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_4084686
_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_moiety         'C77 H66 Cl3 N O2 W, 0.5(C4 H10 O)'
_chemical_formula_sum            'C79 H71 Cl3 N O2.5 W'
_chemical_formula_weight         1364.56
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                87.484(3)
_cell_angle_beta                 88.749(3)
_cell_angle_gamma                69.065(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8493(18)
_cell_length_b                   13.6749(19)
_cell_length_c                   20.269(3)
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      2.69
_cell_volume                     3323.1(8)
_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-2012 (Sheldrick, 2012)'
_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 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            108220
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.596
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.112
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         20238
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.1405P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16354
_reflns_number_total             20238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5006676_si_001.cif
_cod_data_source_block           X8_13201
_cod_original_cell_volume        3323.2(8)
_cod_original_formula_sum        'C79 H71 Cl3 N O2.50 W'
_cod_database_code               4084686
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2012-9
_shelx_res_checksum              73201
_shelx_hkl_checksum              22058