Crystal structures of 4-bromo-2-formyl-1-tosyl-1<i>H</i>-pyrrole, (<i>E</i>)-4-bromo-2-(2-nitrovinyl)-1-tosyl-1<i>H</i>-pyrrole and 6-(4-bromo-1-tosylpyrrol-2-yl)-4,4-dimethyl-5-nitrohexan-2-one
Kingsbury, Christopher J.; Sample, Harry C.; Senge, Mathias O.; Acta Crystallographica Section E 77 (2021) 341–345; doi:10.1107/S2056989021002280

data_2243774
_publ_section_title
;
 Crystal structures of 4-bromo-2-formyl-1-tosyl-1<i>H</i>-pyrrole,
 (<i>E</i>)-4-bromo-2-(2-nitrovinyl)-1-tosyl-1<i>H</i>-pyrrole and
 6-(4-bromo-1-tosylpyrrol-2-yl)-4,4-dimethyl-5-nitrohexan-2-one
;
_journal_coeditor_code           TX2036
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              341
_journal_page_last               345
_journal_paper_doi               10.1107/S2056989021002280
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C12 H10 Br N O3 S'
_chemical_formula_moiety         'C12 H10 Br N O3 S'
_chemical_formula_sum            'C12 H10 Br N O3 S'
_chemical_formula_weight         328.18
_chemical_name_common            4-Bromo-2-formyl-1-tosyl-1<i>H</i>-pyrrole
_chemical_name_systematic
4-Bromo-1-[(4-methylbenzene)sulfonyl]pyrrole-2-carbaldehyde
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8436(5)
_cell_length_b                   13.9149(13)
_cell_length_c                   18.5479(17)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.93
_cell_volume                     1250.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_molecular_graphics    '<i>shelXle</i> (H\"ubschle, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL2018/3</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT2018/2</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23296
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         1.830
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 (SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       rod
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.4002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0450
_reflns_number_gt                3714
_reflns_number_total             3972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2036sup1.cif
_cod_data_source_block           1
_cod_database_code               2243774
_cod_database_fobs_code          2243774
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.833
_shelx_hkl_checksum              94628
_shelx_res_checksum              81064