#------------------------------------------------------------------------------
#$Date: 2021-09-28 01:59:49 +0300 (Tue, 28 Sep 2021) $
#$Revision: 269333 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/84/7708452.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_7708452
loop_
_publ_author_name
'Huang, Li'
'Ouyang, Congrui'
'Liu, Xing'
'Zhou, Jian'
'Zou, Hua-Hong'
'Yuan, Hua'
'Wen, Dou'
_publ_section_title
;
 A series of organic hybrid polyoxovanadate clusters incorporating
 tris(hydroxymethyl)methane derivatives
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02912F
_journal_year                    2021
_chemical_formula_moiety         'C35 H75 N8 O46 V14, 2(H2 O)'
_chemical_formula_sum            'C35 H79 N8 O48 V14'
_chemical_formula_weight         2093.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-08-29 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.460(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8462(18)
_cell_length_b                   19.9961(18)
_cell_length_c                   18.8270(16)
_cell_measurement_reflns_used    88077
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5120
_cell_measurement_theta_min      2.1911
_cell_volume                     6998.5(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85127
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.992
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_description       block
_exptl_crystal_F_000             4204
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   0.853
_exptl_transmission_factor_min   0.777
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8021
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+158.9745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5971
_reflns_number_total             8021
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02912f2.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7708452
_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.
;
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.858
loop_
_space_group_symop_operation_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'
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
V1 V 0.36450(6) 0.46026(6) 0.37935(6) 0.0336(3) Uani 1 1 d . . . . .
V2 V 0.27789(6) 0.35496(5) 0.47505(6) 0.0291(2) Uani 1 1 d . . . . .
V3 V 0.32648(7) 0.19667(6) 0.40398(6) 0.0355(3) Uani 1 1 d . . . . .
V4 V 0.23995(6) 0.34006(6) 0.32850(6) 0.0333(3) Uani 1 1 d . . . . .
V5 V 0.41602(6) 0.31372(6) 0.39323(7) 0.0359(3) Uani 1 1 d . . . . .
V6 V 0.23637(7) 0.50674(6) 0.46719(7) 0.0389(3) Uani 1 1 d . . . . .
V7 V 0.19874(7) 0.49455(6) 0.29547(7) 0.0418(3) Uani 1 1 d . . . . .
O1 O 0.4290(3) 0.2451(2) 0.4703(3) 0.0411(12) Uani 1 1 d . . . . .
O2 O 0.3938(3) 0.2296(2) 0.3344(3) 0.0396(11) Uani 1 1 d . . . . .
O3 O 0.5378(9) 0.0661(8) 0.4799(10) 0.162(7) Uani 0.723(15) 1 d D . P A 1
H3E H 0.5660 0.0348 0.4810 0.243 Uiso 0.723(15) 1 calc R U P A 1
O3B O 0.5860(17) 0.1296(17) 0.383(3) 0.162(7) Uani 0.277(15) 1 d D U P A 2
H3F H 0.6190 0.1030 0.3826 0.243 Uiso 0.277(15) 1 calc R U P A 2
O4 O 0.2828(3) 0.4352(2) 0.5335(2) 0.0359(10) Uani 1 1 d . . . . .
O5 O 0.3909(2) 0.3900(2) 0.4578(2) 0.0313(9) Uani 1 1 d . . . . .
O6 O 0.5014(4) 0.3298(4) 0.6522(4) 0.077(2) Uani 1 1 d . . . . .
H6C H 0.4953 0.2973 0.6770 0.116 Uiso 1 1 calc R U . . .
O7 O 0.3589(3) 0.3763(2) 0.3182(2) 0.0357(11) Uani 1 1 d . . . . .
O8 O 0.2158(3) 0.4075(2) 0.2524(2) 0.0398(11) Uani 1 1 d . . . . .
O9 O 0.3693(7) 0.2721(6) 0.1323(7) 0.071(4) Uani 0.563(16) 1 d . . P B 1
H9A H 0.4089 0.2871 0.1280 0.106 Uiso 0.563(16) 1 calc R U P B 1
O9B O 0.2586(10) 0.2973(8) 0.0753(8) 0.075(6) Uani 0.437(16) 1 d . . P B 2
H9B H 0.2381 0.3289 0.0529 0.112 Uiso 0.437(16) 1 calc R U P B 2
O10 O 0.2009(3) 0.5571(2) 0.3770(3) 0.0420(12) Uani 1 1 d . . . . .
O11 O 0.3361(3) 0.5263(2) 0.4502(3) 0.0376(11) Uani 1 1 d . . . . .
O12 O 0.3036(3) 0.5133(2) 0.3019(3) 0.0388(11) Uani 1 1 d . . . . .
O13 O 0.1122(3) 0.4549(3) 0.3301(3) 0.0533(14) Uani 1 1 d . . . . .
O14 O 0.1370(3) 0.4620(3) 0.4521(4) 0.0539(15) Uani 1 1 d . . . . .
O15 O 0.2227(4) 0.5624(3) 0.5238(3) 0.0596(16) Uani 1 1 d . . . . .
O16 O 0.1617(3) 0.5371(3) 0.2277(3) 0.0588(15) Uani 1 1 d . . . . .
O17 O 0.2628(3) 0.1653(3) 0.3481(3) 0.0496(13) Uani 1 1 d . . . . .
O18 O 0.4425(3) 0.4877(3) 0.3726(3) 0.0466(13) Uani 1 1 d . . . . .
O19 O 0.4970(3) 0.3303(3) 0.3833(3) 0.0564(15) Uani 1 1 d . . . . .
O20 O 0.1643(3) 0.3044(3) 0.3304(3) 0.0431(12) Uani 1 1 d . . . . .
O21 O 0.3043(2) 0.2918(2) 0.4045(2) 0.0298(9) Uani 1 1 d . . . . .
O22 O 0.2069(3) 0.3200(2) 0.5015(2) 0.0354(10) Uani 1 1 d . . . . .
O23 O 0.2541(2) 0.4183(2) 0.3943(2) 0.0293(9) Uani 1 1 d . . . . .
N1 N 0.3988(4) 0.1166(3) 0.4163(4) 0.0571(19) Uani 1 1 d . . . . .
H1A H 0.4018 0.0979 0.4596 0.069 Uiso 1 1 calc R U . . .
H1B H 0.3865 0.0856 0.3826 0.069 Uiso 1 1 calc R U . . .
N2 N 0.3550(3) 0.3238(3) 0.5631(3) 0.0380(13) Uani 1 1 d . . . . .
H2C H 0.3339 0.3076 0.5985 0.046 Uiso 1 1 calc R U . . .
H2D H 0.3840 0.2927 0.5498 0.046 Uiso 1 1 calc R U . . .
N3 N 0.2752(3) 0.2902(3) 0.2404(3) 0.0405(14) Uani 1 1 d . . . . .
H3C H 0.3100 0.2611 0.2559 0.049 Uiso 1 1 calc R U . . .
H3D H 0.2389 0.2687 0.2136 0.049 Uiso 1 1 calc R U . . .
N4 N 0.3317(4) 0.6921(4) 0.3559(4) 0.0563(18) Uani 1 1 d D . . . .
H4A H 0.338(5) 0.721(4) 0.393(3) 0.068 Uiso 1 1 d D U . . .
H4B H 0.375(2) 0.700(5) 0.345(5) 0.068 Uiso 1 1 d D U . . .
C1 C 0.4670(5) 0.1501(4) 0.4075(6) 0.060(2) Uani 1 1 d . . . . .
C2 C 0.4851(5) 0.1987(5) 0.4688(5) 0.060(2) Uani 1 1 d . . . . .
H2A H 0.4937 0.1744 0.5139 0.072 Uiso 1 1 calc R U . . .
H2B H 0.5288 0.2226 0.4637 0.072 Uiso 1 1 calc R U . . .
C3 C 0.4509(5) 0.1836(4) 0.3344(5) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.4934 0.2069 0.3244 0.067 Uiso 1 1 calc R U . . .
H3B H 0.4376 0.1502 0.2972 0.067 Uiso 1 1 calc R U . . .
C4 C 0.5280(8) 0.0967(7) 0.4094(9) 0.108(5) Uani 1 1 d D . . . .
H4C H 0.5143 0.0633 0.3724 0.130 Uiso 0.723(15) 1 calc R U P A 1
H4D H 0.5722 0.1178 0.4011 0.130 Uiso 0.723(15) 1 calc R U P A 1
H4E H 0.5434 0.0808 0.4582 0.130 Uiso 0.277(15) 1 calc R U P A 2
H4F H 0.5111 0.0589 0.3790 0.130 Uiso 0.277(15) 1 calc R U P A 2
C5 C 0.3955(4) 0.3864(4) 0.5859(4) 0.0413(16) Uani 1 1 d . . . . .
C6 C 0.3403(4) 0.4404(4) 0.5929(4) 0.0397(16) Uani 1 1 d . . . . .
H6A H 0.3219 0.4348 0.6378 0.048 Uiso 1 1 calc R U . . .
H6B H 0.3625 0.4842 0.5932 0.048 Uiso 1 1 calc R U . . .
C7 C 0.4372(4) 0.4025(4) 0.5251(4) 0.0425(17) Uani 1 1 d . . . . .
H7A H 0.4522 0.4490 0.5278 0.051 Uiso 1 1 calc R U . . .
H7B H 0.4798 0.3746 0.5290 0.051 Uiso 1 1 calc R U . . .
C8 C 0.4472(5) 0.3784(5) 0.6575(4) 0.056(2) Uani 1 1 d . . . . .
H8A H 0.4699 0.4211 0.6712 0.067 Uiso 1 1 calc R U . . .
H8B H 0.4202 0.3651 0.6948 0.067 Uiso 1 1 calc R U . . .
C9 C 0.3022(5) 0.3456(4) 0.1989(4) 0.0463(18) Uani 1 1 d . . . . .
C10 C 0.3692(4) 0.3741(4) 0.2447(4) 0.0447(18) Uani 1 1 d . . . . .
H10A H 0.4104 0.3464 0.2403 0.054 Uiso 1 1 calc R U . . .
H10B H 0.3783 0.4188 0.2283 0.054 Uiso 1 1 calc R U . . .
C11 C 0.2420(5) 0.3972(4) 0.1865(4) 0.050(2) Uani 1 1 d . . . . .
H11A H 0.2599 0.4390 0.1702 0.061 Uiso 1 1 calc R U . . .
H11B H 0.2034 0.3814 0.1498 0.061 Uiso 1 1 calc R U . . .
C12 C 0.3211(6) 0.3221(5) 0.1263(5) 0.061(2) Uani 1 1 d . . . . .
H12A H 0.2773 0.3074 0.0957 0.073 Uiso 0.563(16) 1 calc R U P B 1
H12B H 0.3399 0.3597 0.1028 0.073 Uiso 0.563(16) 1 calc R U P B 1
H12C H 0.3427 0.3590 0.1042 0.073 Uiso 0.437(16) 1 calc R U P B 2
H12D H 0.3566 0.2867 0.1352 0.073 Uiso 0.437(16) 1 calc R U P B 2
C13 C 0.3101(4) 0.6216(4) 0.3663(4) 0.0427(17) Uani 1 1 d . . . . .
C14 C 0.2294(4) 0.6229(3) 0.3694(4) 0.0459(18) Uani 1 1 d . . . . .
H14A H 0.2211 0.6503 0.4097 0.055 Uiso 1 1 calc R U . . .
H14B H 0.2041 0.6432 0.3257 0.055 Uiso 1 1 calc R U . . .
C15 C 0.3523(4) 0.5944(3) 0.4353(4) 0.0427(17) Uani 1 1 d . . . . .
H15A H 0.4032 0.5978 0.4328 0.051 Uiso 1 1 calc R U . . .
H15B H 0.3430 0.6221 0.4750 0.051 Uiso 1 1 calc R U . . .
C16 C 0.3234(4) 0.5827(3) 0.3004(4) 0.0406(16) Uani 1 1 d . . . . .
H16A H 0.2964 0.6033 0.2577 0.049 Uiso 1 1 calc R U . . .
H16B H 0.3741 0.5857 0.2968 0.049 Uiso 1 1 calc R U . . .
C17 C 0.0988(5) 0.4468(4) 0.3936(7) 0.063(3) Uani 1 1 d D . . . .
H17A H 0.0549 0.4269 0.3969 0.075 Uiso 1 1 calc R U . C 1
O2W O -0.049(2) 0.379(2) 0.305(2) 0.30(2) Uani 0.5 1 d . U P D 1
H2E H -0.0207 0.4026 0.2878 0.449 Uiso 0.5 1 d R U P D 1
H2F H -0.0375 0.3393 0.3108 0.449 Uiso 0.5 1 d R U P D 1
C18 C 0.0200(13) 0.4181(19) 0.3824(18) 0.145(14) Uani 0.5 1 d D . P E 2
H18A H -0.0029 0.4311 0.4222 0.218 Uiso 0.5 1 calc R U P E 2
H18B H 0.0216 0.3702 0.3796 0.218 Uiso 0.5 1 calc R U P E 2
H18C H -0.0067 0.4357 0.3385 0.218 Uiso 0.5 1 calc R U P E 2
O1W O 0.4763(9) 0.2254(10) 0.7360(16) 0.132(8) Uani 0.5 1 d . . P . .
H1C H 0.4499 0.2110 0.7630 0.199 Uiso 0.5 1 d R U P . .
H1D H 0.4733 0.2066 0.6969 0.199 Uiso 0.5 1 d R U P . .
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
_geom_angle_publ_flag
O18 V1 O12 100.6(2) . . ?
O18 V1 O11 100.2(2) . . ?
O12 V1 O11 87.3(2) . . ?
O18 V1 O7 101.6(2) . . ?
O12 V1 O7 93.1(2) . . ?
O11 V1 O7 157.7(2) . . ?
O18 V1 O5 100.2(2) . . ?
O12 V1 O5 159.0(2) . . ?
O11 V1 O5 91.83(18) . . ?
O7 V1 O5 79.90(18) . . ?
O18 V1 O23 177.3(2) . . ?
O12 V1 O23 82.02(18) . . ?
O11 V1 O23 79.30(18) . . ?
O7 V1 O23 78.70(17) . . ?
O5 V1 O23 77.21(16) . . ?
O18 V1 V5 93.0(2) . . ?
O12 V1 V5 134.34(15) . . ?
O11 V1 V5 132.99(14) . . ?
O7 V1 V5 41.26(14) . . ?
O5 V1 V5 41.25(13) . . ?
O23 V1 V5 85.51(11) . . ?
O22 V2 O4 98.3(2) . . ?
O22 V2 O21 103.8(2) . . ?
O4 V2 O21 157.9(2) . . ?
O22 V2 O23 114.2(2) . . ?
O4 V2 O23 83.68(19) . . ?
O21 V2 O23 86.71(18) . . ?
O22 V2 N2 97.2(2) . . ?
O4 V2 N2 80.6(2) . . ?
O21 V2 N2 97.1(2) . . ?
O23 V2 N2 146.6(2) . . ?
O22 V2 O5 167.6(2) . . ?
O4 V2 O5 82.55(18) . . ?
O21 V2 O5 75.97(17) . . ?
O23 V2 O5 78.20(17) . . ?
N2 V2 O5 70.68(19) . . ?
O22 V2 V4 99.55(18) . . ?
O4 V2 V4 129.73(14) . . ?
O21 V2 V4 45.75(13) . . ?
O23 V2 V4 46.18(13) . . ?
N2 V2 V4 141.98(16) . . ?
O5 V2 V4 89.15(11) . . ?
O17 V3 O21 104.4(2) . . ?
O17 V3 O22 102.0(2) . 7_556 ?
O21 V3 O22 93.31(18) . 7_556 ?
O17 V3 O2 100.4(2) . . ?
O21 V3 O2 81.26(18) . . ?
O22 V3 O2 157.5(2) 7_556 . ?
O17 V3 N1 100.3(3) . . ?
O21 V3 N1 152.1(3) . . ?
O22 V3 N1 93.9(2) 7_556 . ?
O2 V3 N1 81.8(2) . . ?
O17 V3 O1 170.9(2) . . ?
O21 V3 O1 75.60(18) . . ?
O22 V3 O1 86.97(19) 7_556 . ?
O2 V3 O1 70.56(19) . . ?
N1 V3 O1 77.9(3) . . ?
O17 V3 V5 130.9(2) . . ?
O21 V3 V5 48.93(13) . . ?
O22 V3 V5 117.63(15) 7_556 . ?
O2 V3 V5 43.92(14) . . ?
N1 V3 V5 104.4(2) . . ?
O1 V3 V5 42.66(12) . . ?
O20 V4 O8 102.8(2) . . ?
O20 V4 O21 102.1(2) . . ?
O8 V4 O21 155.1(2) . . ?
O20 V4 O23 111.5(2) . . ?
O8 V4 O23 84.58(19) . . ?
O21 V4 O23 85.97(18) . . ?
O20 V4 N3 101.6(3) . . ?
O8 V4 N3 79.5(2) . . ?
O21 V4 N3 95.9(2) . . ?
O23 V4 N3 145.7(2) . . ?
O20 V4 O7 170.6(2) . . ?
O8 V4 O7 80.84(19) . . ?
O21 V4 O7 74.63(17) . . ?
O23 V4 O7 77.33(17) . . ?
N3 V4 O7 70.3(2) . . ?
O20 V4 V2 96.43(19) . . ?
O8 V4 V2 130.39(15) . . ?
O21 V4 V2 45.31(12) . . ?
O23 V4 V2 45.81(12) . . ?
N3 V4 V2 140.18(19) . . ?
O7 V4 V2 87.49(12) . . ?
O19 V5 O1 102.9(3) . . ?
O19 V5 O2 102.9(3) . . ?
O1 V5 O2 79.3(2) . . ?
O19 V5 O5 103.4(3) . . ?
O1 V5 O5 95.39(19) . . ?
O2 V5 O5 153.66(19) . . ?
O19 V5 O7 101.3(3) . . ?
O1 V5 O7 155.8(2) . . ?
O2 V5 O7 95.3(2) . . ?
O5 V5 O7 78.97(18) . . ?
O19 V5 O21 178.8(3) . . ?
O1 V5 O21 78.18(18) . . ?
O2 V5 O21 76.77(17) . . ?
O5 V5 O21 76.89(17) . . ?
O7 V5 O21 77.66(17) . . ?
O19 V5 V3 138.4(2) . . ?
O1 V5 V3 52.82(16) . . ?
O2 V5 V3 45.45(13) . . ?
O5 V5 V3 111.31(13) . . ?
O7 V5 V3 107.07(14) . . ?
O21 V5 V3 41.96(11) . . ?
O19 V5 V1 94.9(2) . . ?
O1 V5 V1 135.95(15) . . ?
O2 V5 V1 135.31(16) . . ?
O5 V5 V1 40.93(12) . . ?
O7 V5 V1 40.62(13) . . ?
O21 V5 V1 84.53(12) . . ?
V3 V5 V1 126.27(5) . . ?
O15 V6 O10 98.6(3) . . ?
O15 V6 O11 103.3(3) . . ?
O10 V6 O11 87.6(2) . . ?
O15 V6 O4 100.6(3) . . ?
O10 V6 O4 160.60(19) . . ?
O11 V6 O4 85.0(2) . . ?
O15 V6 O14 98.8(3) . . ?
O10 V6 O14 86.1(2) . . ?
O11 V6 O14 157.7(2) . . ?
O4 V6 O14 94.0(2) . . ?
O15 V6 O23 174.0(2) . . ?
O10 V6 O23 86.64(18) . . ?
O11 V6 O23 79.76(18) . . ?
O4 V6 O23 74.41(17) . . ?
O14 V6 O23 78.5(2) . . ?
O16 V7 O8 102.8(3) . . ?
O16 V7 O10 103.5(3) . . ?
O8 V7 O10 153.7(2) . . ?
O16 V7 O12 104.3(3) . . ?
O8 V7 O12 88.0(2) . . ?
O10 V7 O12 86.6(2) . . ?
O16 V7 O13 101.4(3) . . ?
O8 V7 O13 88.9(2) . . ?
O10 V7 O13 84.9(2) . . ?
O12 V7 O13 154.2(2) . . ?
C2 O1 V5 116.3(5) . . ?
C2 O1 V3 105.9(5) . . ?
V5 O1 V3 84.52(19) . . ?
C3 O2 V5 116.9(5) . . ?
C3 O2 V3 109.8(4) . . ?
V5 O2 V3 90.63(18) . . ?
C4 O3 H3E 109.5 . . ?
C4 O3B H3F 109.5 . . ?
C6 O4 V2 117.7(4) . . ?
C6 O4 V6 129.4(4) . . ?
V2 O4 V6 105.2(2) . . ?
C7 O5 V1 124.0(4) . . ?
C7 O5 V5 119.0(4) . . ?
V1 O5 V5 97.82(19) . . ?
C7 O5 V2 111.6(4) . . ?
V1 O5 V2 100.92(18) . . ?
V5 O5 V2 99.52(18) . . ?
C8 O6 H6C 109.5 . . ?
C10 O7 V1 124.9(4) . . ?
C10 O7 V5 120.5(4) . . ?
V1 O7 V5 98.1(2) . . ?
C10 O7 V4 110.3(4) . . ?
V1 O7 V4 99.59(18) . . ?
V5 O7 V4 98.70(17) . . ?
C11 O8 V4 117.7(4) . . ?
C11 O8 V7 126.2(5) . . ?
V4 O8 V7 109.9(2) . . ?
C12 O9 H9A 109.5 . . ?
C12 O9B H9B 109.5 . . ?
C14 O10 V7 117.6(4) . . ?
C14 O10 V6 118.0(5) . . ?
V7 O10 V6 107.6(2) . . ?
C15 O11 V6 117.0(4) . . ?
C15 O11 V1 113.9(4) . . ?
V6 O11 V1 109.7(2) . . ?
C16 O12 V7 116.0(4) . . ?
C16 O12 V1 113.9(4) . . ?
V7 O12 V1 112.8(2) . . ?
C17 O13 V7 130.5(6) . . ?
C17 O14 V6 127.4(5) . . ?
V3 O21 V2 135.5(2) . . ?
V3 O21 V4 125.6(2) . . ?
V2 O21 V4 88.95(17) . . ?
V3 O21 V5 89.11(17) . . ?
V2 O21 V5 107.0(2) . . ?
V4 O21 V5 108.47(19) . . ?
V2 O22 V3 136.2(3) . 7_556 ?
V2 O23 V4 88.01(17) . . ?
V2 O23 V6 94.04(17) . . ?
V4 O23 V6 164.1(2) . . ?
V2 O23 V1 103.42(19) . . ?
V4 O23 V1 104.01(18) . . ?
V6 O23 V1 90.87(16) . . ?
C1 N1 V3 101.7(5) . . ?
C1 N1 H1A 111.4 . . ?
V3 N1 H1A 111.4 . . ?
C1 N1 H1B 111.4 . . ?
V3 N1 H1B 111.4 . . ?
H1A N1 H1B 109.3 . . ?
C5 N2 V2 103.4(4) . . ?
C5 N2 H2C 111.1 . . ?
V2 N2 H2C 111.1 . . ?
C5 N2 H2D 111.1 . . ?
V2 N2 H2D 111.1 . . ?
H2C N2 H2D 109.0 . . ?
C9 N3 V4 103.7(4) . . ?
C9 N3 H3C 111.0 . . ?
V4 N3 H3C 111.0 . . ?
C9 N3 H3D 111.0 . . ?
V4 N3 H3D 111.0 . . ?
H3C N3 H3D 109.0 . . ?
C13 N4 H4A 121(6) . . ?
C13 N4 H4B 118(6) . . ?
H4A N4 H4B 93(8) . . ?
N1 C1 C2 107.4(7) . . ?
N1 C1 C3 104.7(8) . . ?
C2 C1 C3 113.4(7) . . ?
N1 C1 C4 109.6(8) . . ?
C2 C1 C4 110.6(10) . . ?
C3 C1 C4 111.0(8) . . ?
O1 C2 C1 111.4(7) . . ?
O1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
O1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C1 109.0(6) . . ?
O2 C3 H3A 109.9 . . ?
C1 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C1 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
O3B C4 C1 106.2(16) . . ?
O3 C4 C1 107.0(10) . . ?
O3 C4 H4C 110.3 . . ?
C1 C4 H4C 110.3 . . ?
O3 C4 H4D 110.3 . . ?
C1 C4 H4D 110.3 . . ?
H4C C4 H4D 108.6 . . ?
O3B C4 H4E 110.5 . . ?
C1 C4 H4E 110.5 . . ?
O3B C4 H4F 110.5 . . ?
C1 C4 H4F 110.5 . . ?
H4E C4 H4F 108.7 . . ?
N2 C5 C6 107.2(6) . . ?
N2 C5 C7 105.2(6) . . ?
C6 C5 C7 111.1(6) . . ?
N2 C5 C8 112.7(6) . . ?
C6 C5 C8 110.1(6) . . ?
C7 C5 C8 110.5(6) . . ?
O4 C6 C5 108.8(6) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O5 C7 C5 108.2(6) . . ?
O5 C7 H7A 110.1 . . ?
C5 C7 H7A 110.1 . . ?
O5 C7 H7B 110.1 . . ?
C5 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O6 C8 C5 111.7(7) . . ?
O6 C8 H8A 109.3 . . ?
C5 C8 H8A 109.3 . . ?
O6 C8 H8B 109.3 . . ?
C5 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N3 C9 C10 107.8(6) . . ?
N3 C9 C11 105.8(6) . . ?
C10 C9 C11 111.3(7) . . ?
N3 C9 C12 112.6(7) . . ?
C10 C9 C12 109.1(7) . . ?
C11 C9 C12 110.2(7) . . ?
O7 C10 C9 109.2(6) . . ?
O7 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O7 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O8 C11 C9 108.7(6) . . ?
O8 C11 H11A 109.9 . . ?
C9 C11 H11A 109.9 . . ?
O8 C11 H11B 109.9 . . ?
C9 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O9 C12 C9 113.9(9) . . ?
O9B C12 C9 113.9(9) . . ?
O9 C12 H12A 108.8 . . ?
C9 C12 H12A 108.8 . . ?
O9 C12 H12B 108.8 . . ?
C9 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O9B C12 H12C 108.8 . . ?
C9 C12 H12C 108.8 . . ?
O9B C12 H12D 108.8 . . ?
C9 C12 H12D 108.8 . . ?
H12C C12 H12D 107.7 . . ?
N4 C13 C15 109.8(6) . . ?
N4 C13 C16 106.9(6) . . ?
C15 C13 C16 112.5(6) . . ?
N4 C13 C14 106.5(6) . . ?
C15 C13 C14 111.1(6) . . ?
C16 C13 C14 109.8(6) . . ?
O10 C14 C13 112.3(6) . . ?
O10 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
O10 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
O11 C15 C13 114.4(6) . . ?
O11 C15 H15A 108.7 . . ?
C13 C15 H15A 108.7 . . ?
O11 C15 H15B 108.7 . . ?
C13 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
O12 C16 C13 113.6(5) . . ?
O12 C16 H16A 108.9 . . ?
C13 C16 H16A 108.9 . . ?
O12 C16 H16B 108.9 . . ?
C13 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
O14 C17 O13 128.6(8) . . ?
O14 C17 C18 126.9(15) . . ?
O13 C17 C18 104.4(15) . . ?
O14 C17 H17A 115.7 . . ?
O13 C17 H17A 115.7 . . ?
H2E O2W H2F 115.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1W O1W H1C 105.3 2_656 . ?
O1W O1W H1D 114.4 2_656 . ?
H1C O1W H1D 115.9 . . ?
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 O18 1.594(5) . ?
V1 O12 2.005(5) . ?
V1 O11 2.011(5) . ?
V1 O7 2.028(5) . ?
V1 O5 2.040(4) . ?
V1 O23 2.304(4) . ?
V1 V5 3.0845(16) . ?
V2 O22 1.657(4) . ?
V2 O4 1.940(5) . ?
V2 O21 1.955(4) . ?
V2 O23 1.973(4) . ?
V2 N2 2.111(6) . ?
V2 O5 2.315(4) . ?
V2 V4 2.7503(16) . ?
V3 O17 1.588(6) . ?
V3 O21 1.947(4) . ?
V3 O22 2.011(4) 7_556 ?
V3 O2 2.075(4) . ?
V3 N1 2.091(6) . ?
V3 O1 2.331(6) . ?
V3 V5 2.9119(17) . ?
V4 O20 1.599(5) . ?
V4 O8 1.966(5) . ?
V4 O21 1.970(5) . ?
V4 O23 1.986(4) . ?
V4 N3 2.132(6) . ?
V4 O7 2.394(5) . ?
V5 O19 1.602(5) . ?
V5 O1 1.982(5) . ?
V5 O2 2.020(5) . ?
V5 O5 2.053(5) . ?
V5 O7 2.055(5) . ?
V5 O21 2.196(4) . ?
V6 O15 1.591(5) . ?
V6 O10 1.994(5) . ?
V6 O11 1.997(5) . ?
V6 O4 2.003(5) . ?
V6 O14 2.053(7) . ?
V6 O23 2.297(4) . ?
V7 O16 1.595(6) . ?
V7 O8 1.970(5) . ?
V7 O10 1.975(5) . ?
V7 O12 1.996(5) . ?
V7 O13 2.017(6) . ?
O1 C2 1.410(9) . ?
O2 C3 1.415(9) . ?
O3 C4 1.445(18) . ?
O3 H3E 0.8200 . ?
O3B C4 1.43(2) . ?
O3B H3F 0.8200 . ?
O4 C6 1.427(8) . ?
O5 C7 1.438(8) . ?
O6 C8 1.424(11) . ?
O6 H6C 0.8200 . ?
O7 C10 1.429(7) . ?
O8 C11 1.423(8) . ?
O9 C12 1.344(14) . ?
O9 H9A 0.8200 . ?
O9B C12 1.477(19) . ?
O9B H9B 0.8200 . ?
O10 C14 1.436(8) . ?
O11 C15 1.433(8) . ?
O12 C16 1.437(8) . ?
O13 C17 1.271(11) . ?
O14 C17 1.251(12) . ?
O22 V3 2.011(4) 7_556 ?
N1 C1 1.482(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C5 1.492(9) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N3 C9 1.494(9) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N4 C13 1.490(9) . ?
N4 H4A 0.894(10) . ?
N4 H4B 0.891(10) . ?
C1 C2 1.504(14) . ?
C1 C3 1.516(13) . ?
C1 C4 1.565(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 H4E 0.9700 . ?
C4 H4F 0.9700 . ?
C5 C6 1.521(10) . ?
C5 C7 1.527(9) . ?
C5 C8 1.535(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.518(12) . ?
C9 C11 1.523(11) . ?
C9 C12 1.542(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C12 H12D 0.9700 . ?
C13 C15 1.509(11) . ?
C13 C16 1.520(10) . ?
C13 C14 1.531(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.573(17) . ?
C17 H17A 0.9300 . ?
O2W H2E 0.8200 . ?
O2W H2F 0.8200 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O1W O1W 0.96(3) 2_656 ?
O1W H1C 0.8200 . ?
O1W H1D 0.8200 . ?
