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_7131209
_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         'C60 H63 Si'
_chemical_formula_sum            'C60 H63 Si'
_chemical_formula_weight         812.19
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2d9q4l
_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                 106.295(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5678(8)
_cell_length_b                   17.3752(8)
_cell_length_c                   12.8103(6)
_cell_measurement_reflns_used    929
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      58.8090
_cell_measurement_theta_min      2.0430
_cell_volume                     4821.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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      160.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_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     -8.00 124.00   0.50    2.00    --   35.19  15.00  51.00  264
  2  \w   -129.00 -88.00   0.50   10.00    -- -100.00-111.00  95.00   82
  3  \w   -117.00 -44.00   0.50   10.00    -- -100.00 133.00 -92.00  146
  4  \w     28.00 147.00   0.50   10.00    --  107.62  15.00  51.00  238
  5  \w     62.00 118.00   0.50    2.00    --   35.19 179.00 -60.00  112
  6  \w    -48.00 -23.00   0.50   10.00    -- -100.00  45.00 150.00   50
  7  \w     34.00  59.00   0.50   10.00    --  107.62-111.00  30.00   50
  8  \w     24.00 106.00   0.50   10.00    --  107.62 -94.00  60.00  164
  9  \w     35.00  62.00   0.50   10.00    --  107.62 -61.00 150.00   54
 10  \w     76.00 108.00   0.50   10.00    --  107.62-111.00  30.00   64
 11  \w     30.00  56.00   0.50   10.00    --  107.62-111.00  60.00   52
 12  \w     69.00  95.00   0.50   10.00    --  107.62-111.00  60.00   52
 13  \w     27.00  53.00   0.50   10.00    --  107.62 -45.00  60.00   52
;
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.835
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13422
_diffrn_reflns_point_group_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         4.405
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7116
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1292P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3974
_reflns_number_total             7116
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.6235\% 
around [1.00 0.01 0.01] (reciprocal) or [0.88 0.01 0.47] (direct)
;
_cod_data_source_file            d2cc06083c2.cif
_cod_data_source_block           exp_824_11
_cod_depositor_comments
'Adding full bibliography for 7131209--7131211.cif.'
_cod_database_code               7131209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.934
_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. Restrained distances
 C57-C58A \\sim C57-C58
 with sigma of 0.02
 C57-C60A \\sim C57-C60
 with sigma of 0.02
 C57-C59A \\sim C57-C59
 with sigma of 0.02
 C54A-C56A \\sim C54-C56
 with sigma of 0.04
 C55A-C56A \\sim C55-C56
 with sigma of 0.04
 C5-C53A \\sim C5-C53
 with sigma of 0.02
 C53A-C55A \\sim C53-C55
 with sigma of 0.02
 C53A-C54A \\sim C53-C54
 with sigma of 0.02
 C53A-C56A \\sim C53-C56
 with sigma of 0.02
 C55A-C54A \\sim C55-C54
 with sigma of 0.04
 C5-C55A \\sim C5-C55
 with sigma of 0.04
 C5-C54A \\sim C5-C54
 with sigma of 0.04
 C5-C56A \\sim C5-C56
 with sigma of 0.04
 C46-C44 \\sim C44-C45
 with sigma of 0.02
3. Rigid bond restraints
 Si1, C44, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C53 \\sim C54 \\sim C54A \\sim C56 \\sim C56A \\sim C55 \\sim C55A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C57 \\sim C59 \\sim C59A \\sim C58 \\sim C58A \\sim C60A \\sim C60: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si1 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
5. Others
 Sof(C59)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C58)=Sof(H58D)=Sof(H58E)=Sof(H58F)=
 Sof(C60)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Sof(C54)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C53)=Sof(C55)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C56)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(2)
 Sof(C53A)=Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C54A)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C50(H50), C47(H47), C44(H44)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C10(H10), C7(H7), C4(H4), C12(H12), C13(H13), C16(H16),
 C3(H3), C30(H30), C6(H6), C9(H9), C25(H25), C37(H37), C17(H17), C40(H40),
 C19(H19), C38(H38), C24(H24), C33(H33), C39(H39), C32(H32), C18(H18), C31(H31)
6.c Idealised Me refined as rotating group:
 C58A(H58A,H58B,H58C), C52(H52A,H52B,H52C), C55A(H55A,H55B,H55C), C54A(H54A,
 H54B,H54C), C56A(H56A,H56B,H56C), C51(H51A,H51B,H51C), C60A(H60A,H60B,H60C),
 C49(H49A,H49B,H49C), C59A(H59A,H59B,H59C), C46(H46A,H46B,H46C), C48(H48A,H48B,
 H48C), C59(H59D,H59E,H59F), C58(H58D,H58E,H58F), C60(H60D,H60E,H60F), C54(H54D,
 H54E,H54F), C55(H55D,H55E,H55F), C56(H56D,H56E,H56F), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              93765
_shelx_hkl_checksum              65007
_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
;