# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H12 N8 Ni O8 V2'
_chemical_formula_weight         460.81

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

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

_cell_length_a                   15.9628(9)
_cell_length_b                   15.9628(9)
_cell_length_c                   14.4867(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3196.8(4)
_cell_formula_units_Z            9
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2070
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_T_max  0.7238
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6750
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         28.26
_reflns_number_total             1760
_reflns_number_gt                1388
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0891P)²+32.0769P] 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         1760
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1633
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Ni1 Ni 0.0000 0.0000 -0.25942(6) 0.0187(3) Uani 1 3 d S . .
V1 V -0.15211(6) -0.18561(6) -0.43062(5) 0.0214(3) Uani 1 1 d . . .
N1 N -0.1161(3) -0.0218(3) -0.1807(3) 0.0208(8) Uani 1 1 d . . .
O1 O -0.09379(13) -0.11320(13) -0.34388(13) 0.0457(11) Uani 1 1 d . . .
H1WA H -0.4101 -0.0186 -0.1227 0.055 Uiso 1 1 d R . .
H1WB H -0.4678 -0.1155 -0.1046 0.055 Uiso 1 1 d R . .
O1W O -0.44392(13) -0.07384(13) -0.14761(13) 0.0476(12) Uani 1 1 d R . .
C1 C -0.20035(13) -0.03634(13) -0.20812(13) 0.0274(11) Uani 1 1 d R . .
Ni2 Ni 0.00000(13) 0.00000(13) 0.00000(13) 0.0180(3) Uani 1 6 d SR . .
N2 N -0.11705(13) -0.02040(13) -0.08474(13) 0.0215(8) Uani 1 1 d R . .
O2 O -0.21039(13) -0.13825(13) -0.50244(13) 0.0367(9) Uani 1 1 d R . .
C2 C -0.20228(13) -0.03345(13) -0.05855(13) 0.0334(12) Uani 1 1 d R . .
H2A H -0.2222 -0.0351 0.0021 0.040 Uiso 1 1 calc R . .
O3 O -0.2368(3) -0.2866(3) -0.3883(3) 0.0462(11) Uani 1 1 d . . .
N3 N -0.2558(3) -0.0440(4) -0.1353(4) 0.0391(12) Uani 1 1 d . . .
H3A H -0.3138 -0.0537 -0.1368 0.047 Uiso 1 1 calc R . .
N4 N -0.2390(5) -0.0519(5) -0.2917(4) 0.0661(19) Uani 1 1 d . . .
H4A H -0.2069 -0.0536 -0.3386 0.079 Uiso 1 1 calc R . .
H4B H -0.2962 -0.0604 -0.2990 0.079 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
Ni1 N1 2.053(4) 3 ?
Ni1 N1 2.053(4) . ?
Ni1 N1 2.053(4) 2 ?
Ni1 O1 2.0731(19) 3 ?
Ni1 O1 2.0732(19) . ?
Ni1 O1 2.0732(19) 2 ?
V1 O3 1.620(4) . ?
V1 O1 1.645(2) . ?
V1 O2 1.795(2) . ?
V1 O2 1.798(2) 12_554 ?
N1 C1 1.307(4) . ?
N1 N2 1.390(4) . ?
C1 N4 1.324(6) . ?
C1 N3 1.343(5) . ?
Ni2 N2 2.120(4) 10 ?
Ni2 N2 2.120(3) 12 ?
Ni2 N2 2.120(3) 3 ?
Ni2 N2 2.120(3) 11 ?
Ni2 N2 2.1204 . ?
Ni2 N2 2.120(3) 2 ?
N2 C2 1.3247 . ?
O2 V1 1.798(2) 11_554 ?
C2 N3 1.360(6) . ?

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
N1 Ni1 N1 92.10(15) 3 . ?
N1 Ni1 N1 92.10(15) 3 2 ?
N1 Ni1 N1 92.10(15) . 2 ?
N1 Ni1 O1 89.02(12) 3 3 ?
N1 Ni1 O1 90.12(12) . 3 ?
N1 Ni1 O1 177.47(12) 2 3 ?
N1 Ni1 O1 177.48(12) 3 . ?
N1 Ni1 O1 89.01(12) . . ?
N1 Ni1 O1 90.12(12) 2 . ?
O1 Ni1 O1 88.72(8) 3 . ?
N1 Ni1 O1 90.12(12) 3 2 ?
N1 Ni1 O1 177.48(13) . 2 ?
N1 Ni1 O1 89.01(12) 2 2 ?
O1 Ni1 O1 88.72(8) 3 2 ?
O1 Ni1 O1 88.72(8) . 2 ?
O3 V1 O1 107.91(19) . . ?
O3 V1 O2 106.75(18) . . ?
O1 V1 O2 112.16(11) . . ?
O3 V1 O2 108.46(19) . 12_554 ?
O1 V1 O2 110.62(13) . 12_554 ?
O2 V1 O2 110.76(6) . 12_554 ?
C1 N1 N2 106.8(3) . . ?
C1 N1 Ni1 128.5(3) . . ?
N2 N1 Ni1 124.7(2) . . ?
V1 O1 Ni1 166.32(12) . . ?
N1 C1 N4 130.7(4) . . ?
N1 C1 N3 110.5(3) . . ?
N4 C1 N3 118.5(4) . . ?
N2 Ni2 N2 89.84(12) 10 12 ?
N2 Ni2 N2 90.16(12) 10 3 ?
N2 Ni2 N2 180.00(13) 12 3 ?
N2 Ni2 N2 89.84(12) 10 11 ?
N2 Ni2 N2 89.84(14) 12 11 ?
N2 Ni2 N2 90.16(10) 3 11 ?
N2 Ni2 N2 180.00(18) 10 . ?
N2 Ni2 N2 90.16(7) 12 . ?
N2 Ni2 N2 89.84(7) 3 . ?
N2 Ni2 N2 90.16(7) 11 . ?
N2 Ni2 N2 90.16(12) 10 2 ?
N2 Ni2 N2 90.16(10) 12 2 ?
N2 Ni2 N2 89.8 3 2 ?
N2 Ni2 N2 180.00(12) 11 2 ?
N2 Ni2 N2 89.84(7) . 2 ?
C2 N2 N1 107.60(17) . . ?
C2 N2 Ni2 128.0 . . ?
N1 N2 Ni2 124.44(17) . . ?
V1 O2 V1 141.72(12) . 11_554 ?
N2 C2 N3 108.5(2) . . ?
C1 N3 C2 106.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.730
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.168
_database_code_depnum_ccdc_archive 'CCDC 992973'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H32 N24 Ni3 O22 V6'
_chemical_formula_weight         1346.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.7732(6)
_cell_length_b                   10.5394(6)
_cell_length_c                   11.4624(7)
_cell_angle_alpha                105.6930(10)
_cell_angle_beta                 91.6000(10)
_cell_angle_gamma                114.3860(10)
_cell_volume                     1022.05(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             670
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_T_max  0.6360
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5287
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3589
_reflns_number_gt                3148
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0466P)²+1.7985P] 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         3589
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 0.21253(4) 0.59149(4) 0.31356(4) 0.01369(12) Uani 1 1 d . . .
V1 V 0.21260(6) 0.86981(6) 0.58539(5) 0.01657(15) Uani 1 1 d . . .
O1 O 0.1929(3) 0.7227(3) 0.4765(2) 0.0307(6) Uani 1 1 d . . .
N1 N 0.2407(3) 0.7440(3) 0.2242(3) 0.0191(6) Uani 1 1 d . . .
C1 C -0.1134(4) 0.4841(4) 0.3459(3) 0.0192(7) Uani 1 1 d . . .
H4 H -0.0852 0.5024 0.4292 0.023 Uiso 1 1 calc R . .
O1W O 0.0084(7) 0.8596(7) 0.3063(6) 0.133(2) Uani 1 1 d . . .
H1WA H 0.0994 0.8825 0.2931 0.160 Uiso 1 1 d R . .
H1WB H 0.0002 0.9386 0.3374 0.160 Uiso 1 1 d R . .
Ni2 Ni 0.0000 0.5000 0.0000 0.01339(14) Uani 1 2 d S . .
V2 V 0.16107(6) 0.26181(6) 0.38070(5) 0.01698(15) Uani 1 1 d . . .
O2 O 0.0288(3) 0.8582(3) 0.6113(3) 0.0423(8) Uani 1 1 d . . .
N2 N 0.1633(3) 0.7084(3) 0.1084(3) 0.0193(6) Uani 1 1 d . . .
C2 C -0.2478(4) 0.4224(4) 0.1702(3) 0.0197(7) Uani 1 1 d . . .
H3 H -0.3303 0.3895 0.1092 0.024 Uiso 1 1 calc R . .
O2W O 0.8956(4) 0.0318(4) 0.0946(3) 0.0616(10) Uani 1 1 d . . .
H2WA H 0.9439 0.0872 0.1658 0.074 Uiso 1 1 d R . .
H2WB H 0.8344 -0.0502 0.1014 0.074 Uiso 1 1 d R . .
V3 V 0.62124(6) 0.77607(6) 0.39854(5) 0.01640(14) Uani 1 1 d . . .
O3 O 0.3210(3) 1.0307(3) 0.5431(3) 0.0316(6) Uani 1 1 d . . .
N3 N -0.1053(3) 0.4664(3) 0.1537(2) 0.0162(6) Uani 1 1 d . . .
C3 C 0.3431(4) 0.4164(4) 0.1387(3) 0.0205(7) Uani 1 1 d . . .
H8 H 0.4217 0.4382 0.1995 0.025 Uiso 1 1 calc R . .
O4 O 0.3005(3) 0.8778(3) 0.7113(3) 0.0428(8) Uani 1 1 d . . .
N4 N -0.0198(3) 0.5049(3) 0.2664(2) 0.0170(6) Uani 1 1 d . . .
C4 C 0.1932(4) 0.3254(4) -0.0350(3) 0.0219(7) Uani 1 1 d . . .
H7 H 0.1484 0.2717 -0.1161 0.026 Uiso 1 1 calc R . .
O5 O 0.1761(3) 0.4269(2) 0.3898(2) 0.0200(5) Uani 1 1 d . . .
N5 N -0.2563(3) 0.4321(3) 0.2893(3) 0.0172(6) Uani 1 1 d . . .
C5 C 0.2175(4) 0.8267(4) 0.0745(3) 0.0213(7) Uani 1 1 d . . .
H12 H 0.1854 0.8335 0.0002 0.026 Uiso 1 1 calc R . .
O6 O 0.2906(4) 0.2841(3) 0.5041(3) 0.0552(10) Uani 1 1 d . . .
N6 N -0.3923(3) 0.3928(3) 0.3399(3) 0.0231(7) Uani 1 1 d . . .
H1 H -0.3969 0.3330 0.3796 0.028 Uiso 1 1 d R . .
H2 H -0.3924 0.4705 0.3892 0.028 Uiso 1 1 d R . .
C6 C 0.3373(4) 0.8827(4) 0.2566(3) 0.0210(7) Uani 1 1 d . . .
H11 H 0.4025 0.9354 0.3311 0.025 Uiso 1 1 calc R . .
O7 O 0.2016(4) 0.1908(3) 0.2509(3) 0.0438(8) Uani 1 1 d . . .
N7 N 0.1460(3) 0.4102(3) 0.0411(3) 0.0171(6) Uani 1 1 d . . .
O8 O 0.4361(3) 0.6867(3) 0.3867(3) 0.0326(6) Uani 1 1 d . . .
N8 N 0.2403(3) 0.4667(3) 0.1528(2) 0.0175(6) Uani 1 1 d . . .
O9 O 0.6645(4) 0.7337(4) 0.2640(3) 0.0603(10) Uani 1 1 d . . .
N9 N 0.3174(3) 0.3284(3) 0.0229(3) 0.0205(6) Uani 1 1 d . . .
N10 N 0.4112(3) 0.2602(4) -0.0230(3) 0.0279(7) Uani 1 1 d . . .
H5 H 0.3822 0.1793 -0.0060 0.034 Uiso 1 1 d R . .
H6 H 0.4028 0.2425 -0.1013 0.034 Uiso 1 1 d R . .
N11 N 0.3270(3) 0.9370(3) 0.1639(3) 0.0200(6) Uani 1 1 d . . .
N12 N 0.4142(4) 1.0799(3) 0.1580(3) 0.0273(7) Uani 1 1 d . . .
H9 H 0.4270 1.0756 0.0833 0.033 Uiso 1 1 d R . .
H10 H 0.3668 1.1326 0.1831 0.033 Uiso 1 1 d 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
Ni1 O8 2.029(3) . ?
Ni1 N8 2.052(3) . ?
Ni1 O5 2.056(2) . ?
Ni1 N4 2.058(3) . ?
Ni1 N1 2.062(3) . ?
Ni1 O1 2.069(3) . ?
V1 O4 1.623(3) . ?
V1 O1 1.641(2) . ?
V1 O2 1.788(3) . ?
V1 O3 1.795(3) . ?
N1 C6 1.309(4) . ?
N1 N2 1.383(4) . ?
C1 N4 1.306(4) . ?
C1 N5 1.341(4) . ?
C1 H4 0.9300 . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8499 . ?
Ni2 N3 2.104(3) . ?
Ni2 N3 2.104(3) 2_565 ?
Ni2 N2 2.106(3) . ?
Ni2 N2 2.106(3) 2_565 ?
Ni2 N7 2.115(3) . ?
Ni2 N7 2.115(3) 2_565 ?
V2 O7 1.614(3) . ?
V2 O5 1.658(2) . ?
V2 O6 1.770(3) . ?
V2 O2 1.785(3) 2_566 ?
O2 V2 1.785(3) 2_566 ?
N2 C5 1.310(4) . ?
C2 N3 1.311(4) . ?
C2 N5 1.348(4) . ?
C2 H3 0.9300 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8499 . ?
V3 O9 1.606(3) . ?
V3 O8 1.640(3) . ?
V3 O6 1.781(3) 2_666 ?
V3 O3 1.791(3) 2_676 ?
O3 V3 1.791(3) 2_676 ?
N3 N4 1.381(4) . ?
C3 N8 1.311(4) . ?
C3 N9 1.345(4) . ?
C3 H8 0.9300 . ?
C4 N7 1.309(5) . ?
C4 N9 1.352(4) . ?
C4 H7 0.9300 . ?
N5 N6 1.412(4) . ?
C5 N11 1.347(4) . ?
C5 H12 0.9300 . ?
O6 V3 1.781(3) 2_666 ?
N6 H1 0.8600 . ?
N6 H2 0.8600 . ?
C6 N11 1.355(4) . ?
C6 H11 0.9300 . ?
N7 N8 1.383(4) . ?
N9 N10 1.414(4) . ?
N10 H5 0.8600 . ?
N10 H6 0.8600 . ?
N11 N12 1.414(4) . ?
N12 H9 0.8600 . ?
N12 H10 0.8598 . ?

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 Ni1 N8 94.01(11) . . ?
O8 Ni1 O5 89.49(10) . . ?
N8 Ni1 O5 90.05(10) . . ?
O8 Ni1 N4 171.30(11) . . ?
N8 Ni1 N4 94.22(11) . . ?
O5 Ni1 N4 87.70(10) . . ?
O8 Ni1 N1 93.27(11) . . ?
N8 Ni1 N1 86.26(11) . . ?
O5 Ni1 N1 175.54(10) . . ?
N4 Ni1 N1 90.06(11) . . ?
O8 Ni1 O1 84.05(11) . . ?
N8 Ni1 O1 177.88(11) . . ?
O5 Ni1 O1 90.79(10) . . ?
N4 Ni1 O1 87.76(11) . . ?
N1 Ni1 O1 92.98(11) . . ?
O4 V1 O1 109.06(15) . . ?
O4 V1 O2 108.32(17) . . ?
O1 V1 O2 109.35(14) . . ?
O4 V1 O3 109.38(14) . . ?
O1 V1 O3 110.11(13) . . ?
O2 V1 O3 110.58(13) . . ?
V1 O1 Ni1 160.40(16) . . ?
C6 N1 N2 107.6(3) . . ?
C6 N1 Ni1 129.2(2) . . ?
N2 N1 Ni1 123.0(2) . . ?
N4 C1 N5 109.6(3) . . ?
N4 C1 H4 125.2 . . ?
N5 C1 H4 125.2 . . ?
H1WA O1W H1WB 107.7 . . ?
N3 Ni2 N3 180.0 . 2_565 ?
N3 Ni2 N2 90.44(11) . . ?
N3 Ni2 N2 89.56(11) 2_565 . ?
N3 Ni2 N2 89.56(11) . 2_565 ?
N3 Ni2 N2 90.44(11) 2_565 2_565 ?
N2 Ni2 N2 179.999(1) . 2_565 ?
N3 Ni2 N7 90.74(10) . . ?
N3 Ni2 N7 89.26(10) 2_565 . ?
N2 Ni2 N7 88.96(11) . . ?
N2 Ni2 N7 91.04(11) 2_565 . ?
N3 Ni2 N7 89.26(10) . 2_565 ?
N3 Ni2 N7 90.74(10) 2_565 2_565 ?
N2 Ni2 N7 91.04(11) . 2_565 ?
N2 Ni2 N7 88.96(11) 2_565 2_565 ?
N7 Ni2 N7 180.0 . 2_565 ?
O7 V2 O5 109.96(14) . . ?
O7 V2 O6 110.66(18) . . ?
O5 V2 O6 107.08(13) . . ?
O7 V2 O2 107.35(16) . 2_566 ?
O5 V2 O2 110.90(12) . 2_566 ?
O6 V2 O2 110.93(17) . 2_566 ?
V2 O2 V1 144.81(17) 2_566 . ?
C5 N2 N1 107.3(3) . . ?
C5 N2 Ni2 125.7(2) . . ?
N1 N2 Ni2 126.9(2) . . ?
N3 C2 N5 109.4(3) . . ?
N3 C2 H3 125.3 . . ?
N5 C2 H3 125.3 . . ?
H2WA O2W H2WB 107.7 . . ?
O9 V3 O8 107.45(18) . . ?
O9 V3 O6 108.6(2) . 2_666 ?
O8 V3 O6 108.59(16) . 2_666 ?
O9 V3 O3 110.49(17) . 2_676 ?
O8 V3 O3 110.10(13) . 2_676 ?
O6 V3 O3 111.52(14) 2_666 2_676 ?
V3 O3 V1 138.05(17) 2_676 . ?
C2 N3 N4 107.0(3) . . ?
C2 N3 Ni2 131.9(2) . . ?
N4 N3 Ni2 120.9(2) . . ?
N8 C3 N9 109.5(3) . . ?
N8 C3 H8 125.3 . . ?
N9 C3 H8 125.3 . . ?
C1 N4 N3 107.5(3) . . ?
C1 N4 Ni1 123.2(2) . . ?
N3 N4 Ni1 129.3(2) . . ?
N7 C4 N9 109.2(3) . . ?
N7 C4 H7 125.4 . . ?
N9 C4 H7 125.4 . . ?
V2 O5 Ni1 151.02(14) . . ?
C1 N5 C2 106.5(3) . . ?
C1 N5 N6 128.5(3) . . ?
C2 N5 N6 124.9(3) . . ?
N2 C5 N11 109.4(3) . . ?
N2 C5 H12 125.3 . . ?
N11 C5 H12 125.3 . . ?
V2 O6 V3 155.4(2) . 2_666 ?
N5 N6 H1 109.1 . . ?
N5 N6 H2 109.0 . . ?
H1 N6 H2 109.5 . . ?
N1 C6 N11 108.9(3) . . ?
N1 C6 H11 125.5 . . ?
N11 C6 H11 125.5 . . ?
C4 N7 N8 107.4(3) . . ?
C4 N7 Ni2 128.4(2) . . ?
N8 N7 Ni2 122.1(2) . . ?
V3 O8 Ni1 159.31(18) . . ?
C3 N8 N7 107.2(3) . . ?
C3 N8 Ni1 126.6(2) . . ?
N7 N8 Ni1 126.0(2) . . ?
C3 N9 C4 106.6(3) . . ?
C3 N9 N10 123.5(3) . . ?
C4 N9 N10 129.8(3) . . ?
N9 N10 H5 109.1 . . ?
N9 N10 H6 109.0 . . ?
H5 N10 H6 109.5 . . ?
C5 N11 C6 106.8(3) . . ?
C5 N11 N12 125.3(3) . . ?
C6 N11 N12 128.0(3) . . ?
N11 N12 H9 109.4 . . ?
N11 N12 H10 109.2 . . ?
H9 N12 H10 109.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V1 O1 Ni1 -118.7(5) . . . . ?
O2 V1 O1 Ni1 123.0(5) . . . . ?
O3 V1 O1 Ni1 1.3(6) . . . . ?
O5 Ni1 O1 V1 155.6(5) . . . . ?
N4 Ni1 O1 V1 -116.7(5) . . . . ?
N1 Ni1 O1 V1 -26.8(5) . . . . ?
O8 Ni1 N1 C6 -31.6(3) . . . . ?
N8 Ni1 N1 C6 -125.4(3) . . . . ?
N4 Ni1 N1 C6 140.3(3) . . . . ?
O1 Ni1 N1 C6 52.6(3) . . . . ?
O8 Ni1 N1 N2 142.3(3) . . . . ?
N8 Ni1 N1 N2 48.4(2) . . . . ?
N4 Ni1 N1 N2 -45.8(3) . . . . ?
O1 Ni1 N1 N2 -133.5(3) . . . . ?
O4 V1 O2 V2 -80.8(4) . . . 2_566 ?
O1 V1 O2 V2 37.9(4) . . . 2_566 ?
O3 V1 O2 V2 159.3(3) . . . 2_566 ?
C6 N1 N2 C5 0.8(4) . . . . ?
Ni1 N1 N2 C5 -174.2(2) . . . . ?
C6 N1 N2 Ni2 176.6(2) . . . . ?
Ni1 N1 N2 Ni2 1.6(4) . . . . ?
N3 Ni2 N2 C5 -140.3(3) . . . . ?
N3 Ni2 N2 C5 39.7(3) 2_565 . . . ?
N7 Ni2 N2 C5 129.0(3) . . . . ?
N7 Ni2 N2 C5 -51.0(3) 2_565 . . . ?
N3 Ni2 N2 N1 44.6(3) . . . . ?
N3 Ni2 N2 N1 -135.4(3) 2_565 . . . ?
N7 Ni2 N2 N1 -46.2(3) . . . . ?
N7 Ni2 N2 N1 133.8(3) 2_565 . . . ?
O4 V1 O3 V3 -65.9(3) . . . 2_676 ?
O1 V1 O3 V3 174.2(2) . . . 2_676 ?
O2 V1 O3 V3 53.3(3) . . . 2_676 ?
N5 C2 N3 N4 0.3(4) . . . . ?
N5 C2 N3 Ni2 -174.0(2) . . . . ?
N2 Ni2 N3 C2 130.7(3) . . . . ?
N2 Ni2 N3 C2 -49.3(3) 2_565 . . . ?
N7 Ni2 N3 C2 -140.3(3) . . . . ?
N7 Ni2 N3 C2 39.7(3) 2_565 . . . ?
N2 Ni2 N3 N4 -43.0(2) . . . . ?
N2 Ni2 N3 N4 137.0(2) 2_565 . . . ?
N7 Ni2 N3 N4 46.0(2) . . . . ?
N7 Ni2 N3 N4 -134.0(2) 2_565 . . . ?
N5 C1 N4 N3 0.7(4) . . . . ?
N5 C1 N4 Ni1 177.5(2) . . . . ?
C2 N3 N4 C1 -0.6(4) . . . . ?
Ni2 N3 N4 C1 174.5(2) . . . . ?
C2 N3 N4 Ni1 -177.2(2) . . . . ?
Ni2 N3 N4 Ni1 -2.1(4) . . . . ?
N8 Ni1 N4 C1 145.5(3) . . . . ?
O5 Ni1 N4 C1 55.6(3) . . . . ?
N1 Ni1 N4 C1 -128.3(3) . . . . ?
O1 Ni1 N4 C1 -35.3(3) . . . . ?
N8 Ni1 N4 N3 -38.4(3) . . . . ?
O5 Ni1 N4 N3 -128.3(3) . . . . ?
N1 Ni1 N4 N3 47.9(3) . . . . ?
O1 Ni1 N4 N3 140.8(3) . . . . ?
O7 V2 O5 Ni1 5.1(3) . . . . ?
O6 V2 O5 Ni1 125.3(3) . . . . ?
O2 V2 O5 Ni1 -113.5(3) 2_566 . . . ?
O8 Ni1 O5 V2 -94.1(3) . . . . ?
N8 Ni1 O5 V2 -0.1(3) . . . . ?
N4 Ni1 O5 V2 94.1(3) . . . . ?
O1 Ni1 O5 V2 -178.2(3) . . . . ?
N4 C1 N5 C2 -0.4(4) . . . . ?
N4 C1 N5 N6 179.1(3) . . . . ?
N3 C2 N5 C1 0.0(4) . . . . ?
N3 C2 N5 N6 -179.5(3) . . . . ?
N1 N2 C5 N11 0.1(4) . . . . ?
Ni2 N2 C5 N11 -175.8(2) . . . . ?
O7 V2 O6 V3 -66.8(7) . . . 2_666 ?
O5 V2 O6 V3 173.4(6) . . . 2_666 ?
O2 V2 O6 V3 52.3(7) 2_566 . . 2_666 ?
N2 N1 C6 N11 -1.3(4) . . . . ?
Ni1 N1 C6 N11 173.3(2) . . . . ?
N9 C4 N7 N8 -1.6(4) . . . . ?
N9 C4 N7 Ni2 161.7(2) . . . . ?
N3 Ni2 N7 C4 141.6(3) . . . . ?
N3 Ni2 N7 C4 -38.4(3) 2_565 . . . ?
N2 Ni2 N7 C4 -128.0(3) . . . . ?
N2 Ni2 N7 C4 52.0(3) 2_565 . . . ?
N3 Ni2 N7 N8 -57.2(2) . . . . ?
N3 Ni2 N7 N8 122.8(2) 2_565 . . . ?
N2 Ni2 N7 N8 33.2(2) . . . . ?
N2 Ni2 N7 N8 -146.8(2) 2_565 . . . ?
O9 V3 O8 Ni1 -35.1(5) . . . . ?
O6 V3 O8 Ni1 -152.3(5) 2_666 . . . ?
O3 V3 O8 Ni1 85.3(5) 2_676 . . . ?
N8 Ni1 O8 V3 53.3(5) . . . . ?
O5 Ni1 O8 V3 143.3(5) . . . . ?
N1 Ni1 O8 V3 -33.2(5) . . . . ?
O1 Ni1 O8 V3 -125.9(5) . . . . ?
N9 C3 N8 N7 -0.7(4) . . . . ?
N9 C3 N8 Ni1 174.4(2) . . . . ?
C4 N7 N8 C3 1.4(4) . . . . ?
Ni2 N7 N8 C3 -163.2(2) . . . . ?
C4 N7 N8 Ni1 -173.8(2) . . . . ?
Ni2 N7 N8 Ni1 21.6(3) . . . . ?
O8 Ni1 N8 C3 29.7(3) . . . . ?
O5 Ni1 N8 C3 -59.8(3) . . . . ?
N4 Ni1 N8 C3 -147.5(3) . . . . ?
N1 Ni1 N8 C3 122.7(3) . . . . ?
O8 Ni1 N8 N7 -156.0(3) . . . . ?
O5 Ni1 N8 N7 114.5(3) . . . . ?
N4 Ni1 N8 N7 26.8(3) . . . . ?
N1 Ni1 N8 N7 -63.0(3) . . . . ?
N8 C3 N9 C4 -0.2(4) . . . . ?
N8 C3 N9 N10 177.9(3) . . . . ?
N7 C4 N9 C3 1.1(4) . . . . ?
N7 C4 N9 N10 -176.9(3) . . . . ?
N2 C5 N11 C6 -0.9(4) . . . . ?
N2 C5 N11 N12 178.0(3) . . . . ?
N1 C6 N11 C5 1.4(4) . . . . ?
N1 C6 N11 N12 -177.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.095
_database_code_depnum_ccdc_archive 'CCDC 992974'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H32 Co3 N24 O22 V6'
_chemical_formula_weight         1347.05

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.8432(7)
_cell_length_b                   10.5655(7)
_cell_length_c                   11.5289(8)
_cell_angle_alpha                105.8110(10)
_cell_angle_beta                 91.5940(10)
_cell_angle_gamma                114.2520(10)
_cell_volume                     1038.38(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             667
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7001
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5376
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3643
_reflns_number_gt                3049
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3643
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1094
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Co1 Co 0.71518(6) 0.09221(6) 0.31923(5) 0.01556(17) Uani 1 1 d . . .
V1 V 0.65905(8) -0.24208(7) 0.38104(7) 0.0188(2) Uani 1 1 d . . .
O1 O 0.6757(3) -0.0768(3) 0.3896(3) 0.0237(7) Uani 1 1 d . . .
C1 C 0.8438(5) -0.0850(5) 0.1386(4) 0.0237(10) Uani 1 1 d . . .
H1A H 0.9211 -0.0640 0.1992 0.028 Uiso 1 1 calc R . .
N1 N 0.7438(4) -0.0342(4) 0.1527(3) 0.0197(8) Uani 1 1 d . . .
O1W O 0.3958(5) -0.4695(5) 0.0922(4) 0.0622(12) Uani 1 1 d . . .
H1WA H 0.3578 -0.4501 0.1562 0.075 Uiso 1 1 d R . .
H1WB H 0.4912 -0.4237 0.1114 0.075 Uiso 1 1 d R . .
Co2 Co 0.5000 0.0000 0.0000 0.0155(2) Uani 1 2 d S . .
V2 V 0.87734(8) -0.27767(7) 0.60103(6) 0.0184(2) Uani 1 1 d . . .
C2 C 0.6972(5) -0.1749(5) -0.0336(4) 0.0228(10) Uani 1 1 d . . .
H2A H 0.6530 -0.2285 -0.1144 0.027 Uiso 1 1 calc R . .
N2 N 0.6493(4) -0.0904(4) 0.0418(3) 0.0200(8) Uani 1 1 d . . .
O2 O 0.7038(5) -0.3118(4) 0.2532(4) 0.0504(10) Uani 1 1 d . . .
O2W O 0.4961(8) -0.3574(8) 0.6950(7) 0.138(3) Uani 1 1 d . . .
H2WA H 0.5023 -0.4376 0.6662 0.166 Uiso 1 1 d R . .
H2WB H 0.4051 -0.3776 0.7048 0.166 Uiso 1 1 d R . .
V3 V 0.71278(8) -0.62922(7) 0.58952(6) 0.01799(19) Uani 1 1 d . . .
N3 N 0.8192(4) -0.1726(4) 0.0231(3) 0.0217(8) Uani 1 1 d . . .
O3 O 0.7822(5) -0.2216(4) 0.5071(4) 0.0609(14) Uani 1 1 d . . .
C3 C 0.3853(5) -0.0147(5) 0.3470(4) 0.0209(9) Uani 1 1 d . . .
H3A H 0.4133 0.0040 0.4299 0.025 Uiso 1 1 calc R . .
N4 N 0.9122(4) -0.2415(4) -0.0220(4) 0.0294(9) Uani 1 1 d . . .
H4C H 0.9285 -0.2425 -0.0902 0.035 Uiso 1 1 d R . .
H4B H 0.8744 -0.3292 -0.0112 0.035 Uiso 1 1 d R . .
C4 C 0.2525(5) -0.0791(5) 0.1721(4) 0.0221(10) Uani 1 1 d . . .
H4A H 0.1705 -0.1139 0.1111 0.027 Uiso 1 1 calc R . .
O4 O 0.8441(5) -0.2305(5) 0.7380(4) 0.0605(12) Uani 1 1 d . . .
C5 C 0.8398(5) 0.3841(5) 0.2567(4) 0.0224(10) Uani 1 1 d . . .
H5A H 0.9059 0.4365 0.3301 0.027 Uiso 1 1 calc R . .
O5 O 1.0598(4) -0.1896(4) 0.6052(3) 0.0365(8) Uani 1 1 d . . .
N5 N 0.4786(4) 0.0057(4) 0.2677(3) 0.0193(8) Uani 1 1 d . . .
O6 O 0.8207(4) -0.4709(3) 0.5457(3) 0.0347(8) Uani 1 1 d . . .
N6 N 0.3928(4) -0.0351(4) 0.1555(3) 0.0204(8) Uani 1 1 d . . .
C6 C 0.7202(5) 0.3296(5) 0.0787(4) 0.0246(10) Uani 1 1 d . . .
H6A H 0.6877 0.3367 0.0052 0.030 Uiso 1 1 calc R . .
O7 O 0.7991(4) -0.6200(4) 0.7150(3) 0.0455(10) Uani 1 1 d . . .
N7 N 0.2437(4) -0.0666(4) 0.2909(3) 0.0186(8) Uani 1 1 d . . .
O8 O 0.5309(4) -0.6388(4) 0.6155(4) 0.0430(10) Uani 1 1 d . . .
N8 N 0.1081(4) -0.1055(4) 0.3407(3) 0.0253(8) Uani 1 1 d . . .
H8A H 0.1087 -0.1429 0.3835 0.030 Uiso 1 1 d R . .
H8B H 0.1166 -0.0334 0.3904 0.030 Uiso 1 1 d R . .
O9 O 0.6927(4) -0.7777(3) 0.4826(3) 0.0348(8) Uani 1 1 d . . .
N9 N 0.7442(4) 0.2477(4) 0.2267(3) 0.0217(8) Uani 1 1 d . . .
N10 N 0.6660(4) 0.2117(4) 0.1113(3) 0.0221(8) Uani 1 1 d . . .
N11 N 0.8293(4) 0.4389(4) 0.1661(3) 0.0205(8) Uani 1 1 d . . .
N12 N 0.9148(4) 0.5803(4) 0.1575(4) 0.0282(9) Uani 1 1 d . . .
H12A H 1.0062 0.6003 0.1768 0.034 Uiso 1 1 d R . .
H12B H 0.8819 0.6470 0.2056 0.034 Uiso 1 1 d 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
Co1 O1 2.058(3) . ?
Co1 O5 2.063(3) 2_756 ?
Co1 O9 2.085(3) 1_565 ?
Co1 N5 2.119(3) . ?
Co1 N1 2.120(4) . ?
Co1 N9 2.122(3) . ?
V1 O2 1.619(4) . ?
V1 O1 1.660(3) . ?
V1 O3 1.773(3) . ?
V1 O8 1.783(3) 2_646 ?
C1 N1 1.295(6) . ?
C1 N3 1.347(5) . ?
N1 N2 1.385(5) . ?
Co2 N6 2.147(3) . ?
Co2 N6 2.147(3) 2_655 ?
Co2 N10 2.153(3) . ?
Co2 N10 2.153(3) 2_655 ?
Co2 N2 2.160(3) . ?
Co2 N2 2.160(3) 2_655 ?
V2 O4 1.607(4) . ?
V2 O5 1.640(3) . ?
V2 O3 1.775(3) . ?
V2 O6 1.795(3) . ?
C2 N2 1.312(6) . ?
C2 N3 1.339(5) . ?
V3 O7 1.616(3) . ?
V3 O9 1.643(3) . ?
V3 O8 1.789(3) . ?
V3 O6 1.792(3) . ?
N3 N4 1.416(5) . ?
C3 N5 1.311(5) . ?
C3 N7 1.338(5) . ?
C4 N6 1.302(6) . ?
C4 N7 1.349(5) . ?
C5 N9 1.296(5) . ?
C5 N11 1.344(5) . ?
O5 Co1 2.063(3) 2_756 ?
N5 N6 1.382(5) . ?
C6 N10 1.302(6) . ?
C6 N11 1.338(5) . ?
N7 N8 1.414(5) . ?
O8 V1 1.783(3) 2_646 ?
O9 Co1 2.085(3) 1_545 ?
N9 N10 1.391(5) . ?
N11 N12 1.415(5) . ?

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 Co1 O5 90.62(13) . 2_756 ?
O1 Co1 O9 91.95(13) . 1_565 ?
O5 Co1 O9 84.10(14) 2_756 1_565 ?
O1 Co1 N5 87.91(13) . . ?
O5 Co1 N5 171.56(14) 2_756 . ?
O9 Co1 N5 87.64(14) 1_565 . ?
O1 Co1 N1 89.41(13) . . ?
O5 Co1 N1 94.72(14) 2_756 . ?
O9 Co1 N1 178.21(14) 1_565 . ?
N5 Co1 N1 93.58(13) . . ?
O1 Co1 N9 173.36(12) . . ?
O5 Co1 N9 93.33(14) 2_756 . ?
O9 Co1 N9 93.77(14) 1_565 . ?
N5 Co1 N9 88.95(14) . . ?
N1 Co1 N9 84.95(14) . . ?
O2 V1 O1 109.55(18) . . ?
O2 V1 O3 111.0(2) . . ?
O1 V1 O3 107.20(16) . . ?
O2 V1 O8 107.50(19) . 2_646 ?
O1 V1 O8 110.87(16) . 2_646 ?
O3 V1 O8 110.7(2) . 2_646 ?
V1 O1 Co1 152.98(18) . . ?
N1 C1 N3 110.0(4) . . ?
C1 N1 N2 107.4(4) . . ?
C1 N1 Co1 126.2(3) . . ?
N2 N1 Co1 126.1(3) . . ?
N6 Co2 N6 180.0 . 2_655 ?
N6 Co2 N10 90.52(13) . . ?
N6 Co2 N10 89.48(13) 2_655 . ?
N6 Co2 N10 89.48(13) . 2_655 ?
N6 Co2 N10 90.52(13) 2_655 2_655 ?
N10 Co2 N10 180.000(1) . 2_655 ?
N6 Co2 N2 90.82(13) . . ?
N6 Co2 N2 89.18(13) 2_655 . ?
N10 Co2 N2 88.29(13) . . ?
N10 Co2 N2 91.71(13) 2_655 . ?
N6 Co2 N2 89.18(13) . 2_655 ?
N6 Co2 N2 90.82(13) 2_655 2_655 ?
N10 Co2 N2 91.71(13) . 2_655 ?
N10 Co2 N2 88.29(13) 2_655 2_655 ?
N2 Co2 N2 180.0 . 2_655 ?
O4 V2 O5 107.1(2) . . ?
O4 V2 O3 108.7(2) . . ?
O5 V2 O3 108.8(2) . . ?
O4 V2 O6 110.7(2) . . ?
O5 V2 O6 109.69(17) . . ?
O3 V2 O6 111.74(17) . . ?
N2 C2 N3 109.9(4) . . ?
C2 N2 N1 106.6(3) . . ?
C2 N2 Co2 128.7(3) . . ?
N1 N2 Co2 122.6(3) . . ?
O7 V3 O9 108.92(19) . . ?
O7 V3 O8 108.0(2) . . ?
O9 V3 O8 109.55(18) . . ?
O7 V3 O6 109.54(18) . . ?
O9 V3 O6 110.10(17) . . ?
O8 V3 O6 110.68(16) . . ?
C2 N3 C1 106.1(4) . . ?
C2 N3 N4 130.3(4) . . ?
C1 N3 N4 123.6(4) . . ?
V1 O3 V2 156.6(3) . . ?
N5 C3 N7 109.8(4) . . ?
N6 C4 N7 109.9(4) . . ?
N9 C5 N11 110.1(4) . . ?
V2 O5 Co1 156.0(2) . 2_756 ?
C3 N5 N6 107.1(3) . . ?
C3 N5 Co1 122.2(3) . . ?
N6 N5 Co1 130.7(3) . . ?
V3 O6 V2 138.0(2) . . ?
C4 N6 N5 107.0(3) . . ?
C4 N6 Co2 132.3(3) . . ?
N5 N6 Co2 120.4(3) . . ?
N10 C6 N11 110.3(4) . . ?
C3 N7 C4 106.2(4) . . ?
C3 N7 N8 129.0(3) . . ?
C4 N7 N8 124.9(3) . . ?
V1 O8 V3 144.7(2) 2_646 . ?
V3 O9 Co1 158.9(2) . 1_545 ?
C5 N9 N10 107.1(3) . . ?
C5 N9 Co1 129.6(3) . . ?
N10 N9 Co1 123.1(3) . . ?
C6 N10 N9 106.6(3) . . ?
C6 N10 Co2 125.8(3) . . ?
N9 N10 Co2 127.5(3) . . ?
C6 N11 C5 106.0(3) . . ?
C6 N11 N12 124.5(3) . . ?
C5 N11 N12 129.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.135
_database_code_depnum_ccdc_archive 'CCDC 992975'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H32 N24 O22 V6 Zn3'
_chemical_formula_weight         1366.37

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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.8440(5)
_cell_length_b                   10.5676(5)
_cell_length_c                   11.5430(6)
_cell_angle_alpha                105.8870(10)
_cell_angle_beta                 91.7970(10)
_cell_angle_gamma                114.1830(10)
_cell_volume                     1039.38(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_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    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5367
_exptl_absorpt_correction_T_max  0.5769
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5278
_diffrn_reflns_av_R_equivalents  0.0101
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3643
_reflns_number_gt                3471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3643
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.1072
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
Zn1 Zn -0.21745(3) 0.40742(3) -0.31962(3) 0.01595(14) Uani 1 1 d . . .
V1 V -0.84181(5) 0.25564(5) -0.61893(4) 0.01806(15) Uani 1 1 d . . .
O1 O -0.1743(2) 0.5802(2) -0.39000(17) 0.0228(4) Uani 1 1 d . . .
N1 N -0.2450(3) 0.2501(3) -0.2272(2) 0.0223(5) Uani 1 1 d . . .
C1 C -0.3414(3) 0.1133(3) -0.2576(3) 0.0231(6) Uani 1 1 d . . .
H1A H -0.4079 0.0605 -0.3310 0.028 Uiso 1 1 calc R . .
O1W O -1.1017(4) 0.0337(4) -0.9072(2) 0.0598(8) Uani 1 1 d . . .
H1WA H -1.1719 -0.0528 -0.9296 0.072 Uiso 1 1 d R . .
H1WB H -1.1119 0.0778 -0.8368 0.072 Uiso 1 1 d R . .
Zn2 Zn 0.0000 0.5000 0.0000 0.01653(15) Uani 1 2 d S . .
V2 V -0.62127(5) 0.22235(5) -0.39954(4) 0.01740(15) Uani 1 1 d . . .
O2 O -0.1914(3) 0.2770(2) -0.4855(2) 0.0344(5) Uani 1 1 d . . .
N2 N -0.1665(3) 0.2868(3) -0.1120(2) 0.0235(5) Uani 1 1 d . . .
C2 C -0.2207(3) 0.1690(3) -0.0784(3) 0.0237(6) Uani 1 1 d . . .
H2A H -0.1881 0.1625 -0.0047 0.028 Uiso 1 1 calc R . .
O2W O -1.0007(6) 0.1429(6) -0.3085(5) 0.1268(18) Uani 1 1 d . . .
H2WA H -1.0578 0.1843 -0.2865 0.152 Uiso 1 1 d R . .
H2WB H -1.0401 0.0593 -0.2985 0.152 Uiso 1 1 d R . .
V3 V -0.78732(5) -0.12755(5) -0.40862(4) 0.01706(15) Uani 1 1 d . . .
N3 N -0.3300(3) 0.0596(3) -0.1659(2) 0.0206(5) Uani 1 1 d . . .
O3 O -0.7955(3) 0.1876(3) -0.7451(3) 0.0506(7) Uani 1 1 d . . .
C3 C 0.1141(3) 0.5130(3) -0.3487(2) 0.0194(6) Uani 1 1 d . . .
H3A H 0.0858 0.4924 -0.4318 0.023 Uiso 1 1 calc R . .
N4 N -0.4154(3) -0.0803(3) -0.1566(2) 0.0284(6) Uani 1 1 d . . .
H4B H -0.5036 -0.1012 -0.1763 0.034 Uiso 1 1 d R . .
H4C H -0.3927 -0.1514 -0.2140 0.034 Uiso 1 1 d R . .
C4 C 0.2485(3) 0.5800(3) -0.1730(2) 0.0214(6) Uani 1 1 d . . .
H4A H 0.3309 0.6151 -0.1120 0.026 Uiso 1 1 calc R . .
O4 O -0.7200(3) 0.2772(3) -0.4911(3) 0.0596(9) Uani 1 1 d . . .
C5 C -0.3462(3) 0.5866(3) -0.1380(2) 0.0232(6) Uani 1 1 d . . .
H5A H -0.4240 0.5655 -0.1985 0.028 Uiso 1 1 calc R . .
O5 O -0.4395(2) 0.3092(3) -0.4007(2) 0.0361(5) Uani 1 1 d . . .
N5 N 0.0216(3) 0.4940(3) -0.2691(2) 0.0196(5) Uani 1 1 d . . .
O6 O -0.6490(4) 0.2716(4) -0.2616(3) 0.0598(8) Uani 1 1 d . . .
N6 N 0.1072(3) 0.5357(3) -0.1568(2) 0.0202(5) Uani 1 1 d . . .
C6 C -0.1992(3) 0.6754(3) 0.0338(2) 0.0236(6) Uani 1 1 d . . .
H6A H -0.1550 0.7284 0.1147 0.028 Uiso 1 1 calc R . .
N7 N 0.2554(2) 0.5666(2) -0.2917(2) 0.0181(5) Uani 1 1 d . . .
O7 O -0.6799(3) 0.0292(2) -0.4541(2) 0.0334(5) Uani 1 1 d . . .
N8 N 0.3902(3) 0.6047(3) -0.3431(2) 0.0240(5) Uani 1 1 d . . .
H8A H 0.3956 0.6632 -0.3772 0.029 Uiso 1 1 d R . .
H8B H 0.3934 0.5312 -0.3898 0.029 Uiso 1 1 d R . .
O8 O -0.9679(3) -0.1353(3) -0.3824(3) 0.0438(7) Uani 1 1 d . . .
N9 N -0.2457(3) 0.5360(3) -0.1520(2) 0.0197(5) Uani 1 1 d . . .
O9 O -0.7002(3) -0.1179(3) -0.2823(2) 0.0455(6) Uani 1 1 d . . .
N10 N -0.1516(3) 0.5915(3) -0.0411(2) 0.0205(5) Uani 1 1 d . . .
N11 N -0.3204(3) 0.6744(3) -0.0223(2) 0.0214(5) Uani 1 1 d . . .
N12 N -0.4140(3) 0.7431(3) 0.0225(2) 0.0296(6) Uani 1 1 d . . .
H12A H -0.4230 0.7559 0.0898 0.036 Uiso 1 1 d R . .
H12B H -0.3858 0.8315 0.0112 0.036 Uiso 1 1 d 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
Zn1 O5 2.052(2) . ?
Zn1 O1 2.0913(19) . ?
Zn1 O2 2.123(2) . ?
Zn1 N9 2.138(2) . ?
Zn1 N5 2.138(2) . ?
Zn1 N1 2.144(2) . ?
V1 O3 1.608(2) . ?
V1 O1 1.6491(19) 2_464 ?
V1 O4 1.774(2) . ?
V1 O8 1.785(2) 2_354 ?
O1 V1 1.6492(19) 2_464 ?
N1 C1 1.301(4) . ?
N1 N2 1.387(3) . ?
C1 N3 1.352(4) . ?
Zn2 N2 2.163(2) . ?
Zn2 N2 2.163(2) 2_565 ?
Zn2 N6 2.167(2) 2_565 ?
Zn2 N6 2.167(2) . ?
Zn2 N10 2.185(2) 2_565 ?
Zn2 N10 2.185(2) . ?
V2 O6 1.604(3) . ?
V2 O5 1.645(2) . ?
V2 O4 1.769(2) . ?
V2 O7 1.790(2) . ?
O2 V3 1.640(2) 2_454 ?
N2 C2 1.311(4) . ?
C2 N3 1.337(4) . ?
V3 O9 1.625(2) . ?
V3 O2 1.640(2) 2_454 ?
V3 O8 1.785(2) . ?
V3 O7 1.793(2) . ?
N3 N4 1.407(3) . ?
C3 N5 1.310(4) . ?
C3 N7 1.334(4) . ?
C4 N6 1.311(4) . ?
C4 N7 1.345(4) . ?
C5 N9 1.299(4) . ?
C5 N11 1.348(4) . ?
N5 N6 1.379(3) . ?
C6 N10 1.304(4) . ?
C6 N11 1.334(4) . ?
N7 N8 1.421(3) . ?
O8 V1 1.785(2) 2_354 ?
N9 N10 1.382(3) . ?
N11 N12 1.420(3) . ?

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
O5 Zn1 O1 90.71(9) . . ?
O5 Zn1 O2 83.20(10) . . ?
O1 Zn1 O2 91.58(8) . . ?
O5 Zn1 N9 96.45(9) . . ?
O1 Zn1 N9 89.16(8) . . ?
O2 Zn1 N9 179.18(8) . . ?
O5 Zn1 N5 169.14(10) . . ?
O1 Zn1 N5 86.91(8) . . ?
O2 Zn1 N5 86.27(9) . . ?
N9 Zn1 N5 94.12(9) . . ?
O5 Zn1 N1 94.45(9) . . ?
O1 Zn1 N1 173.01(8) . . ?
O2 Zn1 N1 93.71(9) . . ?
N9 Zn1 N1 85.58(9) . . ?
N5 Zn1 N1 88.87(9) . . ?
O3 V1 O1 109.48(12) . 2_464 ?
O3 V1 O4 111.40(16) . . ?
O1 V1 O4 106.82(12) 2_464 . ?
O3 V1 O8 107.57(14) . 2_354 ?
O1 V1 O8 110.97(11) 2_464 2_354 ?
O4 V1 O8 110.62(15) . 2_354 ?
V1 O1 Zn1 152.81(12) 2_464 . ?
C1 N1 N2 107.4(2) . . ?
C1 N1 Zn1 129.44(19) . . ?
N2 N1 Zn1 122.81(17) . . ?
N1 C1 N3 109.4(2) . . ?
N2 Zn2 N2 180.0 . 2_565 ?
N2 Zn2 N6 89.43(9) . 2_565 ?
N2 Zn2 N6 90.57(9) 2_565 2_565 ?
N2 Zn2 N6 90.57(9) . . ?
N2 Zn2 N6 89.43(9) 2_565 . ?
N6 Zn2 N6 180.0 2_565 . ?
N2 Zn2 N10 91.43(9) . 2_565 ?
N2 Zn2 N10 88.57(9) 2_565 2_565 ?
N6 Zn2 N10 90.97(9) 2_565 2_565 ?
N6 Zn2 N10 89.03(9) . 2_565 ?
N2 Zn2 N10 88.57(9) . . ?
N2 Zn2 N10 91.43(9) 2_565 . ?
N6 Zn2 N10 89.03(9) 2_565 . ?
N6 Zn2 N10 90.97(9) . . ?
N10 Zn2 N10 180.0 2_565 . ?
O6 V2 O5 107.62(15) . . ?
O6 V2 O4 108.64(18) . . ?
O5 V2 O4 108.54(14) . . ?
O6 V2 O7 110.62(15) . . ?
O5 V2 O7 109.81(12) . . ?
O4 V2 O7 111.50(12) . . ?
V3 O2 Zn1 157.65(14) 2_454 . ?
C2 N2 N1 106.7(2) . . ?
C2 N2 Zn2 125.5(2) . . ?
N1 N2 Zn2 127.56(18) . . ?
N2 C2 N3 109.8(2) . . ?
O9 V3 O2 108.68(13) . 2_454 ?
O9 V3 O8 107.88(15) . . ?
O2 V3 O8 109.73(12) 2_454 . ?
O9 V3 O7 110.01(13) . . ?
O2 V3 O7 109.99(11) 2_454 . ?
O8 V3 O7 110.50(11) . . ?
C2 N3 C1 106.5(2) . . ?
C2 N3 N4 124.2(2) . . ?
C1 N3 N4 129.3(2) . . ?
N5 C3 N7 109.3(2) . . ?
N6 C4 N7 109.2(2) . . ?
V2 O4 V1 156.11(19) . . ?
N9 C5 N11 109.5(2) . . ?
V2 O5 Zn1 152.16(15) . . ?
C3 N5 N6 107.5(2) . . ?
C3 N5 Zn1 122.53(18) . . ?
N6 N5 Zn1 130.00(17) . . ?
C4 N6 N5 107.0(2) . . ?
C4 N6 Zn2 132.00(18) . . ?
N5 N6 Zn2 120.64(17) . . ?
N10 C6 N11 110.4(2) . . ?
C3 N7 C4 107.0(2) . . ?
C3 N7 N8 127.9(2) . . ?
C4 N7 N8 125.1(2) . . ?
V2 O7 V3 137.89(14) . . ?
V3 O8 V1 143.87(14) . 2_354 ?
C5 N9 N10 107.5(2) . . ?
C5 N9 Zn1 126.30(18) . . ?
N10 N9 Zn1 125.96(17) . . ?
C6 N10 N9 106.5(2) . . ?
C6 N10 Zn2 129.07(19) . . ?
N9 N10 Zn2 122.45(17) . . ?
C6 N11 C5 106.1(2) . . ?
C6 N11 N12 130.9(2) . . ?
C5 N11 N12 123.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.439
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.100



#===END

_database_code_depnum_ccdc_archive 'CCDC 992976'
