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_4515640
_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_moiety         'C41 H65 Mo N3 Si2'
_chemical_formula_sum            'C41 H65 Mo N3 Si2'
_chemical_formula_weight         752.08
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 115.2300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2640(2)
_cell_length_b                   17.5505(2)
_cell_length_c                   23.2268(3)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.81
_cell_measurement_theta_min      4.21
_cell_volume                     4153.65(11)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 2008)'
_computing_data_collection       'BRUKER APEX II software suite (Bruker AXS)'
_computing_data_reduction        'BRUKER APEX II software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Farrugia, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25954
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.10
_diffrn_reflns_theta_min         3.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.350
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs 2008/2'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+3.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                6294
_reflns_number_total             7047
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cs8b00924_si_003.cif
_cod_data_source_block           zrt40
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4153.65(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4515640