# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1063206'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H28 Mn N4 O6 V2'
_chemical_formula_weight         649.34

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   21.5654(11)
_cell_length_b                   21.5654(11)
_cell_length_c                   13.0149(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6052.8(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16913
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      25.02

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2648
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_T_max  0.8162
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16913
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2674
_reflns_number_gt                2106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.125 106 10 ' '
2 0.000 0.750 -0.125 106 10 ' '
3 -0.004 0.545 0.043 11 1 ' '
4 0.004 0.955 0.043 11 1 ' '
5 0.500 0.250 0.375 106 10 ' '
6 0.295 0.254 0.206 11 1 ' '
7 0.705 0.246 0.206 10 1 ' '
8 0.204 0.245 0.295 10 1 ' '
9 0.796 0.254 0.295 11 1 ' '
10 0.500 0.750 0.625 106 10 ' '
11 0.496 0.545 0.456 11 1 ' '
12 0.504 0.955 0.456 10 1 ' '
13 0.504 0.454 0.545 10 1 ' '
14 0.495 0.046 0.545 11 1 ' '
15 0.205 0.746 0.706 10 1 ' '
16 0.795 0.754 0.706 11 1 ' '
17 0.296 0.754 0.795 11 1 ' '
18 0.704 0.745 0.795 10 1 ' '
19 -0.005 0.046 0.955 10 1 ' '
20 0.005 0.454 0.955 10 1 ' '
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0488P)²+25.0277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2674
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1173
_refine_ls_wR_factor_gt          0.1089
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 1.0000 0.0000 0.01902(19) Uani 1 2 d S . .
V1 V 0.50188(3) 0.86005(3) 0.15698(5) 0.0286(2) Uani 1 1 d . . .
C1 C 0.5371(2) 0.97140(19) -0.2255(3) 0.0405(10) Uani 1 1 d . . .
H1A H 0.5177 1.0106 -0.2344 0.049 Uiso 1 1 calc R . .
C2 C 0.5637(2) 0.9431(2) -0.3097(3) 0.0456(11) Uani 1 1 d . . .
H2A H 0.5618 0.9631 -0.3747 0.055 Uiso 1 1 calc R . .
C3 C 0.59277(19) 0.8869(2) -0.3015(3) 0.0417(10) Uani 1 1 d . . .
C4 C 0.5921(2) 0.8599(2) -0.2056(4) 0.0517(12) Uani 1 1 d . . .
H4A H 0.6106 0.8204 -0.1954 0.062 Uiso 1 1 calc R . .
C5 C 0.5644(2) 0.8904(2) -0.1241(4) 0.0475(11) Uani 1 1 d . . .
H5A H 0.5646 0.8707 -0.0588 0.057 Uiso 1 1 calc R . .
C6 C 0.63757(18) 0.97798(19) 0.0643(3) 0.0372(9) Uani 1 1 d . . .
H6A H 0.6251 0.9357 0.0621 0.045 Uiso 1 1 calc R . .
C7 C 0.69886(19) 0.99140(19) 0.0849(3) 0.0387(10) Uani 1 1 d . . .
H7A H 0.7275 0.9586 0.0961 0.046 Uiso 1 1 calc R . .
C8 C 0.71883(18) 1.05210(19) 0.0893(3) 0.0358(9) Uani 1 1 d . . .
C9 C 0.67394(19) 1.0976(2) 0.0750(3) 0.0399(10) Uani 1 1 d . . .
H9A H 0.6848 1.1402 0.0801 0.048 Uiso 1 1 calc R . .
C10 C 0.61379(19) 1.08077(19) 0.0533(3) 0.0375(9) Uani 1 1 d . . .
H10A H 0.5842 1.1126 0.0420 0.045 Uiso 1 1 calc R . .
C11 C 0.78676(19) 1.0662(2) 0.1087(4) 0.0436(10) Uani 1 1 d . . .
H11A H 0.7980 1.0490 0.1767 0.052 Uiso 1 1 calc R . .
H11B H 0.8116 1.0438 0.0565 0.052 Uiso 1 1 calc R . .
C12 C 0.6242(2) 0.8568(2) -0.3920(4) 0.0539(13) Uani 1 1 d . . .
H12A H 0.6063 0.8737 -0.4562 0.054 Uiso 1 1 calc R . .
H12B H 0.6157 0.8117 -0.3906 0.054 Uiso 1 1 calc R . .
N1 N 0.53739(15) 0.94607(14) -0.1318(3) 0.0353(8) Uani 1 1 d . . .
N2 N 0.59493(15) 1.02180(15) 0.0474(2) 0.0346(7) Uani 1 1 d . . .
O1 O 0.50205(12) 0.92422(11) 0.0878(2) 0.0345(6) Uani 1 1 d . . .
O2 O 0.50474(18) 0.87821(17) 0.2772(2) 0.0639(10) Uani 1 1 d . . .
O3 O 0.43326(14) 0.81807(15) 0.1297(3) 0.0619(10) Uani 1 1 d . . .
C13 C 0.8057(2) 1.1332(2) 0.1066(4) 0.0538(13) Uani 1 1 d . . .
H13A H 0.7873 1.1544 0.1667 0.054 Uiso 1 1 calc R . .
H13B H 0.7885 1.1527 0.0440 0.054 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 1.995(2) 9_675 ?
Mn1 O1 1.995(2) . ?
Mn1 N2 2.189(3) 9_675 ?
Mn1 N2 2.189(3) . ?
Mn1 N1 2.224(3) 9_675 ?
Mn1 N1 2.224(3) . ?
V1 O2 1.615(3) . ?
V1 O1 1.651(2) . ?
V1 O3 1.771(3) . ?
V1 O3 1.772(3) 15_565 ?
C1 N1 1.335(5) . ?
C1 C2 1.379(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.370(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(6) . ?
C3 C12 1.507(6) . ?
C4 C5 1.384(6) . ?
C4 H4A 0.9500 . ?
C5 N1 1.337(5) . ?
C5 H5A 0.9500 . ?
C6 N2 1.337(5) . ?
C6 C7 1.379(6) . ?
C6 H6A 0.9500 . ?
C7 C8 1.379(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.391(6) . ?
C8 C11 1.517(6) . ?
C9 C10 1.376(6) . ?
C9 H9A 0.9500 . ?
C10 N2 1.337(5) . ?
C10 H10A 0.9500 . ?
C11 C13 1.501(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.526(6) 2_674 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O3 V1 1.772(3) 12_766 ?
C13 C12 1.526(6) 2_675 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 180.00(14) 9_675 . ?
O1 Mn1 N2 89.64(11) 9_675 9_675 ?
O1 Mn1 N2 90.36(11) . 9_675 ?
O1 Mn1 N2 90.36(11) 9_675 . ?
O1 Mn1 N2 89.64(11) . . ?
N2 Mn1 N2 180.0 9_675 . ?
O1 Mn1 N1 90.31(11) 9_675 9_675 ?
O1 Mn1 N1 89.69(11) . 9_675 ?
N2 Mn1 N1 89.47(12) 9_675 9_675 ?
N2 Mn1 N1 90.53(12) . 9_675 ?
O1 Mn1 N1 89.69(11) 9_675 . ?
O1 Mn1 N1 90.31(11) . . ?
N2 Mn1 N1 90.53(12) 9_675 . ?
N2 Mn1 N1 89.47(12) . . ?
N1 Mn1 N1 180.0 9_675 . ?
O2 V1 O1 108.99(16) . . ?
O2 V1 O3 110.49(19) . . ?
O1 V1 O3 108.73(15) . . ?
O2 V1 O3 111.01(19) . 15_565 ?
O1 V1 O3 107.05(15) . 15_565 ?
O3 V1 O3 110.5(2) . 15_565 ?
N1 C1 C2 122.8(4) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 121.3(4) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C2 C3 C4 116.1(4) . . ?
C2 C3 C12 121.8(4) . . ?
C4 C3 C12 122.1(4) . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
N1 C5 C4 123.8(4) . . ?
N1 C5 H5A 118.1 . . ?
C4 C5 H5A 118.1 . . ?
N2 C6 C7 122.9(4) . . ?
N2 C6 H6A 118.6 . . ?
C7 C6 H6A 118.6 . . ?
C8 C7 C6 120.4(4) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C7 C8 C9 116.5(4) . . ?
C7 C8 C11 119.9(4) . . ?
C9 C8 C11 123.6(4) . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
N2 C10 C9 123.3(4) . . ?
N2 C10 H10A 118.3 . . ?
C9 C10 H10A 118.3 . . ?
C13 C11 C8 116.9(4) . . ?
C13 C11 H11A 108.1 . . ?
C8 C11 H11A 108.1 . . ?
C13 C11 H11B 108.1 . . ?
C8 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C3 C12 C13 113.2(4) . 2_674 ?
C3 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 2_674 . ?
C3 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 2_674 . ?
H12A C12 H12B 107.8 . . ?
C1 N1 C5 116.0(4) . . ?
C1 N1 Mn1 119.2(3) . . ?
C5 N1 Mn1 124.7(3) . . ?
C6 N2 C10 117.0(3) . . ?
C6 N2 Mn1 122.5(3) . . ?
C10 N2 Mn1 120.3(3) . . ?
V1 O1 Mn1 177.64(18) . . ?
V1 O3 V1 155.1(2) . 12_766 ?
C11 C13 C12 114.0(4) . 2_675 ?
C11 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 2_675 . ?
C11 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 2_675 . ?
H13A C13 H13B 107.6 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.086
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1063207'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H56 Ag4 N8 O15 V4'
_chemical_formula_weight         1668.29

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   12.382(3)
_cell_length_b                   9.697(2)
_cell_length_c                   25.365(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.003(4)
_cell_angle_gamma                90.00
_cell_volume                     3043.5(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16812
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_T_max  0.6894
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16812
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         24.99
_reflns_number_total             5338
_reflns_number_gt                3069
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1005P)²+6.5896P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5338
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1890
_refine_ls_wR_factor_gt          0.1537
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag -0.10681(7) 1.08248(8) 0.98125(3) 0.0538(3) Uani 1 1 d . . .
Ag2 Ag -0.03613(8) 0.63055(9) 0.46977(3) 0.0639(3) Uani 1 1 d . . .
V1 V -0.54255(13) 0.35100(16) 0.42939(6) 0.0382(4) Uani 1 1 d . . .
V2 V -0.30957(14) 0.44313(16) 0.48689(6) 0.0403(4) Uani 1 1 d . . .
C1 C -0.0306(11) 0.4398(12) 0.3704(5) 0.074(4) Uani 1 1 d . . .
H1A H -0.1046 0.4320 0.3746 0.089 Uiso 1 1 calc R . .
C2 C 0.0137(10) 0.3644(13) 0.3316(5) 0.069(4) Uani 1 1 d . . .
H2A H -0.0297 0.3090 0.3097 0.083 Uiso 1 1 calc R . .
C3 C 0.1238(10) 0.3708(10) 0.3251(5) 0.055(3) Uani 1 1 d . . .
C4 C 0.1825(11) 0.2847(11) 0.2855(5) 0.075(4) Uani 1 1 d . . .
H4A H 0.1303 0.2330 0.2641 0.090 Uiso 1 1 calc R . .
H4B H 0.2291 0.2192 0.3042 0.090 Uiso 1 1 calc R . .
C5 C 0.1812(9) 0.4553(10) 0.3590(4) 0.050(3) Uani 1 1 d . . .
H5A H 0.2558 0.4609 0.3566 0.060 Uiso 1 1 calc R . .
C6 C 0.1321(10) 0.5307(10) 0.3961(4) 0.055(3) Uani 1 1 d . . .
H6A H 0.1737 0.5891 0.4176 0.066 Uiso 1 1 calc R . .
C7 C 0.2500 0.3731(17) 0.2500 0.064(5) Uani 1 2 d S . .
H7A H 0.2028 0.4319 0.2285 0.077 Uiso 0.50 1 calc PR . .
H7B H 0.2972 0.4319 0.2715 0.077 Uiso 0.50 1 calc PR . .
C8 C -0.1389(10) 0.8161(12) 0.5489(4) 0.058(3) Uani 1 1 d . . .
H8A H -0.1992 0.7639 0.5389 0.070 Uiso 1 1 calc R . .
C9 C -0.1516(9) 0.9212(12) 0.5836(4) 0.058(3) Uani 1 1 d . . .
H9A H -0.2186 0.9362 0.5980 0.070 Uiso 1 1 calc R . .
C10 C -0.0647(10) 1.0067(10) 0.5978(4) 0.051(3) Uani 1 1 d . . .
C11 C 0.0325(10) 0.9728(11) 0.5775(4) 0.059(3) Uani 1 1 d . . .
H11A H 0.0936 1.0247 0.5864 0.070 Uiso 1 1 calc R . .
C12 C 0.0401(9) 0.8627(12) 0.5439(4) 0.059(3) Uani 1 1 d . . .
H12A H 0.1074 0.8409 0.5310 0.070 Uiso 1 1 calc R . .
C13 C -0.0767(11) 1.1277(11) 0.6341(4) 0.066(3) Uani 1 1 d . . .
H13A H -0.1445 1.1741 0.6255 0.079 Uiso 1 1 calc R . .
H13B H -0.0186 1.1926 0.6285 0.079 Uiso 1 1 calc R . .
C14 C -0.0747(10) 1.0857(10) 0.6927(4) 0.055(3) Uani 1 1 d . . .
H14A H -0.1349 1.0243 0.6988 0.066 Uiso 1 1 calc R . .
H14B H -0.0085 1.0356 0.7011 0.066 Uiso 1 1 calc R . .
C15 C -0.0816(11) 1.2076(10) 0.7288(4) 0.062(3) Uani 1 1 d . . .
H15A H -0.1468 1.2586 0.7193 0.074 Uiso 1 1 calc R . .
H15B H -0.0207 1.2677 0.7226 0.074 Uiso 1 1 calc R . .
C16 C -0.0826(9) 1.1758(10) 0.7871(4) 0.047(3) Uani 1 1 d . . .
C17 C -0.0776(9) 1.0446(10) 0.8068(4) 0.050(3) Uani 1 1 d . . .
H17A H -0.0724 0.9697 0.7841 0.060 Uiso 1 1 calc R . .
C18 C -0.0804(8) 1.0239(10) 0.8611(4) 0.048(3) Uani 1 1 d . . .
H18A H -0.0753 0.9341 0.8738 0.058 Uiso 1 1 calc R . .
C19 C -0.0946(9) 1.2528(10) 0.8772(4) 0.054(3) Uani 1 1 d . . .
H19A H -0.1006 1.3255 0.9008 0.065 Uiso 1 1 calc R . .
C20 C -0.0909(9) 1.2818(10) 0.8244(4) 0.051(3) Uani 1 1 d . . .
H20A H -0.0940 1.3730 0.8132 0.062 Uiso 1 1 calc R . .
C21 C -0.1723(9) 0.8534(11) 1.0602(4) 0.052(3) Uani 1 1 d . . .
H21A H -0.1599 0.7980 1.0311 0.062 Uiso 1 1 calc R . .
C22 C -0.1986(9) 0.7913(11) 1.1065(4) 0.057(3) Uani 1 1 d . . .
H22A H -0.2064 0.6960 1.1078 0.068 Uiso 1 1 calc R . .
C23 C -0.2138(9) 0.8697(11) 1.1514(4) 0.051(3) Uani 1 1 d . . .
C24 C -0.1792(8) 1.0681(11) 1.0973(4) 0.051(3) Uani 1 1 d . . .
H24A H -0.1726 1.1633 1.0945 0.061 Uiso 1 1 calc R . .
C25 C -0.2048(9) 1.0115(11) 1.1452(4) 0.053(3) Uani 1 1 d . . .
H25A H -0.2162 1.0692 1.1738 0.064 Uiso 1 1 calc R . .
C26 C -0.2353(11) 0.7965(11) 1.2021(4) 0.068(4) Uani 1 1 d . . .
H26A H -0.1757 0.7340 1.2100 0.082 Uiso 1 1 calc R . .
H26B H -0.2999 0.7409 1.1969 0.082 Uiso 1 1 calc R . .
C27 C -0.2500 0.8896(15) 1.2500 0.061(4) Uani 1 2 d S . .
H27A H -0.3129 0.9481 1.2443 0.073 Uiso 0.50 1 calc PR . .
H27B H -0.1871 0.9481 1.2557 0.073 Uiso 0.50 1 calc PR . .
N1 N 0.0241(8) 0.5239(9) 0.4028(3) 0.056(2) Uani 1 1 d . . .
N2 N -0.0456(7) 0.7845(9) 0.5288(3) 0.050(2) Uani 1 1 d . . .
N3 N -0.0901(7) 1.1257(8) 0.8959(3) 0.045(2) Uani 1 1 d . . .
N4 N -0.1636(7) 0.9897(9) 1.0550(3) 0.045(2) Uani 1 1 d . . .
O1 O -0.5419(6) 0.2024(7) 0.4575(3) 0.061(2) Uani 1 1 d . . .
O2 O -0.5727(6) 0.3325(7) 0.3676(3) 0.0568(19) Uani 1 1 d . . .
O3 O -0.6339(6) 0.4661(8) 0.4599(3) 0.061(2) Uani 1 1 d . . .
O4 O -0.4078(6) 0.4226(8) 0.4327(3) 0.063(2) Uani 1 1 d . . .
O5 O -0.2663(6) 0.2969(7) 0.5071(3) 0.064(2) Uani 1 1 d . . .
O6 O -0.2114(7) 0.5310(9) 0.4644(3) 0.080(3) Uani 1 1 d . . .
O1W O 0.7500 0.2696(18) 0.2500 0.149(7) Uani 1 2 d S . .
O2W O 0.6347(14) 0.4219(14) 0.3226(5) 0.179(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N4 2.212(8) . ?
Ag1 N3 2.222(8) . ?
Ag1 Ag1 3.2069(18) 3_577 ?
Ag2 N2 2.121(8) . ?
Ag2 N1 2.145(9) . ?
Ag2 O6 2.374(8) . ?
Ag2 Ag2 3.0767(19) 3_566 ?
V1 O1 1.607(7) . ?
V1 O2 1.608(7) . ?
V1 O3 1.785(7) . ?
V1 O4 1.807(8) . ?
V2 O5 1.594(8) . ?
V2 O6 1.606(8) . ?
V2 O3 1.775(7) 3_466 ?
V2 O4 1.814(7) . ?
C1 N1 1.327(13) . ?
C1 C2 1.356(16) . ?
C1 H1A 0.9300 . ?
C2 C3 1.380(16) . ?
C2 H2A 0.9300 . ?
C3 C5 1.370(14) . ?
C3 C4 1.511(15) . ?
C4 C7 1.516(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.351(14) . ?
C5 H5A 0.9300 . ?
C6 N1 1.355(13) . ?
C6 H6A 0.9300 . ?
C7 C4 1.516(14) 2 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.315(14) . ?
C8 C9 1.359(15) . ?
C8 H8A 0.9300 . ?
C9 C10 1.396(15) . ?
C9 H9A 0.9300 . ?
C10 C11 1.365(15) . ?
C10 C13 1.503(14) . ?
C11 C12 1.372(15) . ?
C11 H11A 0.9300 . ?
C12 N2 1.348(13) . ?
C12 H12A 0.9300 . ?
C13 C14 1.541(14) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.500(14) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.511(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.368(13) . ?
C16 C20 1.403(13) . ?
C17 C18 1.393(13) . ?
C17 H17A 0.9300 . ?
C18 N3 1.331(12) . ?
C18 H18A 0.9300 . ?
C19 N3 1.321(12) . ?
C19 C20 1.369(13) . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9300 . ?
C21 N4 1.334(12) . ?
C21 C22 1.368(14) . ?
C21 H21A 0.9300 . ?
C22 C23 1.387(14) . ?
C22 H22A 0.9300 . ?
C23 C25 1.390(14) . ?
C23 C26 1.501(14) . ?
C24 N4 1.335(12) . ?
C24 C25 1.380(14) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.530(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C26 1.530(13) 2_457 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
O3 V2 1.775(7) 3_466 ?

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
N4 Ag1 N3 160.7(3) . . ?
N4 Ag1 Ag1 80.2(2) . 3_577 ?
N3 Ag1 Ag1 106.2(2) . 3_577 ?
N2 Ag2 N1 158.1(3) . . ?
N2 Ag2 O6 104.7(3) . . ?
N1 Ag2 O6 95.8(3) . . ?
N2 Ag2 Ag2 104.4(2) . 3_566 ?
N1 Ag2 Ag2 83.9(2) . 3_566 ?
O6 Ag2 Ag2 86.7(2) . 3_566 ?
O1 V1 O2 109.3(4) . . ?
O1 V1 O3 111.2(4) . . ?
O2 V1 O3 111.3(4) . . ?
O1 V1 O4 109.5(4) . . ?
O2 V1 O4 105.7(4) . . ?
O3 V1 O4 109.8(3) . . ?
O5 V2 O6 109.6(4) . . ?
O5 V2 O3 109.5(4) . 3_466 ?
O6 V2 O3 109.3(4) . 3_466 ?
O5 V2 O4 110.7(4) . . ?
O6 V2 O4 106.6(4) . . ?
O3 V2 O4 111.0(3) 3_466 . ?
N1 C1 C2 124.8(12) . . ?
N1 C1 H1A 117.6 . . ?
C2 C1 H1A 117.6 . . ?
C1 C2 C3 119.2(11) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C5 C3 C2 116.4(11) . . ?
C5 C3 C4 119.8(11) . . ?
C2 C3 C4 123.7(10) . . ?
C3 C4 C7 111.7(9) . . ?
C3 C4 H4A 109.3 . . ?
C7 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C7 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C3 121.6(10) . . ?
C6 C5 H5A 119.2 . . ?
C3 C5 H5A 119.2 . . ?
C5 C6 N1 122.1(10) . . ?
C5 C6 H6A 119.0 . . ?
N1 C6 H6A 119.0 . . ?
C4 C7 C4 111.1(13) 2 . ?
C4 C7 H7A 109.4 2 . ?
C4 C7 H7A 109.4 . . ?
C4 C7 H7B 109.4 2 . ?
C4 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C9 123.3(11) . . ?
N2 C8 H8A 118.4 . . ?
C9 C8 H8A 118.4 . . ?
C8 C9 C10 120.4(11) . . ?
C8 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C11 C10 C9 116.2(10) . . ?
C11 C10 C13 121.8(11) . . ?
C9 C10 C13 122.0(11) . . ?
C10 C11 C12 120.2(11) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
N2 C12 C11 122.9(11) . . ?
N2 C12 H12A 118.5 . . ?
C11 C12 H12A 118.5 . . ?
C10 C13 C14 112.7(9) . . ?
C10 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
C10 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 112.4(8) . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 116.0(8) . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15B 108.3 . . ?
C16 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C17 C16 C20 116.0(9) . . ?
C17 C16 C15 123.1(8) . . ?
C20 C16 C15 120.9(9) . . ?
C16 C17 C18 119.5(9) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
N3 C18 C17 123.6(9) . . ?
N3 C18 H18A 118.2 . . ?
C17 C18 H18A 118.2 . . ?
N3 C19 C20 122.7(9) . . ?
N3 C19 H19A 118.6 . . ?
C20 C19 H19A 118.6 . . ?
C19 C20 C16 120.9(9) . . ?
C19 C20 H20A 119.5 . . ?
C16 C20 H20A 119.5 . . ?
N4 C21 C22 123.0(9) . . ?
N4 C21 H21A 118.5 . . ?
C22 C21 H21A 118.5 . . ?
C21 C22 C23 120.4(10) . . ?
C21 C22 H22A 119.8 . . ?
C23 C22 H22A 119.8 . . ?
C22 C23 C25 115.9(9) . . ?
C22 C23 C26 118.5(9) . . ?
C25 C23 C26 125.6(9) . . ?
N4 C24 C25 121.7(10) . . ?
N4 C24 H24A 119.1 . . ?
C25 C24 H24A 119.1 . . ?
C24 C25 C23 121.0(10) . . ?
C24 C25 H25A 119.5 . . ?
C23 C25 H25A 119.5 . . ?
C23 C26 C27 115.5(9) . . ?
C23 C26 H26A 108.4 . . ?
C27 C26 H26A 108.4 . . ?
C23 C26 H26B 108.4 . . ?
C27 C26 H26B 108.4 . . ?
H26A C26 H26B 107.5 . . ?
C26 C27 C26 107.6(12) . 2_457 ?
C26 C27 H27A 110.2 . . ?
C26 C27 H27A 110.2 2_457 . ?
C26 C27 H27B 110.2 . . ?
C26 C27 H27B 110.2 2_457 . ?
H27A C27 H27B 108.5 . . ?
C1 N1 C6 115.8(10) . . ?
C1 N1 Ag2 127.1(8) . . ?
C6 N1 Ag2 116.6(7) . . ?
C8 N2 C12 116.9(9) . . ?
C8 N2 Ag2 120.6(7) . . ?
C12 N2 Ag2 122.3(7) . . ?
C19 N3 C18 117.2(9) . . ?
C19 N3 Ag1 121.5(6) . . ?
C18 N3 Ag1 121.3(6) . . ?
C24 N4 C21 118.0(9) . . ?
C24 N4 Ag1 120.5(7) . . ?
C21 N4 Ag1 121.1(6) . . ?
V2 O3 V1 155.9(5) 3_466 . ?
V1 O4 V2 132.1(5) . . ?
V2 O6 Ag2 153.8(5) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.140
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1063208'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H62 N8 Ni3 O24 V6'
_chemical_formula_weight         1664.87

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   13.081(3)
_cell_length_b                   16.379(4)
_cell_length_c                   15.407(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.368(5)
_cell_angle_gamma                90.00
_cell_volume                     3224.4(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_T_max  0.7079
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23558
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.39
_reflns_number_total             8053
_reflns_number_gt                5893
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0428P)²+1.3139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8053
_refine_ls_number_parameters     429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.48884(3) 0.30586(2) 0.57391(2) 0.01853(9) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.5000 0.5000 0.01546(11) Uani 1 2 d S . .
V1 V 0.34094(4) 0.33234(3) 0.35453(3) 0.01890(11) Uani 1 1 d . . .
V2 V 0.27631(4) 0.65855(3) 0.25152(3) 0.02237(12) Uani 1 1 d . . .
V3 V 0.21851(4) 0.50397(3) 0.37800(3) 0.01623(10) Uani 1 1 d . . .
O1 O 0.11347(15) 0.49888(11) 0.42107(12) 0.0214(4) Uani 1 1 d . . .
O1W O 0.5917(2) 0.31690(17) 0.48587(18) 0.0314(6) Uani 1 1 d . . .
H1 H 0.559(3) 0.332(2) 0.436(2) 0.031 Uiso 1 1 d . . .
O2 O 0.20195(16) 0.58293(11) 0.29693(13) 0.0246(5) Uani 1 1 d . . .
O2W O 0.47952(19) 0.43386(13) 0.57782(16) 0.0265(5) Uani 1 1 d . . .
H3 H 0.522(3) 0.454(2) 0.576(2) 0.026 Uiso 1 1 d . . .
H4 H 0.428(3) 0.460(2) 0.539(2) 0.026 Uiso 1 1 d . . .
O3 O 0.32286(16) 0.52339(12) 0.45662(13) 0.0258(5) Uani 1 1 d . . .
O4 O 0.62118(17) 0.31387(12) 0.67173(13) 0.0284(5) Uani 1 1 d . . .
O5 O 0.3161(2) 0.61948(18) 0.16844(16) 0.0556(8) Uani 1 1 d . . .
O6 O 0.23726(18) 0.40738(12) 0.33093(13) 0.0296(5) Uani 1 1 d . . .
O9 O 0.3033(2) 0.24596(14) 0.28597(17) 0.0485(7) Uani 1 1 d . . .
O8 O 0.36682(16) 0.30945(12) 0.46192(13) 0.0246(4) Uani 1 1 d . . .
O7 O 0.44761(19) 0.36896(17) 0.33248(15) 0.0452(6) Uani 1 1 d . . .
N1 N 0.01124(19) 0.36893(14) 0.51236(15) 0.0207(5) Uani 1 1 d . . .
N2 N -0.11911(19) 0.47963(13) 0.38675(14) 0.0186(5) Uani 1 1 d . . .
N3 N 0.48422(19) 0.17877(14) 0.57567(15) 0.0220(5) Uani 1 1 d . . .
N4 N 0.38962(19) 0.30581(14) 0.66265(15) 0.0209(5) Uani 1 1 d . . .
C1 C -0.1074(2) 0.42908(17) 0.32090(18) 0.0221(6) Uani 1 1 d . . .
H1A H -0.0406 0.4104 0.3198 0.027 Uiso 1 1 calc R . .
C25 C 0.0179(2) 0.19754(17) 0.51764(19) 0.0238(6) Uani 1 1 d . . .
C30 C 0.2471(2) 0.30951(17) 0.77491(19) 0.0235(6) Uani 1 1 d . . .
C34 C 0.4216(2) 0.3197(2) 0.7497(2) 0.0331(8) Uani 1 1 d . . .
H34A H 0.4925 0.3286 0.7728 0.040 Uiso 1 1 calc R . .
C36 C 0.5545(3) 0.13502(19) 0.6321(2) 0.0295(7) Uani 1 1 d . . .
H36A H 0.6127 0.1617 0.6654 0.035 Uiso 1 1 calc R . .
C37 C 0.2163(2) 0.29613(18) 0.6849(2) 0.0263(6) Uani 1 1 d . . .
H37A H 0.1458 0.2883 0.6595 0.032 Uiso 1 1 calc R . .
C40 C 0.0765(2) 0.24181(17) 0.46991(19) 0.0251(6) Uani 1 1 d . . .
H40A H 0.1198 0.2149 0.4386 0.030 Uiso 1 1 calc R . .
C42 C 0.5451(3) 0.05175(19) 0.6435(2) 0.0326(8) Uani 1 1 d . . .
H42A H 0.5965 0.0238 0.6836 0.039 Uiso 1 1 calc R . .
C46 C -0.0463(2) 0.32597(17) 0.5585(2) 0.0268(7) Uani 1 1 d . . .
H46A H -0.0884 0.3543 0.5898 0.032 Uiso 1 1 calc R . .
C47 C -0.2150(2) 0.50720(17) 0.38435(18) 0.0231(6) Uani 1 1 d . . .
H47A H -0.2245 0.5437 0.4282 0.028 Uiso 1 1 calc R . .
C48 C -0.2905(2) 0.43118(17) 0.25405(18) 0.0234(6) Uani 1 1 d . . .
C50 C -0.1896(2) 0.40377(18) 0.25519(19) 0.0256(6) Uani 1 1 d . . .
H50A H -0.1778 0.3682 0.2113 0.031 Uiso 1 1 calc R . .
C52 C 0.0268(3) 0.10586(17) 0.5226(2) 0.0293(7) Uani 1 1 d . . .
H52A H 0.0303 0.0846 0.4645 0.035 Uiso 1 1 calc R . .
H52B H -0.0352 0.0835 0.5387 0.035 Uiso 1 1 calc R . .
C53 C -0.3012(2) 0.48483(18) 0.32060(19) 0.0267(7) Uani 1 1 d . . .
H53A H -0.3667 0.5059 0.3224 0.032 Uiso 1 1 calc R . .
C54 C 0.3529(3) 0.3213(2) 0.8066(2) 0.0356(8) Uani 1 1 d . . .
H54A H 0.3784 0.3304 0.8670 0.043 Uiso 1 1 calc R . .
C55 C 0.0713(2) 0.32570(17) 0.46843(18) 0.0231(6) Uani 1 1 d . . .
H55A H 0.1114 0.3539 0.4353 0.028 Uiso 1 1 calc R . .
C59 C -0.3849(2) 0.4052(2) 0.1865(2) 0.0312(7) Uani 1 1 d . . .
H59A H -0.4457 0.4339 0.1977 0.037 Uiso 1 1 calc R . .
H59B H -0.3962 0.3473 0.1934 0.037 Uiso 1 1 calc R . .
C64 C 0.1246(3) 0.07824(18) 0.5911(2) 0.0301(7) Uani 1 1 d . . .
H64A H 0.1353 0.0202 0.5839 0.036 Uiso 1 1 calc R . .
H64B H 0.1854 0.1067 0.5798 0.036 Uiso 1 1 calc R . .
C65 C 0.4025(2) 0.13795(18) 0.52804(19) 0.0245(6) Uani 1 1 d . . .
H65A H 0.3529 0.1668 0.4872 0.029 Uiso 1 1 calc R . .
C68 C 0.4604(3) 0.01019(18) 0.5961(2) 0.0278(7) Uani 1 1 d . . .
C69 C 0.3885(2) 0.05524(19) 0.5367(2) 0.0282(7) Uani 1 1 d . . .
H69A H 0.3302 0.0297 0.5024 0.034 Uiso 1 1 calc R . .
C71 C -0.0463(3) 0.24141(18) 0.5619(2) 0.0288(7) Uani 1 1 d . . .
H71A H -0.0890 0.2142 0.5936 0.035 Uiso 1 1 calc R . .
C72 C 0.1695(3) 0.31666(18) 0.8332(2) 0.0298(7) Uani 1 1 d . . .
H72A H 0.2009 0.2982 0.8928 0.036 Uiso 1 1 calc R . .
H72B H 0.1090 0.2827 0.8102 0.036 Uiso 1 1 calc R . .
C76 C 0.2880(2) 0.29429(18) 0.63262(19) 0.0248(6) Uani 1 1 d . . .
H76A H 0.2643 0.2843 0.5722 0.030 Uiso 1 1 calc R . .
C78 C 0.1361(3) 0.40553(19) 0.8356(2) 0.0372(8) Uani 1 1 d . . .
H78A H 0.1975 0.4386 0.8583 0.045 Uiso 1 1 calc R . .
H78B H 0.1066 0.4234 0.7755 0.045 Uiso 1 1 calc R . .
C79 C 0.4438(3) -0.07979(19) 0.6074(2) 0.0349(8) Uani 1 1 d . . .
H79A H 0.5097 -0.1051 0.6352 0.042 Uiso 1 1 calc R . .
H79B H 0.4196 -0.1048 0.5496 0.042 Uiso 1 1 calc R . .
O3W O 0.3284(4) 0.4495(3) 0.1335(3) 0.1100(14) Uiso 1 1 d . . .
H2 H 0.617(3) 0.348(2) 0.502(3) 0.042(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.042(2) . ?
Ni1 N4 2.077(2) . ?
Ni1 N3 2.083(2) . ?
Ni1 O8 2.085(2) . ?
Ni1 O2W 2.102(2) . ?
Ni1 O1W 2.113(3) . ?
Ni2 N2 2.102(2) 3_566 ?
Ni2 N2 2.102(2) . ?
Ni2 O1 2.111(2) 3_566 ?
Ni2 O1 2.111(2) . ?
Ni2 N1 2.158(2) 3_566 ?
Ni2 N1 2.158(2) . ?
V1 O7 1.620(2) . ?
V1 O8 1.659(2) . ?
V1 O9 1.771(2) . ?
V1 O6 1.809(2) . ?
V2 O5 1.614(2) . ?
V2 O4 1.650(2) 3_666 ?
V2 O9 1.792(2) 2 ?
V2 O2 1.8059(19) . ?
V3 O3 1.650(2) . ?
V3 O1 1.651(2) . ?
V3 O2 1.7786(19) . ?
V3 O6 1.779(2) . ?
O1W H1 0.83(4) . ?
O1W H2 0.63(4) . ?
O2W H3 0.65(3) . ?
O2W H4 0.90(3) . ?
O4 V2 1.650(2) 3_666 ?
O9 V2 1.792(2) 2_545 ?
N1 C46 1.340(4) . ?
N1 C55 1.343(4) . ?
N2 C47 1.326(4) . ?
N2 C1 1.343(3) . ?
N3 C36 1.331(4) . ?
N3 C65 1.338(4) . ?
N4 C76 1.324(4) . ?
N4 C34 1.336(4) . ?
C1 C50 1.374(4) . ?
C1 H1A 0.9300 . ?
C25 C40 1.377(4) . ?
C25 C71 1.390(4) . ?
C25 C52 1.507(4) . ?
C30 C37 1.377(4) . ?
C30 C54 1.380(4) . ?
C30 C72 1.497(4) . ?
C34 C54 1.384(4) . ?
C34 H34A 0.9300 . ?
C36 C42 1.384(4) . ?
C36 H36A 0.9300 . ?
C37 C76 1.361(4) . ?
C37 H37A 0.9300 . ?
C40 C55 1.376(4) . ?
C40 H40A 0.9300 . ?
C42 C68 1.371(5) . ?
C42 H42A 0.9300 . ?
C46 C71 1.386(4) . ?
C46 H46A 0.9300 . ?
C47 C53 1.377(4) . ?
C47 H47A 0.9300 . ?
C48 C53 1.380(4) . ?
C48 C50 1.390(4) . ?
C48 C59 1.496(4) . ?
C50 H50A 0.9300 . ?
C52 C64 1.542(4) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9300 . ?
C54 H54A 0.9300 . ?
C55 H55A 0.9300 . ?
C59 C64 1.525(4) 4_565 ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C64 C59 1.525(4) 4_666 ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 C69 1.377(4) . ?
C65 H65A 0.9300 . ?
C68 C69 1.377(4) . ?
C68 C79 1.505(4) . ?
C69 H69A 0.9300 . ?
C71 H71A 0.9300 . ?
C72 C78 1.523(4) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C76 H76A 0.9300 . ?
C78 C79 1.521(4) 2_556 ?
C78 H78A 0.9700 . ?
C78 H78B 0.9700 . ?
C79 C78 1.521(4) 2_546 ?
C79 H79A 0.9700 . ?
C79 H79B 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
O4 Ni1 N4 93.71(9) . . ?
O4 Ni1 N3 94.42(9) . . ?
N4 Ni1 N3 88.12(9) . . ?
O4 Ni1 O8 170.66(8) . . ?
N4 Ni1 O8 93.97(9) . . ?
N3 Ni1 O8 91.14(9) . . ?
O4 Ni1 O2W 87.70(9) . . ?
N4 Ni1 O2W 86.17(9) . . ?
N3 Ni1 O2W 174.03(9) . . ?
O8 Ni1 O2W 87.52(9) . . ?
O4 Ni1 O1W 84.98(10) . . ?
N4 Ni1 O1W 175.00(10) . . ?
N3 Ni1 O1W 96.79(10) . . ?
O8 Ni1 O1W 86.92(10) . . ?
O2W Ni1 O1W 88.96(10) . . ?
N2 Ni2 N2 180.0 3_566 . ?
N2 Ni2 O1 90.46(8) 3_566 3_566 ?
N2 Ni2 O1 89.54(8) . 3_566 ?
N2 Ni2 O1 89.54(8) 3_566 . ?
N2 Ni2 O1 90.46(8) . . ?
O1 Ni2 O1 180.0 3_566 . ?
N2 Ni2 N1 86.55(8) 3_566 3_566 ?
N2 Ni2 N1 93.45(8) . 3_566 ?
O1 Ni2 N1 89.95(8) 3_566 3_566 ?
O1 Ni2 N1 90.05(8) . 3_566 ?
N2 Ni2 N1 93.45(8) 3_566 . ?
N2 Ni2 N1 86.55(8) . . ?
O1 Ni2 N1 90.05(8) 3_566 . ?
O1 Ni2 N1 89.95(8) . . ?
N1 Ni2 N1 180.0 3_566 . ?
O7 V1 O8 106.97(11) . . ?
O7 V1 O9 108.21(13) . . ?
O8 V1 O9 112.68(12) . . ?
O7 V1 O6 110.40(12) . . ?
O8 V1 O6 109.76(10) . . ?
O9 V1 O6 108.80(11) . . ?
O5 V2 O4 109.05(13) . 3_666 ?
O5 V2 O9 108.97(14) . 2 ?
O4 V2 O9 109.84(11) 3_666 2 ?
O5 V2 O2 109.10(12) . . ?
O4 V2 O2 109.44(10) 3_666 . ?
O9 V2 O2 110.41(11) 2 . ?
O3 V3 O1 110.09(10) . . ?
O3 V3 O2 109.42(10) . . ?
O1 V3 O2 109.41(10) . . ?
O3 V3 O6 107.82(10) . . ?
O1 V3 O6 108.56(10) . . ?
O2 V3 O6 111.53(10) . . ?
V3 O1 Ni2 168.40(12) . . ?
Ni1 O1W H1 110(2) . . ?
Ni1 O1W H2 99(4) . . ?
H1 O1W H2 105(5) . . ?
V3 O2 V2 140.90(12) . . ?
Ni1 O2W H3 117(3) . . ?
Ni1 O2W H4 119(2) . . ?
H3 O2W H4 105(4) . . ?
V2 O4 Ni1 167.78(13) 3_666 . ?
V3 O6 V1 133.26(12) . . ?
V1 O9 V2 153.98(18) . 2_545 ?
V1 O8 Ni1 142.01(12) . . ?
C46 N1 C55 116.5(2) . . ?
C46 N1 Ni2 122.27(19) . . ?
C55 N1 Ni2 121.08(19) . . ?
C47 N2 C1 116.7(2) . . ?
C47 N2 Ni2 119.84(18) . . ?
C1 N2 Ni2 122.7(2) . . ?
C36 N3 C65 116.6(3) . . ?
C36 N3 Ni1 121.9(2) . . ?
C65 N3 Ni1 120.9(2) . . ?
C76 N4 C34 116.8(3) . . ?
C76 N4 Ni1 119.48(19) . . ?
C34 N4 Ni1 123.7(2) . . ?
N2 C1 C50 123.0(3) . . ?
N2 C1 H1A 118.5 . . ?
C50 C1 H1A 118.5 . . ?
C40 C25 C71 117.0(3) . . ?
C40 C25 C52 120.4(3) . . ?
C71 C25 C52 122.6(3) . . ?
C37 C30 C54 115.7(3) . . ?
C37 C30 C72 121.9(3) . . ?
C54 C30 C72 122.3(3) . . ?
N4 C34 C54 122.2(3) . . ?
N4 C34 H34A 118.9 . . ?
C54 C34 H34A 118.9 . . ?
N3 C36 C42 123.0(3) . . ?
N3 C36 H36A 118.5 . . ?
C42 C36 H36A 118.5 . . ?
C76 C37 C30 120.7(3) . . ?
C76 C37 H37A 119.7 . . ?
C30 C37 H37A 119.7 . . ?
C55 C40 C25 120.2(3) . . ?
C55 C40 H40A 119.9 . . ?
C25 C40 H40A 119.9 . . ?
C68 C42 C36 120.4(3) . . ?
C68 C42 H42A 119.8 . . ?
C36 C42 H42A 119.8 . . ?
N1 C46 C71 123.3(3) . . ?
N1 C46 H46A 118.3 . . ?
C71 C46 H46A 118.3 . . ?
N2 C47 C53 123.7(3) . . ?
N2 C47 H47A 118.2 . . ?
C53 C47 H47A 118.2 . . ?
C53 C48 C50 116.3(3) . . ?
C53 C48 C59 119.9(3) . . ?
C50 C48 C59 123.8(3) . . ?
C1 C50 C48 120.2(3) . . ?
C1 C50 H50A 119.9 . . ?
C48 C50 H50A 119.9 . . ?
C25 C52 C64 111.8(2) . . ?
C25 C52 H52A 109.3 . . ?
C64 C52 H52A 109.3 . . ?
C25 C52 H52B 109.3 . . ?
C64 C52 H52B 109.3 . . ?
H52A C52 H52B 107.9 . . ?
C47 C53 C48 120.1(3) . . ?
C47 C53 H53A 119.9 . . ?
C48 C53 H53A 119.9 . . ?
C30 C54 C34 120.8(3) . . ?
C30 C54 H54A 119.6 . . ?
C34 C54 H54A 119.6 . . ?
N1 C55 C40 123.4(3) . . ?
N1 C55 H55A 118.3 . . ?
C40 C55 H55A 118.3 . . ?
C48 C59 C64 113.2(3) . 4_565 ?
C48 C59 H59A 108.9 . . ?
C64 C59 H59A 108.9 4_565 . ?
C48 C59 H59B 108.9 . . ?
C64 C59 H59B 108.9 4_565 . ?
H59A C59 H59B 107.8 . . ?
C59 C64 C52 112.4(3) 4_666 . ?
C59 C64 H64A 109.1 4_666 . ?
C52 C64 H64A 109.1 . . ?
C59 C64 H64B 109.1 4_666 . ?
C52 C64 H64B 109.1 . . ?
H64A C64 H64B 107.9 . . ?
N3 C65 C69 123.0(3) . . ?
N3 C65 H65A 118.5 . . ?
C69 C65 H65A 118.5 . . ?
C42 C68 C69 116.6(3) . . ?
C42 C68 C79 123.0(3) . . ?
C69 C68 C79 120.5(3) . . ?
C68 C69 C65 120.4(3) . . ?
C68 C69 H69A 119.8 . . ?
C65 C69 H69A 119.8 . . ?
C46 C71 C25 119.5(3) . . ?
C46 C71 H71A 120.2 . . ?
C25 C71 H71A 120.2 . . ?
C30 C72 C78 108.9(2) . . ?
C30 C72 H72A 109.9 . . ?
C78 C72 H72A 109.9 . . ?
C30 C72 H72B 109.9 . . ?
C78 C72 H72B 109.9 . . ?
H72A C72 H72B 108.3 . . ?
N4 C76 C37 123.9(3) . . ?
N4 C76 H76A 118.1 . . ?
C37 C76 H76A 118.1 . . ?
C79 C78 C72 113.7(3) 2_556 . ?
C79 C78 H78A 108.8 2_556 . ?
C72 C78 H78A 108.8 . . ?
C79 C78 H78B 108.8 2_556 . ?
C72 C78 H78B 108.8 . . ?
H78A C78 H78B 107.7 . . ?
C68 C79 C78 110.8(3) . 2_546 ?
C68 C79 H79A 109.5 . . ?
C78 C79 H79A 109.5 2_546 . ?
C68 C79 H79B 109.5 . . ?
C78 C79 H79B 109.5 2_546 . ?
H79A C79 H79B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1063209'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H56 N8 O24 V6 Zn3'
_chemical_formula_weight         1678.80

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.1897(16)
_cell_length_b                   16.438(2)
_cell_length_c                   15.4725(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.345(2)
_cell_angle_gamma                90.00
_cell_volume                     3277.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    1.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6595
_exptl_absorpt_correction_T_max  0.6819
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24043
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         28.33
_reflns_number_total             8156
_reflns_number_gt                5403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0902P)²+0.4295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8156
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1667
_refine_ls_wR_factor_gt          0.1431
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V -0.65963(5) -0.16658(4) -0.14810(5) 0.01931(17) Uani 1 1 d . . .
V2 V -0.21802(5) -0.00420(4) 0.12255(5) 0.01707(17) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.0000 0.0000 0.02483(18) Uani 1 2 d S . .
Zn2 Zn -0.50973(4) -0.19508(3) 0.07205(4) 0.02749(16) Uani 1 1 d . . .
V3 V -0.27440(6) -0.16026(5) 0.24685(5) 0.02363(19) Uani 1 1 d . . .
C2 C 0.3749(4) 0.0768(3) 0.4094(3) 0.0291(10) Uani 1 1 d . . .
H2A H 0.3653 0.0187 0.4152 0.029 Uiso 1 1 calc R . .
H2B H 0.3144 0.1040 0.4219 0.029 Uiso 1 1 calc R . .
C3 C -0.5979(3) -0.3646(3) 0.0271(3) 0.0280(10) Uani 1 1 d . . .
H3A H -0.6468 -0.3355 -0.0134 0.034 Uiso 1 1 calc R . .
C5 C -0.7119(3) -0.2046(3) 0.1324(3) 0.0262(10) Uani 1 1 d . . .
H5A H -0.7354 -0.2137 0.0721 0.031 Uiso 1 1 calc R . .
C6 C -0.0715(4) 0.1764(3) 0.0324(3) 0.0246(9) Uani 1 1 d . . .
H6A H -0.1108 0.1480 0.0657 0.030 Uiso 1 1 calc R . .
C7 C -0.6130(4) -0.4468(3) 0.0358(3) 0.0301(11) Uani 1 1 d . . .
H7A H -0.6711 -0.4719 0.0015 0.036 Uiso 1 1 calc R . .
C8 C -0.4477(4) -0.3685(3) 0.1322(3) 0.0329(11) Uani 1 1 d . . .
H8A H -0.3906 -0.3420 0.1662 0.039 Uiso 1 1 calc R . .
C9 C -0.8297(4) -0.1854(3) 0.3327(3) 0.0328(11) Uani 1 1 d . . .
H9A H -0.7985 -0.2042 0.3918 0.039 Uiso 1 1 calc R . .
H9B H -0.8898 -0.2190 0.3095 0.039 Uiso 1 1 calc R . .
C10 C -0.4575(4) -0.4503(3) 0.1439(3) 0.0355(12) Uani 1 1 d . . .
H10A H -0.4071 -0.4780 0.1846 0.043 Uiso 1 1 calc R . .
C11 C -0.8623(5) -0.0960(3) 0.3354(4) 0.0416(14) Uani 1 1 d . . .
H11A H -0.8011 -0.0633 0.3579 0.042 Uiso 1 1 calc R . .
H11B H -0.8916 -0.0779 0.2756 0.042 Uiso 1 1 calc R . .
C15 C 0.1102(3) 0.0719(3) 0.1809(3) 0.0229(9) Uani 1 1 d . . .
H15A H 0.0440 0.0910 0.1817 0.028 Uiso 1 1 calc R . .
C18 C -0.0778(4) 0.2600(3) 0.0305(3) 0.0263(10) Uani 1 1 d . . .
H18A H -0.1217 0.2866 0.0610 0.032 Uiso 1 1 calc R . .
C19 C -0.7835(3) -0.2026(3) 0.1840(3) 0.0274(10) Uani 1 1 d . . .
H19A H -0.8535 -0.2090 0.1584 0.033 Uiso 1 1 calc R . .
C20 C 0.0460(4) 0.1766(3) -0.0571(3) 0.0293(10) Uani 1 1 d . . .
H20A H 0.0880 0.1484 -0.0881 0.035 Uiso 1 1 calc R . .
C21 C -0.5804(4) -0.1818(3) 0.2499(3) 0.0350(12) Uani 1 1 d . . .
H21A H -0.5101 -0.1736 0.2735 0.042 Uiso 1 1 calc R . .
C22 C 0.3014(4) 0.0159(3) 0.1809(3) 0.0281(10) Uani 1 1 d . . .
H22A H 0.3665 -0.0050 0.1790 0.034 Uiso 1 1 calc R . .
C24 C 0.3829(4) 0.0956(3) 0.3150(3) 0.0340(11) Uani 1 1 d . . .
H24A H 0.3915 0.1538 0.3094 0.041 Uiso 1 1 calc R . .
H24B H 0.4445 0.0694 0.3033 0.041 Uiso 1 1 calc R . .
C25 C 0.2166(3) -0.0066(3) 0.1178(3) 0.0242(9) Uani 1 1 d . . .
H25A H 0.2261 -0.0435 0.0746 0.029 Uiso 1 1 calc R . .
C26 C 0.1905(3) 0.0966(3) 0.2470(3) 0.0266(10) Uani 1 1 d . . .
H26A H 0.1788 0.1313 0.2913 0.032 Uiso 1 1 calc R . .
C27 C -0.6476(4) -0.1802(4) 0.3060(3) 0.0374(13) Uani 1 1 d . . .
H27A H -0.6224 -0.1718 0.3662 0.045 Uiso 1 1 calc R . .
C28 C -0.0268(4) 0.3958(3) -0.0213(3) 0.0306(11) Uani 1 1 d . . .
H28A H 0.0347 0.4182 -0.0372 0.031 Uiso 1 1 calc R . .
H28B H -0.0306 0.4167 0.0365 0.031 Uiso 1 1 calc R . .
C29 C 0.0458(4) 0.2610(3) -0.0602(3) 0.0282(10) Uani 1 1 d . . .
H29A H 0.0887 0.2882 -0.0911 0.034 Uiso 1 1 calc R . .
C44 C -0.5590(4) -0.5817(3) 0.1074(4) 0.0386(13) Uani 1 1 d . . .
H44A H -0.4937 -0.6073 0.1348 0.039 Uiso 1 1 calc R . .
H44B H -0.5836 -0.6066 0.0499 0.039 Uiso 1 1 calc R . .
N1 N -0.6106(3) -0.1945(2) 0.1628(2) 0.0225(8) Uani 1 1 d . . .
N2 N 0.1211(3) 0.0213(2) 0.1147(2) 0.0205(7) Uani 1 1 d . . .
C55 C -0.0184(4) 0.3049(3) -0.0171(3) 0.0268(10) Uani 1 1 d . . .
N3 N -0.0117(3) 0.1337(2) -0.0111(2) 0.0210(8) Uani 1 1 d . . .
C57 C 0.2910(3) 0.0688(3) 0.2467(3) 0.0246(10) Uani 1 1 d . . .
C56 C -0.7526(4) -0.1911(3) 0.2738(3) 0.0249(9) Uani 1 1 d . . .
N4 N -0.5160(3) -0.3245(2) 0.0744(2) 0.0234(8) Uani 1 1 d . . .
C58 C -0.5415(4) -0.4924(3) 0.0957(3) 0.0309(11) Uani 1 1 d . . .
O1 O -0.6339(2) -0.19195(19) -0.0420(2) 0.0262(7) Uani 1 1 d . . .
O2 O -0.3768(2) -0.1862(2) 0.1706(2) 0.0310(8) Uani 1 1 d . . .
O3 O -0.6963(3) -0.2519(2) -0.2184(3) 0.0472(11) Uani 1 1 d . . .
O5 O -0.1130(2) 0.00119(17) 0.0795(2) 0.0225(7) Uani 1 1 d . . .
O6 O -0.2013(2) -0.08336(19) 0.2028(2) 0.0259(7) Uani 1 1 d . . .
O1W O -0.4092(2) -0.1777(2) -0.0183(2) 0.0312(8) Uani 1 1 d . . .
H1 H -0.3741 -0.1348 -0.0023 0.037 Uiso 1 1 d R . .
H2 H -0.3987 -0.2273 -0.0036 0.037 Uiso 1 1 d R . .
O4 O -0.3207(2) -0.02342(19) 0.0438(2) 0.0267(7) Uani 1 1 d . . .
O2W O -0.5225(2) -0.0637(2) 0.0766(2) 0.0304(8) Uani 1 1 d . . .
H3 H -0.5686 -0.0372 0.0407 0.036 Uiso 1 1 d R . .
H4 H -0.4634 -0.0513 0.0667 0.036 Uiso 1 1 d R . .
O8 O -0.5541(3) -0.1279(3) -0.1690(2) 0.0465(10) Uani 1 1 d . . .
O10 O -0.7629(3) -0.09212(19) -0.1699(2) 0.0312(8) Uani 1 1 d . . .
O7 O -0.3124(3) -0.1231(3) 0.3309(3) 0.0551(12) Uani 1 1 d . . .
O3W O -0.3331(6) 0.0466(4) 0.3652(5) 0.125(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O8 1.624(4) . ?
V1 O1 1.656(3) . ?
V1 O3 1.777(3) . ?
V1 O10 1.809(3) . ?
V2 O4 1.647(3) . ?
V2 O5 1.663(3) . ?
V2 O6 1.780(3) . ?
V2 O10 1.785(3) 3_455 ?
Zn1 O5 2.126(3) 3 ?
Zn1 O5 2.126(3) . ?
Zn1 N2 2.148(3) 3 ?
Zn1 N2 2.148(3) . ?
Zn1 N3 2.207(3) . ?
Zn1 N3 2.207(3) 3 ?
Zn2 O2 2.068(3) . ?
Zn2 N4 2.130(4) . ?
Zn2 N1 2.131(4) . ?
Zn2 O1 2.137(3) . ?
Zn2 O1W 2.141(3) . ?
Zn2 O2W 2.169(3) . ?
Zn2 H2 2.1288 . ?
V3 O7 1.611(4) . ?
V3 O2 1.648(3) . ?
V3 O3 1.789(4) 4_656 ?
V3 O6 1.809(3) . ?
C2 C24 1.518(7) . ?
C2 C28 1.562(6) 4_666 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N4 1.341(6) . ?
C3 C7 1.377(7) . ?
C3 H3A 0.9300 . ?
C5 N1 1.329(5) . ?
C5 C19 1.360(6) . ?
C5 H5A 0.9300 . ?
C6 N3 1.340(6) . ?
C6 C18 1.377(6) . ?
C6 H6A 0.9300 . ?
C7 C58 1.391(7) . ?
C7 H7A 0.9300 . ?
C8 N4 1.338(6) . ?
C8 C10 1.367(7) . ?
C8 H8A 0.9300 . ?
C9 C56 1.506(6) . ?
C9 C11 1.534(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C58 1.382(7) . ?
C10 H10A 0.9300 . ?
C11 C44 1.520(7) 2_355 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C15 N2 1.350(5) . ?
C15 C26 1.367(6) . ?
C15 H15A 0.9300 . ?
C18 C55 1.396(7) . ?
C18 H18A 0.9300 . ?
C19 C56 1.375(7) . ?
C19 H19A 0.9300 . ?
C20 N3 1.347(6) . ?
C20 C29 1.389(6) . ?
C20 H20A 0.9300 . ?
C21 N1 1.339(6) . ?
C21 C27 1.366(7) . ?
C21 H21A 0.9300 . ?
C22 C57 1.368(6) . ?
C22 C25 1.370(6) . ?
C22 H22A 0.9300 . ?
C24 C57 1.494(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N2 1.331(6) . ?
C25 H25A 0.9300 . ?
C26 C57 1.404(6) . ?
C26 H26A 0.9300 . ?
C27 C56 1.380(6) . ?
C27 H27A 0.9300 . ?
C28 C55 1.499(6) . ?
C28 C2 1.562(6) 4_565 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C55 1.385(7) . ?
C29 H29A 0.9300 . ?
C44 C58 1.503(7) . ?
C44 C11 1.520(7) 2_345 ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
O3 V3 1.789(4) 4 ?
O1W H1 0.8501 . ?
O1W H2 0.8499 . ?
O2W H3 0.8501 . ?
O2W H4 0.8501 . ?
O10 V2 1.785(3) 3_455 ?

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 O1 107.06(18) . . ?
O8 V1 O3 108.6(2) . . ?
O1 V1 O3 112.28(18) . . ?
O8 V1 O10 109.96(19) . . ?
O1 V1 O10 109.96(16) . . ?
O3 V1 O10 108.91(16) . . ?
O4 V2 O5 109.71(16) . . ?
O4 V2 O6 109.63(15) . . ?
O5 V2 O6 109.20(15) . . ?
O4 V2 O10 107.95(15) . 3_455 ?
O5 V2 O10 108.64(15) . 3_455 ?
O6 V2 O10 111.68(16) . 3_455 ?
O5 Zn1 O5 180.00(13) 3 . ?
O5 Zn1 N2 90.59(12) 3 3 ?
O5 Zn1 N2 89.41(12) . 3 ?
O5 Zn1 N2 89.41(12) 3 . ?
O5 Zn1 N2 90.59(12) . . ?
N2 Zn1 N2 180.0(2) 3 . ?
O5 Zn1 N3 90.57(12) 3 . ?
O5 Zn1 N3 89.43(12) . . ?
N2 Zn1 N3 94.06(13) 3 . ?
N2 Zn1 N3 85.94(13) . . ?
O5 Zn1 N3 89.43(12) 3 3 ?
O5 Zn1 N3 90.57(12) . 3 ?
N2 Zn1 N3 85.94(13) 3 3 ?
N2 Zn1 N3 94.06(13) . 3 ?
N3 Zn1 N3 180.00(19) . 3 ?
O2 Zn2 N4 95.04(14) . . ?
O2 Zn2 N1 93.69(14) . . ?
N4 Zn2 N1 87.77(14) . . ?
O2 Zn2 O1 170.67(12) . . ?
N4 Zn2 O1 90.71(13) . . ?
N1 Zn2 O1 93.87(13) . . ?
O2 Zn2 O1W 85.78(13) . . ?
N4 Zn2 O1W 100.17(14) . . ?
N1 Zn2 O1W 172.05(14) . . ?
O1 Zn2 O1W 85.98(12) . . ?
O2 Zn2 O2W 88.01(13) . . ?
N4 Zn2 O2W 172.20(13) . . ?
N1 Zn2 O2W 84.86(13) . . ?
O1 Zn2 O2W 87.22(12) . . ?
O1W Zn2 O2W 87.19(13) . . ?
O2 Zn2 H2 81.3 . . ?
N4 Zn2 H2 78.2 . . ?
N1 Zn2 H2 164.5 . . ?
O1 Zn2 H2 92.7 . . ?
O1W Zn2 H2 23.0 . . ?
O2W Zn2 H2 109.4 . . ?
O7 V3 O2 109.1(2) . . ?
O7 V3 O3 108.8(2) . 4_656 ?
O2 V3 O3 109.71(17) . 4_656 ?
O7 V3 O6 108.78(19) . . ?
O2 V3 O6 109.45(15) . . ?
O3 V3 O6 111.00(16) 4_656 . ?
C24 C2 C28 112.6(4) . 4_666 ?
C24 C2 H2A 109.1 . . ?
C28 C2 H2A 109.1 4_666 . ?
C24 C2 H2B 109.1 . . ?
C28 C2 H2B 109.1 4_666 . ?
H2A C2 H2B 107.8 . . ?
N4 C3 C7 123.1(4) . . ?
N4 C3 H3A 118.5 . . ?
C7 C3 H3A 118.5 . . ?
N1 C5 C19 124.1(4) . . ?
N1 C5 H5A 118.0 . . ?
C19 C5 H5A 118.0 . . ?
N3 C6 C18 123.5(4) . . ?
N3 C6 H6A 118.3 . . ?
C18 C6 H6A 118.3 . . ?
C3 C7 C58 120.1(5) . . ?
C3 C7 H7A 119.9 . . ?
C58 C7 H7A 119.9 . . ?
N4 C8 C10 123.4(5) . . ?
N4 C8 H8A 118.3 . . ?
C10 C8 H8A 118.3 . . ?
C56 C9 C11 107.8(4) . . ?
C56 C9 H9A 110.2 . . ?
C11 C9 H9A 110.2 . . ?
C56 C9 H9B 110.2 . . ?
C11 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C8 C10 C58 120.5(5) . . ?
C8 C10 H10A 119.7 . . ?
C58 C10 H10A 119.7 . . ?
C44 C11 C9 113.2(4) 2_355 . ?
C44 C11 H11A 108.9 2_355 . ?
C9 C11 H11A 108.9 . . ?
C44 C11 H11B 108.9 2_355 . ?
C9 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N2 C15 C26 124.0(4) . . ?
N2 C15 H15A 118.0 . . ?
C26 C15 H15A 118.0 . . ?
C6 C18 C55 120.0(4) . . ?
C6 C18 H18A 120.0 . . ?
C55 C18 H18A 120.0 . . ?
C5 C19 C56 120.3(4) . . ?
C5 C19 H19A 119.8 . . ?
C56 C19 H19A 119.8 . . ?
N3 C20 C29 123.0(4) . . ?
N3 C20 H20A 118.5 . . ?
C29 C20 H20A 118.5 . . ?
N1 C21 C27 123.2(4) . . ?
N1 C21 H21A 118.4 . . ?
C27 C21 H21A 118.4 . . ?
C57 C22 C25 120.3(4) . . ?
C57 C22 H22A 119.8 . . ?
C25 C22 H22A 119.8 . . ?
C57 C24 C2 114.1(4) . . ?
C57 C24 H24A 108.7 . . ?
C2 C24 H24A 108.7 . . ?
C57 C24 H24B 108.7 . . ?
C2 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
N2 C25 C22 123.7(4) . . ?
N2 C25 H25A 118.2 . . ?
C22 C25 H25A 118.2 . . ?
C15 C26 C57 118.8(4) . . ?
C15 C26 H26A 120.6 . . ?
C57 C26 H26A 120.6 . . ?
C21 C27 C56 120.4(4) . . ?
C21 C27 H27A 119.8 . . ?
C56 C27 H27A 119.8 . . ?
C55 C28 C2 111.1(4) . 4_565 ?
C55 C28 H28A 109.4 . . ?
C2 C28 H28A 109.4 4_565 . ?
C55 C28 H28B 109.4 . . ?
C2 C28 H28B 109.4 4_565 . ?
H28A C28 H28B 108.0 . . ?
C55 C29 C20 120.0(4) . . ?
C55 C29 H29A 120.0 . . ?
C20 C29 H29A 120.0 . . ?
C58 C44 C11 111.3(4) . 2_345 ?
C58 C44 H44A 109.4 . . ?
C11 C44 H44A 109.4 2_345 . ?
C58 C44 H44B 109.4 . . ?
C11 C44 H44B 109.4 2_345 . ?
H44A C44 H44B 108.0 . . ?
C5 N1 C21 115.9(4) . . ?
C5 N1 Zn2 119.3(3) . . ?
C21 N1 Zn2 124.8(3) . . ?
C25 N2 C15 116.0(4) . . ?
C25 N2 Zn1 120.2(3) . . ?
C15 N2 Zn1 123.1(3) . . ?
C29 C55 C18 116.7(4) . . ?
C29 C55 C28 123.1(4) . . ?
C18 C55 C28 120.3(4) . . ?
C6 N3 C20 116.8(4) . . ?
C6 N3 Zn1 121.4(3) . . ?
C20 N3 Zn1 121.6(3) . . ?
C22 C57 C26 117.1(4) . . ?
C22 C57 C24 121.3(4) . . ?
C26 C57 C24 121.6(4) . . ?
C19 C56 C27 116.1(4) . . ?
C19 C56 C9 121.9(4) . . ?
C27 C56 C9 122.0(4) . . ?
C8 N4 C3 116.6(4) . . ?
C8 N4 Zn2 121.9(3) . . ?
C3 N4 Zn2 120.7(3) . . ?
C10 C58 C7 116.2(4) . . ?
C10 C58 C44 123.3(5) . . ?
C7 C58 C44 120.5(5) . . ?
V1 O1 Zn2 141.52(18) . . ?
V3 O2 Zn2 169.0(2) . . ?
V1 O3 V3 152.3(3) . 4 ?
V2 O5 Zn1 168.13(18) . . ?
V2 O6 V3 140.96(18) . . ?
Zn2 O1W H1 107.2 . . ?
Zn2 O1W H2 77.7 . . ?
H1 O1W H2 132.0 . . ?
Zn2 O2W H3 122.5 . . ?
Zn2 O2W H4 98.8 . . ?
H3 O2W H4 108.4 . . ?
V2 O10 V1 133.66(19) 3_455 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.144
