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_4113807
_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         C21H24MoN2O.C6H6
_chemical_formula_sum            'C27 H30 Mo N2 O'
_chemical_formula_weight         494.47
_chemical_name_common            'Cp*Mo(NO)(h2-C6H4)(NC5H5).benzene (9)'
_chemical_name_systematic
;
Molybdenum,[(5,6-.eta.)-1,3-cyclohexadien-5-yne]nitrosyl
[(5-.eta.)pentamethylcyclopentadienyl](pyridine)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8177(4)
_cell_length_b                   14.3141(9)
_cell_length_c                   20.5603(10)
_cell_measurement_temperature    173(2)
_cell_volume                     2300.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5080
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.591
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                3987
_reflns_number_total             5080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0349094si20030227_045859.cif
_cod_data_source_block           pl240
_cod_database_code               4113807