Dinuclear oxofluorometallates as a new structural type of <i>d</i>^0^ transition metal oxofluoride compound
Udovenko, Anatoly A.; Laptash, Natalia M.; Acta Crystallographica Section B 68 (2012) 602–609; doi:10.1107/S0108768112042577

data_2105286
_publ_section_title
;
 Dinuclear oxofluorometallates as a new structural type of <i>d</i>^0^
 transition metal oxofluoride compound
;
_journal_coeditor_code           BP5045
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              602
_journal_page_last               609
_journal_paper_doi               10.1107/S0108768112042577
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         3(F9Nb2O2),F,10(K)
_chemical_formula_structural     'K3(Nb2O2F9) (KF)0.3333'
_chemical_formula_sum            'F28 K10 Nb6 O6'
_chemical_formula_weight         1576.46
_chemical_name_systematic        'potassium oxofluoroniobate'
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   20.1095(6)
_cell_length_b                   7.8045(2)
_cell_length_c                   11.4938(4)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      31.90
_cell_measurement_theta_min      2.69
_cell_volume                     1803.89(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20107
_diffrn_reflns_theta_full        31.91
_diffrn_reflns_theta_max         31.91
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    3.162
_exptl_absorpt_correction_T_max  0.5999
_exptl_absorpt_correction_T_min  0.4311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.775
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_coef       0.00013(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+4.7059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                5889
_reflns_number_total             5975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5045.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     P2ac-2
_cod_original_sg_symbol_H-M      Pmn2(1)
_cod_original_formula_sum        ' F28 Nb6 O6 K10'
_cod_database_code               2105286
_cod_database_fobs_code          2105286