#------------------------------------------------------------------------------
#$Date: 2017-05-06 01:09:07 +0300 (Sat, 06 May 2017) $
#$Revision: 196441 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/25/7042539.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_7042539
loop_
_publ_author_name
'Bayaguud, Aruuhan'
'Li, JianDa'
'She, Shan'
'Wei, Yongge'
_publ_section_title
;
 A simple synthetic route to polyoxovanadate-based organic-inorganic
 hybrids using EEDQ as an ester coupling agent.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4602
_journal_page_last               4608
_journal_paper_doi               10.1039/c7dt00274b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C24 H42 O29 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H114 N2 O29 V6'
_chemical_formula_weight         1585.13
_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   geom
_audit_creation_date             2016-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.504(3)
_cell_length_b                   17.740(4)
_cell_length_c                   15.324(3)
_cell_measurement_reflns_used    12190
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      29.1270
_cell_measurement_theta_min      1.9624
_cell_volume                     3478.5(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0586
_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)+(0.0683P)²+3.6987P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6264
_reflns_number_total             6820
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           qinshui
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_original_cell_volume        3478.5(13)
_cod_database_code               7042539
_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_max   0.847
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1E-C1D
 1.4 with sigma of 0.001
3. Rigid bond restraints
 C1F, C1H, C1I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1F \\sim C1H \\sim C1I: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Others
 Sof(H1FC)=Sof(H1FD)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=1-FVAR(1)
 Sof(H1FA)=Sof(H1FB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C7(H7A,H7B), C1(H1A,H1B), C2(H2A,
 H2B), C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B), C3(H3A,H3B), C4(H4A,H4B),
  C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C13(H13A,H13B), C16(H16A,H16B),
 C19(H19A,H19B), C1A(H1AA,H1AB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1F(H1FC,H1FD),
  C1G(H1GA,H1GB)
6.b Me refined with riding coordinates:
 C1D(H1DA,H1DB,H1DC), C1I(H1IA,H1IB,H1IC)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1H(H1HA,H1HB,
 H1HC)
;
_shelx_shelxl_version_number     2014/7
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45710(4) 0.11516(3) 0.03564(4) 0.03185(16) Uani 1 1 d . . . . .
V2 V 0.41041(4) -0.06187(3) 0.07882(4) 0.03268(16) Uani 1 1 d . . . . .
V3 V 0.37231(4) -0.00544(3) -0.13614(4) 0.03321(16) Uani 1 1 d . . . . .
O1 O 0.34153(16) 0.09302(12) -0.08132(15) 0.0309(5) Uani 1 1 d . . . . .
O2 O 0.53878(17) 0.14340(13) -0.03224(17) 0.0373(5) Uani 1 1 d . . . . .
O4 O 0.56955(17) 0.09630(14) 0.14031(16) 0.0380(5) Uani 1 1 d . . . . .
O5 O 0.5000 0.0000 0.0000 0.0266(6) Uani 1 2 d S T P . .
O6 O 0.37272(16) 0.04619(12) 0.09080(14) 0.0302(5) Uani 1 1 d . . . . .
O7 O 0.47029(18) 0.04758(14) -0.17243(15) 0.0383(5) Uani 1 1 d . . . . .
O8 O 0.40998(18) 0.19283(13) 0.05858(17) 0.0401(6) Uani 1 1 d . . . . .
C8 C 0.2657(2) 0.06485(19) 0.0773(2) 0.0333(7) Uani 1 1 d . . . . .
H8A H 0.2614 0.1164 0.0968 0.040 Uiso 1 1 calc R . . . .
H8B H 0.2387 0.0322 0.1152 0.040 Uiso 1 1 calc R . . . .
C11 C 0.2356(2) 0.10926(19) -0.0858(2) 0.0344(7) Uani 1 1 d . . . . .
H11A H 0.1901 0.1040 -0.1489 0.041 Uiso 1 1 calc R . . . .
H11B H 0.2311 0.1610 -0.0669 0.041 Uiso 1 1 calc R . . . .
C12 C 0.0845(2) 0.07606(18) -0.0305(2) 0.0321(7) Uani 1 1 d . . . . .
C14 C 0.1981(2) 0.05626(19) -0.0237(2) 0.0332(7) Uani 1 1 d . . . . .
O3 O 0.30285(16) -0.04987(12) -0.04921(15) 0.0314(5) Uani 1 1 d . . . . .
O9 O 0.27082(19) -0.00331(15) -0.22621(17) 0.0449(6) Uani 1 1 d . . . . .
O10 O 0.33127(19) -0.09881(14) 0.12561(18) 0.0428(6) Uani 1 1 d . . . . .
O11 O 0.02648(19) 0.09033(17) -0.11482(19) 0.0520(7) Uani 1 1 d . . . . .
O12 O 0.0544(2) 0.07509(18) 0.03572(19) 0.0561(7) Uani 1 1 d . . . . .
C9 C 0.1993(2) -0.02591(19) -0.0566(2) 0.0338(7) Uani 1 1 d . . . . .
H9A H 0.1711 -0.0588 -0.0199 0.041 Uiso 1 1 calc R . . . .
H9B H 0.1550 -0.0300 -0.1203 0.041 Uiso 1 1 calc R . . . .
O13 O -0.0759(2) 0.23553(18) -0.16463(19) 0.0580(8) Uani 1 1 d . . . . .
O14 O -0.1198(2) 0.39863(18) -0.1618(2) 0.0640(8) Uani 1 1 d . . . . .
O15 O -0.1567(3) 0.4962(2) -0.0209(3) 0.0755(10) Uani 1 1 d . . . . .
C7 C -0.1194(3) 0.1652(3) -0.2017(3) 0.0548(10) Uani 1 1 d . . . . .
H7A H -0.0971 0.1524 -0.2540 0.066 Uiso 1 1 calc R . . . .
H7B H -0.1951 0.1684 -0.2226 0.066 Uiso 1 1 calc R . . . .
C1 C -0.0840(3) 0.1064(3) -0.1294(3) 0.0556(11) Uani 1 1 d . . . . .
H1A H -0.0932 0.1239 -0.0725 0.067 Uiso 1 1 calc R . . . .
H1B H -0.1251 0.0609 -0.1487 0.067 Uiso 1 1 calc R . . . .
C2 C -0.1073(4) 0.4766(3) -0.1541(3) 0.0668(13) Uani 1 1 d . . . . .
H2A H -0.1151 0.4982 -0.2141 0.080 Uiso 1 1 calc R . . . .
H2B H -0.0377 0.4885 -0.1135 0.080 Uiso 1 1 calc R . . . .
C15 C -0.1878(4) 0.5100(3) -0.1160(4) 0.0693(13) Uani 1 1 d . . . . .
H15A H -0.1935 0.5639 -0.1276 0.083 Uiso 1 1 calc R . . . .
H15B H -0.2555 0.4873 -0.1459 0.083 Uiso 1 1 calc R . . . .
C17 C -0.0802(4) 0.2894(3) -0.2340(3) 0.0656(13) Uani 1 1 d . . . . .
H17A H -0.1516 0.2938 -0.2747 0.079 Uiso 1 1 calc R . . . .
H17B H -0.0375 0.2722 -0.2703 0.079 Uiso 1 1 calc R . . . .
C20 C -0.0425(4) 0.3649(3) -0.1939(3) 0.0653(12) Uani 1 1 d . . . . .
H20A H 0.0221 0.3594 -0.1432 0.078 Uiso 1 1 calc R . . . .
H20B H -0.0290 0.3967 -0.2403 0.078 Uiso 1 1 calc R . . . .
N1 N 0.7652(3) 0.29883(18) 0.0896(2) 0.0486(8) Uani 1 1 d . . . . .
C3 C 0.6991(3) 0.3585(2) 0.1147(3) 0.0538(10) Uani 1 1 d . . . . .
H3A H 0.6914 0.4007 0.0728 0.065 Uiso 1 1 calc R . . . .
H3B H 0.7359 0.3766 0.1762 0.065 Uiso 1 1 calc R . . . .
C4 C 0.8703(3) 0.3346(2) 0.0970(3) 0.0489(9) Uani 1 1 d . . . . .
H4A H 0.9042 0.3495 0.1605 0.059 Uiso 1 1 calc R . . . .
H4B H 0.8578 0.3800 0.0598 0.059 Uiso 1 1 calc R . . . .
C5 C 0.5904(4) 0.3321(3) 0.1118(4) 0.0679(13) Uani 1 1 d . . . . .
H5A H 0.5648 0.2971 0.0609 0.082 Uiso 1 1 calc R . . . .
H5B H 0.5974 0.3043 0.1680 0.082 Uiso 1 1 calc R . . . .
C6 C 0.7798(4) 0.2318(2) 0.1548(4) 0.0667(13) Uani 1 1 d . . . . .
H6A H 0.7119 0.2097 0.1472 0.080 Uiso 1 1 calc R . . . .
H6B H 0.8218 0.1941 0.1371 0.080 Uiso 1 1 calc R . . . .
C10 C 1.0496(3) 0.3217(3) 0.0862(3) 0.0600(11) Uani 1 1 d . . . . .
H10A H 1.0779 0.3328 0.1515 0.072 Uiso 1 1 calc R . . . .
H10B H 1.0405 0.3691 0.0529 0.072 Uiso 1 1 calc R . . . .
C13 C 0.7126(4) 0.2702(3) -0.0076(3) 0.0596(12) Uani 1 1 d . . . . .
H13A H 0.6495 0.2434 -0.0092 0.071 Uiso 1 1 calc R . . . .
H13B H 0.7589 0.2345 -0.0230 0.071 Uiso 1 1 calc R . . . .
C16 C 0.9450(3) 0.2837(2) 0.0667(3) 0.0564(10) Uani 1 1 d . . . . .
H16A H 0.9536 0.2362 0.0996 0.068 Uiso 1 1 calc R . . . .
H16B H 0.9157 0.2732 0.0013 0.068 Uiso 1 1 calc R . . . .
C18 C 1.1273(4) 0.2719(3) 0.0576(4) 0.0708(13) Uani 1 1 d . . . . .
H18A H 1.1354 0.2246 0.0896 0.106 Uiso 1 1 calc GR . . . .
H18B H 1.1937 0.2969 0.0730 0.106 Uiso 1 1 calc GR . . . .
H18C H 1.1013 0.2631 -0.0076 0.106 Uiso 1 1 calc GR . . . .
C19 C 0.6842(4) 0.3316(3) -0.0806(3) 0.0659(13) Uani 1 1 d . . . . .
H19A H 0.6345 0.3659 -0.0679 0.079 Uiso 1 1 calc R . . . .
H19B H 0.7465 0.3602 -0.0776 0.079 Uiso 1 1 calc R . . . .
C1A C 0.6377(4) 0.2996(4) -0.1760(4) 0.0864(18) Uani 1 1 d . . . . .
H1AA H 0.6896 0.2689 -0.1906 0.104 Uiso 1 1 calc R . . . .
H1AB H 0.5792 0.2673 -0.1773 0.104 Uiso 1 1 calc R . . . .
C1B C -0.2173(5) 0.5370(3) 0.0234(5) 0.0915(18) Uani 1 1 d . . . . .
H1BA H -0.2122 0.5900 0.0127 0.137 Uiso 1 1 calc GR . . . .
H1BB H -0.1917 0.5273 0.0884 0.137 Uiso 1 1 calc GR . . . .
H1BC H -0.2890 0.5215 -0.0008 0.137 Uiso 1 1 calc GR . . . .
C1C C 0.6011(5) 0.3594(4) -0.2469(4) 0.098(2) Uani 1 1 d . . . . .
H1CA H 0.5501 0.3903 -0.2324 0.147 Uiso 1 1 calc GR . . . .
H1CB H 0.5702 0.3366 -0.3062 0.147 Uiso 1 1 calc GR . . . .
H1CC H 0.6593 0.3901 -0.2479 0.147 Uiso 1 1 calc GR . . . .
C1D C 0.5298(5) 0.4626(4) 0.1365(7) 0.157(4) Uani 1 1 d D . . . .
H1DA H 0.4643 0.4889 0.1204 0.235 Uiso 1 1 calc R . . . .
H1DB H 0.5603 0.4613 0.2023 0.235 Uiso 1 1 calc R . . . .
H1DC H 0.5762 0.4882 0.1103 0.235 Uiso 1 1 calc R . . . .
C1E C 0.5132(6) 0.3890(3) 0.1024(7) 0.149(4) Uani 1 1 d D . . . .
H1EA H 0.4781 0.3940 0.0367 0.179 Uiso 1 1 calc R . . . .
H1EB H 0.4623 0.3674 0.1277 0.179 Uiso 1 1 calc R . . . .
C1F C 0.8358(6) 0.1787(4) 0.3120(5) 0.113(2) Uani 1 1 d . U . . .
H1FA H 0.7660 0.1574 0.2926 0.136 Uiso 0.511(8) 1 calc R . . A 1
H1FB H 0.8799 0.1433 0.2933 0.136 Uiso 0.511(8) 1 calc R . . A 1
H1FC H 0.8377 0.1346 0.2753 0.136 Uiso 0.489(8) 1 calc R . . A 2
H1FD H 0.8990 0.1793 0.3648 0.136 Uiso 0.489(8) 1 calc R . . A 2
C1G C 0.8306(6) 0.2501(4) 0.2544(4) 0.100(2) Uani 1 1 d . . . . .
H1GA H 0.7906 0.2886 0.2733 0.120 Uiso 1 1 calc R . . . .
H1GB H 0.9005 0.2693 0.2642 0.120 Uiso 1 1 calc R . . . .
C1H C 0.7496(12) 0.1755(8) 0.3413(10) 0.112(2) Uani 0.511(8) 1 d . U . A 2
H1HA H 0.7106 0.2216 0.3253 0.168 Uiso 0.511(8) 1 calc GR . . A 2
H1HB H 0.7717 0.1690 0.4069 0.168 Uiso 0.511(8) 1 calc GR . . A 2
H1HC H 0.7062 0.1338 0.3122 0.168 Uiso 0.511(8) 1 calc GR . . A 2
C1I C 0.8656(13) 0.1788(8) 0.3957(10) 0.112(2) Uani 0.489(8) 1 d . U . A 1
H1IA H 0.8626 0.1284 0.4177 0.168 Uiso 0.489(8) 1 calc R . . A 1
H1IB H 0.9362 0.1969 0.4181 0.168 Uiso 0.489(8) 1 calc R . . A 1
H1IC H 0.8213 0.2110 0.4174 0.168 Uiso 0.489(8) 1 calc R . . A 1
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
V2 V1 V3 66.45(2) 3_655 3_655
O1 V1 V2 81.73(6) . 3_655
O1 V1 V3 125.20(7) . 3_655
O1 V1 O5 77.94(6) . .
O1 V1 O6 82.76(9) . .
O2 V1 V2 34.24(7) . 3_655
O2 V1 V3 88.05(8) . 3_655
O2 V1 O1 89.06(10) . .
O2 V1 O4 93.78(11) . .
O2 V1 O5 81.93(8) . .
O2 V1 O6 158.57(10) . .
O4 V1 V2 88.43(7) . 3_655
O4 V1 V3 33.41(7) . 3_655
O4 V1 O1 158.04(10) . .
O4 V1 O5 80.91(7) . .
O4 V1 O6 86.82(10) . .
O5 V1 V2 47.703(15) . 3_655
O5 V1 V3 47.50(2) . 3_655
O6 V1 V2 124.52(7) . 3_655
O6 V1 V3 80.69(6) . 3_655
O6 V1 O5 77.00(6) . .
O8 V1 V2 138.11(9) . 3_655
O8 V1 V3 136.93(9) . 3_655
O8 V1 O1 96.57(11) . .
O8 V1 O2 104.20(12) . .
O8 V1 O4 103.79(12) . .
O8 V1 O5 171.83(9) . .
O8 V1 O6 96.42(11) . .
V3 V2 V1 66.04(2) 3_655 3_655
O2 V2 V1 33.66(7) 3_655 3_655
O2 V2 V3 88.60(7) 3_655 3_655
O2 V2 O5 81.03(7) 3_655 .
O2 V2 O6 157.42(10) 3_655 .
O2 V2 O3 87.03(10) 3_655 .
O5 V2 V1 47.382(19) . 3_655
O5 V2 V3 47.58(2) . 3_655
O6 V2 V1 124.40(6) . 3_655
O6 V2 V3 81.22(6) . 3_655
O6 V2 O5 77.22(6) . .
O6 V2 O3 82.25(9) . .
O7 V2 V1 87.80(8) 3_655 3_655
O7 V2 V3 34.45(7) 3_655 3_655
O7 V2 O2 94.02(11) 3_655 3_655
O7 V2 O5 82.03(8) 3_655 .
O7 V2 O6 88.92(10) 3_655 .
O7 V2 O3 158.46(10) 3_655 .
O3 V2 V1 81.19(6) . 3_655
O3 V2 V3 124.25(7) . 3_655
O3 V2 O5 76.88(6) . .
O10 V2 V1 137.06(10) . 3_655
O10 V2 V3 138.92(10) . 3_655
O10 V2 O2 103.67(12) . 3_655
O10 V2 O5 171.21(9) . .
O10 V2 O6 97.16(11) . .
O10 V2 O7 104.81(12) . 3_655
O10 V2 O3 95.79(11) . .
V2 V3 V1 66.25(3) 3_655 3_655
O1 V3 V1 124.24(7) . 3_655
O1 V3 V2 81.30(6) . 3_655
O1 V3 O5 77.13(6) . .
O4 V3 V1 34.47(7) 3_655 3_655
O4 V3 V2 88.29(7) 3_655 3_655
O4 V3 O1 158.34(10) 3_655 .
O4 V3 O5 81.80(7) 3_655 .
O4 V3 O7 94.74(11) 3_655 .
O4 V3 O3 88.50(10) 3_655 .
O5 V3 V1 47.34(2) . 3_655
O5 V3 V2 47.74(2) . 3_655
O7 V3 V1 88.78(8) . 3_655
O7 V3 V2 33.44(7) . 3_655
O7 V3 O1 87.01(10) . .
O7 V3 O5 81.17(7) . .
O7 V3 O3 157.79(10) . .
O3 V3 V1 81.49(7) . 3_655
O3 V3 V2 125.06(7) . 3_655
O3 V3 O1 82.16(9) . .
O3 V3 O5 77.54(6) . .
O9 V3 V1 138.86(10) . 3_655
O9 V3 V2 136.27(10) . 3_655
O9 V3 O1 95.95(11) . .
O9 V3 O4 104.62(12) . 3_655
O9 V3 O5 171.80(9) . .
O9 V3 O7 103.06(12) . .
O9 V3 O3 97.33(12) . .
V1 O1 V3 109.49(10) . .
C11 O1 V1 118.78(19) . .
C11 O1 V3 118.85(19) . .
V1 O2 V2 112.10(12) . 3_655
V3 O4 V1 112.11(12) 3_655 .
V1 O5 V1 180.0 3_655 .
V1 O5 V2 95.09(2) . .
V1 O5 V2 84.91(2) 3_655 .
V1 O5 V2 84.91(2) . 3_655
V1 O5 V2 95.09(2) 3_655 3_655
V1 O5 V3 94.83(2) . .
V1 O5 V3 94.83(2) 3_655 3_655
V1 O5 V3 85.17(2) . 3_655
V1 O5 V3 85.17(2) 3_655 .
V2 O5 V2 180.0 3_655 .
V3 O5 V2 95.33(3) . .
V3 O5 V2 84.67(3) . 3_655
V3 O5 V2 84.67(3) 3_655 .
V3 O5 V2 95.33(3) 3_655 3_655
V3 O5 V3 180.0 . 3_655
V2 O6 V1 110.18(10) . .
C8 O6 V1 118.37(19) . .
C8 O6 V2 118.77(19) . .
V2 O7 V3 112.11(12) 3_655 .
O6 C8 H8A 109.3 . .
O6 C8 H8B 109.3 . .
O6 C8 C14 111.8(2) . .
H8A C8 H8B 107.9 . .
C14 C8 H8A 109.3 . .
C14 C8 H8B 109.3 . .
O1 C11 H11A 109.3 . .
O1 C11 H11B 109.3 . .
O1 C11 C14 111.6(3) . .
H11A C11 H11B 108.0 . .
C14 C11 H11A 109.3 . .
C14 C11 H11B 109.3 . .
O11 C12 C14 112.3(3) . .
O12 C12 C14 122.3(3) . .
O12 C12 O11 125.3(3) . .
C8 C14 C11 110.9(3) . .
C8 C14 C12 107.7(3) . .
C8 C14 C9 111.0(3) . .
C11 C14 C12 109.7(3) . .
C11 C14 C9 109.6(3) . .
C12 C14 C9 107.9(3) . .
V3 O3 V2 109.66(10) . .
C9 O3 V2 118.91(19) . .
C9 O3 V3 118.69(19) . .
C12 O11 C1 116.7(3) . .
C14 C9 H9A 109.3 . .
C14 C9 H9B 109.3 . .
O3 C9 C14 111.5(2) . .
O3 C9 H9A 109.3 . .
O3 C9 H9B 109.3 . .
H9A C9 H9B 108.0 . .
C17 O13 C7 112.3(3) . .
C2 O14 C20 111.4(4) . .
C15 O15 C1B 112.4(4) . .
O13 C7 H7A 109.9 . .
O13 C7 H7B 109.9 . .
O13 C7 C1 109.1(3) . .
H7A C7 H7B 108.3 . .
C1 C7 H7A 109.9 . .
C1 C7 H7B 109.9 . .
O11 C1 C7 108.7(3) . .
O11 C1 H1A 110.0 . .
O11 C1 H1B 110.0 . .
C7 C1 H1A 110.0 . .
C7 C1 H1B 110.0 . .
H1A C1 H1B 108.3 . .
O14 C2 H2A 109.7 . .
O14 C2 H2B 109.7 . .
O14 C2 C15 109.9(4) . .
H2A C2 H2B 108.2 . .
C15 C2 H2A 109.7 . .
C15 C2 H2B 109.7 . .
O15 C15 C2 108.6(4) . .
O15 C15 H15A 110.0 . .
O15 C15 H15B 110.0 . .
C2 C15 H15A 110.0 . .
C2 C15 H15B 110.0 . .
H15A C15 H15B 108.3 . .
O13 C17 H17A 109.3 . .
O13 C17 H17B 109.3 . .
O13 C17 C20 111.6(4) . .
H17A C17 H17B 108.0 . .
C20 C17 H17A 109.3 . .
C20 C17 H17B 109.3 . .
O14 C20 C17 109.2(4) . .
O14 C20 H20A 109.8 . .
O14 C20 H20B 109.8 . .
C17 C20 H20A 109.8 . .
C17 C20 H20B 109.8 . .
H20A C20 H20B 108.3 . .
C3 N1 C4 107.5(3) . .
C3 N1 C6 110.0(3) . .
C3 N1 C13 110.8(3) . .
C4 N1 C6 110.7(3) . .
C13 N1 C4 110.2(3) . .
C13 N1 C6 107.8(3) . .
N1 C3 H3A 108.6 . .
N1 C3 H3B 108.6 . .
N1 C3 C5 114.7(4) . .
H3A C3 H3B 107.6 . .
C5 C3 H3A 108.6 . .
C5 C3 H3B 108.6 . .
N1 C4 H4A 108.6 . .
N1 C4 H4B 108.6 . .
N1 C4 C16 114.7(3) . .
H4A C4 H4B 107.6 . .
C16 C4 H4A 108.6 . .
C16 C4 H4B 108.6 . .
C3 C5 H5A 108.1 . .
C3 C5 H5B 108.1 . .
H5A C5 H5B 107.3 . .
C1E C5 C3 116.8(5) . .
C1E C5 H5A 108.1 . .
C1E C5 H5B 108.1 . .
N1 C6 H6A 108.5 . .
N1 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C1G C6 N1 115.0(4) . .
C1G C6 H6A 108.5 . .
C1G C6 H6B 108.5 . .
H10A C10 H10B 108.0 . .
C16 C10 H10A 109.3 . .
C16 C10 H10B 109.3 . .
C16 C10 C18 111.6(4) . .
C18 C10 H10A 109.3 . .
C18 C10 H10B 109.3 . .
N1 C13 H13A 108.7 . .
N1 C13 H13B 108.7 . .
N1 C13 C19 114.3(4) . .
H13A C13 H13B 107.6 . .
C19 C13 H13A 108.7 . .
C19 C13 H13B 108.7 . .
C4 C16 H16A 109.7 . .
C4 C16 H16B 109.7 . .
C10 C16 C4 110.0(4) . .
C10 C16 H16A 109.7 . .
C10 C16 H16B 109.7 . .
H16A C16 H16B 108.2 . .
C10 C18 H18A 109.5 . .
C10 C18 H18B 109.5 . .
C10 C18 H18C 109.5 . .
H18A C18 H18B 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C13 C19 H19A 109.2 . .
C13 C19 H19B 109.2 . .
H19A C19 H19B 107.9 . .
C1A C19 C13 111.9(4) . .
C1A C19 H19A 109.2 . .
C1A C19 H19B 109.2 . .
C19 C1A H1AA 109.2 . .
C19 C1A H1AB 109.2 . .
H1AA C1A H1AB 107.9 . .
C1C C1A C19 112.3(5) . .
C1C C1A H1AA 109.2 . .
C1C C1A H1AB 109.2 . .
O15 C1B H1BA 109.5 . .
O15 C1B H1BB 109.5 . .
O15 C1B H1BC 109.5 . .
H1BA C1B H1BB 109.5 . .
H1BA C1B H1BC 109.5 . .
H1BB C1B H1BC 109.5 . .
C1A C1C H1CA 109.5 . .
C1A C1C H1CB 109.5 . .
C1A C1C H1CC 109.5 . .
H1CA C1C H1CB 109.5 . .
H1CA C1C H1CC 109.5 . .
H1CB C1C H1CC 109.5 . .
H1DA C1D H1DB 109.5 . .
H1DA C1D H1DC 109.5 . .
H1DB C1D H1DC 109.5 . .
C1E C1D H1DA 109.5 . .
C1E C1D H1DB 109.5 . .
C1E C1D H1DC 109.5 . .
C5 C1E H1EA 105.6 . .
C5 C1E H1EB 105.6 . .
C1D C1E C5 126.8(7) . .
C1D C1E H1EA 105.6 . .
C1D C1E H1EB 105.6 . .
H1EA C1E H1EB 106.1 . .
H1FA C1F H1FB 106.5 . .
H1FC C1F H1FD 108.2 . .
C1G C1F H1FA 106.6 . .
C1G C1F H1FB 106.6 . .
C1G C1F H1FC 109.8 . .
C1G C1F H1FD 109.8 . .
C1H C1F H1FC 109.8 . .
C1H C1F H1FD 109.8 . .
C1H C1F C1G 109.5(8) . .
C1I C1F H1FA 106.6 . .
C1I C1F H1FB 106.6 . .
C1I C1F C1G 123.1(10) . .
C6 C1G C1F 109.3(6) . .
C6 C1G H1GA 109.8 . .
C6 C1G H1GB 109.8 . .
C1F C1G H1GA 109.8 . .
C1F C1G H1GB 109.8 . .
H1GA C1G H1GB 108.3 . .
C1F C1H H1HA 109.5 . .
C1F C1H H1HB 109.5 . .
C1F C1H H1HC 109.5 . .
H1HA C1H H1HB 109.5 . .
H1HA C1H H1HC 109.5 . .
H1HB C1H H1HC 109.5 . .
C1F C1I H1IA 109.5 . .
C1F C1I H1IB 109.5 . .
C1F C1I H1IC 109.5 . .
H1IA C1I H1IB 109.5 . .
H1IA C1I H1IC 109.5 . .
H1IB C1I H1IC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 V2 3.0295(10) 3_655
V1 V3 3.0331(11) 3_655
V1 O1 2.004(2) .
V1 O2 1.812(2) .
V1 O4 1.853(2) .
V1 O5 2.2382(7) .
V1 O6 2.031(2) .
V1 O8 1.603(2) .
V2 V1 3.0296(10) 3_655
V2 V3 3.0264(10) 3_655
V2 O2 1.840(2) 3_655
V2 O5 2.2498(7) .
V2 O6 2.007(2) .
V2 O7 1.800(2) 3_655
V2 O3 2.045(2) .
V2 O10 1.605(2) .
V3 V1 3.0330(10) 3_655
V3 V2 3.0264(10) 3_655
V3 O1 2.038(2) .
V3 O4 1.803(2) 3_655
V3 O5 2.2440(10) .
V3 O7 1.848(2) .
V3 O3 2.018(2) .
V3 O9 1.605(2) .
O1 C11 1.440(4) .
O2 V2 1.840(2) 3_655
O4 V3 1.803(2) 3_655
O5 V1 2.2382(7) 3_655
O5 V2 2.2497(7) 3_655
O5 V3 2.2441(10) 3_655
O6 C8 1.432(4) .
O7 V2 1.800(2) 3_655
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C14 1.532(4) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 C14 1.534(5) .
C12 C14 1.544(4) .
C12 O11 1.305(4) .
C12 O12 1.207(4) .
C14 C9 1.544(5) .
O3 C9 1.431(4) .
O11 C1 1.464(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
O13 C7 1.417(5) .
O13 C17 1.417(5) .
O14 C2 1.394(6) .
O14 C20 1.419(5) .
O15 C15 1.404(6) .
O15 C1B 1.418(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C1 1.486(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C15 1.509(7) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 C20 1.494(7) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
N1 C3 1.512(5) .
N1 C4 1.524(5) .
N1 C6 1.525(5) .
N1 C13 1.518(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 C5 1.528(6) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C16 1.533(6) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C1E 1.425(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C1G 1.495(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 C16 1.507(6) .
C10 C18 1.539(6) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C19 1.520(7) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19 C1A 1.506(6) .
C1A H1AA 0.9700 .
C1A H1AB 0.9700 .
C1A C1C 1.487(9) .
C1B H1BA 0.9600 .
C1B H1BB 0.9600 .
C1B H1BC 0.9600 .
C1C H1CA 0.9600 .
C1C H1CB 0.9600 .
C1C H1CC 0.9600 .
C1D H1DA 0.9600 .
C1D H1DB 0.9600 .
C1D H1DC 0.9600 .
C1D C1E 1.3981(11) .
C1E H1EA 0.9700 .
C1E H1EB 0.9700 .
C1F H1FA 0.9700 .
C1F H1FB 0.9700 .
C1F H1FC 0.9700 .
C1F H1FD 0.9700 .
C1F C1G 1.531(8) .
C1F C1H 1.377(13) .
C1F C1I 1.216(15) .
C1G H1GA 0.9700 .
C1G H1GB 0.9700 .
C1H H1HA 0.9600 .
C1H H1HB 0.9600 .
C1H H1HC 0.9600 .
C1I H1IA 0.9600 .
C1I H1IB 0.9600 .
C1I H1IC 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
V1 V3 O7 V2 -45.66(12) 3_655 3_655
V1 O1 C11 C14 -68.8(3) . .
V1 O6 C8 C14 68.1(3) . .
V2 V1 O4 V3 -46.83(11) 3_655 3_655
V2 O6 C8 C14 -69.9(3) . .
V2 O3 C9 C14 67.3(3) . .
V3 V1 O2 V2 48.66(11) 3_655 3_655
V3 O1 C11 C14 68.7(3) . .
V3 O3 C9 C14 -70.5(3) . .
O1 V1 O2 V2 -76.61(13) . 3_655
O1 V1 O4 V3 16.2(3) . 3_655
O1 V3 O7 V2 78.71(13) . 3_655
O1 C11 C14 C8 61.0(3) . .
O1 C11 C14 C12 179.8(2) . .
O1 C11 C14 C9 -62.0(3) . .
O2 V1 O4 V3 -80.67(14) . 3_655
O4 V1 O2 V2 81.60(13) . 3_655
O4 V3 O7 V2 -79.65(14) 3_655 3_655
O5 V1 O2 V2 1.35(10) . 3_655
O5 V1 O4 V3 0.53(10) . 3_655
O5 V3 O7 V2 1.29(11) . 3_655
O6 V1 O2 V2 -9.3(3) . 3_655
O6 V1 O4 V3 77.87(13) . 3_655
O6 C8 C14 C11 -61.1(3) . .
O6 C8 C14 C12 178.9(3) . .
O6 C8 C14 C9 61.0(3) . .
O8 V1 O2 V2 -173.14(13) . 3_655
O8 V1 O4 V3 173.70(13) . 3_655
C8 C14 C9 O3 -60.0(3) . .
C11 C14 C9 O3 62.9(3) . .
C12 C14 C9 O3 -177.8(3) . .
C12 O11 C1 C7 143.4(4) . .
C14 C12 O11 C1 177.3(3) . .
O3 V3 O7 V2 18.0(3) . 3_655
O9 V3 O7 V2 174.14(14) . 3_655
O11 C12 C14 C8 162.7(3) . .
O11 C12 C14 C11 41.9(4) . .
O11 C12 C14 C9 -77.4(4) . .
O12 C12 C14 C8 -20.0(4) . .
O12 C12 C14 C11 -140.7(3) . .
O12 C12 C14 C9 99.9(4) . .
O12 C12 O11 C1 0.0(6) . .
O13 C7 C1 O11 -72.7(4) . .
O13 C17 C20 O14 -74.2(5) . .
O14 C2 C15 O15 76.7(5) . .
C7 O13 C17 C20 175.1(4) . .
C2 O14 C20 C17 -159.0(4) . .
C17 O13 C7 C1 162.9(3) . .
C20 O14 C2 C15 -177.6(4) . .
N1 C3 C5 C1E -158.5(6) . .
N1 C4 C16 C10 -174.2(3) . .
N1 C6 C1G C1F 177.5(4) . .
N1 C13 C19 C1A 176.9(4) . .
C3 N1 C4 C16 -175.5(3) . .
C3 N1 C6 C1G -58.9(5) . .
C3 N1 C13 C19 54.9(4) . .
C3 C5 C1E C1D -32.1(13) . .
C4 N1 C3 C5 -179.4(4) . .
C4 N1 C6 C1G 59.7(5) . .
C4 N1 C13 C19 -63.9(5) . .
C6 N1 C3 C5 -58.9(5) . .
C6 N1 C4 C16 64.4(4) . .
C6 N1 C13 C19 175.2(4) . .
C13 N1 C3 C5 60.1(5) . .
C13 N1 C4 C16 -54.7(5) . .
C13 N1 C6 C1G -179.7(4) . .
C13 C19 C1A C1C 175.0(5) . .
C18 C10 C16 C4 179.4(4) . .
C1B O15 C15 C2 169.3(4) . .
C1H C1F C1G C6 -93.5(10) . .
C1I C1F C1G C6 -173.8(10) . .
