A <i>cis</i>-β-iron(III) SALPN catalyst for hydrogen atom transfer reductions and olefin cross couplings.
Ricca, Michael; Yao, Shaolei; Le, Tommy; White, Jonathan M.; Donnelly, Paul S.; Rizzacasa, Mark A.; Organic & biomolecular chemistry 21 (2023) 6789–6793; doi:10.1039/d3ob01085f

data_7159513
_publ_section_title
;
 A <i>cis</i>-&#x3b2;-iron(III) SALPN catalyst for hydrogen atom transfer
 reductions and olefin cross couplings.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6789
_journal_page_last               6793
_journal_paper_doi               10.1039/d3ob01085f
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C25 H34 O4 Si'
_chemical_formula_sum            'C25 H34 O4 Si'
_chemical_formula_weight         426.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5438(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.35425(16)
_cell_length_b                   11.58392(18)
_cell_length_c                   21.9396(3)
_cell_measurement_reflns_used    75174
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      50.0060
_cell_measurement_theta_min      2.5430
_cell_volume                     2372.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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    -44.00 -19.00   0.50    5.00    --  -30.00 -54.00  73.13   50
  2  \w    -46.00 -21.00   0.50    5.00    --  -34.00 -53.00 109.71   50
  3  \w    -53.00 -24.00   0.50    5.00    --  -38.00 -50.00 141.79   58
  4  \w    -70.00 -42.00   0.50    5.00    --  -54.42 -46.00  50.15   56
  5  \w    -72.00 -42.00   0.50    5.00    --  -54.42 -45.00 -36.38   60
  6  \w    -50.00 -24.00   0.50    5.00    --  -38.00 -51.00 -42.59   52
  7  \w    -50.00 -24.00   0.50    5.00    --  -38.00 -51.00 -99.08   52
  8  \w    -49.00 -24.00   0.50    5.00    --  -38.00 -51.00-153.47   50
  9  \w    -71.00 -44.00   0.50    5.00    --  -54.42 -45.00-133.91   54
 10  \w   -110.00 -42.00   0.50    5.00    --  -54.42 -44.00-106.58  136
 11  \w    -87.00 -42.00   0.50    5.00    --  -54.42 -44.00  22.27   90
 12  \w   -109.00 -42.00   0.50    5.00    --  -54.42 -46.00 159.42  134
 13  \w   -121.00 -41.00   0.50    5.00    --  -54.00 -46.00  92.21  160
 14  \w   -122.00 -41.00   0.50    5.00    --  -54.00 -46.00 -66.89  162
 15  \w     -7.00  20.00   0.50    2.00    --   14.00  72.00  69.73   54
 16  \w     20.00  46.00   0.50    5.00    --   34.00  53.00 146.66   52
 17  \w     95.00 122.00   0.50    5.00    --   55.35 125.00  30.00   54
 18  \w     81.00 106.00   0.50    5.00    --   55.35 113.00-108.00   50
 19  \w     -8.00  17.00   0.50    2.00    --   14.00  75.00-103.04   50
 20  \w    -77.00  13.00   0.50    5.00    --  -54.42  77.00-150.00  180
 21  \w    -95.00 -41.00   0.50    5.00    --  -54.42 125.00   0.00  108
 22  \w    -96.00 -35.00   0.50    5.00    --  -54.42 113.00-108.00  122
 23  \w     10.00  75.00   0.50    5.00    --   55.35-113.00 159.00  130
 24  \w     17.00  74.00   0.50    5.00    --   55.35-125.00 150.00  114
 25  \w     19.00  85.00   0.50    5.00    --   55.35-125.00   0.00  132
 26  \w    -16.00  37.00   0.50    5.00    --   55.35 -57.00  30.00  106
 27  \w    -16.00  18.00   0.50    5.00    --   55.35 -57.00  60.00   68
 28  \w    -16.00  36.00   0.50    5.00    --   55.35 -57.00 -30.00  104
 29  \w    -12.00  34.00   0.50    5.00    --   55.35 -57.00-120.00   92
 30  \w    -15.00  40.00   0.50    5.00    --   55.35 -57.00-180.00  110
 31  \w    -95.00 -39.00   0.50    5.00    --  -54.42 125.00 -30.00  112
 32  \w    -59.00 -34.00   0.50    5.00    --  -54.42 125.00 150.00   50
 33  \w   -101.00 -64.00   0.50    5.00    --  -54.42 125.00 150.00   74
 34  \w   -125.00 -41.00   0.50    5.00    --  -54.00 -46.00  -1.39  168
 35  \w   -119.00 -42.00   0.50    5.00    --  -54.42 -46.00 119.29  154
 36  \w   -126.00 -74.00   0.50    5.00    --  -54.42 -46.00  50.15  104
 37  \w   -126.00 -81.00   0.50    5.00    --  -54.42 -45.00 -36.38   90
 38  \w   -126.00 -81.00   0.50    5.00    --  -54.42 -45.00-133.91   90
 39  \w   -126.00 -42.00   0.50    5.00    --  -54.42 -46.00-163.19  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271475000
_diffrn_orient_matrix_UB_12      -0.0124933000
_diffrn_orient_matrix_UB_13      0.0287574000
_diffrn_orient_matrix_UB_21      0.0706620000
_diffrn_orient_matrix_UB_22      0.0005976000
_diffrn_orient_matrix_UB_23      0.0137120000
_diffrn_orient_matrix_UB_31      -0.0063164000
_diffrn_orient_matrix_UB_32      0.0599491000
_diffrn_orient_matrix_UB_33      0.0058574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            278224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         51.415
_diffrn_reflns_theta_min         2.181
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         26138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0705P)^2^+0.1478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14765
_reflns_number_total             26138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01085f2.cif
_cod_data_source_block           jmwmr636_mo_abs
_cod_depositor_comments
'Adding full bibliography for 7159510--7159513.cif.'
_cod_original_cell_volume        2372.80(7)
_cod_database_code               7159513
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H34 O4 Si'
_chemical_oxdiff_usercomment     Lactone
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C18(H18), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C2(H2), C16(H16), C6(H6), C3(H3), C14(H14), C5(H5), C15(H15),
 C13(H13), C4(H4)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C10(H10A,H10B,H10C),
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              32686
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.596