# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_utpi3
_database_code_depnum_ccdc_archive 'CCDC 929523'
#TrackingRef 'form 1a.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 B2 I N12 U'
_chemical_formula_sum            'C30 H44 B2 I N12 U'
_chemical_formula_weight         959.32
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.3449(3)
_cell_length_b                   11.7790(2)
_cell_length_c                   14.8966(3)
_cell_angle_alpha                82.721(5)
_cell_angle_beta                 86.981(7)
_cell_angle_gamma                64.714(6)
_cell_volume                     1785.42(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.19
_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             926
_exptl_absorpt_coefficient_mu    5.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2191
_exptl_absorpt_correction_T_max  0.4087
_exptl_absorpt_process_details   'sadabs; Sheldrick 2004'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26272
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         26.37
_reflns_number_total             7268
_reflns_number_gt                6909
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+0.9883P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7268
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0178
_refine_ls_wR_factor_ref         0.0431
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.364882(7) 0.310990(8) 0.270138(6) 0.01513(3) Uani 1 1 d . . .
I1 I 0.506445(16) 0.497652(16) 0.236391(13) 0.02933(5) Uani 1 1 d . . .
N42 N 0.51239(19) 0.2393(2) 0.13727(14) 0.0203(4) Uani 1 1 d . . .
N41 N 0.63548(18) 0.14378(19) 0.14819(14) 0.0184(4) Uani 1 1 d . . .
N51 N 0.68325(18) 0.11494(19) 0.31841(14) 0.0184(4) Uani 1 1 d . . .
N52 N 0.57339(19) 0.19718(19) 0.35838(14) 0.0199(4) Uani 1 1 d . . .
N61 N 0.57684(18) -0.00745(19) 0.25547(13) 0.0183(4) Uani 1 1 d . . .
N62 N 0.44958(18) 0.06226(19) 0.28177(14) 0.0191(4) Uani 1 1 d . . .
N22 N 0.20771(18) 0.2691(2) 0.17285(13) 0.0198(4) Uani 1 1 d . . .
N21 N 0.07970(18) 0.32541(19) 0.20192(13) 0.0189(4) Uani 1 1 d . . .
N11 N 0.11217(19) 0.50871(19) 0.24313(13) 0.0185(4) Uani 1 1 d . . .
N12 N 0.16905(19) 0.5405(2) 0.31048(14) 0.0198(4) Uani 1 1 d . . .
N31 N 0.07529(18) 0.36158(19) 0.36655(14) 0.0186(4) Uani 1 1 d . . .
N32 N 0.20391(18) 0.28246(19) 0.38691(13) 0.0191(4) Uani 1 1 d . . .
C41 C 0.7034(2) 0.1439(3) 0.07096(17) 0.0231(5) Uani 1 1 d . . .
C42 C 0.6240(3) 0.2404(3) 0.00995(18) 0.0270(6) Uani 1 1 d . . .
H42 H 0.6454 0.2630 -0.0501 0.032 Uiso 1 1 calc R . .
C43 C 0.5057(2) 0.2982(3) 0.05369(17) 0.0239(5) Uani 1 1 d . . .
C45 C 0.3839(3) 0.4088(3) 0.02026(19) 0.0351(7) Uani 1 1 d . . .
H45A H 0.3111 0.3844 0.0252 0.053 Uiso 1 1 calc R . .
H45B H 0.3951 0.4365 -0.0432 0.053 Uiso 1 1 calc R . .
H45C H 0.3655 0.4781 0.0568 0.053 Uiso 1 1 calc R . .
C44 C 0.8412(2) 0.0504(3) 0.0601(2) 0.0326(6) Uani 1 1 d . . .
H44A H 0.8961 0.0575 0.1057 0.049 Uiso 1 1 calc R . .
H44B H 0.8723 0.0677 -0.0005 0.049 Uiso 1 1 calc R . .
H44C H 0.8458 -0.0352 0.0678 0.049 Uiso 1 1 calc R . .
C53 C 0.6134(3) 0.2334(3) 0.42819(17) 0.0247(6) Uani 1 1 d . . .
C52 C 0.7483(3) 0.1737(3) 0.43416(18) 0.0286(6) Uani 1 1 d . . .
H52 H 0.8014 0.1815 0.4780 0.034 Uiso 1 1 calc R . .
C51 C 0.7898(2) 0.1005(3) 0.36351(18) 0.0253(6) Uani 1 1 d . . .
C54 C 0.9261(2) 0.0180(3) 0.3379(2) 0.0381(7) Uani 1 1 d . . .
H54A H 0.9332 -0.0665 0.3315 0.057 Uiso 1 1 calc R . .
H54B H 0.9863 0.0117 0.3851 0.057 Uiso 1 1 calc R . .
H54C H 0.9484 0.0545 0.2804 0.057 Uiso 1 1 calc R . .
C55 C 0.5177(3) 0.3271(3) 0.4839(2) 0.0358(7) Uani 1 1 d . . .
H55A H 0.4292 0.3487 0.4635 0.054 Uiso 1 1 calc R . .
H55B H 0.5330 0.4036 0.4776 0.054 Uiso 1 1 calc R . .
H55C H 0.5276 0.2910 0.5476 0.054 Uiso 1 1 calc R . .
C63 C 0.3941(2) -0.0191(2) 0.29219(17) 0.0217(5) Uani 1 1 d . . .
C62 C 0.4820(2) -0.1374(3) 0.27186(18) 0.0250(6) Uani 1 1 d . . .
H62 H 0.4665 -0.2108 0.2736 0.030 Uiso 1 1 calc R . .
C61 C 0.5967(2) -0.1272(2) 0.24863(17) 0.0231(5) Uani 1 1 d . . .
C64 C 0.7223(3) -0.2270(3) 0.2211(2) 0.0358(7) Uani 1 1 d . . .
H64A H 0.7466 -0.1999 0.1609 0.054 Uiso 1 1 calc R . .
H64B H 0.7128 -0.3056 0.2197 0.054 Uiso 1 1 calc R . .
H64C H 0.7903 -0.2412 0.2648 0.054 Uiso 1 1 calc R . .
C65 C 0.2558(2) 0.0172(3) 0.3218(2) 0.0283(6) Uani 1 1 d . . .
H65A H 0.2540 -0.0136 0.3859 0.042 Uiso 1 1 calc R . .
H65B H 0.2153 -0.0206 0.2856 0.042 Uiso 1 1 calc R . .
H65C H 0.2076 0.1094 0.3132 0.042 Uiso 1 1 calc R . .
C21 C 0.0072(2) 0.2778(2) 0.16477(17) 0.0217(5) Uani 1 1 d . . .
C24 C -0.1352(3) 0.3216(3) 0.1813(2) 0.0351(7) Uani 1 1 d . . .
H24A H -0.1502 0.3002 0.2453 0.053 Uiso 1 1 calc R . .
H24B H -0.1698 0.2799 0.1439 0.053 Uiso 1 1 calc R . .
H24C H -0.1795 0.4133 0.1655 0.053 Uiso 1 1 calc R . .
C22 C 0.0884(2) 0.1896(3) 0.11078(18) 0.0261(6) Uani 1 1 d . . .
H22 H 0.0649 0.1403 0.0759 0.031 Uiso 1 1 calc R . .
C23 C 0.2118(2) 0.1864(2) 0.11707(17) 0.0223(5) Uani 1 1 d . . .
C25 C 0.3336(3) 0.1066(3) 0.06976(19) 0.0293(6) Uani 1 1 d . . .
H25A H 0.3400 0.1519 0.0112 0.044 Uiso 1 1 calc R . .
H25B H 0.3308 0.0270 0.0602 0.044 Uiso 1 1 calc R . .
H25C H 0.4096 0.0887 0.1070 0.044 Uiso 1 1 calc R . .
C13 C 0.1675(2) 0.6517(3) 0.2798(2) 0.0266(6) Uani 1 1 d . . .
C12 C 0.1101(3) 0.6935(3) 0.1938(2) 0.0322(6) Uani 1 1 d . . .
H12 H 0.0970 0.7703 0.1576 0.039 Uiso 1 1 calc R . .
C11 C 0.0766(2) 0.6019(3) 0.17260(18) 0.0270(6) Uani 1 1 d . . .
C14 C 0.0112(3) 0.5944(3) 0.09093(19) 0.0414(8) Uani 1 1 d . . .
H14A H 0.0691 0.5202 0.0617 0.062 Uiso 1 1 calc R . .
H14B H -0.0087 0.6709 0.0485 0.062 Uiso 1 1 calc R . .
H14C H -0.0698 0.5871 0.1088 0.062 Uiso 1 1 calc R . .
C15 C 0.2211(3) 0.7147(3) 0.3358(2) 0.0377(7) Uani 1 1 d . . .
H15A H 0.1495 0.7785 0.3666 0.057 Uiso 1 1 calc R . .
H15B H 0.2676 0.7555 0.2968 0.057 Uiso 1 1 calc R . .
H15C H 0.2814 0.6516 0.3810 0.057 Uiso 1 1 calc R . .
C33 C 0.2068(3) 0.2354(3) 0.47356(17) 0.0250(6) Uani 1 1 d . . .
C32 C 0.0813(3) 0.2857(3) 0.50930(19) 0.0321(6) Uani 1 1 d . . .
H32 H 0.0563 0.2685 0.5695 0.039 Uiso 1 1 calc R . .
C31 C 0.0010(2) 0.3649(3) 0.44059(18) 0.0252(6) Uani 1 1 d . . .
C34 C -0.1428(3) 0.4456(3) 0.4414(2) 0.0343(7) Uani 1 1 d . . .
H34A H -0.1609 0.5308 0.4120 0.051 Uiso 1 1 calc R . .
H34B H -0.1738 0.4505 0.5040 0.051 Uiso 1 1 calc R . .
H34C H -0.1877 0.4085 0.4085 0.051 Uiso 1 1 calc R . .
C35 C 0.3311(3) 0.1403(3) 0.51674(19) 0.0354(7) Uani 1 1 d . . .
H35A H 0.4030 0.1270 0.4738 0.053 Uiso 1 1 calc R . .
H35B H 0.3243 0.0602 0.5342 0.053 Uiso 1 1 calc R . .
H35C H 0.3478 0.1710 0.5707 0.053 Uiso 1 1 calc R . .
B2 B 0.6747(3) 0.0505(3) 0.23596(19) 0.0197(6) Uani 1 1 d . . .
H2 H 0.7624 -0.0192 0.2265 0.024 Uiso 1 1 calc R . .
B1 B 0.0379(3) 0.4236(3) 0.27006(19) 0.0194(6) Uani 1 1 d . . .
H1 H -0.0583 0.4764 0.2659 0.023 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.01315(5) 0.01321(5) 0.01794(5) -0.00138(4) 0.00184(3) -0.00487(4)
I1 0.02502(9) 0.02205(10) 0.04361(11) -0.00479(8) 0.01029(7) -0.01341(8)
N42 0.0192(10) 0.0174(11) 0.0215(11) -0.0009(9) 0.0028(8) -0.0057(9)
N41 0.0160(9) 0.0177(11) 0.0228(11) -0.0062(9) 0.0042(8) -0.0077(8)
N51 0.0150(9) 0.0146(11) 0.0237(11) -0.0001(9) -0.0017(8) -0.0048(8)
N52 0.0194(10) 0.0169(11) 0.0228(11) -0.0043(9) -0.0010(8) -0.0065(9)
N61 0.0169(9) 0.0139(11) 0.0216(11) -0.0017(8) 0.0013(8) -0.0043(8)
N62 0.0159(9) 0.0148(11) 0.0248(11) -0.0006(9) 0.0012(8) -0.0055(8)
N22 0.0156(9) 0.0198(11) 0.0220(11) -0.0054(9) 0.0002(8) -0.0049(9)
N21 0.0146(9) 0.0187(11) 0.0220(10) -0.0047(9) 0.0003(8) -0.0050(8)
N11 0.0215(10) 0.0157(11) 0.0169(10) -0.0018(8) 0.0007(8) -0.0066(9)
N12 0.0184(9) 0.0199(11) 0.0226(11) -0.0043(9) 0.0018(8) -0.0090(9)
N31 0.0159(9) 0.0161(11) 0.0220(11) -0.0029(9) 0.0042(8) -0.0054(8)
N32 0.0187(9) 0.0166(11) 0.0198(10) -0.0003(9) 0.0015(8) -0.0061(9)
C41 0.0249(12) 0.0248(14) 0.0255(13) -0.0105(11) 0.0087(10) -0.0149(11)
C42 0.0327(14) 0.0304(16) 0.0202(13) -0.0037(11) 0.0072(11) -0.0161(13)
C43 0.0268(13) 0.0234(14) 0.0233(13) -0.0014(11) 0.0029(10) -0.0131(12)
C45 0.0347(15) 0.0334(17) 0.0278(15) 0.0090(13) 0.0021(12) -0.0090(13)
C44 0.0262(13) 0.0361(17) 0.0350(16) -0.0137(13) 0.0143(12) -0.0117(13)
C53 0.0323(13) 0.0208(14) 0.0232(13) 0.0000(11) -0.0038(11) -0.0134(12)
C52 0.0326(14) 0.0304(16) 0.0282(14) 0.0018(12) -0.0100(11) -0.0188(13)
C51 0.0224(12) 0.0254(15) 0.0298(14) 0.0039(12) -0.0051(10) -0.0130(11)
C54 0.0176(12) 0.047(2) 0.0475(18) -0.0036(15) -0.0050(12) -0.0110(13)
C55 0.0426(16) 0.0371(18) 0.0319(16) -0.0142(14) 0.0004(13) -0.0182(15)
C63 0.0227(12) 0.0203(14) 0.0253(13) -0.0009(11) -0.0004(10) -0.0125(11)
C62 0.0294(13) 0.0179(14) 0.0315(14) -0.0023(11) -0.0005(11) -0.0138(12)
C61 0.0277(13) 0.0149(13) 0.0252(13) -0.0001(11) -0.0022(10) -0.0080(11)
C64 0.0323(14) 0.0175(15) 0.0537(19) -0.0099(14) 0.0080(13) -0.0060(12)
C65 0.0233(13) 0.0208(14) 0.0443(17) -0.0033(12) 0.0055(12) -0.0135(12)
C21 0.0218(12) 0.0204(14) 0.0242(13) -0.0025(11) -0.0041(10) -0.0097(11)
C24 0.0228(13) 0.0361(18) 0.0513(19) -0.0159(15) 0.0002(12) -0.0142(13)
C22 0.0288(13) 0.0251(15) 0.0275(14) -0.0060(12) -0.0059(11) -0.0129(12)
C23 0.0255(12) 0.0201(14) 0.0205(13) -0.0034(11) 0.0003(10) -0.0088(11)
C25 0.0284(13) 0.0316(16) 0.0273(14) -0.0117(12) 0.0032(11) -0.0104(12)
C13 0.0187(12) 0.0189(14) 0.0414(16) -0.0094(12) 0.0083(11) -0.0064(11)
C12 0.0300(14) 0.0195(15) 0.0413(17) 0.0098(12) 0.0011(12) -0.0087(12)
C11 0.0271(13) 0.0239(15) 0.0244(14) 0.0040(11) 0.0013(11) -0.0077(12)
C14 0.0456(17) 0.045(2) 0.0247(15) 0.0041(14) -0.0072(13) -0.0117(16)
C15 0.0312(15) 0.0269(16) 0.061(2) -0.0159(15) 0.0058(14) -0.0153(13)
C33 0.0296(13) 0.0253(15) 0.0212(13) 0.0015(11) 0.0008(10) -0.0137(12)
C32 0.0357(15) 0.0394(18) 0.0226(14) 0.0007(13) 0.0087(11) -0.0194(14)
C31 0.0258(13) 0.0258(15) 0.0272(14) -0.0075(12) 0.0106(11) -0.0139(12)
C34 0.0253(13) 0.0410(19) 0.0353(16) -0.0087(14) 0.0121(12) -0.0130(13)
C35 0.0348(15) 0.0382(18) 0.0272(15) 0.0147(13) -0.0055(12) -0.0144(14)
B2 0.0142(12) 0.0159(15) 0.0263(15) -0.0026(12) 0.0015(11) -0.0039(11)
B1 0.0173(12) 0.0159(15) 0.0224(14) -0.0011(11) -0.0013(10) -0.0045(11)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 N52 2.5085(19) . ?
U1 N42 2.510(2) . ?
U1 N32 2.5525(19) . ?
U1 N22 2.5937(19) . ?
U1 N62 2.650(2) . ?
U1 N12 2.783(2) . ?
U1 N11 2.826(2) . ?
U1 I1 3.2121(2) . ?
N42 C43 1.335(3) . ?
N42 N41 1.370(3) . ?
N41 C41 1.351(3) . ?
N41 B2 1.548(3) . ?
N51 C51 1.351(3) . ?
N51 N52 1.372(3) . ?
N51 B2 1.551(3) . ?
N52 C53 1.341(3) . ?
N61 C61 1.347(3) . ?
N61 N62 1.386(3) . ?
N61 B2 1.531(3) . ?
N62 C63 1.343(3) . ?
N22 C23 1.343(3) . ?
N22 N21 1.386(3) . ?
N21 C21 1.349(3) . ?
N21 B1 1.539(3) . ?
N11 C11 1.359(3) . ?
N11 N12 1.390(3) . ?
N11 B1 1.569(3) . ?
N12 C13 1.324(3) . ?
N31 C31 1.347(3) . ?
N31 N32 1.379(3) . ?
N31 B1 1.521(3) . ?
N32 C33 1.335(3) . ?
C41 C42 1.371(4) . ?
C41 C44 1.494(3) . ?
C42 C43 1.389(4) . ?
C42 H42 0.9500 . ?
C43 C45 1.491(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C53 C52 1.387(4) . ?
C53 C55 1.483(4) . ?
C52 C51 1.379(4) . ?
C52 H52 0.9500 . ?
C51 C54 1.493(4) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C63 C62 1.385(4) . ?
C63 C65 1.497(3) . ?
C62 C61 1.379(4) . ?
C62 H62 0.9500 . ?
C61 C64 1.487(4) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C21 C22 1.375(4) . ?
C21 C24 1.488(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C22 C23 1.392(3) . ?
C22 H22 0.9500 . ?
C23 C25 1.498(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C13 C12 1.400(4) . ?
C13 C15 1.487(4) . ?
C12 C11 1.362(4) . ?
C12 H12 0.9500 . ?
C11 C14 1.489(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C33 C32 1.393(4) . ?
C33 C35 1.490(4) . ?
C32 C31 1.370(4) . ?
C32 H32 0.9500 . ?
C31 C34 1.497(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
B2 H2 1.0000 . ?
B1 H1 1.0000 . ?
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
N52 U1 N42 83.23(6) . . ?
N52 U1 N32 100.24(6) . . ?
N42 U1 N32 150.13(7) . . ?
N52 U1 N22 141.32(6) . . ?
N42 U1 N22 81.80(6) . . ?
N32 U1 N22 77.16(6) . . ?
N52 U1 N62 68.01(6) . . ?
N42 U1 N62 73.13(6) . . ?
N32 U1 N62 80.67(6) . . ?
N22 U1 N62 73.55(6) . . ?
N52 U1 N12 123.14(6) . . ?
N42 U1 N12 134.71(6) . . ?
N32 U1 N12 67.55(6) . . ?
N22 U1 N12 92.02(6) . . ?
N62 U1 N12 147.44(6) . . ?
N52 U1 N11 151.51(6) . . ?
N42 U1 N11 120.01(6) . . ?
N32 U1 N11 68.40(6) . . ?
N22 U1 N11 63.84(6) . . ?
N62 U1 N11 131.39(6) . . ?
N12 U1 N11 28.69(5) . . ?
N52 U1 I1 75.68(5) . . ?
N42 U1 I1 74.84(5) . . ?
N32 U1 I1 134.93(5) . . ?
N22 U1 I1 132.98(5) . . ?
N62 U1 I1 133.59(4) . . ?
N12 U1 I1 77.42(4) . . ?
N11 U1 I1 93.76(4) . . ?
C43 N42 N41 107.14(19) . . ?
C43 N42 U1 129.50(17) . . ?
N41 N42 U1 121.37(14) . . ?
C41 N41 N42 109.0(2) . . ?
C41 N41 B2 129.8(2) . . ?
N42 N41 B2 121.00(19) . . ?
C51 N51 N52 109.5(2) . . ?
C51 N51 B2 129.0(2) . . ?
N52 N51 B2 121.51(18) . . ?
C53 N52 N51 106.85(19) . . ?
C53 N52 U1 128.54(17) . . ?
N51 N52 U1 120.05(14) . . ?
C61 N61 N62 110.13(19) . . ?
C61 N61 B2 127.4(2) . . ?
N62 N61 B2 122.46(19) . . ?
C63 N62 N61 105.46(19) . . ?
C63 N62 U1 135.68(16) . . ?
N61 N62 U1 117.61(14) . . ?
C23 N22 N21 106.05(19) . . ?
C23 N22 U1 139.24(16) . . ?
N21 N22 U1 112.19(13) . . ?
C21 N21 N22 110.18(19) . . ?
C21 N21 B1 128.6(2) . . ?
N22 N21 B1 121.14(18) . . ?
C11 N11 N12 109.5(2) . . ?
C11 N11 B1 123.6(2) . . ?
N12 N11 B1 119.30(19) . . ?
C11 N11 U1 124.80(15) . . ?
N12 N11 U1 73.95(11) . . ?
B1 N11 U1 95.63(13) . . ?
C13 N12 N11 106.0(2) . . ?
C13 N12 U1 123.54(16) . . ?
N11 N12 U1 77.35(12) . . ?
C31 N31 N32 109.8(2) . . ?
C31 N31 B1 130.7(2) . . ?
N32 N31 B1 119.42(19) . . ?
C33 N32 N31 106.51(19) . . ?
C33 N32 U1 137.21(16) . . ?
N31 N32 U1 113.79(14) . . ?
N41 C41 C42 108.2(2) . . ?
N41 C41 C44 122.6(2) . . ?
C42 C41 C44 129.2(2) . . ?
C41 C42 C43 106.1(2) . . ?
C41 C42 H42 127.0 . . ?
C43 C42 H42 127.0 . . ?
N42 C43 C42 109.6(2) . . ?
N42 C43 C45 120.8(2) . . ?
C42 C43 C45 129.6(2) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N52 C53 C52 109.7(2) . . ?
N52 C53 C55 120.5(2) . . ?
C52 C53 C55 129.8(2) . . ?
C51 C52 C53 106.1(2) . . ?
C51 C52 H52 126.9 . . ?
C53 C52 H52 126.9 . . ?
N51 C51 C52 107.9(2) . . ?
N51 C51 C54 123.7(2) . . ?
C52 C51 C54 128.4(2) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N62 C63 C62 110.6(2) . . ?
N62 C63 C65 123.2(2) . . ?
C62 C63 C65 126.2(2) . . ?
C61 C62 C63 106.1(2) . . ?
C61 C62 H62 127.0 . . ?
C63 C62 H62 127.0 . . ?
N61 C61 C62 107.7(2) . . ?
N61 C61 C64 124.2(2) . . ?
C62 C61 C64 128.1(2) . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N21 C21 C22 107.3(2) . . ?
N21 C21 C24 123.0(2) . . ?
C22 C21 C24 129.7(2) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22 C23 106.9(2) . . ?
C21 C22 H22 126.6 . . ?
C23 C22 H22 126.6 . . ?
N22 C23 C22 109.6(2) . . ?
N22 C23 C25 123.0(2) . . ?
C22 C23 C25 127.4(2) . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N12 C13 C12 110.5(2) . . ?
N12 C13 C15 120.3(3) . . ?
C12 C13 C15 129.2(3) . . ?
C11 C12 C13 106.2(2) . . ?
C11 C12 H12 126.9 . . ?
C13 C12 H12 126.9 . . ?
N11 C11 C12 107.7(2) . . ?
N11 C11 C14 121.5(2) . . ?
C12 C11 C14 130.8(3) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N32 C33 C32 109.5(2) . . ?
N32 C33 C35 120.7(2) . . ?
C32 C33 C35 129.7(2) . . ?
C31 C32 C33 106.6(2) . . ?
C31 C32 H32 126.7 . . ?
C33 C32 H32 126.7 . . ?
N31 C31 C32 107.6(2) . . ?
N31 C31 C34 122.8(2) . . ?
C32 C31 C34 129.6(2) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N61 B2 N41 109.85(19) . . ?
N61 B2 N51 109.8(2) . . ?
N41 B2 N51 112.1(2) . . ?
N61 B2 H2 108.3 . . ?
N41 B2 H2 108.3 . . ?
N51 B2 H2 108.3 . . ?
N31 B1 N21 111.9(2) . . ?
N31 B1 N11 108.54(19) . . ?
N21 B1 N11 106.63(19) . . ?
N31 B1 H1 109.9 . . ?
N21 B1 H1 109.9 . . ?
N11 B1 H1 109.9 . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.081


data_utpi
_database_code_depnum_ccdc_archive 'CCDC 929524'
#TrackingRef 'form 1b.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 B2 N12 U, I'
_chemical_formula_sum            'C30 H44 B2 I N12 U'
_chemical_formula_weight         959.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
C C 0.0033 0.0016 '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'
I I -0.4742 1.8119 '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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a                   16.6266(4)
_cell_length_b                   12.9635(3)
_cell_length_c                   8.3714(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8060(10)
_cell_angle_gamma                90.00
_cell_volume                     1803.47(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4960
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      27.20
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             926
_exptl_absorpt_coefficient_mu    5.395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3832
_exptl_absorpt_correction_T_max  0.8131
_exptl_absorpt_process_details   'sadabs; Sheldrick 2004'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5267
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             1671
_reflns_number_gt                1670
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+1.9453P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1671
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0440
_refine_ls_wR_factor_gt          0.0440
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.0000 0.5000 0.01519(8) Uani 1 4 d S . .
I1 I 0.0000 0.0000 0.0000 0.04880(15) Uani 1 4 d S . .
N12 N 0.41902(13) 0.11505(18) 0.6718(2) 0.0189(5) Uani 1 1 d . . .
N11 N 0.33831(13) 0.09831(17) 0.6914(2) 0.0156(5) Uani 1 1 d . . .
N22 N 0.36208(18) 0.0000 0.3591(3) 0.0172(7) Uani 1 2 d S . .
N21 N 0.29281(18) 0.0000 0.4445(3) 0.0153(6) Uani 1 2 d S . .
C13 C 0.43655(17) 0.2078(2) 0.7340(3) 0.0228(6) Uani 1 1 d . . .
C15 C 0.5204(2) 0.2489(2) 0.7322(4) 0.0363(8) Uani 1 1 d . . .
H15A H 0.5533 0.2043 0.6659 0.054 Uiso 1 1 calc R . .
H15B H 0.5433 0.2504 0.8414 0.054 Uiso 1 1 calc R . .
H15C H 0.5197 0.3189 0.6880 0.054 Uiso 1 1 calc R . .
C12 C 0.36785(18) 0.2513(2) 0.7938(3) 0.0266(6) Uani 1 1 d . . .
H12 H 0.3636 0.3164 0.8449 0.032 Uiso 1 1 calc R . .
C11 C 0.30685(17) 0.1815(2) 0.7643(3) 0.0215(6) Uani 1 1 d . . .
C14 C 0.2192(2) 0.1918(3) 0.7950(4) 0.0382(8) Uani 1 1 d . . .
H14C H 0.1883 0.1882 0.6934 0.057 Uiso 1 1 calc R . .
H14A H 0.2092 0.2583 0.8465 0.057 Uiso 1 1 calc R . .
H14B H 0.2024 0.1358 0.8651 0.057 Uiso 1 1 calc R . .
C23 C 0.3390(2) 0.0000 0.2043(4) 0.0199(8) Uani 1 2 d S . .
C25 C 0.4015(3) 0.0000 0.0776(5) 0.0306(10) Uani 1 2 d S . .
H25C H 0.4535 0.0211 0.1251 0.046 Uiso 0.50 1 calc PR . .
H25B H 0.3854 0.0484 -0.0075 0.046 Uiso 0.50 1 calc PR . .
H25A H 0.4061 -0.0695 0.0328 0.046 Uiso 0.50 1 calc PR . .
C22 C 0.2558(3) 0.0000 0.1892(5) 0.0254(9) Uani 1 2 d S . .
H22 H 0.2241 0.0000 0.0927 0.031 Uiso 1 2 calc SR . .
C21 C 0.2281(2) 0.0000 0.3436(4) 0.0199(8) Uani 1 2 d S . .
C24 C 0.1438(3) 0.0000 0.3982(5) 0.0329(11) Uani 1 2 d S . .
H24B H 0.1318 -0.0668 0.4467 0.049 Uiso 0.50 1 calc PR . .
H24C H 0.1068 0.0120 0.3066 0.049 Uiso 0.50 1 calc PR . .
H24A H 0.1373 0.0549 0.4773 0.049 Uiso 0.50 1 calc PR . .
B1 B 0.2951(2) 0.0000 0.6295(4) 0.0148(8) Uani 1 2 d S . .
H1 H 0.234(2) 0.0000 0.668(4) 0.017(10) Uiso 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.01028(11) 0.01806(12) 0.01748(11) 0.000 0.00445(7) 0.000
I1 0.0853(4) 0.0192(2) 0.0394(2) 0.000 -0.0375(2) 0.000
N12 0.0126(11) 0.0198(12) 0.0244(11) -0.0050(9) 0.0030(9) -0.0014(9)
N11 0.0116(11) 0.0195(13) 0.0157(10) -0.0021(8) 0.0018(8) 0.0018(9)
N22 0.0152(16) 0.0218(18) 0.0148(14) 0.000 0.0023(12) 0.000
N21 0.0104(15) 0.0178(17) 0.0176(14) 0.000 -0.0001(11) 0.000
C13 0.0192(15) 0.0218(16) 0.0273(13) -0.0060(12) 0.0016(11) -0.0025(12)
C15 0.0252(17) 0.0294(19) 0.0549(19) -0.0184(16) 0.0090(14) -0.0108(14)
C12 0.0252(16) 0.0203(16) 0.0344(14) -0.0112(12) 0.0020(12) 0.0015(13)
C11 0.0190(15) 0.0214(15) 0.0242(13) -0.0055(11) 0.0014(11) 0.0055(12)
C14 0.0217(17) 0.038(2) 0.0550(19) -0.0172(16) 0.0078(15) 0.0058(15)
C23 0.023(2) 0.022(2) 0.0147(16) 0.000 0.0000(15) 0.000
C25 0.027(2) 0.047(3) 0.0180(18) 0.000 0.0042(17) 0.000
C22 0.027(2) 0.033(3) 0.0159(17) 0.000 -0.0063(15) 0.000
C21 0.014(2) 0.021(2) 0.0244(18) 0.000 -0.0054(15) 0.000
C24 0.017(2) 0.055(3) 0.026(2) 0.000 -0.0031(17) 0.000
B1 0.0081(19) 0.021(2) 0.0157(18) 0.000 0.0029(15) 0.000
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 N12 2.495(2) 6 ?
U1 N12 2.495(2) . ?
U1 N12 2.495(2) 5_656 ?
U1 N12 2.495(2) 2_656 ?
U1 N22 2.546(3) 5_656 ?
U1 N22 2.546(3) . ?
N12 C13 1.339(4) . ?
N12 N11 1.374(3) . ?
N11 C11 1.352(3) . ?
N11 B1 1.545(3) . ?
N22 C23 1.340(5) . ?
N22 N21 1.374(4) . ?
N21 C21 1.347(5) . ?
N21 B1 1.549(5) . ?
C13 C12 1.382(4) . ?
C13 C15 1.493(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 C11 1.376(4) . ?
C12 H12 0.9500 . ?
C11 C14 1.494(4) . ?
C14 H14C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C23 C22 1.386(6) . ?
C23 C25 1.508(5) . ?
C25 H25C 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25A 0.9800 . ?
C22 C21 1.386(6) . ?
C22 H22 0.9500 . ?
C21 C24 1.488(5) . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 H24A 0.9800 . ?
B1 N11 1.545(3) 6 ?
B1 H1 1.08(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
N12 U1 N12 73.40(10) 6 . ?
N12 U1 N12 106.60(10) 6 5_656 ?
N12 U1 N12 180.00(8) . 5_656 ?
N12 U1 N12 180.0 6 2_656 ?
N12 U1 N12 106.60(10) . 2_656 ?
N12 U1 N12 73.40(10) 5_656 2_656 ?
N12 U1 N22 103.15(7) 6 5_656 ?
N12 U1 N22 103.15(7) . 5_656 ?
N12 U1 N22 76.85(7) 5_656 5_656 ?
N12 U1 N22 76.85(7) 2_656 5_656 ?
N12 U1 N22 76.85(7) 6 . ?
N12 U1 N22 76.85(7) . . ?
N12 U1 N22 103.15(7) 5_656 . ?
N12 U1 N22 103.15(7) 2_656 . ?
N22 U1 N22 180.0 5_656 . ?
C13 N12 N11 107.3(2) . . ?
C13 N12 U1 130.25(18) . . ?
N11 N12 U1 121.41(15) . . ?
C11 N11 N12 108.7(2) . . ?
C11 N11 B1 128.8(2) . . ?
N12 N11 B1 122.4(2) . . ?
C23 N22 N21 106.5(3) . . ?
C23 N22 U1 132.4(2) . . ?
N21 N22 U1 121.1(2) . . ?
C21 N21 N22 109.9(3) . . ?
C21 N21 B1 128.4(3) . . ?
N22 N21 B1 121.7(3) . . ?
N12 C13 C12 109.6(3) . . ?
N12 C13 C15 120.5(3) . . ?
C12 C13 C15 129.9(3) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 C13 106.3(3) . . ?
C11 C12 H12 126.9 . . ?
C13 C12 H12 126.9 . . ?
N11 C11 C12 108.2(2) . . ?
N11 C11 C14 122.9(3) . . ?
C12 C11 C14 128.9(3) . . ?
C11 C14 H14C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N22 C23 C22 110.1(3) . . ?
N22 C23 C25 119.9(4) . . ?
C22 C23 C25 130.1(3) . . ?
C23 C25 H25C 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
C23 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C21 C22 C23 105.9(4) . . ?
C21 C22 H22 127.0 . . ?
C23 C22 H22 127.0 . . ?
N21 C21 C22 107.6(4) . . ?
N21 C21 C24 123.3(3) . . ?
C22 C21 C24 129.1(4) . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
N11 B1 N11 111.2(3) . 6 ?
N11 B1 N21 109.38(18) . . ?
N11 B1 N21 109.38(18) 6 . ?
N11 B1 H1 109.6(10) . . ?
N11 B1 H1 109.6(10) 6 . ?
N21 B1 H1 108(2) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.108


data_utpithf
_database_code_depnum_ccdc_archive 'CCDC 929525'
#TrackingRef 'form1c thf.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 B2 I N12 U, C4 H8 O'
_chemical_formula_sum            'C34 H52 B2 I N12 O U'
_chemical_formula_weight         1031.43
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.4623(4)
_cell_length_b                   11.8183(5)
_cell_length_c                   18.0014(7)
_cell_angle_alpha                97.883(2)
_cell_angle_beta                 103.934(2)
_cell_angle_gamma                94.987(2)
_cell_volume                     2123.18(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9398
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      27.03
_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1006
_exptl_absorpt_coefficient_mu    4.591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3932
_exptl_absorpt_correction_T_max  0.5459
_exptl_absorpt_process_details   'sadabs; Sheldrick 2004'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18754
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.03
_reflns_number_total             7298
_reflns_number_gt                6424
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.1142P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7298
_refine_ls_number_parameters     473
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.440321(16) 0.162594(14) 0.265534(9) 0.01866(7) Uani 1 1 d . . .
I1 I 0.67198(3) 0.00280(3) 0.26909(2) 0.03520(10) Uani 1 1 d . . .
N11 N 0.5280(4) 0.1978(3) 0.4544(2) 0.0236(9) Uani 1 1 d . . .
N12 N 0.6059(4) 0.2281(3) 0.4066(2) 0.0259(9) Uani 1 1 d . . .
N21 N 0.3727(4) 0.3438(3) 0.4115(2) 0.0212(8) Uani 1 1 d . . .
N22 N 0.3942(4) 0.3498(3) 0.3390(2) 0.0219(8) Uani 1 1 d . . .
N31 N 0.2753(4) 0.1357(3) 0.4047(2) 0.0217(8) Uani 1 1 d . . .
N32 N 0.2586(4) 0.0917(3) 0.3276(2) 0.0216(8) Uani 1 1 d . . .
N41 N 0.4287(4) 0.2457(3) 0.0869(2) 0.0219(8) Uani 1 1 d . . .
N42 N 0.5067(4) 0.2565(3) 0.1612(2) 0.0226(9) Uani 1 1 d . . .
N51 N 0.3361(4) 0.0349(3) 0.0722(2) 0.0214(8) Uani 1 1 d . . .
N52 N 0.3482(4) 0.0027(3) 0.1438(2) 0.0233(9) Uani 1 1 d . . .
N61 N 0.1951(4) 0.1903(3) 0.0960(2) 0.0229(9) Uani 1 1 d . . .
N62 N 0.2166(4) 0.2201(3) 0.1754(2) 0.0227(9) Uani 1 1 d . . .
B1 B 0.3868(5) 0.2347(5) 0.4493(3) 0.0233(12) Uani 1 1 d . . .
H1 H 0.3771 0.2538 0.5034 0.028 Uiso 1 1 calc R . .
B2 B 0.3041(5) 0.1571(5) 0.0573(3) 0.0226(12) Uani 1 1 d . . .
H2 H 0.2704 0.1546 0.0001 0.027 Uiso 1 1 calc R . .
C11 C 0.6052(5) 0.1654(4) 0.5183(3) 0.0290(11) Uani 1 1 d . . .
C12 C 0.7325(5) 0.1757(4) 0.5120(3) 0.0290(11) Uani 1 1 d . . .
H12 H 0.8080 0.1586 0.5480 0.035 Uiso 1 1 calc R . .
C13 C 0.7310(5) 0.2158(4) 0.4431(3) 0.0271(11) Uani 1 1 d . . .
C14 C 0.5504(6) 0.1277(5) 0.5814(3) 0.0410(14) Uani 1 1 d . . .
H14A H 0.5264 0.1946 0.6114 0.061 Uiso 1 1 calc R . .
H14B H 0.6174 0.0923 0.6157 0.061 Uiso 1 1 calc R . .
H14C H 0.4713 0.0715 0.5587 0.061 Uiso 1 1 calc R . .
C15 C 0.8471(5) 0.2505(5) 0.4133(3) 0.0417(14) Uani 1 1 d . . .
H15A H 0.8521 0.1916 0.3705 0.062 Uiso 1 1 calc R . .
H15B H 0.9286 0.2587 0.4551 0.062 Uiso 1 1 calc R . .
H15C H 0.8369 0.3242 0.3947 0.062 Uiso 1 1 calc R . .
C21 C 0.3376(5) 0.4451(4) 0.4401(3) 0.0265(11) Uani 1 1 d . . .
C22 C 0.3361(5) 0.5174(4) 0.3862(3) 0.0324(12) Uani 1 1 d . . .
H22 H 0.3153 0.5943 0.3904 0.039 Uiso 1 1 calc R . .
C23 C 0.3709(5) 0.4553(4) 0.3246(3) 0.0286(11) Uani 1 1 d . . .
C24 C 0.3041(6) 0.4674(5) 0.5168(3) 0.0386(13) Uani 1 1 d . . .
H24A H 0.2285 0.4123 0.5168 0.058 Uiso 1 1 calc R . .
H24B H 0.2811 0.5459 0.5255 0.058 Uiso 1 1 calc R . .
H24C H 0.3809 0.4586 0.5583 0.058 Uiso 1 1 calc R . .
C25 C 0.3815(6) 0.4940(5) 0.2490(3) 0.0406(14) Uani 1 1 d . . .
H25A H 0.4748 0.5183 0.2519 0.061 Uiso 1 1 calc R . .
H25B H 0.3302 0.5586 0.2404 0.061 Uiso 1 1 calc R . .
H25C H 0.3465 0.4299 0.2061 0.061 Uiso 1 1 calc R . .
C31 C 0.1696(5) 0.0949(4) 0.4290(3) 0.0251(11) Uani 1 1 d . . .
C32 C 0.0836(5) 0.0240(4) 0.3657(3) 0.0264(11) Uani 1 1 d . . .
H32 H 0.0010 -0.0173 0.3646 0.032 Uiso 1 1 calc R . .
C33 C 0.1413(5) 0.0252(4) 0.3049(3) 0.0241(10) Uani 1 1 d . . .
C34 C 0.1563(5) 0.1229(4) 0.5094(3) 0.0328(12) Uani 1 1 d . . .
H34A H 0.2162 0.0814 0.5435 0.049 Uiso 1 1 calc R . .
H34B H 0.0645 0.0999 0.5105 0.049 Uiso 1 1 calc R . .
H34C H 0.1792 0.2059 0.5275 0.049 Uiso 1 1 calc R . .
C35 C 0.0831(5) -0.0338(5) 0.2222(3) 0.0335(12) Uani 1 1 d . . .
H35A H 0.1360 -0.0053 0.1890 0.050 Uiso 1 1 calc R . .
H35B H -0.0085 -0.0173 0.2045 0.050 Uiso 1 1 calc R . .
H35C H 0.0841 -0.1171 0.2195 0.050 Uiso 1 1 calc R . .
C41 C 0.4820(5) 0.3201(4) 0.0476(3) 0.0266(11) Uani 1 1 d . . .
C42 C 0.5980(5) 0.3799(4) 0.0994(3) 0.0337(12) Uani 1 1 d . . .
H42 H 0.6572 0.4378 0.0890 0.040 Uiso 1 1 calc R . .
C43 C 0.6095(5) 0.3376(4) 0.1687(3) 0.0277(11) Uani 1 1 d . . .
C44 C 0.4202(5) 0.3309(5) -0.0343(3) 0.0352(13) Uani 1 1 d . . .
H44A H 0.4067 0.2553 -0.0671 0.053 Uiso 1 1 calc R . .
H44B H 0.4787 0.3845 -0.0520 0.053 Uiso 1 1 calc R . .
H44C H 0.3344 0.3600 -0.0377 0.053 Uiso 1 1 calc R . .
C45 C 0.7141(5) 0.3668(5) 0.2432(3) 0.0424(14) Uani 1 1 d . . .
H45A H 0.6774 0.4074 0.2830 0.064 Uiso 1 1 calc R . .
H45B H 0.7889 0.4162 0.2361 0.064 Uiso 1 1 calc R . .
H45C H 0.7446 0.2959 0.2596 0.064 Uiso 1 1 calc R . .
C51 C 0.3314(4) -0.0585(4) 0.0181(3) 0.0238(10) Uani 1 1 d . . .
C52 C 0.3398(5) -0.1518(4) 0.0555(3) 0.0267(11) Uani 1 1 d . . .
H52 H 0.3392 -0.2293 0.0327 0.032 Uiso 1 1 calc R . .
C53 C 0.3493(5) -0.1119(4) 0.1329(3) 0.0276(11) Uani 1 1 d . . .
C54 C 0.3202(5) -0.0520(5) -0.0660(3) 0.0338(12) Uani 1 1 d . . .
H54A H 0.2312 -0.0348 -0.0904 0.051 Uiso 1 1 calc R . .
H54B H 0.3354 -0.1259 -0.0924 0.051 Uiso 1 1 calc R . .
H54C H 0.3867 0.0090 -0.0701 0.051 Uiso 1 1 calc R . .
C55 C 0.3549(6) -0.1801(4) 0.1972(3) 0.0377(13) Uani 1 1 d . . .
H55A H 0.4305 -0.2245 0.2015 0.057 Uiso 1 1 calc R . .
H55B H 0.2726 -0.2328 0.1863 0.057 Uiso 1 1 calc R . .
H55C H 0.3653 -0.1278 0.2460 0.057 Uiso 1 1 calc R . .
C61 C 0.0679(5) 0.1948(4) 0.0599(3) 0.0289(11) Uani 1 1 d . . .
C62 C 0.0040(5) 0.2307(4) 0.1166(3) 0.0303(12) Uani 1 1 d . . .
H62 H -0.0866 0.2426 0.1087 0.036 Uiso 1 1 calc R . .
C63 C 0.0983(5) 0.2456(4) 0.1869(3) 0.0243(10) Uani 1 1 d . . .
C64 C 0.0153(5) 0.1636(5) -0.0268(3) 0.0439(15) Uani 1 1 d . . .
H64A H 0.0704 0.2082 -0.0522 0.066 Uiso 1 1 calc R . .
H64B H -0.0764 0.1810 -0.0421 0.066 Uiso 1 1 calc R . .
H64C H 0.0176 0.0812 -0.0426 0.066 Uiso 1 1 calc R . .
C65 C 0.0766(5) 0.2842(4) 0.2650(3) 0.0308(12) Uani 1 1 d . . .
H65A H 0.1519 0.2693 0.3053 0.046 Uiso 1 1 calc R . .
H65B H -0.0052 0.2418 0.2695 0.046 Uiso 1 1 calc R . .
H65C H 0.0691 0.3668 0.2715 0.046 Uiso 1 1 calc R . .
C1 C -0.1237(16) 0.6626(14) 0.2205(7) 0.189(9) Uani 1 1 d . . .
H1A H -0.1628 0.5881 0.1869 0.227 Uiso 1 1 calc R . .
H1B H -0.1195 0.7244 0.1889 0.227 Uiso 1 1 calc R . .
C2 C 0.0135(12) 0.6560(11) 0.2798(7) 0.124(4) Uani 1 1 d . . .
H2A H 0.0633 0.5982 0.2579 0.149 Uiso 1 1 calc R . .
H2B H 0.0691 0.7317 0.2943 0.149 Uiso 1 1 calc R . .
C3 C -0.0287(13) 0.6202(12) 0.3486(6) 0.147(5) Uani 1 1 d . . .
H3A H -0.0137 0.5390 0.3505 0.176 Uiso 1 1 calc R . .
H3B H 0.0297 0.6674 0.3964 0.176 Uiso 1 1 calc R . .
C4 C -0.1567(13) 0.6300(8) 0.3495(6) 0.103(4) Uani 1 1 d . . .
H4A H -0.1633 0.6721 0.3996 0.124 Uiso 1 1 calc R . .
H4B H -0.2111 0.5538 0.3382 0.124 Uiso 1 1 calc R . .
O1 O -0.1928(14) 0.6941(8) 0.2888(11) 0.265(7) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.02043(10) 0.01931(10) 0.01605(10) 0.00225(7) 0.00349(7) 0.00580(7)
I1 0.0341(2) 0.0384(2) 0.0327(2) 0.00114(15) 0.00515(16) 0.01968(16)
N11 0.025(2) 0.025(2) 0.019(2) 0.0010(17) 0.0021(17) 0.0048(17)
N12 0.023(2) 0.031(2) 0.021(2) -0.0013(18) 0.0022(18) 0.0077(18)
N21 0.018(2) 0.021(2) 0.022(2) -0.0007(16) 0.0034(17) 0.0056(16)
N22 0.021(2) 0.020(2) 0.022(2) 0.0011(16) 0.0015(17) 0.0052(16)
N31 0.023(2) 0.022(2) 0.019(2) 0.0036(16) 0.0048(17) 0.0035(17)
N32 0.026(2) 0.021(2) 0.015(2) 0.0020(16) 0.0016(17) -0.0003(17)
N41 0.021(2) 0.025(2) 0.021(2) 0.0070(17) 0.0038(17) 0.0051(17)
N42 0.025(2) 0.022(2) 0.021(2) 0.0042(16) 0.0035(17) 0.0031(17)
N51 0.023(2) 0.024(2) 0.016(2) 0.0041(16) 0.0028(17) 0.0041(17)
N52 0.030(2) 0.019(2) 0.021(2) 0.0044(16) 0.0043(18) 0.0073(17)
N61 0.021(2) 0.026(2) 0.020(2) 0.0051(17) 0.0016(17) 0.0046(17)
N62 0.024(2) 0.024(2) 0.018(2) 0.0048(16) 0.0024(17) 0.0036(17)
B1 0.027(3) 0.027(3) 0.016(3) 0.002(2) 0.005(2) 0.006(2)
B2 0.027(3) 0.025(3) 0.015(3) 0.003(2) 0.002(2) 0.003(2)
C11 0.039(3) 0.020(3) 0.023(3) 0.000(2) -0.001(2) 0.007(2)
C12 0.028(3) 0.028(3) 0.025(3) -0.001(2) -0.004(2) 0.012(2)
C13 0.024(3) 0.025(3) 0.027(3) -0.005(2) 0.000(2) 0.009(2)
C14 0.048(4) 0.045(3) 0.034(3) 0.016(3) 0.010(3) 0.017(3)
C15 0.023(3) 0.048(3) 0.050(4) 0.003(3) 0.002(3) 0.014(3)
C21 0.021(3) 0.023(3) 0.033(3) -0.004(2) 0.007(2) 0.004(2)
C22 0.034(3) 0.013(2) 0.049(3) -0.002(2) 0.009(3) 0.008(2)
C23 0.028(3) 0.020(3) 0.037(3) 0.005(2) 0.006(2) 0.004(2)
C24 0.045(3) 0.030(3) 0.040(3) -0.009(2) 0.017(3) 0.008(3)
C25 0.057(4) 0.028(3) 0.043(3) 0.017(3) 0.013(3) 0.016(3)
C31 0.028(3) 0.022(2) 0.028(3) 0.007(2) 0.011(2) 0.007(2)
C32 0.021(3) 0.026(3) 0.032(3) 0.009(2) 0.005(2) 0.003(2)
C33 0.027(3) 0.019(2) 0.026(3) 0.005(2) 0.005(2) 0.004(2)
C34 0.038(3) 0.038(3) 0.025(3) 0.005(2) 0.013(2) 0.003(2)
C35 0.030(3) 0.038(3) 0.026(3) -0.003(2) 0.003(2) -0.007(2)
C41 0.027(3) 0.022(3) 0.036(3) 0.012(2) 0.012(2) 0.008(2)
C42 0.030(3) 0.025(3) 0.048(3) 0.010(2) 0.013(3) 0.001(2)
C43 0.025(3) 0.023(3) 0.037(3) 0.005(2) 0.010(2) 0.005(2)
C44 0.038(3) 0.040(3) 0.035(3) 0.022(3) 0.013(3) 0.009(2)
C45 0.039(3) 0.034(3) 0.044(4) 0.005(3) -0.002(3) -0.012(3)
C51 0.018(2) 0.025(3) 0.025(3) -0.001(2) 0.003(2) 0.000(2)
C52 0.021(3) 0.025(3) 0.031(3) -0.004(2) 0.006(2) 0.003(2)
C53 0.024(3) 0.027(3) 0.029(3) 0.003(2) 0.004(2) 0.003(2)
C54 0.036(3) 0.040(3) 0.023(3) -0.005(2) 0.011(2) -0.003(2)
C55 0.046(3) 0.027(3) 0.041(3) 0.014(2) 0.008(3) 0.009(2)
C61 0.019(3) 0.034(3) 0.028(3) 0.007(2) -0.005(2) 0.001(2)
C62 0.018(3) 0.039(3) 0.033(3) 0.005(2) 0.002(2) 0.008(2)
C63 0.023(3) 0.019(2) 0.032(3) 0.005(2) 0.008(2) 0.005(2)
C64 0.024(3) 0.072(4) 0.031(3) 0.008(3) -0.003(2) 0.005(3)
C65 0.021(3) 0.038(3) 0.036(3) 0.002(2) 0.010(2) 0.010(2)
C1 0.224(17) 0.227(16) 0.089(9) 0.089(10) 0.003(10) -0.117(14)
C2 0.122(10) 0.129(9) 0.134(11) 0.061(8) 0.038(9) 0.012(7)
C3 0.148(12) 0.161(12) 0.088(8) -0.028(8) 0.012(8) -0.084(10)
C4 0.173(11) 0.060(5) 0.107(8) 0.001(5) 0.099(8) 0.023(6)
O1 0.298(17) 0.092(7) 0.40(2) 0.081(10) 0.042(15) 0.072(9)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 N42 2.511(4) . ?
U1 N32 2.562(4) . ?
U1 N22 2.563(4) . ?
U1 N52 2.613(4) . ?
U1 N12 2.675(4) . ?
U1 N62 2.706(4) . ?
U1 I1 3.1936(4) . ?
N11 C11 1.361(6) . ?
N11 N12 1.380(5) . ?
N11 B1 1.561(6) . ?
N12 C13 1.345(6) . ?
N21 C21 1.354(6) . ?
N21 N22 1.385(5) . ?
N21 B1 1.542(6) . ?
N22 C23 1.340(6) . ?
N31 C31 1.359(6) . ?
N31 N32 1.377(5) . ?
N31 B1 1.559(7) . ?
N32 C33 1.340(6) . ?
N41 C41 1.362(6) . ?
N41 N42 1.372(5) . ?
N41 B2 1.534(7) . ?
N42 C43 1.345(6) . ?
N51 C51 1.356(6) . ?
N51 N52 1.375(5) . ?
N51 B2 1.554(6) . ?
N52 C53 1.344(6) . ?
N61 C61 1.342(6) . ?
N61 N62 1.383(5) . ?
N61 B2 1.525(6) . ?
N62 C63 1.355(6) . ?
B1 H1 1.0000 . ?
B2 H2 1.0000 . ?
C11 C12 1.360(7) . ?
C11 C14 1.492(7) . ?
C12 C13 1.385(7) . ?
C12 H12 0.9500 . ?
C13 C15 1.489(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 C22 1.377(7) . ?
C21 C24 1.499(7) . ?
C22 C23 1.385(7) . ?
C22 H22 0.9500 . ?
C23 C25 1.519(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C31 C32 1.387(7) . ?
C31 C34 1.483(6) . ?
C32 C33 1.373(6) . ?
C32 H32 0.9500 . ?
C33 C35 1.509(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C41 C42 1.402(7) . ?
C41 C44 1.488(7) . ?
C42 C43 1.389(7) . ?
C42 H42 0.9500 . ?
C43 C45 1.489(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C51 C52 1.367(7) . ?
C51 C54 1.504(6) . ?
C52 C53 1.386(7) . ?
C52 H52 0.9500 . ?
C53 C55 1.490(7) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C61 C62 1.388(7) . ?
C61 C64 1.506(7) . ?
C62 C63 1.383(7) . ?
C62 H62 0.9500 . ?
C63 C65 1.493(7) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C1 C2 1.585(16) . ?
C1 O1 1.587(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.510(14) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.358(14) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O1 1.410(16) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
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
N42 U1 N32 149.53(12) . . ?
N42 U1 N22 94.66(12) . . ?
N32 U1 N22 77.49(12) . . ?
N42 U1 N52 78.30(12) . . ?
N32 U1 N52 91.03(12) . . ?
N22 U1 N52 144.42(12) . . ?
N42 U1 N12 114.14(12) . . ?
N32 U1 N12 89.84(12) . . ?
N22 U1 N12 66.19(11) . . ?
N52 U1 N12 148.35(12) . . ?
N42 U1 N62 72.93(11) . . ?
N32 U1 N62 76.61(11) . . ?
N22 U1 N62 74.16(11) . . ?
N52 U1 N62 70.42(11) . . ?
N12 U1 N62 140.04(11) . . ?
N42 U1 I1 90.46(8) . . ?
N32 U1 I1 114.67(8) . . ?
N22 U1 I1 139.78(8) . . ?
N52 U1 I1 75.61(8) . . ?
N12 U1 I1 75.33(8) . . ?
N62 U1 I1 144.46(8) . . ?
C11 N11 N12 109.5(4) . . ?
C11 N11 B1 124.1(4) . . ?
N12 N11 B1 123.5(4) . . ?
C13 N12 N11 106.0(4) . . ?
C13 N12 U1 137.7(3) . . ?
N11 N12 U1 102.1(3) . . ?
C21 N21 N22 109.5(4) . . ?
C21 N21 B1 127.9(4) . . ?
N22 N21 B1 122.6(3) . . ?
C23 N22 N21 106.0(4) . . ?
C23 N22 U1 137.6(3) . . ?
N21 N22 U1 116.1(2) . . ?
C31 N31 N32 109.8(4) . . ?
C31 N31 B1 126.7(4) . . ?
N32 N31 B1 122.5(4) . . ?
C33 N32 N31 106.3(4) . . ?
C33 N32 U1 137.6(3) . . ?
N31 N32 U1 116.1(3) . . ?
C41 N41 N42 109.9(4) . . ?
C41 N41 B2 128.8(4) . . ?
N42 N41 B2 121.3(3) . . ?
C43 N42 N41 107.3(4) . . ?
C43 N42 U1 128.2(3) . . ?
N41 N42 U1 123.8(3) . . ?
C51 N51 N52 110.2(4) . . ?
C51 N51 B2 127.1(4) . . ?
N52 N51 B2 121.6(4) . . ?
C53 N52 N51 106.0(4) . . ?
C53 N52 U1 132.5(3) . . ?
N51 N52 U1 117.4(3) . . ?
C61 N61 N62 110.7(4) . . ?
C61 N61 B2 126.3(4) . . ?
N62 N61 B2 123.0(4) . . ?
C63 N62 N61 105.5(4) . . ?
C63 N62 U1 134.7(3) . . ?
N61 N62 U1 117.2(3) . . ?
N21 B1 N31 110.9(4) . . ?
N21 B1 N11 110.0(4) . . ?
N31 B1 N11 111.8(4) . . ?
N21 B1 H1 108.0 . . ?
N31 B1 H1 108.0 . . ?
N11 B1 H1 108.0 . . ?
N61 B2 N41 111.3(4) . . ?
N61 B2 N51 109.1(4) . . ?
N41 B2 N51 111.2(4) . . ?
N61 B2 H2 108.4 . . ?
N41 B2 H2 108.4 . . ?
N51 B2 H2 108.4 . . ?
N11 C11 C12 107.7(4) . . ?
N11 C11 C14 122.7(5) . . ?
C12 C11 C14 129.7(5) . . ?
C11 C12 C13 106.9(4) . . ?
C11 C12 H12 126.5 . . ?
C13 C12 H12 126.5 . . ?
N12 C13 C12 109.8(4) . . ?
N12 C13 C15 122.5(4) . . ?
C12 C13 C15 127.5(5) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N21 C21 C22 107.8(4) . . ?
N21 C21 C24 123.5(4) . . ?
C22 C21 C24 128.6(4) . . ?
C21 C22 C23 106.1(4) . . ?
C21 C22 H22 126.9 . . ?
C23 C22 H22 126.9 . . ?
N22 C23 C22 110.5(4) . . ?
N22 C23 C25 121.7(4) . . ?
C22 C23 C25 127.8(4) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N31 C31 C32 106.9(4) . . ?
N31 C31 C34 124.2(4) . . ?
C32 C31 C34 128.9(4) . . ?
C33 C32 C31 106.6(4) . . ?
C33 C32 H32 126.7 . . ?
C31 C32 H32 126.7 . . ?
N32 C33 C32 110.5(4) . . ?
N32 C33 C35 122.6(4) . . ?
C32 C33 C35 126.9(4) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N41 C41 C42 106.8(4) . . ?
N41 C41 C44 123.3(4) . . ?
C42 C41 C44 129.9(5) . . ?
C43 C42 C41 106.4(4) . . ?
C43 C42 H42 126.8 . . ?
C41 C42 H42 126.8 . . ?
N42 C43 C42 109.6(4) . . ?
N42 C43 C45 119.9(4) . . ?
C42 C43 C45 130.5(4) . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N51 C51 C52 107.1(4) . . ?
N51 C51 C54 123.3(4) . . ?
C52 C51 C54 129.6(4) . . ?
C51 C52 C53 107.0(4) . . ?
C51 C52 H52 126.5 . . ?
C53 C52 H52 126.5 . . ?
N52 C53 C52 109.7(4) . . ?
N52 C53 C55 122.1(4) . . ?
C52 C53 C55 128.1(5) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N61 C61 C62 107.3(4) . . ?
N61 C61 C64 122.2(5) . . ?
C62 C61 C64 130.5(5) . . ?
C63 C62 C61 106.5(4) . . ?
C63 C62 H62 126.8 . . ?
C61 C62 H62 126.8 . . ?
N62 C63 C62 110.0(4) . . ?
N62 C63 C65 123.7(4) . . ?
C62 C63 C65 126.3(4) . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C2 C1 O1 92.0(9) . . ?
C2 C1 H1A 113.4 . . ?
O1 C1 H1A 113.3 . . ?
C2 C1 H1B 113.3 . . ?
O1 C1 H1B 113.1 . . ?
H1A C1 H1B 110.6 . . ?
C3 C2 C1 102.8(9) . . ?
C3 C2 H2A 111.3 . . ?
C1 C2 H2A 111.0 . . ?
C3 C2 H2B 111.2 . . ?
C1 C2 H2B 111.3 . . ?
H2A C2 H2B 109.1 . . ?
C4 C3 C2 116.1(12) . . ?
C4 C3 H3A 108.3 . . ?
C2 C3 H3A 108.2 . . ?
C4 C3 H3B 108.4 . . ?
C2 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C3 C4 O1 99.9(11) . . ?
C3 C4 H4A 111.7 . . ?
O1 C4 H4A 111.9 . . ?
C3 C4 H4B 111.8 . . ?
O1 C4 H4B 111.8 . . ?
H4A C4 H4B 109.5 . . ?
C4 O1 C1 113.1(10) . . ?
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.110