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_2105287
_publ_section_title
;
 Dinuclear oxofluorometallates as a new structural type of <i>d</i>^0^
 transition metal oxofluoride compound
;
_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(NH4)
_chemical_formula_structural     '(NH4)3(Nb2O2F9) (NH4F)0.333'
_chemical_formula_sum            'F28 H40 N10 Nb6 O6'
_chemical_formula_weight         1325.56
_chemical_name_systematic        'ammonium oxofluoroniobate'
_space_group_IT_number           164
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   20.3757(4)
_cell_length_b                   20.3757(4)
_cell_length_c                   8.0851(3)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.67
_cell_measurement_theta_min      2.77
_cell_volume                     2906.97(13)
_computing_cell_refinement       'Bruker SAINT v6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker Smart v5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT v6.02a (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_publication_material  'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_structure_refinement  'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_structure_solution    'Bruker SHELXTL v5.1 (Bruker, 1998)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34445
_diffrn_reflns_theta_full        31.86
_diffrn_reflns_theta_max         31.86
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  0.6508
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shere
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.018
_refine_diff_density_min         -2.186
_refine_ls_extinction_coef       0.00016(12)
_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   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+30.7776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.224
_reflns_number_gt                3158
_reflns_number_total             3484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5045.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      P-3m1
_cod_original_formula_sum        ' F28 Nb6 O6 (NH4)10'
_cod_database_code               2105287