pb1 O3 4_665 8_556 66.81(11) ?
O3 Pb1 O3 12_656 8_556 116.01(5) ?
O3 Pb1 O3 11_666 8_556 116.01(5) ?
O2 Pb1 P 9_665 . 165.30(9) ?
O2 Pb1 P 7_655 . 90.50(7) ?
O2 Pb1 P 10 . 101.36(9) ?
O1 Pb1 P . . 27.30(9) ?
O1 Pb1 P 3_655 . 97.37(8) ?
O1 Pb1 P 4_665 . 65.76(9) ?
O3 Pb1 P 12_656 . 92.35(7) ?
O3 Pb1 P 11_666 . 120.64(7) ?
O3 Pb1 P 8_556 . 27.89(6) ?
O2 Pb1 P 9_665 3_655 90.50(7) ?
O2 Pb1 P 7_655 3_655 101.36(9) ?
O2 Pb1 P 10 3_655 165.30(9) ?
O1 Pb1 P . 3_655 65.76(9) ?
O1 Pb1 P 3_655 3_655 27.30(9) ?
O1 Pb1 P 4_665 3_655 97.37(8) ?
O3 Pb1 P 12_656 3_655 27.89(6) ?
O3 Pb1 P 11_666 3_655 92.35(7) ?
O3 Pb1 P 8_556 3_655 120.65(7) ?
P Pb1 P . 3_655 92.79(3) ?
O2 Pb1 P 9_665 4_665 101.36(9) ?
O2 Pb1 P 7_655 4_665 165.30(9) ?
O2 Pb1 P 10 4_665 90.50(7) ?
O1 Pb1 P . 4_665 97.37(8) ?
O1 Pb1 P 3_655 4_665 65.76(9) ?
O1 Pb1 P 4_665 4_665 27.30(9) ?
O3 Pb1 P 12_656 4_665 120.65(7) ?
O3 Pb1 P 11_666 4_665 27.89(6) ?
O3 Pb1 P 8_556 4_665 92.35(7) ?
P Pb1 P . 4_665 92.79(3) ?
P Pb1 P 3_655 4_665 92.79(3) ?
O1 Pb2 O3 . 2_654 85.56(8) ?
O1 Pb2 O3 . 7_656 85.56(8) ?
O3 Pb2 O3 2_654 7_656 137.15(17) ?
O1 Pb2 O3 . 12_656 74.78(12) ?
O3 Pb2 O3 2_654 12_656 80.24(6) ?
O3 Pb2 O3 7_656 12_656 136.55(12) ?
O1 Pb2 O3 . 3_655 74.78(12) ?
O3 Pb2 O3 2_654 3_655 136.56(12) ?
O3 Pb2 O3 7_656 3_655 80.24(6) ?
O3 Pb2 O3 12_656 3_655 57.50(14) ?
O1 Pb2 P . 3_655 70.15(10) ?
O3 Pb2 P 2_654 3_655 108.03(8) ?
O3 Pb2 P 7_656 3_655 108.03(8) ?
O3 Pb2 P 12_656 3_655 28.84(7) ?
O3 Pb2 P 3_655 3_655 28.84(7) ?
O1 Pb2 Pb1 . 7_655 76.71(9) ?
O3 Pb2 Pb1 2_654 7_655 43.42(9) ?
O3 Pb2 Pb1 7_656 7_655 93.78(9) ?
O3 Pb2 Pb1 12_656 7_655 117.84(8) ?
O3 Bi2 Pb1 3_655 7_655 151.22(8) ?
P Pb2 Pb1 3_655 7_655 138.169(19) ?
O1 Pb2 Pb1 . 2_655 76.71(9) ?
O3 Pb2 Pb1 2_654 2_655 93.78(9) ?
O3 Pb2 Pb1 7_656 2_655 43.42(9) ?
O3 Pb2 Pb1 12_656 2_655 151.22(8) ?
O3 Pb2 Pb1 3_655 2_655 117.84(8) ?
P Pb2 Pb1 3_655 2_655 138.168(19) ?
Pb1 Pb2 Pb1 7_655 2_655 50.37(4) ?
O1 Pb2 Pb1 . . 34.53(6) ?
O3 Pb2 Pb1 2_654 . 69.58(7) ?
O3 Pb2 Pb1 7_656 . 118.33(7) ?
O3 Pb2 Pb1 12_656 . 43.48(8) ?
O3 Pb2 Pb1 3_655 . 72.54(7) ?
P Pb2 Pb1 3_655 . 52.177(19) ?
Pb1 Pb2 Pb1 7_655 . 86.136(7) ?
Pb1 Pb2 Pb1 2_655 . 108.004(6) ?
O1 Pb2 Pb1 . 8_556 34.53(6) ?
O3 Pb2 Pb1 2_654 8_556 118.33(7) ?
O3 Pb2 Pb1 7_656 8_556 69.58(7) ?
O3 Pb2 Pb1 12_656 8_556 72.54(7) ?
O3 Pb2 Pb1 3_655 8_556 43.48(8) ?
P Pb2 Pb1 3_655 8_556 52.177(19) ?
Pb1 Pb2 Pb1 7_655 8_556 108.003(6) ?
Pb1 Pb2 Pb1 2_655 8_556 86.135(7) ?
Pb1 Pb2 Pb1 . 8_556 52.50(4) ?
O2 P O3 . 8_556 112.64(14) yes
O2 P O3 . . 112.64(14) yes
O3 P O3 8_556 . 106.0(3) yes
O2 P O1 . . 111.0(2) yes
O3 P O1 8_556 . 107.11(17) yes
O3 P O1 . . 107.11(17) yes
O2 P Pb2 . 4_665 135.66(16) ?
O3 P Pb2 8_556 4_665 53.24(13) ?
O3 P Pb2 . 4_665 53.24(13) ?
O1 P Pb2 . 4_665 113.39(16) ?
O2 P Pb1 . . 135.32(10) ?
O3 P Pb1 8_556 . 59.45(14) ?
O3 P Pb1 . . 111.59(13) ?
O1 P Pb1 . . 48.31(11) ?
Pb2 P Pb1 4_665 . 78.41(2) ?
Pb2 P Pb1 4_665 8_556 78.40(2) ?
Pb1 P Pb1 . 8_556 66.53(5) ?
O2 P Pb1 . 8_556 135.32(10) ?
O3 P Pb1 8_556 8_556 111.59(13) ?
O3 P Pb1 . 8_556 59.45(14) ?
O1 P Pb1 . 8_556 48.31(11) ?
Pb2 P Pb1 4_665 8_556 78.40(2) ?
Pb1 P Pb1 . 8_556 66.53(5) ?
P O1 Pb2 . . 123.5(2) ?
P O1 Pb1 . . 104.40(15) ?
Pb2 O1 Pb1 . . 114.23(12) ?
P O1 Pb1 . 8_556 104.40(15) ?
Pb2 O1 Pb1 . 8_556 114.23(12) ?
Pb1 O1 Pb1 . 8_556 90.72(14) ?
P O2 Pb1 . 7_655 131.97(9) ?
P O2 Pb1 . 2_655 131.97(9) ?
Pb1 O2 Pb1 7_655 2_655 90.92(13) ?
P O2 Pb2 . 3_545 96.81(18) ?
Pb1 O2 Pb2 7_655 3_545 97.52(10) ?
Pb1 O2 Pb2 2_655 3_545 97.52(10) ?
P O3 Pb2 . 7_656 140.72(17) ?
P O3 Pb2 . 4_665 97.92(16) ?
Pb2 O3 Pb2 7_656 4_665 116.72(12) ?
P O3 Pb1 . 8_556 92.66(16) ?
Pb2 O3 Pb1 7_656 8_556 99.71(13) ?
Pb2 O3 Pb1 4_665 8_556 98.14(10) ?
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 O2 9_665 2.418(3) yes
Pb1 O2 7_655 2.418(3) ?
Pb1 O2 10 2.418(3) ?
Pb1 O1 . 2.526(3) yes
Pb1 O1 3_655 2.526(3) ?
Pb1 O1 4_665 2.526(3) ?
Pb1 O3 12_656 2.824(4) yes
Pb1 O3 11_666 2.824(4) ?
Pb1 O3 8_556 2.824(4) ?
Pb1 P . 3.2762(12) ?
Pb1 P 3_655 3.2762(12) ?
Pb1 P 4_665 3.2762(12) ?
Pb2 O1 . 2.310(4) yes
Pb2 O3 2_654 2.466(3) yes
Pb2 O3 7_656 2.466(3) yes
Pb2 O3 12_656 2.548(3) yes
Pb2 O3 3_655 2.548(3) yes
Pb2 O2 4_655 2.948(4) yes
Pb2 P 3_655 3.1500(12) ?
Pb2 Pb1 7_655 4.0505(7) ?
Pb2 Pb1 2_655 4.0505(7) ?
Pb2 Pb1 8_556 4.0630(8) ?
P O2 . 1.515(4) yes
P O3 8_556 1.534(3) yes
P O3 . 1.534(3) yes
P O1 . 1.551(4) yes
P Pb2 4_665 3.1500(12) ?
P Pb1 8_556 3.2762(12) ?
O1 Pb1 8_556 2.526(3) ?
O2 Pb1 7_655 2.418(3) ?
O2 Pb1 2_655 2.418(3) ?
O2 Pb2 3_545 2.948(4) ?
O3 Pb2 7_656 2.466(3) ?
O3 Pb2 4_665 2.548(3) ?
O3 Pb1 8_556 2.824(4) ?
