Electrochemical and Chemical Reduction of Disulfur Dinitride: Formation of [S4N4]-., EPR Spectroscopic Characterization of the [S2N2H]. Radical, and X-ray Structure of [Na(15-crown-5)][S3N3]
Tracey L. Roemmele; Jari Konu; René T. Boeré; Tristram Chivers; Inorganic Chemistry 48 (2009) 9454–9462; doi:10.1021/ic9014114

data_4303342
_publ_section_title
;
Electrochemical and Chemical Reduction of Disulfur Dinitride: Formation of
[S4N4]-., EPR Spectroscopic Characterization of the [S2N2H]. Radical,
and X-ray Structure of [Na(15-crown-5)][S3N3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9454
_journal_page_last               9462
_journal_paper_doi               10.1021/ic9014114
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C10 H20 Na O5, N3  S3'
_chemical_formula_sum            'C10 H20 N3 Na O5 S3'
_chemical_formula_weight         381.46
_chemical_name_systematic
;
 sodium 15-crown-5 trisulfur trintride
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.158(3)
_cell_length_b                   14.383(3)
_cell_length_c                   7.3713(15)
_cell_measurement_reflns_used    2809
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.83
_cell_volume                     1713.1(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX v1.70-01 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2809
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.8612
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+2.0494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                1018
_reflns_number_total             1557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9014114_si_001.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
;
 Replacing data items '_publ_contact_author1', '_publ_contact_author2',
 '_publ_contact_author1_email' and '_publ_contact_author2_email' with
 the _publ_contact_author* loop.

 Antanas Vaitkus,
 2017-03-02
;
_cod_database_code               4303342