data_mates01

_vrf_PLAT302_mates01
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-3  ) .. 100% 
RESPONSE: The cocrystallized diethyl ether molecule is modeled as
disordered over two positions (0.75(1):0.25(1)).
;

_vrf_PLAT860_mates01
;
PROBLEM: _G Number of Least-Squares Restraints ............. 19 
RESPONSE: Analogous bond lengths and angles between the two positions
of the disordered solvent molecule were restrained to be similar.
Anisotropic displacement parameters for proximal atoms were
constrained two be equivalent. Atom pair C14/C14' was constrained
to be isopositional.
;

_audit_creation_date               2019-08-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

#CrysAlisPro, version 171.40.58a
Rigaku Oxford Diffraction (2019). CrysAlisPro Software system,
version 171.40.58a. Rigaku Corporation, Oxford, UK.

#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.

#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C12 H40 Li2 O21 V6, C4 H10 O'
_chemical_formula_sum              'C16 H50 Li2 O22 V6'
_chemical_formula_weight           914.08
_chemical_melting_point            ?
_chemical_oxdiff_formula           ?
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        '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                     17.4358(2)
_cell_length_b                     10.35010(10)
_cell_length_c                     20.6189(2)
_cell_angle_alpha                  90
_cell_angle_beta                   105.5010(10)
_cell_angle_gamma                  90
_cell_volume                       3585.59(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      21340
_cell_measurement_temperature      100.00(10)
_cell_measurement_theta_max        77.5650
_cell_measurement_theta_min        2.6610
_shelx_estimated_absorpt_T_max     0.741
_shelx_estimated_absorpt_T_min     0.149
_exptl_absorpt_coefficient_mu      13.294
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.38429
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              green
_exptl_crystal_colour_primary      green
_exptl_crystal_density_diffrn      1.693
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         needle
_exptl_crystal_F_000               1864
_exptl_crystal_size_max            0.231
_exptl_crystal_size_mid            0.052
_exptl_crystal_size_min            0.024
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0396
_diffrn_reflns_av_unetI/netI       0.0298
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.984
_diffrn_reflns_limit_h_max         22
_diffrn_reflns_limit_h_min         -22
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -13
_diffrn_reflns_limit_l_max         22
_diffrn_reflns_limit_l_min         -26
_diffrn_reflns_number              36183
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.984
_diffrn_reflns_theta_full          74.504
_diffrn_reflns_theta_max           77.967
_diffrn_reflns_theta_min           2.630
_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  1.000
_diffrn_measured_fraction_theta_max  0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -15.00  11.00   0.50    0.44    --   49.75 -83.00  50.00   52
  2  ω     12.00  71.00   0.50    0.44    --   49.75 -83.00  50.00  118
  3  ω     40.00 121.00   0.50    1.74    --  105.75 -83.00  50.00  162
  4  ω     68.00 113.00   0.50    1.74    --  105.75 -77.00  90.00   90
  5  ω     52.00  77.00   0.50    1.74    --  105.75 -61.00  90.00   50
  6  ω     42.00  74.00   0.50    1.74    --  105.75 -61.00 120.00   64
  7  ω     39.00  67.00   0.50    1.74    --  105.75 -61.00 150.00   56
  8  ω     98.00 156.00   0.50    1.74    --  105.75  15.00  90.00  116
  9  ω    106.00 158.00   0.50    1.74    --  105.75  83.00 171.00  104
 10  ω     92.00 150.00   0.50    1.74    --  105.75  61.00  90.00  116
 11  ω    103.00 164.00   0.50    1.74    --  105.75  15.00  30.00  122
 12  ω    143.00 168.00   0.50    1.74    --  105.75  15.00 -30.00   50
 13  ω    140.00 166.00   0.50    1.74    --  105.75  61.00-120.00   52
 14  ω    102.00 136.00   0.50    1.74    --  105.75  15.00 -30.00   68
 15  ω     94.00 120.00   0.50    1.74    --  105.75  61.00-120.00   52
 16  ω     35.00  79.00   0.50    1.74    --  105.75 -61.00 -60.00   88
 17  ω     39.00  64.00   0.50    1.74    --  105.75 -61.00 -30.00   50
 18  ω     34.00  78.00   0.50    1.74    --  105.75 -61.00 -90.00   88
 19  ω     34.00 105.00   0.50    1.74    --  105.75 -94.00-150.00  142
 20  ω     34.00  68.00   0.50    1.74    --  105.75 -61.00-150.00   68
 21  ω     37.00 104.00   0.50    1.74    --  105.75 -94.00  30.00  134
 22  ω     44.00  80.00   0.50    1.74    --  105.75 -61.00  60.00   72
 23  ω    105.00 170.00   0.50    1.74    --  105.75  45.00 120.00  130
 24  ω     -4.00  24.00   0.50    0.44    --  -49.75  19.00  90.00   56
 25  ω     -5.00  22.00   0.50    0.44    --  -49.75  19.00  60.00   54
 26  ω    -42.00   5.00   0.50    0.44    --  -49.75  83.00 171.00   94
 27  ω    -16.00  12.00   0.50    0.44    --   49.75 -19.00 150.00   56
 28  ω   -121.00 -73.00   0.50    0.44    --  -49.75-125.00   0.00   96
 29  ω   -142.00-117.00   0.50    1.74    --  -84.25 -83.00  50.00   50
 30  ω    -43.00 -18.00   0.50    1.74    --  -84.25  45.00   0.00   50
 31  ω     -4.00  24.00   0.50    0.44    --  -49.75  19.00-150.00   56
 32  ω     -5.00  23.00   0.50    0.44    --  -49.75  19.00-180.00   56
 33  ω   -119.00 -75.00   0.50    0.44    --  -49.75-125.00-180.00   88
 34  ω    -84.00 -59.00   0.50    1.74    --  -84.25  83.00 171.00   50
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0814769000
_diffrn_orient_matrix_UB_12        -0.0464391000
_diffrn_orient_matrix_UB_13        0.0066638000
_diffrn_orient_matrix_UB_21        -0.0395464000
_diffrn_orient_matrix_UB_22        0.1216052000
_diffrn_orient_matrix_UB_23        -0.0375255000
_diffrn_orient_matrix_UB_31        -0.0141658000
_diffrn_orient_matrix_UB_32        -0.0722165000
_diffrn_orient_matrix_UB_33        -0.0675284000
_diffrn_oxdiff_digest_frames
;
01bcafc618e1903b228a2bdf119e8d8e8800041d4d1
;
_diffrn_oxdiff_digest_hkl
;
01322952c90b55c395ee6c1f2ca122a6c9cde0
;
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  6850
_reflns_number_total               7544
_reflns_odcompleteness_completeness  99.97
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_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 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max           0.420
_refine_diff_density_min           -0.427
_refine_diff_density_rms           0.075
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.069
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       460
_refine_ls_number_reflns           7544
_refine_ls_number_restraints       19
_refine_ls_R_factor_all            0.0309
_refine_ls_R_factor_gt             0.0277
_refine_ls_restrained_S_all        1.068
_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)+(0.0399P)²+1.8274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0740
_refine_ls_wR_factor_ref           0.0757
_refine_special_details 
;
The cocrystallized diethyl ether molecule is modeled as
disordered over two positions (0.75(1):0.25(1)). Analogous
bond lengths and angles between the two positions of the
disordered solvent molecule were restrained to be similar.
Anisotropic displacement parameters for proximal atoms were
constrained two be equivalent. Atom pair C14/C14' was
constrained to be isopositional.
;
_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. Shared sites
{C14, C14'}
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13')
Uanis(C14) = Uanis(C14')
Uanis(O22) = Uanis(O22')
Uanis(C15) = Uanis(C15')
Uanis(C16) = Uanis(C16')
4. Same fragment restrains
{C16, C15, O22, C14, C13} sigma for 1-2: 0.02, 1-3: 0.04
as
{C13, C14, O22, C15, C16}
{C13, C14, O22, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04
as
{C13', C14', O22', C15', C16'}
5. Others
 Sof(C13')=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14')=Sof(H14C)=Sof(H14D)=
 Sof(O22')=Sof(C15')=Sof(H15C)=Sof(H15D)=Sof(C16')=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(O22)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C14'(H14C,H14D), C15'(H15C,H15D)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C13'(H13D,H13E,H13F), C16'(H16D,H16E,H16F)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap
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 0.67059(2) 0.35704(3) 0.32834(2) 0.01224(8) Uani 1 1 d . . . . .
 V2 V 0.85541(2) 0.30776(3) 0.42259(2) 0.01172(7) Uani 1 1 d . . . . .
 V3 V 0.72700(2) 0.46842(3) 0.48410(2) 0.01104(7) Uani 1 1 d . . . . .
 V4 V 0.60260(2) 0.23291(3) 0.44809(2) 0.01191(8) Uani 1 1 d . . . . .
 V5 V 0.72850(2) 0.07040(3) 0.38598(2) 0.01204(7) Uani 1 1 d . . . . .
 V6 V 0.78611(2) 0.18135(3) 0.54117(2) 0.01157(8) Uani 1 1 d . . . . .
 O1 O 0.63228(8) 0.41879(14) 0.25579(6) 0.0201(3) Uani 1 1 d . . . . .
 O2 O 0.94110(8) 0.33754(14) 0.41218(7) 0.0190(3) Uani 1 1 d . . . . .
 O3 O 0.72583(8) 0.61061(13) 0.51578(6) 0.0168(3) Uani 1 1 d . . . . .
 O4 O 0.51527(8) 0.20423(14) 0.45743(7) 0.0198(3) Uani 1 1 d . . . . .
 O5 O 0.72835(8) -0.07165(13) 0.35399(7) 0.0183(3) Uani 1 1 d . . . . .
 O6 O 0.82389(8) 0.11956(13) 0.61395(6) 0.0186(3) Uani 1 1 d . . . . .
 O7 O 0.78779(7) 0.38795(13) 0.33556(6) 0.0137(2) Uani 1 1 d . . . . .
 O8 O 0.68372(7) 0.51984(12) 0.38556(6) 0.0138(2) Uani 1 1 d . . . . .
 O9 O 0.57391(7) 0.30897(13) 0.35652(6) 0.0151(3) Uani 1 1 d . . . . .
 O10 O 0.68331(8) 0.17360(13) 0.30376(6) 0.0156(3) Uani 1 1 d . . . . .
 O11 O 0.83302(7) 0.47935(12) 0.46214(6) 0.0129(2) Uani 1 1 d . . . . .
 O12 O 0.61917(7) 0.41026(13) 0.48681(6) 0.0140(3) Uani 1 1 d . . . . .
 O13 O 0.62142(7) 0.06069(13) 0.40730(6) 0.0142(2) Uani 1 1 d . . . . .
 O14 O 0.83691(7) 0.12925(13) 0.38581(6) 0.0150(3) Uani 1 1 d . . . . .
 O15 O 0.88379(7) 0.23322(13) 0.51520(6) 0.0139(3) Uani 1 1 d . . . . .
 O16 O 0.77204(7) 0.36423(12) 0.56629(6) 0.0142(2) Uani 1 1 d . . . . .
 O17 O 0.66838(7) 0.14907(13) 0.53422(6) 0.0136(2) Uani 1 1 d . . . . .
 O18 O 0.77202(7) 0.01749(12) 0.48431(6) 0.0138(2) Uani 1 1 d . . . . .
 O19 O 0.72674(7) 0.26829(12) 0.43545(6) 0.0119(2) Uani 1 1 d . . . . .
 C1 C 0.81227(12) 0.3724(2) 0.27481(9) 0.0212(4) Uani 1 1 d . . . . .
 H1A H 0.800461 0.286156 0.258023 0.032 Uiso 1 1 calc GR . . . .
 H1B H 0.868476 0.387632 0.284087 0.032 Uiso 1 1 calc GR . . . .
 H1C H 0.784223 0.433166 0.241706 0.032 Uiso 1 1 calc GR . . . .
 C2 C 0.62181(12) 0.6152(2) 0.37049(10) 0.0215(4) Uani 1 1 d . . . . .
 H2A H 0.599939 0.620728 0.322628 0.032 Uiso 1 1 calc GR . . . .
 H2B H 0.643366 0.697525 0.387600 0.032 Uiso 1 1 calc GR . . . .
 H2C H 0.580682 0.591036 0.391161 0.032 Uiso 1 1 calc GR . . . .
 C3 C 0.49626(12) 0.3538(2) 0.32533(11) 0.0270(5) Uani 1 1 d . . . . .
 H3A H 0.478837 0.409837 0.355665 0.040 Uiso 1 1 calc GR . . . .
 H3B H 0.460680 0.281510 0.313981 0.040 Uiso 1 1 calc GR . . . .
 H3C H 0.496501 0.400458 0.285149 0.040 Uiso 1 1 calc GR . . . .
 C4 C 0.64100(17) 0.1210(2) 0.24179(11) 0.0372(6) Uani 1 1 d . . . . .
 H4A H 0.586395 0.147886 0.231745 0.056 Uiso 1 1 calc GR . . . .
 H4B H 0.643714 0.028376 0.244221 0.056 Uiso 1 1 calc GR . . . .
 H4C H 0.663943 0.150588 0.207013 0.056 Uiso 1 1 calc GR . . . .
 C5 C 0.89952(11) 0.54012(19) 0.50859(10) 0.0184(4) Uani 1 1 d . . . . .
 H5A H 0.925595 0.478735 0.542170 0.028 Uiso 1 1 calc GR . . . .
 H5B H 0.881049 0.611749 0.529878 0.028 Uiso 1 1 calc GR . . . .
 H5C H 0.936357 0.570497 0.484751 0.028 Uiso 1 1 calc GR . . . .
 C6 C 0.59383(12) 0.4477(2) 0.54432(10) 0.0193(4) Uani 1 1 d . . . . .
 H6A H 0.635615 0.430796 0.584367 0.029 Uiso 1 1 calc GR . . . .
 H6B H 0.547319 0.399223 0.545628 0.029 Uiso 1 1 calc GR . . . .
 H6C H 0.581484 0.538248 0.541707 0.029 Uiso 1 1 calc GR . . . .
 C7 C 0.55461(12) 0.0032(2) 0.36040(10) 0.0229(4) Uani 1 1 d . . . . .
 H7A H 0.513577 -0.014005 0.382359 0.034 Uiso 1 1 calc GR . . . .
 H7B H 0.570716 -0.076287 0.343936 0.034 Uiso 1 1 calc GR . . . .
 H7C H 0.534671 0.061226 0.323414 0.034 Uiso 1 1 calc GR . . . .
 C8 C 0.87831(12) 0.0713(2) 0.34273(11) 0.0234(4) Uani 1 1 d . . . . .
 H8A H 0.845806 0.074333 0.297120 0.035 Uiso 1 1 calc GR . . . .
 H8B H 0.890131 -0.017059 0.355835 0.035 Uiso 1 1 calc GR . . . .
 H8C H 0.927012 0.117318 0.346073 0.035 Uiso 1 1 calc GR . . . .
 C9 C 0.95868(11) 0.1713(2) 0.54002(11) 0.0228(4) Uani 1 1 d . . . . .
 H9A H 0.967600 0.113177 0.506499 0.034 Uiso 1 1 calc GR . . . .
 H9B H 0.958925 0.123775 0.580053 0.034 Uiso 1 1 calc GR . . . .
 H9C H 1.000087 0.235205 0.550279 0.034 Uiso 1 1 calc GR . . . .
 C10 C 0.81806(14) 0.4159(2) 0.62809(9) 0.0247(4) Uani 1 1 d . . . . .
 H10A H 0.873427 0.412890 0.629203 0.037 Uiso 1 1 calc GR . . . .
 H10B H 0.809339 0.365982 0.664710 0.037 Uiso 1 1 calc GR . . . .
 H10C H 0.802603 0.503902 0.632245 0.037 Uiso 1 1 calc GR . . . .
 C11 C 0.64486(12) 0.1480(2) 0.59570(9) 0.0210(4) Uani 1 1 d . . . . .
 H11A H 0.670014 0.218483 0.623679 0.032 Uiso 1 1 calc GR . . . .
 H11B H 0.660710 0.067874 0.618817 0.032 Uiso 1 1 calc GR . . . .
 H11C H 0.588110 0.157063 0.585781 0.032 Uiso 1 1 calc GR . . . .
 C12 C 0.83209(12) -0.08089(19) 0.49788(10) 0.0198(4) Uani 1 1 d . . . . .
 H12A H 0.808169 -0.162911 0.482845 0.030 Uiso 1 1 calc GR . . . .
 H12B H 0.856904 -0.084515 0.545385 0.030 Uiso 1 1 calc GR . . . .
 H12C H 0.871421 -0.061119 0.474485 0.030 Uiso 1 1 calc GR . . . .
 Li1 Li 0.7901(2) 0.5611(3) 0.37419(16) 0.0196(7) Uani 1 1 d . . . . .
 Li2 Li 0.6660(2) -0.0231(3) 0.49383(17) 0.0193(7) Uani 1 1 d . . . . .
 C13 C 0.7041(3) 0.7226(5) 0.1848(3) 0.0337(11) Uani 0.753(10) 1 d D . P A 1
 H13A H 0.700987 0.661179 0.218867 0.051 Uiso 0.753(10) 1 calc GR . P A 1
 H13B H 0.659411 0.711248 0.146215 0.051 Uiso 0.753(10) 1 calc GR . P A 1
 H13C H 0.703327 0.808618 0.202088 0.051 Uiso 0.753(10) 1 calc GR . P A 1
 C14 C 0.78059(13) 0.7020(2) 0.16456(10) 0.0269(4) Uani 0.753(10) 1 d D . P A 1
 H14A H 0.784298 0.612498 0.151721 0.032 Uiso 0.753(10) 1 calc R . P A 1
 H14B H 0.780721 0.755978 0.126142 0.032 Uiso 0.753(10) 1 calc R . P A 1
 O22 O 0.8468(3) 0.7336(6) 0.2193(3) 0.0292(12) Uani 0.753(10) 1 d D . P A 1
 C15 C 0.9211(2) 0.7123(6) 0.2049(2) 0.0382(12) Uani 0.753(10) 1 d D . P A 1
 H15A H 0.924399 0.763527 0.166364 0.046 Uiso 0.753(10) 1 calc R . P A 1
 H15B H 0.926521 0.621888 0.194562 0.046 Uiso 0.753(10) 1 calc R . P A 1
 C16 C 0.9861(2) 0.7509(9) 0.2660(2) 0.068(2) Uani 0.753(10) 1 d D . P A 1
 H16A H 0.982096 0.841664 0.274226 0.102 Uiso 0.753(10) 1 calc GR . P A 1
 H16B H 1.036967 0.732771 0.258453 0.102 Uiso 0.753(10) 1 calc GR . P A 1
 H16C H 0.980555 0.702951 0.304386 0.102 Uiso 0.753(10) 1 calc GR . P A 1
 C13' C 0.7125(9) 0.7647(17) 0.1853(11) 0.0337(11) Uani 0.247(10) 1 d D . P A 2
 H13D H 0.699173 0.713379 0.219515 0.051 Uiso 0.247(10) 1 calc GR . P A 2
 H13E H 0.667067 0.770786 0.146945 0.051 Uiso 0.247(10) 1 calc GR . P A 2
 H13F H 0.728006 0.849616 0.202539 0.051 Uiso 0.247(10) 1 calc GR . P A 2
 C14' C 0.78059(13) 0.7020(2) 0.16456(10) 0.0269(4) Uani 0.247(10) 1 d D . P A 2
 H14C H 0.767520 0.613284 0.150742 0.032 Uiso 0.247(10) 1 calc R . P A 2
 H14D H 0.791694 0.748609 0.127279 0.032 Uiso 0.247(10) 1 calc R . P A 2
 O22' O 0.8485(8) 0.706(2) 0.2225(9) 0.0292(12) Uani 0.247(10) 1 d D . P A 2
 C15' C 0.9189(8) 0.6588(18) 0.2078(7) 0.0382(12) Uani 0.247(10) 1 d D . P A 2
 H15C H 0.933914 0.715209 0.175620 0.046 Uiso 0.247(10) 1 calc R . P A 2
 H15D H 0.909586 0.572969 0.188354 0.046 Uiso 0.247(10) 1 calc R . P A 2
 C16' C 0.9840(7) 0.655(3) 0.2720(7) 0.068(2) Uani 0.247(10) 1 d D . P A 2
 H16D H 0.995678 0.740859 0.288960 0.102 Uiso 0.247(10) 1 calc GR . P A 2
 H16E H 1.030777 0.617080 0.263694 0.102 Uiso 0.247(10) 1 calc GR . P A 2
 H16F H 0.967153 0.603463 0.304506 0.102 Uiso 0.247(10) 1 calc GR . P A 2
 O20 O 0.82284(9) 0.71640(14) 0.34570(8) 0.0212(3) Uani 1 1 d . . . B 2
 H20A H 0.8326(17) 0.721(3) 0.3083(15) 0.028(7) Uiso 1 1 d . . . C 2
 H20B H 0.7931(19) 0.781(3) 0.3464(15) 0.038(8) Uiso 1 1 d . . . D 2
 O21 O 0.62862(10) -0.17809(15) 0.51422(8) 0.0243(3) Uani 1 1 d . . . E 2
 H21A H 0.591(2) -0.190(3) 0.5221(15) 0.037(8) Uiso 1 1 d . . . F 2
 H21B H 0.655(2) -0.254(3) 0.5178(16) 0.046(9) Uiso 1 1 d . . . G 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
 V1 O1 1.5995(13) . ?
 V1 O7 2.0343(13) . ?
 V1 O8 2.0344(13) . ?
 V1 O9 1.9874(13) . ?
 V1 O10 1.9928(13) . ?
 V1 O19 2.3502(12) . ?
 V2 O2 1.5953(13) . ?
 V2 O7 2.0416(13) . ?
 V2 O11 2.0351(13) . ?
 V2 O14 1.9905(13) . ?
 V2 O15 1.9952(12) . ?
 V2 O19 2.3639(12) . ?
 V3 O3 1.6125(13) . ?
 V3 O8 2.0399(12) . ?
 V3 O11 2.0204(12) . ?
 V3 O12 1.9891(13) . ?
 V3 O16 1.9850(12) . ?
 V3 O19 2.3009(12) . ?
 V4 O4 1.6126(13) . ?
 V4 O9 1.9823(13) . ?
 V4 O12 1.9917(13) . ?
 V4 O13 2.0347(13) . ?
 V4 O17 2.0333(13) . ?
 V4 O19 2.2779(12) . ?
 V5 O5 1.6111(14) . ?
 V5 O10 1.9803(13) . ?
 V5 O13 2.0317(13) . ?
 V5 O14 1.9868(13) . ?
 V5 O18 2.0407(13) . ?
 V5 O19 2.2920(12) . ?
 V6 O6 1.6020(13) . ?
 V6 O15 1.9908(13) . ?
 V6 O16 1.9948(13) . ?
 V6 O17 2.0466(12) . ?
 V6 O18 2.0389(13) . ?
 V6 O19 2.3296(12) . ?
 O7 C1 1.436(2) . ?
 O7 Li1 1.958(4) . ?
 O8 C2 1.434(2) . ?
 O8 Li1 1.978(4) . ?
 O9 C3 1.413(2) . ?
 O10 C4 1.404(2) . ?
 O11 C5 1.437(2) . ?
 O11 Li1 1.960(4) . ?
 O12 C6 1.425(2) . ?
 O13 C7 1.430(2) . ?
 O13 Li2 1.949(4) . ?
 O14 C8 1.419(2) . ?
 O15 C9 1.421(2) . ?
 O16 C10 1.417(2) . ?
 O17 C11 1.433(2) . ?
 O17 Li2 1.962(4) . ?
 O18 C12 1.434(2) . ?
 O18 Li2 1.956(3) . ?
 C1 H1A 0.9600 . ?
 C1 H1B 0.9600 . ?
 C1 H1C 0.9600 . ?
 C2 H2A 0.9600 . ?
 C2 H2B 0.9600 . ?
 C2 H2C 0.9600 . ?
 C3 H3A 0.9600 . ?
 C3 H3B 0.9600 . ?
 C3 H3C 0.9600 . ?
 C4 H4A 0.9600 . ?
 C4 H4B 0.9600 . ?
 C4 H4C 0.9600 . ?
 C5 H5A 0.9600 . ?
 C5 H5B 0.9600 . ?
 C5 H5C 0.9600 . ?
 C6 H6A 0.9600 . ?
 C6 H6B 0.9600 . ?
 C6 H6C 0.9600 . ?
 C7 H7A 0.9600 . ?
 C7 H7B 0.9600 . ?
 C7 H7C 0.9600 . ?
 C8 H8A 0.9600 . ?
 C8 H8B 0.9600 . ?
 C8 H8C 0.9600 . ?
 C9 H9A 0.9600 . ?
 C9 H9B 0.9600 . ?
 C9 H9C 0.9600 . ?
 C10 H10A 0.9600 . ?
 C10 H10B 0.9600 . ?
 C10 H10C 0.9600 . ?
 C11 H11A 0.9600 . ?
 C11 H11B 0.9600 . ?
 C11 H11C 0.9600 . ?
 C12 H12A 0.9600 . ?
 C12 H12B 0.9600 . ?
 C12 H12C 0.9600 . ?
 Li1 O20 1.853(4) . ?
 Li2 O21 1.823(4) . ?
 Li2 H21A 2.33(3) . ?
 C13 H13A 0.9600 . ?
 C13 H13B 0.9600 . ?
 C13 H13C 0.9600 . ?
 C13 C14 1.516(5) . ?
 C14 H14A 0.9700 . ?
 C14 H14B 0.9700 . ?
 C14 O22 1.420(5) . ?
 O22 C15 1.421(5) . ?
 C15 H15A 0.9700 . ?
 C15 H15B 0.9700 . ?
 C15 C16 1.506(5) . ?
 C16 H16A 0.9600 . ?
 C16 H16B 0.9600 . ?
 C16 H16C 0.9600 . ?
 C13' H13D 0.9600 . ?
 C13' H13E 0.9600 . ?
 C13' H13F 0.9600 . ?
 C13' C14' 1.511(12) . ?
 C14' H14C 0.9700 . ?
 C14' H14D 0.9700 . ?
 C14' O22' 1.440(13) . ?
 O22' C15' 1.429(14) . ?
 C15' H15C 0.9700 . ?
 C15' H15D 0.9700 . ?
 C15' C16' 1.496(13) . ?
 C16' H16D 0.9600 . ?
 C16' H16E 0.9600 . ?
 C16' H16F 0.9600 . ?
 O20 H20A 0.83(3) . ?
 O20 H20B 0.85(3) . ?
 O21 H21A 0.72(3) . ?
 O21 H21B 0.90(4) . ?

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
 O1 V1 O7 99.54(6) . . ?
 O1 V1 O8 99.53(6) . . ?
 O1 V1 O9 101.46(6) . . ?
 O1 V1 O10 100.94(6) . . ?
 O1 V1 O19 179.43(6) . . ?
 O7 V1 O8 82.65(5) . . ?
 O7 V1 O19 80.48(5) . . ?
 O8 V1 O19 79.91(5) . . ?
 O9 V1 O7 158.73(5) . . ?
 O9 V1 O8 90.61(5) . . ?
 O9 V1 O10 89.81(6) . . ?
 O9 V1 O19 78.48(5) . . ?
 O10 V1 O7 89.45(5) . . ?
 O10 V1 O8 159.02(5) . . ?
 O10 V1 O19 79.63(5) . . ?
 O2 V2 O7 98.32(6) . . ?
 O2 V2 O11 99.92(6) . . ?
 O2 V2 O14 100.97(6) . . ?
 O2 V2 O15 101.64(6) . . ?
 O2 V2 O19 178.26(6) . . ?
 O7 V2 O19 80.00(5) . . ?
 O11 V2 O7 82.52(5) . . ?
 O11 V2 O19 79.42(5) . . ?
 O14 V2 O7 92.62(5) . . ?
 O14 V2 O11 159.03(5) . . ?
 O14 V2 O15 88.81(5) . . ?
 O14 V2 O19 79.65(5) . . ?
 O15 V2 O7 159.33(5) . . ?
 O15 V2 O11 88.80(5) . . ?
 O15 V2 O19 79.98(5) . . ?
 O3 V3 O8 97.12(6) . . ?
 O3 V3 O11 98.69(6) . . ?
 O3 V3 O12 98.65(6) . . ?
 O3 V3 O16 101.24(6) . . ?
 O3 V3 O19 178.12(6) . . ?
 O8 V3 O19 81.00(5) . . ?
 O11 V3 O8 83.06(5) . . ?
 O11 V3 O19 81.26(5) . . ?
 O12 V3 O8 90.35(5) . . ?
 O12 V3 O11 162.08(5) . . ?
 O12 V3 O19 81.26(5) . . ?
 O16 V3 O8 161.57(5) . . ?
 O16 V3 O11 92.58(5) . . ?
 O16 V3 O12 88.44(5) . . ?
 O16 V3 O19 80.64(5) . . ?
 O4 V4 O9 100.42(6) . . ?
 O4 V4 O12 99.34(6) . . ?
 O4 V4 O13 98.61(6) . . ?
 O4 V4 O17 98.47(6) . . ?
 O4 V4 O19 178.61(6) . . ?
 O9 V4 O12 89.34(5) . . ?
 O9 V4 O13 88.95(5) . . ?
 O9 V4 O17 160.27(5) . . ?
 O9 V4 O19 80.38(5) . . ?
 O12 V4 O13 161.98(5) . . ?
 O12 V4 O17 93.19(5) . . ?
 O12 V4 O19 81.79(5) . . ?
 O13 V4 O19 80.24(5) . . ?
 O17 V4 O13 82.62(5) . . ?
 O17 V4 O19 80.63(5) . . ?
 O5 V5 O10 100.66(6) . . ?
 O5 V5 O13 98.19(6) . . ?
 O5 V5 O14 100.16(6) . . ?
 O5 V5 O18 96.97(6) . . ?
 O5 V5 O19 177.35(6) . . ?
 O10 V5 O13 91.92(5) . . ?
 O10 V5 O14 89.67(6) . . ?
 O10 V5 O18 162.28(5) . . ?
 O10 V5 O19 81.34(5) . . ?
 O13 V5 O18 83.74(5) . . ?
 O13 V5 O19 79.96(5) . . ?
 O14 V5 O13 160.96(5) . . ?
 O14 V5 O18 89.01(5) . . ?
 O14 V5 O19 81.53(5) . . ?
 O18 V5 O19 80.98(5) . . ?
 O6 V6 O15 101.10(6) . . ?
 O6 V6 O16 100.60(6) . . ?
 O6 V6 O17 98.86(6) . . ?
 O6 V6 O18 99.37(6) . . ?
 O6 V6 O19 177.95(6) . . ?
 O15 V6 O16 89.28(5) . . ?
 O15 V6 O17 159.94(5) . . ?
 O15 V6 O18 92.86(5) . . ?
 O15 V6 O19 80.92(5) . . ?
 O16 V6 O17 88.99(5) . . ?
 O16 V6 O18 159.12(5) . . ?
 O16 V6 O19 79.73(5) . . ?
 O17 V6 O19 79.11(5) . . ?
 O18 V6 O17 81.92(5) . . ?
 O18 V6 O19 80.10(5) . . ?
 V1 O7 V2 109.47(6) . . ?
 C1 O7 V1 116.45(11) . . ?
 C1 O7 V2 119.00(11) . . ?
 C1 O7 Li1 118.59(15) . . ?
 Li1 O7 V1 94.87(11) . . ?
 Li1 O7 V2 94.04(11) . . ?
 V1 O8 V3 108.41(6) . . ?
 C2 O8 V1 118.86(11) . . ?
 C2 O8 V3 116.87(11) . . ?
 C2 O8 Li1 120.08(15) . . ?
 Li1 O8 V1 94.25(11) . . ?
 Li1 O8 V3 93.75(11) . . ?
 V4 O9 V1 111.10(6) . . ?
 C3 O9 V1 124.69(12) . . ?
 C3 O9 V4 122.08(12) . . ?
 V5 O10 V1 110.00(6) . . ?
 C4 O10 V1 122.30(13) . . ?
 C4 O10 V5 124.20(13) . . ?
 V3 O11 V2 109.02(6) . . ?
 C5 O11 V2 116.24(11) . . ?
 C5 O11 V3 119.93(11) . . ?
 C5 O11 Li1 117.92(15) . . ?
 Li1 O11 V2 94.18(11) . . ?
 Li1 O11 V3 94.92(11) . . ?
 V3 O12 V4 107.73(6) . . ?
 C6 O12 V3 116.53(11) . . ?
 C6 O12 V4 122.68(12) . . ?
 V5 O13 V4 107.77(6) . . ?
 C7 O13 V4 116.87(12) . . ?
 C7 O13 V5 120.27(11) . . ?
 C7 O13 Li2 119.18(15) . . ?
 Li2 O13 V4 94.59(11) . . ?
 Li2 O13 V5 93.18(11) . . ?
 V5 O14 V2 109.95(6) . . ?
 C8 O14 V2 124.98(12) . . ?
 C8 O14 V5 121.00(12) . . ?
 V6 O15 V2 110.52(6) . . ?
 C9 O15 V2 119.21(11) . . ?
 C9 O15 V6 123.45(11) . . ?
 V3 O16 V6 109.99(6) . . ?
 C10 O16 V3 124.23(12) . . ?
 C10 O16 V6 120.83(12) . . ?
 V4 O17 V6 108.21(5) . . ?
 C11 O17 V4 123.23(11) . . ?
 C11 O17 V6 117.27(11) . . ?
 C11 O17 Li2 112.96(15) . . ?
 Li2 O17 V4 94.23(11) . . ?
 Li2 O17 V6 94.88(11) . . ?
 V6 O18 V5 107.68(6) . . ?
 C12 O18 V5 116.28(11) . . ?
 C12 O18 V6 120.60(11) . . ?
 C12 O18 Li2 119.27(15) . . ?
 Li2 O18 V5 92.68(11) . . ?
 Li2 O18 V6 95.32(11) . . ?
 V1 O19 V2 89.81(4) . . ?
 V3 O19 V1 90.55(4) . . ?
 V3 O19 V2 90.11(4) . . ?
 V3 O19 V6 89.49(4) . . ?
 V4 O19 V1 90.02(4) . . ?
 V4 O19 V2 179.29(6) . . ?
 V4 O19 V3 89.20(4) . . ?
 V4 O19 V5 91.91(4) . . ?
 V4 O19 V6 91.66(4) . . ?
 V5 O19 V1 89.02(4) . . ?
 V5 O19 V2 88.77(4) . . ?
 V5 O19 V3 178.81(6) . . ?
 V5 O19 V6 90.91(4) . . ?
 V6 O19 V1 178.32(6) . . ?
 V6 O19 V2 88.51(4) . . ?
 O7 C1 H1A 109.5 . . ?
 O7 C1 H1B 109.5 . . ?
 O7 C1 H1C 109.5 . . ?
 H1A C1 H1B 109.5 . . ?
 H1A C1 H1C 109.5 . . ?
 H1B C1 H1C 109.5 . . ?
 O8 C2 H2A 109.5 . . ?
 O8 C2 H2B 109.5 . . ?
 O8 C2 H2C 109.5 . . ?
 H2A C2 H2B 109.5 . . ?
 H2A C2 H2C 109.5 . . ?
 H2B C2 H2C 109.5 . . ?
 O9 C3 H3A 109.5 . . ?
 O9 C3 H3B 109.5 . . ?
 O9 C3 H3C 109.5 . . ?
 H3A C3 H3B 109.5 . . ?
 H3A C3 H3C 109.5 . . ?
 H3B C3 H3C 109.5 . . ?
 O10 C4 H4A 109.5 . . ?
 O10 C4 H4B 109.5 . . ?
 O10 C4 H4C 109.5 . . ?
 H4A C4 H4B 109.5 . . ?
 H4A C4 H4C 109.5 . . ?
 H4B C4 H4C 109.5 . . ?
 O11 C5 H5A 109.5 . . ?
 O11 C5 H5B 109.5 . . ?
 O11 C5 H5C 109.5 . . ?
 H5A C5 H5B 109.5 . . ?
 H5A C5 H5C 109.5 . . ?
 H5B C5 H5C 109.5 . . ?
 O12 C6 H6A 109.5 . . ?
 O12 C6 H6B 109.5 . . ?
 O12 C6 H6C 109.5 . . ?
 H6A C6 H6B 109.5 . . ?
 H6A C6 H6C 109.5 . . ?
 H6B C6 H6C 109.5 . . ?
 O13 C7 H7A 109.5 . . ?
 O13 C7 H7B 109.5 . . ?
 O13 C7 H7C 109.5 . . ?
 H7A C7 H7B 109.5 . . ?
 H7A C7 H7C 109.5 . . ?
 H7B C7 H7C 109.5 . . ?
 O14 C8 H8A 109.5 . . ?
 O14 C8 H8B 109.5 . . ?
 O14 C8 H8C 109.5 . . ?
 H8A C8 H8B 109.5 . . ?
 H8A C8 H8C 109.5 . . ?
 H8B C8 H8C 109.5 . . ?
 O15 C9 H9A 109.5 . . ?
 O15 C9 H9B 109.5 . . ?
 O15 C9 H9C 109.5 . . ?
 H9A C9 H9B 109.5 . . ?
 H9A C9 H9C 109.5 . . ?
 H9B C9 H9C 109.5 . . ?
 O16 C10 H10A 109.5 . . ?
 O16 C10 H10B 109.5 . . ?
 O16 C10 H10C 109.5 . . ?
 H10A C10 H10B 109.5 . . ?
 H10A C10 H10C 109.5 . . ?
 H10B C10 H10C 109.5 . . ?
 O17 C11 H11A 109.5 . . ?
 O17 C11 H11B 109.5 . . ?
 O17 C11 H11C 109.5 . . ?
 H11A C11 H11B 109.5 . . ?
 H11A C11 H11C 109.5 . . ?
 H11B C11 H11C 109.5 . . ?
 O18 C12 H12A 109.5 . . ?
 O18 C12 H12B 109.5 . . ?
 O18 C12 H12C 109.5 . . ?
 H12A C12 H12B 109.5 . . ?
 H12A C12 H12C 109.5 . . ?
 H12B C12 H12C 109.5 . . ?
 O7 Li1 O8 86.12(15) . . ?
 O7 Li1 O11 86.68(15) . . ?
 O11 Li1 O8 86.28(14) . . ?
 O20 Li1 O7 129.79(19) . . ?
 O20 Li1 O8 127.10(19) . . ?
 O20 Li1 O11 126.47(19) . . ?
 O13 Li2 O17 86.73(15) . . ?
 O13 Li2 O18 88.23(14) . . ?
 O13 Li2 H21A 116.5(8) . . ?
 O17 Li2 H21A 121.1(8) . . ?
 O18 Li2 O17 86.24(14) . . ?
 O18 Li2 H21A 142.3(8) . . ?
 O21 Li2 O13 121.54(19) . . ?
 O21 Li2 O17 132.04(19) . . ?
 O21 Li2 O18 128.1(2) . . ?
 O21 Li2 H21A 14.4(8) . . ?
 H13A C13 H13B 109.5 . . ?
 H13A C13 H13C 109.5 . . ?
 H13B C13 H13C 109.5 . . ?
 C14 C13 H13A 109.5 . . ?
 C14 C13 H13B 109.5 . . ?
 C14 C13 H13C 109.5 . . ?
 C13 C14 H14A 109.7 . . ?
 C13 C14 H14B 109.7 . . ?
 H14A C14 H14B 108.2 . . ?
 O22 C14 C13 109.7(3) . . ?
 O22 C14 H14A 109.7 . . ?
 O22 C14 H14B 109.7 . . ?
 C14 O22 C15 113.0(4) . . ?
 O22 C15 H15A 110.1 . . ?
 O22 C15 H15B 110.1 . . ?
 O22 C15 C16 107.9(4) . . ?
 H15A C15 H15B 108.4 . . ?
 C16 C15 H15A 110.1 . . ?
 C16 C15 H15B 110.1 . . ?
 C15 C16 H16A 109.5 . . ?
 C15 C16 H16B 109.5 . . ?
 C15 C16 H16C 109.5 . . ?
 H16A C16 H16B 109.5 . . ?
 H16A C16 H16C 109.5 . . ?
 H16B C16 H16C 109.5 . . ?
 H13D C13' H13E 109.5 . . ?
 H13D C13' H13F 109.5 . . ?
 H13E C13' H13F 109.5 . . ?
 C14' C13' H13D 109.5 . . ?
 C14' C13' H13E 109.5 . . ?
 C14' C13' H13F 109.5 . . ?
 C13' C14' H14C 110.4 . . ?
 C13' C14' H14D 110.4 . . ?
 H14C C14' H14D 108.6 . . ?
 O22' C14' C13' 106.6(10) . . ?
 O22' C14' H14C 110.4 . . ?
 O22' C14' H14D 110.4 . . ?
 C15' O22' C14' 112.1(14) . . ?
 O22' C15' H15C 110.1 . . ?
 O22' C15' H15D 110.1 . . ?
 O22' C15' C16' 108.2(12) . . ?
 H15C C15' H15D 108.4 . . ?
 C16' C15' H15C 110.1 . . ?
 C16' C15' H15D 110.1 . . ?
 C15' C16' H16D 109.5 . . ?
 C15' C16' H16E 109.5 . . ?
 C15' C16' H16F 109.5 . . ?
 H16D C16' H16E 109.5 . . ?
 H16D C16' H16F 109.5 . . ?
 H16E C16' H16F 109.5 . . ?
 Li1 O20 H20A 120.2(19) . . ?
 Li1 O20 H20B 116(2) . . ?
 H20A O20 H20B 104(3) . . ?
 Li2 O21 H21A 127(3) . . ?
 Li2 O21 H21B 126(2) . . ?
 H21A O21 H21B 108(3) . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O20 H20A O22' 0.83(3) 1.87(4) 2.70(2) 171(3) . yes
 O20 H20B O5 0.85(3) 1.93(3) 2.776(2) 177(3) 1_565 yes
 O21 H21A O4 0.72(3) 2.02(3) 2.737(2) 175(3) 3_656 yes
 O21 H21B O3 0.90(4) 1.88(4) 2.762(2) 166(3) 1_545 yes

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
 C13 C14 O22 C15 177.9(4) . . . . ?
 C14 O22 C15 C16 179.2(4) . . . . ?
 C13' C14' O22' C15' -175.3(16) . . . . ?
 C14' O22' C15' C16' -174.5(16) . . . . ?

_olex2_submission_original_sample_id  mates01
_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  2.224
_oxdiff_exptl_absorpt_empirical_full_min  0.695
