B(C6F5)3 Activation of Oxo Tungsten Complexes That Are Relevant to Olefin Metathesis
Peryshkov, Dmitry V.; Forrest, William P.; Schrock, Richard R.; Smith, Stacey J.; Müller, Peter; Organometallics 32 (2013) 5256–; doi:10.1021/om4007906

data_4089620
_publ_section_title
;
 B(C6F5)3 Activation of Oxo Tungsten Complexes That Are Relevant to Olefin
 Metathesis
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5256
_journal_paper_doi               10.1021/om4007906
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C52 H58 O3 W, 0.5(C5 H12)'
_chemical_formula_sum            'C54.5 H64 O3 W'
_chemical_formula_weight         950.90
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 95.7210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5802(7)
_cell_length_b                   32.3113(19)
_cell_length_c                   12.4403(7)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.47
_cell_measurement_theta_min      2.52
_cell_volume                     4631.6(5)
_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 0.998
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            152875
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.509
_diffrn_reflns_theta_min         1.762
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    2.536
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6201
_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             1956
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.028
_refine_diff_density_max         5.219
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         15389
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+11.1441P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13014
_reflns_number_total             15389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4007906_si_001.cif
_cod_data_source_block           x8_12132
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C54.50 H64 O3 W'
_cod_database_code               4089620
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2012-9
_shelx_res_checksum              72153
_shelx_hkl_checksum              35312