# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_mataf28
_database_code_depnum_ccdc_archive 'CCDC 2053153'
loop_
_audit_author_name
_audit_author_address
'William W. Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_vrf_PLAT302_mataf28             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 18% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3  ) .. 100% 
RESPONSE: Butyl group C18-C21 is modeled as disordered over two
positions (0.64(1):0.36(1)). The cocrystallized diethyl ether
solvent molecule is of partial occupancy (0.763(6)).
;

_vrf_PLAT860_mataf28             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 23 
RESPONSE: Analogous bond lengths and angles between the two
positions of the butyl group disorder were restrained to be
similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and restrained toward the
expected motion relative to bond direction.
;

_audit_creation_date             2020-12-05
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C10 H18 N2 O23 V6, 1.526(C4 H10 O), 2(C16 H36 N)'
_chemical_formula_sum            'C48.10 H105.26 N4 O24.52 V6'
_chemical_formula_weight         1437.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.6947(4)
_cell_length_b                   15.5293(5)
_cell_length_c                   18.1049(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.990(4)
_cell_angle_gamma                90
_cell_volume                     3354.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10176
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3410
_cell_measurement_theta_min      3.7290
_shelx_estimated_absorpt_T_max   0.538
_shelx_estimated_absorpt_T_min   0.307
_exptl_absorpt_coefficient_mu    7.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.096
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.169
_diffrn_reflns_theta_min         3.705
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  23.00   0.50    1.08    --  -49.37  86.00 -33.00  194
  2  ω    -30.00  22.00   0.50    1.08    --  -49.37  38.00  60.00  104
  3  ω    -21.00  74.00   0.50    1.08    --   49.37 -86.00-151.00  190
  4  ω     34.00 131.00   0.50    4.31    --  105.75 -86.00-151.00  194
  5  ω     50.00 107.00   0.50    4.31    --  105.75 -94.00-120.00  114
  6  ω     38.00  67.00   0.50    4.31    --  105.75 -61.00 -60.00   58
  7  ω     34.00  87.00   0.50    4.31    --  105.75 -61.00-120.00  106
  8  ω     34.00 109.00   0.50    4.31    --  105.75 -94.00-180.00  150
  9  ω     34.00  87.00   0.50    4.31    --  105.75 -61.00-150.00  106
 10  ω    124.00 151.00   0.50    4.31    --  105.75  15.00 -90.00   54
 11  ω     98.00 178.00   0.50    4.31    --  105.75  86.00 -33.00  160
 12  ω     98.00 164.00   0.50    4.31    --  105.75  15.00  60.00  132
 13  ω     98.00 163.00   0.50    4.31    --  105.75  15.00 150.00  130
 14  ω     92.00 178.00   0.50    4.31    --  105.75 125.00  90.00  172
 15  ω     92.00 178.00   0.50    4.31    --  105.75 125.00 150.00  172
 16  ω     85.00 178.00   0.50    4.31    --  105.75  77.00 -90.00  186
 17  ω     46.00 108.00   0.50    4.31    --  105.75 -94.00 120.00  124
 18  ω     34.00  87.00   0.50    4.31    --  105.75 -61.00 120.00  106
 19  ω     34.00 116.00   0.50    4.31    --  105.75-125.00 120.00  164
 20  ω     34.00  83.00   0.50    4.31    --  105.75 -94.00   0.00   98
 21  ω    -23.00   5.00   0.50    1.08    --   49.37 -19.00-150.00   56
 22  ω   -109.00 -12.00   0.50    4.31    --  -84.25  86.00 -33.00  194
 23  ω   -156.00 -76.00   0.50    4.31    --  -84.25 -86.00-151.00  160
 24  ω   -121.00 -70.00   0.50    1.08    --  -49.37-125.00 -60.00  102
 25  ω   -121.00 -70.00   0.50    1.08    --  -49.37-125.00  30.00  102
 26  ω   -121.00 -70.00   0.50    1.08    --  -49.37-125.00  90.00  102
;
_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      -0.1280227000
_diffrn_orient_matrix_UB_12      0.0030605000
_diffrn_orient_matrix_UB_13      -0.0414419000
_diffrn_orient_matrix_UB_21      -0.0038190000
_diffrn_orient_matrix_UB_22      0.0885977000
_diffrn_orient_matrix_UB_23      0.0371367000
_diffrn_orient_matrix_UB_31      0.0165059000
_diffrn_orient_matrix_UB_32      0.0446555000
_diffrn_orient_matrix_UB_33      -0.0713293000
_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                5465
_reflns_number_total             7044
_reflns_odcompleteness_completeness 99.87
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.085
_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     422
_refine_ls_number_reflns         7044
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.044
_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)+(0.1109P)²+1.8371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1827
_refine_special_details          
;
Butyl group C18-C21 is modeled as disordered over two positions
(0.64(1):0.36(1)). The cocrystallized diethyl ether solvent
molecule is of partial occupancy (0.763(6)). Analogous bond
lengths and angles between the two positions were restrained
to be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and restrained toward the
expected motion relative to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
3. Same fragment restrains
{C18, C19', C20', C21'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C18, C19, C20, C21}
4. Others
 Sof(H18C)=Sof(H18D)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=
 Sof(H20D)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(O13)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C23(H23A,H23B), C24(H24A,H24B), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
  C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C18(H18C,
 H18D), C19(H19A,H19B), C20(H20A,H20B), C19'(H19C,H19D), C20'(H20C,H20D)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C21'(H21D,H21E,
 H21F)
;
_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 0.50568(5) 0.49546(4) 0.62589(4) 0.04495(18) Uani 1 1 d . . . . .
V2 V 0.65435(5) 0.58177(4) 0.52490(4) 0.04521(18) Uani 1 1 d . . . . .
V3 V 0.59426(5) 0.37219(4) 0.51530(4) 0.04465(18) Uani 1 1 d . . . . .
O1 O 0.5174(2) 0.49195(18) 0.71671(16) 0.0549(6) Uani 1 1 d . . . . .
O2 O 0.7689(2) 0.63548(17) 0.55609(16) 0.0542(6) Uani 1 1 d . . . . .
O3 O 0.6768(2) 0.29067(17) 0.53228(16) 0.0533(6) Uani 1 1 d . . . . .
O4 O 0.6425(2) 0.56586(16) 0.63525(14) 0.0471(5) Uani 1 1 d . . . . .
O5 O 0.6015(2) 0.39192(16) 0.62503(14) 0.0470(5) Uani 1 1 d . . . . .
O6 O 0.3755(2) 0.42762(16) 0.57689(15) 0.0488(6) Uani 1 1 d . . . . .
O7 O 0.4140(2) 0.60252(17) 0.59203(14) 0.0472(5) Uani 1 1 d . . . . .
O8 O 0.71965(19) 0.46415(16) 0.54445(14) 0.0463(5) Uani 1 1 d . . . . .
O9 O 0.4598(2) 0.33030(16) 0.48699(14) 0.0486(6) Uani 1 1 d . . . . .
O10 O 0.500000 0.500000 0.500000 0.0420(7) Uani 1 2 d S . P . .
O11 O 0.9785(3) 0.4311(4) 0.7451(2) 0.1122(17) Uani 1 1 d . U . . .
O12 O 0.8824(3) 0.4374(3) 0.8205(2) 0.0969(13) Uani 1 1 d . . . . .
N1 N 0.8911(3) 0.4410(3) 0.7558(2) 0.0669(10) Uani 1 1 d . U . . .
C1 C 0.7419(3) 0.5452(3) 0.6977(2) 0.0521(8) Uani 1 1 d . . . . .
H1A H 0.727463 0.546216 0.746905 0.062 Uiso 1 1 calc R U . . .
H1B H 0.798815 0.588026 0.700583 0.062 Uiso 1 1 calc R U . . .
C2 C 0.7044(3) 0.3837(3) 0.6883(2) 0.0525(9) Uani 1 1 d . . . . .
H2A H 0.738262 0.328501 0.685065 0.063 Uiso 1 1 calc R U . . .
H2B H 0.690547 0.385888 0.737773 0.063 Uiso 1 1 calc R U . . .
C3 C 0.8160(3) 0.4512(3) 0.6113(2) 0.0529(9) Uani 1 1 d . . . . .
H3A H 0.871542 0.494798 0.613120 0.063 Uiso 1 1 calc R U . . .
H3B H 0.848125 0.395223 0.608215 0.063 Uiso 1 1 calc R U . . .
C4 C 0.7848(3) 0.4563(3) 0.6858(2) 0.0527(9) Uani 1 1 d . . . . .
C5 C 0.3156(4) 0.6143(3) 0.6130(3) 0.0593(10) Uani 1 1 d . . . . .
H5A H 0.257866 0.575617 0.582832 0.089 Uiso 1 1 calc R U . . .
H5B H 0.289756 0.672585 0.602227 0.089 Uiso 1 1 calc R U . . .
H5C H 0.333258 0.602484 0.667975 0.089 Uiso 1 1 calc R U . . .
O13 O 1.0275(7) 0.6478(4) 0.8131(5) 0.126(3) Uani 0.763(6) 1 d . . P . .
C22 C 1.0595(9) 0.6802(8) 0.6899(5) 0.129(4) Uani 0.763(6) 1 d . . P . .
H22A H 1.012206 0.637279 0.656474 0.194 Uiso 0.763(6) 1 calc R U P . .
H22B H 1.118694 0.694875 0.670450 0.194 Uiso 0.763(6) 1 calc R U P . .
H22C H 1.015941 0.730630 0.690235 0.194 Uiso 0.763(6) 1 calc R U P . .
C23 C 1.1096(9) 0.6449(7) 0.7732(7) 0.125(4) Uani 0.763(6) 1 d . . P . .
H23A H 1.133727 0.585900 0.771282 0.150 Uiso 0.763(6) 1 calc R U P . .
H23B H 1.174810 0.678718 0.802391 0.150 Uiso 0.763(6) 1 calc R U P . .
C24 C 1.0756(8) 0.6242(6) 0.8915(5) 0.094(2) Uani 0.763(6) 1 d . . P . .
H24A H 1.130660 0.666836 0.919326 0.113 Uiso 0.763(6) 1 calc R U P . .
H24B H 1.113416 0.569251 0.895239 0.113 Uiso 0.763(6) 1 calc R U P . .
C25 C 0.9903(9) 0.6176(7) 0.9268(6) 0.118(3) Uani 0.763(6) 1 d . . P . .
H25A H 0.937040 0.574181 0.900051 0.178 Uiso 0.763(6) 1 calc R U P . .
H25B H 0.952709 0.671952 0.922731 0.178 Uiso 0.763(6) 1 calc R U P . .
H25C H 1.024055 0.602212 0.981175 0.178 Uiso 0.763(6) 1 calc R U P . .
N2 N 0.3363(3) 0.3406(2) 0.79932(19) 0.0559(8) Uani 1 1 d . . . . .
C6 C 0.2703(4) 0.3936(3) 0.7277(2) 0.0573(9) Uani 1 1 d . . . . .
H6A H 0.237770 0.442426 0.745583 0.069 Uiso 1 1 calc R U . . .
H6B H 0.322394 0.416118 0.703950 0.069 Uiso 1 1 calc R U . . .
C7 C 0.1773(4) 0.3472(3) 0.6648(2) 0.0572(9) Uani 1 1 d . . . . .
H7A H 0.126866 0.320659 0.688040 0.069 Uiso 1 1 calc R U . . .
H7B H 0.209004 0.302055 0.641811 0.069 Uiso 1 1 calc R U . . .
C8 C 0.1125(3) 0.4103(3) 0.6011(2) 0.0575(9) Uani 1 1 d . . . . .
H8A H 0.075553 0.452081 0.623736 0.069 Uiso 1 1 calc R U . . .
H8B H 0.164893 0.441123 0.582393 0.069 Uiso 1 1 calc R U . . .
C9 C 0.0252(4) 0.3668(3) 0.5318(3) 0.0635(11) Uani 1 1 d . . . . .
H9A H -0.016000 0.409738 0.495133 0.095 Uiso 1 1 calc R U . . .
H9B H -0.025377 0.334314 0.550105 0.095 Uiso 1 1 calc R U . . .
H9C H 0.061758 0.328821 0.506348 0.095 Uiso 1 1 calc R U . . .
C10 C 0.3771(4) 0.2572(3) 0.7747(2) 0.0586(10) Uani 1 1 d . . . . .
H10A H 0.416178 0.224324 0.821642 0.070 Uiso 1 1 calc R U . . .
H10B H 0.312227 0.223836 0.744111 0.070 Uiso 1 1 calc R U . . .
C11 C 0.4536(4) 0.2667(3) 0.7273(3) 0.0631(10) Uani 1 1 d . . . . .
H11A H 0.525097 0.290353 0.759880 0.076 Uiso 1 1 calc R U . . .
H11B H 0.420452 0.305423 0.683490 0.076 Uiso 1 1 calc R U . . .
C12 C 0.4704(5) 0.1780(3) 0.6973(3) 0.0823(14) Uani 1 1 d . . . . .
H12A H 0.497134 0.139265 0.741854 0.099 Uiso 1 1 calc R U . . .
H12B H 0.398214 0.156741 0.663462 0.099 Uiso 1 1 calc R U . . .
C13 C 0.5494(6) 0.1744(4) 0.6534(4) 0.0897(16) Uani 1 1 d . . . . .
H13A H 0.522953 0.211180 0.608115 0.135 Uiso 1 1 calc R U . . .
H13B H 0.554397 0.116311 0.636788 0.135 Uiso 1 1 calc R U . . .
H13C H 0.622054 0.193446 0.686661 0.135 Uiso 1 1 calc R U . . .
C14 C 0.4346(4) 0.3967(3) 0.8467(2) 0.0570(9) Uani 1 1 d . . . . .
H14A H 0.479344 0.409802 0.814164 0.068 Uiso 1 1 calc R U . . .
H14B H 0.405229 0.450646 0.858433 0.068 Uiso 1 1 calc R U . . .
C15 C 0.5104(4) 0.3583(3) 0.9228(2) 0.0611(10) Uani 1 1 d . . . . .
H15A H 0.536701 0.302435 0.912625 0.073 Uiso 1 1 calc R U . . .
H15B H 0.468704 0.350201 0.958252 0.073 Uiso 1 1 calc R U . . .
C16 C 0.6100(4) 0.4166(3) 0.9611(3) 0.0644(11) Uani 1 1 d . . . . .
H16A H 0.583113 0.474220 0.965196 0.077 Uiso 1 1 calc R U . . .
H16B H 0.649555 0.396060 1.013991 0.077 Uiso 1 1 calc R U . . .
C17 C 0.6910(5) 0.4206(4) 0.9165(3) 0.0825(15) Uani 1 1 d . . . . .
H17A H 0.654166 0.445375 0.865593 0.124 Uiso 1 1 calc R U . . .
H17B H 0.715922 0.363482 0.910521 0.124 Uiso 1 1 calc R U . . .
H17C H 0.754292 0.455422 0.945004 0.124 Uiso 1 1 calc R U . . .
C18 C 0.2650(4) 0.3147(3) 0.8482(3) 0.0636(11) Uani 1 1 d D . . . .
H18A H 0.203400 0.279150 0.816408 0.076 Uiso 0.645(11) 1 calc R U P A 1
H18B H 0.310136 0.280455 0.892472 0.076 Uiso 0.645(11) 1 calc R U P A 1
H18C H 0.199499 0.285786 0.812753 0.076 Uiso 0.355(11) 1 calc R U P A 2
H18D H 0.307430 0.271627 0.885197 0.076 Uiso 0.355(11) 1 calc R U P A 2
C19 C 0.2183(19) 0.3914(8) 0.8784(11) 0.059(3) Uani 0.645(11) 1 d D U P A 1
H19A H 0.277678 0.432653 0.902007 0.070 Uiso 0.645(11) 1 calc R U P A 1
H19B H 0.161326 0.419482 0.835068 0.070 Uiso 0.645(11) 1 calc R U P A 1
C20 C 0.1679(13) 0.3624(10) 0.9387(7) 0.068(3) Uani 0.645(11) 1 d D U P A 1
H20A H 0.121855 0.408627 0.947152 0.082 Uiso 0.645(11) 1 calc R U P A 1
H20B H 0.119214 0.313596 0.917708 0.082 Uiso 0.645(11) 1 calc R U P A 1
C21 C 0.2527(6) 0.3372(5) 1.0168(4) 0.065(2) Uani 0.645(11) 1 d D . P A 1
H21A H 0.291623 0.286283 1.010465 0.097 Uiso 0.645(11) 1 calc R U P A 1
H21B H 0.215117 0.326097 1.053689 0.097 Uiso 0.645(11) 1 calc R U P A 1
H21C H 0.305523 0.383255 1.036050 0.097 Uiso 0.645(11) 1 calc R U P A 1
C19' C 0.223(4) 0.3784(14) 0.895(2) 0.065(6) Uani 0.355(11) 1 d D U P A 2
H19C H 0.286662 0.406196 0.933120 0.077 Uiso 0.355(11) 1 calc R U P A 2
H19D H 0.179515 0.422480 0.859360 0.077 Uiso 0.355(11) 1 calc R U P A 2
C20' C 0.152(3) 0.3376(17) 0.9364(18) 0.070(6) Uani 0.355(11) 1 d D U P A 2
H20C H 0.192590 0.289604 0.967339 0.084 Uiso 0.355(11) 1 calc R U P A 2
H20D H 0.084563 0.314634 0.897360 0.084 Uiso 0.355(11) 1 calc R U P A 2
C21' C 0.117(2) 0.3974(13) 0.9899(12) 0.109(7) Uani 0.355(11) 1 d D . P A 2
H21D H 0.178849 0.405202 1.038008 0.163 Uiso 0.355(11) 1 calc R U P A 2
H21E H 0.054792 0.372980 1.001099 0.163 Uiso 0.355(11) 1 calc R U P A 2
H21F H 0.095739 0.452138 0.964443 0.163 Uiso 0.355(11) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.600(3) . ?
V1 O4 2.009(3) . ?
V1 O5 2.019(3) . ?
V1 O6 1.904(3) . ?
V1 O7 2.002(3) . ?
V1 O10 2.2566(6) . ?
V2 O2 1.603(3) . ?
V2 O4 2.069(3) . ?
V2 O6 1.756(3) 3_666 ?
V2 O8 1.987(3) . ?
V2 O9 1.949(3) 3_666 ?
V2 O10 2.2474(6) . ?
V3 O3 1.604(3) . ?
V3 O5 1.981(2) . ?
V3 O7 1.950(3) 3_666 ?
V3 O8 2.068(3) . ?
V3 O9 1.732(3) . ?
V3 O10 2.2851(6) . ?
O4 C1 1.413(4) . ?
O5 C2 1.419(4) . ?
O7 C5 1.436(5) . ?
O8 C3 1.410(4) . ?
O11 N1 1.199(5) . ?
O12 N1 1.215(5) . ?
N1 C4 1.522(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.525(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.532(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.532(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
O13 C23 1.459(13) . ?
O13 C24 1.388(11) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 C23 1.525(13) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.437(13) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N2 C6 1.522(5) . ?
N2 C10 1.518(5) . ?
N2 C14 1.523(5) . ?
N2 C18 1.520(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.514(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.522(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.519(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.506(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.522(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.478(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.507(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.516(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.510(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 C19 1.514(10) . ?
C18 C19' 1.509(15) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.510(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.507(17) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20' 1.502(17) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C20' C21' 1.51(2) . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 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
O1 V1 O4 99.06(13) . . ?
O1 V1 O5 97.81(12) . . ?
O1 V1 O6 102.77(13) . . ?
O1 V1 O7 100.55(13) . . ?
O1 V1 O10 176.68(11) . . ?
O4 V1 O5 85.90(11) . . ?
O4 V1 O10 78.26(7) . . ?
O5 V1 O10 80.12(7) . . ?
O6 V1 O4 158.08(11) . . ?
O6 V1 O5 89.14(11) . . ?
O6 V1 O7 89.74(11) . . ?
O6 V1 O10 79.85(8) . . ?
O7 V1 O4 88.25(10) . . ?
O7 V1 O5 161.39(10) . . ?
O7 V1 O10 81.40(7) . . ?
O2 V2 O4 94.53(13) . . ?
O2 V2 O6 104.91(14) . 3_666 ?
O2 V2 O8 98.20(12) . . ?
O2 V2 O9 103.02(13) . 3_666 ?
O2 V2 O10 171.38(11) . . ?
O4 V2 O10 77.28(7) . . ?
O6 V2 O4 160.49(12) 3_666 . ?
O6 V2 O8 92.17(11) 3_666 . ?
O6 V2 O9 93.25(11) 3_666 3_666 ?
O6 V2 O10 83.22(9) 3_666 . ?
O8 V2 O4 83.22(10) . . ?
O8 V2 O10 78.37(7) . . ?
O9 V2 O4 83.88(10) 3_666 . ?
O9 V2 O8 155.92(11) 3_666 . ?
O9 V2 O10 79.01(8) 3_666 . ?
O3 V3 O5 97.27(12) . . ?
O3 V3 O7 99.14(13) . 3_666 ?
O3 V3 O8 95.80(12) . . ?
O3 V3 O9 105.84(13) . . ?
O3 V3 O10 171.55(10) . . ?
O5 V3 O8 82.50(10) . . ?
O5 V3 O10 80.21(7) . . ?
O7 V3 O5 159.48(11) 3_666 . ?
O7 V3 O8 83.66(10) 3_666 . ?
O7 V3 O10 81.77(8) 3_666 . ?
O8 V3 O10 75.91(7) . . ?
O9 V3 O5 93.32(11) . . ?
O9 V3 O7 93.96(11) . 3_666 ?
O9 V3 O8 158.32(11) . . ?
O9 V3 O10 82.42(8) . . ?
V1 O4 V2 109.25(11) . . ?
C1 O4 V1 117.0(2) . . ?
C1 O4 V2 117.3(2) . . ?
V3 O5 V1 108.02(11) . . ?
C2 O5 V1 117.1(2) . . ?
C2 O5 V3 120.7(2) . . ?
V2 O6 V1 112.11(13) 3_666 . ?
V3 O7 V1 107.44(12) 3_666 . ?
C5 O7 V1 119.5(2) . . ?
C5 O7 V3 118.9(2) . 3_666 ?
V2 O8 V3 110.58(11) . . ?
C3 O8 V2 118.1(2) . . ?
C3 O8 V3 119.1(2) . . ?
V3 O9 V2 112.95(13) . 3_666 ?
V1 O10 V1 180.0 3_666 . ?
V1 O10 V3 90.91(2) 3_666 3_666 ?
V1 O10 V3 90.91(2) . . ?
V1 O10 V3 89.09(2) 3_666 . ?
V1 O10 V3 89.09(2) . 3_666 ?
V2 O10 V1 95.19(2) 3_666 3_666 ?
V2 O10 V1 95.19(2) . . ?
V2 O10 V1 84.81(2) . 3_666 ?
V2 O10 V1 84.81(2) 3_666 . ?
V2 O10 V2 180.00(3) 3_666 . ?
V2 O10 V3 94.70(2) 3_666 3_666 ?
V2 O10 V3 85.30(2) 3_666 . ?
V2 O10 V3 85.30(2) . 3_666 ?
V2 O10 V3 94.70(2) . . ?
V3 O10 V3 180.0 3_666 . ?
O11 N1 O12 122.9(4) . . ?
O11 N1 C4 119.5(4) . . ?
O12 N1 C4 117.6(4) . . ?
O4 C1 H1A 109.5 . . ?
O4 C1 H1B 109.5 . . ?
O4 C1 C4 110.9(3) . . ?
H1A C1 H1B 108.0 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
O5 C2 H2A 109.6 . . ?
O5 C2 H2B 109.6 . . ?
O5 C2 C4 110.4(3) . . ?
H2A C2 H2B 108.1 . . ?
C4 C2 H2A 109.6 . . ?
C4 C2 H2B 109.6 . . ?
O8 C3 H3A 109.7 . . ?
O8 C3 H3B 109.7 . . ?
O8 C3 C4 109.8(3) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
N1 C4 C1 106.4(3) . . ?
N1 C4 C2 105.7(3) . . ?
N1 C4 C3 107.6(3) . . ?
C1 C4 C2 112.8(3) . . ?
C1 C4 C3 112.5(3) . . ?
C2 C4 C3 111.3(3) . . ?
O7 C5 H5A 109.5 . . ?
O7 C5 H5B 109.5 . . ?
O7 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C24 O13 C23 111.1(8) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
O13 C23 C22 110.6(9) . . ?
O13 C23 H23A 109.5 . . ?
O13 C23 H23B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
O13 C24 H24A 109.7 . . ?
O13 C24 H24B 109.7 . . ?
O13 C24 C25 109.8(8) . . ?
H24A C24 H24B 108.2 . . ?
C25 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C6 N2 C14 106.2(3) . . ?
C10 N2 C6 110.8(3) . . ?
C10 N2 C14 110.9(3) . . ?
C10 N2 C18 106.0(3) . . ?
C18 N2 C6 112.0(3) . . ?
C18 N2 C14 111.1(3) . . ?
N2 C6 H6A 108.2 . . ?
N2 C6 H6B 108.2 . . ?
H6A C6 H6B 107.3 . . ?
C7 C6 N2 116.4(3) . . ?
C7 C6 H6A 108.2 . . ?
C7 C6 H6B 108.2 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C6 C7 C8 110.1(4) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 C7 113.1(4) . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 108.3 . . ?
N2 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N2 115.8(3) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
C10 C11 C12 108.1(4) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
C11 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 C11 115.5(5) . . ?
C13 C12 H12A 108.4 . . ?
C13 C12 H12B 108.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 108.4 . . ?
N2 C14 H14B 108.4 . . ?
H14A C14 H14B 107.4 . . ?
C15 C14 N2 115.7(3) . . ?
C15 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 C16 110.8(4) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C15 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 C15 113.2(4) . . ?
C17 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.0 . . ?
N2 C18 H18B 109.0 . . ?
N2 C18 H18C 106.6 . . ?
N2 C18 H18D 106.6 . . ?
H18A C18 H18B 107.8 . . ?
H18C C18 H18D 106.5 . . ?
C19 C18 N2 112.8(7) . . ?
C19 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C19' C18 N2 123.1(11) . . ?
C19' C18 H18C 106.6 . . ?
C19' C18 H18D 106.6 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 C18 110.0(11) . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C21 C20 C19 114.3(13) . . ?
C21 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C19' H19C 108.9 . . ?
C18 C19' H19D 108.9 . . ?
H19C C19' H19D 107.8 . . ?
C20' C19' C18 113.2(17) . . ?
C20' C19' H19C 108.9 . . ?
C20' C19' H19D 108.9 . . ?
C19' C20' H20C 108.6 . . ?
C19' C20' H20D 108.6 . . ?
C19' C20' C21' 114.8(17) . . ?
H20C C20' H20D 107.5 . . ?
C21' C20' H20C 108.6 . . ?
C21' C20' H20D 108.6 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 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 O4 C1 C4 66.9(4) . . . . ?
V1 O5 C2 C4 -66.3(4) . . . . ?
V2 O4 C1 C4 -65.9(4) . . . . ?
V2 O8 C3 C4 71.2(4) . . . . ?
V3 O5 C2 C4 68.8(4) . . . . ?
V3 O8 C3 C4 -67.7(4) . . . . ?
O3 V3 O9 V2 173.24(14) . . . 3_666 ?
O4 C1 C4 N1 -180.0(3) . . . . ?
O4 C1 C4 C2 -64.6(4) . . . . ?
O4 C1 C4 C3 62.4(4) . . . . ?
O5 V3 O9 V2 74.71(14) . . . 3_666 ?
O5 C2 C4 N1 180.0(3) . . . . ?
O5 C2 C4 C1 64.1(4) . . . . ?
O5 C2 C4 C3 -63.5(4) . . . . ?
O7 V3 O9 V2 -86.09(14) 3_666 . . 3_666 ?
O8 V3 O9 V2 -3.3(4) . . . 3_666 ?
O8 C3 C4 N1 179.4(3) . . . . ?
O8 C3 C4 C1 -63.8(4) . . . . ?
O8 C3 C4 C2 64.1(4) . . . . ?
O10 V3 O9 V2 -4.95(11) . . . 3_666 ?
O11 N1 C4 C1 -118.1(5) . . . . ?
O11 N1 C4 C2 121.7(5) . . . . ?
O11 N1 C4 C3 2.7(6) . . . . ?
O12 N1 C4 C1 63.5(5) . . . . ?
O12 N1 C4 C2 -56.7(5) . . . . ?
O12 N1 C4 C3 -175.7(4) . . . . ?
C23 O13 C24 C25 -173.1(8) . . . . ?
C24 O13 C23 C22 -173.8(8) . . . . ?
N2 C6 C7 C8 174.8(4) . . . . ?
N2 C10 C11 C12 -171.1(4) . . . . ?
N2 C14 C15 C16 175.3(4) . . . . ?
N2 C18 C19 C20 -169.0(11) . . . . ?
N2 C18 C19' C20' 178(2) . . . . ?
C6 N2 C10 C11 60.3(5) . . . . ?
C6 N2 C14 C15 177.9(4) . . . . ?
C6 N2 C18 C19 -59.7(11) . . . . ?
C6 N2 C18 C19' -69(2) . . . . ?
C6 C7 C8 C9 174.3(4) . . . . ?
C10 N2 C6 C7 50.8(5) . . . . ?
C10 N2 C14 C15 -61.7(5) . . . . ?
C10 N2 C18 C19 179.4(10) . . . . ?
C10 N2 C18 C19' 170(2) . . . . ?
C10 C11 C12 C13 -176.4(5) . . . . ?
C14 N2 C6 C7 171.3(4) . . . . ?
C14 N2 C10 C11 -57.3(4) . . . . ?
C14 N2 C18 C19 58.8(11) . . . . ?
C14 N2 C18 C19' 50(2) . . . . ?
C14 C15 C16 C17 -69.1(6) . . . . ?
C18 N2 C6 C7 -67.3(5) . . . . ?
C18 N2 C10 C11 -178.0(3) . . . . ?
C18 N2 C14 C15 55.9(5) . . . . ?
C18 C19 C20 C21 73.1(17) . . . . ?
C18 C19' C20' C21' 174(3) . . . . ?

_olex2_submission_original_sample_id mataf28
_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 2.548
_oxdiff_exptl_absorpt_empirical_full_min 0.463
####################################################################### 
# 
# 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_mataf22
_database_code_depnum_ccdc_archive 'CCDC 2053155'
loop_
_audit_author_name
_audit_author_address
'William W. Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_vrf_PLAT301_mataf22             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 10% 
RESPONSE: One NO2 group is modeled as disordered over two positions
(0.766(8):0.234(8)). The methoxy ligand is modeled as disordered over
three bridging V-O-V sites: O16-C25, 0.550(3), O10-C25', 0.280(3),
O9-C25", 0.170(2).
;

_vrf_PLAT302_mataf22             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 47% 
RESPONSE: Portions of three arms of the cation are modeled as
disordered over two positions each: C13-C16, 0.830(2):0.170(2),
C17-C20, 0.57(1):0.43(1), C21-C24, 0.77(4):0.23(4). The common
disorder ratio between C21-C24 and the occupancy of methoxy
ligand disorder O9-C25" (see response to alert PLAT301) is due
to adjacency, which was additionally confirmed by similar
independent disorder ratios.
;

_vrf_PLAT605_mataf22             
;
PROBLEM: _G Largest Solvent Accessible VOID in the Structure .. 46 A**3 
RESPONSE: The solvent site at a crystallographic inversion center
appeared to contain mostly acetonitrile. Unfortunately, because of
the three-site methoxy ligand disorder, not all electron density was
able to be assigned. Therefore, reflection contributions from this
site were fixed and added to the calculated structure factors
using the SQUEEZE routine of program PLATON (Spek, 2015), which
determined there to be two sites of 47 electrons in 131 \%A^3^
(94 electrons in 262 \%A^3^) per unit cell treated this way.
Because the exact identity and amount of solvent were unknown,
no solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.
;

_vrf_PLAT860_mataf22             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 218 
RESPONSE: Analogous bond lengths and angles were restrained to
be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and additionally restrained
toward the expected motion with respect to bond direction.
;

_vrf_PLAT869_mataf22             
;
PROBLEM: _G ALERTS Related to the Use of SQUEEZE Suppressed! 
RESPONSE: The solvent site at a crystallographic inversion center
appeared to contain mostly acetonitrile. Unfortunately, because of
the three-site methoxy ligand disorder, not all electron density was
able to be assigned. Therefore, reflection contributions from this
site were fixed and added to the calculated structure factors
using the SQUEEZE routine of program PLATON (Spek, 2015), which
determined there to be two sites of 47 electrons in 131 \%A^3^
(94 electrons in 262 \%A^3^) per unit cell treated this way.
Because the exact identity and amount of solvent were unknown,
no solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.
;

_audit_creation_date             2020-09-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H15 N2 O23 V6, C16 H36 N'
_chemical_formula_sum            'C25 H51 N3 O23 V6'
_chemical_formula_weight         1067.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.85930(10)
_cell_length_b                   17.31290(10)
_cell_length_c                   17.69540(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.6180(10)
_cell_angle_gamma                90
_cell_volume                     4173.22(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39776
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3150
_cell_measurement_theta_min      3.5960
_shelx_estimated_absorpt_T_max   0.314
_shelx_estimated_absorpt_T_min   0.141
_exptl_absorpt_coefficient_mu    11.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red-orange
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71313
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.910
_diffrn_reflns_theta_min         3.602
_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 0.998
_diffrn_measured_fraction_theta_max 0.987
_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  24.00   0.50    0.20    --  -49.75  19.00 -90.00   58
  2  ω     -5.00  24.00   0.50    0.20    --  -49.75  19.00 -30.00   58
  3  ω     -5.00  24.00   0.50    0.20    --  -49.75  19.00  60.00   58
  4  ω     22.00  89.00   0.50    0.20    --   49.75-112.00  47.00  134
  5  ω     34.00 112.00   0.50    0.81    --  105.75-112.00  47.00  156
  6  ω     34.00 127.00   0.50    0.81    --  105.75 -77.00  60.00  186
  7  ω     98.00 178.00   0.50    0.81    --  105.75  30.00  60.00  160
  8  ω    100.00 178.00   0.50    0.81    --  105.75 112.00 140.00  156
  9  ω     92.00 178.00   0.50    0.81    --  105.75 125.00 120.00  172
 10  ω     98.00 175.00   0.50    0.81    --  105.75  15.00 -90.00  154
 11  ω     98.00 175.00   0.50    0.81    --  105.75  15.00-150.00  154
 12  ω     98.00 175.00   0.50    0.81    --  105.75  15.00-120.00  154
 13  ω     42.00 121.00   0.50    0.20    --   49.75  38.00  30.00  158
 14  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00  60.00   92
 15  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00  60.00  150
 16  ω     34.00 127.00   0.50    0.81    --  105.75 -77.00 150.00  186
 17  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00  30.00   92
 18  ω     34.00 116.00   0.50    0.81    --  105.75-125.00 120.00  164
 19  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00 120.00  150
 20  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-120.00   92
 21  ω     34.00 109.00   0.50    0.81    --  105.75 -94.00-180.00  150
 22  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-180.00   92
 23  ω     34.00  80.00   0.50    0.81    --  105.75 -61.00-150.00   92
 24  ω     29.00 121.00   0.50    0.20    --   49.75  77.00  60.00  184
 25  ω     29.00 121.00   0.50    0.20    --   49.75  77.00 150.00  184
 26  ω    -86.00   0.00   0.50    0.20    --  -49.75 112.00 140.00  172
 27  ω    -86.00 -12.00   0.50    0.81    --  -84.25 112.00 140.00  148
 28  ω   -121.00 -68.00   0.50    0.20    --  -49.75 -77.00-150.00  106
 29  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00-150.00  102
 30  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00-180.00  102
 31  ω   -121.00 -29.00   0.50    0.20    --  -49.75 -77.00 -90.00  184
 32  ω   -121.00 -29.00   0.50    0.20    --  -49.75 -77.00   0.00  184
 33  ω   -121.00 -70.00   0.50    0.20    --  -49.75-125.00 120.00  102
 34  ω   -156.00 -78.00   0.50    0.81    --  -84.25-112.00  47.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1046485000
_diffrn_orient_matrix_UB_12      -0.0063475000
_diffrn_orient_matrix_UB_13      0.0475378000
_diffrn_orient_matrix_UB_21      -0.0007952000
_diffrn_orient_matrix_UB_22      0.0870808000
_diffrn_orient_matrix_UB_23      0.0177260000
_diffrn_orient_matrix_UB_31      -0.0429139000
_diffrn_orient_matrix_UB_32      -0.0170468000
_diffrn_orient_matrix_UB_33      0.0726172000
_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                8373
_reflns_number_total             8801
_reflns_odcompleteness_completeness 99.83
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         1.047
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0645
_refine_ls_restrained_S_all      1.127
_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)+(0.0530P)²+21.2508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1600
_refine_special_details          
;
The solvent site at a crystallographic inversion center appeared
to contain mostly acetonitrile. Unfortunately, because of the
three-site methoxy ligand disorder, not all electron density was
able to be assigned. Therefore, reflection contributions from this
site were fixed and added to the calculated structure factors
using the SQUEEZE routine of program PLATON (Spek, 2015), which
determined there to be two sites of 47 electrons in 131 Å³
(94 electrons in 262 Å³) per unit cell treated this way.
Because the exact identity and amount of solvent were unknown,
no solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.

Portions of three arms of the cation are modeled as disordered
over two positions each: C13-C16, 0.830(2):0.170(2), C17-C20,
0.57(1):0.43(1), C21-C24, 0.77(4):0.23(4). The common disorder
ratio between C21-C24 and the occupancy of methoxy ligand
isorder O9-C25" (see response to alert PLAT301) is due to
adjacency, which was additionally confirmed by similar
independent disorder ratios.

Analogous bond lengths and angles were restrained to be
similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and additionally restrained
toward the expected motion with respect to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-N2 \\sim C8-N2'
 with sigma of 0.01
 N2-O22 \\sim N2-O23 \\sim N2'-O22' \\sim N2'-O23'
 with sigma of 0.01
 O22-O23 \\sim O22'-O23'
 with sigma of 0.02
 O16-C25 \\sim O10-C25' \\sim O9-C25"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
O22' \\sim N2' \\sim O23': within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
O10 \\sim C25': within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O9 \\sim C25": within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
4. Rigid body (RIGU) restrains
 C8, N2, O22, O23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14', C15', C16'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19', C20'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22', C23', C24'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C13, C14', C15', C16'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C13, C14, C15, C16}
{C18, C19', C20'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C18, C19, C20}
{C21, C22', C23', C24'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C21, C22, C23, C24}
6. Others
 1*[Sof(C25)+Sof(H25A)+Sof(H25B)+Sof(H25C)]+1*[Sof(C25')+Sof(H25D)+Sof(H25E)+
 Sof(H25F)]+1*[Sof(C25")+Sof(H25G)+Sof(H25H)+Sof(H25I)]=1 with esd of 0.0001
 1*[Sof(C25")+Sof(H25G)+Sof(H25H)+Sof(H25I)]+1*[Sof(H13A)+Sof(H13B)+Sof(H13C)+
 Sof(H13D)+Sof(C14)+Sof(H14A)+Sof(H14B)+Sof(C15)+Sof(H15A)+Sof(H15B)+Sof(C16)+
 Sof(H16A)+Sof(H16B)+Sof(H16C)+Sof(C14')+Sof(H14C)+Sof(H14D)+Sof(C15')+
 Sof(H15C)+Sof(H15D)+Sof(C16')+Sof(H16D)+Sof(H16E)+Sof(H16F)]=1 with esd of
 0.0001
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(2)
 Sof(C25")=Sof(H25G)=Sof(H25H)=Sof(H25I)=FVAR(3)
 Sof(N2')=Sof(O22')=Sof(O23')=1-FVAR(4)
 Sof(N2)=Sof(O22)=Sof(O23)=FVAR(4)
 Sof(H13C)=Sof(H13D)=Sof(C14')=Sof(H14C)=Sof(H14D)=Sof(C15')=Sof(H15C)=
 Sof(H15D)=Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(5)
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(5)
 Sof(H18C)=Sof(H18D)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(6)
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(6)
 Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22C)=Sof(H22D)=Sof(C23')=Sof(H23C)=
 Sof(H23D)=Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(7)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(7)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C13(H13C,H13D),
 C14(H14A,H14B), C15(H15A,H15B), C14'(H14C,H14D), C15'(H15C,H15D), C17(H17A,
 H17B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B), C19'(H19C,H19D),
 C21(H21A,H21B), C21(H21C,H21D), C22(H22A,H22B), C23(H23A,H23B), C22'(H22C,
 H22D), C23'(H23C,H23D)
7.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C25'(H25D,H25E,H25F), C25"(H25G,H25H,H25I), C12(H12A,
 H12B,H12C), C16(H16A,H16B,H16C), C16'(H16D,H16E,H16F), C20(H20A,H20B,H20C),
 C20'(H20D,H20E,H20F), C24(H24A,H24B,H24C), 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 0.62282(6) 0.64375(5) 0.52002(6) 0.0372(2) Uani 1 1 d . . . . .
V2 V 0.60444(5) 0.73849(5) 0.35657(4) 0.02450(19) Uani 1 1 d . . . . .
V3 V 0.48522(5) 0.79729(4) 0.49149(4) 0.01821(16) Uani 1 1 d . . . . .
V4 V 0.67468(5) 0.79373(4) 0.60696(4) 0.01488(15) Uani 1 1 d . . . . .
V5 V 0.79353(5) 0.73325(5) 0.47294(4) 0.02298(18) Uani 1 1 d . . . . .
V6 V 0.65767(5) 0.88605(4) 0.44236(4) 0.02098(17) Uani 1 1 d . . . . .
O1 O 0.5994(3) 0.5564(2) 0.5386(3) 0.0614(15) Uani 1 1 d . . . . .
O2 O 0.5661(3) 0.7121(3) 0.2700(2) 0.0453(11) Uani 1 1 d . . . . .
O3 O 0.3716(2) 0.8125(2) 0.4896(2) 0.0302(7) Uani 1 1 d . . . . .
O4 O 0.7134(2) 0.8201(2) 0.69419(17) 0.0277(7) Uani 1 1 d . . . . .
O5 O 0.9076(2) 0.7189(3) 0.4756(2) 0.0442(11) Uani 1 1 d . . . . .
O6 O 0.6822(3) 0.9742(2) 0.4268(2) 0.0423(10) Uani 1 1 d . . . . .
O7 O 0.5827(2) 0.63661(19) 0.4058(2) 0.0311(8) Uani 1 1 d . . . . .
O8 O 0.4852(2) 0.68490(17) 0.51233(17) 0.0224(6) Uani 1 1 d . . . . .
O9 O 0.6524(2) 0.69057(18) 0.61410(18) 0.0251(7) Uani 1 1 d D U . . .
O10 O 0.7513(2) 0.6388(2) 0.5076(2) 0.0370(9) Uani 1 1 d D U . . .
O11 O 0.4721(2) 0.76190(17) 0.38143(15) 0.0179(6) Uani 1 1 d . . . . .
O12 O 0.5421(2) 0.81614(19) 0.58948(16) 0.0225(6) Uani 1 1 d . . . . .
O13 O 0.80659(19) 0.77076(16) 0.58199(15) 0.0163(5) Uani 1 1 d . . . . .
O14 O 0.7363(2) 0.7161(3) 0.3750(2) 0.0399(10) Uani 1 1 d . . . . .
O15 O 0.6259(2) 0.8420(2) 0.34897(17) 0.0356(9) Uani 1 1 d . . . . .
O16 O 0.5272(2) 0.89203(17) 0.45550(19) 0.0263(7) Uani 1 1 d D . . . .
O17 O 0.6957(2) 0.89531(16) 0.55800(16) 0.0191(6) Uani 1 1 d . . . . .
O18 O 0.7941(2) 0.8460(2) 0.45114(16) 0.0270(7) Uani 1 1 d . . . . .
O19 O 0.63938(19) 0.76590(16) 0.48204(15) 0.0146(5) Uani 1 1 d . . . . .
C1 C 0.4975(4) 0.5928(3) 0.3729(4) 0.0379(13) Uani 1 1 d . . . . .
H1A H 0.501781 0.541312 0.394890 0.046 Uiso 1 1 calc R U . . .
H1B H 0.493932 0.588079 0.317868 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4042(3) 0.6387(3) 0.4753(3) 0.0281(10) Uani 1 1 d . . . . .
H2A H 0.342949 0.661720 0.483052 0.034 Uiso 1 1 calc R U . . .
H2B H 0.408787 0.587361 0.497692 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3915(3) 0.7135(2) 0.3513(2) 0.0199(8) Uani 1 1 d . . . . .
H3A H 0.386464 0.708486 0.296116 0.024 Uiso 1 1 calc R U . . .
H3B H 0.331100 0.736437 0.361062 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4056(3) 0.6332(3) 0.3892(3) 0.0268(10) Uani 1 1 d . . . . .
N1 N 0.3169(3) 0.5866(2) 0.3517(3) 0.0351(10) Uani 1 1 d . . . . .
O20 O 0.3257(3) 0.5431(2) 0.2990(2) 0.0443(10) Uani 1 1 d . . . . .
O21 O 0.2404(3) 0.5970(3) 0.3742(3) 0.0549(12) Uani 1 1 d . . . . .
C5 C 0.7798(3) 0.9403(3) 0.5896(3) 0.0269(10) Uani 1 1 d . . . . .
H5A H 0.783744 0.946127 0.644643 0.032 Uiso 1 1 calc R U . . .
H5B H 0.774845 0.991257 0.566524 0.032 Uiso 1 1 calc R U . . .
C6 C 0.8740(3) 0.8936(3) 0.4870(3) 0.0319(11) Uani 1 1 d . . . . .
H6A H 0.867992 0.944716 0.464288 0.038 Uiso 1 1 calc R U . . .
H6B H 0.935767 0.871378 0.479348 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8873(3) 0.8199(3) 0.6129(2) 0.0208(8) Uani 1 1 d . . . . .
H7A H 0.948239 0.797175 0.604140 0.025 Uiso 1 1 calc R U . . .
H7B H 0.891117 0.825821 0.667849 0.025 Uiso 1 1 calc R U . . .
C8 C 0.8722(3) 0.8990(3) 0.5734(3) 0.0257(9) Uani 1 1 d D . . . .
N2 N 0.9556(4) 0.9530(3) 0.6076(3) 0.0362(15) Uani 0.766(8) 1 d D U P A 1
O22 O 0.9580(4) 1.0177(3) 0.5816(3) 0.0407(14) Uani 0.766(8) 1 d D . P A 1
O23 O 1.0129(5) 0.9322(4) 0.6638(4) 0.068(2) Uani 0.766(8) 1 d D U P A 1
N2' N 0.9672(10) 0.9388(16) 0.6121(14) 0.054(3) Uani 0.234(8) 1 d D U P A 2
O22' O 0.9643(14) 0.9625(14) 0.6766(11) 0.059(4) Uani 0.234(8) 1 d D U P A 2
O23' O 1.0447(11) 0.9161(12) 0.5970(11) 0.054(4) Uani 0.234(8) 1 d D U P A 2
C25 C 0.4869(10) 0.9611(5) 0.4855(6) 0.046(3) Uani 0.550(3) 1 d D . P B 1
H25A H 0.417166 0.955446 0.480982 0.068 Uiso 0.550(3) 1 calc R U P B 1
H25B H 0.500696 1.005340 0.456555 0.068 Uiso 0.550(3) 1 calc R U P B 1
H25C H 0.516360 0.967844 0.538548 0.068 Uiso 0.550(3) 1 calc R U P B 1
C25' C 0.7829(13) 0.5633(8) 0.4936(12) 0.036(2) Uani 0.280(3) 1 d D U P C 2
H25D H 0.758183 0.549437 0.441054 0.054 Uiso 0.280(3) 1 calc R U P C 2
H25E H 0.758704 0.527474 0.527075 0.054 Uiso 0.280(3) 1 calc R U P C 2
H25F H 0.853389 0.561670 0.503104 0.054 Uiso 0.280(3) 1 calc R U P C 2
C25" C 0.609(2) 0.6440(15) 0.6656(14) 0.029(4) Uani 0.170(2) 1 d D U P D 3
H25G H 0.599921 0.592360 0.645914 0.044 Uiso 0.170(2) 1 calc R U P D 3
H25H H 0.546126 0.665366 0.670269 0.044 Uiso 0.170(2) 1 calc R U P D 3
H25I H 0.650771 0.643234 0.715210 0.044 Uiso 0.170(2) 1 calc R U P D 3
N3 N 0.8976(3) 0.6065(2) 0.2484(2) 0.0194(7) Uani 1 1 d . . . . .
C9 C 0.9702(3) 0.5525(3) 0.2206(2) 0.0224(9) Uani 1 1 d . . . . .
H9A H 0.934809 0.522718 0.177922 0.027 Uiso 1 1 calc R U . . .
H9B H 1.018011 0.583817 0.200874 0.027 Uiso 1 1 calc R U . . .
C10 C 1.0253(3) 0.4965(3) 0.2792(3) 0.0263(9) Uani 1 1 d . . . . .
H10A H 0.979161 0.463930 0.299397 0.032 Uiso 1 1 calc R U . . .
H10B H 1.063657 0.524946 0.321611 0.032 Uiso 1 1 calc R U . . .
C11 C 1.0933(3) 0.4466(3) 0.2403(3) 0.0287(10) Uani 1 1 d . . . . .
H11A H 1.056225 0.425252 0.193049 0.034 Uiso 1 1 calc R U . . .
H11B H 1.145146 0.478663 0.227014 0.034 Uiso 1 1 calc R U . . .
C12 C 1.1381(5) 0.3818(4) 0.2918(4) 0.0542(17) Uani 1 1 d . . . . .
H12A H 1.170837 0.402631 0.340015 0.081 Uiso 1 1 calc R U . . .
H12B H 1.184654 0.354590 0.267670 0.081 Uiso 1 1 calc R U . . .
H12C H 1.087434 0.346942 0.300452 0.081 Uiso 1 1 calc R U . . .
C13 C 0.9496(3) 0.6635(3) 0.3080(2) 0.0239(9) Uani 1 1 d D . . . .
H13A H 0.985696 0.634723 0.351140 0.029 Uiso 0.830(2) 1 calc R U P E 1
H13B H 0.900413 0.694119 0.326956 0.029 Uiso 0.830(2) 1 calc R U P E 1
H13C H 0.898003 0.694541 0.323135 0.029 Uiso 0.170(2) 1 calc R U P E 2
H13D H 0.977039 0.632753 0.352614 0.029 Uiso 0.170(2) 1 calc R U P E 2
C14 C 1.0207(7) 0.7183(6) 0.2778(4) 0.0244(15) Uani 0.830(2) 1 d D U P E 1
H14A H 1.070742 0.688563 0.259063 0.029 Uiso 0.830(2) 1 calc R U P E 1
H14B H 0.985336 0.748446 0.235364 0.029 Uiso 0.830(2) 1 calc R U P E 1
C15 C 1.0691(5) 0.7724(4) 0.3422(4) 0.0284(13) Uani 0.830(2) 1 d D U P E 1
H15A H 1.018051 0.799310 0.362535 0.034 Uiso 0.830(2) 1 calc R U P E 1
H15B H 1.105894 0.741578 0.383427 0.034 Uiso 0.830(2) 1 calc R U P E 1
C16 C 1.1371(4) 0.8313(4) 0.3173(4) 0.0317(13) Uani 0.830(2) 1 d D U P E 1
H16A H 1.185028 0.805476 0.293534 0.048 Uiso 0.830(2) 1 calc R U P E 1
H16B H 1.169642 0.859561 0.361371 0.048 Uiso 0.830(2) 1 calc R U P E 1
H16C H 1.099822 0.866342 0.281183 0.048 Uiso 0.830(2) 1 calc R U P E 1
C14' C 1.030(4) 0.720(3) 0.297(2) 0.027(5) Uani 0.170(2) 1 d D U P E 2
H14C H 1.003416 0.759221 0.259584 0.033 Uiso 0.170(2) 1 calc R U P E 2
H14D H 1.082274 0.693242 0.278580 0.033 Uiso 0.170(2) 1 calc R U P E 2
C15' C 1.069(3) 0.7579(19) 0.3748(18) 0.036(5) Uani 0.170(2) 1 d D U P E 2
H15C H 1.014404 0.775998 0.397204 0.044 Uiso 0.170(2) 1 calc R U P E 2
H15D H 1.104771 0.719817 0.409225 0.044 Uiso 0.170(2) 1 calc R U P E 2
C16' C 1.136(2) 0.8249(18) 0.367(2) 0.045(6) Uani 0.170(2) 1 d D U P E 2
H16D H 1.199108 0.805772 0.360698 0.067 Uiso 0.170(2) 1 calc R U P E 2
H16E H 1.143425 0.856478 0.412244 0.067 Uiso 0.170(2) 1 calc R U P E 2
H16F H 1.108232 0.855232 0.322826 0.067 Uiso 0.170(2) 1 calc R U P E 2
C17 C 0.8435(3) 0.6475(3) 0.1774(2) 0.0230(9) Uani 1 1 d . . . . .
H17A H 0.890598 0.677535 0.155499 0.028 Uiso 1 1 calc R U . . .
H17B H 0.816343 0.608825 0.139815 0.028 Uiso 1 1 calc R U . . .
C18 C 0.7616(4) 0.7004(3) 0.1902(3) 0.0297(10) Uani 1 1 d D . . . .
H18A H 0.788442 0.741330 0.225291 0.036 Uiso 0.574(14) 1 calc R U P F 1
H18B H 0.715069 0.671499 0.213789 0.036 Uiso 0.574(14) 1 calc R U P F 1
H18C H 0.784468 0.733706 0.233904 0.036 Uiso 0.426(14) 1 calc R U P F 2
H18D H 0.707142 0.670026 0.201337 0.036 Uiso 0.426(14) 1 calc R U P F 2
C19 C 0.7086(15) 0.7358(17) 0.1156(12) 0.048(4) Uani 0.574(14) 1 d D U P F 1
H19A H 0.659437 0.771428 0.127373 0.057 Uiso 0.574(14) 1 calc R U P F 1
H19B H 0.755547 0.765574 0.093183 0.057 Uiso 0.574(14) 1 calc R U P F 1
C20 C 0.6593(7) 0.6791(8) 0.0567(6) 0.051(3) Uani 0.574(14) 1 d D . P F 1
H20A H 0.707571 0.655587 0.031489 0.076 Uiso 0.574(14) 1 calc R U P F 1
H20B H 0.611645 0.705582 0.019376 0.076 Uiso 0.574(14) 1 calc R U P F 1
H20C H 0.627279 0.639988 0.081508 0.076 Uiso 0.574(14) 1 calc R U P F 1
C19' C 0.727(2) 0.749(2) 0.1189(16) 0.046(5) Uani 0.426(14) 1 d D U P F 2
H19C H 0.782486 0.779799 0.108717 0.055 Uiso 0.426(14) 1 calc R U P F 2
H19D H 0.707353 0.715363 0.075264 0.055 Uiso 0.426(14) 1 calc R U P F 2
C20' C 0.6435(10) 0.8033(8) 0.1252(10) 0.047(4) Uani 0.426(14) 1 d D . P F 2
H20D H 0.586323 0.773510 0.129681 0.071 Uiso 0.426(14) 1 calc R U P F 2
H20E H 0.629472 0.835163 0.080171 0.071 Uiso 0.426(14) 1 calc R U P F 2
H20F H 0.661255 0.835313 0.169904 0.071 Uiso 0.426(14) 1 calc R U P F 2
C21 C 0.8277(3) 0.5628(3) 0.2896(3) 0.0232(9) Uani 1 1 d D . . . .
H21A H 0.783545 0.599452 0.307067 0.028 Uiso 0.77(4) 1 calc R U P G 1
H21B H 0.865206 0.537820 0.334659 0.028 Uiso 0.77(4) 1 calc R U P G 1
H21C H 0.868370 0.540050 0.334547 0.028 Uiso 0.23(4) 1 calc R U P G 2
H21D H 0.788305 0.602024 0.308756 0.028 Uiso 0.23(4) 1 calc R U P G 2
C22 C 0.7667(9) 0.5017(7) 0.2394(7) 0.0235(17) Uani 0.77(4) 1 d D U P G 1
H22A H 0.809501 0.463769 0.222407 0.028 Uiso 0.77(4) 1 calc R U P G 1
H22B H 0.727641 0.525758 0.194455 0.028 Uiso 0.77(4) 1 calc R U P G 1
C23 C 0.6994(8) 0.4625(7) 0.2878(9) 0.041(3) Uani 0.77(4) 1 d D U P G 1
H23A H 0.739310 0.439811 0.333188 0.049 Uiso 0.77(4) 1 calc R U P G 1
H23B H 0.657388 0.501174 0.304781 0.049 Uiso 0.77(4) 1 calc R U P G 1
C24 C 0.6370(8) 0.4011(6) 0.2438(11) 0.051(4) Uani 0.77(4) 1 d D U P G 1
H24A H 0.585037 0.424714 0.207923 0.077 Uiso 0.77(4) 1 calc R U P G 1
H24B H 0.609550 0.369190 0.278850 0.077 Uiso 0.77(4) 1 calc R U P G 1
H24C H 0.676520 0.369984 0.216472 0.077 Uiso 0.77(4) 1 calc R U P G 1
C22' C 0.756(3) 0.500(2) 0.256(2) 0.024(4) Uani 0.23(4) 1 d D U P G 2
H22C H 0.792178 0.456553 0.240554 0.029 Uiso 0.23(4) 1 calc R U P G 2
H22D H 0.712955 0.519595 0.210591 0.029 Uiso 0.23(4) 1 calc R U P G 2
C23' C 0.694(3) 0.473(2) 0.314(3) 0.042(5) Uani 0.23(4) 1 d D U P G 2
H23C H 0.736678 0.448721 0.357911 0.050 Uiso 0.23(4) 1 calc R U P G 2
H23D H 0.662412 0.516643 0.333251 0.050 Uiso 0.23(4) 1 calc R U P G 2
C24' C 0.618(3) 0.416(3) 0.278(4) 0.058(8) Uani 0.23(4) 1 d D U P G 2
H24D H 0.568040 0.442342 0.243142 0.087 Uiso 0.23(4) 1 calc R U P G 2
H24E H 0.590127 0.390892 0.317220 0.087 Uiso 0.23(4) 1 calc R U P G 2
H24F H 0.648568 0.377806 0.250417 0.087 Uiso 0.23(4) 1 calc R U P G 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.594(4) . ?
V1 O7 1.998(4) . ?
V1 O8 2.017(3) . ?
V1 O9 1.829(3) . ?
V1 O10 1.836(4) . ?
V1 O19 2.244(3) . ?
V2 O2 1.594(3) . ?
V2 O7 2.015(4) . ?
V2 O11 2.005(3) . ?
V2 O14 1.838(3) . ?
V2 O15 1.826(4) . ?
V2 O19 2.235(3) . ?
V3 O3 1.591(3) . ?
V3 O8 1.981(3) . ?
V3 O11 2.018(3) . ?
V3 O12 1.798(3) . ?
V3 O16 1.889(3) . ?
V3 O19 2.240(3) . ?
V4 O4 1.604(3) . ?
V4 O9 1.821(3) . ?
V4 O12 1.847(3) . ?
V4 O13 1.998(3) . ?
V4 O17 2.005(3) . ?
V4 O19 2.227(3) . ?
V5 O5 1.593(3) . ?
V5 O10 1.877(4) . ?
V5 O13 2.012(3) . ?
V5 O14 1.793(3) . ?
V5 O18 1.990(4) . ?
V5 O19 2.244(3) . ?
V6 O6 1.599(4) . ?
V6 O15 1.799(3) . ?
V6 O16 1.869(3) . ?
V6 O17 2.023(3) . ?
V6 O18 1.993(3) . ?
V6 O19 2.225(3) . ?
O7 C1 1.434(5) . ?
O8 C2 1.434(5) . ?
O9 C25" 1.432(11) . ?
O10 C25' 1.416(10) . ?
O11 C3 1.419(5) . ?
O13 C7 1.431(5) . ?
O16 C25 1.459(9) . ?
O17 C5 1.427(5) . ?
O18 C6 1.432(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.526(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.532(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.540(6) . ?
C4 N1 1.518(5) . ?
N1 O20 1.221(6) . ?
N1 O21 1.214(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C8 1.538(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C8 1.537(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.533(6) . ?
C8 N2 1.523(6) . ?
C8 N2' 1.532(10) . ?
N2 O22 1.212(6) . ?
N2 O23 1.208(6) . ?
N2' O22' 1.220(9) . ?
N2' O23' 1.218(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25' H25D 0.9600 . ?
C25' H25E 0.9600 . ?
C25' H25F 0.9600 . ?
C25" H25G 0.9600 . ?
C25" H25H 0.9600 . ?
C25" H25I 0.9600 . ?
N3 C9 1.519(5) . ?
N3 C13 1.525(5) . ?
N3 C17 1.516(6) . ?
N3 C21 1.518(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.519(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.532(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.506(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C13 C14 1.534(7) . ?
C13 C14' 1.522(18) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.530(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.508(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C14' H14C 0.9700 . ?
C14' H14D 0.9700 . ?
C14' C15' 1.53(2) . ?
C15' H15C 0.9700 . ?
C15' H15D 0.9700 . ?
C15' C16' 1.51(2) . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.507(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 C19 1.516(11) . ?
C18 C19' 1.521(15) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.50(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20' 1.51(4) . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C21 C22 1.532(8) . ?
C21 C22' 1.518(17) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.535(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.496(10) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?
C22' C23' 1.53(2) . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C23' C24' 1.50(2) . ?
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
O1 V1 O7 96.9(2) . . ?
O1 V1 O8 97.04(19) . . ?
O1 V1 O9 104.6(2) . . ?
O1 V1 O10 102.7(2) . . ?
O1 V1 O19 172.85(16) . . ?
O7 V1 O8 82.54(13) . . ?
O7 V1 O19 77.30(12) . . ?
O8 V1 O19 78.15(11) . . ?
O9 V1 O7 157.19(14) . . ?
O9 V1 O8 87.46(14) . . ?
O9 V1 O10 93.99(15) . . ?
O9 V1 O19 80.61(12) . . ?
O10 V1 O7 88.36(16) . . ?
O10 V1 O8 159.13(16) . . ?
O10 V1 O19 81.55(14) . . ?
O2 V2 O7 96.6(2) . . ?
O2 V2 O11 96.43(15) . . ?
O2 V2 O14 104.77(17) . . ?
O2 V2 O15 103.9(2) . . ?
O2 V2 O19 171.58(16) . . ?
O7 V2 O19 77.18(12) . . ?
O11 V2 O7 82.32(13) . . ?
O11 V2 O19 77.21(10) . . ?
O14 V2 O7 87.79(17) . . ?
O14 V2 O11 157.51(14) . . ?
O14 V2 O19 80.93(12) . . ?
O15 V2 O7 158.53(14) . . ?
O15 V2 O11 89.18(14) . . ?
O15 V2 O14 92.88(18) . . ?
O15 V2 O19 81.73(12) . . ?
O3 V3 O8 97.62(16) . . ?
O3 V3 O11 96.69(15) . . ?
O3 V3 O12 104.32(16) . . ?
O3 V3 O16 102.32(17) . . ?
O3 V3 O19 172.94(14) . . ?
O8 V3 O11 83.01(12) . . ?
O8 V3 O19 78.97(11) . . ?
O11 V3 O19 76.83(11) . . ?
O12 V3 O8 90.80(14) . . ?
O12 V3 O11 158.73(13) . . ?
O12 V3 O16 93.44(15) . . ?
O12 V3 O19 82.02(12) . . ?
O16 V3 O8 157.87(14) . . ?
O16 V3 O11 85.24(13) . . ?
O16 V3 O19 80.13(12) . . ?
O4 V4 O9 104.09(17) . . ?
O4 V4 O12 104.34(15) . . ?
O4 V4 O13 96.41(14) . . ?
O4 V4 O17 96.69(16) . . ?
O4 V4 O19 171.86(13) . . ?
O9 V4 O12 92.39(14) . . ?
O9 V4 O13 89.63(13) . . ?
O9 V4 O17 158.46(13) . . ?
O9 V4 O19 81.23(12) . . ?
O12 V4 O13 157.97(12) . . ?
O12 V4 O17 87.87(13) . . ?
O12 V4 O19 81.34(11) . . ?
O13 V4 O17 82.37(12) . . ?
O13 V4 O19 77.29(10) . . ?
O17 V4 O19 77.51(11) . . ?
O5 V5 O10 102.8(2) . . ?
O5 V5 O13 96.22(15) . . ?
O5 V5 O14 105.24(17) . . ?
O5 V5 O18 96.9(2) . . ?
O5 V5 O19 171.97(15) . . ?
O10 V5 O13 86.90(14) . . ?
O10 V5 O18 158.48(14) . . ?
O10 V5 O19 80.67(12) . . ?
O13 V5 O19 76.61(10) . . ?
O14 V5 O10 93.59(18) . . ?
O14 V5 O13 157.83(14) . . ?
O14 V5 O18 89.54(17) . . ?
O14 V5 O19 81.59(13) . . ?
O18 V5 O13 82.33(12) . . ?
O18 V5 O19 78.73(11) . . ?
O6 V6 O15 105.66(19) . . ?
O6 V6 O16 102.11(19) . . ?
O6 V6 O17 94.26(17) . . ?
O6 V6 O18 96.72(18) . . ?
O6 V6 O19 170.85(15) . . ?
O15 V6 O16 93.39(15) . . ?
O15 V6 O17 159.49(15) . . ?
O15 V6 O18 89.56(15) . . ?
O15 V6 O19 82.60(14) . . ?
O16 V6 O17 87.00(13) . . ?
O16 V6 O18 159.37(14) . . ?
O16 V6 O19 80.99(12) . . ?
O17 V6 O19 77.21(11) . . ?
O18 V6 O17 83.22(12) . . ?
O18 V6 O19 79.15(12) . . ?
V1 O7 V2 110.34(14) . . ?
C1 O7 V1 119.9(4) . . ?
C1 O7 V2 117.7(3) . . ?
V3 O8 V1 109.07(13) . . ?
C2 O8 V1 119.0(3) . . ?
C2 O8 V3 119.4(3) . . ?
V4 O9 V1 112.58(15) . . ?
C25" O9 V1 106.3(12) . . ?
C25" O9 V4 133.9(13) . . ?
V1 O10 V5 111.47(17) . . ?
C25' O10 V1 113.7(8) . . ?
C25' O10 V5 128.5(9) . . ?
V2 O11 V3 110.45(13) . . ?
C3 O11 V2 119.1(3) . . ?
C3 O11 V3 117.8(2) . . ?
V3 O12 V4 111.68(15) . . ?
V4 O13 V5 110.61(12) . . ?
C7 O13 V4 118.7(2) . . ?
C7 O13 V5 118.9(2) . . ?
V5 O14 V2 112.62(17) . . ?
V6 O15 V2 111.32(17) . . ?
V6 O16 V3 111.02(15) . . ?
C25 O16 V3 115.3(5) . . ?
C25 O16 V6 122.3(6) . . ?
V4 O17 V6 109.62(13) . . ?
C5 O17 V4 118.8(3) . . ?
C5 O17 V6 118.8(3) . . ?
V5 O18 V6 108.59(14) . . ?
C6 O18 V5 120.6(3) . . ?
C6 O18 V6 118.7(3) . . ?
V1 O19 V5 86.29(10) . . ?
V2 O19 V1 94.71(11) . . ?
V2 O19 V3 95.20(10) . . ?
V2 O19 V5 84.84(9) . . ?
V3 O19 V1 93.14(10) . . ?
V3 O19 V5 179.43(15) . . ?
V4 O19 V1 85.55(10) . . ?
V4 O19 V2 179.71(15) . . ?
V4 O19 V3 84.92(9) . . ?
V4 O19 V5 95.04(10) . . ?
V6 O19 V1 178.70(14) . . ?
V6 O19 V2 84.34(9) . . ?
V6 O19 V3 87.84(10) . . ?
V6 O19 V4 95.39(11) . . ?
V6 O19 V5 92.73(10) . . ?
O7 C1 H1A 109.8 . . ?
O7 C1 H1B 109.8 . . ?
O7 C1 C4 109.5(4) . . ?
H1A C1 H1B 108.2 . . ?
C4 C1 H1A 109.8 . . ?
C4 C1 H1B 109.8 . . ?
O8 C2 H2A 109.7 . . ?
O8 C2 H2B 109.7 . . ?
O8 C2 C4 109.6(4) . . ?
H2A C2 H2B 108.2 . . ?
C4 C2 H2A 109.7 . . ?
C4 C2 H2B 109.7 . . ?
O11 C3 H3A 109.7 . . ?
O11 C3 H3B 109.7 . . ?
O11 C3 C4 109.9(3) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C1 C4 C2 112.3(4) . . ?
C1 C4 C3 112.1(4) . . ?
C2 C4 C3 110.7(4) . . ?
N1 C4 C1 108.1(4) . . ?
N1 C4 C2 108.1(4) . . ?
N1 C4 C3 105.2(3) . . ?
O20 N1 C4 118.3(4) . . ?
O21 N1 C4 117.6(4) . . ?
O21 N1 O20 124.0(4) . . ?
O17 C5 H5A 109.9 . . ?
O17 C5 H5B 109.9 . . ?
O17 C5 C8 108.7(4) . . ?
H5A C5 H5B 108.3 . . ?
C8 C5 H5A 109.9 . . ?
C8 C5 H5B 109.9 . . ?
O18 C6 H6A 109.9 . . ?
O18 C6 H6B 109.9 . . ?
O18 C6 C8 108.9(3) . . ?
H6A C6 H6B 108.3 . . ?
C8 C6 H6A 109.9 . . ?
C8 C6 H6B 109.9 . . ?
O13 C7 H7A 109.9 . . ?
O13 C7 H7B 109.9 . . ?
O13 C7 C8 109.0(3) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
C6 C8 C5 112.4(4) . . ?
C7 C8 C5 112.2(4) . . ?
C7 C8 C6 111.8(4) . . ?
N2 C8 C5 103.8(4) . . ?
N2 C8 C6 106.4(4) . . ?
N2 C8 C7 109.7(4) . . ?
N2' C8 C5 112.6(9) . . ?
N2' C8 C6 107.5(10) . . ?
N2' C8 C7 99.5(13) . . ?
O22 N2 C8 119.2(5) . . ?
O23 N2 C8 118.6(5) . . ?
O23 N2 O22 121.9(6) . . ?
O22' N2' C8 113.3(15) . . ?
O23' N2' C8 118.5(14) . . ?
O23' N2' O22' 119.7(17) . . ?
O16 C25 H25A 109.5 . . ?
O16 C25 H25B 109.5 . . ?
O16 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C25' H25D 109.5 . . ?
O10 C25' H25E 109.5 . . ?
O10 C25' H25F 109.5 . . ?
H25D C25' H25E 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
O9 C25" H25G 109.5 . . ?
O9 C25" H25H 109.5 . . ?
O9 C25" H25I 109.5 . . ?
H25G C25" H25H 109.5 . . ?
H25G C25" H25I 109.5 . . ?
H25H C25" H25I 109.5 . . ?
C9 N3 C13 111.5(3) . . ?
C17 N3 C9 106.0(3) . . ?
C17 N3 C13 111.6(3) . . ?
C17 N3 C21 111.6(3) . . ?
C21 N3 C9 111.6(3) . . ?
C21 N3 C13 104.6(3) . . ?
N3 C9 H9A 108.1 . . ?
N3 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C10 C9 N3 116.9(3) . . ?
C10 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C9 C10 C11 109.1(4) . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.6(4) . . ?
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 . . ?
N3 C13 H13A 108.7 . . ?
N3 C13 H13B 108.7 . . ?
N3 C13 H13C 105.7 . . ?
N3 C13 H13D 105.7 . . ?
N3 C13 C14 114.3(4) . . ?
H13A C13 H13B 107.6 . . ?
H13C C13 H13D 106.2 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C14' C13 N3 126.3(12) . . ?
C14' C13 H13C 105.7 . . ?
C14' C13 H13D 105.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 C13 109.9(5) . . ?
C15 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C14 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 C14 114.1(5) . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
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 . . ?
C13 C14' H14C 110.1 . . ?
C13 C14' H14D 110.1 . . ?
C13 C14' C15' 108.0(19) . . ?
H14C C14' H14D 108.4 . . ?
C15' C14' H14C 110.1 . . ?
C15' C14' H14D 110.1 . . ?
C14' C15' H15C 109.3 . . ?
C14' C15' H15D 109.3 . . ?
H15C C15' H15D 107.9 . . ?
C16' C15' C14' 112(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 . . ?
N3 C17 H17A 108.4 . . ?
N3 C17 H17B 108.4 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N3 115.6(3) . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
C17 C18 H18C 109.7 . . ?
C17 C18 H18D 109.7 . . ?
C17 C18 C19 111.9(13) . . ?
C17 C18 C19' 110.0(16) . . ?
H18A C18 H18B 107.9 . . ?
H18C C18 H18D 108.2 . . ?
C19 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C19' C18 H18C 109.7 . . ?
C19' C18 H18D 109.7 . . ?
C18 C19 H19A 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 C18 115.2(18) . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
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 . . ?
C18 C19' H19C 108.7 . . ?
C18 C19' H19D 108.7 . . ?
H19C C19' H19D 107.6 . . ?
C20' C19' C18 114(2) . . ?
C20' C19' H19C 108.7 . . ?
C20' C19' H19D 108.7 . . ?
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 . . ?
N3 C21 H21A 108.9 . . ?
N3 C21 H21B 108.9 . . ?
N3 C21 H21C 105.6 . . ?
N3 C21 H21D 105.6 . . ?
N3 C21 C22 113.5(6) . . ?
H21A C21 H21B 107.7 . . ?
H21C C21 H21D 106.1 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C22' C21 N3 126.7(15) . . ?
C22' C21 H21C 105.6 . . ?
C22' C21 H21D 105.6 . . ?
C21 C22 H22A 110.1 . . ?
C21 C22 H22B 110.1 . . ?
C21 C22 C23 108.0(6) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.1 . . ?
C23 C22 H22B 110.1 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 C22 112.1(8) . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
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 . . ?
C21 C22' H22C 109.4 . . ?
C21 C22' H22D 109.4 . . ?
C21 C22' C23' 111(2) . . ?
H22C C22' H22D 108.0 . . ?
C23' C22' H22C 109.4 . . ?
C23' C22' H22D 109.4 . . ?
C22' C23' H23C 109.6 . . ?
C22' C23' H23D 109.6 . . ?
H23C C23' H23D 108.1 . . ?
C24' C23' C22' 110(2) . . ?
C24' C23' H23C 109.6 . . ?
C24' C23' H23D 109.6 . . ?
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 C4 68.5(5) . . . . ?
V1 O8 C2 C4 -68.4(4) . . . . ?
V2 O7 C1 C4 -70.4(5) . . . . ?
V2 O11 C3 C4 68.5(4) . . . . ?
V3 O8 C2 C4 69.3(4) . . . . ?
V3 O11 C3 C4 -69.8(4) . . . . ?
V4 O13 C7 C8 -69.8(4) . . . . ?
V4 O17 C5 C8 69.6(4) . . . . ?
V5 O13 C7 C8 69.8(4) . . . . ?
V5 O18 C6 C8 -68.5(5) . . . . ?
V6 O17 C5 C8 -68.1(4) . . . . ?
V6 O18 C6 C8 69.7(5) . . . . ?
O1 V1 O9 V4 -176.4(2) . . . . ?
O1 V1 O9 C25" -21.8(13) . . . . ?
O1 V1 O10 V5 173.0(2) . . . . ?
O1 V1 O10 C25' 18.4(10) . . . . ?
O2 V2 O14 V5 -174.8(3) . . . . ?
O2 V2 O15 V6 173.83(19) . . . . ?
O3 V3 O12 V4 175.13(19) . . . . ?
O3 V3 O16 V6 -174.05(17) . . . . ?
O3 V3 O16 C25 41.5(6) . . . . ?
O4 V4 O9 V1 -172.35(17) . . . . ?
O4 V4 O9 C25" 42.6(16) . . . . ?
O4 V4 O12 V3 175.75(18) . . . . ?
O5 V5 O10 V1 173.75(19) . . . . ?
O5 V5 O10 C25' -36.4(10) . . . . ?
O5 V5 O14 V2 -174.6(3) . . . . ?
O6 V6 O15 V2 175.8(2) . . . . ?
O6 V6 O16 V3 -170.43(19) . . . . ?
O6 V6 O16 C25 -28.8(6) . . . . ?
O7 V1 O9 V4 -15.9(5) . . . . ?
O7 V1 O9 C25" 138.7(13) . . . . ?
O7 V1 O10 V5 76.27(19) . . . . ?
O7 V1 O10 C25' -78.3(10) . . . . ?
O7 V2 O14 V5 -78.5(2) . . . . ?
O7 V2 O15 V6 11.1(5) . . . . ?
O7 C1 C4 C2 -62.4(6) . . . . ?
O7 C1 C4 C3 62.9(5) . . . . ?
O7 C1 C4 N1 178.5(4) . . . . ?
O8 V1 O9 V4 -79.77(17) . . . . ?
O8 V1 O9 C25" 74.8(13) . . . . ?
O8 V1 O10 V5 12.3(5) . . . . ?
O8 V1 O10 C25' -142.2(10) . . . . ?
O8 V3 O12 V4 77.05(18) . . . . ?
O8 V3 O16 V6 -20.2(4) . . . . ?
O8 V3 O16 C25 -164.7(6) . . . . ?
O8 C2 C4 C1 63.0(5) . . . . ?
O8 C2 C4 C3 -63.2(5) . . . . ?
O8 C2 C4 N1 -177.9(4) . . . . ?
O9 V1 O10 V5 -81.01(19) . . . . ?
O9 V1 O10 C25' 124.4(10) . . . . ?
O9 V4 O12 V3 -79.05(19) . . . . ?
O10 V1 O9 V4 79.4(2) . . . . ?
O10 V1 O9 C25" -126.1(13) . . . . ?
O10 V5 O14 V2 81.1(2) . . . . ?
O11 V2 O14 V5 -14.8(6) . . . . ?
O11 V2 O15 V6 77.41(18) . . . . ?
O11 V3 O12 V4 4.5(5) . . . . ?
O11 V3 O16 V6 -78.23(16) . . . . ?
O11 V3 O16 C25 137.3(6) . . . . ?
O11 C3 C4 C1 -61.7(5) . . . . ?
O11 C3 C4 C2 64.6(4) . . . . ?
O11 C3 C4 N1 -178.9(4) . . . . ?
O12 V3 O16 V6 80.48(17) . . . . ?
O12 V3 O16 C25 -64.0(6) . . . . ?
O12 V4 O9 V1 82.23(18) . . . . ?
O12 V4 O9 C25" -62.9(16) . . . . ?
O13 V4 O9 V1 -75.83(17) . . . . ?
O13 V4 O9 C25" 139.1(16) . . . . ?
O13 V4 O12 V3 15.9(5) . . . . ?
O13 V5 O10 V1 78.07(19) . . . . ?
O13 V5 O10 C25' -132.1(10) . . . . ?
O13 V5 O14 V2 -9.5(6) . . . . ?
O13 C7 C8 C5 63.2(4) . . . . ?
O13 C7 C8 C6 -64.2(4) . . . . ?
O13 C7 C8 N2 178.0(4) . . . . ?
O13 C7 C8 N2' -177.5(8) . . . . ?
O14 V2 O15 V6 -80.2(2) . . . . ?
O14 V5 O10 V1 -79.7(2) . . . . ?
O14 V5 O10 C25' 70.1(10) . . . . ?
O15 V2 O14 V5 80.0(2) . . . . ?
O15 V6 O16 V3 82.75(19) . . . . ?
O15 V6 O16 C25 -135.7(5) . . . . ?
O16 V3 O12 V4 -81.22(18) . . . . ?
O16 V6 O15 V2 -80.67(19) . . . . ?
O17 V4 O9 V1 -8.0(5) . . . . ?
O17 V4 O9 C25" -153.1(16) . . . . ?
O17 V4 O12 V3 79.39(18) . . . . ?
O17 V6 O15 V2 9.8(5) . . . . ?
O17 V6 O16 V3 -76.71(17) . . . . ?
O17 V6 O16 C25 64.9(5) . . . . ?
O17 C5 C8 C6 64.0(5) . . . . ?
O17 C5 C8 C7 -63.1(5) . . . . ?
O17 C5 C8 N2 178.5(4) . . . . ?
O17 C5 C8 N2' -174.4(13) . . . . ?
O18 V5 O10 V1 18.2(5) . . . . ?
O18 V5 O10 C25' 168.0(10) . . . . ?
O18 V5 O14 V2 -77.5(2) . . . . ?
O18 V6 O15 V2 78.90(19) . . . . ?
O18 V6 O16 V3 -15.0(5) . . . . ?
O18 V6 O16 C25 126.5(6) . . . . ?
O18 C6 C8 C5 -64.6(5) . . . . ?
O18 C6 C8 C7 62.7(5) . . . . ?
O18 C6 C8 N2 -177.5(4) . . . . ?
O18 C6 C8 N2' 170.9(12) . . . . ?
O19 V1 O9 V4 -1.36(15) . . . . ?
O19 V1 O9 C25" 153.2(13) . . . . ?
O19 V1 O10 V5 -1.13(17) . . . . ?
O19 V1 O10 C25' -155.7(10) . . . . ?
O19 V2 O14 V5 -1.1(2) . . . . ?
O19 V2 O15 V6 0.22(17) . . . . ?
O19 V3 O12 V4 -1.69(16) . . . . ?
O19 V3 O16 V6 -0.80(15) . . . . ?
O19 V3 O16 C25 -145.3(6) . . . . ?
O19 V4 O9 V1 1.37(15) . . . . ?
O19 V4 O9 C25" -143.7(16) . . . . ?
O19 V4 O12 V3 1.70(16) . . . . ?
O19 V5 O10 V1 1.14(17) . . . . ?
O19 V5 O10 C25' 151.0(10) . . . . ?
O19 V5 O14 V2 1.1(2) . . . . ?
O19 V6 O15 V2 -0.22(17) . . . . ?
O19 V6 O16 V3 0.80(15) . . . . ?
O19 V6 O16 C25 142.4(5) . . . . ?
C1 C4 N1 O20 -21.6(6) . . . . ?
C1 C4 N1 O21 161.0(5) . . . . ?
C2 C4 N1 O20 -143.4(5) . . . . ?
C2 C4 N1 O21 39.2(6) . . . . ?
C3 C4 N1 O20 98.3(5) . . . . ?
C3 C4 N1 O21 -79.1(6) . . . . ?
C5 C8 N2 O22 -62.4(7) . . . . ?
C5 C8 N2 O23 111.6(9) . . . . ?
C5 C8 N2' O22' 39(3) . . . . ?
C5 C8 N2' O23' -173(2) . . . . ?
C6 C8 N2 O22 56.3(8) . . . . ?
C6 C8 N2 O23 -129.6(8) . . . . ?
C6 C8 N2' O22' 164(2) . . . . ?
C6 C8 N2' O23' -48(3) . . . . ?
C7 C8 N2 O22 177.5(6) . . . . ?
C7 C8 N2 O23 -8.5(10) . . . . ?
C7 C8 N2' O22' -80(3) . . . . ?
C7 C8 N2' O23' 68(3) . . . . ?
N3 C9 C10 C11 179.2(4) . . . . ?
N3 C13 C14 C15 -179.6(6) . . . . ?
N3 C13 C14' C15' -173(2) . . . . ?
N3 C17 C18 C19 -177.3(11) . . . . ?
N3 C17 C18 C19' 168.8(14) . . . . ?
N3 C21 C22 C23 -179.8(7) . . . . ?
N3 C21 C22' C23' -177(2) . . . . ?
C9 N3 C13 C14 62.7(7) . . . . ?
C9 N3 C13 C14' 57(4) . . . . ?
C9 N3 C17 C18 175.7(4) . . . . ?
C9 N3 C21 C22 -59.5(8) . . . . ?
C9 N3 C21 C22' -61(3) . . . . ?
C9 C10 C11 C12 -171.1(5) . . . . ?
C13 N3 C9 C10 66.0(5) . . . . ?
C13 N3 C17 C18 -62.7(5) . . . . ?
C13 N3 C21 C22 179.8(7) . . . . ?
C13 N3 C21 C22' 179(3) . . . . ?
C13 C14 C15 C16 -177.3(7) . . . . ?
C13 C14' C15' C16' -170(4) . . . . ?
C17 N3 C9 C10 -172.4(4) . . . . ?
C17 N3 C13 C14 -55.7(7) . . . . ?
C17 N3 C13 C14' -61(4) . . . . ?
C17 N3 C21 C22 58.9(8) . . . . ?
C17 N3 C21 C22' 58(3) . . . . ?
C17 C18 C19 C20 61.5(17) . . . . ?
C17 C18 C19' C20' 178.6(17) . . . . ?
C21 N3 C9 C10 -50.6(5) . . . . ?
C21 N3 C13 C14 -176.5(6) . . . . ?
C21 N3 C13 C14' 178(4) . . . . ?
C21 N3 C17 C18 53.9(5) . . . . ?
C21 C22 C23 C24 -179.6(10) . . . . ?
C21 C22' C23' C24' 175(4) . . . . ?

_olex2_submission_original_sample_id mataf22
_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 3.942
_oxdiff_exptl_absorpt_empirical_full_min 0.556
####################################################################### 
# 
# 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_mataf27
_database_code_depnum_ccdc_archive 'CCDC 2053154'
loop_
_audit_author_name
_audit_author_address
'William W. Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_vrf_PLAT301_mataf27             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 3% 
RESPONSE: The methoxy ligand is modeled as disordered over
two positions (0.50:0.50, due to symmetry).
;

_vrf_PLAT302_mataf27             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 100% 
RESPONSE: The tetrabutylphosphonium cation is modeled as disordered
over a crystallographic two-fold axis (0.50:0.50).
;

_vrf_PLAT860_mataf27             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 108 
RESPONSE: Analogous bond lengths and angles in the cation were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained toward the expected motion
relative to bond direction.
;

_audit_creation_date             2020-11-12
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H21 O19 V6, C16 H36 P'
_chemical_formula_sum            'C27 H57 O19 P V6'
_chemical_formula_weight         1022.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.0905(4)
_cell_length_b                   16.6569(5)
_cell_length_c                   18.2558(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.394(3)
_cell_angle_gamma                90
_cell_volume                     3977.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11892
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4690
_cell_measurement_theta_min      4.3150
_shelx_estimated_absorpt_T_max   0.594
_shelx_estimated_absorpt_T_min   0.265
_exptl_absorpt_coefficient_mu    12.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red-orange
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.047
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23900
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.983
_diffrn_reflns_theta_min         4.298
_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 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  22.00   0.50    3.81    --  -49.62  33.00 -62.00   86
  2  ω    -42.00 -12.00   0.50   15.25    --  -84.25  45.00  30.00   60
  3  ω    -42.00 -12.00   0.50   15.25    --  -84.25  45.00  90.00   60
  4  ω    -42.00 -12.00   0.50   15.25    --  -84.25  45.00 120.00   60
  5  ω    -75.00 -12.00   0.50   15.25    --  -84.25  61.00 -60.00  126
  6  ω   -121.00 -42.00   0.50    3.81    --  -49.62 -33.00 139.00  158
  7  ω   -121.00 -29.00   0.50    3.81    --  -49.62 -77.00 120.00  184
  8  ω     43.00 122.00   0.50    3.81    --   49.62  33.00 -62.00  158
  9  ω     98.00 178.00   0.50   15.25    --  105.75  33.00 -62.00  160
 10  ω     98.00 164.00   0.50   15.25    --  105.75  15.00  60.00  132
 11  ω     92.00 178.00   0.50   15.25    --  105.75 125.00-180.00  172
 12  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00-150.00  106
 13  ω     34.00 109.00   0.50   15.25    --  105.75 -94.00 -90.00  150
 14  ω     34.00 109.00   0.50   15.25    --  105.75 -94.00 -30.00  150
 15  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00 120.00  106
 16  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00 150.00  106
 17  ω     34.00 109.00   0.50   15.25    --  105.75 -94.00  90.00  150
 18  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00  90.00  106
 19  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00   0.00  106
 20  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00 -60.00  106
 21  ω     34.00  87.00   0.50   15.25    --  105.75 -61.00-180.00  106
 22  ω     29.00 122.00   0.50    3.81    --   49.62  77.00   0.00  186
 23  ω    -22.00  33.00   0.50    3.81    --   49.62 -33.00 139.00  110
 24  ω    -23.00   5.00   0.50    3.81    --   49.62 -19.00   0.00   56
 25  ω    -23.00   5.00   0.50    3.81    --   49.62 -19.00 -30.00   56
 26  ω   -121.00 -42.00   0.50    3.81    --  -49.62 -38.00-120.00  158
 27  ω   -156.00 -76.00   0.50   15.25    --  -84.25 -33.00 139.00  160
;
_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      -0.1096821000
_diffrn_orient_matrix_UB_12      -0.0310211000
_diffrn_orient_matrix_UB_13      -0.0154536000
_diffrn_orient_matrix_UB_21      0.0283497000
_diffrn_orient_matrix_UB_22      -0.0247212000
_diffrn_orient_matrix_UB_23      -0.0778530000
_diffrn_orient_matrix_UB_31      0.0323986000
_diffrn_orient_matrix_UB_32      -0.0835578000
_diffrn_orient_matrix_UB_33      0.0287774000
_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                3412
_reflns_number_total             4147
_reflns_odcompleteness_completeness 99.15
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.110
_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)+(0.0913P)²+1.6444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1444
_refine_special_details          
;
The methoxy ligand is modeled as disordered over two positions
(0.50:0.50, due to symmetry). The tetrabutylphosphonium cation
is modeled as disordered over a crystallographic two-fold axis
(0.50:0.50). Analogous bond lengths and angles in the cation were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained toward the expected motion
relative to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
C13 \\sim C22: within 8A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 8A
3. Rigid body (RIGU) restrains
 C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{P1, C15, C16, C17, C18} sigma for 1-2: 0.02, 1-3: 0.04
{P1, C11, C12, C13, C14} sigma for 1-2: 0.02, 1-3: 0.04
{P1, C19, C20, C21, C22} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1, C7, C8, C9, C10}
5. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) P1(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5)
 H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   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 0.83866(5) 0.35088(4) 0.45104(3) 0.05422(19) Uani 1 1 d . . . . .
V2 V 0.88757(4) 0.18164(3) 0.53869(3) 0.05070(18) Uani 1 1 d . . . . .
V3 V 0.73323(5) 0.31672(3) 0.60593(3) 0.04969(18) Uani 1 1 d . . . . .
O1 O 0.9123(2) 0.42042(16) 0.42413(14) 0.0658(7) Uani 1 1 d . . . . .
O2 O 0.9920(2) 0.14370(14) 0.57183(13) 0.0598(6) Uani 1 1 d . . . . .
O3 O 0.7360(2) 0.36188(15) 0.68320(13) 0.0622(6) Uani 1 1 d . . . . .
O4 O 0.94923(17) 0.28163(14) 0.49768(12) 0.0533(5) Uani 1 1 d . . . . .
O5 O 0.82528(18) 0.39007(13) 0.55325(12) 0.0530(5) Uani 1 1 d . . . . .
O6 O 0.71102(19) 0.38559(13) 0.42824(12) 0.0563(6) Uani 1 1 d . . . . .
O7 O 0.83818(19) 0.27932(15) 0.37129(12) 0.0571(5) Uani 1 1 d . . . . .
O8 O 0.86289(17) 0.25324(13) 0.62391(12) 0.0510(5) Uani 1 1 d . . . . .
O9 O 0.62464(19) 0.35795(14) 0.55614(13) 0.0567(6) Uani 1 1 d . . . . .
O10 O 0.750000 0.250000 0.500000 0.0478(7) Uani 1 2 d S . P . .
C1 C 1.0309(3) 0.3203(2) 0.5393(2) 0.0585(8) Uani 1 1 d . . . . .
H1A H 1.060451 0.361851 0.509636 0.070 Uiso 1 1 calc R U . . .
H1B H 1.083897 0.281220 0.551438 0.070 Uiso 1 1 calc R U . . .
C2 C 0.9134(3) 0.4220(2) 0.59186(19) 0.0583(8) Uani 1 1 d . . . . .
H2A H 0.892739 0.446527 0.637084 0.070 Uiso 1 1 calc R U . . .
H2B H 0.943456 0.463463 0.562312 0.070 Uiso 1 1 calc R U . . .
C3 C 0.9486(3) 0.2932(2) 0.65828(19) 0.0552(8) Uani 1 1 d . . . . .
H3A H 1.000979 0.253865 0.671048 0.066 Uiso 1 1 calc R U . . .
H3B H 0.927580 0.317912 0.703357 0.066 Uiso 1 1 calc R U . . .
C4 C 0.9939(3) 0.3575(2) 0.6098(2) 0.0588(8) Uani 1 1 d . . . . .
C5 C 1.0848(3) 0.3967(2) 0.6515(2) 0.0668(10) Uani 1 1 d . . . . .
H5A H 1.133786 0.356200 0.665979 0.100 Uiso 1 1 calc R U . . .
H5B H 1.061308 0.423263 0.694363 0.100 Uiso 1 1 calc R U . . .
H5C H 1.116188 0.435148 0.620438 0.100 Uiso 1 1 calc R U . . .
C6 C 0.9319(6) 0.2758(5) 0.3294(4) 0.0621(17) Uani 0.5 1 d . . P . .
H6A H 0.952821 0.329308 0.317469 0.093 Uiso 0.5 1 calc R U P . .
H6B H 0.918643 0.245902 0.285090 0.093 Uiso 0.5 1 calc R U P . .
H6C H 0.985169 0.249983 0.358418 0.093 Uiso 0.5 1 calc R U P . .
P1 P 0.4960(8) 0.49867(10) 0.2485(6) 0.0580(7) Uani 0.5 1 d D . P A -1
C7 C 0.5479(6) 0.5813(4) 0.3024(4) 0.0597(16) Uani 0.5 1 d D . P A -1
H7A H 0.600173 0.607595 0.274894 0.072 Uiso 0.5 1 calc R U P A -1
H7B H 0.493935 0.619992 0.309560 0.072 Uiso 0.5 1 calc R U P A -1
C8 C 0.5946(7) 0.5569(5) 0.3776(4) 0.0626(17) Uani 0.5 1 d D . P A -1
H8A H 0.541769 0.532965 0.406255 0.075 Uiso 0.5 1 calc R U P A -1
H8B H 0.646798 0.516616 0.370862 0.075 Uiso 0.5 1 calc R U P A -1
C9 C 0.642(3) 0.6271(11) 0.4201(11) 0.085(7) Uani 0.5 1 d D . P A -1
H9A H 0.690859 0.653795 0.390113 0.102 Uiso 0.5 1 calc R U P A -1
H9B H 0.588508 0.665554 0.430546 0.102 Uiso 0.5 1 calc R U P A -1
C10 C 0.6933(16) 0.6009(14) 0.4900(10) 0.111(8) Uani 0.5 1 d D . P A -1
H10A H 0.643226 0.581579 0.522630 0.166 Uiso 0.5 1 calc R U P A -1
H10B H 0.729402 0.645414 0.512174 0.166 Uiso 0.5 1 calc R U P A -1
H10C H 0.740826 0.558627 0.480318 0.166 Uiso 0.5 1 calc R U P A -1
C11 C 0.3882(7) 0.4610(4) 0.2949(4) 0.0624(17) Uani 0.5 1 d D . P A -1
H11A H 0.410178 0.445627 0.344350 0.075 Uiso 0.5 1 calc R U P A -1
H11B H 0.338147 0.503589 0.298514 0.075 Uiso 0.5 1 calc R U P A -1
C12 C 0.3372(7) 0.3883(6) 0.2562(5) 0.078(2) Uani 0.5 1 d D . P A -1
H12A H 0.305480 0.405547 0.209904 0.093 Uiso 0.5 1 calc R U P A -1
H12B H 0.389197 0.348894 0.245721 0.093 Uiso 0.5 1 calc R U P A -1
C13 C 0.2601(8) 0.3509(6) 0.3004(5) 0.070(2) Uani 0.5 1 d D U P A -1
H13A H 0.298489 0.331853 0.343571 0.085 Uiso 0.5 1 calc R U P A -1
H13B H 0.240434 0.302975 0.273071 0.085 Uiso 0.5 1 calc R U P A -1
C14 C 0.1640(9) 0.3801(6) 0.3289(6) 0.092(3) Uani 0.5 1 d D . P A -1
H14A H 0.178573 0.418161 0.367459 0.138 Uiso 0.5 1 calc R U P A -1
H14B H 0.126416 0.335764 0.347848 0.138 Uiso 0.5 1 calc R U P A -1
H14C H 0.124161 0.405549 0.290185 0.138 Uiso 0.5 1 calc R U P A -1
C15 C 0.4597(7) 0.5322(4) 0.1573(4) 0.0618(17) Uani 0.5 1 d D . P A -1
H15A H 0.519253 0.554911 0.135144 0.074 Uiso 0.5 1 calc R U P A -1
H15B H 0.437907 0.486088 0.128212 0.074 Uiso 0.5 1 calc R U P A -1
C16 C 0.3738(8) 0.5948(6) 0.1547(4) 0.075(2) Uani 0.5 1 d D . P A -1
H16A H 0.312336 0.570289 0.172459 0.090 Uiso 0.5 1 calc R U P A -1
H16B H 0.392840 0.638412 0.187737 0.090 Uiso 0.5 1 calc R U P A -1
C17 C 0.350(2) 0.6291(8) 0.0795(7) 0.058(4) Uani 0.5 1 d D . P A -1
H17A H 0.299326 0.671081 0.084685 0.070 Uiso 0.5 1 calc R U P A -1
H17B H 0.411537 0.654760 0.063308 0.070 Uiso 0.5 1 calc R U P A -1
C18 C 0.3117(18) 0.5746(11) 0.0193(7) 0.094(6) Uani 0.5 1 d D . P A -1
H18A H 0.365979 0.539761 0.005377 0.141 Uiso 0.5 1 calc R U P A -1
H18B H 0.288469 0.606015 -0.022165 0.141 Uiso 0.5 1 calc R U P A -1
H18C H 0.256052 0.542916 0.036195 0.141 Uiso 0.5 1 calc R U P A -1
C19 C 0.5878(7) 0.4182(5) 0.2437(4) 0.0674(18) Uani 0.5 1 d D . P A -1
H19A H 0.601213 0.397050 0.292634 0.081 Uiso 0.5 1 calc R U P A -1
H19B H 0.557726 0.375290 0.213961 0.081 Uiso 0.5 1 calc R U P A -1
C20 C 0.6885(7) 0.4420(5) 0.2120(5) 0.078(2) Uani 0.5 1 d D . P A -1
H20A H 0.708050 0.492059 0.235813 0.093 Uiso 0.5 1 calc R U P A -1
H20B H 0.672862 0.454964 0.161009 0.093 Uiso 0.5 1 calc R U P A -1
C21 C 0.7849(11) 0.3914(8) 0.2125(9) 0.123(4) Uani 0.5 1 d D . P A -1
H21A H 0.834818 0.414205 0.180658 0.147 Uiso 0.5 1 calc R U P A -1
H21B H 0.815338 0.386625 0.261684 0.147 Uiso 0.5 1 calc R U P A -1
C22 C 0.7496(13) 0.3154(8) 0.1857(9) 0.117(4) Uani 0.5 1 d D U P A -1
H22A H 0.789670 0.273390 0.208711 0.176 Uiso 0.5 1 calc R U P A -1
H22B H 0.756274 0.313073 0.133611 0.176 Uiso 0.5 1 calc R U P A -1
H22C H 0.679116 0.308535 0.196884 0.176 Uiso 0.5 1 calc R U P A -1


_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 1.598(3) . ?
V1 O4 2.012(2) . ?
V1 O5 1.991(2) . ?
V1 O6 1.800(2) . ?
V1 O7 1.881(3) . ?
V1 O10 2.2486(6) . ?
V2 O2 1.602(2) . ?
V2 O4 2.009(2) . ?
V2 O6 1.830(3) 7_656 ?
V2 O8 1.997(2) . ?
V2 O9 1.853(2) 7_656 ?
V2 O10 2.2209(5) . ?
V3 O3 1.598(2) . ?
V3 O5 1.992(2) . ?
V3 O7 1.907(3) 7_656 ?
V3 O8 2.015(2) . ?
V3 O9 1.792(2) . ?
V3 O10 2.2491(5) . ?
O4 C1 1.438(4) . ?
O5 C2 1.429(4) . ?
O7 C6 1.473(8) . ?
O8 C3 1.427(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.525(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.530(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.525(5) . ?
C4 C5 1.532(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
P1 C7 1.807(9) . ?
P1 C11 1.789(11) . ?
P1 C15 1.801(11) . ?
P1 C19 1.805(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.534(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.519(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.485(13) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.541(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.457(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.465(12) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.534(10) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.508(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.495(11) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.514(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.517(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.427(13) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 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
O1 V1 O4 96.49(12) . . ?
O1 V1 O5 97.37(12) . . ?
O1 V1 O6 105.21(12) . . ?
O1 V1 O7 101.77(13) . . ?
O1 V1 O10 172.85(9) . . ?
O4 V1 O10 77.14(7) . . ?
O5 V1 O4 83.18(9) . . ?
O5 V1 O10 78.78(7) . . ?
O6 V1 O4 157.87(11) . . ?
O6 V1 O5 89.68(10) . . ?
O6 V1 O7 92.95(11) . . ?
O6 V1 O10 80.94(8) . . ?
O7 V1 O4 86.75(10) . . ?
O7 V1 O5 159.25(10) . . ?
O7 V1 O10 81.31(8) . . ?
O2 V2 O4 96.77(12) . . ?
O2 V2 O6 103.69(12) . 7_656 ?
O2 V2 O8 96.01(11) . . ?
O2 V2 O9 104.56(12) . 7_656 ?
O2 V2 O10 172.07(10) . . ?
O4 V2 O10 77.85(7) . . ?
O6 V2 O4 158.44(10) 7_656 . ?
O6 V2 O8 88.23(10) 7_656 . ?
O6 V2 O9 93.20(11) 7_656 7_656 ?
O6 V2 O10 81.08(7) 7_656 . ?
O8 V2 O4 82.87(10) . . ?
O8 V2 O10 77.65(6) . . ?
O9 V2 O4 88.12(10) 7_656 . ?
O9 V2 O8 158.39(10) 7_656 . ?
O9 V2 O10 81.27(7) 7_656 . ?
O3 V3 O5 98.38(12) . . ?
O3 V3 O7 101.28(12) . 7_656 ?
O3 V3 O8 96.63(12) . . ?
O3 V3 O9 104.80(13) . . ?
O3 V3 O10 172.92(10) . . ?
O5 V3 O8 83.00(9) . . ?
O5 V3 O10 78.77(7) . . ?
O7 V3 O5 158.70(10) 7_656 . ?
O7 V3 O8 86.65(10) 7_656 . ?
O7 V3 O10 80.76(7) 7_656 . ?
O8 V3 O10 76.65(6) . . ?
O9 V3 O5 90.17(11) . . ?
O9 V3 O7 92.66(11) . 7_656 ?
O9 V3 O8 158.25(10) . . ?
O9 V3 O10 81.78(8) . . ?
V2 O4 V1 109.87(11) . . ?
C1 O4 V1 118.2(2) . . ?
C1 O4 V2 118.39(19) . . ?
V1 O5 V3 109.27(10) . . ?
C2 O5 V1 118.9(2) . . ?
C2 O5 V3 118.83(19) . . ?
V1 O6 V2 112.81(11) . 7_656 ?
V1 O7 V3 110.39(12) . 7_656 ?
C6 O7 V1 116.8(4) . . ?
C6 O7 V3 120.4(4) . 7_656 ?
V2 O8 V3 110.43(10) . . ?
C3 O8 V2 118.1(2) . . ?
C3 O8 V3 117.92(19) . . ?
V3 O9 V2 111.91(12) . 7_656 ?
V1 O10 V1 180.00(2) 7_656 . ?
V1 O10 V3 92.47(2) 7_656 7_656 ?
V1 O10 V3 87.53(2) 7_656 . ?
V1 O10 V3 87.53(2) . 7_656 ?
V1 O10 V3 92.47(2) . . ?
V2 O10 V1 94.84(2) 7_656 7_656 ?
V2 O10 V1 85.16(2) . 7_656 ?
V2 O10 V1 85.16(2) 7_656 . ?
V2 O10 V1 94.84(2) . . ?
V2 O10 V2 180.00(3) 7_656 . ?
V2 O10 V3 85.02(2) 7_656 . ?
V2 O10 V3 94.98(2) 7_656 7_656 ?
V2 O10 V3 85.02(2) . 7_656 ?
V2 O10 V3 94.98(2) . . ?
V3 O10 V3 180.0 . 7_656 ?
O4 C1 H1A 109.2 . . ?
O4 C1 H1B 109.2 . . ?
O4 C1 C4 111.9(3) . . ?
H1A C1 H1B 107.9 . . ?
C4 C1 H1A 109.2 . . ?
C4 C1 H1B 109.2 . . ?
O5 C2 H2A 109.2 . . ?
O5 C2 H2B 109.2 . . ?
O5 C2 C4 112.2(3) . . ?
H2A C2 H2B 107.9 . . ?
C4 C2 H2A 109.2 . . ?
C4 C2 H2B 109.2 . . ?
O8 C3 H3A 109.0 . . ?
O8 C3 H3B 109.0 . . ?
O8 C3 C4 112.9(3) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C1 C4 C2 110.2(3) . . ?
C1 C4 C5 109.0(3) . . ?
C2 C4 C5 108.7(3) . . ?
C3 C4 C1 110.5(3) . . ?
C3 C4 C2 109.7(3) . . ?
C3 C4 C5 108.9(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O7 C6 H6A 109.5 . . ?
O7 C6 H6B 109.5 . . ?
O7 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C11 P1 C7 107.2(6) . . ?
C11 P1 C15 111.3(7) . . ?
C11 P1 C19 107.6(5) . . ?
C15 P1 C7 110.2(4) . . ?
C15 P1 C19 109.6(6) . . ?
C19 P1 C7 110.9(7) . . ?
P1 C7 H7A 108.7 . . ?
P1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C8 C7 P1 114.4(6) . . ?
C8 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 C7 113.0(9) . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 C8 111.8(14) . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
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 . . ?
P1 C11 H11A 108.9 . . ?
P1 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C12 C11 P1 113.2(6) . . ?
C12 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 C11 112.3(7) . . ?
C13 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C12 C13 H13A 104.0 . . ?
C12 C13 H13B 104.0 . . ?
C12 C13 C14 132.8(9) . . ?
H13A C13 H13B 105.5 . . ?
C14 C13 H13A 104.0 . . ?
C14 C13 H13B 104.0 . . ?
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 . . ?
P1 C15 H15A 108.8 . . ?
P1 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 P1 113.9(6) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C15 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 C15 114.2(11) . . ?
C17 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C16 C17 H17A 107.5 . . ?
C16 C17 H17B 107.5 . . ?
H17A C17 H17B 107.0 . . ?
C18 C17 C16 119.3(12) . . ?
C18 C17 H17A 107.5 . . ?
C18 C17 H17B 107.5 . . ?
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 . . ?
P1 C19 H19A 108.6 . . ?
P1 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 P1 114.6(7) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C19 C20 H20A 105.8 . . ?
C19 C20 H20B 105.8 . . ?
C19 C20 C21 126.2(9) . . ?
H20A C20 H20B 106.2 . . ?
C21 C20 H20A 105.8 . . ?
C21 C20 H20B 105.8 . . ?
C20 C21 H21A 111.1 . . ?
C20 C21 H21B 111.1 . . ?
H21A C21 H21B 109.0 . . ?
C22 C21 C20 103.5(12) . . ?
C22 C21 H21A 111.1 . . ?
C22 C21 H21B 111.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O4 C1 C4 68.4(3) . . . . ?
V1 O5 C2 C4 -68.3(3) . . . . ?
V2 O4 C1 C4 -68.3(3) . . . . ?
V2 O8 C3 C4 68.6(3) . . . . ?
V3 O5 C2 C4 68.9(3) . . . . ?
V3 O8 C3 C4 -68.4(3) . . . . ?
O1 V1 O6 V2 -175.20(14) . . . 7_656 ?
O1 V1 O7 V3 173.44(13) . . . 7_656 ?
O1 V1 O7 C6 31.0(4) . . . . ?
O3 V3 O9 V2 176.04(14) . . . 7_656 ?
O4 V1 O6 V2 -6.9(4) . . . 7_656 ?
O4 V1 O7 V3 77.48(12) . . . 7_656 ?
O4 V1 O7 C6 -65.0(4) . . . . ?
O4 C1 C4 C2 -61.4(4) . . . . ?
O4 C1 C4 C3 59.9(4) . . . . ?
O4 C1 C4 C5 179.5(3) . . . . ?
O5 V1 O6 V2 -77.65(13) . . . 7_656 ?
O5 V1 O7 V3 16.5(4) . . . 7_656 ?
O5 V1 O7 C6 -125.9(4) . . . . ?
O5 V3 O9 V2 77.33(14) . . . 7_656 ?
O5 C2 C4 C1 61.1(4) . . . . ?
O5 C2 C4 C3 -60.6(4) . . . . ?
O5 C2 C4 C5 -179.5(3) . . . . ?
O6 V1 O7 V3 -80.36(13) . . . 7_656 ?
O6 V1 O7 C6 137.2(4) . . . . ?
O7 V1 O6 V2 81.76(14) . . . 7_656 ?
O7 V3 O9 V2 -81.56(14) 7_656 . . 7_656 ?
O8 V3 O9 V2 6.1(4) . . . 7_656 ?
O8 C3 C4 C1 -60.5(4) . . . . ?
O8 C3 C4 C2 61.1(4) . . . . ?
O8 C3 C4 C5 179.9(3) . . . . ?
O10 V1 O6 V2 1.04(10) . . . 7_656 ?
O10 V1 O7 V3 0.00(9) . . . 7_656 ?
O10 V1 O7 C6 -142.4(4) . . . . ?
O10 V3 O9 V2 -1.30(11) . . . 7_656 ?
P1 C7 C8 C9 177.5(16) . . . . ?
P1 C11 C12 C13 171.1(8) . . . . ?
P1 C15 C16 C17 174.4(11) . . . . ?
P1 C19 C20 C21 169.5(10) . . . . ?
C7 P1 C11 C12 -178.4(6) . . . . ?
C7 P1 C15 C16 -63.6(9) . . . . ?
C7 P1 C19 C20 -57.7(9) . . . . ?
C7 C8 C9 C10 -175.5(19) . . . . ?
C11 P1 C7 C8 66.6(8) . . . . ?
C11 P1 C15 C16 55.2(7) . . . . ?
C11 P1 C19 C20 -174.6(7) . . . . ?
C11 C12 C13 C14 61.9(15) . . . . ?
C15 P1 C7 C8 -172.1(7) . . . . ?
C15 P1 C11 C12 60.9(7) . . . . ?
C15 P1 C19 C20 64.2(8) . . . . ?
C15 C16 C17 C18 62(3) . . . . ?
C19 P1 C7 C8 -50.6(9) . . . . ?
C19 P1 C11 C12 -59.1(9) . . . . ?
C19 P1 C15 C16 174.1(7) . . . . ?
C19 C20 C21 C22 49.1(17) . . . . ?

_olex2_submission_original_sample_id mataf27
_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 2.537
_oxdiff_exptl_absorpt_empirical_full_min 0.419
####################################################################### 
# 
# 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_mataf29
_database_code_depnum_ccdc_archive 'CCDC 2053156'
loop_
_audit_author_name
_audit_author_address
'William W. Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_vrf_PLAT302_mataf29             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 47% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3  ) .. 24% 
RESPONSE: Parts of or whole butyl groups were modeled as disordered
over two positions: C25-C28, 0.59(1):0.41(1), C33-C36, 0.74(2):0.26(2),
C37-C40, 0.71(1):0.29(1), C41-C44, 0.63(1):0.37(1).
;

_vrf_PLAT860_mataf29             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 216 
RESPONSE: Analogous bond lengths and angles between the two
positions of the disordered butyl groups were restrained to
be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and restrained toward the
expected motion relative to bond direction.
;

_audit_creation_date             2020-12-21
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H24 O19 V6, 2(C16 H36 N), C2 H3 N'
_chemical_formula_sum            'C46 H99 N3 O19 V6'
_chemical_formula_weight         1303.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.13612(16)
_cell_length_b                   16.90558(16)
_cell_length_c                   19.59064(19)
_cell_angle_alpha                90
_cell_angle_beta                 100.8308(9)
_cell_angle_gamma                90
_cell_volume                     5899.53(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35039
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      76.3000
_cell_measurement_theta_min      3.0230
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.364
_exptl_absorpt_coefficient_mu    8.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.049
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.886
_diffrn_reflns_theta_min         3.048
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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    -21.00  71.00   0.50    2.22    --   49.75 -78.00  56.00  184
  2  ω     34.00 127.00   0.50    8.87    --  105.75 -78.00  56.00  186
  3  ω     98.00 164.00   0.50    8.87    --  105.75  15.00 120.00  132
  4  ω    129.00 163.00   0.50    8.87    --  105.75  15.00 150.00   68
  5  ω     98.00 164.00   0.50    8.87    --  105.75  15.00  90.00  132
  6  ω     98.00 164.00   0.50    8.87    --  105.75  15.00  30.00  132
  7  ω    105.00 135.00   0.50    8.87    --  105.75  30.00 150.00   60
  8  ω     92.00 178.00   0.50    8.87    --  105.75  61.00 150.00  172
  9  ω     90.00 137.00   0.50    8.87    --  105.75  77.00 -90.00   94
 10  ω    135.00 160.00   0.50    8.87    --  105.75  15.00-150.00   50
 11  ω     85.00 178.00   0.50    8.87    --  105.75  78.00-177.00  186
 12  ω     51.00  85.00   0.50    8.87    --  105.75 -61.00  60.00   68
 13  ω     34.00  87.00   0.50    8.87    --  105.75 -61.00 -30.00  106
 14  ω     34.00  87.00   0.50    8.87    --  105.75 -61.00 -90.00  106
 15  ω     34.00  87.00   0.50    8.87    --  105.75 -61.00-120.00  106
 16  ω     34.00  87.00   0.50    8.87    --  105.75 -61.00-150.00  106
 17  ω     51.00 115.00   0.50    8.87    --  105.75-125.00-150.00  128
 18  ω     36.00  86.00   0.50    8.87    --  105.75 -61.00   0.00  100
 19  ω     34.00  87.00   0.50    8.87    --  105.75 -61.00  90.00  106
 20  ω     38.00 101.00   0.50    8.87    --  105.75 -94.00  30.00  126
 21  ω    -23.00   5.00   0.50    2.22    --   49.75 -19.00-120.00   56
 22  ω     29.00 121.00   0.50    2.22    --   49.75  78.00-177.00  184
 23  ω    -23.00   5.00   0.50    2.22    --   49.75 -19.00  60.00   56
 24  ω    -71.00  22.00   0.50    2.22    --  -49.75  78.00-177.00  186
 25  ω    -42.00 -12.00   0.50    8.87    --  -84.25  45.00  30.00   60
 26  ω    -42.00 -12.00   0.50    8.87    --  -84.25  45.00   0.00   60
 27  ω   -105.00 -12.00   0.50    8.87    --  -84.25  78.00-177.00  186
 28  ω   -121.00 -29.00   0.50    2.22    --  -49.75 -78.00  56.00  184
 29  ω   -121.00 -70.00   0.50    2.22    --  -49.75-125.00 -60.00  102
;
_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      -0.0427906000
_diffrn_orient_matrix_UB_12      0.0377257000
_diffrn_orient_matrix_UB_13      -0.0675359000
_diffrn_orient_matrix_UB_21      -0.0583857000
_diffrn_orient_matrix_UB_22      -0.0670915000
_diffrn_orient_matrix_UB_23      -0.0070797000
_diffrn_orient_matrix_UB_31      -0.0472791000
_diffrn_orient_matrix_UB_32      0.0488115000
_diffrn_orient_matrix_UB_33      0.0424200000
_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                10455
_reflns_number_total             12405
_reflns_odcompleteness_completeness 99.84
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         12405
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      1.060
_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)+(0.0761P)²+7.5303P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1542
_refine_special_details          
;
Parts of or whole butyl groups were modeled as disordered over
two positions: C25-C28, 0.59(1):0.41(1), C33-C36, 0.74(2):0.26(2),
C37-C40, 0.71(1):0.29(1), C41-C44, 0.63(1):0.37(1). Analogous
bond lengths and angles were restrained to be similar. Anisotropic
displacement parameters for proximal atoms were restrained to be
imilar and restrained toward the expected motion relative to bond
direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C35 \\sim C34-C35' \\sim C35-C36 \\sim C35'-C36'
 with sigma of 0.01
 C38-C39 \\sim C38-C39' \\sim C39-C40 \\sim C39'-C40'
 with sigma of 0.01
 N2-C41 \\sim N2-C41'
 with sigma of 0.01
 N1-C25 \\sim N1-C25'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
C28 \\sim C28': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 C34, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C35', C36'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C39', C40'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41', C42', C43', C44'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25', C26', C27', C28'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C25, C26, C27, C28} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C25', C26', C27', C28'}
{C41, C42, C43, C44} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C41', C42', C43', C44'}
6. Others
 Sof(C25')=Sof(H25C)=Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=Sof(C27')=
 Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H34C)=Sof(H34D)=Sof(C35')=Sof(H35C)=Sof(H35D)=Sof(C36')=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(2)
 Sof(H38C)=Sof(H38D)=Sof(C39')=Sof(H39C)=Sof(H39D)=Sof(C40')=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(3)
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=FVAR(3)
 Sof(C41')=Sof(H41C)=Sof(H41D)=Sof(C42')=Sof(H42C)=Sof(H42D)=Sof(C43')=
 Sof(H43C)=Sof(H43D)=Sof(C44')=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(4)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C25'(H25C,H25D), C26'(H26C,H26D),
 C27'(H27C,H27D), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,
 H33B), C34(H34A,H34B), C34(H34C,H34D), C37(H37A,H37B), C38(H38A,H38B),
 C38(H38C,H38D), C35(H35A,H35B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C35'(H35C,H35D), C39'(H39C,H39D), C41'(H41C,H41D), C42'(H42C,
 H42D), C43'(H43C,H43D)
7.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,
 H28B,H28C), C28'(H28D,H28E,H28F), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C),
 C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C36'(H36D,H36E,H36F), C40'(H40D,H40E,
 H40F), C44'(H44D,H44E,H44F), C46(H46A,H46B,H46C)
;
_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 0.52799(3) 0.57192(3) 0.31007(3) 0.03837(14) Uani 1 1 d . . . . .
V2 V 0.38634(3) 0.69896(4) 0.27378(3) 0.04026(14) Uani 1 1 d . . . . .
V3 V 0.55829(3) 0.76313(3) 0.32200(3) 0.03758(14) Uani 1 1 d . . . . .
V4 V 0.60467(3) 0.65401(3) 0.20325(3) 0.03779(14) Uani 1 1 d . . . . .
V5 V 0.42959(3) 0.59925(3) 0.15688(3) 0.04178(15) Uani 1 1 d . . . . .
V6 V 0.46903(3) 0.78755(3) 0.17365(3) 0.04146(14) Uani 1 1 d . . . . .
O1 O 0.54311(14) 0.49806(14) 0.36335(14) 0.0487(6) Uani 1 1 d . . . . .
O2 O 0.31277(13) 0.71500(16) 0.30689(13) 0.0491(6) Uani 1 1 d . . . . .
O3 O 0.60208(14) 0.81589(15) 0.38531(13) 0.0474(6) Uani 1 1 d . . . . .
O4 O 0.68098(13) 0.64124(15) 0.17410(13) 0.0481(6) Uani 1 1 d . . . . .
O5 O 0.38685(15) 0.54399(17) 0.09534(14) 0.0548(6) Uani 1 1 d . . . . .
O6 O 0.45318(16) 0.86129(16) 0.12108(14) 0.0549(6) Uani 1 1 d . . . . .
O7 O 0.42731(12) 0.60679(13) 0.33357(12) 0.0383(5) Uani 1 1 d . . . . .
O8 O 0.57002(12) 0.65709(13) 0.37511(11) 0.0375(5) Uani 1 1 d . . . . .
O9 O 0.60724(13) 0.57080(13) 0.26861(13) 0.0432(5) Uani 1 1 d . . . . .
O10 O 0.46487(13) 0.51868(13) 0.22862(13) 0.0437(5) Uani 1 1 d . . . . .
O11 O 0.45770(12) 0.76303(13) 0.34654(11) 0.0373(5) Uani 1 1 d . . . . .
O12 O 0.64373(12) 0.72769(13) 0.28258(12) 0.0405(5) Uani 1 1 d . . . . .
O13 O 0.53330(13) 0.59271(14) 0.13252(12) 0.0428(5) Uani 1 1 d . . . . .
O14 O 0.35340(12) 0.62928(15) 0.20259(13) 0.0450(5) Uani 1 1 d . . . . .
O15 O 0.38653(13) 0.78409(14) 0.21407(13) 0.0437(5) Uani 1 1 d . . . . .
O16 O 0.53014(13) 0.83240(13) 0.25298(12) 0.0404(5) Uani 1 1 d . . . . .
O17 O 0.56585(13) 0.75067(13) 0.14617(12) 0.0404(5) Uani 1 1 d . . . . .
O18 O 0.42171(13) 0.70306(15) 0.10740(12) 0.0443(5) Uani 1 1 d . . . . .
O19 O 0.49748(11) 0.67676(11) 0.24037(11) 0.0325(4) Uani 1 1 d . . . . .
C1 C 0.42276(18) 0.6088(2) 0.40543(17) 0.0415(7) Uani 1 1 d . . . . .
H1A H 0.436979 0.557373 0.425724 0.050 Uiso 1 1 calc R U . . .
H1B H 0.371084 0.618509 0.409607 0.050 Uiso 1 1 calc R U . . .
C2 C 0.55494(19) 0.6562(2) 0.44409(18) 0.0427(7) Uani 1 1 d . . . . .
H2A H 0.585609 0.696027 0.471562 0.051 Uiso 1 1 calc R U . . .
H2B H 0.569188 0.605049 0.464960 0.051 Uiso 1 1 calc R U . . .
C3 C 0.45070(19) 0.7541(2) 0.41753(17) 0.0418(7) Uani 1 1 d . . . . .
H3A H 0.399146 0.764626 0.421631 0.050 Uiso 1 1 calc R U . . .
H3B H 0.482272 0.792988 0.445371 0.050 Uiso 1 1 calc R U . . .
C4 C 0.47261(19) 0.6717(2) 0.44650(18) 0.0415(7) Uani 1 1 d . . . . .
C5 C 0.4620(2) 0.6695(2) 0.52228(19) 0.0517(9) Uani 1 1 d . . . . .
H5A H 0.492645 0.709448 0.548428 0.078 Uiso 1 1 calc R U . . .
H5B H 0.476377 0.618422 0.541782 0.078 Uiso 1 1 calc R U . . .
H5C H 0.410204 0.679135 0.524084 0.078 Uiso 1 1 calc R U . . .
C6 C 0.5691(2) 0.7480(2) 0.07394(18) 0.0474(8) Uani 1 1 d . . . . .
H6A H 0.620169 0.736599 0.068918 0.057 Uiso 1 1 calc R U . . .
H6B H 0.555875 0.799688 0.053702 0.057 Uiso 1 1 calc R U . . .
C7 C 0.4356(2) 0.7050(3) 0.03808(19) 0.0538(9) Uani 1 1 d . . . . .
H7A H 0.423151 0.757112 0.018631 0.065 Uiso 1 1 calc R U . . .
H7B H 0.402825 0.667113 0.010070 0.065 Uiso 1 1 calc R U . . .
C8 C 0.5384(2) 0.6033(2) 0.0614(2) 0.0518(9) Uani 1 1 d . . . . .
H8A H 0.506101 0.565065 0.033483 0.062 Uiso 1 1 calc R U . . .
H8B H 0.589589 0.592643 0.055970 0.062 Uiso 1 1 calc R U . . .
C9 C 0.5166(2) 0.6860(2) 0.03372(19) 0.0520(9) Uani 1 1 d . . . . .
C10 C 0.5239(3) 0.6890(3) -0.0435(2) 0.0692(13) Uani 1 1 d . . . . .
H10A H 0.575167 0.679708 -0.047304 0.104 Uiso 1 1 calc R U . . .
H10B H 0.508473 0.740082 -0.062326 0.104 Uiso 1 1 calc R U . . .
H10C H 0.492505 0.648995 -0.068878 0.104 Uiso 1 1 calc R U . . .
C11 C 0.4909(2) 0.4439(2) 0.2083(3) 0.0599(11) Uani 1 1 d . . . . .
H11A H 0.537514 0.451149 0.192508 0.090 Uiso 1 1 calc R U . . .
H11B H 0.454312 0.421940 0.171336 0.090 Uiso 1 1 calc R U . . .
H11C H 0.498458 0.408507 0.247263 0.090 Uiso 1 1 calc R U . . .
C12 C 0.7115(2) 0.7053(3) 0.3309(2) 0.0565(9) Uani 1 1 d . . . . .
H12A H 0.726443 0.747811 0.363026 0.085 Uiso 1 1 calc R U . . .
H12B H 0.750853 0.694631 0.305590 0.085 Uiso 1 1 calc R U . . .
H12C H 0.701849 0.658834 0.355919 0.085 Uiso 1 1 calc R U . . .
N1 N 0.77703(17) 0.4328(2) 0.31964(17) 0.0549(8) Uani 1 1 d D . . . .
C13 C 0.7505(2) 0.4689(2) 0.2479(2) 0.0532(9) Uani 1 1 d . . . . .
H13A H 0.761340 0.525117 0.250116 0.064 Uiso 1 1 calc R U . . .
H13B H 0.696466 0.462662 0.235035 0.064 Uiso 1 1 calc R U . . .
C14 C 0.7873(2) 0.4315(3) 0.1917(2) 0.0584(10) Uani 1 1 d . . . . .
H14A H 0.840660 0.442981 0.201297 0.070 Uiso 1 1 calc R U . . .
H14B H 0.781077 0.374551 0.192369 0.070 Uiso 1 1 calc R U . . .
C15 C 0.7524(3) 0.4634(3) 0.1201(2) 0.0628(11) Uani 1 1 d . . . . .
H15A H 0.756000 0.520694 0.121003 0.075 Uiso 1 1 calc R U . . .
H15B H 0.781115 0.444170 0.086527 0.075 Uiso 1 1 calc R U . . .
C16 C 0.6743(3) 0.4413(3) 0.0973(2) 0.0701(12) Uani 1 1 d . . . . .
H16A H 0.643919 0.468407 0.125067 0.105 Uiso 1 1 calc R U . . .
H16B H 0.669042 0.385217 0.102453 0.105 Uiso 1 1 calc R U . . .
H16C H 0.658365 0.455612 0.049420 0.105 Uiso 1 1 calc R U . . .
C17 C 0.7574(2) 0.3464(3) 0.3210(2) 0.0597(10) Uani 1 1 d . . . . .
H17A H 0.771900 0.327009 0.368181 0.072 Uiso 1 1 calc R U . . .
H17B H 0.786419 0.317569 0.292301 0.072 Uiso 1 1 calc R U . . .
C18 C 0.6749(2) 0.3286(3) 0.2956(3) 0.0683(12) Uani 1 1 d . . . . .
H18A H 0.645165 0.366039 0.316408 0.082 Uiso 1 1 calc R U . . .
H18B H 0.662979 0.335833 0.245607 0.082 Uiso 1 1 calc R U . . .
C19 C 0.6540(3) 0.2460(4) 0.3129(4) 0.0896(18) Uani 1 1 d . . . . .
H19A H 0.662430 0.240119 0.363012 0.108 Uiso 1 1 calc R U . . .
H19B H 0.686396 0.208798 0.295102 0.108 Uiso 1 1 calc R U . . .
C20 C 0.5733(4) 0.2260(4) 0.2831(5) 0.130(3) Uani 1 1 d . . . . .
H20A H 0.540959 0.264993 0.297729 0.194 Uiso 1 1 calc R U . . .
H20B H 0.561520 0.174853 0.299452 0.194 Uiso 1 1 calc R U . . .
H20C H 0.565961 0.225523 0.233327 0.194 Uiso 1 1 calc R U . . .
C21 C 0.7390(2) 0.4792(3) 0.3694(2) 0.0622(11) Uani 1 1 d . . . . .
H21A H 0.685556 0.481062 0.350646 0.075 Uiso 1 1 calc R U . . .
H21B H 0.757562 0.533123 0.371425 0.075 Uiso 1 1 calc R U . . .
C22 C 0.7500(3) 0.4468(3) 0.4438(2) 0.0662(12) Uani 1 1 d . . . . .
H22A H 0.721720 0.398188 0.444131 0.079 Uiso 1 1 calc R U . . .
H22B H 0.802683 0.434889 0.460220 0.079 Uiso 1 1 calc R U . . .
C23 C 0.7239(3) 0.5070(4) 0.4920(2) 0.0826(16) Uani 1 1 d . . . . .
H23A H 0.674533 0.525996 0.470379 0.099 Uiso 1 1 calc R U . . .
H23B H 0.718865 0.480542 0.534838 0.099 Uiso 1 1 calc R U . . .
C24 C 0.7754(5) 0.5774(4) 0.5097(3) 0.109(2) Uani 1 1 d . . . . .
H24A H 0.756924 0.610520 0.542546 0.163 Uiso 1 1 calc R U . . .
H24B H 0.777056 0.607073 0.468205 0.163 Uiso 1 1 calc R U . . .
H24C H 0.825000 0.559313 0.529503 0.163 Uiso 1 1 calc R U . . .
C25 C 0.8624(4) 0.4476(8) 0.3394(15) 0.053(3) Uani 0.592(12) 1 d D U P A 1
H25A H 0.876906 0.437010 0.388725 0.063 Uiso 0.592(12) 1 calc R U P A 1
H25B H 0.886642 0.407730 0.315600 0.063 Uiso 0.592(12) 1 calc R U P A 1
C26 C 0.8966(6) 0.5271(7) 0.3258(5) 0.067(2) Uani 0.592(12) 1 d D U P A 1
H26A H 0.893986 0.532655 0.276159 0.080 Uiso 0.592(12) 1 calc R U P A 1
H26B H 0.866160 0.568692 0.340351 0.080 Uiso 0.592(12) 1 calc R U P A 1
C27 C 0.9746(6) 0.5392(9) 0.3607(8) 0.095(4) Uani 0.592(12) 1 d D U P A 1
H27A H 0.991057 0.589977 0.345885 0.114 Uiso 0.592(12) 1 calc R U P A 1
H27B H 1.005182 0.498897 0.344359 0.114 Uiso 0.592(12) 1 calc R U P A 1
C28 C 0.9901(10) 0.5376(11) 0.4371(7) 0.149(5) Uani 0.592(12) 1 d D U P A 1
H28A H 0.956078 0.572458 0.454327 0.224 Uiso 0.592(12) 1 calc R U P A 1
H28B H 1.040815 0.554500 0.454008 0.224 Uiso 0.592(12) 1 calc R U P A 1
H28C H 0.983680 0.484706 0.452854 0.224 Uiso 0.592(12) 1 calc R U P A 1
C25' C 0.8631(5) 0.4301(12) 0.342(3) 0.066(5) Uani 0.408(12) 1 d D U P A 2
H25C H 0.877752 0.398219 0.383067 0.080 Uiso 0.408(12) 1 calc R U P A 2
H25D H 0.885824 0.408068 0.304740 0.080 Uiso 0.408(12) 1 calc R U P A 2
C26' C 0.8870(9) 0.5155(11) 0.3556(13) 0.094(5) Uani 0.408(12) 1 d D U P A 2
H26C H 0.874486 0.544662 0.312310 0.113 Uiso 0.408(12) 1 calc R U P A 2
H26D H 0.857635 0.537797 0.387462 0.113 Uiso 0.408(12) 1 calc R U P A 2
C27' C 0.9664(12) 0.5287(14) 0.3844(14) 0.121(8) Uani 0.408(12) 1 d D U P A 2
H27C H 0.996105 0.520214 0.348716 0.145 Uiso 0.408(12) 1 calc R U P A 2
H27D H 0.983133 0.491458 0.421845 0.145 Uiso 0.408(12) 1 calc R U P A 2
C28' C 0.9770(14) 0.6097(13) 0.4108(13) 0.156(6) Uani 0.408(12) 1 d D U P A 2
H28D H 0.951652 0.645759 0.376397 0.234 Uiso 0.408(12) 1 calc R U P A 2
H28E H 1.029642 0.621912 0.420805 0.234 Uiso 0.408(12) 1 calc R U P A 2
H28F H 0.956726 0.614466 0.452466 0.234 Uiso 0.408(12) 1 calc R U P A 2
N2 N 0.31260(19) 0.9762(2) 0.2887(2) 0.0712(11) Uani 1 1 d D . . . .
C29 C 0.2821(3) 0.9793(3) 0.3567(3) 0.0768(15) Uani 1 1 d . . . . .
H29A H 0.310852 1.018202 0.387048 0.092 Uiso 1 1 calc R U . . .
H29B H 0.230554 0.997672 0.346121 0.092 Uiso 1 1 calc R U . . .
C30 C 0.2840(3) 0.9026(3) 0.3958(3) 0.0768(14) Uani 1 1 d . . . . .
H30A H 0.335602 0.884584 0.408179 0.092 Uiso 1 1 calc R U . . .
H30B H 0.255933 0.863006 0.365789 0.092 Uiso 1 1 calc R U . . .
C31 C 0.2511(3) 0.9107(4) 0.4615(3) 0.0891(18) Uani 1 1 d . . . . .
H31A H 0.275112 0.954880 0.488503 0.107 Uiso 1 1 calc R U . . .
H31B H 0.198047 0.922705 0.448445 0.107 Uiso 1 1 calc R U . . .
C32 C 0.2601(3) 0.8396(4) 0.5055(3) 0.0877(17) Uani 1 1 d . . . . .
H32A H 0.233749 0.796225 0.480246 0.132 Uiso 1 1 calc R U . . .
H32B H 0.240042 0.849393 0.546653 0.132 Uiso 1 1 calc R U . . .
H32C H 0.312460 0.826721 0.518203 0.132 Uiso 1 1 calc R U . . .
C33 C 0.2659(2) 0.9215(3) 0.2368(3) 0.0615(11) Uani 1 1 d . . . . .
H33A H 0.269016 0.868372 0.255812 0.074 Uiso 1 1 calc R U . . .
H33B H 0.286856 0.920369 0.194744 0.074 Uiso 1 1 calc R U . . .
C34 C 0.1841(2) 0.9453(3) 0.2181(3) 0.0767(14) Uani 1 1 d D . . . .
H34A H 0.161536 0.943609 0.259224 0.092 Uiso 0.74(2) 1 calc R U P B 1
H34B H 0.180119 0.998917 0.200190 0.092 Uiso 0.74(2) 1 calc R U P B 1
H34C H 0.161738 0.934748 0.258438 0.092 Uiso 0.26(2) 1 calc R U P B 2
H34D H 0.182740 1.002151 0.211338 0.092 Uiso 0.26(2) 1 calc R U P B 2
C37 C 0.3129(3) 1.0594(3) 0.2636(4) 0.0867(18) Uani 1 1 d . . . . .
H37A H 0.350615 1.088922 0.295221 0.104 Uiso 1 1 calc R U . . .
H37B H 0.264492 1.083101 0.265039 0.104 Uiso 1 1 calc R U . . .
C38 C 0.3285(3) 1.0674(3) 0.1909(4) 0.0931(19) Uani 1 1 d D . . . .
H38A H 0.367973 1.031277 0.183910 0.112 Uiso 0.705(10) 1 calc R U P C 1
H38B H 0.283718 1.055815 0.156776 0.112 Uiso 0.705(10) 1 calc R U P C 1
H38C H 0.293944 1.031227 0.162786 0.112 Uiso 0.295(10) 1 calc R U P C 2
H38D H 0.378172 1.045138 0.192954 0.112 Uiso 0.295(10) 1 calc R U P C 2
C35 C 0.1438(8) 0.8895(6) 0.1643(6) 0.075(3) Uani 0.74(2) 1 d D U P B 1
H35A H 0.094835 0.911089 0.144713 0.091 Uiso 0.74(2) 1 calc R U P B 1
H35B H 0.171915 0.884389 0.126961 0.091 Uiso 0.74(2) 1 calc R U P B 1
C36 C 0.1343(5) 0.8099(5) 0.1940(8) 0.092(4) Uani 0.74(2) 1 d D U P B 1
H36A H 0.180495 0.780895 0.198377 0.138 Uiso 0.74(2) 1 calc R U P B 1
H36B H 0.095192 0.781742 0.163868 0.138 Uiso 0.74(2) 1 calc R U P B 1
H36C H 0.121204 0.815721 0.238993 0.138 Uiso 0.74(2) 1 calc R U P B 1
C39 C 0.3527(4) 1.1520(4) 0.1840(4) 0.079(2) Uani 0.705(10) 1 d D U P C 1
H39A H 0.404829 1.159178 0.205909 0.095 Uiso 0.705(10) 1 calc R U P C 1
H39B H 0.321924 1.187908 0.205261 0.095 Uiso 0.705(10) 1 calc R U P C 1
C40 C 0.3420(5) 1.1664(5) 0.1065(5) 0.098(3) Uani 0.705(10) 1 d D U P C 1
H40A H 0.291051 1.154590 0.085281 0.147 Uiso 0.705(10) 1 calc R U P C 1
H40B H 0.375422 1.132893 0.087008 0.147 Uiso 0.705(10) 1 calc R U P C 1
H40C H 0.352676 1.220746 0.098157 0.147 Uiso 0.705(10) 1 calc R U P C 1
C41 C 0.3906(3) 0.9355(4) 0.3086(4) 0.0457(17) Uani 0.629(10) 1 d D U P D 1
H41A H 0.382585 0.881718 0.322734 0.055 Uiso 0.629(10) 1 calc R U P D 1
H41B H 0.412438 0.932499 0.267106 0.055 Uiso 0.629(10) 1 calc R U P D 1
C42 C 0.4482(4) 0.9743(5) 0.3661(4) 0.0610(19) Uani 0.629(10) 1 d D U P D 1
H42A H 0.422708 1.013894 0.388931 0.073 Uiso 0.629(10) 1 calc R U P D 1
H42B H 0.467185 0.934254 0.400408 0.073 Uiso 0.629(10) 1 calc R U P D 1
C43 C 0.5119(4) 1.0116(6) 0.3436(5) 0.080(3) Uani 0.629(10) 1 d D U P D 1
H43A H 0.493365 1.053410 0.310904 0.096 Uiso 0.629(10) 1 calc R U P D 1
H43B H 0.536494 0.972714 0.319163 0.096 Uiso 0.629(10) 1 calc R U P D 1
C44 C 0.5687(5) 1.0459(8) 0.4015(6) 0.086(3) Uani 0.629(10) 1 d D U P D 1
H44A H 0.544732 1.083760 0.426720 0.129 Uiso 0.629(10) 1 calc R U P D 1
H44B H 0.607595 1.071656 0.382637 0.129 Uiso 0.629(10) 1 calc R U P D 1
H44C H 0.590199 1.004405 0.432387 0.129 Uiso 0.629(10) 1 calc R U P D 1
C35' C 0.1341(19) 0.9095(14) 0.1569(13) 0.064(5) Uani 0.26(2) 1 d D U P B 2
H35C H 0.082166 0.915213 0.161997 0.077 Uiso 0.26(2) 1 calc R U P B 2
H35D H 0.140390 0.937270 0.115052 0.077 Uiso 0.26(2) 1 calc R U P B 2
C36' C 0.1516(13) 0.8245(15) 0.1502(17) 0.078(7) Uani 0.26(2) 1 d D U P B 2
H36D H 0.162318 0.814656 0.104831 0.116 Uiso 0.26(2) 1 calc R U P B 2
H36E H 0.109255 0.793161 0.156686 0.116 Uiso 0.26(2) 1 calc R U P B 2
H36F H 0.194446 0.810568 0.184835 0.116 Uiso 0.26(2) 1 calc R U P B 2
C39' C 0.3271(12) 1.1424(7) 0.1469(10) 0.088(5) Uani 0.295(10) 1 d D U P C 2
H39C H 0.347073 1.127381 0.106156 0.106 Uiso 0.295(10) 1 calc R U P C 2
H39D H 0.274554 1.154877 0.130562 0.106 Uiso 0.295(10) 1 calc R U P C 2
C40' C 0.3652(9) 1.2201(10) 0.1723(9) 0.075(5) Uani 0.295(10) 1 d D . P C 2
H40D H 0.417618 1.210875 0.189693 0.113 Uiso 0.295(10) 1 calc R U P C 2
H40E H 0.342396 1.241439 0.208696 0.113 Uiso 0.295(10) 1 calc R U P C 2
H40F H 0.359708 1.257045 0.134414 0.113 Uiso 0.295(10) 1 calc R U P C 2
C41' C 0.3959(4) 0.9577(7) 0.2837(8) 0.055(3) Uani 0.371(10) 1 d D U P D 2
H41C H 0.406187 0.902898 0.296644 0.066 Uiso 0.371(10) 1 calc R U P D 2
H41D H 0.401334 0.963527 0.235657 0.066 Uiso 0.371(10) 1 calc R U P D 2
C42' C 0.4554(8) 1.0097(8) 0.3291(8) 0.077(4) Uani 0.371(10) 1 d D U P D 2
H42C H 0.492376 1.023806 0.301304 0.092 Uiso 0.371(10) 1 calc R U P D 2
H42D H 0.430873 1.058396 0.338697 0.092 Uiso 0.371(10) 1 calc R U P D 2
C43' C 0.4951(11) 0.9802(10) 0.3939(9) 0.103(6) Uani 0.371(10) 1 d D U P D 2
H43C H 0.519332 0.931161 0.384762 0.124 Uiso 0.371(10) 1 calc R U P D 2
H43D H 0.458533 0.967173 0.422419 0.124 Uiso 0.371(10) 1 calc R U P D 2
C44' C 0.5532(10) 1.0319(14) 0.4357(10) 0.089(5) Uani 0.371(10) 1 d D U P D 2
H44D H 0.592098 1.042582 0.409845 0.133 Uiso 0.371(10) 1 calc R U P D 2
H44E H 0.574326 1.005745 0.478391 0.133 Uiso 0.371(10) 1 calc R U P D 2
H44F H 0.530530 1.080810 0.445840 0.133 Uiso 0.371(10) 1 calc R U P D 2
N3 N 0.6066(3) 0.8456(4) 0.5643(3) 0.1065(18) Uani 1 1 d . U . . .
C45 C 0.6653(3) 0.8303(3) 0.5556(3) 0.0815(15) Uani 1 1 d . U . . .
C46 C 0.7388(3) 0.8141(4) 0.5431(4) 0.100(2) Uani 1 1 d . . . . .
H46A H 0.735277 0.781942 0.502260 0.150 Uiso 1 1 calc R U . . .
H46B H 0.767141 0.786522 0.582291 0.150 Uiso 1 1 calc R U . . .
H46C H 0.763501 0.862951 0.536463 0.150 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.618(2) . ?
V1 O7 2.052(2) . ?
V1 O8 1.978(2) . ?
V1 O9 1.779(2) . ?
V1 O10 1.995(2) . ?
V1 O19 2.242(2) . ?
V2 O2 1.612(2) . ?
V2 O7 2.006(2) . ?
V2 O11 2.046(2) . ?
V2 O14 1.838(2) . ?
V2 O15 1.855(2) . ?
V2 O19 2.2646(19) . ?
V3 O3 1.611(2) . ?
V3 O8 2.064(2) . ?
V3 O11 1.972(2) . ?
V3 O12 1.951(2) . ?
V3 O16 1.789(2) . ?
V3 O19 2.290(2) . ?
V4 O4 1.608(2) . ?
V4 O9 1.897(2) . ?
V4 O12 2.014(2) . ?
V4 O13 1.999(2) . ?
V4 O17 2.030(2) . ?
V4 O19 2.2332(19) . ?
V5 O5 1.605(2) . ?
V5 O10 1.975(3) . ?
V5 O13 2.029(2) . ?
V5 O14 1.853(2) . ?
V5 O18 1.997(3) . ?
V5 O19 2.270(2) . ?
V6 O6 1.608(3) . ?
V6 O15 1.820(2) . ?
V6 O16 1.890(2) . ?
V6 O17 2.029(2) . ?
V6 O18 2.011(2) . ?
V6 O19 2.287(2) . ?
O7 C1 1.426(4) . ?
O8 C2 1.428(4) . ?
O10 C11 1.432(4) . ?
O11 C3 1.428(4) . ?
O12 C12 1.453(4) . ?
O13 C8 1.426(4) . ?
O17 C6 1.428(4) . ?
O18 C7 1.427(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.525(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.526(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.527(5) . ?
C4 C5 1.533(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C9 1.531(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C9 1.522(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.524(6) . ?
C9 C10 1.544(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 C13 1.525(5) . ?
N1 C17 1.505(6) . ?
N1 C21 1.516(5) . ?
N1 C25 1.543(7) . ?
N1 C25' 1.540(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.527(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.525(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.451(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.514(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.503(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.508(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.533(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.524(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.513(9) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.525(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.464(11) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.471(17) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C25' H25C 0.9700 . ?
C25' H25D 0.9700 . ?
C25' C26' 1.518(17) . ?
C26' H26C 0.9700 . ?
C26' H26D 0.9700 . ?
C26' C27' 1.462(15) . ?
C27' H27C 0.9700 . ?
C27' H27D 0.9700 . ?
C27' C28' 1.46(2) . ?
C28' H28D 0.9600 . ?
C28' H28E 0.9600 . ?
C28' H28F 0.9600 . ?
N2 C29 1.537(7) . ?
N2 C33 1.512(5) . ?
N2 C37 1.489(7) . ?
N2 C41 1.555(6) . ?
N2 C41' 1.564(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.502(8) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.525(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.469(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.513(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C34 H34D 0.9700 . ?
C34 C35 1.500(7) . ?
C34 C35' 1.490(10) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.511(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C38 H38D 0.9700 . ?
C38 C39 1.509(7) . ?
C38 C39' 1.530(10) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.489(9) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.513(9) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.533(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.454(9) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.500(11) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C35' H35C 0.9700 . ?
C35' H35D 0.9700 . ?
C35' C36' 1.483(10) . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
C39' H39C 0.9700 . ?
C39' H39D 0.9700 . ?
C39' C40' 1.524(10) . ?
C40' H40D 0.9600 . ?
C40' H40E 0.9600 . ?
C40' H40F 0.9600 . ?
C41' H41C 0.9700 . ?
C41' H41D 0.9700 . ?
C41' C42' 1.539(13) . ?
C42' H42C 0.9700 . ?
C42' H42D 0.9700 . ?
C42' C43' 1.426(15) . ?
C43' H43C 0.9700 . ?
C43' H43D 0.9700 . ?
C43' C44' 1.490(15) . ?
C44' H44D 0.9600 . ?
C44' H44E 0.9600 . ?
C44' H44F 0.9600 . ?
N3 C45 1.140(7) . ?
C45 C46 1.426(8) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 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
O1 V1 O7 97.30(11) . . ?
O1 V1 O8 98.52(12) . . ?
O1 V1 O9 103.47(11) . . ?
O1 V1 O10 99.79(12) . . ?
O1 V1 O19 174.66(10) . . ?
O7 V1 O19 77.37(8) . . ?
O8 V1 O7 84.14(9) . . ?
O8 V1 O10 159.61(10) . . ?
O8 V1 O19 80.68(8) . . ?
O9 V1 O7 159.23(10) . . ?
O9 V1 O8 93.17(10) . . ?
O9 V1 O10 91.22(11) . . ?
O9 V1 O19 81.87(9) . . ?
O10 V1 O7 84.72(9) . . ?
O10 V1 O19 80.25(9) . . ?
O2 V2 O7 98.01(12) . . ?
O2 V2 O11 95.38(11) . . ?
O2 V2 O14 103.74(12) . . ?
O2 V2 O15 102.89(12) . . ?
O2 V2 O19 173.19(11) . . ?
O7 V2 O11 83.57(9) . . ?
O7 V2 O19 77.75(8) . . ?
O11 V2 O19 78.94(8) . . ?
O14 V2 O7 88.69(11) . . ?
O14 V2 O11 160.21(10) . . ?
O14 V2 O15 93.30(11) . . ?
O14 V2 O19 81.63(9) . . ?
O15 V2 O7 157.87(10) . . ?
O15 V2 O11 87.29(10) . . ?
O15 V2 O19 80.74(9) . . ?
O3 V3 O8 95.95(11) . . ?
O3 V3 O11 99.07(11) . . ?
O3 V3 O12 99.30(12) . . ?
O3 V3 O16 104.41(12) . . ?
O3 V3 O19 173.72(11) . . ?
O8 V3 O19 77.80(8) . . ?
O11 V3 O8 83.61(9) . . ?
O11 V3 O19 79.83(8) . . ?
O12 V3 O8 85.33(9) . . ?
O12 V3 O11 159.42(10) . . ?
O12 V3 O19 80.90(8) . . ?
O16 V3 O8 159.63(10) . . ?
O16 V3 O11 92.24(10) . . ?
O16 V3 O12 92.12(10) . . ?
O16 V3 O19 81.84(9) . . ?
O4 V4 O9 103.10(12) . . ?
O4 V4 O12 98.96(11) . . ?
O4 V4 O13 99.94(11) . . ?
O4 V4 O17 98.34(12) . . ?
O4 V4 O19 177.25(11) . . ?
O9 V4 O12 88.70(10) . . ?
O9 V4 O13 90.80(10) . . ?
O9 V4 O17 158.57(9) . . ?
O9 V4 O19 79.65(9) . . ?
O12 V4 O17 87.85(9) . . ?
O12 V4 O19 81.00(8) . . ?
O13 V4 O12 160.70(9) . . ?
O13 V4 O17 85.59(10) . . ?
O13 V4 O19 79.93(8) . . ?
O17 V4 O19 78.91(8) . . ?
O5 V5 O10 100.32(13) . . ?
O5 V5 O13 97.47(12) . . ?
O5 V5 O14 102.93(12) . . ?
O5 V5 O18 99.59(13) . . ?
O5 V5 O19 175.88(11) . . ?
O10 V5 O13 86.51(10) . . ?
O10 V5 O18 159.29(10) . . ?
O10 V5 O19 79.98(8) . . ?
O13 V5 O19 78.43(8) . . ?
O14 V5 O10 90.94(10) . . ?
O14 V5 O13 159.57(10) . . ?
O14 V5 O18 90.11(11) . . ?
O14 V5 O19 81.16(9) . . ?
O18 V5 O13 85.33(10) . . ?
O18 V5 O19 79.75(8) . . ?
O6 V6 O15 103.94(13) . . ?
O6 V6 O16 102.84(12) . . ?
O6 V6 O17 97.34(12) . . ?
O6 V6 O18 97.70(12) . . ?
O6 V6 O19 174.25(12) . . ?
O15 V6 O16 93.34(11) . . ?
O15 V6 O17 158.19(10) . . ?
O15 V6 O18 88.39(10) . . ?
O15 V6 O19 80.83(9) . . ?
O16 V6 O17 86.47(10) . . ?
O16 V6 O18 158.30(10) . . ?
O16 V6 O19 79.87(9) . . ?
O17 V6 O19 77.66(8) . . ?
O18 V6 O17 84.03(9) . . ?
O18 V6 O19 79.06(9) . . ?
V2 O7 V1 109.86(10) . . ?
C1 O7 V1 116.57(19) . . ?
C1 O7 V2 118.32(19) . . ?
V1 O8 V3 108.47(10) . . ?
C2 O8 V1 118.83(19) . . ?
C2 O8 V3 117.82(19) . . ?
V1 O9 V4 112.38(11) . . ?
V5 O10 V1 108.57(10) . . ?
C11 O10 V1 116.8(2) . . ?
C11 O10 V5 119.3(2) . . ?
V3 O11 V2 108.88(10) . . ?
C3 O11 V2 117.51(19) . . ?
C3 O11 V3 119.54(19) . . ?
V3 O12 V4 107.76(10) . . ?
C12 O12 V3 117.4(2) . . ?
C12 O12 V4 118.3(2) . . ?
V4 O13 V5 108.48(10) . . ?
C8 O13 V4 117.4(2) . . ?
C8 O13 V5 117.2(2) . . ?
V2 O14 V5 112.14(11) . . ?
V6 O15 V2 113.47(12) . . ?
V3 O16 V6 113.51(11) . . ?
V6 O17 V4 109.22(10) . . ?
C6 O17 V4 116.5(2) . . ?
C6 O17 V6 118.1(2) . . ?
V5 O18 V6 109.15(11) . . ?
C7 O18 V5 118.2(2) . . ?
C7 O18 V6 117.9(2) . . ?
V1 O19 V2 94.95(7) . . ?
V1 O19 V3 92.72(8) . . ?
V1 O19 V5 91.20(7) . . ?
V1 O19 V6 177.21(11) . . ?
V2 O19 V3 91.75(7) . . ?
V2 O19 V5 84.96(7) . . ?
V2 O19 V6 84.95(7) . . ?
V4 O19 V1 86.09(7) . . ?
V4 O19 V2 177.78(11) . . ?
V4 O19 V3 90.16(7) . . ?
V4 O19 V5 93.06(8) . . ?
V4 O19 V6 94.11(7) . . ?
V5 O19 V3 175.09(10) . . ?
V5 O19 V6 91.57(8) . . ?
V6 O19 V3 84.50(7) . . ?
O7 C1 H1A 108.9 . . ?
O7 C1 H1B 108.9 . . ?
O7 C1 C4 113.5(3) . . ?
H1A C1 H1B 107.7 . . ?
C4 C1 H1A 108.9 . . ?
C4 C1 H1B 108.9 . . ?
O8 C2 H2A 109.0 . . ?
O8 C2 H2B 109.0 . . ?
O8 C2 C4 113.0(3) . . ?
H2A C2 H2B 107.8 . . ?
C4 C2 H2A 109.0 . . ?
C4 C2 H2B 109.0 . . ?
O11 C3 H3A 108.9 . . ?
O11 C3 H3B 108.9 . . ?
O11 C3 C4 113.2(3) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C1 C4 C2 110.5(3) . . ?
C1 C4 C3 110.7(3) . . ?
C1 C4 C5 108.9(3) . . ?
C2 C4 C3 109.5(3) . . ?
C2 C4 C5 109.1(3) . . ?
C3 C4 C5 108.1(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O17 C6 H6A 108.9 . . ?
O17 C6 H6B 108.9 . . ?
O17 C6 C9 113.2(3) . . ?
H6A C6 H6B 107.7 . . ?
C9 C6 H6A 108.9 . . ?
C9 C6 H6B 108.9 . . ?
O18 C7 H7A 108.9 . . ?
O18 C7 H7B 108.9 . . ?
O18 C7 C9 113.2(3) . . ?
H7A C7 H7B 107.8 . . ?
C9 C7 H7A 108.9 . . ?
C9 C7 H7B 108.9 . . ?
O13 C8 H8A 108.8 . . ?
O13 C8 H8B 108.8 . . ?
O13 C8 C9 113.7(3) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C6 C9 C10 108.8(3) . . ?
C7 C9 C6 109.9(3) . . ?
C7 C9 C8 111.2(3) . . ?
C7 C9 C10 108.0(3) . . ?
C8 C9 C6 110.5(3) . . ?
C8 C9 C10 108.3(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 . . ?
O10 C11 H11A 109.5 . . ?
O10 C11 H11B 109.5 . . ?
O10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O12 C12 H12A 109.5 . . ?
O12 C12 H12B 109.5 . . ?
O12 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 N1 C25 107.1(10) . . ?
C13 N1 C25' 113.4(18) . . ?
C17 N1 C13 111.7(3) . . ?
C17 N1 C21 110.7(3) . . ?
C17 N1 C25 112.5(6) . . ?
C17 N1 C25' 101.4(8) . . ?
C21 N1 C13 106.4(3) . . ?
C21 N1 C25 108.2(9) . . ?
C21 N1 C25' 113.3(17) . . ?
N1 C13 H13A 109.0 . . ?
N1 C13 H13B 109.0 . . ?
N1 C13 C14 113.1(3) . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 C13 110.7(3) . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C14 113.9(4) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
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 . . ?
N1 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 . . ?
N1 C17 C18 114.1(3) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C17 C18 H18A 109.0 . . ?
C17 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C19 C18 C17 112.7(4) . . ?
C19 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C18 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C18 C19 C20 112.9(5) . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
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 . . ?
N1 C21 H21A 108.4 . . ?
N1 C21 H21B 108.4 . . ?
N1 C21 C22 115.6(3) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 C21 110.5(4) . . ?
C23 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
C22 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.6(5) . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
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 . . ?
N1 C25 H25A 107.0 . . ?
N1 C25 H25B 107.0 . . ?
H25A C25 H25B 106.7 . . ?
C26 C25 N1 121.4(10) . . ?
C26 C25 H25A 107.0 . . ?
C26 C25 H25B 107.0 . . ?
C25 C26 H26A 108.4 . . ?
C25 C26 H26B 108.4 . . ?
H26A C26 H26B 107.4 . . ?
C27 C26 C25 115.6(9) . . ?
C27 C26 H26A 108.4 . . ?
C27 C26 H26B 108.4 . . ?
C26 C27 H27A 108.0 . . ?
C26 C27 H27B 108.0 . . ?
C26 C27 C28 117.1(11) . . ?
H27A C27 H27B 107.3 . . ?
C28 C27 H27A 108.0 . . ?
C28 C27 H27B 108.0 . . ?
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 . . ?
N1 C25' H25C 110.7 . . ?
N1 C25' H25D 110.7 . . ?
H25C C25' H25D 108.8 . . ?
C26' C25' N1 105.2(12) . . ?
C26' C25' H25C 110.7 . . ?
C26' C25' H25D 110.7 . . ?
C25' C26' H26C 108.2 . . ?
C25' C26' H26D 108.2 . . ?
H26C C26' H26D 107.4 . . ?
C27' C26' C25' 116.2(14) . . ?
C27' C26' H26C 108.2 . . ?
C27' C26' H26D 108.2 . . ?
C26' C27' H27C 109.8 . . ?
C26' C27' H27D 109.8 . . ?
C26' C27' C28' 109.4(18) . . ?
H27C C27' H27D 108.2 . . ?
C28' C27' H27C 109.8 . . ?
C28' C27' H27D 109.8 . . ?
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 . . ?
C29 N2 C41 104.8(4) . . ?
C29 N2 C41' 124.7(6) . . ?
C33 N2 C29 110.9(4) . . ?
C33 N2 C41 105.4(4) . . ?
C33 N2 C41' 105.2(5) . . ?
C37 N2 C29 106.1(4) . . ?
C37 N2 C33 113.1(4) . . ?
C37 N2 C41 116.2(4) . . ?
C37 N2 C41' 96.0(6) . . ?
N2 C29 H29A 108.3 . . ?
N2 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 N2 115.8(3) . . ?
C30 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
C29 C30 C31 112.2(4) . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C30 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 C30 113.8(4) . . ?
C32 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 C33 H33A 108.9 . . ?
N2 C33 H33B 108.9 . . ?
N2 C33 C34 113.5(3) . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 H33A 108.9 . . ?
C34 C33 H33B 108.9 . . ?
C33 C34 H34A 109.8 . . ?
C33 C34 H34B 109.8 . . ?
C33 C34 H34C 107.2 . . ?
C33 C34 H34D 107.2 . . ?
H34A C34 H34B 108.3 . . ?
H34C C34 H34D 106.8 . . ?
C35 C34 C33 109.2(7) . . ?
C35 C34 H34A 109.8 . . ?
C35 C34 H34B 109.8 . . ?
C35' C34 C33 120.5(13) . . ?
C35' C34 H34C 107.2 . . ?
C35' C34 H34D 107.2 . . ?
N2 C37 H37A 108.7 . . ?
N2 C37 H37B 108.7 . . ?
N2 C37 C38 114.1(4) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C37 C38 H38A 110.5 . . ?
C37 C38 H38B 110.5 . . ?
C37 C38 H38C 105.2 . . ?
C37 C38 H38D 105.2 . . ?
C37 C38 C39' 128.3(10) . . ?
H38A C38 H38B 108.7 . . ?
H38C C38 H38D 105.9 . . ?
C39 C38 C37 106.2(6) . . ?
C39 C38 H38A 110.5 . . ?
C39 C38 H38B 110.5 . . ?
C39' C38 H38C 105.2 . . ?
C39' C38 H38D 105.2 . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 C34 111.7(8) . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C39 H39A 110.8 . . ?
C38 C39 H39B 110.8 . . ?
C38 C39 C40 104.9(7) . . ?
H39A C39 H39B 108.8 . . ?
C40 C39 H39A 110.8 . . ?
C40 C39 H39B 110.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N2 C41 H41A 108.0 . . ?
N2 C41 H41B 108.0 . . ?
H41A C41 H41B 107.2 . . ?
C42 C41 N2 117.3(5) . . ?
C42 C41 H41A 108.0 . . ?
C42 C41 H41B 108.0 . . ?
C41 C42 H42A 108.4 . . ?
C41 C42 H42B 108.4 . . ?
H42A C42 H42B 107.4 . . ?
C43 C42 C41 115.6(7) . . ?
C43 C42 H42A 108.4 . . ?
C43 C42 H42B 108.4 . . ?
C42 C43 H43A 108.7 . . ?
C42 C43 H43B 108.7 . . ?
C42 C43 C44 114.2(8) . . ?
H43A C43 H43B 107.6 . . ?
C44 C43 H43A 108.7 . . ?
C44 C43 H43B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C34 C35' H35C 109.5 . . ?
C34 C35' H35D 109.5 . . ?
H35C C35' H35D 108.0 . . ?
C36' C35' C34 110.9(16) . . ?
C36' C35' H35C 109.5 . . ?
C36' C35' H35D 109.5 . . ?
C35' C36' H36D 109.5 . . ?
C35' C36' H36E 109.5 . . ?
C35' C36' H36F 109.5 . . ?
H36D C36' H36E 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C38 C39' H39C 106.1 . . ?
C38 C39' H39D 106.1 . . ?
H39C C39' H39D 106.3 . . ?
C40' C39' C38 124.9(14) . . ?
C40' C39' H39C 106.1 . . ?
C40' C39' H39D 106.1 . . ?
C39' C40' H40D 109.5 . . ?
C39' C40' H40E 109.5 . . ?
C39' C40' H40F 109.5 . . ?
H40D C40' H40E 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 109.5 . . ?
N2 C41' H41C 108.4 . . ?
N2 C41' H41D 108.4 . . ?
H41C C41' H41D 107.5 . . ?
C42' C41' N2 115.5(10) . . ?
C42' C41' H41C 108.4 . . ?
C42' C41' H41D 108.4 . . ?
C41' C42' H42C 107.4 . . ?
C41' C42' H42D 107.4 . . ?
H42C C42' H42D 106.9 . . ?
C43' C42' C41' 119.8(12) . . ?
C43' C42' H42C 107.4 . . ?
C43' C42' H42D 107.4 . . ?
C42' C43' H43C 107.8 . . ?
C42' C43' H43D 107.8 . . ?
C42' C43' C44' 118.0(14) . . ?
H43C C43' H43D 107.1 . . ?
C44' C43' H43C 107.8 . . ?
C44' C43' H43D 107.8 . . ?
C43' C44' H44D 109.5 . . ?
C43' C44' H44E 109.5 . . ?
C43' C44' H44F 109.5 . . ?
H44D C44' H44E 109.5 . . ?
H44D C44' H44F 109.5 . . ?
H44E C44' H44F 109.5 . . ?
N3 C45 C46 177.6(8) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 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 C4 66.7(3) . . . . ?
V1 O8 C2 C4 -67.9(3) . . . . ?
V2 O7 C1 C4 -67.8(3) . . . . ?
V2 O11 C3 C4 66.9(3) . . . . ?
V3 O8 C2 C4 66.5(3) . . . . ?
V3 O11 C3 C4 -68.7(3) . . . . ?
V4 O13 C8 C9 -66.6(4) . . . . ?
V4 O17 C6 C9 66.6(4) . . . . ?
V5 O13 C8 C9 65.2(3) . . . . ?
V5 O18 C7 C9 -66.3(4) . . . . ?
V6 O17 C6 C9 -66.5(4) . . . . ?
V6 O18 C7 C9 68.5(4) . . . . ?
O1 V1 O9 V4 -179.04(14) . . . . ?
O2 V2 O14 V5 -178.61(14) . . . . ?
O2 V2 O15 V6 174.89(13) . . . . ?
O3 V3 O16 V6 -174.65(13) . . . . ?
O4 V4 O9 V1 179.36(14) . . . . ?
O5 V5 O14 V2 -176.61(15) . . . . ?
O6 V6 O15 V2 175.96(14) . . . . ?
O6 V6 O16 V3 -179.55(14) . . . . ?
O7 V1 O9 V4 2.3(4) . . . . ?
O7 V2 O14 V5 -80.68(13) . . . . ?
O7 V2 O15 V6 14.4(4) . . . . ?
O7 C1 C4 C2 -61.3(4) . . . . ?
O7 C1 C4 C3 60.2(4) . . . . ?
O7 C1 C4 C5 178.9(3) . . . . ?
O8 V1 O9 V4 -79.49(13) . . . . ?
O8 V3 O16 V6 2.9(4) . . . . ?
O8 C2 C4 C1 60.3(4) . . . . ?
O8 C2 C4 C3 -61.9(4) . . . . ?
O8 C2 C4 C5 179.9(3) . . . . ?
O10 V1 O9 V4 80.60(14) . . . . ?
O10 V5 O14 V2 82.57(14) . . . . ?
O11 V2 O14 V5 -13.9(4) . . . . ?
O11 V2 O15 V6 79.99(13) . . . . ?
O11 V3 O16 V6 -74.69(13) . . . . ?
O11 C3 C4 C1 -60.3(4) . . . . ?
O11 C3 C4 C2 61.8(4) . . . . ?
O11 C3 C4 C5 -179.4(3) . . . . ?
O12 V3 O16 V6 85.19(13) . . . . ?
O12 V4 O9 V1 80.46(13) . . . . ?
O13 V4 O9 V1 -80.24(14) . . . . ?
O13 V5 O14 V2 0.1(4) . . . . ?
O13 C8 C9 C6 61.5(4) . . . . ?
O13 C8 C9 C7 -60.9(4) . . . . ?
O13 C8 C9 C10 -179.4(3) . . . . ?
O14 V2 O15 V6 -80.20(14) . . . . ?
O15 V2 O14 V5 77.27(14) . . . . ?
O15 V6 O16 V3 75.33(13) . . . . ?
O16 V6 O15 V2 -79.92(13) . . . . ?
O17 V4 O9 V1 -0.3(4) . . . . ?
O17 V6 O15 V2 8.9(4) . . . . ?
O17 V6 O16 V3 -82.82(13) . . . . ?
O17 C6 C9 C7 61.2(4) . . . . ?
O17 C6 C9 C8 -61.9(4) . . . . ?
O17 C6 C9 C10 179.3(4) . . . . ?
O18 V5 O14 V2 -76.75(14) . . . . ?
O18 V6 O15 V2 78.42(14) . . . . ?
O18 V6 O16 V3 -18.7(3) . . . . ?
O18 C7 C9 C6 -62.1(4) . . . . ?
O18 C7 C9 C8 60.6(4) . . . . ?
O18 C7 C9 C10 179.3(3) . . . . ?
O19 V1 O9 V4 0.62(12) . . . . ?
O19 V2 O14 V5 -2.86(12) . . . . ?
O19 V2 O15 V6 0.76(12) . . . . ?
O19 V3 O16 V6 4.70(11) . . . . ?
O19 V4 O9 V1 -0.63(12) . . . . ?
O19 V5 O14 V2 2.86(12) . . . . ?
O19 V6 O15 V2 -0.75(12) . . . . ?
O19 V6 O16 V3 -4.73(11) . . . . ?
N1 C13 C14 C15 173.7(4) . . . . ?
N1 C17 C18 C19 -166.6(4) . . . . ?
N1 C21 C22 C23 168.0(4) . . . . ?
N1 C25 C26 C27 166.7(15) . . . . ?
N1 C25' C26' C27' 174(2) . . . . ?
C13 N1 C17 C18 -54.2(4) . . . . ?
C13 N1 C21 C22 172.9(4) . . . . ?
C13 N1 C25 C26 43(2) . . . . ?
C13 N1 C25' C26' 71(3) . . . . ?
C13 C14 C15 C16 -66.0(5) . . . . ?
C17 N1 C13 C14 -62.3(4) . . . . ?
C17 N1 C21 C22 51.4(5) . . . . ?
C17 N1 C25 C26 165.9(15) . . . . ?
C17 N1 C25' C26' -169(2) . . . . ?
C17 C18 C19 C20 -175.7(6) . . . . ?
C21 N1 C13 C14 176.8(4) . . . . ?
C21 N1 C17 C18 64.2(5) . . . . ?
C21 N1 C25 C26 -71(2) . . . . ?
C21 N1 C25' C26' -50(3) . . . . ?
C21 C22 C23 C24 -73.3(6) . . . . ?
C25 N1 C13 C14 61.3(8) . . . . ?
C25 N1 C17 C18 -174.7(12) . . . . ?
C25 N1 C21 C22 -72.3(10) . . . . ?
C25 C26 C27 C28 -61(2) . . . . ?
C25' N1 C13 C14 51.5(12) . . . . ?
C25' N1 C17 C18 -175(2) . . . . ?
C25' N1 C21 C22 -61.8(15) . . . . ?
C25' C26' C27' C28' -166(3) . . . . ?
N2 C29 C30 C31 -178.6(4) . . . . ?
N2 C33 C34 C35 177.5(7) . . . . ?
N2 C33 C34 C35' 166.2(17) . . . . ?
N2 C37 C38 C39 -161.1(5) . . . . ?
N2 C37 C38 C39' 174.8(10) . . . . ?
N2 C41 C42 C43 -109.7(8) . . . . ?
N2 C41' C42' C43' 99.8(19) . . . . ?
C29 N2 C33 C34 59.3(5) . . . . ?
C29 N2 C37 C38 -170.0(4) . . . . ?
C29 N2 C41 C42 -57.5(7) . . . . ?
C29 N2 C41' C42' -53.7(13) . . . . ?
C29 C30 C31 C32 -173.1(5) . . . . ?
C33 N2 C29 C30 62.8(5) . . . . ?
C33 N2 C37 C38 -48.2(5) . . . . ?
C33 N2 C41 C42 -174.6(6) . . . . ?
C33 N2 C41' C42' 176.6(9) . . . . ?
C33 C34 C35 C36 71.6(13) . . . . ?
C33 C34 C35' C36' 38(4) . . . . ?
C37 N2 C29 C30 -173.9(4) . . . . ?
C37 N2 C33 C34 -59.9(6) . . . . ?
C37 N2 C41 C42 59.3(8) . . . . ?
C37 N2 C41' C42' 60.7(11) . . . . ?
C37 C38 C39 C40 -161.0(6) . . . . ?
C37 C38 C39' C40' 48(2) . . . . ?
C41 N2 C29 C30 -50.5(5) . . . . ?
C41 N2 C33 C34 172.2(5) . . . . ?
C41 N2 C37 C38 73.9(6) . . . . ?
C41 C42 C43 C44 -177.6(8) . . . . ?
C41' N2 C29 C30 -64.5(8) . . . . ?
C41' N2 C33 C34 -163.4(7) . . . . ?
C41' N2 C37 C38 61.1(7) . . . . ?
C41' C42' C43' C44' 179.0(16) . . . . ?

_olex2_submission_original_sample_id mataf29
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.720
