Cationic tungsten-oxo-alkylidene-N-heterocyclic carbene complexes: highly active olefin metathesis catalysts.
Schowner, Roman; Frey, Wolfgang; Buchmeiser, Michael R.; Journal of the American Chemical Society 137 (2015) 6188–6191; doi:10.1021/jacs.5b03788

data_4123663
_publ_section_title
;
 Cationic tungsten-oxo-alkylidene-N-heterocyclic carbene complexes: highly
 active olefin metathesis catalysts.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6188
_journal_page_last               6191
_journal_paper_doi               10.1021/jacs.5b03788
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C39 H47 CL2 N2 O P W, C4 H8 O'
_chemical_formula_sum            'C43 H55 Cl2 N2 O2 P W'
_chemical_formula_weight         917.61
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                103.326(3)
_cell_angle_beta                 96.653(3)
_cell_angle_gamma                102.402(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2691(6)
_cell_length_b                   13.0224(7)
_cell_length_c                   16.5658(9)
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.66
_cell_volume                     2275.1(2)
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40548
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_T_max  0.7147
_exptl_absorpt_correction_T_min  0.4686
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.924
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         10350
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+1.2959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                8952
_reflns_number_total             10350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b03788_si_001.cif
_cod_data_source_block           buch89
_cod_depositor_comments
'Adding full bibliography for 4123661--4123664.cif.'
_cod_database_code               4123663