Cis-thioindigo (TI) ‒ a new ligand with accessible radical anion and dianion states. Strong magnetic coupling in the {[TI-(μ2-O),(μ-O)] Cp*Cr}2 dimers.
Konarev, Dmitri V.; Khasanov, Salavat S.; Shestakov, Alexander F.; Fatalov, Alexey M.; Batov, Mikhail S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02878D

data_7044321
_publ_section_title
;
 Cis-thioindigo (TI) -- a new ligand with accessible radical anion and
 dianion states. Strong magnetic coupling in the {[TI-(\m2-O),(\m-O)]
 Cp*Cr}2 dimers.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02878D
_journal_year                    2017
_chemical_compound_source        no
_chemical_formula_moiety         'C18 H36 N2 Na1 O6, C16 H8 O2 S2'
_chemical_formula_sum            'C34 H44 N2 Na O8 S2'
_chemical_formula_weight         695.82
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'salt of thioindigo radical anions with cryptand[2,2,2] sodium'
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-28
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2584(3)
_cell_length_b                   14.4597(3)
_cell_length_c                   19.1968(5)
_cell_measurement_reflns_used    10780
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.0800
_cell_measurement_theta_min      2.5130
_cell_volume                     3380.21(14)
_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
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29401
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90925
_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    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             1476
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/o-dichlorobenzene'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(14)
_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     960
_refine_ls_number_reflns         13553
_refine_ls_number_restraints     436
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0296P)^2^+1.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10803
_reflns_number_total             13553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02878d2.cif
_cod_data_source_block           ThioindigoCryptandNa
_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 
;
_cod_database_code               7044321
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2013-4
_shelx_res_checksum              12901