One-pot Synthesis of Benzotripyrrole Derivatives from 1H-pyrroles
Pandeeti, Obaiah; Kumar, Sathish B.; Panda, Pradeepta; New Journal of Chemistry 43 (2019) 18437–18441; doi:10.1039/C9NJ04700J

data_7058956
_publ_section_title
;
 One-pot Synthesis of Benzotripyrrole Derivatives from 1H-pyrroles
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18437
_journal_page_last               18441
_journal_paper_doi               10.1039/C9NJ04700J
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C8 H9 Br I N O2'
_chemical_formula_sum            'C8 H9 Br I N O2'
_chemical_formula_weight         357.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-19 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9046(5)
_cell_length_b                   8.2466(4)
_cell_length_c                   14.0533(6)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.92
_cell_volume                     1106.56(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18333
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.108
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_min         3.825
_exptl_absorpt_coefficient_mu    6.475
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0424
_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^)+(0.1000P)^2^+0.2933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                3530
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04700j2.cif
_cod_data_source_block           bripe
_cod_database_code               7058956
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.7158
_shelx_estimated_absorpt_t_max   0.7459
_shelx_res_checksum              10634