# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 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_mates15
_database_code_depnum_ccdc_archive 'CCDC 2215270'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;

_vrf_PLAT341_mates15             
;
PROBLEM: _B Low Bond Precision on C-C Bonds ...............     0.0169 Ang. 
RESPONSE: All crystals examined resulted in medium-to-low quality
structures. However, the connectivity and identification of the
charged species are unambiguious.
;

_vrf_DIFMX02_mates15             
;
PROBLEM: _C  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
RESPONSE: The largest residual peak is located 0.92 \%A from
atom Co2. It is likely a cobalt position of a third component
of disorder, which was not modeled.
;

_vrf_PLAT097_mates15             
;
PROBLEM: _C Large Reported Max.  (Positive) Residual Density .. 2.39 eA-3 
RESPONSE: The largest residual peak is located 0.92 \%A from
atom Co2. It is likely a cobalt position of a third component
of disorder, which was not modeled.
;

_vrf_PLAT301_mates15             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 3% 
RESPONSE: Methoxy ligand O8-C1 is modeled as disordered over two
positions (0.68(6):0.32(6)).
;

_vrf_PLAT302_mates15             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  3-4) .. 100% 
RESPONSE: Cobaltocenium cation Co2 is modeled as disordered over
two positions (0.742(5):0.258(5)).
;

_vrf_PLAT605_mates15             
;
PROBLEM: _G Largest Solvent Accessible VOID in the Structure .. 199 A**3 
RESPONSE: Reflection contributions from highly disordered solvent
were fixed and added to the calculated structure factors using
the SQUEEZE routine of program Platon (Spek, 2015), which
determined there to be 718 electrons in 2607 \%A^3^ per unit cell
that were treated this way. Because the exact identity and amount
of solvent were unknown, no solvent was included in the atom list
or molecular formula. Thus all calculated quantities that derive
from the molecular formula (e.g., F(000), density, molecular
weight, etc.) are known to be inaccurate.
;

_vrf_PLAT860_mates15             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 999 
RESPONSE: For the various disordered species, analogous bond lengths
and angles were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar and
restrained toward the expected motion relative to bond direction.
;

_vrf_PLAT869_mates15             
;
PROBLEM: _G ALERTS Related to the Use of SQUEEZE Suppressed! 
RESPONSE: Reflection contributions from highly disordered solvent
were fixed and added to the calculated structure factors using
the SQUEEZE routine of program Platon (Spek, 2015), which
determined there to be 718 electrons in 2607 \%A^3^ per unit cell
that were treated this way. Because the exact identity and amount
of solvent were unknown, no solvent was included in the atom list
or molecular formula. Thus all calculated quantities that derive
from the molecular formula (e.g., F(000), density, molecular
weight, etc.) are known to be inaccurate.
;

_audit_creation_date             2022-03-10
_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         'C11 H33 O19 V6, 2(C10 H10 Co)'
_chemical_formula_sum            'C31 H53 Co2 O19 V6'
_chemical_formula_weight         1153.23
_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'
Co Co -2.3653 3.6143 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   16.8845(2)
_cell_length_b                   41.3260(6)
_cell_length_c                   14.1744(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9890.5(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    21249
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      79.2940
_cell_measurement_theta_min      3.2760
_shelx_estimated_absorpt_T_max   0.329
_shelx_estimated_absorpt_T_min   0.073
_exptl_absorpt_coefficient_mu    14.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08671
_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            'dark blue'
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.097
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67691
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.473
_diffrn_reflns_theta_min         3.296
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(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 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -64.00   0.50    5.38    --  -47.27-139.00-117.00  112
  2  ω    -70.00  25.00   0.50    5.38    --  -47.27  76.00-112.00  190
  3  ω    101.00 178.00   0.50   21.53    --  113.25  44.00  76.00  154
  4  ω     42.00 136.00   0.50   21.53    --  113.25 -76.00 121.00  188
  5  ω     91.00 178.00   0.50   21.53    --  113.25 131.00 128.00  174
  6  ω   -120.00 -73.00   0.50    5.38    --  -47.27-125.00  90.00   94
  7  ω     -3.00  28.00   0.50    5.38    --  -47.27  19.00 150.00   62
  8  ω     -3.00  28.00   0.50    5.38    --  -47.27  19.00 -60.00   62
  9  ω     42.00 106.00   0.50   21.53    --  113.25 -94.00  60.00  128
 10  ω     42.00  80.00   0.50   21.53    --  113.25 -61.00   0.00   76
 11  ω     42.00 106.00   0.50   21.53    --  113.25 -94.00 -90.00  128
 12  ω     42.00 111.00   0.50   21.53    --  113.25-125.00 150.00  138
 13  ω     42.00  80.00   0.50   21.53    --  113.25 -61.00  60.00   76
 14  ω    101.00 178.00   0.50   21.53    --  113.25  45.00-150.00  154
 15  ω     42.00  80.00   0.50   21.53    --  113.25 -61.00-150.00   76
 16  ω     42.00 122.00   0.50   21.53    --  113.25-139.00-117.00  160
 17  ω     25.00 103.00   0.50    5.38    --   47.27  77.00 -30.00  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      -0.0504438000
_diffrn_orient_matrix_UB_12      -0.0021262000
_diffrn_orient_matrix_UB_13      -0.0903236000
_diffrn_orient_matrix_UB_21      -0.0007227000
_diffrn_orient_matrix_UB_22      0.0371963000
_diffrn_orient_matrix_UB_23      -0.0069025000
_diffrn_orient_matrix_UB_31      0.0760416000
_diffrn_orient_matrix_UB_32      -0.0010721000
_diffrn_orient_matrix_UB_33      -0.0600641000
_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                7616
_reflns_number_total             10664
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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         2.392
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         10664
_refine_ls_number_restraints     999
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0854
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1734P)²+15.1708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2566
_refine_ls_wR_factor_ref         0.2815
_refine_special_details          
;
Reflection contributions from highly disordered solvent
were fixed and added to the calculated structure factors using
the SQUEEZE routine of program Platon (Spek, 2015), which
determined there to be 718 electrons in 2607 Å³ per unit cell
that were treated this way. Because the exact identity and amount
of solvent were unknown, no solvent was included in the atom list
or molecular formula. Thus all calculated quantities that derive
from the molecular formula (e.g., F(000), density, molecular
weight, etc.) are known to be inaccurate.

Methoxy ligand O8-C1 is modeled as disordered over two positions
(0.68(6):0.32(6)). Cobaltocenium cation Co2 is modeled as
disordered over two positions (0.742(5):0.258(5)). Analogous
bond lengths and angles were restrained to be similar.
Anisotropic displacement parameters for proximal atoms were
restrained to be similar and restrained toward the expected
motion relative to bond direction.
;
_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. Restrained distances
 Co2-C22 \\sim Co2-C23 \\sim Co2-C24 \\sim Co2-C25 \\sim Co2-C26 \\sim Co2-C27
\\sim Co2-C28 \\sim Co2-C29
 \\sim Co2-C30 \\sim Co2-C31 \\sim Co2'-C22' \\sim Co2'-C23' \\sim Co2'-C24'
\\sim Co2'-C25' \\sim Co2'-
 C26' \\sim Co2'-C27' \\sim Co2'-C28' \\sim Co2'-C29' \\sim Co2'-C30' \\sim
Co2'-C31'
 with sigma of 0.01
 C22-C27 \\sim C23-C28 \\sim C24-C29 \\sim C25-C30 \\sim C26-C31
 with sigma of 0.04
 C22'-C27' \\sim C23'-C28' \\sim C24'-C29' \\sim C25'-C30' \\sim C26'-C31'
 with sigma of 0.04
 O8-C1 \\sim O8-C1'
 with sigma of 0.01
3. Restrained planarity
 C22, C23, C24, C25, C26
 with sigma of 0.04
 C22', C23', C24', C25', C26'
 with sigma of 0.04
 C27, C28, C29, C30, C31
 with sigma of 0.04
 C27', C28', C29', C30', C31'
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
5. Rigid body (RIGU) restrains
 Co2, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Co2', C22', C23', C24', C25', C26', C27', C28', C29', C30', C31'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, C1'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C23, C24, C25, C26, C22} sigma for 1-2: 0.02, 1-3: 0.04
{C26, C25, C24, C23, C22} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C22, C23, C24, C25, C26}
{C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C27, C28, C29, C30, C31}
{C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C22', C23', C24', C25', C26'}
{C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C27', C28', C29', C30', C31'}
7. Others
 Sof(Co2')=Sof(C22')=Sof(H22')=Sof(C23')=Sof(H23')=Sof(C24')=Sof(H24')=
 Sof(C25')=Sof(H25')=Sof(C26')=Sof(H26')=Sof(C27')=Sof(H27')=Sof(C28')=
 Sof(H28')=Sof(C29')=Sof(H29')=Sof(C30')=Sof(H30')=Sof(C31')=Sof(H31')=1-FVAR(1)
 Sof(Co2)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=FVAR(1)
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C22'(H22'), C23'(H23'),
 C24'(H24'), C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29'),
 C30'(H30'), C31'(H31')
8.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1'(H1'A,H1'B,H1'C), 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)
;
_atom_sites_solution_hydrogens   geom
_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 0.64027(6) 0.34319(3) 0.70879(9) 0.0532(3) Uani 1 1 d . . . . .
V2 V 0.54070(6) 0.35451(3) 0.89320(8) 0.0511(3) Uani 1 1 d . . . . .
V3 V 0.60512(7) 0.41710(3) 0.77430(9) 0.0577(3) Uani 1 1 d . . . . .
V4 V 0.51689(7) 0.38980(3) 0.58696(8) 0.0589(3) Uani 1 1 d . . . . .
V5 V 0.45053(6) 0.32878(3) 0.70480(9) 0.0530(3) Uani 1 1 d . . . . .
V6 V 0.41682(6) 0.40189(3) 0.78045(8) 0.0512(3) Uani 1 1 d . . . . .
O1 O 0.7182(3) 0.32340(12) 0.6778(4) 0.0729(14) Uani 1 1 d . . . . .
O2 O 0.5474(3) 0.34219(15) 1.0012(4) 0.0756(15) Uani 1 1 d . . . . .
O3 O 0.6598(4) 0.44786(13) 0.7952(5) 0.0861(17) Uani 1 1 d . . . . .
O4 O 0.5115(4) 0.40120(17) 0.4786(4) 0.0873(18) Uani 1 1 d . . . . .
O5 O 0.3967(3) 0.29774(13) 0.6813(5) 0.0763(14) Uani 1 1 d . . . . .
O6 O 0.3404(3) 0.42309(13) 0.8083(4) 0.0723(14) Uani 1 1 d . . . . .
O7 O 0.6305(2) 0.33399(11) 0.8304(4) 0.0583(11) Uani 1 1 d . . . . .
O8 O 0.6892(2) 0.38536(11) 0.7348(4) 0.0635(12) Uani 1 1 d D . . . .
O9 O 0.6142(3) 0.36239(12) 0.5801(3) 0.0615(11) Uani 1 1 d . . . . .
O10 O 0.5587(2) 0.31095(10) 0.6749(4) 0.0572(10) Uani 1 1 d . . . . .
O11 O 0.6045(3) 0.39533(12) 0.9008(4) 0.0624(11) Uani 1 1 d . . . . .
O12 O 0.5830(3) 0.42571(11) 0.6379(4) 0.0661(12) Uani 1 1 d . . . . .
O13 O 0.4515(3) 0.34968(14) 0.5798(4) 0.0676(13) Uani 1 1 d . . . . .
O14 O 0.4732(2) 0.31898(9) 0.8410(3) 0.0530(10) Uani 1 1 d . . . . .
O15 O 0.4445(2) 0.38236(11) 0.9051(3) 0.0530(10) Uani 1 1 d . . . . .
O16 O 0.5001(3) 0.43578(10) 0.8062(4) 0.0590(11) Uani 1 1 d . . . . .
O17 O 0.4238(3) 0.41313(12) 0.6438(4) 0.0645(12) Uani 1 1 d . . . . .
O18 O 0.3653(2) 0.35913(12) 0.7488(3) 0.0566(10) Uani 1 1 d . . . . .
O19 O 0.5262(2) 0.37365(9) 0.7391(3) 0.0445(8) Uani 1 1 d . . . . .
C1 C 0.7717(7) 0.3908(7) 0.733(4) 0.117(9) Uani 0.68(6) 1 d D U P A 1
H1A H 0.790219 0.394799 0.797185 0.175 Uiso 0.68(6) 1 calc R U P A 1
H1B H 0.783255 0.409472 0.694280 0.175 Uiso 0.68(6) 1 calc R U P A 1
H1C H 0.798275 0.371931 0.708017 0.175 Uiso 0.68(6) 1 calc R U P A 1
C1' C 0.757(2) 0.3973(11) 0.688(5) 0.099(10) Uani 0.32(6) 1 d D U P A 2
H1'A H 0.788294 0.379262 0.664687 0.149 Uiso 0.32(6) 1 calc R U P A 2
H1'B H 0.788927 0.409727 0.732502 0.149 Uiso 0.32(6) 1 calc R U P A 2
H1'C H 0.741410 0.410993 0.636217 0.149 Uiso 0.32(6) 1 calc R U P A 2
C2 C 0.6735(5) 0.3695(3) 0.5152(7) 0.109(4) Uani 1 1 d . . . . .
H2A H 0.723065 0.360131 0.536209 0.163 Uiso 1 1 calc R U . . .
H2B H 0.679236 0.392797 0.509895 0.163 Uiso 1 1 calc R U . . .
H2C H 0.659398 0.360582 0.454143 0.163 Uiso 1 1 calc R U . . .
C3 C 0.5687(5) 0.29228(19) 0.5929(6) 0.074(2) Uani 1 1 d . . . . .
H3A H 0.567686 0.306292 0.538041 0.110 Uiso 1 1 calc R U . . .
H3B H 0.526254 0.276559 0.588414 0.110 Uiso 1 1 calc R U . . .
H3C H 0.619203 0.281103 0.595739 0.110 Uiso 1 1 calc R U . . .
C4 C 0.6750(6) 0.3935(3) 0.9533(8) 0.102(3) Uani 1 1 d . . . . .
H4A H 0.662361 0.391467 1.019765 0.153 Uiso 1 1 calc R U . . .
H4B H 0.705970 0.412933 0.943130 0.153 Uiso 1 1 calc R U . . .
H4C H 0.705219 0.374760 0.933110 0.153 Uiso 1 1 calc R U . . .
C5 C 0.5638(7) 0.4573(2) 0.6074(8) 0.096(3) Uani 1 1 d . . . . .
H5A H 0.509279 0.462156 0.624013 0.145 Uiso 1 1 calc R U . . .
H5B H 0.570130 0.458747 0.539542 0.145 Uiso 1 1 calc R U . . .
H5C H 0.598665 0.472786 0.637816 0.145 Uiso 1 1 calc R U . . .
C6 C 0.4047(9) 0.3417(3) 0.5017(9) 0.135(5) Uani 1 1 d . . . . .
H6A H 0.427155 0.323054 0.469900 0.202 Uiso 1 1 calc R U . . .
H6B H 0.402961 0.359880 0.458486 0.202 Uiso 1 1 calc R U . . .
H6C H 0.351398 0.336616 0.522639 0.202 Uiso 1 1 calc R U . . .
C7 C 0.4974(4) 0.28652(16) 0.8597(7) 0.068(2) Uani 1 1 d . . . . .
H7A H 0.549947 0.283011 0.834005 0.103 Uiso 1 1 calc R U . . .
H7B H 0.460424 0.271618 0.830400 0.103 Uiso 1 1 calc R U . . .
H7C H 0.498251 0.282871 0.927258 0.103 Uiso 1 1 calc R U . . .
C8 C 0.3824(4) 0.37457(18) 0.9676(5) 0.0651(17) Uani 1 1 d . . . . .
H8A H 0.348378 0.393287 0.975821 0.098 Uiso 1 1 calc R U . . .
H8B H 0.404294 0.368296 1.028193 0.098 Uiso 1 1 calc R U . . .
H8C H 0.351718 0.356787 0.941938 0.098 Uiso 1 1 calc R U . . .
C9 C 0.4935(5) 0.45242(19) 0.8956(6) 0.074(2) Uani 1 1 d . . . . .
H9A H 0.440614 0.461368 0.901867 0.111 Uiso 1 1 calc R U . . .
H9B H 0.532100 0.469762 0.898210 0.111 Uiso 1 1 calc R U . . .
H9C H 0.503212 0.437286 0.946573 0.111 Uiso 1 1 calc R U . . .
C10 C 0.3643(5) 0.4268(2) 0.5872(6) 0.085(3) Uani 1 1 d . . . . .
H10A H 0.332501 0.409652 0.559640 0.127 Uiso 1 1 calc R U . . .
H10B H 0.388349 0.439484 0.537331 0.127 Uiso 1 1 calc R U . . .
H10C H 0.330833 0.440596 0.625557 0.127 Uiso 1 1 calc R U . . .
C11 C 0.2894(4) 0.3577(2) 0.7104(8) 0.091(3) Uani 1 1 d . . . . .
H11A H 0.251138 0.364808 0.757012 0.137 Uiso 1 1 calc R U . . .
H11B H 0.277663 0.335623 0.691821 0.137 Uiso 1 1 calc R U . . .
H11C H 0.286569 0.371689 0.655501 0.137 Uiso 1 1 calc R U . . .
Co1 Co 0.27255(9) 0.27363(3) 1.00198(12) 0.0876(5) Uani 1 1 d . . . . .
C12 C 0.3016(7) 0.3008(2) 1.1146(8) 0.102(3) Uani 1 1 d . . . . .
H12 H 0.287733 0.322467 1.125660 0.123 Uiso 1 1 calc R U . . .
C13 C 0.2589(6) 0.2733(3) 1.1430(9) 0.104(3) Uani 1 1 d . . . . .
H13 H 0.210522 0.273368 1.175752 0.125 Uiso 1 1 calc R U . . .
C14 C 0.3019(6) 0.2451(2) 1.1134(9) 0.105(4) Uani 1 1 d . . . . .
H14 H 0.287619 0.223494 1.124511 0.126 Uiso 1 1 calc R U . . .
C15 C 0.3690(6) 0.2559(2) 1.0649(9) 0.099(3) Uani 1 1 d . . . . .
H15 H 0.407246 0.242558 1.036254 0.118 Uiso 1 1 calc R U . . .
C16 C 0.3698(7) 0.2895(2) 1.0660(10) 0.110(4) Uani 1 1 d . . . . .
H16 H 0.409096 0.302673 1.038903 0.132 Uiso 1 1 calc R U . . .
C17 C 0.2077(7) 0.3023(3) 0.9177(9) 0.112(4) Uani 1 1 d . . . . .
H17 H 0.193021 0.323874 0.929074 0.134 Uiso 1 1 calc R U . . .
C18 C 0.1639(7) 0.2748(4) 0.9432(10) 0.125(4) Uani 1 1 d . . . . .
H18 H 0.114889 0.274554 0.974590 0.149 Uiso 1 1 calc R U . . .
C19 C 0.2070(9) 0.2479(3) 0.9130(12) 0.129(5) Uani 1 1 d . . . . .
H19 H 0.191129 0.226209 0.920563 0.155 Uiso 1 1 calc R U . . .
C20 C 0.2761(7) 0.2577(3) 0.8705(9) 0.108(4) Uani 1 1 d . . . . .
H20 H 0.315405 0.244176 0.845141 0.129 Uiso 1 1 calc R U . . .
C21 C 0.2776(7) 0.2919(3) 0.8719(8) 0.102(3) Uani 1 1 d . . . . .
H21 H 0.317541 0.305302 0.847111 0.122 Uiso 1 1 calc R U . . .
Co2 Co 0.55833(15) 0.45615(6) 0.24719(14) 0.0883(7) Uani 0.742(5) 1 d D U P B 1
C22 C 0.4535(6) 0.4494(5) 0.2899(11) 0.155(6) Uani 0.742(5) 1 d D . P B 1
H22 H 0.433543 0.453382 0.350690 0.186 Uiso 0.742(5) 1 calc R U P B 1
C23 C 0.4848(9) 0.4216(4) 0.2595(13) 0.153(5) Uani 0.742(5) 1 d D U P B 1
H23 H 0.490805 0.402543 0.295158 0.184 Uiso 0.742(5) 1 calc R U P B 1
C24 C 0.5062(9) 0.4257(4) 0.1689(12) 0.157(5) Uani 0.742(5) 1 d D U P B 1
H24 H 0.528705 0.409678 0.130198 0.188 Uiso 0.742(5) 1 calc R U P B 1
C25 C 0.4903(8) 0.4562(4) 0.1421(9) 0.140(5) Uani 0.742(5) 1 d D . P B 1
H25 H 0.501025 0.465492 0.083036 0.168 Uiso 0.742(5) 1 calc R U P B 1
C26 C 0.4555(6) 0.4709(4) 0.2180(13) 0.159(7) Uani 0.742(5) 1 d D . P B 1
H26 H 0.436372 0.492293 0.219764 0.191 Uiso 0.742(5) 1 calc R U P B 1
C27 C 0.6076(9) 0.4777(4) 0.3472(9) 0.137(4) Uani 0.742(5) 1 d D U P B 1
H27 H 0.584220 0.484946 0.403543 0.164 Uiso 0.742(5) 1 calc R U P B 1
C28 C 0.6403(7) 0.4477(4) 0.3328(9) 0.125(4) Uani 0.742(5) 1 d D U P B 1
H28 H 0.643577 0.430911 0.377244 0.150 Uiso 0.742(5) 1 calc R U P B 1
C29 C 0.6672(5) 0.4468(4) 0.2424(11) 0.137(4) Uani 0.742(5) 1 d D U P B 1
H29 H 0.692387 0.429212 0.212947 0.165 Uiso 0.742(5) 1 calc R U P B 1
C30 C 0.6513(7) 0.4756(4) 0.2028(11) 0.143(4) Uani 0.742(5) 1 d D U P B 1
H30 H 0.663577 0.481409 0.140430 0.172 Uiso 0.742(5) 1 calc R U P B 1
C31 C 0.6144(10) 0.4951(3) 0.2674(11) 0.140(5) Uani 0.742(5) 1 d D . P B 1
H31 H 0.597207 0.516456 0.257737 0.168 Uiso 0.742(5) 1 calc R U P B 1
Co2' Co 0.5650(4) 0.4331(2) 0.2374(4) 0.084(2) Uani 0.258(5) 1 d D U P B 2
C22' C 0.541(2) 0.3928(5) 0.292(2) 0.148(9) Uani 0.258(5) 1 d D . P B 2
H22' H 0.557616 0.384801 0.350287 0.177 Uiso 0.258(5) 1 calc R U P B 2
C23' C 0.4740(16) 0.4100(8) 0.275(3) 0.145(6) Uani 0.258(5) 1 d D U P B 2
H23' H 0.436377 0.416135 0.321020 0.174 Uiso 0.258(5) 1 calc R U P B 2
C24' C 0.4709(15) 0.4168(8) 0.183(3) 0.149(6) Uani 0.258(5) 1 d D U P B 2
H24' H 0.430551 0.428557 0.152712 0.179 Uiso 0.258(5) 1 calc R U P B 2
C25' C 0.535(3) 0.4041(8) 0.1407(17) 0.161(7) Uani 0.258(5) 1 d D U P B 2
H25' H 0.547402 0.405443 0.076143 0.193 Uiso 0.258(5) 1 calc R U P B 2
C26' C 0.579(2) 0.3892(4) 0.208(3) 0.159(9) Uani 0.258(5) 1 d D . P B 2
H26' H 0.626568 0.378170 0.197768 0.190 Uiso 0.258(5) 1 calc R U P B 2
C27' C 0.586(2) 0.4663(5) 0.3246(16) 0.131(5) Uani 0.258(5) 1 d D U P B 2
H27' H 0.567315 0.467806 0.386893 0.157 Uiso 0.258(5) 1 calc R U P B 2
C28' C 0.5505(18) 0.4782(3) 0.247(2) 0.109(4) Uani 0.258(5) 1 d D U P B 2
H28' H 0.502526 0.489660 0.245362 0.131 Uiso 0.258(5) 1 calc R U P B 2
C29' C 0.596(2) 0.4707(5) 0.1716(19) 0.138(5) Uani 0.258(5) 1 d D U P B 2
H29' H 0.585353 0.476141 0.108563 0.166 Uiso 0.258(5) 1 calc R U P B 2
C30' C 0.6596(13) 0.4541(8) 0.202(3) 0.142(5) Uani 0.258(5) 1 d D U P B 2
H30' H 0.700414 0.445801 0.163930 0.171 Uiso 0.258(5) 1 calc R U P B 2
C31' C 0.6544(15) 0.4515(7) 0.296(3) 0.137(5) Uani 0.258(5) 1 d D U P B 2
H31' H 0.691474 0.441238 0.335376 0.164 Uiso 0.258(5) 1 calc R U P B 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 1.610(5) . ?
V1 O7 1.772(5) . ?
V1 O8 1.963(5) . ?
V1 O9 2.037(5) . ?
V1 O10 1.975(4) . ?
V1 O19 2.340(4) . ?
V2 O2 1.617(5) . ?
V2 O7 1.952(4) . ?
V2 O11 2.004(5) . ?
V2 O14 2.001(5) . ?
V2 O15 1.998(4) . ?
V2 O19 2.337(4) . ?
V3 O3 1.599(5) . ?
V3 O8 2.012(5) . ?
V3 O11 2.006(5) . ?
V3 O12 2.001(5) . ?
V3 O16 1.986(5) . ?
V3 O19 2.291(4) . ?
V4 O4 1.610(6) . ?
V4 O9 1.998(5) . ?
V4 O12 1.992(6) . ?
V4 O13 1.994(6) . ?
V4 O17 2.011(5) . ?
V4 O19 2.262(4) . ?
V5 O5 1.607(5) . ?
V5 O10 2.015(4) . ?
V5 O13 1.971(5) . ?
V5 O14 2.010(5) . ?
V5 O18 2.008(4) . ?
V5 O19 2.304(4) . ?
V6 O6 1.609(4) . ?
V6 O15 1.998(4) . ?
V6 O16 2.018(5) . ?
V6 O17 1.996(5) . ?
V6 O18 2.020(5) . ?
V6 O19 2.262(4) . ?
O8 C1 1.411(12) . ?
O8 C1' 1.413(13) . ?
O9 C2 1.391(9) . ?
O10 C3 1.405(9) . ?
O11 C4 1.406(10) . ?
O12 C5 1.414(9) . ?
O13 C6 1.400(11) . ?
O14 C7 1.427(7) . ?
O15 C8 1.411(8) . ?
O16 C9 1.446(9) . ?
O17 C10 1.404(8) . ?
O18 C11 1.394(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C1' H1'A 0.9700 . ?
C1' H1'B 0.9700 . ?
C1' H1'C 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
Co1 C12 2.012(12) . ?
Co1 C13 2.012(12) . ?
Co1 C14 2.031(11) . ?
Co1 C15 1.997(11) . ?
Co1 C16 1.987(13) . ?
Co1 C17 2.007(12) . ?
Co1 C18 2.015(14) . ?
Co1 C19 1.987(16) . ?
Co1 C20 1.976(12) . ?
Co1 C21 1.994(11) . ?
C12 H12 0.9400 . ?
C12 C13 1.403(14) . ?
C12 C16 1.420(13) . ?
C13 H13 0.9400 . ?
C13 C14 1.435(14) . ?
C14 H14 0.9400 . ?
C14 C15 1.397(12) . ?
C15 H15 0.9400 . ?
C15 C16 1.390(13) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
C17 C18 1.402(17) . ?
C17 C21 1.413(14) . ?
C18 H18 0.9400 . ?
C18 C19 1.397(18) . ?
C19 H19 0.9400 . ?
C19 C20 1.375(16) . ?
C20 H20 0.9400 . ?
C20 C21 1.414(15) . ?
C21 H21 0.9400 . ?
Co2 C22 1.891(8) . ?
Co2 C23 1.901(8) . ?
Co2 C24 1.896(8) . ?
Co2 C25 1.880(8) . ?
Co2 C26 1.887(8) . ?
Co2 C27 1.869(8) . ?
Co2 C28 1.873(7) . ?
Co2 C29 1.880(8) . ?
Co2 C30 1.872(8) . ?
Co2 C31 1.888(8) . ?
C22 H22 0.9400 . ?
C22 C23 1.338(14) . ?
C22 C26 1.353(14) . ?
C23 H23 0.9400 . ?
C23 C24 1.345(14) . ?
C24 H24 0.9400 . ?
C24 C25 1.341(14) . ?
C25 H25 0.9400 . ?
C25 C26 1.369(14) . ?
C26 H26 0.9400 . ?
C27 H27 0.9400 . ?
C27 C28 1.372(13) . ?
C27 C31 1.344(13) . ?
C28 H28 0.9400 . ?
C28 C29 1.360(13) . ?
C29 H29 0.9400 . ?
C29 C30 1.341(14) . ?
C30 H30 0.9400 . ?
C30 C31 1.370(14) . ?
C31 H31 0.9400 . ?
Co2' C22' 1.878(9) . ?
Co2' C23' 1.887(9) . ?
Co2' C24' 1.890(9) . ?
Co2' C25' 1.888(9) . ?
Co2' C26' 1.877(9) . ?
Co2' C27' 1.880(9) . ?
Co2' C28' 1.885(9) . ?
Co2' C29' 1.888(9) . ?
Co2' C30' 1.886(9) . ?
Co2' C31' 1.883(9) . ?
C22' H22' 0.9400 . ?
C22' C23' 1.349(15) . ?
C22' C26' 1.362(15) . ?
C23' H23' 0.9400 . ?
C23' C24' 1.342(15) . ?
C24' H24' 0.9400 . ?
C24' C25' 1.345(16) . ?
C25' H25' 0.9400 . ?
C25' C26' 1.348(15) . ?
C26' H26' 0.9400 . ?
C27' H27' 0.9400 . ?
C27' C28' 1.346(15) . ?
C27' C31' 1.368(15) . ?
C28' H28' 0.9400 . ?
C28' C29' 1.353(15) . ?
C29' H29' 0.9400 . ?
C29' C30' 1.340(15) . ?
C30' H30' 0.9400 . ?
C30' C31' 1.339(15) . ?
C31' H31' 0.9400 . ?

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 103.4(3) . . ?
O1 V1 O8 99.1(2) . . ?
O1 V1 O9 97.5(3) . . ?
O1 V1 O10 99.2(2) . . ?
O1 V1 O19 174.6(2) . . ?
O7 V1 O8 92.7(2) . . ?
O7 V1 O9 159.05(18) . . ?
O7 V1 O10 91.5(2) . . ?
O7 V1 O19 81.99(16) . . ?
O8 V1 O9 85.0(2) . . ?
O8 V1 O10 159.64(19) . . ?
O8 V1 O19 80.46(16) . . ?
O9 V1 O19 77.09(16) . . ?
O10 V1 O9 83.9(2) . . ?
O10 V1 O19 80.43(15) . . ?
O2 V2 O7 103.9(2) . . ?
O2 V2 O11 100.2(3) . . ?
O2 V2 O14 99.1(3) . . ?
O2 V2 O15 99.1(2) . . ?
O2 V2 O19 177.5(2) . . ?
O7 V2 O11 88.4(2) . . ?
O7 V2 O14 87.44(19) . . ?
O7 V2 O15 156.93(19) . . ?
O7 V2 O19 78.56(17) . . ?
O11 V2 O19 79.70(17) . . ?
O14 V2 O11 160.7(2) . . ?
O14 V2 O19 80.98(16) . . ?
O15 V2 O11 86.98(19) . . ?
O15 V2 O14 89.46(18) . . ?
O15 V2 O19 78.38(16) . . ?
O3 V3 O8 99.4(3) . . ?
O3 V3 O11 101.2(3) . . ?
O3 V3 O12 98.4(3) . . ?
O3 V3 O16 99.5(3) . . ?
O3 V3 O19 178.0(3) . . ?
O8 V3 O19 80.71(16) . . ?
O11 V3 O8 87.7(2) . . ?
O11 V3 O19 80.80(17) . . ?
O12 V3 O8 88.8(2) . . ?
O12 V3 O11 160.4(2) . . ?
O12 V3 O19 79.63(18) . . ?
O16 V3 O8 161.17(19) . . ?
O16 V3 O11 88.1(2) . . ?
O16 V3 O12 89.1(2) . . ?
O16 V3 O19 80.50(17) . . ?
O4 V4 O9 99.5(3) . . ?
O4 V4 O12 99.2(3) . . ?
O4 V4 O13 99.4(3) . . ?
O4 V4 O17 101.4(3) . . ?
O4 V4 O19 179.2(3) . . ?
O9 V4 O17 159.0(2) . . ?
O9 V4 O19 79.74(17) . . ?
O12 V4 O9 88.8(2) . . ?
O12 V4 O13 161.4(2) . . ?
O12 V4 O17 86.3(2) . . ?
O12 V4 O19 80.52(18) . . ?
O13 V4 O9 88.9(2) . . ?
O13 V4 O17 89.2(2) . . ?
O13 V4 O19 80.90(18) . . ?
O17 V4 O19 79.29(17) . . ?
O5 V5 O10 100.2(2) . . ?
O5 V5 O13 99.7(3) . . ?
O5 V5 O14 98.4(3) . . ?
O5 V5 O18 99.1(2) . . ?
O5 V5 O19 179.3(2) . . ?
O10 V5 O19 80.54(15) . . ?
O13 V5 O10 87.9(2) . . ?
O13 V5 O14 161.9(2) . . ?
O13 V5 O18 90.7(2) . . ?
O13 V5 O19 80.32(19) . . ?
O14 V5 O10 87.46(19) . . ?
O14 V5 O19 81.62(16) . . ?
O18 V5 O10 160.63(19) . . ?
O18 V5 O14 87.93(18) . . ?
O18 V5 O19 80.17(16) . . ?
O6 V6 O15 101.0(2) . . ?
O6 V6 O16 97.8(3) . . ?
O6 V6 O17 99.2(2) . . ?
O6 V6 O18 100.7(2) . . ?
O6 V6 O19 178.0(2) . . ?
O15 V6 O16 87.6(2) . . ?
O15 V6 O18 86.77(19) . . ?
O15 V6 O19 80.20(16) . . ?
O16 V6 O18 161.32(18) . . ?
O16 V6 O19 80.56(16) . . ?
O17 V6 O15 159.80(18) . . ?
O17 V6 O16 88.4(2) . . ?
O17 V6 O18 90.8(2) . . ?
O17 V6 O19 79.62(16) . . ?
O18 V6 O19 80.94(15) . . ?
V1 O7 V2 115.0(2) . . ?
V1 O8 V3 109.5(2) . . ?
C1 O8 V1 123.7(11) . . ?
C1 O8 V3 126.6(11) . . ?
C1' O8 V1 124(2) . . ?
C1' O8 V3 118(2) . . ?
V4 O9 V1 110.8(2) . . ?
C2 O9 V1 121.3(5) . . ?
C2 O9 V4 120.2(5) . . ?
V1 O10 V5 109.5(2) . . ?
C3 O10 V1 119.2(4) . . ?
C3 O10 V5 118.9(4) . . ?
V2 O11 V3 109.4(2) . . ?
C4 O11 V2 115.9(5) . . ?
C4 O11 V3 119.5(6) . . ?
V4 O12 V3 108.8(2) . . ?
C5 O12 V3 120.2(6) . . ?
C5 O12 V4 116.7(6) . . ?
V5 O13 V4 108.9(2) . . ?
C6 O13 V4 123.3(6) . . ?
C6 O13 V5 127.0(6) . . ?
V2 O14 V5 108.40(18) . . ?
C7 O14 V2 117.3(4) . . ?
C7 O14 V5 115.0(5) . . ?
V6 O15 V2 110.4(2) . . ?
C8 O15 V2 121.7(4) . . ?
C8 O15 V6 118.3(4) . . ?
V3 O16 V6 108.1(2) . . ?
C9 O16 V3 117.0(5) . . ?
C9 O16 V6 115.8(5) . . ?
V6 O17 V4 108.9(2) . . ?
C10 O17 V4 121.5(5) . . ?
C10 O17 V6 127.2(5) . . ?
V5 O18 V6 107.87(18) . . ?
C11 O18 V5 120.8(5) . . ?
C11 O18 V6 121.3(5) . . ?
V2 O19 V1 84.44(13) . . ?
V3 O19 V1 89.03(13) . . ?
V3 O19 V2 90.04(14) . . ?
V3 O19 V5 178.00(19) . . ?
V4 O19 V1 92.36(15) . . ?
V4 O19 V2 176.6(2) . . ?
V4 O19 V3 90.98(14) . . ?
V4 O19 V5 89.88(15) . . ?
V5 O19 V1 89.13(14) . . ?
V5 O19 V2 89.00(13) . . ?
V6 O19 V1 175.4(2) . . ?
V6 O19 V2 91.01(14) . . ?
V6 O19 V3 90.80(14) . . ?
V6 O19 V4 92.19(14) . . ?
V6 O19 V5 90.98(13) . . ?
O8 C1 H1A 109.5 . . ?
O8 C1 H1B 109.5 . . ?
O8 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O8 C1' H1'A 109.5 . . ?
O8 C1' H1'B 109.5 . . ?
O8 C1' H1'C 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?
O9 C2 H2A 109.5 . . ?
O9 C2 H2B 109.5 . . ?
O9 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O10 C3 H3A 109.5 . . ?
O10 C3 H3B 109.5 . . ?
O10 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O11 C4 H4A 109.5 . . ?
O11 C4 H4B 109.5 . . ?
O11 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O12 C5 H5A 109.5 . . ?
O12 C5 H5B 109.5 . . ?
O12 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O13 C6 H6A 109.5 . . ?
O13 C6 H6B 109.5 . . ?
O13 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O14 C7 H7A 109.5 . . ?
O14 C7 H7B 109.5 . . ?
O14 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O15 C8 H8A 109.5 . . ?
O15 C8 H8B 109.5 . . ?
O15 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O16 C9 H9A 109.5 . . ?
O16 C9 H9B 109.5 . . ?
O16 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O17 C10 H10A 109.5 . . ?
O17 C10 H10B 109.5 . . ?
O17 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O18 C11 H11A 109.5 . . ?
O18 C11 H11B 109.5 . . ?
O18 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 Co1 C13 40.8(4) . . ?
C12 Co1 C14 69.3(5) . . ?
C12 Co1 C18 122.5(5) . . ?
C13 Co1 C14 41.6(4) . . ?
C13 Co1 C18 107.9(5) . . ?
C15 Co1 C12 69.6(4) . . ?
C15 Co1 C13 69.4(4) . . ?
C15 Co1 C14 40.6(4) . . ?
C15 Co1 C17 158.1(4) . . ?
C15 Co1 C18 159.4(5) . . ?
C16 Co1 C12 41.6(4) . . ?
C16 Co1 C13 69.1(5) . . ?
C16 Co1 C14 68.6(5) . . ?
C16 Co1 C15 40.9(4) . . ?
C16 Co1 C17 121.8(5) . . ?
C16 Co1 C18 158.9(5) . . ?
C16 Co1 C19 157.9(5) . . ?
C16 Co1 C21 105.1(5) . . ?
C17 Co1 C12 106.1(5) . . ?
C17 Co1 C13 122.2(4) . . ?
C17 Co1 C14 159.7(4) . . ?
C17 Co1 C18 40.8(5) . . ?
C18 Co1 C14 123.9(5) . . ?
C19 Co1 C12 159.8(5) . . ?
C19 Co1 C13 124.3(5) . . ?
C19 Co1 C14 108.6(5) . . ?
C19 Co1 C15 122.7(5) . . ?
C19 Co1 C17 68.6(6) . . ?
C19 Co1 C18 40.9(5) . . ?
C19 Co1 C21 68.9(5) . . ?
C20 Co1 C12 157.8(5) . . ?
C20 Co1 C13 159.7(5) . . ?
C20 Co1 C14 122.2(5) . . ?
C20 Co1 C15 105.9(5) . . ?
C20 Co1 C16 121.0(5) . . ?
C20 Co1 C17 69.6(5) . . ?
C20 Co1 C18 69.3(5) . . ?
C20 Co1 C19 40.6(5) . . ?
C20 Co1 C21 41.7(5) . . ?
C21 Co1 C12 120.7(5) . . ?
C21 Co1 C13 157.7(5) . . ?
C21 Co1 C14 158.1(4) . . ?
C21 Co1 C15 121.2(4) . . ?
C21 Co1 C17 41.3(4) . . ?
C21 Co1 C18 69.4(5) . . ?
Co1 C12 H12 127.1 . . ?
C13 C12 Co1 69.6(7) . . ?
C13 C12 H12 126.6 . . ?
C13 C12 C16 106.9(9) . . ?
C16 C12 Co1 68.3(7) . . ?
C16 C12 H12 126.6 . . ?
Co1 C13 H13 126.2 . . ?
C12 C13 Co1 69.6(7) . . ?
C12 C13 H13 125.9 . . ?
C12 C13 C14 108.2(8) . . ?
C14 C13 Co1 69.9(7) . . ?
C14 C13 H13 125.9 . . ?
Co1 C14 H14 128.3 . . ?
C13 C14 Co1 68.5(6) . . ?
C13 C14 H14 126.4 . . ?
C15 C14 Co1 68.4(6) . . ?
C15 C14 C13 107.3(8) . . ?
C15 C14 H14 126.4 . . ?
Co1 C15 H15 125.6 . . ?
C14 C15 Co1 71.0(6) . . ?
C14 C15 H15 125.7 . . ?
C16 C15 Co1 69.2(7) . . ?
C16 C15 C14 108.6(8) . . ?
C16 C15 H15 125.7 . . ?
Co1 C16 H16 126.0 . . ?
C12 C16 Co1 70.1(7) . . ?
C12 C16 H16 125.5 . . ?
C15 C16 Co1 69.9(7) . . ?
C15 C16 C12 109.0(9) . . ?
C15 C16 H16 125.5 . . ?
Co1 C17 H17 127.0 . . ?
C18 C17 Co1 69.9(8) . . ?
C18 C17 H17 125.9 . . ?
C18 C17 C21 108.3(9) . . ?
C21 C17 Co1 68.8(7) . . ?
C21 C17 H17 125.9 . . ?
Co1 C18 H18 127.2 . . ?
C17 C18 Co1 69.3(8) . . ?
C17 C18 H18 126.5 . . ?
C19 C18 Co1 68.5(8) . . ?
C19 C18 C17 107.0(9) . . ?
C19 C18 H18 126.5 . . ?
Co1 C19 H19 126.6 . . ?
C18 C19 Co1 70.6(9) . . ?
C18 C19 H19 125.1 . . ?
C20 C19 Co1 69.3(8) . . ?
C20 C19 C18 109.8(10) . . ?
C20 C19 H19 125.1 . . ?
Co1 C20 H20 125.5 . . ?
C19 C20 Co1 70.1(8) . . ?
C19 C20 H20 126.1 . . ?
C19 C20 C21 107.8(10) . . ?
C21 C20 Co1 69.8(6) . . ?
C21 C20 H20 126.1 . . ?
Co1 C21 H21 126.8 . . ?
C17 C21 Co1 69.8(7) . . ?
C17 C21 C20 107.1(9) . . ?
C17 C21 H21 126.4 . . ?
C20 C21 Co1 68.4(7) . . ?
C20 C21 H21 126.4 . . ?
C22 Co2 C23 41.3(4) . . ?
C22 Co2 C24 69.8(6) . . ?
C24 Co2 C23 41.5(4) . . ?
C25 Co2 C22 71.4(6) . . ?
C25 Co2 C23 71.0(6) . . ?
C25 Co2 C24 41.6(4) . . ?
C25 Co2 C26 42.6(4) . . ?
C25 Co2 C31 115.2(7) . . ?
C26 Co2 C22 42.0(4) . . ?
C26 Co2 C23 70.3(6) . . ?
C26 Co2 C24 70.1(6) . . ?
C26 Co2 C31 102.6(8) . . ?
C27 Co2 C22 104.1(7) . . ?
C27 Co2 C23 125.4(7) . . ?
C27 Co2 C24 165.3(8) . . ?
C27 Co2 C25 150.7(8) . . ?
C27 Co2 C26 114.9(8) . . ?
C27 Co2 C28 43.0(4) . . ?
C27 Co2 C29 72.0(5) . . ?
C27 Co2 C30 71.2(6) . . ?
C27 Co2 C31 41.9(4) . . ?
C28 Co2 C22 117.2(7) . . ?
C28 Co2 C23 106.5(7) . . ?
C28 Co2 C24 126.8(7) . . ?
C28 Co2 C25 164.6(7) . . ?
C28 Co2 C26 151.9(7) . . ?
C28 Co2 C29 42.5(4) . . ?
C28 Co2 C31 71.9(5) . . ?
C29 Co2 C22 153.8(8) . . ?
C29 Co2 C23 119.2(8) . . ?
C29 Co2 C24 107.3(7) . . ?
C29 Co2 C25 124.6(7) . . ?
C29 Co2 C26 163.4(8) . . ?
C29 Co2 C31 71.9(6) . . ?
C30 Co2 C22 162.8(9) . . ?
C30 Co2 C23 154.3(9) . . ?
C30 Co2 C24 118.5(8) . . ?
C30 Co2 C25 104.2(7) . . ?
C30 Co2 C26 124.0(8) . . ?
C30 Co2 C28 71.2(6) . . ?
C30 Co2 C29 41.9(4) . . ?
C30 Co2 C31 42.7(4) . . ?
C31 Co2 C22 123.1(8) . . ?
C31 Co2 C23 162.5(9) . . ?
C31 Co2 C24 152.6(8) . . ?
Co2 C22 H22 127.1 . . ?
C23 C22 Co2 69.7(4) . . ?
C23 C22 H22 125.9 . . ?
C23 C22 C26 108.3(10) . . ?
C26 C22 Co2 68.8(4) . . ?
C26 C22 H22 125.9 . . ?
Co2 C23 H23 127.4 . . ?
C22 C23 Co2 68.9(4) . . ?
C22 C23 H23 126.2 . . ?
C22 C23 C24 107.7(9) . . ?
C24 C23 Co2 69.0(4) . . ?
C24 C23 H23 126.2 . . ?
Co2 C24 H24 128.4 . . ?
C23 C24 Co2 69.5(4) . . ?
C23 C24 H24 125.2 . . ?
C25 C24 Co2 68.6(4) . . ?
C25 C24 C23 109.6(10) . . ?
C25 C24 H24 125.2 . . ?
Co2 C25 H25 126.0 . . ?
C24 C25 Co2 69.8(4) . . ?
C24 C25 H25 126.8 . . ?
C24 C25 C26 106.4(10) . . ?
C26 C25 Co2 68.9(4) . . ?
C26 C25 H25 126.8 . . ?
Co2 C26 H26 127.9 . . ?
C22 C26 Co2 69.2(4) . . ?
C22 C26 C25 108.0(10) . . ?
C22 C26 H26 126.0 . . ?
C25 C26 Co2 68.4(4) . . ?
C25 C26 H26 126.0 . . ?
Co2 C27 H27 127.5 . . ?
C28 C27 Co2 68.6(4) . . ?
C28 C27 H27 125.6 . . ?
C31 C27 Co2 69.8(4) . . ?
C31 C27 H27 125.6 . . ?
C31 C27 C28 108.8(9) . . ?
Co2 C28 H28 127.9 . . ?
C27 C28 Co2 68.3(4) . . ?
C27 C28 H28 126.3 . . ?
C29 C28 Co2 69.0(4) . . ?
C29 C28 C27 107.4(8) . . ?
C29 C28 H28 126.3 . . ?
Co2 C29 H29 128.1 . . ?
C28 C29 Co2 68.5(4) . . ?
C28 C29 H29 126.2 . . ?
C30 C29 Co2 68.7(4) . . ?
C30 C29 C28 107.6(9) . . ?
C30 C29 H29 126.2 . . ?
Co2 C30 H30 127.7 . . ?
C29 C30 Co2 69.4(4) . . ?
C29 C30 H30 125.3 . . ?
C29 C30 C31 109.5(10) . . ?
C31 C30 Co2 69.3(4) . . ?
C31 C30 H30 125.3 . . ?
Co2 C31 H31 128.6 . . ?
C27 C31 Co2 68.3(4) . . ?
C27 C31 C30 106.7(10) . . ?
C27 C31 H31 126.7 . . ?
C30 C31 Co2 68.0(4) . . ?
C30 C31 H31 126.7 . . ?
C22' Co2' C23' 42.0(5) . . ?
C22' Co2' C24' 70.6(7) . . ?
C22' Co2' C25' 71.2(8) . . ?
C22' Co2' C27' 114.8(12) . . ?
C22' Co2' C28' 144.9(16) . . ?
C22' Co2' C29' 173.1(16) . . ?
C22' Co2' C30' 134.7(16) . . ?
C22' Co2' C31' 110.8(12) . . ?
C23' Co2' C24' 41.6(5) . . ?
C23' Co2' C25' 70.7(7) . . ?
C23' Co2' C29' 141.6(16) . . ?
C25' Co2' C24' 41.7(5) . . ?
C26' Co2' C22' 42.5(5) . . ?
C26' Co2' C23' 71.1(7) . . ?
C26' Co2' C24' 70.5(8) . . ?
C26' Co2' C25' 42.0(5) . . ?
C26' Co2' C27' 146.2(15) . . ?
C26' Co2' C28' 171.0(16) . . ?
C26' Co2' C29' 130.5(15) . . ?
C26' Co2' C30' 106.4(12) . . ?
C26' Co2' C31' 113.1(12) . . ?
C27' Co2' C23' 109.5(12) . . ?
C27' Co2' C24' 133.3(15) . . ?
C27' Co2' C25' 171.8(15) . . ?
C27' Co2' C28' 41.9(5) . . ?
C27' Co2' C29' 70.8(6) . . ?
C27' Co2' C30' 71.3(7) . . ?
C27' Co2' C31' 42.7(5) . . ?
C28' Co2' C23' 111.9(13) . . ?
C28' Co2' C24' 105.7(11) . . ?
C28' Co2' C25' 130.0(15) . . ?
C28' Co2' C29' 42.0(5) . . ?
C28' Co2' C30' 70.9(7) . . ?
C29' Co2' C24' 109.0(13) . . ?
C29' Co2' C25' 103.7(12) . . ?
C30' Co2' C23' 176.7(16) . . ?
C30' Co2' C24' 140.0(16) . . ?
C30' Co2' C25' 109.0(13) . . ?
C30' Co2' C29' 41.6(5) . . ?
C31' Co2' C23' 137.0(15) . . ?
C31' Co2' C24' 176.0(15) . . ?
C31' Co2' C25' 142.2(16) . . ?
C31' Co2' C28' 70.9(7) . . ?
C31' Co2' C29' 70.2(8) . . ?
C31' Co2' C30' 41.6(5) . . ?
Co2' C22' H22' 127.3 . . ?
C23' C22' Co2' 69.4(4) . . ?
C23' C22' H22' 126.2 . . ?
C23' C22' C26' 107.6(10) . . ?
C26' C22' Co2' 68.7(5) . . ?
C26' C22' H22' 126.2 . . ?
Co2' C23' H23' 127.6 . . ?
C22' C23' Co2' 68.6(4) . . ?
C22' C23' H23' 126.0 . . ?
C24' C23' Co2' 69.3(4) . . ?
C24' C23' C22' 108.0(10) . . ?
C24' C23' H23' 126.0 . . ?
Co2' C24' H24' 127.8 . . ?
C23' C24' Co2' 69.1(4) . . ?
C23' C24' H24' 125.6 . . ?
C23' C24' C25' 108.8(11) . . ?
C25' C24' Co2' 69.1(5) . . ?
C25' C24' H24' 125.6 . . ?
Co2' C25' H25' 127.7 . . ?
C24' C25' Co2' 69.2(5) . . ?
C24' C25' H25' 126.1 . . ?
C24' C25' C26' 107.7(12) . . ?
C26' C25' Co2' 68.5(5) . . ?
C26' C25' H25' 126.1 . . ?
Co2' C26' H26' 127.3 . . ?
C22' C26' Co2' 68.8(4) . . ?
C22' C26' H26' 126.0 . . ?
C25' C26' Co2' 69.5(5) . . ?
C25' C26' C22' 107.9(12) . . ?
C25' C26' H26' 126.0 . . ?
Co2' C27' H27' 127.1 . . ?
C28' C27' Co2' 69.2(4) . . ?
C28' C27' H27' 126.4 . . ?
C28' C27' C31' 107.2(10) . . ?
C31' C27' Co2' 68.8(4) . . ?
C31' C27' H27' 126.4 . . ?
Co2' C28' H28' 127.6 . . ?
C27' C28' Co2' 68.9(4) . . ?
C27' C28' H28' 126.0 . . ?
C27' C28' C29' 107.9(10) . . ?
C29' C28' Co2' 69.1(4) . . ?
C29' C28' H28' 126.0 . . ?
Co2' C29' H29' 127.9 . . ?
C28' C29' Co2' 68.9(4) . . ?
C28' C29' H29' 125.7 . . ?
C30' C29' Co2' 69.1(5) . . ?
C30' C29' C28' 108.6(10) . . ?
C30' C29' H29' 125.7 . . ?
Co2' C30' H30' 127.3 . . ?
C29' C30' Co2' 69.3(5) . . ?
C29' C30' H30' 126.0 . . ?
C31' C30' Co2' 69.0(5) . . ?
C31' C30' C29' 108.0(12) . . ?
C31' C30' H30' 126.0 . . ?
Co2' C31' H31' 127.8 . . ?
C27' C31' Co2' 68.6(4) . . ?
C27' C31' H31' 125.8 . . ?
C30' C31' Co2' 69.3(5) . . ?
C30' C31' C27' 108.3(12) . . ?
C30' C31' H31' 125.8 . . ?

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
O1 V1 O7 V2 179.6(3) . . . . ?
O8 V1 O7 V2 79.5(3) . . . . ?
O9 V1 O7 V2 -3.6(8) . . . . ?
O10 V1 O7 V2 -80.5(3) . . . . ?
O19 V1 O7 V2 -0.4(2) . . . . ?
Co1 C12 C13 C14 59.5(9) . . . . ?
Co1 C12 C16 C15 -59.3(10) . . . . ?
Co1 C13 C14 C15 57.5(9) . . . . ?
Co1 C14 C15 C16 59.2(10) . . . . ?
Co1 C15 C16 C12 59.4(10) . . . . ?
Co1 C17 C18 C19 -58.3(11) . . . . ?
Co1 C17 C21 C20 58.5(9) . . . . ?
Co1 C18 C19 C20 -58.3(11) . . . . ?
Co1 C19 C20 C21 -59.9(10) . . . . ?
Co1 C20 C21 C17 -59.4(9) . . . . ?
C12 C13 C14 Co1 -59.3(9) . . . . ?
C12 C13 C14 C15 -1.7(16) . . . . ?
C13 C12 C16 Co1 59.1(9) . . . . ?
C13 C12 C16 C15 -0.2(16) . . . . ?
C13 C14 C15 Co1 -57.6(9) . . . . ?
C13 C14 C15 C16 1.6(16) . . . . ?
C14 C15 C16 Co1 -60.3(10) . . . . ?
C14 C15 C16 C12 -0.9(16) . . . . ?
C16 C12 C13 Co1 -58.3(9) . . . . ?
C16 C12 C13 C14 1.2(16) . . . . ?
C17 C18 C19 Co1 58.8(11) . . . . ?
C17 C18 C19 C20 0.5(19) . . . . ?
C18 C17 C21 Co1 -58.9(10) . . . . ?
C18 C17 C21 C20 -0.4(16) . . . . ?
C18 C19 C20 Co1 59.1(12) . . . . ?
C18 C19 C20 C21 -0.8(18) . . . . ?
C19 C20 C21 Co1 60.1(11) . . . . ?
C19 C20 C21 C17 0.8(16) . . . . ?
C21 C17 C18 Co1 58.3(10) . . . . ?
C21 C17 C18 C19 0.0(17) . . . . ?
Co2 C22 C23 C24 -58.3(5) . . . . ?
Co2 C22 C26 C25 57.5(7) . . . . ?
Co2 C23 C24 C25 -56.8(6) . . . . ?
Co2 C24 C25 C26 -59.5(7) . . . . ?
Co2 C25 C26 C22 -58.0(7) . . . . ?
Co2 C27 C28 C29 58.1(5) . . . . ?
Co2 C27 C31 C30 -57.3(7) . . . . ?
Co2 C28 C29 C30 57.7(6) . . . . ?
Co2 C29 C30 C31 57.7(7) . . . . ?
Co2 C30 C31 C27 57.5(7) . . . . ?
C22 Co2 C24 C23 -37.6(6) . . . . ?
C22 Co2 C24 C25 84.5(8) . . . . ?
C22 Co2 C25 C24 -80.2(8) . . . . ?
C22 Co2 C25 C26 37.5(8) . . . . ?
C22 Co2 C26 C25 -120.3(12) . . . . ?
C22 Co2 C27 C28 114.9(9) . . . . ?
C22 Co2 C27 C31 -124.2(10) . . . . ?
C22 Co2 C28 C27 -81.4(10) . . . . ?
C22 Co2 C28 C29 158.7(10) . . . . ?
C22 Co2 C29 C28 -46.9(17) . . . . ?
C22 Co2 C29 C30 -167.1(15) . . . . ?
C22 Co2 C30 C29 160(2) . . . . ?
C22 Co2 C30 C31 39(2) . . . . ?
C22 Co2 C31 C27 73.1(10) . . . . ?
C22 Co2 C31 C30 -167.3(9) . . . . ?
C22 C23 C24 Co2 58.2(5) . . . . ?
C22 C23 C24 C25 1.4(8) . . . . ?
C23 Co2 C22 C26 -120.1(10) . . . . ?
C23 Co2 C24 C25 122.1(10) . . . . ?
C23 Co2 C25 C24 -36.4(7) . . . . ?
C23 Co2 C25 C26 81.3(9) . . . . ?
C23 Co2 C26 C22 37.4(7) . . . . ?
C23 Co2 C26 C25 -83.0(8) . . . . ?
C23 Co2 C27 C28 75.4(10) . . . . ?
C23 Co2 C27 C31 -163.8(10) . . . . ?
C23 Co2 C28 C27 -124.7(10) . . . . ?
C23 Co2 C28 C29 115.5(10) . . . . ?
C23 Co2 C29 C28 -82.6(9) . . . . ?
C23 Co2 C29 C30 157.3(10) . . . . ?
C23 Co2 C30 C29 -50.9(17) . . . . ?
C23 Co2 C30 C31 -172.4(13) . . . . ?
C23 Co2 C31 C27 49(2) . . . . ?
C23 Co2 C31 C30 169.0(19) . . . . ?
C23 C22 C26 Co2 -58.8(6) . . . . ?
C23 C22 C26 C25 -1.2(11) . . . . ?
C23 C24 C25 Co2 57.4(6) . . . . ?
C23 C24 C25 C26 -2.1(11) . . . . ?
C24 Co2 C22 C23 37.8(6) . . . . ?
C24 Co2 C22 C26 -82.3(9) . . . . ?
C24 Co2 C25 C26 117.7(12) . . . . ?
C24 Co2 C26 C22 81.6(8) . . . . ?
C24 Co2 C26 C25 -38.7(7) . . . . ?
C24 Co2 C27 C28 51(3) . . . . ?
C24 Co2 C27 C31 172(2) . . . . ?
C24 Co2 C28 C27 -165.7(9) . . . . ?
C24 Co2 C28 C29 74.4(10) . . . . ?
C24 Co2 C29 C28 -126.1(9) . . . . ?
C24 Co2 C29 C30 113.7(10) . . . . ?
C24 Co2 C30 C29 -84.3(10) . . . . ?
C24 Co2 C30 C31 154.2(9) . . . . ?
C24 Co2 C31 C27 -175.7(13) . . . . ?
C24 Co2 C31 C30 -56.1(17) . . . . ?
C24 C25 C26 Co2 60.0(7) . . . . ?
C24 C25 C26 C22 2.0(12) . . . . ?
C25 Co2 C22 C23 82.0(7) . . . . ?
C25 Co2 C22 C26 -38.1(8) . . . . ?
C25 Co2 C24 C23 -122.1(10) . . . . ?
C25 Co2 C26 C22 120.3(12) . . . . ?
C25 Co2 C27 C28 -167.9(13) . . . . ?
C25 Co2 C27 C31 -47.1(16) . . . . ?
C25 Co2 C28 C27 157(2) . . . . ?
C25 Co2 C28 C29 37(3) . . . . ?
C25 Co2 C29 C28 -168.7(9) . . . . ?
C25 Co2 C29 C30 71.2(11) . . . . ?
C25 Co2 C30 C29 -126.5(10) . . . . ?
C25 Co2 C30 C31 111.9(9) . . . . ?
C25 Co2 C31 C27 156.7(9) . . . . ?
C25 Co2 C31 C30 -83.7(10) . . . . ?
C26 Co2 C22 C23 120.1(10) . . . . ?
C26 Co2 C24 C23 -82.5(7) . . . . ?
C26 Co2 C24 C25 39.6(7) . . . . ?
C26 Co2 C25 C24 -117.7(12) . . . . ?
C26 Co2 C27 C28 158.2(9) . . . . ?
C26 Co2 C27 C31 -81.0(10) . . . . ?
C26 Co2 C28 C27 -45.8(16) . . . . ?
C26 Co2 C28 C29 -165.7(15) . . . . ?
C26 Co2 C29 C28 156(2) . . . . ?
C26 Co2 C29 C30 36(3) . . . . ?
C26 Co2 C30 C29 -168.4(9) . . . . ?
C26 Co2 C30 C31 70.0(11) . . . . ?
C26 Co2 C31 C27 113.4(10) . . . . ?
C26 Co2 C31 C30 -127.0(9) . . . . ?
C26 C22 C23 Co2 58.2(6) . . . . ?
C26 C22 C23 C24 -0.1(8) . . . . ?
C27 Co2 C22 C23 -128.2(9) . . . . ?
C27 Co2 C22 C26 111.7(10) . . . . ?
C27 Co2 C24 C23 30(3) . . . . ?
C27 Co2 C24 C25 152(2) . . . . ?
C27 Co2 C25 C24 -166.0(13) . . . . ?
C27 Co2 C25 C26 -48.4(17) . . . . ?
C27 Co2 C26 C22 -83.4(10) . . . . ?
C27 Co2 C26 C25 156.2(9) . . . . ?
C27 Co2 C28 C29 -119.9(8) . . . . ?
C27 Co2 C29 C28 38.5(6) . . . . ?
C27 Co2 C29 C30 -81.6(8) . . . . ?
C27 Co2 C30 C29 83.7(8) . . . . ?
C27 Co2 C30 C31 -37.9(7) . . . . ?
C27 Co2 C31 C30 119.6(11) . . . . ?
C27 C28 C29 Co2 -57.6(5) . . . . ?
C27 C28 C29 C30 0.1(7) . . . . ?
C28 Co2 C22 C23 -84.1(9) . . . . ?
C28 Co2 C22 C26 155.8(9) . . . . ?
C28 Co2 C24 C23 71.8(10) . . . . ?
C28 Co2 C24 C25 -166.1(9) . . . . ?
C28 Co2 C25 C24 47(3) . . . . ?
C28 Co2 C25 C26 164(2) . . . . ?
C28 Co2 C26 C22 -50.8(17) . . . . ?
C28 Co2 C26 C25 -171.2(13) . . . . ?
C28 Co2 C27 C31 120.8(10) . . . . ?
C28 Co2 C29 C30 -120.1(10) . . . . ?
C28 Co2 C30 C29 38.1(7) . . . . ?
C28 Co2 C30 C31 -83.4(8) . . . . ?
C28 Co2 C31 C27 -38.0(7) . . . . ?
C28 Co2 C31 C30 81.6(8) . . . . ?
C28 C27 C31 Co2 57.7(5) . . . . ?
C28 C27 C31 C30 0.4(10) . . . . ?
C28 C29 C30 Co2 -57.6(6) . . . . ?
C28 C29 C30 C31 0.1(11) . . . . ?
C29 Co2 C22 C23 -50.4(16) . . . . ?
C29 Co2 C22 C26 -170.5(14) . . . . ?
C29 Co2 C24 C23 114.8(9) . . . . ?
C29 Co2 C24 C25 -123.1(10) . . . . ?
C29 Co2 C25 C24 76.4(11) . . . . ?
C29 Co2 C25 C26 -165.9(10) . . . . ?
C29 Co2 C26 C22 165(2) . . . . ?
C29 Co2 C26 C25 45(3) . . . . ?
C29 Co2 C27 C28 -38.0(6) . . . . ?
C29 Co2 C27 C31 82.8(8) . . . . ?
C29 Co2 C28 C27 119.9(8) . . . . ?
C29 Co2 C30 C31 -121.6(11) . . . . ?
C29 Co2 C31 C27 -82.9(8) . . . . ?
C29 Co2 C31 C30 36.7(7) . . . . ?
C29 C30 C31 Co2 -57.8(7) . . . . ?
C29 C30 C31 C27 -0.3(12) . . . . ?
C30 Co2 C22 C23 160(2) . . . . ?
C30 Co2 C22 C26 40(2) . . . . ?
C30 Co2 C24 C23 158.9(9) . . . . ?
C30 Co2 C24 C25 -79.0(11) . . . . ?
C30 Co2 C25 C24 117.1(11) . . . . ?
C30 Co2 C25 C26 -125.2(11) . . . . ?
C30 Co2 C26 C22 -166.8(10) . . . . ?
C30 Co2 C26 C25 72.9(12) . . . . ?
C30 Co2 C27 C28 -82.3(7) . . . . ?
C30 Co2 C27 C31 38.6(7) . . . . ?
C30 Co2 C28 C27 82.3(7) . . . . ?
C30 Co2 C28 C29 -37.6(6) . . . . ?
C30 Co2 C29 C28 120.1(10) . . . . ?
C30 Co2 C31 C27 -119.6(11) . . . . ?
C31 Co2 C22 C23 -169.4(9) . . . . ?
C31 Co2 C22 C26 70.5(11) . . . . ?
C31 Co2 C24 C23 -161.3(16) . . . . ?
C31 Co2 C24 C25 -39.2(19) . . . . ?
C31 Co2 C25 C24 161.2(10) . . . . ?
C31 Co2 C25 C26 -81.1(11) . . . . ?
C31 Co2 C26 C22 -126.0(10) . . . . ?
C31 Co2 C26 C25 113.7(10) . . . . ?
C31 Co2 C27 C28 -120.8(10) . . . . ?
C31 Co2 C28 C27 37.1(6) . . . . ?
C31 Co2 C28 C29 -82.7(7) . . . . ?
C31 Co2 C29 C28 82.7(7) . . . . ?
C31 Co2 C29 C30 -37.4(7) . . . . ?
C31 Co2 C30 C29 121.6(11) . . . . ?
C31 C27 C28 Co2 -58.4(6) . . . . ?
C31 C27 C28 C29 -0.3(7) . . . . ?
Co2' C22' C23' C24' 58.3(5) . . . . ?
Co2' C22' C26' C25' -58.6(8) . . . . ?
Co2' C23' C24' C25' 57.7(7) . . . . ?
Co2' C24' C25' C26' 57.9(8) . . . . ?
Co2' C25' C26' C22' 58.2(8) . . . . ?
Co2' C27' C28' C29' -58.2(5) . . . . ?
Co2' C27' C31' C30' 58.0(8) . . . . ?
Co2' C28' C29' C30' -57.8(7) . . . . ?
Co2' C29' C30' C31' -58.3(8) . . . . ?
Co2' C30' C31' C27' -57.6(8) . . . . ?
C22' Co2' C23' C24' -120.1(10) . . . . ?
C22' Co2' C24' C23' 37.8(7) . . . . ?
C22' Co2' C24' C25' -83.2(10) . . . . ?
C22' Co2' C25' C24' 81.6(9) . . . . ?
C22' Co2' C25' C26' -38.3(9) . . . . ?
C22' Co2' C26' C25' 119.9(14) . . . . ?
C22' Co2' C27' C28' -146.6(17) . . . . ?
C22' Co2' C27' C31' 94.3(18) . . . . ?
C22' Co2' C28' C27' 60(2) . . . . ?
C22' Co2' C28' C29' -179.5(19) . . . . ?
C22' Co2' C30' C29' 171.4(17) . . . . ?
C22' Co2' C30' C31' -68.7(19) . . . . ?
C22' Co2' C31' C27' -104.5(18) . . . . ?
C22' Co2' C31' C30' 134.9(19) . . . . ?
C22' C23' C24' Co2' -57.9(5) . . . . ?
C22' C23' C24' C25' -0.1(8) . . . . ?
C23' Co2' C22' C26' 119.6(11) . . . . ?
C23' Co2' C24' C25' -121.0(11) . . . . ?
C23' Co2' C25' C24' 37.1(7) . . . . ?
C23' Co2' C25' C26' -82.8(10) . . . . ?
C23' Co2' C26' C22' -38.0(7) . . . . ?
C23' Co2' C26' C25' 81.9(10) . . . . ?
C23' Co2' C27' C28' -101.4(18) . . . . ?
C23' Co2' C27' C31' 139.5(18) . . . . ?
C23' Co2' C28' C27' 95.2(18) . . . . ?
C23' Co2' C28' C29' -144.7(17) . . . . ?
C23' Co2' C29' C28' 60(2) . . . . ?
C23' Co2' C29' C30' -179.4(19) . . . . ?
C23' Co2' C31' C27' -64(2) . . . . ?
C23' Co2' C31' C30' 175.6(19) . . . . ?
C23' C22' C26' Co2' 58.6(6) . . . . ?
C23' C22' C26' C25' 0.0(12) . . . . ?
C23' C24' C25' Co2' -57.7(6) . . . . ?
C23' C24' C25' C26' 0.1(12) . . . . ?
C24' Co2' C22' C23' -37.5(7) . . . . ?
C24' Co2' C22' C26' 82.0(10) . . . . ?
C24' Co2' C23' C22' 120.1(10) . . . . ?
C24' Co2' C25' C26' -119.9(14) . . . . ?
C24' Co2' C26' C22' -82.2(9) . . . . ?
C24' Co2' C26' C25' 37.7(9) . . . . ?
C24' Co2' C27' C28' -60.5(19) . . . . ?
C24' Co2' C27' C31' -179.6(18) . . . . ?
C24' Co2' C28' C27' 138.9(18) . . . . ?
C24' Co2' C28' C29' -101.0(18) . . . . ?
C24' Co2' C29' C28' 92.7(17) . . . . ?
C24' Co2' C29' C30' -146.4(18) . . . . ?
C24' Co2' C30' C29' 54(2) . . . . ?
C24' Co2' C30' C31' 174.3(19) . . . . ?
C24' C25' C26' Co2' -58.3(8) . . . . ?
C24' C25' C26' C22' -0.1(14) . . . . ?
C25' Co2' C22' C23' -81.8(8) . . . . ?
C25' Co2' C22' C26' 37.8(8) . . . . ?
C25' Co2' C23' C22' 83.0(8) . . . . ?
C25' Co2' C23' C24' -37.1(7) . . . . ?
C25' Co2' C24' C23' 121.0(11) . . . . ?
C25' Co2' C26' C22' -119.9(14) . . . . ?
C25' Co2' C28' C27' 177.9(18) . . . . ?
C25' Co2' C28' C29' -62.0(18) . . . . ?
C25' Co2' C29' C28' 135.9(17) . . . . ?
C25' Co2' C29' C30' -103.2(18) . . . . ?
C25' Co2' C30' C29' 89.5(18) . . . . ?
C25' Co2' C30' C31' -150.7(18) . . . . ?
C25' Co2' C31' C27' 169.8(19) . . . . ?
C25' Co2' C31' C30' 49(2) . . . . ?
C26' Co2' C22' C23' -119.6(11) . . . . ?
C26' Co2' C23' C22' 38.4(7) . . . . ?
C26' Co2' C23' C24' -81.7(8) . . . . ?
C26' Co2' C24' C23' 83.1(8) . . . . ?
C26' Co2' C24' C25' -37.9(9) . . . . ?
C26' Co2' C25' C24' 119.9(14) . . . . ?
C26' Co2' C27' C28' 174(2) . . . . ?
C26' Co2' C27' C31' 55(2) . . . . ?
C26' Co2' C29' C28' 172.9(16) . . . . ?
C26' Co2' C29' C30' -66.2(18) . . . . ?
C26' Co2' C30' C29' 133.5(17) . . . . ?
C26' Co2' C30' C31' -106.6(18) . . . . ?
C26' Co2' C31' C27' -150.5(17) . . . . ?
C26' Co2' C31' C30' 89.0(19) . . . . ?
C26' C22' C23' Co2' -58.2(7) . . . . ?
C26' C22' C23' C24' 0.1(8) . . . . ?
C27' Co2' C22' C23' 92.1(18) . . . . ?
C27' Co2' C22' C26' -148.3(17) . . . . ?
C27' Co2' C23' C22' -105.7(17) . . . . ?
C27' Co2' C23' C24' 134.2(17) . . . . ?
C27' Co2' C24' C23' -68.3(17) . . . . ?
C27' Co2' C24' C25' 170.7(17) . . . . ?
C27' Co2' C26' C22' 59(2) . . . . ?
C27' Co2' C26' C25' 179(2) . . . . ?
C27' Co2' C28' C29' 120.1(10) . . . . ?
C27' Co2' C29' C28' -37.7(7) . . . . ?
C27' Co2' C29' C30' 83.1(10) . . . . ?
C27' Co2' C30' C29' -81.9(9) . . . . ?
C27' Co2' C30' C31' 38.0(9) . . . . ?
C27' Co2' C31' C30' -120.6(14) . . . . ?
C27' C28' C29' Co2' 58.0(5) . . . . ?
C27' C28' C29' C30' 0.2(8) . . . . ?
C28' Co2' C22' C23' 52(2) . . . . ?
C28' Co2' C22' C26' 172(2) . . . . ?
C28' Co2' C23' C22' -150.6(17) . . . . ?
C28' Co2' C23' C24' 89.3(17) . . . . ?
C28' Co2' C24' C23' -105.4(17) . . . . ?
C28' Co2' C24' C25' 133.5(18) . . . . ?
C28' Co2' C25' C24' -65.7(18) . . . . ?
C28' Co2' C25' C26' 174.3(18) . . . . ?
C28' Co2' C27' C31' -119.1(11) . . . . ?
C28' Co2' C29' C30' 120.9(11) . . . . ?
C28' Co2' C30' C29' -37.5(7) . . . . ?
C28' Co2' C30' C31' 82.4(10) . . . . ?
C28' Co2' C31' C27' 38.1(7) . . . . ?
C28' Co2' C31' C30' -82.5(10) . . . . ?
C28' C27' C31' Co2' -58.8(6) . . . . ?
C28' C27' C31' C30' -0.8(12) . . . . ?
C28' C29' C30' Co2' 57.7(6) . . . . ?
C28' C29' C30' C31' -0.7(12) . . . . ?
C29' Co2' C23' C22' 170.8(19) . . . . ?
C29' Co2' C23' C24' 51(2) . . . . ?
C29' Co2' C24' C23' -149.5(17) . . . . ?
C29' Co2' C24' C25' 89.5(18) . . . . ?
C29' Co2' C25' C24' -103.2(19) . . . . ?
C29' Co2' C25' C26' 136.8(19) . . . . ?
C29' Co2' C26' C22' 179.1(18) . . . . ?
C29' Co2' C26' C25' -61(2) . . . . ?
C29' Co2' C27' C28' 37.9(7) . . . . ?
C29' Co2' C27' C31' -81.2(10) . . . . ?
C29' Co2' C28' C27' -120.1(10) . . . . ?
C29' Co2' C30' C31' 119.9(14) . . . . ?
C29' Co2' C31' C27' 82.9(9) . . . . ?
C29' Co2' C31' C30' -37.7(9) . . . . ?
C29' C30' C31' Co2' 58.5(8) . . . . ?
C29' C30' C31' C27' 0.9(14) . . . . ?
C30' Co2' C22' C23' 179.8(19) . . . . ?
C30' Co2' C22' C26' -61(2) . . . . ?
C30' Co2' C24' C23' 175.7(19) . . . . ?
C30' Co2' C24' C25' 55(2) . . . . ?
C30' Co2' C25' C24' -146.3(18) . . . . ?
C30' Co2' C25' C26' 93.7(19) . . . . ?
C30' Co2' C26' C22' 139.8(18) . . . . ?
C30' Co2' C26' C25' -100.3(19) . . . . ?
C30' Co2' C27' C28' 82.0(8) . . . . ?
C30' Co2' C27' C31' -37.1(8) . . . . ?
C30' Co2' C28' C27' -83.0(8) . . . . ?
C30' Co2' C28' C29' 37.1(7) . . . . ?
C30' Co2' C29' C28' -120.9(11) . . . . ?
C30' Co2' C31' C27' 120.6(14) . . . . ?
C31' Co2' C22' C23' 138.4(18) . . . . ?
C31' Co2' C22' C26' -102.0(18) . . . . ?
C31' Co2' C23' C22' -65.5(19) . . . . ?
C31' Co2' C23' C24' 174.3(18) . . . . ?
C31' Co2' C25' C24' -178.5(19) . . . . ?
C31' Co2' C25' C26' 62(2) . . . . ?
C31' Co2' C26' C22' 96.0(18) . . . . ?
C31' Co2' C26' C25' -144.1(18) . . . . ?
C31' Co2' C27' C28' 119.1(11) . . . . ?
C31' Co2' C28' C27' -38.8(7) . . . . ?
C31' Co2' C28' C29' 81.3(8) . . . . ?
C31' Co2' C29' C28' -83.1(8) . . . . ?
C31' Co2' C29' C30' 37.7(8) . . . . ?
C31' Co2' C30' C29' -119.9(14) . . . . ?
C31' C27' C28' Co2' 58.5(6) . . . . ?
C31' C27' C28' C29' 0.3(8) . . . . ?

_olex2_submission_original_sample_id mates15
_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 4.456
_oxdiff_exptl_absorpt_empirical_full_min 0.372
####################################################################### 
# 
# 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_mates20
_database_code_depnum_ccdc_archive 'CCDC 2215271'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;

_vrf_PLAT007_mates20             
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 5 
RESPONSE: The O-H ligand is distributed over five sites in the
asymmetric unit, disordered with methoxy ligands at each (see
response to alert PLAT301).
;

_vrf_PLAT301_mates20             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 25% 
RESPONSE: Five of the six unique (the cluster sits on a
crystallographic inversion center) mu-2 bridging ligand sites are
modeled as disorders of methoxy and hydroxido with the following
disorder ratios: O4-C1:O4-H, 0.732(3):0.268(3), O5-C2:O5-H,
0.930(3):0.070(3), O6-C3:O6-H, 0.956(3):0.044(3), O7-C4:O7-H,
0.941(3):0.059(3), O8-C5:O8-H, 0.956(3):0.044(3). The sixth site
was found to be fully occupied by a bridging methoxy ligand (O9-C6).
Additionally, methoxy ligand O7-C4 is modeled as disordered over
two positions (0.751(2):0.249(2)). Because there is exactly one
O-H ligand per cluster, as confirmed by independent spectroscopic
measurements, the five unique disordered methoxy ligands were
constrained to add up to 4.5 (the sixth unique site being fully
occupied by methoxy), leaving 0.5 for the O-H ligand per half
cluster (thus 1.0 per full cluster). Reassuringly, when the
occupancies of the methoxy ligand carbon atoms were refined freely
and not constrained to add to a specific total, they refined to the
occupancies observed in the disorder ratios listed above.
;

_vrf_PLAT860_mates20             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 9 
RESPONSE: The O-C distances for disordered methoxy ligand
O7-C4/O7-C4' were restrained to be similar and the anisotropic
displacement parameters for the carbon atom of the minor component
(C4') were restrained toward an isotropic model. The hydrogen
atoms for the various disordered positions of the O-H ligand
were placed along the methoxy O-C bonds at distances of 0.85 \%A
and given riding models.
;

_audit_creation_date             2022-02-22
_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         'C11 H34 O19 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C43 H106 N2 O19 V6'
_chemical_formula_weight         1260.93
_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'
N N 0.0311 0.0180 '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                   11.98260(10)
_cell_length_b                   11.99650(10)
_cell_length_c                   13.43130(10)
_cell_angle_alpha                95.1060(10)
_cell_angle_beta                 115.5700(10)
_cell_angle_gamma                113.8640(10)
_cell_volume                     1509.23(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    33917
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6000
_cell_measurement_theta_min      3.8440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78086
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.097
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51188
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.300
_diffrn_reflns_theta_min         3.850
_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 0.997
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00 119.00   0.50    0.09    --   47.30  77.00   0.00  188
  2  ω     25.00 119.00   0.50    0.09    --   47.30  77.00  30.00  188
  3  ω     25.00 119.00   0.50    0.09    --   47.30  77.00 120.00  188
  4  ω     25.00 119.00   0.50    0.09    --   47.30  77.00 -30.00  188
  5  ω     25.00 119.00   0.50    0.09    --   47.30  77.00-120.00  188
  6  ω     25.00 119.00   0.50    0.09    --   47.30  77.00-150.00  188
  7  ω     32.00 119.00   0.50    0.09    --   47.30  57.00-150.00  174
  8  ω     32.00 119.00   0.50    0.09    --   47.30  57.00 -30.00  174
  9  ω     32.00 119.00   0.50    0.09    --   47.30  57.00  90.00  174
 10  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00  60.00   88
 11  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00  90.00   88
 12  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00 150.00   88
 13  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00   0.00   88
 14  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00 -60.00   88
 15  ω    -16.00  28.00   0.50    0.09    --  -47.30  19.00-150.00   88
 16  ω     91.00 178.00   0.50    0.37    --  113.25  77.00  60.00  174
 17  ω    101.00 178.00   0.50    0.37    --  113.25  45.00  30.00  154
 18  ω    101.00 178.00   0.50    0.37    --  113.25  45.00 -60.00  154
 19  ω     91.00 178.00   0.50    0.37    --  113.25  77.00 -30.00  174
 20  ω    101.00 178.00   0.50    0.37    --  113.25  30.00   0.00  154
 21  ω    100.00 178.00   0.50    0.37    --  113.25  15.00  90.00  156
 22  ω    101.00 178.00   0.50    0.37    --  113.25  45.00 -90.00  154
 23  ω    101.00 178.00   0.50    0.37    --  113.25  30.00-150.00  154
 24  ω    101.00 178.00   0.50    0.37    --  113.25  30.00-180.00  154
 25  ω    100.00 178.00   0.50    0.37    --  113.25  15.00 -90.00  156
 26  ω    100.00 178.00   0.50    0.37    --  113.25  15.00 150.00  156
 27  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00  60.00   74
 28  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00  30.00   74
 29  ω    -24.00  70.00   0.50    0.09    --   47.30 -77.00  30.00  188
 30  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00   0.00   74
 31  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00 -30.00   74
 32  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00-120.00   74
 33  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00-180.00   74
 34  ω     95.00 178.00   0.50    0.37    --  113.25 125.00  90.00  166
 35  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00  90.00   74
 36  ω     42.00  79.00   0.50    0.37    --  113.25 -61.00 120.00   74
 37  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00 150.00  128
 38  ω     42.00 111.00   0.50    0.37    --  113.25-125.00 120.00  138
 39  ω     42.00 111.00   0.50    0.37    --  113.25-125.00 150.00  138
 40  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00  90.00  128
 41  ω     42.00 111.00   0.50    0.37    --  113.25-125.00   0.00  138
 42  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00 -90.00  128
 43  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00-120.00  128
 44  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00-150.00  128
 45  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00-180.00  128
 46  ω     34.00  95.00   0.50    0.09    --   47.30-125.00-150.00  122
 47  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00   0.00  128
 48  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00  30.00  128
 49  ω     42.00 106.00   0.50    0.37    --  113.25 -94.00 120.00  128
 50  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00-132.24  188
 51  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00 -95.96  188
 52  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00  30.00  188
 53  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00 -30.00  188
 54  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00  60.00  188
 55  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00 120.00  188
 56  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00 163.51  188
 57  ω   -163.00 -69.00   0.50    0.37    --  -91.75 -77.00 150.00  188
 58  ω   -163.00 -71.00   0.50    0.37    --  -91.75 -71.00  88.83  184
 59  ω   -163.00 -72.00   0.50    0.37    --  -91.75 -69.00  69.88  182
 60  ω   -163.00 -70.00   0.50    0.37    --  -91.75 -74.00 -17.11  186
 61  ω   -163.00 -77.00   0.50    0.37    --  -91.75 -57.00 -74.24  172
 62  ω    -65.00 -19.00   0.50    0.37    --  -91.75  61.00-150.00   92
 63  ω   -163.00 -75.00   0.50    0.37    --  -91.75 -61.00-180.00  176
 64  ω   -163.00 -73.00   0.50    0.37    --  -91.75-125.00-150.00  180
 65  ω   -119.00 -73.00   0.50    0.09    --  -47.30-125.00-180.00   92
 66  ω   -119.00 -73.00   0.50    0.09    --  -47.30-125.00-150.00   92
 67  ω   -119.00 -73.00   0.50    0.09    --  -47.30-125.00  60.00   92
;
_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      -0.1058053000
_diffrn_orient_matrix_UB_12      -0.0020559000
_diffrn_orient_matrix_UB_13      0.0369147000
_diffrn_orient_matrix_UB_21      0.0415540000
_diffrn_orient_matrix_UB_22      0.1392875000
_diffrn_orient_matrix_UB_23      -0.0006596000
_diffrn_orient_matrix_UB_31      -0.1179641000
_diffrn_orient_matrix_UB_32      -0.0505576000
_diffrn_orient_matrix_UB_33      -0.1290093000
_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                6129
_reflns_number_total             6475
_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         1.082
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6475
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.079
_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)+(0.0410P)²+1.5174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0945
_refine_special_details          
;
The O-H ligand is distributed over five sites in the asymmetric
unit, disordered with methoxy ligands at each. Five of the six
unique (the cluster sits on a crystallographic inversion center)
mu-2 bridging ligand sites are modeled as disorders of methoxy
and hydroxido with the following disorder ratios:
O4-C1:O4-H, 0.732(3):0.268(3), O5-C2:O5-H, 0.930(3):0.070(3),
O6-C3:O6-H, 0.956(3):0.044(3), O7-C4:O7-H, 0.941(3):0.059(3),
O8-C5:O8-H, 0.956(3):0.044(3). The sixth site was found to be
fully occupied by a bridging methoxy ligand (O9-C6). Additionally,
methoxy ligand O7-C4 is modeled as disordered over two positions
(0.751(2):0.249(2)). Because there is exactly one O-H ligand per
cluster, as confirmed by independent spectroscopic measurements,
the five unique disordered methoxy ligands were constrained to
add up to 4.5 (the sixth unique site being fully occupied by
methoxy), leaving 0.5 for the O-H ligand per half cluster (thus
1.0 per full cluster). Reassuringly, when the occupancies of the
methoxy ligand carbon atoms were refined freely and not
constrained to add to a specific total, they refined to the
occupancies observed in the disorder ratios listed above.

The O-C distances for disordered methoxy ligand O7-C4/O7-C4'
were restrained to be similar and the anisotropic displacement
parameters for the carbon atom of the minor component (C4')
were restrained toward an isotropic model. The hydrogen atoms
for the various disordered positions of the O-H ligand were
placed along the methoxy O-C bonds at distances of 0.85 Å
and given riding models.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C4 \\sim O7-C4'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C4') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 1*[Sof(H4)+Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(H1C)]+1*[Sof(H5)+Sof(C2)+Sof(H2A)+
 Sof(H2B)+Sof(H2C)]+1*[Sof(H6)+Sof(C3)+Sof(H3A)+Sof(H3B)+Sof(H3C)]+1*[Sof(C4)+
 Sof(H4A)+Sof(H4B)+Sof(H4C)]+1*[Sof(C4')+Sof(H4'A)+Sof(H4'B)+Sof(H4'C)]+1*
 [Sof(H8)+Sof(C5)+Sof(H5A)+Sof(H5B)+Sof(H5C)]=4.5 with esd of 0.0001
 1*[Sof(C4)+Sof(H4A)+Sof(H4B)+Sof(H4C)]+1*[Sof(C4')+Sof(H4'A)+Sof(H4'B)+
 Sof(H4'C)]-1*[Sof(H7)]=0 with esd of 0.0001
 Sof(H4)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
 Sof(H5)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Sof(H6)=1-FVAR(3)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(3)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(4)
 Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(H4'C)=FVAR(5)
 Sof(H8)=1-FVAR(6)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(6)
5.a Riding coordinates:
 O4(H4), O5(H5), O6(H6), O7(H7), O8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C4'(H4'A,
 H4'B,H4'C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,
 H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_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 0.83658(3) 0.78898(3) 0.38156(3) 0.02470(10) Uani 1 1 d . . . . .
V2 V 1.09588(4) 1.03045(3) 0.38083(3) 0.02399(9) Uani 1 1 d . . . . .
V3 V 0.84372(3) 1.06522(3) 0.38992(3) 0.01997(9) Uani 1 1 d . . . . .
O1 O 0.72126(17) 0.64329(15) 0.29687(17) 0.0398(4) Uani 1 1 d . . . . .
O2 O 1.16500(19) 1.05339(18) 0.29991(16) 0.0384(4) Uani 1 1 d . . . . .
O3 O 0.73551(15) 1.11199(14) 0.31305(14) 0.0271(3) Uani 1 1 d . . . . .
O4 O 0.94135(16) 0.84634(14) 0.29671(13) 0.0291(3) Uani 1 1 d . . . . .
H4 H 0.961730 0.792888 0.273728 0.035 Uiso 0.268(3) 1 d R U P A 2
C1 C 0.9748(4) 0.7585(3) 0.2590(3) 0.0351(7) Uani 0.732(3) 1 d . . P A 1
H1A H 1.058428 0.763841 0.324620 0.053 Uiso 0.732(3) 1 calc R U P A 1
H1B H 0.995490 0.778806 0.197705 0.053 Uiso 0.732(3) 1 calc R U P A 1
H1C H 0.894127 0.671270 0.228134 0.053 Uiso 0.732(3) 1 calc R U P A 1
O5 O 0.72740(15) 0.87720(14) 0.30735(14) 0.0307(3) Uani 1 1 d . . . . .
H5 H 0.647954 0.838355 0.243648 0.037 Uiso 0.070(3) 1 d R U P B 2
C2 C 0.5992(3) 0.8145(2) 0.2046(2) 0.0390(7) Uani 0.930(3) 1 d . . P B 1
H2A H 0.606584 0.765583 0.147471 0.058 Uiso 0.930(3) 1 calc R U P B 1
H2B H 0.573640 0.877507 0.174929 0.058 Uiso 0.930(3) 1 calc R U P B 1
H2C H 0.525899 0.755519 0.217943 0.058 Uiso 0.930(3) 1 calc R U P B 1
O6 O 0.78078(15) 0.79315(13) 0.50236(15) 0.0290(3) Uani 1 1 d . . . . .
H6 H 0.769458 0.730669 0.529553 0.035 Uiso 0.059(3) 1 d R U P C 2
C3 C 0.7617(3) 0.6880(2) 0.5481(3) 0.0388(7) Uani 0.941(3) 1 d . . P C 1
H3A H 0.695342 0.606657 0.483727 0.058 Uiso 0.941(3) 1 calc R U P C 1
H3B H 0.723125 0.693617 0.598382 0.058 Uiso 0.941(3) 1 calc R U P C 1
H3C H 0.853450 0.691668 0.593508 0.058 Uiso 0.941(3) 1 calc R U P C 1
O7 O 0.99412(14) 0.76478(12) 0.49303(13) 0.0237(3) Uani 1 1 d D . . . .
H7 H 0.998638 0.695816 0.491987 0.028 Uiso 0.044(3) 1 d R U P D 2
C4 C 1.0027(4) 0.6521(3) 0.4903(3) 0.0351(8) Uani 0.718(2) 1 d D . P E 1
H4A H 0.914702 0.580573 0.424233 0.053 Uiso 0.718(2) 1 calc R U P E 1
H4B H 1.015939 0.633413 0.562944 0.053 Uiso 0.718(2) 1 calc R U P E 1
H4C H 1.083477 0.663098 0.481946 0.053 Uiso 0.718(2) 1 calc R U P E 1
C4' C 1.0298(9) 0.6731(8) 0.4402(8) 0.0214(17) Uani 0.238(2) 1 d D U P E 3
H4'A H 0.941462 0.595188 0.381970 0.032 Uiso 0.238(2) 1 calc R U P E 3
H4'B H 1.088443 0.649712 0.502146 0.032 Uiso 0.238(2) 1 calc R U P E 3
H4'C H 1.082025 0.716316 0.403199 0.032 Uiso 0.238(2) 1 calc R U P E 3
O8 O 0.94679(16) 1.08031(15) 0.30258(13) 0.0267(3) Uani 1 1 d . . . . .
H8 H 0.902789 1.058166 0.228638 0.032 Uiso 0.059(3) 1 d R U P F 2
C5 C 0.8738(3) 1.0436(3) 0.1799(2) 0.0364(6) Uani 0.941(3) 1 d . . P F 1
H5A H 0.942212 1.079733 0.154311 0.055 Uiso 0.941(3) 1 calc R U P F 1
H5B H 0.806364 1.075897 0.152695 0.055 Uiso 0.941(3) 1 calc R U P F 1
H5C H 0.822015 0.949521 0.147378 0.055 Uiso 0.941(3) 1 calc R U P F 1
O9 O 0.78634(14) 1.03260(13) 0.50888(13) 0.0235(3) Uani 1 1 d . . . . .
O10 O 1.000000 1.000000 0.500000 0.0187(4) Uani 1 2 d S . P . .
C6 C 0.6410(2) 0.9791(2) 0.4737(2) 0.0264(4) Uani 1 1 d . . . . .
H6A H 0.588377 0.890217 0.422277 0.040 Uiso 1 1 calc R U . . .
H6B H 0.602678 1.029825 0.431948 0.040 Uiso 1 1 calc R U . . .
H6C H 0.631215 0.980144 0.542500 0.040 Uiso 1 1 calc R U . . .
N1 N 0.51368(16) 0.75098(15) 0.79236(14) 0.0182(3) Uani 1 1 d . . . . .
C7 C 0.65144(19) 0.87600(17) 0.83622(17) 0.0199(4) Uani 1 1 d . . . . .
H7A H 0.705440 0.903946 0.922416 0.024 Uiso 1 1 calc R U . . .
H7B H 0.709288 0.858285 0.809195 0.024 Uiso 1 1 calc R U . . .
C8 C 0.6345(2) 0.98660(18) 0.79830(18) 0.0219(4) Uani 1 1 d . . . . .
H8A H 0.561984 0.994785 0.810501 0.026 Uiso 1 1 calc R U . . .
H8B H 0.601725 0.969015 0.714294 0.026 Uiso 1 1 calc R U . . .
C9 C 0.7762(2) 1.11190(18) 0.86851(18) 0.0236(4) Uani 1 1 d . . . . .
H9A H 0.803013 1.134264 0.951293 0.028 Uiso 1 1 calc R U . . .
H9B H 0.851004 1.099774 0.863978 0.028 Uiso 1 1 calc R U . . .
C10 C 0.7675(2) 1.2219(2) 0.8230(2) 0.0324(5) Uani 1 1 d . . . . .
H10A H 0.743256 1.200824 0.741664 0.049 Uiso 1 1 calc R U . . .
H10B H 0.859486 1.300907 0.870085 0.049 Uiso 1 1 calc R U . . .
H10C H 0.694015 1.234523 0.828125 0.049 Uiso 1 1 calc R U . . .
C11 C 0.4131(2) 0.71339(18) 0.66234(17) 0.0205(4) Uani 1 1 d . . . . .
H11A H 0.387358 0.781461 0.647759 0.025 Uiso 1 1 calc R U . . .
H11B H 0.324715 0.633213 0.638987 0.025 Uiso 1 1 calc R U . . .
C12 C 0.4694(2) 0.69239(19) 0.58426(17) 0.0223(4) Uani 1 1 d . . . . .
H12A H 0.490495 0.620991 0.593735 0.027 Uiso 1 1 calc R U . . .
H12B H 0.558522 0.771136 0.606436 0.027 Uiso 1 1 calc R U . . .
C13 C 0.3577(2) 0.6601(2) 0.45765(19) 0.0276(4) Uani 1 1 d . . . . .
H13A H 0.263777 0.594258 0.441808 0.033 Uiso 1 1 calc R U . . .
H13B H 0.351721 0.738218 0.445634 0.033 Uiso 1 1 calc R U . . .
C14 C 0.3912(3) 0.6102(2) 0.3717(2) 0.0330(5) Uani 1 1 d . . . . .
H14A H 0.319541 0.595247 0.292197 0.049 Uiso 1 1 calc R U . . .
H14B H 0.390234 0.529308 0.379200 0.049 Uiso 1 1 calc R U . . .
H14C H 0.485439 0.673859 0.388560 0.049 Uiso 1 1 calc R U . . .
C15 C 0.4414(2) 0.77082(18) 0.85630(17) 0.0205(4) Uani 1 1 d . . . . .
H15A H 0.430743 0.847329 0.846087 0.025 Uiso 1 1 calc R U . . .
H15B H 0.504894 0.790007 0.940510 0.025 Uiso 1 1 calc R U . . .
C16 C 0.2961(2) 0.65816(19) 0.81782(18) 0.0228(4) Uani 1 1 d . . . . .
H16A H 0.302200 0.578427 0.819428 0.027 Uiso 1 1 calc R U . . .
H16B H 0.226882 0.645631 0.737072 0.027 Uiso 1 1 calc R U . . .
C17 C 0.2462(2) 0.6855(2) 0.8995(2) 0.0273(4) Uani 1 1 d . . . . .
H17A H 0.302609 0.677626 0.975469 0.033 Uiso 1 1 calc R U . . .
H17B H 0.263768 0.775008 0.913059 0.033 Uiso 1 1 calc R U . . .
C18 C 0.0890(3) 0.5940(2) 0.8508(2) 0.0363(5) Uani 1 1 d . . . . .
H18A H 0.032319 0.605678 0.778229 0.054 Uiso 1 1 calc R U . . .
H18B H 0.062848 0.612329 0.907566 0.054 Uiso 1 1 calc R U . . .
H18C H 0.070575 0.505072 0.835171 0.054 Uiso 1 1 calc R U . . .
C19 C 0.5488(2) 0.64404(18) 0.81518(18) 0.0219(4) Uani 1 1 d . . . . .
H19A H 0.459072 0.560731 0.771688 0.026 Uiso 1 1 calc R U . . .
H19B H 0.609287 0.644583 0.783010 0.026 Uiso 1 1 calc R U . . .
C20 C 0.6237(2) 0.6509(2) 0.9417(2) 0.0274(4) Uani 1 1 d . . . . .
H20A H 0.555850 0.626986 0.969754 0.033 Uiso 1 1 calc R U . . .
H20B H 0.701820 0.739854 0.990050 0.033 Uiso 1 1 calc R U . . .
C21 C 0.6840(3) 0.5586(2) 0.9533(2) 0.0380(6) Uani 1 1 d . . . . .
H21A H 0.708596 0.545414 1.030105 0.046 Uiso 1 1 calc R U . . .
H21B H 0.609277 0.474272 0.892614 0.046 Uiso 1 1 calc R U . . .
C22 C 0.8154(3) 0.6060(3) 0.9419(3) 0.0492(7) Uani 1 1 d . . . . .
H22A H 0.791613 0.617464 0.865375 0.074 Uiso 1 1 calc R U . . .
H22B H 0.847951 0.542559 0.949826 0.074 Uiso 1 1 calc R U . . .
H22C H 0.891069 0.688249 1.003080 0.074 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
V1 O1 1.6103(16) . ?
V1 O4 2.0060(17) . ?
V1 O5 2.0018(14) . ?
V1 O6 2.0078(17) . ?
V1 O7 1.9926(14) . ?
V1 O10 2.3145(3) . ?
V2 O2 1.6091(16) . ?
V2 O4 2.0061(16) . ?
V2 O6 2.0002(16) 2_776 ?
V2 O8 2.0024(14) . ?
V2 O9 2.0042(14) 2_776 ?
V2 O10 2.3167(4) . ?
V3 O3 1.6118(14) . ?
V3 O5 1.9843(15) . ?
V3 O7 1.9981(14) 2_776 ?
V3 O8 2.0104(15) . ?
V3 O9 2.0052(15) . ?
V3 O10 2.3036(3) . ?
O4 H4 0.8501 . ?
O4 C1 1.397(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O5 H5 0.8500 . ?
O5 C2 1.371(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O6 H6 0.8502 . ?
O6 C3 1.431(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
O7 H7 0.8499 . ?
O7 C4 1.395(3) . ?
O7 C4' 1.549(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4' H4'A 0.9800 . ?
C4' H4'B 0.9800 . ?
C4' H4'C 0.9800 . ?
O8 H8 0.8500 . ?
O8 C5 1.411(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O9 C6 1.414(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N1 C7 1.524(2) . ?
N1 C11 1.520(2) . ?
N1 C15 1.522(2) . ?
N1 C19 1.520(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.520(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.527(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.524(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.524(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.527(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.524(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.524(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.526(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.522(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.517(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.533(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.525(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
O1 V1 O4 99.62(9) . . ?
O1 V1 O5 99.39(7) . . ?
O1 V1 O6 99.92(9) . . ?
O1 V1 O7 100.93(7) . . ?
O1 V1 O10 178.73(7) . . ?
O4 V1 O6 160.46(6) . . ?
O4 V1 O10 79.87(4) . . ?
O5 V1 O4 88.38(7) . . ?
O5 V1 O6 88.53(7) . . ?
O5 V1 O10 79.45(4) . . ?
O6 V1 O10 80.60(4) . . ?
O7 V1 O4 88.83(6) . . ?
O7 V1 O5 159.67(6) . . ?
O7 V1 O6 87.41(6) . . ?
O7 V1 O10 80.24(4) . . ?
O2 V2 O4 101.04(9) . . ?
O2 V2 O6 98.46(9) . 2_776 ?
O2 V2 O8 99.88(7) . . ?
O2 V2 O9 99.46(7) . 2_776 ?
O2 V2 O10 179.04(8) . . ?
O4 V2 O10 79.81(5) . . ?
O6 V2 O4 160.47(7) 2_776 . ?
O6 V2 O8 87.96(6) 2_776 . ?
O6 V2 O9 90.30(6) 2_776 2_776 ?
O6 V2 O10 80.70(5) 2_776 . ?
O8 V2 O4 87.60(6) . . ?
O8 V2 O9 160.63(6) . 2_776 ?
O8 V2 O10 80.58(4) . . ?
O9 V2 O4 87.64(6) 2_776 . ?
O9 V2 O10 80.10(4) 2_776 . ?
O3 V3 O5 100.34(7) . . ?
O3 V3 O7 99.20(7) . 2_776 ?
O3 V3 O8 98.97(7) . . ?
O3 V3 O9 99.88(7) . . ?
O3 V3 O10 179.50(6) . . ?
O5 V3 O7 160.45(6) . 2_776 ?
O5 V3 O8 89.02(7) . . ?
O5 V3 O9 88.05(7) . . ?
O5 V3 O10 80.07(4) . . ?
O7 V3 O8 88.62(6) 2_776 . ?
O7 V3 O9 87.94(6) 2_776 . ?
O7 V3 O10 80.40(4) 2_776 . ?
O8 V3 O10 80.74(4) . . ?
O9 V3 O8 161.14(6) . . ?
O9 V3 O10 80.41(4) . . ?
V1 O4 V2 109.95(7) . . ?
V1 O4 H4 114.8 . . ?
V2 O4 H4 117.9 . . ?
C1 O4 V1 114.82(17) . . ?
C1 O4 V2 117.90(18) . . ?
O4 C1 H1A 109.5 . . ?
O4 C1 H1B 109.5 . . ?
O4 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
V1 O5 H5 122.4 . . ?
V3 O5 V1 110.28(7) . . ?
V3 O5 H5 126.7 . . ?
C2 O5 V1 122.41(14) . . ?
C2 O5 V3 126.70(14) . . ?
O5 C2 H2A 109.5 . . ?
O5 C2 H2B 109.5 . . ?
O5 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
V1 O6 H6 116.2 . . ?
V2 O6 V1 109.05(6) 2_776 . ?
V2 O6 H6 116.3 2_776 . ?
C3 O6 V1 116.17(15) . . ?
C3 O6 V2 116.35(16) . 2_776 ?
O6 C3 H3A 109.5 . . ?
O6 C3 H3B 109.5 . . ?
O6 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
V1 O7 V3 109.56(6) . 2_776 ?
V1 O7 H7 128.1 . . ?
V3 O7 H7 122.2 2_776 . ?
C4 O7 V1 128.20(17) . . ?
C4 O7 V3 122.07(16) . 2_776 ?
C4' O7 V1 116.7(3) . . ?
O7 C4 H4A 109.5 . . ?
O7 C4 H4B 109.5 . . ?
O7 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O7 C4' H4'A 109.5 . . ?
O7 C4' H4'B 109.5 . . ?
O7 C4' H4'C 109.5 . . ?
H4'A C4' H4'B 109.5 . . ?
H4'A C4' H4'C 109.5 . . ?
H4'B C4' H4'C 109.5 . . ?
V2 O8 V3 108.81(7) . . ?
V2 O8 H8 117.5 . . ?
V3 O8 H8 121.3 . . ?
C5 O8 V2 117.48(14) . . ?
C5 O8 V3 121.30(14) . . ?
O8 C5 H5A 109.5 . . ?
O8 C5 H5B 109.5 . . ?
O8 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
V2 O9 V3 109.34(6) 2_776 . ?
C6 O9 V2 119.25(12) . 2_776 ?
C6 O9 V3 119.01(13) . . ?
V1 O10 V1 179.999(13) . 2_776 ?
V1 O10 V2 90.375(13) . . ?
V1 O10 V2 89.624(13) 2_776 . ?
V1 O10 V2 90.375(13) 2_776 2_776 ?
V1 O10 V2 89.626(13) . 2_776 ?
V2 O10 V2 180.0 2_776 . ?
V3 O10 V1 90.189(12) 2_776 2_776 ?
V3 O10 V1 89.811(12) . 2_776 ?
V3 O10 V1 89.811(12) 2_776 . ?
V3 O10 V1 90.189(12) . . ?
V3 O10 V2 89.861(12) 2_776 2_776 ?
V3 O10 V2 90.139(12) 2_776 . ?
V3 O10 V2 89.860(12) . . ?
V3 O10 V2 90.140(12) . 2_776 ?
V3 O10 V3 179.999(12) . 2_776 ?
O9 C6 H6A 109.5 . . ?
O9 C6 H6B 109.5 . . ?
O9 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C11 N1 C7 111.67(14) . . ?
C11 N1 C15 108.65(14) . . ?
C11 N1 C19 108.25(15) . . ?
C15 N1 C7 108.05(14) . . ?
C19 N1 C7 108.81(14) . . ?
C19 N1 C15 111.44(14) . . ?
N1 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
C8 C7 N1 115.71(15) . . ?
C8 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C7 C8 C9 110.01(16) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
C8 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 C8 111.37(17) . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 108.3 . . ?
N1 C11 H11B 108.3 . . ?
N1 C11 C12 115.95(15) . . ?
H11A C11 H11B 107.4 . . ?
C12 C11 H11A 108.3 . . ?
C12 C11 H11B 108.3 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
C11 C12 C13 109.10(16) . . ?
H12A C12 H12B 108.3 . . ?
C13 C12 H12A 109.9 . . ?
C13 C12 H12B 109.9 . . ?
C12 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 C12 112.54(18) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
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 . . ?
N1 C15 H15A 108.4 . . ?
N1 C15 H15B 108.4 . . ?
N1 C15 C16 115.65(16) . . ?
H15A C15 H15B 107.4 . . ?
C16 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
C15 C16 C17 109.44(17) . . ?
H16A C16 H16B 108.2 . . ?
C17 C16 H16A 109.8 . . ?
C17 C16 H16B 109.8 . . ?
C16 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 C16 112.31(19) . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 108.3 . . ?
N1 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 N1 115.98(16) . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
C19 C20 C21 109.51(19) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C20 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 C20 113.8(2) . . ?
C22 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
N1 C7 C8 C9 167.75(16) . . . . ?
N1 C11 C12 C13 -178.02(15) . . . . ?
N1 C15 C16 C17 172.80(16) . . . . ?
N1 C19 C20 C21 -166.08(17) . . . . ?
C7 N1 C11 C12 59.6(2) . . . . ?
C7 N1 C15 C16 176.02(15) . . . . ?
C7 N1 C19 C20 70.3(2) . . . . ?
C7 C8 C9 C10 173.27(18) . . . . ?
C11 N1 C7 C8 48.4(2) . . . . ?
C11 N1 C15 C16 54.7(2) . . . . ?
C11 N1 C19 C20 -168.18(16) . . . . ?
C11 C12 C13 C14 -167.91(17) . . . . ?
C15 N1 C7 C8 -71.0(2) . . . . ?
C15 N1 C11 C12 178.69(15) . . . . ?
C15 N1 C19 C20 -48.8(2) . . . . ?
C15 C16 C17 C18 166.24(18) . . . . ?
C19 N1 C7 C8 167.83(16) . . . . ?
C19 N1 C11 C12 -60.15(19) . . . . ?
C19 N1 C15 C16 -64.5(2) . . . . ?
C19 C20 C21 C22 74.0(3) . . . . ?

_olex2_submission_original_sample_id mates20
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.821
