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_4514233
_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         'C30 H32 Fe N P S'
_chemical_formula_sum            'C30 H32 Fe N P S'
_chemical_formula_weight         525.44
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-24
_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                 95.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7631(3)
_cell_length_b                   9.2957(2)
_cell_length_c                   35.3175(8)
_cell_measurement_reflns_used    5013
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.9590
_cell_measurement_theta_min      5.0350
_cell_volume                     5149.07(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     43.00  68.00   1.00    1.47    --    0.00  57.00  90.00   25
  2  \w    -14.00  26.00   1.00    5.88    --   54.00 -57.00 120.00   40
  3  \w     28.00 107.00   1.00    5.88    --   54.00-122.00  60.00   79
  4  \w     42.00  95.00   1.00    5.88    --  108.00-111.00  90.00   53
  5  \w     36.00 145.00   1.00    5.88    --  108.00 -91.00 120.00  109
  6  \w     61.00 130.00   1.00    5.88    --  108.00 -63.00 -90.00   69
  7  \w     87.00 153.00   1.00    5.88    --  108.00  63.00 -90.00   66
  8  \w    141.00 167.00   1.00    5.88    --  108.00 111.00  30.00   26
  9  \w    115.00 147.00   1.00    5.88    --  108.00 178.00 120.00   32
 10  \w     86.00 165.00   1.00    5.88    --  108.00  77.00  30.00   79
 11  \w     72.00 114.00   1.00    5.88    --  108.00 178.00-180.00   42
 12  \w     34.00 122.00   1.00    5.88    --   54.00  57.00 -90.00   88
 13  \w     61.00  93.00   1.00    5.88    --  108.00 178.00 120.00   32
 14  \w    -20.00  13.00   1.00    1.47    --    0.00  57.00  90.00   33
 15  \w    -66.00 -18.00   1.00    1.47    --    0.00 151.00 -56.00   48
 16  \w     16.00  75.00   1.00    5.88    --   54.00 -37.00 -90.00   59
 17  \w    -10.00  24.00   1.00    1.47    --    0.00 -77.00-150.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245685000
_diffrn_orient_matrix_UB_12      -0.1559454000
_diffrn_orient_matrix_UB_13      0.0088045000
_diffrn_orient_matrix_UB_21      -0.0052959000
_diffrn_orient_matrix_UB_22      -0.0367127000
_diffrn_orient_matrix_UB_23      -0.0427296000
_diffrn_orient_matrix_UB_31      0.0949313000
_diffrn_orient_matrix_UB_32      -0.0423310000
_diffrn_orient_matrix_UB_33      0.0044831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            9732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.966
_diffrn_reflns_theta_min         4.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.174
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+4.9897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             4874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02527_si_002.cif
_cod_data_source_block           1(NCMe)
_cod_depositor_comments
'Adding full bibliography for 4514233--4514239.cif.'
_cod_original_cell_volume        5149.1(2)
_cod_database_code               4514233
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Me refined with riding coordinates:
 C2(H2A,H2B,H2C)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.363
_oxdiff_exptl_absorpt_empirical_full_min 0.752