One-Electron Oxidations of the Methyldiphenylphosphonium Cyclopentadienylide Complexes M(η5-C5H4PMePh2)(CO)3(M = Cr, Mo, W): Formation and Dimerization of the 17-Electron, Metal-Centered Radicals [M(η5-C5H4PMePh2)(CO)3]+
Brownie, John H.; Baird, Michael C.; Laws, Derek R.; Geiger, William E.; Organometallics 26 (2007) 5890–; doi:10.1021/om700688p

data_4073860
_publ_section_title
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 One-Electron Oxidations of the Methyldiphenylphosphonium
 Cyclopentadienylide Complexes M(\h5-C5H4PMePh2)(CO)3(M = Cr, Mo,
 W):&#x00A0; Formation and Dimerization of the 17-Electron, Metal-Centered
 Radicals [M(\h5-C5H4PMePh2)(CO)3]+
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5890
_journal_paper_doi               10.1021/om700688p
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C93 H40 B2 Cl6 Cr2 F40 O6 P2'
_chemical_formula_weight         2413.51
_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                70.9350(10)
_cell_angle_beta                 83.1200(10)
_cell_angle_gamma                88.6700(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8319(4)
_cell_length_b                   12.8275(6)
_cell_length_c                   19.6330(9)
_cell_measurement_reflns_used    8166
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.29
_cell_volume                     2323.09(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.9184
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         8129
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0596P)^2^+0.8660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                6594
_reflns_number_total             8129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700688p-file002.cif
_cod_data_source_block           mb17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073860