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

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

data_a01
_database_code_depnum_ccdc_archive 'CCDC 1043088'
_audit_update_record             
;
2015-03-11 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H63.33 N9 O27.67 S4.67 V5'
_chemical_formula_weight         1229.07

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

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

_cell_length_a                   20.4115(17)
_cell_length_b                   20.4115(17)
_cell_length_c                   25.444(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9180.3(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2486
_cell_measurement_theta_min      4.15
_cell_measurement_theta_max      22.30

_exptl_crystal_description       Block
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             3800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.966
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8683
_exptl_absorpt_correction_T_max  0.8926
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16080
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.601
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             5459
_reflns_number_gt                3454
_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.

Since most organic amine molecules are disordered and partial
 occupied, the thermal parameters for relative C and N atoms are
 restrained by ISOR or SIMU. Also some C-N and C-C distances 
are restrained. 
;

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1157P)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         5459
_refine_ls_number_parameters     392
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.2063
_refine_ls_wR_factor_gt          0.1817
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.104
_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 0.90717(7) 0.47697(7) 0.2500 0.0284(3) Uani 1 2 d S T P . .
V2 V 0.94191(7) 0.63335(7) 0.2500 0.0341(3) Uani 1 2 d S T P . .
V3 V 0.99640(5) 0.61900(5) 0.35207(4) 0.0376(3) Uani 1 1 d . . . . .
V4 V 1.09950(8) 0.75530(7) 0.2500 0.0437(4) Uani 1 2 d S T P . .
S1 S 0.94837(8) 0.44769(8) 0.36257(5) 0.0372(4) Uani 1 1 d . . . . .
S2 S 0.6667 0.3333 0.46138(11) 0.0545(8) Uani 1 3 d S T P . .
S3 S 1.16286(10) 0.75734(10) 0.36151(7) 0.0622(5) Uani 1 1 d . . . . .
O1 O 1.2323(3) 0.7723(3) 0.3867(2) 0.096(2) Uani 1 1 d . . . . .
O2 O 1.1352(3) 0.8084(3) 0.3780(2) 0.0849(17) Uani 1 1 d . . . . .
O3 O 0.92059(18) 0.55805(19) 0.29910(13) 0.0307(8) Uani 1 1 d . . . . .
O4 O 1.0159(2) 0.6953(2) 0.29948(14) 0.0377(9) Uani 1 1 d . . . . .
O5 O 1.1080(4) 0.8381(3) 0.2500 0.0656(19) Uani 1 2 d S T P . .
O6 O 0.9510(3) 0.6307(2) 0.39790(18) 0.0605(13) Uani 1 1 d . . . . .
O8 O 0.8194(3) 0.4176(3) 0.2500 0.0362(12) Uani 1 2 d S T P . .
O9 O 0.9488(2) 0.4369(2) 0.30368(14) 0.0361(9) Uani 1 1 d . . . . .
O10 O 1.0051(2) 0.5288(2) 0.37300(14) 0.0413(10) Uani 1 1 d . . . . .
O11 O 0.8737(2) 0.4313(2) 0.37967(15) 0.0427(10) Uani 1 1 d . . . . .
O12 O 0.9748(2) 0.4014(2) 0.38736(16) 0.0524(11) Uani 1 1 d . . . . .
O13 O 0.8759(3) 0.6527(3) 0.2500 0.0506(15) Uani 1 2 d S T P . .
O14 O 1.1727(2) 0.7613(2) 0.30295(17) 0.0570(12) Uani 1 1 d . . . . .
O16 O 1.1034(2) 0.6757(2) 0.37444(16) 0.0491(11) Uani 1 1 d . . . . .
O17 O 0.6667 0.3333 0.4041(3) 0.058(2) Uani 1 3 d S T P . .
O18 O 0.7019(3) 0.2899(3) 0.4796(2) 0.0963(19) Uani 1 1 d . . . . .
N1 N 0.7706(3) 0.4903(3) 0.3728(2) 0.0509(13) Uani 1 1 d . . . . .
H1A H 0.7453 0.4495 0.3929 0.061 Uiso 1 1 calc R U . . .
H1B H 0.8172 0.4980 0.3683 0.061 Uiso 1 1 calc R U . . .
C2 C 0.7330(4) 0.4764(5) 0.3213(3) 0.066(2) Uani 1 1 d . . . . .
H2A H 0.7315 0.4332 0.3052 0.098 Uiso 1 1 calc R U . . .
H2B H 0.6824 0.4671 0.3260 0.098 Uiso 1 1 calc R U . . .
H2C H 0.7607 0.5199 0.2993 0.098 Uiso 1 1 calc R U . . .
C1 C 0.7751(5) 0.5554(5) 0.3998(4) 0.091(3) Uani 1 1 d . U . . .
H1C H 0.7999 0.5621 0.4331 0.137 Uiso 1 1 calc R U . . .
H1D H 0.8033 0.5999 0.3787 0.137 Uiso 1 1 calc R U . . .
H1E H 0.7249 0.5470 0.4055 0.137 Uiso 1 1 calc R U . . .
N3 N 1.0205(10) 0.2776(11) 0.4683(7) 0.114(6) Uani 0.5 1 d D . P . .
H3A H 1.0437 0.2536 0.4804 0.137 Uiso 0.5 1 calc R U P . .
H3B H 1.0140 0.2686 0.4339 0.137 Uiso 0.5 1 calc R U P . .
C4 C 0.9409(14) 0.2394(19) 0.4936(13) 0.205(14) Uani 0.5 1 d D U P . .
H4A H 0.9144 0.1865 0.4853 0.307 Uiso 0.5 1 calc R U P . .
H4B H 0.9457 0.2459 0.5310 0.307 Uiso 0.5 1 calc R U P . .
H4C H 0.9131 0.2623 0.4801 0.307 Uiso 0.5 1 calc R U P . .
C5 C 1.0720(9) 0.3575(11) 0.4747(6) 0.087(5) Uani 0.5 1 d D U P . .
H5A H 1.1184 0.3714 0.4566 0.131 Uiso 0.5 1 calc R U P . .
H5B H 1.0497 0.3854 0.4605 0.131 Uiso 0.5 1 calc R U P . .
H5C H 1.0823 0.3690 0.5114 0.131 Uiso 0.5 1 calc R U P . .
C7 C 0.7255(12) 0.6551(13) 0.2500 0.113(5) Uani 0.6667 2 d DS TU P . .
H7A H 0.7273 0.6173 0.2715 0.170 Uiso 0.3333 1 d R U P A .
H7B H 0.7236 0.6418 0.2136 0.170 Uiso 0.3333 1 d R U P . .
H7C H 0.7699 0.7033 0.2562 0.170 Uiso 0.3333 1 d R U P . .
C6 C 0.6268(13) 0.6947(13) 0.2500 0.120(6) Uani 0.6667 2 d DS TU P . .
H6A H 0.5823 0.6758 0.2714 0.181 Uiso 0.3333 1 d R U P A .
H6B H 0.6589 0.7479 0.2562 0.181 Uiso 0.3333 1 d R U P . .
H6C H 0.6125 0.6864 0.2136 0.181 Uiso 0.3333 1 d R U P . .
N4 N 0.6554(16) 0.6478(19) 0.2500 0.121(6) Uani 0.3333 2 d DS TU P A 1
H4D H 0.6333 0.6176 0.2780 0.146 Uiso 0.1667 1 d R U P A 1
N4A N 0.673(2) 0.671(3) 0.2741(13) 0.117(7) Uani 0.1667 1 d D U P A 2
H4AA H 0.6673 0.6639 0.3091 0.141 Uiso 0.1667 1 d R U P A 2
N1A N 1.2184(8) 0.5555(9) 0.2734(6) 0.032(4) Uani 0.25 1 d D U P B 1
H1AA H 1.2508 0.5497 0.2496 0.039 Uiso 0.5 2 d R U P B 1
H1AB H 1.2197 0.5504 0.3085 0.039 Uiso 0.25 1 d R U P B 1
N1AA N 1.1729(10) 0.5782(10) 0.1893(7) 0.038(4) Uani 0.25 1 d . U P B 2
H1AC H 1.2083 0.5710 0.1735 0.046 Uiso 0.25 1 d R U P B 2
H1AD H 1.1426 0.5889 0.1699 0.046 Uiso 0.25 1 d R U P B 2
N2A N 1.0647(4) 0.5949(4) 0.2500 0.057(2) Uani 1 2 d DS TU P . .
H2AA H 1.0650 0.5965 0.2146 0.068 Uiso 0.5 1 d R U P . .
H2AB H 1.0308 0.6018 0.2682 0.068 Uiso 0.5 1 d R U P . .
C2A C 1.1142(8) 0.5818(9) 0.2744(6) 0.078(5) Uani 0.5 1 d D U P B .
H2AC H 1.0858 0.5379 0.2960 0.093 Uiso 0.5 1 d R U P . .
H2AD H 1.1419 0.6238 0.2977 0.093 Uiso 0.5 1 d R U P . .
C1A C 1.1644(4) 0.5724(4) 0.2500 0.0355(18) Uani 1 2 d DS T P . .
H1AG H 1.1556 0.5232 0.2597 0.043 Uiso 0.25 1 d R U P B 2
H1AH H 1.2128 0.6084 0.2642 0.043 Uiso 0.25 1 d R U P B 2
H1AE H 1.1365 0.5329 0.2249 0.043 Uiso 0.25 1 d R U P B 1
H1AF H 1.1938 0.6177 0.2299 0.043 Uiso 0.25 1 d R U P B 1
C1C C 0.8200(11) 0.4267(13) 0.5760(7) 0.091(6) Uani 0.5 1 d D U P C 1
H1CA H 0.7777 0.3940 0.5977 0.137 Uiso 0.5 1 d R U P C 1
H1CB H 0.8635 0.4562 0.5977 0.137 Uiso 0.5 1 d R U P C 1
H1CC H 0.8084 0.4599 0.5565 0.137 Uiso 0.5 1 d R U P C 1
C3C C 0.8812(13) 0.3746(16) 0.5110(7) 0.116(8) Uani 0.5 1 d D U P C 2
H3CA H 0.8636 0.3213 0.5097 0.174 Uiso 0.5 1 calc R U P C 2
H3CB H 0.8815 0.3928 0.4761 0.174 Uiso 0.5 1 calc R U P C 2
H3CC H 0.9315 0.4007 0.5252 0.174 Uiso 0.5 1 calc R U P C 2
C2C C 0.8657(16) 0.4647(14) 0.5405(12) 0.124(8) Uani 0.5 1 d . U P C 2
H2CA H 0.8342 0.4762 0.5622 0.186 Uiso 0.5 1 calc R U P C 2
H2CB H 0.9162 0.4898 0.5543 0.186 Uiso 0.5 1 calc R U P C 2
H2CC H 0.8662 0.4819 0.5053 0.186 Uiso 0.5 1 calc R U P C 2
C4C C 0.9008(15) 0.4355(17) 0.5077(10) 0.123(9) Uani 0.5 1 d . U P C 1
H4CA H 0.9109 0.4055 0.4835 0.185 Uiso 0.5 1 calc R U P C 1
H4CB H 0.8895 0.4691 0.4885 0.185 Uiso 0.5 1 calc R U P C 1
H4CC H 0.9444 0.4644 0.5295 0.185 Uiso 0.5 1 calc R U P C 1
N1C N 0.8371(6) 0.3864(8) 0.5403(4) 0.137(4) Uani 1 1 d . . . . .
H1CF H 0.7967 0.3585 0.5196 0.165 Uiso 0.5 1 d R U P C 1
H1CG H 0.8482 0.3551 0.5580 0.165 Uiso 0.5 1 d R U P C 1
H1CD H 0.8353 0.3681 0.5728 0.165 Uiso 0.5 1 d R U P C 2
H1CE H 0.7902 0.3630 0.5265 0.165 Uiso 0.5 1 d R U P C 2
C1B C 1.1419(16) 0.9966(14) 0.2819(11) 0.093(6) Uani 0.3333 1 d . U P . .
H1BC H 1.1235 0.9433 0.2794 0.140 Uiso 0.3333 1 calc R U P . .
H1BD H 1.1936 1.0241 0.2705 0.140 Uiso 0.3333 1 calc R U P . .
H1BE H 1.1387 1.0096 0.3177 0.140 Uiso 0.3333 1 calc R U P . .
C2B C 1.1171(13) 1.0868(10) 0.2500 0.105(5) Uani 0.6667 2 d S TU P . .
H2BA H 1.0838 1.0941 0.2273 0.158 Uiso 0.3333 1 d R U P . .
H2BB H 1.1136 1.1021 0.2851 0.158 Uiso 0.3333 1 d R U P . .
H2BC H 1.1682 1.1166 0.2376 0.158 Uiso 0.3333 1 d R U P . .
N1B N 1.0978(10) 1.0155(8) 0.2500 0.096(4) Uani 0.6667 2 d S TU P . .
H1BA H 1.0494 0.9881 0.2608 0.115 Uiso 0.3333 1 d R U P . .
H1BB H 1.1000 1.0016 0.2168 0.115 Uiso 0.3333 1 d R U P . .
N1D N 1.0104(10) 0.8383(9) 0.3467(7) 0.062(4) Uani 0.3333 1 d D U P . .
H1DA H 1.0150 0.8562 0.3142 0.075 Uiso 0.3333 1 calc R U P . .
H1DB H 1.0364 0.8140 0.3477 0.075 Uiso 0.3333 1 calc R U P . .
C1D C 1.051(2) 0.9066(18) 0.3826(15) 0.143(14) Uani 0.3333 1 d D U P . .
H1DC H 1.1029 0.9369 0.3713 0.215 Uiso 0.3333 1 calc R U P . .
H1DD H 1.0267 0.9361 0.3812 0.215 Uiso 0.3333 1 calc R U P . .
H1DE H 1.0502 0.8898 0.4180 0.215 Uiso 0.3333 1 calc R U P . .
C2D C 0.9319(13) 0.7819(12) 0.3535(12) 0.094(8) Uani 0.3333 1 d D U P . .
H2DA H 0.9172 0.7439 0.3268 0.142 Uiso 0.3333 1 calc R U P . .
H2DB H 0.9248 0.7590 0.3875 0.142 Uiso 0.3333 1 calc R U P . .
H2DC H 0.9013 0.8054 0.3507 0.142 Uiso 0.3333 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O8 1.583(5) . ?
V1 O3 1.980(3) 10_556 ?
V1 O3 1.980(3) . ?
V1 O9 1.988(4) 10_556 ?
V1 O9 1.988(4) . ?
V1 V2 2.9031(18) . ?
V2 O13 1.584(6) . ?
V2 O3 1.855(4) 10_556 ?
V2 O3 1.856(4) . ?
V2 O4 1.885(4) . ?
V2 O4 1.885(4) 10_556 ?
V2 V3 2.8971(11) . ?
V2 V3 2.8971(11) 10_556 ?
V2 V4 2.9217(19) . ?
V3 O6 1.581(4) . ?
V3 O4 1.938(4) . ?
V3 O3 1.958(3) . ?
V3 O16 1.977(4) . ?
V3 O10 2.008(4) . ?
V4 O5 1.611(6) . ?
V4 O14 1.970(4) 10_556 ?
V4 O14 1.970(4) . ?
V4 O4 1.977(4) . ?
V4 O4 1.977(4) 10_556 ?
S1 O12 1.447(4) . ?
S1 O11 1.455(4) . ?
S1 O10 1.495(4) . ?
S1 O9 1.515(4) . ?
S2 O17 1.458(8) . ?
S2 O18 1.469(6) . ?
S2 O18 1.469(6) 2_655 ?
S2 O18 1.469(6) 3_665 ?
S3 O1 1.443(5) . ?
S3 O2 1.474(6) . ?
S3 O14 1.500(5) . ?
S3 O16 1.528(4) . ?
N1 C1 1.456(9) . ?
N1 C2 1.473(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
N3 C5 1.442(16) . ?
N3 C4 1.548(18) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C7 N4 1.363(18) . ?
C7 N4A 1.413(19) 10_556 ?
C7 N4A 1.413(19) . ?
C7 H7A 0.9601 . ?
C7 H7B 0.9601 . ?
C7 H7C 0.9600 . ?
C6 N4 1.347(18) . ?
C6 N4A 1.392(19) 10_556 ?
C6 N4A 1.392(19) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9601 . ?
N4 H4D 0.9000 . ?
N4A N4A 1.23(7) 10_556 ?
N4A H4AA 0.9000 . ?
N1A N1A 1.19(3) 10_556 ?
N1A C1A 1.439(12) . ?
N1A H1AA 0.9480 . ?
N1A H1AB 0.9000 . ?
N1AA C2A 1.54(2) 10_556 ?
N1AA C1A 1.552(18) . ?
N1AA H1AC 0.9002 . ?
N1AA H1AD 0.9000 . ?
N2A C2A 1.323(12) 10_556 ?
N2A C2A 1.323(12) . ?
N2A H2AA 0.8999 . ?
N2A H2AB 0.8999 . ?
C2A C2A 1.24(3) 10_556 ?
C2A C1A 1.290(12) . ?
C2A N1AA 1.54(2) 10_556 ?
C2A H2AC 0.9600 . ?
C2A H2AD 0.9601 . ?
C1A C2A 1.290(12) 10_556 ?
C1A N1A 1.439(12) 10_556 ?
C1A N1AA 1.552(18) 10_556 ?
C1A H1AG 0.9600 . ?
C1A H1AH 0.9599 . ?
C1A H1AE 0.9599 . ?
C1A H1AF 0.9600 . ?
C1C N1C 1.382(16) . ?
C1C H1CA 0.9599 . ?
C1C H1CB 0.9599 . ?
C1C H1CC 0.9598 . ?
C3C N1C 1.281(18) . ?
C3C H3CA 0.9600 . ?
C3C H3CB 0.9600 . ?
C3C H3CC 0.9600 . ?
C2C N1C 1.40(2) . ?
C2C H2CA 0.9600 . ?
C2C H2CB 0.9600 . ?
C2C H2CC 0.9600 . ?
C4C N1C 1.44(2) . ?
C4C H4CA 0.9600 . ?
C4C H4CB 0.9600 . ?
C4C H4CC 0.9600 . ?
N1C H1CF 0.9000 . ?
N1C H1CG 0.9000 . ?
N1C H1CD 0.9001 . ?
N1C H1CE 0.9001 . ?
C1B N1B 1.40(3) . ?
C1B C1B 1.62(5) 10_556 ?
C1B H1BC 0.9600 . ?
C1B H1BD 0.9600 . ?
C1B H1BE 0.9600 . ?
C2B N1B 1.30(2) . ?
C2B H2BA 0.9599 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9601 . ?
N1B C1B 1.40(3) 10_556 ?
N1B H1BA 0.9000 . ?
N1B H1BB 0.9000 . ?
N1D C2D 1.442(17) . ?
N1D C1D 1.519(19) . ?
N1D H1DA 0.8900 . ?
N1D H1DB 0.8900 . ?
C1D H1DC 0.9600 . ?
C1D H1DD 0.9600 . ?
C1D H1DE 0.9600 . ?
C2D H2DA 0.9600 . ?
C2D H2DB 0.9600 . ?
C2D H2DC 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
O8 V1 O3 105.73(17) . 10_556 ?
O8 V1 O3 105.73(17) . . ?
O3 V1 O3 78.2(2) 10_556 . ?
O8 V1 O9 103.72(17) . 10_556 ?
O3 V1 O9 90.09(14) 10_556 10_556 ?
O3 V1 O9 150.28(16) . 10_556 ?
O8 V1 O9 103.72(17) . . ?
O3 V1 O9 150.27(16) 10_556 . ?
O3 V1 O9 90.09(14) . . ?
O9 V1 O9 86.8(2) 10_556 . ?
O8 V1 V2 113.78(19) . . ?
O3 V1 V2 39.23(10) 10_556 . ?
O3 V1 V2 39.23(10) . . ?
O9 V1 V2 122.19(11) 10_556 . ?
O9 V1 V2 122.19(11) . . ?
O13 V2 O3 109.30(19) . 10_556 ?
O13 V2 O3 109.30(19) . . ?
O3 V2 O3 84.6(2) 10_556 . ?
O13 V2 O4 109.21(19) . . ?
O3 V2 O4 141.49(16) 10_556 . ?
O3 V2 O4 83.31(15) . . ?
O13 V2 O4 109.20(19) . 10_556 ?
O3 V2 O4 83.31(15) 10_556 10_556 ?
O3 V2 O4 141.49(16) . 10_556 ?
O4 V2 O4 83.8(2) . 10_556 ?
O13 V2 V3 116.30(3) . . ?
O3 V2 V3 117.56(11) 10_556 . ?
O3 V2 V3 41.90(10) . . ?
O4 V2 V3 41.41(11) . . ?
O4 V2 V3 116.56(12) 10_556 . ?
O13 V2 V3 116.31(3) . 10_556 ?
O3 V2 V3 41.90(10) 10_556 10_556 ?
O3 V2 V3 117.56(11) . 10_556 ?
O4 V2 V3 116.55(12) . 10_556 ?
O4 V2 V3 41.41(11) 10_556 10_556 ?
V3 V2 V3 127.38(6) . 10_556 ?
O13 V2 V1 120.3(2) . . ?
O3 V2 V1 42.45(10) 10_556 . ?
O3 V2 V1 42.45(10) . . ?
O4 V2 V1 114.25(12) . . ?
O4 V2 V1 114.25(12) 10_556 . ?
V3 V2 V1 77.52(3) . . ?
V3 V2 V1 77.52(3) 10_556 . ?
O13 V2 V4 120.0(2) . . ?
O3 V2 V4 114.08(11) 10_556 . ?
O3 V2 V4 114.08(11) . . ?
O4 V2 V4 42.02(11) . . ?
O4 V2 V4 42.03(11) 10_556 . ?
V3 V2 V4 76.78(3) . . ?
V3 V2 V4 76.78(3) 10_556 . ?
V1 V2 V4 119.76(6) . . ?
O6 V3 O4 106.8(2) . . ?
O6 V3 O3 105.5(2) . . ?
O4 V3 O3 79.32(15) . . ?
O6 V3 O16 105.0(2) . . ?
O4 V3 O16 90.31(16) . . ?
O3 V3 O16 149.46(16) . . ?
O6 V3 O10 105.7(2) . . ?
O4 V3 O10 147.50(16) . . ?
O3 V3 O10 90.24(15) . . ?
O16 V3 O10 83.24(16) . . ?
O6 V3 V2 111.22(19) . . ?
O4 V3 V2 40.06(11) . . ?
O3 V3 V2 39.26(10) . . ?
O16 V3 V2 124.51(13) . . ?
O10 V3 V2 123.02(11) . . ?
O5 V4 O14 104.7(2) . 10_556 ?
O5 V4 O14 104.7(2) . . ?
O14 V4 O14 86.3(3) 10_556 . ?
O5 V4 O4 104.9(2) . . ?
O14 V4 O4 150.14(18) 10_556 . ?
O14 V4 O4 89.77(16) . . ?
O5 V4 O4 104.9(2) . 10_556 ?
O14 V4 O4 89.77(16) 10_556 10_556 ?
O14 V4 O4 150.14(18) . 10_556 ?
O4 V4 O4 79.1(2) . 10_556 ?
O5 V4 V2 112.9(3) . . ?
O14 V4 V2 122.06(13) 10_556 . ?
O14 V4 V2 122.07(13) . . ?
O4 V4 V2 39.68(11) . . ?
O4 V4 V2 39.68(11) 10_556 . ?
O12 S1 O11 114.2(3) . . ?
O12 S1 O10 108.1(2) . . ?
O11 S1 O10 110.1(2) . . ?
O12 S1 O9 107.7(2) . . ?
O11 S1 O9 110.1(2) . . ?
O10 S1 O9 106.2(2) . . ?
O17 S2 O18 108.4(3) . . ?
O17 S2 O18 108.4(3) . 2_655 ?
O18 S2 O18 110.5(3) . 2_655 ?
O17 S2 O18 108.4(3) . 3_665 ?
O18 S2 O18 110.5(3) . 3_665 ?
O18 S2 O18 110.5(3) 2_655 3_665 ?
O1 S3 O2 114.0(4) . . ?
O1 S3 O14 109.8(3) . . ?
O2 S3 O14 109.5(3) . . ?
O1 S3 O16 107.2(3) . . ?
O2 S3 O16 109.5(3) . . ?
O14 S3 O16 106.6(2) . . ?
V2 O3 V3 98.84(16) . . ?
V2 O3 V1 98.32(15) . . ?
V3 O3 V1 134.45(18) . . ?
V2 O4 V3 98.53(16) . . ?
V2 O4 V4 98.29(17) . . ?
V3 O4 V4 134.8(2) . . ?
S1 O9 V1 125.8(2) . . ?
S1 O10 V3 126.4(2) . . ?
S3 O14 V4 126.8(3) . . ?
S3 O16 V3 128.3(3) . . ?
C1 N1 C2 112.6(6) . . ?
C1 N1 H1A 109.1 . . ?
C2 N1 H1A 109.1 . . ?
C1 N1 H1B 109.1 . . ?
C2 N1 H1B 109.1 . . ?
H1A N1 H1B 107.8 . . ?
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 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
C5 N3 C4 120.7(18) . . ?
C5 N3 H3A 107.1 . . ?
C4 N3 H3A 107.1 . . ?
C5 N3 H3B 107.1 . . ?
C4 N3 H3B 107.1 . . ?
H3A N3 H3B 106.8 . . ?
N3 C4 H4A 109.5 . . ?
N3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4A C7 N4A 52(3) 10_556 . ?
N4 C7 H7A 111.8 . . ?
N4A C7 H7A 140.7 10_556 . ?
N4A C7 H7A 106.2 . . ?
N4 C7 H7B 94.4 . . ?
N4A C7 H7B 73.7 10_556 . ?
N4A C7 H7B 123.9 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 120.9 . . ?
N4A C7 H7C 105.8 10_556 . ?
N4A C7 H7C 97.4 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4A C6 N4A 52(3) 10_556 . ?
N4 C6 H6A 111.9 . . ?
N4A C6 H6A 141.1 10_556 . ?
N4A C6 H6A 106.1 . . ?
N4 C6 H6B 120.8 . . ?
N4A C6 H6B 105.5 10_556 . ?
N4A C6 H6B 97.0 . . ?
H6A C6 H6B 109.5 . . ?
N4 C6 H6C 94.4 . . ?
N4A C6 H6C 73.3 10_556 . ?
N4A C6 H6C 124.3 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 N4 C7 137(3) . . ?
C6 N4 H4D 103.9 . . ?
C7 N4 H4D 102.3 . . ?
N4A N4A C6 63.8(14) 10_556 . ?
N4A N4A C7 64.2(14) 10_556 . ?
C6 N4A C7 128(3) . . ?
N4A N4A H4AA 171.3 10_556 . ?
C6 N4A H4AA 116.3 . . ?
C7 N4A H4AA 116.0 . . ?
N1A N1A C1A 65.6(7) 10_556 . ?
N1A N1A H1AA 50.3 10_556 . ?
C1A N1A H1AA 115.7 . . ?
N1A N1A H1AB 172.4 10_556 . ?
C1A N1A H1AB 120.5 . . ?
H1AA N1A H1AB 123.8 . . ?
C2A N1AA C1A 49.3(7) 10_556 . ?
C2A N1AA H1AC 168.5 10_556 . ?
C1A N1AA H1AC 120.1 . . ?
C2A N1AA H1AD 70.8 10_556 . ?
C1A N1AA H1AD 119.9 . . ?
H1AC N1AA H1AD 120.0 . . ?
C2A N2A C2A 55.9(12) 10_556 . ?
C2A N2A H2AA 63.0 10_556 . ?
C2A N2A H2AA 118.9 . . ?
C2A N2A H2AB 176.3 10_556 . ?
C2A N2A H2AB 121.1 . . ?
H2AA N2A H2AB 120.0 . . ?
C2A C2A C1A 61.3(7) 10_556 . ?
C2A C2A N2A 62.1(6) 10_556 . ?
C1A C2A N2A 123.3(12) . . ?
C2A C2A N1AA 126.8(8) 10_556 10_556 ?
C1A C2A N1AA 65.7(9) . 10_556 ?
N2A C2A N1AA 168.6(14) . 10_556 ?
C2A C2A H2AC 125.0 10_556 . ?
C1A C2A H2AC 106.9 . . ?
N2A C2A H2AC 107.0 . . ?
N1AA C2A H2AC 74.5 10_556 . ?
C2A C2A H2AD 128.2 10_556 . ?
C1A C2A H2AD 105.9 . . ?
N2A C2A H2AD 106.0 . . ?
N1AA C2A H2AD 63.1 10_556 . ?
H2AC C2A H2AD 106.8 . . ?
C2A C1A C2A 57.4(13) 10_556 . ?
C2A C1A N1A 174.0(10) 10_556 . ?
C2A C1A N1A 126.6(9) . . ?
C2A C1A N1A 126.7(9) 10_556 10_556 ?
C2A C1A N1A 174.0(10) . 10_556 ?
N1A C1A N1A 48.9(13) . 10_556 ?
C2A C1A N1AA 122.3(10) 10_556 10_556 ?
C2A C1A N1AA 65.0(9) . 10_556 ?
C2A C1A N1AA 65.0(9) 10_556 . ?
C2A C1A N1AA 122.3(10) . . ?
N1AA C1A N1AA 168.6(15) 10_556 . ?
C2A C1A H1AG 122.1 10_556 . ?
C2A C1A H1AG 106.5 . . ?
N1AA C1A H1AG 77.2 10_556 . ?
N1AA C1A H1AG 107.0 . . ?
C2A C1A H1AH 131.0 10_556 . ?
C2A C1A H1AH 107.2 . . ?
N1AA C1A H1AH 62.3 10_556 . ?
N1AA C1A H1AH 106.3 . . ?
H1AG C1A H1AH 106.7 . . ?
C2A C1A H1AE 67.9 10_556 . ?
C2A C1A H1AE 105.3 . . ?
N1A C1A H1AE 106.1 . . ?
N1A C1A H1AE 74.1 10_556 . ?
C2A C1A H1AF 76.3 10_556 . ?
C2A C1A H1AF 105.9 . . ?
N1A C1A H1AF 105.4 . . ?
N1A C1A H1AF 79.9 10_556 . ?
H1AE C1A H1AF 106.1 . . ?
N1C C1C H1CA 111.8 . . ?
N1C C1C H1CB 108.8 . . ?
H1CA C1C H1CB 109.5 . . ?
N1C C1C H1CC 107.8 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
N1C C3C H3CA 109.5 . . ?
N1C C3C H3CB 109.5 . . ?
H3CA C3C H3CB 109.5 . . ?
N1C C3C H3CC 109.5 . . ?
H3CA C3C H3CC 109.5 . . ?
H3CB C3C H3CC 109.5 . . ?
N1C C2C H2CA 109.5 . . ?
N1C C2C H2CB 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
N1C C2C H2CC 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
N1C C4C H4CA 109.5 . . ?
N1C C4C H4CB 109.5 . . ?
H4CA C4C H4CB 109.5 . . ?
N1C C4C H4CC 109.5 . . ?
H4CA C4C H4CC 109.5 . . ?
H4CB C4C H4CC 109.5 . . ?
C3C N1C C2C 107(2) . . ?
C1C N1C C4C 111.9(19) . . ?
C1C N1C H1CF 109.8 . . ?
C4C N1C H1CF 109.0 . . ?
C1C N1C H1CG 108.7 . . ?
C4C N1C H1CG 108.8 . . ?
H1CF N1C H1CG 108.6 . . ?
C3C N1C H1CD 110.0 . . ?
C2C N1C H1CD 112.1 . . ?
C3C N1C H1CE 109.6 . . ?
C2C N1C H1CE 109.4 . . ?
H1CD N1C H1CE 109.0 . . ?
N1B C1B C1B 54.6(12) . 10_556 ?
N1B C1B H1BC 109.5 . . ?
C1B C1B H1BC 86.2 10_556 . ?
N1B C1B H1BD 109.5 . . ?
C1B C1B H1BD 72.3 10_556 . ?
H1BC C1B H1BD 109.5 . . ?
N1B C1B H1BE 109.5 . . ?
C1B C1B H1BE 161.7 10_556 . ?
H1BC C1B H1BE 109.5 . . ?
H1BD C1B H1BE 109.5 . . ?
N1B C2B H2BA 109.4 . . ?
N1B C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
N1B C2B H2BC 109.6 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C2B N1B C1B 115.4(17) . 10_556 ?
C2B N1B C1B 115.4(17) . . ?
C1B N1B C1B 71(2) 10_556 . ?
C2B N1B H1BA 108.7 . . ?
C1B N1B H1BA 131.3 10_556 . ?
C1B N1B H1BA 108.0 . . ?
C2B N1B H1BB 108.6 . . ?
C1B N1B H1BB 39.5 10_556 . ?
C1B N1B H1BB 108.4 . . ?
H1BA N1B H1BB 107.5 . . ?
C2D N1D C1D 123(2) . . ?
C2D N1D H1DA 106.6 . . ?
C1D N1D H1DA 106.6 . . ?
C2D N1D H1DB 106.6 . . ?
C1D N1D H1DB 106.6 . . ?
H1DA N1D H1DB 106.6 . . ?
N1D C1D H1DC 109.5 . . ?
N1D C1D H1DD 109.5 . . ?
H1DC C1D H1DD 109.5 . . ?
N1D C1D H1DE 109.5 . . ?
H1DC C1D H1DE 109.5 . . ?
H1DD C1D H1DE 109.5 . . ?
N1D C2D H2DA 109.5 . . ?
N1D C2D H2DB 109.5 . . ?
H2DA C2D H2DB 109.5 . . ?
N1D C2D H2DC 109.5 . . ?
H2DA C2D H2DC 109.5 . . ?
H2DB C2D H2DC 109.5 . . ?

_refine_diff_density_max         1.394
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.133

