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_4065481
_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         'C36 H46 Cl5 N2 O1 W1'
_chemical_formula_sum            'C36 H46 Cl5 N2 O W'
_chemical_formula_weight         883.85
_chemical_name_common            '[HIdipp][WOCl5].1.5(C6H6)'
_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      2.4
_audit_creation_date             2011-09-05T15:46:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.636(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6504(5)
_cell_length_b                   17.7093(6)
_cell_length_c                   19.4914(9)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3872.7(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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      -0.420792E-1
_diffrn_orient_matrix_UB_12      0.214758E-1
_diffrn_orient_matrix_UB_13      -0.475807E-1
_diffrn_orient_matrix_UB_21      0.785403E-1
_diffrn_orient_matrix_UB_22      0.129935E-1
_diffrn_orient_matrix_UB_23      -0.85381E-2
_diffrn_orient_matrix_UB_31      0.23097E-2
_diffrn_orient_matrix_UB_32      -0.50582E-1
_diffrn_orient_matrix_UB_33      -0.223948E-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  0.1076
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21342
_diffrn_reflns_theta_full        24.68
_diffrn_reflns_theta_max         24.68
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.357
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_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, apart from a single large peak (ca 3 e A-3) close to the tungsten 
atom there are no indications of the usual problems associated with absorption
and we thus judged further processing unnecessary. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.835
_refine_diff_density_min         -3.732
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+65.6286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2112
_reflns_number_gt                4248
_reflns_number_total             6494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200838f_si_010.cif
_cod_data_source_block           cdadv2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
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      P21/n
_cod_original_formula_sum        'C36 H46 Cl5 N2 O1 W1'
_cod_database_code               4065481