# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_po17030_refinalized
_database_code_depnum_ccdc_archive 'CCDC 1886802'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.67(C108 H132 B6 O6 U2), 1.33(C6 H14)'
_chemical_formula_sum            'C80 H106.67 B4 O4 U1.33'
_chemical_formula_weight         1492.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C108 H132 B6 O6 U2'
_chemical_oxdiff_usercomment     '@ 120 K LP_01_12'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   13.8450(2)
_cell_length_b                   14.9545(2)
_cell_length_c                   31.6940(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.5210(10)
_cell_angle_gamma                90
_cell_volume                     6519.63(15)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    39951
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      26.8230
_cell_measurement_theta_min      3.2570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -2 44 0.1331
-10 -2 40 0.1353
-19 -1 8 0.1059
-5 2 -42 0.1445
19 1 0 0.0939
12 1 31 0.1448
-2 21 -5 0.0653
-12 -1 -31 0.1349
0 -21 -1 0.0787
-4 10 39 0.1305
-11 12 28 0.1197
-17 11 4 0.1069
17 -10 -3 0.1062
-6 -5 -40 0.1401

_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.168
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.4458 -2.1886 44.0283 -0.0799 -0.6176 0.7824
-10.2168 -2.3883 40.1423 -0.1227 -0.9399 0.3186
-19.4424 -1.1300 8.2072 -0.1066 -0.8077 -0.5798
-4.8784 1.8998 -41.5350 0.0544 0.4245 -0.9038
19.3781 0.7112 0.1081 0.0908 0.6858 0.7221
12.4689 1.0501 30.8514 -0.0973 0.0218 0.9950
-1.9736 20.8084 -5.0539 -0.9508 0.2279 -0.2099
-12.4719 -0.9343 -30.8598 0.0920 -0.0205 -0.9956
-0.2836 -21.0785 -0.5303 0.9721 -0.2328 0.0300
-4.0232 10.0005 38.9853 -0.6493 -0.5714 0.5001
-11.0216 11.9851 27.9661 -0.7397 -0.6427 0.0443
-17.0126 10.9690 3.9507 -0.6310 -0.5315 -0.5914
17.0110 -9.9688 -2.9517 0.5807 0.5286 0.6062
-5.9813 -5.0194 -40.0131 0.3600 0.2892 -0.9023

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            139328
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.743
_diffrn_reflns_theta_min         2.800
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00 -26.50   0.75    5.00    --   -9.43 104.00  62.36   34
  2  ω    -20.00  27.25   0.75    5.00    --   -9.43 -99.00 150.00   63
  3  ω    -67.00   0.50   0.75    5.00    --   -9.43 -77.00 -90.00   90
  4  ω    -20.00   5.50   0.75    5.00    --   -9.43 -99.00   0.00   34
  5  ω    -79.00 -20.50   0.75    5.00    --   -9.43 -57.00  60.00   78
  6  ω    -84.00 -40.50   0.75    5.00    --   -9.43 155.00   7.53   58
  7  ω    -19.00  28.25   0.75    5.00    --   -9.43 -99.00 -90.00   63
  8  ω      2.00  48.50   0.75    5.00    --   -9.43  57.00-150.00   62
  9  ω     18.00  45.00   0.75    5.00    --   10.84-128.00  22.96   36
 10  ω    -58.00 -31.00   0.75    5.00    --   10.84 -57.00 150.00   36
 11  ω     52.00  79.00   0.75    5.00    --   10.84  57.00  60.00   36
 12  ω     20.00  78.50   0.75    5.00    --   10.84  57.00 -90.00   78
 13  ω     12.00  39.00   0.75    5.00    --   10.84  57.00  30.00   36
 14  ω     22.00  84.25   0.75    5.00    --   10.84  77.00 -30.00   83
 15  ω     23.00  50.00   0.75    5.00    --   10.84 -99.00  90.00   36
 16  ω    -37.00 -10.00   0.75    5.00    --   10.84 -57.00   0.00   36
 17  ω     59.00  84.50   0.75    5.00    --   10.84  77.00   0.00   34
 18  ω    -52.25  37.00   0.75    5.00    --   10.84 -57.00-180.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064000000
_diffrn_orient_matrix_UB_12      -0.0460979000
_diffrn_orient_matrix_UB_13      -0.0041706000
_diffrn_orient_matrix_UB_21      0.0350691000
_diffrn_orient_matrix_UB_22      0.0109186000
_diffrn_orient_matrix_UB_23      -0.0138397000
_diffrn_orient_matrix_UB_31      0.0372522000
_diffrn_orient_matrix_UB_32      -0.0023592000
_diffrn_orient_matrix_UB_33      0.0172765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13836
_reflns_number_total             17270
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         17270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+6.2846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0752
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C01Q(H01A,H01B), C32(H32A,H32B), C01V(H01F,H01G), C027(H02A,H02B)
2.b Aromatic/amide H refined with riding coordinates:
 C333(H333), C335(H335), C225(H225), C124(H124), C113(H113), C223(H223),
 C115(H115), C232(H232), C234(H234), C122(H122), C342(H342), C344(H344)
2.c Idealised Me refined as rotating group:
 C348(H34A,H34B,H34C), C339(H33A,H33B,H33C), C128(H12A,H12B,H12C), C119(H11A,
 H11B,H11C), C229(H22A,H22B,H22C), C117(H11D,H11E,H11F), C236(H23A,H23B,H23C),
 C238(H23D,H23E,H23F), C337(H33D,H33E,H33F), C338(H33G,H33H,H33I), C228(H22D,
 H22E,H22F), C126(H12D,H12E,H12F), C227(H22G,H22H,H22I), C127(H12G,H12H,H12I),
 C346(H34D,H34E,H34F), C118(H11G,H11H,H11I), C237(H23G,H23H,H23I), C347(H34G,
 H34H,H34I), C01R(H01C,H01D,H01E), C01W(H01H,H01I,H01J)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.47251(2) 0.47789(2) 0.31009(2) 0.02061(4) Uani 1 1 d . . . . .
O1 O 0.55486(14) 0.37081(14) 0.34402(6) 0.0256(5) Uani 1 1 d . . . . .
O3 O 0.40181(14) 0.50242(13) 0.23305(6) 0.0233(4) Uani 1 1 d . . . . .
O2 O 0.45856(14) 0.58685(13) 0.35517(6) 0.0253(5) Uani 1 1 d . . . . .
C331 C 0.2783(2) 0.4491(2) 0.27650(9) 0.0258(7) Uani 1 1 d . . . . .
C332 C 0.3035(2) 0.3573(2) 0.28000(10) 0.0288(7) Uani 1 1 d . . . . .
C333 C 0.3043(2) 0.3130(2) 0.31871(10) 0.0296(7) Uani 1 1 d . . . . .
H333 H 0.321493 0.252906 0.320433 0.036 Uiso 1 1 calc R . . . .
C336 C 0.2482(2) 0.4917(2) 0.31264(9) 0.0264(7) Uani 1 1 d . . . . .
C221 C 0.3586(2) 0.6244(2) 0.41555(9) 0.0235(6) Uani 1 1 d . . . . .
C335 C 0.2511(2) 0.4450(2) 0.35096(9) 0.0282(7) Uani 1 1 d . . . . .
H335 H 0.232832 0.474387 0.374665 0.034 Uiso 1 1 calc R . . . .
C230 C 0.5009(2) 0.7368(2) 0.39017(9) 0.0254(6) Uani 1 1 d . . . . .
C334 C 0.2800(2) 0.3565(2) 0.35490(9) 0.0281(7) Uani 1 1 d . . . . .
C340 C 0.2318(2) 0.5677(3) 0.20817(9) 0.0332(8) Uani 1 1 d . . . . .
C112 C 0.5686(2) 0.2264(2) 0.43500(9) 0.0255(6) Uani 1 1 d . . . . .
C111 C 0.5633(2) 0.2330(2) 0.39041(9) 0.0240(6) Uani 1 1 d . . . . .
B3 B 0.3052(3) 0.5060(2) 0.23662(11) 0.0268(8) Uani 1 1 d . . . . .
C125 C 0.7610(2) 0.4221(2) 0.38945(9) 0.0263(7) Uani 1 1 d . . . . .
C222 C 0.2785(2) 0.6829(2) 0.41733(9) 0.0261(7) Uani 1 1 d . . . . .
C235 C 0.4974(2) 0.8010(2) 0.35728(10) 0.0299(7) Uani 1 1 d . . . . .
C226 C 0.3605(2) 0.5455(2) 0.43990(9) 0.0249(7) Uani 1 1 d . . . . .
C120 C 0.7269(2) 0.3359(2) 0.37720(9) 0.0222(6) Uani 1 1 d . . . . .
C348 C 0.3609(3) 0.6894(2) 0.20576(12) 0.0415(9) Uani 1 1 d . . . . .
H34A H 0.382550 0.674297 0.234727 0.062 Uiso 1 1 calc GR . . . .
H34B H 0.359059 0.753255 0.202664 0.062 Uiso 1 1 calc GR . . . .
H34C H 0.404872 0.664628 0.187545 0.062 Uiso 1 1 calc GR . . . .
C339 C 0.2129(2) 0.5872(2) 0.31016(10) 0.0334(8) Uani 1 1 d . . . . .
H33A H 0.259116 0.623779 0.297734 0.050 Uiso 1 1 calc GR . . . .
H33B H 0.205795 0.608548 0.338210 0.050 Uiso 1 1 calc GR . . . .
H33C H 0.151234 0.590005 0.292967 0.050 Uiso 1 1 calc GR . . . .
C128 C 0.6935(3) 0.4989(2) 0.39564(12) 0.0377(8) Uani 1 1 d . . . . .
H12A H 0.675070 0.527661 0.368863 0.057 Uiso 1 1 calc GR . . . .
H12B H 0.725987 0.541084 0.415186 0.057 Uiso 1 1 calc GR . . . .
H12C H 0.636492 0.476717 0.406804 0.057 Uiso 1 1 calc GR . . . .
C225 C 0.2854(2) 0.5266(2) 0.46451(9) 0.0284(7) Uani 1 1 d . . . . .
H225 H 0.289223 0.474835 0.480897 0.034 Uiso 1 1 calc R . . . .
C124 C 0.8605(2) 0.4390(2) 0.39680(10) 0.0333(7) Uani 1 1 d . . . . .
H124 H 0.881464 0.496046 0.405126 0.040 Uiso 1 1 calc R . . . .
C119 C 0.5059(3) 0.1657(2) 0.31831(10) 0.0378(8) Uani 1 1 d . . . . .
H11A H 0.503820 0.225742 0.307476 0.057 Uiso 1 1 calc GR . . . .
H11B H 0.449693 0.133525 0.306010 0.057 Uiso 1 1 calc GR . . . .
H11C H 0.563608 0.136508 0.311130 0.057 Uiso 1 1 calc GR . . . .
C224 C 0.2055(2) 0.5820(2) 0.46543(9) 0.0304(7) Uani 1 1 d . . . . .
B2 B 0.4406(2) 0.6461(2) 0.38537(10) 0.0237(7) Uani 1 1 d . . . . .
C345 C 0.2608(2) 0.6518(3) 0.19375(10) 0.0379(8) Uani 1 1 d . . . . .
B1 B 0.6128(2) 0.3152(2) 0.36903(10) 0.0227(7) Uani 1 1 d . . . . .
C113 C 0.5164(2) 0.1597(2) 0.45366(11) 0.0331(7) Uani 1 1 d . . . . .
H113 H 0.519700 0.157012 0.483107 0.040 Uiso 1 1 calc R . . . .
C229 C 0.4422(2) 0.4791(2) 0.44062(10) 0.0291(7) Uani 1 1 d . . . . .
H22A H 0.440704 0.451346 0.413235 0.044 Uiso 1 1 calc GR . . . .
H22B H 0.434796 0.434208 0.461672 0.044 Uiso 1 1 calc GR . . . .
H22C H 0.503119 0.509297 0.447398 0.044 Uiso 1 1 calc GR . . . .
C116 C 0.5070(2) 0.1680(2) 0.36600(10) 0.0292(7) Uani 1 1 d . . . . .
C117 C 0.6291(2) 0.2911(2) 0.46331(10) 0.0309(7) Uani 1 1 d . . . . .
H11D H 0.695298 0.288928 0.457030 0.046 Uiso 1 1 calc GR . . . .
H11E H 0.626436 0.275098 0.492483 0.046 Uiso 1 1 calc GR . . . .
H11F H 0.604144 0.350580 0.458445 0.046 Uiso 1 1 calc GR . . . .
C236 C 0.5751(2) 0.6888(2) 0.46384(9) 0.0303(7) Uani 1 1 d . . . . .
H23A H 0.512185 0.669434 0.470116 0.045 Uiso 1 1 calc GR . . . .
H23B H 0.608897 0.716876 0.488467 0.045 Uiso 1 1 calc GR . . . .
H23C H 0.611694 0.638034 0.456029 0.045 Uiso 1 1 calc GR . . . .
C238 C 0.4301(3) 0.7901(3) 0.31653(11) 0.0412(9) Uani 1 1 d . . . . .
H23D H 0.404861 0.730254 0.314825 0.062 Uiso 1 1 calc GR . . . .
H23E H 0.465430 0.801311 0.292701 0.062 Uiso 1 1 calc GR . . . .
H23F H 0.377293 0.831805 0.316191 0.062 Uiso 1 1 calc GR . . . .
C223 C 0.2044(2) 0.6600(2) 0.44137(10) 0.0316(7) Uani 1 1 d . . . . .
H223 H 0.151681 0.698532 0.441412 0.038 Uiso 1 1 calc R . . . .
C115 C 0.4574(2) 0.1029(2) 0.38569(11) 0.0342(8) Uani 1 1 d . . . . .
H115 H 0.420888 0.061136 0.369014 0.041 Uiso 1 1 calc R . . . .
C231 C 0.5635(2) 0.7545(2) 0.42764(10) 0.0278(7) Uani 1 1 d . . . . .
C114 C 0.4602(2) 0.0978(2) 0.42958(11) 0.0360(8) Uani 1 1 d . . . . .
C337 C 0.3265(3) 0.3041(2) 0.24172(11) 0.0428(9) Uani 1 1 d . . . . .
H33D H 0.308600 0.338307 0.216389 0.064 Uiso 1 1 calc GR . . . .
H33E H 0.290521 0.249119 0.240272 0.064 Uiso 1 1 calc GR . . . .
H33F H 0.394805 0.291326 0.244233 0.064 Uiso 1 1 calc GR . . . .
C232 C 0.6200(2) 0.8316(2) 0.43103(11) 0.0345(8) Uani 1 1 d . . . . .
H232 H 0.660933 0.841772 0.455921 0.041 Uiso 1 1 calc R . . . .
C234 C 0.5550(3) 0.8772(2) 0.36204(12) 0.0389(8) Uani 1 1 d . . . . .
H234 H 0.551426 0.918560 0.339989 0.047 Uiso 1 1 calc R . . . .
C122 C 0.8958(2) 0.2895(2) 0.37993(10) 0.0338(8) Uani 1 1 d . . . . .
H122 H 0.940856 0.244710 0.376556 0.041 Uiso 1 1 calc R . . . .
C338 C 0.2846(3) 0.3064(2) 0.39659(10) 0.0373(8) Uani 1 1 d . . . . .
H33G H 0.241738 0.255821 0.393370 0.056 Uiso 1 1 calc GR . . . .
H33H H 0.264986 0.345417 0.418136 0.056 Uiso 1 1 calc GR . . . .
H33I H 0.349898 0.286344 0.404698 0.056 Uiso 1 1 calc GR . . . .
C121 C 0.7976(2) 0.2694(2) 0.37253(10) 0.0294(7) Uani 1 1 d . . . . .
C228 C 0.1245(2) 0.5609(3) 0.49146(11) 0.0426(9) Uani 1 1 d . . . . .
H22D H 0.132871 0.501381 0.502683 0.064 Uiso 1 1 calc GR . . . .
H22E H 0.063417 0.564863 0.473925 0.064 Uiso 1 1 calc GR . . . .
H22F H 0.125453 0.602783 0.514440 0.064 Uiso 1 1 calc GR . . . .
C123 C 0.9292(2) 0.3735(3) 0.39210(10) 0.0352(8) Uani 1 1 d . . . . .
C126 C 0.7689(2) 0.1756(2) 0.35908(13) 0.0419(9) Uani 1 1 d . . . . .
H12D H 0.723143 0.152868 0.377001 0.063 Uiso 1 1 calc GR . . . .
H12E H 0.825582 0.138180 0.361543 0.063 Uiso 1 1 calc GR . . . .
H12F H 0.739691 0.176053 0.330122 0.063 Uiso 1 1 calc GR . . . .
C233 C 0.6173(3) 0.8937(2) 0.39835(12) 0.0390(8) Uani 1 1 d . . . . .
C227 C 0.2697(2) 0.7706(2) 0.39347(11) 0.0368(8) Uani 1 1 d . . . . .
H22G H 0.325876 0.806770 0.401898 0.055 Uiso 1 1 calc GR . . . .
H22H H 0.212355 0.801467 0.399857 0.055 Uiso 1 1 calc GR . . . .
H22I H 0.265351 0.759187 0.363505 0.055 Uiso 1 1 calc GR . . . .
C127 C 1.0365(2) 0.3945(3) 0.39979(13) 0.0525(11) Uani 1 1 d . . . . .
H12G H 1.045645 0.458111 0.400245 0.079 Uiso 1 1 calc GR . . . .
H12H H 1.069001 0.368931 0.377461 0.079 Uiso 1 1 calc GR . . . .
H12I H 1.063047 0.369661 0.426560 0.079 Uiso 1 1 calc GR . . . .
C346 C 0.0965(3) 0.4527(3) 0.21051(12) 0.0573(12) Uani 1 1 d . . . . .
H34D H 0.136165 0.405208 0.201601 0.086 Uiso 1 1 calc GR . . . .
H34E H 0.030689 0.444780 0.197909 0.086 Uiso 1 1 calc GR . . . .
H34F H 0.098502 0.451929 0.240884 0.086 Uiso 1 1 calc GR . . . .
C341 C 0.1346(2) 0.5414(3) 0.19655(11) 0.0455(10) Uani 1 1 d . . . . .
C118 C 0.4050(3) 0.0257(3) 0.45026(13) 0.0549(11) Uani 1 1 d . . . . .
H11G H 0.413684 0.033535 0.480517 0.082 Uiso 1 1 calc GR . . . .
H11H H 0.429257 -0.031963 0.443266 0.082 Uiso 1 1 calc GR . . . .
H11I H 0.337143 0.029691 0.440117 0.082 Uiso 1 1 calc GR . . . .
C237 C 0.6808(3) 0.9761(3) 0.40224(16) 0.0611(12) Uani 1 1 d . . . . .
H23G H 0.646538 1.024112 0.414133 0.092 Uiso 1 1 calc GR . . . .
H23H H 0.696596 0.993191 0.374644 0.092 Uiso 1 1 calc GR . . . .
H23I H 0.739455 0.963512 0.420410 0.092 Uiso 1 1 calc GR . . . .
C342 C 0.0720(3) 0.5975(4) 0.17081(13) 0.0638(15) Uani 1 1 d . . . . .
H342 H 0.008050 0.579456 0.163504 0.077 Uiso 1 1 calc R . . . .
C344 C 0.1951(3) 0.7044(3) 0.16796(12) 0.0537(11) Uani 1 1 d . . . . .
H344 H 0.215637 0.759353 0.158573 0.064 Uiso 1 1 calc R . . . .
C343 C 0.1014(4) 0.6778(4) 0.15599(13) 0.0694(15) Uani 1 1 d . . . . .
C347 C 0.0314(4) 0.7356(4) 0.12747(16) 0.111(3) Uani 1 1 d . . . . .
H34G H 0.016345 0.706729 0.100472 0.167 Uiso 1 1 calc GR . . . .
H34H H 0.060772 0.792650 0.123442 0.167 Uiso 1 1 calc GR . . . .
H34I H -0.027331 0.744015 0.140469 0.167 Uiso 1 1 calc GR . . . .
C01Q C -0.0313(4) 0.1471(4) 0.50074(19) 0.0918(18) Uani 1 1 d . . . . .
H01A H -0.042521 0.201366 0.516196 0.110 Uiso 1 1 calc R . . . .
H01B H -0.013176 0.101287 0.521838 0.110 Uiso 1 1 calc R . . . .
C01R C 0.1450(4) 0.2860(4) 0.5174(2) 0.0975(19) Uani 1 1 d . . . . .
H01C H 0.153979 0.330735 0.496490 0.146 Uiso 1 1 calc GR . . . .
H01D H 0.197879 0.288511 0.539737 0.146 Uiso 1 1 calc GR . . . .
H01E H 0.084884 0.296732 0.528978 0.146 Uiso 1 1 calc GR . . . .
C32 C 0.1420(4) 0.1949(5) 0.4970(2) 0.111(2) Uani 1 1 d . . . . .
H32A H 0.184807 0.195990 0.474800 0.133 Uiso 1 1 calc R . . . .
H32B H 0.168910 0.152258 0.518217 0.133 Uiso 1 1 calc R . . . .
C01V C -0.1272(4) 0.1199(5) 0.47778(19) 0.103(2) Uani 1 1 d . . . . .
H01F H -0.149036 0.167317 0.458115 0.124 Uiso 1 1 calc R . . . .
H01G H -0.116756 0.067236 0.460989 0.124 Uiso 1 1 calc R . . . .
C01W C -0.2043(3) 0.1005(4) 0.50296(15) 0.0753(14) Uani 1 1 d . . . . .
H01H H -0.263651 0.091166 0.484662 0.113 Uiso 1 1 calc GR . . . .
H01I H -0.212333 0.149764 0.521647 0.113 Uiso 1 1 calc GR . . . .
H01J H -0.188714 0.047463 0.519422 0.113 Uiso 1 1 calc GR . . . .
C027 C 0.0515(5) 0.1628(6) 0.4793(3) 0.178(4) Uani 1 1 d . . . . .
H02A H 0.064736 0.106455 0.465940 0.214 Uiso 1 1 calc R . . . .
H02B H 0.030042 0.203676 0.456375 0.214 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 U1 3.9682(2) 2_655 ?
U1 O1 2.177(2) . ?
U1 O3 2.5519(19) . ?
U1 O3 2.360(2) 2_655 ?
U1 O2 2.190(2) . ?
U1 C331 2.811(3) . ?
U1 C332 3.022(3) . ?
O1 B1 1.349(4) . ?
O3 B3 1.356(4) . ?
O2 B2 1.348(4) . ?
C331 C332 1.417(4) . ?
C331 C336 1.414(4) . ?
C331 B3 1.603(5) . ?
C332 C333 1.393(4) . ?
C332 C337 1.514(4) . ?
C333 C334 1.393(4) . ?
C336 C335 1.398(4) . ?
C336 C339 1.509(5) . ?
C221 C222 1.419(4) . ?
C221 C226 1.408(4) . ?
C221 B2 1.599(4) . ?
C335 C334 1.383(5) . ?
C230 C235 1.414(4) . ?
C230 B2 1.591(5) . ?
C230 C231 1.413(4) . ?
C334 C338 1.514(4) . ?
C340 B3 1.578(5) . ?
C340 C345 1.412(5) . ?
C340 C341 1.410(5) . ?
C112 C111 1.410(4) . ?
C112 C113 1.402(4) . ?
C112 C117 1.507(4) . ?
C111 B1 1.595(4) . ?
C111 C116 1.419(4) . ?
C125 C120 1.412(4) . ?
C125 C128 1.506(5) . ?
C125 C124 1.394(4) . ?
C222 C223 1.388(4) . ?
C222 C227 1.512(4) . ?
C235 C238 1.513(5) . ?
C235 C234 1.390(5) . ?
C226 C225 1.398(4) . ?
C226 C229 1.503(4) . ?
C120 B1 1.602(4) . ?
C120 C121 1.415(4) . ?
C348 C345 1.503(5) . ?
C225 C224 1.385(4) . ?
C124 C123 1.384(5) . ?
C119 C116 1.510(4) . ?
C224 C223 1.393(5) . ?
C224 C228 1.499(4) . ?
C345 C344 1.394(5) . ?
C113 C114 1.382(5) . ?
C116 C115 1.381(4) . ?
C236 C231 1.506(4) . ?
C115 C114 1.390(5) . ?
C231 C232 1.390(4) . ?
C114 C118 1.513(5) . ?
C232 C233 1.389(5) . ?
C234 C233 1.380(5) . ?
C122 C121 1.386(4) . ?
C122 C123 1.378(5) . ?
C121 C126 1.506(5) . ?
C123 C127 1.511(4) . ?
C233 C237 1.510(5) . ?
C346 C341 1.512(6) . ?
C341 C342 1.399(6) . ?
C342 C343 1.368(7) . ?
C344 C343 1.369(7) . ?
C343 C347 1.518(6) . ?
C01Q C01V 1.497(7) . ?
C01Q C027 1.416(8) . ?
C01R C32 1.506(8) . ?
C32 C027 1.399(9) . ?
C01V C01W 1.434(7) . ?

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
O1 U1 U1 109.10(5) . 2_655 ?
O1 U1 O3 134.48(7) . . ?
O1 U1 O3 91.22(7) . 2_655 ?
O1 U1 O2 107.76(7) . . ?
O1 U1 C331 119.94(8) . . ?
O1 U1 C332 93.46(8) . . ?
O3 U1 U1 34.52(4) . 2_655 ?
O3 U1 U1 37.78(5) 2_655 2_655 ?
O3 U1 O3 69.59(7) 2_655 . ?
O3 U1 C331 122.74(8) 2_655 . ?
O3 U1 C331 54.06(8) . . ?
O3 U1 C332 120.35(7) 2_655 . ?
O3 U1 C332 65.46(8) . . ?
O2 U1 U1 131.83(5) . 2_655 ?
O2 U1 O3 112.81(7) . 2_655 ?
O2 U1 O3 117.68(7) . . ?
O2 U1 C331 102.11(8) . . ?
O2 U1 C332 121.83(8) . . ?
C331 U1 U1 85.18(6) . 2_655 ?
C331 U1 C332 27.82(9) . . ?
C332 U1 U1 85.59(6) . 2_655 ?
B1 O1 U1 170.7(2) . . ?
U1 O3 U1 107.70(7) 2_655 . ?
B3 O3 U1 101.57(18) . . ?
B3 O3 U1 148.59(19) . 2_655 ?
B2 O2 U1 171.6(2) . . ?
C332 C331 U1 84.42(17) . . ?
C332 C331 B3 120.0(3) . . ?
C336 C331 U1 88.91(17) . . ?
C336 C331 C332 117.7(3) . . ?
C336 C331 B3 121.0(3) . . ?
B3 C331 U1 85.35(17) . . ?
C331 C332 U1 67.76(15) . . ?
C331 C332 C337 121.2(3) . . ?
C333 C332 U1 94.42(19) . . ?
C333 C332 C331 120.4(3) . . ?
C333 C332 C337 118.4(3) . . ?
C337 C332 U1 109.9(2) . . ?
C334 C333 C332 121.6(3) . . ?
C331 C336 C339 120.5(3) . . ?
C335 C336 C331 119.8(3) . . ?
C335 C336 C339 119.7(3) . . ?
C222 C221 B2 120.7(3) . . ?
C226 C221 C222 117.4(3) . . ?
C226 C221 B2 121.9(3) . . ?
C334 C335 C336 122.4(3) . . ?
C235 C230 B2 122.3(3) . . ?
C231 C230 C235 117.3(3) . . ?
C231 C230 B2 120.3(3) . . ?
C333 C334 C338 119.8(3) . . ?
C335 C334 C333 117.8(3) . . ?
C335 C334 C338 122.3(3) . . ?
C345 C340 B3 121.1(3) . . ?
C341 C340 B3 121.4(3) . . ?
C341 C340 C345 117.5(3) . . ?
C111 C112 C117 120.9(3) . . ?
C113 C112 C111 120.1(3) . . ?
C113 C112 C117 118.9(3) . . ?
C112 C111 B1 120.2(3) . . ?
C112 C111 C116 117.5(3) . . ?
C116 C111 B1 122.1(3) . . ?
O3 B3 C331 111.4(3) . . ?
O3 B3 C340 123.6(3) . . ?
C340 B3 C331 124.7(3) . . ?
C120 C125 C128 122.6(3) . . ?
C124 C125 C120 120.2(3) . . ?
C124 C125 C128 117.1(3) . . ?
C221 C222 C227 122.3(3) . . ?
C223 C222 C221 120.0(3) . . ?
C223 C222 C227 117.8(3) . . ?
C230 C235 C238 121.5(3) . . ?
C234 C235 C230 120.4(3) . . ?
C234 C235 C238 118.1(3) . . ?
C221 C226 C229 121.9(3) . . ?
C225 C226 C221 120.5(3) . . ?
C225 C226 C229 117.6(3) . . ?
C125 C120 B1 120.9(3) . . ?
C125 C120 C121 117.2(3) . . ?
C121 C120 B1 121.9(3) . . ?
C224 C225 C226 122.5(3) . . ?
C123 C124 C125 122.1(3) . . ?
C225 C224 C223 116.7(3) . . ?
C225 C224 C228 122.3(3) . . ?
C223 C224 C228 121.0(3) . . ?
O2 B2 C221 119.5(3) . . ?
O2 B2 C230 119.4(3) . . ?
C230 B2 C221 121.1(3) . . ?
C340 C345 C348 122.6(3) . . ?
C344 C345 C340 120.1(4) . . ?
C344 C345 C348 117.3(4) . . ?
O1 B1 C111 118.0(3) . . ?
O1 B1 C120 119.1(3) . . ?
C111 B1 C120 122.9(3) . . ?
C114 C113 C112 121.9(3) . . ?
C111 C116 C119 120.2(3) . . ?
C115 C116 C111 120.5(3) . . ?
C115 C116 C119 119.2(3) . . ?
C222 C223 C224 122.9(3) . . ?
C116 C115 C114 122.2(3) . . ?
C230 C231 C236 121.3(3) . . ?
C232 C231 C230 120.4(3) . . ?
C232 C231 C236 118.1(3) . . ?
C113 C114 C115 117.8(3) . . ?
C113 C114 C118 121.2(3) . . ?
C115 C114 C118 121.0(3) . . ?
C233 C232 C231 122.0(3) . . ?
C233 C234 C235 122.3(3) . . ?
C123 C122 C121 122.4(3) . . ?
C120 C121 C126 121.4(3) . . ?
C122 C121 C120 120.4(3) . . ?
C122 C121 C126 118.2(3) . . ?
C124 C123 C127 120.7(3) . . ?
C122 C123 C124 117.5(3) . . ?
C122 C123 C127 121.7(3) . . ?
C232 C233 C237 121.3(4) . . ?
C234 C233 C232 117.6(3) . . ?
C234 C233 C237 121.1(3) . . ?
C340 C341 C346 121.5(3) . . ?
C342 C341 C340 119.6(4) . . ?
C342 C341 C346 118.9(4) . . ?
C343 C342 C341 122.6(4) . . ?
C343 C344 C345 122.3(5) . . ?
C342 C343 C344 117.9(4) . . ?
C342 C343 C347 120.7(5) . . ?
C344 C343 C347 121.4(6) . . ?
C027 C01Q C01V 122.3(6) . . ?
C027 C32 C01R 117.5(6) . . ?
C01W C01V C01Q 117.4(5) . . ?
C32 C027 C01Q 127.0(9) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.190 0.006 0.250 753.5 153.8 ?
2 -0.212 -0.006 0.750 753.5 153.8 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.830

# start Validation Reply Form
_vrf_PLAT910_po17030_refinalized 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: No. of reflections / No. of parameters = 27.7 Therefore
this is not seen as a serious problem
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p17058_tri087
_database_code_depnum_ccdc_archive 'CCDC 1886808'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B6 C181 O9 U2'
_chemical_formula_sum            'C181 B6 O9 U2'
_chemical_formula_weight         2858.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C70 H70 O5 U1 B3'
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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.9113(5)
_cell_length_b                   16.1748(7)
_cell_length_c                   36.3982(10)
_cell_angle_alpha                89.191(3)
_cell_angle_beta                 89.908(2)
_cell_angle_gamma                66.724(3)
_cell_volume                     8604.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17885
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.0850
_cell_measurement_theta_min      3.2000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light grey'
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.212
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1255
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            151109
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.295
_diffrn_reflns_theta_max         24.295
_diffrn_reflns_theta_min         2.870
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00  51.00   1.00   17.50    --  -18.68  77.00-150.00   98
  2  ω    -93.00 -34.00   1.00   17.50    --  -18.68-179.00 -90.00   59
  3  ω    -93.00 -34.00   1.00   17.50    --  -18.68-179.00   0.00   59
  4  ω    -25.00  22.00   1.00   17.50    --  -18.68 -99.00 120.00   47
  5  ω    -25.00  22.00   1.00   17.50    --  -18.68 -99.00  30.00   47
  6  ω      2.00  89.00   1.00   17.50    --   20.25  57.00 -30.00   87
  7  ω    -50.00  43.00   1.00   17.50    --   20.25 -37.00 150.00   93
  8  ω    -52.00  58.00   1.00   17.50    --   20.25 -19.00-150.00  110
  9  ω    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-150.00   47
 10  ω    -82.00  -5.00   1.00   17.50    --  -18.68 138.00  75.74   77
 11  ω    -88.00  10.00   1.00   17.50    --  -18.68 -77.00  60.00   98
 12  ω    -25.00  61.00   1.00   17.50    --   20.25 -99.00   0.00   86
 13  ω    -48.00  39.00   1.00   17.50    --   20.25 -57.00  60.00   87
 14  ω      2.00  89.00   1.00   17.50    --   20.25  57.00-150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0125420000
_diffrn_orient_matrix_UB_12      -0.0012175000
_diffrn_orient_matrix_UB_13      -0.0187619000
_diffrn_orient_matrix_UB_21      -0.0074936000
_diffrn_orient_matrix_UB_22      -0.0400612000
_diffrn_orient_matrix_UB_23      -0.0022079000
_diffrn_orient_matrix_UB_31      -0.0462764000
_diffrn_orient_matrix_UB_32      0.0259419000
_diffrn_orient_matrix_UB_33      -0.0048135000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14908
_reflns_number_total             27315
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.516
_refine_diff_density_min         -6.769
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         27315
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.1161
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1250P)²+241.4568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.3190
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O6-C1 \\sim O5-C1 \\sim O4-C1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: O5(0.5) O4(0.5) O6(0.5) C1(0.5) O4A(0.5) O5A(0.5) O6A(0.5) C1A(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.69887(4) 0.74671(4) 0.33279(2) 0.0246(2) Uiso 1 1 d . U . . .
U1A U 0.79411(4) 0.74943(4) 0.16729(2) 0.02044(19) Uiso 1 1 d . U . . .
O3 O 0.5745(7) 0.8648(8) 0.3331(3) 0.024(2) Uiso 1 1 d . U . . .
O3A O 0.8105(7) 0.8694(7) 0.1544(3) 0.023(2) Uiso 1 1 d . U . . .
O1A O 0.6983(6) 0.7452(7) 0.1271(3) 0.016(2) Uiso 1 1 d . U . . .
O1 O 0.7947(8) 0.7543(8) 0.3710(3) 0.032(3) Uiso 1 1 d . U . . .
O2 O 0.6835(7) 0.6238(8) 0.3443(3) 0.026(3) Uiso 1 1 d . U . . .
O2A O 0.9146(6) 0.6332(7) 0.1666(3) 0.014(2) Uiso 1 1 d . U . . .
C12 C 0.9973(12) 0.6097(12) 0.3582(5) 0.028(4) Uiso 1 1 d . U . . .
C522 C 0.8965(11) 0.7443(12) 0.0839(5) 0.025(4) Uiso 1 1 d . U . . .
C63A C 0.5200(12) 1.1267(13) 0.3928(5) 0.034(4) Uiso 1 1 d . U . . .
C44A C 1.2251(12) 0.5417(12) 0.2392(5) 0.029(4) Uiso 1 1 d . U . . .
C56A C 0.3648(11) 1.0186(12) 0.2867(5) 0.025(4) Uiso 1 1 d . U . . .
C16 C 1.0120(11) 0.6281(12) 0.4227(5) 0.027(4) Uiso 1 1 d . U . . .
C343 C 1.0502(11) 0.2920(12) 0.0490(5) 0.026(4) Uiso 1 1 d . U . . .
C13 C 1.0758(12) 0.5326(13) 0.3591(5) 0.033(4) Uiso 1 1 d . U . . .
C363 C 0.8907(11) 0.4421(11) 0.1657(5) 0.024(4) Uiso 1 1 d . U . . .
C43A C 1.1804(11) 0.6191(12) 0.2174(5) 0.024(4) Uiso 1 1 d . U . . .
C420 C 0.6531(13) 0.6532(14) 0.4257(6) 0.039(5) Uiso 1 1 d . U . . .
C11A C 0.5316(10) 0.8353(11) 0.1108(4) 0.019(3) Uiso 1 1 d . U . . .
C320 C 0.7000(11) 0.4734(12) 0.2795(5) 0.027(4) Uiso 1 1 d . U . . .
C260 C 0.7547(13) 0.8642(13) 0.4525(5) 0.036(4) Uiso 1 1 d . U . . .
C520 C 0.8455(10) 0.8403(10) 0.0743(4) 0.017(3) Uiso 1 1 d . U . . .
C123 C 0.5393(11) 0.8599(11) 0.1792(4) 0.022(4) Uiso 1 1 d . U . . .
C61 C 0.7245(11) 1.0429(11) 0.1555(5) 0.023(4) Uiso 1 1 d . U . . .
C42 C 0.5941(12) 0.6002(13) 0.4160(5) 0.034(4) Uiso 1 1 d . U . . .
C624 C 0.5836(12) 1.1486(13) 0.3185(5) 0.034(4) Uiso 1 1 d . U . . .
C62A C 0.5308(12) 1.0608(13) 0.3659(5) 0.033(4) Uiso 1 1 d . U . . .
C125 C 0.4759(11) 0.8567(12) 0.2103(5) 0.026(4) Uiso 1 1 d . U . . .
C53 C 0.9746(12) 0.8849(13) 0.0594(5) 0.032(4) Uiso 1 1 d . U . . .
C423 C 1.0612(11) 0.7166(12) 0.1741(5) 0.026(4) Uiso 1 1 d . U . . .
C163 C 0.5162(12) 0.8202(12) 0.0415(5) 0.030(4) Uiso 1 1 d . U . . .
C31 C 0.7657(11) 0.4565(11) 0.3441(5) 0.023(4) Uiso 1 1 d . U . . .
C321 C 0.7373(13) 0.5257(14) 0.2529(5) 0.039(5) Uiso 1 1 d . U . . .
C21A C 0.6196(9) 0.6526(10) 0.0977(4) 0.011(3) Uiso 1 1 d . U . . .
C66A C 0.4140(11) 1.0223(12) 0.3938(5) 0.027(4) Uiso 1 1 d . U . . .
C11 C 0.9620(11) 0.6603(12) 0.3903(5) 0.026(4) Uiso 1 1 d . U . . .
C663 C 0.3553(13) 0.9689(13) 0.3949(5) 0.036(4) Uiso 1 1 d . U . . .
C42A C 1.1049(11) 0.6284(11) 0.1952(4) 0.022(4) Uiso 1 1 d . U . . .
C55A C 0.2920(11) 1.0228(12) 0.2645(5) 0.028(4) Uiso 1 1 d . U . . .
C36 C 0.8345(12) 0.4047(13) 0.3694(5) 0.032(4) Uiso 1 1 d . U . . .
C53A C 0.3122(12) 0.8740(12) 0.2818(5) 0.030(4) Uiso 1 1 d . U . . .
C523 C 0.4318(12) 0.7776(13) 0.3265(5) 0.034(4) Uiso 1 1 d . U . . .
C32 C 0.7702(11) 0.4252(11) 0.3086(4) 0.023(4) Uiso 1 1 d . U . . .
C443 C 1.3034(12) 0.5341(13) 0.2646(5) 0.035(4) Uiso 1 1 d . U . . .
B1 B 0.8720(11) 0.7515(12) 0.3882(5) 0.015(4) Uiso 1 1 d . U . . .
C12A C 0.4961(10) 0.8852(11) 0.1420(4) 0.021(3) Uiso 1 1 d . U . . .
C560 C 0.9105(12) 1.0758(13) 0.1472(5) 0.032(4) Uiso 1 1 d . U . . .
C264 C 0.8375(12) 0.5726(13) 0.0529(5) 0.032(4) Uiso 1 1 d . U . . .
C620 C 0.6577(11) 1.0638(12) 0.0915(5) 0.025(4) Uiso 1 1 d . U . . .
C262 C 0.7782(16) 0.8499(17) 0.4944(7) 0.061(6) Uiso 1 1 d . U . . .
C36A C 0.9580(10) 0.4344(10) 0.1350(4) 0.017(3) Uiso 1 1 d . U . . .
C52 C 0.9010(11) 0.8944(11) 0.0818(4) 0.022(4) Uiso 1 1 d . U . . .
C660 C 0.7885(12) 1.0224(13) 0.2211(5) 0.033(4) Uiso 1 1 d . U . . .
C45A C 1.1988(11) 0.4708(12) 0.2355(5) 0.026(4) Uiso 1 1 d . U . . .
C52A C 0.3846(11) 0.8672(12) 0.3054(5) 0.026(4) Uiso 1 1 d . U . . .
C54A C 0.2637(11) 0.9534(12) 0.2621(5) 0.027(4) Uiso 1 1 d . U . . .
C26 C 0.8180(13) 0.8950(13) 0.4316(5) 0.036(4) Uiso 1 1 d . U . . .
C463 C 1.0981(11) 0.3984(12) 0.2123(5) 0.024(4) Uiso 1 1 d . U . . .
C444 C 1.2649(14) 0.6051(15) 0.2959(6) 0.045(5) Uiso 1 1 d . U . . .
C62 C 0.6577(11) 1.0916(11) 0.1303(4) 0.022(4) Uiso 1 1 d . U . . .
C14A C 0.3693(11) 0.9954(11) 0.1072(5) 0.023(4) Uiso 1 1 d . U . . .
C15 C 1.0890(15) 0.5552(16) 0.4236(6) 0.051(6) Uiso 1 1 d . U . . .
C422 C 0.6837(16) 0.6452(16) 0.4666(7) 0.056(6) Uiso 1 1 d . U . . .
C35 C 0.9050(13) 0.3265(13) 0.3598(5) 0.037(4) Uiso 1 1 d . U . . .
C41A C 1.0776(11) 0.5562(12) 0.1919(5) 0.025(4) Uiso 1 1 d . U . . .
C65A C 0.4060(13) 1.0847(14) 0.4202(6) 0.040(5) Uiso 1 1 d . U . . .
C223 C 0.4992(11) 0.6630(12) 0.1456(5) 0.026(4) Uiso 1 1 d . U . . .
C41 C 0.6101(12) 0.5449(12) 0.3872(5) 0.029(4) Uiso 1 1 d . U . . .
C31A C 1.0110(10) 0.4885(11) 0.1342(4) 0.019(3) Uiso 1 1 d . U . . .
C665 C 0.3494(14) 0.9336(14) 0.4335(6) 0.043(5) Uiso 1 1 d . U . . .
C64A C 0.4568(12) 1.1381(13) 0.4207(5) 0.033(4) Uiso 1 1 d . U . . .
C664 C 0.2588(15) 1.0253(16) 0.3811(6) 0.050(5) Uiso 1 1 d . U . . .
C424 C 1.0102(12) 0.7965(13) 0.2000(5) 0.036(4) Uiso 1 1 d . U . . .
C120 C 0.9492(12) 0.6404(12) 0.3205(5) 0.029(4) Uiso 1 1 d . U . . .
C63 C 0.5866(10) 1.1709(11) 0.1419(4) 0.021(3) Uiso 1 1 d . U . . .
C465 C 1.1736(14) 0.3134(15) 0.1993(6) 0.045(5) Uiso 1 1 d . U . . .
C645 C 0.5128(16) 1.1624(17) 0.4816(7) 0.057(6) Uiso 1 1 d . U . . .
C65 C 0.6461(11) 1.1547(12) 0.2016(5) 0.029(4) Uiso 1 1 d . U . . .
C66 C 0.7165(11) 1.0740(12) 0.1926(5) 0.025(4) Uiso 1 1 d . U . . .
C32A C 1.0762(10) 0.4747(11) 0.1062(4) 0.019(3) Uiso 1 1 d . U . . .
C16A C 0.4826(11) 0.8683(12) 0.0772(5) 0.025(4) Uiso 1 1 d . U . . .
C33A C 1.0901(10) 0.4090(11) 0.0797(4) 0.020(3) Uiso 1 1 d . U . . .
C34 C 0.9117(13) 0.2931(13) 0.3233(5) 0.036(4) Uiso 1 1 d . U . . .
C561 C 0.8470(14) 1.1646(15) 0.1332(6) 0.046(5) Uiso 1 1 d . U . . .
C34A C 1.0360(12) 0.3594(12) 0.0799(5) 0.031(4) Uiso 1 1 d . U . . .
C33 C 0.8400(12) 0.3489(13) 0.2989(5) 0.034(4) Uiso 1 1 d . U . . .
C525 C 0.4789(15) 0.7029(16) 0.2992(6) 0.052(6) Uiso 1 1 d . U . . .
C56 C 0.9350(10) 1.0048(11) 0.1179(4) 0.021(3) Uiso 1 1 d . U . . .
B3A B 0.8051(12) 0.9532(12) 0.1427(5) 0.017(4) Uiso 1 1 d . U . . .
C323 C 1.1365(11) 0.5291(12) 0.1047(5) 0.027(4) Uiso 1 1 d . U . . .
C21 C 0.8760(13) 0.8423(14) 0.4039(5) 0.039(5) Uiso 1 1 d . U . . .
C322 C 0.6642(12) 0.4133(13) 0.2578(5) 0.036(4) Uiso 1 1 d . U . . .
C51 C 0.8809(11) 0.9517(11) 0.1135(4) 0.023(4) Uiso 1 1 d . U . . .
B2 B 0.6852(13) 0.5454(14) 0.3587(6) 0.026(4) Uiso 1 1 d . U . . .
C521 C 0.8092(12) 0.8546(13) 0.0348(5) 0.035(4) Uiso 1 1 d . U . . .
C64 C 0.5818(12) 1.2027(12) 0.1764(5) 0.030(4) Uiso 1 1 d . U . . .
C263 C 0.7374(11) 0.6415(12) 0.0473(5) 0.027(4) Uiso 1 1 d . U . . .
C14 C 1.1259(14) 0.4980(15) 0.3908(6) 0.044(5) Uiso 1 1 d . U . . .
C644 C 0.4535(16) 1.2898(16) 0.4377(6) 0.056(6) Uiso 1 1 d . U . . .
C360 C 0.8324(13) 0.4396(13) 0.4083(5) 0.036(4) Uiso 1 1 d . U . . .
C44 C 0.4708(17) 0.5627(18) 0.4357(7) 0.064(7) Uiso 1 1 d . U . . .
C623 C 0.6038(12) 1.0510(12) 0.3364(5) 0.031(4) Uiso 1 1 d . U . . .
C524 C 0.3636(14) 0.7547(15) 0.3502(6) 0.049(5) Uiso 1 1 d . U . . .
C61A C 0.4797(11) 1.0092(12) 0.3653(5) 0.028(4) Uiso 1 1 d . U . . .
C565 C 0.4196(16) 1.1186(17) 0.2495(7) 0.061(6) Uiso 1 1 d . U . . .
C25A C 0.6679(11) 0.5261(12) 0.0560(5) 0.026(4) Uiso 1 1 d . U . . .
C141 C 1.2671(18) 0.3940(18) 0.3603(7) 0.069(7) Uiso 1 1 d . U . . .
C23A C 0.5562(12) 0.5387(13) 0.1014(5) 0.031(4) Uiso 1 1 d . U . . .
C640 C 0.5064(14) 1.2933(14) 0.1875(6) 0.043(5) Uiso 1 1 d . U . . .
C22 C 0.9351(13) 0.8778(13) 0.3857(5) 0.035(4) Uiso 1 1 d . U . . .
C26A C 0.6707(10) 0.6085(11) 0.0675(4) 0.021(3) Uiso 1 1 d . U . . .
C15A C 0.4033(11) 0.9493(12) 0.0767(5) 0.025(4) Uiso 1 1 d . U . . .
C220 C 0.9942(12) 0.8304(13) 0.3539(5) 0.031(4) Uiso 1 1 d . U . . .
C543 C 0.1890(11) 0.9567(12) 0.2355(5) 0.029(4) Uiso 1 1 d . U . . .
C124 C 0.5897(13) 0.9209(14) 0.1886(5) 0.039(5) Uiso 1 1 d . U . . .
C421 C 0.5925(16) 0.7589(16) 0.4168(6) 0.055(6) Uiso 1 1 d . U . . .
C161 C 1.0394(16) 0.7315(17) 0.4701(7) 0.057(6) Uiso 1 1 d . U . . .
C164 C 0.4549(13) 0.7719(13) 0.0301(5) 0.037(4) Uiso 1 1 d . U . . .
C13A C 0.4157(12) 0.9655(13) 0.1407(5) 0.032(4) Uiso 1 1 d . U . . .
C340 C 0.9822(14) 0.2055(14) 0.3126(6) 0.043(5) Uiso 1 1 d . U . . .
C662 C 0.7522(15) 0.9723(15) 0.2479(6) 0.050(5) Uiso 1 1 d . U . . .
B3 B 0.4918(12) 0.9365(13) 0.3350(5) 0.019(4) Uiso 1 1 d . U . . .
C160 C 0.9791(13) 0.6814(14) 0.4584(6) 0.042(5) Uiso 1 1 d . U . . .
C143 C 0.2840(13) 1.0837(14) 0.1049(5) 0.038(5) Uiso 1 1 d . U . . .
B1A B 0.6190(13) 0.7444(14) 0.1118(5) 0.024(4) Uiso 1 1 d . U . . .
C51A C 0.4129(11) 0.9399(11) 0.3078(5) 0.024(4) Uiso 1 1 d . U . . .
C325 C 1.1436(13) 0.5647(13) 0.0655(5) 0.037(4) Uiso 1 1 d . U . . .
C661 C 0.8241(14) 1.0826(14) 0.2423(6) 0.044(5) Uiso 1 1 d . U . . .
C563 C 0.3911(12) 1.0975(13) 0.2873(5) 0.033(4) Uiso 1 1 d . U . . .
C425 C 1.1288(13) 0.7403(14) 0.1503(5) 0.041(5) Uiso 1 1 d . U . . .
C122 C 1.0143(13) 0.6382(14) 0.2901(6) 0.040(5) Uiso 1 1 d . U . . .
C265 C 0.7188(12) 0.6532(13) 0.0063(5) 0.033(4) Uiso 1 1 d . U . . .
C23 C 0.9352(14) 0.9601(14) 0.3981(6) 0.042(5) Uiso 1 1 d . U . . .
C24 C 0.8839(14) 1.0051(15) 0.4267(6) 0.046(5) Uiso 1 1 d . U . . .
C46 C 0.5582(14) 0.4926(15) 0.3826(6) 0.046(5) Uiso 1 1 d . U . . .
C46A C 1.1259(11) 0.4761(11) 0.2126(5) 0.024(4) Uiso 1 1 d . U . . .
C140 C 1.2093(15) 0.4157(16) 0.3932(6) 0.050(5) Uiso 1 1 d . U . . .
C261 C 0.6540(16) 0.9288(17) 0.4458(7) 0.059(6) Uiso 1 1 d . U . . .
C45 C 0.4885(15) 0.5016(16) 0.4063(6) 0.051(5) Uiso 1 1 d . U . . .
C345 C 1.0405(13) 0.2064(13) 0.0618(5) 0.038(5) Uiso 1 1 d . U . . .
C55 C 1.0069(14) 0.9934(15) 0.0931(6) 0.045(5) Uiso 1 1 d . U . . .
C22A C 0.5592(11) 0.6173(11) 0.1131(5) 0.023(4) Uiso 1 1 d . U . . .
C621 C 0.5693(15) 1.0454(15) 0.0847(6) 0.052(5) Uiso 1 1 d . U . . .
C324 C 1.2318(13) 0.4726(13) 0.1203(5) 0.037(5) Uiso 1 1 d . U . . .
C24A C 0.6104(12) 0.4894(13) 0.0723(5) 0.034(4) Uiso 1 1 d . U . . .
C25 C 0.8265(14) 0.9713(15) 0.4445(6) 0.047(5) Uiso 1 1 d . U . . .
C341 C 1.0784(17) 0.1971(18) 0.3213(7) 0.064(7) Uiso 1 1 d . U . . .
C625 C 0.6992(14) 1.0071(15) 0.3501(6) 0.048(5) Uiso 1 1 d . U . . .
C562 C 0.9930(14) 1.0864(14) 0.1637(6) 0.043(5) Uiso 1 1 d . U . . .
C165 C 0.5255(13) 0.8805(13) 0.0102(5) 0.038(5) Uiso 1 1 d . U . . .
C460 C 0.5786(13) 0.4239(14) 0.3530(5) 0.038(5) Uiso 1 1 d . U . . .
C545 C 0.2229(13) 0.8921(13) 0.2054(5) 0.036(4) Uiso 1 1 d . U . . .
C240 C 0.8865(19) 1.0965(19) 0.4392(8) 0.072(7) Uiso 1 1 d . U . . .
C462 C 0.6498(15) 0.3278(16) 0.3685(6) 0.053(6) Uiso 1 1 d . U . . .
C544 C 0.1119(15) 0.9421(15) 0.2575(6) 0.051(5) Uiso 1 1 d . U . . .
C144 C 0.3100(18) 1.1647(19) 0.0974(7) 0.072(7) Uiso 1 1 d . U . . .
C445 C 1.3811(15) 0.5487(16) 0.2445(6) 0.051(5) Uiso 1 1 d . U . . .
C461 C 0.4931(15) 0.4181(16) 0.3361(6) 0.053(6) Uiso 1 1 d . U . . .
C225 C 0.5347(16) 0.6128(16) 0.1813(6) 0.056(6) Uiso 1 1 d . U . . .
C162 C 0.9774(16) 0.6149(17) 0.4903(7) 0.059(6) Uiso 1 1 d . U . . .
C222 C 0.9546(15) 0.8838(15) 0.3182(6) 0.050(5) Uiso 1 1 d . U . . .
C641 C 0.4126(18) 1.2972(19) 0.1780(8) 0.071(7) Uiso 1 1 d . U . . .
C344 C 0.9768(15) 0.3409(16) 0.0185(6) 0.054(6) Uiso 1 1 d . U . . .
C35A C 0.9712(11) 0.3729(11) 0.1079(5) 0.024(4) Uiso 1 1 d . U . . .
C243 C 0.6052(15) 0.4012(16) 0.0618(6) 0.053(6) Uiso 1 1 d . U . . .
C221 C 1.0937(17) 0.8183(17) 0.3591(7) 0.063(6) Uiso 1 1 d . U . . .
C464 C 1.0658(14) 0.3821(15) 0.2511(6) 0.046(5) Uiso 1 1 d . U . . .
C362 C 0.8324(18) 0.3690(19) 0.4373(7) 0.069(7) Uiso 1 1 d . U . . .
C342 C 0.9667(18) 0.1280(19) 0.3316(8) 0.073(7) Uiso 1 1 d . U . . .
C241 C 0.986(2) 1.083(2) 0.4503(9) 0.098(10) Uiso 1 1 d . U . . .
B2A B 0.9957(13) 0.5642(14) 0.1642(5) 0.025(4) Uiso 1 1 d . U . . .
C540 C 1.1136(18) 0.9212(19) 0.0421(8) 0.070(7) Uiso 1 1 d . U . . .
C245 C 0.5005(19) 0.4226(19) 0.0507(8) 0.075(8) Uiso 1 1 d . U . . .
C642 C 0.5222(19) 1.369(2) 0.1658(8) 0.078(8) Uiso 1 1 d . U . . .
C43 C 0.5238(16) 0.6093(17) 0.4410(7) 0.056(6) Uiso 1 1 d . U . . .
C622 C 0.6611(15) 1.1315(16) 0.0632(6) 0.053(6) Uiso 1 1 d . U . . .
C643 C 0.4471(15) 1.2034(16) 0.4511(6) 0.050(5) Uiso 1 1 d . U . . .
C54 C 1.0309(14) 0.9312(15) 0.0650(6) 0.049(5) Uiso 1 1 d . U . . .
C242 C 0.822(2) 1.149(2) 0.4666(10) 0.100(10) Uiso 1 1 d . U . . .
C564 C 0.3146(16) 1.1866(17) 0.3026(7) 0.059(6) Uiso 1 1 d . U . . .
C442 C 0.383(3) 0.622(3) 0.4961(12) 0.131(14) Uiso 1 1 d . U . . .
C361 C 0.9042(18) 0.4729(18) 0.4169(7) 0.069(7) Uiso 1 1 d . U . . .
C244 C 0.662(2) 0.360(2) 0.0302(8) 0.084(8) Uiso 1 1 d . U . . .
C224 C 0.3974(18) 0.6794(19) 0.1400(8) 0.074(7) Uiso 1 1 d . U . . .
C145 C 0.2274(16) 1.1016(17) 0.1414(7) 0.061(6) Uiso 1 1 d . U . . .
C142 C 1.183(2) 0.335(2) 0.4006(9) 0.100(10) Uiso 1 1 d . U . . .
C440 C 0.376(3) 0.581(3) 0.4580(11) 0.118(12) Uiso 1 1 d . U . . .
C541 C 1.113(2) 0.883(2) 0.0058(8) 0.084(8) Uiso 1 1 d . U . . .
C441 C 0.300(4) 0.643(4) 0.4353(15) 0.172(19) Uiso 1 1 d . U . . .
C542 C 1.197(3) 0.868(3) 0.0658(11) 0.118(12) Uiso 1 1 d . U . . .
C364 C 0.8994(12) 0.3541(13) 0.1811(5) 0.034(4) Uiso 1 1 d . U . . .
C365 C 0.7909(12) 0.4907(13) 0.1495(5) 0.033(4) Uiso 1 1 d . U . . .
O5 O 0.7839(19) 0.7722(19) 0.2828(7) 0.048(7) Uiso 0.5 1 d D U P A 1
O4 O 0.6758(15) 0.7234(16) 0.2692(6) 0.027(5) Uiso 0.5 1 d D U P A 1
O6 O 0.7642(13) 0.7390(14) 0.2204(7) 0.014(5) Uiso 0.5 1 d D U P A 1
C1 C 0.7396(17) 0.750(2) 0.2557(7) 0.012(7) Uiso 0.5 1 d D U P A 1
O4A O 0.8199(13) 0.7600(13) 0.2306(5) 0.015(4) Uiso 0.5 1 d . U P A 2
O5A O 0.7187(12) 0.7126(12) 0.2190(5) 0.007(4) Uiso 0.5 1 d . U P A 2
O6A O 0.7352(13) 0.7417(13) 0.2742(6) 0.012(5) Uiso 0.5 1 d . U P A 2
C1A C 0.761(2) 0.739(2) 0.2374(14) 0.018(7) Uiso 0.5 1 d . U P A 2
C121 C 0.8977(13) 0.5804(13) 0.3104(5) 0.037(4) Uiso 1 1 d . U . . .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O3 2.140(11) . ?
U1 O1 2.106(11) . ?
U1 O2 2.132(11) . ?
U1 O5 2.39(3) . ?
U1 O4 2.40(2) . ?
U1 O6A 2.20(2) . ?
U1A O3A 2.105(10) . ?
U1A O1A 2.135(9) . ?
U1A O2A 2.089(10) . ?
U1A O6 2.01(3) . ?
U1A O4A 2.363(19) . ?
U1A O5A 2.421(17) . ?
O3 B3 1.37(2) . ?
O3A B3A 1.38(2) . ?
O1A B1A 1.38(2) . ?
O1 B1 1.365(19) . ?
O2 B2 1.36(2) . ?
O2A B2A 1.33(2) . ?
C12 C13 1.37(3) . ?
C12 C11 1.42(2) . ?
C12 C120 1.55(2) . ?
C522 C520 1.48(2) . ?
C63A C62A 1.42(3) . ?
C63A C64A 1.39(3) . ?
C44A C43A 1.41(2) . ?
C44A C443 1.52(2) . ?
C44A C45A 1.37(2) . ?
C56A C55A 1.39(2) . ?
C56A C51A 1.41(2) . ?
C56A C563 1.49(2) . ?
C16 C11 1.40(2) . ?
C16 C15 1.32(3) . ?
C16 C160 1.54(3) . ?
C343 C34A 1.53(2) . ?
C343 C345 1.52(2) . ?
C343 C344 1.57(3) . ?
C13 C14 1.38(3) . ?
C363 C36A 1.52(2) . ?
C363 C364 1.48(2) . ?
C363 C365 1.58(2) . ?
C43A C42A 1.41(2) . ?
C420 C42 1.54(2) . ?
C420 C422 1.56(3) . ?
C420 C421 1.62(3) . ?
C11A C12A 1.39(2) . ?
C11A C16A 1.43(2) . ?
C11A B1A 1.57(3) . ?
C320 C321 1.54(2) . ?
C320 C32 1.51(2) . ?
C320 C322 1.53(2) . ?
C260 C262 1.56(3) . ?
C260 C26 1.49(2) . ?
C260 C261 1.55(3) . ?
C520 C52 1.494(19) . ?
C520 C521 1.53(2) . ?
C123 C125 1.53(2) . ?
C123 C12A 1.50(2) . ?
C123 C124 1.54(2) . ?
C61 C62 1.38(2) . ?
C61 C66 1.43(2) . ?
C61 B3A 1.59(2) . ?
C42 C41 1.35(3) . ?
C42 C43 1.40(3) . ?
C624 C623 1.61(2) . ?
C62A C623 1.55(2) . ?
C62A C61A 1.38(2) . ?
C53 C52 1.38(2) . ?
C53 C54 1.39(2) . ?
C423 C42A 1.52(2) . ?
C423 C424 1.56(3) . ?
C423 C425 1.54(2) . ?
C163 C16A 1.51(2) . ?
C163 C164 1.53(2) . ?
C163 C165 1.53(3) . ?
C31 C36 1.41(2) . ?
C31 C32 1.39(2) . ?
C31 B2 1.60(3) . ?
C21A C26A 1.39(2) . ?
C21A B1A 1.58(2) . ?
C21A C22A 1.410(19) . ?
C66A C663 1.50(2) . ?
C66A C65A 1.37(3) . ?
C66A C61A 1.43(2) . ?
C11 B1 1.60(2) . ?
C663 C665 1.53(3) . ?
C663 C664 1.53(3) . ?
C42A C41A 1.41(2) . ?
C55A C54A 1.37(2) . ?
C36 C35 1.37(3) . ?
C36 C360 1.53(3) . ?
C53A C52A 1.40(2) . ?
C53A C54A 1.40(2) . ?
C523 C52A 1.54(2) . ?
C523 C525 1.53(3) . ?
C523 C524 1.54(3) . ?
C32 C33 1.35(2) . ?
C443 C444 1.57(3) . ?
C443 C445 1.53(3) . ?
B1 C21 1.61(3) . ?
C12A C13A 1.42(2) . ?
C560 C561 1.48(3) . ?
C560 C56 1.51(2) . ?
C560 C562 1.52(2) . ?
C264 C263 1.55(2) . ?
C620 C62 1.49(2) . ?
C620 C621 1.57(2) . ?
C620 C622 1.51(3) . ?
C36A C31A 1.434(19) . ?
C36A C35A 1.37(2) . ?
C52 C51 1.45(2) . ?
C660 C66 1.52(2) . ?
C660 C662 1.51(3) . ?
C660 C661 1.52(3) . ?
C45A C46A 1.40(2) . ?
C52A C51A 1.42(2) . ?
C54A C543 1.52(2) . ?
C26 C21 1.41(3) . ?
C26 C25 1.38(3) . ?
C463 C465 1.51(3) . ?
C463 C46A 1.49(2) . ?
C463 C464 1.56(3) . ?
C62 C63 1.40(2) . ?
C14A C15A 1.33(2) . ?
C14A C13A 1.40(2) . ?
C14A C143 1.53(3) . ?
C15 C14 1.49(3) . ?
C35 C34 1.43(3) . ?
C41A C46A 1.42(2) . ?
C41A B2A 1.61(2) . ?
C65A C64A 1.40(2) . ?
C223 C22A 1.52(2) . ?
C223 C225 1.51(3) . ?
C223 C224 1.55(3) . ?
C41 B2 1.58(3) . ?
C41 C46 1.41(2) . ?
C31A C32A 1.41(2) . ?
C31A B2A 1.60(3) . ?
C64A C643 1.51(3) . ?
C120 C122 1.50(3) . ?
C120 C121 1.54(2) . ?
C63 C64 1.35(2) . ?
C645 C643 1.49(3) . ?
C65 C66 1.39(2) . ?
C65 C64 1.36(2) . ?
C32A C33A 1.40(2) . ?
C32A C323 1.54(2) . ?
C16A C15A 1.41(2) . ?
C33A C34A 1.39(2) . ?
C34 C33 1.44(3) . ?
C34 C340 1.48(3) . ?
C34A C35A 1.41(2) . ?
C56 C51 1.45(2) . ?
C56 C55 1.41(3) . ?
B3A C51 1.60(2) . ?
C323 C325 1.55(2) . ?
C323 C324 1.53(2) . ?
C21 C22 1.44(2) . ?
C64 C640 1.54(3) . ?
C263 C26A 1.54(2) . ?
C263 C265 1.52(2) . ?
C14 C140 1.46(3) . ?
C644 C643 1.51(3) . ?
C360 C362 1.54(3) . ?
C360 C361 1.48(3) . ?
C44 C45 1.42(3) . ?
C44 C43 1.35(3) . ?
C44 C440 1.64(4) . ?
C623 C625 1.48(3) . ?
C61A B3 1.58(3) . ?
C565 C563 1.52(3) . ?
C25A C26A 1.42(2) . ?
C25A C24A 1.40(2) . ?
C141 C140 1.47(3) . ?
C23A C22A 1.37(2) . ?
C23A C24A 1.41(3) . ?
C640 C641 1.51(3) . ?
C640 C642 1.55(3) . ?
C22 C220 1.51(3) . ?
C22 C23 1.41(3) . ?
C220 C222 1.54(3) . ?
C220 C221 1.53(3) . ?
C543 C545 1.47(3) . ?
C543 C544 1.56(3) . ?
C161 C160 1.54(3) . ?
C340 C341 1.51(3) . ?
C340 C342 1.53(3) . ?
B3 C51A 1.58(2) . ?
C160 C162 1.58(3) . ?
C143 C144 1.54(3) . ?
C143 C145 1.57(3) . ?
C563 C564 1.58(3) . ?
C23 C24 1.35(3) . ?
C24 C25 1.39(3) . ?
C24 C240 1.57(3) . ?
C46 C45 1.37(3) . ?
C46 C460 1.50(3) . ?
C140 C142 1.54(4) . ?
C55 C54 1.39(3) . ?
C24A C243 1.52(3) . ?
C460 C462 1.61(3) . ?
C460 C461 1.53(3) . ?
C240 C241 1.57(4) . ?
C240 C242 1.45(4) . ?
C243 C245 1.61(3) . ?
C243 C244 1.46(4) . ?
C540 C54 1.51(3) . ?
C540 C541 1.47(4) . ?
C540 C542 1.53(4) . ?
C442 C440 1.57(5) . ?
C440 C441 1.47(6) . ?
O5 C1 1.342(18) . ?
O4 C1 1.343(17) . ?
O6 C1 1.336(17) . ?
O4A C1A 1.14(4) . ?
O5A C1A 1.15(4) . ?
O6A C1A 1.40(6) . ?

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
O3 U1 O5 104.2(8) . . ?
O3 U1 O4 90.6(6) . . ?
O3 U1 O6A 100.7(6) . . ?
O1 U1 O3 111.9(4) . . ?
O1 U1 O2 106.5(4) . . ?
O1 U1 O5 91.2(7) . . ?
O1 U1 O4 144.0(6) . . ?
O1 U1 O6A 117.3(6) . . ?
O2 U1 O3 115.0(4) . . ?
O2 U1 O5 125.5(7) . . ?
O2 U1 O4 87.2(6) . . ?
O2 U1 O6A 105.6(6) . . ?
O5 U1 O4 55.1(8) . . ?
O3A U1A O1A 103.6(4) . . ?
O3A U1A O4A 92.9(5) . . ?
O3A U1A O5A 130.0(5) . . ?
O1A U1A O4A 145.1(5) . . ?
O1A U1A O5A 95.4(5) . . ?
O2A U1A O3A 114.9(4) . . ?
O2A U1A O1A 111.6(4) . . ?
O2A U1A O4A 87.9(6) . . ?
O2A U1A O5A 99.5(5) . . ?
O6 U1A O3A 113.5(7) . . ?
O6 U1A O1A 117.5(6) . . ?
O6 U1A O2A 96.3(7) . . ?
O4A U1A O5A 51.7(6) . . ?
B3 O3 U1 175.3(10) . . ?
B3A O3A U1A 169.1(10) . . ?
B1A O1A U1A 160.4(11) . . ?
B1 O1 U1 164.9(11) . . ?
B2 O2 U1 166.8(11) . . ?
B2A O2A U1A 173.9(10) . . ?
C13 C12 C11 121.5(16) . . ?
C13 C12 C120 117.4(16) . . ?
C11 C12 C120 121.1(16) . . ?
C64A C63A C62A 118.5(16) . . ?
C43A C44A C443 121.3(15) . . ?
C45A C44A C43A 118.0(15) . . ?
C45A C44A C443 120.7(16) . . ?
C55A C56A C51A 119.8(15) . . ?
C55A C56A C563 118.8(16) . . ?
C51A C56A C563 121.4(14) . . ?
C11 C16 C160 119.2(17) . . ?
C15 C16 C11 122.2(19) . . ?
C15 C16 C160 118.5(17) . . ?
C34A C343 C344 107.0(15) . . ?
C345 C343 C34A 113.1(15) . . ?
C345 C343 C344 110.0(14) . . ?
C12 C13 C14 123.4(19) . . ?
C36A C363 C365 107.8(13) . . ?
C364 C363 C36A 113.3(15) . . ?
C364 C363 C365 107.9(13) . . ?
C42A C43A C44A 121.5(14) . . ?
C42 C420 C422 114.8(16) . . ?
C42 C420 C421 107.5(15) . . ?
C422 C420 C421 107.5(17) . . ?
C12A C11A C16A 116.7(15) . . ?
C12A C11A B1A 122.6(14) . . ?
C16A C11A B1A 120.6(15) . . ?
C32 C320 C321 110.4(13) . . ?
C32 C320 C322 114.9(14) . . ?
C322 C320 C321 110.1(15) . . ?
C26 C260 C262 112.8(15) . . ?
C26 C260 C261 110.8(17) . . ?
C261 C260 C262 111.7(18) . . ?
C522 C520 C52 111.6(12) . . ?
C522 C520 C521 112.6(14) . . ?
C52 C520 C521 111.4(12) . . ?
C125 C123 C124 111.5(14) . . ?
C12A C123 C125 116.0(13) . . ?
C12A C123 C124 109.5(13) . . ?
C62 C61 C66 118.7(16) . . ?
C62 C61 B3A 118.8(15) . . ?
C66 C61 B3A 122.5(14) . . ?
C41 C42 C420 124.0(16) . . ?
C41 C42 C43 120.9(17) . . ?
C43 C42 C420 115.0(18) . . ?
C63A C62A C623 115.3(15) . . ?
C61A C62A C63A 123.4(17) . . ?
C61A C62A C623 121.4(16) . . ?
C52 C53 C54 123.1(18) . . ?
C42A C423 C424 111.7(14) . . ?
C42A C423 C425 113.9(14) . . ?
C425 C423 C424 108.9(14) . . ?
C16A C163 C164 109.7(14) . . ?
C16A C163 C165 114.4(16) . . ?
C164 C163 C165 111.1(14) . . ?
C36 C31 B2 118.0(15) . . ?
C32 C31 C36 118.1(16) . . ?
C32 C31 B2 123.9(15) . . ?
C26A C21A B1A 122.5(13) . . ?
C26A C21A C22A 117.3(13) . . ?
C22A C21A B1A 119.8(14) . . ?
C65A C66A C663 120.9(16) . . ?
C65A C66A C61A 118.3(15) . . ?
C61A C66A C663 120.7(16) . . ?
C12 C11 B1 120.4(15) . . ?
C16 C11 C12 116.5(16) . . ?
C16 C11 B1 123.0(16) . . ?
C66A C663 C665 112.0(15) . . ?
C66A C663 C664 110.9(16) . . ?
C664 C663 C665 108.9(16) . . ?
C43A C42A C423 116.1(14) . . ?
C43A C42A C41A 120.0(15) . . ?
C41A C42A C423 123.8(14) . . ?
C54A C55A C56A 122.7(16) . . ?
C31 C36 C360 118.8(17) . . ?
C35 C36 C31 122.4(17) . . ?
C35 C36 C360 118.7(17) . . ?
C54A C53A C52A 121.1(15) . . ?
C525 C523 C52A 109.0(16) . . ?
C525 C523 C524 110.5(16) . . ?
C524 C523 C52A 111.7(15) . . ?
C31 C32 C320 123.0(16) . . ?
C33 C32 C320 117.3(16) . . ?
C33 C32 C31 119.7(16) . . ?
C44A C443 C444 108.5(16) . . ?
C44A C443 C445 112.7(16) . . ?
C445 C443 C444 109.9(16) . . ?
O1 B1 C11 121.0(14) . . ?
O1 B1 C21 119.9(15) . . ?
C11 B1 C21 119.0(13) . . ?
C11A C12A C123 123.3(15) . . ?
C11A C12A C13A 121.8(15) . . ?
C13A C12A C123 114.9(15) . . ?
C561 C560 C56 111.8(15) . . ?
C561 C560 C562 108.2(15) . . ?
C56 C560 C562 113.4(15) . . ?
C62 C620 C621 108.5(14) . . ?
C62 C620 C622 114.6(15) . . ?
C622 C620 C621 108.7(15) . . ?
C31A C36A C363 121.4(13) . . ?
C35A C36A C363 119.9(13) . . ?
C35A C36A C31A 118.7(14) . . ?
C53 C52 C520 119.5(15) . . ?
C53 C52 C51 120.5(14) . . ?
C51 C52 C520 119.9(13) . . ?
C66 C660 C661 112.8(15) . . ?
C662 C660 C66 111.2(15) . . ?
C662 C660 C661 109.3(17) . . ?
C44A C45A C46A 122.0(16) . . ?
C53A C52A C523 116.9(15) . . ?
C53A C52A C51A 120.0(16) . . ?
C51A C52A C523 123.1(14) . . ?
C55A C54A C53A 118.3(15) . . ?
C55A C54A C543 121.7(15) . . ?
C53A C54A C543 119.6(15) . . ?
C21 C26 C260 121.9(17) . . ?
C25 C26 C260 115.9(19) . . ?
C25 C26 C21 121.5(18) . . ?
C465 C463 C464 109.8(16) . . ?
C46A C463 C465 112.4(14) . . ?
C46A C463 C464 110.6(14) . . ?
C61 C62 C620 123.1(16) . . ?
C61 C62 C63 118.2(15) . . ?
C63 C62 C620 118.7(14) . . ?
C15A C14A C13A 119.4(17) . . ?
C15A C14A C143 119.9(15) . . ?
C13A C14A C143 120.5(16) . . ?
C16 C15 C14 123(2) . . ?
C36 C35 C34 120.7(18) . . ?
C42A C41A C46A 118.2(14) . . ?
C42A C41A B2A 120.0(15) . . ?
C46A C41A B2A 121.8(14) . . ?
C66A C65A C64A 124.2(18) . . ?
C22A C223 C224 113.1(15) . . ?
C225 C223 C22A 112.2(16) . . ?
C225 C223 C224 110.5(16) . . ?
C42 C41 B2 117.2(15) . . ?
C42 C41 C46 119.9(17) . . ?
C46 C41 B2 122.9(17) . . ?
C36A C31A B2A 120.9(13) . . ?
C32A C31A C36A 118.9(14) . . ?
C32A C31A B2A 120.3(13) . . ?
C63A C64A C65A 117.9(18) . . ?
C63A C64A C643 120.3(16) . . ?
C65A C64A C643 121.7(17) . . ?
C122 C120 C12 113.0(14) . . ?
C122 C120 C121 109.6(15) . . ?
C121 C120 C12 109.5(14) . . ?
C64 C63 C62 123.0(15) . . ?
C64 C65 C66 121.2(17) . . ?
C61 C66 C660 120.3(16) . . ?
C65 C66 C61 119.5(15) . . ?
C65 C66 C660 120.1(16) . . ?
C31A C32A C323 120.9(14) . . ?
C33A C32A C31A 120.9(13) . . ?
C33A C32A C323 118.1(14) . . ?
C11A C16A C163 121.0(16) . . ?
C15A C16A C11A 120.1(16) . . ?
C15A C16A C163 118.8(15) . . ?
C34A C33A C32A 119.6(15) . . ?
C35 C34 C33 114.3(18) . . ?
C35 C34 C340 122.4(18) . . ?
C33 C34 C340 123.1(18) . . ?
C33A C34A C343 117.6(15) . . ?
C33A C34A C35A 119.5(16) . . ?
C35A C34A C343 122.9(14) . . ?
C32 C33 C34 124.7(18) . . ?
C51 C56 C560 120.1(14) . . ?
C55 C56 C560 120.6(15) . . ?
C55 C56 C51 119.2(16) . . ?
O3A B3A C61 121.4(14) . . ?
O3A B3A C51 115.2(15) . . ?
C61 B3A C51 123.3(14) . . ?
C32A C323 C325 112.9(13) . . ?
C324 C323 C32A 110.1(14) . . ?
C324 C323 C325 110.7(14) . . ?
C26 C21 B1 124.4(16) . . ?
C26 C21 C22 117.4(17) . . ?
C22 C21 B1 117.8(17) . . ?
C52 C51 B3A 121.3(13) . . ?
C56 C51 C52 116.4(14) . . ?
C56 C51 B3A 122.2(14) . . ?
O2 B2 C31 115.2(15) . . ?
O2 B2 C41 120.8(17) . . ?
C41 B2 C31 124.0(15) . . ?
C63 C64 C65 119.3(18) . . ?
C63 C64 C640 121.6(16) . . ?
C65 C64 C640 119.1(17) . . ?
C26A C263 C264 110.2(14) . . ?
C265 C263 C264 107.7(15) . . ?
C265 C263 C26A 112.1(13) . . ?
C13 C14 C15 113(2) . . ?
C13 C14 C140 125(2) . . ?
C140 C14 C15 121.2(19) . . ?
C36 C360 C362 111.2(17) . . ?
C361 C360 C36 115.5(17) . . ?
C361 C360 C362 110.5(18) . . ?
C45 C44 C440 115(2) . . ?
C43 C44 C45 121(2) . . ?
C43 C44 C440 124(3) . . ?
C62A C623 C624 108.8(15) . . ?
C625 C623 C624 111.6(14) . . ?
C625 C623 C62A 113.8(16) . . ?
C62A C61A C66A 117.7(16) . . ?
C62A C61A B3 122.9(15) . . ?
C66A C61A B3 119.5(14) . . ?
C24A C25A C26A 122.6(17) . . ?
C22A C23A C24A 122.3(16) . . ?
C64 C640 C642 107.9(18) . . ?
C641 C640 C64 111.2(17) . . ?
C641 C640 C642 109(2) . . ?
C21 C22 C220 121.6(17) . . ?
C23 C22 C21 118.1(19) . . ?
C23 C22 C220 120.3(16) . . ?
C21A C26A C263 122.6(14) . . ?
C21A C26A C25A 119.7(14) . . ?
C25A C26A C263 117.5(15) . . ?
C14A C15A C16A 122.3(16) . . ?
C22 C220 C222 109.3(16) . . ?
C22 C220 C221 112.1(16) . . ?
C221 C220 C222 110.4(16) . . ?
C54A C543 C544 108.7(15) . . ?
C545 C543 C54A 113.2(15) . . ?
C545 C543 C544 111.5(15) . . ?
C14A C13A C12A 119.7(17) . . ?
C34 C340 C341 112.7(17) . . ?
C34 C340 C342 111.0(18) . . ?
C341 C340 C342 109(2) . . ?
O3 B3 C61A 117.8(14) . . ?
O3 B3 C51A 118.4(15) . . ?
C51A B3 C61A 123.8(15) . . ?
C16 C160 C161 113.0(16) . . ?
C16 C160 C162 109.2(17) . . ?
C161 C160 C162 109.4(17) . . ?
C14A C143 C144 111.2(16) . . ?
C14A C143 C145 111.7(16) . . ?
C144 C143 C145 108.2(18) . . ?
O1A B1A C11A 117.9(15) . . ?
O1A B1A C21A 118.7(15) . . ?
C11A B1A C21A 123.4(13) . . ?
C56A C51A C52A 117.9(14) . . ?
C56A C51A B3 120.3(14) . . ?
C52A C51A B3 121.7(15) . . ?
C56A C563 C565 112.2(16) . . ?
C56A C563 C564 114.4(15) . . ?
C565 C563 C564 108.3(18) . . ?
C24 C23 C22 122.7(18) . . ?
C23 C24 C25 120(2) . . ?
C23 C24 C240 120.5(19) . . ?
C25 C24 C240 120(2) . . ?
C41 C46 C460 122.1(18) . . ?
C45 C46 C41 120(2) . . ?
C45 C46 C460 117.8(18) . . ?
C45A C46A C463 118.4(15) . . ?
C45A C46A C41A 120.0(14) . . ?
C41A C46A C463 121.5(13) . . ?
C14 C140 C141 116(2) . . ?
C14 C140 C142 109(2) . . ?
C141 C140 C142 107(2) . . ?
C46 C45 C44 119(2) . . ?
C54 C55 C56 123.3(18) . . ?
C21A C22A C223 120.5(14) . . ?
C23A C22A C21A 122.0(16) . . ?
C23A C22A C223 117.4(14) . . ?
C25A C24A C23A 115.8(16) . . ?
C25A C24A C243 125.2(18) . . ?
C23A C24A C243 119.0(16) . . ?
C26 C25 C24 120(2) . . ?
C46 C460 C462 109.4(17) . . ?
C46 C460 C461 113.7(17) . . ?
C461 C460 C462 112.3(16) . . ?
C24 C240 C241 111(2) . . ?
C242 C240 C24 119(2) . . ?
C242 C240 C241 110(3) . . ?
C36A C35A C34A 122.4(14) . . ?
C24A C243 C245 107.4(19) . . ?
C244 C243 C24A 112.5(19) . . ?
C244 C243 C245 107(2) . . ?
O2A B2A C41A 120.3(16) . . ?
O2A B2A C31A 119.8(14) . . ?
C31A B2A C41A 119.9(15) . . ?
C54 C540 C542 106(2) . . ?
C541 C540 C54 113(2) . . ?
C541 C540 C542 115(3) . . ?
C44 C43 C42 119(2) . . ?
C64A C643 C644 113.0(18) . . ?
C645 C643 C64A 112.4(19) . . ?
C645 C643 C644 110.5(18) . . ?
C53 C54 C540 125(2) . . ?
C55 C54 C53 116.9(19) . . ?
C55 C54 C540 117.9(19) . . ?
C442 C440 C44 108(3) . . ?
C441 C440 C44 108(3) . . ?
C441 C440 C442 113(4) . . ?
C1 O5 U1 97.0(17) . . ?
C1 O4 U1 96.5(15) . . ?
C1 O6 U1A 168(2) . . ?
O5 C1 O4 111(2) . . ?
O6 C1 O5 126(2) . . ?
O6 C1 O4 121.3(19) . . ?
C1A O4A U1A 90(3) . . ?
C1A O5A U1A 87(3) . . ?
C1A O6A U1 177.9(17) . . ?
O4A C1A O5A 131(5) . . ?
O4A C1A O6A 117(3) . . ?
O5A C1A O6A 112(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.697
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p18061
_database_code_depnum_ccdc_archive 'CCDC 1886804'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C74 H92 B4 O5 U'
_chemical_formula_sum            'C74 H92 B4 O5 U'
_chemical_formula_weight         1342.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U1 C100 H100 O4 B4'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1285(10)
_cell_length_b                   15.8427(12)
_cell_length_c                   16.6496(12)
_cell_angle_alpha                103.798(6)
_cell_angle_beta                 105.012(6)
_cell_angle_gamma                98.607(6)
_cell_volume                     3405.7(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6869
_cell_measurement_temperature    170(0)
_cell_measurement_theta_max      22.3200
_cell_measurement_theta_min      3.4450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 18 -18 0.0447
1 -18 18 0.0447
15 5 5 0.0727
-15 -5 -5 0.0727
-17 -1 17 0.0059
17 1 -17 0.0059

_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.012
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9953 18.0046 -18.0141 0.4639 -0.0697 -0.8910
0.9953 -18.0046 18.0141 -0.4639 0.0697 0.8910
14.9985 5.0084 5.0046 -0.9085 0.0994 -0.3808
-14.9985 -5.0084 -5.0046 0.9085 -0.0994 0.3808
-17.0023 -1.0174 17.0072 0.1472 -0.8012 0.5808
17.0023 1.0174 -17.0072 -0.1472 0.8012 -0.5808

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1515
_diffrn_reflns_av_unetI/netI     0.1532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78218
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.803
_diffrn_ambient_temperature      170.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -90.00   45
  2  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00  30.00   45
  3  ω    -50.00  36.00   1.00   30.00    --   18.25 -37.00-120.00   86
  4  ω    -47.00  33.00   1.00   30.00    --   18.25 -57.00-150.00   80
  5  ω    -50.00  36.00   1.00   30.00    --   18.25 -37.00 120.00   86
  6  ω     -7.00  85.00   1.00   30.00    --   18.25  77.00 150.00   92
  7  ω     34.00  89.00   1.00   30.00    --   18.25 179.00-180.00   55
  8  ω    -47.00  33.00   1.00   30.00    --   18.25 -57.00 150.00   80
  9  ω     -7.00  85.00   1.00   30.00    --   18.25  77.00-180.00   92
 10  ω    -25.00  55.00   1.00   30.00    --   18.25 -99.00  30.00   80
 11  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -30.00   45
 12  ω    -82.00  -2.00   1.00   30.00    --  -16.53 -57.00   0.00   80
 13  ω      2.00  39.00   1.00   30.00    --   18.25-133.00 132.94   37
 14  ω      3.00  84.00   1.00   30.00    --   18.25  57.00 -60.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0441474000
_diffrn_orient_matrix_UB_12      -0.0129518000
_diffrn_orient_matrix_UB_13      -0.0362565000
_diffrn_orient_matrix_UB_21      0.0240028000
_diffrn_orient_matrix_UB_22      -0.0273005000
_diffrn_orient_matrix_UB_23      -0.0247458000
_diffrn_orient_matrix_UB_31      -0.0179198000
_diffrn_orient_matrix_UB_32      -0.0364155000
_diffrn_orient_matrix_UB_33      0.0140575000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11506
_reflns_number_total             15623
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.044
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         15623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0688
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0870
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C342(H342), C115(H115), C231(H231), C344(H344), C454(H454), C335(H335),
 C233(H233), C333(H333), C113(H113), C443(H443), C225(H225), C445(H445),
 C223(H223), C122(H122), C124(H124), C452(H452)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C235(H23A,H23B,H23C), C348(H34A,H34B,H34C), C119(H11A,
 H11B,H11C), C237(H23D,H23E,H23F), C337(H33A,H33B,H33C), C339(H33D,H33E,H33F),
 C456(H45A,H45B,H45C), C346(H34D,H34E,H34F), C126(H12A,H12B,H12C), C117(H11D,
 H11E,H11F), C458(H45D,H45E,H45F), C448(H44A,H44B,H44C), C447(H44D,H44E,H44F),
 C236(H23G,H23H,H23I), C457(H45G,H45H,H45I), C227(H22A,H22B,H22C), C118(H11G,
 H11H,H11I), C128(H12D,H12E,H12F), C347(H34G,H34H,H34I), C449(H44G,H44H,H44I),
 C127(H12G,H12H,H12I), C228(H22D,H22E,H22F), C338(H33G,H33H,H33I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.43579(2) 0.33938(2) 0.75899(2) 0.01829(6) Uani 1 1 d . . . . .
O2 O 0.3979(3) 0.2461(2) 0.6365(2) 0.0237(9) Uani 1 1 d . . . . .
O5 O 0.4715(3) 0.4412(2) 0.9144(2) 0.0248(9) Uani 1 1 d . . . . .
O3 O 0.5878(3) 0.4085(2) 0.7836(2) 0.0282(10) Uani 1 1 d . . . . .
O4 O 0.3357(3) 0.4223(2) 0.7229(2) 0.0276(9) Uani 1 1 d . . . . .
O1 O 0.4287(3) 0.2417(2) 0.8283(2) 0.0235(9) Uani 1 1 d . . . . .
C221 C 0.2756(4) 0.0953(4) 0.5638(3) 0.0228(13) Uani 1 1 d . . . . .
C229 C 0.3811(4) 0.1840(3) 0.4768(3) 0.0200(13) Uani 1 1 d . . . . .
C331 C 0.7497(4) 0.3651(4) 0.7739(4) 0.0258(14) Uani 1 1 d . . . . .
C2S C 0.4722(5) 0.5349(3) 0.9290(3) 0.0337(16) Uani 1 1 d . . . . .
H2SA H 0.419496 0.543234 0.881025 0.040 Uiso 1 1 calc R . . . .
H2SB H 0.538136 0.567846 0.930251 0.040 Uiso 1 1 calc R . . . .
C226 C 0.1980(4) 0.1073(4) 0.6005(3) 0.0277(14) Uani 1 1 d . . . . .
C340 C 0.7374(4) 0.5407(4) 0.8321(3) 0.0237(13) Uani 1 1 d . . . . .
C1S C 0.5473(4) 0.4288(4) 0.9851(3) 0.0285(14) Uani 1 1 d . . . . .
H1SA H 0.614553 0.460106 0.987519 0.034 Uiso 1 1 calc R . . . .
H1SB H 0.546507 0.364514 0.974854 0.034 Uiso 1 1 calc R . . . .
C120 C 0.3031(4) 0.1245(4) 0.8519(3) 0.0257(14) Uani 1 1 d . . . . .
C230 C 0.4825(4) 0.2099(3) 0.4795(3) 0.0220(13) Uani 1 1 d . . . . .
C441 C 0.2339(4) 0.5393(4) 0.7403(4) 0.0255(14) Uani 1 1 d . . . . .
C450 C 0.2116(4) 0.4221(3) 0.5796(4) 0.0229(13) Uani 1 1 d . . . . .
C27 C 0.1871(4) 0.1992(4) 0.6445(4) 0.0365(16) Uani 1 1 d . . . . .
H27A H 0.230752 0.219298 0.704854 0.055 Uiso 1 1 calc GR . . . .
H27B H 0.116997 0.196658 0.643288 0.055 Uiso 1 1 calc GR . . . .
H27C H 0.206455 0.241175 0.613638 0.055 Uiso 1 1 calc GR . . . .
C332 C 0.7597(4) 0.2988(4) 0.8168(4) 0.0299(15) Uani 1 1 d . . . . .
C341 C 0.8320(4) 0.5743(4) 0.8948(4) 0.0258(14) Uani 1 1 d . . . . .
C234 C 0.3089(4) 0.1589(3) 0.3946(4) 0.0280(14) Uani 1 1 d . . . . .
C455 C 0.1068(4) 0.4026(4) 0.5436(4) 0.0300(15) Uani 1 1 d . . . . .
C336 C 0.7967(4) 0.3638(4) 0.7095(4) 0.0311(15) Uani 1 1 d . . . . .
C235 C 0.5687(4) 0.2407(4) 0.5640(3) 0.0366(16) Uani 1 1 d . . . . .
H23A H 0.567045 0.300191 0.597446 0.055 Uiso 1 1 calc GR . . . .
H23B H 0.632783 0.243184 0.551198 0.055 Uiso 1 1 calc GR . . . .
H23C H 0.561885 0.198737 0.597992 0.055 Uiso 1 1 calc GR . . . .
C116 C 0.5559(5) 0.0894(4) 0.8191(4) 0.0292(15) Uani 1 1 d . . . . .
C111 C 0.5060(4) 0.1218(3) 0.8778(4) 0.0274(14) Uani 1 1 d . . . . .
C345 C 0.6915(4) 0.6027(4) 0.7960(4) 0.0290(14) Uani 1 1 d . . . . .
C342 C 0.8784(4) 0.6645(4) 0.9194(4) 0.0316(15) Uani 1 1 d . . . . .
H342 H 0.942392 0.685371 0.962561 0.038 Uiso 1 1 calc R . . . .
C121 C 0.2477(5) 0.1790(4) 0.8895(4) 0.0324(15) Uani 1 1 d . . . . .
C442 C 0.1955(4) 0.5290(4) 0.8084(4) 0.0323(15) Uani 1 1 d . . . . .
C444 C 0.1786(4) 0.6826(4) 0.8417(4) 0.0361(16) Uani 1 1 d . . . . .
B2 B 0.3538(5) 0.1785(4) 0.5619(4) 0.0247(16) Uani 1 1 d . . . . .
C115 C 0.6379(5) 0.0523(4) 0.8449(4) 0.0322(15) Uani 1 1 d . . . . .
H115 H 0.670603 0.030201 0.803809 0.039 Uiso 1 1 calc R . . . .
B3 B 0.6873(5) 0.4367(4) 0.7971(4) 0.0248(16) Uani 1 1 d . . . . .
C231 C 0.5072(4) 0.2062(4) 0.4037(4) 0.0301(15) Uani 1 1 d . . . . .
H231 H 0.576045 0.222284 0.407388 0.036 Uiso 1 1 calc R . . . .
C343 C 0.8346(4) 0.7243(4) 0.8833(4) 0.0306(15) Uani 1 1 d . . . . .
C451 C 0.2686(4) 0.4081(4) 0.5219(4) 0.0304(15) Uani 1 1 d . . . . .
C125 C 0.2574(5) 0.0331(4) 0.8127(4) 0.0344(16) Uani 1 1 d . . . . .
C348 C 0.5901(4) 0.5739(4) 0.7260(4) 0.0412(17) Uani 1 1 d . . . . .
H34A H 0.588486 0.519608 0.682060 0.062 Uiso 1 1 calc GR . . . .
H34B H 0.579662 0.621459 0.698616 0.062 Uiso 1 1 calc GR . . . .
H34C H 0.536743 0.561932 0.752144 0.062 Uiso 1 1 calc GR . . . .
C344 C 0.7417(4) 0.6915(4) 0.8218(4) 0.0342(16) Uani 1 1 d . . . . .
H344 H 0.710360 0.731565 0.795815 0.041 Uiso 1 1 calc R . . . .
C454 C 0.0616(4) 0.3691(4) 0.4547(4) 0.0320(15) Uani 1 1 d . . . . .
H454 H -0.009716 0.355533 0.432293 0.038 Uiso 1 1 calc R . . . .
C335 C 0.8470(4) 0.2975(4) 0.6875(4) 0.0361(16) Uani 1 1 d . . . . .
H335 H 0.875317 0.295954 0.641441 0.043 Uiso 1 1 calc R . . . .
C453 C 0.1172(5) 0.3547(4) 0.3976(4) 0.0359(16) Uani 1 1 d . . . . .
C233 C 0.3360(5) 0.1575(3) 0.3203(3) 0.0324(16) Uani 1 1 d . . . . .
H233 H 0.284986 0.140711 0.265838 0.039 Uiso 1 1 calc R . . . .
C114 C 0.6734(5) 0.0466(4) 0.9289(4) 0.0363(16) Uani 1 1 d . . . . .
C333 C 0.8126(4) 0.2346(4) 0.7951(4) 0.0371(16) Uani 1 1 d . . . . .
H333 H 0.818264 0.190662 0.825055 0.044 Uiso 1 1 calc R . . . .
C119 C 0.5243(5) 0.0930(4) 0.7259(3) 0.0442(18) Uani 1 1 d . . . . .
H11A H 0.456863 0.105060 0.711282 0.066 Uiso 1 1 calc GR . . . .
H11B H 0.523720 0.035753 0.686750 0.066 Uiso 1 1 calc GR . . . .
H11C H 0.572056 0.140656 0.719326 0.066 Uiso 1 1 calc GR . . . .
C237 C 0.1968(4) 0.1341(4) 0.3852(4) 0.0378(16) Uani 1 1 d . . . . .
H23D H 0.178699 0.072359 0.386340 0.057 Uiso 1 1 calc GR . . . .
H23E H 0.157185 0.140168 0.329893 0.057 Uiso 1 1 calc GR . . . .
H23F H 0.182612 0.174083 0.433271 0.057 Uiso 1 1 calc GR . . . .
C112 C 0.5418(4) 0.1162(4) 0.9635(4) 0.0298(15) Uani 1 1 d . . . . .
C222 C 0.2817(4) 0.0079(4) 0.5281(4) 0.0285(14) Uani 1 1 d . . . . .
C337 C 0.7124(4) 0.2964(4) 0.8894(4) 0.0413(17) Uani 1 1 d . . . . .
H33A H 0.727369 0.356683 0.929229 0.062 Uiso 1 1 calc GR . . . .
H33B H 0.740284 0.256673 0.921406 0.062 Uiso 1 1 calc GR . . . .
H33C H 0.639428 0.274389 0.864176 0.062 Uiso 1 1 calc GR . . . .
C113 C 0.6244(5) 0.0794(4) 0.9861(4) 0.0375(17) Uani 1 1 d . . . . .
H113 H 0.648099 0.076944 1.044171 0.045 Uiso 1 1 calc R . . . .
C224 C 0.1342(5) -0.0510(4) 0.5633(4) 0.0348(16) Uani 1 1 d . . . . .
C232 C 0.4359(5) 0.1802(4) 0.3233(4) 0.0337(16) Uani 1 1 d . . . . .
C443 C 0.1676(4) 0.5996(4) 0.8570(4) 0.0396(17) Uani 1 1 d . . . . .
H443 H 0.140439 0.591156 0.901756 0.048 Uiso 1 1 calc R . . . .
C446 C 0.2445(4) 0.6229(4) 0.7250(4) 0.0349(16) Uani 1 1 d . . . . .
C339 C 0.7892(4) 0.4324(4) 0.6587(4) 0.0433(18) Uani 1 1 d . . . . .
H33D H 0.718596 0.434567 0.636108 0.065 Uiso 1 1 calc GR . . . .
H33E H 0.816458 0.415398 0.610247 0.065 Uiso 1 1 calc GR . . . .
H33F H 0.827845 0.491304 0.697257 0.065 Uiso 1 1 calc GR . . . .
B1 B 0.4132(5) 0.1650(4) 0.8518(4) 0.0246(16) Uani 1 1 d . . . . .
C334 C 0.8570(4) 0.2338(4) 0.7306(4) 0.0358(16) Uani 1 1 d . . . . .
C456 C 0.3837(4) 0.4316(4) 0.5518(4) 0.0376(16) Uani 1 1 d . . . . .
H45A H 0.408304 0.487142 0.599646 0.056 Uiso 1 1 calc GR . . . .
H45B H 0.407649 0.439329 0.503229 0.056 Uiso 1 1 calc GR . . . .
H45C H 0.408784 0.383340 0.571638 0.056 Uiso 1 1 calc GR . . . .
C225 C 0.1286(4) 0.0350(4) 0.5987(4) 0.0372(16) Uani 1 1 d . . . . .
H225 H 0.075615 0.045003 0.622564 0.045 Uiso 1 1 calc R . . . .
B4 B 0.2645(5) 0.4595(4) 0.6834(5) 0.0273(17) Uani 1 1 d . . . . .
C346 C 0.8894(4) 0.5159(4) 0.9382(4) 0.0471(19) Uani 1 1 d . . . . .
H34D H 0.844040 0.476726 0.956547 0.071 Uiso 1 1 calc GR . . . .
H34E H 0.944734 0.553345 0.989091 0.071 Uiso 1 1 calc GR . . . .
H34F H 0.916523 0.479511 0.897139 0.071 Uiso 1 1 calc GR . . . .
C126 C 0.2908(5) 0.2775(4) 0.9380(4) 0.0504(19) Uani 1 1 d . . . . .
H12A H 0.360079 0.285755 0.974435 0.076 Uiso 1 1 calc GR . . . .
H12B H 0.249872 0.298459 0.974629 0.076 Uiso 1 1 calc GR . . . .
H12C H 0.290086 0.311718 0.896010 0.076 Uiso 1 1 calc GR . . . .
C117 C 0.4958(4) 0.1538(4) 1.0321(4) 0.0402(17) Uani 1 1 d . . . . .
H11D H 0.520356 0.218780 1.053583 0.060 Uiso 1 1 calc GR . . . .
H11E H 0.514599 0.128037 1.080340 0.060 Uiso 1 1 calc GR . . . .
H11F H 0.422397 0.139197 1.007197 0.060 Uiso 1 1 calc GR . . . .
C458 C 0.0373(4) 0.4171(4) 0.5998(4) 0.0496(19) Uani 1 1 d . . . . .
H45D H 0.051568 0.385291 0.643728 0.074 Uiso 1 1 calc GR . . . .
H45E H -0.032873 0.394433 0.563103 0.074 Uiso 1 1 calc GR . . . .
H45F H 0.048643 0.481034 0.628624 0.074 Uiso 1 1 calc GR . . . .
C445 C 0.2174(4) 0.6914(4) 0.7762(4) 0.0373(17) Uani 1 1 d . . . . .
H445 H 0.226145 0.747832 0.765300 0.045 Uiso 1 1 calc R . . . .
C448 C 0.1461(5) 0.7569(4) 0.8948(4) 0.055(2) Uani 1 1 d . . . . .
H44A H 0.081427 0.733561 0.901811 0.082 Uiso 1 1 calc GR . . . .
H44B H 0.138931 0.803202 0.865113 0.082 Uiso 1 1 calc GR . . . .
H44C H 0.196718 0.782543 0.952015 0.082 Uiso 1 1 calc GR . . . .
C223 C 0.2121(5) -0.0628(4) 0.5295(4) 0.0370(16) Uani 1 1 d . . . . .
H223 H 0.218340 -0.121817 0.506132 0.044 Uiso 1 1 calc R . . . .
C122 C 0.1504(5) 0.1435(5) 0.8870(4) 0.0409(17) Uani 1 1 d . . . . .
H122 H 0.114032 0.182315 0.912150 0.049 Uiso 1 1 calc R . . . .
C124 C 0.1599(5) 0.0015(4) 0.8125(4) 0.0457(19) Uani 1 1 d . . . . .
H124 H 0.129858 -0.060080 0.785336 0.055 Uiso 1 1 calc R . . . .
C447 C 0.1786(5) 0.4403(4) 0.8286(4) 0.052(2) Uani 1 1 d . . . . .
H44D H 0.166394 0.391451 0.775737 0.078 Uiso 1 1 calc GR . . . .
H44E H 0.120226 0.434180 0.849947 0.078 Uiso 1 1 calc GR . . . .
H44F H 0.238339 0.438132 0.873190 0.078 Uiso 1 1 calc GR . . . .
C236 C 0.4653(5) 0.1768(4) 0.2417(4) 0.0423(17) Uani 1 1 d . . . . .
H23G H 0.494683 0.237404 0.242903 0.063 Uiso 1 1 calc GR . . . .
H23H H 0.405589 0.151080 0.190721 0.063 Uiso 1 1 calc GR . . . .
H23I H 0.514823 0.139920 0.238665 0.063 Uiso 1 1 calc GR . . . .
C457 C 0.0671(5) 0.3172(4) 0.3010(4) 0.057(2) Uani 1 1 d . . . . .
H45G H 0.057717 0.252129 0.284253 0.086 Uiso 1 1 calc GR . . . .
H45H H 0.109413 0.342302 0.270344 0.086 Uiso 1 1 calc GR . . . .
H45I H 0.001491 0.332722 0.285547 0.086 Uiso 1 1 calc GR . . . .
C452 C 0.2208(4) 0.3755(4) 0.4335(4) 0.0335(16) Uani 1 1 d . . . . .
H452 H 0.260850 0.366965 0.395648 0.040 Uiso 1 1 calc R . . . .
C227 C 0.3636(4) -0.0138(4) 0.4886(4) 0.0410(17) Uani 1 1 d . . . . .
H22A H 0.343248 -0.014099 0.427618 0.061 Uiso 1 1 calc GR . . . .
H22B H 0.374350 -0.072625 0.492183 0.061 Uiso 1 1 calc GR . . . .
H22C H 0.426073 0.031369 0.520569 0.061 Uiso 1 1 calc GR . . . .
C123 C 0.1047(5) 0.0544(5) 0.8495(4) 0.048(2) Uani 1 1 d . . . . .
C118 C 0.7613(5) 0.0045(4) 0.9540(4) 0.056(2) Uani 1 1 d . . . . .
H11G H 0.777474 -0.024232 0.901815 0.084 Uiso 1 1 calc GR . . . .
H11H H 0.743774 -0.040301 0.982632 0.084 Uiso 1 1 calc GR . . . .
H11I H 0.819708 0.050542 0.993980 0.084 Uiso 1 1 calc GR . . . .
C128 C 0.3101(5) -0.0322(4) 0.7693(4) 0.053(2) Uani 1 1 d . . . . .
H12D H 0.329857 -0.011706 0.723712 0.079 Uiso 1 1 calc GR . . . .
H12E H 0.264408 -0.091232 0.743603 0.079 Uiso 1 1 calc GR . . . .
H12F H 0.370156 -0.035807 0.812659 0.079 Uiso 1 1 calc GR . . . .
C347 C 0.8891(5) 0.8205(4) 0.9060(4) 0.0494(19) Uani 1 1 d . . . . .
H34G H 0.857120 0.858820 0.940877 0.074 Uiso 1 1 calc GR . . . .
H34H H 0.885951 0.837142 0.852486 0.074 Uiso 1 1 calc GR . . . .
H34I H 0.959547 0.827872 0.939318 0.074 Uiso 1 1 calc GR . . . .
C449 C 0.2815(5) 0.6388(4) 0.6510(4) 0.055(2) Uani 1 1 d . . . . .
H44G H 0.346325 0.621991 0.655928 0.082 Uiso 1 1 calc GR . . . .
H44H H 0.289705 0.702067 0.653807 0.082 Uiso 1 1 calc GR . . . .
H44I H 0.232486 0.602634 0.595442 0.082 Uiso 1 1 calc GR . . . .
C127 C 0.0004(5) 0.0163(5) 0.8507(4) 0.068(2) Uani 1 1 d . . . . .
H12G H 0.005795 -0.009981 0.898869 0.102 Uiso 1 1 calc GR . . . .
H12H H -0.035806 -0.029723 0.795669 0.102 Uiso 1 1 calc GR . . . .
H12I H -0.036176 0.064045 0.858326 0.102 Uiso 1 1 calc GR . . . .
C228 C 0.0587(5) -0.1304(4) 0.5619(4) 0.059(2) Uani 1 1 d . . . . .
H22D H 0.050412 -0.122279 0.619732 0.089 Uiso 1 1 calc GR . . . .
H22E H 0.082852 -0.184867 0.545624 0.089 Uiso 1 1 calc GR . . . .
H22F H -0.006160 -0.135342 0.519507 0.089 Uiso 1 1 calc GR . . . .
C338 C 0.9153(5) 0.1643(4) 0.7069(4) 0.058(2) Uani 1 1 d . . . . .
H33G H 0.924686 0.162964 0.650302 0.086 Uiso 1 1 calc GR . . . .
H33H H 0.878015 0.105603 0.703707 0.086 Uiso 1 1 calc GR . . . .
H33I H 0.981149 0.179138 0.751150 0.086 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O2 2.095(3) . ?
U1 O5 2.577(3) . ?
U1 O3 2.146(4) . ?
U1 O4 2.140(4) . ?
U1 O1 2.145(3) . ?
O2 B2 1.357(7) . ?
O5 C2S 1.445(6) . ?
O5 C1S 1.445(6) . ?
O3 B3 1.352(7) . ?
O4 B4 1.346(7) . ?
O1 B1 1.368(6) . ?
C221 C226 1.402(7) . ?
C221 B2 1.599(8) . ?
C221 C222 1.396(7) . ?
C229 C230 1.415(7) . ?
C229 C234 1.402(7) . ?
C229 B2 1.581(8) . ?
C331 C332 1.408(7) . ?
C331 C336 1.397(7) . ?
C331 B3 1.575(8) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C2S C1S 1.521(7) 2_667 ?
C226 C27 1.517(7) . ?
C226 C225 1.382(7) . ?
C340 C341 1.399(7) . ?
C340 C345 1.421(7) . ?
C340 B3 1.593(8) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C120 C121 1.395(8) . ?
C120 C125 1.412(7) . ?
C120 B1 1.592(8) . ?
C230 C235 1.520(7) . ?
C230 C231 1.384(7) . ?
C441 C442 1.411(7) . ?
C441 C446 1.400(7) . ?
C441 B4 1.576(8) . ?
C450 C455 1.401(7) . ?
C450 C451 1.404(7) . ?
C450 B4 1.613(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C332 C333 1.384(7) . ?
C332 C337 1.531(7) . ?
C341 C342 1.392(7) . ?
C341 C346 1.510(7) . ?
C234 C233 1.383(7) . ?
C234 C237 1.531(7) . ?
C455 C454 1.383(7) . ?
C455 C458 1.529(7) . ?
C336 C335 1.385(8) . ?
C336 C339 1.527(7) . ?
C235 H23A 0.9800 . ?
C235 H23B 0.9800 . ?
C235 H23C 0.9800 . ?
C116 C111 1.394(7) . ?
C116 C115 1.393(7) . ?
C116 C119 1.518(7) . ?
C111 C112 1.414(7) . ?
C111 B1 1.578(8) . ?
C345 C348 1.518(7) . ?
C345 C344 1.386(7) . ?
C342 H342 0.9500 . ?
C342 C343 1.378(7) . ?
C121 C126 1.523(8) . ?
C121 C122 1.391(7) . ?
C442 C443 1.388(8) . ?
C442 C447 1.520(7) . ?
C444 C443 1.391(8) . ?
C444 C445 1.367(8) . ?
C444 C448 1.502(8) . ?
C115 H115 0.9500 . ?
C115 C114 1.387(7) . ?
C231 H231 0.9500 . ?
C231 C232 1.375(7) . ?
C343 C344 1.374(7) . ?
C343 C347 1.510(7) . ?
C451 C456 1.530(7) . ?
C451 C452 1.382(7) . ?
C125 C124 1.393(8) . ?
C125 C128 1.516(8) . ?
C348 H34A 0.9800 . ?
C348 H34B 0.9800 . ?
C348 H34C 0.9800 . ?
C344 H344 0.9500 . ?
C454 H454 0.9500 . ?
C454 C453 1.382(8) . ?
C335 H335 0.9500 . ?
C335 C334 1.374(7) . ?
C453 C457 1.506(7) . ?
C453 C452 1.385(7) . ?
C233 H233 0.9500 . ?
C233 C232 1.387(7) . ?
C114 C113 1.368(8) . ?
C114 C118 1.508(8) . ?
C333 H333 0.9500 . ?
C333 C334 1.376(7) . ?
C119 H11A 0.9800 . ?
C119 H11B 0.9800 . ?
C119 H11C 0.9800 . ?
C237 H23D 0.9800 . ?
C237 H23E 0.9800 . ?
C237 H23F 0.9800 . ?
C112 C113 1.387(7) . ?
C112 C117 1.503(7) . ?
C222 C223 1.385(7) . ?
C222 C227 1.513(7) . ?
C337 H33A 0.9800 . ?
C337 H33B 0.9800 . ?
C337 H33C 0.9800 . ?
C113 H113 0.9500 . ?
C224 C225 1.372(8) . ?
C224 C223 1.377(8) . ?
C224 C228 1.515(7) . ?
C232 C236 1.513(7) . ?
C443 H443 0.9500 . ?
C446 C445 1.380(8) . ?
C446 C449 1.516(7) . ?
C339 H33D 0.9800 . ?
C339 H33E 0.9800 . ?
C339 H33F 0.9800 . ?
C334 C338 1.510(8) . ?
C456 H45A 0.9800 . ?
C456 H45B 0.9800 . ?
C456 H45C 0.9800 . ?
C225 H225 0.9500 . ?
C346 H34D 0.9800 . ?
C346 H34E 0.9800 . ?
C346 H34F 0.9800 . ?
C126 H12A 0.9800 . ?
C126 H12B 0.9800 . ?
C126 H12C 0.9800 . ?
C117 H11D 0.9800 . ?
C117 H11E 0.9800 . ?
C117 H11F 0.9800 . ?
C458 H45D 0.9800 . ?
C458 H45E 0.9800 . ?
C458 H45F 0.9800 . ?
C445 H445 0.9500 . ?
C448 H44A 0.9800 . ?
C448 H44B 0.9800 . ?
C448 H44C 0.9800 . ?
C223 H223 0.9500 . ?
C122 H122 0.9500 . ?
C122 C123 1.377(8) . ?
C124 H124 0.9500 . ?
C124 C123 1.375(9) . ?
C447 H44D 0.9800 . ?
C447 H44E 0.9800 . ?
C447 H44F 0.9800 . ?
C236 H23G 0.9800 . ?
C236 H23H 0.9800 . ?
C236 H23I 0.9800 . ?
C457 H45G 0.9800 . ?
C457 H45H 0.9800 . ?
C457 H45I 0.9800 . ?
C452 H452 0.9500 . ?
C227 H22A 0.9800 . ?
C227 H22B 0.9800 . ?
C227 H22C 0.9800 . ?
C123 C127 1.513(8) . ?
C118 H11G 0.9800 . ?
C118 H11H 0.9800 . ?
C118 H11I 0.9800 . ?
C128 H12D 0.9800 . ?
C128 H12E 0.9800 . ?
C128 H12F 0.9800 . ?
C347 H34G 0.9800 . ?
C347 H34H 0.9800 . ?
C347 H34I 0.9800 . ?
C449 H44G 0.9800 . ?
C449 H44H 0.9800 . ?
C449 H44I 0.9800 . ?
C127 H12G 0.9800 . ?
C127 H12H 0.9800 . ?
C127 H12I 0.9800 . ?
C228 H22D 0.9800 . ?
C228 H22E 0.9800 . ?
C228 H22F 0.9800 . ?
C338 H33G 0.9800 . ?
C338 H33H 0.9800 . ?
C338 H33I 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O5 173.85(12) . . ?
O2 U1 O3 105.14(13) . . ?
O2 U1 O4 97.28(13) . . ?
O2 U1 O1 95.08(13) . . ?
O3 U1 O5 79.75(12) . . ?
O4 U1 O5 84.39(12) . . ?
O4 U1 O3 109.33(13) . . ?
O4 U1 O1 131.96(13) . . ?
O1 U1 O5 79.50(12) . . ?
O1 U1 O3 111.75(13) . . ?
B2 O2 U1 166.5(4) . . ?
C2S O5 U1 120.1(3) . . ?
C2S O5 C1S 109.8(4) . . ?
C1S O5 U1 119.3(3) . . ?
B3 O3 U1 169.2(4) . . ?
B4 O4 U1 167.1(4) . . ?
B1 O1 U1 165.5(4) . . ?
C226 C221 B2 121.4(5) . . ?
C222 C221 C226 117.5(5) . . ?
C222 C221 B2 121.1(5) . . ?
C230 C229 B2 120.7(5) . . ?
C234 C229 C230 116.3(5) . . ?
C234 C229 B2 122.8(5) . . ?
C332 C331 B3 121.2(5) . . ?
C336 C331 C332 117.0(5) . . ?
C336 C331 B3 121.7(5) . . ?
O5 C2S H2SA 109.8 . . ?
O5 C2S H2SB 109.8 . . ?
O5 C2S C1S 109.5(4) . 2_667 ?
H2SA C2S H2SB 108.2 . . ?
C1S C2S H2SA 109.8 2_667 . ?
C1S C2S H2SB 109.8 2_667 . ?
C221 C226 C27 121.9(5) . . ?
C225 C226 C221 121.0(5) . . ?
C225 C226 C27 117.1(5) . . ?
C341 C340 C345 116.9(5) . . ?
C341 C340 B3 121.7(5) . . ?
C345 C340 B3 121.2(5) . . ?
O5 C1S C2S 110.5(4) . 2_667 ?
O5 C1S H1SA 109.5 . . ?
O5 C1S H1SB 109.5 . . ?
C2S C1S H1SA 109.5 2_667 . ?
C2S C1S H1SB 109.5 2_667 . ?
H1SA C1S H1SB 108.1 . . ?
C121 C120 C125 117.7(5) . . ?
C121 C120 B1 120.9(5) . . ?
C125 C120 B1 121.4(6) . . ?
C229 C230 C235 122.3(5) . . ?
C231 C230 C229 120.6(5) . . ?
C231 C230 C235 117.1(5) . . ?
C442 C441 B4 121.1(5) . . ?
C446 C441 C442 117.8(5) . . ?
C446 C441 B4 121.1(5) . . ?
C455 C450 C451 117.3(5) . . ?
C455 C450 B4 121.2(5) . . ?
C451 C450 B4 121.5(5) . . ?
C226 C27 H27A 109.5 . . ?
C226 C27 H27B 109.5 . . ?
C226 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C331 C332 C337 120.5(5) . . ?
C333 C332 C331 121.3(5) . . ?
C333 C332 C337 118.2(5) . . ?
C340 C341 C346 122.5(5) . . ?
C342 C341 C340 120.9(5) . . ?
C342 C341 C346 116.6(5) . . ?
C229 C234 C237 120.5(5) . . ?
C233 C234 C229 121.5(6) . . ?
C233 C234 C237 118.0(5) . . ?
C450 C455 C458 122.0(5) . . ?
C454 C455 C450 121.1(5) . . ?
C454 C455 C458 116.9(5) . . ?
C331 C336 C339 120.9(5) . . ?
C335 C336 C331 120.5(5) . . ?
C335 C336 C339 118.6(5) . . ?
C230 C235 H23A 109.5 . . ?
C230 C235 H23B 109.5 . . ?
C230 C235 H23C 109.5 . . ?
H23A C235 H23B 109.5 . . ?
H23A C235 H23C 109.5 . . ?
H23B C235 H23C 109.5 . . ?
C111 C116 C119 122.2(5) . . ?
C115 C116 C111 120.3(5) . . ?
C115 C116 C119 117.5(5) . . ?
C116 C111 C112 118.0(5) . . ?
C116 C111 B1 122.1(5) . . ?
C112 C111 B1 119.9(5) . . ?
C340 C345 C348 121.8(5) . . ?
C344 C345 C340 119.8(5) . . ?
C344 C345 C348 118.4(5) . . ?
C341 C342 H342 119.0 . . ?
C343 C342 C341 122.1(6) . . ?
C343 C342 H342 119.0 . . ?
C120 C121 C126 122.6(5) . . ?
C122 C121 C120 120.4(6) . . ?
C122 C121 C126 116.9(6) . . ?
C441 C442 C447 121.9(5) . . ?
C443 C442 C441 120.2(5) . . ?
C443 C442 C447 117.8(5) . . ?
C443 C444 C448 120.0(6) . . ?
C445 C444 C443 117.1(6) . . ?
C445 C444 C448 122.9(6) . . ?
O2 B2 C221 118.3(5) . . ?
O2 B2 C229 119.5(5) . . ?
C229 B2 C221 122.3(5) . . ?
C116 C115 H115 119.0 . . ?
C114 C115 C116 122.1(6) . . ?
C114 C115 H115 119.0 . . ?
O3 B3 C331 118.6(5) . . ?
O3 B3 C340 119.6(5) . . ?
C331 B3 C340 121.7(5) . . ?
C230 C231 H231 118.8 . . ?
C232 C231 C230 122.5(5) . . ?
C232 C231 H231 118.8 . . ?
C342 C343 C347 121.5(6) . . ?
C344 C343 C342 117.1(5) . . ?
C344 C343 C347 121.3(5) . . ?
C450 C451 C456 123.0(5) . . ?
C452 C451 C450 120.0(5) . . ?
C452 C451 C456 117.0(5) . . ?
C120 C125 C128 122.4(6) . . ?
C124 C125 C120 119.1(6) . . ?
C124 C125 C128 118.5(6) . . ?
C345 C348 H34A 109.5 . . ?
C345 C348 H34B 109.5 . . ?
C345 C348 H34C 109.5 . . ?
H34A C348 H34B 109.5 . . ?
H34A C348 H34C 109.5 . . ?
H34B C348 H34C 109.5 . . ?
C345 C344 H344 118.5 . . ?
C343 C344 C345 123.1(5) . . ?
C343 C344 H344 118.5 . . ?
C455 C454 H454 119.1 . . ?
C453 C454 C455 121.9(6) . . ?
C453 C454 H454 119.1 . . ?
C336 C335 H335 119.1 . . ?
C334 C335 C336 121.8(6) . . ?
C334 C335 H335 119.1 . . ?
C454 C453 C457 121.4(6) . . ?
C454 C453 C452 116.8(6) . . ?
C452 C453 C457 121.8(6) . . ?
C234 C233 H233 119.2 . . ?
C234 C233 C232 121.7(6) . . ?
C232 C233 H233 119.2 . . ?
C115 C114 C118 120.5(6) . . ?
C113 C114 C115 117.0(6) . . ?
C113 C114 C118 122.4(6) . . ?
C332 C333 H333 119.6 . . ?
C334 C333 C332 120.7(6) . . ?
C334 C333 H333 119.6 . . ?
C116 C119 H11A 109.5 . . ?
C116 C119 H11B 109.5 . . ?
C116 C119 H11C 109.5 . . ?
H11A C119 H11B 109.5 . . ?
H11A C119 H11C 109.5 . . ?
H11B C119 H11C 109.5 . . ?
C234 C237 H23D 109.5 . . ?
C234 C237 H23E 109.5 . . ?
C234 C237 H23F 109.5 . . ?
H23D C237 H23E 109.5 . . ?
H23D C237 H23F 109.5 . . ?
H23E C237 H23F 109.5 . . ?
C111 C112 C117 121.4(5) . . ?
C113 C112 C111 119.4(5) . . ?
C113 C112 C117 119.1(5) . . ?
C221 C222 C227 122.6(5) . . ?
C223 C222 C221 119.8(5) . . ?
C223 C222 C227 117.6(5) . . ?
C332 C337 H33A 109.5 . . ?
C332 C337 H33B 109.5 . . ?
C332 C337 H33C 109.5 . . ?
H33A C337 H33B 109.5 . . ?
H33A C337 H33C 109.5 . . ?
H33B C337 H33C 109.5 . . ?
C114 C113 C112 123.2(6) . . ?
C114 C113 H113 118.4 . . ?
C112 C113 H113 118.4 . . ?
C225 C224 C223 117.5(5) . . ?
C225 C224 C228 121.7(6) . . ?
C223 C224 C228 120.8(6) . . ?
C231 C232 C233 117.3(5) . . ?
C231 C232 C236 121.2(6) . . ?
C233 C232 C236 121.5(6) . . ?
C442 C443 C444 121.6(6) . . ?
C442 C443 H443 119.2 . . ?
C444 C443 H443 119.2 . . ?
C441 C446 C449 121.3(5) . . ?
C445 C446 C441 119.6(6) . . ?
C445 C446 C449 119.1(5) . . ?
C336 C339 H33D 109.5 . . ?
C336 C339 H33E 109.5 . . ?
C336 C339 H33F 109.5 . . ?
H33D C339 H33E 109.5 . . ?
H33D C339 H33F 109.5 . . ?
H33E C339 H33F 109.5 . . ?
O1 B1 C120 118.3(5) . . ?
O1 B1 C111 118.0(5) . . ?
C111 B1 C120 123.7(5) . . ?
C335 C334 C333 118.6(6) . . ?
C335 C334 C338 120.3(6) . . ?
C333 C334 C338 121.1(6) . . ?
C451 C456 H45A 109.5 . . ?
C451 C456 H45B 109.5 . . ?
C451 C456 H45C 109.5 . . ?
H45A C456 H45B 109.5 . . ?
H45A C456 H45C 109.5 . . ?
H45B C456 H45C 109.5 . . ?
C226 C225 H225 119.2 . . ?
C224 C225 C226 121.6(6) . . ?
C224 C225 H225 119.2 . . ?
O4 B4 C441 118.8(6) . . ?
O4 B4 C450 120.1(5) . . ?
C441 B4 C450 121.1(5) . . ?
C341 C346 H34D 109.5 . . ?
C341 C346 H34E 109.5 . . ?
C341 C346 H34F 109.5 . . ?
H34D C346 H34E 109.5 . . ?
H34D C346 H34F 109.5 . . ?
H34E C346 H34F 109.5 . . ?
C121 C126 H12A 109.5 . . ?
C121 C126 H12B 109.5 . . ?
C121 C126 H12C 109.5 . . ?
H12A C126 H12B 109.5 . . ?
H12A C126 H12C 109.5 . . ?
H12B C126 H12C 109.5 . . ?
C112 C117 H11D 109.5 . . ?
C112 C117 H11E 109.5 . . ?
C112 C117 H11F 109.5 . . ?
H11D C117 H11E 109.5 . . ?
H11D C117 H11F 109.5 . . ?
H11E C117 H11F 109.5 . . ?
C455 C458 H45D 109.5 . . ?
C455 C458 H45E 109.5 . . ?
C455 C458 H45F 109.5 . . ?
H45D C458 H45E 109.5 . . ?
H45D C458 H45F 109.5 . . ?
H45E C458 H45F 109.5 . . ?
C444 C445 C446 123.6(6) . . ?
C444 C445 H445 118.2 . . ?
C446 C445 H445 118.2 . . ?
C444 C448 H44A 109.5 . . ?
C444 C448 H44B 109.5 . . ?
C444 C448 H44C 109.5 . . ?
H44A C448 H44B 109.5 . . ?
H44A C448 H44C 109.5 . . ?
H44B C448 H44C 109.5 . . ?
C222 C223 H223 118.7 . . ?
C224 C223 C222 122.6(6) . . ?
C224 C223 H223 118.7 . . ?
C121 C122 H122 118.6 . . ?
C123 C122 C121 122.8(7) . . ?
C123 C122 H122 118.6 . . ?
C125 C124 H124 118.2 . . ?
C123 C124 C125 123.7(6) . . ?
C123 C124 H124 118.2 . . ?
C442 C447 H44D 109.5 . . ?
C442 C447 H44E 109.5 . . ?
C442 C447 H44F 109.5 . . ?
H44D C447 H44E 109.5 . . ?
H44D C447 H44F 109.5 . . ?
H44E C447 H44F 109.5 . . ?
C232 C236 H23G 109.5 . . ?
C232 C236 H23H 109.5 . . ?
C232 C236 H23I 109.5 . . ?
H23G C236 H23H 109.5 . . ?
H23G C236 H23I 109.5 . . ?
H23H C236 H23I 109.5 . . ?
C453 C457 H45G 109.5 . . ?
C453 C457 H45H 109.5 . . ?
C453 C457 H45I 109.5 . . ?
H45G C457 H45H 109.5 . . ?
H45G C457 H45I 109.5 . . ?
H45H C457 H45I 109.5 . . ?
C451 C452 C453 122.9(6) . . ?
C451 C452 H452 118.5 . . ?
C453 C452 H452 118.5 . . ?
C222 C227 H22A 109.5 . . ?
C222 C227 H22B 109.5 . . ?
C222 C227 H22C 109.5 . . ?
H22A C227 H22B 109.5 . . ?
H22A C227 H22C 109.5 . . ?
H22B C227 H22C 109.5 . . ?
C122 C123 C127 122.0(7) . . ?
C124 C123 C122 116.3(6) . . ?
C124 C123 C127 121.7(7) . . ?
C114 C118 H11G 109.5 . . ?
C114 C118 H11H 109.5 . . ?
C114 C118 H11I 109.5 . . ?
H11G C118 H11H 109.5 . . ?
H11G C118 H11I 109.5 . . ?
H11H C118 H11I 109.5 . . ?
C125 C128 H12D 109.5 . . ?
C125 C128 H12E 109.5 . . ?
C125 C128 H12F 109.5 . . ?
H12D C128 H12E 109.5 . . ?
H12D C128 H12F 109.5 . . ?
H12E C128 H12F 109.5 . . ?
C343 C347 H34G 109.5 . . ?
C343 C347 H34H 109.5 . . ?
C343 C347 H34I 109.5 . . ?
H34G C347 H34H 109.5 . . ?
H34G C347 H34I 109.5 . . ?
H34H C347 H34I 109.5 . . ?
C446 C449 H44G 109.5 . . ?
C446 C449 H44H 109.5 . . ?
C446 C449 H44I 109.5 . . ?
H44G C449 H44H 109.5 . . ?
H44G C449 H44I 109.5 . . ?
H44H C449 H44I 109.5 . . ?
C123 C127 H12G 109.5 . . ?
C123 C127 H12H 109.5 . . ?
C123 C127 H12I 109.5 . . ?
H12G C127 H12H 109.5 . . ?
H12G C127 H12I 109.5 . . ?
H12H C127 H12I 109.5 . . ?
C224 C228 H22D 109.5 . . ?
C224 C228 H22E 109.5 . . ?
C224 C228 H22F 109.5 . . ?
H22D C228 H22E 109.5 . . ?
H22D C228 H22F 109.5 . . ?
H22E C228 H22F 109.5 . . ?
C334 C338 H33G 109.5 . . ?
C334 C338 H33H 109.5 . . ?
C334 C338 H33I 109.5 . . ?
H33G C338 H33H 109.5 . . ?
H33G C338 H33I 109.5 . . ?
H33H C338 H33I 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.881

# start Validation Reply Form
_vrf_PLAT973_p18061              
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       3.78 eA-3  
RESPONSE: Uranium is a heavy metal therefore residual density
could be expected, therefore this is not seen as a serious problem.
;
_vrf_PLAT910_p18061              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note  
RESPONSE: No. of reflections / No. of parameters = 20.0 Therefore
this is not seen as a serious problem.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p18033
_database_code_depnum_ccdc_archive 'CCDC 1886807'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H66 B3 O3 S2 U, C6 H6, C3'
_chemical_formula_sum            'C63 H72 B3 O3 S2 U'
_chemical_formula_weight         1211.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H200 B3 O3 S2 U2'
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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3086(2)
_cell_length_b                   14.3349(2)
_cell_length_c                   21.6092(4)
_cell_angle_alpha                77.2060(10)
_cell_angle_beta                 87.1260(10)
_cell_angle_gamma                84.9070(10)
_cell_volume                     3701.62(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18918
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1830
_cell_measurement_theta_min      3.2990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent red'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1226
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 20 9 0.1334
-1 -20 -9 0.1334
-17 -2 2 0.1781
17 2 -2 0.1781
1 -1 29 0.0230
-1 1 -29 0.0230

_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.046
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9984 19.9905 8.9809 -0.2873 0.9280 -0.2047
-0.9984 -19.9905 -8.9809 0.2873 -0.9280 0.2047
-16.9918 -2.0003 2.0237 0.0788 -0.2488 -0.9516
16.9918 2.0003 -2.0237 -0.0788 0.2488 0.9516
1.0156 -0.9884 28.9926 -0.9458 -0.2792 -0.0714
-1.0156 0.9884 -28.9926 0.9458 0.2792 0.0714

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78705
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.924
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  22.00   0.75    5.00    --  -18.04 103.00  34.26  108
  2  ω    -25.00  20.00   0.75    5.00    --  -18.04 -99.00-120.00   60
  3  ω    -85.00  -1.00   0.75    5.00    --  -18.04 -57.00 -90.00  112
  4  ω     -7.00  86.00   0.75    5.00    --   19.60  77.00 -90.00  124
  5  ω    -48.00  36.00   0.75    5.00    --   19.60 -57.00   0.00  112
  6  ω      3.00  87.00   0.75    5.00    --   19.60  57.00 -90.00  112
  7  ω    -48.00  45.00   0.75    5.00    --   19.60 -77.00 150.00  124
  8  ω    -25.00  20.00   0.75    5.00    --  -18.04 -99.00 120.00   60
  9  ω    -67.00   8.75   0.75    5.00    --  -18.04 117.00-122.00  101
 10  ω    -85.00  -1.00   0.75    5.00    --  -18.04 -57.00   0.00  112
 11  ω     34.00  91.00   0.75    5.00    --   19.60 179.00 -60.00   76
 12  ω      3.00  87.00   0.75    5.00    --   19.60  57.00-180.00  112
 13  ω    -10.00  89.75   0.75    5.00    --   19.60  19.00 150.00  133
 14  ω    -25.00  10.25   0.75    5.00    --   19.60 -99.00-150.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085544000
_diffrn_orient_matrix_UB_12      0.0005694000
_diffrn_orient_matrix_UB_13      -0.0323028000
_diffrn_orient_matrix_UB_21      0.0078122000
_diffrn_orient_matrix_UB_22      0.0497172000
_diffrn_orient_matrix_UB_23      -0.0082083000
_diffrn_orient_matrix_UB_31      0.0567119000
_diffrn_orient_matrix_UB_32      -0.0109058000
_diffrn_orient_matrix_UB_33      -0.0048205000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12610
_reflns_number_total             15098
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.258
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         15098
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0442
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0657P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C7S(0.5) C9S(0.5) C8S(0.5) C11S(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C115(H115), C232(H232), C335(H335), C333(H333), C113(H113), C344(H344),
 C124(H124), C223(H223), C3AA(H3AA), C122(H122), C225(H225), C342(H342),
 C4S(H4S), C3S(H3S), C2S(H2S), C1S(H1S)
3.b Idealised Me refined as rotating group:
 C235(H23A,H23B,H23C), C337(H33A,H33B,H33C), C346(H34A,H34B,H34C), C348(H34D,
 H34E,H34F), C227(H22A,H22B,H22C), C117(H11A,H11B,H11C), C339(H33D,H33E,H33F),
 C119(H11D,H11E,H11F), C234(H23D,H23E,H23F), C126(H12A,H12B,H12C), C229(H22D,
 H22E,H22F), C128(H12D,H12E,H12F), C118(H11G,H11H,H11I), C347(H34G,H34H,H34I),
 C338(H33G,H33H,H33I), C233(H23G,H23H,H23I), C228(H22G,H22H,H22I), C127(H12G,
 H12H,H12I)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.56172(2) 0.49392(2) 0.58229(2) 0.02267(6) Uani 1 1 d . . . . .
S1B S 0.63191(10) 0.57174(9) 0.46224(6) 0.0324(3) Uani 1 1 d . . . . .
S2B S 0.63206(10) 0.42650(9) 0.47065(6) 0.0335(3) Uani 1 1 d . . . . .
O3 O 0.5638(2) 0.6340(2) 0.59387(14) 0.0267(7) Uani 1 1 d . . . . .
O1 O 0.7208(2) 0.4604(2) 0.61229(14) 0.0286(7) Uani 1 1 d . . . . .
O2 O 0.4936(2) 0.4355(2) 0.67069(14) 0.0302(7) Uani 1 1 d . . . . .
C111 C 0.8634(4) 0.3244(3) 0.6548(2) 0.0304(10) Uani 1 1 d . . . . .
C331 C 0.6087(4) 0.7880(3) 0.5197(2) 0.0289(10) Uani 1 1 d . . . . .
C1AA C 0.5790(4) 0.2255(3) 0.7013(2) 0.0319(11) Uani 1 1 d . . . . .
C332 C 0.7147(4) 0.7701(3) 0.4950(2) 0.0312(11) Uani 1 1 d . . . . .
C112 C 0.8756(4) 0.2680(3) 0.7165(2) 0.0313(11) Uani 1 1 d . . . . .
C235 C 0.5827(4) 0.2616(3) 0.6307(2) 0.0347(11) Uani 1 1 d . . . . .
H23A H 0.512989 0.292956 0.617215 0.052 Uiso 1 1 calc GR . . . .
H23B H 0.599842 0.208663 0.610443 0.052 Uiso 1 1 calc GR . . . .
H23C H 0.637694 0.306432 0.619123 0.052 Uiso 1 1 calc GR . . . .
C340 C 0.5289(4) 0.7780(3) 0.6440(2) 0.0337(11) Uani 1 1 d . . . . .
C230 C 0.5159(4) 0.2713(4) 0.7439(2) 0.0357(11) Uani 1 1 d . . . . .
C120 C 0.8727(4) 0.5142(3) 0.6674(2) 0.0314(11) Uani 1 1 d . . . . .
C336 C 0.5379(4) 0.8589(3) 0.4814(2) 0.0376(12) Uani 1 1 d . . . . .
C116 C 0.8923(4) 0.2806(4) 0.6027(2) 0.0378(12) Uani 1 1 d . . . . .
C125 C 0.8145(4) 0.5695(3) 0.7068(2) 0.0321(11) Uani 1 1 d . . . . .
C115 C 0.9304(4) 0.1843(4) 0.6142(3) 0.0466(14) Uani 1 1 d . . . . .
H115 H 0.948213 0.156204 0.579785 0.056 Uiso 1 1 calc R . . . .
C337 C 0.7964(4) 0.6982(4) 0.5335(3) 0.0387(12) Uani 1 1 d . . . . .
H33A H 0.854638 0.731195 0.544597 0.058 Uiso 1 1 calc GR . . . .
H33B H 0.825562 0.653074 0.508923 0.058 Uiso 1 1 calc GR . . . .
H33C H 0.761019 0.664686 0.571530 0.058 Uiso 1 1 calc GR . . . .
C232 C 0.6430(4) 0.1399(4) 0.7236(3) 0.0410(13) Uani 1 1 d . . . . .
H232 H 0.683418 0.110242 0.694775 0.049 Uiso 1 1 calc R . . . .
C221 C 0.3380(4) 0.4050(4) 0.7501(2) 0.0354(11) Uani 1 1 d . . . . .
C335 C 0.5747(5) 0.9071(4) 0.4223(3) 0.0469(14) Uani 1 1 d . . . . .
H335 H 0.527199 0.952879 0.397670 0.056 Uiso 1 1 calc R . . . .
C333 C 0.7471(5) 0.8210(4) 0.4356(3) 0.0438(13) Uani 1 1 d . . . . .
H333 H 0.817371 0.808392 0.419993 0.053 Uiso 1 1 calc R . . . .
B3 B 0.5669(4) 0.7301(4) 0.5864(3) 0.0295(12) Uani 1 1 d . . . . .
C113 C 0.9165(4) 0.1730(4) 0.7247(3) 0.0409(13) Uani 1 1 d . . . . .
H113 H 0.926917 0.137215 0.765777 0.049 Uiso 1 1 calc R . . . .
C222 C 0.2424(4) 0.3617(4) 0.7416(2) 0.0398(12) Uani 1 1 d . . . . .
C121 C 0.9798(4) 0.5345(3) 0.6484(2) 0.0360(12) Uani 1 1 d . . . . .
C341 C 0.5929(4) 0.8405(4) 0.6648(3) 0.0379(12) Uani 1 1 d . . . . .
C345 C 0.4282(4) 0.7577(4) 0.6774(3) 0.0413(13) Uani 1 1 d . . . . .
C231 C 0.5149(4) 0.2252(4) 0.8094(2) 0.0442(13) Uani 1 1 d . . . . .
C344 C 0.3979(5) 0.7991(4) 0.7289(3) 0.0511(15) Uani 1 1 d . . . . .
H344 H 0.331463 0.786170 0.750113 0.061 Uiso 1 1 calc R . . . .
C124 C 0.8631(5) 0.6427(4) 0.7240(3) 0.0453(14) Uani 1 1 d . . . . .
H124 H 0.823780 0.678627 0.749786 0.054 Uiso 1 1 calc R . . . .
C346 C 0.7002(5) 0.8680(4) 0.6321(3) 0.0514(15) Uani 1 1 d . . . . .
H34A H 0.751063 0.812249 0.637232 0.077 Uiso 1 1 calc GR . . . .
H34B H 0.728588 0.915464 0.650595 0.077 Uiso 1 1 calc GR . . . .
H34C H 0.689148 0.893689 0.587758 0.077 Uiso 1 1 calc GR . . . .
C226 C 0.3289(4) 0.4752(4) 0.7867(2) 0.0413(13) Uani 1 1 d . . . . .
C348 C 0.3494(4) 0.6962(5) 0.6576(3) 0.0524(15) Uani 1 1 d . . . . .
H34D H 0.330812 0.722056 0.614170 0.079 Uiso 1 1 calc GR . . . .
H34E H 0.284567 0.695147 0.684211 0.079 Uiso 1 1 calc GR . . . .
H34F H 0.382654 0.632016 0.661616 0.079 Uiso 1 1 calc GR . . . .
C227 C 0.2471(5) 0.2867(4) 0.7016(3) 0.0521(15) Uani 1 1 d . . . . .
H22A H 0.265419 0.315690 0.658332 0.078 Uiso 1 1 calc GR . . . .
H22B H 0.177348 0.260895 0.703725 0.078 Uiso 1 1 calc GR . . . .
H22C H 0.301630 0.236007 0.717490 0.078 Uiso 1 1 calc GR . . . .
B1 B 0.8157(4) 0.4326(4) 0.6439(2) 0.0254(11) Uani 1 1 d . . . . .
C117 C 0.8372(4) 0.3064(4) 0.7737(2) 0.0406(12) Uani 1 1 d . . . . .
H11A H 0.860048 0.370007 0.769090 0.061 Uiso 1 1 calc GR . . . .
H11B H 0.868007 0.265486 0.811041 0.061 Uiso 1 1 calc GR . . . .
H11C H 0.759035 0.308490 0.777486 0.061 Uiso 1 1 calc GR . . . .
C339 C 0.4223(4) 0.8786(4) 0.5042(3) 0.0497(15) Uani 1 1 d . . . . .
H33D H 0.384540 0.821372 0.510124 0.075 Uiso 1 1 calc GR . . . .
H33E H 0.385898 0.928573 0.473250 0.075 Uiso 1 1 calc GR . . . .
H33F H 0.422714 0.898575 0.543782 0.075 Uiso 1 1 calc GR . . . .
B2 B 0.4506(5) 0.3724(4) 0.7201(2) 0.0311(12) Uani 1 1 d . . . . .
C119 C 0.8871(5) 0.3354(4) 0.5352(3) 0.0527(16) Uani 1 1 d . . . . .
H11D H 0.853318 0.398722 0.533873 0.079 Uiso 1 1 calc GR . . . .
H11E H 0.845150 0.302755 0.511580 0.079 Uiso 1 1 calc GR . . . .
H11F H 0.959703 0.339707 0.516893 0.079 Uiso 1 1 calc GR . . . .
C223 C 0.1448(4) 0.3869(4) 0.7701(3) 0.0453(14) Uani 1 1 d . . . . .
H223 H 0.082896 0.358012 0.763538 0.054 Uiso 1 1 calc R . . . .
C234 C 0.7221(5) 0.0087(4) 0.8122(3) 0.0583(17) Uani 1 1 d . . . . .
H23D H 0.753943 -0.015531 0.776819 0.087 Uiso 1 1 calc GR . . . .
H23E H 0.680624 -0.039204 0.838843 0.087 Uiso 1 1 calc GR . . . .
H23F H 0.778870 0.024236 0.836159 0.087 Uiso 1 1 calc GR . . . .
C10 C 0.6473(4) 0.0984(4) 0.7880(3) 0.0445(14) Uani 1 1 d . . . . .
C3AA C 0.5821(5) 0.1404(4) 0.8292(3) 0.0481(14) Uani 1 1 d . . . . .
H3AA H 0.582485 0.111435 0.872223 0.058 Uiso 1 1 calc R . . . .
C224 C 0.1356(4) 0.4532(5) 0.8077(3) 0.0496(15) Uani 1 1 d . . . . .
C114 C 0.9427(4) 0.1292(4) 0.6741(3) 0.0471(14) Uani 1 1 d . . . . .
C126 C 1.0491(4) 0.4778(4) 0.6065(3) 0.0494(14) Uani 1 1 d . . . . .
H12A H 1.060728 0.412020 0.628635 0.074 Uiso 1 1 calc GR . . . .
H12B H 1.118225 0.504686 0.596442 0.074 Uiso 1 1 calc GR . . . .
H12C H 1.011954 0.481009 0.567943 0.074 Uiso 1 1 calc GR . . . .
C123 C 0.9684(5) 0.6645(4) 0.7043(3) 0.0516(15) Uani 1 1 d . . . . .
C334 C 0.6774(5) 0.8901(4) 0.3989(3) 0.0470(14) Uani 1 1 d . . . . .
C122 C 1.0249(5) 0.6096(4) 0.6673(3) 0.0513(15) Uani 1 1 d . . . . .
H122 H 1.096196 0.622615 0.654203 0.062 Uiso 1 1 calc R . . . .
C229 C 0.4274(5) 0.5227(5) 0.7979(3) 0.0542(15) Uani 1 1 d . . . . .
H22D H 0.442120 0.507033 0.842388 0.081 Uiso 1 1 calc GR . . . .
H22E H 0.414223 0.591041 0.783989 0.081 Uiso 1 1 calc GR . . . .
H22F H 0.489128 0.500628 0.774545 0.081 Uiso 1 1 calc GR . . . .
C343 C 0.4632(5) 0.8586(5) 0.7495(3) 0.0558(16) Uani 1 1 d . . . . .
C225 C 0.2296(5) 0.4971(4) 0.8148(3) 0.0508(15) Uani 1 1 d . . . . .
H225 H 0.225088 0.542952 0.839505 0.061 Uiso 1 1 calc R . . . .
C128 C 0.7005(4) 0.5516(4) 0.7329(3) 0.0422(13) Uani 1 1 d . . . . .
H12D H 0.648581 0.584190 0.702041 0.063 Uiso 1 1 calc GR . . . .
H12E H 0.688314 0.575278 0.771061 0.063 Uiso 1 1 calc GR . . . .
H12F H 0.691905 0.483951 0.742093 0.063 Uiso 1 1 calc GR . . . .
C342 C 0.5595(5) 0.8802(4) 0.7158(3) 0.0512(15) Uani 1 1 d . . . . .
H342 H 0.602870 0.922596 0.727839 0.061 Uiso 1 1 calc R . . . .
C118 C 0.9811(6) 0.0237(4) 0.6866(4) 0.072(2) Uani 1 1 d . . . . .
H11G H 0.927858 -0.011018 0.672138 0.107 Uiso 1 1 calc GR . . . .
H11H H 0.990304 -0.000260 0.731329 0.107 Uiso 1 1 calc GR . . . .
H11I H 1.049441 0.015335 0.664300 0.107 Uiso 1 1 calc GR . . . .
C347 C 0.4293(7) 0.9007(6) 0.8066(3) 0.083(2) Uani 1 1 d . . . . .
H34G H 0.351077 0.907781 0.810302 0.125 Uiso 1 1 calc GR . . . .
H34H H 0.457614 0.962308 0.801382 0.125 Uiso 1 1 calc GR . . . .
H34I H 0.457601 0.858628 0.844261 0.125 Uiso 1 1 calc GR . . . .
C338 C 0.7155(7) 0.9445(5) 0.3356(3) 0.077(2) Uani 1 1 d . . . . .
H33G H 0.670197 0.933939 0.303274 0.116 Uiso 1 1 calc GR . . . .
H33H H 0.789739 0.922856 0.327268 0.116 Uiso 1 1 calc GR . . . .
H33I H 0.711031 1.011794 0.335395 0.116 Uiso 1 1 calc GR . . . .
C233 C 0.4453(6) 0.2613(5) 0.8589(3) 0.075(2) Uani 1 1 d . . . . .
H23G H 0.463499 0.324583 0.860097 0.112 Uiso 1 1 calc GR . . . .
H23H H 0.457656 0.219147 0.899494 0.112 Uiso 1 1 calc GR . . . .
H23I H 0.369863 0.263435 0.848848 0.112 Uiso 1 1 calc GR . . . .
C228 C 0.0292(5) 0.4775(5) 0.8405(3) 0.0656(19) Uani 1 1 d . . . . .
H22G H -0.029940 0.478600 0.812901 0.098 Uiso 1 1 calc GR . . . .
H22H H 0.030340 0.539349 0.850502 0.098 Uiso 1 1 calc GR . . . .
H22I H 0.019299 0.429945 0.878878 0.098 Uiso 1 1 calc GR . . . .
C127 C 1.0232(6) 0.7428(5) 0.7252(4) 0.080(2) Uani 1 1 d . . . . .
H12G H 0.968805 0.784611 0.740996 0.120 Uiso 1 1 calc GR . . . .
H12H H 1.062294 0.779047 0.689626 0.120 Uiso 1 1 calc GR . . . .
H12I H 1.073174 0.714192 0.758054 0.120 Uiso 1 1 calc GR . . . .
C4S C 0.0095(9) 0.0029(9) 0.8963(5) 0.126(4) Uiso 1 1 d . . . . .
H4S H -0.028313 -0.052091 0.906178 0.151 Uiso 1 1 calc R . . . .
C5S C -0.0275(9) 0.0696(9) 0.9198(5) 0.124(4) Uiso 1 1 d . . . . .
C6S C 0.0293(12) 0.1559(10) 0.9072(6) 0.134(4) Uiso 1 1 d . . . . .
C3S C 0.1132(12) -0.0005(11) 0.8516(6) 0.160(5) Uiso 1 1 d . . . . .
H3S H 0.138370 -0.050330 0.832033 0.192 Uiso 1 1 calc R . . . .
C2S C 0.1590(11) 0.0833(10) 0.8470(6) 0.146(4) Uiso 1 1 d . . . . .
H2S H 0.224322 0.092875 0.823837 0.175 Uiso 1 1 calc R . . . .
C1S C 0.1148(13) 0.1513(11) 0.8739(7) 0.162(5) Uiso 1 1 d . . . . .
H1S H 0.153643 0.205669 0.866968 0.194 Uiso 1 1 calc R . . . .
C10S C 0.0679(6) 1.0558(5) 0.4816(3) 0.0640(18) Uiso 1 1 d . . . . .
C7S C 0.1206(7) 0.8979(6) 0.5528(4) 0.0268(19) Uiso 0.5 1 d . . P . .
C9S C 0.0477(11) 0.9727(10) 0.5161(6) 0.060(3) Uiso 0.5 1 d . . P . .
C8S C 0.1431(13) 0.9798(12) 0.5210(7) 0.077(4) Uiso 0.5 1 d . . P . .
C11S C -0.0120(14) 1.1230(12) 0.4466(8) 0.086(5) Uiso 0.5 1 d . . P . .
H5S H -0.111(3) 0.108(3) 0.9524(19) 0.021(11) Uiso 1 1 d . . . . .
H6S H -0.025(3) 0.179(3) 0.9397(18) 0.007(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 U1 3.8998(3) 2_666 ?
U1 S1B 2.9192(12) 2_666 ?
U1 S1B 2.7175(12) . ?
U1 S2B 2.8598(12) . ?
U1 S2B 2.7408(12) 2_666 ?
U1 O3 2.081(3) . ?
U1 O1 2.075(3) . ?
U1 O2 2.076(3) . ?
S1B S2B 2.0492(18) . ?
O3 B3 1.354(6) . ?
O1 B1 1.366(6) . ?
O2 B2 1.356(6) . ?
C111 C112 1.406(6) . ?
C111 C116 1.421(7) . ?
C111 B1 1.580(7) . ?
C331 C332 1.409(6) . ?
C331 C336 1.421(6) . ?
C331 B3 1.582(7) . ?
C1AA C235 1.498(6) . ?
C1AA C230 1.410(7) . ?
C1AA C232 1.402(7) . ?
C332 C337 1.513(7) . ?
C332 C333 1.388(7) . ?
C112 C113 1.385(7) . ?
C112 C117 1.500(7) . ?
C235 H23A 0.9600 . ?
C235 H23B 0.9600 . ?
C235 H23C 0.9600 . ?
C340 B3 1.583(7) . ?
C340 C341 1.401(7) . ?
C340 C345 1.423(7) . ?
C230 C231 1.424(7) . ?
C230 B2 1.585(7) . ?
C120 C125 1.415(7) . ?
C120 C121 1.397(7) . ?
C120 B1 1.601(7) . ?
C336 C335 1.386(8) . ?
C336 C339 1.506(8) . ?
C116 C115 1.391(7) . ?
C116 C119 1.497(7) . ?
C125 C124 1.381(7) . ?
C125 C128 1.508(7) . ?
C115 H115 0.9300 . ?
C115 C114 1.366(8) . ?
C337 H33A 0.9600 . ?
C337 H33B 0.9600 . ?
C337 H33C 0.9600 . ?
C232 H232 0.9300 . ?
C232 C10 1.387(7) . ?
C221 C222 1.416(7) . ?
C221 C226 1.405(7) . ?
C221 B2 1.578(7) . ?
C335 H335 0.9300 . ?
C335 C334 1.360(8) . ?
C333 H333 0.9300 . ?
C333 C334 1.383(8) . ?
C113 H113 0.9300 . ?
C113 C114 1.389(8) . ?
C222 C227 1.518(8) . ?
C222 C223 1.377(7) . ?
C121 C126 1.529(7) . ?
C121 C122 1.398(8) . ?
C341 C346 1.508(8) . ?
C341 C342 1.377(7) . ?
C345 C344 1.394(7) . ?
C345 C348 1.504(7) . ?
C231 C3AA 1.404(7) . ?
C231 C233 1.490(8) . ?
C344 H344 0.9300 . ?
C344 C343 1.377(9) . ?
C124 H124 0.9300 . ?
C124 C123 1.385(8) . ?
C346 H34A 0.9600 . ?
C346 H34B 0.9600 . ?
C346 H34C 0.9600 . ?
C226 C229 1.497(8) . ?
C226 C225 1.381(7) . ?
C348 H34D 0.9600 . ?
C348 H34E 0.9600 . ?
C348 H34F 0.9600 . ?
C227 H22A 0.9600 . ?
C227 H22B 0.9600 . ?
C227 H22C 0.9600 . ?
C117 H11A 0.9600 . ?
C117 H11B 0.9600 . ?
C117 H11C 0.9600 . ?
C339 H33D 0.9600 . ?
C339 H33E 0.9600 . ?
C339 H33F 0.9600 . ?
C119 H11D 0.9600 . ?
C119 H11E 0.9600 . ?
C119 H11F 0.9600 . ?
C223 H223 0.9300 . ?
C223 C224 1.376(8) . ?
C234 H23D 0.9600 . ?
C234 H23E 0.9600 . ?
C234 H23F 0.9600 . ?
C234 C10 1.522(7) . ?
C10 C3AA 1.371(8) . ?
C3AA H3AA 0.9300 . ?
C224 C225 1.396(8) . ?
C224 C228 1.508(8) . ?
C114 C118 1.512(8) . ?
C126 H12A 0.9600 . ?
C126 H12B 0.9600 . ?
C126 H12C 0.9600 . ?
C123 C122 1.367(8) . ?
C123 C127 1.518(8) . ?
C334 C338 1.493(8) . ?
C122 H122 0.9300 . ?
C229 H22D 0.9600 . ?
C229 H22E 0.9600 . ?
C229 H22F 0.9600 . ?
C343 C342 1.382(9) . ?
C343 C347 1.514(8) . ?
C225 H225 0.9300 . ?
C128 H12D 0.9600 . ?
C128 H12E 0.9600 . ?
C128 H12F 0.9600 . ?
C342 H342 0.9300 . ?
C118 H11G 0.9600 . ?
C118 H11H 0.9600 . ?
C118 H11I 0.9600 . ?
C347 H34G 0.9600 . ?
C347 H34H 0.9600 . ?
C347 H34I 0.9600 . ?
C338 H33G 0.9600 . ?
C338 H33H 0.9600 . ?
C338 H33I 0.9600 . ?
C233 H23G 0.9600 . ?
C233 H23H 0.9600 . ?
C233 H23I 0.9600 . ?
C228 H22G 0.9600 . ?
C228 H22H 0.9600 . ?
C228 H22I 0.9600 . ?
C127 H12G 0.9600 . ?
C127 H12H 0.9600 . ?
C127 H12I 0.9600 . ?
C4S H4S 0.9300 . ?
C4S C5S 1.221(14) . ?
C4S C3S 1.567(16) . ?
C5S C6S 1.442(15) . ?
C5S H5S 1.36(4) . ?
C6S C1S 1.251(16) . ?
C6S H6S 1.03(4) . ?
C3S H3S 0.9300 . ?
C3S C2S 1.354(16) . ?
C2S H2S 0.9300 . ?
C2S C1S 1.307(16) . ?
C1S H1S 0.9300 . ?
C10S C9S 1.510(15) 2_576 ?
C10S C9S 1.296(14) . ?
C10S C8S 1.503(17) . ?
C10S C11S 1.431(17) . ?
C7S C9S 1.451(15) . ?
C7S C8S 1.268(18) . ?
C7S C11S 1.394(18) 2_576 ?
C9S C9S 1.47(3) 2_576 ?
C9S C8S 1.199(19) . ?
C9S C11S 1.52(2) 2_576 ?

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
S1B U1 U1 48.40(3) . 2_666 ?
S1B U1 U1 44.12(2) 2_666 2_666 ?
S1B U1 S1B 92.52(3) . 2_666 ?
S1B U1 S2B 79.53(4) . 2_666 ?
S1B U1 S2B 43.02(4) . . ?
S2B U1 U1 47.14(3) 2_666 2_666 ?
S2B U1 U1 44.63(2) . 2_666 ?
S2B U1 S1B 74.33(3) . 2_666 ?
S2B U1 S1B 42.31(4) 2_666 2_666 ?
S2B U1 S2B 91.76(3) 2_666 . ?
O3 U1 U1 107.53(8) . 2_666 ?
O3 U1 S1B 83.03(9) . . ?
O3 U1 S1B 121.02(8) . 2_666 ?
O3 U1 S2B 125.90(9) . . ?
O3 U1 S2B 79.44(8) . 2_666 ?
O1 U1 U1 130.58(8) . 2_666 ?
O1 U1 S1B 91.62(9) . . ?
O1 U1 S1B 147.42(9) . 2_666 ?
O1 U1 S2B 87.11(9) . . ?
O1 U1 S2B 168.02(9) . 2_666 ?
O1 U1 O3 91.57(12) . . ?
O1 U1 O2 93.66(12) . . ?
O2 U1 U1 126.61(9) . 2_666 ?
O2 U1 S1B 174.64(9) . . ?
O2 U1 S1B 82.52(9) . 2_666 ?
O2 U1 S2B 95.38(9) . 2_666 ?
O2 U1 S2B 136.33(9) . . ?
O2 U1 O3 97.75(12) . . ?
U1 S1B U1 87.48(3) . 2_666 ?
S2B S1B U1 64.19(5) . 2_666 ?
S2B S1B U1 72.19(5) . . ?
U1 S2B U1 88.24(3) 2_666 . ?
S1B S2B U1 73.50(5) . 2_666 ?
S1B S2B U1 64.79(5) . . ?
B3 O3 U1 166.6(3) . . ?
B1 O1 U1 168.4(3) . . ?
B2 O2 U1 161.6(3) . . ?
C112 C111 C116 118.1(4) . . ?
C112 C111 B1 120.7(4) . . ?
C116 C111 B1 121.1(4) . . ?
C332 C331 C336 117.4(5) . . ?
C332 C331 B3 122.2(4) . . ?
C336 C331 B3 120.3(4) . . ?
C230 C1AA C235 124.2(4) . . ?
C232 C1AA C235 115.2(5) . . ?
C232 C1AA C230 120.6(5) . . ?
C331 C332 C337 120.8(4) . . ?
C333 C332 C331 120.3(4) . . ?
C333 C332 C337 118.8(4) . . ?
C111 C112 C117 121.1(4) . . ?
C113 C112 C111 119.6(5) . . ?
C113 C112 C117 119.1(4) . . ?
C1AA C235 H23A 109.5 . . ?
C1AA C235 H23B 109.5 . . ?
C1AA C235 H23C 109.5 . . ?
H23A C235 H23B 109.5 . . ?
H23A C235 H23C 109.5 . . ?
H23B C235 H23C 109.5 . . ?
C341 C340 B3 121.9(4) . . ?
C341 C340 C345 117.4(5) . . ?
C345 C340 B3 120.7(4) . . ?
C1AA C230 C231 117.9(4) . . ?
C1AA C230 B2 121.3(4) . . ?
C231 C230 B2 120.8(5) . . ?
C125 C120 B1 120.6(4) . . ?
C121 C120 C125 118.2(5) . . ?
C121 C120 B1 121.2(4) . . ?
C331 C336 C339 119.9(5) . . ?
C335 C336 C331 119.7(5) . . ?
C335 C336 C339 120.4(5) . . ?
C111 C116 C119 122.4(4) . . ?
C115 C116 C111 119.4(5) . . ?
C115 C116 C119 118.1(5) . . ?
C120 C125 C128 123.3(4) . . ?
C124 C125 C120 119.8(5) . . ?
C124 C125 C128 116.9(5) . . ?
C116 C115 H115 118.7 . . ?
C114 C115 C116 122.7(5) . . ?
C114 C115 H115 118.7 . . ?
C332 C337 H33A 109.5 . . ?
C332 C337 H33B 109.5 . . ?
C332 C337 H33C 109.5 . . ?
H33A C337 H33B 109.5 . . ?
H33A C337 H33C 109.5 . . ?
H33B C337 H33C 109.5 . . ?
C1AA C232 H232 119.4 . . ?
C10 C232 C1AA 121.3(5) . . ?
C10 C232 H232 119.4 . . ?
C222 C221 B2 120.0(5) . . ?
C226 C221 C222 118.0(5) . . ?
C226 C221 B2 122.1(5) . . ?
C336 C335 H335 118.7 . . ?
C334 C335 C336 122.7(5) . . ?
C334 C335 H335 118.7 . . ?
C332 C333 H333 119.2 . . ?
C334 C333 C332 121.7(5) . . ?
C334 C333 H333 119.2 . . ?
O3 B3 C331 117.3(4) . . ?
O3 B3 C340 118.9(4) . . ?
C331 B3 C340 123.8(4) . . ?
C112 C113 H113 118.7 . . ?
C112 C113 C114 122.6(5) . . ?
C114 C113 H113 118.7 . . ?
C221 C222 C227 120.2(5) . . ?
C223 C222 C221 120.2(5) . . ?
C223 C222 C227 119.7(5) . . ?
C120 C121 C126 121.7(5) . . ?
C120 C121 C122 119.5(5) . . ?
C122 C121 C126 118.7(5) . . ?
C340 C341 C346 121.6(5) . . ?
C342 C341 C340 121.1(5) . . ?
C342 C341 C346 117.3(5) . . ?
C340 C345 C348 122.5(5) . . ?
C344 C345 C340 119.5(5) . . ?
C344 C345 C348 117.9(5) . . ?
C230 C231 C233 123.7(5) . . ?
C3AA C231 C230 119.0(5) . . ?
C3AA C231 C233 117.4(5) . . ?
C345 C344 H344 118.9 . . ?
C343 C344 C345 122.2(6) . . ?
C343 C344 H344 118.9 . . ?
C125 C124 H124 118.9 . . ?
C125 C124 C123 122.3(5) . . ?
C123 C124 H124 118.9 . . ?
C341 C346 H34A 109.5 . . ?
C341 C346 H34B 109.5 . . ?
C341 C346 H34C 109.5 . . ?
H34A C346 H34B 109.5 . . ?
H34A C346 H34C 109.5 . . ?
H34B C346 H34C 109.5 . . ?
C221 C226 C229 120.4(5) . . ?
C225 C226 C221 119.6(5) . . ?
C225 C226 C229 119.9(5) . . ?
C345 C348 H34D 109.5 . . ?
C345 C348 H34E 109.5 . . ?
C345 C348 H34F 109.5 . . ?
H34D C348 H34E 109.5 . . ?
H34D C348 H34F 109.5 . . ?
H34E C348 H34F 109.5 . . ?
C222 C227 H22A 109.5 . . ?
C222 C227 H22B 109.5 . . ?
C222 C227 H22C 109.5 . . ?
H22A C227 H22B 109.5 . . ?
H22A C227 H22C 109.5 . . ?
H22B C227 H22C 109.5 . . ?
O1 B1 C111 119.4(4) . . ?
O1 B1 C120 116.7(4) . . ?
C111 B1 C120 123.8(4) . . ?
C112 C117 H11A 109.5 . . ?
C112 C117 H11B 109.5 . . ?
C112 C117 H11C 109.5 . . ?
H11A C117 H11B 109.5 . . ?
H11A C117 H11C 109.5 . . ?
H11B C117 H11C 109.5 . . ?
C336 C339 H33D 109.5 . . ?
C336 C339 H33E 109.5 . . ?
C336 C339 H33F 109.5 . . ?
H33D C339 H33E 109.5 . . ?
H33D C339 H33F 109.5 . . ?
H33E C339 H33F 109.5 . . ?
O2 B2 C230 118.3(4) . . ?
O2 B2 C221 117.3(4) . . ?
C221 B2 C230 124.4(4) . . ?
C116 C119 H11D 109.5 . . ?
C116 C119 H11E 109.5 . . ?
C116 C119 H11F 109.5 . . ?
H11D C119 H11E 109.5 . . ?
H11D C119 H11F 109.5 . . ?
H11E C119 H11F 109.5 . . ?
C222 C223 H223 118.8 . . ?
C224 C223 C222 122.4(5) . . ?
C224 C223 H223 118.8 . . ?
H23D C234 H23E 109.5 . . ?
H23D C234 H23F 109.5 . . ?
H23E C234 H23F 109.5 . . ?
C10 C234 H23D 109.5 . . ?
C10 C234 H23E 109.5 . . ?
C10 C234 H23F 109.5 . . ?
C232 C10 C234 121.0(5) . . ?
C3AA C10 C232 118.2(5) . . ?
C3AA C10 C234 120.8(5) . . ?
C231 C3AA H3AA 118.6 . . ?
C10 C3AA C231 122.8(5) . . ?
C10 C3AA H3AA 118.6 . . ?
C223 C224 C225 117.1(5) . . ?
C223 C224 C228 121.9(6) . . ?
C225 C224 C228 121.0(6) . . ?
C115 C114 C113 117.5(5) . . ?
C115 C114 C118 122.6(6) . . ?
C113 C114 C118 119.8(6) . . ?
C121 C126 H12A 109.5 . . ?
C121 C126 H12B 109.5 . . ?
C121 C126 H12C 109.5 . . ?
H12A C126 H12B 109.5 . . ?
H12A C126 H12C 109.5 . . ?
H12B C126 H12C 109.5 . . ?
C124 C123 C127 122.2(6) . . ?
C122 C123 C124 117.6(5) . . ?
C122 C123 C127 120.1(6) . . ?
C335 C334 C333 118.3(5) . . ?
C335 C334 C338 121.5(6) . . ?
C333 C334 C338 120.2(6) . . ?
C121 C122 H122 118.7 . . ?
C123 C122 C121 122.6(5) . . ?
C123 C122 H122 118.7 . . ?
C226 C229 H22D 109.5 . . ?
C226 C229 H22E 109.5 . . ?
C226 C229 H22F 109.5 . . ?
H22D C229 H22E 109.5 . . ?
H22D C229 H22F 109.5 . . ?
H22E C229 H22F 109.5 . . ?
C344 C343 C342 118.0(5) . . ?
C344 C343 C347 120.9(6) . . ?
C342 C343 C347 121.1(6) . . ?
C226 C225 C224 122.6(6) . . ?
C226 C225 H225 118.7 . . ?
C224 C225 H225 118.7 . . ?
C125 C128 H12D 109.5 . . ?
C125 C128 H12E 109.5 . . ?
C125 C128 H12F 109.5 . . ?
H12D C128 H12E 109.5 . . ?
H12D C128 H12F 109.5 . . ?
H12E C128 H12F 109.5 . . ?
C341 C342 C343 121.8(6) . . ?
C341 C342 H342 119.1 . . ?
C343 C342 H342 119.1 . . ?
C114 C118 H11G 109.5 . . ?
C114 C118 H11H 109.5 . . ?
C114 C118 H11I 109.5 . . ?
H11G C118 H11H 109.5 . . ?
H11G C118 H11I 109.5 . . ?
H11H C118 H11I 109.5 . . ?
C343 C347 H34G 109.5 . . ?
C343 C347 H34H 109.5 . . ?
C343 C347 H34I 109.5 . . ?
H34G C347 H34H 109.5 . . ?
H34G C347 H34I 109.5 . . ?
H34H C347 H34I 109.5 . . ?
C334 C338 H33G 109.5 . . ?
C334 C338 H33H 109.5 . . ?
C334 C338 H33I 109.5 . . ?
H33G C338 H33H 109.5 . . ?
H33G C338 H33I 109.5 . . ?
H33H C338 H33I 109.5 . . ?
C231 C233 H23G 109.5 . . ?
C231 C233 H23H 109.5 . . ?
C231 C233 H23I 109.5 . . ?
H23G C233 H23H 109.5 . . ?
H23G C233 H23I 109.5 . . ?
H23H C233 H23I 109.5 . . ?
C224 C228 H22G 109.5 . . ?
C224 C228 H22H 109.5 . . ?
C224 C228 H22I 109.5 . . ?
H22G C228 H22H 109.5 . . ?
H22G C228 H22I 109.5 . . ?
H22H C228 H22I 109.5 . . ?
C123 C127 H12G 109.5 . . ?
C123 C127 H12H 109.5 . . ?
C123 C127 H12I 109.5 . . ?
H12G C127 H12H 109.5 . . ?
H12G C127 H12I 109.5 . . ?
H12H C127 H12I 109.5 . . ?
C5S C4S H4S 116.3 . . ?
C5S C4S C3S 127.5(13) . . ?
C3S C4S H4S 116.3 . . ?
C4S C5S C6S 118.6(13) . . ?
C4S C5S H5S 148(2) . . ?
C6S C5S H5S 93(2) . . ?
C5S C6S H6S 87(2) . . ?
C1S C6S C5S 113.8(14) . . ?
C1S C6S H6S 158(3) . . ?
C4S C3S H3S 126.8 . . ?
C2S C3S C4S 106.4(13) . . ?
C2S C3S H3S 126.8 . . ?
C3S C2S H2S 118.7 . . ?
C1S C2S C3S 122.5(16) . . ?
C1S C2S H2S 118.7 . . ?
C6S C1S C2S 131.1(17) . . ?
C6S C1S H1S 114.5 . . ?
C2S C1S H1S 114.5 . . ?
C9S C10S C9S 62.6(10) . 2_576 ?
C9S C10S C8S 50.1(8) . . ?
C9S C10S C11S 124.6(11) . . ?
C8S C10S C9S 112.6(10) . 2_576 ?
C11S C10S C9S 62.1(9) . 2_576 ?
C11S C10S C8S 174.6(11) . . ?
C8S C7S C9S 51.8(9) . . ?
C8S C7S C11S 116.3(12) . 2_576 ?
C11S C7S C9S 64.5(9) 2_576 . ?
C10S C9S C10S 117.5(10) . 2_576 ?
C10S C9S C7S 130.2(12) . . ?
C10S C9S C9S 65.9(10) . 2_576 ?
C10S C9S C11S 56.4(8) 2_576 2_576 ?
C10S C9S C11S 173.8(13) . 2_576 ?
C7S C9S C10S 112.4(11) . 2_576 ?
C7S C9S C9S 163.9(17) . 2_576 ?
C7S C9S C11S 56.0(9) . 2_576 ?
C9S C9S C10S 51.6(9) 2_576 2_576 ?
C9S C9S C11S 108.0(15) 2_576 2_576 ?
C8S C9S C10S 168.6(15) . 2_576 ?
C8S C9S C10S 74.0(12) . . ?
C8S C9S C7S 56.2(10) . . ?
C8S C9S C9S 139.8(19) . 2_576 ?
C8S C9S C11S 112.2(14) . 2_576 ?
C7S C8S C10S 127.9(13) . . ?
C9S C8S C10S 56.0(10) . . ?
C9S C8S C7S 72.0(12) . . ?
C10S C11S C9S 61.5(9) . 2_576 ?
C7S C11S C10S 121.1(13) 2_576 . ?
C7S C11S C9S 59.6(9) 2_576 2_576 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.521 -0.460 0.000 1026.2 25.3 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.626

# start Validation Reply Form
_vrf_PLAT245_p18033              
;
PROBLEM: U(iso) H5S       Smaller than U(eq) C5S       by      0.103 Ang**2
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT351_p18033              
;
PROBLEM: Long   C-H (X0.96,N1.08A)  C5S      - H5S      .       1.36 Ang.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT410_p18033              
;
PROBLEM: Short Intra H...H Contact  H5S      ..H6S      .       1.51 Ang.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT770_p18033              
;
PROBLEM: Suspect C-H Bond in CIF:  C5S      --H5S       .       1.36 Ang.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT232_p18033              
;
PROBLEM: Hirshfeld Test Diff (M-X)  U1       --S2B      .       10.7 s.u.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT332_p18033              
;
PROBLEM: Large Phenyl C-C Range     C1S       -C6S      .       0.34 Ang.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
_vrf_PLAT369_p18033              
;
PROBLEM: Long   C(sp2)-C(sp2) Bond  C3S      - C4S      .       1.57 Ang.  
RESPONSE: This alert was generated because there is a large
amount of disorder in particular the disordered lattice solvent is very
dynamic. Short contacts between disordered fragments are to be expected.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p18053_tri
_database_code_depnum_ccdc_archive 'CCDC 1886810'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C36 H76 B N3 O Si6 U)'
_chemical_formula_sum            'C72 H152 B2 N6 O2 Si12 U2'
_chemical_formula_weight         1968.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U1 C100 H100 B3 O3'
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'
B B 0.0013 0.0007 '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'
Si Si 0.0817 0.0704 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0703(2)
_cell_length_b                   13.1641(2)
_cell_length_c                   15.6746(3)
_cell_angle_alpha                102.222(2)
_cell_angle_beta                 98.2700(10)
_cell_angle_gamma                90.1220(10)
_cell_volume                     2407.48(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    20349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0100
_cell_measurement_theta_min      3.4180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1004
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 1 14 0.1327
-11 -1 -14 0.1327
3 17 -13 0.3672
-3 -17 13 0.3672
-6 8 17 0.0418
6 -8 -17 0.0418

_exptl_crystal_size_max          0.792
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.084
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.9942 0.9814 13.9820 0.1594 0.9393 -0.3069
-10.9942 -0.9814 -13.9820 -0.1594 -0.9393 0.3069
2.9899 16.9925 -12.9826 -0.0624 -0.4228 -0.9122
-2.9899 -16.9925 12.9826 0.0624 0.4228 0.9122
-5.9894 7.9732 16.9928 -0.8246 0.5353 -0.2051
5.9894 -7.9732 -16.9928 0.8246 -0.5353 0.2051

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51203
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.964
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  22.00   1.00   10.00    --  -18.68 -99.00  30.00   47
  2  ω    -93.00 -34.00   1.00   10.00    --  -18.68-179.00 -30.00   59
  3  ω    -25.00  22.00   1.00   10.00    --  -18.68 -99.00-120.00   47
  4  ω    -49.00  49.00   1.00   10.00    --   20.40 -77.00 150.00   98
  5  ω      2.00  89.00   1.00   10.00    --   20.40  57.00   0.00   87
  6  ω     34.00  95.00   1.00   10.00    --   20.40 179.00 -60.00   61
  7  ω    -18.00  93.00   1.00   10.00    --   20.40  19.00 -60.00  111
  8  ω    -87.00   0.00   1.00   10.00    --  -18.68 -57.00 150.00   87
  9  ω    -25.00  22.00   1.00   10.00    --  -18.68 -99.00 120.00   47
 10  ω    -25.00  61.00   1.00   10.00    --   20.40 -99.00-120.00   86
 11  ω    -25.00  61.00   1.00   10.00    --   20.40 -99.00   0.00   86
 12  ω      2.00  89.00   1.00   10.00    --   20.40  57.00  90.00   87
 13  ω    -48.00  39.00   1.00   10.00    --   20.40 -57.00 -60.00   87
 14  ω    -14.00  68.00   1.00   10.00    --   20.40-112.00 134.08   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0431569000
_diffrn_orient_matrix_UB_12      -0.0270313000
_diffrn_orient_matrix_UB_13      -0.0206338000
_diffrn_orient_matrix_UB_21      0.0318861000
_diffrn_orient_matrix_UB_22      0.0015946000
_diffrn_orient_matrix_UB_23      0.0419951000
_diffrn_orient_matrix_UB_31      -0.0255137000
_diffrn_orient_matrix_UB_32      -0.0480589000
_diffrn_orient_matrix_UB_33      0.0014872000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8900
_reflns_number_total             9835
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9835
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0240
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+0.9968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0552
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C124(H124), C4AA(H4AA), C2AA(H2AA), C115(H115)
2.b Idealised Me refined as rotating group:
 C123(H12A,H12B,H12C), C351(H35A,H35B,H35C), C113(H11A,H11B,H11C), C242(H24A,
 H24B,H24C), C122(H12D,H12E,H12F), C112(H11D,H11E,H11F), C243(H24D,H24E,H24F),
 C362(H36A,H36B,H36C), C352(H35D,H35E,H35F), C128(H12G,H12H,H12I), C121(H12J,
 H12K,H12L), C232(H23A,H23B,H23C), C126(H12M,H12N,H12O), C363(H36D,H36E,H36F),
 C111(H11G,H11H,H11I), C361(H36G,H36H,H36I), C353(H35G,H35H,H35I), C117(H11J,
 H11K,H11L), C241(H24G,H24H,H24I), C119(H11M,H11N,H11O), C231(H23D,H23E,H23F),
 C233(H23G,H23H,H23I), C127(H12P,H12Q,H12R), C118(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.31057(2) 0.64762(2) 0.75467(2) 0.01745(4) Uani 1 1 d . . . . .
Si5 Si 0.22940(7) 0.59380(6) 0.93618(5) 0.02359(18) Uani 1 1 d . . . . .
Si1 Si 0.55616(7) 0.78024(6) 0.89768(6) 0.02439(18) Uani 1 1 d . . . . .
Si6 Si 0.08241(7) 0.75177(7) 0.87406(6) 0.02698(19) Uani 1 1 d . . . . .
Si3 Si 0.40619(7) 0.37978(6) 0.71286(6) 0.02509(18) Uani 1 1 d . . . . .
Si4 Si 0.17898(7) 0.42602(6) 0.63308(6) 0.02617(19) Uani 1 1 d . . . . .
O1 O 0.25597(16) 0.75193(14) 0.66911(13) 0.0215(4) Uani 1 1 d . . . . .
N1 N 0.48647(19) 0.71791(17) 0.79414(15) 0.0197(5) Uani 1 1 d . . . . .
N3 N 0.19789(19) 0.67228(17) 0.85978(16) 0.0204(5) Uani 1 1 d . . . . .
N2 N 0.30429(19) 0.47198(17) 0.70058(16) 0.0208(5) Uani 1 1 d . . . . .
C123 C 0.4791(3) 0.6152(2) 0.6063(2) 0.0295(7) Uani 1 1 d . . . . .
H12A H 0.454559 0.555129 0.625063 0.044 Uiso 1 1 calc GR . . . .
H12B H 0.527273 0.594323 0.562514 0.044 Uiso 1 1 calc GR . . . .
H12C H 0.415178 0.648364 0.581683 0.044 Uiso 1 1 calc GR . . . .
C120 C 0.2656(2) 0.8362(2) 0.53528(19) 0.0201(6) Uani 1 1 d . . . . .
C351 C 0.3774(3) 0.5525(2) 0.9335(2) 0.0312(7) Uani 1 1 d . . . . .
H35A H 0.390487 0.532419 0.873288 0.047 Uiso 1 1 calc GR . . . .
H35B H 0.389941 0.494650 0.961604 0.047 Uiso 1 1 calc GR . . . .
H35C H 0.427791 0.609361 0.964087 0.047 Uiso 1 1 calc GR . . . .
C0AA C 0.1709(2) 0.9304(2) 0.67954(19) 0.0226(6) Uani 1 1 d . . . . .
C113 C 0.6542(3) 0.6922(3) 0.9488(2) 0.0342(8) Uani 1 1 d . . . . .
H11A H 0.612599 0.633249 0.956326 0.051 Uiso 1 1 calc GR . . . .
H11B H 0.690992 0.729316 1.005191 0.051 Uiso 1 1 calc GR . . . .
H11C H 0.709089 0.668836 0.910990 0.051 Uiso 1 1 calc GR . . . .
C242 C 0.0765(3) 0.5324(2) 0.6498(2) 0.0329(8) Uani 1 1 d . . . . .
H24A H 0.062287 0.546187 0.709810 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.007745 0.511347 0.610756 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.106996 0.594229 0.637411 0.049 Uiso 1 1 calc GR . . . .
C125 C 0.2390(2) 0.7525(2) 0.4622(2) 0.0230(6) Uani 1 1 d . . . . .
C3AA C 0.3148(2) 0.9273(2) 0.5186(2) 0.0236(6) Uani 1 1 d . . . . .
C122 C 0.5675(3) 0.8332(2) 0.6650(2) 0.0362(8) Uani 1 1 d . . . . .
H12D H 0.493831 0.859285 0.653745 0.054 Uiso 1 1 calc GR . . . .
H12E H 0.600633 0.820684 0.611796 0.054 Uiso 1 1 calc GR . . . .
H12F H 0.613024 0.883450 0.709722 0.054 Uiso 1 1 calc GR . . . .
C112 C 0.4552(3) 0.8277(3) 0.9765(2) 0.0341(8) Uani 1 1 d . . . . .
H11D H 0.437657 0.898329 0.974666 0.051 Uiso 1 1 calc GR . . . .
H11E H 0.488477 0.824170 1.035219 0.051 Uiso 1 1 calc GR . . . .
H11F H 0.387908 0.784817 0.960050 0.051 Uiso 1 1 calc GR . . . .
C124 C 0.2577(2) 0.7604(2) 0.3785(2) 0.0265(7) Uani 1 1 d . . . . .
H124 H 0.237185 0.704538 0.331361 0.032 Uiso 1 1 calc R . . . .
C243 C 0.1148(3) 0.3092(3) 0.6588(2) 0.0399(9) Uani 1 1 d . . . . .
H24D H 0.160836 0.250548 0.643928 0.060 Uiso 1 1 calc GR . . . .
H24E H 0.041473 0.294850 0.625024 0.060 Uiso 1 1 calc GR . . . .
H24F H 0.109131 0.322037 0.720563 0.060 Uiso 1 1 calc GR . . . .
C362 C 0.0116(3) 0.7786(3) 0.7684(2) 0.0361(8) Uani 1 1 d . . . . .
H36A H 0.066568 0.799152 0.736223 0.054 Uiso 1 1 calc GR . . . .
H36B H -0.039851 0.833476 0.780323 0.054 Uiso 1 1 calc GR . . . .
H36C H -0.028504 0.716918 0.734037 0.054 Uiso 1 1 calc GR . . . .
C352 C 0.1382(3) 0.4733(3) 0.9111(2) 0.0373(8) Uani 1 1 d . . . . .
H35D H 0.062233 0.491803 0.916325 0.056 Uiso 1 1 calc GR . . . .
H35E H 0.163377 0.430376 0.952075 0.056 Uiso 1 1 calc GR . . . .
H35F H 0.142226 0.435781 0.852111 0.056 Uiso 1 1 calc GR . . . .
C1AA C 0.0640(3) 0.9548(2) 0.6418(2) 0.0249(7) Uani 1 1 d . . . . .
C4AA C 0.3346(3) 0.9312(2) 0.4345(2) 0.0285(7) Uani 1 1 d . . . . .
H4AA H 0.368256 0.991026 0.425696 0.034 Uiso 1 1 calc R . . . .
B1 B 0.2339(3) 0.8343(2) 0.6299(2) 0.0221(7) Uani 1 1 d . . . . .
C128 C 0.1848(3) 0.6522(2) 0.4716(2) 0.0309(7) Uani 1 1 d . . . . .
H12G H 0.233776 0.621169 0.512143 0.046 Uiso 1 1 calc GR . . . .
H12H H 0.171357 0.605027 0.415141 0.046 Uiso 1 1 calc GR . . . .
H12I H 0.115056 0.666878 0.493644 0.046 Uiso 1 1 calc GR . . . .
C121 C 0.7037(3) 0.6632(3) 0.7229(2) 0.0359(8) Uani 1 1 d . . . . .
H12J H 0.747726 0.713538 0.768599 0.054 Uiso 1 1 calc GR . . . .
H12K H 0.736000 0.654930 0.669486 0.054 Uiso 1 1 calc GR . . . .
H12L H 0.702394 0.597799 0.740628 0.054 Uiso 1 1 calc GR . . . .
C232 C 0.3707(3) 0.2890(3) 0.7836(2) 0.0400(9) Uani 1 1 d . . . . .
H23A H 0.343923 0.328119 0.835087 0.060 Uiso 1 1 calc GR . . . .
H23B H 0.436389 0.253098 0.801112 0.060 Uiso 1 1 calc GR . . . .
H23C H 0.313584 0.239333 0.750589 0.060 Uiso 1 1 calc GR . . . .
C126 C 0.3476(3) 1.0231(2) 0.5902(2) 0.0350(8) Uani 1 1 d . . . . .
H12M H 0.282085 1.061675 0.601916 0.052 Uiso 1 1 calc GR . . . .
H12N H 0.399723 1.065691 0.571213 0.052 Uiso 1 1 calc GR . . . .
H12O H 0.381912 1.002809 0.642924 0.052 Uiso 1 1 calc GR . . . .
C116 C 0.2177(3) 0.9916(2) 0.7617(2) 0.0276(7) Uani 1 1 d . . . . .
C363 C 0.1260(3) 0.8781(3) 0.9516(3) 0.0459(9) Uani 1 1 d . . . . .
H36D H 0.161812 0.865297 1.006905 0.069 Uiso 1 1 calc GR . . . .
H36E H 0.061294 0.918873 0.960861 0.069 Uiso 1 1 calc GR . . . .
H36F H 0.177477 0.915153 0.926848 0.069 Uiso 1 1 calc GR . . . .
C5AA C 0.3060(3) 0.8491(2) 0.3631(2) 0.0293(7) Uani 1 1 d . . . . .
C111 C 0.6421(3) 0.8972(3) 0.8934(2) 0.0399(9) Uani 1 1 d . . . . .
H11G H 0.698676 0.876296 0.856560 0.060 Uiso 1 1 calc GR . . . .
H11H H 0.677172 0.929248 0.951895 0.060 Uiso 1 1 calc GR . . . .
H11I H 0.594638 0.945910 0.869545 0.060 Uiso 1 1 calc GR . . . .
C361 C -0.0311(3) 0.6902(3) 0.9184(2) 0.0392(9) Uani 1 1 d . . . . .
H36G H -0.060976 0.628824 0.876411 0.059 Uiso 1 1 calc GR . . . .
H36H H -0.089686 0.738519 0.928574 0.059 Uiso 1 1 calc GR . . . .
H36I H -0.000644 0.671788 0.972919 0.059 Uiso 1 1 calc GR . . . .
C353 C 0.2281(3) 0.6602(3) 1.0538(2) 0.0409(9) Uani 1 1 d . . . . .
H35G H 0.276170 0.721456 1.068064 0.061 Uiso 1 1 calc GR . . . .
H35H H 0.254269 0.613873 1.091519 0.061 Uiso 1 1 calc GR . . . .
H35I H 0.153092 0.679400 1.062200 0.061 Uiso 1 1 calc GR . . . .
C117 C 0.0055(3) 0.8898(2) 0.5561(2) 0.0358(8) Uani 1 1 d . . . . .
H11J H 0.049363 0.891719 0.509991 0.054 Uiso 1 1 calc GR . . . .
H11K H -0.066868 0.917012 0.541646 0.054 Uiso 1 1 calc GR . . . .
H11L H -0.003194 0.819285 0.562174 0.054 Uiso 1 1 calc GR . . . .
C241 C 0.1917(3) 0.3922(3) 0.5131(2) 0.0410(9) Uani 1 1 d . . . . .
H24G H 0.120148 0.397645 0.478927 0.062 Uiso 1 1 calc GR . . . .
H24H H 0.216478 0.322242 0.498042 0.062 Uiso 1 1 calc GR . . . .
H24I H 0.245047 0.439177 0.500612 0.062 Uiso 1 1 calc GR . . . .
C2AA C 0.0072(3) 1.0364(2) 0.6864(2) 0.0298(7) Uani 1 1 d . . . . .
H2AA H -0.063563 1.051583 0.660930 0.036 Uiso 1 1 calc R . . . .
C119 C 0.3328(3) 0.9735(3) 0.8066(2) 0.0404(8) Uani 1 1 d . . . . .
H11M H 0.357242 0.906805 0.778940 0.061 Uiso 1 1 calc GR . . . .
H11N H 0.330265 0.975244 0.867786 0.061 Uiso 1 1 calc GR . . . .
H11O H 0.384278 1.026870 0.801520 0.061 Uiso 1 1 calc GR . . . .
C231 C 0.4272(3) 0.2984(2) 0.6040(2) 0.0386(8) Uani 1 1 d . . . . .
H23D H 0.359870 0.257981 0.577718 0.058 Uiso 1 1 calc GR . . . .
H23E H 0.487749 0.252669 0.612353 0.058 Uiso 1 1 calc GR . . . .
H23F H 0.444669 0.342565 0.565969 0.058 Uiso 1 1 calc GR . . . .
C233 C 0.5464(3) 0.4414(3) 0.7637(3) 0.0403(9) Uani 1 1 d . . . . .
H23G H 0.579630 0.468153 0.720543 0.060 Uiso 1 1 calc GR . . . .
H23H H 0.593869 0.390515 0.784327 0.060 Uiso 1 1 calc GR . . . .
H23I H 0.537748 0.497307 0.812521 0.060 Uiso 1 1 calc GR . . . .
C127 C 0.3280(3) 0.8570(3) 0.2724(2) 0.0462(9) Uani 1 1 d . . . . .
H12P H 0.303174 0.793563 0.230993 0.069 Uiso 1 1 calc GR . . . .
H12Q H 0.406750 0.868553 0.273446 0.069 Uiso 1 1 calc GR . . . .
H12R H 0.287902 0.914000 0.254907 0.069 Uiso 1 1 calc GR . . . .
C115 C 0.1583(3) 1.0726(2) 0.8037(2) 0.0302(7) Uani 1 1 d . . . . .
H115 H 0.190234 1.112639 0.857917 0.036 Uiso 1 1 calc R . . . .
C118 C -0.0120(3) 1.1819(3) 0.8161(3) 0.0442(9) Uani 1 1 d . . . . .
H11P H -0.052785 1.217629 0.774740 0.066 Uiso 1 1 calc GR . . . .
H11Q H 0.039305 1.229936 0.858006 0.066 Uiso 1 1 calc GR . . . .
H11R H -0.063501 1.152729 0.846440 0.066 Uiso 1 1 calc GR . . . .
C114 C 0.0529(3) 1.0951(2) 0.7668(2) 0.0327(8) Uani 1 1 d . . . . .
Si2 Si 0.55777(7) 0.70884(6) 0.70372(6) 0.02300(18) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 Si5 3.3480(8) . ?
U1 Si4 3.3795(8) . ?
U1 O1 2.1559(18) . ?
U1 N1 2.262(2) . ?
U1 N3 2.256(2) . ?
U1 N2 2.285(2) . ?
U1 Si2 3.3373(8) . ?
Si5 N3 1.744(2) . ?
Si5 C351 1.872(3) . ?
Si5 C352 1.867(3) . ?
Si5 C353 1.868(3) . ?
Si1 N1 1.748(2) . ?
Si1 C113 1.874(3) . ?
Si1 C112 1.873(3) . ?
Si1 C111 1.873(3) . ?
Si6 N3 1.756(2) . ?
Si6 C362 1.854(3) . ?
Si6 C363 1.864(4) . ?
Si6 C361 1.877(3) . ?
Si3 N2 1.749(2) . ?
Si3 C232 1.881(3) . ?
Si3 C231 1.864(3) . ?
Si3 C233 1.868(3) . ?
Si4 N2 1.743(2) . ?
Si4 C242 1.872(3) . ?
Si4 C243 1.864(3) . ?
Si4 C241 1.868(3) . ?
O1 B1 1.365(4) . ?
N1 Si2 1.745(2) . ?
C123 H12A 0.9600 . ?
C123 H12B 0.9600 . ?
C123 H12C 0.9600 . ?
C123 Si2 1.880(3) . ?
C120 C125 1.410(4) . ?
C120 C3AA 1.425(4) . ?
C120 B1 1.589(4) . ?
C351 H35A 0.9600 . ?
C351 H35B 0.9600 . ?
C351 H35C 0.9600 . ?
C0AA C1AA 1.408(4) . ?
C0AA B1 1.594(4) . ?
C0AA C116 1.406(4) . ?
C113 H11A 0.9600 . ?
C113 H11B 0.9600 . ?
C113 H11C 0.9600 . ?
C242 H24A 0.9600 . ?
C242 H24B 0.9600 . ?
C242 H24C 0.9600 . ?
C125 C124 1.387(4) . ?
C125 C128 1.517(4) . ?
C3AA C4AA 1.385(4) . ?
C3AA C126 1.509(4) . ?
C122 H12D 0.9600 . ?
C122 H12E 0.9600 . ?
C122 H12F 0.9600 . ?
C122 Si2 1.871(3) . ?
C112 H11D 0.9600 . ?
C112 H11E 0.9600 . ?
C112 H11F 0.9600 . ?
C124 H124 0.9300 . ?
C124 C5AA 1.385(4) . ?
C243 H24D 0.9600 . ?
C243 H24E 0.9600 . ?
C243 H24F 0.9600 . ?
C362 H36A 0.9600 . ?
C362 H36B 0.9600 . ?
C362 H36C 0.9600 . ?
C352 H35D 0.9600 . ?
C352 H35E 0.9600 . ?
C352 H35F 0.9600 . ?
C1AA C117 1.508(4) . ?
C1AA C2AA 1.391(4) . ?
C4AA H4AA 0.9300 . ?
C4AA C5AA 1.384(4) . ?
C128 H12G 0.9600 . ?
C128 H12H 0.9600 . ?
C128 H12I 0.9600 . ?
C121 H12J 0.9600 . ?
C121 H12K 0.9600 . ?
C121 H12L 0.9600 . ?
C121 Si2 1.866(3) . ?
C232 H23A 0.9600 . ?
C232 H23B 0.9600 . ?
C232 H23C 0.9600 . ?
C126 H12M 0.9600 . ?
C126 H12N 0.9600 . ?
C126 H12O 0.9600 . ?
C116 C119 1.507(4) . ?
C116 C115 1.388(4) . ?
C363 H36D 0.9600 . ?
C363 H36E 0.9600 . ?
C363 H36F 0.9600 . ?
C5AA C127 1.508(4) . ?
C111 H11G 0.9600 . ?
C111 H11H 0.9600 . ?
C111 H11I 0.9600 . ?
C361 H36G 0.9600 . ?
C361 H36H 0.9600 . ?
C361 H36I 0.9600 . ?
C353 H35G 0.9600 . ?
C353 H35H 0.9600 . ?
C353 H35I 0.9600 . ?
C117 H11J 0.9600 . ?
C117 H11K 0.9600 . ?
C117 H11L 0.9600 . ?
C241 H24G 0.9600 . ?
C241 H24H 0.9600 . ?
C241 H24I 0.9600 . ?
C2AA H2AA 0.9300 . ?
C2AA C114 1.370(5) . ?
C119 H11M 0.9600 . ?
C119 H11N 0.9600 . ?
C119 H11O 0.9600 . ?
C231 H23D 0.9600 . ?
C231 H23E 0.9600 . ?
C231 H23F 0.9600 . ?
C233 H23G 0.9600 . ?
C233 H23H 0.9600 . ?
C233 H23I 0.9600 . ?
C127 H12P 0.9600 . ?
C127 H12Q 0.9600 . ?
C127 H12R 0.9600 . ?
C115 H115 0.9300 . ?
C115 C114 1.379(5) . ?
C118 H11P 0.9600 . ?
C118 H11Q 0.9600 . ?
C118 H11R 0.9600 . ?
C118 C114 1.523(5) . ?

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
Si5 U1 Si4 89.77(2) . . ?
O1 U1 Si5 134.83(5) . . ?
O1 U1 Si4 99.19(5) . . ?
O1 U1 N1 94.85(8) . . ?
O1 U1 N3 106.19(8) . . ?
O1 U1 N2 120.44(8) . . ?
O1 U1 Si2 80.69(5) . . ?
N1 U1 Si5 107.01(6) . . ?
N1 U1 Si4 138.83(6) . . ?
N1 U1 N2 113.72(8) . . ?
N1 U1 Si2 28.96(6) . . ?
N3 U1 Si5 28.64(6) . . ?
N3 U1 Si4 95.89(6) . . ?
N3 U1 N1 116.96(9) . . ?
N3 U1 N2 105.00(8) . . ?
N3 U1 Si2 145.45(6) . . ?
N2 U1 Si5 86.46(6) . . ?
N2 U1 Si4 28.25(6) . . ?
N2 U1 Si2 99.73(6) . . ?
Si2 U1 Si5 133.55(2) . . ?
Si2 U1 Si4 116.77(2) . . ?
N3 Si5 U1 38.33(8) . . ?
N3 Si5 C351 108.15(13) . . ?
N3 Si5 C352 113.08(14) . . ?
N3 Si5 C353 115.09(14) . . ?
C351 Si5 U1 72.34(10) . . ?
C352 Si5 U1 112.29(12) . . ?
C352 Si5 C351 107.45(15) . . ?
C352 Si5 C353 108.53(16) . . ?
C353 Si5 U1 138.16(12) . . ?
C353 Si5 C351 103.89(16) . . ?
N1 Si1 C113 112.05(14) . . ?
N1 Si1 C112 111.49(13) . . ?
N1 Si1 C111 112.85(14) . . ?
C112 Si1 C113 107.44(15) . . ?
C111 Si1 C113 106.51(16) . . ?
C111 Si1 C112 106.10(16) . . ?
N3 Si6 C362 112.35(14) . . ?
N3 Si6 C363 110.76(15) . . ?
N3 Si6 C361 112.95(14) . . ?
C362 Si6 C363 108.65(17) . . ?
C362 Si6 C361 104.02(15) . . ?
C363 Si6 C361 107.77(17) . . ?
N2 Si3 C232 113.05(14) . . ?
N2 Si3 C231 111.36(14) . . ?
N2 Si3 C233 112.22(13) . . ?
C231 Si3 C232 107.33(16) . . ?
C231 Si3 C233 105.63(17) . . ?
C233 Si3 C232 106.80(17) . . ?
N2 Si4 U1 38.36(8) . . ?
N2 Si4 C242 107.20(13) . . ?
N2 Si4 C243 114.49(14) . . ?
N2 Si4 C241 113.53(15) . . ?
C242 Si4 U1 69.88(10) . . ?
C243 Si4 U1 134.91(12) . . ?
C243 Si4 C242 107.09(16) . . ?
C243 Si4 C241 106.42(16) . . ?
C241 Si4 U1 117.47(11) . . ?
C241 Si4 C242 107.77(16) . . ?
B1 O1 U1 167.23(19) . . ?
Si1 N1 U1 130.12(12) . . ?
Si2 N1 U1 112.15(12) . . ?
Si2 N1 Si1 117.70(13) . . ?
Si5 N3 U1 113.03(11) . . ?
Si5 N3 Si6 115.86(13) . . ?
Si6 N3 U1 131.05(12) . . ?
Si3 N2 U1 130.28(12) . . ?
Si4 N2 U1 113.39(11) . . ?
Si4 N2 Si3 116.28(13) . . ?
H12A C123 H12B 109.5 . . ?
H12A C123 H12C 109.5 . . ?
H12B C123 H12C 109.5 . . ?
Si2 C123 H12A 109.5 . . ?
Si2 C123 H12B 109.5 . . ?
Si2 C123 H12C 109.5 . . ?
C125 C120 C3AA 116.4(3) . . ?
C125 C120 B1 122.5(2) . . ?
C3AA C120 B1 120.9(3) . . ?
Si5 C351 H35A 109.5 . . ?
Si5 C351 H35B 109.5 . . ?
Si5 C351 H35C 109.5 . . ?
H35A C351 H35B 109.5 . . ?
H35A C351 H35C 109.5 . . ?
H35B C351 H35C 109.5 . . ?
C1AA C0AA B1 119.9(3) . . ?
C116 C0AA C1AA 118.0(3) . . ?
C116 C0AA B1 122.1(3) . . ?
Si1 C113 H11A 109.5 . . ?
Si1 C113 H11B 109.5 . . ?
Si1 C113 H11C 109.5 . . ?
H11A C113 H11B 109.5 . . ?
H11A C113 H11C 109.5 . . ?
H11B C113 H11C 109.5 . . ?
Si4 C242 H24A 109.5 . . ?
Si4 C242 H24B 109.5 . . ?
Si4 C242 H24C 109.5 . . ?
H24A C242 H24B 109.5 . . ?
H24A C242 H24C 109.5 . . ?
H24B C242 H24C 109.5 . . ?
C120 C125 C128 121.1(3) . . ?
C124 C125 C120 121.1(3) . . ?
C124 C125 C128 117.7(3) . . ?
C120 C3AA C126 122.5(3) . . ?
C4AA C3AA C120 120.7(3) . . ?
C4AA C3AA C126 116.8(3) . . ?
H12D C122 H12E 109.5 . . ?
H12D C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
Si2 C122 H12D 109.5 . . ?
Si2 C122 H12E 109.5 . . ?
Si2 C122 H12F 109.5 . . ?
Si1 C112 H11D 109.5 . . ?
Si1 C112 H11E 109.5 . . ?
Si1 C112 H11F 109.5 . . ?
H11D C112 H11E 109.5 . . ?
H11D C112 H11F 109.5 . . ?
H11E C112 H11F 109.5 . . ?
C125 C124 H124 119.0 . . ?
C5AA C124 C125 121.9(3) . . ?
C5AA C124 H124 119.0 . . ?
Si4 C243 H24D 109.5 . . ?
Si4 C243 H24E 109.5 . . ?
Si4 C243 H24F 109.5 . . ?
H24D C243 H24E 109.5 . . ?
H24D C243 H24F 109.5 . . ?
H24E C243 H24F 109.5 . . ?
Si6 C362 H36A 109.5 . . ?
Si6 C362 H36B 109.5 . . ?
Si6 C362 H36C 109.5 . . ?
H36A C362 H36B 109.5 . . ?
H36A C362 H36C 109.5 . . ?
H36B C362 H36C 109.5 . . ?
Si5 C352 H35D 109.5 . . ?
Si5 C352 H35E 109.5 . . ?
Si5 C352 H35F 109.5 . . ?
H35D C352 H35E 109.5 . . ?
H35D C352 H35F 109.5 . . ?
H35E C352 H35F 109.5 . . ?
C0AA C1AA C117 121.3(3) . . ?
C2AA C1AA C0AA 120.0(3) . . ?
C2AA C1AA C117 118.6(3) . . ?
C3AA C4AA H4AA 118.9 . . ?
C5AA C4AA C3AA 122.2(3) . . ?
C5AA C4AA H4AA 118.9 . . ?
O1 B1 C120 122.3(3) . . ?
O1 B1 C0AA 118.7(3) . . ?
C120 B1 C0AA 119.0(2) . . ?
C125 C128 H12G 109.5 . . ?
C125 C128 H12H 109.5 . . ?
C125 C128 H12I 109.5 . . ?
H12G C128 H12H 109.5 . . ?
H12G C128 H12I 109.5 . . ?
H12H C128 H12I 109.5 . . ?
H12J C121 H12K 109.5 . . ?
H12J C121 H12L 109.5 . . ?
H12K C121 H12L 109.5 . . ?
Si2 C121 H12J 109.5 . . ?
Si2 C121 H12K 109.5 . . ?
Si2 C121 H12L 109.5 . . ?
Si3 C232 H23A 109.5 . . ?
Si3 C232 H23B 109.5 . . ?
Si3 C232 H23C 109.5 . . ?
H23A C232 H23B 109.5 . . ?
H23A C232 H23C 109.5 . . ?
H23B C232 H23C 109.5 . . ?
C3AA C126 H12M 109.5 . . ?
C3AA C126 H12N 109.5 . . ?
C3AA C126 H12O 109.5 . . ?
H12M C126 H12N 109.5 . . ?
H12M C126 H12O 109.5 . . ?
H12N C126 H12O 109.5 . . ?
C0AA C116 C119 122.1(3) . . ?
C115 C116 C0AA 120.0(3) . . ?
C115 C116 C119 117.8(3) . . ?
Si6 C363 H36D 109.5 . . ?
Si6 C363 H36E 109.5 . . ?
Si6 C363 H36F 109.5 . . ?
H36D C363 H36E 109.5 . . ?
H36D C363 H36F 109.5 . . ?
H36E C363 H36F 109.5 . . ?
C124 C5AA C127 121.9(3) . . ?
C4AA C5AA C124 117.6(3) . . ?
C4AA C5AA C127 120.5(3) . . ?
Si1 C111 H11G 109.5 . . ?
Si1 C111 H11H 109.5 . . ?
Si1 C111 H11I 109.5 . . ?
H11G C111 H11H 109.5 . . ?
H11G C111 H11I 109.5 . . ?
H11H C111 H11I 109.5 . . ?
Si6 C361 H36G 109.5 . . ?
Si6 C361 H36H 109.5 . . ?
Si6 C361 H36I 109.5 . . ?
H36G C361 H36H 109.5 . . ?
H36G C361 H36I 109.5 . . ?
H36H C361 H36I 109.5 . . ?
Si5 C353 H35G 109.5 . . ?
Si5 C353 H35H 109.5 . . ?
Si5 C353 H35I 109.5 . . ?
H35G C353 H35H 109.5 . . ?
H35G C353 H35I 109.5 . . ?
H35H C353 H35I 109.5 . . ?
C1AA C117 H11J 109.5 . . ?
C1AA C117 H11K 109.5 . . ?
C1AA C117 H11L 109.5 . . ?
H11J C117 H11K 109.5 . . ?
H11J C117 H11L 109.5 . . ?
H11K C117 H11L 109.5 . . ?
Si4 C241 H24G 109.5 . . ?
Si4 C241 H24H 109.5 . . ?
Si4 C241 H24I 109.5 . . ?
H24G C241 H24H 109.5 . . ?
H24G C241 H24I 109.5 . . ?
H24H C241 H24I 109.5 . . ?
C1AA C2AA H2AA 119.2 . . ?
C114 C2AA C1AA 121.7(3) . . ?
C114 C2AA H2AA 119.2 . . ?
C116 C119 H11M 109.5 . . ?
C116 C119 H11N 109.5 . . ?
C116 C119 H11O 109.5 . . ?
H11M C119 H11N 109.5 . . ?
H11M C119 H11O 109.5 . . ?
H11N C119 H11O 109.5 . . ?
Si3 C231 H23D 109.5 . . ?
Si3 C231 H23E 109.5 . . ?
Si3 C231 H23F 109.5 . . ?
H23D C231 H23E 109.5 . . ?
H23D C231 H23F 109.5 . . ?
H23E C231 H23F 109.5 . . ?
Si3 C233 H23G 109.5 . . ?
Si3 C233 H23H 109.5 . . ?
Si3 C233 H23I 109.5 . . ?
H23G C233 H23H 109.5 . . ?
H23G C233 H23I 109.5 . . ?
H23H C233 H23I 109.5 . . ?
C5AA C127 H12P 109.5 . . ?
C5AA C127 H12Q 109.5 . . ?
C5AA C127 H12R 109.5 . . ?
H12P C127 H12Q 109.5 . . ?
H12P C127 H12R 109.5 . . ?
H12Q C127 H12R 109.5 . . ?
C116 C115 H115 119.2 . . ?
C114 C115 C116 121.6(3) . . ?
C114 C115 H115 119.2 . . ?
H11P C118 H11Q 109.5 . . ?
H11P C118 H11R 109.5 . . ?
H11Q C118 H11R 109.5 . . ?
C114 C118 H11P 109.5 . . ?
C114 C118 H11Q 109.5 . . ?
C114 C118 H11R 109.5 . . ?
C2AA C114 C115 118.7(3) . . ?
C2AA C114 C118 120.9(3) . . ?
C115 C114 C118 120.3(3) . . ?
N1 Si2 U1 38.89(8) . . ?
N1 Si2 C123 109.27(13) . . ?
N1 Si2 C122 114.18(14) . . ?
N1 Si2 C121 113.76(13) . . ?
C123 Si2 U1 71.40(10) . . ?
C122 Si2 U1 116.61(11) . . ?
C122 Si2 C123 104.59(15) . . ?
C121 Si2 U1 135.64(11) . . ?
C121 Si2 C123 107.89(15) . . ?
C121 Si2 C122 106.60(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.711

# start Validation Reply Form
_vrf_PLAT910_p18053_tri          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE: No. of reflections / No. of parameters = 21.5 Therefore
this is not seen as a serious problem.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p18089
_database_code_depnum_ccdc_archive 'CCDC 1886809'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.67(C108 H132 B6 K2 O8 U2)'
_chemical_formula_sum            'C72 H88 B4 K1.33 O5.33 U1.33'
_chemical_formula_weight         1451.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U2 O6 B6 C100 H100 P2'
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.3907(2)
_cell_length_b                   22.7218(2)
_cell_length_c                   16.9809(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.680(2)
_cell_angle_gamma                90
_cell_volume                     5591.43(13)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    26955
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2430
_cell_measurement_theta_min      3.1960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -13 -18 0.0824
5 13 18 0.0824
-11 -25 12 0.1463
-18 4 19 0.1442
2 -31 3 0.0788
3 30 -9 0.1187
17 4 -20 0.1037
-15 21 13 0.1312
20 13 -6 0.1020
9 -14 14 0.0655
-3 19 -17 0.0860
-13 9 -11 0.0980
-20 -5 -2 0.1280
-19 13 3 0.1002
2 -22 -17 0.0870

_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.162
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0000 -12.9999 -18.0000 -0.2949 0.9495 0.0716
5.0000 12.9999 18.0000 0.2949 -0.9495 -0.0716
-11.0000 -25.0000 12.0000 -0.0399 0.1921 -0.9750
-18.0000 3.9999 19.0000 -0.6194 -0.5059 -0.6021
2.0000 -31.0000 3.0000 0.5050 0.4485 -0.7188
3.0000 30.0000 -9.0000 -0.3434 -0.2844 0.9054
17.0000 4.0001 -20.0000 0.4645 0.4047 0.7864
-15.0000 21.0000 13.0000 -0.7668 -0.6527 -0.0504
20.0000 13.0000 -6.0000 0.6673 -0.3010 0.6944
9.0000 -14.0001 14.0000 0.7529 -0.3549 -0.5119
-3.0000 19.0001 -17.0000 -0.5812 0.2865 0.7724
-13.0000 9.0001 -11.0000 -0.8344 0.3963 0.2785
-20.0000 -4.9999 -2.0000 -0.8658 0.4344 -0.3324
-19.0000 13.0000 3.0000 -0.9763 -0.0941 -0.0440
2.0000 -21.9999 -17.0000 0.1426 0.9886 -0.0533

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            109506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.811
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  20.00   1.00   15.00    --  -16.53 -99.00  90.00   45
  2  ω    -87.00 -34.00   1.00   15.00    --  -16.53-179.00 150.00   53
  3  ω    -31.00  49.00   1.00   15.00    --  -16.53  57.00-150.00   80
  4  ω    -25.00  20.00   1.00   15.00    --  -16.53 -99.00 -90.00   45
  5  ω    -85.00   1.00   1.00   15.00    --  -16.53 -37.00  30.00   86
  6  ω    -31.00  49.00   1.00   15.00    --  -16.53  57.00-120.00   80
  7  ω     34.00  89.00   1.00   15.00    --   18.25 179.00  30.00   55
  8  ω    -47.00  33.00   1.00   15.00    --   18.25 -57.00-180.00   80
  9  ω      3.00  84.00   1.00   15.00    --   18.25  57.00 150.00   81
 10  ω      1.00  87.00   1.00   15.00    --   18.25  37.00  30.00   86
 11  ω    -48.00  43.00   1.00   15.00    --   18.25 -77.00  30.00   91
 12  ω      3.00  84.00   1.00   15.00    --   18.25  57.00-120.00   81
 13  ω      5.00  40.00   1.00   15.00    --   18.25-137.00 176.60   35
 14  ω    -50.00  36.00   1.00   15.00    --   18.25 -37.00  60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0450628000
_diffrn_orient_matrix_UB_12      -0.0121587000
_diffrn_orient_matrix_UB_13      0.0126490000
_diffrn_orient_matrix_UB_21      -0.0134847000
_diffrn_orient_matrix_UB_22      -0.0187675000
_diffrn_orient_matrix_UB_23      -0.0354493000
_diffrn_orient_matrix_UB_31      0.0135194000
_diffrn_orient_matrix_UB_32      0.0217873000
_diffrn_orient_matrix_UB_33      -0.0234704000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8129
_reflns_number_total             10220
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+2.0433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C234(H234), C225(H225), C333(H333), C223(H223), C335(H335), C122(H122),
 C342(H342), C124(H124), C113(H113), C232(H232), C344(H344), C115(H115)
2.b Idealised Me refined as rotating group:
 C229(H22A,H22B,H22C), C128(H12A,H12B,H12C), C238(H23A,H23B,H23C), C337(H33A,
 H33B,H33C), C227(H22D,H22E,H22F), C346(H34A,H34B,H34C), C228(H22G,H22H,H22I),
 C348(H34D,H34E,H34F), C236(H23D,H23E,H23F), C117(H11A,H11B,H11C), C126(H12D,
 H12E,H12F), C339(H33D,H33E,H33F), C338(H33G,H33H,H33I), C347(H34G,H34H,H34I),
 C119(H11D,H11E,H11F), C237(H23G,H23H,H23I), C127(H12G,H12H,H12I), C118(H11G,
 H11H,H11I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.07738(2) 0.52193(2) 0.09437(2) 0.02739(5) Uani 1 1 d . . . . .
K1 K -0.04028(7) 0.36860(4) 0.12096(6) 0.0496(3) Uani 1 1 d . . . . .
O4 O -0.01352(15) 0.45151(9) 0.03215(14) 0.0278(5) Uani 1 1 d . . . . .
O2 O 0.21331(17) 0.51561(11) 0.08182(17) 0.0423(7) Uani 1 1 d . . . . .
O1 O 0.04526(19) 0.60663(10) 0.14186(16) 0.0436(7) Uani 1 1 d . . . . .
O3 O 0.10689(18) 0.47173(10) 0.21347(16) 0.0410(6) Uani 1 1 d . . . . .
C230 C 0.3863(2) 0.50189(15) 0.1261(2) 0.0296(8) Uani 1 1 d . . . . .
C120 C 0.0167(2) 0.69737(14) 0.0514(2) 0.0317(8) Uani 1 1 d . . . . .
C235 C 0.4154(2) 0.51149(15) 0.2128(2) 0.0332(9) Uani 1 1 d . . . . .
C226 C 0.2268(2) 0.55845(15) -0.0926(2) 0.0318(8) Uani 1 1 d . . . . .
C229 C 0.1812(3) 0.49907(17) -0.1162(3) 0.0431(10) Uani 1 1 d . . . . .
H22A H 0.180627 0.478925 -0.066720 0.065 Uiso 1 1 calc GR . . . .
H22B H 0.215050 0.476200 -0.143658 0.065 Uiso 1 1 calc GR . . . .
H22C H 0.119015 0.504368 -0.153343 0.065 Uiso 1 1 calc GR . . . .
C221 C 0.2832(2) 0.57120(14) -0.0103(2) 0.0305(8) Uani 1 1 d . . . . .
C234 C 0.5007(3) 0.49045(16) 0.2636(2) 0.0387(9) Uani 1 1 d . . . . .
H234 H 0.519423 0.497668 0.320778 0.046 Uiso 1 1 calc R . . . .
C222 C 0.3264(3) 0.62716(15) 0.0043(2) 0.0363(9) Uani 1 1 d . . . . .
C125 C -0.0708(3) 0.69491(15) -0.0117(2) 0.0353(9) Uani 1 1 d . . . . .
C332 C 0.2963(3) 0.40440(15) 0.3055(2) 0.0346(9) Uani 1 1 d . . . . .
C331 C 0.2399(3) 0.43575(15) 0.3413(2) 0.0340(8) Uani 1 1 d . . . . .
C121 C 0.0846(3) 0.73196(16) 0.0350(3) 0.0398(9) Uani 1 1 d . . . . .
C224 C 0.2529(3) 0.65537(16) -0.1404(3) 0.0396(9) Uani 1 1 d . . . . .
C128 C -0.1462(3) 0.65663(18) -0.0006(3) 0.0485(11) Uani 1 1 d . . . . .
H12A H -0.144413 0.618558 -0.024502 0.073 Uiso 1 1 calc GR . . . .
H12B H -0.205091 0.674576 -0.028093 0.073 Uiso 1 1 calc GR . . . .
H12C H -0.136864 0.652439 0.057965 0.073 Uiso 1 1 calc GR . . . .
C225 C 0.2134(2) 0.59961(16) -0.1559(2) 0.0354(9) Uani 1 1 d . . . . .
H225 H 0.177057 0.589689 -0.210104 0.042 Uiso 1 1 calc R . . . .
C238 C 0.3565(3) 0.54447(17) 0.2536(2) 0.0428(10) Uani 1 1 d . . . . .
H23A H 0.340004 0.582157 0.227230 0.064 Uiso 1 1 calc GR . . . .
H23B H 0.390448 0.549886 0.311946 0.064 Uiso 1 1 calc GR . . . .
H23C H 0.301475 0.522284 0.247461 0.064 Uiso 1 1 calc GR . . . .
C337 C 0.2616(3) 0.38254(17) 0.2161(2) 0.0417(9) Uani 1 1 d . . . . .
H33A H 0.196699 0.374409 0.199932 0.063 Uiso 1 1 calc GR . . . .
H33B H 0.293923 0.347225 0.211849 0.063 Uiso 1 1 calc GR . . . .
H33C H 0.272013 0.412107 0.179940 0.063 Uiso 1 1 calc GR . . . .
C111 C 0.0556(3) 0.70197(15) 0.2235(2) 0.0371(9) Uani 1 1 d . . . . .
C340 C 0.0551(2) 0.42778(15) 0.3269(2) 0.0338(8) Uani 1 1 d . . . . .
C333 C 0.3880(3) 0.39280(16) 0.3516(2) 0.0374(9) Uani 1 1 d . . . . .
H333 H 0.423384 0.371117 0.327067 0.045 Uiso 1 1 calc R . . . .
C345 C -0.0054(3) 0.46830(17) 0.3443(2) 0.0408(10) Uani 1 1 d . . . . .
C334 C 0.4286(3) 0.41255(16) 0.4332(2) 0.0390(9) Uani 1 1 d . . . . .
C223 C 0.3092(3) 0.66760(16) -0.0600(3) 0.0422(10) Uani 1 1 d . . . . .
H223 H 0.336638 0.704522 -0.048458 0.051 Uiso 1 1 calc R . . . .
C335 C 0.3734(3) 0.44430(17) 0.4672(2) 0.0465(10) Uani 1 1 d . . . . .
H335 H 0.399310 0.458725 0.521325 0.056 Uiso 1 1 calc R . . . .
C227 C 0.3905(3) 0.64418(17) 0.0902(3) 0.0500(11) Uani 1 1 d . . . . .
H22D H 0.355204 0.651099 0.126401 0.075 Uiso 1 1 calc GR . . . .
H22E H 0.423341 0.679360 0.086275 0.075 Uiso 1 1 calc GR . . . .
H22F H 0.433728 0.612913 0.112668 0.075 Uiso 1 1 calc GR . . . .
C231 C 0.4444(3) 0.46856(15) 0.0938(2) 0.0339(9) Uani 1 1 d . . . . .
C112 C -0.0015(3) 0.74996(17) 0.2288(3) 0.0431(10) Uani 1 1 d . . . . .
B1 B 0.0389(3) 0.66497(18) 0.1393(3) 0.0346(10) Uani 1 1 d . . . . .
C122 C 0.0645(3) 0.76241(16) -0.0401(3) 0.0497(11) Uani 1 1 d . . . . .
H122 H 0.111333 0.783501 -0.050391 0.060 Uiso 1 1 calc R . . . .
C233 C 0.5584(3) 0.45939(17) 0.2323(3) 0.0393(9) Uani 1 1 d . . . . .
C116 C 0.1294(3) 0.68737(16) 0.2965(3) 0.0376(9) Uani 1 1 d . . . . .
C336 C 0.2810(3) 0.45565(16) 0.4241(2) 0.0399(9) Uani 1 1 d . . . . .
C341 C 0.0445(3) 0.36849(16) 0.3443(2) 0.0369(9) Uani 1 1 d . . . . .
B2 B 0.2905(3) 0.52798(17) 0.0662(3) 0.0352(10) Uani 1 1 d . . . . .
C342 C -0.0220(3) 0.35115(18) 0.3780(2) 0.0433(10) Uani 1 1 d . . . . .
H342 H -0.028757 0.311337 0.387300 0.052 Uiso 1 1 calc R . . . .
C124 C -0.0889(3) 0.72813(17) -0.0841(3) 0.0442(10) Uani 1 1 d . . . . .
H124 H -0.147944 0.727273 -0.123552 0.053 Uiso 1 1 calc R . . . .
C346 C 0.1064(3) 0.32161(17) 0.3288(3) 0.0512(11) Uani 1 1 d . . . . .
H34A H 0.103901 0.323450 0.271553 0.077 Uiso 1 1 calc GR . . . .
H34B H 0.086010 0.283557 0.339851 0.077 Uiso 1 1 calc GR . . . .
H34C H 0.168704 0.328038 0.365000 0.077 Uiso 1 1 calc GR . . . .
C123 C -0.0222(3) 0.76244(16) -0.0997(3) 0.0490(11) Uani 1 1 d . . . . .
C228 C 0.2350(3) 0.70083(18) -0.2091(3) 0.0589(12) Uani 1 1 d . . . . .
H22G H 0.183057 0.688898 -0.256150 0.088 Uiso 1 1 calc GR . . . .
H22H H 0.288474 0.704321 -0.225867 0.088 Uiso 1 1 calc GR . . . .
H22I H 0.222215 0.738146 -0.188846 0.088 Uiso 1 1 calc GR . . . .
C113 C 0.0137(3) 0.77870(18) 0.3042(3) 0.0505(11) Uani 1 1 d . . . . .
H113 H -0.025107 0.809534 0.306413 0.061 Uiso 1 1 calc R . . . .
C348 C 0.0004(3) 0.53352(17) 0.3287(3) 0.0533(12) Uani 1 1 d . . . . .
H34D H 0.044849 0.551418 0.376700 0.080 Uiso 1 1 calc GR . . . .
H34E H -0.058927 0.551282 0.318960 0.080 Uiso 1 1 calc GR . . . .
H34F H 0.018899 0.539249 0.280647 0.080 Uiso 1 1 calc GR . . . .
C232 C 0.5286(3) 0.44810(16) 0.1475(2) 0.0382(9) Uani 1 1 d . . . . .
H232 H 0.566015 0.426091 0.125603 0.046 Uiso 1 1 calc R . . . .
C114 C 0.0843(3) 0.76323(18) 0.3760(3) 0.0519(12) Uani 1 1 d . . . . .
C343 C -0.0783(3) 0.3913(2) 0.3981(2) 0.0481(11) Uani 1 1 d . . . . .
C344 C -0.0689(3) 0.4496(2) 0.3807(3) 0.0475(11) Uani 1 1 d . . . . .
H344 H -0.106259 0.477365 0.393816 0.057 Uiso 1 1 calc R . . . .
C236 C 0.4151(3) 0.45382(17) 0.0026(2) 0.0424(10) Uani 1 1 d . . . . .
H23D H 0.360325 0.430137 -0.012520 0.064 Uiso 1 1 calc GR . . . .
H23E H 0.463550 0.432408 -0.008456 0.064 Uiso 1 1 calc GR . . . .
H23F H 0.402834 0.489477 -0.029583 0.064 Uiso 1 1 calc GR . . . .
C115 C 0.1427(3) 0.71796(18) 0.3708(3) 0.0472(10) Uani 1 1 d . . . . .
H115 H 0.192005 0.707778 0.418087 0.057 Uiso 1 1 calc R . . . .
C117 C -0.0821(3) 0.77074(19) 0.1557(3) 0.0558(12) Uani 1 1 d . . . . .
H11A H -0.060905 0.782216 0.110851 0.084 Uiso 1 1 calc GR . . . .
H11B H -0.110557 0.803811 0.172457 0.084 Uiso 1 1 calc GR . . . .
H11C H -0.126204 0.739452 0.137214 0.084 Uiso 1 1 calc GR . . . .
C126 C 0.1810(3) 0.7358(2) 0.0992(3) 0.0581(12) Uani 1 1 d . . . . .
H12D H 0.200481 0.697405 0.121943 0.087 Uiso 1 1 calc GR . . . .
H12E H 0.180520 0.762009 0.143415 0.087 Uiso 1 1 calc GR . . . .
H12F H 0.222978 0.750397 0.072897 0.087 Uiso 1 1 calc GR . . . .
C339 C 0.2278(3) 0.4926(2) 0.4669(3) 0.0589(13) Uani 1 1 d . . . . .
H33D H 0.208528 0.528649 0.436539 0.088 Uiso 1 1 calc GR . . . .
H33E H 0.266738 0.501392 0.523045 0.088 Uiso 1 1 calc GR . . . .
H33F H 0.174579 0.471214 0.468334 0.088 Uiso 1 1 calc GR . . . .
C338 C 0.5291(3) 0.40082(18) 0.4812(3) 0.0537(12) Uani 1 1 d . . . . .
H33G H 0.537168 0.360040 0.496788 0.081 Uiso 1 1 calc GR . . . .
H33H H 0.548513 0.424769 0.530703 0.081 Uiso 1 1 calc GR . . . .
H33I H 0.565451 0.410196 0.446801 0.081 Uiso 1 1 calc GR . . . .
B3 B 0.1327(3) 0.44756(17) 0.2894(3) 0.0340(10) Uani 1 1 d . . . . .
C347 C -0.1461(3) 0.3716(2) 0.4400(3) 0.0635(13) Uani 1 1 d . . . . .
H34G H -0.183198 0.339999 0.408547 0.095 Uiso 1 1 calc GR . . . .
H34H H -0.185210 0.404010 0.442337 0.095 Uiso 1 1 calc GR . . . .
H34I H -0.112927 0.358340 0.495755 0.095 Uiso 1 1 calc GR . . . .
C119 C 0.1974(3) 0.63912(18) 0.2985(3) 0.0525(11) Uani 1 1 d . . . . .
H11D H 0.167572 0.601570 0.294303 0.079 Uiso 1 1 calc GR . . . .
H11E H 0.248328 0.641114 0.350153 0.079 Uiso 1 1 calc GR . . . .
H11F H 0.219617 0.643964 0.252463 0.079 Uiso 1 1 calc GR . . . .
C237 C 0.6523(3) 0.4396(2) 0.2895(3) 0.0567(12) Uani 1 1 d . . . . .
H23G H 0.696508 0.470375 0.294062 0.085 Uiso 1 1 calc GR . . . .
H23H H 0.670721 0.404962 0.266757 0.085 Uiso 1 1 calc GR . . . .
H23I H 0.649351 0.430907 0.343812 0.085 Uiso 1 1 calc GR . . . .
C127 C -0.0438(4) 0.79984(19) -0.1775(3) 0.0742(16) Uani 1 1 d . . . . .
H12G H -0.001238 0.790613 -0.206098 0.111 Uiso 1 1 calc GR . . . .
H12H H -0.038108 0.840686 -0.162183 0.111 Uiso 1 1 calc GR . . . .
H12I H -0.105598 0.791973 -0.213714 0.111 Uiso 1 1 calc GR . . . .
C118 C 0.0972(4) 0.7944(2) 0.4584(3) 0.0786(16) Uani 1 1 d . . . . .
H11G H 0.114694 0.834535 0.454562 0.118 Uiso 1 1 calc GR . . . .
H11H H 0.144634 0.774912 0.502499 0.118 Uiso 1 1 calc GR . . . .
H11I H 0.040375 0.793308 0.470049 0.118 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 U1 3.4346(3) 3_565 ?
U1 K1 4.0214(9) . ?
U1 K1 4.2985(9) 3_565 ?
U1 O4 2.154(2) . ?
U1 O4 2.127(2) 3_565 ?
U1 O2 2.178(2) . ?
U1 O1 2.206(2) . ?
U1 O3 2.231(2) . ?
K1 O4 2.532(2) . ?
K1 O3 3.270(3) . ?
K1 C120 3.415(4) 3_565 ?
K1 C226 3.207(3) 3_565 ?
K1 C125 3.253(4) 3_565 ?
K1 C121 3.389(4) 3_565 ?
K1 C224 3.442(4) 3_565 ?
K1 C225 3.006(4) 3_565 ?
K1 C122 3.247(4) 3_565 ?
K1 C124 3.164(4) 3_565 ?
K1 C123 3.187(4) 3_565 ?
O2 B2 1.331(5) . ?
O1 B1 1.329(5) . ?
O3 B3 1.333(5) . ?
C230 C235 1.405(5) . ?
C230 C231 1.415(5) . ?
C230 B2 1.597(6) . ?
C120 C125 1.413(5) . ?
C120 C121 1.408(5) . ?
C120 B1 1.595(6) . ?
C235 C234 1.390(5) . ?
C235 C238 1.512(5) . ?
C226 C229 1.511(5) . ?
C226 C221 1.405(5) . ?
C226 C225 1.387(5) . ?
C221 C222 1.418(5) . ?
C221 B2 1.602(6) . ?
C234 C233 1.373(5) . ?
C222 C223 1.383(5) . ?
C222 C227 1.510(5) . ?
C125 C128 1.512(5) . ?
C125 C124 1.389(5) . ?
C332 C331 1.410(5) . ?
C332 C337 1.512(5) . ?
C332 C333 1.389(5) . ?
C331 C336 1.409(5) . ?
C331 B3 1.610(6) . ?
C121 C122 1.391(6) . ?
C121 C126 1.519(6) . ?
C224 C225 1.392(5) . ?
C224 C223 1.377(5) . ?
C224 C228 1.512(5) . ?
C111 C112 1.422(5) . ?
C111 B1 1.603(6) . ?
C111 C116 1.409(5) . ?
C340 C345 1.410(5) . ?
C340 C341 1.401(5) . ?
C340 B3 1.595(6) . ?
C333 C334 1.389(5) . ?
C345 C348 1.513(5) . ?
C345 C344 1.387(6) . ?
C334 C335 1.380(5) . ?
C334 C338 1.510(5) . ?
C335 C336 1.387(5) . ?
C231 C232 1.390(5) . ?
C231 C236 1.497(5) . ?
C112 C113 1.385(6) . ?
C112 C117 1.505(6) . ?
C122 C123 1.377(6) . ?
C233 C232 1.380(5) . ?
C233 C237 1.513(5) . ?
C116 C115 1.392(5) . ?
C116 C119 1.509(5) . ?
C336 C339 1.518(6) . ?
C341 C342 1.387(5) . ?
C341 C346 1.511(5) . ?
C342 C343 1.377(5) . ?
C124 C123 1.383(6) . ?
C123 C127 1.511(6) . ?
C113 C114 1.378(6) . ?
C114 C115 1.388(6) . ?
C114 C118 1.519(6) . ?
C343 C344 1.376(6) . ?
C343 C347 1.516(6) . ?

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
U1 U1 K1 61.470(14) 3_565 3_565 ?
U1 U1 K1 69.905(16) 3_565 . ?
K1 U1 K1 131.376(10) . 3_565 ?
O4 U1 U1 36.91(6) 3_565 3_565 ?
O4 U1 U1 36.38(6) . 3_565 ?
O4 U1 K1 24.87(6) 3_565 3_565 ?
O4 U1 K1 106.67(6) 3_565 . ?
O4 U1 K1 33.77(6) . . ?
O4 U1 K1 97.72(6) . 3_565 ?
O4 U1 O4 73.29(9) 3_565 . ?
O4 U1 O2 112.93(9) . . ?
O4 U1 O2 92.99(9) 3_565 . ?
O4 U1 O1 129.72(9) . . ?
O4 U1 O1 92.14(9) 3_565 . ?
O4 U1 O3 160.80(9) 3_565 . ?
O4 U1 O3 88.00(9) . . ?
O2 U1 U1 106.06(7) . 3_565 ?
O2 U1 K1 115.95(7) . . ?
O2 U1 K1 79.15(7) . 3_565 ?
O2 U1 O1 115.73(10) . . ?
O2 U1 O3 98.39(10) . . ?
O1 U1 U1 115.08(7) . 3_565 ?
O1 U1 K1 123.36(7) . . ?
O1 U1 K1 79.87(7) . 3_565 ?
O1 U1 O3 96.72(9) . . ?
O3 U1 U1 124.26(7) . 3_565 ?
O3 U1 K1 174.27(7) . 3_565 ?
O3 U1 K1 54.36(7) . . ?
O4 K1 U1 28.22(5) . . ?
O4 K1 O3 61.81(7) . . ?
O4 K1 C120 74.37(8) . 3_565 ?
O4 K1 C226 80.96(8) . 3_565 ?
O4 K1 C125 76.60(9) . 3_565 ?
O4 K1 C121 93.80(9) . 3_565 ?
O4 K1 C224 121.71(9) . 3_565 ?
O4 K1 C225 105.75(9) . 3_565 ?
O4 K1 C122 116.66(10) . 3_565 ?
O4 K1 C124 99.20(9) . 3_565 ?
O4 K1 C123 120.78(10) . 3_565 ?
O3 K1 U1 33.68(4) . . ?
O3 K1 C120 118.04(8) . 3_565 ?
O3 K1 C121 141.55(8) . 3_565 ?
O3 K1 C224 126.48(8) . 3_565 ?
C120 K1 U1 95.87(6) 3_565 . ?
C120 K1 C224 113.06(9) 3_565 3_565 ?
C226 K1 U1 87.10(6) 3_565 . ?
C226 K1 O3 98.16(8) 3_565 . ?
C226 K1 C120 116.49(9) 3_565 3_565 ?
C226 K1 C125 139.39(10) 3_565 3_565 ?
C226 K1 C121 107.26(10) 3_565 3_565 ?
C226 K1 C224 42.64(9) 3_565 3_565 ?
C226 K1 C122 116.16(11) 3_565 3_565 ?
C125 K1 U1 88.70(7) 3_565 . ?
C125 K1 O3 100.35(8) 3_565 . ?
C125 K1 C120 24.30(9) 3_565 3_565 ?
C125 K1 C121 42.38(9) 3_565 3_565 ?
C125 K1 C224 133.16(10) 3_565 3_565 ?
C121 K1 U1 118.43(7) 3_565 . ?
C121 K1 C120 23.88(8) 3_565 3_565 ?
C121 K1 C224 91.19(9) 3_565 3_565 ?
C224 K1 U1 128.80(6) 3_565 . ?
C225 K1 U1 106.05(7) 3_565 . ?
C225 K1 O3 104.46(9) 3_565 . ?
C225 K1 C120 129.16(10) 3_565 3_565 ?
C225 K1 C226 25.53(9) 3_565 3_565 ?
C225 K1 C125 152.88(11) 3_565 3_565 ?
C225 K1 C121 110.96(10) 3_565 3_565 ?
C225 K1 C224 23.71(9) 3_565 3_565 ?
C225 K1 C122 108.70(11) 3_565 3_565 ?
C225 K1 C124 149.72(11) 3_565 3_565 ?
C225 K1 C123 124.63(11) 3_565 3_565 ?
C122 K1 U1 137.62(8) 3_565 . ?
C122 K1 O3 145.34(10) 3_565 . ?
C122 K1 C120 42.70(9) 3_565 3_565 ?
C122 K1 C125 50.18(10) 3_565 3_565 ?
C122 K1 C121 24.08(10) 3_565 3_565 ?
C122 K1 C224 85.30(10) 3_565 3_565 ?
C124 K1 U1 104.06(8) 3_565 . ?
C124 K1 O3 102.30(9) 3_565 . ?
C124 K1 C120 43.15(10) 3_565 3_565 ?
C124 K1 C226 156.83(11) 3_565 3_565 ?
C124 K1 C125 24.94(9) 3_565 3_565 ?
C124 K1 C121 49.58(10) 3_565 3_565 ?
C124 K1 C224 126.17(10) 3_565 3_565 ?
C124 K1 C122 43.10(11) 3_565 3_565 ?
C124 K1 C123 25.16(11) 3_565 3_565 ?
C123 K1 U1 129.21(9) 3_565 . ?
C123 K1 O3 122.50(10) 3_565 . ?
C123 K1 C120 50.91(10) 3_565 3_565 ?
C123 K1 C226 139.02(11) 3_565 3_565 ?
C123 K1 C125 44.29(10) 3_565 3_565 ?
C123 K1 C121 43.16(11) 3_565 3_565 ?
C123 K1 C224 101.32(11) 3_565 3_565 ?
C123 K1 C122 24.70(11) 3_565 3_565 ?
U1 O4 U1 106.71(9) 3_565 . ?
U1 O4 K1 134.45(10) 3_565 . ?
U1 O4 K1 118.01(10) . . ?
B2 O2 U1 163.0(3) . . ?
B1 O1 U1 151.8(3) . . ?
U1 O3 K1 91.97(8) . . ?
B3 O3 U1 172.2(3) . . ?
B3 O3 K1 95.9(2) . . ?
C235 C230 C231 118.0(3) . . ?
C235 C230 B2 120.6(3) . . ?
C231 C230 B2 121.4(3) . . ?
C125 C120 K1 71.4(2) . 3_565 ?
C125 C120 B1 122.8(3) . . ?
C121 C120 K1 77.0(2) . 3_565 ?
C121 C120 C125 117.0(3) . . ?
C121 C120 B1 120.2(3) . . ?
B1 C120 K1 123.3(2) . 3_565 ?
C230 C235 C238 121.9(3) . . ?
C234 C235 C230 119.8(3) . . ?
C234 C235 C238 118.3(3) . . ?
C229 C226 K1 96.3(2) . 3_565 ?
C221 C226 K1 105.3(2) . 3_565 ?
C221 C226 C229 121.6(3) . . ?
C225 C226 K1 69.11(19) . 3_565 ?
C225 C226 C229 117.5(3) . . ?
C225 C226 C221 120.8(3) . . ?
C226 C221 C222 117.1(3) . . ?
C226 C221 B2 122.1(3) . . ?
C222 C221 B2 120.5(3) . . ?
C233 C234 C235 122.4(4) . . ?
C221 C222 C227 120.9(3) . . ?
C223 C222 C221 120.3(4) . . ?
C223 C222 C227 118.8(3) . . ?
C120 C125 K1 84.3(2) . 3_565 ?
C120 C125 C128 120.3(3) . . ?
C128 C125 K1 112.9(2) . 3_565 ?
C124 C125 K1 73.9(2) . 3_565 ?
C124 C125 C120 120.4(4) . . ?
C124 C125 C128 119.4(4) . . ?
C331 C332 C337 122.5(3) . . ?
C333 C332 C331 120.6(3) . . ?
C333 C332 C337 116.9(3) . . ?
C332 C331 B3 121.0(3) . . ?
C336 C331 C332 117.3(3) . . ?
C336 C331 B3 121.7(3) . . ?
C120 C121 K1 79.1(2) . 3_565 ?
C120 C121 C126 120.0(4) . . ?
C122 C121 K1 72.2(2) . 3_565 ?
C122 C121 C120 120.5(4) . . ?
C122 C121 C126 119.4(4) . . ?
C126 C121 K1 119.4(3) . 3_565 ?
C225 C224 K1 60.3(2) . 3_565 ?
C225 C224 C228 121.5(4) . . ?
C223 C224 K1 103.7(2) . 3_565 ?
C223 C224 C225 117.4(4) . . ?
C223 C224 C228 121.2(4) . . ?
C228 C224 K1 104.5(3) . 3_565 ?
C226 C225 K1 85.4(2) . 3_565 ?
C226 C225 C224 121.8(4) . . ?
C224 C225 K1 96.0(2) . 3_565 ?
C112 C111 B1 122.7(4) . . ?
C116 C111 C112 117.2(4) . . ?
C116 C111 B1 120.1(3) . . ?
C345 C340 B3 122.4(3) . . ?
C341 C340 C345 116.8(3) . . ?
C341 C340 B3 120.8(3) . . ?
C334 C333 C332 122.1(4) . . ?
C340 C345 C348 121.4(4) . . ?
C344 C345 C340 120.5(4) . . ?
C344 C345 C348 118.0(4) . . ?
C333 C334 C338 121.1(4) . . ?
C335 C334 C333 116.9(4) . . ?
C335 C334 C338 122.0(4) . . ?
C224 C223 C222 122.6(4) . . ?
C334 C335 C336 122.9(4) . . ?
C230 C231 C236 120.7(3) . . ?
C232 C231 C230 119.7(3) . . ?
C232 C231 C236 119.5(3) . . ?
C111 C112 C117 123.0(4) . . ?
C113 C112 C111 120.2(4) . . ?
C113 C112 C117 116.7(4) . . ?
O1 B1 C120 118.8(3) . . ?
O1 B1 C111 120.4(4) . . ?
C120 B1 C111 120.8(3) . . ?
C121 C122 K1 83.7(2) . 3_565 ?
C123 C122 K1 75.2(2) . 3_565 ?
C123 C122 C121 122.4(4) . . ?
C234 C233 C232 117.9(4) . . ?
C234 C233 C237 120.5(4) . . ?
C232 C233 C237 121.6(4) . . ?
C111 C116 C119 122.5(4) . . ?
C115 C116 C111 120.5(4) . . ?
C115 C116 C119 116.9(4) . . ?
C331 C336 C339 121.5(4) . . ?
C335 C336 C331 120.1(4) . . ?
C335 C336 C339 118.2(4) . . ?
C340 C341 C346 121.0(3) . . ?
C342 C341 C340 121.0(3) . . ?
C342 C341 C346 117.9(3) . . ?
O2 B2 C230 119.4(4) . . ?
O2 B2 C221 117.8(4) . . ?
C230 B2 C221 122.8(3) . . ?
C343 C342 C341 121.8(4) . . ?
C125 C124 K1 81.1(2) . 3_565 ?
C123 C124 K1 78.3(2) . 3_565 ?
C123 C124 C125 122.4(4) . . ?
C122 C123 K1 80.1(2) . 3_565 ?
C122 C123 C124 117.2(4) . . ?
C122 C123 C127 121.1(4) . . ?
C124 C123 K1 76.5(2) . 3_565 ?
C124 C123 C127 121.7(4) . . ?
C127 C123 K1 114.3(3) . 3_565 ?
C114 C113 C112 122.4(4) . . ?
C233 C232 C231 122.1(4) . . ?
C113 C114 C115 117.8(4) . . ?
C113 C114 C118 121.0(4) . . ?
C115 C114 C118 121.2(5) . . ?
C342 C343 C347 120.7(4) . . ?
C344 C343 C342 117.7(4) . . ?
C344 C343 C347 121.6(4) . . ?
C343 C344 C345 122.1(4) . . ?
C114 C115 C116 121.8(4) . . ?
O3 B3 C331 121.0(4) . . ?
O3 B3 C340 118.9(4) . . ?
C340 B3 C331 120.1(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.252 0.143 0.199 217.3 48.0 ?
2 0.248 0.357 0.699 217.3 47.8 ?
3 -0.248 0.643 0.301 217.3 48.6 ?
4 0.252 0.857 0.801 217.3 48.4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.932

# start Validation Reply Form
_vrf_PLAT910_p18089              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         13 Note  
RESPONSE: No. of reflections / No. of parameters = 17.4 Therefore
this is not seen as a serious problem.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p18047
_database_code_depnum_ccdc_archive 'CCDC 1886806'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C90 H96 B3 O5 P2 U), 0.5(C72 H88 B5 O6 U)'
_chemical_formula_sum            'C81 H92 B4 O5.50 P U'
_chemical_formula_weight         1465.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H200 B3 O3 P2 U2'
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'
B B 0.0013 0.0007 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.2121(4)
_cell_length_b                   23.0300(4)
_cell_length_c                   23.4449(6)
_cell_angle_alpha                72.304(2)
_cell_angle_beta                 80.146(2)
_cell_angle_gamma                70.091(2)
_cell_volume                     8300.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.3100
_cell_measurement_theta_min      3.0020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2996
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 13 3 0.0394
18 -13 -3 0.0394
-10 -21 -30 0.0651
0 1 -31 0.0673
14 30 17 0.0724
4 8 33 0.0714
-13 -29 3 0.0736

_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.079
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.9847 12.9952 2.9999 0.8304 0.5835 -0.0502
17.9847 -12.9952 -2.9999 -0.8304 -0.5835 0.0502
-9.9748 -20.9355 -30.0237 0.2230 -0.4057 0.8845
0.0361 1.0721 -30.9541 -0.1365 0.2507 0.9544
13.9937 29.9678 17.0696 -0.4230 0.7632 -0.4690
3.9657 7.9254 32.9791 0.0043 0.0019 -0.9997
-13.0164 -29.0139 2.9063 0.4737 -0.8787 -0.1440

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            190436
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.838
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00   4.00   0.70   15.00    --  -24.72 -77.00 120.00  140
  2  ω    -53.00  42.90   0.70   15.00    --  -24.72  77.00-120.00  137
  3  ω      1.00  85.00   0.70   15.00    --   26.28-131.00  14.37  120
  4  ω    -43.00  55.00   0.70   15.00    --   26.28 -77.00  60.00  140
  5  ω     -2.00  93.90   0.70   15.00    --   26.28  77.00-180.00  137
  6  ω     32.00  99.90   0.70   15.00    --   26.28-179.00  90.00   97
  7  ω    -45.00  95.70   0.70   15.00    --   26.28   0.00 -90.00  201
  8  ω    -99.00 -35.30   0.70   15.00    --  -24.72-179.00  60.00   91
  9  ω    -93.00  -7.60   0.70   15.00    --  -24.72 -57.00   0.00  122
 10  ω    -94.00   4.00   0.70   15.00    --  -24.72 -77.00 -90.00  140
 11  ω    -89.00  -8.50   0.70   15.00    --  -24.72 140.00 122.57  115
 12  ω    -99.00 -35.30   0.70   15.00    --  -24.72-179.00   0.00   91
 13  ω      4.00  95.70   0.70   15.00    --   26.28  37.00   0.00  131
 14  ω     -2.00  48.40   0.70   15.00    --   26.28  77.00  30.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0429682000
_diffrn_orient_matrix_UB_12      0.0033995000
_diffrn_orient_matrix_UB_13      0.0044789000
_diffrn_orient_matrix_UB_21      -0.0092280000
_diffrn_orient_matrix_UB_22      0.0337302000
_diffrn_orient_matrix_UB_23      -0.0069401000
_diffrn_orient_matrix_UB_31      -0.0007381000
_diffrn_orient_matrix_UB_32      0.0022140000
_diffrn_orient_matrix_UB_33      -0.0307577000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                21884
_reflns_number_total             33893
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1708
_refine_ls_number_reflns         33893
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      0.999
_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)+(0.0454P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1226
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C452(H452), C448(H448), C450(H450), C568(H568), C93(H93), C663(H663),
 C232(H232), C446(H446), C451(H451), C449(H449), C552(H552), C558(H558),
 C458(H458), C564(H564), C442(H442), C234(H234), C124(H124), C562(H562),
 C556(H556), C775(H775), C444(H444), C454(H454), C567(H567), C113(H113),
 C115(H115), C95(H95), C443(H443), C894(H894), C773(H773), C672(H672),
 C554(H554), C333(H333), C555(H555), C885(H885), C122(H122), C883(H883),
 C782(H782), C445(H445), C553(H553), C565(H565), C566(H566), C335(H335),
 C223(H223), C457(H457), C561(H561), C455(H455), C225(H225), C674(H674),
 C559(H559), C784(H784), C665(H665), C105(H105), C456(H456), C892(H892),
 C560(H560), C103(H103), C342(H342), C344(H344)
2.b Idealised Me refined as rotating group:
 C779(H77A,H77B,H77C), C119(H11A,H11B,H11C), C667(H66A,H66B,H66C), C339(H33A,
 H33B,H33C), C117(H11D,H11E,H11F), C788(H78A,H78B,H78C), C898(H89A,H89B,H89C),
 C669(H66D,H66E,H66F), C777(H77D,H77E,H77F), C97(H97A,H97B,H97C), C237(H23A,
 H23B,H23C), C238(H23D,H23E,H23F), C98(H98A,H98B,H98C), C676(H67A,H67B,H67C),
 C896(H89D,H89E,H89F), C227(H22A,H22B,H22C), C786(H78D,H78E,H78F), C678(H67D,
 H67E,H67F), C229(H22D,H22E,H22F), C126(H12A,H12B,H12C), C128(H12D,H12E,H12F),
 C99(H99A,H99B,H99C), C887(H88A,H88B,H88C), C889(H88D,H88E,H88F), C348(H34A,
 H34B,H34C), C668(H66G,H66H,H66I), C888(H88G,H88H,H88I), C337(H33D,H33E,H33F),
 C778(H77G,H77H,H77I), C127(H12G,H12H,H12I), C346(H34D,H34E,H34F), C228(H22G,
 H22H,H22I), C677(H67G,H67H,H67I), C118(H11G,H11H,H11I), C897(H89G,H89H,H89I),
 C338(H33G,H33H,H33I), C109(H10A,H10B,H10C), C107(H10D,H10E,H10F), C108(H10G,
 H10H,H10I), C787(H78G,H78H,H78I), C347(H34G,H34H,H34I), C236(H23G,H23H,H23I)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.16128(2) 0.56143(2) 0.25849(2) 0.02388(6) Uani 1 1 d . . . . .
U2 U 0.29149(2) 0.03649(2) 0.22980(2) 0.03054(7) Uani 1 1 d . . . . .
P4 P 0.06760(9) 0.74017(7) 0.19569(7) 0.0265(3) Uani 1 1 d . . . . .
P5 P 0.26024(9) 0.38403(7) 0.32131(7) 0.0289(4) Uani 1 1 d . . . . .
O3 O 0.2400(3) 0.55473(19) 0.17928(17) 0.0422(11) Uani 1 1 d . . . . .
O1 O 0.0430(2) 0.54955(19) 0.26398(19) 0.0410(11) Uani 1 1 d . . . . .
O5 O 0.2123(2) 0.45388(17) 0.29784(17) 0.0341(10) Uani 1 1 d . . . . .
O4 O 0.1037(2) 0.66789(17) 0.21769(16) 0.0306(9) Uani 1 1 d . . . . .
O7 O 0.3719(2) -0.06191(19) 0.25201(17) 0.0394(11) Uani 1 1 d . . . . .
O6 O 0.1973(2) 0.03182(19) 0.30358(18) 0.0399(10) Uani 1 1 d . . . . .
O8 O 0.3887(2) 0.06926(19) 0.24597(18) 0.0404(11) Uani 1 1 d . . . . .
O2 O 0.2014(2) 0.57639(19) 0.33259(17) 0.0378(10) Uani 1 1 d . . . . .
O10 O 0.1618(3) 0.1166(2) 0.10325(19) 0.0511(13) Uani 1 1 d . . . . .
O11 O 0.2259(3) 0.1326(2) 0.1773(2) 0.0528(13) Uani 1 1 d . . . . .
O9 O 0.2468(3) 0.0166(2) 0.1578(2) 0.0614(14) Uani 1 1 d . . . . .
C447 C -0.0198(3) 0.7669(3) 0.2448(2) 0.0288(13) Uani 1 1 d . . . . .
C230 C 0.1699(3) 0.6534(3) 0.3969(2) 0.0276(13) Uani 1 1 d . . . . .
C452 C -0.0323(4) 0.8185(3) 0.2675(3) 0.0378(15) Uani 1 1 d . . . . .
H452 H 0.006378 0.840674 0.257140 0.045 Uiso 1 1 calc R . . . .
C551 C 0.2305(3) 0.3563(3) 0.3992(3) 0.0308(14) Uani 1 1 d . . . . .
C448 C -0.0792(3) 0.7348(3) 0.2614(3) 0.0339(14) Uani 1 1 d . . . . .
H448 H -0.072472 0.699927 0.246821 0.041 Uiso 1 1 calc R . . . .
C771 C 0.4725(3) -0.1567(3) 0.3156(3) 0.0300(14) Uani 1 1 d . . . . .
C890 C 0.4441(4) 0.0834(3) 0.3337(3) 0.0409(16) Uani 1 1 d . . . . .
C557 C 0.3688(4) 0.3736(3) 0.3113(3) 0.0348(15) Uani 1 1 d . . . . .
C111 C -0.0364(3) 0.4709(3) 0.3054(3) 0.0327(14) Uani 1 1 d . . . . .
C235 C 0.2103(3) 0.6945(3) 0.4043(2) 0.0307(14) Uani 1 1 d . . . . .
C780 C 0.4629(4) -0.1430(3) 0.1958(3) 0.0388(16) Uani 1 1 d . . . . .
C450 C -0.1583(4) 0.8051(3) 0.3214(3) 0.0396(16) Uani 1 1 d . . . . .
H450 H -0.204258 0.817464 0.347344 0.047 Uiso 1 1 calc R . . . .
C441 C 0.1419(3) 0.7781(3) 0.1956(3) 0.0304(14) Uani 1 1 d . . . . .
C661 C 0.1460(3) 0.0521(3) 0.4051(3) 0.0352(15) Uani 1 1 d . . . . .
C453 C 0.0328(4) 0.7635(3) 0.1220(3) 0.0308(14) Uani 1 1 d . . . . .
C331 C 0.3315(4) 0.4885(3) 0.1103(3) 0.0416(16) Uani 1 1 d . . . . .
C563 C 0.2413(3) 0.3369(3) 0.2810(2) 0.0307(14) Uani 1 1 d . . . . .
C670 C 0.0464(4) 0.0395(3) 0.3296(3) 0.0387(15) Uani 1 1 d . . . . .
C881 C 0.5462(4) 0.0399(3) 0.2404(3) 0.0372(15) Uani 1 1 d . . . . .
C101 C 0.1181(4) 0.2277(3) 0.1146(3) 0.0406(16) Uani 1 1 d . . . . .
C92 C 0.2247(4) -0.0045(3) 0.0290(3) 0.0397(16) Uani 1 1 d . . . . .
C91 C 0.1700(4) 0.0166(3) 0.0757(3) 0.0409(16) Uani 1 1 d . . . . .
C568 C 0.3029(4) 0.2834(3) 0.2686(3) 0.0409(16) Uani 1 1 d . . . . .
H568 H 0.355563 0.272029 0.281499 0.049 Uiso 1 1 calc R . . . .
C675 C -0.0271(4) 0.0889(3) 0.3360(3) 0.0391(16) Uani 1 1 d . . . . .
C120 C -0.0991(4) 0.5948(3) 0.2277(3) 0.0353(15) Uani 1 1 d . . . . .
C221 C 0.2918(4) 0.5352(3) 0.4214(3) 0.0349(15) Uani 1 1 d . . . . .
C93 C 0.2030(4) -0.0390(3) -0.0020(3) 0.0452(17) Uani 1 1 d . . . . .
H93 H 0.239437 -0.052572 -0.032948 0.054 Uiso 1 1 calc R . . . .
C125 C -0.1772(4) 0.6214(3) 0.2555(3) 0.0366(15) Uani 1 1 d . . . . .
C891 C 0.4706(4) 0.1328(3) 0.3381(3) 0.0467(17) Uani 1 1 d . . . . .
C776 C 0.4236(4) -0.1721(3) 0.3687(3) 0.0367(15) Uani 1 1 d . . . . .
C779 C 0.3299(4) -0.1451(3) 0.3702(3) 0.0444(17) Uani 1 1 d . . . . .
H77A H 0.312876 -0.101952 0.373588 0.067 Uiso 1 1 calc GR . . . .
H77B H 0.305896 -0.170910 0.404051 0.067 Uiso 1 1 calc GR . . . .
H77C H 0.311540 -0.145400 0.333882 0.067 Uiso 1 1 calc GR . . . .
C663 C 0.1911(4) 0.1089(3) 0.4581(3) 0.0437(17) Uani 1 1 d . . . . .
H663 H 0.210716 0.142195 0.457173 0.052 Uiso 1 1 calc R . . . .
C116 C -0.0139(3) 0.4468(3) 0.3651(3) 0.0349(15) Uani 1 1 d . . . . .
C231 C 0.0829(4) 0.6724(3) 0.4041(3) 0.0322(14) Uani 1 1 d . . . . .
C232 C 0.0390(4) 0.7299(3) 0.4187(3) 0.0362(15) Uani 1 1 d . . . . .
H232 H -0.018445 0.740850 0.425051 0.043 Uiso 1 1 calc R . . . .
C446 C 0.1758(4) 0.7663(3) 0.2497(3) 0.0380(15) Uani 1 1 d . . . . .
H446 H 0.161017 0.737888 0.284079 0.046 Uiso 1 1 calc R . . . .
C666 C 0.1302(4) 0.0112(3) 0.4614(3) 0.0406(16) Uani 1 1 d . . . . .
C662 C 0.1765(4) 0.1018(3) 0.4044(3) 0.0380(15) Uani 1 1 d . . . . .
C112 C -0.0558(4) 0.4288(3) 0.2807(3) 0.0420(16) Uani 1 1 d . . . . .
C451 C -0.1013(4) 0.8378(3) 0.3055(3) 0.0456(17) Uani 1 1 d . . . . .
H451 H -0.108931 0.872823 0.320139 0.055 Uiso 1 1 calc R . . . .
C772 C 0.5595(4) -0.1821(3) 0.3183(3) 0.0419(16) Uani 1 1 d . . . . .
C336 C 0.2854(4) 0.4478(3) 0.1141(3) 0.0432(17) Uani 1 1 d . . . . .
C781 C 0.4722(4) -0.2067(4) 0.1979(3) 0.0494(19) Uani 1 1 d . . . . .
B8 B 0.4560(4) 0.0641(3) 0.2725(3) 0.0374(18) Uani 1 1 d . . . . .
C882 C 0.5652(4) 0.0625(3) 0.1798(3) 0.0469(17) Uani 1 1 d . . . . .
C449 C -0.1477(4) 0.7542(3) 0.2991(3) 0.0437(17) Uani 1 1 d . . . . .
H449 H -0.186981 0.732608 0.309590 0.052 Uiso 1 1 calc R . . . .
C96 C 0.0951(4) 0.0025(4) 0.0881(3) 0.0511(19) Uani 1 1 d . . . . .
C119 C 0.0068(4) 0.4879(3) 0.3969(3) 0.0464(17) Uani 1 1 d . . . . .
H11A H 0.061906 0.490139 0.383478 0.070 Uiso 1 1 calc GR . . . .
H11B H 0.003672 0.469072 0.439483 0.070 Uiso 1 1 calc GR . . . .
H11C H -0.031962 0.530216 0.387766 0.070 Uiso 1 1 calc GR . . . .
C233 C 0.0788(4) 0.7714(3) 0.4242(3) 0.0395(16) Uani 1 1 d . . . . .
C552 C 0.2157(4) 0.2982(3) 0.4235(3) 0.0436(16) Uani 1 1 d . . . . .
H552 H 0.221063 0.271779 0.399033 0.052 Uiso 1 1 calc R . . . .
C667 C 0.1957(4) 0.1476(3) 0.3463(3) 0.0479(18) Uani 1 1 d . . . . .
H66A H 0.253319 0.132286 0.333459 0.072 Uiso 1 1 calc GR . . . .
H66B H 0.183516 0.189222 0.352371 0.072 Uiso 1 1 calc GR . . . .
H66C H 0.162500 0.150171 0.316046 0.072 Uiso 1 1 calc GR . . . .
C339 C 0.1927(4) 0.4681(3) 0.1252(3) 0.0535(19) Uani 1 1 d . . . . .
H33A H 0.177900 0.465805 0.167068 0.080 Uiso 1 1 calc GR . . . .
H33B H 0.171082 0.440129 0.113975 0.080 Uiso 1 1 calc GR . . . .
H33C H 0.169766 0.511254 0.101782 0.080 Uiso 1 1 calc GR . . . .
B2 B 0.2200(4) 0.5881(3) 0.3806(3) 0.0294(16) Uani 1 1 d . . . . .
C886 C 0.6112(4) -0.0099(3) 0.2745(3) 0.0395(16) Uani 1 1 d . . . . .
C558 C 0.4036(4) 0.3945(3) 0.2554(3) 0.0511(19) Uani 1 1 d . . . . .
H558 H 0.371082 0.412538 0.222827 0.061 Uiso 1 1 calc R . . . .
C895 C 0.4083(4) 0.0487(3) 0.3865(3) 0.0416(16) Uani 1 1 d . . . . .
B3 B 0.2877(5) 0.5542(4) 0.1277(3) 0.0398(18) Uani 1 1 d . . . . .
C458 C -0.0403(4) 0.8131(3) 0.1065(3) 0.055(2) Uani 1 1 d . . . . .
H458 H -0.071775 0.834561 0.134638 0.066 Uiso 1 1 calc R . . . .
C671 C 0.0415(4) -0.0081(3) 0.3072(3) 0.0420(16) Uani 1 1 d . . . . .
C664 C 0.1773(4) 0.0683(3) 0.5123(3) 0.0429(17) Uani 1 1 d . . . . .
C564 C 0.1625(4) 0.3514(3) 0.2624(3) 0.0430(16) Uani 1 1 d . . . . .
H564 H 0.119777 0.385824 0.271272 0.052 Uiso 1 1 calc R . . . .
C442 C 0.1652(4) 0.8192(3) 0.1455(3) 0.0377(15) Uani 1 1 d . . . . .
H442 H 0.143079 0.827410 0.109330 0.045 Uiso 1 1 calc R . . . .
C234 C 0.1632(4) 0.7520(3) 0.4180(3) 0.0382(15) Uani 1 1 d . . . . .
H234 H 0.190801 0.778173 0.423269 0.046 Uiso 1 1 calc R . . . .
C102 C 0.1473(5) 0.2729(3) 0.0700(3) 0.0530(19) Uani 1 1 d . . . . .
C226 C 0.2775(4) 0.5159(3) 0.4841(3) 0.0425(16) Uani 1 1 d . . . . .
C124 C -0.2325(4) 0.6766(3) 0.2225(3) 0.0457(17) Uani 1 1 d . . . . .
H124 H -0.283983 0.694047 0.241003 0.055 Uiso 1 1 calc R . . . .
C94 C 0.1296(4) -0.0536(3) 0.0114(3) 0.0464(17) Uani 1 1 d . . . . .
C562 C 0.4184(4) 0.3451(3) 0.3595(3) 0.0480(18) Uani 1 1 d . . . . .
H562 H 0.395448 0.330087 0.397803 0.058 Uiso 1 1 calc R . . . .
C556 C 0.2226(4) 0.3942(3) 0.4373(3) 0.0391(15) Uani 1 1 d . . . . .
H556 H 0.232737 0.433446 0.421674 0.047 Uiso 1 1 calc R . . . .
C775 C 0.4588(4) -0.2115(3) 0.4207(3) 0.0502(18) Uani 1 1 d . . . . .
H775 H 0.424570 -0.221293 0.455069 0.060 Uiso 1 1 calc R . . . .
C444 C 0.2541(4) 0.8382(3) 0.2007(3) 0.0420(17) Uani 1 1 d . . . . .
H444 H 0.291407 0.858713 0.202471 0.050 Uiso 1 1 calc R . . . .
C332 C 0.4172(4) 0.4685(3) 0.0947(3) 0.0458(17) Uani 1 1 d . . . . .
C785 C 0.4788(4) -0.1022(4) 0.1406(3) 0.054(2) Uani 1 1 d . . . . .
C454 C 0.0784(4) 0.7316(3) 0.0801(3) 0.0502(18) Uani 1 1 d . . . . .
H454 H 0.127780 0.698929 0.089458 0.060 Uiso 1 1 calc R . . . .
C117 C -0.0798(5) 0.4502(3) 0.2172(3) 0.064(2) Uani 1 1 d . . . . .
H11D H -0.126497 0.488421 0.212155 0.095 Uiso 1 1 calc GR . . . .
H11E H -0.094268 0.417090 0.208709 0.095 Uiso 1 1 calc GR . . . .
H11F H -0.034051 0.458833 0.190105 0.095 Uiso 1 1 calc GR . . . .
C222 C 0.3715(4) 0.5103(3) 0.3953(3) 0.0468(18) Uani 1 1 d . . . . .
C345 C 0.3261(5) 0.6591(4) 0.1135(4) 0.066(2) Uani 1 1 d . . . . .
B6 B 0.1324(4) 0.0414(3) 0.3443(3) 0.0330(16) Uani 1 1 d . . . . .
C567 C 0.2866(4) 0.2470(3) 0.2374(3) 0.0476(18) Uani 1 1 d . . . . .
H567 H 0.328140 0.211592 0.229274 0.057 Uiso 1 1 calc R . . . .
C788 C 0.4726(5) -0.0328(4) 0.1329(3) 0.072(2) Uani 1 1 d . . . . .
H78A H 0.416010 -0.006468 0.128256 0.108 Uiso 1 1 calc GR . . . .
H78B H 0.506530 -0.018835 0.097861 0.108 Uiso 1 1 calc GR . . . .
H78C H 0.491305 -0.029293 0.167609 0.108 Uiso 1 1 calc GR . . . .
B10 B 0.1729(5) 0.1553(4) 0.1343(3) 0.0430(19) Uani 1 1 d . . . . .
C884 C 0.7045(4) -0.0108(3) 0.1858(3) 0.0525(19) Uani 1 1 d . . . . .
C113 C -0.0517(4) 0.3674(3) 0.3153(3) 0.0497(18) Uani 1 1 d . . . . .
H113 H -0.065005 0.340629 0.298391 0.060 Uiso 1 1 calc R . . . .
C898 C 0.3790(4) -0.0059(3) 0.3861(3) 0.0522(19) Uani 1 1 d . . . . .
H89A H 0.321377 0.010091 0.378631 0.078 Uiso 1 1 calc GR . . . .
H89B H 0.386493 -0.037172 0.424275 0.078 Uiso 1 1 calc GR . . . .
H89C H 0.410529 -0.025354 0.355050 0.078 Uiso 1 1 calc GR . . . .
C115 C -0.0115(4) 0.3855(3) 0.3978(3) 0.0444(17) Uani 1 1 d . . . . .
H115 H 0.002381 0.371599 0.437441 0.053 Uiso 1 1 calc R . . . .
C95 C 0.0751(4) -0.0320(3) 0.0563(3) 0.0520(19) Uani 1 1 d . . . . .
H95 H 0.024682 -0.040556 0.065479 0.062 Uiso 1 1 calc R . . . .
C669 C 0.0993(4) -0.0438(3) 0.4653(3) 0.0520(19) Uani 1 1 d . . . . .
H66D H 0.046234 -0.027599 0.449031 0.078 Uiso 1 1 calc GR . . . .
H66E H 0.094250 -0.067341 0.506593 0.078 Uiso 1 1 calc GR . . . .
H66F H 0.137891 -0.071564 0.442909 0.078 Uiso 1 1 calc GR . . . .
C443 C 0.2221(4) 0.8488(3) 0.1485(3) 0.0451(17) Uani 1 1 d . . . . .
H443 H 0.238352 0.876201 0.113943 0.054 Uiso 1 1 calc R . . . .
C777 C 0.6174(4) -0.1671(3) 0.2642(3) 0.0537(19) Uani 1 1 d . . . . .
H77D H 0.614183 -0.187969 0.235310 0.081 Uiso 1 1 calc GR . . . .
H77E H 0.673106 -0.182206 0.276029 0.081 Uiso 1 1 calc GR . . . .
H77F H 0.601973 -0.121673 0.246730 0.081 Uiso 1 1 calc GR . . . .
C97 C 0.3067(5) 0.0094(4) 0.0135(3) 0.070(2) Uani 1 1 d . . . . .
H97A H 0.297687 0.053974 0.008970 0.106 Uiso 1 1 calc GR . . . .
H97B H 0.331839 -0.001159 -0.023383 0.106 Uiso 1 1 calc GR . . . .
H97C H 0.342760 -0.015946 0.045115 0.106 Uiso 1 1 calc GR . . . .
C894 C 0.4038(4) 0.0639(3) 0.4401(3) 0.0530(19) Uani 1 1 d . . . . .
H894 H 0.381943 0.040298 0.474858 0.064 Uiso 1 1 calc R . . . .
C773 C 0.5925(4) -0.2207(3) 0.3727(3) 0.054(2) Uani 1 1 d . . . . .
H773 H 0.649728 -0.235908 0.374552 0.064 Uiso 1 1 calc R . . . .
C672 C -0.0338(5) -0.0064(4) 0.2912(3) 0.0518(19) Uani 1 1 d . . . . .
H672 H -0.035424 -0.038944 0.276144 0.062 Uiso 1 1 calc R . . . .
C237 C 0.0307(4) 0.8330(3) 0.4400(3) 0.056(2) Uani 1 1 d . . . . .
H23A H 0.019684 0.867284 0.403938 0.085 Uiso 1 1 calc GR . . . .
H23B H 0.062468 0.841847 0.464465 0.085 Uiso 1 1 calc GR . . . .
H23C H -0.020688 0.829338 0.461812 0.085 Uiso 1 1 calc GR . . . .
C121 C -0.0818(4) 0.6231(3) 0.1676(3) 0.0439(17) Uani 1 1 d . . . . .
C554 C 0.1849(4) 0.3172(3) 0.5199(3) 0.0475(18) Uani 1 1 d . . . . .
H554 H 0.168705 0.304128 0.560506 0.057 Uiso 1 1 calc R . . . .
C238 C 0.3046(4) 0.6764(3) 0.3977(3) 0.0489(18) Uani 1 1 d . . . . .
H23D H 0.327467 0.635673 0.425349 0.073 Uiso 1 1 calc GR . . . .
H23E H 0.321416 0.708394 0.406309 0.073 Uiso 1 1 calc GR . . . .
H23F H 0.324169 0.673860 0.357434 0.073 Uiso 1 1 calc GR . . . .
C333 C 0.4541(5) 0.4076(4) 0.0855(3) 0.059(2) Uani 1 1 d . . . . .
H333 H 0.510801 0.394322 0.075210 0.071 Uiso 1 1 calc R . . . .
C98 C 0.1109(5) -0.0945(3) -0.0210(3) 0.063(2) Uani 1 1 d . . . . .
H98A H 0.131118 -0.083799 -0.062364 0.094 Uiso 1 1 calc GR . . . .
H98B H 0.052119 -0.086690 -0.018355 0.094 Uiso 1 1 calc GR . . . .
H98C H 0.137623 -0.138884 -0.002680 0.094 Uiso 1 1 calc GR . . . .
C676 C 0.1171(4) -0.0645(3) 0.2983(3) 0.0528(19) Uani 1 1 d . . . . .
H67A H 0.148898 -0.051029 0.261783 0.079 Uiso 1 1 calc GR . . . .
H67B H 0.098965 -0.098734 0.295804 0.079 Uiso 1 1 calc GR . . . .
H67C H 0.150788 -0.079244 0.331568 0.079 Uiso 1 1 calc GR . . . .
C123 C -0.2138(4) 0.7060(3) 0.1641(3) 0.0508(18) Uani 1 1 d . . . . .
C896 C 0.5125(4) 0.1698(3) 0.2833(3) 0.0533(19) Uani 1 1 d . . . . .
H89D H 0.567075 0.142876 0.274637 0.080 Uiso 1 1 calc GR . . . .
H89E H 0.516492 0.207055 0.291428 0.080 Uiso 1 1 calc GR . . . .
H89F H 0.480376 0.182643 0.249404 0.080 Uiso 1 1 calc GR . . . .
C555 C 0.2004(4) 0.3750(3) 0.4971(3) 0.0477(17) Uani 1 1 d . . . . .
H555 H 0.195745 0.400788 0.522116 0.057 Uiso 1 1 calc R . . . .
C885 C 0.6861(4) -0.0333(3) 0.2458(3) 0.0460(17) Uani 1 1 d . . . . .
H885 H 0.726836 -0.066184 0.268253 0.055 Uiso 1 1 calc R . . . .
C122 C -0.1384(4) 0.6783(3) 0.1362(3) 0.0540(19) Uani 1 1 d . . . . .
H122 H -0.125482 0.696666 0.096101 0.065 Uiso 1 1 calc R . . . .
C227 C 0.3924(4) 0.5286(4) 0.3287(4) 0.077(3) Uani 1 1 d . . . . .
H22A H 0.372699 0.504982 0.310152 0.115 Uiso 1 1 calc GR . . . .
H22B H 0.451436 0.518821 0.320753 0.115 Uiso 1 1 calc GR . . . .
H22C H 0.366552 0.573648 0.312731 0.115 Uiso 1 1 calc GR . . . .
C883 C 0.6436(4) 0.0380(3) 0.1521(3) 0.060(2) Uani 1 1 d . . . . .
H883 H 0.654826 0.054412 0.111265 0.072 Uiso 1 1 calc R . . . .
C786 C 0.4585(4) -0.2555(3) 0.2542(4) 0.063(2) Uani 1 1 d . . . . .
H78D H 0.504985 -0.270044 0.278021 0.094 Uiso 1 1 calc GR . . . .
H78E H 0.452663 -0.291187 0.244143 0.094 Uiso 1 1 calc GR . . . .
H78F H 0.409036 -0.236731 0.276572 0.094 Uiso 1 1 calc GR . . . .
C782 C 0.4941(4) -0.2252(4) 0.1451(4) 0.067(2) Uani 1 1 d . . . . .
H782 H 0.497415 -0.266798 0.146679 0.080 Uiso 1 1 calc R . . . .
C106 C 0.0387(5) 0.2487(3) 0.1398(3) 0.059(2) Uani 1 1 d . . . . .
C445 C 0.2305(4) 0.7964(3) 0.2519(3) 0.0473(18) Uani 1 1 d . . . . .
H445 H 0.252298 0.788858 0.288089 0.057 Uiso 1 1 calc R . . . .
C678 C -0.0292(4) 0.1439(3) 0.3596(3) 0.057(2) Uani 1 1 d . . . . .
H67D H -0.013588 0.127549 0.400254 0.086 Uiso 1 1 calc GR . . . .
H67E H -0.084195 0.173600 0.358516 0.086 Uiso 1 1 calc GR . . . .
H67F H 0.008862 0.165294 0.335103 0.086 Uiso 1 1 calc GR . . . .
B9 B 0.1950(5) 0.0511(4) 0.1145(3) 0.043(2) Uani 1 1 d . . . . .
B1 B -0.0296(4) 0.5388(3) 0.2655(3) 0.0342(17) Uani 1 1 d . . . . .
C553 C 0.1930(5) 0.2791(3) 0.4840(3) 0.057(2) Uani 1 1 d . . . . .
H553 H 0.183294 0.239734 0.500020 0.068 Uiso 1 1 calc R . . . .
C565 C 0.1477(4) 0.3151(3) 0.2310(3) 0.0525(19) Uani 1 1 d . . . . .
H565 H 0.095317 0.325910 0.217959 0.063 Uiso 1 1 calc R . . . .
B7 B 0.4333(4) -0.1166(3) 0.2542(3) 0.0346(17) Uani 1 1 d . . . . .
C229 C 0.1931(4) 0.5388(3) 0.5153(3) 0.061(2) Uani 1 1 d . . . . .
H22D H 0.179070 0.583832 0.511367 0.091 Uiso 1 1 calc GR . . . .
H22E H 0.193898 0.516038 0.557120 0.091 Uiso 1 1 calc GR . . . .
H22F H 0.152688 0.531051 0.497461 0.091 Uiso 1 1 calc GR . . . .
C341 C 0.2832(6) 0.6431(4) 0.0282(4) 0.074(3) Uani 1 1 d . . . . .
C114 C -0.0289(4) 0.3441(3) 0.3736(3) 0.0497(18) Uani 1 1 d . . . . .
C774 C 0.5429(5) -0.2369(3) 0.4233(4) 0.059(2) Uani 1 1 d . . . . .
C126 C -0.0010(4) 0.5951(3) 0.1328(3) 0.056(2) Uani 1 1 d . . . . .
H12A H 0.042212 0.608159 0.141150 0.084 Uiso 1 1 calc GR . . . .
H12B H -0.008420 0.610317 0.090553 0.084 Uiso 1 1 calc GR . . . .
H12C H 0.013784 0.549198 0.144826 0.084 Uiso 1 1 calc GR . . . .
C566 C 0.2091(4) 0.2635(3) 0.2187(3) 0.0460(17) Uani 1 1 d . . . . .
H566 H 0.198172 0.239408 0.197373 0.055 Uiso 1 1 calc R . . . .
C128 C -0.2009(4) 0.5938(3) 0.3199(3) 0.060(2) Uani 1 1 d . . . . .
H12D H -0.191251 0.548671 0.327181 0.090 Uiso 1 1 calc GR . . . .
H12E H -0.258471 0.614320 0.329023 0.090 Uiso 1 1 calc GR . . . .
H12F H -0.168038 0.600689 0.345022 0.090 Uiso 1 1 calc GR . . . .
C335 C 0.3257(5) 0.3874(3) 0.1045(3) 0.058(2) Uani 1 1 d . . . . .
H335 H 0.294698 0.360375 0.107231 0.070 Uiso 1 1 calc R . . . .
C223 C 0.4337(4) 0.4682(3) 0.4327(4) 0.061(2) Uani 1 1 d . . . . .
H223 H 0.486618 0.452056 0.415494 0.073 Uiso 1 1 calc R . . . .
C457 C -0.0656(5) 0.8302(4) 0.0495(4) 0.069(2) Uani 1 1 d . . . . .
H457 H -0.113479 0.864180 0.038805 0.083 Uiso 1 1 calc R . . . .
C561 C 0.5017(5) 0.3392(4) 0.3502(3) 0.069(2) Uani 1 1 d . . . . .
H561 H 0.535008 0.320629 0.382352 0.083 Uiso 1 1 calc R . . . .
C455 C 0.0491(6) 0.7491(4) 0.0234(3) 0.069(2) Uani 1 1 d . . . . .
H455 H 0.078330 0.726883 -0.004616 0.083 Uiso 1 1 calc R . . . .
C225 C 0.3417(5) 0.4733(3) 0.5187(3) 0.058(2) Uani 1 1 d . . . . .
H225 H 0.331305 0.460426 0.560141 0.069 Uiso 1 1 calc R . . . .
C674 C -0.1011(4) 0.0894(4) 0.3189(3) 0.059(2) Uani 1 1 d . . . . .
H674 H -0.148888 0.123084 0.322428 0.071 Uiso 1 1 calc R . . . .
C99 C 0.0347(5) 0.0247(5) 0.1381(3) 0.083(3) Uani 1 1 d . . . . .
H99A H 0.063514 0.013077 0.173477 0.125 Uiso 1 1 calc GR . . . .
H99B H -0.008246 0.004758 0.146664 0.125 Uiso 1 1 calc GR . . . .
H99C H 0.010478 0.070412 0.125794 0.125 Uiso 1 1 calc GR . . . .
C559 C 0.4863(4) 0.3890(4) 0.2468(3) 0.066(2) Uani 1 1 d . . . . .
H559 H 0.509309 0.404649 0.208709 0.079 Uiso 1 1 calc R . . . .
C887 C 0.5014(4) 0.1155(3) 0.1401(3) 0.062(2) Uani 1 1 d . . . . .
H88A H 0.467251 0.097221 0.127111 0.093 Uiso 1 1 calc GR . . . .
H88B H 0.529230 0.137489 0.105644 0.093 Uiso 1 1 calc GR . . . .
H88C H 0.467434 0.145188 0.162288 0.093 Uiso 1 1 calc GR . . . .
C784 C 0.5041(4) -0.1255(4) 0.0890(3) 0.067(2) Uani 1 1 d . . . . .
H784 H 0.516291 -0.098124 0.052813 0.080 Uiso 1 1 calc R . . . .
C889 C 0.6001(4) -0.0391(3) 0.3407(3) 0.056(2) Uani 1 1 d . . . . .
H88D H 0.587942 -0.006706 0.361656 0.084 Uiso 1 1 calc GR . . . .
H88E H 0.650154 -0.072289 0.354001 0.084 Uiso 1 1 calc GR . . . .
H88F H 0.555213 -0.056946 0.348895 0.084 Uiso 1 1 calc GR . . . .
C665 C 0.1464(4) 0.0201(3) 0.5134(3) 0.0483(18) Uani 1 1 d . . . . .
H665 H 0.136186 -0.007256 0.550147 0.058 Uiso 1 1 calc R . . . .
C224 C 0.4196(5) 0.4498(3) 0.4939(4) 0.068(3) Uani 1 1 d . . . . .
C348 C 0.3458(5) 0.6389(5) 0.1771(4) 0.092(3) Uani 1 1 d . . . . .
H34A H 0.380765 0.661535 0.181931 0.139 Uiso 1 1 calc GR . . . .
H34B H 0.373912 0.593651 0.188321 0.139 Uiso 1 1 calc GR . . . .
H34C H 0.295373 0.648288 0.202251 0.139 Uiso 1 1 calc GR . . . .
C105 C -0.0096(5) 0.3118(4) 0.1195(4) 0.066(2) Uani 1 1 d . . . . .
H105 H -0.063084 0.324729 0.137148 0.079 Uiso 1 1 calc R . . . .
C456 C -0.0215(6) 0.7981(4) 0.0086(3) 0.067(2) Uani 1 1 d . . . . .
H456 H -0.039550 0.809683 -0.029598 0.080 Uiso 1 1 calc R . . . .
C892 C 0.4609(4) 0.1473(4) 0.3927(4) 0.056(2) Uani 1 1 d . . . . .
H892 H 0.475667 0.182014 0.394352 0.068 Uiso 1 1 calc R . . . .
C668 C 0.1976(5) 0.0747(4) 0.5702(3) 0.066(2) Uani 1 1 d . . . . .
H66G H 0.254121 0.049920 0.577727 0.100 Uiso 1 1 calc GR . . . .
H66H H 0.161467 0.059374 0.602850 0.100 Uiso 1 1 calc GR . . . .
H66I H 0.190215 0.118899 0.566510 0.100 Uiso 1 1 calc GR . . . .
C888 C 0.7887(5) -0.0396(4) 0.1564(4) 0.090(3) Uani 1 1 d . . . . .
H88G H 0.820238 -0.010196 0.146869 0.135 Uiso 1 1 calc GR . . . .
H88H H 0.781667 -0.048003 0.120177 0.135 Uiso 1 1 calc GR . . . .
H88I H 0.817554 -0.078999 0.183393 0.135 Uiso 1 1 calc GR . . . .
C337 C 0.4721(5) 0.5096(4) 0.0882(4) 0.077(3) Uani 1 1 d . . . . .
H33D H 0.451164 0.549825 0.059299 0.116 Uiso 1 1 calc GR . . . .
H33E H 0.527453 0.488043 0.074834 0.116 Uiso 1 1 calc GR . . . .
H33F H 0.472622 0.516981 0.126233 0.116 Uiso 1 1 calc GR . . . .
C104 C 0.0179(6) 0.3553(4) 0.0750(3) 0.064(2) Uani 1 1 d . . . . .
C560 C 0.5352(4) 0.3605(4) 0.2941(4) 0.065(2) Uani 1 1 d . . . . .
H560 H 0.591609 0.355629 0.287871 0.078 Uiso 1 1 calc R . . . .
C334 C 0.4095(5) 0.3666(4) 0.0910(4) 0.064(2) Uani 1 1 d . . . . .
C103 C 0.0975(5) 0.3347(4) 0.0509(4) 0.072(2) Uani 1 1 d . . . . .
H103 H 0.118441 0.363676 0.020698 0.086 Uiso 1 1 calc R . . . .
C783 C 0.5112(5) -0.1863(6) 0.0906(4) 0.079(3) Uani 1 1 d . . . . .
C673 C -0.1056(5) 0.0418(4) 0.2972(3) 0.055(2) Uani 1 1 d . . . . .
C893 C 0.4304(5) 0.1123(4) 0.4438(3) 0.058(2) Uani 1 1 d . . . . .
C342 C 0.2945(6) 0.7027(4) -0.0060(4) 0.102(4) Uani 1 1 d . . . . .
H342 H 0.283065 0.717726 -0.046210 0.123 Uiso 1 1 calc R . . . .
C344 C 0.3371(5) 0.7153(5) 0.0769(6) 0.096(4) Uani 1 1 d . . . . .
H344 H 0.356419 0.739116 0.093631 0.115 Uiso 1 1 calc R . . . .
C778 C 0.5795(5) -0.2807(4) 0.4809(4) 0.086(3) Uani 1 1 d . . . . .
H77G H 0.537698 -0.277355 0.513598 0.129 Uiso 1 1 calc GR . . . .
H77H H 0.624503 -0.268702 0.487837 0.129 Uiso 1 1 calc GR . . . .
H77I H 0.599535 -0.324113 0.477850 0.129 Uiso 1 1 calc GR . . . .
C127 C -0.2733(5) 0.7680(4) 0.1298(4) 0.098(3) Uani 1 1 d . . . . .
H12G H -0.329194 0.766833 0.140562 0.146 Uiso 1 1 calc GR . . . .
H12H H -0.260878 0.772714 0.087422 0.146 Uiso 1 1 calc GR . . . .
H12I H -0.267217 0.803674 0.139739 0.146 Uiso 1 1 calc GR . . . .
C343 C 0.3218(6) 0.7386(4) 0.0184(6) 0.106(5) Uani 1 1 d . . . . .
C346 C 0.2495(7) 0.6068(4) -0.0014(3) 0.111(4) Uani 1 1 d . . . . .
H34D H 0.231559 0.633400 -0.040024 0.166 Uiso 1 1 calc GR . . . .
H34E H 0.203420 0.595702 0.023459 0.166 Uiso 1 1 calc GR . . . .
H34F H 0.292247 0.568495 -0.006044 0.166 Uiso 1 1 calc GR . . . .
C228 C 0.4906(5) 0.4054(4) 0.5335(4) 0.098(3) Uani 1 1 d . . . . .
H22G H 0.529427 0.376662 0.512182 0.147 Uiso 1 1 calc GR . . . .
H22H H 0.468519 0.381217 0.569733 0.147 Uiso 1 1 calc GR . . . .
H22I H 0.518044 0.430652 0.543386 0.147 Uiso 1 1 calc GR . . . .
C677 C -0.1866(5) 0.0448(4) 0.2774(4) 0.089(3) Uani 1 1 d . . . . .
H67G H -0.209279 0.085832 0.250113 0.134 Uiso 1 1 calc GR . . . .
H67H H -0.225027 0.038757 0.311887 0.134 Uiso 1 1 calc GR . . . .
H67I H -0.176756 0.011705 0.257734 0.134 Uiso 1 1 calc GR . . . .
C118 C -0.0227(5) 0.2766(3) 0.4091(3) 0.076(3) Uani 1 1 d . . . . .
H11G H -0.061732 0.277170 0.443663 0.115 Uiso 1 1 calc GR . . . .
H11H H 0.032390 0.254972 0.421912 0.115 Uiso 1 1 calc GR . . . .
H11I H -0.034723 0.254617 0.384575 0.115 Uiso 1 1 calc GR . . . .
C897 C 0.4223(6) 0.1267(4) 0.5032(4) 0.096(3) Uani 1 1 d . . . . .
H89G H 0.367336 0.154124 0.510026 0.144 Uiso 1 1 calc GR . . . .
H89H H 0.461901 0.147710 0.503032 0.144 Uiso 1 1 calc GR . . . .
H89I H 0.432448 0.087450 0.534649 0.144 Uiso 1 1 calc GR . . . .
C338 C 0.4515(6) 0.3003(4) 0.0812(5) 0.113(4) Uani 1 1 d . . . . .
H33G H 0.498410 0.301269 0.052496 0.169 Uiso 1 1 calc GR . . . .
H33H H 0.412971 0.287580 0.066329 0.169 Uiso 1 1 calc GR . . . .
H33I H 0.469704 0.270255 0.118534 0.169 Uiso 1 1 calc GR . . . .
C109 C 0.0060(6) 0.2027(5) 0.1912(5) 0.144(5) Uani 1 1 d . . . . .
H10A H -0.021515 0.181492 0.175531 0.216 Uiso 1 1 calc GR . . . .
H10B H -0.032572 0.225924 0.217344 0.216 Uiso 1 1 calc GR . . . .
H10C H 0.051225 0.171446 0.213193 0.216 Uiso 1 1 calc GR . . . .
C107 C 0.2351(5) 0.2523(4) 0.0413(4) 0.104(4) Uani 1 1 d . . . . .
H10D H 0.274033 0.238154 0.071241 0.156 Uiso 1 1 calc GR . . . .
H10E H 0.245326 0.287933 0.010341 0.156 Uiso 1 1 calc GR . . . .
H10F H 0.241357 0.217951 0.024105 0.156 Uiso 1 1 calc GR . . . .
C108 C -0.0366(6) 0.4234(4) 0.0533(4) 0.107(4) Uani 1 1 d . . . . .
H10G H -0.032417 0.436202 0.010236 0.160 Uiso 1 1 calc GR . . . .
H10H H -0.019003 0.451070 0.068145 0.160 Uiso 1 1 calc GR . . . .
H10I H -0.093028 0.426129 0.067829 0.160 Uiso 1 1 calc GR . . . .
C787 C 0.5398(6) -0.2121(5) 0.0353(4) 0.117(4) Uani 1 1 d . . . . .
H78G H 0.585112 -0.250999 0.044476 0.176 Uiso 1 1 calc GR . . . .
H78H H 0.557594 -0.180931 0.002977 0.176 Uiso 1 1 calc GR . . . .
H78I H 0.494799 -0.220522 0.023579 0.176 Uiso 1 1 calc GR . . . .
C347 C 0.3338(6) 0.8023(4) -0.0196(6) 0.157(6) Uani 1 1 d . . . . .
H34G H 0.376631 0.794726 -0.051012 0.235 Uiso 1 1 calc GR . . . .
H34H H 0.349358 0.822113 0.005359 0.235 Uiso 1 1 calc GR . . . .
H34I H 0.282953 0.829962 -0.036880 0.235 Uiso 1 1 calc GR . . . .
C236 C 0.0341(4) 0.6313(3) 0.3989(3) 0.0464(17) Uani 1 1 d . . . . .
H23G H 0.024841 0.639562 0.357570 0.070 Uiso 1 1 calc GR . . . .
H23H H -0.018286 0.641051 0.421897 0.070 Uiso 1 1 calc GR . . . .
H23I H 0.064469 0.586917 0.414032 0.070 Uiso 1 1 calc GR . . . .
C340 C 0.2994(4) 0.6207(3) 0.0879(3) 0.0521(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O3 2.116(4) . ?
U1 O1 2.122(4) . ?
U1 O5 2.272(4) . ?
U1 O4 2.270(4) . ?
U1 O2 2.133(4) . ?
U2 O7 2.172(4) . ?
U2 O6 2.162(4) . ?
U2 O8 2.183(4) . ?
U2 O11 2.193(4) . ?
U2 O9 2.192(4) . ?
P4 O4 1.519(4) . ?
P4 C447 1.781(6) . ?
P4 C441 1.777(6) . ?
P4 C453 1.790(6) . ?
P5 O5 1.511(4) . ?
P5 C551 1.788(6) . ?
P5 C557 1.785(6) . ?
P5 C563 1.775(6) . ?
O3 B3 1.341(8) . ?
O1 B1 1.347(7) . ?
O7 B7 1.334(8) . ?
O6 B6 1.343(7) . ?
O8 B8 1.360(7) . ?
O2 B2 1.346(7) . ?
O10 B10 1.387(8) . ?
O10 B9 1.376(9) . ?
O11 B10 1.338(8) . ?
O9 B9 1.340(8) . ?
C447 C452 1.385(8) . ?
C447 C448 1.395(7) . ?
C230 C235 1.415(7) . ?
C230 C231 1.404(7) . ?
C230 B2 1.582(8) . ?
C452 H452 0.9300 . ?
C452 C451 1.386(8) . ?
C551 C552 1.378(8) . ?
C551 C556 1.388(8) . ?
C448 H448 0.9300 . ?
C448 C449 1.378(8) . ?
C771 C776 1.400(8) . ?
C771 C772 1.416(8) . ?
C771 B7 1.575(9) . ?
C890 C891 1.398(8) . ?
C890 B8 1.587(10) . ?
C890 C895 1.423(9) . ?
C557 C558 1.360(8) . ?
C557 C562 1.390(8) . ?
C111 C116 1.408(8) . ?
C111 C112 1.421(8) . ?
C111 B1 1.590(9) . ?
C235 C234 1.397(8) . ?
C235 C238 1.524(8) . ?
C780 C781 1.407(9) . ?
C780 C785 1.396(9) . ?
C780 B7 1.598(9) . ?
C450 H450 0.9300 . ?
C450 C451 1.369(8) . ?
C450 C449 1.367(8) . ?
C441 C446 1.400(7) . ?
C441 C442 1.362(8) . ?
C661 C666 1.414(8) . ?
C661 C662 1.409(8) . ?
C661 B6 1.586(9) . ?
C453 C458 1.394(8) . ?
C453 C454 1.379(8) . ?
C331 C336 1.395(9) . ?
C331 B3 1.588(9) . ?
C331 C332 1.406(9) . ?
C563 C568 1.396(8) . ?
C563 C564 1.394(8) . ?
C670 C675 1.405(8) . ?
C670 C671 1.383(8) . ?
C670 B6 1.594(9) . ?
C881 B8 1.599(9) . ?
C881 C882 1.380(8) . ?
C881 C886 1.442(8) . ?
C101 C102 1.395(9) . ?
C101 B10 1.580(9) . ?
C101 C106 1.378(9) . ?
C92 C91 1.408(8) . ?
C92 C93 1.394(8) . ?
C92 C97 1.513(9) . ?
C91 C96 1.397(9) . ?
C91 B9 1.563(9) . ?
C568 H568 0.9300 . ?
C568 C567 1.384(8) . ?
C675 C678 1.518(8) . ?
C675 C674 1.394(8) . ?
C120 C125 1.410(8) . ?
C120 C121 1.389(8) . ?
C120 B1 1.581(9) . ?
C221 B2 1.610(9) . ?
C221 C226 1.404(8) . ?
C221 C222 1.406(8) . ?
C93 H93 0.9300 . ?
C93 C94 1.378(9) . ?
C125 C124 1.396(8) . ?
C125 C128 1.495(8) . ?
C891 C896 1.526(9) . ?
C891 C892 1.388(9) . ?
C776 C779 1.517(8) . ?
C776 C775 1.371(8) . ?
C779 H77A 0.9600 . ?
C779 H77B 0.9600 . ?
C779 H77C 0.9600 . ?
C663 H663 0.9300 . ?
C663 C662 1.392(8) . ?
C663 C664 1.368(9) . ?
C116 C119 1.526(8) . ?
C116 C115 1.377(8) . ?
C231 C232 1.395(8) . ?
C231 C236 1.507(8) . ?
C232 H232 0.9300 . ?
C232 C233 1.397(8) . ?
C446 H446 0.9300 . ?
C446 C445 1.361(8) . ?
C666 C669 1.506(8) . ?
C666 C665 1.383(8) . ?
C662 C667 1.512(8) . ?
C112 C117 1.502(8) . ?
C112 C113 1.384(8) . ?
C451 H451 0.9300 . ?
C772 C777 1.502(9) . ?
C772 C773 1.397(9) . ?
C336 C339 1.503(9) . ?
C336 C335 1.396(9) . ?
C781 C786 1.495(10) . ?
C781 C782 1.380(9) . ?
C882 C883 1.403(9) . ?
C882 C887 1.519(8) . ?
C449 H449 0.9300 . ?
C96 C95 1.392(9) . ?
C96 C99 1.518(9) . ?
C119 H11A 0.9600 . ?
C119 H11B 0.9600 . ?
C119 H11C 0.9600 . ?
C233 C234 1.363(8) . ?
C233 C237 1.501(8) . ?
C552 H552 0.9300 . ?
C552 C553 1.379(8) . ?
C667 H66A 0.9600 . ?
C667 H66B 0.9600 . ?
C667 H66C 0.9600 . ?
C339 H33A 0.9600 . ?
C339 H33B 0.9600 . ?
C339 H33C 0.9600 . ?
C886 C885 1.363(8) . ?
C886 C889 1.499(9) . ?
C558 H558 0.9300 . ?
C558 C559 1.371(9) . ?
C895 C898 1.509(8) . ?
C895 C894 1.387(8) . ?
B3 C340 1.592(10) . ?
C458 H458 0.9300 . ?
C458 C457 1.378(9) . ?
C671 C672 1.396(9) . ?
C671 C676 1.531(9) . ?
C664 C665 1.376(9) . ?
C664 C668 1.517(8) . ?
C564 H564 0.9300 . ?
C564 C565 1.373(8) . ?
C442 H442 0.9300 . ?
C442 C443 1.391(8) . ?
C234 H234 0.9300 . ?
C102 C103 1.369(9) . ?
C102 C107 1.523(10) . ?
C226 C229 1.509(9) . ?
C226 C225 1.388(8) . ?
C124 H124 0.9300 . ?
C124 C123 1.368(9) . ?
C94 C95 1.378(9) . ?
C94 C98 1.512(9) . ?
C562 H562 0.9300 . ?
C562 C561 1.379(9) . ?
C556 H556 0.9300 . ?
C556 C555 1.366(8) . ?
C775 H775 0.9300 . ?
C775 C774 1.369(9) . ?
C444 H444 0.9300 . ?
C444 C443 1.350(8) . ?
C444 C445 1.389(8) . ?
C332 C333 1.396(9) . ?
C332 C337 1.512(9) . ?
C785 C788 1.521(10) . ?
C785 C784 1.411(9) . ?
C454 H454 0.9300 . ?
C454 C455 1.395(9) . ?
C117 H11D 0.9600 . ?
C117 H11E 0.9600 . ?
C117 H11F 0.9600 . ?
C222 C227 1.502(10) . ?
C222 C223 1.398(9) . ?
C345 C348 1.483(11) . ?
C345 C344 1.372(11) . ?
C345 C340 1.431(10) . ?
C567 H567 0.9300 . ?
C567 C566 1.368(9) . ?
C788 H78A 0.9600 . ?
C788 H78B 0.9600 . ?
C788 H78C 0.9600 . ?
C884 C885 1.366(9) . ?
C884 C883 1.388(9) . ?
C884 C888 1.516(9) . ?
C113 H113 0.9300 . ?
C113 C114 1.381(9) . ?
C898 H89A 0.9600 . ?
C898 H89B 0.9600 . ?
C898 H89C 0.9600 . ?
C115 H115 0.9300 . ?
C115 C114 1.382(9) . ?
C95 H95 0.9300 . ?
C669 H66D 0.9600 . ?
C669 H66E 0.9600 . ?
C669 H66F 0.9600 . ?
C443 H443 0.9300 . ?
C777 H77D 0.9600 . ?
C777 H77E 0.9600 . ?
C777 H77F 0.9600 . ?
C97 H97A 0.9600 . ?
C97 H97B 0.9600 . ?
C97 H97C 0.9600 . ?
C894 H894 0.9300 . ?
C894 C893 1.371(9) . ?
C773 H773 0.9300 . ?
C773 C774 1.370(10) . ?
C672 H672 0.9300 . ?
C672 C673 1.371(10) . ?
C237 H23A 0.9600 . ?
C237 H23B 0.9600 . ?
C237 H23C 0.9600 . ?
C121 C122 1.392(8) . ?
C121 C126 1.528(8) . ?
C554 H554 0.9300 . ?
C554 C555 1.376(9) . ?
C554 C553 1.352(9) . ?
C238 H23D 0.9600 . ?
C238 H23E 0.9600 . ?
C238 H23F 0.9600 . ?
C333 H333 0.9300 . ?
C333 C334 1.371(10) . ?
C98 H98A 0.9600 . ?
C98 H98B 0.9600 . ?
C98 H98C 0.9600 . ?
C676 H67A 0.9600 . ?
C676 H67B 0.9600 . ?
C676 H67C 0.9600 . ?
C123 C122 1.385(9) . ?
C123 C127 1.524(9) . ?
C896 H89D 0.9600 . ?
C896 H89E 0.9600 . ?
C896 H89F 0.9600 . ?
C555 H555 0.9300 . ?
C885 H885 0.9300 . ?
C122 H122 0.9300 . ?
C227 H22A 0.9600 . ?
C227 H22B 0.9600 . ?
C227 H22C 0.9600 . ?
C883 H883 0.9300 . ?
C786 H78D 0.9600 . ?
C786 H78E 0.9600 . ?
C786 H78F 0.9600 . ?
C782 H782 0.9300 . ?
C782 C783 1.370(12) . ?
C106 C105 1.384(9) . ?
C106 C109 1.513(11) . ?
C445 H445 0.9300 . ?
C678 H67D 0.9600 . ?
C678 H67E 0.9600 . ?
C678 H67F 0.9600 . ?
C553 H553 0.9300 . ?
C565 H565 0.9300 . ?
C565 C566 1.364(9) . ?
C229 H22D 0.9600 . ?
C229 H22E 0.9600 . ?
C229 H22F 0.9600 . ?
C341 C342 1.422(11) . ?
C341 C346 1.529(11) . ?
C341 C340 1.378(10) . ?
C114 C118 1.499(9) . ?
C774 C778 1.506(9) . ?
C126 H12A 0.9600 . ?
C126 H12B 0.9600 . ?
C126 H12C 0.9600 . ?
C566 H566 0.9300 . ?
C128 H12D 0.9600 . ?
C128 H12E 0.9600 . ?
C128 H12F 0.9600 . ?
C335 H335 0.9300 . ?
C335 C334 1.369(10) . ?
C223 H223 0.9300 . ?
C223 C224 1.370(11) . ?
C457 H457 0.9300 . ?
C457 C456 1.357(11) . ?
C561 H561 0.9300 . ?
C561 C560 1.356(10) . ?
C455 H455 0.9300 . ?
C455 C456 1.356(10) . ?
C225 H225 0.9300 . ?
C225 C224 1.363(11) . ?
C674 H674 0.9300 . ?
C674 C673 1.371(10) . ?
C99 H99A 0.9600 . ?
C99 H99B 0.9600 . ?
C99 H99C 0.9600 . ?
C559 H559 0.9300 . ?
C559 C560 1.367(9) . ?
C887 H88A 0.9600 . ?
C887 H88B 0.9600 . ?
C887 H88C 0.9600 . ?
C784 H784 0.9300 . ?
C784 C783 1.355(11) . ?
C889 H88D 0.9600 . ?
C889 H88E 0.9600 . ?
C889 H88F 0.9600 . ?
C665 H665 0.9300 . ?
C224 C228 1.536(9) . ?
C348 H34A 0.9600 . ?
C348 H34B 0.9600 . ?
C348 H34C 0.9600 . ?
C105 H105 0.9300 . ?
C105 C104 1.356(10) . ?
C456 H456 0.9300 . ?
C892 H892 0.9300 . ?
C892 C893 1.360(10) . ?
C668 H66G 0.9600 . ?
C668 H66H 0.9600 . ?
C668 H66I 0.9600 . ?
C888 H88G 0.9600 . ?
C888 H88H 0.9600 . ?
C888 H88I 0.9600 . ?
C337 H33D 0.9600 . ?
C337 H33E 0.9600 . ?
C337 H33F 0.9600 . ?
C104 C103 1.370(10) . ?
C104 C108 1.507(10) . ?
C560 H560 0.9300 . ?
C334 C338 1.521(10) . ?
C103 H103 0.9300 . ?
C783 C787 1.524(10) . ?
C673 C677 1.516(9) . ?
C893 C897 1.502(10) . ?
C342 H342 0.9300 . ?
C342 C343 1.369(14) . ?
C344 H344 0.9300 . ?
C344 C343 1.349(14) . ?
C778 H77G 0.9600 . ?
C778 H77H 0.9600 . ?
C778 H77I 0.9600 . ?
C127 H12G 0.9600 . ?
C127 H12H 0.9600 . ?
C127 H12I 0.9600 . ?
C343 C347 1.528(11) . ?
C346 H34D 0.9600 . ?
C346 H34E 0.9600 . ?
C346 H34F 0.9600 . ?
C228 H22G 0.9600 . ?
C228 H22H 0.9600 . ?
C228 H22I 0.9600 . ?
C677 H67G 0.9600 . ?
C677 H67H 0.9600 . ?
C677 H67I 0.9600 . ?
C118 H11G 0.9600 . ?
C118 H11H 0.9600 . ?
C118 H11I 0.9600 . ?
C897 H89G 0.9600 . ?
C897 H89H 0.9600 . ?
C897 H89I 0.9600 . ?
C338 H33G 0.9600 . ?
C338 H33H 0.9600 . ?
C338 H33I 0.9600 . ?
C109 H10A 0.9600 . ?
C109 H10B 0.9600 . ?
C109 H10C 0.9600 . ?
C107 H10D 0.9600 . ?
C107 H10E 0.9600 . ?
C107 H10F 0.9600 . ?
C108 H10G 0.9600 . ?
C108 H10H 0.9600 . ?
C108 H10I 0.9600 . ?
C787 H78G 0.9600 . ?
C787 H78H 0.9600 . ?
C787 H78I 0.9600 . ?
C347 H34G 0.9600 . ?
C347 H34H 0.9600 . ?
C347 H34I 0.9600 . ?
C236 H23G 0.9600 . ?
C236 H23H 0.9600 . ?
C236 H23I 0.9600 . ?

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
O3 U1 O1 118.57(16) . . ?
O3 U1 O5 90.48(14) . . ?
O3 U1 O4 90.08(14) . . ?
O3 U1 O2 120.86(16) . . ?
O1 U1 O5 88.00(14) . . ?
O1 U1 O4 88.78(14) . . ?
O1 U1 O2 120.53(16) . . ?
O4 U1 O5 176.60(13) . . ?
O2 U1 O5 89.58(14) . . ?
O2 U1 O4 93.01(14) . . ?
O7 U2 O8 90.41(15) . . ?
O7 U2 O11 160.94(16) . . ?
O7 U2 O9 88.90(15) . . ?
O6 U2 O7 100.34(15) . . ?
O6 U2 O8 112.96(15) . . ?
O6 U2 O11 96.13(17) . . ?
O6 U2 O9 105.75(17) . . ?
O8 U2 O11 91.96(15) . . ?
O8 U2 O9 140.75(18) . . ?
O9 U2 O11 77.38(16) . . ?
O4 P4 C447 109.0(2) . . ?
O4 P4 C441 110.6(2) . . ?
O4 P4 C453 111.2(2) . . ?
C447 P4 C453 107.6(3) . . ?
C441 P4 C447 108.6(3) . . ?
C441 P4 C453 109.7(3) . . ?
O5 P5 C551 109.9(2) . . ?
O5 P5 C557 110.0(3) . . ?
O5 P5 C563 110.7(2) . . ?
C557 P5 C551 109.8(3) . . ?
C563 P5 C551 109.2(3) . . ?
C563 P5 C557 107.2(3) . . ?
B3 O3 U1 176.6(4) . . ?
B1 O1 U1 176.0(4) . . ?
P5 O5 U1 170.5(3) . . ?
P4 O4 U1 174.4(2) . . ?
B7 O7 U2 165.7(4) . . ?
B6 O6 U2 168.6(4) . . ?
B8 O8 U2 155.3(4) . . ?
B2 O2 U1 175.3(4) . . ?
B9 O10 B10 127.1(5) . . ?
B10 O11 U2 134.3(4) . . ?
B9 O9 U2 135.5(4) . . ?
C452 C447 P4 123.2(5) . . ?
C452 C447 C448 117.6(5) . . ?
C448 C447 P4 119.1(4) . . ?
C235 C230 B2 121.7(5) . . ?
C231 C230 C235 117.8(5) . . ?
C231 C230 B2 120.5(5) . . ?
C447 C452 H452 119.3 . . ?
C447 C452 C451 121.4(6) . . ?
C451 C452 H452 119.3 . . ?
C552 C551 P5 122.7(5) . . ?
C552 C551 C556 118.1(6) . . ?
C556 C551 P5 119.2(5) . . ?
C447 C448 H448 119.7 . . ?
C449 C448 C447 120.7(6) . . ?
C449 C448 H448 119.7 . . ?
C776 C771 C772 117.2(5) . . ?
C776 C771 B7 122.0(5) . . ?
C772 C771 B7 120.8(6) . . ?
C891 C890 B8 121.8(6) . . ?
C891 C890 C895 118.1(6) . . ?
C895 C890 B8 120.1(6) . . ?
C558 C557 P5 119.3(5) . . ?
C558 C557 C562 119.4(6) . . ?
C562 C557 P5 121.3(5) . . ?
C116 C111 C112 116.7(5) . . ?
C116 C111 B1 121.2(5) . . ?
C112 C111 B1 121.7(6) . . ?
C230 C235 C238 120.6(5) . . ?
C234 C235 C230 119.6(5) . . ?
C234 C235 C238 119.9(5) . . ?
C781 C780 B7 121.8(6) . . ?
C785 C780 C781 118.0(6) . . ?
C785 C780 B7 120.1(6) . . ?
C451 C450 H450 119.9 . . ?
C449 C450 H450 119.9 . . ?
C449 C450 C451 120.1(6) . . ?
C446 C441 P4 118.2(4) . . ?
C442 C441 P4 122.6(4) . . ?
C442 C441 C446 119.2(5) . . ?
C666 C661 B6 121.4(5) . . ?
C662 C661 C666 117.9(6) . . ?
C662 C661 B6 120.7(6) . . ?
C458 C453 P4 120.8(5) . . ?
C454 C453 P4 119.6(5) . . ?
C454 C453 C458 119.6(6) . . ?
C336 C331 B3 119.7(6) . . ?
C336 C331 C332 119.0(6) . . ?
C332 C331 B3 121.2(6) . . ?
C568 C563 P5 121.8(4) . . ?
C564 C563 P5 120.3(5) . . ?
C564 C563 C568 117.9(6) . . ?
C675 C670 B6 120.4(5) . . ?
C671 C670 C675 117.6(6) . . ?
C671 C670 B6 121.9(6) . . ?
C882 C881 B8 123.0(5) . . ?
C882 C881 C886 117.0(6) . . ?
C886 C881 B8 119.9(6) . . ?
C102 C101 B10 121.4(7) . . ?
C106 C101 C102 117.1(6) . . ?
C106 C101 B10 121.5(6) . . ?
C91 C92 C97 120.0(6) . . ?
C93 C92 C91 119.4(6) . . ?
C93 C92 C97 120.6(6) . . ?
C92 C91 B9 120.8(6) . . ?
C96 C91 C92 117.5(6) . . ?
C96 C91 B9 121.6(6) . . ?
C563 C568 H568 119.6 . . ?
C567 C568 C563 120.8(6) . . ?
C567 C568 H568 119.6 . . ?
C670 C675 C678 122.3(5) . . ?
C674 C675 C670 120.2(6) . . ?
C674 C675 C678 117.6(6) . . ?
C125 C120 B1 120.9(6) . . ?
C121 C120 C125 118.4(6) . . ?
C121 C120 B1 120.4(6) . . ?
C226 C221 B2 120.7(5) . . ?
C226 C221 C222 118.4(6) . . ?
C222 C221 B2 120.7(6) . . ?
C92 C93 H93 118.8 . . ?
C94 C93 C92 122.4(6) . . ?
C94 C93 H93 118.8 . . ?
C120 C125 C128 121.8(6) . . ?
C124 C125 C120 119.0(6) . . ?
C124 C125 C128 119.2(6) . . ?
C890 C891 C896 120.1(6) . . ?
C892 C891 C890 120.1(7) . . ?
C892 C891 C896 119.8(6) . . ?
C771 C776 C779 120.5(5) . . ?
C775 C776 C771 121.2(6) . . ?
C775 C776 C779 118.2(6) . . ?
C776 C779 H77A 109.5 . . ?
C776 C779 H77B 109.5 . . ?
C776 C779 H77C 109.5 . . ?
H77A C779 H77B 109.5 . . ?
H77A C779 H77C 109.5 . . ?
H77B C779 H77C 109.5 . . ?
C662 C663 H663 119.1 . . ?
C664 C663 H663 119.1 . . ?
C664 C663 C662 121.8(6) . . ?
C111 C116 C119 121.6(5) . . ?
C115 C116 C111 121.4(6) . . ?
C115 C116 C119 117.0(6) . . ?
C230 C231 C236 122.0(5) . . ?
C232 C231 C230 120.3(5) . . ?
C232 C231 C236 117.7(5) . . ?
C231 C232 H232 119.1 . . ?
C231 C232 C233 121.8(6) . . ?
C233 C232 H232 119.1 . . ?
C441 C446 H446 120.0 . . ?
C445 C446 C441 119.9(6) . . ?
C445 C446 H446 120.0 . . ?
C661 C666 C669 120.7(6) . . ?
C665 C666 C661 119.8(6) . . ?
C665 C666 C669 119.4(6) . . ?
C661 C662 C667 121.6(6) . . ?
C663 C662 C661 119.9(6) . . ?
C663 C662 C667 118.5(6) . . ?
C111 C112 C117 120.4(6) . . ?
C113 C112 C111 119.6(6) . . ?
C113 C112 C117 119.9(6) . . ?
C452 C451 H451 120.2 . . ?
C450 C451 C452 119.6(6) . . ?
C450 C451 H451 120.2 . . ?
C771 C772 C777 121.3(6) . . ?
C773 C772 C771 119.5(6) . . ?
C773 C772 C777 119.2(6) . . ?
C331 C336 C339 122.0(6) . . ?
C331 C336 C335 119.5(7) . . ?
C335 C336 C339 118.5(6) . . ?
C780 C781 C786 123.5(6) . . ?
C782 C781 C780 118.6(8) . . ?
C782 C781 C786 117.9(7) . . ?
O8 B8 C890 120.1(6) . . ?
O8 B8 C881 118.8(6) . . ?
C890 B8 C881 121.1(5) . . ?
C881 C882 C883 121.8(6) . . ?
C881 C882 C887 121.1(6) . . ?
C883 C882 C887 117.0(6) . . ?
C448 C449 H449 119.7 . . ?
C450 C449 C448 120.5(6) . . ?
C450 C449 H449 119.7 . . ?
C91 C96 C99 118.8(6) . . ?
C95 C96 C91 121.8(6) . . ?
C95 C96 C99 119.4(6) . . ?
C116 C119 H11A 109.5 . . ?
C116 C119 H11B 109.5 . . ?
C116 C119 H11C 109.5 . . ?
H11A C119 H11B 109.5 . . ?
H11A C119 H11C 109.5 . . ?
H11B C119 H11C 109.5 . . ?
C232 C233 C237 121.3(6) . . ?
C234 C233 C232 117.3(6) . . ?
C234 C233 C237 121.3(6) . . ?
C551 C552 H552 119.8 . . ?
C551 C552 C553 120.4(6) . . ?
C553 C552 H552 119.8 . . ?
C662 C667 H66A 109.5 . . ?
C662 C667 H66B 109.5 . . ?
C662 C667 H66C 109.5 . . ?
H66A C667 H66B 109.5 . . ?
H66A C667 H66C 109.5 . . ?
H66B C667 H66C 109.5 . . ?
C336 C339 H33A 109.5 . . ?
C336 C339 H33B 109.5 . . ?
C336 C339 H33C 109.5 . . ?
H33A C339 H33B 109.5 . . ?
H33A C339 H33C 109.5 . . ?
H33B C339 H33C 109.5 . . ?
O2 B2 C230 119.3(5) . . ?
O2 B2 C221 119.8(5) . . ?
C230 B2 C221 120.9(5) . . ?
C881 C886 C889 123.2(6) . . ?
C885 C886 C881 119.3(6) . . ?
C885 C886 C889 117.4(6) . . ?
C557 C558 H558 119.8 . . ?
C557 C558 C559 120.4(6) . . ?
C559 C558 H558 119.8 . . ?
C890 C895 C898 121.7(6) . . ?
C894 C895 C890 118.8(6) . . ?
C894 C895 C898 119.4(6) . . ?
O3 B3 C331 119.4(6) . . ?
O3 B3 C340 117.1(6) . . ?
C331 B3 C340 123.4(6) . . ?
C453 C458 H458 120.2 . . ?
C457 C458 C453 119.7(7) . . ?
C457 C458 H458 120.2 . . ?
C670 C671 C672 120.7(6) . . ?
C670 C671 C676 122.6(6) . . ?
C672 C671 C676 116.7(6) . . ?
C663 C664 C665 118.6(6) . . ?
C663 C664 C668 121.0(6) . . ?
C665 C664 C668 120.3(6) . . ?
C563 C564 H564 119.8 . . ?
C565 C564 C563 120.4(6) . . ?
C565 C564 H564 119.8 . . ?
C441 C442 H442 120.0 . . ?
C441 C442 C443 120.1(6) . . ?
C443 C442 H442 120.0 . . ?
C235 C234 H234 118.5 . . ?
C233 C234 C235 123.1(6) . . ?
C233 C234 H234 118.5 . . ?
C101 C102 C107 119.2(7) . . ?
C103 C102 C101 120.8(7) . . ?
C103 C102 C107 120.0(7) . . ?
C221 C226 C229 121.8(6) . . ?
C225 C226 C221 119.9(7) . . ?
C225 C226 C229 118.3(6) . . ?
C125 C124 H124 118.8 . . ?
C123 C124 C125 122.4(6) . . ?
C123 C124 H124 118.8 . . ?
C93 C94 C98 120.6(7) . . ?
C95 C94 C93 118.4(6) . . ?
C95 C94 C98 121.0(6) . . ?
C557 C562 H562 120.2 . . ?
C561 C562 C557 119.6(6) . . ?
C561 C562 H562 120.2 . . ?
C551 C556 H556 119.3 . . ?
C555 C556 C551 121.4(6) . . ?
C555 C556 H556 119.3 . . ?
C776 C775 H775 119.1 . . ?
C774 C775 C776 121.8(7) . . ?
C774 C775 H775 119.1 . . ?
C443 C444 H444 120.4 . . ?
C443 C444 C445 119.2(6) . . ?
C445 C444 H444 120.4 . . ?
C331 C332 C337 123.1(6) . . ?
C333 C332 C331 118.9(7) . . ?
C333 C332 C337 118.0(7) . . ?
C780 C785 C788 122.9(6) . . ?
C780 C785 C784 120.0(8) . . ?
C784 C785 C788 117.1(7) . . ?
C453 C454 H454 120.6 . . ?
C453 C454 C455 118.8(7) . . ?
C455 C454 H454 120.6 . . ?
C112 C117 H11D 109.5 . . ?
C112 C117 H11E 109.5 . . ?
C112 C117 H11F 109.5 . . ?
H11D C117 H11E 109.5 . . ?
H11D C117 H11F 109.5 . . ?
H11E C117 H11F 109.5 . . ?
C221 C222 C227 122.1(6) . . ?
C223 C222 C221 118.9(7) . . ?
C223 C222 C227 119.0(7) . . ?
C344 C345 C348 119.2(9) . . ?
C344 C345 C340 118.4(9) . . ?
C340 C345 C348 122.3(7) . . ?
O6 B6 C661 118.3(5) . . ?
O6 B6 C670 118.2(6) . . ?
C661 B6 C670 123.5(5) . . ?
C568 C567 H567 120.2 . . ?
C566 C567 C568 119.7(6) . . ?
C566 C567 H567 120.2 . . ?
C785 C788 H78A 109.5 . . ?
C785 C788 H78B 109.5 . . ?
C785 C788 H78C 109.5 . . ?
H78A C788 H78B 109.5 . . ?
H78A C788 H78C 109.5 . . ?
H78B C788 H78C 109.5 . . ?
O10 B10 C101 114.2(5) . . ?
O11 B10 O10 122.3(6) . . ?
O11 B10 C101 123.4(6) . . ?
C885 C884 C883 118.3(6) . . ?
C885 C884 C888 120.8(6) . . ?
C883 C884 C888 120.8(7) . . ?
C112 C113 H113 118.4 . . ?
C114 C113 C112 123.2(6) . . ?
C114 C113 H113 118.4 . . ?
C895 C898 H89A 109.5 . . ?
C895 C898 H89B 109.5 . . ?
C895 C898 H89C 109.5 . . ?
H89A C898 H89B 109.5 . . ?
H89A C898 H89C 109.5 . . ?
H89B C898 H89C 109.5 . . ?
C116 C115 H115 119.0 . . ?
C116 C115 C114 122.0(6) . . ?
C114 C115 H115 119.0 . . ?
C96 C95 H95 119.8 . . ?
C94 C95 C96 120.4(6) . . ?
C94 C95 H95 119.8 . . ?
C666 C669 H66D 109.5 . . ?
C666 C669 H66E 109.5 . . ?
C666 C669 H66F 109.5 . . ?
H66D C669 H66E 109.5 . . ?
H66D C669 H66F 109.5 . . ?
H66E C669 H66F 109.5 . . ?
C442 C443 H443 119.5 . . ?
C444 C443 C442 120.9(6) . . ?
C444 C443 H443 119.5 . . ?
C772 C777 H77D 109.5 . . ?
C772 C777 H77E 109.5 . . ?
C772 C777 H77F 109.5 . . ?
H77D C777 H77E 109.5 . . ?
H77D C777 H77F 109.5 . . ?
H77E C777 H77F 109.5 . . ?
C92 C97 H97A 109.5 . . ?
C92 C97 H97B 109.5 . . ?
C92 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C895 C894 H894 118.8 . . ?
C893 C894 C895 122.4(7) . . ?
C893 C894 H894 118.8 . . ?
C772 C773 H773 119.1 . . ?
C774 C773 C772 121.8(6) . . ?
C774 C773 H773 119.1 . . ?
C671 C672 H672 119.1 . . ?
C673 C672 C671 121.9(7) . . ?
C673 C672 H672 119.1 . . ?
C233 C237 H23A 109.5 . . ?
C233 C237 H23B 109.5 . . ?
C233 C237 H23C 109.5 . . ?
H23A C237 H23B 109.5 . . ?
H23A C237 H23C 109.5 . . ?
H23B C237 H23C 109.5 . . ?
C120 C121 C122 120.9(6) . . ?
C120 C121 C126 122.0(6) . . ?
C122 C121 C126 117.1(6) . . ?
C555 C554 H554 119.7 . . ?
C553 C554 H554 119.7 . . ?
C553 C554 C555 120.6(6) . . ?
C235 C238 H23D 109.5 . . ?
C235 C238 H23E 109.5 . . ?
C235 C238 H23F 109.5 . . ?
H23D C238 H23E 109.5 . . ?
H23D C238 H23F 109.5 . . ?
H23E C238 H23F 109.5 . . ?
C332 C333 H333 118.9 . . ?
C334 C333 C332 122.2(7) . . ?
C334 C333 H333 118.9 . . ?
C94 C98 H98A 109.5 . . ?
C94 C98 H98B 109.5 . . ?
C94 C98 H98C 109.5 . . ?
H98A C98 H98B 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C671 C676 H67A 109.5 . . ?
C671 C676 H67B 109.5 . . ?
C671 C676 H67C 109.5 . . ?
H67A C676 H67B 109.5 . . ?
H67A C676 H67C 109.5 . . ?
H67B C676 H67C 109.5 . . ?
C124 C123 C122 118.4(6) . . ?
C124 C123 C127 121.7(7) . . ?
C122 C123 C127 119.9(7) . . ?
C891 C896 H89D 109.5 . . ?
C891 C896 H89E 109.5 . . ?
C891 C896 H89F 109.5 . . ?
H89D C896 H89E 109.5 . . ?
H89D C896 H89F 109.5 . . ?
H89E C896 H89F 109.5 . . ?
C556 C555 C554 119.2(6) . . ?
C556 C555 H555 120.4 . . ?
C554 C555 H555 120.4 . . ?
C886 C885 C884 123.4(6) . . ?
C886 C885 H885 118.3 . . ?
C884 C885 H885 118.3 . . ?
C121 C122 H122 119.6 . . ?
C123 C122 C121 120.8(6) . . ?
C123 C122 H122 119.6 . . ?
C222 C227 H22A 109.5 . . ?
C222 C227 H22B 109.5 . . ?
C222 C227 H22C 109.5 . . ?
H22A C227 H22B 109.5 . . ?
H22A C227 H22C 109.5 . . ?
H22B C227 H22C 109.5 . . ?
C882 C883 H883 120.0 . . ?
C884 C883 C882 120.0(7) . . ?
C884 C883 H883 120.0 . . ?
C781 C786 H78D 109.5 . . ?
C781 C786 H78E 109.5 . . ?
C781 C786 H78F 109.5 . . ?
H78D C786 H78E 109.5 . . ?
H78D C786 H78F 109.5 . . ?
H78E C786 H78F 109.5 . . ?
C781 C782 H782 117.8 . . ?
C783 C782 C781 124.4(8) . . ?
C783 C782 H782 117.8 . . ?
C101 C106 C105 120.3(7) . . ?
C101 C106 C109 119.2(7) . . ?
C105 C106 C109 120.5(8) . . ?
C446 C445 C444 120.7(6) . . ?
C446 C445 H445 119.7 . . ?
C444 C445 H445 119.7 . . ?
C675 C678 H67D 109.5 . . ?
C675 C678 H67E 109.5 . . ?
C675 C678 H67F 109.5 . . ?
H67D C678 H67E 109.5 . . ?
H67D C678 H67F 109.5 . . ?
H67E C678 H67F 109.5 . . ?
O10 B9 C91 118.4(6) . . ?
O9 B9 O10 121.8(6) . . ?
O9 B9 C91 119.8(7) . . ?
O1 B1 C111 116.5(5) . . ?
O1 B1 C120 116.8(5) . . ?
C120 B1 C111 126.8(5) . . ?
C552 C553 H553 119.8 . . ?
C554 C553 C552 120.3(7) . . ?
C554 C553 H553 119.8 . . ?
C564 C565 H565 119.6 . . ?
C566 C565 C564 120.7(6) . . ?
C566 C565 H565 119.6 . . ?
O7 B7 C771 119.3(6) . . ?
O7 B7 C780 120.1(6) . . ?
C771 B7 C780 120.5(6) . . ?
C226 C229 H22D 109.5 . . ?
C226 C229 H22E 109.5 . . ?
C226 C229 H22F 109.5 . . ?
H22D C229 H22E 109.5 . . ?
H22D C229 H22F 109.5 . . ?
H22E C229 H22F 109.5 . . ?
C342 C341 C346 119.2(8) . . ?
C340 C341 C342 119.4(9) . . ?
C340 C341 C346 121.3(7) . . ?
C113 C114 C115 117.0(6) . . ?
C113 C114 C118 121.8(7) . . ?
C115 C114 C118 121.2(7) . . ?
C775 C774 C778 120.4(8) . . ?
C773 C774 C775 118.4(7) . . ?
C773 C774 C778 121.2(7) . . ?
C121 C126 H12A 109.5 . . ?
C121 C126 H12B 109.5 . . ?
C121 C126 H12C 109.5 . . ?
H12A C126 H12B 109.5 . . ?
H12A C126 H12C 109.5 . . ?
H12B C126 H12C 109.5 . . ?
C567 C566 H566 119.8 . . ?
C565 C566 C567 120.4(6) . . ?
C565 C566 H566 119.8 . . ?
C125 C128 H12D 109.5 . . ?
C125 C128 H12E 109.5 . . ?
C125 C128 H12F 109.5 . . ?
H12D C128 H12E 109.5 . . ?
H12D C128 H12F 109.5 . . ?
H12E C128 H12F 109.5 . . ?
C336 C335 H335 119.0 . . ?
C334 C335 C336 122.0(7) . . ?
C334 C335 H335 119.0 . . ?
C222 C223 H223 118.8 . . ?
C224 C223 C222 122.3(7) . . ?
C224 C223 H223 118.8 . . ?
C458 C457 H457 119.7 . . ?
C456 C457 C458 120.7(8) . . ?
C456 C457 H457 119.7 . . ?
C562 C561 H561 120.0 . . ?
C560 C561 C562 120.0(7) . . ?
C560 C561 H561 120.0 . . ?
C454 C455 H455 119.5 . . ?
C456 C455 C454 121.1(8) . . ?
C456 C455 H455 119.5 . . ?
C226 C225 H225 119.0 . . ?
C224 C225 C226 122.0(7) . . ?
C224 C225 H225 119.0 . . ?
C675 C674 H674 119.0 . . ?
C673 C674 C675 121.9(7) . . ?
C673 C674 H674 119.0 . . ?
C96 C99 H99A 109.5 . . ?
C96 C99 H99B 109.5 . . ?
C96 C99 H99C 109.5 . . ?
H99A C99 H99B 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C558 C559 H559 119.9 . . ?
C560 C559 C558 120.1(7) . . ?
C560 C559 H559 119.9 . . ?
C882 C887 H88A 109.5 . . ?
C882 C887 H88B 109.5 . . ?
C882 C887 H88C 109.5 . . ?
H88A C887 H88B 109.5 . . ?
H88A C887 H88C 109.5 . . ?
H88B C887 H88C 109.5 . . ?
C785 C784 H784 118.9 . . ?
C783 C784 C785 122.1(8) . . ?
C783 C784 H784 118.9 . . ?
C886 C889 H88D 109.5 . . ?
C886 C889 H88E 109.5 . . ?
C886 C889 H88F 109.5 . . ?
H88D C889 H88E 109.5 . . ?
H88D C889 H88F 109.5 . . ?
H88E C889 H88F 109.5 . . ?
C666 C665 H665 119.0 . . ?
C664 C665 C666 122.0(6) . . ?
C664 C665 H665 119.0 . . ?
C223 C224 C228 120.6(9) . . ?
C225 C224 C223 118.4(7) . . ?
C225 C224 C228 121.0(9) . . ?
C345 C348 H34A 109.5 . . ?
C345 C348 H34B 109.5 . . ?
C345 C348 H34C 109.5 . . ?
H34A C348 H34B 109.5 . . ?
H34A C348 H34C 109.5 . . ?
H34B C348 H34C 109.5 . . ?
C106 C105 H105 118.7 . . ?
C104 C105 C106 122.7(8) . . ?
C104 C105 H105 118.7 . . ?
C457 C456 H456 119.9 . . ?
C455 C456 C457 120.1(7) . . ?
C455 C456 H456 119.9 . . ?
C891 C892 H892 119.1 . . ?
C893 C892 C891 121.9(7) . . ?
C893 C892 H892 119.1 . . ?
C664 C668 H66G 109.5 . . ?
C664 C668 H66H 109.5 . . ?
C664 C668 H66I 109.5 . . ?
H66G C668 H66H 109.5 . . ?
H66G C668 H66I 109.5 . . ?
H66H C668 H66I 109.5 . . ?
C884 C888 H88G 109.5 . . ?
C884 C888 H88H 109.5 . . ?
C884 C888 H88I 109.5 . . ?
H88G C888 H88H 109.5 . . ?
H88G C888 H88I 109.5 . . ?
H88H C888 H88I 109.5 . . ?
C332 C337 H33D 109.5 . . ?
C332 C337 H33E 109.5 . . ?
C332 C337 H33F 109.5 . . ?
H33D C337 H33E 109.5 . . ?
H33D C337 H33F 109.5 . . ?
H33E C337 H33F 109.5 . . ?
C105 C104 C103 116.9(7) . . ?
C105 C104 C108 121.4(8) . . ?
C103 C104 C108 121.7(8) . . ?
C561 C560 C559 120.3(7) . . ?
C561 C560 H560 119.8 . . ?
C559 C560 H560 119.8 . . ?
C333 C334 C338 121.0(8) . . ?
C335 C334 C333 118.4(7) . . ?
C335 C334 C338 120.6(8) . . ?
C102 C103 C104 122.1(7) . . ?
C102 C103 H103 118.9 . . ?
C104 C103 H103 118.9 . . ?
C782 C783 C787 120.7(10) . . ?
C784 C783 C782 116.9(8) . . ?
C784 C783 C787 122.4(10) . . ?
C672 C673 C674 117.7(6) . . ?
C672 C673 C677 121.6(7) . . ?
C674 C673 C677 120.6(8) . . ?
C894 C893 C897 119.5(7) . . ?
C892 C893 C894 118.6(7) . . ?
C892 C893 C897 121.9(7) . . ?
C341 C342 H342 119.0 . . ?
C343 C342 C341 122.0(10) . . ?
C343 C342 H342 119.0 . . ?
C345 C344 H344 117.7 . . ?
C343 C344 C345 124.7(10) . . ?
C343 C344 H344 117.7 . . ?
C774 C778 H77G 109.5 . . ?
C774 C778 H77H 109.5 . . ?
C774 C778 H77I 109.5 . . ?
H77G C778 H77H 109.5 . . ?
H77G C778 H77I 109.5 . . ?
H77H C778 H77I 109.5 . . ?
C123 C127 H12G 109.5 . . ?
C123 C127 H12H 109.5 . . ?
C123 C127 H12I 109.5 . . ?
H12G C127 H12H 109.5 . . ?
H12G C127 H12I 109.5 . . ?
H12H C127 H12I 109.5 . . ?
C342 C343 C347 120.9(13) . . ?
C344 C343 C342 117.1(9) . . ?
C344 C343 C347 122.0(12) . . ?
C341 C346 H34D 109.5 . . ?
C341 C346 H34E 109.5 . . ?
C341 C346 H34F 109.5 . . ?
H34D C346 H34E 109.5 . . ?
H34D C346 H34F 109.5 . . ?
H34E C346 H34F 109.5 . . ?
C224 C228 H22G 109.5 . . ?
C224 C228 H22H 109.5 . . ?
C224 C228 H22I 109.5 . . ?
H22G C228 H22H 109.5 . . ?
H22G C228 H22I 109.5 . . ?
H22H C228 H22I 109.5 . . ?
C673 C677 H67G 109.5 . . ?
C673 C677 H67H 109.5 . . ?
C673 C677 H67I 109.5 . . ?
H67G C677 H67H 109.5 . . ?
H67G C677 H67I 109.5 . . ?
H67H C677 H67I 109.5 . . ?
C114 C118 H11G 109.5 . . ?
C114 C118 H11H 109.5 . . ?
C114 C118 H11I 109.5 . . ?
H11G C118 H11H 109.5 . . ?
H11G C118 H11I 109.5 . . ?
H11H C118 H11I 109.5 . . ?
C893 C897 H89G 109.5 . . ?
C893 C897 H89H 109.5 . . ?
C893 C897 H89I 109.5 . . ?
H89G C897 H89H 109.5 . . ?
H89G C897 H89I 109.5 . . ?
H89H C897 H89I 109.5 . . ?
C334 C338 H33G 109.5 . . ?
C334 C338 H33H 109.5 . . ?
C334 C338 H33I 109.5 . . ?
H33G C338 H33H 109.5 . . ?
H33G C338 H33I 109.5 . . ?
H33H C338 H33I 109.5 . . ?
C106 C109 H10A 109.5 . . ?
C106 C109 H10B 109.5 . . ?
C106 C109 H10C 109.5 . . ?
H10A C109 H10B 109.5 . . ?
H10A C109 H10C 109.5 . . ?
H10B C109 H10C 109.5 . . ?
C102 C107 H10D 109.5 . . ?
C102 C107 H10E 109.5 . . ?
C102 C107 H10F 109.5 . . ?
H10D C107 H10E 109.5 . . ?
H10D C107 H10F 109.5 . . ?
H10E C107 H10F 109.5 . . ?
C104 C108 H10G 109.5 . . ?
C104 C108 H10H 109.5 . . ?
C104 C108 H10I 109.5 . . ?
H10G C108 H10H 109.5 . . ?
H10G C108 H10I 109.5 . . ?
H10H C108 H10I 109.5 . . ?
C783 C787 H78G 109.5 . . ?
C783 C787 H78H 109.5 . . ?
C783 C787 H78I 109.5 . . ?
H78G C787 H78H 109.5 . . ?
H78G C787 H78I 109.5 . . ?
H78H C787 H78I 109.5 . . ?
C343 C347 H34G 109.5 . . ?
C343 C347 H34H 109.5 . . ?
C343 C347 H34I 109.5 . . ?
H34G C347 H34H 109.5 . . ?
H34G C347 H34I 109.5 . . ?
H34H C347 H34I 109.5 . . ?
C231 C236 H23G 109.5 . . ?
C231 C236 H23H 109.5 . . ?
C231 C236 H23I 109.5 . . ?
H23G C236 H23H 109.5 . . ?
H23G C236 H23I 109.5 . . ?
H23H C236 H23I 109.5 . . ?
C345 C340 B3 120.7(7) . . ?
C341 C340 B3 121.0(7) . . ?
C341 C340 C345 118.3(7) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.302 0.633 0.746 735.6 124.8 ?
2 0.342 0.087 0.880 10.2 0.0 ?
3 0.371 0.104 0.055 16.3 0.0 ?
4 0.698 0.367 0.254 735.6 132.0 ?
5 0.629 0.896 0.945 16.3 0.0 ?
6 0.658 0.913 0.120 10.2 0.4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.094
_oxdiff_exptl_absorpt_empirical_full_min 0.883

# start Validation Reply Form
_vrf_PLAT973_p18047              
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       2.14 eA-3  
RESPONSE: Uranium is a heavy metal therefore residual density
could be expected, therefore this is not seen as a serious problem.
;
_vrf_PLAT910_p18047              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         49 Note  
RESPONSE: No. of reflections / No. of parameters = 19.8 Therefore
this is not seen as a serious problem.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p16133_087mono
_database_code_depnum_ccdc_archive 'CCDC 1886803'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C94 H147.98 B3 O4 U'
_chemical_formula_sum            'C94 H147.98 B3 O4 U'
_chemical_formula_weight         1612.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H100 B3 O3 U'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.5344(7)
_cell_length_b                   27.8539(8)
_cell_length_c                   20.2709(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.880(4)
_cell_angle_gamma                90
_cell_volume                     9247.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.7660
_cell_measurement_theta_min      3.3100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.800
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3404
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 1 21 0.0871
18 -1 -21 0.0871
1 39 -3 0.0219
-1 -39 3 0.0219
-14 -6 -20 0.0230
14 6 20 0.0230

_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.044
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-18.0000 0.9999 21.0000 0.8794 -0.3934 0.2684
18.0000 -0.9999 -21.0000 -0.8794 0.3934 -0.2684
1.0000 38.9999 -3.0000 0.1778 -0.0918 -0.9788
-1.0000 -38.9999 3.0000 -0.1778 0.0918 0.9788
-14.0000 -6.0000 -20.0000 0.3489 0.9380 0.0762
14.0000 6.0000 20.0000 -0.3489 -0.9380 -0.0762

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2674
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            131250
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.886
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  50.00   1.00   45.00    --  -18.53  57.00-120.00   87
  2  ω    -90.00  53.00   1.00   45.00    --  -18.53   0.00  30.00  143
  3  ω    -25.00  22.00   1.00   45.00    --  -18.53 -99.00 -90.00   47
  4  ω    -25.00  22.00   1.00   45.00    --  -18.53 -99.00 120.00   47
  5  ω    -88.00  10.00   1.00   45.00    --  -18.53 -77.00  30.00   98
  6  ω    -25.00  22.00   1.00   45.00    --  -18.53 -99.00  90.00   47
  7  ω    -18.00  92.00   1.00   45.00    --   20.09  19.00 -30.00  110
  8  ω    -93.00 -32.00   1.00   45.00    --  -18.53 179.00  30.00   61
  9  ω    -47.00  51.00   1.00   45.00    --  -18.53  77.00 150.00   98
 10  ω    -25.00   0.00   1.00   45.00    --  -18.53 -99.00 150.00   25
 11  ω    -25.00  61.00   1.00   45.00    --   20.09 -99.00  30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0390978000
_diffrn_orient_matrix_UB_12      0.0061814000
_diffrn_orient_matrix_UB_13      0.0080679000
_diffrn_orient_matrix_UB_21      -0.0173632000
_diffrn_orient_matrix_UB_22      -0.0044786000
_diffrn_orient_matrix_UB_23      -0.0334045000
_diffrn_orient_matrix_UB_31      -0.0067147000
_diffrn_orient_matrix_UB_32      -0.0242956000
_diffrn_orient_matrix_UB_33      0.0081811000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8850
_reflns_number_total             14671
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         14671
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0801
_refine_ls_restrained_S_all      1.030
_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)+(0.0180P)²+13.3799P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1155
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C601 \\sim C600: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C640) = Uanis(C540)
3. Rigid body (RIGU) restrains
 C601, C600
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H60f(0.33) H60g(0.33) H60h(0.66) H60i(0.66) C603(0.33) H60j(0.33)
 H60k(0.33) H60l(0.33) C604(0.67) H60m(0.67) H60n(0.67) H60o(0.67)
5.a Ternary CH refined with riding coordinates:
 C620(H620), C420(H420), C520(H520), C320(H320), C560(H560), C220(H220),
 C360(H360), C460(H460), C660(H660), C140(H140), C260(H260), C340(H340),
 C120(H120), C160(H160), C540(H540), C240(H240), C440(H440), C640(H640)
5.b Secondary CH2 refined with riding coordinates:
 C600(H60a,H60b), C602(H60f,H60g), C602(H60h,H60i)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C23(H23), C45(H45), C43(H43), C35(H35), C63(H63), C55(H55),
 C33(H33), C25(H25), C13(H13), C53(H53), C65(H65)
5.d Idealised Me refined as rotating group:
 C621(H62a,H62b,H62c), C321(H32a,H32b,H32c), C422(H42a,H42b,H42c), C322(H32d,
 H32e,H32f), C221(H22a,H22b,H22c), C362(H36a,H36b,H36c), C141(H14a,H14b,H14c),
 C561(H56a,H56b,H56c), C622(H62d,H62e,H62f), C661(H66a,H66b,H66c), C461(H46a,
 H46b,H46c), C421(H42d,H42e,H42f), C562(H56d,H56e,H56f), C162(H16a,H16b,H16c),
 C541(H54a,H54b,H54c), C161(H16d,H16e,H16f), C262(H26a,H26b,H26c), C361(H36d,
 H36e,H36f), C342(H34a,H34b,H34c), C601(H60c,H60d,H60e), C242(H24a,H24b,H24c),
 C142(H14d,H14e,H14f), C261(H26d,H26e,H26f), C341(H34d,H34e,H34f), C121(H12a,
 H12b,H12c), C441(H44a,H44b,H44c), C521(H52a,H52b,H52c), C462(H46d,H46e,H46f),
 C522(H52d,H52e,H52f), C122(H12d,H12e,H12f), C222(H22d,H22e,H22f), C241(H24d,
 H24e,H24f), C662(H66d,H66e,H66f), C641(H64a,H64b,H64c), C442(H44d,H44e,H44f),
 C542(H54d,H54e,H54f), C642(H64d,H64e,H64f), C603(H60j,H60k,H60l), C604(H60m,
 H60n,H60o)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.50446(2) 0.26521(2) 0.60971(2) 0.02797(10) Uani 1 1 d . . . . .
O3 O 0.5873(3) 0.32170(18) 0.6526(2) 0.0300(15) Uani 1 1 d . . . . .
O1 O 0.3828(3) 0.25830(18) 0.6404(2) 0.0311(14) Uani 1 1 d . . . . .
O2 O 0.5715(3) 0.19809(18) 0.6280(2) 0.0317(14) Uani 1 1 d . . . . .
O4 O 0.4681(4) 0.2951(2) 0.4915(3) 0.0457(16) Uani 1 1 d . . . . .
C11 C 0.2468(5) 0.2151(3) 0.6517(4) 0.021(2) Uani 1 1 d . . . . .
C621 C 0.6997(5) 0.2669(3) 0.5240(4) 0.048(2) Uani 1 1 d . . . . .
H62A H 0.642111 0.271245 0.524116 0.071 Uiso 1 1 calc GR . . . .
H62B H 0.714337 0.234442 0.536442 0.071 Uiso 1 1 calc GR . . . .
H62C H 0.713101 0.273210 0.480250 0.071 Uiso 1 1 calc GR . . . .
C620 C 0.7466(5) 0.3015(3) 0.5738(4) 0.035(2) Uani 1 1 d . . . . .
H620 H 0.735130 0.292785 0.618388 0.043 Uiso 1 1 calc R . . . .
C321 C 0.5577(5) 0.1721(3) 0.4439(4) 0.052(3) Uani 1 1 d . . . . .
H32A H 0.568641 0.203137 0.463733 0.077 Uiso 1 1 calc GR . . . .
H32B H 0.501489 0.170410 0.424367 0.077 Uiso 1 1 calc GR . . . .
H32C H 0.592090 0.167182 0.409953 0.077 Uiso 1 1 calc GR . . . .
C26 C 0.2591(5) 0.3049(3) 0.7602(4) 0.036(2) Uani 1 1 d . . . . .
C32 C 0.6627(5) 0.1346(3) 0.5301(4) 0.028(2) Uani 1 1 d . . . . .
C21 C 0.2786(5) 0.3062(3) 0.6949(4) 0.030(2) Uani 1 1 d . . . . .
C420 C 0.6358(5) 0.2087(3) 0.7816(4) 0.043(2) Uani 1 1 d . . . . .
H420 H 0.649297 0.220440 0.738867 0.051 Uiso 1 1 calc R . . . .
C15 C 0.2113(5) 0.1340(3) 0.6815(4) 0.031(2) Uani 1 1 d . . . . .
H15 H 0.227980 0.104258 0.699411 0.038 Uiso 1 1 calc R . . . .
C62 C 0.7194(5) 0.3538(3) 0.5603(4) 0.034(2) Uani 1 1 d . . . . .
C12 C 0.1637(5) 0.2212(3) 0.6277(4) 0.028(2) Uani 1 1 d . . . . .
C22 C 0.2693(5) 0.3506(3) 0.6606(4) 0.029(2) Uani 1 1 d . . . . .
C56 C 0.6101(6) 0.3864(3) 0.7825(4) 0.032(2) Uani 1 1 d . . . . .
C23 C 0.2390(5) 0.3902(3) 0.6903(4) 0.039(2) Uani 1 1 d . . . . .
H23 H 0.233636 0.419187 0.667223 0.047 Uiso 1 1 calc R . . . .
C31 C 0.6874(5) 0.1462(3) 0.5979(4) 0.027(2) Uani 1 1 d . . . . .
C52 C 0.7519(6) 0.3688(3) 0.7732(4) 0.036(2) Uani 1 1 d . . . . .
B1 B 0.3084(6) 0.2598(4) 0.6595(4) 0.028(2) Uani 1 1 d . . . . .
C51 C 0.6697(5) 0.3718(3) 0.7433(4) 0.026(2) Uani 1 1 d . . . . .
C45 C 0.5950(5) 0.0570(3) 0.7711(5) 0.042(3) Uani 1 1 d . . . . .
H45 H 0.585347 0.024069 0.769508 0.050 Uiso 1 1 calc R . . . .
C520 C 0.8212(6) 0.3555(3) 0.7359(4) 0.043(3) Uani 1 1 d . . . . .
H520 H 0.797027 0.343828 0.692012 0.052 Uiso 1 1 calc R . . . .
C320 C 0.5752(5) 0.1329(3) 0.4978(4) 0.038(2) Uani 1 1 d . . . . .
H320 H 0.540373 0.139056 0.532266 0.045 Uiso 1 1 calc R . . . .
C42 C 0.6224(5) 0.1554(3) 0.7751(4) 0.030(2) Uani 1 1 d . . . . .
C41 C 0.6138(5) 0.1316(3) 0.7130(4) 0.029(2) Uani 1 1 d . . . . .
C43 C 0.6170(5) 0.1284(3) 0.8321(4) 0.037(2) Uani 1 1 d . . . . .
H43 H 0.623272 0.144384 0.872798 0.045 Uiso 1 1 calc R . . . .
C560 C 0.5210(5) 0.3948(3) 0.7549(4) 0.041(2) Uani 1 1 d . . . . .
H560 H 0.516145 0.390847 0.706513 0.050 Uiso 1 1 calc R . . . .
C35 C 0.8276(6) 0.1349(3) 0.5809(4) 0.041(2) Uani 1 1 d . . . . .
H35 H 0.882651 0.135338 0.598298 0.049 Uiso 1 1 calc R . . . .
C422 C 0.5581(5) 0.2343(3) 0.7949(5) 0.067(3) Uani 1 1 d . . . . .
H42A H 0.515611 0.228760 0.758468 0.100 Uiso 1 1 calc GR . . . .
H42B H 0.568398 0.268161 0.799452 0.100 Uiso 1 1 calc GR . . . .
H42C H 0.541396 0.222155 0.835274 0.100 Uiso 1 1 calc GR . . . .
C16 C 0.2706(5) 0.1692(3) 0.6775(4) 0.030(2) Uani 1 1 d . . . . .
C36 C 0.7697(5) 0.1455(3) 0.6228(4) 0.028(2) Uani 1 1 d . . . . .
C14 C 0.1300(5) 0.1410(3) 0.6606(4) 0.033(2) Uani 1 1 d . . . . .
C322 C 0.5513(5) 0.0845(3) 0.4665(4) 0.057(3) Uani 1 1 d . . . . .
H32D H 0.493059 0.082936 0.455251 0.086 Uiso 1 1 calc GR . . . .
H32E H 0.569264 0.059354 0.497533 0.086 Uiso 1 1 calc GR . . . .
H32F H 0.576544 0.080484 0.426910 0.086 Uiso 1 1 calc GR . . . .
C44 C 0.6030(6) 0.0800(3) 0.8322(5) 0.048(3) Uani 1 1 d . . . . .
C61 C 0.6795(5) 0.3808(3) 0.6048(4) 0.033(2) Uani 1 1 d . . . . .
C220 C 0.2933(6) 0.3562(3) 0.5907(4) 0.037(2) Uani 1 1 d . . . . .
H220 H 0.302225 0.323999 0.573510 0.044 Uiso 1 1 calc R . . . .
C221 C 0.3735(6) 0.3839(3) 0.5942(4) 0.054(3) Uani 1 1 d . . . . .
H22A H 0.367365 0.414865 0.613874 0.081 Uiso 1 1 calc GR . . . .
H22B H 0.387398 0.388002 0.550111 0.081 Uiso 1 1 calc GR . . . .
H22C H 0.416062 0.366425 0.620884 0.081 Uiso 1 1 calc GR . . . .
C600 C 0.4049(6) 0.2759(3) 0.4441(5) 0.064(3) Uani 1 1 d . U . . .
H60A H 0.427605 0.266193 0.404462 0.077 Uiso 1 1 calc R . . . .
H60B H 0.364286 0.300514 0.431356 0.077 Uiso 1 1 calc R . . . .
C360 C 0.8018(5) 0.1569(3) 0.6950(4) 0.036(2) Uani 1 1 d . . . . .
H360 H 0.756575 0.171360 0.714561 0.043 Uiso 1 1 calc R . . . .
C63 C 0.7393(6) 0.3747(3) 0.5018(4) 0.044(3) Uani 1 1 d . . . . .
H63 H 0.766047 0.356555 0.472936 0.053 Uiso 1 1 calc R . . . .
C46 C 0.6009(5) 0.0816(3) 0.7117(4) 0.034(2) Uani 1 1 d . . . . .
C24 C 0.2165(5) 0.3879(3) 0.7534(5) 0.041(2) Uani 1 1 d . . . . .
C34 C 0.8057(6) 0.1235(3) 0.5140(4) 0.036(2) Uani 1 1 d . . . . .
C362 C 0.8718(5) 0.1926(3) 0.7045(4) 0.052(3) Uani 1 1 d . . . . .
H36A H 0.919077 0.178604 0.689398 0.078 Uiso 1 1 calc GR . . . .
H36B H 0.884203 0.200621 0.750856 0.078 Uiso 1 1 calc GR . . . .
H36C H 0.856475 0.221119 0.679304 0.078 Uiso 1 1 calc GR . . . .
C55 C 0.6330(6) 0.3957(3) 0.8498(5) 0.045(3) Uani 1 1 d . . . . .
H55 H 0.593024 0.404477 0.875571 0.054 Uiso 1 1 calc R . . . .
C460 C 0.5892(6) 0.0534(3) 0.6470(4) 0.043(3) Uani 1 1 d . . . . .
H460 H 0.580929 0.076574 0.610398 0.052 Uiso 1 1 calc R . . . .
C660 C 0.6201(6) 0.4625(3) 0.6332(5) 0.048(3) Uani 1 1 d . . . . .
H660 H 0.603107 0.442240 0.668384 0.057 Uiso 1 1 calc R . . . .
C140 C 0.0667(5) 0.1018(3) 0.6686(4) 0.041(2) Uani 1 1 d . . . . .
H140 H 0.012883 0.114485 0.650824 0.050 Uiso 1 1 calc R . . . .
C141 C 0.0821(6) 0.0574(3) 0.6278(5) 0.069(3) Uani 1 1 d . . . . .
H14A H 0.081740 0.066448 0.582000 0.103 Uiso 1 1 calc GR . . . .
H14B H 0.039958 0.034177 0.630946 0.103 Uiso 1 1 calc GR . . . .
H14C H 0.134173 0.043843 0.644621 0.103 Uiso 1 1 calc GR . . . .
C260 C 0.2730(5) 0.2593(3) 0.8017(4) 0.042(2) Uani 1 1 d . . . . .
H260 H 0.300522 0.236308 0.775832 0.050 Uiso 1 1 calc R . . . .
C33 C 0.7243(6) 0.1235(3) 0.4908(4) 0.033(2) Uani 1 1 d . . . . .
H33 H 0.708438 0.115645 0.446335 0.040 Uiso 1 1 calc R . . . .
C561 C 0.4621(5) 0.3586(3) 0.7803(4) 0.055(3) Uani 1 1 d . . . . .
H56A H 0.473048 0.327074 0.764684 0.082 Uiso 1 1 calc GR . . . .
H56B H 0.406842 0.367440 0.763833 0.082 Uiso 1 1 calc GR . . . .
H56C H 0.469559 0.358850 0.828063 0.082 Uiso 1 1 calc GR . . . .
C25 C 0.2280(5) 0.3453(3) 0.7887(4) 0.046(3) Uani 1 1 d . . . . .
H25 H 0.214890 0.343639 0.831789 0.055 Uiso 1 1 calc R . . . .
C622 C 0.8376(5) 0.2948(3) 0.5721(4) 0.061(3) Uani 1 1 d . . . . .
H62D H 0.851920 0.261761 0.580696 0.092 Uiso 1 1 calc GR . . . .
H62E H 0.867740 0.314680 0.605490 0.092 Uiso 1 1 calc GR . . . .
H62F H 0.850536 0.303712 0.528997 0.092 Uiso 1 1 calc GR . . . .
C661 C 0.5437(6) 0.4850(4) 0.5977(5) 0.078(4) Uani 1 1 d . . . . .
H66A H 0.557698 0.507268 0.564960 0.117 Uiso 1 1 calc GR . . . .
H66B H 0.515555 0.501588 0.629243 0.117 Uiso 1 1 calc GR . . . .
H66C H 0.508878 0.460387 0.576088 0.117 Uiso 1 1 calc GR . . . .
C13 C 0.1073(5) 0.1846(3) 0.6322(4) 0.037(2) Uani 1 1 d . . . . .
H13 H 0.052809 0.189882 0.615597 0.044 Uiso 1 1 calc R . . . .
C53 C 0.7712(5) 0.3788(3) 0.8405(4) 0.042(2) Uani 1 1 d . . . . .
H53 H 0.825244 0.376452 0.860164 0.051 Uiso 1 1 calc R . . . .
C461 C 0.5157(6) 0.0205(3) 0.6399(4) 0.062(3) Uani 1 1 d . . . . .
H46A H 0.525777 -0.005799 0.670624 0.092 Uiso 1 1 calc GR . . . .
H46B H 0.505875 0.008252 0.595259 0.092 Uiso 1 1 calc GR . . . .
H46C H 0.468696 0.038071 0.649408 0.092 Uiso 1 1 calc GR . . . .
C66 C 0.6625(5) 0.4291(3) 0.5884(4) 0.040(2) Uani 1 1 d . . . . .
C421 C 0.7054(5) 0.2230(3) 0.8350(4) 0.051(3) Uani 1 1 d . . . . .
H42D H 0.692905 0.213094 0.877811 0.077 Uiso 1 1 calc GR . . . .
H42E H 0.712318 0.257193 0.834562 0.077 Uiso 1 1 calc GR . . . .
H42F H 0.754826 0.207673 0.826234 0.077 Uiso 1 1 calc GR . . . .
C340 C 0.8697(6) 0.1112(4) 0.4685(4) 0.049(3) Uani 1 1 d . . . . .
H340 H 0.844507 0.116924 0.422520 0.059 Uiso 1 1 calc R . . . .
C54 C 0.7118(6) 0.3924(3) 0.8794(4) 0.049(3) Uani 1 1 d . . . . .
B3 B 0.6443(6) 0.3568(4) 0.6676(5) 0.036(3) Uani 1 1 d . . . . .
C562 C 0.4929(6) 0.4460(3) 0.7680(4) 0.058(3) Uani 1 1 d . . . . .
H56D H 0.487728 0.449508 0.814343 0.088 Uiso 1 1 calc GR . . . .
H56E H 0.441048 0.451954 0.741691 0.088 Uiso 1 1 calc GR . . . .
H56F H 0.532350 0.468569 0.756126 0.088 Uiso 1 1 calc GR . . . .
C120 C 0.1301(5) 0.2671(3) 0.5933(4) 0.042(2) Uani 1 1 d . . . . .
H120 H 0.176898 0.288336 0.590972 0.050 Uiso 1 1 calc R . . . .
C160 C 0.3596(6) 0.1565(3) 0.6971(5) 0.048(3) Uani 1 1 d . . . . .
H160 H 0.389502 0.186741 0.705733 0.058 Uiso 1 1 calc R . . . .
C64 C 0.7200(7) 0.4215(4) 0.4864(5) 0.061(3) Uani 1 1 d . . . . .
C65 C 0.6823(6) 0.4481(3) 0.5298(5) 0.054(3) Uani 1 1 d . . . . .
H65 H 0.669591 0.480030 0.519655 0.065 Uiso 1 1 calc R . . . .
C162 C 0.3918(6) 0.1323(3) 0.6379(5) 0.071(3) Uani 1 1 d . . . . .
H16A H 0.362642 0.102911 0.627248 0.107 Uiso 1 1 calc GR . . . .
H16B H 0.448910 0.125566 0.649283 0.107 Uiso 1 1 calc GR . . . .
H16C H 0.383899 0.153394 0.600065 0.107 Uiso 1 1 calc GR . . . .
B2 B 0.6214(6) 0.1607(3) 0.6452(5) 0.029(3) Uani 1 1 d . . . . .
C540 C 0.7353(8) 0.4005(5) 0.9552(6) 0.092(3) Uani 1 1 d . . . . .
H540 H 0.794907 0.398354 0.964514 0.110 Uiso 1 1 calc R . . . .
C541 C 0.7022(7) 0.3612(4) 0.9923(5) 0.082(4) Uani 1 1 d . . . . .
H54A H 0.643748 0.360674 0.982080 0.123 Uiso 1 1 calc GR . . . .
H54B H 0.717288 0.366154 1.039229 0.123 Uiso 1 1 calc GR . . . .
H54C H 0.723967 0.331100 0.979711 0.123 Uiso 1 1 calc GR . . . .
C240 C 0.1780(6) 0.4309(3) 0.7839(5) 0.056(3) Uani 1 1 d . . . . .
H240 H 0.161059 0.420336 0.826067 0.067 Uiso 1 1 calc R . . . .
C161 C 0.3774(6) 0.1265(3) 0.7585(5) 0.088(4) Uani 1 1 d . . . . .
H16D H 0.357046 0.142354 0.794954 0.132 Uiso 1 1 calc GR . . . .
H16E H 0.435345 0.122091 0.769020 0.132 Uiso 1 1 calc GR . . . .
H16F H 0.351361 0.095823 0.751054 0.132 Uiso 1 1 calc GR . . . .
C262 C 0.3289(6) 0.2679(3) 0.8670(4) 0.062(3) Uani 1 1 d . . . . .
H26A H 0.378677 0.282645 0.857929 0.093 Uiso 1 1 calc GR . . . .
H26B H 0.341137 0.237766 0.889201 0.093 Uiso 1 1 calc GR . . . .
H26C H 0.302139 0.288622 0.895079 0.093 Uiso 1 1 calc GR . . . .
C440 C 0.5964(8) 0.0530(4) 0.8962(5) 0.075(4) Uani 1 1 d . . . . .
H440 H 0.646738 0.060041 0.926101 0.090 Uiso 1 1 calc R . . . .
C361 C 0.8260(6) 0.1113(3) 0.7346(4) 0.059(3) Uani 1 1 d . . . . .
H36D H 0.778130 0.092541 0.738249 0.088 Uiso 1 1 calc GR . . . .
H36E H 0.852107 0.119754 0.778302 0.088 Uiso 1 1 calc GR . . . .
H36F H 0.863099 0.092900 0.712148 0.088 Uiso 1 1 calc GR . . . .
C342 C 0.8897(7) 0.0586(4) 0.4748(5) 0.089(4) Uani 1 1 d . . . . .
H34A H 0.908190 0.050973 0.520545 0.133 Uiso 1 1 calc GR . . . .
H34B H 0.931879 0.051045 0.448264 0.133 Uiso 1 1 calc GR . . . .
H34C H 0.841775 0.040071 0.459481 0.133 Uiso 1 1 calc GR . . . .
C601 C 0.3645(6) 0.2330(4) 0.4723(4) 0.070(3) Uani 1 1 d . U . . .
H60C H 0.323676 0.220017 0.438803 0.106 Uiso 1 1 calc GR . . . .
H60D H 0.339492 0.242920 0.510050 0.106 Uiso 1 1 calc GR . . . .
H60E H 0.404931 0.208877 0.485789 0.106 Uiso 1 1 calc GR . . . .
C602 C 0.5066(7) 0.3372(4) 0.4680(5) 0.073(4) Uani 1 1 d . . . . .
H60F H 0.526799 0.355056 0.507984 0.087 Uiso 0.33 1 calc R . P A 1
H60G H 0.554664 0.325198 0.450769 0.087 Uiso 0.33 1 calc R . P A 1
H60H H 0.467578 0.363344 0.465046 0.087 Uiso 0.66 1 calc R . P B 2
H60I H 0.552022 0.346031 0.501337 0.087 Uiso 0.66 1 calc R . P B 2
C242 C 0.2383(7) 0.4716(3) 0.7993(5) 0.088(4) Uani 1 1 d . . . . .
H24A H 0.287391 0.459640 0.824664 0.132 Uiso 1 1 calc GR . . . .
H24B H 0.214755 0.495832 0.824511 0.132 Uiso 1 1 calc GR . . . .
H24C H 0.250818 0.485276 0.758390 0.132 Uiso 1 1 calc GR . . . .
C142 C 0.0651(7) 0.0897(4) 0.7406(5) 0.088(4) Uani 1 1 d . . . . .
H14D H 0.117348 0.077335 0.759500 0.132 Uiso 1 1 calc GR . . . .
H14E H 0.023789 0.066011 0.744077 0.132 Uiso 1 1 calc GR . . . .
H14F H 0.053127 0.118157 0.764237 0.132 Uiso 1 1 calc GR . . . .
C261 C 0.1920(6) 0.2367(3) 0.8136(4) 0.065(3) Uani 1 1 d . . . . .
H26D H 0.166807 0.256197 0.844066 0.098 Uiso 1 1 calc GR . . . .
H26E H 0.201818 0.205128 0.831971 0.098 Uiso 1 1 calc GR . . . .
H26F H 0.156390 0.234478 0.772053 0.098 Uiso 1 1 calc GR . . . .
C341 C 0.9455(6) 0.1421(4) 0.4807(5) 0.072(3) Uani 1 1 d . . . . .
H34D H 0.930297 0.175345 0.476863 0.108 Uiso 1 1 calc GR . . . .
H34E H 0.980873 0.134559 0.448312 0.108 Uiso 1 1 calc GR . . . .
H34F H 0.973449 0.135971 0.524561 0.108 Uiso 1 1 calc GR . . . .
C121 C 0.0903(6) 0.2589(3) 0.5222(4) 0.074(3) Uani 1 1 d . . . . .
H12A H 0.127111 0.241577 0.498200 0.111 Uiso 1 1 calc GR . . . .
H12B H 0.077387 0.289282 0.500998 0.111 Uiso 1 1 calc GR . . . .
H12C H 0.041061 0.240625 0.522419 0.111 Uiso 1 1 calc GR . . . .
C441 C 0.5901(9) 0.0009(4) 0.8932(6) 0.128(6) Uani 1 1 d . . . . .
H44A H 0.543384 -0.008015 0.862138 0.192 Uiso 1 1 calc GR . . . .
H44B H 0.584111 -0.011349 0.936528 0.192 Uiso 1 1 calc GR . . . .
H44C H 0.638531 -0.012150 0.879003 0.192 Uiso 1 1 calc GR . . . .
C521 C 0.8753(7) 0.3164(4) 0.7677(5) 0.085(4) Uani 1 1 d . . . . .
H52A H 0.901225 0.326887 0.810557 0.128 Uiso 1 1 calc GR . . . .
H52B H 0.916238 0.308906 0.739964 0.128 Uiso 1 1 calc GR . . . .
H52C H 0.843196 0.288276 0.772959 0.128 Uiso 1 1 calc GR . . . .
C462 C 0.6653(6) 0.0240(3) 0.6386(5) 0.069(3) Uani 1 1 d . . . . .
H46D H 0.711321 0.045036 0.639348 0.104 Uiso 1 1 calc GR . . . .
H46E H 0.656603 0.007239 0.596775 0.104 Uiso 1 1 calc GR . . . .
H46F H 0.675564 0.001166 0.674238 0.104 Uiso 1 1 calc GR . . . .
C522 C 0.8728(7) 0.3983(4) 0.7248(6) 0.099(5) Uani 1 1 d . . . . .
H52D H 0.839800 0.421876 0.699099 0.148 Uiso 1 1 calc GR . . . .
H52E H 0.916494 0.388545 0.701091 0.148 Uiso 1 1 calc GR . . . .
H52F H 0.894992 0.411817 0.766925 0.148 Uiso 1 1 calc GR . . . .
C122 C 0.0716(6) 0.2940(3) 0.6332(5) 0.071(3) Uani 1 1 d . . . . .
H12D H 0.022967 0.275291 0.633976 0.106 Uiso 1 1 calc GR . . . .
H12E H 0.057516 0.324429 0.612489 0.106 Uiso 1 1 calc GR . . . .
H12F H 0.097740 0.299061 0.677893 0.106 Uiso 1 1 calc GR . . . .
C222 C 0.2268(6) 0.3809(3) 0.5415(4) 0.062(3) Uani 1 1 d . . . . .
H22D H 0.176422 0.363581 0.540061 0.093 Uiso 1 1 calc GR . . . .
H22E H 0.243323 0.381341 0.497909 0.093 Uiso 1 1 calc GR . . . .
H22F H 0.219294 0.413257 0.555891 0.093 Uiso 1 1 calc GR . . . .
C241 C 0.1043(7) 0.4487(4) 0.7407(6) 0.121(6) Uani 1 1 d . . . . .
H24D H 0.118755 0.457844 0.698151 0.181 Uiso 1 1 calc GR . . . .
H24E H 0.082537 0.475920 0.761240 0.181 Uiso 1 1 calc GR . . . .
H24F H 0.063932 0.423679 0.734622 0.181 Uiso 1 1 calc GR . . . .
C662 C 0.6784(7) 0.4991(4) 0.6677(6) 0.108(5) Uani 1 1 d . . . . .
H66D H 0.693793 0.521364 0.635441 0.162 Uiso 1 1 calc GR . . . .
H66E H 0.726243 0.483157 0.689441 0.162 Uiso 1 1 calc GR . . . .
H66F H 0.652332 0.516149 0.700139 0.162 Uiso 1 1 calc GR . . . .
C641 C 0.6785(9) 0.4731(5) 0.3867(7) 0.157(7) Uani 1 1 d . . . . .
H64A H 0.626204 0.457563 0.381180 0.235 Uiso 1 1 calc GR . . . .
H64B H 0.691490 0.483005 0.344025 0.235 Uiso 1 1 calc GR . . . .
H64C H 0.676992 0.500690 0.414882 0.235 Uiso 1 1 calc GR . . . .
C442 C 0.5289(9) 0.0735(5) 0.9288(6) 0.149(7) Uani 1 1 d . . . . .
H44D H 0.536315 0.107529 0.933857 0.224 Uiso 1 1 calc GR . . . .
H44E H 0.529002 0.059001 0.971765 0.224 Uiso 1 1 calc GR . . . .
H44F H 0.477637 0.067142 0.901729 0.224 Uiso 1 1 calc GR . . . .
C640 C 0.7396(9) 0.4403(5) 0.4166(6) 0.092(3) Uani 1 1 d . . . . .
H640 H 0.739627 0.412508 0.386981 0.110 Uiso 1 1 calc R . . . .
C542 C 0.7130(10) 0.4475(5) 0.9756(6) 0.147(7) Uani 1 1 d . . . . .
H54D H 0.738094 0.471291 0.950796 0.220 Uiso 1 1 calc GR . . . .
H54E H 0.731392 0.451568 1.022276 0.220 Uiso 1 1 calc GR . . . .
H54F H 0.654771 0.450985 0.967365 0.220 Uiso 1 1 calc GR . . . .
C642 C 0.8132(10) 0.4595(8) 0.4233(8) 0.254(13) Uani 1 1 d . . . . .
H64D H 0.812826 0.489376 0.446904 0.381 Uiso 1 1 calc GR . . . .
H64E H 0.828829 0.465212 0.380055 0.381 Uiso 1 1 calc GR . . . .
H64F H 0.851515 0.437960 0.447728 0.381 Uiso 1 1 calc GR . . . .
C603 C 0.477(3) 0.3688(12) 0.4262(19) 0.113(17) Uani 0.33 1 d . . P C 1
H60J H 0.470352 0.355329 0.382195 0.170 Uiso 0.33 1 calc GR . P C 1
H60K H 0.513093 0.395815 0.428126 0.170 Uiso 0.33 1 calc GR . P C 1
H60L H 0.424690 0.378978 0.436786 0.170 Uiso 0.33 1 calc GR . P C 1
C604 C 0.5360(9) 0.3332(6) 0.4062(7) 0.064(5) Uani 0.67 1 d . . P C 2
H60M H 0.575033 0.307556 0.408104 0.095 Uiso 0.67 1 calc GR . P C 2
H60N H 0.561700 0.362786 0.396341 0.095 Uiso 0.67 1 calc GR . P C 2
H60O H 0.491310 0.326602 0.371906 0.095 Uiso 0.67 1 calc GR . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O3 2.187(5) . ?
U1 O1 2.195(5) . ?
U1 O2 2.179(5) . ?
U1 O4 2.530(5) . ?
O3 B3 1.362(11) . ?
O1 B1 1.339(10) . ?
O2 B2 1.344(10) . ?
O4 C600 1.423(9) . ?
O4 C602 1.445(10) . ?
C11 C12 1.402(10) . ?
C11 B1 1.603(12) . ?
C11 C16 1.417(10) . ?
C621 H62A 0.9600 . ?
C621 H62B 0.9600 . ?
C621 H62C 0.9600 . ?
C621 C620 1.527(10) . ?
C620 H620 0.9800 . ?
C620 C62 1.538(10) . ?
C620 C622 1.520(11) . ?
C321 H32A 0.9600 . ?
C321 H32B 0.9600 . ?
C321 H32C 0.9600 . ?
C321 C320 1.545(10) . ?
C26 C21 1.405(10) . ?
C26 C260 1.522(11) . ?
C26 C25 1.396(11) . ?
C32 C31 1.416(10) . ?
C32 C320 1.505(11) . ?
C32 C33 1.410(11) . ?
C21 C22 1.416(10) . ?
C21 B1 1.590(12) . ?
C420 H420 0.9800 . ?
C420 C42 1.506(10) . ?
C420 C422 1.526(11) . ?
C420 C421 1.520(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.398(11) . ?
C15 C14 1.367(10) . ?
C62 C61 1.408(11) . ?
C62 C63 1.401(10) . ?
C12 C13 1.393(10) . ?
C12 C120 1.524(10) . ?
C22 C23 1.385(10) . ?
C22 C220 1.530(11) . ?
C56 C51 1.408(11) . ?
C56 C560 1.521(11) . ?
C56 C55 1.390(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.382(11) . ?
C31 C36 1.385(10) . ?
C31 B2 1.601(12) . ?
C52 C51 1.412(11) . ?
C52 C520 1.503(11) . ?
C52 C53 1.385(10) . ?
C51 B3 1.591(13) . ?
C45 H45 0.9300 . ?
C45 C44 1.383(11) . ?
C45 C46 1.402(10) . ?
C520 H520 0.9800 . ?
C520 C521 1.498(11) . ?
C520 C522 1.501(11) . ?
C320 H320 0.9800 . ?
C320 C322 1.520(10) . ?
C42 C41 1.411(10) . ?
C42 C43 1.390(10) . ?
C41 C46 1.411(10) . ?
C41 B2 1.615(12) . ?
C43 H43 0.9300 . ?
C43 C44 1.369(10) . ?
C560 H560 0.9800 . ?
C560 C561 1.537(11) . ?
C560 C562 1.534(10) . ?
C35 H35 0.9300 . ?
C35 C36 1.396(10) . ?
C35 C34 1.391(11) . ?
C422 H42A 0.9600 . ?
C422 H42B 0.9600 . ?
C422 H42C 0.9600 . ?
C16 C160 1.512(11) . ?
C36 C360 1.521(10) . ?
C14 C140 1.537(10) . ?
C14 C13 1.374(10) . ?
C322 H32D 0.9600 . ?
C322 H32E 0.9600 . ?
C322 H32F 0.9600 . ?
C44 C440 1.517(12) . ?
C61 C66 1.404(11) . ?
C61 B3 1.614(12) . ?
C220 H220 0.9800 . ?
C220 C221 1.528(11) . ?
C220 C222 1.542(11) . ?
C221 H22A 0.9600 . ?
C221 H22B 0.9600 . ?
C221 H22C 0.9600 . ?
C600 H60A 0.9700 . ?
C600 H60B 0.9700 . ?
C600 C601 1.519(11) . ?
C360 H360 0.9800 . ?
C360 C362 1.519(10) . ?
C360 C361 1.526(10) . ?
C63 H63 0.9300 . ?
C63 C64 1.368(11) . ?
C46 C460 1.518(11) . ?
C24 C25 1.384(11) . ?
C24 C240 1.526(11) . ?
C34 C33 1.363(11) . ?
C34 C340 1.535(11) . ?
C362 H36A 0.9600 . ?
C362 H36B 0.9600 . ?
C362 H36C 0.9600 . ?
C55 H55 0.9300 . ?
C55 C54 1.360(12) . ?
C460 H460 0.9800 . ?
C460 C461 1.514(11) . ?
C460 C462 1.529(11) . ?
C660 H660 0.9800 . ?
C660 C661 1.504(11) . ?
C660 C66 1.535(11) . ?
C660 C662 1.508(12) . ?
C140 H140 0.9800 . ?
C140 C141 1.528(11) . ?
C140 C142 1.501(11) . ?
C141 H14A 0.9600 . ?
C141 H14B 0.9600 . ?
C141 H14C 0.9600 . ?
C260 H260 0.9800 . ?
C260 C262 1.527(10) . ?
C260 C261 1.529(10) . ?
C33 H33 0.9300 . ?
C561 H56A 0.9600 . ?
C561 H56B 0.9600 . ?
C561 H56C 0.9600 . ?
C25 H25 0.9300 . ?
C622 H62D 0.9600 . ?
C622 H62E 0.9600 . ?
C622 H62F 0.9600 . ?
C661 H66A 0.9600 . ?
C661 H66B 0.9600 . ?
C661 H66C 0.9600 . ?
C13 H13 0.9300 . ?
C53 H53 0.9300 . ?
C53 C54 1.393(11) . ?
C461 H46A 0.9600 . ?
C461 H46B 0.9600 . ?
C461 H46C 0.9600 . ?
C66 C65 1.380(11) . ?
C421 H42D 0.9600 . ?
C421 H42E 0.9600 . ?
C421 H42F 0.9600 . ?
C340 H340 0.9800 . ?
C340 C342 1.506(11) . ?
C340 C341 1.512(12) . ?
C54 C540 1.550(14) . ?
C562 H56D 0.9600 . ?
C562 H56E 0.9600 . ?
C562 H56F 0.9600 . ?
C120 H120 0.9800 . ?
C120 C121 1.518(10) . ?
C120 C122 1.539(11) . ?
C160 H160 0.9800 . ?
C160 C162 1.535(12) . ?
C160 C161 1.494(11) . ?
C64 C65 1.364(12) . ?
C64 C640 1.584(13) . ?
C65 H65 0.9300 . ?
C162 H16A 0.9600 . ?
C162 H16B 0.9600 . ?
C162 H16C 0.9600 . ?
C540 H540 0.9800 . ?
C540 C541 1.475(12) . ?
C540 C542 1.435(14) . ?
C541 H54A 0.9600 . ?
C541 H54B 0.9600 . ?
C541 H54C 0.9600 . ?
C240 H240 0.9800 . ?
C240 C242 1.514(12) . ?
C240 C241 1.486(13) . ?
C161 H16D 0.9600 . ?
C161 H16E 0.9600 . ?
C161 H16F 0.9600 . ?
C262 H26A 0.9600 . ?
C262 H26B 0.9600 . ?
C262 H26C 0.9600 . ?
C440 H440 0.9800 . ?
C440 C441 1.455(13) . ?
C440 C442 1.486(15) . ?
C361 H36D 0.9600 . ?
C361 H36E 0.9600 . ?
C361 H36F 0.9600 . ?
C342 H34A 0.9600 . ?
C342 H34B 0.9600 . ?
C342 H34C 0.9600 . ?
C601 H60C 0.9600 . ?
C601 H60D 0.9600 . ?
C601 H60E 0.9600 . ?
C602 H60F 0.9700 . ?
C602 H60G 0.9700 . ?
C602 H60H 0.9700 . ?
C602 H60I 0.9700 . ?
C602 C603 1.27(3) . ?
C602 C604 1.410(15) . ?
C242 H24A 0.9600 . ?
C242 H24B 0.9600 . ?
C242 H24C 0.9600 . ?
C142 H14D 0.9600 . ?
C142 H14E 0.9600 . ?
C142 H14F 0.9600 . ?
C261 H26D 0.9600 . ?
C261 H26E 0.9600 . ?
C261 H26F 0.9600 . ?
C341 H34D 0.9600 . ?
C341 H34E 0.9600 . ?
C341 H34F 0.9600 . ?
C121 H12A 0.9600 . ?
C121 H12B 0.9600 . ?
C121 H12C 0.9600 . ?
C441 H44A 0.9600 . ?
C441 H44B 0.9600 . ?
C441 H44C 0.9600 . ?
C521 H52A 0.9600 . ?
C521 H52B 0.9600 . ?
C521 H52C 0.9600 . ?
C462 H46D 0.9600 . ?
C462 H46E 0.9600 . ?
C462 H46F 0.9600 . ?
C522 H52D 0.9600 . ?
C522 H52E 0.9600 . ?
C522 H52F 0.9600 . ?
C122 H12D 0.9600 . ?
C122 H12E 0.9600 . ?
C122 H12F 0.9600 . ?
C222 H22D 0.9600 . ?
C222 H22E 0.9600 . ?
C222 H22F 0.9600 . ?
C241 H24D 0.9600 . ?
C241 H24E 0.9600 . ?
C241 H24F 0.9600 . ?
C662 H66D 0.9600 . ?
C662 H66E 0.9600 . ?
C662 H66F 0.9600 . ?
C641 H64A 0.9600 . ?
C641 H64B 0.9600 . ?
C641 H64C 0.9600 . ?
C641 C640 1.432(15) . ?
C442 H44D 0.9600 . ?
C442 H44E 0.9600 . ?
C442 H44F 0.9600 . ?
C640 H640 0.9800 . ?
C640 C642 1.320(17) . ?
C542 H54D 0.9600 . ?
C542 H54E 0.9600 . ?
C542 H54F 0.9600 . ?
C642 H64D 0.9600 . ?
C642 H64E 0.9600 . ?
C642 H64F 0.9600 . ?
C603 H60J 0.9600 . ?
C603 H60K 0.9600 . ?
C603 H60L 0.9600 . ?
C604 H60M 0.9600 . ?
C604 H60N 0.9600 . ?
C604 H60O 0.9600 . ?

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
O3 U1 O1 119.92(19) . . ?
O3 U1 O4 101.22(18) . . ?
O1 U1 O4 100.95(18) . . ?
O2 U1 O3 105.86(19) . . ?
O2 U1 O1 109.96(19) . . ?
O2 U1 O4 119.48(18) . . ?
B3 O3 U1 168.8(6) . . ?
B1 O1 U1 173.2(6) . . ?
B2 O2 U1 171.2(5) . . ?
C600 O4 U1 125.0(5) . . ?
C600 O4 C602 113.5(7) . . ?
C602 O4 U1 121.3(5) . . ?
C12 C11 B1 121.3(7) . . ?
C12 C11 C16 116.6(7) . . ?
C16 C11 B1 121.5(7) . . ?
H62A C621 H62B 109.5 . . ?
H62A C621 H62C 109.5 . . ?
H62B C621 H62C 109.5 . . ?
C620 C621 H62A 109.5 . . ?
C620 C621 H62B 109.5 . . ?
C620 C621 H62C 109.5 . . ?
C621 C620 H620 108.0 . . ?
C621 C620 C62 111.7(7) . . ?
C62 C620 H620 108.0 . . ?
C622 C620 C621 108.8(7) . . ?
C622 C620 H620 108.0 . . ?
C622 C620 C62 112.2(7) . . ?
H32A C321 H32B 109.5 . . ?
H32A C321 H32C 109.5 . . ?
H32B C321 H32C 109.5 . . ?
C320 C321 H32A 109.5 . . ?
C320 C321 H32B 109.5 . . ?
C320 C321 H32C 109.5 . . ?
C21 C26 C260 120.5(8) . . ?
C25 C26 C21 120.8(8) . . ?
C25 C26 C260 118.7(8) . . ?
C31 C32 C320 124.1(8) . . ?
C33 C32 C31 117.6(8) . . ?
C33 C32 C320 118.2(8) . . ?
C26 C21 C22 117.6(8) . . ?
C26 C21 B1 121.9(7) . . ?
C22 C21 B1 120.5(8) . . ?
C42 C420 H420 107.5 . . ?
C42 C420 C422 111.1(7) . . ?
C42 C420 C421 114.1(7) . . ?
C422 C420 H420 107.5 . . ?
C421 C420 H420 107.5 . . ?
C421 C420 C422 109.0(7) . . ?
C16 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C14 C15 C16 123.3(8) . . ?
C61 C62 C620 123.0(8) . . ?
C63 C62 C620 116.7(8) . . ?
C63 C62 C61 120.3(8) . . ?
C11 C12 C120 122.6(7) . . ?
C13 C12 C11 121.4(7) . . ?
C13 C12 C120 116.0(8) . . ?
C21 C22 C220 121.3(8) . . ?
C23 C22 C21 120.2(8) . . ?
C23 C22 C220 118.5(8) . . ?
C51 C56 C560 123.8(8) . . ?
C55 C56 C51 119.4(9) . . ?
C55 C56 C560 116.8(8) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.6(8) . . ?
C24 C23 H23 119.2 . . ?
C32 C31 B2 120.7(8) . . ?
C36 C31 C32 119.2(8) . . ?
C36 C31 B2 120.1(8) . . ?
C51 C52 C520 123.6(8) . . ?
C53 C52 C51 119.3(9) . . ?
C53 C52 C520 117.1(8) . . ?
O1 B1 C11 122.9(8) . . ?
O1 B1 C21 120.6(8) . . ?
C21 B1 C11 116.4(7) . . ?
C56 C51 C52 118.7(8) . . ?
C56 C51 B3 120.5(8) . . ?
C52 C51 B3 120.7(8) . . ?
C44 C45 H45 118.9 . . ?
C44 C45 C46 122.2(8) . . ?
C46 C45 H45 118.9 . . ?
C52 C520 H520 107.2 . . ?
C521 C520 C52 114.5(8) . . ?
C521 C520 H520 107.2 . . ?
C521 C520 C522 108.9(9) . . ?
C522 C520 C52 111.6(8) . . ?
C522 C520 H520 107.2 . . ?
C321 C320 H320 108.0 . . ?
C32 C320 C321 111.1(7) . . ?
C32 C320 H320 108.0 . . ?
C32 C320 C322 113.0(7) . . ?
C322 C320 C321 108.6(7) . . ?
C322 C320 H320 108.0 . . ?
C41 C42 C420 122.4(8) . . ?
C43 C42 C420 119.0(8) . . ?
C43 C42 C41 118.6(8) . . ?
C42 C41 C46 118.4(8) . . ?
C42 C41 B2 120.9(7) . . ?
C46 C41 B2 120.6(7) . . ?
C42 C43 H43 117.9 . . ?
C44 C43 C42 124.2(8) . . ?
C44 C43 H43 117.9 . . ?
C56 C560 H560 107.0 . . ?
C56 C560 C561 113.7(7) . . ?
C56 C560 C562 112.4(7) . . ?
C561 C560 H560 107.0 . . ?
C562 C560 H560 107.0 . . ?
C562 C560 C561 109.3(7) . . ?
C36 C35 H35 118.9 . . ?
C34 C35 H35 118.9 . . ?
C34 C35 C36 122.1(9) . . ?
C420 C422 H42A 109.5 . . ?
C420 C422 H42B 109.5 . . ?
C420 C422 H42C 109.5 . . ?
H42A C422 H42B 109.5 . . ?
H42A C422 H42C 109.5 . . ?
H42B C422 H42C 109.5 . . ?
C11 C16 C160 121.3(8) . . ?
C15 C16 C11 119.6(8) . . ?
C15 C16 C160 119.0(8) . . ?
C31 C36 C35 120.2(8) . . ?
C31 C36 C360 123.0(8) . . ?
C35 C36 C360 116.8(8) . . ?
C15 C14 C140 121.3(8) . . ?
C15 C14 C13 117.2(8) . . ?
C13 C14 C140 121.5(8) . . ?
C320 C322 H32D 109.5 . . ?
C320 C322 H32E 109.5 . . ?
C320 C322 H32F 109.5 . . ?
H32D C322 H32E 109.5 . . ?
H32D C322 H32F 109.5 . . ?
H32E C322 H32F 109.5 . . ?
C45 C44 C440 121.8(9) . . ?
C43 C44 C45 116.9(8) . . ?
C43 C44 C440 121.4(9) . . ?
C62 C61 B3 122.3(8) . . ?
C66 C61 C62 117.2(8) . . ?
C66 C61 B3 120.1(8) . . ?
C22 C220 H220 107.9 . . ?
C22 C220 C222 113.1(7) . . ?
C221 C220 C22 110.0(7) . . ?
C221 C220 H220 107.9 . . ?
C221 C220 C222 109.9(7) . . ?
C222 C220 H220 107.9 . . ?
C220 C221 H22A 109.5 . . ?
C220 C221 H22B 109.5 . . ?
C220 C221 H22C 109.5 . . ?
H22A C221 H22B 109.5 . . ?
H22A C221 H22C 109.5 . . ?
H22B C221 H22C 109.5 . . ?
O4 C600 H60A 109.4 . . ?
O4 C600 H60B 109.4 . . ?
O4 C600 C601 111.2(7) . . ?
H60A C600 H60B 108.0 . . ?
C601 C600 H60A 109.4 . . ?
C601 C600 H60B 109.4 . . ?
C36 C360 H360 106.8 . . ?
C36 C360 C361 111.4(7) . . ?
C362 C360 C36 114.7(7) . . ?
C362 C360 H360 106.8 . . ?
C362 C360 C361 109.7(7) . . ?
C361 C360 H360 106.8 . . ?
C62 C63 H63 119.5 . . ?
C64 C63 C62 121.0(8) . . ?
C64 C63 H63 119.5 . . ?
C45 C46 C41 119.7(8) . . ?
C45 C46 C460 118.3(8) . . ?
C41 C46 C460 122.0(8) . . ?
C23 C24 C25 118.9(8) . . ?
C23 C24 C240 121.2(9) . . ?
C25 C24 C240 119.9(8) . . ?
C35 C34 C340 121.9(9) . . ?
C33 C34 C35 116.7(9) . . ?
C33 C34 C340 121.4(8) . . ?
C360 C362 H36A 109.5 . . ?
C360 C362 H36B 109.5 . . ?
C360 C362 H36C 109.5 . . ?
H36A C362 H36B 109.5 . . ?
H36A C362 H36C 109.5 . . ?
H36B C362 H36C 109.5 . . ?
C56 C55 H55 118.8 . . ?
C54 C55 C56 122.4(9) . . ?
C54 C55 H55 118.8 . . ?
C46 C460 H460 107.5 . . ?
C46 C460 C462 111.4(8) . . ?
C461 C460 C46 113.6(7) . . ?
C461 C460 H460 107.5 . . ?
C461 C460 C462 109.1(7) . . ?
C462 C460 H460 107.5 . . ?
C661 C660 H660 106.4 . . ?
C661 C660 C66 113.0(8) . . ?
C661 C660 C662 112.5(9) . . ?
C66 C660 H660 106.4 . . ?
C662 C660 H660 106.4 . . ?
C662 C660 C66 111.7(8) . . ?
C14 C140 H140 107.6 . . ?
C141 C140 C14 110.5(7) . . ?
C141 C140 H140 107.6 . . ?
C142 C140 C14 111.5(7) . . ?
C142 C140 H140 107.6 . . ?
C142 C140 C141 111.9(8) . . ?
C140 C141 H14A 109.5 . . ?
C140 C141 H14B 109.5 . . ?
C140 C141 H14C 109.5 . . ?
H14A C141 H14B 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
C26 C260 H260 107.2 . . ?
C26 C260 C262 112.2(7) . . ?
C26 C260 C261 111.2(7) . . ?
C262 C260 H260 107.2 . . ?
C262 C260 C261 111.6(7) . . ?
C261 C260 H260 107.2 . . ?
C32 C33 H33 118.0 . . ?
C34 C33 C32 124.1(8) . . ?
C34 C33 H33 118.0 . . ?
C560 C561 H56A 109.5 . . ?
C560 C561 H56B 109.5 . . ?
C560 C561 H56C 109.5 . . ?
H56A C561 H56B 109.5 . . ?
H56A C561 H56C 109.5 . . ?
H56B C561 H56C 109.5 . . ?
C26 C25 H25 119.7 . . ?
C24 C25 C26 120.7(8) . . ?
C24 C25 H25 119.7 . . ?
C620 C622 H62D 109.5 . . ?
C620 C622 H62E 109.5 . . ?
C620 C622 H62F 109.5 . . ?
H62D C622 H62E 109.5 . . ?
H62D C622 H62F 109.5 . . ?
H62E C622 H62F 109.5 . . ?
C660 C661 H66A 109.5 . . ?
C660 C661 H66B 109.5 . . ?
C660 C661 H66C 109.5 . . ?
H66A C661 H66B 109.5 . . ?
H66A C661 H66C 109.5 . . ?
H66B C661 H66C 109.5 . . ?
C12 C13 H13 119.1 . . ?
C14 C13 C12 121.8(8) . . ?
C14 C13 H13 119.1 . . ?
C52 C53 H53 119.1 . . ?
C52 C53 C54 121.8(9) . . ?
C54 C53 H53 119.1 . . ?
C460 C461 H46A 109.5 . . ?
C460 C461 H46B 109.5 . . ?
C460 C461 H46C 109.5 . . ?
H46A C461 H46B 109.5 . . ?
H46A C461 H46C 109.5 . . ?
H46B C461 H46C 109.5 . . ?
C61 C66 C660 122.2(8) . . ?
C65 C66 C61 120.5(8) . . ?
C65 C66 C660 117.2(8) . . ?
C420 C421 H42D 109.5 . . ?
C420 C421 H42E 109.5 . . ?
C420 C421 H42F 109.5 . . ?
H42D C421 H42E 109.5 . . ?
H42D C421 H42F 109.5 . . ?
H42E C421 H42F 109.5 . . ?
C34 C340 H340 107.3 . . ?
C342 C340 C34 109.2(8) . . ?
C342 C340 H340 107.3 . . ?
C342 C340 C341 111.9(9) . . ?
C341 C340 C34 113.5(8) . . ?
C341 C340 H340 107.3 . . ?
C55 C54 C53 118.4(8) . . ?
C55 C54 C540 121.4(10) . . ?
C53 C54 C540 120.1(10) . . ?
O3 B3 C51 119.1(8) . . ?
O3 B3 C61 115.8(8) . . ?
C51 B3 C61 125.1(8) . . ?
C560 C562 H56D 109.5 . . ?
C560 C562 H56E 109.5 . . ?
C560 C562 H56F 109.5 . . ?
H56D C562 H56E 109.5 . . ?
H56D C562 H56F 109.5 . . ?
H56E C562 H56F 109.5 . . ?
C12 C120 H120 106.7 . . ?
C12 C120 C122 112.6(7) . . ?
C121 C120 C12 113.1(8) . . ?
C121 C120 H120 106.7 . . ?
C121 C120 C122 110.4(8) . . ?
C122 C120 H120 106.7 . . ?
C16 C160 H160 107.2 . . ?
C16 C160 C162 109.0(8) . . ?
C162 C160 H160 107.2 . . ?
C161 C160 C16 115.1(8) . . ?
C161 C160 H160 107.2 . . ?
C161 C160 C162 110.9(8) . . ?
C63 C64 C640 116.6(10) . . ?
C65 C64 C63 118.9(9) . . ?
C65 C64 C640 124.4(10) . . ?
C66 C65 H65 119.0 . . ?
C64 C65 C66 122.0(9) . . ?
C64 C65 H65 119.0 . . ?
C160 C162 H16A 109.5 . . ?
C160 C162 H16B 109.5 . . ?
C160 C162 H16C 109.5 . . ?
H16A C162 H16B 109.5 . . ?
H16A C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
O2 B2 C31 119.0(8) . . ?
O2 B2 C41 119.6(8) . . ?
C31 B2 C41 121.4(8) . . ?
C54 C540 H540 106.9 . . ?
C541 C540 C54 109.7(11) . . ?
C541 C540 H540 106.9 . . ?
C542 C540 C54 112.3(10) . . ?
C542 C540 H540 106.9 . . ?
C542 C540 C541 113.7(11) . . ?
C540 C541 H54A 109.5 . . ?
C540 C541 H54B 109.5 . . ?
C540 C541 H54C 109.5 . . ?
H54A C541 H54B 109.5 . . ?
H54A C541 H54C 109.5 . . ?
H54B C541 H54C 109.5 . . ?
C24 C240 H240 107.7 . . ?
C242 C240 C24 111.9(9) . . ?
C242 C240 H240 107.7 . . ?
C241 C240 C24 112.1(9) . . ?
C241 C240 H240 107.7 . . ?
C241 C240 C242 109.5(9) . . ?
C160 C161 H16D 109.5 . . ?
C160 C161 H16E 109.5 . . ?
C160 C161 H16F 109.5 . . ?
H16D C161 H16E 109.5 . . ?
H16D C161 H16F 109.5 . . ?
H16E C161 H16F 109.5 . . ?
C260 C262 H26A 109.5 . . ?
C260 C262 H26B 109.5 . . ?
C260 C262 H26C 109.5 . . ?
H26A C262 H26B 109.5 . . ?
H26A C262 H26C 109.5 . . ?
H26B C262 H26C 109.5 . . ?
C44 C440 H440 106.0 . . ?
C441 C440 C44 118.1(9) . . ?
C441 C440 H440 106.0 . . ?
C441 C440 C442 110.3(10) . . ?
C442 C440 C44 109.7(10) . . ?
C442 C440 H440 106.0 . . ?
C360 C361 H36D 109.5 . . ?
C360 C361 H36E 109.5 . . ?
C360 C361 H36F 109.5 . . ?
H36D C361 H36E 109.5 . . ?
H36D C361 H36F 109.5 . . ?
H36E C361 H36F 109.5 . . ?
C340 C342 H34A 109.5 . . ?
C340 C342 H34B 109.5 . . ?
C340 C342 H34C 109.5 . . ?
H34A C342 H34B 109.5 . . ?
H34A C342 H34C 109.5 . . ?
H34B C342 H34C 109.5 . . ?
C600 C601 H60C 109.5 . . ?
C600 C601 H60D 109.5 . . ?
C600 C601 H60E 109.5 . . ?
H60C C601 H60D 109.5 . . ?
H60C C601 H60E 109.5 . . ?
H60D C601 H60E 109.5 . . ?
O4 C602 H60F 105.0 . . ?
O4 C602 H60G 105.0 . . ?
O4 C602 H60H 108.1 . . ?
O4 C602 H60I 108.1 . . ?
H60F C602 H60G 105.8 . . ?
H60H C602 H60I 107.3 . . ?
C603 C602 O4 129(2) . . ?
C603 C602 H60F 105.0 . . ?
C603 C602 H60G 105.0 . . ?
C604 C602 O4 116.7(11) . . ?
C604 C602 H60H 108.1 . . ?
C604 C602 H60I 108.1 . . ?
C240 C242 H24A 109.5 . . ?
C240 C242 H24B 109.5 . . ?
C240 C242 H24C 109.5 . . ?
H24A C242 H24B 109.5 . . ?
H24A C242 H24C 109.5 . . ?
H24B C242 H24C 109.5 . . ?
C140 C142 H14D 109.5 . . ?
C140 C142 H14E 109.5 . . ?
C140 C142 H14F 109.5 . . ?
H14D C142 H14E 109.5 . . ?
H14D C142 H14F 109.5 . . ?
H14E C142 H14F 109.5 . . ?
C260 C261 H26D 109.5 . . ?
C260 C261 H26E 109.5 . . ?
C260 C261 H26F 109.5 . . ?
H26D C261 H26E 109.5 . . ?
H26D C261 H26F 109.5 . . ?
H26E C261 H26F 109.5 . . ?
C340 C341 H34D 109.5 . . ?
C340 C341 H34E 109.5 . . ?
C340 C341 H34F 109.5 . . ?
H34D C341 H34E 109.5 . . ?
H34D C341 H34F 109.5 . . ?
H34E C341 H34F 109.5 . . ?
C120 C121 H12A 109.5 . . ?
C120 C121 H12B 109.5 . . ?
C120 C121 H12C 109.5 . . ?
H12A C121 H12B 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C440 C441 H44A 109.5 . . ?
C440 C441 H44B 109.5 . . ?
C440 C441 H44C 109.5 . . ?
H44A C441 H44B 109.5 . . ?
H44A C441 H44C 109.5 . . ?
H44B C441 H44C 109.5 . . ?
C520 C521 H52A 109.5 . . ?
C520 C521 H52B 109.5 . . ?
C520 C521 H52C 109.5 . . ?
H52A C521 H52B 109.5 . . ?
H52A C521 H52C 109.5 . . ?
H52B C521 H52C 109.5 . . ?
C460 C462 H46D 109.5 . . ?
C460 C462 H46E 109.5 . . ?
C460 C462 H46F 109.5 . . ?
H46D C462 H46E 109.5 . . ?
H46D C462 H46F 109.5 . . ?
H46E C462 H46F 109.5 . . ?
C520 C522 H52D 109.5 . . ?
C520 C522 H52E 109.5 . . ?
C520 C522 H52F 109.5 . . ?
H52D C522 H52E 109.5 . . ?
H52D C522 H52F 109.5 . . ?
H52E C522 H52F 109.5 . . ?
C120 C122 H12D 109.5 . . ?
C120 C122 H12E 109.5 . . ?
C120 C122 H12F 109.5 . . ?
H12D C122 H12E 109.5 . . ?
H12D C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
C220 C222 H22D 109.5 . . ?
C220 C222 H22E 109.5 . . ?
C220 C222 H22F 109.5 . . ?
H22D C222 H22E 109.5 . . ?
H22D C222 H22F 109.5 . . ?
H22E C222 H22F 109.5 . . ?
C240 C241 H24D 109.5 . . ?
C240 C241 H24E 109.5 . . ?
C240 C241 H24F 109.5 . . ?
H24D C241 H24E 109.5 . . ?
H24D C241 H24F 109.5 . . ?
H24E C241 H24F 109.5 . . ?
C660 C662 H66D 109.5 . . ?
C660 C662 H66E 109.5 . . ?
C660 C662 H66F 109.5 . . ?
H66D C662 H66E 109.5 . . ?
H66D C662 H66F 109.5 . . ?
H66E C662 H66F 109.5 . . ?
H64A C641 H64B 109.5 . . ?
H64A C641 H64C 109.5 . . ?
H64B C641 H64C 109.5 . . ?
C640 C641 H64A 109.5 . . ?
C640 C641 H64B 109.5 . . ?
C640 C641 H64C 109.5 . . ?
C440 C442 H44D 109.5 . . ?
C440 C442 H44E 109.5 . . ?
C440 C442 H44F 109.5 . . ?
H44D C442 H44E 109.5 . . ?
H44D C442 H44F 109.5 . . ?
H44E C442 H44F 109.5 . . ?
C64 C640 H640 107.7 . . ?
C641 C640 C64 111.7(11) . . ?
C641 C640 H640 107.7 . . ?
C642 C640 C64 109.9(13) . . ?
C642 C640 C641 111.8(14) . . ?
C642 C640 H640 107.7 . . ?
C540 C542 H54D 109.5 . . ?
C540 C542 H54E 109.5 . . ?
C540 C542 H54F 109.5 . . ?
H54D C542 H54E 109.5 . . ?
H54D C542 H54F 109.5 . . ?
H54E C542 H54F 109.5 . . ?
C640 C642 H64D 109.5 . . ?
C640 C642 H64E 109.5 . . ?
C640 C642 H64F 109.5 . . ?
H64D C642 H64E 109.5 . . ?
H64D C642 H64F 109.5 . . ?
H64E C642 H64F 109.5 . . ?
C602 C603 H60J 109.5 . . ?
C602 C603 H60K 109.5 . . ?
C602 C603 H60L 109.5 . . ?
H60J C603 H60K 109.5 . . ?
H60J C603 H60L 109.5 . . ?
H60K C603 H60L 109.5 . . ?
C602 C604 H60M 109.5 . . ?
C602 C604 H60N 109.5 . . ?
C602 C604 H60O 109.5 . . ?
H60M C604 H60N 109.5 . . ?
H60M C604 H60O 109.5 . . ?
H60N C604 H60O 109.5 . . ?

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
U1 O3 B3 C51 -165(2) . . . . ?
U1 O3 B3 C61 16(3) . . . . ?
U1 O4 C600 C601 -3.2(11) . . . . ?
U1 O4 C602 C603 -146(3) . . . . ?
U1 O4 C602 C604 132.7(10) . . . . ?
C11 C12 C13 C14 0.4(13) . . . . ?
C11 C12 C120 C121 119.0(9) . . . . ?
C11 C12 C120 C122 -114.9(9) . . . . ?
C11 C16 C160 C162 -93.3(9) . . . . ?
C11 C16 C160 C161 141.4(9) . . . . ?
C621 C620 C62 C61 114.2(9) . . . . ?
C621 C620 C62 C63 -68.5(10) . . . . ?
C620 C62 C61 C66 176.1(8) . . . . ?
C620 C62 C61 B3 -11.2(13) . . . . ?
C620 C62 C63 C64 -177.9(9) . . . . ?
C26 C21 C22 C23 -2.5(12) . . . . ?
C26 C21 C22 C220 176.8(7) . . . . ?
C26 C21 B1 O1 -117.8(9) . . . . ?
C26 C21 B1 C11 59.4(10) . . . . ?
C32 C31 C36 C35 1.7(12) . . . . ?
C32 C31 C36 C360 -179.4(7) . . . . ?
C32 C31 B2 O2 -57.1(11) . . . . ?
C32 C31 B2 C41 123.1(8) . . . . ?
C21 C26 C260 C262 122.7(9) . . . . ?
C21 C26 C260 C261 -111.5(9) . . . . ?
C21 C26 C25 C24 -0.7(14) . . . . ?
C21 C22 C23 C24 -0.5(13) . . . . ?
C21 C22 C220 C221 -104.9(9) . . . . ?
C21 C22 C220 C222 131.8(8) . . . . ?
C420 C42 C41 C46 -179.6(7) . . . . ?
C420 C42 C41 B2 2.2(12) . . . . ?
C420 C42 C43 C44 178.4(8) . . . . ?
C15 C16 C160 C162 83.2(10) . . . . ?
C15 C16 C160 C161 -42.1(12) . . . . ?
C15 C14 C140 C141 -63.4(11) . . . . ?
C15 C14 C140 C142 61.7(11) . . . . ?
C15 C14 C13 C12 -3.0(13) . . . . ?
C62 C61 C66 C660 -179.3(8) . . . . ?
C62 C61 C66 C65 1.9(13) . . . . ?
C62 C61 B3 O3 -59.3(12) . . . . ?
C62 C61 B3 C51 122.1(10) . . . . ?
C62 C63 C64 C65 1.4(16) . . . . ?
C62 C63 C64 C640 -175.6(10) . . . . ?
C12 C11 B1 O1 -136.0(8) . . . . ?
C12 C11 B1 C21 46.9(10) . . . . ?
C12 C11 C16 C15 -3.7(11) . . . . ?
C12 C11 C16 C160 172.7(8) . . . . ?
C22 C21 B1 O1 63.4(11) . . . . ?
C22 C21 B1 C11 -119.4(8) . . . . ?
C22 C23 C24 C25 2.8(14) . . . . ?
C22 C23 C24 C240 -176.0(9) . . . . ?
C56 C51 B3 O3 -55.0(11) . . . . ?
C56 C51 B3 C61 123.5(9) . . . . ?
C56 C55 C54 C53 -0.5(15) . . . . ?
C56 C55 C54 C540 -176.9(9) . . . . ?
C23 C22 C220 C221 74.3(10) . . . . ?
C23 C22 C220 C222 -49.0(11) . . . . ?
C23 C24 C25 C26 -2.3(14) . . . . ?
C23 C24 C240 C242 -68.4(12) . . . . ?
C23 C24 C240 C241 55.1(13) . . . . ?
C31 C32 C320 C321 114.9(9) . . . . ?
C31 C32 C320 C322 -122.7(8) . . . . ?
C31 C32 C33 C34 -0.5(13) . . . . ?
C31 C36 C360 C362 -131.4(8) . . . . ?
C31 C36 C360 C361 103.2(9) . . . . ?
C52 C51 B3 O3 122.2(9) . . . . ?
C52 C51 B3 C61 -59.2(12) . . . . ?
C52 C53 C54 C55 0.1(14) . . . . ?
C52 C53 C54 C540 176.5(9) . . . . ?
B1 C11 C12 C13 -168.0(7) . . . . ?
B1 C11 C12 C120 14.2(12) . . . . ?
B1 C11 C16 C15 167.3(7) . . . . ?
B1 C11 C16 C160 -16.3(12) . . . . ?
B1 C21 C22 C23 176.4(8) . . . . ?
B1 C21 C22 C220 -4.4(12) . . . . ?
C51 C56 C560 C561 113.3(9) . . . . ?
C51 C56 C560 C562 -121.8(9) . . . . ?
C51 C56 C55 C54 1.6(14) . . . . ?
C51 C52 C520 C521 -129.4(9) . . . . ?
C51 C52 C520 C522 106.3(10) . . . . ?
C51 C52 C53 C54 -0.8(13) . . . . ?
C45 C44 C440 C441 6.6(17) . . . . ?
C45 C44 C440 C442 -120.9(12) . . . . ?
C45 C46 C460 C461 46.6(11) . . . . ?
C45 C46 C460 C462 -77.1(10) . . . . ?
C520 C52 C51 C56 -177.7(8) . . . . ?
C520 C52 C51 B3 5.0(13) . . . . ?
C520 C52 C53 C54 178.8(8) . . . . ?
C320 C32 C31 C36 178.4(7) . . . . ?
C320 C32 C31 B2 -2.7(12) . . . . ?
C320 C32 C33 C34 -179.7(8) . . . . ?
C42 C41 C46 C45 1.5(12) . . . . ?
C42 C41 C46 C460 178.6(8) . . . . ?
C42 C41 B2 O2 -57.5(11) . . . . ?
C42 C41 B2 C31 122.4(9) . . . . ?
C42 C43 C44 C45 0.9(14) . . . . ?
C42 C43 C44 C440 -178.9(9) . . . . ?
C41 C42 C43 C44 -0.7(13) . . . . ?
C41 C46 C460 C461 -130.6(9) . . . . ?
C41 C46 C460 C462 105.7(9) . . . . ?
C43 C42 C41 C46 -0.5(12) . . . . ?
C43 C42 C41 B2 -178.7(7) . . . . ?
C43 C44 C440 C441 -173.7(11) . . . . ?
C43 C44 C440 C442 58.8(14) . . . . ?
C560 C56 C51 C52 174.9(7) . . . . ?
C560 C56 C51 B3 -7.8(12) . . . . ?
C560 C56 C55 C54 -175.8(8) . . . . ?
C35 C36 C360 C362 47.6(10) . . . . ?
C35 C36 C360 C361 -77.9(9) . . . . ?
C35 C34 C33 C32 0.7(13) . . . . ?
C35 C34 C340 C342 85.7(11) . . . . ?
C35 C34 C340 C341 -39.8(12) . . . . ?
C422 C420 C42 C41 104.8(9) . . . . ?
C422 C420 C42 C43 -74.3(10) . . . . ?
C16 C11 C12 C13 3.0(11) . . . . ?
C16 C11 C12 C120 -174.8(7) . . . . ?
C16 C11 B1 O1 53.4(11) . . . . ?
C16 C11 B1 C21 -123.6(8) . . . . ?
C16 C15 C14 C140 -177.5(8) . . . . ?
C16 C15 C14 C13 2.2(13) . . . . ?
C36 C31 B2 O2 121.9(9) . . . . ?
C36 C31 B2 C41 -58.0(11) . . . . ?
C36 C35 C34 C33 0.3(13) . . . . ?
C36 C35 C34 C340 -179.2(8) . . . . ?
C14 C15 C16 C11 1.2(13) . . . . ?
C14 C15 C16 C160 -175.3(8) . . . . ?
C44 C45 C46 C41 -1.3(13) . . . . ?
C44 C45 C46 C460 -178.6(8) . . . . ?
C61 C62 C63 C64 -0.5(14) . . . . ?
C61 C66 C65 C64 -1.1(15) . . . . ?
C220 C22 C23 C24 -179.7(8) . . . . ?
C600 O4 C602 C603 29(3) . . . . ?
C600 O4 C602 C604 -52.5(15) . . . . ?
C63 C62 C61 C66 -1.1(13) . . . . ?
C63 C62 C61 B3 171.5(8) . . . . ?
C63 C64 C65 C66 -0.6(17) . . . . ?
C63 C64 C640 C641 143.4(13) . . . . ?
C63 C64 C640 C642 -91.9(17) . . . . ?
C46 C45 C44 C43 0.2(14) . . . . ?
C46 C45 C44 C440 179.9(9) . . . . ?
C46 C41 B2 O2 124.4(9) . . . . ?
C46 C41 B2 C31 -55.7(11) . . . . ?
C34 C35 C36 C31 -1.5(13) . . . . ?
C34 C35 C36 C360 179.5(8) . . . . ?
C55 C56 C51 C52 -2.3(12) . . . . ?
C55 C56 C51 B3 175.0(8) . . . . ?
C55 C56 C560 C561 -69.4(10) . . . . ?
C55 C56 C560 C562 55.5(11) . . . . ?
C55 C54 C540 C541 67.9(14) . . . . ?
C55 C54 C540 C542 -59.6(15) . . . . ?
C660 C66 C65 C64 -180.0(10) . . . . ?
C140 C14 C13 C12 176.7(8) . . . . ?
C260 C26 C21 C22 -175.9(7) . . . . ?
C260 C26 C21 B1 5.3(12) . . . . ?
C260 C26 C25 C24 178.3(8) . . . . ?
C33 C32 C31 C36 -0.7(11) . . . . ?
C33 C32 C31 B2 178.2(7) . . . . ?
C33 C32 C320 C321 -66.0(9) . . . . ?
C33 C32 C320 C322 56.4(10) . . . . ?
C33 C34 C340 C342 -93.7(11) . . . . ?
C33 C34 C340 C341 140.7(9) . . . . ?
C25 C26 C21 C22 3.0(12) . . . . ?
C25 C26 C21 B1 -175.8(8) . . . . ?
C25 C26 C260 C262 -56.2(11) . . . . ?
C25 C26 C260 C261 69.5(10) . . . . ?
C25 C24 C240 C242 112.7(10) . . . . ?
C25 C24 C240 C241 -123.8(10) . . . . ?
C622 C620 C62 C61 -123.3(9) . . . . ?
C622 C620 C62 C63 54.1(10) . . . . ?
C661 C660 C66 C61 -123.7(9) . . . . ?
C661 C660 C66 C65 55.1(12) . . . . ?
C13 C12 C120 C121 -58.9(10) . . . . ?
C13 C12 C120 C122 67.2(10) . . . . ?
C13 C14 C140 C141 116.9(9) . . . . ?
C13 C14 C140 C142 -118.0(9) . . . . ?
C53 C52 C51 C56 1.9(12) . . . . ?
C53 C52 C51 B3 -175.4(8) . . . . ?
C53 C52 C520 C521 51.0(12) . . . . ?
C53 C52 C520 C522 -73.3(11) . . . . ?
C53 C54 C540 C541 -108.4(11) . . . . ?
C53 C54 C540 C542 124.1(12) . . . . ?
C66 C61 B3 O3 113.1(9) . . . . ?
C66 C61 B3 C51 -65.5(12) . . . . ?
C421 C420 C42 C41 -131.6(8) . . . . ?
C421 C420 C42 C43 49.3(11) . . . . ?
C340 C34 C33 C32 -179.8(8) . . . . ?
B3 C61 C66 C660 7.9(13) . . . . ?
B3 C61 C66 C65 -170.9(9) . . . . ?
C120 C12 C13 C14 178.3(7) . . . . ?
C65 C64 C640 C641 -33.4(18) . . . . ?
C65 C64 C640 C642 91.3(18) . . . . ?
B2 C31 C36 C35 -177.2(7) . . . . ?
B2 C31 C36 C360 1.7(12) . . . . ?
B2 C41 C46 C45 179.6(8) . . . . ?
B2 C41 C46 C460 -3.2(12) . . . . ?
C240 C24 C25 C26 176.6(9) . . . . ?
C602 O4 C600 C601 -177.8(9) . . . . ?
C662 C660 C66 C61 108.3(10) . . . . ?
C662 C660 C66 C65 -72.9(12) . . . . ?
C640 C64 C65 C66 176.2(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.103
_oxdiff_exptl_absorpt_empirical_full_min 0.903
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p16121_087mono
_database_code_depnum_ccdc_archive 'CCDC 1886805'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_audit_creation_date             2018-12-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C120 H184 B4 O4 U, C7 H8'
_chemical_formula_sum            'C127 H192 B4 O4 U'
_chemical_formula_weight         2064.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H100 B3 O3 U'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.0131(4)
_cell_length_b                   19.4020(3)
_cell_length_c                   30.6714(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.923(2)
_cell_angle_gamma                90
_cell_volume                     12391.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    28581
_cell_measurement_temperature    170
_cell_measurement_theta_max      23.2550
_cell_measurement_theta_min      3.0280
_shelx_estimated_absorpt_T_max   0.876
_shelx_estimated_absorpt_T_min   0.784
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-20 -19 -5 0.0684
20 19 5 0.0684
21 -20 -16 0.0656
-21 20 16 0.0656
-1 3 -40 0.0501
1 -3 40 0.0501

_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19.9578 -18.9475 -5.0059 -0.5906 0.3649 -0.7276
19.9578 18.9475 5.0059 0.5906 -0.3649 0.7276
21.0080 -19.9720 -15.9996 -0.6967 0.4124 0.6007
-21.0080 19.9720 15.9996 0.6967 -0.4124 -0.6007
-0.9922 3.0078 -39.9753 -0.6705 -0.7072 -0.1998
0.9922 -3.0078 39.9753 0.6705 0.7072 0.1998

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            218483
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.800
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00   0.00   1.00   30.00    --  -18.53 -57.00   0.00   87
  2  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00-150.00   47
  3  ω    -25.00  61.00   1.00   30.00    --   20.25 -99.00 -30.00   86
  4  ω    -48.00  39.00   1.00   30.00    --   20.25 -57.00 -60.00   87
  5  ω      2.00  89.00   1.00   30.00    --   20.25  57.00-180.00   87
  6  ω      2.00  89.00   1.00   30.00    --   20.25  57.00 -90.00   87
  7  ω    -50.00  43.00   1.00   30.00    --   20.25 -38.00  30.00   93
  8  ω    -37.00  50.00   1.00   30.00    --  -18.53  57.00 150.00   87
  9  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 -90.00   47
 10  ω    -93.00 -32.00   1.00   30.00    --  -18.53 179.00 120.00   61
 11  ω    -25.00  61.00   1.00   30.00    --   20.25 -99.00  30.00   86
 12  ω      2.00  89.00   1.00   30.00    --   20.25  57.00  90.00   87
 13  ω     34.00  94.00   1.00   30.00    --   20.25 179.00 -90.00   60
 14  ω    -12.00  47.00   1.00   30.00    --   20.25-114.00 174.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029396000
_diffrn_orient_matrix_UB_12      0.0232024000
_diffrn_orient_matrix_UB_13      0.0184447000
_diffrn_orient_matrix_UB_21      0.0046040000
_diffrn_orient_matrix_UB_22      -0.0281896000
_diffrn_orient_matrix_UB_23      0.0154557000
_diffrn_orient_matrix_UB_31      0.0336244000
_diffrn_orient_matrix_UB_32      0.0018457000
_diffrn_orient_matrix_UB_33      0.0043023000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12561
_reflns_number_total             19685
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.484
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         19685
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.027
_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)+(0.0498P)²+19.3178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1164
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C740 \\sim C741 \\sim C742: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C740, C741, C742
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C560(H560), C360(H360), C440(H440), C620(H620), C760(H760), C140(H140),
 C160(H160), C460(H460), C420(H420), C720(H720), C840(H840), C220(H220),
 C640(H640), C860(H860), C120(H120), C260(H260), C660(H660), C820(H820),
 C740(H740), C540(H540), C320(H320), C240(H240), C520(H520), C340(H340)
4.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C23(H23), C33(H33), C45(H45), C73(H73), C63(H63), C25(H25),
 C83(H83), C65(H65), C85(H85), C55(H55), C35(H35), C15(H15), C75(H75), C13(H13),
  C53(H53), C6S(H6S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S)
4.c Fitted hexagon refined as free rotating group:
 C6S(C1S,C2S,C3S,C4S,C5S)
4.d Idealised Me refined as rotating group:
 C421(H42A,H42B,H42C), C621(H62A,H62B,H62C), C762(H76A,H76B,H76C), C521(H52A,
 H52B,H52C), C122(H12A,H12B,H12C), C262(H26A,H26B,H26C), C341(H34A,H34B,H34C),
 C822(H82A,H82B,H82C), C142(H14A,H14B,H14C), C221(H22A,H22B,H22C), C361(H36A,
 H36B,H36C), C661(H66A,H66B,H66C), C721(H72A,H72B,H72C), C222(H22D,H22E,H22F),
 C541(H54A,H54B,H54C), C322(H32A,H32B,H32C), C761(H76D,H76E,H76F), C261(H26D,
 H26E,H26F), C162(H16A,H16B,H16C), C422(H42D,H42E,H42F), C862(H86A,H86B,H86C),
 C622(H62D,H62E,H62F), C861(H86D,H86E,H86F), C522(H52D,H52E,H52F), C442(H44A,
 H44B,H44C), C462(H46A,H46B,H46C), C362(H36D,H36E,H36F), C842(H84A,H84B,H84C),
 C342(H34D,H34E,H34F), C562(H56A,H56B,H56C), C542(H54D,H54E,H54F), C662(H66D,
 H66E,H66F), C242(H24A,H24B,H24C), C461(H46D,H46E,H46F), C321(H32D,H32E,H32F),
 C641(H64A,H64B,H64C), C441(H44D,H44E,H44F), C722(H72D,H72E,H72F), C121(H12D,
 H12E,H12F), C642(H64D,H64E,H64F), C561(H56D,H56E,H56F), C141(H14D,H14E,H14F),
 C241(H24D,H24E,H24F), C821(H82D,H82E,H82F), C742(H74A,H74B,H74C), C841(H84D,
 H84E,H84F), C161(H16D,H16E,H16F), C741(H74D,H74E,H74F), C7S(H7SA,H7SB,H7SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.25067(2) 0.43835(2) 0.25122(2) 0.02637(7) Uani 1 1 d . . . . .
O1 O 0.17310(15) 0.51131(17) 0.22857(11) 0.0297(8) Uani 1 1 d . . . . .
O3 O 0.22779(16) 0.37100(18) 0.19150(11) 0.0344(9) Uani 1 1 d . . . . .
O2 O 0.25890(15) 0.38918(17) 0.31602(11) 0.0298(8) Uani 1 1 d . . . . .
C16 C 0.1507(3) 0.6684(3) 0.18625(19) 0.0377(14) Uani 1 1 d . . . . .
O4 O 0.34456(15) 0.48493(17) 0.26887(11) 0.0302(8) Uani 1 1 d . . . . .
C560 C 0.2268(3) 0.2049(3) 0.20822(19) 0.0484(16) Uani 1 1 d . . . . .
H560 H 0.257041 0.244190 0.210480 0.058 Uiso 1 1 calc R . . . .
C421 C 0.3729(3) 0.3107(3) 0.2808(2) 0.0549(17) Uani 1 1 d . . . . .
H42A H 0.388020 0.267975 0.270694 0.082 Uiso 1 1 calc GR . . . .
H42B H 0.392587 0.350298 0.270792 0.082 Uiso 1 1 calc GR . . . .
H42C H 0.326068 0.313578 0.267284 0.082 Uiso 1 1 calc GR . . . .
C43 C 0.3722(3) 0.1886(3) 0.35230(17) 0.0343(13) Uani 1 1 d . . . . .
H43 H 0.410043 0.177175 0.345358 0.041 Uiso 1 1 calc R . . . .
C23 C -0.0276(3) 0.4503(3) 0.22983(19) 0.0390(14) Uani 1 1 d . . . . .
H23 H -0.046299 0.405627 0.224278 0.047 Uiso 1 1 calc R . . . .
C360 C 0.1450(3) 0.4167(3) 0.36082(19) 0.0407(14) Uani 1 1 d . . . . .
H360 H 0.153886 0.388448 0.336308 0.049 Uiso 1 1 calc R . . . .
C440 C 0.3609(3) 0.0623(3) 0.3674(2) 0.0520(17) Uani 1 1 d . . . . .
H440 H 0.330495 0.034111 0.378207 0.062 Uiso 1 1 calc R . . . .
C52 C 0.1087(3) 0.2760(3) 0.09620(18) 0.0393(14) Uani 1 1 d . . . . .
C620 C 0.2087(3) 0.4840(3) 0.11398(19) 0.0395(14) Uani 1 1 d . . . . .
H620 H 0.178045 0.461404 0.127443 0.047 Uiso 1 1 calc R . . . .
C71 C 0.4687(2) 0.4820(3) 0.28923(18) 0.0307(13) Uani 1 1 d . . . . .
C760 C 0.4322(3) 0.4570(3) 0.20185(19) 0.0435(15) Uani 1 1 d . . . . .
H760 H 0.393578 0.482346 0.203728 0.052 Uiso 1 1 calc R . . . .
C621 C 0.2568(3) 0.5258(3) 0.1519(2) 0.0563(18) Uani 1 1 d . . . . .
H62A H 0.284861 0.494375 0.174610 0.085 Uiso 1 1 calc GR . . . .
H62B H 0.233560 0.555410 0.166985 0.085 Uiso 1 1 calc GR . . . .
H62C H 0.282724 0.554361 0.138330 0.085 Uiso 1 1 calc GR . . . .
C11 C 0.1107(2) 0.6106(3) 0.17558(18) 0.0321(13) Uani 1 1 d . . . . .
C26 C 0.0277(2) 0.5794(3) 0.24747(18) 0.0332(13) Uani 1 1 d . . . . .
C22 C 0.0275(2) 0.4635(3) 0.21851(17) 0.0305(13) Uani 1 1 d . . . . .
C140 C 0.0832(4) 0.7788(4) 0.0772(3) 0.073(2) Uani 1 1 d . . . . .
H140 H 0.067149 0.753766 0.047118 0.088 Uiso 1 1 calc R . . . .
C72 C 0.5201(3) 0.4801(3) 0.33158(18) 0.0350(13) Uani 1 1 d . . . . .
C160 C 0.2036(3) 0.6776(3) 0.2325(2) 0.0449(15) Uani 1 1 d . . . . .
H160 H 0.201338 0.637974 0.252757 0.054 Uiso 1 1 calc R . . . .
C76 C 0.4808(3) 0.4547(3) 0.24972(19) 0.0385(14) Uani 1 1 d . . . . .
C460 C 0.2017(2) 0.2373(3) 0.38383(18) 0.0347(14) Uani 1 1 d . . . . .
H460 H 0.195066 0.288374 0.381617 0.042 Uiso 1 1 calc R . . . .
C33 C 0.3103(3) 0.4256(3) 0.48233(18) 0.0354(13) Uani 1 1 d . . . . .
H33 H 0.345736 0.426299 0.510099 0.042 Uiso 1 1 calc R . . . .
C420 C 0.3915(2) 0.3109(3) 0.33313(18) 0.0338(13) Uani 1 1 d . . . . .
H420 H 0.380608 0.357148 0.342898 0.041 Uiso 1 1 calc R . . . .
C720 C 0.5147(3) 0.5100(3) 0.37635(17) 0.0353(13) Uani 1 1 d . . . . .
H720 H 0.468033 0.515754 0.372414 0.042 Uiso 1 1 calc R . . . .
C840 C 0.4180(4) 0.8078(3) 0.3538(3) 0.066(2) Uani 1 1 d . . . . .
H840 H 0.429765 0.837600 0.331193 0.079 Uiso 1 1 calc R . . . .
C82 C 0.3801(3) 0.6149(3) 0.33912(18) 0.0343(13) Uani 1 1 d . . . . .
C31 C 0.2659(2) 0.3907(3) 0.40190(17) 0.0300(13) Uani 1 1 d . . . . .
C45 C 0.2847(3) 0.1547(3) 0.37587(18) 0.0372(13) Uani 1 1 d . . . . .
H45 H 0.261041 0.119711 0.384917 0.045 Uiso 1 1 calc R . . . .
C73 C 0.5789(3) 0.4526(3) 0.3336(2) 0.0544(18) Uani 1 1 d . . . . .
H73 H 0.612802 0.453327 0.362217 0.065 Uiso 1 1 calc R . . . .
C220 C 0.0556(2) 0.4047(3) 0.19814(18) 0.0323(13) Uani 1 1 d . . . . .
H220 H 0.083082 0.425875 0.181400 0.039 Uiso 1 1 calc R . . . .
C640 C 0.3354(3) 0.4181(4) 0.0104(2) 0.0614(19) Uani 1 1 d . . . . .
H640 H 0.339219 0.375589 -0.006928 0.074 Uiso 1 1 calc R . . . .
C762 C 0.4106(3) 0.3856(3) 0.1826(2) 0.0592(19) Uani 1 1 d . . . . .
H76A H 0.448361 0.356393 0.186573 0.089 Uiso 1 1 calc GR . . . .
H76B H 0.385899 0.389165 0.149801 0.089 Uiso 1 1 calc GR . . . .
H76C H 0.383713 0.365166 0.199189 0.089 Uiso 1 1 calc GR . . . .
C521 C 0.1181(3) 0.3182(4) 0.02018(19) 0.0587(19) Uani 1 1 d . . . . .
H52A H 0.164289 0.308215 0.031176 0.088 Uiso 1 1 calc GR . . . .
H52B H 0.109699 0.357267 -0.001177 0.088 Uiso 1 1 calc GR . . . .
H52C H 0.094695 0.277609 0.004249 0.088 Uiso 1 1 calc GR . . . .
C122 C -0.0527(3) 0.5705(3) 0.1238(2) 0.0550(17) Uani 1 1 d . . . . .
H12A H -0.045333 0.586932 0.155343 0.083 Uiso 1 1 calc GR . . . .
H12B H -0.080912 0.530117 0.117954 0.083 Uiso 1 1 calc GR . . . .
H12C H -0.072997 0.607149 0.101935 0.083 Uiso 1 1 calc GR . . . .
C860 C 0.4560(3) 0.6360(3) 0.24331(19) 0.0398(15) Uani 1 1 d . . . . .
H860 H 0.443663 0.587712 0.232709 0.048 Uiso 1 1 calc R . . . .
C61 C 0.2475(2) 0.3594(3) 0.11397(17) 0.0332(13) Uani 1 1 d . . . . .
C262 C 0.0678(3) 0.6694(3) 0.3106(2) 0.0562(18) Uani 1 1 d . . . . .
H26A H 0.026378 0.673840 0.315831 0.084 Uiso 1 1 calc GR . . . .
H26B H 0.091160 0.713126 0.317855 0.084 Uiso 1 1 calc GR . . . .
H26C H 0.093111 0.632951 0.330493 0.084 Uiso 1 1 calc GR . . . .
C63 C 0.2722(3) 0.4452(3) 0.0637(2) 0.0464(16) Uani 1 1 d . . . . .
H63 H 0.269320 0.491549 0.053262 0.056 Uiso 1 1 calc R . . . .
C32 C 0.3172(2) 0.3917(3) 0.44400(17) 0.0308(12) Uani 1 1 d . . . . .
C25 C -0.0279(3) 0.5635(3) 0.25785(19) 0.0397(14) Uani 1 1 d . . . . .
H25 H -0.046588 0.597908 0.271538 0.048 Uiso 1 1 calc R . . . .
C120 C 0.0116(3) 0.5509(3) 0.11794(18) 0.0406(14) Uani 1 1 d . . . . .
H120 H 0.029196 0.510630 0.138552 0.049 Uiso 1 1 calc R . . . .
C41 C 0.2966(2) 0.2756(3) 0.35938(16) 0.0279(12) Uani 1 1 d . . . . .
C86 C 0.4314(2) 0.6495(3) 0.28388(18) 0.0349(13) Uani 1 1 d . . . . .
C260 C 0.0566(3) 0.6508(3) 0.25999(19) 0.0396(14) Uani 1 1 d . . . . .
H260 H 0.099627 0.650246 0.255522 0.048 Uiso 1 1 calc R . . . .
C341 C 0.1874(3) 0.4871(4) 0.5327(2) 0.071(2) Uani 1 1 d . . . . .
H34A H 0.190229 0.509664 0.561928 0.107 Uiso 1 1 calc GR . . . .
H34B H 0.180237 0.437616 0.535123 0.107 Uiso 1 1 calc GR . . . .
H34C H 0.151568 0.506885 0.507870 0.107 Uiso 1 1 calc GR . . . .
C660 C 0.2902(3) 0.2372(3) 0.1125(2) 0.0473(16) Uani 1 1 d . . . . .
H660 H 0.271569 0.233532 0.138194 0.057 Uiso 1 1 calc R . . . .
B2 B 0.2726(3) 0.3539(3) 0.3568(2) 0.0300(15) Uani 1 1 d . . . . .
C83 C 0.3849(3) 0.6821(3) 0.3541(2) 0.0436(15) Uani 1 1 d . . . . .
H83 H 0.368485 0.693408 0.378288 0.052 Uiso 1 1 calc R . . . .
C42 C 0.3527(2) 0.2566(3) 0.34896(17) 0.0297(12) Uani 1 1 d . . . . .
C822 C 0.3682(3) 0.5705(3) 0.41416(19) 0.0498(17) Uani 1 1 d . . . . .
H82A H 0.415175 0.569569 0.427401 0.075 Uiso 1 1 calc GR . . . .
H82B H 0.349991 0.532706 0.427067 0.075 Uiso 1 1 calc GR . . . .
H82C H 0.352115 0.614607 0.421545 0.075 Uiso 1 1 calc GR . . . .
C142 C 0.0284(5) 0.8214(4) 0.0761(3) 0.117(4) Uani 1 1 d . . . . .
H14A H -0.008125 0.791801 0.075124 0.175 Uiso 1 1 calc GR . . . .
H14B H 0.016813 0.850766 0.048610 0.175 Uiso 1 1 calc GR . . . .
H14C H 0.039467 0.850329 0.103740 0.175 Uiso 1 1 calc GR . . . .
C46 C 0.2635(2) 0.2229(3) 0.37362(16) 0.0310(12) Uani 1 1 d . . . . .
C221 C 0.0057(3) 0.3602(3) 0.1637(2) 0.0484(16) Uani 1 1 d . . . . .
H22A H -0.019653 0.335348 0.179661 0.073 Uiso 1 1 calc GR . . . .
H22B H 0.027438 0.326985 0.149729 0.073 Uiso 1 1 calc GR . . . .
H22C H -0.022651 0.389492 0.139655 0.073 Uiso 1 1 calc GR . . . .
C361 C 0.0918(3) 0.3804(3) 0.3743(2) 0.0575(18) Uani 1 1 d . . . . .
H36A H 0.108565 0.337506 0.390682 0.086 Uiso 1 1 calc GR . . . .
H36B H 0.055742 0.369835 0.346480 0.086 Uiso 1 1 calc GR . . . .
H36C H 0.076962 0.410617 0.394423 0.086 Uiso 1 1 calc GR . . . .
C661 C 0.3604(3) 0.2182(3) 0.1324(3) 0.078(2) Uani 1 1 d . . . . .
H66A H 0.380285 0.220511 0.108042 0.117 Uiso 1 1 calc GR . . . .
H66B H 0.364423 0.171296 0.144813 0.117 Uiso 1 1 calc GR . . . .
H66C H 0.382148 0.250522 0.157060 0.117 Uiso 1 1 calc GR . . . .
C820 C 0.3487(3) 0.5624(3) 0.36181(18) 0.0351(13) Uani 1 1 d . . . . .
H820 H 0.362082 0.515359 0.355123 0.042 Uiso 1 1 calc R . . . .
C51 C 0.1615(3) 0.2757(3) 0.13740(18) 0.0350(13) Uani 1 1 d . . . . .
C62 C 0.2439(3) 0.4277(3) 0.09707(19) 0.0381(14) Uani 1 1 d . . . . .
C54 C 0.0707(3) 0.1650(3) 0.1134(2) 0.0503(16) Uani 1 1 d . . . . .
C65 C 0.3079(3) 0.3308(3) 0.06205(19) 0.0437(15) Uani 1 1 d . . . . .
H65 H 0.329860 0.297122 0.050353 0.052 Uiso 1 1 calc R . . . .
C721 C 0.5465(3) 0.5804(3) 0.3869(2) 0.0511(17) Uani 1 1 d . . . . .
H72A H 0.592914 0.575406 0.393213 0.077 Uiso 1 1 calc GR . . . .
H72B H 0.538452 0.600177 0.413849 0.077 Uiso 1 1 calc GR . . . .
H72C H 0.528789 0.610851 0.360280 0.077 Uiso 1 1 calc GR . . . .
C222 C 0.0988(3) 0.3594(3) 0.23609(19) 0.0456(15) Uani 1 1 d . . . . .
H22D H 0.131533 0.388008 0.257869 0.068 Uiso 1 1 calc GR . . . .
H22E H 0.119791 0.324906 0.222493 0.068 Uiso 1 1 calc GR . . . .
H22F H 0.072978 0.336151 0.252362 0.068 Uiso 1 1 calc GR . . . .
C541 C 0.0474(5) 0.0495(4) 0.0765(4) 0.123(4) Uani 1 1 d . . . . .
H54A H 0.051107 0.068036 0.047790 0.185 Uiso 1 1 calc GR . . . .
H54B H 0.017318 0.010642 0.069557 0.185 Uiso 1 1 calc GR . . . .
H54C H 0.089635 0.033705 0.096337 0.185 Uiso 1 1 calc GR . . . .
C740 C 0.6552(4) 0.3905(8) 0.2976(3) 0.143(5) Uani 1 1 d . U . . .
H740 H 0.651216 0.365085 0.268416 0.171 Uiso 1 1 calc R . . . .
C540 C 0.0229(4) 0.1052(4) 0.1012(2) 0.070(2) Uani 1 1 d . . . . .
H540 H 0.021223 0.085124 0.130778 0.084 Uiso 1 1 calc R . . . .
C322 C 0.4391(3) 0.4010(3) 0.4736(2) 0.0491(16) Uani 1 1 d . . . . .
H32A H 0.434855 0.444981 0.457176 0.074 Uiso 1 1 calc GR . . . .
H32B H 0.478237 0.377503 0.473009 0.074 Uiso 1 1 calc GR . . . .
H32C H 0.441739 0.409630 0.505688 0.074 Uiso 1 1 calc GR . . . .
C761 C 0.4573(3) 0.4952(4) 0.1672(2) 0.0628(19) Uani 1 1 d . . . . .
H76D H 0.475445 0.539691 0.180252 0.094 Uiso 1 1 calc GR . . . .
H76E H 0.421899 0.502806 0.138524 0.094 Uiso 1 1 calc GR . . . .
H76F H 0.490695 0.467430 0.160871 0.094 Uiso 1 1 calc GR . . . .
C85 C 0.4354(3) 0.7158(3) 0.3006(2) 0.0429(15) Uani 1 1 d . . . . .
H85 H 0.454759 0.750149 0.287399 0.051 Uiso 1 1 calc R . . . .
C261 C 0.0170(3) 0.7068(3) 0.2284(2) 0.0553(17) Uani 1 1 d . . . . .
H26D H 0.014531 0.697280 0.196513 0.083 Uiso 1 1 calc GR . . . .
H26E H 0.037411 0.751758 0.237804 0.083 Uiso 1 1 calc GR . . . .
H26F H -0.026419 0.707468 0.230662 0.083 Uiso 1 1 calc GR . . . .
C162 C 0.1964(3) 0.7448(3) 0.2574(2) 0.0589(18) Uani 1 1 d . . . . .
H16A H 0.202689 0.784536 0.239619 0.088 Uiso 1 1 calc GR . . . .
H16B H 0.228660 0.745718 0.288191 0.088 Uiso 1 1 calc GR . . . .
H16C H 0.153369 0.746731 0.260223 0.088 Uiso 1 1 calc GR . . . .
C36 C 0.2072(3) 0.4220(3) 0.40120(18) 0.0339(13) Uani 1 1 d . . . . .
C422 C 0.4637(3) 0.3006(3) 0.3543(2) 0.0593(19) Uani 1 1 d . . . . .
H42D H 0.476246 0.257792 0.342482 0.089 Uiso 1 1 calc GR . . . .
H42E H 0.475222 0.297693 0.387903 0.089 Uiso 1 1 calc GR . . . .
H42F H 0.486217 0.339551 0.346128 0.089 Uiso 1 1 calc GR . . . .
C56 C 0.1686(3) 0.2160(3) 0.16579(19) 0.0403(14) Uani 1 1 d . . . . .
C66 C 0.2806(2) 0.3114(3) 0.09541(18) 0.0374(13) Uani 1 1 d . . . . .
B3 B 0.2128(3) 0.3372(3) 0.1504(2) 0.0358(16) Uani 1 1 d . . . . .
C55 C 0.1231(3) 0.1640(3) 0.1538(2) 0.0506(17) Uani 1 1 d . . . . .
H55 H 0.127940 0.125769 0.173977 0.061 Uiso 1 1 calc R . . . .
C64 C 0.3040(3) 0.3977(3) 0.0454(2) 0.0475(16) Uani 1 1 d . . . . .
C24 C -0.0563(3) 0.5005(3) 0.24903(19) 0.0392(14) Uani 1 1 d . . . . .
C35 C 0.2037(3) 0.4558(3) 0.44076(19) 0.0420(15) Uani 1 1 d . . . . .
H35 H 0.164783 0.478164 0.439465 0.050 Uiso 1 1 calc R . . . .
C862 C 0.5291(3) 0.6399(3) 0.2582(2) 0.0537(17) Uani 1 1 d . . . . .
H86A H 0.543133 0.686487 0.269237 0.081 Uiso 1 1 calc GR . . . .
H86B H 0.543417 0.629026 0.231871 0.081 Uiso 1 1 calc GR . . . .
H86C H 0.547629 0.606632 0.282987 0.081 Uiso 1 1 calc GR . . . .
C622 C 0.1704(3) 0.5326(3) 0.0754(2) 0.0620(19) Uani 1 1 d . . . . .
H62D H 0.146328 0.565503 0.087647 0.093 Uiso 1 1 calc GR . . . .
H62E H 0.140509 0.505703 0.050574 0.093 Uiso 1 1 calc GR . . . .
H62F H 0.200073 0.557787 0.063182 0.093 Uiso 1 1 calc GR . . . .
C320 C 0.3810(2) 0.3559(3) 0.45045(18) 0.0348(13) Uani 1 1 d . . . . .
H320 H 0.382479 0.344273 0.419046 0.042 Uiso 1 1 calc R . . . .
C861 C 0.4254(3) 0.6830(4) 0.2025(2) 0.0617(19) Uani 1 1 d . . . . .
H86D H 0.378620 0.681409 0.194675 0.093 Uiso 1 1 calc GR . . . .
H86E H 0.437498 0.667575 0.176007 0.093 Uiso 1 1 calc GR . . . .
H86F H 0.440458 0.730333 0.210495 0.093 Uiso 1 1 calc GR . . . .
C522 C 0.0246(3) 0.3570(3) 0.0437(2) 0.0564(18) Uani 1 1 d . . . . .
H52D H -0.000850 0.319329 0.025360 0.085 Uiso 1 1 calc GR . . . .
H52E H 0.019597 0.398336 0.024474 0.085 Uiso 1 1 calc GR . . . .
H52F H 0.009838 0.366713 0.069935 0.085 Uiso 1 1 calc GR . . . .
C240 C -0.1171(3) 0.4842(3) 0.2612(2) 0.0567(18) Uani 1 1 d . . . . .
H240 H -0.129952 0.527619 0.273464 0.068 Uiso 1 1 calc R . . . .
C442 C 0.4274(4) 0.0524(4) 0.4020(3) 0.081(2) Uani 1 1 d . . . . .
H44A H 0.458004 0.082053 0.393657 0.121 Uiso 1 1 calc GR . . . .
H44B H 0.440342 0.004116 0.401713 0.121 Uiso 1 1 calc GR . . . .
H44C H 0.426910 0.064635 0.432846 0.121 Uiso 1 1 calc GR . . . .
B1 B 0.1178(3) 0.5480(3) 0.2122(2) 0.0325(15) Uani 1 1 d . . . . .
C520 C 0.0958(3) 0.3360(3) 0.06139(18) 0.0419(14) Uani 1 1 d . . . . .
H520 H 0.121189 0.376684 0.077461 0.050 Uiso 1 1 calc R . . . .
C340 C 0.2493(3) 0.4983(4) 0.5224(2) 0.0576(19) Uani 1 1 d . . . . .
H340 H 0.285049 0.482365 0.550010 0.069 Uiso 1 1 calc R . . . .
C14 C 0.0934(3) 0.7205(3) 0.1118(2) 0.0487(16) Uani 1 1 d . . . . .
C21 C 0.0564(2) 0.5291(3) 0.22721(16) 0.0277(12) Uani 1 1 d . . . . .
C462 C 0.2045(3) 0.2164(4) 0.4319(2) 0.079(3) Uani 1 1 d . . . . .
H46A H 0.207729 0.166152 0.434770 0.119 Uiso 1 1 calc GR . . . .
H46B H 0.165395 0.231981 0.437657 0.119 Uiso 1 1 calc GR . . . .
H46C H 0.242054 0.237599 0.454451 0.119 Uiso 1 1 calc GR . . . .
C15 C 0.1412(3) 0.7216(3) 0.1538(2) 0.0473(16) Uani 1 1 d . . . . .
H15 H 0.169217 0.760241 0.161238 0.057 Uiso 1 1 calc R . . . .
C362 C 0.1206(3) 0.4862(3) 0.3402(2) 0.0514(17) Uani 1 1 d . . . . .
H36D H 0.079411 0.480458 0.315663 0.077 Uiso 1 1 calc GR . . . .
H36E H 0.151817 0.506914 0.327433 0.077 Uiso 1 1 calc GR . . . .
H36F H 0.114931 0.516404 0.364226 0.077 Uiso 1 1 calc GR . . . .
C12 C 0.0603(3) 0.6096(3) 0.13262(19) 0.0389(14) Uani 1 1 d . . . . .
C44 C 0.3390(3) 0.1366(3) 0.36534(18) 0.0363(13) Uani 1 1 d . . . . .
C75 C 0.5406(3) 0.4263(4) 0.2544(2) 0.062(2) Uani 1 1 d . . . . .
H75 H 0.547607 0.407615 0.227766 0.075 Uiso 1 1 calc R . . . .
C81 C 0.4036(2) 0.5969(3) 0.30312(17) 0.0304(12) Uani 1 1 d . . . . .
C842 C 0.4718(5) 0.8124(5) 0.3985(4) 0.121(4) Uani 1 1 d . . . . .
H84A H 0.479444 0.860832 0.407830 0.181 Uiso 1 1 calc GR . . . .
H84B H 0.510839 0.792753 0.394804 0.181 Uiso 1 1 calc GR . . . .
H84C H 0.460456 0.786687 0.422289 0.181 Uiso 1 1 calc GR . . . .
C342 C 0.2596(4) 0.5738(4) 0.5166(3) 0.088(3) Uani 1 1 d . . . . .
H34D H 0.226486 0.590856 0.488851 0.132 Uiso 1 1 calc GR . . . .
H34E H 0.302074 0.580894 0.513450 0.132 Uiso 1 1 calc GR . . . .
H34F H 0.256913 0.599045 0.543565 0.132 Uiso 1 1 calc GR . . . .
C13 C 0.0533(3) 0.6640(3) 0.1023(2) 0.0463(15) Uani 1 1 d . . . . .
H13 H 0.019400 0.662388 0.073757 0.056 Uiso 1 1 calc R . . . .
C562 C 0.2094(3) 0.2033(3) 0.25204(19) 0.0578(18) Uani 1 1 d . . . . .
H56A H 0.194141 0.248891 0.257506 0.087 Uiso 1 1 calc GR . . . .
H56B H 0.247366 0.190797 0.278029 0.087 Uiso 1 1 calc GR . . . .
H56C H 0.175460 0.169156 0.248972 0.087 Uiso 1 1 calc GR . . . .
C74 C 0.5903(3) 0.4240(4) 0.2957(2) 0.072(2) Uani 1 1 d . . . . .
C542 C -0.0442(3) 0.1254(5) 0.0733(3) 0.092(3) Uani 1 1 d . . . . .
H54D H -0.057784 0.164777 0.087962 0.138 Uiso 1 1 calc GR . . . .
H54E H -0.073242 0.086499 0.071700 0.138 Uiso 1 1 calc GR . . . .
H54F H -0.045510 0.138213 0.042130 0.138 Uiso 1 1 calc GR . . . .
C662 C 0.2548(4) 0.1863(4) 0.0761(3) 0.082(2) Uani 1 1 d . . . . .
H66D H 0.272198 0.187900 0.050471 0.123 Uiso 1 1 calc GR . . . .
H66E H 0.209084 0.198073 0.064850 0.123 Uiso 1 1 calc GR . . . .
H66F H 0.260253 0.139810 0.089299 0.123 Uiso 1 1 calc GR . . . .
C242 C -0.1047(4) 0.4312(4) 0.2987(3) 0.088(3) Uani 1 1 d . . . . .
H24A H -0.092568 0.387489 0.287715 0.132 Uiso 1 1 calc GR . . . .
H24B H -0.143607 0.424503 0.307036 0.132 Uiso 1 1 calc GR . . . .
H24C H -0.069681 0.446930 0.325710 0.132 Uiso 1 1 calc GR . . . .
C461 C 0.1444(3) 0.2051(4) 0.3483(2) 0.084(3) Uani 1 1 d . . . . .
H46D H 0.141203 0.222603 0.317631 0.125 Uiso 1 1 calc GR . . . .
H46E H 0.105274 0.216996 0.355256 0.125 Uiso 1 1 calc GR . . . .
H46F H 0.149552 0.154950 0.348880 0.125 Uiso 1 1 calc GR . . . .
C34 C 0.2544(3) 0.4580(3) 0.48142(19) 0.0394(14) Uani 1 1 d . . . . .
C321 C 0.3865(3) 0.2884(3) 0.4768(2) 0.0574(18) Uani 1 1 d . . . . .
H32D H 0.384623 0.297739 0.507756 0.086 Uiso 1 1 calc GR . . . .
H32E H 0.427489 0.266118 0.479323 0.086 Uiso 1 1 calc GR . . . .
H32F H 0.351044 0.257836 0.460374 0.086 Uiso 1 1 calc GR . . . .
C641 C 0.4024(4) 0.4446(6) 0.0341(3) 0.123(4) Uani 1 1 d . . . . .
H64A H 0.400381 0.485610 0.052248 0.184 Uiso 1 1 calc GR . . . .
H64B H 0.422537 0.456608 0.010934 0.184 Uiso 1 1 calc GR . . . .
H64C H 0.427791 0.408824 0.054536 0.184 Uiso 1 1 calc GR . . . .
C441 C 0.3576(4) 0.0356(3) 0.3203(2) 0.064(2) Uani 1 1 d . . . . .
H44D H 0.384907 0.063951 0.307815 0.096 Uiso 1 1 calc GR . . . .
H44E H 0.313093 0.037762 0.299515 0.096 Uiso 1 1 calc GR . . . .
H44F H 0.372508 -0.012305 0.322948 0.096 Uiso 1 1 calc GR . . . .
C722 C 0.5441(3) 0.4630(3) 0.4176(2) 0.0511(16) Uani 1 1 d . . . . .
H72D H 0.527000 0.416202 0.410089 0.077 Uiso 1 1 calc GR . . . .
H72E H 0.533276 0.480237 0.444161 0.077 Uiso 1 1 calc GR . . . .
H72F H 0.590834 0.462134 0.424935 0.077 Uiso 1 1 calc GR . . . .
C121 C -0.0011(4) 0.5272(4) 0.0682(2) 0.071(2) Uani 1 1 d . . . . .
H12D H -0.035654 0.492921 0.060093 0.106 Uiso 1 1 calc GR . . . .
H12E H 0.038041 0.506663 0.065264 0.106 Uiso 1 1 calc GR . . . .
H12F H -0.013796 0.566885 0.047486 0.106 Uiso 1 1 calc GR . . . .
C642 C 0.2969(4) 0.4702(4) -0.0245(2) 0.076(2) Uani 1 1 d . . . . .
H64D H 0.252151 0.454712 -0.036957 0.114 Uiso 1 1 calc GR . . . .
H64E H 0.315042 0.474397 -0.049600 0.114 Uiso 1 1 calc GR . . . .
H64F H 0.298451 0.515012 -0.009468 0.114 Uiso 1 1 calc GR . . . .
C561 C 0.2623(3) 0.1381(3) 0.2054(2) 0.0630(19) Uani 1 1 d . . . . .
H56D H 0.236579 0.098506 0.208807 0.095 Uiso 1 1 calc GR . . . .
H56E H 0.303847 0.137393 0.230082 0.095 Uiso 1 1 calc GR . . . .
H56F H 0.269299 0.135579 0.175447 0.095 Uiso 1 1 calc GR . . . .
C141 C 0.1385(4) 0.8112(6) 0.0742(4) 0.163(6) Uani 1 1 d . . . . .
H14D H 0.127142 0.840797 0.046856 0.245 Uiso 1 1 calc GR . . . .
H14E H 0.169453 0.776256 0.071883 0.245 Uiso 1 1 calc GR . . . .
H14F H 0.157686 0.839291 0.101834 0.245 Uiso 1 1 calc GR . . . .
C241 C -0.1721(3) 0.4641(5) 0.2194(3) 0.109(3) Uani 1 1 d . . . . .
H24D H -0.180021 0.500774 0.196275 0.164 Uiso 1 1 calc GR . . . .
H24E H -0.210720 0.456970 0.228119 0.164 Uiso 1 1 calc GR . . . .
H24F H -0.161485 0.421271 0.206486 0.164 Uiso 1 1 calc GR . . . .
C821 C 0.2759(3) 0.5667(3) 0.3416(2) 0.0481(16) Uani 1 1 d . . . . .
H82D H 0.261427 0.611477 0.349161 0.072 Uiso 1 1 calc GR . . . .
H82E H 0.256595 0.529804 0.354551 0.072 Uiso 1 1 calc GR . . . .
H82F H 0.262928 0.561457 0.308036 0.072 Uiso 1 1 calc GR . . . .
C742 C 0.6798(5) 0.3438(5) 0.3391(4) 0.141(4) Uani 1 1 d . U . . .
H74A H 0.713714 0.313949 0.335310 0.211 Uiso 1 1 calc GR . . . .
H74B H 0.644482 0.315296 0.341833 0.211 Uiso 1 1 calc GR . . . .
H74C H 0.697202 0.371774 0.366946 0.211 Uiso 1 1 calc GR . . . .
C841 C 0.3562(4) 0.8353(3) 0.3576(3) 0.101(3) Uani 1 1 d . . . . .
H84D H 0.343345 0.807679 0.379921 0.152 Uiso 1 1 calc GR . . . .
H84E H 0.322643 0.832815 0.327437 0.152 Uiso 1 1 calc GR . . . .
H84F H 0.362132 0.883370 0.367948 0.152 Uiso 1 1 calc GR . . . .
C53 C 0.0651(3) 0.2216(3) 0.0849(2) 0.0487(16) Uani 1 1 d . . . . .
H53 H 0.030481 0.223396 0.056706 0.058 Uiso 1 1 calc R . . . .
C84 C 0.4125(3) 0.7344(3) 0.3357(2) 0.0473(16) Uani 1 1 d . . . . .
C161 C 0.2704(3) 0.6781(3) 0.2277(2) 0.0560(17) Uani 1 1 d . . . . .
H16D H 0.279271 0.632862 0.216859 0.084 Uiso 1 1 calc GR . . . .
H16E H 0.302431 0.688131 0.257645 0.084 Uiso 1 1 calc GR . . . .
H16F H 0.272298 0.713520 0.205400 0.084 Uiso 1 1 calc GR . . . .
B4 B 0.4017(3) 0.5190(3) 0.28566(19) 0.0326(15) Uani 1 1 d . . . . .
C741 C 0.7030(5) 0.4455(8) 0.3055(6) 0.242(9) Uani 1 1 d . U . . .
H74D H 0.686080 0.483012 0.283506 0.362 Uiso 1 1 calc GR . . . .
H74E H 0.742356 0.427353 0.301399 0.362 Uiso 1 1 calc GR . . . .
H74F H 0.712743 0.463128 0.337004 0.362 Uiso 1 1 calc GR . . . .
C6S C 0.1794(4) 0.7859(5) 0.4628(3) 0.191(5) Uani 1 1 d . U . . .
H6S H 0.180069 0.745240 0.480204 0.229 Uiso 1 1 calc R . . . .
C1S C 0.2048(4) 0.7851(4) 0.4268(3) 0.166(5) Uani 1 1 d G U . . .
C2S C 0.2039(4) 0.8446(5) 0.4014(3) 0.163(4) Uani 1 1 d G U . . .
H2S H 0.221236 0.844054 0.376767 0.195 Uiso 1 1 calc R . . . .
C3S C 0.1775(4) 0.9049(4) 0.4119(3) 0.176(5) Uani 1 1 d G U . . .
H3S H 0.176863 0.945584 0.394510 0.211 Uiso 1 1 calc R . . . .
C4S C 0.1521(4) 0.9057(4) 0.4479(3) 0.193(6) Uani 1 1 d G U . . .
H4S H 0.134093 0.946944 0.455099 0.232 Uiso 1 1 calc R . . . .
C5S C 0.1531(4) 0.8462(6) 0.4733(3) 0.177(5) Uani 1 1 d G U . . .
H5S H 0.135695 0.846772 0.497947 0.212 Uiso 1 1 calc R . . . .
C7S C 0.2250(6) 0.7219(6) 0.4121(4) 0.162(5) Uani 1 1 d . . . . .
H7SA H 0.271727 0.717399 0.425757 0.243 Uiso 1 1 calc GR . . . .
H7SB H 0.213231 0.721767 0.378413 0.243 Uiso 1 1 calc GR . . . .
H7SC H 0.204038 0.683239 0.421984 0.243 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O1 2.152(3) . ?
U1 O3 2.172(3) . ?
U1 O2 2.159(3) . ?
U1 O4 2.158(3) . ?
O1 B1 1.358(7) . ?
O3 B3 1.363(7) . ?
O2 B2 1.372(6) . ?
C16 C11 1.398(7) . ?
C16 C160 1.528(8) . ?
C16 C15 1.401(7) . ?
O4 B4 1.365(7) . ?
C560 H560 1.0000 . ?
C560 C56 1.516(8) . ?
C560 C562 1.512(8) . ?
C560 C561 1.531(8) . ?
C421 H42A 0.9800 . ?
C421 H42B 0.9800 . ?
C421 H42C 0.9800 . ?
C421 C420 1.522(7) . ?
C43 H43 0.9500 . ?
C43 C42 1.381(7) . ?
C43 C44 1.379(7) . ?
C23 H23 0.9500 . ?
C23 C22 1.390(7) . ?
C23 C24 1.390(7) . ?
C360 H360 1.0000 . ?
C360 C361 1.535(7) . ?
C360 C36 1.524(7) . ?
C360 C362 1.512(8) . ?
C440 H440 1.0000 . ?
C440 C442 1.516(10) . ?
C440 C44 1.515(7) . ?
C440 C441 1.517(8) . ?
C52 C51 1.413(7) . ?
C52 C520 1.542(7) . ?
C52 C53 1.391(8) . ?
C620 H620 1.0000 . ?
C620 C621 1.526(8) . ?
C620 C62 1.524(7) . ?
C620 C622 1.536(8) . ?
C71 C72 1.420(7) . ?
C71 C76 1.425(7) . ?
C71 B4 1.612(8) . ?
C760 H760 1.0000 . ?
C760 C76 1.511(8) . ?
C760 C762 1.520(8) . ?
C760 C761 1.537(8) . ?
C621 H62A 0.9800 . ?
C621 H62B 0.9800 . ?
C621 H62C 0.9800 . ?
C11 B1 1.625(8) . ?
C11 C12 1.421(7) . ?
C26 C25 1.397(7) . ?
C26 C260 1.520(7) . ?
C26 C21 1.411(7) . ?
C22 C220 1.525(7) . ?
C22 C21 1.409(7) . ?
C140 H140 1.0000 . ?
C140 C142 1.454(10) . ?
C140 C14 1.516(8) . ?
C140 C141 1.400(10) . ?
C72 C720 1.531(7) . ?
C72 C73 1.381(7) . ?
C160 H160 1.0000 . ?
C160 C162 1.544(8) . ?
C160 C161 1.524(8) . ?
C76 C75 1.391(8) . ?
C460 H460 1.0000 . ?
C460 C46 1.518(7) . ?
C460 C462 1.511(7) . ?
C460 C461 1.510(8) . ?
C33 H33 0.9500 . ?
C33 C32 1.397(7) . ?
C33 C34 1.375(7) . ?
C420 H420 1.0000 . ?
C420 C42 1.532(7) . ?
C420 C422 1.523(7) . ?
C720 H720 1.0000 . ?
C720 C721 1.521(7) . ?
C720 C722 1.523(7) . ?
C840 H840 1.0000 . ?
C840 C842 1.497(11) . ?
C840 C841 1.500(9) . ?
C840 C84 1.520(8) . ?
C82 C83 1.375(7) . ?
C82 C820 1.521(7) . ?
C82 C81 1.407(7) . ?
C31 C32 1.413(7) . ?
C31 B2 1.604(8) . ?
C31 C36 1.421(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.397(7) . ?
C45 C44 1.380(7) . ?
C73 H73 0.9500 . ?
C73 C74 1.383(8) . ?
C220 H220 1.0000 . ?
C220 C221 1.521(7) . ?
C220 C222 1.522(7) . ?
C640 H640 1.0000 . ?
C640 C64 1.507(8) . ?
C640 C641 1.508(10) . ?
C640 C642 1.514(9) . ?
C762 H76A 0.9800 . ?
C762 H76B 0.9800 . ?
C762 H76C 0.9800 . ?
C521 H52A 0.9800 . ?
C521 H52B 0.9800 . ?
C521 H52C 0.9800 . ?
C521 C520 1.537(7) . ?
C122 H12A 0.9800 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C122 C120 1.532(8) . ?
C860 H860 1.0000 . ?
C860 C86 1.533(7) . ?
C860 C862 1.524(7) . ?
C860 C861 1.518(8) . ?
C61 C62 1.417(7) . ?
C61 C66 1.410(7) . ?
C61 B3 1.603(8) . ?
C262 H26A 0.9800 . ?
C262 H26B 0.9800 . ?
C262 H26C 0.9800 . ?
C262 C260 1.534(8) . ?
C63 H63 0.9500 . ?
C63 C62 1.400(7) . ?
C63 C64 1.382(8) . ?
C32 C320 1.522(7) . ?
C25 H25 0.9500 . ?
C25 C24 1.361(7) . ?
C120 H120 1.0000 . ?
C120 C12 1.530(8) . ?
C120 C121 1.529(8) . ?
C41 B2 1.602(8) . ?
C41 C42 1.420(7) . ?
C41 C46 1.406(7) . ?
C86 C85 1.378(7) . ?
C86 C81 1.414(7) . ?
C260 H260 1.0000 . ?
C260 C261 1.527(8) . ?
C341 H34A 0.9800 . ?
C341 H34B 0.9800 . ?
C341 H34C 0.9800 . ?
C341 C340 1.511(8) . ?
C660 H660 1.0000 . ?
C660 C661 1.513(8) . ?
C660 C66 1.524(8) . ?
C660 C662 1.505(8) . ?
C83 H83 0.9500 . ?
C83 C84 1.394(7) . ?
C822 H82A 0.9800 . ?
C822 H82B 0.9800 . ?
C822 H82C 0.9800 . ?
C822 C820 1.530(7) . ?
C142 H14A 0.9800 . ?
C142 H14B 0.9800 . ?
C142 H14C 0.9800 . ?
C221 H22A 0.9800 . ?
C221 H22B 0.9800 . ?
C221 H22C 0.9800 . ?
C361 H36A 0.9800 . ?
C361 H36B 0.9800 . ?
C361 H36C 0.9800 . ?
C661 H66A 0.9800 . ?
C661 H66B 0.9800 . ?
C661 H66C 0.9800 . ?
C820 H820 1.0000 . ?
C820 C821 1.520(8) . ?
C51 C56 1.426(7) . ?
C51 B3 1.603(8) . ?
C54 C540 1.529(9) . ?
C54 C55 1.393(8) . ?
C54 C53 1.384(8) . ?
C65 H65 0.9500 . ?
C65 C66 1.396(7) . ?
C65 C64 1.387(8) . ?
C721 H72A 0.9800 . ?
C721 H72B 0.9800 . ?
C721 H72C 0.9800 . ?
C222 H22D 0.9800 . ?
C222 H22E 0.9800 . ?
C222 H22F 0.9800 . ?
C541 H54A 0.9800 . ?
C541 H54B 0.9800 . ?
C541 H54C 0.9800 . ?
C541 C540 1.515(10) . ?
C740 H740 1.0000 . ?
C740 C74 1.554(10) . ?
C740 C742 1.513(14) . ?
C740 C741 1.463(17) . ?
C540 H540 1.0000 . ?
C540 C542 1.500(9) . ?
C322 H32A 0.9800 . ?
C322 H32B 0.9800 . ?
C322 H32C 0.9800 . ?
C322 C320 1.523(7) . ?
C761 H76D 0.9800 . ?
C761 H76E 0.9800 . ?
C761 H76F 0.9800 . ?
C85 H85 0.9500 . ?
C85 C84 1.376(7) . ?
C261 H26D 0.9800 . ?
C261 H26E 0.9800 . ?
C261 H26F 0.9800 . ?
C162 H16A 0.9800 . ?
C162 H16B 0.9800 . ?
C162 H16C 0.9800 . ?
C36 C35 1.403(7) . ?
C422 H42D 0.9800 . ?
C422 H42E 0.9800 . ?
C422 H42F 0.9800 . ?
C56 C55 1.386(8) . ?
C55 H55 0.9500 . ?
C24 C240 1.535(7) . ?
C35 H35 0.9500 . ?
C35 C34 1.378(8) . ?
C862 H86A 0.9800 . ?
C862 H86B 0.9800 . ?
C862 H86C 0.9800 . ?
C622 H62D 0.9800 . ?
C622 H62E 0.9800 . ?
C622 H62F 0.9800 . ?
C320 H320 1.0000 . ?
C320 C321 1.524(8) . ?
C861 H86D 0.9800 . ?
C861 H86E 0.9800 . ?
C861 H86F 0.9800 . ?
C522 H52D 0.9800 . ?
C522 H52E 0.9800 . ?
C522 H52F 0.9800 . ?
C522 C520 1.537(7) . ?
C240 H240 1.0000 . ?
C240 C242 1.500(9) . ?
C240 C241 1.502(10) . ?
C442 H44A 0.9800 . ?
C442 H44B 0.9800 . ?
C442 H44C 0.9800 . ?
B1 C21 1.606(8) . ?
C520 H520 1.0000 . ?
C340 H340 1.0000 . ?
C340 C342 1.503(9) . ?
C340 C34 1.514(7) . ?
C14 C15 1.376(8) . ?
C14 C13 1.377(8) . ?
C462 H46A 0.9800 . ?
C462 H46B 0.9800 . ?
C462 H46C 0.9800 . ?
C15 H15 0.9500 . ?
C362 H36D 0.9800 . ?
C362 H36E 0.9800 . ?
C362 H36F 0.9800 . ?
C12 C13 1.381(7) . ?
C75 H75 0.9500 . ?
C75 C74 1.381(9) . ?
C81 B4 1.598(8) . ?
C842 H84A 0.9800 . ?
C842 H84B 0.9800 . ?
C842 H84C 0.9800 . ?
C342 H34D 0.9800 . ?
C342 H34E 0.9800 . ?
C342 H34F 0.9800 . ?
C13 H13 0.9500 . ?
C562 H56A 0.9800 . ?
C562 H56B 0.9800 . ?
C562 H56C 0.9800 . ?
C542 H54D 0.9800 . ?
C542 H54E 0.9800 . ?
C542 H54F 0.9800 . ?
C662 H66D 0.9800 . ?
C662 H66E 0.9800 . ?
C662 H66F 0.9800 . ?
C242 H24A 0.9800 . ?
C242 H24B 0.9800 . ?
C242 H24C 0.9800 . ?
C461 H46D 0.9800 . ?
C461 H46E 0.9800 . ?
C461 H46F 0.9800 . ?
C321 H32D 0.9800 . ?
C321 H32E 0.9800 . ?
C321 H32F 0.9800 . ?
C641 H64A 0.9800 . ?
C641 H64B 0.9800 . ?
C641 H64C 0.9800 . ?
C441 H44D 0.9800 . ?
C441 H44E 0.9800 . ?
C441 H44F 0.9800 . ?
C722 H72D 0.9800 . ?
C722 H72E 0.9800 . ?
C722 H72F 0.9800 . ?
C121 H12D 0.9800 . ?
C121 H12E 0.9800 . ?
C121 H12F 0.9800 . ?
C642 H64D 0.9800 . ?
C642 H64E 0.9800 . ?
C642 H64F 0.9800 . ?
C561 H56D 0.9800 . ?
C561 H56E 0.9800 . ?
C561 H56F 0.9800 . ?
C141 H14D 0.9800 . ?
C141 H14E 0.9800 . ?
C141 H14F 0.9800 . ?
C241 H24D 0.9800 . ?
C241 H24E 0.9800 . ?
C241 H24F 0.9800 . ?
C821 H82D 0.9800 . ?
C821 H82E 0.9800 . ?
C821 H82F 0.9800 . ?
C742 H74A 0.9800 . ?
C742 H74B 0.9800 . ?
C742 H74C 0.9800 . ?
C841 H84D 0.9800 . ?
C841 H84E 0.9800 . ?
C841 H84F 0.9800 . ?
C53 H53 0.9500 . ?
C161 H16D 0.9800 . ?
C161 H16E 0.9800 . ?
C161 H16F 0.9800 . ?
C741 H74D 0.9800 . ?
C741 H74E 0.9800 . ?
C741 H74F 0.9800 . ?
C6S H6S 0.9500 . ?
C6S C1S 1.3900 . ?
C6S C5S 1.3900 . ?
C1S C2S 1.3900 . ?
C1S C7S 1.426(12) . ?
C2S H2S 0.9500 . ?
C2S C3S 1.3900 . ?
C3S H3S 0.9500 . ?
C3S C4S 1.3900 . ?
C4S H4S 0.9500 . ?
C4S C5S 1.3900 . ?
C5S H5S 0.9500 . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?

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
O1 U1 O3 100.41(13) . . ?
O1 U1 O2 114.13(12) . . ?
O1 U1 O4 113.61(13) . . ?
O2 U1 O3 115.97(13) . . ?
O4 U1 O3 113.88(12) . . ?
O4 U1 O2 99.59(12) . . ?
B1 O1 U1 170.5(4) . . ?
B3 O3 U1 171.7(4) . . ?
B2 O2 U1 171.4(3) . . ?
C11 C16 C160 123.0(5) . . ?
C11 C16 C15 119.2(5) . . ?
C15 C16 C160 117.8(5) . . ?
B4 O4 U1 171.0(3) . . ?
C56 C560 H560 108.0 . . ?
C56 C560 C561 112.1(5) . . ?
C562 C560 H560 108.0 . . ?
C562 C560 C56 112.3(5) . . ?
C562 C560 C561 108.3(5) . . ?
C561 C560 H560 108.0 . . ?
H42A C421 H42B 109.5 . . ?
H42A C421 H42C 109.5 . . ?
H42B C421 H42C 109.5 . . ?
C420 C421 H42A 109.5 . . ?
C420 C421 H42B 109.5 . . ?
C420 C421 H42C 109.5 . . ?
C42 C43 H43 118.7 . . ?
C44 C43 H43 118.7 . . ?
C44 C43 C42 122.5(5) . . ?
C22 C23 H23 119.0 . . ?
C22 C23 C24 121.9(5) . . ?
C24 C23 H23 119.0 . . ?
C361 C360 H360 107.7 . . ?
C36 C360 H360 107.7 . . ?
C36 C360 C361 112.1(5) . . ?
C362 C360 H360 107.7 . . ?
C362 C360 C361 108.9(5) . . ?
C362 C360 C36 112.5(5) . . ?
C442 C440 H440 107.3 . . ?
C44 C440 H440 107.3 . . ?
C44 C440 C442 111.9(6) . . ?
C44 C440 C441 111.7(5) . . ?
C441 C440 H440 107.3 . . ?
C441 C440 C442 111.1(5) . . ?
C51 C52 C520 122.4(5) . . ?
C53 C52 C51 121.3(5) . . ?
C53 C52 C520 116.3(5) . . ?
C621 C620 H620 108.2 . . ?
C621 C620 C622 109.4(5) . . ?
C62 C620 H620 108.2 . . ?
C62 C620 C621 109.7(5) . . ?
C62 C620 C622 113.0(5) . . ?
C622 C620 H620 108.2 . . ?
C72 C71 C76 117.0(5) . . ?
C72 C71 B4 121.0(4) . . ?
C76 C71 B4 121.8(5) . . ?
C76 C760 H760 107.8 . . ?
C76 C760 C762 112.5(5) . . ?
C76 C760 C761 112.7(5) . . ?
C762 C760 H760 107.8 . . ?
C762 C760 C761 108.0(5) . . ?
C761 C760 H760 107.8 . . ?
C620 C621 H62A 109.5 . . ?
C620 C621 H62B 109.5 . . ?
C620 C621 H62C 109.5 . . ?
H62A C621 H62B 109.5 . . ?
H62A C621 H62C 109.5 . . ?
H62B C621 H62C 109.5 . . ?
C16 C11 B1 121.7(5) . . ?
C16 C11 C12 118.1(5) . . ?
C12 C11 B1 120.2(5) . . ?
C25 C26 C260 118.0(5) . . ?
C25 C26 C21 119.9(5) . . ?
C21 C26 C260 122.1(5) . . ?
C23 C22 C220 117.8(5) . . ?
C23 C22 C21 119.8(5) . . ?
C21 C22 C220 122.3(4) . . ?
C142 C140 H140 102.2 . . ?
C142 C140 C14 112.0(6) . . ?
C14 C140 H140 102.2 . . ?
C141 C140 H140 102.2 . . ?
C141 C140 C142 118.4(8) . . ?
C141 C140 C14 116.5(7) . . ?
C71 C72 C720 122.6(5) . . ?
C73 C72 C71 120.6(5) . . ?
C73 C72 C720 116.8(5) . . ?
C16 C160 H160 108.0 . . ?
C16 C160 C162 112.9(5) . . ?
C162 C160 H160 108.0 . . ?
C161 C160 C16 112.3(5) . . ?
C161 C160 H160 108.0 . . ?
C161 C160 C162 107.5(5) . . ?
C71 C76 C760 123.1(5) . . ?
C75 C76 C71 119.5(5) . . ?
C75 C76 C760 117.4(5) . . ?
C46 C460 H460 106.9 . . ?
C462 C460 H460 106.9 . . ?
C462 C460 C46 113.4(5) . . ?
C461 C460 H460 106.9 . . ?
C461 C460 C46 111.7(5) . . ?
C461 C460 C462 110.7(5) . . ?
C32 C33 H33 118.7 . . ?
C34 C33 H33 118.7 . . ?
C34 C33 C32 122.6(5) . . ?
C421 C420 H420 108.0 . . ?
C421 C420 C42 110.2(4) . . ?
C421 C420 C422 109.6(5) . . ?
C42 C420 H420 108.0 . . ?
C422 C420 H420 108.0 . . ?
C422 C420 C42 112.8(5) . . ?
C72 C720 H720 108.1 . . ?
C721 C720 C72 111.4(4) . . ?
C721 C720 H720 108.1 . . ?
C721 C720 C722 108.6(5) . . ?
C722 C720 C72 112.4(5) . . ?
C722 C720 H720 108.1 . . ?
C842 C840 H840 107.1 . . ?
C842 C840 C841 112.1(7) . . ?
C842 C840 C84 109.7(7) . . ?
C841 C840 H840 107.1 . . ?
C841 C840 C84 113.3(6) . . ?
C84 C840 H840 107.1 . . ?
C83 C82 C820 118.6(5) . . ?
C83 C82 C81 119.4(5) . . ?
C81 C82 C820 122.0(5) . . ?
C32 C31 B2 121.6(4) . . ?
C32 C31 C36 117.4(5) . . ?
C36 C31 B2 120.9(5) . . ?
C46 C45 H45 119.0 . . ?
C44 C45 H45 119.0 . . ?
C44 C45 C46 122.0(5) . . ?
C72 C73 H73 118.7 . . ?
C72 C73 C74 122.7(6) . . ?
C74 C73 H73 118.7 . . ?
C22 C220 H220 107.3 . . ?
C221 C220 C22 114.3(4) . . ?
C221 C220 H220 107.3 . . ?
C221 C220 C222 109.5(5) . . ?
C222 C220 C22 110.8(4) . . ?
C222 C220 H220 107.3 . . ?
C64 C640 H640 107.4 . . ?
C64 C640 C642 113.4(5) . . ?
C641 C640 H640 107.4 . . ?
C641 C640 C64 110.4(6) . . ?
C641 C640 C642 110.5(7) . . ?
C642 C640 H640 107.4 . . ?
C760 C762 H76A 109.5 . . ?
C760 C762 H76B 109.5 . . ?
C760 C762 H76C 109.5 . . ?
H76A C762 H76B 109.5 . . ?
H76A C762 H76C 109.5 . . ?
H76B C762 H76C 109.5 . . ?
H52A C521 H52B 109.5 . . ?
H52A C521 H52C 109.5 . . ?
H52B C521 H52C 109.5 . . ?
C520 C521 H52A 109.5 . . ?
C520 C521 H52B 109.5 . . ?
C520 C521 H52C 109.5 . . ?
H12A C122 H12B 109.5 . . ?
H12A C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C120 C122 H12A 109.5 . . ?
C120 C122 H12B 109.5 . . ?
C120 C122 H12C 109.5 . . ?
C86 C860 H860 107.1 . . ?
C862 C860 H860 107.1 . . ?
C862 C860 C86 111.4(5) . . ?
C861 C860 H860 107.1 . . ?
C861 C860 C86 112.8(5) . . ?
C861 C860 C862 111.1(5) . . ?
C62 C61 B3 121.6(5) . . ?
C66 C61 C62 116.4(5) . . ?
C66 C61 B3 122.0(5) . . ?
H26A C262 H26B 109.5 . . ?
H26A C262 H26C 109.5 . . ?
H26B C262 H26C 109.5 . . ?
C260 C262 H26A 109.5 . . ?
C260 C262 H26B 109.5 . . ?
C260 C262 H26C 109.5 . . ?
C62 C63 H63 118.7 . . ?
C64 C63 H63 118.7 . . ?
C64 C63 C62 122.6(6) . . ?
C33 C32 C31 120.2(5) . . ?
C33 C32 C320 116.9(5) . . ?
C31 C32 C320 122.9(4) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 C26 122.3(5) . . ?
C24 C25 H25 118.9 . . ?
C122 C120 H120 107.7 . . ?
C12 C120 C122 111.5(5) . . ?
C12 C120 H120 107.7 . . ?
C121 C120 C122 108.4(5) . . ?
C121 C120 H120 107.7 . . ?
C121 C120 C12 113.6(5) . . ?
C42 C41 B2 122.2(4) . . ?
C46 C41 B2 120.6(4) . . ?
C46 C41 C42 117.1(5) . . ?
C85 C86 C860 117.8(5) . . ?
C85 C86 C81 120.2(5) . . ?
C81 C86 C860 122.0(5) . . ?
C26 C260 C262 112.7(5) . . ?
C26 C260 H260 107.0 . . ?
C26 C260 C261 112.5(5) . . ?
C262 C260 H260 107.0 . . ?
C261 C260 C262 110.3(5) . . ?
C261 C260 H260 107.0 . . ?
H34A C341 H34B 109.5 . . ?
H34A C341 H34C 109.5 . . ?
H34B C341 H34C 109.5 . . ?
C340 C341 H34A 109.5 . . ?
C340 C341 H34B 109.5 . . ?
C340 C341 H34C 109.5 . . ?
C661 C660 H660 107.0 . . ?
C661 C660 C66 112.2(5) . . ?
C66 C660 H660 107.0 . . ?
C662 C660 H660 107.0 . . ?
C662 C660 C661 110.7(6) . . ?
C662 C660 C66 112.6(5) . . ?
O2 B2 C31 120.7(5) . . ?
O2 B2 C41 119.2(5) . . ?
C41 B2 C31 120.1(5) . . ?
C82 C83 H83 118.3 . . ?
C82 C83 C84 123.5(5) . . ?
C84 C83 H83 118.3 . . ?
C43 C42 C420 119.2(4) . . ?
C43 C42 C41 120.3(5) . . ?
C41 C42 C420 120.5(4) . . ?
H82A C822 H82B 109.5 . . ?
H82A C822 H82C 109.5 . . ?
H82B C822 H82C 109.5 . . ?
C820 C822 H82A 109.5 . . ?
C820 C822 H82B 109.5 . . ?
C820 C822 H82C 109.5 . . ?
C140 C142 H14A 109.5 . . ?
C140 C142 H14B 109.5 . . ?
C140 C142 H14C 109.5 . . ?
H14A C142 H14B 109.5 . . ?
H14A C142 H14C 109.5 . . ?
H14B C142 H14C 109.5 . . ?
C45 C46 C460 118.2(5) . . ?
C45 C46 C41 120.4(5) . . ?
C41 C46 C460 121.3(5) . . ?
C220 C221 H22A 109.5 . . ?
C220 C221 H22B 109.5 . . ?
C220 C221 H22C 109.5 . . ?
H22A C221 H22B 109.5 . . ?
H22A C221 H22C 109.5 . . ?
H22B C221 H22C 109.5 . . ?
C360 C361 H36A 109.5 . . ?
C360 C361 H36B 109.5 . . ?
C360 C361 H36C 109.5 . . ?
H36A C361 H36B 109.5 . . ?
H36A C361 H36C 109.5 . . ?
H36B C361 H36C 109.5 . . ?
C660 C661 H66A 109.5 . . ?
C660 C661 H66B 109.5 . . ?
C660 C661 H66C 109.5 . . ?
H66A C661 H66B 109.5 . . ?
H66A C661 H66C 109.5 . . ?
H66B C661 H66C 109.5 . . ?
C82 C820 C822 113.3(5) . . ?
C82 C820 H820 108.0 . . ?
C822 C820 H820 108.0 . . ?
C821 C820 C82 110.6(4) . . ?
C821 C820 C822 108.9(4) . . ?
C821 C820 H820 108.0 . . ?
C52 C51 C56 116.5(5) . . ?
C52 C51 B3 121.9(5) . . ?
C56 C51 B3 121.6(5) . . ?
C61 C62 C620 121.3(5) . . ?
C63 C62 C620 118.0(5) . . ?
C63 C62 C61 120.6(5) . . ?
C55 C54 C540 120.8(6) . . ?
C53 C54 C540 122.3(6) . . ?
C53 C54 C55 116.8(6) . . ?
C66 C65 H65 118.9 . . ?
C64 C65 H65 118.9 . . ?
C64 C65 C66 122.1(5) . . ?
C720 C721 H72A 109.5 . . ?
C720 C721 H72B 109.5 . . ?
C720 C721 H72C 109.5 . . ?
H72A C721 H72B 109.5 . . ?
H72A C721 H72C 109.5 . . ?
H72B C721 H72C 109.5 . . ?
C220 C222 H22D 109.5 . . ?
C220 C222 H22E 109.5 . . ?
C220 C222 H22F 109.5 . . ?
H22D C222 H22E 109.5 . . ?
H22D C222 H22F 109.5 . . ?
H22E C222 H22F 109.5 . . ?
H54A C541 H54B 109.5 . . ?
H54A C541 H54C 109.5 . . ?
H54B C541 H54C 109.5 . . ?
C540 C541 H54A 109.5 . . ?
C540 C541 H54B 109.5 . . ?
C540 C541 H54C 109.5 . . ?
C74 C740 H740 111.1 . . ?
C742 C740 H740 111.1 . . ?
C742 C740 C74 110.8(8) . . ?
C741 C740 H740 111.1 . . ?
C741 C740 C74 107.7(11) . . ?
C741 C740 C742 104.8(8) . . ?
C54 C540 H540 107.4 . . ?
C541 C540 C54 109.7(6) . . ?
C541 C540 H540 107.4 . . ?
C542 C540 C54 114.4(6) . . ?
C542 C540 C541 110.3(7) . . ?
C542 C540 H540 107.4 . . ?
H32A C322 H32B 109.5 . . ?
H32A C322 H32C 109.5 . . ?
H32B C322 H32C 109.5 . . ?
C320 C322 H32A 109.5 . . ?
C320 C322 H32B 109.5 . . ?
C320 C322 H32C 109.5 . . ?
C760 C761 H76D 109.5 . . ?
C760 C761 H76E 109.5 . . ?
C760 C761 H76F 109.5 . . ?
H76D C761 H76E 109.5 . . ?
H76D C761 H76F 109.5 . . ?
H76E C761 H76F 109.5 . . ?
C86 C85 H85 118.6 . . ?
C84 C85 C86 122.8(5) . . ?
C84 C85 H85 118.6 . . ?
C260 C261 H26D 109.5 . . ?
C260 C261 H26E 109.5 . . ?
C260 C261 H26F 109.5 . . ?
H26D C261 H26E 109.5 . . ?
H26D C261 H26F 109.5 . . ?
H26E C261 H26F 109.5 . . ?
C160 C162 H16A 109.5 . . ?
C160 C162 H16B 109.5 . . ?
C160 C162 H16C 109.5 . . ?
H16A C162 H16B 109.5 . . ?
H16A C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C31 C36 C360 123.8(5) . . ?
C35 C36 C360 116.6(5) . . ?
C35 C36 C31 119.4(5) . . ?
C420 C422 H42D 109.5 . . ?
C420 C422 H42E 109.5 . . ?
C420 C422 H42F 109.5 . . ?
H42D C422 H42E 109.5 . . ?
H42D C422 H42F 109.5 . . ?
H42E C422 H42F 109.5 . . ?
C51 C56 C560 122.4(5) . . ?
C55 C56 C560 117.4(5) . . ?
C55 C56 C51 120.1(5) . . ?
C61 C66 C660 121.0(5) . . ?
C65 C66 C61 121.3(5) . . ?
C65 C66 C660 117.6(5) . . ?
O3 B3 C61 119.3(5) . . ?
O3 B3 C51 121.9(5) . . ?
C61 B3 C51 118.9(5) . . ?
C54 C55 H55 118.5 . . ?
C56 C55 C54 123.0(6) . . ?
C56 C55 H55 118.5 . . ?
C63 C64 C640 121.7(6) . . ?
C63 C64 C65 117.0(5) . . ?
C65 C64 C640 121.3(5) . . ?
C23 C24 C240 120.7(5) . . ?
C25 C24 C23 118.2(5) . . ?
C25 C24 C240 121.1(5) . . ?
C36 C35 H35 118.6 . . ?
C34 C35 C36 122.8(5) . . ?
C34 C35 H35 118.6 . . ?
C860 C862 H86A 109.5 . . ?
C860 C862 H86B 109.5 . . ?
C860 C862 H86C 109.5 . . ?
H86A C862 H86B 109.5 . . ?
H86A C862 H86C 109.5 . . ?
H86B C862 H86C 109.5 . . ?
C620 C622 H62D 109.5 . . ?
C620 C622 H62E 109.5 . . ?
C620 C622 H62F 109.5 . . ?
H62D C622 H62E 109.5 . . ?
H62D C622 H62F 109.5 . . ?
H62E C622 H62F 109.5 . . ?
C32 C320 C322 113.5(5) . . ?
C32 C320 H320 107.2 . . ?
C32 C320 C321 111.9(4) . . ?
C322 C320 H320 107.2 . . ?
C322 C320 C321 109.6(5) . . ?
C321 C320 H320 107.2 . . ?
C860 C861 H86D 109.5 . . ?
C860 C861 H86E 109.5 . . ?
C860 C861 H86F 109.5 . . ?
H86D C861 H86E 109.5 . . ?
H86D C861 H86F 109.5 . . ?
H86E C861 H86F 109.5 . . ?
H52D C522 H52E 109.5 . . ?
H52D C522 H52F 109.5 . . ?
H52E C522 H52F 109.5 . . ?
C520 C522 H52D 109.5 . . ?
C520 C522 H52E 109.5 . . ?
C520 C522 H52F 109.5 . . ?
C24 C240 H240 107.0 . . ?
C242 C240 C24 111.7(5) . . ?
C242 C240 H240 107.0 . . ?
C242 C240 C241 111.9(6) . . ?
C241 C240 C24 111.8(6) . . ?
C241 C240 H240 107.0 . . ?
C440 C442 H44A 109.5 . . ?
C440 C442 H44B 109.5 . . ?
C440 C442 H44C 109.5 . . ?
H44A C442 H44B 109.5 . . ?
H44A C442 H44C 109.5 . . ?
H44B C442 H44C 109.5 . . ?
O1 B1 C11 121.4(5) . . ?
O1 B1 C21 120.7(5) . . ?
C21 B1 C11 117.9(5) . . ?
C52 C520 H520 107.9 . . ?
C521 C520 C52 111.3(5) . . ?
C521 C520 C522 109.3(5) . . ?
C521 C520 H520 107.9 . . ?
C522 C520 C52 112.4(5) . . ?
C522 C520 H520 107.9 . . ?
C341 C340 H340 107.1 . . ?
C341 C340 C34 114.5(6) . . ?
C342 C340 C341 110.2(6) . . ?
C342 C340 H340 107.1 . . ?
C342 C340 C34 110.4(5) . . ?
C34 C340 H340 107.1 . . ?
C15 C14 C140 122.6(6) . . ?
C15 C14 C13 116.9(5) . . ?
C13 C14 C140 120.5(6) . . ?
C26 C21 B1 120.4(5) . . ?
C22 C21 C26 118.0(4) . . ?
C22 C21 B1 121.5(4) . . ?
C460 C462 H46A 109.5 . . ?
C460 C462 H46B 109.5 . . ?
C460 C462 H46C 109.5 . . ?
H46A C462 H46B 109.5 . . ?
H46A C462 H46C 109.5 . . ?
H46B C462 H46C 109.5 . . ?
C16 C15 H15 118.4 . . ?
C14 C15 C16 123.1(6) . . ?
C14 C15 H15 118.4 . . ?
C360 C362 H36D 109.5 . . ?
C360 C362 H36E 109.5 . . ?
C360 C362 H36F 109.5 . . ?
H36D C362 H36E 109.5 . . ?
H36D C362 H36F 109.5 . . ?
H36E C362 H36F 109.5 . . ?
C11 C12 C120 123.0(5) . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 C120 117.2(5) . . ?
C43 C44 C440 121.1(5) . . ?
C43 C44 C45 117.6(5) . . ?
C45 C44 C440 121.3(5) . . ?
C76 C75 H75 118.4 . . ?
C74 C75 C76 123.3(5) . . ?
C74 C75 H75 118.4 . . ?
C82 C81 C86 117.8(5) . . ?
C82 C81 B4 121.4(4) . . ?
C86 C81 B4 120.7(4) . . ?
C840 C842 H84A 109.5 . . ?
C840 C842 H84B 109.5 . . ?
C840 C842 H84C 109.5 . . ?
H84A C842 H84B 109.5 . . ?
H84A C842 H84C 109.5 . . ?
H84B C842 H84C 109.5 . . ?
C340 C342 H34D 109.5 . . ?
C340 C342 H34E 109.5 . . ?
C340 C342 H34F 109.5 . . ?
H34D C342 H34E 109.5 . . ?
H34D C342 H34F 109.5 . . ?
H34E C342 H34F 109.5 . . ?
C14 C13 C12 122.9(6) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
C560 C562 H56A 109.5 . . ?
C560 C562 H56B 109.5 . . ?
C560 C562 H56C 109.5 . . ?
H56A C562 H56B 109.5 . . ?
H56A C562 H56C 109.5 . . ?
H56B C562 H56C 109.5 . . ?
C73 C74 C740 123.5(6) . . ?
C75 C74 C73 116.9(6) . . ?
C75 C74 C740 119.5(6) . . ?
C540 C542 H54D 109.5 . . ?
C540 C542 H54E 109.5 . . ?
C540 C542 H54F 109.5 . . ?
H54D C542 H54E 109.5 . . ?
H54D C542 H54F 109.5 . . ?
H54E C542 H54F 109.5 . . ?
C660 C662 H66D 109.5 . . ?
C660 C662 H66E 109.5 . . ?
C660 C662 H66F 109.5 . . ?
H66D C662 H66E 109.5 . . ?
H66D C662 H66F 109.5 . . ?
H66E C662 H66F 109.5 . . ?
C240 C242 H24A 109.5 . . ?
C240 C242 H24B 109.5 . . ?
C240 C242 H24C 109.5 . . ?
H24A C242 H24B 109.5 . . ?
H24A C242 H24C 109.5 . . ?
H24B C242 H24C 109.5 . . ?
C460 C461 H46D 109.5 . . ?
C460 C461 H46E 109.5 . . ?
C460 C461 H46F 109.5 . . ?
H46D C461 H46E 109.5 . . ?
H46D C461 H46F 109.5 . . ?
H46E C461 H46F 109.5 . . ?
C33 C34 C35 117.5(5) . . ?
C33 C34 C340 121.8(5) . . ?
C35 C34 C340 120.7(5) . . ?
C320 C321 H32D 109.5 . . ?
C320 C321 H32E 109.5 . . ?
C320 C321 H32F 109.5 . . ?
H32D C321 H32E 109.5 . . ?
H32D C321 H32F 109.5 . . ?
H32E C321 H32F 109.5 . . ?
C640 C641 H64A 109.5 . . ?
C640 C641 H64B 109.5 . . ?
C640 C641 H64C 109.5 . . ?
H64A C641 H64B 109.5 . . ?
H64A C641 H64C 109.5 . . ?
H64B C641 H64C 109.5 . . ?
C440 C441 H44D 109.5 . . ?
C440 C441 H44E 109.5 . . ?
C440 C441 H44F 109.5 . . ?
H44D C441 H44E 109.5 . . ?
H44D C441 H44F 109.5 . . ?
H44E C441 H44F 109.5 . . ?
C720 C722 H72D 109.5 . . ?
C720 C722 H72E 109.5 . . ?
C720 C722 H72F 109.5 . . ?
H72D C722 H72E 109.5 . . ?
H72D C722 H72F 109.5 . . ?
H72E C722 H72F 109.5 . . ?
C120 C121 H12D 109.5 . . ?
C120 C121 H12E 109.5 . . ?
C120 C121 H12F 109.5 . . ?
H12D C121 H12E 109.5 . . ?
H12D C121 H12F 109.5 . . ?
H12E C121 H12F 109.5 . . ?
C640 C642 H64D 109.5 . . ?
C640 C642 H64E 109.5 . . ?
C640 C642 H64F 109.5 . . ?
H64D C642 H64E 109.5 . . ?
H64D C642 H64F 109.5 . . ?
H64E C642 H64F 109.5 . . ?
C560 C561 H56D 109.5 . . ?
C560 C561 H56E 109.5 . . ?
C560 C561 H56F 109.5 . . ?
H56D C561 H56E 109.5 . . ?
H56D C561 H56F 109.5 . . ?
H56E C561 H56F 109.5 . . ?
C140 C141 H14D 109.5 . . ?
C140 C141 H14E 109.5 . . ?
C140 C141 H14F 109.5 . . ?
H14D C141 H14E 109.5 . . ?
H14D C141 H14F 109.5 . . ?
H14E C141 H14F 109.5 . . ?
C240 C241 H24D 109.5 . . ?
C240 C241 H24E 109.5 . . ?
C240 C241 H24F 109.5 . . ?
H24D C241 H24E 109.5 . . ?
H24D C241 H24F 109.5 . . ?
H24E C241 H24F 109.5 . . ?
C820 C821 H82D 109.5 . . ?
C820 C821 H82E 109.5 . . ?
C820 C821 H82F 109.5 . . ?
H82D C821 H82E 109.5 . . ?
H82D C821 H82F 109.5 . . ?
H82E C821 H82F 109.5 . . ?
C740 C742 H74A 109.5 . . ?
C740 C742 H74B 109.5 . . ?
C740 C742 H74C 109.5 . . ?
H74A C742 H74B 109.5 . . ?
H74A C742 H74C 109.5 . . ?
H74B C742 H74C 109.5 . . ?
C840 C841 H84D 109.5 . . ?
C840 C841 H84E 109.5 . . ?
C840 C841 H84F 109.5 . . ?
H84D C841 H84E 109.5 . . ?
H84D C841 H84F 109.5 . . ?
H84E C841 H84F 109.5 . . ?
C52 C53 H53 118.9 . . ?
C54 C53 C52 122.1(6) . . ?
C54 C53 H53 118.9 . . ?
C83 C84 C840 121.9(5) . . ?
C85 C84 C840 121.8(5) . . ?
C85 C84 C83 116.4(5) . . ?
C160 C161 H16D 109.5 . . ?
C160 C161 H16E 109.5 . . ?
C160 C161 H16F 109.5 . . ?
H16D C161 H16E 109.5 . . ?
H16D C161 H16F 109.5 . . ?
H16E C161 H16F 109.5 . . ?
O4 B4 C71 121.3(5) . . ?
O4 B4 C81 120.3(5) . . ?
C81 B4 C71 118.3(5) . . ?
C740 C741 H74D 109.5 . . ?
C740 C741 H74E 109.5 . . ?
C740 C741 H74F 109.5 . . ?
H74D C741 H74E 109.5 . . ?
H74D C741 H74F 109.5 . . ?
H74E C741 H74F 109.5 . . ?
C1S C6S H6S 120.0 . . ?
C1S C6S C5S 120.0 . . ?
C5S C6S H6S 120.0 . . ?
C6S C1S C7S 120.6(8) . . ?
C2S C1S C6S 120.0 . . ?
C2S C1S C7S 119.0(8) . . ?
C1S C2S H2S 120.0 . . ?
C1S C2S C3S 120.0 . . ?
C3S C2S H2S 120.0 . . ?
C2S C3S H3S 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3S 120.0 . . ?
C3S C4S H4S 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C5S C4S H4S 120.0 . . ?
C6S C5S H5S 120.0 . . ?
C4S C5S C6S 120.0 . . ?
C4S C5S H5S 120.0 . . ?
C1S C7S H7SA 109.5 . . ?
C1S C7S H7SB 109.5 . . ?
C1S C7S H7SC 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.108 0.135 0.984 30.3 0.0 ?
2 0.108 0.365 0.484 30.3 0.0 ?
3 0.500 0.500 0.000 504.8 92.7 ?
4 0.500 1.000 0.500 504.8 92.7 ?
5 0.892 0.635 0.516 30.3 0.0 ?
6 0.892 0.865 0.016 30.3 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.864
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_P18083
_database_code_depnum_ccdc_archive 'CCDC 1886811'
loop_
_audit_author_name
_audit_author_address
'polly arnold' 'university of edinburgh'
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H100 B N3 O Si6 U'
_chemical_formula_weight         1152.68

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'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.9897(2)
_cell_length_b                   17.1462(2)
_cell_length_c                   36.7532(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11966.9(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34926
_cell_measurement_theta_min      3.1950
_cell_measurement_theta_max      26.0670

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_F_000             4784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.866
_shelx_estimated_absorpt_T_min   0.512
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 16.1042
_diffrn_reflns_number            226405
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.833
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10934
_reflns_number_gt                8715
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+28.1040P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10934
_refine_ls_number_parameters     571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.58077(2) 0.95441(2) 0.14341(2) 0.01791(5) Uani 1 1 d . . . . .
Si1 Si 0.59611(7) 0.97130(7) 0.05256(3) 0.0293(3) Uani 1 1 d . . . . .
Si2 Si 0.73324(7) 0.92330(8) 0.08365(3) 0.0294(3) Uani 1 1 d . . . . .
Si3 Si 0.71423(7) 0.97684(7) 0.20771(3) 0.0275(3) Uani 1 1 d . . . . .
Si4 Si 0.62911(7) 0.83278(7) 0.21855(3) 0.0258(3) Uani 1 1 d . . . . .
Si5 Si 0.48461(7) 1.07084(8) 0.19841(4) 0.0350(3) Uani 1 1 d . . . . .
Si6 Si 0.56300(7) 1.16552(7) 0.14315(4) 0.0400(3) Uani 1 1 d . . . . .
O1 O 0.49279(14) 0.88546(15) 0.12402(7) 0.0187(6) Uani 1 1 d . . . . .
N1 N 0.64496(17) 0.9478(2) 0.09177(9) 0.0232(8) Uani 1 1 d . . . . .
N2 N 0.64495(17) 0.91694(19) 0.19303(9) 0.0212(8) Uani 1 1 d . . . . .
N3 N 0.54217(19) 1.0737(2) 0.16136(10) 0.0274(8) Uani 1 1 d . . . . .
B1 B 0.4459(2) 0.8315(3) 0.11148(12) 0.0181(10) Uani 1 1 d . . . . .
C1 C 0.4526(2) 0.7432(2) 0.12580(10) 0.0175(9) Uani 1 1 d . . . . .
C2 C 0.5102(2) 0.6951(2) 0.11722(10) 0.0184(9) Uani 1 1 d . . . . .
C3 C 0.5117(2) 0.6177(2) 0.12880(11) 0.0243(10) Uani 1 1 d . . . . .
H3 H 0.5499 0.5867 0.1224 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4583(2) 0.5853(2) 0.14955(11) 0.0245(10) Uani 1 1 d . . . . .
C5 C 0.4023(2) 0.6338(2) 0.15893(11) 0.0244(10) Uani 1 1 d . . . . .
H5 H 0.3661 0.6137 0.1732 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3987(2) 0.7112(2) 0.14774(11) 0.0216(9) Uani 1 1 d . . . . .
C7 C 0.5729(2) 0.7240(2) 0.09487(11) 0.0253(10) Uani 1 1 d . . . . .
H7 H 0.5620 0.7768 0.0864 0.030 Uiso 1 1 calc R U . . .
C8 C 0.5881(2) 0.6740(3) 0.06165(12) 0.0315(11) Uani 1 1 d . . . . .
H8A H 0.6047 0.6237 0.0693 0.047 Uiso 1 1 calc R U . . .
H8B H 0.6235 0.6988 0.0470 0.047 Uiso 1 1 calc R U . . .
H8C H 0.5458 0.6679 0.0477 0.047 Uiso 1 1 calc R U . . .
C9 C 0.6389(2) 0.7289(3) 0.11884(13) 0.0373(12) Uani 1 1 d . . . . .
H9A H 0.6307 0.7650 0.1383 0.056 Uiso 1 1 calc R U . . .
H9B H 0.6780 0.7464 0.1045 0.056 Uiso 1 1 calc R U . . .
H9C H 0.6491 0.6783 0.1287 0.056 Uiso 1 1 calc R U . . .
C10 C 0.4588(3) 0.5003(3) 0.16059(13) 0.0342(11) Uani 1 1 d . . . . .
H10 H 0.4260 0.4946 0.1810 0.041 Uiso 1 1 calc R U . . .
C11 C 0.5300(3) 0.4716(3) 0.17340(17) 0.0565(16) Uani 1 1 d . . . . .
H11A H 0.5622 0.4707 0.1533 0.085 Uiso 1 1 calc R U . . .
H11B H 0.5253 0.4200 0.1832 0.085 Uiso 1 1 calc R U . . .
H11C H 0.5477 0.5060 0.1919 0.085 Uiso 1 1 calc R U . . .
C12 C 0.4318(3) 0.4490(3) 0.12973(17) 0.0586(16) Uani 1 1 d . . . . .
H12A H 0.3873 0.4685 0.1214 0.088 Uiso 1 1 calc R U . . .
H12B H 0.4262 0.3965 0.1383 0.088 Uiso 1 1 calc R U . . .
H12C H 0.4650 0.4497 0.1100 0.088 Uiso 1 1 calc R U . . .
C13 C 0.3364(2) 0.7600(3) 0.16027(11) 0.0252(10) Uani 1 1 d . . . . .
H13 H 0.3455 0.8138 0.1525 0.030 Uiso 1 1 calc R U . . .
C14 C 0.3293(3) 0.7614(3) 0.20148(12) 0.0408(13) Uani 1 1 d . . . . .
H14A H 0.3178 0.7101 0.2101 0.061 Uiso 1 1 calc R U . . .
H14B H 0.2927 0.7971 0.2083 0.061 Uiso 1 1 calc R U . . .
H14C H 0.3731 0.7779 0.2121 0.061 Uiso 1 1 calc R U . . .
C15 C 0.2677(2) 0.7350(3) 0.14270(14) 0.0419(12) Uani 1 1 d . . . . .
H15A H 0.2723 0.7373 0.1167 0.063 Uiso 1 1 calc R U . . .
H15B H 0.2306 0.7692 0.1504 0.063 Uiso 1 1 calc R U . . .
H15C H 0.2568 0.6826 0.1499 0.063 Uiso 1 1 calc R U . . .
C16 C 0.3803(2) 0.8504(2) 0.08467(10) 0.0187(9) Uani 1 1 d . . . . .
C17 C 0.3307(2) 0.9109(2) 0.09123(11) 0.0229(9) Uani 1 1 d . . . . .
C18 C 0.2663(2) 0.9116(3) 0.07308(11) 0.0278(10) Uani 1 1 d . . . . .
H18 H 0.2340 0.9505 0.0788 0.033 Uiso 1 1 calc R U . . .
C19 C 0.2482(2) 0.8574(3) 0.04699(11) 0.0253(10) Uani 1 1 d . . . . .
C20 C 0.2984(2) 0.8021(2) 0.03885(11) 0.0248(10) Uani 1 1 d . . . . .
H20 H 0.2886 0.7662 0.0206 0.030 Uiso 1 1 calc R U . . .
C21 C 0.3627(2) 0.7969(2) 0.05644(11) 0.0222(9) Uani 1 1 d . . . . .
C22 C 0.3424(2) 0.9783(3) 0.11766(12) 0.0280(10) Uani 1 1 d . . . . .
H22 H 0.3903 0.9740 0.1274 0.034 Uiso 1 1 calc R U . . .
C23 C 0.2908(3) 0.9759(3) 0.14972(12) 0.0403(13) Uani 1 1 d . . . . .
H23A H 0.2434 0.9758 0.1407 0.060 Uiso 1 1 calc R U . . .
H23B H 0.2979 1.0209 0.1648 0.060 Uiso 1 1 calc R U . . .
H23C H 0.2988 0.9295 0.1637 0.060 Uiso 1 1 calc R U . . .
C24 C 0.3362(3) 1.0567(3) 0.09747(14) 0.0382(12) Uani 1 1 d . . . . .
H24A H 0.3651 1.0556 0.0761 0.057 Uiso 1 1 calc R U . . .
H24B H 0.3515 1.0981 0.1132 0.057 Uiso 1 1 calc R U . . .
H24C H 0.2880 1.0653 0.0906 0.057 Uiso 1 1 calc R U . . .
C25 C 0.1772(2) 0.8552(3) 0.02848(13) 0.0370(12) Uani 1 1 d . . . . .
H25 H 0.1852 0.8377 0.0034 0.044 Uiso 1 1 calc R U . . .
C26 C 0.1404(3) 0.9335(3) 0.02626(14) 0.0515(15) Uani 1 1 d . . . . .
H26A H 0.1267 0.9498 0.0502 0.077 Uiso 1 1 calc R U . . .
H26B H 0.0993 0.9288 0.0112 0.077 Uiso 1 1 calc R U . . .
H26C H 0.1718 0.9714 0.0160 0.077 Uiso 1 1 calc R U . . .
C27 C 0.1305(3) 0.7944(4) 0.04669(18) 0.0660(18) Uani 1 1 d . . . . .
H27A H 0.1533 0.7445 0.0459 0.099 Uiso 1 1 calc R U . . .
H27B H 0.0863 0.7915 0.0341 0.099 Uiso 1 1 calc R U . . .
H27C H 0.1225 0.8090 0.0716 0.099 Uiso 1 1 calc R U . . .
C28 C 0.4126(2) 0.7338(2) 0.04283(11) 0.0232(9) Uani 1 1 d . . . . .
H28 H 0.4573 0.7402 0.0558 0.028 Uiso 1 1 calc R U . . .
C29 C 0.3853(3) 0.6521(3) 0.05108(13) 0.0372(12) Uani 1 1 d . . . . .
H29A H 0.3778 0.6468 0.0768 0.056 Uiso 1 1 calc R U . . .
H29B H 0.4193 0.6142 0.0432 0.056 Uiso 1 1 calc R U . . .
H29C H 0.3417 0.6438 0.0384 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4277(2) 0.7425(3) 0.00199(12) 0.0345(11) Uani 1 1 d . . . . .
H30A H 0.3849 0.7353 -0.0115 0.052 Uiso 1 1 calc R U . . .
H30B H 0.4615 0.7039 -0.0053 0.052 Uiso 1 1 calc R U . . .
H30C H 0.4462 0.7936 -0.0027 0.052 Uiso 1 1 calc R U . . .
C31 C 0.6430(3) 1.0366(3) 0.01981(13) 0.0443(13) Uani 1 1 d . . . . .
H31A H 0.6581 1.0830 0.0322 0.066 Uiso 1 1 calc R U . . .
H31B H 0.6118 1.0505 0.0003 0.066 Uiso 1 1 calc R U . . .
H31C H 0.6833 1.0099 0.0101 0.066 Uiso 1 1 calc R U . . .
C32 C 0.5668(3) 0.8847(3) 0.02608(12) 0.0431(13) Uani 1 1 d . . . . .
H32A H 0.6062 0.8508 0.0219 0.065 Uiso 1 1 calc R U . . .
H32B H 0.5478 0.9014 0.0032 0.065 Uiso 1 1 calc R U . . .
H32C H 0.5312 0.8572 0.0395 0.065 Uiso 1 1 calc R U . . .
C33 C 0.5136(2) 1.0235(3) 0.06621(13) 0.0387(12) Uani 1 1 d . . . . .
H33A H 0.4752 0.9871 0.0671 0.058 Uiso 1 1 calc R U . . .
H33B H 0.5033 1.0635 0.0487 0.058 Uiso 1 1 calc R U . . .
H33C H 0.5200 1.0466 0.0898 0.058 Uiso 1 1 calc R U . . .
C34 C 0.7749(2) 0.8729(3) 0.12323(13) 0.0362(12) Uani 1 1 d . . . . .
H34A H 0.7388 0.8525 0.1389 0.054 Uiso 1 1 calc R U . . .
H34B H 0.8033 0.9093 0.1365 0.054 Uiso 1 1 calc R U . . .
H34C H 0.8039 0.8309 0.1146 0.054 Uiso 1 1 calc R U . . .
C35 C 0.7896(3) 1.0107(3) 0.07418(14) 0.0439(13) Uani 1 1 d . . . . .
H35A H 0.7748 1.0345 0.0518 0.066 Uiso 1 1 calc R U . . .
H35B H 0.8379 0.9948 0.0722 0.066 Uiso 1 1 calc R U . . .
H35C H 0.7849 1.0475 0.0937 0.066 Uiso 1 1 calc R U . . .
C36 C 0.7449(3) 0.8560(3) 0.04367(13) 0.0461(13) Uani 1 1 d . . . . .
H36A H 0.7190 0.8088 0.0478 0.069 Uiso 1 1 calc R U . . .
H36B H 0.7940 0.8440 0.0407 0.069 Uiso 1 1 calc R U . . .
H36C H 0.7277 0.8810 0.0221 0.069 Uiso 1 1 calc R U . . .
C37 C 0.7338(3) 1.0500(3) 0.17126(12) 0.0388(12) Uani 1 1 d . . . . .
H37A H 0.7280 1.0262 0.1478 0.058 Uiso 1 1 calc R U . . .
H37B H 0.7814 1.0681 0.1738 0.058 Uiso 1 1 calc R U . . .
H37C H 0.7021 1.0933 0.1735 0.058 Uiso 1 1 calc R U . . .
C38 C 0.6987(3) 1.0372(3) 0.24913(14) 0.0498(14) Uani 1 1 d . . . . .
H38A H 0.6678 1.0797 0.2432 0.075 Uiso 1 1 calc R U . . .
H38B H 0.7428 1.0574 0.2578 0.075 Uiso 1 1 calc R U . . .
H38C H 0.6775 1.0056 0.2677 0.075 Uiso 1 1 calc R U . . .
C39 C 0.7970(2) 0.9225(3) 0.21867(14) 0.0423(13) Uani 1 1 d . . . . .
H39A H 0.7914 0.8956 0.2414 0.063 Uiso 1 1 calc R U . . .
H39B H 0.8355 0.9586 0.2205 0.063 Uiso 1 1 calc R U . . .
H39C H 0.8066 0.8854 0.1997 0.063 Uiso 1 1 calc R U . . .
C40 C 0.6214(3) 0.8553(3) 0.26809(12) 0.0439(13) Uani 1 1 d . . . . .
H40A H 0.6653 0.8760 0.2768 0.066 Uiso 1 1 calc R U . . .
H40B H 0.6103 0.8085 0.2812 0.066 Uiso 1 1 calc R U . . .
H40C H 0.5847 0.8930 0.2718 0.066 Uiso 1 1 calc R U . . .
C41 C 0.6993(3) 0.7568(3) 0.21378(13) 0.0400(12) Uani 1 1 d . . . . .
H41A H 0.7104 0.7499 0.1885 0.060 Uiso 1 1 calc R U . . .
H41B H 0.6828 0.7084 0.2238 0.060 Uiso 1 1 calc R U . . .
H41C H 0.7407 0.7733 0.2266 0.060 Uiso 1 1 calc R U . . .
C42 C 0.5444(3) 0.7859(3) 0.20473(13) 0.0373(12) Uani 1 1 d . . . . .
H42A H 0.5070 0.8048 0.2199 0.056 Uiso 1 1 calc R U . . .
H42B H 0.5483 0.7304 0.2074 0.056 Uiso 1 1 calc R U . . .
H42C H 0.5344 0.7985 0.1798 0.056 Uiso 1 1 calc R U . . .
C43 C 0.4558(3) 0.9672(3) 0.20577(12) 0.0383(12) Uani 1 1 d . . . . .
H43A H 0.4390 0.9458 0.1832 0.057 Uiso 1 1 calc R U . . .
H43B H 0.4188 0.9659 0.2235 0.057 Uiso 1 1 calc R U . . .
H43C H 0.4950 0.9369 0.2143 0.057 Uiso 1 1 calc R U . . .
C44 C 0.5224(3) 1.1002(4) 0.24323(14) 0.0606(17) Uani 1 1 d . . . . .
H44A H 0.5526 1.0595 0.2521 0.091 Uiso 1 1 calc R U . . .
H44B H 0.4850 1.1090 0.2603 0.091 Uiso 1 1 calc R U . . .
H44C H 0.5492 1.1473 0.2403 0.091 Uiso 1 1 calc R U . . .
C45 C 0.4046(3) 1.1332(3) 0.19258(16) 0.0535(15) Uani 1 1 d . . . . .
H45A H 0.4180 1.1872 0.1932 0.080 Uiso 1 1 calc R U . . .
H45B H 0.3719 1.1227 0.2119 0.080 Uiso 1 1 calc R U . . .
H45C H 0.3828 1.1217 0.1696 0.080 Uiso 1 1 calc R U . . .
C46 C 0.5905(3) 1.2354(3) 0.17924(16) 0.0578(16) Uani 1 1 d . . . . .
H46A H 0.5514 1.2456 0.1951 0.087 Uiso 1 1 calc R U . . .
H46B H 0.6056 1.2833 0.1682 0.087 Uiso 1 1 calc R U . . .
H46C H 0.6285 1.2134 0.1930 0.087 Uiso 1 1 calc R U . . .
C47 C 0.6372(3) 1.1596(3) 0.10943(14) 0.0465(14) Uani 1 1 d . . . . .
H47A H 0.6808 1.1712 0.1214 0.070 Uiso 1 1 calc R U . . .
H47B H 0.6294 1.1967 0.0903 0.070 Uiso 1 1 calc R U . . .
H47C H 0.6392 1.1080 0.0994 0.070 Uiso 1 1 calc R U . . .
C48 C 0.4879(3) 1.2129(3) 0.11878(19) 0.0683(19) Uani 1 1 d . . . . .
H48A H 0.4659 1.1755 0.1030 0.102 Uiso 1 1 calc R U . . .
H48B H 0.5052 1.2559 0.1046 0.102 Uiso 1 1 calc R U . . .
H48C H 0.4542 1.2315 0.1362 0.102 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 O1 2.167(3) . ?
U1 N1 2.259(3) . ?
U1 N3 2.271(3) . ?
U1 N2 2.286(3) . ?
U1 Si1 3.3644(12) . ?
U1 Si5 3.3770(13) . ?
Si1 N1 1.760(3) . ?
Si1 C32 1.860(5) . ?
Si1 C31 1.870(5) . ?
Si1 C33 1.873(5) . ?
Si2 N1 1.754(4) . ?
Si2 C34 1.868(5) . ?
Si2 C35 1.874(5) . ?
Si2 C36 1.881(5) . ?
Si3 N2 1.754(4) . ?
Si3 C38 1.865(5) . ?
Si3 C39 1.871(5) . ?
Si3 C37 1.873(5) . ?
Si4 N2 1.747(3) . ?
Si4 C40 1.867(5) . ?
Si4 C42 1.869(5) . ?
Si4 C41 1.872(5) . ?
Si5 N3 1.747(4) . ?
Si5 C44 1.867(5) . ?
Si5 C45 1.870(5) . ?
Si5 C43 1.879(5) . ?
Si6 N3 1.756(4) . ?
Si6 C46 1.862(5) . ?
Si6 C48 1.869(6) . ?
Si6 C47 1.879(5) . ?
O1 B1 1.365(5) . ?
B1 C1 1.608(6) . ?
B1 C16 1.621(6) . ?
C1 C2 1.405(5) . ?
C1 C6 1.414(6) . ?
C2 C3 1.394(6) . ?
C2 C7 1.530(5) . ?
C3 C4 1.384(6) . ?
C4 C5 1.394(6) . ?
C4 C10 1.512(6) . ?
C5 C6 1.391(6) . ?
C6 C13 1.520(6) . ?
C7 C8 1.519(6) . ?
C7 C9 1.533(6) . ?
C10 C11 1.514(7) . ?
C10 C12 1.524(7) . ?
C13 C15 1.518(6) . ?
C13 C14 1.521(6) . ?
C16 C17 1.422(6) . ?
C16 C21 1.425(5) . ?
C17 C18 1.393(6) . ?
C17 C22 1.526(6) . ?
C18 C19 1.379(6) . ?
C19 C20 1.377(6) . ?
C19 C25 1.510(6) . ?
C20 C21 1.384(6) . ?
C21 C28 1.522(6) . ?
C22 C23 1.533(6) . ?
C22 C24 1.541(6) . ?
C25 C26 1.516(7) . ?
C25 C27 1.524(7) . ?
C28 C29 1.525(6) . ?
C28 C30 1.535(6) . ?

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
O1 U1 N1 96.44(11) . . ?
O1 U1 N3 109.77(11) . . ?
N1 U1 N3 117.61(13) . . ?
O1 U1 N2 121.34(11) . . ?
N1 U1 N2 111.63(12) . . ?
N3 U1 N2 101.17(12) . . ?
O1 U1 Si1 77.71(7) . . ?
N1 U1 Si1 28.78(9) . . ?
N3 U1 Si1 103.81(9) . . ?
N2 U1 Si1 140.35(8) . . ?
O1 U1 Si5 95.89(7) . . ?
N1 U1 Si5 145.53(9) . . ?
N3 U1 Si5 28.26(10) . . ?
N2 U1 Si5 88.68(8) . . ?
Si1 U1 Si5 126.15(3) . . ?
N1 Si1 C32 113.8(2) . . ?
N1 Si1 C31 114.4(2) . . ?
C32 Si1 C31 106.5(2) . . ?
N1 Si1 C33 109.33(19) . . ?
C32 Si1 C33 105.7(2) . . ?
C31 Si1 C33 106.5(2) . . ?
N1 Si1 U1 38.14(11) . . ?
C32 Si1 U1 115.13(16) . . ?
C31 Si1 U1 137.01(17) . . ?
C33 Si1 U1 72.72(15) . . ?
N1 Si2 C34 112.52(19) . . ?
N1 Si2 C35 112.7(2) . . ?
C34 Si2 C35 105.8(2) . . ?
N1 Si2 C36 113.1(2) . . ?
C34 Si2 C36 105.9(2) . . ?
C35 Si2 C36 106.1(2) . . ?
N2 Si3 C38 117.2(2) . . ?
N2 Si3 C39 113.9(2) . . ?
C38 Si3 C39 103.5(2) . . ?
N2 Si3 C37 108.75(19) . . ?
C38 Si3 C37 104.1(2) . . ?
C39 Si3 C37 108.7(2) . . ?
N2 Si4 C40 111.5(2) . . ?
N2 Si4 C42 110.96(19) . . ?
C40 Si4 C42 106.6(2) . . ?
N2 Si4 C41 113.7(2) . . ?
C40 Si4 C41 106.9(2) . . ?
C42 Si4 C41 106.8(2) . . ?
N3 Si5 C44 116.1(2) . . ?
N3 Si5 C45 113.8(2) . . ?
C44 Si5 C45 105.0(3) . . ?
N3 Si5 C43 108.72(19) . . ?
C44 Si5 C43 103.9(3) . . ?
C45 Si5 C43 108.7(2) . . ?
N3 Si5 U1 37.98(12) . . ?
C44 Si5 U1 118.67(19) . . ?
C45 Si5 U1 135.13(18) . . ?
C43 Si5 U1 71.60(14) . . ?
N3 Si6 C46 111.6(2) . . ?
N3 Si6 C48 113.6(2) . . ?
C46 Si6 C48 106.0(3) . . ?
N3 Si6 C47 111.9(2) . . ?
C46 Si6 C47 107.1(3) . . ?
C48 Si6 C47 106.2(3) . . ?
B1 O1 U1 169.8(3) . . ?
Si2 N1 Si1 114.79(18) . . ?
Si2 N1 U1 132.13(18) . . ?
Si1 N1 U1 113.08(17) . . ?
Si4 N2 Si3 116.60(19) . . ?
Si4 N2 U1 124.66(18) . . ?
Si3 N2 U1 118.73(17) . . ?
Si5 N3 Si6 117.6(2) . . ?
Si5 N3 U1 113.76(18) . . ?
Si6 N3 U1 128.6(2) . . ?
O1 B1 C1 118.4(4) . . ?
O1 B1 C16 124.8(4) . . ?
C1 B1 C16 116.7(3) . . ?
C2 C1 C6 117.6(4) . . ?
C2 C1 B1 122.8(3) . . ?
C6 C1 B1 119.6(3) . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 C7 117.2(4) . . ?
C1 C2 C7 122.4(4) . . ?
C4 C3 C2 122.4(4) . . ?
C3 C4 C5 117.1(4) . . ?
C3 C4 C10 122.0(4) . . ?
C5 C4 C10 120.9(4) . . ?
C6 C5 C4 122.3(4) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 C13 118.3(4) . . ?
C1 C6 C13 121.5(4) . . ?
C8 C7 C2 113.4(4) . . ?
C8 C7 C9 109.7(4) . . ?
C2 C7 C9 110.2(3) . . ?
C4 C10 C11 113.7(4) . . ?
C4 C10 C12 110.7(4) . . ?
C11 C10 C12 110.1(4) . . ?
C15 C13 C6 112.6(4) . . ?
C15 C13 C14 110.7(4) . . ?
C6 C13 C14 112.3(4) . . ?
C17 C16 C21 116.0(4) . . ?
C17 C16 B1 123.5(3) . . ?
C21 C16 B1 119.6(3) . . ?
C18 C17 C16 120.4(4) . . ?
C18 C17 C22 115.3(4) . . ?
C16 C17 C22 124.3(4) . . ?
C19 C18 C17 123.1(4) . . ?
C20 C19 C18 116.3(4) . . ?
C20 C19 C25 120.2(4) . . ?
C18 C19 C25 123.5(4) . . ?
C19 C20 C21 123.6(4) . . ?
C20 C21 C16 120.4(4) . . ?
C20 C21 C28 116.2(4) . . ?
C16 C21 C28 123.4(4) . . ?
C17 C22 C23 112.1(4) . . ?
C17 C22 C24 110.1(4) . . ?
C23 C22 C24 110.2(4) . . ?
C19 C25 C26 114.5(4) . . ?
C19 C25 C27 109.8(4) . . ?
C26 C25 C27 111.1(4) . . ?
C21 C28 C29 112.1(4) . . ?
C21 C28 C30 111.7(4) . . ?
C29 C28 C30 110.3(4) . . ?

_refine_diff_density_max         0.753
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.088

_shelxl_version_number           2014-3

