Effective magnetic coupling with strong spin frustration in (Ph3MeP+)(C60•) and reversible C60• dimerization in (Ph3MeP+)(C60•)C6H5CN . Effect of solvent on structure and properties
Konarev, Dmitri V.; Khasanov, Salavat S.; Kuz`min, Alexey V.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; New J. Chem. 40 (2016) 2792–2798; doi:10.1039/C5NJ02886H

data_7055315
_publ_section_title
;
 Effective magnetic coupling with strong spin frustration in
 (Ph3MeP+)(C60&#x2022;&#xF02D;) and reversible C60&#x2022;&#xF02D;
 dimerization in (Ph3MeP+)(C60&#x2022;&#xF02D;)&#xF0D7;C6H5CN . Effect of
 solvent on structure and properties
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2792
_journal_page_last               2798
_journal_paper_doi               10.1039/C5NJ02886H
_journal_volume                  40
_journal_year                    2016
_chemical_compound_source        no
_chemical_formula_moiety         'C120, 2(C19 H18 P), 2(C7 H5 N)'
_chemical_formula_sum            'C172 H46 N2 P2'
_chemical_formula_weight         2202.05
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'fullerene C60 salt with triphenylmethylphosphonium cations, benzonitrile solvate'
_chemical_properties_physical    Air-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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                101.006(11)
_cell_angle_beta                 113.801(13)
_cell_angle_gamma                90.849(11)
_cell_formula_units_Z            1
_cell_length_a                   12.5760(18)
_cell_length_b                   13.8505(17)
_cell_length_c                   15.035(2)
_cell_measurement_reflns_used    3655
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0590
_cell_measurement_theta_min      1.4520
_cell_volume                     2339.7(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.4752
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.1621
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.758
_diffrn_reflns_theta_min         1.506
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             1122
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichlorobenzene/benzonitrile'
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         11111
_refine_ls_number_restraints     1263
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1885
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0415P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             11111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02886h2.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        2339.8(6)
_cod_database_code               7055315
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2013-2
_shelx_res_checksum              5513