# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1479864'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 N3 O3 V, 0.67(H2 O)'
_chemical_formula_sum            'C22 H21.33 N3 O3.67 V'
_chemical_formula_weight         437.36

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.390(3)
_cell_length_b                   17.480(4)
_cell_length_c                   22.770(5)
_cell_angle_alpha                100.25(3)
_cell_angle_beta                 98.44(3)
_cell_angle_gamma                106.11(3)
_cell_volume                     5665(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12000
_cell_measurement_theta_min      0.929
_cell_measurement_theta_max      25.999

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             2720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.560
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71074
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22234
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         0.929
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             22234
_reflns_number_gt                18937
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0994P)²+9.4564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22234
_refine_ls_number_parameters     1616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1619
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.27697(4) 0.36924(3) 0.79144(2) 0.01859(13) Uani 1 1 d . . . . .
O1 O 0.38535(17) 0.37524(16) 0.79708(12) 0.0296(6) Uani 1 1 d . . . . .
O2 O 0.21339(17) 0.27427(15) 0.77871(11) 0.0268(5) Uani 1 1 d . . . . .
O3 O 0.26880(18) 0.40328(14) 0.87443(11) 0.0264(5) Uani 1 1 d . . . . .
N1 N 0.24570(19) 0.35942(18) 0.69582(13) 0.0210(6) Uani 1 1 d . . . . .
N2 N 0.25741(19) 0.48259(17) 0.78126(12) 0.0202(6) Uani 1 1 d . . . . .
N3 N 0.3993(2) 0.56745(18) 1.07527(13) 0.0249(6) Uani 1 1 d . . . . .
C1 C 0.2430(2) 0.2934(2) 0.65547(16) 0.0251(7) Uani 1 1 d . . . . .
H1 H 0.2519 0.2487 0.6695 0.030 Uiso 1 1 calc R U . . .
C2 C 0.2273(2) 0.2887(2) 0.59262(17) 0.0284(8) Uani 1 1 d . . . . .
H2 H 0.2264 0.2418 0.5654 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2133(2) 0.3540(2) 0.57164(16) 0.0271(7) Uani 1 1 d . . . . .
H3 H 0.2037 0.3519 0.5300 0.032 Uiso 1 1 calc R U . . .
C4 C 0.2135(2) 0.4249(2) 0.61331(15) 0.0225(7) Uani 1 1 d . . . . .
C5 C 0.2011(2) 0.4960(2) 0.59698(16) 0.0242(7) Uani 1 1 d . . . . .
H5 H 0.1906 0.4982 0.5561 0.029 Uiso 1 1 calc R U . . .
C6 C 0.2046(2) 0.5618(2) 0.64140(17) 0.0257(7) Uani 1 1 d . . . . .
H6 H 0.1967 0.6084 0.6300 0.031 Uiso 1 1 calc R U . . .
C7 C 0.2198(2) 0.5608(2) 0.70387(16) 0.0236(7) Uani 1 1 d . . . . .
H7 H 0.2194 0.6053 0.7330 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2352(2) 0.4933(2) 0.72146(15) 0.0206(7) Uani 1 1 d . . . . .
C9 C 0.2313(2) 0.4249(2) 0.67613(15) 0.0193(6) Uani 1 1 d . . . . .
C10 C 0.2811(2) 0.5470(2) 0.82784(16) 0.0212(7) Uani 1 1 d . . . . .
H10 H 0.2802 0.5965 0.8184 0.025 Uiso 1 1 calc R U . . .
C11 C 0.3072(2) 0.5484(2) 0.88976(15) 0.0213(7) Uani 1 1 d . . . . .
C12 C 0.3374(2) 0.6245(2) 0.93249(16) 0.0226(7) Uani 1 1 d . . . . .
H12 H 0.3368 0.6712 0.9185 0.027 Uiso 1 1 calc R U . . .
C13 C 0.3673(2) 0.6324(2) 0.99311(16) 0.0251(7) Uani 1 1 d . . . . .
C14 C 0.4004(3) 0.7149(2) 1.03701(18) 0.0408(10) Uani 1 1 d . . . . .
H14A H 0.4647 0.7415 1.0368 0.049 Uiso 1 1 calc R U . . .
H14B H 0.3647 0.7488 1.0237 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3915(4) 0.7081(3) 1.0992(2) 0.0466(11) Uani 1 1 d . . . . .
H15A H 0.3267 0.6955 1.1013 0.056 Uiso 1 1 calc R U . . .
H15B H 0.4244 0.7607 1.1269 0.056 Uiso 1 1 calc R U . . .
C16 C 0.4271(3) 0.6456(3) 1.11970(18) 0.0403(10) Uani 1 1 d . . . . .
H16A H 0.4940 0.6666 1.1299 0.048 Uiso 1 1 calc R U . . .
H16B H 0.4060 0.6363 1.1567 0.048 Uiso 1 1 calc R U . . .
C17 C 0.4077(4) 0.4972(3) 1.09901(18) 0.0417(10) Uani 1 1 d . . . . .
H17A H 0.3535 0.4757 1.1153 0.050 Uiso 1 1 calc R U . . .
H17B H 0.4612 0.5151 1.1323 0.050 Uiso 1 1 calc R U . . .
C18 C 0.4174(3) 0.4302(3) 1.05230(19) 0.0361(9) Uani 1 1 d . . . . .
H18A H 0.4143 0.3826 1.0692 0.043 Uiso 1 1 calc R U . . .
H18B H 0.4770 0.4479 1.0412 0.043 Uiso 1 1 calc R U . . .
C19 C 0.3413(3) 0.4078(2) 0.99618(17) 0.0278(8) Uani 1 1 d . . . . .
H19A H 0.3525 0.3691 0.9644 0.033 Uiso 1 1 calc R U . . .
H19B H 0.2824 0.3820 1.0059 0.033 Uiso 1 1 calc R U . . .
C20 C 0.3375(2) 0.4829(2) 0.97368(15) 0.0214(7) Uani 1 1 d . . . . .
C21 C 0.3682(2) 0.5602(2) 1.01502(15) 0.0209(7) Uani 1 1 d . . . . .
C22 C 0.3049(2) 0.4767(2) 0.91196(15) 0.0218(7) Uani 1 1 d . . . . .
V4 V 0.67442(4) 0.12637(3) 0.24093(2) 0.01776(13) Uani 1 1 d . . . . .
O10 O 0.63110(17) 0.11772(16) 0.16955(11) 0.0274(5) Uani 1 1 d . . . . .
O11 O 0.71414(17) 0.22259(14) 0.27604(12) 0.0264(5) Uani 1 1 d . . . . .
O12 O 0.56739(16) 0.09589(14) 0.27541(11) 0.0233(5) Uani 1 1 d . . . . .
N10 N 0.81210(19) 0.13341(17) 0.23188(12) 0.0193(5) Uani 1 1 d . . . . .
N11 N 0.69011(18) 0.01227(17) 0.25286(12) 0.0181(5) Uani 1 1 d . . . . .
N12 N 0.2552(2) -0.06189(19) 0.26059(14) 0.0268(6) Uani 1 1 d . . . . .
C67 C 0.8696(2) 0.1984(2) 0.22088(16) 0.0240(7) Uani 1 1 d . . . . .
H67 H 0.8501 0.2438 0.2185 0.029 Uiso 1 1 calc R U . . .
C68 C 0.9593(2) 0.2017(2) 0.21269(16) 0.0263(7) Uani 1 1 d . . . . .
H68 H 0.9979 0.2481 0.2045 0.032 Uiso 1 1 calc R U . . .
C69 C 0.9890(2) 0.1358(2) 0.21695(15) 0.0249(7) Uani 1 1 d . . . . .
H69 H 1.0479 0.1369 0.2113 0.030 Uiso 1 1 calc R U . . .
C70 C 0.9298(2) 0.0656(2) 0.23006(14) 0.0195(6) Uani 1 1 d . . . . .
C71 C 0.9525(2) -0.0065(2) 0.23439(15) 0.0229(7) Uani 1 1 d . . . . .
H71 H 1.0101 -0.0100 0.2288 0.028 Uiso 1 1 calc R U . . .
C72 C 0.8900(2) -0.0711(2) 0.24686(15) 0.0228(7) Uani 1 1 d . . . . .
H72 H 0.9060 -0.1181 0.2497 0.027 Uiso 1 1 calc R U . . .
C73 C 0.8024(2) -0.0683(2) 0.25548(15) 0.0210(7) Uani 1 1 d . . . . .
H73 H 0.7620 -0.1123 0.2653 0.025 Uiso 1 1 calc R U . . .
C74 C 0.7761(2) -0.0001(2) 0.24939(13) 0.0173(6) Uani 1 1 d . . . . .
C75 C 0.8406(2) 0.0671(2) 0.23697(13) 0.0172(6) Uani 1 1 d . . . . .
C76 C 0.6191(2) -0.05060(19) 0.25311(14) 0.0180(6) Uani 1 1 d . . . . .
H76 H 0.6297 -0.1008 0.2506 0.022 Uiso 1 1 calc R U . . .
C77 C 0.5294(2) -0.0495(2) 0.25680(14) 0.0192(6) Uani 1 1 d . . . . .
C78 C 0.4604(2) -0.1250(2) 0.25169(15) 0.0215(7) Uani 1 1 d . . . . .
H78 H 0.4769 -0.1728 0.2467 0.026 Uiso 1 1 calc R U . . .
C79 C 0.3706(2) -0.1303(2) 0.25383(15) 0.0231(7) Uani 1 1 d . . . . .
C80 C 0.3001(3) -0.2121(2) 0.24913(18) 0.0299(8) Uani 1 1 d . . . . .
H80A H 0.3033 -0.2247 0.2890 0.036 Uiso 1 1 calc R U . . .
H80B H 0.3139 -0.2546 0.2220 0.036 Uiso 1 1 calc R U . . .
C81 C 0.2037(3) -0.2104(3) 0.2251(2) 0.0380(9) Uani 1 1 d . . . . .
H81A H 0.1971 -0.2080 0.1825 0.046 Uiso 1 1 calc R U . . .
H81B H 0.1585 -0.2602 0.2278 0.046 Uiso 1 1 calc R U . . .
C82 C 0.1859(3) -0.1379(3) 0.2609(2) 0.0365(9) Uani 1 1 d . . . . .
H82A H 0.1251 -0.1364 0.2435 0.044 Uiso 1 1 calc R U . . .
H82B H 0.1865 -0.1432 0.3026 0.044 Uiso 1 1 calc R U . . .
C83 C 0.2286(3) 0.0122(3) 0.2742(2) 0.0402(10) Uani 1 1 d . . . . .
H83A H 0.2398 0.0322 0.3181 0.048 Uiso 1 1 calc R U . . .
H83B H 0.1631 -0.0003 0.2580 0.048 Uiso 1 1 calc R U . . .
C84 C 0.2828(3) 0.0776(2) 0.2468(2) 0.0373(9) Uani 1 1 d . . . . .
H84A H 0.2649 0.1266 0.2569 0.045 Uiso 1 1 calc R U . . .
H84B H 0.2692 0.0590 0.2028 0.045 Uiso 1 1 calc R U . . .
C85 C 0.3857(2) 0.0970(2) 0.27144(17) 0.0261(7) Uani 1 1 d . . . . .
H85A H 0.4204 0.1319 0.2487 0.031 Uiso 1 1 calc R U . . .
H85B H 0.4012 0.1263 0.3139 0.031 Uiso 1 1 calc R U . . .
C86 C 0.3450(2) -0.0568(2) 0.26054(14) 0.0211(7) Uani 1 1 d . . . . .
C87 C 0.4123(2) 0.0193(2) 0.26630(15) 0.0201(6) Uani 1 1 d . . . . .
C88 C 0.5039(2) 0.0231(2) 0.26620(14) 0.0192(6) Uani 1 1 d . . . . .
V6 V 1.01927(4) 0.14569(3) -0.08582(2) 0.01587(12) Uani 1 1 d . . . . .
O16 O 1.05527(18) 0.21912(17) -0.02401(14) 0.0368(7) Uani 1 1 d . . . . .
O17 O 1.00653(18) 0.1870(2) -0.14377(14) 0.0389(7) Uani 1 1 d . . . . .
O18 O 0.89180(16) 0.09888(14) -0.08421(12) 0.0257(5) Uani 1 1 d . . . . .
N16 N 1.15616(18) 0.15219(16) -0.09638(12) 0.0165(5) Uani 1 1 d . . . . .
N17 N 1.03046(18) 0.02859(16) -0.08074(12) 0.0160(5) Uani 1 1 d . . . . .
N18 N 0.59593(19) -0.06300(17) -0.06874(13) 0.0199(6) Uani 1 1 d . . . . .
C111 C 1.2137(2) 0.2159(2) -0.10858(15) 0.0211(7) Uani 1 1 d . . . . .
H111 H 1.1944 0.2611 -0.1122 0.025 Uiso 1 1 calc R U . . .
C112 C 1.3036(2) 0.2179(2) -0.11635(16) 0.0231(7) Uani 1 1 d . . . . .
H112 H 1.3423 0.2634 -0.1256 0.028 Uiso 1 1 calc R U . . .
C113 C 1.3330(2) 0.1526(2) -0.11020(15) 0.0217(7) Uani 1 1 d . . . . .
H113 H 1.3922 0.1536 -0.1150 0.026 Uiso 1 1 calc R U . . .
C114 C 1.2734(2) 0.0832(2) -0.09652(14) 0.0176(6) Uani 1 1 d . . . . .
C115 C 1.2967(2) 0.0125(2) -0.08990(14) 0.0203(7) Uani 1 1 d . . . . .
H115 H 1.3549 0.0093 -0.0943 0.024 Uiso 1 1 calc R U . . .
C116 C 1.2342(2) -0.0516(2) -0.07707(15) 0.0211(7) Uani 1 1 d . . . . .
H116 H 1.2509 -0.0975 -0.0717 0.025 Uiso 1 1 calc R U . . .
C117 C 1.1450(2) -0.0493(2) -0.07186(15) 0.0201(6) Uani 1 1 d . . . . .
H117 H 1.1037 -0.0933 -0.0627 0.024 Uiso 1 1 calc R U . . .
C118 C 1.1184(2) 0.0180(2) -0.08022(13) 0.0165(6) Uani 1 1 d . . . . .
C119 C 1.1840(2) 0.08542(19) -0.09081(13) 0.0158(6) Uani 1 1 d . . . . .
C120 C 0.9614(2) -0.03670(18) -0.07945(14) 0.0168(6) Uani 1 1 d . . . . .
H120 H 0.9758 -0.0848 -0.0786 0.020 Uiso 1 1 calc R U . . .
C121 C 0.8704(2) -0.04035(19) -0.07924(14) 0.0175(6) Uani 1 1 d . . . . .
C122 C 0.8071(2) -0.11557(19) -0.07599(15) 0.0193(6) Uani 1 1 d . . . . .
H122 H 0.8280 -0.1607 -0.0764 0.023 Uiso 1 1 calc R U . . .
C123 C 0.7181(2) -0.12436(19) -0.07231(14) 0.0188(6) Uani 1 1 d . . . . .
C124 C 0.6550(2) -0.2050(2) -0.06639(17) 0.0243(7) Uani 1 1 d . . . . .
H12A H 0.6690 -0.2498 -0.0907 0.029 Uiso 1 1 calc R U . . .
H12B H 0.6658 -0.2090 -0.0242 0.029 Uiso 1 1 calc R U . . .
C125 C 0.5551(2) -0.2122(2) -0.08726(17) 0.0266(7) Uani 1 1 d . . . . .
H12C H 0.5158 -0.2604 -0.0779 0.032 Uiso 1 1 calc R U . . .
H12D H 0.5413 -0.2180 -0.1311 0.032 Uiso 1 1 calc R U . . .
C126 C 0.5356(2) -0.1363(2) -0.05541(16) 0.0238(7) Uani 1 1 d . . . . .
H12E H 0.4714 -0.1406 -0.0694 0.029 Uiso 1 1 calc R U . . .
H12F H 0.5465 -0.1319 -0.0117 0.029 Uiso 1 1 calc R U . . .
C127 C 0.5629(2) 0.0080(2) -0.06174(16) 0.0227(7) Uani 1 1 d . . . . .
H12G H 0.5801 0.0373 -0.0193 0.027 Uiso 1 1 calc R U . . .
H12H H 0.4961 -0.0099 -0.0738 0.027 Uiso 1 1 calc R U . . .
C128 C 0.6046(2) 0.0645(2) -0.10093(16) 0.0237(7) Uani 1 1 d . . . . .
H12I H 0.5853 0.0360 -0.1436 0.028 Uiso 1 1 calc R U . . .
H12J H 0.5829 0.1118 -0.0958 0.028 Uiso 1 1 calc R U . . .
C129 C 0.7092(2) 0.0918(2) -0.08236(16) 0.0222(7) Uani 1 1 d . . . . .
H12K H 0.7357 0.1199 -0.1117 0.027 Uiso 1 1 calc R U . . .
H12L H 0.7288 0.1300 -0.0428 0.027 Uiso 1 1 calc R U . . .
C130 C 0.6848(2) -0.05522(19) -0.07316(13) 0.0163(6) Uani 1 1 d . . . . .
C131 C 0.7442(2) 0.01969(18) -0.07903(14) 0.0159(6) Uani 1 1 d . . . . .
C132 C 0.8366(2) 0.02773(19) -0.08044(14) 0.0176(6) Uani 1 1 d . . . . .
V3 V 0.61066(4) 0.35571(3) 0.46066(2) 0.01737(12) Uani 1 1 d . . . . .
O7 O 0.5155(2) 0.28289(18) 0.45750(13) 0.0416(7) Uani 1 1 d . . . . .
O8 O 0.6904(2) 0.3132(2) 0.44878(12) 0.0417(7) Uani 1 1 d . . . . .
O9 O 0.65372(18) 0.40074(14) 0.54647(11) 0.0256(5) Uani 1 1 d . . . . .
N7 N 0.57893(18) 0.35201(16) 0.36576(12) 0.0175(5) Uani 1 1 d . . . . .
N8 N 0.59908(18) 0.47293(16) 0.45591(12) 0.0165(5) Uani 1 1 d . . . . .
N9 N 0.7270(2) 0.55761(17) 0.75133(12) 0.0216(6) Uani 1 1 d . . . . .
C45 C 0.5751(2) 0.2888(2) 0.32226(15) 0.0211(7) Uani 1 1 d . . . . .
H45 H 0.5857 0.2430 0.3333 0.025 Uiso 1 1 calc R U . . .
C46 C 0.5555(2) 0.2891(2) 0.26014(16) 0.0235(7) Uani 1 1 d . . . . .
H46 H 0.5549 0.2444 0.2308 0.028 Uiso 1 1 calc R U . . .
C47 C 0.5374(2) 0.3546(2) 0.24277(15) 0.0212(7) Uani 1 1 d . . . . .
H47 H 0.5236 0.3546 0.2016 0.025 Uiso 1 1 calc R U . . .
C48 C 0.5398(2) 0.42315(19) 0.28788(14) 0.0170(6) Uani 1 1 d . . . . .
C49 C 0.5231(2) 0.4945(2) 0.27529(15) 0.0202(6) Uani 1 1 d . . . . .
H49 H 0.5090 0.4989 0.2351 0.024 Uiso 1 1 calc R U . . .
C50 C 0.5276(2) 0.5576(2) 0.32252(15) 0.0207(7) Uani 1 1 d . . . . .
H50 H 0.5150 0.6039 0.3139 0.025 Uiso 1 1 calc R U . . .
C51 C 0.5509(2) 0.5534(2) 0.38350(15) 0.0205(6) Uani 1 1 d . . . . .
H51 H 0.5535 0.5968 0.4147 0.025 Uiso 1 1 calc R U . . .
C52 C 0.5701(2) 0.4854(2) 0.39764(14) 0.0178(6) Uani 1 1 d . . . . .
C53 C 0.5626(2) 0.41945(19) 0.34935(14) 0.0163(6) Uani 1 1 d . . . . .
C54 C 0.6166(2) 0.53551(19) 0.50368(14) 0.0169(6) Uani 1 1 d . . . . .
H54 H 0.6081 0.5833 0.4951 0.020 Uiso 1 1 calc R U . . .
C55 C 0.6460(2) 0.53745(19) 0.56488(15) 0.0183(6) Uani 1 1 d . . . . .
C56 C 0.6584(2) 0.6104(2) 0.60843(15) 0.0193(6) Uani 1 1 d . . . . .
H56 H 0.6474 0.6545 0.5947 0.023 Uiso 1 1 calc R U . . .
C57 C 0.6857(2) 0.6190(2) 0.66914(15) 0.0193(6) Uani 1 1 d . . . . .
C58 C 0.6978(2) 0.6982(2) 0.71343(15) 0.0244(7) Uani 1 1 d . . . . .
H58A H 0.7228 0.7438 0.6955 0.029 Uiso 1 1 calc R U . . .
H58B H 0.6381 0.7000 0.7214 0.029 Uiso 1 1 calc R U . . .
C59 C 0.7619(3) 0.7065(2) 0.77265(17) 0.0299(8) Uani 1 1 d . . . . .
H59A H 0.8245 0.7148 0.7662 0.036 Uiso 1 1 calc R U . . .
H59B H 0.7618 0.7535 0.8025 0.036 Uiso 1 1 calc R U . . .
C60 C 0.7310(3) 0.6304(2) 0.79609(16) 0.0272(7) Uani 1 1 d . . . . .
H60A H 0.7735 0.6353 0.8335 0.033 Uiso 1 1 calc R U . . .
H60B H 0.6703 0.6246 0.8054 0.033 Uiso 1 1 calc R U . . .
C61 C 0.7315(3) 0.4864(2) 0.77502(16) 0.0292(8) Uani 1 1 d . . . . .
H61A H 0.6699 0.4548 0.7773 0.035 Uiso 1 1 calc R U . . .
H61B H 0.7695 0.5041 0.8159 0.035 Uiso 1 1 calc R U . . .
C62 C 0.7719(3) 0.4335(2) 0.73423(16) 0.0290(8) Uani 1 1 d . . . . .
H62A H 0.7747 0.3863 0.7504 0.035 Uiso 1 1 calc R U . . .
H62B H 0.8342 0.4644 0.7329 0.035 Uiso 1 1 calc R U . . .
C63 C 0.7120(2) 0.4055(2) 0.67040(15) 0.0244(7) Uani 1 1 d . . . . .
H63A H 0.7430 0.3793 0.6428 0.029 Uiso 1 1 calc R U . . .
H63B H 0.6539 0.3656 0.6706 0.029 Uiso 1 1 calc R U . . .
C64 C 0.7024(2) 0.5503(2) 0.69035(14) 0.0184(6) Uani 1 1 d . . . . .
C65 C 0.6930(2) 0.4770(2) 0.64815(15) 0.0197(6) Uani 1 1 d . . . . .
C66 C 0.6641(2) 0.47016(19) 0.58579(14) 0.0185(6) Uani 1 1 d . . . . .
V2 V 0.31432(4) 0.07580(3) 0.58644(2) 0.01954(13) Uani 1 1 d . . . . .
O4 O 0.33209(18) 0.14493(16) 0.64925(12) 0.0313(6) Uani 1 1 d . . . . .
O5 O 0.29205(18) 0.11436(17) 0.52762(12) 0.0302(6) Uani 1 1 d . . . . .
O6 O 0.19448(17) 0.00667(15) 0.58306(13) 0.0301(6) Uani 1 1 d . . . . .
N4 N 0.4567(2) 0.11228(17) 0.58362(12) 0.0219(6) Uani 1 1 d . . . . .
N5 N 0.35436(19) -0.03161(17) 0.58775(12) 0.0193(5) Uani 1 1 d . . . . .
N6 N -0.0718(2) -0.19108(19) 0.60592(15) 0.0290(7) Uani 1 1 d . . . . .
C23 C 0.5027(3) 0.1873(2) 0.58019(16) 0.0275(8) Uani 1 1 d . . . . .
H23 H 0.4727 0.2269 0.5823 0.033 Uiso 1 1 calc R U . . .
C24 C 0.5947(3) 0.2090(2) 0.57351(16) 0.0301(8) Uani 1 1 d . . . . .
H24 H 0.6249 0.2620 0.5709 0.036 Uiso 1 1 calc R U . . .
C25 C 0.6400(3) 0.1519(2) 0.57086(16) 0.0281(8) Uani 1 1 d . . . . .
H25 H 0.7011 0.1659 0.5664 0.034 Uiso 1 1 calc R U . . .
C26 C 0.5942(2) 0.0717(2) 0.57488(14) 0.0213(7) Uani 1 1 d . . . . .
C27 C 0.6324(2) 0.0066(2) 0.57045(15) 0.0243(7) Uani 1 1 d . . . . .
H27 H 0.6938 0.0159 0.5670 0.029 Uiso 1 1 calc R U . . .
C28 C 0.5797(2) -0.0695(2) 0.57127(15) 0.0252(7) Uani 1 1 d . . . . .
H28 H 0.6058 -0.1117 0.5680 0.030 Uiso 1 1 calc R U . . .
C29 C 0.4869(2) -0.0867(2) 0.57684(15) 0.0227(7) Uani 1 1 d . . . . .
H29 H 0.4525 -0.1397 0.5768 0.027 Uiso 1 1 calc R U . . .
C30 C 0.4466(2) -0.0250(2) 0.58235(14) 0.0216(7) Uani 1 1 d . . . . .
C31 C 0.5007(2) 0.0547(2) 0.58075(14) 0.0200(6) Uani 1 1 d . . . . .
C32 C 0.3022(2) -0.1012(2) 0.59625(14) 0.0207(7) Uani 1 1 d . . . . .
H32 H 0.3300 -0.1417 0.5993 0.025 Uiso 1 1 calc R U . . .
C33 C 0.2093(2) -0.1201(2) 0.60107(14) 0.0202(6) Uani 1 1 d . . . . .
C34 C 0.1637(2) -0.1980(2) 0.61070(15) 0.0229(7) Uani 1 1 d . . . . .
H34 H 0.1974 -0.2341 0.6153 0.027 Uiso 1 1 calc R U . . .
C35 C 0.0726(2) -0.2221(2) 0.61353(15) 0.0227(7) Uani 1 1 d . . . . .
C36 C 0.0264(3) -0.3060(2) 0.62388(17) 0.0276(7) Uani 1 1 d . . . . .
H36A H 0.0545 -0.3449 0.6054 0.033 Uiso 1 1 calc R U . . .
H36B H 0.0356 -0.3036 0.6673 0.033 Uiso 1 1 calc R U . . .
C37 C -0.0761(3) -0.3344(2) 0.59650(19) 0.0328(8) Uani 1 1 d . . . . .
H37A H -0.0856 -0.3455 0.5524 0.039 Uiso 1 1 calc R U . . .
H37B H -0.1058 -0.3847 0.6079 0.039 Uiso 1 1 calc R U . . .
C38 C -0.1182(3) -0.2697(2) 0.61905(19) 0.0333(8) Uani 1 1 d . . . . .
H38A H -0.1832 -0.2873 0.5997 0.040 Uiso 1 1 calc R U . . .
H38B H -0.1138 -0.2628 0.6627 0.040 Uiso 1 1 calc R U . . .
C39 C -0.1231(3) -0.1318(3) 0.6082(2) 0.0402(10) Uani 1 1 d . . . . .
H39A H -0.1119 -0.1005 0.6498 0.048 Uiso 1 1 calc R U . . .
H39B H -0.1888 -0.1604 0.5949 0.048 Uiso 1 1 calc R U . . .
C40 C -0.0928(3) -0.0747(3) 0.5674(2) 0.0428(10) Uani 1 1 d . . . . .
H40A H -0.1075 -0.1057 0.5254 0.051 Uiso 1 1 calc R U . . .
H40B H -0.1262 -0.0350 0.5697 0.051 Uiso 1 1 calc R U . . .
C41 C 0.0095(2) -0.0306(2) 0.58578(18) 0.0291(8) Uani 1 1 d . . . . .
H41A H 0.0221 0.0111 0.6230 0.035 Uiso 1 1 calc R U . . .
H41B H 0.0295 -0.0036 0.5541 0.035 Uiso 1 1 calc R U . . .
C42 C 0.0202(2) -0.1669(2) 0.60562(15) 0.0240(7) Uani 1 1 d . . . . .
C43 C 0.0636(2) -0.0892(2) 0.59590(15) 0.0230(7) Uani 1 1 d . . . . .
C44 C 0.1568(2) -0.0654(2) 0.59406(15) 0.0221(7) Uani 1 1 d . . . . .
V5 V 0.95014(4) 0.42660(3) 0.16115(2) 0.01687(12) Uani 1 1 d . . . . .
O13 O 1.04056(17) 0.39496(16) 0.15705(11) 0.0285(5) Uani 1 1 d . . . . .
O14 O 0.86387(18) 0.35336(16) 0.16944(12) 0.0308(6) Uani 1 1 d . . . . .
O15 O 0.98607(18) 0.49386(14) 0.24105(11) 0.0253(5) Uani 1 1 d . . . . .
N13 N 0.90572(18) 0.38927(16) 0.06512(13) 0.0202(6) Uani 1 1 d . . . . .
N14 N 0.93632(18) 0.53368(16) 0.13341(12) 0.0166(5) Uani 1 1 d . . . . .
N15 N 1.0590(2) 0.69852(19) 0.42367(13) 0.0286(7) Uani 1 1 d . . . . .
C89 C 0.8942(2) 0.3141(2) 0.03398(16) 0.0234(7) Uani 1 1 d . . . . .
H89 H 0.8991 0.2744 0.0554 0.028 Uiso 1 1 calc R U . . .
C90 C 0.8751(2) 0.2923(2) -0.02994(17) 0.0275(8) Uani 1 1 d . . . . .
H90 H 0.8684 0.2393 -0.0504 0.033 Uiso 1 1 calc R U . . .
C91 C 0.8663(2) 0.3502(2) -0.06178(17) 0.0259(7) Uani 1 1 d . . . . .
H91 H 0.8547 0.3366 -0.1042 0.031 Uiso 1 1 calc R U . . .
C92 C 0.8747(2) 0.4299(2) -0.03084(15) 0.0212(7) Uani 1 1 d . . . . .
C93 C 0.8682(2) 0.4947(2) -0.05886(15) 0.0221(7) Uani 1 1 d . . . . .
H93 H 0.8545 0.4855 -0.1012 0.027 Uiso 1 1 calc R U . . .
C94 C 0.8819(2) 0.5707(2) -0.02374(16) 0.0225(7) Uani 1 1 d . . . . .
H94 H 0.8765 0.6125 -0.0428 0.027 Uiso 1 1 calc R U . . .
C95 C 0.9038(2) 0.5876(2) 0.04032(15) 0.0205(6) Uani 1 1 d . . . . .
H95 H 0.9132 0.6401 0.0629 0.025 Uiso 1 1 calc R U . . .
C96 C 0.9116(2) 0.5265(2) 0.06983(15) 0.0183(6) Uani 1 1 d . . . . .
C97 C 0.8964(2) 0.4472(2) 0.03387(15) 0.0187(6) Uani 1 1 d . . . . .
C98 C 0.9474(2) 0.60489(19) 0.17044(15) 0.0182(6) Uani 1 1 d . . . . .
H98 H 0.9361 0.6457 0.1522 0.022 Uiso 1 1 calc R U . . .
C99 C 0.9740(2) 0.62516(19) 0.23378(14) 0.0175(6) Uani 1 1 d . . . . .
C100 C 0.9816(2) 0.7050(2) 0.26620(16) 0.0212(7) Uani 1 1 d . . . . .
H100 H 0.9687 0.7419 0.2441 0.025 Uiso 1 1 calc R U . . .
C101 C 1.0069(2) 0.7298(2) 0.32788(15) 0.0211(7) Uani 1 1 d . . . . .
C102 C 1.0092(3) 0.8143(2) 0.36032(17) 0.0270(7) Uani 1 1 d . . . . .
H10A H 1.0288 0.8530 0.3355 0.032 Uiso 1 1 calc R U . . .
H10B H 0.9475 0.8132 0.3658 0.032 Uiso 1 1 calc R U . . .
C103 C 1.0742(3) 0.8415(3) 0.42129(18) 0.0384(9) Uani 1 1 d . . . . .
H10C H 1.1373 0.8530 0.4156 0.046 Uiso 1 1 calc R U . . .
H10D H 1.0677 0.8914 0.4439 0.046 Uiso 1 1 calc R U . . .
C104 C 1.0543(4) 0.7769(3) 0.45674(19) 0.0426(10) Uani 1 1 d . . . . .
H10E H 1.0986 0.7948 0.4953 0.051 Uiso 1 1 calc R U . . .
H10F H 0.9931 0.7692 0.4656 0.051 Uiso 1 1 calc R U . . .
C105 C 1.0664(4) 0.6387(3) 0.45952(19) 0.0533(14) Uani 1 1 d . . . . .
H10G H 1.1086 0.6667 0.4982 0.064 Uiso 1 1 calc R U . . .
H10H H 1.0063 0.6141 0.4681 0.064 Uiso 1 1 calc R U . . .
C106 C 1.0982(5) 0.5750(3) 0.4304(2) 0.0579(15) Uani 1 1 d . . . . .
H10I H 1.0930 0.5341 0.4545 0.069 Uiso 1 1 calc R U . . .
H10J H 1.1631 0.5980 0.4301 0.069 Uiso 1 1 calc R U . . .
C107 C 1.0465(3) 0.5335(2) 0.36593(16) 0.0263(7) Uani 1 1 d . . . . .
H10K H 0.9897 0.4924 0.3667 0.032 Uiso 1 1 calc R U . . .
H10L H 1.0839 0.5060 0.3449 0.032 Uiso 1 1 calc R U . . .
C108 C 1.0302(2) 0.6742(2) 0.36202(15) 0.0224(7) Uani 1 1 d . . . . .
C109 C 1.0241(2) 0.5943(2) 0.33169(15) 0.0212(7) Uani 1 1 d . . . . .
C110 C 0.9942(2) 0.5691(2) 0.26841(15) 0.0195(6) Uani 1 1 d . . . . .
O1W O 0.4701(2) 0.27810(19) 0.73222(16) 0.0466(8) Uani 1 1 d G . . . .
H1WA H 0.4307 0.2362 0.7079 0.070 Uiso 1 1 d G U . . .
H1WB H 0.4428 0.3027 0.7553 0.070 Uiso 1 1 d G U . . .
O3W O 0.7092(2) 0.22025(19) 0.09886(15) 0.0458(8) Uani 1 1 d G . . . .
H3WA H 0.6826 0.1906 0.1209 0.069 Uiso 1 1 d G U . . .
H3WB H 0.7577 0.2565 0.1208 0.069 Uiso 1 1 d G U . . .
O4W O 1.0628(3) 0.24348(19) 0.10094(15) 0.0453(8) Uani 1 1 d G . . . .
H4WA H 1.0583 0.2898 0.1166 0.068 Uiso 1 1 d G U . . .
H4WB H 1.0679 0.2414 0.0641 0.068 Uiso 1 1 d G U . . .
O2W O 0.3409(3) 0.2569(2) 0.48303(19) 0.0541(9) Uani 1 1 d G . . . .
H2WA H 0.3178 0.2109 0.4914 0.081 Uiso 1 1 d G U . . .
H2WB H 0.3941 0.2601 0.4754 0.081 Uiso 1 1 d G U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O2 1.625(2) . ?
V1 O1 1.626(3) . ?
V1 O3 1.911(2) . ?
V1 N1 2.125(3) . ?
V1 N2 2.132(3) . ?
O3 C22 1.327(4) . ?
N1 C1 1.328(5) . ?
N1 C9 1.362(4) . ?
N2 C10 1.327(4) . ?
N2 C8 1.413(4) . ?
N3 C21 1.356(4) . ?
N3 C17 1.457(5) . ?
N3 C16 1.460(5) . ?
C1 C2 1.400(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.419(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.412(5) . ?
C4 C9 1.416(5) . ?
C5 C6 1.374(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.411(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.379(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.415(5) . ?
C10 C11 1.402(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.412(5) . ?
C11 C22 1.425(5) . ?
C12 C13 1.359(5) . ?
C12 H12 0.9300 . ?
C13 C21 1.440(5) . ?
C13 C14 1.506(5) . ?
C14 C15 1.464(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.466(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.490(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.512(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.504(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C22 1.395(5) . ?
C20 C21 1.413(5) . ?
V4 O10 1.627(3) . ?
V4 O11 1.628(2) . ?
V4 O12 1.912(2) . ?
V4 N10 2.131(3) . ?
V4 N11 2.133(3) . ?
O12 C88 1.331(4) . ?
N10 C67 1.322(4) . ?
N10 C75 1.366(4) . ?
N11 C76 1.319(4) . ?
N11 C74 1.410(4) . ?
N12 C86 1.359(4) . ?
N12 C82 1.457(5) . ?
N12 C83 1.460(5) . ?
C67 C68 1.407(5) . ?
C67 H67 0.9300 . ?
C68 C69 1.365(5) . ?
C68 H68 0.9300 . ?
C69 C70 1.419(5) . ?
C69 H69 0.9300 . ?
C70 C75 1.411(4) . ?
C70 C71 1.413(5) . ?
C71 C72 1.368(5) . ?
C71 H71 0.9300 . ?
C72 C73 1.404(5) . ?
C72 H72 0.9300 . ?
C73 C74 1.384(5) . ?
C73 H73 0.9300 . ?
C74 C75 1.414(5) . ?
C76 C77 1.400(5) . ?
C76 H76 0.9300 . ?
C77 C78 1.420(5) . ?
C77 C88 1.421(5) . ?
C78 C79 1.368(5) . ?
C78 H78 0.9300 . ?
C79 C86 1.435(5) . ?
C79 C80 1.512(5) . ?
C80 C81 1.515(6) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C81 C82 1.495(6) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C83 C84 1.506(6) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 C85 1.520(5) . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C85 C87 1.514(5) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C86 C87 1.411(5) . ?
C87 C88 1.393(5) . ?
V6 O17 1.626(3) . ?
V6 O16 1.634(3) . ?
V6 O18 1.913(2) . ?
V6 N17 2.123(3) . ?
V6 N16 2.129(3) . ?
O18 C132 1.323(4) . ?
N16 C111 1.318(4) . ?
N16 C119 1.370(4) . ?
N17 C120 1.335(4) . ?
N17 C118 1.415(4) . ?
N18 C130 1.357(4) . ?
N18 C127 1.458(4) . ?
N18 C126 1.468(4) . ?
C111 C112 1.412(5) . ?
C111 H111 0.9300 . ?
C112 C113 1.360(5) . ?
C112 H112 0.9300 . ?
C113 C114 1.419(5) . ?
C113 H113 0.9300 . ?
C114 C115 1.405(5) . ?
C114 C119 1.411(4) . ?
C115 C116 1.366(5) . ?
C115 H115 0.9300 . ?
C116 C117 1.405(5) . ?
C116 H116 0.9300 . ?
C117 C118 1.383(4) . ?
C117 H117 0.9300 . ?
C118 C119 1.407(4) . ?
C120 C121 1.385(4) . ?
C120 H120 0.9300 . ?
C121 C122 1.424(4) . ?
C121 C132 1.428(4) . ?
C122 C123 1.351(5) . ?
C122 H122 0.9300 . ?
C123 C130 1.440(4) . ?
C123 C124 1.515(4) . ?
C124 C125 1.504(5) . ?
C124 H12A 0.9700 . ?
C124 H12B 0.9700 . ?
C125 C126 1.522(5) . ?
C125 H12C 0.9700 . ?
C125 H12D 0.9700 . ?
C126 H12E 0.9700 . ?
C126 H12F 0.9700 . ?
C127 C128 1.521(5) . ?
C127 H12G 0.9700 . ?
C127 H12H 0.9700 . ?
C128 C129 1.516(5) . ?
C128 H12I 0.9700 . ?
C128 H12J 0.9700 . ?
C129 C131 1.512(4) . ?
C129 H12K 0.9700 . ?
C129 H12L 0.9700 . ?
C130 C131 1.415(4) . ?
C131 C132 1.394(4) . ?
V3 O8 1.632(3) . ?
V3 O7 1.634(3) . ?
V3 O9 1.913(2) . ?
V3 N8 2.125(3) . ?
V3 N7 2.129(3) . ?
O9 C66 1.328(4) . ?
N7 C45 1.327(4) . ?
N7 C53 1.373(4) . ?
N8 C54 1.334(4) . ?
N8 C52 1.411(4) . ?
N9 C64 1.358(4) . ?
N9 C61 1.457(5) . ?
N9 C60 1.463(4) . ?
C45 C46 1.403(5) . ?
C45 H45 0.9300 . ?
C46 C47 1.361(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.420(5) . ?
C47 H47 0.9300 . ?
C48 C53 1.410(4) . ?
C48 C49 1.410(5) . ?
C49 C50 1.375(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.402(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.380(5) . ?
C51 H51 0.9300 . ?
C52 C53 1.411(5) . ?
C54 C55 1.392(4) . ?
C54 H54 0.9300 . ?
C55 C56 1.416(5) . ?
C55 C66 1.425(4) . ?
C56 C57 1.353(5) . ?
C56 H56 0.9300 . ?
C57 C64 1.442(5) . ?
C57 C58 1.508(5) . ?
C58 C59 1.508(5) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.501(5) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C62 1.512(5) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.518(5) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C65 1.512(4) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 C65 1.417(5) . ?
C65 C66 1.398(5) . ?
V2 O4 1.633(3) . ?
V2 O5 1.637(2) . ?
V2 O6 1.886(3) . ?
V2 N4 2.119(3) . ?
V2 N5 2.136(3) . ?
O6 C44 1.318(4) . ?
N4 C23 1.329(5) . ?
N4 C31 1.358(4) . ?
N5 C32 1.323(4) . ?
N5 C30 1.417(4) . ?
N6 C42 1.362(5) . ?
N6 C39 1.465(5) . ?
N6 C38 1.467(5) . ?
C23 C24 1.400(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.364(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.410(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.414(5) . ?
C26 C31 1.417(5) . ?
C27 C28 1.358(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.405(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.382(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.420(5) . ?
C32 C33 1.400(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.420(5) . ?
C33 C44 1.427(5) . ?
C34 C35 1.363(5) . ?
C34 H34 0.9300 . ?
C35 C42 1.437(5) . ?
C35 C36 1.518(5) . ?
C36 C37 1.512(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.504(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.509(6) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.505(6) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C43 1.515(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.409(5) . ?
C43 C44 1.388(5) . ?
V5 O14 1.629(3) . ?
V5 O13 1.642(2) . ?
V5 O15 1.892(3) . ?
V5 N13 2.117(3) . ?
V5 N14 2.133(3) . ?
O15 C110 1.315(4) . ?
N13 C89 1.327(4) . ?
N13 C97 1.363(4) . ?
N14 C98 1.325(4) . ?
N14 C96 1.415(4) . ?
N15 C108 1.359(5) . ?
N15 C105 1.455(5) . ?
N15 C104 1.467(5) . ?
C89 C90 1.402(5) . ?
C89 H89 0.9300 . ?
C90 C91 1.369(5) . ?
C90 H90 0.9300 . ?
C91 C92 1.407(5) . ?
C91 H91 0.9300 . ?
C92 C93 1.415(5) . ?
C92 C97 1.420(5) . ?
C93 C94 1.366(5) . ?
C93 H93 0.9300 . ?
C94 C95 1.405(5) . ?
C94 H94 0.9300 . ?
C95 C96 1.381(5) . ?
C95 H95 0.9300 . ?
C96 C97 1.417(5) . ?
C98 C99 1.392(5) . ?
C98 H98 0.9300 . ?
C99 C100 1.423(5) . ?
C99 C110 1.431(4) . ?
C100 C101 1.357(5) . ?
C100 H100 0.9300 . ?
C101 C108 1.435(5) . ?
C101 C102 1.518(5) . ?
C102 C103 1.499(5) . ?
C102 H10A 0.9700 . ?
C102 H10B 0.9700 . ?
C103 C104 1.492(6) . ?
C103 H10C 0.9700 . ?
C103 H10D 0.9700 . ?
C104 H10E 0.9700 . ?
C104 H10F 0.9700 . ?
C105 C106 1.432(7) . ?
C105 H10G 0.9700 . ?
C105 H10H 0.9700 . ?
C106 C107 1.507(6) . ?
C106 H10I 0.9700 . ?
C106 H10J 0.9700 . ?
C107 C109 1.509(5) . ?
C107 H10K 0.9700 . ?
C107 H10L 0.9700 . ?
C108 C109 1.414(5) . ?
C109 C110 1.396(5) . ?
O1W H1WA 0.8494 . ?
O1W H1WB 0.8500 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8503 . ?
O4W H4WA 0.8504 . ?
O4W H4WB 0.8500 . ?
O2W H2WA 0.8508 . ?
O2W H2WB 0.8505 . ?

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
O2 V1 O1 110.24(14) . . ?
O2 V1 O3 98.41(12) . . ?
O1 V1 O3 102.74(13) . . ?
O2 V1 N1 87.78(12) . . ?
O1 V1 N1 96.98(12) . . ?
O3 V1 N1 155.70(11) . . ?
O2 V1 N2 137.16(12) . . ?
O1 V1 N2 110.43(12) . . ?
O3 V1 N2 85.28(11) . . ?
N1 V1 N2 74.53(11) . . ?
C22 O3 V1 129.1(2) . . ?
C1 N1 C9 119.7(3) . . ?
C1 N1 V1 122.3(2) . . ?
C9 N1 V1 117.9(2) . . ?
C10 N2 C8 118.9(3) . . ?
C10 N2 V1 122.1(2) . . ?
C8 N2 V1 117.9(2) . . ?
C21 N3 C17 121.5(3) . . ?
C21 N3 C16 122.2(3) . . ?
C17 N3 C16 116.3(3) . . ?
N1 C1 C2 122.2(3) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C9 118.0(3) . . ?
C5 C4 C3 125.0(3) . . ?
C9 C4 C3 116.9(3) . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 N2 128.2(3) . . ?
C7 C8 C9 119.1(3) . . ?
N2 C8 C9 112.7(3) . . ?
N1 C9 C8 116.8(3) . . ?
N1 C9 C4 121.8(3) . . ?
C8 C9 C4 121.4(3) . . ?
N2 C10 C11 126.9(3) . . ?
N2 C10 H10 116.6 . . ?
C11 C10 H10 116.6 . . ?
C10 C11 C12 118.6(3) . . ?
C10 C11 C22 123.3(3) . . ?
C12 C11 C22 118.1(3) . . ?
C13 C12 C11 122.9(3) . . ?
C13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C12 C13 C21 118.8(3) . . ?
C12 C13 C14 121.2(3) . . ?
C21 C13 C14 120.0(3) . . ?
C15 C14 C13 111.7(4) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 114.1(4) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N3 C16 C15 114.6(3) . . ?
N3 C16 H16A 108.6 . . ?
C15 C16 H16A 108.6 . . ?
N3 C16 H16B 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
N3 C17 C18 113.4(3) . . ?
N3 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
N3 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 C19 110.4(3) . . ?
C17 C18 H18A 109.6 . . ?
C19 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 110.4(3) . . ?
C20 C19 H19A 109.6 . . ?
C18 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C22 C20 C21 119.8(3) . . ?
C22 C20 C19 120.2(3) . . ?
C21 C20 C19 119.9(3) . . ?
N3 C21 C20 120.7(3) . . ?
N3 C21 C13 119.4(3) . . ?
C20 C21 C13 119.9(3) . . ?
O3 C22 C20 119.4(3) . . ?
O3 C22 C11 120.2(3) . . ?
C20 C22 C11 120.4(3) . . ?
O10 V4 O11 109.69(14) . . ?
O10 V4 O12 103.27(12) . . ?
O11 V4 O12 98.37(12) . . ?
O10 V4 N10 97.78(12) . . ?
O11 V4 N10 87.65(12) . . ?
O12 V4 N10 154.58(11) . . ?
O10 V4 N11 109.27(12) . . ?
O11 V4 N11 138.85(12) . . ?
O12 V4 N11 85.15(10) . . ?
N10 V4 N11 74.46(11) . . ?
C88 O12 V4 129.4(2) . . ?
C67 N10 C75 119.4(3) . . ?
C67 N10 V4 122.7(2) . . ?
C75 N10 V4 117.9(2) . . ?
C76 N11 C74 119.0(3) . . ?
C76 N11 V4 122.1(2) . . ?
C74 N11 V4 117.9(2) . . ?
C86 N12 C82 122.3(3) . . ?
C86 N12 C83 120.4(3) . . ?
C82 N12 C83 115.9(3) . . ?
N10 C67 C68 122.5(3) . . ?
N10 C67 H67 118.7 . . ?
C68 C67 H67 118.7 . . ?
C69 C68 C67 119.1(3) . . ?
C69 C68 H68 120.4 . . ?
C67 C68 H68 120.4 . . ?
C68 C69 C70 119.9(3) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C75 C70 C71 117.9(3) . . ?
C75 C70 C69 117.3(3) . . ?
C71 C70 C69 124.7(3) . . ?
C72 C71 C70 120.1(3) . . ?
C72 C71 H71 119.9 . . ?
C70 C71 H71 119.9 . . ?
C71 C72 C73 121.7(3) . . ?
C71 C72 H72 119.1 . . ?
C73 C72 H72 119.1 . . ?
C74 C73 C72 120.0(3) . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C73 C74 N11 128.3(3) . . ?
C73 C74 C75 118.5(3) . . ?
N11 C74 C75 113.1(3) . . ?
N10 C75 C70 121.8(3) . . ?
N10 C75 C74 116.5(3) . . ?
C70 C75 C74 121.7(3) . . ?
N11 C76 C77 126.7(3) . . ?
N11 C76 H76 116.6 . . ?
C77 C76 H76 116.6 . . ?
C76 C77 C78 118.3(3) . . ?
C76 C77 C88 123.6(3) . . ?
C78 C77 C88 118.1(3) . . ?
C79 C78 C77 122.5(3) . . ?
C79 C78 H78 118.8 . . ?
C77 C78 H78 118.8 . . ?
C78 C79 C86 118.7(3) . . ?
C78 C79 C80 120.4(3) . . ?
C86 C79 C80 120.9(3) . . ?
C79 C80 C81 110.4(3) . . ?
C79 C80 H80A 109.6 . . ?
C81 C80 H80A 109.6 . . ?
C79 C80 H80B 109.6 . . ?
C81 C80 H80B 109.6 . . ?
H80A C80 H80B 108.1 . . ?
C82 C81 C80 110.6(3) . . ?
C82 C81 H81A 109.5 . . ?
C80 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 108.1 . . ?
N12 C82 C81 111.3(3) . . ?
N12 C82 H82A 109.4 . . ?
C81 C82 H82A 109.4 . . ?
N12 C82 H82B 109.4 . . ?
C81 C82 H82B 109.4 . . ?
H82A C82 H82B 108.0 . . ?
N12 C83 C84 110.8(3) . . ?
N12 C83 H83A 109.5 . . ?
C84 C83 H83A 109.5 . . ?
N12 C83 H83B 109.5 . . ?
C84 C83 H83B 109.5 . . ?
H83A C83 H83B 108.1 . . ?
C83 C84 C85 109.8(3) . . ?
C83 C84 H84A 109.7 . . ?
C85 C84 H84A 109.7 . . ?
C83 C84 H84B 109.7 . . ?
C85 C84 H84B 109.7 . . ?
H84A C84 H84B 108.2 . . ?
C87 C85 C84 110.8(3) . . ?
C87 C85 H85A 109.5 . . ?
C84 C85 H85A 109.5 . . ?
C87 C85 H85B 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 108.1 . . ?
N12 C86 C87 120.9(3) . . ?
N12 C86 C79 119.0(3) . . ?
C87 C86 C79 120.0(3) . . ?
C88 C87 C86 120.0(3) . . ?
C88 C87 C85 119.4(3) . . ?
C86 C87 C85 120.6(3) . . ?
O12 C88 C87 119.1(3) . . ?
O12 C88 C77 120.4(3) . . ?
C87 C88 C77 120.5(3) . . ?
O17 V6 O16 107.79(17) . . ?
O17 V6 O18 98.91(13) . . ?
O16 V6 O18 102.23(13) . . ?
O17 V6 N17 131.11(14) . . ?
O16 V6 N17 118.87(13) . . ?
O18 V6 N17 85.35(10) . . ?
O17 V6 N16 89.52(12) . . ?
O16 V6 N16 93.00(12) . . ?
O18 V6 N16 159.29(10) . . ?
N17 V6 N16 74.96(10) . . ?
C132 O18 V6 137.6(2) . . ?
C111 N16 C119 119.3(3) . . ?
C111 N16 V6 123.6(2) . . ?
C119 N16 V6 117.2(2) . . ?
C120 N17 C118 116.9(3) . . ?
C120 N17 V6 125.8(2) . . ?
C118 N17 V6 117.3(2) . . ?
C130 N18 C127 120.9(3) . . ?
C130 N18 C126 122.1(3) . . ?
C127 N18 C126 115.4(3) . . ?
N16 C111 C112 122.3(3) . . ?
N16 C111 H111 118.9 . . ?
C112 C111 H111 118.9 . . ?
C113 C112 C111 119.4(3) . . ?
C113 C112 H112 120.3 . . ?
C111 C112 H112 120.3 . . ?
C112 C113 C114 120.1(3) . . ?
C112 C113 H113 119.9 . . ?
C114 C113 H113 119.9 . . ?
C115 C114 C119 118.5(3) . . ?
C115 C114 C113 124.5(3) . . ?
C119 C114 C113 116.9(3) . . ?
C116 C115 C114 120.1(3) . . ?
C116 C115 H115 119.9 . . ?
C114 C115 H115 119.9 . . ?
C115 C116 C117 121.1(3) . . ?
C115 C116 H116 119.4 . . ?
C117 C116 H116 119.4 . . ?
C118 C117 C116 120.4(3) . . ?
C118 C117 H117 119.8 . . ?
C116 C117 H117 119.8 . . ?
C117 C118 C119 118.5(3) . . ?
C117 C118 N17 128.1(3) . . ?
C119 C118 N17 113.4(3) . . ?
N16 C119 C118 116.7(3) . . ?
N16 C119 C114 122.1(3) . . ?
C118 C119 C114 121.2(3) . . ?
N17 C120 C121 126.8(3) . . ?
N17 C120 H120 116.6 . . ?
C121 C120 H120 116.6 . . ?
C120 C121 C122 118.4(3) . . ?
C120 C121 C132 123.8(3) . . ?
C122 C121 C132 117.8(3) . . ?
C123 C122 C121 123.0(3) . . ?
C123 C122 H122 118.5 . . ?
C121 C122 H122 118.5 . . ?
C122 C123 C130 118.8(3) . . ?
C122 C123 C124 120.7(3) . . ?
C130 C123 C124 120.5(3) . . ?
C125 C124 C123 111.0(3) . . ?
C125 C124 H12A 109.4 . . ?
C123 C124 H12A 109.4 . . ?
C125 C124 H12B 109.4 . . ?
C123 C124 H12B 109.4 . . ?
H12A C124 H12B 108.0 . . ?
C124 C125 C126 109.8(3) . . ?
C124 C125 H12C 109.7 . . ?
C126 C125 H12C 109.7 . . ?
C124 C125 H12D 109.7 . . ?
C126 C125 H12D 109.7 . . ?
H12C C125 H12D 108.2 . . ?
N18 C126 C125 109.9(3) . . ?
N18 C126 H12E 109.7 . . ?
C125 C126 H12E 109.7 . . ?
N18 C126 H12F 109.7 . . ?
C125 C126 H12F 109.7 . . ?
H12E C126 H12F 108.2 . . ?
N18 C127 C128 110.2(3) . . ?
N18 C127 H12G 109.6 . . ?
C128 C127 H12G 109.6 . . ?
N18 C127 H12H 109.6 . . ?
C128 C127 H12H 109.6 . . ?
H12G C127 H12H 108.1 . . ?
C129 C128 C127 109.6(3) . . ?
C129 C128 H12I 109.8 . . ?
C127 C128 H12I 109.8 . . ?
C129 C128 H12J 109.8 . . ?
C127 C128 H12J 109.8 . . ?
H12I C128 H12J 108.2 . . ?
C131 C129 C128 111.1(3) . . ?
C131 C129 H12K 109.4 . . ?
C128 C129 H12K 109.4 . . ?
C131 C129 H12L 109.4 . . ?
C128 C129 H12L 109.4 . . ?
H12K C129 H12L 108.0 . . ?
N18 C130 C131 120.6(3) . . ?
N18 C130 C123 119.3(3) . . ?
C131 C130 C123 120.0(3) . . ?
C132 C131 C130 119.8(3) . . ?
C132 C131 C129 119.6(3) . . ?
C130 C131 C129 120.6(3) . . ?
O18 C132 C131 119.0(3) . . ?
O18 C132 C121 120.6(3) . . ?
C131 C132 C121 120.5(3) . . ?
O8 V3 O7 107.81(18) . . ?
O8 V3 O9 98.49(13) . . ?
O7 V3 O9 102.55(13) . . ?
O8 V3 N8 132.63(14) . . ?
O7 V3 N8 117.31(14) . . ?
O9 V3 N8 85.63(11) . . ?
O8 V3 N7 89.41(12) . . ?
O7 V3 N7 93.39(13) . . ?
O9 V3 N7 158.99(11) . . ?
N8 V3 N7 74.83(11) . . ?
C66 O9 V3 137.5(2) . . ?
C45 N7 C53 118.9(3) . . ?
C45 N7 V3 123.6(2) . . ?
C53 N7 V3 117.5(2) . . ?
C54 N8 C52 117.4(3) . . ?
C54 N8 V3 125.2(2) . . ?
C52 N8 V3 117.4(2) . . ?
C64 N9 C61 120.3(3) . . ?
C64 N9 C60 122.2(3) . . ?
C61 N9 C60 116.3(3) . . ?
N7 C45 C46 122.1(3) . . ?
N7 C45 H45 119.0 . . ?
C46 C45 H45 119.0 . . ?
C47 C46 C45 120.1(3) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C47 C48 119.6(3) . . ?
C46 C47 H47 120.2 . . ?
C48 C47 H47 120.2 . . ?
C53 C48 C49 118.4(3) . . ?
C53 C48 C47 117.0(3) . . ?
C49 C48 C47 124.6(3) . . ?
C50 C49 C48 119.9(3) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C49 C50 C51 121.2(3) . . ?
C49 C50 H50 119.4 . . ?
C51 C50 H50 119.4 . . ?
C52 C51 C50 120.6(3) . . ?
C52 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C51 C52 C53 118.4(3) . . ?
C51 C52 N8 128.0(3) . . ?
C53 C52 N8 113.6(3) . . ?
N7 C53 C48 122.3(3) . . ?
N7 C53 C52 116.2(3) . . ?
C48 C53 C52 121.5(3) . . ?
N8 C54 C55 127.5(3) . . ?
N8 C54 H54 116.3 . . ?
C55 C54 H54 116.3 . . ?
C54 C55 C56 117.9(3) . . ?
C54 C55 C66 123.5(3) . . ?
C56 C55 C66 118.6(3) . . ?
C57 C56 C55 123.1(3) . . ?
C57 C56 H56 118.4 . . ?
C55 C56 H56 118.4 . . ?
C56 C57 C64 118.3(3) . . ?
C56 C57 C58 120.8(3) . . ?
C64 C57 C58 120.9(3) . . ?
C59 C58 C57 111.0(3) . . ?
C59 C58 H58A 109.4 . . ?
C57 C58 H58A 109.4 . . ?
C59 C58 H58B 109.4 . . ?
C57 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C60 C59 C58 109.7(3) . . ?
C60 C59 H59A 109.7 . . ?
C58 C59 H59A 109.7 . . ?
C60 C59 H59B 109.7 . . ?
C58 C59 H59B 109.7 . . ?
H59A C59 H59B 108.2 . . ?
N9 C60 C59 111.3(3) . . ?
N9 C60 H60A 109.4 . . ?
C59 C60 H60A 109.4 . . ?
N9 C60 H60B 109.4 . . ?
C59 C60 H60B 109.4 . . ?
H60A C60 H60B 108.0 . . ?
N9 C61 C62 110.4(3) . . ?
N9 C61 H61A 109.6 . . ?
C62 C61 H61A 109.6 . . ?
N9 C61 H61B 109.6 . . ?
C62 C61 H61B 109.6 . . ?
H61A C61 H61B 108.1 . . ?
C61 C62 C63 109.5(3) . . ?
C61 C62 H62A 109.8 . . ?
C63 C62 H62A 109.8 . . ?
C61 C62 H62B 109.8 . . ?
C63 C62 H62B 109.8 . . ?
H62A C62 H62B 108.2 . . ?
C65 C63 C62 110.9(3) . . ?
C65 C63 H63A 109.5 . . ?
C62 C63 H63A 109.5 . . ?
C65 C63 H63B 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 108.0 . . ?
N9 C64 C65 121.0(3) . . ?
N9 C64 C57 118.7(3) . . ?
C65 C64 C57 120.4(3) . . ?
C66 C65 C64 119.7(3) . . ?
C66 C65 C63 120.0(3) . . ?
C64 C65 C63 120.3(3) . . ?
O9 C66 C65 119.5(3) . . ?
O9 C66 C55 120.5(3) . . ?
C65 C66 C55 120.0(3) . . ?
O4 V2 O5 109.42(14) . . ?
O4 V2 O6 102.19(13) . . ?
O5 V2 O6 99.22(13) . . ?
O4 V2 N4 91.83(13) . . ?
O5 V2 N4 89.95(12) . . ?
O6 V2 N4 159.49(11) . . ?
O4 V2 N5 120.70(12) . . ?
O5 V2 N5 127.71(13) . . ?
O6 V2 N5 84.71(11) . . ?
N4 V2 N5 75.23(11) . . ?
C44 O6 V2 137.5(2) . . ?
C23 N4 C31 118.7(3) . . ?
C23 N4 V2 122.8(2) . . ?
C31 N4 V2 118.2(2) . . ?
C32 N5 C30 118.2(3) . . ?
C32 N5 V2 125.5(2) . . ?
C30 N5 V2 116.2(2) . . ?
C42 N6 C39 120.3(3) . . ?
C42 N6 C38 122.0(3) . . ?
C39 N6 C38 116.0(3) . . ?
N4 C23 C24 122.4(3) . . ?
N4 C23 H23 118.8 . . ?
C24 C23 H23 118.8 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C27 125.3(3) . . ?
C25 C26 C31 116.7(3) . . ?
C27 C26 C31 118.0(3) . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 122.2(3) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C30 C29 C28 120.1(3) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 N5 127.5(3) . . ?
C29 C30 C31 118.3(3) . . ?
N5 C30 C31 114.2(3) . . ?
N4 C31 C26 122.6(3) . . ?
N4 C31 C30 115.9(3) . . ?
C26 C31 C30 121.5(3) . . ?
N5 C32 C33 126.6(3) . . ?
N5 C32 H32 116.7 . . ?
C33 C32 H32 116.7 . . ?
C32 C33 C34 119.2(3) . . ?
C32 C33 C44 122.6(3) . . ?
C34 C33 C44 118.1(3) . . ?
C35 C34 C33 122.6(3) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C34 C35 C42 118.7(3) . . ?
C34 C35 C36 121.0(3) . . ?
C42 C35 C36 120.3(3) . . ?
C37 C36 C35 110.7(3) . . ?
C37 C36 H36A 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C38 C37 C36 109.9(3) . . ?
C38 C37 H37A 109.7 . . ?
C36 C37 H37A 109.7 . . ?
C38 C37 H37B 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
N6 C38 C37 111.6(3) . . ?
N6 C38 H38A 109.3 . . ?
C37 C38 H38A 109.3 . . ?
N6 C38 H38B 109.3 . . ?
C37 C38 H38B 109.3 . . ?
H38A C38 H38B 108.0 . . ?
N6 C39 C40 109.9(3) . . ?
N6 C39 H39A 109.7 . . ?
C40 C39 H39A 109.7 . . ?
N6 C39 H39B 109.7 . . ?
C40 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
C41 C40 C39 111.1(4) . . ?
C41 C40 H40A 109.4 . . ?
C39 C40 H40A 109.4 . . ?
C41 C40 H40B 109.4 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
C40 C41 C43 111.2(3) . . ?
C40 C41 H41A 109.4 . . ?
C43 C41 H41A 109.4 . . ?
C40 C41 H41B 109.4 . . ?
C43 C41 H41B 109.4 . . ?
H41A C41 H41B 108.0 . . ?
N6 C42 C43 120.5(3) . . ?
N6 C42 C35 119.5(3) . . ?
C43 C42 C35 120.0(3) . . ?
C44 C43 C42 120.4(3) . . ?
C44 C43 C41 118.5(3) . . ?
C42 C43 C41 121.1(3) . . ?
O6 C44 C43 118.8(3) . . ?
O6 C44 C33 120.9(3) . . ?
C43 C44 C33 120.2(3) . . ?
O14 V5 O13 110.25(14) . . ?
O14 V5 O15 100.33(13) . . ?
O13 V5 O15 100.85(12) . . ?
O14 V5 N13 90.60(12) . . ?
O13 V5 N13 90.46(12) . . ?
O15 V5 N13 160.32(11) . . ?
O14 V5 N14 124.00(12) . . ?
O13 V5 N14 123.47(12) . . ?
O15 V5 N14 85.02(10) . . ?
N13 V5 N14 75.31(11) . . ?
C110 O15 V5 138.6(2) . . ?
C89 N13 C97 118.9(3) . . ?
C89 N13 V5 122.9(2) . . ?
C97 N13 V5 118.0(2) . . ?
C98 N14 C96 118.0(3) . . ?
C98 N14 V5 125.6(2) . . ?
C96 N14 V5 116.3(2) . . ?
C108 N15 C105 120.0(3) . . ?
C108 N15 C104 120.6(3) . . ?
C105 N15 C104 116.5(3) . . ?
N13 C89 C90 122.6(3) . . ?
N13 C89 H89 118.7 . . ?
C90 C89 H89 118.7 . . ?
C91 C90 C89 119.0(3) . . ?
C91 C90 H90 120.5 . . ?
C89 C90 H90 120.5 . . ?
C90 C91 C92 120.5(3) . . ?
C90 C91 H91 119.7 . . ?
C92 C91 H91 119.7 . . ?
C91 C92 C93 125.4(3) . . ?
C91 C92 C97 116.7(3) . . ?
C93 C92 C97 117.8(3) . . ?
C94 C93 C92 120.0(3) . . ?
C94 C93 H93 120.0 . . ?
C92 C93 H93 120.0 . . ?
C93 C94 C95 122.0(3) . . ?
C93 C94 H94 119.0 . . ?
C95 C94 H94 119.0 . . ?
C96 C95 C94 120.3(3) . . ?
C96 C95 H95 119.9 . . ?
C94 C95 H95 119.9 . . ?
C95 C96 N14 127.5(3) . . ?
C95 C96 C97 118.3(3) . . ?
N14 C96 C97 114.2(3) . . ?
N13 C97 C96 116.0(3) . . ?
N13 C97 C92 122.3(3) . . ?
C96 C97 C92 121.7(3) . . ?
N14 C98 C99 127.0(3) . . ?
N14 C98 H98 116.5 . . ?
C99 C98 H98 116.5 . . ?
C98 C99 C100 119.1(3) . . ?
C98 C99 C110 123.1(3) . . ?
C100 C99 C110 117.9(3) . . ?
C101 C100 C99 123.0(3) . . ?
C101 C100 H100 118.5 . . ?
C99 C100 H100 118.5 . . ?
C100 C101 C108 118.7(3) . . ?
C100 C101 C102 120.7(3) . . ?
C108 C101 C102 120.5(3) . . ?
C103 C102 C101 110.7(3) . . ?
C103 C102 H10A 109.5 . . ?
C101 C102 H10A 109.5 . . ?
C103 C102 H10B 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 108.1 . . ?
C104 C103 C102 110.6(4) . . ?
C104 C103 H10C 109.5 . . ?
C102 C103 H10C 109.5 . . ?
C104 C103 H10D 109.5 . . ?
C102 C103 H10D 109.5 . . ?
H10C C103 H10D 108.1 . . ?
N15 C104 C103 112.2(3) . . ?
N15 C104 H10E 109.2 . . ?
C103 C104 H10E 109.2 . . ?
N15 C104 H10F 109.2 . . ?
C103 C104 H10F 109.2 . . ?
H10E C104 H10F 107.9 . . ?
C106 C105 N15 114.0(4) . . ?
C106 C105 H10G 108.8 . . ?
N15 C105 H10G 108.8 . . ?
C106 C105 H10H 108.8 . . ?
N15 C105 H10H 108.8 . . ?
H10G C105 H10H 107.7 . . ?
C105 C106 C107 114.6(4) . . ?
C105 C106 H10I 108.6 . . ?
C107 C106 H10I 108.6 . . ?
C105 C106 H10J 108.6 . . ?
C107 C106 H10J 108.6 . . ?
H10I C106 H10J 107.6 . . ?
C106 C107 C109 111.2(3) . . ?
C106 C107 H10K 109.4 . . ?
C109 C107 H10K 109.4 . . ?
C106 C107 H10L 109.4 . . ?
C109 C107 H10L 109.4 . . ?
H10K C107 H10L 108.0 . . ?
N15 C108 C109 119.9(3) . . ?
N15 C108 C101 119.9(3) . . ?
C109 C108 C101 120.2(3) . . ?
C110 C109 C108 119.9(3) . . ?
C110 C109 C107 118.1(3) . . ?
C108 C109 C107 121.9(3) . . ?
O15 C110 C109 119.2(3) . . ?
O15 C110 C99 120.6(3) . . ?
C109 C110 C99 120.2(3) . . ?
H1WA O1W H1WB 109.5 . . ?
H3WA O3W H3WB 109.3 . . ?
H4WA O4W H4WB 109.5 . . ?
H2WA O2W H2WB 109.3 . . ?

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
C9 N1 C1 C2 1.1(5) . . . . ?
V1 N1 C1 C2 -176.5(3) . . . . ?
N1 C1 C2 C3 -0.6(5) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 179.1(3) . . . . ?
C2 C3 C4 C9 1.8(5) . . . . ?
C9 C4 C5 C6 -1.4(5) . . . . ?
C3 C4 C5 C6 -178.6(3) . . . . ?
C4 C5 C6 C7 -0.4(5) . . . . ?
C5 C6 C7 C8 2.5(5) . . . . ?
C6 C7 C8 N2 175.6(3) . . . . ?
C6 C7 C8 C9 -2.8(5) . . . . ?
C10 N2 C8 C7 -11.6(5) . . . . ?
V1 N2 C8 C7 -179.8(3) . . . . ?
C10 N2 C8 C9 167.0(3) . . . . ?
V1 N2 C8 C9 -1.3(3) . . . . ?
C1 N1 C9 C8 -179.9(3) . . . . ?
V1 N1 C9 C8 -2.2(4) . . . . ?
C1 N1 C9 C4 -0.1(5) . . . . ?
V1 N1 C9 C4 177.6(2) . . . . ?
C7 C8 C9 N1 -179.1(3) . . . . ?
N2 C8 C9 N1 2.2(4) . . . . ?
C7 C8 C9 C4 1.1(5) . . . . ?
N2 C8 C9 C4 -177.6(3) . . . . ?
C5 C4 C9 N1 -178.8(3) . . . . ?
C3 C4 C9 N1 -1.3(5) . . . . ?
C5 C4 C9 C8 1.0(5) . . . . ?
C3 C4 C9 C8 178.4(3) . . . . ?
C8 N2 C10 C11 -178.4(3) . . . . ?
V1 N2 C10 C11 -10.7(5) . . . . ?
N2 C10 C11 C12 174.9(3) . . . . ?
N2 C10 C11 C22 -5.2(5) . . . . ?
C10 C11 C12 C13 -177.6(3) . . . . ?
C22 C11 C12 C13 2.5(5) . . . . ?
C11 C12 C13 C21 -0.2(5) . . . . ?
C11 C12 C13 C14 178.9(4) . . . . ?
C12 C13 C14 C15 155.6(4) . . . . ?
C21 C13 C14 C15 -25.3(6) . . . . ?
C13 C14 C15 C16 47.4(6) . . . . ?
C21 N3 C16 C15 19.0(6) . . . . ?
C17 N3 C16 C15 -161.7(4) . . . . ?
C14 C15 C16 N3 -45.3(6) . . . . ?
C21 N3 C17 C18 23.6(6) . . . . ?
C16 N3 C17 C18 -155.7(4) . . . . ?
N3 C17 C18 C19 -51.6(5) . . . . ?
C17 C18 C19 C20 52.4(4) . . . . ?
C18 C19 C20 C22 151.9(3) . . . . ?
C18 C19 C20 C21 -27.2(5) . . . . ?
C17 N3 C21 C20 3.9(5) . . . . ?
C16 N3 C21 C20 -176.8(3) . . . . ?
C17 N3 C21 C13 -175.6(4) . . . . ?
C16 N3 C21 C13 3.7(5) . . . . ?
C22 C20 C21 N3 179.4(3) . . . . ?
C19 C20 C21 N3 -1.5(5) . . . . ?
C22 C20 C21 C13 -1.1(5) . . . . ?
C19 C20 C21 C13 178.0(3) . . . . ?
C12 C13 C21 N3 178.9(3) . . . . ?
C14 C13 C21 N3 -0.2(5) . . . . ?
C12 C13 C21 C20 -0.6(5) . . . . ?
C14 C13 C21 C20 -179.7(4) . . . . ?
V1 O3 C22 C20 -143.8(3) . . . . ?
V1 O3 C22 C11 38.5(5) . . . . ?
C21 C20 C22 O3 -174.2(3) . . . . ?
C19 C20 C22 O3 6.8(5) . . . . ?
C21 C20 C22 C11 3.5(5) . . . . ?
C19 C20 C22 C11 -175.6(3) . . . . ?
C10 C11 C22 O3 -6.5(5) . . . . ?
C12 C11 C22 O3 173.5(3) . . . . ?
C10 C11 C22 C20 175.9(3) . . . . ?
C12 C11 C22 C20 -4.1(5) . . . . ?
C75 N10 C67 C68 1.5(5) . . . . ?
V4 N10 C67 C68 -177.6(3) . . . . ?
N10 C67 C68 C69 -0.8(5) . . . . ?
C67 C68 C69 C70 -0.6(5) . . . . ?
C68 C69 C70 C75 1.2(5) . . . . ?
C68 C69 C70 C71 178.8(3) . . . . ?
C75 C70 C71 C72 -2.0(5) . . . . ?
C69 C70 C71 C72 -179.5(3) . . . . ?
C70 C71 C72 C73 0.2(5) . . . . ?
C71 C72 C73 C74 2.2(5) . . . . ?
C72 C73 C74 N11 176.1(3) . . . . ?
C72 C73 C74 C75 -2.6(5) . . . . ?
C76 N11 C74 C73 -11.0(5) . . . . ?
V4 N11 C74 C73 -179.9(3) . . . . ?
C76 N11 C74 C75 167.8(3) . . . . ?
V4 N11 C74 C75 -1.1(3) . . . . ?
C67 N10 C75 C70 -0.8(5) . . . . ?
V4 N10 C75 C70 178.3(2) . . . . ?
C67 N10 C75 C74 179.4(3) . . . . ?
V4 N10 C75 C74 -1.5(4) . . . . ?
C71 C70 C75 N10 -178.3(3) . . . . ?
C69 C70 C75 N10 -0.6(4) . . . . ?
C71 C70 C75 C74 1.6(4) . . . . ?
C69 C70 C75 C74 179.3(3) . . . . ?
C73 C74 C75 N10 -179.4(3) . . . . ?
N11 C74 C75 N10 1.7(4) . . . . ?
C73 C74 C75 C70 0.7(4) . . . . ?
N11 C74 C75 C70 -178.2(3) . . . . ?
C74 N11 C76 C77 179.4(3) . . . . ?
V4 N11 C76 C77 -12.1(4) . . . . ?
N11 C76 C77 C78 175.2(3) . . . . ?
N11 C76 C77 C88 -5.6(5) . . . . ?
C76 C77 C78 C79 -179.0(3) . . . . ?
C88 C77 C78 C79 1.8(5) . . . . ?
C77 C78 C79 C86 1.0(5) . . . . ?
C77 C78 C79 C80 -179.1(3) . . . . ?
C78 C79 C80 C81 -155.1(3) . . . . ?
C86 C79 C80 C81 24.8(5) . . . . ?
C79 C80 C81 C82 -51.0(4) . . . . ?
C86 N12 C82 C81 -34.5(5) . . . . ?
C83 N12 C82 C81 158.9(4) . . . . ?
C80 C81 C82 N12 56.2(5) . . . . ?
C86 N12 C83 C84 38.0(5) . . . . ?
C82 N12 C83 C84 -155.1(4) . . . . ?
N12 C83 C84 C85 -58.5(5) . . . . ?
C83 C84 C85 C87 49.4(4) . . . . ?
C82 N12 C86 C87 -173.7(3) . . . . ?
C83 N12 C86 C87 -7.7(5) . . . . ?
C82 N12 C86 C79 7.0(5) . . . . ?
C83 N12 C86 C79 173.0(3) . . . . ?
C78 C79 C86 N12 177.8(3) . . . . ?
C80 C79 C86 N12 -2.2(5) . . . . ?
C78 C79 C86 C87 -1.5(5) . . . . ?
C80 C79 C86 C87 178.5(3) . . . . ?
N12 C86 C87 C88 179.9(3) . . . . ?
C79 C86 C87 C88 -0.8(5) . . . . ?
N12 C86 C87 C85 -1.2(5) . . . . ?
C79 C86 C87 C85 178.1(3) . . . . ?
C84 C85 C87 C88 158.2(3) . . . . ?
C84 C85 C87 C86 -20.7(5) . . . . ?
V4 O12 C88 C87 -144.9(3) . . . . ?
V4 O12 C88 C77 35.5(4) . . . . ?
C86 C87 C88 O12 -175.9(3) . . . . ?
C85 C87 C88 O12 5.2(5) . . . . ?
C86 C87 C88 C77 3.7(5) . . . . ?
C85 C87 C88 C77 -175.2(3) . . . . ?
C76 C77 C88 O12 -3.7(5) . . . . ?
C78 C77 C88 O12 175.4(3) . . . . ?
C76 C77 C88 C87 176.7(3) . . . . ?
C78 C77 C88 C87 -4.2(5) . . . . ?
C119 N16 C111 C112 0.2(5) . . . . ?
V6 N16 C111 C112 -178.9(2) . . . . ?
N16 C111 C112 C113 -1.0(5) . . . . ?
C111 C112 C113 C114 0.4(5) . . . . ?
C112 C113 C114 C115 179.3(3) . . . . ?
C112 C113 C114 C119 0.9(5) . . . . ?
C119 C114 C115 C116 -1.2(5) . . . . ?
C113 C114 C115 C116 -179.6(3) . . . . ?
C114 C115 C116 C117 1.7(5) . . . . ?
C115 C116 C117 C118 0.6(5) . . . . ?
C116 C117 C118 C119 -3.3(5) . . . . ?
C116 C117 C118 N17 175.4(3) . . . . ?
C120 N17 C118 C117 -7.8(5) . . . . ?
V6 N17 C118 C117 173.8(3) . . . . ?
C120 N17 C118 C119 171.0(3) . . . . ?
V6 N17 C118 C119 -7.4(3) . . . . ?
C111 N16 C119 C118 -177.5(3) . . . . ?
V6 N16 C119 C118 1.6(3) . . . . ?
C111 N16 C119 C114 1.3(4) . . . . ?
V6 N16 C119 C114 -179.6(2) . . . . ?
C117 C118 C119 N16 -177.4(3) . . . . ?
N17 C118 C119 N16 3.7(4) . . . . ?
C117 C118 C119 C114 3.8(4) . . . . ?
N17 C118 C119 C114 -175.1(3) . . . . ?
C115 C114 C119 N16 179.7(3) . . . . ?
C113 C114 C119 N16 -1.8(4) . . . . ?
C115 C114 C119 C118 -1.6(4) . . . . ?
C113 C114 C119 C118 176.9(3) . . . . ?
C118 N17 C120 C121 179.6(3) . . . . ?
V6 N17 C120 C121 -2.2(5) . . . . ?
N17 C120 C121 C122 -178.2(3) . . . . ?
N17 C120 C121 C132 0.0(5) . . . . ?
C120 C121 C122 C123 176.4(3) . . . . ?
C132 C121 C122 C123 -1.9(5) . . . . ?
C121 C122 C123 C130 1.5(5) . . . . ?
C121 C122 C123 C124 -177.5(3) . . . . ?
C122 C123 C124 C125 -157.8(3) . . . . ?
C130 C123 C124 C125 23.2(4) . . . . ?
C123 C124 C125 C126 -51.5(4) . . . . ?
C130 N18 C126 C125 -37.2(4) . . . . ?
C127 N18 C126 C125 157.6(3) . . . . ?
C124 C125 C126 N18 58.5(4) . . . . ?
C130 N18 C127 C128 38.9(4) . . . . ?
C126 N18 C127 C128 -155.7(3) . . . . ?
N18 C127 C128 C129 -58.8(4) . . . . ?
C127 C128 C129 C131 49.3(4) . . . . ?
C127 N18 C130 C131 -8.2(4) . . . . ?
C126 N18 C130 C131 -172.7(3) . . . . ?
C127 N18 C130 C123 172.3(3) . . . . ?
C126 N18 C130 C123 7.8(4) . . . . ?
C122 C123 C130 N18 -179.2(3) . . . . ?
C124 C123 C130 N18 -0.2(4) . . . . ?
C122 C123 C130 C131 1.3(5) . . . . ?
C124 C123 C130 C131 -179.7(3) . . . . ?
N18 C130 C131 C132 176.8(3) . . . . ?
C123 C130 C131 C132 -3.7(4) . . . . ?
N18 C130 C131 C129 -1.8(4) . . . . ?
C123 C130 C131 C129 177.7(3) . . . . ?
C128 C129 C131 C132 161.3(3) . . . . ?
C128 C129 C131 C130 -20.1(4) . . . . ?
V6 O18 C132 C131 178.2(2) . . . . ?
V6 O18 C132 C121 -3.2(5) . . . . ?
C130 C131 C132 O18 -178.1(3) . . . . ?
C129 C131 C132 O18 0.5(4) . . . . ?
C130 C131 C132 C121 3.3(5) . . . . ?
C129 C131 C132 C121 -178.1(3) . . . . ?
C120 C121 C132 O18 2.6(5) . . . . ?
C122 C121 C132 O18 -179.2(3) . . . . ?
C120 C121 C132 C131 -178.8(3) . . . . ?
C122 C121 C132 C131 -0.6(4) . . . . ?
C53 N7 C45 C46 0.5(5) . . . . ?
V3 N7 C45 C46 -178.9(2) . . . . ?
N7 C45 C46 C47 -1.7(5) . . . . ?
C45 C46 C47 C48 0.9(5) . . . . ?
C46 C47 C48 C53 0.9(5) . . . . ?
C46 C47 C48 C49 179.4(3) . . . . ?
C53 C48 C49 C50 -1.2(5) . . . . ?
C47 C48 C49 C50 -179.6(3) . . . . ?
C48 C49 C50 C51 1.6(5) . . . . ?
C49 C50 C51 C52 0.0(5) . . . . ?
C50 C51 C52 C53 -2.1(5) . . . . ?
C50 C51 C52 N8 176.5(3) . . . . ?
C54 N8 C52 C51 -4.9(5) . . . . ?
V3 N8 C52 C51 174.7(3) . . . . ?
C54 N8 C52 C53 173.7(3) . . . . ?
V3 N8 C52 C53 -6.7(3) . . . . ?
C45 N7 C53 C48 1.5(5) . . . . ?
V3 N7 C53 C48 -179.1(2) . . . . ?
C45 N7 C53 C52 -178.4(3) . . . . ?
V3 N7 C53 C52 1.0(4) . . . . ?
C49 C48 C53 N7 179.3(3) . . . . ?
C47 C48 C53 N7 -2.2(4) . . . . ?
C49 C48 C53 C52 -0.9(5) . . . . ?
C47 C48 C53 C52 177.7(3) . . . . ?
C51 C52 C53 N7 -177.6(3) . . . . ?
N8 C52 C53 N7 3.6(4) . . . . ?
C51 C52 C53 C48 2.5(5) . . . . ?
N8 C52 C53 C48 -176.2(3) . . . . ?
C52 N8 C54 C55 -179.8(3) . . . . ?
V3 N8 C54 C55 0.6(5) . . . . ?
N8 C54 C55 C56 -178.6(3) . . . . ?
N8 C54 C55 C66 1.3(5) . . . . ?
C54 C55 C56 C57 179.1(3) . . . . ?
C66 C55 C56 C57 -0.8(5) . . . . ?
C55 C56 C57 C64 -0.3(5) . . . . ?
C55 C56 C57 C58 180.0(3) . . . . ?
C56 C57 C58 C59 -157.5(3) . . . . ?
C64 C57 C58 C59 22.7(4) . . . . ?
C57 C58 C59 C60 -51.1(4) . . . . ?
C64 N9 C60 C59 -34.3(5) . . . . ?
C61 N9 C60 C59 158.3(3) . . . . ?
C58 C59 C60 N9 57.3(4) . . . . ?
C64 N9 C61 C62 39.5(4) . . . . ?
C60 N9 C61 C62 -152.9(3) . . . . ?
N9 C61 C62 C63 -59.6(4) . . . . ?
C61 C62 C63 C65 49.8(4) . . . . ?
C61 N9 C64 C65 -8.8(5) . . . . ?
C60 N9 C64 C65 -175.7(3) . . . . ?
C61 N9 C64 C57 171.1(3) . . . . ?
C60 N9 C64 C57 4.2(5) . . . . ?
C56 C57 C64 N9 -178.0(3) . . . . ?
C58 C57 C64 N9 1.7(5) . . . . ?
C56 C57 C64 C65 1.8(5) . . . . ?
C58 C57 C64 C65 -178.4(3) . . . . ?
N9 C64 C65 C66 177.5(3) . . . . ?
C57 C64 C65 C66 -2.4(5) . . . . ?
N9 C64 C65 C63 -1.0(5) . . . . ?
C57 C64 C65 C63 179.1(3) . . . . ?
C62 C63 C65 C66 160.8(3) . . . . ?
C62 C63 C65 C64 -20.7(4) . . . . ?
V3 O9 C66 C65 175.2(2) . . . . ?
V3 O9 C66 C55 -4.8(5) . . . . ?
C64 C65 C66 O9 -178.8(3) . . . . ?
C63 C65 C66 O9 -0.2(5) . . . . ?
C64 C65 C66 C55 1.3(5) . . . . ?
C63 C65 C66 C55 179.8(3) . . . . ?
C54 C55 C66 O9 0.4(5) . . . . ?
C56 C55 C66 O9 -179.7(3) . . . . ?
C54 C55 C66 C65 -179.7(3) . . . . ?
C56 C55 C66 C65 0.3(5) . . . . ?
O4 V2 O6 C44 -103.0(4) . . . . ?
O5 V2 O6 C44 144.7(4) . . . . ?
N4 V2 O6 C44 29.1(6) . . . . ?
N5 V2 O6 C44 17.3(3) . . . . ?
C31 N4 C23 C24 0.3(5) . . . . ?
V2 N4 C23 C24 -174.8(3) . . . . ?
N4 C23 C24 C25 -0.6(5) . . . . ?
C23 C24 C25 C26 0.0(5) . . . . ?
C24 C25 C26 C27 177.5(3) . . . . ?
C24 C25 C26 C31 0.9(5) . . . . ?
C25 C26 C27 C28 -175.9(3) . . . . ?
C31 C26 C27 C28 0.7(5) . . . . ?
C26 C27 C28 C29 -0.4(5) . . . . ?
C27 C28 C29 C30 -0.7(5) . . . . ?
C28 C29 C30 N5 179.3(3) . . . . ?
C28 C29 C30 C31 1.4(5) . . . . ?
C32 N5 C30 C29 9.3(5) . . . . ?
V2 N5 C30 C29 -174.1(3) . . . . ?
C32 N5 C30 C31 -172.8(3) . . . . ?
V2 N5 C30 C31 3.8(3) . . . . ?
C23 N4 C31 C26 0.7(5) . . . . ?
V2 N4 C31 C26 176.0(2) . . . . ?
C23 N4 C31 C30 -177.7(3) . . . . ?
V2 N4 C31 C30 -2.4(4) . . . . ?
C25 C26 C31 N4 -1.2(5) . . . . ?
C27 C26 C31 N4 -178.1(3) . . . . ?
C25 C26 C31 C30 177.1(3) . . . . ?
C27 C26 C31 C30 0.2(5) . . . . ?
C29 C30 C31 N4 177.2(3) . . . . ?
N5 C30 C31 N4 -1.0(4) . . . . ?
C29 C30 C31 C26 -1.2(5) . . . . ?
N5 C30 C31 C26 -179.4(3) . . . . ?
C30 N5 C32 C33 -178.3(3) . . . . ?
V2 N5 C32 C33 5.5(5) . . . . ?
N5 C32 C33 C34 -179.5(3) . . . . ?
N5 C32 C33 C44 3.3(5) . . . . ?
C32 C33 C34 C35 -177.4(3) . . . . ?
C44 C33 C34 C35 -0.1(5) . . . . ?
C33 C34 C35 C42 0.9(5) . . . . ?
C33 C34 C35 C36 180.0(3) . . . . ?
C34 C35 C36 C37 -153.0(3) . . . . ?
C42 C35 C36 C37 26.1(4) . . . . ?
C35 C36 C37 C38 -52.2(4) . . . . ?
C42 N6 C38 C37 -32.9(5) . . . . ?
C39 N6 C38 C37 161.7(4) . . . . ?
C36 C37 C38 N6 56.1(4) . . . . ?
C42 N6 C39 C40 40.9(5) . . . . ?
C38 N6 C39 C40 -153.5(4) . . . . ?
N6 C39 C40 C41 -58.1(5) . . . . ?
C39 C40 C41 C43 47.0(5) . . . . ?
C39 N6 C42 C43 -12.0(5) . . . . ?
C38 N6 C42 C43 -176.7(3) . . . . ?
C39 N6 C42 C35 169.8(3) . . . . ?
C38 N6 C42 C35 5.1(5) . . . . ?
C34 C35 C42 N6 177.4(3) . . . . ?
C36 C35 C42 N6 -1.7(5) . . . . ?
C34 C35 C42 C43 -0.8(5) . . . . ?
C36 C35 C42 C43 -179.9(3) . . . . ?
N6 C42 C43 C44 -178.3(3) . . . . ?
C35 C42 C43 C44 -0.2(5) . . . . ?
N6 C42 C43 C41 0.2(5) . . . . ?
C35 C42 C43 C41 178.4(3) . . . . ?
C40 C41 C43 C44 160.0(3) . . . . ?
C40 C41 C43 C42 -18.6(5) . . . . ?
V2 O6 C44 C43 168.7(3) . . . . ?
V2 O6 C44 C33 -14.3(5) . . . . ?
C42 C43 C44 O6 178.0(3) . . . . ?
C41 C43 C44 O6 -0.6(5) . . . . ?
C42 C43 C44 C33 1.0(5) . . . . ?
C41 C43 C44 C33 -177.6(3) . . . . ?
C32 C33 C44 O6 -0.6(5) . . . . ?
C34 C33 C44 O6 -177.8(3) . . . . ?
C32 C33 C44 C43 176.4(3) . . . . ?
C34 C33 C44 C43 -0.8(5) . . . . ?
O14 V5 O15 C110 -120.2(4) . . . . ?
O13 V5 O15 C110 126.7(3) . . . . ?
N13 V5 O15 C110 2.6(6) . . . . ?
N14 V5 O15 C110 3.5(3) . . . . ?
C97 N13 C89 C90 1.6(5) . . . . ?
V5 N13 C89 C90 -172.6(2) . . . . ?
N13 C89 C90 C91 -1.0(5) . . . . ?
C89 C90 C91 C92 -1.2(5) . . . . ?
C90 C91 C92 C93 179.2(3) . . . . ?
C90 C91 C92 C97 2.7(5) . . . . ?
C91 C92 C93 C94 -176.9(3) . . . . ?
C97 C92 C93 C94 -0.5(5) . . . . ?
C92 C93 C94 C95 0.9(5) . . . . ?
C93 C94 C95 C96 -0.5(5) . . . . ?
C94 C95 C96 N14 177.5(3) . . . . ?
C94 C95 C96 C97 -0.3(5) . . . . ?
C98 N14 C96 C95 5.3(5) . . . . ?
V5 N14 C96 C95 -175.8(3) . . . . ?
C98 N14 C96 C97 -176.8(3) . . . . ?
V5 N14 C96 C97 2.1(3) . . . . ?
C89 N13 C97 C96 -178.6(3) . . . . ?
V5 N13 C97 C96 -4.2(4) . . . . ?
C89 N13 C97 C92 0.1(5) . . . . ?
V5 N13 C97 C92 174.5(2) . . . . ?
C95 C96 C97 N13 179.4(3) . . . . ?
N14 C96 C97 N13 1.3(4) . . . . ?
C95 C96 C97 C92 0.7(5) . . . . ?
N14 C96 C97 C92 -177.4(3) . . . . ?
C91 C92 C97 N13 -2.2(5) . . . . ?
C93 C92 C97 N13 -179.0(3) . . . . ?
C91 C92 C97 C96 176.5(3) . . . . ?
C93 C92 C97 C96 -0.3(5) . . . . ?
C96 N14 C98 C99 -178.0(3) . . . . ?
V5 N14 C98 C99 3.2(5) . . . . ?
N14 C98 C99 C100 -179.5(3) . . . . ?
N14 C98 C99 C110 0.4(5) . . . . ?
C98 C99 C100 C101 179.8(3) . . . . ?
C110 C99 C100 C101 0.0(5) . . . . ?
C99 C100 C101 C108 2.3(5) . . . . ?
C99 C100 C101 C102 -176.9(3) . . . . ?
C100 C101 C102 C103 -156.0(3) . . . . ?
C108 C101 C102 C103 24.9(5) . . . . ?
C101 C102 C103 C104 -50.4(5) . . . . ?
C108 N15 C104 C103 -35.6(6) . . . . ?
C105 N15 C104 C103 163.5(4) . . . . ?
C102 C103 C104 N15 56.7(5) . . . . ?
C108 N15 C105 C106 36.8(7) . . . . ?
C104 N15 C105 C106 -162.2(5) . . . . ?
N15 C105 C106 C107 -50.6(7) . . . . ?
C105 C106 C107 C109 39.3(6) . . . . ?
C105 N15 C108 C109 -11.8(6) . . . . ?
C104 N15 C108 C109 -172.0(4) . . . . ?
C105 N15 C108 C101 168.7(4) . . . . ?
C104 N15 C108 C101 8.5(5) . . . . ?
C100 C101 C108 N15 177.6(3) . . . . ?
C102 C101 C108 N15 -3.2(5) . . . . ?
C100 C101 C108 C109 -1.9(5) . . . . ?
C102 C101 C108 C109 177.3(3) . . . . ?
N15 C108 C109 C110 179.7(3) . . . . ?
C101 C108 C109 C110 -0.8(5) . . . . ?
N15 C108 C109 C107 1.5(5) . . . . ?
C101 C108 C109 C107 -179.0(3) . . . . ?
C106 C107 C109 C110 166.7(4) . . . . ?
C106 C107 C109 C108 -15.0(5) . . . . ?
V5 O15 C110 C109 179.5(3) . . . . ?
V5 O15 C110 C99 -1.4(5) . . . . ?
C108 C109 C110 O15 -177.9(3) . . . . ?
C107 C109 C110 O15 0.5(5) . . . . ?
C108 C109 C110 C99 3.0(5) . . . . ?
C107 C109 C110 C99 -178.6(3) . . . . ?
C98 C99 C110 O15 -1.6(5) . . . . ?
C100 C99 C110 O15 178.2(3) . . . . ?
C98 C99 C110 C109 177.5(3) . . . . ?
C100 C99 C110 C109 -2.7(5) . . . . ?

_refine_diff_density_max         2.995
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.100

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex2_sq
_database_code_depnum_ccdc_archive 'CCDC 1479865'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             2016-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C44 H40 N6 O3 Re 1+), Cl6 Re 2-, 7(C3 H7 N O)'
_chemical_formula_sum            'C109 H127 Cl6 N19 O13 Re3'
_chemical_formula_weight         2682.59
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.838(3)
_cell_length_b                   20.449(4)
_cell_length_c                   31.770(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10939(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.929
_cell_measurement_theta_min      1.282
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.528
_exptl_absorpt_correction_T_max  0.4308
_exptl_absorpt_correction_T_min  0.3479
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1056 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.8076.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             5380
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1491
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            183663
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.929
_diffrn_reflns_theta_min         1.282
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.974
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71074
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9073
_reflns_number_total             12773
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.00134(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         12773
_refine_ls_number_restraints     642
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0674P)²+23.4019P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1244
_refine_special_details          
;
SQUEEZE function of PLATON was used to remove the contribution of electron density
in the solvent-accessible void with the void volume of 164 Ang^3 and 37 electrons 
-very close to 40 e in a DMF molecule
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15A-C14B \\sim C15B-C14A
 with sigma of 0.02
 C16-C15B \\sim C16-C15A
 with sigma of 0.02
 C14B-C13 \\sim C14A-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) = Uanis(C14A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C14B(0.5) H14A(0.5) H14B(0.5) C15A(0.5) H15A(0.5) H15B(0.5)
 C15B(0.5) H15C(0.5) H15D(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5)
 C14A(0.5) H14C(0.5) H14D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C14B(H14A,H14B), C15A(H15A,H15B), C15B(H15C,H15D), C16(H16A,H16B), C16(H16C,
 H16D), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C14A(H14C,H14D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C3W(H3W),
  C9W(H9W), C6W(H6W)
6.c Idealised Me refined as rotating group:
 C4W(H4WA,H4WB,H4WC), C1W(H1WA,H1WB,H1WC), C2W(H2WA,H2WB,H2WC), C7W(H7WA,H7WB,
 H7WC), C8W(H8WA,H8WB,H8WC), C5W(H5WA,H5WB,H5WC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Re1 Re 0.30266(2) 0.40726(2) 0.54284(2) 0.02382(8) Uani 1 1 d . U . . .
O1 O 0.3695(2) 0.3547(2) 0.52205(14) 0.0283(9) Uani 1 1 d . U . . .
O2 O 0.2437(2) 0.3495(2) 0.58237(13) 0.0260(8) Uani 1 1 d . U . . .
O3 O 0.2271(2) 0.4779(2) 0.55421(13) 0.0273(9) Uani 1 1 d . U . . .
N1 N 0.3600(3) 0.4845(2) 0.50921(15) 0.0245(10) Uani 1 1 d . U . . .
N2 N 0.3680(3) 0.4468(2) 0.59006(16) 0.0248(10) Uani 1 1 d . U . . .
N3 N 0.2068(4) 0.2151(3) 0.70141(18) 0.0371(12) Uani 1 1 d . U . . .
N4 N 0.2821(3) 0.3648(3) 0.41618(17) 0.0323(11) Uani 1 1 d . U . . .
N5 N 0.2169(3) 0.3824(2) 0.49599(16) 0.0269(10) Uani 1 1 d . U . . .
N6 N 0.0854(4) 0.6756(3) 0.5308(2) 0.0418(14) Uani 1 1 d . U . . .
C1 C 0.3558(4) 0.4976(3) 0.46881(19) 0.0279(12) Uani 1 1 d . U . . .
H1 H 0.3241 0.4717 0.4516 0.033 Uiso 1 1 calc R . . . .
C2 C 0.3983(4) 0.5501(3) 0.4509(2) 0.0306(13) Uani 1 1 d . U . . .
H2 H 0.3949 0.5586 0.4221 0.037 Uiso 1 1 calc R . . . .
C4 C 0.4494(4) 0.5760(3) 0.5196(2) 0.0260(12) Uani 1 1 d . U . . .
C3 C 0.4444(4) 0.5883(3) 0.4760(2) 0.0294(12) Uani 1 1 d . U . . .
H3 H 0.4728 0.6229 0.4644 0.035 Uiso 1 1 calc R . . . .
C5 C 0.4947(4) 0.6127(3) 0.5486(2) 0.0299(12) Uani 1 1 d . U . . .
H5 H 0.5238 0.6485 0.5391 0.036 Uiso 1 1 calc R . . . .
C6 C 0.4965(4) 0.5969(3) 0.5902(2) 0.0330(13) Uani 1 1 d . U . . .
H6 H 0.5264 0.6222 0.6087 0.040 Uiso 1 1 calc R . . . .
C7 C 0.4537(4) 0.5425(3) 0.6058(2) 0.0272(12) Uani 1 1 d . U . . .
H7 H 0.4550 0.5329 0.6344 0.033 Uiso 1 1 calc R . . . .
C8 C 0.4106(3) 0.5042(3) 0.57919(19) 0.0246(11) Uani 1 1 d . U . . .
C9 C 0.4062(3) 0.5220(3) 0.53543(19) 0.0251(11) Uani 1 1 d . U . . .
C10 C 0.3741(4) 0.4202(3) 0.6280(2) 0.0292(13) Uani 1 1 d . U . . .
H10 H 0.4110 0.4386 0.6463 0.035 Uiso 1 1 calc R . . . .
C11 C 0.3304(4) 0.3673(3) 0.6430(2) 0.0308(13) Uani 1 1 d . U . . .
C12 C 0.3478(5) 0.3466(3) 0.6850(2) 0.0397(16) Uani 1 1 d . U . . .
H12 H 0.3884 0.3677 0.6994 0.048 Uiso 1 1 calc R . . . .
C13 C 0.3085(5) 0.2978(3) 0.7046(2) 0.0412(16) Uani 1 1 d D U . . .
C14B C 0.3161(11) 0.2806(7) 0.7514(4) 0.039(3) Uani 0.5 1 d D U . A 1
H14A H 0.3659 0.2969 0.7625 0.047 Uiso 0.5 1 calc R . . A 1
H14B H 0.2729 0.2999 0.7672 0.047 Uiso 0.5 1 calc R . . A 1
C15A C 0.3132(9) 0.2060(7) 0.7546(5) 0.047(3) Uani 0.5 1 d D U . A 1
H15A H 0.3534 0.1866 0.7366 0.056 Uiso 0.5 1 calc R . . A 1
H15B H 0.3229 0.1922 0.7833 0.056 Uiso 0.5 1 calc R . . A 1
C15B C 0.2753(9) 0.2358(7) 0.7678(4) 0.043(3) Uani 0.5 1 d D U . A 2
H15C H 0.2952 0.2148 0.7931 0.051 Uiso 0.5 1 calc R . . A 2
H15D H 0.2370 0.2686 0.7764 0.051 Uiso 0.5 1 calc R . . A 2
C16 C 0.2337(5) 0.1851(4) 0.7410(2) 0.0452(17) Uani 1 1 d D U . . .
H16A H 0.2336 0.1380 0.7376 0.054 Uiso 0.5 1 calc R . . A 1
H16B H 0.1959 0.1958 0.7630 0.054 Uiso 0.5 1 calc R . . A 1
H16C H 0.2697 0.1494 0.7349 0.054 Uiso 0.5 1 calc R . . A 2
H16D H 0.1884 0.1676 0.7561 0.054 Uiso 0.5 1 calc R . . A 2
C17 C 0.1403(5) 0.1830(4) 0.6809(2) 0.0442(17) Uani 1 1 d . U . . .
H17A H 0.1046 0.1658 0.7022 0.053 Uiso 1 1 calc R . . . .
H17B H 0.1598 0.1465 0.6644 0.053 Uiso 1 1 calc R . . . .
C18 C 0.0952(5) 0.2290(4) 0.6528(2) 0.0461(18) Uani 1 1 d . U . . .
H18A H 0.0723 0.2641 0.6693 0.055 Uiso 1 1 calc R . . . .
H18B H 0.0523 0.2058 0.6389 0.055 Uiso 1 1 calc R . . . .
C19 C 0.1519(4) 0.2570(3) 0.6202(2) 0.0331(14) Uani 1 1 d . U . . .
H19A H 0.1694 0.2226 0.6013 0.040 Uiso 1 1 calc R . . . .
H19B H 0.1248 0.2900 0.6035 0.040 Uiso 1 1 calc R . . . .
C20 C 0.2228(4) 0.2872(3) 0.6419(2) 0.0296(12) Uani 1 1 d . U . . .
C21 C 0.2449(4) 0.2658(3) 0.68289(19) 0.0302(12) Uani 1 1 d . U . . .
C22 C 0.2659(4) 0.3350(3) 0.62140(19) 0.0281(12) Uani 1 1 d . U . . .
C23 C 0.3150(4) 0.3558(4) 0.3791(2) 0.0411(16) Uani 1 1 d . U . . .
H23 H 0.3298 0.3926 0.3637 0.049 Uiso 1 1 calc R . . . .
C24 C 0.3292(5) 0.2942(4) 0.3613(3) 0.0490(18) Uani 1 1 d . U . . .
H24 H 0.3540 0.2906 0.3352 0.059 Uiso 1 1 calc R . . . .
C25 C 0.3064(5) 0.2399(4) 0.3825(2) 0.0465(17) Uani 1 1 d . U . . .
H25 H 0.3145 0.1988 0.3707 0.056 Uiso 1 1 calc R . . . .
C26 C 0.2703(4) 0.2456(3) 0.4226(2) 0.0359(14) Uani 1 1 d . U . . .
C27 C 0.2473(5) 0.1912(4) 0.4469(2) 0.0432(16) Uani 1 1 d . U . . .
H27 H 0.2548 0.1490 0.4367 0.052 Uiso 1 1 calc R . . . .
C28 C 0.2138(4) 0.2010(3) 0.4856(2) 0.0408(16) Uani 1 1 d . U . . .
H28 H 0.1988 0.1651 0.5017 0.049 Uiso 1 1 calc R . . . .
C29 C 0.2015(4) 0.2642(3) 0.5015(2) 0.0342(14) Uani 1 1 d . U . . .
H29 H 0.1776 0.2699 0.5276 0.041 Uiso 1 1 calc R . . . .
C30 C 0.2250(4) 0.3179(3) 0.4783(2) 0.0270(12) Uani 1 1 d . U . . .
C31 C 0.2602(4) 0.3100(3) 0.4378(2) 0.0300(13) Uani 1 1 d . U . . .
C32 C 0.1650(4) 0.4216(3) 0.47926(19) 0.0273(12) Uani 1 1 d . U . . .
H32 H 0.1367 0.4058 0.4563 0.033 Uiso 1 1 calc R . . . .
C33 C 0.1474(4) 0.4860(3) 0.49275(19) 0.0290(12) Uani 1 1 d . U . . .
C34 C 0.0925(4) 0.5240(3) 0.4698(2) 0.0352(14) Uani 1 1 d . U . . .
H34 H 0.0695 0.5058 0.4459 0.042 Uiso 1 1 calc R . . . .
C35 C 0.0711(4) 0.5866(3) 0.4808(2) 0.0361(14) Uani 1 1 d . U . . .
C36 C 0.0136(5) 0.6264(4) 0.4550(2) 0.0464(18) Uani 1 1 d . U . . .
H36A H 0.0240 0.6189 0.4253 0.056 Uiso 1 1 calc R . . . .
H36B H -0.0401 0.6117 0.4609 0.056 Uiso 1 1 calc R . . . .
C37 C 0.0194(7) 0.6962(5) 0.4637(4) 0.079(3) Uani 1 1 d . U . . .
H37A H 0.0625 0.7136 0.4469 0.094 Uiso 1 1 calc R . . . .
H37B H -0.0291 0.7167 0.4540 0.094 Uiso 1 1 calc R . . . .
C38 C 0.0320(7) 0.7159(4) 0.5062(3) 0.070(3) Uani 1 1 d . U . . .
H38A H -0.0191 0.7170 0.5203 0.084 Uiso 1 1 calc R . . . .
H38B H 0.0526 0.7602 0.5060 0.084 Uiso 1 1 calc R . . . .
C39 C 0.1196(5) 0.7056(3) 0.5683(3) 0.0477(18) Uani 1 1 d . U . . .
H39A H 0.0819 0.7365 0.5800 0.057 Uiso 1 1 calc R . . . .
H39B H 0.1671 0.7296 0.5605 0.057 Uiso 1 1 calc R . . . .
C40 C 0.1403(5) 0.6554(3) 0.6010(2) 0.0433(17) Uani 1 1 d . U . . .
H40A H 0.0923 0.6347 0.6113 0.052 Uiso 1 1 calc R . . . .
H40B H 0.1665 0.6765 0.6246 0.052 Uiso 1 1 calc R . . . .
C41 C 0.1947(4) 0.6046(3) 0.5822(2) 0.0378(15) Uani 1 1 d . U . . .
H41A H 0.2028 0.5695 0.6022 0.045 Uiso 1 1 calc R . . . .
H41B H 0.2459 0.6241 0.5761 0.045 Uiso 1 1 calc R . . . .
C42 C 0.1592(4) 0.5771(3) 0.5420(2) 0.0304(12) Uani 1 1 d . U . . .
C43 C 0.1062(4) 0.6140(3) 0.5182(2) 0.0338(14) Uani 1 1 d . U . . .
C44 C 0.1782(4) 0.5140(3) 0.5295(2) 0.0278(12) Uani 1 1 d . U . . .
Re2 Re 0.5000 0.51972(2) 0.7500 0.02883(10) Uani 1 2 d S TU P . .
Cl1 Cl 0.37432(10) 0.51930(8) 0.71736(5) 0.0351(3) Uani 1 1 d . U . . .
Cl2 Cl 0.54550(10) 0.60178(9) 0.70368(5) 0.0401(4) Uani 1 1 d . U . . .
Cl3 Cl 0.54290(13) 0.43859(11) 0.70289(9) 0.0731(8) Uani 1 1 d . U . . .
N2W N 0.2126(6) 0.5130(5) 0.3289(3) 0.084(3) Uani 1 1 d . U . . .
C4W C 0.2002(8) 0.4557(6) 0.3068(4) 0.095(4) Uani 1 1 d . U . . .
H4WA H 0.1610 0.4630 0.2854 0.142 Uiso 1 1 calc GR . . . .
H4WB H 0.1819 0.4223 0.3257 0.142 Uiso 1 1 calc GR . . . .
H4WC H 0.2491 0.4420 0.2940 0.142 Uiso 1 1 calc GR . . . .
O1W O 0.5736(5) 0.1318(4) 0.6143(3) 0.107(3) Uani 1 1 d . U . . .
N1W N 0.5553(4) 0.2356(4) 0.6380(3) 0.068(2) Uani 1 1 d . U . . .
C1W C 0.5631(7) 0.3028(5) 0.6276(4) 0.087(3) Uani 1 1 d . U . . .
H1WA H 0.5122 0.3237 0.6295 0.130 Uiso 1 1 calc GR . . . .
H1WB H 0.5831 0.3068 0.5994 0.130 Uiso 1 1 calc GR . . . .
H1WC H 0.5994 0.3233 0.6468 0.130 Uiso 1 1 calc GR . . . .
C2W C 0.5119(6) 0.2186(6) 0.6753(4) 0.089(3) Uani 1 1 d . U . . .
H2WA H 0.5204 0.2514 0.6964 0.133 Uiso 1 1 calc GR . . . .
H2WB H 0.5299 0.1771 0.6856 0.133 Uiso 1 1 calc GR . . . .
H2WC H 0.4563 0.2161 0.6688 0.133 Uiso 1 1 calc GR . . . .
C3W C 0.5807(6) 0.1902(6) 0.6113(4) 0.084(3) Uani 1 1 d . U . . .
H3W H 0.6070 0.2053 0.5874 0.101 Uiso 1 1 calc R . . . .
O3W O 0.0884(12) 0.5730(11) 0.7149(6) 0.251(9) Uani 1 1 d . U . . .
N3W N 0.1080(6) 0.5019(7) 0.6657(4) 0.109(3) Uani 1 1 d . U . . .
C7W C 0.1788(8) 0.4790(8) 0.6783(4) 0.114(5) Uani 1 1 d . U . . .
H7WA H 0.1713 0.4398 0.6944 0.170 Uiso 1 1 calc GR . . . .
H7WB H 0.2047 0.5113 0.6954 0.170 Uiso 1 1 calc GR . . . .
H7WC H 0.2110 0.4696 0.6542 0.170 Uiso 1 1 calc GR . . . .
C8W C 0.0666(9) 0.4763(10) 0.6325(4) 0.148(6) Uani 1 1 d . U . . .
H8WA H 0.0907 0.4902 0.6066 0.223 Uiso 1 1 calc GR . . . .
H8WB H 0.0127 0.4913 0.6336 0.223 Uiso 1 1 calc GR . . . .
H8WC H 0.0676 0.4294 0.6341 0.223 Uiso 1 1 calc GR . . . .
C9W C 0.0532(14) 0.5408(12) 0.6864(7) 0.173(8) Uani 1 1 d . U . . .
H9W H -0.0008 0.5431 0.6803 0.207 Uiso 1 1 calc R . . . .
C5W C 0.2436(10) 0.5678(7) 0.3048(5) 0.128(5) Uani 1 1 d . U . . .
H5WA H 0.2835 0.5524 0.2856 0.191 Uiso 1 1 calc GR . . . .
H5WB H 0.2666 0.5993 0.3236 0.191 Uiso 1 1 calc GR . . . .
H5WC H 0.2012 0.5878 0.2892 0.191 Uiso 1 1 calc GR . . . .
C6W C 0.1980(15) 0.5140(9) 0.3683(5) 0.187(9) Uani 1 1 d . U . . .
H6W H 0.1679 0.4838 0.3834 0.224 Uiso 1 1 calc R . . . .
O2W O 0.2351(17) 0.5682(8) 0.3842(6) 0.298(11) Uani 1 1 d . U . . .
C14A C 0.3447(9) 0.2698(8) 0.7454(4) 0.039(3) Uani 0.5 1 d D U . A 2
H14C H 0.3866 0.2388 0.7390 0.047 Uiso 0.5 1 calc R . . A 2
H14D H 0.3664 0.3045 0.7627 0.047 Uiso 0.5 1 calc R . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Re1 O1 1.691(4) . ?
Re1 O2 1.990(4) . ?
Re1 O3 1.958(4) . ?
Re1 N1 2.137(5) . ?
Re1 N2 2.029(5) . ?
Re1 N5 2.135(5) . ?
O2 C22 1.328(7) . ?
O3 C44 1.356(7) . ?
N1 C1 1.313(8) . ?
N1 C9 1.374(8) . ?
N2 C8 1.417(7) . ?
N2 C10 1.328(8) . ?
N3 C16 1.470(9) . ?
N3 C17 1.453(9) . ?
N3 C21 1.353(8) . ?
N4 C23 1.315(9) . ?
N4 C31 1.366(8) . ?
N5 C30 1.441(7) . ?
N5 C32 1.299(8) . ?
N6 C38 1.449(10) . ?
N6 C39 1.457(10) . ?
N6 C43 1.368(8) . ?
C1 H1 0.9300 . ?
C1 C2 1.411(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.360(9) . ?
C4 C3 1.410(9) . ?
C4 C5 1.411(9) . ?
C4 C9 1.414(8) . ?
C3 H3 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.362(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.414(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.362(8) . ?
C8 C9 1.439(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.392(8) . ?
C11 C12 1.429(9) . ?
C11 C22 1.444(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.351(9) . ?
C13 C14B 1.531(13) . ?
C13 C21 1.432(9) . ?
C13 C14A 1.541(13) . ?
C14B H14A 0.9700 . ?
C14B H14B 0.9700 . ?
C14B C15A 1.530(16) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C15A C16 1.470(15) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
C15B C16 1.514(14) . ?
C15B C14A 1.536(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.504(10) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.520(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.511(9) . ?
C20 C21 1.423(9) . ?
C20 C22 1.381(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.402(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.354(11) . ?
C25 H25 0.9300 . ?
C25 C26 1.417(10) . ?
C26 C27 1.407(10) . ?
C26 C31 1.414(9) . ?
C27 H27 0.9300 . ?
C27 C28 1.370(11) . ?
C28 H28 0.9300 . ?
C28 C29 1.402(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.380(9) . ?
C30 C31 1.425(9) . ?
C32 H32 0.9300 . ?
C32 C33 1.416(8) . ?
C33 C34 1.412(9) . ?
C33 C44 1.399(9) . ?
C34 H34 0.9300 . ?
C34 C35 1.374(9) . ?
C35 C36 1.506(9) . ?
C35 C43 1.441(10) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.457(12) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.422(13) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.503(10) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.509(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.517(9) . ?
C42 C43 1.393(9) . ?
C42 C44 1.387(8) . ?
Re2 Cl1 2.3566(16) . ?
Re2 Cl1 2.3566(16) 3_656 ?
Re2 Cl2 2.3597(17) 3_656 ?
Re2 Cl2 2.3598(17) . ?
Re2 Cl3 2.348(2) . ?
Re2 Cl3 2.348(2) 3_656 ?
N2W C4W 1.382(13) . ?
N2W C5W 1.456(15) . ?
N2W C6W 1.276(17) . ?
C4W H4WA 0.9600 . ?
C4W H4WB 0.9600 . ?
C4W H4WC 0.9600 . ?
O1W C3W 1.203(13) . ?
N1W C1W 1.421(12) . ?
N1W C2W 1.433(14) . ?
N1W C3W 1.329(13) . ?
C1W H1WA 0.9600 . ?
C1W H1WB 0.9600 . ?
C1W H1WC 0.9600 . ?
C2W H2WA 0.9600 . ?
C2W H2WB 0.9600 . ?
C2W H2WC 0.9600 . ?
C3W H3W 0.9300 . ?
O3W C9W 1.27(2) . ?
N3W C7W 1.343(16) . ?
N3W C8W 1.367(16) . ?
N3W C9W 1.38(2) . ?
C7W H7WA 0.9600 . ?
C7W H7WB 0.9600 . ?
C7W H7WC 0.9600 . ?
C8W H8WA 0.9600 . ?
C8W H8WB 0.9600 . ?
C8W H8WC 0.9600 . ?
C9W H9W 0.9300 . ?
C5W H5WA 0.9600 . ?
C5W H5WB 0.9600 . ?
C5W H5WC 0.9600 . ?
C6W H6W 0.9300 . ?
C6W O2W 1.37(2) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?

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
O1 Re1 O2 101.59(19) . . ?
O1 Re1 O3 166.77(19) . . ?
O1 Re1 N1 88.49(19) . . ?
O1 Re1 N2 100.4(2) . . ?
O1 Re1 N5 91.5(2) . . ?
O2 Re1 N1 168.47(18) . . ?
O2 Re1 N2 92.35(18) . . ?
O2 Re1 N5 87.78(18) . . ?
O3 Re1 O2 89.86(17) . . ?
O3 Re1 N1 80.85(18) . . ?
O3 Re1 N2 85.52(18) . . ?
O3 Re1 N5 82.22(18) . . ?
N2 Re1 N1 80.21(19) . . ?
N2 Re1 N5 167.75(19) . . ?
N5 Re1 N1 97.63(19) . . ?
C22 O2 Re1 125.5(4) . . ?
C44 O3 Re1 133.5(4) . . ?
C1 N1 Re1 128.0(4) . . ?
C1 N1 C9 120.6(5) . . ?
C9 N1 Re1 111.4(4) . . ?
C8 N2 Re1 115.1(4) . . ?
C10 N2 Re1 123.4(4) . . ?
C10 N2 C8 121.5(5) . . ?
C17 N3 C16 115.6(5) . . ?
C21 N3 C16 123.1(6) . . ?
C21 N3 C17 121.1(6) . . ?
C23 N4 C31 116.8(6) . . ?
C30 N5 Re1 115.2(4) . . ?
C32 N5 Re1 126.4(4) . . ?
C32 N5 C30 117.9(5) . . ?
C38 N6 C39 116.6(6) . . ?
C43 N6 C38 121.6(6) . . ?
C43 N6 C39 121.7(6) . . ?
N1 C1 H1 119.2 . . ?
N1 C1 C2 121.6(6) . . ?
C2 C1 H1 119.2 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(6) . . ?
C3 C2 H2 120.4 . . ?
C3 C4 C5 125.3(6) . . ?
C3 C4 C9 117.2(6) . . ?
C5 C4 C9 117.5(6) . . ?
C2 C3 C4 120.6(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.2(6) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 119.5 . . ?
C5 C6 C7 121.0(6) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.5(6) . . ?
C8 C7 H7 119.8 . . ?
N2 C8 C9 114.8(5) . . ?
C7 C8 N2 126.5(6) . . ?
C7 C8 C9 118.7(5) . . ?
N1 C9 C4 120.8(5) . . ?
N1 C9 C8 118.3(5) . . ?
C4 C9 C8 120.9(5) . . ?
N2 C10 H10 117.0 . . ?
N2 C10 C11 126.0(6) . . ?
C11 C10 H10 117.0 . . ?
C10 C11 C12 116.1(6) . . ?
C10 C11 C22 126.2(6) . . ?
C12 C11 C22 117.6(6) . . ?
C11 C12 H12 118.3 . . ?
C13 C12 C11 123.3(6) . . ?
C13 C12 H12 118.3 . . ?
C12 C13 C14B 125.2(9) . . ?
C12 C13 C21 118.8(6) . . ?
C12 C13 C14A 117.9(8) . . ?
C21 C13 C14B 115.2(8) . . ?
C21 C13 C14A 122.1(8) . . ?
C13 C14B H14A 110.3 . . ?
C13 C14B H14B 110.3 . . ?
H14A C14B H14B 108.6 . . ?
C15A C14B C13 106.9(11) . . ?
C15A C14B H14A 110.3 . . ?
C15A C14B H14B 110.3 . . ?
C14B C15A H15A 110.2 . . ?
C14B C15A H15B 110.2 . . ?
H15A C15A H15B 108.5 . . ?
C16 C15A C14B 107.4(12) . . ?
C16 C15A H15A 110.2 . . ?
C16 C15A H15B 110.2 . . ?
H15C C15B H15D 107.7 . . ?
C16 C15B H15C 108.8 . . ?
C16 C15B H15D 108.8 . . ?
C16 C15B C14A 113.6(12) . . ?
C14A C15B H15C 108.8 . . ?
C14A C15B H15D 108.8 . . ?
N3 C16 C15A 114.2(8) . . ?
N3 C16 C15B 109.8(8) . . ?
N3 C16 H16A 108.7 . . ?
N3 C16 H16B 108.7 . . ?
N3 C16 H16C 109.7 . . ?
N3 C16 H16D 109.7 . . ?
C15A C16 H16A 108.7 . . ?
C15A C16 H16B 108.7 . . ?
C15B C16 H16C 109.7 . . ?
C15B C16 H16D 109.7 . . ?
H16A C16 H16B 107.6 . . ?
H16C C16 H16D 108.2 . . ?
N3 C17 H17A 109.2 . . ?
N3 C17 H17B 109.2 . . ?
N3 C17 C18 111.9(6) . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C17 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
C17 C18 C19 108.9(6) . . ?
H18A C18 H18B 108.3 . . ?
C19 C18 H18A 109.9 . . ?
C19 C18 H18B 109.9 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 C18 109.8(6) . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C21 C20 C19 119.9(5) . . ?
C22 C20 C19 119.2(6) . . ?
C22 C20 C21 120.8(6) . . ?
N3 C21 C13 119.6(6) . . ?
N3 C21 C20 120.6(6) . . ?
C20 C21 C13 119.7(6) . . ?
O2 C22 C11 123.6(5) . . ?
O2 C22 C20 116.7(6) . . ?
C20 C22 C11 119.6(6) . . ?
N4 C23 H23 118.0 . . ?
N4 C23 C24 124.0(7) . . ?
C24 C23 H23 118.0 . . ?
C23 C24 H24 120.4 . . ?
C25 C24 C23 119.2(7) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.2(7) . . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 123.1(7) . . ?
C27 C26 C31 121.0(6) . . ?
C31 C26 C25 115.8(7) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.4(7) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 119.4 . . ?
C27 C28 C29 121.3(7) . . ?
C29 C28 H28 119.4 . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.9(6) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 N5 119.6(6) . . ?
C29 C30 C31 120.7(6) . . ?
C31 C30 N5 119.7(5) . . ?
N4 C31 C26 124.0(6) . . ?
N4 C31 C30 118.3(6) . . ?
C26 C31 C30 117.7(6) . . ?
N5 C32 H32 116.9 . . ?
N5 C32 C33 126.2(6) . . ?
C33 C32 H32 116.9 . . ?
C34 C33 C32 119.6(6) . . ?
C44 C33 C32 123.7(6) . . ?
C44 C33 C34 116.6(6) . . ?
C33 C34 H34 118.2 . . ?
C35 C34 C33 123.6(6) . . ?
C35 C34 H34 118.2 . . ?
C34 C35 C36 122.2(7) . . ?
C34 C35 C43 117.7(6) . . ?
C43 C35 C36 120.1(6) . . ?
C35 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C37 C36 C35 112.4(7) . . ?
C37 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
C36 C37 H37A 107.8 . . ?
C36 C37 H37B 107.8 . . ?
H37A C37 H37B 107.1 . . ?
C38 C37 C36 118.0(9) . . ?
C38 C37 H37A 107.8 . . ?
C38 C37 H37B 107.8 . . ?
N6 C38 H38A 108.2 . . ?
N6 C38 H38B 108.2 . . ?
C37 C38 N6 116.3(8) . . ?
C37 C38 H38A 108.2 . . ?
C37 C38 H38B 108.2 . . ?
H38A C38 H38B 107.4 . . ?
N6 C39 H39A 109.3 . . ?
N6 C39 H39B 109.3 . . ?
N6 C39 C40 111.7(6) . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.3 . . ?
C40 C39 H39B 109.3 . . ?
C39 C40 H40A 109.7 . . ?
C39 C40 H40B 109.7 . . ?
C39 C40 C41 109.7(6) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 C42 110.6(6) . . ?
H41A C41 H41B 108.1 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
C43 C42 C41 120.5(6) . . ?
C44 C42 C41 119.7(6) . . ?
C44 C42 C43 119.8(6) . . ?
N6 C43 C35 119.7(6) . . ?
N6 C43 C42 120.3(6) . . ?
C42 C43 C35 120.0(6) . . ?
O3 C44 C33 119.1(6) . . ?
O3 C44 C42 118.7(6) . . ?
C42 C44 C33 122.2(6) . . ?
Cl1 Re2 Cl1 179.58(8) 3_656 . ?
Cl1 Re2 Cl2 89.16(6) . 3_656 ?
Cl1 Re2 Cl2 91.13(6) . . ?
Cl1 Re2 Cl2 89.17(6) 3_656 . ?
Cl1 Re2 Cl2 91.13(6) 3_656 3_656 ?
Cl2 Re2 Cl2 89.35(10) 3_656 . ?
Cl3 Re2 Cl1 89.61(7) . . ?
Cl3 Re2 Cl1 90.09(6) . 3_656 ?
Cl3 Re2 Cl1 90.09(6) 3_656 . ?
Cl3 Re2 Cl1 89.61(7) 3_656 3_656 ?
Cl3 Re2 Cl2 90.29(9) . . ?
Cl3 Re2 Cl2 90.29(9) 3_656 3_656 ?
Cl3 Re2 Cl2 178.72(7) 3_656 . ?
Cl3 Re2 Cl2 178.72(7) . 3_656 ?
Cl3 Re2 Cl3 90.10(16) . 3_656 ?
C4W N2W C5W 116.0(11) . . ?
C6W N2W C4W 118.9(12) . . ?
C6W N2W C5W 125.0(13) . . ?
N2W C4W H4WA 109.5 . . ?
N2W C4W H4WB 109.5 . . ?
N2W C4W H4WC 109.5 . . ?
H4WA C4W H4WB 109.5 . . ?
H4WA C4W H4WC 109.5 . . ?
H4WB C4W H4WC 109.5 . . ?
C1W N1W C2W 118.3(9) . . ?
C3W N1W C1W 119.8(11) . . ?
C3W N1W C2W 121.5(10) . . ?
N1W C1W H1WA 109.5 . . ?
N1W C1W H1WB 109.5 . . ?
N1W C1W H1WC 109.5 . . ?
H1WA C1W H1WB 109.5 . . ?
H1WA C1W H1WC 109.5 . . ?
H1WB C1W H1WC 109.5 . . ?
N1W C2W H2WA 109.5 . . ?
N1W C2W H2WB 109.5 . . ?
N1W C2W H2WC 109.5 . . ?
H2WA C2W H2WB 109.5 . . ?
H2WA C2W H2WC 109.5 . . ?
H2WB C2W H2WC 109.5 . . ?
O1W C3W N1W 127.6(13) . . ?
O1W C3W H3W 116.2 . . ?
N1W C3W H3W 116.2 . . ?
C7W N3W C8W 123.3(16) . . ?
C7W N3W C9W 130.6(15) . . ?
C8W N3W C9W 104.3(15) . . ?
N3W C7W H7WA 109.5 . . ?
N3W C7W H7WB 109.5 . . ?
N3W C7W H7WC 109.5 . . ?
H7WA C7W H7WB 109.5 . . ?
H7WA C7W H7WC 109.5 . . ?
H7WB C7W H7WC 109.5 . . ?
N3W C8W H8WA 109.5 . . ?
N3W C8W H8WB 109.5 . . ?
N3W C8W H8WC 109.5 . . ?
H8WA C8W H8WB 109.5 . . ?
H8WA C8W H8WC 109.5 . . ?
H8WB C8W H8WC 109.5 . . ?
O3W C9W N3W 109(2) . . ?
O3W C9W H9W 125.5 . . ?
N3W C9W H9W 125.5 . . ?
N2W C5W H5WA 109.5 . . ?
N2W C5W H5WB 109.5 . . ?
N2W C5W H5WC 109.5 . . ?
H5WA C5W H5WB 109.5 . . ?
H5WA C5W H5WC 109.5 . . ?
H5WB C5W H5WC 109.5 . . ?
N2W C6W H6W 126.7 . . ?
N2W C6W O2W 106.6(17) . . ?
O2W C6W H6W 126.7 . . ?
C13 C14A H14C 110.8 . . ?
C13 C14A H14D 110.8 . . ?
C15B C14A C13 105.0(10) . . ?
C15B C14A H14C 110.8 . . ?
C15B C14A H14D 110.8 . . ?
H14C C14A H14D 108.8 . . ?

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
Re1 O2 C22 C11 9.7(8) . . . . ?
Re1 O2 C22 C20 -171.5(4) . . . . ?
Re1 O3 C44 C33 30.0(8) . . . . ?
Re1 O3 C44 C42 -151.3(5) . . . . ?
Re1 N1 C1 C2 -179.1(4) . . . . ?
Re1 N1 C9 C4 -179.9(4) . . . . ?
Re1 N1 C9 C8 1.3(6) . . . . ?
Re1 N2 C8 C7 174.8(5) . . . . ?
Re1 N2 C8 C9 -5.2(6) . . . . ?
Re1 N2 C10 C11 -8.5(9) . . . . ?
Re1 N5 C30 C29 75.3(6) . . . . ?
Re1 N5 C30 C31 -102.0(6) . . . . ?
Re1 N5 C32 C33 -9.4(9) . . . . ?
N1 C1 C2 C3 -0.4(10) . . . . ?
N2 C8 C9 N1 2.5(8) . . . . ?
N2 C8 C9 C4 -176.3(5) . . . . ?
N2 C10 C11 C12 179.3(6) . . . . ?
N2 C10 C11 C22 -5.5(11) . . . . ?
N3 C17 C18 C19 57.6(8) . . . . ?
N4 C23 C24 C25 1.7(12) . . . . ?
N5 C30 C31 N4 -2.9(9) . . . . ?
N5 C30 C31 C26 177.1(6) . . . . ?
N5 C32 C33 C34 176.3(6) . . . . ?
N5 C32 C33 C44 -7.3(10) . . . . ?
N6 C39 C40 C41 55.2(9) . . . . ?
C1 N1 C9 C4 0.7(9) . . . . ?
C1 N1 C9 C8 -178.1(5) . . . . ?
C1 C2 C3 C4 -0.3(10) . . . . ?
C4 C5 C6 C7 0.6(10) . . . . ?
C3 C4 C5 C6 -179.5(6) . . . . ?
C3 C4 C9 N1 -1.4(8) . . . . ?
C3 C4 C9 C8 177.4(5) . . . . ?
C5 C4 C3 C2 -179.4(6) . . . . ?
C5 C4 C9 N1 179.2(5) . . . . ?
C5 C4 C9 C8 -2.1(9) . . . . ?
C5 C6 C7 C8 1.0(10) . . . . ?
C6 C7 C8 N2 176.9(6) . . . . ?
C6 C7 C8 C9 -3.1(9) . . . . ?
C7 C8 C9 N1 -177.5(5) . . . . ?
C7 C8 C9 C4 3.7(9) . . . . ?
C8 N2 C10 C11 174.5(6) . . . . ?
C9 N1 C1 C2 0.2(9) . . . . ?
C9 C4 C3 C2 1.2(9) . . . . ?
C9 C4 C5 C6 -0.1(9) . . . . ?
C10 N2 C8 C7 -8.0(9) . . . . ?
C10 N2 C8 C9 172.0(5) . . . . ?
C10 C11 C12 C13 177.2(7) . . . . ?
C10 C11 C22 O2 5.0(11) . . . . ?
C10 C11 C22 C20 -173.6(6) . . . . ?
C11 C12 C13 C14B -170.3(10) . . . . ?
C11 C12 C13 C21 -1.2(12) . . . . ?
C11 C12 C13 C14A 166.4(10) . . . . ?
C12 C11 C22 O2 -179.8(6) . . . . ?
C12 C11 C22 C20 1.5(9) . . . . ?
C12 C13 C14B C15A -141.9(11) . . . . ?
C12 C13 C21 N3 177.4(7) . . . . ?
C12 C13 C21 C20 -2.1(11) . . . . ?
C12 C13 C14A C15B 160.0(10) . . . . ?
C13 C14B C15A C16 -65.3(15) . . . . ?
C14B C13 C21 N3 -12.5(11) . . . . ?
C14B C13 C21 C20 168.1(9) . . . . ?
C14B C15A C16 N3 47.7(14) . . . . ?
C16 N3 C17 C18 155.9(7) . . . . ?
C16 N3 C21 C13 -8.0(10) . . . . ?
C16 N3 C21 C20 171.5(7) . . . . ?
C16 C15B C14A C13 55.1(16) . . . . ?
C17 N3 C16 C15A 163.3(9) . . . . ?
C17 N3 C16 C15B -155.6(9) . . . . ?
C17 N3 C21 C13 177.8(7) . . . . ?
C17 N3 C21 C20 -2.8(10) . . . . ?
C17 C18 C19 C20 -53.9(8) . . . . ?
C18 C19 C20 C21 24.1(9) . . . . ?
C18 C19 C20 C22 -156.4(6) . . . . ?
C19 C20 C21 N3 5.2(10) . . . . ?
C19 C20 C21 C13 -175.4(6) . . . . ?
C19 C20 C22 O2 -3.0(9) . . . . ?
C19 C20 C22 C11 175.8(6) . . . . ?
C21 N3 C16 C15A -11.2(12) . . . . ?
C21 N3 C16 C15B 29.9(11) . . . . ?
C21 N3 C17 C18 -29.5(10) . . . . ?
C21 C13 C14B C15A 48.7(14) . . . . ?
C21 C13 C14A C15B -32.8(16) . . . . ?
C21 C20 C22 O2 176.4(6) . . . . ?
C21 C20 C22 C11 -4.8(9) . . . . ?
C22 C11 C12 C13 1.6(11) . . . . ?
C22 C20 C21 N3 -174.3(6) . . . . ?
C22 C20 C21 C13 5.2(10) . . . . ?
C23 N4 C31 C26 -0.5(9) . . . . ?
C23 N4 C31 C30 179.5(6) . . . . ?
C23 C24 C25 C26 -1.4(12) . . . . ?
C24 C25 C26 C27 -178.1(7) . . . . ?
C24 C25 C26 C31 0.3(11) . . . . ?
C25 C26 C27 C28 179.0(7) . . . . ?
C25 C26 C31 N4 0.7(10) . . . . ?
C25 C26 C31 C30 -179.2(6) . . . . ?
C26 C27 C28 C29 0.4(11) . . . . ?
C27 C26 C31 N4 179.1(6) . . . . ?
C27 C26 C31 C30 -0.8(10) . . . . ?
C27 C28 C29 C30 -1.4(11) . . . . ?
C28 C29 C30 N5 -176.0(6) . . . . ?
C28 C29 C30 C31 1.3(10) . . . . ?
C29 C30 C31 N4 179.8(6) . . . . ?
C29 C30 C31 C26 -0.2(9) . . . . ?
C30 N5 C32 C33 178.5(6) . . . . ?
C31 N4 C23 C24 -0.8(10) . . . . ?
C31 C26 C27 C28 0.8(11) . . . . ?
C32 N5 C30 C29 -111.8(7) . . . . ?
C32 N5 C30 C31 70.9(8) . . . . ?
C32 C33 C34 C35 179.2(6) . . . . ?
C32 C33 C44 O3 -0.8(9) . . . . ?
C32 C33 C44 C42 -179.5(6) . . . . ?
C33 C34 C35 C36 178.6(7) . . . . ?
C33 C34 C35 C43 -0.8(11) . . . . ?
C34 C33 C44 O3 175.7(6) . . . . ?
C34 C33 C44 C42 -2.9(9) . . . . ?
C34 C35 C36 C37 -160.9(9) . . . . ?
C34 C35 C43 N6 -178.6(7) . . . . ?
C34 C35 C43 C42 -0.6(10) . . . . ?
C35 C36 C37 C38 -38.7(14) . . . . ?
C36 C35 C43 N6 1.9(10) . . . . ?
C36 C35 C43 C42 179.9(7) . . . . ?
C36 C37 C38 N6 38.5(16) . . . . ?
C38 N6 C39 C40 153.1(8) . . . . ?
C38 N6 C43 C35 -3.6(11) . . . . ?
C38 N6 C43 C42 178.4(8) . . . . ?
C39 N6 C38 C37 160.0(9) . . . . ?
C39 N6 C43 C35 -179.7(7) . . . . ?
C39 N6 C43 C42 2.3(11) . . . . ?
C39 C40 C41 C42 -52.3(8) . . . . ?
C40 C41 C42 C43 26.0(9) . . . . ?
C40 C41 C42 C44 -152.3(6) . . . . ?
C41 C42 C43 N6 -0.1(10) . . . . ?
C41 C42 C43 C35 -178.1(6) . . . . ?
C41 C42 C44 O3 1.4(9) . . . . ?
C41 C42 C44 C33 180.0(6) . . . . ?
C43 N6 C38 C37 -16.2(14) . . . . ?
C43 N6 C39 C40 -30.7(11) . . . . ?
C43 C35 C36 C37 18.5(11) . . . . ?
C43 C42 C44 O3 -177.0(6) . . . . ?
C43 C42 C44 C33 1.6(10) . . . . ?
C44 C33 C34 C35 2.6(10) . . . . ?
C44 C42 C43 N6 178.2(6) . . . . ?
C44 C42 C43 C35 0.2(10) . . . . ?
C4W N2W C6W O2W 163.5(17) . . . . ?
C1W N1W C3W O1W -174.7(12) . . . . ?
C2W N1W C3W O1W -1.9(19) . . . . ?
C7W N3W C9W O3W 23(3) . . . . ?
C8W N3W C9W O3W -172.3(19) . . . . ?
C5W N2W C6W O2W -15(3) . . . . ?
C14A C13 C21 N3 10.3(13) . . . . ?
C14A C13 C21 C20 -169.2(10) . . . . ?
C14A C15B C16 N3 -55.4(14) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 1479866'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             2016-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C22 H24 N3 O5 U 1+), C22 H20 N3 O, 2(N O3 1-), 4(H2 O)'
_chemical_formula_sum            'C66 H76 N11 O21 U2'
_chemical_formula_weight         1835.43
_chemical_melting_point          ?
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.416(3)
_cell_length_b                   15.959(3)
_cell_length_c                   16.435(3)
_cell_angle_alpha                105.45(3)
_cell_angle_beta                 113.33(3)
_cell_angle_gamma                90.57(3)
_cell_volume                     3548.2(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.925
_cell_measurement_theta_min      1.335
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.639
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1802
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60448
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_min         1.335
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.916
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71074
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11059
_reflns_number_total             15564
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0060(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15564
_refine_ls_number_restraints     947
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0510
_refine_ls_restrained_S_all      1.020
_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)+(0.0596P)²+11.1362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1280
_refine_special_details          
;
1. Both disordered nitrate anions (N2N and N3N) share the positions with 
   disordered water molecules
2. A solvent-accessible void of 145 Å^3 with diffuse electron density of 
   up to 1.5 e/ Å^3 in it
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 N2N-O1N2
 1.26 with sigma of 0.02
 N2N-O2N2
 1.26 with sigma of 0.02
 N2N-O3N2
 1.26 with sigma of 0.02
 O1N3-N3N = O2N3-N3N = O3N3-N3N
 1.27 with sigma of 0.02
 C62A-C61A \\sim C62B-C61B \\sim C63-C62A \\sim C63-C62B
 with sigma of 0.02
3. Restrained planarity
 O1N2, O2N2, O3N2, N2N
 with sigma of 0.1
 O3N3, N3N, O1N3, O2N3
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C61A(0.5) H61A(0.5) H61B(0.5) C61B(0.5) H61C(0.5) H61D(0.5)
 C62A(0.5) H62A(0.5) H62B(0.5) C62B(0.5) H62C(0.5) H62D(0.5) H63A(0.5)
 H63B(0.5) O1N2(0.5) O2N2(0.5) O3N2(0.5) N2N(0.5) O7W(0.5) O9W(0.5) O8W(0.5)
 O10W(0.3) O3N3(0.5) N3N(0.5) O1N3(0.5) O12W(0.2) O2N3(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O6W(H6WA,H6WB)
6.b Free rotating group:
 O5W(H5WA,H5WB)
6.c Rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB)
6.d Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C58(H58A,H58B), C59(H59A,H59B),
  C60(H60A,H60B), C61A(H61A,H61B), C61B(H61C,H61D), C62A(H62A,H62B), C62B(H62C,
 H62D), C63(H63A,H63B)
6.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C54(H54), C56(H56)
6.f Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
U1 U 0.46683(2) 0.78143(2) 0.18001(2) 0.03267(9) Uani 1 1 d . U . . .
O1 O 0.3514(4) 0.8065(3) 0.1701(4) 0.0412(12) Uani 1 1 d . U . . .
O1W O 0.4864(5) 0.7351(4) 0.3134(5) 0.0616(16) Uani 1 1 d . U . . .
H1WA H 0.4698 0.7483 0.3628 0.092 Uiso 1 1 d R . . . .
H1WB H 0.5340 0.7004 0.3271 0.092 Uiso 1 1 d R . . . .
O2 O 0.5819(3) 0.7534(3) 0.1937(4) 0.0389(12) Uani 1 1 d . U . . .
O2W O 0.5401(5) 0.9098(4) 0.3149(4) 0.0580(16) Uani 1 1 d . U . . .
H2WA H 0.5114 0.9536 0.3390 0.087 Uiso 1 1 d R . . . .
H2WB H 0.6024 0.9095 0.3531 0.087 Uiso 1 1 d R . . . .
O3 O 0.4805(3) 0.8844(3) 0.1172(4) 0.0346(10) Uani 1 1 d . U . . .
N0AA N 0.4062(4) 0.6131(4) 0.1123(5) 0.0402(13) Uani 1 1 d . U . . .
N2 N 0.3969(4) 0.7199(3) 0.0078(4) 0.0318(12) Uani 1 1 d . U . . .
N3 N 0.3718(4) 1.1255(4) 0.0042(5) 0.0425(14) Uani 1 1 d . U . . .
C1 C 0.4021(5) 0.5624(5) 0.1634(7) 0.0483(18) Uani 1 1 d . U . A 1
H1 H 0.4118 0.5884 0.2246 0.058 Uiso 1 1 calc R . . A 1
C2 C 0.3831(5) 0.4691(5) 0.1268(8) 0.055(2) Uani 1 1 d . U . . .
H2 H 0.3780 0.4352 0.1632 0.066 Uiso 1 1 calc R . . A .
C3 C 0.3726(5) 0.4306(5) 0.0393(8) 0.0544(19) Uani 1 1 d . U . . .
H3 H 0.3611 0.3698 0.0156 0.065 Uiso 1 1 calc R . . . .
C4 C 0.3789(5) 0.4818(4) -0.0166(7) 0.0488(17) Uani 1 1 d . U . . .
C5 C 0.3682(5) 0.4466(5) -0.1090(7) 0.0536(19) Uani 1 1 d . U . . .
H5 H 0.3565 0.3861 -0.1359 0.064 Uiso 1 1 calc R . . . .
C6 C 0.3748(5) 0.4994(5) -0.1590(7) 0.053(2) Uani 1 1 d . U . . .
H6 H 0.3719 0.4749 -0.2183 0.064 Uiso 1 1 calc R . . . .
C7 C 0.3861(5) 0.5921(5) -0.1219(6) 0.0438(17) Uani 1 1 d . U . . .
H7 H 0.3896 0.6279 -0.1572 0.053 Uiso 1 1 calc R . . . .
C8 C 0.3920(5) 0.6292(4) -0.0335(6) 0.0382(15) Uani 1 1 d . U . . .
C9 C 0.3927(5) 0.5738(4) 0.0225(6) 0.0398(15) Uani 1 1 d . U . . .
C10 C 0.3468(5) 0.7632(4) -0.0497(5) 0.0318(14) Uani 1 1 d . U . . .
H10 H 0.3052 0.7298 -0.1090 0.038 Uiso 1 1 calc R . . . .
C11 C 0.3502(5) 0.8556(4) -0.0299(5) 0.0311(13) Uani 1 1 d . U . . .
C12 C 0.2859(5) 0.8916(5) -0.0983(5) 0.0353(15) Uani 1 1 d . U . . .
H12 H 0.2386 0.8542 -0.1518 0.042 Uiso 1 1 calc R . . . .
C13 C 0.2926(5) 0.9796(5) -0.0867(6) 0.0378(15) Uani 1 1 d . U . . .
C14 C 0.2262(6) 1.0171(6) -0.1602(7) 0.0464(18) Uani 1 1 d . U . . .
H14A H 0.1732 1.0360 -0.1454 0.056 Uiso 1 1 calc R . . . .
H14B H 0.2010 0.9725 -0.2199 0.056 Uiso 1 1 calc R . . . .
C15 C 0.2805(6) 1.0944(6) -0.1646(7) 0.0505(19) Uani 1 1 d . U . . .
H15A H 0.3313 1.0747 -0.1828 0.061 Uiso 1 1 calc R . . . .
H15B H 0.2379 1.1197 -0.2105 0.061 Uiso 1 1 calc R . . . .
C16 C 0.3212(6) 1.1611(5) -0.0726(7) 0.0503(18) Uani 1 1 d . U . . .
H16A H 0.3648 1.2049 -0.0732 0.060 Uiso 1 1 calc R . . . .
H16B H 0.2700 1.1903 -0.0620 0.060 Uiso 1 1 calc R . . . .
C17 C 0.4410(6) 1.1895(5) 0.0884(7) 0.0456(17) Uani 1 1 d . U . . .
H17A H 0.4142 1.2440 0.0994 0.055 Uiso 1 1 calc R . . . .
H17B H 0.4980 1.2016 0.0797 0.055 Uiso 1 1 calc R . . . .
C18 C 0.4670(5) 1.1562(4) 0.1711(6) 0.0426(17) Uani 1 1 d . U . . .
H18A H 0.4122 1.1527 0.1858 0.051 Uiso 1 1 calc R . . . .
H18B H 0.5177 1.1967 0.2242 0.051 Uiso 1 1 calc R . . . .
C19 C 0.4995(5) 1.0657(4) 0.1522(6) 0.0381(16) Uani 1 1 d . U . . .
H19A H 0.5595 1.0705 0.1464 0.046 Uiso 1 1 calc R . . . .
H19B H 0.5095 1.0426 0.2037 0.046 Uiso 1 1 calc R . . . .
C20 C 0.3639(5) 1.0377(4) -0.0045(6) 0.0358(14) Uani 1 1 d . U . . .
C21 C 0.4262(5) 1.0049(4) 0.0651(5) 0.0337(14) Uani 1 1 d . U . . .
C22 C 0.4186(5) 0.9147(4) 0.0522(5) 0.0313(13) Uani 1 1 d . U . . .
U2 U -0.19585(2) 0.72107(2) -0.18315(2) 0.04072(10) Uani 1 1 d . U . . .
O3W O -0.2498(5) 0.5945(4) -0.3237(5) 0.0637(17) Uani 1 1 d . U . . .
H3WA H -0.2656 0.6102 -0.3778 0.096 Uiso 1 1 d GR . . . .
H3WB H -0.3034 0.5605 -0.3323 0.096 Uiso 1 1 d GR . . . .
O4 O -0.3008(4) 0.6986(3) -0.1680(4) 0.0463(13) Uani 1 1 d . U . . .
O4W O -0.2954(5) 0.7720(4) -0.3126(5) 0.074(2) Uani 1 1 d . U . . .
H4WA H -0.3593 0.7485 -0.3377 0.111 Uiso 1 1 d GR . . . .
H4WB H -0.2773 0.7573 -0.3620 0.111 Uiso 1 1 d GR . . . .
O5 O -0.0949(4) 0.7485(4) -0.2012(5) 0.0509(14) Uani 1 1 d . U . . .
O6 O -0.1329(3) 0.6129(3) -0.1313(4) 0.0350(10) Uani 1 1 d . U . . .
N4 N -0.1911(5) 0.8885(4) -0.1079(6) 0.0487(15) Uani 1 1 d . U . . .
N5 N -0.1111(4) 0.7760(4) -0.0099(5) 0.0396(13) Uani 1 1 d . U . . .
N6 N -0.1315(4) 0.3658(3) -0.0201(4) 0.0322(12) Uani 1 1 d . U . . .
C23 C -0.2362(7) 0.9421(5) -0.1563(9) 0.062(2) Uani 1 1 d . U . . .
H23 H -0.2792 0.9185 -0.2178 0.074 Uiso 1 1 calc R . . . .
C24 C -0.2197(8) 1.0343(6) -0.1156(10) 0.076(3) Uani 1 1 d . U . . .
H24 H -0.2554 1.0701 -0.1490 0.091 Uiso 1 1 calc R . . . .
C25 C -0.1546(8) 1.0693(6) -0.0311(10) 0.072(2) Uani 1 1 d . U . . .
H25 H -0.1429 1.1300 -0.0062 0.087 Uiso 1 1 calc R . . . .
C26 C -0.1007(7) 1.0155(5) 0.0237(9) 0.066(2) Uani 1 1 d . U . . .
C27 C -0.0301(7) 1.0485(5) 0.1124(9) 0.071(2) Uani 1 1 d . U . . .
H27 H -0.0155 1.1088 0.1401 0.085 Uiso 1 1 calc R . . . .
C28 C 0.0186(7) 0.9926(6) 0.1596(9) 0.069(2) Uani 1 1 d . U . . .
H28 H 0.0685 1.0153 0.2178 0.083 Uiso 1 1 calc R . . . .
C29 C -0.0064(6) 0.9002(5) 0.1205(7) 0.054(2) Uani 1 1 d . U . . .
H29 H 0.0259 0.8627 0.1535 0.065 Uiso 1 1 calc R . . . .
C30 C -0.0792(5) 0.8665(4) 0.0330(7) 0.0472(17) Uani 1 1 d . U . . .
C31 C -0.1257(6) 0.9227(5) -0.0201(8) 0.0519(17) Uani 1 1 d . U . . .
C32 C -0.1099(5) 0.7273(4) 0.0442(6) 0.0363(15) Uani 1 1 d . U . . .
H32 H -0.0972 0.7578 0.1052 0.044 Uiso 1 1 calc R . . . .
C33 C -0.1252(4) 0.6349(4) 0.0214(5) 0.0312(13) Uani 1 1 d . U . . .
C34 C -0.1268(4) 0.5969(4) 0.0892(5) 0.0325(14) Uani 1 1 d . U . . .
H34 H -0.1241 0.6333 0.1449 0.039 Uiso 1 1 calc R . . . .
C35 C -0.1321(4) 0.5084(4) 0.0760(5) 0.0301(13) Uani 1 1 d . U . . .
C36 C -0.1371(5) 0.4664(5) 0.1458(5) 0.0364(15) Uani 1 1 d . U . . .
H36A H -0.2027 0.4446 0.1288 0.044 Uiso 1 1 calc R . . . .
H36B H -0.1134 0.5095 0.2065 0.044 Uiso 1 1 calc R . . . .
C37 C -0.0769(5) 0.3907(5) 0.1492(6) 0.0415(16) Uani 1 1 d . U . . .
H37A H -0.0107 0.4126 0.1686 0.050 Uiso 1 1 calc R . . . .
H37B H -0.0807 0.3625 0.1934 0.050 Uiso 1 1 calc R . . . .
C38 C -0.1146(5) 0.3254(5) 0.0534(5) 0.0382(15) Uani 1 1 d . U . . .
H38A H -0.0693 0.2840 0.0517 0.046 Uiso 1 1 calc R . . . .
H38B H -0.1738 0.2928 0.0419 0.046 Uiso 1 1 calc R . . . .
C39 C -0.1406(5) 0.3048(4) -0.1080(5) 0.0353(14) Uani 1 1 d . U . . .
H39A H -0.1754 0.2494 -0.1179 0.042 Uiso 1 1 calc R . . . .
H39B H -0.0776 0.2939 -0.1045 0.042 Uiso 1 1 calc R . . . .
C40 C -0.1912(5) 0.3391(4) -0.1892(5) 0.0342(14) Uani 1 1 d . U . . .
H40A H -0.2572 0.3423 -0.1988 0.041 Uiso 1 1 calc R . . . .
H40B H -0.1900 0.2996 -0.2448 0.041 Uiso 1 1 calc R . . . .
C41 C -0.1426(5) 0.4297(4) -0.1708(5) 0.0365(15) Uani 1 1 d . U . . .
H41A H -0.0793 0.4254 -0.1692 0.044 Uiso 1 1 calc R . . . .
H41B H -0.1788 0.4541 -0.2204 0.044 Uiso 1 1 calc R . . . .
C42 C -0.1326(4) 0.4536(4) -0.0082(5) 0.0280(12) Uani 1 1 d . U . . .
C43 C -0.1358(4) 0.4886(4) -0.0801(5) 0.0276(12) Uani 1 1 d . U . . .
C44 C -0.1331(4) 0.5796(4) -0.0648(5) 0.0307(13) Uani 1 1 d . U . . .
O7 O 0.1699(5) 0.5982(4) -0.3646(5) 0.0604(17) Uani 1 1 d . U . . .
H7A H 0.1346 0.5575 -0.3678 0.091 Uiso 1 1 calc GR . . . .
N7 N 0.1231(5) 0.3785(5) -0.3592(5) 0.0507(16) Uani 1 1 d . U . . .
N8 N 0.0148(6) 0.5030(5) -0.3889(5) 0.0560(18) Uani 1 1 d . U . . .
N9 N 0.1432(7) 0.8866(6) -0.3955(6) 0.070(2) Uani 1 1 d . U . . .
C45 C 0.1819(8) 0.3196(6) -0.3383(7) 0.061(2) Uani 1 1 d . U . . .
H45 H 0.2443 0.3315 -0.3306 0.073 Uiso 1 1 calc R . . . .
C46 C 0.1554(9) 0.2402(7) -0.3270(7) 0.072(3) Uani 1 1 d . U . . .
H46 H 0.1989 0.2004 -0.3142 0.086 Uiso 1 1 calc R . . . .
C47 C 0.0658(9) 0.2226(7) -0.3351(7) 0.072(2) Uani 1 1 d . U . . .
H47 H 0.0479 0.1717 -0.3252 0.087 Uiso 1 1 calc R . . . .
C48 C -0.0009(8) 0.2828(6) -0.3590(6) 0.065(2) Uani 1 1 d . U . . .
C49 C -0.0990(9) 0.2707(8) -0.3711(8) 0.081(3) Uani 1 1 d . U . . .
H49 H -0.1235 0.2206 -0.3647 0.097 Uiso 1 1 calc R . . . .
C50 C -0.1527(9) 0.3326(8) -0.3915(8) 0.080(3) Uani 1 1 d . U . . .
H50 H -0.2162 0.3229 -0.4014 0.096 Uiso 1 1 calc R . . . .
C51 C -0.1223(8) 0.4105(8) -0.3994(7) 0.075(3) Uani 1 1 d . U . . .
H51 H -0.1638 0.4517 -0.4129 0.090 Uiso 1 1 calc R . . . .
C52 C -0.0279(7) 0.4260(7) -0.3864(6) 0.057(2) Uani 1 1 d . U . . .
C53 C 0.0325(7) 0.3609(6) -0.3689(6) 0.0524(18) Uani 1 1 d . U . . .
C54 C -0.0229(7) 0.5765(6) -0.3970(6) 0.056(2) Uani 1 1 d . U . . .
H54 H -0.0865 0.5763 -0.4065 0.067 Uiso 1 1 calc R . . . .
C55 C 0.0232(7) 0.6530(6) -0.3927(6) 0.0545(19) Uani 1 1 d . U . . .
C56 C -0.0294(7) 0.7263(7) -0.4032(6) 0.062(2) Uani 1 1 d . U . . .
H56 H -0.0920 0.7208 -0.4094 0.074 Uiso 1 1 calc R . . . .
C57 C 0.0075(7) 0.8020(7) -0.4044(6) 0.060(2) Uani 1 1 d . U . . .
C58 C -0.0508(9) 0.8754(7) -0.4187(7) 0.077(3) Uani 1 1 d . U . . .
H58A H -0.0953 0.8757 -0.3903 0.092 Uiso 1 1 calc R . . . .
H58B H -0.0873 0.8660 -0.4845 0.092 Uiso 1 1 calc R . . . .
C59 C 0.0118(9) 0.9635(7) -0.3768(8) 0.080(3) Uani 1 1 d . U . . .
H59A H -0.0267 1.0090 -0.3935 0.095 Uiso 1 1 calc R . . . .
H59B H 0.0405 0.9776 -0.3097 0.095 Uiso 1 1 calc R . . . .
C60 C 0.0882(11) 0.9596(9) -0.4121(11) 0.101(4) Uani 1 1 d . U . . .
H60A H 0.0592 0.9528 -0.4781 0.122 Uiso 1 1 calc R . . . .
H60B H 0.1309 1.0143 -0.3815 0.122 Uiso 1 1 calc R . . . .
C61A C 0.2215(17) 0.8871(13) -0.4076(14) 0.059(4) Uani 0.5 1 d D U P B 2
H61A H 0.2458 0.9466 -0.3989 0.071 Uiso 0.5 1 calc R . P B 2
H61B H 0.2096 0.8522 -0.4700 0.071 Uiso 0.5 1 calc R . P B 2
C61B C 0.2554(18) 0.9099(13) -0.3729(17) 0.065(5) Uani 0.5 1 d D U P B 1
H61C H 0.2606 0.9418 -0.4138 0.078 Uiso 0.5 1 calc R . P B 1
H61D H 0.2887 0.9470 -0.3095 0.078 Uiso 0.5 1 calc R . P B 1
C62A C 0.2932(14) 0.8495(9) -0.3376(11) 0.049(3) Uani 0.5 1 d D U P B 2
H62A H 0.3553 0.8588 -0.3381 0.059 Uiso 0.5 1 calc R . P B 2
H62B H 0.2980 0.8799 -0.2761 0.059 Uiso 0.5 1 calc R . P B 2
C62B C 0.3001(15) 0.8281(10) -0.3859(17) 0.067(5) Uani 0.5 1 d D U P B 1
H62C H 0.3684 0.8428 -0.3503 0.081 Uiso 0.5 1 calc R . P B 1
H62D H 0.2886 0.8060 -0.4507 0.081 Uiso 0.5 1 calc R . P B 1
C63 C 0.2660(8) 0.7548(6) -0.3581(8) 0.065(2) Uani 1 1 d D U . . .
H63A H 0.3045 0.7343 -0.3061 0.077 Uiso 0.5 1 calc R . P B 2
H63B H 0.2748 0.7218 -0.4125 0.077 Uiso 0.5 1 calc R . P B 2
C64 C 0.1060(8) 0.8126(6) -0.3920(6) 0.060(2) Uani 1 1 d . U . . .
C65 C 0.1631(7) 0.7439(6) -0.3751(6) 0.054(2) Uani 1 1 d . U . . .
C66 C 0.1215(7) 0.6657(6) -0.3774(6) 0.055(2) Uani 1 1 d . U . . .
O1N2 O 0.2116(18) 0.8761(10) 0.3025(14) 0.119(7) Uani 0.5 1 d D U P C 1
O2N2 O 0.2511(18) 1.0173(11) 0.3618(16) 0.128(8) Uani 0.5 1 d D U P C 1
O3N2 O 0.1837(17) 0.9500(12) 0.4070(15) 0.116(7) Uani 0.5 1 d D U P C 1
N2N N 0.2251(10) 0.9433(10) 0.3577(11) 0.062(4) Uani 0.5 1 d D U P C 1
O1N1 O 0.7070(8) 0.7462(6) 0.5097(7) 0.111(3) Uani 1 1 d . U . . .
O2N1 O 0.7292(6) 0.6103(6) 0.5072(5) 0.082(2) Uani 1 1 d . U . . .
O3N1 O 0.6337(7) 0.6396(7) 0.3816(6) 0.103(3) Uani 1 1 d . U . . .
N1N N 0.6895(7) 0.6641(7) 0.4674(7) 0.085(3) Uani 1 1 d . U . . .
O5W O 0.7076(7) 0.8914(6) 0.4386(6) 0.099(3) Uani 1 1 d . U . . .
H5WA H 0.7025 0.8527 0.4640 0.148 Uiso 1 1 d G . . . .
H5WB H 0.7138 0.9421 0.4756 0.148 Uiso 1 1 d G . . . .
O7W O -0.3910(16) 0.4876(14) -0.3528(11) 0.131(9) Uani 0.5 1 d . U P . .
O9W O 0.4513(13) 1.0356(12) 0.3724(18) 0.128(9) Uani 0.5 1 d . U P . .
O8W O 0.3825(17) 0.7913(16) 0.4118(15) 0.130(8) Uani 0.5 1 d . U P . .
O6W O 0.3343(8) 0.5611(7) -0.3670(9) 0.136(4) Uani 1 1 d . U . . .
H6WA H 0.3347 0.5095 -0.3621 0.204 Uiso 1 1 d R . . . .
H6WB H 0.2925 0.5856 -0.3510 0.204 Uiso 1 1 d R . . . .
O10W O 0.266(2) 0.925(2) 0.412(2) 0.087(8) Uiso 0.3 1 d . U P D 2
O3N3 O -0.6122(12) 0.641(2) -0.4859(16) 0.170(10) Uani 0.5 1 d D U P E 2
N3N N -0.5316(15) 0.682(2) -0.4237(19) 0.195(11) Uani 0.5 1 d D U P E 2
O1N3 O -0.4812(14) 0.755(2) -0.402(2) 0.200(12) Uani 0.5 1 d D U P E 2
O12W O -0.489(3) 0.652(2) -0.510(3) 0.073(10) Uiso 0.2 1 d . U P F 1
O2N3 O -0.494(2) 0.654(3) -0.352(2) 0.233(14) Uani 0.5 1 d D U P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
U1 O1 1.780(5) . ?
U1 O1W 2.407(6) . ?
U1 O2 1.776(5) . ?
U1 O2W 2.437(6) . ?
U1 O3 2.208(4) . ?
U1 N0AA 2.620(6) . ?
U1 N2 2.493(6) . ?
O1W H1WA 0.9178 . ?
O1W H1WB 0.9163 . ?
O2W H2WA 0.9161 . ?
O2W H2WB 0.9176 . ?
O3 C22 1.328(8) . ?
N0AA C1 1.329(10) . ?
N0AA C9 1.369(11) . ?
N2 C8 1.413(8) . ?
N2 C10 1.323(9) . ?
N3 C16 1.461(10) . ?
N3 C17 1.467(11) . ?
N3 C20 1.369(8) . ?
C1 H1 0.9300 . ?
C1 C2 1.428(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.347(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.411(13) . ?
C4 C5 1.413(14) . ?
C4 C9 1.413(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.353(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.422(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.381(12) . ?
C8 C9 1.433(11) . ?
C10 H10 0.9300 . ?
C10 C11 1.418(9) . ?
C11 C12 1.432(10) . ?
C11 C22 1.413(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.363(10) . ?
C13 C14 1.510(10) . ?
C13 C20 1.425(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.517(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.480(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.500(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.527(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C21 1.491(10) . ?
C20 C21 1.402(10) . ?
C21 C22 1.395(9) . ?
U2 O3W 2.463(7) . ?
U2 O4 1.779(5) . ?
U2 O4W 2.429(7) . ?
U2 O5 1.768(5) . ?
U2 O6 2.194(5) . ?
U2 N4 2.614(6) . ?
U2 N5 2.506(7) . ?
O3W H3WA 0.9278 . ?
O3W H3WB 0.9243 . ?
O4W H4WA 0.9319 . ?
O4W H4WB 0.9338 . ?
O6 C44 1.336(9) . ?
N4 C23 1.335(11) . ?
N4 C31 1.347(12) . ?
N5 C30 1.412(8) . ?
N5 C32 1.324(10) . ?
N6 C38 1.453(9) . ?
N6 C39 1.464(9) . ?
N6 C42 1.365(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.418(13) . ?
C24 H24 0.9300 . ?
C24 C25 1.311(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.440(16) . ?
C26 C27 1.382(16) . ?
C26 C31 1.436(10) . ?
C27 H27 0.9300 . ?
C27 C28 1.373(16) . ?
C28 H28 0.9300 . ?
C28 C29 1.423(11) . ?
C29 H29 0.9300 . ?
C29 C30 1.383(13) . ?
C30 C31 1.420(13) . ?
C32 H32 0.9300 . ?
C32 C33 1.414(9) . ?
C33 C34 1.411(10) . ?
C33 C44 1.413(10) . ?
C34 H34 0.9300 . ?
C34 C35 1.367(9) . ?
C35 C36 1.500(10) . ?
C35 C42 1.423(10) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.530(10) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.514(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.504(10) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.519(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C43 1.498(10) . ?
C42 C43 1.419(9) . ?
C43 C44 1.404(8) . ?
O7 H7A 0.8200 . ?
O7 C66 1.332(10) . ?
N7 C45 1.329(12) . ?
N7 C53 1.359(12) . ?
N8 C52 1.406(12) . ?
N8 C54 1.329(12) . ?
N9 C60 1.468(14) . ?
N9 C61A 1.30(3) . ?
N9 C61B 1.64(3) . ?
N9 C64 1.332(13) . ?
C45 H45 0.9300 . ?
C45 C46 1.406(14) . ?
C46 H46 0.9300 . ?
C46 C47 1.353(16) . ?
C47 H47 0.9300 . ?
C47 C48 1.427(16) . ?
C48 C49 1.449(16) . ?
C48 C53 1.416(13) . ?
C49 H49 0.9300 . ?
C49 C50 1.322(18) . ?
C50 H50 0.9300 . ?
C50 C51 1.379(17) . ?
C51 H51 0.9300 . ?
C51 C52 1.394(14) . ?
C52 C53 1.413(14) . ?
C54 H54 0.9300 . ?
C54 C55 1.376(14) . ?
C55 C56 1.439(13) . ?
C55 C66 1.437(13) . ?
C56 H56 0.9300 . ?
C56 C57 1.340(15) . ?
C57 C58 1.494(13) . ?
C57 C64 1.451(15) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C59 1.521(16) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.501(18) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61A H61A 0.9700 . ?
C61A H61B 0.9700 . ?
C61A C62A 1.510(16) . ?
C61B H61C 0.9700 . ?
C61B H61D 0.9700 . ?
C61B C62B 1.486(16) . ?
C62A H62A 0.9700 . ?
C62A H62B 0.9700 . ?
C62A C63 1.475(14) . ?
C62B H62C 0.9700 . ?
C62B H62D 0.9700 . ?
C62B C63 1.521(15) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C65 1.498(14) . ?
C64 C65 1.429(13) . ?
C65 C66 1.383(13) . ?
O1N2 N2N 1.159(15) . ?
O2N2 N2N 1.220(16) . ?
O3N2 N2N 1.199(16) . ?
O1N1 N1N 1.277(13) . ?
O2N1 N1N 1.238(12) . ?
O3N1 N1N 1.273(12) . ?
O5W H5WA 0.8508 . ?
O5W H5WB 0.8509 . ?
O6W H6WA 0.8498 . ?
O6W H6WB 0.8503 . ?
O3N3 N3N 1.281(18) . ?
N3N O1N3 1.263(19) . ?
N3N O2N3 1.296(19) . ?

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
O1 U1 O1W 88.8(2) . . ?
O1 U1 O2W 90.4(2) . . ?
O1 U1 O3 90.8(2) . . ?
O1 U1 N0AA 91.4(2) . . ?
O1 U1 N2 87.8(2) . . ?
O1W U1 O2W 73.3(2) . . ?
O1W U1 N0AA 75.7(2) . . ?
O1W U1 N2 138.9(2) . . ?
O2 U1 O1 177.1(2) . . ?
O2 U1 O1W 88.5(2) . . ?
O2 U1 O2W 89.5(2) . . ?
O2 U1 O3 92.0(2) . . ?
O2 U1 N0AA 87.2(2) . . ?
O2 U1 N2 93.8(2) . . ?
O2W U1 N0AA 148.9(2) . . ?
O2W U1 N2 147.64(19) . . ?
O3 U1 O1W 150.8(2) . . ?
O3 U1 O2W 77.5(2) . . ?
O3 U1 N0AA 133.5(2) . . ?
O3 U1 N2 70.21(18) . . ?
N2 U1 N0AA 63.5(2) . . ?
U1 O1W H1WA 140.5 . . ?
U1 O1W H1WB 112.2 . . ?
H1WA O1W H1WB 106.0 . . ?
U1 O2W H2WA 128.7 . . ?
U1 O2W H2WB 116.1 . . ?
H2WA O2W H2WB 114.2 . . ?
C22 O3 U1 133.2(4) . . ?
C1 N0AA U1 123.7(6) . . ?
C1 N0AA C9 118.5(7) . . ?
C9 N0AA U1 117.0(4) . . ?
C8 N2 U1 120.0(5) . . ?
C10 N2 U1 123.8(5) . . ?
C10 N2 C8 114.9(6) . . ?
C16 N3 C17 114.9(6) . . ?
C20 N3 C16 122.8(7) . . ?
C20 N3 C17 121.8(7) . . ?
N0AA C1 H1 119.1 . . ?
N0AA C1 C2 121.8(9) . . ?
C2 C1 H1 119.1 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.6(8) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(7) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 123.9(7) . . ?
C3 C4 C9 116.9(9) . . ?
C9 C4 C5 119.1(8) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(7) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(9) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.1(8) . . ?
C8 C7 H7 119.9 . . ?
N2 C8 C9 115.8(7) . . ?
C7 C8 N2 124.8(7) . . ?
C7 C8 C9 119.5(7) . . ?
N0AA C9 C4 122.7(8) . . ?
N0AA C9 C8 118.0(6) . . ?
C4 C9 C8 119.3(8) . . ?
N2 C10 H10 116.8 . . ?
N2 C10 C11 126.3(7) . . ?
C11 C10 H10 116.8 . . ?
C10 C11 C12 119.0(7) . . ?
C22 C11 C10 123.1(6) . . ?
C22 C11 C12 117.8(6) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.3(7) . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C14 121.1(7) . . ?
C12 C13 C20 119.9(7) . . ?
C20 C13 C14 118.9(7) . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.3(7) . . ?
H14A C14 H14B 108.3 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C14 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 C14 109.6(7) . . ?
C16 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
N3 C16 C15 113.9(7) . . ?
N3 C16 H16A 108.8 . . ?
N3 C16 H16B 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N3 C17 H17A 109.4 . . ?
N3 C17 H17B 109.4 . . ?
N3 C17 C18 111.3(6) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 C19 110.8(7) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C18 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.2 . . ?
C21 C19 C18 110.1(6) . . ?
C21 C19 H19A 109.6 . . ?
C21 C19 H19B 109.6 . . ?
N3 C20 C13 118.9(7) . . ?
N3 C20 C21 120.8(7) . . ?
C21 C20 C13 120.3(6) . . ?
C20 C21 C19 120.5(6) . . ?
C22 C21 C19 120.3(7) . . ?
C22 C21 C20 119.2(7) . . ?
O3 C22 C11 120.0(6) . . ?
O3 C22 C21 118.5(6) . . ?
C21 C22 C11 121.5(7) . . ?
O3W U2 N4 148.8(2) . . ?
O3W U2 N5 147.3(2) . . ?
O4 U2 O3W 90.3(3) . . ?
O4 U2 O4W 87.4(3) . . ?
O4 U2 O6 91.7(2) . . ?
O4 U2 N4 90.0(2) . . ?
O4 U2 N5 87.3(2) . . ?
O4W U2 O3W 72.7(2) . . ?
O4W U2 N4 76.1(3) . . ?
O4W U2 N5 139.6(2) . . ?
O5 U2 O3W 90.3(3) . . ?
O5 U2 O4 176.5(2) . . ?
O5 U2 O4W 89.5(3) . . ?
O5 U2 O6 91.8(2) . . ?
O5 U2 N4 87.6(2) . . ?
O5 U2 N5 94.0(3) . . ?
O6 U2 O3W 76.3(2) . . ?
O6 U2 O4W 149.0(2) . . ?
O6 U2 N4 134.9(2) . . ?
O6 U2 N5 71.22(19) . . ?
N5 U2 N4 63.9(2) . . ?
U2 O3W H3WA 113.4 . . ?
U2 O3W H3WB 112.6 . . ?
H3WA O3W H3WB 105.6 . . ?
U2 O4W H4WA 113.0 . . ?
U2 O4W H4WB 113.0 . . ?
H4WA O4W H4WB 105.4 . . ?
C44 O6 U2 134.5(4) . . ?
C23 N4 U2 123.3(7) . . ?
C23 N4 C31 119.4(7) . . ?
C31 N4 U2 116.1(5) . . ?
C30 N5 U2 119.0(6) . . ?
C32 N5 U2 122.6(5) . . ?
C32 N5 C30 117.3(7) . . ?
C38 N6 C39 114.2(5) . . ?
C42 N6 C38 123.9(6) . . ?
C42 N6 C39 121.8(6) . . ?
N4 C23 H23 119.4 . . ?
N4 C23 C24 121.2(11) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(11) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.2(9) . . ?
C26 C25 H25 119.4 . . ?
C27 C26 C25 123.9(8) . . ?
C27 C26 C31 121.0(10) . . ?
C31 C26 C25 115.1(11) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.2(8) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.7(11) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.2 . . ?
C30 C29 C28 119.5(10) . . ?
C30 C29 H29 120.2 . . ?
N5 C30 C31 115.7(8) . . ?
C29 C30 N5 123.5(8) . . ?
C29 C30 C31 120.8(7) . . ?
N4 C31 C26 122.5(9) . . ?
N4 C31 C30 120.1(7) . . ?
C30 C31 C26 117.5(10) . . ?
N5 C32 H32 115.7 . . ?
N5 C32 C33 128.5(7) . . ?
C33 C32 H32 115.7 . . ?
C32 C33 C44 122.1(7) . . ?
C34 C33 C32 118.8(7) . . ?
C34 C33 C44 119.0(6) . . ?
C33 C34 H34 118.8 . . ?
C35 C34 C33 122.4(7) . . ?
C35 C34 H34 118.8 . . ?
C34 C35 C36 123.3(7) . . ?
C34 C35 C42 118.2(6) . . ?
C42 C35 C36 118.6(6) . . ?
C35 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
C35 C36 C37 109.5(6) . . ?
H36A C36 H36B 108.2 . . ?
C37 C36 H36A 109.8 . . ?
C37 C36 H36B 109.8 . . ?
C36 C37 H37A 110.0 . . ?
C36 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
C38 C37 C36 108.5(6) . . ?
C38 C37 H37A 110.0 . . ?
C38 C37 H37B 110.0 . . ?
N6 C38 C37 113.6(6) . . ?
N6 C38 H38A 108.9 . . ?
N6 C38 H38B 108.9 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
N6 C39 H39A 109.1 . . ?
N6 C39 H39B 109.1 . . ?
N6 C39 C40 112.5(6) . . ?
H39A C39 H39B 107.8 . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C39 C40 H40A 109.7 . . ?
C39 C40 H40B 109.7 . . ?
C39 C40 C41 109.7(6) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C40 C41 H41A 109.7 . . ?
C40 C41 H41B 109.7 . . ?
H41A C41 H41B 108.2 . . ?
C43 C41 C40 109.9(6) . . ?
C43 C41 H41A 109.7 . . ?
C43 C41 H41B 109.7 . . ?
N6 C42 C35 119.0(6) . . ?
N6 C42 C43 119.8(6) . . ?
C43 C42 C35 121.2(6) . . ?
C42 C43 C41 120.8(6) . . ?
C44 C43 C41 120.5(6) . . ?
C44 C43 C42 118.7(6) . . ?
O6 C44 C33 121.0(6) . . ?
O6 C44 C43 118.7(6) . . ?
C43 C44 C33 120.2(7) . . ?
C66 O7 H7A 109.5 . . ?
C45 N7 C53 117.5(8) . . ?
C54 N8 C52 127.9(9) . . ?
C60 N9 C61B 112.7(11) . . ?
C61A N9 C60 116.4(13) . . ?
C61A N9 C64 118.9(12) . . ?
C64 N9 C60 122.6(11) . . ?
C64 N9 C61B 124.4(10) . . ?
N7 C45 H45 118.0 . . ?
N7 C45 C46 123.9(11) . . ?
C46 C45 H45 118.0 . . ?
C45 C46 H46 120.4 . . ?
C47 C46 C45 119.1(12) . . ?
C47 C46 H46 120.4 . . ?
C46 C47 H47 120.3 . . ?
C46 C47 C48 119.4(10) . . ?
C48 C47 H47 120.3 . . ?
C47 C48 C49 124.6(10) . . ?
C53 C48 C47 117.3(10) . . ?
C53 C48 C49 118.0(11) . . ?
C48 C49 H49 120.8 . . ?
C50 C49 C48 118.5(12) . . ?
C50 C49 H49 120.8 . . ?
C49 C50 H50 117.4 . . ?
C49 C50 C51 125.3(12) . . ?
C51 C50 H50 117.4 . . ?
C50 C51 H51 120.8 . . ?
C50 C51 C52 118.4(13) . . ?
C52 C51 H51 120.8 . . ?
N8 C52 C53 115.2(9) . . ?
C51 C52 N8 125.4(11) . . ?
C51 C52 C53 119.4(10) . . ?
N7 C53 C48 122.7(10) . . ?
N7 C53 C52 117.0(8) . . ?
C52 C53 C48 120.2(10) . . ?
N8 C54 H54 116.8 . . ?
N8 C54 C55 126.3(9) . . ?
C55 C54 H54 116.8 . . ?
C54 C55 C56 118.5(9) . . ?
C54 C55 C66 124.5(9) . . ?
C66 C55 C56 116.9(9) . . ?
C55 C56 H56 118.5 . . ?
C57 C56 C55 123.1(10) . . ?
C57 C56 H56 118.5 . . ?
C56 C57 C58 121.3(11) . . ?
C56 C57 C64 119.2(9) . . ?
C64 C57 C58 119.6(10) . . ?
C57 C58 H58A 109.4 . . ?
C57 C58 H58B 109.4 . . ?
C57 C58 C59 111.3(10) . . ?
H58A C58 H58B 108.0 . . ?
C59 C58 H58A 109.4 . . ?
C59 C58 H58B 109.4 . . ?
C58 C59 H59A 109.8 . . ?
C58 C59 H59B 109.8 . . ?
H59A C59 H59B 108.2 . . ?
C60 C59 C58 109.5(11) . . ?
C60 C59 H59A 109.8 . . ?
C60 C59 H59B 109.8 . . ?
N9 C60 C59 111.9(11) . . ?
N9 C60 H60A 109.2 . . ?
N9 C60 H60B 109.2 . . ?
C59 C60 H60A 109.2 . . ?
C59 C60 H60B 109.2 . . ?
H60A C60 H60B 107.9 . . ?
N9 C61A H61A 110.1 . . ?
N9 C61A H61B 110.1 . . ?
N9 C61A C62A 108.2(18) . . ?
H61A C61A H61B 108.4 . . ?
C62A C61A H61A 110.1 . . ?
C62A C61A H61B 110.1 . . ?
N9 C61B H61C 109.6 . . ?
N9 C61B H61D 109.6 . . ?
H61C C61B H61D 108.1 . . ?
C62B C61B N9 110.2(16) . . ?
C62B C61B H61C 109.6 . . ?
C62B C61B H61D 109.6 . . ?
C61A C62A H62A 109.3 . . ?
C61A C62A H62B 109.3 . . ?
H62A C62A H62B 108.0 . . ?
C63 C62A C61A 111.6(14) . . ?
C63 C62A H62A 109.3 . . ?
C63 C62A H62B 109.3 . . ?
C61B C62B H62C 108.3 . . ?
C61B C62B H62D 108.3 . . ?
C61B C62B C63 116.1(17) . . ?
H62C C62B H62D 107.4 . . ?
C63 C62B H62C 108.3 . . ?
C63 C62B H62D 108.3 . . ?
C62A C63 H63A 110.5 . . ?
C62A C63 H63B 110.5 . . ?
C62A C63 C65 106.1(10) . . ?
H63A C63 H63B 108.7 . . ?
C65 C63 C62B 117.5(11) . . ?
C65 C63 H63A 110.5 . . ?
C65 C63 H63B 110.5 . . ?
N9 C64 C57 120.0(9) . . ?
N9 C64 C65 120.2(11) . . ?
C65 C64 C57 119.8(10) . . ?
C64 C65 C63 120.8(9) . . ?
C66 C65 C63 119.9(8) . . ?
C66 C65 C64 119.2(10) . . ?
O7 C66 C55 116.1(9) . . ?
O7 C66 C65 122.4(9) . . ?
C65 C66 C55 121.6(9) . . ?
O1N2 N2N O2N2 132(2) . . ?
O1N2 N2N O3N2 116.9(19) . . ?
O3N2 N2N O2N2 107.3(18) . . ?
O2N1 N1N O1N1 121.1(11) . . ?
O2N1 N1N O3N1 120.8(11) . . ?
O3N1 N1N O1N1 117.9(11) . . ?
H5WA O5W H5WB 109.2 . . ?
H6WA O6W H6WB 109.4 . . ?
O3N3 N3N O2N3 116(3) . . ?
O1N3 N3N O3N3 138(3) . . ?
O1N3 N3N O2N3 104(3) . . ?

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
U1 O3 C22 C11 -44.1(9) . . . . ?
U1 O3 C22 C21 139.3(5) . . . . ?
U1 N0AA C1 C2 -169.9(5) . . . . ?
U1 N0AA C9 C4 167.0(5) . . . . ?
U1 N0AA C9 C8 -13.5(8) . . . . ?
U1 N2 C8 C7 -157.0(6) . . . . ?
U1 N2 C8 C9 23.6(7) . . . . ?
U1 N2 C10 C11 22.8(9) . . . . ?
N0AA C1 C2 C3 2.6(11) . . . . ?
N2 C8 C9 N0AA -5.6(9) . . . . ?
N2 C8 C9 C4 174.0(6) . . . . ?
N2 C10 C11 C12 -175.6(6) . . . . ?
N2 C10 C11 C22 8.8(11) . . . . ?
N3 C17 C18 C19 53.0(8) . . . . ?
N3 C20 C21 C19 2.9(10) . . . . ?
N3 C20 C21 C22 -177.5(6) . . . . ?
C1 N0AA C9 C4 -3.0(10) . . . . ?
C1 N0AA C9 C8 176.6(6) . . . . ?
C1 C2 C3 C4 -0.9(12) . . . . ?
C2 C3 C4 C5 -179.6(7) . . . . ?
C2 C3 C4 C9 -2.5(11) . . . . ?
C3 C4 C5 C6 179.8(7) . . . . ?
C3 C4 C9 N0AA 4.5(10) . . . . ?
C3 C4 C9 C8 -175.0(6) . . . . ?
C4 C5 C6 C7 -4.4(12) . . . . ?
C5 C4 C9 N0AA -178.2(7) . . . . ?
C5 C4 C9 C8 2.2(10) . . . . ?
C5 C6 C7 C8 1.0(11) . . . . ?
C6 C7 C8 N2 -175.5(6) . . . . ?
C6 C7 C8 C9 3.9(10) . . . . ?
C7 C8 C9 N0AA 174.9(6) . . . . ?
C7 C8 C9 C4 -5.5(10) . . . . ?
C8 N2 C10 C11 -170.0(6) . . . . ?
C9 N0AA C1 C2 -0.7(10) . . . . ?
C9 C4 C5 C6 2.7(11) . . . . ?
C10 N2 C8 C7 35.3(9) . . . . ?
C10 N2 C8 C9 -144.2(6) . . . . ?
C10 C11 C12 C13 -173.3(6) . . . . ?
C10 C11 C22 O3 -3.4(10) . . . . ?
C10 C11 C22 C21 173.1(6) . . . . ?
C11 C12 C13 C14 178.4(7) . . . . ?
C11 C12 C13 C20 -0.8(10) . . . . ?
C12 C11 C22 O3 -179.1(6) . . . . ?
C12 C11 C22 C21 -2.6(10) . . . . ?
C12 C13 C14 C15 -143.5(8) . . . . ?
C12 C13 C20 N3 177.5(6) . . . . ?
C12 C13 C20 C21 -1.1(10) . . . . ?
C13 C14 C15 C16 -57.9(9) . . . . ?
C13 C20 C21 C19 -178.5(6) . . . . ?
C13 C20 C21 C22 1.1(10) . . . . ?
C14 C13 C20 N3 -1.7(10) . . . . ?
C14 C13 C20 C21 179.7(7) . . . . ?
C14 C15 C16 N3 48.4(9) . . . . ?
C16 N3 C17 C18 162.5(6) . . . . ?
C16 N3 C20 C13 -10.4(10) . . . . ?
C16 N3 C20 C21 168.3(7) . . . . ?
C17 N3 C16 C15 158.4(6) . . . . ?
C17 N3 C20 C13 177.5(6) . . . . ?
C17 N3 C20 C21 -3.9(10) . . . . ?
C17 C18 C19 C21 -53.3(8) . . . . ?
C18 C19 C21 C20 25.9(9) . . . . ?
C18 C19 C21 C22 -153.7(6) . . . . ?
C19 C21 C22 O3 -3.0(10) . . . . ?
C19 C21 C22 C11 -179.6(6) . . . . ?
C20 N3 C16 C15 -14.3(10) . . . . ?
C20 N3 C17 C18 -24.8(9) . . . . ?
C20 C13 C14 C15 35.7(10) . . . . ?
C20 C21 C22 O3 177.4(6) . . . . ?
C20 C21 C22 C11 0.8(10) . . . . ?
C22 C11 C12 C13 2.6(10) . . . . ?
U2 O6 C44 C33 -39.8(9) . . . . ?
U2 O6 C44 C43 143.8(5) . . . . ?
U2 N4 C23 C24 -170.0(6) . . . . ?
U2 N4 C31 C26 166.7(5) . . . . ?
U2 N4 C31 C30 -13.8(8) . . . . ?
U2 N5 C30 C29 -157.3(6) . . . . ?
U2 N5 C30 C31 21.6(8) . . . . ?
U2 N5 C32 C33 21.8(10) . . . . ?
N4 C23 C24 C25 4.8(13) . . . . ?
N5 C30 C31 N4 -4.3(10) . . . . ?
N5 C30 C31 C26 175.2(6) . . . . ?
N5 C32 C33 C34 -175.8(7) . . . . ?
N5 C32 C33 C44 8.2(11) . . . . ?
N6 C39 C40 C41 53.7(8) . . . . ?
N6 C42 C43 C41 2.9(9) . . . . ?
N6 C42 C43 C44 -177.5(5) . . . . ?
C23 N4 C31 C26 -1.3(10) . . . . ?
C23 N4 C31 C30 178.2(7) . . . . ?
C23 C24 C25 C26 -2.4(13) . . . . ?
C24 C25 C26 C27 178.8(8) . . . . ?
C24 C25 C26 C31 -1.5(12) . . . . ?
C25 C26 C27 C28 -179.3(8) . . . . ?
C25 C26 C31 N4 3.5(11) . . . . ?
C25 C26 C31 C30 -176.0(7) . . . . ?
C26 C27 C28 C29 -3.7(12) . . . . ?
C27 C26 C31 N4 -176.9(7) . . . . ?
C27 C26 C31 C30 3.6(11) . . . . ?
C27 C28 C29 C30 1.5(12) . . . . ?
C28 C29 C30 N5 -177.7(7) . . . . ?
C28 C29 C30 C31 3.4(11) . . . . ?
C29 C30 C31 N4 174.7(7) . . . . ?
C29 C30 C31 C26 -5.8(10) . . . . ?
C30 N5 C32 C33 -170.5(6) . . . . ?
C31 N4 C23 C24 -2.9(11) . . . . ?
C31 C26 C27 C28 1.0(12) . . . . ?
C32 N5 C30 C29 34.6(10) . . . . ?
C32 N5 C30 C31 -146.5(7) . . . . ?
C32 C33 C34 C35 -173.6(6) . . . . ?
C32 C33 C44 O6 -4.7(10) . . . . ?
C32 C33 C44 C43 171.7(6) . . . . ?
C33 C34 C35 C36 -177.9(6) . . . . ?
C33 C34 C35 C42 2.2(9) . . . . ?
C34 C33 C44 O6 179.3(6) . . . . ?
C34 C33 C44 C43 -4.3(9) . . . . ?
C34 C35 C36 C37 -141.0(6) . . . . ?
C34 C35 C42 N6 175.7(6) . . . . ?
C34 C35 C42 C43 -5.3(9) . . . . ?
C35 C36 C37 C38 -58.6(7) . . . . ?
C35 C42 C43 C41 -176.1(6) . . . . ?
C35 C42 C43 C44 3.5(9) . . . . ?
C36 C35 C42 N6 -4.2(8) . . . . ?
C36 C35 C42 C43 174.9(6) . . . . ?
C36 C37 C38 N6 46.6(8) . . . . ?
C38 N6 C39 C40 159.6(6) . . . . ?
C38 N6 C42 C35 -10.1(9) . . . . ?
C38 N6 C42 C43 170.8(6) . . . . ?
C39 N6 C38 C37 162.9(6) . . . . ?
C39 N6 C42 C35 174.5(6) . . . . ?
C39 N6 C42 C43 -4.6(9) . . . . ?
C39 C40 C41 C43 -53.9(8) . . . . ?
C40 C41 C43 C42 27.0(9) . . . . ?
C40 C41 C43 C44 -152.6(6) . . . . ?
C41 C43 C44 O6 -2.6(9) . . . . ?
C41 C43 C44 C33 -179.0(6) . . . . ?
C42 N6 C38 C37 -12.8(9) . . . . ?
C42 N6 C39 C40 -24.6(8) . . . . ?
C42 C35 C36 C37 38.9(8) . . . . ?
C42 C43 C44 O6 177.8(5) . . . . ?
C42 C43 C44 C33 1.4(9) . . . . ?
C44 C33 C34 C35 2.5(9) . . . . ?
N7 C45 C46 C47 -2.0(16) . . . . ?
N8 C52 C53 N7 -1.8(12) . . . . ?
N8 C52 C53 C48 175.9(8) . . . . ?
N8 C54 C55 C56 179.9(9) . . . . ?
N8 C54 C55 C66 -0.7(15) . . . . ?
N9 C61A C62A C63 69.0(19) . . . . ?
N9 C61B C62B C63 -36(3) . . . . ?
N9 C64 C65 C63 1.9(14) . . . . ?
N9 C64 C65 C66 -176.0(9) . . . . ?
C45 N7 C53 C48 -0.9(12) . . . . ?
C45 N7 C53 C52 176.8(8) . . . . ?
C45 C46 C47 C48 2.9(15) . . . . ?
C46 C47 C48 C49 179.0(9) . . . . ?
C46 C47 C48 C53 -2.8(13) . . . . ?
C47 C48 C49 C50 178.7(10) . . . . ?
C47 C48 C53 N7 1.9(13) . . . . ?
C47 C48 C53 C52 -175.8(8) . . . . ?
C48 C49 C50 C51 -2.4(17) . . . . ?
C49 C48 C53 N7 -179.9(8) . . . . ?
C49 C48 C53 C52 2.5(12) . . . . ?
C49 C50 C51 C52 1.1(17) . . . . ?
C50 C51 C52 N8 -177.6(9) . . . . ?
C50 C51 C52 C53 2.1(14) . . . . ?
C51 C52 C53 N7 178.4(8) . . . . ?
C51 C52 C53 C48 -3.8(13) . . . . ?
C52 N8 C54 C55 175.2(9) . . . . ?
C53 N7 C45 C46 0.9(14) . . . . ?
C53 C48 C49 C50 0.5(14) . . . . ?
C54 N8 C52 C51 5.1(15) . . . . ?
C54 N8 C52 C53 -174.6(8) . . . . ?
C54 C55 C56 C57 -176.8(9) . . . . ?
C54 C55 C66 O7 -1.6(14) . . . . ?
C54 C55 C66 C65 179.2(9) . . . . ?
C55 C56 C57 C58 177.9(9) . . . . ?
C55 C56 C57 C64 -1.8(14) . . . . ?
C56 C55 C66 O7 177.7(8) . . . . ?
C56 C55 C66 C65 -1.5(13) . . . . ?
C56 C57 C58 C59 155.0(10) . . . . ?
C56 C57 C64 N9 178.1(9) . . . . ?
C56 C57 C64 C65 -2.5(13) . . . . ?
C57 C58 C59 C60 52.3(13) . . . . ?
C57 C64 C65 C63 -177.5(9) . . . . ?
C57 C64 C65 C66 4.6(13) . . . . ?
C58 C57 C64 N9 -1.6(13) . . . . ?
C58 C57 C64 C65 177.8(9) . . . . ?
C58 C59 C60 N9 -54.5(14) . . . . ?
C60 N9 C61A C62A 145.5(13) . . . . ?
C60 N9 C61B C62B -162.4(16) . . . . ?
C60 N9 C64 C57 -0.2(15) . . . . ?
C60 N9 C64 C65 -179.6(10) . . . . ?
C61A N9 C60 C59 -167.6(14) . . . . ?
C61A N9 C64 C57 -163.0(12) . . . . ?
C61A N9 C64 C65 17.7(17) . . . . ?
C61A C62A C63 C65 -47.9(18) . . . . ?
C61B N9 C60 C59 -145.5(14) . . . . ?
C61B N9 C64 C57 173.9(12) . . . . ?
C61B N9 C64 C65 -5.5(17) . . . . ?
C61B C62B C63 C65 36(2) . . . . ?
C62A C63 C65 C64 15.3(14) . . . . ?
C62A C63 C65 C66 -166.8(10) . . . . ?
C62B C63 C65 C64 -16.8(17) . . . . ?
C62B C63 C65 C66 161.1(13) . . . . ?
C63 C65 C66 O7 0.3(15) . . . . ?
C63 C65 C66 C55 179.5(9) . . . . ?
C64 N9 C60 C59 29.3(17) . . . . ?
C64 N9 C61A C62A -50.6(19) . . . . ?
C64 N9 C61B C62B 23(2) . . . . ?
C64 C57 C58 C59 -25.3(13) . . . . ?
C64 C65 C66 O7 178.2(9) . . . . ?
C64 C65 C66 C55 -2.6(14) . . . . ?
C66 C55 C56 C57 3.8(14) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 1479867'
_audit_update_record             
;
2016-07-27 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             2016-07-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H28 N3 O5 U, C H4 O, N O3'
_chemical_formula_sum            'C25 H32 N4 O9 U'
_chemical_formula_weight         770.57
_chemical_melting_point          ?
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.447(2)
_cell_length_b                   15.650(3)
_cell_length_c                   15.962(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.58(3)
_cell_angle_gamma                90
_cell_volume                     2677.0(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.902
_cell_measurement_theta_min      1.884
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.123
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44068
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.901
_diffrn_reflns_theta_min         1.884
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71074
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5689
_reflns_number_total             6353
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.370
_refine_diff_density_min         -3.251
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0258P)²+26.6349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C24-H5
 1.915356 with sigma of 0.02
 U1-H5
 3.059805 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C23) = Uanis(C24)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5A), C6(H6), C7(H7), C10(H10), C12(H12)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
U1 U 0.41141(2) 0.62367(2) 0.15999(2) 0.01696(6) Uani 1 1 d D . . . .
O1 O 0.4296(4) 0.7339(2) 0.1902(3) 0.0219(8) Uani 1 1 d . . . . .
O2 O 0.3902(4) 0.5157(2) 0.1220(3) 0.0227(8) Uani 1 1 d . . . . .
O3 O 0.4816(3) 0.5816(2) 0.3004(2) 0.0189(7) Uani 1 1 d . . . . .
O4 O 0.4503(4) 0.6641(3) 0.0253(3) 0.0299(9) Uani 1 1 d . . . . .
H4 H 0.492(8) 0.711(6) 0.016(6) 0.045 Uiso 1 1 d R . . . .
O5 O 0.6364(4) 0.6140(3) 0.1916(3) 0.0288(9) Uani 1 1 d D . . . .
H5 H 0.6874(17) 0.578(3) 0.225(4) 0.043 Uiso 1 1 d DR . . . .
N1 N 0.1925(4) 0.6541(3) 0.0406(3) 0.0200(9) Uani 1 1 d . . . . .
N2 N 0.2329(4) 0.6135(3) 0.2139(3) 0.0179(8) Uani 1 1 d . . . . .
N3 N 0.6481(4) 0.6168(3) 0.6165(3) 0.0221(9) Uani 1 1 d . . . . .
C1 C 0.1715(6) 0.6821(4) -0.0421(4) 0.0251(12) Uani 1 1 d . . . . .
H1 H 0.2384 0.7040 -0.0554 0.030 Uiso 1 1 calc R . . . .
C2 C 0.0540(6) 0.6803(4) -0.1102(4) 0.0283(13) Uani 1 1 d . . . . .
H2 H 0.0434 0.7024 -0.1664 0.034 Uiso 1 1 calc R . . . .
C3 C -0.0446(6) 0.6458(4) -0.0932(4) 0.0275(13) Uani 1 1 d . . . . .
H3 H -0.1224 0.6423 -0.1384 0.033 Uiso 1 1 calc R . . . .
C4 C -0.0281(5) 0.6149(3) -0.0054(4) 0.0232(11) Uani 1 1 d . . . . .
C5 C -0.1252(5) 0.5793(4) 0.0178(4) 0.0276(12) Uani 1 1 d . . . . .
H5A H -0.2046 0.5740 -0.0253 0.033 Uiso 1 1 calc R . . . .
C6 C -0.1034(5) 0.5522(4) 0.1034(4) 0.0256(12) Uani 1 1 d . . . . .
H6 H -0.1672 0.5266 0.1178 0.031 Uiso 1 1 calc R . . . .
C7 C 0.0163(5) 0.5630(3) 0.1706(4) 0.0217(11) Uani 1 1 d . . . . .
H7 H 0.0294 0.5455 0.2289 0.026 Uiso 1 1 calc R . . . .
C8 C 0.1125(5) 0.5988(3) 0.1505(3) 0.0188(10) Uani 1 1 d . . . . .
C9 C 0.0932(5) 0.6226(3) 0.0602(3) 0.0210(10) Uani 1 1 d . . . . .
C10 C 0.2402(5) 0.6338(3) 0.2957(4) 0.0192(10) Uani 1 1 d . . . . .
H10 H 0.1654 0.6471 0.3034 0.023 Uiso 1 1 calc R . . . .
C11 C 0.3488(5) 0.6376(3) 0.3729(3) 0.0178(10) Uani 1 1 d . . . . .
C12 C 0.3379(5) 0.6645(3) 0.4551(4) 0.0190(10) Uani 1 1 d . . . . .
H12 H 0.2614 0.6850 0.4545 0.023 Uiso 1 1 calc R . . . .
C13 C 0.4355(5) 0.6615(3) 0.5347(3) 0.0199(10) Uani 1 1 d . . . . .
C14 C 0.5528(5) 0.6259(3) 0.5367(3) 0.0188(10) Uani 1 1 d . . . . .
C15 C 0.4235(5) 0.6922(4) 0.6204(4) 0.0230(11) Uani 1 1 d . . . . .
H15A H 0.3366 0.6909 0.6154 0.028 Uiso 1 1 calc R . . . .
H15B H 0.4527 0.7508 0.6317 0.028 Uiso 1 1 calc R . . . .
C16 C 0.5001(6) 0.6357(4) 0.6977(4) 0.0267(12) Uani 1 1 d . . . . .
H16A H 0.4954 0.6575 0.7533 0.032 Uiso 1 1 calc R . . . .
H16B H 0.4664 0.5782 0.6889 0.032 Uiso 1 1 calc R . . . .
C17 C 0.6346(6) 0.6338(4) 0.7033(4) 0.0284(12) Uani 1 1 d . . . . .
H17A H 0.6732 0.6883 0.7260 0.034 Uiso 1 1 calc R . . . .
H17B H 0.6787 0.5899 0.7455 0.034 Uiso 1 1 calc R . . . .
C18 C 0.7701(5) 0.5839(4) 0.6227(4) 0.0243(7) Uani 1 1 d . . . . .
H18A H 0.7727 0.5230 0.6347 0.029 Uiso 1 1 calc R . . . .
H18B H 0.8335 0.6110 0.6730 0.029 Uiso 1 1 calc R . . . .
C19 C 0.8008(5) 0.5984(4) 0.5401(4) 0.0243(7) Uani 1 1 d . . . . .
H19A H 0.8770 0.5683 0.5450 0.029 Uiso 1 1 calc R . . . .
H19B H 0.8139 0.6589 0.5334 0.029 Uiso 1 1 calc R . . . .
C20 C 0.6913(5) 0.5654(4) 0.4569(4) 0.0243(7) Uani 1 1 d . . . . .
H20A H 0.7050 0.5829 0.4027 0.029 Uiso 1 1 calc R . . . .
H20B H 0.6894 0.5035 0.4580 0.029 Uiso 1 1 calc R . . . .
C21 C 0.5682(5) 0.6001(3) 0.4559(3) 0.0166(9) Uani 1 1 d . . . . .
C22 C 0.4681(5) 0.6071(3) 0.3752(3) 0.0167(10) Uani 1 1 d . . . . .
C23 C 0.4672(9) 0.6089(5) -0.0407(6) 0.0520(15) Uani 1 1 d . . . . .
H23A H 0.4652 0.6419 -0.0919 0.078 Uiso 1 1 calc GR . . . .
H23B H 0.4014 0.5672 -0.0584 0.078 Uiso 1 1 calc GR . . . .
H23C H 0.5462 0.5804 -0.0162 0.078 Uiso 1 1 calc GR . . . .
C24 C 0.7091(9) 0.6857(5) 0.1776(6) 0.0520(15) Uani 1 1 d D . . . .
H24A H 0.7122 0.6827 0.1183 0.078 Uiso 1 1 calc GR . . . .
H24B H 0.7924 0.6832 0.2207 0.078 Uiso 1 1 calc GR . . . .
H24C H 0.6706 0.7385 0.1845 0.078 Uiso 1 1 calc GR . . . .
O9 O 0.8185(4) 0.5132(3) 0.2827(3) 0.0346(10) Uani 1 1 d . . . . .
H9 H 0.8722 0.5403 0.3213 0.052 Uiso 1 1 calc GR . . . .
C25 C 0.8267(7) 0.4261(5) 0.3070(6) 0.0444(17) Uani 1 1 d . . . . .
H25A H 0.7563 0.3959 0.2669 0.067 Uiso 1 1 calc GR . . . .
H25B H 0.8271 0.4209 0.3671 0.067 Uiso 1 1 calc GR . . . .
H25C H 0.9022 0.4024 0.3037 0.067 Uiso 1 1 calc GR . . . .
O6 O 0.0588(5) 0.6955(4) 0.5021(4) 0.0423(12) Uani 1 1 d . . . . .
O7 O 0.0236(5) 0.5875(4) 0.4115(4) 0.0519(15) Uani 1 1 d . . . . .
O8 O -0.1055(6) 0.6945(4) 0.3807(4) 0.0518(14) Uani 1 1 d . . . . .
N4 N -0.0077(5) 0.6592(4) 0.4308(4) 0.0371(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
U1 O1 1.784(4) . ?
U1 O2 1.783(4) . ?
U1 O3 2.199(4) . ?
U1 O4 2.428(4) . ?
U1 O5 2.449(4) . ?
U1 N1 2.604(5) . ?
U1 N2 2.486(4) . ?
O3 C22 1.318(6) . ?
O4 H4 0.92(9) . ?
O4 C23 1.427(9) . ?
O5 H5 0.854(9) . ?
O5 C24 1.461(9) . ?
N1 C1 1.329(7) . ?
N1 C9 1.372(7) . ?
N2 C8 1.413(6) . ?
N2 C10 1.317(7) . ?
N3 C14 1.363(6) . ?
N3 C17 1.471(7) . ?
N3 C18 1.458(7) . ?
C1 H1 0.9300 . ?
C1 C2 1.402(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.362(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.431(8) . ?
C4 C5 1.404(9) . ?
C4 C9 1.421(7) . ?
C5 H5A 0.9300 . ?
C5 C6 1.368(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.422(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.371(8) . ?
C8 C9 1.428(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.411(7) . ?
C11 C12 1.423(7) . ?
C11 C22 1.436(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.367(7) . ?
C13 C14 1.444(8) . ?
C13 C15 1.501(7) . ?
C14 C21 1.420(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.521(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.511(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.497(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.559(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.505(8) . ?
C21 C22 1.396(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O9 H9 0.8200 . ?
O9 C25 1.411(8) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O6 N4 1.261(7) . ?
O7 N4 1.248(8) . ?
O8 N4 1.253(8) . ?

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
O1 U1 O3 92.74(16) . . ?
O1 U1 O4 86.96(17) . . ?
O1 U1 O5 89.39(17) . . ?
O1 U1 N1 90.68(16) . . ?
O1 U1 N2 90.02(16) . . ?
O2 U1 O1 176.08(17) . . ?
O2 U1 O3 91.17(16) . . ?
O2 U1 O4 89.48(17) . . ?
O2 U1 O5 91.10(17) . . ?
O2 U1 N1 86.76(16) . . ?
O2 U1 N2 91.56(16) . . ?
O3 U1 O4 149.94(15) . . ?
O3 U1 O5 77.91(14) . . ?
O3 U1 N1 135.53(15) . . ?
O3 U1 N2 71.22(14) . . ?
O4 U1 O5 72.04(15) . . ?
O4 U1 N1 74.51(15) . . ?
O4 U1 N2 138.81(15) . . ?
O5 U1 N1 146.50(15) . . ?
O5 U1 N2 149.05(14) . . ?
N2 U1 N1 64.45(15) . . ?
C22 O3 U1 135.7(3) . . ?
U1 O4 H4 129(5) . . ?
C23 O4 U1 127.6(4) . . ?
C23 O4 H4 99(5) . . ?
U1 O5 H5 127.6(17) . . ?
C24 O5 U1 122.4(4) . . ?
C24 O5 H5 107.8(16) . . ?
C1 N1 U1 125.3(4) . . ?
C1 N1 C9 118.0(5) . . ?
C9 N1 U1 115.3(3) . . ?
C8 N2 U1 118.4(3) . . ?
C10 N2 U1 123.7(3) . . ?
C10 N2 C8 117.1(5) . . ?
C14 N3 C17 123.1(5) . . ?
C14 N3 C18 122.2(5) . . ?
C18 N3 C17 114.5(4) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(6) . . ?
C2 C1 H1 118.2 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.3(6) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.7(5) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 123.2(5) . . ?
C5 C4 C9 120.0(5) . . ?
C9 C4 C3 116.8(6) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 C4 120.2(5) . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(6) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
N2 C8 C9 116.5(5) . . ?
C7 C8 N2 124.1(5) . . ?
C7 C8 C9 119.4(5) . . ?
N1 C9 C4 122.4(5) . . ?
N1 C9 C8 118.5(5) . . ?
C4 C9 C8 119.1(5) . . ?
N2 C10 H10 116.4 . . ?
N2 C10 C11 127.3(5) . . ?
C11 C10 H10 116.4 . . ?
C10 C11 C12 118.8(5) . . ?
C10 C11 C22 123.0(5) . . ?
C12 C11 C22 117.8(5) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 C11 122.6(5) . . ?
C13 C12 H12 118.7 . . ?
C12 C13 C14 118.9(5) . . ?
C12 C13 C15 122.0(5) . . ?
C14 C13 C15 119.1(5) . . ?
N3 C14 C13 119.6(5) . . ?
N3 C14 C21 120.3(5) . . ?
C21 C14 C13 120.1(5) . . ?
C13 C15 H15A 109.7 . . ?
C13 C15 H15B 109.7 . . ?
C13 C15 C16 110.0(5) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C17 C16 C15 110.1(5) . . ?
C17 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
N3 C17 C16 113.0(5) . . ?
N3 C17 H17A 109.0 . . ?
N3 C17 H17B 109.0 . . ?
C16 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N3 C18 H18A 108.8 . . ?
N3 C18 H18B 108.8 . . ?
N3 C18 C19 113.8(4) . . ?
H18A C18 H18B 107.7 . . ?
C19 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
C18 C19 C20 109.4(5) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 C19 111.0(5) . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C14 C21 C20 120.6(5) . . ?
C22 C21 C14 119.5(5) . . ?
C22 C21 C20 120.0(5) . . ?
O3 C22 C11 119.5(4) . . ?
O3 C22 C21 119.5(5) . . ?
C21 C22 C11 120.9(5) . . ?
O4 C23 H23A 109.5 . . ?
O4 C23 H23B 109.5 . . ?
O4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O5 C24 H24A 109.5 . . ?
O5 C24 H24B 109.5 . . ?
O5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 O9 H9 109.5 . . ?
O9 C25 H25A 109.5 . . ?
O9 C25 H25B 109.5 . . ?
O9 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O7 N4 O6 119.5(6) . . ?
O7 N4 O8 120.6(6) . . ?
O8 N4 O6 119.9(6) . . ?

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
U1 O3 C22 C11 37.8(7) . . . . ?
U1 O3 C22 C21 -145.2(4) . . . . ?
U1 N1 C1 C2 165.7(4) . . . . ?
U1 N1 C9 C4 -164.3(4) . . . . ?
U1 N1 C9 C8 17.2(6) . . . . ?
U1 N2 C8 C7 156.2(4) . . . . ?
U1 N2 C8 C9 -23.1(6) . . . . ?
U1 N2 C10 C11 -21.9(7) . . . . ?
N1 C1 C2 C3 -2.3(9) . . . . ?
N2 C8 C9 N1 2.8(7) . . . . ?
N2 C8 C9 C4 -175.7(4) . . . . ?
N2 C10 C11 C12 177.4(5) . . . . ?
N2 C10 C11 C22 -9.5(8) . . . . ?
N3 C14 C21 C20 -2.3(7) . . . . ?
N3 C14 C21 C22 177.7(5) . . . . ?
N3 C18 C19 C20 -51.4(6) . . . . ?
C1 N1 C9 C4 3.5(8) . . . . ?
C1 N1 C9 C8 -175.0(5) . . . . ?
C1 C2 C3 C4 2.4(8) . . . . ?
C2 C3 C4 C5 179.3(5) . . . . ?
C2 C3 C4 C9 0.2(8) . . . . ?
C3 C4 C5 C6 -178.9(5) . . . . ?
C3 C4 C9 N1 -3.2(8) . . . . ?
C3 C4 C9 C8 175.3(5) . . . . ?
C4 C5 C6 C7 2.5(8) . . . . ?
C5 C4 C9 N1 177.6(5) . . . . ?
C5 C4 C9 C8 -3.9(8) . . . . ?
C5 C6 C7 C8 -1.5(8) . . . . ?
C6 C7 C8 N2 178.4(5) . . . . ?
C6 C7 C8 C9 -2.3(8) . . . . ?
C7 C8 C9 N1 -176.5(5) . . . . ?
C7 C8 C9 C4 4.9(7) . . . . ?
C8 N2 C10 C11 168.8(5) . . . . ?
C9 N1 C1 C2 -0.7(8) . . . . ?
C9 C4 C5 C6 0.2(8) . . . . ?
C10 N2 C8 C7 -33.9(7) . . . . ?
C10 N2 C8 C9 146.8(5) . . . . ?
C10 C11 C12 C13 172.9(5) . . . . ?
C10 C11 C22 O3 6.8(7) . . . . ?
C10 C11 C22 C21 -170.1(5) . . . . ?
C11 C12 C13 C14 -3.1(8) . . . . ?
C11 C12 C13 C15 178.4(5) . . . . ?
C12 C11 C22 O3 180.0(4) . . . . ?
C12 C11 C22 C21 3.1(7) . . . . ?
C12 C13 C14 N3 -175.3(5) . . . . ?
C12 C13 C14 C21 4.4(8) . . . . ?
C12 C13 C15 C16 143.8(5) . . . . ?
C13 C14 C21 C20 178.0(5) . . . . ?
C13 C14 C21 C22 -1.9(7) . . . . ?
C13 C15 C16 C17 56.4(6) . . . . ?
C14 N3 C17 C16 17.5(8) . . . . ?
C14 N3 C18 C19 26.1(7) . . . . ?
C14 C13 C15 C16 -34.7(7) . . . . ?
C14 C21 C22 O3 -178.7(4) . . . . ?
C14 C21 C22 C11 -1.8(7) . . . . ?
C15 C13 C14 N3 3.3(7) . . . . ?
C15 C13 C14 C21 -177.1(5) . . . . ?
C15 C16 C17 N3 -48.6(6) . . . . ?
C17 N3 C14 C13 6.2(8) . . . . ?
C17 N3 C14 C21 -173.5(5) . . . . ?
C17 N3 C18 C19 -157.6(5) . . . . ?
C18 N3 C14 C13 -177.9(5) . . . . ?
C18 N3 C14 C21 2.5(8) . . . . ?
C18 N3 C17 C16 -158.7(5) . . . . ?
C18 C19 C20 C21 50.1(6) . . . . ?
C19 C20 C21 C14 -24.7(7) . . . . ?
C19 C20 C21 C22 155.3(5) . . . . ?
C20 C21 C22 O3 1.3(7) . . . . ?
C20 C21 C22 C11 178.2(5) . . . . ?
C22 C11 C12 C13 -0.6(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
