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_4116310
_publ_section_title
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 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)
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_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 H42 F6 P3 W'
_chemical_formula_weight         865.46
_chemical_name_systematic
;
 ?
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.424(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3763(8)
_cell_length_b                   16.6844(15)
_cell_length_c                   15.0123(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      19.3
_cell_measurement_theta_min      17.5
_cell_volume                     3541.4(5)
_computing_cell_refinement       'Enraf-Nonius EXPRESS'
_computing_data_collection       'Enraf-Nonius EXPRESS'
_computing_data_reduction        'XCAD4, Harms; Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w:2\q 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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19459
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.4216
_exptl_absorpt_correction_T_min  0.3384
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6226
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.1624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0861
_refine_ls_wR_factor_obs         0.0767
_reflns_number_observed          4577
_reflns_number_total             6226
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9834881_1.cif
_cod_data_source_block           '[Cp*WH3(dppe)]PF6'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.1624P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.1624P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116310