A Stable Anionic Dithiolene Radical.
Wang, Yuzhong; Hickox, Hunter P.; Xie, Yaoming; Wei, Pingrong; Blair, Soshawn A.; Johnson, Michael K.; Schaefer, 3rd, Henry F; Robinson, Gregory H.; Journal of the American Chemical Society 139 (2017) 6859–6862; doi:10.1021/jacs.7b03794

data_4126036
_publ_section_title
;
 A Stable Anionic Dithiolene Radical.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6859
_journal_page_last               6862
_journal_paper_doi               10.1021/jacs.7b03794
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C76 H112 Cl Ge Li N4 O6 S6'
_chemical_formula_weight         1485.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.3660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9377(6)
_cell_length_b                   14.9604(6)
_cell_length_c                   37.2578(15)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.49
_cell_volume                     8319.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 CMOS'
_diffrn_measurement_method       'Phi\Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            254457
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.927
_diffrn_source                   Imus
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.396
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_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         16389
_refine_ls_number_restraints     335
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+3.9067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11789
_reflns_number_total             16389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03794_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 4126034--4126036.cif.'
_cod_original_cell_volume        8319.0(6)
_cod_database_code               4126036
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              82389
_shelx_hkl_checksum              57027