Optical and magnetic properties of trans-indigo˙− radical anions. Magnetic coupling between trans-indigo˙− (S = 1/2) mediated by intermolecular hydrogen N‒H⋯OC bonds
Konarev, Dmitri V.; Zorina, Leokadiya V.; Batov, Mikhail S.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; New Journal of Chemistry 43 (2019) 7350–; doi:10.1039/C9NJ00802K

data_7058278
_publ_section_title
;
 Optical and magnetic properties of trans-indigo&#x02D9;&#x2212; radical
 anions. Magnetic coupling between trans-indigo&#x02D9;&#x2212; (S = 1/2)
 mediated by intermolecular hydrogen N--H&#x22EF;O&#xE001;C bonds
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7350
_journal_paper_doi               10.1039/C9NJ00802K
_journal_volume                  43
_journal_year                    2019
_chemical_compound_source        no
_chemical_formula_moiety
'6(C18 H36 K N2 O6), 7(C16 H10 N2 O2), 5.5(C6 H4 Cl2)'
_chemical_formula_sum            'C253 H308 Cl11 K6 N26 O50'
_chemical_formula_weight         5137.79
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'salt of trans-indigo with cryptand[2.2.2](K+) cations, o-dichlorobenzene solvate'
_chemical_properties_physical    Air-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_method           SHELXL-2016/6
_audit_update_record
;
2019-02-13 deposited with the CCDC.    2019-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                97.646(2)
_cell_angle_beta                 98.970(2)
_cell_angle_gamma                106.968(3)
_cell_formula_units_Z            1
_cell_length_a                   15.2735(5)
_cell_length_b                   17.5699(5)
_cell_length_c                   25.9540(6)
_cell_measurement_reflns_used    12659
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.1140
_cell_measurement_theta_min      1.5940
_cell_volume                     6461.6(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    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.886
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.2125
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            49133
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.444
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93943
_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    1.320
_exptl_crystal_description       prism
_exptl_crystal_F_000             2709
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/n-hexane'
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.135
_refine_diff_density_max         2.755
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2132
_refine_ls_number_reflns         49133
_refine_ls_number_restraints     3176
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2076
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15231
_reflns_number_total             31762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00802k2.cif
_cod_data_source_block           7indigo6cryptK5C6H4Cl2
_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 7058278.cif.
;
_cod_database_code               7058278
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.936
_oxdiff_exptl_absorpt_empirical_full_max 1.086
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_twin_integration_method  simultaneous
_twin_special_details
;
Component 2 rotated by -180\% around [1 -1 1] (reciprocal)
;
_shelx_res_checksum              39503