# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_matbp48
_database_code_depnum_ccdc_archive 'CCDC 1990062'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;

_vrf_PLAT971_matbp48             
;
PROBLEM: _A Check Calcd Resid. Dens.  0.84A   From W1 .. 4.04 eA-3 
         _B Check Calcd Resid. Dens.  1.14A   From W3 .. 2.85 eA-3 
RESPONSE: Absorption is likely not the problem since the crystal was
a tiny cube. The crystal was cracked, however, with a 85:15 component
mass ratio. No non-merohedral twin modeling was successful, likely
since the reflections of the two components could not be resolved well.
To date no other crystals have been presented for analysis.
;

_vrf_PLAT973_matbp48             
;
PROBLEM: _A Check Calcd Positive Resid. Density on W1' .. 2.47 eA-3 
RESPONSE: See above response to alert PLAT971.
;

_vrf_PLAT342_matbp48             
;
PROBLEM: _B Low Bond Precision on  C-C Bonds ............... 0.031 Ang. 
RESPONSE: See above response to alert PLAT971.
;

_vrf_PLAT972_matbp48             
;
PROBLEM: _B Check Calcd Resid. Dens.  0.74A   From W1' .. -2.80 eA-3 
RESPONSE: See above response to alert PLAT971.
;

_vrf_RINTA01_matbp48             
;
PROBLEM: _C  The value of Rint is greater than 0.12
            Rint given   0.121
RESPONSE: See above response to alert PLAT971.
;

_vrf_PLAT020_matbp48             
;
PROBLEM: _C The Value of Rint is Greater Than 0.12 ......... 0.121 
RESPONSE: See above response to alert PLAT971.
;
_vrf_PLAT084_matbp48             
;
PROBLEM: _C High wR2 Value (i.e. > 0.25) ................... 0.32 
RESPONSE: See above response to alert PLAT971.
;

_vrf_PLAT301_matbp48             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 12% 
RESPONSE: Three ethoxy ligands are modeled as disordered over two
positions each: O10-C7-C8, 0.50(3):0.50(3), O14-C15-C16, 0.60(3):0.40(3),
O17-C21-C22, 0.52(3):0.48(3).
;

_vrf_PLAT302_matbp48             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 74% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3-4 ) .. 100% 
RESPONSE: A major portion of the tungsten cluster was modeled as
disordered over two positions (0.740(1):0.260(1)). An additional methyl
group of an ethoxy ligand on this cluster was also modeled as disordered
over two positions (0.78(7):0.22(7)). 
;

_vrf_PLAT860_matbp48             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 238 
RESPONSE: For each disordered moiety analogous bond lengths and
angles between the two defined positions were restrained to be
similar. Anisotropic displacement parameters for proximal atoms
were constrained to be equivalent and/or restrained to be similar.
;

_audit_creation_date             2020-02-29
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cl5 O8 W3, C24 H60 Cl O18 V6'
_chemical_formula_sum            'C28 H70 Cl6 O26 V6 W3'
_chemical_formula_weight         1892.73
_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'
Cl Cl 0.3639 0.7018 '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'
W W -5.4734 5.5774 '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                   10.7819(4)
_cell_length_b                   15.5823(4)
_cell_length_c                   16.9994(5)
_cell_angle_alpha                81.532(2)
_cell_angle_beta                 87.046(3)
_cell_angle_gamma                83.092(3)
_cell_volume                     2802.71(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15382
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2920
_cell_measurement_theta_min      2.6730
_shelx_estimated_absorpt_T_max   0.509
_shelx_estimated_absorpt_T_min   0.348
_exptl_absorpt_coefficient_mu    22.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48081
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         79.864
_diffrn_reflns_theta_min         2.629
_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 0.992
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  22.00   0.50    1.76    --  -49.75  19.00-120.00   54
  2  ω    -34.00  22.00   0.50    1.76    --  -49.75  38.00 -60.00  112
  3  ω     -5.00  21.00   0.50    1.76    --  -49.75  19.00  30.00   52
  4  ω    -40.00 -13.00   0.50    7.02    --  -84.25  45.00 -90.00   54
  5  ω    -83.00  -8.00   0.50    1.76    --  -49.75 115.00  49.00  150
  6  ω    -42.00 -15.00   0.50    7.02    --  -84.25  45.00  60.00   54
  7  ω    -72.00 -47.00   0.50    7.02    --  -84.25 115.00  49.00   50
  8  ω   -117.00 -84.00   0.50    1.76    --  -49.75 170.00-167.00   66
  9  ω     84.00 114.00   0.50    1.76    --   49.75 170.00-167.00   60
 10  ω     85.00 110.00   0.50    7.02    --  105.75 170.00-167.00   50
 11  ω    133.00 166.00   0.50    7.02    --  105.75 125.00 -30.00   66
 12  ω    115.00 140.00   0.50    7.02    --  105.75 115.00  49.00   50
 13  ω     96.00 130.00   0.50    7.02    --  105.75 125.00 -30.00   68
 14  ω     97.00 177.00   0.50    7.02    --  105.75  45.00  60.00  160
 15  ω    116.00 170.00   0.50    7.02    --  105.75  15.00 -60.00  108
 16  ω    102.00 152.00   0.50    7.02    --  105.75  30.00-150.00  100
 17  ω    109.00 135.00   0.50    7.02    --  105.75  61.00-180.00   52
 18  ω    105.00 178.00   0.50    7.02    --  105.75  45.00 -30.00  146
 19  ω     98.00 174.00   0.50    7.02    --  105.75  15.00  60.00  152
 20  ω     91.00 119.00   0.50    7.02    --  105.75 -77.00 120.00   56
 21  ω     90.00 116.00   0.50    7.02    --  105.75 -84.00 143.90   52
 22  ω     75.00 105.00   0.50    7.02    --  105.75 -94.00 150.00   60
 23  ω     79.00 106.00   0.50    7.02    --  105.75 -96.00 100.45   54
 24  ω     65.00  90.00   0.50    1.76    --   49.75-170.00 177.00   50
 25  ω     68.00 102.00   0.50    7.02    --  105.75-170.00 177.00   68
 26  ω     51.00  77.00   0.50    7.02    --  105.75 -77.00 120.00   52
 27  ω     42.00  67.00   0.50    7.02    --  105.75 -94.00 150.00   50
 28  ω     39.00  73.00   0.50    7.02    --  105.75 -61.00 120.00   68
 29  ω     36.00  68.00   0.50    7.02    --  105.75 -94.00  90.00   64
 30  ω     38.00  63.00   0.50    7.02    --  105.75 -61.00  30.00   50
 31  ω     52.00  94.00   0.50    7.02    --  105.75 -77.00   0.00   84
 32  ω     75.00 104.00   0.50    7.02    --  105.75 -94.00 -60.00   58
 33  ω     85.00 111.00   0.50    7.02    --  105.75-125.00 -90.00   52
 34  ω     71.00 105.00   0.50    7.02    --  105.75 -94.00 -90.00   68
 35  ω     50.00  76.00   0.50    7.02    --  105.75-115.00 -39.00   52
 36  ω     35.00 106.00   0.50    7.02    --  105.75 -97.00  17.60  142
 37  ω     38.00 106.00   0.50    7.02    --  105.75 -94.00  60.00  136
 38  ω     40.00  67.00   0.50    7.02    --  105.75 -94.00 -60.00   54
 39  ω     43.00 107.00   0.50    7.02    --  105.75-106.00 -89.29  128
 40  ω     43.00  78.00   0.50    7.02    --  105.75 -61.00-180.00   70
 41  ω     34.00 105.00   0.50    7.02    --  105.75 -94.00-180.00  142
 42  ω     36.00  67.00   0.50    7.02    --  105.75-125.00 -90.00   62
 43  ω     36.00  94.00   0.50    7.02    --  105.75-125.00 -60.00  116
 44  ω     34.00  59.00   0.50    1.76    --   49.75-115.00 -39.00   50
 45  ω     35.00  61.00   0.50    7.02    --  105.75 -61.00 -30.00   52
 46  ω     34.00 106.00   0.50    7.02    --  105.75 -94.00 -30.00  144
 47  ω     38.00  64.00   0.50    7.02    --  105.75-125.00  60.00   52
 48  ω     42.00 102.00   0.50    7.02    --  105.75 -94.00 120.00  120
 49  ω     35.00  72.00   0.50    7.02    --  105.75 -96.00 100.45   74
 50  ω     98.00 152.00   0.50    7.02    --  105.75  15.00 150.00  108
 51  ω     98.00 178.00   0.50    7.02    --  105.75  30.00 150.00  160
 52  ω     34.00  74.00   0.50    7.02    --  105.75 -61.00 -90.00   80
 53  ω    -88.00 -47.00   0.50    1.76    --  -49.75-170.00 177.00   82
 54  ω   -121.00 -33.00   0.50    1.76    --  -49.75 -77.00   0.00  176
 55  ω   -114.00 -89.00   0.50    7.02    --  -84.25-115.00 -39.00   50
 56  ω   -121.00 -73.00   0.50    1.76    --  -49.75-125.00  30.00   96
 57  ω   -119.00 -74.00   0.50    1.76    --  -49.75-125.00   0.00   90
 58  ω   -114.00 -89.00   0.50    7.02    --  -84.25-170.00 177.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0288948000
_diffrn_orient_matrix_UB_12      -0.0045274000
_diffrn_orient_matrix_UB_13      0.0901209000
_diffrn_orient_matrix_UB_21      0.1108951000
_diffrn_orient_matrix_UB_22      0.0517055000
_diffrn_orient_matrix_UB_23      0.0075608000
_diffrn_orient_matrix_UB_31      -0.0872217000
_diffrn_orient_matrix_UB_32      0.0861911000
_diffrn_orient_matrix_UB_33      -0.0150276000
_diffrn_oxdiff_digest_frames     
;
01b10cc4aa192927d798816e8a01a5e2140477678d1
;
_diffrn_oxdiff_digest_hkl        
;
01c4099cce23a2957693149b2c97374e86b72f
;
_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                8069
_reflns_number_total             11712
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         3.821
_refine_diff_density_min         -3.025
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       0.00034(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         11712
_refine_ls_number_restraints     238
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.1002
_refine_ls_restrained_S_all      1.075
_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)+(0.1901P)²+12.3525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2861
_refine_ls_wR_factor_ref         0.3201
_refine_special_details          
;
Three ethoxy ligands are modeled as disordered over two
positions each: O10-C7-C8, 0.50(3):0.50(3), O14-C15-C16,
0.60(3):0.40(3), O17-C21-C22, 0.52(3):0.48(3). A major portion
of the tungsten cluster was modeled as disordered over two
positions (0.740(1):0.260(1)). An additional methyl group of
an ethoxy ligand on this cluster was also modeled as disordered
over two positions (0.78(7):0.22(7)).

For each disordered moiety analogous bond lengths and angles
between the two defined positions were restrained to be
similar. Anisotropic displacement parameters for proximal atoms
were constrained to be equivalent and/or restrained to be similar.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O14-C15 \\sim O14-C15'
 with sigma of 0.01
 C15-C16 \\sim C15'-C16'
 with sigma of 0.01
 O14-C16 \\sim O14-C16'
 with sigma of 0.02
 O10-C7 \\sim O10-C7'
 with sigma of 0.01
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 O10-C8 \\sim O10-C8'
 with sigma of 0.02
 O17-C21 \\sim O17-C21'
 with sigma of 0.01
 C21-C22 \\sim C21'-C22'
 with sigma of 0.01
 O17-C22 \\sim O17-C22'
 with sigma of 0.02
 W1-Cl2 \\sim W1'-Cl2'
 with sigma of 0.01
 W1-O20 \\sim W1'-O20'
 with sigma of 0.01
 W1-O25 \\sim W1'-O25' \\sim O25-W3 \\sim O25'-W3
 with sigma of 0.01
 W2-O21 \\sim W2'-O21'
 with sigma of 0.01
 W2-O26 \\sim W2'-O26'
 with sigma of 0.01
 W2-O24 \\sim W2-O24' \\sim O24-W3 \\sim O24'-W3
 with sigma of 0.01
 W1-O23 \\sim W2-O23 \\sim W1'-O23' \\sim W2'-O23'
 with sigma of 0.01
 W1-Cl6 \\sim W2-Cl6 \\sim W3-Cl6 \\sim W1'-Cl6' \\sim W2'-Cl6' \\sim W3-Cl6'
 with sigma of 0.02
 C27-C28' \\sim C27-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(W1) = Uanis(W1')
Uanis(W2) = Uanis(W2')
Uanis(O20) = Uanis(O20')
Uanis(O21) = Uanis(O21')
Uanis(O23) = Uanis(O23')
Uanis(O24) = Uanis(O24')
Uanis(O25) = Uanis(O25')
Uanis(Cl2) = Uanis(Cl2')
Uanis(Cl3) = Uanis(Cl3')
Uanis(Cl4) = Uanis(Cl4')
Uanis(Cl6) = Uanis(Cl6')
Uanis(O26) = Uanis(O26')
Uanis(C25) = Uanis(C25')
Uanis(C26) = Uanis(C26')
Uanis(C28') = Uanis(C28)
4. Rigid body (RIGU) restrains
 O10, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C7', C8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O14, C15', C16'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, C21', C22'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 W1, O20, O25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 W1', O20', O25'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O26, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
as
{O26', C25', C26'}
6. Others
 Sof(W1')=Sof(W2')=Sof(Cl2')=Sof(Cl3')=Sof(Cl4')=Sof(Cl6')=Sof(O20')=Sof(O21')=
 Sof(O23')=Sof(O24')=Sof(O25')=Sof(O26')=Sof(C25')=Sof(H25C)=Sof(H25D)=
 Sof(C26')=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(W1)=Sof(W2)=Sof(Cl2)=Sof(Cl3)=Sof(Cl4)=Sof(Cl6)=Sof(O20)=Sof(O21)=
 Sof(O23)=Sof(O24)=Sof(O25)=Sof(O26)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Sof(C15')=Sof(H15C)=Sof(H15D)=Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(3)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(3)
 Sof(C21')=Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(4)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(4)
 Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(5)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C25(H25A,H25B), C25'(H25C,H25D), C1(H1A,H1B),
 C3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B),
 C17(H17A,H17B), C19(H19A,H19B), C23(H23A,H23B), C7(H7A,H7B), C15(H15A,H15B),
 C21(H21A,H21B), C7'(H7'A,H7'B), C15'(H15C,H15D), C21'(H21C,H21D)
7.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C26'(H26D,H26E,H26F), C28'(H28D,
 H28E,H28F), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C),
 C8'(H8'A,H8'B,H8'C), C16'(H16D,H16E,H16F), C22'(H22D,H22E,H22F)
7.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C)
;
_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
W3 W 0.41464(7) 0.70526(4) 0.12487(5) 0.0724(3) Uani 1 1 d D U . . .
Cl5 Cl 0.4342(4) 0.8064(3) 0.0081(2) 0.0785(9) Uani 1 1 d . U . . .
O22 O 0.3921(13) 0.6164(8) 0.0839(9) 0.097(4) Uani 1 1 d . U . . .
O27 O 0.2528(11) 0.7600(7) 0.1375(6) 0.073(3) Uani 1 1 d . U . . .
C27 C 0.1867(15) 0.8414(11) 0.1457(10) 0.075(4) Uani 1 1 d D U . . .
H27A H 0.236052 0.887413 0.122468 0.090 Uiso 0.78(7) 1 calc R . P A 1
H27B H 0.171747 0.846119 0.201736 0.090 Uiso 0.78(7) 1 calc R . P A 1
H27C H 0.202417 0.882648 0.098744 0.090 Uiso 0.22(7) 1 calc R . P A 2
H27D H 0.216338 0.862786 0.191266 0.090 Uiso 0.22(7) 1 calc R . P A 2
W1 W 0.49334(13) 0.69098(10) 0.31725(8) 0.0919(4) Uani 0.7398(15) 1 d D U P B 1
W2 W 0.70544(8) 0.75405(6) 0.16489(6) 0.0655(3) Uani 0.7398(15) 1 d D U P B 1
Cl2 Cl 0.2852(7) 0.7421(8) 0.3489(5) 0.0983(18) Uani 0.7398(15) 1 d D U P B 1
Cl3 Cl 0.5481(9) 0.7914(8) 0.3990(4) 0.133(3) Uani 0.7398(15) 1 d . U P B 1
Cl4 Cl 0.7783(8) 0.8431(5) 0.2499(4) 0.104(2) Uani 0.7398(15) 1 d . U P B 1
Cl6 Cl 0.4752(5) 0.8415(3) 0.2021(3) 0.0661(12) Uani 0.7398(15) 1 d D U P B 1
O20 O 0.511(3) 0.6007(18) 0.3807(18) 0.161(8) Uani 0.7398(15) 1 d D U P B 1
O21 O 0.8400(12) 0.6910(10) 0.1432(10) 0.079(4) Uani 0.7398(15) 1 d D U P B 1
O23 O 0.6526(10) 0.6868(11) 0.2622(7) 0.093(4) Uani 0.7398(15) 1 d D U P B 1
O24 O 0.5926(7) 0.6958(9) 0.1151(8) 0.067(3) Uani 0.7398(15) 1 d D U P B 1
O25 O 0.4191(15) 0.6471(8) 0.2332(4) 0.088(3) Uani 0.7398(15) 1 d D U P B 1
O26 O 0.7052(13) 0.8499(9) 0.0837(9) 0.067(3) Uani 0.7398(15) 1 d D U P B 1
C25 C 0.665(2) 0.9412(12) 0.0784(16) 0.083(4) Uani 0.7398(15) 1 d D U P B 1
H25A H 0.641090 0.956426 0.130809 0.099 Uiso 0.7398(15) 1 calc R . P B 1
H25B H 0.593303 0.956642 0.044819 0.099 Uiso 0.7398(15) 1 calc R . P B 1
C26 C 0.768(3) 0.9876(15) 0.0446(15) 0.085(6) Uani 0.7398(15) 1 d D U P B 1
H26A H 0.743520 1.049312 0.040381 0.128 Uiso 0.7398(15) 1 calc R . P B 1
H26B H 0.838335 0.971948 0.078366 0.128 Uiso 0.7398(15) 1 calc R . P B 1
H26C H 0.790746 0.972163 -0.007269 0.128 Uiso 0.7398(15) 1 calc R . P B 1
C28 C 0.063(3) 0.8524(17) 0.105(3) 0.113(7) Uani 0.78(7) 1 d D U P A 1
H28A H 0.019364 0.908437 0.111246 0.169 Uiso 0.78(7) 1 calc R . P A 1
H28B H 0.078374 0.848495 0.049456 0.169 Uiso 0.78(7) 1 calc R . P A 1
H28C H 0.014181 0.807273 0.128586 0.169 Uiso 0.78(7) 1 calc R . P A 1
W1' W 0.4548(4) 0.7001(3) 0.3473(2) 0.0919(4) Uani 0.2602(15) 1 d D U P B 2
W2' W 0.6915(3) 0.76033(17) 0.2116(2) 0.0655(3) Uani 0.2602(15) 1 d D U P B 2
Cl2' Cl 0.2429(15) 0.755(3) 0.3594(17) 0.0983(18) Uani 0.2602(15) 1 d D U P B 2
Cl3' Cl 0.486(3) 0.799(3) 0.4285(13) 0.133(3) Uani 0.2602(15) 1 d . U P B 2
Cl4' Cl 0.740(2) 0.8605(16) 0.2944(13) 0.104(2) Uani 0.2602(15) 1 d . U P B 2
Cl6' Cl 0.4439(13) 0.8361(9) 0.2182(8) 0.0661(12) Uani 0.2602(15) 1 d D U P B 2
O20' O 0.458(8) 0.607(4) 0.407(6) 0.161(8) Uani 0.2602(15) 1 d D U P B 2
O21' O 0.836(2) 0.703(2) 0.211(3) 0.079(4) Uani 0.2602(15) 1 d D U P B 2
O23' O 0.6232(16) 0.696(3) 0.305(2) 0.093(4) Uani 0.2602(15) 1 d D U P B 2
O24' O 0.5870(14) 0.700(3) 0.147(2) 0.067(3) Uani 0.2602(15) 1 d D U P B 2
O25' O 0.438(5) 0.676(2) 0.2392(6) 0.088(3) Uani 0.2602(15) 1 d D U P B 2
O26' O 0.717(4) 0.842(2) 0.1211(19) 0.067(3) Uani 0.2602(15) 1 d D U P B 2
C25' C 0.692(6) 0.914(3) 0.060(3) 0.083(4) Uani 0.2602(15) 1 d D U P B 2
H25C H 0.604450 0.938194 0.063986 0.099 Uiso 0.2602(15) 1 calc R . P B 2
H25D H 0.708633 0.896235 0.008339 0.099 Uiso 0.2602(15) 1 calc R . P B 2
C26' C 0.772(9) 0.979(4) 0.072(5) 0.085(6) Uani 0.2602(15) 1 d D U P B 2
H26D H 0.757180 1.028996 0.032247 0.128 Uiso 0.2602(15) 1 calc R . P B 2
H26E H 0.753978 0.996310 0.123989 0.128 Uiso 0.2602(15) 1 calc R . P B 2
H26F H 0.857688 0.954541 0.068595 0.128 Uiso 0.2602(15) 1 calc R . P B 2
C28' C 0.048(3) 0.836(6) 0.157(12) 0.113(7) Uani 0.22(7) 1 d D U P A 2
H28D H 0.005452 0.892577 0.162054 0.169 Uiso 0.22(7) 1 calc R . P A 2
H28E H 0.018021 0.815656 0.111166 0.169 Uiso 0.22(7) 1 calc R . P A 2
H28F H 0.031930 0.795812 0.203608 0.169 Uiso 0.22(7) 1 calc R . P A 2
V1 V 1.0344(2) 0.18763(14) 0.20021(13) 0.0566(5) Uani 1 1 d . U . . .
V2 V 1.2600(2) 0.26975(16) 0.25967(16) 0.0645(6) Uani 1 1 d . U . . .
V3 V 1.0269(2) 0.39119(14) 0.17446(13) 0.0595(5) Uani 1 1 d . U . . .
V4 V 0.8335(2) 0.29635(15) 0.29948(16) 0.0653(6) Uani 1 1 d . U . . .
V5 V 1.0673(3) 0.17271(14) 0.38409(13) 0.0640(6) Uani 1 1 d . U . . .
V6 V 1.0610(3) 0.38220(14) 0.36390(13) 0.0620(6) Uani 1 1 d . U . . .
Cl1 Cl 1.0206(5) 0.0902(3) 0.1156(3) 0.0968(13) Uani 1 1 d . U . . .
O2 O 1.4097(12) 0.2645(9) 0.2462(9) 0.100(4) Uani 1 1 d . U . . .
O3 O 1.0144(12) 0.4708(6) 0.1010(6) 0.078(3) Uani 1 1 d . U . . .
O4 O 0.6879(12) 0.3064(9) 0.3155(9) 0.097(4) Uani 1 1 d . U . . .
O5 O 1.0809(15) 0.0936(8) 0.4603(8) 0.099(4) Uani 1 1 d . U . . .
O6 O 1.0695(13) 0.4536(6) 0.4211(6) 0.081(3) Uani 1 1 d . U . . .
O7 O 1.2178(8) 0.1881(6) 0.1914(6) 0.060(2) Uani 1 1 d . U . . .
O8 O 1.0196(10) 0.2941(6) 0.1181(5) 0.064(2) Uani 1 1 d . U . . .
O9 O 0.8541(9) 0.2120(6) 0.2248(6) 0.069(2) Uani 1 1 d . U . . .
O10 O 1.0540(10) 0.1040(6) 0.2993(6) 0.067(2) Uani 1 1 d D U . . .
O11 O 1.2079(10) 0.3660(6) 0.1715(6) 0.069(2) Uani 1 1 d . U . . .
O12 O 0.8507(9) 0.3891(6) 0.2064(6) 0.068(2) Uani 1 1 d . U . . .
O13 O 0.8859(11) 0.2013(6) 0.3854(6) 0.073(3) Uani 1 1 d . U . . .
O14 O 1.2447(11) 0.1776(7) 0.3521(7) 0.079(3) Uani 1 1 d D U . . .
O15 O 1.2379(10) 0.3562(6) 0.3342(6) 0.073(3) Uani 1 1 d . U . . .
O16 O 1.0439(10) 0.4602(6) 0.2617(5) 0.066(2) Uani 1 1 d . U . . .
O17 O 0.8800(11) 0.3790(7) 0.3681(6) 0.074(3) Uani 1 1 d D U . . .
O18 O 1.0758(12) 0.2729(6) 0.4404(6) 0.073(3) Uani 1 1 d . U . . .
O19 O 1.0476(7) 0.2831(5) 0.2796(5) 0.0513(17) Uani 1 1 d . U . . .
C1 C 1.3008(13) 0.1624(8) 0.1282(9) 0.063(3) Uani 1 1 d . U . . .
H1A H 1.366683 0.200389 0.119515 0.076 Uiso 1 1 calc R . . . .
H1B H 1.255000 0.169555 0.079641 0.076 Uiso 1 1 calc R . . . .
C2 C 1.3572(15) 0.0712(9) 0.1458(10) 0.072(4) Uani 1 1 d . U . . .
H2A H 1.424381 0.067791 0.181478 0.108 Uiso 1 1 calc GR . . . .
H2B H 1.388911 0.050764 0.097288 0.108 Uiso 1 1 calc GR . . . .
H2C H 1.295033 0.035608 0.170176 0.108 Uiso 1 1 calc GR . . . .
C3 C 1.021(2) 0.3028(11) 0.0333(8) 0.084(5) Uani 1 1 d . U . . .
H3A H 1.045665 0.245695 0.017274 0.100 Uiso 1 1 calc R . . . .
H3B H 1.084826 0.339958 0.012054 0.100 Uiso 1 1 calc R . . . .
C4 C 0.9033(18) 0.3388(12) -0.0019(12) 0.087(5) Uani 1 1 d . U . . .
H4A H 0.840260 0.301671 0.017512 0.131 Uiso 1 1 calc GR . . . .
H4B H 0.912029 0.342567 -0.058753 0.131 Uiso 1 1 calc GR . . . .
H4C H 0.879495 0.396067 0.012258 0.131 Uiso 1 1 calc GR . . . .
C5 C 0.7566(14) 0.1962(11) 0.1726(10) 0.074(4) Uani 1 1 d . U . . .
H5A H 0.795125 0.180112 0.123176 0.088 Uiso 1 1 calc R . . . .
H5B H 0.700217 0.249296 0.159904 0.088 Uiso 1 1 calc R . . . .
C6 C 0.6842(19) 0.1246(14) 0.2125(12) 0.098(6) Uani 1 1 d . U . . .
H6A H 0.640114 0.142646 0.258871 0.147 Uiso 1 1 calc GR . . . .
H6B H 0.740698 0.073016 0.227863 0.147 Uiso 1 1 calc GR . . . .
H6C H 0.625438 0.112194 0.176299 0.147 Uiso 1 1 calc GR . . . .
C9 C 1.2872(16) 0.4298(10) 0.1327(9) 0.075(4) Uani 1 1 d . U . . .
H9A H 1.238113 0.486516 0.122872 0.090 Uiso 1 1 calc R . . . .
H9B H 1.353520 0.434455 0.167763 0.090 Uiso 1 1 calc R . . . .
C10 C 1.341(3) 0.4066(14) 0.0592(12) 0.115(8) Uani 1 1 d . U . . .
H10A H 1.384558 0.348828 0.068244 0.172 Uiso 1 1 calc GR . . . .
H10B H 1.398053 0.447302 0.037595 0.172 Uiso 1 1 calc GR . . . .
H10C H 1.275681 0.408025 0.022432 0.172 Uiso 1 1 calc GR . . . .
C11 C 0.758(2) 0.4654(12) 0.1871(13) 0.096(5) Uani 1 1 d . U . . .
H11A H 0.729332 0.488571 0.235587 0.115 Uiso 1 1 calc R . . . .
H11B H 0.796983 0.510386 0.152329 0.115 Uiso 1 1 calc R . . . .
C12 C 0.6531(19) 0.4434(17) 0.1488(13) 0.109(7) Uani 1 1 d . U . . .
H12A H 0.629220 0.388690 0.175209 0.164 Uiso 1 1 calc GR . . . .
H12B H 0.675488 0.438441 0.094116 0.164 Uiso 1 1 calc GR . . . .
H12C H 0.584314 0.488211 0.151434 0.164 Uiso 1 1 calc GR . . . .
C13 C 0.803(3) 0.185(2) 0.4543(16) 0.130(9) Uani 1 1 d . U . . .
H13A H 0.851576 0.180052 0.501590 0.156 Uiso 1 1 calc R . . . .
H13B H 0.741359 0.235759 0.454923 0.156 Uiso 1 1 calc R . . . .
C14 C 0.742(3) 0.114(2) 0.4598(16) 0.148(11) Uani 1 1 d . U . . .
H14A H 0.794504 0.068611 0.438032 0.222 Uiso 1 1 calc GR . . . .
H14B H 0.666863 0.128601 0.430511 0.222 Uiso 1 1 calc GR . . . .
H14C H 0.721543 0.095037 0.514614 0.222 Uiso 1 1 calc GR . . . .
C17 C 1.333(3) 0.4122(19) 0.3462(17) 0.132(9) Uani 1 1 d . U . . .
H17A H 1.384790 0.420784 0.298118 0.158 Uiso 1 1 calc R . . . .
H17B H 1.291543 0.468809 0.355582 0.158 Uiso 1 1 calc R . . . .
C18 C 1.411(2) 0.3759(18) 0.4123(13) 0.112(7) Uani 1 1 d . U . . .
H18A H 1.464672 0.326283 0.398623 0.167 Uiso 1 1 calc GR . . . .
H18B H 1.358934 0.358014 0.458051 0.167 Uiso 1 1 calc GR . . . .
H18C H 1.460209 0.419252 0.424246 0.167 Uiso 1 1 calc GR . . . .
C19 C 1.016(2) 0.5514(10) 0.2548(12) 0.099(6) Uani 1 1 d . U . . .
H19A H 0.952856 0.564225 0.295687 0.119 Uiso 1 1 calc R . . . .
H19B H 0.977875 0.571553 0.203776 0.119 Uiso 1 1 calc R . . . .
C20 C 1.115(2) 0.6012(14) 0.2606(15) 0.109(7) Uani 1 1 d . U . . .
H20A H 1.150830 0.584755 0.311969 0.164 Uiso 1 1 calc GR . . . .
H20B H 1.084023 0.662128 0.254011 0.164 Uiso 1 1 calc GR . . . .
H20C H 1.177637 0.590549 0.219933 0.164 Uiso 1 1 calc GR . . . .
C23 C 1.1378(19) 0.2641(12) 0.5145(10) 0.085(4) Uani 1 1 d . U . . .
H23A H 1.216065 0.289449 0.504937 0.102 Uiso 1 1 calc R . . . .
H23B H 1.157586 0.202471 0.533845 0.102 Uiso 1 1 calc R . . . .
C24 C 1.065(2) 0.3053(13) 0.5753(10) 0.103(7) Uani 1 1 d . U . . .
H24A H 1.029473 0.362635 0.553020 0.155 Uiso 1 1 calc GR . . . .
H24B H 1.117877 0.309714 0.617934 0.155 Uiso 1 1 calc GR . . . .
H24C H 0.999088 0.270862 0.595476 0.155 Uiso 1 1 calc GR . . . .
C7 C 1.103(3) 0.0121(12) 0.3079(19) 0.070(7) Uani 0.50(3) 1 d D U P C 1
H7A H 1.167727 0.000612 0.347158 0.084 Uiso 0.50(3) 1 calc R . P C 1
H7B H 1.141175 -0.001707 0.257594 0.084 Uiso 0.50(3) 1 calc R . P C 1
C8 C 1.004(4) -0.0438(16) 0.333(3) 0.085(8) Uani 0.50(3) 1 d D U P C 1
H8A H 1.038226 -0.104056 0.338144 0.128 Uiso 0.50(3) 1 calc R . P C 1
H8B H 0.967145 -0.030824 0.383033 0.128 Uiso 0.50(3) 1 calc R . P C 1
H8C H 0.940633 -0.033140 0.293603 0.128 Uiso 0.50(3) 1 calc R . P C 1
C15 C 1.349(4) 0.138(3) 0.406(2) 0.129(15) Uani 0.60(3) 1 d D U P D 1
H15A H 1.406157 0.180913 0.408457 0.155 Uiso 0.60(3) 1 calc R . P D 1
H15B H 1.314483 0.122370 0.459446 0.155 Uiso 0.60(3) 1 calc R . P D 1
C16 C 1.419(3) 0.060(2) 0.3802(19) 0.095(9) Uani 0.60(3) 1 d D U P D 1
H16A H 1.484166 0.037483 0.416646 0.143 Uiso 0.60(3) 1 calc R . P D 1
H16B H 1.363608 0.016468 0.378946 0.143 Uiso 0.60(3) 1 calc R . P D 1
H16C H 1.455308 0.075028 0.327943 0.143 Uiso 0.60(3) 1 calc R . P D 1
C21 C 0.801(4) 0.399(2) 0.4380(17) 0.097(9) Uani 0.48(3) 1 d D U P E 1
H21A H 0.734985 0.361392 0.446219 0.116 Uiso 0.48(3) 1 calc R . P E 1
H21B H 0.851120 0.387941 0.484857 0.116 Uiso 0.48(3) 1 calc R . P E 1
C22 C 0.746(4) 0.488(3) 0.429(3) 0.101(8) Uani 0.48(3) 1 d D U P E 1
H22A H 0.695917 0.498133 0.475103 0.151 Uiso 0.48(3) 1 calc R . P E 1
H22B H 0.811286 0.525481 0.421422 0.151 Uiso 0.48(3) 1 calc R . P E 1
H22C H 0.695204 0.498944 0.382802 0.151 Uiso 0.48(3) 1 calc R . P E 1
C7' C 0.992(3) 0.0250(14) 0.312(2) 0.081(9) Uani 0.50(3) 1 d D U P C 2
H7'A H 0.944932 0.021538 0.265836 0.098 Uiso 0.50(3) 1 calc R . P C 2
H7'B H 0.933284 0.026999 0.357487 0.098 Uiso 0.50(3) 1 calc R . P C 2
C8' C 1.084(4) -0.0528(14) 0.327(3) 0.089(8) Uani 0.50(3) 1 d D U P C 2
H8'A H 1.041507 -0.104317 0.335679 0.134 Uiso 0.50(3) 1 calc R . P C 2
H8'B H 1.141007 -0.055139 0.282163 0.134 Uiso 0.50(3) 1 calc R . P C 2
H8'C H 1.129381 -0.049689 0.373644 0.134 Uiso 0.50(3) 1 calc R . P C 2
C15' C 1.329(4) 0.093(2) 0.360(3) 0.086(13) Uani 0.40(3) 1 d D U P D 2
H15C H 1.278363 0.044736 0.364125 0.103 Uiso 0.40(3) 1 calc R . P D 2
H15D H 1.382893 0.091128 0.312814 0.103 Uiso 0.40(3) 1 calc R . P D 2
C16' C 1.405(5) 0.082(3) 0.430(3) 0.104(11) Uani 0.40(3) 1 d D U P D 2
H16D H 1.457695 0.027736 0.433586 0.156 Uiso 0.40(3) 1 calc R . P D 2
H16E H 1.456118 0.129364 0.425782 0.156 Uiso 0.40(3) 1 calc R . P D 2
H16F H 1.351693 0.083020 0.477042 0.156 Uiso 0.40(3) 1 calc R . P D 2
C21' C 0.787(4) 0.451(2) 0.389(2) 0.099(9) Uani 0.52(3) 1 d D U P E 2
H21C H 0.824411 0.505483 0.378096 0.119 Uiso 0.52(3) 1 calc R . P E 2
H21D H 0.715850 0.456256 0.355356 0.119 Uiso 0.52(3) 1 calc R . P E 2
C22' C 0.746(4) 0.438(3) 0.4698(18) 0.097(8) Uani 0.52(3) 1 d D U P E 2
H22D H 0.686088 0.486270 0.480320 0.145 Uiso 0.52(3) 1 calc R . P E 2
H22E H 0.707232 0.384920 0.480569 0.145 Uiso 0.52(3) 1 calc R . P E 2
H22F H 0.815788 0.434145 0.503308 0.145 Uiso 0.52(3) 1 calc R . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W3 Cl5 2.362(4) . ?
W3 O22 1.686(13) . ?
W3 O27 1.864(10) . ?
W3 Cl6 2.811(5) . ?
W3 O24 1.907(7) . ?
W3 O25 1.930(7) . ?
W3 Cl6' 2.816(14) . ?
W3 O24' 1.905(10) . ?
W3 O25' 1.953(9) . ?
O27 C27 1.400(18) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C27 H27D 0.9700 . ?
C27 C28 1.51(3) . ?
C27 C28' 1.51(3) . ?
W1 Cl2 2.352(7) . ?
W1 Cl3 2.382(11) . ?
W1 Cl6 2.819(5) . ?
W1 O20 1.639(18) . ?
W1 O23 1.912(8) . ?
W1 O25 1.920(8) . ?
W2 Cl4 2.366(7) . ?
W2 Cl6 2.775(5) . ?
W2 O21 1.707(13) . ?
W2 O23 1.922(7) . ?
W2 O24 1.903(8) . ?
W2 O26 1.879(14) . ?
O26 C25 1.43(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.45(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
W1' Cl2' 2.349(11) . ?
W1' Cl3' 2.27(3) . ?
W1' Cl6' 2.814(13) . ?
W1' O20' 1.64(2) . ?
W1' O23' 1.914(9) . ?
W1' O25' 1.948(9) . ?
W2' Cl4' 2.37(2) . ?
W2' Cl6' 2.790(13) . ?
W2' O21' 1.699(16) . ?
W2' O23' 1.916(9) . ?
W2' O24' 2.01(3) . ?
W2' O26' 1.876(17) . ?
O26' C25' 1.42(3) . ?
C25' H25C 0.9700 . ?
C25' H25D 0.9700 . ?
C25' C26' 1.45(4) . ?
C26' H26D 0.9600 . ?
C26' H26E 0.9600 . ?
C26' H26F 0.9600 . ?
C28' H28D 0.9600 . ?
C28' H28E 0.9600 . ?
C28' H28F 0.9600 . ?
V1 Cl1 2.262(5) . ?
V1 O7 1.977(9) . ?
V1 O8 2.001(9) . ?
V1 O9 1.970(10) . ?
V1 O10 1.976(10) . ?
V1 O19 2.172(7) . ?
V2 O2 1.613(13) . ?
V2 O7 1.950(9) . ?
V2 O11 2.008(11) . ?
V2 O14 1.981(11) . ?
V2 O15 1.968(10) . ?
V2 O19 2.287(8) . ?
V3 O3 1.624(10) . ?
V3 O8 1.917(9) . ?
V3 O11 1.944(11) . ?
V3 O12 1.952(11) . ?
V3 O16 1.984(9) . ?
V3 O19 2.268(8) . ?
V4 O4 1.572(13) . ?
V4 O9 1.945(10) . ?
V4 O12 1.997(11) . ?
V4 O13 1.973(11) . ?
V4 O17 1.981(10) . ?
V4 O19 2.305(8) . ?
V5 O5 1.651(14) . ?
V5 O10 1.939(10) . ?
V5 O13 1.953(12) . ?
V5 O14 1.968(12) . ?
V5 O18 1.961(9) . ?
V5 O19 2.283(8) . ?
V6 O6 1.594(10) . ?
V6 O15 1.958(12) . ?
V6 O16 1.972(9) . ?
V6 O17 1.956(12) . ?
V6 O18 1.979(10) . ?
V6 O19 2.277(7) . ?
O7 C1 1.433(16) . ?
O8 C3 1.428(16) . ?
O9 C5 1.476(17) . ?
O10 C7 1.46(2) . ?
O10 C7' 1.46(2) . ?
O11 C9 1.452(16) . ?
O12 C11 1.47(2) . ?
O13 C13 1.45(2) . ?
O14 C15 1.51(3) . ?
O14 C15' 1.50(3) . ?
O15 C17 1.46(3) . ?
O16 C19 1.406(18) . ?
O17 C21 1.48(2) . ?
O17 C21' 1.48(2) . ?
O18 C23 1.437(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.471(19) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.45(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.50(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.43(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.43(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.34(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.44(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.41(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.45(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.47(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.46(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.42(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C7' C8' 1.47(3) . ?
C8' H8'A 0.9600 . ?
C8' H8'B 0.9600 . ?
C8' H8'C 0.9600 . ?
C15' H15C 0.9700 . ?
C15' H15D 0.9700 . ?
C15' C16' 1.46(4) . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
C21' C22' 1.42(3) . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?

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
Cl5 W3 Cl6 84.07(14) . . ?
Cl5 W3 Cl6' 90.0(3) . . ?
O22 W3 Cl5 99.7(5) . . ?
O22 W3 O27 103.1(6) . . ?
O22 W3 Cl6 173.5(5) . . ?
O22 W3 O24 98.6(6) . . ?
O22 W3 O25 95.8(6) . . ?
O22 W3 Cl6' 170.2(6) . . ?
O22 W3 O24' 109.0(15) . . ?
O22 W3 O25' 111.4(11) . . ?
O27 W3 Cl5 87.1(4) . . ?
O27 W3 Cl6 82.3(3) . . ?
O27 W3 O24 156.9(5) . . ?
O27 W3 O25 93.7(6) . . ?
O27 W3 Cl6' 76.1(4) . . ?
O27 W3 O24' 147.5(14) . . ?
O27 W3 O25' 93.7(15) . . ?
O24 W3 Cl5 81.5(5) . . ?
O24 W3 Cl6 76.6(4) . . ?
O24 W3 O25 92.0(7) . . ?
O25 W3 Cl5 163.9(3) . . ?
O25 W3 Cl6 80.1(3) . . ?
O24' W3 Cl5 92.8(14) . . ?
O24' W3 Cl6' 71.4(14) . . ?
O24' W3 O25' 70(2) . . ?
O25' W3 Cl5 147.7(10) . . ?
O25' W3 Cl6' 59.2(10) . . ?
C27 O27 W3 141.9(11) . . ?
O27 C27 H27A 109.5 . . ?
O27 C27 H27B 109.5 . . ?
O27 C27 H27C 109.3 . . ?
O27 C27 H27D 109.3 . . ?
O27 C27 C28 110.6(16) . . ?
O27 C27 C28' 112(4) . . ?
H27A C27 H27B 108.1 . . ?
H27C C27 H27D 108.0 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C28' C27 H27C 109.3 . . ?
C28' C27 H27D 109.3 . . ?
Cl2 W1 Cl3 85.4(4) . . ?
Cl2 W1 Cl6 83.2(3) . . ?
Cl3 W1 Cl6 82.2(3) . . ?
O20 W1 Cl2 100.1(10) . . ?
O20 W1 Cl3 99.5(15) . . ?
O20 W1 Cl6 176.4(11) . . ?
O20 W1 O23 101.3(10) . . ?
O20 W1 O25 98.8(15) . . ?
O23 W1 Cl2 158.6(5) . . ?
O23 W1 Cl3 92.6(7) . . ?
O23 W1 Cl6 75.4(4) . . ?
O23 W1 O25 91.7(8) . . ?
O25 W1 Cl2 83.5(6) . . ?
O25 W1 Cl3 160.0(5) . . ?
O25 W1 Cl6 80.0(3) . . ?
Cl4 W2 Cl6 82.7(2) . . ?
O21 W2 Cl4 101.4(6) . . ?
O21 W2 Cl6 174.3(5) . . ?
O21 W2 O23 100.0(6) . . ?
O21 W2 O24 97.9(7) . . ?
O21 W2 O26 102.4(7) . . ?
O23 W2 Cl4 84.6(6) . . ?
O23 W2 Cl6 76.4(4) . . ?
O24 W2 Cl4 159.6(4) . . ?
O24 W2 Cl6 77.6(4) . . ?
O24 W2 O23 85.4(7) . . ?
O26 W2 Cl4 87.5(4) . . ?
O26 W2 Cl6 81.6(5) . . ?
O26 W2 O23 157.3(6) . . ?
O26 W2 O24 95.1(6) . . ?
W3 Cl6 W1 74.05(13) . . ?
W2 Cl6 W3 75.96(14) . . ?
W2 Cl6 W1 76.84(13) . . ?
W1 O23 W2 130.1(7) . . ?
W2 O24 W3 128.9(7) . . ?
W1 O25 W3 123.4(6) . . ?
C25 O26 W2 134.9(16) . . ?
O26 C25 H25A 110.2 . . ?
O26 C25 H25B 110.2 . . ?
O26 C25 C26 107.7(19) . . ?
H25A C25 H25B 108.5 . . ?
C26 C25 H25A 110.2 . . ?
C26 C25 H25B 110.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl2' W1' Cl6' 80.7(9) . . ?
Cl3' W1' Cl2' 84.8(12) . . ?
Cl3' W1' Cl6' 88.8(9) . . ?
O20' W1' Cl2' 101(3) . . ?
O20' W1' Cl3' 104(4) . . ?
O20' W1' Cl6' 167(4) . . ?
O20' W1' O23' 102(3) . . ?
O20' W1' O25' 108(4) . . ?
O23' W1' Cl2' 156.9(11) . . ?
O23' W1' Cl3' 93(2) . . ?
O23' W1' Cl6' 76.3(6) . . ?
O23' W1' O25' 77(2) . . ?
O25' W1' Cl2' 92.9(17) . . ?
O25' W1' Cl3' 147.8(13) . . ?
O25' W1' Cl6' 59.2(10) . . ?
Cl4' W2' Cl6' 87.7(7) . . ?
O21' W2' Cl4' 96.5(18) . . ?
O21' W2' Cl6' 173.3(14) . . ?
O21' W2' O23' 98.1(15) . . ?
O21' W2' O24' 105(2) . . ?
O21' W2' O26' 97(2) . . ?
O23' W2' Cl4' 87.0(19) . . ?
O23' W2' Cl6' 76.9(6) . . ?
O23' W2' O24' 88(2) . . ?
O24' W2' Cl4' 158.4(12) . . ?
O24' W2' Cl6' 70.7(10) . . ?
O26' W2' Cl4' 90.3(13) . . ?
O26' W2' Cl6' 87.9(14) . . ?
O26' W2' O23' 164.6(16) . . ?
O26' W2' O24' 89.1(18) . . ?
W1' Cl6' W3 85.3(4) . . ?
W2' Cl6' W3 81.0(4) . . ?
W2' Cl6' W1' 76.5(4) . . ?
W1' O23' W2' 130.0(10) . . ?
W3 O24' W2' 137(2) . . ?
W1' O25' W3 156.1(19) . . ?
C25' O26' W2' 159(5) . . ?
O26' C25' H25C 110.3 . . ?
O26' C25' H25D 110.3 . . ?
O26' C25' C26' 107(3) . . ?
H25C C25' H25D 108.5 . . ?
C26' C25' H25C 110.3 . . ?
C26' C25' H25D 110.3 . . ?
C25' C26' H26D 109.5 . . ?
C25' C26' H26E 109.5 . . ?
C25' C26' H26F 109.5 . . ?
H26D C26' H26E 109.5 . . ?
H26D C26' H26F 109.5 . . ?
H26E C26' H26F 109.5 . . ?
C27 C28' H28D 109.5 . . ?
C27 C28' H28E 109.5 . . ?
C27 C28' H28F 109.5 . . ?
H28D C28' H28E 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
O7 V1 Cl1 97.3(3) . . ?
O7 V1 O8 88.2(4) . . ?
O7 V1 O19 82.6(3) . . ?
O8 V1 Cl1 96.4(3) . . ?
O8 V1 O19 82.5(3) . . ?
O9 V1 Cl1 97.4(3) . . ?
O9 V1 O7 165.2(4) . . ?
O9 V1 O8 88.2(4) . . ?
O9 V1 O10 90.6(4) . . ?
O9 V1 O19 82.7(4) . . ?
O10 V1 Cl1 98.0(3) . . ?
O10 V1 O7 89.3(4) . . ?
O10 V1 O8 165.6(4) . . ?
O10 V1 O19 83.1(3) . . ?
O19 V1 Cl1 178.9(3) . . ?
O2 V2 O7 101.8(5) . . ?
O2 V2 O11 99.6(7) . . ?
O2 V2 O14 101.3(7) . . ?
O2 V2 O15 98.6(5) . . ?
O2 V2 O19 177.6(5) . . ?
O7 V2 O11 87.3(4) . . ?
O7 V2 O14 88.4(4) . . ?
O7 V2 O15 159.6(4) . . ?
O7 V2 O19 80.3(3) . . ?
O11 V2 O19 79.2(4) . . ?
O14 V2 O11 159.1(5) . . ?
O14 V2 O19 79.9(4) . . ?
O15 V2 O11 88.8(4) . . ?
O15 V2 O14 88.2(5) . . ?
O15 V2 O19 79.4(4) . . ?
O3 V3 O8 100.0(4) . . ?
O3 V3 O11 98.3(6) . . ?
O3 V3 O12 99.5(6) . . ?
O3 V3 O16 98.6(4) . . ?
O3 V3 O19 178.0(4) . . ?
O8 V3 O11 88.3(4) . . ?
O8 V3 O12 90.0(4) . . ?
O8 V3 O16 161.3(4) . . ?
O8 V3 O19 81.9(3) . . ?
O11 V3 O12 162.2(4) . . ?
O11 V3 O16 87.6(4) . . ?
O11 V3 O19 81.0(4) . . ?
O12 V3 O16 88.3(4) . . ?
O12 V3 O19 81.2(4) . . ?
O16 V3 O19 79.5(3) . . ?
O4 V4 O9 101.8(6) . . ?
O4 V4 O12 101.2(6) . . ?
O4 V4 O13 100.6(7) . . ?
O4 V4 O17 99.4(6) . . ?
O4 V4 O19 178.3(6) . . ?
O9 V4 O12 87.5(4) . . ?
O9 V4 O13 89.1(4) . . ?
O9 V4 O17 158.8(4) . . ?
O9 V4 O19 79.8(3) . . ?
O12 V4 O19 79.4(4) . . ?
O13 V4 O12 158.2(4) . . ?
O13 V4 O17 87.5(4) . . ?
O13 V4 O19 78.8(4) . . ?
O17 V4 O12 87.9(4) . . ?
O17 V4 O19 79.0(4) . . ?
O5 V5 O10 99.5(5) . . ?
O5 V5 O13 100.0(6) . . ?
O5 V5 O14 100.0(6) . . ?
O5 V5 O18 99.3(5) . . ?
O5 V5 O19 179.4(5) . . ?
O10 V5 O13 89.0(4) . . ?
O10 V5 O14 88.3(5) . . ?
O10 V5 O18 161.2(4) . . ?
O10 V5 O19 81.0(3) . . ?
O13 V5 O14 160.0(4) . . ?
O13 V5 O18 87.8(5) . . ?
O13 V5 O19 79.7(4) . . ?
O14 V5 O19 80.3(4) . . ?
O18 V5 O14 88.4(5) . . ?
O18 V5 O19 80.2(3) . . ?
O6 V6 O15 100.4(6) . . ?
O6 V6 O16 99.0(4) . . ?
O6 V6 O17 99.6(6) . . ?
O6 V6 O18 101.5(4) . . ?
O6 V6 O19 178.5(4) . . ?
O15 V6 O16 87.5(5) . . ?
O15 V6 O18 88.4(5) . . ?
O15 V6 O19 79.8(3) . . ?
O16 V6 O18 159.5(4) . . ?
O16 V6 O19 79.5(3) . . ?
O17 V6 O15 160.0(4) . . ?
O17 V6 O16 88.6(5) . . ?
O17 V6 O18 88.4(5) . . ?
O17 V6 O19 80.2(3) . . ?
O18 V6 O19 80.0(3) . . ?
V2 O7 V1 107.0(4) . . ?
C1 O7 V1 127.5(8) . . ?
C1 O7 V2 121.8(8) . . ?
V3 O8 V1 106.0(4) . . ?
C3 O8 V1 130.8(9) . . ?
C3 O8 V3 122.7(9) . . ?
V4 O9 V1 107.7(4) . . ?
C5 O9 V1 123.2(9) . . ?
C5 O9 V4 125.2(9) . . ?
V5 O10 V1 106.4(4) . . ?
C7 O10 V1 128.0(14) . . ?
C7 O10 V5 120.8(14) . . ?
C7' O10 V1 121.5(16) . . ?
C7' O10 V5 121.6(16) . . ?
V3 O11 V2 109.5(5) . . ?
C9 O11 V2 125.1(10) . . ?
C9 O11 V3 121.3(10) . . ?
V3 O12 V4 109.6(4) . . ?
C11 O12 V3 121.9(11) . . ?
C11 O12 V4 124.0(11) . . ?
V5 O13 V4 111.5(5) . . ?
C13 O13 V4 118.9(15) . . ?
C13 O13 V5 125.2(15) . . ?
V5 O14 V2 109.8(4) . . ?
C15 O14 V2 125(2) . . ?
C15 O14 V5 123(2) . . ?
C15' O14 V2 122(2) . . ?
C15' O14 V5 117(2) . . ?
V6 O15 V2 110.7(4) . . ?
C17 O15 V2 123.8(15) . . ?
C17 O15 V6 123.1(15) . . ?
V6 O16 V3 110.0(4) . . ?
C19 O16 V3 123.9(9) . . ?
C19 O16 V6 124.2(10) . . ?
V6 O17 V4 110.8(5) . . ?
C21 O17 V4 121(2) . . ?
C21 O17 V6 122(2) . . ?
C21' O17 V4 120(2) . . ?
C21' O17 V6 124(2) . . ?
V5 O18 V6 109.8(4) . . ?
C23 O18 V5 121.8(9) . . ?
C23 O18 V6 123.1(10) . . ?
V1 O19 V2 90.1(3) . . ?
V1 O19 V3 89.6(3) . . ?
V1 O19 V4 89.8(3) . . ?
V1 O19 V5 89.4(3) . . ?
V1 O19 V6 179.4(4) . . ?
V2 O19 V4 179.9(4) . . ?
V3 O19 V2 90.3(3) . . ?
V3 O19 V4 89.8(3) . . ?
V3 O19 V5 179.0(4) . . ?
V3 O19 V6 91.0(3) . . ?
V5 O19 V2 90.0(3) . . ?
V5 O19 V4 90.0(3) . . ?
V6 O19 V2 90.1(3) . . ?
V6 O19 V4 90.1(3) . . ?
V6 O19 V5 90.0(3) . . ?
O7 C1 H1A 109.2 . . ?
O7 C1 H1B 109.2 . . ?
O7 C1 C2 112.2(12) . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 H3A 108.7 . . ?
O8 C3 H3B 108.7 . . ?
O8 C3 C4 114.4(16) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O9 C5 H5A 109.5 . . ?
O9 C5 H5B 109.5 . . ?
O9 C5 C6 110.6(13) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O11 C9 H9A 109.3 . . ?
O11 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 O11 111.7(13) . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
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 . . ?
O12 C11 H11A 109.3 . . ?
O12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 O12 111.5(17) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 C13 H13A 108.1 . . ?
O13 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 O13 117(3) . . ?
C14 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
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 . . ?
O15 C17 H17A 109.1 . . ?
O15 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 O15 113(2) . . ?
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 . . ?
O16 C19 H19A 107.9 . . ?
O16 C19 H19B 107.9 . . ?
O16 C19 C20 118(2) . . ?
H19A C19 H19B 107.2 . . ?
C20 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O18 C23 H23A 108.8 . . ?
O18 C23 H23B 108.8 . . ?
O18 C23 C24 113.7(16) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O10 C7 H7A 109.5 . . ?
O10 C7 H7B 109.5 . . ?
O10 C7 C8 110.9(19) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O14 C15 H15A 109.0 . . ?
O14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C16 C15 O14 113(2) . . ?
C16 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O17 C21 H21A 109.2 . . ?
O17 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 O17 112(2) . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
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 . . ?
O10 C7' H7'A 109.6 . . ?
O10 C7' H7'B 109.6 . . ?
O10 C7' C8' 110(2) . . ?
H7'A C7' H7'B 108.1 . . ?
C8' C7' H7'A 109.6 . . ?
C8' C7' H7'B 109.6 . . ?
C7' C8' H8'A 109.5 . . ?
C7' C8' H8'B 109.5 . . ?
C7' C8' H8'C 109.5 . . ?
H8'A C8' H8'B 109.5 . . ?
H8'A C8' H8'C 109.5 . . ?
H8'B C8' H8'C 109.5 . . ?
O14 C15' H15C 109.3 . . ?
O14 C15' H15D 109.3 . . ?
H15C C15' H15D 108.0 . . ?
C16' C15' O14 111(2) . . ?
C16' C15' H15C 109.3 . . ?
C16' C15' H15D 109.3 . . ?
C15' C16' H16D 109.5 . . ?
C15' C16' H16E 109.5 . . ?
C15' C16' H16F 109.5 . . ?
H16D C16' H16E 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
O17 C21' H21C 109.1 . . ?
O17 C21' H21D 109.1 . . ?
H21C C21' H21D 107.8 . . ?
C22' C21' O17 113(2) . . ?
C22' C21' H21C 109.1 . . ?
C22' C21' H21D 109.1 . . ?
C21' C22' H22D 109.5 . . ?
C21' C22' H22E 109.5 . . ?
C21' C22' H22F 109.5 . . ?
H22D C22' H22E 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 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
W3 O27 C27 C28 145(3) . . . . ?
W3 O27 C27 C28' -178(8) . . . . ?
Cl5 W3 O27 C27 -58.3(15) . . . . ?
O22 W3 O27 C27 -157.6(16) . . . . ?
W2 O26 C25 C26 128.2(18) . . . . ?
Cl4 W2 O26 C25 -44.4(17) . . . . ?
Cl6 W3 O27 C27 26.1(15) . . . . ?
Cl6 W2 O26 C25 38.7(17) . . . . ?
O21 W2 O26 C25 -145.5(18) . . . . ?
O23 W2 O26 C25 25(3) . . . . ?
O24 W3 O27 C27 2(2) . . . . ?
O24 W2 O26 C25 115.3(17) . . . . ?
O25 W3 O27 C27 105.6(16) . . . . ?
W2' O26' C25' C26' 114(9) . . . . ?
Cl4' W2' O26' C25' -83(9) . . . . ?
Cl6' W3 O27 C27 32.5(15) . . . . ?
Cl6' W2' O26' C25' 5(9) . . . . ?
O21' W2' O26' C25' -179(9) . . . . ?
O23' W2' O26' C25' -3(14) . . . . ?
O24' W3 O27 C27 32(3) . . . . ?
O24' W2' O26' C25' 76(9) . . . . ?
O25' W3 O27 C27 89.4(18) . . . . ?
V1 O7 C1 C2 -95.3(14) . . . . ?
V1 O8 C3 C4 112.2(15) . . . . ?
V1 O9 C5 C6 113.4(15) . . . . ?
V1 O10 C7 C8 -110(3) . . . . ?
V1 O10 C7' C8' 122(3) . . . . ?
V2 O7 C1 C2 109.2(12) . . . . ?
V2 O11 C9 C10 98.4(18) . . . . ?
V2 O14 C15 C16 -91(4) . . . . ?
V2 O14 C15' C16' 117(4) . . . . ?
V2 O15 C17 C18 -94(2) . . . . ?
V3 O8 C3 C4 -77.7(16) . . . . ?
V3 O11 C9 C10 -106.8(17) . . . . ?
V3 O12 C11 C12 127.8(17) . . . . ?
V3 O16 C19 C20 -115.3(17) . . . . ?
V4 O9 C5 C6 -91.8(16) . . . . ?
V4 O12 C11 C12 -79(2) . . . . ?
V4 O13 C13 C14 106(3) . . . . ?
V4 O17 C21 C22 -114(4) . . . . ?
V4 O17 C21' C22' 109(4) . . . . ?
V5 O10 C7 C8 98(3) . . . . ?
V5 O10 C7' C8' -98(3) . . . . ?
V5 O13 C13 C14 -100(3) . . . . ?
V5 O14 C15 C16 109(3) . . . . ?
V5 O14 C15' C16' -103(4) . . . . ?
V5 O18 C23 C24 -131.9(15) . . . . ?
V6 O15 C17 C18 105(2) . . . . ?
V6 O16 C19 C20 82(2) . . . . ?
V6 O17 C21 C22 96(4) . . . . ?
V6 O17 C21' C22' -98(4) . . . . ?
V6 O18 C23 C24 77(2) . . . . ?

_olex2_submission_original_sample_id matbp48
_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 3.617
_oxdiff_exptl_absorpt_empirical_full_min 0.232
####################################################################### 
# 
# 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_matbp32
_database_code_depnum_ccdc_archive 'CCDC 1990064'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;

_vrf_PLAT341_matbp32             
;
PROBLEM: _B Low Bond Precision on  C-C Bonds ............... 0.02 Ang. 
RESPONSE: The best crystals were poorly-diffracting multiple-component
twins.
;

_vrf_PLAT301_matbp32             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 55% 
RESPONSE: The two unique terminal ligand sites were modeled as
disorders of O and Cl, fixed in a summed ratio of 1.66667:0.33333,
which was the ratio provided by the chemist from known synthetic
and independent spectroscopic means. As a test, when the occupancies
at the two sites were allowed to refine independently, the ratios
and R1 (strong data) remained essentially the same. Ethoxy ligands
O3-C1-C2 and O6-C7-C8 are modeled as disordered over two positions,
0.54(1):0.46(1) and 0.68(1):0.32(1), respectively. Ethoxy ligand
O4-C3-C4 is modeled as disordered over a crystallographic two-fold
axis (0.50:0.50).
;

_vrf_PLAT860_matbp32             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 36 
RESPONSE: For the two unique terminal ligand site disorders, the
V-O and V-Cl bond lengths were restrained to be similar,
respectively. Analogous bond lengths and angles for the disordered
ethoxy ligands were restrained to be similar. Anisotropic
displacement parameters for proximal atoms were restrained to be
similar and/or constrained to be equivalent.
;

_vrf_PLAT870_matbp32             
;
PROBLEM: _G ALERTS Related to Twinning Effects Suppressed! 
RESPONSE: All the crystals appeared to be twinned to varying
degrees. Attempts to integrate the intensity data as
non-merohedrally twinned did not appear to improve the overall
structure quality. However, post-integration application of
non-merohedral twin law
[0.501 0.499 0.452 / 1.501 -0.501 0.452 / 0 0 -1], a 180 degree
rotation around direct lattice [110], using the TWINROTMAT
routine of program Platon (Spek, 2015) improved R1 (strong data)
from 0.093 to 0.071. The mass ratio of the two components
refined to 0.641(12):0.359(12).
;

_audit_creation_date             2019-09-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H60 Cl1 O18 V6'
_chemical_formula_sum            'C24 H60 Cl O18 V6'
_chemical_formula_weight         977.71
_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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 1 2/m 1'
_space_group_name_Hall           '-I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.7617(7)
_cell_length_b                   17.7653(9)
_cell_length_c                   10.9667(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.866(7)
_cell_angle_gamma                90
_cell_volume                     1995.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2544
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      75.6040
_cell_measurement_theta_min      4.9260
_shelx_estimated_absorpt_T_max   0.389
_shelx_estimated_absorpt_T_min   0.171
_exptl_absorpt_coefficient_mu    12.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1006
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.093
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            2173
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.049
_diffrn_reflns_theta_min         4.914
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     52.00  78.00   0.50    0.05    --   49.62  46.00  20.00   52
  2  ω     81.00 122.00   0.50    0.05    --   49.62  46.00  20.00   82
  3  ω   -154.00-116.00   0.50    0.09    --  -84.25 -46.00-128.00   76
  4  ω    123.00 177.00   0.50    0.09    --  105.75  46.00  20.00  108
  5  ω    116.00 174.00   0.50    0.09    --  105.75  99.00-120.00  116
  6  ω     37.00 106.00   0.50    0.09    --  105.75 -84.00  26.00  138
  7  ω    -84.00 -47.00   0.50    0.05    --  -49.62 -46.00-128.00   74
  8  ω   -119.00 -92.00   0.50    0.05    --  -49.62 -46.00-128.00   54
  9  ω   -121.00 -73.00   0.50    0.05    --  -49.62-125.00 150.00   96
 10  ω     -4.00  21.00   0.50    0.05    --  -49.62  19.00 150.00   50
 11  ω    -14.00  11.00   0.50    0.05    --   49.62 -19.00  30.00   50
 12  ω    100.00 164.00   0.50    0.09    --  105.75  15.00 -60.00  128
 13  ω     48.00  73.00   0.50    0.09    --  105.75 -61.00 -90.00   50
 14  ω     40.00  74.00   0.50    0.09    --  105.75 -61.00-180.00   68
 15  ω     74.00 102.00   0.50    0.09    --  105.75 -94.00 -30.00   56
 16  ω    138.00 174.00   0.50    0.09    --  105.75  15.00   0.00   72
 17  ω     41.00  67.00   0.50    0.09    --  105.75 -61.00 150.00   52
 18  ω    104.00 133.00   0.50    0.09    --  105.75  45.00   0.00   58
 19  ω    151.00 176.00   0.50    0.09    --  105.75  45.00   0.00   50
 20  ω    114.00 153.00   0.50    0.09    --  105.75  30.00-120.00   78
 21  ω     98.00 126.00   0.50    0.09    --  105.75  15.00   0.00   56
 22  ω     51.00  77.00   0.50    0.09    --  105.75 -61.00 -30.00   52
 23  ω     36.00  78.00   0.50    0.09    --  105.75 -61.00-150.00   84
 24  ω     35.00  78.00   0.50    0.09    --  105.75 -61.00  30.00   86
 25  ω   -121.00 -88.00   0.50    0.05    --  -49.87 -46.00-128.00   66
 26  ω   -118.00 -82.00   0.50    0.05    --  -49.87-125.00  30.00   72
 27  ω    -46.00  15.00   0.50    0.05    --  -49.87  46.00  20.00  122
 28  ω    -12.00  13.00   0.50    0.05    --   49.87 -19.00  60.00   50
 29  ω     50.00  80.00   0.50    0.09    --  105.75 -61.00 -60.00   60
 30  ω     49.00  75.00   0.50    0.09    --  105.75 -61.00  60.00   52
 31  ω    111.00 137.00   0.50    0.09    --  105.75  15.00 150.00   52
 32  ω     61.00  88.00   0.50    0.09    --  105.75 -94.00  90.00   54
 33  ω     98.00 170.00   0.50    0.09    --  105.75  30.00  90.00  144
 34  ω     35.00  78.00   0.50    0.09    --  105.75 -61.00  90.00   86
 35  ω    106.00 135.00   0.50    0.09    --  105.75  15.00-180.00   58
 36  ω    150.00 175.00   0.50    0.09    --  105.75  15.00-180.00   50
 37  ω     49.00  75.00   0.50    0.09    --  105.75 -61.00-120.00   52
 38  ω     51.00  77.00   0.50    0.09    --  105.75 -61.00 -90.00   52
 39  ω     37.00  67.00   0.50    0.09    --  105.75 -61.00 120.00   60
 40  ω    100.00 126.00   0.50    0.09    --  105.75  48.00 -62.00   52
 41  ω    -44.00 -16.00   0.50    0.05    --  -49.87  57.00  90.00   56
 42  ω     60.00  87.00   0.50    0.05    --   49.87-125.00 -30.00   54
 43  ω     44.00  71.00   0.50    0.09    --  105.75 -94.00-150.00   54
 44  ω     65.00 105.00   0.50    0.09    --  105.75 -94.00 150.00   80
 45  ω     47.00  73.00   0.50    0.09    --  105.75 -94.00  90.00   52
 46  ω     81.00 106.00   0.50    0.09    --  105.75 -94.00  90.00   50
 47  ω     53.00  79.00   0.50    0.09    --  105.75 -61.00   0.00   52
 48  ω     34.00  59.00   0.50    0.09    --  105.75 -61.00  30.00   50
 49  ω     81.00 106.00   0.50    0.09    --  105.75 -94.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0753410000
_diffrn_orient_matrix_UB_12      0.0367035000
_diffrn_orient_matrix_UB_13      0.0834140000
_diffrn_orient_matrix_UB_21      0.1277238000
_diffrn_orient_matrix_UB_22      0.0353746000
_diffrn_orient_matrix_UB_23      0.0854730000
_diffrn_orient_matrix_UB_31      -0.0249951000
_diffrn_orient_matrix_UB_32      0.0701525000
_diffrn_orient_matrix_UB_33      -0.0867270000
_diffrn_oxdiff_digest_frames     
;
016bcaa00497f3789a65e58c5c20f1c1bf0336647ce
;
_diffrn_oxdiff_digest_hkl        
;
01bb6dea735aa33a591d9929ed49dc081a30c1
;
_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                1400
_reflns_number_total             2173
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0712
_refine_ls_restrained_S_all      1.040
_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)+(0.1499P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2392
_refine_special_details          
;
All the crystals appeared to be twinned to varying
degrees. Attempts to integrate the intensity data as
non-merohedrally twinned did not appear to improve the overall
structure quality. However, post-integration application of
non-merohedral twin law
[0.501 0.499 0.452 / 1.501 -0.501 0.452 / 0 0 -1], a 180 degree
rotation around direct lattice [110], using the TWINROTMAT
routine of program Platon (Spek, 2015) improved R1 (strong data)
from 0.093 to 0.071. The mass ratio of the two components
refined to 0.641(12):0.359(12).

The two unique terminal ligand sites were modeled as disorders
of O and Cl, fixed in a summed ratio of 1.66667:0.33333,
which was the ratio provided by the chemist from known synthetic
and independent spectroscopic means. As a test, when the occupancies
at the two sites were allowed to refine independently, the ratios
and R1 (strong data) remained essentially the same. Ethoxy ligands
O3-C1-C2 and O6-C7-C8 are modeled as disordered over two positions,
0.54(1):0.46(1) and 0.68(1):0.32(1), respectively. Ethoxy ligand
O4-C3-C4 is modeled as disordered over a crystallographic two-fold
axis (0.50:0.50).

For the two unique terminal ligand site disorders, the V-O and
V-Cl bond lengths were restrained to be similar, respectively.
Analogous bond lengths and angles for the disordered ethoxy
ligands were restrained to be similar. Anisotropic displacement
parameters for proximal atoms were restrained to be similar
and/or constrained to be equivalent.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.641(12)
 0.359(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 V1-O1 \\sim V2-O2
 with sigma of 0.01
 V1-Cl1 \\sim V2-Cl2
 with sigma of 0.01
 O3-C1 \\sim O3-C1' \\sim O6-C7 \\sim O6-C7'
 with sigma of 0.01
 C1-C2 \\sim C1'-C2'
 with sigma of 0.01
 O3-C2 \\sim O3-C2
 with sigma of 0.02
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 O6-C8 \\sim O6-C8'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim C1 \\sim C2: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
O4 \\sim C3 \\sim C4: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C7) = Uanis(C7')
Uanis(C8) = Uanis(C8')
Uanis(O1) = Uanis(Cl1)
Uanis(O2) = Uanis(Cl2)
Uanis(C1) = Uanis(C1')
Uanis(C2) = Uanis(C2')
5. Others
 1*[Sof(O1)+Sof(Cl1)]+1*[Sof(O2)+Sof(Cl2)]=1.66667 with esd of 0.0001
 Sof(Cl1)=0.5*(1-FVAR(2))
 Sof(O1)=0.5*FVAR(2)
 Sof(Cl2)=1-FVAR(2)
 Sof(O2)=FVAR(2)
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(H2'C)=1-FVAR(3)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(3)
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=1-FVAR(4)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(4)
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 H5A(0.5) H5B(0.5) H6B(0.5) H6C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C1'(H1'A,H1'B), C7'(H7'A,
 H7'B)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C2'(H2'A,
 H2'B,H2'C), C8'(H8'A,H8'B,H8'C)
;
_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 0.31844(13) 0.500000 0.56536(13) 0.0703(5) Uani 1 2 d DS T P A .
V2 V 0.59119(10) 0.59061(5) 0.64627(9) 0.0701(4) Uani 1 1 d D . . . .
O1 O 0.1880(8) 0.500000 0.6092(10) 0.093(2) Uani 0.831(2) 2 d DS T P A 1
O2 O 0.6565(7) 0.6556(4) 0.7465(6) 0.0957(16) Uani 0.836(2) 1 d D . . A 1
O3 O 0.4223(5) 0.5783(2) 0.6807(4) 0.0785(11) Uani 1 1 d D U . . .
O4 O 0.500000 0.6551(3) 0.500000 0.0750(14) Uani 1 2 d S TU P A .
O5 O 0.6552(6) 0.500000 0.7505(5) 0.0778(15) Uani 1 2 d S T P A .
O6 O 0.7323(4) 0.5777(2) 0.5699(4) 0.0760(10) Uani 1 1 d D . . . .
O7 O 0.500000 0.500000 0.500000 0.0590(15) Uani 1 4 d S T P A .
C1 C 0.4014(16) 0.5944(8) 0.8045(10) 0.098(3) Uani 0.538(10) 1 d D U . B 1
H1A H 0.372426 0.548579 0.835586 0.117 Uiso 0.538(10) 1 calc R . . B 1
H1B H 0.484372 0.608484 0.865522 0.117 Uiso 0.538(10) 1 calc R . . B 1
C2 C 0.310(3) 0.6516(17) 0.801(2) 0.157(7) Uani 0.538(10) 1 d D U . B 1
H2A H 0.302479 0.658496 0.885387 0.236 Uiso 0.538(10) 1 calc R . . B 1
H2B H 0.339036 0.697710 0.772970 0.236 Uiso 0.538(10) 1 calc R . . B 1
H2C H 0.226896 0.637700 0.742982 0.236 Uiso 0.538(10) 1 calc R . . B 1
C3 C 0.5457(16) 0.7307(7) 0.4819(18) 0.103(4) Uani 0.5 1 d . U . A -1
H3A H 0.630691 0.739586 0.543666 0.123 Uiso 0.5 1 calc R . . A -1
H3B H 0.554209 0.735015 0.396627 0.123 Uiso 0.5 1 calc R . . A -1
C4 C 0.4541(18) 0.7859(7) 0.498(3) 0.130(8) Uani 0.5 1 d . U . A -1
H4A H 0.484246 0.835378 0.486299 0.194 Uiso 0.5 1 calc R . . A -1
H4B H 0.370315 0.777254 0.436320 0.194 Uiso 0.5 1 calc R . . A -1
H4C H 0.446607 0.781813 0.582992 0.194 Uiso 0.5 1 calc R . . A -1
C5 C 0.6833(14) 0.500000 0.8901(11) 0.124(4) Uani 1 2 d S T P . .
H5A H 0.642760 0.544019 0.913987 0.149 Uiso 0.5 1 calc R . . A .
H5B H 0.642760 0.455981 0.913986 0.149 Uiso 0.5 1 calc R . . . .
C6 C 0.8113(17) 0.500000 0.9589(14) 0.184(8) Uani 1 2 d S T P A .
H6A H 0.819948 0.500000 1.048656 0.276 Uiso 1 2 calc RS T P . .
H6B H 0.852448 0.455878 0.938422 0.276 Uiso 0.5 1 calc R . . . .
H6C H 0.852448 0.544122 0.938422 0.276 Uiso 0.5 1 calc R . . . .
C7 C 0.8685(8) 0.5952(6) 0.6361(12) 0.098(3) Uani 0.677(10) 1 d D . . C 1
H7A H 0.885852 0.587167 0.727280 0.117 Uiso 0.677(10) 1 calc R . . C 1
H7B H 0.923905 0.561288 0.606700 0.117 Uiso 0.677(10) 1 calc R . . C 1
C8 C 0.9004(11) 0.6712(7) 0.6146(14) 0.122(4) Uani 0.677(10) 1 d D . . C 1
H8A H 0.990762 0.680495 0.659780 0.184 Uiso 0.677(10) 1 calc R . . C 1
H8B H 0.885023 0.679181 0.524618 0.184 Uiso 0.677(10) 1 calc R . . C 1
H8C H 0.846989 0.705048 0.645140 0.184 Uiso 0.677(10) 1 calc R . . C 1
Cl1 Cl 0.1615(17) 0.500000 0.658(2) 0.093(2) Uani 0.169(2) 2 d DS T P A 2
Cl2 Cl 0.6678(15) 0.6713(8) 0.8078(12) 0.0957(16) Uani 0.164(2) 1 d D . . A 2
C1' C 0.3579(18) 0.6429(8) 0.7196(14) 0.098(3) Uani 0.462(10) 1 d D . . B 2
H1'A H 0.399972 0.689294 0.707310 0.117 Uiso 0.462(10) 1 calc R . . B 2
H1'B H 0.266955 0.645025 0.667768 0.117 Uiso 0.462(10) 1 calc R . . B 2
C2' C 0.367(3) 0.634(2) 0.8491(18) 0.157(7) Uani 0.462(10) 1 d D . . B 2
H2'A H 0.325313 0.676129 0.875975 0.236 Uiso 0.462(10) 1 calc R . . B 2
H2'B H 0.324711 0.588406 0.860299 0.236 Uiso 0.462(10) 1 calc R . . B 2
H2'C H 0.457263 0.632521 0.899703 0.236 Uiso 0.462(10) 1 calc R . . B 2
C7' C 0.8327(16) 0.6350(11) 0.583(2) 0.098(3) Uani 0.323(10) 1 d D . . C 2
H7'A H 0.852608 0.639625 0.503117 0.117 Uiso 0.323(10) 1 calc R . . C 2
H7'B H 0.799679 0.683185 0.601410 0.117 Uiso 0.323(10) 1 calc R . . C 2
C8' C 0.9493(17) 0.6169(16) 0.684(3) 0.122(4) Uani 0.323(10) 1 d D . . C 2
H8'A H 1.013099 0.655658 0.689871 0.184 Uiso 0.323(10) 1 calc R . . C 2
H8'B H 0.930086 0.613204 0.763333 0.184 Uiso 0.323(10) 1 calc R . . C 2
H8'C H 0.982968 0.569683 0.665128 0.184 Uiso 0.323(10) 1 calc R . . C 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 1.617(7) . ?
V1 O3 1.979(4) 6_565 ?
V1 O3 1.979(4) . ?
V1 O6 1.976(4) 5_666 ?
V1 O6 1.976(4) 2_656 ?
V1 O7 2.2783(13) . ?
V1 Cl1 2.221(11) . ?
V2 O2 1.600(6) . ?
V2 O3 1.979(5) . ?
V2 O4 1.971(3) . ?
V2 O5 1.972(3) . ?
V2 O6 1.960(4) . ?
V2 O7 2.2718(9) . ?
V2 Cl2 2.231(10) . ?
O3 C1 1.470(9) . ?
O3 C1' 1.469(9) . ?
O4 C3 1.465(14) . ?
O5 C5 1.467(13) . ?
O6 C7 1.455(8) . ?
O6 C7' 1.459(10) . ?
C1 C2 1.406(16) . ?
C3 C4 1.44(2) . ?
C5 C6 1.352(19) . ?
C7 C8 1.431(14) . ?
C1' C2' 1.402(17) . ?
C7' C8' 1.429(15) . ?

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 O3 100.4(3) . . ?
O1 V1 O3 100.4(3) . 6_565 ?
O1 V1 O6 99.1(3) . 5_666 ?
O1 V1 O6 99.1(3) . 2_656 ?
O1 V1 O7 179.0(4) . . ?
O3 V1 O3 89.3(3) . 6_565 ?
O3 V1 O7 80.25(13) . . ?
O3 V1 O7 80.26(13) 6_565 . ?
O3 V1 Cl1 93.9(4) . . ?
O3 V1 Cl1 93.9(5) 6_565 . ?
O6 V1 O3 160.48(19) 2_656 6_565 ?
O6 V1 O3 160.48(19) 5_666 . ?
O6 V1 O3 87.75(18) 2_656 . ?
O6 V1 O3 87.75(18) 5_666 6_565 ?
O6 V1 O6 88.6(3) 5_666 2_656 ?
O6 V1 O7 80.23(12) 2_656 . ?
O6 V1 O7 80.23(12) 5_666 . ?
O6 V1 Cl1 105.6(4) 5_666 . ?
O6 V1 Cl1 105.6(4) 2_656 . ?
Cl1 V1 O7 171.7(6) . . ?
O2 V2 O3 100.6(3) . . ?
O2 V2 O4 98.3(3) . . ?
O2 V2 O5 100.9(3) . . ?
O2 V2 O6 98.2(3) . . ?
O2 V2 O7 178.5(3) . . ?
O3 V2 O7 80.42(12) . . ?
O3 V2 Cl2 93.2(4) . . ?
O4 V2 O3 87.84(14) . . ?
O4 V2 O5 160.84(18) . . ?
O4 V2 O7 80.67(12) . . ?
O4 V2 Cl2 104.1(4) . . ?
O5 V2 O3 88.7(2) . . ?
O5 V2 O7 80.17(13) . . ?
O5 V2 Cl2 94.9(4) . . ?
O6 V2 O3 161.14(17) . . ?
O6 V2 O4 88.74(13) . . ?
O6 V2 O5 88.5(2) . . ?
O6 V2 O7 80.73(11) . . ?
O6 V2 Cl2 105.6(4) . . ?
Cl2 V2 O7 172.0(4) . . ?
V2 O3 V1 109.08(18) . . ?
C1 O3 V1 120.7(7) . . ?
C1 O3 V2 124.3(7) . . ?
C1' O3 V1 120.7(8) . . ?
C1' O3 V2 120.8(8) . . ?
V2 O4 V2 108.9(2) . 2_656 ?
C3 O4 V2 121.8(8) . 2_656 ?
C3 O4 V2 122.7(7) . . ?
V2 O5 V2 109.4(3) 6_565 . ?
C5 O5 V2 121.9(2) . . ?
C5 O5 V2 121.9(2) . 6_565 ?
V2 O6 V1 109.29(17) . 5_666 ?
C7 O6 V1 121.9(6) . 5_666 ?
C7 O6 V2 123.7(6) . . ?
C7' O6 V2 121.5(12) . . ?
V1 O7 V1 180.0 5_666 . ?
V2 O7 V1 89.76(4) 5_666 . ?
V2 O7 V1 89.76(4) 2_656 . ?
V2 O7 V1 90.24(4) 6_565 . ?
V2 O7 V1 89.76(4) 6_565 5_666 ?
V2 O7 V1 90.24(3) . . ?
V2 O7 V1 90.24(3) 5_666 5_666 ?
V2 O7 V1 89.76(4) . 5_666 ?
V2 O7 V1 90.24(4) 2_656 5_666 ?
V2 O7 V2 180.0 6_565 2_656 ?
V2 O7 V2 90.23(5) 5_666 2_656 ?
V2 O7 V2 89.77(5) 2_656 . ?
V2 O7 V2 180.0 5_666 . ?
V2 O7 V2 90.23(5) 6_565 . ?
V2 O7 V2 89.77(5) 5_666 6_565 ?
C2 C1 O3 114.8(14) . . ?
C4 C3 O4 109.7(12) . . ?
C6 C5 O5 115.5(13) . . ?
C8 C7 O6 112.1(8) . . ?
C2' C1' O3 108.5(14) . . ?
C8' C7' O6 111.6(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O3 C1 C2 -92(2) . . . . ?
V1 O3 C1' C2' 109(2) . . . . ?
V1 O6 C7 C8 117.4(10) 5_666 . . . ?
V1 O6 C7' C8' -104(2) 5_666 . . . ?
V2 O3 C1 C2 118(2) . . . . ?
V2 O3 C1' C2' -109(2) . . . . ?
V2 O4 C3 C4 99.4(16) 2_656 . . . ?
V2 O4 C3 C4 -112.4(15) . . . . ?
V2 O5 C5 C6 -105.9(5) . . . . ?
V2 O5 C5 C6 105.9(5) 6_565 . . . ?
V2 O6 C7 C8 -90.6(11) . . . . ?
V2 O6 C7' C8' 99(2) . . . . ?

_olex2_submission_original_sample_id matbp32
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.011
_oxdiff_exptl_absorpt_empirical_full_min 0.631
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.641(12)
2 0.359(12)

####################################################################### 
# 
# 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_matbp43
_database_code_depnum_ccdc_archive 'CCDC 1990063'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;

_vrf_PLAT301_matbp43             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 34% 
RESPONSE: The triflato ligand is modeled as disordered over two
positions (0.890(5):0.110(5)). Several ethoxy ligands are modeled
as disordered over two positions each: O10-C7-C8, 0.61(1):0.39(1),
O13-C13-C14, 0.76(3):0.24(3), O15-C17-C18, 0.67(1):0.33(1),
O16-C19-C20, 0.66(1):0.34(1), O17-C21-C22, 0.54(3):0.46(3),
O18-C23-C24, 0.75(1):0.25(1).
;

_vrf_PLAT860_matbp43             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 379 
RESPONSE: For each disordered ligand, analogous bond lengths and
angles were restrained to be similar and anisotropic displacement
parameters for proximal atoms were restrained to be similar. For
the triflato ligand disorder, anisotropic displacement parameters
were restrained toward appropriate relative thermal motion.
;

_audit_creation_date             2019-10-14
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H60 F3 O21 S V6'
_chemical_formula_sum            'C25 H60 F3 O21 S V6'
_chemical_formula_weight         1091.43
_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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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                   10.7375(2)
_cell_length_b                   11.6187(3)
_cell_length_c                   19.2768(4)
_cell_angle_alpha                83.447(2)
_cell_angle_beta                 77.638(2)
_cell_angle_gamma                64.530(2)
_cell_volume                     2120.16(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14744
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5050
_cell_measurement_theta_min      2.3940
_shelx_estimated_absorpt_T_max   0.667
_shelx_estimated_absorpt_T_min   0.205
_exptl_absorpt_coefficient_mu    11.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.037
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35608
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.893
_diffrn_reflns_theta_min         2.347
_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 0.996
_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     -5.00  20.00   0.50    1.11    --  -49.62  19.00  60.00   50
  2  ω     -5.00  24.00   0.50    1.11    --  -49.62  19.00   0.00   58
  3  ω     -3.00  22.00   0.50    1.11    --  -49.62  19.00 -30.00   50
  4  ω     -5.00  22.00   0.50    1.11    --  -49.62  19.00  30.00   54
  5  ω    -31.00  20.00   0.50    1.11    --  -49.62  38.00 -60.00  102
  6  ω    -77.00 -52.00   0.50    1.11    --  -49.62 131.00-106.00   50
  7  ω    -63.00 -37.00   0.50    1.11    --  -49.62 138.00  69.00   52
  8  ω    -21.00   7.00   0.50    1.11    --   49.62 -19.00-120.00   56
  9  ω    -23.00   2.00   0.50    1.11    --   49.62 -19.00 -60.00   50
 10  ω    -22.00  10.00   0.50    1.11    --   49.62 -19.00   0.00   64
 11  ω    -21.00  11.00   0.50    1.11    --   49.62 -19.00  90.00   64
 12  ω    -23.00  11.00   0.50    1.11    --   49.62 -19.00 150.00   68
 13  ω     64.00 102.00   0.50    1.11    --   49.62-138.00   7.00   76
 14  ω     39.00  82.00   0.50    1.11    --   49.62-131.00-176.00   86
 15  ω    -97.00 -71.00   0.50    1.11    --  -49.62-131.00-176.00   52
 16  ω   -100.00 -75.00   0.50    1.11    --  -49.62-125.00-120.00   50
 17  ω    -97.00 -70.00   0.50    1.11    --  -49.62-138.00   7.00   54
 18  ω   -116.00 -78.00   0.50    1.11    --  -49.62-125.00  90.00   76
 19  ω    -40.00 -13.00   0.50    4.44    --  -84.25  45.00-120.00   54
 20  ω    -77.00 -52.00   0.50    4.44    --  -84.25 131.00-106.00   50
 21  ω   -111.00 -86.00   0.50    4.44    --  -84.25-138.00   7.00   50
 22  ω   -137.00-112.00   0.50    4.44    --  -84.25-131.00-176.00   50
 23  ω     36.00  72.00   0.50    4.44    --  105.75 -61.00 120.00   72
 24  ω     93.00 120.00   0.50    4.44    --  105.75 -77.00 120.00   54
 25  ω     82.00 121.00   0.50    4.44    --  105.75-138.00   7.00   78
 26  ω    102.00 127.00   0.50    4.44    --  105.75 -77.00   0.00   50
 27  ω     73.00 105.00   0.50    4.44    --  105.75 -94.00 -30.00   64
 28  ω     81.00 106.00   0.50    4.44    --  105.75-125.00  30.00   50
 29  ω     62.00 106.00   0.50    4.44    --  105.75 -94.00  30.00   88
 30  ω     52.00  97.00   0.50    4.44    --  105.75-125.00  90.00   90
 31  ω     42.00  72.00   0.50    4.44    --  105.75-125.00  30.00   60
 32  ω     35.00  72.00   0.50    4.44    --  105.75 -77.00   0.00   74
 33  ω     36.00  79.00   0.50    4.44    --  105.75 -61.00 -60.00   86
 34  ω     50.00  96.00   0.50    4.44    --  105.75 -77.00-120.00   92
 35  ω     90.00 116.00   0.50    4.44    --  105.75 -77.00-180.00   52
 36  ω     78.00 116.00   0.50    4.44    --  105.75-131.00-176.00   76
 37  ω     86.00 111.00   0.50    4.44    --  105.75-125.00-150.00   50
 38  ω     61.00 108.00   0.50    4.44    --  105.75-107.00-146.36   94
 39  ω     38.00  74.00   0.50    4.44    --  105.75 -61.00-180.00   72
 40  ω     45.00  70.00   0.50    4.44    --  105.75 -61.00-120.00   50
 41  ω     39.00 106.00   0.50    4.44    --  105.75 -94.00-120.00  134
 42  ω     37.00  77.00   0.50    4.44    --  105.75 -61.00   0.00   80
 43  ω     35.00 106.00   0.50    4.44    --  105.75 -94.00 -60.00  142
 44  ω     98.00 132.00   0.50    4.44    --  105.75  15.00  60.00   68
 45  ω    135.00 174.00   0.50    4.44    --  105.75  15.00  60.00   78
 46  ω    131.00 172.00   0.50    4.44    --  105.75  61.00  60.00   82
 47  ω    133.00 159.00   0.50    4.44    --  105.75  30.00   0.00   52
 48  ω    104.00 177.00   0.50    4.44    --  105.75  61.00  90.00  146
 49  ω    123.00 175.00   0.50    4.44    --  105.75  30.00 150.00  104
 50  ω    117.00 142.00   0.50    4.44    --  105.75 138.00  69.00   50
 51  ω     93.00 121.00   0.50    4.44    --  105.75  61.00  60.00   56
 52  ω     99.00 125.00   0.50    4.44    --  105.75  30.00   0.00   52
 53  ω     98.00 170.00   0.50    4.44    --  105.75  45.00 -60.00  144
 54  ω    110.00 135.00   0.50    4.44    --  105.75 131.00-106.00   50
 55  ω    100.00 161.00   0.50    4.44    --  105.75  61.00-120.00  122
 56  ω     98.00 157.00   0.50    4.44    --  105.75  45.00-150.00  118
 57  ω    102.00 168.00   0.50    4.44    --  105.75  15.00-150.00  132
 58  ω     35.00  73.00   0.50    4.44    --  105.75 -94.00-180.00   76
 59  ω     43.00 111.00   0.50    4.44    --  105.75-125.00 120.00  136
 60  ω     35.00 109.00   0.50    4.44    --  105.75-125.00 150.00  148
 61  ω     38.00  74.00   0.50    4.44    --  105.75 -77.00 120.00   72
;
_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      0.0552496000
_diffrn_orient_matrix_UB_12      -0.0845891000
_diffrn_orient_matrix_UB_13      0.0639640000
_diffrn_orient_matrix_UB_21      -0.1123075000
_diffrn_orient_matrix_UB_22      0.1030430000
_diffrn_orient_matrix_UB_23      0.0509996000
_diffrn_orient_matrix_UB_31      -0.1023482000
_diffrn_orient_matrix_UB_32      -0.0617297000
_diffrn_orient_matrix_UB_33      0.0023527000
_diffrn_oxdiff_digest_frames     
;
014878adda3c364841cb3ba0bf1bca630000029f921
;
_diffrn_oxdiff_digest_hkl        
;
017d77738b2d5980851873bbc9b03b7591b65d
;
_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                7347
_reflns_number_total             8882
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.894
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         8882
_refine_ls_number_restraints     371
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0732
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1428P)²+2.5673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2154
_refine_special_details          
;
The triflato ligand is modeled as disordered over two
positions (0.890(5):0.110(5)). Several ethoxy ligands are modeled
as disordered over two positions each: O10-C7-C8, 0.61(1):0.39(1),
O13-C13-C14, 0.76(3):0.24(3), O15-C17-C18, 0.67(1):0.33(1),
O16-C19-C20, 0.66(1):0.34(1), O17-C21-C22, 0.54(3):0.46(3),
O18-C23-C24, 0.75(1):0.25(1).

For each disordered ligand, analogous bond lengths and angles
were restrained to be similar and anisotropic displacement
parameters for proximal atoms were restrained to be similar. For
the triflato ligand disorder, anisotropic displacement parameters
were restrained toward appropriate relative thermal motion
(Thorn et al., 2012).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-S1 \\sim O1-S1'
 with sigma of 0.01
 S1-O20 \\sim S1-O21 \\sim S1'-O20' \\sim S1'-O21'
 with sigma of 0.01
 S1-C25 \\sim S1'-C25'
 with sigma of 0.01
 C25-F1 \\sim C25-F2 \\sim C25-F3 \\sim C25'-F1' \\sim C25'-F2' \\sim C25'-F3'
 with sigma of 0.01
 O10-C7 \\sim O10-C7'
 with sigma of 0.01
 C7-C8 \\sim C7'-C8'
 with sigma of 0.01
 O10-C8 \\sim O10-C8'
 with sigma of 0.02
 O13-C13 \\sim O13-C13'
 with sigma of 0.01
 C13-C14 \\sim C13'-C14'
 with sigma of 0.01
 O13-C14 \\sim O13-C14'
 with sigma of 0.02
 O15-C17 \\sim O15-C17'
 with sigma of 0.01
 C17-C18 \\sim C17'-C18'
 with sigma of 0.01
 O15-C18 \\sim O15-C18'
 with sigma of 0.02
 O16-C19 \\sim O16-C19'
 with sigma of 0.01
 C19-C20 \\sim C19'-C20'
 with sigma of 0.01
 O16-C20 \\sim O16-C20'
 with sigma of 0.02
 O17-C21 \\sim O17-C21'
 with sigma of 0.01
 C21-C22 \\sim C21'-C22'
 with sigma of 0.01
 O17-C22 \\sim O17-C22'
 with sigma of 0.02
 O18-C23 \\sim O18-C23'
 with sigma of 0.01
 C23-C24 \\sim C23'-C24'
 with sigma of 0.01
 O18-C24 \\sim O18-C24'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.4A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S1, O20, O21, C25, F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1', O20', O21', C25', F1', F2', F3'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1')=Sof(O20')=Sof(O21')=Sof(C25')=Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(S1)=Sof(O20)=Sof(O21)=Sof(C25)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Sof(C13')=Sof(H13C)=Sof(H13D)=Sof(C14')=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
 Sof(C17')=Sof(H17C)=Sof(H17D)=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(4)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(4)
 Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(5)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(5)
 Sof(C21')=Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(6)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(6)
 Sof(C23')=Sof(H23C)=Sof(H23D)=Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(7)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(7)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C7'(H7'A,H7'B), C13'(H13C,H13D), C17'(H17C,
 H17D), C19'(H19C,H19D), C21'(H21C,H21D), C23'(H23C,H23D)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C8'(H8'A,H8'B,H8'C), C14'(H14D,H14E,H14F), C18'(H18D,H18E,H18F),
 C20'(H20D,H20E,H20F), C22'(H22D,H22E,H22F), C24'(H24D,H24E,H24F)
;
_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 0.26717(8) 0.38262(6) 0.19298(4) 0.03181(19) Uani 1 1 d . U . . .
V2 V 0.52185(8) 0.28614(7) 0.27274(4) 0.03458(19) Uani 1 1 d . U . . .
V3 V 0.19787(8) 0.37514(6) 0.35892(4) 0.03141(19) Uani 1 1 d . U . . .
V4 V 0.15208(9) 0.18334(7) 0.26671(4) 0.0369(2) Uani 1 1 d . U . . .
V5 V 0.47508(9) 0.09469(7) 0.18093(4) 0.0405(2) Uani 1 1 d . U . . .
V6 V 0.41289(8) 0.07420(7) 0.35368(4) 0.0353(2) Uani 1 1 d . U . . .
O2 O 0.6485(4) 0.3216(3) 0.27460(18) 0.0444(7) Uani 1 1 d . U . . .
O3 O 0.1008(3) 0.4757(3) 0.41903(17) 0.0391(7) Uani 1 1 d . U . . .
O4 O 0.0253(4) 0.1466(3) 0.2645(2) 0.0484(8) Uani 1 1 d . U . . .
O5 O 0.5702(4) -0.0058(3) 0.1212(2) 0.0563(9) Uani 1 1 d . U . . .
O6 O 0.4650(4) -0.0368(3) 0.41259(18) 0.0449(8) Uani 1 1 d . U . . .
O7 O 0.4306(3) 0.4128(3) 0.20078(16) 0.0359(6) Uani 1 1 d . U . . .
O8 O 0.1556(3) 0.4902(3) 0.27563(16) 0.0344(6) Uani 1 1 d . U . . .
O9 O 0.1184(3) 0.3257(3) 0.19659(16) 0.0367(7) Uani 1 1 d . U . . .
O10 O 0.3916(4) 0.2477(3) 0.12373(17) 0.0426(7) Uani 1 1 d D U . . .
O11 O 0.3728(3) 0.3992(3) 0.34742(16) 0.0347(6) Uani 1 1 d . U . . .
O12 O 0.0640(3) 0.3095(3) 0.34302(17) 0.0383(7) Uani 1 1 d . U . . .
O13 O 0.3000(4) 0.0719(3) 0.19256(18) 0.0447(8) Uani 1 1 d D U . . .
O14 O 0.6087(4) 0.1597(3) 0.19618(18) 0.0441(7) Uani 1 1 d . U . . .
O15 O 0.5575(3) 0.1439(3) 0.34272(17) 0.0378(7) Uani 1 1 d D U . . .
O16 O 0.2826(3) 0.2223(3) 0.41579(16) 0.0358(6) Uani 1 1 d D U . . .
O17 O 0.2431(4) 0.0565(3) 0.33811(18) 0.0404(7) Uani 1 1 d D U . . .
O18 O 0.5175(4) -0.0201(3) 0.26347(17) 0.0404(7) Uani 1 1 d D U . . .
O19 O 0.3360(3) 0.2369(2) 0.26905(14) 0.0334(7) Uani 1 1 d . U . . .
C1 C 0.5131(5) 0.4545(4) 0.1425(3) 0.0412(10) Uani 1 1 d . U . . .
H1A H 0.470620 0.472158 0.100588 0.049 Uiso 1 1 calc R . . . .
H1B H 0.606994 0.387252 0.131424 0.049 Uiso 1 1 calc R . . . .
C2 C 0.5210(6) 0.5723(5) 0.1618(3) 0.0544(13) Uani 1 1 d . U . . .
H2A H 0.427854 0.637173 0.175251 0.082 Uiso 1 1 calc GR . . . .
H2B H 0.570290 0.602260 0.121619 0.082 Uiso 1 1 calc GR . . . .
H2C H 0.570022 0.552811 0.200771 0.082 Uiso 1 1 calc GR . . . .
C3 C 0.0354(5) 0.6108(4) 0.2747(3) 0.0406(10) Uani 1 1 d . U . . .
H3A H -0.029621 0.620629 0.319505 0.049 Uiso 1 1 calc R . . . .
H3B H -0.012367 0.612085 0.237077 0.049 Uiso 1 1 calc R . . . .
C4 C 0.0777(7) 0.7201(5) 0.2633(4) 0.0668(17) Uani 1 1 d . U . . .
H4A H 0.109301 0.728492 0.304613 0.100 Uiso 1 1 calc GR . . . .
H4B H -0.001397 0.797408 0.255102 0.100 Uiso 1 1 calc GR . . . .
H4C H 0.152181 0.704258 0.222797 0.100 Uiso 1 1 calc GR . . . .
C5 C 0.0451(6) 0.3377(5) 0.1403(3) 0.0457(11) Uani 1 1 d . U . . .
H5A H 0.063187 0.253440 0.126365 0.055 Uiso 1 1 calc R . . . .
H5B H 0.079727 0.379663 0.099354 0.055 Uiso 1 1 calc R . . . .
C6 C -0.1088(6) 0.4123(6) 0.1626(3) 0.0593(15) Uani 1 1 d . U . . .
H6A H -0.144606 0.367102 0.200378 0.089 Uiso 1 1 calc GR . . . .
H6B H -0.154462 0.423976 0.122956 0.089 Uiso 1 1 calc GR . . . .
H6C H -0.126505 0.494021 0.178756 0.089 Uiso 1 1 calc GR . . . .
C7 C 0.4474(10) 0.2605(8) 0.0488(3) 0.044(2) Uani 0.609(11) 1 d D U P A 1
H7A H 0.549199 0.220078 0.040676 0.052 Uiso 0.609(11) 1 calc R . P A 1
H7B H 0.418126 0.350056 0.035355 0.052 Uiso 0.609(11) 1 calc R . P A 1
C8 C 0.3947(13) 0.1989(10) 0.0047(5) 0.059(3) Uani 0.609(11) 1 d D U P A 1
H8A H 0.420724 0.111170 0.019478 0.089 Uiso 0.609(11) 1 calc GR . P A 1
H8B H 0.435222 0.203662 -0.044460 0.089 Uiso 0.609(11) 1 calc GR . P A 1
H8C H 0.294313 0.242523 0.010724 0.089 Uiso 0.609(11) 1 calc GR . P A 1
C9 C 0.3640(5) 0.5240(4) 0.3583(3) 0.0415(10) Uani 1 1 d . U . . .
H9A H 0.270952 0.576161 0.383588 0.050 Uiso 1 1 calc R . . . .
H9B H 0.378974 0.565355 0.312664 0.050 Uiso 1 1 calc R . . . .
C10 C 0.4722(6) 0.5132(5) 0.4003(3) 0.0504(12) Uani 1 1 d . U . . .
H10A H 0.461586 0.466862 0.444049 0.076 Uiso 1 1 calc GR . . . .
H10B H 0.459332 0.597012 0.410496 0.076 Uiso 1 1 calc GR . . . .
H10C H 0.564464 0.468972 0.373158 0.076 Uiso 1 1 calc GR . . . .
C11 C -0.0863(5) 0.3778(6) 0.3608(3) 0.0521(12) Uani 1 1 d . U . . .
H11A H -0.129755 0.344261 0.333987 0.062 Uiso 1 1 calc R . . . .
H11B H -0.112682 0.467012 0.347252 0.062 Uiso 1 1 calc R . . . .
C12 C -0.1394(7) 0.3667(9) 0.4381(4) 0.079(2) Uani 1 1 d . U . . .
H12A H -0.106546 0.278328 0.452531 0.118 Uiso 1 1 calc GR . . . .
H12B H -0.240187 0.405485 0.447189 0.118 Uiso 1 1 calc GR . . . .
H12C H -0.105828 0.409247 0.464473 0.118 Uiso 1 1 calc GR . . . .
C13 C 0.287(11) -0.038(4) 0.172(3) 0.067(6) Uani 0.24(3) 1 d D U P B 1
H13A H 0.212616 -0.051926 0.205537 0.081 Uiso 0.24(3) 1 calc R . P B 1
H13B H 0.373820 -0.113598 0.173763 0.081 Uiso 0.24(3) 1 calc R . P B 1
C14 C 0.255(6) -0.020(4) 0.099(2) 0.083(8) Uani 0.24(3) 1 d D U P B 1
H14A H 0.162496 0.046373 0.099302 0.124 Uiso 0.24(3) 1 calc GR . P B 1
H14B H 0.258755 -0.098135 0.084667 0.124 Uiso 0.24(3) 1 calc GR . P B 1
H14C H 0.322393 0.002835 0.067074 0.124 Uiso 0.24(3) 1 calc GR . P B 1
C15 C 0.7598(6) 0.0884(6) 0.1785(3) 0.0578(14) Uani 1 1 d . U . . .
H15A H 0.784228 -0.000437 0.192444 0.069 Uiso 1 1 calc R . . . .
H15B H 0.804551 0.120942 0.205080 0.069 Uiso 1 1 calc R . . . .
C16 C 0.8138(8) 0.0980(7) 0.1006(4) 0.084(2) Uani 1 1 d . U . . .
H16A H 0.779394 0.055692 0.074522 0.126 Uiso 1 1 calc GR . . . .
H16B H 0.914531 0.058218 0.091580 0.126 Uiso 1 1 calc GR . . . .
H16C H 0.782022 0.186118 0.085704 0.126 Uiso 1 1 calc GR . . . .
C17 C 0.6245(8) 0.1384(7) 0.4021(4) 0.0413(17) Uani 0.666(11) 1 d D U P C 1
H17A H 0.591121 0.094132 0.442264 0.050 Uiso 0.666(11) 1 calc R . P C 1
H17B H 0.598741 0.224387 0.416337 0.050 Uiso 0.666(11) 1 calc R . P C 1
C18 C 0.7799(8) 0.0715(9) 0.3828(5) 0.055(2) Uani 0.666(11) 1 d D U P C 1
H18A H 0.805501 -0.013038 0.367878 0.082 Uiso 0.666(11) 1 calc GR . P C 1
H18B H 0.820903 0.066722 0.423228 0.082 Uiso 0.666(11) 1 calc GR . P C 1
H18C H 0.813574 0.117725 0.344654 0.082 Uiso 0.666(11) 1 calc GR . P C 1
C19 C 0.3123(8) 0.2281(7) 0.4831(4) 0.0445(19) Uani 0.657(11) 1 d D U P D 1
H19A H 0.338990 0.298055 0.482813 0.053 Uiso 0.657(11) 1 calc R . P D 1
H19B H 0.390714 0.149639 0.492648 0.053 Uiso 0.657(11) 1 calc R . P D 1
C20 C 0.1862(10) 0.2470(9) 0.5411(4) 0.063(3) Uani 0.657(11) 1 d D U P D 1
H20A H 0.108736 0.324779 0.531724 0.095 Uiso 0.657(11) 1 calc GR . P D 1
H20B H 0.208382 0.251714 0.586046 0.095 Uiso 0.657(11) 1 calc GR . P D 1
H20C H 0.161443 0.176581 0.542251 0.095 Uiso 0.657(11) 1 calc GR . P D 1
C21 C 0.169(3) 0.020(2) 0.4023(9) 0.040(4) Uani 0.46(3) 1 d D U P E 1
H21A H 0.080141 0.090960 0.417990 0.047 Uiso 0.46(3) 1 calc R . P E 1
H21B H 0.224225 -0.002166 0.439600 0.047 Uiso 0.46(3) 1 calc R . P E 1
C22 C 0.144(3) -0.0939(17) 0.3878(10) 0.064(5) Uani 0.46(3) 1 d D U P E 1
H22A H 0.065297 -0.065006 0.364279 0.096 Uiso 0.46(3) 1 calc GR . P E 1
H22B H 0.125656 -0.136259 0.431883 0.096 Uiso 0.46(3) 1 calc GR . P E 1
H22C H 0.226145 -0.152222 0.357992 0.096 Uiso 0.46(3) 1 calc GR . P E 1
C23 C 0.6417(7) -0.1398(6) 0.2643(4) 0.0439(16) Uani 0.747(11) 1 d D U P F 1
H23A H 0.700077 -0.132739 0.294137 0.053 Uiso 0.747(11) 1 calc R . P F 1
H23B H 0.696054 -0.158543 0.216531 0.053 Uiso 0.747(11) 1 calc R . P F 1
C24 C 0.5971(11) -0.2467(7) 0.2927(5) 0.059(2) Uani 0.747(11) 1 d D U P F 1
H24A H 0.554100 -0.233395 0.341883 0.088 Uiso 0.747(11) 1 calc GR . P F 1
H24B H 0.678019 -0.327027 0.287893 0.088 Uiso 0.747(11) 1 calc GR . P F 1
H24C H 0.531180 -0.247224 0.266174 0.088 Uiso 0.747(11) 1 calc GR . P F 1
O1 O 0.1873(4) 0.5268(3) 0.12150(17) 0.0418(7) Uani 1 1 d D U . . .
S1 S 0.18725(19) 0.60882(17) 0.05836(9) 0.0413(4) Uani 0.890(5) 1 d D U P G 1
O20 O 0.2399(7) 0.6979(5) 0.0650(4) 0.0804(18) Uani 0.890(5) 1 d D U P G 1
O21 O 0.2364(6) 0.5436(5) -0.0057(2) 0.0770(17) Uani 0.890(5) 1 d D U P G 1
C25 C 0.0001(7) 0.7010(6) 0.0593(3) 0.0533(13) Uani 0.890(5) 1 d D U P G 1
F1 F -0.0219(8) 0.7869(5) 0.0067(3) 0.0532(13) Uani 0.890(5) 1 d D U P G 1
F2 F -0.0570(6) 0.6235(5) 0.0496(4) 0.0827(16) Uani 0.890(5) 1 d D U P G 1
F3 F -0.0656(6) 0.7600(5) 0.1192(2) 0.107(2) Uani 0.890(5) 1 d D U P G 1
S1' S 0.1797(17) 0.6448(13) 0.0813(9) 0.051(3) Uani 0.110(5) 1 d D U P G 2
O20' O 0.158(6) 0.743(3) 0.125(2) 0.082(7) Uani 0.110(5) 1 d D U P G 2
O21' O 0.270(3) 0.639(4) 0.0162(15) 0.073(8) Uani 0.110(5) 1 d D U P G 2
C25' C 0.009(2) 0.710(3) 0.0543(19) 0.057(4) Uani 0.110(5) 1 d D U P G 2
F1' F -0.015(8) 0.815(4) 0.015(3) 0.060(7) Uani 0.110(5) 1 d D U P G 2
F2' F -0.004(4) 0.624(4) 0.0205(18) 0.060(4) Uani 0.110(5) 1 d D U P G 2
F3' F -0.084(3) 0.676(3) 0.0970(18) 0.056(4) Uani 0.110(5) 1 d D U P G 2
C7' C 0.3651(14) 0.2360(13) 0.0541(5) 0.049(3) Uani 0.391(11) 1 d D U P A 2
H7'A H 0.291421 0.315194 0.041157 0.059 Uiso 0.391(11) 1 calc R . P A 2
H7'B H 0.333812 0.168665 0.056244 0.059 Uiso 0.391(11) 1 calc R . P A 2
C8' C 0.4958(17) 0.2065(17) -0.0008(7) 0.066(4) Uani 0.391(11) 1 d D U P A 2
H8'A H 0.533631 0.266958 0.001559 0.100 Uiso 0.391(11) 1 calc GR . P A 2
H8'B H 0.474009 0.211397 -0.047109 0.100 Uiso 0.391(11) 1 calc GR . P A 2
H8'C H 0.563677 0.122017 0.007942 0.100 Uiso 0.391(11) 1 calc GR . P A 2
C13' C 0.305(3) -0.0513(11) 0.1800(10) 0.061(3) Uani 0.76(3) 1 d D U P B 2
H13C H 0.280663 -0.090461 0.224854 0.073 Uiso 0.76(3) 1 calc R . P B 2
H13D H 0.400019 -0.107001 0.158202 0.073 Uiso 0.76(3) 1 calc R . P B 2
C14' C 0.2061(18) -0.0345(11) 0.1326(9) 0.083(4) Uani 0.76(3) 1 d D U P B 2
H14D H 0.111566 0.011452 0.156826 0.125 Uiso 0.76(3) 1 calc GR . P B 2
H14E H 0.217937 -0.116606 0.119875 0.125 Uiso 0.76(3) 1 calc GR . P B 2
H14F H 0.224636 0.012454 0.090382 0.125 Uiso 0.76(3) 1 calc GR . P B 2
C17' C 0.6958(12) 0.0760(14) 0.3576(8) 0.052(4) Uani 0.334(11) 1 d D U P C 2
H17C H 0.763728 0.082668 0.317065 0.062 Uiso 0.334(11) 1 calc R . P C 2
H17D H 0.715528 -0.013544 0.366553 0.062 Uiso 0.334(11) 1 calc R . P C 2
C18' C 0.7077(19) 0.130(2) 0.4210(9) 0.066(5) Uani 0.334(11) 1 d D U P C 2
H18D H 0.679145 0.220179 0.413805 0.099 Uiso 0.334(11) 1 calc GR . P C 2
H18E H 0.803343 0.090431 0.427914 0.099 Uiso 0.334(11) 1 calc GR . P C 2
H18F H 0.648434 0.113948 0.462186 0.099 Uiso 0.334(11) 1 calc GR . P C 2
C19' C 0.2394(17) 0.2170(12) 0.4909(5) 0.039(3) Uani 0.343(11) 1 d D U P D 2
H19C H 0.283267 0.129112 0.507327 0.047 Uiso 0.343(11) 1 calc R . P D 2
H19D H 0.138718 0.243008 0.501424 0.047 Uiso 0.343(11) 1 calc R . P D 2
C20' C 0.2740(17) 0.2987(13) 0.5324(7) 0.045(3) Uani 0.343(11) 1 d D U P D 2
H20D H 0.367104 0.291656 0.512976 0.068 Uiso 0.343(11) 1 calc GR . P D 2
H20E H 0.269064 0.270303 0.581222 0.068 Uiso 0.343(11) 1 calc GR . P D 2
H20F H 0.207971 0.386000 0.529225 0.068 Uiso 0.343(11) 1 calc GR . P D 2
C21' C 0.147(2) 0.0242(15) 0.3927(10) 0.042(4) Uani 0.54(3) 1 d D U P E 2
H21C H 0.057508 0.052086 0.377923 0.050 Uiso 0.54(3) 1 calc R . P E 2
H21D H 0.131675 0.066782 0.436292 0.050 Uiso 0.54(3) 1 calc R . P E 2
C22' C 0.210(2) -0.1200(12) 0.4055(8) 0.060(4) Uani 0.54(3) 1 d D U P E 2
H22D H 0.234457 -0.161632 0.361167 0.090 Uiso 0.54(3) 1 calc GR . P E 2
H22E H 0.143018 -0.143611 0.437695 0.090 Uiso 0.54(3) 1 calc GR . P E 2
H22F H 0.293022 -0.145580 0.425535 0.090 Uiso 0.54(3) 1 calc GR . P E 2
C23' C 0.533(2) -0.1505(10) 0.2576(12) 0.049(4) Uani 0.253(11) 1 d D U P F 2
H23C H 0.541593 -0.168156 0.208369 0.059 Uiso 0.253(11) 1 calc R . P F 2
H23D H 0.451590 -0.161048 0.285146 0.059 Uiso 0.253(11) 1 calc R . P F 2
C24' C 0.665(2) -0.2411(17) 0.2857(16) 0.059(6) Uani 0.253(11) 1 d D U P F 2
H24D H 0.746240 -0.246232 0.251485 0.089 Uiso 0.253(11) 1 calc GR . P F 2
H24E H 0.664987 -0.324305 0.293856 0.089 Uiso 0.253(11) 1 calc GR . P F 2
H24F H 0.665977 -0.210034 0.329474 0.089 Uiso 0.253(11) 1 calc GR . P F 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 O7 1.969(3) . ?
V1 O8 1.971(3) . ?
V1 O9 1.961(3) . ?
V1 O10 1.984(3) . ?
V1 O19 2.094(3) . ?
V1 O1 2.045(3) . ?
V2 O2 1.590(3) . ?
V2 O7 1.981(3) . ?
V2 O11 1.999(3) . ?
V2 O14 1.983(3) . ?
V2 O15 1.966(3) . ?
V2 O19 2.317(3) . ?
V3 O3 1.594(3) . ?
V3 O8 1.967(3) . ?
V3 O11 1.978(3) . ?
V3 O12 1.982(3) . ?
V3 O16 1.943(3) . ?
V3 O19 2.295(3) . ?
V4 O4 1.602(3) . ?
V4 O9 1.969(3) . ?
V4 O12 1.977(3) . ?
V4 O13 1.981(4) . ?
V4 O17 1.974(3) . ?
V4 O19 2.322(3) . ?
V5 O5 1.584(4) . ?
V5 O10 1.945(3) . ?
V5 O13 1.972(4) . ?
V5 O14 1.970(4) . ?
V5 O18 1.955(3) . ?
V5 O19 2.297(3) . ?
V6 O6 1.607(3) . ?
V6 O15 2.004(3) . ?
V6 O16 2.009(3) . ?
V6 O17 2.007(3) . ?
V6 O18 2.007(3) . ?
V6 O19 2.334(3) . ?
O7 C1 1.450(5) . ?
O8 C3 1.442(5) . ?
O9 C5 1.434(5) . ?
O10 C7 1.457(7) . ?
O10 C7' 1.462(9) . ?
O11 C9 1.448(5) . ?
O12 C11 1.441(6) . ?
O13 C13 1.453(10) . ?
O13 C13' 1.452(6) . ?
O14 C15 1.451(6) . ?
O15 C17 1.460(7) . ?
O15 C17' 1.426(10) . ?
O16 C19 1.417(7) . ?
O16 C19' 1.425(9) . ?
O17 C21 1.445(9) . ?
O17 C21' 1.445(9) . ?
O18 C23 1.457(6) . ?
O18 C23' 1.466(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.499(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.502(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.488(9) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.501(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.509(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.490(9) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.485(18) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.501(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.487(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.511(11) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.525(14) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.522(10) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O1 S1 1.458(3) . ?
O1 S1' 1.475(9) . ?
S1 O20 1.404(5) . ?
S1 O21 1.404(5) . ?
S1 C25 1.823(6) . ?
C25 F1 1.322(5) . ?
C25 F2 1.336(6) . ?
C25 F3 1.311(6) . ?
S1' O20' 1.402(9) . ?
S1' O21' 1.401(9) . ?
S1' C25' 1.821(11) . ?
C25' F1' 1.321(9) . ?
C25' F2' 1.324(9) . ?
C25' F3' 1.320(9) . ?
F2' F3' 1.58(5) . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C7' C8' 1.497(12) . ?
C8' H8'A 0.9600 . ?
C8' H8'B 0.9600 . ?
C8' H8'C 0.9600 . ?
C13' H13C 0.9700 . ?
C13' H13D 0.9700 . ?
C13' C14' 1.487(16) . ?
C14' H14D 0.9600 . ?
C14' H14E 0.9600 . ?
C14' H14F 0.9600 . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C17' C18' 1.487(13) . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20' 1.511(12) . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
C21' C22' 1.526(14) . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C23' C24' 1.523(13) . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?

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
O7 V1 O8 90.24(13) . . ?
O7 V1 O10 88.91(14) . . ?
O7 V1 O19 84.96(12) . . ?
O7 V1 O1 98.03(13) . . ?
O8 V1 O10 168.92(13) . . ?
O8 V1 O19 84.69(12) . . ?
O8 V1 O1 93.26(13) . . ?
O9 V1 O7 169.60(13) . . ?
O9 V1 O8 89.89(13) . . ?
O9 V1 O10 88.96(14) . . ?
O9 V1 O19 84.69(12) . . ?
O9 V1 O1 92.34(13) . . ?
O10 V1 O19 84.23(13) . . ?
O10 V1 O1 97.79(14) . . ?
O1 V1 O19 176.40(13) . . ?
O2 V2 O7 100.25(15) . . ?
O2 V2 O11 101.23(16) . . ?
O2 V2 O14 100.63(17) . . ?
O2 V2 O15 100.27(16) . . ?
O2 V2 O19 179.23(15) . . ?
O7 V2 O11 87.89(13) . . ?
O7 V2 O14 87.10(14) . . ?
O7 V2 O19 78.98(11) . . ?
O11 V2 O19 78.66(11) . . ?
O14 V2 O11 158.11(14) . . ?
O14 V2 O19 79.46(13) . . ?
O15 V2 O7 159.47(14) . . ?
O15 V2 O11 88.57(13) . . ?
O15 V2 O14 88.70(14) . . ?
O15 V2 O19 80.49(12) . . ?
O3 V3 O8 98.14(14) . . ?
O3 V3 O11 99.97(15) . . ?
O3 V3 O12 100.20(16) . . ?
O3 V3 O16 101.32(15) . . ?
O3 V3 O19 177.70(13) . . ?
O8 V3 O11 87.14(13) . . ?
O8 V3 O12 89.07(13) . . ?
O8 V3 O19 79.59(11) . . ?
O11 V3 O12 159.81(14) . . ?
O11 V3 O19 79.61(12) . . ?
O12 V3 O19 80.20(12) . . ?
O16 V3 O8 160.49(13) . . ?
O16 V3 O11 88.20(13) . . ?
O16 V3 O12 88.80(13) . . ?
O16 V3 O19 80.94(11) . . ?
O4 V4 O9 101.01(16) . . ?
O4 V4 O12 100.64(18) . . ?
O4 V4 O13 100.95(18) . . ?
O4 V4 O17 99.96(16) . . ?
O4 V4 O19 179.58(16) . . ?
O9 V4 O12 88.70(13) . . ?
O9 V4 O13 88.13(14) . . ?
O9 V4 O17 159.03(14) . . ?
O9 V4 O19 78.67(11) . . ?
O12 V4 O13 158.39(14) . . ?
O12 V4 O19 79.63(12) . . ?
O13 V4 O19 78.79(12) . . ?
O17 V4 O12 87.53(14) . . ?
O17 V4 O13 87.83(15) . . ?
O17 V4 O19 80.37(12) . . ?
O5 V5 O10 101.17(18) . . ?
O5 V5 O13 99.63(19) . . ?
O5 V5 O14 100.6(2) . . ?
O5 V5 O18 97.90(18) . . ?
O5 V5 O19 178.70(17) . . ?
O10 V5 O13 88.34(15) . . ?
O10 V5 O14 88.37(15) . . ?
O10 V5 O18 160.90(14) . . ?
O10 V5 O19 79.86(12) . . ?
O13 V5 O19 79.56(12) . . ?
O14 V5 O13 159.78(14) . . ?
O14 V5 O19 80.22(12) . . ?
O18 V5 O13 87.33(15) . . ?
O18 V5 O14 89.29(15) . . ?
O18 V5 O19 81.06(11) . . ?
O6 V6 O15 100.64(16) . . ?
O6 V6 O16 100.75(16) . . ?
O6 V6 O17 100.63(16) . . ?
O6 V6 O18 101.47(16) . . ?
O6 V6 O19 179.42(16) . . ?
O15 V6 O16 87.70(13) . . ?
O15 V6 O17 158.73(13) . . ?
O15 V6 O18 88.30(14) . . ?
O15 V6 O19 79.32(12) . . ?
O16 V6 O19 78.67(11) . . ?
O17 V6 O16 87.91(14) . . ?
O17 V6 O19 79.41(11) . . ?
O18 V6 O16 157.78(13) . . ?
O18 V6 O17 87.94(15) . . ?
O18 V6 O19 79.11(11) . . ?
V1 O7 V2 105.36(13) . . ?
C1 O7 V1 124.7(3) . . ?
C1 O7 V2 120.7(3) . . ?
V3 O8 V1 105.03(13) . . ?
C3 O8 V1 126.0(3) . . ?
C3 O8 V3 125.7(3) . . ?
V1 O9 V4 106.10(15) . . ?
C5 O9 V1 126.2(3) . . ?
C5 O9 V4 121.8(3) . . ?
V5 O10 V1 105.32(15) . . ?
C7 O10 V1 129.2(4) . . ?
C7 O10 V5 123.0(4) . . ?
C7' O10 V1 125.7(6) . . ?
C7' O10 V5 119.4(6) . . ?
V3 O11 V2 111.06(14) . . ?
C9 O11 V2 120.6(3) . . ?
C9 O11 V3 119.3(3) . . ?
V4 O12 V3 110.54(15) . . ?
C11 O12 V3 123.9(3) . . ?
C11 O12 V4 121.0(3) . . ?
V5 O13 V4 111.56(15) . . ?
C13 O13 V4 119(4) . . ?
C13 O13 V5 126(4) . . ?
C13' O13 V4 120.3(12) . . ?
C13' O13 V5 120.1(12) . . ?
V5 O14 V2 110.69(16) . . ?
C15 O14 V2 121.2(3) . . ?
C15 O14 V5 123.0(3) . . ?
V2 O15 V6 110.86(15) . . ?
C17 O15 V2 121.1(3) . . ?
C17 O15 V6 120.6(3) . . ?
C17' O15 V2 118.9(7) . . ?
C17' O15 V6 125.7(7) . . ?
V3 O16 V6 110.97(14) . . ?
C19 O16 V3 121.8(4) . . ?
C19 O16 V6 118.9(4) . . ?
C19' O16 V3 122.2(6) . . ?
C19' O16 V6 126.3(6) . . ?
V4 O17 V6 110.77(14) . . ?
C21 O17 V4 124.8(13) . . ?
C21 O17 V6 112.7(12) . . ?
C21' O17 V4 114.2(10) . . ?
C21' O17 V6 125.1(11) . . ?
V5 O18 V6 110.50(14) . . ?
C23 O18 V5 125.4(3) . . ?
C23 O18 V6 120.3(3) . . ?
C23' O18 V5 117.2(8) . . ?
C23' O18 V6 119.8(9) . . ?
V1 O19 V2 90.69(10) . . ?
V1 O19 V3 90.68(10) . . ?
V1 O19 V4 90.54(11) . . ?
V1 O19 V5 90.59(10) . . ?
V1 O19 V6 179.9(2) . . ?
V2 O19 V4 178.75(14) . . ?
V2 O19 V6 89.33(10) . . ?
V3 O19 V2 90.64(10) . . ?
V3 O19 V4 89.63(10) . . ?
V3 O19 V5 178.70(13) . . ?
V3 O19 V6 89.41(10) . . ?
V4 O19 V6 89.45(9) . . ?
V5 O19 V2 89.61(10) . . ?
V5 O19 V4 90.10(10) . . ?
V5 O19 V6 89.32(10) . . ?
O7 C1 H1A 109.6 . . ?
O7 C1 H1B 109.6 . . ?
O7 C1 C2 110.3(4) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 H3A 109.4 . . ?
O8 C3 H3B 109.4 . . ?
O8 C3 C4 111.3(4) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O9 C5 H5A 109.4 . . ?
O9 C5 H5B 109.4 . . ?
O9 C5 C6 111.2(4) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O10 C7 H7A 109.8 . . ?
O10 C7 H7B 109.8 . . ?
O10 C7 C8 109.5(6) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O11 C9 H9A 109.5 . . ?
O11 C9 H9B 109.5 . . ?
O11 C9 C10 110.8(4) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
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 . . ?
O12 C11 H11A 109.3 . . ?
O12 C11 H11B 109.3 . . ?
O12 C11 C12 111.8(5) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 C13 H13A 109.4 . . ?
O13 C13 H13B 109.4 . . ?
O13 C13 C14 111.0(15) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
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 . . ?
O14 C15 H15A 109.3 . . ?
O14 C15 H15B 109.3 . . ?
O14 C15 C16 111.7(5) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O15 C17 H17A 109.4 . . ?
O15 C17 H17B 109.4 . . ?
O15 C17 C18 111.3(6) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
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 . . ?
O16 C19 H19A 109.5 . . ?
O16 C19 H19B 109.5 . . ?
O16 C19 C20 110.9(6) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O17 C21 H21A 109.8 . . ?
O17 C21 H21B 109.8 . . ?
O17 C21 C22 109.4(11) . . ?
H21A C21 H21B 108.2 . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
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 . . ?
O18 C23 H23A 109.8 . . ?
O18 C23 H23B 109.8 . . ?
O18 C23 C24 109.4(6) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
S1 O1 V1 157.9(2) . . ?
S1' O1 V1 152.4(8) . . ?
O1 S1 C25 102.0(2) . . ?
O20 S1 O1 112.5(3) . . ?
O20 S1 C25 105.8(3) . . ?
O21 S1 O1 114.0(3) . . ?
O21 S1 O20 116.7(4) . . ?
O21 S1 C25 103.9(3) . . ?
F1 C25 S1 111.1(5) . . ?
F1 C25 F2 106.8(5) . . ?
F2 C25 S1 109.5(4) . . ?
F3 C25 S1 112.0(4) . . ?
F3 C25 F1 108.4(6) . . ?
F3 C25 F2 108.9(6) . . ?
O1 S1' C25' 104.0(14) . . ?
O20' S1' O1 113(2) . . ?
O20' S1' C25' 100(3) . . ?
O21' S1' O1 120(2) . . ?
O21' S1' O20' 114(3) . . ?
O21' S1' C25' 102(2) . . ?
F1' C25' S1' 113(4) . . ?
F1' C25' F2' 110(4) . . ?
F2' C25' S1' 111(3) . . ?
F3' C25' S1' 114(2) . . ?
F3' C25' F1' 128(4) . . ?
F3' C25' F2' 73(3) . . ?
C25' F2' F3' 53.2(13) . . ?
C25' F3' F2' 53.5(13) . . ?
O10 C7' H7'A 109.6 . . ?
O10 C7' H7'B 109.6 . . ?
O10 C7' C8' 110.3(10) . . ?
H7'A C7' H7'B 108.1 . . ?
C8' C7' H7'A 109.6 . . ?
C8' C7' H7'B 109.6 . . ?
C7' C8' H8'A 109.5 . . ?
C7' C8' H8'B 109.5 . . ?
C7' C8' H8'C 109.5 . . ?
H8'A C8' H8'B 109.5 . . ?
H8'A C8' H8'C 109.5 . . ?
H8'B C8' H8'C 109.5 . . ?
O13 C13' H13C 109.7 . . ?
O13 C13' H13D 109.7 . . ?
O13 C13' C14' 109.7(9) . . ?
H13C C13' H13D 108.2 . . ?
C14' C13' H13C 109.7 . . ?
C14' C13' H13D 109.7 . . ?
C13' C14' H14D 109.5 . . ?
C13' C14' H14E 109.5 . . ?
C13' C14' H14F 109.5 . . ?
H14D C14' H14E 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
O15 C17' H17C 109.8 . . ?
O15 C17' H17D 109.8 . . ?
O15 C17' C18' 109.6(10) . . ?
H17C C17' H17D 108.2 . . ?
C18' C17' H17C 109.8 . . ?
C18' C17' H17D 109.8 . . ?
C17' C18' H18D 109.5 . . ?
C17' C18' H18E 109.5 . . ?
C17' C18' H18F 109.5 . . ?
H18D C18' H18E 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
O16 C19' H19C 108.5 . . ?
O16 C19' H19D 108.5 . . ?
O16 C19' C20' 115.1(9) . . ?
H19C C19' H19D 107.5 . . ?
C20' C19' H19C 108.5 . . ?
C20' C19' H19D 108.5 . . ?
C19' C20' H20D 109.5 . . ?
C19' C20' H20E 109.5 . . ?
C19' C20' H20F 109.5 . . ?
H20D C20' H20E 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
O17 C21' H21C 109.9 . . ?
O17 C21' H21D 109.9 . . ?
O17 C21' C22' 108.7(10) . . ?
H21C C21' H21D 108.3 . . ?
C22' C21' H21C 109.9 . . ?
C22' C21' H21D 109.9 . . ?
C21' C22' H22D 109.5 . . ?
C21' C22' H22E 109.5 . . ?
C21' C22' H22F 109.5 . . ?
H22D C22' H22E 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
O18 C23' H23C 110.2 . . ?
O18 C23' H23D 110.2 . . ?
O18 C23' C24' 107.7(11) . . ?
H23C C23' H23D 108.5 . . ?
C24' C23' H23C 110.2 . . ?
C24' C23' H23D 110.2 . . ?
C23' C24' H24D 109.5 . . ?
C23' C24' H24E 109.5 . . ?
C23' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 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
V1 O7 C1 C2 125.7(4) . . . . ?
V1 O8 C3 C4 -91.5(5) . . . . ?
V1 O9 C5 C6 -121.5(4) . . . . ?
V1 O10 C7 C8 -118.0(7) . . . . ?
V1 O10 C7' C8' 135.8(10) . . . . ?
V1 O1 S1 O20 -75.4(7) . . . . ?
V1 O1 S1 O21 60.4(7) . . . . ?
V1 O1 S1 C25 171.7(6) . . . . ?
V1 O1 S1' O20' -53(3) . . . . ?
V1 O1 S1' O21' 87(3) . . . . ?
V1 O1 S1' C25' -160.1(16) . . . . ?
V2 O7 C1 C2 -92.5(4) . . . . ?
V2 O11 C9 C10 -78.6(5) . . . . ?
V2 O14 C15 C16 -128.0(5) . . . . ?
V2 O15 C17 C18 -89.0(6) . . . . ?
V2 O15 C17' C18' 94.9(13) . . . . ?
V3 O8 C3 C4 111.8(4) . . . . ?
V3 O11 C9 C10 137.3(4) . . . . ?
V3 O12 C11 C12 -79.1(6) . . . . ?
V3 O16 C19 C20 86.8(7) . . . . ?
V3 O16 C19' C20' -67.8(14) . . . . ?
V4 O9 C5 C6 89.4(4) . . . . ?
V4 O12 C11 C12 127.3(5) . . . . ?
V4 O13 C13 C14 110(6) . . . . ?
V4 O13 C13' C14' 82.9(17) . . . . ?
V4 O17 C21 C22 91(2) . . . . ?
V4 O17 C21' C22' 136.5(16) . . . . ?
V5 O10 C7 C8 82.5(8) . . . . ?
V5 O10 C7' C8' -83.0(12) . . . . ?
V5 O13 C13 C14 -93(7) . . . . ?
V5 O13 C13' C14' -131.0(17) . . . . ?
V5 O14 C15 C16 79.6(6) . . . . ?
V5 O18 C23 C24 -126.2(5) . . . . ?
V5 O18 C23' C24' 133.6(16) . . . . ?
V6 O15 C17 C18 124.0(5) . . . . ?
V6 O15 C17' C18' -111.3(12) . . . . ?
V6 O16 C19 C20 -127.8(6) . . . . ?
V6 O16 C19' C20' 121.4(10) . . . . ?
V6 O17 C21 C22 -130(2) . . . . ?
V6 O17 C21' C22' -81(2) . . . . ?
V6 O18 C23 C24 77.7(6) . . . . ?
V6 O18 C23' C24' -87.9(19) . . . . ?
O1 S1 C25 F1 177.0(4) . . . . ?
O1 S1 C25 F2 -65.2(5) . . . . ?
O1 S1 C25 F3 55.6(5) . . . . ?
O1 S1' C25' F1' -178(4) . . . . ?
O1 S1' C25' F2' -54(3) . . . . ?
O1 S1' C25' F3' 27(4) . . . . ?
O20 S1 C25 F1 59.2(5) . . . . ?
O20 S1 C25 F2 176.9(5) . . . . ?
O20 S1 C25 F3 -62.2(6) . . . . ?
O21 S1 C25 F1 -64.3(5) . . . . ?
O21 S1 C25 F2 53.5(5) . . . . ?
O21 S1 C25 F3 174.3(5) . . . . ?
S1' C25' F2' F3' 110(3) . . . . ?
S1' C25' F3' F2' -106(3) . . . . ?
O20' S1' C25' F1' 65(4) . . . . ?
O20' S1' C25' F2' -171(3) . . . . ?
O20' S1' C25' F3' -90(4) . . . . ?
O21' S1' C25' F1' -52(5) . . . . ?
O21' S1' C25' F2' 72(4) . . . . ?
O21' S1' C25' F3' 152(4) . . . . ?
F1' C25' F2' F3' -125(4) . . . . ?
F1' C25' F3' F2' 103(5) . . . . ?

_olex2_submission_original_sample_id matbp43
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.223
_oxdiff_exptl_absorpt_empirical_full_min 0.401
