K<sub>3</sub>Mo<sub>2</sub>O<sub>5.6</sub>F<sub>3.4</sub> and K<sub>3</sub>V<sub>2</sub>O<sub>3.3</sub>F<sub>5.7</sub> - exploring transition metal cation valence and anion distribution in oxyfluorides.
Zimmerhofer, Fabian; Wolf, Eric; Öcal, Baris; Olthof, Selina; Reimann, Maximilian Kai; Pöttgen, Rainer; Huppertz, Hubert; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4278–4290; doi:10.1039/d4dt00064a

data_7715093
_publ_section_title
;
 K<sub>3</sub>Mo<sub>2</sub>O<sub>5.6</sub>F<sub>3.4</sub> and
 K<sub>3</sub>V<sub>2</sub>O<sub>3.3</sub>F<sub>5.7</sub> - exploring
 transition metal cation valence and anion distribution in oxyfluorides.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4278
_journal_page_last               4290
_journal_paper_doi               10.1039/d4dt00064a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'F3.4 K3 Mo2 O5.6'
_chemical_formula_sum            'F3.4 K3 Mo2 O5.6'
_chemical_formula_weight         463.349
_chemical_name_common            'potassium fluoridooxidomolybdate'
_chemical_name_systematic        'potassium fluoridooxidomolybdate'
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_symmetry_Int_Tables_number      166
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   5.7983(1)
_cell_length_b                   5.7983(1)
_cell_length_c                   21.1801(5)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      36.3695
_cell_measurement_theta_min      4.1708
_cell_volume                     616.68(2)
_computing_cell_refinement       'Bruker SAINT-V 8.40B'
_computing_data_collection       'Bruker Apex 4 v2021.4-0'
_computing_data_reduction        'Bruker SAINT-V 8.40B'
_computing_molecular_graphics    'DIAMOND v4.6.8 (Crystal Impact, 2022)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    SHELXTL-2018/2
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.9820
_diffrn_measured_fraction_theta_max 0.9905
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C14'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.9820
_diffrn_reflns_Laue_measured_fraction_max 0.9905
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            11993
_diffrn_reflns_point_group_measured_fraction_full 0.9820
_diffrn_reflns_point_group_measured_fraction_max 0.9905
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    4.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2016/2)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.743
_exptl_crystal_description       block
_exptl_crystal_F_000             641.432
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7481
_exptl_transmission_factor_min   0.6522
_refine_diff_density_max         1.2506
_refine_diff_density_min         -0.7931
_refine_diff_density_rms         0.1627
_refine_ls_d_res_high            0.6615
_refine_ls_d_res_low             7.0600
_refine_ls_extinction_coef       0.013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0189
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     28
_refine_ls_number_reflns         314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0189
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1223P)^2^+3.0465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              4
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -29
_reflns_number_gt                291
_reflns_number_total             314
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00064a1.cif
_cod_data_source_block           Molybdenum
_cod_depositor_comments
'Adding full bibliography for 7715092--7715093.cif.'
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7715093
_olex2_refinement_description
;
1. Shared sites
{F1, O1}
2. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(O1)
3. Others
 Fixed Sof: Mo1(0.16) F1(0.0333) O1(0.46665) Mo2(0.006667)
;