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_4514238
_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         'C29 H29 Fe O P S'
_chemical_formula_sum            'C29 H29 Fe O P S'
_chemical_formula_weight         512.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2n -2ac'
_space_group_name_H-M_alt        'P c 21 n'
_symmetry_space_group_name_Hall  'P -2n -2ac'
_symmetry_space_group_name_H-M   'P c 21 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-07
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1455(6)
_cell_length_b                   14.4475(9)
_cell_length_c                   16.7227(12)
_cell_measurement_reflns_used    7530
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.622
_cell_measurement_theta_min      2.739
_cell_volume                     2451.2(3)
_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     0.710
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14705
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.346
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8459.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.031(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4270
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                3654
_reflns_number_total             4270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02527_si_002.cif
_cod_data_source_block           1(CO)
_cod_depositor_comments
'Adding full bibliography for 4514233--4514239.cif.'
_cod_database_code               4514238
_shelxl_version_number           2013-4
_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:
 C7(H7), C18(H18), C15(H15), C19(H19), C6(H6), C16(H16), C9(H9), C13(H13),
 C4(H4), C11(H11), C17(H17), C12(H12), C10(H10), C5(H5)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'