Copper-catalyzed C-H/N-H annulation of enaminones and alkynyl esters for densely substituted pyrrole synthesis
Fu, Leiqing; Wan, Jie-Ping; Zhou, Liyun; Liu, Yunyun; Chemical Communications  (2022) –; doi:10.1039/D1CC06768K

data_7129543
_publ_section_title
;
 Copper-catalyzed C-H/N-H annulation of enaminones and alkynyl esters for
 densely substituted pyrrole synthesis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06768K
_journal_year                    2022
_chemical_formula_moiety         'C20 H20 N2 O5, H2 O'
_chemical_formula_sum            'C20 H22 N O6'
_chemical_formula_weight         372.38
_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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
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_cell_length_b                   8.4598(17)
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_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     990.4(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
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_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      295(2)
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_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0670
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_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       8
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_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.981
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_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.995
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       plate
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     253
_refine_ls_number_reflns         3434
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0845P)^2^+0.1041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
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_reflns_number_total             3434
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           shx97
_cod_original_cell_volume        990.3(4)
_cod_database_code               7129543
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              41358