A Tungsten Complex with a Bidentate, Hemilabile N-Heterocyclic Carbene Ligand, Facile Displacement of the Weakly Bound W−(CC) Bond, and the Vulnerability of the NHC Ligand toward Catalyst Deactivation during Ketone Hydrogenation
Wu, Fan; Dioumaev, Vladimir K.; Szalda, David J.; Hanson, Jonathan; Bullock, R. Morris; Organometallics 26 (2007) 5079–; doi:10.1021/om700694e

data_4073869
_publ_section_title
;
 A Tungsten Complex with a Bidentate, Hemilabile N-Heterocyclic Carbene
 Ligand, Facile Displacement of the Weakly Bound W&#x2212;(CC) Bond, and
 the Vulnerability of the NHC Ligand toward Catalyst Deactivation during
 Ketone Hydrogenation
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5079
_journal_paper_doi               10.1021/om700694e
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '( C28 H30 N2 O2 Mo ) (C3.5 H4 )'
_chemical_formula_sum            'C31.5 H34 Mo N2 O2'
_chemical_formula_weight         568.55
_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                106.97(3)
_cell_angle_beta                 95.45(3)
_cell_angle_gamma                92.94(3)
_cell_formula_units_Z            4
_cell_length_a                   8.5080(17)
_cell_length_b                   16.515(3)
_cell_length_c                   21.351(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      3.3
_cell_volume                     2846.6(11)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4VAX (Sheldrick, 1993)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2860
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10795
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        '50% corrected for decay'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  1.159
_exptl_absorpt_correction_T_min  .965
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.755
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.2577
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                4413
_reflns_number_total             10795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700694e-file004.cif
_cod_data_source_block           moabsh
_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_cell_volume        2846.6(10)
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C31.50 H34 Mo N2 O2'
_cod_database_code               4073869