Reversible dissociation of singly-bonded (C60−)2 dimers in (MV˙+)2(C60−)2·solvent salt containing paramagnetic methyl viologen MV˙+ radical cations
Konarev, Dmitri V.; Khasanov, Salavat S.; Obraztsov, Oleg A.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; New Journal of Chemistry 45 (2021) 1163–1167; doi:10.1039/D0NJ05076H

data_7060169
_publ_section_title
;
 Reversible dissociation of singly-bonded (C60&#x2212;)2 dimers in
 (MV&#x02D9;+)2(C60&#x2212;)2&#x00B7;solvent salt containing paramagnetic
 methyl viologen MV&#x02D9;+ radical cations
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1163
_journal_page_last               1167
_journal_paper_doi               10.1039/D0NJ05076H
_journal_volume                  45
_journal_year                    2021
_chemical_compound_source        no
_chemical_formula_moiety
'C120, 2(C12 H14 N2), 2.5(C6 H4 Cl2), 0.5(C6 H6)'
_chemical_formula_sum            'C162 H41 Cl5 N4'
_chemical_formula_weight         2220.24
_chemical_melting_point          ?
_chemical_name_systematic
'salt of singly-bonded fullerene (C60-)2 dimer with methylviologen radical cations, dichlorobenzene-benzene solvate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmsp
_audit_creation_date             2020-10-10
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-10-10 deposited with the CCDC.	2020-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                98.039(6)
_cell_angle_beta                 91.161(6)
_cell_angle_gamma                110.473(6)
_cell_formula_units_Z            1
_cell_length_a                   9.8950(6)
_cell_length_b                   14.1098(10)
_cell_length_c                   17.6549(14)
_cell_measurement_reflns_used    2849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.9060
_cell_measurement_theta_min      2.3320
_cell_volume                     2280.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.823
_diffrn_measured_fraction_theta_max 0.853
_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_unetI/netI     0.1363
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9678
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         2.200
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             1126
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/benzene/n-hexane'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1856
_refine_ls_number_reflns         9678
_refine_ls_number_restraints     3558
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.0955
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1579P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2384
_refine_ls_wR_factor_ref         0.2642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4701
_reflns_number_total             9678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05076h2.cif
_cod_data_source_block           (C60)2-2Viologen-3DCB
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7060169.cif.
;
_cod_database_code               7060169
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2013-2
_shelx_res_checksum              30882