#------------------------------------------------------------------------------
#$Date: 2026-03-13 00:57:40 +0100 (Fri 13 de Mar de 2026) $
#$Revision: 305066 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/06/7720687.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_7720687
loop_
_publ_author_name
'Shibata, Kaname'
'Michiue, Kenji'
'Motuzis, Ignas'
'Elsegood, Mark Robert James'
'Redshaw, Carl'
_publ_section_title
;
 Vanadyl complexes supported by O,O-and N,O-chelate ligation: Structures
 and polymerization catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00387G
_journal_year                    2026
_chemical_formula_moiety         'C38 H43 I4 N2 O3 V, 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H44.5 I4 N2.5 O3 V'
_chemical_formula_weight         1154.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.109(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3991(6)
_cell_length_b                   12.4635(3)
_cell_length_c                   27.4973(8)
_cell_measurement_reflns_used    43357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.82
_cell_measurement_theta_min      1.83
_cell_volume                     8362.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix Arc-100 detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            135095
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.000
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    25.463
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) 
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4440
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.000010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/3 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         15531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0288P)²+58.7809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12215
_reflns_number_total             15531
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00387g2.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C39 H44.50 I4 N2.50 O3 V'
_cod_database_code               7720687
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.883
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.90634(4) 0.52741(8) 0.60982(4) 0.0181(2) Uani 1 1 d . . . . .
O3 O 0.90539(17) 0.5678(3) 0.66478(16) 0.0243(10) Uani 1 1 d . . . . .
O1 O 0.84268(16) 0.4724(3) 0.56475(16) 0.0221(10) Uani 1 1 d . . . . .
C1 C 0.8306(2) 0.3693(5) 0.5523(2) 0.0212(14) Uani 1 1 d . . . . .
C2 C 0.7755(3) 0.3357(5) 0.5358(3) 0.0254(15) Uani 1 1 d . . . . .
I1 I 0.71340(2) 0.44540(4) 0.53843(2) 0.04287(14) Uani 1 1 d . . . . .
C3 C 0.7617(3) 0.2308(5) 0.5215(2) 0.0236(15) Uani 1 1 d . . . . .
H3 H 0.724231 0.210311 0.509825 0.028 Uiso 1 1 calc R U . . .
C4 C 0.8025(3) 0.1557(5) 0.5242(2) 0.0227(14) Uani 1 1 d . . . . .
I2 I 0.78114(2) -0.00382(3) 0.50409(2) 0.02990(11) Uani 1 1 d . . . . .
C5 C 0.8575(3) 0.1844(5) 0.5433(2) 0.0214(14) Uani 1 1 d . . . . .
H5 H 0.885573 0.131992 0.547093 0.026 Uiso 1 1 calc R U . . .
C6 C 0.8708(2) 0.2910(5) 0.5567(2) 0.0191(13) Uani 1 1 d . . . . .
C7 C 0.9300(2) 0.3230(5) 0.5809(2) 0.0212(14) Uani 1 1 d . . . . .
H7A H 0.952904 0.257974 0.590745 0.025 Uiso 1 1 calc R U . . .
H7B H 0.944170 0.364058 0.556345 0.025 Uiso 1 1 calc R U . . .
N1 N 0.93287(19) 0.3894(4) 0.62600(19) 0.0190(11) Uani 1 1 d . . . . .
C8 C 0.9506(2) 0.3379(5) 0.6751(2) 0.0200(14) Uani 1 1 d . . . . .
C9 C 0.9129(3) 0.2978(5) 0.6985(2) 0.0243(15) Uani 1 1 d . . . . .
C10 C 0.9332(3) 0.2517(6) 0.7464(3) 0.0340(17) Uani 1 1 d . . . . .
H10 H 0.908328 0.223582 0.763408 0.041 Uiso 1 1 calc R U . . .
C11 C 0.9892(3) 0.2464(6) 0.7695(3) 0.0406(19) Uani 1 1 d . . . . .
H11 H 1.002173 0.215007 0.802175 0.049 Uiso 1 1 calc R U . . .
C12 C 1.0264(3) 0.2866(6) 0.7453(3) 0.0368(18) Uani 1 1 d . . . . .
H12 H 1.064632 0.281651 0.761337 0.044 Uiso 1 1 calc R U . . .
C13 C 1.0080(3) 0.3338(5) 0.6979(3) 0.0273(15) Uani 1 1 d . . . . .
C14 C 0.8509(3) 0.3045(6) 0.6760(3) 0.0289(16) Uani 1 1 d . . . . .
H14 H 0.844084 0.336703 0.641509 0.035 Uiso 1 1 calc R U . . .
C15 C 0.8251(3) 0.3783(6) 0.7066(3) 0.0415(19) Uani 1 1 d . . . . .
H15A H 0.828664 0.346621 0.739992 0.062 Uiso 1 1 calc R U . . .
H15B H 0.786183 0.388117 0.688952 0.062 Uiso 1 1 calc R U . . .
H15C H 0.843638 0.448054 0.710712 0.062 Uiso 1 1 calc R U . . .
C16 C 0.8245(3) 0.1934(7) 0.6694(3) 0.047(2) Uani 1 1 d . . . . .
H16A H 0.841518 0.148713 0.648673 0.071 Uiso 1 1 calc R U . . .
H16B H 0.785182 0.200291 0.652709 0.071 Uiso 1 1 calc R U . . .
H16C H 0.829769 0.159918 0.702695 0.071 Uiso 1 1 calc R U . . .
C17 C 1.0484(3) 0.3822(6) 0.6727(3) 0.0290(16) Uani 1 1 d . . . . .
H17 H 1.027964 0.398086 0.636809 0.035 Uiso 1 1 calc R U . . .
C18 C 1.0957(3) 0.3083(7) 0.6719(3) 0.043(2) Uani 1 1 d . . . . .
H18A H 1.116168 0.289970 0.706690 0.065 Uiso 1 1 calc R U . . .
H18B H 1.120149 0.344662 0.655173 0.065 Uiso 1 1 calc R U . . .
H18C H 1.081431 0.242574 0.653342 0.065 Uiso 1 1 calc R U . . .
C19 C 1.0698(3) 0.4896(6) 0.6984(3) 0.043(2) Uani 1 1 d . . . . .
H19A H 1.038858 0.537525 0.697049 0.065 Uiso 1 1 calc R U . . .
H19B H 1.094172 0.523026 0.680657 0.065 Uiso 1 1 calc R U . . .
H19C H 1.090135 0.476710 0.733785 0.065 Uiso 1 1 calc R U . . .
O2 O 0.96687(16) 0.5695(3) 0.58711(18) 0.0242(10) Uani 1 1 d . . . . .
C20 C 0.9875(2) 0.6614(5) 0.5760(2) 0.0211(14) Uani 1 1 d . . . . .
C21 C 1.0361(2) 0.6610(5) 0.5607(2) 0.0216(14) Uani 1 1 d . . . . .
I3 I 1.07363(2) 0.51439(3) 0.55354(2) 0.02854(11) Uani 1 1 d . . . . .
C22 C 1.0611(3) 0.7547(5) 0.5518(2) 0.0258(15) Uani 1 1 d . . . . .
H22 H 1.093589 0.752248 0.541196 0.031 Uiso 1 1 calc R U . . .
C23 C 1.0381(3) 0.8517(5) 0.5587(3) 0.0247(15) Uani 1 1 d . . . . .
I4 I 1.07996(2) 0.99467(4) 0.55278(2) 0.03866(13) Uani 1 1 d . . . . .
C24 C 0.9883(2) 0.8559(5) 0.5701(2) 0.0241(15) Uani 1 1 d . . . . .
H24 H 0.971572 0.923068 0.572681 0.029 Uiso 1 1 calc R U . . .
C25 C 0.9632(2) 0.7613(5) 0.5778(2) 0.0210(14) Uani 1 1 d . . . . .
C26 C 0.9088(3) 0.7704(6) 0.5877(5) 0.063(3) Uani 1 1 d . . . . .
H26A H 0.914703 0.782727 0.624428 0.076 Uiso 1 1 calc R U . . .
H26B H 0.890072 0.834632 0.569800 0.076 Uiso 1 1 calc R U . . .
N2 N 0.87348(18) 0.6823(4) 0.57343(19) 0.0157(11) Uani 1 1 d . . . . .
H2 H 0.878278 0.669358 0.539025 0.019 Uiso 1 1 calc R U . . .
C27 C 0.8148(2) 0.7079(5) 0.5587(2) 0.0160(13) Uani 1 1 d . . . . .
C28 C 0.7862(2) 0.6953(5) 0.5074(2) 0.0189(13) Uani 1 1 d . . . . .
C29 C 0.7301(3) 0.7206(5) 0.4931(3) 0.0260(15) Uani 1 1 d . . . . .
H29 H 0.709732 0.713963 0.458599 0.031 Uiso 1 1 calc R U . . .
C30 C 0.7043(3) 0.7543(5) 0.5276(3) 0.0283(16) Uani 1 1 d . . . . .
H30 H 0.666342 0.771228 0.517003 0.034 Uiso 1 1 calc R U . . .
C31 C 0.7329(2) 0.7639(5) 0.5776(3) 0.0244(15) Uani 1 1 d . . . . .
H31 H 0.714030 0.785419 0.601401 0.029 Uiso 1 1 calc R U . . .
C32 C 0.7891(2) 0.7429(5) 0.5945(2) 0.0191(13) Uani 1 1 d . . . . .
C33 C 0.8146(3) 0.6579(6) 0.4687(2) 0.0272(15) Uani 1 1 d . . . . .
H33 H 0.844170 0.607138 0.486510 0.033 Uiso 1 1 calc R U . . .
C34 C 0.7763(3) 0.5959(9) 0.4249(3) 0.071(3) Uani 1 1 d . . . . .
H34A H 0.758682 0.537530 0.438388 0.107 Uiso 1 1 calc R U . . .
H34B H 0.797543 0.566028 0.403281 0.107 Uiso 1 1 calc R U . . .
H34C H 0.748221 0.644566 0.404929 0.107 Uiso 1 1 calc R U . . .
C35 C 0.8420(4) 0.7488(7) 0.4489(3) 0.057(3) Uani 1 1 d . . . . .
H35A H 0.814146 0.799072 0.430008 0.086 Uiso 1 1 calc R U . . .
H35B H 0.862563 0.719964 0.426434 0.086 Uiso 1 1 calc R U . . .
H35C H 0.867208 0.786206 0.477310 0.086 Uiso 1 1 calc R U . . .
C36 C 0.8185(3) 0.7592(7) 0.6499(3) 0.0359(18) Uani 1 1 d . . . . .
H36 H 0.857858 0.739096 0.655333 0.043 Uiso 1 1 calc R U . . .
C37 C 0.7945(3) 0.6866(8) 0.6826(3) 0.056(3) Uani 1 1 d . . . . .
H37A H 0.756738 0.708444 0.679774 0.084 Uiso 1 1 calc R U . . .
H37B H 0.816480 0.692359 0.717960 0.084 Uiso 1 1 calc R U . . .
H37C H 0.794901 0.612197 0.671195 0.084 Uiso 1 1 calc R U . . .
C38 C 0.8162(4) 0.8782(7) 0.6648(3) 0.055(3) Uani 1 1 d . . . . .
H38A H 0.832593 0.922904 0.643620 0.082 Uiso 1 1 calc R U . . .
H38B H 0.836489 0.887682 0.700478 0.082 Uiso 1 1 calc R U . . .
H38C H 0.777885 0.899473 0.659887 0.082 Uiso 1 1 calc R U . . .
V2 V 0.62313(4) 0.85911(9) 0.68893(4) 0.0231(2) Uani 1 1 d . . . . .
O6 O 0.66362(18) 0.7804(4) 0.67165(17) 0.0310(11) Uani 1 1 d . . . . .
O4 O 0.64376(18) 1.0041(4) 0.70094(17) 0.0295(11) Uani 1 1 d . . . . .
C39 C 0.6841(3) 1.0597(6) 0.7325(2) 0.0261(15) Uani 1 1 d . . . . .
C40 C 0.6848(3) 1.1711(6) 0.7295(3) 0.0287(16) Uani 1 1 d . . . . .
I5 I 0.61986(2) 1.25157(4) 0.67807(2) 0.04278(14) Uani 1 1 d . . . . .
C41 C 0.7259(3) 1.2317(6) 0.7608(3) 0.0332(17) Uani 1 1 d . . . . .
H41 H 0.725725 1.307616 0.757720 0.040 Uiso 1 1 calc R U . . .
C42 C 0.7677(3) 1.1805(6) 0.7970(3) 0.0309(16) Uani 1 1 d . . . . .
I6 I 0.82793(2) 1.27107(4) 0.84718(2) 0.04431(14) Uani 1 1 d . . . . .
C43 C 0.7674(3) 1.0708(6) 0.8016(3) 0.0278(16) Uani 1 1 d . . . . .
H43 H 0.795724 1.036390 0.826691 0.033 Uiso 1 1 calc R U . . .
C44 C 0.7264(3) 1.0099(6) 0.7702(3) 0.0274(15) Uani 1 1 d . . . . .
C45 C 0.7262(3) 0.8900(6) 0.7765(3) 0.0350(18) Uani 1 1 d . . . . .
H45A H 0.740428 0.855290 0.750297 0.042 Uiso 1 1 calc R U . . .
H45B H 0.750395 0.869962 0.810107 0.042 Uiso 1 1 calc R U . . .
N3 N 0.6690(2) 0.8514(4) 0.77169(19) 0.0216(12) Uani 1 1 d . . . . .
H3A H 0.653432 0.915259 0.784800 0.026 Uiso 1 1 calc R U . . .
C46 C 0.6628(3) 0.7700(5) 0.8074(2) 0.0238(15) Uani 1 1 d . . . . .
C47 C 0.6894(3) 0.6696(6) 0.8102(3) 0.0288(16) Uani 1 1 d . . . . .
C48 C 0.6851(3) 0.5987(6) 0.8485(3) 0.0328(17) Uani 1 1 d . . . . .
H48 H 0.702738 0.530894 0.851181 0.039 Uiso 1 1 calc R U . . .
C49 C 0.6563(3) 0.6243(6) 0.8821(3) 0.0321(17) Uani 1 1 d . . . . .
H49 H 0.655294 0.576127 0.908600 0.039 Uiso 1 1 calc R U . . .
C50 C 0.6285(3) 0.7207(6) 0.8773(3) 0.0296(16) Uani 1 1 d . . . . .
H50 H 0.607902 0.737144 0.900294 0.036 Uiso 1 1 calc R U . . .
C51 C 0.6299(3) 0.7943(6) 0.8398(2) 0.0260(15) Uani 1 1 d . . . . .
C52 C 0.7198(3) 0.6321(6) 0.7735(3) 0.0359(18) Uani 1 1 d . . . . .
H52 H 0.722265 0.693853 0.751050 0.043 Uiso 1 1 calc R U . . .
C53 C 0.6874(4) 0.5428(7) 0.7404(3) 0.053(2) Uani 1 1 d . . . . .
H53A H 0.683844 0.481697 0.761740 0.080 Uiso 1 1 calc R U . . .
H53B H 0.706589 0.520018 0.715819 0.080 Uiso 1 1 calc R U . . .
H53C H 0.650813 0.569326 0.722446 0.080 Uiso 1 1 calc R U . . .
C54 C 0.7779(3) 0.5962(7) 0.8005(3) 0.050(2) Uani 1 1 d . . . . .
H54A H 0.798001 0.655822 0.820547 0.075 Uiso 1 1 calc R U . . .
H54B H 0.796575 0.573873 0.775394 0.075 Uiso 1 1 calc R U . . .
H54C H 0.776552 0.535730 0.822917 0.075 Uiso 1 1 calc R U . . .
C55 C 0.5979(3) 0.8981(6) 0.8367(3) 0.0324(17) Uani 1 1 d . . . . .
H55 H 0.591730 0.926851 0.801600 0.039 Uiso 1 1 calc R U . . .
C56 C 0.6304(3) 0.9811(6) 0.8727(3) 0.049(2) Uani 1 1 d . . . . .
H56A H 0.639674 0.953029 0.907345 0.073 Uiso 1 1 calc R U . . .
H56B H 0.608359 1.046443 0.870646 0.073 Uiso 1 1 calc R U . . .
H56C H 0.664075 0.997843 0.863542 0.073 Uiso 1 1 calc R U . . .
C57 C 0.5412(3) 0.8797(7) 0.8454(3) 0.049(2) Uani 1 1 d . . . . .
H57A H 0.522184 0.821787 0.823279 0.073 Uiso 1 1 calc R U . . .
H57B H 0.519516 0.945753 0.837573 0.073 Uiso 1 1 calc R U . . .
H57C H 0.545732 0.859946 0.880806 0.073 Uiso 1 1 calc R U . . .
O5 O 0.56909(17) 0.7977(4) 0.71416(16) 0.0251(10) Uani 1 1 d . . . . .
C58 C 0.5140(3) 0.7969(5) 0.6931(2) 0.0218(14) Uani 1 1 d . . . . .
C59 C 0.4816(3) 0.7227(5) 0.7092(2) 0.0264(15) Uani 1 1 d . . . . .
I7 I 0.51926(2) 0.60442(4) 0.76127(2) 0.03593(12) Uani 1 1 d . . . . .
C60 C 0.4245(3) 0.7229(6) 0.6887(3) 0.0330(17) Uani 1 1 d . . . . .
H60 H 0.402239 0.674106 0.700676 0.040 Uiso 1 1 calc R U . . .
C61 C 0.4015(3) 0.7948(6) 0.6512(3) 0.0304(16) Uani 1 1 d . . . . .
I8 I 0.31619(2) 0.78980(4) 0.61739(2) 0.03898(13) Uani 1 1 d . . . . .
C62 C 0.4329(3) 0.8670(5) 0.6334(3) 0.0278(15) Uani 1 1 d . . . . .
H62 H 0.415788 0.914758 0.606796 0.033 Uiso 1 1 calc R U . . .
C63 C 0.4895(3) 0.8706(5) 0.6541(3) 0.0264(15) Uani 1 1 d . . . . .
C64 C 0.5255(3) 0.9466(6) 0.6355(3) 0.0252(15) Uani 1 1 d . . . . .
H64A H 0.504378 0.979764 0.603249 0.030 Uiso 1 1 calc R U . . .
H64B H 0.538450 1.004516 0.660585 0.030 Uiso 1 1 calc R U . . .
N4 N 0.5730(2) 0.8879(4) 0.6276(2) 0.0237(12) Uani 1 1 d . . . . .
C65 C 0.5688(2) 0.8593(6) 0.5751(2) 0.0249(15) Uani 1 1 d . . . . .
C66 C 0.5793(3) 0.9415(6) 0.5438(3) 0.0291(16) Uani 1 1 d . . . . .
C67 C 0.5693(3) 0.9176(7) 0.4922(3) 0.0387(19) Uani 1 1 d . . . . .
H67 H 0.574904 0.971494 0.469735 0.046 Uiso 1 1 calc R U . . .
C68 C 0.5515(3) 0.8181(8) 0.4736(3) 0.043(2) Uani 1 1 d . . . . .
H68 H 0.543963 0.804562 0.438345 0.051 Uiso 1 1 calc R U . . .
C69 C 0.5444(3) 0.7381(7) 0.5052(3) 0.040(2) Uani 1 1 d . . . . .
H69 H 0.533400 0.668837 0.491750 0.048 Uiso 1 1 calc R U . . .
C70 C 0.5533(3) 0.7569(6) 0.5574(3) 0.0312(16) Uani 1 1 d . . . . .
C71 C 0.6045(3) 1.0476(6) 0.5654(3) 0.0328(17) Uani 1 1 d . . . . .
H71 H 0.588468 1.068045 0.593468 0.039 Uiso 1 1 calc R U . . .
C72 C 0.6672(3) 1.0359(7) 0.5882(3) 0.0397(19) Uani 1 1 d . . . . .
H72A H 0.674777 0.979294 0.613927 0.060 Uiso 1 1 calc R U . . .
H72B H 0.682472 1.103975 0.603782 0.060 Uiso 1 1 calc R U . . .
H72C H 0.684080 1.017196 0.561322 0.060 Uiso 1 1 calc R U . . .
C73 C 0.5940(3) 1.1400(7) 0.5272(3) 0.051(2) Uani 1 1 d . . . . .
H73A H 0.612833 1.125427 0.501252 0.077 Uiso 1 1 calc R U . . .
H73B H 0.608008 1.207021 0.544748 0.077 Uiso 1 1 calc R U . . .
H73C H 0.554581 1.146711 0.511257 0.077 Uiso 1 1 calc R U . . .
C74 C 0.5445(3) 0.6647(6) 0.5904(3) 0.0411(19) Uani 1 1 d . . . . .
H74 H 0.551027 0.692809 0.625679 0.049 Uiso 1 1 calc R U . . .
C75 C 0.5865(4) 0.5745(8) 0.5919(4) 0.068(3) Uani 1 1 d . . . . .
H75A H 0.581701 0.546625 0.557581 0.101 Uiso 1 1 calc R U . . .
H75B H 0.580775 0.516478 0.613911 0.101 Uiso 1 1 calc R U . . .
H75C H 0.623685 0.603083 0.605004 0.101 Uiso 1 1 calc R U . . .
C76 C 0.4858(4) 0.6232(8) 0.5733(4) 0.064(3) Uani 1 1 d . . . . .
H76A H 0.460339 0.682061 0.573790 0.096 Uiso 1 1 calc R U . . .
H76B H 0.480955 0.566282 0.596352 0.096 Uiso 1 1 calc R U . . .
H76C H 0.478253 0.594429 0.538926 0.096 Uiso 1 1 calc R U . . .
N5 N 1.0465(4) 0.5547(8) 0.8583(3) 0.092(4) Uani 1 1 d . . . . .
C77 C 1.0063(5) 0.5388(7) 0.8293(4) 0.060(3) Uani 1 1 d . . . . .
C78 C 0.9541(4) 0.5189(7) 0.7923(3) 0.061(3) Uani 1 1 d . . . . .
H78A H 0.937255 0.587460 0.778952 0.091 Uiso 1 1 calc R U . . .
H78B H 0.929858 0.480365 0.808485 0.091 Uiso 1 1 calc R U . . .
H78C H 0.959983 0.475583 0.764554 0.091 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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 N1 99.5(2) . . ?
O3 V1 O1 120.3(2) . . ?
N1 V1 O1 90.5(2) . . ?
O3 V1 O2 116.9(2) . . ?
N1 V1 O2 93.5(2) . . ?
O1 V1 O2 121.0(2) . . ?
O3 V1 N2 92.8(2) . . ?
N1 V1 N2 167.6(2) . . ?
O1 V1 N2 82.72(17) . . ?
O2 V1 N2 81.29(18) . . ?
C1 O1 V1 127.9(4) . . ?
O1 C1 C6 122.5(5) . . ?
O1 C1 C2 120.2(5) . . ?
C6 C1 C2 117.3(6) . . ?
C3 C2 C1 121.6(6) . . ?
C3 C2 I1 119.4(5) . . ?
C1 C2 I1 118.9(5) . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.3(6) . . ?
C3 C4 I2 119.5(4) . . ?
C5 C4 I2 120.1(5) . . ?
C6 C5 C4 119.1(6) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 121.8(6) . . ?
C1 C6 C7 117.9(5) . . ?
C5 C6 C7 120.1(5) . . ?
N1 C7 C6 109.0(5) . . ?
N1 C7 H7A 109.9 . . ?
C6 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C8 N1 C7 117.7(5) . . ?
C8 N1 V1 129.2(4) . . ?
C7 N1 V1 112.9(4) . . ?
C9 C8 C13 122.6(6) . . ?
C9 C8 N1 121.1(5) . . ?
C13 C8 N1 116.3(6) . . ?
C8 C9 C10 117.7(6) . . ?
C8 C9 C14 124.0(6) . . ?
C10 C9 C14 118.3(6) . . ?
C11 C10 C9 120.9(7) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.6(7) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 120.4(7) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C8 117.8(6) . . ?
C12 C13 C17 120.3(6) . . ?
C8 C13 C17 121.8(6) . . ?
C15 C14 C9 111.5(6) . . ?
C15 C14 C16 111.8(6) . . ?
C9 C14 C16 111.6(6) . . ?
C15 C14 H14 107.2 . . ?
C9 C14 H14 107.2 . . ?
C16 C14 H14 107.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C18 113.9(6) . . ?
C13 C17 C19 109.7(6) . . ?
C18 C17 C19 110.6(6) . . ?
C13 C17 H17 107.5 . . ?
C18 C17 H17 107.5 . . ?
C19 C17 H17 107.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 V1 136.4(4) . . ?
O2 C20 C25 123.5(6) . . ?
O2 C20 C21 119.9(6) . . ?
C25 C20 C21 116.5(6) . . ?
C22 C21 C20 122.2(6) . . ?
C22 C21 I3 118.5(5) . . ?
C20 C21 I3 119.3(5) . . ?
C23 C22 C21 119.0(6) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.8(6) . . ?
C22 C23 I4 119.4(5) . . ?
C24 C23 I4 119.9(5) . . ?
C25 C24 C23 119.4(6) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C20 121.7(6) . . ?
C24 C25 C26 117.1(6) . . ?
C20 C25 C26 121.2(6) . . ?
N2 C26 C25 116.4(7) . . ?
N2 C26 H26A 108.2 . . ?
C25 C26 H26A 108.2 . . ?
N2 C26 H26B 108.2 . . ?
C25 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C26 N2 C27 115.4(5) . . ?
C26 N2 V1 114.9(5) . . ?
C27 N2 V1 122.5(4) . . ?
C26 N2 H2 99.0 . . ?
C27 N2 H2 99.0 . . ?
V1 N2 H2 99.0 . . ?
C32 C27 C28 122.2(5) . . ?
C32 C27 N2 120.8(5) . . ?
C28 C27 N2 117.0(5) . . ?
C29 C28 C27 117.1(6) . . ?
C29 C28 C33 121.2(6) . . ?
C27 C28 C33 121.7(5) . . ?
C30 C29 C28 121.5(6) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C29 C30 C31 120.2(6) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C32 121.7(6) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C27 C32 C31 117.3(6) . . ?
C27 C32 C36 123.8(5) . . ?
C31 C32 C36 118.9(6) . . ?
C35 C33 C28 112.4(6) . . ?
C35 C33 C34 110.5(7) . . ?
C28 C33 C34 112.7(6) . . ?
C35 C33 H33 107.0 . . ?
C28 C33 H33 107.0 . . ?
C34 C33 H33 107.0 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C37 110.5(7) . . ?
C32 C36 C38 110.6(6) . . ?
C37 C36 C38 111.3(7) . . ?
C32 C36 H36 108.1 . . ?
C37 C36 H36 108.1 . . ?
C38 C36 H36 108.1 . . ?
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 . . ?
O6 V2 N4 100.8(2) . . ?
O6 V2 O5 117.6(2) . . ?
N4 V2 O5 91.6(2) . . ?
O6 V2 O4 118.3(2) . . ?
N4 V2 O4 93.5(2) . . ?
O5 V2 O4 121.7(2) . . ?
O6 V2 N3 94.5(2) . . ?
N4 V2 N3 164.7(2) . . ?
O5 V2 N3 80.50(18) . . ?
O4 V2 N3 79.80(19) . . ?
C39 O4 V2 137.4(4) . . ?
O4 C39 C40 119.9(6) . . ?
O4 C39 C44 122.5(6) . . ?
C40 C39 C44 117.6(6) . . ?
C41 C40 C39 121.9(6) . . ?
C41 C40 I5 118.3(5) . . ?
C39 C40 I5 119.7(5) . . ?
C40 C41 C42 119.3(7) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C43 C42 C41 120.0(6) . . ?
C43 C42 I6 120.0(5) . . ?
C41 C42 I6 119.9(5) . . ?
C42 C43 C44 120.8(6) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C39 120.3(6) . . ?
C43 C44 C45 120.0(6) . . ?
C39 C44 C45 119.7(6) . . ?
N3 C45 C44 110.0(6) . . ?
N3 C45 H45A 109.7 . . ?
C44 C45 H45A 109.7 . . ?
N3 C45 H45B 109.7 . . ?
C44 C45 H45B 109.7 . . ?
H45A C45 H45B 108.2 . . ?
C46 N3 C45 116.7(5) . . ?
C46 N3 V2 126.2(4) . . ?
C45 N3 V2 107.0(4) . . ?
C46 N3 H3A 100.6 . . ?
C45 N3 H3A 100.6 . . ?
V2 N3 H3A 100.6 . . ?
C47 C46 C51 120.8(6) . . ?
C47 C46 N3 121.1(6) . . ?
C51 C46 N3 118.1(6) . . ?
C48 C47 C46 117.7(6) . . ?
C48 C47 C52 118.0(6) . . ?
C46 C47 C52 124.3(6) . . ?
C49 C48 C47 121.9(7) . . ?
C49 C48 H48 119.1 . . ?
C47 C48 H48 119.1 . . ?
C48 C49 C50 119.5(7) . . ?
C48 C49 H49 120.2 . . ?
C50 C49 H49 120.2 . . ?
C49 C50 C51 122.0(7) . . ?
C49 C50 H50 119.0 . . ?
C51 C50 H50 119.0 . . ?
C50 C51 C46 117.8(6) . . ?
C50 C51 C55 118.8(6) . . ?
C46 C51 C55 123.3(6) . . ?
C47 C52 C54 111.9(6) . . ?
C47 C52 C53 109.5(6) . . ?
C54 C52 C53 111.4(7) . . ?
C47 C52 H52 107.9 . . ?
C54 C52 H52 107.9 . . ?
C53 C52 H52 107.9 . . ?
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 . . ?
C56 C55 C51 111.2(6) . . ?
C56 C55 C57 111.3(7) . . ?
C51 C55 C57 111.9(6) . . ?
C56 C55 H55 107.4 . . ?
C51 C55 H55 107.4 . . ?
C57 C55 H55 107.4 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C58 O5 V2 128.5(4) . . ?
O5 C58 C59 120.0(6) . . ?
O5 C58 C63 120.1(6) . . ?
C59 C58 C63 119.9(6) . . ?
C58 C59 C60 120.5(6) . . ?
C58 C59 I7 119.3(5) . . ?
C60 C59 I7 120.1(5) . . ?
C61 C60 C59 118.8(7) . . ?
C61 C60 H60 120.6 . . ?
C59 C60 H60 120.6 . . ?
C60 C61 C62 121.7(6) . . ?
C60 C61 I8 119.0(5) . . ?
C62 C61 I8 119.2(5) . . ?
C61 C62 C63 120.6(6) . . ?
C61 C62 H62 119.7 . . ?
C63 C62 H62 119.7 . . ?
C62 C63 C58 118.4(6) . . ?
C62 C63 C64 122.6(6) . . ?
C58 C63 C64 119.0(6) . . ?
N4 C64 C63 109.7(5) . . ?
N4 C64 H64A 109.7 . . ?
C63 C64 H64A 109.7 . . ?
N4 C64 H64B 109.7 . . ?
C63 C64 H64B 109.7 . . ?
H64A C64 H64B 108.2 . . ?
C65 N4 C64 115.3(5) . . ?
C65 N4 V2 134.3(4) . . ?
C64 N4 V2 110.3(4) . . ?
C70 C65 C66 122.7(6) . . ?
C70 C65 N4 120.4(6) . . ?
C66 C65 N4 116.8(6) . . ?
C67 C66 C65 116.8(7) . . ?
C67 C66 C71 121.4(7) . . ?
C65 C66 C71 121.6(6) . . ?
C68 C67 C66 121.3(8) . . ?
C68 C67 H67 119.4 . . ?
C66 C67 H67 119.4 . . ?
C69 C68 C67 120.8(8) . . ?
C69 C68 H68 119.6 . . ?
C67 C68 H68 119.6 . . ?
C68 C69 C70 120.9(8) . . ?
C68 C69 H69 119.5 . . ?
C70 C69 H69 119.5 . . ?
C65 C70 C69 117.4(7) . . ?
C65 C70 C74 124.2(6) . . ?
C69 C70 C74 118.4(7) . . ?
C66 C71 C73 114.3(7) . . ?
C66 C71 C72 110.6(6) . . ?
C73 C71 C72 108.2(6) . . ?
C66 C71 H71 107.8 . . ?
C73 C71 H71 107.8 . . ?
C72 C71 H71 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C70 C74 C76 111.5(7) . . ?
C70 C74 C75 110.5(7) . . ?
C76 C74 C75 111.8(8) . . ?
C70 C74 H74 107.6 . . ?
C76 C74 H74 107.6 . . ?
C75 C74 H74 107.6 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N5 C77 C78 179.3(14) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 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 1.599(4) . ?
V1 N1 1.856(5) . ?
V1 O1 1.873(4) . ?
V1 O2 1.887(4) . ?
V1 N2 2.228(5) . ?
O1 C1 1.344(7) . ?
C1 C6 1.392(8) . ?
C1 C2 1.409(8) . ?
C2 C3 1.383(9) . ?
C2 I1 2.104(6) . ?
C3 C4 1.384(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(8) . ?
C4 I2 2.094(6) . ?
C5 C6 1.396(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.520(8) . ?
C7 N1 1.477(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.450(8) . ?
C8 C9 1.386(9) . ?
C8 C13 1.420(9) . ?
C9 C10 1.398(9) . ?
C9 C14 1.526(9) . ?
C10 C11 1.389(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(10) . ?
C12 H12 0.9500 . ?
C13 C17 1.512(10) . ?
C14 C15 1.514(10) . ?
C14 C16 1.528(10) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.521(9) . ?
C17 C19 1.541(10) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.331(7) . ?
C20 C25 1.397(9) . ?
C20 C21 1.410(9) . ?
C21 C22 1.382(9) . ?
C21 I3 2.096(6) . ?
C22 C23 1.378(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(9) . ?
C23 I4 2.104(6) . ?
C24 C25 1.385(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.485(9) . ?
C26 N2 1.402(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
N2 C27 1.468(7) . ?
N2 H2 1.0000 . ?
C27 C32 1.393(9) . ?
C27 C28 1.407(8) . ?
C28 C29 1.404(8) . ?
C28 C33 1.513(9) . ?
C29 C30 1.361(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.371(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.399(8) . ?
C31 H31 0.9500 . ?
C32 C36 1.511(9) . ?
C33 C35 1.509(11) . ?
C33 C34 1.532(10) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.517(11) . ?
C36 C38 1.545(11) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
V2 O6 1.587(5) . ?
V2 N4 1.845(5) . ?
V2 O5 1.865(4) . ?
V2 O4 1.885(5) . ?
V2 N3 2.253(5) . ?
O4 C39 1.339(8) . ?
C39 C40 1.391(9) . ?
C39 C44 1.412(9) . ?
C40 C41 1.380(10) . ?
C40 I5 2.106(6) . ?
C41 C42 1.391(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(10) . ?
C42 I6 2.085(7) . ?
C43 C44 1.381(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.505(9) . ?
C45 N3 1.500(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
N3 C46 1.451(8) . ?
N3 H3A 1.0000 . ?
C46 C47 1.413(9) . ?
C46 C51 1.414(9) . ?
C47 C48 1.402(10) . ?
C47 C52 1.505(10) . ?
C48 C49 1.366(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(10) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(10) . ?
C50 H50 0.9500 . ?
C51 C55 1.516(10) . ?
C52 C54 1.524(10) . ?
C52 C53 1.527(11) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.509(10) . ?
C55 C57 1.543(10) . ?
C55 H55 1.0000 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
O5 C58 1.359(7) . ?
C58 C59 1.389(9) . ?
C58 C63 1.418(9) . ?
C59 C60 1.402(9) . ?
C59 I7 2.092(6) . ?
C60 C61 1.369(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.379(10) . ?
C61 I8 2.108(6) . ?
C62 C63 1.391(9) . ?
C62 H62 0.9500 . ?
C63 C64 1.503(9) . ?
C64 N4 1.477(8) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
N4 C65 1.462(8) . ?
C65 C70 1.385(10) . ?
C65 C66 1.410(10) . ?
C66 C67 1.401(10) . ?
C66 C71 1.517(11) . ?
C67 C68 1.370(12) . ?
C67 H67 0.9500 . ?
C68 C69 1.366(11) . ?
C68 H68 0.9500 . ?
C69 C70 1.410(10) . ?
C69 H69 0.9500 . ?
C70 C74 1.519(10) . ?
C71 C73 1.532(10) . ?
C71 C72 1.547(9) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C76 1.525(12) . ?
C74 C75 1.543(11) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N5 C77 1.124(12) . ?
C77 C78 1.451(13) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7B I3 0.99 3.30 4.193(7) 151.4 3_766 yes
C24 H24 N5 0.95 2.64 3.429(11) 140.3 2_756 yes
C45 H45A O6 0.99 2.65 3.187(9) 114.4 . yes
C64 H64B O4 0.99 2.60 3.126(8) 113.6 . yes
C64 H64B I7 0.99 3.17 3.875(7) 129.2 2_656 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 V1 O1 C1 -104.5(5) . . . . ?
N1 V1 O1 C1 -3.2(5) . . . . ?
O2 V1 O1 C1 91.2(5) . . . . ?
N2 V1 O1 C1 166.5(5) . . . . ?
V1 O1 C1 C6 -24.0(9) . . . . ?
V1 O1 C1 C2 153.5(5) . . . . ?
O1 C1 C2 C3 178.4(6) . . . . ?
C6 C1 C2 C3 -4.0(10) . . . . ?
O1 C1 C2 I1 -6.4(8) . . . . ?
C6 C1 C2 I1 171.2(5) . . . . ?
C1 C2 C3 C4 1.3(10) . . . . ?
I1 C2 C3 C4 -173.9(5) . . . . ?
C2 C3 C4 C5 2.7(10) . . . . ?
C2 C3 C4 I2 178.6(5) . . . . ?
C3 C4 C5 C6 -3.8(10) . . . . ?
I2 C4 C5 C6 -179.6(5) . . . . ?
O1 C1 C6 C5 -179.6(6) . . . . ?
C2 C1 C6 C5 2.8(9) . . . . ?
O1 C1 C6 C7 5.4(9) . . . . ?
C2 C1 C6 C7 -172.2(6) . . . . ?
C4 C5 C6 C1 1.0(9) . . . . ?
C4 C5 C6 C7 175.9(6) . . . . ?
C1 C6 C7 N1 43.3(8) . . . . ?
C5 C6 C7 N1 -131.8(6) . . . . ?
C6 C7 N1 C8 100.6(6) . . . . ?
C6 C7 N1 V1 -74.1(5) . . . . ?
O3 V1 N1 C8 -3.5(5) . . . . ?
O1 V1 N1 C8 -124.3(5) . . . . ?
O2 V1 N1 C8 114.6(5) . . . . ?
N2 V1 N1 C8 179(58) . . . . ?
O3 V1 N1 C7 170.5(4) . . . . ?
O1 V1 N1 C7 49.7(4) . . . . ?
O2 V1 N1 C7 -71.5(4) . . . . ?
N2 V1 N1 C7 -6.7(11) . . . . ?
C7 N1 C8 C9 -95.3(7) . . . . ?
V1 N1 C8 C9 78.4(7) . . . . ?
C7 N1 C8 C13 86.4(7) . . . . ?
V1 N1 C8 C13 -99.9(6) . . . . ?
C13 C8 C9 C10 -0.1(10) . . . . ?
N1 C8 C9 C10 -178.4(6) . . . . ?
C13 C8 C9 C14 177.7(6) . . . . ?
N1 C8 C9 C14 -0.6(10) . . . . ?
C8 C9 C10 C11 0.0(10) . . . . ?
C14 C9 C10 C11 -178.0(7) . . . . ?
C9 C10 C11 C12 -0.3(12) . . . . ?
C10 C11 C12 C13 0.8(12) . . . . ?
C11 C12 C13 C8 -0.9(11) . . . . ?
C11 C12 C13 C17 177.0(7) . . . . ?
C9 C8 C13 C12 0.6(10) . . . . ?
N1 C8 C13 C12 179.0(6) . . . . ?
C9 C8 C13 C17 -177.3(6) . . . . ?
N1 C8 C13 C17 1.1(9) . . . . ?
C8 C9 C14 C15 -112.6(7) . . . . ?
C10 C9 C14 C15 65.2(8) . . . . ?
C8 C9 C14 C16 121.5(7) . . . . ?
C10 C9 C14 C16 -60.7(8) . . . . ?
C12 C13 C17 C18 49.9(9) . . . . ?
C8 C13 C17 C18 -132.2(7) . . . . ?
C12 C13 C17 C19 -74.6(8) . . . . ?
C8 C13 C17 C19 103.2(7) . . . . ?
O3 V1 O2 C20 -63.8(6) . . . . ?
N1 V1 O2 C20 -166.3(6) . . . . ?
O1 V1 O2 C20 101.0(6) . . . . ?
N2 V1 O2 C20 25.0(6) . . . . ?
V1 O2 C20 C25 -2.5(10) . . . . ?
V1 O2 C20 C21 178.4(4) . . . . ?
O2 C20 C21 C22 -175.8(6) . . . . ?
C25 C20 C21 C22 5.0(9) . . . . ?
O2 C20 C21 I3 2.0(8) . . . . ?
C25 C20 C21 I3 -177.2(4) . . . . ?
C20 C21 C22 C23 0.7(9) . . . . ?
I3 C21 C22 C23 -177.1(5) . . . . ?
C21 C22 C23 C24 -5.4(10) . . . . ?
C21 C22 C23 I4 173.6(5) . . . . ?
C22 C23 C24 C25 4.0(10) . . . . ?
I4 C23 C24 C25 -175.0(5) . . . . ?
C23 C24 C25 C20 2.1(10) . . . . ?
C23 C24 C25 C26 -177.4(8) . . . . ?
O2 C20 C25 C24 174.5(6) . . . . ?
C21 C20 C25 C24 -6.4(9) . . . . ?
O2 C20 C25 C26 -6.1(11) . . . . ?
C21 C20 C25 C26 173.0(8) . . . . ?
C24 C25 C26 N2 152.4(7) . . . . ?
C20 C25 C26 N2 -27.1(12) . . . . ?
C25 C26 N2 C27 -150.1(7) . . . . ?
C25 C26 N2 V1 58.7(10) . . . . ?
C26 N2 C27 C32 -69.2(9) . . . . ?
V1 N2 C27 C32 79.6(6) . . . . ?
C26 N2 C27 C28 110.8(8) . . . . ?
V1 N2 C27 C28 -100.3(6) . . . . ?
C32 C27 C28 C29 0.6(9) . . . . ?
N2 C27 C28 C29 -179.5(5) . . . . ?
C32 C27 C28 C33 179.5(6) . . . . ?
N2 C27 C28 C33 -0.5(9) . . . . ?
C27 C28 C29 C30 -1.0(10) . . . . ?
C33 C28 C29 C30 -179.9(6) . . . . ?
C28 C29 C30 C31 -0.3(11) . . . . ?
C29 C30 C31 C32 2.0(10) . . . . ?
C28 C27 C32 C31 1.0(9) . . . . ?
N2 C27 C32 C31 -179.0(5) . . . . ?
C28 C27 C32 C36 -179.0(6) . . . . ?
N2 C27 C32 C36 1.0(9) . . . . ?
C30 C31 C32 C27 -2.3(9) . . . . ?
C30 C31 C32 C36 177.7(6) . . . . ?
C29 C28 C33 C35 94.9(8) . . . . ?
C27 C28 C33 C35 -84.0(8) . . . . ?
C29 C28 C33 C34 -30.7(10) . . . . ?
C27 C28 C33 C34 150.4(7) . . . . ?
C27 C32 C36 C37 -119.3(7) . . . . ?
C31 C32 C36 C37 60.7(8) . . . . ?
C27 C32 C36 C38 117.0(7) . . . . ?
C31 C32 C36 C38 -62.9(9) . . . . ?
O6 V2 O4 C39 -62.3(7) . . . . ?
N4 V2 O4 C39 -166.5(7) . . . . ?
O5 V2 O4 C39 99.4(7) . . . . ?
N3 V2 O4 C39 27.4(6) . . . . ?
V2 O4 C39 C40 -179.7(5) . . . . ?
V2 O4 C39 C44 -0.8(11) . . . . ?
O4 C39 C40 C41 -179.2(7) . . . . ?
C44 C39 C40 C41 1.9(11) . . . . ?
O4 C39 C40 I5 3.6(9) . . . . ?
C44 C39 C40 I5 -175.3(5) . . . . ?
C39 C40 C41 C42 -0.7(11) . . . . ?
I5 C40 C41 C42 176.4(5) . . . . ?
C40 C41 C42 C43 -0.6(11) . . . . ?
C40 C41 C42 I6 -176.9(5) . . . . ?
C41 C42 C43 C44 0.8(11) . . . . ?
I6 C42 C43 C44 177.1(5) . . . . ?
C42 C43 C44 C39 0.3(11) . . . . ?
C42 C43 C44 C45 -178.8(7) . . . . ?
O4 C39 C44 C43 179.5(6) . . . . ?
C40 C39 C44 C43 -1.7(10) . . . . ?
O4 C39 C44 C45 -1.4(11) . . . . ?
C40 C39 C44 C45 177.5(7) . . . . ?
C43 C44 C45 N3 137.8(7) . . . . ?
C39 C44 C45 N3 -41.3(9) . . . . ?
C44 C45 N3 C46 -137.9(6) . . . . ?
C44 C45 N3 V2 74.4(6) . . . . ?
C45 N3 C46 C47 -59.4(8) . . . . ?
V2 N3 C46 C47 81.2(7) . . . . ?
C45 N3 C46 C51 119.8(7) . . . . ?
V2 N3 C46 C51 -99.5(6) . . . . ?
C51 C46 C47 C48 -4.5(10) . . . . ?
N3 C46 C47 C48 174.8(6) . . . . ?
C51 C46 C47 C52 172.7(6) . . . . ?
N3 C46 C47 C52 -8.1(10) . . . . ?
C46 C47 C48 C49 0.2(10) . . . . ?
C52 C47 C48 C49 -177.1(7) . . . . ?
C47 C48 C49 C50 2.7(11) . . . . ?
C48 C49 C50 C51 -1.4(10) . . . . ?
C49 C50 C51 C46 -2.7(10) . . . . ?
C49 C50 C51 C55 179.5(6) . . . . ?
C47 C46 C51 C50 5.7(9) . . . . ?
N3 C46 C51 C50 -173.6(6) . . . . ?
C47 C46 C51 C55 -176.6(6) . . . . ?
N3 C46 C51 C55 4.1(9) . . . . ?
C48 C47 C52 C54 -55.9(9) . . . . ?
C46 C47 C52 C54 126.9(7) . . . . ?
C48 C47 C52 C53 68.1(8) . . . . ?
C46 C47 C52 C53 -109.0(8) . . . . ?
C50 C51 C55 C56 83.9(8) . . . . ?
C46 C51 C55 C56 -93.8(8) . . . . ?
C50 C51 C55 C57 -41.4(9) . . . . ?
C46 C51 C55 C57 141.0(7) . . . . ?
O6 V2 O5 C58 -111.7(5) . . . . ?
N4 V2 O5 C58 -8.7(5) . . . . ?
O4 V2 O5 C58 86.5(5) . . . . ?
N3 V2 O5 C58 158.1(5) . . . . ?
V2 O5 C58 C59 161.4(5) . . . . ?
V2 O5 C58 C63 -17.7(9) . . . . ?
O5 C58 C59 C60 178.3(6) . . . . ?
C63 C58 C59 C60 -2.6(10) . . . . ?
O5 C58 C59 I7 -5.5(8) . . . . ?
C63 C58 C59 I7 173.6(5) . . . . ?
C58 C59 C60 C61 2.5(11) . . . . ?
I7 C59 C60 C61 -173.7(5) . . . . ?
C59 C60 C61 C62 -0.5(11) . . . . ?
C59 C60 C61 I8 176.7(5) . . . . ?
C60 C61 C62 C63 -1.4(11) . . . . ?
I8 C61 C62 C63 -178.5(5) . . . . ?
C61 C62 C63 C58 1.2(10) . . . . ?
C61 C62 C63 C64 179.0(6) . . . . ?
O5 C58 C63 C62 179.9(6) . . . . ?
C59 C58 C63 C62 0.7(10) . . . . ?
O5 C58 C63 C64 2.0(9) . . . . ?
C59 C58 C63 C64 -177.1(6) . . . . ?
C62 C63 C64 N4 -132.4(6) . . . . ?
C58 C63 C64 N4 45.4(8) . . . . ?
C63 C64 N4 C65 100.5(6) . . . . ?
C63 C64 N4 V2 -75.6(6) . . . . ?
O6 V2 N4 C65 -4.5(7) . . . . ?
O5 V2 N4 C65 -122.9(6) . . . . ?
O4 V2 N4 C65 115.2(6) . . . . ?
N3 V2 N4 C65 178.7(7) . . . . ?
O6 V2 N4 C64 170.5(4) . . . . ?
O5 V2 N4 C64 52.1(4) . . . . ?
O4 V2 N4 C64 -69.8(4) . . . . ?
N3 V2 N4 C64 -6.3(11) . . . . ?
C64 N4 C65 C70 -99.4(7) . . . . ?
V2 N4 C65 C70 75.4(8) . . . . ?
C64 N4 C65 C66 78.4(7) . . . . ?
V2 N4 C65 C66 -106.8(7) . . . . ?
C70 C65 C66 C67 4.7(9) . . . . ?
N4 C65 C66 C67 -173.0(5) . . . . ?
C70 C65 C66 C71 -170.5(6) . . . . ?
N4 C65 C66 C71 11.8(9) . . . . ?
C65 C66 C67 C68 -1.7(10) . . . . ?
C71 C66 C67 C68 173.6(6) . . . . ?
C66 C67 C68 C69 -1.8(11) . . . . ?
C67 C68 C69 C70 2.4(11) . . . . ?
C66 C65 C70 C69 -4.2(10) . . . . ?
N4 C65 C70 C69 173.4(6) . . . . ?
C66 C65 C70 C74 176.7(6) . . . . ?
N4 C65 C70 C74 -5.7(10) . . . . ?
C68 C69 C70 C65 0.6(10) . . . . ?
C68 C69 C70 C74 179.7(7) . . . . ?
C67 C66 C71 C73 26.4(9) . . . . ?
C65 C66 C71 C73 -158.6(6) . . . . ?
C67 C66 C71 C72 -96.0(8) . . . . ?
C65 C66 C71 C72 79.0(8) . . . . ?
C65 C70 C74 C76 119.2(8) . . . . ?
C69 C70 C74 C76 -59.9(9) . . . . ?
C65 C70 C74 C75 -115.9(8) . . . . ?
C69 C70 C74 C75 65.0(9) . . . . ?
