Pyridine(diimine) Molybdenum-Catalyzed Hydrogenation of Arenes and Hindered Olefins: Insights into Precatalyst Activation and Deactivation Pathways
Joannou, Matthew V.; Bezdek, Máté J.; Chirik, Paul J.; ACS Catalysis 8 (2018) 5276–; doi:10.1021/acscatal.8b00924

data_4515638
_publ_section_title
;
 Pyridine(diimine) Molybdenum-Catalyzed Hydrogenation of Arenes and
 Hindered Olefins: Insights into Precatalyst Activation and Deactivation
 Pathways
;
_journal_issue                   6
_journal_name_full               'ACS Catalysis'
_journal_page_first              5276
_journal_paper_doi               10.1021/acscatal.8b00924
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C37 H47 Mo N3 O'
_chemical_formula_weight         645.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.2310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8128(8)
_cell_length_b                   13.0267(7)
_cell_length_c                   16.0929(8)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.06
_cell_measurement_theta_min      2.77
_cell_volume                     3280.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37309
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.086
_diffrn_reflns_theta_min         3.665
_exptl_absorpt_coefficient_mu    3.509
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+2.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6063
_reflns_number_total             6199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00924_si_003.cif
_cod_data_source_block           mj9
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515638
_shelx_estimated_absorpt_t_min   0.457
_shelx_estimated_absorpt_t_max   0.654
_shelxl_version_number           2014-3
_shelx_res_checksum              30933
_shelx_hkl_checksum              67667