A Highly Stable N-Heterocyclic Carbene Complex of Trichloro-oxo-vanadium(V) Displaying Novel Cl-Ccarbene Bonding Interactions
Colin D. Abernethy; Gareth M. Codd; Mark D. Spicer; Michelle K. Taylor; Journal of the American Chemical Society 125 (2003) 1128–1129; doi:10.1021/ja0276321

data_4113424
_publ_section_title
;
 A Highly Stable N-Heterocyclic Carbene Complex of
 Trichloro-oxo-vanadium(V) Displaying Novel Cl-Ccarbene Bonding
 Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1128
_journal_page_last               1129
_journal_paper_doi               10.1021/ja0276321
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H24 Cl3 N2 O1 V1'
_chemical_formula_sum            'C21 H24 Cl3 N2 O V'
_chemical_formula_weight         477.74
_chemical_name_common            'VOCl3 + carbene'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2002-01-21T15:09:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.3880
_cell_angle_beta                 91.1320(10)
_cell_angle_gamma                108.1750
_cell_formula_units_Z            2
_cell_length_a                   7.8641(2)
_cell_length_b                   8.2857(2)
_cell_length_c                   18.2282(5)
_cell_measurement_reflns_used    4547
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     1097.39(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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 Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.57005E-2
_diffrn_orient_matrix_UB_12      -0.483834E-1
_diffrn_orient_matrix_UB_13      0.459912E-1
_diffrn_orient_matrix_UB_21      0.115674
_diffrn_orient_matrix_UB_22      0.92825E-1
_diffrn_orient_matrix_UB_23      0.224127E-1
_diffrn_orient_matrix_UB_31      -0.682426E-1
_diffrn_orient_matrix_UB_32      0.780964E-1
_diffrn_orient_matrix_UB_33      0.237707E-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  0.026
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8549
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       needle
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0310P)^2^+1.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3914
_reflns_number_total             4972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0276321-2_s2.cif
_cod_data_source_block           vocl3car
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               4113424