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_2019731
_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 Cl N2 O2'
_chemical_formula_moiety         'C6 H5 Cl N2 O2'
_chemical_formula_sum            'C6 H5 Cl N2 O2'
_chemical_formula_weight         172.6
_chemical_melting_point          378
_chemical_name_systematic
;
4-Chloro-3-nitroaniline
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 110.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7260(4)
_cell_length_b                   7.9721(2)
_cell_length_c                   15.0098(4)
_cell_measurement_reflns_used    14208
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      66.9519
_cell_measurement_theta_min      3.1383
_cell_volume                     1427.73(7)
_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      120.00(10)
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '4-circle 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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0104
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23718
_diffrn_reflns_theta_full        67.05
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         3.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.335
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro (Agilent Technologies, 2012)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.6052
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.4474
_exptl_crystal_size_mid          0.1313
_exptl_crystal_size_min          0.0624
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.16
_refine_ls_abs_structure_details
'  2479 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.504(15)
_refine_ls_extinction_coef       96E1(9)
_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   1.94
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    58
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.0496
_refine_ls_shift/su_mean         0.0122
_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          0.0647
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                4733
_reflns_number_total             5014
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            sk3557sup1.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2019731
_cod_database_fobs_code          2019731