Sulfur-directed carbon-sulfur bond cleavage for Rh-catalyzed regioselective alkynylthiolation of alkynes
Shibata, Takanori; Mitake, Akihito; Akiyama, Yosuke; Kanyiva, Kyalo Stephen; Chem. Commun.  (2017) –; doi:10.1039/C7CC04997H

data_7120484
_publ_section_title
;
 Sulfur-directed carbon-sulfur bond cleavage for Rh-catalyzed
 regioselective alkynylthiolation of alkynes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04997H
_journal_year                    2017
_chemical_formula_moiety         'C43 H45 F3 N O3 P2 Rh S3'
_chemical_formula_sum            'C43 H45 F3 N O3 P2 Rh S3'
_chemical_formula_weight         941.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                97.252(7)
_cell_angle_beta                 101.441(7)
_cell_angle_gamma                112.006(8)
_cell_formula_units_Z            2
_cell_length_a                   10.500(3)
_cell_length_b                   11.062(3)
_cell_length_c                   20.906(6)
_cell_measurement_reflns_used    10987
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      3.06
_cell_volume                     2152.2(11)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17773
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.058
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             968.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.09
_refine_diff_density_min         -1.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1878
_refine_ls_R_factor_gt           0.1393
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0420P)^2^+51.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3003
_refine_ls_wR_factor_ref         0.3303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5703
_reflns_number_total             9199
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7cc04997h2.cif
_cod_data_source_block           20170605shibata-mitake2
_cod_original_cell_volume        2152.1(11)
_cod_database_code               7120484
_shelxl_version_number           2014/6
_shelx_res_checksum              8265