The Reactivity of Mo(PMe3)6 towards Heterocyclic Nitrogen Compounds: Transformations Relevant to Hydrodenitrogenation
Guang Zhu; Joseph M. Tanski; David G. Churchill; Kevin E. Janak; Gerard Parkin; Journal of the American Chemical Society 124 (2002) 13658–13659; doi:10.1021/ja028512w

data_4115324
_publ_section_title
;
 The Reactivity of Mo(PMe3)6 towards Heterocyclic Nitrogen Compounds:
 Transformations Relevant to Hydrodenitrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13658
_journal_page_last               13659
_journal_paper_doi               10.1021/ja028512w
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C18 H34 Mo N P3'
_chemical_formula_weight         453.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.604(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.891(2)
_cell_length_b                   18.871(3)
_cell_length_c                   16.272(3)
_cell_measurement_temperature    243(2)
_cell_volume                     4424.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      243(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28747
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.8548
_exptl_absorpt_correction_T_min  0.8548
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00000(6)
_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   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.817
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+1.0130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                7390
_reflns_number_total             10050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028512w-2_s5.cif
_cod_data_source_block           gzs10
_cod_database_code               4115324