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_1569070
_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         '2(Br), C19 H29 N2'
_chemical_formula_sum            'C19 H29 Br2 N2'
_chemical_formula_weight         445.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6157(17)
_cell_length_b                   13.7323(16)
_cell_length_c                   10.4556(10)
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9410
_cell_measurement_theta_min      3.5810
_cell_volume                     2242.1(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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     19.00  45.00   0.50   35.00    --    5.13-115.00 -19.00   52
  2  \w     13.00  59.00   0.50   35.00    --    5.13  57.00 -60.00   92
  3  \w      3.00  64.00   0.50   35.00    --    5.13  38.00 -90.00  122
  4  \w     -4.00  39.00   0.50   35.00    --    5.13 -99.00-180.00   86
  5  \w    -10.00  16.00   0.50   35.00    --   -5.59 -99.00 -30.00   52
  6  \w    -13.00  30.00   0.50   35.00    --   -5.59 -99.00  90.00   86
;
_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      0.0405158000
_diffrn_orient_matrix_UB_12      -0.0162012000
_diffrn_orient_matrix_UB_13      0.0220738000
_diffrn_orient_matrix_UB_21      0.0191381000
_diffrn_orient_matrix_UB_22      0.0430310000
_diffrn_orient_matrix_UB_23      -0.0242939000
_diffrn_orient_matrix_UB_31      -0.0072335000
_diffrn_orient_matrix_UB_32      0.0236143000
_diffrn_orient_matrix_UB_33      0.0593710000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.095
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49676
_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    1.319
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.541
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2472
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1246P)^2^+4.0133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1500
_reflns_number_total             2472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm00040k2.cif
_cod_data_source_block           ms_01072019
_cod_depositor_comments
'Adding full bibliography for 1569069--1569071.cif.'
_cod_database_code               1569070
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C32 H32 N32 O32 Br32 '
_diffrn_oxdiff_ac3_digest_frames
;
01ab1de49cd8466e84613d6f904d3c4161000253487
;
_diffrn_oxdiff_ac3_digest_hkl
;
017cd296d1079b12fe77ffdfa5899aa60a4a53
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C004(H00D,H00E), C005(H00F,H00G), C006(H00H,H00I)
3.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00D(H00J), C5(H5), C3(H3)
3.c Idealised Me refined as rotating group:
 C003(H00A,H00B,H00C)
;
_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 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.712