C(sp3)-H Oxidation and Chlorination Catalysed by A Bioinspired Pincer Iron(III) Complex
Han, Jian; Tan, Liming; Wan, Yanjun; Li, Gang; Anderson, Stephen N.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02005J

data_7710768
_publ_section_title
;
 C(sp3)-H Oxidation and Chlorination Catalysed by A Bioinspired Pincer
 Iron(III) Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02005J
_journal_year                    2022
_chemical_formula_moiety         'C30 H22 Cl2 Fe N3 O2'
_chemical_formula_sum            'C30 H22 Cl2 Fe N3 O2'
_chemical_formula_weight         1166.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                78.630(3)
_cell_angle_beta                 79.475(3)
_cell_angle_gamma                89.481(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3885(3)
_cell_length_b                   13.9248(4)
_cell_length_c                   16.7200(7)
_cell_measurement_reflns_used    10206
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.8150
_cell_measurement_theta_min      1.8120
_cell_volume                     2554.73(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.951
_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     24.00 101.00   0.50   64.83    --   20.00  54.00   0.00  154
  2  \w    -72.00 -47.00   0.50   64.83    --   20.00  54.00-150.00   50
  3  \w    -34.00  50.00   0.50   64.83    --   20.00  54.00-150.00  168
  4  \w     71.00 110.00   0.50   64.83    --   20.00  54.00-150.00   78
  5  \w    -71.00 109.00   0.50   64.83    --   20.00  54.00 111.66  360
  6  \w    -72.00  66.00   0.50   64.83    --   20.00  54.00 -85.81  276
  7  \w     72.00  97.00   0.50   64.83    --   20.00  54.00 -85.81   50
  8  \w    -68.00  46.00   0.50   64.83    --   20.00  54.00 150.00  228
  9  \w     58.00  84.00   0.50   64.83    --   20.00  54.00 150.00   52
 10  \w    -71.00   2.00   0.50   64.83    --   20.00  54.00  60.00  146
 11  \w     10.00  36.00   0.50   64.83    --   20.00  54.00  60.00   52
 12  \w     75.00 109.00   0.50   64.83    --   20.00  54.00  60.00   68
 13  \w    -65.00 -35.00   0.50   64.83    --   20.00  54.00 -60.00   60
 14  \w      6.00  31.00   0.50   64.83    --   20.00  54.00 -60.00   50
 15  \w     60.00  85.00   0.50   64.83    --   20.00  54.00 -60.00   50
 16  \w    -67.00  47.00   0.50   64.83    --   20.00  54.00-120.00  228
 17  \w    -69.00 -41.00   0.50   64.83    --   20.00  54.00 -30.00   56
 18  \w    -16.00   9.00   0.50   64.83    --   20.00  54.00 -30.00   50
 19  \w    -69.00  46.00   0.50   64.83    --   20.00  54.00-180.00  230
 20  \w    -64.00   5.00   0.50   64.83    --   20.00  54.00   0.00  138
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0020378000
_diffrn_orient_matrix_UB_12      -0.0117917000
_diffrn_orient_matrix_UB_13      0.0434912000
_diffrn_orient_matrix_UB_21      -0.0630701000
_diffrn_orient_matrix_UB_22      0.0035949000
_diffrn_orient_matrix_UB_23      0.0068183000
_diffrn_orient_matrix_UB_31      -0.0058385000
_diffrn_orient_matrix_UB_32      -0.0504949000
_diffrn_orient_matrix_UB_33      -0.0006592000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56896
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.671
_diffrn_reflns_theta_min         1.753
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_preparation       'See lit'
_exptl_crystal_recrystallization_method 'See lit'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.118
_refine_diff_density_max         2.095
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         15030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1052P)^2^+1.5667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9045
_reflns_number_total             15030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02005j2.cif
_cod_data_source_block           r1_smart_4_form_x2
_cod_depositor_comments
;

2024-12-16
Z value fixed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            2
_cod_database_code               7710768
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C60H44Cl4Fe2N4O6
_chemical_oxdiff_usercomment     'Fe Pincer dichloro'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.777
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24B(H24B), C24A(H24A), C1B(H1B), C1A(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C23B(H23C,H23D), C23A(H23A,H23B), C8B(H8BA,H8BB), C8A(H8AA,H8AB)
2.c Aromatic/amide H refined with riding coordinates:
 C13B(H13B), C20A(H20A), C11B(H11B), C26A(H26A), C11A(H11A), C13A(H13A),
 C20B(H20B), C18B(H18B), C19B(H19B), C19A(H19A), C18A(H18A), C26B(H26B),
 C12B(H12B), C12A(H12A), C30A(H30A), C30B(H30B), C27A(H27A), C7B(H7B), C5B(H5B),
  C3B(H3B), C7A(H7A), C6B(H6B), C27B(H27B), C3A(H3A), C29B(H29B), C29A(H29A),
 C6A(H6A), C28A(H28A), C5A(H5A), C4B(H4B), C28B(H28B), C4A(H4A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48494
_olex2_exptl_crystal_mounting_method 'Paratin oil on a silcon loop.'
_olex2_submission_original_sample_id Need
_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 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.819