Stable Paramagnetic Half-Sandwich Mo(V) and W(V) Polyhydride Complexes. Structural, Spectroscopic, Electrochemical, Theoretical, and Decomposition Mechanism Studies of [Cp*MH3(dppe)]+ (M = Mo, W)
Brett Pleune; Dolores Morales; Rita Meunier-Prest; Philippe Richard; Edmond Collange; James C. Fettinger; Rinaldo Poli; Journal of the American Chemical Society 121 (1999) 2209–2225; doi:10.1021/ja9834881

data_4116311
_publ_section_title
;
 Stable Paramagnetic Half-Sandwich Mo(V) and W(V) Polyhydride Complexes.
 Structural, Spectroscopic, Electrochemical, Theoretical, and
 Decomposition Mechanism Studies of [Cp*MH3(dppe)]+ (M = Mo, W)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2209
_journal_page_last               2225
_journal_paper_doi               10.1021/ja9834881
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C36 H43 F6 P3 W'
_chemical_formula_weight         866.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.140(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4683(15)
_cell_length_b                   16.4788(15)
_cell_length_c                   15.0809(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      19.3
_cell_measurement_theta_min      17.6
_cell_volume                     3539.4(6)
_computing_cell_refinement       'Enraf-Nonius EXPRESS'
_computing_data_collection       'Enraf-Nonius EXPRESS'
_computing_data_reduction        'Harms (1997) XCAD4; Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       '\w 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  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1132
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9640
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    3.456
_exptl_absorpt_correction_T_max  0.3590
_exptl_absorpt_correction_T_min  0.2640
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Clear, Colorless'
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       'Irregular Block'
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         4617
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                3033
_reflns_number_total             4617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9834881_2.cif
_cod_data_source_block           '[Cp*WH4(dppe)]PF6'
_cod_database_code               4116311