From symmetrical tetrasulfides to trisulfide dioxides via photocatalysis
Gong, Kai; Zhou, Yilin; Jiang, Xuefeng; Green Chemistry 23 (2021) 9865–9869; doi:10.1039/D1GC03242A

data_7243874
_publ_section_title
;
 From symmetrical tetrasulfides to trisulfide dioxides via photocatalysis
;
_journal_issue                   24
_journal_name_full               'Green Chemistry'
_journal_page_first              9865
_journal_page_last               9869
_journal_paper_doi               10.1039/D1GC03242A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C10 H13 N O4 S3'
_chemical_formula_sum            'C10 H13 N O4 S3'
_chemical_formula_weight         307.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-24 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8766(3)
_cell_length_b                   6.30850(10)
_cell_length_c                   16.9497(4)
_cell_measurement_reflns_used    4967
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.2380
_cell_measurement_theta_min      5.2350
_cell_volume                     1376.86(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     44.00  89.00   1.00    1.00    --    0.00  19.00-120.00   45
  2  \w    -25.00  41.00   1.00    1.00    --    0.00  77.00 -30.00   66
  3  \w    -83.00 -26.00   1.00    1.00    --    0.00 -19.00 -90.00   57
  4  \w    -22.00   8.00   1.00    1.00    --    0.00  19.00-120.00   30
  5  \w     48.00  84.00   1.00    1.00    --    0.00  77.00 -30.00   36
  6  \w     -8.00  24.00   1.00    1.00    --    0.00 -19.00 -90.00   32
  7  \w     78.00 104.00   1.00    2.00    --   95.80 -82.00  30.00   26
  8  \w    104.00 182.00   1.00    2.00    --   95.80  15.00-180.00   78
  9  \w     24.00 116.00   1.00    2.00    --   95.80 -45.00 -30.00   92
 10  \w     30.00 120.00   1.00    2.00    --   95.80 -61.00  90.00   90
 11  \w     81.00 185.00   1.00    2.00    --   95.80  30.00 120.00  104
 12  \w    101.00 151.00   1.00    2.00    --   95.80  30.00-150.00   50
 13  \w     51.00 120.00   1.00    2.00    --   95.80 -82.00  90.00   69
 14  \w     70.00 103.00   1.00    2.00    --   95.80 -82.00-180.00   33
 15  \w      9.00 121.00   1.00    2.00    --   95.80 -82.00-120.00  112
 16  \w     27.00  98.00   1.00    2.00    --   95.80 -82.00   0.00   71
 17  \w     93.00 124.00   1.00    2.00    --   95.80 -77.00 -60.00   31
 18  \w     30.00  56.00   1.00    2.00    --   95.80 -77.00 -60.00   26
 19  \w     12.00 107.00   1.00    2.00    --   95.80 -61.00-120.00   95
 20  \w     85.00 183.00   1.00    2.00    --   95.80  30.00  90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0106104000
_diffrn_orient_matrix_UB_12      0.1949283000
_diffrn_orient_matrix_UB_13      -0.0541049000
_diffrn_orient_matrix_UB_21      -0.1192083000
_diffrn_orient_matrix_UB_22      -0.0162355000
_diffrn_orient_matrix_UB_23      0.0053229000
_diffrn_orient_matrix_UB_31      0.0008465000
_diffrn_orient_matrix_UB_32      0.1462841000
_diffrn_orient_matrix_UB_33      0.0727745000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11537
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.029
_diffrn_reflns_theta_max         67.029
_diffrn_reflns_theta_min         5.219
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 924 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2332
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.3313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.882
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                2244
_reflns_number_total             2332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1gc03242a2.cif
_cod_data_source_block           exp_1905
_cod_depositor_comments          'Adding full bibliography for 7243874.cif.'
_cod_database_code               7243874
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              3113
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.462
_oxdiff_exptl_absorpt_empirical_full_min 0.437