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_2243775
_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_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_moiety         'C13 H11 Br N2 O4 S'
_chemical_formula_sum            'C13 H11 Br N2 O4 S'
_chemical_formula_weight         371.21
_chemical_name_common            (E)-4-bromo-2-(2-nitrovinyl)-1-tosyl-1H-pyrrole
_chemical_name_systematic        (E)-4-bromo-2-(2-nitrovinyl)-1-tosyl-1H-pyrrole
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                83.423(3)
_cell_angle_beta                 80.393(3)
_cell_angle_gamma                85.693(3)
_cell_formula_units_Z            2
_cell_length_a                   6.8904(4)
_cell_length_b                   8.3224(4)
_cell_length_c                   12.8763(7)
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      3.50
_cell_volume                     722.06(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7190
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.205
_diffrn_reflns_theta_min         3.500
_exptl_absorpt_coefficient_mu    5.403
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5443
_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    1.707
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.627
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0491
_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^)+(0.1118P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                2378
_reflns_number_total             2617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2036sup1.cif
_cod_data_source_block           2
_cod_database_code               2243775
_cod_database_fobs_code          2243775
_shelx_estimated_absorpt_t_min   0.672
_shelx_estimated_absorpt_t_max   0.948
_shelx_hkl_checksum              58160
_shelx_res_checksum              59569