#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:43:09 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230236 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/71/7057100.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_7057100
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_sum            'C66 H116 N4 O25 V6'
_chemical_formula_weight         1671.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                107.72(3)
_cell_angle_beta                 94.21(3)
_cell_angle_gamma                104.66(3)
_cell_formula_units_Z            1
_cell_length_a                   11.187(2)
_cell_length_b                   13.547(3)
_cell_length_c                   14.326(3)
_cell_measurement_reflns_used    1993
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.1827
_cell_measurement_theta_min      2.4687
_cell_volume                     1973.9(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13073
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.564
_diffrn_reflns_theta_min         1.512
_exptl_absorpt_coefficient_mu    0.756
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7302
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1755P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4460
_reflns_number_total             7302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj04727d2.cif
_cod_data_source_block           lbzda
_cod_depositor_comments
'Adding full bibliography for 7057098--7057101.cif.'
_cod_original_cell_volume        1974.0(8)
_cod_database_code               7057100
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.15050(9) 1.15921(8) 0.55665(7) 0.0488(3) Uani 1 1 d . . . . .
V3 V -0.14474(8) 1.06515(8) 0.44388(7) 0.0492(3) Uani 1 1 d . . . . .
O1 O 0.0000 1.0000 0.5000 0.0352(10) Uani 1 2 d S . P . .
O2 O 0.1761(3) 1.0979(3) 0.4153(3) 0.0459(9) Uani 1 1 d . . . . .
O3 O -0.0604(4) 1.0220(3) 0.3242(3) 0.0479(9) Uani 1 1 d . . . . .
O4 O 0.2397(4) 1.0761(3) 0.5924(3) 0.0572(11) Uani 1 1 d . . . . .
O5 O 0.0697(4) 1.1732(3) 0.6642(3) 0.0587(11) Uani 1 1 d . . . . .
O6 O 0.0082(4) 1.1944(3) 0.4891(3) 0.0480(9) Uani 1 1 d . . . . .
O7 O -0.1686(4) 1.0978(3) 0.5728(3) 0.0595(11) Uani 1 1 d . . . . .
O8 O 0.1063(5) 0.9183(4) 0.2475(3) 0.0679(12) Uani 1 1 d . . . . .
C1 C 0.0778(6) 1.1960(5) 0.3314(4) 0.0518(14) Uani 1 1 d . . . . .
O9 O 0.2506(4) 1.2754(3) 0.5813(3) 0.0701(13) Uani 1 1 d . . . . .
O10 O -0.2319(4) 1.1233(4) 0.3993(4) 0.0765(14) Uani 1 1 d . . . . .
O11 O 0.1426(5) 1.2300(4) 0.1817(3) 0.0723(13) Uani 1 1 d . . . . .
C2 C 0.0391(6) 1.2580(5) 0.4245(4) 0.0520(14) Uani 1 1 d . . . . .
H H 0.1068 1.3230 0.4599 0.062 Uiso 1 1 calc R U . . .
HA H -0.0330 1.2799 0.4068 0.062 Uiso 1 1 calc R U . . .
C3 C 0.1956(6) 1.1659(5) 0.3572(4) 0.0544(15) Uani 1 1 d . . . . .
HB H 0.2221 1.1296 0.2963 0.065 Uiso 1 1 calc R U . . .
HC H 0.2623 1.2315 0.3932 0.065 Uiso 1 1 calc R U . . .
C4 C -0.0285(6) 1.0938(5) 0.2713(4) 0.0564(15) Uani 1 1 d . . . . .
HD H -0.1017 1.1147 0.2540 0.068 Uiso 1 1 calc R U . . .
HE H -0.0027 1.0575 0.2101 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1049(8) 1.2758(6) 0.2723(5) 0.0718(19) Uani 1 1 d . . . . .
HF H 0.0301 1.2965 0.2595 0.086 Uiso 1 1 calc R U . . .
HG H 0.1703 1.3408 0.3120 0.086 Uiso 1 1 calc R U . . .
O13 O 0.1388(7) 1.3847(5) 0.0790(4) 0.113(2) Uani 1 1 d . . . . .
C7 C 0.2752(7) 1.2300(7) 0.0615(5) 0.074(2) Uani 1 1 d . . . . .
C6 C 0.2602(8) 1.2772(7) 0.1667(6) 0.082(2) Uani 1 1 d . . . . .
C8 C 0.2023(7) 1.2334(6) -0.0167(5) 0.0716(19) Uani 1 1 d . . . . .
C13 C 0.1098(9) 1.2999(7) 0.0069(5) 0.093(3) Uani 1 1 d . . . . .
C12 C 0.3634(10) 1.1770(10) 0.0410(7) 0.117(3) Uani 1 1 d . . . . .
HH H 0.4144 1.1756 0.0946 0.141 Uiso 1 1 calc R U . . .
O12 O 0.3388(6) 1.3411(6) 0.2328(4) 0.120(2) Uani 1 1 d . . . . .
N1 N 0.0079(9) 1.2695(8) -0.0549(6) 0.144(4) Uani 1 1 d . . . . .
HI H -0.0026 1.2156 -0.1086 0.173 Uiso 1 1 calc R U . . .
C11 C 0.3829(11) 1.1262(10) -0.0509(8) 0.135(4) Uani 1 1 d . . . . .
HJ H 0.4449 1.0913 -0.0611 0.163 Uiso 1 1 calc R U . . .
C10 C 0.3038(10) 1.1292(9) -0.1308(6) 0.109(3) Uani 1 1 d . . . . .
HK H 0.3110 1.0933 -0.1958 0.130 Uiso 1 1 calc R U . . .
C9 C 0.2169(8) 1.1843(7) -0.1130(5) 0.084(2) Uani 1 1 d . . . . .
HL H 0.1675 1.1888 -0.1658 0.101 Uiso 1 1 calc R U . . .
N2 N 0.3644(6) 0.6851(5) 0.3337(4) 0.0750(17) Uani 1 1 d . . . . .
C51 C 0.4269(7) 0.8086(6) 0.3670(6) 0.075(2) Uani 1 1 d . . . . .
H51A H 0.3936 0.8429 0.4249 0.090 Uiso 1 1 calc R U . . .
H51B H 0.5159 0.8225 0.3874 0.090 Uiso 1 1 calc R U . . .
C21 C 0.3831(9) 0.6243(8) 0.2377(7) 0.099(3) Uani 1 1 d . U . . .
H21A H 0.3559 0.6543 0.1893 0.119 Uiso 1 1 calc R U . . .
H21B H 0.3303 0.5503 0.2199 0.119 Uiso 1 1 calc R U . . .
C31 C 0.4060(9) 0.6409(8) 0.4133(7) 0.098(3) Uani 1 1 d . U . . .
H31A H 0.3639 0.5638 0.3908 0.118 Uiso 1 1 calc R U . . .
H31B H 0.4949 0.6492 0.4150 0.118 Uiso 1 1 calc R U . . .
C53 C 0.4589(7) 0.9831(6) 0.3399(6) 0.081(2) Uani 1 1 d . . . . .
H53A H 0.4093 1.0064 0.3905 0.097 Uiso 1 1 calc R U . . .
H53B H 0.5447 1.0023 0.3727 0.097 Uiso 1 1 calc R U . . .
C41 C 0.2196(8) 0.6734(7) 0.3312(8) 0.102(3) Uani 1 1 d . U . . .
H41A H 0.2097 0.7239 0.3926 0.123 Uiso 1 1 calc R U . . .
H41B H 0.1917 0.6960 0.2775 0.123 Uiso 1 1 calc R U . . .
C52 C 0.4107(8) 0.8606(6) 0.2927(6) 0.084(2) Uani 1 1 d . . . . .
H52A H 0.3227 0.8397 0.2648 0.101 Uiso 1 1 calc R U . . .
H52B H 0.4562 0.8365 0.2392 0.101 Uiso 1 1 calc R U . . .
C32 C 0.3860(14) 0.6868(10) 0.5167(8) 0.144(4) Uani 1 1 d . U . . .
H32A H 0.3000 0.6889 0.5167 0.172 Uiso 1 1 calc R U . . .
H32B H 0.4404 0.7604 0.5459 0.172 Uiso 1 1 calc R U . . .
V1 V 0.06330(10) 0.94377(8) 0.35306(7) 0.0489(3) Uani 1 1 d . . . . .
C54 C 0.4553(9) 1.0431(8) 0.2687(7) 0.101(3) Uani 1 1 d . . . . .
H54A H 0.4870 1.1196 0.3038 0.151 Uiso 1 1 calc R U . . .
H54B H 0.5061 1.0223 0.2193 0.151 Uiso 1 1 calc R U . . .
H54C H 0.3705 1.0263 0.2371 0.151 Uiso 1 1 calc R U . . .
C14 C -0.0915(14) 1.3223(13) -0.0384(10) 0.183(6) Uani 1 1 d D U . . .
HM H -0.1121 1.3418 -0.0961 0.219 Uiso 1 1 calc R U . . .
HN H -0.0608 1.3886 0.0182 0.219 Uiso 1 1 calc R U . . .
C15 C -0.2070(16) 1.2527(18) -0.0200(13) 0.234(9) Uani 1 1 d D U . . .
HO H -0.2707 1.2903 -0.0143 0.281 Uiso 1 1 calc R U . . .
HP H -0.2376 1.1869 -0.0770 0.281 Uiso 1 1 calc R U . . .
C16 C -0.1895(18) 1.223(2) 0.0703(15) 0.260(10) Uani 1 1 d D U . . .
HQ H -0.1368 1.2868 0.1227 0.312 Uiso 1 1 calc R U . . .
HR H -0.1441 1.1694 0.0566 0.312 Uiso 1 1 calc R U . . .
C17 C -0.304(2) 1.180(2) 0.109(2) 0.297(12) Uani 1 1 d D U . . .
HS H -0.2807 1.1636 0.1670 0.446 Uiso 1 1 calc R U . . .
HT H -0.3490 1.2327 0.1251 0.446 Uiso 1 1 calc R U . . .
HU H -0.3563 1.1149 0.0587 0.446 Uiso 1 1 calc R U . . .
C22 C 0.5149(9) 0.6228(11) 0.2310(8) 0.131(4) Uani 1 1 d . U . . .
H22A H 0.5658 0.6965 0.2435 0.157 Uiso 1 1 calc R U . . .
H22B H 0.5440 0.5997 0.2840 0.157 Uiso 1 1 calc R U . . .
C24 C 0.6572(15) 0.5372(16) 0.1350(14) 0.212(8) Uani 1 1 d . U . . .
H24A H 0.6587 0.4912 0.0694 0.318 Uiso 1 1 calc R U . . .
H24B H 0.7207 0.6050 0.1504 0.318 Uiso 1 1 calc R U . . .
H24C H 0.6728 0.5028 0.1822 0.318 Uiso 1 1 calc R U . . .
C23 C 0.5382(14) 0.5556(12) 0.1391(12) 0.176(6) Uani 1 1 d . U . . .
H23A H 0.4758 0.4856 0.1204 0.212 Uiso 1 1 calc R U . . .
H23B H 0.5235 0.5873 0.0887 0.212 Uiso 1 1 calc R U . . .
C33 C 0.4133(16) 0.6196(14) 0.5788(9) 0.193(7) Uani 1 1 d D U . . .
H33A H 0.3925 0.5441 0.5374 0.232 Uiso 1 1 calc R U . . .
H33B H 0.5017 0.6440 0.6062 0.232 Uiso 1 1 calc R U . . .
C34 C 0.338(2) 0.631(2) 0.6606(17) 0.344(16) Uani 1 1 d D U . . .
H34A H 0.3551 0.5883 0.6999 0.516 Uiso 1 1 calc R U . . .
H34B H 0.3594 0.7055 0.7018 0.516 Uiso 1 1 calc R U . . .
H34C H 0.2504 0.6059 0.6331 0.516 Uiso 1 1 calc R U . . .
C42 C 0.1337(10) 0.5645(9) 0.3186(10) 0.136(4) Uani 1 1 d D U . . .
H42A H 0.1587 0.5408 0.3725 0.163 Uiso 0.67(3) 1 calc R U P A 1
H42B H 0.1406 0.5129 0.2568 0.163 Uiso 0.67(3) 1 calc R U P A 1
H42C H 0.1287 0.5543 0.3825 0.163 Uiso 0.33(3) 1 calc R U P A 2
H42D H 0.1635 0.5079 0.2765 0.163 Uiso 0.33(3) 1 calc R U P A 2
C43A C -0.0011(13) 0.567(2) 0.3178(17) 0.168(9) Uani 0.67(3) 1 d D U P A 1
H43A H -0.0176 0.5871 0.3856 0.201 Uiso 0.67(3) 1 calc R U P A 1
H43B H -0.0133 0.6217 0.2906 0.201 Uiso 0.67(3) 1 calc R U P A 1
C44A C -0.092(4) 0.460(3) 0.258(3) 0.43(4) Uani 0.67(3) 1 d D U P A 1
H44A H -0.1762 0.4658 0.2599 0.641 Uiso 0.67(3) 1 calc R U P A 1
H44B H -0.0777 0.4405 0.1907 0.641 Uiso 0.67(3) 1 calc R U P A 1
H44C H -0.0821 0.4059 0.2856 0.641 Uiso 0.67(3) 1 calc R U P A 1
C43B C 0.007(2) 0.561(3) 0.271(4) 0.185(17) Uani 0.33(3) 1 d D U P A 2
H43C H 0.0000 0.6340 0.2822 0.222 Uiso 0.33(3) 1 calc R U P A 2
H43D H -0.0082 0.5229 0.2001 0.222 Uiso 0.33(3) 1 calc R U P A 2
C44B C -0.082(3) 0.503(4) 0.322(3) 0.19(2) Uani 0.33(3) 1 d D U P A 2
H44D H -0.1667 0.4965 0.2963 0.284 Uiso 0.33(3) 1 calc R U P A 2
H44E H -0.0731 0.4315 0.3106 0.284 Uiso 0.33(3) 1 calc R U P A 2
H44F H -0.0650 0.5417 0.3921 0.284 Uiso 0.33(3) 1 calc R U P A 2
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
O9 V2 O5 104.4(2) . .
O9 V2 O4 104.7(2) . .
O5 V2 O4 93.6(2) . .
O9 V2 O2 96.4(2) . .
O5 V2 O2 157.52(17) . .
O4 V2 O2 89.26(18) . .
O9 V2 O6 96.0(2) . .
O5 V2 O6 87.36(18) . .
O4 V2 O6 158.34(17) . .
O2 V2 O6 81.98(15) . .
O9 V2 O1 171.05(17) . .
O5 V2 O1 80.95(13) . .
O4 V2 O1 81.94(13) . .
O2 V2 O1 77.38(11) . .
O6 V2 O1 76.84(11) . .
O9 V2 V3 138.74(18) . 2_576
O5 V2 V3 87.80(13) . 2_576
O4 V2 V3 34.40(13) . 2_576
O2 V2 V3 82.02(11) . 2_576
O6 V2 V3 124.21(12) . 2_576
O1 V2 V3 47.55(3) . 2_576
O9 V2 V1 137.49(19) . 2_576
O5 V2 V1 33.52(13) . 2_576
O4 V2 V1 88.21(13) . 2_576
O2 V2 V1 124.53(11) . 2_576
O6 V2 V1 80.67(11) . 2_576
O1 V2 V1 47.43(3) . 2_576
V3 V2 V1 66.06(4) 2_576 2_576
O10 V3 O7 102.8(2) . .
O10 V3 O4 104.4(2) . 2_576
O7 V3 O4 94.4(2) . 2_576
O10 V3 O6 95.4(2) . .
O7 V3 O6 87.64(18) . .
O4 V3 O6 159.11(18) 2_576 .
O10 V3 O3 97.1(2) . .
O7 V3 O3 158.65(17) . .
O4 V3 O3 88.15(18) 2_576 .
O6 V3 O3 82.72(16) . .
O10 V3 O1 171.62(17) . .
O7 V3 O1 81.44(13) . .
O4 V3 O1 82.30(13) 2_576 .
O6 V3 O1 77.45(11) . .
O3 V3 O1 77.90(11) . .
O10 V3 V2 138.83(19) . 2_576
O7 V3 V2 88.13(13) . 2_576
O4 V3 V2 34.57(12) 2_576 2_576
O6 V3 V2 125.00(12) . 2_576
O3 V3 V2 81.98(11) . 2_576
O1 V3 V2 47.73(4) . 2_576
O10 V3 V1 136.3(2) . 2_576
O7 V3 V1 33.95(13) . 2_576
O4 V3 V1 89.03(13) 2_576 2_576
O6 V3 V1 81.07(11) . 2_576
O3 V3 V1 125.15(11) . 2_576
O1 V3 V1 47.49(3) . 2_576
V2 V3 V1 66.24(5) 2_576 2_576
V3 O1 V3 180.00(4) . 2_576
V3 O1 V1 94.87(4) . .
V3 O1 V1 85.13(4) 2_576 .
V3 O1 V1 85.13(4) . 2_576
V3 O1 V1 94.87(4) 2_576 2_576
V1 O1 V1 180.0 . 2_576
V3 O1 V2 95.27(4) . .
V3 O1 V2 84.73(4) 2_576 .
V1 O1 V2 94.94(5) . .
V1 O1 V2 85.06(5) 2_576 .
V3 O1 V2 84.73(4) . 2_576
V3 O1 V2 95.27(4) 2_576 2_576
V1 O1 V2 85.06(5) . 2_576
V1 O1 V2 94.94(5) 2_576 2_576
V2 O1 V2 180.0 . 2_576
C3 O2 V2 118.8(3) . .
C3 O2 V1 119.1(3) . .
V2 O2 V1 109.79(17) . .
C4 O3 V3 118.7(4) . .
C4 O3 V1 119.4(4) . .
V3 O3 V1 109.06(16) . .
V3 O4 V2 111.04(19) 2_576 .
V1 O5 V2 112.7(2) 2_576 .
C2 O6 V3 118.7(3) . .
C2 O6 V2 117.6(3) . .
V3 O6 V2 109.99(17) . .
V3 O7 V1 112.3(2) . 2_576
C2 C1 C3 110.1(5) . .
C2 C1 C4 110.9(5) . .
C3 C1 C4 110.4(5) . .
C2 C1 C5 104.4(5) . .
C3 C1 C5 110.7(5) . .
C4 C1 C5 110.2(5) . .
C6 O11 C5 118.4(6) . .
O6 C2 C1 112.1(5) . .
O2 C3 C1 112.3(5) . .
O3 C4 C1 112.1(5) . .
O11 C5 C1 111.8(6) . .
C8 C7 C12 117.4(8) . .
C8 C7 C6 123.5(8) . .
C12 C7 C6 119.0(8) . .
O12 C6 O11 122.3(7) . .
O12 C6 C7 126.9(8) . .
O11 C6 C7 110.7(6) . .
C7 C8 C9 121.0(8) . .
C7 C8 C13 117.1(7) . .
C9 C8 C13 121.8(7) . .
O13 C13 N1 122.1(10) . .
O13 C13 C8 120.0(8) . .
N1 C13 C8 117.6(8) . .
C11 C12 C7 125.1(10) . .
C13 N1 C14 123.1(9) . .
C12 C11 C10 116.2(11) . .
C9 C10 C11 120.2(9) . .
C10 C9 C8 120.0(8) . .
C21 N2 C31 110.9(7) . .
C21 N2 C51 115.4(7) . .
C31 N2 C51 109.5(6) . .
C21 N2 C41 108.7(6) . .
C31 N2 C41 107.7(7) . .
C51 N2 C41 104.2(5) . .
C52 C51 N2 116.0(6) . .
N2 C21 C22 114.4(7) . .
C32 C31 N2 119.8(8) . .
C54 C53 C52 114.3(7) . .
C42 C41 N2 117.9(7) . .
C51 C52 C53 110.3(7) . .
C31 C32 C33 111.1(9) . .
O8 V1 O5 102.9(2) . 2_576
O8 V1 O7 104.5(2) . 2_576
O5 V1 O7 94.42(19) 2_576 2_576
O8 V1 O2 97.9(2) . .
O5 V1 O2 157.62(18) 2_576 .
O7 V1 O2 88.19(18) 2_576 .
O8 V1 O3 96.2(2) . .
O5 V1 O3 87.88(18) 2_576 .
O7 V1 O3 157.96(18) 2_576 .
O2 V1 O3 81.72(15) . .
O8 V1 O1 172.50(17) . .
O5 V1 O1 81.28(13) 2_576 .
O7 V1 O1 81.13(14) 2_576 .
O2 V1 O1 77.17(11) . .
O3 V1 O1 77.56(11) . .
O8 V1 V3 138.13(18) . 2_576
O5 V1 V3 88.31(13) 2_576 2_576
O7 V1 V3 33.75(13) 2_576 2_576
O2 V1 V3 81.56(11) . 2_576
O3 V1 V3 124.71(11) . 2_576
O1 V1 V3 47.38(3) . 2_576
O8 V1 V2 136.40(18) . 2_576
O5 V1 V2 33.77(13) 2_576 2_576
O7 V1 V2 88.30(14) 2_576 2_576
O2 V1 V2 124.40(11) . 2_576
O3 V1 V2 81.47(11) . 2_576
O1 V1 V2 47.51(4) . 2_576
V3 V1 V2 66.22(4) 2_576 2_576
N1 C14 C15 112.9(14) . .
C16 C15 C14 114.3(16) . .
C15 C16 C17 117.3(18) . .
C23 C22 C21 117.2(9) . .
C24 C23 C22 119.0(16) . .
C34 C33 C32 109.5(14) . .
C41 C42 C43B 106.3(15) . .
C41 C42 C43A 111.4(12) . .
C44A C43A C42 113(2) . .
C44B C43B C42 103(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V2 O9 1.603(4) .
V2 O5 1.828(4) .
V2 O4 1.837(4) .
V2 O2 2.014(4) .
V2 O6 2.034(4) .
V2 O1 2.2452(14) .
V2 V3 3.0215(15) 2_576
V2 V1 3.0337(16) 2_576
V3 O10 1.607(5) .
V3 O7 1.820(4) .
V3 O4 1.829(4) 2_576
V3 O6 2.011(4) .
V3 O3 2.020(4) .
V3 O1 2.2387(11) .
V3 V2 3.0215(15) 2_576
V3 V1 3.0313(16) 2_576
O1 V3 2.2388(11) 2_576
O1 V1 2.2425(11) .
O1 V1 2.2425(11) 2_576
O1 V2 2.2453(14) 2_576
O2 C3 1.407(6) .
O2 V1 2.028(4) .
O3 C4 1.401(7) .
O3 V1 2.033(4) .
O4 V3 1.829(4) 2_576
O5 V1 1.816(4) 2_576
O6 C2 1.449(6) .
O7 V1 1.830(4) 2_576
O8 V1 1.584(4) .
C1 C2 1.502(8) .
C1 C3 1.528(9) .
C1 C4 1.537(8) .
C1 C5 1.552(8) .
O11 C6 1.374(9) .
O11 C5 1.403(8) .
O13 C13 1.238(9) .
C7 C8 1.356(10) .
C7 C12 1.359(12) .
C7 C6 1.489(10) .
C6 O12 1.188(8) .
C8 C9 1.380(10) .
C8 C13 1.527(13) .
C13 N1 1.284(10) .
C12 C11 1.350(13) .
N1 C14 1.463(15) .
C11 C10 1.410(14) .
C10 C9 1.362(13) .
N2 C21 1.433(10) .
N2 C31 1.535(10) .
N2 C51 1.545(9) .
N2 C41 1.584(10) .
C51 C52 1.468(11) .
C21 C22 1.490(12) .
C31 C32 1.479(13) .
C53 C54 1.490(11) .
C53 C52 1.521(10) .
C41 C42 1.491(13) .
C32 C33 1.518(16) .
V1 O5 1.816(4) 2_576
V1 O7 1.830(4) 2_576
V1 V3 3.0313(16) 2_576
V1 V2 3.0337(16) 2_576
C14 C15 1.488(9) .
C15 C16 1.480(9) .
C16 C17 1.485(10) .
C22 C23 1.438(15) .
C24 C23 1.418(17) .
C33 C34 1.487(9) .
C42 C43B 1.515(10) .
C42 C43A 1.517(10) .
C43A C44A 1.495(10) .
C43B C44B 1.493(10) .
