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_1561295
_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         '0.5(H2 O8 S2), C7.4 H18.2 N, 0.6(C H3)'
_chemical_formula_sum            'C8 H21 N O4 S'
_chemical_formula_weight         227.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.781(5)
_cell_length_b                   8.548(3)
_cell_length_c                   16.228(5)
_cell_measurement_reflns_used    1031
_cell_measurement_temperature    360.00(13)
_cell_measurement_theta_max      15.5340
_cell_measurement_theta_min      2.9010
_cell_volume                     2605.2(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      360.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.4350
_diffrn_detector_type            'Sapphire1, long nozzle'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -67.00 122.60   1.20   35.00    --   28.00   0.00   0.00  158
  2  \w    -36.00  79.20   1.20   35.00    --   34.00 -84.00   0.00   96
  3  \w    -36.00  79.20   1.20   35.00    --   34.00 -84.00  88.00   96
  4  \w    -36.00  79.20   1.20   35.00    --   34.00 -84.00 180.00   96
  5  \w    -36.00  79.20   1.20   35.00    --   34.00 -84.00 268.00   96
  6  \w    -26.00 115.60   1.20   35.00    --   28.00  45.00  45.00  118
  7  \w    -26.00 115.60   1.20   35.00    --   28.00  45.00 135.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0356064000
_diffrn_orient_matrix_UB_12      0.0280876000
_diffrn_orient_matrix_UB_13      -0.0003032000
_diffrn_orient_matrix_UB_21      -0.0127721000
_diffrn_orient_matrix_UB_22      0.0779659000
_diffrn_orient_matrix_UB_23      0.0021964000
_diffrn_orient_matrix_UB_31      0.0009005000
_diffrn_orient_matrix_UB_32      -0.0036479000
_diffrn_orient_matrix_UB_33      0.0435798000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1177
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.988
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1325
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      12.523
_refine_ls_R_factor_all          0.2227
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2841
_refine_ls_wR_factor_ref         0.3409
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                430
_reflns_number_total             1325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc7.cif
_cod_data_source_block           dbaso4_360k_pomiar
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1561295
_chemical_oxdiff_formula         'C64 H80 N8 O32 S8 '
_reflns_odcompleteness_completeness 92.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3D,H3C,H3B} of C3, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H4BA,H4BB,H4BC} of C4B, {H5BA,H5BB,H5BC} of C5B, {H5DA,
  H5DB,H5DC} of C5D, {H5CA,H5CB,H5CC} of C5C, {H5AA,H5AB,H5AC} of C5A, {H4AA,
  H4AB,H4AC} of C4A, {H4CA,H4CB,H4CC} of C4C, {H4DA,H4DB,H4DC} of C4D
2. Restrained distances
 N1-C2_$1
 1.42 with sigma of 0.03
 C5A-C3
 1.45 with sigma of 0.03
 C4C-C3 = C5B-C3 = C5D-C3 = C4D-C3 = C5C-C3 = C4A-C3 = C4B-C3 = C3-C2
 1.45 with sigma of 0.05
 C3-H3A
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5C) \\sim Ueq, Uanis(C4D) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C4B)
\\sim Ueq, Uanis(C4C) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C5D) \\sim Ueq,
Uanis(C5A) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.025
4. Others
 Fixed Sof: H3D(0.2) H3C(0.2) H3B(0.3) C4B(0.3) H4BA(0.3) H4BB(0.3) H4BC(0.3)
 C5B(0.3) H5BA(0.3) H5BB(0.3) H5BC(0.3) C5D(0.2) H5DA(0.2) H5DB(0.2) H5DC(0.2)
 C5C(0.2) H5CA(0.2) H5CB(0.2) H5CC(0.2) C5A(0.3) H5AA(0.3) H5AB(0.3) H5AC(0.3)
 C4A(0.3) H4AA(0.3) H4AB(0.3) H4AC(0.3) C4C(0.2) H4CA(0.2) H4CB(0.2) H4CC(0.2)
 C4D(0.2) H4DA(0.2) H4DB(0.2) H4DC(0.2) H3A(0.3)
5.a Ternary CH refined with riding coordinates:
 C3(H3D), C3(H3C), C3(H3B)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B)
5.c Idealised Me refined as rotating group:
 C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C5D(H5DA,H5DB,H5DC), C5C(H5CA,H5CB,
 H5CC), C5A(H5AA,H5AB,H5AC), C4A(H4AA,H4AB,H4AC), C4C(H4CA,H4CB,H4CC), C4D(H4DA,
 H4DB,H4DC)
;
_olex2_date_sample_data_collection 2014-10-27
_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 1.098
_oxdiff_exptl_absorpt_empirical_full_min 0.916