C<sub>sp<sup>2</sup></sub>-H/F bond activation and borylation with iron.
Zars, Ethan; Pick, Lisa; Kankanamge, Achala; Gau, Michael R.; Meyer, Karsten; Mindiola, Daniel J.; Chemical communications (Cambridge, England) 60 (2024) 14415–14418; doi:10.1039/d4cc04127e

data_7133848
_publ_section_title
;
 C<sub>sp<sup>2</sup></sub>-H/F bond activation and borylation with iron.
;
_journal_issue                   97
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14415
_journal_page_last               14418
_journal_paper_doi               10.1039/d4cc04127e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C53 H76 Fe K N3 O6, C6 H6'
_chemical_formula_sum            'C59 H82 Fe K N3 O6'
_chemical_formula_weight         1024.22
_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             2022-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-08-13 deposited with the CCDC.	2024-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7507(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.65310(4)
_cell_length_b                   23.67132(8)
_cell_length_c                   22.34027(8)
_cell_measurement_reflns_used    79462
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.3640
_cell_measurement_theta_min      3.9440
_cell_volume                     5605.26(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-6000HE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -121.00 -30.00   0.50    0.50    --  -47.28  -9.00 -23.00  182
  2  \w    -28.00  27.00   0.50    0.50    --  -47.28   9.00 150.00  110
  3  \w    -26.00  22.00   0.50    0.50    --   47.28  -9.00 -23.00   96
  4  \w     29.00 121.00   0.50    0.50    --   47.28   9.00 150.00  184
  5  \w   -164.00 -72.00   0.50    2.00    --  -90.00  -9.00 -23.00  184
  6  \w     95.00 178.00   0.50    2.00    --  113.25   9.00 150.00  166
  7  \w    -45.00  26.00   0.50    0.50    --  -47.28  37.00-180.00  142
  8  \w    -24.00  62.00   0.50    0.50    --   47.28 -57.00-150.00  172
  9  \w     25.00 119.00   0.50    0.50    --   47.28  77.00   0.00  188
 10  \w    -24.00  62.00   0.50    0.50    --   47.28 -57.00 -30.00  172
 11  \w    -27.00  24.00   0.50    0.50    --   47.28 -19.00 -90.00  102
 12  \w   -114.00 -17.00   0.50    2.00    --  -90.00  80.00 146.77  194
 13  \w   -114.00 -17.00   0.50    2.00    --  -90.00  80.00-135.11  194
 14  \w   -114.00 -17.00   0.50    2.00    --  -90.00  80.00  78.70  194
 15  \w   -114.00 -17.00   0.50    2.00    --  -90.00  80.00 -34.36  194
 16  \w     42.00 108.00   0.50    2.00    --  113.25 -78.00 157.40  132
 17  \w     91.00 178.00   0.50    2.00    --  113.25  77.00  60.00  174
 18  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00-120.00   52
 19  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00  30.00   52
 20  \w    100.00 178.00   0.50    2.00    --  113.25  15.00-180.00  156
 21  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00 -30.00   52
 22  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00 120.00   52
 23  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00 119.23  190
 24  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00 179.34  190
 25  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00  26.72  190
 26  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00 126.60  190
 27  \w    101.00 178.00   0.50    2.00    --  113.25  30.00 -30.00  154
 28  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00 -59.79  190
 29  \w     97.00 178.00   0.50    2.00    --  113.25  61.00-150.00  162
 30  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00-180.00   52
 31  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00  90.00  122
 32  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00-124.53  190
 33  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00 -23.56  190
 34  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00  90.00   52
 35  \w    101.00 178.00   0.50    2.00    --  113.25  30.00  30.00  154
 36  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00  60.00   52
 37  \w    101.00 178.00   0.50    2.00    --  113.25  30.00 -90.00  154
 38  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00 -60.00   52
 39  \w    101.00 178.00   0.50    2.00    --  113.25  30.00 120.00  154
 40  \w     91.00 178.00   0.50    2.00    --  113.25  77.00 150.00  174
 41  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00 -90.00  122
 42  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00-180.00  122
 43  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00   0.00  122
 44  \w    101.00 178.00   0.50    2.00    --  113.25  45.00  30.00  154
 45  \w    100.00 178.00   0.50    2.00    --  113.25  15.00-120.00  156
 46  \w     42.00 137.00   0.50    2.00    --  113.25 -80.00-116.30  190
 47  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00 -60.00  122
 48  \w     42.00 103.00   0.50    2.00    --  113.25 -77.00  30.00  122
 49  \w     25.00  83.00   0.50    0.50    --   47.28  77.00 120.00  116
 50  \w     25.00 119.00   0.50    0.50    --   47.28  77.00-150.00  188
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054574000
_diffrn_orient_matrix_UB_12      0.0037099000
_diffrn_orient_matrix_UB_13      -0.0690552000
_diffrn_orient_matrix_UB_21      0.1443189000
_diffrn_orient_matrix_UB_22      0.0074076000
_diffrn_orient_matrix_UB_23      0.0047697000
_diffrn_orient_matrix_UB_31      0.0162817000
_diffrn_orient_matrix_UB_32      -0.0645580000
_diffrn_orient_matrix_UB_33      -0.0034247000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            137772
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_min         3.978
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11418
_refine_ls_number_restraints     462
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+1.9840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                10907
_reflns_number_total             11418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04127e2.cif
_cod_data_source_block           9985_cmpd3
_cod_depositor_comments
'Adding full bibliography for 7133846--7133849.cif.'
_cod_database_code               7133848
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe O K B'
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.435
_shelx_res_checksum              91651
_shelx_hkl_checksum              30831
_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 1.692
_oxdiff_exptl_absorpt_empirical_full_min 0.719