# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_pa-zba
_database_code_depnum_ccdc_archive 'CCDC 1541544'
_audit_update_record             
;
2017-03-31 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H112 N4 O25 V6'
_chemical_formula_weight         1643.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.733(3)
_cell_length_b                   17.259(4)
_cell_length_c                   16.297(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.51(3)
_cell_angle_gamma                90
_cell_volume                     3770.9(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8656
_cell_measurement_theta_min      2.308
_cell_measurement_theta_max      29.677

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             1724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.790
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25611
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.741
_diffrn_reflns_theta_max         24.846
_diffrn_reflns_theta_full        24.846
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6444
_reflns_number_gt                3103
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0914P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6444
_refine_ls_number_parameters     448
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1939
_refine_ls_wR_factor_gt          0.1507
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.989
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.0000 0.0000 0.5000 0.0444(13) Uani 1 2 d S . P . .
C1 C 0.0080(4) 0.0303(4) 0.2521(4) 0.0555(16) Uani 1 1 d . . . . .
N1 N -0.2043(5) 0.2971(4) 0.0957(4) 0.097(2) Uani 1 1 d . . . . .
H1A H -0.2681 0.2949 0.0894 0.116 Uiso 1 1 calc R U . . .
V1 V 0.12724(7) 0.06004(6) 0.46152(6) 0.0545(3) Uani 1 1 d . . . . .
V2 V -0.00042(8) -0.10206(6) 0.41329(7) 0.0570(3) Uani 1 1 d . . . . .
O2 O 0.1025(3) -0.0302(2) 0.3819(2) 0.0514(10) Uani 1 1 d . . . . .
C2 C 0.0101(5) 0.1092(4) 0.2937(4) 0.0611(17) Uani 1 1 d . . . . .
H2A H 0.0703 0.1363 0.2882 0.073 Uiso 1 1 calc R U . . .
H2B H -0.0465 0.1394 0.2645 0.073 Uiso 1 1 calc R U . . .
N2 N -0.4417(4) 0.1899(3) 0.3777(3) 0.0582(13) Uani 1 1 d . . . . .
V3 V -0.11666(7) 0.06613(7) 0.41180(7) 0.0579(3) Uani 1 1 d . . . . .
O3 O -0.0936(3) -0.0278(2) 0.3421(2) 0.0550(10) Uani 1 1 d . . . . .
C3 C 0.1000(4) -0.0162(4) 0.2941(4) 0.0594(17) Uani 1 1 d . . . . .
H3A H 0.0999 -0.0654 0.2653 0.071 Uiso 1 1 calc R U . . .
H3B H 0.1596 0.0119 0.2890 0.071 Uiso 1 1 calc R U . . .
O4 O 0.0073(3) 0.1041(2) 0.3810(2) 0.0530(10) Uani 1 1 d . . . . .
C4 C -0.0860(5) -0.0146(4) 0.2558(4) 0.0649(18) Uani 1 1 d . . . . .
H4A H -0.1438 0.0141 0.2266 0.078 Uiso 1 1 calc R U . . .
H4B H -0.0851 -0.0640 0.2276 0.078 Uiso 1 1 calc R U . . .
O5 O 0.0977(3) -0.1337(2) 0.5025(2) 0.0608(11) Uani 1 1 d . . . . .
C5 C 0.0174(5) 0.0400(5) 0.1596(4) 0.078(2) Uani 1 1 d . . . . .
H5A H 0.0718 0.0749 0.1564 0.093 Uiso 1 1 calc R U . . .
H5B H 0.0306 -0.0097 0.1364 0.093 Uiso 1 1 calc R U . . .
O6 O -0.1976(3) 0.0029(2) 0.4590(2) 0.0561(11) Uani 1 1 d . . . . .
C6 C -0.0782(7) 0.0917(5) 0.0333(5) 0.085(2) Uani 1 1 d . . . . .
O7 O 0.2100(3) 0.1024(3) 0.4221(3) 0.0663(12) Uani 1 1 d . . . . .
C7 C -0.1800(6) 0.1148(4) -0.0113(4) 0.0692(19) Uani 1 1 d . . . . .
O8 O -0.1010(3) -0.1316(2) 0.4609(2) 0.0594(11) Uani 1 1 d . . . . .
C8 C -0.2316(8) 0.0637(5) -0.0684(5) 0.095(3) Uani 1 1 d . . . . .
H8A H -0.2020 0.0176 -0.0797 0.114 Uiso 1 1 calc R U . . .
O9 O -0.1931(3) 0.1093(3) 0.3383(3) 0.0752(13) Uani 1 1 d . . . . .
C9 C -0.3294(8) 0.0812(6) -0.1099(5) 0.106(3) Uani 1 1 d . . . . .
H9A H -0.3652 0.0465 -0.1487 0.128 Uiso 1 1 calc R U . . .
O10 O 0.0004(4) -0.1658(3) 0.3423(3) 0.0765(13) Uani 1 1 d . . . . .
C10 C -0.3725(7) 0.1500(6) -0.0932(5) 0.102(3) Uani 1 1 d . . . . .
H10A H -0.4380 0.1609 -0.1199 0.122 Uiso 1 1 calc R U . . .
O11 O -0.0755(3) 0.0712(3) 0.1135(3) 0.0844(15) Uani 1 1 d . . . . .
C11 C -0.3196(6) 0.2027(5) -0.0372(5) 0.084(2) Uani 1 1 d . . . . .
H11A H -0.3489 0.2494 -0.0275 0.100 Uiso 1 1 calc R U . . .
O12 O -0.0070(4) 0.0854(3) 0.0003(3) 0.1055(19) Uani 1 1 d . . . . .
C12 C -0.2225(6) 0.1859(5) 0.0047(4) 0.073(2) Uani 1 1 d . . . . .
C13 C -0.1591(6) 0.2418(5) 0.0621(5) 0.077(2) Uani 1 1 d . . . . .
O13 O -0.0663(4) 0.2380(4) 0.0747(4) 0.113(2) Uani 1 1 d . . . . .
C14 C -0.1510(7) 0.3620(5) 0.1434(6) 0.120(3) Uani 1 1 d D U . . .
H14A H -0.0946 0.3745 0.1188 0.144 Uiso 1 1 calc R U . . .
H14B H -0.1952 0.4065 0.1346 0.144 Uiso 1 1 calc R U . . .
C15 C -0.1141(14) 0.3537(10) 0.2322(6) 0.278(12) Uani 1 1 d D U . . .
H15A H -0.1023 0.4053 0.2560 0.333 Uiso 1 1 calc R U . . .
H15B H -0.0499 0.3280 0.2408 0.333 Uiso 1 1 calc R U . . .
C16 C -0.1741(12) 0.3123(10) 0.2800(8) 0.270(10) Uani 1 1 d D U . . .
H16A H -0.1405 0.3113 0.3381 0.404 Uiso 1 1 calc R U . . .
H16B H -0.2373 0.3379 0.2745 0.404 Uiso 1 1 calc R U . . .
H16C H -0.1846 0.2603 0.2593 0.404 Uiso 1 1 calc R U . . .
C21 C -0.4034(5) 0.1868(4) 0.2965(4) 0.0653(18) Uani 1 1 d . . . . .
H21A H -0.4280 0.2322 0.2634 0.078 Uiso 1 1 calc R U . . .
H21B H -0.3312 0.1906 0.3112 0.078 Uiso 1 1 calc R U . . .
C22 C -0.4299(5) 0.1179(5) 0.2426(4) 0.077(2) Uani 1 1 d . . . . .
H22A H -0.5019 0.1133 0.2264 0.092 Uiso 1 1 calc R U . . .
H22B H -0.4041 0.0718 0.2739 0.092 Uiso 1 1 calc R U . . .
C23 C -0.3864(6) 0.1237(5) 0.1630(4) 0.087(2) Uani 1 1 d . . . . .
H23A H -0.4192 0.1658 0.1282 0.105 Uiso 1 1 calc R U . . .
H23B H -0.3160 0.1361 0.1795 0.105 Uiso 1 1 calc R U . . .
C24 C -0.3986(8) 0.0517(6) 0.1129(5) 0.122(3) Uani 1 1 d . . . . .
H24A H -0.3704 0.0586 0.0644 0.183 Uiso 1 1 calc R U . . .
H24B H -0.3650 0.0100 0.1465 0.183 Uiso 1 1 calc R U . . .
H24C H -0.4683 0.0397 0.0952 0.183 Uiso 1 1 calc R U . . .
C31 C -0.3990(5) 0.1213(4) 0.4321(4) 0.0682(19) Uani 1 1 d . . . . .
H31A H -0.3270 0.1224 0.4397 0.082 Uiso 1 1 calc R U . . .
H31B H -0.4224 0.0742 0.4018 0.082 Uiso 1 1 calc R U . . .
C32 C -0.4241(5) 0.1170(4) 0.5186(4) 0.075(2) Uani 1 1 d . . . . .
H32A H -0.4086 0.1661 0.5473 0.090 Uiso 1 1 calc R U . . .
H32B H -0.4949 0.1074 0.5123 0.090 Uiso 1 1 calc R U . . .
C33 C -0.3658(6) 0.0531(5) 0.5704(4) 0.083(2) Uani 1 1 d . . . . .
H33A H -0.3763 0.0052 0.5386 0.100 Uiso 1 1 calc R U . . .
H33B H -0.2952 0.0654 0.5803 0.100 Uiso 1 1 calc R U . . .
C34 C -0.3938(6) 0.0408(5) 0.6530(4) 0.095(3) Uani 1 1 d . . . . .
H34A H -0.3542 -0.0003 0.6828 0.142 Uiso 1 1 calc R U . . .
H34B H -0.3820 0.0876 0.6856 0.142 Uiso 1 1 calc R U . . .
H34C H -0.4631 0.0274 0.6438 0.142 Uiso 1 1 calc R U . . .
C41 C -0.5538(5) 0.1846(4) 0.3608(4) 0.0690(19) Uani 1 1 d . U . . .
H41A H -0.5736 0.1343 0.3363 0.083 Uiso 1 1 calc R U . . .
H41B H -0.5741 0.1871 0.4141 0.083 Uiso 1 1 calc R U . . .
C42 C -0.6094(5) 0.2453(5) 0.3042(4) 0.084(2) Uani 1 1 d . U . . .
H42A H -0.5774 0.2543 0.2575 0.101 Uiso 1 1 calc R U . . .
H42B H -0.6089 0.2935 0.3349 0.101 Uiso 1 1 calc R U . . .
C43 C -0.7162(6) 0.2190(7) 0.2712(6) 0.134(4) Uani 1 1 d . U . . .
H43A H -0.7147 0.1681 0.2463 0.160 Uiso 1 1 calc R U . . .
H43B H -0.7478 0.2134 0.3186 0.160 Uiso 1 1 calc R U . . .
C44 C -0.7748(8) 0.2659(9) 0.2133(6) 0.193(6) Uani 1 1 d . U . . .
H44A H -0.8403 0.2439 0.1969 0.289 Uiso 1 1 calc R U . . .
H44B H -0.7792 0.3162 0.2375 0.289 Uiso 1 1 calc R U . . .
H44C H -0.7460 0.2707 0.1649 0.289 Uiso 1 1 calc R U . . .
C51 C -0.4084(5) 0.2660(4) 0.4218(4) 0.0723(19) Uani 1 1 d . . . . .
H51A H -0.4292 0.3080 0.3822 0.087 Uiso 1 1 calc R U . . .
H51B H -0.4428 0.2726 0.4674 0.087 Uiso 1 1 calc R U . . .
C52 C -0.2988(5) 0.2735(5) 0.4566(5) 0.093(2) Uani 1 1 d . . . . .
H52A H -0.2786 0.2349 0.5002 0.111 Uiso 1 1 calc R U . . .
H52B H -0.2635 0.2628 0.4124 0.111 Uiso 1 1 calc R U . . .
C53 C -0.2695(7) 0.3512(6) 0.4922(7) 0.123(3) Uani 1 1 d . . . . .
H53A H -0.3041 0.3615 0.5370 0.147 Uiso 1 1 calc R U . . .
H53B H -0.2906 0.3898 0.4488 0.147 Uiso 1 1 calc R U . . .
C54 C -0.1592(8) 0.3591(7) 0.5262(7) 0.160(5) Uani 1 1 d . . . . .
H54A H -0.1447 0.4104 0.5483 0.240 Uiso 1 1 calc R U . . .
H54B H -0.1379 0.3218 0.5702 0.240 Uiso 1 1 calc R U . . .
H54C H -0.1244 0.3502 0.4819 0.240 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 V3 2.2219(12) 3_556 ?
O1 V3 2.2220(12) . ?
O1 V1 2.2349(11) . ?
O1 V1 2.2350(11) 3_556 ?
O1 V2 2.2574(10) . ?
O1 V2 2.2575(10) 3_556 ?
C1 C4 1.518(8) . ?
C1 C2 1.518(9) . ?
C1 C3 1.528(8) . ?
C1 C5 1.551(8) . ?
N1 C13 1.320(9) . ?
N1 C14 1.467(10) . ?
V1 O7 1.598(4) . ?
V1 O6 1.803(4) 3_556 ?
V1 O8 1.857(4) 3_556 ?
V1 O2 2.009(4) . ?
V1 O4 2.019(4) . ?
V1 V3 3.0256(16) 3_556 ?
V1 V2 3.0433(16) 3_556 ?
V2 O10 1.598(4) . ?
V2 O8 1.799(4) . ?
V2 O5 1.838(4) . ?
V2 O3 1.996(4) . ?
V2 O2 2.028(4) . ?
V2 V3 3.0181(18) 3_556 ?
V2 V1 3.0433(16) 3_556 ?
O2 C3 1.443(6) . ?
C2 O4 1.435(6) . ?
N2 C41 1.507(8) . ?
N2 C31 1.518(7) . ?
N2 C51 1.520(8) . ?
N2 C21 1.526(7) . ?
V3 O9 1.596(4) . ?
V3 O5 1.795(4) 3_556 ?
V3 O6 1.840(4) . ?
V3 O4 1.988(4) . ?
V3 O3 2.044(4) . ?
V3 V2 3.0182(18) 3_556 ?
V3 V1 3.0257(16) 3_556 ?
O3 C4 1.450(7) . ?
O5 V3 1.795(4) 3_556 ?
C5 O11 1.437(7) . ?
O6 V1 1.803(4) 3_556 ?
C6 O12 1.218(8) . ?
C6 O11 1.347(8) . ?
C6 C7 1.484(10) . ?
C7 C8 1.363(10) . ?
C7 C12 1.408(9) . ?
O8 V1 1.857(4) 3_556 ?
C8 C9 1.399(12) . ?
C9 C10 1.380(12) . ?
C10 C11 1.378(10) . ?
C11 C12 1.392(9) . ?
C12 C13 1.487(10) . ?
C13 O13 1.247(8) . ?
C14 C15 1.432(8) . ?
C15 C16 1.441(9) . ?
C21 C22 1.475(9) . ?
C22 C23 1.544(9) . ?
C23 C24 1.477(11) . ?
C31 C32 1.524(8) . ?
C32 C33 1.509(9) . ?
C33 C34 1.493(9) . ?
C41 C42 1.492(8) . ?
C42 C43 1.518(11) . ?
C43 C44 1.365(12) . ?
C51 C52 1.494(9) . ?
C52 C53 1.481(11) . ?
C53 C54 1.503(12) . ?

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
V3 O1 V3 180.0 3_556 . ?
V3 O1 V1 85.51(4) 3_556 . ?
V3 O1 V1 94.49(4) . . ?
V3 O1 V1 94.49(4) 3_556 3_556 ?
V3 O1 V1 85.51(4) . 3_556 ?
V1 O1 V1 180.0 . 3_556 ?
V3 O1 V2 84.72(4) 3_556 . ?
V3 O1 V2 95.28(4) . . ?
V1 O1 V2 94.72(4) . . ?
V1 O1 V2 85.28(4) 3_556 . ?
V3 O1 V2 95.29(4) 3_556 3_556 ?
V3 O1 V2 84.72(4) . 3_556 ?
V1 O1 V2 85.29(4) . 3_556 ?
V1 O1 V2 94.72(4) 3_556 3_556 ?
V2 O1 V2 180.0 . 3_556 ?
C4 C1 C2 112.1(5) . . ?
C4 C1 C3 109.9(5) . . ?
C2 C1 C3 109.7(5) . . ?
C4 C1 C5 110.1(5) . . ?
C2 C1 C5 109.9(5) . . ?
C3 C1 C5 104.9(5) . . ?
C13 N1 C14 123.1(8) . . ?
O7 V1 O6 104.4(2) . 3_556 ?
O7 V1 O8 103.2(2) . 3_556 ?
O6 V1 O8 93.67(18) 3_556 3_556 ?
O7 V1 O2 97.51(19) . . ?
O6 V1 O2 89.23(17) 3_556 . ?
O8 V1 O2 157.64(17) 3_556 . ?
O7 V1 O4 96.73(19) . . ?
O6 V1 O4 158.24(17) 3_556 . ?
O8 V1 O4 86.62(17) 3_556 . ?
O2 V1 O4 82.65(16) . . ?
O7 V1 O1 172.75(16) . . ?
O6 V1 O1 81.29(12) 3_556 . ?
O8 V1 O1 80.71(13) 3_556 . ?
O2 V1 O1 77.82(11) . . ?
O4 V1 O1 77.29(11) . . ?
O7 V1 V3 138.33(16) . 3_556 ?
O6 V1 V3 34.24(12) 3_556 3_556 ?
O8 V1 V3 88.22(13) 3_556 3_556 ?
O2 V1 V3 81.76(11) . 3_556 ?
O4 V1 V3 124.17(11) . 3_556 ?
O1 V1 V3 47.06(3) . 3_556 ?
O7 V1 V2 136.06(16) . 3_556 ?
O6 V1 V2 87.53(12) 3_556 3_556 ?
O8 V1 V2 33.05(12) 3_556 3_556 ?
O2 V1 V2 125.23(11) . 3_556 ?
O4 V1 V2 80.88(11) . 3_556 ?
O1 V1 V2 47.67(3) . 3_556 ?
V3 V1 V2 66.11(4) 3_556 3_556 ?
O10 V2 O8 104.1(2) . . ?
O10 V2 O5 104.4(2) . . ?
O8 V2 O5 94.31(19) . . ?
O10 V2 O3 97.2(2) . . ?
O8 V2 O3 88.68(17) . . ?
O5 V2 O3 156.72(17) . . ?
O10 V2 O2 97.1(2) . . ?
O8 V2 O2 157.64(17) . . ?
O5 V2 O2 87.10(17) . . ?
O3 V2 O2 81.65(16) . . ?
O10 V2 O1 172.19(17) . . ?
O8 V2 O1 81.30(13) . . ?
O5 V2 O1 80.49(12) . . ?
O3 V2 O1 77.15(11) . . ?
O2 V2 O1 76.92(11) . . ?
O10 V2 V3 137.67(18) . 3_556 ?
O8 V2 V3 87.27(13) . 3_556 ?
O5 V2 V3 33.37(12) . 3_556 ?
O3 V2 V3 124.11(12) . 3_556 ?
O2 V2 V3 81.67(11) . 3_556 ?
O1 V2 V3 47.14(3) . 3_556 ?
O10 V2 V1 138.08(17) . 3_556 ?
O8 V2 V1 34.26(12) . 3_556 ?
O5 V2 V1 88.22(12) . 3_556 ?
O3 V2 V1 81.31(11) . 3_556 ?
O2 V2 V1 123.72(11) . 3_556 ?
O1 V2 V1 47.05(3) . 3_556 ?
V3 V2 V1 65.35(4) 3_556 3_556 ?
C3 O2 V1 118.3(4) . . ?
C3 O2 V2 119.0(3) . . ?
V1 O2 V2 109.89(17) . . ?
O4 C2 C1 112.6(5) . . ?
C41 N2 C31 108.0(5) . . ?
C41 N2 C51 109.2(5) . . ?
C31 N2 C51 111.0(5) . . ?
C41 N2 C21 111.7(5) . . ?
C31 N2 C21 108.5(5) . . ?
C51 N2 C21 108.4(5) . . ?
O9 V3 O5 104.0(2) . 3_556 ?
O9 V3 O6 103.4(2) . . ?
O5 V3 O6 93.36(18) 3_556 . ?
O9 V3 O4 96.7(2) . . ?
O5 V3 O4 89.73(18) 3_556 . ?
O6 V3 O4 158.27(17) . . ?
O9 V3 O3 96.3(2) . . ?
O5 V3 O3 159.15(17) 3_556 . ?
O6 V3 O3 86.68(17) . . ?
O4 V3 O3 82.92(16) . . ?
O9 V3 O1 171.93(16) . . ?
O5 V3 O1 82.39(13) 3_556 . ?
O6 V3 O1 80.87(12) . . ?
O4 V3 O1 78.23(11) . . ?
O3 V3 O1 77.02(11) . . ?
O9 V3 V2 137.91(18) . 3_556 ?
O5 V3 V2 34.28(12) 3_556 3_556 ?
O6 V3 V2 88.49(12) . 3_556 ?
O4 V3 V2 82.01(12) . 3_556 ?
O3 V3 V2 124.98(11) . 3_556 ?
O1 V3 V2 48.14(3) . 3_556 ?
O9 V3 V1 136.66(17) . 3_556 ?
O5 V3 V1 87.51(13) 3_556 3_556 ?
O6 V3 V1 33.45(12) . 3_556 ?
O4 V3 V1 125.47(12) . 3_556 ?
O3 V3 V1 81.06(11) . 3_556 ?
O1 V3 V1 47.42(3) . 3_556 ?
V2 V3 V1 66.29(4) 3_556 3_556 ?
C4 O3 V2 119.5(3) . . ?
C4 O3 V3 117.8(4) . . ?
V2 O3 V3 110.05(17) . . ?
O2 C3 C1 111.8(5) . . ?
C2 O4 V3 118.7(3) . . ?
C2 O4 V1 118.3(3) . . ?
V3 O4 V1 109.51(18) . . ?
O3 C4 C1 111.1(5) . . ?
V3 O5 V2 112.3(2) 3_556 . ?
O11 C5 C1 107.3(5) . . ?
V1 O6 V3 112.31(19) 3_556 . ?
O12 C6 O11 123.2(8) . . ?
O12 C6 C7 124.7(7) . . ?
O11 C6 C7 111.8(6) . . ?
C8 C7 C12 121.1(8) . . ?
C8 C7 C6 117.1(8) . . ?
C12 C7 C6 121.8(7) . . ?
V2 O8 V1 112.7(2) . 3_556 ?
C7 C8 C9 119.5(9) . . ?
C10 C9 C8 119.8(9) . . ?
C11 C10 C9 120.8(9) . . ?
C6 O11 C5 116.2(6) . . ?
C10 C11 C12 119.9(8) . . ?
C11 C12 C7 118.8(7) . . ?
C11 C12 C13 122.8(7) . . ?
C7 C12 C13 118.3(7) . . ?
O13 C13 N1 121.7(8) . . ?
O13 C13 C12 120.5(8) . . ?
N1 C13 C12 117.7(7) . . ?
C15 C14 N1 119.0(10) . . ?
C14 C15 C16 118.5(13) . . ?
C22 C21 N2 117.2(5) . . ?
C21 C22 C23 111.0(6) . . ?
C24 C23 C22 113.0(7) . . ?
N2 C31 C32 116.3(5) . . ?
C33 C32 C31 110.8(5) . . ?
C34 C33 C32 113.5(6) . . ?
C42 C41 N2 115.9(5) . . ?
C41 C42 C43 109.6(6) . . ?
C44 C43 C42 116.5(9) . . ?
C52 C51 N2 115.4(6) . . ?
C53 C52 C51 113.1(7) . . ?
C52 C53 C54 113.2(8) . . ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.075

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_4931
_database_code_depnum_ccdc_archive 'CCDC 1569404'
_audit_update_record             
;
2017-08-17 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_audit_creation_date             2017-05-03
_audit_creation_method           
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C38 H36 N2 O25 V6, C32 H72 N2'
_chemical_formula_sum            'C70 H108 N4 O25 V6'
_chemical_formula_weight         1711.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   12.0059(8)
_cell_length_b                   13.8979(12)
_cell_length_c                   14.0548(7)
_cell_angle_alpha                66.339(6)
_cell_angle_beta                 78.031(5)
_cell_angle_gamma                67.630(7)
_cell_volume                     1982.2(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4396
_cell_measurement_temperature    107.2
_cell_measurement_theta_max      29.3056
_cell_measurement_theta_min      2.9921
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14862
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.00
_diffrn_ambient_temperature      107.2
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -40.00  -15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046   77.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -72.00  -45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -37.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega   -5.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   60.0000 89

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  -42.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
  8 omega   -4.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000  -30.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0119413000
_diffrn_orient_matrix_UB_12      -0.0491072000
_diffrn_orient_matrix_UB_13      0.0085117000
_diffrn_orient_matrix_UB_21      -0.0626384000
_diffrn_orient_matrix_UB_22      0.0305079000
_diffrn_orient_matrix_UB_23      -0.0030383000
_diffrn_orient_matrix_UB_31      0.0057564000
_diffrn_orient_matrix_UB_32      0.0119824000
_diffrn_orient_matrix_UB_33      -0.0544683000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6740
_reflns_number_total             7776
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7776
_refine_ls_number_restraints     564
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0673
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+11.1045P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1614
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.69342(7) 0.39489(7) 0.02895(6) 0.01798(19) Uani 1 1 d . . .
V2 V 0.44548(7) 0.36434(6) -0.00384(6) 0.01809(19) Uani 1 1 d . . .
V3 V 0.53416(7) 0.57247(6) -0.17349(6) 0.01736(18) Uani 1 1 d . . .
O4 O 0.6237(3) 0.3524(3) 0.1657(2) 0.0200(7) Uani 1 1 d . . .
O8 O 0.6237(3) 0.2908(3) 0.0079(2) 0.0185(7) Uani 1 1 d . . .
O1 O 0.5000 0.5000 0.0000 0.0153(9) Uani 1 2 d S . .
O3 O 0.5773(3) 0.6659(3) -0.1335(2) 0.0209(7) Uani 1 1 d . . .
O10 O 0.4981(3) 0.4376(3) -0.1552(2) 0.0182(7) Uani 1 1 d . . .
O2 O 0.7021(3) 0.5178(3) 0.0335(2) 0.0201(7) Uani 1 1 d . . .
O9 O 0.6992(3) 0.4584(3) -0.1261(2) 0.0171(6) Uani 1 1 d . . .
O7 O 0.4191(3) 0.2668(3) -0.0202(3) 0.0259(8) Uani 1 1 d . . .
O5 O 0.8292(3) 0.3098(3) 0.0416(3) 0.0247(7) Uani 1 1 d . . .
O11 O 0.7812(3) 0.2967(3) -0.3448(2) 0.0237(7) Uani 1 1 d . . .
O6 O 0.5721(3) 0.6065(3) -0.2956(2) 0.0238(7) Uani 1 1 d . . .
C4 C 0.6996(4) 0.3051(4) -0.1724(3) 0.0189(9) Uani 1 1 d . . .
O13 O 0.8618(4) 0.1564(3) -0.5184(3) 0.0417(10) Uani 1 1 d . . .
O12 O 0.6534(4) 0.2313(3) -0.3786(3) 0.0390(10) Uani 1 1 d . . .
C13 C 0.7975(5) 0.2241(4) -0.5896(4) 0.0269(11) Uani 1 1 d . . .
C6 C 0.7133(5) 0.2905(4) -0.4073(4) 0.0261(11) Uani 1 1 d . . .
C7 C 0.7177(4) 0.3754(4) -0.5150(4) 0.0243(10) Uani 1 1 d . . .
N1 N 0.7684(4) 0.1987(3) -0.6640(3) 0.0248(9) Uani 1 1 d . . .
H1 H 0.7214 0.2531 -0.7098 0.030 Uiso 1 1 calc R . .
C10 C 0.7065(5) 0.5401(4) -0.7119(4) 0.0294(11) Uani 1 1 d . . .
H10 H 0.7036 0.5949 -0.7778 0.035 Uiso 1 1 calc R . .
C2 C 0.7628(4) 0.3870(4) -0.1836(4) 0.0195(9) Uani 1 1 d . . .
H2A H 0.8436 0.3453 -0.1596 0.023 Uiso 1 1 calc R . .
H2B H 0.7702 0.4320 -0.2566 0.023 Uiso 1 1 calc R . .
C11 C 0.7421(4) 0.4296(4) -0.7021(4) 0.0262(11) Uani 1 1 d . . .
H11 H 0.7624 0.4108 -0.7615 0.031 Uiso 1 1 calc R . .
C1 C 0.6924(4) 0.2291(4) -0.0573(3) 0.0215(10) Uani 1 1 d . . .
H1A H 0.6559 0.1754 -0.0514 0.026 Uiso 1 1 calc R . .
H1B H 0.7734 0.1883 -0.0336 0.026 Uiso 1 1 calc R . .
C12 C 0.7479(4) 0.3450(4) -0.6029(4) 0.0240(10) Uani 1 1 d . . .
C15 C 0.9013(5) 0.0026(4) -0.6221(4) 0.0275(11) Uani 1 1 d . . .
H15 H 0.9415 0.0084 -0.5758 0.033 Uiso 1 1 calc R . .
C16 C 0.9354(5) -0.0972(5) -0.6391(5) 0.0374(14) Uani 1 1 d . . .
H16 H 0.9992 -0.1576 -0.6045 0.045 Uiso 1 1 calc R . .
C3 C 0.5717(4) 0.3677(4) -0.2116(4) 0.0191(9) Uani 1 1 d . . .
H3A H 0.5769 0.4126 -0.2848 0.023 Uiso 1 1 calc R . .
H3B H 0.5344 0.3141 -0.2046 0.023 Uiso 1 1 calc R . .
C9 C 0.6754(5) 0.5696(5) -0.6249(4) 0.0340(12) Uani 1 1 d . . .
H9 H 0.6507 0.6441 -0.6320 0.041 Uiso 1 1 calc R . .
C5 C 0.7740(4) 0.2305(4) -0.2351(4) 0.0234(10) Uani 1 1 d . . .
H5A H 0.8547 0.1910 -0.2105 0.028 Uiso 1 1 calc R . .
H5B H 0.7368 0.1759 -0.2250 0.028 Uiso 1 1 calc R . .
C14 C 0.8072(4) 0.0929(4) -0.6741(4) 0.0249(11) Uani 1 1 d . . .
C8 C 0.6813(5) 0.4865(5) -0.5251(4) 0.0313(12) Uani 1 1 d . . .
H8 H 0.6608 0.5060 -0.4661 0.038 Uiso 1 1 calc R . .
C19 C 0.7474(5) 0.0835(4) -0.7440(4) 0.0330(12) Uani 1 1 d . . .
H19 H 0.6839 0.1440 -0.7789 0.040 Uiso 1 1 calc R . .
C18 C 0.7826(6) -0.0154(5) -0.7611(5) 0.0402(14) Uani 1 1 d . . .
H18 H 0.7439 -0.0205 -0.8090 0.048 Uiso 1 1 calc R . .
C17 C 0.8752(6) -0.1073(5) -0.7075(5) 0.0401(14) Uani 1 1 d . . .
H17 H 0.8966 -0.1747 -0.7171 0.048 Uiso 1 1 calc R . .
C20 C 0.9302(11) 0.8285(13) -0.1990(10) 0.034(3) Uani 0.50 1 d PDU A -1
H20A H 1.0152 0.7857 -0.2033 0.041 Uiso 0.50 1 calc PR A -1
H20B H 0.9167 0.8992 -0.2565 0.041 Uiso 0.50 1 calc PR A -1
N2 N 0.8574(7) 0.7665(7) -0.2123(7) 0.0321(18) Uani 0.50 1 d PDU A -1
C24 C 0.7243(9) 0.8349(9) -0.2115(10) 0.038(2) Uani 0.50 1 d PDU A -1
H24A H 0.6982 0.8373 -0.1421 0.045 Uiso 0.50 1 calc PR A -1
H24B H 0.6800 0.7963 -0.2245 0.045 Uiso 0.50 1 calc PR A -1
C21 C 0.9015(11) 0.8508(10) -0.0984(9) 0.035(2) Uani 0.50 1 d PDU A -1
H21A H 0.9257 0.7807 -0.0406 0.043 Uiso 0.50 1 calc PR A -1
H21B H 0.8150 0.8857 -0.0892 0.043 Uiso 0.50 1 calc PR A -1
C22 C 0.9657(10) 0.9256(8) -0.0979(8) 0.035(2) Uani 0.50 1 d PDU A -1
H22A H 1.0516 0.8929 -0.1121 0.042 Uiso 0.50 1 calc PR A -1
H22B H 0.9375 0.9972 -0.1532 0.042 Uiso 0.50 1 calc PR A -1
C32 C 0.8716(9) 0.6569(8) -0.1207(9) 0.036(2) Uani 0.50 1 d PDU A -1
H32A H 0.8439 0.6730 -0.0571 0.043 Uiso 0.50 1 calc PR A -1
H32B H 0.8197 0.6217 -0.1284 0.043 Uiso 0.50 1 calc PR A -1
C23 C 0.9450(12) 0.9431(11) 0.0045(10) 0.048(3) Uani 0.50 1 d PDU A -1
H23A H 0.9817 0.9957 -0.0008 0.072 Uiso 0.50 1 calc PR A -1
H23B H 0.9803 0.8735 0.0584 0.072 Uiso 0.50 1 calc PR A -1
H23C H 0.8599 0.9712 0.0210 0.072 Uiso 0.50 1 calc PR A -1
C35 C 0.9924(14) 0.4983(15) 0.0876(10) 0.059(4) Uani 0.50 1 d PDU A -1
H35A H 0.9150 0.5543 0.0887 0.089 Uiso 0.50 1 calc PR A -1
H35B H 1.0546 0.5254 0.0883 0.089 Uiso 0.50 1 calc PR A -1
H35C H 0.9958 0.4322 0.1477 0.089 Uiso 0.50 1 calc PR A -1
C28 C 0.9047(14) 0.7472(14) -0.3142(10) 0.046(3) Uani 0.50 1 d PDU A -1
H28A H 0.9914 0.7107 -0.3124 0.055 Uiso 0.50 1 calc PR A -1
H28B H 0.8902 0.8193 -0.3699 0.055 Uiso 0.50 1 calc PR A -1
C30 C 0.929(2) 0.6426(18) -0.4298(15) 0.093(6) Uani 0.50 1 d PDU A -1
H30A H 0.9355 0.7086 -0.4882 0.111 Uiso 0.50 1 calc PR A -1
H30B H 1.0099 0.5974 -0.4067 0.111 Uiso 0.50 1 calc PR A -1
C29 C 0.8517(17) 0.6785(18) -0.3418(14) 0.073(4) Uani 0.50 1 d PDU A -1
H29A H 0.8484 0.6133 -0.2813 0.088 Uiso 0.50 1 calc PR A -1
H29B H 0.7701 0.7225 -0.3630 0.088 Uiso 0.50 1 calc PR A -1
C47 C 1.1620(15) 0.3598(14) 0.4425(13) 0.067(4) Uani 0.50 1 d PDU B -1
H47A H 1.2221 0.3950 0.4101 0.101 Uiso 0.50 1 calc PR B -1
H47B H 1.2008 0.2812 0.4760 0.101 Uiso 0.50 1 calc PR B -1
H47C H 1.1130 0.3907 0.4934 0.101 Uiso 0.50 1 calc PR B -1
C25 C 0.6891(11) 0.9536(10) -0.2888(11) 0.047(3) Uani 0.50 1 d PDU A -1
H25A H 0.7059 0.9536 -0.3594 0.056 Uiso 0.50 1 calc PR A -1
H25B H 0.7352 0.9933 -0.2800 0.056 Uiso 0.50 1 calc PR A -1
C27 C 0.5212(15) 1.0360(14) -0.1687(14) 0.056(4) Uani 0.50 1 d PDU A -1
H27A H 0.5646 1.0818 -0.1695 0.084 Uiso 0.50 1 calc PR A -1
H27B H 0.5421 0.9676 -0.1100 0.084 Uiso 0.50 1 calc PR A -1
H27C H 0.4360 1.0746 -0.1636 0.084 Uiso 0.50 1 calc PR A -1
C26 C 0.5544(11) 1.0104(14) -0.2693(12) 0.054(4) Uani 0.50 1 d PDU A -1
H26A H 0.5112 0.9629 -0.2670 0.065 Uiso 0.50 1 calc PR A -1
H26B H 0.5273 1.0796 -0.3276 0.065 Uiso 0.50 1 calc PR A -1
N3 N 1.2733(9) 0.1135(8) 0.2919(7) 0.041(2) Uani 0.50 1 d PDU B -1
C40 C 1.1713(11) 0.0829(10) 0.2763(9) 0.045(3) Uani 0.50 1 d PDU B -1
H40A H 1.1082 0.0924 0.3307 0.054 Uiso 0.50 1 calc PR B -1
H40B H 1.2016 0.0046 0.2853 0.054 Uiso 0.50 1 calc PR B -1
C36 C 1.3750(11) 0.1049(9) 0.2078(9) 0.042(3) Uani 0.50 1 d PDU B -1
H36A H 1.3402 0.1448 0.1406 0.050 Uiso 0.50 1 calc PR B -1
H36B H 1.4268 0.1423 0.2113 0.050 Uiso 0.50 1 calc PR B -1
C48 C 1.3204(11) 0.0359(11) 0.3986(9) 0.047(3) Uani 0.50 1 d PDU B -1
H48A H 1.3392 -0.0397 0.4019 0.057 Uiso 0.50 1 calc PR B -1
H48B H 1.2540 0.0485 0.4498 0.057 Uiso 0.50 1 calc PR B -1
C44 C 1.2287(12) 0.2315(10) 0.2888(10) 0.049(3) Uani 0.50 1 d PDU B -1
H44A H 1.2147 0.2809 0.2172 0.059 Uiso 0.50 1 calc PR B -1
H44B H 1.2924 0.2438 0.3102 0.059 Uiso 0.50 1 calc PR B -1
C43 C 1.1161(15) 0.1613(14) -0.0151(11) 0.074(5) Uani 0.50 1 d PDU B -1
H43A H 1.1256 0.1153 -0.0541 0.111 Uiso 0.50 1 calc PR B -1
H43B H 1.1672 0.2063 -0.0472 0.111 Uiso 0.50 1 calc PR B -1
H43C H 1.0335 0.2085 -0.0139 0.111 Uiso 0.50 1 calc PR B -1
C50 C 1.4974(16) -0.0724(15) 0.5148(13) 0.101(6) Uani 0.50 1 d PDU B -1
H50A H 1.4430 -0.0856 0.5765 0.121 Uiso 0.50 1 calc PR B -1
H50B H 1.5645 -0.0629 0.5341 0.121 Uiso 0.50 1 calc PR B -1
C42 C 1.1510(18) 0.0883(14) 0.0951(11) 0.068(4) Uani 0.50 1 d PDU B -1
H42A H 1.2378 0.0519 0.0940 0.081 Uiso 0.50 1 calc PR B -1
H42B H 1.1140 0.0306 0.1204 0.081 Uiso 0.50 1 calc PR B -1
C49 C 1.4300(13) 0.0403(15) 0.4344(12) 0.077(4) Uani 0.50 1 d PDU B -1
H49A H 1.4035 0.0974 0.4651 0.092 Uiso 0.50 1 calc PR B -1
H49B H 1.4849 0.0605 0.3746 0.092 Uiso 0.50 1 calc PR B -1
C45 C 1.1151(16) 0.2646(13) 0.3551(15) 0.064(5) Uani 0.50 1 d PDU B -1
H45A H 1.1237 0.2090 0.4248 0.077 Uiso 0.50 1 calc PR B -1
H45B H 1.0480 0.2645 0.3268 0.077 Uiso 0.50 1 calc PR B -1
C46 C 1.0847(17) 0.3789(12) 0.3623(14) 0.067(4) Uani 0.50 1 d PDU B -1
H46A H 1.1027 0.4314 0.2958 0.081 Uiso 0.50 1 calc PR B -1
H46B H 0.9999 0.4078 0.3829 0.081 Uiso 0.50 1 calc PR B -1
C41 C 1.1147(16) 0.1492(14) 0.1711(12) 0.056(4) Uani 0.50 1 d PDU B -1
H41A H 1.0276 0.1718 0.1834 0.067 Uiso 0.50 1 calc PR B -1
H41B H 1.1364 0.2164 0.1387 0.067 Uiso 0.50 1 calc PR B -1
C39 C 1.6294(12) -0.1269(10) 0.1336(12) 0.054(3) Uani 0.50 1 d PDU B -1
H39A H 1.6841 -0.1257 0.0730 0.082 Uiso 0.50 1 calc PR B -1
H39B H 1.5868 -0.1770 0.1449 0.082 Uiso 0.50 1 calc PR B -1
H39C H 1.6741 -0.1514 0.1931 0.082 Uiso 0.50 1 calc PR B -1
C34 C 1.0108(13) 0.4714(9) -0.0105(10) 0.046(3) Uani 0.50 1 d PDU A -1
H34A H 0.9514 0.4388 -0.0084 0.055 Uiso 0.50 1 calc PR A -1
H34B H 1.0902 0.4168 -0.0125 0.055 Uiso 0.50 1 calc PR A -1
C51 C 1.549(2) -0.1815(18) 0.4902(12) 0.170(14) Uani 0.50 1 d PDU B -1
H51A H 1.6091 -0.1744 0.4333 0.255 Uiso 0.50 1 calc PR B -1
H51B H 1.4848 -0.1946 0.4715 0.255 Uiso 0.50 1 calc PR B -1
H51C H 1.5846 -0.2429 0.5504 0.255 Uiso 0.50 1 calc PR B -1
C33 C 0.9995(9) 0.5751(10) -0.1096(9) 0.038(3) Uani 0.50 1 d PDU A -1
H33A H 1.0532 0.6118 -0.1082 0.045 Uiso 0.50 1 calc PR A -1
H33B H 1.0247 0.5524 -0.1697 0.045 Uiso 0.50 1 calc PR A -1
C37 C 1.4527(12) -0.0122(10) 0.2129(11) 0.038(3) Uani 0.50 1 d PDU B -1
H37A H 1.4013 -0.0538 0.2178 0.045 Uiso 0.50 1 calc PR B -1
H37B H 1.4978 -0.0497 0.2749 0.045 Uiso 0.50 1 calc PR B -1
C38 C 1.5400(12) -0.0109(10) 0.1176(9) 0.041(3) Uani 0.50 1 d PDU B -1
H38A H 1.4957 0.0147 0.0568 0.049 Uiso 0.50 1 calc PR B -1
H38B H 1.5827 0.0401 0.1059 0.049 Uiso 0.50 1 calc PR B -1
C31 C 0.884(2) 0.578(2) -0.4669(18) 0.112(9) Uani 0.50 1 d PDU A -1
H31A H 0.9322 0.5667 -0.5274 0.168 Uiso 0.50 1 calc PR A -1
H31B H 0.8014 0.6192 -0.4841 0.168 Uiso 0.50 1 calc PR A -1
H31C H 0.8887 0.5075 -0.4129 0.168 Uiso 0.50 1 calc PR A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V2 3.0251(12) 2_665 ?
V1 V3 3.0483(11) 2_665 ?
V1 O4 1.882(3) . ?
V1 O8 2.062(3) . ?
V1 O1 2.2415(8) . ?
V1 O2 1.777(3) . ?
V1 O9 1.993(3) . ?
V1 O5 1.604(3) . ?
V2 V1 3.0251(12) 2_665 ?
V2 V3 3.0356(11) 2_665 ?
V2 O8 1.999(3) . ?
V2 O1 2.2409(8) . ?
V2 O3 1.788(3) 2_665 ?
V2 O10 2.038(3) . ?
V2 O2 1.883(3) 2_665 ?
V2 O7 1.612(3) . ?
V3 V1 3.0483(11) 2_665 ?
V3 V2 3.0356(11) 2_665 ?
V3 O4 1.787(3) 2_665 ?
V3 O1 2.2487(8) . ?
V3 O3 1.867(3) . ?
V3 O10 1.988(3) . ?
V3 O9 2.048(3) . ?
V3 O6 1.601(3) . ?
O4 V3 1.787(3) 2_665 ?
O8 C1 1.425(5) . ?
O1 V1 2.2415(8) 2_665 ?
O1 V2 2.2409(8) 2_665 ?
O1 V3 2.2487(8) 2_665 ?
O3 V2 1.788(3) 2_665 ?
O10 C3 1.424(5) . ?
O2 V2 1.883(3) 2_665 ?
O9 C2 1.426(5) . ?
O11 C6 1.362(6) . ?
O11 C5 1.448(6) . ?
C4 C2 1.536(6) . ?
C4 C1 1.543(6) . ?
C4 C3 1.539(6) . ?
C4 C5 1.533(6) . ?
O13 C13 1.222(6) . ?
O12 C6 1.191(6) . ?
C13 N1 1.372(6) . ?
C13 C12 1.498(7) . ?
C6 C7 1.506(7) . ?
C7 C12 1.397(7) . ?
C7 C8 1.390(7) . ?
N1 H1 0.8600 . ?
N1 C14 1.421(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.385(7) . ?
C10 C9 1.379(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.412(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C15 H15 0.9300 . ?
C15 C16 1.392(8) . ?
C15 C14 1.383(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.394(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C9 H9 0.9300 . ?
C9 C8 1.409(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C14 C19 1.402(7) . ?
C8 H8 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.381(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.389(8) . ?
C17 H17 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 N2 1.522(11) . ?
C20 C21 1.509(12) . ?
N2 C24 1.517(10) . ?
N2 C32 1.525(10) . ?
N2 C28 1.516(11) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.517(11) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.515(11) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.510(11) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.518(11) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C35 C34 1.522(12) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.527(12) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C29 1.520(13) . ?
C30 C31 1.494(13) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C47 C46 1.486(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.527(12) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 C26 1.532(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
N3 C40 1.521(11) . ?
N3 C36 1.519(11) . ?
N3 C48 1.523(11) . ?
N3 C44 1.504(11) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.531(12) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.517(12) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.534(12) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.510(12) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C43 C42 1.513(13) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 C49 1.543(13) . ?
C50 C51 1.556(14) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C41 1.516(13) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.529(12) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C39 C38 1.514(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.534(11) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.518(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 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
V2 V1 V3 66.00(3) 2_665 2_665 ?
O4 V1 V2 88.86(10) . 2_665 ?
O4 V1 V3 32.83(9) . 2_665 ?
O4 V1 O8 85.46(13) . . ?
O4 V1 O1 80.11(10) . . ?
O4 V1 O9 157.34(13) . . ?
O8 V1 V2 124.34(9) . 2_665 ?
O8 V1 V3 81.10(9) . 2_665 ?
O8 V1 O1 77.00(9) . . ?
O1 V1 V2 47.55(2) . 2_665 ?
O1 V1 V3 47.34(2) . 2_665 ?
O2 V1 V2 35.40(10) . 2_665 ?
O2 V1 V3 87.11(11) . 2_665 ?
O2 V1 O4 93.56(14) . . ?
O2 V1 O8 159.71(14) . . ?
O2 V1 O1 82.87(10) . . ?
O2 V1 O9 90.99(14) . . ?
O9 V1 V2 82.07(9) . 2_665 ?
O9 V1 V3 125.59(9) . 2_665 ?
O9 V1 O8 82.67(12) . . ?
O9 V1 O1 78.45(9) . . ?
O5 V1 V2 139.48(13) . 2_665 ?
O5 V1 V3 135.12(13) . 2_665 ?
O5 V1 O4 102.44(16) . . ?
O5 V1 O8 95.55(15) . . ?
O5 V1 O1 171.99(13) . . ?
O5 V1 O2 104.43(16) . . ?
O5 V1 O9 97.87(15) . . ?
V1 V2 V3 65.91(3) 2_665 2_665 ?
O8 V2 V1 125.61(10) . 2_665 ?
O8 V2 V3 82.37(9) . 2_665 ?
O8 V2 O1 78.27(9) . . ?
O8 V2 O10 82.10(12) . . ?
O1 V2 V1 47.57(2) . 2_665 ?
O1 V2 V3 47.56(2) . 2_665 ?
O3 V2 V1 86.90(11) 2_665 2_665 ?
O3 V2 V3 34.69(10) 2_665 2_665 ?
O3 V2 O8 90.73(14) 2_665 . ?
O3 V2 O1 82.20(10) 2_665 . ?
O3 V2 O10 158.63(14) 2_665 . ?
O3 V2 O2 94.11(14) 2_665 2_665 ?
O10 V2 V1 81.13(9) . 2_665 ?
O10 V2 V3 124.01(9) . 2_665 ?
O10 V2 O1 76.64(9) . . ?
O2 V2 V1 33.14(10) 2_665 2_665 ?
O2 V2 V3 89.18(10) 2_665 2_665 ?
O2 V2 O8 157.49(14) 2_665 . ?
O2 V2 O1 80.63(10) 2_665 . ?
O2 V2 O10 85.51(13) 2_665 . ?
O7 V2 V1 135.61(13) . 2_665 ?
O7 V2 V3 138.88(13) . 2_665 ?
O7 V2 O8 97.44(16) . . ?
O7 V2 O1 172.18(13) . . ?
O7 V2 O3 104.52(16) . 2_665 ?
O7 V2 O10 96.39(15) . . ?
O7 V2 O2 102.57(16) . 2_665 ?
V2 V3 V1 65.87(3) 2_665 2_665 ?
O4 V3 V1 34.81(10) 2_665 2_665 ?
O4 V3 V2 86.84(10) 2_665 2_665 ?
O4 V3 O1 81.90(10) 2_665 . ?
O4 V3 O3 93.65(15) 2_665 . ?
O4 V3 O10 90.21(14) 2_665 . ?
O4 V3 O9 158.92(14) 2_665 . ?
O1 V3 V1 47.15(2) . 2_665 ?
O1 V3 V2 47.35(2) . 2_665 ?
O3 V3 V1 88.85(10) . 2_665 ?
O3 V3 V2 33.03(10) . 2_665 ?
O3 V3 O1 80.33(10) . . ?
O3 V3 O10 156.66(14) . . ?
O3 V3 O9 85.48(13) . . ?
O10 V3 V1 81.26(9) . 2_665 ?
O10 V3 V2 124.58(9) . 2_665 ?
O10 V3 O1 77.44(9) . . ?
O10 V3 O9 82.75(12) . . ?
O9 V3 V1 124.15(9) . 2_665 ?
O9 V3 V2 80.99(9) . 2_665 ?
O9 V3 O1 77.19(9) . . ?
O6 V3 V1 139.15(13) . 2_665 ?
O6 V3 V2 136.67(13) . 2_665 ?
O6 V3 O4 104.82(16) . 2_665 ?
O6 V3 O1 171.70(13) . . ?
O6 V3 O3 103.79(16) . . ?
O6 V3 O10 97.42(15) . . ?
O6 V3 O9 95.81(15) . . ?
V3 O4 V1 112.36(16) 2_665 . ?
V2 O8 V1 109.08(14) . . ?
C1 O8 V1 118.0(3) . . ?
C1 O8 V2 119.7(3) . . ?
V1 O1 V1 180.0 2_665 . ?
V1 O1 V3 85.51(3) 2_665 . ?
V1 O1 V3 94.49(3) . . ?
V1 O1 V3 94.49(3) 2_665 2_665 ?
V1 O1 V3 85.51(3) . 2_665 ?
V2 O1 V1 95.11(3) 2_665 2_665 ?
V2 O1 V1 95.11(3) . . ?
V2 O1 V1 84.89(3) . 2_665 ?
V2 O1 V1 84.89(3) 2_665 . ?
V2 O1 V2 180.00(4) . 2_665 ?
V2 O1 V3 94.91(3) 2_665 2_665 ?
V2 O1 V3 94.91(3) . . ?
V2 O1 V3 85.09(3) 2_665 . ?
V2 O1 V3 85.09(3) . 2_665 ?
V3 O1 V3 180.00(4) . 2_665 ?
V2 O3 V3 112.29(16) 2_665 . ?
V3 O10 V2 110.47(15) . . ?
C3 O10 V2 118.3(3) . . ?
C3 O10 V3 119.2(3) . . ?
V1 O2 V2 111.45(16) . 2_665 ?
V1 O9 V3 109.35(14) . . ?
C2 O9 V1 119.4(3) . . ?
C2 O9 V3 117.8(3) . . ?
C6 O11 C5 116.8(4) . . ?
C2 C4 C1 109.8(4) . . ?
C2 C4 C3 111.0(4) . . ?
C3 C4 C1 109.6(4) . . ?
C5 C4 C2 109.3(4) . . ?
C5 C4 C1 107.7(4) . . ?
C5 C4 C3 109.5(4) . . ?
O13 C13 N1 124.5(5) . . ?
O13 C13 C12 120.5(5) . . ?
N1 C13 C12 115.0(4) . . ?
O11 C6 C7 109.9(4) . . ?
O12 C6 O11 124.6(5) . . ?
O12 C6 C7 125.3(5) . . ?
C12 C7 C6 121.2(4) . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 C12 120.7(5) . . ?
C13 N1 H1 116.3 . . ?
C13 N1 C14 127.4(4) . . ?
C14 N1 H1 116.3 . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.5(5) . . ?
O9 C2 C4 112.5(4) . . ?
O9 C2 H2A 109.1 . . ?
O9 C2 H2B 109.1 . . ?
C4 C2 H2A 109.1 . . ?
C4 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.7(5) . . ?
C12 C11 H11 119.7 . . ?
O8 C1 C4 112.1(4) . . ?
O8 C1 H1A 109.2 . . ?
O8 C1 H1B 109.2 . . ?
C4 C1 H1A 109.2 . . ?
C4 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C7 C12 C13 119.4(4) . . ?
C7 C12 C11 118.5(5) . . ?
C11 C12 C13 121.8(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(5) . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.7(5) . . ?
C17 C16 H16 119.6 . . ?
O10 C3 C4 111.8(4) . . ?
O10 C3 H3A 109.2 . . ?
O10 C3 H3B 109.2 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C10 C9 H9 120.1 . . ?
C10 C9 C8 119.8(5) . . ?
C8 C9 H9 120.1 . . ?
O11 C5 C4 110.4(4) . . ?
O11 C5 H5A 109.6 . . ?
O11 C5 H5B 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C15 C14 N1 123.7(5) . . ?
C15 C14 C19 119.7(5) . . ?
C19 C14 N1 116.5(4) . . ?
C7 C8 C9 119.8(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C14 C19 H19 119.9 . . ?
C18 C19 C14 120.1(5) . . ?
C18 C19 H19 119.9 . . ?
C19 C18 H18 119.7 . . ?
C19 C18 C17 120.6(6) . . ?
C17 C18 H18 119.7 . . ?
C16 C17 H17 120.5 . . ?
C18 C17 C16 119.1(5) . . ?
C18 C17 H17 120.5 . . ?
H20A C20 H20B 107.5 . . ?
N2 C20 H20A 108.5 . . ?
N2 C20 H20B 108.5 . . ?
C21 C20 H20A 108.5 . . ?
C21 C20 H20B 108.5 . . ?
C21 C20 N2 115.1(10) . . ?
C20 N2 C32 110.2(9) . . ?
C24 N2 C20 109.4(9) . . ?
C24 N2 C32 106.6(7) . . ?
C28 N2 C20 106.6(8) . . ?
C28 N2 C24 112.6(10) . . ?
C28 N2 C32 111.5(9) . . ?
N2 C24 H24A 108.2 . . ?
N2 C24 H24B 108.2 . . ?
N2 C24 C25 116.5(9) . . ?
H24A C24 H24B 107.3 . . ?
C25 C24 H24A 108.2 . . ?
C25 C24 H24B 108.2 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C20 C21 C22 111.4(9) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 C21 112.5(10) . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
N2 C32 H32A 108.6 . . ?
N2 C32 H32B 108.6 . . ?
H32A C32 H32B 107.6 . . ?
C33 C32 N2 114.6(9) . . ?
C33 C32 H32A 108.6 . . ?
C33 C32 H32B 108.6 . . ?
N2 C28 H28A 108.1 . . ?
N2 C28 H28B 108.1 . . ?
N2 C28 C29 116.7(11) . . ?
H28A C28 H28B 107.3 . . ?
C29 C28 H28A 108.1 . . ?
C29 C28 H28B 108.1 . . ?
H30A C30 H30B 107.5 . . ?
C29 C30 H30A 108.6 . . ?
C29 C30 H30B 108.6 . . ?
C31 C30 H30A 108.6 . . ?
C31 C30 H30B 108.6 . . ?
C31 C30 C29 114.9(16) . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
C30 C29 C28 109.8(13) . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C24 C25 H25A 110.1 . . ?
C24 C25 H25B 110.1 . . ?
C24 C25 C26 108.2(10) . . ?
H25A C25 H25B 108.4 . . ?
C26 C25 H25A 110.1 . . ?
C26 C25 H25B 110.1 . . ?
C25 C26 C27 114.4(13) . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
C27 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C40 N3 C48 108.1(8) . . ?
C36 N3 C40 112.1(9) . . ?
C36 N3 C48 110.3(9) . . ?
C44 N3 C40 110.7(10) . . ?
C44 N3 C36 107.0(8) . . ?
C44 N3 C48 108.6(10) . . ?
N3 C40 H40A 108.3 . . ?
N3 C40 H40B 108.3 . . ?
N3 C40 C41 116.1(11) . . ?
H40A C40 H40B 107.4 . . ?
C41 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
N3 C36 H36A 108.3 . . ?
N3 C36 H36B 108.3 . . ?
H36A C36 H36B 107.4 . . ?
C37 C36 N3 115.9(9) . . ?
C37 C36 H36A 108.3 . . ?
C37 C36 H36B 108.3 . . ?
N3 C48 H48A 107.1 . . ?
N3 C48 H48B 107.1 . . ?
N3 C48 C49 120.7(10) . . ?
H48A C48 H48B 106.8 . . ?
C49 C48 H48A 107.1 . . ?
C49 C48 H48B 107.1 . . ?
N3 C44 H44A 108.2 . . ?
N3 C44 H44B 108.2 . . ?
N3 C44 C45 116.6(10) . . ?
H44A C44 H44B 107.3 . . ?
C45 C44 H44A 108.2 . . ?
C45 C44 H44B 108.2 . . ?
H50A C50 H50B 106.7 . . ?
C49 C50 H50A 106.9 . . ?
C49 C50 H50B 106.9 . . ?
C49 C50 C51 121.8(14) . . ?
C51 C50 H50A 106.9 . . ?
C51 C50 H50B 106.9 . . ?
C43 C42 H42A 108.6 . . ?
C43 C42 H42B 108.6 . . ?
C43 C42 C41 114.7(14) . . ?
H42A C42 H42B 107.6 . . ?
C41 C42 H42A 108.6 . . ?
C41 C42 H42B 108.6 . . ?
C48 C49 C50 111.7(13) . . ?
C48 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
C50 C49 H49A 109.3 . . ?
C50 C49 H49B 109.3 . . ?
H49A C49 H49B 107.9 . . ?
C44 C45 H45A 108.7 . . ?
C44 C45 H45B 108.7 . . ?
C44 C45 C46 114.3(13) . . ?
H45A C45 H45B 107.6 . . ?
C46 C45 H45A 108.7 . . ?
C46 C45 H45B 108.7 . . ?
C47 C46 C45 105.1(16) . . ?
C47 C46 H46A 110.7 . . ?
C47 C46 H46B 110.7 . . ?
C45 C46 H46A 110.7 . . ?
C45 C46 H46B 110.7 . . ?
H46A C46 H46B 108.8 . . ?
C40 C41 H41A 108.4 . . ?
C40 C41 H41B 108.4 . . ?
C42 C41 C40 115.5(12) . . ?
C42 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C35 C34 C33 112.1(10) . . ?
H34A C34 H34B 107.9 . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
C32 C33 C34 112.4(9) . . ?
C32 C33 H33A 109.1 . . ?
C32 C33 H33B 109.1 . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
C36 C37 C38 111.4(10) . . ?
H37A C37 H37B 108.0 . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
C39 C38 C37 109.8(11) . . ?
C39 C38 H38A 109.7 . . ?
C39 C38 H38B 109.7 . . ?
C37 C38 H38A 109.7 . . ?
C37 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 V2 O8 V1 10.92(19) 2_665 . . . ?
V1 V2 O8 C1 -129.4(3) 2_665 . . . ?
V1 V2 O1 V1 180.0 2_665 . . . ?
V1 V2 O1 V2 119(100) 2_665 . . 2_665 ?
V1 V2 O1 V3 94.97(3) 2_665 . . 2_665 ?
V1 V2 O1 V3 -85.03(3) 2_665 . . . ?
V1 V2 O10 V3 42.19(12) 2_665 . . . ?
V1 V2 O10 C3 -175.5(3) 2_665 . . . ?
V1 V3 O1 V1 180.0 2_665 . . . ?
V1 V3 O1 V2 -95.53(3) 2_665 . . 2_665 ?
V1 V3 O1 V2 84.47(3) 2_665 . . . ?
V1 V3 O1 V3 -122(100) 2_665 . . 2_665 ?
V1 V3 O3 V2 43.99(16) 2_665 . . 2_665 ?
V1 V3 O10 V2 -41.78(12) 2_665 . . . ?
V1 V3 O10 C3 176.3(3) 2_665 . . . ?
V1 V3 O9 V1 -10.41(19) 2_665 . . . ?
V1 V3 O9 C2 130.2(3) 2_665 . . . ?
V1 O8 C1 C4 -67.9(4) . . . . ?
V1 O9 C2 C4 69.5(4) . . . . ?
V2 V1 O4 V3 43.96(15) 2_665 . . 2_665 ?
V2 V1 O8 V2 -10.75(19) 2_665 . . . ?
V2 V1 O8 C1 130.3(3) 2_665 . . . ?
V2 V1 O1 V1 -66(100) 2_665 . . 2_665 ?
V2 V1 O1 V2 180.0 2_665 . . . ?
V2 V1 O1 V3 84.65(3) 2_665 . . . ?
V2 V1 O1 V3 -95.35(3) 2_665 . . 2_665 ?
V2 V1 O9 V3 -42.20(12) 2_665 . . . ?
V2 V1 O9 C2 177.9(3) 2_665 . . . ?
V2 V3 O1 V1 -84.47(3) 2_665 . . . ?
V2 V3 O1 V1 95.53(3) 2_665 . . 2_665 ?
V2 V3 O1 V2 180.0 2_665 . . . ?
V2 V3 O1 V3 -26(100) 2_665 . . 2_665 ?
V2 V3 O10 V2 10.76(19) 2_665 . . . ?
V2 V3 O10 C3 -131.2(3) 2_665 . . . ?
V2 V3 O9 V1 42.16(12) 2_665 . . . ?
V2 V3 O9 C2 -177.2(3) 2_665 . . . ?
V2 O8 C1 C4 69.0(4) . . . . ?
V2 O10 C3 C4 -69.6(4) . . . . ?
V3 V1 O8 V2 41.98(12) 2_665 . . . ?
V3 V1 O8 C1 -176.9(3) 2_665 . . . ?
V3 V1 O1 V1 29(100) 2_665 . . 2_665 ?
V3 V1 O1 V2 95.35(3) 2_665 . . 2_665 ?
V3 V1 O1 V2 -84.65(3) 2_665 . . . ?
V3 V1 O1 V3 180.0 2_665 . . . ?
V3 V1 O2 V2 -50.80(14) 2_665 . . 2_665 ?
V3 V1 O9 V3 10.60(19) 2_665 . . . ?
V3 V1 O9 C2 -129.3(3) 2_665 . . . ?
V3 V2 O8 V1 -42.03(12) 2_665 . . . ?
V3 V2 O8 C1 177.7(3) 2_665 . . . ?
V3 V2 O1 V1 85.03(3) 2_665 . . . ?
V3 V2 O1 V1 -94.97(3) 2_665 . . 2_665 ?
V3 V2 O1 V2 24(100) 2_665 . . 2_665 ?
V3 V2 O1 V3 180.0 2_665 . . . ?
V3 V2 O10 V3 -10.68(19) 2_665 . . . ?
V3 V2 O10 C3 131.7(3) 2_665 . . . ?
V3 O10 C3 C4 69.4(4) . . . . ?
V3 O9 C2 C4 -67.1(4) . . . . ?
O4 V1 O8 V2 74.76(16) . . . . ?
O4 V1 O8 C1 -144.2(3) . . . . ?
O4 V1 O1 V1 32(100) . . . 2_665 ?
O4 V1 O1 V2 -82.40(10) . . . . ?
O4 V1 O1 V2 97.60(10) . . . 2_665 ?
O4 V1 O1 V3 2.25(10) . . . 2_665 ?
O4 V1 O1 V3 -177.75(10) . . . . ?
O4 V1 O2 V2 -83.01(18) . . . 2_665 ?
O4 V1 O9 V3 25.1(4) . . . . ?
O4 V1 O9 C2 -114.8(4) . . . . ?
O4 V3 O1 V1 2.36(11) 2_665 . . 2_665 ?
O4 V3 O1 V1 -177.64(11) 2_665 . . . ?
O4 V3 O1 V2 86.82(11) 2_665 . . . ?
O4 V3 O1 V2 -93.18(11) 2_665 . . 2_665 ?
O4 V3 O1 V3 -119(100) 2_665 . . 2_665 ?
O4 V3 O3 V2 78.49(19) 2_665 . . 2_665 ?
O4 V3 O10 V2 -75.55(16) 2_665 . . . ?
O4 V3 O10 C3 142.5(3) 2_665 . . . ?
O4 V3 O9 V1 -13.3(5) 2_665 . . . ?
O4 V3 O9 C2 127.3(4) 2_665 . . . ?
O8 V1 O4 V3 -80.62(18) . . . 2_665 ?
O8 V1 O1 V1 119(100) . . . 2_665 ?
O8 V1 O1 V2 -174.82(9) . . . 2_665 ?
O8 V1 O1 V2 5.18(9) . . . . ?
O8 V1 O1 V3 -90.17(9) . . . . ?
O8 V1 O1 V3 89.83(9) . . . 2_665 ?
O8 V1 O2 V2 3.5(5) . . . 2_665 ?
O8 V1 O9 V3 84.11(15) . . . . ?
O8 V1 O9 C2 -55.8(3) . . . . ?
O8 V2 O1 V1 174.68(9) . . . 2_665 ?
O8 V2 O1 V1 -5.32(9) . . . . ?
O8 V2 O1 V2 -66(100) . . . 2_665 ?
O8 V2 O1 V3 89.65(9) . . . . ?
O8 V2 O1 V3 -90.35(9) . . . 2_665 ?
O8 V2 O10 V3 -85.89(16) . . . . ?
O8 V2 O10 C3 56.5(3) . . . . ?
O1 V1 O4 V3 -3.05(14) . . . 2_665 ?
O1 V1 O8 V2 -6.12(11) . . . . ?
O1 V1 O8 C1 135.0(3) . . . . ?
O1 V1 O2 V2 -3.45(14) . . . 2_665 ?
O1 V1 O9 V3 5.96(11) . . . . ?
O1 V1 O9 C2 -133.9(3) . . . . ?
O1 V2 O8 V1 6.09(11) . . . . ?
O1 V2 O8 C1 -134.2(3) . . . . ?
O1 V2 O10 V3 -6.14(11) . . . . ?
O1 V2 O10 C3 136.2(3) . . . . ?
O1 V3 O3 V2 -2.65(14) . . . 2_665 ?
O1 V3 O10 V2 6.10(11) . . . . ?
O1 V3 O10 C3 -135.9(3) . . . . ?
O1 V3 O9 V1 -5.97(11) . . . . ?
O1 V3 O9 C2 134.7(3) . . . . ?
O3 V2 O8 V1 -75.79(16) 2_665 . . . ?
O3 V2 O8 C1 143.9(3) 2_665 . . . ?
O3 V2 O1 V1 -92.93(11) 2_665 . . 2_665 ?
O3 V2 O1 V1 87.07(11) 2_665 . . . ?
O3 V2 O1 V2 26(100) 2_665 . . 2_665 ?
O3 V2 O1 V3 2.04(11) 2_665 . . 2_665 ?
O3 V2 O1 V3 -177.96(11) 2_665 . . . ?
O3 V2 O10 V3 -14.5(5) 2_665 . . . ?
O3 V2 O10 C3 127.8(4) 2_665 . . . ?
O3 V3 O1 V1 -82.51(11) . . . . ?
O3 V3 O1 V1 97.49(11) . . . 2_665 ?
O3 V3 O1 V2 1.96(10) . . . 2_665 ?
O3 V3 O1 V2 -178.04(10) . . . . ?
O3 V3 O1 V3 -24(100) . . . 2_665 ?
O3 V3 O10 V2 24.2(4) . . . . ?
O3 V3 O10 C3 -117.8(4) . . . . ?
O3 V3 O9 V1 75.12(16) . . . . ?
O3 V3 O9 C2 -144.3(3) . . . . ?
O10 V2 O8 V1 84.00(15) . . . . ?
O10 V2 O8 C1 -56.3(3) . . . . ?
O10 V2 O1 V1 -89.86(9) . . . . ?
O10 V2 O1 V1 90.14(9) . . . 2_665 ?
O10 V2 O1 V2 -151(100) . . . 2_665 ?
O10 V2 O1 V3 -174.90(9) . . . 2_665 ?
O10 V2 O1 V3 5.10(9) . . . . ?
O10 V3 O1 V1 90.32(9) . . . . ?
O10 V3 O1 V1 -89.68(9) . . . 2_665 ?
O10 V3 O1 V2 -5.21(9) . . . . ?
O10 V3 O1 V2 174.79(9) . . . 2_665 ?
O10 V3 O1 V3 149(100) . . . 2_665 ?
O10 V3 O3 V2 -20.6(5) . . . 2_665 ?
O10 V3 O9 V1 -84.67(16) . . . . ?
O10 V3 O9 C2 55.9(3) . . . . ?
O2 V1 O4 V3 79.07(19) . . . 2_665 ?
O2 V1 O8 V2 -13.2(5) . . . . ?
O2 V1 O8 C1 127.9(4) . . . . ?
O2 V1 O1 V1 -63(100) . . . 2_665 ?
O2 V1 O1 V2 2.71(11) . . . 2_665 ?
O2 V1 O1 V2 -177.29(11) . . . . ?
O2 V1 O1 V3 -92.64(11) . . . 2_665 ?
O2 V1 O1 V3 87.36(11) . . . . ?
O2 V1 O9 V3 -76.56(16) . . . . ?
O2 V1 O9 C2 143.6(3) . . . . ?
O2 V2 O8 V1 26.8(4) 2_665 . . . ?
O2 V2 O8 C1 -113.5(4) 2_665 . . . ?
O2 V2 O1 V1 2.57(10) 2_665 . . 2_665 ?
O2 V2 O1 V1 -177.43(10) 2_665 . . . ?
O2 V2 O1 V2 122(100) 2_665 . . 2_665 ?
O2 V2 O1 V3 97.53(10) 2_665 . . 2_665 ?
O2 V2 O1 V3 -82.47(10) 2_665 . . . ?
O2 V2 O10 V3 75.28(16) 2_665 . . . ?
O2 V2 O10 C3 -142.4(3) 2_665 . . . ?
O9 V1 O4 V3 -22.1(5) . . . 2_665 ?
O9 V1 O8 V2 -85.90(15) . . . . ?
O9 V1 O8 C1 55.2(3) . . . . ?
O9 V1 O1 V1 -156(100) . . . 2_665 ?
O9 V1 O1 V2 -89.78(9) . . . 2_665 ?
O9 V1 O1 V2 90.22(9) . . . . ?
O9 V1 O1 V3 -5.13(9) . . . . ?
O9 V1 O1 V3 174.87(9) . . . 2_665 ?
O9 V1 O2 V2 74.78(17) . . . 2_665 ?
O9 V3 O1 V1 5.02(9) . . . . ?
O9 V3 O1 V1 -174.98(9) . . . 2_665 ?
O9 V3 O1 V2 -90.52(9) . . . . ?
O9 V3 O1 V2 89.48(9) . . . 2_665 ?
O9 V3 O1 V3 63(100) . . . 2_665 ?
O9 V3 O3 V2 -80.40(18) . . . 2_665 ?
O9 V3 O10 V2 84.53(15) . . . . ?
O9 V3 O10 C3 -57.4(3) . . . . ?
O7 V2 O8 V1 179.46(17) . . . . ?
O7 V2 O8 C1 39.1(3) . . . . ?
O7 V2 O1 V1 -62.6(10) . . . . ?
O7 V2 O1 V1 117.4(10) . . . 2_665 ?
O7 V2 O1 V2 -123(100) . . . 2_665 ?
O7 V2 O1 V3 -147.7(10) . . . 2_665 ?
O7 V2 O1 V3 32.3(10) . . . . ?
O7 V2 O10 V3 177.45(17) . . . . ?
O7 V2 O10 C3 -40.2(3) . . . . ?
O5 V1 O4 V3 -175.31(19) . . . 2_665 ?
O5 V1 O8 V2 176.85(17) . . . . ?
O5 V1 O8 C1 -42.1(3) . . . . ?
O5 V1 O1 V1 141(100) . . . 2_665 ?
O5 V1 O1 V2 26.9(10) . . . . ?
O5 V1 O1 V2 -153.1(10) . . . 2_665 ?
O5 V1 O1 V3 -68.5(10) . . . . ?
O5 V1 O1 V3 111.5(10) . . . 2_665 ?
O5 V1 O2 V2 173.17(18) . . . 2_665 ?
O5 V1 O9 V3 178.73(17) . . . . ?
O5 V1 O9 C2 38.8(3) . . . . ?
O11 C6 C7 C12 128.1(5) . . . . ?
O11 C6 C7 C8 -57.1(6) . . . . ?
O6 V3 O1 V1 -142.0(9) . . . 2_665 ?
O6 V3 O1 V1 38.0(9) . . . . ?
O6 V3 O1 V2 -57.6(9) . . . . ?
O6 V3 O1 V2 122.4(9) . . . 2_665 ?
O6 V3 O1 V3 96(100) . . . 2_665 ?
O6 V3 O3 V2 -175.28(18) . . . 2_665 ?
O6 V3 O10 V2 179.48(17) . . . . ?
O6 V3 O10 C3 37.5(3) . . . . ?
O6 V3 O9 V1 178.56(17) . . . . ?
O6 V3 O9 C2 -40.8(3) . . . . ?
O13 C13 N1 C14 -1.0(9) . . . . ?
O13 C13 C12 C7 -33.9(7) . . . . ?
O13 C13 C12 C11 139.5(5) . . . . ?
O12 C6 C7 C12 -56.4(7) . . . . ?
O12 C6 C7 C8 118.5(6) . . . . ?
C13 N1 C14 C15 -14.1(8) . . . . ?
C13 N1 C14 C19 168.1(5) . . . . ?
C6 O11 C5 C4 -106.0(5) . . . . ?
C6 C7 C12 C13 -10.8(7) . . . . ?
C6 C7 C12 C11 175.5(4) . . . . ?
C6 C7 C8 C9 -175.3(5) . . . . ?
N1 C13 C12 C7 148.3(5) . . . . ?
N1 C13 C12 C11 -38.2(7) . . . . ?
N1 C14 C19 C18 177.7(5) . . . . ?
C10 C11 C12 C13 -173.9(5) . . . . ?
C10 C11 C12 C7 -0.4(7) . . . . ?
C10 C9 C8 C7 -0.4(8) . . . . ?
C2 C4 C1 O8 61.6(5) . . . . ?
C2 C4 C3 O10 -59.8(5) . . . . ?
C2 C4 C5 O11 -62.5(5) . . . . ?
C11 C10 C9 C8 0.8(8) . . . . ?
C1 C4 C2 O9 -61.4(5) . . . . ?
C1 C4 C3 O10 61.6(5) . . . . ?
C1 C4 C5 O11 178.3(4) . . . . ?
C12 C13 N1 C14 176.7(5) . . . . ?
C12 C7 C8 C9 -0.4(8) . . . . ?
C15 C16 C17 C18 2.0(9) . . . . ?
C15 C14 C19 C18 -0.3(8) . . . . ?
C16 C15 C14 N1 -178.1(5) . . . . ?
C16 C15 C14 C19 -0.3(8) . . . . ?
C3 C4 C2 O9 59.9(5) . . . . ?
C3 C4 C1 O8 -60.5(5) . . . . ?
C3 C4 C5 O11 59.3(5) . . . . ?
C9 C10 C11 C12 -0.4(8) . . . . ?
C5 O11 C6 O12 -3.3(7) . . . . ?
C5 O11 C6 C7 172.3(4) . . . . ?
C5 C4 C2 O9 -179.3(4) . . . . ?
C5 C4 C1 O8 -179.5(4) . . . . ?
C5 C4 C3 O10 179.4(4) . . . . ?
C14 C15 C16 C17 -0.6(8) . . . . ?
C14 C19 C18 C17 1.7(9) . . . . ?
C8 C7 C12 C13 174.5(5) . . . . ?
C8 C7 C12 C11 0.8(7) . . . . ?
C19 C18 C17 C16 -2.5(9) . . . . ?
C20 N2 C24 C25 54.4(14) . . . . ?
C20 N2 C32 C33 -62.6(13) . . . . ?
C20 N2 C28 C29 175.8(14) . . . . ?
C20 C21 C22 C23 -176.3(10) . . . . ?
N2 C20 C21 C22 -172.5(10) . . . . ?
N2 C24 C25 C26 -175.4(11) . . . . ?
N2 C32 C33 C34 174.4(10) . . . . ?
N2 C28 C29 C30 -165.7(16) . . . . ?
C24 N2 C32 C33 178.8(10) . . . . ?
C24 N2 C28 C29 -64.3(16) . . . . ?
C24 C25 C26 C27 71.4(18) . . . . ?
C21 C20 N2 C24 61.2(14) . . . . ?
C21 C20 N2 C32 -55.7(13) . . . . ?
C21 C20 N2 C28 -176.9(12) . . . . ?
C32 N2 C24 C25 173.5(11) . . . . ?
C32 N2 C28 C29 55.4(17) . . . . ?
C35 C34 C33 C32 -68.0(15) . . . . ?
C28 N2 C24 C25 -63.9(14) . . . . ?
C28 N2 C32 C33 55.6(13) . . . . ?
N3 C40 C41 C42 104.2(17) . . . . ?
N3 C36 C37 C38 172.3(11) . . . . ?
N3 C48 C49 C50 -153.5(13) . . . . ?
N3 C44 C45 C46 171.0(14) . . . . ?
C40 N3 C36 C37 -72.1(14) . . . . ?
C40 N3 C48 C49 175.7(13) . . . . ?
C40 N3 C44 C45 48.8(17) . . . . ?
C36 N3 C40 C41 -56.1(14) . . . . ?
C36 N3 C48 C49 52.9(16) . . . . ?
C36 N3 C44 C45 171.3(14) . . . . ?
C36 C37 C38 C39 170.6(12) . . . . ?
C48 N3 C40 C41 -177.8(11) . . . . ?
C48 N3 C36 C37 48.4(14) . . . . ?
C48 N3 C44 C45 -69.7(16) . . . . ?
C44 N3 C40 C41 63.3(14) . . . . ?
C44 N3 C36 C37 166.3(12) . . . . ?
C44 N3 C48 C49 -64.1(15) . . . . ?
C44 C45 C46 C47 -81(2) . . . . ?
C43 C42 C41 C40 -167.7(15) . . . . ?
C51 C50 C49 C48 58(2) . . . . ?
C31 C30 C29 C28 -178(2) . . . . ?

####################################################################### 
# 
# 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_lbzda
_database_code_depnum_ccdc_archive 'CCDC 1541545'
_audit_update_record             
;
2017-05-03 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H116 N4 O25 V6'
_chemical_formula_weight         1671.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.187(2)
_cell_length_b                   13.547(3)
_cell_length_c                   14.326(3)
_cell_angle_alpha                107.72(3)
_cell_angle_beta                 94.21(3)
_cell_angle_gamma                104.66(3)
_cell_volume                     1974.0(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1993
_cell_measurement_theta_min      2.4687
_cell_measurement_theta_max      20.1827

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             878
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    0.756
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13073
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.512
_diffrn_reflns_theta_max         25.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             7302
_reflns_number_gt                4460
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1755P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7302
_refine_ls_number_parameters     476
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2798
_refine_ls_wR_factor_gt          0.2246
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.005
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.15050(9) 1.15921(8) 0.55665(7) 0.0488(3) Uani 1 1 d . . . . .
V3 V -0.14474(8) 1.06515(8) 0.44388(7) 0.0492(3) Uani 1 1 d . . . . .
O1 O 0.0000 1.0000 0.5000 0.0352(10) Uani 1 2 d S . P . .
O2 O 0.1761(3) 1.0979(3) 0.4153(3) 0.0459(9) Uani 1 1 d . . . . .
O3 O -0.0604(4) 1.0220(3) 0.3242(3) 0.0479(9) Uani 1 1 d . . . . .
O4 O 0.2397(4) 1.0761(3) 0.5924(3) 0.0572(11) Uani 1 1 d . . . . .
O5 O 0.0697(4) 1.1732(3) 0.6642(3) 0.0587(11) Uani 1 1 d . . . . .
O6 O 0.0082(4) 1.1944(3) 0.4891(3) 0.0480(9) Uani 1 1 d . . . . .
O7 O -0.1686(4) 1.0978(3) 0.5728(3) 0.0595(11) Uani 1 1 d . . . . .
O8 O 0.1063(5) 0.9183(4) 0.2475(3) 0.0679(12) Uani 1 1 d . . . . .
C1 C 0.0778(6) 1.1960(5) 0.3314(4) 0.0518(14) Uani 1 1 d . . . . .
O9 O 0.2506(4) 1.2754(3) 0.5813(3) 0.0701(13) Uani 1 1 d . . . . .
O10 O -0.2319(4) 1.1233(4) 0.3993(4) 0.0765(14) Uani 1 1 d . . . . .
O11 O 0.1426(5) 1.2300(4) 0.1817(3) 0.0723(13) Uani 1 1 d . . . . .
C2 C 0.0391(6) 1.2580(5) 0.4245(4) 0.0520(14) Uani 1 1 d . . . . .
H H 0.1068 1.3230 0.4599 0.062 Uiso 1 1 calc R U . . .
HA H -0.0330 1.2799 0.4068 0.062 Uiso 1 1 calc R U . . .
C3 C 0.1956(6) 1.1659(5) 0.3572(4) 0.0544(15) Uani 1 1 d . . . . .
HB H 0.2221 1.1296 0.2963 0.065 Uiso 1 1 calc R U . . .
HC H 0.2623 1.2315 0.3932 0.065 Uiso 1 1 calc R U . . .
C4 C -0.0285(6) 1.0938(5) 0.2713(4) 0.0564(15) Uani 1 1 d . . . . .
HD H -0.1017 1.1147 0.2540 0.068 Uiso 1 1 calc R U . . .
HE H -0.0027 1.0575 0.2101 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1049(8) 1.2758(6) 0.2723(5) 0.0718(19) Uani 1 1 d . . . . .
HF H 0.0301 1.2965 0.2595 0.086 Uiso 1 1 calc R U . . .
HG H 0.1703 1.3408 0.3120 0.086 Uiso 1 1 calc R U . . .
O13 O 0.1388(7) 1.3847(5) 0.0790(4) 0.113(2) Uani 1 1 d . . . . .
C7 C 0.2752(7) 1.2300(7) 0.0615(5) 0.074(2) Uani 1 1 d . . . . .
C6 C 0.2602(8) 1.2772(7) 0.1667(6) 0.082(2) Uani 1 1 d . . . . .
C8 C 0.2023(7) 1.2334(6) -0.0167(5) 0.0716(19) Uani 1 1 d . . . . .
C13 C 0.1098(9) 1.2999(7) 0.0069(5) 0.093(3) Uani 1 1 d . . . . .
C12 C 0.3634(10) 1.1770(10) 0.0410(7) 0.117(3) Uani 1 1 d . . . . .
HH H 0.4144 1.1756 0.0946 0.141 Uiso 1 1 calc R U . . .
O12 O 0.3388(6) 1.3411(6) 0.2328(4) 0.120(2) Uani 1 1 d . . . . .
N1 N 0.0079(9) 1.2695(8) -0.0549(6) 0.144(4) Uani 1 1 d . . . . .
HI H -0.0026 1.2156 -0.1086 0.173 Uiso 1 1 calc R U . . .
C11 C 0.3829(11) 1.1262(10) -0.0509(8) 0.135(4) Uani 1 1 d . . . . .
HJ H 0.4449 1.0913 -0.0611 0.163 Uiso 1 1 calc R U . . .
C10 C 0.3038(10) 1.1292(9) -0.1308(6) 0.109(3) Uani 1 1 d . . . . .
HK H 0.3110 1.0933 -0.1958 0.130 Uiso 1 1 calc R U . . .
C9 C 0.2169(8) 1.1843(7) -0.1130(5) 0.084(2) Uani 1 1 d . . . . .
HL H 0.1675 1.1888 -0.1658 0.101 Uiso 1 1 calc R U . . .
N2 N 0.3644(6) 0.6851(5) 0.3337(4) 0.0750(17) Uani 1 1 d . . . . .
C51 C 0.4269(7) 0.8086(6) 0.3670(6) 0.075(2) Uani 1 1 d . . . . .
H51A H 0.3936 0.8429 0.4249 0.090 Uiso 1 1 calc R U . . .
H51B H 0.5159 0.8225 0.3874 0.090 Uiso 1 1 calc R U . . .
C21 C 0.3831(9) 0.6243(8) 0.2377(7) 0.099(3) Uani 1 1 d . U . . .
H21A H 0.3559 0.6543 0.1893 0.119 Uiso 1 1 calc R U . . .
H21B H 0.3303 0.5503 0.2199 0.119 Uiso 1 1 calc R U . . .
C31 C 0.4060(9) 0.6409(8) 0.4133(7) 0.098(3) Uani 1 1 d . U . . .
H31A H 0.3639 0.5638 0.3908 0.118 Uiso 1 1 calc R U . . .
H31B H 0.4949 0.6492 0.4150 0.118 Uiso 1 1 calc R U . . .
C53 C 0.4589(7) 0.9831(6) 0.3399(6) 0.081(2) Uani 1 1 d . . . . .
H53A H 0.4093 1.0064 0.3905 0.097 Uiso 1 1 calc R U . . .
H53B H 0.5447 1.0023 0.3727 0.097 Uiso 1 1 calc R U . . .
C41 C 0.2196(8) 0.6734(7) 0.3312(8) 0.102(3) Uani 1 1 d . U . . .
H41A H 0.2097 0.7239 0.3926 0.123 Uiso 1 1 calc R U . . .
H41B H 0.1917 0.6960 0.2775 0.123 Uiso 1 1 calc R U . . .
C52 C 0.4107(8) 0.8606(6) 0.2927(6) 0.084(2) Uani 1 1 d . . . . .
H52A H 0.3227 0.8397 0.2648 0.101 Uiso 1 1 calc R U . . .
H52B H 0.4562 0.8365 0.2392 0.101 Uiso 1 1 calc R U . . .
C32 C 0.3860(14) 0.6868(10) 0.5167(8) 0.144(4) Uani 1 1 d . U . . .
H32A H 0.3000 0.6889 0.5167 0.172 Uiso 1 1 calc R U . . .
H32B H 0.4404 0.7604 0.5459 0.172 Uiso 1 1 calc R U . . .
V1 V 0.06330(10) 0.94377(8) 0.35306(7) 0.0489(3) Uani 1 1 d . . . . .
C54 C 0.4553(9) 1.0431(8) 0.2687(7) 0.101(3) Uani 1 1 d . . . . .
H54A H 0.4870 1.1196 0.3038 0.151 Uiso 1 1 calc R U . . .
H54B H 0.5061 1.0223 0.2193 0.151 Uiso 1 1 calc R U . . .
H54C H 0.3705 1.0263 0.2371 0.151 Uiso 1 1 calc R U . . .
C14 C -0.0915(14) 1.3223(13) -0.0384(10) 0.183(6) Uani 1 1 d D U . . .
HM H -0.1121 1.3418 -0.0961 0.219 Uiso 1 1 calc R U . . .
HN H -0.0608 1.3886 0.0182 0.219 Uiso 1 1 calc R U . . .
C15 C -0.2070(16) 1.2527(18) -0.0200(13) 0.234(9) Uani 1 1 d D U . . .
HO H -0.2707 1.2903 -0.0143 0.281 Uiso 1 1 calc R U . . .
HP H -0.2376 1.1869 -0.0770 0.281 Uiso 1 1 calc R U . . .
C16 C -0.1895(18) 1.223(2) 0.0703(15) 0.260(10) Uani 1 1 d D U . . .
HQ H -0.1368 1.2868 0.1227 0.312 Uiso 1 1 calc R U . . .
HR H -0.1441 1.1694 0.0566 0.312 Uiso 1 1 calc R U . . .
C17 C -0.304(2) 1.180(2) 0.109(2) 0.297(12) Uani 1 1 d D U . . .
HS H -0.2807 1.1636 0.1670 0.446 Uiso 1 1 calc R U . . .
HT H -0.3490 1.2327 0.1251 0.446 Uiso 1 1 calc R U . . .
HU H -0.3563 1.1149 0.0587 0.446 Uiso 1 1 calc R U . . .
C22 C 0.5149(9) 0.6228(11) 0.2310(8) 0.131(4) Uani 1 1 d . U . . .
H22A H 0.5658 0.6965 0.2435 0.157 Uiso 1 1 calc R U . . .
H22B H 0.5440 0.5997 0.2840 0.157 Uiso 1 1 calc R U . . .
C24 C 0.6572(15) 0.5372(16) 0.1350(14) 0.212(8) Uani 1 1 d . U . . .
H24A H 0.6587 0.4912 0.0694 0.318 Uiso 1 1 calc R U . . .
H24B H 0.7207 0.6050 0.1504 0.318 Uiso 1 1 calc R U . . .
H24C H 0.6728 0.5028 0.1822 0.318 Uiso 1 1 calc R U . . .
C23 C 0.5382(14) 0.5556(12) 0.1391(12) 0.176(6) Uani 1 1 d . U . . .
H23A H 0.4758 0.4856 0.1204 0.212 Uiso 1 1 calc R U . . .
H23B H 0.5235 0.5873 0.0887 0.212 Uiso 1 1 calc R U . . .
C33 C 0.4133(16) 0.6196(14) 0.5788(9) 0.193(7) Uani 1 1 d D U . . .
H33A H 0.3925 0.5441 0.5374 0.232 Uiso 1 1 calc R U . . .
H33B H 0.5017 0.6440 0.6062 0.232 Uiso 1 1 calc R U . . .
C34 C 0.338(2) 0.631(2) 0.6606(17) 0.344(16) Uani 1 1 d D U . . .
H34A H 0.3551 0.5883 0.6999 0.516 Uiso 1 1 calc R U . . .
H34B H 0.3594 0.7055 0.7018 0.516 Uiso 1 1 calc R U . . .
H34C H 0.2504 0.6059 0.6331 0.516 Uiso 1 1 calc R U . . .
C42 C 0.1337(10) 0.5645(9) 0.3186(10) 0.136(4) Uani 1 1 d D U . . .
H42A H 0.1587 0.5408 0.3725 0.163 Uiso 0.67(3) 1 calc R U P A 1
H42B H 0.1406 0.5129 0.2568 0.163 Uiso 0.67(3) 1 calc R U P A 1
H42C H 0.1287 0.5543 0.3825 0.163 Uiso 0.33(3) 1 calc R U P A 2
H42D H 0.1635 0.5079 0.2765 0.163 Uiso 0.33(3) 1 calc R U P A 2
C43A C -0.0011(13) 0.567(2) 0.3178(17) 0.168(9) Uani 0.67(3) 1 d D U P A 1
H43A H -0.0176 0.5871 0.3856 0.201 Uiso 0.67(3) 1 calc R U P A 1
H43B H -0.0133 0.6217 0.2906 0.201 Uiso 0.67(3) 1 calc R U P A 1
C44A C -0.092(4) 0.460(3) 0.258(3) 0.43(4) Uani 0.67(3) 1 d D U P A 1
H44A H -0.1762 0.4658 0.2599 0.641 Uiso 0.67(3) 1 calc R U P A 1
H44B H -0.0777 0.4405 0.1907 0.641 Uiso 0.67(3) 1 calc R U P A 1
H44C H -0.0821 0.4059 0.2856 0.641 Uiso 0.67(3) 1 calc R U P A 1
C43B C 0.007(2) 0.561(3) 0.271(4) 0.185(17) Uani 0.33(3) 1 d D U P A 2
H43C H 0.0000 0.6340 0.2822 0.222 Uiso 0.33(3) 1 calc R U P A 2
H43D H -0.0082 0.5229 0.2001 0.222 Uiso 0.33(3) 1 calc R U P A 2
C44B C -0.082(3) 0.503(4) 0.322(3) 0.19(2) Uani 0.33(3) 1 d D U P A 2
H44D H -0.1667 0.4965 0.2963 0.284 Uiso 0.33(3) 1 calc R U P A 2
H44E H -0.0731 0.4315 0.3106 0.284 Uiso 0.33(3) 1 calc R U P A 2
H44F H -0.0650 0.5417 0.3921 0.284 Uiso 0.33(3) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O9 1.603(4) . ?
V2 O5 1.828(4) . ?
V2 O4 1.837(4) . ?
V2 O2 2.014(4) . ?
V2 O6 2.034(4) . ?
V2 O1 2.2452(14) . ?
V2 V3 3.0215(15) 2_576 ?
V2 V1 3.0337(16) 2_576 ?
V3 O10 1.607(5) . ?
V3 O7 1.820(4) . ?
V3 O4 1.829(4) 2_576 ?
V3 O6 2.011(4) . ?
V3 O3 2.020(4) . ?
V3 O1 2.2387(11) . ?
V3 V2 3.0215(15) 2_576 ?
V3 V1 3.0313(16) 2_576 ?
O1 V3 2.2388(11) 2_576 ?
O1 V1 2.2425(11) . ?
O1 V1 2.2425(11) 2_576 ?
O1 V2 2.2453(14) 2_576 ?
O2 C3 1.407(6) . ?
O2 V1 2.028(4) . ?
O3 C4 1.401(7) . ?
O3 V1 2.033(4) . ?
O4 V3 1.829(4) 2_576 ?
O5 V1 1.816(4) 2_576 ?
O6 C2 1.449(6) . ?
O7 V1 1.830(4) 2_576 ?
O8 V1 1.584(4) . ?
C1 C2 1.502(8) . ?
C1 C3 1.528(9) . ?
C1 C4 1.537(8) . ?
C1 C5 1.552(8) . ?
O11 C6 1.374(9) . ?
O11 C5 1.403(8) . ?
O13 C13 1.238(9) . ?
C7 C8 1.356(10) . ?
C7 C12 1.359(12) . ?
C7 C6 1.489(10) . ?
C6 O12 1.188(8) . ?
C8 C9 1.380(10) . ?
C8 C13 1.527(13) . ?
C13 N1 1.284(10) . ?
C12 C11 1.350(13) . ?
N1 C14 1.463(15) . ?
C11 C10 1.410(14) . ?
C10 C9 1.362(13) . ?
N2 C21 1.433(10) . ?
N2 C31 1.535(10) . ?
N2 C51 1.545(9) . ?
N2 C41 1.584(10) . ?
C51 C52 1.468(11) . ?
C21 C22 1.490(12) . ?
C31 C32 1.479(13) . ?
C53 C54 1.490(11) . ?
C53 C52 1.521(10) . ?
C41 C42 1.491(13) . ?
C32 C33 1.518(16) . ?
V1 O5 1.816(4) 2_576 ?
V1 O7 1.830(4) 2_576 ?
V1 V3 3.0313(16) 2_576 ?
V1 V2 3.0337(16) 2_576 ?
C14 C15 1.488(9) . ?
C15 C16 1.480(9) . ?
C16 C17 1.485(10) . ?
C22 C23 1.438(15) . ?
C24 C23 1.418(17) . ?
C33 C34 1.487(9) . ?
C42 C43B 1.515(10) . ?
C42 C43A 1.517(10) . ?
C43A C44A 1.495(10) . ?
C43B C44B 1.493(10) . ?

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
O9 V2 O5 104.4(2) . . ?
O9 V2 O4 104.7(2) . . ?
O5 V2 O4 93.6(2) . . ?
O9 V2 O2 96.4(2) . . ?
O5 V2 O2 157.52(17) . . ?
O4 V2 O2 89.26(18) . . ?
O9 V2 O6 96.0(2) . . ?
O5 V2 O6 87.36(18) . . ?
O4 V2 O6 158.34(17) . . ?
O2 V2 O6 81.98(15) . . ?
O9 V2 O1 171.05(17) . . ?
O5 V2 O1 80.95(13) . . ?
O4 V2 O1 81.94(13) . . ?
O2 V2 O1 77.38(11) . . ?
O6 V2 O1 76.84(11) . . ?
O9 V2 V3 138.74(18) . 2_576 ?
O5 V2 V3 87.80(13) . 2_576 ?
O4 V2 V3 34.40(13) . 2_576 ?
O2 V2 V3 82.02(11) . 2_576 ?
O6 V2 V3 124.21(12) . 2_576 ?
O1 V2 V3 47.55(3) . 2_576 ?
O9 V2 V1 137.49(19) . 2_576 ?
O5 V2 V1 33.52(13) . 2_576 ?
O4 V2 V1 88.21(13) . 2_576 ?
O2 V2 V1 124.53(11) . 2_576 ?
O6 V2 V1 80.67(11) . 2_576 ?
O1 V2 V1 47.43(3) . 2_576 ?
V3 V2 V1 66.06(4) 2_576 2_576 ?
O10 V3 O7 102.8(2) . . ?
O10 V3 O4 104.4(2) . 2_576 ?
O7 V3 O4 94.4(2) . 2_576 ?
O10 V3 O6 95.4(2) . . ?
O7 V3 O6 87.64(18) . . ?
O4 V3 O6 159.11(18) 2_576 . ?
O10 V3 O3 97.1(2) . . ?
O7 V3 O3 158.65(17) . . ?
O4 V3 O3 88.15(18) 2_576 . ?
O6 V3 O3 82.72(16) . . ?
O10 V3 O1 171.62(17) . . ?
O7 V3 O1 81.44(13) . . ?
O4 V3 O1 82.30(13) 2_576 . ?
O6 V3 O1 77.45(11) . . ?
O3 V3 O1 77.90(11) . . ?
O10 V3 V2 138.83(19) . 2_576 ?
O7 V3 V2 88.13(13) . 2_576 ?
O4 V3 V2 34.57(12) 2_576 2_576 ?
O6 V3 V2 125.00(12) . 2_576 ?
O3 V3 V2 81.98(11) . 2_576 ?
O1 V3 V2 47.73(4) . 2_576 ?
O10 V3 V1 136.3(2) . 2_576 ?
O7 V3 V1 33.95(13) . 2_576 ?
O4 V3 V1 89.03(13) 2_576 2_576 ?
O6 V3 V1 81.07(11) . 2_576 ?
O3 V3 V1 125.15(11) . 2_576 ?
O1 V3 V1 47.49(3) . 2_576 ?
V2 V3 V1 66.24(5) 2_576 2_576 ?
V3 O1 V3 180.00(4) . 2_576 ?
V3 O1 V1 94.87(4) . . ?
V3 O1 V1 85.13(4) 2_576 . ?
V3 O1 V1 85.13(4) . 2_576 ?
V3 O1 V1 94.87(4) 2_576 2_576 ?
V1 O1 V1 180.0 . 2_576 ?
V3 O1 V2 95.27(4) . . ?
V3 O1 V2 84.73(4) 2_576 . ?
V1 O1 V2 94.94(5) . . ?
V1 O1 V2 85.06(5) 2_576 . ?
V3 O1 V2 84.73(4) . 2_576 ?
V3 O1 V2 95.27(4) 2_576 2_576 ?
V1 O1 V2 85.06(5) . 2_576 ?
V1 O1 V2 94.94(5) 2_576 2_576 ?
V2 O1 V2 180.0 . 2_576 ?
C3 O2 V2 118.8(3) . . ?
C3 O2 V1 119.1(3) . . ?
V2 O2 V1 109.79(17) . . ?
C4 O3 V3 118.7(4) . . ?
C4 O3 V1 119.4(4) . . ?
V3 O3 V1 109.06(16) . . ?
V3 O4 V2 111.04(19) 2_576 . ?
V1 O5 V2 112.7(2) 2_576 . ?
C2 O6 V3 118.7(3) . . ?
C2 O6 V2 117.6(3) . . ?
V3 O6 V2 109.99(17) . . ?
V3 O7 V1 112.3(2) . 2_576 ?
C2 C1 C3 110.1(5) . . ?
C2 C1 C4 110.9(5) . . ?
C3 C1 C4 110.4(5) . . ?
C2 C1 C5 104.4(5) . . ?
C3 C1 C5 110.7(5) . . ?
C4 C1 C5 110.2(5) . . ?
C6 O11 C5 118.4(6) . . ?
O6 C2 C1 112.1(5) . . ?
O2 C3 C1 112.3(5) . . ?
O3 C4 C1 112.1(5) . . ?
O11 C5 C1 111.8(6) . . ?
C8 C7 C12 117.4(8) . . ?
C8 C7 C6 123.5(8) . . ?
C12 C7 C6 119.0(8) . . ?
O12 C6 O11 122.3(7) . . ?
O12 C6 C7 126.9(8) . . ?
O11 C6 C7 110.7(6) . . ?
C7 C8 C9 121.0(8) . . ?
C7 C8 C13 117.1(7) . . ?
C9 C8 C13 121.8(7) . . ?
O13 C13 N1 122.1(10) . . ?
O13 C13 C8 120.0(8) . . ?
N1 C13 C8 117.6(8) . . ?
C11 C12 C7 125.1(10) . . ?
C13 N1 C14 123.1(9) . . ?
C12 C11 C10 116.2(11) . . ?
C9 C10 C11 120.2(9) . . ?
C10 C9 C8 120.0(8) . . ?
C21 N2 C31 110.9(7) . . ?
C21 N2 C51 115.4(7) . . ?
C31 N2 C51 109.5(6) . . ?
C21 N2 C41 108.7(6) . . ?
C31 N2 C41 107.7(7) . . ?
C51 N2 C41 104.2(5) . . ?
C52 C51 N2 116.0(6) . . ?
N2 C21 C22 114.4(7) . . ?
C32 C31 N2 119.8(8) . . ?
C54 C53 C52 114.3(7) . . ?
C42 C41 N2 117.9(7) . . ?
C51 C52 C53 110.3(7) . . ?
C31 C32 C33 111.1(9) . . ?
O8 V1 O5 102.9(2) . 2_576 ?
O8 V1 O7 104.5(2) . 2_576 ?
O5 V1 O7 94.42(19) 2_576 2_576 ?
O8 V1 O2 97.9(2) . . ?
O5 V1 O2 157.62(18) 2_576 . ?
O7 V1 O2 88.19(18) 2_576 . ?
O8 V1 O3 96.2(2) . . ?
O5 V1 O3 87.88(18) 2_576 . ?
O7 V1 O3 157.96(18) 2_576 . ?
O2 V1 O3 81.72(15) . . ?
O8 V1 O1 172.50(17) . . ?
O5 V1 O1 81.28(13) 2_576 . ?
O7 V1 O1 81.13(14) 2_576 . ?
O2 V1 O1 77.17(11) . . ?
O3 V1 O1 77.56(11) . . ?
O8 V1 V3 138.13(18) . 2_576 ?
O5 V1 V3 88.31(13) 2_576 2_576 ?
O7 V1 V3 33.75(13) 2_576 2_576 ?
O2 V1 V3 81.56(11) . 2_576 ?
O3 V1 V3 124.71(11) . 2_576 ?
O1 V1 V3 47.38(3) . 2_576 ?
O8 V1 V2 136.40(18) . 2_576 ?
O5 V1 V2 33.77(13) 2_576 2_576 ?
O7 V1 V2 88.30(14) 2_576 2_576 ?
O2 V1 V2 124.40(11) . 2_576 ?
O3 V1 V2 81.47(11) . 2_576 ?
O1 V1 V2 47.51(4) . 2_576 ?
V3 V1 V2 66.22(4) 2_576 2_576 ?
N1 C14 C15 112.9(14) . . ?
C16 C15 C14 114.3(16) . . ?
C15 C16 C17 117.3(18) . . ?
C23 C22 C21 117.2(9) . . ?
C24 C23 C22 119.0(16) . . ?
C34 C33 C32 109.5(14) . . ?
C41 C42 C43B 106.3(15) . . ?
C41 C42 C43A 111.4(12) . . ?
C44A C43A C42 113(2) . . ?
C44B C43B C42 103(2) . . ?

_refine_diff_density_max         0.779
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.127

####################################################################### 
# 
# 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_lbxba
_database_code_depnum_ccdc_archive 'CCDC 1541546'
_audit_update_record             
;
2017-05-02 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_audit_creation_date             2017-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H36 N2 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C64 H108 N4 O25 V6'
_chemical_formula_weight         1639.18
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.5838(19)
_cell_length_b                   17.309(2)
_cell_length_c                   16.326(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.950(2)
_cell_angle_gamma                90
_cell_volume                     3755.4(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18.907
_cell_measurement_theta_min      2.353
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0695 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.9277.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28892
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.273
_diffrn_reflns_theta_min         1.735
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3733
_reflns_number_total             7549
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7549
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0944P)²+2.9775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.2132
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1AA-C2AA
 1.33 with sigma of 0.01
3. Rigid bond restraints
 C54, C53, C52, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1AA \\sim C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B), C14(H14A,H14B), C51(H51A,H51B),
 C41(H41A,H41B), C31(H31A,H31B), C21(H21A,H21B), C22(H22A,H22B), C52(H52A,H52B),
  C42(H42A,H42B), C23(H23A,H23B), C43(H43A,H43B), C32(H32A,H32B), C33(H33A,
 H33B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 N13(H13), C11(H11), C8(H8), C9(H9), C10(H10), C1AA(H1AA)
5.c X=CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C24(H24A,H24B,H24C), C54(H54A,H54B,
 H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.50308(7) -0.10288(6) 0.91613(6) 0.0500(3) Uani 1 1 d . . . . .
V3 V 0.38110(7) 0.06246(6) 0.91076(6) 0.0508(3) Uani 1 1 d . . . . .
O1 O 0.5000 0.0000 1.0000 0.0379(11) Uani 1 2 d S T P . .
O2 O 0.6072(3) -0.0302(2) 0.8823(2) 0.0439(9) Uani 1 1 d . . . . .
O3 O 0.5052(3) 0.1020(2) 0.8785(2) 0.0471(9) Uani 1 1 d . . . . .
O4 O 0.4074(3) -0.0318(2) 0.8436(2) 0.0494(9) Uani 1 1 d . . . . .
O5 O 0.3003(2) -0.0008(2) 0.9599(2) 0.0504(10) Uani 1 1 d . . . . .
O6 O 0.6034(3) -0.1317(2) 1.0053(2) 0.0529(10) Uani 1 1 d . . . . .
O7 O 0.4023(3) -0.1331(2) 0.9649(2) 0.0540(10) Uani 1 1 d . . . . .
C4 C 0.5085(4) 0.1051(4) 0.7909(3) 0.0540(15) Uani 1 1 d . . . . .
H4A H 0.5679 0.1335 0.7842 0.065 Uiso 1 1 calc R . . . .
H4B H 0.4499 0.1329 0.7610 0.065 Uiso 1 1 calc R . . . .
O8 O 0.7102(3) 0.1029(2) 0.9201(2) 0.0613(11) Uani 1 1 d . . . . .
O9 O 0.5063(3) -0.1678(2) 0.8464(3) 0.0675(12) Uani 1 1 d . . . . .
O10 O 0.3028(3) 0.1029(3) 0.8368(3) 0.0668(12) Uani 1 1 d . . . . .
O11 O 0.4245(3) 0.0665(3) 0.6143(2) 0.0686(12) Uani 1 1 d . . . . .
O12 O 0.4968(4) 0.0861(3) 0.5043(3) 0.0812(15) Uani 1 1 d . . . . .
C3 C 0.6023(5) -0.0178(4) 0.7966(4) 0.0522(15) Uani 1 1 d . . . . .
O13 O 0.4317(4) 0.2349(3) 0.5821(3) 0.0903(16) Uani 1 1 d . . . . .
C2 C 0.4154(5) -0.0199(4) 0.7586(3) 0.0578(16) Uani 1 1 d . . . . .
H2A H 0.3566 0.0079 0.7292 0.069 Uiso 1 1 calc R . . . .
H2B H 0.4170 -0.0696 0.7314 0.069 Uiso 1 1 calc R . . . .
N13 N 0.2891(4) 0.2938(3) 0.5985(4) 0.0761(16) Uani 1 1 d . . . . .
H13 H 0.2245 0.2917 0.5886 0.091 Uiso 1 1 calc R . . . .
C7 C 0.3236(5) 0.1138(4) 0.4918(4) 0.0584(16) Uani 1 1 d . . . . .
C12 C 0.2793(5) 0.1839(4) 0.5058(4) 0.0609(17) Uani 1 1 d . . . . .
C5 C 0.5187(5) 0.0351(4) 0.6616(3) 0.0637(18) Uani 1 1 d . . . . .
H5A H 0.5738 0.0696 0.6576 0.076 Uiso 1 1 calc R . . . .
H5B H 0.5319 -0.0147 0.6387 0.076 Uiso 1 1 calc R . . . .
C6 C 0.4235(5) 0.0901(4) 0.5362(4) 0.0659(18) Uani 1 1 d . . . . .
C1 C 0.3391(5) 0.2400(4) 0.5651(4) 0.0657(18) Uani 1 1 d . . . . .
C0AA C 0.5107(4) 0.0260(4) 0.7528(3) 0.0521(15) Uani 1 1 d . . . . .
C11 C 0.1803(5) 0.2003(4) 0.4615(5) 0.074(2) Uani 1 1 d . . . . .
H11 H 0.1496 0.2467 0.4706 0.089 Uiso 1 1 calc R . . . .
C8 C 0.2707(6) 0.0625(5) 0.4343(4) 0.075(2) Uani 1 1 d . . . . .
H8 H 0.3010 0.0163 0.4240 0.089 Uiso 1 1 calc R . . . .
C14 C 0.3396(7) 0.3561(5) 0.6509(6) 0.100(3) Uani 1 1 d . . . . .
H14A H 0.4046 0.3643 0.6366 0.120 Uiso 1 1 calc R . . . .
H14B H 0.3007 0.4029 0.6363 0.120 Uiso 1 1 calc R . . . .
C9 C 0.1726(7) 0.0783(5) 0.3911(5) 0.092(2) Uani 1 1 d . . . . .
H9 H 0.1367 0.0428 0.3536 0.110 Uiso 1 1 calc R . . . .
C10 C 0.1308(6) 0.1483(5) 0.4060(5) 0.089(2) Uani 1 1 d . . . . .
H10 H 0.0662 0.1602 0.3768 0.106 Uiso 1 1 calc R . . . .
N2 N 0.0559(3) 0.1916(3) 0.8782(3) 0.0524(12) Uani 1 1 d . . . . .
C51 C -0.0577(4) 0.1862(4) 0.8600(4) 0.0632(17) Uani 1 1 d . U . . .
H51A H -0.0765 0.1359 0.8354 0.076 Uiso 1 1 calc R . . . .
H51B H -0.0795 0.1882 0.9129 0.076 Uiso 1 1 calc R . . . .
C41 C 0.0984(5) 0.1226(4) 0.9322(4) 0.0651(17) Uani 1 1 d . . . . .
H41A H 0.0748 0.0757 0.9019 0.078 Uiso 1 1 calc R . . . .
H41B H 0.1712 0.1236 0.9398 0.078 Uiso 1 1 calc R . . . .
C31 C 0.0891(5) 0.2679(4) 0.9204(4) 0.0719(19) Uani 1 1 d . . . . .
H31A H 0.0541 0.2754 0.9658 0.086 Uiso 1 1 calc R . . . .
H31B H 0.0685 0.3091 0.8802 0.086 Uiso 1 1 calc R . . . .
C21 C 0.0941(5) 0.1880(4) 0.7977(4) 0.0610(17) Uani 1 1 d . . . . .
H21A H 0.0704 0.2338 0.7653 0.073 Uiso 1 1 calc R . . . .
H21B H 0.1669 0.1910 0.8119 0.073 Uiso 1 1 calc R . . . .
C22 C 0.0661(5) 0.1193(4) 0.7422(4) 0.0717(19) Uani 1 1 d . . . . .
H22A H -0.0065 0.1164 0.7248 0.086 Uiso 1 1 calc R . . . .
H22B H 0.0892 0.0726 0.7731 0.086 Uiso 1 1 calc R . . . .
C52 C -0.1147(5) 0.2455(5) 0.8040(4) 0.083(2) Uani 1 1 d . U . . .
H52A H -0.0798 0.2568 0.7592 0.100 Uiso 1 1 calc R . . . .
H52B H -0.1172 0.2928 0.8355 0.100 Uiso 1 1 calc R . . . .
C42 C 0.0721(5) 0.1185(4) 1.0167(4) 0.0706(19) Uani 1 1 d . . . . .
H42A H 0.0868 0.1678 1.0447 0.085 Uiso 1 1 calc R . . . .
H42B H 0.0005 0.1089 1.0099 0.085 Uiso 1 1 calc R . . . .
C23 C 0.1125(6) 0.1243(5) 0.6654(4) 0.078(2) Uani 1 1 d . . . . .
H23A H 0.0810 0.1663 0.6303 0.094 Uiso 1 1 calc R . . . .
H23B H 0.1835 0.1364 0.6832 0.094 Uiso 1 1 calc R . . . .
C43 C 0.1290(5) 0.0566(4) 1.0695(4) 0.0721(19) Uani 1 1 d . . . . .
H43A H 0.2002 0.0682 1.0782 0.086 Uiso 1 1 calc R . . . .
H43B H 0.1178 0.0082 1.0390 0.086 Uiso 1 1 calc R . . . .
C32 C 0.2012(6) 0.2755(5) 0.9550(5) 0.095(2) Uani 1 1 d . . . . .
H32A H 0.2211 0.2372 0.9987 0.114 Uiso 1 1 calc R . . . .
H32B H 0.2368 0.2641 0.9107 0.114 Uiso 1 1 calc R . . . .
C34 C 0.3419(8) 0.3594(7) 1.0265(8) 0.147(4) Uani 1 1 d . . . . .
H34A H 0.3794 0.3587 0.9827 0.220 Uiso 1 1 calc GR . . . .
H34B H 0.3631 0.3172 1.0642 0.220 Uiso 1 1 calc GR . . . .
H34C H 0.3535 0.4073 1.0566 0.220 Uiso 1 1 calc GR . . . .
C44 C 0.1019(6) 0.0458(5) 1.1528(5) 0.093(2) Uani 1 1 d . . . . .
H44A H 0.0305 0.0388 1.1454 0.140 Uiso 1 1 calc GR . . . .
H44B H 0.1221 0.0905 1.1869 0.140 Uiso 1 1 calc GR . . . .
H44C H 0.1358 0.0010 1.1797 0.140 Uiso 1 1 calc GR . . . .
C33 C 0.2317(7) 0.3514(5) 0.9890(7) 0.124(4) Uani 1 1 d . . . . .
H33A H 0.1939 0.3634 1.0317 0.149 Uiso 1 1 calc R . . . .
H33B H 0.2137 0.3893 0.9447 0.149 Uiso 1 1 calc R . . . .
C24 C 0.1021(7) 0.0521(6) 0.6150(5) 0.109(3) Uani 1 1 d . . . . .
H24A H 0.1366 0.0580 0.5696 0.163 Uiso 1 1 calc GR . . . .
H24B H 0.0321 0.0421 0.5929 0.163 Uiso 1 1 calc GR . . . .
H24C H 0.1308 0.0098 0.6498 0.163 Uiso 1 1 calc GR . . . .
V1 V 0.62743(7) 0.06097(6) 0.95978(6) 0.0480(3) Uani 1 1 d . . . . .
C53 C -0.2212(6) 0.2195(7) 0.7665(6) 0.136(4) Uani 1 1 d . U . . .
H53A H -0.2170 0.1698 0.7400 0.163 Uiso 1 1 calc R . . . .
H53B H -0.2555 0.2111 0.8123 0.163 Uiso 1 1 calc R . . . .
C54 C -0.2808(8) 0.2667(9) 0.7093(7) 0.179(6) Uani 1 1 d . U . . .
H54A H -0.2941 0.3137 0.7362 0.269 Uiso 1 1 calc GR . . . .
H54B H -0.3431 0.2409 0.6868 0.269 Uiso 1 1 calc GR . . . .
H54C H -0.2468 0.2784 0.6647 0.269 Uiso 1 1 calc GR . . . .
C1AA C 0.3549(11) 0.3466(8) 0.7370(9) 0.164(5) Uani 1 1 d D U . . .
H1AA H 0.3585 0.3929 0.7664 0.197 Uiso 1 1 calc R . . . .
C2AA C 0.3650(10) 0.2866(8) 0.7840(9) 0.181(5) Uani 1 1 d D U . . .
H2AA H 0.3625 0.2376 0.7603 0.217 Uiso 1 1 calc R . . . .
H2AB H 0.3749 0.2921 0.8418 0.217 Uiso 1 1 calc R . . . .
H3A H 0.602(3) -0.066(3) 0.770(3) 0.026(12) Uiso 1 1 d . . . . .
H3B H 0.660(5) 0.007(3) 0.787(4) 0.063(18) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 V3 3.0185(15) 3_657 ?
V2 O1 2.2521(9) . ?
V2 O2 2.052(4) . ?
V2 O4 1.992(4) . ?
V2 O6 1.844(4) . ?
V2 O7 1.798(4) . ?
V2 O9 1.606(4) . ?
V2 V1 3.0432(13) 3_657 ?
V3 V2 3.0184(15) 3_657 ?
V3 O1 2.2193(10) . ?
V3 O3 1.988(4) . ?
V3 O4 2.038(4) . ?
V3 O5 1.847(4) . ?
V3 O6 1.800(4) 3_657 ?
V3 O10 1.596(4) . ?
V3 V1 3.0242(14) 3_657 ?
O1 V2 2.2521(9) 3_657 ?
O1 V3 2.2193(10) 3_657 ?
O1 V1 2.2387(9) . ?
O1 V1 2.2386(9) 3_657 ?
O2 C3 1.404(7) . ?
O2 V1 2.005(4) . ?
O3 C4 1.442(6) . ?
O3 V1 2.027(4) . ?
O4 C2 1.429(6) . ?
O5 V1 1.799(4) 3_657 ?
O6 V3 1.800(4) 3_657 ?
O7 V1 1.855(4) 3_657 ?
C4 C0AA 1.506(8) . ?
O8 V1 1.585(4) . ?
O11 C5 1.455(7) . ?
O11 C6 1.337(7) . ?
O12 C6 1.217(7) . ?
C3 C0AA 1.506(8) . ?
O13 C1 1.234(7) . ?
C2 C0AA 1.539(8) . ?
N13 C1 1.333(8) . ?
N13 C14 1.456(9) . ?
C7 C12 1.394(9) . ?
C7 C6 1.459(9) . ?
C7 C8 1.381(9) . ?
C12 C1 1.488(9) . ?
C12 C11 1.417(9) . ?
C5 C0AA 1.524(7) . ?
C11 C10 1.354(10) . ?
C8 C9 1.400(10) . ?
C14 C1AA 1.388(14) . ?
C9 C10 1.381(11) . ?
N2 C51 1.513(7) . ?
N2 C41 1.525(7) . ?
N2 C31 1.514(8) . ?
N2 C21 1.512(7) . ?
C51 C52 1.482(8) . ?
C41 C42 1.496(8) . ?
C31 C32 1.515(10) . ?
C21 C22 1.496(9) . ?
C22 C23 1.517(8) . ?
C52 C53 1.517(11) . ?
C42 C43 1.488(8) . ?
C23 C24 1.486(10) . ?
C43 C44 1.493(9) . ?
C32 C33 1.453(11) . ?
C34 C33 1.502(12) . ?
V1 V2 3.0432(13) 3_657 ?
V1 V3 3.0243(14) 3_657 ?
V1 O5 1.799(4) 3_657 ?
V1 O7 1.855(4) 3_657 ?
C53 C54 1.371(12) . ?
C1AA C2AA 1.281(9) . ?

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
V3 V2 V1 65.41(3) 3_657 3_657 ?
O1 V2 V3 47.08(3) . 3_657 ?
O1 V2 V1 47.15(2) . 3_657 ?
O2 V2 V3 81.67(10) . 3_657 ?
O2 V2 O1 77.25(10) . . ?
O2 V2 V1 124.17(10) . 3_657 ?
O4 V2 V3 124.25(11) . 3_657 ?
O4 V2 O1 77.35(11) . . ?
O4 V2 O2 82.08(14) . . ?
O4 V2 V1 81.39(10) . 3_657 ?
O6 V2 V3 33.62(11) . 3_657 ?
O6 V2 O1 80.67(11) . . ?
O6 V2 O2 86.60(16) . . ?
O6 V2 O4 157.01(17) . . ?
O6 V2 V1 88.63(11) . 3_657 ?
O7 V2 V3 87.11(13) . 3_657 ?
O7 V2 O1 81.31(12) . . ?
O7 V2 O2 158.08(16) . . ?
O7 V2 O4 88.87(17) . . ?
O7 V2 O6 94.44(18) . . ?
O7 V2 V1 34.16(12) . 3_657 ?
O9 V2 V3 137.76(17) . 3_657 ?
O9 V2 O1 172.13(17) . . ?
O9 V2 O2 96.73(18) . . ?
O9 V2 O4 96.9(2) . . ?
O9 V2 O6 104.2(2) . . ?
O9 V2 O7 104.2(2) . . ?
O9 V2 V1 138.02(16) . 3_657 ?
V2 V3 V1 66.26(3) 3_657 3_657 ?
O1 V3 V2 48.00(3) . 3_657 ?
O1 V3 V1 47.55(3) . 3_657 ?
O3 V3 V2 82.09(11) . 3_657 ?
O3 V3 O1 78.46(10) . . ?
O3 V3 O4 83.12(14) . . ?
O3 V3 V1 125.83(11) . 3_657 ?
O4 V3 V2 125.03(11) . 3_657 ?
O4 V3 O1 77.21(11) . . ?
O4 V3 V1 81.21(11) . 3_657 ?
O5 V3 V2 88.41(12) . 3_657 ?
O5 V3 O1 81.00(12) . . ?
O5 V3 O3 158.69(16) . . ?
O5 V3 O4 86.88(15) . . ?
O5 V3 V1 33.45(11) . 3_657 ?
O6 V3 V2 34.56(12) 3_657 3_657 ?
O6 V3 O1 82.52(12) 3_657 . ?
O6 V3 O3 90.04(16) 3_657 . ?
O6 V3 O4 159.52(16) 3_657 . ?
O6 V3 O5 92.88(17) 3_657 . ?
O6 V3 V1 87.34(12) 3_657 3_657 ?
O10 V3 V2 137.99(17) . 3_657 ?
O10 V3 O1 172.17(15) . . ?
O10 V3 O3 96.73(19) . . ?
O10 V3 O4 96.18(19) . . ?
O10 V3 O5 103.0(2) . . ?
O10 V3 O6 103.8(2) . 3_657 ?
O10 V3 V1 136.28(17) . 3_657 ?
V2 O1 V2 180.00(5) . 3_657 ?
V3 O1 V2 95.09(4) 3_657 3_657 ?
V3 O1 V2 84.91(4) . 3_657 ?
V3 O1 V2 95.09(4) . . ?
V3 O1 V2 84.91(4) 3_657 . ?
V3 O1 V3 180.00(5) . 3_657 ?
V3 O1 V1 94.56(4) 3_657 3_657 ?
V3 O1 V1 85.44(4) 3_657 . ?
V3 O1 V1 94.57(4) . . ?
V3 O1 V1 85.43(4) . 3_657 ?
V1 O1 V2 85.32(4) 3_657 . ?
V1 O1 V2 94.68(4) . . ?
V1 O1 V2 85.32(4) . 3_657 ?
V1 O1 V2 94.68(4) 3_657 3_657 ?
V1 O1 V1 180.00(3) 3_657 . ?
C3 O2 V2 118.0(4) . . ?
C3 O2 V1 118.7(4) . . ?
V1 O2 V2 108.96(15) . . ?
V3 O3 V1 109.30(16) . . ?
C4 O3 V3 118.6(3) . . ?
C4 O3 V1 118.2(3) . . ?
V2 O4 V3 109.87(17) . . ?
C2 O4 V2 119.6(3) . . ?
C2 O4 V3 117.7(4) . . ?
V1 O5 V3 112.06(18) 3_657 . ?
V3 O6 V2 111.82(18) 3_657 . ?
V2 O7 V1 112.86(19) . 3_657 ?
O3 C4 C0AA 112.5(5) . . ?
C6 O11 C5 117.0(5) . . ?
O2 C3 C0AA 114.4(5) . . ?
O4 C2 C0AA 111.6(5) . . ?
C1 N13 C14 122.7(7) . . ?
C12 C7 C6 123.5(6) . . ?
C8 C7 C12 119.3(6) . . ?
C8 C7 C6 117.2(6) . . ?
C7 C12 C1 118.6(6) . . ?
C7 C12 C11 119.2(6) . . ?
C11 C12 C1 122.2(6) . . ?
O11 C5 C0AA 108.9(4) . . ?
O11 C6 C7 112.6(5) . . ?
O12 C6 O11 122.9(6) . . ?
O12 C6 C7 124.2(6) . . ?
O13 C1 N13 122.6(7) . . ?
O13 C1 C12 119.5(6) . . ?
N13 C1 C12 117.8(6) . . ?
C4 C0AA C2 110.8(5) . . ?
C4 C0AA C5 108.7(5) . . ?
C3 C0AA C4 110.3(5) . . ?
C3 C0AA C2 109.5(5) . . ?
C3 C0AA C5 107.3(5) . . ?
C5 C0AA C2 110.1(5) . . ?
C10 C11 C12 119.7(7) . . ?
C7 C8 C9 121.6(7) . . ?
C1AA C14 N13 117.5(9) . . ?
C10 C9 C8 117.8(7) . . ?
C11 C10 C9 122.4(8) . . ?
C51 N2 C41 108.3(4) . . ?
C51 N2 C31 109.9(5) . . ?
C31 N2 C41 112.3(5) . . ?
C21 N2 C51 110.2(5) . . ?
C21 N2 C41 108.2(4) . . ?
C21 N2 C31 107.9(5) . . ?
C52 C51 N2 117.4(5) . . ?
C42 C41 N2 115.8(5) . . ?
N2 C31 C32 115.3(6) . . ?
C22 C21 N2 118.0(5) . . ?
C21 C22 C23 111.0(6) . . ?
C51 C52 C53 112.1(7) . . ?
C43 C42 C41 111.9(5) . . ?
C24 C23 C22 113.7(7) . . ?
C42 C43 C44 115.0(6) . . ?
C33 C32 C31 113.9(7) . . ?
C32 C33 C34 114.9(8) . . ?
V3 V1 V2 65.87(3) 3_657 3_657 ?
O1 V1 V2 47.52(3) . 3_657 ?
O1 V1 V3 47.01(3) . 3_657 ?
O2 V1 V2 125.79(10) . 3_657 ?
O2 V1 V3 82.24(10) . 3_657 ?
O2 V1 O1 78.50(10) . . ?
O2 V1 O3 82.87(15) . . ?
O3 V1 V2 80.86(10) . 3_657 ?
O3 V1 V3 124.06(11) . 3_657 ?
O3 V1 O1 77.22(10) . . ?
O5 V1 V2 87.60(11) 3_657 3_657 ?
O5 V1 V3 34.48(11) 3_657 3_657 ?
O5 V1 O1 81.49(11) 3_657 . ?
O5 V1 O2 89.26(16) 3_657 . ?
O5 V1 O3 158.37(16) 3_657 . ?
O5 V1 O7 93.87(17) 3_657 3_657 ?
O7 V1 V2 32.97(11) 3_657 3_657 ?
O7 V1 V3 88.10(12) 3_657 3_657 ?
O7 V1 O1 80.49(12) 3_657 . ?
O7 V1 O2 158.05(16) 3_657 . ?
O7 V1 O3 86.37(16) 3_657 . ?
O8 V1 V2 136.30(16) . 3_657 ?
O8 V1 V3 137.92(16) . 3_657 ?
O8 V1 O1 173.11(15) . . ?
O8 V1 O2 96.85(18) . . ?
O8 V1 O3 97.26(19) . . ?
O8 V1 O5 103.68(19) . 3_657 ?
O8 V1 O7 103.47(19) . 3_657 ?
C54 C53 C52 118.5(9) . . ?
C2AA C1AA C14 132.7(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
