Nucleophilic Reactivity and Oxo/Sulfido Substitution Reactions of MVIO3 Groups (M = Mo, W)
David V. Partyka; Richard J. Staples; R. H. Holm; Inorganic Chemistry 42 (2003) 7877–7886; doi:10.1021/ic030185l

data_4312561
_publ_section_title
;
 Nucleophilic Reactivity and Oxo/Sulfido Substitution Reactions of MVIO3
 Groups (M = Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7877
_journal_page_last               7886
_journal_paper_doi               10.1021/ic030185l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C32 H66 F6 Mo2 N6 O11 S2'
_chemical_formula_weight         1080.91
_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                70.98(3)
_cell_angle_beta                 74.29(3)
_cell_angle_gamma                88.13(3)
_cell_formula_units_Z            1
_cell_length_a                   10.071(2)
_cell_length_b                   10.541(2)
_cell_length_c                   11.868(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1144.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7815
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.721
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             558
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.9700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                4418
_reflns_number_total             5384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030185l_06.cif
_cod_data_source_block           Compound8
_cod_original_cell_volume        1144.5(4)
_cod_database_code               4312561