Synthesis and magnetic properties of two fluorophosphates K2Mn(PO3F)F3 and Na2Mn(HPO4)F3 with a S = 2 uniform spin chain structure
Luo, Qi; Li, Ningxia; Zhao, Zhiying; Cui, Meiyan; He, Zhangzhen; CrystEngComm 26 (2024) 2796–2802; doi:10.1039/D4CE00180J

data_7248574
_publ_section_title
;
 Synthesis and magnetic properties of two fluorophosphates K2Mn(PO3F)F3
 and Na2Mn(HPO4)F3 with a S = 2 uniform spin chain structure
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              2796
_journal_page_last               2802
_journal_paper_doi               10.1039/D4CE00180J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'F3 H Mn Na2 O4 P'
_chemical_formula_sum            'F3 H Mn Na2 O4 P'
_chemical_formula_weight         253.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-21
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.673(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.6785(3)
_cell_length_b                   7.7011(3)
_cell_length_c                   6.8171(4)
_cell_measurement_reflns_used    2086
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      30.0680
_cell_measurement_theta_min      3.1540
_cell_volume                     280.72(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.858
_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    -15.00  49.00   0.50    0.07    --   10.12 -99.00 120.00  128
  2  \w    -69.00  14.00   0.50    0.07    --   10.12 -21.00 169.00  166
  3  \w    -60.00 -32.00   0.50    0.07    --   10.12 -77.00  30.00   56
  4  \w      4.00  37.00   0.50    0.07    --   10.12 -77.00  30.00   66
  5  \w    -18.00  41.00   0.50    0.07    --   10.12 -99.00 -90.00  118
  6  \w    -18.00  28.00   0.50    0.07    --   -9.26 -99.00-180.00   92
  7  \w    -26.00  45.00   0.50    0.07    --   -9.26  21.00 -24.00  142
  8  \w    -12.00  29.00   0.50    0.07    --   -9.26 -99.00  30.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1319873000
_diffrn_orient_matrix_UB_12      -0.0088442000
_diffrn_orient_matrix_UB_13      -0.0332722000
_diffrn_orient_matrix_UB_21      -0.0014945000
_diffrn_orient_matrix_UB_22      -0.0231273000
_diffrn_orient_matrix_UB_23      -0.1011621000
_diffrn_orient_matrix_UB_31      0.0135359000
_diffrn_orient_matrix_UB_32      -0.0886706000
_diffrn_orient_matrix_UB_33      0.0296099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3512
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.193
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.004
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0250
_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^+0.2586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                701
_reflns_number_total             764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00180j2.cif
_cod_data_source_block           Na2Mn
_cod_depositor_comments
'Adding full bibliography for 7248573--7248574.cif.'
_cod_database_code               7248574
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Na Mn P O F'
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.603
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              17756
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.811
_oxdiff_exptl_absorpt_empirical_full_min 0.691