Synthesis of a new potassium-substituted lead fluorapatite and its structural characterization
Hamza, Mariam; Hamdi, Besma; Ben Ahmed, Ali; Capitelli, Francesco; El Feki, Hafed; RSC Advances 14 (2024) 16876–16885; doi:10.1039/D4RA01014K

data_7248685
_publ_section_title
;
 Synthesis of a new potassium-substituted lead fluorapatite and its
 structural characterization
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              16876
_journal_page_last               16885
_journal_paper_doi               10.1039/D4RA01014K
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'K1.13 O24 P6 Pb5.09, 0.866(F), 3.776(Ca)'
_chemical_formula_sum            'Ca3.78 F0.87 K1.13 O24 P6 Pb5.09'
_chemical_formula_weight         1836.27
_chemical_melting_point          1273
_chemical_name_common            apatite
_chemical_name_systematic        Pb~5.09~Ca~3.78~K~1.13~(PO~4~)~6~F~0.87~
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   No_H
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   9.7190(5)
_cell_length_b                   9.7190(5)
_cell_length_c                   7.1700(6)
_cell_measurement_reflns_used    156
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.39
_cell_measurement_theta_min      2.67
_cell_volume                     586.53(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2(Bruker, 2006)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2006)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker Software, 1999'
_computing_publication_material  WinGXv1.80.05
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4561
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.007
_diffrn_reflns_theta_min         3.733
_exptl_absorpt_coefficient_mu    37.944
_exptl_absorpt_correction_T_max  0.326
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'CrysAlisPro, Rigaku Oxford Diffraction, 2019'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    5.199
_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_F_000             804.1
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.0325
_exptl_crystal_size_min          0.0295
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.328
_refine_ls_extinction_coef       0.0036(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         923
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                673
_reflns_number_total             925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra01014k1.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        586.53(8)
_cod_database_code               7248685
_exptl_absorpt_special_details   'Systematic and Grid Sampling are used'
_shelx_shelxl_version_number     2016/6