High- and low-temperature phases in isostructural 4-chloro-3-nitroaniline and 4-iodo-3-nitroaniline
Fábry, Jan; Dušek, Michal; Vaněk, Přemysl; Rafalovskyi, Iegor; Hlinka, Jiří; Urban, Jiří; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614024632

data_2019732
_publ_section_title
;
 High- and low-temperature phases in isostructural 4-chloro-3-nitroaniline
 and 4-iodo-3-nitroaniline
;
_journal_coeditor_code           SK3557
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614024632
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C6 H5 I N2 O2'
_chemical_formula_moiety         'C6 H5 I N2 O2'
_chemical_formula_sum            'C6 H5 I N2 O2'
_chemical_formula_weight         264
_chemical_melting_point          413
_chemical_name_systematic
;
4-Iodo-3-nitroaniline
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 111.556(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.5219(8)
_cell_length_b                   4.2601(3)
_cell_length_c                   16.0008(9)
_cell_measurement_reflns_used    3022
_cell_measurement_temperature    293
_cell_measurement_theta_max      66.7290
_cell_measurement_theta_min      3.8580
_cell_volume                     793.86(9)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
<i>PLATON</i> (Spek, 2009) and <i>DIAMOND</i> (Brandenburg & Putz,
2010)
;
_computing_structure_refinement
;
<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
<i>SIR97</i> (Altomare <i>et al.</i>, 1997)
;
_diffrn_ambient_temperature      293
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_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur (Atlas, Gemini ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5100
_diffrn_reflns_theta_full        67.03
_diffrn_reflns_theta_max         67.03
_diffrn_reflns_theta_min         3.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.339
_exptl_absorpt_correction_T_max  0.361
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.2083
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.5031
_exptl_crystal_size_mid          0.2430
_exptl_crystal_size_min          0.0460
_refine_diff_density_max         1.90
_refine_diff_density_min         -0.85
_refine_ls_extinction_coef       22E1(5)
_refine_ls_extinction_method
;
B--C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). <i>Acta Cryst.</i> A<b>30</b>, 129--147]
;
_refine_ls_goodness_of_fit_ref   2.31
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    14
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1380
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.0149
_refine_ls_shift/su_mean         0.0022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                1093
_reflns_number_total             1380
_reflns_threshold_expression     I>3\s(I)
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_cod_data_source_block           IIa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019732
_cod_database_fobs_code          2019732