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_7120802
_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 H62 N3 O2 W, C F3 O3 S'
_chemical_formula_sum            'C47 H62 F3 N3 O5 S W'
_chemical_formula_weight         1021.91
_chemical_name_systematic
; 
complex 2 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.557(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2173(8)
_cell_length_b                   17.5402(9)
_cell_length_c                   17.1966(9)
_cell_measurement_reflns_used    11172
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      1.71
_cell_volume                     4609.4(4)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52954
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.611
_exptl_absorpt_correction_T_max  0.6048
_exptl_absorpt_correction_T_min  0.4304
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         9.946
_refine_diff_density_min         -2.192
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         13998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+35.0921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                11172
_reflns_number_total             13998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc07471a2.cif
_cod_data_source_block           buch191
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7120802