Low-melting Multicharge Ionic Liquids with [Ln(NO3)5]2− (Ln = Ho–Lu): Structural, Electrostatic, Thermochemical, and Fluorescence Properties
Wang, Shuang-Long; Yuan, Wen-Li; Zhao, Ying; Cheng, Kun-Lun; Tao, Guo-Hong; He, Ling; Dalton Transactions  (2023) –; doi:10.1039/D3DT00937H

data_7713171
_publ_section_title
;
 Low-melting Multicharge Ionic Liquids with [Ln(NO3)5]2&#x2212; (Ln =
 Ho--Lu): Structural, Electrostatic, Thermochemical, and Fluorescence
 Properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00937H
_journal_year                    2023
_chemical_formula_moiety         'Er N5 O15, 2(C6 H11 N2)'
_chemical_formula_sum            'C12 H22 Er N9 O15'
_chemical_formula_weight         699.64
_chemical_name_systematic        '[MC1mim]2[Er(NO3)5]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-05-21 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.496(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6110(2)
_cell_length_b                   9.6805(2)
_cell_length_c                   15.5021(3)
_cell_measurement_reflns_used    8544
_cell_measurement_temperature    276(2)
_cell_measurement_theta_max      72.6380
_cell_measurement_theta_min      3.8660
_cell_volume                     2491.93(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      276(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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     31.00  97.00   1.00    1.00    --   36.54-137.00  53.00   66
  2  \w    -31.00  53.00   1.00    1.00    --   36.54 -57.00  30.00   84
  3  \w    -33.00  55.00   1.00    1.00    --   36.54 -38.00-180.00   88
  4  \w     23.00  90.00   1.00    1.00    --   36.54-125.00 -90.00   67
  5  \w    -33.00  55.00   1.00    1.00    --   36.54 -38.00  60.00   88
  6  \w    -31.00  63.00   1.00    1.00    --   36.54 -77.00 -90.00   94
  7  \w     87.00 178.00   1.00    1.73    --  108.00  30.00-150.00   91
  8  \w     38.00  91.00   1.00    1.73    --  108.00 -30.00 -60.00   53
  9  \w     38.00  91.00   1.00    1.73    --  108.00 -30.00   0.00   53
 10  \w     38.00  91.00   1.00    1.73    --  108.00 -30.00  90.00   53
 11  \w    100.00 178.00   1.00    1.73    --  108.00 111.00  30.00   78
 12  \w    100.00 178.00   1.00    1.73    --  108.00 111.00 120.00   78
 13  \w     41.00 126.00   1.00    1.73    --  108.00 -61.00 -60.00   85
 14  \w     40.00  98.00   1.00    1.73    --  108.00 -45.00-120.00   58
 15  \w     57.00 150.00   1.00    1.73    --  108.00 178.00 -30.00   93
 16  \w     10.00 104.00   1.00    1.00    --   36.54  77.00-120.00   94
 17  \w     20.00 104.00   1.00    1.00    --   36.54  57.00  90.00   84
 18  \w     20.00 104.00   1.00    1.00    --   36.54  57.00-180.00   84
 19  \w     10.00 104.00   1.00    1.00    --   36.54  77.00 -30.00   94
 20  \w     70.00 178.00   1.00    1.73    --  108.00  15.00  90.00  108
 21  \w     70.00 178.00   1.00    1.73    --  108.00  15.00   0.00  108
 22  \w     91.00 176.00   1.00    1.73    --  108.00  45.00 -90.00   85
 23  \w     87.00 178.00   1.00    1.73    --  108.00  30.00 150.00   91
 24  \w     41.00 126.00   1.00    1.73    --  108.00 -61.00  90.00   85
 25  \w     38.00  67.00   1.00    1.73    --  108.00-111.00 -30.00   29
 26  \w     39.00 109.00   1.00    1.73    --  108.00 -94.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0075203000
_diffrn_orient_matrix_UB_12      -0.1295665000
_diffrn_orient_matrix_UB_13      -0.0574187000
_diffrn_orient_matrix_UB_21      -0.0924622000
_diffrn_orient_matrix_UB_22      0.0091030000
_diffrn_orient_matrix_UB_23      0.0033163000
_diffrn_orient_matrix_UB_31      -0.0014271000
_diffrn_orient_matrix_UB_32      0.0918882000
_diffrn_orient_matrix_UB_33      -0.0811094000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12039
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.721
_diffrn_reflns_theta_min         5.289
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.048
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.865
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.00292(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0696P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2342
_reflns_number_total             2462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00937h2.cif
_cod_data_source_block           tgh-m3er-2-rt
_cod_database_code               7713171
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C6H11Er0.5N4.5O7.5
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.192
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              50809
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.763