Synthesis of Polycarbonyl Pyrroles via K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>-Mediated Oxidative Cyclization of Enamines.
Gao, Peng; Wang, Juan; Bai, Zi-Jing; Shen, Li; Yan, Yun-Yun; Yang, De-Suo; Fan, Ming-Jin; Guan, Zheng-Hui; Organic letters 18 (2016) 6074–6077; doi:10.1021/acs.orglett.6b03060

data_1555934
_publ_section_title
;
 Synthesis of Polycarbonyl Pyrroles via
 K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>-Mediated Oxidative Cyclization of
 Enamines.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              6074
_journal_page_last               6077
_journal_paper_doi               10.1021/acs.orglett.6b03060
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C24 H21 N O6'
_chemical_formula_weight         419.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.190(2)
_cell_angle_beta                 75.871(2)
_cell_angle_gamma                74.332(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3578(5)
_cell_length_b                   12.1840(10)
_cell_length_c                   13.0111(10)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.96
_cell_volume                     1089.10(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21510
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.9817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1151P)^2^+0.1254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1936
_reflns_number_gt                3368
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03060_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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      P-1
_cod_database_code               1555934