#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313549.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313549
loop_
_publ_author_name
'M. Ishaque Khan'
'Elizabeth Yohannes'
'Robert J. Doedens'
_publ_section_title
;
 A Novel Series of Materials Composed of Arrays of Vanadium Oxide
 Container Molecules, {V18O42(X)} (X = H2O, Cl-, Br-): Synthesis and
 Characterization of [M2(H2N(CH2)2NH2)5][{M(H2N(CH2)2NH2)2}2V18O42(X)].
 9H2O (M = Zn, Cd)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3125
_journal_page_last               3129
_journal_paper_doi               10.1021/ic025889u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C9 H46 N9 O26 V9 Zn2'
_chemical_formula_weight         1285.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   n/a
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.3320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3723(7)
_cell_length_b                   20.9837(11)
_cell_length_c                   15.8379(8)
_cell_measurement_reflns_used    6095
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.4
_cell_volume                     4078.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '20s frames at 0.3 deg omega increments'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43312
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_absorpt_process_details   'computed via SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.974
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.100P)²+40.0P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.1970
_reflns_number_gt                8950
_reflns_number_total             10080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025889usi20021029_094446.cif
_cod_data_source_block           isk35
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4313549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 0.14527(8) 0.7500 0.02586(6) 0.0205(2) Uani 1 2 d S . .
Zn2 Zn 0.5000 0.5000 0.0000 0.0306(3) Uani 1 2 d S . .
Zn3 Zn 0.26879(6) 0.55247(4) 0.43172(5) 0.02801(19) Uani 1 1 d . . .
V1 V 0.39950(10) 0.7500 0.27939(8) 0.0114(2) Uani 1 2 d S . .
V2 V 0.43584(10) 0.7500 0.09760(8) 0.0130(2) Uani 1 2 d S . .
V3 V 0.63743(10) 0.7500 0.02760(8) 0.0124(2) Uani 1 2 d S . .
V4 V 0.87760(10) 0.7500 0.08528(8) 0.0136(3) Uani 1 2 d S . .
V5 V 0.96240(11) 0.7500 0.42392(9) 0.0197(3) Uani 1 2 d S . .
V6 V 0.53818(11) 0.7500 0.45110(9) 0.0180(3) Uani 1 2 d S . .
V7 V 0.95891(8) 0.66223(5) 0.28613(6) 0.0208(2) Uani 1 1 d . . .
V8 V 0.79572(8) 0.66090(5) 0.46554(6) 0.0194(2) Uani 1 1 d . . .
V9 V 0.51851(7) 0.62471(4) 0.15401(6) 0.01387(19) Uani 1 1 d . . .
V10 V 0.81163(8) 0.62177(4) 0.13040(6) 0.0159(2) Uani 1 1 d . . .
V11 V 0.56815(8) 0.62217(4) 0.38978(6) 0.0160(2) Uani 1 1 d . . .
V12 V 0.70483(8) 0.56963(5) 0.27140(6) 0.0184(2) Uani 1 1 d . . .
O1 O 0.2715(5) 0.7500 0.2870(4) 0.0185(11) Uani 1 2 d S . .
O2 O 0.3274(5) 0.7500 0.0264(4) 0.0202(12) Uani 1 2 d S . .
O3 O 0.6094(5) 0.7500 -0.0751(4) 0.0222(12) Uani 1 2 d S . .
O4 O 0.9594(5) 0.7500 0.0116(4) 0.0194(11) Uani 1 2 d S . .
O5 O 1.0724(5) 0.7500 0.4913(4) 0.0308(15) Uani 1 2 d S . .
O6 O 0.4673(5) 0.7500 0.5294(4) 0.0220(12) Uani 1 2 d S . .
O7 O 1.0711(4) 0.6221(3) 0.2930(3) 0.0408(14) Uani 1 1 d . . .
O8 O 0.8380(4) 0.6248(2) 0.5543(3) 0.0291(10) Uani 1 1 d . . .
O9 O 0.4474(3) 0.5677(2) 0.1030(3) 0.0202(8) Uani 1 1 d . . .
O10 O 0.8590(4) 0.5642(2) 0.0752(3) 0.0271(10) Uani 1 1 d . . .
O11 O 0.5090(4) 0.5681(2) 0.4416(3) 0.0245(9) Uani 1 1 d . . .
O12 O 0.7124(4) 0.4922(2) 0.2713(3) 0.0295(10) Uani 1 1 d . . .
O13 O 0.4222(3) 0.69006(18) 0.1888(2) 0.0140(7) Uani 1 1 d . . .
O14 O 0.4694(3) 0.69153(18) 0.3661(2) 0.0157(7) Uani 1 1 d . . .
O15 O 0.5426(3) 0.68890(18) 0.0707(2) 0.0143(7) Uani 1 1 d . . .
O16 O 0.7563(3) 0.69135(18) 0.0573(2) 0.0146(7) Uani 1 1 d . . .
O17 O 0.9249(3) 0.6837(2) 0.1665(2) 0.0178(8) Uani 1 1 d . . .
O18 O 0.9907(5) 0.7500 0.3070(4) 0.0212(12) Uani 1 2 d S . .
O19 O 0.9145(3) 0.6637(2) 0.3973(3) 0.0205(8) Uani 1 1 d . . .
O20 O 0.8341(5) 0.7500 0.4804(4) 0.0206(12) Uani 1 2 d S . .
O21 O 0.6417(3) 0.6845(2) 0.4696(3) 0.0196(8) Uani 1 1 d . . .
O22 O 0.8432(4) 0.6045(2) 0.2513(3) 0.0221(9) Uani 1 1 d . . .
O23 O 0.7200(3) 0.6003(2) 0.3868(3) 0.0192(8) Uani 1 1 d . . .
O24 O 0.5550(3) 0.59938(19) 0.2720(3) 0.0189(8) Uani 1 1 d . . .
O25 O 0.6687(3) 0.59914(19) 0.1552(3) 0.0176(8) Uani 1 1 d . . .
O30 O 0.6948(10) 0.7500 0.2667(8) 0.073(3) Uani 1 2 d S . .
O31 O 1.0237(5) 0.4979(3) 0.1812(4) 0.0499(15) Uani 1 1 d . . .
O32 O 0.8193(5) 0.5649(4) -0.0982(4) 0.0536(17) Uani 1 1 d . . .
O33 O 0.8973(8) 0.4149(5) 0.2685(6) 0.080(2) Uiso 1 1 d . . .
O34 O 0.3711(14) 0.7500 -0.1742(11) 0.103(5) Uiso 1 2 d S . .
O35 O 0.8881(10) 0.6835(6) -0.1436(8) 0.115(4) Uiso 1 1 d . . .
N1 N 0.1570(4) 0.6755(3) 0.1167(3) 0.0236(10) Uani 1 1 d . . .
N2 N 0.1279(5) 0.6723(4) -0.0614(4) 0.0428(17) Uani 1 1 d . . .
N3 N 0.4247(5) 0.4233(3) 0.0599(4) 0.0256(11) Uani 1 1 d . . .
N4 N 0.6420(5) 0.4670(3) 0.0738(4) 0.0254(11) Uani 1 1 d . . .
N5 N 0.3416(5) 0.5462(3) 0.5585(4) 0.0266(11) Uani 1 1 d . . .
N6 N 0.2596(5) 0.6514(3) 0.4649(5) 0.0360(14) Uani 1 1 d . . .
N7 N 0.3363(5) 0.4612(3) 0.3968(4) 0.0340(14) Uani 1 1 d . . .
N8 N 0.2903(5) 0.5738(3) 0.3054(4) 0.0379(16) Uani 1 1 d . . .
N9 N 0.1072(5) 0.5196(3) 0.4270(4) 0.0328(13) Uani 1 1 d . . .
C1 C 0.1758(6) 0.6156(4) 0.0720(6) 0.0410(19) Uani 1 1 d . . .
C2 C 0.1059(7) 0.6151(4) -0.0122(7) 0.049(2) Uani 1 1 d . . .
C3 C 0.5042(6) 0.4034(3) 0.1331(5) 0.0315(14) Uani 1 1 d . . .
C4 C 0.6181(6) 0.4027(3) 0.1057(5) 0.0298(14) Uani 1 1 d . . .
C5 C 0.3654(6) 0.6110(3) 0.5937(5) 0.0341(15) Uani 1 1 d . . .
C6 C 0.2725(6) 0.6547(3) 0.5588(6) 0.0399(19) Uani 1 1 d . . .
C7 C 0.3736(8) 0.4700(5) 0.3136(6) 0.048(2) Uani 1 1 d . . .
C8 C 0.3059(8) 0.5152(5) 0.2617(5) 0.049(2) Uani 1 1 d . . .
C9 C 0.0562(5) 0.5156(3) 0.5070(4) 0.0273(13) Uani 1 1 d . . .
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'
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 Zn1 N1 95.2(3) 4_575 . ?
N1 Zn1 N2 176.9(3) 4_575 . ?
N1 Zn1 N2 82.4(3) . . ?
N1 Zn1 N2 82.4(3) 4_575 4_575 ?
N1 Zn1 N2 176.9(3) . 4_575 ?
N2 Zn1 N2 99.9(5) . 4_575 ?
N1 Zn1 O2 90.90(18) 4_575 . ?
N1 Zn1 O2 90.90(18) . . ?
N2 Zn1 O2 91.2(2) . . ?
N2 Zn1 O2 91.2(2) 4_575 . ?
N1 Zn1 O4 92.76(18) 4_575 1_455 ?
N1 Zn1 O4 92.76(18) . 1_455 ?
N2 Zn1 O4 85.3(2) . 1_455 ?
N2 Zn1 O4 85.3(2) 4_575 1_455 ?
O2 Zn1 O4 174.6(2) . 1_455 ?
N4 Zn2 N4 180.0(4) 3_665 . ?
N4 Zn2 N3 83.4(2) 3_665 3_665 ?
N4 Zn2 N3 96.6(2) . 3_665 ?
N4 Zn2 N3 96.6(2) 3_665 . ?
N4 Zn2 N3 83.4(2) . . ?
N3 Zn2 N3 180.0(3) 3_665 . ?
N4 Zn2 O9 95.75(18) 3_665 3_665 ?
N4 Zn2 O9 84.25(18) . 3_665 ?
N3 Zn2 O9 88.38(17) 3_665 3_665 ?
N3 Zn2 O9 91.62(17) . 3_665 ?
N4 Zn2 O9 84.25(18) 3_665 . ?
N4 Zn2 O9 95.75(18) . . ?
N3 Zn2 O9 91.62(17) 3_665 . ?
N3 Zn2 O9 88.38(17) . . ?
O9 Zn2 O9 180.00(16) 3_665 . ?
N5 Zn3 N8 146.5(2) . . ?
N5 Zn3 N9 107.7(2) . . ?
N8 Zn3 N9 105.7(3) . . ?
N5 Zn3 N6 81.7(2) . . ?
N8 Zn3 N6 92.6(3) . . ?
N9 Zn3 N6 104.2(2) . . ?
N5 Zn3 N7 93.2(2) . . ?
N8 Zn3 N7 81.2(2) . . ?
N9 Zn3 N7 95.5(3) . . ?
N6 Zn3 N7 160.3(2) . . ?
O1 V1 O13 106.9(2) . . ?
O1 V1 O13 106.9(2) . 4_575 ?
O13 V1 O13 80.1(2) . 4_575 ?
O1 V1 O14 107.4(2) . 4_575 ?
O13 V1 O14 145.67(17) . 4_575 ?
O13 V1 O14 91.14(16) 4_575 4_575 ?
O1 V1 O14 107.4(2) . . ?
O13 V1 O14 91.14(16) . . ?
O13 V1 O14 145.67(17) 4_575 . ?
O14 V1 O14 77.6(2) 4_575 . ?
O1 V1 V2 110.2(2) . . ?
O13 V1 V2 40.09(11) . . ?
O13 V1 V2 40.09(11) 4_575 . ?
O14 V1 V2 124.89(12) 4_575 . ?
O14 V1 V2 124.89(12) . . ?
O1 V1 V6 112.6(2) . . ?
O13 V1 V6 122.80(12) . . ?
O13 V1 V6 122.80(12) 4_575 . ?
O14 V1 V6 38.79(12) 4_575 . ?
O14 V1 V6 38.79(12) . . ?
V2 V1 V6 137.13(6) . . ?
O2 V2 O15 111.84(19) . 4_575 ?
O2 V2 O15 111.84(19) . . ?
O15 V2 O15 83.4(2) 4_575 . ?
O2 V2 O13 111.79(19) . 4_575 ?
O15 V2 O13 81.96(16) 4_575 4_575 ?
O15 V2 O13 136.34(17) . 4_575 ?
O2 V2 O13 111.79(19) . . ?
O15 V2 O13 136.34(17) 4_575 . ?
O15 V2 O13 81.96(16) . . ?
O13 V2 O13 80.9(2) 4_575 . ?
O2 V2 V3 114.3(2) . . ?
O15 V2 V3 42.02(11) 4_575 . ?
O15 V2 V3 42.02(11) . . ?
O13 V2 V3 116.91(12) 4_575 . ?
O13 V2 V3 116.91(12) . . ?
O2 V2 V9 115.76(3) . 4_575 ?
O15 V2 V9 40.98(11) 4_575 4_575 ?
O15 V2 V9 116.34(12) . 4_575 ?
O13 V2 V9 41.26(11) 4_575 4_575 ?
O13 V2 V9 114.62(12) . 4_575 ?
V3 V2 V9 80.19(3) . 4_575 ?
O2 V2 V9 115.76(3) . . ?
O15 V2 V9 116.34(12) 4_575 . ?
O15 V2 V9 40.98(11) . . ?
O13 V2 V9 114.62(12) 4_575 . ?
O13 V2 V9 41.26(11) . . ?
V3 V2 V9 80.19(3) . . ?
V9 V2 V9 128.46(6) 4_575 . ?
O2 V2 V1 117.1(2) . . ?
O15 V2 V1 114.01(12) 4_575 . ?
O15 V2 V1 114.01(12) . . ?
O13 V2 V1 40.49(11) 4_575 . ?
O13 V2 V1 40.49(11) . . ?
V3 V2 V1 128.61(6) . . ?
V9 V2 V1 78.10(3) 4_575 . ?
V9 V2 V1 78.10(3) . . ?
O3 V3 O15 107.2(2) . . ?
O3 V3 O15 107.2(2) . 4_575 ?
O15 V3 O15 83.7(2) . 4_575 ?
O3 V3 O16 107.7(2) . 4_575 ?
O15 V3 O16 145.09(17) . 4_575 ?
O15 V3 O16 88.22(16) 4_575 4_575 ?
O3 V3 O16 107.7(2) . . ?
O15 V3 O16 88.22(16) . . ?
O15 V3 O16 145.09(17) 4_575 . ?
O16 V3 O16 79.3(2) 4_575 . ?
O3 V3 V2 107.7(2) . . ?
O15 V3 V2 42.15(12) . . ?
O15 V3 V2 42.15(12) 4_575 . ?
O16 V3 V2 125.57(12) 4_575 . ?
O16 V3 V2 125.57(12) . . ?
O3 V3 V4 112.5(2) . . ?
O15 V3 V4 121.25(12) . . ?
O15 V3 V4 121.25(12) 4_575 . ?
O16 V3 V4 39.63(11) 4_575 . ?
O16 V3 V4 39.63(11) . . ?
V2 V3 V4 139.75(6) . . ?
O4 V4 O17 108.13(18) . 4_575 ?
O4 V4 O17 108.13(18) . . ?
O17 V4 O17 92.0(3) 4_575 . ?
O4 V4 O16 111.47(19) . . ?
O17 V4 O16 139.91(17) 4_575 . ?
O17 V4 O16 81.72(17) . . ?
O4 V4 O16 111.47(19) . 4_575 ?
O17 V4 O16 81.72(17) 4_575 4_575 ?
O17 V4 O16 139.91(17) . 4_575 ?
O16 V4 O16 78.4(2) . 4_575 ?
O4 V4 V10 112.99(3) . . ?
O17 V4 V10 124.69(13) 4_575 . ?
O17 V4 V10 41.12(13) . . ?
O16 V4 V10 40.86(11) . . ?
O16 V4 V10 113.94(12) 4_575 . ?
O4 V4 V10 112.99(3) . 4_575 ?
O17 V4 V10 41.12(13) 4_575 4_575 ?
O17 V4 V10 124.69(13) . 4_575 ?
O16 V4 V10 113.94(12) . 4_575 ?
O16 V4 V10 40.86(11) 4_575 4_575 ?
V10 V4 V10 133.67(6) . 4_575 ?
O4 V4 V3 117.5(2) . . ?
O17 V4 V3 114.04(13) 4_575 . ?
O17 V4 V3 114.04(13) . . ?
O16 V4 V3 39.20(11) . . ?
O16 V4 V3 39.20(11) 4_575 . ?
V10 V4 V3 77.16(3) . . ?
V10 V4 V3 77.16(3) 4_575 . ?
O5 V5 O20 111.6(3) . . ?
O5 V5 O18 113.1(3) . . ?
O20 V5 O18 135.2(3) . . ?
O5 V5 O19 110.63(13) . . ?
O20 V5 O19 81.56(14) . . ?
O18 V5 O19 83.02(14) . . ?
O5 V5 O19 110.63(13) . 4_575 ?
O20 V5 O19 81.56(14) . 4_575 ?
O18 V5 O19 83.02(14) . 4_575 ?
O19 V5 O19 138.7(3) . 4_575 ?
O5 V5 V7 115.71(17) . . ?
O20 V5 V7 115.10(13) . . ?
O18 V5 V7 41.57(5) . . ?
O19 V5 V7 41.78(12) . . ?
O19 V5 V7 117.58(13) 4_575 . ?
O5 V5 V7 115.71(17) . 4_575 ?
O20 V5 V7 115.10(13) . 4_575 ?
O18 V5 V7 41.57(5) . 4_575 ?
O19 V5 V7 117.58(13) . 4_575 ?
O19 V5 V7 41.78(12) 4_575 4_575 ?
V7 V5 V7 80.46(5) . 4_575 ?
O5 V5 V8 114.19(18) . . ?
O20 V5 V8 40.96(5) . . ?
O18 V5 V8 115.89(13) . . ?
O19 V5 V8 40.96(12) . . ?
O19 V5 V8 116.28(14) 4_575 . ?
V7 V5 V8 79.46(3) . . ?
V7 V5 V8 130.09(5) 4_575 . ?
O5 V5 V8 114.19(18) . 4_575 ?
O20 V5 V8 40.96(5) . 4_575 ?
O18 V5 V8 115.89(13) . 4_575 ?
O19 V5 V8 116.28(14) . 4_575 ?
O19 V5 V8 40.96(12) 4_575 4_575 ?
V7 V5 V8 130.09(5) . 4_575 ?
V7 V5 V8 79.46(3) 4_575 4_575 ?
V8 V5 V8 79.61(5) . 4_575 ?
O6 V6 O21 108.0(2) . 4_575 ?
O6 V6 O21 108.0(2) . . ?
O21 V6 O21 94.2(3) 4_575 . ?
O6 V6 O14 107.6(2) . . ?
O21 V6 O14 143.47(19) 4_575 . ?
O21 V6 O14 82.83(17) . . ?
O6 V6 O14 107.6(2) . 4_575 ?
O21 V6 O14 82.83(17) 4_575 4_575 ?
O21 V6 O14 143.47(19) . 4_575 ?
O14 V6 O14 78.6(2) . 4_575 ?
O6 V6 V11 111.40(4) . . ?
O21 V6 V11 128.12(14) 4_575 . ?
O21 V6 V11 42.18(13) . . ?
O14 V6 V11 40.79(11) . . ?
O14 V6 V11 114.72(12) 4_575 . ?
O6 V6 V11 111.40(4) . 4_575 ?
O21 V6 V11 42.18(13) 4_575 4_575 ?
O21 V6 V11 128.12(14) . 4_575 ?
O14 V6 V11 114.72(12) . 4_575 ?
O14 V6 V11 40.79(11) 4_575 4_575 ?
V11 V6 V11 136.03(6) . 4_575 ?
O6 V6 V1 113.0(2) . . ?
O21 V6 V1 115.98(13) 4_575 . ?
O21 V6 V1 115.98(13) . . ?
O14 V6 V1 39.32(11) . . ?
O14 V6 V1 39.32(11) 4_575 . ?
V11 V6 V1 77.32(3) . . ?
V11 V6 V1 77.32(3) 4_575 . ?
O7 V7 O22 107.2(3) . . ?
O7 V7 O18 109.6(3) . . ?
O22 V7 O18 142.9(2) . . ?
O7 V7 O19 107.0(2) . . ?
O22 V7 O19 89.07(19) . . ?
O18 V7 O19 84.3(2) . . ?
O7 V7 O17 105.3(2) . . ?
O22 V7 O17 78.69(18) . . ?
O18 V7 O17 87.6(2) . . ?
O19 V7 O17 147.55(18) . . ?
O7 V7 V5 110.9(2) . . ?
O22 V7 V5 124.80(13) . . ?
O18 V7 V5 42.22(18) . . ?
O19 V7 V5 42.44(14) . . ?
O17 V7 V5 125.25(13) . . ?
O7 V7 V10 109.6(2) . . ?
O22 V7 V10 39.18(12) . . ?
O18 V7 V10 120.51(17) . . ?
O19 V7 V10 123.17(14) . . ?
O17 V7 V10 39.57(13) . . ?
V5 V7 V10 139.57(5) . . ?
O8 V8 O19 108.3(2) . . ?
O8 V8 O20 107.4(3) . . ?
O19 V8 O20 81.1(2) . . ?
O8 V8 O23 109.1(2) . . ?
O19 V8 O23 89.99(18) . . ?
O20 V8 O23 143.4(2) . . ?
O8 V8 O21 107.1(2) . . ?
O19 V8 O21 144.54(18) . . ?
O20 V8 O21 88.6(2) . . ?
O23 V8 O21 78.26(17) . . ?
O8 V8 V5 109.60(18) . . ?
O19 V8 V5 40.97(13) . . ?
O20 V8 V5 40.54(17) . . ?
O23 V8 V5 124.91(13) . . ?
O21 V8 V5 123.89(13) . . ?
O8 V8 V11 113.48(18) . . ?
O19 V8 V11 121.43(13) . . ?
O20 V8 V11 120.58(17) . . ?
O23 V8 V11 38.70(12) . . ?
O21 V8 V11 39.56(13) . . ?
V5 V8 V11 136.90(5) . . ?
O9 V9 O25 104.94(19) . . ?
O9 V9 O15 107.02(19) . . ?
O25 V9 O15 88.19(16) . . ?
O9 V9 O24 108.6(2) . . ?
O25 V9 O24 79.00(17) . . ?
O15 V9 O24 144.12(17) . . ?
O9 V9 O13 110.22(19) . . ?
O25 V9 O13 144.84(17) . . ?
O15 V9 O13 81.66(16) . . ?
O24 V9 O13 89.78(17) . . ?
O9 V9 V2 111.23(16) . . ?
O25 V9 V2 123.50(12) . . ?
O15 V9 V2 40.77(12) . . ?
O24 V9 V2 124.81(13) . . ?
O13 V9 V2 41.17(11) . . ?
O9 V9 V12 110.26(16) . . ?
O25 V9 V12 39.25(12) . . ?
O15 V9 V12 121.17(12) . . ?
O24 V9 V12 39.81(12) . . ?
O13 V9 V12 123.13(12) . . ?
V2 V9 V12 138.38(4) . . ?
O10 V10 O25 109.1(2) . . ?
O10 V10 O16 111.1(2) . . ?
O25 V10 O16 92.54(17) . . ?
O10 V10 O22 110.3(2) . . ?
O25 V10 O22 80.01(18) . . ?
O16 V10 O22 138.08(18) . . ?
O10 V10 O17 110.8(2) . . ?
O25 V10 O17 138.96(17) . . ?
O16 V10 O17 81.81(16) . . ?
O22 V10 O17 77.78(18) . . ?
O10 V10 V4 114.63(17) . . ?
O25 V10 V4 124.77(13) . . ?
O16 V10 V4 41.23(12) . . ?
O22 V10 V4 112.71(14) . . ?
O17 V10 V4 40.84(12) . . ?
O10 V10 V12 110.81(17) . . ?
O25 V10 V12 40.47(12) . . ?
O16 V10 V12 125.13(12) . . ?
O22 V10 V12 40.13(13) . . ?
O17 V10 V12 113.71(12) . . ?
V4 V10 V12 133.82(4) . . ?
O10 V10 V7 115.20(18) . . ?
O25 V10 V7 112.41(13) . . ?
O16 V10 V7 114.23(12) . . ?
O22 V10 V7 38.32(14) . . ?
O17 V10 V7 39.51(12) . . ?
V4 V10 V7 77.36(4) . . ?
V12 V10 V7 76.45(4) . . ?
O11 V11 O14 108.2(2) . . ?
O11 V11 O24 109.3(2) . . ?
O14 V11 O24 91.53(17) . . ?
O11 V11 O23 110.3(2) . . ?
O14 V11 O23 140.70(18) . . ?
O24 V11 O23 83.05(18) . . ?
O11 V11 O21 110.0(2) . . ?
O14 V11 O21 81.38(17) . . ?
O24 V11 O21 140.37(18) . . ?
O23 V11 O21 78.60(18) . . ?
O11 V11 V6 113.07(17) . . ?
O14 V11 V6 41.56(12) . . ?
O24 V11 V6 124.11(13) . . ?
O23 V11 V6 113.15(14) . . ?
O21 V11 V6 39.95(12) . . ?
O11 V11 V12 113.46(16) . . ?
O14 V11 V12 125.14(12) . . ?
O24 V11 V12 42.08(12) . . ?
O23 V11 V12 41.20(13) . . ?
O21 V11 V12 114.19(13) . . ?
V6 V11 V12 132.87(5) . . ?
O11 V11 V8 116.25(17) . . ?
O14 V11 V8 114.42(13) . . ?
O24 V11 V8 114.36(13) . . ?
O23 V11 V8 38.62(13) . . ?
O21 V11 V8 39.98(12) . . ?
V6 V11 V8 76.74(4) . . ?
V12 V11 V8 76.62(4) . . ?
O12 V12 O23 109.7(2) . . ?
O12 V12 O22 109.1(2) . . ?
O23 V12 O22 92.82(18) . . ?
O12 V12 O25 108.9(2) . . ?
O23 V12 O25 141.01(18) . . ?
O22 V12 O25 79.84(17) . . ?
O12 V12 O24 111.9(2) . . ?
O23 V12 O24 82.31(17) . . ?
O22 V12 O24 137.95(18) . . ?
O25 V12 O24 78.42(17) . . ?
O12 V12 V11 114.74(17) . . ?
O23 V12 V11 41.62(12) . . ?
O22 V12 V11 124.57(14) . . ?
O25 V12 V11 114.20(12) . . ?
O24 V12 V11 40.92(12) . . ?
O12 V12 V10 109.80(16) . . ?
O23 V12 V10 126.63(13) . . ?
O22 V12 V10 40.48(13) . . ?
O25 V12 V10 39.95(12) . . ?
O24 V12 V10 113.69(12) . . ?
V11 V12 V10 134.76(4) . . ?
O12 V12 V9 115.0(2) . . ?
O23 V12 V9 115.68(12) . . ?
O22 V12 V9 112.35(13) . . ?
O25 V12 V9 39.07(12) . . ?
O24 V12 V9 39.40(12) . . ?
V11 V12 V9 77.81(3) . . ?
V10 V12 V9 76.76(3) . . ?
V2 O2 Zn1 137.2(3) . . ?
V4 O4 Zn1 129.5(3) . 1_655 ?
V9 O9 Zn2 127.9(2) . . ?
V2 O13 V9 97.57(17) . . ?
V2 O13 V1 99.43(17) . . ?
V9 O13 V1 144.4(2) . . ?
V11 O14 V6 97.65(18) . . ?
V11 O14 V1 146.1(2) . . ?
V6 O14 V1 101.89(18) . . ?
V3 O15 V2 95.82(17) . . ?
V3 O15 V9 149.4(2) . . ?
V2 O15 V9 98.25(17) . . ?
V3 O16 V10 145.9(2) . . ?
V3 O16 V4 101.17(18) . . ?
V10 O16 V4 97.91(17) . . ?
V4 O17 V7 145.7(2) . . ?
V4 O17 V10 98.04(18) . . ?
V7 O17 V10 100.92(18) . . ?
V7 O18 V7 150.8(3) 4_575 . ?
V7 O18 V5 96.21(18) 4_575 . ?
V7 O18 V5 96.21(18) . . ?
V7 O19 V8 147.5(2) . . ?
V7 O19 V5 95.78(19) . . ?
V8 O19 V5 98.1(2) . . ?
V5 O20 V8 98.50(18) . . ?
V5 O20 V8 98.50(18) . 4_575 ?
V8 O20 V8 149.9(3) . 4_575 ?
V6 O21 V11 97.87(18) . . ?
V6 O21 V8 145.1(2) . . ?
V11 O21 V8 100.45(19) . . ?
V7 O22 V12 147.7(2) . . ?
V7 O22 V10 102.5(2) . . ?
V12 O22 V10 99.4(2) . . ?
V12 O23 V8 144.3(2) . . ?
V12 O23 V11 97.18(19) . . ?
V8 O23 V11 102.69(19) . . ?
V11 O24 V9 148.4(2) . . ?
V11 O24 V12 97.01(19) . . ?
V9 O24 V12 100.79(18) . . ?
V10 O25 V9 147.1(2) . . ?
V10 O25 V12 99.58(19) . . ?
V9 O25 V12 101.67(18) . . ?
C1 N1 Zn1 107.8(5) . . ?
C2 N2 Zn1 106.8(5) . . ?
C3 N3 Zn2 106.0(4) . . ?
C4 N4 Zn2 107.5(4) . . ?
C5 N5 Zn3 110.0(4) . . ?
C6 N6 Zn3 106.8(4) . . ?
C7 N7 Zn3 107.0(5) . . ?
C8 N8 Zn3 108.5(5) . . ?
C9 N9 Zn3 119.5(5) . . ?
N1 C1 C2 108.9(6) . . ?
N2 C2 C1 110.0(6) . . ?
N3 C3 C4 109.0(5) . . ?
N4 C4 C3 108.6(5) . . ?
N5 C5 C6 108.2(6) . . ?
N6 C6 C5 108.5(6) . . ?
C8 C7 N7 111.5(8) . . ?
N8 C8 C7 113.0(7) . . ?
N9 C9 C9 112.2(7) . 3_566 ?
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 N1 2.116(5) 4_575 ?
Zn1 N1 2.116(5) . ?
Zn1 N2 2.131(6) . ?
Zn1 N2 2.131(6) 4_575 ?
Zn1 O2 2.252(6) . ?
Zn1 O4 2.281(6) 1_455 ?
Zn2 N4 2.100(6) 3_665 ?
Zn2 N4 2.100(6) . ?
Zn2 N3 2.142(5) 3_665 ?
Zn2 N3 2.142(5) . ?
Zn2 O9 2.319(4) 3_665 ?
Zn2 O9 2.319(4) . ?
Zn3 N5 2.098(6) . ?
Zn3 N8 2.101(6) . ?
Zn3 N9 2.107(6) . ?
Zn3 N6 2.149(7) . ?
Zn3 N7 2.187(6) . ?
V1 O1 1.603(6) . ?
V1 O13 1.955(4) . ?
V1 O13 1.955(4) 4_575 ?
V1 O14 1.959(4) 4_575 ?
V1 O14 1.959(4) . ?
V1 V2 2.9703(17) . ?
V1 V6 3.0246(19) . ?
V2 O2 1.639(6) . ?
V2 O15 1.927(4) 4_575 ?
V2 O15 1.927(4) . ?
V2 O13 1.939(4) 4_575 ?
V2 O13 1.939(4) . ?
V2 V3 2.8558(18) . ?
V2 V9 2.9195(11) 4_575 ?
V2 V9 2.9195(11) . ?
V3 O3 1.619(6) . ?
V3 O15 1.922(4) . ?
V3 O15 1.922(4) 4_575 ?
V3 O16 1.930(4) 4_575 ?
V3 O16 1.930(4) . ?
V3 V4 2.9952(18) . ?
V4 O4 1.640(6) . ?
V4 O17 1.933(4) 4_575 ?
V4 O17 1.933(4) . ?
V4 O16 1.947(4) . ?
V4 O16 1.947(4) 4_575 ?
V4 V10 2.9267(11) . ?
V4 V10 2.9267(11) 4_575 ?
V5 O5 1.619(6) . ?
V5 O20 1.919(6) . ?
V5 O18 1.928(6) . ?
V5 O19 1.934(4) . ?
V5 O19 1.934(4) 4_575 ?
V5 V7 2.8517(15) . ?
V5 V7 2.8517(15) 4_575 ?
V5 V8 2.9206(15) . ?
V5 V8 2.9206(15) 4_575 ?
V6 O6 1.608(6) . ?
V6 O21 1.875(4) 4_575 ?
V6 O21 1.875(4) . ?
V6 O14 1.936(4) . ?
V6 O14 1.936(4) 4_575 ?
V6 V11 2.8927(11) . ?
V6 V11 2.8927(11) 4_575 ?
V7 O7 1.615(5) . ?
V7 O22 1.903(5) . ?
V7 O18 1.9033(19) . ?
V7 O19 1.910(4) . ?
V7 O17 1.941(4) . ?
V7 V10 2.9962(14) . ?
V8 O8 1.623(4) . ?
V8 O19 1.934(4) . ?
V8 O20 1.9359(19) . ?
V8 O23 1.937(4) . ?
V8 O21 1.978(4) . ?
V8 V11 3.0274(14) . ?
V9 O9 1.636(4) . ?
V9 O25 1.932(4) . ?
V9 O15 1.935(4) . ?
V9 O24 1.940(4) . ?
V9 O13 1.942(4) . ?
V9 V12 3.0020(14) . ?
V10 O10 1.642(4) . ?
V10 O25 1.919(4) . ?
V10 O16 1.933(4) . ?
V10 O22 1.939(4) . ?
V10 O17 1.944(4) . ?
V10 V12 2.9468(13) . ?
V11 O11 1.627(4) . ?
V11 O14 1.907(4) . ?
V11 O24 1.912(4) . ?
V11 O23 1.940(4) . ?
V11 O21 1.961(4) . ?
V11 V12 2.8981(13) . ?
V12 O12 1.629(5) . ?
V12 O23 1.924(4) . ?
V12 O22 1.925(4) . ?
V12 O25 1.940(4) . ?
V12 O24 1.957(4) . ?
O4 Zn1 2.281(6) 1_655 ?
O18 V7 1.9033(19) 4_575 ?
O20 V8 1.9359(18) 4_575 ?
N1 C1 1.476(9) . ?
N2 C2 1.475(13) . ?
N3 C3 1.481(10) . ?
N4 C4 1.483(9) . ?
N5 C5 1.485(9) . ?
N6 C6 1.477(12) . ?
N7 C7 1.462(10) . ?
N8 C8 1.436(12) . ?
N9 C9 1.489(9) . ?
C1 C2 1.494(13) . ?
C3 C4 1.526(10) . ?
C5 C6 1.519(11) . ?
C7 C8 1.449(13) . ?
C9 C9 1.526(12) 3_566 ?
