New Modes for Coordination of Aromatic Heterocyclic Nitrogen Compounds to Molybdenum: Catalytic Hydrogenation of Quinoline, Isoquinoline, and Quinoxaline by Mo(PMe3)4H4
Guang Zhu; Keliang Pang; Gerard Parkin; Journal of the American Chemical Society 130 (2008) 1564–1565; doi:10.1021/ja078102d

data_4107385
_publ_section_title
;
 New Modes for Coordination of Aromatic Heterocyclic Nitrogen Compounds to
 Molybdenum: Catalytic Hydrogenation of Quinoline, Isoquinoline, and
 Quinoxaline by Mo(PMe3)4H4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1564
_journal_page_last               1565
_journal_paper_doi               10.1021/ja078102d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C21 H43 Mo N P4'
_chemical_formula_weight         529.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   12.4605(18)
_cell_length_b                   16.177(3)
_cell_length_c                   27.824(4)
_cell_measurement_temperature    243(2)
_cell_volume                     5608.6(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1260
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34063
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.9330
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.819
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00086(14)
_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   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                2947
_reflns_number_total             5737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078102d-file006.cif
_cod_data_source_block           iqmos20
_cod_database_code               4107385