# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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_exp_3912
_database_code_depnum_ccdc_archive 'CCDC 1484788'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H106 N2 O27 V6'
_chemical_formula_weight         1569.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.5756(3)
_cell_length_b                   15.3260(4)
_cell_length_c                   20.1152(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.354(2)
_cell_angle_gamma                90.00
_cell_volume                     3498.75(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    104.1
_cell_measurement_reflns_used    5576
_cell_measurement_theta_min      2.9854
_cell_measurement_theta_max      29.2569

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1644
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      104.1
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17371
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         29.32
_reflns_number_total             8064
_reflns_number_gt                6176
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0726P)²+5.1297P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8064
_refine_ls_number_parameters     498
_refine_ls_number_restraints     256
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1550
_refine_ls_wR_factor_gt          0.1416
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.96136(4) 0.64168(4) 0.01536(3) 0.02595(14) Uani 1 1 d . . .
V2 V 0.92125(4) 0.49997(4) -0.11118(3) 0.02549(14) Uani 1 1 d . . .
V3 V 0.83694(4) 0.45031(4) 0.03142(3) 0.02574(14) Uani 1 1 d . . .
O1 O 0.93346(19) 0.45962(16) 0.11570(11) 0.0300(5) Uani 1 1 d . . .
O2 O 1.03376(19) 0.61397(15) 0.10197(11) 0.0306(5) Uani 1 1 d . . .
O3 O 1.0000 0.5000 0.0000 0.0223(6) Uani 1 2 d S . .
O4 O 1.10040(18) 0.65431(15) -0.01356(11) 0.0298(5) Uani 1 1 d . . .
O5 O 0.91642(19) 0.74021(15) 0.02157(12) 0.0316(5) Uani 1 1 d . . .
O6 O 0.71064(19) 0.42460(16) 0.04745(11) 0.0323(5) Uani 1 1 d . . .
O7 O 0.8486(2) 0.50478(15) -0.18865(11) 0.0322(5) Uani 1 1 d . . .
O8 O 0.88271(18) 0.62164(14) -0.08251(10) 0.0257(5) Uani 1 1 d . . .
O9 O 0.78204(17) 0.46848(14) -0.06862(11) 0.0254(5) Uani 1 1 d . . .
O10 O 0.81576(17) 0.58131(15) 0.03382(10) 0.0269(5) Uani 1 1 d . . .
O11 O 0.5534(3) 0.73477(19) -0.07565(16) 0.0557(8) Uani 1 1 d . . .
O12 O 0.3959(6) 0.7694(4) -0.1429(4) 0.203(4) Uani 1 1 d . . .
N1 N 1.0940(2) 0.70244(19) -0.25936(13) 0.0288(6) Uani 1 1 d . . .
C1 C 0.6707(3) 0.5104(2) -0.09184(17) 0.0307(7) Uani 1 1 d . . .
H1A H 0.6109 0.4814 -0.0722 0.037 Uiso 1 1 calc R . .
H1B H 0.6487 0.5048 -0.1407 0.037 Uiso 1 1 calc R . .
C2 C 0.7660(3) 0.6545(2) -0.10569(17) 0.0297(7) Uani 1 1 d . . .
H2A H 0.7446 0.6475 -0.1545 0.036 Uiso 1 1 calc R . .
H2B H 0.7647 0.7163 -0.0957 0.036 Uiso 1 1 calc R . .
C3 C 0.6749(3) 0.6076(2) -0.07255(16) 0.0307(7) Uani 1 1 d . . .
C4 C 0.7031(3) 0.6176(2) 0.00437(16) 0.0308(7) Uani 1 1 d . . .
H4A H 0.7022 0.6790 0.0158 0.037 Uiso 1 1 calc R . .
H4B H 0.6425 0.5887 0.0235 0.037 Uiso 1 1 calc R . .
C5 C 0.5522(3) 0.6460(2) -0.10030(19) 0.0370(8) Uani 1 1 d . . .
H5A H 0.5357 0.6452 -0.1495 0.044 Uiso 1 1 calc R . .
H5B H 0.4921 0.6122 -0.0844 0.044 Uiso 1 1 calc R . .
C6 C 0.4752(5) 0.7908(3) -0.1010(3) 0.0662(14) Uani 1 1 d . A .
C7 C 0.4880(4) 0.8802(3) -0.0678(2) 0.0529(10) Uani 1 1 d U . .
H7A H 0.4188 0.8907 -0.0476 0.063 Uiso 0.609(5) 1 calc PR A 1
H7B H 0.5130 0.8725 -0.0187 0.063 Uiso 0.391(5) 1 d PR A 2
C8A C 0.6003(9) 0.8923(6) -0.0116(4) 0.071(2) Uani 0.609(5) 1 d PU A 1
H8AA H 0.5884 0.9416 0.0166 0.086 Uiso 0.609(5) 1 calc PR A 1
H8AB H 0.6111 0.8408 0.0169 0.086 Uiso 0.609(5) 1 calc PR A 1
C9A C 0.7063(11) 0.9069(9) -0.0384(7) 0.088(3) Uani 0.609(5) 1 d PU A 1
H9A H 0.7787 0.9012 -0.0089 0.105 Uiso 0.609(5) 1 calc PR A 1
C10A C 0.7059(8) 0.9276(8) -0.1014(7) 0.090(3) Uani 0.609(5) 1 d PU A 1
H10 H 0.7783 0.9314 -0.1146 0.107 Uiso 0.609(5) 1 calc PR A 1
C11A C 0.6004(9) 0.9453(10) -0.1530(7) 0.082(3) Uani 0.609(5) 1 d PU A 1
H11A H 0.5881 0.8979 -0.1856 0.098 Uiso 0.609(5) 1 calc PR A 1
H11B H 0.6119 0.9985 -0.1771 0.098 Uiso 0.609(5) 1 calc PR A 1
C12A C 0.4941(6) 0.9549(4) -0.1221(3) 0.0432(15) Uani 0.609(5) 1 d PU A 1
H12 H 0.5021 1.0105 -0.0976 0.052 Uiso 0.609(5) 1 calc PR A 1
C13A C 0.3787(12) 0.9558(12) -0.1677(9) 0.083(4) Uani 0.609(5) 1 d PU A 1
O13A O 0.2880(7) 0.9731(6) -0.1438(4) 0.091(2) Uani 0.609(5) 1 d PU A 1
O14A O 0.3707(5) 0.9673(4) -0.2313(3) 0.0740(19) Uani 0.609(5) 1 d PU A 1
H14C H 0.3022 0.9781 -0.2489 0.111 Uiso 0.609(5) 1 calc PR A 1
C8B C 0.3703(11) 0.9272(10) -0.0803(7) 0.070(4) Uani 0.391(5) 1 d PU A 2
H8BA H 0.3730 0.9763 -0.0497 0.084 Uiso 0.391(5) 1 calc PR A 2
H8BB H 0.3082 0.8879 -0.0731 0.084 Uiso 0.391(5) 1 calc PR A 2
C9B C 0.3431(17) 0.9645(11) -0.1673(11) 0.061(4) Uani 0.391(5) 1 d PU A 2
H9B H 0.2692 0.9801 -0.1916 0.073 Uiso 0.391(5) 1 calc PR A 2
C10B C 0.4276(13) 0.9666(13) -0.1892(7) 0.059(4) Uani 0.391(5) 1 d PU A 2
H10A H 0.4159 0.9929 -0.2316 0.071 Uiso 0.391(5) 1 calc PR A 2
C11B C 0.5446(13) 0.9387(12) -0.1668(8) 0.057(3) Uani 0.391(5) 1 d PU A 2
H11C H 0.5968 0.9830 -0.1787 0.069 Uiso 0.391(5) 1 calc PR A 2
H11D H 0.5566 0.8860 -0.1912 0.069 Uiso 0.391(5) 1 calc PR A 2
C12B C 0.5797(9) 0.9209(8) -0.0933(5) 0.050(2) Uani 0.391(5) 1 d PU A 2
H12A H 0.5861 0.9789 -0.0724 0.060 Uiso 0.391(5) 1 calc PR A 2
C13B C 0.7037(12) 0.8819(9) -0.0716(8) 0.050(3) Uani 0.391(5) 1 d PU A 2
O13B O 0.7372(9) 0.8674(7) -0.0094(5) 0.071(3) Uani 0.391(5) 1 d PU A 2
H13A H 0.7891 0.8302 -0.0038 0.106 Uiso 0.391(5) 1 calc PR A 2
O14B O 0.7653(8) 0.8690(6) -0.1151(5) 0.073(3) Uani 0.391(5) 1 d PU A 2
C14 C 1.0930(3) 0.7344(2) -0.18734(16) 0.0315(7) Uani 1 1 d . . .
H14A H 1.0377 0.6987 -0.1688 0.038 Uiso 1 1 calc R . .
H14B H 1.1705 0.7244 -0.1598 0.038 Uiso 1 1 calc R . .
C15 C 1.0609(3) 0.8298(2) -0.18009(18) 0.0357(8) Uani 1 1 d . . .
H15A H 0.9824 0.8410 -0.2060 0.043 Uiso 1 1 calc R . .
H15B H 1.1158 0.8669 -0.1976 0.043 Uiso 1 1 calc R . .
C16 C 1.0655(5) 0.8502(3) -0.1054(2) 0.0567(12) Uani 1 1 d . . .
H16A H 1.0078 0.8143 -0.0892 0.068 Uiso 1 1 calc R . .
H16B H 1.1427 0.8345 -0.0798 0.068 Uiso 1 1 calc R . .
C17 C 1.0420(4) 0.9448(3) -0.0915(2) 0.0591(12) Uani 1 1 d . . .
H17A H 1.0980 0.9811 -0.1079 0.089 Uiso 1 1 calc R . .
H17B H 1.0494 0.9534 -0.0436 0.089 Uiso 1 1 calc R . .
H17C H 0.9637 0.9601 -0.1142 0.089 Uiso 1 1 calc R . .
C18 C 0.9769(3) 0.7210(3) -0.30641(16) 0.0335(7) Uani 1 1 d . . .
H18A H 0.9716 0.7832 -0.3151 0.040 Uiso 1 1 calc R . .
H18B H 0.9769 0.6921 -0.3493 0.040 Uiso 1 1 calc R . .
C19 C 0.8682(3) 0.6929(2) -0.28128(17) 0.0348(8) Uani 1 1 d . . .
H19A H 0.8625 0.7252 -0.2406 0.042 Uiso 1 1 calc R . .
H19B H 0.8735 0.6313 -0.2701 0.042 Uiso 1 1 calc R . .
C20 C 0.7589(3) 0.7098(3) -0.3358(2) 0.0471(10) Uani 1 1 d . . .
H20A H 0.7618 0.7689 -0.3526 0.057 Uiso 1 1 calc R . .
H20B H 0.7589 0.6702 -0.3735 0.057 Uiso 1 1 calc R . .
C21 C 0.6462(4) 0.6976(3) -0.3095(2) 0.0576(12) Uani 1 1 d . . .
H21A H 0.5798 0.7066 -0.3458 0.086 Uiso 1 1 calc R . .
H21B H 0.6437 0.7389 -0.2740 0.086 Uiso 1 1 calc R . .
H21C H 0.6436 0.6394 -0.2921 0.086 Uiso 1 1 calc R . .
C22 C 1.1916(3) 0.7500(2) -0.28611(16) 0.0324(7) Uani 1 1 d . . .
H22A H 1.1707 0.8113 -0.2914 0.039 Uiso 1 1 calc R . .
H22B H 1.2637 0.7460 -0.2522 0.039 Uiso 1 1 calc R . .
C23 C 1.2161(3) 0.7167(3) -0.35281(17) 0.0373(8) Uani 1 1 d . . .
H23A H 1.1463 0.7233 -0.3881 0.045 Uiso 1 1 calc R . .
H23B H 1.2361 0.6552 -0.3488 0.045 Uiso 1 1 calc R . .
C24 C 1.3175(3) 0.7678(3) -0.3715(2) 0.0468(10) Uani 1 1 d . . .
H24A H 1.3858 0.7626 -0.3350 0.056 Uiso 1 1 calc R . .
H24B H 1.2960 0.8290 -0.3760 0.056 Uiso 1 1 calc R . .
C25 C 1.3506(4) 0.7365(4) -0.4375(2) 0.0615(14) Uani 1 1 d . . .
H25A H 1.2829 0.7401 -0.4736 0.092 Uiso 1 1 calc R . .
H25B H 1.3772 0.6771 -0.4323 0.092 Uiso 1 1 calc R . .
H25C H 1.4123 0.7727 -0.4479 0.092 Uiso 1 1 calc R . .
C26 C 1.1150(3) 0.6044(2) -0.25675(16) 0.0320(7) Uani 1 1 d . . .
H26A H 1.1030 0.5826 -0.3029 0.038 Uiso 1 1 calc R . .
H26B H 1.0562 0.5774 -0.2352 0.038 Uiso 1 1 calc R . .
C27 C 1.2363(3) 0.5753(2) -0.21947(17) 0.0313(7) Uani 1 1 d . . .
H27A H 1.2957 0.5966 -0.2434 0.038 Uiso 1 1 calc R . .
H27B H 1.2522 0.6004 -0.1743 0.038 Uiso 1 1 calc R . .
C28 C 1.2440(3) 0.4764(3) -0.2142(2) 0.0411(9) Uani 1 1 d . . .
H28A H 1.2304 0.4512 -0.2593 0.049 Uiso 1 1 calc R . .
H28B H 1.1833 0.4549 -0.1913 0.049 Uiso 1 1 calc R . .
C29 C 1.3650(4) 0.4478(3) -0.1749(2) 0.0473(10) Uani 1 1 d . . .
H29A H 1.4250 0.4681 -0.1979 0.071 Uiso 1 1 calc R . .
H29B H 1.3679 0.3853 -0.1720 0.071 Uiso 1 1 calc R . .
H29C H 1.3781 0.4721 -0.1300 0.071 Uiso 1 1 calc R . .


_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 O5 1.610(2) . ?
V1 O4 1.826(2) . ?
V1 O2 1.828(2) . ?
V1 O10 2.020(2) . ?
V1 O8 2.023(2) . ?
V1 O3 2.2504(6) . ?
V1 V3 3.0314(8) 3_765 ?
V1 V2 3.0402(8) 3_765 ?
V2 O7 1.620(2) . ?
V2 O1 1.811(2) 3_765 ?
V2 O2 1.821(2) 3_765 ?
V2 O9 2.026(2) . ?
V2 O8 2.027(2) . ?
V2 O3 2.2427(5) . ?
V2 V3 3.0367(7) 3_765 ?
V2 V1 3.0402(8) 3_765 ?
V3 O6 1.607(2) . ?
V3 O4 1.825(2) 3_765 ?
V3 O1 1.843(2) . ?
V3 O9 2.007(2) . ?
V3 O10 2.024(2) . ?
V3 O3 2.2387(5) . ?
V3 V1 3.0314(8) 3_765 ?
V3 V2 3.0367(7) 3_765 ?
O1 V2 1.811(2) 3_765 ?
O2 V2 1.821(2) 3_765 ?
O3 V3 2.2387(5) 3_765 ?
O3 V2 2.2427(5) 3_765 ?
O3 V1 2.2504(6) 3_765 ?
O4 V3 1.825(2) 3_765 ?
O8 C2 1.431(4) . ?
O9 C1 1.433(4) . ?
O10 C4 1.435(4) . ?
O11 C6 1.278(5) . ?
O11 C5 1.447(5) . ?
O12 C6 1.165(6) . ?
N1 C18 1.519(4) . ?
N1 C26 1.521(4) . ?
N1 C22 1.529(4) . ?
N1 C14 1.531(4) . ?
C1 C3 1.538(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.533(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.525(5) . ?
C3 C5 1.538(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.519(7) . ?
C7 C12B 1.413(12) . ?
C7 C8B 1.518(12) . ?
C7 C8A 1.556(9) . ?
C7 C12A 1.594(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9799 . ?
C8A C9A 1.451(17) . ?
C8A H7B 1.0377 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C9A C10A 1.307(17) . ?
C9A H9A 0.9300 . ?
C10A C11A 1.464(14) . ?
C10A H10 0.9300 . ?
C11A C12A 1.491(12) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C12A C13A 1.464(11) . ?
C12A H12 0.9800 . ?
C13A O13A 1.265(18) . ?
C13A O14A 1.277(19) . ?
O14A H14C 0.8200 . ?
C8B C9B 1.81(2) . ?
C8B H8BA 0.9700 . ?
C8B H8BB 0.9700 . ?
C9B C10B 1.15(2) . ?
C9B H9B 0.9300 . ?
C10B C11B 1.41(2) . ?
C10B H10A 0.9300 . ?
C11B C12B 1.478(18) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C12B C13B 1.537(17) . ?
C12B H12A 0.9800 . ?
C13B O14B 1.249(15) . ?
C13B O13B 1.253(17) . ?
O13B H13A 0.8200 . ?
C14 C15 1.522(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.525(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.511(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.508(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.525(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.513(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.514(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.518(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.529(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.522(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.522(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.531(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 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
O5 V1 O4 104.11(11) . . ?
O5 V1 O2 103.79(11) . . ?
O4 V1 O2 93.49(10) . . ?
O5 V1 O10 96.96(11) . . ?
O4 V1 O10 157.92(10) . . ?
O2 V1 O10 87.76(9) . . ?
O5 V1 O8 97.32(10) . . ?
O4 V1 O8 87.83(9) . . ?
O2 V1 O8 157.82(10) . . ?
O10 V1 O8 82.96(8) . . ?
O5 V1 O3 172.56(8) . . ?
O4 V1 O3 81.21(7) . . ?
O2 V1 O3 80.82(7) . . ?
O10 V1 O3 77.23(7) . . ?
O8 V1 O3 77.50(6) . . ?
O5 V1 V3 137.79(9) . 3_765 ?
O4 V1 V3 33.85(7) . 3_765 ?
O2 V1 V3 87.20(7) . 3_765 ?
O10 V1 V3 124.44(7) . 3_765 ?
O8 V1 V3 81.60(6) . 3_765 ?
O3 V1 V3 47.362(14) . 3_765 ?
O5 V1 V2 137.00(8) . 3_765 ?
O4 V1 V2 88.04(7) . 3_765 ?
O2 V1 V2 33.51(7) . 3_765 ?
O10 V1 V2 80.87(6) . 3_765 ?
O8 V1 V2 124.61(7) . 3_765 ?
O3 V1 V2 47.313(14) . 3_765 ?
V3 V1 V2 65.750(18) 3_765 3_765 ?
O7 V2 O1 104.34(11) . 3_765 ?
O7 V2 O2 103.03(11) . 3_765 ?
O1 V2 O2 94.77(11) 3_765 3_765 ?
O7 V2 O9 96.40(10) . . ?
O1 V2 O9 157.85(10) 3_765 . ?
O2 V2 O9 87.93(10) 3_765 . ?
O7 V2 O8 97.47(10) . . ?
O1 V2 O8 87.60(10) 3_765 . ?
O2 V2 O8 158.05(9) 3_765 . ?
O9 V2 O8 82.02(9) . . ?
O7 V2 O3 172.38(9) . . ?
O1 V2 O3 81.42(7) 3_765 . ?
O2 V2 O3 81.19(7) 3_765 . ?
O9 V2 O3 77.27(6) . . ?
O8 V2 O3 77.59(6) . . ?
O7 V2 V3 138.32(9) . 3_765 ?
O1 V2 V3 34.13(7) 3_765 3_765 ?
O2 V2 V3 88.36(7) 3_765 3_765 ?
O9 V2 V3 124.30(6) . 3_765 ?
O8 V2 V3 81.40(6) . 3_765 ?
O3 V2 V3 47.287(13) . 3_765 ?
O7 V2 V1 136.46(9) . 3_765 ?
O1 V2 V1 88.42(7) 3_765 3_765 ?
O2 V2 V1 33.66(7) 3_765 3_765 ?
O9 V2 V1 81.69(6) . 3_765 ?
O8 V2 V1 124.92(6) . 3_765 ?
O3 V2 V1 47.527(14) . 3_765 ?
V3 V2 V1 66.031(18) 3_765 3_765 ?
O6 V3 O4 103.69(11) . 3_765 ?
O6 V3 O1 104.19(11) . . ?
O4 V3 O1 93.24(10) 3_765 . ?
O6 V3 O9 96.56(10) . . ?
O4 V3 O9 89.09(10) 3_765 . ?
O1 V3 O9 157.90(9) . . ?
O6 V3 O10 96.85(11) . . ?
O4 V3 O10 158.59(9) 3_765 . ?
O1 V3 O10 87.46(10) . . ?
O9 V3 O10 82.55(9) . . ?
O6 V3 O3 172.32(9) . . ?
O4 V3 O3 81.57(7) 3_765 . ?
O1 V3 O3 80.86(7) . . ?
O9 V3 O3 77.75(6) . . ?
O10 V3 O3 77.42(6) . . ?
O6 V3 V1 137.30(9) . 3_765 ?
O4 V3 V1 33.88(7) 3_765 3_765 ?
O1 V3 V1 87.54(7) . 3_765 ?
O9 V3 V1 82.21(6) . 3_765 ?
O10 V3 V1 124.95(6) . 3_765 ?
O3 V3 V1 47.688(14) . 3_765 ?
O6 V3 V2 137.38(9) . 3_765 ?
O4 V3 V2 87.92(7) 3_765 3_765 ?
O1 V3 V2 33.47(7) . 3_765 ?
O9 V3 V2 124.89(6) . 3_765 ?
O10 V3 V2 80.90(6) . 3_765 ?
O3 V3 V2 47.397(14) . 3_765 ?
V1 V3 V2 66.079(17) 3_765 3_765 ?
V2 O1 V3 112.40(11) 3_765 . ?
V2 O2 V1 112.82(12) 3_765 . ?
V3 O3 V3 180.00(2) 3_765 . ?
V3 O3 V2 94.684(19) 3_765 3_765 ?
V3 O3 V2 85.316(19) . 3_765 ?
V3 O3 V2 85.316(19) 3_765 . ?
V3 O3 V2 94.684(19) . . ?
V2 O3 V2 180.00(3) 3_765 . ?
V3 O3 V1 84.95(2) 3_765 . ?
V3 O3 V1 95.05(2) . . ?
V2 O3 V1 85.16(2) 3_765 . ?
V2 O3 V1 94.84(2) . . ?
V3 O3 V1 95.05(2) 3_765 3_765 ?
V3 O3 V1 84.95(2) . 3_765 ?
V2 O3 V1 94.84(2) 3_765 3_765 ?
V2 O3 V1 85.16(2) . 3_765 ?
V1 O3 V1 180.0 . 3_765 ?
V3 O4 V1 112.27(11) 3_765 . ?
C2 O8 V1 118.61(19) . . ?
C2 O8 V2 118.50(19) . . ?
V1 O8 V2 109.53(10) . . ?
C1 O9 V3 118.41(19) . . ?
C1 O9 V2 119.64(19) . . ?
V3 O9 V2 109.60(9) . . ?
C4 O10 V1 118.06(19) . . ?
C4 O10 V3 118.62(19) . . ?
V1 O10 V3 109.91(10) . . ?
C6 O11 C5 122.4(3) . . ?
C18 N1 C26 108.9(3) . . ?
C18 N1 C22 108.8(2) . . ?
C26 N1 C22 111.0(3) . . ?
C18 N1 C14 111.0(3) . . ?
C26 N1 C14 108.3(2) . . ?
C22 N1 C14 108.9(3) . . ?
O9 C1 C3 111.7(2) . . ?
O9 C1 H1A 109.3 . . ?
C3 C1 H1A 109.3 . . ?
O9 C1 H1B 109.3 . . ?
C3 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
O8 C2 C3 112.3(3) . . ?
O8 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
O8 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 111.5(3) . . ?
C4 C3 C1 110.1(3) . . ?
C2 C3 C1 109.6(3) . . ?
C4 C3 C5 109.1(3) . . ?
C2 C3 C5 109.1(3) . . ?
C1 C3 C5 107.3(3) . . ?
O10 C4 C3 112.0(3) . . ?
O10 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
O10 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O11 C5 C3 106.8(3) . . ?
O11 C5 H5A 110.4 . . ?
C3 C5 H5A 110.4 . . ?
O11 C5 H5B 110.4 . . ?
C3 C5 H5B 110.4 . . ?
H5A C5 H5B 108.6 . . ?
O12 C6 O11 119.7(5) . . ?
O12 C6 C7 124.5(5) . . ?
O11 C6 C7 115.5(4) . . ?
C12B C7 C8B 116.3(8) . . ?
C12B C7 C6 104.7(6) . . ?
C8B C7 C6 110.4(7) . . ?
C12B C7 C8A 68.3(6) . . ?
C8B C7 C8A 131.1(7) . . ?
C6 C7 C8A 115.0(5) . . ?
C12B C7 C12A 45.2(5) . . ?
C8B C7 C12A 72.8(6) . . ?
C6 C7 C12A 111.1(4) . . ?
C8A C7 C12A 105.5(5) . . ?
C12B C7 H7A 144.2 . . ?
C8B C7 H7A 37.8 . . ?
C6 C7 H7A 108.3 . . ?
C8A C7 H7A 108.3 . . ?
C12A C7 H7A 108.3 . . ?
C12B C7 H7B 109.0 . . ?
C8B C7 H7B 107.6 . . ?
C6 C7 H7B 108.6 . . ?
C8A C7 H7B 40.9 . . ?
C12A C7 H7B 137.2 . . ?
H7A C7 H7B 73.0 . . ?
C9A C8A C7 113.3(7) . . ?
C9A C8A H7B 150.0 . . ?
C7 C8A H7B 38.2 . . ?
C9A C8A H8AA 108.9 . . ?
C7 C8A H8AA 108.9 . . ?
H7B C8A H8AA 93.6 . . ?
C9A C8A H8AB 108.9 . . ?
C7 C8A H8AB 108.9 . . ?
H7B C8A H8AB 81.4 . . ?
H8AA C8A H8AB 107.7 . . ?
C10A C9A C8A 123.7(9) . . ?
C10A C9A H9A 118.1 . . ?
C8A C9A H9A 118.1 . . ?
C9A C10A C11A 125.2(10) . . ?
C9A C10A H10 117.4 . . ?
C11A C10A H10 117.4 . . ?
C10A C11A C12A 111.4(10) . . ?
C10A C11A H11A 109.4 . . ?
C12A C11A H11A 109.4 . . ?
C10A C11A H11B 109.4 . . ?
C12A C11A H11B 109.4 . . ?
H11A C11A H11B 108.0 . . ?
C13A C12A C11A 117.8(11) . . ?
C13A C12A C7 106.2(9) . . ?
C11A C12A C7 111.5(6) . . ?
C13A C12A H12 106.9 . . ?
C11A C12A H12 106.9 . . ?
C7 C12A H12 106.9 . . ?
O13A C13A O14A 116.8(9) . . ?
O13A C13A C12A 119.1(14) . . ?
O14A C13A C12A 120.4(15) . . ?
C13A O14A H14C 109.5 . . ?
C7 C8B C9B 106.9(9) . . ?
C7 C8B H8BA 110.3 . . ?
C9B C8B H8BA 110.3 . . ?
C7 C8B H8BB 110.3 . . ?
C9B C8B H8BB 110.3 . . ?
H8BA C8B H8BB 108.6 . . ?
C10B C9B C8B 112.4(17) . . ?
C10B C9B H9B 123.8 . . ?
C8B C9B H9B 123.8 . . ?
C9B C10B C11B 135.0(18) . . ?
C9B C10B H10A 112.5 . . ?
C11B C10B H10A 112.5 . . ?
C10B C11B C12B 115.7(13) . . ?
C10B C11B H11C 108.4 . . ?
C12B C11B H11C 108.4 . . ?
C10B C11B H11D 108.4 . . ?
C12B C11B H11D 108.4 . . ?
H11C C11B H11D 107.4 . . ?
C7 C12B C11B 111.5(10) . . ?
C7 C12B C13B 116.8(9) . . ?
C11B C12B C13B 114.4(10) . . ?
C7 C12B H12A 104.1 . . ?
C11B C12B H12A 104.1 . . ?
C13B C12B H12A 104.1 . . ?
O14B C13B O13B 124.4(13) . . ?
O14B C13B C12B 119.5(13) . . ?
O13B C13B C12B 116.1(11) . . ?
C13B O13B H13A 109.5 . . ?
C15 C14 N1 116.4(3) . . ?
C15 C14 H14A 108.2 . . ?
N1 C14 H14A 108.2 . . ?
C15 C14 H14B 108.2 . . ?
N1 C14 H14B 108.2 . . ?
H14A C14 H14B 107.3 . . ?
C14 C15 C16 109.3(3) . . ?
C14 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
C17 C16 C15 114.0(4) . . ?
C17 C16 H16A 108.7 . . ?
C15 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 116.0(3) . . ?
C19 C18 H18A 108.3 . . ?
N1 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
N1 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C18 C19 C20 109.8(3) . . ?
C18 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C21 C20 C19 112.2(3) . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N1 115.6(3) . . ?
C23 C22 H22A 108.4 . . ?
N1 C22 H22A 108.4 . . ?
C23 C22 H22B 108.4 . . ?
N1 C22 H22B 108.4 . . ?
H22A C22 H22B 107.5 . . ?
C22 C23 C24 109.5(3) . . ?
C22 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
C23 C24 C25 113.0(4) . . ?
C23 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C26 C27 115.6(3) . . ?
N1 C26 H26A 108.4 . . ?
C27 C26 H26A 108.4 . . ?
N1 C26 H26B 108.4 . . ?
C27 C26 H26B 108.4 . . ?
H26A C26 H26B 107.4 . . ?
C28 C27 C26 111.3(3) . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 C29 110.9(3) . . ?
C27 C28 H28A 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C29 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
O6 V3 O1 V2 -173.73(13) . . . 3_765 ?
O4 V3 O1 V2 81.28(13) 3_765 . . 3_765 ?
O9 V3 O1 V2 -14.3(3) . . . 3_765 ?
O10 V3 O1 V2 -77.30(13) . . . 3_765 ?
O3 V3 O1 V2 0.36(10) . . . 3_765 ?
V1 V3 O1 V2 47.87(11) 3_765 . . 3_765 ?
O5 V1 O2 V2 173.41(12) . . . 3_765 ?
O4 V1 O2 V2 -81.13(13) . . . 3_765 ?
O10 V1 O2 V2 76.79(13) . . . 3_765 ?
O8 V1 O2 V2 11.7(3) . . . 3_765 ?
O3 V1 O2 V2 -0.63(10) . . . 3_765 ?
V3 V1 O2 V2 -47.86(11) 3_765 . . 3_765 ?
O6 V3 O3 V3 -123(100) . . . 3_765 ?
O4 V3 O3 V3 11(100) 3_765 . . 3_765 ?
O1 V3 O3 V3 105(100) . . . 3_765 ?
O9 V3 O3 V3 -80(100) . . . 3_765 ?
O10 V3 O3 V3 -165(100) . . . 3_765 ?
V1 V3 O3 V3 10(100) 3_765 . . 3_765 ?
V2 V3 O3 V3 106(100) 3_765 . . 3_765 ?
O6 V3 O3 V2 131.4(7) . . . 3_765 ?
O4 V3 O3 V2 -94.96(7) 3_765 . . 3_765 ?
O1 V3 O3 V2 -0.27(8) . . . 3_765 ?
O9 V3 O3 V2 174.13(7) . . . 3_765 ?
O10 V3 O3 V2 89.15(6) . . . 3_765 ?
V1 V3 O3 V2 -95.29(2) 3_765 . . 3_765 ?
O6 V3 O3 V2 -48.6(7) . . . . ?
O4 V3 O3 V2 85.04(7) 3_765 . . . ?
O1 V3 O3 V2 179.73(8) . . . . ?
O9 V3 O3 V2 -5.87(7) . . . . ?
O10 V3 O3 V2 -90.85(6) . . . . ?
V1 V3 O3 V2 84.71(2) 3_765 . . . ?
V2 V3 O3 V2 180.0 3_765 . . . ?
O6 V3 O3 V1 46.7(7) . . . . ?
O4 V3 O3 V1 -179.67(7) 3_765 . . . ?
O1 V3 O3 V1 -84.98(8) . . . . ?
O9 V3 O3 V1 89.43(7) . . . . ?
O10 V3 O3 V1 4.44(6) . . . . ?
V1 V3 O3 V1 180.0 3_765 . . . ?
V2 V3 O3 V1 -84.71(2) 3_765 . . . ?
O6 V3 O3 V1 -133.3(7) . . . 3_765 ?
O4 V3 O3 V1 0.33(7) 3_765 . . 3_765 ?
O1 V3 O3 V1 95.02(8) . . . 3_765 ?
O9 V3 O3 V1 -90.57(7) . . . 3_765 ?
O10 V3 O3 V1 -175.56(6) . . . 3_765 ?
V2 V3 O3 V1 95.29(2) 3_765 . . 3_765 ?
O7 V2 O3 V3 -139.9(7) . . . 3_765 ?
O1 V2 O3 V3 -0.27(8) 3_765 . . 3_765 ?
O2 V2 O3 V3 95.96(7) 3_765 . . 3_765 ?
O9 V2 O3 V3 -174.18(7) . . . 3_765 ?
O8 V2 O3 V3 -89.70(6) . . . 3_765 ?
V1 V2 O3 V3 95.48(2) 3_765 . . 3_765 ?
O7 V2 O3 V3 40.1(7) . . . . ?
O1 V2 O3 V3 179.73(8) 3_765 . . . ?
O2 V2 O3 V3 -84.04(7) 3_765 . . . ?
O9 V2 O3 V3 5.82(7) . . . . ?
O8 V2 O3 V3 90.30(6) . . . . ?
V3 V2 O3 V3 180.0 3_765 . . . ?
V1 V2 O3 V3 -84.52(2) 3_765 . . . ?
O7 V2 O3 V2 55(100) . . . 3_765 ?
O1 V2 O3 V2 -165(100) 3_765 . . 3_765 ?
O2 V2 O3 V2 -69(100) 3_765 . . 3_765 ?
O9 V2 O3 V2 21(100) . . . 3_765 ?
O8 V2 O3 V2 106(100) . . . 3_765 ?
V3 V2 O3 V2 -165(100) 3_765 . . 3_765 ?
V1 V2 O3 V2 -69(100) 3_765 . . 3_765 ?
O7 V2 O3 V1 -55.4(7) . . . . ?
O1 V2 O3 V1 84.24(8) 3_765 . . . ?
O2 V2 O3 V1 -179.53(7) 3_765 . . . ?
O9 V2 O3 V1 -89.66(7) . . . . ?
O8 V2 O3 V1 -5.18(6) . . . . ?
V3 V2 O3 V1 84.52(2) 3_765 . . . ?
V1 V2 O3 V1 180.0 3_765 . . . ?
O7 V2 O3 V1 124.6(7) . . . 3_765 ?
O1 V2 O3 V1 -95.76(8) 3_765 . . 3_765 ?
O2 V2 O3 V1 0.47(7) 3_765 . . 3_765 ?
O9 V2 O3 V1 90.34(7) . . . 3_765 ?
O8 V2 O3 V1 174.82(6) . . . 3_765 ?
V3 V2 O3 V1 -95.48(2) 3_765 . . 3_765 ?
O5 V1 O3 V3 136.4(7) . . . 3_765 ?
O4 V1 O3 V3 0.33(7) . . . 3_765 ?
O2 V1 O3 V3 -94.68(7) . . . 3_765 ?
O10 V1 O3 V3 175.55(6) . . . 3_765 ?
O8 V1 O3 V3 90.04(6) . . . 3_765 ?
V2 V1 O3 V3 -95.150(19) 3_765 . . 3_765 ?
O5 V1 O3 V3 -43.6(7) . . . . ?
O4 V1 O3 V3 -179.67(7) . . . . ?
O2 V1 O3 V3 85.32(7) . . . . ?
O10 V1 O3 V3 -4.45(6) . . . . ?
O8 V1 O3 V3 -89.96(6) . . . . ?
V3 V1 O3 V3 180.0 3_765 . . . ?
V2 V1 O3 V3 84.850(19) 3_765 . . . ?
O5 V1 O3 V2 -128.4(7) . . . 3_765 ?
O4 V1 O3 V2 95.48(7) . . . 3_765 ?
O2 V1 O3 V2 0.47(7) . . . 3_765 ?
O10 V1 O3 V2 -89.30(6) . . . 3_765 ?
O8 V1 O3 V2 -174.81(6) . . . 3_765 ?
V3 V1 O3 V2 95.150(19) 3_765 . . 3_765 ?
O5 V1 O3 V2 51.6(7) . . . . ?
O4 V1 O3 V2 -84.52(7) . . . . ?
O2 V1 O3 V2 -179.53(7) . . . . ?
O10 V1 O3 V2 90.70(6) . . . . ?
O8 V1 O3 V2 5.19(6) . . . . ?
V3 V1 O3 V2 -84.850(19) 3_765 . . . ?
V2 V1 O3 V2 180.0 3_765 . . . ?
O5 V1 O3 V1 -17(72) . . . 3_765 ?
O4 V1 O3 V1 -153(72) . . . 3_765 ?
O2 V1 O3 V1 112(72) . . . 3_765 ?
O10 V1 O3 V1 22(72) . . . 3_765 ?
O8 V1 O3 V1 -63(72) . . . 3_765 ?
V3 V1 O3 V1 -153(72) 3_765 . . 3_765 ?
V2 V1 O3 V1 112(72) 3_765 . . 3_765 ?
O5 V1 O4 V3 -175.13(12) . . . 3_765 ?
O2 V1 O4 V3 79.71(13) . . . 3_765 ?
O10 V1 O4 V3 -12.9(3) . . . 3_765 ?
O8 V1 O4 V3 -78.12(12) . . . 3_765 ?
O3 V1 O4 V3 -0.44(10) . . . 3_765 ?
V2 V1 O4 V3 46.63(10) 3_765 . . 3_765 ?
O5 V1 O8 C2 -40.3(2) . . . . ?
O4 V1 O8 C2 -144.2(2) . . . . ?
O2 V1 O8 C2 121.9(3) . . . . ?
O10 V1 O8 C2 55.9(2) . . . . ?
O3 V1 O8 C2 134.3(2) . . . . ?
V3 V1 O8 C2 -177.7(2) 3_765 . . . ?
V2 V1 O8 C2 129.66(19) 3_765 . . . ?
O5 V1 O8 V2 179.35(11) . . . . ?
O4 V1 O8 V2 75.40(11) . . . . ?
O2 V1 O8 V2 -18.5(3) . . . . ?
O10 V1 O8 V2 -84.49(11) . . . . ?
O3 V1 O8 V2 -6.08(7) . . . . ?
V3 V1 O8 V2 41.96(8) 3_765 . . . ?
V2 V1 O8 V2 -10.71(12) 3_765 . . . ?
O7 V2 O8 C2 39.8(2) . . . . ?
O1 V2 O8 C2 143.9(2) 3_765 . . . ?
O2 V2 O8 C2 -119.2(3) 3_765 . . . ?
O9 V2 O8 C2 -55.7(2) . . . . ?
O3 V2 O8 C2 -134.3(2) . . . . ?
V3 V2 O8 C2 177.7(2) 3_765 . . . ?
V1 V2 O8 C2 -129.67(18) 3_765 . . . ?
O7 V2 O8 V1 -179.80(11) . . . . ?
O1 V2 O8 V1 -75.64(11) 3_765 . . . ?
O2 V2 O8 V1 21.2(3) 3_765 . . . ?
O9 V2 O8 V1 84.74(10) . . . . ?
O3 V2 O8 V1 6.10(7) . . . . ?
V3 V2 O8 V1 -41.90(8) 3_765 . . . ?
V1 V2 O8 V1 10.75(13) 3_765 . . . ?
O6 V3 O9 C1 39.5(2) . . . . ?
O4 V3 O9 C1 143.2(2) 3_765 . . . ?
O1 V3 O9 C1 -120.4(3) . . . . ?
O10 V3 O9 C1 -56.6(2) . . . . ?
O3 V3 O9 C1 -135.3(2) . . . . ?
V1 V3 O9 C1 176.5(2) 3_765 . . . ?
V2 V3 O9 C1 -130.01(19) 3_765 . . . ?
O6 V3 O9 V2 -178.37(12) . . . . ?
O4 V3 O9 V2 -74.69(11) 3_765 . . . ?
O1 V3 O9 V2 21.7(3) . . . . ?
O10 V3 O9 V2 85.55(11) . . . . ?
O3 V3 O9 V2 6.87(8) . . . . ?
V1 V3 O9 V2 -41.40(9) 3_765 . . . ?
V2 V3 O9 V2 12.13(14) 3_765 . . . ?
O7 V2 O9 C1 -41.0(2) . . . . ?
O1 V2 O9 C1 118.6(3) 3_765 . . . ?
O2 V2 O9 C1 -143.8(2) 3_765 . . . ?
O8 V2 O9 C1 55.7(2) . . . . ?
O3 V2 O9 C1 134.7(2) . . . . ?
V3 V2 O9 C1 129.6(2) 3_765 . . . ?
V1 V2 O9 C1 -177.1(2) 3_765 . . . ?
O7 V2 O9 V3 177.44(12) . . . . ?
O1 V2 O9 V3 -23.0(3) 3_765 . . . ?
O2 V2 O9 V3 74.56(11) 3_765 . . . ?
O8 V2 O9 V3 -85.88(11) . . . . ?
O3 V2 O9 V3 -6.87(8) . . . . ?
V3 V2 O9 V3 -12.05(14) 3_765 . . . ?
V1 V2 O9 V3 41.32(9) 3_765 . . . ?
O5 V1 O10 C4 40.1(2) . . . . ?
O4 V1 O10 C4 -122.5(3) . . . . ?
O2 V1 O10 C4 143.7(2) . . . . ?
O8 V1 O10 C4 -56.5(2) . . . . ?
O3 V1 O10 C4 -135.2(2) . . . . ?
V3 V1 O10 C4 -131.20(19) 3_765 . . . ?
V2 V1 O10 C4 176.7(2) 3_765 . . . ?
O5 V1 O10 V3 -179.50(11) . . . . ?
O4 V1 O10 V3 17.9(3) . . . . ?
O2 V1 O10 V3 -75.88(11) . . . . ?
O8 V1 O10 V3 83.94(10) . . . . ?
O3 V1 O10 V3 5.22(7) . . . . ?
V3 V1 O10 V3 9.19(13) 3_765 . . . ?
V2 V1 O10 V3 -42.89(8) 3_765 . . . ?
O6 V3 O10 C4 -39.9(2) . . . . ?
O4 V3 O10 C4 123.7(3) 3_765 . . . ?
O1 V3 O10 C4 -143.9(2) . . . . ?
O9 V3 O10 C4 55.9(2) . . . . ?
O3 V3 O10 C4 134.9(2) . . . . ?
V1 V3 O10 C4 130.89(18) 3_765 . . . ?
V2 V3 O10 C4 -176.9(2) 3_765 . . . ?
O6 V3 O10 V1 179.95(11) . . . . ?
O4 V3 O10 V1 -16.4(3) 3_765 . . . ?
O1 V3 O10 V1 75.96(11) . . . . ?
O9 V3 O10 V1 -84.29(10) . . . . ?
O3 V3 O10 V1 -5.24(7) . . . . ?
V1 V3 O10 V1 -9.25(13) 3_765 . . . ?
V2 V3 O10 V1 42.95(8) 3_765 . . . ?
V3 O9 C1 C3 69.8(3) . . . . ?
V2 O9 C1 C3 -68.5(3) . . . . ?
V1 O8 C2 C3 -67.0(3) . . . . ?
V2 O8 C2 C3 69.8(3) . . . . ?
O8 C2 C3 C4 59.8(4) . . . . ?
O8 C2 C3 C1 -62.4(3) . . . . ?
O8 C2 C3 C5 -179.6(3) . . . . ?
O9 C1 C3 C4 -61.9(3) . . . . ?
O9 C1 C3 C2 61.1(3) . . . . ?
O9 C1 C3 C5 179.5(3) . . . . ?
V1 O10 C4 C3 68.7(3) . . . . ?
V3 O10 C4 C3 -68.3(3) . . . . ?
C2 C3 C4 O10 -60.6(4) . . . . ?
C1 C3 C4 O10 61.2(3) . . . . ?
C5 C3 C4 O10 178.8(3) . . . . ?
C6 O11 C5 C3 164.3(4) . . . . ?
C4 C3 C5 O11 54.7(4) . . . . ?
C2 C3 C5 O11 -67.3(4) . . . . ?
C1 C3 C5 O11 174.0(3) . . . . ?
C5 O11 C6 O12 4.4(10) . . . . ?
C5 O11 C6 C7 178.4(4) . . . . ?
O12 C6 C7 C12B -109.0(9) . . . . ?
O11 C6 C7 C12B 77.4(7) . . . . ?
O12 C6 C7 C8B 16.9(11) . . . . ?
O11 C6 C7 C8B -156.7(7) . . . . ?
O12 C6 C7 C8A 178.4(9) . . . . ?
O11 C6 C7 C8A 4.8(8) . . . . ?
O12 C6 C7 C12A -61.8(10) . . . . ?
O11 C6 C7 C12A 124.5(5) . . . . ?
C12B C7 C8A C9A -18.8(9) . . . . ?
C8B C7 C8A C9A -125.5(11) . . . . ?
C6 C7 C8A C9A 77.8(9) . . . . ?
C12A C7 C8A C9A -45.0(9) . . . . ?
C7 C8A C9A C10A 14.8(17) . . . . ?
C8A C9A C10A C11A 5(2) . . . . ?
C9A C10A C11A C12A 12(2) . . . . ?
C10A C11A C12A C13A -168.4(12) . . . . ?
C10A C11A C12A C7 -45.3(13) . . . . ?
C12B C7 C12A C13A 156.0(13) . . . . ?
C8B C7 C12A C13A -39.8(11) . . . . ?
C6 C7 C12A C13A 66.0(10) . . . . ?
C8A C7 C12A C13A -168.7(10) . . . . ?
C12B C7 C12A C11A 26.5(10) . . . . ?
C8B C7 C12A C11A -169.3(10) . . . . ?
C6 C7 C12A C11A -63.5(8) . . . . ?
C8A C7 C12A C11A 61.8(9) . . . . ?
C11A C12A C13A O13A -172.5(14) . . . . ?
C7 C12A C13A O13A 61.7(17) . . . . ?
C11A C12A C13A O14A -15(2) . . . . ?
C7 C12A C13A O14A -140.7(13) . . . . ?
C12B C7 C8B C9B 43.6(13) . . . . ?
C6 C7 C8B C9B -75.4(11) . . . . ?
C8A C7 C8B C9B 127.1(10) . . . . ?
C12A C7 C8B C9B 31.2(9) . . . . ?
C7 C8B C9B C10B -19(2) . . . . ?
C8B C9B C10B C11B 8(3) . . . . ?
C9B C10B C11B C12B -18(3) . . . . ?
C8B C7 C12B C11B -55.1(13) . . . . ?
C6 C7 C12B C11B 67.1(11) . . . . ?
C8A C7 C12B C11B 178.6(12) . . . . ?
C12A C7 C12B C11B -38.2(9) . . . . ?
C8B C7 C12B C13B 170.7(11) . . . . ?
C6 C7 C12B C13B -67.1(11) . . . . ?
C8A C7 C12B C13B 44.3(10) . . . . ?
C12A C7 C12B C13B -172.4(15) . . . . ?
C10B C11B C12B C7 38.8(19) . . . . ?
C10B C11B C12B C13B 174.2(15) . . . . ?
C7 C12B C13B O14B 133.7(12) . . . . ?
C11B C12B C13B O14B 1(2) . . . . ?
C7 C12B C13B O13B -48.3(17) . . . . ?
C11B C12B C13B O13B 178.8(13) . . . . ?
C18 N1 C14 C15 -54.7(4) . . . . ?
C26 N1 C14 C15 -174.1(3) . . . . ?
C22 N1 C14 C15 65.0(4) . . . . ?
N1 C14 C15 C16 -179.5(3) . . . . ?
C14 C15 C16 C17 176.6(4) . . . . ?
C26 N1 C18 C19 69.6(4) . . . . ?
C22 N1 C18 C19 -169.3(3) . . . . ?
C14 N1 C18 C19 -49.5(4) . . . . ?
N1 C18 C19 C20 -175.9(3) . . . . ?
C18 C19 C20 C21 -170.2(4) . . . . ?
C18 N1 C22 C23 -67.4(4) . . . . ?
C26 N1 C22 C23 52.4(4) . . . . ?
C14 N1 C22 C23 171.5(3) . . . . ?
N1 C22 C23 C24 -178.0(3) . . . . ?
C22 C23 C24 C25 178.4(3) . . . . ?
C18 N1 C26 C27 171.9(3) . . . . ?
C22 N1 C26 C27 52.2(3) . . . . ?
C14 N1 C26 C27 -67.3(3) . . . . ?
N1 C26 C27 C28 174.7(3) . . . . ?
C26 C27 C28 C29 -178.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.842
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_exp_3913
_database_code_depnum_ccdc_archive 'CCDC 1484789'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_audit_creation_date             2016-03-17
_audit_creation_method           
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(C13 H13 O13.5 V3), 2(C16 H36 N)'
_chemical_formula_sum            'C58 H98 N2 O27 V6'
_chemical_formula_weight         1561.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.3754(2)
_cell_length_b                   16.3585(3)
_cell_length_c                   18.4016(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.0881(18)
_cell_angle_gamma                90.00
_cell_volume                     3381.27(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    103.7
_cell_measurement_theta_max      29.2539
_cell_measurement_theta_min      2.9235
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15669
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.93
_diffrn_ambient_temperature      103.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   34.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
  2 omega  -26.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827  -37.0000  -30.0000 43

#__ type_ start__ end____ width___ exp.time_
  3 omega   52.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   52.0000  175.0000 38

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000   90.0000 52

#__ type_ start__ end____ width___ exp.time_
  5 omega   -5.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000  -30.0000 68
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0627220000
_diffrn_orient_matrix_UB_12      -0.0050281000
_diffrn_orient_matrix_UB_13      0.0055761000
_diffrn_orient_matrix_UB_21      0.0063408000
_diffrn_orient_matrix_UB_22      0.0340407000
_diffrn_orient_matrix_UB_23      0.0241828000
_diffrn_orient_matrix_UB_31      -0.0037628000
_diffrn_orient_matrix_UB_32      -0.0263745000
_diffrn_orient_matrix_UB_33      0.0301315000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5314
_reflns_number_total             6633
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0474P)²+5.6236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1213
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.82989(5) 0.95936(3) 0.03614(3) 0.01340(14) Uani 1 1 d . . .
V2 V 0.96403(5) 1.13343(3) 0.00993(3) 0.01333(14) Uani 1 1 d . . .
V3 V 0.92808(5) 0.99337(3) -0.12105(3) 0.01292(14) Uani 1 1 d . . .
O5 O 0.89195(18) 0.86033(13) 0.02495(12) 0.0149(5) Uani 1 1 d . . .
O10 O 0.81433(18) 1.08287(13) 0.03272(12) 0.0132(5) Uani 1 1 d . . .
O7 O 0.96670(19) 0.88487(13) -0.10347(12) 0.0147(5) Uani 1 1 d . . .
O6 O 0.92453(19) 0.97586(14) 0.12828(12) 0.0152(5) Uani 1 1 d . . .
O4 O 1.0000 1.0000 0.0000 0.0112(6) Uani 1 2 d S . .
O1 O 0.91978(19) 1.22706(14) 0.00918(12) 0.0167(5) Uani 1 1 d . . .
O8 O 0.78165(18) 0.97022(13) -0.07194(12) 0.0129(5) Uani 1 1 d . . .
O9 O 0.89005(18) 1.10897(13) -0.09659(12) 0.0122(5) Uani 1 1 d . . .
O2 O 0.7000(2) 0.94131(14) 0.05590(13) 0.0181(5) Uani 1 1 d . . .
O3 O 0.85825(19) 0.99239(14) -0.20491(12) 0.0166(5) Uani 1 1 d . . .
O11 O 0.5590(2) 1.22565(15) -0.09143(14) 0.0261(6) Uani 1 1 d . . .
N1 N 1.1136(2) 1.19442(17) -0.27666(15) 0.0185(6) Uani 1 1 d . . .
C18 C 1.2099(3) 1.2459(2) -0.30410(19) 0.0208(8) Uani 1 1 d . . .
H18A H 1.1840 1.3024 -0.3065 0.025 Uiso 1 1 calc R . .
H18B H 1.2815 1.2428 -0.2678 0.025 Uiso 1 1 calc R . .
O14 O 0.3471(3) 1.49649(18) -0.19586(19) 0.0429(8) Uani 1 1 d . . .
H14 H 0.2757 1.4930 -0.2115 0.064 Uiso 1 1 calc R . .
C4 C 0.6776(3) 1.1022(2) -0.08366(18) 0.0132(7) Uani 1 1 d . . .
C3 C 0.7023(3) 1.1178(2) -0.00026(18) 0.0151(7) Uani 1 1 d . . .
H3A H 0.7034 1.1762 0.0089 0.018 Uiso 1 1 calc R . .
H3B H 0.6387 1.0941 0.0223 0.018 Uiso 1 1 calc R . .
C5 C 0.5569(3) 1.1409(2) -0.11432(19) 0.0175(7) Uani 1 1 d . . .
H5A H 0.5428 1.1374 -0.1676 0.021 Uiso 1 1 calc R . .
H5B H 0.4934 1.1120 -0.0957 0.021 Uiso 1 1 calc R . .
C15 C 1.2637(3) 1.0780(2) -0.24086(19) 0.0209(8) Uani 1 1 d . . .
H15A H 1.2747 1.0938 -0.1894 0.025 Uiso 1 1 calc R . .
H15B H 1.3244 1.1050 -0.2638 0.025 Uiso 1 1 calc R . .
C13 C 0.3856(3) 1.4261(3) -0.1631(2) 0.0282(9) Uani 1 1 d . . .
C19 C 1.2419(3) 1.2230(2) -0.3777(2) 0.0221(8) Uani 1 1 d . . .
H19A H 1.1741 1.2313 -0.4161 0.027 Uiso 1 1 calc R . .
H19B H 1.2647 1.1658 -0.3778 0.027 Uiso 1 1 calc R . .
C1 C 0.6709(3) 1.0107(2) -0.09903(18) 0.0140(7) Uani 1 1 d . . .
H1A H 0.6080 0.9870 -0.0758 0.017 Uiso 1 1 calc R . .
H1B H 0.6510 1.0018 -0.1517 0.017 Uiso 1 1 calc R . .
C2 C 0.7737(3) 1.1409(2) -0.12233(18) 0.0143(7) Uani 1 1 d . . .
H2A H 0.7539 1.1313 -0.1749 0.017 Uiso 1 1 calc R . .
H2B H 0.7743 1.1995 -0.1143 0.017 Uiso 1 1 calc R . .
C23 C 1.0562(3) 1.3051(2) -0.1888(2) 0.0251(8) Uani 1 1 d . . .
H23A H 0.9716 1.3049 -0.2077 0.030 Uiso 1 1 calc R . .
H23B H 1.0943 1.3440 -0.2174 0.030 Uiso 1 1 calc R . .
O13 O 0.3329(3) 1.3636(2) -0.1679(2) 0.0598(10) Uani 1 1 d . . .
C16 C 1.2758(3) 0.9855(2) -0.2472(2) 0.0253(8) Uani 1 1 d . . .
H16A H 1.2662 0.9702 -0.2987 0.030 Uiso 1 1 calc R . .
H16B H 1.2134 0.9589 -0.2255 0.030 Uiso 1 1 calc R . .
C22 C 1.1072(3) 1.2205(2) -0.19720(18) 0.0204(8) Uani 1 1 d . . .
H22A H 1.0590 1.1810 -0.1758 0.025 Uiso 1 1 calc R . .
H22B H 1.1868 1.2185 -0.1691 0.025 Uiso 1 1 calc R . .
C26 C 0.9952(3) 1.2101(2) -0.32677(19) 0.0212(8) Uani 1 1 d . . .
H26A H 0.9785 1.2683 -0.3269 0.025 Uiso 1 1 calc R . .
H26B H 1.0034 1.1946 -0.3766 0.025 Uiso 1 1 calc R . .
C17 C 1.3972(3) 0.9562(3) -0.2082(2) 0.0340(10) Uani 1 1 d . . .
H17A H 1.4590 0.9842 -0.2281 0.051 Uiso 1 1 calc R . .
H17B H 1.4043 0.8984 -0.2155 0.051 Uiso 1 1 calc R . .
H17C H 1.4043 0.9675 -0.1565 0.051 Uiso 1 1 calc R . .
C21 C 1.3887(3) 1.2599(3) -0.4643(2) 0.0324(10) Uani 1 1 d . . .
H21A H 1.3244 1.2686 -0.5041 0.049 Uiso 1 1 calc R . .
H21B H 1.4152 1.2043 -0.4650 0.049 Uiso 1 1 calc R . .
H21C H 1.4534 1.2959 -0.4699 0.049 Uiso 1 1 calc R . .
C14 C 1.1410(3) 1.1039(2) -0.27860(19) 0.0195(7) Uani 1 1 d . . .
H14A H 1.1319 1.0869 -0.3297 0.023 Uiso 1 1 calc R . .
H14B H 1.0821 1.0747 -0.2559 0.023 Uiso 1 1 calc R . .
C6 C 0.5510(4) 1.2849(3) -0.1400(2) 0.0356(10) Uani 1 1 d . . .
C20 C 1.3464(3) 1.2773(2) -0.3918(2) 0.0270(9) Uani 1 1 d . . .
H20A H 1.3222 1.3341 -0.3910 0.032 Uiso 1 1 calc R . .
H20B H 1.4124 1.2694 -0.3520 0.032 Uiso 1 1 calc R . .
C11 C 0.5465(4) 1.5106(3) -0.0885(2) 0.0355(10) Uani 1 1 d . . .
H11 H 0.4997 1.5569 -0.0993 0.043 Uiso 1 1 calc R . .
O12 O 0.5328(4) 1.2737(2) -0.20607(18) 0.0629(11) Uani 1 1 d . . .
C28 C 0.7722(3) 1.1938(3) -0.3505(2) 0.0360(10) Uani 1 1 d . . .
H28A H 0.7805 1.1940 -0.4022 0.043 Uiso 1 1 calc R . .
H28B H 0.7096 1.1553 -0.3443 0.043 Uiso 1 1 calc R . .
C29 C 0.7374(4) 1.2744(3) -0.3301(3) 0.0558(14) Uani 1 1 d . . .
H29A H 0.6610 1.2878 -0.3576 0.084 Uiso 1 1 calc R . .
H29B H 0.7952 1.3137 -0.3406 0.084 Uiso 1 1 calc R . .
H29C H 0.7328 1.2754 -0.2784 0.084 Uiso 1 1 calc R . .
C12 C 0.5076(4) 1.4354(3) -0.1189(2) 0.0338(10) Uani 1 1 d . . .
C9 C 0.7233(4) 1.4487(3) -0.0256(3) 0.0394(11) Uani 1 1 d . . .
H9 H 0.7947 1.4532 0.0067 0.047 Uiso 1 1 calc R . .
C7 C 0.5797(4) 1.3668(3) -0.1036(2) 0.0327(9) Uani 1 1 d . . .
C10 C 0.6541(4) 1.5165(3) -0.0424(2) 0.0371(10) Uani 1 1 d . . .
H10 H 0.6798 1.5669 -0.0226 0.044 Uiso 1 1 calc R . .
C25 C 1.0272(4) 1.4155(3) -0.0970(3) 0.0407(11) Uani 1 1 d . . .
H25A H 1.0663 1.4549 -0.1236 0.061 Uiso 1 1 calc R . .
H25B H 1.0413 1.4287 -0.0455 0.061 Uiso 1 1 calc R . .
H25C H 0.9431 1.4164 -0.1147 0.061 Uiso 1 1 calc R . .
C24 C 1.0757(4) 1.3312(2) -0.1084(2) 0.0293(9) Uani 1 1 d . . .
H24A H 1.0374 1.2920 -0.0802 0.035 Uiso 1 1 calc R . .
H24B H 1.1603 1.3304 -0.0896 0.035 Uiso 1 1 calc R . .
C27 C 0.8895(3) 1.1646(3) -0.3050(2) 0.0299(9) Uani 1 1 d . . .
H27A H 0.8870 1.1734 -0.2531 0.036 Uiso 1 1 calc R . .
H27B H 0.8989 1.1064 -0.3126 0.036 Uiso 1 1 calc R . .
C8 C 0.6885(4) 1.3732(3) -0.0559(2) 0.0354(10) Uani 1 1 d . . .
H8 H 0.7367 1.3275 -0.0448 0.042 Uiso 1 1 calc R . .


_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 V2 3.0243(8) 3_775 ?
V1 V3 3.0431(7) 3_775 ?
V1 O5 1.792(2) . ?
V1 O10 2.028(2) . ?
V1 O6 1.879(2) . ?
V1 O4 2.2439(5) . ?
V1 O8 1.986(2) . ?
V1 O2 1.604(2) . ?
V2 V1 3.0243(8) 3_775 ?
V2 V3 3.0327(8) 3_775 ?
V2 O5 1.854(2) 3_775 ?
V2 O10 1.996(2) . ?
V2 O7 1.801(2) 3_775 ?
V2 O4 2.2335(5) . ?
V2 O1 1.612(2) . ?
V2 O9 2.047(2) . ?
V3 V1 3.0431(7) 3_775 ?
V3 V2 3.0327(8) 3_775 ?
V3 O7 1.845(2) . ?
V3 O6 1.776(2) 3_775 ?
V3 O4 2.2511(5) . ?
V3 O8 2.052(2) . ?
V3 O9 2.007(2) . ?
V3 O3 1.620(2) . ?
O5 V2 1.854(2) 3_775 ?
O10 C3 1.441(4) . ?
O7 V2 1.801(2) 3_775 ?
O6 V3 1.776(2) 3_775 ?
O4 V1 2.2440(5) 3_775 ?
O4 V2 2.2335(5) 3_775 ?
O4 V3 2.2511(5) 3_775 ?
O8 C1 1.441(4) . ?
O9 C2 1.433(4) . ?
O11 C5 1.448(4) . ?
O11 C6 1.311(5) . ?
N1 C18 1.530(4) . ?
N1 C22 1.536(4) . ?
N1 C26 1.529(4) . ?
N1 C14 1.514(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.505(5) . ?
O14 H14 0.8200 . ?
O14 C13 1.340(5) . ?
C4 C3 1.537(4) . ?
C4 C5 1.536(4) . ?
C4 C1 1.524(5) . ?
C4 C2 1.531(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.526(5) . ?
C15 C14 1.518(4) . ?
C13 O13 1.181(5) . ?
C13 C12 1.501(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.538(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.517(5) . ?
C23 C24 1.523(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.528(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.521(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C20 1.517(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C6 O12 1.215(5) . ?
C6 C7 1.510(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.394(6) . ?
C11 C10 1.378(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.445(7) . ?
C28 C27 1.535(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C12 C7 1.393(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.367(6) . ?
C9 C8 1.386(6) . ?
C7 C8 1.404(5) . ?
C10 H10 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 C24 1.512(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C8 H8 0.9300 . ?

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
V2 V1 V3 65.980(18) 3_775 3_775 ?
O5 V1 V2 34.63(7) . 3_775 ?
O5 V1 V3 87.01(7) . 3_775 ?
O5 V1 O10 158.60(10) . . ?
O5 V1 O6 93.07(10) . . ?
O5 V1 O4 81.95(7) . . ?
O5 V1 O8 91.00(10) . . ?
O10 V1 V2 123.99(6) . 3_775 ?
O10 V1 V3 80.23(6) . 3_775 ?
O10 V1 O4 76.75(6) . . ?
O6 V1 V2 88.05(7) . 3_775 ?
O6 V1 V3 32.56(7) . 3_775 ?
O6 V1 O10 85.39(9) . . ?
O6 V1 O4 80.03(7) . . ?
O6 V1 O8 156.82(10) . . ?
O4 V1 V2 47.364(15) . 3_775 ?
O4 V1 V3 47.490(14) . 3_775 ?
O8 V1 V2 82.41(6) . 3_775 ?
O8 V1 V3 125.17(7) . 3_775 ?
O8 V1 O10 82.58(9) . . ?
O8 V1 O4 77.96(6) . . ?
O2 V1 V2 138.92(9) . 3_775 ?
O2 V1 V3 136.19(9) . 3_775 ?
O2 V1 O5 104.67(11) . . ?
O2 V1 O10 96.40(10) . . ?
O2 V1 O6 103.83(11) . . ?
O2 V1 O4 171.97(9) . . ?
O2 V1 O8 97.16(11) . . ?
V1 V2 V3 66.213(18) 3_775 3_775 ?
O5 V2 V1 33.31(7) 3_775 3_775 ?
O5 V2 V3 89.17(7) 3_775 3_775 ?
O5 V2 O10 157.69(10) 3_775 . ?
O5 V2 O4 80.92(7) 3_775 . ?
O5 V2 O9 86.06(9) 3_775 . ?
O10 V2 V1 125.15(7) . 3_775 ?
O10 V2 V3 80.96(6) . 3_775 ?
O10 V2 O4 77.63(6) . . ?
O10 V2 O9 83.39(9) . . ?
O7 V2 V1 86.73(7) 3_775 3_775 ?
O7 V2 V3 34.17(7) 3_775 3_775 ?
O7 V2 O5 93.60(10) 3_775 3_775 ?
O7 V2 O10 89.39(9) 3_775 . ?
O7 V2 O4 81.81(7) 3_775 . ?
O7 V2 O9 159.11(10) 3_775 . ?
O4 V2 V1 47.657(15) . 3_775 ?
O4 V2 V3 47.695(15) . 3_775 ?
O1 V2 V1 136.84(9) . 3_775 ?
O1 V2 V3 138.45(8) . 3_775 ?
O1 V2 O5 103.68(11) . 3_775 ?
O1 V2 O10 96.88(10) . . ?
O1 V2 O7 104.77(11) . 3_775 ?
O1 V2 O4 171.52(8) . . ?
O1 V2 O9 95.57(10) . . ?
O9 V2 V1 81.55(6) . 3_775 ?
O9 V2 V3 124.99(6) . 3_775 ?
O9 V2 O4 77.50(6) . . ?
V2 V3 V1 65.832(18) 3_775 3_775 ?
O7 V3 V1 89.04(7) . 3_775 ?
O7 V3 V2 33.27(7) . 3_775 ?
O7 V3 O4 80.42(7) . . ?
O7 V3 O8 86.13(9) . . ?
O7 V3 O9 157.08(10) . . ?
O6 V3 V1 34.71(7) 3_775 3_775 ?
O6 V3 V2 87.59(7) 3_775 3_775 ?
O6 V3 O7 94.84(10) 3_775 . ?
O6 V3 O4 81.98(7) 3_775 . ?
O6 V3 O8 157.99(10) 3_775 . ?
O6 V3 O9 89.38(10) 3_775 . ?
O4 V3 V1 47.292(14) . 3_775 ?
O4 V3 V2 47.204(15) . 3_775 ?
O8 V3 V1 123.52(6) . 3_775 ?
O8 V3 V2 81.20(6) . 3_775 ?
O8 V3 O4 76.49(6) . . ?
O9 V3 V1 81.66(6) . 3_775 ?
O9 V3 V2 124.88(6) . 3_775 ?
O9 V3 O4 77.89(6) . . ?
O9 V3 O8 81.74(9) . . ?
O3 V3 V1 139.40(8) . 3_775 ?
O3 V3 V2 136.11(9) . 3_775 ?
O3 V3 O7 103.00(11) . . ?
O3 V3 O6 104.97(11) . 3_775 ?
O3 V3 O4 171.81(8) . . ?
O3 V3 O8 96.18(10) . . ?
O3 V3 O9 97.61(10) . . ?
V1 O5 V2 112.06(11) . 3_775 ?
V2 O10 V1 110.24(10) . . ?
C3 O10 V1 118.37(18) . . ?
C3 O10 V2 118.34(18) . . ?
V2 O7 V3 112.56(12) 3_775 . ?
V3 O6 V1 112.73(12) 3_775 . ?
V1 O4 V1 180.0 3_775 . ?
V1 O4 V3 85.22(2) 3_775 . ?
V1 O4 V3 94.78(2) . . ?
V1 O4 V3 94.78(2) 3_775 3_775 ?
V1 O4 V3 85.22(2) . 3_775 ?
V2 O4 V1 84.98(2) . 3_775 ?
V2 O4 V1 84.98(2) 3_775 . ?
V2 O4 V1 95.02(2) 3_775 3_775 ?
V2 O4 V1 95.02(2) . . ?
V2 O4 V2 180.00(3) 3_775 . ?
V2 O4 V3 85.10(2) . 3_775 ?
V2 O4 V3 85.10(2) 3_775 . ?
V2 O4 V3 94.90(2) . . ?
V2 O4 V3 94.90(2) 3_775 3_775 ?
V3 O4 V3 180.000(1) . 3_775 ?
V1 O8 V3 110.03(10) . . ?
C1 O8 V1 118.41(18) . . ?
C1 O8 V3 119.29(18) . . ?
V3 O9 V2 109.18(10) . . ?
C2 O9 V2 117.65(18) . . ?
C2 O9 V3 119.36(18) . . ?
C6 O11 C5 120.9(3) . . ?
C18 N1 C22 107.8(3) . . ?
C26 N1 C18 108.5(2) . . ?
C26 N1 C22 111.0(3) . . ?
C14 N1 C18 111.6(3) . . ?
C14 N1 C22 109.6(2) . . ?
C14 N1 C26 108.4(3) . . ?
N1 C18 H18A 108.1 . . ?
N1 C18 H18B 108.1 . . ?
H18A C18 H18B 107.3 . . ?
C19 C18 N1 116.6(3) . . ?
C19 C18 H18A 108.1 . . ?
C19 C18 H18B 108.1 . . ?
C13 O14 H14 109.5 . . ?
C5 C4 C3 108.1(3) . . ?
C1 C4 C3 110.1(3) . . ?
C1 C4 C5 108.7(3) . . ?
C1 C4 C2 109.8(3) . . ?
C2 C4 C3 111.4(3) . . ?
C2 C4 C5 108.7(3) . . ?
O10 C3 C4 111.4(3) . . ?
O10 C3 H3A 109.4 . . ?
O10 C3 H3B 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O11 C5 C4 108.3(3) . . ?
O11 C5 H5A 110.0 . . ?
O11 C5 H5B 110.0 . . ?
C4 C5 H5A 110.0 . . ?
C4 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
H15A C15 H15B 108.3 . . ?
C16 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
C14 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
C14 C15 C16 109.3(3) . . ?
O14 C13 C12 111.4(3) . . ?
O13 C13 O14 125.7(4) . . ?
O13 C13 C12 122.9(4) . . ?
C18 C19 H19A 110.1 . . ?
C18 C19 H19B 110.1 . . ?
C18 C19 C20 108.1(3) . . ?
H19A C19 H19B 108.4 . . ?
C20 C19 H19A 110.1 . . ?
C20 C19 H19B 110.1 . . ?
O8 C1 C4 111.8(2) . . ?
O8 C1 H1A 109.3 . . ?
O8 C1 H1B 109.3 . . ?
C4 C1 H1A 109.3 . . ?
C4 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
O9 C2 C4 112.7(3) . . ?
O9 C2 H2A 109.1 . . ?
O9 C2 H2B 109.1 . . ?
C4 C2 H2A 109.1 . . ?
C4 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
H23A C23 H23B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.8(3) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.2(3) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
N1 C22 H22A 108.5 . . ?
N1 C22 H22B 108.5 . . ?
C23 C22 N1 115.2(3) . . ?
C23 C22 H22A 108.5 . . ?
C23 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
N1 C26 H26A 108.6 . . ?
N1 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 N1 114.6(3) . . ?
C27 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
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 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
N1 C14 C15 116.1(3) . . ?
N1 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
C15 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
O11 C6 C7 111.5(3) . . ?
O12 C6 O11 123.6(4) . . ?
O12 C6 C7 124.6(4) . . ?
C19 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 C19 113.6(3) . . ?
C21 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.3(4) . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
C29 C28 C27 113.1(4) . . ?
C27 C28 H28A 109.0 . . ?
C27 C28 H28B 109.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C11 C12 C13 121.0(4) . . ?
C7 C12 C13 119.5(4) . . ?
C7 C12 C11 119.3(4) . . ?
C10 C9 H9 119.5 . . ?
C10 C9 C8 120.9(4) . . ?
C8 C9 H9 119.5 . . ?
C12 C7 C6 123.1(4) . . ?
C12 C7 C8 119.9(4) . . ?
C8 C7 C6 116.8(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 C11 120.4(4) . . ?
C9 C10 H10 119.8 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C25 C24 C23 112.9(3) . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C26 C27 C28 111.0(3) . . ?
C26 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C28 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C9 C8 C7 119.1(4) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?

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 V2 O10 V1 8.78(13) 3_775 . . . ?
V1 V2 O10 C3 -131.96(19) 3_775 . . . ?
V1 V2 O4 V1 180.0 3_775 . . . ?
V1 V2 O4 V2 49(100) 3_775 . . 3_775 ?
V1 V2 O4 V3 -84.75(2) 3_775 . . . ?
V1 V2 O4 V3 95.25(2) 3_775 . . 3_775 ?
V1 V2 O9 V3 42.24(8) 3_775 . . . ?
V1 V2 O9 C2 -177.6(2) 3_775 . . . ?
V1 V3 O7 V2 43.86(10) 3_775 . . 3_775 ?
V1 V3 O4 V1 180.0 3_775 . . . ?
V1 V3 O4 V2 -95.47(2) 3_775 . . 3_775 ?
V1 V3 O4 V2 84.53(2) 3_775 . . . ?
V1 V3 O4 V3 -21(41) 3_775 . . 3_775 ?
V1 V3 O8 V1 -12.33(13) 3_775 . . . ?
V1 V3 O8 C1 129.41(19) 3_775 . . . ?
V1 V3 O9 V2 -41.90(8) 3_775 . . . ?
V1 V3 O9 C2 178.7(2) 3_775 . . . ?
V1 O10 C3 C4 -68.1(3) . . . . ?
V1 O8 C1 C4 70.5(3) . . . . ?
V2 V1 O10 V2 -8.65(13) 3_775 . . . ?
V2 V1 O10 C3 132.07(19) 3_775 . . . ?
V2 V1 O6 V3 45.29(11) 3_775 . . 3_775 ?
V2 V1 O4 V1 -76(100) 3_775 . . 3_775 ?
V2 V1 O4 V2 180.0 3_775 . . . ?
V2 V1 O4 V3 -95.36(2) 3_775 . . 3_775 ?
V2 V1 O4 V3 84.64(2) 3_775 . . . ?
V2 V1 O8 V3 -40.82(8) 3_775 . . . ?
V2 V1 O8 C1 177.1(2) 3_775 . . . ?
V2 V3 O4 V1 95.47(2) 3_775 . . 3_775 ?
V2 V3 O4 V1 -84.53(2) 3_775 . . . ?
V2 V3 O4 V2 180.0 3_775 . . . ?
V2 V3 O4 V3 75(41) 3_775 . . 3_775 ?
V2 V3 O8 V1 40.83(8) 3_775 . . . ?
V2 V3 O8 C1 -177.4(2) 3_775 . . . ?
V2 V3 O9 V2 10.76(13) 3_775 . . . ?
V2 V3 O9 C2 -128.65(18) 3_775 . . . ?
V2 O10 C3 C4 69.5(3) . . . . ?
V2 O9 C2 C4 -66.4(3) . . . . ?
V3 V1 O5 V2 -50.09(10) 3_775 . . 3_775 ?
V3 V1 O10 V2 43.45(8) 3_775 . . . ?
V3 V1 O10 C3 -175.8(2) 3_775 . . . ?
V3 V1 O4 V1 20(100) 3_775 . . 3_775 ?
V3 V1 O4 V2 -84.64(2) 3_775 . . . ?
V3 V1 O4 V2 95.36(2) 3_775 . . 3_775 ?
V3 V1 O4 V3 180.0 3_775 . . . ?
V3 V1 O8 V3 12.58(13) 3_775 . . . ?
V3 V1 O8 C1 -129.54(18) 3_775 . . . ?
V3 V2 O10 V1 -43.52(8) 3_775 . . . ?
V3 V2 O10 C3 175.7(2) 3_775 . . . ?
V3 V2 O4 V1 84.75(2) 3_775 . . . ?
V3 V2 O4 V1 -95.25(2) 3_775 . . 3_775 ?
V3 V2 O4 V2 -47(100) 3_775 . . 3_775 ?
V3 V2 O4 V3 180.0 3_775 . . . ?
V3 V2 O9 V3 -10.77(13) 3_775 . . . ?
V3 V2 O9 C2 129.42(18) 3_775 . . . ?
V3 O8 C1 C4 -68.1(3) . . . . ?
V3 O9 C2 C4 69.7(3) . . . . ?
O5 V1 O10 V2 -10.8(3) . . . . ?
O5 V1 O10 C3 129.9(3) . . . . ?
O5 V1 O6 V3 79.57(13) . . . 3_775 ?
O5 V1 O4 V1 -74(100) . . . 3_775 ?
O5 V1 O4 V2 -177.98(7) . . . . ?
O5 V1 O4 V2 2.02(7) . . . 3_775 ?
O5 V1 O4 V3 86.67(7) . . . . ?
O5 V1 O4 V3 -93.33(7) . . . 3_775 ?
O5 V1 O8 V3 -74.46(11) . . . . ?
O5 V1 O8 C1 143.4(2) . . . . ?
O5 V2 O10 V1 21.2(3) 3_775 . . . ?
O5 V2 O10 C3 -119.5(3) 3_775 . . . ?
O5 V2 O4 V1 -178.04(7) 3_775 . . . ?
O5 V2 O4 V1 1.96(7) 3_775 . . 3_775 ?
O5 V2 O4 V2 51(100) 3_775 . . 3_775 ?
O5 V2 O4 V3 97.21(7) 3_775 . . 3_775 ?
O5 V2 O4 V3 -82.79(7) 3_775 . . . ?
O5 V2 O9 V3 75.45(11) 3_775 . . . ?
O5 V2 O9 C2 -144.4(2) 3_775 . . . ?
O10 V1 O5 V2 3.1(3) . . . 3_775 ?
O10 V1 O6 V3 -79.03(12) . . . 3_775 ?
O10 V1 O4 V1 109(100) . . . 3_775 ?
O10 V1 O4 V2 -175.83(6) . . . 3_775 ?
O10 V1 O4 V2 4.17(6) . . . . ?
O10 V1 O4 V3 -91.19(6) . . . . ?
O10 V1 O4 V3 88.81(6) . . . 3_775 ?
O10 V1 O8 V3 85.05(11) . . . . ?
O10 V1 O8 C1 -57.1(2) . . . . ?
O10 V2 O4 V1 175.78(6) . . . 3_775 ?
O10 V2 O4 V1 -4.22(6) . . . . ?
O10 V2 O4 V2 -136(100) . . . 3_775 ?
O10 V2 O4 V3 91.03(6) . . . . ?
O10 V2 O4 V3 -88.97(6) . . . 3_775 ?
O10 V2 O9 V3 -84.86(11) . . . . ?
O10 V2 O9 C2 55.3(2) . . . . ?
O7 V2 O10 V1 -76.79(11) 3_775 . . . ?
O7 V2 O10 C3 142.5(2) 3_775 . . . ?
O7 V2 O4 V1 -93.04(7) 3_775 . . 3_775 ?
O7 V2 O4 V1 86.95(7) 3_775 . . . ?
O7 V2 O4 V2 -44(100) 3_775 . . 3_775 ?
O7 V2 O4 V3 2.21(7) 3_775 . . 3_775 ?
O7 V2 O4 V3 -177.79(7) 3_775 . . . ?
O7 V2 O9 V3 -14.3(3) 3_775 . . . ?
O7 V2 O9 C2 125.9(3) 3_775 . . . ?
O7 V3 O4 V1 -82.37(7) . . . . ?
O7 V3 O4 V1 97.63(7) . . . 3_775 ?
O7 V3 O4 V2 -177.84(7) . . . . ?
O7 V3 O4 V2 2.16(7) . . . 3_775 ?
O7 V3 O4 V3 77(41) . . . 3_775 ?
O7 V3 O8 V1 73.95(11) . . . . ?
O7 V3 O8 C1 -144.3(2) . . . . ?
O7 V3 O9 V2 25.1(3) . . . . ?
O7 V3 O9 C2 -114.3(3) . . . . ?
O6 V1 O5 V2 -82.09(12) . . . 3_775 ?
O6 V1 O10 V2 75.87(11) . . . . ?
O6 V1 O10 C3 -143.4(2) . . . . ?
O6 V1 O4 V1 21(100) . . . 3_775 ?
O6 V1 O4 V2 96.60(7) . . . 3_775 ?
O6 V1 O4 V2 -83.40(7) . . . . ?
O6 V1 O4 V3 -178.76(7) . . . . ?
O6 V1 O4 V3 1.24(7) . . . 3_775 ?
O6 V1 O8 V3 25.7(3) . . . . ?
O6 V1 O8 C1 -116.4(3) . . . . ?
O6 V3 O7 V2 78.12(13) 3_775 . . 3_775 ?
O6 V3 O4 V1 1.31(7) 3_775 . . 3_775 ?
O6 V3 O4 V1 -178.69(7) 3_775 . . . ?
O6 V3 O4 V2 85.84(8) 3_775 . . . ?
O6 V3 O4 V2 -94.16(8) 3_775 . . 3_775 ?
O6 V3 O4 V3 -19(41) 3_775 . . 3_775 ?
O6 V3 O8 V1 -19.4(3) 3_775 . . . ?
O6 V3 O8 C1 122.3(3) 3_775 . . . ?
O6 V3 O9 V2 -75.88(11) 3_775 . . . ?
O6 V3 O9 C2 144.7(2) 3_775 . . . ?
O4 V1 O5 V2 -2.62(9) . . . 3_775 ?
O4 V1 O10 V2 -4.96(8) . . . . ?
O4 V1 O10 C3 135.8(2) . . . . ?
O4 V1 O6 V3 -1.70(10) . . . 3_775 ?
O4 V1 O8 V3 7.09(8) . . . . ?
O4 V1 O8 C1 -135.0(2) . . . . ?
O4 V2 O10 V1 4.96(8) . . . . ?
O4 V2 O10 C3 -135.8(2) . . . . ?
O4 V2 O9 V3 -6.11(7) . . . . ?
O4 V2 O9 C2 134.1(2) . . . . ?
O4 V3 O7 V2 -2.89(9) . . . 3_775 ?
O4 V3 O8 V1 -7.11(8) . . . . ?
O4 V3 O8 C1 134.6(2) . . . . ?
O4 V3 O9 V2 6.05(7) . . . . ?
O4 V3 O9 C2 -133.4(2) . . . . ?
O1 V2 O10 V1 178.40(11) . . . . ?
O1 V2 O10 C3 37.7(2) . . . . ?
O1 V2 O4 V1 125.5(6) . . . 3_775 ?
O1 V2 O4 V1 -54.5(6) . . . . ?
O1 V2 O4 V2 174(100) . . . 3_775 ?
O1 V2 O4 V3 40.7(6) . . . . ?
O1 V2 O4 V3 -139.3(6) . . . 3_775 ?
O1 V2 O9 V3 178.83(11) . . . . ?
O1 V2 O9 C2 -41.0(2) . . . . ?
O8 V1 O5 V2 75.08(12) . . . 3_775 ?
O8 V1 O10 V2 -84.27(11) . . . . ?
O8 V1 O10 C3 56.5(2) . . . . ?
O8 V1 O6 V3 -20.2(3) . . . 3_775 ?
O8 V1 O4 V1 -166(100) . . . 3_775 ?
O8 V1 O4 V2 89.27(7) . . . . ?
O8 V1 O4 V2 -90.73(7) . . . 3_775 ?
O8 V1 O4 V3 -6.09(7) . . . . ?
O8 V1 O4 V3 173.91(7) . . . 3_775 ?
O8 V3 O7 V2 -79.83(12) . . . 3_775 ?
O8 V3 O4 V1 5.93(6) . . . . ?
O8 V3 O4 V1 -174.07(6) . . . 3_775 ?
O8 V3 O4 V2 90.46(6) . . . 3_775 ?
O8 V3 O4 V2 -89.54(6) . . . . ?
O8 V3 O4 V3 165(41) . . . 3_775 ?
O8 V3 O9 V2 83.92(10) . . . . ?
O8 V3 O9 C2 -55.5(2) . . . . ?
O9 V2 O10 V1 83.56(11) . . . . ?
O9 V2 O10 C3 -57.2(2) . . . . ?
O9 V2 O4 V1 89.91(6) . . . 3_775 ?
O9 V2 O4 V1 -90.09(6) . . . . ?
O9 V2 O4 V2 139(100) . . . 3_775 ?
O9 V2 O4 V3 -174.84(6) . . . 3_775 ?
O9 V2 O4 V3 5.16(6) . . . . ?
O9 V3 O7 V2 -21.8(3) . . . 3_775 ?
O9 V3 O4 V1 -89.79(6) . . . 3_775 ?
O9 V3 O4 V1 90.21(6) . . . . ?
O9 V3 O4 V2 174.74(6) . . . 3_775 ?
O9 V3 O4 V2 -5.26(6) . . . . ?
O9 V3 O4 V3 -110(41) . . . 3_775 ?
O9 V3 O8 V1 -86.55(11) . . . . ?
O9 V3 O8 C1 55.2(2) . . . . ?
O2 V1 O5 V2 172.74(12) . . . 3_775 ?
O2 V1 O10 V2 179.30(12) . . . . ?
O2 V1 O10 C3 -40.0(2) . . . . ?
O2 V1 O6 V3 -174.50(13) . . . 3_775 ?
O2 V1 O4 V1 140(100) . . . 3_775 ?
O2 V1 O4 V2 36.0(7) . . . . ?
O2 V1 O4 V2 -144.0(7) . . . 3_775 ?
O2 V1 O4 V3 -59.3(7) . . . . ?
O2 V1 O4 V3 120.7(7) . . . 3_775 ?
O2 V1 O8 V3 -179.39(12) . . . . ?
O2 V1 O8 C1 38.5(2) . . . . ?
O3 V3 O7 V2 -175.29(12) . . . 3_775 ?
O3 V3 O4 V1 -147.1(6) . . . 3_775 ?
O3 V3 O4 V1 32.9(6) . . . . ?
O3 V3 O4 V2 117.5(6) . . . 3_775 ?
O3 V3 O4 V2 -62.5(6) . . . . ?
O3 V3 O4 V3 -168(41) . . . 3_775 ?
O3 V3 O8 V1 176.62(12) . . . . ?
O3 V3 O8 C1 -41.6(2) . . . . ?
O3 V3 O9 V2 179.11(11) . . . . ?
O3 V3 O9 C2 39.7(2) . . . . ?
O11 C6 C7 C12 -130.8(4) . . . . ?
O11 C6 C7 C8 53.3(5) . . . . ?
N1 C18 C19 C20 -175.5(3) . . . . ?
N1 C26 C27 C28 171.2(3) . . . . ?
C18 N1 C22 C23 70.1(4) . . . . ?
C18 N1 C26 C27 -178.4(3) . . . . ?
C18 N1 C14 C15 52.1(4) . . . . ?
C18 C19 C20 C21 179.4(3) . . . . ?
O14 C13 C12 C11 28.1(5) . . . . ?
O14 C13 C12 C7 -156.6(4) . . . . ?
C3 C4 C5 O11 53.4(3) . . . . ?
C3 C4 C1 O8 -62.1(3) . . . . ?
C3 C4 C2 O9 60.5(3) . . . . ?
C5 O11 C6 O12 5.5(6) . . . . ?
C5 O11 C6 C7 -168.6(3) . . . . ?
C5 C4 C3 O10 179.7(2) . . . . ?
C5 C4 C1 O8 179.8(2) . . . . ?
C5 C4 C2 O9 179.4(3) . . . . ?
C13 C12 C7 C6 11.0(6) . . . . ?
C13 C12 C7 C8 -173.2(4) . . . . ?
C1 C4 C3 O10 61.2(3) . . . . ?
C1 C4 C5 O11 172.9(3) . . . . ?
C1 C4 C2 O9 -61.8(3) . . . . ?
C2 C4 C3 O10 -60.9(3) . . . . ?
C2 C4 C5 O11 -67.7(3) . . . . ?
C2 C4 C1 O8 61.0(3) . . . . ?
O13 C13 C12 C11 -152.5(5) . . . . ?
O13 C13 C12 C7 22.7(6) . . . . ?
C16 C15 C14 N1 179.3(3) . . . . ?
C22 N1 C18 C19 172.5(3) . . . . ?
C22 N1 C26 C27 -60.2(4) . . . . ?
C22 N1 C14 C15 -67.2(4) . . . . ?
C22 C23 C24 C25 179.6(3) . . . . ?
C26 N1 C18 C19 -67.2(4) . . . . ?
C26 N1 C22 C23 -48.6(4) . . . . ?
C26 N1 C14 C15 171.5(3) . . . . ?
C14 N1 C18 C19 52.1(4) . . . . ?
C14 N1 C22 C23 -168.2(3) . . . . ?
C14 N1 C26 C27 60.2(4) . . . . ?
C14 C15 C16 C17 -178.6(3) . . . . ?
C6 O11 C5 C4 115.9(3) . . . . ?
C6 C7 C8 C9 175.1(4) . . . . ?
C11 C12 C7 C6 -173.6(4) . . . . ?
C11 C12 C7 C8 2.1(6) . . . . ?
O12 C6 C7 C12 55.2(7) . . . . ?
O12 C6 C7 C8 -120.7(5) . . . . ?
C29 C28 C27 C26 -72.4(5) . . . . ?
C12 C11 C10 C9 -0.5(7) . . . . ?
C12 C7 C8 C9 -0.9(6) . . . . ?
C10 C11 C12 C13 173.9(4) . . . . ?
C10 C11 C12 C7 -1.4(6) . . . . ?
C10 C9 C8 C7 -1.0(7) . . . . ?
C24 C23 C22 N1 -169.1(3) . . . . ?
C8 C9 C10 C11 1.8(7) . . . . ?

####################################################################### 
# 
# 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_zyt-1
_database_code_depnum_ccdc_archive 'CCDC 1484790'
_audit_update_record             
;
2016-08-05 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H94 N2 O23 V6'
_chemical_formula_weight         1396.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.020(2)
_cell_length_b                   15.154(3)
_cell_length_c                   19.352(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.36(3)
_cell_angle_gamma                90.00
_cell_volume                     3205.0(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    99.99(10)
_cell_measurement_reflns_used    9365
_cell_measurement_theta_min      4.9900
_cell_measurement_theta_max      76.6960

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    7.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5479
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      99.99(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20587
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.72
_diffrn_reflns_theta_max         76.80
_reflns_number_total             6676
_reflns_number_gt                5849
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0717P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6676
_refine_ls_number_parameters     367
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1420
_refine_ls_wR_factor_gt          0.1370
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_restrained_S_all      1.391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.47533(4) 1.14569(3) 0.51091(2) 0.03209(13) Uani 1 1 d . . .
V3 V 0.42634(4) 0.99578(3) 0.38651(2) 0.03187(13) Uani 1 1 d . . .
O1 O 0.31455(17) 1.09783(12) 0.53372(8) 0.0324(4) Uani 1 1 d . . .
O2 O 0.27380(17) 0.97722(12) 0.43388(9) 0.0327(4) Uani 1 1 d . . .
O3 O 0.39934(17) 1.12279(12) 0.41120(8) 0.0312(4) Uani 1 1 d . . .
O4 O 0.62484(18) 1.14621(12) 0.47680(10) 0.0368(4) Uani 1 1 d . . .
O5 O 0.54252(19) 1.12164(13) 0.59926(9) 0.0372(4) Uani 1 1 d . . .
O6 O 0.5000 1.0000 0.5000 0.0291(5) Uani 1 2 d S . .
O7 O 0.58352(19) 1.02370(13) 0.37773(9) 0.0361(4) Uani 1 1 d . . .
O8 O 0.43931(19) 1.24836(13) 0.51297(9) 0.0377(4) Uani 1 1 d . . .
O9 O 0.3566(2) 0.99855(13) 0.30803(9) 0.0382(4) Uani 1 1 d . . .
O11 O 0.0766(2) 1.26219(14) 0.40973(11) 0.0450(5) Uani 1 1 d . . .
O10 O 0.18462(18) 0.94918(13) 0.55664(10) 0.0392(4) Uani 1 1 d . . .
N1 N 0.3831(2) 0.69402(17) 0.27103(11) 0.0417(5) Uani 1 1 d . . .
C4 C 0.2035(3) 1.13923(18) 0.50376(13) 0.0366(5) Uani 1 1 d . . .
H4A H 0.2085 1.2021 0.5131 0.044 Uiso 1 1 calc R . .
H4B H 0.1357 1.1158 0.5255 0.044 Uiso 1 1 calc R . .
C5 C 0.0596(3) 1.16869(19) 0.39492(14) 0.0395(6) Uani 1 1 d . . .
C3 C 0.1647(3) 1.02492(18) 0.40911(14) 0.0366(5) Uani 1 1 d . . .
H3A H 0.0971 1.0019 0.4312 0.044 Uiso 1 1 calc R . .
H3B H 0.1456 1.0163 0.3592 0.044 Uiso 1 1 calc R . .
C12 C 0.2363(3) 0.5642(2) 0.23617(14) 0.0419(6) Uani 1 1 d . . .
H12A H 0.1729 0.5895 0.2605 0.050 Uiso 1 1 calc R . .
H12B H 0.2228 0.5838 0.1881 0.050 Uiso 1 1 calc R . .
C11 C 0.3615(3) 0.5952(2) 0.27009(13) 0.0416(6) Uani 1 1 d . . .
H11A H 0.3734 0.5741 0.3178 0.050 Uiso 1 1 calc R . .
H11B H 0.4234 0.5676 0.2459 0.050 Uiso 1 1 calc R . .
C1 C 0.1791(2) 1.12406(18) 0.42464(12) 0.0343(5) Uani 1 1 d . . .
C2 C 0.2835(3) 1.16244(17) 0.38824(13) 0.0342(5) Uani 1 1 d . . .
H2A H 0.2643 1.1540 0.3383 0.041 Uiso 1 1 calc R . .
H2B H 0.2890 1.2254 0.3970 0.041 Uiso 1 1 calc R . .
C44 C 0.1131(3) 0.7375(2) 0.46386(16) 0.0493(7) Uani 1 1 d . . .
H44A H 0.0500 0.7761 0.4759 0.074 Uiso 1 1 calc R . .
H44B H 0.1812 0.7387 0.5002 0.074 Uiso 1 1 calc R . .
H44C H 0.0818 0.6785 0.4585 0.074 Uiso 1 1 calc R . .
C41 C 0.2824(3) 0.7429(2) 0.30240(14) 0.0438(6) Uani 1 1 d . . .
H41A H 0.3046 0.8048 0.3065 0.053 Uiso 1 1 calc R . .
H41B H 0.2076 0.7388 0.2701 0.053 Uiso 1 1 calc R . .
O12 O -0.0961(3) 1.2916(2) 0.34145(15) 0.0701(8) Uani 1 1 d . . .
C42 C 0.2557(3) 0.7108(2) 0.37312(14) 0.0422(6) Uani 1 1 d . . .
H42A H 0.3288 0.7151 0.4067 0.051 Uiso 1 1 calc R . .
H42B H 0.2300 0.6495 0.3701 0.051 Uiso 1 1 calc R . .
C21 C 0.5052(3) 0.7130(2) 0.31559(15) 0.0470(7) Uani 1 1 d . . .
H21A H 0.5121 0.7762 0.3229 0.056 Uiso 1 1 calc R . .
H21B H 0.5040 0.6857 0.3608 0.056 Uiso 1 1 calc R . .
C31 C 0.3843(3) 0.7260(2) 0.19595(14) 0.0441(6) Uani 1 1 d . . .
H31A H 0.4416 0.6899 0.1743 0.053 Uiso 1 1 calc R . .
H31B H 0.3037 0.7164 0.1704 0.053 Uiso 1 1 calc R . .
C43 C 0.1546(3) 0.7679(2) 0.39612(15) 0.0455(6) Uani 1 1 d . . .
H43A H 0.1836 0.8282 0.4016 0.055 Uiso 1 1 calc R . .
H43B H 0.0850 0.7674 0.3599 0.055 Uiso 1 1 calc R . .
C22 C 0.6182(3) 0.6813(2) 0.28576(16) 0.0514(8) Uani 1 1 d . . .
H22A H 0.6263 0.7132 0.2431 0.062 Uiso 1 1 calc R . .
H22B H 0.6101 0.6191 0.2746 0.062 Uiso 1 1 calc R . .
C6 C -0.0085(3) 1.3169(2) 0.37981(17) 0.0513(7) Uani 1 1 d . . .
C32 C 0.4185(3) 0.8224(2) 0.18835(16) 0.0511(7) Uani 1 1 d . . .
H32A H 0.5027 0.8318 0.2086 0.061 Uiso 1 1 calc R . .
H32B H 0.3664 0.8593 0.2130 0.061 Uiso 1 1 calc R . .
C13 C 0.2301(3) 0.4640(2) 0.23902(18) 0.0514(7) Uani 1 1 d . . .
H13A H 0.2441 0.4449 0.2872 0.062 Uiso 1 1 calc R . .
H13B H 0.2944 0.4392 0.2151 0.062 Uiso 1 1 calc R . .
C23 C 0.7323(3) 0.6961(3) 0.33826(17) 0.0568(8) Uani 1 1 d . . .
H23A H 0.7355 0.7574 0.3529 0.068 Uiso 1 1 calc R . .
H23B H 0.7272 0.6598 0.3791 0.068 Uiso 1 1 calc R . .
C33 C 0.4031(4) 0.8476(2) 0.11149(18) 0.0625(10) Uani 1 1 d . . .
H33A H 0.4490 0.8062 0.0866 0.075 Uiso 1 1 calc R . .
H33B H 0.3174 0.8420 0.0928 0.075 Uiso 1 1 calc R . .
C7 C 0.0171(4) 1.4103(3) 0.4004(2) 0.0692(10) Uani 1 1 d D . .
C34 C 0.4447(5) 0.9388(3) 0.0982(2) 0.0807(14) Uani 1 1 d . . .
H34A H 0.4318 0.9506 0.0491 0.121 Uiso 1 1 calc R . .
H34B H 0.5302 0.9444 0.1150 0.121 Uiso 1 1 calc R . .
H34C H 0.3989 0.9803 0.1220 0.121 Uiso 1 1 calc R . .
C24 C 0.8475(4) 0.6735(4) 0.3076(2) 0.0792(13) Uani 1 1 d . . .
H24A H 0.9172 0.6834 0.3418 0.119 Uiso 1 1 calc R . .
H24B H 0.8535 0.7100 0.2677 0.119 Uiso 1 1 calc R . .
H24C H 0.8451 0.6126 0.2938 0.119 Uiso 1 1 calc R . .
C9 C -0.0709(8) 1.4701(4) 0.3795(5) 0.148(4) Uani 1 1 d D . .
H9A H -0.0606 1.5288 0.3930 0.177 Uiso 1 1 calc R . .
H9B H -0.1419 1.4525 0.3516 0.177 Uiso 1 1 calc R . .
C8 C 0.1303(5) 1.4314(3) 0.4439(3) 0.0973(17) Uani 1 1 d D . .
H8A H 0.1335 1.4937 0.4530 0.146 Uiso 1 1 calc R . .
H8B H 0.1983 1.4148 0.4203 0.146 Uiso 1 1 calc R . .
H8C H 0.1341 1.3998 0.4871 0.146 Uiso 1 1 calc R . .
C14 C 0.1060(4) 0.4291(3) 0.2053(2) 0.0655(10) Uani 1 1 d . . .
H14A H 0.1053 0.3659 0.2080 0.098 Uiso 1 1 calc R . .
H14B H 0.0925 0.4470 0.1573 0.098 Uiso 1 1 calc R . .
H14C H 0.0423 0.4527 0.2294 0.098 Uiso 1 1 calc R . .
V1 V 0.32130(4) 0.96398(3) 0.53692(2) 0.03269(13) Uani 1 1 d . . .


_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
V2 O8 1.607(2) . ?
V2 O5 1.8110(19) . ?
V2 O4 1.852(2) . ?
V2 O1 2.0151(19) . ?
V2 O3 2.0325(18) . ?
V2 O6 2.2377(6) . ?
V2 V3 3.0265(8) 3_676 ?
V2 V1 3.0286(8) 3_676 ?
V3 O9 1.612(2) . ?
V3 O7 1.812(2) . ?
V3 O5 1.826(2) 3_676 ?
V3 O3 2.0143(18) . ?
V3 O2 2.0347(19) . ?
V3 O6 2.2427(7) . ?
V3 V2 3.0265(8) 3_676 ?
V3 V1 3.0405(11) 3_676 ?
O1 C4 1.430(3) . ?
O1 V1 2.0304(19) . ?
O2 C3 1.432(3) . ?
O2 V1 2.0057(19) . ?
O3 C2 1.430(3) . ?
O4 V1 1.803(2) 3_676 ?
O5 V3 1.826(2) 3_676 ?
O6 V2 2.2377(6) 3_676 ?
O6 V3 2.2427(7) 3_676 ?
O6 V1 2.2465(6) 3_676 ?
O6 V1 2.2465(6) . ?
O7 V1 1.849(2) 3_676 ?
O11 C6 1.327(4) . ?
O11 C5 1.453(4) . ?
O10 V1 1.616(2) . ?
N1 C11 1.516(4) . ?
N1 C41 1.524(4) . ?
N1 C21 1.529(4) . ?
N1 C31 1.533(3) . ?
C4 C1 1.537(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C1 1.525(4) . ?
C3 C1 1.536(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C12 C13 1.522(4) . ?
C12 C11 1.523(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C1 C2 1.538(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C44 C43 1.514(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C41 C42 1.516(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
O12 C6 1.203(5) . ?
C42 C43 1.522(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C21 C22 1.517(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C31 C32 1.521(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C22 C23 1.528(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C6 C7 1.488(5) . ?
C32 C33 1.524(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C13 C14 1.532(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C23 C24 1.508(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C33 C34 1.490(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C7 C9 1.351(6) . ?
C7 C8 1.448(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C9 H9A 0.9300 . ?
C9 H9B 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
V1 O4 1.803(2) 3_676 ?
V1 O7 1.849(2) 3_676 ?
V1 V2 3.0286(8) 3_676 ?
V1 V3 3.0405(11) 3_676 ?

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
O8 V2 O5 104.11(9) . . ?
O8 V2 O4 103.80(10) . . ?
O5 V2 O4 93.59(9) . . ?
O8 V2 O1 96.67(9) . . ?
O5 V2 O1 89.16(9) . . ?
O4 V2 O1 157.98(8) . . ?
O8 V2 O3 96.65(9) . . ?
O5 V2 O3 158.56(8) . . ?
O4 V2 O3 86.53(8) . . ?
O1 V2 O3 83.09(7) . . ?
O8 V2 O6 172.16(8) . . ?
O5 V2 O6 81.41(6) . . ?
O4 V2 O6 81.15(6) . . ?
O1 V2 O6 77.67(5) . . ?
O3 V2 O6 77.42(5) . . ?
O8 V2 V3 137.58(7) . 3_676 ?
O5 V2 V3 33.85(6) . 3_676 ?
O4 V2 V3 88.67(6) . 3_676 ?
O1 V2 V3 81.50(6) . 3_676 ?
O3 V2 V3 124.83(5) . 3_676 ?
O6 V2 V3 47.577(15) . 3_676 ?
O8 V2 V1 137.18(8) . 3_676 ?
O5 V2 V1 87.09(7) . 3_676 ?
O4 V2 V1 33.53(6) . 3_676 ?
O1 V2 V1 125.12(6) . 3_676 ?
O3 V2 V1 81.21(6) . 3_676 ?
O6 V2 V1 47.637(13) . 3_676 ?
V3 V2 V1 66.11(2) 3_676 3_676 ?
O9 V3 O7 104.57(10) . . ?
O9 V3 O5 103.00(9) . 3_676 ?
O7 V3 O5 94.48(9) . 3_676 ?
O9 V3 O3 97.56(9) . . ?
O7 V3 O3 88.35(8) . . ?
O5 V3 O3 157.78(8) 3_676 . ?
O9 V3 O2 96.11(10) . . ?
O7 V3 O2 158.33(8) . . ?
O5 V3 O2 86.99(8) 3_676 . ?
O3 V3 O2 82.51(7) . . ?
O9 V3 O6 172.18(8) . . ?
O7 V3 O6 81.65(6) . . ?
O5 V3 O6 80.95(6) 3_676 . ?
O3 V3 O6 77.67(5) . . ?
O2 V3 O6 77.23(6) . . ?
O9 V3 V2 136.35(7) . 3_676 ?
O7 V3 V2 87.75(6) . 3_676 ?
O5 V3 V2 33.53(6) 3_676 3_676 ?
O3 V3 V2 124.93(5) . 3_676 ?
O2 V3 V2 81.58(6) . 3_676 ?
O6 V3 V2 47.438(16) . 3_676 ?
O9 V3 V1 138.56(8) . 3_676 ?
O7 V3 V1 34.24(6) . 3_676 ?
O5 V3 V1 88.82(7) 3_676 3_676 ?
O3 V3 V1 81.17(6) . 3_676 ?
O2 V3 V1 124.40(6) . 3_676 ?
O6 V3 V1 47.42(2) . 3_676 ?
V2 V3 V1 66.06(2) 3_676 3_676 ?
C4 O1 V2 118.94(15) . . ?
C4 O1 V1 118.47(16) . . ?
V2 O1 V1 109.66(8) . . ?
C3 O2 V1 118.97(15) . . ?
C3 O2 V3 119.08(15) . . ?
V1 O2 V3 109.66(9) . . ?
C2 O3 V3 118.75(15) . . ?
C2 O3 V2 117.79(14) . . ?
V3 O3 V2 109.45(8) . . ?
V1 O4 V2 111.91(9) 3_676 . ?
V2 O5 V3 112.62(10) . 3_676 ?
V2 O6 V2 180.0 . 3_676 ?
V2 O6 V3 84.986(16) . 3_676 ?
V2 O6 V3 95.014(16) 3_676 3_676 ?
V2 O6 V3 95.014(16) . . ?
V2 O6 V3 84.986(16) 3_676 . ?
V3 O6 V3 180.0 3_676 . ?
V2 O6 V1 84.970(18) . 3_676 ?
V2 O6 V1 95.030(18) 3_676 3_676 ?
V3 O6 V1 94.74(3) 3_676 3_676 ?
V3 O6 V1 85.26(3) . 3_676 ?
V2 O6 V1 95.030(18) . . ?
V2 O6 V1 84.970(18) 3_676 . ?
V3 O6 V1 85.26(3) 3_676 . ?
V3 O6 V1 94.74(3) . . ?
V1 O6 V1 180.0 3_676 . ?
V3 O7 V1 112.30(9) . 3_676 ?
C6 O11 C5 117.2(3) . . ?
C11 N1 C41 111.3(2) . . ?
C11 N1 C21 108.6(2) . . ?
C41 N1 C21 108.5(2) . . ?
C11 N1 C31 108.7(2) . . ?
C41 N1 C31 108.6(2) . . ?
C21 N1 C31 111.2(2) . . ?
O1 C4 C1 111.7(2) . . ?
O1 C4 H4A 109.3 . . ?
C1 C4 H4A 109.3 . . ?
O1 C4 H4B 109.3 . . ?
C1 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O11 C5 C1 106.0(2) . . ?
O2 C3 C1 111.5(2) . . ?
O2 C3 H3A 109.3 . . ?
C1 C3 H3A 109.3 . . ?
O2 C3 H3B 109.3 . . ?
C1 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C13 C12 C11 109.5(3) . . ?
C13 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
N1 C11 C12 116.2(3) . . ?
N1 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N1 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C5 C1 C3 107.3(2) . . ?
C5 C1 C4 110.0(2) . . ?
C3 C1 C4 110.0(2) . . ?
C5 C1 C2 108.6(2) . . ?
C3 C1 C2 110.2(2) . . ?
C4 C1 C2 110.7(2) . . ?
O3 C2 C1 112.9(2) . . ?
O3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
O3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C41 N1 116.0(3) . . ?
C42 C41 H41A 108.3 . . ?
N1 C41 H41A 108.3 . . ?
C42 C41 H41B 108.3 . . ?
N1 C41 H41B 108.3 . . ?
H41A C41 H41B 107.4 . . ?
C41 C42 C43 108.4(3) . . ?
C41 C42 H42A 110.0 . . ?
C43 C42 H42A 110.0 . . ?
C41 C42 H42B 110.0 . . ?
C43 C42 H42B 110.0 . . ?
H42A C42 H42B 108.4 . . ?
C22 C21 N1 115.6(2) . . ?
C22 C21 H21A 108.4 . . ?
N1 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N1 C21 H21B 108.4 . . ?
H21A C21 H21B 107.4 . . ?
C32 C31 N1 115.3(2) . . ?
C32 C31 H31A 108.4 . . ?
N1 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
N1 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C44 C43 C42 113.2(3) . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C42 C43 H43B 108.9 . . ?
H43A C43 H43B 107.8 . . ?
C21 C22 C23 110.3(3) . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
O12 C6 O11 122.5(3) . . ?
O12 C6 C7 125.3(4) . . ?
O11 C6 C7 112.2(3) . . ?
C31 C32 C33 109.7(3) . . ?
C31 C32 H32A 109.7 . . ?
C33 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C12 C13 C14 111.7(3) . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C24 C23 C22 111.6(3) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C34 C33 C32 113.7(3) . . ?
C34 C33 H33A 108.8 . . ?
C32 C33 H33A 108.8 . . ?
C34 C33 H33B 108.8 . . ?
C32 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C9 C7 C8 123.9(5) . . ?
C9 C7 C6 117.0(5) . . ?
C8 C7 C6 119.1(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C9 H9A 120.0 . . ?
C7 C9 H9B 120.0 . . ?
H9A C9 H9B 120.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O10 V1 O4 103.92(10) . 3_676 ?
O10 V1 O7 104.01(10) . 3_676 ?
O4 V1 O7 93.75(9) 3_676 3_676 ?
O10 V1 O2 96.68(9) . . ?
O4 V1 O2 89.72(8) 3_676 . ?
O7 V1 O2 157.50(8) 3_676 . ?
O10 V1 O1 96.56(9) . . ?
O4 V1 O1 158.77(8) 3_676 . ?
O7 V1 O1 86.60(8) 3_676 . ?
O2 V1 O1 82.29(7) . . ?
O10 V1 O6 172.00(7) . . ?
O4 V1 O6 81.94(6) 3_676 . ?
O7 V1 O6 80.77(6) 3_676 . ?
O2 V1 O6 77.71(6) . . ?
O1 V1 O6 77.16(5) . . ?
O10 V1 V2 138.12(8) . 3_676 ?
O4 V1 V2 34.56(6) 3_676 3_676 ?
O7 V1 V2 88.35(7) 3_676 3_676 ?
O2 V1 V2 81.96(6) . 3_676 ?
O1 V1 V2 124.37(5) . 3_676 ?
O6 V1 V2 47.392(17) . 3_676 ?
O10 V1 V3 137.27(7) . 3_676 ?
O4 V1 V3 87.69(7) 3_676 3_676 ?
O7 V1 V3 33.46(6) 3_676 3_676 ?
O2 V1 V3 124.77(6) . 3_676 ?
O1 V1 V3 80.92(5) . 3_676 ?
O6 V1 V3 47.315(16) . 3_676 ?
V2 V1 V3 65.959(19) 3_676 3_676 ?

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
O8 V2 O1 C4 39.38(17) . . . . ?
O5 V2 O1 C4 143.48(17) . . . . ?
O4 V2 O1 C4 -119.0(2) . . . . ?
O3 V2 O1 C4 -56.55(17) . . . . ?
O6 V2 O1 C4 -135.12(16) . . . . ?
V3 V2 O1 C4 176.60(16) 3_676 . . . ?
V1 V2 O1 C4 -130.68(15) 3_676 . . . ?
O8 V2 O1 V1 -179.73(9) . . . . ?
O5 V2 O1 V1 -75.63(9) . . . . ?
O4 V2 O1 V1 21.9(2) . . . . ?
O3 V2 O1 V1 84.34(8) . . . . ?
O6 V2 O1 V1 5.77(6) . . . . ?
V3 V2 O1 V1 -42.51(6) 3_676 . . . ?
V1 V2 O1 V1 10.22(10) 3_676 . . . ?
O9 V3 O2 C3 -40.71(19) . . . . ?
O7 V3 O2 C3 121.9(2) . . . . ?
O5 V3 O2 C3 -143.48(18) 3_676 . . . ?
O3 V3 O2 C3 56.14(18) . . . . ?
O6 V3 O2 C3 135.13(17) . . . . ?
V2 V3 O2 C3 -176.75(17) 3_676 . . . ?
V1 V3 O2 C3 130.02(16) 3_676 . . . ?
O9 V3 O2 V1 177.36(10) . . . . ?
O7 V3 O2 V1 -20.0(3) . . . . ?
O5 V3 O2 V1 74.60(9) 3_676 . . . ?
O3 V3 O2 V1 -85.78(9) . . . . ?
O6 V3 O2 V1 -6.80(6) . . . . ?
V2 V3 O2 V1 41.33(7) 3_676 . . . ?
V1 V3 O2 V1 -11.91(11) 3_676 . . . ?
O9 V3 O3 C2 39.99(17) . . . . ?
O7 V3 O3 C2 144.47(16) . . . . ?
O5 V3 O3 C2 -117.7(3) 3_676 . . . ?
O2 V3 O3 C2 -55.22(16) . . . . ?
O6 V3 O3 C2 -133.72(15) . . . . ?
V2 V3 O3 C2 -129.43(14) 3_676 . . . ?
V1 V3 O3 C2 178.12(15) 3_676 . . . ?
O9 V3 O3 V2 179.25(10) . . . . ?
O7 V3 O3 V2 -76.27(9) . . . . ?
O5 V3 O3 V2 21.6(3) 3_676 . . . ?
O2 V3 O3 V2 84.04(9) . . . . ?
O6 V3 O3 V2 5.55(6) . . . . ?
V2 V3 O3 V2 9.83(11) 3_676 . . . ?
V1 V3 O3 V2 -42.62(7) 3_676 . . . ?
O8 V2 O3 C2 -40.66(18) . . . . ?
O5 V2 O3 C2 124.9(2) . . . . ?
O4 V2 O3 C2 -144.16(17) . . . . ?
O1 V2 O3 C2 55.29(16) . . . . ?
O6 V2 O3 C2 134.14(16) . . . . ?
V3 V2 O3 C2 129.89(15) 3_676 . . . ?
V1 V2 O3 C2 -177.47(16) 3_676 . . . ?
O8 V2 O3 V3 179.64(10) . . . . ?
O5 V2 O3 V3 -14.8(3) . . . . ?
O4 V2 O3 V3 76.14(9) . . . . ?
O1 V2 O3 V3 -84.41(9) . . . . ?
O6 V2 O3 V3 -5.56(6) . . . . ?
V3 V2 O3 V3 -9.81(11) 3_676 . . . ?
V1 V2 O3 V3 42.83(7) 3_676 . . . ?
O8 V2 O4 V1 -175.30(10) . . . 3_676 ?
O5 V2 O4 V1 79.22(11) . . . 3_676 ?
O1 V2 O4 V1 -17.4(3) . . . 3_676 ?
O3 V2 O4 V1 -79.30(10) . . . 3_676 ?
O6 V2 O4 V1 -1.50(8) . . . 3_676 ?
V3 V2 O4 V1 45.71(9) 3_676 . . 3_676 ?
O8 V2 O5 V3 172.58(11) . . . 3_676 ?
O4 V2 O5 V3 -82.22(11) . . . 3_676 ?
O1 V2 O5 V3 75.92(11) . . . 3_676 ?
O3 V2 O5 V3 7.4(3) . . . 3_676 ?
O6 V2 O5 V3 -1.73(9) . . . 3_676 ?
V1 V2 O5 V3 -49.31(10) 3_676 . . 3_676 ?
O8 V2 O6 V2 42(100) . . . 3_676 ?
O5 V2 O6 V2 177(100) . . . 3_676 ?
O4 V2 O6 V2 -88(100) . . . 3_676 ?
O1 V2 O6 V2 86(100) . . . 3_676 ?
O3 V2 O6 V2 0(100) . . . 3_676 ?
V3 V2 O6 V2 176(100) 3_676 . . 3_676 ?
V1 V2 O6 V2 -89(100) 3_676 . . 3_676 ?
O8 V2 O6 V3 -133.9(5) . . . 3_676 ?
O5 V2 O6 V3 1.31(7) . . . 3_676 ?
O4 V2 O6 V3 96.34(7) . . . 3_676 ?
O1 V2 O6 V3 -89.71(6) . . . 3_676 ?
O3 V2 O6 V3 -175.27(5) . . . 3_676 ?
V1 V2 O6 V3 95.22(3) 3_676 . . 3_676 ?
O8 V2 O6 V3 46.1(5) . . . . ?
O5 V2 O6 V3 -178.69(7) . . . . ?
O4 V2 O6 V3 -83.66(7) . . . . ?
O1 V2 O6 V3 90.29(6) . . . . ?
O3 V2 O6 V3 4.73(5) . . . . ?
V3 V2 O6 V3 180.0 3_676 . . . ?
V1 V2 O6 V3 -84.78(3) 3_676 . . . ?
O8 V2 O6 V1 130.8(5) . . . 3_676 ?
O5 V2 O6 V1 -93.91(7) . . . 3_676 ?
O4 V2 O6 V1 1.12(6) . . . 3_676 ?
O1 V2 O6 V1 175.07(5) . . . 3_676 ?
O3 V2 O6 V1 89.51(6) . . . 3_676 ?
V3 V2 O6 V1 -95.22(3) 3_676 . . 3_676 ?
O8 V2 O6 V1 -49.2(5) . . . . ?
O5 V2 O6 V1 86.09(7) . . . . ?
O4 V2 O6 V1 -178.88(6) . . . . ?
O1 V2 O6 V1 -4.93(5) . . . . ?
O3 V2 O6 V1 -90.49(6) . . . . ?
V3 V2 O6 V1 84.78(3) 3_676 . . . ?
V1 V2 O6 V1 180.0 3_676 . . . ?
O9 V3 O6 V2 -57.8(5) . . . . ?
O7 V3 O6 V2 85.36(6) . . . . ?
O5 V3 O6 V2 -178.70(7) 3_676 . . . ?
O3 V3 O6 V2 -4.77(5) . . . . ?
O2 V3 O6 V2 -89.75(5) . . . . ?
V2 V3 O6 V2 180.0 3_676 . . . ?
V1 V3 O6 V2 84.515(17) 3_676 . . . ?
O9 V3 O6 V2 122.2(5) . . . 3_676 ?
O7 V3 O6 V2 -94.64(6) . . . 3_676 ?
O5 V3 O6 V2 1.30(7) 3_676 . . 3_676 ?
O3 V3 O6 V2 175.23(5) . . . 3_676 ?
O2 V3 O6 V2 90.25(5) . . . 3_676 ?
V1 V3 O6 V2 -95.485(18) 3_676 . . 3_676 ?
O9 V3 O6 V3 -17(100) . . . 3_676 ?
O7 V3 O6 V3 126(100) . . . 3_676 ?
O5 V3 O6 V3 -138(100) 3_676 . . 3_676 ?
O3 V3 O6 V3 36(100) . . . 3_676 ?
O2 V3 O6 V3 -49(100) . . . 3_676 ?
V2 V3 O6 V3 -139(100) 3_676 . . 3_676 ?
V1 V3 O6 V3 125(100) 3_676 . . 3_676 ?
O9 V3 O6 V1 -142.3(5) . . . 3_676 ?
O7 V3 O6 V1 0.85(6) . . . 3_676 ?
O5 V3 O6 V1 96.78(7) 3_676 . . 3_676 ?
O3 V3 O6 V1 -89.28(5) . . . 3_676 ?
O2 V3 O6 V1 -174.27(5) . . . 3_676 ?
V2 V3 O6 V1 95.485(17) 3_676 . . 3_676 ?
O9 V3 O6 V1 37.7(5) . . . . ?
O7 V3 O6 V1 -179.15(6) . . . . ?
O5 V3 O6 V1 -83.22(7) 3_676 . . . ?
O3 V3 O6 V1 90.72(5) . . . . ?
O2 V3 O6 V1 5.73(5) . . . . ?
V2 V3 O6 V1 -84.515(17) 3_676 . . . ?
V1 V3 O6 V1 180.0 3_676 . . . ?
O9 V3 O7 V1 174.05(10) . . . 3_676 ?
O5 V3 O7 V1 -81.27(11) 3_676 . . 3_676 ?
O3 V3 O7 V1 76.66(10) . . . 3_676 ?
O2 V3 O7 V1 11.9(3) . . . 3_676 ?
O6 V3 O7 V1 -1.11(8) . . . 3_676 ?
V2 V3 O7 V1 -48.39(9) 3_676 . . 3_676 ?
V2 O1 C4 C1 68.6(2) . . . . ?
V1 O1 C4 C1 -68.9(2) . . . . ?
C6 O11 C5 C1 170.2(2) . . . . ?
V1 O2 C3 C1 69.7(2) . . . . ?
V3 O2 C3 C1 -68.7(2) . . . . ?
C41 N1 C11 C12 52.9(3) . . . . ?
C21 N1 C11 C12 172.2(2) . . . . ?
C31 N1 C11 C12 -66.7(3) . . . . ?
C13 C12 C11 N1 179.5(2) . . . . ?
O11 C5 C1 C3 -179.38(19) . . . . ?
O11 C5 C1 C4 61.0(3) . . . . ?
O11 C5 C1 C2 -60.3(3) . . . . ?
O2 C3 C1 C5 178.8(2) . . . . ?
O2 C3 C1 C4 -61.6(3) . . . . ?
O2 C3 C1 C2 60.7(3) . . . . ?
O1 C4 C1 C5 179.6(2) . . . . ?
O1 C4 C1 C3 61.6(3) . . . . ?
O1 C4 C1 C2 -60.3(3) . . . . ?
V3 O3 C2 C1 68.3(2) . . . . ?
V2 O3 C2 C1 -67.6(2) . . . . ?
C5 C1 C2 O3 -178.3(2) . . . . ?
C3 C1 C2 O3 -61.0(3) . . . . ?
C4 C1 C2 O3 60.8(3) . . . . ?
C11 N1 C41 C42 52.1(3) . . . . ?
C21 N1 C41 C42 -67.3(3) . . . . ?
C31 N1 C41 C42 171.8(2) . . . . ?
N1 C41 C42 C43 179.3(2) . . . . ?
C11 N1 C21 C22 68.1(3) . . . . ?
C41 N1 C21 C22 -170.8(3) . . . . ?
C31 N1 C21 C22 -51.5(4) . . . . ?
C11 N1 C31 C32 -173.8(3) . . . . ?
C41 N1 C31 C32 64.9(3) . . . . ?
C21 N1 C31 C32 -54.3(4) . . . . ?
C41 C42 C43 C44 175.6(3) . . . . ?
N1 C21 C22 C23 -174.4(3) . . . . ?
C5 O11 C6 O12 -0.6(5) . . . . ?
C5 O11 C6 C7 178.4(3) . . . . ?
N1 C31 C32 C33 -174.1(3) . . . . ?
C11 C12 C13 C14 -179.8(3) . . . . ?
C21 C22 C23 C24 -174.5(4) . . . . ?
C31 C32 C33 C34 -175.0(4) . . . . ?
O12 C6 C7 C9 6.5(8) . . . . ?
O11 C6 C7 C9 -172.4(6) . . . . ?
O12 C6 C7 C8 -176.4(4) . . . . ?
O11 C6 C7 C8 4.7(6) . . . . ?
C3 O2 V1 O10 39.01(19) . . . . ?
V3 O2 V1 O10 -179.02(10) . . . . ?
C3 O2 V1 O4 142.99(18) . . . 3_676 ?
V3 O2 V1 O4 -75.04(10) . . . 3_676 ?
C3 O2 V1 O7 -117.9(2) . . . 3_676 ?
V3 O2 V1 O7 24.1(3) . . . 3_676 ?
C3 O2 V1 O1 -56.74(17) . . . . ?
V3 O2 V1 O1 85.24(9) . . . . ?
C3 O2 V1 O6 -135.20(17) . . . . ?
V3 O2 V1 O6 6.77(6) . . . . ?
C3 O2 V1 V2 176.78(17) . . . 3_676 ?
V3 O2 V1 V2 -41.24(7) . . . 3_676 ?
C3 O2 V1 V3 -130.01(16) . . . 3_676 ?
V3 O2 V1 V3 11.96(11) . . . 3_676 ?
C4 O1 V1 O10 -39.63(17) . . . . ?
V2 O1 V1 O10 179.27(9) . . . . ?
C4 O1 V1 O4 125.0(2) . . . 3_676 ?
V2 O1 V1 O4 -16.1(3) . . . 3_676 ?
C4 O1 V1 O7 -143.36(16) . . . 3_676 ?
V2 O1 V1 O7 75.54(9) . . . 3_676 ?
C4 O1 V1 O2 56.26(16) . . . . ?
V2 O1 V1 O2 -84.84(9) . . . . ?
C4 O1 V1 O6 135.34(15) . . . . ?
V2 O1 V1 O6 -5.76(6) . . . . ?
C4 O1 V1 V2 130.98(14) . . . 3_676 ?
V2 O1 V1 V2 -10.12(10) . . . 3_676 ?
C4 O1 V1 V3 -176.55(15) . . . 3_676 ?
V2 O1 V1 V3 42.35(7) . . . 3_676 ?
V2 O6 V1 O10 43.6(6) . . . . ?
V2 O6 V1 O10 -136.4(6) 3_676 . . . ?
V3 O6 V1 O10 128.2(6) 3_676 . . . ?
V3 O6 V1 O10 -51.8(6) . . . . ?
V1 O6 V1 O10 -38(100) 3_676 . . . ?
V2 O6 V1 O4 -178.85(6) . . . 3_676 ?
V2 O6 V1 O4 1.15(6) 3_676 . . 3_676 ?
V3 O6 V1 O4 -94.32(6) 3_676 . . 3_676 ?
V3 O6 V1 O4 85.68(6) . . . 3_676 ?
V1 O6 V1 O4 99(100) 3_676 . . 3_676 ?
V2 O6 V1 O7 -83.70(6) . . . 3_676 ?
V2 O6 V1 O7 96.31(6) 3_676 . . 3_676 ?
V3 O6 V1 O7 0.83(6) 3_676 . . 3_676 ?
V3 O6 V1 O7 -179.17(6) . . . 3_676 ?
V1 O6 V1 O7 -166(100) 3_676 . . 3_676 ?
V2 O6 V1 O2 89.67(6) . . . . ?
V2 O6 V1 O2 -90.33(6) 3_676 . . . ?
V3 O6 V1 O2 174.20(6) 3_676 . . . ?
V3 O6 V1 O2 -5.80(6) . . . . ?
V1 O6 V1 O2 8(100) 3_676 . . . ?
V2 O6 V1 O1 4.90(5) . . . . ?
V2 O6 V1 O1 -175.10(5) 3_676 . . . ?
V3 O6 V1 O1 89.43(5) 3_676 . . . ?
V3 O6 V1 O1 -90.57(5) . . . . ?
V1 O6 V1 O1 -77(100) 3_676 . . . ?
V2 O6 V1 V2 180.0 . . . 3_676 ?
V3 O6 V1 V2 -95.471(17) 3_676 . . 3_676 ?
V3 O6 V1 V2 84.529(17) . . . 3_676 ?
V1 O6 V1 V2 98(100) 3_676 . . 3_676 ?
V2 O6 V1 V3 -84.529(17) . . . 3_676 ?
V2 O6 V1 V3 95.471(17) 3_676 . . 3_676 ?
V3 O6 V1 V3 180.0 . . . 3_676 ?
V1 O6 V1 V3 -167(100) 3_676 . . 3_676 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        76.8031
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.073
