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_7127765
_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_formula_moiety         'C48 H44 Cl2 Li2 N4 Si2, 2(C2 H3 N)'
_chemical_formula_sum            'C52 H50 Cl2 Li2 N6 Si2'
_chemical_formula_weight         899.94
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2020-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.799(2)
_cell_angle_beta                 74.843(2)
_cell_angle_gamma                78.754(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9867(2)
_cell_length_b                   11.6858(3)
_cell_length_c                   12.4491(3)
_cell_measurement_reflns_used    13069
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.6780
_cell_measurement_theta_min      3.7150
_cell_volume                     1219.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (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    '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 0.998
_diffrn_measured_fraction_theta_max 0.916
_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    -77.00   2.00   1.00   40.00    --  -18.40 127.00 152.03   79
  2  \w    -94.00   8.00   1.00   40.00    --  -18.40 -38.00-120.00  102
  3  \w    -97.00  15.00   1.00   40.00    --  -18.40 -77.00  30.00  112
  4  \w    -52.00  60.00   1.00   40.00    --  -18.40  77.00  30.00  112
  5  \w    -92.00  11.00   1.00   40.00    --  -18.40 -57.00 150.00  103
  6  \w    -54.00  50.00   1.00   40.00    --   19.96 -57.00 -90.00  104
  7  \w     -4.00  62.00   1.00   40.00    --   19.96 -99.00 150.00   66
  8  \w    -65.00 -16.00   1.00   40.00    --  -18.40 107.00 -56.00   49
  9  \w    -96.00 -16.00   1.00   40.00    --  -18.40 155.00  24.65   80
;
_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      0.0318170000
_diffrn_orient_matrix_UB_12      -0.0598082000
_diffrn_orient_matrix_UB_13      0.0160680000
_diffrn_orient_matrix_UB_21      -0.0094250000
_diffrn_orient_matrix_UB_22      0.0101277000
_diffrn_orient_matrix_UB_23      0.0557595000
_diffrn_orient_matrix_UB_31      -0.0757343000
_diffrn_orient_matrix_UB_32      -0.0162296000
_diffrn_orient_matrix_UB_33      0.0148347000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28897
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.457
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Tetrahydrofuran'
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         15510
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0372P)^2^+0.1453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                13734
_reflns_number_total             15510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05682k2.cif
_cod_data_source_block           rx17dcm_ap_non_abs
_cod_database_code               7127765
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H50Cl2Li2N6Si2
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_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:
 C12(H12A,H12B), C6(H6A,H6B), C36(H36A,H36B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C28(H28), C8(H8), C48(H48), C9(H9), C44(H44), C10(H10), C25(H25),
 C34(H34), C22(H22), C42(H42), C18(H18), C17(H17), C24(H24), C20(H20), C16(H16),
  C31(H31), C1(H1), C23(H23), C15(H15), C2(H2), C27(H27), C21(H21), C4(H4),
 C47(H47), C40(H40), C45(H45), C38(H38), C14(H14), C41(H41), C39(H39), C26(H26),
  C46(H46), C32(H32), C33(H33), C3(H3)
2.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              53343
_shelx_hkl_checksum              15113
_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 0.827