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_1569071
_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, C9 H19 N, H2 O'
_chemical_formula_sum            'C9 H21 Br N O'
_chemical_formula_weight         239.18
_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                94.525(5)
_cell_angle_beta                 105.831(5)
_cell_angle_gamma                117.457(7)
_cell_formula_units_Z            2
_cell_length_a                   8.7747(6)
_cell_length_b                   8.8458(6)
_cell_length_c                   8.9862(5)
_cell_measurement_reflns_used    7724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.8170
_cell_volume                     578.09(8)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.00  53.00   0.50    7.50    --    3.67-122.00 -58.00  106
  2  \w     16.00  72.00   0.50    7.50    --    3.67-151.00 139.00  112
  3  \w     16.00  64.00   0.50    7.50    --   -3.98-151.00 139.00   96
  4  \w    -20.00  40.00   0.50    7.50    --    3.67 -99.00-180.00  120
  5  \w    -59.00  15.00   0.50    7.50    --    3.67 -57.00  30.00  148
  6  \w    -19.00  68.00   0.50    7.50    --    3.67  77.00-180.00  174
  7  \w    -66.00   9.00   0.50    7.50    --    3.67 -19.00  60.00  150
  8  \w    -66.00   9.00   0.50    7.50    --    3.67 -19.00 150.00  150
  9  \w      0.00  70.00   0.50    7.50    --    3.67  38.00 120.00  140
 10  \w    -57.00 -26.00   0.50    7.50    --   -3.98 128.00 171.81   62
 11  \w    -10.00  66.00   0.50    7.50    --   -3.98  19.00   0.00  152
 12  \w    -56.00 -24.00   0.50    7.50    --   -3.98 126.00  74.31   64
 13  \w    -68.00  19.00   0.50    7.50    --   -3.98 -77.00   0.00  174
 14  \w    -56.00 -24.00   0.50    7.50    --   -3.98 126.00 -11.41   64
 15  \w    -55.00 -23.00   0.50    7.50    --   -3.98 125.00 135.60   64
 16  \w    -67.00   8.00   0.50    7.50    --   -3.98 -57.00-120.00  150
 17  \w    -59.00 -27.00   0.50    7.50    --   -3.98 131.00-158.65   64
 18  \w    -62.00 -31.00   0.50    7.50    --   -3.98 137.00-109.45   62
 19  \w    -59.00 -27.00   0.50    7.50    --   -3.98 131.00 -47.23   64
 20  \w     -2.00  52.00   0.50    7.50    --    3.67-120.00  14.51  108
 21  \w    -20.00  40.00   0.50    7.50    --    3.67 -99.00-150.00  120
 22  \w     -2.00  52.00   0.50    7.50    --    3.67-120.00-172.17  108
 23  \w    -71.00 -36.00   0.50    7.50    --   -3.98 150.00-148.35   70
 24  \w    -70.00  -1.00   0.50    7.50    --   -3.98 -38.00  90.00  138
 25  \w    -20.00  32.00   0.50    7.50    --   -3.98 -99.00 -90.00  104
;
_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      0.0117967000
_diffrn_orient_matrix_UB_12      0.0017723000
_diffrn_orient_matrix_UB_13      0.0815319000
_diffrn_orient_matrix_UB_21      -0.0951406000
_diffrn_orient_matrix_UB_22      -0.0597830000
_diffrn_orient_matrix_UB_23      -0.0212124000
_diffrn_orient_matrix_UB_31      0.0161965000
_diffrn_orient_matrix_UB_32      -0.0713187000
_diffrn_orient_matrix_UB_33      -0.0066343000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22871
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.723
_diffrn_reflns_theta_min         3.420
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14393
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0766
_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^)+(0.0930P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             2438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm00040k2.cif
_cod_data_source_block           ms_29072019
_cod_depositor_comments
'Adding full bibliography for 1569069--1569071.cif.'
_cod_original_cell_volume        578.09(7)
_cod_database_code               1569071
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C16 H34 Br2 N4 O2 '
_diffrn_oxdiff_ac3_digest_frames
;
01a353dd1e6b445ba9390ae3b322e76ea7000264de2
;
_diffrn_oxdiff_ac3_digest_hkl
;
01e48a57c1f8a251daf7ae1b4e62572dafc34b
;
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C009(H00L,
 H00M), C00A(H00N,H00O), C00B(H00P,H00Q), C00C(H00R,H00S)
2.b Idealised Me refined as rotating group:
 C008(H00I,H00J,H00K)
;
_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 4.096
_oxdiff_exptl_absorpt_empirical_full_min 0.470