Redox-Noninnocent Ligand-Supported Vanadium Catalysts for the Chemoselective Reduction of C═X (X = O, N) Functionalities.
Zhang, Guoqi; Wu, Jing; Zheng, Shengping; Neary, Michelle C.; Mao, Jincheng; Flores, Marco; Trovitch, Ryan J.; Dub, Pavel A.; Journal of the American Chemical Society 141 (2019) 15230–15239; doi:10.1021/jacs.9b07062

data_4129020
_publ_section_title
;
 Redox-Noninnocent Ligand-Supported Vanadium Catalysts for the
 Chemoselective Reduction of C&#x2550;X (X = O, N) Functionalities.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15230
_journal_page_last               15239
_journal_paper_doi               10.1021/jacs.9b07062
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C29 H37 N3 Si2 V'
_chemical_formula_sum            'C29 H37 N3 Si2 V'
_chemical_formula_weight         534.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.164(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9192(11)
_cell_length_b                   9.2597(5)
_cell_length_c                   19.7266(12)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.41
_cell_volume                     2907.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66883
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.290
_diffrn_reflns_theta_min         2.407
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         8044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+1.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5562
_reflns_number_total             8044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07062_si_004.cif
_cod_data_source_block           gz1130
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129020
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.792
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              38828
_shelx_hkl_checksum              4326