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_4089621
_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         'C61 H84 O3 W, 0.79(C5 H12)'
_chemical_formula_sum            'C64.96 H93.5 O3 W'
_chemical_formula_weight         1106.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 102.7040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.8965(16)
_cell_length_b                   22.8988(16)
_cell_length_c                   24.2316(17)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.48
_cell_volume                     12935.0(15)
_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 1.000
_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  0.0741
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            171463
_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         29.130
_diffrn_reflns_theta_min         1.246
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4650
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.768
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         17408
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+53.4547P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12556
_reflns_number_total             17408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4007906_si_002.cif
_cod_data_source_block           x13008_sq_s
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C64.96 H93.50 O3 W'
_cod_database_code               4089621
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.931
_shelxl_version_number           2012-9
_shelx_res_checksum              7304
_shelx_hkl_checksum              49614
_shelx_fab_checksum              94010