#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/59/4325946.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_4325946
loop_
_publ_author_name
'Lucy Clowes'
'Carl Redshaw'
'David L. Hughes'
_publ_section_title
;
 Vanadium-Based Pro-Catalysts Bearing Depleted 1,3-Calix[4]arenes for
 Ethylene or ε-Caprolactone Polymerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7838
_journal_page_last               7845
_journal_paper_doi               10.1021/ic2010198
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C100 H136 O14 V4,2(C2H3N)'
_chemical_formula_structural
'[{V2O2(m3-O)(m-OnPr)(OnPr)(calix,C44H54O2)}2].2(MeCN)'
_chemical_formula_sum            'C104 H142 N2 O14 V4'
_chemical_formula_weight         1847.96
_chemical_name_common            'Compound 4'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and CrysAlisPro RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.105(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3632(7)
_cell_length_b                   21.7638(10)
_cell_length_c                   19.9295(12)
_cell_measurement_reflns_used    5865
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      25.0000
_cell_measurement_theta_min      3.4211
_cell_volume                     5152.0(5)
_computing_cell_refinement
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_collection
;
 CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_reduction
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55
;
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 1997)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_measurement_method       'Thin slice φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1796
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58567
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.024
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
 empirical absorption correction using spherical harmonics,
  implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0699P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                3440
_reflns_number_total             6711
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2010198_si_001_4.cif
_cod_data_source_block           lucyc13a
_cod_original_formula_sum        'C104 H142 O14 N2 V4'
_cod_database_code               4325946
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
V1 V 0.49561(9) 0.56191(5) 0.47474(6) 0.0227(3) Uani 1 1 d .
V2 V 0.23922(9) 0.46572(5) 0.47426(6) 0.0248(3) Uani 1 1 d .
O7 O 0.4533(4) 0.61077(18) 0.5199(2) 0.0327(12) Uani 1 1 d .
O8 O 0.1323(4) 0.42591(19) 0.4737(2) 0.0389(13) Uani 1 1 d .
O9 O 0.4023(3) 0.49428(17) 0.4702(2) 0.0248(11) Uani 1 1 d .
O1 O 0.1985(3) 0.49117(17) 0.3851(2) 0.0254(11) Uani 1 1 d .
C11 C 0.1021(5) 0.4790(3) 0.3326(3) 0.0212(16) Uani 1 1 d .
C12 C 0.0112(5) 0.5199(3) 0.3193(3) 0.0234(17) Uani 1 1 d .
C13 C -0.0809(5) 0.5075(3) 0.2639(3) 0.0236(16) Uani 1 1 d .
H13 H -0.1411 0.5348 0.2547 0.028 Uiso 1 1 calc R
C14 C -0.0890(5) 0.4565(3) 0.2207(3) 0.0257(17) Uani 1 1 d .
C141 C -0.1904(6) 0.4437(3) 0.1579(4) 0.0383(19) Uani 1 1 d .
C142 C -0.1510(7) 0.4299(4) 0.0929(4) 0.085(3) Uani 1 1 d .
H14A H -0.1117 0.4649 0.0820 0.127 Uiso 1 1 calc R
H14B H -0.2152 0.4211 0.0541 0.127 Uiso 1 1 calc R
H14C H -0.1016 0.3950 0.1018 0.127 Uiso 1 1 calc R
C143 C -0.2732(6) 0.4982(3) 0.1406(4) 0.045(2) Uani 1 1 d .
H14D H -0.2354 0.5336 0.1291 0.067 Uiso 1 1 calc R
H14E H -0.3000 0.5073 0.1803 0.067 Uiso 1 1 calc R
H14F H -0.3357 0.4877 0.1015 0.067 Uiso 1 1 calc R
C144 C -0.2541(6) 0.3888(3) 0.1754(4) 0.064(3) Uani 1 1 d .
H14G H -0.3180 0.3800 0.1365 0.096 Uiso 1 1 calc R
H14H H -0.2793 0.3981 0.2157 0.096 Uiso 1 1 calc R
H14I H -0.2052 0.3537 0.1851 0.096 Uiso 1 1 calc R
C15 C 0.0016(6) 0.4160(3) 0.2366(3) 0.0241(17) Uani 1 1 d .
H15 H -0.0017 0.3811 0.2092 0.029 Uiso 1 1 calc R
C16 C 0.0974(5) 0.4258(3) 0.2924(3) 0.0212(16) Uani 1 1 d .
C17 C 0.1975(5) 0.3824(3) 0.3042(3) 0.0258(17) Uani 1 1 d .
H17A H 0.1711 0.3419 0.2871 0.031 Uiso 1 1 calc R
H17B H 0.2338 0.3791 0.3539 0.031 Uiso 1 1 calc R
C22 C 0.2830(5) 0.4048(3) 0.2672(3) 0.0199(16) Uani 1 1 d .
C23 C 0.2668(5) 0.3888(3) 0.1966(3) 0.0291(17) Uani 1 1 d .
H23 H 0.2053 0.3648 0.1739 0.035 Uiso 1 1 calc R
C21 C 0.3721(5) 0.4415(3) 0.2996(3) 0.0203(15) Uani 1 1 d .
H21 H 0.3826 0.4525 0.3460 0.024 Uiso 1 1 calc R
C24 C 0.3414(6) 0.4086(3) 0.1608(3) 0.0270(17) Uani 1 1 d .
C241 C 0.3207(7) 0.3908(4) 0.0828(4) 0.047(2) Uani 1 1 d .
C242 C 0.3441(14) 0.3261(4) 0.0779(5) 0.190(9) Uani 1 1 d .
H24A H 0.3000 0.3027 0.1015 0.285 Uiso 1 1 calc R
H24B H 0.4226 0.3186 0.0992 0.285 Uiso 1 1 calc R
H24C H 0.3252 0.3142 0.0296 0.285 Uiso 1 1 calc R
C243 C 0.3872(8) 0.4279(3) 0.0448(4) 0.063(3) Uani 1 1 d .
H24D H 0.3686 0.4706 0.0466 0.094 Uiso 1 1 calc R
H24E H 0.3694 0.4148 -0.0030 0.094 Uiso 1 1 calc R
H24F H 0.4661 0.4222 0.0665 0.094 Uiso 1 1 calc R
C244 C 0.1969(9) 0.4057(7) 0.0430(5) 0.147(6) Uani 1 1 d .
H24G H 0.1831 0.4487 0.0472 0.221 Uiso 1 1 calc R
H24H H 0.1472 0.3823 0.0625 0.221 Uiso 1 1 calc R
H24I H 0.1837 0.3954 -0.0055 0.221 Uiso 1 1 calc R
C25 C 0.4297(6) 0.4454(3) 0.1943(4) 0.0288(18) Uani 1 1 d .
H25 H 0.4793 0.4594 0.1702 0.035 Uiso 1 1 calc R
C26 C 0.4467(5) 0.4626(3) 0.2645(3) 0.0204(16) Uani 1 1 d .
C27 C 0.5412(5) 0.5062(3) 0.2975(3) 0.0212(16) Uani 1 1 d .
H27A H 0.6059 0.4972 0.2805 0.025 Uiso 1 1 calc R
H27B H 0.5633 0.5007 0.3477 0.025 Uiso 1 1 calc R
O3 O 0.4529(3) 0.58480(17) 0.3863(2) 0.0244(11) Uani 1 1 d .
C31 C 0.4575(5) 0.6084(3) 0.3242(3) 0.0224(16) Uani 1 1 d .
C32 C 0.5045(5) 0.5725(3) 0.2800(3) 0.0221(16) Uani 1 1 d .
C33 C 0.5090(5) 0.5988(3) 0.2192(3) 0.0267(17) Uani 1 1 d .
H33 H 0.5396 0.5758 0.1896 0.032 Uiso 1 1 calc R
C34 C 0.4712(5) 0.6579(3) 0.1976(4) 0.0289(17) Uani 1 1 d .
C341 C 0.4777(6) 0.6832(3) 0.1266(4) 0.038(2) Uani 1 1 d .
C342 C 0.6009(7) 0.6854(3) 0.1273(4) 0.058(3) Uani 1 1 d .
H34A H 0.6411 0.7126 0.1636 0.087 Uiso 1 1 calc R
H34B H 0.6067 0.7000 0.0830 0.087 Uiso 1 1 calc R
H34C H 0.6326 0.6449 0.1356 0.087 Uiso 1 1 calc R
C343 C 0.4161(8) 0.6400(4) 0.0684(4) 0.074(3) Uani 1 1 d .
H34D H 0.4474 0.5995 0.0775 0.110 Uiso 1 1 calc R
H34E H 0.4243 0.6545 0.0246 0.110 Uiso 1 1 calc R
H34F H 0.3376 0.6388 0.0665 0.110 Uiso 1 1 calc R
C344 C 0.4269(8) 0.7469(3) 0.1124(4) 0.069(3) Uani 1 1 d .
H34G H 0.4656 0.7743 0.1489 0.104 Uiso 1 1 calc R
H34H H 0.3487 0.7452 0.1109 0.104 Uiso 1 1 calc R
H34I H 0.4342 0.7614 0.0684 0.104 Uiso 1 1 calc R
C35 C 0.4261(5) 0.6909(3) 0.2440(4) 0.0302(18) Uani 1 1 d .
H35 H 0.4006 0.7307 0.2319 0.036 Uiso 1 1 calc R
C36 C 0.4175(5) 0.6675(3) 0.3067(3) 0.0195(16) Uani 1 1 d .
C37 C 0.3568(5) 0.7022(3) 0.3501(3) 0.0269(17) Uani 1 1 d .
H37A H 0.3693 0.7459 0.3462 0.032 Uiso 1 1 calc R
H37B H 0.3865 0.6906 0.3987 0.032 Uiso 1 1 calc R
C41 C 0.1854(5) 0.6445(3) 0.3573(3) 0.0205(16) Uani 1 1 d .
H41 H 0.2299 0.6234 0.3957 0.025 Uiso 1 1 calc R
C42 C 0.2316(5) 0.6890(3) 0.3263(3) 0.0214(16) Uani 1 1 d .
C43 C 0.1660(6) 0.7202(3) 0.2674(4) 0.0296(18) Uani 1 1 d .
H43 H 0.1992 0.7499 0.2461 0.035 Uiso 1 1 calc R
C44 C 0.0538(6) 0.7074(3) 0.2408(4) 0.0335(19) Uani 1 1 d .
C441 C -0.0183(7) 0.7429(3) 0.1765(4) 0.053(2) Uani 1 1 d .
C442 C 0.0543(8) 0.7684(4) 0.1315(5) 0.091(4) Uani 1 1 d .
H44A H 0.0901 0.7351 0.1145 0.136 Uiso 1 1 calc R
H44B H 0.1107 0.7954 0.1592 0.136 Uiso 1 1 calc R
H44C H 0.0075 0.7908 0.0927 0.136 Uiso 1 1 calc R
C443 C -0.1059(7) 0.7019(3) 0.1308(4) 0.064(3) Uani 1 1 d .
H44D H -0.0698 0.6682 0.1146 0.097 Uiso 1 1 calc R
H44E H -0.1497 0.7249 0.0915 0.097 Uiso 1 1 calc R
H44F H -0.1543 0.6863 0.1571 0.097 Uiso 1 1 calc R
C444 C -0.0722(9) 0.7952(4) 0.2012(5) 0.128(5) Uani 1 1 d .
H44G H -0.0154 0.8211 0.2303 0.191 Uiso 1 1 calc R
H44H H -0.1210 0.7803 0.2275 0.191 Uiso 1 1 calc R
H44I H -0.1153 0.8183 0.1618 0.191 Uiso 1 1 calc R
C45 C 0.0078(6) 0.6622(3) 0.2735(4) 0.0326(19) Uani 1 1 d .
H45 H -0.0682 0.6527 0.2561 0.039 Uiso 1 1 calc R
C46 C 0.0722(6) 0.6305(3) 0.3319(4) 0.0251(17) Uani 1 1 d .
C47 C 0.0190(6) 0.5791(3) 0.3621(4) 0.0312(18) Uani 1 1 d .
H47A H -0.0560 0.5914 0.3631 0.037 Uiso 1 1 calc R
H47B H 0.0631 0.5714 0.4098 0.037 Uiso 1 1 calc R
O5 O 0.6531(3) 0.59539(18) 0.4833(2) 0.0283(11) Uani 1 1 d .
C51 C 0.6751(6) 0.6576(3) 0.4633(4) 0.041(2) Uani 1 1 d .
H51A H 0.7191 0.6792 0.5044 0.049 Uiso 1 1 calc R
H51B H 0.6040 0.6791 0.4463 0.049 Uiso 1 1 calc R
C52 C 0.7356(7) 0.6600(4) 0.4091(5) 0.067(3) Uani 1 1 d .
H52A H 0.6961 0.6347 0.3699 0.081 Uiso 1 1 calc R
H52B H 0.8104 0.6429 0.4279 0.081 Uiso 1 1 calc R
C53 C 0.7460(10) 0.7241(4) 0.3836(6) 0.126(5) Uani 1 1 d .
H53A H 0.7848 0.7230 0.3480 0.189 Uiso 1 1 calc R
H53B H 0.7876 0.7490 0.4218 0.189 Uiso 1 1 calc R
H53C H 0.6723 0.7413 0.3646 0.189 Uiso 1 1 calc R
O6 O 0.2318(3) 0.52472(18) 0.5319(2) 0.0302(12) Uani 1 1 d .
C61 C 0.1578(6) 0.5353(3) 0.5748(4) 0.045(2) Uani 1 1 d .
H61A H 0.1717 0.5045 0.6114 0.054 Uiso 1 1 calc R
H61B H 0.0805 0.5308 0.5466 0.054 Uiso 1 1 calc R
C62 C 0.1731(7) 0.5973(3) 0.6071(4) 0.048(2) Uani 1 1 d .
H62A H 0.2496 0.6012 0.6368 0.058 Uiso 1 1 calc R
H62B H 0.1225 0.6020 0.6362 0.058 Uiso 1 1 calc R
C63 C 0.1505(7) 0.6475(3) 0.5530(5) 0.063(3) Uani 1 1 d .
H63A H 0.1627 0.6868 0.5758 0.094 Uiso 1 1 calc R
H63B H 0.0740 0.6448 0.5246 0.094 Uiso 1 1 calc R
H63C H 0.2005 0.6430 0.5240 0.094 Uiso 1 1 calc R
N91 N 0.1127(11) 0.6058(6) 0.0677(6) 0.176(6) Uani 1 1 d .
C92 C 0.1423(9) 0.5833(5) 0.1240(6) 0.083(3) Uani 1 1 d .
C93 C 0.1802(6) 0.5579(3) 0.1896(4) 0.045(2) Uani 1 1 d .
H93A H 0.2566 0.5444 0.1973 0.068 Uiso 1 1 calc R
H93B H 0.1338 0.5234 0.1933 0.068 Uiso 1 1 calc R
H93C H 0.1766 0.5880 0.2241 0.068 Uiso 1 1 calc R
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
O7 V1 O3 109.0(2) . .
O7 V1 O9 105.2(2) . .
O3 V1 O9 99.55(19) . .
O7 V1 O9 112.5(2) . 3_666
O3 V1 O9 137.16(17) . 3_666
O9 V1 O9 79.6(2) . 3_666
O7 V1 O5 99.9(2) . .
O3 V1 O5 89.79(18) . .
O9 V1 O5 148.46(17) . .
O9 V1 O5 73.30(17) 3_666 .
O7 V1 V1 114.87(16) . 3_666
O3 V1 V1 125.96(14) . 3_666
O9 V1 V1 40.06(13) . 3_666
O9 V1 V1 39.55(12) 3_666 3_666
O5 V1 V1 111.33(13) . 3_666
O8 V2 O6 102.2(2) . .
O8 V2 O1 99.1(2) . .
O6 V2 O1 111.94(19) . .
O8 V2 O5 95.8(2) . 3_666
O6 V2 O5 112.3(2) . 3_666
O1 V2 O5 128.68(18) . 3_666
O8 V2 O9 163.5(2) . .
O6 V2 O9 91.90(17) . .
O1 V2 O9 83.20(17) . .
O5 V2 O9 70.67(16) 3_666 .
V1 O9 V1 100.4(2) . 3_666
V1 O9 V2 144.1(2) . .
V1 O9 V2 106.13(18) 3_666 .
C11 O1 V2 129.8(4) . .
O1 C11 C12 120.2(5) . .
O1 C11 C16 119.0(5) . .
C12 C11 C16 120.8(6) . .
C13 C12 C11 118.1(6) . .
C13 C12 C47 121.4(6) . .
C11 C12 C47 120.3(6) . .
C12 C13 C14 123.7(6) . .
C12 C13 H13 118.1 . .
C14 C13 H13 118.1 . .
C13 C14 C15 116.7(6) . .
C13 C14 C141 123.6(6) . .
C15 C14 C141 119.7(6) . .
C144 C141 C14 108.2(6) . .
C144 C141 C142 110.2(7) . .
C14 C141 C142 110.3(6) . .
C144 C141 C143 107.6(6) . .
C14 C141 C143 112.6(6) . .
C142 C141 C143 107.9(6) . .
C141 C142 H14A 109.5 . .
C141 C142 H14B 109.5 . .
H14A C142 H14B 109.5 . .
C141 C142 H14C 109.5 . .
H14A C142 H14C 109.5 . .
H14B C142 H14C 109.5 . .
C141 C143 H14D 109.5 . .
C141 C143 H14E 109.5 . .
H14D C143 H14E 109.5 . .
C141 C143 H14F 109.5 . .
H14D C143 H14F 109.5 . .
H14E C143 H14F 109.5 . .
C141 C144 H14G 109.5 . .
C141 C144 H14H 109.5 . .
H14G C144 H14H 109.5 . .
C141 C144 H14I 109.5 . .
H14G C144 H14I 109.5 . .
H14H C144 H14I 109.5 . .
C14 C15 C16 122.4(6) . .
C14 C15 H15 118.8 . .
C16 C15 H15 118.8 . .
C15 C16 C11 118.2(6) . .
C15 C16 C17 120.1(6) . .
C11 C16 C17 121.4(6) . .
C16 C17 C22 111.7(5) . .
C16 C17 H17A 109.3 . .
C22 C17 H17A 109.3 . .
C16 C17 H17B 109.3 . .
C22 C17 H17B 109.3 . .
H17A C17 H17B 107.9 . .
C21 C22 C23 119.2(6) . .
C21 C22 C17 122.2(6) . .
C23 C22 C17 118.5(6) . .
C24 C23 C22 120.5(6) . .
C24 C23 H23 119.7 . .
C22 C23 H23 119.7 . .
C22 C21 C26 121.2(6) . .
C22 C21 H21 119.4 . .
C26 C21 H21 119.4 . .
C25 C24 C23 119.1(6) . .
C25 C24 C241 121.5(6) . .
C23 C24 C241 119.4(6) . .
C242 C241 C243 110.1(7) . .
C242 C241 C244 110.9(9) . .
C243 C241 C244 103.3(8) . .
C242 C241 C24 109.3(7) . .
C243 C241 C24 114.1(6) . .
C244 C241 C24 109.0(6) . .
C241 C242 H24A 109.5 . .
C241 C242 H24B 109.5 . .
H24A C242 H24B 109.5 . .
C241 C242 H24C 109.5 . .
H24A C242 H24C 109.5 . .
H24B C242 H24C 109.5 . .
C241 C243 H24D 109.5 . .
C241 C243 H24E 109.5 . .
H24D C243 H24E 109.5 . .
C241 C243 H24F 109.5 . .
H24D C243 H24F 109.5 . .
H24E C243 H24F 109.5 . .
C241 C244 H24G 109.5 . .
C241 C244 H24H 109.5 . .
H24G C244 H24H 109.5 . .
C241 C244 H24I 109.5 . .
H24G C244 H24I 109.5 . .
H24H C244 H24I 109.5 . .
C24 C25 C26 121.3(6) . .
C24 C25 H25 119.3 . .
C26 C25 H25 119.3 . .
C21 C26 C25 118.6(6) . .
C21 C26 C27 122.2(6) . .
C25 C26 C27 119.0(5) . .
C26 C27 C32 110.6(5) . .
C26 C27 H27A 109.5 . .
C32 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
C32 C27 H27B 109.5 . .
H27A C27 H27B 108.1 . .
C31 O3 V1 160.3(4) . .
O3 C31 C36 118.6(5) . .
O3 C31 C32 119.1(6) . .
C36 C31 C32 122.3(6) . .
C33 C32 C31 116.6(6) . .
C33 C32 C27 121.4(6) . .
C31 C32 C27 121.9(5) . .
C32 C33 C34 124.9(6) . .
C32 C33 H33 117.6 . .
C34 C33 H33 117.6 . .
C33 C34 C35 115.4(6) . .
C33 C34 C341 121.0(6) . .
C35 C34 C341 123.6(6) . .
C344 C341 C342 109.6(6) . .
C344 C341 C343 109.1(7) . .
C342 C341 C343 108.3(6) . .
C344 C341 C34 112.0(6) . .
C342 C341 C34 108.1(6) . .
C343 C341 C34 109.6(6) . .
C341 C342 H34A 109.5 . .
C341 C342 H34B 109.5 . .
H34A C342 H34B 109.5 . .
C341 C342 H34C 109.5 . .
H34A C342 H34C 109.5 . .
H34B C342 H34C 109.5 . .
C341 C343 H34D 109.5 . .
C341 C343 H34E 109.5 . .
H34D C343 H34E 109.5 . .
C341 C343 H34F 109.5 . .
H34D C343 H34F 109.5 . .
H34E C343 H34F 109.5 . .
C341 C344 H34G 109.5 . .
C341 C344 H34H 109.5 . .
H34G C344 H34H 109.5 . .
C341 C344 H34I 109.5 . .
H34G C344 H34I 109.5 . .
H34H C344 H34I 109.5 . .
C36 C35 C34 123.5(6) . .
C36 C35 H35 118.2 . .
C34 C35 H35 118.2 . .
C35 C36 C31 117.2(5) . .
C35 C36 C37 120.9(5) . .
C31 C36 C37 121.6(5) . .
C36 C37 C42 110.9(5) . .
C36 C37 H37A 109.5 . .
C42 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
C42 C37 H37B 109.5 . .
H37A C37 H37B 108.1 . .
C42 C41 C46 120.1(6) . .
C42 C41 H41 119.9 . .
C46 C41 H41 119.9 . .
C41 C42 C43 120.5(6) . .
C41 C42 C37 121.1(6) . .
C43 C42 C37 118.2(6) . .
C44 C43 C42 121.0(6) . .
C44 C43 H43 119.5 . .
C42 C43 H43 119.5 . .
C43 C44 C45 117.7(6) . .
C43 C44 C441 120.5(6) . .
C45 C44 C441 121.7(6) . .
C444 C441 C443 110.2(8) . .
C444 C441 C442 107.9(8) . .
C443 C441 C442 107.5(7) . .
C444 C441 C44 108.6(7) . .
C443 C441 C44 111.0(6) . .
C442 C441 C44 111.5(7) . .
C441 C442 H44A 109.5 . .
C441 C442 H44B 109.5 . .
H44A C442 H44B 109.5 . .
C441 C442 H44C 109.5 . .
H44A C442 H44C 109.5 . .
H44B C442 H44C 109.5 . .
C441 C443 H44D 109.5 . .
C441 C443 H44E 109.5 . .
H44D C443 H44E 109.5 . .
C441 C443 H44F 109.5 . .
H44D C443 H44F 109.5 . .
H44E C443 H44F 109.5 . .
C441 C444 H44G 109.5 . .
C441 C444 H44H 109.5 . .
H44G C444 H44H 109.5 . .
C441 C444 H44I 109.5 . .
H44G C444 H44I 109.5 . .
H44H C444 H44I 109.5 . .
C44 C45 C46 121.9(6) . .
C44 C45 H45 119.1 . .
C46 C45 H45 119.1 . .
C41 C46 C45 118.8(6) . .
C41 C46 C47 121.9(6) . .
C45 C46 C47 119.2(6) . .
C46 C47 C12 111.7(5) . .
C46 C47 H47A 109.3 . .
C12 C47 H47A 109.3 . .
C46 C47 H47B 109.3 . .
C12 C47 H47B 109.3 . .
H47A C47 H47B 108.0 . .
C51 O5 V2 127.5(4) . 3_666
C51 O5 V1 123.7(4) . .
V2 O5 V1 108.69(18) 3_666 .
O5 C51 C52 113.8(6) . .
O5 C51 H51A 108.8 . .
C52 C51 H51A 108.8 . .
O5 C51 H51B 108.8 . .
C52 C51 H51B 108.8 . .
H51A C51 H51B 107.7 . .
C51 C52 C53 112.9(8) . .
C51 C52 H52A 109.0 . .
C53 C52 H52A 109.0 . .
C51 C52 H52B 109.0 . .
C53 C52 H52B 109.0 . .
H52A C52 H52B 107.8 . .
C52 C53 H53A 109.5 . .
C52 C53 H53B 109.5 . .
H53A C53 H53B 109.5 . .
C52 C53 H53C 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
C61 O6 V2 132.1(4) . .
O6 C61 C62 112.2(5) . .
O6 C61 H61A 109.2 . .
C62 C61 H61A 109.2 . .
O6 C61 H61B 109.2 . .
C62 C61 H61B 109.2 . .
H61A C61 H61B 107.9 . .
C61 C62 C63 111.9(6) . .
C61 C62 H62A 109.2 . .
C63 C62 H62A 109.2 . .
C61 C62 H62B 109.2 . .
C63 C62 H62B 109.2 . .
H62A C62 H62B 107.9 . .
C62 C63 H63A 109.5 . .
C62 C63 H63B 109.5 . .
H63A C63 H63B 109.5 . .
C62 C63 H63C 109.5 . .
H63A C63 H63C 109.5 . .
H63B C63 H63C 109.5 . .
N91 C92 C93 178.1(14) . .
C92 C93 H93A 109.5 . .
C92 C93 H93B 109.5 . .
H93A C93 H93B 109.5 . .
C92 C93 H93C 109.5 . .
H93A C93 H93C 109.5 . .
H93B C93 H93C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O7 1.573(4) .
V1 O3 1.766(4) .
V1 O9 1.857(4) .
V1 O9 1.877(4) 3_666
V1 O5 2.042(4) .
V1 V1 2.868(2) 3_666
V2 O8 1.578(4) .
V2 O6 1.742(4) .
V2 O1 1.795(4) .
V2 O5 1.906(4) 3_666
V2 O9 2.133(4) .
O9 V1 1.877(4) 3_666
O1 C11 1.375(7) .
C11 C12 1.399(8) .
C11 C16 1.400(8) .
C12 C13 1.375(8) .
C12 C47 1.535(8) .
C13 C14 1.390(8) .
C13 H13 0.9300 .
C14 C15 1.391(8) .
C14 C141 1.531(9) .
C141 C144 1.524(9) .
C141 C142 1.535(9) .
C141 C143 1.543(9) .
C142 H14A 0.9600 .
C142 H14B 0.9600 .
C142 H14C 0.9600 .
C143 H14D 0.9600 .
C143 H14E 0.9600 .
C143 H14F 0.9600 .
C144 H14G 0.9600 .
C144 H14H 0.9600 .
C144 H14I 0.9600 .
C15 C16 1.398(8) .
C15 H15 0.9300 .
C16 C17 1.522(8) .
C17 C22 1.526(8) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C22 C21 1.368(8) .
C22 C23 1.410(8) .
C23 C24 1.382(8) .
C23 H23 0.9300 .
C21 C26 1.382(8) .
C21 H21 0.9300 .
C24 C25 1.370(8) .
C24 C241 1.554(9) .
C241 C242 1.445(11) .
C241 C243 1.499(9) .
C241 C244 1.551(12) .
C242 H24A 0.9600 .
C242 H24B 0.9600 .
C242 H24C 0.9600 .
C243 H24D 0.9600 .
C243 H24E 0.9600 .
C243 H24F 0.9600 .
C244 H24G 0.9600 .
C244 H24H 0.9600 .
C244 H24I 0.9600 .
C25 C26 1.405(8) .
C25 H25 0.9300 .
C26 C27 1.508(8) .
C27 C32 1.524(8) .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
O3 C31 1.355(7) .
C31 C36 1.387(8) .
C31 C32 1.417(8) .
C32 C33 1.356(8) .
C33 C34 1.394(8) .
C33 H33 0.9300 .
C34 C35 1.404(8) .
C34 C341 1.540(9) .
C341 C344 1.514(9) .
C341 C342 1.520(9) .
C341 C343 1.524(10) .
C342 H34A 0.9600 .
C342 H34B 0.9600 .
C342 H34C 0.9600 .
C343 H34D 0.9600 .
C343 H34E 0.9600 .
C343 H34F 0.9600 .
C344 H34G 0.9600 .
C344 H34H 0.9600 .
C344 H34I 0.9600 .
C35 C36 1.380(8) .
C35 H35 0.9300 .
C36 C37 1.497(8) .
C37 C42 1.515(8) .
C37 H37A 0.9700 .
C37 H37B 0.9700 .
C41 C42 1.357(8) .
C41 C46 1.383(8) .
C41 H41 0.9300 .
C42 C43 1.403(8) .
C43 C44 1.369(9) .
C43 H43 0.9300 .
C44 C45 1.387(9) .
C44 C441 1.549(10) .
C441 C444 1.471(11) .
C441 C443 1.500(10) .
C441 C442 1.539(11) .
C442 H44A 0.9600 .
C442 H44B 0.9600 .
C442 H44C 0.9600 .
C443 H44D 0.9600 .
C443 H44E 0.9600 .
C443 H44F 0.9600 .
C444 H44G 0.9600 .
C444 H44H 0.9600 .
C444 H44I 0.9600 .
C45 C46 1.396(9) .
C45 H45 0.9300 .
C46 C47 1.505(8) .
C47 H47A 0.9700 .
C47 H47B 0.9700 .
O5 C51 1.458(7) .
O5 V2 1.906(4) 3_666
C51 C52 1.475(10) .
C51 H51A 0.9700 .
C51 H51B 0.9700 .
C52 C53 1.502(10) .
C52 H52A 0.9700 .
C52 H52B 0.9700 .
C53 H53A 0.9600 .
C53 H53B 0.9600 .
C53 H53C 0.9600 .
O6 C61 1.433(7) .
C61 C62 1.485(9) .
C61 H61A 0.9700 .
C61 H61B 0.9700 .
C62 C63 1.506(9) .
C62 H62A 0.9700 .
C62 H62B 0.9700 .
C63 H63A 0.9600 .
C63 H63B 0.9600 .
C63 H63C 0.9600 .
N91 C92 1.185(12) .
C92 C93 1.378(12) .
C93 H93A 0.9600 .
C93 H93B 0.9600 .
C93 H93C 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
O7 V1 O9 V1 -110.7(2) . 3_666
O3 V1 O9 V1 136.48(18) . 3_666
O9 V1 O9 V1 0.0 3_666 3_666
O5 V1 O9 V1 31.0(4) . 3_666
O7 V1 O9 V2 26.7(4) . .
O3 V1 O9 V2 -86.2(4) . .
O9 V1 O9 V2 137.3(5) 3_666 .
O5 V1 O9 V2 168.3(3) . .
V1 V1 O9 V2 137.3(5) 3_666 .
O8 V2 O9 V1 179.1(6) . .
O6 V2 O9 V1 -31.9(4) . .
O1 V2 O9 V1 80.0(4) . .
O5 V2 O9 V1 -144.9(4) 3_666 .
O8 V2 O9 V1 -44.8(8) . 3_666
O6 V2 O9 V1 104.2(2) . 3_666
O1 V2 O9 V1 -143.9(2) . 3_666
O5 V2 O9 V1 -8.79(18) 3_666 3_666
O8 V2 O1 C11 0.0(5) . .
O6 V2 O1 C11 -107.2(5) . .
O5 V2 O1 C11 104.9(5) 3_666 .
O9 V2 O1 C11 163.5(5) . .
V2 O1 C11 C12 94.5(6) . .
V2 O1 C11 C16 -86.4(6) . .
O1 C11 C12 C13 176.5(5) . .
C16 C11 C12 C13 -2.6(8) . .
O1 C11 C12 C47 1.2(8) . .
C16 C11 C12 C47 -177.9(5) . .
C11 C12 C13 C14 0.5(9) . .
C47 C12 C13 C14 175.8(5) . .
C12 C13 C14 C15 1.2(9) . .
C12 C13 C14 C141 -178.4(6) . .
C13 C14 C141 C144 -109.5(7) . .
C15 C14 C141 C144 70.9(7) . .
C13 C14 C141 C142 129.9(7) . .
C15 C14 C141 C142 -49.7(9) . .
C13 C14 C141 C143 9.3(9) . .
C15 C14 C141 C143 -170.3(5) . .
C13 C14 C15 C16 -0.9(9) . .
C141 C14 C15 C16 178.7(5) . .
C14 C15 C16 C11 -1.1(9) . .
C14 C15 C16 C17 -175.6(5) . .
O1 C11 C16 C15 -176.2(5) . .
C12 C11 C16 C15 2.8(8) . .
O1 C11 C16 C17 -1.8(8) . .
C12 C11 C16 C17 177.2(5) . .
C15 C16 C17 C22 91.9(7) . .
C11 C16 C17 C22 -82.4(7) . .
C16 C17 C22 C21 92.0(7) . .
C16 C17 C22 C23 -85.6(7) . .
C21 C22 C23 C24 1.7(9) . .
C17 C22 C23 C24 179.4(6) . .
C23 C22 C21 C26 -0.7(9) . .
C17 C22 C21 C26 -178.2(5) . .
C22 C23 C24 C25 -1.9(9) . .
C22 C23 C24 C241 -179.4(6) . .
C25 C24 C241 C242 110.6(9) . .
C23 C24 C241 C242 -71.9(10) . .
C25 C24 C241 C243 -13.1(10) . .
C23 C24 C241 C243 164.3(7) . .
C25 C24 C241 C244 -128.0(8) . .
C23 C24 C241 C244 49.4(10) . .
C23 C24 C25 C26 1.1(10) . .
C241 C24 C25 C26 178.6(6) . .
C22 C21 C26 C25 -0.1(9) . .
C22 C21 C26 C27 176.1(5) . .
C24 C25 C26 C21 -0.1(9) . .
C24 C25 C26 C27 -176.4(6) . .
C21 C26 C27 C32 -93.2(7) . .
C25 C26 C27 C32 83.0(7) . .
O7 V1 O3 C31 101.5(12) . .
O9 V1 O3 C31 -148.6(11) . .
O9 V1 O3 C31 -63.6(12) 3_666 .
O5 V1 O3 C31 1.1(12) . .
V1 V1 O3 C31 -115.4(11) 3_666 .
V1 O3 C31 C36 -99.5(12) . .
V1 O3 C31 C32 79.6(13) . .
O3 C31 C32 C33 -178.8(5) . .
C36 C31 C32 C33 0.2(9) . .
O3 C31 C32 C27 5.1(9) . .
C36 C31 C32 C27 -175.9(6) . .
C26 C27 C32 C33 -83.7(7) . .
C26 C27 C32 C31 92.3(7) . .
C31 C32 C33 C34 0.1(10) . .
C27 C32 C33 C34 176.2(6) . .
C32 C33 C34 C35 0.2(10) . .
C32 C33 C34 C341 -178.7(6) . .
C33 C34 C341 C344 177.2(7) . .
C35 C34 C341 C344 -1.6(10) . .
C33 C34 C341 C342 -61.9(8) . .
C35 C34 C341 C342 119.3(7) . .
C33 C34 C341 C343 55.9(9) . .
C35 C34 C341 C343 -122.9(7) . .
C33 C34 C35 C36 -0.7(10) . .
C341 C34 C35 C36 178.1(6) . .
C34 C35 C36 C31 1.0(10) . .
C34 C35 C36 C37 -173.0(6) . .
O3 C31 C36 C35 178.3(6) . .
C32 C31 C36 C35 -0.7(9) . .
O3 C31 C36 C37 -7.8(9) . .
C32 C31 C36 C37 173.2(6) . .
C35 C36 C37 C42 85.2(7) . .
C31 C36 C37 C42 -88.5(7) . .
C46 C41 C42 C43 -1.5(9) . .
C46 C41 C42 C37 -175.8(5) . .
C36 C37 C42 C41 94.3(7) . .
C36 C37 C42 C43 -80.1(7) . .
C41 C42 C43 C44 1.3(9) . .
C37 C42 C43 C44 175.8(6) . .
C42 C43 C44 C45 -0.7(10) . .
C42 C43 C44 C441 178.9(6) . .
C43 C44 C441 C444 -93.8(9) . .
C45 C44 C441 C444 85.8(9) . .
C43 C44 C441 C443 144.8(7) . .
C45 C44 C441 C443 -35.6(10) . .
C43 C44 C441 C442 24.9(10) . .
C45 C44 C441 C442 -155.5(7) . .
C43 C44 C45 C46 0.3(10) . .
C441 C44 C45 C46 -179.3(6) . .
C42 C41 C46 C45 1.1(9) . .
C42 C41 C46 C47 176.5(5) . .
C44 C45 C46 C41 -0.5(9) . .
C44 C45 C46 C47 -176.0(6) . .
C41 C46 C47 C12 -96.9(7) . .
C45 C46 C47 C12 78.5(7) . .
C13 C12 C47 C46 -89.2(7) . .
C11 C12 C47 C46 86.0(7) . .
O7 V1 O5 C51 -56.7(5) . .
O3 V1 O5 C51 52.6(5) . .
O9 V1 O5 C51 160.7(4) . .
O9 V1 O5 C51 -167.4(5) 3_666 .
V1 V1 O5 C51 -178.5(4) 3_666 .
O7 V1 O5 V2 119.9(2) . 3_666
O3 V1 O5 V2 -130.9(2) . 3_666
O9 V1 O5 V2 -22.8(4) . 3_666
O9 V1 O5 V2 9.17(18) 3_666 3_666
V1 V1 O5 V2 -1.9(2) 3_666 3_666
V2 O5 C51 C52 63.0(8) 3_666 .
V1 O5 C51 C52 -121.1(6) . .
O5 C51 C52 C53 173.6(7) . .
O8 V2 O6 C61 5.2(6) . .
O1 V2 O6 C61 110.4(6) . .
O5 V2 O6 C61 -96.3(6) 3_666 .
O9 V2 O6 C61 -166.2(6) . .
V2 O6 C61 C62 -171.0(5) . .
O6 C61 C62 C63 60.0(8) . .
