Construction of indeno[1,2-b]pyrroles via chemoselective N-acylation/cyclization/Wittig reaction sequence.
Edukondalu, Athukuri; Vagh, Sandip Sambhaji; Lin, Ting-Han; Lin, Wenwei; Chemical communications (Cambridge, England) 57 (2021) 2045–2048; doi:10.1039/d0cc08184a

data_7127803
_publ_section_title
;
 Construction of indeno[1,2-b]pyrroles via chemoselective
 N-acylation/cyclization/Wittig reaction sequence.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2045
_journal_page_last               2048
_journal_paper_doi               10.1039/d0cc08184a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C31 H21 Br N2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C31 H22 Br N2 O2.5'
_chemical_formula_weight         542.41
_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
_audit_update_record
;
2020-06-14 deposited with the CCDC.	2021-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                96.769(8)
_cell_angle_beta                 100.451(8)
_cell_angle_gamma                97.043(8)
_cell_formula_units_Z            4
_cell_length_a                   11.994(4)
_cell_length_b                   12.841(5)
_cell_length_c                   16.952(6)
_cell_measurement_reflns_used    8059
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19.957
_cell_measurement_theta_min      2.333
_cell_volume                     2521.8(16)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Venture'
_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  0.2092
_diffrn_reflns_av_sigmaI/netI    0.1473
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81656
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         8981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.2037
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+11.6178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.2056
_reflns_number_gt                4395
_reflns_number_total             8981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc08184a2.cif
_cod_data_source_block           d21987
_cod_depositor_comments
;
Adding full bibliography for 7127803--7127811.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2521.9(15)
_cod_original_formula_moiety     'C62 H44 Br2 N4 O5'
_cod_original_formula_sum        'C62 H44 Br2 N4 O5'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1084.83
_cod_database_code               7127803