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_7127766
_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 F12 Li2 N4 P2 Si2, 0.7(C1 H2 Cl2)'
_chemical_formula_sum            'C48.7 H45.4 Cl1.4 F12 Li2 N4 P2 Si2'
_chemical_formula_weight         1096.32
_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             2020-07-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2020-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.57120(10)
_cell_length_b                   18.1992(2)
_cell_length_c                   27.2894(3)
_cell_measurement_reflns_used    12030
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      71.5640
_cell_measurement_theta_min      4.0830
_cell_volume                     5157.42(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.76a (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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.956
_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    -42.00  27.00   1.00   11.00    --   40.72 -19.00 120.00   69
  2  \w    -42.00  27.00   1.00   11.00    --   40.72 -19.00  60.00   69
  3  \w    -40.00  23.00   1.00   11.00    --   40.72 -19.00-180.00   63
  4  \w     85.00 175.00   1.00   50.00    --  104.78  61.00 -90.00   90
  5  \w     80.00 177.00   1.00   50.00    --  104.78  77.00-180.00   97
  6  \w     76.00 157.00   1.00   50.00    --  104.78  45.00-120.00   81
  7  \w     37.00  83.00   1.00   50.00    --  104.78-111.00 150.00   46
  8  \w     30.00  82.00   1.00   50.00    --  104.78-111.00 120.00   52
  9  \w     26.00  71.00   1.00   50.00    --  104.78 -95.00-180.00   45
 10  \w     40.00  68.00   1.00   50.00    --  104.78 -61.00-150.00   28
;
_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      0.1460156000
_diffrn_orient_matrix_UB_12      -0.0121477000
_diffrn_orient_matrix_UB_13      0.0047128000
_diffrn_orient_matrix_UB_21      0.0261742000
_diffrn_orient_matrix_UB_22      0.0696348000
_diffrn_orient_matrix_UB_23      0.0323793000
_diffrn_orient_matrix_UB_31      0.0012031000
_diffrn_orient_matrix_UB_32      -0.0465033000
_diffrn_orient_matrix_UB_33      0.0472714000
_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  0.0171
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18202
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.860
_diffrn_reflns_theta_min         4.096
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.76a (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    1.412
_exptl_crystal_description       plate
_exptl_crystal_F_000             2246
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/Pentane'
_exptl_crystal_size_max          0.634
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         9665
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+2.5924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8917
_reflns_number_total             9665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05682k2.cif
_cod_data_source_block           rx_318_mp_abs_ana
_cod_original_formula_sum        'C48.70 H45.40 Cl1.40 F12 Li2 N4 P2 Si2'
_cod_database_code               7127766
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48.6H45.1Cl1.1F12Li2N4P2Si2
_reflns_odcompleteness_completeness 98.28
_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. Restrained distances
 C23A-C22 \\sim C23B-C22 \\sim C24B-C23B \\sim C23A-C24A \\sim C24A-C19 \\sim
C24B-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C23B \\sim C23A \\sim C24B \\sim C24A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.7A
4. Others
 Sof(H22A)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(H22)=Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=FVAR(1)
 Fixed Sof: Cl2(0.7) Cl1(0.7) C49(0.7) H49A(0.7) H49B(0.7)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C36(H36A,H36B), C6(H6A,H6B), C30(H30A,H30B), C49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C14(H14), C2(H2), C38(H38), C48(H48),
 C42(H42), C8(H8), C9(H9), C20(H20), C3(H3), C25(H25), C15(H15), C34(H34),
 C46(H46), C18(H18), C31(H31), C28(H28), C39(H39), C44(H44), C26(H26), C41(H41),
  C21(H21), C47(H47), C40(H40), C27(H27), C16(H16), C32(H32), C33(H33),
 C22(H22), C22(H22A), C45(H45), C24A(H24A), C17(H17), C23A(H23A), C23B(H23B),
 C24B(H24B)
;
_shelx_res_checksum              46164
_shelx_hkl_checksum              33281
_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 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.715