Aqueous Chemistry of the Metallocene [Cp2MoCl2]BF4: Evidence of Autocatalytic Molybdenum(V) Reduction in Water
Kuo, Louis Y.; Shari’ati, Yusef A.; Valente, Edward J.; Organometallics 32 (2013) 2902–; doi:10.1021/om301262u

data_4080665
_publ_section_title
;
 Aqueous Chemistry of the Metallocene [Cp2MoCl2]BF4: Evidence of
 Autocatalytic Molybdenum(V) Reduction in Water
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2902
_journal_paper_doi               10.1021/om301262u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C10 H10 B1 Cl2 F4 Mo1'
_chemical_formula_sum            'C10 H10 B Cl2 F4 Mo'
_chemical_formula_weight         383.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2a'
_symmetry_space_group_name_H-M   'P m n m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5714(3)
_cell_length_b                   6.8640(2)
_cell_length_c                   9.3036(3)
_cell_measurement_reflns_used    1201
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     611.23(3)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2307
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.65
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.8138
_exptl_absorpt_correction_T_min  0.5324
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0015(11)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0250P)^2^+0.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                937
_reflns_number_total             1000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301262u_si_001.cif
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      'P m n m'
_cod_database_code               4080665