Crystal structure of ethyl 2-[(4-bromophenyl)amino]-3,4-dimethylpent-3-enoate
Zukerman-Schpector, Julio; Caracelli, I.; Stefani, Hélio A.; Khan, Amna N.; Tiekink, Edward R. T.; Acta Crystallographica Section E 70 (2014) o1122–o1123; doi:10.1107/S1600536814020832

data_2240003
_publ_section_title
;
 Crystal structure of ethyl
 2-[(4-bromophenyl)amino]-3,4-dimethylpent-3-enoate
;
_journal_coeditor_code           HG5408
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1122
_journal_page_last               o1123
_journal_paper_doi               10.1107/S1600536814020832
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C15 H20 Br N O2'
_chemical_formula_moiety         'C15 H20 Br N O2'
_chemical_formula_sum            'C15 H20 Br N O2'
_chemical_formula_weight         326.22
_chemical_name_systematic
;
Ethyl 2-[(4-bromophenyl)amino]-3,4-dimethylpent-3-enoate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                97.557(3)
_cell_angle_beta                 110.520(2)
_cell_angle_gamma                113.866(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8746(6)
_cell_length_b                   12.2023(5)
_cell_length_c                   13.7760(6)
_cell_measurement_reflns_used    6830
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.83
_cell_volume                     1620.20(14)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012),
<i>QMol</i> (Gans & Shalloway, 2001) and
 DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
<i>MarvinSketch</i> (Chemaxon, 2010) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18794
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.277
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.728
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5927
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.9501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                4054
_reflns_number_total             5927
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg5408sup1.cif
_cod_data_source_block           I
_cod_database_code               2240003
_cod_database_fobs_code          2240003