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_2019733
_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           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_cell_angle_alpha                90
_cell_angle_beta                 111.141(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5188(9)
_cell_length_b                   8.2955(5)
_cell_length_c                   15.9287(10)
_cell_measurement_reflns_used    5556
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      32.6326
_cell_measurement_theta_min      3.0056
_cell_volume                     1542.86(19)
_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(14)
_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  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27795
_diffrn_reflns_theta_full        31.5
_diffrn_reflns_theta_max         31.5
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.1
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.2726
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.58
_refine_diff_density_min         -2.00
_refine_ls_abs_structure_details
'  3424 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.41(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.32
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    30
_refine_ls_number_parameters     224
_refine_ls_number_reflns         9998
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.0196
_refine_ls_shift/su_mean         0.0020
_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          0.0932
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                4208
_reflns_number_total             9998
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            sk3557sup1.cif
_cod_data_source_block           IIb
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2019733
_cod_database_fobs_code          2019733