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_4073871
_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
;
(C33 H41 N2 O3  W1 1+), (C24  B1 F20 1-)
;
_chemical_formula_sum            'C57 H41 B F20 N2 O3 W'
_chemical_formula_weight         1376.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.636(4)
_cell_length_b                   17.126(3)
_cell_length_c                   35.532(7)
_cell_measurement_temperature    150(2)
_cell_volume                     10732(4)
_computing_cell_refinement
;
average of cell contants determined on each image plate
;
_computing_data_collection
;
see M.J. Gray etal for a descroption of data collection at beamline x7b
;
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski)'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  Huber
_diffrn_measurement_method       Mar345
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source
;
National Synchrotron Light Source beamline x7b
;
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.92200
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            22257
_diffrn_reflns_theta_full        31.16
_diffrn_reflns_theta_max         31.16
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         6833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+47.7292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                4622
_reflns_number_total             6833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700694e-file004.cif
_cod_data_source_block           walbr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Pbca
_cod_database_code               4073871