#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:31:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179382 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/79/4327929.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_4327929
loop_
_publ_author_name
'Andrew J. Lewis'
'Ursula J. Williams'
'James M. Kikkawa'
'Patrick J. Carroll'
'Eric J. Schelter'
_publ_section_title
;
 Uranium Pyrrolylamine Complexes Featuring a Trigonal Binding Pocket and
 Interligand Noncovalent Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              37
_journal_page_last               39
_journal_paper_doi               10.1021/ic202411f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C128 H92 F36 K2 N18 U'
_chemical_formula_weight         2882.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.741(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8967(6)
_cell_length_b                   29.6220(13)
_cell_length_c                   15.2447(6)
_cell_measurement_temperature    143(1)
_cell_volume                     6157.8(4)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            84402
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.467
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         14113
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.471
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0215P)²+17.9172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                10796
_reflns_number_total             14113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202411f_si_002_2.cif
_cod_data_source_block           UP4048(CMPD2)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4327929
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.5000 0.5000 0.02287(8) Uani 1 2 d S . .
N1 N 0.6092(3) 0.44603(14) 0.6413(3) 0.0220(9) Uani 1 1 d . . .
N2 N 0.4377(3) 0.42048(14) 0.4849(3) 0.0207(9) Uani 1 1 d . . .
N3 N 0.5148(3) 0.52538(14) 0.6612(3) 0.0233(9) Uani 1 1 d . . .
N4 N 0.6722(3) 0.49291(14) 0.5153(3) 0.0232(10) Uani 1 1 d . . .
C1 C 0.6017(4) 0.39936(17) 0.6055(4) 0.0231(11) Uani 1 1 d . . .
H1a H 0.6278 0.3786 0.6592 0.031 Uiso 1 1 calc R . .
H1b H 0.6400 0.3962 0.5673 0.031 Uiso 1 1 calc R . .
C2 C 0.4976(4) 0.38819(18) 0.5464(4) 0.0234(11) Uani 1 1 d . . .
C3 C 0.4492(4) 0.34844(19) 0.5418(4) 0.0330(13) Uani 1 1 d . . .
H3 H 0.4747 0.3223 0.5769 0.044 Uiso 1 1 calc R . .
C4 C 0.3529(4) 0.35500(19) 0.4732(4) 0.0316(13) Uani 1 1 d . . .
H4 H 0.3022 0.3340 0.4542 0.042 Uiso 1 1 calc R . .
C5 C 0.3483(4) 0.39864(18) 0.4393(4) 0.0265(11) Uani 1 1 d . . .
C6 C 0.2558(4) 0.41654(18) 0.3654(4) 0.0280(12) Uani 1 1 d . . .
C7 C 0.1716(4) 0.4131(2) 0.3838(4) 0.0345(13) Uani 1 1 d . . .
H7 H 0.1772 0.4045 0.4445 0.046 Uiso 1 1 calc R . .
C8 C 0.0801(4) 0.4221(2) 0.3134(5) 0.0418(15) Uani 1 1 d . . .
C9 C 0.0691(4) 0.4356(2) 0.2228(5) 0.0457(17) Uani 1 1 d . . .
H9 H 0.0073 0.4420 0.1759 0.061 Uiso 1 1 calc R . .
C10 C 0.1515(4) 0.4392(2) 0.2033(4) 0.0368(14) Uani 1 1 d . . .
C11 C 0.2442(4) 0.43011(18) 0.2742(4) 0.0300(12) Uani 1 1 d . . .
H11 H 0.2991 0.4332 0.2602 0.040 Uiso 1 1 calc R . .
C12 C -0.0083(6) 0.4160(3) 0.3351(7) 0.064(2) Uani 1 1 d . . .
C13 C 0.1410(5) 0.4520(3) 0.1058(5) 0.0502(18) Uani 1 1 d . . .
C14 C 0.5740(4) 0.44894(18) 0.7183(4) 0.0252(11) Uani 1 1 d . . .
H14a H 0.6214 0.4350 0.7759 0.033 Uiso 1 1 calc R . .
H14b H 0.5125 0.4327 0.6997 0.033 Uiso 1 1 calc R . .
C15 C 0.5595(4) 0.4971(2) 0.7378(4) 0.0293(11) Uani 1 1 d . . .
C16 C 0.5833(4) 0.5179(2) 0.8235(4) 0.0344(13) Uani 1 1 d . . .
H16 H 0.6143 0.5051 0.8840 0.046 Uiso 1 1 calc R . .
C17 C 0.5515(4) 0.5626(2) 0.8022(4) 0.0324(13) Uani 1 1 d . . .
H17 H 0.5575 0.5854 0.8461 0.043 Uiso 1 1 calc R . .
C18 C 0.5097(4) 0.56632(19) 0.7040(4) 0.0270(12) Uani 1 1 d . . .
C19 C 0.4630(4) 0.60898(18) 0.6561(4) 0.0257(11) Uani 1 1 d . . .
C20 C 0.3642(4) 0.61251(19) 0.5965(4) 0.0270(12) Uani 1 1 d . . .
H20 H 0.3264 0.5866 0.5755 0.036 Uiso 1 1 calc R . .
C21 C 0.3212(4) 0.65485(19) 0.5682(4) 0.0289(12) Uani 1 1 d . . .
C22 C 0.3761(5) 0.6938(2) 0.5958(5) 0.0406(15) Uani 1 1 d . . .
H22 H 0.3470 0.7219 0.5764 0.054 Uiso 1 1 calc R . .
C23 C 0.4745(5) 0.6903(2) 0.6526(5) 0.0388(14) Uani 1 1 d . . .
C24 C 0.5183(4) 0.64856(19) 0.6829(4) 0.0328(13) Uani 1 1 d . . .
H24 H 0.5850 0.6469 0.7214 0.044 Uiso 1 1 calc R . .
C25 C 0.2143(5) 0.6581(2) 0.5074(5) 0.0432(16) Uani 1 1 d . . .
C26 C 0.5344(6) 0.7328(2) 0.6835(7) 0.060(2) Uani 1 1 d . . .
C27 C 0.7124(4) 0.46098(18) 0.6776(4) 0.0252(11) Uani 1 1 d . . .
H27a H 0.7212 0.4873 0.7180 0.034 Uiso 1 1 calc R . .
H27b H 0.7547 0.4372 0.7162 0.034 Uiso 1 1 calc R . .
C28 C 0.7404(4) 0.47211(18) 0.5977(4) 0.0249(11) Uani 1 1 d . . .
C29 C 0.8278(4) 0.4656(2) 0.5898(4) 0.0303(12) Uani 1 1 d . . .
H29 H 0.8840 0.4524 0.6351 0.040 Uiso 1 1 calc R . .
C30 C 0.8161(4) 0.4826(2) 0.5009(4) 0.0308(12) Uani 1 1 d . . .
H30 H 0.8633 0.4826 0.4754 0.041 Uiso 1 1 calc R . .
C31 C 0.7223(3) 0.4993(2) 0.4572(3) 0.0258(9) Uani 1 1 d . . .
C32 C 0.6832(4) 0.51840(18) 0.3593(4) 0.0248(11) Uani 1 1 d . . .
C33 C 0.6643(4) 0.56435(19) 0.3383(4) 0.0276(12) Uani 1 1 d . . .
H33 H 0.6666 0.5842 0.3864 0.037 Uiso 1 1 calc R . .
C34 C 0.6422(4) 0.58064(18) 0.2467(4) 0.0325(13) Uani 1 1 d D A .
C35 C 0.6369(5) 0.5521(2) 0.1728(4) 0.0355(14) Uani 1 1 d . . .
H35 H 0.6210 0.5631 0.1112 0.047 Uiso 1 1 calc R . .
C36 C 0.6562(4) 0.5065(2) 0.1933(4) 0.0366(14) Uani 1 1 d D B .
C37 C 0.6793(4) 0.49016(18) 0.2843(4) 0.0316(14) Uani 1 1 d . . .
H37 H 0.6927 0.4596 0.2962 0.042 Uiso 1 1 calc R . .
C38 C 0.6241(5) 0.6298(2) 0.2261(4) 0.0497(16) Uani 1 1 d DU . .
C39 C 0.6554(5) 0.4754(2) 0.1164(4) 0.0520(17) Uani 1 1 d DU . .
F1 F -0.0128(5) 0.4423(3) 0.3994(6) 0.133(3) Uani 1 1 d . . .
F2 F -0.0122(5) 0.3755(3) 0.3677(7) 0.154(4) Uani 1 1 d . . .
F3 F -0.0899(4) 0.4203(4) 0.2627(5) 0.165(4) Uani 1 1 d . . .
F4 F 0.1984(4) 0.4280(2) 0.0747(3) 0.0833(16) Uani 1 1 d . . .
F5 F 0.0503(3) 0.44567(19) 0.0397(3) 0.0805(16) Uani 1 1 d . . .
F6 F 0.1624(4) 0.49463(17) 0.0973(3) 0.0904(18) Uani 1 1 d . . .
F7 F 0.1607(3) 0.62971(15) 0.5329(3) 0.0600(12) Uani 1 1 d . . .
F8 F 0.1929(3) 0.64956(16) 0.4147(3) 0.0614(12) Uani 1 1 d . . .
F9 F 0.1783(3) 0.69941(15) 0.5085(4) 0.0751(15) Uani 1 1 d . . .
F10 F 0.6146(5) 0.72771(19) 0.7567(6) 0.141(3) Uani 1 1 d . . .
F11 F 0.5557(7) 0.7502(2) 0.6187(5) 0.160(4) Uani 1 1 d . . .
F12 F 0.4888(5) 0.76403(18) 0.7103(7) 0.145(3) Uani 1 1 d . . .
F13 F 0.6778(7) 0.6556(2) 0.2985(5) 0.080(2) Uani 0.70 1 d PDU A 1
F14 F 0.6376(11) 0.6437(3) 0.1513(7) 0.106(4) Uani 0.70 1 d PDU A 1
F15 F 0.5326(5) 0.6408(3) 0.2111(9) 0.096(3) Uani 0.70 1 d PDU A 1
F13' F 0.7058(10) 0.6528(5) 0.246(2) 0.106(7) Uani 0.30 1 d PDU A 2
F14' F 0.5725(19) 0.6375(6) 0.1342(8) 0.095(8) Uani 0.30 1 d PDU A 2
F15' F 0.5781(19) 0.6502(6) 0.2711(16) 0.091(6) Uani 0.30 1 d PDU A 2
F16 F 0.7258(10) 0.4437(4) 0.1517(7) 0.098(5) Uani 0.50 1 d PDU B 1
F17 F 0.5750(8) 0.4559(5) 0.0636(11) 0.094(5) Uani 0.50 1 d PDU B 1
F18 F 0.6871(11) 0.4968(5) 0.0571(10) 0.080(4) Uani 0.50 1 d PDU B 1
F16' F 0.7192(10) 0.4821(5) 0.0805(11) 0.077(4) Uani 0.50 1 d PDU B 2
F17' F 0.6554(11) 0.4321(3) 0.1403(8) 0.077(3) Uani 0.50 1 d PDU B 2
F18' F 0.5685(8) 0.4774(4) 0.0410(8) 0.073(4) Uani 0.50 1 d PDU B 2
K1 K 0.09470(13) 0.69260(6) 0.23999(13) 0.0591(4) Uani 1 1 d . . .
N5 N -0.0339(5) 0.6244(3) 0.2441(5) 0.070(2) Uani 1 1 d . . .
N6 N 0.1915(6) 0.6516(3) 0.1374(5) 0.0669(19) Uani 1 1 d . . .
N7 N 0.2491(6) 0.7575(2) 0.3043(5) 0.0673(19) Uani 1 1 d . . .
N8 N -0.0080(7) 0.7472(4) 0.3150(8) 0.125(4) Uani 1 1 d . . .
N9 N -0.0572(10) 0.7222(5) 0.0686(8) 0.131(5) Uani 1 1 d . . .
C40 C -0.0474(7) 0.6202(4) 0.3232(7) 0.081(3) Uani 1 1 d . . .
H40 H -0.0310 0.6448 0.3647 0.107 Uiso 1 1 calc R . .
C41 C -0.0835(8) 0.5830(6) 0.3497(9) 0.109(5) Uani 1 1 d . . .
H41 H -0.0925 0.5825 0.4066 0.145 Uiso 1 1 calc R . .
C42 C -0.1052(8) 0.5476(5) 0.2929(12) 0.113(5) Uani 1 1 d . . .
H42 H -0.1292 0.5216 0.3098 0.150 Uiso 1 1 calc R . .
C43 C -0.0923(7) 0.5492(4) 0.2086(9) 0.088(3) Uani 1 1 d . . .
H43 H -0.1066 0.5245 0.1676 0.117 Uiso 1 1 calc R . .
C44 C -0.0574(6) 0.5889(3) 0.1871(6) 0.070(2) Uani 1 1 d . . .
H44 H -0.0501 0.5908 0.1294 0.093 Uiso 1 1 calc R . .
C45 C 0.1678(6) 0.6125(3) 0.0897(6) 0.061(2) Uani 1 1 d . . .
H45 H 0.1212 0.5943 0.0984 0.081 Uiso 1 1 calc R . .
C46 C 0.2075(7) 0.5981(3) 0.0298(6) 0.069(2) Uani 1 1 d . . .
H46 H 0.1884 0.5707 -0.0022 0.092 Uiso 1 1 calc R . .
C47 C 0.2767(8) 0.6244(3) 0.0165(7) 0.081(3) Uani 1 1 d . . .
H47 H 0.3057 0.6153 -0.0244 0.108 Uiso 1 1 calc R . .
C48 C 0.3020(8) 0.6641(3) 0.0646(7) 0.085(3) Uani 1 1 d . . .
H48 H 0.3484 0.6828 0.0568 0.113 Uiso 1 1 calc R . .
C49 C 0.2585(8) 0.6763(3) 0.1242(6) 0.073(3) Uani 1 1 d . . .
H49 H 0.2771 0.7034 0.1574 0.097 Uiso 1 1 calc R . .
C50 C 0.2259(8) 0.7986(3) 0.2688(7) 0.075(3) Uani 1 1 d . . .
H50 H 0.1608 0.8043 0.2287 0.100 Uiso 1 1 calc R . .
C51 C 0.2897(10) 0.8325(3) 0.2868(7) 0.083(3) Uani 1 1 d . . .
H51 H 0.2692 0.8610 0.2604 0.110 Uiso 1 1 calc R . .
C52 C 0.3857(10) 0.8247(4) 0.3446(10) 0.096(4) Uani 1 1 d . . .
H52 H 0.4321 0.8476 0.3573 0.128 Uiso 1 1 calc R . .
C53 C 0.4131(8) 0.7817(4) 0.3844(8) 0.091(3) Uani 1 1 d . . .
H53 H 0.4776 0.7751 0.4248 0.121 Uiso 1 1 calc R . .
C54 C 0.3410(7) 0.7499(3) 0.3614(7) 0.068(2) Uani 1 1 d . . .
H54 H 0.3580 0.7213 0.3878 0.091 Uiso 1 1 calc R . .
C55 C -0.1028(9) 0.7464(6) 0.2646(10) 0.134(6) Uani 1 1 d . . .
H55 H -0.1311 0.7197 0.2336 0.178 Uiso 1 1 calc R . .
C56 C -0.1599(10) 0.7814(5) 0.2555(10) 0.116(5) Uani 1 1 d . . .
H56 H -0.2263 0.7804 0.2154 0.154 Uiso 1 1 calc R . .
C57 C -0.1202(12) 0.8179(4) 0.3051(13) 0.132(6) Uani 1 1 d . . .
H57 H -0.1596 0.8429 0.3003 0.175 Uiso 1 1 calc R . .
C58 C -0.0214(12) 0.8202(4) 0.3640(12) 0.135(6) Uani 1 1 d . . .
H58 H 0.0067 0.8457 0.4002 0.180 Uiso 1 1 calc R . .
C59 C 0.0316(8) 0.7829(4) 0.3656(7) 0.083(3) Uani 1 1 d . . .
H59 H 0.0984 0.7828 0.4040 0.110 Uiso 1 1 calc R . .
C60 C -0.1441(15) 0.7016(6) 0.0417(11) 0.154(7) Uani 1 1 d . . .
H60 H -0.1437 0.6725 0.0649 0.205 Uiso 1 1 calc R . .
C61 C -0.2309(13) 0.7183(5) -0.0147(9) 0.146(6) Uani 1 1 d . . .
H61 H -0.2880 0.7012 -0.0334 0.194 Uiso 1 1 calc R . .
C62 C -0.2317(11) 0.7614(5) -0.0434(8) 0.107(4) Uani 1 1 d . . .
H62 H -0.2913 0.7746 -0.0820 0.142 Uiso 1 1 calc R . .
C63 C -0.1498(11) 0.7856(5) -0.0182(8) 0.106(4) Uani 1 1 d . . .
H63 H -0.1517 0.8156 -0.0368 0.141 Uiso 1 1 calc R . .
C64 C -0.0631(10) 0.7650(5) 0.0358(9) 0.111(4) Uani 1 1 d . . .
H64 H -0.0053 0.7812 0.0509 0.148 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
N4 U1 N4 180.0 . 3_666
N4 U1 N3 75.27(14) . 3_666
N4 U1 N3 104.73(14) 3_666 3_666
N4 U1 N3 104.73(14) . .
N4 U1 N3 75.27(14) 3_666 .
N3 U1 N3 180.000(1) 3_666 .
N4 U1 N2 75.02(13) . 3_666
N4 U1 N2 104.98(13) 3_666 3_666
N3 U1 N2 104.84(13) 3_666 3_666
N3 U1 N2 75.16(13) . 3_666
N4 U1 N2 104.98(13) . .
N4 U1 N2 75.02(13) 3_666 .
N3 U1 N2 75.16(13) 3_666 .
N3 U1 N2 104.84(13) . .
N2 U1 N2 180.0 3_666 .
N4 U1 N1 66.45(13) . .
N4 U1 N1 113.55(13) 3_666 .
N3 U1 N1 113.63(13) 3_666 .
N3 U1 N1 66.37(13) . .
N2 U1 N1 114.14(13) 3_666 .
N2 U1 N1 65.86(13) . .
N4 U1 N1 113.55(13) . 3_666
N4 U1 N1 66.45(13) 3_666 3_666
N3 U1 N1 66.37(13) 3_666 3_666
N3 U1 N1 113.63(13) . 3_666
N2 U1 N1 65.86(13) 3_666 3_666
N2 U1 N1 114.14(13) . 3_666
N1 U1 N1 180.000(1) . 3_666
C14 N1 C1 110.6(4) . .
C14 N1 C27 109.6(4) . .
C1 N1 C27 109.4(4) . .
C14 N1 U1 108.3(3) . .
C1 N1 U1 109.6(3) . .
C27 N1 U1 109.2(3) . .
C2 N2 C5 104.1(4) . .
C2 N2 U1 118.2(3) . .
C5 N2 U1 136.7(3) . .
C15 N3 C18 103.4(4) . .
C15 N3 U1 118.4(3) . .
C18 N3 U1 136.4(3) . .
C31 N4 C28 104.5(4) . .
C31 N4 U1 136.9(3) . .
C28 N4 U1 118.0(3) . .
N1 C1 C2 109.8(4) . .
C3 C2 N2 112.1(5) . .
C3 C2 C1 128.6(5) . .
N2 C2 C1 119.2(4) . .
C2 C3 C4 106.1(5) . .
C5 C4 C3 106.8(5) . .
C4 C5 N2 110.8(5) . .
C4 C5 C6 120.6(5) . .
N2 C5 C6 128.6(5) . .
C11 C6 C7 117.5(5) . .
C11 C6 C5 124.6(5) . .
C7 C6 C5 117.1(5) . .
C8 C7 C6 121.1(6) . .
C7 C8 C9 121.0(6) . .
C7 C8 C12 119.2(7) . .
C9 C8 C12 119.8(6) . .
C10 C9 C8 118.8(6) . .
C9 C10 C11 120.4(6) . .
C9 C10 C13 119.6(6) . .
C11 C10 C13 119.9(6) . .
C6 C11 C10 121.2(5) . .
F1 C12 F3 106.2(8) . .
F1 C12 F2 104.1(9) . .
F3 C12 F2 104.2(9) . .
F1 C12 C8 114.9(7) . .
F3 C12 C8 114.4(8) . .
F2 C12 C8 111.9(7) . .
F6 C13 F5 105.7(6) . .
F6 C13 F4 105.0(7) . .
F5 C13 F4 104.9(6) . .
F6 C13 C10 114.2(6) . .
F5 C13 C10 112.8(6) . .
F4 C13 C10 113.4(6) . .
N1 C14 C15 110.0(4) . .
C16 C15 N3 113.1(6) . .
C16 C15 C14 128.6(5) . .
N3 C15 C14 118.3(5) . .
C15 C16 C17 105.9(5) . .
C18 C17 C16 106.9(5) . .
C17 C18 N3 110.7(5) . .
C17 C18 C19 121.4(5) . .
N3 C18 C19 127.8(5) . .
C20 C19 C24 118.3(5) . .
C20 C19 C18 123.3(5) . .
C24 C19 C18 117.8(5) . .
C19 C20 C21 120.3(5) . .
C22 C21 C20 121.1(5) . .
C22 C21 C25 119.4(6) . .
C20 C21 C25 119.5(5) . .
C23 C22 C21 118.7(6) . .
C22 C23 C24 121.1(6) . .
C22 C23 C26 118.9(6) . .
C24 C23 C26 120.1(6) . .
C23 C24 C19 120.5(6) . .
F7 C25 F9 106.5(5) . .
F7 C25 F8 106.0(6) . .
F9 C25 F8 105.0(6) . .
F7 C25 C21 113.5(6) . .
F9 C25 C21 112.6(6) . .
F8 C25 C21 112.6(5) . .
F11 C26 F10 106.9(9) . .
F11 C26 F12 106.3(8) . .
F10 C26 F12 103.4(8) . .
F11 C26 C23 113.6(7) . .
F10 C26 C23 113.9(7) . .
F12 C26 C23 111.9(7) . .
C28 C27 N1 110.8(4) . .
C29 C28 N4 110.9(5) . .
C29 C28 C27 129.5(5) . .
N4 C28 C27 119.6(4) . .
C28 C29 C30 106.5(5) . .
C31 C30 C29 107.9(5) . .
C30 C31 N4 110.2(5) . .
C30 C31 C32 122.5(5) . .
N4 C31 C32 127.2(4) . .
C37 C32 C33 117.1(5) . .
C37 C32 C31 117.8(5) . .
C33 C32 C31 124.3(5) . .
C34 C33 C32 120.9(5) . .
C33 C34 C35 121.3(5) . .
C33 C34 C38 120.1(5) . .
C35 C34 C38 118.5(5) . .
C34 C35 C36 118.1(5) . .
C37 C36 C35 120.9(5) . .
C37 C36 C39 119.7(5) . .
C35 C36 C39 119.3(5) . .
C36 C37 C32 121.7(5) . .
F15' C38 F14 128.0(11) . .
F15' C38 F13 63.7(11) . .
F14 C38 F13 107.2(7) . .
F15' C38 F14' 106.0(12) . .
F14 C38 F14' 41.0(11) . .
F13 C38 F14' 133.6(10) . .
F15' C38 F13' 105.9(12) . .
F14 C38 F13' 65.2(11) . .
F13 C38 F13' 46.9(11) . .
F14' C38 F13' 104.0(11) . .
F15' C38 F15 41.7(11) . .
F14 C38 F15 106.3(8) . .
F13 C38 F15 103.7(7) . .
F14' C38 F15 69.8(12) . .
F13' C38 F15 134.4(10) . .
F15' C38 C34 115.6(9) . .
F14 C38 C34 114.6(7) . .
F13 C38 C34 113.1(6) . .
F14' C38 C34 111.8(9) . .
F13' C38 C34 112.6(9) . .
F15 C38 C34 111.2(6) . .
F17 C39 F16' 117.6(13) . .
F17 C39 F17' 68.7(9) . .
F16' C39 F17' 110.1(9) . .
F17 C39 F18 106.5(10) . .
F16' C39 F18 28.1(9) . .
F17' C39 F18 132.8(9) . .
F17 C39 F18' 31.4(8) . .
F16' C39 F18' 104.5(9) . .
F17' C39 F18' 99.9(8) . .
F18 C39 F18' 83.2(11) . .
F17 C39 F16 108.5(9) . .
F16' C39 F16 71.8(9) . .
F17' C39 F16 46.1(7) . .
F18 C39 F16 99.8(8) . .
F18' C39 F16 134.4(9) . .
F17 C39 C36 119.0(9) . .
F16' C39 C36 117.8(9) . .
F17' C39 C36 112.4(6) . .
F18 C39 C36 110.2(8) . .
F18' C39 C36 110.3(8) . .
F16 C39 C36 111.1(6) . .
C25 F8 K1 137.2(4) . .
N8 K1 F8 92.1(3) . .
N8 K1 N6 168.4(3) . .
F8 K1 N6 98.35(18) . .
N8 K1 N5 85.2(3) . .
F8 K1 N5 75.45(18) . .
N6 K1 N5 102.1(2) . .
N8 K1 N9 80.3(3) . .
F8 K1 N9 161.2(3) . .
N6 K1 N9 91.1(3) . .
N5 K1 N9 86.8(4) . .
N8 K1 N7 88.2(3) . .
F8 K1 N7 86.51(19) . .
N6 K1 N7 87.6(2) . .
N5 K1 N7 160.5(2) . .
N9 K1 N7 110.2(4) . .
N8 K1 C55 20.1(3) . .
F8 K1 C55 104.3(3) . .
N6 K1 C55 154.7(3) . .
N5 K1 C55 73.4(3) . .
N9 K1 C55 64.0(3) . .
N7 K1 C55 104.7(3) . .
C40 N5 C44 115.8(9) . .
C40 N5 K1 116.7(7) . .
C44 N5 K1 124.2(6) . .
C49 N6 C45 116.6(7) . .
C49 N6 K1 115.9(6) . .
C45 N6 K1 126.8(6) . .
C54 N7 C50 117.4(9) . .
C54 N7 K1 126.5(6) . .
C50 N7 K1 116.0(7) . .
C59 N8 C55 119.2(11) . .
C59 N8 K1 121.7(8) . .
C55 N8 K1 113.0(8) . .
C60 N9 C64 113.8(13) . .
C60 N9 K1 117.3(11) . .
C64 N9 K1 122.8(11) . .
N5 C40 C41 125.3(11) . .
C42 C41 C40 118.2(12) . .
C41 C42 C43 120.0(12) . .
C42 C43 C44 117.3(11) . .
N5 C44 C43 123.3(9) . .
N6 C45 C46 123.7(8) . .
C45 C46 C47 118.9(8) . .
C48 C47 C46 118.4(8) . .
C47 C48 C49 119.2(9) . .
N6 C49 C48 123.3(8) . .
N7 C50 C51 124.2(10) . .
C50 C51 C52 118.7(10) . .
C51 C52 C53 118.8(10) . .
C54 C53 C52 117.1(11) . .
N7 C54 C53 123.8(9) . .
N8 C55 C56 123.2(15) . .
N8 C55 K1 46.8(6) . .
C56 C55 K1 152.4(12) . .
C55 C56 C57 117.8(14) . .
C56 C57 C58 121.8(13) . .
C59 C58 C57 115.7(13) . .
N8 C59 C58 122.0(11) . .
C61 C60 N9 126.8(18) . .
C60 C61 C62 116.3(18) . .
C63 C62 C61 122.0(14) . .
C62 C63 C64 117.8(14) . .
N9 C64 C63 123.2(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N4 2.490(4) .
U1 N4 2.490(4) 3_666
U1 N3 2.493(4) 3_666
U1 N3 2.493(4) .
U1 N2 2.508(4) 3_666
U1 N2 2.508(4) .
U1 N1 2.649(4) .
U1 N1 2.649(4) 3_666
N1 C14 1.468(6) .
N1 C1 1.473(6) .
N1 C27 1.477(6) .
N2 C2 1.384(6) .
N2 C5 1.390(7) .
N3 C15 1.371(7) .
N3 C18 1.394(7) .
N4 C31 1.383(6) .
N4 C28 1.400(6) .
C1 C2 1.483(7) .
C2 C3 1.368(8) .
C3 C4 1.407(8) .
C4 C5 1.383(8) .
C5 C6 1.483(7) .
C6 C11 1.389(8) .
C6 C7 1.396(8) .
C7 C8 1.380(8) .
C8 C9 1.382(10) .
C8 C12 1.492(10) .
C9 C10 1.378(9) .
C10 C11 1.395(8) .
C10 C13 1.479(9) .
C12 F1 1.273(10) .
C12 F3 1.277(10) .
C12 F2 1.310(11) .
C13 F6 1.323(9) .
C13 F5 1.335(8) .
C13 F4 1.335(9) .
C14 C15 1.492(8) .
C15 C16 1.356(8) .
C16 C17 1.398(8) .
C17 C18 1.375(7) .
C18 C19 1.485(8) .
C19 C20 1.388(8) .
C19 C24 1.396(8) .
C20 C21 1.395(8) .
C21 C22 1.379(8) .
C21 C25 1.488(8) .
C22 C23 1.374(9) .
C23 C24 1.389(8) .
C23 C26 1.503(9) .
C25 F7 1.321(8) .
C25 F9 1.340(7) .
C25 F8 1.342(8) .
C26 F11 1.263(10) .
C26 F10 1.273(9) .
C26 F12 1.308(10) .
C27 C28 1.475(7) .
C28 C29 1.368(7) .
C29 C30 1.390(8) .
C30 C31 1.376(7) .
C31 C32 1.478(7) .
C32 C37 1.399(8) .
C32 C33 1.401(8) .
C33 C34 1.385(7) .
C34 C35 1.387(8) .
C34 C38 1.492(8) .
C35 C36 1.389(9) .
C36 C37 1.376(8) .
C36 C39 1.486(8) .
C38 F15' 1.299(9) .
C38 F14 1.301(7) .
C38 F13 1.315(7) .
C38 F14' 1.318(9) .
C38 F13' 1.320(9) .
C38 F15 1.329(7) .
C39 F17 1.280(8) .
C39 F16' 1.289(8) .
C39 F17' 1.333(8) .
C39 F18 1.337(8) .
C39 F18' 1.343(8) .
C39 F16 1.349(8) .
F8 K1 2.778(4) .
K1 N8 2.770(8) .
K1 N6 2.796(7) .
K1 N5 2.802(8) .
K1 N9 2.820(11) .
K1 N7 2.851(8) .
K1 C55 3.496(12) .
N5 C40 1.306(12) .
N5 C44 1.317(11) .
N6 C49 1.318(11) .
N6 C45 1.336(10) .
N7 C54 1.313(11) .
N7 C50 1.322(11) .
N8 C59 1.302(13) .
N8 C55 1.308(14) .
N9 C60 1.34(2) .
N9 C64 1.353(17) .
C40 C41 1.358(17) .
C41 C42 1.313(18) .
C42 C43 1.376(17) .
C43 C44 1.377(13) .
C45 C46 1.342(11) .
C46 C47 1.371(12) .
C47 C48 1.356(12) .
C48 C49 1.360(11) .
C50 C51 1.334(13) .
C51 C52 1.364(15) .
C52 C53 1.399(15) .
C53 C54 1.364(13) .
C55 C56 1.312(17) .
C56 C57 1.317(19) .
C57 C58 1.383(18) .
C58 C59 1.352(15) .
C60 C61 1.327(19) .
C61 C62 1.348(18) .
C62 C63 1.332(17) .
C63 C64 1.366(16) .
