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_7159510
_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         'C26 H31 Fe N2 O6, H2 O, C H4 O'
_chemical_formula_sum            'C27 H37 Fe N2 O8'
_chemical_formula_weight         573.43
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2d049w
_audit_creation_date             2022-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.177(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2988(4)
_cell_length_b                   29.2753(7)
_cell_length_c                   8.8713(3)
_cell_measurement_reflns_used    17911
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      33.7170
_cell_measurement_theta_min      2.3460
_cell_volume                     2787.98(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      100.0(2)
_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 0.862
_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    -28.00  54.00   0.50   10.00    --  -12.24  65.00  63.00  164
  2  \w      2.00  85.00   0.50   10.00    --   12.86  65.00  63.00  166
  3  \w    -59.00   3.00   0.50   10.00    --  -12.24 -57.00 120.00  124
  4  \w    -84.00  -1.00   0.50   10.00    --  -12.24 -65.00 -71.00  166
  5  \w    -59.00 -11.00   0.50   10.00    --   12.86 -19.00-120.00   96
  6  \w     46.00  85.00   0.50   10.00    --   12.86-178.00  60.00   78
  7  \w     46.00  84.00   0.50   10.00    --   12.86-178.00 -90.00   76
;
_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      0.0002097000
_diffrn_orient_matrix_UB_12      0.0180213000
_diffrn_orient_matrix_UB_13      -0.0533442000
_diffrn_orient_matrix_UB_21      0.0658976000
_diffrn_orient_matrix_UB_22      -0.0011320000
_diffrn_orient_matrix_UB_23      0.0224005000
_diffrn_orient_matrix_UB_31      -0.0043760000
_diffrn_orient_matrix_UB_32      -0.0161561000
_diffrn_orient_matrix_UB_33      -0.0610543000
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.669
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.193
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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 dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0349P)^2^+1.0254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7117
_reflns_number_total             9552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01085f2.cif
_cod_data_source_block           jmwmr202_mo_abs
_cod_depositor_comments
'Adding full bibliography for 7159510--7159513.cif.'
_cod_database_code               7159510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H37 N2 O8 Fe'
_chemical_oxdiff_usercomment     'Fe(SALPN)acac complex from iPrOH'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.754
_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 Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C20(H20A,H20B), C10(H10A,H10B), C2(H2A,H2B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C6(H6), C9(H9), C13(H13), C17(H17), C15(H15), C4(H4), C16(H16),
 C5(H5)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C27(H27A,H27B,
 H27C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              37852
_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 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.750