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_7127763
_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         'C26 H26 N2 Si'
_chemical_formula_sum            'C26 H26 N2 Si'
_chemical_formula_weight         394.57
_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             2020-06-24
_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                100.776(2)
_cell_angle_beta                 93.428(2)
_cell_angle_gamma                109.092(2)
_cell_formula_units_Z            4
_cell_length_a                   10.2134(2)
_cell_length_b                   14.0734(3)
_cell_length_c                   16.2616(3)
_cell_measurement_reflns_used    10888
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.3130
_cell_measurement_theta_min      3.8940
_cell_volume                     2151.38(8)
_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  (Sheldrick, 2015)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.963
_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    -98.00 -22.00   1.00    2.00    --  -39.78 125.00-180.00   76
  2  \w      1.00  87.00   1.00    2.00    --   39.78-125.00  90.00   86
  3  \w    -43.00  27.00   1.00    2.00    --   39.78 -19.00-120.00   70
  4  \w    -43.00  27.00   1.00    2.00    --   39.78 -19.00-180.00   70
  5  \w    -43.00  27.00   1.00    2.00    --   39.78 -19.00 120.00   70
  6  \w     25.00  84.00   1.00   12.00    --  104.85-111.00 -30.00   59
  7  \w     80.00 178.00   1.00   12.00    --  104.85  77.00 150.00   98
  8  \w     76.00 178.00   1.00   12.00    --  104.85  45.00-150.00  102
  9  \w     71.00 178.00   1.00   12.00    --  104.85  30.00 -90.00  107
 10  \w     17.00 143.00   1.00   12.00    --  104.85 -88.00 -14.16  126
 11  \w     17.00 143.00   1.00   12.00    --  104.85 -88.00  62.17  126
 12  \w     76.00 178.00   1.00   12.00    --  104.85  45.00 120.00  102
 13  \w     17.00 143.00   1.00   12.00    --  104.85 -88.00 146.09  126
 14  \w     29.00  71.00   1.00   12.00    --  104.85 -61.00-120.00   42
 15  \w     18.00 143.00   1.00   12.00    --  104.85 -87.00-133.63  125
 16  \w      6.00  97.00   1.00    2.00    --   39.78  73.00-160.13   91
;
_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      0.0196191000
_diffrn_orient_matrix_UB_12      0.0709602000
_diffrn_orient_matrix_UB_13      -0.0632536000
_diffrn_orient_matrix_UB_21      -0.0315275000
_diffrn_orient_matrix_UB_22      -0.0941030000
_diffrn_orient_matrix_UB_23      -0.0736346000
_diffrn_orient_matrix_UB_31      -0.1566478000
_diffrn_orient_matrix_UB_32      -0.0142605000
_diffrn_orient_matrix_UB_33      -0.0061264000
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17359
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.507
_diffrn_reflns_theta_min         3.406
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.756
_exptl_crystal_size_mid          0.616
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0519P)^2^+0.6022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7390
_reflns_number_total             8084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05682k2.cif
_cod_data_source_block           ph2silut2_ap_abs_gaus
_cod_depositor_comments
;

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C26 H26 N2 Si)'
_cod_original_formula_sum        'C52 H52 N4 Si2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     789.15
_cod_database_code               7127763
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H52N4Si2
_reflns_odcompleteness_completeness 98.62
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1(H1A,H1B), C27(H27A,H27B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C20(H20), C22(H22), C16(H16), C12(H12), C10(H10), C29(H29),
 C52(H52), C42(H42), C46(H46), C11(H11), C36(H36), C18(H18), C48(H48), C19(H19),
  C51(H51), C49(H49), C17(H17), C31(H31), C43(H43), C50(H50), C30(H30),
 C38(H38), C23(H23), C3(H3), C25(H25), C37(H37), C5(H5), C44(H44), C24(H24),
 C45(H45), C4(H4)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              323
_shelx_hkl_checksum              10040
_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 1.588
_oxdiff_exptl_absorpt_empirical_full_min 0.728