#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:17:41 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261687 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/59/7705996.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7705996
loop_
_publ_author_name
'Valentine, Andrew J.'
'Geer, Ana M.'
'Taylor, Laurence J.'
'Teale, Andrew M.'
'Wood, Katherine E.'
'Williams, Huw E. L.'
'Lewis, William'
'Argent, Stephen P.'
'McMaster, Jonathan'
'Kays, Deborah L.'
_publ_section_title
;
 Structural and electronic studies of substituted m-terphenyl lithium
 complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              722
_journal_page_last               728
_journal_paper_doi               10.1039/d0dt03972a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C45.985 H40 F5.955 Li2'
_chemical_formula_sum            'C46 H40 F6 Li2'
_chemical_formula_weight         720.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.087(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2343(6)
_cell_length_b                   16.3983(5)
_cell_length_c                   15.5748(5)
_cell_measurement_reflns_used    10684
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4220
_cell_measurement_theta_min      4.0640
_cell_volume                     3755.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width tₑₓₚ ω θ κ φ Frames -------------------------------------------------------------------------- 1 ω -125.00 48.00 1.00 10.00 -- -38.50 0.00 30.00 173 2 ω 23.00 98.00 1.00 10.00 -- 43.38-125.00 30.00 75 3 ω 35.00 98.00 1.00 40.00 -- 106.13 -45.00 120.00 63 4 ω 25.00 109.00 1.00 40.00 -- 106.13 -95.00 -30.00 84 5 ω 31.00 91.00 1.00 40.00 -- 106.13 -30.00 60.00 60 6 ω 35.00 98.00 1.00 40.00 -- 106.13 -45.00 -30.00 63 7 ω 61.00 178.00 1.00 40.00 -- 106.13 15.00 30.00 117 8 ω 94.00 178.00 1.00 40.00 -- 106.13 125.00 30.00 84 9 ω 31.00 91.00 1.00 40.00 -- 106.13 -30.00-120.00 60 10 ω 35.00 121.00 1.00 40.00 -- 106.13-125.00 120.00 86 11 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00 0.00 105 12 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00-180.00 105 13 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00 -90.00 105 14 ω 75.00 178.00 1.00 40.00 -- 106.13 77.00 -90.00 103 15 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00 120.00 97 16 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00 60.00 97 17 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00-120.00 97 18 ω 75.00 178.00 1.00 40.00 -- 106.13 77.00 0.00 103 19 ω 61.00 178.00 1.00 40.00 -- 106.13 15.00-120.00 117'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0065825000
_diffrn_orient_matrix_UB_12      -0.0726642000
_diffrn_orient_matrix_UB_13      -0.0594672000
_diffrn_orient_matrix_UB_21      -0.0632344000
_diffrn_orient_matrix_UB_22      0.0444794000
_diffrn_orient_matrix_UB_23      -0.0913857000
_diffrn_orient_matrix_UB_31      0.0833063000
_diffrn_orient_matrix_UB_32      0.0395835000
_diffrn_orient_matrix_UB_33      -0.0063849000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.536
_diffrn_reflns_theta_min         4.038
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3818
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0369
_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/[σ²(Fo²)+(0.0488P)²+1.8878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3440
_reflns_number_total             3818
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           liajvf
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_database_code               7705996
_nottingham_internal_coll_name   LIAJVF
_nottingham_internal_coll_number 16599
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   24/10/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 28/10/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 30/11/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 30/11/16
_nottingham_internal_refinement_user pcxav1/pczspa
_nottingham_internal_self_archive_date 30/11/16
_nottingham_internal_self_validation_date 30/11/16
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 08/06/2020
_nottingham_internal_validation_user pczspa
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H20 F3 Li1'
_chemical_oxdiff_usercomment
'LIAJVF #16599 SN-1067 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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. Shared sites
{C23A, C23B, C23C}
3. Uiso/Uaniso restraints and constraints
F1B \\sim F2B \\sim F3B \\sim F1A \\sim F2A \\sim F3A \\sim F1C \\sim F3C \\sim
F2C: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2.5A
Uanis(C23A) = Uanis(C23B) = Uanis(C23C)
4. Rigid body (RIGU) restrains
 F1B, F2B, F3B, F1A, F2A, F3A, F1C, F3C, F2C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23B, F1B, F2B, F3B}
{C23B, F1B, F2B, F3B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23A, F1A, F2A, F3A}
{C23B, F1B, F2B, F3B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23C, F1C, F3C, F2C}
6. Others
 1*[Sof(C23B)+Sof(F1B)+Sof(F2B)+Sof(F3B)]+1*[Sof(C23A)+Sof(F1A)+Sof(F2A)+
 Sof(F3A)]+1*[Sof(C23C)+Sof(F1C)+Sof(F3C)+Sof(F2C)]=1 with esd of 0.002
 Sof(C23B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(1)
 Sof(C23A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(C23C)=Sof(F1C)=Sof(F3C)=Sof(F2C)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
7.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_olex2_date_sample_data_collection 2016-10-24
_olex2_date_sample_submission    2016-10-21
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id LIAJVF
_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 1.938
_oxdiff_exptl_absorpt_empirical_full_min 0.569
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.40179(6) 0.31740(6) 0.28085(7) 0.0221(2) Uani 1 1 d . . . . .
C2 C 0.38334(7) 0.26052(6) 0.33877(7) 0.0220(2) Uani 1 1 d . . . . .
C3 C 0.30736(7) 0.26535(6) 0.35855(7) 0.0243(2) Uani 1 1 d . . . . .
H3 H 0.297474 0.225238 0.397191 0.029 Uiso 1 1 calc R U . . .
C4 C 0.24633(7) 0.32910(6) 0.32143(7) 0.0243(2) Uani 1 1 d . . . . .
C5 C 0.26091(7) 0.38728(6) 0.26462(7) 0.0237(2) Uani 1 1 d . . . . .
H5 H 0.219520 0.431288 0.239461 0.028 Uiso 1 1 calc R U . . .
C6 C 0.33680(7) 0.38072(6) 0.24466(7) 0.0220(2) Uani 1 1 d . . . . .
C7 C 0.44541(7) 0.18855(6) 0.37774(7) 0.0231(2) Uani 1 1 d . . . . .
C8 C 0.51544(7) 0.19003(7) 0.47009(8) 0.0286(2) Uani 1 1 d . . . . .
C9 C 0.57034(8) 0.12150(8) 0.50378(8) 0.0360(3) Uani 1 1 d . . . . .
H9 H 0.618148 0.122241 0.565933 0.043 Uiso 1 1 calc R U . . .
C10 C 0.55676(9) 0.05254(8) 0.44877(9) 0.0383(3) Uani 1 1 d . . . . .
H10 H 0.595109 0.006421 0.472966 0.046 Uiso 1 1 calc R U . . .
C11 C 0.48721(8) 0.05066(7) 0.35830(9) 0.0365(3) Uani 1 1 d . . . . .
H11 H 0.477569 0.002845 0.320824 0.044 Uiso 1 1 calc R U . . .
C12 C 0.43106(7) 0.11830(7) 0.32153(8) 0.0292(2) Uani 1 1 d . . . . .
C13 C 0.52921(9) 0.26324(8) 0.53315(8) 0.0384(3) Uani 1 1 d . . . . .
H13A H 0.525540 0.313062 0.496950 0.058 Uiso 1 1 calc R U . . .
H13B H 0.589137 0.259998 0.586960 0.058 Uiso 1 1 calc R U . . .
H13C H 0.481896 0.264286 0.556548 0.058 Uiso 1 1 calc R U . . .
C14 C 0.35379(9) 0.11500(8) 0.22331(10) 0.0424(3) Uani 1 1 d . . . . .
H14A H 0.296985 0.130902 0.226550 0.064 Uiso 1 1 calc R U . . .
H14B H 0.347969 0.059386 0.198371 0.064 Uiso 1 1 calc R U . . .
H14C H 0.366369 0.152572 0.181405 0.064 Uiso 1 1 calc R U . . .
C15 C 0.34790(7) 0.44427(7) 0.18078(7) 0.0261(2) Uani 1 1 d . . . . .
C16 C 0.33130(8) 0.42359(9) 0.08710(8) 0.0370(3) Uani 1 1 d . . . . .
C17 C 0.33814(10) 0.48438(12) 0.02804(10) 0.0596(5) Uani 1 1 d . . . . .
H17 H 0.326215 0.471210 -0.035553 0.072 Uiso 1 1 calc R U . . .
C18 C 0.36166(11) 0.56273(12) 0.05945(13) 0.0686(5) Uani 1 1 d . . . . .
H18 H 0.365193 0.603272 0.017572 0.082 Uiso 1 1 calc R U . . .
C19 C 0.38012(10) 0.58264(9) 0.15148(13) 0.0566(4) Uani 1 1 d . . . . .
H19 H 0.397658 0.636810 0.173153 0.068 Uiso 1 1 calc R U . . .
C20 C 0.37345(8) 0.52426(7) 0.21376(9) 0.0361(3) Uani 1 1 d . . . . .
C21 C 0.30386(10) 0.33889(10) 0.04949(9) 0.0472(3) Uani 1 1 d . . . . .
H21A H 0.357084 0.302961 0.075061 0.071 Uiso 1 1 calc R U . . .
H21B H 0.279221 0.339666 -0.019862 0.071 Uiso 1 1 calc R U . . .
H21C H 0.257360 0.318698 0.068684 0.071 Uiso 1 1 calc R U . . .
C22 C 0.39330(10) 0.54755(8) 0.31404(12) 0.0497(4) Uani 1 1 d . . . . .
H22A H 0.336301 0.549712 0.321393 0.075 Uiso 1 1 calc R U . . .
H22B H 0.422663 0.601182 0.328343 0.075 Uiso 1 1 calc R U . . .
H22C H 0.433861 0.506923 0.357723 0.075 Uiso 1 1 calc R U . . .
Li1 Li 0.500000 0.24496(16) 0.250000 0.0325(6) Uani 1 2 d S T P . .
Li2 Li 0.500000 0.38720(16) 0.250000 0.0314(6) Uani 1 2 d S T P . .
C23B C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.717(12) 1 d D . P A 1
F1B F 0.09355(17) 0.2913(3) 0.2712(2) 0.0533(8) Uani 0.717(12) 1 d D U P A 1
F2B F 0.1324(3) 0.4081(2) 0.3391(4) 0.0526(9) Uani 0.717(12) 1 d D U P A 1
F3B F 0.1734(3) 0.2977(3) 0.4197(2) 0.0490(10) Uani 0.717(12) 1 d D U P A 1
C23A C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.052(2) 1 d D . P A 2
F1A F 0.1133(13) 0.2668(9) 0.3236(18) 0.057(4) Uiso 0.052(2) 1 d D U P A 2
F2A F 0.1010(13) 0.3899(12) 0.2849(14) 0.050(4) Uiso 0.052(2) 1 d D U P A 2
F3A F 0.1808(13) 0.3546(16) 0.4293(9) 0.062(4) Uiso 0.052(2) 1 d D U P A 2
C23C C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.224(12) 1 d D . P A 3
F1C F 0.0869(4) 0.3288(11) 0.2580(6) 0.057(2) Uani 0.224(12) 1 d D U P A 3
F3C F 0.1578(9) 0.2847(7) 0.4011(9) 0.045(2) Uani 0.224(12) 1 d D U P A 3
F2C F 0.1570(9) 0.4086(6) 0.3715(10) 0.0475(18) Uani 0.224(12) 1 d D U P A 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 5 -8 0.0403
-8 -5 8 0.0476
5 -9 -5 0.0364
6 -8 -5 0.0482
-4 9 5 0.0574
5 2 6 0.2316
-9 -5 1 0.1732
8 -4 -8 0.0351
-2 8 -5 0.1736
-1 4 -8 0.1954
1 11 0 0.0610
2 10 -3 0.0666
7 -6 -8 0.0293
-4 -9 6 0.0649
-4 10 3 0.0820
-6 8 6 0.0669
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 114.43(9) . . ?
C2 C1 Li1 98.76(8) . 2_655 ?
C2 C1 Li1 98.76(8) . . ?
C2 C1 Li2 149.39(8) . 2_655 ?
C2 C1 Li2 149.39(8) . . ?
C6 C1 Li1 142.78(8) . . ?
C6 C1 Li1 142.78(8) . 2_655 ?
C6 C1 Li2 91.06(8) . 2_655 ?
C6 C1 Li2 91.06(8) . . ?
Li1 C1 Li1 0.00(12) 2_655 . ?
Li2 C1 Li1 64.45(9) 2_655 . ?
Li2 C1 Li1 64.45(9) 2_655 2_655 ?
Li2 C1 Li1 64.45(9) . 2_655 ?
Li2 C1 Li1 64.45(9) . . ?
Li2 C1 Li2 0.00(12) 2_655 . ?
C1 C2 C7 119.22(9) . . ?
C3 C2 C1 123.33(9) . . ?
C3 C2 C7 117.38(9) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.56(9) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 119.94(9) . . ?
C3 C4 C23B 120.41(9) . . ?
C3 C4 C23A 120.41(9) . . ?
C3 C4 C23C 120.41(9) . . ?
C5 C4 C23B 119.58(9) . . ?
C5 C4 C23A 119.58(9) . . ?
C5 C4 C23C 119.58(9) . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.59(9) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C15 119.57(9) . . ?
C5 C6 C1 123.14(9) . . ?
C5 C6 C15 117.28(9) . . ?
C2 C7 Li1 78.70(7) . . ?
C2 C7 Li1 78.70(7) . 2_655 ?
C8 C7 C2 120.85(9) . . ?
C8 C7 Li1 112.18(7) . . ?
C8 C7 Li1 112.18(7) . 2_655 ?
C12 C7 C2 119.12(9) . . ?
C12 C7 C8 120.01(10) . . ?
C12 C7 Li1 80.74(8) . . ?
C12 C7 Li1 80.74(8) . 2_655 ?
Li1 C7 Li1 0.0 2_655 . ?
C7 C8 C13 120.85(10) . . ?
C9 C8 C7 118.88(11) . . ?
C9 C8 C13 120.24(10) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.33(11) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.85(11) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.64(11) . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C14 120.43(10) . . ?
C11 C12 C7 119.28(10) . . ?
C11 C12 C14 120.26(10) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li2 79.83(7) . 2_655 ?
C6 C15 Li2 79.83(7) . . ?
C16 C15 C6 119.65(10) . . ?
C16 C15 Li2 94.54(7) . . ?
C16 C15 Li2 94.54(7) . 2_655 ?
C20 C15 C6 120.30(10) . . ?
C20 C15 C16 120.04(11) . . ?
C20 C15 Li2 96.35(9) . . ?
C20 C15 Li2 96.35(9) . 2_655 ?
Li2 C15 Li2 0.00(11) 2_655 . ?
C15 C16 C21 121.49(11) . . ?
C17 C16 C15 118.57(14) . . ?
C17 C16 C21 119.90(13) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.58(15) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.00(13) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 120.92(15) . . ?
C20 C19 H19 119.5 . . ?
C15 C20 C22 121.10(11) . . ?
C19 C20 C15 118.86(13) . . ?
C19 C20 C22 120.04(13) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 Li1 C1 114.59(13) 2_655 . ?
C1 Li1 C2 140.03(11) . 2_655 ?
C1 Li1 C2 30.09(3) 2_655 2_655 ?
C1 Li1 C7 148.51(5) 2_655 . ?
C1 Li1 C7 61.48(3) . . ?
C1 Li1 C7 148.50(5) . 2_655 ?
C1 Li1 C7 61.48(3) 2_655 2_655 ?
C7 Li1 C2 155.88(7) . 2_655 ?
C7 Li1 C2 31.88(3) 2_655 2_655 ?
C7 Li1 C7 139.36(12) 2_655 . ?
Li1 Li1 C1 0(10) 2_655 . ?
Li1 Li1 C1 0(10) 2_655 2_655 ?
Li1 Li1 C2 0(10) 2_655 2_655 ?
Li1 Li1 C7 0(10) 2_655 2_655 ?
Li1 Li1 C7 0(10) 2_655 . ?
C1 Li2 C1 116.50(13) . 2_655 ?
C1 Li2 C6 32.75(3) 2_655 2_655 ?
C1 Li2 C6 142.98(11) . 2_655 ?
C1 Li2 C15 143.95(4) . 2_655 ?
C1 Li2 C15 143.95(4) 2_655 . ?
C1 Li2 C15 66.28(4) . . ?
C1 Li2 C15 66.28(4) 2_655 2_655 ?
C1 Li2 Li1 58.25(6) 2_655 2_655 ?
C1 Li2 Li1 58.25(6) . 2_655 ?
C15 Li2 C6 34.43(3) 2_655 2_655 ?
C15 Li2 C6 148.89(8) . 2_655 ?
C15 Li2 C15 134.59(12) 2_655 . ?
Li1 Li2 C6 87.67(6) 2_655 2_655 ?
Li1 Li2 C15 112.71(6) 2_655 . ?
Li1 Li2 C15 112.71(6) 2_655 2_655 ?
Li2 Li2 C1 0(10) 2_655 2_655 ?
Li2 Li2 C1 0(10) 2_655 . ?
Li2 Li2 C6 0(10) 2_655 2_655 ?
Li2 Li2 C15 0(6) 2_655 2_655 ?
Li2 Li2 C15 0(10) 2_655 . ?
Li2 Li2 Li1 0(10) 2_655 2_655 ?
F1B C23B C4 111.05(14) . . ?
F2B C23B C4 114.51(19) . . ?
F2B C23B F1B 107.01(17) . . ?
F2B C23B F3B 107.2(2) . . ?
F3B C23B C4 112.4(2) . . ?
F3B C23B F1B 103.96(19) . . ?
F1A C23A C4 117.6(9) . . ?
F1A C23A F2A 103.0(11) . . ?
F1A C23A F3A 103.9(12) . . ?
F2A C23A C4 114.5(9) . . ?
F2A C23A F3A 104.0(12) . . ?
F3A C23A C4 112.4(8) . . ?
F1C C23C C4 112.3(4) . . ?
F1C C23C F2C 103.1(5) . . ?
F3C C23C C4 117.1(6) . . ?
F3C C23C F1C 110.4(6) . . ?
F3C C23C F2C 103.8(7) . . ?
F2C C23C C4 108.8(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.4152(14) . ?
C1 C6 1.4160(14) . ?
C1 Li1 2.1985(17) 2_655 ?
C1 Li1 2.1985(17) . ?
C1 Li2 2.1754(17) . ?
C1 Li2 2.1754(17) 2_655 ?
C2 C3 1.3946(14) . ?
C2 C7 1.5025(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.3867(14) . ?
C4 C5 1.3882(15) . ?
C4 C23B 1.4920(14) . ?
C4 C23A 1.4920(14) . ?
C4 C23C 1.4920(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.3967(14) . ?
C6 C15 1.5035(14) . ?
C7 C8 1.4055(15) . ?
C7 C12 1.4053(15) . ?
C7 Li1 2.6635(13) 2_655 ?
C7 Li1 2.6635(13) . ?
C8 C9 1.3913(16) . ?
C8 C13 1.5065(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.3789(19) . ?
C10 H10 0.9500 . ?
C10 C11 1.3827(18) . ?
C11 H11 0.9500 . ?
C11 C12 1.3953(16) . ?
C12 C14 1.5130(16) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.4081(16) . ?
C15 C20 1.4055(16) . ?
C15 Li2 2.4245(14) 2_655 ?
C15 Li2 2.4245(14) . ?
C16 C17 1.3923(19) . ?
C16 C21 1.500(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.370(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.374(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.3994(19) . ?
C20 C22 1.504(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Li1 Li1 0.000000(3) 2_655 ?
Li2 Li2 0.000(5) 2_655 ?
C23B F1B 1.352(2) . ?
C23B F2B 1.321(3) . ?
C23B F3B 1.339(3) . ?
C23A F1A 1.315(12) . ?
C23A F2A 1.357(12) . ?
C23A F3A 1.365(12) . ?
C23C F1C 1.331(7) . ?
C23C F3C 1.291(10) . ?
C23C F2C 1.355(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.85(15) . . . . ?
C1 C2 C7 C8 97.11(12) . . . . ?
C1 C2 C7 C12 -84.71(12) . . . . ?
C1 C2 C7 Li1 -12.11(9) . . . . ?
C1 C2 C7 Li1 -12.11(9) . . . 2_655 ?
C1 C6 C15 C16 72.64(13) . . . . ?
C1 C6 C15 C20 -108.25(12) . . . . ?
C1 C6 C15 Li2 -16.80(9) . . . 2_655 ?
C1 C6 C15 Li2 -16.80(9) . . . . ?
C2 C1 C6 C5 0.41(14) . . . . ?
C2 C1 C6 C15 -178.98(9) . . . . ?
C2 C3 C4 C5 0.33(15) . . . . ?
C2 C3 C4 C23B 177.31(10) . . . . ?
C2 C3 C4 C23A 177.31(10) . . . . ?
C2 C3 C4 C23C 177.31(10) . . . . ?
C2 C7 C8 C9 178.97(10) . . . . ?
C2 C7 C8 C13 1.04(15) . . . . ?
C2 C7 C12 C11 -178.50(10) . . . . ?
C2 C7 C12 C14 -0.36(16) . . . . ?
C3 C2 C7 C8 -85.83(12) . . . . ?
C3 C2 C7 C12 92.35(12) . . . . ?
C3 C2 C7 Li1 164.95(9) . . . 2_655 ?
C3 C2 C7 Li1 164.95(9) . . . . ?
C3 C4 C5 C6 0.50(15) . . . . ?
C3 C4 C23B F1B -87.6(3) . . . . ?
C3 C4 C23B F2B 151.1(3) . . . . ?
C3 C4 C23B F3B 28.4(3) . . . . ?
C3 C4 C23A F1A -47.7(13) . . . . ?
C3 C4 C23A F2A -168.9(12) . . . . ?
C3 C4 C23A F3A 72.8(12) . . . . ?
C3 C4 C23C F1C -117.4(8) . . . . ?
C3 C4 C23C F3C 11.9(8) . . . . ?
C3 C4 C23C F2C 129.1(6) . . . . ?
C4 C5 C6 C1 -0.90(15) . . . . ?
C4 C5 C6 C15 178.51(9) . . . . ?
C5 C4 C23B F1B 89.4(3) . . . . ?
C5 C4 C23B F2B -31.9(3) . . . . ?
C5 C4 C23B F3B -154.6(3) . . . . ?
C5 C4 C23A F1A 129.2(13) . . . . ?
C5 C4 C23A F2A 8.1(12) . . . . ?
C5 C4 C23A F3A -110.2(12) . . . . ?
C5 C4 C23C F1C 59.5(9) . . . . ?
C5 C4 C23C F3C -171.2(8) . . . . ?
C5 C4 C23C F2C -54.0(7) . . . . ?
C5 C6 C15 C16 -106.78(11) . . . . ?
C5 C6 C15 C20 72.32(13) . . . . ?
C5 C6 C15 Li2 163.77(9) . . . 2_655 ?
C5 C6 C15 Li2 163.77(9) . . . . ?
C6 C1 C2 C3 0.47(14) . . . . ?
C6 C1 C2 C7 177.35(8) . . . . ?
C6 C15 C16 C17 177.21(11) . . . . ?
C6 C15 C16 C21 -0.85(17) . . . . ?
C6 C15 C20 C19 -177.81(11) . . . . ?
C6 C15 C20 C22 2.08(17) . . . . ?
C7 C2 C3 C4 -177.78(9) . . . . ?
C7 C8 C9 C10 -0.55(17) . . . . ?
C8 C7 C12 C11 -0.30(16) . . . . ?
C8 C7 C12 C14 177.84(11) . . . . ?
C8 C9 C10 C11 -0.21(19) . . . . ?
C9 C10 C11 C12 0.72(19) . . . . ?
C10 C11 C12 C7 -0.46(18) . . . . ?
C10 C11 C12 C14 -178.61(12) . . . . ?
C12 C7 C8 C9 0.80(15) . . . . ?
C12 C7 C8 C13 -177.12(10) . . . . ?
C13 C8 C9 C10 177.39(11) . . . . ?
C15 C16 C17 C18 0.9(2) . . . . ?
C16 C15 C20 C19 1.29(17) . . . . ?
C16 C15 C20 C22 -178.82(11) . . . . ?
C16 C17 C18 C19 0.7(3) . . . . ?
C17 C18 C19 C20 -1.4(3) . . . . ?
C18 C19 C20 C15 0.3(2) . . . . ?
C18 C19 C20 C22 -179.54(14) . . . . ?
C20 C15 C16 C17 -1.90(17) . . . . ?
C20 C15 C16 C21 -179.96(11) . . . . ?
C21 C16 C17 C18 178.99(15) . . . . ?
Li1 C1 C2 C3 -162.27(9) 2_655 . . . ?
Li1 C1 C2 C3 -162.27(9) . . . . ?
Li1 C1 C2 C7 14.60(10) 2_655 . . . ?
Li1 C1 C2 C7 14.60(10) . . . . ?
Li1 C1 C6 C5 151.41(12) 2_655 . . . ?
Li1 C1 C6 C5 151.41(12) . . . . ?
Li1 C1 C6 C15 -27.98(18) . . . . ?
Li1 C1 C6 C15 -27.98(18) 2_655 . . . ?
Li1 C7 C8 C9 -91.20(12) 2_655 . . . ?
Li1 C7 C8 C9 -91.20(12) . . . . ?
Li1 C7 C8 C13 90.88(12) . . . . ?
Li1 C7 C8 C13 90.88(12) 2_655 . . . ?
Li1 C7 C12 C11 110.04(10) . . . . ?
Li1 C7 C12 C11 110.04(10) 2_655 . . . ?
Li1 C7 C12 C14 -71.82(11) 2_655 . . . ?
Li1 C7 C12 C14 -71.82(11) . . . . ?
Li2 C1 C2 C3 144.34(15) 2_655 . . . ?
Li2 C1 C2 C3 144.34(15) . . . . ?
Li2 C1 C2 C7 -38.8(2) . . . . ?
Li2 C1 C2 C7 -38.8(2) 2_655 . . . ?
Li2 C1 C6 C5 -162.12(9) . . . . ?
Li2 C1 C6 C5 -162.12(9) 2_655 . . . ?
Li2 C1 C6 C15 18.49(10) . . . . ?
Li2 C1 C6 C15 18.49(10) 2_655 . . . ?
Li2 C15 C16 C17 -101.92(13) . . . . ?
Li2 C15 C16 C17 -101.92(13) 2_655 . . . ?
Li2 C15 C16 C21 80.02(13) . . . . ?
Li2 C15 C16 C21 80.02(13) 2_655 . . . ?
Li2 C15 C20 C19 100.29(11) . . . . ?
Li2 C15 C20 C19 100.29(11) 2_655 . . . ?
Li2 C15 C20 C22 -79.83(12) . . . . ?
Li2 C15 C20 C22 -79.83(12) 2_655 . . . ?
C23B C4 C5 C6 -176.50(9) . . . . ?
C23A C4 C5 C6 -176.50(9) . . . . ?
C23C C4 C5 C6 -176.50(9) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.9885 4.9926 -7.9909 0.1650 0.4472 0.9141
-7.9885 -4.9926 7.9909 -0.1650 -0.4472 -0.9141
4.9956 -8.9913 -4.9927 0.9831 -0.2596 0.0921
5.9941 -7.9926 -4.9925 0.9171 -0.2783 0.2148
-3.9970 8.9911 4.9931 -0.9766 0.1964 -0.0090
4.9927 1.9973 5.9963 -0.4688 -0.7748 0.4567
-8.9869 -4.9928 0.9966 0.2444 0.2551 -0.9527
7.9906 -3.9975 -7.9897 0.8182 0.0471 0.5584
-1.9990 7.9913 -4.9974 -0.2967 0.9385 0.1817
-0.9993 3.9953 -7.9939 0.1785 0.9714 0.1259
0.9961 10.9877 -0.0011 -0.7918 0.4258 0.5179
1.9951 9.9885 -2.9980 -0.5344 0.5921 0.5807
6.9924 -5.9951 -7.9898 0.9568 0.0213 0.3962
-3.9928 -8.9890 5.9945 0.2704 -0.6952 -0.7267
-3.9971 9.9899 2.9947 -0.9303 0.4234 0.0433
-5.9941 7.9927 5.9916 -0.9765 0.1870 -0.2212
