Comproportionation of Cationic and Anionic Tungsten Complexes Having an N-Heterocyclic Carbene Ligand To Give the Isolable 17-Electron Tungsten Radical CpW(CO)2(IMes).
John A. S. Roberts; James A. Franz; Edwin F. van der Eide; Eric D. Walter; Jeffrey L. Petersen; Daniel L. DuBois; R. Morris Bullock; Journal of the American Chemical Society 133 (2011) 14593–14603; doi:10.1021/ja202754e

data_4106768
_publ_section_title
;
 Comproportionation of Cationic and Anionic Tungsten Complexes Having an
 N-Heterocyclic Carbene Ligand To Give the Isolable 17-Electron Tungsten
 Radical CpW(CO)2(IMes).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14593
_journal_page_last               14603
_journal_paper_doi               10.1021/ja202754e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C28 H29 N2 O2 W'
_chemical_formula_weight         609.38
_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                77.913(1)
_cell_angle_beta                 81.191(1)
_cell_angle_gamma                86.769(1)
_cell_formula_units_Z            4
_cell_length_a                   8.4766(5)
_cell_length_b                   16.4875(11)
_cell_length_c                   18.8928(13)
_cell_measurement_reflns_used    6542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.32
_cell_volume                     2550.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17782
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.555
_exptl_absorpt_correction_T_max  0.634
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+2.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                9262
_reflns_number_total             11371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202754e_si_002.cif
_cod_data_source_block           mb2ccd
_cod_database_code               4106768