Synthesis and properties of 1-methylthiopropargylammonium salts and their use as key precursors to sulfur-containing enediynes.
Murai, Toshiaki; Fukushima, Kozue; Mutoh, Yuichiro; Organic letters 9 (2007) 5295–5298; doi:10.1021/ol7024923

data_1505653
_publ_section_title
;
 Synthesis and properties of 1-methylthiopropargylammonium salts and their
 use as key precursors to sulfur-containing enediynes.
;
_journal_issue                   25
_journal_name_full               'Organic letters'
_journal_page_first              5295
_journal_page_last               5298
_journal_paper_doi               10.1021/ol7024923
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C44 H36 S2 Si2 '
_chemical_formula_sum            'C44 H36 S2 Si2'
_chemical_formula_weight         685.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                83.02(1)
_cell_angle_beta                 79.53(1)
_cell_angle_gamma                71.495(9)
_cell_formula_units_Z            1
_cell_length_a                   8.861(3)
_cell_length_b                   9.632(4)
_cell_length_c                   11.954(5)
_cell_measurement_reflns_used    3075
_cell_measurement_temperature    253.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     949.2(6)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  'teXsan Ver. 2.0'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9689
_diffrn_measured_fraction_theta_max 0.9689
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7398
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             360.00
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.340
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4214
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.12400(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                3805
_reflns_number_total             4214
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol7024923-file003.cif
_cod_data_source_block           '_5g'
_cod_original_cell_volume        949.1(7)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C44 H36 S2 Si2 '
_cod_database_code               1505653