# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1003692'
_audit_update_record             
;
2014-11-22 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H46 N14 Ni2 O14 V4'
_chemical_formula_weight         1123.97

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'
O O 0.0106 0.0060 '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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.4022(8)
_cell_length_b                   13.4466(12)
_cell_length_c                   17.5161(15)
_cell_angle_alpha                89.367(2)
_cell_angle_beta                 87.3580(10)
_cell_angle_gamma                87.4490(10)
_cell_volume                     2209.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2863
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      26.758

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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            11303
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7665
_reflns_number_gt                4873
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0240P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7665
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 0.48168(6) 0.89456(4) 0.25308(4) 0.03191(17) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.5000 0.5000 0.0263(2) Uani 1 2 d S . .
Ni3 Ni 1.0000 0.5000 0.0000 0.0302(2) Uani 1 2 d S . .
V1 V 0.10930(8) 0.87841(6) 0.32105(5) 0.0315(2) Uani 1 1 d . . .
V2 V 0.11913(9) 0.62499(6) 0.32249(5) 0.0368(2) Uani 1 1 d . . .
V3 V 0.85805(8) 0.88278(6) 0.18476(5) 0.0303(2) Uani 1 1 d . . .
V4 V 0.88484(9) 0.63205(6) 0.17693(5) 0.0340(2) Uani 1 1 d . . .
N1 N 0.2949(4) 0.8632(3) 0.0423(3) 0.0406(11) Uani 1 1 d . . .
N2 N 0.4257(4) 0.8855(3) 0.1411(2) 0.0369(10) Uani 1 1 d . . .
N3 N 0.3968(5) 1.2039(3) 0.2695(3) 0.0565(13) Uani 1 1 d . . .
N4 N 0.4739(4) 1.0488(3) 0.2494(2) 0.0381(10) Uani 1 1 d . . .
N5 N 0.6680(4) 0.8806(3) 0.4665(2) 0.0400(11) Uani 1 1 d . . .
N6 N 0.5358(4) 0.8941(3) 0.3661(2) 0.0370(10) Uani 1 1 d . . .
N7 N -0.1244(4) 0.2288(3) 0.4058(2) 0.0390(10) Uani 1 1 d . . .
N8 N -0.0609(4) 0.3775(3) 0.4372(2) 0.0311(9) Uani 1 1 d . . .
N9 N -0.4254(4) 0.6120(3) 0.5123(3) 0.0401(11) Uani 1 1 d . . .
N10 N -0.2011(4) 0.5677(3) 0.4858(2) 0.0319(10) Uani 1 1 d . . .
N11 N 1.1188(4) 0.2121(3) 0.0874(2) 0.0412(11) Uani 1 1 d . . .
N12 N 1.0560(4) 0.3688(3) 0.0620(2) 0.0372(10) Uani 1 1 d . . .
N13 N 1.4132(4) 0.6104(3) -0.0114(3) 0.0480(12) Uani 1 1 d . . .
N14 N 1.1994(4) 0.5568(3) 0.0153(2) 0.0362(10) Uani 1 1 d . . .
O1 O 0.0872(4) 0.7532(3) 0.3477(2) 0.0663(12) Uani 1 1 d . . .
O2 O 0.2697(3) 0.8928(3) 0.28441(19) 0.0480(10) Uani 1 1 d . . .
O3 O 0.0881(4) 0.9449(3) 0.3978(2) 0.0736(13) Uani 1 1 d . . .
O4 O 0.9781(3) 0.9157(3) 0.2553(2) 0.0547(11) Uani 1 1 d . . .
O5 O 0.0057(4) 0.5964(3) 0.2482(2) 0.0659(12) Uani 1 1 d . . .
O6 O 0.0769(3) 0.5618(2) 0.39931(17) 0.0351(8) Uani 1 1 d . . .
O7 O 0.2849(4) 0.6011(3) 0.2975(3) 0.0824(14) Uani 1 1 d . . .
O8 O 0.9052(3) 0.7595(2) 0.15135(18) 0.0442(9) Uani 1 1 d . . .
O9 O 0.6939(3) 0.8870(2) 0.22089(18) 0.0387(8) Uani 1 1 d . . .
O10 O 0.8679(4) 0.9587(3) 0.1130(2) 0.0590(11) Uani 1 1 d . . .
O11 O 0.9209(3) 0.5648(2) 0.10066(17) 0.0373(8) Uani 1 1 d . . .
O12 O 0.7232(4) 0.6149(3) 0.2083(2) 0.0709(13) Uani 1 1 d . . .
O13 O 0.4922(3) 0.7378(2) 0.2586(2) 0.0541(10) Uani 1 1 d . . .
H13C H 0.4262 0.6988 0.2710 0.065 Uiso 1 1 d R . .
H13D H 0.5651 0.7030 0.2428 0.065 Uiso 1 1 d R . .
O14 O 0.5245(5) 0.4643(3) 0.2455(3) 0.0939(16) Uani 1 1 d . . .
H14C H 0.5895 0.5042 0.2332 0.113 Uiso 1 1 d R . .
H14D H 0.4509 0.4985 0.2614 0.113 Uiso 1 1 d R . .
C1 C 0.2977(6) 0.8652(4) 0.1185(3) 0.0422(13) Uani 1 1 d . . .
H1 H 0.2196 0.8538 0.1514 0.051 Uiso 1 1 calc R . .
C2 C 0.5062(6) 0.8969(4) 0.0763(3) 0.0520(16) Uani 1 1 d . . .
H2 H 0.6020 0.9118 0.0742 0.062 Uiso 1 1 calc R . .
C3 C 0.4277(6) 0.8837(4) 0.0147(3) 0.0530(16) Uani 1 1 d . . .
H3 H 0.4586 0.8879 -0.0364 0.064 Uiso 1 1 calc R . .
C4 C 0.1728(6) 0.8412(4) -0.0016(3) 0.0591(17) Uani 1 1 d . . .
H4A H 0.1849 0.7748 -0.0213 0.089 Uiso 1 1 calc R . .
H4B H 0.1653 0.8878 -0.0433 0.089 Uiso 1 1 calc R . .
H4C H 0.0877 0.8464 0.0307 0.089 Uiso 1 1 calc R . .
C5 C 0.3687(6) 1.1069(4) 0.2761(3) 0.0490(15) Uani 1 1 d . . .
H5 H 0.2837 1.0838 0.2973 0.059 Uiso 1 1 calc R . .
C6 C 0.5734(6) 1.1124(4) 0.2242(4) 0.0613(17) Uani 1 1 d . . .
H6 H 0.6607 1.0928 0.2006 0.074 Uiso 1 1 calc R . .
C7 C 0.5298(7) 1.2079(4) 0.2375(4) 0.0684(19) Uani 1 1 d . . .
H7 H 0.5807 1.2646 0.2269 0.082 Uiso 1 1 calc R . .
C8 C 0.3014(8) 1.2874(5) 0.2951(5) 0.107(3) Uani 1 1 d . . .
H8A H 0.2633 1.3211 0.2514 0.161 Uiso 1 1 calc R . .
H8B H 0.3537 1.3330 0.3235 0.161 Uiso 1 1 calc R . .
H8C H 0.2248 1.2628 0.3270 0.161 Uiso 1 1 calc R . .
C9 C 0.6677(5) 0.8881(4) 0.3900(3) 0.0409(13) Uani 1 1 d . . .
H9 H 0.7493 0.8889 0.3579 0.049 Uiso 1 1 calc R . .
C10 C 0.4497(6) 0.8891(4) 0.4308(3) 0.0460(14) Uani 1 1 d . . .
H10 H 0.3506 0.8910 0.4320 0.055 Uiso 1 1 calc R . .
C11 C 0.5307(5) 0.8811(4) 0.4932(3) 0.0446(14) Uani 1 1 d . . .
H11 H 0.4981 0.8768 0.5440 0.054 Uiso 1 1 calc R . .
C12 C 0.7951(5) 0.8667(4) 0.5108(3) 0.0561(17) Uani 1 1 d . . .
H12A H 0.8054 0.7983 0.5269 0.084 Uiso 1 1 calc R . .
H12B H 0.7861 0.9086 0.5549 0.084 Uiso 1 1 calc R . .
H12C H 0.8774 0.8839 0.4798 0.084 Uiso 1 1 calc R . .
C13 C -0.0858(5) 0.2882(4) 0.4607(3) 0.0339(12) Uani 1 1 d . . .
H13 H -0.0775 0.2674 0.5112 0.041 Uiso 1 1 calc R . .
C14 C -0.0868(6) 0.3772(4) 0.3603(3) 0.0468(15) Uani 1 1 d . . .
H14 H -0.0789 0.4314 0.3271 0.056 Uiso 1 1 calc R . .
C15 C -0.1252(6) 0.2861(4) 0.3410(3) 0.0492(15) Uani 1 1 d . . .
H15 H -0.1481 0.2659 0.2927 0.059 Uiso 1 1 calc R . .
C16 C -0.1588(6) 0.1238(4) 0.4115(3) 0.0567(16) Uani 1 1 d . . .
H16A H -0.1409 0.0992 0.4620 0.085 Uiso 1 1 calc R . .
H16B H -0.1006 0.0861 0.3747 0.085 Uiso 1 1 calc R . .
H16C H -0.2575 0.1172 0.4016 0.085 Uiso 1 1 calc R . .
C17 C -0.3058(5) 0.5680(3) 0.5371(3) 0.0354(12) Uani 1 1 d . . .
H17 H -0.2981 0.5406 0.5858 0.042 Uiso 1 1 calc R . .
C18 C -0.2582(5) 0.6131(4) 0.4223(3) 0.0423(14) Uani 1 1 d . . .
H18 H -0.2095 0.6238 0.3757 0.051 Uiso 1 1 calc R . .
C19 C -0.3966(5) 0.6395(4) 0.4390(3) 0.0458(14) Uani 1 1 d . . .
H19 H -0.4600 0.6706 0.4062 0.055 Uiso 1 1 calc R . .
C20 C -0.5605(5) 0.6270(4) 0.5556(3) 0.0554(16) Uani 1 1 d . . .
H20A H -0.5703 0.5747 0.5930 0.083 Uiso 1 1 calc R . .
H20B H -0.6374 0.6259 0.5215 0.083 Uiso 1 1 calc R . .
H20C H -0.5627 0.6901 0.5808 0.083 Uiso 1 1 calc R . .
C21 C 1.1094(5) 0.2849(4) 0.0347(3) 0.0342(12) Uani 1 1 d . . .
H21 H 1.1383 0.2762 -0.0164 0.041 Uiso 1 1 calc R . .
C22 C 1.0277(7) 0.3486(5) 0.1376(3) 0.084(2) Uani 1 1 d . . .
H22 H 0.9892 0.3942 0.1732 0.101 Uiso 1 1 calc R . .
C23 C 1.0640(8) 0.2526(5) 0.1529(3) 0.082(2) Uani 1 1 d . . .
H23 H 1.0533 0.2203 0.1999 0.098 Uiso 1 1 calc R . .
C24 C 1.1715(6) 0.1092(4) 0.0767(3) 0.0549(16) Uani 1 1 d . . .
H24A H 1.2572 0.0978 0.1038 0.082 Uiso 1 1 calc R . .
H24B H 1.1912 0.0973 0.0232 0.082 Uiso 1 1 calc R . .
H24C H 1.1006 0.0650 0.0960 0.082 Uiso 1 1 calc R . .
C25 C 1.2985(5) 0.5701(4) -0.0385(3) 0.0419(13) Uani 1 1 d . . .
H25 H 1.2901 0.5534 -0.0894 0.050 Uiso 1 1 calc R . .
C26 C 1.2561(5) 0.5895(4) 0.0805(3) 0.0466(14) Uani 1 1 d . . .
H26 H 1.2110 0.5890 0.1289 0.056 Uiso 1 1 calc R . .
C27 C 1.3880(6) 0.6226(4) 0.0640(4) 0.0532(16) Uani 1 1 d . . .
H27 H 1.4490 0.6487 0.0981 0.064 Uiso 1 1 calc R . .
C28 C 1.5413(6) 0.6355(4) -0.0568(4) 0.073(2) Uani 1 1 d . . .
H28A H 1.5491 0.5959 -0.1022 0.109 Uiso 1 1 calc R . .
H28B H 1.6237 0.6223 -0.0272 0.109 Uiso 1 1 calc R . .
H28C H 1.5353 0.7048 -0.0707 0.109 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 O2 2.043(3) . ?
Ni1 O9 2.046(3) . ?
Ni1 N2 2.060(4) . ?
Ni1 N6 2.067(4) . ?
Ni1 N4 2.073(4) . ?
Ni1 O13 2.107(3) . ?
Ni2 O6 2.056(3) 2_566 ?
Ni2 O6 2.056(3) . ?
Ni2 N10 2.086(4) 2_566 ?
Ni2 N10 2.086(4) . ?
Ni2 N8 2.105(4) 2_566 ?
Ni2 N8 2.105(4) . ?
Ni3 O11 2.068(3) . ?
Ni3 O11 2.068(3) 2_765 ?
Ni3 N14 2.085(4) . ?
Ni3 N14 2.085(4) 2_765 ?
Ni3 N12 2.120(4) . ?
Ni3 N12 2.120(4) 2_765 ?
V1 O3 1.623(4) . ?
V1 O2 1.631(3) . ?
V1 O1 1.760(3) . ?
V1 O4 1.778(3) 1_455 ?
V2 O7 1.618(4) . ?
V2 O6 1.626(3) . ?
V2 O5 1.776(4) . ?
V2 O1 1.794(4) . ?
V3 O10 1.612(3) . ?
V3 O9 1.640(3) . ?
V3 O4 1.784(3) . ?
V3 O8 1.795(3) . ?
V4 O12 1.618(4) . ?
V4 O11 1.636(3) . ?
V4 O5 1.775(3) 1_655 ?
V4 O8 1.782(3) . ?
N1 C1 1.336(6) . ?
N1 C3 1.357(6) . ?
N1 C4 1.454(6) . ?
N2 C1 1.325(6) . ?
N2 C2 1.346(6) . ?
N3 C5 1.345(6) . ?
N3 C7 1.350(7) . ?
N3 C8 1.466(7) . ?
N4 C5 1.305(6) . ?
N4 C6 1.351(6) . ?
N5 C9 1.343(6) . ?
N5 C11 1.352(6) . ?
N5 C12 1.459(5) . ?
N6 C9 1.326(6) . ?
N6 C10 1.364(6) . ?
N7 C13 1.330(6) . ?
N7 C15 1.365(6) . ?
N7 C16 1.464(6) . ?
N8 C13 1.293(5) . ?
N8 C14 1.381(6) . ?
N9 C17 1.336(5) . ?
N9 C19 1.350(6) . ?
N9 C20 1.456(6) . ?
N10 C17 1.302(5) . ?
N10 C18 1.382(5) . ?
N11 C21 1.339(5) . ?
N11 C23 1.346(7) . ?
N11 C24 1.460(6) . ?
N12 C21 1.301(6) . ?
N12 C22 1.366(6) . ?
N13 C25 1.337(6) . ?
N13 C27 1.341(7) . ?
N13 C28 1.463(6) . ?
N14 C25 1.311(6) . ?
N14 C26 1.368(6) . ?
O4 V1 1.778(3) 1_655 ?
O5 V4 1.775(3) 1_455 ?
O13 H13C 0.8500 . ?
O13 H13D 0.8500 . ?
O14 H14C 0.8500 . ?
O14 H14D 0.8500 . ?
C1 H1 0.9300 . ?
C2 C3 1.353(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5 0.9300 . ?
C6 C7 1.351(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9 0.9300 . ?
C10 C11 1.361(6) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9300 . ?
C14 C15 1.344(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17 0.9300 . ?
C18 C19 1.354(6) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21 0.9300 . ?
C22 C23 1.347(8) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9300 . ?
C26 C27 1.354(7) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O9 176.48(14) . . ?
O2 Ni1 N2 87.91(15) . . ?
O9 Ni1 N2 91.41(14) . . ?
O2 Ni1 N6 91.30(15) . . ?
O9 Ni1 N6 89.16(14) . . ?
N2 Ni1 N6 176.38(16) . . ?
O2 Ni1 N4 91.41(15) . . ?
O9 Ni1 N4 92.07(15) . . ?
N2 Ni1 N4 92.32(15) . . ?
N6 Ni1 N4 91.23(16) . . ?
O2 Ni1 O13 89.04(13) . . ?
O9 Ni1 O13 87.49(13) . . ?
N2 Ni1 O13 88.73(15) . . ?
N6 Ni1 O13 87.73(15) . . ?
N4 Ni1 O13 178.87(15) . . ?
O6 Ni2 O6 180.0 2_566 . ?
O6 Ni2 N10 91.13(13) 2_566 2_566 ?
O6 Ni2 N10 88.87(13) . 2_566 ?
O6 Ni2 N10 88.87(13) 2_566 . ?
O6 Ni2 N10 91.13(13) . . ?
N10 Ni2 N10 180.000(1) 2_566 . ?
O6 Ni2 N8 88.49(13) 2_566 2_566 ?
O6 Ni2 N8 91.51(13) . 2_566 ?
N10 Ni2 N8 89.10(15) 2_566 2_566 ?
N10 Ni2 N8 90.90(15) . 2_566 ?
O6 Ni2 N8 91.51(13) 2_566 . ?
O6 Ni2 N8 88.49(13) . . ?
N10 Ni2 N8 90.90(15) 2_566 . ?
N10 Ni2 N8 89.10(15) . . ?
N8 Ni2 N8 180.00(12) 2_566 . ?
O11 Ni3 O11 180.00(9) . 2_765 ?
O11 Ni3 N14 90.64(14) . . ?
O11 Ni3 N14 89.36(14) 2_765 . ?
O11 Ni3 N14 89.36(14) . 2_765 ?
O11 Ni3 N14 90.64(14) 2_765 2_765 ?
N14 Ni3 N14 180.0(2) . 2_765 ?
O11 Ni3 N12 89.40(14) . . ?
O11 Ni3 N12 90.60(14) 2_765 . ?
N14 Ni3 N12 91.24(15) . . ?
N14 Ni3 N12 88.76(15) 2_765 . ?
O11 Ni3 N12 90.60(14) . 2_765 ?
O11 Ni3 N12 89.40(14) 2_765 2_765 ?
N14 Ni3 N12 88.76(15) . 2_765 ?
N14 Ni3 N12 91.24(15) 2_765 2_765 ?
N12 Ni3 N12 180.00(18) . 2_765 ?
O3 V1 O2 108.42(19) . . ?
O3 V1 O1 107.6(2) . . ?
O2 V1 O1 110.46(19) . . ?
O3 V1 O4 109.82(19) . 1_455 ?
O2 V1 O4 111.26(17) . 1_455 ?
O1 V1 O4 109.19(17) . 1_455 ?
O7 V2 O6 109.63(19) . . ?
O7 V2 O5 111.3(2) . . ?
O6 V2 O5 110.02(17) . . ?
O7 V2 O1 111.5(2) . . ?
O6 V2 O1 105.40(17) . . ?
O5 V2 O1 108.78(17) . . ?
O10 V3 O9 108.80(17) . . ?
O10 V3 O4 110.25(18) . . ?
O9 V3 O4 110.27(17) . . ?
O10 V3 O8 108.43(18) . . ?
O9 V3 O8 109.68(16) . . ?
O4 V3 O8 109.38(15) . . ?
O12 V4 O11 109.50(19) . . ?
O12 V4 O5 109.8(2) . 1_655 ?
O11 V4 O5 109.27(17) . 1_655 ?
O12 V4 O8 110.36(18) . . ?
O11 V4 O8 108.12(15) . . ?
O5 V4 O8 109.75(16) 1_655 . ?
C1 N1 C3 106.7(4) . . ?
C1 N1 C4 126.0(5) . . ?
C3 N1 C4 127.2(5) . . ?
C1 N2 C2 105.2(4) . . ?
C1 N2 Ni1 125.4(4) . . ?
C2 N2 Ni1 129.4(3) . . ?
C5 N3 C7 106.6(5) . . ?
C5 N3 C8 125.8(6) . . ?
C7 N3 C8 127.6(5) . . ?
C5 N4 C6 104.1(5) . . ?
C5 N4 Ni1 125.7(4) . . ?
C6 N4 Ni1 130.1(4) . . ?
C9 N5 C11 107.6(4) . . ?
C9 N5 C12 125.1(4) . . ?
C11 N5 C12 127.2(5) . . ?
C9 N6 C10 105.4(4) . . ?
C9 N6 Ni1 125.1(4) . . ?
C10 N6 Ni1 129.2(3) . . ?
C13 N7 C15 105.6(4) . . ?
C13 N7 C16 128.4(4) . . ?
C15 N7 C16 126.0(5) . . ?
C13 N8 C14 104.7(4) . . ?
C13 N8 Ni2 129.1(3) . . ?
C14 N8 Ni2 126.2(3) . . ?
C17 N9 C19 106.5(4) . . ?
C17 N9 C20 126.8(5) . . ?
C19 N9 C20 126.8(4) . . ?
C17 N10 C18 104.9(4) . . ?
C17 N10 Ni2 124.6(3) . . ?
C18 N10 Ni2 130.3(3) . . ?
C21 N11 C23 105.5(5) . . ?
C21 N11 C24 128.1(5) . . ?
C23 N11 C24 126.4(5) . . ?
C21 N12 C22 104.0(4) . . ?
C21 N12 Ni3 127.5(3) . . ?
C22 N12 Ni3 128.0(4) . . ?
C25 N13 C27 107.3(5) . . ?
C25 N13 C28 125.4(5) . . ?
C27 N13 C28 127.3(5) . . ?
C25 N14 C26 104.7(4) . . ?
C25 N14 Ni3 125.9(4) . . ?
C26 N14 Ni3 129.4(4) . . ?
V1 O1 V2 146.6(3) . . ?
V1 O2 Ni1 170.1(2) . . ?
V1 O4 V3 149.1(2) 1_655 . ?
V4 O5 V2 151.7(2) 1_455 . ?
V2 O6 Ni2 170.9(2) . . ?
V4 O8 V3 141.2(2) . . ?
V3 O9 Ni1 173.3(2) . . ?
V4 O11 Ni3 168.1(2) . . ?
Ni1 O13 H13C 128.5 . . ?
Ni1 O13 H13D 122.8 . . ?
H13C O13 H13D 108.3 . . ?
H14C O14 H14D 108.2 . . ?
N2 C1 N1 111.5(5) . . ?
N2 C1 H1 124.2 . . ?
N1 C1 H1 124.2 . . ?
N2 C2 C3 110.2(5) . . ?
N2 C2 H2 124.9 . . ?
C3 C2 H2 124.9 . . ?
C2 C3 N1 106.3(5) . . ?
C2 C3 H3 126.8 . . ?
N1 C3 H3 126.8 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 N3 112.5(5) . . ?
N4 C5 H5 123.8 . . ?
N3 C5 H5 123.8 . . ?
C7 C6 N4 111.3(6) . . ?
C7 C6 H6 124.4 . . ?
N4 C6 H6 124.4 . . ?
N3 C7 C6 105.5(5) . . ?
N3 C7 H7 127.3 . . ?
C6 C7 H7 127.3 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 N5 111.1(5) . . ?
N6 C9 H9 124.5 . . ?
N5 C9 H9 124.5 . . ?
C11 C10 N6 109.8(5) . . ?
C11 C10 H10 125.1 . . ?
N6 C10 H10 125.1 . . ?
N5 C11 C10 106.3(5) . . ?
N5 C11 H11 126.9 . . ?
C10 C11 H11 126.9 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N8 C13 N7 113.6(4) . . ?
N8 C13 H13 123.2 . . ?
N7 C13 H13 123.2 . . ?
C15 C14 N8 109.0(5) . . ?
C15 C14 H14 125.5 . . ?
N8 C14 H14 125.5 . . ?
C14 C15 N7 107.1(5) . . ?
C14 C15 H15 126.4 . . ?
N7 C15 H15 126.4 . . ?
N7 C16 H16A 109.5 . . ?
N7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N10 C17 N9 112.7(4) . . ?
N10 C17 H17 123.6 . . ?
N9 C17 H17 123.6 . . ?
C19 C18 N10 108.8(5) . . ?
C19 C18 H18 125.6 . . ?
N10 C18 H18 125.6 . . ?
N9 C19 C18 107.2(4) . . ?
N9 C19 H19 126.4 . . ?
C18 C19 H19 126.4 . . ?
N9 C20 H20A 109.5 . . ?
N9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N12 C21 N11 113.5(5) . . ?
N12 C21 H21 123.3 . . ?
N11 C21 H21 123.3 . . ?
C23 C22 N12 109.8(5) . . ?
C23 C22 H22 125.1 . . ?
N12 C22 H22 125.1 . . ?
N11 C23 C22 107.2(5) . . ?
N11 C23 H23 126.4 . . ?
C22 C23 H23 126.4 . . ?
N11 C24 H24A 109.5 . . ?
N11 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N11 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N14 C25 N13 111.9(5) . . ?
N14 C25 H25 124.0 . . ?
N13 C25 H25 124.0 . . ?
C27 C26 N14 109.7(5) . . ?
C27 C26 H26 125.2 . . ?
N14 C26 H26 125.2 . . ?
N13 C27 C26 106.5(5) . . ?
N13 C27 H27 126.8 . . ?
C26 C27 H27 126.8 . . ?
N13 C28 H28A 109.5 . . ?
N13 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N13 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

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
O2 Ni1 N2 C1 -11.7(4) . . . . ?
O9 Ni1 N2 C1 164.9(4) . . . . ?
N6 Ni1 N2 C1 66(3) . . . . ?
N4 Ni1 N2 C1 -103.0(4) . . . . ?
O13 Ni1 N2 C1 77.4(4) . . . . ?
O2 Ni1 N2 C2 169.2(5) . . . . ?
O9 Ni1 N2 C2 -14.2(5) . . . . ?
N6 Ni1 N2 C2 -113(3) . . . . ?
N4 Ni1 N2 C2 77.9(5) . . . . ?
O13 Ni1 N2 C2 -101.7(5) . . . . ?
O2 Ni1 N4 C5 12.0(4) . . . . ?
O9 Ni1 N4 C5 -168.5(4) . . . . ?
N2 Ni1 N4 C5 100.0(4) . . . . ?
N6 Ni1 N4 C5 -79.3(4) . . . . ?
O13 Ni1 N4 C5 -101(8) . . . . ?
O2 Ni1 N4 C6 -171.8(5) . . . . ?
O9 Ni1 N4 C6 7.6(5) . . . . ?
N2 Ni1 N4 C6 -83.9(5) . . . . ?
N6 Ni1 N4 C6 96.8(5) . . . . ?
O13 Ni1 N4 C6 75(9) . . . . ?
O2 Ni1 N6 C9 175.2(4) . . . . ?
O9 Ni1 N6 C9 -1.4(4) . . . . ?
N2 Ni1 N6 C9 98(3) . . . . ?
N4 Ni1 N6 C9 -93.4(4) . . . . ?
O13 Ni1 N6 C9 86.2(4) . . . . ?
O2 Ni1 N6 C10 2.8(4) . . . . ?
O9 Ni1 N6 C10 -173.7(4) . . . . ?
N2 Ni1 N6 C10 -75(3) . . . . ?
N4 Ni1 N6 C10 94.3(4) . . . . ?
O13 Ni1 N6 C10 -86.1(4) . . . . ?
O6 Ni2 N8 C13 -21.1(4) 2_566 . . . ?
O6 Ni2 N8 C13 158.9(4) . . . . ?
N10 Ni2 N8 C13 70.0(4) 2_566 . . . ?
N10 Ni2 N8 C13 -110.0(4) . . . . ?
N8 Ni2 N8 C13 174(100) 2_566 . . . ?
O6 Ni2 N8 C14 157.0(4) 2_566 . . . ?
O6 Ni2 N8 C14 -23.0(4) . . . . ?
N10 Ni2 N8 C14 -111.8(4) 2_566 . . . ?
N10 Ni2 N8 C14 68.2(4) . . . . ?
N8 Ni2 N8 C14 -8(100) 2_566 . . . ?
O6 Ni2 N10 C17 8.0(4) 2_566 . . . ?
O6 Ni2 N10 C17 -172.0(4) . . . . ?
N10 Ni2 N10 C17 54(100) 2_566 . . . ?
N8 Ni2 N10 C17 -80.4(4) 2_566 . . . ?
N8 Ni2 N10 C17 99.6(4) . . . . ?
O6 Ni2 N10 C18 -166.1(4) 2_566 . . . ?
O6 Ni2 N10 C18 13.9(4) . . . . ?
N10 Ni2 N10 C18 -120(100) 2_566 . . . ?
N8 Ni2 N10 C18 105.4(4) 2_566 . . . ?
N8 Ni2 N10 C18 -74.6(4) . . . . ?
O11 Ni3 N12 C21 175.8(4) . . . . ?
O11 Ni3 N12 C21 -4.2(4) 2_765 . . . ?
N14 Ni3 N12 C21 -93.5(4) . . . . ?
N14 Ni3 N12 C21 86.5(4) 2_765 . . . ?
N12 Ni3 N12 C21 87(100) 2_765 . . . ?
O11 Ni3 N12 C22 5.1(5) . . . . ?
O11 Ni3 N12 C22 -174.9(5) 2_765 . . . ?
N14 Ni3 N12 C22 95.7(5) . . . . ?
N14 Ni3 N12 C22 -84.3(5) 2_765 . . . ?
N12 Ni3 N12 C22 -84(100) 2_765 . . . ?
O11 Ni3 N14 C25 -158.8(4) . . . . ?
O11 Ni3 N14 C25 21.2(4) 2_765 . . . ?
N14 Ni3 N14 C25 -80(100) 2_765 . . . ?
N12 Ni3 N14 C25 111.8(4) . . . . ?
N12 Ni3 N14 C25 -68.2(4) 2_765 . . . ?
O11 Ni3 N14 C26 20.2(4) . . . . ?
O11 Ni3 N14 C26 -159.8(4) 2_765 . . . ?
N14 Ni3 N14 C26 99(100) 2_765 . . . ?
N12 Ni3 N14 C26 -69.2(4) . . . . ?
N12 Ni3 N14 C26 110.8(4) 2_765 . . . ?
O3 V1 O1 V2 -160.5(4) . . . . ?
O2 V1 O1 V2 -42.3(5) . . . . ?
O4 V1 O1 V2 80.3(4) 1_455 . . . ?
O7 V2 O1 V1 50.4(5) . . . . ?
O6 V2 O1 V1 169.3(4) . . . . ?
O5 V2 O1 V1 -72.7(4) . . . . ?
O3 V1 O2 Ni1 77.0(14) . . . . ?
O1 V1 O2 Ni1 -40.7(14) . . . . ?
O4 V1 O2 Ni1 -162.1(13) 1_455 . . . ?
O9 Ni1 O2 V1 59(3) . . . . ?
N2 Ni1 O2 V1 137.7(14) . . . . ?
N6 Ni1 O2 V1 -38.8(14) . . . . ?
N4 Ni1 O2 V1 -130.0(14) . . . . ?
O13 Ni1 O2 V1 48.9(14) . . . . ?
O10 V3 O4 V1 -135.5(4) . . . 1_655 ?
O9 V3 O4 V1 104.4(5) . . . 1_655 ?
O8 V3 O4 V1 -16.3(5) . . . 1_655 ?
O7 V2 O5 V4 -111.9(5) . . . 1_455 ?
O6 V2 O5 V4 126.3(5) . . . 1_455 ?
O1 V2 O5 V4 11.3(6) . . . 1_455 ?
O7 V2 O6 Ni2 151.9(12) . . . . ?
O5 V2 O6 Ni2 -85.4(12) . . . . ?
O1 V2 O6 Ni2 31.8(12) . . . . ?
O6 Ni2 O6 V2 3(100) 2_566 . . . ?
N10 Ni2 O6 V2 -150.6(12) 2_566 . . . ?
N10 Ni2 O6 V2 29.4(12) . . . . ?
N8 Ni2 O6 V2 -61.6(12) 2_566 . . . ?
N8 Ni2 O6 V2 118.4(12) . . . . ?
O12 V4 O8 V3 43.0(4) . . . . ?
O11 V4 O8 V3 162.8(3) . . . . ?
O5 V4 O8 V3 -78.1(3) 1_655 . . . ?
O10 V3 O8 V4 -159.0(3) . . . . ?
O9 V3 O8 V4 -40.3(4) . . . . ?
O4 V3 O8 V4 80.7(3) . . . . ?
O10 V3 O9 Ni1 35.5(17) . . . . ?
O4 V3 O9 Ni1 156.6(17) . . . . ?
O8 V3 O9 Ni1 -82.9(17) . . . . ?
O2 Ni1 O9 V3 89(3) . . . . ?
N2 Ni1 O9 V3 10.5(17) . . . . ?
N6 Ni1 O9 V3 -173.1(17) . . . . ?
N4 Ni1 O9 V3 -81.9(17) . . . . ?
O13 Ni1 O9 V3 99.2(17) . . . . ?
O12 V4 O11 Ni3 160.6(9) . . . . ?
O5 V4 O11 Ni3 -79.1(9) 1_655 . . . ?
O8 V4 O11 Ni3 40.3(9) . . . . ?
O11 Ni3 O11 V4 -128(100) 2_765 . . . ?
N14 Ni3 O11 V4 24.5(9) . . . . ?
N14 Ni3 O11 V4 -155.5(9) 2_765 . . . ?
N12 Ni3 O11 V4 115.7(9) . . . . ?
N12 Ni3 O11 V4 -64.3(9) 2_765 . . . ?
C2 N2 C1 N1 0.2(6) . . . . ?
Ni1 N2 C1 N1 -179.1(3) . . . . ?
C3 N1 C1 N2 -0.3(6) . . . . ?
C4 N1 C1 N2 178.7(4) . . . . ?
C1 N2 C2 C3 0.0(6) . . . . ?
Ni1 N2 C2 C3 179.3(3) . . . . ?
N2 C2 C3 N1 -0.2(6) . . . . ?
C1 N1 C3 C2 0.3(6) . . . . ?
C4 N1 C3 C2 -178.6(5) . . . . ?
C6 N4 C5 N3 -0.5(6) . . . . ?
Ni1 N4 C5 N3 176.5(3) . . . . ?
C7 N3 C5 N4 -0.9(7) . . . . ?
C8 N3 C5 N4 -179.1(5) . . . . ?
C5 N4 C6 C7 1.7(7) . . . . ?
Ni1 N4 C6 C7 -175.0(4) . . . . ?
C5 N3 C7 C6 1.9(7) . . . . ?
C8 N3 C7 C6 180.0(6) . . . . ?
N4 C6 C7 N3 -2.3(7) . . . . ?
C10 N6 C9 N5 -0.6(6) . . . . ?
Ni1 N6 C9 N5 -174.5(3) . . . . ?
C11 N5 C9 N6 0.4(6) . . . . ?
C12 N5 C9 N6 176.1(4) . . . . ?
C9 N6 C10 C11 0.6(6) . . . . ?
Ni1 N6 C10 C11 174.1(3) . . . . ?
C9 N5 C11 C10 0.0(6) . . . . ?
C12 N5 C11 C10 -175.6(5) . . . . ?
N6 C10 C11 N5 -0.4(6) . . . . ?
C14 N8 C13 N7 0.7(5) . . . . ?
Ni2 N8 C13 N7 179.1(3) . . . . ?
C15 N7 C13 N8 -0.5(6) . . . . ?
C16 N7 C13 N8 179.3(4) . . . . ?
C13 N8 C14 C15 -0.6(6) . . . . ?
Ni2 N8 C14 C15 -179.1(4) . . . . ?
N8 C14 C15 N7 0.3(6) . . . . ?
C13 N7 C15 C14 0.1(6) . . . . ?
C16 N7 C15 C14 -179.7(5) . . . . ?
C18 N10 C17 N9 -1.3(6) . . . . ?
Ni2 N10 C17 N9 -176.7(3) . . . . ?
C19 N9 C17 N10 1.8(6) . . . . ?
C20 N9 C17 N10 -178.5(5) . . . . ?
C17 N10 C18 C19 0.4(6) . . . . ?
Ni2 N10 C18 C19 175.4(3) . . . . ?
C17 N9 C19 C18 -1.4(6) . . . . ?
C20 N9 C19 C18 178.8(5) . . . . ?
N10 C18 C19 N9 0.7(6) . . . . ?
C22 N12 C21 N11 -0.5(6) . . . . ?
Ni3 N12 C21 N11 -173.0(3) . . . . ?
C23 N11 C21 N12 1.4(6) . . . . ?
C24 N11 C21 N12 179.2(4) . . . . ?
C21 N12 C22 C23 -0.6(7) . . . . ?
Ni3 N12 C22 C23 171.8(4) . . . . ?
C21 N11 C23 C22 -1.7(7) . . . . ?
C24 N11 C23 C22 -179.5(5) . . . . ?
N12 C22 C23 N11 1.5(8) . . . . ?
C26 N14 C25 N13 -0.9(5) . . . . ?
Ni3 N14 C25 N13 178.2(3) . . . . ?
C27 N13 C25 N14 0.9(6) . . . . ?
C28 N13 C25 N14 -179.3(5) . . . . ?
C25 N14 C26 C27 0.6(6) . . . . ?
Ni3 N14 C26 C27 -178.5(3) . . . . ?
C25 N13 C27 C26 -0.4(6) . . . . ?
C28 N13 C27 C26 179.7(5) . . . . ?
N14 C26 C27 N13 -0.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_compound1
_audit_block_doi                 10.5517/cc12pf6d
_database_code_depnum_ccdc_archive 'CCDC 1003693'
_audit_update_record             
;
2014-11-22 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H34 Co2 N10 O14 V4'
_chemical_formula_weight         960.19

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   11.4770(11)
_cell_length_b                   17.8350(16)
_cell_length_c                   17.8350(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3650.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6637
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17748
_diffrn_reflns_av_R_equivalents  0.1323
_diffrn_reflns_av_sigmaI/netI    0.1674
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         25.02
_reflns_number_total             6412
_reflns_number_gt                3332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0955P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_number_reflns         6412
_refine_ls_number_parameters     456
_refine_ls_number_restraints     810
_refine_ls_R_factor_all          0.1628
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2213
_refine_ls_wR_factor_gt          0.1929
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.016
_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 0.85626(15) 0.19172(11) 0.76053(10) 0.0328(5) Uani 1 1 d . . .
Co2 Co 0.95238(16) 0.01529(10) 0.47098(11) 0.0366(5) Uani 1 1 d . . .
V1 V 0.88751(18) 0.20517(12) 0.54896(13) 0.0300(6) Uani 1 1 d . . .
V2 V 0.60714(17) 0.19237(13) 0.52980(14) 0.0343(6) Uani 1 1 d . . .
V3 V 0.96756(18) -0.19317(13) 0.44472(12) 0.0298(5) Uani 1 1 d . . .
V4 V 0.81258(17) 0.20427(12) 0.96861(13) 0.0294(5) Uani 1 1 d . . .
O1 O 0.7500(9) 0.2292(5) 0.5056(5) 0.043(2) Uani 1 1 d U . .
O2 O 0.9388(8) 0.1245(5) 0.5127(5) 0.0450(17) Uani 1 1 d U . .
O3 O 0.8673(7) 0.1958(5) 0.6400(5) 0.0375(15) Uani 1 1 d U . .
O4 O 0.9947(8) 0.2778(5) 0.5351(6) 0.044(2) Uani 1 1 d U . .
O5 O 0.5739(9) 0.2175(6) 0.6129(5) 0.053(3) Uani 1 1 d U . .
O6 O 0.6131(8) 0.0995(5) 0.5271(6) 0.046(2) Uani 1 1 d U . .
O7 O 0.8382(8) -0.2358(5) 0.4802(5) 0.043(2) Uani 1 1 d U . .
O8 O 0.9558(8) -0.1005(5) 0.4505(5) 0.0429(17) Uani 1 1 d U . .
O9 O 0.9877(8) -0.2171(6) 0.3578(5) 0.056(3) Uani 1 1 d U . .
O10 O 1.0902(8) -0.2206(5) 0.4999(5) 0.037(2) Uani 1 1 d U . .
O11 O 0.8375(8) 0.1867(5) 0.8788(5) 0.0434(18) Uani 1 1 d U . .
O12 O 0.8321(8) 0.1288(5) 1.0189(6) 0.047(3) Uani 1 1 d U . .
O13 O 0.6731(7) 0.1782(5) 0.7493(5) 0.043(2) Uani 1 1 d U . .
H13C H 0.6439 0.1900 0.7072 0.065 Uiso 1 1 d R . .
H13D H 0.6246 0.1898 0.7834 0.065 Uiso 1 1 d R . .
O14 O 0.7916(8) 0.0007(5) 0.5085(5) 0.048(2) Uani 1 1 d U . .
H14C H 0.7400 0.0345 0.5139 0.072 Uiso 1 1 d R . .
H14D H 0.7584 -0.0418 0.5112 0.072 Uiso 1 1 d R . .
N1 N 1.2299(10) 0.1982(7) 0.7404(7) 0.048(2) Uani 1 1 d U . .
N2 N 1.0370(10) 0.2013(7) 0.7688(7) 0.0464(17) Uani 1 1 d U . .
N3 N 0.8668(11) -0.0475(7) 0.7885(8) 0.050(2) Uani 1 1 d U . .
N4 N 0.8704(10) 0.0733(7) 0.7585(7) 0.0451(18) Uani 1 1 d U . .
N5 N 0.8000(11) 0.4311(7) 0.7332(8) 0.051(2) Uani 1 1 d U . .
N6 N 0.8323(10) 0.3109(8) 0.7653(7) 0.0485(19) Uani 1 1 d U . .
N7 N 1.3100(11) -0.0229(7) 0.5031(7) 0.049(2) Uani 1 1 d U . .
N8 N 1.1252(10) 0.0137(6) 0.5003(7) 0.0458(19) Uani 1 1 d U . .
N9 N 0.9458(11) 0.0341(6) 0.2404(7) 0.045(2) Uani 1 1 d U . .
N10 N 0.9539(11) 0.0434(6) 0.3631(7) 0.0458(19) Uani 1 1 d U . .
C1 C 1.1202(12) 0.1889(8) 0.7189(9) 0.045(2) Uani 1 1 d U . .
H1 H 1.1023 0.1742 0.6702 0.054 Uiso 1 1 calc R . .
C2 C 1.1089(13) 0.2212(8) 0.8286(9) 0.051(2) Uani 1 1 d U . .
H2 H 1.0794 0.2344 0.8753 0.061 Uiso 1 1 calc R . .
C3 C 1.2225(13) 0.2200(8) 0.8141(9) 0.051(3) Uani 1 1 d U . .
H3 H 1.2834 0.2313 0.8466 0.061 Uiso 1 1 calc R . .
C4 C 1.3353(13) 0.1866(10) 0.6948(9) 0.064(4) Uani 1 1 d U . .
H4A H 1.4011 0.2086 0.7197 0.096 Uiso 1 1 calc R . .
H4B H 1.3252 0.2098 0.6467 0.096 Uiso 1 1 calc R . .
H4C H 1.3484 0.1338 0.6883 0.096 Uiso 1 1 calc R . .
C5 C 0.8662(13) 0.0246(9) 0.8125(9) 0.050(2) Uani 1 1 d U . .
H5 H 0.8631 0.0379 0.8628 0.060 Uiso 1 1 calc R . .
C6 C 0.8773(14) 0.0283(9) 0.6956(10) 0.053(2) Uani 1 1 d U . .
H6 H 0.8817 0.0462 0.6467 0.063 Uiso 1 1 calc R . .
C7 C 0.8767(15) -0.0447(9) 0.7143(10) 0.057(3) Uani 1 1 d U . .
H7 H 0.8822 -0.0853 0.6817 0.069 Uiso 1 1 calc R . .
C8 C 0.8658(17) -0.1163(9) 0.8335(10) 0.074(4) Uani 1 1 d U . .
H8A H 0.9197 -0.1518 0.8126 0.111 Uiso 1 1 calc R . .
H8B H 0.7889 -0.1374 0.8333 0.111 Uiso 1 1 calc R . .
H8C H 0.8883 -0.1048 0.8841 0.111 Uiso 1 1 calc R . .
C9 C 0.8093(13) 0.3576(8) 0.7096(10) 0.051(2) Uani 1 1 d U . .
H9 H 0.8005 0.3426 0.6600 0.061 Uiso 1 1 calc R . .
C10 C 0.8380(15) 0.3582(9) 0.8257(10) 0.056(2) Uani 1 1 d U . .
H10 H 0.8554 0.3429 0.8743 0.068 Uiso 1 1 calc R . .
C11 C 0.8146(15) 0.4310(10) 0.8057(10) 0.060(3) Uani 1 1 d U . .
H11 H 0.8102 0.4722 0.8376 0.073 Uiso 1 1 calc R . .
C12 C 0.7782(17) 0.4974(9) 0.6874(10) 0.072(4) Uani 1 1 d U . .
H12A H 0.7204 0.5281 0.7113 0.108 Uiso 1 1 calc R . .
H12B H 0.7506 0.4822 0.6389 0.108 Uiso 1 1 calc R . .
H12C H 0.8491 0.5254 0.6819 0.108 Uiso 1 1 calc R . .
C13 C 1.1975(13) -0.0450(8) 0.4983(8) 0.045(2) Uani 1 1 d U . .
H13 H 1.1735 -0.0947 0.4942 0.054 Uiso 1 1 calc R . .
C14 C 1.1961(13) 0.0749(8) 0.5094(9) 0.047(2) Uani 1 1 d U . .
H14 H 1.1690 0.1237 0.5146 0.057 Uiso 1 1 calc R . .
C15 C 1.3132(14) 0.0553(8) 0.5100(9) 0.051(3) Uani 1 1 d U . .
H15 H 1.3779 0.0864 0.5140 0.061 Uiso 1 1 calc R . .
C16 C 1.4122(13) -0.0726(9) 0.4994(10) 0.062(4) Uani 1 1 d U . .
H16A H 1.3877 -0.1222 0.4856 0.093 Uiso 1 1 calc R . .
H16B H 1.4495 -0.0742 0.5476 0.093 Uiso 1 1 calc R . .
H16C H 1.4660 -0.0538 0.4627 0.093 Uiso 1 1 calc R . .
C17 C 0.9336(12) -0.0020(8) 0.3048(9) 0.045(2) Uani 1 1 d U . .
H17 H 0.9135 -0.0523 0.3090 0.054 Uiso 1 1 calc R . .
C18 C 0.9820(13) 0.1153(8) 0.3297(9) 0.049(2) Uani 1 1 d U . .
H18 H 0.9997 0.1586 0.3565 0.059 Uiso 1 1 calc R . .
C19 C 0.9788(14) 0.1103(8) 0.2520(9) 0.050(3) Uani 1 1 d U . .
H19 H 0.9942 0.1472 0.2166 0.060 Uiso 1 1 calc R . .
C20 C 0.9344(15) 0.0015(10) 0.1635(9) 0.067(4) Uani 1 1 d U . .
H20A H 1.0097 -0.0139 0.1458 0.101 Uiso 1 1 calc R . .
H20B H 0.9028 0.0385 0.1301 0.101 Uiso 1 1 calc R . .
H20C H 0.8833 -0.0411 0.1651 0.101 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
Co1 N2 2.086(12) . ?
Co1 N4 2.118(12) . ?
Co1 O11 2.122(10) . ?
Co1 O13 2.126(9) . ?
Co1 N6 2.145(13) . ?
Co1 O3 2.155(9) . ?
Co2 O14 1.980(9) . ?
Co2 N10 1.988(13) . ?
Co2 N8 2.051(12) . ?
Co2 O2 2.091(9) . ?
Co2 O8 2.098(9) . ?
V1 O3 1.649(9) . ?
V1 O2 1.684(9) . ?
V1 O4 1.803(9) . ?
V1 O1 1.809(10) . ?
V2 O5 1.594(10) . ?
V2 O6 1.659(9) . ?
V2 O4 1.814(9) 3_456 ?
V2 O1 1.818(10) . ?
V3 O9 1.625(10) . ?
V3 O8 1.661(9) . ?
V3 O7 1.784(9) . ?
V3 O10 1.785(9) . ?
V4 O12 1.633(9) . ?
V4 O11 1.657(10) . ?
V4 O7 1.831(9) 2_655 ?
V4 O10 1.832(9) 4_756 ?
O4 V2 1.814(9) 3_556 ?
O7 V4 1.831(9) 2_654 ?
O10 V4 1.832(9) 4_746 ?
O13 H13C 0.8501 . ?
O13 H13D 0.8499 . ?
O14 H14C 0.8500 . ?
O14 H14D 0.8499 . ?
N1 C1 1.327(17) . ?
N1 C3 1.373(18) . ?
N1 C4 1.472(18) . ?
N2 C1 1.324(17) . ?
N2 C2 1.394(18) . ?
N3 C7 1.33(2) . ?
N3 C5 1.356(18) . ?
N3 C8 1.467(19) . ?
N4 C5 1.297(18) . ?
N4 C6 1.381(18) . ?
N5 C11 1.30(2) . ?
N5 C9 1.380(18) . ?
N5 C12 1.459(19) . ?
N6 C9 1.324(18) . ?
N6 C10 1.369(19) . ?
N7 C13 1.353(17) . ?
N7 C15 1.401(18) . ?
N7 C16 1.471(17) . ?
N8 C13 1.337(17) . ?
N8 C14 1.371(17) . ?
N9 C17 1.324(17) . ?
N9 C19 1.425(17) . ?
N9 C20 1.496(19) . ?
N10 C17 1.338(17) . ?
N10 C18 1.450(17) . ?
C1 H1 0.9300 . ?
C2 C3 1.33(2) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5 0.9300 . ?
C6 C7 1.34(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9 0.9300 . ?
C10 C11 1.37(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9300 . ?
C14 C15 1.388(19) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17 0.9300 . ?
C18 C19 1.39(2) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Co1 N4 90.3(5) . . ?
N2 Co1 O11 92.0(4) . . ?
N4 Co1 O11 89.0(4) . . ?
N2 Co1 O13 177.7(4) . . ?
N4 Co1 O13 87.8(4) . . ?
O11 Co1 O13 89.3(4) . . ?
N2 Co1 N6 92.5(5) . . ?
N4 Co1 N6 176.8(5) . . ?
O11 Co1 N6 89.4(4) . . ?
O13 Co1 N6 89.4(4) . . ?
N2 Co1 O3 90.5(4) . . ?
N4 Co1 O3 90.7(4) . . ?
O11 Co1 O3 177.5(3) . . ?
O13 Co1 O3 88.2(3) . . ?
N6 Co1 O3 90.8(4) . . ?
O14 Co2 N10 111.6(5) . . ?
O14 Co2 N8 144.4(4) . . ?
N10 Co2 N8 104.0(5) . . ?
O14 Co2 O2 86.1(4) . . ?
N10 Co2 O2 96.3(4) . . ?
N8 Co2 O2 89.7(4) . . ?
O14 Co2 O8 87.0(4) . . ?
N10 Co2 O8 94.6(4) . . ?
N8 Co2 O8 90.7(4) . . ?
O2 Co2 O8 168.7(4) . . ?
O3 V1 O2 109.9(5) . . ?
O3 V1 O4 107.6(5) . . ?
O2 V1 O4 108.9(4) . . ?
O3 V1 O1 108.8(4) . . ?
O2 V1 O1 110.1(5) . . ?
O4 V1 O1 111.5(4) . . ?
O5 V2 O6 108.5(5) . . ?
O5 V2 O4 109.9(5) . 3_456 ?
O6 V2 O4 107.7(5) . 3_456 ?
O5 V2 O1 109.5(5) . . ?
O6 V2 O1 108.5(4) . . ?
O4 V2 O1 112.6(4) 3_456 . ?
O9 V3 O8 109.4(5) . . ?
O9 V3 O7 110.2(5) . . ?
O8 V3 O7 109.5(4) . . ?
O9 V3 O10 110.0(5) . . ?
O8 V3 O10 107.6(4) . . ?
O7 V3 O10 110.1(4) . . ?
O12 V4 O11 110.6(5) . . ?
O12 V4 O7 108.7(5) . 2_655 ?
O11 V4 O7 109.3(5) . 2_655 ?
O12 V4 O10 110.5(5) . 4_756 ?
O11 V4 O10 109.3(4) . 4_756 ?
O7 V4 O10 108.5(4) 2_655 4_756 ?
V1 O1 V2 126.9(5) . . ?
V1 O2 Co2 163.5(6) . . ?
V1 O3 Co1 173.9(5) . . ?
V1 O4 V2 141.6(6) . 3_556 ?
V3 O7 V4 128.0(5) . 2_654 ?
V3 O8 Co2 172.6(6) . . ?
V3 O10 V4 148.2(5) . 4_746 ?
V4 O11 Co1 166.0(6) . . ?
Co1 O13 H13C 116.4 . . ?
Co1 O13 H13D 123.5 . . ?
H13C O13 H13D 108.3 . . ?
Co2 O14 H14C 126.5 . . ?
Co2 O14 H14D 123.7 . . ?
H14C O14 H14D 108.2 . . ?
C1 N1 C3 104.7(12) . . ?
C1 N1 C4 127.1(13) . . ?
C3 N1 C4 128.3(13) . . ?
C1 N2 C2 97.4(13) . . ?
C1 N2 Co1 131.0(11) . . ?
C2 N2 Co1 131.6(10) . . ?
C7 N3 C5 106.2(14) . . ?
C7 N3 C8 125.2(15) . . ?
C5 N3 C8 128.4(15) . . ?
C5 N4 C6 102.4(13) . . ?
C5 N4 Co1 130.7(11) . . ?
C6 N4 Co1 126.7(11) . . ?
C11 N5 C9 106.9(14) . . ?
C11 N5 C12 125.3(15) . . ?
C9 N5 C12 127.7(15) . . ?
C9 N6 C10 102.2(14) . . ?
C9 N6 Co1 128.3(11) . . ?
C10 N6 Co1 129.5(11) . . ?
C13 N7 C15 108.7(12) . . ?
C13 N7 C16 125.6(13) . . ?
C15 N7 C16 125.6(13) . . ?
C13 N8 C14 104.9(12) . . ?
C13 N8 Co2 127.2(10) . . ?
C14 N8 Co2 126.4(10) . . ?
C17 N9 C19 111.4(13) . . ?
C17 N9 C20 126.7(13) . . ?
C19 N9 C20 121.8(13) . . ?
C17 N10 C18 104.7(13) . . ?
C17 N10 Co2 126.7(10) . . ?
C18 N10 Co2 128.5(10) . . ?
N2 C1 N1 118.0(14) . . ?
N2 C1 H1 121.0 . . ?
N1 C1 H1 121.0 . . ?
C3 C2 N2 115.3(15) . . ?
C3 C2 H2 122.3 . . ?
N2 C2 H2 122.3 . . ?
C2 C3 N1 104.6(14) . . ?
C2 C3 H3 127.7 . . ?
N1 C3 H3 127.7 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 N3 113.6(15) . . ?
N4 C5 H5 123.2 . . ?
N3 C5 H5 123.2 . . ?
C7 C6 N4 111.3(16) . . ?
C7 C6 H6 124.4 . . ?
N4 C6 H6 124.4 . . ?
N3 C7 C6 106.4(15) . . ?
N3 C7 H7 126.8 . . ?
C6 C7 H7 126.8 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 N5 112.6(15) . . ?
N6 C9 H9 123.7 . . ?
N5 C9 H9 123.7 . . ?
N6 C10 C11 111.7(16) . . ?
N6 C10 H10 124.2 . . ?
C11 C10 H10 124.2 . . ?
N5 C11 C10 106.5(16) . . ?
N5 C11 H11 126.7 . . ?
C10 C11 H11 126.7 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N8 C13 N7 111.3(13) . . ?
N8 C13 H13 124.4 . . ?
N7 C13 H13 124.4 . . ?
N8 C14 C15 112.1(13) . . ?
N8 C14 H14 124.0 . . ?
C15 C14 H14 124.0 . . ?
C14 C15 N7 102.9(13) . . ?
C14 C15 H15 128.5 . . ?
N7 C15 H15 128.5 . . ?
N7 C16 H16A 109.5 . . ?
N7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N9 C17 N10 111.2(13) . . ?
N9 C17 H17 124.4 . . ?
N10 C17 H17 124.4 . . ?
C19 C18 N10 110.3(13) . . ?
C19 C18 H18 124.8 . . ?
N10 C18 H18 124.8 . . ?
C18 C19 N9 102.3(13) . . ?
C18 C19 H19 128.8 . . ?
N9 C19 H19 128.8 . . ?
N9 C20 H20A 109.5 . . ?
N9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.172
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1003694'
_audit_update_record             
;
2014-11-22 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H18 Cd N4 O7 V2'
_chemical_formula_weight         520.56

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'
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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                   9.4328(11)
_cell_length_b                   16.3873(17)
_cell_length_c                   11.3981(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.731(2)
_cell_angle_gamma                90.00
_cell_volume                     1736.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4824
_exptl_absorpt_correction_T_max  0.7693
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8569
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3035
_reflns_number_gt                2332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0155P)²+4.1541P] 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         3035
_refine_ls_number_parameters     219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
Cd1 Cd 1.05519(4) 0.08002(2) 0.40850(3) 0.02550(11) Uani 1 1 d . . .
V1 V 0.67079(8) 0.02639(4) 0.36662(7) 0.02187(19) Uani 1 1 d . . .
V2 V 0.55969(8) -0.13586(4) 0.48862(7) 0.02202(19) Uani 1 1 d . . .
N1 N 0.8944(4) 0.2693(2) 0.6173(4) 0.0330(10) Uani 1 1 d . . .
N2 N 1.0079(4) 0.1721(2) 0.5386(4) 0.0313(10) Uani 1 1 d . . .
N3 N 1.1874(4) -0.1084(2) 0.1847(4) 0.0328(10) Uani 1 1 d . . .
N4 N 1.0866(4) -0.0094(2) 0.2705(3) 0.0314(10) Uani 1 1 d . . .
O1 O 0.5710(3) -0.06652(19) 0.3675(3) 0.0320(8) Uani 1 1 d . . .
O2 O 0.8397(3) 0.01302(17) 0.4370(3) 0.0244(7) Uani 1 1 d . . .
O3 O 0.6745(4) 0.0548(2) 0.2315(3) 0.0366(9) Uani 1 1 d . . .
O4 O 0.5883(4) 0.1055(2) 0.4401(3) 0.0386(9) Uani 1 1 d . . .
O5 O 0.5334(4) -0.22796(19) 0.4357(3) 0.0362(9) Uani 1 1 d . . .
O6 O 1.2873(3) 0.1315(2) 0.4180(3) 0.0325(8) Uani 1 1 d . . .
O7 O 0.9147(4) 0.1632(2) 0.2512(3) 0.0484(10) Uani 1 1 d . . .
H7B H 0.8462 0.1363 0.2109 0.058 Uiso 1 1 d R . .
H7C H 0.9669 0.1840 0.2051 0.058 Uiso 1 1 d R . .
C1 C 0.8889(6) 0.2147(3) 0.5302(5) 0.0358(13) Uani 1 1 d . . .
H1 H 0.8098 0.2076 0.4703 0.043 Uiso 1 1 calc R . .
C2 C 1.0943(6) 0.2014(3) 0.6385(5) 0.0435(14) Uani 1 1 d . . .
H2 H 1.1864 0.1825 0.6682 0.052 Uiso 1 1 calc R . .
C3 C 1.0262(6) 0.2613(3) 0.6874(5) 0.0408(14) Uani 1 1 d . . .
H3 H 1.0618 0.2913 0.7553 0.049 Uiso 1 1 calc R . .
C4 C 0.7844(6) 0.3315(3) 0.6285(5) 0.0445(14) Uani 1 1 d . . .
H4A H 0.7853 0.3430 0.7122 0.053 Uiso 1 1 calc R . .
H4B H 0.6901 0.3102 0.5955 0.053 Uiso 1 1 calc R . .
C5 C 0.8094(7) 0.4083(4) 0.5663(6) 0.0631(19) Uani 1 1 d . . .
H5A H 0.9034 0.4289 0.5976 0.095 Uiso 1 1 calc R . .
H5B H 0.7383 0.4479 0.5785 0.095 Uiso 1 1 calc R . .
H5C H 0.8026 0.3978 0.4827 0.095 Uiso 1 1 calc R . .
C6 C 1.2014(6) -0.0562(3) 0.2747(5) 0.0384(13) Uani 1 1 d . . .
H6 H 1.2824 -0.0529 0.3337 0.046 Uiso 1 1 calc R . .
C7 C 0.9964(6) -0.0334(3) 0.1706(5) 0.0426(14) Uani 1 1 d . . .
H7 H 0.9059 -0.0113 0.1436 0.051 Uiso 1 1 calc R . .
C8 C 1.0572(6) -0.0937(4) 0.1167(5) 0.0485(15) Uani 1 1 d . . .
H8 H 1.0179 -0.1203 0.0466 0.058 Uiso 1 1 calc R . .
C9 C 1.2957(6) -0.1675(3) 0.1594(5) 0.0476(15) Uani 1 1 d . . .
H9A H 1.2473 -0.2143 0.1185 0.057 Uiso 1 1 calc R . .
H9B H 1.3511 -0.1865 0.2339 0.057 Uiso 1 1 calc R . .
C10 C 1.3940(8) -0.1318(4) 0.0855(7) 0.078(2) Uani 1 1 d . . .
H10A H 1.3416 -0.1198 0.0077 0.116 Uiso 1 1 calc R . .
H10B H 1.4695 -0.1699 0.0788 0.116 Uiso 1 1 calc R . .
H10C H 1.4350 -0.0824 0.1219 0.116 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
Cd1 N4 2.205(4) . ?
Cd1 N2 2.213(4) . ?
Cd1 O6 2.331(3) . ?
Cd1 O2 2.381(3) . ?
Cd1 O2 2.412(3) 3_756 ?
Cd1 O7 2.454(3) . ?
V1 O3 1.615(3) . ?
V1 O2 1.672(3) . ?
V1 O1 1.791(3) . ?
V1 O4 1.792(3) . ?
V2 O5 1.629(3) . ?
V2 O6 1.644(3) 3_756 ?
V2 O4 1.800(3) 3_656 ?
V2 O1 1.805(3) . ?
N1 C1 1.330(6) . ?
N1 C3 1.366(6) . ?
N1 C4 1.476(6) . ?
N2 C1 1.312(6) . ?
N2 C2 1.370(6) . ?
N3 C6 1.325(6) . ?
N3 C8 1.358(6) . ?
N3 C9 1.471(6) . ?
N4 C6 1.322(6) . ?
N4 C7 1.360(6) . ?
O2 Cd1 2.412(3) 3_756 ?
O4 V2 1.800(3) 3_656 ?
O6 V2 1.644(3) 3_756 ?
O7 H7B 0.8500 . ?
O7 H7C 0.8499 . ?
C1 H1 0.9300 . ?
C2 C3 1.345(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.483(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6 0.9300 . ?
C7 C8 1.343(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.476(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cd1 N2 175.68(15) . . ?
N4 Cd1 O6 92.02(13) . . ?
N2 Cd1 O6 90.92(13) . . ?
N4 Cd1 O2 90.68(13) . . ?
N2 Cd1 O2 87.11(13) . . ?
O6 Cd1 O2 167.77(10) . . ?
N4 Cd1 O2 90.72(12) . 3_756 ?
N2 Cd1 O2 92.65(13) . 3_756 ?
O6 Cd1 O2 85.84(10) . 3_756 ?
O2 Cd1 O2 82.19(10) . 3_756 ?
N4 Cd1 O7 88.21(14) . . ?
N2 Cd1 O7 88.05(14) . . ?
O6 Cd1 O7 102.71(11) . . ?
O2 Cd1 O7 89.29(11) . . ?
O2 Cd1 O7 171.41(11) 3_756 . ?
O3 V1 O2 108.84(16) . . ?
O3 V1 O1 110.25(16) . . ?
O2 V1 O1 110.17(14) . . ?
O3 V1 O4 108.59(17) . . ?
O2 V1 O4 108.91(16) . . ?
O1 V1 O4 110.04(16) . . ?
O5 V2 O6 110.01(17) . 3_756 ?
O5 V2 O4 110.00(17) . 3_656 ?
O6 V2 O4 111.07(17) 3_756 3_656 ?
O5 V2 O1 108.97(16) . . ?
O6 V2 O1 107.97(15) 3_756 . ?
O4 V2 O1 108.78(16) 3_656 . ?
C1 N1 C3 106.8(4) . . ?
C1 N1 C4 126.1(4) . . ?
C3 N1 C4 126.8(4) . . ?
C1 N2 C2 104.8(4) . . ?
C1 N2 Cd1 125.5(3) . . ?
C2 N2 Cd1 129.6(3) . . ?
C6 N3 C8 106.9(4) . . ?
C6 N3 C9 126.5(4) . . ?
C8 N3 C9 126.6(4) . . ?
C6 N4 C7 104.8(4) . . ?
C6 N4 Cd1 124.6(3) . . ?
C7 N4 Cd1 130.5(3) . . ?
V1 O1 V2 129.67(18) . . ?
V1 O2 Cd1 129.80(16) . . ?
V1 O2 Cd1 132.37(16) . 3_756 ?
Cd1 O2 Cd1 97.81(10) . 3_756 ?
V1 O4 V2 147.4(2) . 3_656 ?
V2 O6 Cd1 139.56(18) 3_756 . ?
Cd1 O7 H7B 112.1 . . ?
Cd1 O7 H7C 112.1 . . ?
H7B O7 H7C 109.9 . . ?
N2 C1 N1 112.2(5) . . ?
N2 C1 H1 123.9 . . ?
N1 C1 H1 123.9 . . ?
C3 C2 N2 110.0(5) . . ?
C3 C2 H2 125.0 . . ?
N2 C2 H2 125.0 . . ?
C2 C3 N1 106.2(5) . . ?
C2 C3 H3 126.9 . . ?
N1 C3 H3 126.9 . . ?
N1 C4 C5 112.0(5) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 N3 111.9(5) . . ?
N4 C6 H6 124.1 . . ?
N3 C6 H6 124.1 . . ?
C8 C7 N4 109.9(5) . . ?
C8 C7 H7 125.0 . . ?
N4 C7 H7 125.0 . . ?
C7 C8 N3 106.5(4) . . ?
C7 C8 H8 126.8 . . ?
N3 C8 H8 126.8 . . ?
N3 C9 C10 112.0(5) . . ?
N3 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N3 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
N4 Cd1 N2 C1 3(2) . . . . ?
O6 Cd1 N2 C1 136.1(4) . . . . ?
O2 Cd1 N2 C1 -55.9(4) . . . . ?
O2 Cd1 N2 C1 -138.0(4) 3_756 . . . ?
O7 Cd1 N2 C1 33.5(4) . . . . ?
N4 Cd1 N2 C2 -172.0(18) . . . . ?
O6 Cd1 N2 C2 -39.2(4) . . . . ?
O2 Cd1 N2 C2 128.7(4) . . . . ?
O2 Cd1 N2 C2 46.7(4) 3_756 . . . ?
O7 Cd1 N2 C2 -141.9(4) . . . . ?
N2 Cd1 N4 C6 179(54) . . . . ?
O6 Cd1 N4 C6 46.2(4) . . . . ?
O2 Cd1 N4 C6 -121.8(4) . . . . ?
O2 Cd1 N4 C6 -39.6(4) 3_756 . . . ?
O7 Cd1 N4 C6 148.9(4) . . . . ?
N2 Cd1 N4 C7 -6(2) . . . . ?
O6 Cd1 N4 C7 -138.7(5) . . . . ?
O2 Cd1 N4 C7 53.3(5) . . . . ?
O2 Cd1 N4 C7 135.5(5) 3_756 . . . ?
O7 Cd1 N4 C7 -36.0(5) . . . . ?
O3 V1 O1 V2 166.9(2) . . . . ?
O2 V1 O1 V2 46.8(3) . . . . ?
O4 V1 O1 V2 -73.3(3) . . . . ?
O5 V2 O1 V1 -149.2(2) . . . . ?
O6 V2 O1 V1 -29.8(3) 3_756 . . . ?
O4 V2 O1 V1 90.8(3) 3_656 . . . ?
O3 V1 O2 Cd1 30.5(3) . . . . ?
O1 V1 O2 Cd1 151.51(19) . . . . ?
O4 V1 O2 Cd1 -87.7(2) . . . . ?
O3 V1 O2 Cd1 -147.2(2) . . . 3_756 ?
O1 V1 O2 Cd1 -26.2(3) . . . 3_756 ?
O4 V1 O2 Cd1 94.5(2) . . . 3_756 ?
N4 Cd1 O2 V1 -87.7(2) . . . . ?
N2 Cd1 O2 V1 88.6(2) . . . . ?
O6 Cd1 O2 V1 169.5(4) . . . . ?
O2 Cd1 O2 V1 -178.3(3) 3_756 . . . ?
O7 Cd1 O2 V1 0.5(2) . . . . ?
N4 Cd1 O2 Cd1 90.64(13) . . . 3_756 ?
N2 Cd1 O2 Cd1 -93.08(13) . . . 3_756 ?
O6 Cd1 O2 Cd1 -12.1(6) . . . 3_756 ?
O2 Cd1 O2 Cd1 0.0 3_756 . . 3_756 ?
O7 Cd1 O2 Cd1 178.84(12) . . . 3_756 ?
O3 V1 O4 V2 116.2(4) . . . 3_656 ?
O2 V1 O4 V2 -125.4(4) . . . 3_656 ?
O1 V1 O4 V2 -4.5(4) . . . 3_656 ?
N4 Cd1 O6 V2 -113.1(3) . . . 3_756 ?
N2 Cd1 O6 V2 70.0(3) . . . 3_756 ?
O2 Cd1 O6 V2 -10.5(7) . . . 3_756 ?
O2 Cd1 O6 V2 -22.5(3) 3_756 . . 3_756 ?
O7 Cd1 O6 V2 158.3(3) . . . 3_756 ?
C2 N2 C1 N1 0.5(6) . . . . ?
Cd1 N2 C1 N1 -175.8(3) . . . . ?
C3 N1 C1 N2 -0.2(6) . . . . ?
C4 N1 C1 N2 174.4(4) . . . . ?
C1 N2 C2 C3 -0.6(6) . . . . ?
Cd1 N2 C2 C3 175.5(4) . . . . ?
N2 C2 C3 N1 0.5(6) . . . . ?
C1 N1 C3 C2 -0.2(6) . . . . ?
C4 N1 C3 C2 -174.8(5) . . . . ?
C1 N1 C4 C5 -88.7(6) . . . . ?
C3 N1 C4 C5 84.9(7) . . . . ?
C7 N4 C6 N3 -0.8(6) . . . . ?
Cd1 N4 C6 N3 175.3(3) . . . . ?
C8 N3 C6 N4 1.2(6) . . . . ?
C9 N3 C6 N4 177.9(5) . . . . ?
C6 N4 C7 C8 0.1(6) . . . . ?
Cd1 N4 C7 C8 -175.7(4) . . . . ?
N4 C7 C8 N3 0.6(7) . . . . ?
C6 N3 C8 C7 -1.1(6) . . . . ?
C9 N3 C8 C7 -177.8(5) . . . . ?
C6 N3 C9 C10 -87.9(7) . . . . ?
C8 N3 C9 C10 88.2(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.118
