Synthesis of Tungsten Imido Alkylidene Complexes that Contain an Electron-Withdrawing Imido Ligand.
Axtell, Jonathan C.; Schrock, Richard R.; Müller, Peter; Smith, Stacey J.; Hoveyda, Amir H.; Organometallics 33 (2014) 5342–5348; doi:10.1021/om5006676

data_4084684
_publ_section_title
;
 Synthesis of Tungsten Imido Alkylidene Complexes that Contain an
 Electron-Withdrawing Imido Ligand.
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5342
_journal_page_last               5348
_journal_paper_doi               10.1021/om5006676
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C52 H56 F24 N4 W2'
_chemical_formula_weight         1560.70
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.329(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8640(19)
_cell_length_b                   14.775(2)
_cell_length_c                   14.478(2)
_cell_measurement_reflns_used    9532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.36
_cell_volume                     2941.5(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            82838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         1.915
_diffrn_source                   'fine-focus sealed tube, graphite'
_exptl_absorpt_coefficient_mu    4.022
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     617
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.8287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8241
_reflns_number_total             8967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5006676_si_001.cif
_cod_data_source_block           14011
_cod_original_cell_volume        2941.6(7)
_cod_database_code               4084684
_shelx_estimated_absorpt_t_min   0.259
_shelx_estimated_absorpt_t_max   0.623
_shelxl_version_number           2013-4
_shelx_res_checksum              74306
_shelx_hkl_checksum              94671