Pincer Iron Hydride Complexes for Alkene Isomerization: Catalytic Approach to Trisubstituted (Z)-Alkenyl Boronates
Xu, Songgen; Geng, Peiyu; Li, Yuling; Liu, Guixia; Zhang, Lei; Guo, Yinlong; Huang, Zheng; ACS Catalysis  (2021) 10138–10147; doi:10.1021/acscatal.1c02432

data_4518927
_publ_section_title
;
 Pincer Iron Hydride Complexes for Alkene Isomerization: Catalytic
 Approach to Trisubstituted (Z)-Alkenyl Boronates
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10138
_journal_page_last               10147
_journal_paper_doi               10.1021/acscatal.1c02432
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C27 H40 Cl2 Fe N3 P'
_chemical_formula_sum            'C27 H40 Cl2 Fe N3 P'
_chemical_formula_weight         564.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.8090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3707(3)
_cell_length_b                   11.8804(3)
_cell_length_c                   12.9994(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.920
_cell_measurement_theta_min      3.060
_cell_volume                     1399.12(7)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      172.99
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12920
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.907
_diffrn_reflns_theta_min         3.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.524
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1689 before and 0.0776 after correction. The Ratio of minimum to maximum transmission is 0.7056. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.027(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0103P)^2^+0.1889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4204
_reflns_number_total             4454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c02432_si_002.cif
_cod_data_source_block           mj19774_0m
_cod_database_code               4518927
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.973(7)
 0.027(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C27: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C25(0.75) H25A(0.75) H25B(0.75) H25C(0.75) C26(0.75) H26A(0.75)
 H26B(0.75) H26C(0.75) C27(0.75) H27A(0.75) H27B(0.75) H27C(0.75) C28(0.25)
 H28A(0.25) H28B(0.25) H28C(0.25) C29(0.25) H29A(0.25) H29B(0.25) H29C(0.25)
 C30(0.25) H30A(0.25) H30B(0.25) H30C(0.25)
5.a Ternary CH refined with riding coordinates:
 C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              81383
_shelx_hkl_checksum              63280
_olex2_submission_special_instructions 'No special instructions were received'