# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_mates22
_database_code_depnum_ccdc_archive 'CCDC 2234804'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2023-01-06 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;

_vrf_PLAT112_mates22             
;
PROBLEM: _C ADDSYM Detects New (Pseudo) Symm. Elem         A         92 %Fit 
RESPONSE: The structure can be modeled with additional imposed symmetry.
However, the structure is of much poorer quality with significant disorder.
;

_vrf_PLAT302_mates22             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 40% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3-4  ) .. 100% 
RESPONSE: Both tetrahydrofuran molecules of crystallization are
modeled as disordered over two positions each: O20/C13-C16,
0.50(1):0.50(1), O21/C17-C20, 0.80(1):0.20(1).
;

_vrf_PLAT860_mates22             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 101 
RESPONSE: Analogous bond lengths and angles between the two positions
of each disordered tetrahydrofuran molecule were restrained to be
similar. Anisotropic displacement parameters for proximal atoms
were restrained to be similar and some were restrained toward the
expected motion relative to bond direction.
;

_audit_creation_date             2022-03-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H38 O19 V6, 2(C4 H8 O)'
_chemical_formula_sum            'C20 H54 O21 V6'
_chemical_formula_weight         936.27
_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'
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                   9.2190(2)
_cell_length_b                   10.6059(2)
_cell_length_c                   18.4535(2)
_cell_angle_alpha                96.3890(10)
_cell_angle_beta                 90.1810(10)
_cell_angle_gamma                91.4940(10)
_cell_volume                     1792.46(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26024
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6380
_cell_measurement_theta_min      4.5380
_shelx_estimated_absorpt_T_max   0.796
_shelx_estimated_absorpt_T_min   0.228
_exptl_absorpt_coefficient_mu    13.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange-brown
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54875
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.353
_diffrn_reflns_theta_min         4.196
_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 0.994
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  25.00   0.50    0.55    --  -47.27  76.00 -75.00  190
  2  ω   -120.00 -25.00   0.50    0.55    --  -47.27 -76.00 158.00  190
  3  ω     25.00 120.00   0.50    0.55    --   47.27  76.00 -75.00  190
  4  ω   -163.00 -69.00   0.50    2.20    --  -91.75 -76.00 158.00  188
  5  ω   -100.00 -19.00   0.50    2.20    --  -91.75  76.00 -75.00  162
  6  ω     42.00 114.00   0.50    2.20    --  113.25 -76.00 158.00  144
  7  ω     91.00 178.00   0.50    2.20    --  113.25  76.00 -75.00  174
  8  ω    -16.00  28.00   0.50    0.55    --  -47.27  19.00 -60.00   88
  9  ω    -35.00  26.00   0.50    0.55    --  -47.27  38.00-120.00  122
 10  ω    -16.00  28.00   0.50    0.55    --  -47.27  19.00  90.00   88
 11  ω   -120.00 -73.00   0.50    0.55    --  -47.27-125.00-120.00   94
 12  ω    -86.00 -13.00   0.50    0.55    --  -47.27 125.00-180.00  146
 13  ω    -16.00  28.00   0.50    0.55    --  -47.27  19.00-150.00   88
 14  ω    -24.00  70.00   0.50    0.55    --   47.27 -76.00 158.00  188
 15  ω    -65.00 -19.00   0.50    2.20    --  -91.75  61.00 120.00   92
 16  ω    -65.00 -19.00   0.50    2.20    --  -91.75  61.00  60.00   92
 17  ω    -65.00 -19.00   0.50    2.20    --  -91.75  61.00  90.00   92
 18  ω    101.00 178.00   0.50    2.20    --  113.25  30.00-120.00  154
 19  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00 120.00  128
 20  ω     42.00 111.00   0.50    2.20    --  113.25-125.00  90.00  138
 21  ω    101.00 178.00   0.50    2.20    --  113.25  45.00  90.00  154
 22  ω     42.00 111.00   0.50    2.20    --  113.25-125.00  30.00  138
 23  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00  75.43  128
 24  ω    101.00 178.00   0.50    2.20    --  113.25  30.00 -90.00  154
 25  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00-150.00  128
 26  ω     42.00  79.00   0.50    2.20    --  113.25 -61.00   0.00   74
 27  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00 -90.00  128
 28  ω     42.00  79.00   0.50    2.20    --  113.25 -61.00 -60.00   74
 29  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00 150.00  128
 30  ω    101.00 178.00   0.50    2.20    --  113.25  30.00 150.00  154
 31  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00 -60.00  128
 32  ω     42.00 108.00   0.50    2.20    --  113.25-110.00  67.62  132
 33  ω     42.00  79.00   0.50    2.20    --  113.25 -61.00 150.00   74
 34  ω     97.00 178.00   0.50    2.20    --  113.25  61.00-150.00  162
 35  ω     42.00 111.00   0.50    2.20    --  113.25-125.00 -90.00  138
 36  ω    101.00 178.00   0.50    2.20    --  113.25  45.00   0.00  154
 37  ω     42.00 136.00   0.50    2.20    --  113.25 -77.00  30.00  188
 38  ω    101.00 178.00   0.50    2.20    --  113.25  45.00 -60.00  154
 39  ω     42.00  79.00   0.50    2.20    --  113.25 -61.00-120.00   74
 40  ω     95.00 178.00   0.50    2.20    --  113.25 125.00 120.00  166
 41  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00-120.00  128
 42  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00 -30.00  128
 43  ω     42.00 106.00   0.50    2.20    --  113.25 -94.00  90.00  128
 44  ω    100.00 178.00   0.50    2.20    --  113.25  15.00-150.00  156
 45  ω   -120.00 -25.00   0.50    0.55    --  -47.27 -77.00-150.00  190
 46  ω   -120.00 -25.00   0.50    0.55    --  -47.27 -77.00 120.00  190
 47  ω   -120.00 -35.00   0.50    0.55    --  -47.27 -38.00 -90.00  170
 48  ω   -120.00 -32.00   0.50    0.55    --  -47.27 -57.00  30.00  176
 49  ω   -120.00 -32.00   0.50    0.55    --  -47.27 -57.00-150.00  176
 50  ω   -120.00 -25.00   0.50    0.55    --  -47.27 -77.00 -30.00  190
 51  ω     25.00 120.00   0.50    0.55    --   47.27  77.00-150.00  190
 52  ω     32.00 120.00   0.50    0.55    --   47.27  57.00   0.00  176
 53  ω     25.00 120.00   0.50    0.55    --   47.27  77.00  90.00  190
 54  ω     25.00 120.00   0.50    0.55    --   47.27  77.00  30.00  190
 55  ω   -163.00 -70.00   0.50    2.20    --  -91.75 -75.00  42.97  186
 56  ω   -163.00 -71.00   0.50    2.20    --  -91.75 -73.00  98.49  184
 57  ω   -163.00 -73.00   0.50    2.20    --  -91.75 -67.00 -29.70  180
 58  ω   -163.00 -69.00   0.50    2.20    --  -91.75 -77.00-155.90  188
 59  ω   -163.00 -71.00   0.50    2.20    --  -91.75 -71.00 126.01  184
 60  ω   -163.00 -69.00   0.50    2.20    --  -91.75 -76.00  72.69  188
 61  ω   -163.00 -70.00   0.50    2.20    --  -91.75 -74.00 -56.55  186
 62  ω   -163.00 -69.00   0.50    2.20    --  -91.75 -76.00   7.19  188
 63  ω   -163.00 -69.00   0.50    2.20    --  -91.75 -77.00 -96.86  188
 64  ω    101.00 178.00   0.50    2.20    --  113.25  45.00 -30.00  154
 65  ω    100.00 178.00   0.50    2.20    --  113.25  15.00  60.00  156
;
_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      0.1153846000
_diffrn_orient_matrix_UB_12      -0.0415069000
_diffrn_orient_matrix_UB_13      0.0524093000
_diffrn_orient_matrix_UB_21      -0.0077842000
_diffrn_orient_matrix_UB_22      0.1296234000
_diffrn_orient_matrix_UB_23      0.0464566000
_diffrn_orient_matrix_UB_31      -0.1207091000
_diffrn_orient_matrix_UB_32      -0.0534199000
_diffrn_orient_matrix_UB_33      0.0463914000
_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                6585
_reflns_number_total             7646
_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 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7646
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0360
_refine_ls_restrained_S_all      1.116
_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)+(0.0460P)²+1.9749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1030
_refine_special_details          
;
Both tetrahydrofuran molecules of crystallization are modeled
as disordered over two positions each: O20/C13-C16,
0.50(1):0.50(1), O21/C17-C20, 0.80(1):0.20(1). Analogous bond
lengths and angles between the two positions of each disordered
tetrahydrofuran molecule were restrained to be similar.
Anisotropic displacement parameters for proximal atoms were
restrained to be similar and some were restrained toward the
expected motion relative to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C13-C14 \\sim C13-C14' \\sim C14-C15 \\sim C14'-C15' \\sim C15-C16 \\sim
C15'-C16
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1A
4. Rigid body (RIGU) restrains
 O21, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O21, C20, C19, C18, C17} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21, C17, C18, C19, C20}
{O21, C17, C18, C19, C20} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21', C17', C18', C19', C20'}
6. Others
 Sof(O21')=Sof(C17')=Sof(H17C)=Sof(H17D)=Sof(C18')=Sof(H18C)=Sof(H18D)=
 Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(O21)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(1)
 Sof(H13C)=Sof(H13D)=Sof(H16C)=Sof(H16D)=Sof(C14')=Sof(H14C)=Sof(H14D)=
 Sof(C15')=Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H16A)=Sof(H16B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13C,H13D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C16(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C17'(H17C,H17D), C18'(H18C,H18D), C19'(H19C,H19D), C20'(H20C,
 H20D), C14'(H14C,H14D), C15'(H15C,H15D)
7.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), 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)
;
_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 0.64067(4) 0.42041(4) 0.25748(2) 0.01602(10) Uani 1 1 d . . . . .
V2 V 0.34509(5) 0.33910(4) 0.17825(2) 0.01740(11) Uani 1 1 d . . . . .
V3 V 0.64502(5) 0.18161(4) 0.13994(2) 0.01822(11) Uani 1 1 d . . . . .
V4 V 0.69368(5) 0.15760(4) 0.31557(2) 0.01925(11) Uani 1 1 d . . . . .
V5 V 0.39442(5) 0.31493(4) 0.35329(2) 0.01883(11) Uani 1 1 d . . . . .
V6 V 0.38976(5) 0.06364(4) 0.23509(2) 0.02003(11) Uani 1 1 d . . . . .
O1 O 0.7589(2) 0.58974(18) 0.26566(11) 0.0246(4) Uani 1 1 d . . . . .
H1A H 0.800(4) 0.630(4) 0.304(2) 0.050(12) Uiso 1 1 d . . . . .
H1B H 0.804(5) 0.616(4) 0.232(3) 0.066(14) Uiso 1 1 d . . . . .
O2 O 0.2232(2) 0.39972(18) 0.13180(10) 0.0241(4) Uani 1 1 d . . . . .
O3 O 0.7265(2) 0.13239(18) 0.06619(10) 0.0258(4) Uani 1 1 d . . . . .
O4 O 0.8121(2) 0.09072(18) 0.36100(11) 0.0265(4) Uani 1 1 d . . . . .
O5 O 0.3070(2) 0.35804(19) 0.42605(10) 0.0275(4) Uani 1 1 d . . . . .
O6 O 0.2986(2) -0.06767(18) 0.22598(11) 0.0288(4) Uani 1 1 d . . . . .
O7 O 0.48849(19) 0.48412(16) 0.19751(9) 0.0186(4) Uani 1 1 d . . . . .
O8 O 0.74254(18) 0.34953(16) 0.16871(9) 0.0179(3) Uani 1 1 d . . . . .
O9 O 0.77840(19) 0.33191(17) 0.31524(9) 0.0199(4) Uani 1 1 d . . . . .
O10 O 0.5279(2) 0.46471(16) 0.34608(9) 0.0203(4) Uani 1 1 d . . . . .
O11 O 0.47879(19) 0.26965(17) 0.09882(9) 0.0193(4) Uani 1 1 d . . . . .
O12 O 0.7703(2) 0.11406(17) 0.21432(10) 0.0211(4) Uani 1 1 d . . . . .
O13 O 0.5601(2) 0.22679(17) 0.39507(10) 0.0223(4) Uani 1 1 d . . . . .
O14 O 0.26638(19) 0.37961(17) 0.27903(10) 0.0203(4) Uani 1 1 d . . . . .
O15 O 0.26217(19) 0.16028(17) 0.17972(10) 0.0211(4) Uani 1 1 d . . . . .
O16 O 0.5070(2) 0.03285(17) 0.14904(10) 0.0219(4) Uani 1 1 d . . . . .
O17 O 0.5459(2) 0.01339(16) 0.29423(10) 0.0224(4) Uani 1 1 d . . . . .
O18 O 0.29848(19) 0.14405(17) 0.32172(10) 0.0223(4) Uani 1 1 d . . . . .
O19 O 0.51915(18) 0.24728(15) 0.24686(9) 0.0174(4) Uani 1 1 d . . . . .
C1 C 0.4681(3) 0.6067(2) 0.17684(17) 0.0262(6) Uani 1 1 d . . . . .
H1C H 0.395751 0.650246 0.208636 0.039 Uiso 1 1 calc R U . . .
H1D H 0.434068 0.599725 0.126141 0.039 Uiso 1 1 calc R U . . .
H1E H 0.560215 0.655191 0.181383 0.039 Uiso 1 1 calc R U . . .
C2 C 0.8971(3) 0.3572(3) 0.16175(15) 0.0229(5) Uani 1 1 d . . . . .
H2A H 0.930632 0.445808 0.171990 0.034 Uiso 1 1 calc R U . . .
H2B H 0.924330 0.324559 0.112010 0.034 Uiso 1 1 calc R U . . .
H2C H 0.942063 0.306304 0.196478 0.034 Uiso 1 1 calc R U . . .
C3 C 0.8500(3) 0.3894(3) 0.37947(15) 0.0283(6) Uani 1 1 d . . . . .
H3A H 0.878890 0.476985 0.372982 0.042 Uiso 1 1 calc R U . . .
H3B H 0.936354 0.341477 0.388658 0.042 Uiso 1 1 calc R U . . .
H3C H 0.784012 0.389303 0.421003 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5393(3) 0.5687(3) 0.40084(15) 0.0296(6) Uani 1 1 d . . . . .
H4A H 0.595548 0.544667 0.442064 0.044 Uiso 1 1 calc R U . . .
H4B H 0.442008 0.593122 0.417384 0.044 Uiso 1 1 calc R U . . .
H4C H 0.588137 0.640475 0.381084 0.044 Uiso 1 1 calc R U . . .
C5 C 0.5134(3) 0.3482(3) 0.04321(14) 0.0234(5) Uani 1 1 d . . . . .
H5A H 0.424319 0.383935 0.025978 0.035 Uiso 1 1 calc R U . . .
H5B H 0.559736 0.297522 0.002484 0.035 Uiso 1 1 calc R U . . .
H5C H 0.579943 0.417246 0.062894 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8263(3) -0.0091(3) 0.19661(16) 0.0276(6) Uani 1 1 d . . . . .
H6A H 0.748836 -0.073101 0.200262 0.041 Uiso 1 1 calc R U . . .
H6B H 0.904895 -0.022336 0.230625 0.041 Uiso 1 1 calc R U . . .
H6C H 0.863852 -0.016851 0.146726 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5272(3) 0.1543(3) 0.45363(15) 0.0289(6) Uani 1 1 d . . . . .
H7A H 0.451331 0.090432 0.438200 0.043 Uiso 1 1 calc R U . . .
H7B H 0.492952 0.210653 0.495445 0.043 Uiso 1 1 calc R U . . .
H7C H 0.614591 0.112028 0.467586 0.043 Uiso 1 1 calc R U . . .
C8 C 0.2036(3) 0.5001(3) 0.29798(15) 0.0270(6) Uani 1 1 d . . . . .
H8A H 0.278344 0.567248 0.296784 0.040 Uiso 1 1 calc R U . . .
H8B H 0.162882 0.503555 0.347133 0.040 Uiso 1 1 calc R U . . .
H8C H 0.126330 0.512429 0.263045 0.040 Uiso 1 1 calc R U . . .
C9 C 0.1887(3) 0.1032(3) 0.11572(16) 0.0290(6) Uani 1 1 d . . . . .
H9A H 0.098798 0.147848 0.109026 0.043 Uiso 1 1 calc R U . . .
H9B H 0.165697 0.013889 0.120899 0.043 Uiso 1 1 calc R U . . .
H9C H 0.251282 0.108483 0.073266 0.043 Uiso 1 1 calc R U . . .
C10 C 0.4942(3) -0.0739(3) 0.09551(16) 0.0295(6) Uani 1 1 d . . . . .
H10A H 0.428012 -0.055013 0.056727 0.044 Uiso 1 1 calc R U . . .
H10B H 0.455862 -0.147204 0.118073 0.044 Uiso 1 1 calc R U . . .
H10C H 0.589851 -0.093345 0.074790 0.044 Uiso 1 1 calc R U . . .
C11 C 0.5509(3) -0.1040(3) 0.32479(17) 0.0304(6) Uani 1 1 d . . . . .
H11A H 0.639425 -0.105574 0.354216 0.046 Uiso 1 1 calc R U . . .
H11B H 0.550995 -0.174247 0.285475 0.046 Uiso 1 1 calc R U . . .
H11C H 0.465874 -0.113090 0.355685 0.046 Uiso 1 1 calc R U . . .
C12 C 0.1433(3) 0.1356(3) 0.32859(16) 0.0278(6) Uani 1 1 d . . . . .
H12A H 0.116485 0.158058 0.379656 0.042 Uiso 1 1 calc R U . . .
H12B H 0.109067 0.048669 0.312518 0.042 Uiso 1 1 calc R U . . .
H12C H 0.098445 0.194255 0.298263 0.042 Uiso 1 1 calc R U . . .
O20 O 0.8980(2) 0.68585(19) 0.15472(10) 0.0274(4) Uani 1 1 d . . . . .
C13 C 0.8283(3) 0.6647(4) 0.08518(16) 0.0358(7) Uani 1 1 d D . . . .
H13A H 0.733485 0.706578 0.086259 0.043 Uiso 0.797(10) 1 calc R U P A 1
H13B H 0.812398 0.572759 0.070365 0.043 Uiso 0.797(10) 1 calc R U P A 1
H13C H 0.786883 0.743533 0.070835 0.043 Uiso 0.203(10) 1 calc R U P A 2
H13D H 0.750951 0.597996 0.084183 0.043 Uiso 0.203(10) 1 calc R U P A 2
C14 C 0.9312(4) 0.7222(4) 0.0332(2) 0.0347(12) Uani 0.797(10) 1 d D . P A 1
H14A H 0.922907 0.815578 0.036391 0.042 Uiso 0.797(10) 1 calc R U P A 1
H14B H 0.914555 0.684964 -0.017849 0.042 Uiso 0.797(10) 1 calc R U P A 1
C15 C 1.0772(6) 0.6846(7) 0.0624(2) 0.0406(16) Uani 0.797(10) 1 d D U P A 1
H15A H 1.097644 0.594642 0.046513 0.049 Uiso 0.797(10) 1 calc R U P A 1
H15B H 1.157678 0.739299 0.047268 0.049 Uiso 0.797(10) 1 calc R U P A 1
C16 C 1.0515(3) 0.7071(3) 0.14433(16) 0.0324(6) Uani 1 1 d D . . . .
H16A H 1.108203 0.647486 0.170047 0.039 Uiso 0.797(10) 1 calc R U P A 1
H16B H 1.080926 0.794960 0.163445 0.039 Uiso 0.797(10) 1 calc R U P A 1
H16C H 1.106899 0.632138 0.154384 0.039 Uiso 0.203(10) 1 calc R U P A 2
H16D H 1.088184 0.782182 0.176455 0.039 Uiso 0.203(10) 1 calc R U P A 2
O21 O 0.9162(18) 0.717(2) 0.3704(9) 0.036(3) Uani 0.498(9) 1 d D U P B 1
C17 C 1.035(2) 0.7865(19) 0.3448(7) 0.025(3) Uani 0.498(9) 1 d D U P B 1
H17A H 1.000889 0.864311 0.325832 0.030 Uiso 0.498(9) 1 calc R U P B 1
H17B H 1.083750 0.734259 0.304582 0.030 Uiso 0.498(9) 1 calc R U P B 1
C18 C 1.1397(19) 0.821(3) 0.4063(8) 0.033(3) Uani 0.498(9) 1 d D U P B 1
H18A H 1.237617 0.789306 0.394035 0.040 Uiso 0.498(9) 1 calc R U P B 1
H18B H 1.146341 0.914155 0.419533 0.040 Uiso 0.498(9) 1 calc R U P B 1
C19 C 1.0738(9) 0.7562(7) 0.4658(3) 0.049(2) Uani 0.498(9) 1 d D . P B 1
H19A H 1.117134 0.672264 0.467919 0.058 Uiso 0.498(9) 1 calc R U P B 1
H19B H 1.088832 0.807754 0.513424 0.058 Uiso 0.498(9) 1 calc R U P B 1
C20 C 0.9177(13) 0.7417(18) 0.4478(8) 0.058(4) Uani 0.498(9) 1 d D U P B 1
H20A H 0.872749 0.669934 0.470392 0.069 Uiso 0.498(9) 1 calc R U P B 1
H20B H 0.865796 0.820170 0.464337 0.069 Uiso 0.498(9) 1 calc R U P B 1
O21' O 0.8898(18) 0.739(2) 0.3778(9) 0.035(3) Uani 0.502(9) 1 d D U P B 2
C17' C 1.0062(19) 0.806(2) 0.3483(8) 0.028(3) Uani 0.502(9) 1 d D U P B 2
H17C H 0.972323 0.886516 0.332121 0.034 Uiso 0.502(9) 1 calc R U P B 2
H17D H 1.048646 0.754547 0.306117 0.034 Uiso 0.502(9) 1 calc R U P B 2
C18' C 1.1168(18) 0.833(3) 0.4090(8) 0.036(3) Uani 0.502(9) 1 d D U P B 2
H18C H 1.171607 0.757223 0.417390 0.043 Uiso 0.502(9) 1 calc R U P B 2
H18D H 1.185085 0.903841 0.400571 0.043 Uiso 0.502(9) 1 calc R U P B 2
C19' C 1.0127(8) 0.8700(8) 0.4689(3) 0.045(2) Uani 0.502(9) 1 d D . P B 2
H19C H 0.979970 0.957747 0.467044 0.054 Uiso 0.502(9) 1 calc R U P B 2
H19D H 1.057391 0.863681 0.517143 0.054 Uiso 0.502(9) 1 calc R U P B 2
C20' C 0.8891(14) 0.7761(18) 0.4544(9) 0.056(4) Uani 0.502(9) 1 d D U P B 2
H20C H 0.902856 0.701690 0.481500 0.067 Uiso 0.502(9) 1 calc R U P B 2
H20D H 0.796090 0.815323 0.469498 0.067 Uiso 0.502(9) 1 calc R U P B 2
C14' C 0.9574(13) 0.6209(17) 0.0362(8) 0.046(6) Uani 0.203(10) 1 d D . P A 2
H14C H 0.992353 0.536922 0.046035 0.055 Uiso 0.203(10) 1 calc R U P A 2
H14D H 0.934927 0.619998 -0.016384 0.055 Uiso 0.203(10) 1 calc R U P A 2
C15' C 1.063(3) 0.7292(18) 0.0641(5) 0.034(4) Uani 0.203(10) 1 d D U P A 2
H15C H 1.027803 0.813382 0.054666 0.041 Uiso 0.203(10) 1 calc R U P A 2
H15D H 1.161962 0.716949 0.044622 0.041 Uiso 0.203(10) 1 calc R U P A 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 2.0671(19) . ?
V1 O7 1.9636(18) . ?
V1 O8 1.9756(17) . ?
V1 O9 1.9763(18) . ?
V1 O10 1.9597(18) . ?
V1 O19 2.1158(16) . ?
V2 O2 1.6013(19) . ?
V2 O7 2.0021(17) . ?
V2 O11 2.0072(18) . ?
V2 O14 2.0041(18) . ?
V2 O15 2.0293(18) . ?
V2 O19 2.3386(17) . ?
V3 O3 1.5992(19) . ?
V3 O8 1.9913(17) . ?
V3 O11 2.0053(18) . ?
V3 O12 1.9956(18) . ?
V3 O16 2.0229(18) . ?
V3 O19 2.3400(17) . ?
V4 O4 1.6012(19) . ?
V4 O9 1.9888(18) . ?
V4 O12 2.0091(18) . ?
V4 O13 2.0068(19) . ?
V4 O17 2.0259(18) . ?
V4 O19 2.3316(17) . ?
V5 O5 1.5973(19) . ?
V5 O10 2.0002(18) . ?
V5 O13 2.0068(19) . ?
V5 O14 1.9958(18) . ?
V5 O18 2.0210(18) . ?
V5 O19 2.3319(17) . ?
V6 O6 1.5999(19) . ?
V6 O15 1.9408(19) . ?
V6 O16 1.9262(19) . ?
V6 O17 1.9252(19) . ?
V6 O18 1.9322(19) . ?
V6 O19 2.2464(16) . ?
O1 H1A 0.87(4) . ?
O1 H1B 0.82(5) . ?
O7 C1 1.412(3) . ?
O8 C2 1.432(3) . ?
O9 C3 1.423(3) . ?
O10 C4 1.412(3) . ?
O11 C5 1.424(3) . ?
O12 C6 1.422(3) . ?
O13 C7 1.423(3) . ?
O14 C8 1.425(3) . ?
O15 C9 1.426(3) . ?
O16 C10 1.420(3) . ?
O17 C11 1.425(3) . ?
O18 C12 1.438(3) . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
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 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
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 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 . ?
O20 C13 1.426(3) . ?
O20 C16 1.444(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 H13C 0.9900 . ?
C13 H13D 0.9900 . ?
C13 C14 1.516(4) . ?
C13 C14' 1.547(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.528(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.524(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 H16C 0.9900 . ?
C16 H16D 0.9900 . ?
C16 C15' 1.529(8) . ?
O21 C17 1.416(11) . ?
O21 C20 1.423(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.495(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.483(17) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.475(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O21' C17' 1.416(10) . ?
O21' C20' 1.425(10) . ?
C17' H17C 0.9900 . ?
C17' H17D 0.9900 . ?
C17' C18' 1.510(11) . ?
C18' H18C 0.9900 . ?
C18' H18D 0.9900 . ?
C18' C19' 1.491(17) . ?
C19' H19C 0.9900 . ?
C19' H19D 0.9900 . ?
C19' C20' 1.498(12) . ?
C20' H20C 0.9900 . ?
C20' H20D 0.9900 . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
C14' C15' 1.528(8) . ?
C15' H15C 0.9900 . ?
C15' H15D 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
O1 V1 O19 178.87(7) . . ?
O7 V1 O1 93.15(8) . . ?
O7 V1 O8 90.44(7) . . ?
O7 V1 O9 171.55(7) . . ?
O7 V1 O19 86.08(7) . . ?
O8 V1 O1 93.52(8) . . ?
O8 V1 O9 88.22(7) . . ?
O8 V1 O19 85.66(7) . . ?
O9 V1 O1 95.26(8) . . ?
O9 V1 O19 85.51(7) . . ?
O10 V1 O1 94.92(8) . . ?
O10 V1 O7 90.88(8) . . ?
O10 V1 O8 171.37(7) . . ?
O10 V1 O9 89.22(8) . . ?
O10 V1 O19 85.92(7) . . ?
O2 V2 O7 101.73(9) . . ?
O2 V2 O11 100.96(9) . . ?
O2 V2 O14 100.15(9) . . ?
O2 V2 O15 100.84(9) . . ?
O2 V2 O19 178.71(8) . . ?
O7 V2 O11 86.63(7) . . ?
O7 V2 O14 89.51(7) . . ?
O7 V2 O15 157.39(8) . . ?
O7 V2 O19 79.45(6) . . ?
O11 V2 O15 87.88(8) . . ?
O11 V2 O19 79.58(7) . . ?
O14 V2 O11 158.89(8) . . ?
O14 V2 O15 87.76(8) . . ?
O14 V2 O19 79.31(7) . . ?
O15 V2 O19 77.99(6) . . ?
O3 V3 O8 102.64(9) . . ?
O3 V3 O11 99.92(9) . . ?
O3 V3 O12 101.27(9) . . ?
O3 V3 O16 100.37(9) . . ?
O3 V3 O19 177.79(8) . . ?
O8 V3 O11 89.55(7) . . ?
O8 V3 O12 86.84(7) . . ?
O8 V3 O16 156.96(7) . . ?
O8 V3 O19 79.53(6) . . ?
O11 V3 O16 87.68(8) . . ?
O11 V3 O19 79.59(6) . . ?
O12 V3 O11 158.78(8) . . ?
O12 V3 O16 87.53(8) . . ?
O12 V3 O19 79.20(7) . . ?
O16 V3 O19 77.48(7) . . ?
O4 V4 O9 102.28(9) . . ?
O4 V4 O12 99.70(9) . . ?
O4 V4 O13 101.36(9) . . ?
O4 V4 O17 100.61(9) . . ?
O4 V4 O19 177.76(8) . . ?
O9 V4 O12 88.95(7) . . ?
O9 V4 O13 88.20(8) . . ?
O9 V4 O17 157.10(8) . . ?
O9 V4 O19 79.66(7) . . ?
O12 V4 O17 87.94(8) . . ?
O12 V4 O19 79.14(7) . . ?
O13 V4 O12 158.87(8) . . ?
O13 V4 O17 86.59(8) . . ?
O13 V4 O19 79.75(7) . . ?
O17 V4 O19 77.47(7) . . ?
O5 V5 O10 101.95(9) . . ?
O5 V5 O13 100.16(9) . . ?
O5 V5 O14 100.43(9) . . ?
O5 V5 O18 101.12(9) . . ?
O5 V5 O19 178.62(8) . . ?
O10 V5 O13 88.50(8) . . ?
O10 V5 O18 156.85(8) . . ?
O10 V5 O19 79.42(6) . . ?
O13 V5 O18 89.37(8) . . ?
O13 V5 O19 79.75(7) . . ?
O14 V5 O10 88.51(8) . . ?
O14 V5 O13 159.37(8) . . ?
O14 V5 O18 85.43(8) . . ?
O14 V5 O19 79.64(7) . . ?
O18 V5 O19 77.51(7) . . ?
O6 V6 O15 97.96(9) . . ?
O6 V6 O16 97.65(9) . . ?
O6 V6 O17 98.35(9) . . ?
O6 V6 O18 99.19(9) . . ?
O6 V6 O19 179.40(10) . . ?
O15 V6 O19 82.08(7) . . ?
O16 V6 O15 88.17(8) . . ?
O16 V6 O18 162.97(8) . . ?
O16 V6 O19 81.75(7) . . ?
O17 V6 O15 163.67(8) . . ?
O17 V6 O16 90.42(8) . . ?
O17 V6 O18 89.66(8) . . ?
O17 V6 O19 81.61(7) . . ?
O18 V6 O15 86.99(8) . . ?
O18 V6 O19 81.41(7) . . ?
V1 O1 H1A 128(3) . . ?
V1 O1 H1B 124(3) . . ?
H1A O1 H1B 103(4) . . ?
V1 O7 V2 104.84(8) . . ?
C1 O7 V1 130.53(16) . . ?
C1 O7 V2 124.31(16) . . ?
V1 O8 V3 105.00(8) . . ?
C2 O8 V1 122.63(15) . . ?
C2 O8 V3 117.29(15) . . ?
V1 O9 V4 104.96(8) . . ?
C3 O9 V1 123.92(17) . . ?
C3 O9 V4 118.37(16) . . ?
V1 O10 V5 104.95(8) . . ?
C4 O10 V1 131.65(16) . . ?
C4 O10 V5 123.06(16) . . ?
V3 O11 V2 110.93(8) . . ?
C5 O11 V2 117.51(15) . . ?
C5 O11 V3 116.32(15) . . ?
V3 O12 V4 111.44(9) . . ?
C6 O12 V3 117.39(16) . . ?
C6 O12 V4 117.62(16) . . ?
V5 O13 V4 110.49(8) . . ?
C7 O13 V4 119.79(17) . . ?
C7 O13 V5 116.76(17) . . ?
V5 O14 V2 111.16(8) . . ?
C8 O14 V2 118.73(16) . . ?
C8 O14 V5 117.14(16) . . ?
V6 O15 V2 109.76(8) . . ?
C9 O15 V2 117.55(16) . . ?
C9 O15 V6 121.36(16) . . ?
V6 O16 V3 110.63(8) . . ?
C10 O16 V3 123.20(17) . . ?
C10 O16 V6 126.02(17) . . ?
V6 O17 V4 110.54(8) . . ?
C11 O17 V4 124.16(17) . . ?
C11 O17 V6 125.04(17) . . ?
V6 O18 V5 110.57(8) . . ?
C12 O18 V5 116.62(16) . . ?
C12 O18 V6 119.57(16) . . ?
V1 O19 V2 89.61(6) . . ?
V1 O19 V3 89.72(6) . . ?
V1 O19 V4 89.87(6) . . ?
V1 O19 V5 89.71(6) . . ?
V1 O19 V6 179.74(9) . . ?
V2 O19 V3 89.90(6) . . ?
V4 O19 V2 179.46(8) . . ?
V4 O19 V3 90.20(6) . . ?
V4 O19 V5 90.00(6) . . ?
V5 O19 V2 89.89(6) . . ?
V5 O19 V3 179.40(8) . . ?
V6 O19 V2 90.17(6) . . ?
V6 O19 V3 90.14(6) . . ?
V6 O19 V4 90.35(6) . . ?
V6 O19 V5 90.43(6) . . ?
O7 C1 H1C 109.5 . . ?
O7 C1 H1D 109.5 . . ?
O7 C1 H1E 109.5 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 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 . . ?
C13 O20 C16 109.0(2) . . ?
O20 C13 H13A 110.7 . . ?
O20 C13 H13B 110.7 . . ?
O20 C13 H13C 111.6 . . ?
O20 C13 H13D 111.6 . . ?
O20 C13 C14 105.2(2) . . ?
O20 C13 C14' 100.8(7) . . ?
H13A C13 H13B 108.8 . . ?
H13C C13 H13D 109.4 . . ?
C14 C13 H13A 110.7 . . ?
C14 C13 H13B 110.7 . . ?
C14' C13 H13C 111.6 . . ?
C14' C13 H13D 111.6 . . ?
C13 C14 H14A 111.6 . . ?
C13 C14 H14B 111.6 . . ?
C13 C14 C15 100.6(3) . . ?
H14A C14 H14B 109.4 . . ?
C15 C14 H14A 111.6 . . ?
C15 C14 H14B 111.6 . . ?
C14 C15 H15A 111.6 . . ?
C14 C15 H15B 111.6 . . ?
H15A C15 H15B 109.4 . . ?
C16 C15 C14 100.8(3) . . ?
C16 C15 H15A 111.6 . . ?
C16 C15 H15B 111.6 . . ?
O20 C16 C15 106.3(3) . . ?
O20 C16 H16A 110.5 . . ?
O20 C16 H16B 110.5 . . ?
O20 C16 H16C 111.0 . . ?
O20 C16 H16D 111.0 . . ?
O20 C16 C15' 103.7(10) . . ?
C15 C16 H16A 110.5 . . ?
C15 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
H16C C16 H16D 109.0 . . ?
C15' C16 H16C 111.0 . . ?
C15' C16 H16D 111.0 . . ?
C17 O21 C20 107.0(10) . . ?
O21 C17 H17A 109.9 . . ?
O21 C17 H17B 109.9 . . ?
O21 C17 C18 108.8(10) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
C17 C18 H18A 111.3 . . ?
C17 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
C19 C18 C17 102.3(10) . . ?
C19 C18 H18A 111.3 . . ?
C19 C18 H18B 111.3 . . ?
C18 C19 H19A 110.6 . . ?
C18 C19 H19B 110.6 . . ?
H19A C19 H19B 108.8 . . ?
C20 C19 C18 105.5(10) . . ?
C20 C19 H19A 110.6 . . ?
C20 C19 H19B 110.6 . . ?
O21 C20 C19 103.3(9) . . ?
O21 C20 H20A 111.1 . . ?
O21 C20 H20B 111.1 . . ?
C19 C20 H20A 111.1 . . ?
C19 C20 H20B 111.1 . . ?
H20A C20 H20B 109.1 . . ?
C17' O21' C20' 107.3(10) . . ?
O21' C17' H17C 110.5 . . ?
O21' C17' H17D 110.5 . . ?
O21' C17' C18' 106.0(10) . . ?
H17C C17' H17D 108.7 . . ?
C18' C17' H17C 110.5 . . ?
C18' C17' H17D 110.5 . . ?
C17' C18' H18C 112.3 . . ?
C17' C18' H18D 112.3 . . ?
H18C C18' H18D 109.9 . . ?
C19' C18' C17' 97.2(11) . . ?
C19' C18' H18C 112.3 . . ?
C19' C18' H18D 112.3 . . ?
C18' C19' H19C 111.0 . . ?
C18' C19' H19D 111.0 . . ?
C18' C19' C20' 103.9(10) . . ?
H19C C19' H19D 109.0 . . ?
C20' C19' H19C 111.0 . . ?
C20' C19' H19D 111.0 . . ?
O21' C20' C19' 105.6(9) . . ?
O21' C20' H20C 110.6 . . ?
O21' C20' H20D 110.6 . . ?
C19' C20' H20C 110.6 . . ?
C19' C20' H20D 110.6 . . ?
H20C C20' H20D 108.7 . . ?
C13 C14' H14C 112.4 . . ?
C13 C14' H14D 112.4 . . ?
H14C C14' H14D 110.0 . . ?
C15' C14' C13 96.7(13) . . ?
C15' C14' H14C 112.4 . . ?
C15' C14' H14D 112.4 . . ?
C16 C15' H15C 112.7 . . ?
C16 C15' H15D 112.7 . . ?
C14' C15' C16 95.4(9) . . ?
C14' C15' H15C 112.7 . . ?
C14' C15' H15D 112.7 . . ?
H15C C15' H15D 110.1 . . ?

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
O1 H1A O21 0.87(4) 1.79(5) 2.640(14) 168(4) . yes
O1 H1A O21' 0.87(4) 1.86(5) 2.720(13) 171(4) . yes
O1 H1B O20 0.82(5) 1.88(5) 2.700(3) 175(5) . 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
O20 C13 C14 C15 38.9(4) . . . . ?
O20 C13 C14' C15' -49.4(12) . . . . ?
O20 C16 C15' C14' -43.6(15) . . . . ?
C13 O20 C16 C15 -5.6(4) . . . . ?
C13 O20 C16 C15' 13.4(9) . . . . ?
C13 C14 C15 C16 -40.6(5) . . . . ?
C13 C14' C15' C16 55.4(16) . . . . ?
C14 C15 C16 O20 29.4(5) . . . . ?
C16 O20 C13 C14 -21.2(4) . . . . ?
C16 O20 C13 C14' 22.5(7) . . . . ?
O21 C17 C18 C19 4(2) . . . . ?
C17 O21 C20 C19 -33(2) . . . . ?
C17 C18 C19 C20 -25(2) . . . . ?
C18 C19 C20 O21 36(2) . . . . ?
C20 O21 C17 C18 18(2) . . . . ?
O21' C17' C18' C19' -42(2) . . . . ?
C17' O21' C20' C19' 0(2) . . . . ?
C17' C18' C19' C20' 41(2) . . . . ?
C18' C19' C20' O21' -27(2) . . . . ?
C20' O21' C17' C18' 27(2) . . . . ?

_olex2_submission_original_sample_id mates22
_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 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.619
