Temperature-induced reversible structural phase transition and X-ray diffuse scattering in 2-amino-3-nitropyridinium hydrogen sulfate
Bednarchuk, Tamara J.; Kowalska, Dorota; Kinzhybalo, Vasyl; Wołcyrz, Marek; Acta Crystallographica Section B 73 (2017) 337–346; doi:10.1107/S2052520617001524

data_2108094
_publ_section_title
;
 Temperature-induced reversible structural phase transition and X-ray
 diffuse scattering in 2-amino-3-nitropyridinium hydrogen sulfate
;
_journal_coeditor_code           WF5131
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              337
_journal_page_last               346
_journal_paper_doi               10.1107/S2052520617001524
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C5 H6 N3 O2, H O4 S'
_chemical_formula_sum            'C5 H7 N3 O6 S'
_chemical_formula_weight         237.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.891(5)
_cell_length_b                   4.586(3)
_cell_length_c                   10.941(4)
_cell_measurement_reflns_used    2457
_cell_measurement_temperature    304.00(13)
_cell_measurement_theta_max      25.7640
_cell_measurement_theta_min      2.9330
_cell_volume                     897.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      304.00(13)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5597
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.609
_diffrn_reflns_theta_min         2.941
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.247
_refine_ls_abs_structure_details
;
 Flack x determined using 525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       0.0065(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1951
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.1468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                1528
_reflns_number_total             1951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wf5131sup1.cif
_cod_data_source_block           I
_cod_database_code               2108094
_cod_database_fobs_code          2108094