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_4332482
_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_sum            'C12 H36 F3 Mo7 N3 Na2 O28'
_chemical_formula_weight         1445.00
_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                108.660(3)
_cell_angle_beta                 93.991(3)
_cell_angle_gamma                106.434(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7628(11)
_cell_length_b                   11.8564(11)
_cell_length_c                   17.0575(16)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      61.076
_cell_measurement_theta_min      5.121
_cell_volume                     2128.0(4)
_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 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'pho 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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21964
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.9201
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs, G. Sheldrick, Goettingen'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0362P)^2^+3.2051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                5684
_reflns_number_total             8726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604359sup1.cif
_cod_data_source_block           tricap
_cod_database_code               4332482