# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1413240'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H59 N2 O5 V, 0.5(C2 H3 N)'
_chemical_formula_sum            'C43 H60.50 N2.50 O5 V'
_chemical_formula_weight         743.38

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   P2(1)/n
_symmetry_space_group_name_Hall  -P2yn

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

_cell_length_a                   15.7992(10)
_cell_length_b                   13.8716(8)
_cell_length_c                   19.3649(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.760(2)
_cell_angle_gamma                90.00
_cell_volume                     4242.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    137245
_cell_measurement_theta_min      4.463
_cell_measurement_theta_max      39.773

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            132448
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         26.46
_reflns_number_total             8704
_reflns_number_gt                6289
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_cell_refinement       
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_reduction        
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_solution    
'XS V2008/1 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_refinement  
'XL V2008/4 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0829P)²+50.6124P] 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     SHELXL
_refine_ls_extinction_coef       0.0039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8704
_refine_ls_number_parameters     494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1032
_refine_ls_wR_factor_ref         0.3247
_refine_ls_wR_factor_gt          0.3070
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.000
_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 0.16248(6) 0.26255(7) 0.54710(5) 0.0155(3) Uani 1 1 d . . .
O1 O 0.1537(3) 0.2064(3) 0.4754(2) 0.0214(10) Uani 1 1 d . . .
N1 N 0.1740(3) 0.3588(4) 0.6532(3) 0.0163(10) Uani 1 1 d . . .
C1 C 0.0020(4) 0.2627(4) 0.6265(3) 0.0159(12) Uani 1 1 d . . .
O2 O 0.2217(3) 0.1735(3) 0.5998(2) 0.0193(9) Uani 1 1 d . . .
C2 C 0.0171(4) 0.3403(4) 0.6713(3) 0.0152(12) Uani 1 1 d . . .
N2 N 0.3066(4) 0.6331(4) 0.6358(3) 0.0366(15) Uani 1 1 d . . .
O3 O 0.0568(3) 0.2402(3) 0.5780(2) 0.0174(9) Uani 1 1 d . . .
C3 C -0.0428(4) 0.3620(4) 0.7208(3) 0.0145(12) Uani 1 1 d . . .
H3 H -0.0315 0.4118 0.7519 0.017 Uiso 1 1 calc R . .
N3 N 0.6003(13) 0.215(2) 0.5661(12) 0.089(7) Uani 0.50 1 d P . .
O4 O 0.1220(3) 0.3893(3) 0.5113(2) 0.0209(10) Uani 1 1 d . . .
C4 C -0.1181(4) 0.3122(5) 0.7251(3) 0.0194(13) Uani 1 1 d . . .
O5 O 0.2774(3) 0.3161(3) 0.5276(2) 0.0224(10) Uani 1 1 d . . .
C5 C -0.1315(4) 0.2357(5) 0.6788(3) 0.0209(13) Uani 1 1 d . . .
H5 H -0.1823 0.2019 0.6807 0.025 Uiso 1 1 calc R . .
C6 C -0.0738(4) 0.2076(4) 0.6307(3) 0.0173(12) Uani 1 1 d . . .
C7 C 0.0918(4) 0.4061(4) 0.6644(3) 0.0173(12) Uani 1 1 d . . .
H7B H 0.0800 0.4496 0.6261 0.021 Uiso 1 1 calc R . .
H7A H 0.0972 0.4449 0.7059 0.021 Uiso 1 1 calc R . .
C8 C 0.1929(4) 0.2931(4) 0.7121(3) 0.0157(12) Uani 1 1 d . . .
H8B H 0.1474 0.2467 0.7155 0.019 Uiso 1 1 calc R . .
H8A H 0.1954 0.3303 0.7545 0.019 Uiso 1 1 calc R . .
C9 C 0.2754(4) 0.2401(4) 0.7047(3) 0.0171(12) Uani 1 1 d . . .
C10 C 0.3424(4) 0.2489(4) 0.7552(3) 0.0194(13) Uani 1 1 d . . .
H10 H 0.3376 0.2930 0.7910 0.023 Uiso 1 1 calc R . .
C11 C 0.4128(4) 0.1940(4) 0.7517(3) 0.0175(12) Uani 1 1 d . . .
C12 C 0.4196(4) 0.1301(5) 0.6963(3) 0.0200(13) Uani 1 1 d . . .
H12 H 0.4687 0.0936 0.6936 0.024 Uiso 1 1 calc R . .
C13 C 0.3566(4) 0.1184(4) 0.6449(3) 0.0193(13) Uani 1 1 d . . .
C14 C 0.2841(4) 0.1778(4) 0.6489(3) 0.0172(12) Uani 1 1 d . . .
C15 C 0.2410(4) 0.4330(4) 0.6464(3) 0.0183(13) Uani 1 1 d . . .
H15B H 0.2270 0.4707 0.6054 0.022 Uiso 1 1 calc R . .
H15A H 0.2936 0.3997 0.6380 0.022 Uiso 1 1 calc R . .
C16 C 0.2577(4) 0.5037(5) 0.7062(3) 0.0215(13) Uani 1 1 d . . .
H16B H 0.2065 0.5396 0.7153 0.026 Uiso 1 1 calc R . .
H16A H 0.2745 0.4686 0.7477 0.026 Uiso 1 1 calc R . .
C17 C 0.3259(4) 0.5709(4) 0.6871(3) 0.0219(13) Uani 1 1 d . . .
C18 C 0.4050(5) 0.5706(6) 0.7194(4) 0.0370(19) Uani 1 1 d . . .
H18 H 0.4178 0.5276 0.7551 0.044 Uiso 1 1 calc R . .
C19 C 0.4662(5) 0.6372(7) 0.6970(5) 0.049(3) Uani 1 1 d . . .
H19 H 0.5203 0.6384 0.7173 0.059 Uiso 1 1 calc R . .
C20 C 0.4446(6) 0.6989(6) 0.6456(5) 0.052(3) Uani 1 1 d . . .
H20 H 0.4836 0.7438 0.6306 0.063 Uiso 1 1 calc R . .
C21 C 0.3653(6) 0.6953(6) 0.6157(5) 0.052(2) Uani 1 1 d . . .
H21 H 0.3517 0.7378 0.5799 0.062 Uiso 1 1 calc R . .
C22 C -0.1871(4) 0.3393(5) 0.7763(3) 0.0226(14) Uani 1 1 d . . .
C23 C -0.2656(5) 0.3744(7) 0.7360(4) 0.042(2) Uani 1 1 d . . .
H23C H -0.3085 0.3920 0.7677 0.063 Uiso 1 1 calc R . .
H23B H -0.2865 0.3238 0.7062 0.063 Uiso 1 1 calc R . .
H23A H -0.2513 0.4294 0.7087 0.063 Uiso 1 1 calc R . .
C24 C -0.2097(6) 0.2515(6) 0.8193(4) 0.044(2) Uani 1 1 d . . .
H24C H -0.1600 0.2285 0.8438 0.066 Uiso 1 1 calc R . .
H24B H -0.2316 0.2016 0.7894 0.066 Uiso 1 1 calc R . .
H24A H -0.2518 0.2691 0.8517 0.066 Uiso 1 1 calc R . .
C25 C -0.1574(5) 0.4176(6) 0.8264(4) 0.0339(17) Uani 1 1 d . . .
H25C H -0.2013 0.4311 0.8582 0.051 Uiso 1 1 calc R . .
H25B H -0.1445 0.4750 0.8012 0.051 Uiso 1 1 calc R . .
H25A H -0.1076 0.3960 0.8516 0.051 Uiso 1 1 calc R . .
C26 C -0.0906(4) 0.1201(5) 0.5833(3) 0.0216(13) Uani 1 1 d . . .
C27 C -0.0202(5) 0.0460(5) 0.5962(4) 0.0306(16) Uani 1 1 d . . .
H27C H 0.0331 0.0731 0.5837 0.046 Uiso 1 1 calc R . .
H27B H -0.0317 -0.0105 0.5688 0.046 Uiso 1 1 calc R . .
H27A H -0.0177 0.0287 0.6442 0.046 Uiso 1 1 calc R . .
C28 C -0.1747(5) 0.0705(5) 0.5982(4) 0.0334(17) Uani 1 1 d . . .
H28C H -0.1733 0.0473 0.6449 0.050 Uiso 1 1 calc R . .
H28B H -0.1833 0.0173 0.5670 0.050 Uiso 1 1 calc R . .
H28A H -0.2202 0.1158 0.5920 0.050 Uiso 1 1 calc R . .
C29 C -0.0945(5) 0.1523(5) 0.5080(3) 0.0275(15) Uani 1 1 d . . .
H29C H -0.1356 0.2028 0.5022 0.041 Uiso 1 1 calc R . .
H29B H -0.1104 0.0986 0.4790 0.041 Uiso 1 1 calc R . .
H29A H -0.0399 0.1757 0.4953 0.041 Uiso 1 1 calc R . .
C30 C 0.3632(4) 0.0430(5) 0.5876(3) 0.0219(13) Uani 1 1 d . . .
C31 C 0.2874(4) -0.0281(5) 0.5892(4) 0.0289(15) Uani 1 1 d . . .
H31A H 0.2873 -0.0599 0.6332 0.043 Uiso 1 1 calc R . .
H31B H 0.2927 -0.0751 0.5532 0.043 Uiso 1 1 calc R . .
H31C H 0.2354 0.0069 0.5822 0.043 Uiso 1 1 calc R . .
C32 C 0.3650(5) 0.0907(6) 0.5160(3) 0.0320(17) Uani 1 1 d . . .
H32C H 0.3139 0.1269 0.5079 0.048 Uiso 1 1 calc R . .
H32B H 0.3695 0.0419 0.4812 0.048 Uiso 1 1 calc R . .
H32A H 0.4129 0.1332 0.5142 0.048 Uiso 1 1 calc R . .
C33 C 0.4442(4) -0.0181(5) 0.5958(4) 0.0287(15) Uani 1 1 d . . .
H33C H 0.4929 0.0231 0.5938 0.043 Uiso 1 1 calc R . .
H33B H 0.4457 -0.0647 0.5593 0.043 Uiso 1 1 calc R . .
H33A H 0.4446 -0.0507 0.6396 0.043 Uiso 1 1 calc R . .
C34 C 0.4813(4) 0.2057(5) 0.8089(4) 0.0266(15) Uani 1 1 d . . .
C35 C 0.5063(5) 0.3125(5) 0.8172(5) 0.039(2) Uani 1 1 d . . .
H35C H 0.4571 0.3498 0.8275 0.059 Uiso 1 1 calc R . .
H35B H 0.5296 0.3354 0.7751 0.059 Uiso 1 1 calc R . .
H35A H 0.5477 0.3189 0.8543 0.059 Uiso 1 1 calc R . .
C36 C 0.5620(4) 0.1482(6) 0.7946(4) 0.0340(17) Uani 1 1 d . . .
H36A H 0.5833 0.1671 0.7507 0.051 Uiso 1 1 calc R . .
H36B H 0.5492 0.0806 0.7940 0.051 Uiso 1 1 calc R . .
H36C H 0.6041 0.1612 0.8303 0.051 Uiso 1 1 calc R . .
C37 C 0.4477(5) 0.1715(5) 0.8773(4) 0.0317(16) Uani 1 1 d . . .
H37C H 0.4905 0.1797 0.9130 0.048 Uiso 1 1 calc R . .
H37B H 0.4327 0.1045 0.8738 0.048 Uiso 1 1 calc R . .
H37A H 0.3985 0.2084 0.8883 0.048 Uiso 1 1 calc R . .
C38 C 0.1037(5) 0.5331(5) 0.4484(4) 0.0355(17) Uani 1 1 d . . .
H38C H 0.0979 0.5772 0.4861 0.053 Uiso 1 1 calc R . .
H38B H 0.0487 0.5104 0.4333 0.053 Uiso 1 1 calc R . .
H38A H 0.1301 0.5654 0.4108 0.053 Uiso 1 1 calc R . .
C39 C 0.1573(4) 0.4490(5) 0.4715(3) 0.0243(14) Uani 1 1 d . . .
C40 C 0.2402(5) 0.4429(5) 0.4520(4) 0.0319(16) Uani 1 1 d . . .
H40 H 0.2584 0.4820 0.4164 0.038 Uiso 1 1 calc R . .
C41 C 0.2975(4) 0.3798(5) 0.4840(4) 0.0269(15) Uani 1 1 d . . .
C42 C 0.3901(5) 0.3894(7) 0.4718(5) 0.050(2) Uani 1 1 d . . .
H42C H 0.4141 0.4367 0.5028 0.075 Uiso 1 1 calc R . .
H42B H 0.3981 0.4094 0.4250 0.075 Uiso 1 1 calc R . .
H42A H 0.4174 0.3284 0.4797 0.075 Uiso 1 1 calc R . .
C43 C 0.5130(18) 0.3352(15) 0.6201(9) 0.073(8) Uani 0.50 1 d P . .
H43C H 0.5198 0.3318 0.6695 0.110 Uiso 0.50 1 calc PR . .
H43B H 0.4548 0.3241 0.6069 0.110 Uiso 0.50 1 calc PR . .
H43A H 0.5297 0.3980 0.6046 0.110 Uiso 0.50 1 calc PR . .
C44 C 0.5622(13) 0.2673(18) 0.5909(10) 0.053(5) Uani 0.50 1 d P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.594(4) . ?
V1 O3 1.817(4) . ?
V1 O2 1.839(4) . ?
V1 O4 1.989(4) . ?
V1 O5 2.008(4) . ?
V1 N1 2.452(5) . ?
N1 C7 1.476(7) . ?
N1 C8 1.483(7) . ?
N1 C15 1.485(8) . ?
C1 O3 1.335(7) . ?
C1 C2 1.397(8) . ?
C1 C6 1.425(8) . ?
O2 C14 1.350(7) . ?
C2 C3 1.402(8) . ?
C2 C7 1.501(8) . ?
N2 C21 1.333(10) . ?
N2 C17 1.345(9) . ?
C3 C4 1.381(9) . ?
C3 H3 0.9300 . ?
N3 C44 1.07(3) . ?
O4 C39 1.272(8) . ?
C4 C5 1.401(9) . ?
C4 C22 1.541(8) . ?
O5 C41 1.270(8) . ?
C5 C6 1.381(9) . ?
C5 H5 0.9300 . ?
C6 C26 1.540(8) . ?
C7 H7B 0.9700 . ?
C7 H7A 0.9700 . ?
C8 C9 1.507(8) . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C14 1.394(9) . ?
C9 C10 1.425(9) . ?
C10 C11 1.352(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(9) . ?
C11 C34 1.533(8) . ?
C12 C13 1.396(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.414(8) . ?
C13 C30 1.532(9) . ?
C15 C16 1.534(8) . ?
C15 H15B 0.9700 . ?
C15 H15A 0.9700 . ?
C16 C17 1.480(9) . ?
C16 H16B 0.9700 . ?
C16 H16A 0.9700 . ?
C17 C18 1.380(10) . ?
C18 C19 1.415(12) . ?
C18 H18 0.9300 . ?
C19 C20 1.349(14) . ?
C19 H19 0.9300 . ?
C20 C21 1.364(15) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C25 1.522(10) . ?
C22 C24 1.524(10) . ?
C22 C23 1.525(9) . ?
C23 H23C 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23A 0.9600 . ?
C24 H24C 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24A 0.9600 . ?
C25 H25C 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25A 0.9600 . ?
C26 C29 1.525(9) . ?
C26 C27 1.530(9) . ?
C26 C28 1.532(9) . ?
C27 H27C 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27A 0.9600 . ?
C28 H28C 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28A 0.9600 . ?
C29 H29C 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29A 0.9600 . ?
C30 C32 1.537(9) . ?
C30 C33 1.539(9) . ?
C30 C31 1.551(10) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32C 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32A 0.9600 . ?
C33 H33C 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33A 0.9600 . ?
C34 C37 1.517(10) . ?
C34 C36 1.538(10) . ?
C34 C35 1.540(9) . ?
C35 H35C 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35A 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37C 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37A 0.9600 . ?
C38 C39 1.502(10) . ?
C38 H38C 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38A 0.9600 . ?
C39 C40 1.376(10) . ?
C40 C41 1.391(10) . ?
C40 H40 0.9300 . ?
C41 C42 1.495(10) . ?
C42 H42C 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42A 0.9600 . ?
C43 C44 1.36(3) . ?
C43 H43C 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43A 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 98.5(2) . . ?
O1 V1 O2 100.6(2) . . ?
O3 V1 O2 99.2(2) . . ?
O1 V1 O4 96.3(2) . . ?
O3 V1 O4 88.66(18) . . ?
O2 V1 O4 160.01(19) . . ?
O1 V1 O5 94.2(2) . . ?
O3 V1 O5 165.91(19) . . ?
O2 V1 O5 84.54(19) . . ?
O4 V1 O5 83.73(18) . . ?
O1 V1 N1 176.2(2) . . ?
O3 V1 N1 82.05(18) . . ?
O2 V1 N1 82.96(18) . . ?
O4 V1 N1 79.93(17) . . ?
O5 V1 N1 84.94(17) . . ?
C7 N1 C8 108.5(5) . . ?
C7 N1 C15 109.7(5) . . ?
C8 N1 C15 111.5(5) . . ?
C7 N1 V1 108.8(4) . . ?
C8 N1 V1 108.5(3) . . ?
C15 N1 V1 109.8(4) . . ?
O3 C1 C2 120.9(5) . . ?
O3 C1 C6 118.6(5) . . ?
C2 C1 C6 120.5(5) . . ?
C14 O2 V1 135.2(4) . . ?
C1 C2 C3 118.9(5) . . ?
C1 C2 C7 122.3(5) . . ?
C3 C2 C7 118.7(5) . . ?
C21 N2 C17 119.1(8) . . ?
C1 O3 V1 144.6(4) . . ?
C4 C3 C2 122.4(5) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C39 O4 V1 130.1(4) . . ?
C3 C4 C5 117.0(5) . . ?
C3 C4 C22 123.0(6) . . ?
C5 C4 C22 120.0(6) . . ?
C41 O5 V1 128.9(4) . . ?
C6 C5 C4 123.8(6) . . ?
C6 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C5 C6 C1 117.4(6) . . ?
C5 C6 C26 121.3(6) . . ?
C1 C6 C26 121.3(5) . . ?
N1 C7 C2 116.1(5) . . ?
N1 C7 H7B 108.3 . . ?
C2 C7 H7B 108.3 . . ?
N1 C7 H7A 108.3 . . ?
C2 C7 H7A 108.3 . . ?
H7B C7 H7A 107.4 . . ?
N1 C8 C9 112.4(5) . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
H8B C8 H8A 107.8 . . ?
C14 C9 C10 119.8(5) . . ?
C14 C9 C8 118.9(5) . . ?
C10 C9 C8 121.3(5) . . ?
C11 C10 C9 120.9(5) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 118.5(6) . . ?
C10 C11 C34 117.9(6) . . ?
C12 C11 C34 123.6(6) . . ?
C13 C12 C11 123.5(6) . . ?
C13 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
C12 C13 C14 117.1(6) . . ?
C12 C13 C30 122.3(6) . . ?
C14 C13 C30 120.7(6) . . ?
O2 C14 C9 119.0(5) . . ?
O2 C14 C13 120.8(5) . . ?
C9 C14 C13 120.1(5) . . ?
N1 C15 C16 118.9(5) . . ?
N1 C15 H15B 107.6 . . ?
C16 C15 H15B 107.6 . . ?
N1 C15 H15A 107.6 . . ?
C16 C15 H15A 107.6 . . ?
H15B C15 H15A 107.0 . . ?
C17 C16 C15 108.9(5) . . ?
C17 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
C17 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
H16B C16 H16A 108.3 . . ?
N2 C17 C18 121.3(7) . . ?
N2 C17 C16 116.0(6) . . ?
C18 C17 C16 122.8(7) . . ?
C17 C18 C19 118.5(8) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 119.9(8) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
N2 C21 C20 122.5(9) . . ?
N2 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
C25 C22 C24 107.1(6) . . ?
C25 C22 C23 109.2(6) . . ?
C24 C22 C23 109.5(7) . . ?
C25 C22 C4 112.0(5) . . ?
C24 C22 C4 109.8(6) . . ?
C23 C22 C4 109.2(5) . . ?
C22 C23 H23C 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
C22 C24 H24C 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
C22 C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
C22 C25 H25C 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
C22 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C29 C26 C27 111.2(6) . . ?
C29 C26 C28 107.6(6) . . ?
C27 C26 C28 107.3(6) . . ?
C29 C26 C6 109.9(5) . . ?
C27 C26 C6 108.8(5) . . ?
C28 C26 C6 112.1(5) . . ?
C26 C27 H27C 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27C C27 H27B 109.5 . . ?
C26 C27 H27A 109.5 . . ?
H27C C27 H27A 109.5 . . ?
H27B C27 H27A 109.5 . . ?
C26 C28 H28C 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C26 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
C26 C29 H29C 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29C C29 H29B 109.5 . . ?
C26 C29 H29A 109.5 . . ?
H29C C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
C13 C30 C32 111.3(5) . . ?
C13 C30 C33 112.0(5) . . ?
C32 C30 C33 107.0(5) . . ?
C13 C30 C31 110.4(5) . . ?
C32 C30 C31 109.2(6) . . ?
C33 C30 C31 106.7(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32C 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32C C32 H32B 109.5 . . ?
C30 C32 H32A 109.5 . . ?
H32C C32 H32A 109.5 . . ?
H32B C32 H32A 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33C C33 H33B 109.5 . . ?
C30 C33 H33A 109.5 . . ?
H33C C33 H33A 109.5 . . ?
H33B C33 H33A 109.5 . . ?
C37 C34 C11 109.8(5) . . ?
C37 C34 C36 108.0(6) . . ?
C11 C34 C36 112.7(6) . . ?
C37 C34 C35 107.8(6) . . ?
C11 C34 C35 110.5(5) . . ?
C36 C34 C35 107.8(6) . . ?
C34 C35 H35C 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35C C35 H35B 109.5 . . ?
C34 C35 H35A 109.5 . . ?
H35C C35 H35A 109.5 . . ?
H35B C35 H35A 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37C 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37C C37 H37B 109.5 . . ?
C34 C37 H37A 109.5 . . ?
H37C C37 H37A 109.5 . . ?
H37B C37 H37A 109.5 . . ?
C39 C38 H38C 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38C C38 H38B 109.5 . . ?
C39 C38 H38A 109.5 . . ?
H38C C38 H38A 109.5 . . ?
H38B C38 H38A 109.5 . . ?
O4 C39 C40 124.4(6) . . ?
O4 C39 C38 115.6(6) . . ?
C40 C39 C38 119.9(6) . . ?
C39 C40 C41 121.8(6) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
O5 C41 C40 124.2(6) . . ?
O5 C41 C42 115.6(7) . . ?
C40 C41 C42 120.0(7) . . ?
C41 C42 H42C 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42C C42 H42B 109.5 . . ?
C41 C42 H42A 109.5 . . ?
H42C C42 H42A 109.5 . . ?
H42B C42 H42A 109.5 . . ?
C44 C43 H43C 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43C C43 H43B 109.5 . . ?
C44 C43 H43A 109.5 . . ?
H43C C43 H43A 109.5 . . ?
H43B C43 H43A 109.5 . . ?
N3 C44 C43 178(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 N1 C7 61(3) . . . . ?
O3 V1 N1 C7 -37.0(4) . . . . ?
O2 V1 N1 C7 -137.3(4) . . . . ?
O4 V1 N1 C7 53.0(4) . . . . ?
O5 V1 N1 C7 137.5(4) . . . . ?
O1 V1 N1 C8 179(100) . . . . ?
O3 V1 N1 C8 80.9(4) . . . . ?
O2 V1 N1 C8 -19.4(4) . . . . ?
O4 V1 N1 C8 171.0(4) . . . . ?
O5 V1 N1 C8 -104.5(4) . . . . ?
O1 V1 N1 C15 -59(3) . . . . ?
O3 V1 N1 C15 -157.0(4) . . . . ?
O2 V1 N1 C15 102.7(4) . . . . ?
O4 V1 N1 C15 -67.0(4) . . . . ?
O5 V1 N1 C15 17.5(4) . . . . ?
O1 V1 O2 C14 142.0(5) . . . . ?
O3 V1 O2 C14 -117.5(5) . . . . ?
O4 V1 O2 C14 -5.5(9) . . . . ?
O5 V1 O2 C14 48.8(6) . . . . ?
N1 V1 O2 C14 -36.8(5) . . . . ?
O3 C1 C2 C3 179.2(5) . . . . ?
C6 C1 C2 C3 0.9(9) . . . . ?
O3 C1 C2 C7 4.3(9) . . . . ?
C6 C1 C2 C7 -174.0(5) . . . . ?
C2 C1 O3 V1 11.3(10) . . . . ?
C6 C1 O3 V1 -170.4(5) . . . . ?
O1 V1 O3 C1 -171.0(7) . . . . ?
O2 V1 O3 C1 86.7(7) . . . . ?
O4 V1 O3 C1 -74.8(7) . . . . ?
O5 V1 O3 C1 -17.6(12) . . . . ?
N1 V1 O3 C1 5.2(7) . . . . ?
C1 C2 C3 C4 -2.9(9) . . . . ?
C7 C2 C3 C4 172.2(6) . . . . ?
O1 V1 O4 C39 -70.6(6) . . . . ?
O3 V1 O4 C39 -169.0(5) . . . . ?
O2 V1 O4 C39 77.3(8) . . . . ?
O5 V1 O4 C39 22.9(5) . . . . ?
N1 V1 O4 C39 108.8(5) . . . . ?
C2 C3 C4 C5 2.0(9) . . . . ?
C2 C3 C4 C22 -176.0(6) . . . . ?
O1 V1 O5 C41 69.8(6) . . . . ?
O3 V1 O5 C41 -83.9(10) . . . . ?
O2 V1 O5 C41 170.1(5) . . . . ?
O4 V1 O5 C41 -26.2(5) . . . . ?
N1 V1 O5 C41 -106.5(5) . . . . ?
C3 C4 C5 C6 0.8(10) . . . . ?
C22 C4 C5 C6 178.9(6) . . . . ?
C4 C5 C6 C1 -2.6(9) . . . . ?
C4 C5 C6 C26 177.3(6) . . . . ?
O3 C1 C6 C5 -176.6(5) . . . . ?
C2 C1 C6 C5 1.7(9) . . . . ?
O3 C1 C6 C26 3.5(8) . . . . ?
C2 C1 C6 C26 -178.2(5) . . . . ?
C8 N1 C7 C2 -58.8(6) . . . . ?
C15 N1 C7 C2 179.2(5) . . . . ?
V1 N1 C7 C2 59.1(6) . . . . ?
C1 C2 C7 N1 -45.4(8) . . . . ?
C3 C2 C7 N1 139.7(6) . . . . ?
C7 N1 C8 C9 179.1(5) . . . . ?
C15 N1 C8 C9 -60.0(6) . . . . ?
V1 N1 C8 C9 61.0(5) . . . . ?
N1 C8 C9 C14 -62.2(7) . . . . ?
N1 C8 C9 C10 120.9(6) . . . . ?
C14 C9 C10 C11 -3.4(9) . . . . ?
C8 C9 C10 C11 173.5(6) . . . . ?
C9 C10 C11 C12 1.8(9) . . . . ?
C9 C10 C11 C34 -178.5(6) . . . . ?
C10 C11 C12 C13 -1.4(9) . . . . ?
C34 C11 C12 C13 178.9(6) . . . . ?
C11 C12 C13 C14 2.5(9) . . . . ?
C11 C12 C13 C30 -175.7(6) . . . . ?
V1 O2 C14 C9 50.6(8) . . . . ?
V1 O2 C14 C13 -130.9(5) . . . . ?
C10 C9 C14 O2 -177.0(5) . . . . ?
C8 C9 C14 O2 6.0(8) . . . . ?
C10 C9 C14 C13 4.5(9) . . . . ?
C8 C9 C14 C13 -172.4(5) . . . . ?
C12 C13 C14 O2 177.5(5) . . . . ?
C30 C13 C14 O2 -4.2(9) . . . . ?
C12 C13 C14 C9 -4.0(9) . . . . ?
C30 C13 C14 C9 174.3(6) . . . . ?
C7 N1 C15 C16 58.9(7) . . . . ?
C8 N1 C15 C16 -61.3(7) . . . . ?
V1 N1 C15 C16 178.4(4) . . . . ?
N1 C15 C16 C17 -179.4(5) . . . . ?
C21 N2 C17 C18 0.3(11) . . . . ?
C21 N2 C17 C16 -179.6(7) . . . . ?
C15 C16 C17 N2 67.9(7) . . . . ?
C15 C16 C17 C18 -112.0(7) . . . . ?
N2 C17 C18 C19 -0.4(10) . . . . ?
C16 C17 C18 C19 179.4(6) . . . . ?
C17 C18 C19 C20 0.8(11) . . . . ?
C18 C19 C20 C21 -0.9(12) . . . . ?
C17 N2 C21 C20 -0.5(12) . . . . ?
C19 C20 C21 N2 0.8(14) . . . . ?
C3 C4 C22 C25 -7.4(9) . . . . ?
C5 C4 C22 C25 174.6(6) . . . . ?
C3 C4 C22 C24 -126.2(7) . . . . ?
C5 C4 C22 C24 55.8(8) . . . . ?
C3 C4 C22 C23 113.8(7) . . . . ?
C5 C4 C22 C23 -64.3(8) . . . . ?
C5 C6 C26 C29 118.1(7) . . . . ?
C1 C6 C26 C29 -62.0(7) . . . . ?
C5 C6 C26 C27 -120.0(7) . . . . ?
C1 C6 C26 C27 60.0(8) . . . . ?
C5 C6 C26 C28 -1.4(9) . . . . ?
C1 C6 C26 C28 178.5(6) . . . . ?
C12 C13 C30 C32 -117.7(7) . . . . ?
C14 C13 C30 C32 64.1(8) . . . . ?
C12 C13 C30 C33 2.1(9) . . . . ?
C14 C13 C30 C33 -176.1(6) . . . . ?
C12 C13 C30 C31 120.9(7) . . . . ?
C14 C13 C30 C31 -57.3(8) . . . . ?
C10 C11 C34 C37 66.2(7) . . . . ?
C12 C11 C34 C37 -114.1(7) . . . . ?
C10 C11 C34 C36 -173.4(6) . . . . ?
C12 C11 C34 C36 6.3(9) . . . . ?
C10 C11 C34 C35 -52.7(8) . . . . ?
C12 C11 C34 C35 127.0(7) . . . . ?
V1 O4 C39 C40 -9.8(10) . . . . ?
V1 O4 C39 C38 173.1(5) . . . . ?
O4 C39 C40 C41 -11.7(12) . . . . ?
C38 C39 C40 C41 165.3(7) . . . . ?
V1 O5 C41 C40 16.8(10) . . . . ?
V1 O5 C41 C42 -167.8(5) . . . . ?
C39 C40 C41 O5 8.0(12) . . . . ?
C39 C40 C41 C42 -167.3(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.46
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.200
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.143
####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1413241'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H59 N2 O5 V, C H4 O'
_chemical_formula_sum            'C40 H63 N2 O6 V'
_chemical_formula_weight         718.86

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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9065(5)
_cell_length_b                   14.5215(9)
_cell_length_c                   19.1809(12)
_cell_angle_alpha                67.981(3)
_cell_angle_beta                 82.406(4)
_cell_angle_gamma                86.889(3)
_cell_volume                     2023.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    97050
_cell_measurement_theta_min      4.435
_cell_measurement_theta_max      47.476

_exptl_crystal_description       Block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8758
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            96907
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         27.81
_reflns_number_total             9500
_reflns_number_gt                7353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_cell_refinement       
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_reduction        
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_solution    
'XS V2008/1 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_refinement  
'XL V2008/4 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0949P)²+0.7023P] 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         9500
_refine_ls_number_parameters     497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1573
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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 0.54869(4) 0.59285(2) 0.661947(18) 0.02082(11) Uani 1 1 d . . .
N1 N 0.2962(2) 0.59529(12) 0.74081(9) 0.0203(3) Uani 1 1 d . . .
O1M O 0.71561(17) 0.59182(11) 0.58727(8) 0.0256(3) Uani 1 1 d . . .
C1 C 0.4319(2) 0.39115(14) 0.75904(11) 0.0212(4) Uani 1 1 d . . .
C1M C 0.8938(3) 0.6009(2) 0.58514(14) 0.0366(5) Uani 1 1 d . . .
H1M1 H 0.9289 0.6689 0.5531 0.055 Uiso 1 1 calc R . .
H1M2 H 0.9539 0.5543 0.5643 0.055 Uiso 1 1 calc R . .
H1M3 H 0.9218 0.5857 0.6366 0.055 Uiso 1 1 calc R . .
O1 O 0.65960(17) 0.58625(11) 0.72695(8) 0.0262(3) Uani 1 1 d . . .
O2 O 0.51017(17) 0.72810(10) 0.62191(8) 0.0242(3) Uani 1 1 d . . .
O2M O 0.36709(18) 0.60191(11) 0.57637(8) 0.0261(3) Uani 1 1 d . . .
H2M H 0.359(3) 0.547(2) 0.5661(15) 0.035(7) Uiso 1 1 d . . .
N2 N 0.2932(3) 0.68018(17) 0.94359(14) 0.0443(5) Uani 1 1 d . . .
C2 C 0.2740(2) 0.41092(15) 0.79326(11) 0.0228(4) Uani 1 1 d . . .
C2M C 0.3459(3) 0.68615(19) 0.51002(13) 0.0367(5) Uani 1 1 d . . .
H2M1 H 0.3079 0.7429 0.5241 0.055 Uiso 1 1 calc R . .
H2M2 H 0.2604 0.6718 0.4829 0.055 Uiso 1 1 calc R . .
H2M3 H 0.4549 0.7019 0.4772 0.055 Uiso 1 1 calc R . .
O3 O 0.49195(17) 0.46026(10) 0.69128(8) 0.0230(3) Uani 1 1 d . . .
C3 C 0.2034(3) 0.34389(16) 0.86196(12) 0.0256(4) Uani 1 1 d . . .
H3 H 0.093(3) 0.3597(17) 0.8865(13) 0.026(6) Uiso 1 1 d . . .
O3M O 0.6928(3) 0.55087(13) 0.46049(10) 0.0459(5) Uani 1 1 d . . .
H3M H 0.678(4) 0.556(2) 0.5055(19) 0.053(9) Uiso 1 1 d . . .
C3M C 0.7733(4) 0.6347(2) 0.40484(15) 0.0443(6) Uani 1 1 d . . .
H3M1 H 0.7298 0.6944 0.4136 0.066 Uiso 1 1 calc R . .
H3M2 H 0.7498 0.6392 0.3548 0.066 Uiso 1 1 calc R . .
H3M3 H 0.8967 0.6293 0.4072 0.066 Uiso 1 1 calc R . .
C4 C 0.2848(3) 0.25421(16) 0.89831(12) 0.0267(4) Uani 1 1 d . . .
C5 C 0.4401(3) 0.23609(16) 0.86221(12) 0.0258(4) Uani 1 1 d . . .
H5 H 0.492(3) 0.1805(18) 0.8826(13) 0.024(6) Uiso 1 1 d . . .
C6 C 0.5184(2) 0.30159(15) 0.79314(11) 0.0239(4) Uani 1 1 d . . .
C7 C 0.1897(2) 0.50765(14) 0.75184(11) 0.0223(4) Uani 1 1 d . . .
H7A H 0.1678 0.5092 0.7018 0.027 Uiso 1 1 calc R . .
H7B H 0.0783 0.5123 0.7807 0.027 Uiso 1 1 calc R . .
C8 C 0.1976(2) 0.68691(14) 0.70208(11) 0.0218(4) Uani 1 1 d . . .
H8A H 0.0848 0.6846 0.7321 0.026 Uiso 1 1 calc R . .
H8B H 0.1781 0.6886 0.6517 0.026 Uiso 1 1 calc R . .
C9 C 0.2878(2) 0.77961(15) 0.69245(11) 0.0221(4) Uani 1 1 d . . .
C10 C 0.2195(3) 0.84536(16) 0.72559(12) 0.0261(4) Uani 1 1 d . . .
H10 H 0.109(3) 0.8296(19) 0.7565(15) 0.035(7) Uiso 1 1 d . . .
C11 C 0.3073(3) 0.92947(16) 0.71695(12) 0.0286(4) Uani 1 1 d . . .
C12 C 0.4638(3) 0.94706(16) 0.67133(13) 0.0295(5) Uani 1 1 d . . .
H12 H 0.528(3) 1.0080(18) 0.6637(13) 0.027(6) Uiso 1 1 d . . .
C13 C 0.5389(3) 0.88390(15) 0.63677(12) 0.0256(4) Uani 1 1 d . . .
C14 C 0.4487(2) 0.79671(15) 0.65031(11) 0.0223(4) Uani 1 1 d . . .
C15 C 0.3362(2) 0.59344(15) 0.81520(11) 0.0233(4) Uani 1 1 d . . .
H15A H 0.4097 0.6510 0.8057 0.028 Uiso 1 1 calc R . .
H15B H 0.4031 0.5325 0.8390 0.028 Uiso 1 1 calc R . .
C16 C 0.1809(3) 0.59622(18) 0.87188(12) 0.0297(5) Uani 1 1 d . . .
H16A H 0.1138 0.6575 0.8496 0.036 Uiso 1 1 calc R . .
H16B H 0.1067 0.5385 0.8828 0.036 Uiso 1 1 calc R . .
C17 C 0.2390(3) 0.59358(17) 0.94414(12) 0.0274(4) Uani 1 1 d . . .
C18 C 0.2373(3) 0.5081(2) 1.00642(14) 0.0377(5) Uani 1 1 d . . .
H18 H 0.203(4) 0.457(2) 1.0055(18) 0.051(9) Uiso 1 1 d . . .
C19 C 0.2937(4) 0.5093(3) 1.07133(16) 0.0490(7) Uani 1 1 d . . .
H19 H 0.291(4) 0.451(3) 1.1129(19) 0.060(9) Uiso 1 1 d . . .
C20 C 0.3494(3) 0.5958(3) 1.07126(17) 0.0501(7) Uani 1 1 d . . .
H20 H 0.388(4) 0.598(2) 1.1156(19) 0.063(10) Uiso 1 1 d . . .
C21 C 0.3464(4) 0.6789(2) 1.00717(19) 0.0517(7) Uani 1 1 d . . .
H21 H 0.380(5) 0.747(3) 1.006(2) 0.071(10) Uiso 1 1 d . . .
C22 C 0.2040(3) 0.18190(17) 0.97492(13) 0.0320(5) Uani 1 1 d . . .
C23 C 0.0302(3) 0.14849(19) 0.96563(15) 0.0399(6) Uani 1 1 d . . .
H23A H -0.0424 0.2068 0.9449 0.060 Uiso 1 1 calc R . .
H23B H -0.0247 0.1047 1.0151 0.060 Uiso 1 1 calc R . .
H23C H 0.0466 0.1125 0.9310 0.060 Uiso 1 1 calc R . .
C24 C 0.3130(3) 0.08878(18) 1.00773(14) 0.0416(6) Uani 1 1 d . . .
H24A H 0.3329 0.0549 0.9718 0.062 Uiso 1 1 calc R . .
H24B H 0.2533 0.0440 1.0556 0.062 Uiso 1 1 calc R . .
H24C H 0.4227 0.1079 1.0168 0.062 Uiso 1 1 calc R . .
C25 C 0.1789(4) 0.23514(19) 1.03165(14) 0.0419(6) Uani 1 1 d . . .
H25A H 0.2891 0.2594 1.0356 0.063 Uiso 1 1 calc R . .
H25B H 0.1313 0.1885 1.0815 0.063 Uiso 1 1 calc R . .
H25C H 0.1003 0.2913 1.0139 0.063 Uiso 1 1 calc R . .
C26 C 0.6921(3) 0.27765(16) 0.75725(12) 0.0278(4) Uani 1 1 d . . .
C27 C 0.6798(3) 0.28457(19) 0.67653(14) 0.0375(5) Uani 1 1 d . . .
H27A H 0.7920 0.2712 0.6536 0.056 Uiso 1 1 calc R . .
H27B H 0.6417 0.3514 0.6464 0.056 Uiso 1 1 calc R . .
H27C H 0.5977 0.2356 0.6778 0.056 Uiso 1 1 calc R . .
C28 C 0.8265(3) 0.35050(19) 0.75542(15) 0.0361(5) Uani 1 1 d . . .
H28A H 0.8394 0.3433 0.8073 0.054 Uiso 1 1 calc R . .
H28B H 0.7904 0.4185 0.7271 0.054 Uiso 1 1 calc R . .
H28C H 0.9358 0.3364 0.7307 0.054 Uiso 1 1 calc R . .
C29 C 0.7541(3) 0.17316(19) 0.80204(15) 0.0405(6) Uani 1 1 d . . .
H29A H 0.8627 0.1598 0.7763 0.061 Uiso 1 1 calc R . .
H29B H 0.6692 0.1245 0.8055 0.061 Uiso 1 1 calc R . .
H29C H 0.7703 0.1682 0.8531 0.061 Uiso 1 1 calc R . .
C30 C 0.7140(3) 0.90617(16) 0.58876(14) 0.0321(5) Uani 1 1 d . . .
C31 C 0.7089(3) 0.89831(19) 0.51180(14) 0.0385(5) Uani 1 1 d . . .
H31A H 0.6714 0.8317 0.5193 0.058 Uiso 1 1 calc R . .
H31B H 0.8231 0.9104 0.4832 0.058 Uiso 1 1 calc R . .
H31C H 0.6289 0.9478 0.4835 0.058 Uiso 1 1 calc R . .
C32 C 0.8439(3) 0.83218(19) 0.63277(16) 0.0396(6) Uani 1 1 d . . .
H32A H 0.8487 0.8396 0.6812 0.059 Uiso 1 1 calc R . .
H32B H 0.9568 0.8453 0.6030 0.059 Uiso 1 1 calc R . .
H32C H 0.8094 0.7643 0.6422 0.059 Uiso 1 1 calc R . .
C33 C 0.7726(3) 1.01161(19) 0.57397(19) 0.0511(7) Uani 1 1 d . . .
H33A H 0.6896 1.0600 0.5468 0.077 Uiso 1 1 calc R . .
H33B H 0.8843 1.0239 0.5432 0.077 Uiso 1 1 calc R . .
H33C H 0.7812 1.0183 0.6224 0.077 Uiso 1 1 calc R . .
C34 C 0.2434(3) 1.00037(19) 0.75677(16) 0.0423(6) Uani 1 1 d . . .
C35 C 0.2279(6) 1.1047(2) 0.6997(2) 0.0824(14) Uani 1 1 d . . .
H35A H 0.1410 1.1065 0.6672 0.124 Uiso 1 1 calc R . .
H35B H 0.3379 1.1254 0.6685 0.124 Uiso 1 1 calc R . .
H35C H 0.1948 1.1500 0.7264 0.124 Uiso 1 1 calc R . .
C36 C 0.0744(4) 0.9686(2) 0.80502(17) 0.0486(7) Uani 1 1 d . . .
H36A H -0.0125 0.9693 0.7728 0.073 Uiso 1 1 calc R . .
H36B H 0.0407 1.0145 0.8311 0.073 Uiso 1 1 calc R . .
H36C H 0.0851 0.9013 0.8425 0.073 Uiso 1 1 calc R . .
C37 C 0.3741(5) 0.9983(4) 0.8106(3) 0.0927(15) Uani 1 1 d . . .
H37A H 0.3387 1.0456 0.8353 0.139 Uiso 1 1 calc R . .
H37B H 0.4868 1.0168 0.7815 0.139 Uiso 1 1 calc R . .
H37C H 0.3795 0.9313 0.8492 0.139 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 O1 1.5884(14) . ?
V1 O1M 1.8187(14) . ?
V1 O2 1.8455(14) . ?
V1 O3 1.8548(14) . ?
V1 O2M 2.2834(15) . ?
V1 N1 2.3472(16) . ?
N1 C15 1.492(2) . ?
N1 C8 1.493(2) . ?
N1 C7 1.497(2) . ?
O1M C1M 1.415(3) . ?
C1 O3 1.354(2) . ?
C1 C2 1.399(3) . ?
C1 C6 1.404(3) . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O2 C14 1.345(2) . ?
O2M C2M 1.418(3) . ?
O2M H2M 0.90(3) . ?
N2 C21 1.335(4) . ?
N2 C17 1.346(3) . ?
C2 C3 1.378(3) . ?
C2 C7 1.500(3) . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?
C3 C4 1.394(3) . ?
C3 H3 0.99(2) . ?
O3M C3M 1.399(3) . ?
O3M H3M 0.89(3) . ?
C3M H3M1 0.9800 . ?
C3M H3M2 0.9800 . ?
C3M H3M3 0.9800 . ?
C4 C5 1.390(3) . ?
C4 C22 1.529(3) . ?
C5 C6 1.395(3) . ?
C5 H5 0.86(3) . ?
C6 C26 1.536(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.496(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.384(3) . ?
C9 C14 1.395(3) . ?
C10 C11 1.382(3) . ?
C10 H10 0.97(3) . ?
C11 C12 1.394(3) . ?
C11 C34 1.526(3) . ?
C12 C13 1.388(3) . ?
C12 H12 1.00(2) . ?
C13 C14 1.408(3) . ?
C13 C30 1.535(3) . ?
C15 C16 1.538(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.503(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.361(3) . ?
C18 C19 1.383(4) . ?
C18 H18 0.81(3) . ?
C19 C20 1.354(5) . ?
C19 H19 0.92(3) . ?
C20 C21 1.363(5) . ?
C20 H20 0.96(3) . ?
C21 H21 1.02(4) . ?
C22 C24 1.532(3) . ?
C22 C23 1.536(3) . ?
C22 C25 1.542(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.527(3) . ?
C26 C29 1.528(3) . ?
C26 C27 1.530(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.528(4) . ?
C30 C32 1.534(3) . ?
C30 C33 1.535(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.508(4) . ?
C34 C35 1.510(4) . ?
C34 C37 1.547(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O1M 100.75(7) . . ?
O1 V1 O2 100.04(7) . . ?
O1M V1 O2 95.42(6) . . ?
O1 V1 O3 100.28(7) . . ?
O1M V1 O3 94.98(6) . . ?
O2 V1 O3 154.98(6) . . ?
O1 V1 O2M 174.62(7) . . ?
O1M V1 O2M 84.63(6) . . ?
O2 V1 O2M 79.53(6) . . ?
O3 V1 O2M 78.87(6) . . ?
O1 V1 N1 90.73(6) . . ?
O1M V1 N1 168.51(6) . . ?
O2 V1 N1 82.73(6) . . ?
O3 V1 N1 82.56(6) . . ?
O2M V1 N1 83.89(6) . . ?
C15 N1 C8 110.42(15) . . ?
C15 N1 C7 110.55(15) . . ?
C8 N1 C7 107.72(14) . . ?
C15 N1 V1 110.37(11) . . ?
C8 N1 V1 108.62(11) . . ?
C7 N1 V1 109.10(12) . . ?
C1M O1M V1 127.85(14) . . ?
O3 C1 C2 116.87(17) . . ?
O3 C1 C6 122.55(17) . . ?
C2 C1 C6 120.54(18) . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C14 O2 V1 135.14(13) . . ?
C2M O2M V1 124.96(14) . . ?
C2M O2M H2M 108.7(17) . . ?
V1 O2M H2M 116.0(17) . . ?
C21 N2 C17 117.0(2) . . ?
C3 C2 C1 120.42(19) . . ?
C3 C2 C7 122.92(18) . . ?
C1 C2 C7 116.66(17) . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?
C1 O3 V1 132.26(12) . . ?
C2 C3 C4 121.21(19) . . ?
C2 C3 H3 119.7(14) . . ?
C4 C3 H3 119.1(14) . . ?
C3M O3M H3M 112(2) . . ?
O3M C3M H3M1 109.5 . . ?
O3M C3M H3M2 109.5 . . ?
H3M1 C3M H3M2 109.5 . . ?
O3M C3M H3M3 109.5 . . ?
H3M1 C3M H3M3 109.5 . . ?
H3M2 C3M H3M3 109.5 . . ?
C5 C4 C3 116.93(19) . . ?
C5 C4 C22 123.1(2) . . ?
C3 C4 C22 119.92(19) . . ?
C4 C5 C6 124.4(2) . . ?
C4 C5 H5 119.2(16) . . ?
C6 C5 H5 116.4(16) . . ?
C5 C6 C1 116.53(18) . . ?
C5 C6 C26 121.57(19) . . ?
C1 C6 C26 121.89(18) . . ?
N1 C7 C2 112.30(15) . . ?
N1 C7 H7A 109.1 . . ?
C2 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C2 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N1 C8 C9 112.33(15) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C14 120.20(18) . . ?
C10 C9 C8 122.34(18) . . ?
C14 C9 C8 117.43(18) . . ?
C11 C10 C9 121.08(19) . . ?
C11 C10 H10 120.9(15) . . ?
C9 C10 H10 118.0(15) . . ?
C10 C11 C12 117.3(2) . . ?
C10 C11 C34 123.1(2) . . ?
C12 C11 C34 119.6(2) . . ?
C13 C12 C11 124.2(2) . . ?
C13 C12 H12 117.5(14) . . ?
C11 C12 H12 118.3(14) . . ?
C12 C13 C14 116.41(19) . . ?
C12 C13 C30 121.71(19) . . ?
C14 C13 C30 121.84(19) . . ?
O2 C14 C9 117.16(17) . . ?
O2 C14 C13 122.18(18) . . ?
C9 C14 C13 120.64(19) . . ?
N1 C15 C16 115.51(16) . . ?
N1 C15 H15A 108.4 . . ?
C16 C15 H15A 108.4 . . ?
N1 C15 H15B 108.4 . . ?
C16 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C17 C16 C15 110.03(17) . . ?
C17 C16 H16A 109.7 . . ?
C15 C16 H16A 109.7 . . ?
C17 C16 H16B 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N2 C17 C18 122.0(2) . . ?
N2 C17 C16 116.3(2) . . ?
C18 C17 C16 121.7(2) . . ?
C17 C18 C19 119.5(3) . . ?
C17 C18 H18 120(2) . . ?
C19 C18 H18 120(2) . . ?
C20 C19 C18 118.9(3) . . ?
C20 C19 H19 123(2) . . ?
C18 C19 H19 118(2) . . ?
C19 C20 C21 118.6(3) . . ?
C19 C20 H20 120(2) . . ?
C21 C20 H20 121(2) . . ?
N2 C21 C20 124.0(3) . . ?
N2 C21 H21 115(2) . . ?
C20 C21 H21 121(2) . . ?
C4 C22 C24 112.95(19) . . ?
C4 C22 C23 109.19(19) . . ?
C24 C22 C23 107.9(2) . . ?
C4 C22 C25 108.95(18) . . ?
C24 C22 C25 108.3(2) . . ?
C23 C22 C25 109.5(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C29 107.33(19) . . ?
C28 C26 C27 109.39(19) . . ?
C29 C26 C27 107.90(19) . . ?
C28 C26 C6 110.00(18) . . ?
C29 C26 C6 111.98(18) . . ?
C27 C26 C6 110.16(17) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C32 110.4(2) . . ?
C31 C30 C33 107.5(2) . . ?
C32 C30 C33 108.3(2) . . ?
C31 C30 C13 111.31(18) . . ?
C32 C30 C13 108.25(19) . . ?
C33 C30 C13 111.13(19) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 109.6(2) . . ?
C36 C34 C11 112.3(2) . . ?
C35 C34 C11 110.6(2) . . ?
C36 C34 C37 107.0(3) . . ?
C35 C34 C37 109.6(3) . . ?
C11 C34 C37 107.8(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 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
O1 V1 N1 C15 1.88(13) . . . . ?
O1M V1 N1 C15 -179.6(3) . . . . ?
O2 V1 N1 C15 -98.15(12) . . . . ?
O3 V1 N1 C15 102.15(12) . . . . ?
O2M V1 N1 C15 -178.32(13) . . . . ?
O1 V1 N1 C8 123.06(12) . . . . ?
O1M V1 N1 C8 -58.4(4) . . . . ?
O2 V1 N1 C8 23.03(12) . . . . ?
O3 V1 N1 C8 -136.67(12) . . . . ?
O2M V1 N1 C8 -57.14(12) . . . . ?
O1 V1 N1 C7 -119.77(12) . . . . ?
O1M V1 N1 C7 58.8(4) . . . . ?
O2 V1 N1 C7 140.19(12) . . . . ?
O3 V1 N1 C7 -19.50(12) . . . . ?
O2M V1 N1 C7 60.02(12) . . . . ?
O1 V1 O1M C1M -9.95(19) . . . . ?
O2 V1 O1M C1M 91.38(18) . . . . ?
O3 V1 O1M C1M -111.42(18) . . . . ?
O2M V1 O1M C1M 170.29(18) . . . . ?
N1 V1 O1M C1M 171.5(3) . . . . ?
O1 V1 O2 C14 -52.62(18) . . . . ?
O1M V1 O2 C14 -154.57(17) . . . . ?
O3 V1 O2 C14 91.3(2) . . . . ?
O2M V1 O2 C14 121.93(18) . . . . ?
N1 V1 O2 C14 36.84(17) . . . . ?
O1 V1 O2M C2M 111.7(7) . . . . ?
O1M V1 O2M C2M -70.77(17) . . . . ?
O2 V1 O2M C2M 25.77(17) . . . . ?
O3 V1 O2M C2M -166.93(17) . . . . ?
N1 V1 O2M C2M 109.48(17) . . . . ?
O3 C1 C2 C3 179.45(17) . . . . ?
C6 C1 C2 C3 1.8(3) . . . . ?
O3 C1 C2 C7 -1.1(3) . . . . ?
C6 C1 C2 C7 -178.84(17) . . . . ?
C2 C1 O3 V1 60.9(2) . . . . ?
C6 C1 O3 V1 -121.48(18) . . . . ?
O1 V1 O3 C1 46.94(17) . . . . ?
O1M V1 O3 C1 148.83(16) . . . . ?
O2 V1 O3 C1 -96.9(2) . . . . ?
O2M V1 O3 C1 -127.66(17) . . . . ?
N1 V1 O3 C1 -42.46(16) . . . . ?
C1 C2 C3 C4 -1.4(3) . . . . ?
C7 C2 C3 C4 179.27(18) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C2 C3 C4 C22 179.36(19) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C22 C4 C5 C6 -178.6(2) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C4 C5 C6 C26 178.72(19) . . . . ?
O3 C1 C6 C5 -178.59(18) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
O3 C1 C6 C26 2.6(3) . . . . ?
C2 C1 C6 C26 -179.81(18) . . . . ?
C15 N1 C7 C2 -57.0(2) . . . . ?
C8 N1 C7 C2 -177.76(16) . . . . ?
V1 N1 C7 C2 64.51(17) . . . . ?
C3 C2 C7 N1 119.0(2) . . . . ?
C1 C2 C7 N1 -60.4(2) . . . . ?
C15 N1 C8 C9 55.6(2) . . . . ?
C7 N1 C8 C9 176.42(16) . . . . ?
V1 N1 C8 C9 -65.54(17) . . . . ?
N1 C8 C9 C10 -118.0(2) . . . . ?
N1 C8 C9 C14 59.9(2) . . . . ?
C14 C9 C10 C11 0.9(3) . . . . ?
C8 C9 C10 C11 178.71(19) . . . . ?
C9 C10 C11 C12 2.3(3) . . . . ?
C9 C10 C11 C34 -175.6(2) . . . . ?
C10 C11 C12 C13 -2.5(3) . . . . ?
C34 C11 C12 C13 175.5(2) . . . . ?
C11 C12 C13 C14 -0.6(3) . . . . ?
C11 C12 C13 C30 -178.4(2) . . . . ?
V1 O2 C14 C9 -55.2(3) . . . . ?
V1 O2 C14 C13 126.65(18) . . . . ?
C10 C9 C14 O2 177.70(18) . . . . ?
C8 C9 C14 O2 -0.2(3) . . . . ?
C10 C9 C14 C13 -4.1(3) . . . . ?
C8 C9 C14 C13 177.93(18) . . . . ?
C12 C13 C14 O2 -178.02(18) . . . . ?
C30 C13 C14 O2 -0.2(3) . . . . ?
C12 C13 C14 C9 3.9(3) . . . . ?
C30 C13 C14 C9 -178.27(19) . . . . ?
C8 N1 C15 C16 59.1(2) . . . . ?
C7 N1 C15 C16 -60.0(2) . . . . ?
V1 N1 C15 C16 179.21(14) . . . . ?
N1 C15 C16 C17 179.78(17) . . . . ?
C21 N2 C17 C18 0.2(4) . . . . ?
C21 N2 C17 C16 -179.5(2) . . . . ?
C15 C16 C17 N2 79.8(2) . . . . ?
C15 C16 C17 C18 -99.9(2) . . . . ?
N2 C17 C18 C19 -0.4(4) . . . . ?
C16 C17 C18 C19 179.3(2) . . . . ?
C17 C18 C19 C20 0.0(4) . . . . ?
C18 C19 C20 C21 0.5(4) . . . . ?
C17 N2 C21 C20 0.3(4) . . . . ?
C19 C20 C21 N2 -0.7(5) . . . . ?
C5 C4 C22 C24 0.8(3) . . . . ?
C3 C4 C22 C24 -178.3(2) . . . . ?
C5 C4 C22 C23 -119.2(2) . . . . ?
C3 C4 C22 C23 61.7(3) . . . . ?
C5 C4 C22 C25 121.2(2) . . . . ?
C3 C4 C22 C25 -57.8(3) . . . . ?
C5 C6 C26 C28 -114.0(2) . . . . ?
C1 C6 C26 C28 64.8(3) . . . . ?
C5 C6 C26 C29 5.3(3) . . . . ?
C1 C6 C26 C29 -176.0(2) . . . . ?
C5 C6 C26 C27 125.4(2) . . . . ?
C1 C6 C26 C27 -55.9(3) . . . . ?
C12 C13 C30 C31 -129.8(2) . . . . ?
C14 C13 C30 C31 52.5(3) . . . . ?
C12 C13 C30 C32 108.8(2) . . . . ?
C14 C13 C30 C32 -69.0(3) . . . . ?
C12 C13 C30 C33 -10.0(3) . . . . ?
C14 C13 C30 C33 172.3(2) . . . . ?
C10 C11 C34 C36 -0.7(4) . . . . ?
C12 C11 C34 C36 -178.6(2) . . . . ?
C10 C11 C34 C35 -123.5(3) . . . . ?
C12 C11 C34 C35 58.6(3) . . . . ?
C10 C11 C34 C37 116.8(3) . . . . ?
C12 C11 C34 C37 -61.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2M H2M O3M 0.90(3) 1.76(3) 2.650(2) 169(3) 2_666
O3M H3M O1M 0.89(3) 1.89(3) 2.741(2) 160(3) .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.81
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.107
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1413242'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H104 N4 O7 V2'
_chemical_formula_sum            'C74 H104 N4 O7 V2'
_chemical_formula_weight         1263.49

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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6149(6)
_cell_length_b                   15.8957(9)
_cell_length_c                   23.0172(12)
_cell_angle_alpha                80.123(3)
_cell_angle_beta                 85.922(3)
_cell_angle_gamma                75.312(3)
_cell_volume                     3699.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    76430
_cell_measurement_theta_min      5.277
_cell_measurement_theta_max      37.804

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            76068
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.1623
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         0.90
_diffrn_reflns_theta_max         28.06
_reflns_number_total             17675
_reflns_number_gt                6272
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_cell_refinement       
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_reduction        
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_solution    
'XS V2008/1 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_refinement  
'XL V2008/4 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;
_iucr_refine-instructions_details 
;

TITL    v2o3 in P -1
CELL   0.71073  10.6149  15.8957  23.0172  80.123  85.922  75.312
ZERR    2       0.0006   0.0009   0.0012   0.003   0.003   0.003
LATT  1
SFAC    C   H   N   O   V
UNIT   148 208   8  14   4
MERG    2
L.S.    180
FMAP    2
PLAN    -10
SIZE 0.3 0.2 0.1
ACTA
CONF
WPDB -1
BOND $H
HTAB
MPLA O1 O2 O3 N1
MPLA O5 O6 O7 N3
 
SADI C26 C27A C26 C27B C26 C28A C26 C28B C26 C29A C26 C29B
SIMU C26 C27A C27B C28A C28B C29A C29B
DELU C26 C27A C27B C28A C28B C29A C29B
SADI C30 C31A C30 C31B C30 C32A C30 C32B C30 C33A C30 C33B
SIMU C30 C31A C31B C32A C32B C33A C33B
DELU C30 C31A C31B C32A C32B C33A C33B
SADI C59 C60A C59 C60B C59 C61A C59 C61B C59 C62A C59 C62B
SIMU C59 C60A C60B C61A C61B C62A C62B
DELU C59 C60A C60B C61A C61B C62A C62B
DFIX 1.100 0.001 C61A C61B
SADI C5 C6A C5 C6B
SADI C6A C7 C6B C7
SADI C42 C43A C42 C43B
SADI C43A C44 C43B C44
SIMU C5 C6A C6B C7
DELU C5 C6A C6B C7
SIMU C42 C43A C43B C44
DELU C42 C43A C43B C44
 
WGHT    0.126300
EXTI    0.015710
FVAR       0.13832   0.56667   0.44182   0.83216   0.84836   0.74491
V1    5    0.358923    0.478321    0.541406    11.00000    0.05668    0.07257 =
         0.04068   -0.01394   -0.01155   -0.00577
O1    4    0.421733    0.357699    0.555638    11.00000    0.07311    0.06516 =
         0.05247   -0.01131   -0.01592   -0.01206
N1    3    0.471961    0.468745    0.629666    11.00000    0.05228    0.06711 =
         0.04087   -0.01077   -0.00621   -0.00946
C1    1    0.079545    0.461251    0.580868    11.00000    0.07830    0.28482 =
         0.06224    0.00218   -0.01722   -0.06278
AFIX  43
H1    2    0.075526    0.481135    0.540456    11.00000   -1.20000
AFIX   0
V2    5   -0.040870    0.558749    0.927345    11.00000    0.05034    0.06055 =
         0.04598   -0.00990   -0.00344   -0.01467
N2    3    0.191277    0.449403    0.606461    11.00000    0.05985    0.11047 =
         0.05132   -0.01101   -0.00905   -0.01321
C2    1   -0.033004    0.445603    0.611069    11.00000    0.07987    0.31709 =
         0.09303    0.00539   -0.01175   -0.07845
AFIX  43
H2    2   -0.109060    0.453587    0.590885    11.00000   -1.20000
AFIX   0
O2    4    0.290001    0.593721    0.553528    11.00000    0.06418    0.07854 =
         0.04880   -0.02408   -0.01338    0.00576
O3    4    0.264723    0.480840    0.489185    11.00000    0.06188    0.08621 =
         0.04730   -0.01654   -0.01506   -0.01043
N3    3    0.183269    0.511921    0.898747    11.00000    0.05953    0.05635 =
         0.04139   -0.00603    0.00093   -0.01235
C3    1   -0.030161    0.419241    0.668832    11.00000    0.09916    0.27174 =
         0.07057   -0.00528    0.00147   -0.06928
AFIX  43
H3    2   -0.104693    0.410046    0.690045    11.00000   -1.20000
AFIX   0
O4    4    0.500000    0.500000    0.500000    10.50000    0.05272    0.06387 =
         0.04749   -0.01269   -0.00547   -0.00557
N4    3   -0.062778    0.625532    0.828672    11.00000    0.06245    0.09928 =
         0.05149   -0.00302   -0.00784   -0.01553
C4    1    0.084026    0.405838    0.696610    11.00000    0.09683    0.21587 =
         0.06301   -0.01857    0.00184   -0.07438
AFIX  43
H4    2    0.088564    0.386649    0.737089    11.00000   -1.20000
AFIX   0
O5    4   -0.054735    0.461017    0.897005    11.00000    0.07045    0.06979 =
         0.06540   -0.02954    0.00041   -0.02044
C5    1    0.192879    0.420923    0.664289    11.00000    0.08093    0.12719 =
         0.05200   -0.02047    0.00044   -0.03617
O6    4    0.008033    0.659117    0.935937    11.00000    0.04477    0.05275 =
         0.06278   -0.00821   -0.00086   -0.01496
PART 1
C6A   1    0.325603    0.387757    0.694883    51.00000    0.08956    0.07654 =
         0.03949   -0.01059   -0.00236   -0.01635
AFIX  23
H6A1  2    0.309727    0.370305    0.736702    51.00000   -1.20000
H6A2  2    0.374797    0.335704    0.679353    51.00000   -1.20000
AFIX   0
PART 2
C6B   1    0.265777    0.476342    0.693714   -51.00000    0.07476    0.11361 =
         0.01567   -0.01306   -0.00041   -0.02106
AFIX  23
H6B1  2    0.235112    0.537856    0.676689   -51.00000   -1.20000
H6B2  2    0.241959    0.470896    0.735417   -51.00000   -1.20000
AFIX   0
PART 0
C7    1    0.405639    0.452123    0.687671    11.00000    0.07658    0.08772 =
         0.04539   -0.00571   -0.00827   -0.01890
AFIX  23
H7A   2    0.471600    0.432542    0.717432    11.00000   -1.20000
H7B   2    0.350345    0.507763    0.695892    11.00000   -1.20000
AFIX   0
O7    4   -0.194666    0.598648    0.934705    11.00000    0.05012    0.07213 =
         0.05804   -0.01162   -0.00581   -0.01426
O8    4    0.000000    0.500000    1.000000    10.50000    0.05888    0.05565 =
         0.04379   -0.00679   -0.00326   -0.01327
C8    1    0.510084    0.554362    0.625267    11.00000    0.05967    0.06380 =
         0.05625   -0.01325   -0.01415   -0.01031
AFIX  23
H8A   2    0.559352    0.563414    0.588580    11.00000   -1.20000
H8B   2    0.567462    0.549560    0.657286    11.00000   -1.20000
AFIX   0
C9    1    0.596324    0.400842    0.626107    11.00000    0.05005    0.07279 =
         0.04772   -0.01469   -0.01441   -0.00329
AFIX  23
H9A   2    0.648488    0.400975    0.659009    11.00000   -1.20000
H9B   2    0.643078    0.418745    0.590260    11.00000   -1.20000
AFIX   0
C10   1    0.504280    0.290362    0.588287    11.00000    0.06368    0.07274 =
         0.04483   -0.01372   -0.00742   -0.00487
C11   1    0.500458    0.202962    0.585480    11.00000    0.08347    0.06611 =
         0.06278   -0.01998   -0.00575   -0.01527
C12   1    0.588409    0.136895    0.620745    11.00000    0.09284    0.06087 =
         0.08474   -0.01793   -0.01786   -0.00364
AFIX  43
H12   2    0.588758    0.078723    0.619307    11.00000   -1.20000
AFIX   0
C13   1    0.674236    0.151666    0.657317    11.00000    0.08881    0.06414 =
         0.07544   -0.01855   -0.01587   -0.00322
C14   1    0.670581    0.238185    0.659855    11.00000    0.06702    0.07141 =
         0.05913   -0.01851   -0.01578   -0.00148
AFIX  43
H14   2    0.726109    0.249991    0.685179    11.00000   -1.20000
AFIX   0
C15   1    0.588212    0.307941    0.626493    11.00000    0.05378    0.06577 =
         0.05297   -0.01724   -0.00751   -0.00372
C16   1    0.296046    0.653551    0.587909    11.00000    0.06068    0.07931 =
         0.04296   -0.01629   -0.00581    0.00047
C17   1    0.201709    0.733711    0.583916    11.00000    0.07105    0.07753 =
         0.05565   -0.01864   -0.00520    0.00876
C18   1    0.213689    0.790370    0.621897    11.00000    0.08068    0.07388 =
         0.07312   -0.02592   -0.00798    0.00899
AFIX  43
H18   2    0.151351    0.843701    0.619809    11.00000   -1.20000
AFIX   0
C19   1    0.309423    0.774316    0.662089    11.00000    0.07899    0.07468 =
         0.08150   -0.03560   -0.00425   -0.00483
C20   1    0.403015    0.693134    0.664362    11.00000    0.08060    0.06903 =
         0.05613   -0.01729   -0.00930   -0.01490
AFIX  43
H20   2    0.469144    0.678992    0.691406    11.00000   -1.20000
AFIX   0
C21   1    0.398759    0.634206    0.627401    11.00000    0.05439    0.06541 =
         0.04808   -0.01732   -0.00273    0.00039
C22   1    0.407028    0.182234    0.545785    11.00000    0.10704    0.08093 =
         0.07687   -0.02206   -0.01894   -0.03256
C23   1    0.268338    0.215802    0.568316    11.00000    0.11481    0.15647 =
         0.11861   -0.02781   -0.03147   -0.06431
AFIX 137
H23A  2    0.260368    0.191050    0.609089    11.00000   -1.50000
H23B  2    0.209126    0.198696    0.545704    11.00000   -1.50000
H23C  2    0.247899    0.278867    0.564390    11.00000   -1.50000
AFIX   0
C24   1    0.421451    0.225187    0.481895    11.00000    0.15753    0.17149 =
         0.07083   -0.04224   -0.01166   -0.07076
AFIX 137
H24A  2    0.411588    0.287255    0.480326    11.00000   -1.50000
H24B  2    0.355733    0.215899    0.458846    11.00000   -1.50000
H24C  2    0.506105    0.199430    0.466319    11.00000   -1.50000
AFIX   0
C25   1    0.425750    0.082963    0.547963    11.00000    0.21267    0.09607 =
         0.20110   -0.04473   -0.10573   -0.03720
AFIX 137
H25A  2    0.508734    0.058947    0.530149    11.00000   -1.50000
H25B  2    0.357703    0.072735    0.526823    11.00000   -1.50000
H25C  2    0.422544    0.055004    0.588282    11.00000   -1.50000
AFIX   0
C26   1    0.768834    0.074093    0.694018    11.00000    0.10735    0.07214 =
         0.11361   -0.00582   -0.04569    0.01180
PART   1
C27A  1    0.693268    0.009963    0.726268    21.00000    0.17865    0.10468 =
         0.20804    0.07368   -0.07810   -0.01842
AFIX 137
H27A  2    0.751500   -0.047141    0.736001    21.00000   -1.50000
H27B  2    0.626674    0.006202    0.701400    21.00000   -1.50000
H27C  2    0.653836    0.030267    0.761800    21.00000   -1.50000
AFIX   0
PART   2
C27B  1    0.787766   -0.010919    0.669936   -21.00000    0.25727    0.04281 =
         0.25848   -0.03065   -0.09147    0.04182
AFIX 137
H27D  2    0.828593   -0.005336    0.631366   -21.00000   -1.50000
H27E  2    0.704678   -0.023486    0.667436   -21.00000   -1.50000
H27F  2    0.842072   -0.058017    0.695687   -21.00000   -1.50000
AFIX   0
PART   1
C28A  1    0.852344    0.018058    0.649093    21.00000    0.15140    0.13024 =
         0.19656   -0.06554   -0.06892    0.06043
AFIX 137
H28A  2    0.898900    0.053786    0.622495    21.00000   -1.50000
H28B  2    0.796262   -0.002872    0.627130    21.00000   -1.50000
H28C  2    0.913262   -0.031223    0.670011    21.00000   -1.50000
AFIX   0
PART   2
C28B  1    0.901965    0.094427    0.683090   -21.00000    0.10418    0.13707 =
         0.22881    0.06760   -0.06880    0.00900
AFIX 137
H28D  2    0.899733    0.148785    0.696457   -21.00000   -1.50000
H28E  2    0.923844    0.099645    0.641653   -21.00000   -1.50000
H28F  2    0.966263    0.047673    0.704269   -21.00000   -1.50000
AFIX   0
PART   1
C29A  1    0.866529    0.096768    0.727416    21.00000    0.20485    0.09872 =
         0.19707   -0.02487   -0.14617    0.00531
AFIX 137
H29A  2    0.822917    0.137902    0.752778    21.00000   -1.50000
H29B  2    0.924326    0.122759    0.700327    21.00000   -1.50000
H29C  2    0.915657    0.044339    0.750788    21.00000   -1.50000
AFIX   0
PART   2
C29B  1    0.741142    0.082370    0.759019   -21.00000    0.19023    0.09268 =
         0.11061    0.03080   -0.05621    0.05005
AFIX 137
H29D  2    0.689396    0.042548    0.776483   -21.00000   -1.50000
H29E  2    0.694685    0.141665    0.762399   -21.00000   -1.50000
H29F  2    0.821921    0.068105    0.779078   -21.00000   -1.50000
AFIX   0
PART   0
C30   1    0.317976    0.840756    0.701183    11.00000    0.12838    0.09553 =
         0.14310   -0.06678   -0.03951    0.00707
PART   1
C31A  1    0.307257    0.927762    0.659808    31.00000    0.23742    0.07842 =
         0.22826   -0.07729   -0.00530   -0.06615
AFIX 137
H31A  2    0.300216    0.974145    0.682534    31.00000   -1.50000
H31B  2    0.231341    0.940166    0.636465    31.00000   -1.50000
H31C  2    0.383455    0.923855    0.634327    31.00000   -1.50000
AFIX   0
PART   2
C31B  1    0.216726    0.928097    0.686848   -31.00000    0.19244    0.14566 =
         0.26037   -0.14289   -0.10393    0.06829
AFIX 137
H31D  2    0.138061    0.925316    0.709579   -31.00000   -1.50000
H31E  2    0.198649    0.939101    0.645580   -31.00000   -1.50000
H31F  2    0.249765    0.974826    0.696367   -31.00000   -1.50000
AFIX   0
PART   1
C32A  1    0.420121    0.805630    0.746991    31.00000    0.18300    0.17366 =
         0.23921   -0.16908   -0.11439    0.03990
AFIX 137
H32A  2    0.434494    0.853463    0.763897    31.00000   -1.50000
H32B  2    0.499874    0.776326    0.728994    31.00000   -1.50000
H32C  2    0.391328    0.764633    0.777381    31.00000   -1.50000
AFIX   0
PART   2
C32B  1    0.448486    0.866368    0.687741   -31.00000    0.15407    0.08704 =
         0.22166   -0.05590   -0.07080   -0.02585
AFIX 137
H32D  2    0.449105    0.915024    0.707235   -31.00000   -1.50000
H32E  2    0.459370    0.883021    0.645936   -31.00000   -1.50000
H32F  2    0.518496    0.817056    0.701656   -31.00000   -1.50000
AFIX   0
PART   1
C33A  1    0.189310    0.857973    0.740201    31.00000    0.16876    0.12360 =
         0.12733   -0.09531   -0.01282    0.01486
AFIX 137
H33A  2    0.182590    0.804122    0.765022    31.00000   -1.50000
H33B  2    0.115606    0.878986    0.715154    31.00000   -1.50000
H33C  2    0.191095    0.901333    0.764275    31.00000   -1.50000
AFIX   0
PART   2
C33B  1    0.314519    0.797100    0.764592   -31.00000    0.28965    0.17526 =
         0.13888   -0.08649   -0.03272   -0.08624
AFIX 137
H33D  2    0.353426    0.735122    0.767222   -31.00000   -1.50000
H33E  2    0.225770    0.806006    0.779004   -31.00000   -1.50000
H33F  2    0.362160    0.822363    0.787945   -31.00000   -1.50000
AFIX   0
PART   0
C34   1    0.093021    0.759940    0.539373    11.00000    0.07146    0.11730 =
         0.07153   -0.02930   -0.01720    0.01700
C35   1    0.001089    0.846905    0.543259    11.00000    0.14042    0.14326 =
         0.17649   -0.08056   -0.08843    0.07875
AFIX 137
H35A  2   -0.039196    0.845955    0.581973    11.00000   -1.50000
H35B  2   -0.064745    0.858648    0.514405    11.00000   -1.50000
H35C  2    0.047936    0.892179    0.535903    11.00000   -1.50000
AFIX   0
C36   1    0.004555    0.692477    0.552849    11.00000    0.08026    0.21855 =
         0.12169   -0.02282   -0.02854   -0.01060
AFIX 137
H36A  2   -0.028305    0.690736    0.592874    11.00000   -1.50000
H36B  2    0.055107    0.634946    0.547339    11.00000   -1.50000
H36C  2   -0.067032    0.710650    0.526543    11.00000   -1.50000
AFIX   0
C37   1    0.146664    0.755118    0.477530    11.00000    0.10178    0.14880 =
         0.05822   -0.00589   -0.02004    0.01762
AFIX 137
H37A  2    0.077062    0.777572    0.450295    11.00000   -1.50000
H37B  2    0.187447    0.694956    0.473868    11.00000   -1.50000
H37C  2    0.209764    0.789746    0.468903    11.00000   -1.50000
AFIX   0
C38   1   -0.182348    0.656427    0.814058    11.00000    0.07329    0.35206 =
         0.08121    0.05283   -0.01842    0.00909
AFIX  43
H38   2   -0.247040    0.647513    0.842166    11.00000   -1.20000
AFIX   0
C39   1   -0.219727    0.701830    0.759261    11.00000    0.10825    0.49726 =
         0.09575    0.10354   -0.01393    0.02270
AFIX  43
H39   2   -0.307617    0.726635    0.752256    11.00000   -1.20000
AFIX   0
C40   1   -0.133428    0.710603    0.716890    11.00000    0.13353    0.31996 =
         0.05951    0.04975   -0.01699   -0.01341
AFIX  43
H40   2   -0.157845    0.739493    0.679219    11.00000   -1.20000
AFIX   0
C41   1   -0.008610    0.676288    0.730007    11.00000    0.10532    0.20081 =
         0.06436    0.02239    0.00107   -0.00869
AFIX  43
H41   2    0.056400    0.680799    0.701193    11.00000   -1.20000
AFIX   0
C42   1    0.023789    0.634139    0.786353    11.00000    0.07793    0.12873 =
         0.05167    0.00978    0.00280   -0.00548
PART 1
C43A  1    0.167588    0.622914    0.806570    61.00000    0.09208    0.09082 =
         0.05615   -0.00510    0.01607   -0.02669
AFIX  23
H43A  2    0.221676    0.635026    0.771924    61.00000   -1.20000
H43B  2    0.166318    0.666467    0.831554    61.00000   -1.20000
AFIX   0
PART 2
C43B  1    0.141235    0.549455    0.790477   -61.00000    0.06703    0.06504 =
         0.02627   -0.00759    0.01524   -0.02767
AFIX  23
H43C  2    0.106135    0.498007    0.794196   -61.00000   -1.20000
H43D  2    0.192069    0.552370    0.753788   -61.00000   -1.20000
AFIX   0
PART 0
C44   1    0.225887    0.537653    0.837835    11.00000    0.07200    0.09935 =
         0.05347   -0.00593    0.00436   -0.02323
AFIX  23
H44A  2    0.318954    0.532330    0.837910    11.00000   -1.20000
H44B  2    0.213193    0.494565    0.815099    11.00000   -1.20000
 
C45   1    0.218721    0.413857    0.913788    11.00000    0.06395    0.05784 =
         0.05992   -0.01109   -0.00116   -0.00737
AFIX  23
H45A  2    0.201160    0.397999    0.955632    11.00000   -1.20000
H45B  2    0.311752    0.392980    0.906774    11.00000   -1.20000
AFIX   0
C46   1    0.258619    0.541402    0.940087    11.00000    0.05072    0.05636 =
         0.05981   -0.00859   -0.00716   -0.00995
AFIX  23
H46A  2    0.350606    0.516871    0.932640    11.00000   -1.20000
H46B  2    0.237586    0.516585    0.980008    11.00000   -1.20000
AFIX   0
C47   1    0.237015    0.638404    0.937061    11.00000    0.04508    0.06479 =
         0.05254   -0.00185   -0.00361   -0.01933
C48   1    0.341624    0.675372    0.940003    11.00000    0.04788    0.06386 =
         0.07157   -0.00659   -0.00129   -0.01114
AFIX  43
H48   2    0.425611    0.639485    0.938835    11.00000   -1.20000
AFIX   0
C49   1    0.326257    0.763369    0.944601    11.00000    0.05212    0.07152 =
         0.07818   -0.00046   -0.00441   -0.02291
C50   1    0.199141    0.815869    0.943067    11.00000    0.05953    0.05006 =
         0.09699   -0.00379   -0.00763   -0.01638
AFIX  43
H50   2    0.186740    0.875409    0.944936    11.00000   -1.20000
AFIX   0
C51   1    0.089920    0.784369    0.938907    11.00000    0.05121    0.06014 =
         0.07112   -0.00611   -0.00300   -0.01716
C52   1    0.110666    0.694129    0.937236    11.00000    0.04743    0.06326 =
         0.05544   -0.00829   -0.00431   -0.01888
C53   1    0.149458    0.365953    0.880489    11.00000    0.08447    0.06025 =
         0.04461   -0.01466    0.00078   -0.01579
C54   1    0.222558    0.290959    0.859397    11.00000    0.09036    0.07265 =
         0.06329   -0.02170    0.00736   -0.02219
AFIX  43
H54   2    0.312857    0.276701    0.861433    11.00000   -1.20000
AFIX   0
C55   1    0.162099    0.236168    0.834977    11.00000    0.12556    0.07489 =
         0.06277   -0.02769    0.01194   -0.02942
C56   1    0.027148    0.262283    0.832300    11.00000    0.12315    0.08406 =
         0.06783   -0.02014   -0.00740   -0.04602
AFIX  43
H56   2   -0.014264    0.227165    0.816019    11.00000   -1.20000
AFIX   0
C57   1   -0.050734    0.336951    0.852116    11.00000    0.09741    0.08111 =
         0.05246   -0.02872    0.00273   -0.02919
C58   1    0.014229    0.389054    0.876946    11.00000    0.07790    0.07266 =
         0.04106   -0.01200    0.00378   -0.02622
C59   1    0.241634    0.150374    0.813579    11.00000    0.15233    0.08989 =
         0.12274   -0.05639    0.01332   -0.02173
PART   1
C60A  1    0.227952    0.161226    0.745635    41.00000    0.27020    0.11178 =
         0.10652   -0.06702    0.05299   -0.02295
AFIX 137
H60A  2    0.138227    0.169164    0.736851    41.00000   -1.50000
H60B  2    0.279531    0.109497    0.731414    41.00000   -1.50000
H60C  2    0.257661    0.211710    0.726744    41.00000   -1.50000
AFIX   0
C61A  1    0.180565    0.073121    0.841072    41.00000    0.19556    0.06052 =
         0.13432   -0.01644   -0.01306   -0.01593
AFIX 137
H61A  2    0.189775    0.062227    0.883074    41.00000   -1.50000
H61B  2    0.224329    0.021144    0.824976    41.00000   -1.50000
H61C  2    0.089808    0.088195    0.832177    41.00000   -1.50000
AFIX   0
C62A  1    0.385498    0.126805    0.829372    41.00000    0.13945    0.18027 =
         0.26906   -0.15334    0.03145    0.00077
AFIX 137
H62A  2    0.424390    0.173695    0.811526    41.00000   -1.50000
H62B  2    0.429968    0.073453    0.815044    41.00000   -1.50000
H62C  2    0.392292    0.118496    0.871443    41.00000   -1.50000
AFIX   0
PART   2
C60B  1    0.334294    0.181301    0.762682   -41.00000    0.14069    0.13755 =
         0.14110   -0.05049    0.04650    0.02840
AFIX 137
H60D  2    0.289751    0.236632    0.740811   -41.00000   -1.50000
H60E  2    0.358908    0.138090    0.736817   -41.00000   -1.50000
H60F  2    0.410878    0.188089    0.779296   -41.00000   -1.50000
AFIX   0
C61B  1    0.151507    0.096542    0.795024   -41.00000    0.23107    0.11126 =
         0.22713   -0.10123   -0.01695   -0.04247
AFIX 137
H61D  2    0.135301    0.113715    0.753644   -41.00000   -1.50000
H61E  2    0.070422    0.107916    0.817078   -41.00000   -1.50000
H61F  2    0.193277    0.034831    0.802922   -41.00000   -1.50000
AFIX   0
C62B  1    0.358850    0.115761    0.855738   -41.00000    0.10336    0.01335 =
         0.16387   -0.03111    0.04326    0.00955
AFIX 137
H62D  2    0.407665    0.058880    0.848050   -41.00000   -1.50000
H62E  2    0.326874    0.111078    0.895943   -41.00000   -1.50000
H62F  2    0.414139    0.156025    0.849165   -41.00000   -1.50000
AFIX   0
PART   0
C63   1   -0.199617    0.357450    0.850207    11.00000    0.10079    0.12896 =
         0.08798   -0.05471   -0.00774   -0.04594
C64   1   -0.262165    0.368829    0.909986    11.00000    0.11025    0.16360 =
         0.08964   -0.03904    0.01714   -0.07335
AFIX 137
H64A  2   -0.355084    0.387559    0.906601    11.00000   -1.50000
H64B  2   -0.231644    0.412406    0.925245    11.00000   -1.50000
H64C  2   -0.239699    0.313785    0.936273    11.00000   -1.50000
AFIX   0
C65   1   -0.253228    0.449686    0.810897    11.00000    0.13629    0.22693 =
         0.10356   -0.00614   -0.03641   -0.03424
AFIX 137
H65A  2   -0.216109    0.448687    0.771677    11.00000   -1.50000
H65B  2   -0.229842    0.494783    0.827598    11.00000   -1.50000
H65C  2   -0.346368    0.461736    0.809487    11.00000   -1.50000
AFIX   0
C66   1   -0.250724    0.297444    0.821500    11.00000    0.13134    0.24373 =
         0.22548   -0.15666   -0.01404   -0.06593
AFIX 137
H66A  2   -0.231429    0.239773    0.844795    11.00000   -1.50000
H66B  2   -0.210692    0.294380    0.782934    11.00000   -1.50000
H66C  2   -0.343356    0.319077    0.818064    11.00000   -1.50000
AFIX   0
C67   1    0.443439    0.800033    0.951984    11.00000    0.05052    0.07611 =
         0.11563   -0.00993   -0.01669   -0.02242
C68   1    0.531437    0.738254    0.998678    11.00000    0.10424    0.14873 =
         0.19533    0.02691   -0.07997   -0.06346
AFIX 137
H68A  2    0.484355    0.734341    1.035829    11.00000   -1.50000
H68B  2    0.606045    0.760536    1.002324    11.00000   -1.50000
H68C  2    0.559523    0.680842    0.987389    11.00000   -1.50000
AFIX   0
C69   1    0.403010    0.889127    0.967606    11.00000    0.09607    0.11087 =
         0.57103   -0.08368   -0.11728   -0.03181
AFIX 137
H69A  2    0.341697    0.926344    0.939640    11.00000   -1.50000
H69B  2    0.477917    0.912767    0.966969    11.00000   -1.50000
H69C  2    0.363033    0.886418    1.006404    11.00000   -1.50000
AFIX   0
C70   1    0.526208    0.797583    0.895411    11.00000    0.16893    0.46110 =
         0.15414   -0.04379    0.02554   -0.23793
AFIX 137
H70A  2    0.512644    0.752322    0.875567    11.00000   -1.50000
H70B  2    0.616478    0.785337    0.904662    11.00000   -1.50000
H70C  2    0.501823    0.853541    0.870243    11.00000   -1.50000
AFIX   0
C71   1   -0.048292    0.845113    0.937556    11.00000    0.05149    0.05266 =
         0.11050   -0.00518    0.00194   -0.01513
C72   1   -0.111741    0.845271    0.880109    11.00000    0.07871    0.11676 =
         0.13347    0.02737   -0.02553    0.00331
AFIX 137
H72A  2   -0.132467    0.789661    0.881056    11.00000   -1.50000
H72B  2   -0.052583    0.854578    0.847498    11.00000   -1.50000
H72C  2   -0.190105    0.891673    0.875618    11.00000   -1.50000
AFIX   0
C73   1   -0.046206    0.941003    0.938478    11.00000    0.06893    0.06659 =
         0.32188   -0.04198    0.00202   -0.00950
AFIX 137
H73A  2   -0.132556    0.978096    0.932758    11.00000   -1.50000
H73B  2    0.011128    0.959232    0.907429    11.00000   -1.50000
H73C  2   -0.015883    0.945700    0.975823    11.00000   -1.50000
AFIX   0
C74   1   -0.131050    0.813423    0.989396    11.00000    0.07541    0.10641 =
         0.11797   -0.02517    0.01367   -0.00673
AFIX 137
H74A  2   -0.214819    0.854371    0.989713    11.00000   -1.50000
H74B  2   -0.088554    0.809417    1.025574    11.00000   -1.50000
H74C  2   -0.141956    0.756499    0.985587    11.00000   -1.50000
 
HKLF  4
 
REM     v2o3 in P -1
REM R1 =  0.0771 for   6272 Fo > 4sig(Fo)  and  0.2302 for all  17675 data
REM    922 parameters refined using    356 restraints
 
END  
     
WGHT      0.1263      0.0000 
REM Highest difference peak  0.498,  deepest hole -0.461,  1-sigma level  0.140
Q1    1   0.6950  0.0307  0.7495  11.00000  0.05    0.50
Q2    1   0.2269  0.9610  0.7276  11.00000  0.05    0.48
Q3    1   0.4536  0.8516  0.7174  11.00000  0.05    0.46
Q4    1   0.4268  0.8758  0.7526  11.00000  0.05    0.46
Q5    1   0.4105  0.9020  0.9776  11.00000  0.05    0.46
Q6    1   0.1271  0.8967  0.5098  11.00000  0.05    0.44
Q7    1   0.3167  0.8701  0.7025  11.00000  0.05    0.44
Q8    1  -0.2079  0.2299  0.8730  11.00000  0.05    0.43
Q9    1   0.3611  0.8501  0.6936  11.00000  0.05    0.42
Q10   1   0.3969  0.9065  0.7211  11.00000  0.05    0.42
;

_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)+(0.1263P)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     SHELXL
_refine_ls_extinction_coef       0.0157(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         17675
_refine_ls_number_parameters     922
_refine_ls_number_restraints     356
_refine_ls_R_factor_all          0.2302
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2632
_refine_ls_wR_factor_gt          0.1833
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.941
_refine_ls_shift/su_max          0.002
_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 0.35892(7) 0.47832(5) 0.54141(3) 0.0574(3) Uani 1 1 d . . .
O1 O 0.4217(3) 0.35770(19) 0.55564(12) 0.0635(8) Uani 1 1 d . A .
N1 N 0.4720(3) 0.4687(2) 0.62967(14) 0.0539(9) Uani 1 1 d . A .
C1 C 0.0795(6) 0.4613(6) 0.5809(3) 0.141(3) Uani 1 1 d . . .
H1 H 0.0755 0.4811 0.5405 0.170 Uiso 1 1 calc R . .
V2 V -0.04087(7) 0.55875(5) 0.92735(3) 0.0518(3) Uani 1 1 d . . .
N2 N 0.1913(4) 0.4494(3) 0.60646(17) 0.0751(12) Uani 1 1 d . A .
C2 C -0.0330(7) 0.4456(6) 0.6111(3) 0.162(4) Uani 1 1 d . . .
H2 H -0.1091 0.4536 0.5909 0.194 Uiso 1 1 calc R . .
O2 O 0.2900(3) 0.5937(2) 0.55353(12) 0.0658(9) Uani 1 1 d . A .
O3 O 0.2647(3) 0.4808(2) 0.48919(12) 0.0652(9) Uani 1 1 d . . .
N3 N 0.1833(3) 0.5119(2) 0.89875(14) 0.0531(9) Uani 1 1 d . B .
C3 C -0.0302(7) 0.4192(6) 0.6688(3) 0.146(3) Uani 1 1 d . . .
H3 H -0.1047 0.4100 0.6900 0.175 Uiso 1 1 calc R . .
O4 O 0.5000 0.5000 0.5000 0.0556(11) Uani 1 2 d S . .
N4 N -0.0628(4) 0.6255(3) 0.82867(17) 0.0727(11) Uani 1 1 d . B .
C4 C 0.0840(7) 0.4058(5) 0.6966(3) 0.119(2) Uani 1 1 d . A .
H4 H 0.0886 0.3866 0.7371 0.143 Uiso 1 1 calc R . .
O5 O -0.0547(3) 0.4610(2) 0.89700(13) 0.0658(9) Uani 1 1 d . B .
C5 C 0.1929(5) 0.4209(4) 0.6643(2) 0.0841(16) Uani 1 1 d DU . .
O6 O 0.0080(3) 0.65912(17) 0.93594(12) 0.0530(7) Uani 1 1 d . B .
C6A C 0.3256(6) 0.3878(4) 0.6949(2) 0.0691(19) Uani 0.848(8) 1 d PDU A 1
H6A1 H 0.3097 0.3703 0.7367 0.083 Uiso 0.848(8) 1 calc PR A 1
H6A2 H 0.3748 0.3357 0.6794 0.083 Uiso 0.848(8) 1 calc PR A 1
C6B C 0.2658(17) 0.4763(18) 0.6937(11) 0.068(7) Uani 0.152(8) 1 d PDU A 2
H6B1 H 0.2351 0.5379 0.6767 0.082 Uiso 0.152(8) 1 calc PR A 2
H6B2 H 0.2420 0.4709 0.7354 0.082 Uiso 0.152(8) 1 calc PR A 2
C7 C 0.4056(5) 0.4521(3) 0.68767(19) 0.0704(13) Uani 1 1 d DU . .
H7A H 0.4716 0.4325 0.7174 0.084 Uiso 1 1 calc R A 1
H7B H 0.3503 0.5078 0.6959 0.084 Uiso 1 1 calc R A 1
O7 O -0.1947(3) 0.59865(19) 0.93471(12) 0.0599(8) Uani 1 1 d . . .
O8 O 0.0000 0.5000 1.0000 0.0530(10) Uani 1 2 d S . .
C8 C 0.5101(4) 0.5544(3) 0.6253(2) 0.0597(12) Uani 1 1 d . . .
H8A H 0.5594 0.5634 0.5886 0.072 Uiso 1 1 calc R A .
H8B H 0.5675 0.5496 0.6573 0.072 Uiso 1 1 calc R . .
C9 C 0.5963(4) 0.4008(3) 0.62611(18) 0.0577(12) Uani 1 1 d . . .
H9A H 0.6485 0.4010 0.6590 0.069 Uiso 1 1 calc R A .
H9B H 0.6431 0.4187 0.5903 0.069 Uiso 1 1 calc R . .
C10 C 0.5043(4) 0.2904(3) 0.58829(19) 0.0618(12) Uani 1 1 d . . .
C11 C 0.5005(5) 0.2030(3) 0.5855(2) 0.0700(14) Uani 1 1 d . A .
C12 C 0.5884(5) 0.1369(3) 0.6207(2) 0.0807(15) Uani 1 1 d . . .
H12 H 0.5888 0.0787 0.6193 0.097 Uiso 1 1 calc R A .
C13 C 0.6742(5) 0.1517(3) 0.6573(2) 0.0774(15) Uani 1 1 d . A .
C14 C 0.6706(4) 0.2382(3) 0.6599(2) 0.0670(13) Uani 1 1 d . . .
H14 H 0.7261 0.2500 0.6852 0.080 Uiso 1 1 calc R A .
C15 C 0.5882(4) 0.3079(3) 0.62649(19) 0.0583(12) Uani 1 1 d . A .
C16 C 0.2960(4) 0.6536(3) 0.58791(19) 0.0632(13) Uani 1 1 d . . .
C17 C 0.2017(5) 0.7337(3) 0.5839(2) 0.0719(14) Uani 1 1 d . A .
C18 C 0.2137(5) 0.7904(3) 0.6219(2) 0.0790(15) Uani 1 1 d . . .
H18 H 0.1514 0.8437 0.6198 0.095 Uiso 1 1 calc R A .
C19 C 0.3094(5) 0.7743(3) 0.6621(2) 0.0780(15) Uani 1 1 d . A .
C20 C 0.4030(5) 0.6931(3) 0.6644(2) 0.0680(13) Uani 1 1 d . . .
H20 H 0.4691 0.6790 0.6914 0.082 Uiso 1 1 calc R A .
C21 C 0.3988(4) 0.6342(3) 0.62740(18) 0.0577(12) Uani 1 1 d . A .
C22 C 0.4070(6) 0.1822(4) 0.5458(2) 0.0846(16) Uani 1 1 d . . .
C23 C 0.2683(7) 0.2158(5) 0.5683(3) 0.122(2) Uani 1 1 d . A .
H23A H 0.2604 0.1910 0.6091 0.183 Uiso 1 1 calc R . .
H23B H 0.2091 0.1987 0.5457 0.183 Uiso 1 1 calc R . .
H23C H 0.2479 0.2789 0.5644 0.183 Uiso 1 1 calc R . .
C24 C 0.4215(7) 0.2252(5) 0.4819(3) 0.125(2) Uani 1 1 d . A .
H24A H 0.4116 0.2873 0.4803 0.187 Uiso 1 1 calc R . .
H24B H 0.3557 0.2159 0.4588 0.187 Uiso 1 1 calc R . .
H24C H 0.5061 0.1994 0.4663 0.187 Uiso 1 1 calc R . .
C25 C 0.4258(8) 0.0830(4) 0.5480(4) 0.163(4) Uani 1 1 d . A .
H25A H 0.5087 0.0589 0.5301 0.244 Uiso 1 1 calc R . .
H25B H 0.3577 0.0727 0.5268 0.244 Uiso 1 1 calc R . .
H25C H 0.4225 0.0550 0.5883 0.244 Uiso 1 1 calc R . .
C26 C 0.7688(6) 0.0741(4) 0.6940(3) 0.1029(19) Uani 1 1 d DU . .
C27A C 0.6933(14) 0.0100(11) 0.7263(9) 0.175(8) Uani 0.567(15) 1 d PDU A 1
H27A H 0.7515 -0.0471 0.7360 0.263 Uiso 0.567(15) 1 calc PR A 1
H27B H 0.6267 0.0062 0.7014 0.263 Uiso 0.567(15) 1 calc PR A 1
H27C H 0.6538 0.0303 0.7618 0.263 Uiso 0.567(15) 1 calc PR A 1
C27B C 0.788(4) -0.0109(14) 0.6699(16) 0.196(14) Uani 0.433(15) 1 d PDU A 2
H27D H 0.8286 -0.0053 0.6314 0.293 Uiso 0.433(15) 1 calc PR A 2
H27E H 0.7047 -0.0235 0.6674 0.293 Uiso 0.433(15) 1 calc PR A 2
H27F H 0.8421 -0.0580 0.6957 0.293 Uiso 0.433(15) 1 calc PR A 2
C28A C 0.852(2) 0.0181(14) 0.6491(9) 0.169(9) Uani 0.567(15) 1 d PDU A 1
H28A H 0.8989 0.0538 0.6225 0.253 Uiso 0.567(15) 1 calc PR A 1
H28B H 0.7963 -0.0029 0.6271 0.253 Uiso 0.567(15) 1 calc PR A 1
H28C H 0.9133 -0.0312 0.6700 0.253 Uiso 0.567(15) 1 calc PR A 1
C28B C 0.9020(16) 0.0944(17) 0.6831(13) 0.172(11) Uani 0.433(15) 1 d PDU A 2
H28D H 0.8997 0.1488 0.6965 0.258 Uiso 0.433(15) 1 calc PR A 2
H28E H 0.9238 0.0996 0.6417 0.258 Uiso 0.433(15) 1 calc PR A 2
H28F H 0.9663 0.0477 0.7043 0.258 Uiso 0.433(15) 1 calc PR A 2
C29A C 0.867(2) 0.0968(13) 0.7274(9) 0.168(9) Uani 0.567(15) 1 d PDU A 1
H29A H 0.8229 0.1379 0.7528 0.251 Uiso 0.567(15) 1 calc PR A 1
H29B H 0.9243 0.1228 0.7003 0.251 Uiso 0.567(15) 1 calc PR A 1
H29C H 0.9157 0.0443 0.7508 0.251 Uiso 0.567(15) 1 calc PR A 1
C29B C 0.741(2) 0.0824(13) 0.7590(5) 0.150(10) Uani 0.433(15) 1 d PDU A 2
H29D H 0.6894 0.0425 0.7765 0.225 Uiso 0.433(15) 1 calc PR A 2
H29E H 0.6947 0.1417 0.7624 0.225 Uiso 0.433(15) 1 calc PR A 2
H29F H 0.8219 0.0681 0.7791 0.225 Uiso 0.433(15) 1 calc PR A 2
C30 C 0.3180(7) 0.8408(4) 0.7012(3) 0.121(2) Uani 1 1 d DU . .
C31A C 0.307(3) 0.9278(10) 0.6598(10) 0.170(9) Uani 0.442(13) 1 d PDU A 1
H31A H 0.3002 0.9741 0.6825 0.255 Uiso 0.442(13) 1 calc PR A 1
H31B H 0.2313 0.9402 0.6365 0.255 Uiso 0.442(13) 1 calc PR A 1
H31C H 0.3835 0.9239 0.6343 0.255 Uiso 0.442(13) 1 calc PR A 1
C31B C 0.217(2) 0.9281(11) 0.6868(11) 0.201(11) Uani 0.558(13) 1 d PDU A 2
H31D H 0.1381 0.9253 0.7096 0.302 Uiso 0.558(13) 1 calc PR A 2
H31E H 0.1986 0.9391 0.6456 0.302 Uiso 0.558(13) 1 calc PR A 2
H31F H 0.2498 0.9748 0.6964 0.302 Uiso 0.558(13) 1 calc PR A 2
C32A C 0.420(2) 0.8056(16) 0.7470(11) 0.192(12) Uani 0.442(13) 1 d PDU A 1
H32A H 0.4345 0.8535 0.7639 0.288 Uiso 0.442(13) 1 calc PR A 1
H32B H 0.4999 0.7763 0.7290 0.288 Uiso 0.442(13) 1 calc PR A 1
H32C H 0.3913 0.7646 0.7774 0.288 Uiso 0.442(13) 1 calc PR A 1
C32B C 0.4485(13) 0.8664(9) 0.6877(8) 0.148(6) Uani 0.558(13) 1 d PDU A 2
H32D H 0.4491 0.9150 0.7072 0.222 Uiso 0.558(13) 1 calc PR A 2
H32E H 0.4594 0.8830 0.6459 0.222 Uiso 0.558(13) 1 calc PR A 2
H32F H 0.5185 0.8171 0.7017 0.222 Uiso 0.558(13) 1 calc PR A 2
C33A C 0.1893(16) 0.8580(13) 0.7402(8) 0.140(7) Uani 0.442(13) 1 d PDU A 1
H33A H 0.1826 0.8041 0.7650 0.209 Uiso 0.442(13) 1 calc PR A 1
H33B H 0.1156 0.8790 0.7152 0.209 Uiso 0.442(13) 1 calc PR A 1
H33C H 0.1911 0.9013 0.7643 0.209 Uiso 0.442(13) 1 calc PR A 1
C33B C 0.315(3) 0.7971(14) 0.7646(6) 0.187(9) Uani 0.558(13) 1 d PDU A 2
H33D H 0.3534 0.7351 0.7672 0.281 Uiso 0.558(13) 1 calc PR A 2
H33E H 0.2258 0.8060 0.7790 0.281 Uiso 0.558(13) 1 calc PR A 2
H33F H 0.3622 0.8224 0.7879 0.281 Uiso 0.558(13) 1 calc PR A 2
C34 C 0.0930(6) 0.7599(4) 0.5394(2) 0.0916(19) Uani 1 1 d . . .
C35 C 0.0011(7) 0.8469(5) 0.5433(4) 0.163(4) Uani 1 1 d . A .
H35A H -0.0392 0.8460 0.5820 0.245 Uiso 1 1 calc R . .
H35B H -0.0647 0.8586 0.5144 0.245 Uiso 1 1 calc R . .
H35C H 0.0479 0.8922 0.5359 0.245 Uiso 1 1 calc R . .
C36 C 0.0046(7) 0.6925(6) 0.5528(3) 0.144(3) Uani 1 1 d . A .
H36A H -0.0283 0.6907 0.5929 0.216 Uiso 1 1 calc R . .
H36B H 0.0551 0.6349 0.5473 0.216 Uiso 1 1 calc R . .
H36C H -0.0670 0.7107 0.5265 0.216 Uiso 1 1 calc R . .
C37 C 0.1467(6) 0.7551(4) 0.4775(2) 0.112(2) Uani 1 1 d . A .
H37A H 0.0771 0.7776 0.4503 0.168 Uiso 1 1 calc R . .
H37B H 0.1874 0.6950 0.4739 0.168 Uiso 1 1 calc R . .
H37C H 0.2098 0.7897 0.4689 0.168 Uiso 1 1 calc R . .
C38 C -0.1823(7) 0.6564(7) 0.8141(3) 0.190(5) Uani 1 1 d . . .
H38 H -0.2470 0.6475 0.8422 0.228 Uiso 1 1 calc R . .
C39 C -0.2197(9) 0.7018(10) 0.7593(4) 0.269(8) Uani 1 1 d . . .
H39 H -0.3076 0.7266 0.7523 0.323 Uiso 1 1 calc R . .
C40 C -0.1334(9) 0.7106(7) 0.7169(3) 0.188(5) Uani 1 1 d . . .
H40 H -0.1578 0.7395 0.6792 0.225 Uiso 1 1 calc R . .
C41 C -0.0086(8) 0.6763(5) 0.7300(3) 0.134(3) Uani 1 1 d . B .
H41 H 0.0564 0.6808 0.7012 0.161 Uiso 1 1 calc R . .
C42 C 0.0238(6) 0.6341(4) 0.7864(2) 0.0929(18) Uani 1 1 d DU . .
C43A C 0.1676(7) 0.6229(5) 0.8066(3) 0.081(2) Uani 0.745(9) 1 d PDU B 1
H43A H 0.2217 0.6350 0.7719 0.097 Uiso 0.745(9) 1 calc PR B 1
H43B H 0.1663 0.6665 0.8316 0.097 Uiso 0.745(9) 1 calc PR B 1
C43B C 0.1412(13) 0.5495(10) 0.7905(6) 0.051(5) Uani 0.255(9) 1 d PDU B 2
H43C H 0.1061 0.4980 0.7942 0.062 Uiso 0.255(9) 1 calc PR B 2
H43D H 0.1921 0.5524 0.7538 0.062 Uiso 0.255(9) 1 calc PR B 2
C44 C 0.2259(3) 0.5377(2) 0.83784(14) 0.0756(14) Uani 1 1 d DU . .
H44A H 0.3190 0.5323 0.8379 0.091 Uiso 1 1 calc R B 1
H44B H 0.2132 0.4946 0.8151 0.091 Uiso 1 1 calc R B 1
C45 C 0.2187(3) 0.4139(2) 0.91379(14) 0.0618(12) Uani 1 1 d R . .
H45A H 0.2012 0.3980 0.9556 0.074 Uiso 1 1 calc R . .
H45B H 0.3118 0.3930 0.9068 0.074 Uiso 1 1 calc R . .
C46 C 0.2586(4) 0.5414(3) 0.9401(2) 0.0560(11) Uani 1 1 d . . .
H46A H 0.3506 0.5169 0.9326 0.067 Uiso 1 1 calc R B .
H46B H 0.2376 0.5166 0.9800 0.067 Uiso 1 1 calc R . .
C47 C 0.2370(4) 0.6384(3) 0.93706(18) 0.0539(11) Uani 1 1 d . B .
C48 C 0.3416(4) 0.6754(3) 0.9400(2) 0.0621(12) Uani 1 1 d . . .
H48 H 0.4256 0.6395 0.9388 0.075 Uiso 1 1 calc R B .
C49 C 0.3263(4) 0.7634(3) 0.9446(2) 0.0671(13) Uani 1 1 d . B .
C50 C 0.1991(5) 0.8159(3) 0.9431(2) 0.0690(14) Uani 1 1 d . . .
H50 H 0.1867 0.8754 0.9449 0.083 Uiso 1 1 calc R B .
C51 C 0.0899(4) 0.7844(3) 0.9389(2) 0.0606(12) Uani 1 1 d . B .
C52 C 0.1107(4) 0.6941(3) 0.93724(19) 0.0544(11) Uani 1 1 d . . .
C53 C 0.1495(5) 0.3660(3) 0.88049(19) 0.0628(13) Uani 1 1 d . B .
C54 C 0.2226(5) 0.2910(3) 0.8594(2) 0.0742(14) Uani 1 1 d . . .
H54 H 0.3129 0.2767 0.8614 0.089 Uiso 1 1 calc R B .
C55 C 0.1621(7) 0.2362(4) 0.8350(2) 0.0856(17) Uani 1 1 d . B .
C56 C 0.0271(7) 0.2623(4) 0.8323(2) 0.0867(17) Uani 1 1 d . . .
H56 H -0.0143 0.2272 0.8160 0.104 Uiso 1 1 calc R B .
C57 C -0.0507(6) 0.3370(4) 0.8521(2) 0.0737(14) Uani 1 1 d . B .
C58 C 0.0142(5) 0.3891(3) 0.87695(19) 0.0624(12) Uani 1 1 d . . .
C59 C 0.2416(8) 0.1504(4) 0.8136(3) 0.119(2) Uani 1 1 d DU . .
C60A C 0.2280(15) 0.1612(7) 0.7456(4) 0.164(5) Uani 0.832(13) 1 d PDU B 1
H60A H 0.1382 0.1692 0.7369 0.246 Uiso 0.832(13) 1 calc PR B 1
H60B H 0.2795 0.1095 0.7314 0.246 Uiso 0.832(13) 1 calc PR B 1
H60C H 0.2577 0.2117 0.7267 0.246 Uiso 0.832(13) 1 calc PR B 1
C61A C 0.1806(11) 0.0731(5) 0.8411(5) 0.132(4) Uani 0.832(13) 1 d PDU B 1
H61A H 0.1898 0.0622 0.8831 0.199 Uiso 0.832(13) 1 calc PR B 1
H61B H 0.2243 0.0211 0.8250 0.199 Uiso 0.832(13) 1 calc PR B 1
H61C H 0.0898 0.0882 0.8322 0.199 Uiso 0.832(13) 1 calc PR B 1
C62A C 0.3855(12) 0.1268(11) 0.8294(8) 0.191(8) Uani 0.832(13) 1 d PDU B 1
H62A H 0.4244 0.1737 0.8115 0.287 Uiso 0.832(13) 1 calc PR B 1
H62B H 0.4300 0.0735 0.8150 0.287 Uiso 0.832(13) 1 calc PR B 1
H62C H 0.3923 0.1185 0.8714 0.287 Uiso 0.832(13) 1 calc PR B 1
C60B C 0.334(5) 0.181(3) 0.763(2) 0.150(16) Uani 0.168(13) 1 d PDU B 2
H60D H 0.2898 0.2366 0.7408 0.225 Uiso 0.168(13) 1 calc PR B 2
H60E H 0.3589 0.1381 0.7368 0.225 Uiso 0.168(13) 1 calc PR B 2
H60F H 0.4109 0.1881 0.7793 0.225 Uiso 0.168(13) 1 calc PR B 2
C61B C 0.152(5) 0.097(3) 0.7950(9) 0.180(18) Uani 0.168(13) 1 d PDU B 2
H61D H 0.1353 0.1137 0.7536 0.270 Uiso 0.168(13) 1 calc PR B 2
H61E H 0.0704 0.1079 0.8171 0.270 Uiso 0.168(13) 1 calc PR B 2
H61F H 0.1933 0.0348 0.8029 0.270 Uiso 0.168(13) 1 calc PR B 2
C62B C 0.359(4) 0.116(3) 0.856(2) 0.098(12) Uani 0.168(13) 1 d PDU B 2
H62D H 0.4077 0.0589 0.8480 0.147 Uiso 0.168(13) 1 calc PR B 2
H62E H 0.3269 0.1111 0.8959 0.147 Uiso 0.168(13) 1 calc PR B 2
H62F H 0.4141 0.1560 0.8492 0.147 Uiso 0.168(13) 1 calc PR B 2
C63 C -0.1996(6) 0.3575(5) 0.8502(3) 0.0979(19) Uani 1 1 d . . .
C64 C -0.2622(6) 0.3688(5) 0.9100(3) 0.113(2) Uani 1 1 d . B .
H64A H -0.3551 0.3876 0.9066 0.169 Uiso 1 1 calc R . .
H64B H -0.2316 0.4124 0.9252 0.169 Uiso 1 1 calc R . .
H64C H -0.2397 0.3138 0.9363 0.169 Uiso 1 1 calc R . .
C65 C -0.2532(8) 0.4497(6) 0.8109(3) 0.158(3) Uani 1 1 d . B .
H65A H -0.2161 0.4487 0.7717 0.237 Uiso 1 1 calc R . .
H65B H -0.2298 0.4948 0.8276 0.237 Uiso 1 1 calc R . .
H65C H -0.3464 0.4617 0.8095 0.237 Uiso 1 1 calc R . .
C66 C -0.2507(8) 0.2974(6) 0.8215(4) 0.182(4) Uani 1 1 d . B .
H66A H -0.2314 0.2398 0.8448 0.272 Uiso 1 1 calc R . .
H66B H -0.2107 0.2944 0.7829 0.272 Uiso 1 1 calc R . .
H66C H -0.3434 0.3191 0.8181 0.272 Uiso 1 1 calc R . .
C67 C 0.4434(5) 0.8000(3) 0.9520(3) 0.0794(16) Uani 1 1 d . . .
C68 C 0.5314(7) 0.7383(5) 0.9987(4) 0.146(3) Uani 1 1 d . B .
H68A H 0.4844 0.7343 1.0358 0.220 Uiso 1 1 calc R . .
H68B H 0.6060 0.7605 1.0023 0.220 Uiso 1 1 calc R . .
H68C H 0.5595 0.6808 0.9874 0.220 Uiso 1 1 calc R . .
C69 C 0.4030(7) 0.8891(5) 0.9676(6) 0.249(7) Uani 1 1 d . B .
H69A H 0.3417 0.9263 0.9396 0.374 Uiso 1 1 calc R . .
H69B H 0.4779 0.9128 0.9670 0.374 Uiso 1 1 calc R . .
H69C H 0.3630 0.8864 1.0064 0.374 Uiso 1 1 calc R . .
C70 C 0.5262(9) 0.7976(8) 0.8954(4) 0.234(6) Uani 1 1 d . B .
H70A H 0.5126 0.7523 0.8756 0.351 Uiso 1 1 calc R . .
H70B H 0.6165 0.7853 0.9047 0.351 Uiso 1 1 calc R . .
H70C H 0.5018 0.8535 0.8702 0.351 Uiso 1 1 calc R . .
C71 C -0.0483(5) 0.8451(3) 0.9376(3) 0.0723(14) Uani 1 1 d . . .
C72 C -0.1117(6) 0.8453(4) 0.8801(3) 0.119(2) Uani 1 1 d . B .
H72A H -0.1325 0.7897 0.8811 0.179 Uiso 1 1 calc R . .
H72B H -0.0526 0.8546 0.8475 0.179 Uiso 1 1 calc R . .
H72C H -0.1901 0.8917 0.8756 0.179 Uiso 1 1 calc R . .
C73 C -0.0462(6) 0.9410(4) 0.9385(4) 0.153(4) Uani 1 1 d . B .
H73A H -0.1326 0.9781 0.9328 0.229 Uiso 1 1 calc R . .
H73B H 0.0111 0.9592 0.9074 0.229 Uiso 1 1 calc R . .
H73C H -0.0159 0.9457 0.9758 0.229 Uiso 1 1 calc R . .
C74 C -0.1311(6) 0.8134(4) 0.9894(3) 0.1027(19) Uani 1 1 d . B .
H74A H -0.2148 0.8544 0.9897 0.154 Uiso 1 1 calc R . .
H74B H -0.0886 0.8094 1.0256 0.154 Uiso 1 1 calc R . .
H74C H -0.1420 0.7565 0.9856 0.154 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 O3 1.606(3) . ?
V1 O4 1.7932(8) . ?
V1 O1 1.843(3) . ?
V1 O2 1.856(3) . ?
V1 N2 2.328(4) . ?
V1 N1 2.395(3) . ?
O1 C10 1.349(5) . ?
N1 C7 1.479(5) . ?
N1 C9 1.486(5) . ?
N1 C8 1.501(5) . ?
C1 N2 1.318(7) . ?
C1 C2 1.395(9) . ?
C1 H1 0.9300 . ?
V2 O7 1.603(3) . ?
V2 O8 1.7941(7) . ?
V2 O6 1.843(3) . ?
V2 O5 1.851(3) . ?
V2 N4 2.337(4) . ?
V2 N3 2.386(3) . ?
N2 C5 1.330(6) . ?
C2 C3 1.324(9) . ?
C2 H2 0.9300 . ?
O2 C16 1.353(5) . ?
N3 C44 1.464(4) . ?
N3 C46 1.489(5) . ?
N3 C45 1.492(5) . ?
C3 C4 1.362(8) . ?
C3 H3 0.9300 . ?
O4 V1 1.7932(8) 2_666 ?
N4 C38 1.286(7) . ?
N4 C42 1.305(6) . ?
C4 C5 1.380(8) . ?
C4 H4 0.9300 . ?
O5 C58 1.329(5) . ?
C5 C6A 1.548(7) . ?
C5 C6B 1.568(18) . ?
O6 C52 1.347(5) . ?
C6A C7 1.469(7) . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
C6B C7 1.439(17) . ?
C6B H6B1 0.9700 . ?
C6B H6B2 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O8 V2 1.7941(7) 2_567 ?
C8 C21 1.504(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C15 1.499(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.403(6) . ?
C10 C11 1.413(6) . ?
C11 C12 1.397(7) . ?
C11 C22 1.525(7) . ?
C12 C13 1.371(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(6) . ?
C13 C26 1.542(7) . ?
C14 C15 1.377(6) . ?
C14 H14 0.9300 . ?
C16 C17 1.400(6) . ?
C16 C21 1.409(6) . ?
C17 C18 1.391(7) . ?
C17 C34 1.528(7) . ?
C18 C19 1.369(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.410(7) . ?
C19 C30 1.523(8) . ?
C20 C21 1.380(6) . ?
C20 H20 0.9300 . ?
C22 C23 1.520(8) . ?
C22 C24 1.526(8) . ?
C22 C25 1.532(8) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C29A 1.481(11) . ?
C26 C27B 1.509(13) . ?
C26 C27A 1.518(11) . ?
C26 C28B 1.522(13) . ?
C26 C29B 1.526(12) . ?
C26 C28A 1.560(12) . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C27B H27D 0.9600 . ?
C27B H27E 0.9600 . ?
C27B H27F 0.9600 . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C28B H28D 0.9600 . ?
C28B H28E 0.9600 . ?
C28B H28F 0.9600 . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C29B H29D 0.9600 . ?
C29B H29E 0.9600 . ?
C29B H29F 0.9600 . ?
C30 C32A 1.501(13) . ?
C30 C33B 1.507(12) . ?
C30 C31A 1.522(13) . ?
C30 C31B 1.526(11) . ?
C30 C32B 1.537(11) . ?
C30 C33A 1.571(12) . ?
C31A H31A 0.9600 . ?
C31A H31B 0.9600 . ?
C31A H31C 0.9600 . ?
C31B H31D 0.9600 . ?
C31B H31E 0.9600 . ?
C31B H31F 0.9600 . ?
C32A H32A 0.9600 . ?
C32A H32B 0.9600 . ?
C32A H32C 0.9600 . ?
C32B H32D 0.9600 . ?
C32B H32E 0.9600 . ?
C32B H32F 0.9600 . ?
C33A H33A 0.9600 . ?
C33A H33B 0.9600 . ?
C33A H33C 0.9600 . ?
C33B H33D 0.9600 . ?
C33B H33E 0.9600 . ?
C33B H33F 0.9600 . ?
C34 C35 1.489(7) . ?
C34 C37 1.502(7) . ?
C34 C36 1.576(9) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C39 1.372(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.304(11) . ?
C39 H39 0.9300 . ?
C40 C41 1.333(10) . ?
C40 H40 0.9300 . ?
C41 C42 1.378(8) . ?
C41 H41 0.9300 . ?
C42 C43B 1.580(14) . ?
C42 C43A 1.585(9) . ?
C43A C44 1.429(7) . ?
C43A H43A 0.9700 . ?
C43A H43B 0.9700 . ?
C43B C44 1.419(13) . ?
C43B H43C 0.9700 . ?
C43B H43D 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C53 1.507(6) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.490(6) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.392(6) . ?
C47 C52 1.408(6) . ?
C48 C49 1.388(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.394(6) . ?
C49 C67 1.532(7) . ?
C50 C51 1.389(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.402(6) . ?
C51 C71 1.537(6) . ?
C53 C54 1.391(6) . ?
C53 C58 1.393(7) . ?
C54 C55 1.410(7) . ?
C54 H54 0.9300 . ?
C55 C56 1.389(8) . ?
C55 C59 1.550(8) . ?
C56 C57 1.391(7) . ?
C56 H56 0.9300 . ?
C57 C58 1.413(7) . ?
C57 C63 1.533(8) . ?
C59 C62A 1.532(11) . ?
C59 C61A 1.552(9) . ?
C59 C60A 1.557(9) . ?
C59 C61B 1.558(16) . ?
C59 C62B 1.560(16) . ?
C59 C60B 1.570(16) . ?
C60A H60A 0.9600 . ?
C60A H60B 0.9600 . ?
C60A H60C 0.9600 . ?
C61A H61A 0.9600 . ?
C61A H61B 0.9600 . ?
C61A H61C 0.9600 . ?
C62A H62A 0.9600 . ?
C62A H62B 0.9600 . ?
C62A H62C 0.9600 . ?
C60B H60D 0.9600 . ?
C60B H60E 0.9600 . ?
C60B H60F 0.9600 . ?
C61B H61D 0.9600 . ?
C61B H61E 0.9600 . ?
C61B H61F 0.9600 . ?
C62B H62D 0.9600 . ?
C62B H62E 0.9600 . ?
C62B H62F 0.9600 . ?
C63 C66 1.473(8) . ?
C63 C64 1.504(8) . ?
C63 C65 1.577(9) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 C69 1.471(9) . ?
C67 C70 1.519(10) . ?
C67 C68 1.519(8) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 C74 1.523(7) . ?
C71 C72 1.525(8) . ?
C71 C73 1.534(7) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 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
O3 V1 O4 100.97(12) . . ?
O3 V1 O1 96.34(14) . . ?
O4 V1 O1 95.59(10) . . ?
O3 V1 O2 96.48(14) . . ?
O4 V1 O2 95.19(11) . . ?
O1 V1 O2 161.36(13) . . ?
O3 V1 N2 86.78(15) . . ?
O4 V1 N2 172.26(10) . . ?
O1 V1 N2 83.52(14) . . ?
O2 V1 N2 83.75(15) . . ?
O3 V1 N1 170.83(15) . . ?
O4 V1 N1 88.19(9) . . ?
O1 V1 N1 82.24(12) . . ?
O2 V1 N1 82.94(12) . . ?
N2 V1 N1 84.06(13) . . ?
C10 O1 V1 144.5(3) . . ?
C7 N1 C9 110.3(3) . . ?
C7 N1 C8 108.1(3) . . ?
C9 N1 C8 105.4(3) . . ?
C7 N1 V1 119.4(3) . . ?
C9 N1 V1 106.5(2) . . ?
C8 N1 V1 106.1(2) . . ?
N2 C1 C2 123.6(6) . . ?
N2 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
O7 V2 O8 101.94(11) . . ?
O7 V2 O6 96.37(13) . . ?
O8 V2 O6 96.73(9) . . ?
O7 V2 O5 95.53(14) . . ?
O8 V2 O5 95.01(10) . . ?
O6 V2 O5 161.18(13) . . ?
O7 V2 N4 86.39(15) . . ?
O8 V2 N4 171.58(11) . . ?
O6 V2 N4 83.38(14) . . ?
O5 V2 N4 82.87(14) . . ?
O7 V2 N3 169.87(13) . . ?
O8 V2 N3 88.18(8) . . ?
O6 V2 N3 82.35(12) . . ?
O5 V2 N3 83.37(13) . . ?
N4 V2 N3 83.49(13) . . ?
C1 N2 C5 116.3(5) . . ?
C1 N2 V1 113.8(4) . . ?
C5 N2 V1 129.9(4) . . ?
C3 C2 C1 119.1(7) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C16 O2 V1 143.8(3) . . ?
C44 N3 C46 109.8(3) . . ?
C44 N3 C45 109.2(3) . . ?
C46 N3 C45 104.4(3) . . ?
C44 N3 V2 119.7(2) . . ?
C46 N3 V2 106.5(2) . . ?
C45 N3 V2 106.1(2) . . ?
C2 C3 C4 118.7(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
V1 O4 V1 180.00(4) . 2_666 ?
C38 N4 C42 115.6(5) . . ?
C38 N4 V2 112.9(4) . . ?
C42 N4 V2 131.5(3) . . ?
C3 C4 C5 119.6(6) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C58 O5 V2 143.4(3) . . ?
N2 C5 C4 122.6(5) . . ?
N2 C5 C6A 118.9(5) . . ?
C4 C5 C6A 117.6(5) . . ?
N2 C5 C6B 108.3(11) . . ?
C4 C5 C6B 112.8(9) . . ?
C6A C5 C6B 52.8(10) . . ?
C52 O6 V2 144.3(3) . . ?
C7 C6A C5 114.9(5) . . ?
C7 C6A H6A1 108.5 . . ?
C5 C6A H6A1 108.5 . . ?
C7 C6A H6A2 108.5 . . ?
C5 C6A H6A2 108.5 . . ?
H6A1 C6A H6A2 107.5 . . ?
C7 C6B C5 115.5(14) . . ?
C7 C6B H6B1 108.4 . . ?
C5 C6B H6B1 108.4 . . ?
C7 C6B H6B2 108.4 . . ?
C5 C6B H6B2 108.4 . . ?
H6B1 C6B H6B2 107.5 . . ?
C6B C7 C6A 56.9(11) . . ?
C6B C7 N1 120.9(11) . . ?
C6A C7 N1 117.4(4) . . ?
C6B C7 H7A 130.5 . . ?
C6A C7 H7A 108.0 . . ?
N1 C7 H7A 108.0 . . ?
C6B C7 H7B 52.2 . . ?
C6A C7 H7B 108.0 . . ?
N1 C7 H7B 108.0 . . ?
H7A C7 H7B 107.2 . . ?
V2 O8 V2 180.00(2) 2_567 . ?
N1 C8 C21 115.3(4) . . ?
N1 C8 H8A 108.4 . . ?
C21 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C21 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
N1 C9 C15 117.5(4) . . ?
N1 C9 H9A 107.9 . . ?
C15 C9 H9A 107.9 . . ?
N1 C9 H9B 107.9 . . ?
C15 C9 H9B 107.9 . . ?
H9A C9 H9B 107.2 . . ?
O1 C10 C15 119.8(4) . . ?
O1 C10 C11 119.3(4) . . ?
C15 C10 C11 120.9(4) . . ?
C12 C11 C10 115.9(4) . . ?
C12 C11 C22 122.2(5) . . ?
C10 C11 C22 121.9(4) . . ?
C13 C12 C11 124.7(5) . . ?
C13 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
C12 C13 C14 116.9(5) . . ?
C12 C13 C26 120.8(5) . . ?
C14 C13 C26 122.3(5) . . ?
C15 C14 C13 122.8(4) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
C14 C15 C10 118.8(4) . . ?
C14 C15 C9 121.1(4) . . ?
C10 C15 C9 119.9(4) . . ?
O2 C16 C17 120.3(4) . . ?
O2 C16 C21 119.1(4) . . ?
C17 C16 C21 120.6(4) . . ?
C18 C17 C16 116.4(4) . . ?
C18 C17 C34 121.0(4) . . ?
C16 C17 C34 122.6(4) . . ?
C19 C18 C17 125.6(5) . . ?
C19 C18 H18 117.2 . . ?
C17 C18 H18 117.2 . . ?
C18 C19 C20 116.2(4) . . ?
C18 C19 C30 122.5(5) . . ?
C20 C19 C30 121.3(5) . . ?
C21 C20 C19 121.5(5) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C16 119.6(4) . . ?
C20 C21 C8 119.9(4) . . ?
C16 C21 C8 120.3(4) . . ?
C23 C22 C11 108.8(4) . . ?
C23 C22 C24 109.4(5) . . ?
C11 C22 C24 111.5(5) . . ?
C23 C22 C25 105.6(6) . . ?
C11 C22 C25 112.3(5) . . ?
C24 C22 C25 109.1(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29A C26 C27B 125.1(17) . . ?
C29A C26 C27A 117.8(11) . . ?
C27B C26 C27A 64.3(13) . . ?
C29A C26 C28B 41.5(12) . . ?
C27B C26 C28B 102.9(17) . . ?
C27A C26 C28B 145.6(10) . . ?
C29A C26 C29B 60.7(11) . . ?
C27B C26 C29B 123.9(16) . . ?
C27A C26 C29B 66.7(11) . . ?
C28B C26 C29B 102.3(14) . . ?
C29A C26 C13 116.5(9) . . ?
C27B C26 C13 112.4(15) . . ?
C27A C26 C13 109.2(7) . . ?
C28B C26 C13 105.2(9) . . ?
C29B C26 C13 107.9(7) . . ?
C29A C26 C28A 104.0(13) . . ?
C27B C26 C28A 37.0(16) . . ?
C27A C26 C28A 100.8(12) . . ?
C28B C26 C28A 69.3(14) . . ?
C29B C26 C28A 145.6(11) . . ?
C13 C26 C28A 106.4(10) . . ?
C26 C27A H27A 109.5 . . ?
C26 C27A H27B 109.5 . . ?
C26 C27A H27C 109.5 . . ?
C26 C27B H27D 109.5 . . ?
C26 C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C26 C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C26 C28A H28A 109.5 . . ?
C26 C28A H28B 109.5 . . ?
C26 C28A H28C 109.5 . . ?
C26 C28B H28D 109.5 . . ?
C26 C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C26 C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C26 C29A H29A 109.5 . . ?
C26 C29A H29B 109.5 . . ?
C26 C29A H29C 109.5 . . ?
C26 C29B H29D 109.5 . . ?
C26 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C26 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C32A C30 C33B 46.9(12) . . ?
C32A C30 C31A 123.0(16) . . ?
C33B C30 C31A 145.4(12) . . ?
C32A C30 C19 113.6(9) . . ?
C33B C30 C19 108.2(9) . . ?
C31A C30 C19 105.6(10) . . ?
C32A C30 C31B 133.6(12) . . ?
C33B C30 C31B 114.5(13) . . ?
C31A C30 C31B 42.6(11) . . ?
C19 C30 C31B 112.8(9) . . ?
C32A C30 C32B 63.0(13) . . ?
C33B C30 C32B 108.9(11) . . ?
C31A C30 C32B 66.2(11) . . ?
C19 C30 C32B 108.7(7) . . ?
C31B C30 C32B 103.6(12) . . ?
C32A C30 C33A 101.9(14) . . ?
C33B C30 C33A 58.8(11) . . ?
C31A C30 C33A 103.4(12) . . ?
C19 C30 C33A 107.9(8) . . ?
C31B C30 C33A 61.1(11) . . ?
C32B C30 C33A 143.3(9) . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31B 109.5 . . ?
C30 C31A H31C 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C32A H32B 109.5 . . ?
C30 C32A H32C 109.5 . . ?
C30 C32B H32D 109.5 . . ?
C30 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C30 C33A H33A 109.5 . . ?
C30 C33A H33B 109.5 . . ?
C30 C33A H33C 109.5 . . ?
C30 C33B H33D 109.5 . . ?
C30 C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C30 C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C35 C34 C37 111.1(6) . . ?
C35 C34 C17 114.1(5) . . ?
C37 C34 C17 111.5(5) . . ?
C35 C34 C36 104.1(6) . . ?
C37 C34 C36 106.3(5) . . ?
C17 C34 C36 109.1(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N4 C38 C39 123.6(8) . . ?
N4 C38 H38 118.2 . . ?
C39 C38 H38 118.2 . . ?
C40 C39 C38 120.8(8) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C39 C40 C41 117.0(7) . . ?
C39 C40 H40 121.5 . . ?
C41 C40 H40 121.5 . . ?
C40 C41 C42 119.8(7) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
N4 C42 C41 123.0(6) . . ?
N4 C42 C43B 111.2(7) . . ?
C41 C42 C43B 115.3(7) . . ?
N4 C42 C43A 115.8(5) . . ?
C41 C42 C43A 118.2(6) . . ?
C43B C42 C43A 51.7(6) . . ?
C44 C43A C42 114.4(5) . . ?
C44 C43A H43A 108.6 . . ?
C42 C43A H43A 108.6 . . ?
C44 C43A H43B 108.6 . . ?
C42 C43A H43B 108.6 . . ?
H43A C43A H43B 107.6 . . ?
C44 C43B C42 115.3(9) . . ?
C44 C43B H43C 108.5 . . ?
C42 C43B H43C 108.5 . . ?
C44 C43B H43D 108.5 . . ?
C42 C43B H43D 108.5 . . ?
H43C C43B H43D 107.5 . . ?
C43B C44 C43A 58.0(7) . . ?
C43B C44 N3 120.7(7) . . ?
C43A C44 N3 119.7(4) . . ?
C43B C44 H44A 130.8 . . ?
C43A C44 H44A 107.4 . . ?
N3 C44 H44A 107.4 . . ?
C43B C44 H44B 50.9 . . ?
C43A C44 H44B 107.4 . . ?
N3 C44 H44B 107.4 . . ?
H44A C44 H44B 106.9 . . ?
N3 C45 C53 115.9(3) . . ?
N3 C45 H45A 108.3 . . ?
C53 C45 H45A 108.3 . . ?
N3 C45 H45B 108.3 . . ?
C53 C45 H45B 108.3 . . ?
H45A C45 H45B 107.4 . . ?
N3 C46 C47 116.4(3) . . ?
N3 C46 H46A 108.2 . . ?
C47 C46 H46A 108.2 . . ?
N3 C46 H46B 108.2 . . ?
C47 C46 H46B 108.2 . . ?
H46A C46 H46B 107.4 . . ?
C48 C47 C52 117.8(4) . . ?
C48 C47 C46 120.4(4) . . ?
C52 C47 C46 121.4(4) . . ?
C49 C48 C47 123.0(4) . . ?
C49 C48 H48 118.5 . . ?
C47 C48 H48 118.5 . . ?
C48 C49 C50 116.6(4) . . ?
C48 C49 C67 121.3(4) . . ?
C50 C49 C67 122.0(5) . . ?
C51 C50 C49 123.8(4) . . ?
C51 C50 H50 118.1 . . ?
C49 C50 H50 118.1 . . ?
C50 C51 C52 117.2(4) . . ?
C50 C51 C71 121.7(4) . . ?
C52 C51 C71 121.1(4) . . ?
O6 C52 C51 119.8(4) . . ?
O6 C52 C47 118.7(4) . . ?
C51 C52 C47 121.5(4) . . ?
C54 C53 C58 120.2(5) . . ?
C54 C53 C45 118.0(4) . . ?
C58 C53 C45 121.3(4) . . ?
C53 C54 C55 121.1(5) . . ?
C53 C54 H54 119.4 . . ?
C55 C54 H54 119.4 . . ?
C56 C55 C54 116.4(5) . . ?
C56 C55 C59 121.8(6) . . ?
C54 C55 C59 121.8(6) . . ?
C55 C56 C57 125.0(5) . . ?
C55 C56 H56 117.5 . . ?
C57 C56 H56 117.5 . . ?
C56 C57 C58 116.5(5) . . ?
C56 C57 C63 121.0(5) . . ?
C58 C57 C63 122.4(5) . . ?
O5 C58 C53 119.8(4) . . ?
O5 C58 C57 119.5(5) . . ?
C53 C58 C57 120.8(5) . . ?
C62A C59 C55 113.0(7) . . ?
C62A C59 C61A 109.1(9) . . ?
C55 C59 C61A 109.3(6) . . ?
C62A C59 C60A 110.5(9) . . ?
C55 C59 C60A 108.4(6) . . ?
C61A C59 C60A 106.3(7) . . ?
C62A C59 C61B 133(2) . . ?
C55 C59 C61B 112(2) . . ?
C61A C59 C61B 41.4(3) . . ?
C60A C59 C61B 66.3(10) . . ?
C62A C59 C62B 25(2) . . ?
C55 C59 C62B 104.6(17) . . ?
C61A C59 C62B 91.6(19) . . ?
C60A C59 C62B 134(2) . . ?
C61B C59 C62B 127(2) . . ?
C62A C59 C60B 66(2) . . ?
C55 C59 C60B 105.0(18) . . ?
C61A C59 C60B 144(2) . . ?
C60A C59 C60B 51(3) . . ?
C61B C59 C60B 114(3) . . ?
C62B C59 C60B 90(3) . . ?
C59 C60A H60A 109.5 . . ?
C59 C60A H60B 109.5 . . ?
C59 C60A H60C 109.5 . . ?
C59 C61A H61A 109.5 . . ?
C59 C61A H61B 109.5 . . ?
C59 C61A H61C 109.5 . . ?
C59 C62A H62A 109.5 . . ?
C59 C62A H62B 109.5 . . ?
C59 C62A H62C 109.5 . . ?
C59 C60B H60D 109.5 . . ?
C59 C60B H60E 109.5 . . ?
H60D C60B H60E 109.5 . . ?
C59 C60B H60F 109.5 . . ?
H60D C60B H60F 109.5 . . ?
H60E C60B H60F 109.5 . . ?
C59 C61B H61D 109.5 . . ?
C59 C61B H61E 109.5 . . ?
H61D C61B H61E 109.5 . . ?
C59 C61B H61F 109.5 . . ?
H61D C61B H61F 109.5 . . ?
H61E C61B H61F 109.5 . . ?
C59 C62B H62D 109.5 . . ?
C59 C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
C59 C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
C66 C63 C64 112.7(6) . . ?
C66 C63 C57 115.1(6) . . ?
C64 C63 C57 111.5(5) . . ?
C66 C63 C65 102.7(7) . . ?
C64 C63 C65 103.9(6) . . ?
C57 C63 C65 109.9(6) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C69 C67 C70 112.0(7) . . ?
C69 C67 C68 110.2(6) . . ?
C70 C67 C68 104.5(6) . . ?
C69 C67 C49 111.9(5) . . ?
C70 C67 C49 108.3(5) . . ?
C68 C67 C49 109.7(5) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C74 C71 C72 109.1(5) . . ?
C74 C71 C73 109.9(5) . . ?
C72 C71 C73 106.1(5) . . ?
C74 C71 C51 110.4(4) . . ?
C72 C71 C51 109.6(4) . . ?
C73 C71 C51 111.7(4) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 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
O3 V1 O1 C10 178.1(5) . . . . ?
O4 V1 O1 C10 76.4(5) . . . . ?
O2 V1 O1 C10 -48.7(8) . . . . ?
N2 V1 O1 C10 -95.9(5) . . . . ?
N1 V1 O1 C10 -11.0(5) . . . . ?
O3 V1 N1 C7 -3.8(10) . . . . ?
O4 V1 N1 C7 178.6(3) . . . . ?
O1 V1 N1 C7 -85.5(3) . . . . ?
O2 V1 N1 C7 83.2(3) . . . . ?
N2 V1 N1 C7 -1.3(3) . . . . ?
O3 V1 N1 C9 121.9(9) . . . . ?
O4 V1 N1 C9 -55.7(3) . . . . ?
O1 V1 N1 C9 40.2(3) . . . . ?
O2 V1 N1 C9 -151.2(3) . . . . ?
N2 V1 N1 C9 124.4(3) . . . . ?
O3 V1 N1 C8 -126.1(9) . . . . ?
O4 V1 N1 C8 56.3(2) . . . . ?
O1 V1 N1 C8 152.2(3) . . . . ?
O2 V1 N1 C8 -39.1(3) . . . . ?
N2 V1 N1 C8 -123.6(3) . . . . ?
C2 C1 N2 C5 0.0(12) . . . . ?
C2 C1 N2 V1 178.3(7) . . . . ?
O3 V1 N2 C1 -11.7(5) . . . . ?
O4 V1 N2 C1 167.8(7) . . . . ?
O1 V1 N2 C1 -108.4(5) . . . . ?
O2 V1 N2 C1 85.2(5) . . . . ?
N1 V1 N2 C1 168.7(5) . . . . ?
O3 V1 N2 C5 166.3(5) . . . . ?
O4 V1 N2 C5 -14.3(12) . . . . ?
O1 V1 N2 C5 69.5(5) . . . . ?
O2 V1 N2 C5 -96.8(5) . . . . ?
N1 V1 N2 C5 -13.3(5) . . . . ?
N2 C1 C2 C3 1.6(15) . . . . ?
O3 V1 O2 C16 175.7(5) . . . . ?
O4 V1 O2 C16 -82.6(5) . . . . ?
O1 V1 O2 C16 42.5(8) . . . . ?
N2 V1 O2 C16 89.7(5) . . . . ?
N1 V1 O2 C16 5.0(5) . . . . ?
O7 V2 N3 C44 -0.3(9) . . . . ?
O8 V2 N3 C44 179.2(2) . . . . ?
O6 V2 N3 C44 -83.7(3) . . . . ?
O5 V2 N3 C44 84.0(3) . . . . ?
N4 V2 N3 C44 0.4(3) . . . . ?
O7 V2 N3 C46 124.8(7) . . . . ?
O8 V2 N3 C46 -55.6(2) . . . . ?
O6 V2 N3 C46 41.4(3) . . . . ?
O5 V2 N3 C46 -150.9(3) . . . . ?
N4 V2 N3 C46 125.6(3) . . . . ?
O7 V2 N3 C45 -124.4(7) . . . . ?
O8 V2 N3 C45 55.2(2) . . . . ?
O6 V2 N3 C45 152.3(2) . . . . ?
O5 V2 N3 C45 -40.0(2) . . . . ?
N4 V2 N3 C45 -123.6(2) . . . . ?
C1 C2 C3 C4 -1.9(15) . . . . ?
O3 V1 O4 V1 42(100) . . . 2_666 ?
O1 V1 O4 V1 140(100) . . . 2_666 ?
O2 V1 O4 V1 -55(100) . . . 2_666 ?
N2 V1 O4 V1 -137(100) . . . 2_666 ?
N1 V1 O4 V1 -138(100) . . . 2_666 ?
O7 V2 N4 C38 -9.3(6) . . . . ?
O8 V2 N4 C38 162.6(8) . . . . ?
O6 V2 N4 C38 -106.1(6) . . . . ?
O5 V2 N4 C38 86.8(6) . . . . ?
N3 V2 N4 C38 170.9(6) . . . . ?
O7 V2 N4 C42 173.2(5) . . . . ?
O8 V2 N4 C42 -14.9(11) . . . . ?
O6 V2 N4 C42 76.3(5) . . . . ?
O5 V2 N4 C42 -90.8(5) . . . . ?
N3 V2 N4 C42 -6.7(5) . . . . ?
C2 C3 C4 C5 0.8(13) . . . . ?
O7 V2 O5 C58 179.7(5) . . . . ?
O8 V2 O5 C58 -77.8(5) . . . . ?
O6 V2 O5 C58 50.7(7) . . . . ?
N4 V2 O5 C58 94.1(5) . . . . ?
N3 V2 O5 C58 9.8(5) . . . . ?
C1 N2 C5 C4 -1.2(9) . . . . ?
V1 N2 C5 C4 -179.1(5) . . . . ?
C1 N2 C5 C6A 167.8(6) . . . . ?
V1 N2 C5 C6A -10.2(8) . . . . ?
C1 N2 C5 C6B -135.2(10) . . . . ?
V1 N2 C5 C6B 46.9(10) . . . . ?
C3 C4 C5 N2 0.8(11) . . . . ?
C3 C4 C5 C6A -168.2(7) . . . . ?
C3 C4 C5 C6B 133.1(13) . . . . ?
O7 V2 O6 C52 179.6(5) . . . . ?
O8 V2 O6 C52 76.7(5) . . . . ?
O5 V2 O6 C52 -51.5(7) . . . . ?
N4 V2 O6 C52 -94.8(5) . . . . ?
N3 V2 O6 C52 -10.5(4) . . . . ?
N2 C5 C6A C7 57.5(7) . . . . ?
C4 C5 C6A C7 -133.0(6) . . . . ?
C6B C5 C6A C7 -34.2(12) . . . . ?
N2 C5 C6B C7 -78(2) . . . . ?
C4 C5 C6B C7 143.4(15) . . . . ?
C6A C5 C6B C7 35.3(13) . . . . ?
C5 C6B C7 C6A -35.3(13) . . . . ?
C5 C6B C7 N1 69(2) . . . . ?
C5 C6A C7 C6B 35.7(12) . . . . ?
C5 C6A C7 N1 -75.0(6) . . . . ?
C9 N1 C7 C6B -149.4(11) . . . . ?
C8 N1 C7 C6B 95.8(12) . . . . ?
V1 N1 C7 C6B -25.5(12) . . . . ?
C9 N1 C7 C6A -83.3(5) . . . . ?
C8 N1 C7 C6A 161.9(4) . . . . ?
V1 N1 C7 C6A 40.6(5) . . . . ?
O7 V2 O8 V2 171(100) . . . 2_567 ?
O6 V2 O8 V2 -91(100) . . . 2_567 ?
O5 V2 O8 V2 74(100) . . . 2_567 ?
N4 V2 O8 V2 -1(100) . . . 2_567 ?
N3 V2 O8 V2 -9(100) . . . 2_567 ?
C7 N1 C8 C21 -62.4(4) . . . . ?
C9 N1 C8 C21 179.6(3) . . . . ?
V1 N1 C8 C21 66.8(4) . . . . ?
C7 N1 C9 C15 66.3(4) . . . . ?
C8 N1 C9 C15 -177.2(3) . . . . ?
V1 N1 C9 C15 -64.7(4) . . . . ?
V1 O1 C10 C15 -5.6(8) . . . . ?
V1 O1 C10 C11 171.4(4) . . . . ?
O1 C10 C11 C12 -179.7(4) . . . . ?
C15 C10 C11 C12 -2.7(7) . . . . ?
O1 C10 C11 C22 1.0(7) . . . . ?
C15 C10 C11 C22 178.0(5) . . . . ?
C10 C11 C12 C13 0.9(8) . . . . ?
C22 C11 C12 C13 -179.8(5) . . . . ?
C11 C12 C13 C14 1.3(9) . . . . ?
C11 C12 C13 C26 -179.3(6) . . . . ?
C12 C13 C14 C15 -1.8(8) . . . . ?
C26 C13 C14 C15 178.8(5) . . . . ?
C13 C14 C15 C10 0.0(7) . . . . ?
C13 C14 C15 C9 -174.0(4) . . . . ?
O1 C10 C15 C14 179.3(4) . . . . ?
C11 C10 C15 C14 2.3(7) . . . . ?
O1 C10 C15 C9 -6.6(6) . . . . ?
C11 C10 C15 C9 176.4(4) . . . . ?
N1 C9 C15 C14 -136.7(4) . . . . ?
N1 C9 C15 C10 49.4(6) . . . . ?
V1 O2 C16 C17 -169.2(4) . . . . ?
V1 O2 C16 C21 11.1(8) . . . . ?
O2 C16 C17 C18 178.5(4) . . . . ?
C21 C16 C17 C18 -1.9(8) . . . . ?
O2 C16 C17 C34 -3.2(8) . . . . ?
C21 C16 C17 C34 176.4(5) . . . . ?
C16 C17 C18 C19 0.3(9) . . . . ?
C34 C17 C18 C19 -178.0(6) . . . . ?
C17 C18 C19 C20 0.1(9) . . . . ?
C17 C18 C19 C30 178.4(6) . . . . ?
C18 C19 C20 C21 1.0(8) . . . . ?
C30 C19 C20 C21 -177.4(6) . . . . ?
C19 C20 C21 C16 -2.5(8) . . . . ?
C19 C20 C21 C8 171.5(5) . . . . ?
O2 C16 C21 C20 -177.4(4) . . . . ?
C17 C16 C21 C20 3.0(7) . . . . ?
O2 C16 C21 C8 8.6(7) . . . . ?
C17 C16 C21 C8 -171.0(5) . . . . ?
N1 C8 C21 C20 131.9(4) . . . . ?
N1 C8 C21 C16 -54.1(6) . . . . ?
C12 C11 C22 C23 114.4(6) . . . . ?
C10 C11 C22 C23 -66.4(7) . . . . ?
C12 C11 C22 C24 -124.9(6) . . . . ?
C10 C11 C22 C24 54.4(7) . . . . ?
C12 C11 C22 C25 -2.1(8) . . . . ?
C10 C11 C22 C25 177.1(6) . . . . ?
C12 C13 C26 C29A 174.0(13) . . . . ?
C14 C13 C26 C29A -6.6(15) . . . . ?
C12 C13 C26 C27B 19.8(19) . . . . ?
C14 C13 C26 C27B -160.8(17) . . . . ?
C12 C13 C26 C27A -49.5(12) . . . . ?
C14 C13 C26 C27A 129.9(11) . . . . ?
C12 C13 C26 C28B 131.0(15) . . . . ?
C14 C13 C26 C28B -49.6(16) . . . . ?
C12 C13 C26 C29B -120.4(13) . . . . ?
C14 C13 C26 C29B 59.0(14) . . . . ?
C12 C13 C26 C28A 58.6(12) . . . . ?
C14 C13 C26 C28A -122.0(11) . . . . ?
C18 C19 C30 C32A 173.0(17) . . . . ?
C20 C19 C30 C32A -8.8(18) . . . . ?
C18 C19 C30 C33B 122.9(13) . . . . ?
C20 C19 C30 C33B -58.9(14) . . . . ?
C18 C19 C30 C31A -49.4(14) . . . . ?
C20 C19 C30 C31A 128.8(13) . . . . ?
C18 C19 C30 C31B -4.8(16) . . . . ?
C20 C19 C30 C31B 173.4(13) . . . . ?
C18 C19 C30 C32B -119.1(9) . . . . ?
C20 C19 C30 C32B 59.1(10) . . . . ?
C18 C19 C30 C33A 60.7(12) . . . . ?
C20 C19 C30 C33A -121.1(11) . . . . ?
C18 C17 C34 C35 -3.1(9) . . . . ?
C16 C17 C34 C35 178.7(6) . . . . ?
C18 C17 C34 C37 123.8(6) . . . . ?
C16 C17 C34 C37 -54.4(8) . . . . ?
C18 C17 C34 C36 -119.1(6) . . . . ?
C16 C17 C34 C36 62.7(7) . . . . ?
C42 N4 C38 C39 -4.9(16) . . . . ?
V2 N4 C38 C39 177.1(11) . . . . ?
N4 C38 C39 C40 5(2) . . . . ?
C38 C39 C40 C41 -2(2) . . . . ?
C39 C40 C41 C42 -0.1(17) . . . . ?
C38 N4 C42 C41 2.4(11) . . . . ?
V2 N4 C42 C41 179.9(5) . . . . ?
C38 N4 C42 C43B -140.7(9) . . . . ?
V2 N4 C42 C43B 36.8(9) . . . . ?
C38 N4 C42 C43A 162.7(7) . . . . ?
V2 N4 C42 C43A -19.8(8) . . . . ?
C40 C41 C42 N4 0.1(13) . . . . ?
C40 C41 C42 C43B 141.8(11) . . . . ?
C40 C41 C42 C43A -159.8(9) . . . . ?
N4 C42 C43A C44 62.7(7) . . . . ?
C41 C42 C43A C44 -136.0(6) . . . . ?
C43B C42 C43A C44 -34.8(8) . . . . ?
N4 C42 C43B C44 -71.5(13) . . . . ?
C41 C42 C43B C44 142.3(10) . . . . ?
C43A C42 C43B C44 35.3(8) . . . . ?
C42 C43B C44 C43A -36.4(8) . . . . ?
C42 C43B C44 N3 71.6(12) . . . . ?
C42 C43A C44 C43B 36.0(8) . . . . ?
C42 C43A C44 N3 -73.6(6) . . . . ?
C46 N3 C44 C43B -155.1(7) . . . . ?
C45 N3 C44 C43B 90.9(8) . . . . ?
V2 N3 C44 C43B -31.6(8) . . . . ?
C46 N3 C44 C43A -86.9(5) . . . . ?
C45 N3 C44 C43A 159.2(4) . . . . ?
V2 N3 C44 C43A 36.7(5) . . . . ?
C44 N3 C45 C53 -66.0(4) . . . . ?
C46 N3 C45 C53 176.6(3) . . . . ?
V2 N3 C45 C53 64.3(3) . . . . ?
C44 N3 C46 C47 65.9(4) . . . . ?
C45 N3 C46 C47 -177.1(3) . . . . ?
V2 N3 C46 C47 -65.1(4) . . . . ?
N3 C46 C47 C48 -138.2(4) . . . . ?
N3 C46 C47 C52 48.4(6) . . . . ?
C52 C47 C48 C49 1.7(7) . . . . ?
C46 C47 C48 C49 -172.0(4) . . . . ?
C47 C48 C49 C50 -3.3(7) . . . . ?
C47 C48 C49 C67 175.8(5) . . . . ?
C48 C49 C50 C51 1.8(8) . . . . ?
C67 C49 C50 C51 -177.2(5) . . . . ?
C49 C50 C51 C52 1.1(7) . . . . ?
C49 C50 C51 C71 179.8(5) . . . . ?
V2 O6 C52 C51 172.4(3) . . . . ?
V2 O6 C52 C47 -7.8(7) . . . . ?
C50 C51 C52 O6 177.0(4) . . . . ?
C71 C51 C52 O6 -1.7(7) . . . . ?
C50 C51 C52 C47 -2.8(7) . . . . ?
C71 C51 C52 C47 178.5(4) . . . . ?
C48 C47 C52 O6 -178.3(4) . . . . ?
C46 C47 C52 O6 -4.7(6) . . . . ?
C48 C47 C52 C51 1.5(6) . . . . ?
C46 C47 C52 C51 175.1(4) . . . . ?
N3 C45 C53 C54 136.8(4) . . . . ?
N3 C45 C53 C58 -51.0(5) . . . . ?
C58 C53 C54 C55 -1.0(7) . . . . ?
C45 C53 C54 C55 171.3(4) . . . . ?
C53 C54 C55 C56 1.2(8) . . . . ?
C53 C54 C55 C59 -177.5(5) . . . . ?
C54 C55 C56 C57 -0.5(8) . . . . ?
C59 C55 C56 C57 178.2(5) . . . . ?
C55 C56 C57 C58 -0.3(8) . . . . ?
C55 C56 C57 C63 -176.7(6) . . . . ?
V2 O5 C58 C53 6.2(8) . . . . ?
V2 O5 C58 C57 -173.6(4) . . . . ?
C54 C53 C58 O5 -179.7(4) . . . . ?
C45 C53 C58 O5 8.2(7) . . . . ?
C54 C53 C58 C57 0.1(7) . . . . ?
C45 C53 C58 C57 -172.0(4) . . . . ?
C56 C57 C58 O5 -179.6(4) . . . . ?
C63 C57 C58 O5 -3.3(7) . . . . ?
C56 C57 C58 C53 0.5(7) . . . . ?
C63 C57 C58 C53 176.9(5) . . . . ?
C56 C55 C59 C62A -171.0(10) . . . . ?
C54 C55 C59 C62A 7.7(12) . . . . ?
C56 C55 C59 C61A -49.2(9) . . . . ?
C54 C55 C59 C61A 129.4(7) . . . . ?
C56 C55 C59 C60A 66.2(9) . . . . ?
C54 C55 C59 C60A -115.2(8) . . . . ?
C56 C55 C59 C61B -4.9(10) . . . . ?
C54 C55 C59 C61B 173.7(7) . . . . ?
C56 C55 C59 C62B -146(2) . . . . ?
C54 C55 C59 C62B 32(2) . . . . ?
C56 C55 C59 C60B 120(3) . . . . ?
C54 C55 C59 C60B -62(3) . . . . ?
C56 C57 C63 C66 -5.2(9) . . . . ?
C58 C57 C63 C66 178.7(6) . . . . ?
C56 C57 C63 C64 124.8(6) . . . . ?
C58 C57 C63 C64 -51.4(8) . . . . ?
C56 C57 C63 C65 -120.6(6) . . . . ?
C58 C57 C63 C65 63.2(7) . . . . ?
C48 C49 C67 C69 -168.7(7) . . . . ?
C50 C49 C67 C69 10.3(9) . . . . ?
C48 C49 C67 C70 67.4(8) . . . . ?
C50 C49 C67 C70 -113.6(7) . . . . ?
C48 C49 C67 C68 -46.1(7) . . . . ?
C50 C49 C67 C68 132.9(6) . . . . ?
C50 C51 C71 C74 -119.9(5) . . . . ?
C52 C51 C71 C74 58.7(6) . . . . ?
C50 C51 C71 C72 119.8(5) . . . . ?
C52 C51 C71 C72 -61.6(6) . . . . ?
C50 C51 C71 C73 2.6(8) . . . . ?
C52 C51 C71 C73 -178.8(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.06
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.140
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1413243'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H92 N2 O8 V2, 2(C3 H6 O)'
_chemical_formula_sum            'C66 H104 N2 O10 V2'
_chemical_formula_weight         1187.39

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   P2(1)/c
_symmetry_space_group_name_Hall  -P2ybc

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                   9.7921(19)
_cell_length_b                   28.523(6)
_cell_length_c                   11.769(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.467(15)
_cell_angle_gamma                90.00
_cell_volume                     3280.9(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    70658
_cell_measurement_theta_min      4.405
_cell_measurement_theta_max      31.889

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9197
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48486
_diffrn_reflns_av_R_equivalents  0.1841
_diffrn_reflns_av_unetI/netI     0.1773
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         29.25
_reflns_number_total             7885
_reflns_number_gt                3839
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_cell_refinement       
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_reduction        
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_solution    
'XS V2008/1 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_refinement  
'XL V2008/4 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;
_iucr_refine-instructions_details 
;
TITL    manar198 in P 1 21/c 1
CELL   0.71073   9.7921  28.5228  11.7685  90.000  93.467  90.000
ZERR     2       0.0019   0.0062   0.0025   0.000   0.015   0.000
LATT  1
SYMM -X, 0.50000+Y, 0.50000-Z
SFAC    C   H   N   O   V
UNIT   132 208   4  20   4
MERG    2
ACTA 50
CONF
WPDB -1
BOND $H
L.S.    30
FMAP    2
PLAN    -10
SIZE  0.050   0.130   0.25
SADI C1SA C3S C1SB C3S C2SA C3S C2SB C3S
SIMU C1SA C1SB C3S C2SA C2SB O1SA O1SB
DELU C1SA C1SB C3S C2SA C2SB O1SA O1SB
SADI C3S O1SA C3S O1SB
OMIT 0 2 0
 
HTAB N1 O3_$1
EQIV $1 [ -x, -y, -z+1 ]
 
WGHT    0.065900    1.096700
FVAR       0.16458   0.41198
V1    5    0.105952    0.040595    0.476201    11.00000    0.02479    0.02335 =
         0.02700   -0.00023    0.00400   -0.00097
O1    4    0.047416   -0.002572    0.594009    11.00000    0.02708    0.02565 =
         0.02326    0.00137    0.00018   -0.00422
AFIX   3
H1O   2    0.096826   -0.008052    0.657210    11.00000   -1.50000
AFIX   0
N1    3   -0.075575    0.085185    0.541086    11.00000    0.02104    0.02629 =
         0.02604   -0.00203    0.00270   -0.00573
H1N   2   -0.134118    0.069206    0.528849    11.00000    0.01020
C1    1    0.191147    0.115469    0.643732    11.00000    0.02937    0.02264 =
         0.02543    0.00369    0.00028   -0.00192
PART   1
O1SA  4    0.299906   -0.039160    0.649422    21.00000    0.03284    0.03291 =
         0.05193    0.01376    0.00738    0.00058
C1SA  1    0.508378   -0.032413    0.738504    21.00000    0.05626    0.06630 =
         0.02598   -0.01053    0.00366   -0.00391
AFIX 137
H1S1  2    0.532372   -0.018556    0.668093    21.00000   -1.50000
H1S2  2    0.514352   -0.065924    0.733069    21.00000   -1.50000
H1S3  2    0.570211   -0.021530    0.799245    21.00000   -1.50000
AFIX   0
C2SA  1    0.299125    0.002972    0.828073    21.00000    0.04252    0.05832 =
         0.04343    0.01286   -0.02151   -0.02084
AFIX 137
H2S1  2    0.354365    0.027937    0.860658    21.00000   -1.50000
H2S2  2    0.272552   -0.017586    0.887438    21.00000   -1.50000
H2S3  2    0.218860    0.015848    0.788873    21.00000   -1.50000
AFIX   0
PART   2
O1SB  4    0.233422   -0.005206    0.778105   -21.00000    0.04569    0.05040 =
         0.04380    0.00606    0.00235    0.00112
C1SB  1    0.422636   -0.038807    0.684173   -21.00000    0.05534    0.04071 =
         0.07659    0.01052   -0.01026   -0.01051
AFIX 137
H1S4  2    0.377424   -0.031043    0.611969   -21.00000   -1.50000
H1S5  2    0.419458   -0.072116    0.695425   -21.00000   -1.50000
H1S6  2    0.516248   -0.028721    0.685431   -21.00000   -1.50000
AFIX   0
C2SB  1    0.437658   -0.003362    0.884202   -21.00000    0.05492    0.05842 =
         0.08064    0.01996    0.00428    0.00805
AFIX 137
H2S4  2    0.497273    0.022775    0.873417   -21.00000   -1.50000
H2S5  2    0.490023   -0.029259    0.915530   -21.00000   -1.50000
H2S6  2    0.369493    0.005367    0.935558   -21.00000   -1.50000
AFIX   0
PART   0
 
C2    1    0.064268    0.126062    0.688860    11.00000    0.02118    0.02488 =
         0.02460    0.00579    0.00116    0.00014
O2    4    0.205711    0.077722    0.578041    11.00000    0.02207    0.02456 =
         0.02813   -0.00148    0.00046   -0.00162
O3    4    0.230147    0.009588    0.435540    11.00000    0.02753    0.02855 =
         0.02837   -0.00005    0.00716    0.00273
C3    1    0.051507    0.165395    0.754998    11.00000    0.01674    0.02871 =
         0.02523    0.00208    0.00259    0.00052
AFIX  43
H3    2   -0.033119    0.172123    0.782973    11.00000   -1.20000
AFIX   0
C3S   1    0.363407   -0.018561    0.762358    11.00000    0.03537    0.05635 =
         0.14267    0.04734   -0.02710   -0.01241
 
O4    4    0.087279    0.080765    0.353502    11.00000    0.02451    0.02388 =
         0.02573    0.00203    0.00349   -0.00068
C4    1    0.160138    0.195338    0.781429    11.00000    0.02511    0.02378 =
         0.02041    0.00129    0.00193    0.00149
C5    1    0.285231    0.184439    0.734614    11.00000    0.02198    0.02597 =
         0.02518    0.00500    0.00006   -0.00209
AFIX  43
H5    2    0.358774    0.204569    0.749880    11.00000   -1.20000
AFIX   0
C6    1    0.305361    0.145509    0.667136    11.00000    0.02266    0.02253 =
         0.02416    0.00373    0.00188    0.00320
C7    1    0.444074    0.135293    0.619010    11.00000    0.01998    0.02649 =
         0.03916    0.00013    0.00180   -0.00333
C8    1    0.551200    0.171729    0.658191    11.00000    0.02683    0.04017 =
         0.05447   -0.00668    0.01174   -0.00141
AFIX 137
H8A   2    0.560093    0.172329    0.739864    11.00000   -1.50000
H8B   2    0.523194    0.202078    0.630271    11.00000   -1.50000
H8C   2    0.637621    0.163673    0.629054    11.00000   -1.50000
AFIX   0
C9    1    0.431524    0.135745    0.488525    11.00000    0.03090    0.03509 =
         0.04265    0.00066    0.01328   -0.00194
AFIX 137
H9A   2    0.517290    0.126713    0.459658    11.00000   -1.50000
H9B   2    0.407754    0.166722    0.462268    11.00000   -1.50000
H9C   2    0.361668    0.114084    0.461944    11.00000   -1.50000
AFIX   0
C10   1    0.497227    0.087472    0.660110    11.00000    0.02499    0.03995 =
         0.04766    0.00489   -0.00120    0.00300
AFIX 137
H10A  2    0.500143    0.086432    0.741755    11.00000   -1.50000
H10B  2    0.587547    0.082614    0.634845    11.00000   -1.50000
H10C  2    0.437386    0.063324    0.629550    11.00000   -1.50000
AFIX   0
C11   1    0.149162    0.238909    0.856347    11.00000    0.02608    0.03002 =
         0.02337   -0.00145    0.00364    0.00049
C12   1    0.011956    0.240691    0.913565    11.00000    0.03886    0.03151 =
         0.04799   -0.01218    0.01200   -0.00406
AFIX 137
H12A  2   -0.061583    0.243745    0.856301    11.00000   -1.50000
H12B  2    0.011577    0.267087    0.964156    11.00000   -1.50000
H12C  2    0.000325    0.212352    0.955915    11.00000   -1.50000
AFIX   0
C13   1    0.163349    0.283244    0.785618    11.00000    0.03797    0.02753 =
         0.04212   -0.00453    0.00551   -0.00105
AFIX 137
H13A  2    0.249071    0.282635    0.750140    11.00000   -1.50000
H13B  2    0.160211    0.310238    0.834115    11.00000   -1.50000
H13C  2    0.089698    0.284770    0.728072    11.00000   -1.50000
AFIX   0
C14   1    0.262025    0.237667    0.951453    11.00000    0.04338    0.03414 =
         0.03120   -0.00801    0.00262   -0.00196
AFIX 137
H14A  2    0.254288    0.209406    0.994896    11.00000   -1.50000
H14B  2    0.253191    0.264321    1.000277    11.00000   -1.50000
H14C  2    0.349643    0.238493    0.919054    11.00000   -1.50000
AFIX   0
C15   1   -0.054331    0.093888    0.664238    11.00000    0.02290    0.02989 =
         0.02214    0.00030    0.00276   -0.00167
AFIX  23
H15A  2   -0.037576    0.064373    0.703589    11.00000   -1.20000
H15B  2   -0.136281    0.107721    0.692317    11.00000   -1.20000
AFIX   0
C16   1   -0.101928    0.129693    0.479417    11.00000    0.02573    0.02491 =
         0.02943   -0.00241    0.00147    0.00154
AFIX  23
H16A  2   -0.027114    0.151091    0.498778    11.00000   -1.20000
H16B  2   -0.184693    0.143589    0.505819    11.00000   -1.20000
AFIX   0
C17   1   -0.117484    0.125152    0.352316    11.00000    0.02457    0.02580 =
         0.02302    0.00048   -0.00023   -0.00411
C18   1   -0.226004    0.146785    0.291808    11.00000    0.02559    0.02577 =
         0.03180   -0.00180    0.00510   -0.00214
AFIX  43
H18   2   -0.292902    0.161726    0.331413    11.00000   -1.20000
AFIX   0
C19   1   -0.237256    0.146690    0.173479    11.00000    0.02590    0.02641 =
         0.03155   -0.00027   -0.00075   -0.00582
C20   1   -0.132266    0.124601    0.118389    11.00000    0.03624    0.02751 =
         0.02255    0.00255    0.00354   -0.00506
AFIX  43
H20   2   -0.136888    0.125078    0.039234    11.00000   -1.20000
AFIX   0
C21   1   -0.021088    0.101902    0.173895    11.00000    0.02987    0.02253 =
         0.02848   -0.00115    0.00449   -0.00361
C22   1   -0.017603    0.101957    0.293800    11.00000    0.02462    0.02433 =
         0.02908    0.00275    0.00611   -0.00120
C23   1   -0.354783    0.170161    0.104030    11.00000    0.02600    0.04307 =
         0.02797    0.01021    0.00159    0.00142
C24   1   -0.301689    0.211341    0.036526    11.00000    0.03558    0.06272 =
         0.05317    0.03122    0.00743    0.00893
AFIX 137
H24A  2   -0.238008    0.200094   -0.016072    11.00000   -1.50000
H24B  2   -0.256697    0.233356    0.087890    11.00000   -1.50000
H24C  2   -0.376977    0.226466   -0.004686    11.00000   -1.50000
AFIX   0
C25   1   -0.423586    0.135046    0.021001    11.00000    0.03528    0.06508 =
         0.04114    0.00187   -0.00373   -0.00078
AFIX 137
H25A  2   -0.357655    0.123391   -0.029141    11.00000   -1.50000
H25B  2   -0.496677    0.150245   -0.022828    11.00000   -1.50000
H25C  2   -0.459677    0.109427    0.062780    11.00000   -1.50000
AFIX   0
C26   1   -0.464894    0.188560    0.180251    11.00000    0.02752    0.04565 =
         0.04144    0.01293    0.00008    0.00651
AFIX 137
H26A  2   -0.538128    0.202356    0.133707    11.00000   -1.50000
H26B  2   -0.425578    0.211756    0.231499    11.00000   -1.50000
H26C  2   -0.499793    0.163069    0.223182    11.00000   -1.50000
AFIX   0
C27   1    0.092114    0.079624    0.108461    11.00000    0.03118    0.02640 =
         0.03042    0.00075    0.00498   -0.00124
C28   1    0.066321    0.085042   -0.020027    11.00000    0.05270    0.04122 =
         0.03348    0.00334    0.01438    0.01172
AFIX 137
H28A  2   -0.017539    0.069556   -0.044109    11.00000   -1.50000
H28B  2    0.140631    0.071248   -0.057852    11.00000   -1.50000
H28C  2    0.059643    0.117733   -0.038965    11.00000   -1.50000
AFIX   0
C29   1    0.102167    0.027104    0.134836    11.00000    0.03113    0.03575 =
         0.02857   -0.00259    0.00085    0.00618
AFIX 137
H29A  2    0.128706    0.022755    0.214001    11.00000   -1.50000
H29B  2    0.169229    0.013040    0.089321    11.00000   -1.50000
H29C  2    0.014868    0.012602    0.117717    11.00000   -1.50000
AFIX   0
C30   1    0.228500    0.103769    0.142208    11.00000    0.03786    0.03883 =
         0.05080   -0.00573    0.02259   -0.00461
AFIX 137
H30A  2    0.221392    0.136625    0.125177    11.00000   -1.50000
H30B  2    0.299687    0.090154    0.100292    11.00000   -1.50000
H30C  2    0.249806    0.099642    0.222280    11.00000   -1.50000
 
HKLF  4
 
REM     manar198 in P 1 21/c 1
REM R1 =  0.0753 for   3839 Fo > 4sig(Fo)  and  0.1733 for all   7885 data
REM    409 parameters refined using     79 restraints
 
END  
     
WGHT      0.0657      1.0974 
REM Highest difference peak  0.539,  deepest hole -0.674,  1-sigma level  0.089
Q1    1   0.3230 -0.0072  0.8063  11.00000  0.05    0.54
Q2    1   0.4441 -0.0005  0.9180  11.00000  0.05    0.53
Q3    1   0.3571 -0.0315  0.7176  11.00000  0.05    0.52
Q4    1   0.2962 -0.0342  0.6223  11.00000  0.05    0.42
Q5    1   0.3149 -0.0410  0.4296  11.00000  0.05    0.41
Q6    1  -0.4445  0.0909  0.1818  11.00000  0.05    0.34
Q7    1   0.7226  0.2351  0.7695  11.00000  0.05    0.32
Q8    1   0.2008  0.0024  0.8358  11.00000  0.05    0.32
Q9    1  -0.3061  0.2253 -0.0503  11.00000  0.05    0.32
Q10   1   0.6793  0.1496  0.8254  11.00000  0.05    0.31
;

_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)+(0.0659P)²+1.0967P] 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         7885
_refine_ls_number_parameters     409
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1617
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.116
_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 0.10595(7) 0.04060(3) 0.47620(6) 0.0249(2) Uani 1 1 d . . .
O1 O 0.0474(3) -0.00257(9) 0.5940(2) 0.0254(7) Uani 1 1 d . . .
H1O H 0.0968 -0.0081 0.6572 0.038 Uiso 1 1 d R . .
N1 N -0.0756(4) 0.08518(13) 0.5411(3) 0.0244(9) Uani 1 1 d . . .
H1N H -0.134(4) 0.0692(14) 0.529(3) 0.010(11) Uiso 1 1 d . . .
C1 C 0.1911(4) 0.11547(15) 0.6437(4) 0.0259(10) Uani 1 1 d . . .
O1SA O 0.2999(8) -0.0392(3) 0.6494(7) 0.039(2) Uani 0.412(7) 1 d PDU A 1
C1SA C 0.5084(12) -0.0324(5) 0.7385(11) 0.049(4) Uani 0.412(7) 1 d PDU A 1
H1S1 H 0.5324 -0.0186 0.6681 0.074 Uiso 0.412(7) 1 calc PR A 1
H1S2 H 0.5144 -0.0659 0.7331 0.074 Uiso 0.412(7) 1 calc PR A 1
H1S3 H 0.5702 -0.0215 0.7992 0.074 Uiso 0.412(7) 1 calc PR A 1
C2SA C 0.2991(15) 0.0030(5) 0.8281(12) 0.049(3) Uani 0.412(7) 1 d PDU A 1
H2S1 H 0.3544 0.0279 0.8607 0.074 Uiso 0.412(7) 1 calc PR A 1
H2S2 H 0.2726 -0.0176 0.8874 0.074 Uiso 0.412(7) 1 calc PR A 1
H2S3 H 0.2189 0.0158 0.7889 0.074 Uiso 0.412(7) 1 calc PR A 1
O1SB O 0.2334(7) -0.0052(2) 0.7781(6) 0.0466(19) Uani 0.588(7) 1 d PDU A 2
C1SB C 0.4226(11) -0.0388(4) 0.6842(9) 0.058(3) Uani 0.588(7) 1 d PDU A 2
H1S4 H 0.3774 -0.0310 0.6120 0.087 Uiso 0.588(7) 1 calc PR A 2
H1S5 H 0.4195 -0.0721 0.6954 0.087 Uiso 0.588(7) 1 calc PR A 2
H1S6 H 0.5162 -0.0287 0.6854 0.087 Uiso 0.588(7) 1 calc PR A 2
C2SB C 0.4377(9) -0.0034(4) 0.8842(8) 0.065(3) Uani 0.588(7) 1 d PDU A 2
H2S4 H 0.4973 0.0228 0.8734 0.097 Uiso 0.588(7) 1 calc PR A 2
H2S5 H 0.4900 -0.0293 0.9155 0.097 Uiso 0.588(7) 1 calc PR A 2
H2S6 H 0.3695 0.0054 0.9356 0.097 Uiso 0.588(7) 1 calc PR A 2
C2 C 0.0643(4) 0.12606(14) 0.6889(3) 0.0236(9) Uani 1 1 d . . .
O2 O 0.2057(3) 0.07772(9) 0.5780(2) 0.0250(7) Uani 1 1 d . . .
O3 O 0.2301(3) 0.00959(10) 0.4355(2) 0.0279(7) Uani 1 1 d . . .
C3 C 0.0515(4) 0.16540(14) 0.7550(3) 0.0235(9) Uani 1 1 d . . .
H3 H -0.0331 0.1721 0.7830 0.028 Uiso 1 1 calc R . .
C3S C 0.3634(6) -0.0186(2) 0.7624(7) 0.079(2) Uani 1 1 d DU . .
O4 O 0.0873(3) 0.08077(9) 0.3535(2) 0.0246(7) Uani 1 1 d . . .
C4 C 0.1601(4) 0.19534(14) 0.7814(3) 0.0231(9) Uani 1 1 d . . .
C5 C 0.2852(4) 0.18444(15) 0.7346(3) 0.0244(9) Uani 1 1 d . . .
H5 H 0.3588 0.2046 0.7499 0.029 Uiso 1 1 calc R . .
C6 C 0.3054(4) 0.14551(14) 0.6671(3) 0.0231(9) Uani 1 1 d . . .
C7 C 0.4441(4) 0.13529(15) 0.6190(4) 0.0285(10) Uani 1 1 d . . .
C8 C 0.5512(4) 0.17173(17) 0.6582(4) 0.0401(12) Uani 1 1 d . . .
H8A H 0.5601 0.1723 0.7399 0.060 Uiso 1 1 calc R . .
H8B H 0.5232 0.2021 0.6303 0.060 Uiso 1 1 calc R . .
H8C H 0.6376 0.1637 0.6291 0.060 Uiso 1 1 calc R . .
C9 C 0.4315(4) 0.13575(16) 0.4885(4) 0.0358(11) Uani 1 1 d . . .
H9A H 0.5173 0.1267 0.4597 0.054 Uiso 1 1 calc R . .
H9B H 0.4078 0.1667 0.4623 0.054 Uiso 1 1 calc R . .
H9C H 0.3617 0.1141 0.4619 0.054 Uiso 1 1 calc R . .
C10 C 0.4972(4) 0.08747(16) 0.6601(4) 0.0377(12) Uani 1 1 d . . .
H10A H 0.5001 0.0864 0.7418 0.057 Uiso 1 1 calc R . .
H10B H 0.5875 0.0826 0.6348 0.057 Uiso 1 1 calc R . .
H10C H 0.4374 0.0633 0.6295 0.057 Uiso 1 1 calc R . .
C11 C 0.1492(4) 0.23891(15) 0.8563(4) 0.0264(10) Uani 1 1 d . . .
C12 C 0.0120(5) 0.24069(16) 0.9136(4) 0.0391(12) Uani 1 1 d . . .
H12A H -0.0616 0.2437 0.8563 0.059 Uiso 1 1 calc R . .
H12B H 0.0116 0.2671 0.9642 0.059 Uiso 1 1 calc R . .
H12C H 0.0003 0.2124 0.9559 0.059 Uiso 1 1 calc R . .
C13 C 0.1633(5) 0.28324(15) 0.7856(4) 0.0357(11) Uani 1 1 d . . .
H13A H 0.2491 0.2826 0.7501 0.054 Uiso 1 1 calc R . .
H13B H 0.1602 0.3102 0.8341 0.054 Uiso 1 1 calc R . .
H13C H 0.0897 0.2848 0.7281 0.054 Uiso 1 1 calc R . .
C14 C 0.2620(5) 0.23767(16) 0.9515(4) 0.0362(11) Uani 1 1 d . . .
H14A H 0.2543 0.2094 0.9949 0.054 Uiso 1 1 calc R . .
H14B H 0.2532 0.2643 1.0003 0.054 Uiso 1 1 calc R . .
H14C H 0.3496 0.2385 0.9191 0.054 Uiso 1 1 calc R . .
C15 C -0.0543(4) 0.09389(15) 0.6642(3) 0.0249(10) Uani 1 1 d . . .
H15A H -0.0376 0.0644 0.7036 0.030 Uiso 1 1 calc R . .
H15B H -0.1363 0.1077 0.6923 0.030 Uiso 1 1 calc R . .
C16 C -0.1019(4) 0.12969(14) 0.4794(4) 0.0267(10) Uani 1 1 d . . .
H16A H -0.0271 0.1511 0.4988 0.032 Uiso 1 1 calc R . .
H16B H -0.1847 0.1436 0.5058 0.032 Uiso 1 1 calc R . .
C17 C -0.1175(4) 0.12515(15) 0.3523(3) 0.0245(10) Uani 1 1 d . . .
C18 C -0.2260(4) 0.14679(15) 0.2918(4) 0.0276(10) Uani 1 1 d . . .
H18 H -0.2929 0.1617 0.3314 0.033 Uiso 1 1 calc R . .
C19 C -0.2373(4) 0.14669(15) 0.1735(4) 0.0281(10) Uani 1 1 d . . .
C20 C -0.1323(4) 0.12460(15) 0.1184(4) 0.0287(10) Uani 1 1 d . . .
H20 H -0.1369 0.1251 0.0392 0.034 Uiso 1 1 calc R . .
C21 C -0.0211(4) 0.10190(15) 0.1739(4) 0.0268(10) Uani 1 1 d . . .
C22 C -0.0176(4) 0.10196(15) 0.2938(4) 0.0258(10) Uani 1 1 d . . .
C23 C -0.3548(4) 0.17016(17) 0.1040(4) 0.0323(11) Uani 1 1 d . . .
C24 C -0.3017(5) 0.21134(19) 0.0365(4) 0.0503(15) Uani 1 1 d . . .
H24A H -0.2380 0.2001 -0.0161 0.075 Uiso 1 1 calc R . .
H24B H -0.2567 0.2334 0.0879 0.075 Uiso 1 1 calc R . .
H24C H -0.3770 0.2265 -0.0047 0.075 Uiso 1 1 calc R . .
C25 C -0.4236(5) 0.13505(19) 0.0210(4) 0.0474(14) Uani 1 1 d . . .
H25A H -0.3577 0.1234 -0.0291 0.071 Uiso 1 1 calc R . .
H25B H -0.4967 0.1502 -0.0228 0.071 Uiso 1 1 calc R . .
H25C H -0.4597 0.1094 0.0628 0.071 Uiso 1 1 calc R . .
C26 C -0.4649(4) 0.18856(17) 0.1803(4) 0.0383(12) Uani 1 1 d . . .
H26A H -0.5381 0.2024 0.1337 0.057 Uiso 1 1 calc R . .
H26B H -0.4256 0.2118 0.2315 0.057 Uiso 1 1 calc R . .
H26C H -0.4998 0.1631 0.2232 0.057 Uiso 1 1 calc R . .
C27 C 0.0921(4) 0.07962(15) 0.1085(4) 0.0292(10) Uani 1 1 d . . .
C28 C 0.0663(5) 0.08504(18) -0.0200(4) 0.0420(13) Uani 1 1 d . . .
H28A H -0.0175 0.0696 -0.0441 0.063 Uiso 1 1 calc R . .
H28B H 0.1406 0.0712 -0.0579 0.063 Uiso 1 1 calc R . .
H28C H 0.0596 0.1177 -0.0390 0.063 Uiso 1 1 calc R . .
C29 C 0.1022(4) 0.02710(15) 0.1348(4) 0.0319(11) Uani 1 1 d . . .
H29A H 0.1287 0.0228 0.2140 0.048 Uiso 1 1 calc R . .
H29B H 0.1692 0.0130 0.0893 0.048 Uiso 1 1 calc R . .
H29C H 0.0149 0.0126 0.1177 0.048 Uiso 1 1 calc R . .
C30 C 0.2285(4) 0.10377(17) 0.1422(4) 0.0417(13) Uani 1 1 d . . .
H30A H 0.2214 0.1366 0.1252 0.063 Uiso 1 1 calc R . .
H30B H 0.2997 0.0902 0.1003 0.063 Uiso 1 1 calc R . .
H30C H 0.2498 0.0996 0.2223 0.063 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 O3 1.600(3) . ?
V1 O2 1.836(3) . ?
V1 O4 1.844(3) . ?
V1 O1 1.965(3) . ?
V1 O1 1.991(3) 3_556 ?
V1 N1 2.350(4) . ?
O1 V1 1.991(3) 3_556 ?
O1 H1O 0.8765 . ?
N1 C15 1.473(5) . ?
N1 C16 1.477(5) . ?
N1 H1N 0.74(4) . ?
C1 O2 1.338(5) . ?
C1 C2 1.413(5) . ?
C1 C6 1.423(5) . ?
O1SA C3S 1.549(10) . ?
C1SA C3S 1.516(11) . ?
C1SA H1S1 0.9600 . ?
C1SA H1S2 0.9600 . ?
C1SA H1S3 0.9600 . ?
C2SA C3S 1.196(12) . ?
C2SA H2S1 0.9600 . ?
C2SA H2S2 0.9600 . ?
C2SA H2S3 0.9600 . ?
O1SB C3S 1.352(8) . ?
C1SB C3S 1.257(10) . ?
C1SB H1S4 0.9600 . ?
C1SB H1S5 0.9600 . ?
C1SB H1S6 0.9600 . ?
C2SB C3S 1.627(10) . ?
C2SB H2S4 0.9600 . ?
C2SB H2S5 0.9600 . ?
C2SB H2S6 0.9600 . ?
C2 C3 1.375(6) . ?
C2 C15 1.495(5) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9300 . ?
O4 C22 1.351(5) . ?
C4 C5 1.408(5) . ?
C4 C11 1.531(6) . ?
C5 C6 1.386(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.531(5) . ?
C7 C8 1.528(6) . ?
C7 C10 1.528(6) . ?
C7 C9 1.533(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.525(6) . ?
C11 C14 1.525(6) . ?
C11 C12 1.540(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.500(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.388(6) . ?
C17 C22 1.396(5) . ?
C18 C19 1.390(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.398(6) . ?
C19 C23 1.525(6) . ?
C20 C21 1.395(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.409(6) . ?
C21 C27 1.526(6) . ?
C23 C24 1.527(6) . ?
C23 C25 1.527(7) . ?
C23 C26 1.536(6) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.526(6) . ?
C27 C29 1.532(6) . ?
C27 C30 1.533(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 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
O3 V1 O2 97.47(13) . . ?
O3 V1 O4 98.65(13) . . ?
O2 V1 O4 100.17(13) . . ?
O3 V1 O1 97.13(13) . . ?
O2 V1 O1 93.85(12) . . ?
O4 V1 O1 157.28(12) . . ?
O3 V1 O1 98.20(13) . 3_556 ?
O2 V1 O1 160.62(12) . 3_556 ?
O4 V1 O1 88.68(12) . 3_556 ?
O1 V1 O1 72.94(13) . 3_556 ?
O3 V1 N1 178.38(14) . . ?
O2 V1 N1 81.88(13) . . ?
O4 V1 N1 82.94(12) . . ?
O1 V1 N1 81.45(12) . . ?
O1 V1 N1 82.14(12) 3_556 . ?
V1 O1 V1 107.06(13) . 3_556 ?
V1 O1 H1O 122.7 . . ?
V1 O1 H1O 128.2 3_556 . ?
C15 N1 C16 110.4(3) . . ?
C15 N1 V1 110.3(2) . . ?
C16 N1 V1 114.7(2) . . ?
C15 N1 H1N 111(3) . . ?
C16 N1 H1N 109(3) . . ?
V1 N1 H1N 101(3) . . ?
O2 C1 C2 121.1(4) . . ?
O2 C1 C6 119.1(4) . . ?
C2 C1 C6 119.8(4) . . ?
C3S C1SA H1S1 109.5 . . ?
C3S C1SA H1S2 109.5 . . ?
C3S C1SA H1S3 109.5 . . ?
C3S C2SA H2S1 109.5 . . ?
C3S C2SA H2S2 109.5 . . ?
C3S C2SA H2S3 109.5 . . ?
C3S C1SB H1S4 109.5 . . ?
C3S C1SB H1S5 109.5 . . ?
H1S4 C1SB H1S5 109.5 . . ?
C3S C1SB H1S6 109.5 . . ?
H1S4 C1SB H1S6 109.5 . . ?
H1S5 C1SB H1S6 109.5 . . ?
C3S C2SB H2S4 109.5 . . ?
C3S C2SB H2S5 109.5 . . ?
H2S4 C2SB H2S5 109.5 . . ?
C3S C2SB H2S6 109.5 . . ?
H2S4 C2SB H2S6 109.5 . . ?
H2S5 C2SB H2S6 109.5 . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 C15 121.0(3) . . ?
C1 C2 C15 119.1(4) . . ?
C1 O2 V1 140.4(3) . . ?
C2 C3 C4 122.4(4) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C2SA C3S C1SB 173.3(11) . . ?
C2SA C3S O1SB 39.7(6) . . ?
C1SB C3S O1SB 135.2(9) . . ?
C2SA C3S C1SA 142.1(12) . . ?
C1SB C3S C1SA 42.8(6) . . ?
O1SB C3S C1SA 177.0(9) . . ?
C2SA C3S O1SA 123.4(9) . . ?
C1SB C3S O1SA 51.4(7) . . ?
O1SB C3S O1SA 83.8(5) . . ?
C1SA C3S O1SA 94.2(8) . . ?
C2SA C3S C2SB 61.2(9) . . ?
C1SB C3S C2SB 124.5(7) . . ?
O1SB C3S C2SB 100.3(7) . . ?
C1SA C3S C2SB 81.9(6) . . ?
O1SA C3S C2SB 172.9(6) . . ?
C22 O4 V1 136.2(2) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C11 123.4(4) . . ?
C5 C4 C11 119.8(4) . . ?
C6 C5 C4 123.9(4) . . ?
C6 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C5 C6 C1 117.1(4) . . ?
C5 C6 C7 121.6(4) . . ?
C1 C6 C7 121.2(4) . . ?
C8 C7 C10 107.3(4) . . ?
C8 C7 C6 111.5(4) . . ?
C10 C7 C6 110.2(3) . . ?
C8 C7 C9 108.0(4) . . ?
C10 C7 C9 109.3(4) . . ?
C6 C7 C9 110.5(3) . . ?
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 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C14 109.5(4) . . ?
C13 C11 C4 110.3(3) . . ?
C14 C11 C4 109.3(3) . . ?
C13 C11 C12 108.8(4) . . ?
C14 C11 C12 107.0(4) . . ?
C4 C11 C12 111.8(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C2 110.9(3) . . ?
N1 C15 H15A 109.5 . . ?
C2 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
C2 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N1 C16 C17 114.8(3) . . ?
N1 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
N1 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C22 119.7(4) . . ?
C18 C17 C16 120.1(4) . . ?
C22 C17 C16 120.1(4) . . ?
C17 C18 C19 121.7(4) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C20 116.7(4) . . ?
C18 C19 C23 123.2(4) . . ?
C20 C19 C23 120.1(4) . . ?
C21 C20 C19 124.5(4) . . ?
C21 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
C20 C21 C22 116.1(4) . . ?
C20 C21 C27 121.8(4) . . ?
C22 C21 C27 122.1(4) . . ?
O4 C22 C17 119.2(4) . . ?
O4 C22 C21 119.4(4) . . ?
C17 C22 C21 121.3(4) . . ?
C19 C23 C24 110.3(3) . . ?
C19 C23 C25 110.1(4) . . ?
C24 C23 C25 108.8(4) . . ?
C19 C23 C26 111.7(4) . . ?
C24 C23 C26 108.3(4) . . ?
C25 C23 C26 107.4(4) . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C21 112.1(4) . . ?
C28 C27 C29 107.7(4) . . ?
C21 C27 C29 110.2(3) . . ?
C28 C27 C30 107.5(4) . . ?
C21 C27 C30 109.3(4) . . ?
C29 C27 C30 110.0(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
O3 V1 O1 V1 -96.43(15) . . . 3_556 ?
O2 V1 O1 V1 165.53(13) . . . 3_556 ?
O4 V1 O1 V1 37.3(4) . . . 3_556 ?
O1 V1 O1 V1 0.0 3_556 . . 3_556 ?
N1 V1 O1 V1 84.35(14) . . . 3_556 ?
O3 V1 N1 C15 28(5) . . . . ?
O2 V1 N1 C15 -38.3(3) . . . . ?
O4 V1 N1 C15 -139.7(3) . . . . ?
O1 V1 N1 C15 56.9(3) . . . . ?
O1 V1 N1 C15 130.7(3) 3_556 . . . ?
O3 V1 N1 C16 154(5) . . . . ?
O2 V1 N1 C16 87.1(3) . . . . ?
O4 V1 N1 C16 -14.3(3) . . . . ?
O1 V1 N1 C16 -177.7(3) . . . . ?
O1 V1 N1 C16 -103.9(3) 3_556 . . . ?
O2 C1 C2 C3 -179.2(4) . . . . ?
C6 C1 C2 C3 0.1(6) . . . . ?
O2 C1 C2 C15 1.2(6) . . . . ?
C6 C1 C2 C15 -179.5(4) . . . . ?
C2 C1 O2 V1 29.8(6) . . . . ?
C6 C1 O2 V1 -149.5(3) . . . . ?
O3 V1 O2 C1 172.4(4) . . . . ?
O4 V1 O2 C1 72.1(4) . . . . ?
O1 V1 O2 C1 -89.9(4) . . . . ?
O1 V1 O2 C1 -43.9(6) 3_556 . . . ?
N1 V1 O2 C1 -9.1(4) . . . . ?
C1 C2 C3 C4 -1.1(6) . . . . ?
C15 C2 C3 C4 178.6(4) . . . . ?
O3 V1 O4 C22 143.5(4) . . . . ?
O2 V1 O4 C22 -117.2(4) . . . . ?
O1 V1 O4 C22 10.0(6) . . . . ?
O1 V1 O4 C22 45.4(4) 3_556 . . . ?
N1 V1 O4 C22 -36.8(4) . . . . ?
C2 C3 C4 C5 1.7(6) . . . . ?
C2 C3 C4 C11 -179.0(4) . . . . ?
C3 C4 C5 C6 -1.5(6) . . . . ?
C11 C4 C5 C6 179.1(4) . . . . ?
C4 C5 C6 C1 0.7(6) . . . . ?
C4 C5 C6 C7 -179.7(4) . . . . ?
O2 C1 C6 C5 179.4(4) . . . . ?
C2 C1 C6 C5 0.0(6) . . . . ?
O2 C1 C6 C7 -0.2(6) . . . . ?
C2 C1 C6 C7 -179.6(4) . . . . ?
C5 C6 C7 C8 1.8(6) . . . . ?
C1 C6 C7 C8 -178.6(4) . . . . ?
C5 C6 C7 C10 120.9(4) . . . . ?
C1 C6 C7 C10 -59.5(5) . . . . ?
C5 C6 C7 C9 -118.3(4) . . . . ?
C1 C6 C7 C9 61.3(5) . . . . ?
C3 C4 C11 C13 -111.9(4) . . . . ?
C5 C4 C11 C13 67.4(5) . . . . ?
C3 C4 C11 C14 127.6(4) . . . . ?
C5 C4 C11 C14 -53.1(5) . . . . ?
C3 C4 C11 C12 9.3(6) . . . . ?
C5 C4 C11 C12 -171.4(4) . . . . ?
C16 N1 C15 C2 -59.4(4) . . . . ?
V1 N1 C15 C2 68.4(4) . . . . ?
C3 C2 C15 N1 128.5(4) . . . . ?
C1 C2 C15 N1 -51.9(5) . . . . ?
C15 N1 C16 C17 176.8(3) . . . . ?
V1 N1 C16 C17 51.5(4) . . . . ?
N1 C16 C17 C18 132.4(4) . . . . ?
N1 C16 C17 C22 -52.2(5) . . . . ?
C22 C17 C18 C19 -1.0(6) . . . . ?
C16 C17 C18 C19 174.4(4) . . . . ?
C17 C18 C19 C20 -1.4(6) . . . . ?
C17 C18 C19 C23 -179.9(4) . . . . ?
C18 C19 C20 C21 1.9(6) . . . . ?
C23 C19 C20 C21 -179.5(4) . . . . ?
C19 C20 C21 C22 -0.1(6) . . . . ?
C19 C20 C21 C27 -178.3(4) . . . . ?
V1 O4 C22 C17 47.9(6) . . . . ?
V1 O4 C22 C21 -134.7(3) . . . . ?
C18 C17 C22 O4 -179.6(4) . . . . ?
C16 C17 C22 O4 4.9(6) . . . . ?
C18 C17 C22 C21 3.0(6) . . . . ?
C16 C17 C22 C21 -172.4(4) . . . . ?
C20 C21 C22 O4 -179.8(4) . . . . ?
C27 C21 C22 O4 -1.6(6) . . . . ?
C20 C21 C22 C17 -2.5(6) . . . . ?
C27 C21 C22 C17 175.8(4) . . . . ?
C18 C19 C23 C24 114.1(5) . . . . ?
C20 C19 C23 C24 -64.3(5) . . . . ?
C18 C19 C23 C25 -125.7(4) . . . . ?
C20 C19 C23 C25 55.8(5) . . . . ?
C18 C19 C23 C26 -6.4(6) . . . . ?
C20 C19 C23 C26 175.1(4) . . . . ?
C20 C21 C27 C28 -0.6(6) . . . . ?
C22 C21 C27 C28 -178.8(4) . . . . ?
C20 C21 C27 C29 -120.6(4) . . . . ?
C22 C21 C27 C29 61.3(5) . . . . ?
C20 C21 C27 C30 118.4(4) . . . . ?
C22 C21 C27 C30 -59.7(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O3 0.74(4) 2.48(4) 3.118(5) 145(4) 3_556

_diffrn_measured_fraction_theta_max 0.881
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1413244'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H90 N2 O7 V2'
_chemical_formula_sum            'C60 H90 N2 O7 V2'
_chemical_formula_weight         1053.22

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           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn
_symmetry_space_group_name_Hall  -P2n2ab

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

_cell_length_a                   24.9968(16)
_cell_length_b                   11.8900(8)
_cell_length_c                   19.5013(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5796.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41562
_cell_measurement_theta_min      4.481
_cell_measurement_theta_max      48.502

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8804
_exptl_absorpt_correction_T_max  0.9324
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22722
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.51
_reflns_number_total             5365
_reflns_number_gt                3408
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_cell_refinement       
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_reduction        
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_solution    
'XS V2008/1 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_refinement  
'XL V2008/4 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1249P)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     SHELXL
_refine_ls_extinction_coef       0.031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5365
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0851
_refine_ls_wR_factor_ref         0.2319
_refine_ls_wR_factor_gt          0.1938
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_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 0.99024(3) 0.31235(5) 0.15973(4) 0.0321(3) Uani 1 1 d . . .
O1 O 0.92088(11) 0.2661(2) 0.17096(15) 0.0386(7) Uani 1 1 d . . .
N1 N 0.96150(14) 0.3452(3) 0.0578(2) 0.0350(8) Uani 1 1 d . . .
H1N H 0.9884(17) 0.352(3) 0.034(2) 0.023(10) Uiso 1 1 d . . .
C1 C 0.87927(16) 0.2220(3) 0.1345(2) 0.0346(9) Uani 1 1 d . . .
O2 O 1.02913(11) 0.4393(2) 0.13511(15) 0.0342(7) Uani 1 1 d . . .
C2 C 0.83332(18) 0.1826(3) 0.1690(2) 0.0379(10) Uani 1 1 d . . .
O3 O 1.02587(13) 0.2090(2) 0.13668(16) 0.0395(7) Uani 1 1 d . . .
C3 C 0.79298(18) 0.1363(4) 0.1276(3) 0.0417(11) Uani 1 1 d . . .
H3 H 0.761(2) 0.105(4) 0.147(2) 0.041(12) Uiso 1 1 d . . .
O4 O 1.0000 0.3300(3) 0.2500 0.0381(10) Uani 1 2 d S . .
C4 C 0.79585(16) 0.1273(4) 0.0567(2) 0.0393(10) Uani 1 1 d . . .
C5 C 0.84124(18) 0.1707(3) 0.0262(3) 0.0388(10) Uani 1 1 d . . .
H5 H 0.8456(18) 0.168(3) -0.022(3) 0.036(12) Uiso 1 1 d . . .
C6 C 0.88278(16) 0.2161(3) 0.0632(2) 0.0342(10) Uani 1 1 d . . .
C7 C 0.75147(18) 0.0720(4) 0.0143(3) 0.0471(12) Uani 1 1 d . . .
C8 C 0.7148(3) -0.0005(7) 0.0590(4) 0.096(2) Uani 1 1 d . . .
H8A H 0.6909 -0.0425 0.0302 0.144 Uiso 1 1 calc R . .
H8B H 0.6945 0.0469 0.0891 0.144 Uiso 1 1 calc R . .
H8C H 0.7361 -0.0516 0.0857 0.144 Uiso 1 1 calc R . .
C9 C 0.7747(2) -0.0039(6) -0.0393(4) 0.081(2) Uani 1 1 d . . .
H9A H 0.7473 -0.0531 -0.0564 0.122 Uiso 1 1 calc R . .
H9B H 0.8030 -0.0478 -0.0196 0.122 Uiso 1 1 calc R . .
H9C H 0.7886 0.0406 -0.0763 0.122 Uiso 1 1 calc R . .
C10 C 0.7186(3) 0.1619(5) -0.0198(4) 0.086(2) Uani 1 1 d . . .
H10A H 0.7410 0.2052 -0.0498 0.129 Uiso 1 1 calc R . .
H10B H 0.7034 0.2102 0.0145 0.129 Uiso 1 1 calc R . .
H10C H 0.6904 0.1275 -0.0458 0.129 Uiso 1 1 calc R . .
C11 C 0.8290(2) 0.1847(4) 0.2476(3) 0.0484(12) Uani 1 1 d . . .
C12 C 0.8708(2) 0.1042(5) 0.2776(3) 0.0591(14) Uani 1 1 d . . .
H12A H 0.8687 0.1056 0.3268 0.089 Uiso 1 1 calc R . .
H12B H 0.9059 0.1274 0.2634 0.089 Uiso 1 1 calc R . .
H12C H 0.8640 0.0293 0.2615 0.089 Uiso 1 1 calc R . .
C13 C 0.8372(3) 0.3024(4) 0.2749(3) 0.0658(16) Uani 1 1 d . . .
H13A H 0.8125 0.3528 0.2530 0.099 Uiso 1 1 calc R . .
H13B H 0.8732 0.3263 0.2654 0.099 Uiso 1 1 calc R . .
H13C H 0.8313 0.3030 0.3235 0.099 Uiso 1 1 calc R . .
C14 C 0.7738(2) 0.1449(5) 0.2720(3) 0.0629(15) Uani 1 1 d . . .
H14A H 0.7467 0.1934 0.2535 0.094 Uiso 1 1 calc R . .
H14B H 0.7724 0.1472 0.3211 0.094 Uiso 1 1 calc R . .
H14C H 0.7677 0.0693 0.2566 0.094 Uiso 1 1 calc R . .
C15 C 0.93291(16) 0.2501(3) 0.0261(2) 0.0363(10) Uani 1 1 d . . .
H15A H 0.9568 0.1859 0.0241 0.044 Uiso 1 1 calc R . .
H15B H 0.9237 0.2701 -0.0207 0.044 Uiso 1 1 calc R . .
C16 C 0.93067(16) 0.4500(3) 0.0566(2) 0.0369(10) Uani 1 1 d . . .
H16A H 0.8989 0.4404 0.0846 0.044 Uiso 1 1 calc R . .
H16B H 0.9190 0.4642 0.0100 0.044 Uiso 1 1 calc R . .
C17 C 0.96115(16) 0.5509(3) 0.0821(2) 0.0331(9) Uani 1 1 d . . .
C18 C 0.93813(17) 0.6559(4) 0.0709(2) 0.0363(10) Uani 1 1 d . . .
H18 H 0.9033(17) 0.654(3) 0.046(2) 0.027(10) Uiso 1 1 d . . .
C19 C 0.96068(16) 0.7540(3) 0.0968(2) 0.0354(10) Uani 1 1 d . . .
C20 C 1.00976(17) 0.7432(3) 0.1306(2) 0.0365(10) Uani 1 1 d . . .
H20 H 1.0272(19) 0.815(3) 0.146(2) 0.032(11) Uiso 1 1 d . . .
C21 C 1.03553(16) 0.6402(3) 0.1413(2) 0.0320(9) Uani 1 1 d . . .
C22 C 1.00867(16) 0.5424(3) 0.1198(2) 0.0323(9) Uani 1 1 d . . .
C23 C 0.93177(18) 0.8669(4) 0.0890(2) 0.0407(11) Uani 1 1 d . . .
C24 C 0.9611(2) 0.9619(4) 0.1259(3) 0.0528(13) Uani 1 1 d . . .
H24A H 0.9414 1.0307 0.1206 0.079 Uiso 1 1 calc R . .
H24B H 0.9962 0.9707 0.1065 0.079 Uiso 1 1 calc R . .
H24C H 0.9642 0.9441 0.1738 0.079 Uiso 1 1 calc R . .
C25 C 0.9263(2) 0.8971(4) 0.0124(3) 0.0525(13) Uani 1 1 d . . .
H25A H 0.9077 0.8379 -0.0111 0.079 Uiso 1 1 calc R . .
H25B H 0.9613 0.9061 -0.0073 0.079 Uiso 1 1 calc R . .
H25C H 0.9067 0.9661 0.0078 0.079 Uiso 1 1 calc R . .
C26 C 0.87532(19) 0.8588(4) 0.1196(3) 0.0471(12) Uani 1 1 d . . .
H26A H 0.8557 0.8007 0.0966 0.071 Uiso 1 1 calc R . .
H26B H 0.8572 0.9294 0.1140 0.071 Uiso 1 1 calc R . .
H26C H 0.8778 0.8412 0.1676 0.071 Uiso 1 1 calc R . .
C27 C 1.09054(16) 0.6352(3) 0.1775(2) 0.0352(10) Uani 1 1 d . . .
C28 C 1.08437(18) 0.5774(4) 0.2470(2) 0.0388(10) Uani 1 1 d . . .
H28A H 1.1188 0.5703 0.2683 0.058 Uiso 1 1 calc R . .
H28B H 1.0691 0.5040 0.2405 0.058 Uiso 1 1 calc R . .
H28C H 1.0613 0.6214 0.2757 0.058 Uiso 1 1 calc R . .
C29 C 1.13103(16) 0.5698(3) 0.1327(2) 0.0353(10) Uani 1 1 d . . .
H29A H 1.1363 0.6090 0.0902 0.053 Uiso 1 1 calc R . .
H29B H 1.1174 0.4958 0.1236 0.053 Uiso 1 1 calc R . .
H29C H 1.1645 0.5640 0.1565 0.053 Uiso 1 1 calc R . .
C30 C 1.11367(17) 0.7527(4) 0.1891(2) 0.0416(11) Uani 1 1 d . . .
H30A H 1.1157 0.7918 0.1462 0.062 Uiso 1 1 calc R . .
H30B H 1.1489 0.7463 0.2085 0.062 Uiso 1 1 calc R . .
H30C H 1.0910 0.7936 0.2201 0.062 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 O3 1.583(3) . ?
V1 O4 1.7896(9) . ?
V1 O1 1.832(3) . ?
V1 O2 1.859(3) . ?
V1 N1 2.149(4) . ?
O1 C1 1.365(5) . ?
N1 C16 1.464(5) . ?
N1 C15 1.475(5) . ?
N1 H1N 0.82(4) . ?
C1 C6 1.395(6) . ?
C1 C2 1.411(6) . ?
O2 C22 1.361(5) . ?
C2 C3 1.404(6) . ?
C2 C11 1.536(7) . ?
C3 C4 1.390(7) . ?
C3 H3 0.96(5) . ?
O4 V1 1.7896(9) 4_755 ?
C4 C5 1.381(6) . ?
C4 C7 1.531(6) . ?
C5 C6 1.375(6) . ?
C5 H5 0.95(5) . ?
C6 C15 1.503(6) . ?
C7 C9 1.499(8) . ?
C7 C10 1.503(7) . ?
C7 C8 1.529(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.512(6) . ?
C11 C12 1.534(7) . ?
C11 C14 1.534(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.506(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.391(6) . ?
C17 C22 1.401(6) . ?
C18 C19 1.390(6) . ?
C18 H18 0.99(4) . ?
C19 C20 1.399(6) . ?
C19 C23 1.532(6) . ?
C20 C21 1.399(6) . ?
C20 H20 1.01(4) . ?
C21 C22 1.406(6) . ?
C21 C27 1.547(6) . ?
C23 C24 1.527(7) . ?
C23 C26 1.535(6) . ?
C23 C25 1.543(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.527(6) . ?
C27 C30 1.528(6) . ?
C27 C29 1.547(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 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
O3 V1 O4 107.06(16) . . ?
O3 V1 O1 109.46(15) . . ?
O4 V1 O1 92.66(10) . . ?
O3 V1 O2 105.25(15) . . ?
O4 V1 O2 95.03(14) . . ?
O1 V1 O2 140.34(13) . . ?
O3 V1 N1 93.84(15) . . ?
O4 V1 N1 159.06(15) . . ?
O1 V1 N1 81.31(14) . . ?
O2 V1 N1 77.77(13) . . ?
C1 O1 V1 140.7(3) . . ?
C16 N1 C15 113.0(3) . . ?
C16 N1 V1 110.2(3) . . ?
C15 N1 V1 114.3(3) . . ?
C16 N1 H1N 110(3) . . ?
C15 N1 H1N 104(3) . . ?
V1 N1 H1N 105(3) . . ?
O1 C1 C6 119.4(4) . . ?
O1 C1 C2 120.0(4) . . ?
C6 C1 C2 120.7(4) . . ?
C22 O2 V1 126.3(2) . . ?
C3 C2 C1 116.1(4) . . ?
C3 C2 C11 121.9(4) . . ?
C1 C2 C11 121.9(4) . . ?
C4 C3 C2 124.4(4) . . ?
C4 C3 H3 114(3) . . ?
C2 C3 H3 122(3) . . ?
V1 O4 V1 166.6(3) . 4_755 ?
C5 C4 C3 116.2(4) . . ?
C5 C4 C7 121.6(4) . . ?
C3 C4 C7 122.2(4) . . ?
C6 C5 C4 122.8(5) . . ?
C6 C5 H5 117(3) . . ?
C4 C5 H5 121(3) . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C15 118.9(4) . . ?
C1 C6 C15 121.3(4) . . ?
C9 C7 C10 109.3(6) . . ?
C9 C7 C8 106.8(5) . . ?
C10 C7 C8 109.0(5) . . ?
C9 C7 C4 110.8(4) . . ?
C10 C7 C4 109.2(4) . . ?
C8 C7 C4 111.7(5) . . ?
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 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 110.5(5) . . ?
C13 C11 C14 107.4(4) . . ?
C12 C11 C14 107.6(4) . . ?
C13 C11 C2 110.9(4) . . ?
C12 C11 C2 108.8(4) . . ?
C14 C11 C2 111.6(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C6 114.1(4) . . ?
N1 C15 H15A 108.7 . . ?
C6 C15 H15A 108.7 . . ?
N1 C15 H15B 108.7 . . ?
C6 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N1 C16 C17 114.0(3) . . ?
N1 C16 H16A 108.8 . . ?
C17 C16 H16A 108.8 . . ?
N1 C16 H16B 108.8 . . ?
C17 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C18 C17 C22 119.8(4) . . ?
C18 C17 C16 117.0(4) . . ?
C22 C17 C16 123.0(4) . . ?
C19 C18 C17 121.9(4) . . ?
C19 C18 H18 124(2) . . ?
C17 C18 H18 114(2) . . ?
C18 C19 C20 116.7(4) . . ?
C18 C19 C23 120.6(4) . . ?
C20 C19 C23 122.8(4) . . ?
C19 C20 C21 123.7(4) . . ?
C19 C20 H20 116(3) . . ?
C21 C20 H20 120(3) . . ?
C20 C21 C22 117.4(4) . . ?
C20 C21 C27 120.7(4) . . ?
C22 C21 C27 121.9(4) . . ?
O2 C22 C17 119.9(4) . . ?
O2 C22 C21 120.0(4) . . ?
C17 C22 C21 120.1(4) . . ?
C24 C23 C19 112.0(4) . . ?
C24 C23 C26 107.7(4) . . ?
C19 C23 C26 109.9(4) . . ?
C24 C23 C25 109.1(4) . . ?
C19 C23 C25 109.9(4) . . ?
C26 C23 C25 108.1(4) . . ?
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 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C30 108.6(4) . . ?
C28 C27 C29 109.9(4) . . ?
C30 C27 C29 107.2(3) . . ?
C28 C27 C21 109.5(3) . . ?
C30 C27 C21 111.7(4) . . ?
C29 C27 C21 110.0(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
O3 V1 O1 C1 -62.5(5) . . . . ?
O4 V1 O1 C1 -171.7(4) . . . . ?
O2 V1 O1 C1 87.2(5) . . . . ?
N1 V1 O1 C1 28.5(4) . . . . ?
O3 V1 N1 C16 -172.6(3) . . . . ?
O4 V1 N1 C16 3.8(5) . . . . ?
O1 V1 N1 C16 78.3(3) . . . . ?
O2 V1 N1 C16 -67.8(3) . . . . ?
O3 V1 N1 C15 58.9(3) . . . . ?
O4 V1 N1 C15 -124.7(4) . . . . ?
O1 V1 N1 C15 -50.2(3) . . . . ?
O2 V1 N1 C15 163.7(3) . . . . ?
V1 O1 C1 C6 -9.6(7) . . . . ?
V1 O1 C1 C2 170.2(3) . . . . ?
O3 V1 O2 C22 152.9(3) . . . . ?
O4 V1 O2 C22 -97.8(3) . . . . ?
O1 V1 O2 C22 2.5(4) . . . . ?
N1 V1 O2 C22 62.2(3) . . . . ?
O1 C1 C2 C3 -178.7(4) . . . . ?
C6 C1 C2 C3 1.2(6) . . . . ?
O1 C1 C2 C11 -1.7(6) . . . . ?
C6 C1 C2 C11 178.2(4) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C11 C2 C3 C4 -176.8(4) . . . . ?
O3 V1 O4 V1 -38.59(13) . . . 4_755 ?
O1 V1 O4 V1 72.71(10) . . . 4_755 ?
O2 V1 O4 V1 -146.24(9) . . . 4_755 ?
N1 V1 O4 V1 145.1(4) . . . 4_755 ?
C2 C3 C4 C5 -2.1(6) . . . . ?
C2 C3 C4 C7 177.7(4) . . . . ?
C3 C4 C5 C6 2.8(6) . . . . ?
C7 C4 C5 C6 -176.9(4) . . . . ?
C4 C5 C6 C1 -1.6(6) . . . . ?
C4 C5 C6 C15 173.6(4) . . . . ?
O1 C1 C6 C5 179.3(4) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
O1 C1 C6 C15 4.2(6) . . . . ?
C2 C1 C6 C15 -175.6(4) . . . . ?
C5 C4 C7 C9 43.4(7) . . . . ?
C3 C4 C7 C9 -136.4(5) . . . . ?
C5 C4 C7 C10 -77.1(6) . . . . ?
C3 C4 C7 C10 103.2(6) . . . . ?
C5 C4 C7 C8 162.3(5) . . . . ?
C3 C4 C7 C8 -17.4(7) . . . . ?
C3 C2 C11 C13 -126.8(5) . . . . ?
C1 C2 C11 C13 56.4(6) . . . . ?
C3 C2 C11 C12 111.5(5) . . . . ?
C1 C2 C11 C12 -65.3(5) . . . . ?
C3 C2 C11 C14 -7.1(6) . . . . ?
C1 C2 C11 C14 176.1(4) . . . . ?
C16 N1 C15 C6 -64.5(5) . . . . ?
V1 N1 C15 C6 62.6(4) . . . . ?
C5 C6 C15 N1 149.7(4) . . . . ?
C1 C6 C15 N1 -35.1(5) . . . . ?
C15 N1 C16 C17 -174.0(4) . . . . ?
V1 N1 C16 C17 56.8(4) . . . . ?
N1 C16 C17 C18 168.7(4) . . . . ?
N1 C16 C17 C22 -15.9(6) . . . . ?
C22 C17 C18 C19 -0.6(6) . . . . ?
C16 C17 C18 C19 175.1(4) . . . . ?
C17 C18 C19 C20 4.2(6) . . . . ?
C17 C18 C19 C23 -174.6(4) . . . . ?
C18 C19 C20 C21 -2.1(6) . . . . ?
C23 C19 C20 C21 176.7(4) . . . . ?
C19 C20 C21 C22 -3.7(6) . . . . ?
C19 C20 C21 C27 178.4(4) . . . . ?
V1 O2 C22 C17 -38.9(5) . . . . ?
V1 O2 C22 C21 141.8(3) . . . . ?
C18 C17 C22 O2 175.1(4) . . . . ?
C16 C17 C22 O2 -0.2(6) . . . . ?
C18 C17 C22 C21 -5.5(6) . . . . ?
C16 C17 C22 C21 179.1(4) . . . . ?
C20 C21 C22 O2 -173.2(4) . . . . ?
C27 C21 C22 O2 4.7(6) . . . . ?
C20 C21 C22 C17 7.5(6) . . . . ?
C27 C21 C22 C17 -174.6(4) . . . . ?
C18 C19 C23 C24 175.3(4) . . . . ?
C20 C19 C23 C24 -3.4(6) . . . . ?
C18 C19 C23 C26 55.6(5) . . . . ?
C20 C19 C23 C26 -123.1(5) . . . . ?
C18 C19 C23 C25 -63.2(5) . . . . ?
C20 C19 C23 C25 118.0(5) . . . . ?
C20 C21 C27 C28 112.4(4) . . . . ?
C22 C21 C27 C28 -65.4(5) . . . . ?
C20 C21 C27 C30 -7.8(5) . . . . ?
C22 C21 C27 C30 174.3(4) . . . . ?
C20 C21 C27 C29 -126.7(4) . . . . ?
C22 C21 C27 C29 55.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.51
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.208
