#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316437.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_4316437
loop_
_publ_author_name
'Steven J. Kraft'
'Justin Walensky'
'Phillip E. Fanwick'
'Michael B. Hall'
'Suzanne C. Bart'
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Fanwick, Phillip E.'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Crystallographic Evidence of a Base-Free Uranium(IV) Terminal Oxo Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7620
_journal_page_last               7622
_journal_paper_doi               10.1021/ic101136j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C30 H44 B2 N12 O1 U1,C4 H10 O1'
_chemical_formula_sum            'C34 H54 B2 N12 O2 U'
_chemical_formula_weight         922.54
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             23-07-10
_audit_creation_method           'SHELXL and local programs'
_audit_update_record             ' ?'
_cell_angle_alpha                99.854(2)
_cell_angle_beta                 97.554(4)
_cell_angle_gamma                101.455(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4963(5)
_cell_length_b                   11.0303(4)
_cell_length_c                   17.8461(6)
_cell_measurement_reflns_used    6606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      2
_cell_volume                     1965.64(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.8540
_diffrn_measured_fraction_theta_max 0.8540
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. 
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17368
_diffrn_reflns_theta_full        72.0
_diffrn_reflns_theta_max         72.05
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.866
_exptl_absorpt_correction_T_max  0.5255
_exptl_absorpt_correction_T_min  0.5064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.15
_refine_diff_density_min         -1.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0821P)²+3.9446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.106
_reflns_number_gt                6536
_reflns_number_total             6599
_reflns_threshold_expression     >2.0σ(I)
_cod_data_source_file            ic101136j_si_004.cif
_cod_data_source_block           SCB199
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1965.64(13)
_cod_original_formula_sum        'C34 H54 B2 N12 O2 U1'
_cod_database_code               4316437
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_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 0.082114(14) 0.228842(12) 0.262688(7) 0.02285(9) Uani 1 1 d . . .
O1 -0.0885(4) 0.2422(5) 0.2270(3) 0.0446(11) Uani 1 1 d . . .
O93 0.4279(5) 0.2839(4) -0.1799(3) 0.0480(11) Uani 1 1 d . . .
N11 0.1706(5) 0.4126(4) 0.3768(2) 0.0260(9) Uani 1 1 d . . .
N12 0.1595(4) 0.3956(4) 0.4506(2) 0.0247(9) Uani 1 1 d . . .
N21 -0.0497(5) 0.1542(4) 0.3694(3) 0.0267(9) Uani 1 1 d . . .
N22 0.0088(5) 0.1823(4) 0.4464(3) 0.0259(10) Uani 1 1 d . . .
N31 0.2270(4) 0.1307(4) 0.3642(2) 0.0256(9) Uani 1 1 d . . .
N32 0.2481(4) 0.1937(4) 0.4403(2) 0.0244(9) Uani 1 1 d . . .
N41 0.1077(5) 0.0497(4) 0.1604(2) 0.0271(9) Uani 1 1 d . . .
N42 0.1720(5) 0.0672(4) 0.1000(2) 0.0272(9) Uani 1 1 d . . .
N51 0.1094(5) 0.3256(4) 0.1390(3) 0.0285(10) Uani 1 1 d . . .
N52 0.2014(5) 0.3009(4) 0.0940(3) 0.0287(10) Uani 1 1 d . . .
N61 0.3452(4) 0.2853(4) 0.2462(2) 0.0230(9) Uani 1 1 d . . .
N62 0.3754(5) 0.2327(4) 0.1762(3) 0.0250(10) Uani 1 1 d . . .
C13 0.1797(5) 0.5093(5) 0.4984(3) 0.0248(10) Uani 1 1 d . . .
C14 0.2067(6) 0.6014(5) 0.4559(3) 0.0306(12) Uani 1 1 d . . .
C15 0.2014(6) 0.5384(5) 0.3812(3) 0.0298(12) Uani 1 1 d . . .
C16 0.1630(6) 0.5261(5) 0.5816(3) 0.0341(13) Uani 1 1 d . . .
C17 0.2263(8) 0.5919(6) 0.3111(4) 0.0428(16) Uani 1 1 d . . .
C23 -0.0781(6) 0.1334(5) 0.4893(3) 0.0278(11) Uani 1 1 d . . .
C24 -0.1939(6) 0.0741(5) 0.4396(4) 0.0329(12) Uani 1 1 d . . .
C25 -0.1722(6) 0.0884(5) 0.3663(3) 0.0281(11) Uani 1 1 d . . .
C26 -0.0444(6) 0.1458(5) 0.5751(3) 0.0348(12) Uani 1 1 d . . .
C27 -0.2701(6) 0.0393(6) 0.2919(4) 0.0390(13) Uani 1 1 d . . .
C33 0.3579(5) 0.1694(5) 0.4799(3) 0.0265(11) Uani 1 1 d . . .
C34 0.4077(6) 0.0899(5) 0.4292(3) 0.0311(12) Uani 1 1 d . . .
C35 0.3236(6) 0.0689(5) 0.3576(3) 0.0269(11) Uani 1 1 d . . .
C36 0.4102(7) 0.2263(6) 0.5629(3) 0.0389(14) Uani 1 1 d . . .
C37 0.3360(6) -0.0132(5) 0.2846(3) 0.0334(12) Uani 1 1 d . . .
C43 0.1419(6) -0.0408(6) 0.0464(3) 0.0334(13) Uani 1 1 d . . .
C44 0.0587(6) -0.1306(5) 0.0733(4) 0.0379(13) Uani 1 1 d . . .
C45 0.0384(6) -0.0705(5) 0.1443(3) 0.0325(12) Uani 1 1 d . . .
C46 0.1933(7) -0.0546(7) -0.0276(3) 0.0455(16) Uani 1 1 d . . .
C47 -0.0421(8) -0.1212(6) 0.1997(5) 0.0468(17) Uani 1 1 d . . .
C53 0.2149(6) 0.3817(5) 0.0453(3) 0.0316(12) Uani 1 1 d . . .
C54 0.1306(6) 0.4602(5) 0.0592(3) 0.0331(12) Uani 1 1 d . . .
C55 0.0656(6) 0.4217(5) 0.1172(3) 0.0304(12) Uani 1 1 d . . .
C56 0.3091(7) 0.3807(7) -0.0104(4) 0.0445(15) Uani 1 1 d . . .
C57 -0.0416(7) 0.4730(7) 0.1497(4) 0.0430(15) Uani 1 1 d . . .
C63 0.5046(6) 0.2368(5) 0.1830(3) 0.0313(12) Uani 1 1 d . . .
C64 0.5619(6) 0.2921(5) 0.2585(3) 0.0295(11) Uani 1 1 d . . .
C65 0.4600(6) 0.3227(5) 0.2952(3) 0.0259(12) Uani 1 1 d . . .
C66 0.5728(7) 0.1926(6) 0.1194(4) 0.0408(14) Uani 1 1 d . . .
C67 0.4732(6) 0.3911(5) 0.3767(3) 0.0319(12) Uani 1 1 d . . .
C91 0.2847(9) 0.3883(8) -0.2424(5) 0.059(2) Uani 1 1 d . . .
C92 0.4216(8) 0.3948(7) -0.2094(5) 0.0562(19) Uani 1 1 d . . .
C94 0.5562(9) 0.2806(9) -0.1452(6) 0.069(2) Uani 1 1 d . . .
C95 0.5492(11) 0.1634(10) -0.1123(5) 0.075(3) Uani 1 1 d . . .
B1 0.1475(6) 0.2639(6) 0.4736(3) 0.0261(12) Uani 1 1 d . . .
B2 0.2728(6) 0.1925(6) 0.1013(3) 0.0273(12) Uani 1 1 d . . .
H1 0.170(7) 0.284(7) 0.530(4) 0.040(18) Uiso 1 1 d . . .
H2 0.313(6) 0.169(6) 0.051(4) 0.031(16) Uiso 1 1 d . . .
H14 0.2251 0.6903 0.4742 0.037 Uiso 1 1 calc R . .
H24 -0.2732 0.0317 0.4529 0.039 Uiso 1 1 calc R . .
H34 0.4830 0.0562 0.4402 0.037 Uiso 1 1 calc R . .
H44 0.0227 -0.2162 0.0483 0.045 Uiso 1 1 calc R . .
H54 0.1190 0.5276 0.0342 0.040 Uiso 1 1 calc R . .
H64 0.6523 0.3063 0.2808 0.035 Uiso 1 1 calc R . .
H16A 0.0751 0.4792 0.5852 0.051 Uiso 1 1 calc R . .
H16B 0.1725 0.6160 0.6030 0.051 Uiso 1 1 calc R . .
H16C 0.2303 0.4940 0.6107 0.051 Uiso 1 1 calc R . .
H17A 0.2254 0.5231 0.2680 0.064 Uiso 1 1 calc R . .
H17B 0.3125 0.6513 0.3224 0.064 Uiso 1 1 calc R . .
H17C 0.1572 0.6361 0.2970 0.064 Uiso 1 1 calc R . .
H26A 0.0342 0.1127 0.5872 0.052 Uiso 1 1 calc R . .
H26B -0.1185 0.0976 0.5936 0.052 Uiso 1 1 calc R . .
H26C -0.0270 0.2350 0.6004 0.052 Uiso 1 1 calc R . .
H27A -0.2329 0.0722 0.2499 0.058 Uiso 1 1 calc R . .
H27B -0.3520 0.0673 0.2977 0.058 Uiso 1 1 calc R . .
H27C -0.2890 -0.0532 0.2800 0.058 Uiso 1 1 calc R . .
H36A 0.4351 0.3185 0.5697 0.058 Uiso 1 1 calc R . .
H36B 0.4878 0.1947 0.5798 0.058 Uiso 1 1 calc R . .
H36C 0.3421 0.2032 0.5938 0.058 Uiso 1 1 calc R . .
H37A 0.2501 -0.0694 0.2615 0.050 Uiso 1 1 calc R . .
H37B 0.4004 -0.0638 0.2959 0.050 Uiso 1 1 calc R . .
H37C 0.3657 0.0397 0.2485 0.050 Uiso 1 1 calc R . .
H46A 0.1720 0.0102 -0.0553 0.068 Uiso 1 1 calc R . .
H46B 0.1524 -0.1385 -0.0593 0.068 Uiso 1 1 calc R . .
H46C 0.2892 -0.0446 -0.0170 0.068 Uiso 1 1 calc R . .
H47A -0.0282 -0.0570 0.2472 0.070 Uiso 1 1 calc R . .
H47B -0.0154 -0.1968 0.2121 0.070 Uiso 1 1 calc R . .
H47C -0.1357 -0.1432 0.1764 0.070 Uiso 1 1 calc R . .
H56A 0.3987 0.3923 0.0178 0.067 Uiso 1 1 calc R . .
H56B 0.3054 0.4495 -0.0382 0.067 Uiso 1 1 calc R . .
H56C 0.2849 0.2997 -0.0472 0.067 Uiso 1 1 calc R . .
H57A -0.1241 0.4430 0.1125 0.064 Uiso 1 1 calc R . .
H57B -0.0174 0.5655 0.1602 0.064 Uiso 1 1 calc R . .
H57C -0.0536 0.4442 0.1979 0.064 Uiso 1 1 calc R . .
H66A 0.5324 0.1037 0.0966 0.061 Uiso 1 1 calc R . .
H66B 0.6663 0.2016 0.1397 0.061 Uiso 1 1 calc R . .
H66C 0.5646 0.2435 0.0797 0.061 Uiso 1 1 calc R . .
H67A 0.5030 0.4821 0.3798 0.048 Uiso 1 1 calc R . .
H67B 0.5378 0.3621 0.4101 0.048 Uiso 1 1 calc R . .
H67C 0.3876 0.3738 0.3938 0.048 Uiso 1 1 calc R . .
H91A 0.2531 0.3139 -0.2843 0.089 Uiso 1 1 calc R . .
H91B 0.2794 0.4647 -0.2626 0.089 Uiso 1 1 calc R . .
H91C 0.2296 0.3819 -0.2023 0.089 Uiso 1 1 calc R . .
H92A 0.4778 0.4015 -0.2496 0.067 Uiso 1 1 calc R . .
H92B 0.4545 0.4705 -0.1674 0.067 Uiso 1 1 calc R . .
H94A 0.5926 0.3564 -0.1037 0.083 Uiso 1 1 calc R . .
H94B 0.6152 0.2807 -0.1842 0.083 Uiso 1 1 calc R . .
H95A 0.4942 0.1658 -0.0720 0.113 Uiso 1 1 calc R . .
H95B 0.6382 0.1590 -0.0901 0.113 Uiso 1 1 calc R . .
H95C 0.5106 0.0889 -0.1534 0.113 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_radius_bond
U 1.42
O 0.73
N 0.75
C 0.77
B 0.82
H 0.32
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N41 101.0(2) . . . ?
O1 U1 N11 105.2(2) . . . ?
N41 U1 N11 153.15(15) . . . ?
O1 U1 N51 77.10(16) . . . ?
N41 U1 N51 74.49(14) . . . ?
N11 U1 N51 105.51(14) . . . ?
O1 U1 N21 77.24(16) . . . ?
N41 U1 N21 114.07(14) . . . ?
N11 U1 N21 78.01(13) . . . ?
N51 U1 N21 154.09(15) . . . ?
O1 U1 N31 143.69(16) . . . ?
N41 U1 N31 86.05(14) . . . ?
N11 U1 N31 76.46(13) . . . ?
N51 U1 N31 138.37(14) . . . ?
N21 U1 N31 67.53(14) . . . ?
O1 U1 N61 146.11(15) . . . ?
N41 U1 N61 74.58(13) . . . ?
N11 U1 N61 80.34(13) . . . ?
N51 U1 N61 69.30(13) . . . ?
N21 U1 N61 135.81(13) . . . ?
N31 U1 N61 70.17(13) . . . ?
C94 O93 C92 114.1(6) . . . ?
C15 N11 N12 106.1(4) . . . ?
C15 N11 U1 131.7(3) . . . ?
N12 N11 U1 120.1(3) . . . ?
C13 N12 N11 109.6(4) . . . ?
C13 N12 B1 127.3(4) . . . ?
N11 N12 B1 122.5(4) . . . ?
C25 N21 N22 106.1(4) . . . ?
C25 N21 U1 132.9(4) . . . ?
N22 N21 U1 121.0(3) . . . ?
C23 N22 N21 109.8(5) . . . ?
C23 N22 B1 128.6(5) . . . ?
N21 N22 B1 121.5(4) . . . ?
C35 N31 N32 106.5(4) . . . ?
C35 N31 U1 132.8(3) . . . ?
N32 N31 U1 115.1(3) . . . ?
C33 N32 N31 109.5(4) . . . ?
C33 N32 B1 127.7(4) . . . ?
N31 N32 B1 122.3(4) . . . ?
C45 N41 N42 107.2(4) . . . ?
C45 N41 U1 127.3(4) . . . ?
N42 N41 U1 123.7(3) . . . ?
C43 N42 N41 109.5(5) . . . ?
C43 N42 B2 128.3(5) . . . ?
N41 N42 B2 122.1(4) . . . ?
C55 N51 N52 106.6(4) . . . ?
C55 N51 U1 129.8(4) . . . ?
N52 N51 U1 122.1(3) . . . ?
C53 N52 N51 110.1(5) . . . ?
C53 N52 B2 128.1(5) . . . ?
N51 N52 B2 121.8(4) . . . ?
C65 N61 N62 105.7(4) . . . ?
C65 N61 U1 134.7(4) . . . ?
N62 N61 U1 116.7(3) . . . ?
C63 N62 N61 110.3(5) . . . ?
C63 N62 B2 127.0(5) . . . ?
N61 N62 B2 122.3(5) . . . ?
N12 C13 C14 108.1(5) . . . ?
N12 C13 C16 123.8(5) . . . ?
C14 C13 C16 127.9(5) . . . ?
C13 C14 C15 106.0(5) . . . ?
C13 C14 H14 127.00 . . . ?
C15 C14 H14 127.00 . . . ?
N11 C15 C14 110.2(5) . . . ?
N11 C15 C17 120.7(5) . . . ?
C14 C15 C17 129.0(5) . . . ?
C13 C16 H16A 109.50 . . . ?
C13 C16 H16B 109.50 . . . ?
H16A C16 H16B 109.50 . . . ?
C13 C16 H16C 109.50 . . . ?
H16A C16 H16C 109.50 . . . ?
H16B C16 H16C 109.50 . . . ?
C15 C17 H17A 109.50 . . . ?
C15 C17 H17B 109.50 . . . ?
H17A C17 H17B 109.50 . . . ?
C15 C17 H17C 109.50 . . . ?
H17A C17 H17C 109.50 . . . ?
H17B C17 H17C 109.50 . . . ?
N22 C23 C24 107.3(5) . . . ?
N22 C23 C26 123.0(5) . . . ?
C24 C23 C26 129.7(5) . . . ?
C23 C24 C25 106.5(5) . . . ?
C23 C24 H24 126.80 . . . ?
C25 C24 H24 126.80 . . . ?
N21 C25 C24 110.4(5) . . . ?
N21 C25 C27 123.0(5) . . . ?
C24 C25 C27 126.7(5) . . . ?
C23 C26 H26A 109.50 . . . ?
C23 C26 H26B 109.50 . . . ?
H26A C26 H26B 109.50 . . . ?
C23 C26 H26C 109.50 . . . ?
H26A C26 H26C 109.50 . . . ?
H26B C26 H26C 109.50 . . . ?
C25 C27 H27A 109.50 . . . ?
C25 C27 H27B 109.50 . . . ?
H27A C27 H27B 109.50 . . . ?
C25 C27 H27C 109.50 . . . ?
H27A C27 H27C 109.50 . . . ?
H27B C27 H27C 109.50 . . . ?
N32 C33 C34 107.9(5) . . . ?
N32 C33 C36 123.1(5) . . . ?
C34 C33 C36 129.0(5) . . . ?
C33 C34 C35 105.6(5) . . . ?
C33 C34 H34 127.20 . . . ?
C35 C34 H34 127.20 . . . ?
N31 C35 C34 110.4(5) . . . ?
N31 C35 C37 123.8(5) . . . ?
C34 C35 C37 125.7(5) . . . ?
C33 C36 H36A 109.50 . . . ?
C33 C36 H36B 109.50 . . . ?
H36A C36 H36B 109.50 . . . ?
C33 C36 H36C 109.50 . . . ?
H36A C36 H36C 109.50 . . . ?
H36B C36 H36C 109.50 . . . ?
C35 C37 H37A 109.50 . . . ?
C35 C37 H37B 109.50 . . . ?
H37A C37 H37B 109.50 . . . ?
C35 C37 H37C 109.50 . . . ?
H37A C37 H37C 109.50 . . . ?
H37B C37 H37C 109.50 . . . ?
N42 C43 C44 108.0(5) . . . ?
N42 C43 C46 123.7(6) . . . ?
C44 C43 C46 128.3(5) . . . ?
C43 C44 C45 106.1(5) . . . ?
C43 C44 H44 127.00 . . . ?
C45 C44 H44 127.00 . . . ?
N41 C45 C44 109.2(5) . . . ?
N41 C45 C47 120.9(5) . . . ?
C44 C45 C47 129.9(5) . . . ?
C43 C46 H46A 109.50 . . . ?
C43 C46 H46B 109.50 . . . ?
H46A C46 H46B 109.50 . . . ?
C43 C46 H46C 109.50 . . . ?
H46A C46 H46C 109.50 . . . ?
H46B C46 H46C 109.50 . . . ?
C45 C47 H47A 109.50 . . . ?
C45 C47 H47B 109.50 . . . ?
H47A C47 H47B 109.50 . . . ?
C45 C47 H47C 109.50 . . . ?
H47A C47 H47C 109.50 . . . ?
H47B C47 H47C 109.50 . . . ?
N52 C53 C54 107.2(5) . . . ?
N52 C53 C56 123.2(6) . . . ?
C54 C53 C56 129.5(5) . . . ?
C53 C54 C55 106.5(5) . . . ?
C53 C54 H54 126.70 . . . ?
C55 C54 H54 126.70 . . . ?
N51 C55 C54 109.6(5) . . . ?
N51 C55 C57 123.2(5) . . . ?
C54 C55 C57 127.2(5) . . . ?
C53 C56 H56A 109.50 . . . ?
C53 C56 H56B 109.50 . . . ?
H56A C56 H56B 109.50 . . . ?
C53 C56 H56C 109.50 . . . ?
H56A C56 H56C 109.50 . . . ?
H56B C56 H56C 109.50 . . . ?
C55 C57 H57A 109.50 . . . ?
C55 C57 H57B 109.50 . . . ?
H57A C57 H57B 109.50 . . . ?
C55 C57 H57C 109.50 . . . ?
H57A C57 H57C 109.50 . . . ?
H57B C57 H57C 109.50 . . . ?
N62 C63 C64 107.8(5) . . . ?
N62 C63 C66 125.3(5) . . . ?
C64 C63 C66 126.9(6) . . . ?
C63 C64 C65 105.8(5) . . . ?
C63 C64 H64 127.10 . . . ?
C65 C64 H64 127.10 . . . ?
N61 C65 C64 110.4(5) . . . ?
N61 C65 C67 123.3(5) . . . ?
C64 C65 C67 126.3(5) . . . ?
C63 C66 H66A 109.50 . . . ?
C63 C66 H66B 109.50 . . . ?
H66A C66 H66B 109.50 . . . ?
C63 C66 H66C 109.50 . . . ?
H66A C66 H66C 109.50 . . . ?
H66B C66 H66C 109.50 . . . ?
C65 C67 H67A 109.50 . . . ?
C65 C67 H67B 109.50 . . . ?
H67A C67 H67B 109.50 . . . ?
C65 C67 H67C 109.50 . . . ?
H67A C67 H67C 109.50 . . . ?
H67B C67 H67C 109.50 . . . ?
C92 C91 H91A 109.50 . . . ?
C92 C91 H91B 109.50 . . . ?
H91A C91 H91B 109.50 . . . ?
C92 C91 H91C 109.50 . . . ?
H91A C91 H91C 109.50 . . . ?
H91B C91 H91C 109.50 . . . ?
O93 C92 C91 109.0(6) . . . ?
O93 C92 H92A 109.90 . . . ?
C91 C92 H92A 109.90 . . . ?
O93 C92 H92B 109.90 . . . ?
C91 C92 H92B 109.90 . . . ?
H92A C92 H92B 108.30 . . . ?
O93 C94 C95 109.2(8) . . . ?
O93 C94 H94A 109.80 . . . ?
C95 C94 H94A 109.80 . . . ?
O93 C94 H94B 109.80 . . . ?
C95 C94 H94B 109.80 . . . ?
H94A C94 H94B 108.30 . . . ?
C94 C95 H95A 109.50 . . . ?
C94 C95 H95B 109.50 . . . ?
H95A C95 H95B 109.50 . . . ?
C94 C95 H95C 109.50 . . . ?
H95A C95 H95C 109.50 . . . ?
H95B C95 H95C 109.50 . . . ?
N22 B1 N32 109.6(4) . . . ?
N22 B1 N12 111.3(5) . . . ?
N32 B1 N12 111.1(4) . . . ?
N22 B1 H1 112(4) . . . ?
N32 B1 H1 109(4) . . . ?
N12 B1 H1 104(4) . . . ?
N62 B2 N52 108.4(4) . . . ?
N62 B2 N42 111.7(4) . . . ?
N52 B2 N42 110.8(5) . . . ?
N62 B2 H2 114(4) . . . ?
N52 B2 H2 110(4) . . . ?
N42 B2 H2 102(3) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.863(4) . . ?
U1 N41 2.532(4) . . ?
U1 N11 2.541(4) . . ?
U1 N51 2.635(4) . . ?
U1 N21 2.645(4) . . ?
U1 N31 2.714(4) . . ?
U1 N61 2.774(4) . . ?
O93 C94 1.417(10) . . ?
O93 C92 1.422(9) . . ?
N11 C15 1.347(7) . . ?
N11 N12 1.378(6) . . ?
N12 C13 1.351(6) . . ?
N12 B1 1.563(7) . . ?
N21 C25 1.335(7) . . ?
N21 N22 1.385(6) . . ?
N22 C23 1.355(7) . . ?
N22 B1 1.520(8) . . ?
N31 C35 1.335(7) . . ?
N31 N32 1.384(6) . . ?
N32 C33 1.368(7) . . ?
N32 B1 1.549(8) . . ?
N41 C45 1.343(7) . . ?
N41 N42 1.367(6) . . ?
N42 C43 1.346(7) . . ?
N42 B2 1.560(8) . . ?
N51 C55 1.331(7) . . ?
N51 N52 1.374(7) . . ?
N52 C53 1.348(7) . . ?
N52 B2 1.547(8) . . ?
N61 C65 1.337(7) . . ?
N61 N62 1.388(6) . . ?
N62 C63 1.336(8) . . ?
N62 B2 1.540(7) . . ?
C13 C14 1.375(8) . . ?
C13 C16 1.502(7) . . ?
C14 C15 1.384(8) . . ?
C14 H14 0.9500 . . ?
C15 C17 1.503(8) . . ?
C16 H16A 0.9800 . . ?
C16 H16B 0.9800 . . ?
C16 H16C 0.9800 . . ?
C17 H17A 0.9800 . . ?
C17 H17B 0.9800 . . ?
C17 H17C 0.9800 . . ?
C23 C24 1.376(8) . . ?
C23 C26 1.502(8) . . ?
C24 C25 1.386(8) . . ?
C24 H24 0.9500 . . ?
C25 C27 1.512(8) . . ?
C26 H26A 0.9800 . . ?
C26 H26B 0.9800 . . ?
C26 H26C 0.9800 . . ?
C27 H27A 0.9800 . . ?
C27 H27B 0.9800 . . ?
C27 H27C 0.9800 . . ?
C33 C34 1.377(8) . . ?
C33 C36 1.490(8) . . ?
C34 C35 1.409(8) . . ?
C34 H34 0.9500 . . ?
C35 C37 1.491(7) . . ?
C36 H36A 0.9800 . . ?
C36 H36B 0.9800 . . ?
C36 H36C 0.9800 . . ?
C37 H37A 0.9800 . . ?
C37 H37B 0.9800 . . ?
C37 H37C 0.9800 . . ?
C43 C44 1.380(9) . . ?
C43 C46 1.486(9) . . ?
C44 C45 1.390(9) . . ?
C44 H44 0.9500 . . ?
C45 C47 1.492(9) . . ?
C46 H46A 0.9800 . . ?
C46 H46B 0.9800 . . ?
C46 H46C 0.9800 . . ?
C47 H47A 0.9800 . . ?
C47 H47B 0.9800 . . ?
C47 H47C 0.9800 . . ?
C53 C54 1.372(9) . . ?
C53 C56 1.491(9) . . ?
C54 C55 1.393(8) . . ?
C54 H54 0.9500 . . ?
C55 C57 1.495(9) . . ?
C56 H56A 0.9800 . . ?
C56 H56B 0.9800 . . ?
C56 H56C 0.9800 . . ?
C57 H57A 0.9800 . . ?
C57 H57B 0.9800 . . ?
C57 H57C 0.9800 . . ?
C63 C64 1.382(8) . . ?
C63 C66 1.484(9) . . ?
C64 C65 1.393(9) . . ?
C64 H64 0.9500 . . ?
C65 C67 1.496(8) . . ?
C66 H66A 0.9800 . . ?
C66 H66B 0.9800 . . ?
C66 H66C 0.9800 . . ?
C67 H67A 0.9800 . . ?
C67 H67B 0.9800 . . ?
C67 H67C 0.9800 . . ?
C91 C92 1.463(12) . . ?
C91 H91A 0.9800 . . ?
C91 H91B 0.9800 . . ?
C91 H91C 0.9800 . . ?
C92 H92A 0.9900 . . ?
C92 H92B 0.9900 . . ?
C94 C95 1.502(14) . . ?
C94 H94A 0.9900 . . ?
C94 H94B 0.9900 . . ?
C95 H95A 0.9800 . . ?
C95 H95B 0.9800 . . ?
C95 H95C 0.9800 . . ?
B1 H1 0.97(7) . . ?
B2 H2 1.05(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 U1 N11 C15 -67.5(5) . . . . ?
N41 U1 N11 C15 99.3(6) . . . . ?
N51 U1 N11 C15 13.1(5) . . . . ?
N21 U1 N11 C15 -140.5(5) . . . . ?
N31 U1 N11 C15 150.0(5) . . . . ?
N61 U1 N11 C15 78.3(5) . . . . ?
O1 U1 N11 N12 93.6(4) . . . . ?
N41 U1 N11 N12 -99.7(4) . . . . ?
N51 U1 N11 N12 174.1(4) . . . . ?
N21 U1 N11 N12 20.6(4) . . . . ?
N31 U1 N11 N12 -48.9(4) . . . . ?
N61 U1 N11 N12 -120.7(4) . . . . ?
C15 N11 N12 C13 1.6(6) . . . . ?
U1 N11 N12 C13 -163.8(3) . . . . ?
C15 N11 N12 B1 -169.7(5) . . . . ?
U1 N11 N12 B1 24.9(6) . . . . ?
O1 U1 N21 C25 35.9(5) . . . . ?
N41 U1 N21 C25 -60.5(5) . . . . ?
N11 U1 N21 C25 144.8(5) . . . . ?
N51 U1 N21 C25 43.9(6) . . . . ?
N31 U1 N21 C25 -135.1(5) . . . . ?
N61 U1 N21 C25 -152.9(4) . . . . ?
O1 U1 N21 N22 -144.5(4) . . . . ?
N41 U1 N21 N22 119.1(4) . . . . ?
N11 U1 N21 N22 -35.6(4) . . . . ?
N51 U1 N21 N22 -136.5(4) . . . . ?
N31 U1 N21 N22 44.5(3) . . . . ?
N61 U1 N21 N22 26.7(4) . . . . ?
C25 N21 N22 C23 0.1(6) . . . . ?
U1 N21 N22 C23 -179.6(3) . . . . ?
C25 N21 N22 B1 -176.3(5) . . . . ?
U1 N21 N22 B1 4.0(6) . . . . ?
O1 U1 N31 C35 135.0(5) . . . . ?
N41 U1 N31 C35 31.8(4) . . . . ?
N11 U1 N31 C35 -127.6(5) . . . . ?
N51 U1 N31 C35 -29.4(5) . . . . ?
N21 U1 N31 C35 149.9(5) . . . . ?
N61 U1 N31 C35 -43.2(4) . . . . ?
O1 U1 N31 N32 -75.6(5) . . . . ?
N41 U1 N31 N32 -178.8(3) . . . . ?
N11 U1 N31 N32 21.7(3) . . . . ?
N51 U1 N31 N32 120.0(3) . . . . ?
N21 U1 N31 N32 -60.7(3) . . . . ?
N61 U1 N31 N32 106.2(3) . . . . ?
C35 N31 N32 C33 -0.2(5) . . . . ?
U1 N31 N32 C33 -157.2(3) . . . . ?
C35 N31 N32 B1 -172.6(4) . . . . ?
U1 N31 N32 B1 30.3(5) . . . . ?
O1 U1 N41 C45 -63.8(5) . . . . ?
N11 U1 N41 C45 129.3(5) . . . . ?
N51 U1 N41 C45 -136.9(5) . . . . ?
N21 U1 N41 C45 17.0(5) . . . . ?
N31 U1 N41 C45 80.3(5) . . . . ?
N61 U1 N41 C45 150.8(5) . . . . ?
O1 U1 N41 N42 99.0(4) . . . . ?
N11 U1 N41 N42 -68.0(5) . . . . ?
N51 U1 N41 N42 25.9(4) . . . . ?
N21 U1 N41 N42 179.8(4) . . . . ?
N31 U1 N41 N42 -117.0(4) . . . . ?
N61 U1 N41 N42 -46.5(4) . . . . ?
C45 N41 N42 C43 0.6(6) . . . . ?
U1 N41 N42 C43 -165.1(4) . . . . ?
C45 N41 N42 B2 -174.4(5) . . . . ?
U1 N41 N42 B2 19.9(6) . . . . ?
O1 U1 N51 C55 47.4(5) . . . . ?
N41 U1 N51 C55 152.8(5) . . . . ?
N11 U1 N51 C55 -55.1(5) . . . . ?
N21 U1 N51 C55 39.4(6) . . . . ?
N31 U1 N51 C55 -142.0(4) . . . . ?
N61 U1 N51 C55 -128.1(5) . . . . ?
O1 U1 N51 N52 -148.7(4) . . . . ?
N41 U1 N51 N52 -43.3(4) . . . . ?
N11 U1 N51 N52 108.8(4) . . . . ?
N21 U1 N51 N52 -156.7(3) . . . . ?
N31 U1 N51 N52 21.9(5) . . . . ?
N61 U1 N51 N52 35.8(4) . . . . ?
C55 N51 N52 C53 0.5(6) . . . . ?
U1 N51 N52 C53 -166.7(3) . . . . ?
C55 N51 N52 B2 -178.6(5) . . . . ?
U1 N51 N52 B2 14.2(6) . . . . ?
O1 U1 N61 C65 140.1(5) . . . . ?
N41 U1 N61 C65 -133.2(5) . . . . ?
N11 U1 N61 C65 37.2(5) . . . . ?
N51 U1 N61 C65 147.9(5) . . . . ?
N21 U1 N61 C65 -24.3(5) . . . . ?
N31 U1 N61 C65 -41.8(5) . . . . ?
O1 U1 N61 N62 -62.6(5) . . . . ?
N41 U1 N61 N62 24.1(3) . . . . ?
N11 U1 N61 N62 -165.5(3) . . . . ?
N51 U1 N61 N62 -54.8(3) . . . . ?
N21 U1 N61 N62 133.0(3) . . . . ?
N31 U1 N61 N62 115.5(3) . . . . ?
C65 N61 N62 C63 0.8(5) . . . . ?
U1 N61 N62 C63 -162.6(3) . . . . ?
C65 N61 N62 B2 -172.3(5) . . . . ?
U1 N61 N62 B2 24.3(6) . . . . ?
N11 N12 C13 C14 -1.1(6) . . . . ?
B1 N12 C13 C14 169.7(5) . . . . ?
N11 N12 C13 C16 174.3(5) . . . . ?
B1 N12 C13 C16 -15.0(9) . . . . ?
N12 C13 C14 C15 0.2(6) . . . . ?
C16 C13 C14 C15 -175.0(5) . . . . ?
N12 N11 C15 C14 -1.5(6) . . . . ?
U1 N11 C15 C14 161.5(4) . . . . ?
N12 N11 C15 C17 177.7(6) . . . . ?
U1 N11 C15 C17 -19.3(9) . . . . ?
C13 C14 C15 N11 0.9(7) . . . . ?
C13 C14 C15 C17 -178.2(6) . . . . ?
N21 N22 C23 C24 -0.5(6) . . . . ?
B1 N22 C23 C24 175.6(5) . . . . ?
N21 N22 C23 C26 179.1(5) . . . . ?
B1 N22 C23 C26 -4.7(9) . . . . ?
N22 C23 C24 C25 0.6(6) . . . . ?
C26 C23 C24 C25 -178.9(5) . . . . ?
N22 N21 C25 C24 0.3(6) . . . . ?
U1 N21 C25 C24 180.0(4) . . . . ?
N22 N21 C25 C27 179.8(5) . . . . ?
U1 N21 C25 C27 -0.5(8) . . . . ?
C23 C24 C25 N21 -0.6(7) . . . . ?
C23 C24 C25 C27 179.9(5) . . . . ?
N31 N32 C33 C34 -0.3(5) . . . . ?
B1 N32 C33 C34 171.7(5) . . . . ?
N31 N32 C33 C36 178.1(5) . . . . ?
B1 N32 C33 C36 -10.0(8) . . . . ?
N32 C33 C34 C35 0.6(6) . . . . ?
C36 C33 C34 C35 -177.6(5) . . . . ?
N32 N31 C35 C34 0.5(5) . . . . ?
U1 N31 C35 C34 151.8(4) . . . . ?
N32 N31 C35 C37 178.8(5) . . . . ?
U1 N31 C35 C37 -29.9(7) . . . . ?
C33 C34 C35 N31 -0.7(6) . . . . ?
C33 C34 C35 C37 -179.0(5) . . . . ?
N41 N42 C43 C44 -1.2(6) . . . . ?
B2 N42 C43 C44 173.4(5) . . . . ?
N41 N42 C43 C46 179.0(5) . . . . ?
B2 N42 C43 C46 -6.4(9) . . . . ?
N42 C43 C44 C45 1.3(7) . . . . ?
C46 C43 C44 C45 -178.9(6) . . . . ?
N42 N41 C45 C44 0.2(6) . . . . ?
U1 N41 C45 C44 165.3(4) . . . . ?
N42 N41 C45 C47 179.1(6) . . . . ?
U1 N41 C45 C47 -15.8(8) . . . . ?
C43 C44 C45 N41 -0.9(7) . . . . ?
C43 C44 C45 C47 -179.7(7) . . . . ?
N51 N52 C53 C54 0.2(6) . . . . ?
B2 N52 C53 C54 179.2(5) . . . . ?
N51 N52 C53 C56 179.0(5) . . . . ?
B2 N52 C53 C56 -2.0(9) . . . . ?
N52 C53 C54 C55 -0.8(6) . . . . ?
C56 C53 C54 C55 -179.5(6) . . . . ?
N52 N51 C55 C54 -1.0(6) . . . . ?
U1 N51 C55 C54 164.9(4) . . . . ?
N52 N51 C55 C57 176.7(5) . . . . ?
U1 N51 C55 C57 -17.5(8) . . . . ?
C53 C54 C55 N51 1.1(6) . . . . ?
C53 C54 C55 C57 -176.4(6) . . . . ?
N61 N62 C63 C64 0.3(6) . . . . ?
B2 N62 C63 C64 173.0(5) . . . . ?
N61 N62 C63 C66 -178.0(5) . . . . ?
B2 N62 C63 C66 -5.3(9) . . . . ?
N62 C63 C64 C65 -1.3(6) . . . . ?
C66 C63 C64 C65 177.0(6) . . . . ?
N62 N61 C65 C64 -1.6(5) . . . . ?
U1 N61 C65 C64 157.4(4) . . . . ?
N62 N61 C65 C67 176.7(5) . . . . ?
U1 N61 C65 C67 -24.3(8) . . . . ?
C63 C64 C65 N61 1.8(6) . . . . ?
C63 C64 C65 C67 -176.4(5) . . . . ?
C94 O93 C92 C91 -179.1(7) . . . . ?
C92 O93 C94 C95 176.7(7) . . . . ?
C23 N22 B1 N32 117.7(6) . . . . ?
N21 N22 B1 N32 -66.6(6) . . . . ?
C23 N22 B1 N12 -119.0(6) . . . . ?
N21 N22 B1 N12 56.7(6) . . . . ?
C33 N32 B1 N22 -126.9(5) . . . . ?
N31 N32 B1 N22 44.1(6) . . . . ?
C33 N32 B1 N12 109.8(5) . . . . ?
N31 N32 B1 N12 -79.2(5) . . . . ?
C13 N12 B1 N22 112.7(6) . . . . ?
N11 N12 B1 N22 -77.6(6) . . . . ?
C13 N12 B1 N32 -124.9(5) . . . . ?
N11 N12 B1 N32 44.8(6) . . . . ?
C63 N62 B2 N52 -124.6(6) . . . . ?
N61 N62 B2 N52 47.3(6) . . . . ?
C63 N62 B2 N42 113.0(6) . . . . ?
N61 N62 B2 N42 -75.1(6) . . . . ?
C53 N52 B2 N62 107.0(6) . . . . ?
N51 N52 B2 N62 -74.1(6) . . . . ?
C53 N52 B2 N42 -130.1(5) . . . . ?
N51 N52 B2 N42 48.8(6) . . . . ?
C43 N42 B2 N62 -124.3(6) . . . . ?
N41 N42 B2 N62 49.7(7) . . . . ?
C43 N42 B2 N52 114.7(6) . . . . ?
N41 N42 B2 N52 -71.3(6) . . . . ?
