Synthesis of Amide Enol Carbamates and Carbonates through Cu(OTf)<sub>2</sub>-Catalyzed Reactions of Ynamides with <i>t</i>-Butyl Carbamates/Carbonates.
Han, Pan; Mao, Zhuo-Ya; Li, Ming; Si, Chang-Mei; Wei, Bang-Guo; Lin, Guo-Qiang; The Journal of organic chemistry 85 (2020) 4740–4752; doi:10.1021/acs.joc.9b03512

data_4038082
_publ_section_title
;
 Synthesis of Amide Enol Carbamates and Carbonates through
 Cu(OTf)<sub>2</sub>-Catalyzed Reactions of Ynamides with <i>t</i>-Butyl
 Carbamates/Carbonates.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4740
_journal_page_last               4752
_journal_paper_doi               10.1021/acs.joc.9b03512
_journal_volume                  85
_journal_year                    2020
_chemical_formula_sum            'C28 H28 Br N2 O5 S'
_chemical_formula_weight         584.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                73.900(4)
_cell_angle_beta                 73.965(4)
_cell_angle_gamma                79.977(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3713(10)
_cell_length_b                   12.9078(15)
_cell_length_c                   13.4996(15)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    274.(2)
_cell_measurement_theta_max      69.0594
_cell_measurement_theta_min      3.5840
_cell_volume                     1339.4(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      274.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'd8 venture'
_diffrn_radiation_type           'cu k\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0407
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18284
_diffrn_reflns_theta_full        69.08
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_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    3.161
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.762
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0421P)^2^+1.2776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                4608
_reflns_number_total             4798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03512_si_002.cif
_cod_data_source_block           20190720ASCM110
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4038081--4038082.cif.
;
_cod_database_code               4038082
_shelx_res_checksum              73042
_shelx_hkl_checksum              16393