Synthesis of Methylidene Complexes that Contain a 2,6-Dimesitylphenylimido Ligand and Ethenolysis of 2,3-Dicarbomethoxynorbornadiene
Gerber, Laura C. H.; Schrock, Richard R.; Organometallics 32 (2013) 5573–; doi:10.1021/om400844k

data_4081695
_publ_section_title
;
 Synthesis of Methylidene Complexes that Contain a
 2,6-Dimesitylphenylimido Ligand and Ethenolysis of
 2,3-Dicarbomethoxynorbornadiene
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5573
_journal_paper_doi               10.1021/om400844k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C49 H50 N2 O Si W'
_chemical_formula_weight         894.85
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.836(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6649(12)
_cell_length_b                   23.348(3)
_cell_length_c                   16.8858(19)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.49
_cell_measurement_theta_min      2.49
_cell_volume                     4195.2(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2010)'
_computing_data_collection       'APEX2 v2010.7.0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2010)'
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            145022
_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         30.999
_diffrn_reflns_theta_min         1.490
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.4339
_exptl_absorpt_correction_T_min  0.3390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         13374
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+3.8688P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11927
_reflns_number_total             13374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400844k_si_002.cif
_cod_data_source_block           x13095a
_cod_original_cell_volume        4195.2(8)
_cod_database_code               4081695
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.728