A mechanistic study on the SHi reaction at tin atoms in a radical cascade reaction
Kamimura, Akio; Yoshinaga, Tatsuro; Noguchi, Fumiaki; Miyazaki, Koichiro; Uno, Hidemitsu; Organic Chemistry Frontiers 2 (2015) 713–; doi:10.1039/C5QO00063G

data_1553118
_publ_section_title
;
 A mechanistic study on the SHi reaction at tin atoms in a radical cascade
 reaction
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              713
_journal_paper_doi               10.1039/C5QO00063G
_journal_volume                  2
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C32 H37 N O4 S Sn'
_chemical_formula_sum            'C32 H37 N O4 S Sn'
_chemical_formula_weight         650.40
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-02-20 deposited with the CCDC.
2015-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.673(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   8.592(7)
_cell_length_b                   10.956(9)
_cell_length_c                   16.545(14)
_cell_measurement_reflns_used    5696
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.98
_cell_measurement_theta_min      2.23
_cell_volume                     1556(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28818
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             668.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.810
_refine_diff_density_min         -2.430
_refine_ls_abs_structure_details
;
 Flack x determined using 2089 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0869
_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^)+(0.0964P)^2^+1.0155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                6877
_reflns_number_total             8807
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5qo00063g2.cif
_cod_data_source_block           ProfKamimura
_cod_original_cell_volume        1556(3)
_cod_database_code               1553118
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-2
_shelx_res_checksum              56212
_shelx_hkl_checksum              68290