Intermolecular Activation of Hydrocarbon C-H Bonds under Ambient Conditions by 16-Electron Neopentylidene and Benzyne Complexes of Molybdenum
Kenji Wada; Craig B. Pamplin; Peter Legzdins; Brian O. Patrick; Irina Tsyba; Robert Bau; Journal of the American Chemical Society 125 (2003) 7035–7048; doi:10.1021/ja0349094

data_4113803
_publ_section_title
;
 Intermolecular Activation of Hydrocarbon C-H Bonds under Ambient
 Conditions by 16-Electron Neopentylidene and Benzyne Complexes of
 Molybdenum
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7035
_journal_page_last               7048
_journal_paper_doi               10.1021/ja0349094
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         C20H37MoNO
_chemical_formula_sum            'C20 H37 Mo N O'
_chemical_formula_weight         403.45
_chemical_name_common            'Cp*Mo(NO)(CH2CMe3)2 (1)'
_chemical_name_systematic
; 
Molybdenum,bis(2,2-dimethylpropyl)nitrosyl
[(5-.eta.)pentamethylcyclopentadienyl]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.610(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9121(17)
_cell_length_b                   21.702(4)
_cell_length_c                   11.260(2)
_cell_measurement_reflns_used    6358
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.55
_cell_volume                     2097.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12541
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          7.589
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+2.1158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                3798
_reflns_number_total             4652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0349094si20030227_045749.cif
_cod_data_source_block           bau01
_cod_original_cell_volume        2097.4(7)
_cod_database_code               4113803