# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1495357'
_audit_update_record             
;
2017-11-12 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H72 N14 O30 Pd V10'
_chemical_formula_sum            'C52 H72 N14 O30 Pd V10'
_chemical_formula_weight         1957.03

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'
Pd Pd -0.9988 1.0072 '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                   11.353(6)
_cell_length_b                   13.219(7)
_cell_length_c                   13.408(7)
_cell_angle_alpha                89.754(8)
_cell_angle_beta                 77.245(8)
_cell_angle_gamma                64.976(7)
_cell_volume                     1769.2(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4149
_cell_measurement_theta_min      2.431
_cell_measurement_theta_max      28.529

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_F_000             982
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.593
_shelx_estimated_absorpt_T_min   0.721
_shelx_estimated_absorpt_T_max   0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7207
_exptl_absorpt_correction_T_max  0.8318
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9619
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.565
_diffrn_reflns_theta_max         25.549
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             6538
_reflns_number_gt                5408
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0037P)²+5.1740P] 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         6538
_refine_ls_number_parameters     536
_refine_ls_number_restraints     345
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.979
_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
Pd1 Pd 1.0000 0.5000 0.0000 0.03456(11) Uani 1 2 d S . P . .
V1 V 0.26942(5) -0.13904(5) 0.44168(4) 0.02687(13) Uani 1 1 d . . . . .
V2 V 0.17068(6) -0.13229(5) 0.67943(5) 0.03313(15) Uani 1 1 d . . . . .
V3 V 0.03872(5) 0.07606(4) 0.56976(4) 0.02138(12) Uani 1 1 d . . . . .
V4 V 0.11844(6) 0.07687(5) 0.33389(4) 0.02569(13) Uani 1 1 d . . . . .
V5 V -0.12427(6) 0.28172(5) 0.46747(5) 0.03239(15) Uani 1 1 d . . . . .
N1 N 0.9064(3) 0.3492(2) 0.1442(2) 0.0387(7) Uani 1 1 d . . . . .
H1 H 0.9256 0.3159 0.1976 0.046 Uiso 1 1 calc R U . . .
N2 N 0.8221(3) 0.5328(2) 0.0977(2) 0.0364(7) Uani 1 1 d . . . . .
N3 N 0.9870(3) 0.6548(2) 0.0273(2) 0.0364(7) Uani 1 1 d . . . . .
N4 N 0.7814(4) 0.3589(3) 0.7800(2) 0.0482(9) Uani 1 1 d . . . . .
H16 H 0.8049 0.3229 0.7203 0.058 Uiso 1 1 calc R U . . .
N5 N 0.7064(4) 0.5421(3) 0.8522(3) 0.0505(9) Uani 1 1 d . . . . .
N6 N 0.7626(3) 0.2040(3) 0.8386(2) 0.0373(7) Uani 1 1 d . . . . .
H6 H 0.7995 0.1730 0.7766 0.045 Uiso 1 1 calc R U . . .
N7 N 0.5732(4) 0.7719(3) 0.5766(3) 0.0595(10) Uani 1 1 d D U . . .
H7 H 0.4926 0.7957 0.5501 0.071 Uiso 1 1 calc DR U . A 1
O1 O -0.0635(2) 0.08814(16) 0.45564(15) 0.0209(4) Uani 1 1 d . . . . .
O2 O 0.1869(2) 0.02926(17) 0.45837(16) 0.0235(5) Uani 1 1 d . . . . .
O3 O 0.4058(2) -0.1630(2) 0.3588(2) 0.0400(6) Uani 1 1 d . . . . .
O4 O 0.2625(2) -0.27419(18) 0.43625(18) 0.0326(5) Uani 1 1 d . . . . .
O5 O 0.3122(2) -0.14702(19) 0.56228(18) 0.0317(5) Uani 1 1 d . . . . .
O6 O 0.2452(3) -0.1513(3) 0.7708(2) 0.0525(8) Uani 1 1 d . . . . .
O7 O 0.1163(2) 0.03348(19) 0.66544(17) 0.0291(5) Uani 1 1 d . . . . .
O8 O -0.1398(2) 0.08787(17) 0.65550(16) 0.0229(5) Uani 1 1 d . . . . .
O9 O 0.2545(2) 0.0518(2) 0.24979(18) 0.0380(6) Uani 1 1 d . . . . .
O10 O 0.0021(2) 0.0908(2) 0.25212(17) 0.0327(5) Uani 1 1 d . . . . .
O11 O -0.0156(2) 0.21624(18) 0.57530(17) 0.0291(5) Uani 1 1 d . . . . .
O12 O 0.0508(2) 0.21945(18) 0.37597(18) 0.0314(5) Uani 1 1 d . . . . .
O13 O -0.1936(2) 0.2733(2) 0.35902(19) 0.0378(6) Uani 1 1 d . . . . .
O14 O -0.1520(3) 0.4098(2) 0.4828(2) 0.0482(7) Uani 1 1 d . . . . .
C1 C 0.8063(4) 0.4575(3) 0.1595(3) 0.0359(8) Uani 1 1 d . . . . .
C2 C 0.6904(4) 0.4859(3) 0.2370(3) 0.0464(10) Uani 1 1 d . . . . .
H2 H 0.6838 0.4342 0.2826 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5868(4) 0.5892(4) 0.2460(3) 0.0544(11) Uani 1 1 d . . . . .
H3 H 0.5090 0.6088 0.2977 0.065 Uiso 1 1 calc R U . . .
C4 C 0.5980(4) 0.6655(4) 0.1771(3) 0.0528(11) Uani 1 1 d . . . . .
H4 H 0.5269 0.7355 0.1797 0.063 Uiso 1 1 calc R U . . .
C5 C 0.7159(4) 0.6346(3) 0.1058(3) 0.0452(10) Uani 1 1 d . . . . .
H5 H 0.7244 0.6857 0.0602 0.054 Uiso 1 1 calc R U . . .
C6 C 0.9331(4) 0.7100(4) 0.1233(3) 0.0465(10) Uani 1 1 d . . . . .
H6A H 0.9145 0.6710 0.1778 0.056 Uiso 1 1 calc R U . . .
C7 C 0.9052(5) 0.8194(4) 0.1431(3) 0.0540(11) Uani 1 1 d . . . . .
H7A H 0.8687 0.8546 0.2098 0.065 Uiso 1 1 calc R U . . .
C8 C 0.9320(5) 0.8773(4) 0.0624(4) 0.0579(12) Uani 1 1 d . . . . .
H8 H 0.9103 0.9532 0.0735 0.069 Uiso 1 1 calc R U . . .
C9 C 0.9905(4) 0.8229(3) -0.0338(3) 0.0490(10) Uani 1 1 d . . . . .
H9 H 1.0091 0.8610 -0.0890 0.059 Uiso 1 1 calc R U . . .
C10 C 1.0222(4) 0.7094(3) -0.0486(3) 0.0366(8) Uani 1 1 d . . . . .
C11 C 0.7221(5) 0.6369(4) 0.8517(4) 0.0572(12) Uani 1 1 d . . . . .
H11 H 0.6611 0.6963 0.9002 0.069 Uiso 1 1 calc R U . . .
C12 C 0.8209(5) 0.6525(4) 0.7851(4) 0.0545(12) Uani 1 1 d . . . . .
H12 H 0.8294 0.7192 0.7899 0.065 Uiso 1 1 calc R U . . .
C13 C 0.9085(4) 0.5661(4) 0.7101(4) 0.0518(11) Uani 1 1 d . . . . .
H13 H 0.9765 0.5738 0.6623 0.062 Uiso 1 1 calc R U . . .
C14 C 0.8931(4) 0.4691(3) 0.7076(3) 0.0452(10) Uani 1 1 d . . . . .
H14 H 0.9490 0.4105 0.6568 0.054 Uiso 1 1 calc R U . . .
C15 C 0.7934(4) 0.4595(3) 0.7815(3) 0.0395(9) Uani 1 1 d . . . . .
C16 C 0.7373(4) 0.3095(3) 0.8607(3) 0.0362(8) Uani 1 1 d . . . . .
C17 C 0.6723(4) 0.3622(4) 0.9609(3) 0.0496(11) Uani 1 1 d . . . . .
H17 H 0.6510 0.4373 0.9762 0.060 Uiso 1 1 calc R U . . .
C18 C 0.6413(5) 0.3012(4) 1.0346(3) 0.0548(12) Uani 1 1 d . . . . .
H18 H 0.5993 0.3346 1.1016 0.066 Uiso 1 1 calc R U . . .
C19 C 0.6712(5) 0.1902(4) 1.0117(3) 0.0552(12) Uani 1 1 d . . . . .
H19 H 0.6514 0.1474 1.0622 0.066 Uiso 1 1 calc R U . . .
C20 C 0.7310(4) 0.1455(4) 0.9122(3) 0.0480(10) Uani 1 1 d . . . . .
H20 H 0.7506 0.0711 0.8950 0.058 Uiso 1 1 calc R U . . .
C21 C 0.6506(9) 0.7423(10) 0.4590(6) 0.079(3) Uani 0.417(7) 1 d D U P B 2
H21A H 0.6275 0.6909 0.4252 0.095 Uiso 0.417(7) 1 calc DR U P B 2
H21B H 0.6297 0.8096 0.4235 0.095 Uiso 0.417(7) 1 calc DR U P B 2
C22 C 0.7929(10) 0.6895(13) 0.4609(13) 0.100(5) Uani 0.417(7) 1 d D U P B 2
H22A H 0.8072 0.7300 0.5127 0.150 Uiso 0.417(7) 1 calc R U P B 2
H22B H 0.8465 0.6907 0.3951 0.150 Uiso 0.417(7) 1 calc R U P B 2
H22C H 0.8179 0.6132 0.4763 0.150 Uiso 0.417(7) 1 calc R U P B 2
C23 C 0.5866(13) 0.8485(12) 0.6458(14) 0.086(4) Uani 0.417(7) 1 d D U P B 2
H23A H 0.6524 0.8722 0.6082 0.104 Uiso 0.417(7) 1 calc R U P B 2
H23B H 0.6221 0.8074 0.7006 0.104 Uiso 0.417(7) 1 calc R U P B 2
C24 C 0.4600(18) 0.9526(13) 0.6940(17) 0.083(5) Uani 0.417(7) 1 d D U P B 2
H24A H 0.4720 1.0183 0.6746 0.124 Uiso 0.417(7) 1 calc R U P B 2
H24B H 0.4417 0.9533 0.7675 0.124 Uiso 0.417(7) 1 calc R U P B 2
H24C H 0.3863 0.9521 0.6705 0.124 Uiso 0.417(7) 1 calc R U P B 2
C25 C 0.5781(12) 0.6652(8) 0.6235(9) 0.061(3) Uani 0.417(7) 1 d D U P B 2
H25A H 0.5105 0.6846 0.6878 0.073 Uiso 0.417(7) 1 calc R U P B 2
H25B H 0.6651 0.6228 0.6378 0.073 Uiso 0.417(7) 1 calc R U P B 2
C26 C 0.5526(13) 0.5933(10) 0.5484(9) 0.053(3) Uani 0.417(7) 1 d D U P B 2
H26A H 0.4602 0.6285 0.5460 0.079 Uiso 0.417(7) 1 calc R U P B 2
H26B H 0.5738 0.5201 0.5714 0.079 Uiso 0.417(7) 1 calc R U P B 2
H26C H 0.6082 0.5864 0.4811 0.079 Uiso 0.417(7) 1 calc R U P B 2
C21' C 0.6776(9) 0.8009(9) 0.5073(7) 0.084(3) Uani 0.583(7) 1 d D U P B 1
H21C H 0.6430 0.8820 0.5121 0.101 Uiso 0.583(7) 1 calc R U P B 1
H21D H 0.7567 0.7727 0.5347 0.101 Uiso 0.583(7) 1 calc R U P B 1
C22' C 0.7208(9) 0.7580(10) 0.3951(7) 0.086(3) Uani 0.583(7) 1 d D U P B 1
H22D H 0.7741 0.6782 0.3874 0.130 Uiso 0.583(7) 1 calc R U P B 1
H22E H 0.7726 0.7935 0.3576 0.130 Uiso 0.583(7) 1 calc R U P B 1
H22F H 0.6430 0.7748 0.3689 0.130 Uiso 0.583(7) 1 calc R U P B 1
C23' C 0.5422(9) 0.8356(7) 0.6799(6) 0.058(2) Uani 0.583(7) 1 d D U P B 1
H23C H 0.6219 0.8109 0.7063 0.070 Uiso 0.583(7) 1 calc R U P B 1
H23D H 0.4735 0.8240 0.7292 0.070 Uiso 0.583(7) 1 calc R U P B 1
C24' C 0.4925(14) 0.9604(8) 0.6603(13) 0.085(4) Uani 0.583(7) 1 d D U P B 1
H24D H 0.5503 0.9675 0.5994 0.128 Uiso 0.583(7) 1 calc R U P B 1
H24E H 0.4935 1.0026 0.7179 0.128 Uiso 0.583(7) 1 calc R U P B 1
H24F H 0.4029 0.9886 0.6514 0.128 Uiso 0.583(7) 1 calc R U P B 1
C25' C 0.6351(10) 0.6513(6) 0.5792(11) 0.084(3) Uani 0.583(7) 1 d D U P B 1
H25C H 0.6930 0.6334 0.6265 0.101 Uiso 0.583(7) 1 calc R U P B 1
H25D H 0.6911 0.6168 0.5114 0.101 Uiso 0.583(7) 1 calc R U P B 1
C26' C 0.5401(11) 0.6016(10) 0.6102(12) 0.100(4) Uani 0.583(7) 1 d D U P B 1
H26D H 0.5888 0.5218 0.6092 0.150 Uiso 0.583(7) 1 calc R U P B 1
H26E H 0.4831 0.6177 0.5633 0.150 Uiso 0.583(7) 1 calc R U P B 1
H26F H 0.4865 0.6329 0.6784 0.150 Uiso 0.583(7) 1 calc R U P B 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
Pd1 N3 2.017(3) . ?
Pd1 N3 2.017(3) 2_765 ?
Pd1 N2 2.020(3) . ?
Pd1 N2 2.020(3) 2_765 ?
V1 O3 1.600(2) . ?
V1 O5 1.779(3) . ?
V1 O4 1.824(2) . ?
V1 O2 2.007(2) . ?
V1 O8 2.078(2) 2_556 ?
V1 O1 2.252(2) 2_556 ?
V1 V5 3.0789(13) 2_556 ?
V1 V3 3.1064(13) . ?
V2 O6 1.598(3) . ?
V2 O10 1.813(3) 2_556 ?
V2 O13 1.829(3) 2_556 ?
V2 O5 1.926(3) . ?
V2 O7 2.030(3) . ?
V2 O1 2.338(2) 2_556 ?
V2 V5 3.0710(14) 2_556 ?
V2 V3 3.0725(14) . ?
V2 V4 3.0929(18) 2_556 ?
V3 O7 1.677(2) . ?
V3 O11 1.683(2) . ?
V3 O2 1.860(2) . ?
V3 O8 2.039(2) . ?
V3 O1 2.083(2) . ?
V3 O1 2.087(2) 2_556 ?
V3 V5 3.0868(13) . ?
V3 V4 3.0925(17) . ?
V4 O9 1.602(2) . ?
V4 O12 1.748(2) . ?
V4 O10 1.848(2) . ?
V4 O2 1.984(2) . ?
V4 O8 2.095(2) 2_556 ?
V4 O1 2.282(2) . ?
V4 V2 3.0928(18) 2_556 ?
V4 V5 3.1118(13) . ?
V5 O14 1.591(3) . ?
V5 O13 1.824(3) . ?
V5 O4 1.837(2) 2_556 ?
V5 O12 1.919(2) . ?
V5 O11 2.058(3) . ?
V5 O1 2.348(2) . ?
V5 V2 3.0710(14) 2_556 ?
V5 V1 3.0789(13) 2_556 ?
N1 C1 1.381(5) . ?
N1 C10 1.386(5) 2_765 ?
N2 C1 1.336(5) . ?
N2 C5 1.359(5) . ?
N3 C10 1.332(5) . ?
N3 C6 1.359(5) . ?
N4 C16 1.372(5) . ?
N4 C15 1.393(5) . ?
N5 C15 1.323(5) . ?
N5 C11 1.338(5) . ?
N6 C16 1.320(5) . ?
N6 C20 1.331(5) . ?
N7 C25' 1.449(7) . ?
N7 C23 1.453(9) . ?
N7 C21 1.586(6) . ?
N7 C23' 1.515(7) . ?
N7 C25 1.527(8) . ?
N7 C21' 1.520(7) . ?
O1 V3 2.087(2) 2_556 ?
O1 V1 2.252(2) 2_556 ?
O1 V2 2.338(2) 2_556 ?
O4 V5 1.837(2) 2_556 ?
O8 V1 2.078(2) 2_556 ?
O8 V4 2.095(2) 2_556 ?
O10 V2 1.813(3) 2_556 ?
O13 V2 1.829(3) 2_556 ?
C1 C2 1.392(5) . ?
C2 C3 1.358(6) . ?
C3 C4 1.391(6) . ?
C4 C5 1.360(6) . ?
C6 C7 1.357(6) . ?
C7 C8 1.377(6) . ?
C8 C9 1.358(6) . ?
C9 C10 1.390(5) . ?
C10 N1 1.386(5) 2_765 ?
C11 C12 1.361(6) . ?
C12 C13 1.383(6) . ?
C13 C14 1.366(6) . ?
C14 C15 1.380(5) . ?
C16 C17 1.403(5) . ?
C17 C18 1.353(6) . ?
C18 C19 1.378(6) . ?
C19 C20 1.363(6) . ?
C21 C22 1.470(9) . ?
C23 C24 1.518(9) . ?
C25 C26 1.539(9) . ?
C21' C22' 1.507(8) . ?
C23' C24' 1.543(9) . ?
C25' C26' 1.472(8) . ?

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
N3 Pd1 N3 180.0 . 2_765 ?
N3 Pd1 N2 94.29(12) . . ?
N3 Pd1 N2 85.71(12) 2_765 . ?
N3 Pd1 N2 85.71(12) . 2_765 ?
N3 Pd1 N2 94.29(12) 2_765 2_765 ?
N2 Pd1 N2 180.0 . 2_765 ?
O3 V1 O5 104.53(13) . . ?
O3 V1 O4 102.49(12) . . ?
O5 V1 O4 96.72(11) . . ?
O3 V1 O2 99.44(11) . . ?
O5 V1 O2 91.99(10) . . ?
O4 V1 O2 153.49(10) . . ?
O3 V1 O8 98.49(12) . 2_556 ?
O5 V1 O8 154.93(10) . 2_556 ?
O4 V1 O8 87.76(10) . 2_556 ?
O2 V1 O8 74.36(8) . 2_556 ?
O3 V1 O1 172.20(11) . 2_556 ?
O5 V1 O1 81.67(10) . 2_556 ?
O4 V1 O1 81.18(9) . 2_556 ?
O2 V1 O1 75.36(8) . 2_556 ?
O8 V1 O1 74.64(9) 2_556 2_556 ?
O3 V1 V5 135.15(10) . 2_556 ?
O5 V1 V5 83.88(8) . 2_556 ?
O4 V1 V5 32.88(7) . 2_556 ?
O2 V1 V5 124.59(7) . 2_556 ?
O8 V1 V5 86.80(7) 2_556 2_556 ?
O1 V1 V5 49.32(6) 2_556 2_556 ?
O3 V1 V3 133.76(10) . . ?
O5 V1 V3 77.73(8) . . ?
O4 V1 V3 123.36(8) . . ?
O2 V1 V3 34.98(6) . . ?
O8 V1 V3 79.24(7) 2_556 . ?
O1 V1 V3 42.19(5) 2_556 . ?
V5 V1 V3 91.06(5) 2_556 . ?
O6 V2 O10 102.45(13) . 2_556 ?
O6 V2 O13 103.30(14) . 2_556 ?
O10 V2 O13 92.28(11) 2_556 2_556 ?
O6 V2 O5 101.53(13) . . ?
O10 V2 O5 154.91(10) 2_556 . ?
O13 V2 O5 89.31(11) 2_556 . ?
O6 V2 O7 101.44(13) . . ?
O10 V2 O7 86.20(10) 2_556 . ?
O13 V2 O7 154.95(10) 2_556 . ?
O5 V2 O7 81.92(10) . . ?
O6 V2 O1 174.47(13) . 2_556 ?
O10 V2 O1 78.93(9) 2_556 2_556 ?
O13 V2 O1 81.93(9) 2_556 2_556 ?
O5 V2 O1 76.51(9) . 2_556 ?
O7 V2 O1 73.23(8) . 2_556 ?
O6 V2 V5 136.00(12) . 2_556 ?
O10 V2 V5 85.97(8) 2_556 2_556 ?
O13 V2 V5 32.74(8) 2_556 2_556 ?
O5 V2 V5 81.91(8) . 2_556 ?
O7 V2 V5 122.32(7) . 2_556 ?
O1 V2 V5 49.19(6) 2_556 2_556 ?
O6 V2 V3 131.91(12) . . ?
O10 V2 V3 81.66(8) 2_556 . ?
O13 V2 V3 124.57(9) 2_556 . ?
O5 V2 V3 76.89(7) . . ?
O7 V2 V3 30.50(6) . . ?
O1 V2 V3 42.74(5) 2_556 . ?
V5 V2 V3 91.86(4) 2_556 . ?
O6 V2 V4 134.84(11) . 2_556 ?
O10 V2 V4 32.69(8) 2_556 2_556 ?
O13 V2 V4 80.80(8) 2_556 2_556 ?
O5 V2 V4 123.60(8) . 2_556 ?
O7 V2 V4 84.62(7) . 2_556 ?
O1 V2 V4 47.20(5) 2_556 2_556 ?
V5 V2 V4 60.64(2) 2_556 2_556 ?
V3 V2 V4 64.92(2) . 2_556 ?
O7 V3 O11 106.55(11) . . ?
O7 V3 O2 99.79(11) . . ?
O11 V3 O2 100.97(10) . . ?
O7 V3 O8 93.52(11) . . ?
O11 V3 O8 93.09(10) . . ?
O2 V3 O8 156.93(9) . . ?
O7 V3 O1 164.21(10) . . ?
O11 V3 O1 87.98(10) . . ?
O2 V3 O1 83.05(10) . . ?
O8 V3 O1 79.23(9) . . ?
O7 V3 O1 87.39(10) . 2_556 ?
O11 V3 O1 164.61(10) . 2_556 ?
O2 V3 O1 82.57(9) . 2_556 ?
O8 V3 O1 79.27(8) . 2_556 ?
O1 V3 O1 77.53(9) . 2_556 ?
O7 V3 V2 37.91(8) . . ?
O11 V3 V2 144.12(8) . . ?
O2 V3 V2 92.58(7) . . ?
O8 V3 V2 86.39(7) . . ?
O1 V3 V2 126.86(6) . . ?
O1 V3 V2 49.48(6) 2_556 . ?
O7 V3 V5 144.97(8) . . ?
O11 V3 V5 38.55(8) . . ?
O2 V3 V5 92.40(7) . . ?
O8 V3 V5 87.25(7) . . ?
O1 V3 V5 49.47(6) . . ?
O1 V3 V5 126.92(7) 2_556 . ?
V2 V3 V5 173.29(3) . . ?
O7 V3 V4 137.57(9) . . ?
O11 V3 V4 86.11(8) . . ?
O2 V3 V4 37.82(7) . . ?
O8 V3 V4 126.77(6) . . ?
O1 V3 V4 47.54(6) . . ?
O1 V3 V4 87.84(6) 2_556 . ?
V2 V3 V4 122.36(3) . . ?
V5 V3 V4 60.47(3) . . ?
O7 V3 V1 85.39(9) . . ?
O11 V3 V1 139.15(8) . . ?
O2 V3 V1 38.19(7) . . ?
O8 V3 V1 125.71(7) . . ?
O1 V3 V1 87.52(7) . . ?
O1 V3 V1 46.44(6) 2_556 . ?
V2 V3 V1 60.76(4) . . ?
V5 V3 V1 121.99(4) . . ?
V4 V3 V1 61.66(3) . . ?
O9 V4 O12 105.21(12) . . ?
O9 V4 O10 101.77(13) . . ?
O12 V4 O10 96.36(11) . . ?
O9 V4 O2 101.19(12) . . ?
O12 V4 O2 93.17(10) . . ?
O10 V4 O2 151.82(10) . . ?
O9 V4 O8 98.95(11) . 2_556 ?
O12 V4 O8 154.65(10) . 2_556 ?
O10 V4 O8 86.01(10) . 2_556 ?
O2 V4 O8 74.46(8) . 2_556 ?
O9 V4 O1 172.54(11) . . ?
O12 V4 O1 81.75(9) . . ?
O10 V4 O1 79.79(10) . . ?
O2 V4 O1 75.42(9) . . ?
O8 V4 O1 73.81(8) 2_556 . ?
O9 V4 V3 135.61(10) . . ?
O12 V4 V3 78.07(8) . . ?
O10 V4 V3 122.13(8) . . ?
O2 V4 V3 35.11(6) . . ?
O8 V4 V3 79.34(6) 2_556 . ?
O1 V4 V3 42.34(5) . . ?
O9 V4 V2 133.61(10) . 2_556 ?
O12 V4 V2 83.97(8) . 2_556 ?
O10 V4 V2 32.01(7) . 2_556 ?
O2 V4 V2 123.99(6) . 2_556 ?
O8 V4 V2 84.94(6) 2_556 2_556 ?
O1 V4 V2 48.74(6) . 2_556 ?
V3 V4 V2 90.68(3) . 2_556 ?
O9 V4 V5 138.54(10) . . ?
O12 V4 V5 33.62(8) . . ?
O10 V4 V5 84.20(8) . . ?
O2 V4 V5 89.32(7) . . ?
O8 V4 V5 122.48(7) 2_556 . ?
O1 V4 V5 48.67(6) . . ?
V3 V4 V5 59.67(3) . . ?
V2 V4 V5 59.33(3) 2_556 . ?
O14 V5 O13 104.65(13) . . ?
O14 V5 O4 103.28(12) . 2_556 ?
O13 V5 O4 94.19(12) . 2_556 ?
O14 V5 O12 100.81(12) . . ?
O13 V5 O12 88.81(12) . . ?
O4 V5 O12 154.09(10) 2_556 . ?
O14 V5 O11 100.43(13) . . ?
O13 V5 O11 154.55(10) . . ?
O4 V5 O11 84.15(11) 2_556 . ?
O12 V5 O11 82.24(10) . . ?
O14 V5 O1 173.17(13) . . ?
O13 V5 O1 81.75(9) . . ?
O4 V5 O1 78.31(9) 2_556 . ?
O12 V5 O1 76.67(8) . . ?
O11 V5 O1 73.02(8) . . ?
O14 V5 V2 137.47(12) . 2_556 ?
O13 V5 V2 32.85(8) . 2_556 ?
O4 V5 V2 86.59(8) 2_556 2_556 ?
O12 V5 V2 82.06(8) . 2_556 ?
O11 V5 V2 121.85(7) . 2_556 ?
O1 V5 V2 48.90(6) . 2_556 ?
O14 V5 V1 135.69(10) . 2_556 ?
O13 V5 V1 82.12(8) . 2_556 ?
O4 V5 V1 32.62(7) 2_556 2_556 ?
O12 V5 V1 123.29(7) . 2_556 ?
O11 V5 V1 83.02(7) . 2_556 ?
O1 V5 V1 46.66(6) . 2_556 ?
V2 V5 V1 61.08(4) 2_556 2_556 ?
O14 V5 V3 130.97(12) . . ?
O13 V5 V3 123.97(8) . . ?
O4 V5 V3 80.86(8) 2_556 . ?
O12 V5 V3 76.19(7) . . ?
O11 V5 V3 30.65(6) . . ?
O1 V5 V3 42.41(5) . . ?
V2 V5 V3 91.20(4) 2_556 . ?
V1 V5 V3 64.17(4) 2_556 . ?
O14 V5 V4 131.06(10) . . ?
O13 V5 V4 80.33(9) . . ?
O4 V5 V4 125.17(8) 2_556 . ?
O12 V5 V4 30.29(7) . . ?
O11 V5 V4 79.99(7) . . ?
O1 V5 V4 46.87(5) . . ?
V2 V5 V4 60.03(4) 2_556 . ?
V1 V5 V4 93.19(5) 2_556 . ?
V3 V5 V4 59.85(4) . . ?
C1 N1 C10 124.4(3) . 2_765 ?
C1 N2 C5 117.9(3) . . ?
C1 N2 Pd1 121.4(2) . . ?
C5 N2 Pd1 120.7(3) . . ?
C10 N3 C6 117.6(3) . . ?
C10 N3 Pd1 121.5(2) . . ?
C6 N3 Pd1 120.7(3) . . ?
C16 N4 C15 128.8(3) . . ?
C15 N5 C11 116.5(4) . . ?
C16 N6 C20 120.1(3) . . ?
C23 N7 C21 123.0(9) . . ?
C25' N7 C23' 112.8(7) . . ?
C23 N7 C25 113.2(10) . . ?
C21 N7 C25 109.7(7) . . ?
C25' N7 C21' 106.5(7) . . ?
C23' N7 C21' 104.6(5) . . ?
V3 O1 V3 102.47(9) . 2_556 ?
V3 O1 V1 98.08(9) . 2_556 ?
V3 O1 V1 91.38(8) 2_556 2_556 ?
V3 O1 V4 90.12(9) . . ?
V3 O1 V4 98.40(8) 2_556 . ?
V1 O1 V4 165.62(10) 2_556 . ?
V3 O1 V2 168.88(10) . 2_556 ?
V3 O1 V2 87.78(8) 2_556 2_556 ?
V1 O1 V2 85.82(8) 2_556 2_556 ?
V4 O1 V2 84.06(8) . 2_556 ?
V3 O1 V5 88.12(7) . . ?
V3 O1 V5 168.97(11) 2_556 . ?
V1 O1 V5 84.02(7) 2_556 . ?
V4 O1 V5 84.46(7) . . ?
V2 O1 V5 81.91(7) 2_556 . ?
V3 O2 V4 107.07(11) . . ?
V3 O2 V1 106.83(10) . . ?
V4 O2 V1 105.52(10) . . ?
V1 O4 V5 114.51(12) . 2_556 ?
V1 O5 V2 114.99(12) . . ?
V3 O7 V2 111.60(11) . . ?
V3 O8 V1 105.40(10) . 2_556 ?
V3 O8 V4 106.35(9) . 2_556 ?
V1 O8 V4 99.17(9) 2_556 2_556 ?
V2 O10 V4 115.30(13) 2_556 . ?
V3 O11 V5 110.80(11) . . ?
V4 O12 V5 116.09(12) . . ?
V5 O13 V2 114.40(12) . 2_556 ?
N2 C1 N1 119.0(3) . . ?
N2 C1 C2 121.2(3) . . ?
N1 C1 C2 119.8(3) . . ?
C3 C2 C1 119.8(4) . . ?
C2 C3 C4 119.4(4) . . ?
C5 C4 C3 118.0(4) . . ?
N2 C5 C4 123.3(4) . . ?
C7 C6 N3 122.9(4) . . ?
C6 C7 C8 118.6(4) . . ?
C9 C8 C7 119.6(4) . . ?
C8 C9 C10 119.2(4) . . ?
N3 C10 N1 118.8(3) . 2_765 ?
N3 C10 C9 121.7(4) . . ?
N1 C10 C9 119.5(3) 2_765 . ?
N5 C11 C12 124.6(4) . . ?
C11 C12 C13 117.9(4) . . ?
C14 C13 C12 118.7(4) . . ?
C13 C14 C15 119.1(4) . . ?
N5 C15 C14 123.2(4) . . ?
N5 C15 N4 118.3(3) . . ?
C14 C15 N4 118.5(3) . . ?
N6 C16 N4 114.8(3) . . ?
N6 C16 C17 120.4(3) . . ?
N4 C16 C17 124.8(3) . . ?
C18 C17 C16 118.5(4) . . ?
C17 C18 C19 120.8(4) . . ?
C20 C19 C18 117.4(4) . . ?
N6 C20 C19 122.7(4) . . ?
C22 C21 N7 104.2(9) . . ?
N7 C23 C24 116.5(11) . . ?
N7 C25 C26 109.7(8) . . ?
C22' C21' N7 117.6(7) . . ?
N7 C23' C24' 105.7(8) . . ?
N7 C25' C26' 114.6(8) . . ?

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
O7 V3 O2 V4 -177.88(10) . . . . ?
O11 V3 O2 V4 -68.75(12) . . . . ?
O8 V3 O2 V4 57.8(3) . . . . ?
O1 V3 O2 V4 17.82(9) . . . . ?
O1 V3 O2 V4 96.08(10) 2_556 . . . ?
V2 V3 O2 V4 144.65(8) . . . . ?
V5 V3 O2 V4 -30.85(9) . . . . ?
V1 V3 O2 V4 112.67(14) . . . . ?
O7 V3 O2 V1 69.45(12) . . . . ?
O11 V3 O2 V1 178.58(11) . . . . ?
O8 V3 O2 V1 -54.9(3) . . . . ?
O1 V3 O2 V1 -94.85(10) . . . . ?
O1 V3 O2 V1 -16.59(10) 2_556 . . . ?
V2 V3 O2 V1 31.98(9) . . . . ?
V5 V3 O2 V1 -143.52(8) . . . . ?
V4 V3 O2 V1 -112.67(14) . . . . ?
O3 V1 O4 V5 174.22(14) . . . 2_556 ?
O5 V1 O4 V5 67.67(15) . . . 2_556 ?
O2 V1 O4 V5 -40.7(3) . . . 2_556 ?
O8 V1 O4 V5 -87.58(14) 2_556 . . 2_556 ?
O1 V1 O4 V5 -12.78(12) 2_556 . . 2_556 ?
V3 V1 O4 V5 -12.03(17) . . . 2_556 ?
O3 V1 O5 V2 -175.75(13) . . . . ?
O4 V1 O5 V2 -70.95(14) . . . . ?
O2 V1 O5 V2 83.96(13) . . . . ?
O8 V1 O5 V2 28.2(3) 2_556 . . . ?
O1 V1 O5 V2 9.08(11) 2_556 . . . ?
V5 V1 O5 V2 -40.62(11) 2_556 . . . ?
V3 V1 O5 V2 51.81(11) . . . . ?
O11 V3 O7 V2 173.82(11) . . . . ?
O2 V3 O7 V2 -81.55(12) . . . . ?
O8 V3 O7 V2 79.53(12) . . . . ?
O1 V3 O7 V2 17.6(4) . . . . ?
O1 V3 O7 V2 0.46(11) 2_556 . . . ?
V5 V3 O7 V2 169.78(5) . . . . ?
V4 V3 O7 V2 -83.47(14) . . . . ?
V1 V3 O7 V2 -46.04(10) . . . . ?
O9 V4 O10 V2 -174.85(14) . . . 2_556 ?
O12 V4 O10 V2 -67.82(14) . . . 2_556 ?
O2 V4 O10 V2 41.2(3) . . . 2_556 ?
O8 V4 O10 V2 86.83(13) 2_556 . . 2_556 ?
O1 V4 O10 V2 12.58(12) . . . 2_556 ?
V3 V4 O10 V2 12.06(17) . . . 2_556 ?
V5 V4 O10 V2 -36.41(12) . . . 2_556 ?
O7 V3 O11 V5 -176.28(11) . . . . ?
O2 V3 O11 V5 79.94(13) . . . . ?
O8 V3 O11 V5 -81.68(12) . . . . ?
O1 V3 O11 V5 -2.58(11) . . . . ?
O1 V3 O11 V5 -22.1(4) 2_556 . . . ?
V2 V3 O11 V5 -169.80(5) . . . . ?
V4 V3 O11 V5 44.99(10) . . . . ?
V1 V3 O11 V5 81.28(15) . . . . ?
O9 V4 O12 V5 173.51(14) . . . . ?
O10 V4 O12 V5 69.45(15) . . . . ?
O2 V4 O12 V5 -83.99(14) . . . . ?
O8 V4 O12 V5 -24.7(3) 2_556 . . . ?
O1 V4 O12 V5 -9.23(12) . . . . ?
V3 V4 O12 V5 -52.11(11) . . . . ?
V2 V4 O12 V5 39.87(12) 2_556 . . . ?
O14 V5 O13 V2 178.01(14) . . . 2_556 ?
O4 V5 O13 V2 -77.09(14) 2_556 . . 2_556 ?
O12 V5 O13 V2 77.14(14) . . . 2_556 ?
O11 V5 O13 V2 8.1(3) . . . 2_556 ?
O1 V5 O13 V2 0.44(12) . . . 2_556 ?
V1 V5 O13 V2 -46.72(12) 2_556 . . 2_556 ?
V3 V5 O13 V2 4.70(18) . . . 2_556 ?
V4 V5 O13 V2 47.90(12) . . . 2_556 ?
C5 N2 C1 N1 172.0(3) . . . . ?
Pd1 N2 C1 N1 -11.0(5) . . . . ?
C5 N2 C1 C2 -6.7(6) . . . . ?
Pd1 N2 C1 C2 170.4(3) . . . . ?
C10 N1 C1 N2 -40.0(6) 2_765 . . . ?
C10 N1 C1 C2 138.7(4) 2_765 . . . ?
N2 C1 C2 C3 4.8(6) . . . . ?
N1 C1 C2 C3 -173.8(4) . . . . ?
C1 C2 C3 C4 0.2(7) . . . . ?
C2 C3 C4 C5 -2.9(7) . . . . ?
C1 N2 C5 C4 3.8(6) . . . . ?
Pd1 N2 C5 C4 -173.3(3) . . . . ?
C3 C4 C5 N2 1.0(7) . . . . ?
C10 N3 C6 C7 4.9(6) . . . . ?
Pd1 N3 C6 C7 -170.7(3) . . . . ?
N3 C6 C7 C8 0.3(7) . . . . ?
C6 C7 C8 C9 -2.7(7) . . . . ?
C7 C8 C9 C10 0.0(7) . . . . ?
C6 N3 C10 N1 171.4(3) . . . 2_765 ?
Pd1 N3 C10 N1 -13.1(5) . . . 2_765 ?
C6 N3 C10 C9 -7.8(6) . . . . ?
Pd1 N3 C10 C9 167.8(3) . . . . ?
C8 C9 C10 N3 5.5(7) . . . . ?
C8 C9 C10 N1 -173.6(4) . . . 2_765 ?
C15 N5 C11 C12 -0.9(7) . . . . ?
N5 C11 C12 C13 2.6(7) . . . . ?
C11 C12 C13 C14 -1.1(7) . . . . ?
C12 C13 C14 C15 -1.8(6) . . . . ?
C11 N5 C15 C14 -2.4(6) . . . . ?
C11 N5 C15 N4 179.4(4) . . . . ?
C13 C14 C15 N5 3.7(6) . . . . ?
C13 C14 C15 N4 -178.0(4) . . . . ?
C16 N4 C15 N5 -32.4(6) . . . . ?
C16 N4 C15 C14 149.2(4) . . . . ?
C20 N6 C16 N4 176.3(4) . . . . ?
C20 N6 C16 C17 -2.5(6) . . . . ?
C15 N4 C16 N6 -166.8(4) . . . . ?
C15 N4 C16 C17 12.0(7) . . . . ?
N6 C16 C17 C18 2.6(6) . . . . ?
N4 C16 C17 C18 -176.1(4) . . . . ?
C16 C17 C18 C19 -0.8(7) . . . . ?
C17 C18 C19 C20 -0.9(7) . . . . ?
C16 N6 C20 C19 0.6(7) . . . . ?
C18 C19 C20 N6 1.1(7) . . . . ?
C23 N7 C21 C22 61.6(13) . . . . ?
C25 N7 C21 C22 -75.3(10) . . . . ?
C21 N7 C23 C24 118.9(17) . . . . ?
C25 N7 C23 C24 -105.5(18) . . . . ?
C23 N7 C25 C26 175.8(10) . . . . ?
C21 N7 C25 C26 -42.7(11) . . . . ?
C25' N7 C21' C22' 65.7(11) . . . . ?
C23' N7 C21' C22' -174.7(9) . . . . ?
C25' N7 C23' C24' 173.7(9) . . . . ?
C21' N7 C23' C24' 58.5(9) . . . . ?
C23' N7 C25' C26' 86.6(13) . . . . ?
C21' N7 C25' C26' -159.2(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O13 0.86 2.48 3.176(4) 138.0 1_655
N4 H16 O4 0.86 2.56 3.324(4) 148.8 2_656
N4 H16 O11 0.86 2.40 3.158(4) 147.2 1_655
N6 H6 O8 0.86 1.80 2.647(4) 167.5 1_655
N7 H7 O5 0.98 1.83 2.744(4) 154.4 1_565
C2 H2 O13 0.93 2.37 3.176(5) 144.9 1_655
C4 H4 O3 0.93 2.54 3.058(5) 115.3 1_565
C7 H7A O7 0.93 2.32 3.130(5) 145.5 2_666
C9 H9 O10 0.93 2.29 3.135(5) 150.6 2_665
C12 H12 O12 0.93 2.65 3.211(5) 119.3 2_666
C14 H14 O11 0.93 2.63 3.421(5) 143.6 1_655
C17 H17 N5 0.93 2.31 2.904(6) 121.3 .
C20 H20 O9 0.93 2.56 3.328(5) 139.9 2_656
C21 H21B O3 0.97 2.75 3.128(12) 104.2 1_565
C22 H22A O11 0.96 2.77 3.210(14) 108.6 2_666
C22 H22C O14 0.96 2.57 3.502(16) 164.6 1_655
C23 H23A O9 0.97 2.75 3.178(10) 107.4 2_666
C24 H24C O5 0.96 2.45 3.30(2) 146.6 1_565
C21' H21C O2 0.97 2.74 3.295(10) 116.8 2_666
C22' H22F O3 0.96 2.50 3.423(10) 162.1 1_565
C23' H23D O6 0.97 2.41 3.252(10) 145.7 1_565
C25' H25D O14 0.97 2.53 3.136(10) 120.6 1_655

_refine_diff_density_max         0.531
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.075

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_131105c
_database_code_depnum_ccdc_archive 'CCDC 975175'
_audit_update_record             
;
2017-11-12 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H52 N12 O36 Pd3 V10'
_chemical_formula_sum            'H52 N12 O36 Pd3 V10'
_chemical_formula_weight         1625.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Pd Pd -0.9988 1.0072 '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'

_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                   9.5424(8)
_cell_length_b                   11.2379(9)
_cell_length_c                   11.8608(11)
_cell_angle_alpha                115.251(2)
_cell_angle_beta                 108.0690(10)
_cell_angle_gamma                98.8730(10)
_cell_volume                     1031.12(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2854
_cell_measurement_theta_min      3.302
_cell_measurement_theta_max      28.171

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.542
_shelx_estimated_absorpt_T_min   0.437
_shelx_estimated_absorpt_T_max   0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4371
_exptl_absorpt_correction_T_max  0.5377
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5199
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.043
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             3550
_reflns_number_gt                2948
_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-2014/6 (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)+(0.0375P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3550
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0702
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pd1 Pd 0.74289(4) 0.73747(3) 0.46827(3) 0.02118(11) Uani 1 1 d . . . . .
Pd2 Pd 0.5000 0.0000 0.0000 0.02762(14) Uani 1 2 d S . P . .
V1 V 0.82880(8) 0.52193(7) -0.02165(7) 0.01721(17) Uani 1 1 d . . . . .
V2 V 0.68215(9) 0.20514(7) -0.15876(8) 0.02235(18) Uani 1 1 d . . . . .
V3 V 0.95304(9) 0.36566(7) 0.13542(7) 0.02080(18) Uani 1 1 d . . . . .
V4 V 1.11054(9) 0.68430(7) 0.27296(7) 0.02040(18) Uani 1 1 d . . . . .
V5 V 0.99813(9) 0.83626(7) 0.11405(8) 0.02347(19) Uani 1 1 d . . . . .
N1 N 0.7004(5) 0.6999(4) 0.2744(4) 0.0281(9) Uani 1 1 d . . . . .
H1A H 0.6027 0.6428 0.2172 0.042 Uiso 1 1 calc R U . . .
H1B H 0.7666 0.6605 0.2471 0.042 Uiso 1 1 calc R U . . .
H1C H 0.7132 0.7800 0.2743 0.042 Uiso 1 1 calc R U . . .
N2 N 0.8295(5) 0.5760(4) 0.4351(4) 0.0344(10) Uani 1 1 d . . . . .
H2A H 0.8775 0.5797 0.5145 0.052 Uiso 1 1 calc R U . . .
H2B H 0.8974 0.5828 0.3991 0.052 Uiso 1 1 calc R U . . .
H2C H 0.7513 0.4953 0.3773 0.052 Uiso 1 1 calc R U . . .
N3 N 0.7841(5) 0.7746(4) 0.6612(4) 0.0290(9) Uani 1 1 d . . . . .
H3A H 0.7753 0.8568 0.7097 0.044 Uiso 1 1 calc R U . . .
H3B H 0.8802 0.7756 0.7019 0.044 Uiso 1 1 calc R U . . .
H3C H 0.7148 0.7077 0.6564 0.044 Uiso 1 1 calc R U . . .
N4 N 0.6532(5) 0.8960(4) 0.4988(4) 0.0285(9) Uani 1 1 d . . . . .
H4A H 0.5493 0.8611 0.4593 0.043 Uiso 1 1 calc R U . . .
H4B H 0.6852 0.9428 0.4618 0.043 Uiso 1 1 calc R U . . .
H4C H 0.6860 0.9535 0.5885 0.043 Uiso 1 1 calc R U . . .
N5 N 0.6872(5) 0.1104(4) 0.1879(4) 0.0397(11) Uani 1 1 d . . . . .
H5A H 0.7245 0.0515 0.2096 0.060 Uiso 1 1 calc R U . . .
H5B H 0.6571 0.1618 0.2511 0.060 Uiso 1 1 calc R U . . .
H5C H 0.7614 0.1660 0.1848 0.060 Uiso 1 1 calc R U . . .
N6 N 0.3632(5) 0.0899(4) 0.0885(4) 0.0378(10) Uani 1 1 d . . . . .
H6A H 0.3138 0.0335 0.1090 0.057 Uiso 1 1 calc R U . . .
H6B H 0.2933 0.1042 0.0301 0.057 Uiso 1 1 calc R U . . .
H6C H 0.4229 0.1710 0.1649 0.057 Uiso 1 1 calc R U . . .
O1 O 0.6527(3) 0.3958(3) -0.0991(3) 0.0211(7) Uani 1 1 d . . . . .
O2 O 0.8966(3) 0.5377(3) 0.1550(3) 0.0180(6) Uani 1 1 d . . . . .
O3 O 1.0696(3) 0.6385(3) 0.0605(3) 0.0156(6) Uani 1 1 d . . . . .
O4 O 0.7921(3) 0.6745(3) 0.0220(3) 0.0206(6) Uani 1 1 d . . . . .
O5 O 0.8453(3) 0.4958(3) -0.1889(3) 0.0179(6) Uani 1 1 d . . . . .
O6 O 0.7462(3) 0.2610(3) 0.0279(3) 0.0218(7) Uani 1 1 d . . . . .
O7 O 0.6952(3) 0.2192(3) -0.3076(3) 0.0217(7) Uani 1 1 d . . . . .
O8 O 0.7896(3) 0.0797(3) -0.1826(3) 0.0235(7) Uani 1 1 d . . . . .
O9 O 0.5037(4) 0.1085(3) -0.2247(3) 0.0307(8) Uani 1 1 d . . . . .
O10 O 1.0263(3) 0.2245(3) 0.0664(3) 0.0233(7) Uani 1 1 d . . . . .
O11 O 0.9757(4) 0.3815(3) 0.2836(3) 0.0278(7) Uani 1 1 d . . . . .
O12 O 1.0249(3) 0.8171(3) 0.2689(3) 0.0212(7) Uani 1 1 d . . . . .
O13 O 1.1299(4) 0.7000(3) 0.4201(3) 0.0274(7) Uani 1 1 d . . . . .
O14 O 0.9323(4) 0.9648(3) 0.1466(3) 0.0302(8) Uani 1 1 d . . . . .
O20 O 0.5975(4) 0.5282(4) 0.6542(4) 0.0432(9) Uani 1 1 d . . . . .
H20C H 0.6753 0.5287 0.7141 0.052 Uiso 1 1 d R U . . .
H20B H 0.5169 0.5114 0.6687 0.052 Uiso 1 1 d R U . . .
O21 O 0.5381(4) 0.3771(3) 0.1361(3) 0.0412(9) Uani 1 1 d . . . . .
H21C H 0.5876 0.3365 0.0920 0.049 Uiso 1 1 d R U . . .
H21D H 0.4446 0.3541 0.0795 0.049 Uiso 1 1 d R U . . .
O22 O 0.5869(5) 0.3010(5) 0.4105(4) 0.0713(14) Uani 1 1 d . . . . .
H22C H 0.5748 0.3672 0.4728 0.086 Uiso 1 1 d R U . . .
H22D H 0.6707 0.2889 0.4483 0.086 Uiso 1 1 d R U . . .
O23 O 0.8700(5) 0.0209(4) 0.3992(4) 0.0504(10) Uani 1 1 d . . . . .
H23C H 0.8720 0.1038 0.4460 0.060 Uiso 1 1 d R U . . .
H23D H 0.9098 0.0199 0.3440 0.060 Uiso 1 1 d 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
Pd1 N3 2.035(4) . ?
Pd1 N4 2.038(4) . ?
Pd1 N1 2.043(4) . ?
Pd1 N2 2.046(4) . ?
Pd2 N6 2.044(4) 2_655 ?
Pd2 N6 2.044(4) . ?
Pd2 N5 2.046(4) 2_655 ?
Pd2 N5 2.046(4) . ?
V1 O4 1.695(3) . ?
V1 O1 1.695(3) . ?
V1 O2 1.910(3) . ?
V1 O5 1.939(3) . ?
V1 O3 2.124(3) 2_765 ?
V1 O3 2.130(3) . ?
V2 O9 1.603(3) . ?
V2 O8 1.845(3) . ?
V2 O6 1.877(3) . ?
V2 O7 1.878(3) . ?
V2 O1 2.046(3) . ?
V2 O3 2.305(3) 2_765 ?
V2 V5 3.0742(11) 2_765 ?
V2 V4 3.1034(10) 2_765 ?
V3 O11 1.629(3) . ?
V3 O10 1.807(3) . ?
V3 O6 1.830(3) . ?
V3 O5 2.001(3) 2_765 ?
V3 O2 2.024(3) . ?
V3 O3 2.245(3) 2_765 ?
V3 V5 3.0943(10) 2_765 ?
V4 O13 1.625(3) . ?
V4 O7 1.819(3) 2_765 ?
V4 O12 1.820(3) . ?
V4 O2 2.016(3) . ?
V4 O5 2.017(3) 2_765 ?
V4 O3 2.233(3) . ?
V4 V2 3.1035(10) 2_765 ?
V5 O14 1.608(3) . ?
V5 O8 1.841(3) 2_765 ?
V5 O10 1.870(3) 2_765 ?
V5 O12 1.884(3) . ?
V5 O4 2.057(3) . ?
V5 O3 2.311(3) . ?
V5 V2 3.0742(11) 2_765 ?
V5 V3 3.0943(10) 2_765 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
O3 V1 2.124(3) 2_765 ?
O3 V3 2.245(3) 2_765 ?
O3 V2 2.305(3) 2_765 ?
O5 V3 2.001(3) 2_765 ?
O5 V4 2.017(3) 2_765 ?
O7 V4 1.819(3) 2_765 ?
O8 V5 1.841(3) 2_765 ?
O10 V5 1.870(3) 2_765 ?
O20 H20C 0.8499 . ?
O20 H20B 0.8500 . ?
O21 H21C 0.8500 . ?
O21 H21D 0.8500 . ?
O22 H22C 0.8501 . ?
O22 H22D 0.8500 . ?
O23 H23C 0.8500 . ?
O23 H23D 0.8501 . ?

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
N3 Pd1 N4 90.81(15) . . ?
N3 Pd1 N1 179.72(15) . . ?
N4 Pd1 N1 89.06(15) . . ?
N3 Pd1 N2 89.64(16) . . ?
N4 Pd1 N2 179.07(16) . . ?
N1 Pd1 N2 90.49(16) . . ?
N6 Pd2 N6 180.0 2_655 . ?
N6 Pd2 N5 89.49(17) 2_655 2_655 ?
N6 Pd2 N5 90.51(17) . 2_655 ?
N6 Pd2 N5 90.51(17) 2_655 . ?
N6 Pd2 N5 89.49(17) . . ?
N5 Pd2 N5 180.0 2_655 . ?
O4 V1 O1 106.08(14) . . ?
O4 V1 O2 97.96(13) . . ?
O1 V1 O2 98.20(13) . . ?
O4 V1 O5 96.43(13) . . ?
O1 V1 O5 96.50(13) . . ?
O2 V1 O5 155.69(12) . . ?
O4 V1 O3 166.12(12) . 2_765 ?
O1 V1 O3 87.69(12) . 2_765 ?
O2 V1 O3 81.43(11) . 2_765 ?
O5 V1 O3 79.92(11) . 2_765 ?
O4 V1 O3 87.70(12) . . ?
O1 V1 O3 166.13(12) . . ?
O2 V1 O3 81.06(11) . . ?
O5 V1 O3 80.05(11) . . ?
O3 V1 O3 78.49(11) 2_765 . ?
O9 V2 O8 103.58(14) . . ?
O9 V2 O6 102.18(15) . . ?
O8 V2 O6 91.57(13) . . ?
O9 V2 O7 101.65(15) . . ?
O8 V2 O7 91.06(13) . . ?
O6 V2 O7 154.68(12) . . ?
O9 V2 O1 99.45(14) . . ?
O8 V2 O1 156.97(12) . . ?
O6 V2 O1 83.85(12) . . ?
O7 V2 O1 83.94(12) . . ?
O9 V2 O3 174.66(14) . 2_765 ?
O8 V2 O3 81.76(11) . 2_765 ?
O6 V2 O3 77.76(11) . 2_765 ?
O7 V2 O3 77.72(11) . 2_765 ?
O1 V2 O3 75.21(10) . 2_765 ?
O9 V2 V5 137.02(12) . 2_765 ?
O8 V2 V5 33.44(9) . 2_765 ?
O6 V2 V5 84.06(9) . 2_765 ?
O7 V2 V5 84.36(9) . 2_765 ?
O1 V2 V5 123.53(8) . 2_765 ?
O3 V2 V5 48.32(7) 2_765 2_765 ?
O9 V2 V4 133.89(12) . 2_765 ?
O8 V2 V4 81.62(9) . 2_765 ?
O6 V2 V4 123.66(9) . 2_765 ?
O7 V2 V4 32.32(9) . 2_765 ?
O1 V2 V4 82.23(8) . 2_765 ?
O3 V2 V4 45.90(7) 2_765 2_765 ?
V5 V2 V4 60.47(2) 2_765 2_765 ?
O11 V3 O10 101.97(14) . . ?
O11 V3 O6 102.51(14) . . ?
O10 V3 O6 95.64(13) . . ?
O11 V3 O5 100.64(14) . 2_765 ?
O10 V3 O5 90.28(12) . 2_765 ?
O6 V3 O5 154.32(12) . 2_765 ?
O11 V3 O2 100.53(13) . . ?
O10 V3 O2 155.54(12) . . ?
O6 V3 O2 88.73(12) . . ?
O5 V3 O2 76.20(11) 2_765 . ?
O11 V3 O3 175.63(13) . 2_765 ?
O10 V3 O3 80.96(12) . 2_765 ?
O6 V3 O3 80.30(11) . 2_765 ?
O5 V3 O3 75.98(10) 2_765 2_765 ?
O2 V3 O3 76.07(10) . 2_765 ?
O11 V3 V5 135.11(11) . 2_765 ?
O10 V3 V5 33.33(9) . 2_765 ?
O6 V3 V5 84.21(9) . 2_765 ?
O5 V3 V5 87.22(8) 2_765 2_765 ?
O2 V3 V5 124.15(8) . 2_765 ?
O3 V3 V5 48.12(7) 2_765 2_765 ?
O13 V4 O7 103.61(15) . 2_765 ?
O13 V4 O12 102.79(14) . . ?
O7 V4 O12 95.46(13) 2_765 . ?
O13 V4 O2 98.59(14) . . ?
O7 V4 O2 155.37(12) 2_765 . ?
O12 V4 O2 89.83(12) . . ?
O13 V4 O5 99.85(13) . 2_765 ?
O7 V4 O5 89.67(12) 2_765 2_765 ?
O12 V4 O5 154.86(12) . 2_765 ?
O2 V4 O5 76.03(11) . 2_765 ?
O13 V4 O3 173.82(13) . . ?
O7 V4 O3 80.81(11) 2_765 . ?
O12 V4 O3 80.86(11) . . ?
O2 V4 O3 76.31(10) . . ?
O5 V4 O3 75.69(10) 2_765 . ?
O13 V4 V2 136.96(11) . 2_765 ?
O7 V4 V2 33.50(9) 2_765 2_765 ?
O12 V4 V2 84.14(9) . 2_765 ?
O2 V4 V2 124.10(8) . 2_765 ?
O5 V4 V2 86.77(8) 2_765 2_765 ?
O3 V4 V2 47.84(7) . 2_765 ?
O14 V5 O8 103.57(14) . 2_765 ?
O14 V5 O10 102.25(15) . 2_765 ?
O8 V5 O10 91.81(13) 2_765 2_765 ?
O14 V5 O12 101.60(15) . . ?
O8 V5 O12 90.76(13) 2_765 . ?
O10 V5 O12 154.69(12) 2_765 . ?
O14 V5 O4 99.67(14) . . ?
O8 V5 O4 156.75(12) 2_765 . ?
O10 V5 O4 83.98(12) 2_765 . ?
O12 V5 O4 83.78(12) . . ?
O14 V5 O3 174.70(13) . . ?
O8 V5 O3 81.70(11) 2_765 . ?
O10 V5 O3 77.94(11) 2_765 . ?
O12 V5 O3 77.53(11) . . ?
O4 V5 O3 75.06(10) . . ?
O14 V5 V2 137.10(12) . 2_765 ?
O8 V5 V2 33.53(9) 2_765 2_765 ?
O10 V5 V2 84.32(9) 2_765 2_765 ?
O12 V5 V2 84.01(9) . 2_765 ?
O4 V5 V2 123.23(8) . 2_765 ?
O3 V5 V2 48.17(7) . 2_765 ?
O14 V5 V3 134.25(12) . 2_765 ?
O8 V5 V3 82.38(9) 2_765 2_765 ?
O10 V5 V3 32.06(9) 2_765 2_765 ?
O12 V5 V3 123.87(9) . 2_765 ?
O4 V5 V3 82.01(8) . 2_765 ?
O3 V5 V3 46.34(7) . 2_765 ?
V2 V5 V3 60.67(2) 2_765 2_765 ?
Pd1 N1 H1A 109.5 . . ?
Pd1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
Pd1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Pd1 N2 H2A 109.5 . . ?
Pd1 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
Pd1 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Pd1 N3 H3A 109.5 . . ?
Pd1 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
Pd1 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Pd1 N4 H4A 109.5 . . ?
Pd1 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
Pd1 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
Pd2 N5 H5A 109.5 . . ?
Pd2 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
Pd2 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
Pd2 N6 H6A 109.5 . . ?
Pd2 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
Pd2 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
V1 O1 V2 109.64(14) . . ?
V1 O2 V4 107.17(13) . . ?
V1 O2 V3 107.13(12) . . ?
V4 O2 V3 99.99(12) . . ?
V1 O3 V1 101.51(11) 2_765 . ?
V1 O3 V4 94.12(11) 2_765 . ?
V1 O3 V4 92.77(10) . . ?
V1 O3 V3 92.83(10) 2_765 2_765 ?
V1 O3 V3 93.34(10) . 2_765 ?
V4 O3 V3 169.65(13) . 2_765 ?
V1 O3 V2 87.44(10) 2_765 2_765 ?
V1 O3 V2 171.04(13) . 2_765 ?
V4 O3 V2 86.26(9) . 2_765 ?
V3 O3 V2 86.40(9) 2_765 2_765 ?
V1 O3 V5 170.89(13) 2_765 . ?
V1 O3 V5 87.54(10) . . ?
V4 O3 V5 86.38(9) . . ?
V3 O3 V5 85.54(9) 2_765 . ?
V2 O3 V5 83.51(9) 2_765 . ?
V1 O4 V5 109.69(15) . . ?
V1 O5 V3 107.80(13) . 2_765 ?
V1 O5 V4 107.51(13) . 2_765 ?
V3 O5 V4 100.75(12) 2_765 2_765 ?
V3 O6 V2 114.38(14) . . ?
V4 O7 V2 114.18(15) 2_765 . ?
V5 O8 V2 113.03(14) 2_765 . ?
V3 O10 V5 114.61(15) . 2_765 ?
V4 O12 V5 114.23(14) . . ?
H20C O20 H20B 109.5 . . ?
H21C O21 H21D 108.7 . . ?
H22C O22 H22D 108.0 . . ?
H23C O23 H23D 107.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.89 2.26 3.076(5) 151.4 2_665
N1 H1A O21 0.89 2.61 3.141(5) 118.7 .
N1 H1B O2 0.89 2.17 3.054(5) 171.2 .
N1 H1C O9 0.89 2.62 3.231(5) 126.5 2_665
N1 H1C O23 0.89 2.39 3.159(5) 144.7 1_565
N2 H2A O11 0.89 2.17 3.055(5) 170.5 2_766
N2 H2B O11 0.89 2.46 3.016(5) 120.7 .
N2 H2B O13 0.89 2.28 3.080(5) 149.6 .
N2 H2C O21 0.89 2.53 3.242(5) 137.4 .
N3 H3A O8 0.89 2.23 3.107(5) 167.8 1_566
N3 H3B O10 0.89 2.61 3.171(5) 121.5 2_766
N3 H3B O11 0.89 2.43 3.170(5) 141.0 2_766
N3 H3C O20 0.89 2.14 3.007(5) 165.4 .
N4 H4A O7 0.89 2.20 3.060(5) 161.2 2_665
N4 H4B O9 0.89 2.58 3.102(5) 118.6 2_665
N4 H4B O23 0.89 2.31 3.110(5) 150.2 1_565
N4 H4C O8 0.89 2.23 3.114(5) 172.0 1_566
N5 H5A O14 0.89 2.52 3.098(5) 123.5 1_545
N5 H5A O23 0.89 2.44 3.212(6) 144.7 .
N5 H5B O22 0.89 2.25 3.139(6) 177.1 .
N5 H5C O6 0.89 2.49 3.146(5) 130.8 .
N5 H5C O11 0.89 2.45 3.267(5) 153.5 .
N6 H6A O8 0.89 2.11 2.995(5) 173.0 2_655
N6 H6B O14 0.89 2.22 3.038(5) 152.7 2_665
N6 H6C O21 0.89 2.61 3.118(5) 117.1 .
N6 H6C O22 0.89 2.43 3.229(6) 149.5 .
O20 H20C O5 0.85 1.87 2.702(4) 167.0 1_556
O20 H20B O21 0.85 2.38 3.026(5) 132.7 2_666
O21 H21C O6 0.85 2.04 2.872(4) 167.4 .
O21 H21D O4 0.85 2.10 2.936(4) 167.6 2_665
O22 H22C O20 0.85 2.05 2.885(5) 165.7 .
O22 H22D O13 0.85 2.00 2.828(5) 165.5 2_766
O23 H23C O13 0.85 2.10 2.949(5) 172.0 2_766
O23 H23D O12 0.85 2.61 3.042(4) 112.4 1_545
O23 H23D O14 0.85 2.24 3.056(5) 160.2 1_545

_refine_diff_density_max         0.694
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.116

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1_sq_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 974935'
_audit_update_record             
;
2017-11-12 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H50 N4 O28 V10'
_chemical_formula_sum            'C16 H50 N4 O28 V10'
_chemical_formula_weight         1256.00

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'
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'
H H 0.0000 0.0000 '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                   12.6170(12)
_cell_length_b                   12.6550(12)
_cell_length_c                   15.6028(15)
_cell_angle_alpha                68.3170(10)
_cell_angle_beta                 83.535(2)
_cell_angle_gamma                78.824(2)
_cell_volume                     2268.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4950
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.045
_shelx_estimated_absorpt_T_min   0.570
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5697
_exptl_absorpt_correction_T_max  0.6395
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11291
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.406
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             7843
_reflns_number_gt                5909
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7843
_refine_ls_number_parameters     539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.2797
_refine_ls_wR_factor_gt          0.2033
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_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
V1 V 0.18496(8) 0.13307(8) 0.35041(6) 0.0197(3) Uani 1 1 d . . . . .
V2 V 0.08366(8) 0.33569(8) 0.16365(6) 0.0213(3) Uani 1 1 d . . . . .
V3 V 0.17153(8) 0.08135(9) 0.17135(7) 0.0256(3) Uani 1 1 d . . . . .
V4 V 0.09133(8) 0.40276(8) 0.33964(7) 0.0237(3) Uani 1 1 d . . . . .
V5 V -0.07835(7) 0.25411(8) 0.33185(6) 0.0218(3) Uani 1 1 d . . . . .
V6 V 0.33330(8) 0.23320(9) 0.17580(7) 0.0264(3) Uani 1 1 d . . . . .
V7 V 0.02015(8) -0.00867(8) 0.34079(6) 0.0238(3) Uani 1 1 d . . . . .
V8 V 0.24881(8) 0.48363(9) 0.16910(8) 0.0303(3) Uani 1 1 d . . . . .
V9 V -0.07357(8) 0.17647(9) 0.16438(7) 0.0264(3) Uani 1 1 d . . . . .
V10 V 0.33649(8) 0.29846(9) 0.34995(7) 0.0288(3) Uani 1 1 d . . . . .
O1 O -0.1649(4) 0.3093(4) 0.3944(3) 0.0352(10) Uani 1 1 d . . . . .
O2 O 0.0056(4) 0.4604(4) 0.4005(3) 0.0358(11) Uani 1 1 d . . . . .
O3 O 0.2580(4) 0.0218(4) 0.1124(3) 0.0384(11) Uani 1 1 d . . . . .
O4 O -0.0751(3) 0.0906(3) 0.4023(2) 0.0236(9) Uani 1 1 d . . . . .
H4 H -0.1099 0.0644 0.4535 0.028 Uiso 1 1 d R U . . .
O5 O 0.1264(3) -0.0471(3) 0.2668(3) 0.0260(9) Uani 1 1 d . . . . .
O6 O 0.4194(4) 0.1748(4) 0.1162(3) 0.0383(11) Uani 1 1 d . . . . .
O7 O 0.0629(3) 0.2328(3) 0.4030(3) 0.0232(9) Uani 1 1 d . . . . .
H7 H 0.0548 0.2091 0.4615 0.028 Uiso 1 1 d R U . . .
O8 O 0.1952(3) 0.2411(4) 0.1187(3) 0.0270(9) Uani 1 1 d . . . . .
O9 O 0.1357(3) 0.5213(3) 0.2490(3) 0.0281(9) Uani 1 1 d . . . . .
O10 O 0.1371(3) 0.0084(3) 0.4140(3) 0.0254(9) Uani 1 1 d . . . . .
O11 O 0.3436(3) 0.4391(4) 0.2615(3) 0.0352(10) Uani 1 1 d . . . . .
O12 O 0.0486(3) 0.1134(4) 0.1119(3) 0.0286(9) Uani 1 1 d . . . . .
O13 O 0.2687(3) 0.0884(3) 0.2636(3) 0.0252(9) Uani 1 1 d . . . . .
O14 O 0.3312(3) 0.3860(4) 0.1145(3) 0.0324(10) Uani 1 1 d . . . . .
O15 O 0.1235(3) 0.4618(4) 0.1076(3) 0.0290(10) Uani 1 1 d . . . . .
O16 O 0.2732(4) 0.6076(4) 0.1025(3) 0.0435(12) Uani 1 1 d . . . . .
O17 O -0.0074(3) 0.3807(3) 0.2583(3) 0.0243(9) Uani 1 1 d . . . . .
O18 O -0.0093(4) -0.1318(3) 0.4128(3) 0.0316(10) Uani 1 1 d . . . . .
O19 O -0.1660(4) 0.1907(4) 0.0965(3) 0.0391(11) Uani 1 1 d . . . . .
O20 O -0.0836(3) 0.0361(4) 0.2549(3) 0.0302(10) Uani 1 1 d . . . . .
O21 O 0.0588(3) 0.1675(3) 0.2622(3) 0.0217(9) Uani 1 1 d . . . . .
O22 O 0.1975(3) 0.2997(3) 0.2625(3) 0.0234(9) Uani 1 1 d . . . . .
O23 O 0.2794(3) 0.1438(4) 0.4131(3) 0.0264(9) Uani 1 1 d . . . . .
O24 O -0.0183(3) 0.3252(3) 0.1067(3) 0.0269(9) Uani 1 1 d . . . . .
O25 O -0.1531(3) 0.2534(4) 0.2444(3) 0.0305(10) Uani 1 1 d . . . . .
O26 O 0.4094(3) 0.2260(4) 0.2694(3) 0.0342(10) Uani 1 1 d . . . . .
O27 O 0.2129(3) 0.3575(4) 0.4056(3) 0.0304(10) Uani 1 1 d . . . . .
O28 O 0.4290(4) 0.2813(4) 0.4185(3) 0.0427(12) Uani 1 1 d . . . . .
N1 N 0.0440(4) 0.2060(4) 0.8616(3) 0.0305(11) Uani 1 1 d . . . . .
N2 N 0.6357(4) 0.9944(5) 0.3429(4) 0.0342(12) Uani 1 1 d . . . . .
N3 N 0.3072(5) 0.6782(4) 0.3775(4) 0.0397(13) Uani 1 1 d . . . . .
N4 N 0.6312(4) 0.4852(5) 0.1398(4) 0.0375(13) Uani 1 1 d . . . . .
C1 C 0.0521(8) 0.2493(6) 0.7586(4) 0.056(2) Uani 1 1 d . . . . .
H1A H 0.0505 0.1873 0.7376 0.084 Uiso 1 1 calc R U . . .
H1B H 0.1187 0.2786 0.7373 0.084 Uiso 1 1 calc R U . . .
H1C H -0.0076 0.3098 0.7348 0.084 Uiso 1 1 calc R U . . .
C2 C 0.0624(7) 0.3011(6) 0.8921(5) 0.0477(18) Uani 1 1 d . . . . .
H2A H 0.0060 0.3662 0.8703 0.072 Uiso 1 1 calc R U . . .
H2B H 0.1311 0.3235 0.8671 0.072 Uiso 1 1 calc R U . . .
H2C H 0.0617 0.2739 0.9583 0.072 Uiso 1 1 calc R U . . .
C8 C 0.7229(5) 0.8924(6) 0.3681(5) 0.0429(16) Uani 1 1 d . . . . .
H8A H 0.7892 0.9138 0.3356 0.064 Uiso 1 1 calc R U . . .
H8B H 0.7036 0.8329 0.3514 0.064 Uiso 1 1 calc R U . . .
H8C H 0.7322 0.8643 0.4334 0.064 Uiso 1 1 calc R U . . .
C3 C 0.1212(7) 0.0994(6) 0.9013(5) 0.058(2) Uani 1 1 d . . . . .
H3A H 0.1208 0.0792 0.9670 0.086 Uiso 1 1 calc R U . . .
H3B H 0.1925 0.1112 0.8751 0.086 Uiso 1 1 calc R U . . .
H3C H 0.1008 0.0383 0.8876 0.086 Uiso 1 1 calc R U . . .
C13 C 0.7403(6) 0.5178(7) 0.1122(6) 0.055(2) Uani 1 1 d . . . . .
H13A H 0.7939 0.4494 0.1269 0.082 Uiso 1 1 calc R U . . .
H13B H 0.7532 0.5648 0.1449 0.082 Uiso 1 1 calc R U . . .
H13C H 0.7442 0.5602 0.0470 0.082 Uiso 1 1 calc R U . . .
C7 C 0.6560(7) 1.0767(7) 0.3846(6) 0.058(2) Uani 1 1 d . . . . .
H7A H 0.6635 1.0377 0.4499 0.087 Uiso 1 1 calc R U . . .
H7B H 0.5964 1.1394 0.3737 0.087 Uiso 1 1 calc R U . . .
H7C H 0.7213 1.1061 0.3571 0.087 Uiso 1 1 calc R U . . .
C6 C 0.6341(6) 1.0538(7) 0.2389(5) 0.058(2) Uani 1 1 d . . . . .
H6A H 0.5809 1.1226 0.2237 0.087 Uiso 1 1 calc R U . . .
H6B H 0.6165 1.0029 0.2118 0.087 Uiso 1 1 calc R U . . .
H6C H 0.7041 1.0736 0.2152 0.087 Uiso 1 1 calc R U . . .
C11 C 0.1925(6) 0.6658(7) 0.3941(6) 0.058(2) Uani 1 1 d . . . . .
H11A H 0.1756 0.6372 0.4593 0.086 Uiso 1 1 calc R U . . .
H11B H 0.1785 0.6127 0.3676 0.086 Uiso 1 1 calc R U . . .
H11C H 0.1484 0.7395 0.3661 0.086 Uiso 1 1 calc R U . . .
C15 C 0.6153(6) 0.4369(8) 0.2454(5) 0.065(2) Uani 1 1 d . . . . .
H15A H 0.5549 0.3963 0.2623 0.097 Uiso 1 1 calc R U . . .
H15B H 0.6018 0.4992 0.2684 0.097 Uiso 1 1 calc R U . . .
H15C H 0.6794 0.3850 0.2716 0.097 Uiso 1 1 calc R U . . .
C5 C 0.5303(6) 0.9546(7) 0.3770(6) 0.063(2) Uani 1 1 d . . . . .
H5A H 0.5300 0.9170 0.4429 0.094 Uiso 1 1 calc R U . . .
H5B H 0.5199 0.9015 0.3491 0.094 Uiso 1 1 calc R U . . .
H5C H 0.4730 1.0197 0.3609 0.094 Uiso 1 1 calc R U . . .
C9 C 0.3229(7) 0.7695(8) 0.4121(6) 0.063(2) Uani 1 1 d . . . . .
H9A H 0.2625 0.8313 0.3964 0.095 Uiso 1 1 calc R U . . .
H9B H 0.3881 0.7986 0.3841 0.095 Uiso 1 1 calc R U . . .
H9C H 0.3282 0.7373 0.4779 0.095 Uiso 1 1 calc R U . . .
C4 C -0.0649(8) 0.1795(8) 0.8914(6) 0.067(3) Uani 1 1 d . . . . .
H4A H -0.0797 0.1270 0.8647 0.101 Uiso 1 1 calc R U . . .
H4B H -0.1166 0.2494 0.8715 0.101 Uiso 1 1 calc R U . . .
H4C H -0.0699 0.1450 0.9575 0.101 Uiso 1 1 calc R U . . .
C14 C 0.6183(7) 0.3951(8) 0.1030(6) 0.062(2) Uani 1 1 d . . . . .
H14A H 0.5589 0.3574 0.1357 0.093 Uiso 1 1 calc R U . . .
H14B H 0.6835 0.3394 0.1111 0.093 Uiso 1 1 calc R U . . .
H14C H 0.6043 0.4306 0.0385 0.093 Uiso 1 1 calc R U . . .
C12 C 0.3770(7) 0.5656(7) 0.4242(8) 0.076(3) Uani 1 1 d . . . . .
H12A H 0.4487 0.5664 0.3960 0.114 Uiso 1 1 calc R U . . .
H12B H 0.3474 0.5044 0.4182 0.114 Uiso 1 1 calc R U . . .
H12C H 0.3799 0.5534 0.4884 0.114 Uiso 1 1 calc R U . . .
C10 C 0.3306(9) 0.7216(9) 0.2735(6) 0.076(3) Uani 1 1 d . . . . .
H10A H 0.2792 0.7893 0.2446 0.113 Uiso 1 1 calc R U . . .
H10B H 0.3251 0.6627 0.2500 0.113 Uiso 1 1 calc R U . . .
H10C H 0.4024 0.7402 0.2602 0.113 Uiso 1 1 calc R U . . .
C16 C 0.5456(6) 0.5919(7) 0.1043(6) 0.061(2) Uani 1 1 d . . . . .
H16A H 0.5572 0.6286 0.0389 0.091 Uiso 1 1 calc R U . . .
H16B H 0.5505 0.6446 0.1344 0.091 Uiso 1 1 calc R U . . .
H16C H 0.4752 0.5700 0.1172 0.091 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O23 1.679(4) . ?
V1 O10 1.708(4) . ?
V1 O13 1.811(4) . ?
V1 O22 2.073(4) . ?
V1 O7 2.089(4) . ?
V1 O21 2.097(4) . ?
V2 O15 1.657(4) . ?
V2 O24 1.696(4) . ?
V2 O8 1.911(4) . ?
V2 O17 1.953(4) . ?
V2 O22 2.091(4) . ?
V2 O21 2.174(4) . ?
V3 O3 1.603(4) . ?
V3 O12 1.798(4) . ?
V3 O5 1.887(4) . ?
V3 O8 1.950(4) . ?
V3 O13 2.030(4) . ?
V3 O21 2.304(4) . ?
V4 O2 1.606(4) . ?
V4 O9 1.773(4) . ?
V4 O27 1.823(4) . ?
V4 O17 1.998(4) . ?
V4 O7 2.093(4) . ?
V4 O22 2.251(4) . ?
V5 O1 1.613(4) . ?
V5 O25 1.748(4) . ?
V5 O17 1.910(4) . ?
V5 O4 1.947(4) . ?
V5 O7 2.125(4) . ?
V5 O21 2.258(4) . ?
V6 O6 1.600(4) . ?
V6 O26 1.803(5) . ?
V6 O14 1.809(4) . ?
V6 O8 2.014(4) . ?
V6 O13 2.091(4) . ?
V6 O22 2.288(4) . ?
V7 O18 1.633(4) . ?
V7 O5 1.783(4) . ?
V7 O20 1.838(4) . ?
V7 O4 1.997(4) . ?
V7 O10 2.053(4) . ?
V7 O21 2.231(4) . ?
V8 O16 1.595(5) . ?
V8 O11 1.831(4) . ?
V8 O14 1.848(4) . ?
V8 O9 1.895(4) . ?
V8 O15 2.049(4) . ?
V8 O22 2.414(4) . ?
V9 O19 1.604(4) . ?
V9 O20 1.833(4) . ?
V9 O12 1.845(4) . ?
V9 O25 1.936(4) . ?
V9 O24 1.988(4) . ?
V9 O21 2.347(4) . ?
V10 O28 1.602(4) . ?
V10 O11 1.817(4) . ?
V10 O27 1.862(4) . ?
V10 O26 1.879(5) . ?
V10 O23 2.069(4) . ?
V10 O22 2.335(4) . ?
O4 H4 0.8501 . ?
O7 H7 0.8500 . ?
N1 C4 1.461(9) . ?
N1 C3 1.469(8) . ?
N1 C1 1.493(8) . ?
N1 C2 1.511(8) . ?
N2 C8 1.484(8) . ?
N2 C5 1.486(8) . ?
N2 C7 1.488(9) . ?
N2 C6 1.517(8) . ?
N3 C11 1.469(9) . ?
N3 C12 1.494(9) . ?
N3 C9 1.496(9) . ?
N3 C10 1.523(9) . ?
N4 C13 1.485(8) . ?
N4 C14 1.496(10) . ?
N4 C16 1.521(9) . ?
N4 C15 1.535(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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
O23 V1 O10 106.1(2) . . ?
O23 V1 O13 101.0(2) . . ?
O10 V1 O13 100.35(19) . . ?
O23 V1 O22 87.54(18) . . ?
O10 V1 O22 163.55(18) . . ?
O13 V1 O22 85.54(17) . . ?
O23 V1 O7 92.82(18) . . ?
O10 V1 O7 92.66(18) . . ?
O13 V1 O7 157.44(18) . . ?
O22 V1 O7 77.29(16) . . ?
O23 V1 O21 164.70(18) . . ?
O10 V1 O21 86.46(18) . . ?
O13 V1 O21 84.77(17) . . ?
O22 V1 O21 78.75(16) . . ?
O7 V1 O21 77.67(15) . . ?
O15 V2 O24 108.7(2) . . ?
O15 V2 O8 98.63(19) . . ?
O24 V2 O8 96.69(19) . . ?
O15 V2 O17 96.68(19) . . ?
O24 V2 O17 96.62(18) . . ?
O8 V2 O17 155.30(18) . . ?
O15 V2 O22 89.18(19) . . ?
O24 V2 O22 162.12(18) . . ?
O8 V2 O22 81.45(17) . . ?
O17 V2 O22 79.51(16) . . ?
O15 V2 O21 165.75(19) . . ?
O24 V2 O21 85.49(17) . . ?
O8 V2 O21 80.88(16) . . ?
O17 V2 O21 79.53(16) . . ?
O22 V2 O21 76.64(16) . . ?
O3 V3 O12 103.4(2) . . ?
O3 V3 O5 102.3(2) . . ?
O12 V3 O5 92.26(19) . . ?
O3 V3 O8 102.0(2) . . ?
O12 V3 O8 92.78(19) . . ?
O5 V3 O8 153.29(17) . . ?
O3 V3 O13 100.5(2) . . ?
O12 V3 O13 155.70(18) . . ?
O5 V3 O13 86.95(18) . . ?
O8 V3 O13 77.87(17) . . ?
O3 V3 O21 175.3(2) . . ?
O12 V3 O21 81.22(16) . . ?
O5 V3 O21 78.11(15) . . ?
O8 V3 O21 76.79(15) . . ?
O13 V3 O21 74.85(15) . . ?
O2 V4 O9 104.5(2) . . ?
O2 V4 O27 102.8(2) . . ?
O9 V4 O27 96.8(2) . . ?
O2 V4 O17 100.7(2) . . ?
O9 V4 O17 92.50(19) . . ?
O27 V4 O17 151.64(18) . . ?
O2 V4 O7 98.38(19) . . ?
O9 V4 O7 155.32(18) . . ?
O27 V4 O7 87.00(18) . . ?
O17 V4 O7 74.01(16) . . ?
O2 V4 O22 171.38(19) . . ?
O9 V4 O22 83.24(17) . . ?
O27 V4 O22 79.75(17) . . ?
O17 V4 O22 74.79(16) . . ?
O7 V4 O22 73.40(15) . . ?
O1 V5 O25 104.9(2) . . ?
O1 V5 O17 102.6(2) . . ?
O25 V5 O17 97.02(19) . . ?
O1 V5 O4 100.4(2) . . ?
O25 V5 O4 93.80(19) . . ?
O17 V5 O4 150.98(17) . . ?
O1 V5 O7 98.44(19) . . ?
O25 V5 O7 156.48(17) . . ?
O17 V5 O7 75.03(16) . . ?
O4 V5 O7 84.40(16) . . ?
O1 V5 O21 171.48(19) . . ?
O25 V5 O21 83.26(17) . . ?
O17 V5 O21 78.28(16) . . ?
O4 V5 O21 76.35(15) . . ?
O7 V5 O21 73.50(14) . . ?
O6 V6 O26 103.9(2) . . ?
O6 V6 O14 103.5(2) . . ?
O26 V6 O14 94.8(2) . . ?
O6 V6 O8 100.4(2) . . ?
O26 V6 O8 153.01(18) . . ?
O14 V6 O8 90.66(19) . . ?
O6 V6 O13 99.7(2) . . ?
O26 V6 O13 89.40(19) . . ?
O14 V6 O13 154.64(18) . . ?
O8 V6 O13 75.09(17) . . ?
O6 V6 O22 172.8(2) . . ?
O26 V6 O22 80.06(17) . . ?
O14 V6 O22 81.93(17) . . ?
O8 V6 O22 74.55(15) . . ?
O13 V6 O22 74.16(15) . . ?
O18 V7 O5 104.5(2) . . ?
O18 V7 O20 102.5(2) . . ?
O5 V7 O20 94.3(2) . . ?
O18 V7 O4 96.74(19) . . ?
O5 V7 O4 157.77(17) . . ?
O20 V7 O4 87.39(18) . . ?
O18 V7 O10 98.41(19) . . ?
O5 V7 O10 87.58(18) . . ?
O20 V7 O10 157.74(18) . . ?
O4 V7 O10 82.75(16) . . ?
O18 V7 O21 170.82(18) . . ?
O5 V7 O21 82.20(16) . . ?
O20 V7 O21 82.97(16) . . ?
O4 V7 O21 76.01(14) . . ?
O10 V7 O21 75.30(15) . . ?
O16 V8 O11 104.3(2) . . ?
O16 V8 O14 103.0(2) . . ?
O11 V8 O14 91.9(2) . . ?
O16 V8 O9 102.3(2) . . ?
O11 V8 O9 89.7(2) . . ?
O14 V8 O9 153.47(19) . . ?
O16 V8 O15 102.7(2) . . ?
O11 V8 O15 152.95(18) . . ?
O14 V8 O15 83.90(19) . . ?
O9 V8 O15 82.69(18) . . ?
O16 V8 O22 174.9(2) . . ?
O11 V8 O22 80.69(16) . . ?
O14 V8 O22 77.72(16) . . ?
O9 V8 O22 76.42(15) . . ?
O15 V8 O22 72.30(15) . . ?
O19 V9 O20 102.8(2) . . ?
O19 V9 O12 102.8(2) . . ?
O20 V9 O12 91.1(2) . . ?
O19 V9 O25 100.7(2) . . ?
O20 V9 O25 90.08(19) . . ?
O12 V9 O25 155.59(19) . . ?
O19 V9 O24 102.4(2) . . ?
O20 V9 O24 154.62(18) . . ?
O12 V9 O24 86.27(18) . . ?
O25 V9 O24 82.28(18) . . ?
O19 V9 O21 176.6(2) . . ?
O20 V9 O21 79.87(16) . . ?
O12 V9 O21 79.12(16) . . ?
O25 V9 O21 77.10(15) . . ?
O24 V9 O21 74.85(16) . . ?
O28 V10 O11 104.2(2) . . ?
O28 V10 O27 102.9(2) . . ?
O11 V10 O27 91.6(2) . . ?
O28 V10 O26 102.2(2) . . ?
O11 V10 O26 90.5(2) . . ?
O27 V10 O26 153.6(2) . . ?
O28 V10 O23 100.2(2) . . ?
O11 V10 O23 155.59(19) . . ?
O27 V10 O23 83.99(18) . . ?
O26 V10 O23 83.33(18) . . ?
O28 V10 O22 172.6(2) . . ?
O11 V10 O22 83.20(17) . . ?
O27 V10 O22 76.75(16) . . ?
O26 V10 O22 77.33(17) . . ?
O23 V10 O22 72.41(15) . . ?
V5 O4 V7 112.20(18) . . ?
V5 O4 H4 123.9 . . ?
V7 O4 H4 123.9 . . ?
V7 O5 V3 113.4(2) . . ?
V1 O7 V4 105.81(17) . . ?
V1 O7 V5 106.36(17) . . ?
V4 O7 V5 96.62(16) . . ?
V1 O7 H7 115.3 . . ?
V4 O7 H7 115.4 . . ?
V5 O7 H7 115.3 . . ?
V2 O8 V3 109.66(19) . . ?
V2 O8 V6 107.4(2) . . ?
V3 O8 V6 102.15(18) . . ?
V4 O9 V8 115.8(2) . . ?
V1 O10 V7 107.8(2) . . ?
V10 O11 V8 115.2(2) . . ?
V3 O12 V9 116.1(2) . . ?
V1 O13 V3 108.7(2) . . ?
V1 O13 V6 106.08(19) . . ?
V3 O13 V6 96.91(17) . . ?
V6 O14 V8 116.4(2) . . ?
V2 O15 V8 112.3(2) . . ?
V5 O17 V2 107.78(19) . . ?
V5 O17 V4 107.41(19) . . ?
V2 O17 V4 106.98(18) . . ?
V9 O20 V7 112.9(2) . . ?
V1 O21 V2 100.28(16) . . ?
V1 O21 V7 89.41(14) . . ?
V2 O21 V7 169.0(2) . . ?
V1 O21 V5 101.51(16) . . ?
V2 O21 V5 89.52(14) . . ?
V7 O21 V5 93.64(14) . . ?
V1 O21 V3 90.35(14) . . ?
V2 O21 V3 89.61(14) . . ?
V7 O21 V3 85.13(13) . . ?
V5 O21 V3 168.07(19) . . ?
V1 O21 V9 171.08(19) . . ?
V2 O21 V9 86.01(13) . . ?
V7 O21 V9 83.80(14) . . ?
V5 O21 V9 84.75(13) . . ?
V3 O21 V9 83.32(13) . . ?
V1 O22 V2 103.88(18) . . ?
V1 O22 V4 100.93(16) . . ?
V2 O22 V4 93.94(15) . . ?
V1 O22 V6 91.34(15) . . ?
V2 O22 V6 92.42(15) . . ?
V4 O22 V6 164.4(2) . . ?
V1 O22 V10 88.96(14) . . ?
V2 O22 V10 167.0(2) . . ?
V4 O22 V10 85.57(14) . . ?
V6 O22 V10 85.04(13) . . ?
V1 O22 V8 168.6(2) . . ?
V2 O22 V8 86.17(14) . . ?
V4 O22 V8 83.50(13) . . ?
V6 O22 V8 82.73(13) . . ?
V10 O22 V8 80.86(13) . . ?
V1 O23 V10 110.8(2) . . ?
V2 O24 V9 113.5(2) . . ?
V5 O25 V9 114.7(2) . . ?
V6 O26 V10 116.1(2) . . ?
V4 O27 V10 115.5(2) . . ?
C4 N1 C3 107.8(7) . . ?
C4 N1 C1 108.0(6) . . ?
C3 N1 C1 111.4(5) . . ?
C4 N1 C2 109.8(6) . . ?
C3 N1 C2 112.0(6) . . ?
C1 N1 C2 107.8(5) . . ?
C8 N2 C5 108.5(6) . . ?
C8 N2 C7 109.0(5) . . ?
C5 N2 C7 111.6(6) . . ?
C8 N2 C6 110.3(5) . . ?
C5 N2 C6 108.5(6) . . ?
C7 N2 C6 109.0(6) . . ?
C11 N3 C12 110.3(6) . . ?
C11 N3 C9 107.5(6) . . ?
C12 N3 C9 112.1(7) . . ?
C11 N3 C10 107.6(7) . . ?
C12 N3 C10 111.3(7) . . ?
C9 N3 C10 107.8(6) . . ?
C13 N4 C14 109.7(6) . . ?
C13 N4 C16 109.4(6) . . ?
C14 N4 C16 111.2(6) . . ?
C13 N4 C15 110.6(6) . . ?
C14 N4 C15 108.7(6) . . ?
C16 N4 C15 107.1(6) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C16 H16C O16 0.96 2.52 3.408(9) 153.5 .
C10 H10A O5 0.96 2.64 3.483(11) 147.0 1_565
C14 H14B O19 0.96 2.46 3.393(10) 164.9 1_655
C4 H4C O19 0.96 2.56 3.351(10) 139.4 1_556
C4 H4B O16 0.96 2.51 3.401(11) 153.4 2_566
C9 H9C O1 0.96 2.69 3.358(10) 127.1 2_566
C9 H9A O10 0.96 2.57 3.455(10) 154.1 1_565
C9 H9A O5 0.96 2.62 3.437(10) 143.3 1_565
C5 H5C O26 0.96 2.49 3.350(10) 149.4 1_565
C15 H15C O25 0.96 2.53 3.364(9) 145.9 1_655
C15 H15A O11 0.96 2.62 3.404(9) 139.6 .
C11 H11C O18 0.96 2.54 3.314(9) 138.1 1_565
C6 H6C O19 0.96 2.56 3.447(9) 154.1 1_665
C6 H6A O26 0.96 2.48 3.329(9) 147.5 1_565
C6 H6A O6 0.96 2.61 3.278(9) 126.5 1_565
C7 H7A O23 0.96 2.54 3.406(10) 150.4 2_666
C13 H13C O14 0.96 2.60 3.452(10) 148.7 2_665
C13 H13A O25 0.96 2.50 3.322(9) 144.1 1_655
C13 H13A O24 0.96 2.63 3.528(9) 155.1 1_655
C3 H3A O12 0.96 2.50 3.371(9) 151.1 1_556
C8 H8C O23 0.96 2.35 3.271(8) 160.9 2_666
C8 H8A O20 0.96 2.37 3.281(9) 158.0 1_665
C2 H2C O12 0.96 2.52 3.382(9) 149.7 1_556
C2 H2A O15 0.96 2.56 3.433(9) 150.7 2_566
C2 H2A O9 0.96 2.55 3.399(9) 147.7 2_566
C1 H1C O9 0.96 2.49 3.347(9) 148.1 2_566
O7 H7 O18 0.85 1.92 2.745(5) 163.8 2_556
O4 H4 O10 0.85 1.95 2.759(5) 159.3 2_556

_refine_diff_density_max         1.367
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.271

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 975174'
_audit_update_record             
;
2017-11-12 deposited with the CCDC.
2017-11-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H42 N8 O32 Pd2 V10'
_chemical_formula_sum            'C8 H42 N8 O32 Pd2 V10'
_chemical_formula_weight         1484.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Pd Pd -0.9988 1.0072 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.715(7)
_cell_length_b                   10.642(7)
_cell_length_c                   19.195(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.083(12)
_cell_angle_gamma                90
_cell_volume                     1982(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4311
_cell_measurement_theta_min      2.189
_cell_measurement_theta_max      28.120

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.233
_shelx_estimated_absorpt_T_min   0.487
_shelx_estimated_absorpt_T_max   0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4869
_exptl_absorpt_correction_T_max  0.5641
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8598
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.125
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.925
_reflns_number_total             3314
_reflns_number_gt                2650
_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-2014/6 (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)+(0.1856P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3314
_refine_ls_number_parameters     271
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.2518
_refine_ls_wR_factor_gt          0.2254
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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
Pd1 Pd 0.68179(8) 0.14697(6) 0.16126(4) 0.0397(4) Uani 1 1 d . . . . .
V1 V 0.63534(15) 0.43200(12) 0.03894(7) 0.0293(4) Uani 1 1 d . . . . .
V2 V 0.64187(18) 0.65211(13) 0.14611(8) 0.0363(5) Uani 1 1 d . . . . .
V3 V 0.37257(16) 0.49022(13) 0.12290(7) 0.0328(4) Uani 1 1 d . . . . .
V4 V 0.34705(16) 0.28692(12) 0.01298(8) 0.0338(5) Uani 1 1 d . . . . .
V5 V 0.60406(17) 0.21658(12) -0.06676(8) 0.0375(5) Uani 1 1 d . . . . .
N1 N 0.6778(10) 0.2852(7) 0.2357(4) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.6253 0.3488 0.2201 0.057 Uiso 1 1 calc R U . . .
H1B H 0.6429 0.2551 0.2742 0.057 Uiso 1 1 calc R U . . .
N2 N 0.8870(9) 0.1828(7) 0.1641(4) 0.047(2) Uani 1 1 d . . . . .
H2 H 0.9025 0.2506 0.1309 0.057 Uiso 1 1 calc DR U . . .
N3 N 0.7242(11) 0.0115(8) 0.0901(5) 0.060(3) Uani 1 1 d . . . . .
H3A H 0.7071 -0.0643 0.1072 0.073 Uiso 1 1 calc R U . . .
H3B H 0.6714 0.0222 0.0512 0.073 Uiso 1 1 calc R U . . .
N4 N 0.0174(10) 0.6541(10) 0.0706(6) 0.067(3) Uani 1 1 d . . . . .
H4C H -0.0426 0.6255 0.1018 0.081 Uiso 1 1 d R U . . .
H4D H -0.0151 0.7275 0.0516 0.081 Uiso 1 1 d R U . . .
H4F H 0.0256 0.5960 0.0363 0.081 Uiso 1 1 d R U . . .
H4E H 0.1016 0.6670 0.0927 0.081 Uiso 1 1 d R U . . .
O1 O 0.7211(6) 0.5408(5) -0.0258(3) 0.0319(13) Uani 1 1 d . . . . .
O2 O 0.7214(7) 0.4862(5) 0.1134(3) 0.0376(15) Uani 1 1 d . . . . .
O3 O 0.4822(7) 0.3553(5) 0.0865(3) 0.0334(14) Uani 1 1 d . . . . .
O4 O 0.7100(6) 0.2938(5) 0.0174(3) 0.0353(14) Uani 1 1 d . . . . .
O5 O 0.7418(7) 0.7242(5) 0.0755(3) 0.0379(14) Uani 1 1 d . . . . .
O6 O 0.7424(8) 0.6751(7) 0.2149(4) 0.0515(18) Uani 1 1 d . . . . .
O7 O 0.5180(7) 0.7851(5) 0.1432(3) 0.0387(15) Uani 1 1 d . . . . .
O8 O 0.5063(7) 0.5417(6) 0.1844(3) 0.0389(15) Uani 1 1 d . . . . .
O9 O 0.2843(7) 0.6574(5) 0.1180(3) 0.0360(14) Uani 1 1 d . . . . .
O10 O 0.2653(8) 0.4147(7) 0.1691(4) 0.0528(19) Uani 1 1 d . . . . .
O11 O 0.2435(7) 0.2097(5) 0.0605(4) 0.0457(17) Uani 1 1 d . . . . .
O12 O 0.4778(7) 0.1635(5) -0.0070(3) 0.0364(14) Uani 1 1 d . . . . .
O13 O 0.6984(8) 0.0940(6) -0.0773(4) 0.0519(19) Uani 1 1 d . . . . .
O14 O 0.4959(6) 0.4063(4) -0.0470(3) 0.0274(12) Uani 1 1 d . . . . .
O15 O 0.4732(10) 0.1038(8) 0.1642(4) 0.067(2) Uani 1 1 d . . . . .
H15A H 0.4576 0.0684 0.2027 0.080 Uiso 1 1 d R U . . .
H15B H 0.4485 0.0543 0.1311 0.080 Uiso 1 1 d R U . . .
O16 O 0.9994(9) 0.3764(7) 0.0765(5) 0.067(2) Uani 1 1 d . . . . .
H16C H 0.9362 0.4301 0.0823 0.080 Uiso 1 1 d DR U . . .
H16D H 1.0667 0.3920 0.1054 0.080 Uiso 1 1 d R U . . .
C1 C 0.8242(12) 0.3299(10) 0.2514(6) 0.052(3) Uani 1 1 d . . . . .
H1C H 0.8412 0.4041 0.2237 0.062 Uiso 1 1 calc R U . . .
H1D H 0.8360 0.3529 0.3003 0.062 Uiso 1 1 calc R U . . .
C2 C 0.9258(13) 0.2307(12) 0.2356(6) 0.064(3) Uani 1 1 d . . . . .
H2A H 0.9230 0.1631 0.2694 0.077 Uiso 1 1 calc R U . . .
H2B H 1.0183 0.2653 0.2372 0.077 Uiso 1 1 calc R U . . .
C3 C 0.9566(15) 0.0696(10) 0.1397(7) 0.074(4) Uani 1 1 d . . . . .
H3C H 0.9596 0.0055 0.1757 0.088 Uiso 1 1 calc R U . . .
H3D H 1.0504 0.0894 0.1286 0.088 Uiso 1 1 calc R U . . .
C4 C 0.8745(17) 0.0221(11) 0.0744(8) 0.081(5) Uani 1 1 d . . . . .
H4A H 0.8849 0.0801 0.0361 0.097 Uiso 1 1 calc R U . . .
H4B H 0.9092 -0.0593 0.0609 0.097 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
Pd1 N2 2.028(9) . ?
Pd1 N3 2.044(9) . ?
Pd1 N1 2.052(8) . ?
Pd1 O15 2.081(9) . ?
V1 O4 1.700(6) . ?
V1 O2 1.716(7) . ?
V1 O1 1.922(5) . ?
V1 O3 1.964(6) . ?
V1 O14 2.095(6) . ?
V1 O14 2.152(5) 3_665 ?
V2 O6 1.619(8) . ?
V2 O7 1.857(6) . ?
V2 O5 1.874(6) . ?
V2 O8 1.939(6) . ?
V2 O2 2.040(6) . ?
V2 O14 2.351(6) 3_665 ?
V2 V5 3.097(3) 3_665 ?
V3 O10 1.618(6) . ?
V3 O8 1.794(7) . ?
V3 O3 1.940(6) . ?
V3 O9 1.974(6) . ?
V3 O1 2.056(6) 3_665 ?
V3 O14 2.274(5) 3_665 ?
V4 O11 1.618(6) . ?
V4 O5 1.866(7) 3_665 ?
V4 O12 1.881(6) . ?
V4 O1 1.969(6) 3_665 ?
V4 O3 2.011(7) . ?
V4 O14 2.282(5) . ?
V5 O13 1.613(7) . ?
V5 O12 1.815(6) . ?
V5 O7 1.836(7) 3_665 ?
V5 O9 2.014(6) 3_665 ?
V5 O4 2.041(7) . ?
V5 O14 2.316(5) . ?
V5 V2 3.097(3) 3_665 ?
N1 C1 1.515(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C3 1.471(14) . ?
N2 C2 1.493(15) . ?
N2 H2 0.9800 . ?
N3 C4 1.511(18) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 H4C 0.9111 . ?
N4 H4D 0.9114 . ?
N4 H4F 0.9108 . ?
N4 H4E 0.9110 . ?
O1 V4 1.969(6) 3_665 ?
O1 V3 2.056(6) 3_665 ?
O5 V4 1.866(7) 3_665 ?
O7 V5 1.836(7) 3_665 ?
O9 V5 2.014(6) 3_665 ?
O14 V1 2.152(5) 3_665 ?
O14 V3 2.274(5) 3_665 ?
O14 V2 2.351(6) 3_665 ?
O15 H15A 0.8498 . ?
O15 H15B 0.8500 . ?
O16 H16C 0.8501 . ?
O16 H16D 0.8501 . ?
C1 C2 1.488(17) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.53(2) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
N2 Pd1 N3 85.3(4) . . ?
N2 Pd1 N1 84.4(3) . . ?
N3 Pd1 N1 169.5(4) . . ?
N2 Pd1 O15 176.4(3) . . ?
N3 Pd1 O15 95.4(4) . . ?
N1 Pd1 O15 94.9(3) . . ?
O4 V1 O2 107.3(3) . . ?
O4 V1 O1 99.1(3) . . ?
O2 V1 O1 97.3(3) . . ?
O4 V1 O3 95.6(2) . . ?
O2 V1 O3 95.8(3) . . ?
O1 V1 O3 156.4(3) . . ?
O4 V1 O14 87.8(3) . . ?
O2 V1 O14 164.7(3) . . ?
O1 V1 O14 81.6(2) . . ?
O3 V1 O14 80.6(3) . . ?
O4 V1 O14 166.2(3) . 3_665 ?
O2 V1 O14 86.3(3) . 3_665 ?
O1 V1 O14 81.0(2) . 3_665 ?
O3 V1 O14 80.4(2) . 3_665 ?
O14 V1 O14 78.5(2) . 3_665 ?
O6 V2 O7 105.7(3) . . ?
O6 V2 O5 102.4(4) . . ?
O7 V2 O5 91.5(3) . . ?
O6 V2 O8 100.1(3) . . ?
O7 V2 O8 91.2(3) . . ?
O5 V2 O8 155.7(3) . . ?
O6 V2 O2 99.2(3) . . ?
O7 V2 O2 155.0(3) . . ?
O5 V2 O2 84.9(2) . . ?
O8 V2 O2 82.5(2) . . ?
O6 V2 O14 173.2(3) . 3_665 ?
O7 V2 O14 80.6(2) . 3_665 ?
O5 V2 O14 79.4(2) . 3_665 ?
O8 V2 O14 77.2(2) . 3_665 ?
O2 V2 O14 74.4(2) . 3_665 ?
O6 V2 V5 138.5(3) . 3_665 ?
O7 V2 V5 32.8(2) . 3_665 ?
O5 V2 V5 82.8(2) . 3_665 ?
O8 V2 V5 86.4(2) . 3_665 ?
O2 V2 V5 122.3(2) . 3_665 ?
O14 V2 V5 47.96(13) 3_665 3_665 ?
O10 V3 O8 104.9(4) . . ?
O10 V3 O3 102.2(3) . . ?
O8 V3 O3 94.1(3) . . ?
O10 V3 O9 100.5(3) . . ?
O8 V3 O9 93.1(3) . . ?
O3 V3 O9 153.5(2) . . ?
O10 V3 O1 98.6(3) . 3_665 ?
O8 V3 O1 156.2(2) . 3_665 ?
O3 V3 O1 77.2(3) . 3_665 ?
O9 V3 O1 86.1(3) . 3_665 ?
O10 V3 O14 173.0(3) . 3_665 ?
O8 V3 O14 82.0(2) . 3_665 ?
O3 V3 O14 77.8(2) . 3_665 ?
O9 V3 O14 77.9(2) . 3_665 ?
O1 V3 O14 74.5(2) 3_665 3_665 ?
O11 V4 O5 102.1(3) . 3_665 ?
O11 V4 O12 102.0(3) . . ?
O5 V4 O12 93.1(3) 3_665 . ?
O11 V4 O1 100.3(3) . 3_665 ?
O5 V4 O1 91.8(3) 3_665 3_665 ?
O12 V4 O1 155.6(3) . 3_665 ?
O11 V4 O3 101.0(3) . . ?
O5 V4 O3 156.0(2) 3_665 . ?
O12 V4 O3 88.4(3) . . ?
O1 V4 O3 77.7(2) 3_665 . ?
O11 V4 O14 175.6(3) . . ?
O5 V4 O14 81.4(2) 3_665 . ?
O12 V4 O14 80.4(2) . . ?
O1 V4 O14 76.8(2) 3_665 . ?
O3 V4 O14 75.2(2) . . ?
O13 V5 O12 103.6(3) . . ?
O13 V5 O7 103.8(3) . 3_665 ?
O12 V5 O7 94.2(3) . 3_665 ?
O13 V5 O9 98.8(3) . 3_665 ?
O12 V5 O9 156.4(2) . 3_665 ?
O7 V5 O9 87.6(3) 3_665 3_665 ?
O13 V5 O4 99.2(3) . . ?
O12 V5 O4 87.4(3) . . ?
O7 V5 O4 155.9(3) 3_665 . ?
O9 V5 O4 81.7(3) 3_665 . ?
O13 V5 O14 172.3(3) . . ?
O12 V5 O14 80.8(2) . . ?
O7 V5 O14 82.0(2) 3_665 . ?
O9 V5 O14 76.2(2) 3_665 . ?
O4 V5 O14 74.5(2) . . ?
O13 V5 V2 137.0(3) . 3_665 ?
O12 V5 V2 85.5(2) . 3_665 ?
O7 V5 V2 33.24(18) 3_665 3_665 ?
O9 V5 V2 83.1(2) 3_665 3_665 ?
O4 V5 V2 123.40(17) . 3_665 ?
O14 V5 V2 48.90(15) . 3_665 ?
C1 N1 Pd1 108.1(6) . . ?
C1 N1 H1A 110.1 . . ?
Pd1 N1 H1A 110.1 . . ?
C1 N1 H1B 110.1 . . ?
Pd1 N1 H1B 110.1 . . ?
H1A N1 H1B 108.4 . . ?
C3 N2 C2 118.3(10) . . ?
C3 N2 Pd1 107.8(7) . . ?
C2 N2 Pd1 106.7(6) . . ?
C3 N2 H2 107.9 . . ?
C2 N2 H2 107.9 . . ?
Pd1 N2 H2 107.9 . . ?
C4 N3 Pd1 108.2(7) . . ?
C4 N3 H3A 110.1 . . ?
Pd1 N3 H3A 110.1 . . ?
C4 N3 H3B 110.1 . . ?
Pd1 N3 H3B 110.1 . . ?
H3A N3 H3B 108.4 . . ?
H4C N4 H4D 109.3 . . ?
H4C N4 H4F 109.4 . . ?
H4D N4 H4F 109.5 . . ?
H4C N4 H4E 109.6 . . ?
H4D N4 H4E 109.9 . . ?
H4F N4 H4E 109.1 . . ?
V1 O1 V4 108.6(3) . 3_665 ?
V1 O1 V3 107.6(3) . 3_665 ?
V4 O1 V3 97.3(3) 3_665 3_665 ?
V1 O2 V2 111.8(3) . . ?
V3 O3 V1 107.7(2) . . ?
V3 O3 V4 99.8(3) . . ?
V1 O3 V4 107.9(3) . . ?
V1 O4 V5 109.7(3) . . ?
V4 O5 V2 113.6(3) 3_665 . ?
V5 O7 V2 113.9(3) 3_665 . ?
V3 O8 V2 114.7(3) . . ?
V3 O9 V5 112.3(3) . 3_665 ?
V5 O12 V4 113.5(3) . . ?
V1 O14 V1 101.5(2) . 3_665 ?
V1 O14 V3 94.5(2) . 3_665 ?
V1 O14 V3 90.80(19) 3_665 3_665 ?
V1 O14 V4 94.4(2) . . ?
V1 O14 V4 90.9(2) 3_665 . ?
V3 O14 V4 170.4(3) 3_665 . ?
V1 O14 V5 87.9(2) . . ?
V1 O14 V5 169.8(3) 3_665 . ?
V3 O14 V5 92.38(19) 3_665 . ?
V4 O14 V5 84.44(17) . . ?
V1 O14 V2 171.0(3) . 3_665 ?
V1 O14 V2 87.5(2) 3_665 3_665 ?
V3 O14 V2 85.65(19) 3_665 3_665 ?
V4 O14 V2 84.98(19) . 3_665 ?
V5 O14 V2 83.14(18) . 3_665 ?
Pd1 O15 H15A 110.0 . . ?
Pd1 O15 H15B 110.7 . . ?
H15A O15 H15B 108.6 . . ?
H16C O16 H16D 108.6 . . ?
C2 C1 N1 111.2(9) . . ?
C2 C1 H1C 109.4 . . ?
N1 C1 H1C 109.4 . . ?
C2 C1 H1D 109.4 . . ?
N1 C1 H1D 109.4 . . ?
H1C C1 H1D 108.0 . . ?
C1 C2 N2 107.0(10) . . ?
C1 C2 H2A 110.3 . . ?
N2 C2 H2A 110.3 . . ?
C1 C2 H2B 110.3 . . ?
N2 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N2 C3 C4 107.6(11) . . ?
N2 C3 H3C 110.2 . . ?
C4 C3 H3C 110.2 . . ?
N2 C3 H3D 110.2 . . ?
C4 C3 H3D 110.2 . . ?
H3C C3 H3D 108.5 . . ?
N3 C4 C3 109.2(10) . . ?
N3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2B O6 0.97 2.63 3.364(15) 132.2 2_745
C1 H1C O2 0.97 2.52 3.240(13) 131.2 .
O16 H16D O10 0.85 2.24 3.082(12) 170.3 1_655
O16 H16C O2 0.85 2.28 3.060(10) 152.5 .
O16 H16C N4 0.85 2.53 2.964(13) 113.1 1_655
O15 H15B O13 0.85 2.33 3.113(11) 153.2 3_655
O15 H15A O8 0.85 2.20 2.976(10) 152.7 2_645
N4 H4E O9 0.91 1.82 2.702(12) 162.8 .
N4 H4F O16 0.91 2.19 2.839(14) 128.0 3_665
N4 H4F O16 0.91 2.48 2.964(13) 113.6 1_455
N3 H3B O13 0.89 2.61 3.327(12) 138.4 .
N3 H3B O12 0.89 2.57 3.086(12) 117.9 3_655
N3 H3B O12 0.89 2.61 3.367(13) 143.2 .
N3 H3A O7 0.89 2.56 3.328(10) 144.9 1_545
N3 H3A O5 0.89 2.36 3.076(10) 137.4 1_545
N2 H2 O16 0.98 1.97 2.908(8) 160.2 .
N1 H1B O9 0.89 2.39 3.124(10) 140.2 2_645
N1 H1B O7 0.89 2.31 3.082(10) 145.5 2_645
N1 H1A O8 0.89 2.44 3.320(11) 172.1 .
C2 H2B O6 0.97 2.63 3.364(15) 132.2 2_745
C1 H1C O2 0.97 2.52 3.240(13) 131.2 .
O16 H16D O10 0.85 2.24 3.082(12) 170.3 1_655
O16 H16C O2 0.85 2.28 3.060(10) 152.5 .
O16 H16C N4 0.85 2.53 2.964(13) 113.1 1_655
O15 H15B O13 0.85 2.33 3.113(11) 153.2 3_655
O15 H15A O8 0.85 2.20 2.976(10) 152.7 2_645
N4 H4E O9 0.91 1.82 2.702(12) 162.8 .
N4 H4F O16 0.91 2.19 2.839(14) 128.0 3_665
N4 H4F O16 0.91 2.48 2.964(13) 113.6 1_455
N3 H3B O13 0.89 2.61 3.327(12) 138.4 .
N3 H3B O12 0.89 2.57 3.086(12) 117.9 3_655
N3 H3B O12 0.89 2.61 3.367(13) 143.2 .
N3 H3A O7 0.89 2.56 3.328(10) 144.9 1_545
N3 H3A O5 0.89 2.36 3.076(10) 137.4 1_545
N2 H2 O16 0.98 1.97 2.908(8) 160.2 .
N1 H1B O9 0.89 2.39 3.124(10) 140.2 2_645
N1 H1B O7 0.89 2.31 3.082(10) 145.5 2_645
N1 H1A O8 0.89 2.44 3.320(11) 172.1 .

_refine_diff_density_max         1.733
_refine_diff_density_min         -3.143
_refine_diff_density_rms         0.257

_shelxl_version_number           2014/6

