Application of imidazolinium salts and N-heterocyclic olefins for the synthesis of anionic and neutral tungsten imido alkylidene complexes
Dominik A. Imbrich; Wolfgang Frey; Stefan Naumann; Michael R. Buchmeiser; Chem.Commun. 52 (2016) 6099–; doi:

data_7119050
_publ_section_title
;
 Application of imidazolinium salts and N-heterocyclic olefins for the
 synthesis of anionic and neutral tungsten imido alkylidene complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6099
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C28 H37 Cl2 N2 W, C27 H39 N2'
_chemical_formula_sum            'C55 H76 Cl2 N4 W'
_chemical_formula_weight         1047.95
_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
;
2016-03-01 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.879(2)
_cell_angle_beta                 81.476(2)
_cell_angle_gamma                88.576(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5591(3)
_cell_length_b                   13.6270(5)
_cell_length_c                   21.2326(7)
_cell_measurement_reflns_used    12720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      1.74
_cell_volume                     3016.47(17)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52893
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         14996
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                12720
_reflns_number_total             14996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc02483a2.cif
_cod_data_source_block           buch151
_cod_database_code               7119050