#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/74/4107440.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_4107440
loop_
_publ_author_name
'Christophe Aronica'
'Guillaume Chastanet'
'Ekaterina Zueva'
'Serguei A. Borshch'
'Juan M. Clemente-Juan'
'Dominique Luneau'
_publ_section_title
;
 A Mixed-Valence Polyoxovanadate(III,IV) Cluster with a Calixarene Cap
 Exhibiting Ferromagnetic V(III)-V(IV) Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2365
_journal_page_last               2371
_journal_paper_doi               10.1021/ja078030q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C59 H96 N1 O19 V6'
_chemical_formula_sum            'C59 H96 N O19 V6'
_chemical_formula_weight         1429.04
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-07-12
_audit_creation_method           CRYSTALS_ver_12.50
_cell_angle_alpha                90
_cell_angle_beta                 104.546(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.805(5)
_cell_length_b                   15.638(5)
_cell_length_c                   15.833(5)
_cell_measurement_reflns_used    7316
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0
_cell_volume                     6903(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13928
_diffrn_reflns_theta_full        25.683
_diffrn_reflns_theta_max         27.916
_diffrn_reflns_theta_min         1.329
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_correction_T_min  0.9190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       square
_exptl_crystal_F_000             2491
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1063
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000201
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.09 0.871 0.774 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0964
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0594
_reflns_limit_h_max              36
_reflns_limit_h_min              -37
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4100
_reflns_number_total             8430
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ja078030q-file003.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'C 1 2/m 1 '
_cod_original_formula_sum        'C59 H96 N1 O19 V6'
_cod_database_code               4107440
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z
x,-y,z
-x+1/2,y+1/2,-z
x+1/2,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
V1 V 0.24564(3) 0.0000 0.25095(5) 0.0345 1.0000 Uani S T
V2 V 0.08705(3) 0.0000 0.18237(6) 0.0446 1.0000 Uani S T
V3 V 0.16837(3) 0.0000 0.06809(5) 0.0419 1.0000 Uani S T
V4 V 0.17097(3) 0.0000 0.36707(5) 0.0400 1.0000 Uani S T
V5 V 0.16954(2) -0.15057(4) 0.21734(4) 0.0417 1.0000 Uani . .
N1 N 0.75087(18) 0.0000 0.2495(3) 0.0598 1.0000 Uani S T
O1 O 0.17265(12) 0.0000 0.2192(2) 0.0382 1.0000 Uani S T
O2 O 0.02958(14) 0.0000 0.1603(3) 0.0607 1.0000 Uani S T
O3 O 0.32369(14) 0.0000 0.2834(3) 0.0645 1.0000 Uani S T
O4 O 0.17029(15) 0.0000 -0.0326(3) 0.0604 1.0000 Uani S T
O5 O 0.17399(15) 0.0000 0.4692(2) 0.0565 1.0000 Uani S T
O6 O 0.17153(11) -0.25269(19) 0.2185(2) 0.0618 1.0000 Uani . .
O7 O 0.24083(12) 0.0000 0.1261(2) 0.0393 1.0000 Uani S T
O8 O 0.24349(12) 0.0000 0.3730(2) 0.0380 1.0000 Uani S T
O9 O 0.24214(8) -0.12486(16) 0.24908(15) 0.0382 1.0000 Uani . .
O10 O 0.09919(13) 0.0000 0.0620(2) 0.0510 1.0000 Uani S T
O12 O 0.10111(12) 0.0000 0.3138(2) 0.0491 1.0000 Uani S T
O11 O 0.09959(10) -0.12718(19) 0.18778(19) 0.0519 1.0000 Uani . .
O13 O 0.16907(9) -0.12609(18) 0.09273(16) 0.0457 1.0000 Uani . .
O14 O 0.17112(9) -0.12593(17) 0.34264(17) 0.0451 1.0000 Uani . .
C1 C 0.28150(17) 0.0000 0.0962(3) 0.0418 1.0000 Uani S T
C2 C 0.30274(13) 0.0784(3) 0.0851(2) 0.0450 1.0000 Uani . .
C3 C 0.34528(15) 0.0760(3) 0.0590(3) 0.0548 1.0000 Uani . .
C4 C 0.3676(2) 0.0000 0.0457(4) 0.0547 1.0000 Uani S T
C5 C 0.4160(2) 0.0000 0.0219(6) 0.0757 1.0000 Uani S T
C6 C 0.4201(5) -0.0733(8) -0.0339(13) 0.2388 1.0000 Uani . .
C7 C 0.4531(3) 0.0000 0.1016(9) 0.2423 1.0000 Uani S T
C8 C 0.28203(13) 0.1632(3) 0.1052(2) 0.0455 1.0000 Uani . .
C9 C 0.28338(12) -0.1718(2) 0.2669(2) 0.0408 1.0000 Uani . .
C10 C 0.30432(13) -0.1927(2) 0.1980(2) 0.0450 1.0000 Uani . .
C11 C 0.34756(14) -0.2367(3) 0.2183(3) 0.0508 1.0000 Uani . .
C12 C 0.37119(14) -0.2598(3) 0.3030(3) 0.0519 1.0000 Uani . .
C13 C 0.35002(14) -0.2361(3) 0.3693(3) 0.0502 1.0000 Uani . .
C14 C 0.30626(13) -0.1921(2) 0.3531(2) 0.0430 1.0000 Uani . .
C15 C 0.42011(16) -0.3068(4) 0.3228(4) 0.0705 1.0000 Uani . .
C16 C 0.4277(4) -0.3611(9) 0.4001(7) 0.1825 1.0000 Uani . .
C17 C 0.4584(3) -0.2427(7) 0.3398(13) 0.2427 1.0000 Uani . .
C18 C 0.4244(4) -0.3638(9) 0.2515(7) 0.1977 1.0000 Uani . .
C19 C 0.28628(13) -0.1622(2) 0.4285(2) 0.0428 1.0000 Uani . .
C20 C 0.28528(18) 0.0000 0.4384(3) 0.0375 1.0000 Uani S T
C21 C 0.30736(13) 0.0779(2) 0.4674(2) 0.0417 1.0000 Uani . .
C22 C 0.35121(13) 0.0761(3) 0.5311(2) 0.0471 1.0000 Uani . .
C23 C 0.37311(19) 0.0000 0.5640(4) 0.0488 1.0000 Uani S T
C24 C 0.4219(2) 0.0000 0.6326(4) 0.0632 1.0000 Uani S T
C25 C 0.4603(4) 0.0000 0.5879(10) 0.2531 1.0000 Uani S T
C26 C 0.4276(4) -0.0740(7) 0.6913(8) 0.2007 1.0000 Uani . .
C27 C 0.0653(3) 0.0000 0.3593(5) 0.0882 1.0000 Uani S T
C28 C 0.0628(2) 0.0000 -0.0151(5) 0.0877 1.0000 Uani S T
C29 C 0.0635(2) -0.1875(4) 0.1652(5) 0.0966 1.0000 Uani . .
C30 C 0.14471(18) -0.1800(3) 0.3850(3) 0.0671 1.0000 Uani . .
C31 C 0.14388(19) -0.1815(4) 0.0263(3) 0.0692 1.0000 Uani . .
C32 C 0.3701(3) 0.0000 0.3055(8) 0.1169 1.0000 Uani S T
C33 C 0.7814(4) 0.0573(8) 0.3210(7) 0.0784 0.5000 Uani . .
C34 C 0.7492(3) 0.1127(5) 0.3620(6) 0.0546 0.5000 Uani . .
C35 C 0.7832(5) -0.0509(9) 0.2069(8) 0.0919 0.5000 Uani . .
C36 C 0.7530(4) -0.1089(7) 0.1375(6) 0.0756 0.5000 Uani . .
C37 C 0.7179(5) -0.0620(8) 0.1828(8) 0.0929 0.5000 Uani . .
C38 C 0.7174(5) -0.0579(8) 0.2837(10) 0.0899 0.5000 Uani . .
H181 H 0.4566 -0.3918 0.2627 0.2044 1.0000 Uiso . .
H182 H 0.3986 -0.4064 0.2352 0.2044 1.0000 Uiso . .
H183 H 0.4221 -0.3262 0.1945 0.2044 1.0000 Uiso . .
H171 H 0.4909 -0.2688 0.3557 0.2651 1.0000 Uiso . .
H172 H 0.4560 -0.2054 0.3939 0.2651 1.0000 Uiso . .
H173 H 0.4556 -0.2019 0.2906 0.2651 1.0000 Uiso . .
H161 H 0.4585 -0.3931 0.4105 0.2105 1.0000 Uiso . .
H162 H 0.4251 -0.3297 0.4524 0.2105 1.0000 Uiso . .
H163 H 0.4006 -0.4083 0.3887 0.2105 1.0000 Uiso . .
H92 H 0.3664 -0.2519 0.4317 0.0589 1.0000 Uiso . .
H94 H 0.3621 -0.2518 0.1687 0.0595 1.0000 Uiso . .
H191 H 0.2931 -0.2068 0.4759 0.0512 1.0000 Uiso . .
H192 H 0.2504 -0.1559 0.4069 0.0512 1.0000 Uiso . .
H81 H 0.2882 0.2073 0.0628 0.0563 1.0000 Uiso . .
H82 H 0.2465 0.1570 0.0966 0.0563 1.0000 Uiso . .
H281 H 0.0311 -0.1599 0.1524 0.1155 1.0000 Uiso . .
H282 H 0.0661 -0.2308 0.2125 0.1155 1.0000 Uiso . .
H283 H 0.0663 -0.2190 0.1101 0.1155 1.0000 Uiso . .
H301 H 0.1467 -0.1606 -0.0325 0.0862 1.0000 Uiso . .
H302 H 0.1567 -0.2407 0.0358 0.0862 1.0000 Uiso . .
H303 H 0.1087 -0.1822 0.0257 0.0862 1.0000 Uiso . .
H311 H 0.1482 -0.1611 0.4464 0.0847 1.0000 Uiso . .
H312 H 0.1563 -0.2406 0.3848 0.0847 1.0000 Uiso . .
H313 H 0.1096 -0.1784 0.3532 0.0847 1.0000 Uiso . .
H291 H 0.0798 0.0000 0.4237 0.1154 1.0000 Uiso . .
H292 H 0.0444 -0.0586 0.3436 0.1154 1.0000 Uiso . .
H271 H 0.0773 0.0000 -0.0677 0.1024 1.0000 Uiso . .
H272 H 0.0422 -0.0586 -0.0192 0.1024 1.0000 Uiso . .
H204 H 0.3672 0.1317 0.5532 0.0554 1.0000 Uiso . .
H251 H 0.4924 0.0000 0.6319 0.2866 1.0000 Uiso . .
H252 H 0.4581 -0.0586 0.5505 0.2866 1.0000 Uiso . .
H261 H 0.4597 -0.0754 0.7334 0.1932 1.0000 Uiso . .
H262 H 0.4017 -0.0773 0.7221 0.1932 1.0000 Uiso . .
H263 H 0.4252 -0.1300 0.6540 0.1932 1.0000 Uiso . .
H61 H 0.4524 -0.0749 -0.0481 0.3154 1.0000 Uiso . .
H62 H 0.4174 -0.1303 -0.0021 0.3154 1.0000 Uiso . .
H63 H 0.3945 -0.0741 -0.0896 0.3154 1.0000 Uiso . .
H71 H 0.4851 0.0000 0.0883 0.2832 1.0000 Uiso . .
H73 H 0.4499 0.0458 0.1367 0.2832 1.0000 Uiso . .
H14 H 0.3615 0.1300 0.0510 0.0664 1.0000 Uiso . .
H321 H 0.3828 0.0000 0.2509 0.1454 1.0000 Uiso . .
H322 H 0.3824 0.0586 0.3400 0.1454 1.0000 Uiso . .
H341 H 0.7687 0.1510 0.4085 0.0702 0.5000 Uiso . .
H342 H 0.7282 0.1501 0.3155 0.0702 0.5000 Uiso . .
H343 H 0.7280 0.0759 0.3880 0.0702 0.5000 Uiso . .
H351 H 0.7728 -0.1451 0.1068 0.0845 0.5000 Uiso . .
H352 H 0.7332 -0.1506 0.1646 0.0845 0.5000 Uiso . .
H353 H 0.7292 -0.0755 0.0914 0.0845 0.5000 Uiso . .
H381 H 0.6920 -0.0980 0.2965 0.1192 0.5000 Uiso . .
H382 H 0.7488 -0.0723 0.3218 0.1192 0.5000 Uiso . .
H383 H 0.7079 -0.0024 0.2984 0.1192 1.0000 Uiso . .
H331 H 0.8032 0.0947 0.2951 0.1020 0.5000 Uiso . .
H332 H 0.8031 0.0205 0.3676 0.1020 0.5000 Uiso . .
H371 H 0.7304 -0.1144 0.1576 0.1129 0.5000 Uiso . .
H372 H 0.6895 -0.0398 0.1342 0.1129 0.5000 Uiso . .
H361 H 0.8073 -0.0845 0.2534 0.1144 0.5000 Uiso . .
H362 H 0.8033 -0.0094 0.1802 0.1144 0.5000 Uiso . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780
1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 6_555 V1 O1 . 87.15(7) yes
O9 6_555 V1 O3 . 92.85(7) yes
O1 . V1 O3 . 179.39(16) yes
O9 6_555 V1 O7 . 89.68(8) yes
O1 . V1 O7 . 86.79(14) yes
O3 . V1 O7 . 92.61(16) yes
O9 6_555 V1 O8 . 90.04(8) yes
O1 . V1 O8 . 87.51(14) yes
O3 . V1 O8 . 93.10(16) yes
O7 . V1 O8 . 174.29(14) yes
O9 6_555 V1 O9 . 174.29(14) yes
O1 . V1 O9 . 87.15(7) yes
O3 . V1 O9 . 92.85(7) yes
O7 . V1 O9 . 89.68(8) yes
O8 . V1 O9 . 90.04(8) yes
O11 6_555 V2 O1 . 80.03(8) yes
O11 6_555 V2 O2 . 99.97(8) yes
O1 . V2 O2 . 178.46(19) yes
O11 6_555 V2 O10 . 88.20(9) yes
O1 . V2 O10 . 79.51(13) yes
O2 . V2 O10 . 102.03(19) yes
O11 6_555 V2 O12 . 88.21(9) yes
O1 . V2 O12 . 79.65(13) yes
O2 . V2 O12 . 98.81(19) yes
O10 . V2 O12 . 159.16(15) yes
O11 6_555 V2 O11 . 160.06(16) yes
O1 . V2 O11 . 80.03(8) yes
O2 . V2 O11 . 99.97(8) yes
O10 . V2 O11 . 88.20(9) yes
O12 . V2 O11 . 88.21(9) yes
O13 6_555 V3 O1 . 78.94(8) yes
O13 6_555 V3 O4 . 101.03(8) yes
O1 . V3 O4 . 175.21(18) yes
O13 6_555 V3 O7 . 87.35(8) yes
O1 . V3 O7 . 76.07(12) yes
O4 . V3 O7 . 99.14(18) yes
O13 6_555 V3 O10 . 88.29(8) yes
O1 . V3 O10 . 81.04(13) yes
O4 . V3 O10 . 103.75(18) yes
O7 . V3 O10 . 157.11(15) yes
O13 6_555 V3 O13 . 157.87(15) yes
O1 . V3 O13 . 78.94(8) yes
O4 . V3 O13 . 101.03(8) yes
O7 . V3 O13 . 87.35(8) yes
O10 . V3 O13 . 88.29(8) yes
O14 6_555 V4 O1 . 78.86(8) yes
O14 6_555 V4 O5 . 101.12(8) yes
O1 . V4 O5 . 175.85(18) yes
O14 6_555 V4 O8 . 87.58(8) yes
O1 . V4 O8 . 76.83(12) yes
O5 . V4 O8 . 99.02(18) yes
O14 6_555 V4 O12 . 88.22(8) yes
O1 . V4 O12 . 81.31(13) yes
O5 . V4 O12 . 102.85(19) yes
O8 . V4 O12 . 158.14(15) yes
O14 6_555 V4 O14 . 157.72(15) yes
O1 . V4 O14 . 78.86(8) yes
O5 . V4 O14 . 101.12(8) yes
O8 . V4 O14 . 87.58(8) yes
O12 . V4 O14 . 88.22(8) yes
O1 . V5 O6 . 175.89(14) yes
O1 . V5 O9 . 76.66(11) yes
O6 . V5 O9 . 99.25(13) yes
O1 . V5 O11 . 81.48(12) yes
O6 . V5 O11 . 102.60(14) yes
O9 . V5 O11 . 158.14(11) yes
O1 . V5 O13 . 79.21(12) yes
O6 . V5 O13 . 101.16(15) yes
O9 . V5 O13 . 87.62(10) yes
O11 . V5 O13 . 88.70(11) yes
O1 . V5 O14 . 78.72(11) yes
O6 . V5 O14 . 100.85(14) yes
O9 . V5 O14 . 87.25(10) yes
O11 . V5 O14 . 88.13(11) yes
O13 . V5 O14 . 157.93(11) yes
C33 6_555 N1 C37 6_555 175.1(7) yes
C33 6_555 N1 C35 6_555 109.5(8) yes
C37 6_555 N1 C35 6_555 73.1(9) yes
C33 6_555 N1 C33 . 71.4(10) yes
C37 6_555 N1 C33 . 105.9(7) yes
C35 6_555 N1 C33 . 73.6(6) yes
C33 6_555 N1 C35 . 73.6(6) yes
C37 6_555 N1 C35 . 111.3(8) yes
C35 6_555 N1 C35 . 63.7(11) yes
C33 . N1 C35 . 109.5(8) yes
C33 6_555 N1 C37 . 105.9(7) yes
C37 6_555 N1 C37 . 76.5(9) yes
C35 6_555 N1 C37 . 111.3(8) yes
C33 . N1 C37 . 175.1(7) yes
C35 . N1 C37 . 73.1(9) yes
V1 . O1 V4 . 91.87(13) yes
V1 . O1 V5 6_555 92.10(8) yes
V4 . O1 V5 6_555 90.15(9) yes
V1 . O1 V5 . 92.10(8) yes
V4 . O1 V5 . 90.15(9) yes
V5 6_555 O1 V5 . 175.77(16) yes
V1 . O1 V3 . 92.16(13) yes
V4 . O1 V3 . 175.97(16) yes
V5 6_555 O1 V3 . 89.71(9) yes
V5 . O1 V3 . 89.71(9) yes
V1 . O1 V2 . 179.88(18) yes
V4 . O1 V2 . 88.01(12) yes
V5 6_555 O1 V2 . 87.90(8) yes
V5 . O1 V2 . 87.90(8) yes
V3 . O1 V2 . 87.96(11) yes
V1 . O3 C32 . 178.1(7) yes
V3 . O7 V1 . 104.99(15) yes
V3 . O7 C1 . 134.8(3) yes
V1 . O7 C1 . 120.2(3) yes
V4 . O8 V1 . 103.79(14) yes
V4 . O8 C20 . 135.8(3) yes
V1 . O8 C20 . 120.4(3) yes
V5 . O9 V1 . 104.09(11) yes
V5 . O9 C9 . 136.2(2) yes
V1 . O9 C9 . 119.7(2) yes
V2 . O10 V3 . 111.49(17) yes
V2 . O10 C28 . 123.7(4) yes
V3 . O10 C28 . 124.8(4) yes
V2 . O12 V4 . 111.03(17) yes
V2 . O12 C27 . 123.3(4) yes
V4 . O12 C27 . 125.7(4) yes
V2 . O11 V5 . 110.59(13) yes
V2 . O11 C29 . 123.1(3) yes
V5 . O11 C29 . 126.1(3) yes
V3 . O13 V5 . 112.05(12) yes
V3 . O13 C31 . 118.6(3) yes
V5 . O13 C31 . 119.3(3) yes
V5 . O14 V4 . 112.19(12) yes
V5 . O14 C30 . 118.1(3) yes
V4 . O14 C30 . 117.9(3) yes
C2 6_555 C1 O7 . 118.8(2) yes
C2 6_555 C1 C2 . 122.1(5) yes
O7 . C1 C2 . 118.8(2) yes
C1 . C2 C3 . 117.3(4) yes
C1 . C2 C8 . 122.0(3) yes
C3 . C2 C8 . 120.6(4) yes
C2 . C3 C4 . 123.0(4) yes
C2 . C3 H14 . 119.609 no
C4 . C3 H14 . 117.392 no
C3 . C4 C3 6_555 117.3(5) yes
C3 . C4 C5 . 121.3(3) yes
C3 6_555 C4 C5 . 121.3(3) yes
C4 . C5 C6 6_555 111.3(5) yes
C4 . C5 C6 . 111.3(5) yes
C6 6_555 C5 C6 . 102.5(15) yes
C4 . C5 C7 . 107.8(7) yes
C6 6_555 C5 C7 . 112.0(9) yes
C6 . C5 C7 . 112.0(9) yes
C5 . C6 H61 . 111.691 no
C5 . C6 H62 . 110.661 no
H61 . C6 H62 . 105.762 no
C5 . C6 H63 . 112.808 no
H61 . C6 H63 . 108.730 no
H62 . C6 H63 . 106.834 no
C5 . C7 H73 6_555 111.439 no
C5 . C7 H71 . 109.795 no
H73 6_555 C7 H71 . 111.261 no
C5 . C7 H73 . 111.439 no
H73 6_555 C7 H73 . 101.439 no
H71 . C7 H73 . 111.261 no
C10 6_555 C8 C2 . 112.0(3) yes
C10 6_555 C8 H81 . 109.500 no
C2 . C8 H81 . 108.208 no
C10 6_555 C8 H82 . 109.285 no
C2 . C8 H82 . 109.099 no
H81 . C8 H82 . 108.695 no
O9 . C9 C10 . 119.0(3) yes
O9 . C9 C14 . 119.8(3) yes
C10 . C9 C14 . 121.0(3) yes
C8 6_555 C10 C9 . 121.2(3) yes
C8 6_555 C10 C11 . 120.7(3) yes
C9 . C10 C11 . 118.0(3) yes
C10 . C11 C12 . 123.0(4) yes
C10 . C11 H94 . 117.490 no
C12 . C11 H94 . 119.508 no
C11 . C12 C13 . 117.2(4) yes
C11 . C12 C15 . 121.2(4) yes
C13 . C12 C15 . 121.5(4) yes
C12 . C13 C14 . 122.5(4) yes
C12 . C13 H92 . 119.007 no
C14 . C13 H92 . 118.490 no
C13 . C14 C9 . 118.2(3) yes
C13 . C14 C19 . 120.4(3) yes
C9 . C14 C19 . 121.2(3) yes
C12 . C15 C16 . 112.5(5) yes
C12 . C15 C17 . 108.5(5) yes
C16 . C15 C17 . 107.3(10) yes
C12 . C15 C18 . 112.3(5) yes
C16 . C15 C18 . 105.5(9) yes
C17 . C15 C18 . 110.6(10) yes
C15 . C16 H161 . 111.751 no
C15 . C16 H162 . 112.883 no
H161 . C16 H162 . 111.420 no
C15 . C16 H163 . 108.354 no
H161 . C16 H163 . 105.522 no
H162 . C16 H163 . 106.444 no
C15 . C17 H171 . 112.477 no
C15 . C17 H172 . 109.177 no
H171 . C17 H172 . 105.700 no
C15 . C17 H173 . 112.762 no
H171 . C17 H173 . 110.374 no
H172 . C17 H173 . 105.884 no
C15 . C18 H181 . 112.527 no
C15 . C18 H182 . 114.140 no
H181 . C18 H182 . 110.917 no
C15 . C18 H183 . 108.489 no
H181 . C18 H183 . 104.396 no
H182 . C18 H183 . 105.629 no
C14 . C19 C21 6_555 113.2(3) yes
C14 . C19 H191 . 109.236 no
C21 6_555 C19 H191 . 108.448 no
C14 . C19 H192 . 108.729 no
C21 6_555 C19 H192 . 108.892 no
H191 . C19 H192 . 108.237 no
C21 6_555 C20 O8 . 119.1(2) yes
C21 6_555 C20 C21 . 121.3(5) yes
O8 . C20 C21 . 119.1(2) yes
C19 6_555 C21 C20 . 121.5(3) yes
C19 6_555 C21 C22 . 120.3(3) yes
C20 . C21 C22 . 118.2(4) yes
C21 . C22 C23 . 121.9(4) yes
C21 . C22 H204 . 118.945 no
C23 . C22 H204 . 119.160 no
C22 6_555 C23 C22 . 118.4(5) yes
C22 6_555 C23 C24 . 120.8(2) yes
C22 . C23 C24 . 120.8(2) yes
C23 . C24 C26 6_555 112.5(4) yes
C23 . C24 C25 . 109.0(7) yes
C26 6_555 C24 C25 . 109.3(8) yes
C23 . C24 C26 . 112.5(4) yes
C26 6_555 C24 C26 . 104.1(12) yes
C25 . C24 C26 . 109.3(8) yes
H252 6_555 C25 C24 . 108.601 no
H252 6_555 C25 H251 . 107.170 no
C24 . C25 H251 . 109.936 no
H252 6_555 C25 H252 . 115.290 no
C24 . C25 H252 . 108.601 no
H251 . C25 H252 . 107.170 no
C24 . C26 H261 . 112.331 no
C24 . C26 H262 . 112.136 no
H261 . C26 H262 . 110.792 no
C24 . C26 H263 . 108.765 no
H261 . C26 H263 . 106.003 no
H262 . C26 H263 . 106.427 no
H292 6_555 C27 O12 . 108.567 no
H292 6_555 C27 H291 . 107.384 no
O12 . C27 H291 . 110.591 no
H292 6_555 C27 H292 . 114.340 no
O12 . C27 H292 . 108.567 no
H291 . C27 H292 . 107.384 no
H272 6_555 C28 O10 . 109.344 no
H272 6_555 C28 H271 . 106.322 no
O10 . C28 H271 . 110.108 no
H272 6_555 C28 H272 . 115.268 no
O10 . C28 H272 . 109.344 no
H271 . C28 H272 . 106.322 no
O11 . C29 H281 . 111.077 no
O11 . C29 H282 . 111.037 no
H281 . C29 H282 . 109.735 no
O11 . C29 H283 . 109.432 no
H281 . C29 H283 . 107.635 no
H282 . C29 H283 . 107.808 no
O14 . C30 H311 . 110.518 no
O14 . C30 H312 . 110.117 no
H311 . C30 H312 . 109.265 no
O14 . C30 H313 . 109.896 no
H311 . C30 H313 . 108.759 no
H312 . C30 H313 . 108.238 no
O13 . C31 H301 . 110.094 no
O13 . C31 H302 . 110.826 no
H301 . C31 H302 . 109.166 no
O13 . C31 H303 . 109.851 no
H301 . C31 H303 . 107.898 no
H302 . C31 H303 . 108.944 no
H322 6_555 C32 O3 . 108.842 no
H322 6_555 C32 H321 . 106.661 no
O3 . C32 H321 . 109.752 no
H322 6_555 C32 H322 . 115.949 no
O3 . C32 H322 . 108.842 no
H321 . C32 H322 . 106.661 no
N1 . C33 C35 6_555 52.5(5) yes
N1 . C33 C34 . 110.3(8) yes
C35 6_555 C33 C34 . 128.6(10) yes
N1 . C33 H331 . 109.630 no
C35 6_555 C33 H331 . 57.170 no
C34 . C33 H331 . 110.327 no
N1 . C33 H332 . 109.792 no
C35 6_555 C33 H332 . 121.543 no
C34 . C33 H332 . 109.835 no
H331 . C33 H332 . 106.852 no
C33 . C34 H341 . 111.304 no
C33 . C34 H342 . 109.583 no
H341 . C34 H342 . 108.074 no
C33 . C34 H343 . 110.351 no
H341 . C34 H343 . 109.092 no
H342 . C34 H343 . 108.361 no
N1 . C35 C35 6_555 58.2(6) yes
N1 . C35 H362 6_555 98.315 no
C35 6_555 C35 H362 6_555 40.157 no
N1 . C35 C33 6_555 53.9(5) yes
C35 6_555 C35 C33 6_555 93.2(6) yes
H362 6_555 C35 C33 6_555 120.896 no
N1 . C35 C36 . 109.4(9) yes
C35 6_555 C35 C36 . 126.7(6) yes
H362 6_555 C35 C36 . 116.218 no
C33 6_555 C35 C36 . 121.9(11) yes
N1 . C35 H361 . 109.491 no
C35 6_555 C35 H361 . 121.048 no
H362 6_555 C35 H361 . 110.486 no
C33 6_555 C35 H361 . 55.992 no
C36 . C35 H361 . 112.008 no
N1 . C35 H362 . 109.008 no
C35 6_555 C35 H362 . 50.850 no
H362 6_555 C35 H362 . 10.693 no
C33 6_555 C35 H362 . 126.985 no
C36 . C35 H362 . 111.061 no
H361 . C35 H362 . 105.811 no
C35 . C36 H351 . 113.031 no
C35 . C36 H352 . 110.757 no
H351 . C36 H352 . 106.562 no
C35 . C36 H353 . 111.933 no
H351 . C36 H353 . 107.747 no
H352 . C36 H353 . 106.444 no
N1 . C37 C38 . 57.2(6) yes
N1 . C37 H371 . 123.398 no
C38 . C37 H371 . 121.080 no
N1 . C37 H372 . 121.773 no
C38 . C37 H372 . 121.675 no
H371 . C37 H372 . 105.759 no
C37 . C38 H383 6_555 109.414 no
C37 . C38 H381 . 110.973 no
H383 6_555 C38 H381 . 105.972 no
C37 . C38 H382 . 111.479 no
H383 6_555 C38 H382 . 109.345 no
H381 . C38 H382 . 109.498 no
C37 . C38 H383 . 110.670 no
H383 6_555 C38 H383 . 1.751 no
H381 . C38 H383 . 104.291 no
H382 . C38 H383 . 109.688 no
C38 6_555 H383 C38 . 132.202 no
H332 6_555 H332 C33 . 124.462 no
C35 . H362 C35 6_555 88.993 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O9 6_555 1.955(3) yes
V1 O1 . 2.035(3) yes
V1 O3 . 2.177(4) yes
V1 O7 . 1.947(3) yes
V1 O8 . 1.949(3) yes
V1 O9 . 1.955(3) yes
V2 O11 6_555 2.019(3) yes
V2 O1 . 2.387(3) yes
V2 O2 . 1.604(4) yes
V2 O10 . 2.022(4) yes
V2 O12 . 2.018(4) yes
V2 O11 . 2.019(3) yes
V3 O13 6_555 2.009(3) yes
V3 O1 . 2.365(4) yes
V3 O4 . 1.609(4) yes
V3 O7 . 2.058(3) yes
V3 O10 . 1.971(4) yes
V3 O13 . 2.009(3) yes
V4 O14 6_555 2.007(3) yes
V4 O1 . 2.353(4) yes
V4 O5 . 1.598(4) yes
V4 O8 . 2.067(3) yes
V4 O12 . 1.977(4) yes
V4 O14 . 2.007(3) yes
V5 O1 . 2.3562(10) yes
V5 O6 . 1.598(3) yes
V5 O9 . 2.064(2) yes
V5 O11 . 1.985(3) yes
V5 O13 . 2.006(3) yes
V5 O14 . 2.010(3) yes
N1 C33 6_555 1.536(11) yes
N1 C37 6_555 1.566(12) yes
N1 C35 6_555 1.508(12) yes
N1 C33 . 1.536(11) yes
N1 C35 . 1.508(12) yes
N1 C37 . 1.566(12) yes
O3 C32 . 1.293(9) yes
O7 C1 . 1.369(6) yes
O8 C20 . 1.377(6) yes
O9 C9 . 1.364(4) yes
O10 C28 . 1.395(7) yes
O12 C27 . 1.399(8) yes
O11 C29 . 1.383(6) yes
O13 C31 . 1.414(5) yes
O14 C30 . 1.414(5) yes
C1 C2 6_555 1.402(5) yes
C1 C2 . 1.402(5) yes
C2 C3 . 1.388(5) yes
C2 C8 . 1.520(6) yes
C3 C4 . 1.391(5) yes
C3 H14 . 0.989 no
C4 C5 . 1.534(8) yes
C5 C6 6_555 1.470(12) yes
C5 C6 . 1.470(12) yes
C5 C7 . 1.433(14) yes
C6 H61 . 1.012 no
C6 H62 . 1.036 no
C6 H63 . 0.997 no
C7 H73 6_555 0.926 no
C7 H71 . 0.994 no
C7 H73 . 0.926 no
C8 C10 6_555 1.520(5) yes
C8 H81 . 1.008 no
C8 H82 . 1.001 no
C9 C10 . 1.410(5) yes
C9 C14 . 1.395(5) yes
C10 C11 . 1.388(5) yes
C11 C12 . 1.391(6) yes
C11 H94 . 1.005 no
C12 C13 . 1.391(6) yes
C12 C15 . 1.550(6) yes
C13 C14 . 1.402(5) yes
C13 H92 . 1.013 no
C14 C19 . 1.524(5) yes
C15 C16 . 1.460(10) yes
C15 C17 . 1.464(11) yes
C15 C18 . 1.469(11) yes
C16 H161 . 0.995 no
C16 H162 . 0.982 no
C16 H163 . 1.056 no
C17 H171 . 0.996 no
C17 H172 . 1.053 no
C17 H173 . 0.993 no
C18 H181 . 1.000 no
C18 H182 . 0.983 no
C18 H183 . 1.066 no
C19 C21 6_555 1.517(5) yes
C19 H191 . 1.008 no
C19 H192 . 1.008 no
C20 C21 6_555 1.397(4) yes
C20 C21 . 1.397(4) yes
C21 C22 . 1.405(5) yes
C22 C23 . 1.386(5) yes
C22 H204 . 1.004 no
C23 C24 . 1.546(7) yes
C24 C26 6_555 1.466(9) yes
C24 C25 . 1.454(16) yes
C24 C26 . 1.466(9) yes
C25 H252 6_555 1.085 no
C25 H251 . 1.008 no
C25 H252 . 1.085 no
C26 H261 . 0.995 no
C26 H262 . 0.989 no
C26 H263 . 1.049 no
C27 H292 6_555 1.091 no
C27 H291 . 0.999 no
C27 H292 . 1.091 no
C28 H272 6_555 1.085 no
C28 H271 . 1.020 no
C28 H272 . 1.085 no
C29 H281 . 1.000 no
C29 H282 . 0.997 no
C29 H283 . 1.024 no
C30 H311 . 0.998 no
C30 H312 . 1.005 no
C30 H313 . 1.011 no
C31 H301 . 1.009 no
C31 H302 . 0.995 no
C31 H303 . 1.011 no
C32 H322 6_555 1.081 no
C32 H321 . 1.020 no
C32 H322 . 1.081 no
C33 C35 6_555 1.824(15) yes
C33 C34 . 1.527(15) yes
C33 H331 . 1.017 no
C33 H332 . 1.017 no
C34 H341 . 1.004 no
C34 H342 . 1.013 no
C34 H343 . 1.001 no
C35 C35 6_555 1.59(3) yes
C35 H362 6_555 1.234 no
C35 C36 . 1.520(18) yes
C35 H361 . 1.021 no
C35 H362 . 1.026 no
C36 H351 . 1.010 no
C36 H352 . 1.027 no
C36 H353 . 1.012 no
C37 C38 . 1.604(19) yes
C37 H371 . 1.016 no
C37 H372 . 1.032 no
C38 H383 6_555 1.024 no
C38 H381 . 1.022 no
C38 H382 . 0.978 no
C38 H383 . 0.955 no
H332 H332 6_555 0.642 no
