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_7055314
_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_formula_moiety         'C60, C19 H18 P'
_chemical_formula_sum            'C79 H18 P'
_chemical_formula_weight         997.90
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0792(2)
_cell_length_b                   15.6628(3)
_cell_length_c                   26.4166(5)
_cell_measurement_reflns_used    5099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.16
_cell_volume                     4170.35(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXs-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32109
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.229
_diffrn_reflns_theta_min         1.511
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 - Bruker AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       prism
_exptl_crystal_F_000             2028
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2948 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         9507
_refine_ls_number_restraints     8616
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0523P)^2^+4.8639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.824
_reflns_Friedel_fraction_max     0.737
_reflns_number_gt                8177
_reflns_number_total             9507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02886h2.cif
_cod_data_source_block           Ph3MeP_C60
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               7055314
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2013-4
_shelx_res_checksum              79733