Synthesis of α-methylene-δ-oxo-γ-amino esters via Rh(ii)-catalyzed coupling of 1-sulfonyl-1,2,3-triazoles with Morita-Baylis-Hillman adducts.
Jeon, Hyun Ji; Kwak, Mi Soo; Jung, Da Jung; Bouffard, Jean; Lee, Sang-Gi; Organic & biomolecular chemistry 14 (2016) 11238–11243; doi:10.1039/c6ob02086k

data_7155366
_publ_section_title
;
 Synthesis of \a-methylene-\d-oxo-\g-amino esters via Rh(ii)-catalyzed
 coupling of 1-sulfonyl-1,2,3-triazoles with Morita-Baylis-Hillman
 adducts.
;
_journal_issue                   47
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              11238
_journal_page_last               11243
_journal_paper_doi               10.1039/c6ob02086k
_journal_volume                  14
_journal_year                    2016
_chemical_formula_sum            'C27 H27 N O5 S'
_chemical_formula_weight         477.55
_chemical_name_common            HG-01
_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
_audit_update_record
;
2016-04-19 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                70.003(4)
_cell_angle_beta                 83.089(4)
_cell_angle_gamma                89.062(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1944(8)
_cell_length_b                   10.8330(9)
_cell_length_c                   13.2249(12)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    170.(2)
_cell_measurement_theta_max      28.3799
_cell_measurement_theta_min      2.6095
_cell_volume                     1228.40(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      170.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20790
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.491
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0892
_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^)+4.0725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                3442
_reflns_number_total             4272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob02086k2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7155365--7155366.cif.'
_cod_database_code               7155366