Cooperative Molybdenum-Thiolate Reactivity for Transfer Hydrogenation of Nitriles
Hou, Shu-Fen; Chen, Jia-Yi; Xue, Minghui; Jia, Mengjing; Zhai, Xiaofang; Liao, Rong-Zhen; Tung, Chen-Ho; Wang, Wenguang; ACS Catalysis  (2019) 380–; doi:10.1021/acscatal.9b04455

data_4517182
_publ_section_title
;
 Cooperative Molybdenum-Thiolate Reactivity for Transfer Hydrogenation of
 Nitriles
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              380
_journal_paper_doi               10.1021/acscatal.9b04455
_journal_year                    2019
_chemical_formula_moiety         'C30 H29 Mo O2 P S'
_chemical_formula_sum            'C30 H29 Mo O2 P S'
_chemical_formula_weight         580.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.224(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.389(5)
_cell_length_b                   15.694(4)
_cell_length_c                   17.490(4)
_cell_measurement_reflns_used    3226
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      26.590
_cell_measurement_theta_min      2.374
_cell_volume                     5220(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18443
_diffrn_reflns_theta_full        25.3171
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0545 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.9241.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.4772
_exptl_crystal_description       block
_exptl_crystal_F_000             2372.7616
_refine_diff_density_max         0.5759
_refine_diff_density_min         -0.4627
_refine_diff_density_rms         0.1167
_refine_ls_d_res_high            0.8302
_refine_ls_d_res_low             12.1049
_refine_ls_goodness_of_fit_ref   1.0553
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0553
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+7.7839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3743
_reflns_number_total             4771
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            cs9b04455_si_002.cif
_cod_data_source_block           p
_cod_database_code               4517182
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C26(H26), C30(H30), C17(H17), C20(H20), C24(H24), C23(H23),
 C28(H28), C21(H21), C29(H29), C16(H16), C22(H22), C15(H15), C27(H27)
2.b Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C6(H6a,H6b,H6c), C8(H8a,H8b,H8c),
 C7(H7a,H7b,H7c)
;
_olex2_submission_special_instructions 'No special instructions were received'