Tungsten(II) Alkylimido Complexes from Insertion of Nitriles into Tungsten Hydride: Alkylideneamido Intermediate Stage and Nitrene Group Transfer to Isocyanide
Dai, Qi Xiu; Seino, Hidetake; Mizobe, Yasushi; Organometallics 31 (2012) 4933–; doi:10.1021/om3004338

data_4078818
_publ_section_title
;
 Tungsten(II) Alkylimido Complexes from Insertion of Nitriles into
 Tungsten Hydride: Alkylideneamido Intermediate Stage and Nitrene Group
 Transfer to Isocyanide
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4933
_journal_paper_doi               10.1021/om3004338
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C61 H59 N P4 W '
_chemical_formula_sum            'C61 H59 N P4 W'
_chemical_formula_weight         1113.89
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.2664(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.834(5)
_cell_length_b                   10.813(3)
_cell_length_c                   25.316(7)
_cell_measurement_reflns_used    9161
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.0
_cell_volume                     5088(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      113.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28126
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.39
_refine_diff_density_min         -2.01
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5785 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.020(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     670
_refine_ls_number_reflns         11843
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.0070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.2000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0442
_reflns_number_gt                10902
_reflns_number_total             11843
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3004338_si_002.cif
_cod_data_source_block           '__[W(NCH2Tol)(P4)]_toluene'
_cod_original_formula_sum        'C61 H59 N P4 W '
_cod_database_code               4078818