K5Mo4O14F: A Novel Fluorinated Polyoxomolybdate and Its Structural Stability.
Gong, Pifu; Luo, Siyang; Kang, Lei; Jiang, Xingxing; Xu, Jing; Zhang, Guochun; Lin, Zheshuai; Wu, Yicheng; Chen, Chuangtian; Inorganic chemistry 54 (2015) 6066–6068; doi:10.1021/acs.inorgchem.5b00643

data_4343260
_publ_section_title
;
 K5Mo4O14F: A Novel Fluorinated Polyoxomolybdate and Its Structural
 Stability.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6066
_journal_page_last               6068
_journal_paper_doi               10.1021/acs.inorgchem.5b00643
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'K5 Mo4 O14 F'
_chemical_formula_sum            'F K5 Mo4 O14'
_chemical_formula_weight         822.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.128(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8632(6)
_cell_length_b                   10.6729(3)
_cell_length_c                   8.4569(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1596.13(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2783
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.450
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1535
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.0253(7)
_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   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+18.9097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                1305
_reflns_number_total             1407
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b00643_si_002.cif
_cod_data_source_block           20150112
_cod_depositor_comments          'Adding full bibliography for 4343260.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4343260