#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309182.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_4309182
loop_
_publ_author_name
'Stanislav Groysman'
'Israel Goldberg'
'Zeev Goldschmidt'
'Moshe Kol'
_publ_section_title
;
Vanadium(III) and Vanadium(V) Amine Tris(Phenolate) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5073
_journal_page_last               5080
_journal_paper_doi               10.1021/ic050084i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C49 H66 N O4 V'
_chemical_formula_weight         783.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.933(12)
_cell_angle_beta                 100.196(8)
_cell_angle_gamma                96.432(11)
_cell_formula_units_Z            2
_cell_length_a                   10.3790(17)
_cell_length_b                   11.0330(16)
_cell_length_c                   20.604(3)
_cell_measurement_temperature    298(2)
_cell_volume                     2304.1(6)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B. V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg Phi and Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1237
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7733
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing (1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.295
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.2153
_refine_ls_R_factor_gt           0.1327
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3073
_refine_ls_wR_factor_ref         0.3630
_reflns_number_gt                3973
_reflns_number_total             7733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050084isi20050518_103020_2.cif
_cod_data_source_block           mk103b
_cod_database_code               4309182
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.61137(11) 0.02062(10) 0.28321(6) 0.0401(4) Uani 1 1 d . . .
O2 O 0.5717(11) 0.1859(10) 0.2979(6) 0.037(3) Uani 0.50 1 d P A 1
O3 O 0.6014(18) -0.0939(14) 0.3507(11) 0.040(4) Uani 0.50 1 d P A 1
O4 O 0.6765(11) -0.0910(11) 0.2255(6) 0.044(3) Uani 0.50 1 d P A 1
O2' O 0.5890(13) 0.1797(11) 0.2603(7) 0.049(3) Uani 0.50 1 d P A 2
O3' O 0.5762(17) -0.0472(15) 0.3567(11) 0.046(4) Uani 0.50 1 d P A 2
O4' O 0.6753(10) -0.0239(10) 0.2115(5) 0.032(2) Uani 0.50 1 d P A 2
N5 N 0.4144(5) -0.0353(5) 0.2362(3) 0.0394(14) Uani 1 1 d . A .
O6 O 0.8098(5) 0.0767(4) 0.3337(3) 0.0496(13) Uani 1 1 d . A .
C7 C 0.8873(8) 0.1844(7) 0.3208(5) 0.062(2) Uani 1 1 d . . .
H7A H 0.8611 0.2556 0.3415 0.074 Uiso 1 1 calc R A .
H7B H 0.8772 0.1944 0.2736 0.074 Uiso 1 1 calc R . .
C8 C 1.0268(8) 0.1681(8) 0.3493(5) 0.066(2) Uani 1 1 d . A .
H8A H 1.0503 0.1984 0.3951 0.079 Uiso 1 1 calc R . .
H8B H 1.0880 0.2089 0.3242 0.079 Uiso 1 1 calc R . .
C9 C 1.0236(8) 0.0307(8) 0.3428(5) 0.065(2) Uani 1 1 d . . .
H9A H 1.0300 0.0034 0.2984 0.078 Uiso 1 1 calc R A .
H9B H 1.0943 0.0028 0.3739 0.078 Uiso 1 1 calc R . .
C10 C 0.8950(8) -0.0118(7) 0.3584(5) 0.061(2) Uani 1 1 d . A .
H10A H 0.8622 -0.0919 0.3372 0.073 Uiso 1 1 calc R . .
H10B H 0.9007 -0.0168 0.4057 0.073 Uiso 1 1 calc R . .
C11 C 0.4851(8) -0.1398(9) 0.3716(4) 0.065(3) Uani 1 1 d . . .
C12 C 0.4968(7) -0.1911(6) 0.4328(3) 0.0410(17) Uani 1 1 d . A .
C13 C 0.3844(7) -0.2591(6) 0.4463(3) 0.0429(17) Uani 1 1 d . . .
H13 H 0.3913 -0.2954 0.4866 0.052 Uiso 1 1 calc R A .
C14 C 0.2621(7) -0.2774(7) 0.4041(4) 0.0478(19) Uani 1 1 d . A .
C15 C 0.2462(16) -0.1989(15) 0.3501(10) 0.036(5) Uani 0.50 1 d P A 1
H15 H 0.1721 -0.1603 0.3353 0.043 Uiso 0.50 1 calc PR A 1
C16 C 0.3762(13) -0.1893(12) 0.3200(6) 0.027(3) Uani 0.50 1 d P A 1
C17 C 0.3748(13) -0.1623(12) 0.2489(7) 0.031(3) Uani 0.50 1 d P A 1
C18 C 0.6165(16) -0.1512(18) 0.1634(8) 0.039(4) Uani 0.50 1 d P A 1
C15' C 0.265(2) -0.2518(14) 0.3395(11) 0.039(5) Uani 0.50 1 d P A 2
H15' H 0.2226 -0.3014 0.3027 0.047 Uiso 0.50 1 calc PR A 2
C16' C 0.3525(15) -0.1209(15) 0.3376(7) 0.040(4) Uani 0.50 1 d P A 2
C17' C 0.3219(14) 0.0466(13) 0.2677(7) 0.035(3) Uiso 0.50 1 d P A 2
C18' C 0.6146(17) -0.0865(16) 0.1524(10) 0.043(5) Uani 0.50 1 d P A 2
C19 C 0.6928(7) -0.1636(7) 0.1164(4) 0.0484(19) Uani 1 1 d . . .
C20 C 0.6239(8) -0.2187(6) 0.0551(4) 0.0455(18) Uani 1 1 d . A .
H20 H 0.6735 -0.2489 0.0262 0.055 Uiso 1 1 calc R . .
C21 C 0.4898(8) -0.2309(8) 0.0350(4) 0.060(2) Uani 1 1 d . . .
C22 C 0.4144(15) -0.1502(15) 0.0719(7) 0.042(4) Uani 0.50 1 d P A 1
C23 C 0.4795(15) -0.0864(13) 0.1307(7) 0.041(3) Uani 0.50 1 d P A 1
C24 C 0.4006(17) -0.0044(17) 0.1670(8) 0.032(4) Uani 0.50 1 d P A 1
H24A H 0.4335 0.0808 0.1644 0.038 Uiso 0.50 1 calc PR A 1
H24B H 0.3083 -0.0166 0.1462 0.038 Uiso 0.50 1 calc PR A 1
C25 C 0.4836(15) 0.2381(13) 0.2369(9) 0.031(4) Uani 0.50 1 d P A 1
C22' C 0.4197(16) -0.2301(15) 0.0873(8) 0.048(4) Uani 0.50 1 d P A 2
C23' C 0.4829(14) -0.1871(12) 0.1514(8) 0.044(4) Uani 0.50 1 d P A 2
C24' C 0.4064(14) -0.1720(13) 0.2087(9) 0.046(4) Uani 0.50 1 d P A 2
H24C H 0.4412 -0.2208 0.2445 0.055 Uiso 0.50 1 calc PR A 2
H24D H 0.3145 -0.2035 0.1934 0.055 Uiso 0.50 1 calc PR A 2
C25' C 0.4675(17) 0.2460(16) 0.2727(8) 0.035(4) Uani 0.50 1 d P A 2
C26 C 0.4825(7) 0.3680(6) 0.2558(4) 0.050(2) Uani 1 1 d . . .
C27 C 0.3692(7) 0.4290(6) 0.2274(3) 0.0378(16) Uiso 1 1 d . A .
H27 H 0.3725 0.5136 0.2295 0.045 Uiso 1 1 calc R . .
C28 C 0.2543(8) 0.3528(7) 0.1967(5) 0.059(2) Uani 1 1 d . . .
C29 C 0.2577(15) 0.2219(12) 0.1743(8) 0.044(4) Uani 0.50 1 d P A 1
C30 C 0.3440(13) 0.1773(12) 0.2527(7) 0.037(3) Uani 0.50 1 d P A 1
C31 C 0.3255(14) -0.0297(17) 0.2841(8) 0.053(4) Uani 0.50 1 d P A 1
C29' C 0.2371(13) 0.2303(13) 0.2197(8) 0.038(3) Uani 0.50 1 d P A 2
C30' C 0.3717(14) 0.1671(13) 0.1972(7) 0.041(3) Uani 0.50 1 d P A 2
C31' C 0.366(2) 0.0386(19) 0.1766(13) 0.054(6) Uani 0.50 1 d P A 2
C32 C 0.6263(7) -0.1767(7) 0.4822(3) 0.0425(17) Uani 1 1 d . . .
C33 C 0.7274(7) -0.2442(7) 0.4538(4) 0.054(2) Uani 1 1 d . A .
H33A H 0.6962 -0.3298 0.4475 0.081 Uiso 1 1 calc R . .
H33B H 0.8102 -0.2326 0.4840 0.081 Uiso 1 1 calc R . .
H33C H 0.7390 -0.2123 0.4122 0.081 Uiso 1 1 calc R . .
C34 C 0.6804(8) -0.0417(7) 0.4977(4) 0.059(2) Uani 1 1 d . A .
H34A H 0.6888 -0.0031 0.4573 0.089 Uiso 1 1 calc R . .
H34B H 0.7652 -0.0356 0.5259 0.089 Uiso 1 1 calc R . .
H34C H 0.6209 -0.0018 0.5195 0.089 Uiso 1 1 calc R . .
C35 C 0.6103(8) -0.2336(9) 0.5471(4) 0.064(2) Uani 1 1 d . A .
H35A H 0.5415 -0.1995 0.5644 0.096 Uiso 1 1 calc R . .
H35B H 0.6915 -0.2168 0.5782 0.096 Uiso 1 1 calc R . .
H35C H 0.5878 -0.3203 0.5395 0.096 Uiso 1 1 calc R . .
C36 C 0.1434(7) -0.3525(7) 0.4253(4) 0.054(2) Uani 1 1 d . . .
C37 C 0.0202(8) -0.3539(9) 0.3740(4) 0.072(3) Uani 1 1 d . A .
H37A H 0.0355 -0.3853 0.3324 0.108 Uiso 1 1 calc R . .
H37B H -0.0028 -0.2723 0.3697 0.108 Uiso 1 1 calc R . .
H37C H -0.0506 -0.4049 0.3874 0.108 Uiso 1 1 calc R . .
C38 C 0.1764(10) -0.4779(9) 0.4411(7) 0.103(4) Uani 1 1 d . A .
H38A H 0.1030 -0.5236 0.4552 0.155 Uiso 1 1 calc R . .
H38B H 0.2523 -0.4721 0.4757 0.155 Uiso 1 1 calc R . .
H38C H 0.1950 -0.5185 0.4024 0.155 Uiso 1 1 calc R . .
C39 C 0.1171(9) -0.2896(11) 0.4876(5) 0.087(3) Uani 1 1 d . A .
H39A H 0.0491 -0.3388 0.5043 0.130 Uiso 1 1 calc R . .
H39B H 0.0892 -0.2112 0.4776 0.130 Uiso 1 1 calc R . .
H39C H 0.1963 -0.2791 0.5204 0.130 Uiso 1 1 calc R . .
C40 C 0.4161(8) -0.2809(7) -0.0311(4) 0.053(2) Uani 1 1 d . A .
C41 C 0.3473(12) -0.1844(9) -0.0690(5) 0.093(3) Uani 1 1 d . . .
H41A H 0.2896 -0.1510 -0.0433 0.139 Uiso 1 1 calc R A .
H41B H 0.2967 -0.2204 -0.1100 0.139 Uiso 1 1 calc R . .
H41C H 0.4117 -0.1206 -0.0776 0.139 Uiso 1 1 calc R . .
C42 C 0.5116(11) -0.3251(12) -0.0738(5) 0.102(4) Uani 1 1 d . . .
H42A H 0.5835 -0.2621 -0.0736 0.153 Uiso 1 1 calc R A .
H42B H 0.4655 -0.3437 -0.1183 0.153 Uiso 1 1 calc R . .
H42C H 0.5454 -0.3971 -0.0562 0.153 Uiso 1 1 calc R . .
C43 C 0.3165(11) -0.3918(10) -0.0245(5) 0.101(4) Uani 1 1 d . . .
H43A H 0.3622 -0.4541 -0.0024 0.151 Uiso 1 1 calc R A .
H43B H 0.2719 -0.4231 -0.0677 0.151 Uiso 1 1 calc R . .
H43C H 0.2533 -0.3675 0.0006 0.151 Uiso 1 1 calc R . .
C44 C 0.8428(8) -0.1537(7) 0.1354(4) 0.054(2) Uani 1 1 d . A .
C45 C 0.9030(8) -0.0194(7) 0.1470(4) 0.058(2) Uani 1 1 d . . .
H45A H 0.8815 0.0225 0.1071 0.087 Uiso 1 1 calc R A .
H45B H 0.9970 -0.0152 0.1595 0.087 Uiso 1 1 calc R . .
H45C H 0.8680 0.0185 0.1817 0.087 Uiso 1 1 calc R . .
C46 C 0.9055(9) -0.2101(10) 0.0814(5) 0.079(3) Uani 1 1 d . . .
H46A H 0.8668 -0.2932 0.0711 0.118 Uiso 1 1 calc R A .
H46B H 0.9987 -0.2080 0.0967 0.118 Uiso 1 1 calc R . .
H46C H 0.8903 -0.1643 0.0425 0.118 Uiso 1 1 calc R . .
C47 C 0.8794(9) -0.2212(7) 0.1983(5) 0.072(3) Uani 1 1 d . . .
H47A H 0.8333 -0.1936 0.2314 0.107 Uiso 1 1 calc R A .
H47B H 0.9727 -0.2052 0.2142 0.107 Uiso 1 1 calc R . .
H47C H 0.8553 -0.3074 0.1889 0.107 Uiso 1 1 calc R . .
C48 C 0.6096(7) 0.4486(5) 0.2885(3) 0.0371(16) Uani 1 1 d . A .
C49 C 0.7193(7) 0.4271(6) 0.2497(4) 0.0452(18) Uani 1 1 d . . .
H49A H 0.8022 0.4663 0.2735 0.068 Uiso 1 1 calc R A .
H49B H 0.7005 0.4606 0.2072 0.068 Uiso 1 1 calc R . .
H49C H 0.7236 0.3410 0.2443 0.068 Uiso 1 1 calc R . .
C50 C 0.5925(8) 0.5847(7) 0.2863(4) 0.056(2) Uani 1 1 d . . .
H50A H 0.5176 0.5998 0.3056 0.083 Uiso 1 1 calc R A .
H50B H 0.5789 0.6076 0.2413 0.083 Uiso 1 1 calc R . .
H50C H 0.6702 0.6321 0.3108 0.083 Uiso 1 1 calc R . .
C51 C 0.6507(8) 0.4198(7) 0.3604(4) 0.055(2) Uani 1 1 d . . .
H51A H 0.7354 0.4642 0.3780 0.083 Uiso 1 1 calc R A .
H51B H 0.6559 0.3338 0.3632 0.083 Uiso 1 1 calc R . .
H51C H 0.5868 0.4435 0.3853 0.083 Uiso 1 1 calc R . .
C52 C 0.1351(7) 0.4132(6) 0.1635(4) 0.0481(19) Uani 1 1 d . A .
C53 C 0.1029(14) 0.3610(14) 0.0861(6) 0.134(5) Uani 1 1 d . . .
H53A H 0.0965 0.2734 0.0842 0.201 Uiso 1 1 calc R A .
H53B H 0.1723 0.3932 0.0640 0.201 Uiso 1 1 calc R . .
H53C H 0.0209 0.3858 0.0647 0.201 Uiso 1 1 calc R . .
C54 C 0.0148(11) 0.3710(12) 0.1873(7) 0.128(5) Uani 1 1 d . . .
H54A H 0.0136 0.4145 0.2283 0.192 Uiso 1 1 calc R A .
H54B H 0.0118 0.2851 0.1940 0.192 Uiso 1 1 calc R . .
H54C H -0.0603 0.3854 0.1552 0.192 Uiso 1 1 calc R . .
C55 C 0.1607(11) 0.5460(9) 0.1601(7) 0.120(5) Uani 1 1 d . . .
H55A H 0.0814 0.5771 0.1398 0.180 Uiso 1 1 calc R A .
H55B H 0.2282 0.5649 0.1344 0.180 Uiso 1 1 calc R . .
H55C H 0.1892 0.5829 0.2039 0.180 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'
O O 0.0106 0.0060 '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'
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
O3' V1 O4' 137.2(6) . . ?
O3' V1 O2' 126.1(6) . . ?
O4' V1 O2' 96.7(5) . . ?
O3' V1 O3 18.9(6) . . ?
O4' V1 O3 118.5(6) . . ?
O2' V1 O3 144.7(6) . . ?
O3' V1 O4 112.8(6) . . ?
O4' V1 O4 24.5(3) . . ?
O2' V1 O4 121.1(5) . . ?
O3 V1 O4 94.1(6) . . ?
O3' V1 O2 101.2(6) . . ?
O4' V1 O2 121.5(5) . . ?
O2' V1 O2 25.0(4) . . ?
O3 V1 O2 119.7(6) . . ?
O4 V1 O2 145.9(5) . . ?
O3' V1 N5 89.4(7) . . ?
O4' V1 N5 92.4(4) . . ?
O2' V1 N5 89.0(4) . . ?
O3 V1 N5 92.5(6) . . ?
O4 V1 N5 91.2(4) . . ?
O2 V1 N5 91.2(4) . . ?
O3' V1 O6 89.0(7) . . ?
O4' V1 O6 89.1(4) . . ?
O2' V1 O6 91.6(4) . . ?
O3 V1 O6 86.1(6) . . ?
O4 V1 O6 89.9(4) . . ?
O2 V1 O6 88.7(3) . . ?
N5 V1 O6 178.3(2) . . ?
C25 O2 V1 114.8(9) . . ?
C11 O3 V1 124.8(11) . . ?
C18 O4 V1 131.3(10) . . ?
C25' O2' V1 123.5(10) . . ?
C11 O3' V1 135.9(16) . . ?
C18' O4' V1 131.7(10) . . ?
C17 N5 C24 116.9(11) . . ?
C17 N5 C31 74.7(10) . . ?
C24 N5 C31 131.8(9) . . ?
C17 N5 C31' 129.6(12) . . ?
C24 N5 C31' 25.6(7) . . ?
C31 N5 C31' 109.4(10) . . ?
C17 N5 C24' 36.1(7) . . ?
C24 N5 C24' 85.5(10) . . ?
C31 N5 C24' 109.0(10) . . ?
C31' N5 C24' 106.4(11) . . ?
C17 N5 C17' 107.5(9) . . ?
C24 N5 C17' 105.4(9) . . ?
C31 N5 C17' 34.7(7) . . ?
C31' N5 C17' 79.9(9) . . ?
C24' N5 C17' 137.0(8) . . ?
C17 N5 V1 110.6(6) . . ?
C24 N5 V1 108.3(8) . . ?
C31 N5 V1 110.0(7) . . ?
C31' N5 V1 114.1(10) . . ?
C24' N5 V1 107.7(6) . . ?
C17' N5 V1 107.8(6) . . ?
C7 O6 C10 109.3(6) . . ?
C7 O6 V1 123.9(5) . . ?
C10 O6 V1 120.9(4) . . ?
O6 C7 C8 105.8(7) . . ?
O6 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
O6 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
C7 C8 C9 101.7(7) . . ?
C7 C8 H8A 111.4 . . ?
C9 C8 H8A 111.4 . . ?
C7 C8 H8B 111.4 . . ?
C9 C8 H8B 111.4 . . ?
H8A C8 H8B 109.3 . . ?
C10 C9 C8 102.3(7) . . ?
C10 C9 H9A 111.3 . . ?
C8 C9 H9A 111.3 . . ?
C10 C9 H9B 111.3 . . ?
C8 C9 H9B 111.3 . . ?
H9A C9 H9B 109.2 . . ?
O6 C10 C9 105.8(6) . . ?
O6 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
O6 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
C12 C11 O3' 123.1(11) . . ?
C12 C11 O3 117.6(10) . . ?
O3' C11 O3 25.7(6) . . ?
C12 C11 C16 118.3(8) . . ?
O3' C11 C16 118.6(12) . . ?
O3 C11 C16 116.1(12) . . ?
C12 C11 C16' 118.0(8) . . ?
O3' C11 C16' 109.0(11) . . ?
O3 C11 C16' 123.8(11) . . ?
C16 C11 C16' 36.0(6) . . ?
C11 C12 C13 116.5(6) . . ?
C11 C12 C32 122.2(6) . . ?
C13 C12 C32 121.3(6) . . ?
C12 C13 C14 125.2(7) . . ?
C12 C13 H13 117.4 . . ?
C14 C13 H13 117.4 . . ?
C15' C14 C13 115.1(10) . . ?
C15' C14 C15 27.7(7) . . ?
C13 C14 C15 115.6(9) . . ?
C15' C14 C36 122.5(10) . . ?
C13 C14 C36 120.5(7) . . ?
C15 C14 C36 122.0(9) . . ?
C14 C15 C16 108.1(12) . . ?
C14 C15 H15 126.0 . . ?
C16 C15 H15 125.9 . . ?
C11 C16 C17 121.4(10) . . ?
C11 C16 C15 108.0(12) . . ?
C17 C16 C15 121.5(12) . . ?
C11 C16 C31 98.1(9) . . ?
C17 C16 C31 58.3(8) . . ?
C15 C16 C31 87.0(10) . . ?
N5 C17 C16 116.0(11) . . ?
N5 C17 C31 52.9(7) . . ?
C16 C17 C31 75.6(10) . . ?
C19 C18 O4 118.5(13) . . ?
C19 C18 C23 109.6(12) . . ?
O4 C18 C23 110.1(13) . . ?
C14 C15' C16' 109.1(14) . . ?
C14 C15' H15' 125.4 . . ?
C16' C15' H15' 125.4 . . ?
C11 C16' C15' 104.3(12) . . ?
N5 C17' C31' 48.8(7) . . ?
O4' C18' C19 119.3(14) . . ?
O4' C18' C23' 119.2(14) . . ?
C19 C18' C23' 98.9(12) . . ?
C18 C19 C20 114.8(9) . . ?
C18 C19 C18' 30.2(7) . . ?
C20 C19 C18' 114.9(10) . . ?
C18 C19 C44 120.8(9) . . ?
C20 C19 C44 122.1(7) . . ?
C18' C19 C44 120.9(9) . . ?
C21 C20 C19 125.1(7) . . ?
C21 C20 H20 117.5 . . ?
C19 C20 H20 117.5 . . ?
C20 C21 C22' 113.8(9) . . ?
C20 C21 C40 125.9(7) . . ?
C22' C21 C40 117.5(9) . . ?
C20 C21 C22 116.5(9) . . ?
C22' C21 C22 37.7(7) . . ?
C40 C21 C22 114.2(9) . . ?
C23 C22 C21 119.1(12) . . ?
C22 C23 C24 118.0(14) . . ?
C22 C23 C18 110.7(12) . . ?
C24 C23 C18 127.7(12) . . ?
N5 C24 C23 109.3(11) . . ?
N5 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
N5 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
C26 C25 O2 105.1(11) . . ?
C26 C25 C30 101.9(11) . . ?
O2 C25 C30 95.6(11) . . ?
C21 C22' C23' 121.0(13) . . ?
C22' C23' C24' 122.5(13) . . ?
C22' C23' C18' 113.2(14) . . ?
C24' C23' C18' 116.1(12) . . ?
C23' C24' N5 113.7(11) . . ?
C23' C24' H24C 108.8 . . ?
N5 C24' H24C 108.8 . . ?
C23' C24' H24D 108.8 . . ?
N5 C24' H24D 108.8 . . ?
H24C C24' H24D 107.7 . . ?
C26 C25' O2' 110.9(12) . . ?
C26 C25' C30' 103.1(11) . . ?
O2' C25' C30' 88.4(11) . . ?
C25' C26 C27 121.5(9) . . ?
C25' C26 C25 31.7(6) . . ?
C27 C26 C25 118.8(9) . . ?
C25' C26 C48 117.6(9) . . ?
C27 C26 C48 117.8(6) . . ?
C25 C26 C48 121.3(8) . . ?
C28 C27 C26 116.7(6) . . ?
C28 C27 H27 121.7 . . ?
C26 C27 H27 121.7 . . ?
C27 C28 C29' 116.5(8) . . ?
C27 C28 C29 122.2(8) . . ?
C29' C28 C29 39.4(7) . . ?
C27 C28 C52 118.4(6) . . ?
C29' C28 C52 120.7(8) . . ?
C29 C28 C52 115.9(8) . . ?
C28 C29 C30 95.8(10) . . ?
C25 C30 C29 91.0(10) . . ?
N5 C31 C17 52.4(7) . . ?
N5 C31 C16 90.7(9) . . ?
C17 C31 C16 46.1(7) . . ?
C28 C29' C30' 102.0(10) . . ?
C31' C30' C29' 122.9(13) . . ?
C31' C30' C25' 127.3(15) . . ?
C29' C30' C25' 85.5(10) . . ?
C30' C31' N5 110.3(17) . . ?
C30' C31' C17' 72.3(11) . . ?
N5 C31' C17' 51.2(9) . . ?
C35 C32 C12 111.8(6) . . ?
C35 C32 C34 107.9(6) . . ?
C12 C32 C34 111.3(6) . . ?
C35 C32 C33 106.7(6) . . ?
C12 C32 C33 109.2(6) . . ?
C34 C32 C33 109.8(6) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C38 C36 C37 112.8(8) . . ?
C38 C36 C39 108.3(8) . . ?
C37 C36 C39 106.6(7) . . ?
C38 C36 C14 109.8(7) . . ?
C37 C36 C14 111.3(7) . . ?
C39 C36 C14 107.8(6) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C21 C40 C41 111.5(7) . . ?
C21 C40 C43 111.2(7) . . ?
C41 C40 C43 110.3(8) . . ?
C21 C40 C42 110.6(7) . . ?
C41 C40 C42 106.2(8) . . ?
C43 C40 C42 106.8(8) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C47 C44 C19 109.2(6) . . ?
C47 C44 C46 108.1(7) . . ?
C19 C44 C46 112.1(7) . . ?
C47 C44 C45 109.6(7) . . ?
C19 C44 C45 110.8(6) . . ?
C46 C44 C45 107.0(7) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C51 C48 C50 108.0(6) . . ?
C51 C48 C49 110.2(6) . . ?
C50 C48 C49 107.2(6) . . ?
C51 C48 C26 111.3(6) . . ?
C50 C48 C26 111.5(6) . . ?
C49 C48 C26 108.6(6) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C54 C52 C55 114.8(9) . . ?
C54 C52 C28 112.7(7) . . ?
C55 C52 C28 114.4(7) . . ?
C54 C52 C53 102.9(10) . . ?
C55 C52 C53 104.4(9) . . ?
C28 C52 C53 106.1(7) . . ?
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 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
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 O3' 1.79(2) . ?
V1 O4' 1.799(10) . ?
V1 O2' 1.862(12) . ?
V1 O3 1.919(17) . ?
V1 O4 1.939(11) . ?
V1 O2 1.940(11) . ?
V1 N5 2.116(6) . ?
V1 O6 2.149(5) . ?
O2 C25 1.58(2) . ?
O3 C11 1.400(19) . ?
O4 C18 1.43(2) . ?
O2' C25' 1.58(2) . ?
O3' C11 1.39(2) . ?
O4' C18' 1.39(2) . ?
N5 C17 1.460(14) . ?
N5 C24 1.465(18) . ?
N5 C31 1.469(14) . ?
N5 C31' 1.54(3) . ?
N5 C24' 1.581(16) . ?
N5 C17' 1.592(15) . ?
O6 C7 1.419(9) . ?
O6 C10 1.436(9) . ?
C7 C8 1.496(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.514(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.458(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.390(10) . ?
C11 C16 1.451(15) . ?
C11 C16' 1.470(17) . ?
C12 C13 1.391(10) . ?
C12 C32 1.525(10) . ?
C13 C14 1.396(10) . ?
C13 H13 0.9300 . ?
C14 C15' 1.37(2) . ?
C14 C15 1.430(19) . ?
C14 C36 1.543(10) . ?
C15 C16 1.58(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.50(2) . ?
C16 C31 2.02(2) . ?
C17 C31 1.78(2) . ?
C18 C19 1.369(18) . ?
C18 C23 1.71(2) . ?
C15' C16' 1.63(2) . ?
C15' H15' 0.9300 . ?
C17' C31' 2.01(3) . ?
C18' C19 1.502(19) . ?
C18' C23' 1.66(2) . ?
C19 C20 1.417(10) . ?
C19 C44 1.528(11) . ?
C20 C21 1.369(11) . ?
C20 H20 0.9300 . ?
C21 C22' 1.402(17) . ?
C21 C40 1.493(11) . ?
C21 C22 1.517(17) . ?
C22 C23 1.40(2) . ?
C23 C24 1.54(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.474(17) . ?
C25 C30 1.62(2) . ?
C22' C23' 1.41(2) . ?
C23' C24' 1.55(2) . ?
C24' H24C 0.9700 . ?
C24' H24D 0.9700 . ?
C25' C26 1.399(19) . ?
C25' C30' 1.82(2) . ?
C26 C27 1.463(10) . ?
C26 C48 1.539(10) . ?
C27 C28 1.414(10) . ?
C27 H27 0.9300 . ?
C28 C29' 1.450(16) . ?
C28 C29 1.508(16) . ?
C28 C52 1.535(10) . ?
C29 C30 1.82(2) . ?
C29' C30' 1.755(19) . ?
C30' C31' 1.46(2) . ?
C32 C35 1.523(10) . ?
C32 C34 1.534(10) . ?
C32 C33 1.536(9) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C38 1.494(11) . ?
C36 C37 1.505(11) . ?
C36 C39 1.522(12) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.510(12) . ?
C40 C43 1.536(12) . ?
C40 C42 1.545(12) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 C47 1.527(11) . ?
C44 C46 1.533(11) . ?
C44 C45 1.535(10) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 C51 1.521(10) . ?
C48 C50 1.534(9) . ?
C48 C49 1.535(9) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C54 1.454(12) . ?
C52 C55 1.466(11) . ?
C52 C53 1.642(14) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
