N-Heterocyclic Carbene-Induced Transmethylation in Tungsten Imido Alkylidene Bistriflates: Unexpected Formation of an N-Heterocyclic Olefin Complex
Imbrich, Dominik; Frey, Wolfgang; Buchmeiser, Michael R.; Chem. Commun.  (2017) –; doi:10.1039/C7CC07471A

data_7120801
_publ_section_title
;
 N-Heterocyclic Carbene-Induced Transmethylation in Tungsten Imido
 Alkylidene Bistriflates: Unexpected Formation of an N-Heterocyclic Olefin
 Complex
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07471A
_journal_year                    2017
_chemical_formula_moiety         'C46 H57 F6 N3 O6 S2 W, C4 H10 O'
_chemical_formula_sum            'C50 H67 F6 N3 O7 S2 W'
_chemical_formula_weight         1184.04
_chemical_name_systematic
; 
 complex 4 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_audit_update_record
;
2017-07-05 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                79.289(3)
_cell_angle_beta                 83.831(4)
_cell_angle_gamma                65.484(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0693(8)
_cell_length_b                   12.9179(9)
_cell_length_c                   18.8210(13)
_cell_measurement_reflns_used    13826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      1.75
_cell_volume                     2621.8(3)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76602
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.8642
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker,2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.946
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         15994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+2.6339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                13826
_reflns_number_total             15994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc07471a2.cif
_cod_data_source_block           buch98
_cod_database_code               7120801