Effect of the cation structure on the properties of homobaric imidazolium ionic liquids
Koutsoukos, Spyridon; Philippi, Frederik; Rauber, Daniel; Pugh, David; Kay, Christopher William Michael; Welton, Tom; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D1CP05169E

data_7244549
_publ_section_title
;
 Effect of the cation structure on the properties of homobaric imidazolium
 ionic liquids
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP05169E
_journal_year                    2022
_chemical_formula_moiety         'C7 H9 N2, Br'
_chemical_formula_sum            'C7 H9 Br N2'
_chemical_formula_weight         201.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.339(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7092(3)
_cell_length_b                   15.2680(4)
_cell_length_c                   7.4616(3)
_cell_measurement_reflns_used    2943
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.5510
_cell_measurement_theta_min      2.6350
_cell_volume                     846.97(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_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     -2.00  82.00   1.00    1.22    --   14.27  57.00   0.00   84
  2  \w    -19.00  54.00   1.00    1.22    --   14.27-101.00 117.00   73
  3  \w    -25.00  53.00   1.00    1.22    --   14.27 -99.00 -30.00   78
  4  \w    -50.00  33.00   1.00    1.22    --   14.27 -37.00 -30.00   83
  5  \w    -40.00  51.00   1.00    1.22    --  -13.18  77.00-150.00   91
  6  \w    -80.00  14.00   1.00    1.22    --  -13.18 -77.00  90.00   94
  7  \w    -80.00   3.00   1.00    1.22    --  -13.18 -57.00-150.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148379000
_diffrn_orient_matrix_UB_12      -0.0435876000
_diffrn_orient_matrix_UB_13      0.0253341000
_diffrn_orient_matrix_UB_21      -0.0940122000
_diffrn_orient_matrix_UB_22      0.0078747000
_diffrn_orient_matrix_UB_23      -0.0239479000
_diffrn_orient_matrix_UB_31      -0.0066749000
_diffrn_orient_matrix_UB_32      -0.0140049000
_diffrn_orient_matrix_UB_33      -0.0922117000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5356
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.138
_diffrn_reflns_theta_min         2.668
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 757 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                1685
_reflns_number_total             1757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp05169e5.cif
_cod_data_source_block           '[HCC2C1im]Br'
_cod_original_cell_volume        846.96(5)
_cod_database_code               7244549
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H9 Br N2'
_chemical_oxdiff_usercomment     SK85_acetone
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.433
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
2.d :
 C7(H7)
;
_shelx_res_checksum              98727
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.834