Indium-catalyzed inter- and intramolecular dithianyl-alkyne metathesis reactions.
Chen, Xi; Li, Rui-Peng; Long, Peng; Tang, Yuxi; Li, Jia; Tang, Shouchu; Chemical communications (Cambridge, England) 60 (2024) 1285–1288; doi:10.1039/d3cc05622h

data_7132546
_publ_section_title
;
 Indium-catalyzed inter- and intramolecular dithianyl-alkyne metathesis
 reactions.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1285
_journal_page_last               1288
_journal_paper_doi               10.1039/d3cc05622h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H16 Br N O2 S2'
_chemical_formula_sum            'C18 H16 Br N O2 S2'
_chemical_formula_weight         422.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-15 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3295(3)
_cell_length_b                   10.5061(2)
_cell_length_c                   18.8191(3)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    300.49(10)
_cell_measurement_theta_max      75.9710
_cell_measurement_theta_min      3.3650
_cell_volume                     3624.02(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.49(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_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    -26.00  22.00   0.50    0.05    --   44.44 -17.00  84.00   96
  2  \w    -29.00  20.00   0.50    0.05    --   44.44 -19.00   0.00   98
  3  \w    -25.00  13.00   0.50    0.05    --   44.44 -37.00 -30.00   76
  4  \w    126.00 162.00   0.50    0.05    --  109.62 145.00 -93.00   72
  5  \w     64.00 107.00   0.50    0.05    --  109.62 145.00 -93.00   86
  6  \w     40.00  65.00   0.50    0.05    --  109.62-125.00  60.00   50
  7  \w     84.00 111.00   0.50    0.05    --  109.62-125.00  60.00   54
  8  \w     37.00  98.00   0.50    0.05    --  109.62 -94.00 -60.00  122
  9  \w     75.00 101.00   0.50    0.05    --  109.62 -94.00 -90.00   52
 10  \w    -54.00 -25.00   0.50    0.05    -- -100.00  45.00  30.00   58
 11  \w    -54.00 -26.00   0.50    0.05    -- -100.00  45.00  60.00   56
 12  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00 120.00   50
 13  \w   -150.00 -84.00   0.50    0.05    -- -100.00 -17.00  84.00  132
 14  \w   -165.00 -90.00   0.50    0.05    -- -100.00-109.00 -78.00  150
 15  \w   -115.00 -80.00   0.50    0.05    --  -44.44-179.00 -60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0704888000
_diffrn_orient_matrix_UB_12      0.0731146000
_diffrn_orient_matrix_UB_13      -0.0182704000
_diffrn_orient_matrix_UB_21      0.0419195000
_diffrn_orient_matrix_UB_22      0.1267817000
_diffrn_orient_matrix_UB_23      0.0038419000
_diffrn_orient_matrix_UB_31      0.0181623000
_diffrn_orient_matrix_UB_32      -0.0107470000
_diffrn_orient_matrix_UB_33      -0.0796898000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12880
_diffrn_reflns_theta_full        76.52
_diffrn_reflns_theta_max         76.52
_diffrn_reflns_theta_min         4.70
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+1.7340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                3169
_reflns_number_total             3578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3cc05622h2.cif
_cod_data_source_block           chenxi_tshch_0313_auto
_cod_depositor_comments          'Adding full bibliography for 7132546.cif.'
_cod_database_code               7132546
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C17(H17)
;
_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 3.171
_oxdiff_exptl_absorpt_empirical_full_min 0.500