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_7116449
_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_absolute_configuration unk
_chemical_formula_sum            'C34 H34 N2 O4 S4'
_chemical_formula_weight         662.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-04-09 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.621(7)
_cell_length_b                   26.533(8)
_cell_length_c                   9.756(3)
_cell_measurement_reflns_used    1793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.536
_cell_measurement_theta_min      4.663
_cell_volume                     7409(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 0.979
_diffrn_measured_fraction_theta_max 0.999
_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_unetI/netI     0.2008
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.093
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.045
_platon_squeeze_details
;
;
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
; 
 Flack x determined using 776 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.56(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6523
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0888P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1994
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2591
_reflns_number_total             6523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08829h2.cif
_cod_data_source_block           cd214198
_cod_original_cell_volume        7409(3)
_cod_database_code               7116449
_shelxl_version_number           2013-4
_shelx_res_checksum              10887