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_4107390
_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            'C17 H33 Mo N2 P3'
_chemical_formula_weight         454.30
_chemical_name_common            qoxMoP3
_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                 97.630(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9472(12)
_cell_length_b                   13.4906(9)
_cell_length_c                   18.0490(12)
_cell_measurement_temperature    243(2)
_cell_volume                     4331.3(5)
_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 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28133
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.6919
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0050(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   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                8086
_reflns_number_total             9693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078102d-file011.cif
_cod_data_source_block           gedsgs10
_cod_database_code               4107390