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_4113804
_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         C20H30MoN2O
_chemical_formula_sum            'C20 H30 Mo N2 O'
_chemical_formula_weight         410.40
_chemical_name_common            'Cp*Mo(NO)(=CHCMe3)(NC5H5) (8)'
_chemical_name_systematic
; 
Molybdenum,(2,2-dimethylpropylidene)nitrosyl
[(5-.eta.)pentamethylcyclopentadienyl](pyridine)  
;
_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                81.399(9)
_cell_angle_beta                 79.463(8)
_cell_angle_gamma                69.442(8)
_cell_formula_units_Z            2
_cell_length_a                   8.372(4)
_cell_length_b                   8.944(5)
_cell_length_c                   14.795(8)
_cell_measurement_temperature    160(2)
_cell_volume                     1015.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6036
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.654
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.0000(17)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          11.146
_refine_ls_shift/su_mean         0.050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.2326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                3880
_reflns_number_total             4277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0349094si20030227_045807.cif
_cod_data_source_block           bau02
_cod_database_code               4113804