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_2243776
_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         'C19 H23 Br N2 O5 S'
_chemical_formula_sum            'C19 H23 Br N2 O5 S'
_chemical_formula_weight         471.36
_chemical_name_common
;
6-(4-bromo-1-tosylpyrrol-2-yl)-4,4-dimethyl-5-nitrohexan-2-one
;
_chemical_name_systematic
;
6-(4-bromo-1-tosylpyrrol-2-yl)-4,4-dimethyl-5-nitrohexan-2-one
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7375(2)
_cell_length_b                   15.9728(3)
_cell_length_c                   16.7621(3)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.08
_cell_measurement_theta_min      2.75
_cell_volume                     2068.68(8)
_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 0.999
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            226885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         46.515
_diffrn_reflns_theta_min         1.762
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.614
_exptl_crystal_size_mid          0.558
_exptl_crystal_size_min          0.546
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.719
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         18433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                15578
_reflns_number_total             18433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2036sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243776
_cod_database_fobs_code          2243776
_shelx_estimated_absorpt_t_min   0.356
_shelx_estimated_absorpt_t_max   0.391
_shelx_hkl_checksum              46503
_shelx_res_checksum              17546