Complexation behaviour of LiCl and LiPF<sub>6</sub>- model studies in the solid-state and in solution using a bidentate picolyl-based ligand.
Espinosa-Jalapa, Noel Angel; Berg, Nele; Seidl, Michael; Shenderovich, Ilya G.; Gschwind, Ruth M.; Bauer, Jonathan O.; Chemical communications (Cambridge, England) 56 (2020) 13335–13338; doi:10.1039/d0cc05682k

data_7127764
_publ_section_title
;
 Complexation behaviour of LiCl and LiPF<sub>6</sub>- model studies in the
 solid-state and in solution using a bidentate picolyl-based ligand.
;
_journal_issue                   87
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13335
_journal_page_last               13338
_journal_paper_doi               10.1039/d0cc05682k
_journal_volume                  56
_journal_year                    2020
_chemical_compound_source        Pentane
_chemical_formula_moiety         'C24 H22 N2 Si'
_chemical_formula_sum            'C24 H22 N2 Si'
_chemical_formula_weight         366.52
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2020-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.034(2)
_cell_angle_beta                 64.483(2)
_cell_angle_gamma                87.683(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8911(3)
_cell_length_b                   10.3035(2)
_cell_length_c                   10.8066(2)
_cell_measurement_reflns_used    13118
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.6810
_cell_measurement_theta_min      4.3240
_cell_volume                     984.09(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_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    -99.00 -18.00   1.00   12.50    --  -40.72 125.00-150.00   81
  2  \w     -3.00  92.00   1.00   12.50    --   40.72-125.00 150.00   95
  3  \w      6.00 122.00   1.00   12.50    --   40.72  77.00-120.00  116
  4  \w     12.00 118.00   1.00   12.50    --   40.72  38.00  30.00  106
  5  \w     11.00 129.00   1.00   12.50    --   46.00  79.00  99.82  118
  6  \w     11.00 127.00   1.00   12.50    --   46.00  76.00  12.42  116
  7  \w     15.00 132.00   1.00   12.50    --   50.00  78.00 121.35  117
  8  \w     23.00 140.00   1.00   12.50    --   58.00  78.00-145.48  117
  9  \w     23.00 140.00   1.00   12.50    --   58.00  77.00  45.13  117
 10  \w     27.00 144.00   1.00   12.50    --   62.00  77.00-116.62  117
 11  \w     31.00 148.00   1.00   12.50    --   66.00  78.00 154.18  117
 12  \w     31.00 149.00   1.00   12.50    --   66.00  79.00 -88.29  118
 13  \w     31.00 149.00   1.00   12.50    --   66.00  79.00 -25.04  118
 14  \w     35.00 153.00   1.00   12.50    --   70.00  79.00 111.53  118
 15  \w     35.00 152.00   1.00   12.50    --   70.00  78.00  77.62  117
 16  \w     45.00  75.00   1.00   50.00    --   78.00  69.00  42.48   30
 17  \w     51.00  78.00   1.00   50.00    --   82.00  53.00-127.33   27
 18  \w     72.00  99.00   1.00   50.00    --  104.78  77.00 -30.00   27
 19  \w    111.00 147.00   1.00   50.00    --  104.78  77.00 120.00   36
 20  \w     32.00  99.00   1.00   50.00    --  104.78 -88.00  89.50   67
 21  \w     71.00  98.00   1.00   50.00    --  104.78  77.00 120.00   27
 22  \w    106.00 172.00   1.00   50.00    --  104.78  77.00 -30.00   66
 23  \w     80.00 122.00   1.00   50.00    --  104.78 -90.00  44.45   42
 24  \w     70.00 158.00   1.00   50.00    --  104.78  77.00-150.00   88
 25  \w     76.00 103.00   1.00   50.00    --  104.78  61.00  60.00   27
 26  \w     27.00  54.00   1.00   50.00    --  104.78 -90.00  44.45   27
 27  \w     73.00 100.00   1.00   50.00    --  104.78  61.00   0.00   27
 28  \w     91.00 141.00   1.00   50.00    --  104.78 -91.00-138.51   50
 29  \w     28.00  55.00   1.00   50.00    --  104.78 -91.00-138.51   27
 30  \w     73.00 173.00   1.00   50.00    --  104.78  77.00  90.00  100
 31  \w     36.00 143.00   1.00   50.00    --  104.78 -90.00 151.69  107
 32  \w     76.00 103.00   1.00   50.00    --  104.78  61.00 120.00   27
 33  \w     70.00 167.00   1.00   50.00    --  104.78  77.00 -90.00   97
 34  \w     85.00 136.00   1.00   50.00    --  104.78 -86.00 -66.75   51
 35  \w     75.00 112.00   1.00   50.00    --  104.78  61.00-180.00   37
 36  \w     19.00  64.00   1.00   50.00    --  104.78 -86.00 -66.75   45
 37  \w     70.00 174.00   1.00   50.00    --  104.78  77.00  30.00  104
 38  \w    134.00 161.00   1.00   50.00    --  104.78  79.00-112.00   27
 39  \w    120.00 156.00   1.00   50.00    --  104.78  77.00-120.00   36
 40  \w     70.00  96.00   1.00   50.00    --  104.78  77.00-120.00   26
 41  \w     70.00 128.00   1.00   50.00    --  104.78  79.00-112.00   58
 42  \w     76.00 136.00   1.00   50.00    --  104.78  61.00 150.00   60
 43  \w     70.00 175.00   1.00   50.00    --  104.78  77.00 150.00  105
 44  \w     71.00 178.00   1.00   50.00    --  104.78  77.00 -60.00  107
 45  \w     72.00 178.00   1.00   50.00    --  104.78  77.00-180.00  106
 46  \w     71.00 178.00   1.00   50.00    --  104.78  77.00   0.00  107
 47  \w     29.00  69.00   1.00   50.00    --  104.78 -61.00 -30.00   40
 48  \w    117.00 143.00   1.00   50.00    --  104.78 -88.00  89.50   26
 49  \w     72.00 141.00   1.00   50.00    --  104.78  77.00  60.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0667717000
_diffrn_orient_matrix_UB_12      -0.1276317000
_diffrn_orient_matrix_UB_13      0.0983585000
_diffrn_orient_matrix_UB_21      -0.1086163000
_diffrn_orient_matrix_UB_22      -0.0122001000
_diffrn_orient_matrix_UB_23      -0.0659494000
_diffrn_orient_matrix_UB_31      0.1163785000
_diffrn_orient_matrix_UB_32      -0.0797841000
_diffrn_orient_matrix_UB_33      -0.1067170000
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19425
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.377
_diffrn_reflns_theta_min         4.334
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       plate
_exptl_crystal_F_000             388
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0356P)^2^+0.4052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3510
_reflns_number_total             3796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05682k2.cif
_cod_data_source_block           rx_253_ap_abs_ana
_cod_database_code               7127764
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H22N2Si
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.696
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C24(H24), C12(H12), C20(H20), C14(H14), C10(H10), C11(H11),
 C18(H18), C4(H4), C6(H6), C22(H22), C23(H23), C21(H21), C5(H5), C15(H15),
 C17(H17), C16(H16)
;
_shelx_res_checksum              37006
_shelx_hkl_checksum              49506
_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 2.970
_oxdiff_exptl_absorpt_empirical_full_min 0.686