Structure and magnetic properties of the ionic fullerene salt (TMP+)·(C60˙−)·C6H5CN containing layers of monomeric C60˙− radical anions
Konarev, Dmitri V.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Ishikawa, Manabu; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; New Journal of Chemistry 37 (2013) 2521–; doi:10.1039/c3nj00189j

data_7053148
_publ_section_title
;
 Structure and magnetic properties of the ionic fullerene salt
 (TMP+)&#x00B7;(C60&#x02D9;&#x2212;)&#x00B7;C6H5CN containing layers of
 monomeric C60&#x02D9;&#x2212; radical anions
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2521
_journal_paper_doi               10.1039/c3nj00189j
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C60, C7 H17 N2, C7 H5 N'
_chemical_formula_sum            'C74 H22 N3'
_chemical_formula_weight         952.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.960(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3941(5)
_cell_length_b                   19.4479(10)
_cell_length_c                   19.9677(9)
_cell_measurement_reflns_used    21004
_cell_measurement_temperature    119.9(6)
_cell_measurement_theta_max      30.1402
_cell_measurement_theta_min      1.9565
_cell_volume                     4034.0(3)
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119.9(6)
_diffrn_detector_area_resol_mean 10.4752
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
1 omega -84.00 -58.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- -13.5556 179.0000 30.0000 26

2 omega -96.00 -70.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- -13.5556 179.0000 -120.0000 26

3 omega -20.00 82.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 13.5556 77.0000 -150.0000 102

4 omega -5.00 32.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 13.5556 77.0000 -30.0000 37

5 omega -5.00 90.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 13.5556 37.0000 120.0000 95

6 omega -12.00 74.00 1.0000 60.0000
omega____ theta____ kappa____ phi______ frames
- 13.5556 37.0000 30.0000 86

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40488
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.21
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.9548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1605
_refine_ls_number_reflns         10757
_refine_ls_number_restraints     6551
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                8652
_reflns_number_total             10757
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3nj00189j.txt
_cod_data_source_block           C60_TMP_BzN_120K
_cod_database_code               7053148