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_4514235
_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_sum            'C36 H44 B Fe P S'
_chemical_formula_weight         606.40
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 96.035(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.130(9)
_cell_length_b                   11.240(9)
_cell_length_c                   23.290(18)
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.352
_cell_measurement_theta_min      2.498
_cell_volume                     3158(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS Inc.,2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1503
_diffrn_reflns_av_unetI/netI     0.1514
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21625
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.477
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1415 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.6493.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5549
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2734
_reflns_number_total             5549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02527_si_002.cif
_cod_data_source_block           1H(BBN)
_cod_depositor_comments
'Adding full bibliography for 4514233--4514239.cif.'
_cod_database_code               4514235
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              6608
_shelx_hkl_checksum              31254