#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/38/4303886.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303886
loop_
_publ_author_name
'Michael F. Schettini'
'Guang Wu'
'Trevor W. Hayton'
_publ_section_title
;
Coordination of N-Donor Ligands to a Uranyl(V) β-Diketiminate Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11799
_journal_page_last               11808
_journal_paper_doi               10.1021/ic9018508
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C42.5 H53 N4 O2 U'
_chemical_formula_weight         889.92
_chemical_name_systematic
; 
 Uranyl(V) Ar2nacnac bipyridine 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.795(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.084(3)
_cell_length_b                   13.7180(14)
_cell_length_c                   16.9070(16)
_cell_measurement_temperature    150(2)
_cell_volume                     8092.7(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30823
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            Inidgo
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.188
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8368
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0804P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                5480
_reflns_number_total             8368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9018508_si_001_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8092.6(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C42.50 H53 N4 O2 U'
_cod_database_code               4303886
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.838184(8) 0.69473(2) 0.908484(15) 0.03700(12) Uani 1 1 d . . .
N4 N 0.76728(18) 0.6998(5) 0.9095(4) 0.0369(15) Uani 1 1 d . . .
N1 N 0.85990(18) 0.8038(5) 0.8158(4) 0.0383(15) Uani 1 1 d . . .
O1 O 0.81610(16) 0.6112(4) 0.8208(3) 0.0494(15) Uani 1 1 d . . .
O2 O 0.85682(17) 0.7781(4) 0.9968(3) 0.0497(15) Uani 1 1 d . . .
N3 N 0.81941(19) 0.5854(5) 1.0173(3) 0.0426(16) Uani 1 1 d . . .
C16 C 0.8866(2) 0.7975(7) 0.7807(5) 0.048(2) Uani 1 1 d . . .
C14 C 0.9232(2) 0.6506(7) 0.8646(5) 0.048(2) Uani 1 1 d . . .
N2 N 0.90343(19) 0.6364(6) 0.9160(4) 0.0467(17) Uani 1 1 d . . .
C35 C 0.7537(2) 0.6333(6) 0.9512(4) 0.0389(18) Uani 1 1 d . . .
C18 C 0.8326(2) 0.8820(6) 0.7955(4) 0.0384(19) Uani 1 1 d . . .
C34 C 0.7832(2) 0.5769(6) 1.0173(4) 0.0385(18) Uani 1 1 d . . .
C15 C 0.9144(3) 0.7207(8) 0.8014(5) 0.057(3) Uani 1 1 d . . .
H15 H 0.9291 0.7170 0.7665 0.069 Uiso 1 1 calc R . .
C19 C 0.7980(2) 0.8709(6) 0.7265(5) 0.0420(19) Uani 1 1 d . . .
C13 C 0.9591(3) 0.5905(9) 0.8756(6) 0.072(3) Uani 1 1 d . . .
H13A H 0.9720 0.5781 0.9343 0.108 Uiso 1 1 calc R . .
H13B H 0.9758 0.6258 0.8532 0.108 Uiso 1 1 calc R . .
H13C H 0.9520 0.5298 0.8463 0.108 Uiso 1 1 calc R . .
C36 C 0.7148(2) 0.6195(7) 0.9359(5) 0.045(2) Uani 1 1 d . . .
H36 H 0.7065 0.5719 0.9650 0.055 Uiso 1 1 calc R . .
C37 C 0.6885(3) 0.6777(7) 0.8768(5) 0.055(2) Uani 1 1 d . . .
H37 H 0.6623 0.6703 0.8659 0.065 Uiso 1 1 calc R . .
C20 C 0.7699(2) 0.9428(7) 0.7129(5) 0.050(2) Uani 1 1 d . . .
H20 H 0.7472 0.9370 0.6674 0.060 Uiso 1 1 calc R . .
C24 C 0.7916(3) 0.7880(7) 0.6646(5) 0.052(2) Uani 1 1 d . . .
H24 H 0.811(3) 0.738(7) 0.689(6) 0.062 Uiso 1 1 calc . . .
C30 C 0.8477(3) 0.5419(7) 1.0809(5) 0.055(2) Uani 1 1 d . . .
H30 H 0.8728 0.5482 1.0821 0.066 Uiso 1 1 calc R . .
C28 C 0.8725(3) 1.0139(8) 1.0009(6) 0.075(3) Uani 1 1 d . . .
H28A H 0.8595 1.0755 0.9935 0.112 Uiso 1 1 calc R . .
H28B H 0.8975 1.0203 1.0429 0.112 Uiso 1 1 calc R . .
H28C H 0.8580 0.9660 1.0186 0.112 Uiso 1 1 calc R . .
C31 C 0.8408(3) 0.4882(7) 1.1443(5) 0.057(2) Uani 1 1 d . . .
H31 H 0.8608 0.4587 1.1865 0.068 Uiso 1 1 calc R . .
C1 C 0.9176(2) 0.5677(8) 0.9847(5) 0.055(3) Uani 1 1 d . . .
C23 C 0.8382(2) 0.9643(7) 0.8474(5) 0.049(2) Uani 1 1 d . . .
C21 C 0.7750(3) 1.0222(7) 0.7655(6) 0.055(2) Uani 1 1 d . . .
H21 H 0.7558 1.0685 0.7564 0.065 Uiso 1 1 calc R . .
C33 C 0.7748(3) 0.5240(7) 1.0793(5) 0.052(2) Uani 1 1 d . . .
H33 H 0.7496 0.5183 1.0775 0.062 Uiso 1 1 calc R . .
C22 C 0.8094(3) 1.0328(7) 0.8326(6) 0.055(2) Uani 1 1 d . . .
H22 H 0.8129 1.0867 0.8677 0.066 Uiso 1 1 calc R . .
C39 C 0.7407(3) 0.7551(7) 0.8523(5) 0.048(2) Uani 1 1 d . . .
H39 H 0.7493 0.8021 0.8232 0.057 Uiso 1 1 calc R . .
C27 C 0.8767(3) 0.9822(8) 0.9178(6) 0.060(3) Uani 1 1 d . . .
H27 H 0.891(3) 0.921(7) 0.928(6) 0.072 Uiso 1 1 calc . . .
C6 C 0.9391(3) 0.6019(10) 1.0637(6) 0.067(3) Uani 1 1 d . . .
C10 C 0.9493(3) 0.7074(11) 1.0783(6) 0.081(4) Uani 1 1 d . . .
H10 H 0.935(4) 0.742(9) 1.027(7) 0.097 Uiso 1 1 calc . . .
C17 C 0.8905(3) 0.8729(9) 0.7187(6) 0.077(3) Uani 1 1 d . . .
H17A H 0.8686 0.9154 0.7033 0.116 Uiso 1 1 calc R . .
H17B H 0.8919 0.8408 0.6694 0.116 Uiso 1 1 calc R . .
H17C H 0.9134 0.9103 0.7441 0.116 Uiso 1 1 calc R . .
C2 C 0.9071(3) 0.4685(8) 0.9722(7) 0.068(3) Uani 1 1 d . . .
C32 C 0.8035(3) 0.4803(7) 1.1427(5) 0.057(2) Uani 1 1 d . . .
H32 H 0.7980 0.4455 1.1844 0.069 Uiso 1 1 calc R . .
C38 C 0.7019(3) 0.7464(7) 0.8346(5) 0.053(2) Uani 1 1 d . . .
H38 H 0.6850 0.7864 0.7947 0.063 Uiso 1 1 calc R . .
C25 C 0.7516(3) 0.7415(9) 0.6432(6) 0.070(3) Uani 1 1 d . . .
H25A H 0.7487 0.7156 0.6934 0.105 Uiso 1 1 calc R . .
H25B H 0.7490 0.6899 0.6032 0.105 Uiso 1 1 calc R . .
H25C H 0.7323 0.7900 0.6195 0.105 Uiso 1 1 calc R . .
C7 C 0.8820(3) 0.4256(9) 0.8893(7) 0.075(3) Uani 1 1 d . . .
H7 H 0.874(3) 0.480(8) 0.850(7) 0.090 Uiso 1 1 calc . . .
C5 C 0.9520(3) 0.5394(13) 1.1332(7) 0.090(4) Uani 1 1 d . . .
H5 H 0.9664 0.5636 1.1859 0.108 Uiso 1 1 calc R . .
C3 C 0.9211(4) 0.4060(10) 1.0438(9) 0.091(4) Uani 1 1 d . . .
H3 H 0.9155 0.3398 1.0378 0.109 Uiso 1 1 calc R . .
C4 C 0.9432(4) 0.4424(14) 1.1227(9) 0.104(5) Uani 1 1 d . . .
H4 H 0.9518 0.4003 1.1683 0.125 Uiso 1 1 calc R . .
C29 C 0.8993(4) 1.0604(11) 0.8868(8) 0.110(5) Uani 1 1 d . . .
H29A H 0.8862 1.1218 0.8804 0.165 Uiso 1 1 calc R . .
H29B H 0.9010 1.0407 0.8337 0.165 Uiso 1 1 calc R . .
H29C H 0.9246 1.0670 0.9272 0.165 Uiso 1 1 calc R . .
C26 C 0.7956(4) 0.8206(9) 0.5819(7) 0.093(4) Uani 1 1 d . . .
H26A H 0.7809 0.8789 0.5628 0.140 Uiso 1 1 calc R . .
H26B H 0.7863 0.7701 0.5407 0.140 Uiso 1 1 calc R . .
H26C H 0.8221 0.8332 0.5901 0.140 Uiso 1 1 calc R . .
C12 C 0.9922(4) 0.7267(15) 1.0928(9) 0.136(7) Uani 1 1 d . . .
H12A H 1.0076 0.6960 1.1442 0.204 Uiso 1 1 calc R . .
H12B H 0.9969 0.7956 1.0965 0.204 Uiso 1 1 calc R . .
H12C H 0.9987 0.7004 1.0467 0.204 Uiso 1 1 calc R . .
C11 C 0.9392(4) 0.7553(12) 1.1514(7) 0.102(4) Uani 1 1 d . . .
H11A H 0.9126 0.7445 1.1432 0.154 Uiso 1 1 calc R . .
H11B H 0.9441 0.8241 1.1523 0.154 Uiso 1 1 calc R . .
H11C H 0.9546 0.7269 1.2038 0.154 Uiso 1 1 calc R . .
C9 C 0.9033(4) 0.3524(11) 0.8508(11) 0.120(5) Uani 1 1 d . . .
H9A H 0.9288 0.3756 0.8596 0.181 Uiso 1 1 calc R . .
H9B H 0.8897 0.3462 0.7916 0.181 Uiso 1 1 calc R . .
H9C H 0.9046 0.2900 0.8773 0.181 Uiso 1 1 calc R . .
C8 C 0.8457(3) 0.3796(10) 0.8950(8) 0.095(4) Uani 1 1 d . . .
H8A H 0.8423 0.3990 0.9465 0.142 Uiso 1 1 calc R . .
H8B H 0.8477 0.3099 0.8936 0.142 Uiso 1 1 calc R . .
H8C H 0.8241 0.4008 0.8483 0.142 Uiso 1 1 calc R . .
C41 C 0.0036(5) 0.9164(19) 0.8382(7) 0.236(12) Uiso 1 1 d D . .
C43 C 0.0029(9) 0.9969(19) 0.7924(7) 0.313(18) Uiso 1 1 d D . .
H43 H 0.0066 1.0567 0.8199 0.375 Uiso 1 1 calc R . .
C42 C 0.0022(6) 0.8320(19) 0.7916(6) 0.317(19) Uiso 1 1 d D . .
H42 H 0.0042 0.7723 0.8188 0.381 Uiso 1 1 calc R . .
C40 C 0.0067(9) 0.903(3) 0.9191(12) 0.164(14) Uiso 0.50 1 d PD . .
H40A H 0.0269 0.8571 0.9447 0.247 Uiso 0.50 1 calc PR . .
H40B H -0.0171 0.8780 0.9218 0.247 Uiso 0.50 1 calc PR . .
H40C H 0.0125 0.9639 0.9486 0.247 Uiso 0.50 1 calc PR . .
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'
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 U1 O1 175.9(2) . . ?
O2 U1 N1 91.4(2) . . ?
O1 U1 N1 91.0(2) . . ?
O2 U1 N2 93.8(3) . . ?
O1 U1 N2 90.0(2) . . ?
N1 U1 N2 73.3(2) . . ?
O2 U1 N4 94.6(2) . . ?
O1 U1 N4 81.3(2) . . ?
N1 U1 N4 121.6(2) . . ?
N2 U1 N4 162.6(2) . . ?
O2 U1 N3 84.4(2) . . ?
O1 U1 N3 93.3(2) . . ?
N1 U1 N3 175.4(2) . . ?
N2 U1 N3 105.1(2) . . ?
N4 U1 N3 60.78(19) . . ?
O2 U1 C18 85.1(2) . . ?
O1 U1 C18 95.7(2) . . ?
N1 U1 C18 26.01(19) . . ?
N2 U1 C18 98.8(2) . . ?
N4 U1 C18 96.98(18) . . ?
N3 U1 C18 154.39(19) . . ?
O2 U1 C1 88.3(3) . . ?
O1 U1 C1 94.7(3) . . ?
N1 U1 C1 97.4(2) . . ?
N2 U1 C1 24.6(2) . . ?
N4 U1 C1 140.8(2) . . ?
N3 U1 C1 80.7(2) . . ?
C18 U1 C1 122.2(2) . . ?
C35 N4 C39 116.2(7) . . ?
C35 N4 U1 122.3(5) . . ?
C39 N4 U1 119.7(5) . . ?
C16 N1 C18 121.2(7) . . ?
C16 N1 U1 134.1(6) . . ?
C18 N1 U1 104.4(4) . . ?
C34 N3 C30 117.6(6) . . ?
C34 N3 U1 123.1(5) . . ?
C30 N3 U1 119.0(5) . . ?
N1 C16 C15 121.8(8) . . ?
N1 C16 C17 121.9(8) . . ?
C15 C16 C17 116.3(7) . . ?
N2 C14 C15 124.5(8) . . ?
N2 C14 C13 119.6(8) . . ?
C15 C14 C13 115.8(7) . . ?
C14 N2 C1 119.4(7) . . ?
C14 N2 U1 131.0(6) . . ?
C1 N2 U1 109.2(4) . . ?
N4 C35 C36 122.8(7) . . ?
N4 C35 C34 115.8(7) . . ?
C36 C35 C34 121.4(7) . . ?
C23 C18 C19 120.1(7) . . ?
C23 C18 N1 120.7(7) . . ?
C19 C18 N1 119.0(7) . . ?
C23 C18 U1 108.1(5) . . ?
C19 C18 U1 105.3(5) . . ?
N1 C18 U1 49.6(3) . . ?
N3 C34 C33 121.3(7) . . ?
N3 C34 C35 115.7(6) . . ?
C33 C34 C35 122.8(7) . . ?
C14 C15 C16 131.1(7) . . ?
C14 C15 H15 114.4 . . ?
C16 C15 H15 114.4 . . ?
C20 C19 C18 118.5(8) . . ?
C20 C19 C24 119.0(8) . . ?
C18 C19 C24 122.4(7) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C35 C36 C37 119.2(8) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C38 C37 C36 118.5(8) . . ?
C38 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C21 C20 C19 121.2(8) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C19 C24 C26 112.1(8) . . ?
C19 C24 C25 112.9(8) . . ?
C26 C24 C25 106.9(8) . . ?
C19 C24 H24 108(5) . . ?
C26 C24 H24 108(5) . . ?
C25 C24 H24 108(6) . . ?
N3 C30 C31 123.2(8) . . ?
N3 C30 H30 118.4 . . ?
C31 C30 H30 118.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C31 C30 118.1(8) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
C6 C1 C2 120.7(10) . . ?
C6 C1 N2 119.1(10) . . ?
C2 C1 N2 120.0(8) . . ?
C6 C1 U1 110.3(6) . . ?
C2 C1 U1 106.7(6) . . ?
N2 C1 U1 46.2(3) . . ?
C22 C23 C18 119.6(8) . . ?
C22 C23 C27 119.4(8) . . ?
C18 C23 C27 120.9(8) . . ?
C20 C21 C22 119.7(8) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C32 C33 C34 120.5(8) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C23 C22 C21 120.9(9) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N4 C39 C38 124.2(8) . . ?
N4 C39 H39 117.9 . . ?
C38 C39 H39 117.9 . . ?
C28 C27 C23 113.6(8) . . ?
C28 C27 C29 110.3(9) . . ?
C23 C27 C29 108.2(9) . . ?
C28 C27 H27 108(6) . . ?
C23 C27 H27 108(6) . . ?
C29 C27 H27 108(6) . . ?
C1 C6 C5 121.6(13) . . ?
C1 C6 C10 121.2(9) . . ?
C5 C6 C10 117.3(11) . . ?
C6 C10 C12 112.4(12) . . ?
C6 C10 C11 115.1(11) . . ?
C12 C10 C11 108.3(10) . . ?
C6 C10 H10 107(7) . . ?
C12 C10 H10 107(7) . . ?
C11 C10 H10 107(7) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C2 C3 116.6(11) . . ?
C1 C2 C7 124.4(10) . . ?
C3 C2 C7 119.0(12) . . ?
C33 C32 C31 119.3(8) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C39 C38 C37 119.0(8) . . ?
C39 C38 H38 120.5 . . ?
C37 C38 H38 120.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C2 C7 C8 112.5(10) . . ?
C2 C7 C9 113.7(10) . . ?
C8 C7 C9 110.2(11) . . ?
C2 C7 H7 107(7) . . ?
C8 C7 H7 107(7) . . ?
C9 C7 H7 107(7) . . ?
C4 C5 C6 119.1(13) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C4 C3 C2 121.4(13) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 120.6(12) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C40 C41 C43 133(2) . . ?
C40 C41 C42 116(2) . . ?
C43 C41 C42 111.6(12) . . ?
C41 C43 C43 124.5(7) . 2_556 ?
C41 C43 H43 117.8 . . ?
C43 C43 H43 117.7 2_556 . ?
C42 C42 C41 123.6(7) 2_556 . ?
C42 C42 H42 118.2 2_556 . ?
C41 C42 H42 118.2 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.4 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.821(5) . ?
U1 O1 1.833(5) . ?
U1 N1 2.490(6) . ?
U1 N2 2.510(6) . ?
U1 N4 2.636(6) . ?
U1 N3 2.643(6) . ?
U1 C18 3.166(8) . ?
U1 C1 3.285(8) . ?
N4 C35 1.349(10) . ?
N4 C39 1.356(10) . ?
N1 C16 1.318(10) . ?
N1 C18 1.434(10) . ?
N3 C34 1.348(9) . ?
N3 C30 1.359(10) . ?
C16 C15 1.432(12) . ?
C16 C17 1.513(12) . ?
C14 N2 1.327(10) . ?
C14 C15 1.392(13) . ?
C14 C13 1.522(11) . ?
N2 C1 1.449(11) . ?
C35 C36 1.390(11) . ?
C35 C34 1.487(10) . ?
C18 C23 1.402(11) . ?
C18 C19 1.421(10) . ?
C34 C33 1.394(11) . ?
C15 H15 0.9300 . ?
C19 C20 1.397(12) . ?
C19 C24 1.508(12) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C36 C37 1.390(12) . ?
C36 H36 0.9300 . ?
C37 C38 1.373(13) . ?
C37 H37 0.9300 . ?
C20 C21 1.378(12) . ?
C20 H20 0.9300 . ?
C24 C26 1.522(13) . ?
C24 C25 1.540(14) . ?
C24 H24 0.98(10) . ?
C30 C31 1.394(11) . ?
C30 H30 0.9300 . ?
C28 C27 1.529(12) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 C32 1.377(12) . ?
C31 H31 0.9300 . ?
C1 C6 1.385(13) . ?
C1 C2 1.412(14) . ?
C23 C22 1.380(12) . ?
C23 C27 1.539(13) . ?
C21 C22 1.397(13) . ?
C21 H21 0.9300 . ?
C33 C32 1.367(12) . ?
C33 H33 0.9300 . ?
C22 H22 0.9300 . ?
C39 C38 1.370(12) . ?
C39 H39 0.9300 . ?
C27 C29 1.557(15) . ?
C27 H27 0.98(10) . ?
C6 C5 1.402(15) . ?
C6 C10 1.495(16) . ?
C10 C12 1.548(16) . ?
C10 C11 1.555(16) . ?
C10 H10 0.98(12) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C2 C3 1.430(15) . ?
C2 C7 1.513(15) . ?
C32 H32 0.9300 . ?
C38 H38 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C7 C8 1.520(16) . ?
C7 C9 1.551(15) . ?
C7 H7 0.98(11) . ?
C5 C4 1.367(19) . ?
C5 H5 0.9300 . ?
C3 C4 1.399(19) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C41 C40 1.347(14) . ?
C41 C43 1.344(12) . ?
C41 C42 1.391(12) . ?
C43 C43 1.375(16) 2_556 ?
C43 H43 0.9300 . ?
C42 C42 1.360(17) 2_556 ?
C42 H42 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 U1 N4 C35 -94.0(6) . . . . ?
O1 U1 N4 C35 85.7(6) . . . . ?
N1 U1 N4 C35 171.5(5) . . . . ?
N2 U1 N4 C35 24.9(9) . . . . ?
N3 U1 N4 C35 -13.0(5) . . . . ?
C18 U1 N4 C35 -179.5(5) . . . . ?
C1 U1 N4 C35 -1.0(7) . . . . ?
O2 U1 N4 C39 101.7(6) . . . . ?
O1 U1 N4 C39 -78.6(6) . . . . ?
N1 U1 N4 C39 7.2(7) . . . . ?
N2 U1 N4 C39 -139.5(7) . . . . ?
N3 U1 N4 C39 -177.4(6) . . . . ?
C18 U1 N4 C39 16.1(6) . . . . ?
C1 U1 N4 C39 -165.3(6) . . . . ?
O2 U1 N1 C16 111.1(8) . . . . ?
O1 U1 N1 C16 -72.2(8) . . . . ?
N2 U1 N1 C16 17.5(7) . . . . ?
N4 U1 N1 C16 -152.6(7) . . . . ?
N3 U1 N1 C16 87(3) . . . . ?
C18 U1 N1 C16 -173.2(10) . . . . ?
C1 U1 N1 C16 22.6(8) . . . . ?
O2 U1 N1 C18 -75.7(5) . . . . ?
O1 U1 N1 C18 101.0(5) . . . . ?
N2 U1 N1 C18 -169.3(5) . . . . ?
N4 U1 N1 C18 20.6(5) . . . . ?
N3 U1 N1 C18 -100(2) . . . . ?
C1 U1 N1 C18 -164.2(5) . . . . ?
O2 U1 N3 C34 104.5(6) . . . . ?
O1 U1 N3 C34 -72.1(6) . . . . ?
N1 U1 N3 C34 129(2) . . . . ?
N2 U1 N3 C34 -163.0(6) . . . . ?
N4 U1 N3 C34 6.0(5) . . . . ?
C18 U1 N3 C34 38.4(8) . . . . ?
C1 U1 N3 C34 -166.3(6) . . . . ?
O2 U1 N3 C30 -69.7(6) . . . . ?
O1 U1 N3 C30 113.7(6) . . . . ?
N1 U1 N3 C30 -46(3) . . . . ?
N2 U1 N3 C30 22.8(6) . . . . ?
N4 U1 N3 C30 -168.2(7) . . . . ?
C18 U1 N3 C30 -135.8(6) . . . . ?
C1 U1 N3 C30 19.5(6) . . . . ?
C18 N1 C16 C15 179.0(8) . . . . ?
U1 N1 C16 C15 -8.8(13) . . . . ?
C18 N1 C16 C17 1.2(13) . . . . ?
U1 N1 C16 C17 173.5(7) . . . . ?
C15 C14 N2 C1 -173.9(9) . . . . ?
C13 C14 N2 C1 3.4(13) . . . . ?
C15 C14 N2 U1 14.4(14) . . . . ?
C13 C14 N2 U1 -168.2(7) . . . . ?
O2 U1 N2 C14 -110.3(8) . . . . ?
O1 U1 N2 C14 71.1(8) . . . . ?
N1 U1 N2 C14 -19.9(8) . . . . ?
N4 U1 N2 C14 130.8(8) . . . . ?
N3 U1 N2 C14 164.5(8) . . . . ?
C18 U1 N2 C14 -24.7(9) . . . . ?
C1 U1 N2 C14 172.3(12) . . . . ?
O2 U1 N2 C1 77.5(6) . . . . ?
O1 U1 N2 C1 -101.1(6) . . . . ?
N1 U1 N2 C1 167.8(6) . . . . ?
N4 U1 N2 C1 -41.5(9) . . . . ?
N3 U1 N2 C1 -7.7(6) . . . . ?
C18 U1 N2 C1 163.1(6) . . . . ?
C39 N4 C35 C36 1.5(11) . . . . ?
U1 N4 C35 C36 -163.3(6) . . . . ?
C39 N4 C35 C34 -176.6(6) . . . . ?
U1 N4 C35 C34 18.5(8) . . . . ?
C16 N1 C18 C23 -97.5(9) . . . . ?
U1 N1 C18 C23 88.2(7) . . . . ?
C16 N1 C18 C19 88.6(9) . . . . ?
U1 N1 C18 C19 -85.7(6) . . . . ?
C16 N1 C18 U1 174.3(9) . . . . ?
O2 U1 C18 C23 -11.8(5) . . . . ?
O1 U1 C18 C23 164.1(5) . . . . ?
N1 U1 C18 C23 -115.3(7) . . . . ?
N2 U1 C18 C23 -104.9(5) . . . . ?
N4 U1 C18 C23 82.3(5) . . . . ?
N3 U1 C18 C23 54.2(7) . . . . ?
C1 U1 C18 C23 -96.7(5) . . . . ?
O2 U1 C18 C19 -141.3(5) . . . . ?
O1 U1 C18 C19 34.7(5) . . . . ?
N1 U1 C18 C19 115.2(7) . . . . ?
N2 U1 C18 C19 125.6(5) . . . . ?
N4 U1 C18 C19 -47.2(5) . . . . ?
N3 U1 C18 C19 -75.3(7) . . . . ?
C1 U1 C18 C19 133.9(5) . . . . ?
O2 U1 C18 N1 103.5(5) . . . . ?
O1 U1 C18 N1 -80.6(5) . . . . ?
N2 U1 C18 N1 10.4(5) . . . . ?
N4 U1 C18 N1 -162.4(5) . . . . ?
N3 U1 C18 N1 169.5(5) . . . . ?
C1 U1 C18 N1 18.6(5) . . . . ?
C30 N3 C34 C33 -1.2(12) . . . . ?
U1 N3 C34 C33 -175.5(6) . . . . ?
C30 N3 C34 C35 174.5(7) . . . . ?
U1 N3 C34 C35 0.2(9) . . . . ?
N4 C35 C34 N3 -11.9(10) . . . . ?
C36 C35 C34 N3 169.9(7) . . . . ?
N4 C35 C34 C33 163.7(7) . . . . ?
C36 C35 C34 C33 -14.5(11) . . . . ?
N2 C14 C15 C16 6.8(18) . . . . ?
C13 C14 C15 C16 -170.6(10) . . . . ?
N1 C16 C15 C14 -10.0(16) . . . . ?
C17 C16 C15 C14 167.8(10) . . . . ?
C23 C18 C19 C20 -0.8(11) . . . . ?
N1 C18 C19 C20 173.2(6) . . . . ?
U1 C18 C19 C20 121.2(6) . . . . ?
C23 C18 C19 C24 175.1(7) . . . . ?
N1 C18 C19 C24 -10.9(11) . . . . ?
U1 C18 C19 C24 -62.9(8) . . . . ?
N4 C35 C36 C37 -1.6(12) . . . . ?
C34 C35 C36 C37 176.5(7) . . . . ?
C35 C36 C37 C38 0.7(12) . . . . ?
C18 C19 C20 C21 -1.1(11) . . . . ?
C24 C19 C20 C21 -177.2(8) . . . . ?
C20 C19 C24 C26 72.7(11) . . . . ?
C18 C19 C24 C26 -103.2(10) . . . . ?
C20 C19 C24 C25 -48.0(11) . . . . ?
C18 C19 C24 C25 136.1(8) . . . . ?
C34 N3 C30 C31 1.1(13) . . . . ?
U1 N3 C30 C31 175.7(7) . . . . ?
N3 C30 C31 C32 -0.9(14) . . . . ?
C14 N2 C1 C6 95.8(10) . . . . ?
U1 N2 C1 C6 -90.9(8) . . . . ?
C14 N2 C1 C2 -88.7(11) . . . . ?
U1 N2 C1 C2 84.6(8) . . . . ?
C14 N2 C1 U1 -173.3(10) . . . . ?
O2 U1 C1 C6 8.4(7) . . . . ?
O1 U1 C1 C6 -168.7(7) . . . . ?
N1 U1 C1 C6 99.6(7) . . . . ?
N2 U1 C1 C6 111.4(10) . . . . ?
N4 U1 C1 C6 -86.8(8) . . . . ?
N3 U1 C1 C6 -76.2(7) . . . . ?
C18 U1 C1 C6 91.5(7) . . . . ?
O2 U1 C1 C2 141.2(6) . . . . ?
O1 U1 C1 C2 -36.0(6) . . . . ?
N1 U1 C1 C2 -127.6(6) . . . . ?
N2 U1 C1 C2 -115.8(9) . . . . ?
N4 U1 C1 C2 45.9(7) . . . . ?
N3 U1 C1 C2 56.6(6) . . . . ?
C18 U1 C1 C2 -135.7(6) . . . . ?
O2 U1 C1 N2 -103.0(6) . . . . ?
O1 U1 C1 N2 79.9(6) . . . . ?
N1 U1 C1 N2 -11.8(6) . . . . ?
N4 U1 C1 N2 161.8(5) . . . . ?
N3 U1 C1 N2 172.4(6) . . . . ?
C18 U1 C1 N2 -19.9(7) . . . . ?
C19 C18 C23 C22 2.0(11) . . . . ?
N1 C18 C23 C22 -171.9(7) . . . . ?
U1 C18 C23 C22 -118.6(7) . . . . ?
C19 C18 C23 C27 -174.9(7) . . . . ?
N1 C18 C23 C27 11.2(11) . . . . ?
U1 C18 C23 C27 64.5(8) . . . . ?
C19 C20 C21 C22 1.8(12) . . . . ?
N3 C34 C33 C32 1.0(13) . . . . ?
C35 C34 C33 C32 -174.4(8) . . . . ?
C18 C23 C22 C21 -1.3(13) . . . . ?
C27 C23 C22 C21 175.6(8) . . . . ?
C20 C21 C22 C23 -0.5(13) . . . . ?
C35 N4 C39 C38 -0.8(12) . . . . ?
U1 N4 C39 C38 164.5(7) . . . . ?
C22 C23 C27 C28 47.7(12) . . . . ?
C18 C23 C27 C28 -135.4(9) . . . . ?
C22 C23 C27 C29 -75.1(11) . . . . ?
C18 C23 C27 C29 101.8(11) . . . . ?
C2 C1 C6 C5 1.6(13) . . . . ?
N2 C1 C6 C5 177.0(8) . . . . ?
U1 C1 C6 C5 126.8(9) . . . . ?
C2 C1 C6 C10 -178.0(9) . . . . ?
N2 C1 C6 C10 -2.6(13) . . . . ?
U1 C1 C6 C10 -52.9(10) . . . . ?
C1 C6 C10 C12 -107.6(11) . . . . ?
C5 C6 C10 C12 72.7(13) . . . . ?
C1 C6 C10 C11 127.7(10) . . . . ?
C5 C6 C10 C11 -51.9(13) . . . . ?
C6 C1 C2 C3 -2.5(13) . . . . ?
N2 C1 C2 C3 -177.9(8) . . . . ?
U1 C1 C2 C3 -129.3(7) . . . . ?
C6 C1 C2 C7 176.9(9) . . . . ?
N2 C1 C2 C7 1.5(13) . . . . ?
U1 C1 C2 C7 50.1(10) . . . . ?
C34 C33 C32 C31 -0.7(14) . . . . ?
C30 C31 C32 C33 0.6(14) . . . . ?
N4 C39 C38 C37 0.0(14) . . . . ?
C36 C37 C38 C39 0.0(13) . . . . ?
C1 C2 C7 C8 -119.9(11) . . . . ?
C3 C2 C7 C8 59.5(13) . . . . ?
C1 C2 C7 C9 114.0(12) . . . . ?
C3 C2 C7 C9 -66.6(14) . . . . ?
C1 C6 C5 C4 0.1(16) . . . . ?
C10 C6 C5 C4 179.7(11) . . . . ?
C1 C2 C3 C4 1.9(15) . . . . ?
C7 C2 C3 C4 -177.5(10) . . . . ?
C6 C5 C4 C3 -0.7(18) . . . . ?
C2 C3 C4 C5 -0.3(18) . . . . ?
C40 C41 C43 C43 -176(3) . . . 2_556 ?
C42 C41 C43 C43 7(5) . . . 2_556 ?
C40 C41 C42 C42 178(2) . . . 2_556 ?
C43 C41 C42 C42 -4(4) . . . 2_556 ?
