Synthesis, structure and magnetic behaviors of a new fluorophosphate PbCuPO4F
Long, Jingwen; Huang, Xing; Cui, Meiyan; Zhao, Zhiying; He, Zhangzhen; Journal of Solid State Chemistry 305 (2022) 122666–; doi:10.1016/j.jssc.2021.122666

data_1566059
_publ_section_title
;
 Synthesis, structure and magnetic behaviors of a new fluorophosphate
 PbCuPO4F
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              122666
_journal_paper_doi               10.1016/j.jssc.2021.122666
_journal_volume                  305
_journal_year                    2022
_chemical_formula_moiety         'Cu F O4 P Pb'
_chemical_formula_sum            'Cu F O4 P Pb'
_chemical_formula_weight         384.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.075(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.93230(10)
_cell_length_b                   9.2826(2)
_cell_length_c                   8.8000(2)
_cell_measurement_reflns_used    3916
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0860
_cell_measurement_theta_min      2.2020
_cell_volume                     402.904(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -118.00  62.00   0.50    5.00    --  -28.00  45.00 180.00  360
  2  \w   -118.00  22.00   0.50    5.00    --  -28.00  45.00  90.00  280
  3  \w   -118.00 -38.00   0.50    5.00    --  -28.00  45.00   0.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0824781000
_diffrn_orient_matrix_UB_12      -0.0507350000
_diffrn_orient_matrix_UB_13      -0.0387814000
_diffrn_orient_matrix_UB_21      -0.1169024000
_diffrn_orient_matrix_UB_22      0.0296099000
_diffrn_orient_matrix_UB_23      0.0349912000
_diffrn_orient_matrix_UB_31      -0.0147828000
_diffrn_orient_matrix_UB_32      0.0488507000
_diffrn_orient_matrix_UB_33      -0.0613830000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2191
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.190
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    47.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    6.342
_exptl_crystal_F_000             668
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.374
_refine_ls_extinction_coef       0.0063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         705
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0364
_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^)+33.2624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                702
_reflns_number_total             705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2022-305-122666.cif
_cod_data_source_block           ljw
_cod_database_code               1566059
_reflns_odcompleteness_completeness 94.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.09
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O008) \\sim Ueq, Uanis(O006) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(P003) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O005) \\sim Ueq, Uanis(O008) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F004) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O007) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
;
_shelx_res_checksum              31007
_shelx_hkl_checksum              88623
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.879
_oxdiff_exptl_absorpt_empirical_full_min 0.514