Monomers and dimers of fullerenes in the radical anion salts with dyes, (astrophloxine+)2(C60˙−)2 and (astrophloxine+)2(C70−)2: suppression of the C60˙− dimerization by π-stacking
Sobov, Pavel A.; Faraonov, Maxim A.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; New Journal of Chemistry 48 (2024) 10002–10009; doi:10.1039/D4NJ01402B

data_7063190
_publ_section_title
;
 Monomers and dimers of fullerenes in the radical anion salts with dyes,
 (astrophloxine+)2(C60&#x02D9;&#x2212;)2 and
 (astrophloxine+)2(C70&#x2212;)2: suppression of the C60&#x02D9;&#x2212;
 dimerization by \p-stacking
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10002
_journal_page_last               10009
_journal_paper_doi               10.1039/D4NJ01402B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C70, C27 H33 N2'
_chemical_formula_sum            'C97 H33 N2'
_chemical_formula_weight         1226.25
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-30
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-13 deposited with the CCDC.	2024-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.748(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6964(4)
_cell_length_b                   15.0127(7)
_cell_length_c                   33.7803(14)
_cell_measurement_reflns_used    3617
_cell_measurement_temperature    103.0(10)
_cell_measurement_theta_max      24.6700
_cell_measurement_theta_min      2.3870
_cell_volume                     5418.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.1619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23415
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         10916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0386P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5295
_reflns_number_total             10916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01402b2.cif
_cod_data_source_block           C70-dimer-Astrophloxine
_cod_depositor_comments
'Adding full bibliography for 7063190--7063191.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063190
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2013-2
_shelx_res_checksum              70727
_shelx_hkl_checksum              33695