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_4106767
_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            'C40 H53 K N2 O8 W'
_chemical_formula_weight         912.79
_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                 95.021(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5834(5)
_cell_length_b                   24.881(2)
_cell_length_c                   19.4952(15)
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.25
_cell_volume                     4147.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27106
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9351
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+1.3682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                7846
_reflns_number_total             9351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202754e_si_001.cif
_cod_data_source_block           mb1ccd
_cod_original_cell_volume        4147.6(5)
_cod_database_code               4106767