[4 + 1] Cycloaddition Reaction of α,β-Alkynic Hydrazones and KSCN under Transition-Metal-Free Conditions: Synthesis of N-Iminoisothiazolium Ylides.
Liu, Bei-Bei; Cao, Wen-Bin; Wang, Fei; Wang, Shun-Yi; Ji, Shun-Jun; The Journal of organic chemistry 83 (2018) 11118–11124; doi:10.1021/acs.joc.8b01725

data_4035643
_publ_section_title
;
 [4 + 1] Cycloaddition Reaction of \a,\b-Alkynic Hydrazones and KSCN under
 Transition-Metal-Free Conditions: Synthesis of N-Iminoisothiazolium
 Ylides.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11118
_journal_page_last               11124
_journal_paper_doi               10.1021/acs.joc.8b01725
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C22 H18 N2 O3 S2'
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_space_group_name_Hall           '-P 2ybc'
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_cell_measurement_theta_min      3.3770
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_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'Bruker SHELXTL'
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_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_point_group_measured_fraction_full 0.992
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_diffrn_reflns_theta_max         30.973
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_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0200
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_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     0
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1059P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2796
_reflns_number_total             6457
_reflns_threshold_expression     'I > 2\s(I)'
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