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_4515639
_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            'C47 H60 Mo N5 O'
_chemical_formula_weight         806.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.0833(7)
_cell_length_b                   33.7453(7)
_cell_length_c                   17.8428(4)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      3.12
_cell_volume                     19317.7(7)
_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 0.976
_diffrn_measured_fraction_theta_max 0.993
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25101
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.721
_diffrn_reflns_theta_min         3.122
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             6832
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+9.2646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                7815
_reflns_number_total             8279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00924_si_003.cif
_cod_data_source_block           mj10
_cod_database_code               4515639
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.832
_shelxl_version_number           2014-3
_shelx_res_checksum              15108
_shelx_hkl_checksum              69562
_shelx_fab_checksum              91264