# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'M. Ishaque Khan'
_publ_contact_author_address     
;
Chemistry Department
Illinois Institute of Technology
3101 South Dearborn St.
Chicago
Illinois
IL 60616
UNITED STATES OF AMERICA
;

_publ_contact_author_email       KHAN@IIT.EDU

_publ_section_title              
;
Synthesis and characterization of a novel
polyoxovanadate cluster
;
loop_
_publ_author_name
'M. Khan'
'Samar Ayesh'
'Robert Doedens'

data_isk120
_database_code_depnum_ccdc_archive 'CCDC 269613'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 Cl N8 O46 V16'
_chemical_formula_weight         2235.42

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   16.205(4)
_cell_length_b                   20.186(5)
_cell_length_c                   22.101(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.94(3)
_cell_angle_gamma                90.00
_cell_volume                     7225(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    969
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.26

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          .17
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4420
_exptl_absorpt_coefficient_mu    2.105
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'computed via SADABS'

_exptl_special_details           
;
Crystal orientation and preliminary unit cell constants were obtained from
reflections gathered from three sets of 15 frames each. Refined cell
parameters were computed after data collection on the basis of the setting
angles of 969 reflections with a resolution limit of 0.75 Angstroms.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '25s frames at 0.3 degree omega increments'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            37616
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.29
_diffrn_special_details          
;
A full sphere of data was collected by use of 0.3 degree omega increments
and 25s frame counting times. The first 50 frames were remeasured at the
end of data collection and no evidence of decay was observed. To a
limiting resolution of 0.75 A, the average redundancy was 4.35 and
R(sym) for the uncorrected data was 0.072.

Hydrogen atoms, with the exception of those on O22, O23, N16, N20, and C20
through C23 were included at idealized positions and refined by use of the
riding model.
;

_reflns_number_total             8698
_reflns_number_gt                6985
_reflns_threshold_expression     >2sigma(I)

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

Hydrogen atoms, with the exception of those on O22, O23, N16, N20, and C20
through C23 were included at idealized positions and refined by use of the
riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.03P)^2^+75.0P] where P=(Fo^2^+2Fc^2^)/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         8698
_refine_ls_number_parameters     503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1028
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_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
V1 V 0.69912(4) 0.23622(3) 0.32494(3) 0.00765(13) Uani 1 1 d . . .
V2 V 0.70977(4) 0.25454(3) 0.19377(3) 0.00814(13) Uani 1 1 d . . .
V3 V 0.63256(4) 0.37621(3) 0.30061(3) 0.00777(13) Uani 1 1 d . . .
V4 V 0.56475(4) 0.25460(3) 0.40983(3) 0.00803(13) Uani 1 1 d . . .
V5 V 0.55090(4) 0.11065(3) 0.35659(3) 0.00790(13) Uani 1 1 d . . .
V6 V 0.64238(4) 0.11117(3) 0.21678(3) 0.00792(13) Uani 1 1 d . . .
V7 V 0.56768(4) 0.37607(3) 0.15061(3) 0.00863(13) Uani 1 1 d . . .
V8 V 0.61356(4) 0.16528(3) 0.07827(3) 0.00872(13) Uani 1 1 d . . .
Cl1 Cl 0.5000 0.24848(9) 0.2500 0.0319(4) Uani 1 2 d S . .
O1 O 0.70120(17) 0.18389(13) 0.25778(12) 0.0107(5) Uani 1 1 d . . .
O2 O 0.70526(16) 0.30495(13) 0.26688(12) 0.0100(5) Uani 1 1 d . . .
O3 O 0.64046(17) 0.30482(13) 0.36394(12) 0.0095(5) Uani 1 1 d . . .
O4 O 0.62978(16) 0.18363(13) 0.36748(12) 0.0099(5) Uani 1 1 d . . .
O5 O 0.66025(17) 0.31262(13) 0.14998(12) 0.0110(5) Uani 1 1 d . . .
O6 O 0.66769(17) 0.17685(13) 0.15165(12) 0.0107(5) Uani 1 1 d . . .
O7 O 0.61313(17) 0.40246(13) 0.22356(12) 0.0111(5) Uani 1 1 d . . .
O8 O 0.53660(17) 0.40057(13) 0.33053(12) 0.0109(5) Uani 1 1 d . . .
O9 O 0.49618(17) 0.17637(13) 0.41010(12) 0.0112(5) Uani 1 1 d . . .
O10 O 0.48640(17) 0.31086(13) 0.40321(12) 0.0110(5) Uani 1 1 d . . .
O11 O 0.60240(17) 0.08849(13) 0.28868(12) 0.0108(5) Uani 1 1 d . . .
O12 O 0.55219(17) 0.08752(13) 0.17071(12) 0.0112(5) Uani 1 1 d . . .
O13 O 0.78900(17) 0.22999(13) 0.35665(13) 0.0122(6) Uani 1 1 d . . .
O14 O 0.80437(18) 0.25563(14) 0.17568(13) 0.0138(6) Uani 1 1 d . . .
O15 O 0.69706(17) 0.42991(13) 0.32694(12) 0.0120(6) Uani 1 1 d . . .
O16 O 0.59903(18) 0.25995(14) 0.47863(12) 0.0140(6) Uani 1 1 d . . .
O17 O 0.57648(17) 0.05400(14) 0.40467(12) 0.0130(6) Uani 1 1 d . . .
O18 O 0.71043(17) 0.05497(13) 0.20524(12) 0.0122(6) Uani 1 1 d . . .
O19 O 0.59674(17) 0.43180(14) 0.10384(12) 0.0125(6) Uani 1 1 d . . .
O20 O 0.62922(18) 0.09092(14) 0.05189(12) 0.0129(6) Uani 1 1 d . . .
O21 O 0.64458(18) 0.21922(14) 0.02793(12) 0.0139(6) Uani 1 1 d . . .
O22 O 0.7542(2) 0.52781(17) 0.69103(14) 0.0230(7) Uani 1 1 d . . .
O23 O 0.2952(3) 0.13957(19) 0.57195(19) 0.0449(11) Uani 1 1 d . . .
N1 N 0.0889(2) 0.15833(19) 0.47703(17) 0.0216(8) Uani 1 1 d . . .
H31 H 0.0908 0.1904 0.5040 0.026 Uiso 1 1 calc R . .
N2 N 0.5628(3) 0.03749(19) 0.59198(19) 0.0276(9) Uani 1 1 d . . .
H32 H 0.5592 -0.0058 0.5884 0.033 Uiso 1 1 calc R . .
N3 N 0.7407(2) 0.47625(18) 0.57829(17) 0.0187(8) Uani 1 1 d . . .
H33 H 0.7484 0.5017 0.6103 0.022 Uiso 1 1 calc R . .
C1 C 0.0268(3) 0.1151(2) 0.4781(2) 0.0229(10) Uani 1 1 d . . .
H1 H -0.0145 0.1196 0.5073 0.028 Uiso 1 1 calc R . .
C2 C 0.0223(3) 0.0641(2) 0.4369(2) 0.0241(10) Uani 1 1 d . . .
H2 H -0.0221 0.0334 0.4369 0.029 Uiso 1 1 calc R . .
C3 C 0.0842(3) 0.0585(2) 0.3953(2) 0.0252(10) Uani 1 1 d . . .
H3 H 0.0832 0.0231 0.3670 0.030 Uiso 1 1 calc R . .
C4 C 0.1473(3) 0.1046(3) 0.3951(2) 0.0286(11) Uani 1 1 d . . .
H4 H 0.1895 0.1014 0.3665 0.034 Uiso 1 1 calc R . .
C5 C 0.1482(3) 0.1551(2) 0.4369(2) 0.0243(10) Uani 1 1 d . . .
H5 H 0.1907 0.1874 0.4371 0.029 Uiso 1 1 calc R . .
C6 C 0.6212(3) 0.0629(2) 0.6298(2) 0.0218(9) Uani 1 1 d . . .
H6 H 0.6563 0.0344 0.6532 0.026 Uiso 1 1 calc R . .
C7 C 0.6297(3) 0.1302(2) 0.6344(2) 0.0188(9) Uani 1 1 d . . .
H7 H 0.6711 0.1490 0.6606 0.023 Uiso 1 1 calc R . .
C8 C 0.5766(3) 0.1707(2) 0.6001(2) 0.0218(9) Uani 1 1 d . . .
H8 H 0.5824 0.2175 0.6022 0.026 Uiso 1 1 calc R . .
C9 C 0.5154(3) 0.1430(2) 0.5631(2) 0.0255(10) Uani 1 1 d . . .
H9 H 0.4779 0.1704 0.5405 0.031 Uiso 1 1 calc R . .
C10 C 0.5098(3) 0.0754(2) 0.5595(2) 0.0296(12) Uani 1 1 d . . .
H10 H 0.4684 0.0554 0.5340 0.035 Uiso 1 1 calc R . .
C11 C 0.7109(3) 0.3711(2) 0.5373(2) 0.0238(10) Uani 1 1 d . . .
H11 H 0.6989 0.3255 0.5427 0.029 Uiso 1 1 calc R . .
C12 C 0.7164(3) 0.3980(2) 0.4800(2) 0.0237(10) Uani 1 1 d . . .
H12 H 0.7075 0.3706 0.4453 0.028 Uiso 1 1 calc R . .
C13 C 0.7347(3) 0.4639(2) 0.4728(2) 0.0269(11) Uani 1 1 d . . .
H13 H 0.7391 0.4824 0.4335 0.032 Uiso 1 1 calc R . .
C14 C 0.7467(3) 0.5028(2) 0.5233(2) 0.0246(10) Uani 1 1 d . . .
H14 H 0.7593 0.5485 0.5191 0.029 Uiso 1 1 calc R . .
C15 C 0.7232(3) 0.4120(2) 0.5861(2) 0.0188(9) Uani 1 1 d . . .
H15 H 0.7194 0.3947 0.6258 0.023 Uiso 1 1 calc R . .
N16 N 0.0000 0.0447(3) 0.2500 0.0370(15) Uani 1 2 d S . .
H16 H 0.0000 0.0011 0.2500 0.044 Uiso 1 2 calc SR . .
C17 C 0.0700(3) 0.0797(3) 0.2357(2) 0.0304(11) Uani 1 1 d . . .
H17 H 0.1191 0.0574 0.2250 0.037 Uiso 1 1 calc R . .
C18 C 0.0666(5) 0.1477(3) 0.2374(3) 0.060(2) Uani 1 1 d . . .
H18 H 0.1154 0.1716 0.2290 0.072 Uiso 1 1 calc R . .
C19 C 0.0000 0.1816(3) 0.2500 0.064(4) Uani 1 2 d S . .
H19 H 0.0000 0.2287 0.2500 0.077 Uiso 1 2 calc SR . .
N20 N 0.5000 -0.0495(4) 0.2500 0.052(2) Uani 1 2 d S . .
C21 C 0.5562(4) -0.0824(4) 0.2855(3) 0.0478(18) Uani 1 1 d . . .
C22 C 0.5542(6) -0.1511(5) 0.2828(4) 0.095(4) Uani 1 1 d . . .
C23 C 0.5000 -0.1815(4) 0.2500 0.092(7) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0081(3) 0.0056(3) 0.0092(3) 0.0001(2) -0.0008(2) -0.0006(2)
V2 0.0090(3) 0.0061(3) 0.0093(3) 0.0001(2) 0.0010(2) 0.0005(2)
V3 0.0095(3) 0.0048(3) 0.0090(3) 0.0000(2) -0.0004(2) -0.0009(2)
V4 0.0108(3) 0.0062(3) 0.0071(3) -0.0002(2) -0.0002(2) -0.0015(2)
V5 0.0092(3) 0.0056(3) 0.0088(3) 0.0006(2) -0.0006(2) -0.0006(2)
V6 0.0097(3) 0.0047(3) 0.0093(3) -0.0004(2) -0.0001(2) 0.0008(2)
V7 0.0106(3) 0.0063(3) 0.0089(3) 0.0016(2) 0.0005(2) -0.0002(2)
V8 0.0102(3) 0.0079(3) 0.0081(3) -0.0006(2) 0.0008(2) 0.0014(2)
Cl1 0.0278(9) 0.0351(10) 0.0321(9) 0.000 -0.0094(7) 0.000
O1 0.0143(14) 0.0073(12) 0.0105(13) 0.0004(10) 0.0010(10) 0.0010(10)
O2 0.0104(13) 0.0076(12) 0.0120(13) 0.0007(10) -0.0001(10) 0.0000(10)
O3 0.0115(13) 0.0060(12) 0.0112(13) -0.0003(10) 0.0014(10) 0.0003(10)
O4 0.0105(13) 0.0069(12) 0.0122(13) -0.0012(10) 0.0011(10) -0.0012(10)
O5 0.0133(14) 0.0088(13) 0.0108(13) 0.0006(10) 0.0005(10) 0.0027(11)
O6 0.0139(14) 0.0065(12) 0.0117(13) 0.0003(10) 0.0002(10) -0.0021(10)
O7 0.0130(14) 0.0078(13) 0.0126(13) 0.0007(10) 0.0008(10) 0.0015(10)
O8 0.0118(14) 0.0096(13) 0.0112(13) 0.0014(10) -0.0002(10) 0.0000(10)
O9 0.0143(14) 0.0093(13) 0.0102(13) -0.0022(10) 0.0000(10) -0.0002(11)
O10 0.0125(14) 0.0095(13) 0.0113(13) -0.0001(10) 0.0015(10) -0.0005(11)
O11 0.0143(14) 0.0071(12) 0.0110(13) -0.0011(10) 0.0008(10) -0.0039(10)
O12 0.0133(14) 0.0067(12) 0.0134(13) 0.0002(10) -0.0018(11) -0.0009(10)
O13 0.0087(13) 0.0095(13) 0.0183(14) 0.0002(11) -0.0026(11) -0.0009(10)
O14 0.0125(14) 0.0109(13) 0.0179(14) -0.0008(11) 0.0013(11) 0.0000(11)
O15 0.0133(14) 0.0081(13) 0.0146(14) -0.0016(10) -0.0019(11) -0.0018(11)
O16 0.0204(15) 0.0132(14) 0.0082(13) 0.0000(10) -0.0031(11) -0.0040(12)
O17 0.0146(14) 0.0104(13) 0.0138(13) 0.0021(11) -0.0028(11) -0.0011(11)
O18 0.0131(14) 0.0094(13) 0.0142(14) -0.0001(10) 0.0015(11) 0.0042(11)
O19 0.0135(14) 0.0105(13) 0.0136(14) 0.0011(10) 0.0015(11) -0.0002(11)
O20 0.0153(15) 0.0117(13) 0.0117(13) -0.0027(10) 0.0010(11) 0.0034(11)
O21 0.0154(15) 0.0135(14) 0.0130(14) 0.0020(11) 0.0032(11) -0.0001(11)
O22 0.0243(17) 0.0270(17) 0.0177(15) -0.0004(13) 0.0007(13) 0.0108(14)
O23 0.071(3) 0.0236(19) 0.042(2) -0.0110(17) 0.033(2) -0.0081(19)
N1 0.029(2) 0.0158(18) 0.0192(19) -0.0081(14) -0.0030(16) 0.0026(16)
N2 0.038(2) 0.0105(18) 0.033(2) 0.0059(16) -0.0114(19) -0.0100(17)
N3 0.0153(18) 0.0166(18) 0.0239(19) -0.0059(15) -0.0008(15) 0.0015(14)
C1 0.021(2) 0.033(3) 0.015(2) -0.0032(18) 0.0022(17) 0.004(2)
C2 0.030(3) 0.020(2) 0.022(2) 0.0007(18) -0.0027(19) -0.0052(19)
C3 0.038(3) 0.018(2) 0.020(2) -0.0098(17) -0.005(2) 0.008(2)
C4 0.031(3) 0.034(3) 0.021(2) -0.002(2) 0.009(2) 0.003(2)
C5 0.023(2) 0.023(2) 0.027(2) 0.0046(19) 0.0013(19) -0.0047(19)
C6 0.017(2) 0.018(2) 0.030(2) 0.0080(18) -0.0020(18) -0.0039(17)
C7 0.016(2) 0.017(2) 0.024(2) 0.0029(17) -0.0004(17) -0.0030(17)
C8 0.026(2) 0.013(2) 0.026(2) 0.0054(17) -0.0034(19) -0.0076(18)
C9 0.033(3) 0.019(2) 0.024(2) 0.0049(18) -0.009(2) -0.004(2)
C10 0.039(3) 0.022(2) 0.027(3) 0.0034(19) -0.016(2) -0.017(2)
C11 0.031(3) 0.014(2) 0.026(2) 0.0031(18) -0.0047(19) -0.0067(19)
C12 0.028(3) 0.025(2) 0.018(2) -0.0038(18) -0.0020(18) -0.0040(19)
C13 0.035(3) 0.026(2) 0.021(2) 0.0062(19) 0.008(2) 0.005(2)
C14 0.028(3) 0.014(2) 0.032(3) 0.0049(18) 0.009(2) -0.0013(18)
C15 0.023(2) 0.017(2) 0.015(2) 0.0039(16) -0.0046(17) 0.0006(17)
N16 0.048(4) 0.030(3) 0.032(3) 0.000 0.000(3) 0.000
C17 0.023(3) 0.029(3) 0.039(3) -0.011(2) 0.010(2) 0.001(2)
C18 0.076(5) 0.028(3) 0.078(5) -0.018(3) 0.044(4) -0.028(3)
C19 0.108(9) 0.002(3) 0.089(7) 0.000 0.085(7) 0.000
N20 0.081(6) 0.036(4) 0.042(4) 0.000 0.024(4) 0.000
C21 0.021(3) 0.094(6) 0.028(3) 0.009(3) -0.001(2) -0.016(3)
C22 0.085(7) 0.125(8) 0.077(6) 0.083(6) 0.067(5) 0.099(7)
C23 0.167(17) 0.001(3) 0.115(13) 0.000 0.123(12) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O13 1.600(3) . ?
V1 O1 1.823(3) . ?
V1 O4 1.829(3) . ?
V1 O2 1.895(3) . ?
V1 O3 1.903(3) . ?
V1 V2 2.9331(11) . ?
V1 V4 2.9455(13) . ?
V1 V3 3.0658(11) . ?
V2 O14 1.597(3) . ?
V2 O5 1.704(3) . ?
V2 O2 1.913(3) . ?
V2 O6 1.936(3) . ?
V2 O1 2.017(3) . ?
V3 O15 1.602(3) . ?
V3 O8 1.779(3) . ?
V3 O7 1.801(3) . ?
V3 O3 2.010(3) . ?
V3 O2 2.018(3) . ?
V4 O16 1.605(3) . ?
V4 O10 1.706(3) . ?
V4 O3 1.909(3) . ?
V4 O9 1.931(3) . ?
V4 O4 2.026(3) . ?
V5 O17 1.606(3) . ?
V5 O11 1.798(3) . ?
V5 O12 1.818(3) 2_655 ?
V5 O4 1.960(3) . ?
V5 O9 2.004(3) . ?
V6 O18 1.608(3) . ?
V6 O11 1.796(3) . ?
V6 O12 1.817(3) . ?
V6 O1 1.956(3) . ?
V6 O6 2.010(3) . ?
V7 O19 1.609(3) . ?
V7 O8 1.823(3) 2_655 ?
V7 O7 1.829(3) . ?
V7 O10 1.961(3) 2_655 ?
V7 O5 1.973(3) . ?
V8 O20 1.633(3) . ?
V8 O21 1.647(3) . ?
V8 O9 1.819(3) 2_655 ?
O6 V8 1.832(3) . ?
O8 V7 1.823(3) 2_655 ?
O9 V8 1.819(3) 2_655 ?
O10 V7 1.961(3) 2_655 ?
O12 V5 1.818(3) 2_655 ?
N1 C5 1.331(6) . ?
N1 C1 1.333(6) . ?
N2 C10 1.341(6) . ?
N2 C6 1.343(6) . ?
N3 C14 1.335(6) . ?
N3 C15 1.339(6) . ?
C1 C2 1.374(6) . ?
C2 C3 1.387(7) . ?
C3 C4 1.382(7) . ?
C4 C5 1.376(7) . ?
C6 C7 1.369(6) . ?
C7 C8 1.393(6) . ?
C8 C9 1.383(6) . ?
C9 C10 1.370(7) . ?
C11 C15 1.366(6) . ?
C11 C12 1.385(6) . ?
C12 C13 1.375(7) . ?
C13 C14 1.372(7) . ?
N16 C17 1.383(6) . ?
N16 C17 1.383(6) 2 ?
C17 C18 1.374(8) . ?
C18 C19 1.316(8) . ?
C19 C18 1.316(8) 2 ?
N20 C21 1.356(7) 2_655 ?
N20 C21 1.356(8) . ?
C21 C22 1.387(13) . ?
C22 C23 1.277(13) . ?
C23 C22 1.277(13) 2_655 ?

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
O13 V1 O1 105.64(14) . . ?
O13 V1 O4 107.17(14) . . ?
O1 V1 O4 96.37(12) . . ?
O13 V1 O2 106.64(13) . . ?
O1 V1 O2 82.53(12) . . ?
O4 V1 O2 145.13(12) . . ?
O13 V1 O3 108.67(13) . . ?
O1 V1 O3 144.48(12) . . ?
O4 V1 O3 82.21(12) . . ?
O2 V1 O3 79.18(12) . . ?
O13 V1 V2 111.09(11) . . ?
O1 V1 V2 42.70(9) . . ?
O4 V1 V2 129.72(9) . . ?
O2 V1 V2 39.84(8) . . ?
O3 V1 V2 113.76(9) . . ?
O13 V1 V4 114.36(11) . . ?
O1 V1 V4 128.76(9) . . ?
O4 V1 V4 42.72(9) . . ?
O2 V1 V4 113.33(9) . . ?
O3 V1 V4 39.49(8) . . ?
V2 V1 V4 133.09(3) . . ?
O13 V1 V3 117.32(10) . . ?
O1 V1 V3 114.04(9) . . ?
O4 V1 V3 113.98(9) . . ?
O2 V1 V3 39.87(8) . . ?
O3 V1 V3 39.67(8) . . ?
V2 V1 V3 75.08(2) . . ?
V4 V1 V3 74.47(2) . . ?
O14 V2 O5 106.61(14) . . ?
O14 V2 O2 105.58(14) . . ?
O5 V2 O2 94.76(12) . . ?
O14 V2 O6 102.48(13) . . ?
O5 V2 O6 97.63(13) . . ?
O2 V2 O6 144.50(12) . . ?
O14 V2 O1 105.95(13) . . ?
O5 V2 O1 147.43(13) . . ?
O2 V2 O1 77.19(11) . . ?
O6 V2 O1 74.51(11) . . ?
O14 V2 V1 109.77(11) . . ?
O5 V2 V1 127.29(10) . . ?
O2 V2 V1 39.39(8) . . ?
O6 V2 V1 109.97(8) . . ?
O1 V2 V1 37.80(8) . . ?
O15 V3 O8 104.23(14) . . ?
O15 V3 O7 103.62(14) . . ?
O8 V3 O7 98.22(13) . . ?
O15 V3 O3 101.94(13) . . ?
O8 V3 O3 88.58(12) . . ?
O7 V3 O3 150.96(12) . . ?
O15 V3 O2 103.57(13) . . ?
O8 V3 O2 149.62(12) . . ?
O7 V3 O2 86.90(12) . . ?
O3 V3 O2 73.86(11) . . ?
O15 V3 V1 109.80(10) . . ?
O8 V3 V1 119.75(9) . . ?
O7 V3 V1 119.09(9) . . ?
O3 V3 V1 37.18(8) . . ?
O2 V3 V1 37.01(8) . . ?
O16 V4 O10 105.61(15) . . ?
O16 V4 O3 105.04(14) . . ?
O10 V4 O3 95.21(13) . . ?
O16 V4 O9 103.47(13) . . ?
O10 V4 O9 96.78(13) . . ?
O3 V4 O9 144.68(12) . . ?
O16 V4 O4 108.45(13) . . ?
O10 V4 O4 145.92(12) . . ?
O3 V4 O4 77.08(11) . . ?
O9 V4 O4 74.43(11) . . ?
O16 V4 V1 111.86(11) . . ?
O10 V4 V1 126.39(10) . . ?
O3 V4 V1 39.32(8) . . ?
O9 V4 V1 109.68(9) . . ?
O4 V4 V1 37.76(8) . . ?
O17 V5 O11 104.97(14) . . ?
O17 V5 O12 104.50(14) . 2_655 ?
O11 V5 O12 96.10(13) . 2_655 ?
O17 V5 O4 107.54(13) . . ?
O11 V5 O4 88.30(12) . . ?
O12 V5 O4 145.29(12) 2_655 . ?
O17 V5 O9 100.98(13) . . ?
O11 V5 O9 152.17(12) . . ?
O12 V5 O9 86.90(12) 2_655 . ?
O4 V5 O9 74.32(11) . . ?
O18 V6 O11 103.32(14) . . ?
O18 V6 O12 105.59(14) . . ?
O11 V6 O12 96.98(13) . . ?
O18 V6 O1 106.07(13) . . ?
O11 V6 O1 88.06(12) . . ?
O12 V6 O1 145.80(12) . . ?
O18 V6 O6 101.19(13) . . ?
O11 V6 O6 152.96(12) . . ?
O12 V6 O6 87.23(12) . . ?
O1 V6 O6 74.25(11) . . ?
O19 V7 O8 104.53(14) . 2_655 ?
O19 V7 O7 104.16(13) . . ?
O8 V7 O7 93.91(12) 2_655 . ?
O19 V7 O10 102.38(13) . 2_655 ?
O8 V7 O10 85.53(12) 2_655 2_655 ?
O7 V7 O10 152.70(12) . 2_655 ?
O19 V7 O5 102.14(13) . . ?
O8 V7 O5 152.73(12) 2_655 . ?
O7 V7 O5 84.93(12) . . ?
O10 V7 O5 83.35(12) 2_655 . ?
O20 V8 O21 108.16(14) . . ?
O20 V8 O9 109.15(14) . 2_655 ?
O21 V8 O9 109.64(14) . 2_655 ?
O20 V8 O6 110.95(13) . . ?
O21 V8 O6 111.44(14) . . ?
O9 V8 O6 107.48(13) 2_655 . ?
V1 O1 V6 142.17(16) . . ?
V1 O1 V2 99.50(12) . . ?
V6 O1 V2 104.46(12) . . ?
V1 O2 V2 100.77(13) . . ?
V1 O2 V3 103.13(13) . . ?
V2 O2 V3 136.95(14) . . ?
V1 O3 V4 101.19(12) . . ?
V1 O3 V3 103.15(12) . . ?
V4 O3 V3 136.35(15) . . ?
V1 O4 V5 141.50(15) . . ?
V1 O4 V4 99.51(12) . . ?
V5 O4 V4 103.94(13) . . ?
V2 O5 V7 141.85(16) . . ?
V8 O6 V2 132.77(15) . . ?
V8 O6 V6 116.53(14) . . ?
V2 O6 V6 105.49(13) . . ?
V3 O7 V7 143.15(16) . . ?
V3 O8 V7 147.00(17) . 2_655 ?
V8 O9 V4 131.79(15) 2_655 . ?
V8 O9 V5 117.14(14) 2_655 . ?
V4 O9 V5 105.86(13) . . ?
V4 O10 V7 144.58(16) . 2_655 ?
V6 O11 V5 150.07(17) . . ?
V6 O12 V5 146.25(16) . 2_655 ?
C5 N1 C1 122.8(4) . . ?
C10 N2 C6 122.7(4) . . ?
C14 N3 C15 121.8(4) . . ?
N1 C1 C2 120.1(4) . . ?
C1 C2 C3 118.5(4) . . ?
C4 C3 C2 119.9(4) . . ?
C5 C4 C3 119.2(5) . . ?
N1 C5 C4 119.5(4) . . ?
N2 C6 C7 119.5(4) . . ?
C6 C7 C8 118.9(4) . . ?
C9 C8 C7 120.1(4) . . ?
C10 C9 C8 118.8(4) . . ?
N2 C10 C9 119.8(4) . . ?
C15 C11 C12 118.2(4) . . ?
C13 C12 C11 120.3(4) . . ?
C14 C13 C12 119.0(4) . . ?
N3 C14 C13 119.9(4) . . ?
N3 C15 C11 120.7(4) . . ?
C17 N16 C17 118.5(7) . 2 ?
C18 C17 N16 118.0(5) . . ?
C19 C18 C17 124.1(6) . . ?
C18 C19 C18 117.2(7) 2 . ?
C21 N20 C21 121.2(9) 2_655 . ?
N20 C21 C22 116.8(7) . . ?
C23 C22 C21 121.3(7) . . ?
C22 C23 C22 122.5(10) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.135