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_7244550
_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 H10 N3, Cl'
_chemical_formula_sum            'C7 H10 Cl N3'
_chemical_formula_weight         171.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90.240(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3329(3)
_cell_length_b                   9.3234(4)
_cell_length_c                   12.2867(4)
_cell_measurement_reflns_used    1717
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      72.5560
_cell_measurement_theta_min      5.9420
_cell_volume                     840.00(6)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_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      4.00  93.00   1.00    1.00    --   42.36-125.00-180.00   89
  2  \w     36.00 102.00   1.00    1.00    --  105.13 -77.00-120.00   66
  3  \w     26.00  60.00   1.00    1.00    --   42.36-125.00  60.00   34
  4  \w     74.00 138.00   1.00    1.00    --  105.13 -77.00  60.00   64
  5  \w     92.00 176.00   1.00    1.00    --  105.13  61.00  60.00   84
  6  \w     19.00  45.00   1.00    1.00    --   42.23  57.00 -30.00   26
  7  \w     73.00  98.00   1.00    1.00    --   42.23-125.00-180.00   25
  8  \w     54.00 109.00   1.00    1.00    --   42.23  57.00 -30.00   55
  9  \w     71.00  97.00   1.00    1.00    --  105.13 -95.00-180.00   26
 10  \w     31.00 104.00   1.00    1.00    --  105.13 -30.00 -60.00   73
 11  \w     35.00  74.00   1.00    1.00    --  105.13 -45.00 -90.00   39
 12  \w     42.00  87.00   1.00    1.00    --  105.13 -30.00  90.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1852036000
_diffrn_orient_matrix_UB_12      0.0131060000
_diffrn_orient_matrix_UB_13      -0.0579043000
_diffrn_orient_matrix_UB_21      -0.0235513000
_diffrn_orient_matrix_UB_22      0.1525066000
_diffrn_orient_matrix_UB_23      0.0461467000
_diffrn_orient_matrix_UB_31      0.0963640000
_diffrn_orient_matrix_UB_32      0.0621793000
_diffrn_orient_matrix_UB_33      -0.1011768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3152
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.299
_diffrn_reflns_theta_min         5.958
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88200
_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    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0486P)^2^+0.2804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1374
_reflns_number_total             1629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp05169e5.cif
_cod_data_source_block           '[NC2C1C1im]Cl'
_cod_database_code               7244550
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H10 Cl N3'
_chemical_oxdiff_usercomment     SK62_ISOP
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.461
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              84522
_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 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.823