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_7248872
_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         '0.03(Cl), 0.97(Br), C6 H13 N2'
_chemical_formula_sum            'C6 H13 Br0.97 Cl0.03 N2'
_chemical_formula_weight         191.76
_chemical_name_systematic        dabcoHCl0.03Br0.97
_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             2023-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_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                   6.6645(5)
_cell_length_b                   6.6645(5)
_cell_length_c                   5.3238(4)
_cell_measurement_reflns_used    914
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.9500
_cell_measurement_theta_min      3.5140
_cell_volume                     204.78(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_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 0.902
_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      5.00  95.00   0.25    0.06    --   13.59   1.00  16.00  360
  2  \w     52.00  78.00   0.25    0.06    --   13.59-136.00-163.00  104
  3  \w    -11.00  24.00   0.25    0.06    --  -12.66  19.00   0.00  140
  4  \w    -15.00  15.00   0.25    0.06    --  -12.66 -99.00-120.00  120
  5  \w    -14.00  32.00   0.25    0.06    --  -12.66 -99.00 -60.00  184
  6  \w    -73.00 -21.00   0.25    0.06    --  -12.66 134.00  82.00  208
;
_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      -0.0761673000
_diffrn_orient_matrix_UB_12      -0.1214633000
_diffrn_orient_matrix_UB_13      -0.0005204000
_diffrn_orient_matrix_UB_21      0.0964391000
_diffrn_orient_matrix_UB_22      -0.0179206000
_diffrn_orient_matrix_UB_23      0.0014933000
_diffrn_orient_matrix_UB_31      -0.0013631000
_diffrn_orient_matrix_UB_32      -0.0001411000
_diffrn_orient_matrix_UB_33      0.1332218000
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1438
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.109
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.804
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             97
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 96 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0556P)^2^+0.0213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                231
_reflns_number_total             236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00310a2.cif
_cod_data_source_block           yo_end_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7248867--7248875.cif.'
_cod_database_code               7248872
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H13N2Br0.97Cl0.03
_shelx_estimated_absorpt_t_max   0.432
_shelx_estimated_absorpt_t_min   0.152
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Shared sites
{Cl1, Br1}
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(Br1)
4. Others
 Fixed Sof: Cl1(0.0025) Br1(0.08083) H1(0.083333) H1A(0.5) H1B(0.5)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              89048
_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 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.773