#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:43:09 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230236 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/71/7057101.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_7057101
loop_
_publ_author_name
'Huang, Bo'
'Wang, Nan'
'Yang, Kang'
'Ke, Degang'
'Fang, Yajun'
'Hu, Xunliang'
'Wu, Baolin'
'Xiao, Zicheng'
'Wu, Pingfan'
'Wei, Yongge'
_publ_section_title
;
 Stepwise syntheses and supramolecular assemblies of a series of
 polyoxovanadate hybrids with various architectures
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5853
_journal_paper_doi               10.1039/C7NJ04727D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C32 H36 N2 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C64 H108 N4 O25 V6'
_chemical_formula_weight         1639.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-02 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.950(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5838(19)
_cell_length_b                   17.309(2)
_cell_length_c                   16.326(2)
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18.907
_cell_measurement_theta_min      2.353
_cell_volume                     3755.4(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28892
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.273
_diffrn_reflns_theta_min         1.735
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0695 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.9277.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7549
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0944P)²+2.9775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.2132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3733
_reflns_number_total             7549
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj04727d2.cif
_cod_data_source_block           lbxba
_cod_depositor_comments
'Adding full bibliography for 7057098--7057101.cif.'
_cod_original_cell_volume        3755.4(9)
_cod_database_code               7057101
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1AA-C2AA
 1.33 with sigma of 0.01
3. Rigid bond restraints
 C54, C53, C52, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1AA \\sim C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B), C14(H14A,H14B), C51(H51A,H51B),
 C41(H41A,H41B), C31(H31A,H31B), C21(H21A,H21B), C22(H22A,H22B), C52(H52A,H52B),
  C42(H42A,H42B), C23(H23A,H23B), C43(H43A,H43B), C32(H32A,H32B), C33(H33A,
 H33B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 N13(H13), C11(H11), C8(H8), C9(H9), C10(H10), C1AA(H1AA)
5.c X=CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C24(H24A,H24B,H24C), C54(H54A,H54B,
 H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
V2 V 0.50308(7) -0.10288(6) 0.91613(6) 0.0500(3) Uani 1 1 d . . .
V3 V 0.38110(7) 0.06246(6) 0.91076(6) 0.0508(3) Uani 1 1 d . . .
O1 O 0.5000 0.0000 1.0000 0.0379(11) Uani 1 2 d S T P
O2 O 0.6072(3) -0.0302(2) 0.8823(2) 0.0439(9) Uani 1 1 d . . .
O3 O 0.5052(3) 0.1020(2) 0.8785(2) 0.0471(9) Uani 1 1 d . . .
O4 O 0.4074(3) -0.0318(2) 0.8436(2) 0.0494(9) Uani 1 1 d . . .
O5 O 0.3003(2) -0.0008(2) 0.9599(2) 0.0504(10) Uani 1 1 d . . .
O6 O 0.6034(3) -0.1317(2) 1.0053(2) 0.0529(10) Uani 1 1 d . . .
O7 O 0.4023(3) -0.1331(2) 0.9649(2) 0.0540(10) Uani 1 1 d . . .
C4 C 0.5085(4) 0.1051(4) 0.7909(3) 0.0540(15) Uani 1 1 d . . .
H4A H 0.5679 0.1335 0.7842 0.065 Uiso 1 1 calc R . .
H4B H 0.4499 0.1329 0.7610 0.065 Uiso 1 1 calc R . .
O8 O 0.7102(3) 0.1029(2) 0.9201(2) 0.0613(11) Uani 1 1 d . . .
O9 O 0.5063(3) -0.1678(2) 0.8464(3) 0.0675(12) Uani 1 1 d . . .
O10 O 0.3028(3) 0.1029(3) 0.8368(3) 0.0668(12) Uani 1 1 d . . .
O11 O 0.4245(3) 0.0665(3) 0.6143(2) 0.0686(12) Uani 1 1 d . . .
O12 O 0.4968(4) 0.0861(3) 0.5043(3) 0.0812(15) Uani 1 1 d . . .
C3 C 0.6023(5) -0.0178(4) 0.7966(4) 0.0522(15) Uani 1 1 d . . .
O13 O 0.4317(4) 0.2349(3) 0.5821(3) 0.0903(16) Uani 1 1 d . . .
C2 C 0.4154(5) -0.0199(4) 0.7586(3) 0.0578(16) Uani 1 1 d . . .
H2A H 0.3566 0.0079 0.7292 0.069 Uiso 1 1 calc R . .
H2B H 0.4170 -0.0696 0.7314 0.069 Uiso 1 1 calc R . .
N13 N 0.2891(4) 0.2938(3) 0.5985(4) 0.0761(16) Uani 1 1 d . . .
H13 H 0.2245 0.2917 0.5886 0.091 Uiso 1 1 calc R . .
C7 C 0.3236(5) 0.1138(4) 0.4918(4) 0.0584(16) Uani 1 1 d . . .
C12 C 0.2793(5) 0.1839(4) 0.5058(4) 0.0609(17) Uani 1 1 d . . .
C5 C 0.5187(5) 0.0351(4) 0.6616(3) 0.0637(18) Uani 1 1 d . . .
H5A H 0.5738 0.0696 0.6576 0.076 Uiso 1 1 calc R . .
H5B H 0.5319 -0.0147 0.6387 0.076 Uiso 1 1 calc R . .
C6 C 0.4235(5) 0.0901(4) 0.5362(4) 0.0659(18) Uani 1 1 d . . .
C1 C 0.3391(5) 0.2400(4) 0.5651(4) 0.0657(18) Uani 1 1 d . . .
C0AA C 0.5107(4) 0.0260(4) 0.7528(3) 0.0521(15) Uani 1 1 d . . .
C11 C 0.1803(5) 0.2003(4) 0.4615(5) 0.074(2) Uani 1 1 d . . .
H11 H 0.1496 0.2467 0.4706 0.089 Uiso 1 1 calc R . .
C8 C 0.2707(6) 0.0625(5) 0.4343(4) 0.075(2) Uani 1 1 d . . .
H8 H 0.3010 0.0163 0.4240 0.089 Uiso 1 1 calc R . .
C14 C 0.3396(7) 0.3561(5) 0.6509(6) 0.100(3) Uani 1 1 d . . .
H14A H 0.4046 0.3643 0.6366 0.120 Uiso 1 1 calc R . .
H14B H 0.3007 0.4029 0.6363 0.120 Uiso 1 1 calc R . .
C9 C 0.1726(7) 0.0783(5) 0.3911(5) 0.092(2) Uani 1 1 d . . .
H9 H 0.1367 0.0428 0.3536 0.110 Uiso 1 1 calc R . .
C10 C 0.1308(6) 0.1483(5) 0.4060(5) 0.089(2) Uani 1 1 d . . .
H10 H 0.0662 0.1602 0.3768 0.106 Uiso 1 1 calc R . .
N2 N 0.0559(3) 0.1916(3) 0.8782(3) 0.0524(12) Uani 1 1 d . . .
C51 C -0.0577(4) 0.1862(4) 0.8600(4) 0.0632(17) Uani 1 1 d . U .
H51A H -0.0765 0.1359 0.8354 0.076 Uiso 1 1 calc R . .
H51B H -0.0795 0.1882 0.9129 0.076 Uiso 1 1 calc R . .
C41 C 0.0984(5) 0.1226(4) 0.9322(4) 0.0651(17) Uani 1 1 d . . .
H41A H 0.0748 0.0757 0.9019 0.078 Uiso 1 1 calc R . .
H41B H 0.1712 0.1236 0.9398 0.078 Uiso 1 1 calc R . .
C31 C 0.0891(5) 0.2679(4) 0.9204(4) 0.0719(19) Uani 1 1 d . . .
H31A H 0.0541 0.2754 0.9658 0.086 Uiso 1 1 calc R . .
H31B H 0.0685 0.3091 0.8802 0.086 Uiso 1 1 calc R . .
C21 C 0.0941(5) 0.1880(4) 0.7977(4) 0.0610(17) Uani 1 1 d . . .
H21A H 0.0704 0.2338 0.7653 0.073 Uiso 1 1 calc R . .
H21B H 0.1669 0.1910 0.8119 0.073 Uiso 1 1 calc R . .
C22 C 0.0661(5) 0.1193(4) 0.7422(4) 0.0717(19) Uani 1 1 d . . .
H22A H -0.0065 0.1164 0.7248 0.086 Uiso 1 1 calc R . .
H22B H 0.0892 0.0726 0.7731 0.086 Uiso 1 1 calc R . .
C52 C -0.1147(5) 0.2455(5) 0.8040(4) 0.083(2) Uani 1 1 d . U .
H52A H -0.0798 0.2568 0.7592 0.100 Uiso 1 1 calc R . .
H52B H -0.1172 0.2928 0.8355 0.100 Uiso 1 1 calc R . .
C42 C 0.0721(5) 0.1185(4) 1.0167(4) 0.0706(19) Uani 1 1 d . . .
H42A H 0.0868 0.1678 1.0447 0.085 Uiso 1 1 calc R . .
H42B H 0.0005 0.1089 1.0099 0.085 Uiso 1 1 calc R . .
C23 C 0.1125(6) 0.1243(5) 0.6654(4) 0.078(2) Uani 1 1 d . . .
H23A H 0.0810 0.1663 0.6303 0.094 Uiso 1 1 calc R . .
H23B H 0.1835 0.1364 0.6832 0.094 Uiso 1 1 calc R . .
C43 C 0.1290(5) 0.0566(4) 1.0695(4) 0.0721(19) Uani 1 1 d . . .
H43A H 0.2002 0.0682 1.0782 0.086 Uiso 1 1 calc R . .
H43B H 0.1178 0.0082 1.0390 0.086 Uiso 1 1 calc R . .
C32 C 0.2012(6) 0.2755(5) 0.9550(5) 0.095(2) Uani 1 1 d . . .
H32A H 0.2211 0.2372 0.9987 0.114 Uiso 1 1 calc R . .
H32B H 0.2368 0.2641 0.9107 0.114 Uiso 1 1 calc R . .
C34 C 0.3419(8) 0.3594(7) 1.0265(8) 0.147(4) Uani 1 1 d . . .
H34A H 0.3794 0.3587 0.9827 0.220 Uiso 1 1 calc GR . .
H34B H 0.3631 0.3172 1.0642 0.220 Uiso 1 1 calc GR . .
H34C H 0.3535 0.4073 1.0566 0.220 Uiso 1 1 calc GR . .
C44 C 0.1019(6) 0.0458(5) 1.1528(5) 0.093(2) Uani 1 1 d . . .
H44A H 0.0305 0.0388 1.1454 0.140 Uiso 1 1 calc GR . .
H44B H 0.1221 0.0905 1.1869 0.140 Uiso 1 1 calc GR . .
H44C H 0.1358 0.0010 1.1797 0.140 Uiso 1 1 calc GR . .
C33 C 0.2317(7) 0.3514(5) 0.9890(7) 0.124(4) Uani 1 1 d . . .
H33A H 0.1939 0.3634 1.0317 0.149 Uiso 1 1 calc R . .
H33B H 0.2137 0.3893 0.9447 0.149 Uiso 1 1 calc R . .
C24 C 0.1021(7) 0.0521(6) 0.6150(5) 0.109(3) Uani 1 1 d . . .
H24A H 0.1366 0.0580 0.5696 0.163 Uiso 1 1 calc GR . .
H24B H 0.0321 0.0421 0.5929 0.163 Uiso 1 1 calc GR . .
H24C H 0.1308 0.0098 0.6498 0.163 Uiso 1 1 calc GR . .
V1 V 0.62743(7) 0.06097(6) 0.95978(6) 0.0480(3) Uani 1 1 d . . .
C53 C -0.2212(6) 0.2195(7) 0.7665(6) 0.136(4) Uani 1 1 d . U .
H53A H -0.2170 0.1698 0.7400 0.163 Uiso 1 1 calc R . .
H53B H -0.2555 0.2111 0.8123 0.163 Uiso 1 1 calc R . .
C54 C -0.2808(8) 0.2667(9) 0.7093(7) 0.179(6) Uani 1 1 d . U .
H54A H -0.2941 0.3137 0.7362 0.269 Uiso 1 1 calc GR . .
H54B H -0.3431 0.2409 0.6868 0.269 Uiso 1 1 calc GR . .
H54C H -0.2468 0.2784 0.6647 0.269 Uiso 1 1 calc GR . .
C1AA C 0.3549(11) 0.3466(8) 0.7370(9) 0.164(5) Uani 1 1 d D U .
H1AA H 0.3585 0.3929 0.7664 0.197 Uiso 1 1 calc R . .
C2AA C 0.3650(10) 0.2866(8) 0.7840(9) 0.181(5) Uani 1 1 d D U .
H2AA H 0.3625 0.2376 0.7603 0.217 Uiso 1 1 calc R . .
H2AB H 0.3749 0.2921 0.8418 0.217 Uiso 1 1 calc R . .
H3A H 0.602(3) -0.066(3) 0.770(3) 0.026(12) Uiso 1 1 d . . .
H3B H 0.660(5) 0.007(3) 0.787(4) 0.063(18) Uiso 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'
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
V3 V2 V1 65.41(3) 3_657 3_657
O1 V2 V3 47.08(3) . 3_657
O1 V2 V1 47.15(2) . 3_657
O2 V2 V3 81.67(10) . 3_657
O2 V2 O1 77.25(10) . .
O2 V2 V1 124.17(10) . 3_657
O4 V2 V3 124.25(11) . 3_657
O4 V2 O1 77.35(11) . .
O4 V2 O2 82.08(14) . .
O4 V2 V1 81.39(10) . 3_657
O6 V2 V3 33.62(11) . 3_657
O6 V2 O1 80.67(11) . .
O6 V2 O2 86.60(16) . .
O6 V2 O4 157.01(17) . .
O6 V2 V1 88.63(11) . 3_657
O7 V2 V3 87.11(13) . 3_657
O7 V2 O1 81.31(12) . .
O7 V2 O2 158.08(16) . .
O7 V2 O4 88.87(17) . .
O7 V2 O6 94.44(18) . .
O7 V2 V1 34.16(12) . 3_657
O9 V2 V3 137.76(17) . 3_657
O9 V2 O1 172.13(17) . .
O9 V2 O2 96.73(18) . .
O9 V2 O4 96.9(2) . .
O9 V2 O6 104.2(2) . .
O9 V2 O7 104.2(2) . .
O9 V2 V1 138.02(16) . 3_657
V2 V3 V1 66.26(3) 3_657 3_657
O1 V3 V2 48.00(3) . 3_657
O1 V3 V1 47.55(3) . 3_657
O3 V3 V2 82.09(11) . 3_657
O3 V3 O1 78.46(10) . .
O3 V3 O4 83.12(14) . .
O3 V3 V1 125.83(11) . 3_657
O4 V3 V2 125.03(11) . 3_657
O4 V3 O1 77.21(11) . .
O4 V3 V1 81.21(11) . 3_657
O5 V3 V2 88.41(12) . 3_657
O5 V3 O1 81.00(12) . .
O5 V3 O3 158.69(16) . .
O5 V3 O4 86.88(15) . .
O5 V3 V1 33.45(11) . 3_657
O6 V3 V2 34.56(12) 3_657 3_657
O6 V3 O1 82.52(12) 3_657 .
O6 V3 O3 90.04(16) 3_657 .
O6 V3 O4 159.52(16) 3_657 .
O6 V3 O5 92.88(17) 3_657 .
O6 V3 V1 87.34(12) 3_657 3_657
O10 V3 V2 137.99(17) . 3_657
O10 V3 O1 172.17(15) . .
O10 V3 O3 96.73(19) . .
O10 V3 O4 96.18(19) . .
O10 V3 O5 103.0(2) . .
O10 V3 O6 103.8(2) . 3_657
O10 V3 V1 136.28(17) . 3_657
V2 O1 V2 180.00(5) . 3_657
V3 O1 V2 95.09(4) 3_657 3_657
V3 O1 V2 84.91(4) . 3_657
V3 O1 V2 95.09(4) . .
V3 O1 V2 84.91(4) 3_657 .
V3 O1 V3 180.00(5) . 3_657
V3 O1 V1 94.56(4) 3_657 3_657
V3 O1 V1 85.44(4) 3_657 .
V3 O1 V1 94.57(4) . .
V3 O1 V1 85.43(4) . 3_657
V1 O1 V2 85.32(4) 3_657 .
V1 O1 V2 94.68(4) . .
V1 O1 V2 85.32(4) . 3_657
V1 O1 V2 94.68(4) 3_657 3_657
V1 O1 V1 180.00(3) 3_657 .
C3 O2 V2 118.0(4) . .
C3 O2 V1 118.7(4) . .
V1 O2 V2 108.96(15) . .
V3 O3 V1 109.30(16) . .
C4 O3 V3 118.6(3) . .
C4 O3 V1 118.2(3) . .
V2 O4 V3 109.87(17) . .
C2 O4 V2 119.6(3) . .
C2 O4 V3 117.7(4) . .
V1 O5 V3 112.06(18) 3_657 .
V3 O6 V2 111.82(18) 3_657 .
V2 O7 V1 112.86(19) . 3_657
O3 C4 C0AA 112.5(5) . .
C6 O11 C5 117.0(5) . .
O2 C3 C0AA 114.4(5) . .
O4 C2 C0AA 111.6(5) . .
C1 N13 C14 122.7(7) . .
C12 C7 C6 123.5(6) . .
C8 C7 C12 119.3(6) . .
C8 C7 C6 117.2(6) . .
C7 C12 C1 118.6(6) . .
C7 C12 C11 119.2(6) . .
C11 C12 C1 122.2(6) . .
O11 C5 C0AA 108.9(4) . .
O11 C6 C7 112.6(5) . .
O12 C6 O11 122.9(6) . .
O12 C6 C7 124.2(6) . .
O13 C1 N13 122.6(7) . .
O13 C1 C12 119.5(6) . .
N13 C1 C12 117.8(6) . .
C4 C0AA C2 110.8(5) . .
C4 C0AA C5 108.7(5) . .
C3 C0AA C4 110.3(5) . .
C3 C0AA C2 109.5(5) . .
C3 C0AA C5 107.3(5) . .
C5 C0AA C2 110.1(5) . .
C10 C11 C12 119.7(7) . .
C7 C8 C9 121.6(7) . .
C1AA C14 N13 117.5(9) . .
C10 C9 C8 117.8(7) . .
C11 C10 C9 122.4(8) . .
C51 N2 C41 108.3(4) . .
C51 N2 C31 109.9(5) . .
C31 N2 C41 112.3(5) . .
C21 N2 C51 110.2(5) . .
C21 N2 C41 108.2(4) . .
C21 N2 C31 107.9(5) . .
C52 C51 N2 117.4(5) . .
C42 C41 N2 115.8(5) . .
N2 C31 C32 115.3(6) . .
C22 C21 N2 118.0(5) . .
C21 C22 C23 111.0(6) . .
C51 C52 C53 112.1(7) . .
C43 C42 C41 111.9(5) . .
C24 C23 C22 113.7(7) . .
C42 C43 C44 115.0(6) . .
C33 C32 C31 113.9(7) . .
C32 C33 C34 114.9(8) . .
V3 V1 V2 65.87(3) 3_657 3_657
O1 V1 V2 47.52(3) . 3_657
O1 V1 V3 47.01(3) . 3_657
O2 V1 V2 125.79(10) . 3_657
O2 V1 V3 82.24(10) . 3_657
O2 V1 O1 78.50(10) . .
O2 V1 O3 82.87(15) . .
O3 V1 V2 80.86(10) . 3_657
O3 V1 V3 124.06(11) . 3_657
O3 V1 O1 77.22(10) . .
O5 V1 V2 87.60(11) 3_657 3_657
O5 V1 V3 34.48(11) 3_657 3_657
O5 V1 O1 81.49(11) 3_657 .
O5 V1 O2 89.26(16) 3_657 .
O5 V1 O3 158.37(16) 3_657 .
O5 V1 O7 93.87(17) 3_657 3_657
O7 V1 V2 32.97(11) 3_657 3_657
O7 V1 V3 88.10(12) 3_657 3_657
O7 V1 O1 80.49(12) 3_657 .
O7 V1 O2 158.05(16) 3_657 .
O7 V1 O3 86.37(16) 3_657 .
O8 V1 V2 136.30(16) . 3_657
O8 V1 V3 137.92(16) . 3_657
O8 V1 O1 173.11(15) . .
O8 V1 O2 96.85(18) . .
O8 V1 O3 97.26(19) . .
O8 V1 O5 103.68(19) . 3_657
O8 V1 O7 103.47(19) . 3_657
C54 C53 C52 118.5(9) . .
C2AA C1AA C14 132.7(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V2 V3 3.0185(15) 3_657
V2 O1 2.2521(9) .
V2 O2 2.052(4) .
V2 O4 1.992(4) .
V2 O6 1.844(4) .
V2 O7 1.798(4) .
V2 O9 1.606(4) .
V2 V1 3.0432(13) 3_657
V3 V2 3.0184(15) 3_657
V3 O1 2.2193(10) .
V3 O3 1.988(4) .
V3 O4 2.038(4) .
V3 O5 1.847(4) .
V3 O6 1.800(4) 3_657
V3 O10 1.596(4) .
V3 V1 3.0242(14) 3_657
O1 V2 2.2521(9) 3_657
O1 V3 2.2193(10) 3_657
O1 V1 2.2387(9) .
O1 V1 2.2386(9) 3_657
O2 C3 1.404(7) .
O2 V1 2.005(4) .
O3 C4 1.442(6) .
O3 V1 2.027(4) .
O4 C2 1.429(6) .
O5 V1 1.799(4) 3_657
O6 V3 1.800(4) 3_657
O7 V1 1.855(4) 3_657
C4 C0AA 1.506(8) .
O8 V1 1.585(4) .
O11 C5 1.455(7) .
O11 C6 1.337(7) .
O12 C6 1.217(7) .
C3 C0AA 1.506(8) .
O13 C1 1.234(7) .
C2 C0AA 1.539(8) .
N13 C1 1.333(8) .
N13 C14 1.456(9) .
C7 C12 1.394(9) .
C7 C6 1.459(9) .
C7 C8 1.381(9) .
C12 C1 1.488(9) .
C12 C11 1.417(9) .
C5 C0AA 1.524(7) .
C11 C10 1.354(10) .
C8 C9 1.400(10) .
C14 C1AA 1.388(14) .
C9 C10 1.381(11) .
N2 C51 1.513(7) .
N2 C41 1.525(7) .
N2 C31 1.514(8) .
N2 C21 1.512(7) .
C51 C52 1.482(8) .
C41 C42 1.496(8) .
C31 C32 1.515(10) .
C21 C22 1.496(9) .
C22 C23 1.517(8) .
C52 C53 1.517(11) .
C42 C43 1.488(8) .
C23 C24 1.486(10) .
C43 C44 1.493(9) .
C32 C33 1.453(11) .
C34 C33 1.502(12) .
V1 V2 3.0432(13) 3_657
V1 V3 3.0243(14) 3_657
V1 O5 1.799(4) 3_657
V1 O7 1.855(4) 3_657
C53 C54 1.371(12) .
C1AA C2AA 1.281(9) .
