Synthesis and structure elucidation of triarylmethyl radicals with anthryl substitution.
Wang, Peng; Hu, Jinlian; Xu, Zhuofan; Pu, Zhaofangzhou; Sato, Sota; Zhang, Xiaotao; Hu, Wenping; Sun, Zhe; Chemical communications (Cambridge, England) 59 (2023) 2015–2018; doi:10.1039/d2cc06083c

data_7131210
_publ_section_title
;
 Synthesis and structure elucidation of triarylmethyl radicals with
 anthryl substitution.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2015
_journal_page_last               2018
_journal_paper_doi               10.1039/d2cc06083c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C46 H55 Si'
_chemical_formula_sum            'C46 H55 Si'
_chemical_formula_weight         635.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2d9q5m
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-01-19 deposited with the CCDC.	2023-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.966(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.4174(10)
_cell_length_b                   12.3393(4)
_cell_length_c                   24.1653(7)
_cell_measurement_reflns_used    6823
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      73.6870
_cell_measurement_theta_min      3.3900
_cell_volume                     7731.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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_temperature      293(2)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.938
_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    -40.00 -15.00   0.50    1.00    --  -45.62  27.00 -45.00   50
  2  \w    -53.00 -27.00   0.50    6.00    -- -100.00  61.00 -30.00   52
  3  \w    -67.00 -28.00   0.50    6.00    -- -100.00 125.00 -60.00   78
  4  \w   -108.00 -66.00   0.50    6.00    -- -100.00  27.00 -45.00   84
  5  \w   -117.00 -58.00   0.50    6.00    -- -100.00  61.00 -30.00  118
  6  \w   -104.00 -73.00   0.50    6.00    -- -100.00 125.00 -60.00   62
  7  \w   -119.00 -32.00   0.50    1.00    --  -45.62 -27.00 152.00  174
  8  \w    -14.00  50.00   0.50    1.00    --   45.62 -27.00 152.00  128
  9  \w     75.00 111.00   0.50    6.00    --  101.75 -27.00 152.00   72
 10  \w     29.00 109.00   0.50    6.00    --  101.75-125.00  60.00  160
 11  \w     41.00  67.00   0.50    6.00    --  101.75 -94.00 -30.00   52
 12  \w     21.00  93.00   0.50    1.00    --   45.62-125.00  60.00  144
 13  \w     51.00 117.00   0.50    6.00    --  101.75 -30.00 -30.00  132
 14  \w     92.00 154.00   0.50    6.00    --  101.75  27.00 -45.00  124
 15  \w     45.00 108.00   0.50    6.00    --  101.75 -94.00-120.00  126
 16  \w     32.00  89.00   0.50    1.00    --   45.62  27.00 -45.00  114
 17  \w     56.00 109.00   0.50    6.00    --  101.75 -94.00 120.00  106
 18  \w   -132.00 -88.00   0.50    6.00    -- -100.00 -27.00 152.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23566
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.901
_diffrn_reflns_theta_min         3.409
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       needle
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0697P)^2^+6.8618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6248
_reflns_number_total             7457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06083c2.cif
_cod_data_source_block           exp_559
_cod_depositor_comments
'Adding full bibliography for 7131209--7131211.cif.'
_cod_database_code               7131210
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C30(H30)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C4(H4), C7(H7), C6(H6), C16(H16), C10(H10), C9(H9),
 C26(H26), C23(H23), C12(H12), C19(H19), C17(H17), C18(H18), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C38(H38A,H38B,
 H38C), C45(H45A,H45B,H45C), C41(H41A,H41B,H41C), C31(H31A,H31B,H31C), C37(H37A,
 H37B,H37C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              68176
_shelx_hkl_checksum              48372
_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
;