Insight into the structure and transport properties of pyrrolidinium-based geminal dicationic-organic ionic crystals: unravelling the role of alkyl-chain length.
Mahapatra, Amita; Samantara, Aneeya K.; Barik, Sahadev; Sahoo, Malaya K.; Behera, J. N.; Sarkar, Moloy; Soft matter 19 (2023) 3510–3518; doi:10.1039/d3sm00040k

data_1569069
_publ_section_title
;
 Insight into the structure and transport properties of
 pyrrolidinium-based geminal dicationic-organic ionic crystals:
 unravelling the role of alkyl-chain length.
;
_journal_issue                   19
_journal_name_full               'Soft matter'
_journal_page_first              3510
_journal_page_last               3518
_journal_paper_doi               10.1039/d3sm00040k
_journal_volume                  19
_journal_year                    2023
_chemical_formula_moiety         'Br, C8 H17 N, H2 O'
_chemical_formula_sum            'C8 H19 Br N O'
_chemical_formula_weight         225.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-11-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2023-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                81.434(4)
_cell_angle_beta                 78.227(4)
_cell_angle_gamma                66.545(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2705(3)
_cell_length_b                   8.3119(4)
_cell_length_c                   8.6304(4)
_cell_measurement_reflns_used    12159
_cell_measurement_temperature    294.6(5)
_cell_measurement_theta_max      28.7450
_cell_measurement_theta_min      3.4780
_cell_volume                     531.30(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.6(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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     13.00  63.00   0.50    5.54    --   -0.01-144.00-162.00  100
  2  \w      3.00  52.00   0.50    5.54    --   -0.01-126.00   6.00   98
  3  \w     -3.00  66.00   0.50    5.54    --   -0.01  38.00-180.00  138
  4  \w    -68.00   9.00   0.50    5.54    --   -0.01 -14.00  26.90  154
  5  \w    -20.00  36.00   0.50    5.54    --   -0.01 -99.00 120.00  112
  6  \w    -64.00  23.00   0.50    5.54    --   -0.01 -77.00-120.00  174
  7  \w      0.00  49.00   0.50    5.54    --   -0.01-122.00 107.00   98
  8  \w     -6.00  69.00   0.50    5.54    --   -0.01  19.00-120.00  150
  9  \w    -69.00  15.00   0.50    5.54    --   -0.01  -9.00  60.26  168
 10  \w    -69.00  15.00   0.50    5.54    --   -0.01  -9.00 147.01  168
 11  \w    -68.00   9.00   0.50    5.54    --   -0.01 -13.00 -88.34  154
 12  \w    -68.00   9.00   0.50    5.54    --   -0.01 -13.00-150.60  154
 13  \w     -6.00  69.00   0.50    5.54    --   -0.01  19.00 -30.00  150
 14  \w    -69.00   6.00   0.50    5.54    --   -0.01 -19.00 120.00  150
 15  \w     -6.00  69.00   0.50    5.54    --   -0.01  19.00 120.00  150
 16  \w    -69.00  13.00   0.50    5.54    --   -0.01 -10.00 178.44  164
 17  \w    -23.00   2.00   0.50    5.54    --   -0.01  77.00 -90.00   50
 18  \w    -20.00  36.00   0.50    5.54    --   -0.01 -99.00   0.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0358273000
_diffrn_orient_matrix_UB_12      0.0674267000
_diffrn_orient_matrix_UB_13      -0.0587102000
_diffrn_orient_matrix_UB_21      0.0484444000
_diffrn_orient_matrix_UB_22      -0.0589034000
_diffrn_orient_matrix_UB_23      -0.0600023000
_diffrn_orient_matrix_UB_31      -0.0730595000
_diffrn_orient_matrix_UB_32      -0.0262008000
_diffrn_orient_matrix_UB_33      0.0064171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19379
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
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    1.407
_exptl_crystal_description       needle
_exptl_crystal_F_000             234
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0723P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1959
_reflns_number_total             2191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm00040k2.cif
_cod_data_source_block           ms-a-d6py
_cod_depositor_comments
'Adding full bibliography for 1569069--1569071.cif.'
_cod_database_code               1569069
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C16 H34 Br2 N4 O1 '
_diffrn_oxdiff_ac3_digest_frames
;
01b20ea653cc2baa95b98b2259da183dd3000268fb8
;
_diffrn_oxdiff_ac3_digest_hkl
;
01064a51fd33fc58b8f373295bbf08fa8d3ee4
;
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C004(H00A,H00B), C005(H00C,H00D), C006(H00E,H00F), C007(H00G,H00H), C008(H00I,
 H00J), C009(H00K,H00L), C00B(H00P,H00Q)
2.b Idealised Me refined as rotating group:
 C00A(H00M,H00N,H00O)
;
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.638