Structure, dielectric and electric properties of diisobutylammonium hydrogen sulfate crystal
Bednarchuk, Tamara J.; Kinzhybalo, Vasyl; Markiewicz, Ewa; Hilczer, Bożena; Pietraszko, Adam; Journal of Solid State Chemistry 258 (2018) 753–761; doi:10.1016/j.jssc.2017.11.042

data_1561294
_publ_section_title
;
 Structure, dielectric and electric properties of diisobutylammonium
 hydrogen sulfate crystal
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              753
_journal_page_last               761
_journal_paper_doi               10.1016/j.jssc.2017.11.042
_journal_volume                  258
_journal_year                    2018
_chemical_formula_moiety         'H O4 S, C8 H20 N'
_chemical_formula_sum            'C8 H21 N O4 S'
_chemical_formula_weight         227.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 110.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.12(4)
_cell_length_b                   16.178(5)
_cell_length_c                   8.476(3)
_cell_measurement_reflns_used    1207
_cell_measurement_temperature    330.01(11)
_cell_measurement_theta_max      19.9270
_cell_measurement_theta_min      3.5630
_cell_volume                     1303(5)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      330.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -28.00  85.00   1.00   62.50    --    5.88  77.00 -60.00  113
  2  \w    -89.00  39.00   1.00   62.50    --   -7.21 -19.00  30.00  128
  3  \w    -25.00  48.00   1.00   62.50    --    5.88 -99.00-180.00   73
  4  \w    -25.00  22.00   1.00   62.50    --    5.88 -99.00 -60.00   47
  5  \w    -37.00  67.00   1.00   62.50    --   -7.21  57.00  30.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0676016000
_diffrn_orient_matrix_UB_12      0.0185335000
_diffrn_orient_matrix_UB_13      0.0309433000
_diffrn_orient_matrix_UB_21      -0.0312643000
_diffrn_orient_matrix_UB_22      0.0384864000
_diffrn_orient_matrix_UB_23      0.0064636000
_diffrn_orient_matrix_UB_31      0.0046603000
_diffrn_orient_matrix_UB_32      -0.0098725000
_diffrn_orient_matrix_UB_33      0.0832753000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1853
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4199
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.299
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83764
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         4199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.2487
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.2078
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1170
_reflns_number_total             4199
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9478\% 
 around [-0.38 0.00 0.93] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            mmc6.cif
_cod_data_source_block           dibahs330_2c_twin1_hklf4
_cod_database_code               1561294
_chemical_oxdiff_formula         'C32 H84 N4 O16 S4 '
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.548(3)
 0.452(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Ternary CH refined with riding coordinates:
 C3(H3), C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), N1(H1A,H1B)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.133
_oxdiff_exptl_absorpt_empirical_full_min 0.889
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2