A Rh-catalyzed 1,2-sulfur migration/aza-Diels-Alder cascade initiated by aza-vinyl carbenoids from sulfur-tethered N-sulfonyl-1,2,3-triazoles
Yu Jiang; Xiang-Ying Tang; Min Shi; Chem.Commun. 51 (2015) 2122–; doi:10.1039/C4cc08829H

data_7116450
_publ_section_title
;
 A Rh-catalyzed 1,2-sulfur migration/aza-Diels-Alder cascade initiated by
 aza-vinyl carbenoids from sulfur-tethered N-sulfonyl-1,2,3-triazoles
;
_journal_name_full               Chem.Commun.
_journal_page_first              2122
_journal_paper_doi               10.1039/C4cc08829H
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C36 H38 N2 O4 S4'
_chemical_formula_weight         690.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-10 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.066(3)
_cell_angle_beta                 107.053(3)
_cell_angle_gamma                97.126(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5970(13)
_cell_length_b                   13.9714(19)
_cell_length_c                   14.765(2)
_cell_measurement_reflns_used    4175
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.764
_cell_measurement_theta_min      4.914
_cell_volume                     1784.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10140
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.519
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+0.0712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5329
_reflns_number_total             6514
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           cd214392
_cod_database_code               7116450
_shelxl_version_number           2013-4
_shelx_res_checksum              1832