# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_dwl_v_otolyl_4_li_thf4
_database_code_depnum_ccdc_archive 'CCDC 2334908'
loop_
_audit_author_name
_audit_author_address
'Daniel Laorenza'
;Harvard University
United States of America
;
_audit_update_record             
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'tetrakis(tetrahydrofuran)lithium tetrakis(o-tolyl)vanadate'
_chemical_formula_moiety         
'C28 H28 V, 0.5(C16 H32 Li O4), 0.5(C16 H31 Li O4)'
_chemical_formula_sum            'C44 H59.50 Li O4 V'
_chemical_formula_weight         710.29
_chemical_melting_point          ?
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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.487(4)
_cell_length_b                   16.971(4)
_cell_length_c                   22.100(6)
_cell_angle_alpha                70.281(19)
_cell_angle_beta                 86.57(2)
_cell_angle_gamma                84.97(2)
_cell_volume                     4038(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    811
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.68
_cell_measurement_theta_min      7.41
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.349
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1526
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 10 4 0.3897
1 -3 6 0.2597
5 -16 -30 0.1395
5 4 -30 0.1326
1 30 17 0.2607
-1 10 30 0.1397
-1 -17 30 0.1971
-30 7 7 0.4972
-7 -13 30 0.1934
0 -30 -13 0.2140
1 8 -10 0.1424

_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66732
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.665
_diffrn_reflns_theta_min         2.773
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
 4589 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10141
_reflns_number_total             14814
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14814
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.019
_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)+(0.1183P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1799
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H60,H60A,H60B} of C60, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  {H28A,H28B,H28C} of C28, {H42A,H42B,H42C} of C42, {H35A,H35B,H35C} of C35,
  {H21A,H21B,H21C} of C21, {H56A,H56B,H56C} of C56, {H49A,H49B,H49C} of C49,
  {H7A,H7B,H7C} of C7, {H14A,H14B,H14C} of C14
2. Others
 Fixed Sof: H57A(0.5) H57B(0.5) H57C(0.5) H57D(0.5) H60(0.5) H60A(0.5)
 H60B(0.5) C59(0.5) H59(0.5) C58(0.5) H58A(0.5) H58B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C57(H57C,H57D), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
  C72(H72A,H72B), C73(H73A,H73B), C58(H58A,H58B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54), C60(H60), C59(H59)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
V1 V 0.33902(4) 0.77517(3) -0.02655(2) 0.02624(14) Uani 1 1 d . . . . .
C1 C 0.2932(3) 0.90294(17) -0.07553(13) 0.0294(6) Uani 1 1 d . . . . .
C2 C 0.3724(3) 0.95143(18) -0.12159(13) 0.0328(7) Uani 1 1 d . . . . .
H2 H 0.445989 0.925390 -0.128903 0.039 Uiso 1 1 calc R U . . .
C3 C 0.3473(3) 1.03532(18) -0.15657(14) 0.0382(7) Uani 1 1 d . . . . .
H3 H 0.402650 1.065755 -0.187342 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2408(3) 1.07429(18) -0.14622(14) 0.0401(8) Uani 1 1 d . . . . .
H4 H 0.221994 1.131492 -0.170497 0.048 Uiso 1 1 calc R U . . .
C5 C 0.1621(3) 1.03008(18) -0.10071(14) 0.0375(7) Uani 1 1 d . . . . .
H5 H 0.089753 1.057505 -0.093272 0.045 Uiso 1 1 calc R U . . .
C6 C 0.1871(3) 0.94503(17) -0.06506(13) 0.0313(6) Uani 1 1 d . . . . .
C7 C 0.0984(3) 0.89990(19) -0.01522(15) 0.0433(8) Uani 1 1 d . . . . .
H7A H 0.075297 0.851625 -0.025328 0.065 Uiso 1 1 calc R U . . .
H7B H 0.029505 0.938282 -0.015230 0.065 Uiso 1 1 calc R U . . .
H7C H 0.132776 0.880444 0.027314 0.065 Uiso 1 1 calc R U . . .
C8 C 0.4990(3) 0.73465(17) -0.06092(13) 0.0291(6) Uani 1 1 d . . . . .
C9 C 0.5876(3) 0.69373(18) -0.01767(15) 0.0391(8) Uani 1 1 d . . . . .
H9 H 0.573640 0.685317 0.026802 0.047 Uiso 1 1 calc R U . . .
C10 C 0.6956(3) 0.6650(2) -0.03800(17) 0.0478(9) Uani 1 1 d . . . . .
H10 H 0.753466 0.637129 -0.007538 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7178(3) 0.6772(2) -0.10206(17) 0.0444(8) Uani 1 1 d . . . . .
H11 H 0.791535 0.658698 -0.116215 0.053 Uiso 1 1 calc R U . . .
C12 C 0.6323(3) 0.71650(19) -0.14599(15) 0.0378(7) Uani 1 1 d . . . . .
H12 H 0.647793 0.724839 -0.190347 0.045 Uiso 1 1 calc R U . . .
C13 C 0.5240(3) 0.74392(17) -0.12593(13) 0.0302(6) Uani 1 1 d . . . . .
C14 C 0.4302(3) 0.7807(2) -0.17499(14) 0.0383(7) Uani 1 1 d . . . . .
H14A H 0.364925 0.806592 -0.156018 0.057 Uiso 1 1 calc R U . . .
H14B H 0.402280 0.736058 -0.187997 0.057 Uiso 1 1 calc R U . . .
H14C H 0.462724 0.823282 -0.212726 0.057 Uiso 1 1 calc R U . . .
C15 C 0.3444(3) 0.76268(17) 0.07034(13) 0.0318(7) Uani 1 1 d . . . . .
C16 C 0.2632(3) 0.71380(19) 0.11477(14) 0.0402(8) Uani 1 1 d . . . . .
H16 H 0.209302 0.686066 0.099479 0.048 Uiso 1 1 calc R U . . .
C17 C 0.2587(3) 0.7046(2) 0.17932(14) 0.0472(9) Uani 1 1 d . . . . .
H17 H 0.202852 0.671057 0.207655 0.057 Uiso 1 1 calc R U . . .
C18 C 0.3356(3) 0.7443(2) 0.20203(15) 0.0505(9) Uani 1 1 d . . . . .
H18 H 0.333627 0.738525 0.246357 0.061 Uiso 1 1 calc R U . . .
C19 C 0.4162(3) 0.7929(2) 0.16025(15) 0.0478(9) Uani 1 1 d . . . . .
H19 H 0.469709 0.819946 0.176367 0.057 Uiso 1 1 calc R U . . .
C20 C 0.4207(3) 0.80295(19) 0.09485(14) 0.0382(7) Uani 1 1 d . . . . .
C21 C 0.5091(3) 0.8582(2) 0.05090(16) 0.0487(9) Uani 1 1 d . . . . .
H21A H 0.542791 0.891059 0.073578 0.073 Uiso 1 1 calc R U . . .
H21B H 0.470477 0.896311 0.012479 0.073 Uiso 1 1 calc R U . . .
H21C H 0.571433 0.823101 0.038195 0.073 Uiso 1 1 calc R U . . .
C22 C 0.2168(3) 0.70105(17) -0.04333(13) 0.0304(6) Uani 1 1 d . . . . .
C23 C 0.1286(3) 0.74038(19) -0.08788(15) 0.0373(7) Uani 1 1 d . . . . .
H23 H 0.125408 0.799641 -0.107591 0.045 Uiso 1 1 calc R U . . .
C24 C 0.0461(3) 0.6961(2) -0.10415(16) 0.0440(8) Uani 1 1 d . . . . .
H24 H -0.010457 0.724786 -0.135178 0.053 Uiso 1 1 calc R U . . .
C25 C 0.0473(3) 0.6100(2) -0.07474(17) 0.0472(8) Uani 1 1 d . . . . .
H25 H -0.009637 0.579064 -0.084497 0.057 Uiso 1 1 calc R U . . .
C26 C 0.1327(3) 0.5694(2) -0.03088(16) 0.0437(8) Uani 1 1 d . . . . .
H26 H 0.133722 0.510297 -0.010800 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2167(3) 0.61287(18) -0.01549(14) 0.0348(7) Uani 1 1 d . . . . .
C28 C 0.3103(3) 0.56440(19) 0.03075(16) 0.0465(9) Uani 1 1 d . . . . .
H28A H 0.387172 0.582630 0.012432 0.070 Uiso 1 1 calc R U . . .
H28B H 0.307889 0.504282 0.038150 0.070 Uiso 1 1 calc R U . . .
H28C H 0.296466 0.574893 0.071655 0.070 Uiso 1 1 calc R U . . .
V2 V 0.37445(4) 0.27816(3) 0.47861(2) 0.02574(14) Uani 1 1 d . . . . .
C29 C 0.3191(2) 0.40271(17) 0.42778(13) 0.0277(6) Uani 1 1 d . . . . .
C30 C 0.3759(3) 0.44700(17) 0.37003(13) 0.0306(6) Uani 1 1 d . . . . .
H30 H 0.444909 0.421192 0.356821 0.037 Uiso 1 1 calc R U . . .
C31 C 0.3367(3) 0.52684(19) 0.33098(14) 0.0373(7) Uani 1 1 d . . . . .
H31 H 0.377740 0.554455 0.291989 0.045 Uiso 1 1 calc R U . . .
C32 C 0.2370(3) 0.56530(19) 0.34985(14) 0.0408(8) Uani 1 1 d . . . . .
H32 H 0.207958 0.619356 0.323378 0.049 Uiso 1 1 calc R U . . .
C33 C 0.1798(3) 0.52514(19) 0.40707(14) 0.0379(7) Uani 1 1 d . . . . .
H33 H 0.112290 0.552597 0.420142 0.045 Uiso 1 1 calc R U . . .
C34 C 0.2185(3) 0.44543(18) 0.44610(13) 0.0317(7) Uani 1 1 d . . . . .
C35 C 0.1552(3) 0.4042(2) 0.50947(15) 0.0452(9) Uani 1 1 d . . . . .
H35A H 0.134396 0.348578 0.511540 0.068 Uiso 1 1 calc R U . . .
H35B H 0.083957 0.438880 0.513015 0.068 Uiso 1 1 calc R U . . .
H35C H 0.206168 0.398541 0.544935 0.068 Uiso 1 1 calc R U . . .
C36 C 0.2462(2) 0.20187(18) 0.47114(13) 0.0296(6) Uani 1 1 d . . . . .
C37 C 0.1393(2) 0.23999(19) 0.44367(14) 0.0339(7) Uani 1 1 d . . . . .
H37 H 0.130022 0.299483 0.426318 0.041 Uiso 1 1 calc R U . . .
C38 C 0.0475(3) 0.1942(2) 0.44102(15) 0.0400(8) Uani 1 1 d . . . . .
H38 H -0.023830 0.222035 0.422635 0.048 Uiso 1 1 calc R U . . .
C39 C 0.0598(3) 0.1078(2) 0.46516(15) 0.0409(8) Uani 1 1 d . . . . .
H39 H -0.003276 0.075890 0.463687 0.049 Uiso 1 1 calc R U . . .
C40 C 0.1645(3) 0.06757(19) 0.49163(15) 0.0388(7) Uani 1 1 d . . . . .
H40 H 0.173051 0.008004 0.507960 0.047 Uiso 1 1 calc R U . . .
C41 C 0.2565(3) 0.11351(18) 0.49442(14) 0.0338(7) Uani 1 1 d . . . . .
C42 C 0.3693(3) 0.06754(19) 0.52307(17) 0.0467(9) Uani 1 1 d . . . . .
H42A H 0.432397 0.080462 0.490161 0.070 Uiso 1 1 calc R U . . .
H42B H 0.360490 0.006973 0.538720 0.070 Uiso 1 1 calc R U . . .
H42C H 0.388162 0.085320 0.558950 0.070 Uiso 1 1 calc R U . . .
C43 C 0.3868(3) 0.26578(17) 0.57548(13) 0.0314(6) Uani 1 1 d . . . . .
C44 C 0.3166(3) 0.20874(19) 0.62135(13) 0.0357(7) Uani 1 1 d . . . . .
H44 H 0.271290 0.174169 0.607473 0.043 Uiso 1 1 calc R U . . .
C45 C 0.3112(3) 0.2013(2) 0.68556(14) 0.0460(9) Uani 1 1 d . . . . .
H45 H 0.263322 0.161989 0.715186 0.055 Uiso 1 1 calc R U . . .
C46 C 0.3758(3) 0.2514(2) 0.70640(15) 0.0489(9) Uani 1 1 d . . . . .
H46 H 0.372122 0.247206 0.750417 0.059 Uiso 1 1 calc R U . . .
C47 C 0.4459(3) 0.3076(2) 0.66286(15) 0.0458(8) Uani 1 1 d . . . . .
H47 H 0.490628 0.341850 0.677381 0.055 Uiso 1 1 calc R U . . .
C48 C 0.4521(3) 0.31509(18) 0.59811(14) 0.0349(7) Uani 1 1 d . . . . .
C49 C 0.5301(3) 0.3779(2) 0.55242(15) 0.0461(8) Uani 1 1 d . . . . .
H49A H 0.548497 0.418856 0.572166 0.069 Uiso 1 1 calc R U . . .
H49B H 0.489708 0.406957 0.512256 0.069 Uiso 1 1 calc R U . . .
H49C H 0.602691 0.348441 0.543255 0.069 Uiso 1 1 calc R U . . .
C50 C 0.5323(2) 0.24025(17) 0.44042(13) 0.0293(6) Uani 1 1 d . . . . .
C51 C 0.6285(3) 0.21039(18) 0.48089(14) 0.0355(7) Uani 1 1 d . . . . .
H51 H 0.620162 0.210470 0.523897 0.043 Uiso 1 1 calc R U . . .
C52 C 0.7345(3) 0.18096(19) 0.46036(15) 0.0400(8) Uani 1 1 d . . . . .
H52 H 0.797456 0.161492 0.488912 0.048 Uiso 1 1 calc R U . . .
C53 C 0.7479(3) 0.1802(2) 0.39809(16) 0.0409(8) Uani 1 1 d . . . . .
H53 H 0.820548 0.160605 0.383431 0.049 Uiso 1 1 calc R U . . .
C54 C 0.6558(3) 0.2078(2) 0.35729(16) 0.0417(8) Uani 1 1 d . . . . .
H54 H 0.665343 0.206966 0.314500 0.050 Uiso 1 1 calc R U . . .
C55 C 0.5489(3) 0.23689(19) 0.37789(14) 0.0332(7) Uani 1 1 d . . . . .
C56 C 0.4497(3) 0.2651(2) 0.33161(15) 0.0406(8) Uani 1 1 d . . . . .
H56A H 0.469113 0.315932 0.296389 0.061 Uiso 1 1 calc R U . . .
H56B H 0.378052 0.276941 0.354323 0.061 Uiso 1 1 calc R U . . .
H56C H 0.437731 0.220553 0.314120 0.061 Uiso 1 1 calc R U . . .
O1 O -0.0860(2) 0.61002(14) 0.16724(11) 0.0502(6) Uani 1 1 d . . . . .
O2 O -0.2868(2) 0.49633(15) 0.18645(12) 0.0503(6) Uani 1 1 d . . . . .
O3 O -0.1890(2) 0.49973(16) 0.30872(11) 0.0510(6) Uani 1 1 d . . . . .
O4 O -0.0114(2) 0.42793(16) 0.22821(12) 0.0534(6) Uani 1 1 d . . . . .
C57 C -0.1171(5) 0.6930(3) 0.1671(3) 0.0879(16) Uani 1 1 d . . . . .
H57A H -0.050041 0.718094 0.177872 0.105 Uiso 0.5 1 calc R U P A 1
H57B H -0.183433 0.694438 0.197471 0.105 Uiso 0.5 1 calc R U P A 1
H57C H -0.203188 0.703603 0.167536 0.105 Uiso 0.5 1 calc R U P B 2
H57D H -0.087259 0.700661 0.205669 0.105 Uiso 0.5 1 calc R U P B 2
C60 C -0.0713(4) 0.7031(2) 0.0599(2) 0.0686(12) Uani 1 1 d . . . . .
H60 H -0.033899 0.729194 0.019374 0.082 Uiso 0.5 1 calc R U P C 1
H60A H -0.147849 0.714337 0.039070 0.082 Uiso 0.5 1 calc R U P D 2
H60B H -0.008236 0.719855 0.026543 0.082 Uiso 0.5 1 calc R U P D 2
C61 C -0.0523(4) 0.6140(2) 0.10128(16) 0.0542(10) Uani 1 1 d . . . . .
H61A H -0.100584 0.578223 0.087247 0.065 Uiso 1 1 calc R U . . .
H61B H 0.030949 0.594146 0.098741 0.065 Uiso 1 1 calc R U . . .
C62 C -0.3794(4) 0.5641(2) 0.1766(2) 0.0678(12) Uani 1 1 d . . . . .
H62A H -0.360230 0.613090 0.138764 0.081 Uiso 1 1 calc R U . . .
H62B H -0.390220 0.582119 0.214914 0.081 Uiso 1 1 calc R U . . .
C63 C -0.4862(3) 0.5278(3) 0.1660(2) 0.0632(11) Uani 1 1 d . . . . .
H63A H -0.540826 0.571459 0.138081 0.076 Uiso 1 1 calc R U . . .
H63B H -0.527136 0.498697 0.207216 0.076 Uiso 1 1 calc R U . . .
C64 C -0.4369(3) 0.4668(2) 0.13333(19) 0.0563(10) Uani 1 1 d . . . . .
H64A H -0.416216 0.496020 0.087532 0.068 Uiso 1 1 calc R U . . .
H64B H -0.492537 0.424150 0.136353 0.068 Uiso 1 1 calc R U . . .
C65 C -0.3297(3) 0.4281(2) 0.17153(18) 0.0492(9) Uani 1 1 d . . . . .
H65A H -0.349984 0.382084 0.211282 0.059 Uiso 1 1 calc R U . . .
H65B H -0.270820 0.405715 0.145804 0.059 Uiso 1 1 calc R U . . .
C66 C -0.2904(4) 0.4631(3) 0.3420(2) 0.0804(14) Uani 1 1 d . . . . .
H66A H -0.305789 0.413793 0.330090 0.096 Uiso 1 1 calc R U . . .
H66B H -0.359091 0.504131 0.331156 0.096 Uiso 1 1 calc R U . . .
C67 C -0.2685(6) 0.4373(4) 0.4111(2) 0.103(2) Uani 1 1 d . . . . .
H67A H -0.300808 0.382713 0.434921 0.123 Uiso 1 1 calc R U . . .
H67B H -0.302630 0.479947 0.429777 0.123 Uiso 1 1 calc R U . . .
C68 C -0.1394(6) 0.4306(3) 0.4121(2) 0.107(2) Uani 1 1 d . . . . .
H68A H -0.106442 0.375752 0.409742 0.128 Uiso 1 1 calc R U . . .
H68B H -0.111826 0.438137 0.451271 0.128 Uiso 1 1 calc R U . . .
C69 C -0.1076(4) 0.5009(3) 0.3531(2) 0.0804(14) Uani 1 1 d . . . . .
H69A H -0.115017 0.555144 0.361129 0.097 Uiso 1 1 calc R U . . .
H69B H -0.026674 0.491163 0.337693 0.097 Uiso 1 1 calc R U . . .
C70 C -0.0146(4) 0.3382(2) 0.26320(18) 0.0656(12) Uani 1 1 d . . . . .
H70A H -0.060550 0.311386 0.239971 0.079 Uiso 1 1 calc R U . . .
H70B H -0.050334 0.328362 0.306772 0.079 Uiso 1 1 calc R U . . .
C71 C 0.1108(4) 0.3032(3) 0.26720(18) 0.0680(12) Uani 1 1 d . . . . .
H71A H 0.133408 0.282266 0.231123 0.082 Uiso 1 1 calc R U . . .
H71B H 0.124497 0.257118 0.308369 0.082 Uiso 1 1 calc R U . . .
C72 C 0.1776(4) 0.3788(3) 0.2628(2) 0.0710(13) Uani 1 1 d . . . . .
H72A H 0.180186 0.385938 0.305338 0.085 Uiso 1 1 calc R U . . .
H72B H 0.258478 0.373205 0.245820 0.085 Uiso 1 1 calc R U . . .
C73 C 0.1090(4) 0.4489(3) 0.2179(2) 0.0669(12) Uani 1 1 d . . . . .
H73A H 0.117970 0.501670 0.226472 0.080 Uiso 1 1 calc R U . . .
H73B H 0.135333 0.456363 0.172988 0.080 Uiso 1 1 calc R U . . .
Li1 Li -0.1437(5) 0.5068(4) 0.2227(3) 0.0451(14) Uani 1 1 d . . . . .
C59 C -0.1544(9) 0.7410(4) 0.0916(4) 0.054(2) Uani 0.5 1 d . . P E 1
H59 H -0.215576 0.782805 0.074679 0.065 Uiso 0.5 1 calc R U P E 1
C58 C -0.0679(10) 0.7482(5) 0.1117(6) 0.084(4) Uani 0.5 1 d . . P E 2
H58A H 0.013477 0.757373 0.118669 0.100 Uiso 0.5 1 calc R U P E 2
H58B H -0.114102 0.802995 0.098122 0.100 Uiso 0.5 1 calc R U P E 2
O5 O 0.8639(2) 0.15904(15) 0.69325(11) 0.0541(7) Uani 1 1 d . . . . .
O6 O 0.7103(2) 0.0266(2) 0.68612(14) 0.0659(8) Uani 1 1 d . . . . .
O7 O 0.7935(2) -0.00192(14) 0.82142(11) 0.0481(6) Uani 1 1 d . . . . .
O8 O 0.9771(2) -0.02042(15) 0.72174(10) 0.0479(6) Uani 1 1 d . . . . .
C74 C 0.7052(5) -0.0379(4) 0.6574(3) 0.1002(19) Uani 1 1 d . . . . .
H74A H 0.761689 -0.029742 0.620533 0.120 Uiso 1 1 calc R U . . .
H74B H 0.721968 -0.094415 0.689235 0.120 Uiso 1 1 calc R U . . .
C75 C 0.5874(5) -0.0275(3) 0.6366(3) 0.113(2) Uani 1 1 d . . . . .
H75A H 0.560732 -0.081562 0.637070 0.135 Uiso 1 1 calc R U . . .
H75B H 0.580927 0.013536 0.592583 0.135 Uiso 1 1 calc R U . . .
C76 C 0.5148(4) 0.0051(3) 0.6852(2) 0.0844(16) Uani 1 1 d . . . . .
H76A H 0.439744 0.034347 0.667293 0.101 Uiso 1 1 calc R U . . .
H76B H 0.499207 -0.040909 0.725887 0.101 Uiso 1 1 calc R U . . .
C77 C 0.5932(3) 0.0630(3) 0.6944(2) 0.0715(13) Uani 1 1 d . . . . .
H77A H 0.579925 0.119657 0.662138 0.086 Uiso 1 1 calc R U . . .
H77B H 0.581483 0.067323 0.737981 0.086 Uiso 1 1 calc R U . . .
C78 C 0.7465(4) -0.0837(2) 0.84457(18) 0.0585(10) Uani 1 1 d . . . . .
H78A H 0.793520 -0.123468 0.827257 0.070 Uiso 1 1 calc R U . . .
H78B H 0.664572 -0.079762 0.831645 0.070 Uiso 1 1 calc R U . . .
C79 C 0.7530(4) -0.1113(2) 0.91585(19) 0.0661(12) Uani 1 1 d . . . . .
H79A H 0.830141 -0.140122 0.930433 0.079 Uiso 1 1 calc R U . . .
H79B H 0.690783 -0.149022 0.937270 0.079 Uiso 1 1 calc R U . . .
C80 C 0.7349(4) -0.0292(3) 0.92833(19) 0.0719(13) Uani 1 1 d . . . . .
H80A H 0.764806 -0.034086 0.970627 0.086 Uiso 1 1 calc R U . . .
H80B H 0.651251 -0.009053 0.926584 0.086 Uiso 1 1 calc R U . . .
C81 C 0.8059(3) 0.0281(2) 0.87361(16) 0.0518(9) Uani 1 1 d . . . . .
H81A H 0.774522 0.087240 0.862885 0.062 Uiso 1 1 calc R U . . .
H81B H 0.888920 0.023747 0.884788 0.062 Uiso 1 1 calc R U . . .
C82 C 1.0440(3) -0.0068(3) 0.66247(17) 0.0587(11) Uani 1 1 d . . . . .
H82A H 1.022396 0.049255 0.631217 0.070 Uiso 1 1 calc R U . . .
H82B H 1.031080 -0.050068 0.643179 0.070 Uiso 1 1 calc R U . . .
C83 C 1.1682(3) -0.0131(2) 0.68091(18) 0.0560(10) Uani 1 1 d . . . . .
H83A H 1.221644 -0.032220 0.651035 0.067 Uiso 1 1 calc R U . . .
H83B H 1.191287 0.041610 0.681315 0.067 Uiso 1 1 calc R U . . .
C84 C 1.1690(3) -0.0762(3) 0.74650(19) 0.0651(11) Uani 1 1 d . . . . .
H84A H 1.185329 -0.133651 0.744825 0.078 Uiso 1 1 calc R U . . .
H84B H 1.228224 -0.065195 0.772855 0.078 Uiso 1 1 calc R U . . .
C85 C 1.0501(4) -0.0652(3) 0.77251(19) 0.0802(15) Uani 1 1 d . . . . .
H85A H 1.020094 -0.120670 0.795804 0.096 Uiso 1 1 calc R U . . .
H85B H 1.051459 -0.034113 0.803155 0.096 Uiso 1 1 calc R U . . .
C86 C 0.8278(5) 0.2116(3) 0.63070(19) 0.0779(14) Uani 1 1 d . . . . .
H86A H 0.767556 0.255516 0.634045 0.093 Uiso 1 1 calc R U . . .
H86B H 0.795131 0.178067 0.607672 0.093 Uiso 1 1 calc R U . . .
C88 C 0.9343(6) 0.2499(3) 0.5966(2) 0.102(2) Uani 1 1 d . . . . .
H88A H 0.914722 0.303933 0.562282 0.123 Uiso 1 1 calc R U . . .
H88B H 0.981068 0.211801 0.577501 0.123 Uiso 1 1 calc R U . . .
C89 C 0.9972(4) 0.2626(3) 0.6491(2) 0.0809(16) Uani 1 1 d . . . . .
H89A H 0.973884 0.318328 0.652836 0.097 Uiso 1 1 calc R U . . .
H89B H 1.082823 0.258029 0.641188 0.097 Uiso 1 1 calc R U . . .
C90 C 0.9612(4) 0.1936(2) 0.7089(2) 0.0654(11) Uani 1 1 d . . . . .
H90A H 1.026318 0.149931 0.722969 0.079 Uiso 1 1 calc R U . . .
H90B H 0.939505 0.216300 0.744124 0.079 Uiso 1 1 calc R U . . .
Li2 Li 0.8337(5) 0.0424(4) 0.7324(3) 0.0486(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
V1 C1 2.106(3) . ?
V1 C8 2.096(3) . ?
V1 C15 2.084(3) . ?
V1 C22 2.092(3) . ?
C1 C2 1.413(4) . ?
C1 C6 1.405(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.375(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(4) . ?
C6 C7 1.507(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.406(4) . ?
C8 C13 1.406(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.398(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(4) . ?
C13 C14 1.514(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.414(4) . ?
C15 C20 1.392(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.380(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.369(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.380(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(4) . ?
C20 C21 1.513(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.414(4) . ?
C22 C27 1.413(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.384(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(4) . ?
C27 C28 1.512(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
V2 C29 2.093(3) . ?
V2 C36 2.093(3) . ?
V2 C43 2.092(3) . ?
V2 C50 2.096(3) . ?
C29 C30 1.400(4) . ?
C29 C34 1.421(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.391(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.381(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.376(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.387(4) . ?
C34 C35 1.512(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.407(4) . ?
C36 C41 1.408(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.379(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.378(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.388(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.383(4) . ?
C41 C42 1.509(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.412(4) . ?
C43 C48 1.396(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.380(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.378(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.381(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.391(4) . ?
C48 C49 1.514(4) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.411(4) . ?
C50 C55 1.403(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.385(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.380(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.376(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.392(4) . ?
C55 C56 1.512(4) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
O1 C57 1.420(4) . ?
O1 C61 1.466(4) . ?
O1 Li1 1.915(6) . ?
O2 C62 1.465(4) . ?
O2 C65 1.439(4) . ?
O2 Li1 1.918(6) . ?
O3 C66 1.414(4) . ?
O3 C69 1.401(5) . ?
O3 Li1 1.907(6) . ?
O4 C70 1.460(4) . ?
O4 C73 1.444(5) . ?
O4 Li1 1.916(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 H57C 0.9900 . ?
C57 H57D 0.9900 . ?
C57 C59 1.654(9) . ?
C57 C58 1.390(9) . ?
C60 H60 0.9500 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.484(5) . ?
C60 C59 1.391(9) . ?
C60 C58 1.583(12) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.486(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.505(5) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C64 C65 1.506(5) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.471(7) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.479(8) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.493(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.504(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.524(6) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 C73 1.468(5) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C59 H59 0.9500 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
O5 C86 1.431(4) . ?
O5 C90 1.418(5) . ?
O5 Li2 1.928(7) . ?
O6 C74 1.446(5) . ?
O6 C77 1.459(4) . ?
O6 Li2 1.884(7) . ?
O7 C78 1.448(4) . ?
O7 C81 1.428(4) . ?
O7 Li2 1.899(6) . ?
O8 C82 1.438(4) . ?
O8 C85 1.402(4) . ?
O8 Li2 1.928(6) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.432(6) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C76 1.538(8) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C76 C77 1.461(6) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C78 C79 1.489(5) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C79 C80 1.503(6) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C81 1.517(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.492(5) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.483(5) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.470(5) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C86 C88 1.479(7) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.487(7) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 C90 1.504(5) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?

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
C8 V1 C1 112.01(11) . . ?
C15 V1 C1 106.08(11) . . ?
C15 V1 C8 111.69(12) . . ?
C15 V1 C22 112.37(12) . . ?
C22 V1 C1 110.00(11) . . ?
C22 V1 C8 104.81(11) . . ?
C2 C1 V1 119.6(2) . . ?
C6 C1 V1 124.0(2) . . ?
C6 C1 C2 116.4(2) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 C1 122.8(3) . . ?
C3 C2 H2 118.6 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(3) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 120.6(2) . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 C7 118.9(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 V1 119.8(2) . . ?
C9 C8 C13 116.4(3) . . ?
C13 C8 V1 123.8(2) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 C8 122.1(3) . . ?
C10 C9 H9 119.0 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.7(3) . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C14 119.9(3) . . ?
C12 C13 C8 121.2(3) . . ?
C12 C13 C14 118.8(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 V1 119.4(2) . . ?
C20 C15 V1 124.1(2) . . ?
C20 C15 C16 116.4(3) . . ?
C15 C16 H16 118.5 . . ?
C17 C16 C15 123.0(3) . . ?
C17 C16 H16 118.5 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 H18 120.1 . . ?
C17 C18 C19 119.7(3) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.4(3) . . ?
C20 C19 H19 119.3 . . ?
C15 C20 C19 120.3(3) . . ?
C15 C20 C21 120.4(3) . . ?
C19 C20 C21 119.3(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 V1 118.6(2) . . ?
C27 C22 V1 125.5(2) . . ?
C27 C22 C23 115.8(3) . . ?
C22 C23 H23 118.5 . . ?
C24 C23 C22 122.9(3) . . ?
C24 C23 H23 118.5 . . ?
C23 C24 H24 120.3 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.3 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.1(3) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 119.1 . . ?
C25 C26 C27 121.8(3) . . ?
C27 C26 H26 119.1 . . ?
C22 C27 C28 120.0(3) . . ?
C26 C27 C22 120.9(3) . . ?
C26 C27 C28 119.1(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 V2 C50 111.95(11) . . ?
C36 V2 C29 107.77(11) . . ?
C36 V2 C50 108.07(11) . . ?
C43 V2 C29 108.45(11) . . ?
C43 V2 C36 108.56(12) . . ?
C43 V2 C50 111.91(11) . . ?
C30 C29 V2 120.7(2) . . ?
C30 C29 C34 115.8(2) . . ?
C34 C29 V2 123.3(2) . . ?
C29 C30 H30 118.3 . . ?
C31 C30 C29 123.4(3) . . ?
C31 C30 H30 118.3 . . ?
C30 C31 H31 120.6 . . ?
C32 C31 C30 118.9(3) . . ?
C32 C31 H31 120.6 . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.8(3) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 119.3 . . ?
C32 C33 C34 121.5(3) . . ?
C34 C33 H33 119.3 . . ?
C29 C34 C35 119.5(2) . . ?
C33 C34 C29 120.6(3) . . ?
C33 C34 C35 119.9(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 V2 118.9(2) . . ?
C37 C36 C41 116.4(3) . . ?
C41 C36 V2 124.6(2) . . ?
C36 C37 H37 118.8 . . ?
C38 C37 C36 122.4(3) . . ?
C38 C37 H37 118.8 . . ?
C37 C38 H38 120.2 . . ?
C39 C38 C37 119.7(3) . . ?
C39 C38 H38 120.2 . . ?
C38 C39 H39 120.1 . . ?
C38 C39 C40 119.8(3) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 H40 119.7 . . ?
C41 C40 C39 120.5(3) . . ?
C41 C40 H40 119.7 . . ?
C36 C41 C42 119.9(3) . . ?
C40 C41 C36 121.1(3) . . ?
C40 C41 C42 119.0(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 V2 118.2(2) . . ?
C48 C43 V2 124.8(2) . . ?
C48 C43 C44 116.7(3) . . ?
C43 C44 H44 118.8 . . ?
C45 C44 C43 122.5(3) . . ?
C45 C44 H44 118.8 . . ?
C44 C45 H45 120.3 . . ?
C46 C45 C44 119.5(3) . . ?
C46 C45 H45 120.3 . . ?
C45 C46 H46 120.2 . . ?
C45 C46 C47 119.6(3) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 H47 119.4 . . ?
C46 C47 C48 121.2(3) . . ?
C48 C47 H47 119.4 . . ?
C43 C48 C49 120.4(3) . . ?
C47 C48 C43 120.5(3) . . ?
C47 C48 C49 119.0(3) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 V2 118.8(2) . . ?
C55 C50 V2 125.0(2) . . ?
C55 C50 C51 116.1(3) . . ?
C50 C51 H51 118.7 . . ?
C52 C51 C50 122.6(3) . . ?
C52 C51 H51 118.7 . . ?
C51 C52 H52 120.3 . . ?
C53 C52 C51 119.5(3) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 120.1 . . ?
C54 C53 C52 119.8(3) . . ?
C54 C53 H53 120.1 . . ?
C53 C54 H54 119.6 . . ?
C53 C54 C55 120.9(3) . . ?
C55 C54 H54 119.6 . . ?
C50 C55 C56 120.0(3) . . ?
C54 C55 C50 121.1(3) . . ?
C54 C55 C56 118.9(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C57 O1 C61 108.3(3) . . ?
C57 O1 Li1 128.8(3) . . ?
C61 O1 Li1 116.4(3) . . ?
C62 O2 Li1 118.5(3) . . ?
C65 O2 C62 109.2(3) . . ?
C65 O2 Li1 131.9(3) . . ?
C66 O3 Li1 124.7(3) . . ?
C69 O3 C66 109.5(3) . . ?
C69 O3 Li1 121.9(3) . . ?
C70 O4 Li1 123.4(3) . . ?
C73 O4 C70 108.8(3) . . ?
C73 O4 Li1 125.0(3) . . ?
O1 C57 H57A 111.5 . . ?
O1 C57 H57B 111.5 . . ?
O1 C57 H57C 110.1 . . ?
O1 C57 H57D 110.1 . . ?
O1 C57 C59 101.5(4) . . ?
H57A C57 H57B 109.3 . . ?
H57C C57 H57D 108.4 . . ?
C59 C57 H57A 111.5 . . ?
C59 C57 H57B 111.5 . . ?
C58 C57 O1 107.9(5) . . ?
C58 C57 H57C 110.1 . . ?
C58 C57 H57D 110.1 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60 126.5 . . ?
C61 C60 H60A 111.7 . . ?
C61 C60 H60B 111.7 . . ?
C61 C60 C58 100.4(4) . . ?
C59 C60 H60 126.5 . . ?
C59 C60 C61 107.0(4) . . ?
C58 C60 H60A 111.7 . . ?
C58 C60 H60B 111.7 . . ?
O1 C61 C60 107.0(3) . . ?
O1 C61 H61A 110.3 . . ?
O1 C61 H61B 110.3 . . ?
C60 C61 H61A 110.3 . . ?
C60 C61 H61B 110.3 . . ?
H61A C61 H61B 108.6 . . ?
O2 C62 H62A 110.7 . . ?
O2 C62 H62B 110.7 . . ?
O2 C62 C63 105.0(3) . . ?
H62A C62 H62B 108.8 . . ?
C63 C62 H62A 110.7 . . ?
C63 C62 H62B 110.7 . . ?
C62 C63 H63A 111.3 . . ?
C62 C63 H63B 111.3 . . ?
C62 C63 C64 102.1(3) . . ?
H63A C63 H63B 109.2 . . ?
C64 C63 H63A 111.3 . . ?
C64 C63 H63B 111.3 . . ?
C63 C64 H64A 111.4 . . ?
C63 C64 H64B 111.4 . . ?
C63 C64 C65 101.8(3) . . ?
H64A C64 H64B 109.3 . . ?
C65 C64 H64A 111.4 . . ?
C65 C64 H64B 111.4 . . ?
O2 C65 C64 104.1(3) . . ?
O2 C65 H65A 110.9 . . ?
O2 C65 H65B 110.9 . . ?
C64 C65 H65A 110.9 . . ?
C64 C65 H65B 110.9 . . ?
H65A C65 H65B 109.0 . . ?
O3 C66 H66A 110.3 . . ?
O3 C66 H66B 110.3 . . ?
O3 C66 C67 107.1(4) . . ?
H66A C66 H66B 108.6 . . ?
C67 C66 H66A 110.3 . . ?
C67 C66 H66B 110.3 . . ?
C66 C67 H67A 111.3 . . ?
C66 C67 H67B 111.3 . . ?
C66 C67 C68 102.5(4) . . ?
H67A C67 H67B 109.2 . . ?
C68 C67 H67A 111.3 . . ?
C68 C67 H67B 111.3 . . ?
C67 C68 H68A 111.3 . . ?
C67 C68 H68B 111.3 . . ?
C67 C68 C69 102.4(4) . . ?
H68A C68 H68B 109.2 . . ?
C69 C68 H68A 111.3 . . ?
C69 C68 H68B 111.3 . . ?
O3 C69 C68 103.3(4) . . ?
O3 C69 H69A 111.1 . . ?
O3 C69 H69B 111.1 . . ?
C68 C69 H69A 111.1 . . ?
C68 C69 H69B 111.1 . . ?
H69A C69 H69B 109.1 . . ?
O4 C70 H70A 110.6 . . ?
O4 C70 H70B 110.6 . . ?
O4 C70 C71 105.7(3) . . ?
H70A C70 H70B 108.7 . . ?
C71 C70 H70A 110.6 . . ?
C71 C70 H70B 110.6 . . ?
C70 C71 H71A 111.2 . . ?
C70 C71 H71B 111.2 . . ?
C70 C71 C72 102.9(3) . . ?
H71A C71 H71B 109.1 . . ?
C72 C71 H71A 111.2 . . ?
C72 C71 H71B 111.2 . . ?
C71 C72 H72A 111.2 . . ?
C71 C72 H72B 111.2 . . ?
H72A C72 H72B 109.1 . . ?
C73 C72 C71 102.9(3) . . ?
C73 C72 H72A 111.2 . . ?
C73 C72 H72B 111.2 . . ?
O4 C73 C72 106.5(4) . . ?
O4 C73 H73A 110.4 . . ?
O4 C73 H73B 110.4 . . ?
C72 C73 H73A 110.4 . . ?
C72 C73 H73B 110.4 . . ?
H73A C73 H73B 108.6 . . ?
O1 Li1 O2 105.7(3) . . ?
O1 Li1 O4 102.8(3) . . ?
O3 Li1 O1 117.5(3) . . ?
O3 Li1 O2 103.7(3) . . ?
O3 Li1 O4 106.7(3) . . ?
O4 Li1 O2 121.4(3) . . ?
C57 C59 H59 129.7 . . ?
C60 C59 C57 100.5(5) . . ?
C60 C59 H59 129.7 . . ?
C57 C58 C60 104.1(7) . . ?
C57 C58 H58A 110.9 . . ?
C57 C58 H58B 110.9 . . ?
C60 C58 H58A 110.9 . . ?
C60 C58 H58B 110.9 . . ?
H58A C58 H58B 108.9 . . ?
C86 O5 Li2 125.0(3) . . ?
C90 O5 C86 107.8(3) . . ?
C90 O5 Li2 122.5(3) . . ?
C74 O6 C77 110.5(3) . . ?
C74 O6 Li2 127.4(3) . . ?
C77 O6 Li2 119.3(3) . . ?
C78 O7 Li2 117.3(3) . . ?
C81 O7 C78 110.4(3) . . ?
C81 O7 Li2 132.2(3) . . ?
C82 O8 Li2 125.3(3) . . ?
C85 O8 C82 108.1(3) . . ?
C85 O8 Li2 123.6(3) . . ?
O6 C74 H74A 111.0 . . ?
O6 C74 H74B 111.0 . . ?
H74A C74 H74B 109.0 . . ?
C75 C74 O6 103.7(4) . . ?
C75 C74 H74A 111.0 . . ?
C75 C74 H74B 111.0 . . ?
C74 C75 H75A 110.7 . . ?
C74 C75 H75B 110.7 . . ?
C74 C75 C76 105.0(4) . . ?
H75A C75 H75B 108.8 . . ?
C76 C75 H75A 110.7 . . ?
C76 C75 H75B 110.7 . . ?
C75 C76 H76A 111.6 . . ?
C75 C76 H76B 111.6 . . ?
H76A C76 H76B 109.4 . . ?
C77 C76 C75 100.9(4) . . ?
C77 C76 H76A 111.6 . . ?
C77 C76 H76B 111.6 . . ?
O6 C77 C76 104.6(4) . . ?
O6 C77 H77A 110.8 . . ?
O6 C77 H77B 110.8 . . ?
C76 C77 H77A 110.8 . . ?
C76 C77 H77B 110.8 . . ?
H77A C77 H77B 108.9 . . ?
O7 C78 H78A 110.7 . . ?
O7 C78 H78B 110.7 . . ?
O7 C78 C79 105.1(3) . . ?
H78A C78 H78B 108.8 . . ?
C79 C78 H78A 110.7 . . ?
C79 C78 H78B 110.7 . . ?
C78 C79 H79A 111.4 . . ?
C78 C79 H79B 111.4 . . ?
C78 C79 C80 101.9(3) . . ?
H79A C79 H79B 109.3 . . ?
C80 C79 H79A 111.4 . . ?
C80 C79 H79B 111.4 . . ?
C79 C80 H80A 111.3 . . ?
C79 C80 H80B 111.3 . . ?
C79 C80 C81 102.3(3) . . ?
H80A C80 H80B 109.2 . . ?
C81 C80 H80A 111.3 . . ?
C81 C80 H80B 111.3 . . ?
O7 C81 C80 103.9(3) . . ?
O7 C81 H81A 111.0 . . ?
O7 C81 H81B 111.0 . . ?
C80 C81 H81A 111.0 . . ?
C80 C81 H81B 111.0 . . ?
H81A C81 H81B 109.0 . . ?
O8 C82 H82A 110.8 . . ?
O8 C82 H82B 110.8 . . ?
O8 C82 C83 104.7(3) . . ?
H82A C82 H82B 108.9 . . ?
C83 C82 H82A 110.8 . . ?
C83 C82 H82B 110.8 . . ?
C82 C83 H83A 111.1 . . ?
C82 C83 H83B 111.1 . . ?
H83A C83 H83B 109.1 . . ?
C84 C83 C82 103.2(3) . . ?
C84 C83 H83A 111.1 . . ?
C84 C83 H83B 111.1 . . ?
C83 C84 H84A 111.0 . . ?
C83 C84 H84B 111.0 . . ?
H84A C84 H84B 109.0 . . ?
C85 C84 C83 103.7(3) . . ?
C85 C84 H84A 111.0 . . ?
C85 C84 H84B 111.0 . . ?
O8 C85 C84 109.2(3) . . ?
O8 C85 H85A 109.8 . . ?
O8 C85 H85B 109.8 . . ?
C84 C85 H85A 109.8 . . ?
C84 C85 H85B 109.8 . . ?
H85A C85 H85B 108.3 . . ?
O5 C86 H86A 110.6 . . ?
O5 C86 H86B 110.6 . . ?
O5 C86 C88 105.8(4) . . ?
H86A C86 H86B 108.7 . . ?
C88 C86 H86A 110.6 . . ?
C88 C86 H86B 110.6 . . ?
C86 C88 H88A 111.3 . . ?
C86 C88 H88B 111.3 . . ?
C86 C88 C89 102.1(4) . . ?
H88A C88 H88B 109.2 . . ?
C89 C88 H88A 111.3 . . ?
C89 C88 H88B 111.3 . . ?
C88 C89 H89A 110.8 . . ?
C88 C89 H89B 110.8 . . ?
C88 C89 C90 104.7(4) . . ?
H89A C89 H89B 108.9 . . ?
C90 C89 H89A 110.8 . . ?
C90 C89 H89B 110.8 . . ?
O5 C90 C89 107.0(4) . . ?
O5 C90 H90A 110.3 . . ?
O5 C90 H90B 110.3 . . ?
C89 C90 H90A 110.3 . . ?
C89 C90 H90B 110.3 . . ?
H90A C90 H90B 108.6 . . ?
O5 Li2 O8 105.9(3) . . ?
O6 Li2 O5 105.1(3) . . ?
O6 Li2 O7 108.0(3) . . ?
O6 Li2 O8 112.8(3) . . ?
O7 Li2 O5 120.4(3) . . ?
O7 Li2 O8 104.8(3) . . ?

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
V1 C1 C2 C3 178.7(2) . . . . ?
V1 C1 C6 C5 -178.7(2) . . . . ?
V1 C1 C6 C7 1.6(4) . . . . ?
V1 C8 C9 C10 179.6(2) . . . . ?
V1 C8 C13 C12 179.4(2) . . . . ?
V1 C8 C13 C14 -3.5(4) . . . . ?
V1 C15 C16 C17 -177.9(2) . . . . ?
V1 C15 C20 C19 178.2(2) . . . . ?
V1 C15 C20 C21 -1.7(4) . . . . ?
V1 C22 C23 C24 177.5(2) . . . . ?
V1 C22 C27 C26 -178.7(2) . . . . ?
V1 C22 C27 C28 0.1(4) . . . . ?
C1 C2 C3 C4 0.4(5) . . . . ?
C2 C1 C6 C5 1.9(4) . . . . ?
C2 C1 C6 C7 -177.8(3) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C4 C5 C6 C7 179.2(3) . . . . ?
C6 C1 C2 C3 -1.9(4) . . . . ?
C8 C9 C10 C11 0.5(5) . . . . ?
C9 C8 C13 C12 -2.2(4) . . . . ?
C9 C8 C13 C14 174.9(3) . . . . ?
C9 C10 C11 C12 -1.2(5) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C11 C12 C13 C8 1.7(5) . . . . ?
C11 C12 C13 C14 -175.5(3) . . . . ?
C13 C8 C9 C10 1.1(5) . . . . ?
C15 C16 C17 C18 0.1(5) . . . . ?
C16 C15 C20 C19 1.2(4) . . . . ?
C16 C15 C20 C21 -178.7(3) . . . . ?
C16 C17 C18 C19 0.0(5) . . . . ?
C17 C18 C19 C20 0.4(5) . . . . ?
C18 C19 C20 C15 -1.1(5) . . . . ?
C18 C19 C20 C21 178.8(3) . . . . ?
C20 C15 C16 C17 -0.8(5) . . . . ?
C22 C23 C24 C25 1.7(5) . . . . ?
C23 C22 C27 C26 -1.2(4) . . . . ?
C23 C22 C27 C28 177.6(3) . . . . ?
C23 C24 C25 C26 -1.7(5) . . . . ?
C24 C25 C26 C27 0.2(5) . . . . ?
C25 C26 C27 C22 1.2(5) . . . . ?
C25 C26 C27 C28 -177.6(3) . . . . ?
C27 C22 C23 C24 -0.2(4) . . . . ?
V2 C29 C30 C31 173.6(2) . . . . ?
V2 C29 C34 C33 -173.7(2) . . . . ?
V2 C29 C34 C35 7.8(4) . . . . ?
V2 C36 C37 C38 -175.4(2) . . . . ?
V2 C36 C41 C40 175.4(2) . . . . ?
V2 C36 C41 C42 -4.5(4) . . . . ?
V2 C43 C44 C45 -174.4(2) . . . . ?
V2 C43 C48 C47 173.7(2) . . . . ?
V2 C43 C48 C49 -5.9(4) . . . . ?
V2 C50 C51 C52 177.4(2) . . . . ?
V2 C50 C55 C54 -177.5(2) . . . . ?
V2 C50 C55 C56 2.4(4) . . . . ?
C29 C30 C31 C32 0.4(5) . . . . ?
C30 C29 C34 C33 1.7(4) . . . . ?
C30 C29 C34 C35 -176.8(3) . . . . ?
C30 C31 C32 C33 1.3(5) . . . . ?
C31 C32 C33 C34 -1.4(5) . . . . ?
C32 C33 C34 C29 -0.1(5) . . . . ?
C32 C33 C34 C35 178.4(3) . . . . ?
C34 C29 C30 C31 -1.9(4) . . . . ?
C36 C37 C38 C39 -0.8(5) . . . . ?
C37 C36 C41 C40 -1.6(4) . . . . ?
C37 C36 C41 C42 178.4(3) . . . . ?
C37 C38 C39 C40 -0.3(5) . . . . ?
C38 C39 C40 C41 0.5(5) . . . . ?
C39 C40 C41 C36 0.6(5) . . . . ?
C39 C40 C41 C42 -179.5(3) . . . . ?
C41 C36 C37 C38 1.8(4) . . . . ?
C43 C44 C45 C46 0.4(5) . . . . ?
C44 C43 C48 C47 -0.5(4) . . . . ?
C44 C43 C48 C49 179.9(3) . . . . ?
C44 C45 C46 C47 -0.7(5) . . . . ?
C45 C46 C47 C48 0.3(5) . . . . ?
C46 C47 C48 C43 0.3(5) . . . . ?
C46 C47 C48 C49 179.9(3) . . . . ?
C48 C43 C44 C45 0.2(4) . . . . ?
C50 C51 C52 C53 -0.2(5) . . . . ?
C51 C50 C55 C54 -1.7(4) . . . . ?
C51 C50 C55 C56 178.2(3) . . . . ?
C51 C52 C53 C54 -0.6(5) . . . . ?
C52 C53 C54 C55 0.2(5) . . . . ?
C53 C54 C55 C50 1.0(5) . . . . ?
C53 C54 C55 C56 -178.9(3) . . . . ?
C55 C50 C51 C52 1.4(5) . . . . ?
O1 C57 C59 C60 -38.2(7) . . . . ?
O1 C57 C58 C60 33.5(9) . . . . ?
O2 C62 C63 C64 -31.8(4) . . . . ?
O3 C66 C67 C68 -21.9(6) . . . . ?
O4 C70 C71 C72 25.9(4) . . . . ?
C57 O1 C61 C60 -3.5(5) . . . . ?
C61 O1 C57 C59 24.3(6) . . . . ?
C61 O1 C57 C58 -19.9(8) . . . . ?
C61 C60 C59 C57 36.6(7) . . . . ?
C61 C60 C58 C57 -33.9(8) . . . . ?
C62 O2 C65 C64 16.9(4) . . . . ?
C62 C63 C64 C65 41.7(4) . . . . ?
C63 C64 C65 O2 -36.2(4) . . . . ?
C65 O2 C62 C63 9.5(4) . . . . ?
C66 O3 C69 C68 25.1(5) . . . . ?
C66 C67 C68 C69 36.2(5) . . . . ?
C67 C68 C69 O3 -38.0(5) . . . . ?
C69 O3 C66 C67 -2.1(6) . . . . ?
C70 O4 C73 C72 -16.9(4) . . . . ?
C70 C71 C72 C73 -35.7(4) . . . . ?
C71 C72 C73 O4 32.7(4) . . . . ?
C73 O4 C70 C71 -6.4(4) . . . . ?
Li1 O1 C57 C59 -125.8(5) . . . . ?
Li1 O1 C57 C58 -170.0(7) . . . . ?
Li1 O1 C61 C60 150.7(3) . . . . ?
Li1 O2 C62 C63 -164.7(3) . . . . ?
Li1 O2 C65 C64 -169.9(3) . . . . ?
Li1 O3 C66 C67 155.9(4) . . . . ?
Li1 O3 C69 C68 -133.7(4) . . . . ?
Li1 O4 C70 C71 -168.3(3) . . . . ?
Li1 O4 C73 C72 144.7(3) . . . . ?
C59 C60 C61 O1 -23.7(6) . . . . ?
C58 C60 C61 O1 21.9(6) . . . . ?
O5 C86 C88 C89 -35.8(5) . . . . ?
O6 C74 C75 C76 -31.3(6) . . . . ?
O7 C78 C79 C80 32.2(4) . . . . ?
O8 C82 C83 C84 33.0(4) . . . . ?
C74 O6 C77 C76 13.9(5) . . . . ?
C74 O6 Li2 O5 129.4(4) . . . . ?
C74 O6 Li2 O7 -100.9(5) . . . . ?
C74 O6 Li2 O8 14.5(6) . . . . ?
C74 C75 C76 C77 39.8(6) . . . . ?
C75 C76 C77 O6 -31.4(4) . . . . ?
C77 O6 C74 C75 11.5(6) . . . . ?
C77 O6 Li2 O5 -71.3(4) . . . . ?
C77 O6 Li2 O7 58.5(5) . . . . ?
C77 O6 Li2 O8 173.8(3) . . . . ?
C78 O7 C81 C80 -14.2(4) . . . . ?
C78 O7 Li2 O5 166.3(3) . . . . ?
C78 O7 Li2 O6 45.7(4) . . . . ?
C78 O7 Li2 O8 -74.8(4) . . . . ?
C78 C79 C80 C81 -40.3(4) . . . . ?
C79 C80 C81 O7 33.8(4) . . . . ?
C81 O7 C78 C79 -11.4(4) . . . . ?
C81 O7 Li2 O5 -17.5(6) . . . . ?
C81 O7 Li2 O6 -138.1(4) . . . . ?
C81 O7 Li2 O8 101.4(4) . . . . ?
C82 O8 C85 C84 3.9(5) . . . . ?
C82 C83 C84 C85 -30.2(5) . . . . ?
C83 C84 C85 O8 17.0(5) . . . . ?
C85 O8 C82 C83 -23.1(4) . . . . ?
C86 O5 C90 C89 -8.9(4) . . . . ?
C86 C88 C89 C90 29.6(5) . . . . ?
C88 C89 C90 O5 -13.6(5) . . . . ?
C90 O5 C86 C88 28.3(4) . . . . ?
Li2 O5 C86 C88 -127.8(4) . . . . ?
Li2 O5 C90 C89 147.9(3) . . . . ?
Li2 O6 C74 C75 172.3(4) . . . . ?
Li2 O6 C77 C76 -148.6(4) . . . . ?
Li2 O7 C78 C79 165.6(3) . . . . ?
Li2 O7 C81 C80 169.4(4) . . . . ?
Li2 O8 C82 C83 137.6(3) . . . . ?
Li2 O8 C85 C84 -157.3(4) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '60.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   13.0
_STOE_evaluation_integration_B   1.3
_STOE_evaluation_integration_EMS 0.012
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 95.6
_STOE_evaluation_LANA_DXS_max_order -
_STOE_evaluation_LANA_DYS_max_order -
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 141.4
_STOE_evaluation_LANA_max_2theta_desired 141.4
_STOE_evaluation_LANA_mean_redundancy 4.5
_STOE_evaluation_LANA_number_refls_after_OR 66732
_STOE_evaluation_LANA_number_refls_outliers 3620
_STOE_evaluation_LANA_number_refls_total 70352
_STOE_evaluation_LANA_number_refls_unique 14814
_STOE_evaluation_LANA_number_refls_written 66732
_STOE_evaluation_LANA_OR_c1      0.050
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      1.0
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          12.7   27.9   43.1   58.3   73.5   88.7  103.9  119.1  134.3
#----------------------------------------------------------------------------
<Resolution>    5.36   3.04   2.07   1.57   1.28   1.10   0.99   0.90   0.84
N(total)         482   2684   4741   8549  12694  14330  11352  10575   4945
<Redundancy>     4.2    5.4    4.6    5.3    5.7    5.5    4.1    3.8    2.5
Complet. [%%]    97.0  100.0  100.0   99.9   99.2   98.9   94.5   97.1   82.9
<I/sigma>      166.9   79.8   35.8   16.8    8.4    5.2    4.2    2.7    2.1
R(int)         0.016  0.020  0.023  0.034  0.058  0.085  0.105  0.157  0.195
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     dwl_V_otolyl_3_norbornyl_Li_THF4_second_xta;
_STOE_measurement_max_exposure_per_frame '1.0 s'
_STOE_measurement_mean_exposure_per_frame '1.0 s'
_STOE_measurement_min_exposure_per_frame '1.0 s'
_STOE_measurement_total_exposure_time '76 min'
_STOE_measurement_total_frame_number 4589
_STOE_measurement_total_run_number 68
_STOE_measurement_tube_power     '50.0 W'
_exptl_crystal_recrystallization_method 'Solvent layering'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_otolyl_4
_database_code_depnum_ccdc_archive 'CCDC 2334909'
loop_
_audit_author_name
_audit_author_address
'Daniel Laorenza'
;Harvard University
United States of America
;
_audit_update_record             
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        tetra(o-tolyl)molybdenum
_chemical_formula_moiety         'C28 H28 Mo'
_chemical_formula_sum            'C28 H28 Mo'
_chemical_formula_weight         460.44
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.8490(2)
_cell_length_b                   11.8490(2)
_cell_length_c                   7.8931(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1108.18(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      34.076
_cell_measurement_theta_min      2.431
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1142 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.9028.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             476
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            40785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.103
_diffrn_reflns_theta_min         2.431
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.99
_diffrn_source_power             0.0495
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                2066
_reflns_number_total             2577
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Flack x determined using 795 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.206(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.127
_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/[σ²(Fo²)+(0.0330P)²+1.2034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0917
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7C,H7B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mo1 Mo 0.500000 0.500000 0.500000 0.01787(9) Uani 1 4 d S T P . .
C1 C 0.3526(3) 0.4735(3) 0.3531(4) 0.0273(6) Uani 1 1 d . . . . .
C2 C 0.2563(3) 0.5382(3) 0.3922(5) 0.0301(6) Uani 1 1 d . . . . .
H2 H 0.260971 0.595370 0.476365 0.036 Uiso 1 1 calc R U . . .
C3 C 0.1539(3) 0.5194(3) 0.3086(5) 0.0354(8) Uani 1 1 d . . . . .
H3 H 0.089605 0.563921 0.334803 0.043 Uiso 1 1 calc R U . . .
C4 C 0.1471(3) 0.4354(3) 0.1876(5) 0.0360(7) Uani 1 1 d . . . . .
H4 H 0.077136 0.420448 0.133300 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2417(3) 0.3730(3) 0.1450(5) 0.0354(7) Uani 1 1 d . . . . .
H5 H 0.236272 0.316565 0.059950 0.042 Uiso 1 1 calc R U . . .
C6 C 0.3452(3) 0.3919(3) 0.2253(5) 0.0313(6) Uani 1 1 d . . . . .
C7 C 0.4473(4) 0.3289(4) 0.1673(6) 0.0422(9) Uani 1 1 d . . . . .
H7A H 0.502192 0.382095 0.119879 0.063 Uiso 1 1 calc R U . . .
H7C H 0.425521 0.274087 0.080241 0.063 Uiso 1 1 calc R U . . .
H7B H 0.481100 0.289213 0.263628 0.063 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mo1 C1 2.120(3) 3_566 ?
Mo1 C1 2.120(3) . ?
Mo1 C1 2.120(3) 4_656 ?
Mo1 C1 2.120(3) 2_665 ?
C1 C2 1.409(5) . ?
C1 C6 1.400(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.399(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.398(5) . ?
C6 C7 1.493(5) . ?
C7 H7A 0.9800 . ?
C7 H7C 0.9800 . ?
C7 H7B 0.9800 . ?

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
C1 Mo1 C1 113.66(17) 3_566 4_656 ?
C1 Mo1 C1 107.42(8) 4_656 . ?
C1 Mo1 C1 107.42(8) 3_566 . ?
C1 Mo1 C1 107.42(8) 3_566 2_665 ?
C1 Mo1 C1 107.42(8) 4_656 2_665 ?
C1 Mo1 C1 113.66(17) 2_665 . ?
C2 C1 Mo1 117.8(2) . . ?
C6 C1 Mo1 123.2(3) . . ?
C6 C1 C2 118.9(3) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 121.0(3) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 119.4(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7C 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7C C7 H7B 109.5 . . ?

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
Mo1 C1 C2 C3 -175.4(3) . . . . ?
Mo1 C1 C6 C5 174.2(3) . . . . ?
Mo1 C1 C6 C7 -8.9(5) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C2 C1 C6 C5 -2.9(5) . . . . ?
C2 C1 C6 C7 174.0(4) . . . . ?
C2 C3 C4 C5 -2.2(6) . . . . ?
C3 C4 C5 C6 1.2(6) . . . . ?
C4 C5 C6 C1 1.4(6) . . . . ?
C4 C5 C6 C7 -175.6(4) . . . . ?
C6 C1 C2 C3 1.9(5) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mounted under N2 in paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_al_metms_4_li_12_crown_4_2
_database_code_depnum_ccdc_archive 'CCDC 2334911'
loop_
_audit_author_name
_audit_author_address
'Daniel Laorenza'
;Harvard University
United States of America
;
_audit_update_record             
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis(12-crown-4)lithium tetrakis(trimethylsilylmethyl)aluminate'
_chemical_formula_moiety         'C16 H32 Li O8, C16 H44 Al Si4'
_chemical_formula_sum            'C32 H76 Al Li O8 Si4'
_chemical_formula_weight         735.20
_chemical_melting_point          ?
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'
Al Al 0.2130 0.2455 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4242(13)
_cell_length_b                   21.275(2)
_cell_length_c                   20.498(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.574(10)
_cell_angle_gamma                90
_cell_volume                     4399.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.00
_cell_measurement_theta_min      7.65
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.8542
_exptl_absorpt_correction_T_min  0.5382
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 30 3 0.5568
8 -30 -5 0.2322
8 -30 -15 0.4176
24 -1 -30 0.7298
0 30 -1 0.3481
0 15 4 0.4149
1 3 30 1.0047
-30 -5 -7 0.7364
-9 30 -4 0.3094
-4 15 3 0.2695
-9 30 11 0.3456
-25 2 30 0.6766
0 -1 0 0.3696
1 -15 -4 0.2582

_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33028
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.009
_diffrn_reflns_theta_min         3.046
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
 2222 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_d_resolution_high        0.820
_reflns_d_resolution_low         14.509
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              -19
_reflns_number_gt                5858
_reflns_number_total             8151
_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     I>4u(I)
_computing_cell_refinement       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      0.892
_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)+(0.0331P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0632
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C13(H13A,H13B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Si1 Si 0.91238(4) 0.60733(2) 0.55194(2) 0.01685(9) Uani 1 1 d . . . . .
Si2 Si 0.51264(4) 0.75188(2) 0.48431(2) 0.01767(9) Uani 1 1 d . . . . .
Si3 Si 0.92988(4) 0.87766(2) 0.54115(2) 0.01675(9) Uani 1 1 d . . . . .
Si4 Si 1.03518(4) 0.75792(2) 0.75678(2) 0.01772(10) Uani 1 1 d . . . . .
Al1 Al 0.81160(4) 0.74761(2) 0.60311(2) 0.01439(9) Uani 1 1 d . . . . .
C1 C 0.82302(15) 0.65245(7) 0.60287(8) 0.0178(3) Uani 1 1 d . . . . .
H1A H 0.860941 0.639697 0.650255 0.021 Uiso 1 1 calc R U . . .
H1B H 0.730546 0.636894 0.590491 0.021 Uiso 1 1 calc R U . . .
C2 C 0.90334(17) 0.52029(7) 0.56830(9) 0.0263(4) Uani 1 1 d . . . . .
H2A H 0.810942 0.506296 0.553849 0.040 Uiso 1 1 calc R U . . .
H2B H 0.937802 0.512017 0.616577 0.040 Uiso 1 1 calc R U . . .
H2C H 0.956574 0.497377 0.542957 0.040 Uiso 1 1 calc R U . . .
C3 C 0.83956(17) 0.62022(8) 0.45983(8) 0.0262(4) Uani 1 1 d . . . . .
H3A H 0.882985 0.592339 0.433897 0.039 Uiso 1 1 calc R U . . .
H3B H 0.853127 0.664058 0.448471 0.039 Uiso 1 1 calc R U . . .
H3C H 0.744409 0.611036 0.448826 0.039 Uiso 1 1 calc R U . . .
C4 C 1.09200(15) 0.62947(8) 0.57047(9) 0.0289(4) Uani 1 1 d . . . . .
H4A H 1.132842 0.624095 0.618719 0.043 Uiso 1 1 calc R U . . .
H4B H 1.099990 0.673459 0.557867 0.043 Uiso 1 1 calc R U . . .
H4C H 1.137072 0.602429 0.544523 0.043 Uiso 1 1 calc R U . . .
C5 C 0.61793(14) 0.77154(7) 0.56844(8) 0.0167(3) Uani 1 1 d . . . . .
H5A H 0.572099 0.754202 0.601299 0.020 Uiso 1 1 calc R U . . .
H5B H 0.614310 0.817852 0.572373 0.020 Uiso 1 1 calc R U . . .
C6 C 0.35458(16) 0.79895(8) 0.46405(9) 0.0303(4) Uani 1 1 d . . . . .
H6A H 0.301523 0.787779 0.495593 0.046 Uiso 1 1 calc R U . . .
H6B H 0.304114 0.789682 0.417886 0.046 Uiso 1 1 calc R U . . .
H6C H 0.375842 0.843873 0.468120 0.046 Uiso 1 1 calc R U . . .
C7 C 0.46174(17) 0.66674(7) 0.47867(9) 0.0273(4) Uani 1 1 d . . . . .
H7A H 0.540414 0.640255 0.494260 0.041 Uiso 1 1 calc R U . . .
H7B H 0.418048 0.656263 0.431781 0.041 Uiso 1 1 calc R U . . .
H7C H 0.400254 0.659391 0.507017 0.041 Uiso 1 1 calc R U . . .
C8 C 0.59241(17) 0.76648(8) 0.41291(8) 0.0269(4) Uani 1 1 d . . . . .
H8A H 0.608629 0.811603 0.409596 0.040 Uiso 1 1 calc R U . . .
H8B H 0.533411 0.751722 0.370609 0.040 Uiso 1 1 calc R U . . .
H8C H 0.676742 0.743733 0.421355 0.040 Uiso 1 1 calc R U . . .
C9 C 0.92211(15) 0.79134(7) 0.54885(8) 0.0181(3) Uani 1 1 d . . . . .
H9A H 1.014410 0.776771 0.566986 0.022 Uiso 1 1 calc R U . . .
H9B H 0.892826 0.774648 0.502382 0.022 Uiso 1 1 calc R U . . .
C10 C 0.98903(16) 0.91850(7) 0.62449(8) 0.0226(4) Uani 1 1 d . . . . .
H10A H 0.929850 0.908275 0.653310 0.034 Uiso 1 1 calc R U . . .
H10B H 0.988963 0.964045 0.617305 0.034 Uiso 1 1 calc R U . . .
H10C H 1.079169 0.904515 0.646360 0.034 Uiso 1 1 calc R U . . .
C11 C 0.76399(15) 0.91380(8) 0.50155(8) 0.0243(4) Uani 1 1 d . . . . .
H11A H 0.729086 0.896132 0.456414 0.037 Uiso 1 1 calc R U . . .
H11B H 0.773948 0.959403 0.498147 0.037 Uiso 1 1 calc R U . . .
H11C H 0.702469 0.904723 0.529457 0.037 Uiso 1 1 calc R U . . .
C12 C 1.04471(16) 0.90229(8) 0.48800(9) 0.0269(4) Uani 1 1 d . . . . .
H12A H 1.134665 0.887510 0.509017 0.040 Uiso 1 1 calc R U . . .
H12B H 1.044869 0.948226 0.484455 0.040 Uiso 1 1 calc R U . . .
H12C H 1.014332 0.883948 0.442883 0.040 Uiso 1 1 calc R U . . .
C13 C 0.86978(14) 0.77452(7) 0.70074(7) 0.0168(3) Uani 1 1 d . . . . .
H13A H 0.858350 0.820708 0.701044 0.020 Uiso 1 1 calc R U . . .
H13B H 0.804427 0.756543 0.723197 0.020 Uiso 1 1 calc R U . . .
C14 C 1.04959(17) 0.67424(8) 0.78616(9) 0.0342(5) Uani 1 1 d . . . . .
H14A H 0.990121 0.667108 0.815619 0.051 Uiso 1 1 calc R U . . .
H14B H 1.141159 0.665683 0.811137 0.051 Uiso 1 1 calc R U . . .
H14C H 1.025041 0.646160 0.747099 0.051 Uiso 1 1 calc R U . . .
C15 C 1.06953(17) 0.80879(9) 0.83412(9) 0.0339(4) Uani 1 1 d . . . . .
H15A H 1.063749 0.853130 0.820741 0.051 Uiso 1 1 calc R U . . .
H15B H 1.158662 0.799836 0.862099 0.051 Uiso 1 1 calc R U . . .
H15C H 1.004095 0.799947 0.859866 0.051 Uiso 1 1 calc R U . . .
C16 C 1.17661(16) 0.77097(8) 0.71684(9) 0.0316(4) Uani 1 1 d . . . . .
H16A H 1.169173 0.741616 0.679227 0.047 Uiso 1 1 calc R U . . .
H16B H 1.260706 0.763871 0.750373 0.047 Uiso 1 1 calc R U . . .
H16C H 1.173745 0.814222 0.700098 0.047 Uiso 1 1 calc R U . . .
O1 O 0.59547(10) 0.43593(5) 0.33732(5) 0.0194(2) Uani 1 1 d . . . . .
O2 O 0.43075(10) 0.39455(5) 0.21901(5) 0.0205(2) Uani 1 1 d . . . . .
O3 O 0.27429(10) 0.49743(5) 0.22370(5) 0.0184(2) Uani 1 1 d . . . . .
O4 O 0.43914(10) 0.53900(5) 0.34155(5) 0.0187(2) Uani 1 1 d . . . . .
O5 O 0.68101(10) 0.56184(5) 0.29406(5) 0.0191(2) Uani 1 1 d . . . . .
O6 O 0.69355(10) 0.45882(5) 0.21376(5) 0.0203(2) Uani 1 1 d . . . . .
O7 O 0.46066(10) 0.50188(5) 0.13063(5) 0.0186(2) Uani 1 1 d . . . . .
O8 O 0.44978(10) 0.60412(5) 0.21041(5) 0.0195(2) Uani 1 1 d . . . . .
C17 C 0.47010(15) 0.49813(7) 0.39815(8) 0.0202(3) Uani 1 1 d . . . . .
H17A H 0.400690 0.465557 0.394043 0.024 Uiso 1 1 calc R U . . .
H17B H 0.476113 0.522071 0.440225 0.024 Uiso 1 1 calc R U . . .
C18 C 0.60176(15) 0.46815(7) 0.39910(8) 0.0198(3) Uani 1 1 d . . . . .
H18A H 0.671216 0.500966 0.405988 0.024 Uiso 1 1 calc R U . . .
H18B H 0.625981 0.438120 0.437112 0.024 Uiso 1 1 calc R U . . .
C19 C 0.54399(16) 0.37367(7) 0.33501(8) 0.0214(3) Uani 1 1 d . . . . .
H19A H 0.461033 0.373311 0.350193 0.026 Uiso 1 1 calc R U . . .
H19B H 0.608963 0.345519 0.364692 0.026 Uiso 1 1 calc R U . . .
C20 C 0.51767(16) 0.35230(7) 0.26315(8) 0.0220(4) Uani 1 1 d . . . . .
H20A H 0.602508 0.349551 0.249906 0.026 Uiso 1 1 calc R U . . .
H20B H 0.477507 0.309847 0.258892 0.026 Uiso 1 1 calc R U . . .
C21 C 0.29379(15) 0.38449(7) 0.21527(8) 0.0220(4) Uani 1 1 d . . . . .
H21A H 0.280524 0.376984 0.260789 0.026 Uiso 1 1 calc R U . . .
H21B H 0.260389 0.347574 0.186624 0.026 Uiso 1 1 calc R U . . .
C22 C 0.22182(15) 0.44320(7) 0.18498(8) 0.0205(3) Uani 1 1 d . . . . .
H22A H 0.230472 0.448340 0.138277 0.025 Uiso 1 1 calc R U . . .
H22B H 0.126408 0.439067 0.183213 0.025 Uiso 1 1 calc R U . . .
C23 C 0.21925(15) 0.50837(7) 0.27963(8) 0.0195(3) Uani 1 1 d . . . . .
H23A H 0.220567 0.469262 0.305958 0.023 Uiso 1 1 calc R U . . .
H23B H 0.126392 0.522956 0.263917 0.023 Uiso 1 1 calc R U . . .
C24 C 0.30345(15) 0.55807(7) 0.32220(8) 0.0191(3) Uani 1 1 d . . . . .
H24A H 0.295623 0.597858 0.296457 0.023 Uiso 1 1 calc R U . . .
H24B H 0.271336 0.565714 0.363039 0.023 Uiso 1 1 calc R U . . .
C25 C 0.79701(15) 0.55274(7) 0.27038(8) 0.0225(4) Uani 1 1 d . . . . .
H25A H 0.876125 0.568369 0.304023 0.027 Uiso 1 1 calc R U . . .
H25B H 0.789243 0.575842 0.227634 0.027 Uiso 1 1 calc R U . . .
C26 C 0.80926(15) 0.48313(7) 0.25941(8) 0.0210(4) Uani 1 1 d . . . . .
H26A H 0.887277 0.475220 0.241272 0.025 Uiso 1 1 calc R U . . .
H26B H 0.823513 0.460990 0.303132 0.025 Uiso 1 1 calc R U . . .
C27 C 0.68859(15) 0.46987(8) 0.14460(8) 0.0214(3) Uani 1 1 d . . . . .
H27A H 0.747122 0.440089 0.128705 0.026 Uiso 1 1 calc R U . . .
H27B H 0.717314 0.513277 0.138129 0.026 Uiso 1 1 calc R U . . .
C28 C 0.54612(15) 0.46014(7) 0.10662(8) 0.0205(3) Uani 1 1 d . . . . .
H28A H 0.536654 0.467644 0.057975 0.025 Uiso 1 1 calc R U . . .
H28B H 0.520003 0.416131 0.112289 0.025 Uiso 1 1 calc R U . . .
C29 C 0.45073(16) 0.56265(7) 0.10080(8) 0.0211(3) Uani 1 1 d . . . . .
H29A H 0.399155 0.560618 0.053165 0.025 Uiso 1 1 calc R U . . .
H29B H 0.540061 0.579327 0.102220 0.025 Uiso 1 1 calc R U . . .
C30 C 0.38172(15) 0.60439(7) 0.14079(8) 0.0203(3) Uani 1 1 d . . . . .
H30A H 0.377847 0.647868 0.123182 0.024 Uiso 1 1 calc R U . . .
H30B H 0.289697 0.589483 0.135487 0.024 Uiso 1 1 calc R U . . .
C31 C 0.56042(15) 0.64597(7) 0.22663(8) 0.0219(4) Uani 1 1 d . . . . .
H31A H 0.529918 0.689926 0.227849 0.026 Uiso 1 1 calc R U . . .
H31B H 0.612708 0.642806 0.192582 0.026 Uiso 1 1 calc R U . . .
C32 C 0.64302(16) 0.62650(7) 0.29488(8) 0.0211(3) Uani 1 1 d . . . . .
H32A H 0.723324 0.653143 0.307581 0.025 Uiso 1 1 calc R U . . .
H32B H 0.591631 0.632630 0.328954 0.025 Uiso 1 1 calc R U . . .
Li1 Li 0.5022(3) 0.50016(13) 0.24675(15) 0.0231(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Si1 C1 1.8352(15) . ?
Si1 C2 1.8886(16) . ?
Si1 C3 1.8695(17) . ?
Si1 C4 1.8746(16) . ?
Si2 C5 1.8441(15) . ?
Si2 C6 1.8830(16) . ?
Si2 C7 1.8827(16) . ?
Si2 C8 1.8821(17) . ?
Si3 C9 1.8466(15) . ?
Si3 C10 1.8771(16) . ?
Si3 C11 1.8799(16) . ?
Si3 C12 1.8844(16) . ?
Si4 C13 1.8493(15) . ?
Si4 C14 1.8732(17) . ?
Si4 C15 1.8780(18) . ?
Si4 C16 1.8782(18) . ?
Al1 C1 2.0282(15) . ?
Al1 C5 2.0293(15) . ?
Al1 C9 2.0186(16) . ?
Al1 C13 2.0223(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 C18 1.4269(18) . ?
O1 C19 1.4255(17) . ?
O1 Li1 2.313(3) . ?
O2 C20 1.4265(18) . ?
O2 C21 1.4265(17) . ?
O2 Li1 2.390(3) . ?
O3 C22 1.4289(17) . ?
O3 C23 1.4242(17) . ?
O3 Li1 2.304(3) . ?
O4 C17 1.4205(17) . ?
O4 C24 1.4283(17) . ?
O4 Li1 2.352(3) . ?
O5 C25 1.4250(18) . ?
O5 C32 1.4328(18) . ?
O5 Li1 2.286(3) . ?
O6 C26 1.4248(18) . ?
O6 C27 1.4248(18) . ?
O6 Li1 2.427(3) . ?
O7 C28 1.4300(17) . ?
O7 C29 1.4227(17) . ?
O7 Li1 2.310(3) . ?
O8 C30 1.4248(18) . ?
O8 C31 1.4285(17) . ?
O8 Li1 2.354(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.509(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.499(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.508(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.505(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.508(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.508(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.508(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.505(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?

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
C1 Si1 C2 110.90(7) . . ?
C1 Si1 C3 111.25(7) . . ?
C1 Si1 C4 112.17(8) . . ?
C3 Si1 C2 107.31(8) . . ?
C3 Si1 C4 107.39(8) . . ?
C4 Si1 C2 107.60(8) . . ?
C5 Si2 C6 111.56(7) . . ?
C5 Si2 C7 111.59(7) . . ?
C5 Si2 C8 114.47(7) . . ?
C7 Si2 C6 106.30(8) . . ?
C8 Si2 C6 105.90(8) . . ?
C8 Si2 C7 106.49(8) . . ?
C9 Si3 C10 113.21(7) . . ?
C9 Si3 C11 112.85(7) . . ?
C9 Si3 C12 111.95(7) . . ?
C10 Si3 C11 105.03(7) . . ?
C10 Si3 C12 106.64(8) . . ?
C11 Si3 C12 106.60(7) . . ?
C13 Si4 C14 111.59(7) . . ?
C13 Si4 C15 111.35(7) . . ?
C13 Si4 C16 114.36(8) . . ?
C14 Si4 C15 107.06(9) . . ?
C14 Si4 C16 105.80(8) . . ?
C15 Si4 C16 106.19(9) . . ?
C1 Al1 C5 107.66(6) . . ?
C9 Al1 C1 114.63(6) . . ?
C9 Al1 C5 110.29(7) . . ?
C9 Al1 C13 110.13(7) . . ?
C13 Al1 C1 106.37(6) . . ?
C13 Al1 C5 107.44(6) . . ?
Si1 C1 Al1 124.20(8) . . ?
Si1 C1 H1A 106.3 . . ?
Si1 C1 H1B 106.3 . . ?
Al1 C1 H1A 106.3 . . ?
Al1 C1 H1B 106.3 . . ?
H1A C1 H1B 106.4 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 Al1 125.18(8) . . ?
Si2 C5 H5A 106.0 . . ?
Si2 C5 H5B 106.0 . . ?
Al1 C5 H5A 106.0 . . ?
Al1 C5 H5B 106.0 . . ?
H5A C5 H5B 106.3 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C9 Al1 123.28(8) . . ?
Si3 C9 H9A 106.5 . . ?
Si3 C9 H9B 106.5 . . ?
Al1 C9 H9A 106.5 . . ?
Al1 C9 H9B 106.5 . . ?
H9A C9 H9B 106.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 Al1 124.13(8) . . ?
Si4 C13 H13A 106.3 . . ?
Si4 C13 H13B 106.3 . . ?
Al1 C13 H13A 106.3 . . ?
Al1 C13 H13B 106.3 . . ?
H13A C13 H13B 106.4 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 O1 Li1 110.15(11) . . ?
C19 O1 C18 114.13(12) . . ?
C19 O1 Li1 116.33(11) . . ?
C20 O2 Li1 109.35(11) . . ?
C21 O2 C20 114.02(12) . . ?
C21 O2 Li1 113.68(11) . . ?
C22 O3 Li1 111.41(11) . . ?
C23 O3 C22 113.80(11) . . ?
C23 O3 Li1 115.75(11) . . ?
C17 O4 C24 113.97(11) . . ?
C17 O4 Li1 113.97(11) . . ?
C24 O4 Li1 109.48(11) . . ?
C25 O5 C32 113.27(11) . . ?
C25 O5 Li1 116.66(11) . . ?
C32 O5 Li1 110.97(11) . . ?
C26 O6 C27 113.98(11) . . ?
C26 O6 Li1 107.74(11) . . ?
C27 O6 Li1 113.00(11) . . ?
C28 O7 Li1 111.91(11) . . ?
C29 O7 C28 113.63(12) . . ?
C29 O7 Li1 115.58(11) . . ?
C30 O8 C31 113.58(11) . . ?
C30 O8 Li1 109.76(11) . . ?
C31 O8 Li1 113.73(11) . . ?
O4 C17 H17A 110.4 . . ?
O4 C17 H17B 110.4 . . ?
O4 C17 C18 106.76(12) . . ?
H17A C17 H17B 108.6 . . ?
C18 C17 H17A 110.4 . . ?
C18 C17 H17B 110.4 . . ?
O1 C18 C17 110.67(12) . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O1 C19 H19A 110.4 . . ?
O1 C19 H19B 110.4 . . ?
O1 C19 C20 106.78(12) . . ?
H19A C19 H19B 108.6 . . ?
C20 C19 H19A 110.4 . . ?
C20 C19 H19B 110.4 . . ?
O2 C20 C19 111.22(13) . . ?
O2 C20 H20A 109.4 . . ?
O2 C20 H20B 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
O2 C21 H21A 110.4 . . ?
O2 C21 H21B 110.4 . . ?
O2 C21 C22 106.59(12) . . ?
H21A C21 H21B 108.6 . . ?
C22 C21 H21A 110.4 . . ?
C22 C21 H21B 110.4 . . ?
O3 C22 C21 111.03(12) . . ?
O3 C22 H22A 109.4 . . ?
O3 C22 H22B 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
O3 C23 H23A 110.4 . . ?
O3 C23 H23B 110.4 . . ?
O3 C23 C24 106.70(12) . . ?
H23A C23 H23B 108.6 . . ?
C24 C23 H23A 110.4 . . ?
C24 C23 H23B 110.4 . . ?
O4 C24 C23 110.72(12) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
O5 C25 H25A 110.3 . . ?
O5 C25 H25B 110.3 . . ?
O5 C25 C26 107.16(12) . . ?
H25A C25 H25B 108.5 . . ?
C26 C25 H25A 110.3 . . ?
C26 C25 H25B 110.3 . . ?
O6 C26 C25 111.40(13) . . ?
O6 C26 H26A 109.3 . . ?
O6 C26 H26B 109.3 . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
O6 C27 H27A 110.5 . . ?
O6 C27 H27B 110.5 . . ?
O6 C27 C28 105.99(12) . . ?
H27A C27 H27B 108.7 . . ?
C28 C27 H27A 110.5 . . ?
C28 C27 H27B 110.5 . . ?
O7 C28 C27 110.79(13) . . ?
O7 C28 H28A 109.5 . . ?
O7 C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
O7 C29 H29A 110.3 . . ?
O7 C29 H29B 110.3 . . ?
O7 C29 C30 107.13(12) . . ?
H29A C29 H29B 108.5 . . ?
C30 C29 H29A 110.3 . . ?
C30 C29 H29B 110.3 . . ?
O8 C30 C29 110.89(12) . . ?
O8 C30 H30A 109.5 . . ?
O8 C30 H30B 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
O8 C31 H31A 110.4 . . ?
O8 C31 H31B 110.4 . . ?
O8 C31 C32 106.53(12) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.4 . . ?
C32 C31 H31B 110.4 . . ?
O5 C32 C31 110.41(13) . . ?
O5 C32 H32A 109.6 . . ?
O5 C32 H32B 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
O1 Li1 O2 71.24(9) . . ?
O1 Li1 O4 72.12(9) . . ?
O1 Li1 O6 78.50(9) . . ?
O1 Li1 O8 145.72(14) . . ?
O2 Li1 O6 79.74(9) . . ?
O3 Li1 O1 110.68(12) . . ?
O3 Li1 O2 71.57(9) . . ?
O3 Li1 O4 71.94(9) . . ?
O3 Li1 O6 144.24(14) . . ?
O3 Li1 O7 82.69(10) . . ?
O3 Li1 O8 79.25(10) . . ?
O4 Li1 O2 113.05(12) . . ?
O4 Li1 O6 141.05(13) . . ?
O4 Li1 O8 80.82(10) . . ?
O5 Li1 O1 82.27(10) . . ?
O5 Li1 O2 144.33(14) . . ?
O5 Li1 O3 142.20(14) . . ?
O5 Li1 O4 79.36(10) . . ?
O5 Li1 O6 71.74(9) . . ?
O5 Li1 O7 110.46(12) . . ?
O5 Li1 O8 72.21(9) . . ?
O7 Li1 O1 140.20(14) . . ?
O7 Li1 O2 78.67(10) . . ?
O7 Li1 O4 145.76(14) . . ?
O7 Li1 O6 70.89(9) . . ?
O7 Li1 O8 71.98(9) . . ?
O8 Li1 O2 140.75(13) . . ?
O8 Li1 O6 113.21(12) . . ?

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
C2 Si1 C1 Al1 178.23(9) . . . . ?
C3 Si1 C1 Al1 -62.42(12) . . . . ?
C4 Si1 C1 Al1 57.89(12) . . . . ?
C6 Si2 C5 Al1 -165.87(9) . . . . ?
C7 Si2 C5 Al1 75.39(11) . . . . ?
C8 Si2 C5 Al1 -45.64(12) . . . . ?
C10 Si3 C9 Al1 58.45(11) . . . . ?
C11 Si3 C9 Al1 -60.69(12) . . . . ?
C12 Si3 C9 Al1 179.03(9) . . . . ?
C14 Si4 C13 Al1 -76.66(12) . . . . ?
C15 Si4 C13 Al1 163.76(10) . . . . ?
C16 Si4 C13 Al1 43.38(12) . . . . ?
O1 C19 C20 O2 -56.30(16) . . . . ?
O2 C21 C22 O3 -56.68(16) . . . . ?
O3 C23 C24 O4 -56.39(16) . . . . ?
O4 C17 C18 O1 -57.40(16) . . . . ?
O5 C25 C26 O6 56.94(17) . . . . ?
O6 C27 C28 O7 58.63(16) . . . . ?
O7 C29 C30 O8 55.70(16) . . . . ?
O8 C31 C32 O5 56.87(16) . . . . ?
C17 O4 C24 C23 -81.88(16) . . . . ?
C18 O1 C19 C20 168.31(12) . . . . ?
C19 O1 C18 C17 -84.24(15) . . . . ?
C20 O2 C21 C22 163.12(12) . . . . ?
C21 O2 C20 C19 -82.19(16) . . . . ?
C22 O3 C23 C24 168.70(12) . . . . ?
C23 O3 C22 C21 -84.53(15) . . . . ?
C24 O4 C17 C18 163.83(12) . . . . ?
C25 O5 C32 C31 84.60(15) . . . . ?
C26 O6 C27 C28 -162.62(12) . . . . ?
C27 O6 C26 C25 80.17(16) . . . . ?
C28 O7 C29 C30 -168.59(12) . . . . ?
C29 O7 C28 C27 84.00(15) . . . . ?
C30 O8 C31 C32 -163.56(12) . . . . ?
C31 O8 C30 C29 82.16(16) . . . . ?
C32 O5 C25 C26 -169.13(12) . . . . ?
Li1 O1 C18 C17 48.77(15) . . . . ?
Li1 O1 C19 C20 38.30(16) . . . . ?
Li1 O2 C20 C19 46.30(15) . . . . ?
Li1 O2 C21 C22 36.85(16) . . . . ?
Li1 O3 C22 C21 48.55(16) . . . . ?
Li1 O3 C23 C24 37.72(16) . . . . ?
Li1 O4 C17 C18 37.17(16) . . . . ?
Li1 O4 C24 C23 47.09(15) . . . . ?
Li1 O5 C25 C26 -38.46(17) . . . . ?
Li1 O5 C32 C31 -48.85(16) . . . . ?
Li1 O6 C26 C25 -46.08(16) . . . . ?
Li1 O6 C27 C28 -39.17(15) . . . . ?
Li1 O7 C28 C27 -49.15(16) . . . . ?
Li1 O7 C29 C30 -37.22(16) . . . . ?
Li1 O8 C30 C29 -46.40(15) . . . . ?
Li1 O8 C31 C32 -37.05(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '60.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   18.0
_STOE_evaluation_integration_B   1.0
_STOE_evaluation_integration_EMS 0.028
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 97.8
_STOE_evaluation_LANA_DXS_max_order -
_STOE_evaluation_LANA_DYS_max_order -
_STOE_evaluation_LANA_FS_max_order 2
_STOE_evaluation_LANA_max_2theta_available 140.1
_STOE_evaluation_LANA_max_2theta_desired 140.1
_STOE_evaluation_LANA_mean_redundancy 4.0
_STOE_evaluation_LANA_number_refls_after_OR 33049
_STOE_evaluation_LANA_number_refls_outliers 838
_STOE_evaluation_LANA_number_refls_total 33887
_STOE_evaluation_LANA_number_refls_unique 8162
_STOE_evaluation_LANA_number_refls_written 33049
_STOE_evaluation_LANA_OR_c1      0.050
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      1.0
_STOE_evaluation_LANA_point_group 2/m
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          11.3   26.5   41.7   56.9   72.1   87.3  102.5  117.7  132.9
#----------------------------------------------------------------------------
<Resolution>    5.63   3.20   2.16   1.59   1.29   1.12   1.00   0.90   0.85
N(total)         152   1033   2148   3378   5907   6995   5646   5782   2846
<Redundancy>     2.9    4.7    4.3    4.1    5.1    5.1    3.8    3.8    2.4
Complet. [%%]    95.7  100.0  100.0   99.9  100.0   99.9   96.3   99.9   90.8
<I/sigma>       58.2   66.3   27.2   16.0    9.1    6.5    5.4    4.8    4.3
R(int)         0.022  0.017  0.021  0.025  0.037  0.045  0.056  0.061  0.067
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     Al_MeTMS_4_Li_12_crown_4_2
_STOE_measurement_max_exposure_per_frame '3.0 s'
_STOE_measurement_mean_exposure_per_frame '2.8 s'
_STOE_measurement_min_exposure_per_frame '1.0 s'
_STOE_measurement_total_exposure_time '104 min'
_STOE_measurement_total_frame_number 2222
_STOE_measurement_total_run_number 28
_STOE_measurement_tube_power     '50.0 W'
_exptl_crystal_recrystallization_method layering
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dwl_4_59
_database_code_depnum_ccdc_archive 'CCDC 2334912'
loop_
_audit_author_name
_audit_author_address
'Daniel Laorenza'
;Harvard University
United States of America
;
_audit_update_record             
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_audit_creation_date             2022-10-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis(12-crown-4)lithium tetrakis(trimethylsilylmethyl)vanadate'
_chemical_formula_moiety         'C16 H44 Si4 V, C16 H32 Li O8'
_chemical_formula_sum            'C32 H76 Li O8 Si4 V'
_chemical_formula_weight         759.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'V Si4 C32 Li O8 H60'
_chemical_oxdiff_usercomment     'purple needles'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4055(2)
_cell_length_b                   21.3852(3)
_cell_length_c                   20.4877(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.167(2)
_cell_angle_gamma                90
_cell_volume                     4420.34(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    36131
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.2180
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.794
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.078
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66678
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.100
_diffrn_reflns_theta_min         2.163
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00 -23.78   0.38   15.00    --    5.03 -40.00 -31.00   69
  2  ω     -7.00  51.14   0.38   15.00    --    5.03  40.00 122.00  153
  3  ω    -70.00   3.72   0.38   15.00    --    5.03 -19.00 120.00  194
  4  ω    -11.00  38.02   0.38   15.00    --    5.03 -99.00 -60.00  129
  5  ω    -70.00   3.72   0.38   15.00    --    5.03 -19.00-150.00  194
  6  ω    -65.00 -20.92   0.38   15.00    --    5.03 -77.00 150.00  116
  7  ω     -5.00  25.40   0.38   15.00    --    5.03  37.00-150.00   80
  8  ω     51.00  77.22   0.38   15.00    --    5.03  37.00-150.00   69
  9  ω    -23.00  21.08   0.38   15.00    --   -5.49 -99.00-150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0386607000
_diffrn_orient_matrix_UB_12      0.0115696000
_diffrn_orient_matrix_UB_13      0.0310764000
_diffrn_orient_matrix_UB_21      -0.0580398000
_diffrn_orient_matrix_UB_22      0.0120587000
_diffrn_orient_matrix_UB_23      0.0077268000
_diffrn_orient_matrix_UB_31      -0.0088539000
_diffrn_orient_matrix_UB_32      -0.0286563000
_diffrn_orient_matrix_UB_33      0.0157834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9710
_reflns_number_total             11931
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         11931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+0.9894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0828
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C13(H13A,H13B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
V1 V 0.81241(2) 0.25264(2) 0.60407(2) 0.01326(5) Uani 1 1 d . . . . .
Si1 Si 0.93400(3) 0.12078(2) 0.54011(2) 0.01598(7) Uani 1 1 d . . . . .
Si2 Si 1.03587(3) 0.24161(2) 0.76120(2) 0.01762(7) Uani 1 1 d . . . . .
Si3 Si 0.91125(3) 0.39585(2) 0.55289(2) 0.01608(7) Uani 1 1 d . . . . .
Si4 Si 0.50739(3) 0.24814(2) 0.48385(2) 0.01719(7) Uani 1 1 d . . . . .
C1 C 0.92866(12) 0.20652(5) 0.54775(6) 0.0183(2) Uani 1 1 d . . . . .
H1A H 0.900944 0.223220 0.501350 0.022 Uiso 1 1 calc R U . . .
H1B H 1.021180 0.220455 0.566151 0.022 Uiso 1 1 calc R U . . .
C2 C 1.04859(13) 0.09446(6) 0.48722(7) 0.0251(3) Uani 1 1 d . . . . .
H2A H 1.019984 0.112809 0.442160 0.038 Uiso 1 1 calc R U . . .
H2B H 1.046299 0.048755 0.483684 0.038 Uiso 1 1 calc R U . . .
H2C H 1.139140 0.108124 0.508300 0.038 Uiso 1 1 calc R U . . .
C3 C 0.76650(12) 0.08657(6) 0.50075(7) 0.0235(3) Uani 1 1 d . . . . .
H3A H 0.705030 0.096646 0.528624 0.035 Uiso 1 1 calc R U . . .
H3B H 0.774150 0.041068 0.497499 0.035 Uiso 1 1 calc R U . . .
H3C H 0.733023 0.104178 0.455620 0.035 Uiso 1 1 calc R U . . .
C4 C 0.99104(12) 0.08095(6) 0.62408(6) 0.0219(3) Uani 1 1 d . . . . .
H4A H 1.081678 0.094213 0.645567 0.033 Uiso 1 1 calc R U . . .
H4B H 0.989105 0.035528 0.617595 0.033 Uiso 1 1 calc R U . . .
H4C H 0.932064 0.092366 0.652845 0.033 Uiso 1 1 calc R U . . .
C5 C 0.87054(12) 0.22522(5) 0.70576(6) 0.0170(2) Uani 1 1 d . . . . .
H5A H 0.805110 0.243639 0.728071 0.020 Uiso 1 1 calc R U . . .
H5B H 0.858374 0.179331 0.706404 0.020 Uiso 1 1 calc R U . . .
C6 C 1.17537(14) 0.22932(8) 0.71929(8) 0.0338(3) Uani 1 1 d . . . . .
H6A H 1.172295 0.186412 0.702187 0.051 Uiso 1 1 calc R U . . .
H6B H 1.260155 0.236361 0.751984 0.051 Uiso 1 1 calc R U . . .
H6C H 1.166499 0.258784 0.681805 0.051 Uiso 1 1 calc R U . . .
C7 C 1.07219(15) 0.19029(7) 0.83786(8) 0.0346(3) Uani 1 1 d . . . . .
H7A H 1.007519 0.198639 0.864432 0.052 Uiso 1 1 calc R U . . .
H7B H 1.161658 0.199138 0.865161 0.052 Uiso 1 1 calc R U . . .
H7C H 1.066359 0.146313 0.824010 0.052 Uiso 1 1 calc R U . . .
C8 C 1.04853(15) 0.32476(6) 0.79080(8) 0.0359(4) Uani 1 1 d . . . . .
H8A H 1.024017 0.352778 0.751880 0.054 Uiso 1 1 calc R U . . .
H8B H 1.139765 0.333543 0.815760 0.054 Uiso 1 1 calc R U . . .
H8C H 0.988432 0.331460 0.820252 0.054 Uiso 1 1 calc R U . . .
C9 C 0.82465(12) 0.35148(5) 0.60565(6) 0.0184(2) Uani 1 1 d . . . . .
H9A H 0.732414 0.367255 0.595118 0.022 Uiso 1 1 calc R U . . .
H9B H 0.865426 0.363568 0.652820 0.022 Uiso 1 1 calc R U . . .
C10 C 0.83405(14) 0.38198(6) 0.46158(6) 0.0263(3) Uani 1 1 d . . . . .
H10A H 0.846769 0.338184 0.450533 0.039 Uiso 1 1 calc R U . . .
H10B H 0.875902 0.409252 0.434336 0.039 Uiso 1 1 calc R U . . .
H10C H 0.739021 0.391222 0.452014 0.039 Uiso 1 1 calc R U . . .
C11 C 1.08970(13) 0.37254(6) 0.56941(8) 0.0301(3) Uani 1 1 d . . . . .
H11A H 1.131573 0.376947 0.617530 0.045 Uiso 1 1 calc R U . . .
H11B H 1.135086 0.399535 0.543518 0.045 Uiso 1 1 calc R U . . .
H11C H 1.095885 0.328916 0.555831 0.045 Uiso 1 1 calc R U . . .
C12 C 0.90450(15) 0.48277(6) 0.56859(7) 0.0266(3) Uani 1 1 d . . . . .
H12A H 0.812215 0.496989 0.555528 0.040 Uiso 1 1 calc R U . . .
H12B H 0.956317 0.504990 0.541879 0.040 Uiso 1 1 calc R U . . .
H12C H 0.941467 0.491383 0.616494 0.040 Uiso 1 1 calc R U . . .
C13 C 0.61083(11) 0.22853(5) 0.56816(6) 0.0169(2) Uani 1 1 d . . . . .
H13A H 0.606312 0.182507 0.572306 0.020 Uiso 1 1 calc R U . . .
H13B H 0.564591 0.246229 0.600824 0.020 Uiso 1 1 calc R U . . .
C14 C 0.35045(14) 0.20082(7) 0.46244(8) 0.0320(3) Uani 1 1 d . . . . .
H14A H 0.372384 0.156206 0.466804 0.048 Uiso 1 1 calc R U . . .
H14B H 0.301820 0.209835 0.416075 0.048 Uiso 1 1 calc R U . . .
H14C H 0.295333 0.211749 0.493289 0.048 Uiso 1 1 calc R U . . .
C15 C 0.59067(14) 0.23424(6) 0.41363(7) 0.0268(3) Uani 1 1 d . . . . .
H15A H 0.674233 0.257559 0.422460 0.040 Uiso 1 1 calc R U . . .
H15B H 0.532547 0.248420 0.371051 0.040 Uiso 1 1 calc R U . . .
H15C H 0.608734 0.189492 0.410695 0.040 Uiso 1 1 calc R U . . .
C16 C 0.45694(14) 0.33274(6) 0.47914(7) 0.0268(3) Uani 1 1 d . . . . .
H16A H 0.391554 0.339343 0.505709 0.040 Uiso 1 1 calc R U . . .
H16B H 0.417959 0.344150 0.432133 0.040 Uiso 1 1 calc R U . . .
H16C H 0.535002 0.358830 0.497126 0.040 Uiso 1 1 calc R U . . .
O1 O 0.46176(8) 0.49773(4) 0.13057(4) 0.01847(17) Uani 1 1 d . . . . .
O2 O 0.45285(8) 0.39600(4) 0.21094(4) 0.01902(17) Uani 1 1 d . . . . .
O3 O 0.68374(8) 0.43926(4) 0.29371(4) 0.01878(17) Uani 1 1 d . . . . .
O4 O 0.69436(8) 0.54154(4) 0.21263(4) 0.01975(18) Uani 1 1 d . . . . .
O5 O 0.27624(8) 0.50246(4) 0.22413(4) 0.01811(17) Uani 1 1 d . . . . .
O6 O 0.44081(8) 0.46133(4) 0.34150(4) 0.01779(17) Uani 1 1 d . . . . .
O7 O 0.59645(8) 0.56423(4) 0.33687(4) 0.01895(17) Uani 1 1 d . . . . .
O8 O 0.43174(8) 0.60506(4) 0.21891(4) 0.01967(18) Uani 1 1 d . . . . .
C17 C 0.45322(13) 0.43704(6) 0.10118(6) 0.0204(2) Uani 1 1 d . . . . .
H17A H 0.542938 0.420828 0.102500 0.025 Uiso 1 1 calc R U . . .
H17B H 0.401826 0.438658 0.053658 0.025 Uiso 1 1 calc R U . . .
C18 C 0.38493(12) 0.39544(6) 0.14153(6) 0.0195(2) Uani 1 1 d . . . . .
H18A H 0.292684 0.409977 0.136483 0.023 Uiso 1 1 calc R U . . .
H18B H 0.381715 0.352152 0.124076 0.023 Uiso 1 1 calc R U . . .
C19 C 0.56400(12) 0.35487(5) 0.22730(6) 0.0207(2) Uani 1 1 d . . . . .
H19A H 0.616339 0.357874 0.193050 0.025 Uiso 1 1 calc R U . . .
H19B H 0.534184 0.311084 0.229082 0.025 Uiso 1 1 calc R U . . .
C20 C 0.64634(12) 0.37500(5) 0.29519(6) 0.0197(2) Uani 1 1 d . . . . .
H20A H 0.594884 0.369105 0.329477 0.024 Uiso 1 1 calc R U . . .
H20B H 0.726892 0.348687 0.307934 0.024 Uiso 1 1 calc R U . . .
C21 C 0.79861(12) 0.44846(6) 0.26917(7) 0.0217(3) Uani 1 1 d . . . . .
H21A H 0.790376 0.425419 0.226436 0.026 Uiso 1 1 calc R U . . .
H21B H 0.878167 0.433041 0.302321 0.026 Uiso 1 1 calc R U . . .
C22 C 0.81039(12) 0.51773(6) 0.25792(6) 0.0209(2) Uani 1 1 d . . . . .
H22A H 0.824526 0.539887 0.301532 0.025 Uiso 1 1 calc R U . . .
H22B H 0.888279 0.525670 0.239405 0.025 Uiso 1 1 calc R U . . .
C23 C 0.68901(12) 0.53060(6) 0.14351(6) 0.0204(2) Uani 1 1 d . . . . .
H23A H 0.718805 0.487602 0.136969 0.025 Uiso 1 1 calc R U . . .
H23B H 0.746616 0.560580 0.127194 0.025 Uiso 1 1 calc R U . . .
C24 C 0.54624(12) 0.53945(6) 0.10614(6) 0.0198(2) Uani 1 1 d . . . . .
H24A H 0.519177 0.583120 0.111680 0.024 Uiso 1 1 calc R U . . .
H24B H 0.536850 0.531842 0.057529 0.024 Uiso 1 1 calc R U . . .
C25 C 0.22055(12) 0.49118(6) 0.27999(6) 0.0184(2) Uani 1 1 d . . . . .
H25A H 0.128017 0.476302 0.264315 0.022 Uiso 1 1 calc R U . . .
H25B H 0.220814 0.530014 0.306325 0.022 Uiso 1 1 calc R U . . .
C26 C 0.30557(12) 0.44181(5) 0.32258(6) 0.0182(2) Uani 1 1 d . . . . .
H26A H 0.273375 0.434081 0.363509 0.022 Uiso 1 1 calc R U . . .
H26B H 0.298512 0.402210 0.296919 0.022 Uiso 1 1 calc R U . . .
C27 C 0.47107(12) 0.50222(6) 0.39810(6) 0.0193(2) Uani 1 1 d . . . . .
H27A H 0.477031 0.478462 0.440213 0.023 Uiso 1 1 calc R U . . .
H27B H 0.401378 0.534506 0.394060 0.023 Uiso 1 1 calc R U . . .
C28 C 0.60241(12) 0.53217(6) 0.39863(6) 0.0194(2) Uani 1 1 d . . . . .
H28A H 0.626308 0.562090 0.436552 0.023 Uiso 1 1 calc R U . . .
H28B H 0.672058 0.499612 0.405398 0.023 Uiso 1 1 calc R U . . .
C29 C 0.54446(12) 0.62626(5) 0.33481(6) 0.0205(2) Uani 1 1 d . . . . .
H29A H 0.609231 0.654368 0.364231 0.025 Uiso 1 1 calc R U . . .
H29B H 0.461422 0.626514 0.350227 0.025 Uiso 1 1 calc R U . . .
C30 C 0.51820(13) 0.64734(5) 0.26255(6) 0.0208(2) Uani 1 1 d . . . . .
H30A H 0.477766 0.689518 0.258180 0.025 Uiso 1 1 calc R U . . .
H30B H 0.603127 0.650097 0.249068 0.025 Uiso 1 1 calc R U . . .
C31 C 0.29485(12) 0.61470(6) 0.21582(7) 0.0203(2) Uani 1 1 d . . . . .
H31A H 0.261023 0.651465 0.187436 0.024 Uiso 1 1 calc R U . . .
H31B H 0.281667 0.621933 0.261467 0.024 Uiso 1 1 calc R U . . .
C32 C 0.22324(12) 0.55614(6) 0.18557(6) 0.0199(2) Uani 1 1 d . . . . .
H32A H 0.127771 0.560025 0.184104 0.024 Uiso 1 1 calc R U . . .
H32B H 0.232104 0.551116 0.138835 0.024 Uiso 1 1 calc R U . . .
Li1 Li 0.5034(2) 0.50004(9) 0.24693(11) 0.0211(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
V1 C1 2.1097(12) . ?
V1 C5 2.1055(12) . ?
V1 C9 2.1173(11) . ?
V1 C13 2.1099(12) . ?
Si1 C1 1.8423(12) . ?
Si1 C2 1.8828(13) . ?
Si1 C3 1.8801(13) . ?
Si1 C4 1.8809(13) . ?
Si2 C5 1.8483(12) . ?
Si2 C6 1.8771(15) . ?
Si2 C7 1.8771(14) . ?
Si2 C8 1.8729(14) . ?
Si3 C9 1.8324(12) . ?
Si3 C10 1.8702(13) . ?
Si3 C11 1.8718(14) . ?
Si3 C12 1.8907(13) . ?
Si4 C13 1.8461(12) . ?
Si4 C14 1.8795(14) . ?
Si4 C15 1.8760(15) . ?
Si4 C16 1.8796(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 C17 1.4244(14) . ?
O1 C24 1.4263(14) . ?
O1 Li1 2.317(2) . ?
O2 C18 1.4247(15) . ?
O2 C19 1.4261(14) . ?
O2 Li1 2.362(2) . ?
O3 C20 1.4307(14) . ?
O3 C21 1.4192(15) . ?
O3 Li1 2.291(2) . ?
O4 C22 1.4248(14) . ?
O4 C23 1.4228(15) . ?
O4 Li1 2.432(2) . ?
O5 C25 1.4242(14) . ?
O5 C32 1.4259(14) . ?
O5 Li1 2.295(2) . ?
O6 C26 1.4275(14) . ?
O6 C27 1.4248(14) . ?
O6 Li1 2.341(2) . ?
O7 C28 1.4271(15) . ?
O7 C29 1.4293(14) . ?
O7 Li1 2.312(2) . ?
O8 C30 1.4257(15) . ?
O8 C31 1.4253(14) . ?
O8 Li1 2.392(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.5057(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.5069(17) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5087(17) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.5074(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.5102(17) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.5070(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.5072(18) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5104(17) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?

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
C1 V1 C9 115.77(5) . . ?
C1 V1 C13 110.44(5) . . ?
C5 V1 C1 110.28(5) . . ?
C5 V1 C9 105.14(5) . . ?
C5 V1 C13 107.30(5) . . ?
C13 V1 C9 107.47(5) . . ?
C1 Si1 C2 112.51(6) . . ?
C1 Si1 C3 112.31(6) . . ?
C1 Si1 C4 112.48(6) . . ?
C3 Si1 C2 106.74(6) . . ?
C3 Si1 C4 105.55(6) . . ?
C4 Si1 C2 106.77(6) . . ?
C5 Si2 C6 113.58(6) . . ?
C5 Si2 C7 111.71(6) . . ?
C5 Si2 C8 111.11(6) . . ?
C6 Si2 C7 106.32(7) . . ?
C8 Si2 C6 106.26(8) . . ?
C8 Si2 C7 107.48(7) . . ?
C9 Si3 C10 110.80(6) . . ?
C9 Si3 C11 111.39(6) . . ?
C9 Si3 C12 111.39(6) . . ?
C10 Si3 C11 107.63(7) . . ?
C10 Si3 C12 107.54(6) . . ?
C11 Si3 C12 107.92(6) . . ?
C13 Si4 C14 111.73(6) . . ?
C13 Si4 C15 114.11(6) . . ?
C13 Si4 C16 110.99(6) . . ?
C14 Si4 C16 106.89(7) . . ?
C15 Si4 C14 105.89(7) . . ?
C15 Si4 C16 106.78(6) . . ?
V1 C1 H1A 106.6 . . ?
V1 C1 H1B 106.6 . . ?
Si1 C1 V1 123.03(6) . . ?
Si1 C1 H1A 106.6 . . ?
Si1 C1 H1B 106.6 . . ?
H1A C1 H1B 106.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
V1 C5 H5A 106.4 . . ?
V1 C5 H5B 106.4 . . ?
Si2 C5 V1 123.65(6) . . ?
Si2 C5 H5A 106.4 . . ?
Si2 C5 H5B 106.4 . . ?
H5A C5 H5B 106.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
V1 C9 H9A 106.6 . . ?
V1 C9 H9B 106.6 . . ?
Si3 C9 V1 122.98(6) . . ?
Si3 C9 H9A 106.6 . . ?
Si3 C9 H9B 106.6 . . ?
H9A C9 H9B 106.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
V1 C13 H13A 106.1 . . ?
V1 C13 H13B 106.1 . . ?
Si4 C13 V1 124.96(6) . . ?
Si4 C13 H13A 106.1 . . ?
Si4 C13 H13B 106.1 . . ?
H13A C13 H13B 106.3 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 O1 C24 113.68(9) . . ?
C17 O1 Li1 115.53(9) . . ?
C24 O1 Li1 111.82(9) . . ?
C18 O2 C19 113.90(9) . . ?
C18 O2 Li1 109.73(8) . . ?
C19 O2 Li1 113.69(8) . . ?
C20 O3 Li1 110.77(9) . . ?
C21 O3 C20 113.43(9) . . ?
C21 O3 Li1 116.61(9) . . ?
C22 O4 Li1 107.67(9) . . ?
C23 O4 C22 114.21(9) . . ?
C23 O4 Li1 113.07(8) . . ?
C25 O5 C32 113.79(9) . . ?
C25 O5 Li1 115.72(9) . . ?
C32 O5 Li1 111.73(9) . . ?
C26 O6 Li1 109.51(8) . . ?
C27 O6 C26 114.03(9) . . ?
C27 O6 Li1 113.94(8) . . ?
C28 O7 C29 113.95(9) . . ?
C28 O7 Li1 109.90(8) . . ?
C29 O7 Li1 116.48(9) . . ?
C30 O8 Li1 109.47(8) . . ?
C31 O8 C30 113.99(9) . . ?
C31 O8 Li1 113.32(8) . . ?
O1 C17 H17A 110.3 . . ?
O1 C17 H17B 110.3 . . ?
O1 C17 C18 107.17(10) . . ?
H17A C17 H17B 108.5 . . ?
C18 C17 H17A 110.3 . . ?
C18 C17 H17B 110.3 . . ?
O2 C18 C17 110.95(10) . . ?
O2 C18 H18A 109.4 . . ?
O2 C18 H18B 109.4 . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
O2 C19 H19A 110.4 . . ?
O2 C19 H19B 110.4 . . ?
O2 C19 C20 106.62(9) . . ?
H19A C19 H19B 108.6 . . ?
C20 C19 H19A 110.4 . . ?
C20 C19 H19B 110.4 . . ?
O3 C20 C19 110.54(10) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
O3 C21 H21A 110.3 . . ?
O3 C21 H21B 110.3 . . ?
O3 C21 C22 107.29(10) . . ?
H21A C21 H21B 108.5 . . ?
C22 C21 H21A 110.3 . . ?
C22 C21 H21B 110.3 . . ?
O4 C22 C21 111.27(10) . . ?
O4 C22 H22A 109.4 . . ?
O4 C22 H22B 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
O4 C23 H23A 110.5 . . ?
O4 C23 H23B 110.5 . . ?
O4 C23 C24 106.18(9) . . ?
H23A C23 H23B 108.7 . . ?
C24 C23 H23A 110.5 . . ?
C24 C23 H23B 110.5 . . ?
O1 C24 C23 111.02(10) . . ?
O1 C24 H24A 109.4 . . ?
O1 C24 H24B 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
O5 C25 H25A 110.4 . . ?
O5 C25 H25B 110.4 . . ?
O5 C25 C26 106.66(9) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
O6 C26 C25 110.59(9) . . ?
O6 C26 H26A 109.5 . . ?
O6 C26 H26B 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
O6 C27 H27A 110.4 . . ?
O6 C27 H27B 110.4 . . ?
O6 C27 C28 106.63(9) . . ?
H27A C27 H27B 108.6 . . ?
C28 C27 H27A 110.4 . . ?
C28 C27 H27B 110.4 . . ?
O7 C28 C27 110.81(10) . . ?
O7 C28 H28A 109.5 . . ?
O7 C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
O7 C29 H29A 110.4 . . ?
O7 C29 H29B 110.4 . . ?
O7 C29 C30 106.44(10) . . ?
H29A C29 H29B 108.6 . . ?
C30 C29 H29A 110.4 . . ?
C30 C29 H29B 110.4 . . ?
O8 C30 C29 111.17(10) . . ?
O8 C30 H30A 109.4 . . ?
O8 C30 H30B 109.4 . . ?
C29 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
O8 C31 H31A 110.4 . . ?
O8 C31 H31B 110.4 . . ?
O8 C31 C32 106.60(9) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.4 . . ?
C32 C31 H31B 110.4 . . ?
O5 C32 C31 110.80(10) . . ?
O5 C32 H32A 109.5 . . ?
O5 C32 H32B 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
O1 Li1 O2 71.79(7) . . ?
O1 Li1 O4 70.77(7) . . ?
O1 Li1 O6 145.51(10) . . ?
O1 Li1 O8 78.71(7) . . ?
O2 Li1 O4 112.88(9) . . ?
O2 Li1 O8 140.99(10) . . ?
O3 Li1 O1 110.25(9) . . ?
O3 Li1 O2 72.14(6) . . ?
O3 Li1 O4 71.60(7) . . ?
O3 Li1 O5 142.68(10) . . ?
O3 Li1 O6 79.54(7) . . ?
O3 Li1 O7 82.12(7) . . ?
O3 Li1 O8 143.94(10) . . ?
O5 Li1 O1 82.37(7) . . ?
O5 Li1 O2 79.53(7) . . ?
O5 Li1 O4 143.77(10) . . ?
O5 Li1 O6 72.25(7) . . ?
O5 Li1 O7 111.01(9) . . ?
O5 Li1 O8 71.64(7) . . ?
O6 Li1 O2 80.77(7) . . ?
O6 Li1 O4 141.32(10) . . ?
O6 Li1 O8 113.41(9) . . ?
O7 Li1 O1 140.28(10) . . ?
O7 Li1 O2 145.68(10) . . ?
O7 Li1 O4 78.53(7) . . ?
O7 Li1 O6 72.38(7) . . ?
O7 Li1 O8 71.27(6) . . ?
O8 Li1 O4 79.44(7) . . ?

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
C2 Si1 C1 V1 -179.36(7) . . . . ?
C3 Si1 C1 V1 60.17(9) . . . . ?
C4 Si1 C1 V1 -58.73(9) . . . . ?
C6 Si2 C5 V1 -41.87(10) . . . . ?
C7 Si2 C5 V1 -162.12(8) . . . . ?
C8 Si2 C5 V1 77.87(9) . . . . ?
C10 Si3 C9 V1 61.31(9) . . . . ?
C11 Si3 C9 V1 -58.47(9) . . . . ?
C12 Si3 C9 V1 -179.02(7) . . . . ?
C14 Si4 C13 V1 164.50(8) . . . . ?
C15 Si4 C13 V1 44.41(9) . . . . ?
C16 Si4 C13 V1 -76.30(9) . . . . ?
O1 C17 C18 O2 -55.95(13) . . . . ?
O2 C19 C20 O3 -57.00(13) . . . . ?
O3 C21 C22 O4 -57.31(13) . . . . ?
O4 C23 C24 O1 -58.46(12) . . . . ?
O5 C25 C26 O6 56.11(12) . . . . ?
O6 C27 C28 O7 57.48(12) . . . . ?
O7 C29 C30 O8 56.31(13) . . . . ?
O8 C31 C32 O5 56.90(13) . . . . ?
C17 O1 C24 C23 -83.83(12) . . . . ?
C18 O2 C19 C20 163.26(10) . . . . ?
C19 O2 C18 C17 -82.19(12) . . . . ?
C20 O3 C21 C22 169.32(9) . . . . ?
C21 O3 C20 C19 -84.05(12) . . . . ?
C22 O4 C23 C24 162.24(10) . . . . ?
C23 O4 C22 C21 -80.31(13) . . . . ?
C24 O1 C17 C18 168.62(9) . . . . ?
C25 O5 C32 C31 84.92(12) . . . . ?
C26 O6 C27 C28 -164.12(9) . . . . ?
C27 O6 C26 C25 81.90(12) . . . . ?
C28 O7 C29 C30 -168.16(10) . . . . ?
C29 O7 C28 C27 84.23(12) . . . . ?
C30 O8 C31 C32 -163.43(10) . . . . ?
C31 O8 C30 C29 81.84(12) . . . . ?
C32 O5 C25 C26 -168.75(9) . . . . ?
Li1 O1 C17 C18 37.38(13) . . . . ?
Li1 O1 C24 C23 49.21(12) . . . . ?
Li1 O2 C18 C17 46.54(12) . . . . ?
Li1 O2 C19 C20 36.56(13) . . . . ?
Li1 O3 C20 C19 49.29(12) . . . . ?
Li1 O3 C21 C22 38.83(13) . . . . ?
Li1 O4 C22 C21 46.13(12) . . . . ?
Li1 O4 C23 C24 38.65(12) . . . . ?
Li1 O5 C25 C26 -37.34(12) . . . . ?
Li1 O5 C32 C31 -48.41(12) . . . . ?
Li1 O6 C26 C25 -47.10(11) . . . . ?
Li1 O6 C27 C28 -37.39(12) . . . . ?
Li1 O7 C28 C27 -48.59(12) . . . . ?
Li1 O7 C29 C30 -38.55(13) . . . . ?
Li1 O8 C30 C29 -46.25(12) . . . . ?
Li1 O8 C31 C32 -37.34(12) . . . . ?

_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.380
_exptl_crystal_recrystallization_method layering
_chemical_properties_physical    
Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_al_otolyl_4_lithf_4
_database_code_depnum_ccdc_archive 'CCDC 2334910'
loop_
_audit_author_name
_audit_author_address
'Daniel Laorenza'
;Harvard University
United States of America
;
_audit_update_record             
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'tetrakis(tetrahydrofuran)lithium tetrakis(o-tolyl)aluminate'
_chemical_formula_moiety         'C28 H28 Al, C16 H32 Li O4'
_chemical_formula_sum            'C44 H60 Al Li O4'
_chemical_formula_weight         686.84
_chemical_melting_point          ?
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'
Al Al 0.2130 0.2455 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.461(6)
_cell_length_b                   16.903(11)
_cell_length_c                   22.031(10)
_cell_angle_alpha                70.41(4)
_cell_angle_beta                 86.22(4)
_cell_angle_gamma                85.05(5)
_cell_volume                     4003(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18236
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.51
_cell_measurement_theta_min      5.50
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.6178
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 2 2 0.0607
30 3 2 0.1267
3 10 6 0.6388
-1 1 10 2.9855
-8 -30 -7 0.7347
-30 -2 -3 0.0639
-15 -2 -3 0.1102
-30 6 1 0.1822
-30 -7 -3 0.1731
-5 -10 -6 0.4546
11 30 9 0.6117

_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51576
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.796
_diffrn_reflns_theta_min         2.781
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details      
;
 3817 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7669
_reflns_number_total             14313
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14313
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      0.795
_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)+(0.0520P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1026
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C84-C83 \\sim C84-C82
 with sigma of 0.02
 C81-C83 \\sim C81-C82
 with sigma of 0.02
3. Others
 Fixed Sof: H81A(0.5) H81B(0.5) H81C(0.5) H81D(0.5) H84A(0.5) H84B(0.5)
 H84C(0.5) H84D(0.5) C83(0.5) H83A(0.5) H83B(0.5) C82(0.5) H82A(0.5) H82B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80A,H80B), C81(H81A,H81B), C81(H81C,H81D), C84(H84A,H84B), C84(H84C,H84D),
  C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C83(H83A,H83B), C82(H82A,H82B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Al1 Al 0.33706(5) 0.27391(4) 0.97381(3) 0.02884(15) Uani 1 1 d . . . . .
C1 C 0.21673(18) 0.20306(13) 0.95792(10) 0.0302(5) Uani 1 1 d . . . . .
C2 C 0.21810(18) 0.11408(14) 0.98488(10) 0.0332(5) Uani 1 1 d . . . . .
C3 C 0.1335(2) 0.07062(14) 0.96912(11) 0.0390(6) Uani 1 1 d . . . . .
H3 H 0.134714 0.011183 0.988496 0.047 Uiso 1 1 calc R U . . .
C4 C 0.0481(2) 0.11147(15) 0.92622(12) 0.0433(6) Uani 1 1 d . . . . .
H4 H -0.008463 0.080451 0.916058 0.052 Uiso 1 1 calc R U . . .
C5 C 0.04539(19) 0.19784(14) 0.89810(12) 0.0409(6) Uani 1 1 d . . . . .
H5 H -0.012643 0.226994 0.868203 0.049 Uiso 1 1 calc R U . . .
C6 C 0.12871(18) 0.24127(14) 0.91422(10) 0.0343(5) Uani 1 1 d . . . . .
H6 H 0.125990 0.300673 0.894385 0.041 Uiso 1 1 calc R U . . .
C7 C 0.3118(2) 0.06438(14) 1.03015(11) 0.0412(6) Uani 1 1 d . . . . .
H7A H 0.385223 0.092613 1.018168 0.062 Uiso 1 1 calc R U . . .
H7B H 0.323880 0.007631 1.027242 0.062 Uiso 1 1 calc R U . . .
H7C H 0.287272 0.060618 1.074432 0.062 Uiso 1 1 calc R U . . .
C8 C 0.34241(18) 0.26020(13) 1.06809(10) 0.0314(5) Uani 1 1 d . . . . .
C9 C 0.26261(19) 0.21074(14) 1.11295(10) 0.0366(5) Uani 1 1 d . . . . .
H9 H 0.209223 0.182365 1.097735 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2570(2) 0.20087(15) 1.17774(11) 0.0425(6) Uani 1 1 d . . . . .
H10 H 0.201094 0.166693 1.205981 0.051 Uiso 1 1 calc R U . . .
C11 C 0.3339(2) 0.24136(15) 1.20105(11) 0.0458(6) Uani 1 1 d . . . . .
H11 H 0.332154 0.234765 1.245648 0.055 Uiso 1 1 calc R U . . .
C12 C 0.4133(2) 0.29143(15) 1.15890(11) 0.0435(6) Uani 1 1 d . . . . .
H12 H 0.466106 0.319299 1.174955 0.052 Uiso 1 1 calc R U . . .
C13 C 0.41783(19) 0.30207(14) 1.09341(11) 0.0358(5) Uani 1 1 d . . . . .
C14 C 0.5054(2) 0.35923(15) 1.04946(11) 0.0462(6) Uani 1 1 d . . . . .
H14A H 0.566933 0.325317 1.034536 0.069 Uiso 1 1 calc R U . . .
H14B H 0.540515 0.390413 1.073128 0.069 Uiso 1 1 calc R U . . .
H14C H 0.465385 0.398979 1.012264 0.069 Uiso 1 1 calc R U . . .
C15 C 0.29472(18) 0.39718(13) 0.92552(10) 0.0298(5) Uani 1 1 d . . . . .
C16 C 0.37522(19) 0.44521(13) 0.87973(10) 0.0348(5) Uani 1 1 d . . . . .
H16 H 0.448540 0.418391 0.872439 0.042 Uiso 1 1 calc R U . . .
C17 C 0.3527(2) 0.52983(14) 0.84472(11) 0.0394(6) Uani 1 1 d . . . . .
H17 H 0.409474 0.559510 0.814042 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2472(2) 0.57049(14) 0.85484(11) 0.0395(6) Uani 1 1 d . . . . .
H18 H 0.230307 0.628206 0.830978 0.047 Uiso 1 1 calc R U . . .
C19 C 0.1667(2) 0.52621(13) 0.90003(11) 0.0366(5) Uani 1 1 d . . . . .
H19 H 0.094203 0.554107 0.907215 0.044 Uiso 1 1 calc R U . . .
C20 C 0.18940(19) 0.44120(13) 0.93549(10) 0.0319(5) Uani 1 1 d . . . . .
C21 C 0.09919(19) 0.39832(14) 0.98622(11) 0.0407(6) Uani 1 1 d . . . . .
H21A H 0.073812 0.349803 0.976935 0.061 Uiso 1 1 calc R U . . .
H21B H 0.031548 0.438061 0.985955 0.061 Uiso 1 1 calc R U . . .
H21C H 0.133630 0.379240 1.028705 0.061 Uiso 1 1 calc R U . . .
C22 C 0.49324(18) 0.23594(13) 0.94112(10) 0.0310(5) Uani 1 1 d . . . . .
C23 C 0.58131(19) 0.19560(13) 0.98464(11) 0.0357(5) Uani 1 1 d . . . . .
H23 H 0.566384 0.188948 1.028948 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6891(2) 0.16499(14) 0.96603(12) 0.0425(6) Uani 1 1 d . . . . .
H24 H 0.745009 0.136505 0.997397 0.051 Uiso 1 1 calc R U . . .
C25 C 0.7144(2) 0.17609(14) 0.90218(12) 0.0435(6) Uani 1 1 d . . . . .
H25 H 0.788933 0.157265 0.888723 0.052 Uiso 1 1 calc R U . . .
C26 C 0.63043(19) 0.21486(14) 0.85763(12) 0.0391(6) Uani 1 1 d . . . . .
H26 H 0.647827 0.222410 0.813360 0.047 Uiso 1 1 calc R U . . .
C27 C 0.52051(18) 0.24321(13) 0.87631(11) 0.0316(5) Uani 1 1 d . . . . .
C28 C 0.43093(19) 0.27838(14) 0.82533(10) 0.0384(6) Uani 1 1 d . . . . .
H28A H 0.352849 0.280373 0.845995 0.058 Uiso 1 1 calc R U . . .
H28B H 0.432220 0.242322 0.798492 0.058 Uiso 1 1 calc R U . . .
H28C H 0.449420 0.335344 0.798334 0.058 Uiso 1 1 calc R U . . .
Al2 Al 0.37281(5) 0.77720(4) 0.47979(3) 0.02807(15) Uani 1 1 d . . . . .
C29 C 0.24667(17) 0.70386(13) 0.47298(10) 0.0292(5) Uani 1 1 d . . . . .
C30 C 0.13972(18) 0.74087(14) 0.44599(10) 0.0325(5) Uani 1 1 d . . . . .
H30 H 0.129925 0.800551 0.429441 0.039 Uiso 1 1 calc R U . . .
C31 C 0.04758(18) 0.69526(14) 0.44213(11) 0.0361(5) Uani 1 1 d . . . . .
H31 H -0.023356 0.723351 0.423437 0.043 Uiso 1 1 calc R U . . .
C32 C 0.05984(19) 0.60868(14) 0.46569(11) 0.0384(6) Uani 1 1 d . . . . .
H32 H -0.003287 0.576525 0.464231 0.046 Uiso 1 1 calc R U . . .
C33 C 0.16461(19) 0.56883(14) 0.49148(11) 0.0366(5) Uani 1 1 d . . . . .
H33 H 0.173506 0.509081 0.506840 0.044 Uiso 1 1 calc R U . . .
C34 C 0.25758(18) 0.61499(13) 0.49531(10) 0.0328(5) Uani 1 1 d . . . . .
C35 C 0.37050(19) 0.56807(13) 0.52313(12) 0.0416(6) Uani 1 1 d . . . . .
H35A H 0.432593 0.578520 0.489162 0.062 Uiso 1 1 calc R U . . .
H35B H 0.359495 0.507617 0.540634 0.062 Uiso 1 1 calc R U . . .
H35C H 0.392690 0.587617 0.557637 0.062 Uiso 1 1 calc R U . . .
C36 C 0.38555(17) 0.76413(13) 0.57384(10) 0.0303(5) Uani 1 1 d . . . . .
C37 C 0.31732(18) 0.70666(13) 0.62039(10) 0.0339(5) Uani 1 1 d . . . . .
H37 H 0.271552 0.672078 0.606587 0.041 Uiso 1 1 calc R U . . .
C38 C 0.31287(19) 0.69750(15) 0.68497(11) 0.0402(6) Uani 1 1 d . . . . .
H38 H 0.265893 0.656959 0.714567 0.048 Uiso 1 1 calc R U . . .
C39 C 0.3770(2) 0.74749(15) 0.70638(11) 0.0420(6) Uani 1 1 d . . . . .
H39 H 0.374312 0.742299 0.750733 0.050 Uiso 1 1 calc R U . . .
C40 C 0.4451(2) 0.80528(15) 0.66223(11) 0.0413(6) Uani 1 1 d . . . . .
H40 H 0.490007 0.839569 0.676830 0.050 Uiso 1 1 calc R U . . .
C41 C 0.44989(18) 0.81468(13) 0.59702(11) 0.0339(5) Uani 1 1 d . . . . .
C42 C 0.5251(2) 0.87990(14) 0.55144(11) 0.0431(6) Uani 1 1 d . . . . .
H42A H 0.597025 0.852040 0.539338 0.065 Uiso 1 1 calc R U . . .
H42B H 0.545306 0.919097 0.572693 0.065 Uiso 1 1 calc R U . . .
H42C H 0.481878 0.910948 0.512691 0.065 Uiso 1 1 calc R U . . .
C43 C 0.52650(17) 0.74105(13) 0.44296(10) 0.0293(5) Uani 1 1 d . . . . .
C44 C 0.62297(18) 0.71340(13) 0.48304(11) 0.0321(5) Uani 1 1 d . . . . .
H44 H 0.613994 0.714667 0.525883 0.038 Uiso 1 1 calc R U . . .
C45 C 0.73066(19) 0.68434(14) 0.46290(11) 0.0378(6) Uani 1 1 d . . . . .
H45 H 0.793685 0.666683 0.491416 0.045 Uiso 1 1 calc R U . . .
C46 C 0.74496(19) 0.68144(14) 0.40120(11) 0.0393(6) Uani 1 1 d . . . . .
H46 H 0.818039 0.661759 0.386671 0.047 Uiso 1 1 calc R U . . .
C47 C 0.65191(19) 0.70744(14) 0.36041(11) 0.0387(6) Uani 1 1 d . . . . .
H47 H 0.661941 0.705544 0.317763 0.046 Uiso 1 1 calc R U . . .
C48 C 0.54396(18) 0.73630(14) 0.38075(11) 0.0338(5) Uani 1 1 d . . . . .
C49 C 0.44620(19) 0.76086(15) 0.33365(11) 0.0391(6) Uani 1 1 d . . . . .
H49A H 0.371535 0.767224 0.356477 0.059 Uiso 1 1 calc R U . . .
H49B H 0.442150 0.716980 0.314101 0.059 Uiso 1 1 calc R U . . .
H49C H 0.461588 0.814280 0.299845 0.059 Uiso 1 1 calc R U . . .
C50 C 0.32133(17) 0.89824(13) 0.42956(10) 0.0285(5) Uani 1 1 d . . . . .
C51 C 0.38006(18) 0.94160(13) 0.37179(10) 0.0322(5) Uani 1 1 d . . . . .
H51 H 0.448257 0.914703 0.358414 0.039 Uiso 1 1 calc R U . . .
C52 C 0.34322(19) 1.02226(14) 0.33306(10) 0.0362(5) Uani 1 1 d . . . . .
H52 H 0.385644 1.049323 0.294095 0.043 Uiso 1 1 calc R U . . .
C53 C 0.2451(2) 1.06255(14) 0.35151(11) 0.0381(6) Uani 1 1 d . . . . .
H53 H 0.217955 1.117102 0.324898 0.046 Uiso 1 1 calc R U . . .
C54 C 0.18646(19) 1.02326(13) 0.40877(11) 0.0369(5) Uani 1 1 d . . . . .
H54 H 0.119538 1.051614 0.421942 0.044 Uiso 1 1 calc R U . . .
C55 C 0.22344(18) 0.94246(13) 0.44796(10) 0.0318(5) Uani 1 1 d . . . . .
C56 C 0.15815(19) 0.90379(14) 0.51152(10) 0.0378(5) Uani 1 1 d . . . . .
H56A H 0.138394 0.847037 0.515250 0.057 Uiso 1 1 calc R U . . .
H56B H 0.086034 0.938602 0.513564 0.057 Uiso 1 1 calc R U . . .
H56C H 0.207661 0.900621 0.546977 0.057 Uiso 1 1 calc R U . . .
O1 O 0.79316(14) 0.49903(10) 0.82195(8) 0.0461(4) Uani 1 1 d . . . . .
O2 O 0.97862(13) 0.47995(10) 0.72167(7) 0.0462(4) Uani 1 1 d . . . . .
O3 O 0.86545(14) 0.66028(10) 0.69544(8) 0.0463(4) Uani 1 1 d . . . . .
O4 O 0.71310(14) 0.52856(12) 0.68605(9) 0.0550(5) Uani 1 1 d . . . . .
C57 C 0.7471(2) 0.41665(16) 0.84475(13) 0.0528(7) Uani 1 1 d . . . . .
H57A H 0.794704 0.377506 0.826647 0.063 Uiso 1 1 calc R U . . .
H57B H 0.665036 0.420065 0.832147 0.063 Uiso 1 1 calc R U . . .
C58 C 0.7538(3) 0.38762(16) 0.91645(13) 0.0592(8) Uani 1 1 d . . . . .
H58A H 0.830995 0.358539 0.930501 0.071 Uiso 1 1 calc R U . . .
H58B H 0.691213 0.349603 0.937770 0.071 Uiso 1 1 calc R U . . .
C59 C 0.7361(3) 0.46953(18) 0.93017(13) 0.0651(8) Uani 1 1 d . . . . .
H59A H 0.766882 0.464110 0.972415 0.078 Uiso 1 1 calc R U . . .
H59B H 0.652243 0.489581 0.929308 0.078 Uiso 1 1 calc R U . . .
C60 C 0.8064(2) 0.52738(16) 0.87515(12) 0.0484(6) Uani 1 1 d . . . . .
H60A H 0.775462 0.586640 0.865428 0.058 Uiso 1 1 calc R U . . .
H60B H 0.889913 0.522785 0.885717 0.058 Uiso 1 1 calc R U . . .
C61 C 1.0513(2) 0.43411(19) 0.77364(13) 0.0682(9) Uani 1 1 d . . . . .
H61A H 1.018569 0.379628 0.798133 0.082 Uiso 1 1 calc R U . . .
H61B H 1.055979 0.466487 0.803331 0.082 Uiso 1 1 calc R U . . .
C62 C 1.1698(2) 0.41965(19) 0.74597(13) 0.0619(8) Uani 1 1 d . . . . .
H62A H 1.181351 0.362075 0.743483 0.074 Uiso 1 1 calc R U . . .
H62B H 1.231738 0.427896 0.772106 0.074 Uiso 1 1 calc R U . . .
C63 C 1.1709(2) 0.48466(16) 0.67978(13) 0.0511(7) Uani 1 1 d . . . . .
H63A H 1.195464 0.538958 0.680715 0.061 Uiso 1 1 calc R U . . .
H63B H 1.223527 0.465489 0.649237 0.061 Uiso 1 1 calc R U . . .
C64 C 1.0451(2) 0.49175(18) 0.66241(12) 0.0538(7) Uani 1 1 d . . . . .
H64A H 1.024416 0.547801 0.630783 0.065 Uiso 1 1 calc R U . . .
H64B H 1.030385 0.448011 0.643704 0.065 Uiso 1 1 calc R U . . .
C65 C 0.9645(2) 0.69439(16) 0.71222(13) 0.0536(7) Uani 1 1 d . . . . .
H65A H 1.030419 0.650991 0.724339 0.064 Uiso 1 1 calc R U . . .
H65B H 0.943321 0.714737 0.748994 0.064 Uiso 1 1 calc R U . . .
C66 C 0.9983(2) 0.76681(16) 0.65271(14) 0.0619(8) Uani 1 1 d . . . . .
H66A H 0.968539 0.821548 0.656932 0.074 Uiso 1 1 calc R U . . .
H66B H 1.084520 0.766477 0.645491 0.074 Uiso 1 1 calc R U . . .
C67 C 0.9415(3) 0.75128(19) 0.59884(15) 0.0740(9) Uani 1 1 d . . . . .
H67A H 0.922793 0.804591 0.563620 0.089 Uiso 1 1 calc R U . . .
H67B H 0.992233 0.713032 0.581214 0.089 Uiso 1 1 calc R U . . .
C68 C 0.8327(3) 0.71119(17) 0.63141(12) 0.0598(8) Uani 1 1 d . . . . .
H68A H 0.769903 0.754549 0.633056 0.072 Uiso 1 1 calc R U . . .
H68B H 0.804574 0.675967 0.608177 0.072 Uiso 1 1 calc R U . . .
C69 C 0.7084(3) 0.4655(2) 0.65595(17) 0.0833(11) Uani 1 1 d . . . . .
H69A H 0.725672 0.408508 0.687170 0.100 Uiso 1 1 calc R U . . .
H69B H 0.765758 0.474841 0.619026 0.100 Uiso 1 1 calc R U . . .
C70 C 0.5894(3) 0.4744(2) 0.6342(2) 0.0927(13) Uani 1 1 d . . . . .
H70A H 0.564288 0.419930 0.634080 0.111 Uiso 1 1 calc R U . . .
H70B H 0.582789 0.516104 0.590371 0.111 Uiso 1 1 calc R U . . .
C71 C 0.5161(2) 0.5051(2) 0.68378(15) 0.0731(10) Uani 1 1 d . . . . .
H71A H 0.440963 0.534518 0.666153 0.088 Uiso 1 1 calc R U . . .
H71B H 0.500076 0.458005 0.723908 0.088 Uiso 1 1 calc R U . . .
C72 C 0.5956(2) 0.56410(18) 0.69480(14) 0.0596(8) Uani 1 1 d . . . . .
H72A H 0.582493 0.621385 0.663284 0.072 Uiso 1 1 calc R U . . .
H72B H 0.582751 0.566977 0.738912 0.072 Uiso 1 1 calc R U . . .
Li1 Li 0.8370(3) 0.5433(3) 0.7328(2) 0.0446(10) Uani 1 1 d . . . . .
O5 O -0.18614(13) 0.99957(11) 0.30873(8) 0.0488(4) Uani 1 1 d . . . . .
O6 O -0.01181(14) 0.92481(10) 0.22634(8) 0.0468(4) Uani 1 1 d . . . . .
O7 O -0.08452(14) 1.10876(10) 0.16849(8) 0.0433(4) Uani 1 1 d . . . . .
O8 O -0.28719(13) 0.99563(10) 0.18716(8) 0.0468(4) Uani 1 1 d . . . . .
C73 C -0.2896(2) 0.9646(2) 0.34413(14) 0.0699(9) Uani 1 1 d . . . . .
H73A H -0.310931 0.917187 0.331198 0.084 Uiso 1 1 calc R U . . .
H73B H -0.355980 1.007865 0.335708 0.084 Uiso 1 1 calc R U . . .
C74 C -0.2625(3) 0.9348(2) 0.41338(14) 0.0791(10) Uani 1 1 d . . . . .
H74A H -0.294476 0.879517 0.436180 0.095 Uiso 1 1 calc R U . . .
H74B H -0.295298 0.975637 0.434453 0.095 Uiso 1 1 calc R U . . .
C75 C -0.1321(3) 0.92791(19) 0.41301(15) 0.0828(11) Uani 1 1 d . . . . .
H75A H -0.099862 0.872784 0.410498 0.099 Uiso 1 1 calc R U . . .
H75B H -0.103220 0.935835 0.451818 0.099 Uiso 1 1 calc R U . . .
C76 C -0.1011(2) 0.9980(2) 0.35344(13) 0.0623(8) Uani 1 1 d . . . . .
H76A H -0.105204 1.052089 0.361949 0.075 Uiso 1 1 calc R U . . .
H76B H -0.021040 0.987161 0.336853 0.075 Uiso 1 1 calc R U . . .
C77 C -0.0149(2) 0.83623(15) 0.26199(13) 0.0570(7) Uani 1 1 d . . . . .
H77A H -0.060805 0.808460 0.239365 0.068 Uiso 1 1 calc R U . . .
H77B H -0.051060 0.827474 0.305611 0.068 Uiso 1 1 calc R U . . .
C78 C 0.1114(2) 0.80080(17) 0.26632(13) 0.0596(8) Uani 1 1 d . . . . .
H78A H 0.124002 0.754087 0.307337 0.072 Uiso 1 1 calc R U . . .
H78B H 0.135238 0.780494 0.229799 0.072 Uiso 1 1 calc R U . . .
C79 C 0.1769(2) 0.87550(18) 0.26327(13) 0.0621(8) Uani 1 1 d . . . . .
H79A H 0.176679 0.882800 0.306021 0.075 Uiso 1 1 calc R U . . .
H79B H 0.258867 0.870102 0.247173 0.075 Uiso 1 1 calc R U . . .
C80 C 0.1083(2) 0.94653(17) 0.21670(13) 0.0521(7) Uani 1 1 d . . . . .
H80A H 0.116171 0.999768 0.225112 0.063 Uiso 1 1 calc R U . . .
H80B H 0.136566 0.953530 0.171880 0.063 Uiso 1 1 calc R U . . .
C81 C -0.1150(3) 1.19183(18) 0.17065(17) 0.0797(10) Uani 1 1 d D . . . .
H81A H -0.201302 1.202282 0.172536 0.096 Uiso 0.5 1 calc R U P A 1
H81B H -0.083403 1.198101 0.209418 0.096 Uiso 0.5 1 calc R U P A 1
H81C H -0.047083 1.216671 0.181083 0.096 Uiso 0.5 1 calc R U P B 2
H81D H -0.180458 1.192193 0.202244 0.096 Uiso 0.5 1 calc R U P B 2
C84 C -0.0745(3) 1.20522(16) 0.06219(14) 0.0631(8) Uani 1 1 d D . . . .
H84A H -0.152506 1.216987 0.042993 0.076 Uiso 0.5 1 calc R U P C 1
H84B H -0.013113 1.222769 0.027516 0.076 Uiso 0.5 1 calc R U P C 1
H84C H -0.000262 1.233556 0.054820 0.076 Uiso 0.5 1 calc R U P D 2
H84D H -0.104264 1.210015 0.019835 0.076 Uiso 0.5 1 calc R U P D 2
C85 C -0.0544(2) 1.11475(15) 0.10223(11) 0.0462(6) Uani 1 1 d . . . . .
H85A H -0.104287 1.079565 0.088243 0.055 Uiso 1 1 calc R U . . .
H85B H 0.028635 1.095154 0.097867 0.055 Uiso 1 1 calc R U . . .
C86 C -0.3779(2) 1.06384(16) 0.17754(14) 0.0557(7) Uani 1 1 d . . . . .
H86A H -0.356670 1.113080 0.140122 0.067 Uiso 1 1 calc R U . . .
H86B H -0.389157 1.081308 0.216278 0.067 Uiso 1 1 calc R U . . .
C87 C -0.4877(2) 1.02919(17) 0.16548(13) 0.0542(7) Uani 1 1 d . . . . .
H87A H -0.531284 1.001129 0.206323 0.065 Uiso 1 1 calc R U . . .
H87B H -0.539779 1.073941 0.136779 0.065 Uiso 1 1 calc R U . . .
C88 C -0.4388(2) 0.96688(17) 0.13331(13) 0.0539(7) Uani 1 1 d . . . . .
H88A H -0.417142 0.995362 0.087324 0.065 Uiso 1 1 calc R U . . .
H88B H -0.495223 0.924308 0.136669 0.065 Uiso 1 1 calc R U . . .
C89 C -0.3316(2) 0.92773(15) 0.17206(12) 0.0453(6) Uani 1 1 d . . . . .
H89A H -0.353017 0.881875 0.211907 0.054 Uiso 1 1 calc R U . . .
H89B H -0.272523 0.904700 0.146419 0.054 Uiso 1 1 calc R U . . .
Li2 Li -0.1445(3) 1.0049(3) 0.2232(2) 0.0436(10) Uani 1 1 d . . . . .
C83 C -0.0666(5) 1.2494(3) 0.1145(3) 0.0605(17) Uani 0.5 1 d D . P E 1
H83A H 0.015699 1.258049 0.120331 0.073 Uiso 0.5 1 calc R U P E 1
H83B H -0.112600 1.304394 0.102473 0.073 Uiso 0.5 1 calc R U P E 1
C82 C -0.1552(5) 1.2418(3) 0.0951(2) 0.0538(14) Uani 0.5 1 d D . P E 2
H82A H -0.236293 1.230874 0.088809 0.065 Uiso 0.5 1 calc R U P E 2
H82B H -0.148196 1.303235 0.082353 0.065 Uiso 0.5 1 calc R U P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Al1 C1 2.022(2) . ?
Al1 C8 2.016(2) . ?
Al1 C15 2.029(3) . ?
Al1 C22 2.019(3) . ?
C1 C2 1.419(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.509(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.404(3) . ?
C8 C13 1.412(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(3) . ?
C13 C14 1.513(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.409(3) . ?
C15 C20 1.406(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.381(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.379(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.397(3) . ?
C20 C21 1.509(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.405(3) . ?
C22 C27 1.408(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.388(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.370(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.379(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.395(3) . ?
C27 C28 1.506(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
Al2 C29 2.028(2) . ?
Al2 C36 2.023(2) . ?
Al2 C43 2.023(2) . ?
Al2 C50 2.029(2) . ?
C29 C30 1.401(3) . ?
C29 C34 1.412(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.383(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.377(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.383(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.397(3) . ?
C34 C35 1.510(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.401(3) . ?
C36 C41 1.409(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.377(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.377(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.380(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.389(3) . ?
C41 C42 1.508(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.408(3) . ?
C43 C48 1.400(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.389(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.375(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.385(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.392(3) . ?
C48 C49 1.513(3) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.399(3) . ?
C50 C55 1.407(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.391(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.374(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.374(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.396(3) . ?
C55 C56 1.510(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
O1 C57 1.447(3) . ?
O1 C60 1.428(3) . ?
O1 Li1 1.902(4) . ?
O2 C61 1.423(3) . ?
O2 C64 1.430(3) . ?
O2 Li1 1.914(5) . ?
O3 C65 1.438(3) . ?
O3 C68 1.439(3) . ?
O3 Li1 1.918(4) . ?
O4 C69 1.439(3) . ?
O4 C72 1.454(3) . ?
O4 Li1 1.889(4) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.494(4) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.508(4) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.513(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.486(4) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.503(4) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.500(3) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.519(3) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.497(4) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.494(4) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.454(4) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.532(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.495(4) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
O5 C73 1.433(3) . ?
O5 C76 1.423(3) . ?
O5 Li2 1.888(5) . ?
O6 C77 1.441(3) . ?
O6 C80 1.439(3) . ?
O6 Li2 1.935(5) . ?
O7 C81 1.433(3) . ?
O7 C85 1.449(3) . ?
O7 Li2 1.920(4) . ?
O8 C86 1.454(3) . ?
O8 C89 1.437(3) . ?
O8 Li2 1.905(4) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.483(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.489(4) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C76 1.490(4) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C77 C78 1.514(4) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C78 C79 1.504(4) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C79 C80 1.493(3) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C81 H81C 0.9900 . ?
C81 H81D 0.9900 . ?
C81 C83 1.407(6) . ?
C81 C82 1.670(6) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 H84C 0.9900 . ?
C84 H84D 0.9900 . ?
C84 C85 1.494(3) . ?
C84 C83 1.581(6) . ?
C84 C82 1.369(6) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C86 C87 1.507(3) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C87 C88 1.507(4) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.515(3) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?

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
C1 Al1 C15 109.37(10) . . ?
C8 Al1 C1 111.74(10) . . ?
C8 Al1 C15 107.64(10) . . ?
C8 Al1 C22 110.50(10) . . ?
C22 Al1 C1 106.62(10) . . ?
C22 Al1 C15 110.99(10) . . ?
C2 C1 Al1 124.69(16) . . ?
C6 C1 Al1 119.73(16) . . ?
C6 C1 C2 115.44(19) . . ?
C1 C2 C7 121.06(19) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 C7 118.6(2) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(2) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.8(2) . . ?
C6 C5 H5 120.6 . . ?
C1 C6 H6 118.0 . . ?
C5 C6 C1 124.1(2) . . ?
C5 C6 H6 118.0 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 Al1 120.22(16) . . ?
C9 C8 C13 115.3(2) . . ?
C13 C8 Al1 124.31(16) . . ?
C8 C9 H9 118.0 . . ?
C10 C9 C8 124.0(2) . . ?
C10 C9 H9 118.0 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 119.1(2) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.3(2) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.2 . . ?
C11 C12 C13 121.5(2) . . ?
C13 C12 H12 119.2 . . ?
C8 C13 C14 120.3(2) . . ?
C12 C13 C8 120.8(2) . . ?
C12 C13 C14 118.9(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 Al1 119.84(17) . . ?
C20 C15 Al1 124.59(16) . . ?
C20 C15 C16 115.54(19) . . ?
C15 C16 H16 118.4 . . ?
C17 C16 C15 123.3(2) . . ?
C17 C16 H16 118.4 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.1(2) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.4(2) . . ?
C20 C19 H19 119.3 . . ?
C15 C20 C21 120.73(19) . . ?
C19 C20 C15 121.1(2) . . ?
C19 C20 C21 118.2(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 Al1 119.95(18) . . ?
C23 C22 C27 115.6(2) . . ?
C27 C22 Al1 124.38(16) . . ?
C22 C23 H23 118.4 . . ?
C24 C23 C22 123.2(2) . . ?
C24 C23 H23 118.4 . . ?
C23 C24 H24 120.2 . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.3(2) . . ?
C26 C25 H25 120.3 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.3(2) . . ?
C27 C26 H26 119.4 . . ?
C22 C27 C28 121.4(2) . . ?
C26 C27 C22 120.9(2) . . ?
C26 C27 C28 117.7(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 Al2 C50 107.56(10) . . ?
C36 Al2 C29 108.26(10) . . ?
C36 Al2 C43 110.93(10) . . ?
C36 Al2 C50 109.68(10) . . ?
C43 Al2 C29 109.23(10) . . ?
C43 Al2 C50 111.07(10) . . ?
C30 C29 Al2 120.07(16) . . ?
C30 C29 C34 115.83(19) . . ?
C34 C29 Al2 124.08(15) . . ?
C29 C30 H30 118.2 . . ?
C31 C30 C29 123.6(2) . . ?
C31 C30 H30 118.2 . . ?
C30 C31 H31 120.4 . . ?
C32 C31 C30 119.3(2) . . ?
C32 C31 H31 120.4 . . ?
C31 C32 H32 120.2 . . ?
C31 C32 C33 119.6(2) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.5 . . ?
C32 C33 C34 121.1(2) . . ?
C34 C33 H33 119.5 . . ?
C29 C34 C35 120.61(19) . . ?
C33 C34 C29 120.7(2) . . ?
C33 C34 C35 118.7(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 Al2 119.14(16) . . ?
C37 C36 C41 115.5(2) . . ?
C41 C36 Al2 125.01(16) . . ?
C36 C37 H37 118.1 . . ?
C38 C37 C36 123.7(2) . . ?
C38 C37 H37 118.1 . . ?
C37 C38 H38 120.2 . . ?
C37 C38 C39 119.6(2) . . ?
C39 C38 H38 120.2 . . ?
C38 C39 H39 120.6 . . ?
C38 C39 C40 118.8(2) . . ?
C40 C39 H39 120.6 . . ?
C39 C40 H40 119.1 . . ?
C39 C40 C41 121.8(2) . . ?
C41 C40 H40 119.1 . . ?
C36 C41 C42 120.6(2) . . ?
C40 C41 C36 120.6(2) . . ?
C40 C41 C42 118.9(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 Al2 118.90(17) . . ?
C48 C43 Al2 124.98(15) . . ?
C48 C43 C44 116.0(2) . . ?
C43 C44 H44 118.4 . . ?
C45 C44 C43 123.1(2) . . ?
C45 C44 H44 118.4 . . ?
C44 C45 H45 120.4 . . ?
C46 C45 C44 119.2(2) . . ?
C46 C45 H45 120.4 . . ?
C45 C46 H46 120.3 . . ?
C45 C46 C47 119.4(2) . . ?
C47 C46 H46 120.3 . . ?
C46 C47 H47 119.4 . . ?
C46 C47 C48 121.2(2) . . ?
C48 C47 H47 119.4 . . ?
C43 C48 C49 121.4(2) . . ?
C47 C48 C43 120.9(2) . . ?
C47 C48 C49 117.6(2) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 Al2 120.67(17) . . ?
C51 C50 C55 115.84(19) . . ?
C55 C50 Al2 123.42(16) . . ?
C50 C51 H51 118.5 . . ?
C52 C51 C50 123.0(2) . . ?
C52 C51 H51 118.5 . . ?
C51 C52 H52 120.2 . . ?
C53 C52 C51 119.6(2) . . ?
C53 C52 H52 120.2 . . ?
C52 C53 H53 120.3 . . ?
C54 C53 C52 119.4(2) . . ?
C54 C53 H53 120.3 . . ?
C53 C54 H54 119.4 . . ?
C53 C54 C55 121.2(2) . . ?
C55 C54 H54 119.4 . . ?
C50 C55 C56 120.29(19) . . ?
C54 C55 C50 120.9(2) . . ?
C54 C55 C56 118.8(2) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C57 O1 Li1 117.3(2) . . ?
C60 O1 C57 109.83(18) . . ?
C60 O1 Li1 132.58(19) . . ?
C61 O2 C64 108.60(19) . . ?
C61 O2 Li1 122.8(2) . . ?
C64 O2 Li1 125.80(19) . . ?
C65 O3 C68 108.77(19) . . ?
C65 O3 Li1 121.65(19) . . ?
C68 O3 Li1 123.4(2) . . ?
C69 O4 C72 110.1(2) . . ?
C69 O4 Li1 127.3(2) . . ?
C72 O4 Li1 119.9(2) . . ?
O1 C57 H57A 110.6 . . ?
O1 C57 H57B 110.6 . . ?
O1 C57 C58 105.5(2) . . ?
H57A C57 H57B 108.8 . . ?
C58 C57 H57A 110.6 . . ?
C58 C57 H57B 110.6 . . ?
C57 C58 H58A 111.4 . . ?
C57 C58 H58B 111.4 . . ?
C57 C58 C59 101.9(2) . . ?
H58A C58 H58B 109.3 . . ?
C59 C58 H58A 111.4 . . ?
C59 C58 H58B 111.4 . . ?
C58 C59 H59A 111.4 . . ?
C58 C59 H59B 111.4 . . ?
C58 C59 C60 101.9(2) . . ?
H59A C59 H59B 109.2 . . ?
C60 C59 H59A 111.4 . . ?
C60 C59 H59B 111.4 . . ?
O1 C60 C59 104.6(2) . . ?
O1 C60 H60A 110.8 . . ?
O1 C60 H60B 110.8 . . ?
C59 C60 H60A 110.8 . . ?
C59 C60 H60B 110.8 . . ?
H60A C60 H60B 108.9 . . ?
O2 C61 H61A 110.1 . . ?
O2 C61 H61B 110.1 . . ?
O2 C61 C62 107.8(2) . . ?
H61A C61 H61B 108.5 . . ?
C62 C61 H61A 110.1 . . ?
C62 C61 H61B 110.1 . . ?
C61 C62 H62A 111.0 . . ?
C61 C62 H62B 111.0 . . ?
C61 C62 C63 103.7(2) . . ?
H62A C62 H62B 109.0 . . ?
C63 C62 H62A 111.0 . . ?
C63 C62 H62B 111.0 . . ?
C62 C63 H63A 111.3 . . ?
C62 C63 H63B 111.3 . . ?
H63A C63 H63B 109.2 . . ?
C64 C63 C62 102.1(2) . . ?
C64 C63 H63A 111.3 . . ?
C64 C63 H63B 111.3 . . ?
O2 C64 C63 105.3(2) . . ?
O2 C64 H64A 110.7 . . ?
O2 C64 H64B 110.7 . . ?
C63 C64 H64A 110.7 . . ?
C63 C64 H64B 110.7 . . ?
H64A C64 H64B 108.8 . . ?
O3 C65 H65A 110.5 . . ?
O3 C65 H65B 110.5 . . ?
O3 C65 C66 106.2(2) . . ?
H65A C65 H65B 108.7 . . ?
C66 C65 H65A 110.5 . . ?
C66 C65 H65B 110.5 . . ?
C65 C66 H66A 110.9 . . ?
C65 C66 H66B 110.9 . . ?
H66A C66 H66B 108.9 . . ?
C67 C66 C65 104.2(2) . . ?
C67 C66 H66A 110.9 . . ?
C67 C66 H66B 110.9 . . ?
C66 C67 H67A 111.3 . . ?
C66 C67 H67B 111.3 . . ?
H67A C67 H67B 109.2 . . ?
C68 C67 C66 102.3(2) . . ?
C68 C67 H67A 111.3 . . ?
C68 C67 H67B 111.3 . . ?
O3 C68 C67 105.5(2) . . ?
O3 C68 H68A 110.7 . . ?
O3 C68 H68B 110.7 . . ?
C67 C68 H68A 110.7 . . ?
C67 C68 H68B 110.7 . . ?
H68A C68 H68B 108.8 . . ?
O4 C69 H69A 110.7 . . ?
O4 C69 H69B 110.7 . . ?
O4 C69 C70 105.3(3) . . ?
H69A C69 H69B 108.8 . . ?
C70 C69 H69A 110.7 . . ?
C70 C69 H69B 110.7 . . ?
C69 C70 H70A 111.0 . . ?
C69 C70 H70B 111.0 . . ?
C69 C70 C71 103.8(3) . . ?
H70A C70 H70B 109.0 . . ?
C71 C70 H70A 111.0 . . ?
C71 C70 H70B 111.0 . . ?
C70 C71 H71A 111.5 . . ?
C70 C71 H71B 111.5 . . ?
H71A C71 H71B 109.4 . . ?
C72 C71 C70 101.2(2) . . ?
C72 C71 H71A 111.5 . . ?
C72 C71 H71B 111.5 . . ?
O4 C72 C71 104.6(2) . . ?
O4 C72 H72A 110.8 . . ?
O4 C72 H72B 110.8 . . ?
C71 C72 H72A 110.8 . . ?
C71 C72 H72B 110.8 . . ?
H72A C72 H72B 108.9 . . ?
O1 Li1 O2 105.6(2) . . ?
O1 Li1 O3 119.4(2) . . ?
O2 Li1 O3 107.4(2) . . ?
O4 Li1 O1 107.4(2) . . ?
O4 Li1 O2 112.5(2) . . ?
O4 Li1 O3 104.6(2) . . ?
C73 O5 Li2 125.1(2) . . ?
C76 O5 C73 108.5(2) . . ?
C76 O5 Li2 122.18(19) . . ?
C77 O6 Li2 123.1(2) . . ?
C80 O6 C77 108.81(19) . . ?
C80 O6 Li2 124.03(19) . . ?
C81 O7 C85 108.5(2) . . ?
C81 O7 Li2 127.8(2) . . ?
C85 O7 Li2 116.42(19) . . ?
C86 O8 Li2 118.5(2) . . ?
C89 O8 C86 109.25(18) . . ?
C89 O8 Li2 131.96(19) . . ?
O5 C73 H73A 110.3 . . ?
O5 C73 H73B 110.3 . . ?
O5 C73 C74 106.9(2) . . ?
H73A C73 H73B 108.6 . . ?
C74 C73 H73A 110.3 . . ?
C74 C73 H73B 110.3 . . ?
C73 C74 H74A 111.0 . . ?
C73 C74 H74B 111.0 . . ?
C73 C74 C75 104.0(2) . . ?
H74A C74 H74B 109.0 . . ?
C75 C74 H74A 111.0 . . ?
C75 C74 H74B 111.0 . . ?
C74 C75 H75A 111.3 . . ?
C74 C75 H75B 111.3 . . ?
C74 C75 C76 102.3(2) . . ?
H75A C75 H75B 109.2 . . ?
C76 C75 H75A 111.3 . . ?
C76 C75 H75B 111.3 . . ?
O5 C76 C75 104.7(2) . . ?
O5 C76 H76A 110.8 . . ?
O5 C76 H76B 110.8 . . ?
C75 C76 H76A 110.8 . . ?
C75 C76 H76B 110.8 . . ?
H76A C76 H76B 108.9 . . ?
O6 C77 H77A 110.5 . . ?
O6 C77 H77B 110.5 . . ?
O6 C77 C78 106.1(2) . . ?
H77A C77 H77B 108.7 . . ?
C78 C77 H77A 110.5 . . ?
C78 C77 H77B 110.5 . . ?
C77 C78 H78A 111.3 . . ?
C77 C78 H78B 111.3 . . ?
H78A C78 H78B 109.2 . . ?
C79 C78 C77 102.5(2) . . ?
C79 C78 H78A 111.3 . . ?
C79 C78 H78B 111.3 . . ?
C78 C79 H79A 111.3 . . ?
C78 C79 H79B 111.3 . . ?
H79A C79 H79B 109.2 . . ?
C80 C79 C78 102.3(2) . . ?
C80 C79 H79A 111.3 . . ?
C80 C79 H79B 111.3 . . ?
O6 C80 C79 106.2(2) . . ?
O6 C80 H80A 110.5 . . ?
O6 C80 H80B 110.5 . . ?
C79 C80 H80A 110.5 . . ?
C79 C80 H80B 110.5 . . ?
H80A C80 H80B 108.7 . . ?
O7 C81 H81A 110.2 . . ?
O7 C81 H81B 110.2 . . ?
O7 C81 H81C 111.6 . . ?
O7 C81 H81D 111.6 . . ?
O7 C81 C82 100.9(3) . . ?
H81A C81 H81B 108.5 . . ?
H81C C81 H81D 109.4 . . ?
C83 C81 O7 107.8(3) . . ?
C83 C81 H81A 110.2 . . ?
C83 C81 H81B 110.2 . . ?
C82 C81 H81C 111.6 . . ?
C82 C81 H81D 111.6 . . ?
H84A C84 H84B 109.4 . . ?
H84C C84 H84D 108.5 . . ?
C85 C84 H84A 111.6 . . ?
C85 C84 H84B 111.6 . . ?
C85 C84 H84C 110.2 . . ?
C85 C84 H84D 110.2 . . ?
C85 C84 C83 101.0(3) . . ?
C83 C84 H84A 111.6 . . ?
C83 C84 H84B 111.6 . . ?
C82 C84 H84C 110.2 . . ?
C82 C84 H84D 110.2 . . ?
C82 C84 C85 107.5(3) . . ?
O7 C85 C84 106.9(2) . . ?
O7 C85 H85A 110.3 . . ?
O7 C85 H85B 110.3 . . ?
C84 C85 H85A 110.3 . . ?
C84 C85 H85B 110.3 . . ?
H85A C85 H85B 108.6 . . ?
O8 C86 H86A 110.6 . . ?
O8 C86 H86B 110.6 . . ?
O8 C86 C87 105.6(2) . . ?
H86A C86 H86B 108.7 . . ?
C87 C86 H86A 110.6 . . ?
C87 C86 H86B 110.6 . . ?
C86 C87 H87A 111.4 . . ?
C86 C87 H87B 111.4 . . ?
H87A C87 H87B 109.3 . . ?
C88 C87 C86 101.9(2) . . ?
C88 C87 H87A 111.4 . . ?
C88 C87 H87B 111.4 . . ?
C87 C88 H88A 111.4 . . ?
C87 C88 H88B 111.4 . . ?
C87 C88 C89 101.8(2) . . ?
H88A C88 H88B 109.3 . . ?
C89 C88 H88A 111.4 . . ?
C89 C88 H88B 111.4 . . ?
O8 C89 C88 104.70(19) . . ?
O8 C89 H89A 110.8 . . ?
O8 C89 H89B 110.8 . . ?
C88 C89 H89A 110.8 . . ?
C88 C89 H89B 110.8 . . ?
H89A C89 H89B 108.9 . . ?
O5 Li2 O6 107.5(2) . . ?
O5 Li2 O7 115.6(2) . . ?
O5 Li2 O8 105.1(2) . . ?
O7 Li2 O6 102.4(2) . . ?
O8 Li2 O6 120.8(2) . . ?
O8 Li2 O7 106.1(2) . . ?
C81 C83 C84 103.1(4) . . ?
C81 C83 H83A 111.1 . . ?
C81 C83 H83B 111.1 . . ?
C84 C83 H83A 111.1 . . ?
C84 C83 H83B 111.1 . . ?
H83A C83 H83B 109.1 . . ?
C81 C82 H82A 111.7 . . ?
C81 C82 H82B 111.7 . . ?
C84 C82 C81 100.3(4) . . ?
C84 C82 H82A 111.7 . . ?
C84 C82 H82B 111.7 . . ?
H82A C82 H82B 109.5 . . ?

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
Al1 C1 C2 C3 -177.65(17) . . . . ?
Al1 C1 C2 C7 1.3(3) . . . . ?
Al1 C1 C6 C5 177.26(19) . . . . ?
Al1 C8 C9 C10 -177.22(18) . . . . ?
Al1 C8 C13 C12 177.75(18) . . . . ?
Al1 C8 C13 C14 -2.4(3) . . . . ?
Al1 C15 C16 C17 179.97(17) . . . . ?
Al1 C15 C20 C19 -179.82(16) . . . . ?
Al1 C15 C20 C21 1.9(3) . . . . ?
Al1 C22 C23 C24 177.51(17) . . . . ?
Al1 C22 C27 C26 -179.54(16) . . . . ?
Al1 C22 C27 C28 -2.1(3) . . . . ?
C1 C2 C3 C4 1.6(4) . . . . ?
C2 C1 C6 C5 1.4(3) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C6 C1 C2 C3 -2.0(3) . . . . ?
C6 C1 C2 C7 177.0(2) . . . . ?
C7 C2 C3 C4 -177.4(2) . . . . ?
C8 C9 C10 C11 -0.1(4) . . . . ?
C9 C8 C13 C12 1.9(3) . . . . ?
C9 C8 C13 C14 -178.3(2) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C11 C12 C13 C8 -1.4(4) . . . . ?
C11 C12 C13 C14 178.8(2) . . . . ?
C13 C8 C9 C10 -1.2(3) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
C16 C15 C20 C19 2.1(3) . . . . ?
C16 C15 C20 C21 -176.14(19) . . . . ?
C16 C17 C18 C19 0.6(4) . . . . ?
C17 C18 C19 C20 -0.3(4) . . . . ?
C18 C19 C20 C15 -1.1(3) . . . . ?
C18 C19 C20 C21 177.2(2) . . . . ?
C20 C15 C16 C17 -1.9(3) . . . . ?
C22 C23 C24 C25 2.1(4) . . . . ?
C23 C22 C27 C26 -2.6(3) . . . . ?
C23 C22 C27 C28 174.79(19) . . . . ?
C23 C24 C25 C26 -2.4(4) . . . . ?
C24 C25 C26 C27 0.2(4) . . . . ?
C25 C26 C27 C22 2.4(3) . . . . ?
C25 C26 C27 C28 -175.1(2) . . . . ?
C27 C22 C23 C24 0.5(3) . . . . ?
Al2 C29 C30 C31 -177.15(17) . . . . ?
Al2 C29 C34 C33 177.11(17) . . . . ?
Al2 C29 C34 C35 -3.6(3) . . . . ?
Al2 C36 C37 C38 -174.98(18) . . . . ?
Al2 C36 C41 C40 174.50(17) . . . . ?
Al2 C36 C41 C42 -5.5(3) . . . . ?
Al2 C43 C44 C45 177.48(16) . . . . ?
Al2 C43 C48 C47 -177.39(16) . . . . ?
Al2 C43 C48 C49 1.6(3) . . . . ?
Al2 C50 C51 C52 175.05(16) . . . . ?
Al2 C50 C55 C54 -174.71(16) . . . . ?
Al2 C50 C55 C56 6.7(3) . . . . ?
C29 C30 C31 C32 -0.1(4) . . . . ?
C30 C29 C34 C33 -1.6(3) . . . . ?
C30 C29 C34 C35 177.8(2) . . . . ?
C30 C31 C32 C33 -1.4(4) . . . . ?
C31 C32 C33 C34 1.4(4) . . . . ?
C32 C33 C34 C29 0.2(4) . . . . ?
C32 C33 C34 C35 -179.2(2) . . . . ?
C34 C29 C30 C31 1.6(3) . . . . ?
C36 C37 C38 C39 0.9(4) . . . . ?
C37 C36 C41 C40 1.0(3) . . . . ?
C37 C36 C41 C42 -179.0(2) . . . . ?
C37 C38 C39 C40 -0.6(4) . . . . ?
C38 C39 C40 C41 0.5(4) . . . . ?
C39 C40 C41 C36 -0.8(4) . . . . ?
C39 C40 C41 C42 179.2(2) . . . . ?
C41 C36 C37 C38 -1.1(3) . . . . ?
C43 C44 C45 C46 -0.5(3) . . . . ?
C44 C43 C48 C47 -1.3(3) . . . . ?
C44 C43 C48 C49 177.65(19) . . . . ?
C44 C45 C46 C47 0.0(3) . . . . ?
C45 C46 C47 C48 -0.2(3) . . . . ?
C46 C47 C48 C43 0.9(3) . . . . ?
C46 C47 C48 C49 -178.1(2) . . . . ?
C48 C43 C44 C45 1.2(3) . . . . ?
C50 C51 C52 C53 0.2(3) . . . . ?
C51 C50 C55 C54 2.4(3) . . . . ?
C51 C50 C55 C56 -176.12(19) . . . . ?
C51 C52 C53 C54 1.6(3) . . . . ?
C52 C53 C54 C55 -1.3(3) . . . . ?
C53 C54 C55 C50 -0.8(3) . . . . ?
C53 C54 C55 C56 177.8(2) . . . . ?
C55 C50 C51 C52 -2.2(3) . . . . ?
O1 C57 C58 C59 31.5(3) . . . . ?
O2 C61 C62 C63 19.4(3) . . . . ?
O3 C65 C66 C67 -18.4(3) . . . . ?
O4 C69 C70 C71 -31.2(4) . . . . ?
C57 O1 C60 C59 -14.9(3) . . . . ?
C57 C58 C59 C60 -39.8(3) . . . . ?
C58 C59 C60 O1 34.1(3) . . . . ?
C60 O1 C57 C58 -10.6(3) . . . . ?
C61 O2 C64 C63 -23.4(3) . . . . ?
C61 C62 C63 C64 -32.3(3) . . . . ?
C62 C63 C64 O2 34.5(3) . . . . ?
C64 O2 C61 C62 2.4(3) . . . . ?
C65 O3 C68 C67 25.1(3) . . . . ?
C65 C66 C67 C68 32.6(3) . . . . ?
C66 C67 C68 O3 -35.8(3) . . . . ?
C68 O3 C65 C66 -4.0(3) . . . . ?
C69 O4 C72 C71 13.8(3) . . . . ?
C69 O4 Li1 O1 -102.5(3) . . . . ?
C69 O4 Li1 O2 13.3(4) . . . . ?
C69 O4 Li1 O3 129.6(3) . . . . ?
C69 C70 C71 C72 38.9(3) . . . . ?
C70 C71 C72 O4 -31.6(3) . . . . ?
C72 O4 C69 C70 11.3(4) . . . . ?
C72 O4 Li1 O1 57.0(3) . . . . ?
C72 O4 Li1 O2 172.8(2) . . . . ?
C72 O4 Li1 O3 -70.8(3) . . . . ?
Li1 O1 C57 C58 163.8(2) . . . . ?
Li1 O1 C60 C59 171.8(2) . . . . ?
Li1 O2 C61 C62 -159.7(2) . . . . ?
Li1 O2 C64 C63 138.0(2) . . . . ?
Li1 O3 C65 C66 149.2(2) . . . . ?
Li1 O3 C68 C67 -127.5(3) . . . . ?
Li1 O4 C69 C70 172.5(3) . . . . ?
Li1 O4 C72 C71 -149.0(2) . . . . ?
O5 C73 C74 C75 -18.7(3) . . . . ?
O6 C77 C78 C79 27.9(3) . . . . ?
O7 C81 C83 C84 33.8(5) . . . . ?
O7 C81 C82 C84 -38.1(4) . . . . ?
O8 C86 C87 C88 -30.6(3) . . . . ?
C73 O5 C76 C75 25.7(3) . . . . ?
C73 O5 Li2 O6 -109.0(3) . . . . ?
C73 O5 Li2 O7 137.5(2) . . . . ?
C73 O5 Li2 O8 20.9(3) . . . . ?
C73 C74 C75 C76 33.3(3) . . . . ?
C74 C75 C76 O5 -36.5(3) . . . . ?
C76 O5 C73 C74 -4.3(3) . . . . ?
C76 O5 Li2 O6 45.2(3) . . . . ?
C76 O5 Li2 O7 -68.4(3) . . . . ?
C76 O5 Li2 O8 175.1(2) . . . . ?
C77 O6 C80 C79 -16.2(3) . . . . ?
C77 C78 C79 C80 -36.8(3) . . . . ?
C78 C79 C80 O6 33.2(3) . . . . ?
C80 O6 C77 C78 -7.6(3) . . . . ?
C81 O7 C85 C84 -3.4(3) . . . . ?
C85 O7 C81 C83 -20.3(4) . . . . ?
C85 O7 C81 C82 23.9(3) . . . . ?
C85 C84 C83 C81 -34.3(4) . . . . ?
C85 C84 C82 C81 36.9(4) . . . . ?
C86 O8 C89 C88 17.1(3) . . . . ?
C86 C87 C88 C89 40.1(3) . . . . ?
C87 C88 C89 O8 -35.8(3) . . . . ?
C89 O8 C86 C87 8.6(3) . . . . ?
Li2 O5 C73 C74 152.8(3) . . . . ?
Li2 O5 C76 C75 -132.3(2) . . . . ?
Li2 O6 C77 C78 -165.8(2) . . . . ?
Li2 O6 C80 C79 141.7(2) . . . . ?
Li2 O7 C81 C83 -169.0(4) . . . . ?
Li2 O7 C81 C82 -124.8(3) . . . . ?
Li2 O7 C85 C84 149.4(2) . . . . ?
Li2 O8 C86 C87 -165.7(2) . . . . ?
Li2 O8 C89 C88 -169.6(2) . . . . ?
C83 C84 C85 O7 22.4(3) . . . . ?
C82 C84 C85 O7 -24.3(4) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '60.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   18.0
_STOE_evaluation_integration_B   1.0
_STOE_evaluation_integration_EMS 0.046
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 94.8
_STOE_evaluation_LANA_DXS_max_order -
_STOE_evaluation_LANA_DYS_max_order -
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 139.6
_STOE_evaluation_LANA_max_2theta_desired 139.6
_STOE_evaluation_LANA_mean_redundancy 3.6
_STOE_evaluation_LANA_number_refls_after_OR 51578
_STOE_evaluation_LANA_number_refls_outliers 637
_STOE_evaluation_LANA_number_refls_total 52215
_STOE_evaluation_LANA_number_refls_unique 14314
_STOE_evaluation_LANA_number_refls_written 51578
_STOE_evaluation_LANA_OR_c1      0.050
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      1.0
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          12.5   27.5   42.5   57.5   72.5   87.5  102.5  117.5  132.5
#----------------------------------------------------------------------------
<Resolution>    5.33   3.08   2.12   1.57   1.29   1.12   1.00   0.90   0.85
N(total)         217   1403   2364   4605   8818  11604   9001   9656   4547
<Redundancy>     2.3    3.2    2.6    3.1    4.3    4.8    3.6    3.6    2.3
Complet. [%%]    91.8  100.0   99.0   98.4   98.8   98.4   91.8   96.9   83.7
<I/sigma>      106.2   55.1   19.5    8.3    4.7    3.1    2.3    1.4    1.2
R(int)         0.017  0.015  0.026  0.041  0.067  0.085  0.110  0.178  0.205
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     Al_otolyl_4_LiTHF_4
_STOE_measurement_max_exposure_per_frame '5.0 s'
_STOE_measurement_mean_exposure_per_frame '4.8 s'
_STOE_measurement_min_exposure_per_frame '1.0 s'
_STOE_measurement_total_exposure_time '5.1 h'
_STOE_measurement_total_frame_number 3817
_STOE_measurement_total_run_number 50
_STOE_measurement_tube_power     '50.0 W'
_exptl_crystal_recrystallization_method layering
_chemical_properties_physical    Moisture-sensitive
