Negatively charged singly-bonded dimers of C1-[C70(CF3)10] and bare C70 fullerene
Konarev, Dmitri V.; Khasanov, Salavat S.; Goryunkov, Alexey A.; Troyanov, Sergey I.; Brotsman, Victor A.; Ioffe, Ilya N.; Lyubovskaya, Rimma N.; New Journal of Chemistry 43 (2019) 2726–; doi:10.1039/C8NJ05847D

data_7058087
_publ_section_title
;
 Negatively charged singly-bonded dimers of C1-[C70(CF3)10] and bare C70
 fullerene
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2726
_journal_paper_doi               10.1039/C8NJ05847D
_journal_volume                  43
_journal_year                    2019
_chemical_compound_source        no
_chemical_formula_moiety         'C140, 2(C16 H32 N2 O5 Na), 3(C6 H4 Cl2)'
_chemical_formula_sum            'C190 H76 Cl6 N4 Na2 O10'
_chemical_formula_weight         2833.22
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'salt of negatively charged C70 dimer with cryptand[2.2.1] sodium, o-dichlorobenzene 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'
_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_date             2016-10-21
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.101(2)
_cell_angle_beta                 74.353(2)
_cell_angle_gamma                83.299(2)
_cell_formula_units_Z            2
_cell_length_a                   16.9600(3)
_cell_length_b                   17.0183(3)
_cell_length_c                   21.5230(4)
_cell_measurement_reflns_used    29998
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.2470
_cell_measurement_theta_min      2.1780
_cell_volume                     5891.59(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'WinGX publication routines (Farrugia, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.982
_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  0.98881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/n-hexane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1958
_refine_ls_number_reflns         28597
_refine_ls_number_restraints     1023
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0642P)^2^+6.1648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20950
_reflns_number_total             28597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05847d2.cif
_cod_data_source_block           C1402Cryptand221Na
_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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7058085--7058087.cif.
;
_cod_original_cell_volume        5891.6(2)
_cod_database_code               7058087
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
_shelx_res_checksum              74353
_shelx_hkl_checksum              12962