Effect of halide solid solution on the structure, phase transition behaviour and dielectric properties of dabcoH+ chains
Ohishi, Yuki; Sambe, Kohei; Dekura, Shun; Akutagawa, Tomoyuki; Masuya-Suzuki, Atsuko; Tsunashima, Ryo; CrystEngComm 26 (2024) 3468–3474; doi:10.1039/D4CE00310A

data_7248869
_publ_section_title
;
 Effect of halide solid solution on the structure, phase transition
 behaviour and dielectric properties of dabcoH+ chains
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3468
_journal_page_last               3474
_journal_paper_doi               10.1039/D4CE00310A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C6 H13 N2, 0.36(I), 0.64(Br)'
_chemical_formula_sum            'C6 H13 Br0.64 I0.36 N2'
_chemical_formula_weight         210.01
_chemical_name_systematic        dabcoHBr0.64I0.36
_space_group_crystal_system      hexagonal
_space_group_IT_number           187
_space_group_name_Hall           'P -6 2'
_space_group_name_H-M_alt        'P -6 m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   6.8337(5)
_cell_length_b                   6.8337(5)
_cell_length_c                   5.3349(3)
_cell_measurement_reflns_used    1051
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.4670
_cell_measurement_theta_min      3.4390
_cell_volume                     215.76(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -85.00 -60.00   0.25    2.16    --  -12.77 157.00 126.00  100
  2  \w    -39.00 -13.00   0.25    2.16    --  -12.77 119.00 -28.00  104
  3  \w     17.00  42.00   0.25    2.16    --   13.32-119.00-113.00  100
  4  \w     61.00  88.00   0.25    2.16    --   13.32-157.00  91.00  108
  5  \w    -88.00  12.00   0.25    2.16    --  -12.77 -57.00-180.00  400
  6  \w    -16.00  58.00   0.25    2.16    --   13.32 -99.00  90.00  296
  7  \w     12.00  40.00   0.25    2.16    --   13.32 -57.00 150.00  112
  8  \w    -62.00 -25.00   0.25    2.16    --   13.32 -57.00 150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0897109000
_diffrn_orient_matrix_UB_12      0.1133015000
_diffrn_orient_matrix_UB_13      -0.0074417000
_diffrn_orient_matrix_UB_21      -0.0791490000
_diffrn_orient_matrix_UB_22      0.0368169000
_diffrn_orient_matrix_UB_23      -0.0203079000
_diffrn_orient_matrix_UB_31      -0.0068665000
_diffrn_orient_matrix_UB_32      0.0122971000
_diffrn_orient_matrix_UB_33      0.1312417000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1547
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         3.442
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       needle
_exptl_crystal_F_000             104
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Flack x determined using 94 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_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0525
_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^)+(0.1013P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                237
_reflns_number_total             240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00310a2.cif
_cod_data_source_block           yo_end_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7248867--7248875.cif.'
_cod_database_code               7248869
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H13N2Br0.65I0.35
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1(10)
 0(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
3. Shared sites
{I1, Br1}
4. Uiso/Uaniso restraints and constraints
Uiso(I1) = Uiso(Br1)
5. Others
 Fixed Sof: H1(0.083333) H1A(0.5) H1B(0.5) I1(0.03) Br1(0.05333)
6.a Ternary CH refined with riding coordinates:
 N1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              15658
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.730