Transfer of chirality in the rhodium-catalyzed intramolecular formal hetero-[5 + 2] cycloaddition of vinyl aziridines and alkynes: stereoselective synthesis of fused azepine derivatives.
Feng, Jian-Jun; Lin, Tao-Yan; Wu, Hai-Hong; Zhang, Junliang; Journal of the American Chemical Society 137 (2015) 3787–3790; doi:10.1021/jacs.5b01305

data_4129369
_publ_section_title
;
 Transfer of chirality in the rhodium-catalyzed intramolecular formal
 hetero-[5 + 2] cycloaddition of vinyl aziridines and alkynes:
 stereoselective synthesis of fused azepine derivatives.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3787
_journal_page_last               3790
_journal_paper_doi               10.1021/jacs.5b01305
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C23 H26 N2 O4 S2'
_chemical_formula_weight         458.58
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
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_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4926(4)
_cell_length_b                   15.1772(8)
_cell_length_c                   21.5393(11)
_cell_measurement_temperature    296(2)
_cell_volume                     2776.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0704
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38207
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_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.218
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_exptl_absorpt_correction_T_min  0.9335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(10)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6713
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_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1086
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                3670
_reflns_number_total             6713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01305_si_001.cif
_cod_data_source_block           z
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4129369