Tungsten(VI) N-Heterocyclic Carbene Complexes: Synthetic, Structural, and Computational Study
Dodds, Christopher A.; Spicer, Mark D.; Tuttle, Tell; Organometallics 30 (2011) 6262–; doi:10.1021/om200838f

data_4065482
_publ_contact_author             'Spicer, Mark D.'
_publ_section_title
;
 Tungsten(VI) N-Heterocyclic Carbene Complexes: Synthetic, Structural, and
 Computational Study
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6262
_journal_paper_doi               10.1021/om200838f
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H36 Cl2 N2 O2 W1, C7 H8'
_chemical_formula_sum            'C34 H44 Cl2 N2 O2 W'
_chemical_formula_weight         767.48
_chemical_name_common            '[WO2Cl2(Idipp)] toluene solvate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-08-24T15:11:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.975(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4185(2)
_cell_length_b                   21.8042(6)
_cell_length_c                   15.8247(4)
_cell_measurement_reflns_used    10323
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3438.23(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.527342E-1
_diffrn_orient_matrix_UB_12      -0.315086E-1
_diffrn_orient_matrix_UB_13      -0.41851E-1
_diffrn_orient_matrix_UB_21      0.620355E-1
_diffrn_orient_matrix_UB_22      0.44498E-2
_diffrn_orient_matrix_UB_23      -0.373687E-1
_diffrn_orient_matrix_UB_31      0.586676E-1
_diffrn_orient_matrix_UB_32      -0.330272E-1
_diffrn_orient_matrix_UB_33      0.348918E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24512
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.93
_refine_diff_density_min         -1.21
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+7.7005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                5400
_reflns_number_total             7826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200838f_si_010.cif
_cod_data_source_block           cdadv1
_cod_original_cell_volume        3438.23(14)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C34 H44 Cl2 N2 O2 W1'
_cod_database_code               4065482
_exptl_absorpt_correction_details
;
While a formal absorption correction was not performed, the data scaling 
process performs what is, to all extents and purposes, a multiscan absorption 
correction. The program used does not allow the extraction of Tmin and Tmax.
However, the absence of unreasonably large peaks in the difference map and
no indications of the usual problems associated with absorption led us to
judge this correction adequate. 
;