Tailoring C-H amination activity <i>via</i> modification of the triazole-derived carbene ligand.
Hudson, Luke A.; Stroek, Wowa; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14795–14800; doi:10.1039/d4dt01715c

data_7716844
_publ_section_title
;
 Tailoring C-H amination activity <i>via</i> modification of the
 triazole-derived carbene ligand.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14795
_journal_page_last               14800
_journal_paper_doi               10.1039/d4dt01715c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C42 H48 Fe N6 O2'
_chemical_formula_sum            'C42 H48 Fe N6 O2'
_chemical_formula_weight         724.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-07 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8494(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1907(2)
_cell_length_b                   24.2458(4)
_cell_length_c                   15.4249(3)
_cell_measurement_reflns_used    42537
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      33.161
_cell_measurement_theta_min      2.127
_cell_volume                     3791.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -11.00  87.00   0.50    8.00    --   13.03  66.00 -38.00  196
  2  \w    -61.00  37.00   0.50    8.00    --   13.03 -66.00-173.00  196
  3  \w    -16.00  83.00   0.50    8.00    --   13.03  77.00 120.00  198
  4  \w    -25.00  68.00   0.50    8.00    --  -13.50  19.00  90.00  186
  5  \w    -19.00  29.00   0.50    8.00    --  -13.50 -99.00 -30.00   96
  6  \w    -19.00  29.00   0.50    8.00    --  -13.50 -99.00  60.00   96
  7  \w    -87.00 -42.00   0.50    8.00    --  -13.50-178.00 -60.00   90
  8  \w    -56.00  42.00   0.50    8.00    --   13.03 -77.00   0.00  196
  9  \w    -18.00  54.00   0.50    8.00    --   13.03 -99.00 -90.00  144
 10  \w    -18.00  54.00   0.50    8.00    --   13.03 -99.00 120.00  144
 11  \w    -19.00  22.00   0.50    8.00    --  -13.50 -99.00 150.00   82
 12  \w    -89.00 -40.00   0.50    8.00    --  -13.50 178.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.527
_diffrn_reflns_theta_min         2.141
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
        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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         21589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15592
_reflns_number_total             21589
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9719\% 
around [1.00 0.00 0.00] (reciprocal) or [1.00 0.00 0.07] (direct)
;
_cod_data_source_file            d4dt01715c2.cif
_cod_data_source_block           23ma017_lah065
_cod_depositor_comments
'Adding full bibliography for 7716844--7716845.cif.'
_cod_original_cell_volume        3791.39(13)
_cod_database_code               7716844
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6646(5)
 0.3354(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C16(H16), C40(H40), C19(H19), C37(H37)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C2(H2), C23(H23), C25(H25), C12(H12), C5(H5), C35(H35), C24(H24),
 C4(H4), C3(H3), C33(H33), C14(H14), C34(H34), C13(H13)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              9356
_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
;