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_7248870
_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, 0.26(I), 0.74(Br1)'
_chemical_formula_sum            'C6 H13 Br0.74 I0.26 N2'
_chemical_formula_weight         205.31
_chemical_name_systematic        dabcoHBr0.74I0.26
_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             2023-07-31
_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                   6.8015(6)
_cell_length_b                   6.8015(6)
_cell_length_c                   5.3298(4)
_cell_measurement_reflns_used    715
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.6690
_cell_measurement_theta_min      3.4500
_cell_volume                     213.53(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 0.949
_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    -30.00  30.00   0.25    0.80    --   -9.50   2.00 -68.00  240
  2  \w    -18.00  30.00   0.25    0.80    --   -9.50 -99.00-180.00  192
  3  \w     30.00  55.00   0.25    0.80    --    9.97-137.00 121.00  100
;
_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      -0.1169026000
_diffrn_orient_matrix_UB_12      -0.0832126000
_diffrn_orient_matrix_UB_13      -0.0035336000
_diffrn_orient_matrix_UB_21      -0.0286819000
_diffrn_orient_matrix_UB_22      0.0869120000
_diffrn_orient_matrix_UB_23      -0.0009337000
_diffrn_orient_matrix_UB_31      0.0033074000
_diffrn_orient_matrix_UB_32      0.0015559000
_diffrn_orient_matrix_UB_33      -0.1331012000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            803
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.246
_diffrn_reflns_theta_min         3.459
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69350
_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    1.597
_exptl_crystal_description       needle
_exptl_crystal_F_000             103
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 92 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_number_reflns         224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0597P)^2^+0.2711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                224
_reflns_number_total             224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00310a2.cif
_cod_data_source_block           yo_end_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7248867--7248875.cif.'
_cod_original_cell_volume        213.53(4)
_cod_database_code               7248870
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H13N2Br0.7I0.3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.312
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Shared sites
{I1, Br1}
3. Uiso/Uaniso restraints and constraints
Uiso(I1) = Uiso(Br1)
4. Others
 Fixed Sof: H1(0.083333) H1A(0.5) H1B(0.5) I1(0.02167) Br1(0.06167)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              16238
_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 1.668
_oxdiff_exptl_absorpt_empirical_full_min 0.410