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_4073861
_publ_section_title
;
 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            'C102 H58 B2 F40 Mo2 O9 P2'
_chemical_formula_weight         2462.92
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 92.466(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0003(18)
_cell_length_b                   10.0517(14)
_cell_length_c                   38.132(5)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.14
_cell_measurement_theta_min      2.19
_cell_volume                     4978.3(12)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            44366
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9028
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0881
_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^)+(0.0646P)^2^+40.8712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2248
_reflns_number_gt                5865
_reflns_number_total             8919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700688p-file003.cif
_cod_data_source_block           mb19_a_sqz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2/n
_cod_database_code               4073861