A New High-Pressure Polymorph of K2MoO2F4
Zimmerhofer, Fabian; Huppertz, Hubert; Dalton Transactions  (2023) –; doi:10.1039/D3DT02992A

data_7714397
_publ_section_title
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 A New High-Pressure Polymorph of K2MoO2F4
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02992A
_journal_year                    2023
_chemical_formula_moiety         'F4 Mo O2, 2(K)'
_chemical_formula_sum            'F4 K2 Mo O2'
_chemical_formula_weight         282.14
_chemical_name_common            'potassium fluoridooxidomolybdate'
_chemical_name_systematic        'potassium fluoridooxidomolybdate'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-13 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.357(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8579(5)
_cell_length_b                   5.8109(2)
_cell_length_c                   6.9442(3)
_cell_measurement_reflns_used    5613
_cell_measurement_temperature    301.00
_cell_measurement_theta_max      38.320
_cell_measurement_theta_min      2.933
_cell_volume                     559.18(4)
_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 4 v4.6.6 (Crystal Impact, 2021)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    SHELXTL-2018/2
_diffrn_ambient_temperature      301.00
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C14'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9484
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.497
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'Incoatec Microfocus'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.842
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0712 before and 0.0471 after correction.
The Ratio of minimum to maximum transmission is 0.8572.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.351
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.827
_refine_diff_density_min         -2.083
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.0082(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0416P)^2^+1.7355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1493
_reflns_number_total             1568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02992a2.cif
_cod_data_source_block           K2MoO2F4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7714397
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9413(11)
 0.0587(11)
2. Shared sites
{F1, O1}
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(O1)
4. Others
 Fixed Sof: O1(0.5) F1(0.5)
;
_shelx_res_checksum              23201
_olex2_submission_special_instructions 'No special instructions were received'