Activation of Epoxides by a Cooperative Iron‒Thiolate Catalyst: Intermediacy of Ferrous Alkoxides in Catalytic Hydroboration
Song, Heng; Ye, Ke; Geng, Peiyu; Han, Xiao; Liao, Rongzhen; Tung, Chen-Ho; Wang, Wenguang; ACS Catalysis 7 (2017) 7709–; doi:10.1021/acscatal.7b02527

data_4514234
_publ_section_title
;
 Activation of Epoxides by a Cooperative Iron--Thiolate Catalyst:
 Intermediacy of Ferrous Alkoxides in Catalytic Hydroboration
;
_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              7709
_journal_paper_doi               10.1021/acscatal.7b02527
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C28 H32 B Fe P S'
_chemical_formula_sum            'C28 H32 B Fe P S'
_chemical_formula_weight         498.22
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.569(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.433(6)
_cell_length_b                   8.274(3)
_cell_length_c                   18.909(7)
_cell_measurement_reflns_used    3581
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.288
_cell_measurement_theta_min      2.745
_cell_volume                     2556.4(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11863
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.743
_exptl_absorpt_coefficient_mu    0.748
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4502
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3578
_reflns_number_total             4502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02527_si_002.cif
_cod_data_source_block           1H(BH2)
_cod_depositor_comments
'Adding full bibliography for 4514233--4514239.cif.'
_cod_original_cell_volume        2556.4(15)
_cod_database_code               4514234
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C23, C19
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C23, C19
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 B1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C18(H18), C11(H11), C4(H4), C3(H3), C5(H5), C14(H14),
 C8(H8), C17(H17), C15(H15), C16(H16), C6(H6), C12(H12)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'