Synthesis of Molybdenum Alkylidene Complexes That Contain the 2,6-Dimesitylphenylimido Ligand
Laura C. H. Gerber; Richard R. Schrock; Peter Müller; Michael K. Takase; Journal of the American Chemical Society 133 (2011) 18142–18144; doi:10.1021/ja208936s

data_4107129
_publ_section_title
;
 Synthesis of Molybdenum Alkylidene Complexes That Contain the
 2,6-Dimesitylphenylimido Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18142
_journal_page_last               18144
_journal_paper_doi               10.1021/ja208936s
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C68.5 H78.5 Cl Mo N2 O2'
_chemical_formula_weight         1093.22
_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                71.259(5)
_cell_angle_beta                 87.158(5)
_cell_angle_gamma                68.692(5)
_cell_formula_units_Z            4
_cell_length_a                   16.251(3)
_cell_length_b                   16.403(4)
_cell_length_c                   24.476(5)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.22
_cell_measurement_theta_min      2.51
_cell_volume                     5739(2)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            248510
_diffrn_reflns_theta_full        30.32
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.9533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             2314
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1848
_refine_ls_number_reflns         34398
_refine_ls_number_restraints     2819
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0353P)^2^+5.4040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                23909
_reflns_number_total             34398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208936s_si_002_3.cif
_cod_data_source_block           x11073
_cod_original_cell_volume        5740(2)
_cod_original_formula_sum        'C68.50 H78.50 Cl Mo N2 O2'
_cod_database_code               4107129