#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/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~(PO~4~)~6~ ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i1 _journal_page_last i2 _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~(PO~4~)~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 none _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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0119P)^2^+3.2549P] where P=(Fo^2^+2Fc^2^)/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>2\s(I) _[local]_cod_data_source_file sk1662.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'Bi0.40 Ca2.59 Na2.39 O24 P6 Pb4.61' _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 ; _cod_database_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_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 Ca1 0.0159(4) 0.0158(4) 0.0112(6) 0.00791(19) 0.000 0.000 Na1 0.0159(4) 0.0158(4) 0.0112(6) 0.00791(19) 0.000 0.000 Pb1 0.0159(4) 0.0158(4) 0.0112(6) 0.00791(19) 0.000 0.000 Bi2 0.02006(11) 0.01364(9) 0.01789(11) 0.00912(7) 0.000 0.000 Pb2 0.02006(11) 0.01364(9) 0.01789(11) 0.00912(7) 0.000 0.000 Na2 0.02006(11) 0.01364(9) 0.01789(11) 0.00912(7) 0.000 0.000 P 0.0121(4) 0.0089(4) 0.0095(5) 0.0050(3) 0.000 0.000 O1 0.0137(14) 0.0190(16) 0.035(3) 0.0056(13) 0.000 0.000 O2 0.0233(17) 0.0100(12) 0.0204(19) 0.0078(12) 0.000 0.000 O3 0.0451(18) 0.0239(13) 0.0161(14) 0.0221(13) 0.0131(13) 0.0050(11) 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) ? 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) ? _cod_database_fobs_code 2013840 _journal_paper_doi 10.1107/S0108270103024971