Semi-organic salts of aniline with inorganic acids: prospective materials for the second harmonic generation
Matulková, Irena; Cihelka, Jaroslav; Fejfarová, Karla; Dušek, Michal; Pojarová, Michaela; Vaněk, Přemysl; Kroupa, Jan; Šála, Michal; Krupková, Radmila; Němec, Ivan; CrystEngComm 13 (2011) 4131–; doi:10.1039/c1ce05170a

data_7205999
_publ_section_title
;
 Semi-organic salts of aniline with inorganic acids: prospective
 materials for the second harmonic generation
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4131
_journal_paper_doi               10.1039/c1ce05170a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         '2(C6 H8 N), O4 S'
_chemical_formula_sum            'C12 H16 N2 O4 S'
_chemical_formula_weight         284.3
_chemical_name_common            'anilinium sulphate'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.612(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.2672(13)
_cell_length_b                   6.2707(2)
_cell_length_c                   7.4449(2)
_cell_measurement_reflns_used    4186
_cell_measurement_temperature    290.0
_cell_measurement_theta_max      58.8521
_cell_measurement_theta_min      3.0319
_cell_volume                     1359.78(8)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Oxford diffraction, 2010)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Diamond (Brandenburg & Putz, 2005)'
_computing_publication_material  Jana2006
_computing_structure_refinement
'Jana2006 (Pet\<r\'i\<cek, Du\<sek & Palatinus, 2006)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      290
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Atlas (Gemini ultra Cu)'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4720
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Oxford diffraction, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        58.73
_diffrn_reflns_theta_max         58.73
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction (2010),
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.3884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.5416
_exptl_crystal_size_mid          0.2369
_exptl_crystal_size_min          0.1150
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details
;
Flack (1983), 823 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.72
_refine_ls_goodness_of_fit_ref   1.68
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    65
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.0194
_refine_ls_shift/su_mean         0.0016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                1707
_reflns_number_total             1887
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c1ce05170a.txt
_cod_data_source_block           an2SO4
_cod_original_formula_sum        'C12 H16 N2 O4 S1'
_cod_database_code               7205999