Large Aromatic Hydrocarbon Radical Cation with Global Aromaticity and State-Associated Magnetic Activity
Guo, Jing; Zhou, Cong; Xie, Sheng; Luo, Shenglian; Gopalakrishna, Tullimilli Y.; Sun, Zhe; Jouha, Jabrane; Wu, Jishan; Zeng, Zebing; Chemistry of Materials 32 (2020) 5927–5936; doi:10.1021/acs.chemmater.9b05099

data_4003633
_publ_section_title
;
 Large Aromatic Hydrocarbon Radical Cation with Global Aromaticity and
 State-Associated Magnetic Activity
;
_journal_issue                   14
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5927
_journal_page_last               5936
_journal_paper_doi               10.1021/acs.chemmater.9b05099
_journal_volume                  32
_journal_year                    2020
_chemical_formula_moiety         'F6 Sb, C72 H78 O8'
_chemical_formula_sum            'C72 H78 F6 O8 Sb'
_chemical_formula_weight         1307.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.2924(7)
_cell_length_b                   23.5585(8)
_cell_length_c                   59.258(2)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      46.53
_cell_measurement_theta_min      3.30
_cell_volume                     25536.7(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            68997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.332
_diffrn_reflns_theta_min         3.297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1659 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.7664. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             10864
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1524
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1432P)^2^+204.1407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2448
_refine_ls_wR_factor_ref         0.2937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3236
_reflns_number_total             6122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b05099_si_005.cif
_cod_data_source_block           wmj18129
_cod_depositor_comments
;Adding full bibliography for 4003630--4003634.cif.

 Adding full bibliography for 4003630--4003634.cif.
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4003633
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C33 = C35-C34 = C35-C36 = C29-C28 = C30-C29 = C30-C31
 1.53 with sigma of 0.02
 C35-C34 = C30-C29
 1.53 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O2 \\sim O4 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C33 \\sim C34 \\sim
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C20(H20), C22(H22)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              34958
_shelx_hkl_checksum              82911
_olex2_submission_special_instructions 'No special instructions were received'