#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:08:11 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242668 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/27/4132763.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_4132763
loop_
_publ_author_name
'Mullane, Kimberly C.'
'Ryu, Ho'
'Cheisson, Thibault'
'Grant, Lauren N.'
'Park, Ji Young'
'Manor, Brian C.'
'Carroll, Patrick J.'
'Baik, Mu-Hyun'
'Mindiola, Daniel J.'
'Schelter, Eric J.'
_publ_section_title
;
 C-H Bond Addition across a Transient Uranium-Nitrido Moiety and Formation
 of a Parent Uranium Imido Complex.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11335
_journal_page_last               11340
_journal_paper_doi               10.1021/jacs.8b06090
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C56 H86 K N3 O3 P2 U, C3 H7'
_chemical_formula_sum            'C59 H93 K N3 O3 P2 U'
_chemical_formula_weight         1231.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.070(2)
_cell_angle_beta                 91.734(2)
_cell_angle_gamma                98.501(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7487(5)
_cell_length_b                   13.6035(6)
_cell_length_c                   17.6124(7)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.49
_cell_volume                     2948.2(2)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            104437
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.921
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       prism
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.046
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13518
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0314P)²+6.1291P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                12684
_reflns_number_total             13518
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b06090_si_001.cif
_cod_data_source_block           4921
_cod_database_code               4132763
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.474
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
U1 U 0.38493(2) 0.25689(2) 0.29196(2) 0.01683(3) Uani 1 1 d . .
K1 K 0.61452(5) 0.11212(5) 0.32023(4) 0.02810(13) Uani 1 1 d . .
P1 P 0.26218(5) 0.15014(5) 0.40276(4) 0.01577(12) Uani 1 1 d . .
P2 P 0.50572(6) 0.40748(5) 0.20387(4) 0.02013(13) Uani 1 1 d . .
N1 N 0.25287(18) 0.34755(16) 0.36293(13) 0.0178(4) Uani 1 1 d . .
N2 N 0.35987(18) 0.21836(17) 0.15215(13) 0.0200(4) Uani 1 1 d . .
N3 N 0.51461(19) 0.28254(18) 0.36414(14) 0.0222(5) Uani 1 1 d . .
H3 H 0.558(3) 0.307(3) 0.398(2) 0.030 Uiso 1 1 d R .
C1 C 0.1997(2) 0.33828(19) 0.42873(15) 0.0170(5) Uani 1 1 d . .
C2 C 0.1455(2) 0.4145(2) 0.47007(17) 0.0215(5) Uani 1 1 d . .
H2 H 0.142117 0.474039 0.450556 0.029 Uiso 1 1 calc R .
C3 C 0.0975(2) 0.4046(2) 0.53787(17) 0.0236(6) Uani 1 1 d . .
H3a H 0.063246 0.458263 0.564133 0.031 Uiso 1 1 calc R .
C4 C 0.0977(2) 0.3184(2) 0.56911(16) 0.0222(5) Uani 1 1 d . .
C5 C 0.1480(2) 0.2417(2) 0.52799(16) 0.0192(5) Uani 1 1 d . .
H5 H 0.148654 0.181676 0.547467 0.026 Uiso 1 1 calc R .
C6 C 0.1975(2) 0.24899(19) 0.45931(15) 0.0163(5) Uani 1 1 d . .
C7 C 0.0468(3) 0.3093(2) 0.64415(19) 0.0316(7) Uani 1 1 d . .
H7a H 0.037684 0.238219 0.649193 0.047 Uiso 1 1 calc GR .
H7b H -0.022798 0.331809 0.643783 0.047 Uiso 1 1 calc GR .
H7c H 0.092293 0.352034 0.688174 0.047 Uiso 1 1 calc GR .
C8 C 0.1499(2) 0.04790(19) 0.35908(16) 0.0191(5) Uani 1 1 d . .
H8 H 0.181255 -0.006721 0.324251 0.025 Uiso 1 1 calc R .
C9 C 0.0793(2) 0.0918(2) 0.30705(17) 0.0232(5) Uani 1 1 d . .
H9a H 0.021047 0.038578 0.281657 0.035 Uiso 1 1 calc GR .
H9b H 0.121610 0.116568 0.267398 0.035 Uiso 1 1 calc GR .
H9c H 0.049947 0.148234 0.338801 0.035 Uiso 1 1 calc GR .
C10 C 0.0851(2) -0.0025(2) 0.41593(18) 0.0266(6) Uani 1 1 d . .
H10a H 0.051856 0.048516 0.450648 0.040 Uiso 1 1 calc GR .
H10b H 0.131898 -0.032358 0.446784 0.040 Uiso 1 1 calc GR .
H10c H 0.029801 -0.056152 0.386896 0.040 Uiso 1 1 calc GR .
C11 C 0.3275(2) 0.0971(2) 0.47696(16) 0.0203(5) Uani 1 1 d . .
H11 H 0.272545 0.074536 0.511705 0.027 Uiso 1 1 calc R .
C12 C 0.4122(2) 0.1790(2) 0.52651(17) 0.0263(6) Uani 1 1 d . .
H12a H 0.447704 0.149665 0.564578 0.039 Uiso 1 1 calc GR .
H12b H 0.378460 0.235370 0.553820 0.039 Uiso 1 1 calc GR .
H12c H 0.464710 0.204361 0.492801 0.039 Uiso 1 1 calc GR .
C13 C 0.3756(2) 0.0046(2) 0.43695(18) 0.0263(6) Uani 1 1 d . .
H13a H 0.432005 0.026118 0.404569 0.040 Uiso 1 1 calc GR .
H13b H 0.320233 -0.045251 0.404220 0.040 Uiso 1 1 calc GR .
H13c H 0.405447 -0.026478 0.476422 0.040 Uiso 1 1 calc GR .
C14 C 0.2532(2) 0.4420(2) 0.33957(15) 0.0188(5) Uani 1 1 d . .
C15 C 0.1759(2) 0.4505(2) 0.28328(17) 0.0249(6) Uani 1 1 d . .
C16 C 0.1769(3) 0.5437(2) 0.26163(17) 0.0272(6) Uani 1 1 d . .
H16 H 0.123640 0.549940 0.224786 0.036 Uiso 1 1 calc R .
C17 C 0.2538(3) 0.6277(2) 0.29262(17) 0.0270(6) Uani 1 1 d . .
C18 C 0.3295(2) 0.6176(2) 0.34708(17) 0.0244(6) Uani 1 1 d . .
H18 H 0.382699 0.674244 0.368147 0.032 Uiso 1 1 calc R .
C19 C 0.3303(2) 0.5265(2) 0.37231(16) 0.0209(5) Uani 1 1 d . .
C20 C 0.0917(3) 0.3612(3) 0.2496(2) 0.0356(7) Uani 1 1 d . .
H20a H 0.043672 0.380573 0.212789 0.053 Uiso 1 1 calc GR .
H20b H 0.051280 0.340311 0.291590 0.053 Uiso 1 1 calc GR .
H20c H 0.125203 0.304541 0.222548 0.053 Uiso 1 1 calc GR .
C21 C 0.2528(3) 0.7276(2) 0.2676(2) 0.0384(8) Uani 1 1 d . .
H21a H 0.209099 0.769012 0.301696 0.058 Uiso 1 1 calc GR .
H21b H 0.222984 0.713996 0.213762 0.058 Uiso 1 1 calc GR .
H21c H 0.325518 0.764294 0.271019 0.058 Uiso 1 1 calc GR .
C22 C 0.4086(2) 0.5209(2) 0.43584(18) 0.0261(6) Uani 1 1 d . .
H22a H 0.457352 0.585551 0.450558 0.039 Uiso 1 1 calc GR .
H22b H 0.449136 0.465625 0.417377 0.039 Uiso 1 1 calc GR .
H22c H 0.370571 0.507782 0.481119 0.039 Uiso 1 1 calc GR .
C23 C 0.4383(2) 0.2257(2) 0.10061(15) 0.0194(5) Uani 1 1 d . .
C24 C 0.4461(2) 0.1497(2) 0.03327(16) 0.0234(5) Uani 1 1 d . .
H24 H 0.394638 0.089723 0.021645 0.031 Uiso 1 1 calc R .
C25 C 0.5278(3) 0.1617(2) -0.01593(17) 0.0268(6) Uani 1 1 d . .
H25 H 0.530994 0.109332 -0.060500 0.036 Uiso 1 1 calc R .
C26 C 0.6051(3) 0.2481(2) -0.00201(17) 0.0263(6) Uani 1 1 d . .
C27 C 0.5988(2) 0.3228(2) 0.06477(17) 0.0244(6) Uani 1 1 d . .
H27 H 0.651105 0.382200 0.075704 0.032 Uiso 1 1 calc R .
C28 C 0.5184(2) 0.3131(2) 0.11592(15) 0.0202(5) Uani 1 1 d . .
C29 C 0.6932(3) 0.2615(3) -0.0560(2) 0.0351(7) Uani 1 1 d . .
H29a H 0.721055 0.197337 -0.071544 0.053 Uiso 1 1 calc GR .
H29b H 0.750276 0.314906 -0.029202 0.053 Uiso 1 1 calc GR .
H29c H 0.665391 0.280877 -0.102296 0.053 Uiso 1 1 calc GR .
C30 C 0.4457(3) 0.5053(2) 0.16410(17) 0.0268(6) Uani 1 1 d . .
H30 H 0.427709 0.556472 0.209382 0.036 Uiso 1 1 calc R .
C31 C 0.3419(3) 0.4551(3) 0.1172(2) 0.0336(7) Uani 1 1 d . .
H31a H 0.304599 0.507730 0.103604 0.050 Uiso 1 1 calc GR .
H31b H 0.296996 0.416115 0.148288 0.050 Uiso 1 1 calc GR .
H31c H 0.357437 0.409340 0.069478 0.050 Uiso 1 1 calc GR .
C32 C 0.5187(3) 0.5628(2) 0.1152(2) 0.0341(7) Uani 1 1 d . .
H32a H 0.538513 0.514429 0.070482 0.051 Uiso 1 1 calc GR .
H32b H 0.582914 0.598459 0.146987 0.051 Uiso 1 1 calc GR .
H32c H 0.481552 0.612266 0.096718 0.051 Uiso 1 1 calc GR .
C33 C 0.6429(2) 0.4715(2) 0.23656(18) 0.0262(6) Uani 1 1 d . .
H33 H 0.675223 0.500654 0.193451 0.035 Uiso 1 1 calc R .
C34 C 0.7113(3) 0.3967(3) 0.2577(2) 0.0340(7) Uani 1 1 d . .
H34a H 0.782334 0.433146 0.277201 0.051 Uiso 1 1 calc GR .
H34b H 0.717216 0.343889 0.211424 0.051 Uiso 1 1 calc GR .
H34c H 0.678341 0.364979 0.298063 0.051 Uiso 1 1 calc GR .
C35 C 0.6387(3) 0.5587(3) 0.3070(2) 0.0376(8) Uani 1 1 d . .
H35a H 0.607565 0.530878 0.349786 0.056 Uiso 1 1 calc GR .
H35b H 0.595018 0.606296 0.292656 0.056 Uiso 1 1 calc GR .
H35c H 0.710829 0.594520 0.323642 0.056 Uiso 1 1 calc GR .
C36 C 0.2848(2) 0.1269(2) 0.14067(15) 0.0196(5) Uani 1 1 d . .
C37 C 0.3071(2) 0.0519(2) 0.18147(15) 0.0193(5) Uani 1 1 d . .
C38 C 0.2289(2) -0.0344(2) 0.17645(16) 0.0217(5) Uani 1 1 d . .
H38 H 0.242578 -0.085634 0.202998 0.029 Uiso 1 1 calc R .
C39 C 0.1328(2) -0.0468(2) 0.13405(17) 0.0250(6) Uani 1 1 d . .
C40 C 0.1135(2) 0.0276(2) 0.09407(17) 0.0265(6) Uani 1 1 d . .
H40 H 0.047778 0.019347 0.064821 0.035 Uiso 1 1 calc R .
C41 C 0.1886(2) 0.1137(2) 0.09611(16) 0.0240(6) Uani 1 1 d . .
C42 C 0.4071(2) 0.0714(2) 0.23058(16) 0.0208(5) Uani 1 1 d . .
H42a H 0.416(3) 0.014(3) 0.250(2) 0.028 Uiso 1 1 d R .
H42b H 0.467(3) 0.088(3) 0.200(2) 0.028 Uiso 1 1 d R .
C43 C 0.0510(3) -0.1409(3) 0.1313(2) 0.0354(7) Uani 1 1 d . .
H43a H 0.066116 -0.196416 0.089851 0.053 Uiso 1 1 calc GR .
H43b H -0.020099 -0.125659 0.120781 0.053 Uiso 1 1 calc GR .
H43c H 0.054199 -0.161340 0.181325 0.053 Uiso 1 1 calc GR .
C44 C 0.1682(3) 0.1916(3) 0.05012(19) 0.0318(7) Uani 1 1 d . .
H44a H 0.098225 0.170563 0.022053 0.048 Uiso 1 1 calc GR .
H44b H 0.223083 0.197111 0.012803 0.048 Uiso 1 1 calc GR .
H44c H 0.169968 0.257850 0.085626 0.048 Uiso 1 1 calc GR .
O1 O 0.74702(18) 0.12527(19) 0.20566(13) 0.0330(5) Uani 1 1 d . .
C45 C 0.6865(3) 0.0929(3) 0.13180(18) 0.0306(6) Uani 1 1 d . .
H45a H 0.641189 0.143677 0.124371 0.041 Uiso 1 1 calc R .
H45b H 0.640594 0.026615 0.128782 0.041 Uiso 1 1 calc R .
C46 C 0.7677(3) 0.0834(3) 0.07096(19) 0.0336(7) Uani 1 1 d . .
H46a H 0.738421 0.090912 0.020142 0.045 Uiso 1 1 calc R .
H46b H 0.794689 0.017722 0.064296 0.045 Uiso 1 1 calc R .
C47 C 0.8530(3) 0.1723(3) 0.1071(2) 0.0396(8) Uani 1 1 d . .
H47a H 0.922807 0.162999 0.086082 0.053 Uiso 1 1 calc R .
H47b H 0.834298 0.237383 0.098531 0.053 Uiso 1 1 calc R .
C48 C 0.8533(3) 0.1686(3) 0.1922(2) 0.0412(8) Uani 1 1 d . .
H48a H 0.905139 0.125930 0.204750 0.055 Uiso 1 1 calc R .
H48b H 0.872839 0.237961 0.225105 0.055 Uiso 1 1 calc R .
O2 O 0.75803(18) 0.13260(17) 0.44102(13) 0.0310(5) Uani 1 1 d . .
C49 C 0.8579(3) 0.1603(3) 0.4116(2) 0.0358(7) Uani 1 1 d . .
H49a H 0.862289 0.119483 0.358534 0.048 Uiso 1 1 calc R .
H49b H 0.916550 0.149870 0.445727 0.048 Uiso 1 1 calc R .
C50 C 0.8636(3) 0.2721(3) 0.4105(2) 0.0364(7) Uani 1 1 d . .
H50a H 0.826352 0.281219 0.362941 0.048 Uiso 1 1 calc R .
H50b H 0.938165 0.306505 0.413894 0.048 Uiso 1 1 calc R .
C51 C 0.8070(3) 0.3121(2) 0.4832(2) 0.0319(7) Uani 1 1 d . .
H51a H 0.858914 0.349189 0.526313 0.042 Uiso 1 1 calc R .
H51b H 0.757893 0.358115 0.472369 0.042 Uiso 1 1 calc R .
C52 C 0.7460(3) 0.2164(2) 0.5031(2) 0.0348(7) Uani 1 1 d . .
H52a H 0.775196 0.206028 0.553072 0.046 Uiso 1 1 calc R .
H52b H 0.669996 0.222573 0.507809 0.046 Uiso 1 1 calc R .
O3 O 0.6262(2) -0.0895(2) 0.28980(15) 0.0410(6) Uani 1 1 d . .
C53 C 0.5870(3) -0.1562(3) 0.2176(2) 0.0432(8) Uani 1 1 d . .
H53a H 0.536951 -0.125209 0.189400 0.058 Uiso 1 1 calc R .
H53b H 0.549935 -0.221817 0.226275 0.058 Uiso 1 1 calc R .
C54 C 0.6851(3) -0.1722(3) 0.1715(2) 0.0465(9) Uani 1 1 d . .
H54a H 0.684505 -0.245265 0.148738 0.062 Uiso 1 1 calc R .
H54b H 0.689062 -0.134125 0.129277 0.062 Uiso 1 1 calc R .
C55 C 0.7772(4) -0.1309(4) 0.2319(3) 0.0605(12) Uani 1 1 d . .
H55a H 0.827859 -0.179892 0.229536 0.080 Uiso 1 1 calc R .
H55b H 0.815544 -0.065466 0.223808 0.080 Uiso 1 1 calc R .
C56 C 0.7271(3) -0.1165(3) 0.3073(2) 0.0472(9) Uani 1 1 d . .
H56a H 0.718230 -0.179992 0.327014 0.063 Uiso 1 1 calc R .
H56b H 0.770306 -0.061454 0.346529 0.063 Uiso 1 1 calc R .
C57 C 0.8438(8) 0.6174(6) 0.1086(6) 0.180(5) Uani 1 1 d . U
H57a H 0.815737 0.612702 0.159130 0.269 Uiso 1 1 calc R .
H57b H 0.885197 0.685156 0.112326 0.269 Uiso 1 1 calc R .
H57c H 0.784647 0.606367 0.069328 0.269 Uiso 1 1 calc R .
C58 C 0.9151(7) 0.5365(7) 0.0852(5) 0.170(5) Uani 1 1 d G U
H58a H 0.873089 0.468511 0.082838 0.226 Uiso 1 1 calc R .
H58b H 0.973571 0.547245 0.125807 0.226 Uiso 1 1 calc R .
C59 C 0.9628(8) 0.5381(7) 0.0067(5) 0.176(5) Uani 1 1 d DG U
H59a H 0.905581 0.520639 -0.035440 0.234 Uiso 1 1 calc R .
H59b H 1.001418 0.606822 0.006887 0.234 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'
K K 0.2009 0.2494 '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'
P P 0.1023 0.0942 '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
P1 U1 P2 167.851(18) .
N1 U1 P1 63.96(5) .
N1 U1 P2 105.71(5) .
N1 U1 C42 138.36(8) .
N2 U1 P1 127.01(6) .
N2 U1 P2 62.29(6) .
N2 U1 N1 116.11(8) .
N2 U1 C42 67.47(8) .
N3 U1 P1 89.73(7) .
N3 U1 P2 87.25(7) .
N3 U1 N1 106.56(9) .
N3 U1 N2 132.38(9) .
N3 U1 C42 94.36(9) .
C42 U1 P1 80.97(7) .
C42 U1 P2 110.99(7) .
O1 K1 N3 113.68(8) .
O1 K1 O2 99.73(7) .
O1 K1 O3 86.67(8) .
O2 K1 N3 102.64(7) .
O2 K1 O3 87.06(7) .
O3 K1 N3 155.04(8) .
C6 P1 U1 103.37(8) .
C6 P1 C8 103.89(12) .
C6 P1 C11 104.08(12) .
C8 P1 U1 116.59(9) .
C11 P1 U1 122.70(9) .
C11 P1 C8 104.00(12) .
C28 P2 U1 96.06(9) .
C28 P2 C30 102.07(13) .
C28 P2 C33 105.47(13) .
C30 P2 U1 124.74(10) .
C33 P2 U1 121.07(10) .
C33 P2 C30 103.53(14) .
C1 N1 U1 133.90(16) .
C1 N1 C14 115.3(2) .
C14 N1 U1 108.87(16) .
C23 N2 U1 126.27(18) .
C23 N2 C36 119.0(2) .
C36 N2 U1 99.83(16) .
U1 N3 K1 105.38(10) .
U1 N3 H3 163(3) .
K1 N3 H3 92(3) .
N1 C1 C2 123.5(2) .
N1 C1 C6 120.4(2) .
C2 C1 C6 116.1(2) .
C3 C2 C1 121.9(2) .
C2 C3 C4 122.1(3) .
C3 C4 C7 121.7(3) .
C5 C4 C3 116.7(3) .
C5 C4 C7 121.6(3) .
C4 C5 C6 122.8(2) .
C1 C6 P1 115.18(19) .
C5 C6 P1 124.4(2) .
C5 C6 C1 120.4(2) .
C9 C8 P1 107.84(18) .
C10 C8 P1 116.2(2) .
C10 C8 C9 111.4(2) .
C12 C11 P1 110.12(19) .
C13 C11 P1 109.59(19) .
C13 C11 C12 111.3(2) .
C15 C14 N1 119.9(2) .
C19 C14 N1 120.3(2) .
C19 C14 C15 119.8(2) .
C14 C15 C20 120.0(3) .
C16 C15 C14 119.1(3) .
C16 C15 C20 120.8(3) .
C17 C16 C15 121.8(3) .
C16 C17 C21 120.4(3) .
C18 C17 C16 118.3(3) .
C18 C17 C21 121.4(3) .
C17 C18 C19 122.2(3) .
C14 C19 C22 120.5(2) .
C18 C19 C14 118.8(3) .
C18 C19 C22 120.6(3) .
N2 C23 C24 124.0(3) .
N2 C23 C28 118.8(2) .
C24 C23 C28 117.2(2) .
C25 C24 C23 121.0(3) .
C24 C25 C26 122.0(3) .
C25 C26 C27 117.4(3) .
C25 C26 C29 122.0(3) .
C27 C26 C29 120.7(3) .
C28 C27 C26 122.3(3) .
C23 C28 P2 115.4(2) .
C27 C28 P2 124.5(2) .
C27 C28 C23 120.2(2) .
C31 C30 P2 109.4(2) .
C31 C30 C32 110.2(3) .
C32 C30 P2 114.6(2) .
C34 C33 P2 111.2(2) .
C34 C33 C35 110.3(3) .
C35 C33 P2 108.9(2) .
C37 C36 N2 117.2(2) .
C41 C36 N2 122.1(3) .
C41 C36 C37 120.5(3) .
C36 C37 C42 118.6(2) .
C38 C37 C36 117.7(2) .
C38 C37 C42 123.6(3) .
C39 C38 C37 122.1(3) .
C38 C39 C40 119.0(3) .
C38 C39 C43 119.9(3) .
C40 C39 C43 121.2(3) .
C41 C40 C39 121.4(3) .
C36 C41 C44 119.9(3) .
C40 C41 C36 119.3(3) .
C40 C41 C44 120.7(3) .
C37 C42 U1 93.45(16) .
C37 C42 H42a 111(2) .
C37 C42 H42b 110(2) .
H42a C42 H42b 110(3) .
C45 O1 K1 108.90(17) .
C45 O1 C48 108.4(2) .
C48 O1 K1 141.6(2) .
O1 C45 C46 105.6(3) .
C45 C46 C47 100.7(3) .
C48 C47 C46 102.3(3) .
O1 C48 C47 106.4(3) .
C49 O2 K1 104.91(19) .
C49 O2 C52 105.5(2) .
C52 O2 K1 111.80(19) .
O2 C49 C50 104.9(3) .
C49 C50 C51 102.4(3) .
C52 C51 C50 104.2(3) .
O2 C52 C51 106.9(3) .
C53 O3 K1 122.6(2) .
C53 O3 C56 105.3(3) .
C56 O3 K1 116.3(2) .
O3 C53 C54 105.4(3) .
C55 C54 C53 103.7(3) .
C56 C55 C54 104.6(4) .
O3 C56 C55 104.1(3) .
C57 C58 C59 113.3 .
C59 C59 C58 108.2(11) 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 P1 3.0107(6) .
U1 P2 3.0847(7) .
U1 N1 2.452(2) .
U1 N2 2.409(2) .
U1 N3 1.997(2) .
U1 C42 2.589(3) .
K1 N3 2.789(3) .
K1 O1 2.688(2) .
K1 O2 2.705(2) .
K1 O3 2.709(3) .
P1 C6 1.816(3) .
P1 C8 1.863(3) .
P1 C11 1.851(3) .
P2 C28 1.822(3) .
P2 C30 1.872(3) .
P2 C33 1.851(3) .
N1 C1 1.379(3) .
N1 C14 1.428(3) .
N2 C23 1.378(3) .
N2 C36 1.426(3) .
N3 H3 0.79(4) .
C1 C2 1.417(4) .
C1 C6 1.425(3) .
C2 C3 1.380(4) .
C3 C4 1.396(4) .
C4 C5 1.391(4) .
C4 C7 1.510(4) .
C5 C6 1.396(4) .
C8 C9 1.531(4) .
C8 C10 1.525(4) .
C11 C12 1.533(4) .
C11 C13 1.530(4) .
C14 C15 1.410(4) .
C14 C19 1.406(4) .
C15 C16 1.397(4) .
C15 C20 1.501(4) .
C16 C17 1.394(5) .
C17 C18 1.381(5) .
C17 C21 1.516(4) .
C18 C19 1.402(4) .
C19 C22 1.498(4) .
C23 C24 1.417(4) .
C23 C28 1.422(4) .
C24 C25 1.387(4) .
C25 C26 1.391(4) .
C26 C27 1.397(4) .
C26 C29 1.508(4) .
C27 C28 1.394(4) .
C30 C31 1.527(5) .
C30 C32 1.528(4) .
C33 C34 1.529(5) .
C33 C35 1.535(4) .
C36 C37 1.421(4) .
C36 C41 1.404(4) .
C37 C38 1.409(4) .
C37 C42 1.476(4) .
C38 C39 1.385(4) .
C39 C40 1.394(4) .
C39 C43 1.518(4) .
C40 C41 1.393(4) .
C41 C44 1.508(4) .
C42 H42a 0.94(4) .
C42 H42b 0.97(4) .
O1 C45 1.442(4) .
O1 C48 1.443(4) .
C45 C46 1.512(4) .
C46 C47 1.516(5) .
C47 C48 1.510(5) .
O2 C49 1.418(4) .
O2 C52 1.435(4) .
C49 C50 1.516(5) .
C50 C51 1.528(5) .
C51 C52 1.526(5) .
O3 C53 1.427(4) .
O3 C56 1.431(5) .
C53 C54 1.529(6) .
C54 C55 1.518(6) .
C55 C56 1.478(6) .
C57 C58 1.5292 .
C58 C59 1.5305 .
C59 C59 1.494(9) 2_765
