Synthesis and Characterization of Novel Fluorinated Poly(oxomolybdates)
Michailovski, Alexej; Rüegger, Heinz; Sheptyakov, Denis; Patzke, Greta R.; Inorganic Chemistry 45 (2006) 5641–5652; doi:10.1021/ic0604359

data_4332481
_publ_section_title
;
 Synthesis and Characterization of Novel Fluorinated Poly(oxomolybdates)
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5641
_journal_page_last               5652
_journal_paper_doi               10.1021/ic0604359
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'F3 Mo3.11 Na1.85 O12.07, C4 H12 N, 1.925(O)'
_chemical_formula_sum            'C4 H12 F3 Mo3.11 N Na1.85 O14'
_chemical_formula_weight         695.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.354(3)
_cell_angle_beta                 97.719(3)
_cell_angle_gamma                109.636(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1659(9)
_cell_length_b                   11.8649(13)
_cell_length_c                   11.9329(13)
_cell_measurement_reflns_used    938
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      66.364
_cell_measurement_theta_min      5.321
_cell_volume                     995.54(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15641
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.05
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.8530
_exptl_absorpt_correction_T_min  0.3045
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs_new
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             667
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.3092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5633
_reflns_number_total             7321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604359sup1.cif
_cod_data_source_block           twin_iucr
_cod_original_cell_volume        995.53(19)
_cod_database_code               4332481