# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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. 
# 
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data_UO2GeLAthf
_database_code_depnum_ccdc_archive 'CCDC 1480061'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H64 Ge N8 O4 U, C4 H8 O'
_chemical_formula_sum            'C70 H72 Ge N8 O5 U'
_chemical_formula_weight         1415.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C66 H64 N8 O4 Ge 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'
Ge Ge 0.1547 1.8001 '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'
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                   11.44279(12)
_cell_length_b                   22.2890(2)
_cell_length_c                   24.0677(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.0274(10)
_cell_angle_gamma                90
_cell_volume                     6078.29(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35068
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.0840
_cell_measurement_theta_min      3.4100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.838
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 0 12 0.0754
-14 0 -12 0.0754
1 -30 -8 0.1197
-1 30 8 0.1197
-3 3 34 0.0524
3 -3 -34 0.0524

_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.105
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
13.9881 0.0297 11.9793 -0.4780 0.8674 0.0089
-13.9881 -0.0297 -11.9793 0.4780 -0.8674 -0.0089
0.9981 -30.0090 -7.9999 0.0310 -0.0386 -0.9828
-0.9981 30.0090 7.9999 -0.0310 0.0386 0.9828
-2.9921 2.9955 33.9649 0.6382 0.7067 0.3264
2.9921 -2.9955 -33.9649 -0.6382 -0.7067 -0.3264

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            139112
_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         27.485
_diffrn_reflns_theta_min         2.801
_diffrn_ambient_temperature      170(2)
_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   27.50    --  -18.53 -99.00 -60.00   47
  2  ω    -37.00  50.00   1.00   27.50    --  -18.53  57.00-150.00   87
  3  ω      2.00  89.00   1.00   27.50    --   20.25  57.00  90.00   87
  4  ω    -48.00  39.00   1.00   27.50    --   20.25 -57.00 -90.00   87
  5  ω     -2.00  91.00   1.00   27.50    --   20.25  38.00  60.00   93
  6  ω    -25.00  61.00   1.00   27.50    --   20.25 -99.00 150.00   86
  7  ω      2.00  89.00   1.00   27.50    --   20.25  57.00-120.00   87
  8  ω     34.00  94.00   1.00   27.50    --   20.25 179.00-180.00   60
  9  ω    -69.00 -38.00   1.00   27.50    --  -18.53 117.00 146.56   31
 10  ω      2.00  89.00   1.00   27.50    --   20.25  57.00-180.00   87
 11  ω    -25.00  61.00   1.00   27.50    --   20.25 -99.00 -30.00   86
 12  ω    -25.00  61.00   1.00   27.50    --   20.25 -99.00  30.00   86
 13  ω      2.00  89.00   1.00   27.50    --   20.25  57.00 -60.00   87
 14  ω     34.00  94.00   1.00   27.50    --   20.25 179.00 120.00   60
;
_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      -0.0471954000
_diffrn_orient_matrix_UB_12      -0.0066594000
_diffrn_orient_matrix_UB_13      0.0152212000
_diffrn_orient_matrix_UB_21      0.0408237000
_diffrn_orient_matrix_UB_22      -0.0039527000
_diffrn_orient_matrix_UB_23      0.0247505000
_diffrn_orient_matrix_UB_31      -0.0049555000
_diffrn_orient_matrix_UB_32      0.0308652000
_diffrn_orient_matrix_UB_33      0.0064521000
_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                11376
_reflns_number_total             13933
_reflns_odcompleteness_completeness 99.83
_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 1.171.38.42b (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         1.324
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13933
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.077
_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)+(0.0260P)²+8.0902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0700
_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. Uiso/Uaniso restraints and constraints
O5 \\sim C80 \\sim C82 \\sim C81 \\sim C83: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 O5, C80, C82, C81, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=1-FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C33(H33A,H33B), C63(H63A,H63B), C62(H62A,H62B), C80(H80A,
 H80B), C4(H4A,H4B), C73(H73A,H73B), C71(H71A,H71B), C82(H82A,H82B), C2A(H2AA,
 H2AB), C81(H81A,H81B), C31(H31A,H31B), C60(H60A,H60B), C72(H72A,H72B),
 C83(H83A,H83B), C61(H61A,H61B), C2B(H2BA,H2BB)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C46(H46), C25(H25), C43(H43), C39(H39), C23(H23), C42(H42),
 C22(H22), C52(H52), C27(H27), C28(H28), C56(H56), C20(H20), C14(H14), C54(H54),
  C10(H10), C13(H13), C36(H36), C12(H12), C49(H49), C51(H51), C41(H41),
 C50(H50), C7(H7), C8(H8), C21(H21), C57(H57), C37(H37)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C5(H5A,H5B,H5C), C3A(H3AA,H3AB,
 H3AC), C3B(H3BA,H3BB,H3BC)
;
_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 0.36131(2) 0.37858(2) 0.05778(2) 0.02352(4) Uani 1 1 d . . . . .
Ge1 Ge 0.25112(3) 0.15782(2) 0.03998(2) 0.02711(8) Uani 1 1 d . . . . .
O1 O 0.3449(2) 0.30024(10) 0.05854(10) 0.0317(5) Uani 1 1 d . . . . .
O2 O 0.3796(2) 0.45661(10) 0.05102(9) 0.0329(5) Uani 1 1 d . . . . .
O3 O 0.3752(2) 0.37539(11) -0.04363(9) 0.0347(5) Uani 1 1 d . . . . .
O4 O 0.2469(2) 0.07654(11) -0.00753(9) 0.0327(5) Uani 1 1 d . . . . .
N3 N 0.1476(2) 0.38768(12) 0.01502(11) 0.0280(6) Uani 1 1 d . . . . .
N1 N 0.4735(3) 0.38585(12) 0.15207(12) 0.0343(7) Uani 1 1 d . . . . .
N4 N 0.2256(3) 0.38586(12) 0.12797(11) 0.0309(6) Uani 1 1 d . . . . .
N2 N 0.5815(2) 0.36018(12) 0.05575(12) 0.0307(6) Uani 1 1 d . . . . .
N6 N 0.4929(2) 0.13698(12) 0.02047(11) 0.0261(6) Uani 1 1 d . . . . .
C18 C 0.6070(3) 0.19587(15) -0.03866(13) 0.0253(7) Uani 1 1 d . . . . .
N8 N 0.1020(2) 0.13749(12) 0.07050(12) 0.0291(6) Uani 1 1 d . . . . .
N5 N 0.3363(2) 0.10946(11) 0.10265(10) 0.0244(6) Uani 1 1 d . . . . .
C19 C 0.6664(3) 0.19789(15) -0.08774(14) 0.0292(7) Uani 1 1 d . . . . .
C53 C 0.1027(3) 0.40538(16) -0.04089(14) 0.0282(7) Uani 1 1 d . . . . .
C48 C 0.0274(3) 0.38296(16) -0.13946(13) 0.0285(7) Uani 1 1 d . . . . .
C17 C 0.5996(3) 0.24849(14) -0.00711(14) 0.0253(7) Uani 1 1 d . . . . .
H17 H 0.5615 0.2473 0.0246 0.030 Uiso 1 1 calc R . . . .
C47 C 0.0651(3) 0.36179(15) -0.08328(13) 0.0254(7) Uani 1 1 d . . . . .
C16 C 0.6486(3) 0.30261(15) -0.02242(14) 0.0273(7) Uani 1 1 d . . . . .
C46 C 0.0606(3) 0.30031(15) -0.07200(14) 0.0272(7) Uani 1 1 d . . . . .
H46 H 0.0838 0.2867 -0.0356 0.033 Uiso 1 1 calc R . . . .
C25 C 0.5187(3) 0.09785(15) 0.05877(14) 0.0285(7) Uani 1 1 d . . . . .
H25 H 0.5876 0.0758 0.0586 0.034 Uiso 1 1 calc R . . . .
C70 C 0.2544(3) 0.08130(18) -0.06764(14) 0.0364(8) Uani 1 1 d . . . . .
H70A H 0.3358 0.0788 -0.0744 0.044 Uiso 1 1 calc R . . . .
H70B H 0.2214 0.1191 -0.0825 0.044 Uiso 1 1 calc R . . . .
N7 N 0.0483(3) 0.17559(13) -0.04737(12) 0.0336(7) Uani 1 1 d . . . . .
C24 C 0.5613(3) 0.13912(15) -0.02321(13) 0.0253(7) Uani 1 1 d . . . . .
C38 C -0.0080(3) 0.15289(17) 0.04214(16) 0.0379(9) Uani 1 1 d . . . . .
C43 C -0.0556(3) 0.23756(17) -0.21272(15) 0.0361(8) Uani 1 1 d . . . . .
H43 H -0.0781 0.2506 -0.2494 0.043 Uiso 1 1 calc R . . . .
C39 C -0.0293(3) 0.17115(17) -0.01506(16) 0.0381(9) Uani 1 1 d . . . . .
H39 H -0.1066 0.1806 -0.0298 0.046 Uiso 1 1 calc R . . . .
C55 C 0.1112(3) 0.36835(16) 0.10716(15) 0.0355(8) Uani 1 1 d . . . . .
C33 C 0.1481(4) 0.06756(16) 0.21374(15) 0.0390(9) Uani 1 1 d . . . . .
H33A H 0.2107 0.0640 0.2452 0.047 Uiso 1 1 calc R . . . .
H33B H 0.0794 0.0836 0.2281 0.047 Uiso 1 1 calc R . . . .
C23 C 0.5792(3) 0.08914(15) -0.05364(14) 0.0294(7) Uani 1 1 d . . . . .
H23 H 0.5513 0.0524 -0.0427 0.035 Uiso 1 1 calc R . . . .
C11 C 0.6434(3) 0.35749(15) 0.00841(16) 0.0313(8) Uani 1 1 d . . . . .
C30 C 0.1874(3) 0.11308(15) 0.17131(13) 0.0305(8) Uani 1 1 d . . . . .
C44 C -0.0139(3) 0.27984(16) -0.17027(13) 0.0288(7) Uani 1 1 d . . . . .
C42 C -0.0628(3) 0.17894(18) -0.20039(16) 0.0405(9) Uani 1 1 d . . . . .
H42 H -0.0914 0.1520 -0.2286 0.049 Uiso 1 1 calc R . . . .
C22 C 0.6390(3) 0.09141(16) -0.10137(15) 0.0341(8) Uani 1 1 d . . . . .
H22 H 0.6505 0.0565 -0.1210 0.041 Uiso 1 1 calc R . . . .
C52 C 0.1002(3) 0.46498(17) -0.05342(16) 0.0374(8) Uani 1 1 d . . . . .
H52 H 0.1239 0.4928 -0.0253 0.045 Uiso 1 1 calc R . . . .
C15 C 0.7077(3) 0.30386(15) -0.07122(15) 0.0310(8) Uani 1 1 d . . . . .
C40 C 0.0129(3) 0.19618(16) -0.10243(15) 0.0308(7) Uani 1 1 d . . . . .
C45 C 0.0223(3) 0.25908(15) -0.11412(14) 0.0275(7) Uani 1 1 d . . . . .
C63 C 0.3600(3) 0.3234(2) -0.08062(16) 0.0473(11) Uani 1 1 d . . . . .
H63A H 0.2862 0.3031 -0.0774 0.057 Uiso 1 1 calc R . . . .
H63B H 0.4244 0.2953 -0.0715 0.057 Uiso 1 1 calc R . . . .
C6 C 0.4553(4) 0.40091(16) 0.20453(15) 0.0420(10) Uani 1 1 d . . . . .
C27 C 0.4798(3) 0.05314(15) 0.15041(15) 0.0345(8) Uani 1 1 d . . . . .
H27 H 0.5500 0.0322 0.1601 0.041 Uiso 1 1 calc R . . . .
C35 C 0.0871(3) 0.12438(15) 0.12460(14) 0.0320(7) Uani 1 1 d . . . . .
C28 C 0.3870(3) 0.05732(15) 0.18203(14) 0.0339(8) Uani 1 1 d . . . . .
H28 H 0.3844 0.0401 0.2170 0.041 Uiso 1 1 calc R . . . .
C56 C 0.0480(4) 0.35694(18) 0.15187(17) 0.0456(10) Uani 1 1 d . . . . .
H56 H -0.0299 0.3442 0.1495 0.055 Uiso 1 1 calc R . . . .
C20 C 0.7139(3) 0.25210(16) -0.10256(15) 0.0328(8) Uani 1 1 d . . . . .
H20 H 0.7511 0.2536 -0.1345 0.039 Uiso 1 1 calc R . . . .
O5 O 0.7402(4) 0.17141(19) 0.20177(19) 0.0909(12) Uani 1 1 d . U . . .
C14 C 0.7613(3) 0.35853(17) -0.08605(18) 0.0411(9) Uani 1 1 d . . . . .
H14 H 0.8004 0.3596 -0.1174 0.049 Uiso 1 1 calc R . . . .
C54 C 0.0736(3) 0.37345(15) 0.04959(15) 0.0330(8) Uani 1 1 d . . . . .
H54 H -0.0053 0.3666 0.0357 0.040 Uiso 1 1 calc R . . . .
C10 C 0.6442(3) 0.37454(16) 0.10343(17) 0.0407(9) Uani 1 1 d . . . . .
H10 H 0.7258 0.3766 0.1051 0.049 Uiso 1 1 calc R . . . .
C62 C 0.3594(7) 0.3478(4) -0.1379(2) 0.101(2) Uani 1 1 d . . . . .
H62A H 0.4002 0.3208 -0.1602 0.121 Uiso 1 1 calc R . . . .
H62B H 0.2789 0.3527 -0.1563 0.121 Uiso 1 1 calc R . . . .
C26 C 0.4481(3) 0.08577(14) 0.10205(13) 0.0272(7) Uani 1 1 d . . . . .
C80 C 0.5761(6) 0.2097(3) 0.2343(3) 0.105(2) Uani 1 1 d . U . . .
H80A H 0.5011 0.1920 0.2397 0.125 Uiso 1 1 calc R . . . .
H80B H 0.5915 0.2438 0.2592 0.125 Uiso 1 1 calc R . . . .
C13 C 0.7556(3) 0.40848(17) -0.0548(2) 0.0467(11) Uani 1 1 d . . . . .
H13 H 0.7921 0.4435 -0.0645 0.056 Uiso 1 1 calc R . . . .
C4 C 0.3373(5) 0.3922(2) 0.28412(16) 0.0648(15) Uani 1 1 d . . . . .
H4A H 0.3968 0.4153 0.3076 0.078 Uiso 1 1 calc R . . . .
H4B H 0.2615 0.4021 0.2953 0.078 Uiso 1 1 calc R . . . .
C73 C 0.1797(4) 0.02397(16) 0.00250(16) 0.0402(9) Uani 1 1 d . . . . .
H73A H 0.1326 0.0310 0.0324 0.048 Uiso 1 1 calc R . . . .
H73B H 0.2312 -0.0101 0.0125 0.048 Uiso 1 1 calc R . . . .
C58 C 0.2332(4) 0.38578(15) 0.18471(15) 0.0380(9) Uani 1 1 d . . . . .
C36 C -0.0310(4) 0.13033(19) 0.13025(17) 0.0472(10) Uani 1 1 d . . . . .
H36 H -0.0644 0.1235 0.1627 0.057 Uiso 1 1 calc R . . . .
C12 C 0.6957(3) 0.40839(17) -0.00828(18) 0.0420(9) Uani 1 1 d . . . . .
H12 H 0.6912 0.4437 0.0119 0.050 Uiso 1 1 calc R . . . .
C29 C 0.2993(3) 0.09164(14) 0.15194(13) 0.0272(7) Uani 1 1 d . . . . .
C1 C 0.3365(4) 0.41236(17) 0.22243(15) 0.0454(10) Uani 1 1 d . . . . .
C49 C -0.0102(3) 0.34116(16) -0.18115(14) 0.0303(8) Uani 1 1 d . . . . .
H49 H -0.0336 0.3547 -0.2176 0.036 Uiso 1 1 calc R . . . .
C71 C 0.1840(4) 0.02935(19) -0.09458(16) 0.0459(10) Uani 1 1 d . . . . .
H71A H 0.2350 -0.0041 -0.1008 0.055 Uiso 1 1 calc R . . . .
H71B H 0.1390 0.0410 -0.1301 0.055 Uiso 1 1 calc R . . . .
C51 C 0.0623(4) 0.48520(17) -0.10861(17) 0.0422(9) Uani 1 1 d . . . . .
H51 H 0.0604 0.5261 -0.1164 0.051 Uiso 1 1 calc R . . . .
C82 C 0.5754(6) 0.2276(3) 0.1762(3) 0.110(2) Uani 1 1 d . U . . .
H82A H 0.5150 0.2060 0.1518 0.132 Uiso 1 1 calc R . . . .
H82B H 0.5607 0.2703 0.1717 0.132 Uiso 1 1 calc R . . . .
C9 C 0.5954(4) 0.38684(18) 0.15177(17) 0.0438(10) Uani 1 1 d . . . . .
C32 C 0.2435(4) 0.22566(16) 0.16648(17) 0.0501(11) Uani 1 1 d . . . . .
H32A H 0.1776 0.2331 0.1380 0.075 Uiso 1 1 calc GR . . . .
H32B H 0.3116 0.2156 0.1492 0.075 Uiso 1 1 calc GR . . . .
H32C H 0.2597 0.2610 0.1891 0.075 Uiso 1 1 calc GR . . . .
C34 C 0.1182(4) 0.00534(17) 0.19043(17) 0.0449(10) Uani 1 1 d . . . . .
H34A H 0.0580 0.0083 0.1585 0.067 Uiso 1 1 calc GR . . . .
H34B H 0.0901 -0.0189 0.2187 0.067 Uiso 1 1 calc GR . . . .
H34C H 0.1875 -0.0127 0.1793 0.067 Uiso 1 1 calc GR . . . .
C2A C 0.2959(12) 0.4778(6) 0.2275(5) 0.038(3) Uani 0.470(10) 1 d . . P A 1
H2AA H 0.2165 0.4780 0.2373 0.046 Uiso 0.470(10) 1 calc R . P A 1
H2AB H 0.3472 0.4973 0.2576 0.046 Uiso 0.470(10) 1 calc R . P A 1
C41 C -0.0275(3) 0.15762(17) -0.14519(16) 0.0384(9) Uani 1 1 d . . . . .
H41 H -0.0318 0.1168 -0.1378 0.046 Uiso 1 1 calc R . . . .
C50 C 0.0286(3) 0.44550(17) -0.15025(15) 0.0361(8) Uani 1 1 d . . . . .
H50 H 0.0058 0.4594 -0.1866 0.043 Uiso 1 1 calc R . . . .
C7 C 0.5650(5) 0.4113(2) 0.23804(18) 0.0638(14) Uani 1 1 d . . . . .
H7 H 0.5761 0.4221 0.2758 0.077 Uiso 1 1 calc R . . . .
C81 C 0.6716(5) 0.1655(3) 0.2446(3) 0.0791(15) Uani 1 1 d . U . . .
H81A H 0.7188 0.1729 0.2807 0.095 Uiso 1 1 calc R . . . .
H81B H 0.6393 0.1253 0.2447 0.095 Uiso 1 1 calc R . . . .
C8 C 0.6511(5) 0.4028(2) 0.20538(19) 0.0651(14) Uani 1 1 d . . . . .
H8 H 0.7319 0.4069 0.2165 0.078 Uiso 1 1 calc R . . . .
C31 C 0.2143(4) 0.17388(16) 0.20319(15) 0.0424(9) Uani 1 1 d . . . . .
H31A H 0.1463 0.1849 0.2209 0.051 Uiso 1 1 calc R . . . .
H31B H 0.2802 0.1679 0.2327 0.051 Uiso 1 1 calc R . . . .
C21 C 0.6792(3) 0.14438(17) -0.11828(15) 0.0341(8) Uani 1 1 d . . . . .
H21 H 0.7159 0.1458 -0.1504 0.041 Uiso 1 1 calc R . . . .
C60 C 0.3993(4) 0.4286(2) -0.07587(17) 0.0517(11) Uani 1 1 d . . . . .
H60A H 0.4696 0.4492 -0.0583 0.062 Uiso 1 1 calc R . . . .
H60B H 0.3332 0.4563 -0.0793 0.062 Uiso 1 1 calc R . . . .
C72 C 0.1030(4) 0.0134(2) -0.05182(17) 0.0507(11) Uani 1 1 d . . . . .
H72A H 0.0339 0.0391 -0.0557 0.061 Uiso 1 1 calc R . . . .
H72B H 0.0778 -0.0282 -0.0555 0.061 Uiso 1 1 calc R . . . .
C57 C 0.1247(4) 0.36849(18) 0.20019(17) 0.0487(11) Uani 1 1 d . . . . .
H57 H 0.1073 0.3653 0.2367 0.058 Uiso 1 1 calc R . . . .
C37 C -0.0903(4) 0.1483(2) 0.07902(19) 0.0548(12) Uani 1 1 d . . . . .
H37 H -0.1708 0.1559 0.0708 0.066 Uiso 1 1 calc R . . . .
C5 C 0.3610(6) 0.3262(2) 0.29602(19) 0.0799(18) Uani 1 1 d . . . . .
H5A H 0.4299 0.3141 0.2802 0.120 Uiso 1 1 calc GR . . . .
H5B H 0.2944 0.3030 0.2795 0.120 Uiso 1 1 calc GR . . . .
H5C H 0.3738 0.3197 0.3358 0.120 Uiso 1 1 calc GR . . . .
C83 C 0.6886(6) 0.2130(3) 0.1636(3) 0.100(2) Uani 1 1 d . U . . .
H83A H 0.6825 0.1966 0.1260 0.120 Uiso 1 1 calc R . . . .
H83B H 0.7371 0.2488 0.1652 0.120 Uiso 1 1 calc R . . . .
C61 C 0.4171(7) 0.4037(4) -0.1324(2) 0.110(3) Uani 1 1 d . . . . .
H61A H 0.3839 0.4307 -0.1621 0.132 Uiso 1 1 calc R . . . .
H61B H 0.5006 0.3988 -0.1346 0.132 Uiso 1 1 calc R . . . .
C3A C 0.2971(8) 0.5131(3) 0.1740(3) 0.042(3) Uani 0.470(10) 1 d . . P A 1
H3AA H 0.3715 0.5074 0.1606 0.062 Uiso 0.470(10) 1 calc GR . P A 1
H3AB H 0.2862 0.5549 0.1813 0.062 Uiso 0.470(10) 1 calc GR . P A 1
H3AC H 0.2345 0.4993 0.1462 0.062 Uiso 0.470(10) 1 calc GR . P A 1
C3B C 0.2297(8) 0.5123(4) 0.2340(5) 0.073(4) Uani 0.530(10) 1 d . . P A 2
H3BA H 0.1627 0.4878 0.2206 0.109 Uiso 0.530(10) 1 calc GR . P A 2
H3BB H 0.2175 0.5521 0.2191 0.109 Uiso 0.530(10) 1 calc GR . P A 2
H3BC H 0.2393 0.5139 0.2742 0.109 Uiso 0.530(10) 1 calc GR . P A 2
C2B C 0.3396(11) 0.4857(6) 0.2152(5) 0.042(3) Uani 0.530(10) 1 d . . P A 2
H2BA H 0.4094 0.5019 0.2376 0.050 Uiso 0.530(10) 1 calc R . P A 2
H2BB H 0.3426 0.4959 0.1762 0.050 Uiso 0.530(10) 1 calc R . P A 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 O1 1.757(2) . ?
U1 O2 1.762(2) . ?
U1 O3 2.469(2) . ?
U1 N3 2.526(3) . ?
U1 N1 2.452(3) . ?
U1 N4 2.454(3) . ?
U1 N2 2.560(3) . ?
Ge1 O4 2.139(2) . ?
Ge1 N8 2.001(3) . ?
Ge1 N5 1.994(3) . ?
O3 C63 1.456(4) . ?
O3 C60 1.464(5) . ?
O4 C70 1.465(4) . ?
O4 C73 1.440(4) . ?
N3 C53 1.427(4) . ?
N3 C54 1.306(4) . ?
N1 C6 1.351(4) . ?
N1 C9 1.395(5) . ?
N4 C55 1.391(5) . ?
N4 C58 1.356(4) . ?
N2 C11 1.424(5) . ?
N2 C10 1.305(5) . ?
N6 C25 1.273(4) . ?
N6 C24 1.396(4) . ?
C18 C19 1.444(5) . ?
C18 C17 1.406(4) . ?
C18 C24 1.438(5) . ?
N8 C38 1.389(4) . ?
N8 C35 1.368(4) . ?
N5 C26 1.386(4) . ?
N5 C29 1.373(4) . ?
C19 C20 1.392(5) . ?
C19 C21 1.419(5) . ?
C53 C47 1.431(5) . ?
C53 C52 1.362(5) . ?
C48 C47 1.440(4) . ?
C48 C49 1.393(5) . ?
C48 C50 1.418(5) . ?
C17 C16 1.401(4) . ?
C47 C46 1.399(5) . ?
C16 C11 1.436(5) . ?
C16 C15 1.436(5) . ?
C46 C45 1.393(5) . ?
C25 C26 1.430(5) . ?
C70 C71 1.505(5) . ?
N7 C39 1.263(5) . ?
N7 C40 1.407(4) . ?
C24 C23 1.364(5) . ?
C38 C39 1.424(5) . ?
C38 C37 1.385(5) . ?
C43 C44 1.422(5) . ?
C43 C42 1.345(5) . ?
C55 C56 1.401(5) . ?
C55 C54 1.397(5) . ?
C33 C30 1.550(5) . ?
C33 C34 1.517(5) . ?
C23 C22 1.418(5) . ?
C11 C12 1.369(5) . ?
C30 C35 1.511(5) . ?
C30 C29 1.500(5) . ?
C30 C31 1.567(5) . ?
C44 C45 1.434(4) . ?
C44 C49 1.394(5) . ?
C42 C41 1.415(5) . ?
C22 C21 1.351(5) . ?
C52 C51 1.412(5) . ?
C15 C20 1.386(5) . ?
C15 C14 1.431(5) . ?
C40 C45 1.437(5) . ?
C40 C41 1.371(5) . ?
C63 C62 1.481(7) . ?
C6 C1 1.504(6) . ?
C6 C7 1.413(6) . ?
C27 C28 1.394(5) . ?
C27 C26 1.377(5) . ?
C35 C36 1.383(5) . ?
C28 C29 1.383(5) . ?
C56 C57 1.380(6) . ?
O5 C81 1.387(7) . ?
O5 C83 1.377(7) . ?
C14 C13 1.351(5) . ?
C10 C9 1.387(6) . ?
C62 C61 1.408(9) . ?
C80 C82 1.453(9) . ?
C80 C81 1.466(8) . ?
C13 C12 1.391(6) . ?
C4 C1 1.550(5) . ?
C4 C5 1.516(6) . ?
C73 C72 1.489(6) . ?
C58 C1 1.508(6) . ?
C58 C57 1.400(6) . ?
C36 C37 1.381(6) . ?
C1 C2A 1.541(15) . ?
C1 C2B 1.644(13) . ?
C71 C72 1.521(5) . ?
C51 C50 1.352(5) . ?
C82 C83 1.410(8) . ?
C9 C8 1.403(5) . ?
C32 C31 1.519(5) . ?
C2A C3A 1.510(15) . ?
C7 C8 1.357(7) . ?
C60 C61 1.509(7) . ?
C3B C2B 1.516(15) . ?

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 O2 175.15(10) . . ?
O1 U1 O3 90.20(9) . . ?
O1 U1 N3 89.17(10) . . ?
O1 U1 N1 95.68(10) . . ?
O1 U1 N4 88.85(10) . . ?
O1 U1 N2 87.01(10) . . ?
O2 U1 O3 84.97(9) . . ?
O2 U1 N3 90.22(10) . . ?
O2 U1 N1 88.08(10) . . ?
O2 U1 N4 95.33(10) . . ?
O2 U1 N2 91.52(10) . . ?
O3 U1 N3 77.98(8) . . ?
O3 U1 N2 77.13(9) . . ?
N3 U1 N2 154.80(9) . . ?
N1 U1 O3 145.01(9) . . ?
N1 U1 N3 136.38(10) . . ?
N1 U1 N4 70.03(10) . . ?
N1 U1 N2 68.81(10) . . ?
N4 U1 O3 144.74(9) . . ?
N4 U1 N3 66.76(9) . . ?
N4 U1 N2 137.96(9) . . ?
N8 Ge1 O4 92.73(10) . . ?
N5 Ge1 O4 85.34(9) . . ?
N5 Ge1 N8 87.23(11) . . ?
C63 O3 U1 127.5(2) . . ?
C63 O3 C60 109.6(3) . . ?
C60 O3 U1 122.9(2) . . ?
C70 O4 Ge1 117.8(2) . . ?
C73 O4 Ge1 124.9(2) . . ?
C73 O4 C70 109.3(3) . . ?
C53 N3 U1 127.4(2) . . ?
C54 N3 U1 113.4(2) . . ?
C54 N3 C53 119.2(3) . . ?
C6 N1 U1 138.8(3) . . ?
C6 N1 C9 106.6(3) . . ?
C9 N1 U1 113.0(2) . . ?
C55 N4 U1 112.8(2) . . ?
C58 N4 U1 137.3(3) . . ?
C58 N4 C55 106.7(3) . . ?
C11 N2 U1 128.5(2) . . ?
C10 N2 U1 111.4(2) . . ?
C10 N2 C11 116.1(3) . . ?
C25 N6 C24 118.1(3) . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 C24 122.9(3) . . ?
C24 C18 C19 118.0(3) . . ?
C38 N8 Ge1 121.6(2) . . ?
C35 N8 Ge1 128.6(2) . . ?
C35 N8 C38 107.2(3) . . ?
C26 N5 Ge1 123.5(2) . . ?
C29 N5 Ge1 129.3(2) . . ?
C29 N5 C26 107.2(3) . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 121.6(3) . . ?
C21 C19 C18 119.5(3) . . ?
N3 C53 C47 121.2(3) . . ?
C52 C53 N3 118.2(3) . . ?
C52 C53 C47 120.6(3) . . ?
C49 C48 C47 118.6(3) . . ?
C49 C48 C50 122.4(3) . . ?
C50 C48 C47 119.0(3) . . ?
C16 C17 C18 121.3(3) . . ?
C53 C47 C48 117.9(3) . . ?
C46 C47 C53 122.8(3) . . ?
C46 C47 C48 119.3(3) . . ?
C17 C16 C11 123.4(3) . . ?
C17 C16 C15 118.9(3) . . ?
C15 C16 C11 117.7(3) . . ?
C45 C46 C47 121.4(3) . . ?
N6 C25 C26 124.0(3) . . ?
O4 C70 C71 105.6(3) . . ?
C39 N7 C40 118.0(3) . . ?
N6 C24 C18 119.2(3) . . ?
C23 C24 N6 121.2(3) . . ?
C23 C24 C18 119.5(3) . . ?
N8 C38 C39 124.5(3) . . ?
C37 C38 N8 108.5(3) . . ?
C37 C38 C39 126.9(4) . . ?
C42 C43 C44 120.7(3) . . ?
N7 C39 C38 125.3(3) . . ?
N4 C55 C56 109.6(3) . . ?
N4 C55 C54 118.6(3) . . ?
C54 C55 C56 131.0(4) . . ?
C34 C33 C30 115.2(3) . . ?
C24 C23 C22 122.1(3) . . ?
N2 C11 C16 120.7(3) . . ?
C12 C11 N2 119.1(3) . . ?
C12 C11 C16 120.2(3) . . ?
C33 C30 C31 107.4(3) . . ?
C35 C30 C33 109.8(3) . . ?
C35 C30 C31 107.3(3) . . ?
C29 C30 C33 109.6(3) . . ?
C29 C30 C35 114.5(3) . . ?
C29 C30 C31 108.0(3) . . ?
C43 C44 C45 119.1(3) . . ?
C49 C44 C43 122.1(3) . . ?
C49 C44 C45 118.8(3) . . ?
C43 C42 C41 121.0(4) . . ?
C21 C22 C23 119.9(3) . . ?
C53 C52 C51 120.9(3) . . ?
C20 C15 C16 119.7(3) . . ?
C20 C15 C14 121.1(3) . . ?
C14 C15 C16 119.2(3) . . ?
N7 C40 C45 118.9(3) . . ?
C41 C40 N7 121.7(3) . . ?
C41 C40 C45 119.4(3) . . ?
C46 C45 C44 119.5(3) . . ?
C46 C45 C40 121.7(3) . . ?
C44 C45 C40 118.7(3) . . ?
O3 C63 C62 105.2(4) . . ?
N1 C6 C1 125.0(3) . . ?
N1 C6 C7 109.5(4) . . ?
C7 C6 C1 125.1(4) . . ?
C26 C27 C28 107.2(3) . . ?
N8 C35 C30 124.1(3) . . ?
N8 C35 C36 109.0(3) . . ?
C36 C35 C30 126.4(3) . . ?
C29 C28 C27 107.7(3) . . ?
C57 C56 C55 106.2(4) . . ?
C15 C20 C19 122.1(3) . . ?
C83 O5 C81 108.9(4) . . ?
C13 C14 C15 120.5(4) . . ?
N3 C54 C55 121.0(3) . . ?
N2 C10 C9 123.3(4) . . ?
C61 C62 C63 107.2(5) . . ?
N5 C26 C25 123.5(3) . . ?
C27 C26 N5 109.1(3) . . ?
C27 C26 C25 127.3(3) . . ?
C82 C80 C81 104.6(5) . . ?
C14 C13 C12 121.0(4) . . ?
C5 C4 C1 116.1(3) . . ?
O4 C73 C72 104.2(3) . . ?
N4 C58 C1 122.7(4) . . ?
N4 C58 C57 109.5(4) . . ?
C57 C58 C1 126.7(3) . . ?
C37 C36 C35 107.8(3) . . ?
C11 C12 C13 121.5(4) . . ?
N5 C29 C30 123.8(3) . . ?
N5 C29 C28 108.9(3) . . ?
C28 C29 C30 127.0(3) . . ?
C6 C1 C4 109.9(3) . . ?
C6 C1 C58 115.1(3) . . ?
C6 C1 C2A 118.5(6) . . ?
C6 C1 C2B 96.0(5) . . ?
C4 C1 C2B 113.1(5) . . ?
C58 C1 C4 111.2(4) . . ?
C58 C1 C2A 101.5(6) . . ?
C58 C1 C2B 110.7(5) . . ?
C2A C1 C4 99.3(5) . . ?
C48 C49 C44 122.4(3) . . ?
C70 C71 C72 103.2(3) . . ?
C50 C51 C52 120.4(3) . . ?
C83 C82 C80 105.1(6) . . ?
N1 C9 C8 109.0(4) . . ?
C10 C9 N1 121.4(3) . . ?
C10 C9 C8 129.6(4) . . ?
C3A C2A C1 112.7(8) . . ?
C40 C41 C42 121.1(4) . . ?
C51 C50 C48 121.1(3) . . ?
C8 C7 C6 107.8(4) . . ?
O5 C81 C80 107.2(5) . . ?
C7 C8 C9 107.1(4) . . ?
C32 C31 C30 114.6(3) . . ?
C22 C21 C19 121.0(3) . . ?
O3 C60 C61 103.8(4) . . ?
C73 C72 C71 102.5(3) . . ?
C56 C57 C58 108.1(3) . . ?
C36 C37 C38 107.4(4) . . ?
O5 C83 C82 109.6(6) . . ?
C62 C61 C60 106.8(5) . . ?
C3B C2B C1 109.0(8) . . ?

_shelx_SHELXL_version_number     2014/7
_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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.880
####################################################################### 
# 
# 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_UO2PbLApyPY-O
_database_code_depnum_ccdc_archive 'CCDC 1480062'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H58 N10 O3 Pb U, 4(C5 H5 N)'
_chemical_formula_sum            'C88 H78 N14 O3 Pb U'
_chemical_formula_weight         1824.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H60 N5 U O3 Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   13.4766(2)
_cell_length_b                   14.4442(2)
_cell_length_c                   23.4695(3)
_cell_angle_alpha                97.6520(10)
_cell_angle_beta                 97.1410(10)
_cell_angle_gamma                110.0560(10)
_cell_volume                     4181.79(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    37782
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.9040
_cell_measurement_theta_min      3.3300
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.3765
_exptl_crystal_size_mid          0.3244
_exptl_crystal_size_min          0.1829
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            19171
_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         27.484
_diffrn_reflns_theta_min         2.867
_diffrn_ambient_temperature      170(2)
_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -45.00   53.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518   38.0000  120.0000 98

#__ type_ start__ end____ width___ exp.time_
  2 omega  -92.00    6.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -38.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   22.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -99.0000   90.0000 47

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   51.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518   77.0000 -150.0000 101

#__ type_ start__ end____ width___ exp.time_
  5 omega   -9.00   49.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   80.0000  -65.0000 58

#__ type_ start__ end____ width___ exp.time_
  6 omega  -25.00   22.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -99.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
  7 omega  -49.00   11.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -80.0000  170.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega  -88.00    2.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4518  -57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
  9 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000  120.0000 89

#__ type_ start__ end____ width___ exp.time_
 10 omega   32.00   98.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -179.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
 11 omega    1.00   91.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 12 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000    0.0000 89

#__ type_ start__ end____ width___ exp.time_
 13 omega  -47.00   43.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -57.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
 14 omega  -25.00   64.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000 -150.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0321813000
_diffrn_orient_matrix_UB_12      -0.0484791000
_diffrn_orient_matrix_UB_13      -0.0162281000
_diffrn_orient_matrix_UB_21      -0.0218355000
_diffrn_orient_matrix_UB_22      0.0219749000
_diffrn_orient_matrix_UB_23      -0.0211358000
_diffrn_orient_matrix_UB_31      0.0416551000
_diffrn_orient_matrix_UB_32      0.0006871000
_diffrn_orient_matrix_UB_33      -0.0158700000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15630
_reflns_number_total             19171
_reflns_odcompleteness_completeness 99.86
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         1.918
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         19171
_refine_ls_number_restraints     207
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²+3.0009P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0717
_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. Uiso/Uaniso restraints and constraints
N11 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim N12 \\sim C122 \\sim C123 \\sim C124 \\sim C125: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N21 \\sim C151 \\sim N151 \\sim C153 \\sim C154 \\sim C155: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N11, C111, C112, C113, C114, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, N12, C122, C123, C124, C125
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, C131, C132, C133, C134, C135
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N21, C151, N151, C153, C154, C155
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C4(H4A,H4B), C2(H2A,H2B), C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C154(H154), C17(H17), C47(H47), C39(H39), C57(H57), C54(H54), C8(H8),
 C115(H115), C43(H43), C52(H52), C36(H36), C41(H41), C10(H10), C14(H14),
 C25(H25), C27(H27), C56(H56), C46(H46), C18(H18), C112(H112), C153(H153),
 C12(H12), C7(H7), C23(H23), C64(H64), C28(H28), C37(H37), C132(H132), C68(H68),
  C133(H133), C123(H123), C111(H111), C60(H60), C59(H59), C121(H121),
 C113(H113), C65(H65), C21(H21), C51(H51), C50(H50), C63(H63), C22(H22),
 C125(H125), C152(H152), C122(H122), C131(H131), C67(H67), C66(H66), C42(H42),
 C124(H124), C13(H13), C61(H61), C62(H62), C134(H134), C151(H151), C155(H155),
 C114(H114), C135(H135)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C34(H34A,H34B,H34C)
;
_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 0.09696(2) 0.43661(2) 0.12756(2) 0.01723(4) Uani 1 1 d . . . . .
Pb1 Pb 0.19052(2) 0.53055(2) 0.32418(2) 0.02275(4) Uani 1 1 d . . . . .
O2 O 0.02630(17) 0.43489(17) 0.05834(10) 0.0233(5) Uani 1 1 d . . . . .
O1 O 0.16964(18) 0.44119(18) 0.19731(10) 0.0261(5) Uani 1 1 d . . . . .
N4 N 0.2195(2) 0.6069(2) 0.11104(11) 0.0194(6) Uani 1 1 d . . . . .
N5 N 0.2466(2) 0.4233(2) 0.08190(12) 0.0227(6) Uani 1 1 d . . . . .
N6 N -0.0060(2) 0.4412(2) 0.35762(13) 0.0300(7) Uani 1 1 d . . . . .
N2 N 0.0719(2) 0.2607(2) 0.10057(12) 0.0213(6) Uani 1 1 d . . . . .
N8 N 0.3727(2) 0.5696(2) 0.36536(11) 0.0209(6) Uani 1 1 d . . . . .
N21 N 0.1948(2) 0.6238(2) 0.42171(13) 0.0309(7) Uani 1 1 d . U . . .
O3 O 0.03226(18) 0.54792(18) 0.17584(11) 0.0277(5) Uani 1 1 d . . . . .
N9 N 0.3231(2) 0.7326(2) 0.33273(12) 0.0240(6) Uani 1 1 d . . . . .
C35 C 0.4206(3) 0.5120(3) 0.38975(14) 0.0230(7) Uani 1 1 d . . . . .
C45 C 0.2487(3) 0.8209(2) 0.26714(14) 0.0223(7) Uani 1 1 d . . . . .
N3 N -0.0901(2) 0.3223(2) 0.13912(12) 0.0231(6) Uani 1 1 d . . . . .
C11 C -0.1812(3) 0.3516(3) 0.13912(15) 0.0248(7) Uani 1 1 d . . . . .
N10 N -0.0313(2) 0.5991(2) 0.16441(14) 0.0295(7) Uani 1 1 d . . . . .
C154 C 0.5010(5) 0.6595(5) 0.2476(3) 0.0819(18) Uani 1 1 d . U . . .
H154 H 0.4499 0.6265 0.2686 0.098 Uiso 1 1 calc R . . . .
C17 C -0.3018(3) 0.4885(3) 0.23927(17) 0.0350(9) Uani 1 1 d . . . . .
H17 H -0.3564 0.5142 0.2365 0.042 Uiso 1 1 calc R . . . .
C6 C 0.1255(3) 0.2051(2) 0.07758(14) 0.0216(7) Uani 1 1 d . . . . .
N12 N 0.3492(6) 0.8660(6) 0.6628(3) 0.120(2) Uani 1 1 d . U . . .
C47 C 0.1685(3) 0.9090(3) 0.20581(16) 0.0297(8) Uani 1 1 d . . . . .
H47 H 0.1448 0.9616 0.2020 0.036 Uiso 1 1 calc R . . . .
C39 C 0.4097(3) 0.7475(3) 0.36952(14) 0.0259(7) Uani 1 1 d . . . . .
H39 H 0.4550 0.8132 0.3856 0.031 Uiso 1 1 calc R . . . .
C20 C -0.1529(3) 0.4655(3) 0.29749(16) 0.0284(8) Uani 1 1 d . . . . .
N7 N 0.1845(2) 0.3999(2) 0.37679(12) 0.0254(6) Uani 1 1 d . . . . .
C9 C -0.0317(3) 0.1941(3) 0.09863(14) 0.0235(7) Uani 1 1 d . . . . .
C16 C -0.1970(3) 0.4037(3) 0.19219(15) 0.0263(8) Uani 1 1 d . . . . .
C31 C 0.3470(3) 0.3644(3) 0.30806(15) 0.0294(8) Uani 1 1 d . . . . .
H31A H 0.3118 0.2920 0.2985 0.035 Uiso 1 1 calc R . . . .
H31B H 0.2985 0.3933 0.2903 0.035 Uiso 1 1 calc R . . . .
C57 C 0.3720(3) 0.3929(3) 0.03548(17) 0.0338(9) Uani 1 1 d . . . . .
H57 H 0.4133 0.3596 0.0197 0.041 Uiso 1 1 calc R . . . .
C19 C -0.2399(3) 0.5021(3) 0.29317(17) 0.0327(9) Uani 1 1 d . . . . .
C54 C 0.2864(3) 0.5984(3) 0.07680(15) 0.0249(7) Uani 1 1 d . . . . .
H54 H 0.3218 0.6531 0.0605 0.030 Uiso 1 1 calc R . . . .
C8 C -0.0421(3) 0.0974(3) 0.07379(16) 0.0304(8) Uani 1 1 d . . . . .
H8 H -0.1035 0.0397 0.0673 0.037 Uiso 1 1 calc R . . . .
C115 C 0.9649(7) 0.0234(6) 0.2147(3) 0.0922(19) Uani 1 1 d . U . . .
H115 H 0.9793 -0.0300 0.1957 0.111 Uiso 1 1 calc R . . . .
C30 C 0.3691(3) 0.3990(3) 0.37573(15) 0.0263(7) Uani 1 1 d . . . . .
C43 C 0.2208(3) 0.9736(3) 0.31127(18) 0.0395(10) Uani 1 1 d . . . . .
H43 H 0.1971 1.0262 0.3073 0.047 Uiso 1 1 calc R . . . .
C52 C 0.1390(3) 0.7006(3) 0.05661(15) 0.0255(7) Uani 1 1 d . . . . .
H52 H 0.1320 0.6546 0.0232 0.031 Uiso 1 1 calc R . . . .
C15 C -0.2853(3) 0.4374(3) 0.18853(16) 0.0308(8) Uani 1 1 d . . . . .
C4 C 0.3043(3) 0.2559(3) 0.14110(16) 0.0326(8) Uani 1 1 d . . . . .
H4A H 0.3811 0.2818 0.1417 0.039 Uiso 1 1 calc R . . . .
H4B H 0.2885 0.3047 0.1673 0.039 Uiso 1 1 calc R . . . .
C36 C 0.5174(3) 0.5736(3) 0.42636(15) 0.0295(8) Uani 1 1 d . . . . .
H36 H 0.5654 0.5527 0.4482 0.035 Uiso 1 1 calc R . . . .
C29 C 0.2630(3) 0.3685(3) 0.39759(14) 0.0260(7) Uani 1 1 d . . . . .
C48 C 0.1590(3) 0.8402(3) 0.15586(15) 0.0249(7) Uani 1 1 d . . . . .
C53 C 0.1860(2) 0.6902(2) 0.10905(14) 0.0208(7) Uani 1 1 d . . . . .
C41 C 0.2989(3) 0.8856(3) 0.37200(16) 0.0324(8) Uani 1 1 d . . . . .
H41 H 0.3265 0.8807 0.4093 0.039 Uiso 1 1 calc R . . . .
C55 C 0.3069(3) 0.5093(3) 0.06372(15) 0.0256(7) Uani 1 1 d . . . . .
C2 C 0.2761(3) 0.1763(3) 0.03440(17) 0.0332(9) Uani 1 1 d . . . . .
H2A H 0.3538 0.1998 0.0397 0.040 Uiso 1 1 calc R . . . .
H2B H 0.2514 0.1100 0.0443 0.040 Uiso 1 1 calc R . . . .
C44 C 0.2116(3) 0.9017(3) 0.26060(16) 0.0287(8) Uani 1 1 d . . . . .
C26 C 0.1015(3) 0.3659(3) 0.40684(15) 0.0305(8) Uani 1 1 d . . . . .
C49 C 0.1966(2) 0.7595(2) 0.16163(14) 0.0199(7) Uani 1 1 d . . . . .
C10 C -0.1110(3) 0.2286(3) 0.11643(14) 0.0247(7) Uani 1 1 d . . . . .
H10 H -0.1809 0.1828 0.1119 0.030 Uiso 1 1 calc R . . . .
C14 C -0.3564(3) 0.4162(3) 0.13383(17) 0.0390(10) Uani 1 1 d . . . . .
H14 H -0.4137 0.4384 0.1313 0.047 Uiso 1 1 calc R . . . .
C25 C 0.0083(3) 0.3900(3) 0.39681(16) 0.0328(9) Uani 1 1 d . . . . .
H25 H -0.0445 0.3682 0.4192 0.039 Uiso 1 1 calc R . . . .
C27 C 0.1292(3) 0.3114(3) 0.44682(18) 0.0404(10) Uani 1 1 d . . . . .
H27 H 0.0874 0.2801 0.4724 0.049 Uiso 1 1 calc R . . . .
C56 C 0.3850(3) 0.4911(3) 0.03515(18) 0.0364(9) Uani 1 1 d . . . . .
H56 H 0.4358 0.5366 0.0191 0.044 Uiso 1 1 calc R . . . .
C46 C 0.2411(2) 0.7519(2) 0.21688(14) 0.0206(7) Uani 1 1 d . . . . .
H46 H 0.2662 0.7001 0.2206 0.025 Uiso 1 1 calc R . . . .
C18 C -0.1325(3) 0.4185(3) 0.24656(15) 0.0251(7) Uani 1 1 d . . . . .
H18 H -0.0750 0.3968 0.2489 0.030 Uiso 1 1 calc R . . . .
C112 C 0.9191(7) 0.1749(5) 0.2646(3) 0.096(2) Uani 1 1 d . U . . .
H112 H 0.9069 0.2302 0.2829 0.115 Uiso 1 1 calc R . . . .
N11 N 0.8628(6) 0.0171(5) 0.2087(3) 0.1128(19) Uani 1 1 d . U . . .
C153 C 0.6515(6) 0.7981(5) 0.2405(3) 0.0923(19) Uani 1 1 d . U . . .
H153 H 0.7047 0.8594 0.2583 0.111 Uiso 1 1 calc R . . . .
C40 C 0.2933(3) 0.8147(3) 0.32506(15) 0.0243(7) Uani 1 1 d . . . . .
C12 C -0.2520(3) 0.3326(3) 0.08882(16) 0.0336(9) Uani 1 1 d . . . . .
H12 H -0.2419 0.2978 0.0551 0.040 Uiso 1 1 calc R . . . .
C24 C -0.0935(3) 0.4743(3) 0.35450(16) 0.0320(9) Uani 1 1 d . . . . .
C7 C 0.0564(3) 0.1042(3) 0.06070(16) 0.0299(8) Uani 1 1 d . . . . .
H7 H 0.0742 0.0514 0.0437 0.036 Uiso 1 1 calc R . . . .
C23 C -0.1195(3) 0.5173(3) 0.40309(18) 0.0409(10) Uani 1 1 d . . . . .
H23 H -0.0802 0.5233 0.4398 0.049 Uiso 1 1 calc R . . . .
C64 C 0.1441(3) 0.6877(3) 0.42610(19) 0.0406(10) Uani 1 1 d . . . . .
H64 H 0.1025 0.6917 0.3925 0.049 Uiso 1 1 calc R . . . .
C28 C 0.2304(3) 0.3130(3) 0.44100(17) 0.0381(9) Uani 1 1 d . . . . .
H28 H 0.2697 0.2828 0.4620 0.046 Uiso 1 1 calc R . . . .
C37 C 0.5281(3) 0.6715(3) 0.42392(16) 0.0307(8) Uani 1 1 d . . . . .
H37 H 0.5850 0.7289 0.4438 0.037 Uiso 1 1 calc R . . . .
C38 C 0.4379(3) 0.6682(3) 0.38619(14) 0.0236(7) Uani 1 1 d . . . . .
C132 C 0.5589(6) 0.9874(6) 0.9329(4) 0.115(2) Uani 1 1 d . U . . .
H132 H 0.6054 0.9580 0.9479 0.138 Uiso 1 1 calc R . . . .
C68 C 0.2537(3) 0.6177(3) 0.46967(16) 0.0395(10) Uani 1 1 d . . . . .
H68 H 0.2895 0.5730 0.4672 0.047 Uiso 1 1 calc R . . . .
C58 C 0.2849(2) 0.3509(3) 0.06397(15) 0.0233(7) Uani 1 1 d . . . . .
C33 C 0.4449(3) 0.3529(3) 0.40514(18) 0.0367(9) Uani 1 1 d . . . . .
H33A H 0.5160 0.3848 0.3966 0.044 Uiso 1 1 calc R . . . .
H33B H 0.4501 0.3686 0.4471 0.044 Uiso 1 1 calc R . . . .
C133 C 0.5955(6) 1.0805(7) 0.9225(5) 0.130(3) Uani 1 1 d . U . . .
H133 H 0.6682 1.1202 0.9320 0.156 Uiso 1 1 calc R . . . .
C32 C 0.4492(3) 0.3949(3) 0.28220(17) 0.0392(10) Uani 1 1 d . . . . .
H32A H 0.4890 0.4655 0.2954 0.059 Uiso 1 1 calc GR . . . .
H32B H 0.4307 0.3806 0.2403 0.059 Uiso 1 1 calc GR . . . .
H32C H 0.4925 0.3580 0.2946 0.059 Uiso 1 1 calc GR . . . .
C123 C 0.4900(7) 0.9720(7) 0.7357(4) 0.128(3) Uani 1 1 d . U . . .
H123 H 0.5437 1.0347 0.7501 0.154 Uiso 1 1 calc R . . . .
C3 C 0.2316(4) 0.1668(3) -0.02980(17) 0.0444(11) Uani 1 1 d . . . . .
H3A H 0.1551 0.1492 -0.0352 0.067 Uiso 1 1 calc GR . . . .
H3B H 0.2477 0.1155 -0.0529 0.067 Uiso 1 1 calc GR . . . .
H3C H 0.2638 0.2296 -0.0419 0.067 Uiso 1 1 calc GR . . . .
C111 C 0.8396(6) 0.0932(6) 0.2339(3) 0.0867(18) Uani 1 1 d . U . . .
H111 H 0.7687 0.0895 0.2302 0.104 Uiso 1 1 calc R . . . .
C60 C -0.0820(3) 0.5893(3) 0.10971(19) 0.0382(9) Uani 1 1 d . . . . .
H60 H -0.0735 0.5462 0.0791 0.046 Uiso 1 1 calc R . . . .
C59 C -0.1463(3) 0.6432(4) 0.0992(2) 0.0509(12) Uani 1 1 d . . . . .
H59 H -0.1808 0.6376 0.0613 0.061 Uiso 1 1 calc R . . . .
C121 C 0.3446(6) 0.7957(6) 0.6920(4) 0.102(3) Uani 1 1 d . . . . .
H121 H 0.2946 0.7322 0.6752 0.123 Uiso 1 1 calc R . . . .
C113 C 1.0220(7) 0.1718(7) 0.2674(4) 0.121(3) Uani 1 1 d . U . . .
H113 H 1.0813 0.2271 0.2874 0.145 Uiso 1 1 calc R . . . .
C65 C 0.1497(4) 0.7485(3) 0.4777(2) 0.0504(12) Uani 1 1 d . . . . .
H65 H 0.1127 0.7923 0.4790 0.061 Uiso 1 1 calc R . . . .
C1 C 0.2451(3) 0.2472(3) 0.07765(15) 0.0248(7) Uani 1 1 d . . . . .
C5 C 0.2763(4) 0.1599(3) 0.16495(19) 0.0469(11) Uani 1 1 d . . . . .
H5A H 0.2000 0.1315 0.1631 0.070 Uiso 1 1 calc GR . . . .
H5B H 0.3123 0.1740 0.2048 0.070 Uiso 1 1 calc GR . . . .
H5C H 0.2988 0.1131 0.1420 0.070 Uiso 1 1 calc GR . . . .
C21 C -0.2629(3) 0.5473(4) 0.34598(19) 0.0447(11) Uani 1 1 d . . . . .
H21 H -0.3177 0.5727 0.3438 0.054 Uiso 1 1 calc R . . . .
C51 C 0.1005(3) 0.7799(3) 0.05159(16) 0.0313(8) Uani 1 1 d . . . . .
H51 H 0.0684 0.7851 0.0153 0.038 Uiso 1 1 calc R . . . .
C50 C 0.1108(3) 0.8478(3) 0.09976(16) 0.0313(8) Uani 1 1 d . . . . .
H50 H 0.0862 0.9000 0.0963 0.038 Uiso 1 1 calc R . . . .
C63 C -0.0424(3) 0.6592(3) 0.21026(19) 0.0396(10) Uani 1 1 d . . . . .
H63 H -0.0068 0.6643 0.2478 0.047 Uiso 1 1 calc R . . . .
C22 C -0.2054(3) 0.5530(4) 0.39843(19) 0.0492(12) Uani 1 1 d . . . . .
H22 H -0.2223 0.5809 0.4322 0.059 Uiso 1 1 calc R . . . .
C125 C 0.4017(9) 0.8037(8) 0.7419(4) 0.116(3) Uani 1 1 d . U . . .
H125 H 0.3896 0.7499 0.7614 0.139 Uiso 1 1 calc R . . . .
C152 C 0.4951(4) 0.6226(5) 0.1918(2) 0.0624(14) Uani 1 1 d . . . . .
H152 H 0.4423 0.5614 0.1734 0.075 Uiso 1 1 calc R . . . .
C122 C 0.4167(8) 0.9534(6) 0.6842(3) 0.125(3) Uani 1 1 d . U . . .
H122 H 0.4173 1.0062 0.6652 0.150 Uiso 1 1 calc R . . . .
C131 C 0.4474(8) 0.9357(7) 0.9202(5) 0.137(3) Uani 1 1 d . U . . .
H131 H 0.4203 0.8703 0.9266 0.164 Uiso 1 1 calc R . . . .
C67 C 0.2635(4) 0.6763(4) 0.52356(18) 0.0551(14) Uani 1 1 d . . . . .
H67 H 0.3050 0.6707 0.5567 0.066 Uiso 1 1 calc R . . . .
C66 C 0.2112(4) 0.7426(4) 0.5271(2) 0.0553(14) Uani 1 1 d . . . . .
H66 H 0.2174 0.7831 0.5627 0.066 Uiso 1 1 calc R . . . .
C34 C 0.4116(4) 0.2393(3) 0.3868(2) 0.0578(13) Uani 1 1 d . . . . .
H34A H 0.3371 0.2072 0.3886 0.087 Uiso 1 1 calc GR . . . .
H34B H 0.4543 0.2157 0.4127 0.087 Uiso 1 1 calc GR . . . .
H34C H 0.4224 0.2238 0.3475 0.087 Uiso 1 1 calc GR . . . .
C42 C 0.2636(3) 0.9654(3) 0.36483(17) 0.0394(10) Uani 1 1 d . . . . .
H42 H 0.2699 1.0130 0.3973 0.047 Uiso 1 1 calc R . . . .
C124 C 0.4782(7) 0.8917(9) 0.7642(4) 0.124(3) Uani 1 1 d . U . . .
H124 H 0.5243 0.8999 0.7990 0.149 Uiso 1 1 calc R . . . .
C13 C -0.3404(3) 0.3636(3) 0.08569(17) 0.0384(10) Uani 1 1 d . . . . .
H13 H -0.3880 0.3481 0.0505 0.046 Uiso 1 1 calc R . . . .
C61 C -0.1596(4) 0.7053(4) 0.1446(3) 0.0598(14) Uani 1 1 d . . . . .
H61 H -0.2033 0.7419 0.1379 0.072 Uiso 1 1 calc R . . . .
N151 N 0.6461(4) 0.7653(4) 0.1847(2) 0.0744(13) Uani 1 1 d . U . . .
N13 N 0.3793(5) 0.9757(7) 0.8995(4) 0.137(3) Uani 1 1 d . . . . .
C62 C -0.1075(4) 0.7128(4) 0.2004(2) 0.0569(13) Uani 1 1 d . . . . .
H62 H -0.1164 0.7545 0.2315 0.068 Uiso 1 1 calc R . . . .
C134 C 0.5214(7) 1.1156(7) 0.8972(5) 0.144(3) Uani 1 1 d . U . . .
H134 H 0.5440 1.1773 0.8853 0.173 Uiso 1 1 calc R . . . .
C151 C 0.5699(5) 0.6777(5) 0.1616(3) 0.0788(17) Uani 1 1 d . U . . .
H151 H 0.5660 0.6512 0.1227 0.095 Uiso 1 1 calc R . . . .
C155 C 0.5834(6) 0.7470(5) 0.2736(3) 0.109(2) Uani 1 1 d . U . . .
H155 H 0.5930 0.7713 0.3134 0.131 Uiso 1 1 calc R . . . .
C114 C 1.0357(6) 0.0907(7) 0.2419(4) 0.101(2) Uani 1 1 d . U . . .
H114 H 1.1042 0.0883 0.2462 0.121 Uiso 1 1 calc R . . . .
C135 C 0.4225(7) 1.0637(8) 0.8901(5) 0.128(3) Uani 1 1 d . U . . .
H135 H 0.3757 1.0938 0.8763 0.154 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 O2 1.771(2) . ?
U1 O1 1.781(2) . ?
U1 N4 2.561(3) . ?
U1 N5 2.449(3) . ?
U1 N2 2.430(3) . ?
U1 O3 2.313(2) . ?
U1 N3 2.567(3) . ?
Pb1 N6 2.782(3) . ?
Pb1 N8 2.366(3) . ?
Pb1 N21 2.480(3) . ?
Pb1 N7 2.374(3) . ?
N4 C54 1.305(4) . ?
N4 C53 1.427(4) . ?
N5 C55 1.387(4) . ?
N5 C58 1.357(4) . ?
N6 C25 1.290(5) . ?
N6 C24 1.414(5) . ?
N2 C6 1.354(4) . ?
N2 C9 1.389(4) . ?
N8 C35 1.357(4) . ?
N8 C38 1.375(4) . ?
N21 C64 1.324(5) . ?
N21 C68 1.325(5) . ?
O3 N10 1.335(4) . ?
N9 C39 1.296(4) . ?
N9 C40 1.402(4) . ?
C35 C30 1.508(5) . ?
C35 C36 1.398(5) . ?
C45 C44 1.437(5) . ?
C45 C46 1.407(4) . ?
C45 C40 1.443(5) . ?
N3 C11 1.429(4) . ?
N3 C10 1.306(4) . ?
C11 C16 1.445(5) . ?
C11 C12 1.354(5) . ?
N10 C60 1.342(5) . ?
N10 C63 1.348(5) . ?
C154 C152 1.328(7) . ?
C154 C155 1.366(9) . ?
C17 C19 1.376(5) . ?
C17 C15 1.399(5) . ?
C6 C7 1.405(5) . ?
C6 C1 1.515(5) . ?
N12 C121 1.287(10) . ?
N12 C122 1.267(9) . ?
C47 C48 1.394(5) . ?
C47 C44 1.377(5) . ?
C39 C38 1.411(5) . ?
C20 C19 1.440(5) . ?
C20 C18 1.399(5) . ?
C20 C24 1.438(5) . ?
N7 C29 1.351(4) . ?
N7 C26 1.378(4) . ?
C9 C8 1.393(5) . ?
C9 C10 1.409(5) . ?
C16 C15 1.430(5) . ?
C16 C18 1.397(5) . ?
C31 C30 1.559(5) . ?
C31 C32 1.524(5) . ?
C57 C56 1.369(5) . ?
C57 C58 1.418(5) . ?
C19 C21 1.441(5) . ?
C54 C55 1.409(5) . ?
C8 C7 1.374(5) . ?
C115 N11 1.335(9) . ?
C115 C114 1.144(9) . ?
C30 C29 1.520(5) . ?
C30 C33 1.542(5) . ?
C43 C44 1.434(5) . ?
C43 C42 1.354(6) . ?
C52 C53 1.363(5) . ?
C52 C51 1.423(5) . ?
C15 C14 1.431(5) . ?
C4 C1 1.567(5) . ?
C4 C5 1.509(6) . ?
C36 C37 1.380(5) . ?
C29 C28 1.400(5) . ?
C48 C49 1.436(5) . ?
C48 C50 1.429(5) . ?
C53 C49 1.440(4) . ?
C41 C40 1.376(5) . ?
C41 C42 1.411(5) . ?
C55 C56 1.395(5) . ?
C2 C3 1.521(5) . ?
C2 C1 1.541(4) . ?
C26 C25 1.416(5) . ?
C26 C27 1.396(5) . ?
C49 C46 1.394(4) . ?
C14 C13 1.358(5) . ?
C27 C28 1.381(5) . ?
C112 C111 1.331(9) . ?
C112 C113 1.396(11) . ?
N11 C111 1.328(9) . ?
C153 N151 1.315(8) . ?
C153 C155 1.362(8) . ?
C12 C13 1.406(5) . ?
C24 C23 1.367(5) . ?
C23 C22 1.417(6) . ?
C64 C65 1.376(6) . ?
C37 C38 1.395(5) . ?
C132 C133 1.332(10) . ?
C132 C131 1.401(11) . ?
C68 C67 1.389(6) . ?
C58 C1 1.502(5) . ?
C33 C34 1.528(6) . ?
C133 C134 1.374(11) . ?
C123 C122 1.393(12) . ?
C123 C124 1.388(12) . ?
C60 C59 1.371(6) . ?
C59 C61 1.370(7) . ?
C121 C125 1.288(11) . ?
C113 C114 1.325(11) . ?
C65 C66 1.370(7) . ?
C21 C22 1.347(6) . ?
C51 C50 1.353(5) . ?
C63 C62 1.373(6) . ?
C125 C124 1.321(12) . ?
C152 C151 1.389(7) . ?
C131 N13 1.319(11) . ?
C67 C66 1.370(7) . ?
C61 C62 1.378(7) . ?
N151 C151 1.318(8) . ?
N13 C135 1.267(10) . ?
C134 C135 1.261(11) . ?

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 O1 178.75(11) . . ?
O2 U1 N4 81.98(9) . . ?
O2 U1 N5 89.80(10) . . ?
O2 U1 N2 91.52(10) . . ?
O2 U1 O3 93.12(9) . . ?
O2 U1 N3 82.32(10) . . ?
O1 U1 N4 96.80(10) . . ?
O1 U1 N5 90.02(10) . . ?
O1 U1 N2 89.59(10) . . ?
O1 U1 O3 86.30(9) . . ?
O1 U1 N3 98.63(10) . . ?
N4 U1 N3 148.74(9) . . ?
N5 U1 N4 68.12(9) . . ?
N5 U1 N3 138.56(9) . . ?
N2 U1 N4 138.35(8) . . ?
N2 U1 N5 70.78(9) . . ?
N2 U1 N3 68.86(9) . . ?
O3 U1 N4 76.94(8) . . ?
O3 U1 N5 144.16(9) . . ?
O3 U1 N2 144.68(8) . . ?
O3 U1 N3 77.11(8) . . ?
N8 Pb1 N6 135.43(9) . . ?
N8 Pb1 N21 81.01(9) . . ?
N8 Pb1 N7 76.44(9) . . ?
N21 Pb1 N6 71.79(9) . . ?
N7 Pb1 N6 65.91(10) . . ?
N7 Pb1 N21 82.95(10) . . ?
C54 N4 U1 112.4(2) . . ?
C54 N4 C53 116.1(3) . . ?
C53 N4 U1 123.11(19) . . ?
C55 N5 U1 114.9(2) . . ?
C58 N5 U1 137.8(2) . . ?
C58 N5 C55 107.0(3) . . ?
C25 N6 Pb1 107.9(2) . . ?
C25 N6 C24 119.8(3) . . ?
C24 N6 Pb1 127.4(2) . . ?
C6 N2 U1 138.3(2) . . ?
C6 N2 C9 106.1(3) . . ?
C9 N2 U1 114.6(2) . . ?
C35 N8 Pb1 129.8(2) . . ?
C35 N8 C38 107.5(3) . . ?
C38 N8 Pb1 119.3(2) . . ?
C64 N21 Pb1 119.8(3) . . ?
C64 N21 C68 118.2(3) . . ?
C68 N21 Pb1 121.8(3) . . ?
N10 O3 U1 139.9(2) . . ?
C39 N9 C40 118.8(3) . . ?
N8 C35 C30 120.8(3) . . ?
N8 C35 C36 109.5(3) . . ?
C36 C35 C30 129.7(3) . . ?
C44 C45 C40 118.4(3) . . ?
C46 C45 C44 118.7(3) . . ?
C46 C45 C40 122.9(3) . . ?
C11 N3 U1 124.8(2) . . ?
C10 N3 U1 111.8(2) . . ?
C10 N3 C11 115.6(3) . . ?
N3 C11 C16 120.5(3) . . ?
C12 C11 N3 119.9(3) . . ?
C12 C11 C16 119.6(3) . . ?
O3 N10 C60 120.8(3) . . ?
O3 N10 C63 116.8(3) . . ?
C60 N10 C63 122.4(3) . . ?
C152 C154 C155 118.7(5) . . ?
C19 C17 C15 122.2(3) . . ?
N2 C6 C7 109.8(3) . . ?
N2 C6 C1 123.1(3) . . ?
C7 C6 C1 126.8(3) . . ?
C122 N12 C121 118.3(8) . . ?
C44 C47 C48 122.2(3) . . ?
N9 C39 C38 122.7(3) . . ?
C18 C20 C19 119.0(3) . . ?
C18 C20 C24 122.4(3) . . ?
C24 C20 C19 118.5(3) . . ?
C29 N7 Pb1 130.5(2) . . ?
C29 N7 C26 107.6(3) . . ?
C26 N7 Pb1 119.1(2) . . ?
N2 C9 C8 110.1(3) . . ?
N2 C9 C10 120.9(3) . . ?
C8 C9 C10 128.9(3) . . ?
C15 C16 C11 117.8(3) . . ?
C18 C16 C11 122.8(3) . . ?
C18 C16 C15 119.3(3) . . ?
C32 C31 C30 112.7(3) . . ?
C56 C57 C58 108.2(3) . . ?
C17 C19 C20 119.2(3) . . ?
C17 C19 C21 121.9(3) . . ?
C20 C19 C21 118.8(4) . . ?
N4 C54 C55 122.3(3) . . ?
C7 C8 C9 106.4(3) . . ?
C114 C115 N11 123.8(8) . . ?
C35 C30 C31 108.4(3) . . ?
C35 C30 C29 108.2(3) . . ?
C35 C30 C33 109.8(3) . . ?
C29 C30 C31 109.2(3) . . ?
C29 C30 C33 111.0(3) . . ?
C33 C30 C31 110.2(3) . . ?
C42 C43 C44 120.4(4) . . ?
C53 C52 C51 121.8(3) . . ?
C17 C15 C16 118.8(3) . . ?
C17 C15 C14 121.4(3) . . ?
C16 C15 C14 119.8(3) . . ?
C5 C4 C1 115.9(3) . . ?
C37 C36 C35 106.9(3) . . ?
N7 C29 C30 120.7(3) . . ?
N7 C29 C28 109.3(3) . . ?
C28 C29 C30 130.0(3) . . ?
C47 C48 C49 118.9(3) . . ?
C47 C48 C50 121.1(3) . . ?
C50 C48 C49 120.0(3) . . ?
N4 C53 C49 120.9(3) . . ?
C52 C53 N4 118.7(3) . . ?
C52 C53 C49 120.3(3) . . ?
C40 C41 C42 121.6(3) . . ?
N5 C55 C54 120.1(3) . . ?
N5 C55 C56 109.9(3) . . ?
C56 C55 C54 130.0(3) . . ?
C3 C2 C1 115.4(3) . . ?
C47 C44 C45 119.5(3) . . ?
C47 C44 C43 121.1(3) . . ?
C43 C44 C45 119.4(3) . . ?
N7 C26 C25 121.5(3) . . ?
N7 C26 C27 109.0(3) . . ?
C27 C26 C25 129.5(3) . . ?
C48 C49 C53 117.4(3) . . ?
C46 C49 C48 119.2(3) . . ?
C46 C49 C53 123.4(3) . . ?
N3 C10 C9 122.5(3) . . ?
C13 C14 C15 120.0(3) . . ?
N6 C25 C26 122.2(3) . . ?
C28 C27 C26 106.8(3) . . ?
C57 C56 C55 106.4(3) . . ?
C49 C46 C45 121.4(3) . . ?
C16 C18 C20 121.3(3) . . ?
C111 C112 C113 115.5(7) . . ?
C111 N11 C115 119.7(7) . . ?
N151 C153 C155 123.5(7) . . ?
N9 C40 C45 119.1(3) . . ?
C41 C40 N9 121.3(3) . . ?
C41 C40 C45 119.5(3) . . ?
C11 C12 C13 122.4(4) . . ?
N6 C24 C20 117.6(3) . . ?
C23 C24 N6 122.3(4) . . ?
C23 C24 C20 120.0(3) . . ?
C8 C7 C6 107.7(3) . . ?
C24 C23 C22 121.1(4) . . ?
N21 C64 C65 123.6(4) . . ?
C27 C28 C29 107.4(3) . . ?
C36 C37 C38 107.3(3) . . ?
N8 C38 C39 121.5(3) . . ?
N8 C38 C37 108.8(3) . . ?
C37 C38 C39 129.7(3) . . ?
C133 C132 C131 117.1(7) . . ?
N21 C68 C67 121.9(4) . . ?
N5 C58 C57 108.6(3) . . ?
N5 C58 C1 124.0(3) . . ?
C57 C58 C1 127.3(3) . . ?
C34 C33 C30 115.5(3) . . ?
C132 C133 C134 117.3(8) . . ?
C124 C123 C122 116.1(8) . . ?
N11 C111 C112 119.1(7) . . ?
N10 C60 C59 119.6(4) . . ?
C61 C59 C60 119.8(5) . . ?
N12 C121 C125 127.1(8) . . ?
C114 C113 C112 120.4(7) . . ?
C66 C65 C64 118.1(5) . . ?
C6 C1 C4 107.4(3) . . ?
C6 C1 C2 110.4(3) . . ?
C2 C1 C4 109.4(3) . . ?
C58 C1 C6 113.9(3) . . ?
C58 C1 C4 106.1(3) . . ?
C58 C1 C2 109.4(3) . . ?
C22 C21 C19 120.4(4) . . ?
C50 C51 C52 119.8(3) . . ?
C51 C50 C48 120.7(3) . . ?
N10 C63 C62 118.6(4) . . ?
C21 C22 C23 121.2(4) . . ?
C121 C125 C124 116.9(10) . . ?
C154 C152 C151 118.3(6) . . ?
N12 C122 C123 121.2(9) . . ?
N13 C131 C132 123.0(9) . . ?
C66 C67 C68 119.0(5) . . ?
C65 C66 C67 119.2(4) . . ?
C43 C42 C41 120.8(3) . . ?
C125 C124 C123 120.1(9) . . ?
C14 C13 C12 120.3(4) . . ?
C59 C61 C62 119.3(4) . . ?
C153 N151 C151 116.0(5) . . ?
C135 N13 C131 114.8(8) . . ?
C63 C62 C61 120.4(4) . . ?
C135 C134 C133 119.6(9) . . ?
N151 C151 C152 124.0(6) . . ?
C153 C155 C154 119.2(7) . . ?
C115 C114 C113 121.4(8) . . ?
C134 C135 N13 127.9(9) . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 6 1 0.1488 -19.0000 6.0000 0.9998 0.3043 0.5256 -0.8032
19 -6 -1 0.1488 19.0000 -6.0000 -0.9998 -0.3043 -0.5256 0.8032
-18 4 16 0.1509 -18.0000 4.0000 16.0000 0.1257 0.1428 -1.0010
18 -4 -16 0.1509 18.0000 -4.0000 -16.0000 -0.1257 -0.1428 1.0010
0 -2 33 0.1763 -0.0000 -2.0000 33.0003 -0.4386 -0.7414 -0.5251
0 2 -33 0.1763 0.0000 2.0000 -33.0003 0.4386 0.7414 0.5251
3 18 -8 0.0914 3.0001 18.0000 -8.0001 -0.8393 0.4991 0.2643
-3 -18 8 0.0914 -3.0001 -18.0000 8.0001 0.8393 -0.4991 -0.2643
-5 20 2 0.1061 -4.9999 20.0000 1.9999 -0.8411 0.5064 -0.2263
5 -20 -2 0.1061 4.9999 -20.0000 -1.9999 0.8411 -0.5064 0.2263

_olex2_submission_special_instructions 'No special instructions were received'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.016 0.000 0.500 512 78 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_Pb2LMe
_database_code_depnum_ccdc_archive 'CCDC 1480063'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H50 N10 Pb2, 2(C5 H5 N)'
_chemical_formula_sum            'C62 H60 N12 Pb2'
_chemical_formula_weight         1387.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C70 H70 N2 O2 Pb 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   11.5029(3)
_cell_length_b                   13.3149(3)
_cell_length_c                   17.9962(6)
_cell_angle_alpha                90.548(2)
_cell_angle_beta                 90.690(2)
_cell_angle_gamma                99.117(2)
_cell_volume                     2721.10(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8668
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.0720
_cell_measurement_theta_min      3.3070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.232
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            ?
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.4602
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.046
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23523
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.869
_diffrn_ambient_temperature      170(2)
_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 0.961
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -24.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000  -60.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega  -16.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000 -150.0000 40

#__ type_ start__ end____ width___ exp.time_
  3 omega  -44.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -57.0000 -180.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega    0.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277   57.0000   60.0000 86

#__ type_ start__ end____ width___ exp.time_
  5 omega    4.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277   57.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
  6 omega  -54.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -19.0000 -120.0000 110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0515230000
_diffrn_orient_matrix_UB_12      0.0329026000
_diffrn_orient_matrix_UB_13      0.0120627000
_diffrn_orient_matrix_UB_21      -0.0166884000
_diffrn_orient_matrix_UB_22      -0.0085507000
_diffrn_orient_matrix_UB_23      0.0375083000
_diffrn_orient_matrix_UB_31      0.0311097000
_diffrn_orient_matrix_UB_32      -0.0419001000
_diffrn_orient_matrix_UB_33      0.0012290000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9191
_reflns_number_total             11982
_reflns_odcompleteness_completeness 96.13
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         2.703
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11982
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      1.019
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1542
_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. Restrained distances
 C70-N69
 1.36 with sigma of 0.02
 N69-C74
 1.36 with sigma of 0.02
 N69-C70 = N69-C74
 1.33 with sigma of 0.02
 C72-C71 = C73-C72
 1.36 with sigma of 0.02
 C71-C70 = C74-C73
 1.35 with sigma of 0.02
 C71-C70 = C74-C73
 1.35 with sigma of 0.01
 N69-C74 = N69-C70
 1.33 with sigma of 0.01
 C72-C71 = C73-C72
 1.36 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C71 \\sim C70 \\sim N69 \\sim C74 \\sim C73 \\sim C72: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(N69)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(N69)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C71, C70, N69, C74, C73, C72
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C62(H62), C42(H42), C58(H58), C9(H9), C34(H34), C20(H20), C12(H12),
 C45(H45), C30(H30), C61(H61), C17(H17), C31(H31), C60(H60), C6(H6), C59(H59),
 C22(H22), C5(H5), C47(H47), C48(H48), C23(H23), C56(H56), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C52(H52), C53(H53), C55(H55), C54(H54), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74)
5.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C41(H41A,H41B,H41C),
 C14(H14A,H14B,H14C), C39(H39A,H39B,H39C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C)
;
_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
Pb1 Pb 0.26712(2) 0.26507(2) 0.63454(2) 0.02553(10) Uani 1 1 d . . . . .
Pb2 Pb 0.39506(2) 0.38687(2) 0.88236(2) 0.02626(10) Uani 1 1 d . . . . .
N10 N 0.3522(5) 0.1950(4) 0.5273(3) 0.0228(12) Uani 1 1 d . . . . .
N57 N 0.4674(5) 0.4222(5) 0.7530(4) 0.0298(14) Uani 1 1 d . . . . .
N33 N 0.2192(6) 0.4906(5) 0.8360(3) 0.0285(14) Uani 1 1 d . . . . .
N50 N 0.5207(6) 0.2357(5) 0.8673(4) 0.0283(14) Uani 1 1 d . . . . .
N25 N 0.0880(5) 0.3664(5) 0.6552(3) 0.0266(13) Uani 1 1 d . . . . .
N8 N 0.3989(5) 0.1181(4) 0.6719(3) 0.0256(13) Uani 1 1 d . . . . .
N35 N 0.4485(6) 0.5691(5) 0.8967(3) 0.0289(14) Uani 1 1 d . . . . .
N44 N 0.5997(5) 0.4375(5) 0.9149(3) 0.0287(14) Uani 1 1 d . . . . .
N19 N 0.1874(6) 0.3183(4) 0.5191(4) 0.0298(14) Uani 1 1 d . . . . .
N51 N 0.1063(6) 0.1207(5) 0.6193(4) 0.0330(16) Uani 1 1 d . . . . .
C36 C 0.5625(7) 0.6089(6) 0.9235(4) 0.0289(17) Uani 1 1 d . . . . .
C7 C 0.4662(7) 0.1073(6) 0.6089(4) 0.0278(16) Uani 1 1 d . . . . .
C37 C 0.6007(7) 0.7119(5) 0.9400(4) 0.0291(17) Uani 1 1 d . . . . .
H37 H 0.5468 0.7569 0.9370 0.035 Uiso 1 1 calc R . . . .
C62 C 0.5459(7) 0.3662(6) 0.7222(4) 0.0326(18) Uani 1 1 d . . . . .
H62 H 0.5720 0.3155 0.7501 0.039 Uiso 1 1 calc R . . . .
C43 C 0.6425(6) 0.5392(6) 0.9317(4) 0.0256(16) Uani 1 1 d . . . . .
C24 C 0.0136(6) 0.3934(5) 0.7068(4) 0.0257(15) Uani 1 1 d . . . . .
C42 C 0.7584(7) 0.5781(6) 0.9533(4) 0.0300(17) Uani 1 1 d . . . . .
H42 H 0.8114 0.5328 0.9598 0.036 Uiso 1 1 calc R . . . .
C29 C 0.1051(7) 0.4799(6) 0.8209(4) 0.0271(16) Uani 1 1 d . . . . .
C21 C 0.0408(7) 0.3848(6) 0.5876(4) 0.0270(16) Uani 1 1 d . . . . .
C58 C 0.4312(8) 0.4945(6) 0.7129(5) 0.038(2) Uani 1 1 d . . . . .
H58 H 0.3775 0.5320 0.7332 0.046 Uiso 1 1 calc R . . . .
C27 C 0.1019(7) 0.2931(6) 0.8026(5) 0.0317(17) Uani 1 1 d . . . . .
H27A H 0.0592 0.2327 0.7797 0.048 Uiso 1 1 calc GR . . . .
H27B H 0.1099 0.2825 0.8550 0.048 Uiso 1 1 calc GR . . . .
H27C H 0.1785 0.3083 0.7811 0.048 Uiso 1 1 calc GR . . . .
C11 C 0.3284(7) 0.2331(5) 0.4558(4) 0.0258(15) Uani 1 1 d . . . . .
C3 C 0.2990(7) 0.1271(6) 0.8114(4) 0.0339(18) Uani 1 1 d . . . . .
H3A H 0.3155 0.1957 0.7938 0.051 Uiso 1 1 calc GR . . . .
H3B H 0.2733 0.1275 0.8619 0.051 Uiso 1 1 calc GR . . . .
H3C H 0.2381 0.0888 0.7810 0.051 Uiso 1 1 calc GR . . . .
C32 C 0.2523(7) 0.5885(6) 0.8636(4) 0.0305(17) Uani 1 1 d . . . . .
C9 C 0.4385(7) 0.1455(6) 0.5397(4) 0.0301(17) Uani 1 1 d . . . . .
H9 H 0.4856 0.1344 0.4998 0.036 Uiso 1 1 calc R . . . .
C34 C 0.3646(7) 0.6256(6) 0.8903(4) 0.0305(17) Uani 1 1 d . . . . .
H34 H 0.3817 0.6938 0.9045 0.037 Uiso 1 1 calc R . . . .
C20 C 0.0919(7) 0.3592(6) 0.5208(4) 0.0311(17) Uani 1 1 d . . . . .
H20 H 0.0560 0.3720 0.4760 0.037 Uiso 1 1 calc R . . . .
C2 C 0.4103(7) 0.0782(5) 0.8073(4) 0.0298(17) Uani 1 1 d . . . . .
C12 C 0.3826(7) 0.2107(6) 0.3909(4) 0.0305(17) Uani 1 1 d . . . . .
H12 H 0.4401 0.1689 0.3932 0.037 Uiso 1 1 calc R . . . .
C40 C 0.7979(7) 0.6803(6) 0.9655(4) 0.0327(18) Uani 1 1 d . . . . .
C26 C 0.0345(6) 0.3826(5) 0.7899(4) 0.0269(16) Uani 1 1 d . . . . .
C45 C 0.6576(7) 0.3637(6) 0.9330(4) 0.0302(17) Uani 1 1 d . . . . .
H45 H 0.7279 0.3795 0.9598 0.036 Uiso 1 1 calc R . . . .
C4 C 0.4555(7) 0.0815(5) 0.7275(4) 0.0307(17) Uani 1 1 d . . . . .
C18 C 0.2411(7) 0.2958(5) 0.4513(4) 0.0273(16) Uani 1 1 d . . . . .
C46 C 0.6176(7) 0.2622(6) 0.9135(4) 0.0314(17) Uani 1 1 d . . . . .
C13 C 0.3545(7) 0.2480(6) 0.3233(4) 0.0323(17) Uani 1 1 d . . . . .
C49 C 0.5066(7) 0.1347(6) 0.8584(4) 0.0312(17) Uani 1 1 d . . . . .
C30 C 0.0588(8) 0.5701(7) 0.8380(5) 0.038(2) Uani 1 1 d . . . . .
H30 H -0.0189 0.5805 0.8325 0.046 Uiso 1 1 calc R . . . .
C38 C 0.7168(7) 0.7492(6) 0.9608(4) 0.0358(19) Uani 1 1 d . . . . .
C61 C 0.5874(8) 0.3834(7) 0.6501(5) 0.046(2) Uani 1 1 d . . . . .
H61 H 0.6395 0.3442 0.6298 0.055 Uiso 1 1 calc R . . . .
C17 C 0.2138(7) 0.3326(6) 0.3824(4) 0.0335(18) Uani 1 1 d . . . . .
H17 H 0.1561 0.3742 0.3793 0.040 Uiso 1 1 calc R . . . .
C31 C 0.1535(8) 0.6395(7) 0.8646(5) 0.042(2) Uani 1 1 d . . . . .
H31 H 0.1522 0.7062 0.8799 0.050 Uiso 1 1 calc R . . . .
C60 C 0.5492(8) 0.4599(7) 0.6096(5) 0.047(2) Uani 1 1 d . . . . .
H60 H 0.5762 0.4732 0.5616 0.057 Uiso 1 1 calc R . . . .
C6 C 0.5622(7) 0.0616(6) 0.6281(5) 0.041(2) Uani 1 1 d . . . . .
H6 H 0.6191 0.0445 0.5961 0.050 Uiso 1 1 calc R . . . .
C1 C 0.3809(8) -0.0331(6) 0.8318(5) 0.039(2) Uani 1 1 d . . . . .
H1A H 0.3653 -0.0352 0.8841 0.059 Uiso 1 1 calc GR . . . .
H1B H 0.4464 -0.0675 0.8218 0.059 Uiso 1 1 calc GR . . . .
H1C H 0.3126 -0.0661 0.8049 0.059 Uiso 1 1 calc GR . . . .
C59 C 0.4714(9) 0.5163(7) 0.6405(5) 0.046(2) Uani 1 1 d . . . . .
H59 H 0.4457 0.5682 0.6138 0.055 Uiso 1 1 calc R . . . .
C22 C -0.0668(7) 0.4225(6) 0.5968(5) 0.0343(18) Uani 1 1 d . . . . .
H22 H -0.1164 0.4400 0.5596 0.041 Uiso 1 1 calc R . . . .
C16 C 0.2695(7) 0.3096(6) 0.3182(4) 0.0316(17) Uani 1 1 d . . . . .
C5 C 0.5575(8) 0.0464(7) 0.7029(5) 0.040(2) Uani 1 1 d . . . . .
H5 H 0.6114 0.0184 0.7319 0.047 Uiso 1 1 calc R . . . .
C47 C 0.6646(9) 0.1743(7) 0.9332(5) 0.047(2) Uani 1 1 d . . . . .
H47 H 0.7299 0.1713 0.9636 0.056 Uiso 1 1 calc R . . . .
C48 C 0.5956(9) 0.0953(7) 0.8991(5) 0.046(2) Uani 1 1 d . . . . .
H48 H 0.6047 0.0273 0.9018 0.055 Uiso 1 1 calc R . . . .
C41 C 0.9246(7) 0.7162(7) 0.9832(5) 0.043(2) Uani 1 1 d . . . . .
H41A H 0.9635 0.6586 0.9919 0.065 Uiso 1 1 calc GR . . . .
H41B H 0.9312 0.7587 1.0269 0.065 Uiso 1 1 calc GR . . . .
H41C H 0.9607 0.7543 0.9422 0.065 Uiso 1 1 calc GR . . . .
C23 C -0.0826(7) 0.4276(6) 0.6725(5) 0.0349(19) Uani 1 1 d . . . . .
H23 H -0.1454 0.4496 0.6964 0.042 Uiso 1 1 calc R . . . .
C14 C 0.4226(9) 0.2237(7) 0.2545(5) 0.044(2) Uani 1 1 d . . . . .
H14A H 0.4875 0.1909 0.2694 0.066 Uiso 1 1 calc GR . . . .
H14B H 0.4518 0.2857 0.2293 0.066 Uiso 1 1 calc GR . . . .
H14C H 0.3712 0.1794 0.2217 0.066 Uiso 1 1 calc GR . . . .
C39 C 0.7514(8) 0.8606(6) 0.9740(5) 0.045(2) Uani 1 1 d . . . . .
H39A H 0.6826 0.8903 0.9847 0.067 Uiso 1 1 calc GR . . . .
H39B H 0.7883 0.8913 0.9304 0.067 Uiso 1 1 calc GR . . . .
H39C H 0.8056 0.8719 1.0153 0.067 Uiso 1 1 calc GR . . . .
C56 C -0.0079(7) 0.1309(8) 0.6191(6) 0.050(2) Uani 1 1 d . . . . .
H56 H -0.0270 0.1947 0.6299 0.060 Uiso 1 1 calc R . . . .
C15 C 0.2403(9) 0.3565(7) 0.2455(5) 0.047(2) Uani 1 1 d . . . . .
H15A H 0.2993 0.4140 0.2353 0.071 Uiso 1 1 calc GR . . . .
H15B H 0.1648 0.3782 0.2488 0.071 Uiso 1 1 calc GR . . . .
H15C H 0.2383 0.3070 0.2061 0.071 Uiso 1 1 calc GR . . . .
N63 N 0.6964(9) 0.1849(8) 0.4305(6) 0.071(3) Uani 1 1 d . . . . .
C64 C 0.7401(12) 0.2766(9) 0.4556(7) 0.080(4) Uani 1 1 d . . . . .
H64 H 0.7360 0.2894 0.5063 0.096 Uiso 1 1 calc R . . . .
C65 C 0.7910(11) 0.3536(9) 0.4119(8) 0.077(4) Uani 1 1 d . . . . .
H65 H 0.8206 0.4169 0.4324 0.093 Uiso 1 1 calc R . . . .
C66 C 0.7977(11) 0.3363(8) 0.3373(7) 0.065(3) Uani 1 1 d . . . . .
H66 H 0.8336 0.3869 0.3061 0.078 Uiso 1 1 calc R . . . .
C67 C 0.7507(12) 0.2434(9) 0.3098(7) 0.077(4) Uani 1 1 d . . . . .
H67 H 0.7530 0.2287 0.2593 0.092 Uiso 1 1 calc R . . . .
C68 C 0.6999(11) 0.1721(8) 0.3582(7) 0.063(3) Uani 1 1 d . . . . .
H68 H 0.6651 0.1096 0.3385 0.075 Uiso 1 1 calc R . . . .
C28 C -0.0856(7) 0.3584(7) 0.8285(5) 0.040(2) Uani 1 1 d . . . . .
H28A H -0.1286 0.4139 0.8218 0.060 Uiso 1 1 calc GR . . . .
H28B H -0.0732 0.3488 0.8806 0.060 Uiso 1 1 calc GR . . . .
H28C H -0.1297 0.2975 0.8072 0.060 Uiso 1 1 calc GR . . . .
C52 C 0.1314(9) 0.0273(7) 0.6055(6) 0.049(2) Uani 1 1 d . . . . .
H52 H 0.2099 0.0181 0.6058 0.059 Uiso 1 1 calc R . . . .
C53 C 0.0451(10) -0.0561(8) 0.5908(6) 0.060(3) Uani 1 1 d . . . . .
H53 H 0.0652 -0.1198 0.5809 0.072 Uiso 1 1 calc R . . . .
C55 C -0.0981(9) 0.0526(9) 0.6039(8) 0.070(4) Uani 1 1 d . . . . .
H55 H -0.1757 0.0643 0.6022 0.084 Uiso 1 1 calc R . . . .
C54 C -0.0727(11) -0.0421(11) 0.5912(6) 0.076(4) Uani 1 1 d . . . . .
H54 H -0.1326 -0.0968 0.5829 0.091 Uiso 1 1 calc R . . . .
N69 N 1.0121(12) 1.0243(10) 0.8975(8) 0.112(3) Uani 1 1 d D U . . .
C70 C 0.9262(12) 1.0589(11) 0.8627(8) 0.099(3) Uani 1 1 d D U . . .
H70 H 0.9027 1.1193 0.8782 0.118 Uiso 1 1 calc R . . . .
C71 C 0.8729(14) 1.0068(11) 0.8049(8) 0.105(3) Uani 1 1 d D U . . .
H71 H 0.8091 1.0293 0.7818 0.126 Uiso 1 1 calc R . . . .
C72 C 0.9106(13) 0.9210(11) 0.7793(9) 0.105(3) Uani 1 1 d D U . . .
H72 H 0.8735 0.8854 0.7386 0.126 Uiso 1 1 calc R . . . .
C73 C 1.0044(13) 0.8879(12) 0.8145(8) 0.106(3) Uani 1 1 d D U . . .
H73 H 1.0327 0.8299 0.7982 0.127 Uiso 1 1 calc R . . . .
C74 C 1.0535(15) 0.9430(11) 0.8733(9) 0.107(4) Uani 1 1 d D U . . .
H74 H 1.1180 0.9233 0.8975 0.129 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
Pb1 N10 2.420(6) . ?
Pb1 N25 2.664(6) . ?
Pb1 N8 2.743(6) . ?
Pb1 N19 2.418(6) . ?
Pb1 N51 2.459(6) . ?
Pb2 N57 2.505(6) . ?
Pb2 N33 2.750(6) . ?
Pb2 N50 2.671(6) . ?
Pb2 N35 2.417(6) . ?
Pb2 N44 2.407(6) . ?
N10 C11 1.426(9) . ?
N10 C9 1.294(9) . ?
N57 C62 1.378(9) . ?
N57 C58 1.325(10) . ?
N33 C29 1.322(9) . ?
N33 C32 1.385(10) . ?
N50 C46 1.380(10) . ?
N50 C49 1.336(9) . ?
N25 C24 1.354(9) . ?
N25 C21 1.367(9) . ?
N8 C7 1.398(9) . ?
N8 C4 1.325(10) . ?
N35 C36 1.411(10) . ?
N35 C34 1.319(9) . ?
N44 C43 1.395(10) . ?
N44 C45 1.314(9) . ?
N19 C20 1.302(9) . ?
N19 C18 1.424(9) . ?
N51 C56 1.341(10) . ?
N51 C52 1.342(11) . ?
C36 C37 1.400(11) . ?
C36 C43 1.413(10) . ?
C7 C9 1.401(11) . ?
C7 C6 1.385(10) . ?
C37 H37 0.9300 . ?
C37 C38 1.394(11) . ?
C62 H62 0.9300 . ?
C62 C61 1.395(11) . ?
C43 C42 1.401(10) . ?
C24 C26 1.522(10) . ?
C24 C23 1.400(10) . ?
C42 H42 0.9300 . ?
C42 C40 1.379(11) . ?
C29 C26 1.513(11) . ?
C29 C30 1.422(10) . ?
C21 C20 1.409(10) . ?
C21 C22 1.418(10) . ?
C58 H58 0.9300 . ?
C58 C59 1.405(12) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 C26 1.538(10) . ?
C11 C12 1.381(10) . ?
C11 C18 1.407(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C2 1.528(10) . ?
C32 C34 1.387(11) . ?
C32 C31 1.413(10) . ?
C9 H9 0.9300 . ?
C34 H34 0.9300 . ?
C20 H20 0.9300 . ?
C2 C4 1.532(11) . ?
C2 C49 1.529(11) . ?
C2 C1 1.538(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.373(11) . ?
C40 C38 1.410(12) . ?
C40 C41 1.490(11) . ?
C26 C28 1.544(10) . ?
C45 H45 0.9300 . ?
C45 C46 1.396(11) . ?
C4 C5 1.405(11) . ?
C18 C17 1.389(11) . ?
C46 C47 1.413(11) . ?
C13 C16 1.376(10) . ?
C13 C14 1.532(11) . ?
C49 C48 1.421(11) . ?
C30 H30 0.9300 . ?
C30 C31 1.390(12) . ?
C38 C39 1.490(12) . ?
C61 H61 0.9300 . ?
C61 C60 1.382(13) . ?
C17 H17 0.9300 . ?
C17 C16 1.383(11) . ?
C31 H31 0.9300 . ?
C60 H60 0.9300 . ?
C60 C59 1.375(13) . ?
C6 H6 0.9300 . ?
C6 C5 1.363(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C59 H59 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.379(12) . ?
C16 C15 1.512(11) . ?
C5 H5 0.9300 . ?
C47 H47 0.9300 . ?
C47 C48 1.351(13) . ?
C48 H48 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C23 H23 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C56 H56 0.9300 . ?
C56 C55 1.372(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N63 C64 1.319(14) . ?
N63 C68 1.312(14) . ?
C64 H64 0.9300 . ?
C64 C65 1.360(17) . ?
C65 H65 0.9300 . ?
C65 C66 1.365(17) . ?
C66 H66 0.9300 . ?
C66 C67 1.355(16) . ?
C67 H67 0.9300 . ?
C67 C68 1.360(16) . ?
C68 H68 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C52 H52 0.9300 . ?
C52 C53 1.389(13) . ?
C53 H53 0.9300 . ?
C53 C54 1.396(16) . ?
C55 H55 0.9300 . ?
C55 C54 1.357(16) . ?
C54 H54 0.9300 . ?
N69 C70 1.309(8) . ?
N69 C74 1.323(8) . ?
C70 H70 0.9300 . ?
C70 C71 1.332(8) . ?
C71 H71 0.9300 . ?
C71 C72 1.363(8) . ?
C72 H72 0.9300 . ?
C72 C73 1.379(8) . ?
C73 H73 0.9300 . ?
C73 C74 1.349(8) . ?
C74 H74 0.9300 . ?

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
N10 Pb1 N25 134.67(19) . . ?
N10 Pb1 N8 67.53(19) . . ?
N10 Pb1 N51 85.6(2) . . ?
N25 Pb1 N8 152.33(18) . . ?
N19 Pb1 N10 67.8(2) . . ?
N19 Pb1 N25 67.40(19) . . ?
N19 Pb1 N8 134.21(19) . . ?
N19 Pb1 N51 82.8(2) . . ?
N51 Pb1 N25 82.1(2) . . ?
N51 Pb1 N8 84.15(19) . . ?
N57 Pb2 N33 82.8(2) . . ?
N57 Pb2 N50 81.0(2) . . ?
N50 Pb2 N33 151.31(19) . . ?
N35 Pb2 N57 82.9(2) . . ?
N35 Pb2 N33 67.3(2) . . ?
N35 Pb2 N50 133.2(2) . . ?
N44 Pb2 N57 83.1(2) . . ?
N44 Pb2 N33 133.8(2) . . ?
N44 Pb2 N50 67.2(2) . . ?
N44 Pb2 N35 67.4(2) . . ?
C11 N10 Pb1 118.2(4) . . ?
C9 N10 Pb1 116.8(5) . . ?
C9 N10 C11 122.7(6) . . ?
C62 N57 Pb2 120.3(5) . . ?
C58 N57 Pb2 121.1(5) . . ?
C58 N57 C62 118.6(7) . . ?
C29 N33 Pb2 143.2(5) . . ?
C29 N33 C32 106.8(6) . . ?
C32 N33 Pb2 104.7(5) . . ?
C46 N50 Pb2 105.0(4) . . ?
C49 N50 Pb2 140.9(5) . . ?
C49 N50 C46 106.6(6) . . ?
C24 N25 Pb1 143.7(5) . . ?
C24 N25 C21 106.2(6) . . ?
C21 N25 Pb1 108.9(4) . . ?
C7 N8 Pb1 104.5(4) . . ?
C4 N8 Pb1 143.7(5) . . ?
C4 N8 C7 105.4(6) . . ?
C36 N35 Pb2 118.7(5) . . ?
C34 N35 Pb2 118.2(5) . . ?
C34 N35 C36 122.2(7) . . ?
C43 N44 Pb2 119.8(4) . . ?
C45 N44 Pb2 115.9(5) . . ?
C45 N44 C43 122.2(7) . . ?
C20 N19 Pb1 118.8(5) . . ?
C20 N19 C18 122.3(7) . . ?
C18 N19 Pb1 118.6(5) . . ?
C56 N51 Pb1 123.2(6) . . ?
C56 N51 C52 117.0(8) . . ?
C52 N51 Pb1 119.7(5) . . ?
N35 C36 C43 116.7(7) . . ?
C37 C36 N35 124.1(7) . . ?
C37 C36 C43 119.1(7) . . ?
N8 C7 C9 121.8(7) . . ?
C6 C7 N8 109.8(7) . . ?
C6 C7 C9 128.3(7) . . ?
C36 C37 H37 118.9 . . ?
C38 C37 C36 122.2(8) . . ?
C38 C37 H37 118.9 . . ?
N57 C62 H62 119.1 . . ?
N57 C62 C61 121.8(8) . . ?
C61 C62 H62 119.1 . . ?
N44 C43 C36 116.7(7) . . ?
N44 C43 C42 125.5(7) . . ?
C42 C43 C36 117.7(7) . . ?
N25 C24 C26 122.4(6) . . ?
N25 C24 C23 110.6(7) . . ?
C23 C24 C26 127.0(7) . . ?
C43 C42 H42 118.4 . . ?
C40 C42 C43 123.2(7) . . ?
C40 C42 H42 118.4 . . ?
N33 C29 C26 123.3(6) . . ?
N33 C29 C30 111.5(7) . . ?
C30 C29 C26 125.2(7) . . ?
N25 C21 C20 121.6(7) . . ?
N25 C21 C22 110.4(7) . . ?
C20 C21 C22 127.8(7) . . ?
N57 C58 H58 119.0 . . ?
N57 C58 C59 122.1(8) . . ?
C59 C58 H58 119.0 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
C12 C11 N10 124.8(7) . . ?
C12 C11 C18 118.1(7) . . ?
C18 C11 N10 117.1(6) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
N33 C32 C34 123.5(7) . . ?
N33 C32 C31 109.7(7) . . ?
C34 C32 C31 126.7(8) . . ?
N10 C9 C7 124.9(7) . . ?
N10 C9 H9 117.5 . . ?
C7 C9 H9 117.5 . . ?
N35 C34 C32 123.3(7) . . ?
N35 C34 H34 118.4 . . ?
C32 C34 H34 118.4 . . ?
N19 C20 C21 122.6(7) . . ?
N19 C20 H20 118.7 . . ?
C21 C20 H20 118.7 . . ?
C3 C2 C4 110.0(6) . . ?
C3 C2 C49 110.5(6) . . ?
C3 C2 C1 108.9(7) . . ?
C4 C2 C1 109.3(6) . . ?
C49 C2 C4 108.9(6) . . ?
C49 C2 C1 109.2(7) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 C11 122.3(7) . . ?
C13 C12 H12 118.8 . . ?
C42 C40 C38 119.0(7) . . ?
C42 C40 C41 119.8(8) . . ?
C38 C40 C41 121.2(8) . . ?
C24 C26 C27 109.1(6) . . ?
C24 C26 C28 108.9(6) . . ?
C29 C26 C24 109.8(6) . . ?
C29 C26 C27 110.0(6) . . ?
C29 C26 C28 110.8(6) . . ?
C27 C26 C28 108.2(6) . . ?
N44 C45 H45 118.8 . . ?
N44 C45 C46 122.4(7) . . ?
C46 C45 H45 118.8 . . ?
N8 C4 C2 122.4(7) . . ?
N8 C4 C5 111.3(7) . . ?
C5 C4 C2 126.3(7) . . ?
C11 C18 N19 116.8(7) . . ?
C17 C18 N19 124.4(7) . . ?
C17 C18 C11 118.8(7) . . ?
N50 C46 C45 121.2(7) . . ?
N50 C46 C47 109.8(7) . . ?
C45 C46 C47 129.0(8) . . ?
C12 C13 C16 120.2(7) . . ?
C12 C13 C14 119.2(7) . . ?
C16 C13 C14 120.6(7) . . ?
N50 C49 C2 121.4(6) . . ?
N50 C49 C48 109.7(8) . . ?
C48 C49 C2 128.8(7) . . ?
C29 C30 H30 127.1 . . ?
C31 C30 C29 105.8(7) . . ?
C31 C30 H30 127.1 . . ?
C37 C38 C40 118.5(8) . . ?
C37 C38 C39 118.8(8) . . ?
C40 C38 C39 122.6(8) . . ?
C62 C61 H61 120.8 . . ?
C60 C61 C62 118.5(8) . . ?
C60 C61 H61 120.8 . . ?
C18 C17 H17 118.9 . . ?
C16 C17 C18 122.2(7) . . ?
C16 C17 H17 118.9 . . ?
C32 C31 H31 126.9 . . ?
C30 C31 C32 106.2(7) . . ?
C30 C31 H31 126.9 . . ?
C61 C60 H60 120.1 . . ?
C59 C60 C61 119.8(9) . . ?
C59 C60 H60 120.1 . . ?
C7 C6 H6 126.5 . . ?
C5 C6 C7 106.9(7) . . ?
C5 C6 H6 126.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C58 C59 H59 120.4 . . ?
C60 C59 C58 119.2(8) . . ?
C60 C59 H59 120.4 . . ?
C21 C22 H22 127.2 . . ?
C23 C22 C21 105.6(7) . . ?
C23 C22 H22 127.2 . . ?
C13 C16 C17 118.5(7) . . ?
C13 C16 C15 121.8(7) . . ?
C17 C16 C15 119.7(7) . . ?
C4 C5 H5 126.7 . . ?
C6 C5 C4 106.5(7) . . ?
C6 C5 H5 126.7 . . ?
C46 C47 H47 126.9 . . ?
C48 C47 C46 106.1(8) . . ?
C48 C47 H47 126.9 . . ?
C49 C48 H48 126.1 . . ?
C47 C48 C49 107.8(8) . . ?
C47 C48 H48 126.1 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C24 C23 H23 126.4 . . ?
C22 C23 C24 107.3(7) . . ?
C22 C23 H23 126.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N51 C56 H56 118.1 . . ?
N51 C56 C55 123.8(10) . . ?
C55 C56 H56 118.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C68 N63 C64 115.6(10) . . ?
N63 C64 H64 118.0 . . ?
N63 C64 C65 123.9(12) . . ?
C65 C64 H64 118.0 . . ?
C64 C65 H65 120.5 . . ?
C64 C65 C66 118.9(10) . . ?
C66 C65 H65 120.5 . . ?
C65 C66 H66 120.9 . . ?
C67 C66 C65 118.3(11) . . ?
C67 C66 H66 120.9 . . ?
C66 C67 H67 120.9 . . ?
C66 C67 C68 118.2(12) . . ?
C68 C67 H67 120.9 . . ?
N63 C68 C67 125.0(11) . . ?
N63 C68 H68 117.5 . . ?
C67 C68 H68 117.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N51 C52 H52 118.7 . . ?
N51 C52 C53 122.7(9) . . ?
C53 C52 H52 118.7 . . ?
C52 C53 H53 120.8 . . ?
C52 C53 C54 118.5(10) . . ?
C54 C53 H53 120.8 . . ?
C56 C55 H55 120.4 . . ?
C54 C55 C56 119.2(10) . . ?
C54 C55 H55 120.4 . . ?
C53 C54 H54 120.6 . . ?
C55 C54 C53 118.9(11) . . ?
C55 C54 H54 120.6 . . ?
C70 N69 C74 121.6(16) . . ?
N69 C70 H70 120.3 . . ?
N69 C70 C71 119.5(16) . . ?
C71 C70 H70 120.3 . . ?
C70 C71 H71 119.6 . . ?
C70 C71 C72 120.8(17) . . ?
C72 C71 H71 119.6 . . ?
C71 C72 H72 120.5 . . ?
C71 C72 C73 119.1(16) . . ?
C73 C72 H72 120.5 . . ?
C72 C73 H73 121.4 . . ?
C74 C73 C72 117.3(16) . . ?
C74 C73 H73 121.4 . . ?
N69 C74 C73 121.6(17) . . ?
N69 C74 H74 119.2 . . ?
C73 C74 H74 119.2 . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
16 0 2 0.1192 16.0000 0.0000 2.0000 0.8485 -0.1920 0.5002
-16 0 -2 0.1192 -16.0000 -0.0000 -2.0000 -0.8485 0.1920 -0.5002
0 19 0 0.1759 -0.0000 19.0000 0.0001 0.6251 -0.1625 -0.7961
0 -19 0 0.1759 0.0000 -19.0000 -0.0001 -0.6251 0.1625 0.7961
-1 -1 25 0.0230 -1.0000 -0.9999 25.0000 0.2171 0.9629 0.0415
1 1 -25 0.0230 1.0000 0.9999 -25.0000 -0.2171 -0.9629 -0.0415
-11 -12 -1 0.1045 -11.0000 -12.0000 -1.0001 -0.9736 0.2487 0.1594
11 12 1 0.1045 11.0000 12.0000 1.0001 0.9736 -0.2487 -0.1594

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT112_UO2PbLAthf          
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.      a/2         96 %Fit  
RESPONSE: Two structures in the asymmetric unit have different bond parameters. See Manuscript Table 1.
;
_vrf_PLAT342_UO2PbLMethf         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02016 Ang.  
RESPONSE: Poor quality twinned data
;
_vrf_PLAT342_UO2PbLMepy          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03146 Ang.  
RESPONSE: Poor Quality data cut at 0.9A
;
# 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_UO2SnLAthf
_database_code_depnum_ccdc_archive 'CCDC 1480064'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H64 N8 O4 Sn U, C4 H8 O'
_chemical_formula_sum            'C70 H71 N8 O5 Sn U'
_chemical_formula_weight         1461.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H70 U Sn N8 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'
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'
Sn Sn -0.6537 1.4246 '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                   11.4369(2)
_cell_length_b                   22.3418(4)
_cell_length_c                   24.1875(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.5479(16)
_cell_angle_gamma                90
_cell_volume                     6126.84(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29780
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.0400
_cell_measurement_theta_min      3.0530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.307
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -22 -21 0.1500
5 22 21 0.1500
0 6 -33 0.1229
0 -6 33 0.1229
15 -10 -6 0.1311
-15 10 6 0.1311

_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.246
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
-4.9840 -21.9852 -20.9775 0.1528 0.6306 0.7750
4.9840 21.9852 20.9775 -0.1528 -0.6306 -0.7750
0.0120 6.0189 -32.9742 0.2295 0.9532 -0.1615
-0.0120 -6.0189 32.9742 -0.2295 -0.9532 0.1615
14.9795 -9.9930 -5.9911 -0.9572 0.2185 -0.0293
-14.9795 9.9930 5.9911 0.9572 -0.2185 0.0293

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            135432
_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         27.103
_diffrn_reflns_theta_min         2.939
_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    -47.00  43.00   1.00   30.00    --   21.95 -57.00 -30.00   90
  2  ω     -8.00  92.00   1.00   30.00    --   21.95  77.00-150.00  100
  3  ω      1.00  91.00   1.00   30.00    --   21.95  57.00 -30.00   90
  4  ω    -50.00  47.00   1.00   30.00    --   21.95 -38.00  60.00   97
  5  ω     -8.00  92.00   1.00   30.00    --   21.95  77.00  90.00  100
  6  ω    -95.00 -34.00   1.00   30.00    --  -19.30-179.00-180.00   61
  7  ω    -95.00 -34.00   1.00   30.00    --  -19.30-179.00 -30.00   61
  8  ω      1.00  91.00   1.00   30.00    --   21.95  57.00  60.00   90
  9  ω      5.00  87.00   1.00   30.00    --   21.95-137.00  48.00   82
 10  ω      2.00  84.00   1.00   30.00    --   21.95-133.00-134.00   82
 11  ω    -47.00  43.00   1.00   30.00    --   21.95 -57.00-180.00   90
 12  ω     34.00  98.00   1.00   30.00    --   21.95 179.00   0.00   64
 13  ω     34.00  98.00   1.00   30.00    --   21.95 179.00 -60.00   64
 14  ω     -4.00  32.00   1.00   30.00    --   21.95  38.00-150.00   36
;
_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      -0.0585147000
_diffrn_orient_matrix_UB_12      0.0110521000
_diffrn_orient_matrix_UB_13      -0.0049626000
_diffrn_orient_matrix_UB_21      0.0020411000
_diffrn_orient_matrix_UB_22      -0.0013334000
_diffrn_orient_matrix_UB_23      -0.0291494000
_diffrn_orient_matrix_UB_31      -0.0220138000
_diffrn_orient_matrix_UB_32      -0.0297451000
_diffrn_orient_matrix_UB_33      -0.0005401000
_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                11216
_reflns_number_total             13495
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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         1.518
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13495
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      0.912
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1232
_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. Uiso/Uaniso restraints and constraints
C59 \\sim C60 \\sim C61 \\sim C62 \\sim O3: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
O5 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C59, O3, C62, C61, C60
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B), C33(H33A,H33B), C59(H59A,
 H59B), C63(H63A,H63B), C64(H64A,H64B), C31(H31A,H31B), C4(H4A,H4B), C60(H60A,
 H60B), C70(H70A,H70B), C61(H61A,H61B), C68(H68A,H68B), C67(H67A,H67B),
 C69(H69A,H69B), C2(H2A,H2B), C2A(H2AA,H2AB)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C54(H54), C46(H46), C25(H25), C23(H23), C56(H56), C22(H22),
 C10(H10), C52(H52), C28(H28), C20(H20), C36(H36), C49(H49), C27(H27), C21(H21),
  C51(H51), C50(H50), C39(H39), C14(H14), C42(H42), C43(H43), C12(H12),
 C13(H13), C41(H41), C57(H57), C8(H8), C37(H37), C7(H7)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C),
 C3A(H3AA,H3AB,H3AC)
;
_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 0.86265(2) 0.37970(2) 0.55787(2) 0.02551(7) Uani 1 1 d . . . . .
Sn1 Sn 0.75694(3) 0.16530(2) 0.53316(2) 0.02906(9) Uani 1 1 d . . . . .
O1 O 0.8467(3) 0.30045(15) 0.55956(13) 0.0354(8) Uani 1 1 d . . . . .
O3 O 0.8763(3) 0.37640(15) 0.45648(14) 0.0381(8) Uani 1 1 d . U . . .
O2 O 0.8805(3) 0.45843(15) 0.55077(14) 0.0365(8) Uani 1 1 d . . . . .
O4 O 0.7538(3) 0.07441(15) 0.48619(13) 0.0343(7) Uani 1 1 d . . . . .
N5 N 0.8405(4) 0.11014(16) 0.60356(15) 0.0285(8) Uani 1 1 d . . . . .
N6 N 0.9946(3) 0.13711(17) 0.52253(16) 0.0289(8) Uani 1 1 d . . . . .
N3 N 0.6490(4) 0.38666(17) 0.51564(17) 0.0306(8) Uani 1 1 d . . . . .
N4 N 0.7261(4) 0.38688(17) 0.62804(16) 0.0331(9) Uani 1 1 d . . . . .
N2 N 1.0836(3) 0.36124(18) 0.55502(18) 0.0340(9) Uani 1 1 d . . . . .
N8 N 0.5983(3) 0.13774(17) 0.57115(16) 0.0301(8) Uani 1 1 d . . . . .
N7 N 0.5448(3) 0.17335(17) 0.45555(17) 0.0340(9) Uani 1 1 d . . . . .
N1 N 0.9754(4) 0.38707(17) 0.65129(17) 0.0371(10) Uani 1 1 d . . . . .
C47 C 0.5666(4) 0.3602(2) 0.41827(18) 0.0257(9) Uani 1 1 d . . . . .
C53 C 0.6039(4) 0.4040(2) 0.46021(19) 0.0302(9) Uani 1 1 d . . . . .
C17 C 1.1002(4) 0.2483(2) 0.49271(19) 0.0291(9) Uani 1 1 d . . . . .
H17 H 1.0617 0.2473 0.5252 0.035 Uiso 1 1 calc R . . . .
C54 C 0.5734(4) 0.3729(2) 0.5504(2) 0.0334(10) Uani 1 1 d . . . . .
H54 H 0.4931 0.3654 0.5366 0.040 Uiso 1 1 calc R . . . .
C55 C 0.6119(5) 0.3693(2) 0.6080(2) 0.0374(11) Uani 1 1 d . . . . .
C24 C 1.0607(4) 0.1395(2) 0.47725(19) 0.0282(9) Uani 1 1 d . . . . .
C45 C 0.5229(4) 0.2571(2) 0.38815(18) 0.0277(9) Uani 1 1 d . . . . .
C46 C 0.5618(4) 0.2988(2) 0.42948(18) 0.0285(9) Uani 1 1 d . . . . .
H46 H 0.5858 0.2851 0.4664 0.034 Uiso 1 1 calc R . . . .
C11 C 1.1449(4) 0.3575(2) 0.5074(2) 0.0347(10) Uani 1 1 d . . . . .
C25 C 1.0219(4) 0.0974(2) 0.56077(19) 0.0309(9) Uani 1 1 d . . . . .
H25 H 1.0926 0.0753 0.5602 0.037 Uiso 1 1 calc R . . . .
C26 C 0.9519(4) 0.08520(19) 0.60349(18) 0.0284(9) Uani 1 1 d . . . . .
C58 C 0.7332(5) 0.3871(2) 0.6848(2) 0.0404(12) Uani 1 1 d . . . . .
C29 C 0.8011(4) 0.09208(19) 0.65174(17) 0.0279(9) Uani 1 1 d . . . . .
C16 C 1.1498(4) 0.3026(2) 0.47692(19) 0.0305(10) Uani 1 1 d . . . . .
C38 C 0.4860(4) 0.1513(2) 0.5442(2) 0.0406(12) Uani 1 1 d . . . . .
C23 C 1.0775(4) 0.0885(2) 0.4470(2) 0.0344(10) Uani 1 1 d . . . . .
H23 H 1.0496 0.0511 0.4586 0.041 Uiso 1 1 calc R . . . .
C6 C 0.9561(5) 0.4022(2) 0.7036(2) 0.0440(13) Uani 1 1 d . . . . .
C30 C 0.6879(5) 0.1139(2) 0.6712(2) 0.0335(11) Uani 1 1 d . . . . .
C56 C 0.5473(5) 0.3574(3) 0.6530(3) 0.0500(14) Uani 1 1 d . . . . .
H56 H 0.4681 0.3440 0.6510 0.060 Uiso 1 1 calc R . . . .
C22 C 1.1360(4) 0.0912(2) 0.3987(2) 0.0374(11) Uani 1 1 d . . . . .
H22 H 1.1470 0.0556 0.3785 0.045 Uiso 1 1 calc R . . . .
C10 C 1.1463(5) 0.3756(2) 0.6028(2) 0.0425(13) Uani 1 1 d . . . . .
H10 H 1.2296 0.3781 0.6043 0.051 Uiso 1 1 calc R . . . .
C62 C 0.8614(5) 0.3248(3) 0.4198(2) 0.0465(12) Uani 1 1 d . U . . .
H62A H 0.7854 0.3046 0.4228 0.056 Uiso 1 1 calc R . . . .
H62B H 0.9263 0.2958 0.4294 0.056 Uiso 1 1 calc R . . . .
C52 C 0.6013(5) 0.4637(2) 0.4468(2) 0.0399(11) Uani 1 1 d . . . . .
H52 H 0.6249 0.4922 0.4751 0.048 Uiso 1 1 calc R . . . .
C44 C 0.4882(4) 0.2772(2) 0.33176(19) 0.0322(10) Uani 1 1 d . . . . .
C35 C 0.5860(5) 0.1245(2) 0.6250(2) 0.0349(11) Uani 1 1 d . . . . .
C9 C 1.0965(6) 0.3873(3) 0.6513(3) 0.0488(14) Uani 1 1 d . . . . .
C28 C 0.8872(4) 0.0568(2) 0.68226(19) 0.0360(11) Uani 1 1 d . . . . .
H28 H 0.8821 0.0390 0.7175 0.043 Uiso 1 1 calc R . . . .
C19 C 1.1637(4) 0.1977(2) 0.41200(19) 0.0304(10) Uani 1 1 d . . . . .
C18 C 1.1067(4) 0.1957(2) 0.46147(19) 0.0284(9) Uani 1 1 d . . . . .
C15 C 1.2081(4) 0.3033(2) 0.4281(2) 0.0332(10) Uani 1 1 d . . . . .
C20 C 1.2118(4) 0.2520(2) 0.3970(2) 0.0345(10) Uani 1 1 d . . . . .
H20 H 1.2486 0.2534 0.3640 0.041 Uiso 1 1 calc R . . . .
C36 C 0.4674(6) 0.1298(3) 0.6327(3) 0.0504(15) Uani 1 1 d . . . . .
H36 H 0.4348 0.1231 0.6663 0.060 Uiso 1 1 calc R . . . .
C65 C 0.6801(5) 0.0252(3) 0.4023(2) 0.0481(13) Uani 1 1 d . . . . .
H65A H 0.7303 -0.0098 0.3966 0.058 Uiso 1 1 calc R . . . .
H65B H 0.6328 0.0358 0.3664 0.058 Uiso 1 1 calc R . . . .
C49 C 0.4940(4) 0.3386(2) 0.32048(19) 0.0335(10) Uani 1 1 d . . . . .
H49 H 0.4724 0.3522 0.2833 0.040 Uiso 1 1 calc R . . . .
C34 C 0.6208(5) 0.0059(3) 0.6905(2) 0.0483(13) Uani 1 1 d . . . . .
H34A H 0.5511 0.0075 0.6623 0.072 Uiso 1 1 calc GR . . . .
H34B H 0.6054 -0.0210 0.7208 0.072 Uiso 1 1 calc GR . . . .
H34C H 0.6883 -0.0091 0.6735 0.072 Uiso 1 1 calc GR . . . .
C40 C 0.5128(4) 0.1938(2) 0.4006(2) 0.0319(10) Uani 1 1 d . . . . .
C48 C 0.5306(4) 0.3806(2) 0.3621(2) 0.0310(10) Uani 1 1 d . . . . .
C66 C 0.7531(4) 0.0773(2) 0.4261(2) 0.0396(11) Uani 1 1 d . . . . .
H66A H 0.8344 0.0745 0.4165 0.047 Uiso 1 1 calc R . . . .
H66B H 0.7179 0.1155 0.4113 0.047 Uiso 1 1 calc R . . . .
C33 C 0.6481(5) 0.0681(2) 0.7138(2) 0.0402(12) Uani 1 1 d . . . . .
H33A H 0.7112 0.0650 0.7458 0.048 Uiso 1 1 calc R . . . .
H33B H 0.5770 0.0840 0.7280 0.048 Uiso 1 1 calc R . . . .
C27 C 0.9807(5) 0.0524(2) 0.6520(2) 0.0381(11) Uani 1 1 d . . . . .
H27 H 1.0518 0.0308 0.6625 0.046 Uiso 1 1 calc R . . . .
C59 C 0.9015(6) 0.4298(3) 0.4249(2) 0.0542(13) Uani 1 1 d . U . . .
H59A H 0.9739 0.4501 0.4425 0.065 Uiso 1 1 calc R . . . .
H59B H 0.8349 0.4584 0.4220 0.065 Uiso 1 1 calc R . . . .
C21 C 1.1762(4) 0.1438(2) 0.3811(2) 0.0383(11) Uani 1 1 d . . . . .
H21 H 1.2130 0.1451 0.3482 0.046 Uiso 1 1 calc R . . . .
C51 C 0.5645(5) 0.4836(2) 0.3920(2) 0.0437(12) Uani 1 1 d . . . . .
H51 H 0.5625 0.5253 0.3840 0.052 Uiso 1 1 calc R . . . .
C50 C 0.5317(4) 0.4431(2) 0.3502(2) 0.0383(11) Uani 1 1 d . . . . .
H50 H 0.5096 0.4568 0.3131 0.046 Uiso 1 1 calc R . . . .
C39 C 0.4645(4) 0.1688(2) 0.4870(2) 0.0389(11) Uani 1 1 d . . . . .
H39 H 0.3857 0.1776 0.4716 0.047 Uiso 1 1 calc R . . . .
C14 C 1.2621(4) 0.3579(2) 0.4119(2) 0.0420(12) Uani 1 1 d . . . . .
H14 H 1.3009 0.3588 0.3795 0.050 Uiso 1 1 calc R . . . .
C63 C 0.6836(5) 0.0240(2) 0.5001(2) 0.0400(11) Uani 1 1 d . . . . .
H63A H 0.6395 0.0339 0.5315 0.048 Uiso 1 1 calc R . . . .
H63B H 0.7339 -0.0114 0.5104 0.048 Uiso 1 1 calc R . . . .
C1 C 0.8377(6) 0.4139(2) 0.7219(2) 0.0493(15) Uani 1 1 d . . . . .
C42 C 0.4392(5) 0.1757(2) 0.3029(2) 0.0426(12) Uani 1 1 d . . . . .
H42 H 0.4106 0.1479 0.2746 0.051 Uiso 1 1 calc R . . . .
C43 C 0.4480(4) 0.2346(2) 0.2897(2) 0.0383(11) Uani 1 1 d . . . . .
H43 H 0.4273 0.2473 0.2522 0.046 Uiso 1 1 calc R . . . .
C64 C 0.6005(5) 0.0126(3) 0.4475(2) 0.0471(13) Uani 1 1 d . . . . .
H64A H 0.5322 0.0401 0.4443 0.057 Uiso 1 1 calc R . . . .
H64B H 0.5718 -0.0293 0.4457 0.057 Uiso 1 1 calc R . . . .
C31 C 0.7141(6) 0.1745(2) 0.7032(2) 0.0442(13) Uani 1 1 d . . . . .
H31A H 0.6441 0.1855 0.7212 0.053 Uiso 1 1 calc R . . . .
H31B H 0.7806 0.1682 0.7332 0.053 Uiso 1 1 calc R . . . .
C12 C 1.1983(5) 0.4080(2) 0.4909(3) 0.0457(13) Uani 1 1 d . . . . .
H12 H 1.1955 0.4437 0.5120 0.055 Uiso 1 1 calc R . . . .
C13 C 1.2570(5) 0.4083(3) 0.4436(3) 0.0526(15) Uani 1 1 d . . . . .
H13 H 1.2938 0.4440 0.4334 0.063 Uiso 1 1 calc R . . . .
C41 C 0.4723(4) 0.1552(2) 0.3586(2) 0.0371(11) Uani 1 1 d . . . . .
H41 H 0.4661 0.1138 0.3666 0.045 Uiso 1 1 calc R . . . .
C57 C 0.6260(6) 0.3700(3) 0.7011(2) 0.0540(16) Uani 1 1 d . . . . .
H57 H 0.6091 0.3672 0.7385 0.065 Uiso 1 1 calc R . . . .
C32 C 0.7443(6) 0.2268(2) 0.6671(2) 0.0548(16) Uani 1 1 d . . . . .
H32A H 0.6758 0.2365 0.6398 0.082 Uiso 1 1 calc GR . . . .
H32B H 0.8109 0.2158 0.6476 0.082 Uiso 1 1 calc GR . . . .
H32C H 0.7656 0.2617 0.6908 0.082 Uiso 1 1 calc GR . . . .
C8 C 1.1546(7) 0.4026(4) 0.7032(3) 0.0693(19) Uani 1 1 d . . . . .
H8 H 1.2374 0.4063 0.7135 0.083 Uiso 1 1 calc R . . . .
C37 C 0.4063(5) 0.1467(3) 0.5814(3) 0.0540(15) Uani 1 1 d . . . . .
H37 H 0.3238 0.1538 0.5737 0.065 Uiso 1 1 calc R . . . .
C7 C 1.0662(6) 0.4117(3) 0.7373(3) 0.0661(19) Uani 1 1 d . . . . .
H7 H 1.0777 0.4222 0.7757 0.079 Uiso 1 1 calc R . . . .
O5 O 0.2406(6) 0.1737(3) 0.7050(3) 0.110(2) Uani 1 1 d . U . . .
C4 C 0.8389(7) 0.3945(3) 0.7834(2) 0.0641(19) Uani 1 1 d . . . . .
H4A H 0.9007 0.4177 0.8066 0.077 Uiso 1 1 calc R . . . .
H4B H 0.7621 0.4054 0.7953 0.077 Uiso 1 1 calc R . . . .
C60 C 0.9180(9) 0.4055(5) 0.3689(3) 0.093(2) Uani 1 1 d . U . . .
H60A H 0.8824 0.4330 0.3393 0.112 Uiso 1 1 calc R . . . .
H60B H 1.0032 0.4017 0.3658 0.112 Uiso 1 1 calc R . . . .
C70 C 0.1703(8) 0.1669(4) 0.7463(4) 0.091(2) Uani 1 1 d . U . . .
H70A H 0.2162 0.1753 0.7831 0.109 Uiso 1 1 calc R . . . .
H70B H 0.1406 0.1253 0.7465 0.109 Uiso 1 1 calc R . . . .
C5 C 0.8607(8) 0.3288(3) 0.7952(3) 0.077(2) Uani 1 1 d . . . . .
H5A H 0.9279 0.3153 0.7771 0.116 Uiso 1 1 calc GR . . . .
H5B H 0.7904 0.3058 0.7805 0.116 Uiso 1 1 calc GR . . . .
H5C H 0.8780 0.3225 0.8355 0.116 Uiso 1 1 calc GR . . . .
C61 C 0.8632(9) 0.3489(4) 0.3623(3) 0.089(2) Uani 1 1 d . U . . .
H61A H 0.9084 0.3219 0.3405 0.106 Uiso 1 1 calc R . . . .
H61B H 0.7820 0.3528 0.3427 0.106 Uiso 1 1 calc R . . . .
C68 C 0.0756(10) 0.2281(5) 0.6803(5) 0.123(3) Uani 1 1 d . U . . .
H68A H 0.0159 0.2067 0.6541 0.148 Uiso 1 1 calc R . . . .
H68B H 0.0596 0.2716 0.6774 0.148 Uiso 1 1 calc R . . . .
C67 C 0.1900(9) 0.2153(5) 0.6684(5) 0.114(3) Uani 1 1 d . U . . .
H67A H 0.1863 0.1999 0.6298 0.137 Uiso 1 1 calc R . . . .
H67B H 0.2380 0.2523 0.6713 0.137 Uiso 1 1 calc R . . . .
C69 C 0.0733(9) 0.2078(5) 0.7360(5) 0.115(3) Uani 1 1 d . U . . .
H69A H 0.0833 0.2417 0.7626 0.138 Uiso 1 1 calc R . . . .
H69B H -0.0021 0.1873 0.7396 0.138 Uiso 1 1 calc R . . . .
C2 C 0.8411(13) 0.4869(6) 0.7137(6) 0.034(3) Uani 0.541(14) 1 d . . P A 2
H2A H 0.9121 0.5039 0.7361 0.041 Uiso 0.541(14) 1 calc R . P A 2
H2B H 0.8434 0.4969 0.6740 0.041 Uiso 0.541(14) 1 calc R . P A 2
C3 C 0.7272(10) 0.5131(5) 0.7337(6) 0.062(4) Uani 0.541(14) 1 d . . P A 2
H3A H 0.6599 0.5068 0.7048 0.092 Uiso 0.541(14) 1 calc GR . P A 2
H3B H 0.7377 0.5561 0.7409 0.092 Uiso 0.541(14) 1 calc GR . P A 2
H3C H 0.7124 0.4929 0.7681 0.092 Uiso 0.541(14) 1 calc GR . P A 2
C2A C 0.7983(17) 0.4805(8) 0.7268(7) 0.044(4) Uani 0.459(14) 1 d . . P A 3
H2AA H 0.7194 0.4815 0.7395 0.053 Uiso 0.459(14) 1 calc R . P A 3
H2AB H 0.8542 0.5011 0.7553 0.053 Uiso 0.459(14) 1 calc R . P A 3
C3A C 0.7935(14) 0.5125(6) 0.6742(6) 0.059(4) Uani 0.459(14) 1 d . . P A 3
H3AA H 0.7283 0.4968 0.6478 0.088 Uiso 0.459(14) 1 calc GR . P A 3
H3AB H 0.8679 0.5069 0.6589 0.088 Uiso 0.459(14) 1 calc GR . P A 3
H3AC H 0.7810 0.5552 0.6804 0.088 Uiso 0.459(14) 1 calc GR . P A 3


_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 1.781(3) . ?
U1 O3 2.479(3) . ?
U1 O2 1.782(3) . ?
U1 N3 2.527(4) . ?
U1 N4 2.458(4) . ?
U1 N2 2.570(4) . ?
U1 N1 2.456(4) . ?
Sn1 O4 2.325(3) . ?
Sn1 N5 2.215(4) . ?
Sn1 N8 2.225(4) . ?
O3 C62 1.451(6) . ?
O3 C59 1.465(7) . ?
O4 C66 1.453(6) . ?
O4 C63 1.450(6) . ?
N5 C26 1.390(6) . ?
N5 C29 1.364(5) . ?
N6 C24 1.411(6) . ?
N6 C25 1.290(6) . ?
N3 C53 1.426(6) . ?
N3 C54 1.319(6) . ?
N4 C55 1.388(7) . ?
N4 C58 1.363(6) . ?
N2 C11 1.428(7) . ?
N2 C10 1.317(7) . ?
N8 C38 1.395(6) . ?
N8 C35 1.361(6) . ?
N7 C40 1.407(6) . ?
N7 C39 1.271(6) . ?
N1 C6 1.356(6) . ?
N1 C9 1.386(8) . ?
C47 C53 1.435(6) . ?
C47 C46 1.400(6) . ?
C47 C48 1.441(6) . ?
C53 C52 1.370(7) . ?
C17 H17 0.9500 . ?
C17 C16 1.413(6) . ?
C17 C18 1.403(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.408(7) . ?
C55 C56 1.419(7) . ?
C24 C23 1.380(6) . ?
C24 C18 1.433(7) . ?
C45 C46 1.395(6) . ?
C45 C44 1.441(6) . ?
C45 C40 1.455(6) . ?
C46 H46 0.9500 . ?
C11 C16 1.436(7) . ?
C11 C12 1.367(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.415(6) . ?
C26 C27 1.387(6) . ?
C58 C1 1.521(8) . ?
C58 C57 1.391(9) . ?
C29 C30 1.515(7) . ?
C29 C28 1.394(6) . ?
C16 C15 1.430(6) . ?
C38 C39 1.428(7) . ?
C38 C37 1.366(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.422(7) . ?
C6 C1 1.501(9) . ?
C6 C7 1.424(8) . ?
C30 C35 1.523(7) . ?
C30 C33 1.561(6) . ?
C30 C31 1.569(7) . ?
C56 H56 0.9500 . ?
C56 C57 1.402(10) . ?
C22 H22 0.9500 . ?
C22 C21 1.350(8) . ?
C10 H10 0.9500 . ?
C10 C9 1.394(9) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C61 1.494(9) . ?
C52 H52 0.9500 . ?
C52 C51 1.409(7) . ?
C44 C49 1.403(7) . ?
C44 C43 1.425(7) . ?
C35 C36 1.398(8) . ?
C9 C8 1.384(8) . ?
C28 H28 0.9500 . ?
C28 C27 1.376(7) . ?
C19 C18 1.437(6) . ?
C19 C20 1.398(7) . ?
C19 C21 1.434(7) . ?
C15 C20 1.375(7) . ?
C15 C14 1.445(7) . ?
C20 H20 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.394(9) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.504(7) . ?
C65 C64 1.539(7) . ?
C49 H49 0.9500 . ?
C49 C48 1.399(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34 C33 1.517(8) . ?
C40 C41 1.367(7) . ?
C48 C50 1.426(7) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C27 H27 0.9500 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.493(9) . ?
C21 H21 0.9500 . ?
C51 H51 0.9500 . ?
C51 C50 1.372(8) . ?
C50 H50 0.9500 . ?
C39 H39 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.368(9) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.506(8) . ?
C1 C4 1.546(8) . ?
C1 C2 1.645(15) . ?
C1 C2A 1.566(19) . ?
C42 H42 0.9500 . ?
C42 C43 1.359(7) . ?
C42 C41 1.426(7) . ?
C43 H43 0.9500 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.524(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.399(9) . ?
C13 H13 0.9500 . ?
C41 H41 0.9500 . ?
C57 H57 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C7 1.402(10) . ?
C37 H37 0.9500 . ?
C7 H7 0.9500 . ?
O5 C70 1.371(11) . ?
O5 C67 1.358(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.510(9) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.411(12) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C69 1.432(12) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C67 1.405(13) . ?
C68 C69 1.426(14) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.562(18) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A C3A 1.45(2) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 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 90.75(13) . . ?
O1 U1 O2 175.61(15) . . ?
O1 U1 N3 88.51(14) . . ?
O1 U1 N4 88.45(13) . . ?
O1 U1 N2 86.85(14) . . ?
O1 U1 N1 95.09(14) . . ?
O3 U1 N3 77.59(12) . . ?
O3 U1 N2 77.22(13) . . ?
O2 U1 O3 84.89(13) . . ?
O2 U1 N3 90.98(14) . . ?
O2 U1 N4 95.36(14) . . ?
O2 U1 N2 91.74(14) . . ?
O2 U1 N1 88.26(14) . . ?
N3 U1 N2 154.31(13) . . ?
N4 U1 O3 144.42(13) . . ?
N4 U1 N3 66.83(13) . . ?
N4 U1 N2 138.17(14) . . ?
N1 U1 O3 144.95(14) . . ?
N1 U1 N3 136.97(14) . . ?
N1 U1 N4 70.41(15) . . ?
N1 U1 N2 68.67(15) . . ?
N5 Sn1 O4 82.36(12) . . ?
N5 Sn1 N8 79.71(14) . . ?
N8 Sn1 O4 89.94(13) . . ?
C62 O3 U1 127.6(3) . . ?
C62 O3 C59 110.0(4) . . ?
C59 O3 U1 122.3(3) . . ?
C66 O4 Sn1 116.5(3) . . ?
C63 O4 Sn1 122.6(3) . . ?
C63 O4 C66 109.7(4) . . ?
C26 N5 Sn1 121.7(3) . . ?
C29 N5 Sn1 131.6(3) . . ?
C29 N5 C26 106.7(4) . . ?
C25 N6 C24 118.6(4) . . ?
C53 N3 U1 127.5(3) . . ?
C54 N3 U1 114.1(3) . . ?
C54 N3 C53 118.5(4) . . ?
C55 N4 U1 113.3(3) . . ?
C58 N4 U1 137.3(4) . . ?
C58 N4 C55 106.3(4) . . ?
C11 N2 U1 128.3(3) . . ?
C10 N2 U1 111.2(3) . . ?
C10 N2 C11 116.9(4) . . ?
C38 N8 Sn1 119.8(3) . . ?
C35 N8 Sn1 130.4(3) . . ?
C35 N8 C38 106.8(4) . . ?
C39 N7 C40 118.2(4) . . ?
C6 N1 U1 138.2(4) . . ?
C6 N1 C9 106.6(5) . . ?
C9 N1 U1 113.8(3) . . ?
C53 C47 C48 118.2(4) . . ?
C46 C47 C53 123.2(4) . . ?
C46 C47 C48 118.6(4) . . ?
N3 C53 C47 121.1(4) . . ?
C52 C53 N3 118.8(4) . . ?
C52 C53 C47 120.1(4) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C18 C17 C16 121.4(4) . . ?
N3 C54 H54 120.0 . . ?
N3 C54 C55 119.9(5) . . ?
C55 C54 H54 120.0 . . ?
N4 C55 C54 119.1(4) . . ?
N4 C55 C56 110.3(5) . . ?
C54 C55 C56 130.1(6) . . ?
N6 C24 C18 119.5(4) . . ?
C23 C24 N6 120.5(4) . . ?
C23 C24 C18 120.0(4) . . ?
C46 C45 C44 119.5(4) . . ?
C46 C45 C40 121.8(4) . . ?
C44 C45 C40 118.6(4) . . ?
C47 C46 H46 118.9 . . ?
C45 C46 C47 122.1(4) . . ?
C45 C46 H46 118.9 . . ?
N2 C11 C16 121.3(4) . . ?
C12 C11 N2 118.2(5) . . ?
C12 C11 C16 120.4(5) . . ?
N6 C25 H25 118.3 . . ?
N6 C25 C26 123.4(4) . . ?
C26 C25 H25 118.3 . . ?
N5 C26 C25 122.0(4) . . ?
C27 C26 N5 109.1(4) . . ?
C27 C26 C25 128.8(4) . . ?
N4 C58 C1 122.4(5) . . ?
N4 C58 C57 110.3(5) . . ?
C57 C58 C1 126.4(5) . . ?
N5 C29 C30 124.2(4) . . ?
N5 C29 C28 109.3(4) . . ?
C28 C29 C30 126.2(4) . . ?
C17 C16 C11 123.5(4) . . ?
C17 C16 C15 118.6(4) . . ?
C15 C16 C11 117.9(4) . . ?
N8 C38 C39 122.9(4) . . ?
C37 C38 N8 109.3(5) . . ?
C37 C38 C39 127.8(5) . . ?
C24 C23 H23 119.5 . . ?
C24 C23 C22 120.9(5) . . ?
C22 C23 H23 119.5 . . ?
N1 C6 C1 125.6(5) . . ?
N1 C6 C7 109.3(6) . . ?
C7 C6 C1 124.7(5) . . ?
C29 C30 C35 115.1(4) . . ?
C29 C30 C33 109.2(4) . . ?
C29 C30 C31 108.4(4) . . ?
C35 C30 C33 109.0(4) . . ?
C35 C30 C31 107.8(4) . . ?
C33 C30 C31 107.0(4) . . ?
C55 C56 H56 127.6 . . ?
C57 C56 C55 104.9(5) . . ?
C57 C56 H56 127.6 . . ?
C23 C22 H22 119.6 . . ?
C21 C22 C23 120.8(4) . . ?
C21 C22 H22 119.6 . . ?
N2 C10 H10 118.4 . . ?
N2 C10 C9 123.2(5) . . ?
C9 C10 H10 118.4 . . ?
O3 C62 H62A 110.6 . . ?
O3 C62 H62B 110.6 . . ?
O3 C62 C61 105.5(6) . . ?
H62A C62 H62B 108.8 . . ?
C61 C62 H62A 110.6 . . ?
C61 C62 H62B 110.6 . . ?
C53 C52 H52 119.2 . . ?
C53 C52 C51 121.7(5) . . ?
C51 C52 H52 119.2 . . ?
C49 C44 C45 118.3(4) . . ?
C49 C44 C43 122.3(4) . . ?
C43 C44 C45 119.4(4) . . ?
N8 C35 C30 124.8(4) . . ?
N8 C35 C36 109.4(5) . . ?
C36 C35 C30 125.3(5) . . ?
N1 C9 C10 121.3(5) . . ?
C8 C9 N1 111.2(6) . . ?
C8 C9 C10 127.5(6) . . ?
C29 C28 H28 126.2 . . ?
C27 C28 C29 107.7(4) . . ?
C27 C28 H28 126.2 . . ?
C20 C19 C18 118.7(4) . . ?
C20 C19 C21 121.6(4) . . ?
C21 C19 C18 119.6(4) . . ?
C17 C18 C24 122.9(4) . . ?
C17 C18 C19 118.9(4) . . ?
C24 C18 C19 118.1(4) . . ?
C16 C15 C14 119.7(5) . . ?
C20 C15 C16 119.6(4) . . ?
C20 C15 C14 120.7(4) . . ?
C19 C20 H20 118.7 . . ?
C15 C20 C19 122.6(4) . . ?
C15 C20 H20 118.7 . . ?
C35 C36 H36 126.7 . . ?
C37 C36 C35 106.7(5) . . ?
C37 C36 H36 126.7 . . ?
H65A C65 H65B 109.2 . . ?
C66 C65 H65A 111.2 . . ?
C66 C65 H65B 111.2 . . ?
C66 C65 C64 102.6(4) . . ?
C64 C65 H65A 111.2 . . ?
C64 C65 H65B 111.2 . . ?
C44 C49 H49 118.9 . . ?
C48 C49 C44 122.3(4) . . ?
C48 C49 H49 118.9 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
N7 C40 C45 119.6(4) . . ?
C41 C40 N7 121.3(4) . . ?
C41 C40 C45 119.2(4) . . ?
C49 C48 C47 119.2(4) . . ?
C49 C48 C50 121.4(4) . . ?
C50 C48 C47 119.4(4) . . ?
O4 C66 C65 106.2(4) . . ?
O4 C66 H66A 110.5 . . ?
O4 C66 H66B 110.5 . . ?
C65 C66 H66A 110.5 . . ?
C65 C66 H66B 110.5 . . ?
H66A C66 H66B 108.7 . . ?
C30 C33 H33A 108.6 . . ?
C30 C33 H33B 108.6 . . ?
C34 C33 C30 114.8(4) . . ?
C34 C33 H33A 108.6 . . ?
C34 C33 H33B 108.6 . . ?
H33A C33 H33B 107.5 . . ?
C26 C27 H27 126.4 . . ?
C28 C27 C26 107.2(4) . . ?
C28 C27 H27 126.4 . . ?
O3 C59 H59A 111.0 . . ?
O3 C59 H59B 111.0 . . ?
O3 C59 C60 103.6(6) . . ?
H59A C59 H59B 109.0 . . ?
C60 C59 H59A 111.0 . . ?
C60 C59 H59B 111.0 . . ?
C22 C21 C19 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C19 C21 H21 119.8 . . ?
C52 C51 H51 119.9 . . ?
C50 C51 C52 120.2(5) . . ?
C50 C51 H51 119.9 . . ?
C48 C50 H50 119.8 . . ?
C51 C50 C48 120.4(5) . . ?
C51 C50 H50 119.8 . . ?
N7 C39 C38 123.8(5) . . ?
N7 C39 H39 118.1 . . ?
C38 C39 H39 118.1 . . ?
C15 C14 H14 120.3 . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 H14 120.3 . . ?
O4 C63 H63A 111.0 . . ?
O4 C63 H63B 111.0 . . ?
O4 C63 C64 104.0(4) . . ?
H63A C63 H63B 109.0 . . ?
C64 C63 H63A 111.0 . . ?
C64 C63 H63B 111.0 . . ?
C58 C1 C4 111.5(6) . . ?
C58 C1 C2 110.3(7) . . ?
C58 C1 C2A 101.9(8) . . ?
C6 C1 C58 115.2(4) . . ?
C6 C1 C4 109.9(5) . . ?
C6 C1 C2 95.8(6) . . ?
C6 C1 C2A 117.9(8) . . ?
C4 C1 C2 113.3(6) . . ?
C4 C1 C2A 99.2(7) . . ?
C43 C42 H42 119.5 . . ?
C43 C42 C41 120.9(5) . . ?
C41 C42 H42 119.5 . . ?
C44 C43 H43 119.8 . . ?
C42 C43 C44 120.3(5) . . ?
C42 C43 H43 119.8 . . ?
C65 C64 H64A 111.4 . . ?
C65 C64 H64B 111.4 . . ?
C63 C64 C65 101.8(5) . . ?
C63 C64 H64A 111.4 . . ?
C63 C64 H64B 111.4 . . ?
H64A C64 H64B 109.3 . . ?
C30 C31 H31A 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 C30 115.0(4) . . ?
C32 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C13 121.5(5) . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 121.0(5) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C40 C41 C42 121.5(5) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 H41 119.3 . . ?
C58 C57 C56 108.2(5) . . ?
C58 C57 H57 125.9 . . ?
C56 C57 H57 125.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C9 C8 H8 127.1 . . ?
C9 C8 C7 105.8(6) . . ?
C7 C8 H8 127.1 . . ?
C38 C37 C36 107.8(5) . . ?
C38 C37 H37 126.1 . . ?
C36 C37 H37 126.1 . . ?
C6 C7 H7 126.5 . . ?
C8 C7 C6 107.1(5) . . ?
C8 C7 H7 126.5 . . ?
C67 O5 C70 108.1(7) . . ?
C1 C4 H4A 108.4 . . ?
C1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C5 C4 C1 115.7(5) . . ?
C5 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C59 C60 H60A 110.0 . . ?
C59 C60 H60B 110.0 . . ?
H60A C60 H60B 108.3 . . ?
C61 C60 C59 108.7(6) . . ?
C61 C60 H60A 110.0 . . ?
C61 C60 H60B 110.0 . . ?
O5 C70 H70A 110.0 . . ?
O5 C70 H70B 110.0 . . ?
O5 C70 C69 108.4(8) . . ?
H70A C70 H70B 108.4 . . ?
C69 C70 H70A 110.0 . . ?
C69 C70 H70B 110.0 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C62 C61 H61A 110.5 . . ?
C62 C61 H61B 110.5 . . ?
C60 C61 C62 106.2(6) . . ?
C60 C61 H61A 110.5 . . ?
C60 C61 H61B 110.5 . . ?
H61A C61 H61B 108.7 . . ?
H68A C68 H68B 108.8 . . ?
C67 C68 H68A 110.7 . . ?
C67 C68 H68B 110.7 . . ?
C67 C68 C69 105.2(9) . . ?
C69 C68 H68A 110.7 . . ?
C69 C68 H68B 110.7 . . ?
O5 C67 C68 109.5(10) . . ?
O5 C67 H67A 109.8 . . ?
O5 C67 H67B 109.8 . . ?
C68 C67 H67A 109.8 . . ?
C68 C67 H67B 109.8 . . ?
H67A C67 H67B 108.2 . . ?
C70 C69 C68 104.9(9) . . ?
C70 C69 H69A 110.8 . . ?
C70 C69 H69B 110.8 . . ?
C68 C69 H69A 110.8 . . ?
C68 C69 H69B 110.8 . . ?
H69A C69 H69B 108.8 . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 C1 107.5(9) . . ?
C3 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C2A H2AA 109.2 . . ?
C1 C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?
C3A C2A C1 112.3(12) . . ?
C3A C2A H2AA 109.2 . . ?
C3A C2A H2AB 109.2 . . ?
C2A C3A H3AA 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
C2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_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 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.731
####################################################################### 
# 
# 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_UO2PbLMethf
_database_code_depnum_ccdc_archive 'CCDC 1480065'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-03-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H48 N8 O3 Pb U'
_chemical_formula_sum            'C46 H48 N8 O3 Pb U'
_chemical_formula_weight         1206.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H70 N8 O4 U Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   12.9064(4)
_cell_length_b                   14.3173(3)
_cell_length_c                   17.8924(5)
_cell_angle_alpha                106.269(2)
_cell_angle_beta                 97.424(2)
_cell_angle_gamma                101.336(2)
_cell_volume                     3051.71(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21989
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.7530
_cell_measurement_theta_min      3.5270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.3978
_exptl_crystal_size_mid          0.2668
_exptl_crystal_size_min          0.0297
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29521
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.172
_diffrn_reflns_theta_min         2.913
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   38.0000    0.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  150.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   26.0000  -45.7048 101

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
  6 omega  -89.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -38.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
  7 omega  -87.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
  8 omega    2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000  120.0000 87

#__ type_ start__ end____ width___ exp.time_
  9 omega  -50.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -38.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
 10 omega  -48.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -57.0000  -60.0000 87

#__ type_ start__ end____ width___ exp.time_
 11 omega  -41.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277   38.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 12 omega  -87.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000  -30.0000 87

#__ type_ start__ end____ width___ exp.time_
 13 omega  -93.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  179.0000  -30.0000 61

#__ type_ start__ end____ width___ exp.time_
 14 omega  -25.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000 -120.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0219981000
_diffrn_orient_matrix_UB_12      -0.0072042000
_diffrn_orient_matrix_UB_13      -0.0349302000
_diffrn_orient_matrix_UB_21      -0.0516558000
_diffrn_orient_matrix_UB_22      -0.0268729000
_diffrn_orient_matrix_UB_23      -0.0232159000
_diffrn_orient_matrix_UB_31      -0.0107071000
_diffrn_orient_matrix_UB_32      0.0453729000
_diffrn_orient_matrix_UB_33      -0.0037728000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6704 23414 49854
2 0.3296 23310 49853

_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20366
_reflns_number_total             29521
_reflns_special_details          
;
 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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         4.381
_refine_diff_density_min         -2.923
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         29521
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0738
_refine_ls_restrained_S_all      1.121
_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)+(0.0954P)²+26.8616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2039
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7028(9) 0.2972(9)
2. 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
3. Restrained distances
 C43-C42
 1.39 with sigma of 0.02
 C44-C45
 1.39 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C42 \\sim O3 \\sim C45 \\sim C44 \\sim C43: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C12 \\sim C11 \\sim N4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N4 \\sim C12 \\sim C11: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Rigid body (RIGU) restrains
 C43, C42, O3, C45, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C42(H42A,H42B), C44(H44A,H44B), C43(H43A,H43B)
6.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C32(H32), C12(H12), C1(H1), C24(H24), C10(H10), C23(H23), C4(H4),
 C3(H3), C9(H9), C39(H39), C34(H34), C30(H30), C29(H29), C14(H14), C19(H19)
6.c Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C7(H7A,H7B,H7C), C36(H36A,H36B,H36C), C27(H27A,H27B,
 H27C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C16(H16A,
 H16B,H16C)
;
_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 0.60457(3) 0.62265(3) 0.85412(3) 0.02424(12) Uani 1 1 d . . . . .
Pb1 Pb 0.52499(4) 0.49096(3) 0.61484(3) 0.02741(13) Uani 1 1 d . . . . .
C21 C 0.5300(9) 0.7236(9) 0.6017(8) 0.029(3) Uani 1 1 d . . . . .
H21 H 0.4996 0.7722 0.5861 0.035 Uiso 1 1 calc R . . . .
N1 N 0.5571(8) 0.4434(7) 0.8523(6) 0.029(2) Uani 1 1 d . . . . .
N4 N 0.5601(9) 0.7769(7) 0.8306(6) 0.029(2) Uani 1 1 d . U . . .
C32 C 0.5694(10) 0.2897(10) 0.6500(7) 0.031(3) Uani 1 1 d . . . . .
H32 H 0.5563 0.2234 0.6531 0.037 Uiso 1 1 calc R . . . .
C12 C 0.6235(11) 0.8586(10) 0.8781(8) 0.036(3) Uani 1 1 d . U . . .
H12 H 0.6024 0.9200 0.8855 0.044 Uiso 1 1 calc R . . . .
O2 O 0.6314(7) 0.5818(6) 0.7544(5) 0.0296(19) Uani 1 1 d . . . . .
N7 N 0.6622(8) 0.4132(8) 0.5946(6) 0.027(2) Uani 1 1 d . . . . .
N5 N 0.5056(8) 0.7004(7) 0.6626(6) 0.027(2) Uani 1 1 d . . . . .
O1 O 0.5700(7) 0.6589(7) 0.9496(6) 0.040(2) Uani 1 1 d . . . . .
N8 N 0.5209(9) 0.3499(8) 0.6886(6) 0.031(2) Uani 1 1 d . . . . .
O3 O 0.4044(7) 0.5729(6) 0.8120(5) 0.0316(18) Uani 1 1 d . U . . .
C1 C 0.6244(10) 0.4229(9) 0.9000(7) 0.030(3) Uani 1 1 d . . . . .
H1 H 0.6060 0.3609 0.9105 0.036 Uiso 1 1 calc R . . . .
N2 N 0.7558(7) 0.5765(7) 0.9168(5) 0.023(2) Uani 1 1 d . . . . .
C13 C 0.4614(10) 0.7855(8) 0.7883(8) 0.028(3) Uani 1 1 d . . . . .
N6 N 0.6430(8) 0.6023(8) 0.5725(7) 0.031(2) Uani 1 1 d . . . . .
C28 C 0.7419(9) 0.4240(9) 0.5536(7) 0.025(2) Uani 1 1 d . . . . .
N3 N 0.7576(8) 0.7683(7) 0.9054(6) 0.030(2) Uani 1 1 d . . . . .
C20 C 0.4360(10) 0.7507(9) 0.7057(9) 0.033(3) Uani 1 1 d . . . . .
C33 C 0.4445(10) 0.3161(9) 0.7324(7) 0.030(3) Uani 1 1 d . . . . .
C24 C 0.7284(11) 0.6546(10) 0.4837(8) 0.036(3) Uani 1 1 d . . . . .
H24 H 0.7772 0.6615 0.4490 0.043 Uiso 1 1 calc R . . . .
C10 C 0.8077(11) 0.9360(10) 0.9704(8) 0.038(3) Uani 1 1 d . . . . .
H10 H 0.8069 1.0047 0.9899 0.045 Uiso 1 1 calc R . . . .
C41 C 0.8598(10) 0.6200(9) 0.9544(8) 0.030(3) Uani 1 1 d . . . . .
C40 C 0.4613(10) 0.3670(8) 0.8144(7) 0.026(3) Uani 1 1 d . . . . .
C23 C 0.6527(11) 0.7089(9) 0.5008(8) 0.032(3) Uani 1 1 d . . . . .
H23 H 0.6380 0.7588 0.4784 0.038 Uiso 1 1 calc R . . . .
C4 C 0.8974(12) 0.5635(11) 0.9993(10) 0.043(4) Uani 1 1 d . . . . .
H4 H 0.9671 0.5784 1.0312 0.052 Uiso 1 1 calc R . . . .
C2 C 0.7267(10) 0.4902(10) 0.9382(8) 0.030(3) Uani 1 1 d . . . . .
C26 C 0.7936(9) 0.5202(10) 0.5396(7) 0.028(3) Uani 1 1 d . . . . .
C31 C 0.6431(10) 0.3168(9) 0.6019(7) 0.026(2) Uani 1 1 d . . . . .
C5 C 0.9228(10) 0.7125(10) 0.9402(8) 0.034(3) Uani 1 1 d . . . . .
C45 C 0.3314(11) 0.5254(12) 0.7369(9) 0.046(3) Uani 1 1 d D U . . .
H45A H 0.3284 0.4529 0.7178 0.055 Uiso 1 1 calc R . . A .
H45B H 0.3545 0.5561 0.6967 0.055 Uiso 1 1 calc R . . A .
C8 C 0.8582(10) 0.7900(9) 0.9467(7) 0.028(3) Uani 1 1 d . . . . .
C25 C 0.7196(10) 0.5858(9) 0.5283(7) 0.028(3) Uani 1 1 d . . . . .
C3 C 0.8123(11) 0.4808(10) 0.9882(9) 0.038(3) Uani 1 1 d . . . . .
H3 H 0.8131 0.4281 1.0107 0.046 Uiso 1 1 calc R . . . .
C9 C 0.8933(13) 0.8933(11) 0.9878(9) 0.042(4) Uani 1 1 d . . . . .
H9 H 0.9616 0.9276 1.0209 0.051 Uiso 1 1 calc R . . . .
C35 C 0.2773(11) 0.2083(10) 0.7388(9) 0.037(3) Uani 1 1 d . . . . .
C39 C 0.3850(11) 0.3368(9) 0.8572(9) 0.036(3) Uani 1 1 d . . . . .
H39 H 0.3960 0.3701 0.9126 0.043 Uiso 1 1 calc R . . . .
C017 C 0.8802(11) 0.5798(12) 0.6133(9) 0.046(4) Uani 1 1 d . . . . .
H01A H 0.8460 0.6012 0.6589 0.069 Uiso 1 1 calc GR . . . .
H01B H 0.9225 0.6390 0.6043 0.069 Uiso 1 1 calc GR . . . .
H01C H 0.9278 0.5376 0.6241 0.069 Uiso 1 1 calc GR . . . .
C34 C 0.3553(10) 0.2379(10) 0.6964(8) 0.033(3) Uani 1 1 d . . . . .
H34 H 0.3461 0.2029 0.6415 0.040 Uiso 1 1 calc R . . . .
C30 C 0.7158(12) 0.2683(11) 0.5669(10) 0.044(4) Uani 1 1 d . . . . .
H30 H 0.7224 0.2027 0.5646 0.053 Uiso 1 1 calc R . . . .
C29 C 0.7767(12) 0.3332(11) 0.5361(9) 0.042(3) Uani 1 1 d . . . . .
H29 H 0.8325 0.3197 0.5079 0.050 Uiso 1 1 calc R . . . .
C37 C 0.2930(11) 0.2590(9) 0.8207(8) 0.032(3) Uani 1 1 d . . . . .
C11 C 0.7243(11) 0.8584(9) 0.9193(8) 0.034(3) Uani 1 1 d . U . . .
C14 C 0.3913(11) 0.8316(10) 0.8310(9) 0.037(3) Uani 1 1 d . . . . .
H14 H 0.4085 0.8545 0.8874 0.044 Uiso 1 1 calc R . . . .
C19 C 0.3407(11) 0.7649(10) 0.6655(9) 0.039(3) Uani 1 1 d . . . . .
H19 H 0.3238 0.7427 0.6091 0.047 Uiso 1 1 calc R . . . .
C7 C 0.9444(12) 0.6801(11) 0.8546(9) 0.044(3) Uani 1 1 d . . . . .
H7A H 0.9896 0.6321 0.8502 0.066 Uiso 1 1 calc GR . . . .
H7B H 0.9815 0.7392 0.8426 0.066 Uiso 1 1 calc GR . . . .
H7C H 0.8758 0.6487 0.8169 0.066 Uiso 1 1 calc GR . . . .
C17 C 0.2722(11) 0.8113(11) 0.7088(10) 0.044(4) Uani 1 1 d . . . . .
C42 C 0.3394(10) 0.5914(14) 0.8737(9) 0.050(3) Uani 1 1 d D U . . .
H42A H 0.3459 0.5468 0.9065 0.060 Uiso 1 1 calc R . . . .
H42B H 0.3639 0.6619 0.9086 0.060 Uiso 1 1 calc R . . . .
C22 C 0.6023(10) 0.6782(9) 0.5558(9) 0.034(3) Uani 1 1 d . . . . .
C36 C 0.1813(13) 0.1215(12) 0.6982(10) 0.056(5) Uani 1 1 d . . . . .
H36A H 0.1713 0.1083 0.6407 0.085 Uiso 1 1 calc GR . . . .
H36B H 0.1168 0.1380 0.7165 0.085 Uiso 1 1 calc GR . . . .
H36C H 0.1932 0.0618 0.7110 0.085 Uiso 1 1 calc GR . . . .
C27 C 0.8498(12) 0.4959(12) 0.4692(9) 0.043(3) Uani 1 1 d . . . . .
H27A H 0.8989 0.4539 0.4776 0.065 Uiso 1 1 calc GR . . . .
H27B H 0.8909 0.5583 0.4641 0.065 Uiso 1 1 calc GR . . . .
H27C H 0.7958 0.4598 0.4205 0.065 Uiso 1 1 calc GR . . . .
C15 C 0.2960(12) 0.8447(11) 0.7919(10) 0.045(4) Uani 1 1 d . . . . .
C38 C 0.2148(12) 0.2287(12) 0.8725(9) 0.046(4) Uani 1 1 d . . . . .
H38A H 0.2164 0.1614 0.8747 0.069 Uiso 1 1 calc GR . . . .
H38B H 0.1416 0.2288 0.8496 0.069 Uiso 1 1 calc GR . . . .
H38C H 0.2365 0.2767 0.9263 0.069 Uiso 1 1 calc GR . . . .
C18 C 0.1712(14) 0.8246(15) 0.6627(12) 0.067(6) Uani 1 1 d . . . . .
H18A H 0.1776 0.8138 0.6071 0.101 Uiso 1 1 calc GR . . . .
H18B H 0.1630 0.8928 0.6858 0.101 Uiso 1 1 calc GR . . . .
H18C H 0.1080 0.7759 0.6654 0.101 Uiso 1 1 calc GR . . . .
C6 C 1.0304(11) 0.7553(12) 0.9986(11) 0.052(4) Uani 1 1 d . . . . .
H6A H 1.0175 0.7811 1.0525 0.078 Uiso 1 1 calc GR . . . .
H6B H 1.0738 0.8099 0.9847 0.078 Uiso 1 1 calc GR . . . .
H6C H 1.0690 0.7024 0.9962 0.078 Uiso 1 1 calc GR . . . .
C16 C 0.2239(15) 0.8935(15) 0.8418(12) 0.070(6) Uani 1 1 d . . . . .
H16A H 0.1516 0.8487 0.8277 0.105 Uiso 1 1 calc GR . . . .
H16B H 0.2198 0.9569 0.8320 0.105 Uiso 1 1 calc GR . . . .
H16C H 0.2534 0.9069 0.8981 0.105 Uiso 1 1 calc GR . . . .
C44 C 0.2262(13) 0.5414(18) 0.7514(11) 0.075(4) Uani 1 1 d D U . B 1
H44A H 0.2090 0.5940 0.7294 0.091 Uiso 1 1 calc R . . B 1
H44B H 0.1697 0.4786 0.7246 0.091 Uiso 1 1 calc R . . B 1
C43 C 0.2280(13) 0.5706(18) 0.8324(11) 0.075(4) Uani 1 1 d D U . . .
H43A H 0.1820 0.5164 0.8463 0.090 Uiso 1 1 calc R . . B .
H43B H 0.2000 0.6314 0.8483 0.090 Uiso 1 1 calc R . . B .


_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 N1 2.508(10) . ?
U1 N4 2.519(10) . ?
U1 O2 1.817(8) . ?
U1 O1 1.783(10) . ?
U1 O3 2.495(8) . ?
U1 N2 2.422(9) . ?
U1 N3 2.435(10) . ?
Pb1 O2 2.530(8) . ?
Pb1 N7 2.285(10) . ?
Pb1 N8 2.700(10) . ?
Pb1 N6 2.335(10) . ?
C21 H21 0.9500 . ?
C21 N5 1.285(16) . ?
C21 C22 1.451(17) . ?
N1 C1 1.272(17) . ?
N1 C40 1.421(15) . ?
N4 C12 1.283(16) . ?
N4 C13 1.440(17) . ?
C32 H32 0.9500 . ?
C32 N8 1.266(16) . ?
C32 C31 1.432(17) . ?
C12 H12 0.9500 . ?
C12 C11 1.41(2) . ?
N7 C28 1.348(15) . ?
N7 C31 1.398(15) . ?
N5 C20 1.428(14) . ?
N8 C33 1.431(16) . ?
O3 C45 1.436(17) . ?
O3 C42 1.468(16) . ?
C1 H1 0.9500 . ?
C1 C2 1.427(18) . ?
N2 C41 1.358(15) . ?
N2 C2 1.389(15) . ?
C13 C20 1.393(19) . ?
C13 C14 1.404(16) . ?
N6 C25 1.360(15) . ?
N6 C22 1.384(16) . ?
C28 C26 1.510(17) . ?
C28 C29 1.423(18) . ?
N3 C8 1.339(16) . ?
N3 C11 1.407(16) . ?
C20 C19 1.423(19) . ?
C33 C40 1.409(17) . ?
C33 C34 1.376(17) . ?
C24 H24 0.9500 . ?
C24 C23 1.377(19) . ?
C24 C25 1.427(18) . ?
C10 H10 0.9500 . ?
C10 C9 1.40(2) . ?
C10 C11 1.391(18) . ?
C41 C4 1.399(19) . ?
C41 C5 1.515(18) . ?
C40 C39 1.399(17) . ?
C23 H23 0.9500 . ?
C23 C22 1.370(18) . ?
C4 H4 0.9500 . ?
C4 C3 1.396(19) . ?
C2 C3 1.382(19) . ?
C26 C25 1.499(17) . ?
C26 C017 1.527(18) . ?
C26 C27 1.525(17) . ?
C31 C30 1.386(18) . ?
C5 C8 1.502(18) . ?
C5 C7 1.550(19) . ?
C5 C6 1.526(18) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C44 1.464(17) . ?
C8 C9 1.405(19) . ?
C3 H3 0.9500 . ?
C9 H9 0.9500 . ?
C35 C34 1.406(18) . ?
C35 C37 1.408(19) . ?
C35 C36 1.504(19) . ?
C39 H39 0.9500 . ?
C39 C37 1.396(17) . ?
C017 H01A 0.9800 . ?
C017 H01B 0.9800 . ?
C017 H01C 0.9800 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C30 C29 1.38(2) . ?
C29 H29 0.9500 . ?
C37 C38 1.536(18) . ?
C14 H14 0.9500 . ?
C14 C15 1.41(2) . ?
C19 H19 0.9500 . ?
C19 C17 1.395(19) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C17 C15 1.40(2) . ?
C17 C18 1.53(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.462(17) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C15 C16 1.51(2) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C43 1.39(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 U1 N4 153.3(4) . . ?
O2 U1 N1 89.7(4) . . ?
O2 U1 N4 90.4(3) . . ?
O2 U1 O3 95.3(3) . . ?
O2 U1 N2 95.5(4) . . ?
O2 U1 N3 96.3(4) . . ?
O1 U1 N1 88.8(4) . . ?
O1 U1 N4 89.5(4) . . ?
O1 U1 O2 176.5(4) . . ?
O1 U1 O3 81.3(4) . . ?
O1 U1 N2 86.9(4) . . ?
O1 U1 N3 86.9(4) . . ?
O3 U1 N1 76.8(3) . . ?
O3 U1 N4 76.6(3) . . ?
N2 U1 N1 68.1(3) . . ?
N2 U1 N4 138.4(3) . . ?
N2 U1 O3 143.1(3) . . ?
N2 U1 N3 70.6(3) . . ?
N3 U1 N1 138.6(3) . . ?
N3 U1 N4 67.8(3) . . ?
N3 U1 O3 142.5(3) . . ?
O2 Pb1 N8 74.1(3) . . ?
N7 Pb1 O2 86.7(3) . . ?
N7 Pb1 N8 68.4(3) . . ?
N7 Pb1 N6 77.6(3) . . ?
N6 Pb1 O2 87.5(3) . . ?
N6 Pb1 N8 141.9(3) . . ?
N5 C21 H21 118.9 . . ?
N5 C21 C22 122.3(12) . . ?
C22 C21 H21 118.9 . . ?
C1 N1 U1 113.6(8) . . ?
C1 N1 C40 116.2(10) . . ?
C40 N1 U1 129.7(8) . . ?
C12 N4 U1 112.8(10) . . ?
C12 N4 C13 116.7(10) . . ?
C13 N4 U1 128.2(7) . . ?
N8 C32 H32 118.5 . . ?
N8 C32 C31 123.1(12) . . ?
C31 C32 H32 118.5 . . ?
N4 C12 H12 119.6 . . ?
N4 C12 C11 120.8(12) . . ?
C11 C12 H12 119.6 . . ?
U1 O2 Pb1 137.8(4) . . ?
C28 N7 Pb1 132.7(8) . . ?
C28 N7 C31 108.7(10) . . ?
C31 N7 Pb1 114.8(7) . . ?
C21 N5 C20 118.6(10) . . ?
C32 N8 Pb1 104.4(8) . . ?
C32 N8 C33 120.0(11) . . ?
C33 N8 Pb1 129.7(8) . . ?
C45 O3 U1 134.3(8) . . ?
C45 O3 C42 107.6(10) . . ?
C42 O3 U1 118.1(7) . . ?
N1 C1 H1 119.0 . . ?
N1 C1 C2 122.0(12) . . ?
C2 C1 H1 119.0 . . ?
C41 N2 U1 138.4(8) . . ?
C41 N2 C2 105.8(10) . . ?
C2 N2 U1 113.7(7) . . ?
C20 C13 N4 120.8(10) . . ?
C20 C13 C14 119.7(12) . . ?
C14 C13 N4 119.5(12) . . ?
C25 N6 Pb1 130.1(8) . . ?
C25 N6 C22 107.5(10) . . ?
C22 N6 Pb1 115.1(8) . . ?
N7 C28 C26 125.2(10) . . ?
N7 C28 C29 107.3(11) . . ?
C29 C28 C26 126.9(11) . . ?
C8 N3 U1 137.0(8) . . ?
C8 N3 C11 107.5(10) . . ?
C11 N3 U1 111.5(8) . . ?
C13 C20 N5 119.5(11) . . ?
C13 C20 C19 119.5(11) . . ?
C19 C20 N5 121.0(13) . . ?
C40 C33 N8 118.1(11) . . ?
C34 C33 N8 121.9(11) . . ?
C34 C33 C40 120.0(12) . . ?
C23 C24 H24 126.6 . . ?
C23 C24 C25 106.8(11) . . ?
C25 C24 H24 126.6 . . ?
C9 C10 H10 126.5 . . ?
C11 C10 H10 126.5 . . ?
C11 C10 C9 107.0(12) . . ?
N2 C41 C4 110.7(11) . . ?
N2 C41 C5 121.2(11) . . ?
C4 C41 C5 127.9(12) . . ?
C33 C40 N1 119.8(11) . . ?
C39 C40 N1 121.7(11) . . ?
C39 C40 C33 118.4(11) . . ?
C24 C23 H23 126.0 . . ?
C22 C23 C24 108.0(12) . . ?
C22 C23 H23 126.0 . . ?
C41 C4 H4 126.8 . . ?
C3 C4 C41 106.4(12) . . ?
C3 C4 H4 126.8 . . ?
N2 C2 C1 118.0(11) . . ?
C3 C2 C1 131.2(12) . . ?
C3 C2 N2 110.3(11) . . ?
C28 C26 C017 106.4(11) . . ?
C28 C26 C27 109.4(10) . . ?
C25 C26 C28 115.5(9) . . ?
C25 C26 C017 107.4(11) . . ?
C25 C26 C27 110.1(11) . . ?
C27 C26 C017 107.6(11) . . ?
N7 C31 C32 119.8(11) . . ?
C30 C31 C32 131.0(12) . . ?
C30 C31 N7 108.5(11) . . ?
C41 C5 C7 107.6(11) . . ?
C41 C5 C6 110.4(12) . . ?
C8 C5 C41 110.5(10) . . ?
C8 C5 C7 108.5(11) . . ?
C8 C5 C6 110.7(11) . . ?
C6 C5 C7 109.0(12) . . ?
O3 C45 H45A 110.6 . . ?
O3 C45 H45B 110.6 . . ?
O3 C45 C44 105.7(13) . . ?
H45A C45 H45B 108.7 . . ?
C44 C45 H45A 110.6 . . ?
C44 C45 H45B 110.6 . . ?
N3 C8 C5 121.9(11) . . ?
N3 C8 C9 110.1(12) . . ?
C9 C8 C5 127.7(12) . . ?
N6 C25 C24 108.2(11) . . ?
N6 C25 C26 122.9(11) . . ?
C24 C25 C26 127.9(11) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 C4 106.8(12) . . ?
C2 C3 H3 126.6 . . ?
C10 C9 C8 106.7(13) . . ?
C10 C9 H9 126.6 . . ?
C8 C9 H9 126.6 . . ?
C34 C35 C37 118.7(12) . . ?
C34 C35 C36 120.7(13) . . ?
C37 C35 C36 120.6(12) . . ?
C40 C39 H39 119.1 . . ?
C37 C39 C40 121.8(13) . . ?
C37 C39 H39 119.1 . . ?
C26 C017 H01A 109.5 . . ?
C26 C017 H01B 109.5 . . ?
C26 C017 H01C 109.5 . . ?
H01A C017 H01B 109.5 . . ?
H01A C017 H01C 109.5 . . ?
H01B C017 H01C 109.5 . . ?
C33 C34 C35 121.8(13) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C31 C30 H30 126.5 . . ?
C29 C30 C31 107.0(12) . . ?
C29 C30 H30 126.5 . . ?
C28 C29 H29 125.8 . . ?
C30 C29 C28 108.4(12) . . ?
C30 C29 H29 125.8 . . ?
C35 C37 C38 122.3(12) . . ?
C39 C37 C35 119.2(12) . . ?
C39 C37 C38 118.4(12) . . ?
N3 C11 C12 119.5(11) . . ?
C10 C11 C12 131.6(12) . . ?
C10 C11 N3 108.6(12) . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(13) . . ?
C15 C14 H14 119.4 . . ?
C20 C19 H19 120.0 . . ?
C17 C19 C20 120.0(14) . . ?
C17 C19 H19 120.0 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C19 C17 C15 120.8(13) . . ?
C19 C17 C18 117.8(15) . . ?
C15 C17 C18 121.4(13) . . ?
O3 C42 H42A 110.4 . . ?
O3 C42 H42B 110.4 . . ?
H42A C42 H42B 108.6 . . ?
C43 C42 O3 106.5(13) . . ?
C43 C42 H42A 110.4 . . ?
C43 C42 H42B 110.4 . . ?
N6 C22 C21 121.2(12) . . ?
C23 C22 C21 128.7(12) . . ?
C23 C22 N6 109.5(11) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C14 C15 C16 118.2(16) . . ?
C17 C15 C14 118.7(13) . . ?
C17 C15 C16 123.1(15) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C45 C44 H44A 109.8 . . ?
C45 C44 H44B 109.8 . . ?
H44A C44 H44B 108.2 . . ?
C43 C44 C45 109.6(15) . . ?
C43 C44 H44A 109.8 . . ?
C43 C44 H44B 109.8 . . ?
C42 C43 H43A 110.1 . . ?
C42 C43 H43B 110.1 . . ?
C44 C43 C42 108.1(15) . . ?
C44 C43 H43A 110.1 . . ?
C44 C43 H43B 110.1 . . ?
H43A C43 H43B 108.4 . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 0 -1 0.0148 0.0003 -0.0003 -0.9990 0.0349 0.0232 0.0038
0 0 1 0.0148 -0.0003 0.0003 0.9990 -0.0349 -0.0232 -0.0038
5 0 -3 0.1318 5.0055 -0.0123 -2.9935 0.2148 -0.1887 -0.0429
-5 0 3 0.1318 -5.0055 0.0123 2.9935 -0.2148 0.1887 0.0429
2 5 -4 0.1810 1.9993 4.9962 -3.9931 0.1475 -0.1448 0.2203
-1 5 -2 0.2114 -1.0040 5.0036 -1.9972 0.0116 -0.0362 0.2453
1 -5 2 0.1809 1.0040 -5.0036 1.9972 -0.0116 0.0362 -0.2453
-5 5 -1 0.1960 -5.0080 5.0129 -1.0009 -0.1113 0.1472 0.2848
-4 0 -5 0.0807 -4.0024 0.0075 -4.9976 0.0865 0.3226 0.0620
4 0 5 0.0807 4.0024 -0.0075 4.9976 -0.0865 -0.3226 -0.0620

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7028(9)
2 0.2972(9)

# start Validation Reply Form
_vrf_PLAT342_p16030_twin_twin1_hklf4_sq 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02016 Ang.  
RESPONSE: Poor quality data. 
;
# 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_UO2PbLMepyPY-O
_database_code_depnum_ccdc_archive 'CCDC 1480066'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H50 N10 O3 Pb U'
_chemical_formula_sum            'C52 H50 N10 O3 Pb U'
_chemical_formula_weight         1308.24
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H50 N10 O3 U Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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'

_cell_length_a                   13.4429(2)
_cell_length_b                   19.5975(3)
_cell_length_c                   21.9112(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5772.42(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19587
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.4250
_cell_measurement_theta_min      3.4610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 27 3 0.0902
-4 -27 -3 0.0902
-16 2 16 0.2214
16 -2 -16 0.2214
11 -8 24 0.0510
-11 8 -24 0.0510

_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.102
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
3.9893 26.9891 2.9953 -0.4783 0.8819 0.0207
-3.9893 -26.9891 -2.9953 0.4783 -0.8819 -0.0207
-15.9949 2.0037 16.0068 0.0256 -0.0255 -0.9923
15.9949 -2.0037 -16.0068 -0.0256 0.0255 0.9923
11.0008 -7.9956 23.9924 -0.8397 -0.5563 0.1025
-11.0008 7.9956 -23.9924 0.8397 0.5563 -0.1025

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            68331
_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         27.484
_diffrn_reflns_theta_min         2.976
_diffrn_ambient_temperature      170(2)
_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    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-120.00   47
  2  ω    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-180.00   47
  3  ω    -87.00   0.00   1.00   17.50    --  -18.68 -57.00 -90.00   87
  4  ω     34.00  94.00   1.00   17.50    --   20.25 179.00-150.00   60
  5  ω    -48.00  39.00   1.00   17.50    --   20.25 -57.00   0.00   87
  6  ω      2.00  89.00   1.00   17.50    --   20.25  57.00 150.00   87
  7  ω      2.00  43.00   1.00   17.50    --   20.25  57.00  30.00   41
  8  ω    -50.00  43.00   1.00   17.50    --   20.25 -38.00-150.00   93
;
_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      -0.0284663000
_diffrn_orient_matrix_UB_12      -0.0106843000
_diffrn_orient_matrix_UB_13      -0.0255068000
_diffrn_orient_matrix_UB_21      -0.0040073000
_diffrn_orient_matrix_UB_22      0.0343675000
_diffrn_orient_matrix_UB_23      -0.0098975000
_diffrn_orient_matrix_UB_31      0.0442451000
_diffrn_orient_matrix_UB_32      -0.0038543000
_diffrn_orient_matrix_UB_33      -0.0172987000
_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         0.824
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11200
_reflns_number_total             13223
_reflns_odcompleteness_completeness 99.77
_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.
 
 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         3.430
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 
;
 Flack x determined using 4427 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         13223
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.050
_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)+(0.0266P)²+15.7017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0851
_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
C11 \\sim C10 \\sim C9 \\sim C16 \\sim C15 \\sim C13: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
C6 \\sim C7 \\sim N1 \\sim C4 \\sim C5: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C10, C9, C16, C15, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9, C16, C15, C13, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C6, C7, N1, C4, C5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C29(H29), C47(H47), C8(H8), C31(H31), C20(H20), C38(H38),
 C45(H45), C36(H36), C41(H41), C40(H40), C015(H015), C19(H19), C26(H26),
 C10(H10), C43(H43), C51(H51), C6(H6), C5(H5), C48(H48), C27(H27), C52(H52),
 C44(H44), C50(H50), C49(H49)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C33(H33A,H33B,
 H33C), C2(H2A,H2B,H2C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C12(H12A,
 H12B,H12C)
;
_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 0.33464(2) 0.24033(2) 0.75365(2) 0.02683(8) Uani 1 1 d . . . . .
Pb1 Pb 0.50620(2) 0.23985(2) 0.60947(2) 0.03348(9) Uani 1 1 d . . . . .
N6 N 0.6205(6) 0.2048(4) 0.7133(4) 0.036(2) Uani 1 1 d . . . . .
N10 N 0.4582(6) 0.3955(4) 0.7401(5) 0.036(2) Uani 1 1 d . . . . .
O2 O 0.2949(5) 0.2917(4) 0.8148(3) 0.0413(18) Uani 1 1 d . . . . .
N3 N 0.2249(6) 0.3116(4) 0.6845(4) 0.0318(19) Uani 1 1 d . . . . .
N7 N 0.3429(6) 0.3065(4) 0.5772(4) 0.0332(18) Uani 1 1 d . . . . .
N2 N 0.4929(6) 0.2177(4) 0.8162(4) 0.0358(18) Uani 1 1 d . . . . .
O3 O 0.4425(5) 0.3289(3) 0.7239(4) 0.0389(18) Uani 1 1 d . . . . .
O1 O 0.3805(5) 0.1892(4) 0.6883(4) 0.0387(17) Uani 1 1 d . . . . .
N4 N 0.1669(6) 0.1946(4) 0.7423(4) 0.0334(17) Uani 1 1 d . . . . .
N8 N 0.4307(6) 0.1901(4) 0.5255(4) 0.035(2) Uani 1 1 d . . . . .
N5 N 0.5885(5) 0.1338(4) 0.6017(4) 0.0310(18) Uani 1 1 d . . . . .
N1 N 0.3208(7) 0.1412(4) 0.8194(4) 0.0361(17) Uani 1 1 d . U . . .
C15 C 0.7336(7) 0.2874(5) 0.7593(6) 0.041(2) Uani 1 1 d . U . . .
H15 H 0.7755 0.2834 0.7257 0.049 Uiso 1 1 calc R . . . .
C16 C 0.6488(7) 0.2493(4) 0.7607(4) 0.036(2) Uani 1 1 d . U . . .
C30 C 0.3125(6) 0.3702(4) 0.6015(5) 0.029(2) Uani 1 1 d . . . . .
C17 C 0.6888(7) 0.1684(5) 0.6892(5) 0.036(2) Uani 1 1 d . . . . .
H17 H 0.7508 0.1670 0.7081 0.043 Uiso 1 1 calc R . . . .
C37 C 0.2558(7) 0.3735(5) 0.6554(5) 0.030(2) Uani 1 1 d . . . . .
C29 C 0.3312(8) 0.2929(5) 0.5197(5) 0.037(2) Uani 1 1 d . . . . .
H29 H 0.2950 0.3234 0.4959 0.044 Uiso 1 1 calc R . . . .
C9 C 0.5839(6) 0.2556(5) 0.8125(4) 0.0364(19) Uani 1 1 d . U . . .
C39 C 0.0980(6) 0.2396(6) 0.7181(5) 0.038(2) Uani 1 1 d . . . . .
C47 C 0.5035(10) 0.4336(6) 0.6982(6) 0.050(3) Uani 1 1 d . . . . .
H47 H 0.5233 0.4143 0.6614 0.060 Uiso 1 1 calc R . . . .
C4 C 0.2468(9) 0.0977(6) 0.8336(6) 0.045(2) Uani 1 1 d . U . . .
C8 C 0.4731(9) 0.1862(6) 0.8670(5) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.5156 0.1891 0.9005 0.057 Uiso 1 1 calc R . . . .
C21 C 0.5973(8) 0.0903(5) 0.5539(5) 0.038(3) Uani 1 1 d . . . . .
N9 N 0.5990(9) 0.3110(6) 0.5190(6) 0.068(3) Uani 1 1 d . . . . .
C31 C 0.3399(8) 0.4330(5) 0.5747(4) 0.033(2) Uani 1 1 d . . . . .
H31 H 0.3771 0.4323 0.5389 0.039 Uiso 1 1 calc R . . . .
C42 C 0.1170(8) 0.1396(5) 0.7609(6) 0.046(3) Uani 1 1 d . . . . .
C20 C 0.6882(8) 0.0573(6) 0.5569(6) 0.044(3) Uani 1 1 d . . . . .
H20 H 0.7112 0.0242 0.5300 0.053 Uiso 1 1 calc R . . . .
C38 C 0.1316(7) 0.2990(5) 0.6888(5) 0.034(2) Uani 1 1 d . . . . .
H38 H 0.0858 0.3294 0.6723 0.040 Uiso 1 1 calc R . . . .
C45 C 0.4918(11) 0.5292(6) 0.7651(8) 0.066(4) Uani 1 1 d . . . . .
H45 H 0.5026 0.5749 0.7743 0.080 Uiso 1 1 calc R . . . .
C28 C 0.3701(8) 0.2349(5) 0.4918(5) 0.040(2) Uani 1 1 d . . . . .
C36 C 0.2318(8) 0.4367(5) 0.6803(5) 0.036(2) Uani 1 1 d . . . . .
H36 H 0.1954 0.4379 0.7164 0.043 Uiso 1 1 calc R . . . .
C25 C 0.4584(7) 0.1399(5) 0.4870(5) 0.037(2) Uani 1 1 d . . . . .
C22 C 0.5131(8) 0.0766(5) 0.5093(5) 0.042(3) Uani 1 1 d . . . . .
C41 C 0.0145(8) 0.1491(6) 0.7492(7) 0.061(3) Uani 1 1 d . . . . .
H41 H -0.0364 0.1183 0.7577 0.073 Uiso 1 1 calc R . . . .
C40 C 0.0044(8) 0.2116(6) 0.7232(6) 0.061(4) Uani 1 1 d . . . . .
H40 H -0.0549 0.2318 0.7111 0.074 Uiso 1 1 calc R . . . .
C11 C 0.6989(8) 0.3394(6) 0.8556(6) 0.046(2) Uani 1 1 d . U . . .
C3 C 0.2234(9) 0.0428(6) 0.7335(6) 0.052(3) Uani 1 1 d . . . . .
H3A H 0.2730 0.0729 0.7171 0.078 Uiso 1 1 calc GR . . . .
H3B H 0.1763 0.0314 0.7021 0.078 Uiso 1 1 calc GR . . . .
H3C H 0.2548 0.0018 0.7480 0.078 Uiso 1 1 calc GR . . . .
C015 C 0.5212(11) 0.5033(6) 0.7098(8) 0.062(4) Uani 1 1 d . . . . .
H015 H 0.5520 0.5308 0.6808 0.074 Uiso 1 1 calc R . . . .
C19 C 0.7391(8) 0.0825(6) 0.6073(6) 0.045(3) Uani 1 1 d . . . . .
H19 H 0.8027 0.0707 0.6202 0.054 Uiso 1 1 calc R . . . .
C14 C 0.8598(9) 0.3682(6) 0.8004(7) 0.065(4) Uani 1 1 d . . . . .
H14A H 0.9104 0.3416 0.8201 0.098 Uiso 1 1 calc GR . . . .
H14B H 0.8561 0.4123 0.8192 0.098 Uiso 1 1 calc GR . . . .
H14C H 0.8758 0.3734 0.7579 0.098 Uiso 1 1 calc GR . . . .
C26 C 0.4182(9) 0.1525(6) 0.4287(5) 0.047(3) Uani 1 1 d . . . . .
H26 H 0.4258 0.1251 0.3943 0.056 Uiso 1 1 calc R . . . .
C1 C 0.1698(9) 0.0778(6) 0.7862(6) 0.049(3) Uani 1 1 d . . . . .
C18 C 0.6744(8) 0.1293(5) 0.6344(5) 0.035(2) Uani 1 1 d . . . . .
C10 C 0.6096(8) 0.3018(5) 0.8581(6) 0.046(2) Uani 1 1 d . U . . .
H10 H 0.5669 0.3080 0.8910 0.055 Uiso 1 1 calc R . . . .
C43 C 0.4305(9) 0.4198(6) 0.7938(6) 0.048(3) Uani 1 1 d . . . . .
H43 H 0.4005 0.3916 0.8226 0.058 Uiso 1 1 calc R . . . .
C51 C 0.6513(11) 0.3394(8) 0.4208(7) 0.078(5) Uani 1 1 d . . . . .
H51 H 0.6543 0.3280 0.3796 0.094 Uiso 1 1 calc R . . . .
C32 C 0.3141(8) 0.4951(5) 0.5993(6) 0.040(3) Uani 1 1 d . . . . .
C34 C 0.2593(9) 0.4973(5) 0.6539(5) 0.038(3) Uani 1 1 d . . . . .
C24 C 0.5567(9) 0.0385(7) 0.4536(6) 0.059(4) Uani 1 1 d . . . . .
H24A H 0.6107 0.0645 0.4368 0.089 Uiso 1 1 calc GR . . . .
H24B H 0.5059 0.0328 0.4233 0.089 Uiso 1 1 calc GR . . . .
H24C H 0.5807 -0.0054 0.4662 0.089 Uiso 1 1 calc GR . . . .
C6 C 0.3460(10) 0.1049(6) 0.9145(6) 0.057(3) Uani 1 1 d . U . . .
H6 H 0.3741 0.0983 0.9529 0.068 Uiso 1 1 calc R . . . .
C33 C 0.3499(11) 0.5604(6) 0.5674(7) 0.065(4) Uani 1 1 d . . . . .
H33A H 0.3822 0.5486 0.5298 0.097 Uiso 1 1 calc GR . . . .
H33B H 0.3959 0.5839 0.5934 0.097 Uiso 1 1 calc GR . . . .
H33C H 0.2939 0.5893 0.5591 0.097 Uiso 1 1 calc GR . . . .
C5 C 0.2582(10) 0.0741(6) 0.8922(6) 0.057(3) Uani 1 1 d . U . . .
H5 H 0.2167 0.0441 0.9129 0.068 Uiso 1 1 calc R . . . .
C2 C 0.0924(10) 0.0282(7) 0.8150(7) 0.071(4) Uani 1 1 d . . . . .
H2A H 0.1260 -0.0116 0.8301 0.106 Uiso 1 1 calc GR . . . .
H2B H 0.0447 0.0149 0.7846 0.106 Uiso 1 1 calc GR . . . .
H2C H 0.0588 0.0507 0.8480 0.106 Uiso 1 1 calc GR . . . .
C48 C 0.6391(13) 0.3686(9) 0.5371(8) 0.087(5) Uani 1 1 d . . . . .
H48 H 0.6385 0.3781 0.5786 0.105 Uiso 1 1 calc R . . . .
C23 C 0.4390(9) 0.0299(6) 0.5430(7) 0.057(3) Uani 1 1 d . . . . .
H23A H 0.4727 -0.0107 0.5563 0.085 Uiso 1 1 calc GR . . . .
H23B H 0.3859 0.0176 0.5158 0.085 Uiso 1 1 calc GR . . . .
H23C H 0.4124 0.0535 0.5777 0.085 Uiso 1 1 calc GR . . . .
C13 C 0.7607(8) 0.3325(6) 0.8065(6) 0.045(2) Uani 1 1 d . U . . .
C7 C 0.3820(9) 0.1461(5) 0.8696(5) 0.042(2) Uani 1 1 d . U . . .
C27 C 0.3665(8) 0.2114(6) 0.4318(5) 0.040(3) Uani 1 1 d . . . . .
H27 H 0.3341 0.2327 0.3995 0.048 Uiso 1 1 calc R . . . .
C52 C 0.6073(10) 0.2971(8) 0.4608(6) 0.071(4) Uani 1 1 d . . . . .
H52 H 0.5815 0.2561 0.4464 0.085 Uiso 1 1 calc R . . . .
C44 C 0.4469(10) 0.4875(6) 0.8061(8) 0.061(4) Uani 1 1 d . . . . .
H44 H 0.4268 0.5053 0.8434 0.073 Uiso 1 1 calc R . . . .
C35 C 0.2321(11) 0.5645(6) 0.6841(7) 0.061(4) Uani 1 1 d . . . . .
H35A H 0.2023 0.5556 0.7232 0.092 Uiso 1 1 calc GR . . . .
H35B H 0.1857 0.5887 0.6588 0.092 Uiso 1 1 calc GR . . . .
H35C H 0.2910 0.5915 0.6895 0.092 Uiso 1 1 calc GR . . . .
C50 C 0.6910(12) 0.3980(8) 0.4408(8) 0.084(5) Uani 1 1 d . . . . .
H50 H 0.7250 0.4265 0.4141 0.101 Uiso 1 1 calc R . . . .
C49 C 0.6812(14) 0.4151(8) 0.4993(8) 0.090(6) Uani 1 1 d . . . . .
H49 H 0.7025 0.4573 0.5137 0.108 Uiso 1 1 calc R . . . .
C12 C 0.7228(11) 0.3889(8) 0.9059(8) 0.078(5) Uani 1 1 d . . . . .
H12A H 0.7234 0.4344 0.8899 0.117 Uiso 1 1 calc GR . . . .
H12B H 0.7870 0.3783 0.9227 0.117 Uiso 1 1 calc GR . . . .
H12C H 0.6733 0.3854 0.9374 0.117 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 1.759(7) . ?
U1 N3 2.535(8) . ?
U1 N2 2.569(8) . ?
U1 O3 2.355(7) . ?
U1 O1 1.853(8) . ?
U1 N4 2.439(8) . ?
U1 N1 2.426(8) . ?
Pb1 N7 2.650(9) . ?
Pb1 O1 2.613(8) . ?
Pb1 N8 2.316(9) . ?
Pb1 N5 2.361(8) . ?
Pb1 N9 2.725(12) . ?
N6 C16 1.409(11) . ?
N6 C17 1.277(13) . ?
N10 O3 1.369(10) . ?
N10 C47 1.330(14) . ?
N10 C43 1.324(15) . ?
N3 C37 1.431(12) . ?
N3 C38 1.282(12) . ?
N7 C30 1.416(11) . ?
N7 C29 1.297(12) . ?
N2 C9 1.433(12) . ?
N2 C8 1.301(13) . ?
N4 C39 1.385(12) . ?
N4 C42 1.334(12) . ?
N8 C28 1.406(14) . ?
N8 C25 1.348(12) . ?
N5 C21 1.355(13) . ?
N5 C18 1.362(13) . ?
N1 C4 1.345(14) . ?
N1 C7 1.379(14) . ?
C15 H15 0.9300 . ?
C15 C16 1.364(13) . ?
C15 C13 1.408(15) . ?
C16 C9 1.436(13) . ?
C30 C37 1.408(14) . ?
C30 C31 1.413(13) . ?
C17 H17 0.9300 . ?
C17 C18 1.437(14) . ?
C37 C36 1.390(14) . ?
C29 H29 0.9300 . ?
C29 C28 1.393(14) . ?
C9 C10 1.391(14) . ?
C39 C38 1.404(14) . ?
C39 C40 1.378(14) . ?
C47 H47 0.9300 . ?
C47 C015 1.409(15) . ?
C4 C1 1.519(17) . ?
C4 C5 1.372(16) . ?
C8 H8 0.9300 . ?
C8 C7 1.456(17) . ?
C21 C20 1.385(14) . ?
C21 C22 1.518(16) . ?
N9 C48 1.312(17) . ?
N9 C52 1.310(17) . ?
C31 H31 0.9300 . ?
C31 C32 1.375(14) . ?
C42 C41 1.413(16) . ?
C42 C1 1.508(16) . ?
C20 H20 0.9300 . ?
C20 C19 1.389(17) . ?
C38 H38 0.9300 . ?
C45 H45 0.9300 . ?
C45 C015 1.37(2) . ?
C45 C44 1.36(2) . ?
C28 C27 1.393(14) . ?
C36 H36 0.9300 . ?
C36 C34 1.372(15) . ?
C25 C22 1.523(15) . ?
C25 C26 1.410(15) . ?
C22 C24 1.546(15) . ?
C22 C23 1.541(16) . ?
C41 H41 0.9300 . ?
C41 C40 1.358(16) . ?
C40 H40 0.9300 . ?
C11 C10 1.409(16) . ?
C11 C13 1.366(17) . ?
C11 C12 1.504(17) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C1 1.525(17) . ?
C015 H015 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.397(14) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C13 1.510(16) . ?
C26 H26 0.9300 . ?
C26 C27 1.349(15) . ?
C1 C2 1.558(15) . ?
C10 H10 0.9300 . ?
C43 H43 0.9300 . ?
C43 C44 1.372(15) . ?
C51 H51 0.9300 . ?
C51 C52 1.343(19) . ?
C51 C50 1.34(2) . ?
C32 C34 1.406(17) . ?
C32 C33 1.535(15) . ?
C34 C35 1.519(15) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C6 H6 0.9300 . ?
C6 C5 1.414(18) . ?
C6 C7 1.361(15) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C5 H5 0.9300 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C48 H48 0.9300 . ?
C48 C49 1.36(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C27 H27 0.9300 . ?
C52 H52 0.9300 . ?
C44 H44 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C50 H50 0.9300 . ?
C50 C49 1.33(2) . ?
C49 H49 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 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
O2 U1 N3 87.8(3) . . ?
O2 U1 N2 86.8(3) . . ?
O2 U1 O3 88.6(3) . . ?
O2 U1 O1 177.5(3) . . ?
O2 U1 N4 90.4(3) . . ?
O2 U1 N1 89.0(3) . . ?
N3 U1 N2 153.6(3) . . ?
O3 U1 N3 77.7(2) . . ?
O3 U1 N2 76.4(3) . . ?
O3 U1 N4 144.3(2) . . ?
O3 U1 N1 143.4(3) . . ?
O1 U1 N3 91.8(3) . . ?
O1 U1 N2 92.5(3) . . ?
O1 U1 O3 88.9(3) . . ?
O1 U1 N4 91.7(3) . . ?
O1 U1 N1 92.9(3) . . ?
N4 U1 N3 66.7(3) . . ?
N4 U1 N2 139.1(3) . . ?
N1 U1 N3 138.7(3) . . ?
N1 U1 N2 67.0(3) . . ?
N1 U1 N4 72.2(3) . . ?
N7 Pb1 N9 86.2(3) . . ?
O1 Pb1 N7 80.1(2) . . ?
O1 Pb1 N9 166.3(3) . . ?
N8 Pb1 N7 68.4(3) . . ?
N8 Pb1 O1 94.7(3) . . ?
N8 Pb1 N5 77.1(3) . . ?
N8 Pb1 N9 80.7(3) . . ?
N5 Pb1 N7 143.4(3) . . ?
N5 Pb1 O1 90.9(3) . . ?
N5 Pb1 N9 100.6(3) . . ?
C17 N6 C16 117.2(8) . . ?
C47 N10 O3 115.3(9) . . ?
C43 N10 O3 122.0(9) . . ?
C43 N10 C47 122.7(10) . . ?
C37 N3 U1 124.4(6) . . ?
C38 N3 U1 114.8(7) . . ?
C38 N3 C37 118.7(8) . . ?
C30 N7 Pb1 125.0(6) . . ?
C29 N7 Pb1 105.0(7) . . ?
C29 N7 C30 120.7(8) . . ?
C9 N2 U1 126.0(6) . . ?
C8 N2 U1 111.7(7) . . ?
C8 N2 C9 117.9(9) . . ?
N10 O3 U1 136.6(6) . . ?
U1 O1 Pb1 121.3(3) . . ?
C39 N4 U1 115.1(6) . . ?
C42 N4 U1 137.0(7) . . ?
C42 N4 C39 107.1(8) . . ?
C28 N8 Pb1 114.1(6) . . ?
C25 N8 Pb1 133.1(7) . . ?
C25 N8 C28 106.7(9) . . ?
C21 N5 Pb1 130.5(7) . . ?
C21 N5 C18 107.0(8) . . ?
C18 N5 Pb1 114.6(6) . . ?
C4 N1 U1 134.5(7) . . ?
C4 N1 C7 107.5(9) . . ?
C7 N1 U1 111.9(7) . . ?
C16 C15 H15 118.5 . . ?
C16 C15 C13 122.9(11) . . ?
C13 C15 H15 118.5 . . ?
N6 C16 C9 118.2(8) . . ?
C15 C16 N6 123.2(9) . . ?
C15 C16 C9 118.6(9) . . ?
C37 C30 N7 120.8(8) . . ?
C37 C30 C31 116.7(9) . . ?
C31 C30 N7 122.4(9) . . ?
N6 C17 H17 118.4 . . ?
N6 C17 C18 123.1(9) . . ?
C18 C17 H17 118.4 . . ?
C30 C37 N3 119.5(9) . . ?
C36 C37 N3 120.8(9) . . ?
C36 C37 C30 119.7(9) . . ?
N7 C29 H29 118.4 . . ?
N7 C29 C28 123.3(10) . . ?
C28 C29 H29 118.4 . . ?
N2 C9 C16 121.2(8) . . ?
C10 C9 N2 120.6(10) . . ?
C10 C9 C16 118.1(9) . . ?
N4 C39 C38 119.3(8) . . ?
C40 C39 N4 109.0(9) . . ?
C40 C39 C38 131.4(10) . . ?
N10 C47 H47 120.1 . . ?
N10 C47 C015 119.8(12) . . ?
C015 C47 H47 120.1 . . ?
N1 C4 C1 120.5(10) . . ?
N1 C4 C5 110.3(11) . . ?
C5 C4 C1 129.0(11) . . ?
N2 C8 H8 121.2 . . ?
N2 C8 C7 117.5(11) . . ?
C7 C8 H8 121.2 . . ?
N5 C21 C20 109.5(10) . . ?
N5 C21 C22 122.9(9) . . ?
C20 C21 C22 127.3(10) . . ?
C48 N9 Pb1 114.2(11) . . ?
C52 N9 Pb1 129.9(9) . . ?
C52 N9 C48 115.9(14) . . ?
C30 C31 H31 118.6 . . ?
C32 C31 C30 122.8(10) . . ?
C32 C31 H31 118.6 . . ?
N4 C42 C41 109.2(10) . . ?
N4 C42 C1 121.6(9) . . ?
C41 C42 C1 129.1(10) . . ?
C21 C20 H20 126.1 . . ?
C21 C20 C19 107.8(10) . . ?
C19 C20 H20 126.1 . . ?
N3 C38 C39 120.5(9) . . ?
N3 C38 H38 119.7 . . ?
C39 C38 H38 119.7 . . ?
C015 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
C44 C45 C015 119.4(12) . . ?
C29 C28 N8 119.7(9) . . ?
C27 C28 N8 108.0(9) . . ?
C27 C28 C29 132.1(11) . . ?
C37 C36 H36 118.6 . . ?
C34 C36 C37 122.9(10) . . ?
C34 C36 H36 118.6 . . ?
N8 C25 C22 121.8(10) . . ?
N8 C25 C26 109.5(10) . . ?
C26 C25 C22 128.2(10) . . ?
C21 C22 C25 115.0(8) . . ?
C21 C22 C24 108.1(9) . . ?
C21 C22 C23 106.2(10) . . ?
C25 C22 C24 108.9(10) . . ?
C25 C22 C23 109.0(9) . . ?
C23 C22 C24 109.6(9) . . ?
C42 C41 H41 126.5 . . ?
C40 C41 C42 107.0(10) . . ?
C40 C41 H41 126.5 . . ?
C39 C40 H40 126.2 . . ?
C41 C40 C39 107.6(10) . . ?
C41 C40 H40 126.2 . . ?
C10 C11 C12 119.4(12) . . ?
C13 C11 C10 119.8(11) . . ?
C13 C11 C12 120.7(12) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
C47 C015 H015 121.0 . . ?
C45 C015 C47 118.0(14) . . ?
C45 C015 H015 121.0 . . ?
C20 C19 H19 127.3 . . ?
C20 C19 C18 105.4(10) . . ?
C18 C19 H19 127.3 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C25 C26 H26 126.3 . . ?
C27 C26 C25 107.5(9) . . ?
C27 C26 H26 126.3 . . ?
C4 C1 C3 108.1(10) . . ?
C4 C1 C2 109.8(10) . . ?
C42 C1 C4 111.5(9) . . ?
C42 C1 C3 107.9(10) . . ?
C42 C1 C2 109.6(10) . . ?
C3 C1 C2 110.0(10) . . ?
N5 C18 C17 121.4(9) . . ?
N5 C18 C19 110.2(10) . . ?
C19 C18 C17 128.5(10) . . ?
C9 C10 C11 121.6(11) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
N10 C43 H43 120.8 . . ?
N10 C43 C44 118.5(13) . . ?
C44 C43 H43 120.8 . . ?
C52 C51 H51 120.3 . . ?
C50 C51 H51 120.3 . . ?
C50 C51 C52 119.3(14) . . ?
C31 C32 C34 119.6(10) . . ?
C31 C32 C33 118.7(11) . . ?
C34 C32 C33 121.7(10) . . ?
C36 C34 C32 118.3(10) . . ?
C36 C34 C35 120.1(11) . . ?
C32 C34 C35 121.6(11) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C5 C6 H6 126.3 . . ?
C7 C6 H6 126.3 . . ?
C7 C6 C5 107.4(11) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 C5 C6 105.9(11) . . ?
C4 C5 H5 127.1 . . ?
C6 C5 H5 127.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N9 C48 H48 117.7 . . ?
N9 C48 C49 124.6(16) . . ?
C49 C48 H48 117.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C13 C14 117.0(12) . . ?
C11 C13 C15 118.9(11) . . ?
C11 C13 C14 124.1(11) . . ?
N1 C7 C8 120.6(10) . . ?
C6 C7 N1 108.9(11) . . ?
C6 C7 C8 130.3(12) . . ?
C28 C27 H27 125.9 . . ?
C26 C27 C28 108.3(10) . . ?
C26 C27 H27 125.9 . . ?
N9 C52 C51 123.1(14) . . ?
N9 C52 H52 118.5 . . ?
C51 C52 H52 118.5 . . ?
C45 C44 C43 121.6(15) . . ?
C45 C44 H44 119.2 . . ?
C43 C44 H44 119.2 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C51 C50 H50 120.3 . . ?
C49 C50 C51 119.5(15) . . ?
C49 C50 H50 120.3 . . ?
C48 C49 H49 121.4 . . ?
C50 C49 C48 117.3(15) . . ?
C50 C49 H49 121.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_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 1.654
_oxdiff_exptl_absorpt_empirical_full_min 0.734

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.059 -0.250 0.500 627 214 ' '
2 -0.084 0.250 0.000 626 214 ' '
3 0.240 0.098 0.330 12 1 ' '
4 0.260 0.902 0.830 13 0 ' '
5 0.740 0.402 0.670 13 0 ' '
6 0.760 0.598 0.170 13 1 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_UO2PbLMepy
_database_code_depnum_ccdc_archive 'CCDC 1480068'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H50 N10 O2 Pb U'
_chemical_formula_sum            'C52 H50 N10 O2 Pb U'
_chemical_formula_weight         1292.24
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H100 N8 U O2 Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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'

_cell_length_a                   10.8424(3)
_cell_length_b                   15.8907(3)
_cell_length_c                   33.2881(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5735.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10887
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      20.4980
_cell_measurement_theta_min      2.9240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.1237
_exptl_crystal_size_mid          0.1188
_exptl_crystal_size_min          0.0469
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            11715
_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         26.372
_diffrn_reflns_theta_min         2.841
_diffrn_ambient_temperature      170(2)
_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000  -30.0000 49

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000 -180.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega  -91.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089 -179.0000  120.0000 57

#__ type_ start__ end____ width___ exp.time_
  4 omega  -35.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089   57.0000  -60.0000 87

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000    0.0000 49

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   19.0000   30.0000 110

#__ type_ start__ end____ width___ exp.time_
  7 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
  8 omega  -20.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   19.0000   90.0000 110

#__ type_ start__ end____ width___ exp.time_
  9 omega  -74.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  129.0000   84.0083 74

#__ type_ start__ end____ width___ exp.time_
 10 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000 -120.0000 87

#__ type_ start__ end____ width___ exp.time_
 11 omega  -18.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714 -107.0000   -6.2344 81

#__ type_ start__ end____ width___ exp.time_
 12 omega   -1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714   57.0000  -60.0000 87

#__ type_ start__ end____ width___ exp.time_
 13 omega  -51.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8714  -57.0000   30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0176164000
_diffrn_orient_matrix_UB_12      -0.0076983000
_diffrn_orient_matrix_UB_13      0.0201885000
_diffrn_orient_matrix_UB_21      -0.0272044000
_diffrn_orient_matrix_UB_22      -0.0386882000
_diffrn_orient_matrix_UB_23      -0.0058790000
_diffrn_orient_matrix_UB_31      0.0568278000
_diffrn_orient_matrix_UB_32      -0.0208914000
_diffrn_orient_matrix_UB_33      0.0034420000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8552
_reflns_number_total             11715
_reflns_odcompleteness_completeness 99.72
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         2.589
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 
;
 Flack x determined using 2540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(7)
_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     591
_refine_ls_number_reflns         11715
_refine_ls_number_restraints     507
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0828
_refine_ls_restrained_S_all      1.045
_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)+(0.0622P)²+28.3352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1576
_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
N00A \\sim N00G \\sim C00H \\sim C010: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N005 \\sim C00S \\sim C00X \\sim C00Y \\sim C00Z \\sim C016: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N00V \\sim C01T \\sim C01O \\sim C027 \\sim C01I \\sim C013: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C00T \\sim C00Y \\sim C01P: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N00A \\sim C00S \\sim C01C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N007 \\sim C00M \\sim C017 \\sim C01H \\sim C01J: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N006 \\sim C00E \\sim N00I \\sim C00J \\sim C00W \\sim C01A \\sim C01E \\sim
C01L: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C00E \\sim C01E \\sim N00I: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
N008 \\sim C00D \\sim C00K \\sim C012 \\sim C00N: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C019 \\sim C00O \\sim C010 \\sim C00H \\sim C00L \\sim C00U: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 N00A, N00G, C00H, C010
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N005, C00S, C00X, C00Y, C00Z, C016
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00V, C01T, C01O, C027, C01I, C013
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00T, C00Y, C01P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00A, C00S, C01C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N007, C00M, C017, C01H, C01J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N006, C00E, N00I, C00J, C00W, C01A, C01E, C01L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00I, C00E, C01E
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N008, C00D, C00K, C012, C00N
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C00O, C010, C00H, C00L, C00U, C019
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00F(H00F), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O),
 C00Q(H00Q), C01T(H01T), C01O(H01O), C027(H027), C01I(H01I), C013(H013),
 C00Z(H00Z), C011(H011), C012(H012), C015(H015), C016(H016), C018(H018),
 C01A(H01D), C01B(H01E), C01C(H01F), C01F(H01K), C01H(H01P), C01J(H01Q),
 C01M(H01R), C01V(H0AA)
4.b Fitted hexagon refined as free rotating group:
 N00V(C01T,C01O,C027,C01I,C013)
4.c Idealised Me refined as rotating group:
 C00T(H00A,H00C,H00D), C014(H01A,H01B,H01C), C01D(H01G,H01H,H01J), C01G(H01L,
 H01M,H01N), C01N(H01S,H01U,H01V), C01P(H01W,H01X,H01Y), C01Q(H01Z,H,HA),
 C01R(H01,HB,HC)
;
_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
U001 U 0.44815(8) 0.16574(5) 0.57913(2) 0.0376(2) Uani 1 1 d . . . . .
Pb00 Pb 0.47509(8) 0.28921(5) 0.70145(2) 0.0414(2) Uani 1 1 d . . . . .
O003 O 0.4832(11) 0.1821(8) 0.6306(4) 0.039(3) Uani 1 1 d . . . . .
N004 N 0.3757(14) 0.3186(10) 0.5667(5) 0.034(4) Uani 1 1 d . . . . .
N005 N 0.4137(15) 0.1855(9) 0.7455(5) 0.035(4) Uani 1 1 d . U . . .
N006 N 0.6708(16) 0.3307(11) 0.6470(5) 0.038(4) Uani 1 1 d . U . . .
N007 N 0.6228(17) 0.0661(10) 0.5725(4) 0.038(4) Uani 1 1 d . U . . .
N008 N 0.6582(15) 0.2304(11) 0.7191(5) 0.041(3) Uani 1 1 d . U . . .
O009 O 0.4142(12) 0.1584(9) 0.5273(4) 0.041(3) Uani 1 1 d . . . . .
N00A N 0.2400(16) 0.2229(13) 0.6864(5) 0.049(5) Uani 1 1 d . U . . .
C00B C 0.3725(19) 0.3746(17) 0.5962(7) 0.049(7) Uani 1 1 d . . . . .
H00B H 0.3975 0.3582 0.6218 0.059 Uiso 1 1 calc R . . . .
N00C N 0.3721(17) 0.0254(11) 0.5907(5) 0.040(4) Uani 1 1 d . . . . .
C00D C 0.7559(18) 0.2297(13) 0.6909(6) 0.038(3) Uani 1 1 d . U . . .
C00E C 0.6679(18) 0.3262(14) 0.5723(6) 0.037(4) Uani 1 1 d . U . . .
C00F C 0.3326(18) 0.3457(15) 0.5303(6) 0.041(5) Uani 1 1 d . . . . .
H00F H 0.3322 0.3081 0.5089 0.049 Uiso 1 1 calc R . . . .
N00G N 0.2246(16) 0.1664(13) 0.6050(5) 0.044(4) Uani 1 1 d . U . . .
C00H C 0.1621(17) 0.2655(14) 0.6589(6) 0.036(4) Uani 1 1 d . U . . .
N00I N 0.6558(14) 0.2358(10) 0.5712(5) 0.034(4) Uani 1 1 d . U . . .
C00J C 0.658(2) 0.3723(14) 0.5367(7) 0.047(5) Uani 1 1 d . U . . .
H00J H 0.6548 0.3425 0.5127 0.056 Uiso 1 1 calc R . . . .
C00K C 0.8415(18) 0.1688(15) 0.7036(7) 0.046(4) Uani 1 1 d . U . . .
H00K H 0.9150 0.1556 0.6907 0.055 Uiso 1 1 calc R . . . .
C00L C 0.1026(18) 0.3401(15) 0.6688(6) 0.042(4) Uani 1 1 d . U . . .
H00L H 0.1052 0.3582 0.6954 0.051 Uiso 1 1 calc R . . . .
C00M C 0.637(2) -0.0173(13) 0.5719(6) 0.045(5) Uani 1 1 d . U . . .
C00N C 0.6846(19) 0.1690(16) 0.7477(7) 0.046(4) Uani 1 1 d . U . . .
C00O C 0.0948(16) 0.2864(14) 0.5910(6) 0.038(4) Uani 1 1 d . U . . .
H00O H 0.0874 0.2678 0.5646 0.046 Uiso 1 1 calc R . . . .
C00P C 0.417(2) -0.0532(14) 0.5886(6) 0.048(6) Uani 1 1 d . . . . .
C00Q C 0.757(2) 0.2800(13) 0.6566(6) 0.037(5) Uani 1 1 d . . . . .
H00Q H 0.8244 0.2763 0.6396 0.045 Uiso 1 1 calc R . . . .
C00R C 0.530(2) -0.0760(12) 0.5630(6) 0.051(6) Uani 1 1 d . . . . .
C00S C 0.289(2) 0.1747(15) 0.7506(6) 0.044(4) Uani 1 1 d . U . . .
C00T C 0.648(3) 0.0693(17) 0.8036(9) 0.084(9) Uani 1 1 d . U . . .
H00A H 0.6396 0.0255 0.7839 0.127 Uiso 1 1 calc GR . . . .
H00C H 0.5972 0.0569 0.8264 0.127 Uiso 1 1 calc GR . . . .
H00D H 0.7328 0.0728 0.8120 0.127 Uiso 1 1 calc GR . . . .
C00U C 0.040(2) 0.3887(13) 0.6413(6) 0.043(4) Uani 1 1 d . U . . .
N00V N 0.4745(16) 0.3806(9) 0.7654(4) 0.062(5) Uani 1 1 d . U . . .
C01T C 0.5491(15) 0.4513(10) 0.7688(5) 0.078(6) Uani 1 1 d G U . . .
H01T H 0.6129 0.4600 0.7507 0.093 Uiso 1 1 calc R . . . .
C01O C 0.5282(18) 0.5091(8) 0.7995(5) 0.088(7) Uani 1 1 d G U . . .
H01O H 0.5781 0.5564 0.8018 0.105 Uiso 1 1 calc R . . . .
C027 C 0.433(2) 0.4961(10) 0.8266(5) 0.083(7) Uani 1 1 d G U . . .
H027 H 0.4187 0.5347 0.8471 0.099 Uiso 1 1 calc R . . . .
C01I C 0.3581(16) 0.4253(12) 0.8232(5) 0.090(8) Uani 1 1 d G U . . .
H01I H 0.2942 0.4166 0.8413 0.108 Uiso 1 1 calc R . . . .
C013 C 0.3790(15) 0.3676(9) 0.7926(5) 0.067(6) Uani 1 1 d G U . . .
H013 H 0.3291 0.3202 0.7903 0.081 Uiso 1 1 calc R . . . .
C00W C 0.651(2) 0.4571(15) 0.5347(7) 0.050(5) Uani 1 1 d . U . . .
C00X C 0.469(2) 0.1536(14) 0.7786(6) 0.050(5) Uani 1 1 d . U . . .
C00Y C 0.607(2) 0.1555(16) 0.7848(6) 0.051(5) Uani 1 1 d . U . . .
C00Z C 0.267(2) 0.1372(16) 0.7885(7) 0.062(6) Uani 1 1 d . U . . .
H00Z H 0.1904 0.1262 0.8002 0.074 Uiso 1 1 calc R . . . .
C010 C 0.1589(18) 0.2367(13) 0.6176(6) 0.035(4) Uani 1 1 d . U . . .
C011 C 0.201(2) 0.0930(15) 0.6217(7) 0.049(6) Uani 1 1 d . . . . .
H011 H 0.1350 0.0890 0.6395 0.059 Uiso 1 1 calc R . . . .
C012 C 0.7979(19) 0.1316(15) 0.7387(7) 0.048(4) Uani 1 1 d . U . . .
H012 H 0.8370 0.0897 0.7534 0.057 Uiso 1 1 calc R . . . .
C014 C 0.499(3) -0.0656(14) 0.5169(7) 0.073(9) Uani 1 1 d . . . . .
H01A H 0.5124 -0.0083 0.5090 0.110 Uiso 1 1 calc GR . . . .
H01B H 0.4142 -0.0803 0.5122 0.110 Uiso 1 1 calc GR . . . .
H01C H 0.5513 -0.1019 0.5014 0.110 Uiso 1 1 calc GR . . . .
C015 C 0.291(2) 0.4235(13) 0.5241(7) 0.050(6) Uani 1 1 d . . . . .
H015 H 0.2628 0.4391 0.4989 0.060 Uiso 1 1 calc R . . . .
C016 C 0.384(2) 0.1201(16) 0.8048(8) 0.061(6) Uani 1 1 d . U . . .
H016 H 0.4011 0.0916 0.8286 0.073 Uiso 1 1 calc R . . . .
C017 C 0.738(2) 0.1008(14) 0.5777(7) 0.045(4) Uani 1 1 d . U . . .
C018 C 0.750(2) 0.1871(15) 0.5763(6) 0.048(6) Uani 1 1 d . . . . .
H018 H 0.8282 0.2110 0.5790 0.057 Uiso 1 1 calc R . . . .
C019 C 0.042(2) 0.3612(13) 0.6010(6) 0.043(4) Uani 1 1 d . U . . .
C01A C 0.663(2) 0.4591(14) 0.6064(7) 0.046(5) Uani 1 1 d . U . . .
H01D H 0.6646 0.4902 0.6301 0.055 Uiso 1 1 calc R . . . .
C01B C 0.334(2) 0.4555(18) 0.5905(7) 0.064(8) Uani 1 1 d . . . . .
H01E H 0.3370 0.4943 0.6113 0.077 Uiso 1 1 calc R . . . .
C01C C 0.201(2) 0.2017(16) 0.7205(7) 0.053(6) Uani 1 1 d . U . . .
H01F H 0.1169 0.2033 0.7263 0.064 Uiso 1 1 calc R . . . .
C01D C 0.568(3) -0.1704(15) 0.5702(8) 0.073(8) Uani 1 1 d . . . . .
H01G H 0.6455 -0.1812 0.5572 0.110 Uiso 1 1 calc GR . . . .
H01H H 0.5060 -0.2070 0.5592 0.110 Uiso 1 1 calc GR . . . .
H01J H 0.5761 -0.1806 0.5985 0.110 Uiso 1 1 calc GR . . . .
C01E C 0.669(2) 0.3725(14) 0.6091(7) 0.042(4) Uani 1 1 d . U . . .
C01F C 0.341(3) -0.1085(15) 0.6093(8) 0.069(8) Uani 1 1 d . . . . .
H01K H 0.3516 -0.1663 0.6122 0.083 Uiso 1 1 calc R . . . .
C01G C -0.020(2) 0.4147(16) 0.5693(6) 0.063(7) Uani 1 1 d . . . . .
H01L H 0.0039 0.3950 0.5431 0.094 Uiso 1 1 calc GR . . . .
H01M H 0.0057 0.4722 0.5725 0.094 Uiso 1 1 calc GR . . . .
H01N H -0.1076 0.4109 0.5721 0.094 Uiso 1 1 calc GR . . . .
C01H C 0.760(2) -0.0387(15) 0.5765(7) 0.053(5) Uani 1 1 d . U . . .
H01P H 0.7933 -0.0925 0.5767 0.064 Uiso 1 1 calc R . . . .
C01J C 0.823(2) 0.0374(14) 0.5808(7) 0.054(5) Uani 1 1 d . U . . .
H01Q H 0.9070 0.0438 0.5849 0.064 Uiso 1 1 calc R . . . .
C01K C 0.269(3) 0.0226(15) 0.6139(7) 0.055(7) Uani 1 1 d . . . . .
C01L C 0.656(3) 0.5032(16) 0.5693(8) 0.065(7) Uani 1 1 d . U . . .
C01M C 0.290(2) 0.4783(15) 0.5539(8) 0.057(7) Uani 1 1 d . . . . .
H01R H 0.2603 0.5324 0.5497 0.069 Uiso 1 1 calc R . . . .
C01N C 0.641(3) 0.5974(17) 0.5699(8) 0.083(10) Uani 1 1 d . . . . .
H01S H 0.6391 0.6181 0.5428 0.125 Uiso 1 1 calc GR . . . .
H01U H 0.7097 0.6223 0.5839 0.125 Uiso 1 1 calc GR . . . .
H01V H 0.5659 0.6117 0.5833 0.125 Uiso 1 1 calc GR . . . .
C01P C 0.635(2) 0.2241(17) 0.8156(7) 0.061(7) Uani 1 1 d . U . . .
H01W H 0.7222 0.2244 0.8214 0.092 Uiso 1 1 calc GR . . . .
H01X H 0.5901 0.2132 0.8398 0.092 Uiso 1 1 calc GR . . . .
H01Y H 0.6117 0.2779 0.8049 0.092 Uiso 1 1 calc GR . . . .
C01Q C -0.017(2) 0.4691(15) 0.6546(7) 0.064(7) Uani 1 1 d . . . . .
H01Z H 0.0114 0.4824 0.6812 0.096 Uiso 1 1 calc GR . . . .
H H -0.1047 0.4637 0.6546 0.096 Uiso 1 1 calc GR . . . .
HA H 0.0073 0.5133 0.6365 0.096 Uiso 1 1 calc GR . . . .
C01R C 0.636(2) 0.4993(17) 0.4927(8) 0.063(7) Uani 1 1 d . . . . .
H01 H 0.7148 0.5007 0.4793 0.095 Uiso 1 1 calc GR . . . .
HB H 0.6062 0.5557 0.4961 0.095 Uiso 1 1 calc GR . . . .
HC H 0.5788 0.4675 0.4769 0.095 Uiso 1 1 calc GR . . . .
C01V C 0.246(3) -0.0598(15) 0.6245(8) 0.066(8) Uani 1 1 d . . . . .
H0AA H 0.1786 -0.0792 0.6393 0.079 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
U001 O003 1.773(12) . ?
U001 N004 2.585(16) . ?
U001 N007 2.478(16) . ?
U001 O009 1.766(12) . ?
U001 N00C 2.409(17) . ?
U001 N00G 2.572(17) . ?
U001 N00I 2.525(16) . ?
Pb00 N005 2.303(15) . ?
Pb00 N008 2.271(16) . ?
Pb00 N00V 2.577(11) . ?
N004 C00B 1.33(3) . ?
N004 C00F 1.37(2) . ?
N005 C00S 1.37(3) . ?
N005 C00X 1.35(3) . ?
N006 C00Q 1.27(3) . ?
N006 C01E 1.43(3) . ?
N007 C00M 1.33(2) . ?
N007 C017 1.38(3) . ?
N008 C00D 1.42(3) . ?
N008 C00N 1.39(3) . ?
N00A C00H 1.42(3) . ?
N00A C01C 1.26(3) . ?
C00B H00B 0.9300 . ?
C00B C01B 1.37(3) . ?
N00C C00P 1.34(3) . ?
N00C C01K 1.36(3) . ?
C00D C00K 1.41(3) . ?
C00D C00Q 1.39(3) . ?
C00E N00I 1.44(2) . ?
C00E C00J 1.40(3) . ?
C00E C01E 1.43(3) . ?
C00F H00F 0.9300 . ?
C00F C015 1.33(3) . ?
N00G C010 1.39(3) . ?
N00G C011 1.32(3) . ?
C00H C00L 1.39(3) . ?
C00H C010 1.45(3) . ?
N00I C018 1.30(2) . ?
C00J H00J 0.9300 . ?
C00J C00W 1.35(3) . ?
C00K H00K 0.9300 . ?
C00K C012 1.39(3) . ?
C00L H00L 0.9300 . ?
C00L C00U 1.38(3) . ?
C00M C00R 1.52(3) . ?
C00M C01H 1.38(3) . ?
C00N C00Y 1.51(3) . ?
C00N C012 1.40(3) . ?
C00O H00O 0.9300 . ?
C00O C010 1.37(3) . ?
C00O C019 1.36(3) . ?
C00P C00R 1.53(3) . ?
C00P C01F 1.39(3) . ?
C00Q H00Q 0.9300 . ?
C00R C014 1.58(3) . ?
C00R C01D 1.58(3) . ?
C00S C00Z 1.42(3) . ?
C00S C01C 1.45(3) . ?
C00T H00A 0.9600 . ?
C00T H00C 0.9600 . ?
C00T H00D 0.9600 . ?
C00T C00Y 1.57(4) . ?
C00U C019 1.41(3) . ?
C00U C01Q 1.48(3) . ?
N00V C01T 1.3900 . ?
N00V C013 1.3900 . ?
C01T H01T 0.9300 . ?
C01T C01O 1.3900 . ?
C01O H01O 0.9300 . ?
C01O C027 1.3900 . ?
C027 H027 0.9300 . ?
C027 C01I 1.3900 . ?
C01I H01I 0.9300 . ?
C01I C013 1.3900 . ?
C013 H013 0.9300 . ?
C00W C01L 1.37(3) . ?
C00W C01R 1.56(3) . ?
C00X C00Y 1.52(3) . ?
C00X C016 1.37(3) . ?
C00Y C01P 1.53(3) . ?
C00Z H00Z 0.9300 . ?
C00Z C016 1.41(3) . ?
C011 H011 0.9300 . ?
C011 C01K 1.36(3) . ?
C012 H012 0.9300 . ?
C014 H01A 0.9600 . ?
C014 H01B 0.9600 . ?
C014 H01C 0.9600 . ?
C015 H015 0.9300 . ?
C015 C01M 1.32(3) . ?
C016 H016 0.9300 . ?
C017 C018 1.38(3) . ?
C017 C01J 1.37(3) . ?
C018 H018 0.9300 . ?
C019 C01G 1.51(3) . ?
C01A H01D 0.9300 . ?
C01A C01E 1.38(3) . ?
C01A C01L 1.42(3) . ?
C01B H01E 0.9300 . ?
C01B C01M 1.35(3) . ?
C01C H01F 0.9300 . ?
C01D H01G 0.9600 . ?
C01D H01H 0.9600 . ?
C01D H01J 0.9600 . ?
C01F H01K 0.9300 . ?
C01F C01V 1.39(4) . ?
C01G H01L 0.9600 . ?
C01G H01M 0.9600 . ?
C01G H01N 0.9600 . ?
C01H H01P 0.9300 . ?
C01H C01J 1.40(3) . ?
C01J H01Q 0.9300 . ?
C01K C01V 1.38(3) . ?
C01L C01N 1.51(3) . ?
C01M H01R 0.9300 . ?
C01N H01S 0.9600 . ?
C01N H01U 0.9600 . ?
C01N H01V 0.9600 . ?
C01P H01W 0.9600 . ?
C01P H01X 0.9600 . ?
C01P H01Y 0.9600 . ?
C01Q H01Z 0.9600 . ?
C01Q H 0.9600 . ?
C01Q HA 0.9600 . ?
C01R H01 0.9600 . ?
C01R HB 0.9600 . ?
C01R HC 0.9600 . ?
C01V H0AA 0.9300 . ?

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
O003 U001 N004 94.7(5) . . ?
O003 U001 N007 90.9(5) . . ?
O003 U001 N00C 93.2(6) . . ?
O003 U001 N00G 83.0(6) . . ?
O003 U001 N00I 81.1(6) . . ?
N007 U001 N004 144.9(5) . . ?
N007 U001 N00G 138.8(6) . . ?
N007 U001 N00I 65.9(6) . . ?
O009 U001 O003 175.3(6) . . ?
O009 U001 N004 81.0(6) . . ?
O009 U001 N007 91.8(5) . . ?
O009 U001 N00C 91.3(6) . . ?
O009 U001 N00G 97.5(6) . . ?
O009 U001 N00I 96.4(6) . . ?
N00C U001 N004 142.3(6) . . ?
N00C U001 N007 71.6(6) . . ?
N00C U001 N00G 68.1(6) . . ?
N00C U001 N00I 136.9(6) . . ?
N00G U001 N004 76.3(6) . . ?
N00I U001 N004 80.8(5) . . ?
N00I U001 N00G 150.9(5) . . ?
N005 Pb00 N00V 82.9(5) . . ?
N008 Pb00 N005 78.1(6) . . ?
N008 Pb00 N00V 91.2(6) . . ?
C00B N004 U001 121.4(13) . . ?
C00B N004 C00F 115.8(18) . . ?
C00F N004 U001 122.7(14) . . ?
C00S N005 Pb00 117.0(13) . . ?
C00X N005 Pb00 131.3(14) . . ?
C00X N005 C00S 106.6(17) . . ?
C00Q N006 C01E 121.9(17) . . ?
C00M N007 U001 136.3(16) . . ?
C00M N007 C017 107.2(18) . . ?
C017 N007 U001 115.3(13) . . ?
C00D N008 Pb00 119.1(13) . . ?
C00N N008 Pb00 130.1(14) . . ?
C00N N008 C00D 107.1(17) . . ?
C01C N00A C00H 121(2) . . ?
N004 C00B H00B 118.8 . . ?
N004 C00B C01B 122(2) . . ?
C01B C00B H00B 118.8 . . ?
C00P N00C U001 136.7(15) . . ?
C00P N00C C01K 107.3(18) . . ?
C01K N00C U001 113.7(15) . . ?
C00K C00D N008 107.4(18) . . ?
C00Q C00D N008 122.9(19) . . ?
C00Q C00D C00K 130(2) . . ?
C00J C00E N00I 119.6(19) . . ?
C00J C00E C01E 117.1(19) . . ?
C01E C00E N00I 122.4(19) . . ?
N004 C00F H00F 118.5 . . ?
C015 C00F N004 123(2) . . ?
C015 C00F H00F 118.5 . . ?
C010 N00G U001 125.9(14) . . ?
C011 N00G U001 108.8(15) . . ?
C011 N00G C010 119.0(19) . . ?
N00A C00H C010 118.4(19) . . ?
C00L C00H N00A 122.1(19) . . ?
C00L C00H C010 118.9(19) . . ?
C00E N00I U001 121.1(12) . . ?
C018 N00I U001 115.4(14) . . ?
C018 N00I C00E 121.3(18) . . ?
C00E C00J H00J 117.6 . . ?
C00W C00J C00E 125(2) . . ?
C00W C00J H00J 117.6 . . ?
C00D C00K H00K 125.6 . . ?
C012 C00K C00D 108.7(19) . . ?
C012 C00K H00K 125.6 . . ?
C00H C00L H00L 118.3 . . ?
C00U C00L C00H 123.4(19) . . ?
C00U C00L H00L 118.3 . . ?
N007 C00M C00R 122(2) . . ?
N007 C00M C01H 111(2) . . ?
C01H C00M C00R 127(2) . . ?
N008 C00N C00Y 123(2) . . ?
N008 C00N C012 109(2) . . ?
C012 C00N C00Y 127(2) . . ?
C010 C00O H00O 118.0 . . ?
C019 C00O H00O 118.0 . . ?
C019 C00O C010 124.0(19) . . ?
N00C C00P C00R 122.6(19) . . ?
N00C C00P C01F 110(2) . . ?
C01F C00P C00R 127(2) . . ?
N006 C00Q C00D 124(2) . . ?
N006 C00Q H00Q 117.8 . . ?
C00D C00Q H00Q 117.8 . . ?
C00M C00R C00P 110.8(17) . . ?
C00M C00R C014 106.7(18) . . ?
C00M C00R C01D 111(2) . . ?
C00P C00R C014 110(2) . . ?
C00P C00R C01D 110.6(18) . . ?
C01D C00R C014 107.6(18) . . ?
N005 C00S C00Z 109(2) . . ?
N005 C00S C01C 121.7(19) . . ?
C00Z C00S C01C 129(2) . . ?
H00A C00T H00C 109.5 . . ?
H00A C00T H00D 109.5 . . ?
H00C C00T H00D 109.5 . . ?
C00Y C00T H00A 109.5 . . ?
C00Y C00T H00C 109.5 . . ?
C00Y C00T H00D 109.5 . . ?
C00L C00U C019 117(2) . . ?
C00L C00U C01Q 119.3(19) . . ?
C019 C00U C01Q 123.6(19) . . ?
C01T N00V Pb00 121.5(8) . . ?
C01T N00V C013 120.0 . . ?
C013 N00V Pb00 117.1(8) . . ?
N00V C01T H01T 120.0 . . ?
N00V C01T C01O 120.0 . . ?
C01O C01T H01T 120.0 . . ?
C01T C01O H01O 120.0 . . ?
C027 C01O C01T 120.0 . . ?
C027 C01O H01O 120.0 . . ?
C01O C027 H027 120.0 . . ?
C01O C027 C01I 120.0 . . ?
C01I C027 H027 120.0 . . ?
C027 C01I H01I 120.0 . . ?
C013 C01I C027 120.0 . . ?
C013 C01I H01I 120.0 . . ?
N00V C013 H013 120.0 . . ?
C01I C013 N00V 120.0 . . ?
C01I C013 H013 120.0 . . ?
C00J C00W C01L 119(2) . . ?
C00J C00W C01R 119(2) . . ?
C01L C00W C01R 122(2) . . ?
N005 C00X C00Y 122.6(19) . . ?
N005 C00X C016 112(2) . . ?
C016 C00X C00Y 126(2) . . ?
C00N C00Y C00T 107(2) . . ?
C00N C00Y C00X 116.3(18) . . ?
C00N C00Y C01P 110(2) . . ?
C00X C00Y C00T 108(2) . . ?
C00X C00Y C01P 108(2) . . ?
C01P C00Y C00T 107(2) . . ?
C00S C00Z H00Z 127.2 . . ?
C016 C00Z C00S 106(2) . . ?
C016 C00Z H00Z 127.2 . . ?
N00G C010 C00H 121.8(18) . . ?
C00O C010 N00G 121.8(19) . . ?
C00O C010 C00H 116.2(19) . . ?
N00G C011 H011 118.6 . . ?
N00G C011 C01K 123(2) . . ?
C01K C011 H011 118.6 . . ?
C00K C012 C00N 107(2) . . ?
C00K C012 H012 126.3 . . ?
C00N C012 H012 126.3 . . ?
C00R C014 H01A 109.5 . . ?
C00R C014 H01B 109.5 . . ?
C00R C014 H01C 109.5 . . ?
H01A C014 H01B 109.5 . . ?
H01A C014 H01C 109.5 . . ?
H01B C014 H01C 109.5 . . ?
C00F C015 H015 120.0 . . ?
C01M C015 C00F 120(2) . . ?
C01M C015 H015 120.0 . . ?
C00X C016 C00Z 107(2) . . ?
C00X C016 H016 126.7 . . ?
C00Z C016 H016 126.7 . . ?
N007 C017 C018 118.7(19) . . ?
C01J C017 N007 109(2) . . ?
C01J C017 C018 132(2) . . ?
N00I C018 C017 121(2) . . ?
N00I C018 H018 119.3 . . ?
C017 C018 H018 119.3 . . ?
C00O C019 C00U 120.4(19) . . ?
C00O C019 C01G 120.5(19) . . ?
C00U C019 C01G 119.0(19) . . ?
C01E C01A H01D 118.3 . . ?
C01E C01A C01L 123(2) . . ?
C01L C01A H01D 118.3 . . ?
C00B C01B H01E 120.5 . . ?
C01M C01B C00B 119(2) . . ?
C01M C01B H01E 120.5 . . ?
N00A C01C C00S 119(2) . . ?
N00A C01C H01F 120.7 . . ?
C00S C01C H01F 120.7 . . ?
C00R C01D H01G 109.5 . . ?
C00R C01D H01H 109.5 . . ?
C00R C01D H01J 109.5 . . ?
H01G C01D H01H 109.5 . . ?
H01G C01D H01J 109.5 . . ?
H01H C01D H01J 109.5 . . ?
N006 C01E C00E 121.2(18) . . ?
C01A C01E N006 121.5(19) . . ?
C01A C01E C00E 117(2) . . ?
C00P C01F H01K 127.2 . . ?
C00P C01F C01V 106(2) . . ?
C01V C01F H01K 127.2 . . ?
C019 C01G H01L 109.5 . . ?
C019 C01G H01M 109.5 . . ?
C019 C01G H01N 109.5 . . ?
H01L C01G H01M 109.5 . . ?
H01L C01G H01N 109.5 . . ?
H01M C01G H01N 109.5 . . ?
C00M C01H H01P 127.2 . . ?
C00M C01H C01J 106(2) . . ?
C01J C01H H01P 127.2 . . ?
C017 C01J C01H 108(2) . . ?
C017 C01J H01Q 126.2 . . ?
C01H C01J H01Q 126.2 . . ?
N00C C01K C011 122(2) . . ?
N00C C01K C01V 109(2) . . ?
C011 C01K C01V 129(3) . . ?
C00W C01L C01A 118(2) . . ?
C00W C01L C01N 123(2) . . ?
C01A C01L C01N 119(2) . . ?
C015 C01M C01B 120(2) . . ?
C015 C01M H01R 120.2 . . ?
C01B C01M H01R 120.2 . . ?
C01L C01N H01S 109.5 . . ?
C01L C01N H01U 109.5 . . ?
C01L C01N H01V 109.5 . . ?
H01S C01N H01U 109.5 . . ?
H01S C01N H01V 109.5 . . ?
H01U C01N H01V 109.5 . . ?
C00Y C01P H01W 109.5 . . ?
C00Y C01P H01X 109.5 . . ?
C00Y C01P H01Y 109.5 . . ?
H01W C01P H01X 109.5 . . ?
H01W C01P H01Y 109.5 . . ?
H01X C01P H01Y 109.5 . . ?
C00U C01Q H01Z 109.5 . . ?
C00U C01Q H 109.5 . . ?
C00U C01Q HA 109.5 . . ?
H01Z C01Q H 109.5 . . ?
H01Z C01Q HA 109.5 . . ?
H C01Q HA 109.5 . . ?
C00W C01R H01 109.5 . . ?
C00W C01R HB 109.5 . . ?
C00W C01R HC 109.5 . . ?
H01 C01R HB 109.5 . . ?
H01 C01R HC 109.5 . . ?
HB C01R HC 109.5 . . ?
C01F C01V H0AA 126.2 . . ?
C01K C01V C01F 108(2) . . ?
C01K C01V H0AA 126.2 . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 22 7 0.0594 -0.0065 21.9776 6.9977 -0.0278 -0.8912 -0.4354
0 -22 -7 0.0594 0.0065 -21.9776 -6.9977 0.0278 0.8912 0.4354
-15 0 -12 0.0543 -14.9976 -0.0056 -11.9936 0.0221 0.4787 -0.8934
15 0 12 0.0543 14.9976 0.0056 11.9936 -0.0221 -0.4787 0.8934
-1 -3 46 0.0235 -0.9959 -2.9975 45.9787 0.9689 -0.1272 0.1643
1 3 -46 0.0235 0.9959 2.9975 -45.9787 -0.9689 0.1272 -0.1643

_olex2_submission_special_instructions 'No special instructions were received'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.104 0.750 0.500 682 181 ' '
2 -0.118 0.250 1.000 682 181 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form
_vrf_PLAT342_p16024-sr           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03146 Ang.  
RESPONSE: Poor quality data cut at 0.9A
;
# 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_UO2PbLAthfPY-O
_database_code_depnum_ccdc_archive 'CCDC 1480069'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C87 H89 N9 O6 Pb U'
_chemical_formula_weight         1801.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   22.2550(3)
_cell_length_b                   16.4556(3)
_cell_length_c                   23.0701(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.360(2)
_cell_angle_gamma                90
_cell_volume                     8146.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    24412
_cell_measurement_theta_min      3.3490
_cell_measurement_theta_max      26.9390

_exptl_crystal_description       'red block'
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3977
_exptl_crystal_size_mid          0.3026
_exptl_crystal_size_min          0.0604
_exptl_absorpt_coefficient_mu    4.106
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_reflns_number            124254
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.966
_diffrn_reflns_theta_max         26.372
_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             16651
_reflns_number_gt                12622
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 2015'
_computing_publication_material  POV-ray
_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)+(0.0392P)²+2.6648P] 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         16651
_refine_ls_number_parameters     917
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.062
_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
C1 C 0.7442(2) -0.1290(3) 0.4733(2) 0.0337(12) Uani 1 1 d . . . . .
C2 C 0.7202(3) -0.2051(4) 0.4366(2) 0.0428(14) Uani 1 1 d . . . . .
H2A H 0.6892 -0.1888 0.4003 0.051 Uiso 1 1 calc R U . . .
H2B H 0.6994 -0.2391 0.4597 0.051 Uiso 1 1 calc R U . . .
C3 C 0.7701(3) -0.2564(4) 0.4186(3) 0.0606(19) Uani 1 1 d . . . . .
H3A H 0.7881 -0.2254 0.3921 0.091 Uiso 1 1 calc R U . . .
H3B H 0.7514 -0.3048 0.3984 0.091 Uiso 1 1 calc R U . . .
H3C H 0.8021 -0.2710 0.4539 0.091 Uiso 1 1 calc R U . . .
C4 C 0.6884(2) -0.0825(4) 0.4868(2) 0.0407(14) Uani 1 1 d . . . . .
H4A H 0.7040 -0.0326 0.5078 0.049 Uiso 1 1 calc R U . . .
H4B H 0.6595 -0.0675 0.4489 0.049 Uiso 1 1 calc R U . . .
C5 C 0.6524(3) -0.1289(4) 0.5241(3) 0.0611(19) Uani 1 1 d . . . . .
H5A H 0.6395 -0.1806 0.5056 0.092 Uiso 1 1 calc R U . . .
H5B H 0.6164 -0.0982 0.5261 0.092 Uiso 1 1 calc R U . . .
H5C H 0.6787 -0.1373 0.5639 0.092 Uiso 1 1 calc R U . . .
C6 C 0.7722(2) -0.0704(3) 0.4362(2) 0.0313(12) Uani 1 1 d . . . . .
C7 C 0.7569(2) -0.0659(4) 0.3731(2) 0.0396(14) Uani 1 1 d . . . . .
H7 H 0.7304 -0.1005 0.3461 0.048 Uiso 1 1 calc R U . . .
C8 C 0.7890(3) -0.0001(4) 0.3590(2) 0.0425(14) Uani 1 1 d . . . . .
H8 H 0.7888 0.0173 0.3206 0.051 Uiso 1 1 calc R U . . .
C9 C 0.8214(2) 0.0350(3) 0.4123(2) 0.0330(12) Uani 1 1 d . . . . .
C10 C 0.8608(2) 0.1030(3) 0.4238(2) 0.0306(11) Uani 1 1 d . . . . .
H10 H 0.8715 0.1276 0.3916 0.037 Uiso 1 1 calc R U . . .
C11 C 0.9333(2) 0.1886(3) 0.4840(2) 0.0257(11) Uani 1 1 d . . . . .
C12 C 0.9857(2) 0.1644(3) 0.4678(2) 0.0357(13) Uani 1 1 d . . . . .
H12 H 0.9866 0.1129 0.4514 0.043 Uiso 1 1 calc R U . . .
C13 C 1.0388(2) 0.2164(4) 0.4757(2) 0.0395(13) Uani 1 1 d . . . . .
H13 H 1.0739 0.1980 0.4652 0.047 Uiso 1 1 calc R U . . .
C14 C 1.0382(2) 0.2925(3) 0.4984(2) 0.0342(12) Uani 1 1 d . . . . .
H14 H 1.0729 0.3259 0.5029 0.041 Uiso 1 1 calc R U . . .
C15 C 0.9841(2) 0.3220(3) 0.5155(2) 0.0280(11) Uani 1 1 d . . . . .
C16 C 0.9308(2) 0.2679(3) 0.5092(2) 0.0262(11) Uani 1 1 d . . . . .
C17 C 0.8796(2) 0.2971(3) 0.52743(19) 0.0245(11) Uani 1 1 d . . . . .
H17 H 0.8462 0.2625 0.5256 0.029 Uiso 1 1 calc R U . . .
C18 C 0.9808(2) 0.4002(3) 0.5354(2) 0.0308(12) Uani 1 1 d . . . . .
H18 H 1.0149 0.4342 0.5387 0.037 Uiso 1 1 calc R U . . .
C19 C 0.8768(2) 0.3770(3) 0.54849(19) 0.0263(11) Uani 1 1 d . . . . .
C20 C 0.9290(2) 0.4306(3) 0.5509(2) 0.0281(11) Uani 1 1 d . . . . .
C21 C 0.9235(2) 0.5127(3) 0.5669(2) 0.0356(13) Uani 1 1 d . . . . .
H21 H 0.9561 0.5485 0.5681 0.043 Uiso 1 1 calc R U . . .
C22 C 0.8716(2) 0.5400(3) 0.5805(2) 0.0363(13) Uani 1 1 d . . . . .
H22 H 0.8687 0.5946 0.5899 0.044 Uiso 1 1 calc R U . . .
C401 C 0.7942(3) 0.3879(4) 0.7346(3) 0.0531(16) Uani 1 1 d . U . . .
H40A H 0.8095 0.4272 0.7107 0.064 Uiso 1 1 calc R U . . .
H40B H 0.8286 0.3540 0.7559 0.064 Uiso 1 1 calc R U . . .
C23 C 0.8216(2) 0.4869(3) 0.5804(2) 0.0359(13) Uani 1 1 d . . . . .
H23 H 0.7870 0.5070 0.5911 0.043 Uiso 1 1 calc R U . . .
C24 C 0.8229(2) 0.4073(3) 0.56520(19) 0.0262(11) Uani 1 1 d . . . . .
C25 C 0.7184(2) 0.3757(3) 0.5430(2) 0.0313(12) Uani 1 1 d . . . . .
H25 H 0.7117 0.4248 0.5223 0.038 Uiso 1 1 calc R U . . .
C26 C 0.6657(2) 0.3295(3) 0.5469(2) 0.0296(12) Uani 1 1 d . . . . .
C27 C 0.6035(2) 0.3484(4) 0.5207(2) 0.0391(13) Uani 1 1 d . . . . .
H27 H 0.5883 0.3934 0.4970 0.047 Uiso 1 1 calc R U . . .
C28 C 0.5688(2) 0.2873(4) 0.5371(2) 0.0392(13) Uani 1 1 d . . . . .
H28 H 0.5256 0.2830 0.5256 0.047 Uiso 1 1 calc R U . . .
C29 C 0.6101(2) 0.2332(3) 0.5737(2) 0.0316(12) Uani 1 1 d . . . . .
C30 C 0.5951(2) 0.1541(4) 0.6004(2) 0.0337(12) Uani 1 1 d . . . . .
C31 C 0.6141(3) 0.0828(4) 0.5653(2) 0.0428(14) Uani 1 1 d . . . . .
H31A H 0.6586 0.0859 0.5698 0.051 Uiso 1 1 calc R U . . .
H31B H 0.6060 0.0322 0.5835 0.051 Uiso 1 1 calc R U . . .
C32 C 0.5808(3) 0.0800(4) 0.4982(2) 0.0591(18) Uani 1 1 d . . . . .
H32A H 0.5374 0.0689 0.4930 0.089 Uiso 1 1 calc R U . . .
H32B H 0.5988 0.0378 0.4793 0.089 Uiso 1 1 calc R U . . .
H32C H 0.5855 0.1313 0.4801 0.089 Uiso 1 1 calc R U . . .
C33 C 0.5238(2) 0.1487(4) 0.5942(3) 0.0509(16) Uani 1 1 d . . . . .
H33A H 0.5023 0.1529 0.5518 0.061 Uiso 1 1 calc R U . . .
H33B H 0.5150 0.0952 0.6075 0.061 Uiso 1 1 calc R U . . .
C34 C 0.4956(3) 0.2117(5) 0.6282(3) 0.075(2) Uani 1 1 d . . . . .
H34A H 0.5163 0.2089 0.6703 0.112 Uiso 1 1 calc R U . . .
H34B H 0.4520 0.2006 0.6221 0.112 Uiso 1 1 calc R U . . .
H34C H 0.5007 0.2650 0.6134 0.112 Uiso 1 1 calc R U . . .
C35 C 0.6305(2) 0.1440(3) 0.6662(2) 0.0304(12) Uani 1 1 d . . . . .
C36 C 0.6077(2) 0.1127(3) 0.7128(2) 0.0374(13) Uani 1 1 d . . . . .
H36 H 0.5672 0.0954 0.7097 0.045 Uiso 1 1 calc R U . . .
C37 C 0.6566(2) 0.1122(3) 0.7638(2) 0.0370(13) Uani 1 1 d . . . . .
H37 H 0.6552 0.0948 0.8018 0.044 Uiso 1 1 calc R U . . .
C38 C 0.7083(2) 0.1423(3) 0.7483(2) 0.0280(11) Uani 1 1 d . . . . .
C39 C 0.7696(2) 0.1539(3) 0.7846(2) 0.0319(12) Uani 1 1 d . . . . .
H39 H 0.7770 0.1446 0.8257 0.038 Uiso 1 1 calc R U . . .
C111 C 0.9935(3) 0.2390(4) 0.6669(2) 0.0451(15) Uani 1 1 d . . . . .
H111 H 0.9597 0.2640 0.6763 0.054 Uiso 1 1 calc R U . . .
C40 C 0.8741(2) 0.1934(3) 0.8059(2) 0.0319(12) Uani 1 1 d . . . . .
C41 C 0.8800(3) 0.2454(4) 0.8533(2) 0.0418(14) Uani 1 1 d . . . . .
H41 H 0.8443 0.2678 0.8604 0.050 Uiso 1 1 calc R U . . .
C42 C 0.9385(3) 0.2661(4) 0.8918(2) 0.0476(16) Uani 1 1 d . . . . .
H42 H 0.9410 0.3011 0.9241 0.057 Uiso 1 1 calc R U . . .
C43 C 0.9905(3) 0.2350(4) 0.8817(2) 0.0457(15) Uani 1 1 d . . . . .
H43 H 1.0290 0.2500 0.9066 0.055 Uiso 1 1 calc R U . . .
C45 C 0.9290(2) 0.1573(3) 0.7952(2) 0.0311(12) Uani 1 1 d . . . . .
C46 C 0.9265(2) 0.0994(3) 0.7509(2) 0.0265(11) Uani 1 1 d . . . . .
H46 H 0.8880 0.0855 0.7254 0.032 Uiso 1 1 calc R U . . .
C47 C 1.0419(2) 0.1444(4) 0.8243(2) 0.0429(14) Uani 1 1 d . . . . .
H47 H 1.0804 0.1609 0.8484 0.051 Uiso 1 1 calc R U . . .
C48 C 1.0402(2) 0.0861(4) 0.7809(2) 0.0350(13) Uani 1 1 d . . . . .
C49 C 0.9801(2) 0.0614(3) 0.7433(2) 0.0303(12) Uani 1 1 d . . . . .
C50 C 1.0946(2) 0.0460(4) 0.7742(2) 0.0444(15) Uani 1 1 d . . . . .
H50 H 1.1335 0.0628 0.7975 0.053 Uiso 1 1 calc R U . . .
C115 C 1.0322(2) 0.1331(4) 0.6178(2) 0.0433(14) Uani 1 1 d . . . . .
H115 H 1.0248 0.0872 0.5934 0.052 Uiso 1 1 calc R U . . .
C51 C 1.0912(3) -0.0151(4) 0.7353(3) 0.0481(16) Uani 1 1 d . . . . .
H51 H 1.1274 -0.0411 0.7324 0.058 Uiso 1 1 calc R U . . .
C52 C 1.0322(2) -0.0407(4) 0.6982(2) 0.0407(14) Uani 1 1 d . . . . .
H52 H 1.0304 -0.0833 0.6713 0.049 Uiso 1 1 calc R U . . .
C53 C 0.9787(2) -0.0037(3) 0.7016(2) 0.0304(12) Uani 1 1 d . . . . .
C54 C 0.9060(2) -0.1054(3) 0.6645(2) 0.0339(12) Uani 1 1 d . . . . .
H54 H 0.9276 -0.1365 0.6970 0.041 Uiso 1 1 calc R U . . .
C55 C 0.8585(2) -0.1426(3) 0.6198(2) 0.0308(12) Uani 1 1 d . . . . .
C56 C 0.8343(3) -0.2195(4) 0.6174(3) 0.0436(14) Uani 1 1 d . . . . .
H56 H 0.8453 -0.2594 0.6469 0.052 Uiso 1 1 calc R U . . .
C113 C 1.1019(3) 0.2315(5) 0.6743(3) 0.072(2) Uani 1 1 d . . . . .
H113 H 1.1420 0.2521 0.6888 0.086 Uiso 1 1 calc R U . . .
C57 C 0.7906(3) -0.2266(4) 0.5630(3) 0.0432(14) Uani 1 1 d . . . . .
H57 H 0.7664 -0.2721 0.5488 0.052 Uiso 1 1 calc R U . . .
C58 C 0.7892(2) -0.1528(3) 0.5330(2) 0.0320(12) Uani 1 1 d . . . . .
C112 C 1.0517(3) 0.2704(4) 0.6880(3) 0.0625(19) Uani 1 1 d . . . . .
H112 H 1.0580 0.3173 0.7113 0.075 Uiso 1 1 calc R U . . .
C403 C 0.6976(4) 0.4392(5) 0.7419(4) 0.087(3) Uani 1 1 d . U . . .
H40C H 0.6698 0.4444 0.7678 0.105 Uiso 1 1 calc R U . . .
H40D H 0.6922 0.4858 0.7152 0.105 Uiso 1 1 calc R U . . .
C402 C 0.7647(5) 0.4303(5) 0.7782(3) 0.091(3) Uani 1 1 d . U . . .
H40E H 0.7838 0.4828 0.7900 0.109 Uiso 1 1 calc R U . . .
H40F H 0.7679 0.3976 0.8139 0.109 Uiso 1 1 calc R U . . .
C404 C 0.6868(3) 0.3612(4) 0.7073(3) 0.066(2) Uani 1 1 d . U . . .
H40G H 0.6726 0.3192 0.7301 0.079 Uiso 1 1 calc R U . . .
H40H H 0.6556 0.3684 0.6693 0.079 Uiso 1 1 calc R U . . .
C81 C 0.1439(3) 0.9009(3) 0.02090(19) 0.083(2) Uani 1 1 d G . . . .
H81 H 0.1684 0.8871 0.0589 0.099 Uiso 1 1 calc R U . . .
C82 C 0.0800(3) 0.9112(3) 0.0112(3) 0.089(3) Uani 1 1 d G . . . .
H82 H 0.0618 0.9043 0.0428 0.106 Uiso 1 1 calc R U . . .
C83 C 0.0434(2) 0.9318(3) -0.0456(3) 0.093(3) Uani 1 1 d G . . . .
H83 H 0.0007 0.9387 -0.0520 0.111 Uiso 1 1 calc R U . . .
C84 C 0.0707(3) 0.9422(3) -0.0928(2) 0.095(3) Uani 1 1 d G . . . .
H84 H 0.0462 0.9560 -0.1308 0.114 Uiso 1 1 calc R U . . .
C85 C 0.1346(3) 0.9319(3) -0.0831(2) 0.085(2) Uani 1 1 d G . . . .
H85 H 0.1528 0.9388 -0.1147 0.102 Uiso 1 1 calc R U . . .
C86 C 0.1712(2) 0.9113(3) -0.0263(3) 0.072(2) Uani 1 1 d G . . . .
H86 H 0.2140 0.9044 -0.0198 0.087 Uiso 1 1 calc R U . . .
C114 C 1.0921(3) 0.1630(5) 0.6395(3) 0.0605(19) Uani 1 1 d . . . . .
H114 H 1.1255 0.1367 0.6305 0.073 Uiso 1 1 calc R U . . .
C91 C 1.06100(19) 0.4937(3) 0.82330(17) 0.074(2) Uani 1 1 d G . . . .
H91 H 1.0919 0.5096 0.8571 0.088 Uiso 1 1 calc R U . . .
C92 C 1.0187(2) 0.4335(3) 0.82805(15) 0.068(2) Uani 1 1 d G . . . .
H92 H 1.0214 0.4091 0.8650 0.081 Uiso 1 1 calc R U . . .
C93 C 0.97250(18) 0.4099(2) 0.77758(19) 0.0583(18) Uani 1 1 d G . . . .
H93 H 0.9442 0.3696 0.7808 0.070 Uiso 1 1 calc R U . . .
C94 C 0.96851(18) 0.4464(3) 0.72235(15) 0.0575(18) Uani 1 1 d G . . . .
H94 H 0.9376 0.4305 0.6886 0.069 Uiso 1 1 calc R U . . .
C95 C 1.0108(2) 0.5065(3) 0.71760(16) 0.069(2) Uani 1 1 d G . . . .
H95 H 1.0081 0.5310 0.6806 0.083 Uiso 1 1 calc R U . . .
C96 C 1.05701(19) 0.5302(3) 0.7681(2) 0.070(2) Uani 1 1 d G . . . .
H96 H 1.0853 0.5705 0.7649 0.084 Uiso 1 1 calc R U . . .
C502 C 0.1865(6) 0.4490(10) 0.6939(4) 0.179(7) Uani 1 1 d D . . . .
H50A H 0.1760 0.4914 0.7187 0.215 Uiso 1 1 calc R U . . .
H50B H 0.1888 0.3975 0.7148 0.215 Uiso 1 1 calc R U . . .
C503 C 0.1436(5) 0.4457(9) 0.6388(6) 0.158(6) Uani 1 1 d . . . . .
H50C H 0.1042 0.4682 0.6417 0.190 Uiso 1 1 calc R U . . .
H50D H 0.1368 0.3897 0.6255 0.190 Uiso 1 1 calc R U . . .
C504 C 0.1674(7) 0.4920(9) 0.5966(5) 0.164(6) Uani 1 1 d . . . . .
H50E H 0.1701 0.4590 0.5626 0.197 Uiso 1 1 calc R U . . .
H50F H 0.1415 0.5391 0.5821 0.197 Uiso 1 1 calc R U . . .
O5 O 0.2274(6) 0.5155(10) 0.6317(9) 0.313(9) Uani 1 1 d . . . . .
O6 O 0.1981(3) 0.2282(5) 0.8481(3) 0.106(2) Uani 1 1 d . . . . .
C601 C 0.2250(4) 0.2194(6) 0.9098(3) 0.095(3) Uani 1 1 d . . . . .
H60A H 0.2694 0.2099 0.9174 0.114 Uiso 1 1 calc R U . . .
H60B H 0.2067 0.1733 0.9250 0.114 Uiso 1 1 calc R U . . .
C602 C 0.2139(4) 0.2939(5) 0.9404(3) 0.080(2) Uani 1 1 d . . . . .
H60C H 0.2530 0.3202 0.9601 0.096 Uiso 1 1 calc R U . . .
H60D H 0.1916 0.2819 0.9703 0.096 Uiso 1 1 calc R U . . .
C603 C 0.1762(3) 0.3462(6) 0.8926(4) 0.088(3) Uani 1 1 d . . . . .
H60E H 0.1918 0.4016 0.8969 0.105 Uiso 1 1 calc R U . . .
H60F H 0.1330 0.3466 0.8939 0.105 Uiso 1 1 calc R U . . .
C44 C 0.9882(2) 0.1794(4) 0.8336(2) 0.0368(13) Uani 1 1 d . . . . .
N2 N 0.81045(17) -0.0083(3) 0.46040(17) 0.0290(10) Uani 1 1 d . . . . .
N3 N 0.88312(17) 0.1334(2) 0.47724(17) 0.0274(9) Uani 1 1 d . . . . .
N4 N 0.92086(17) -0.0286(3) 0.66210(17) 0.0280(9) Uani 1 1 d . . . . .
N5 N 0.83033(17) -0.1007(3) 0.56725(17) 0.0284(9) Uani 1 1 d . . . . .
N6 N 0.77549(17) 0.3528(3) 0.56700(16) 0.0275(9) Uani 1 1 d . . . . .
N7 N 0.66971(17) 0.2587(3) 0.57933(17) 0.0279(9) Uani 1 1 d . . . . .
N8 N 0.69214(17) 0.1612(3) 0.68763(16) 0.0276(9) Uani 1 1 d . . . . .
N9 N 0.81592(18) 0.1763(3) 0.76482(16) 0.0296(10) Uani 1 1 d . . . . .
N10 N 0.98462(19) 0.1714(3) 0.63241(18) 0.0363(11) Uani 1 1 d . . . . .
O1 O 0.80541(15) 0.0799(2) 0.57533(14) 0.0342(8) Uani 1 1 d . . . . .
O2 O 0.94028(15) -0.0065(2) 0.54410(15) 0.0344(8) Uani 1 1 d . . . . .
O3 O 0.92673(15) 0.1434(2) 0.61347(14) 0.0339(8) Uani 1 1 d . . . . .
O4 O 0.74549(16) 0.3395(2) 0.69738(16) 0.0441(10) Uani 1 1 d . . . . .
C501 C 0.2435(5) 0.4664(10) 0.6802(6) 0.164(6) Uani 1 1 d D . . . .
H50G H 0.2629 0.4169 0.6709 0.197 Uiso 1 1 calc R U . . .
H50H H 0.2722 0.4935 0.7136 0.197 Uiso 1 1 calc R U . . .
C604 C 0.1820(5) 0.3104(7) 0.8356(4) 0.123(4) Uani 1 1 d . . . . .
H60G H 0.1429 0.3148 0.8047 0.148 Uiso 1 1 calc R U . . .
H60H H 0.2142 0.3382 0.8218 0.148 Uiso 1 1 calc R U . . .
Pb1 Pb 0.76479(2) 0.21856(2) 0.64260(2) 0.02644(6) Uani 1 1 d . . . . .
U1 U 0.87248(2) 0.03531(2) 0.55942(2) 0.02475(6) 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
C1 C58 1.525(7) . ?
C1 C2 1.526(7) . ?
C1 C6 1.526(7) . ?
C1 C4 1.561(7) . ?
C2 C3 1.539(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.526(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N2 1.353(6) . ?
C6 C7 1.408(7) . ?
C7 C8 1.383(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.377(7) . ?
C8 H8 0.9300 . ?
C9 N2 1.392(6) . ?
C9 C10 1.404(7) . ?
C10 N3 1.301(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(6) . ?
C11 N3 1.416(6) . ?
C11 C16 1.436(7) . ?
C12 C13 1.432(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.358(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.445(7) . ?
C14 H14 0.9300 . ?
C15 C18 1.375(7) . ?
C15 C16 1.459(7) . ?
C16 C17 1.400(6) . ?
C17 C19 1.408(7) . ?
C17 H17 0.9300 . ?
C18 C20 1.388(7) . ?
C18 H18 0.9300 . ?
C19 C24 1.442(6) . ?
C19 C20 1.448(6) . ?
C20 C21 1.415(7) . ?
C21 C22 1.351(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.415(7) . ?
C22 H22 0.9300 . ?
C401 O4 1.434(6) . ?
C401 C402 1.508(9) . ?
C401 H40A 0.9700 . ?
C401 H40B 0.9700 . ?
C23 C24 1.359(7) . ?
C23 H23 0.9300 . ?
C24 N6 1.394(6) . ?
C25 N6 1.301(6) . ?
C25 C26 1.419(7) . ?
C25 H25 0.9300 . ?
C26 N7 1.375(6) . ?
C26 C27 1.392(6) . ?
C27 C28 1.380(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.394(7) . ?
C28 H28 0.9300 . ?
C29 N7 1.364(6) . ?
C29 C30 1.515(7) . ?
C30 C35 1.523(7) . ?
C30 C31 1.546(8) . ?
C30 C33 1.558(7) . ?
C31 C32 1.531(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.531(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N8 1.359(6) . ?
C35 C36 1.401(7) . ?
C36 C37 1.375(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.384(7) . ?
C37 H37 0.9300 . ?
C38 N8 1.384(6) . ?
C38 C39 1.412(6) . ?
C39 N9 1.288(6) . ?
C39 H39 0.9300 . ?
C111 N10 1.353(7) . ?
C111 C112 1.359(8) . ?
C111 H111 0.9300 . ?
C40 C41 1.368(7) . ?
C40 N9 1.415(6) . ?
C40 C45 1.438(7) . ?
C41 C42 1.409(7) . ?
C41 H41 0.9300 . ?
C42 C43 1.343(8) . ?
C42 H42 0.9300 . ?
C43 C44 1.429(8) . ?
C43 H43 0.9300 . ?
C45 C46 1.387(7) . ?
C45 C44 1.427(6) . ?
C46 C49 1.398(7) . ?
C46 H46 0.9300 . ?
C47 C48 1.382(8) . ?
C47 C44 1.391(7) . ?
C47 H47 0.9300 . ?
C48 C50 1.424(7) . ?
C48 C49 1.445(6) . ?
C49 C53 1.434(7) . ?
C50 C51 1.337(8) . ?
C50 H50 0.9300 . ?
C115 N10 1.348(7) . ?
C115 C114 1.385(8) . ?
C115 H115 0.9300 . ?
C51 C52 1.427(8) . ?
C51 H51 0.9300 . ?
C52 C53 1.358(7) . ?
C52 H52 0.9300 . ?
C53 N4 1.427(6) . ?
C54 N4 1.312(6) . ?
C54 C55 1.405(7) . ?
C54 H54 0.9300 . ?
C55 C56 1.372(7) . ?
C55 N5 1.392(6) . ?
C56 C57 1.375(8) . ?
C56 H56 0.9300 . ?
C113 C114 1.367(10) . ?
C113 C112 1.394(10) . ?
C113 H113 0.9300 . ?
C57 C58 1.393(7) . ?
C57 H57 0.9300 . ?
C58 N5 1.347(6) . ?
C112 H112 0.9300 . ?
C403 C404 1.497(9) . ?
C403 C402 1.514(11) . ?
C403 H40C 0.9700 . ?
C403 H40D 0.9700 . ?
C402 H40E 0.9700 . ?
C402 H40F 0.9700 . ?
C404 O4 1.430(6) . ?
C404 H40G 0.9700 . ?
C404 H40H 0.9700 . ?
C81 C82 1.3900 . ?
C81 C86 1.3900 . ?
C81 H81 0.9300 . ?
C82 C83 1.3900 . ?
C82 H82 0.9300 . ?
C83 C84 1.3900 . ?
C83 H83 0.9300 . ?
C84 C85 1.3900 . ?
C84 H84 0.9300 . ?
C85 C86 1.3900 . ?
C85 H85 0.9300 . ?
C86 H86 0.9300 . ?
C114 H114 0.9300 . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C91 H91 0.9300 . ?
C92 C93 1.3900 . ?
C92 H92 0.9300 . ?
C93 C94 1.3900 . ?
C93 H93 0.9300 . ?
C94 C95 1.3900 . ?
C94 H94 0.9300 . ?
C95 C96 1.3900 . ?
C95 H95 0.9300 . ?
C96 H96 0.9300 . ?
C502 C501 1.415(8) . ?
C502 C503 1.374(12) . ?
C502 H50A 0.9700 . ?
C502 H50B 0.9700 . ?
C503 C504 1.443(15) . ?
C503 H50C 0.9700 . ?
C503 H50D 0.9700 . ?
C504 O5 1.420(16) . ?
C504 H50E 0.9700 . ?
C504 H50F 0.9700 . ?
O5 C501 1.349(15) . ?
O6 C601 1.399(9) . ?
O6 C604 1.410(11) . ?
C601 C602 1.468(11) . ?
C601 H60A 0.9700 . ?
C601 H60B 0.9700 . ?
C602 C603 1.474(10) . ?
C602 H60C 0.9700 . ?
C602 H60D 0.9700 . ?
C603 C604 1.478(12) . ?
C603 H60E 0.9700 . ?
C603 H60F 0.9700 . ?
N2 U1 2.443(4) . ?
N3 U1 2.548(4) . ?
N4 U1 2.554(4) . ?
N5 U1 2.452(4) . ?
N7 Pb1 2.326(4) . ?
N8 Pb1 2.340(4) . ?
N10 O3 1.328(5) . ?
O1 U1 1.786(3) . ?
O2 U1 1.777(3) . ?
O3 U1 2.319(3) . ?
O4 Pb1 2.455(4) . ?
C501 H50G 0.9700 . ?
C501 H50H 0.9700 . ?
C604 H60G 0.9700 . ?
C604 H60H 0.9700 . ?

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
C58 C1 C2 109.9(5) . . ?
C58 C1 C6 113.7(4) . . ?
C2 C1 C6 110.1(4) . . ?
C58 C1 C4 108.2(4) . . ?
C2 C1 C4 109.4(4) . . ?
C6 C1 C4 105.4(4) . . ?
C1 C2 C3 115.3(5) . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C1 115.6(5) . . ?
C5 C4 H4A 108.4 . . ?
C1 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 109.9(5) . . ?
N2 C6 C1 123.5(4) . . ?
C7 C6 C1 126.2(5) . . ?
C8 C7 C6 106.6(5) . . ?
C8 C7 H7 126.7 . . ?
C6 C7 H7 126.7 . . ?
C9 C8 C7 107.3(5) . . ?
C9 C8 H8 126.3 . . ?
C7 C8 H8 126.3 . . ?
C8 C9 N2 109.7(5) . . ?
C8 C9 C10 130.9(5) . . ?
N2 C9 C10 119.4(4) . . ?
N3 C10 C9 123.2(5) . . ?
N3 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C12 C11 N3 119.0(5) . . ?
C12 C11 C16 120.0(5) . . ?
N3 C11 C16 121.0(4) . . ?
C11 C12 C13 121.5(5) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C14 C13 C12 120.6(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 120.5(5) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C18 C15 C14 121.9(5) . . ?
C18 C15 C16 119.3(4) . . ?
C14 C15 C16 118.8(5) . . ?
C17 C16 C11 123.7(4) . . ?
C17 C16 C15 117.8(5) . . ?
C11 C16 C15 118.5(4) . . ?
C16 C17 C19 122.5(4) . . ?
C16 C17 H17 118.7 . . ?
C19 C17 H17 118.7 . . ?
C15 C18 C20 123.1(5) . . ?
C15 C18 H18 118.5 . . ?
C20 C18 H18 118.5 . . ?
C17 C19 C24 122.1(4) . . ?
C17 C19 C20 118.3(4) . . ?
C24 C19 C20 119.6(5) . . ?
C18 C20 C21 123.2(5) . . ?
C18 C20 C19 118.9(5) . . ?
C21 C20 C19 117.9(5) . . ?
C22 C21 C20 121.2(5) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 120.9(5) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
O4 C401 C402 105.3(5) . . ?
O4 C401 H40A 110.7 . . ?
C402 C401 H40A 110.7 . . ?
O4 C401 H40B 110.7 . . ?
C402 C401 H40B 110.7 . . ?
H40A C401 H40B 108.8 . . ?
C24 C23 C22 121.7(5) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 N6 122.9(4) . . ?
C23 C24 C19 118.6(5) . . ?
N6 C24 C19 118.4(5) . . ?
N6 C25 C26 123.2(5) . . ?
N6 C25 H25 118.4 . . ?
C26 C25 H25 118.4 . . ?
N7 C26 C27 109.8(4) . . ?
N7 C26 C25 123.6(4) . . ?
C27 C26 C25 126.6(5) . . ?
C28 C27 C26 106.5(5) . . ?
C28 C27 H27 126.8 . . ?
C26 C27 H27 126.8 . . ?
C27 C28 C29 107.7(5) . . ?
C27 C28 H28 126.1 . . ?
C29 C28 H28 126.1 . . ?
N7 C29 C28 109.2(5) . . ?
N7 C29 C30 122.6(4) . . ?
C28 C29 C30 128.0(5) . . ?
C29 C30 C35 112.8(4) . . ?
C29 C30 C31 108.6(4) . . ?
C35 C30 C31 107.4(4) . . ?
C29 C30 C33 109.9(4) . . ?
C35 C30 C33 109.3(4) . . ?
C31 C30 C33 108.8(5) . . ?
C32 C31 C30 115.3(5) . . ?
C32 C31 H31A 108.5 . . ?
C30 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C30 117.4(5) . . ?
C34 C33 H33A 107.9 . . ?
C30 C33 H33A 107.9 . . ?
C34 C33 H33B 107.9 . . ?
C30 C33 H33B 107.9 . . ?
H33A C33 H33B 107.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C36 109.5(4) . . ?
N8 C35 C30 123.0(4) . . ?
C36 C35 C30 127.5(4) . . ?
C37 C36 C35 107.1(4) . . ?
C37 C36 H36 126.5 . . ?
C35 C36 H36 126.5 . . ?
C36 C37 C38 107.5(4) . . ?
C36 C37 H37 126.3 . . ?
C38 C37 H37 126.3 . . ?
C37 C38 N8 109.3(4) . . ?
C37 C38 C39 129.2(4) . . ?
N8 C38 C39 121.5(4) . . ?
N9 C39 C38 124.4(4) . . ?
N9 C39 H39 117.8 . . ?
C38 C39 H39 117.8 . . ?
N10 C111 C112 120.0(6) . . ?
N10 C111 H111 120.0 . . ?
C112 C111 H111 120.0 . . ?
C41 C40 N9 122.5(5) . . ?
C41 C40 C45 119.3(5) . . ?
N9 C40 C45 118.2(4) . . ?
C40 C41 C42 122.2(5) . . ?
C40 C41 H41 118.9 . . ?
C42 C41 H41 118.9 . . ?
C43 C42 C41 119.5(5) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 121.7(5) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C46 C45 C44 118.8(5) . . ?
C46 C45 C40 122.7(4) . . ?
C44 C45 C40 118.4(5) . . ?
C45 C46 C49 122.0(4) . . ?
C45 C46 H46 119.0 . . ?
C49 C46 H46 119.0 . . ?
C48 C47 C44 122.6(5) . . ?
C48 C47 H47 118.7 . . ?
C44 C47 H47 118.7 . . ?
C47 C48 C50 122.6(5) . . ?
C47 C48 C49 118.3(5) . . ?
C50 C48 C49 119.0(5) . . ?
C46 C49 C53 123.4(4) . . ?
C46 C49 C48 118.9(5) . . ?
C53 C49 C48 117.7(5) . . ?
C51 C50 C48 121.4(5) . . ?
C51 C50 H50 119.3 . . ?
C48 C50 H50 119.3 . . ?
N10 C115 C114 119.2(6) . . ?
N10 C115 H115 120.4 . . ?
C114 C115 H115 120.4 . . ?
C50 C51 C52 120.3(5) . . ?
C50 C51 H51 119.8 . . ?
C52 C51 H51 119.8 . . ?
C53 C52 C51 121.0(6) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C52 C53 N4 119.4(5) . . ?
C52 C53 C49 120.7(5) . . ?
N4 C53 C49 119.9(4) . . ?
N4 C54 C55 122.5(5) . . ?
N4 C54 H54 118.7 . . ?
C55 C54 H54 118.7 . . ?
C56 C55 N5 109.9(5) . . ?
C56 C55 C54 130.0(5) . . ?
N5 C55 C54 120.1(5) . . ?
C55 C56 C57 106.9(5) . . ?
C55 C56 H56 126.6 . . ?
C57 C56 H56 126.6 . . ?
C114 C113 C112 119.9(6) . . ?
C114 C113 H113 120.0 . . ?
C112 C113 H113 120.0 . . ?
C56 C57 C58 107.3(5) . . ?
C56 C57 H57 126.4 . . ?
C58 C57 H57 126.4 . . ?
N5 C58 C57 110.0(5) . . ?
N5 C58 C1 123.2(5) . . ?
C57 C58 C1 126.5(5) . . ?
C111 C112 C113 119.3(7) . . ?
C111 C112 H112 120.4 . . ?
C113 C112 H112 120.4 . . ?
C404 C403 C402 101.9(6) . . ?
C404 C403 H40C 111.4 . . ?
C402 C403 H40C 111.4 . . ?
C404 C403 H40D 111.4 . . ?
C402 C403 H40D 111.4 . . ?
H40C C403 H40D 109.2 . . ?
C401 C402 C403 102.5(6) . . ?
C401 C402 H40E 111.3 . . ?
C403 C402 H40E 111.3 . . ?
C401 C402 H40F 111.3 . . ?
C403 C402 H40F 111.3 . . ?
H40E C402 H40F 109.2 . . ?
O4 C404 C403 106.0(6) . . ?
O4 C404 H40G 110.5 . . ?
C403 C404 H40G 110.5 . . ?
O4 C404 H40H 110.5 . . ?
C403 C404 H40H 110.5 . . ?
H40G C404 H40H 108.7 . . ?
C82 C81 C86 120.0 . . ?
C82 C81 H81 120.0 . . ?
C86 C81 H81 120.0 . . ?
C83 C82 C81 120.0 . . ?
C83 C82 H82 120.0 . . ?
C81 C82 H82 120.0 . . ?
C82 C83 C84 120.0 . . ?
C82 C83 H83 120.0 . . ?
C84 C83 H83 120.0 . . ?
C85 C84 C83 120.0 . . ?
C85 C84 H84 120.0 . . ?
C83 C84 H84 120.0 . . ?
C84 C85 C86 120.0 . . ?
C84 C85 H85 120.0 . . ?
C86 C85 H85 120.0 . . ?
C85 C86 C81 120.0 . . ?
C85 C86 H86 120.0 . . ?
C81 C86 H86 120.0 . . ?
C113 C114 C115 119.6(6) . . ?
C113 C114 H114 120.2 . . ?
C115 C114 H114 120.2 . . ?
C92 C91 C96 120.0 . . ?
C92 C91 H91 120.0 . . ?
C96 C91 H91 120.0 . . ?
C93 C92 C91 120.0 . . ?
C93 C92 H92 120.0 . . ?
C91 C92 H92 120.0 . . ?
C92 C93 C94 120.0 . . ?
C92 C93 H93 120.0 . . ?
C94 C93 H93 120.0 . . ?
C93 C94 C95 120.0 . . ?
C93 C94 H94 120.0 . . ?
C95 C94 H94 120.0 . . ?
C96 C95 C94 120.0 . . ?
C96 C95 H95 120.0 . . ?
C94 C95 H95 120.0 . . ?
C95 C96 C91 120.0 . . ?
C95 C96 H96 120.0 . . ?
C91 C96 H96 120.0 . . ?
C501 C502 C503 104.2(9) . . ?
C501 C502 H50A 110.9 . . ?
C503 C502 H50A 110.9 . . ?
C501 C502 H50B 110.9 . . ?
C503 C502 H50B 110.9 . . ?
H50A C502 H50B 108.9 . . ?
C502 C503 C504 108.3(9) . . ?
C502 C503 H50C 110.0 . . ?
C504 C503 H50C 110.0 . . ?
C502 C503 H50D 110.0 . . ?
C504 C503 H50D 110.0 . . ?
H50C C503 H50D 108.4 . . ?
O5 C504 C503 102.4(10) . . ?
O5 C504 H50E 111.3 . . ?
C503 C504 H50E 111.3 . . ?
O5 C504 H50F 111.3 . . ?
C503 C504 H50F 111.3 . . ?
H50E C504 H50F 109.2 . . ?
C501 O5 C504 108.3(12) . . ?
C601 O6 C604 108.9(7) . . ?
O6 C601 C602 108.8(8) . . ?
O6 C601 H60A 109.9 . . ?
C602 C601 H60A 109.9 . . ?
O6 C601 H60B 109.9 . . ?
C602 C601 H60B 109.9 . . ?
H60A C601 H60B 108.3 . . ?
C601 C602 C603 105.2(7) . . ?
C601 C602 H60C 110.7 . . ?
C603 C602 H60C 110.7 . . ?
C601 C602 H60D 110.7 . . ?
C603 C602 H60D 110.7 . . ?
H60C C602 H60D 108.8 . . ?
C602 C603 C604 105.4(8) . . ?
C602 C603 H60E 110.7 . . ?
C604 C603 H60E 110.7 . . ?
C602 C603 H60F 110.7 . . ?
C604 C603 H60F 110.7 . . ?
H60E C603 H60F 108.8 . . ?
C47 C44 C45 119.3(5) . . ?
C47 C44 C43 121.9(5) . . ?
C45 C44 C43 118.8(5) . . ?
C6 N2 C9 106.4(4) . . ?
C6 N2 U1 138.2(3) . . ?
C9 N2 U1 114.8(3) . . ?
C10 N3 C11 116.3(4) . . ?
C10 N3 U1 112.0(3) . . ?
C11 N3 U1 123.4(3) . . ?
C54 N4 C53 116.5(4) . . ?
C54 N4 U1 112.7(3) . . ?
C53 N4 U1 124.2(3) . . ?
C58 N5 C55 106.0(4) . . ?
C58 N5 U1 138.8(3) . . ?
C55 N5 U1 115.1(3) . . ?
C25 N6 C24 117.6(4) . . ?
C29 N7 C26 106.8(4) . . ?
C29 N7 Pb1 132.2(3) . . ?
C26 N7 Pb1 119.9(3) . . ?
C35 N8 C38 106.7(4) . . ?
C35 N8 Pb1 132.3(3) . . ?
C38 N8 Pb1 120.9(3) . . ?
C39 N9 C40 119.7(4) . . ?
O3 N10 C115 120.9(5) . . ?
O3 N10 C111 117.1(5) . . ?
C115 N10 C111 122.0(5) . . ?
N10 O3 U1 139.8(3) . . ?
C404 O4 C401 110.0(5) . . ?
C404 O4 Pb1 125.2(4) . . ?
C401 O4 Pb1 123.5(3) . . ?
C502 C501 O5 104.4(10) . . ?
C502 C501 H50G 110.9 . . ?
O5 C501 H50G 110.9 . . ?
C502 C501 H50H 110.9 . . ?
O5 C501 H50H 110.9 . . ?
H50G C501 H50H 108.9 . . ?
O6 C604 C603 106.1(7) . . ?
O6 C604 H60G 110.5 . . ?
C603 C604 H60G 110.5 . . ?
O6 C604 H60H 110.5 . . ?
C603 C604 H60H 110.5 . . ?
H60G C604 H60H 108.7 . . ?
N7 Pb1 N8 76.84(13) . . ?
N7 Pb1 O4 80.72(13) . . ?
N8 Pb1 O4 82.11(14) . . ?
O2 U1 O1 178.47(16) . . ?
O2 U1 O3 93.18(14) . . ?
O1 U1 O3 85.36(14) . . ?
O2 U1 N2 89.97(14) . . ?
O1 U1 N2 90.96(14) . . ?
O3 U1 N2 144.37(13) . . ?
O2 U1 N5 91.29(15) . . ?
O1 U1 N5 90.16(15) . . ?
O3 U1 N5 144.61(12) . . ?
N2 U1 N5 70.63(13) . . ?
O2 U1 N3 81.16(14) . . ?
O1 U1 N3 98.06(14) . . ?
O3 U1 N3 77.10(12) . . ?
N2 U1 N3 68.35(13) . . ?
N5 U1 N3 138.22(13) . . ?
O2 U1 N4 81.58(14) . . ?
O1 U1 N4 98.53(14) . . ?
O3 U1 N4 77.61(12) . . ?
N2 U1 N4 137.83(14) . . ?
N5 U1 N4 68.37(13) . . ?
N3 U1 N4 148.36(12) . . ?

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
C58 C1 C2 C3 -62.7(6) . . . . ?
C6 C1 C2 C3 63.2(6) . . . . ?
C4 C1 C2 C3 178.7(5) . . . . ?
C58 C1 C4 C5 -57.9(6) . . . . ?
C2 C1 C4 C5 61.8(6) . . . . ?
C6 C1 C4 C5 -179.8(5) . . . . ?
C58 C1 C6 N2 -39.2(7) . . . . ?
C2 C1 C6 N2 -163.0(5) . . . . ?
C4 C1 C6 N2 79.1(6) . . . . ?
C58 C1 C6 C7 148.9(5) . . . . ?
C2 C1 C6 C7 25.1(7) . . . . ?
C4 C1 C6 C7 -92.8(6) . . . . ?
N2 C6 C7 C8 2.0(6) . . . . ?
C1 C6 C7 C8 174.8(5) . . . . ?
C6 C7 C8 C9 -1.4(6) . . . . ?
C7 C8 C9 N2 0.3(6) . . . . ?
C7 C8 C9 C10 -179.7(5) . . . . ?
C8 C9 C10 N3 172.8(5) . . . . ?
N2 C9 C10 N3 -7.2(8) . . . . ?
N3 C11 C12 C13 -177.7(4) . . . . ?
C16 C11 C12 C13 0.3(7) . . . . ?
C11 C12 C13 C14 -1.4(8) . . . . ?
C12 C13 C14 C15 0.5(8) . . . . ?
C13 C14 C15 C18 -176.4(5) . . . . ?
C13 C14 C15 C16 1.4(7) . . . . ?
C12 C11 C16 C17 -179.3(4) . . . . ?
N3 C11 C16 C17 -1.4(7) . . . . ?
C12 C11 C16 C15 1.6(7) . . . . ?
N3 C11 C16 C15 179.6(4) . . . . ?
C18 C15 C16 C17 -3.8(7) . . . . ?
C14 C15 C16 C17 178.4(4) . . . . ?
C18 C15 C16 C11 175.4(4) . . . . ?
C14 C15 C16 C11 -2.4(6) . . . . ?
C11 C16 C17 C19 -175.9(4) . . . . ?
C15 C16 C17 C19 3.2(7) . . . . ?
C14 C15 C18 C20 178.6(4) . . . . ?
C16 C15 C18 C20 0.9(7) . . . . ?
C16 C17 C19 C24 177.8(4) . . . . ?
C16 C17 C19 C20 0.3(7) . . . . ?
C15 C18 C20 C21 -174.8(5) . . . . ?
C15 C18 C20 C19 2.7(7) . . . . ?
C17 C19 C20 C18 -3.2(6) . . . . ?
C24 C19 C20 C18 179.2(4) . . . . ?
C17 C19 C20 C21 174.4(4) . . . . ?
C24 C19 C20 C21 -3.2(6) . . . . ?
C18 C20 C21 C22 178.6(5) . . . . ?
C19 C20 C21 C22 1.1(7) . . . . ?
C20 C21 C22 C23 1.5(8) . . . . ?
C21 C22 C23 C24 -1.9(8) . . . . ?
C22 C23 C24 N6 177.4(4) . . . . ?
C22 C23 C24 C19 -0.2(7) . . . . ?
C17 C19 C24 C23 -174.7(4) . . . . ?
C20 C19 C24 C23 2.8(6) . . . . ?
C17 C19 C24 N6 7.5(6) . . . . ?
C20 C19 C24 N6 -175.0(4) . . . . ?
N6 C25 C26 N7 4.1(8) . . . . ?
N6 C25 C26 C27 -177.6(5) . . . . ?
N7 C26 C27 C28 -0.7(6) . . . . ?
C25 C26 C27 C28 -179.2(5) . . . . ?
C26 C27 C28 C29 1.2(6) . . . . ?
C27 C28 C29 N7 -1.3(6) . . . . ?
C27 C28 C29 C30 -176.5(5) . . . . ?
N7 C29 C30 C35 49.7(6) . . . . ?
C28 C29 C30 C35 -135.7(5) . . . . ?
N7 C29 C30 C31 -69.2(6) . . . . ?
C28 C29 C30 C31 105.4(6) . . . . ?
N7 C29 C30 C33 171.9(4) . . . . ?
C28 C29 C30 C33 -13.5(7) . . . . ?
C29 C30 C31 C32 -60.5(6) . . . . ?
C35 C30 C31 C32 177.2(5) . . . . ?
C33 C30 C31 C32 59.0(6) . . . . ?
C29 C30 C33 C34 -64.0(6) . . . . ?
C35 C30 C33 C34 60.3(7) . . . . ?
C31 C30 C33 C34 177.2(5) . . . . ?
C29 C30 C35 N8 -44.5(7) . . . . ?
C31 C30 C35 N8 75.2(6) . . . . ?
C33 C30 C35 N8 -166.9(5) . . . . ?
C29 C30 C35 C36 139.3(5) . . . . ?
C31 C30 C35 C36 -101.0(6) . . . . ?
C33 C30 C35 C36 16.9(8) . . . . ?
N8 C35 C36 C37 1.0(6) . . . . ?
C30 C35 C36 C37 177.6(5) . . . . ?
C35 C36 C37 C38 -0.4(6) . . . . ?
C36 C37 C38 N8 -0.4(6) . . . . ?
C36 C37 C38 C39 -179.9(5) . . . . ?
C37 C38 C39 N9 174.1(5) . . . . ?
N8 C38 C39 N9 -5.4(8) . . . . ?
N9 C40 C41 C42 -175.9(5) . . . . ?
C45 C40 C41 C42 1.0(8) . . . . ?
C40 C41 C42 C43 0.8(9) . . . . ?
C41 C42 C43 C44 -1.7(9) . . . . ?
C41 C40 C45 C46 175.0(5) . . . . ?
N9 C40 C45 C46 -8.0(7) . . . . ?
C41 C40 C45 C44 -2.0(8) . . . . ?
N9 C40 C45 C44 175.0(5) . . . . ?
C44 C45 C46 C49 0.9(7) . . . . ?
C40 C45 C46 C49 -176.1(5) . . . . ?
C44 C47 C48 C50 -175.3(5) . . . . ?
C44 C47 C48 C49 0.6(8) . . . . ?
C45 C46 C49 C53 174.3(5) . . . . ?
C45 C46 C49 C48 -3.1(7) . . . . ?
C47 C48 C49 C46 2.4(7) . . . . ?
C50 C48 C49 C46 178.5(5) . . . . ?
C47 C48 C49 C53 -175.2(5) . . . . ?
C50 C48 C49 C53 0.9(7) . . . . ?
C47 C48 C50 C51 174.1(6) . . . . ?
C49 C48 C50 C51 -1.8(8) . . . . ?
C48 C50 C51 C52 1.4(9) . . . . ?
C50 C51 C52 C53 0.0(9) . . . . ?
C51 C52 C53 N4 177.4(5) . . . . ?
C51 C52 C53 C49 -0.9(8) . . . . ?
C46 C49 C53 C52 -177.0(5) . . . . ?
C48 C49 C53 C52 0.5(7) . . . . ?
C46 C49 C53 N4 4.6(7) . . . . ?
C48 C49 C53 N4 -177.9(4) . . . . ?
N4 C54 C55 C56 -174.9(5) . . . . ?
N4 C54 C55 N5 7.7(7) . . . . ?
N5 C55 C56 C57 0.1(6) . . . . ?
C54 C55 C56 C57 -177.5(5) . . . . ?
C55 C56 C57 C58 0.1(6) . . . . ?
C56 C57 C58 N5 -0.3(6) . . . . ?
C56 C57 C58 C1 -174.6(5) . . . . ?
C2 C1 C58 N5 161.2(4) . . . . ?
C6 C1 C58 N5 37.4(7) . . . . ?
C4 C1 C58 N5 -79.4(6) . . . . ?
C2 C1 C58 C57 -25.1(7) . . . . ?
C6 C1 C58 C57 -149.0(5) . . . . ?
C4 C1 C58 C57 94.2(6) . . . . ?
N10 C111 C112 C113 -0.9(10) . . . . ?
C114 C113 C112 C111 0.7(11) . . . . ?
O4 C401 C402 C403 -30.3(7) . . . . ?
C404 C403 C402 C401 37.4(7) . . . . ?
C402 C403 C404 O4 -31.5(7) . . . . ?
C86 C81 C82 C83 0.0 . . . . ?
C81 C82 C83 C84 0.0 . . . . ?
C82 C83 C84 C85 0.0 . . . . ?
C83 C84 C85 C86 0.0 . . . . ?
C84 C85 C86 C81 0.0 . . . . ?
C82 C81 C86 C85 0.0 . . . . ?
C112 C113 C114 C115 0.4(11) . . . . ?
N10 C115 C114 C113 -1.3(10) . . . . ?
C96 C91 C92 C93 0.0 . . . . ?
C91 C92 C93 C94 0.0 . . . . ?
C92 C93 C94 C95 0.0 . . . . ?
C93 C94 C95 C96 0.0 . . . . ?
C94 C95 C96 C91 0.0 . . . . ?
C92 C91 C96 C95 0.0 . . . . ?
C501 C502 C503 C504 -23.3(18) . . . . ?
C502 C503 C504 O5 3.8(18) . . . . ?
C503 C504 O5 C501 19(2) . . . . ?
C604 O6 C601 C602 12.6(10) . . . . ?
O6 C601 C602 C603 2.3(10) . . . . ?
C601 C602 C603 C604 -15.5(9) . . . . ?
C48 C47 C44 C45 -2.8(8) . . . . ?
C48 C47 C44 C43 175.1(6) . . . . ?
C46 C45 C44 C47 2.1(8) . . . . ?
C40 C45 C44 C47 179.3(5) . . . . ?
C46 C45 C44 C43 -175.9(5) . . . . ?
C40 C45 C44 C43 1.2(8) . . . . ?
C42 C43 C44 C47 -177.3(6) . . . . ?
C42 C43 C44 C45 0.6(9) . . . . ?
C7 C6 N2 C9 -1.8(6) . . . . ?
C1 C6 N2 C9 -174.8(5) . . . . ?
C7 C6 N2 U1 -172.0(4) . . . . ?
C1 C6 N2 U1 15.0(8) . . . . ?
C8 C9 N2 C6 0.9(6) . . . . ?
C10 C9 N2 C6 -179.1(5) . . . . ?
C8 C9 N2 U1 173.7(3) . . . . ?
C10 C9 N2 U1 -6.2(6) . . . . ?
C9 C10 N3 C11 165.2(5) . . . . ?
C9 C10 N3 U1 15.7(6) . . . . ?
C12 C11 N3 C10 -55.4(6) . . . . ?
C16 C11 N3 C10 126.6(5) . . . . ?
C12 C11 N3 U1 90.3(5) . . . . ?
C16 C11 N3 U1 -87.7(5) . . . . ?
C55 C54 N4 C53 -165.2(4) . . . . ?
C55 C54 N4 U1 -12.5(6) . . . . ?
C52 C53 N4 C54 58.0(6) . . . . ?
C49 C53 N4 C54 -123.6(5) . . . . ?
C52 C53 N4 U1 -91.3(5) . . . . ?
C49 C53 N4 U1 87.1(5) . . . . ?
C57 C58 N5 C55 0.3(6) . . . . ?
C1 C58 N5 C55 174.8(4) . . . . ?
C57 C58 N5 U1 174.2(4) . . . . ?
C1 C58 N5 U1 -11.3(8) . . . . ?
C56 C55 N5 C58 -0.2(6) . . . . ?
C54 C55 N5 C58 177.7(4) . . . . ?
C56 C55 N5 U1 -175.8(3) . . . . ?
C54 C55 N5 U1 2.1(6) . . . . ?
C26 C25 N6 C24 -173.7(4) . . . . ?
C23 C24 N6 C25 47.0(6) . . . . ?
C19 C24 N6 C25 -135.3(5) . . . . ?
C28 C29 N7 C26 0.9(6) . . . . ?
C30 C29 N7 C26 176.4(4) . . . . ?
C28 C29 N7 Pb1 168.7(4) . . . . ?
C30 C29 N7 Pb1 -15.8(7) . . . . ?
C27 C26 N7 C29 -0.1(6) . . . . ?
C25 C26 N7 C29 178.4(5) . . . . ?
C27 C26 N7 Pb1 -169.7(3) . . . . ?
C25 C26 N7 Pb1 8.8(6) . . . . ?
C36 C35 N8 C38 -1.3(6) . . . . ?
C30 C35 N8 C38 -178.1(5) . . . . ?
C36 C35 N8 Pb1 -177.5(4) . . . . ?
C30 C35 N8 Pb1 5.6(8) . . . . ?
C37 C38 N8 C35 1.0(6) . . . . ?
C39 C38 N8 C35 -179.4(5) . . . . ?
C37 C38 N8 Pb1 177.8(3) . . . . ?
C39 C38 N8 Pb1 -2.6(6) . . . . ?
C38 C39 N9 C40 174.1(5) . . . . ?
C41 C40 N9 C39 -51.8(7) . . . . ?
C45 C40 N9 C39 131.3(5) . . . . ?
C114 C115 N10 O3 -178.5(5) . . . . ?
C114 C115 N10 C111 1.1(8) . . . . ?
C112 C111 N10 O3 179.6(5) . . . . ?
C112 C111 N10 C115 0.0(8) . . . . ?
C115 N10 O3 U1 2.9(7) . . . . ?
C111 N10 O3 U1 -176.7(4) . . . . ?
C403 C404 O4 C401 13.1(7) . . . . ?
C403 C404 O4 Pb1 -179.5(4) . . . . ?
C402 C401 O4 C404 11.1(7) . . . . ?
C402 C401 O4 Pb1 -156.6(4) . . . . ?
C503 C502 C501 O5 34.7(19) . . . . ?
C504 O5 C501 C502 -33(2) . . . . ?
C601 O6 C604 C603 -22.4(10) . . . . ?
C602 C603 C604 O6 23.2(10) . . . . ?

_refine_diff_density_max         1.357
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.114


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.068 0.053 0.162 27 3 ' '
2 0.932 -0.053 0.838 27 3 ' '
3 0.390 0.225 0.783 182 33 ' '
4 0.889 0.276 0.284 181 33 ' '
5 0.571 0.452 0.660 26 3 ' '
6 0.432 0.553 0.338 27 3 ' '
7 0.111 0.724 0.716 181 33 ' '
8 0.611 0.776 0.216 181 33 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_UO2PbLAthf
_database_code_depnum_ccdc_archive 'CCDC 1480093'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_audit_creation_date             2016-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H64 N8 O4 Pb U, C4 H8 O'
_chemical_formula_sum            'C70 H72.50 N8 O5 Pb U'
_chemical_formula_weight         1551.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C66 H64 N8 O4 U Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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                   22.7520(2)
_cell_length_b                   22.2812(2)
_cell_length_c                   24.1927(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.5987(10)
_cell_angle_gamma                90
_cell_volume                     12156.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    64694
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.2540
_cell_measurement_theta_min      3.1400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.486
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.749
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6100
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 31 -2 0.2633
0 -31 2 0.2633
-31 2 -2 0.1284
31 -2 2 0.1284
7 0 -34 0.0489
-7 0 34 0.0489

_exptl_crystal_size_max          0.555
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.098
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
0.0019 30.9919 -2.0012 0.0667 0.2862 -0.9438
-0.0019 -30.9919 2.0012 -0.0667 -0.2862 0.9438
-30.9600 2.0138 -1.9922 0.9225 -0.3277 -0.1132
30.9600 -2.0138 1.9922 -0.9225 0.3277 0.1132
6.9938 -0.0171 -33.9499 0.3244 0.9139 0.2396
-6.9938 0.0171 33.9499 -0.3244 -0.9139 -0.2396

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            332738
_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         27.485
_diffrn_reflns_theta_min         2.871
_diffrn_ambient_temperature      170(2)
_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    -88.00  10.00   1.00   30.00    --  -18.68 -77.00  60.00   98
  2  ω    -50.00  53.00   1.00   30.00    --  -18.68  23.00 -51.96  103
  3  ω    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 -60.00   47
  4  ω    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 -90.00   47
  5  ω    -37.00  50.00   1.00   30.00    --  -18.68  57.00 -90.00   87
  6  ω    -47.00  51.00   1.00   30.00    --  -18.68  77.00-180.00   98
  7  ω    -50.00  43.00   1.00   30.00    --   20.25 -38.00 -60.00   93
  8  ω     34.00  94.00   1.00   30.00    --   20.25 179.00 120.00   60
  9  ω    -89.00   4.00   1.00   30.00    --  -18.68 -38.00-150.00   93
 10  ω    -25.00  22.00   1.00   30.00    --  -18.68 -99.00 120.00   47
 11  ω    -87.00   0.00   1.00   30.00    --  -18.68 -57.00 -60.00   87
 12  ω    -93.00 -34.00   1.00   30.00    --  -18.68-179.00   0.00   59
 13  ω    -87.00   0.00   1.00   30.00    --  -18.68 -57.00 150.00   87
 14  ω    -16.00  66.00   1.00   30.00    --   20.25-109.00-170.00   82
 15  ω    -25.00  61.00   1.00   30.00    --   20.25 -99.00  30.00   86
 16  ω    -67.00 -36.00   1.00   30.00    --  -18.68 114.00  12.14   31
 17  ω    -76.00   0.00   1.00   30.00    --  -18.68 129.00-162.79   76
;
_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      -0.0287241000
_diffrn_orient_matrix_UB_12      0.0011547000
_diffrn_orient_matrix_UB_13      -0.0154739000
_diffrn_orient_matrix_UB_21      0.0126487000
_diffrn_orient_matrix_UB_22      0.0076641000
_diffrn_orient_matrix_UB_23      -0.0243182000
_diffrn_orient_matrix_UB_31      0.0020727000
_diffrn_orient_matrix_UB_32      -0.0308801000
_diffrn_orient_matrix_UB_33      -0.0066151000
_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                20316
_reflns_number_total             27853
_reflns_odcompleteness_completeness 99.83
_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 1.171.38.42b (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         1.690
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1539
_refine_ls_number_reflns         27853
_refine_ls_number_restraints     240
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      0.976
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1420
_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. Uiso/Uaniso restraints and constraints
O5 \\sim C504 \\sim C503 \\sim C502 \\sim C501: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C554 \\sim C553 \\sim C552 \\sim C551 \\sim O55: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C531 \\sim C532 \\sim C533 \\sim C534 \\sim O53: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
O3 \\sim C301 \\sim C302 \\sim C303 \\sim C304: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C504, C503, C502, C501, O5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C554, C553, C552, C551, O55
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O53, C531, C532, C533, C534
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C301, C302, C303, C304
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C534(H53A,H53B), C541(H54A,H54B), C401(H40A,H40B), C304(H30A,H30B), C542(H54C,
 H54D), C402(H40C,H40D), C404(H40E,H40F), C301(H30C,H30D), C92(H92A,H92B),
 C543(H54E,H54F), C90(H90A,H90B), C544(H54G,H54H), C31(H31A,H31B), C531(H53C,
 H53D), C403(H40G,H40H), C4(H4A,H4B), C33(H33A,H33B), C61(H61A,H61B), C2(H2A,
 H2B), C63(H63A,H63B), C551(H55A,H55B), C501(H50A,H50B), C553(H55C,H55D),
 C533(H53E,H53F), C552(H55E,H55F), C532(H53G,H53H), C303(H30E,H30F), C302(H30G,
 H30H), C554(H55G,H55H), C503(H50C,H50D), C502(H50E,H50F), C504(H50G,H50H)
4.b Aromatic/amide H refined with riding coordinates:
 C84(H84), C54(H54), C46(H46), C76(H76), C17(H17), C113(H113), C105(H105),
 C25(H25), C86(H86), C23(H23), C81(H81), C39(H39), C7(H7), C52(H52), C12(H12),
 C49(H49), C82(H82), C56(H56), C27(H27), C22(H22), C79(H79), C87(H87), C95(H95),
  C69(H69), C111(H111), C98(H98), C72(H72), C28(H28), C109(H109), C108(H108),
 C57(H57), C20(H20), C80(H80), C37(H37), C8(H8), C96(H96), C115(H115), C73(H73),
  C101(H101), C21(H21), C10(H10), C71(H71), C43(H43), C50(H50), C41(H41),
 C102(H102), C116(H116), C100(H100), C14(H14), C36(H36), C67(H67), C42(H42),
 C110(H110), C51(H51), C13(H13), C66(H66)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C91(H91A,H91B,H91C), C34(H34A,H34B,H34C), C93(H93A,H93B,
 H93C), C62(H62A,H62B,H62C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C64(H64A,H64B,
 H64C)
;
_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 0.06585(2) 0.38155(2) 0.44528(2) 0.01840(6) Uani 1 1 d . . . . .
U2 U 0.57389(2) 0.37608(2) 0.44206(2) 0.01894(6) Uani 1 1 d . . . . .
Pb1 Pb 0.11291(2) 0.17167(2) 0.46809(2) 0.02128(7) Uani 1 1 d . . . . .
Pb2 Pb 0.62096(2) 0.16506(2) 0.47122(2) 0.02132(7) Uani 1 1 d . . . . .
O1 O 0.07668(18) 0.30243(17) 0.44626(18) 0.0279(10) Uani 1 1 d . . . . .
O2 O 0.05454(17) 0.45941(17) 0.45037(18) 0.0278(9) Uani 1 1 d . . . . .
O51 O 0.58169(18) 0.29718(18) 0.44188(18) 0.0293(10) Uani 1 1 d . . . . .
O3 O 0.06248(18) 0.38058(18) 0.54638(17) 0.0290(9) Uani 1 1 d . U . . .
O52 O 0.56499(18) 0.45426(17) 0.44883(17) 0.0278(9) Uani 1 1 d . . . . .
O54 O 0.62080(18) 0.06706(19) 0.52049(18) 0.0295(10) Uani 1 1 d . . . . .
O53 O 0.56183(19) 0.37321(19) 0.54157(17) 0.0305(9) Uani 1 1 d . U . . .
O4 O 0.11755(18) 0.07394(18) 0.51653(18) 0.0295(10) Uani 1 1 d . . . . .
N00D N 0.7040(2) 0.1324(2) 0.4318(2) 0.0221(10) Uani 1 1 d . . . . .
N4 N 0.1314(2) 0.3901(2) 0.3738(2) 0.0226(10) Uani 1 1 d . . . . .
N00F N 0.5027(2) 0.1356(2) 0.4745(2) 0.0224(10) Uani 1 1 d . . . . .
N7 N 0.2233(2) 0.1809(2) 0.5392(2) 0.0260(11) Uani 1 1 d . . . . .
N00H N 0.6463(2) 0.3808(2) 0.3755(2) 0.0244(11) Uani 1 1 d . . . . .
N5 N 0.0704(2) 0.11239(19) 0.3944(2) 0.0219(10) Uani 1 1 d . . . . .
N00J N 0.7289(2) 0.1708(2) 0.5471(2) 0.0279(12) Uani 1 1 d . . . . .
N00K N 0.6790(2) 0.3829(2) 0.4883(2) 0.0226(11) Uani 1 1 d . . . . .
N00L N 0.5233(2) 0.3840(2) 0.3466(2) 0.0278(11) Uani 1 1 d . . . . .
N00M N 0.5806(2) 0.1071(2) 0.3960(2) 0.0215(10) Uani 1 1 d . . . . .
N8 N 0.1945(2) 0.14224(19) 0.4246(2) 0.0224(10) Uani 1 1 d . . . . .
N3 N 0.1730(2) 0.3936(2) 0.4850(2) 0.0260(11) Uani 1 1 d . . . . .
N6 N -0.0038(2) 0.1377(2) 0.4776(2) 0.0235(10) Uani 1 1 d . . . . .
N1 N 0.0063(2) 0.3852(2) 0.3540(2) 0.0262(11) Uani 1 1 d . . . . .
N2 N -0.0434(2) 0.3616(2) 0.4516(2) 0.0238(11) Uani 1 1 d . . . . .
N00S N 0.4627(2) 0.3595(2) 0.4392(2) 0.0244(11) Uani 1 1 d . . . . .
C6 C 0.0135(3) 0.3988(3) 0.3003(3) 0.0293(14) Uani 1 1 d . . . . .
C84 C 0.4886(2) 0.0954(3) 0.4364(2) 0.0236(12) Uani 1 1 d . . . . .
H84 H 0.4534 0.0741 0.4363 0.028 Uiso 1 1 calc R . . . .
C54 C 0.2101(3) 0.3795(2) 0.4491(3) 0.0262(13) Uani 1 1 d . . . . .
H54 H 0.2501 0.3736 0.4619 0.031 Uiso 1 1 calc R . . . .
C55 C 0.1899(3) 0.3735(3) 0.3924(3) 0.0276(13) Uani 1 1 d . . . . .
C46 C 0.2166(2) 0.3042(2) 0.5678(2) 0.0198(11) Uani 1 1 d . . . . .
H46 H 0.2037 0.2923 0.5314 0.024 Uiso 1 1 calc R . . . .
C26 C 0.0159(3) 0.0863(2) 0.3963(2) 0.0240(12) Uani 1 1 d . . . . .
C112 C 0.6993(2) 0.4002(3) 0.5446(3) 0.0256(13) Uani 1 1 d . . . . .
C11 C -0.0725(2) 0.3577(2) 0.5004(3) 0.0235(13) Uani 1 1 d . . . . .
C88 C 0.6021(2) 0.0896(2) 0.3490(2) 0.0211(12) Uani 1 1 d . . . . .
C76 C 0.4505(2) 0.2476(2) 0.5017(2) 0.0232(12) Uani 1 1 d . . . . .
H76 H 0.4698 0.2458 0.4701 0.028 Uiso 1 1 calc R . . . .
C534 C 0.5692(3) 0.3216(3) 0.5789(3) 0.0372(14) Uani 1 1 d . U . . .
H53A H 0.6069 0.3021 0.5769 0.045 Uiso 1 1 calc R . . . .
H53B H 0.5377 0.2927 0.5691 0.045 Uiso 1 1 calc R . . . .
C47 C 0.2159(2) 0.3651(2) 0.5816(2) 0.0206(12) Uani 1 1 d . . . . .
C94 C 0.7111(3) 0.1203(2) 0.3781(3) 0.0254(13) Uani 1 1 d . . . . .
C18 C -0.0549(2) 0.1958(2) 0.5424(2) 0.0211(12) Uani 1 1 d . . . . .
C17 C -0.0523(2) 0.2483(2) 0.5123(2) 0.0230(12) Uani 1 1 d . . . . .
H17 H -0.0350 0.2479 0.4796 0.028 Uiso 1 1 calc R . . . .
C58 C 0.1261(3) 0.3891(2) 0.3172(3) 0.0256(13) Uani 1 1 d . . . . .
C24 C -0.0338(2) 0.1389(3) 0.5246(2) 0.0219(12) Uani 1 1 d . . . . .
C30 C 0.1463(3) 0.1165(2) 0.3265(2) 0.0241(12) Uani 1 1 d . . . . .
C53 C 0.1973(2) 0.4099(3) 0.5401(3) 0.0270(13) Uani 1 1 d . . . . .
C113 C 0.7186(3) 0.3677(2) 0.4556(3) 0.0271(13) Uani 1 1 d . . . . .
H113 H 0.7575 0.3602 0.4712 0.032 Uiso 1 1 calc R . . . .
C117 C 0.6465(3) 0.3810(2) 0.3199(3) 0.0289(14) Uani 1 1 d . . . . .
C83 C 0.4694(2) 0.1387(2) 0.5196(2) 0.0225(12) Uani 1 1 d . . . . .
C97 C 0.7602(3) 0.1452(3) 0.4601(3) 0.0304(14) Uani 1 1 d . . . . .
C89 C 0.6600(3) 0.1109(2) 0.3319(2) 0.0237(12) Uani 1 1 d . . . . .
C77 C 0.4465(2) 0.1959(2) 0.5339(2) 0.0188(11) Uani 1 1 d . . . . .
C35 C 0.1992(3) 0.1279(2) 0.3709(3) 0.0258(13) Uani 1 1 d . . . . .
C105 C 0.7212(2) 0.2949(2) 0.5742(3) 0.0233(12) Uani 1 1 d . . . . .
H105 H 0.7114 0.2823 0.5375 0.028 Uiso 1 1 calc R . . . .
C541 C 0.6233(3) 0.0708(3) 0.5806(3) 0.0340(15) Uani 1 1 d . . . . .
H54A H 0.5841 0.0657 0.5916 0.041 Uiso 1 1 calc R . . . .
H54B H 0.6390 0.1093 0.5942 0.041 Uiso 1 1 calc R . . . .
C106 C 0.7176(2) 0.3560(3) 0.5863(3) 0.0234(12) Uani 1 1 d . . . . .
C29 C 0.0903(2) 0.0947(2) 0.3466(2) 0.0213(12) Uani 1 1 d . . . . .
C85 C 0.5250(2) 0.0832(2) 0.3951(2) 0.0221(12) Uani 1 1 d . . . . .
C401 C 0.1205(3) 0.0774(3) 0.5769(3) 0.0326(15) Uani 1 1 d . . . . .
H40A H 0.0816 0.0713 0.5883 0.039 Uiso 1 1 calc R . . . .
H40B H 0.1357 0.1161 0.5906 0.039 Uiso 1 1 calc R . . . .
C38 C 0.2510(3) 0.1545(3) 0.4500(3) 0.0271(13) Uani 1 1 d . . . . .
C9 C -0.0543(3) 0.3830(3) 0.3551(3) 0.0316(15) Uani 1 1 d . . . . .
C304 C 0.0693(3) 0.3295(3) 0.5845(3) 0.0361(14) Uani 1 1 d . U . . .
H30A H 0.1067 0.3093 0.5823 0.043 Uiso 1 1 calc R . . . .
H30B H 0.0373 0.3009 0.5750 0.043 Uiso 1 1 calc R . . . .
C16 C -0.0753(2) 0.3023(2) 0.5302(2) 0.0221(12) Uani 1 1 d . . . . .
C25 C -0.0183(2) 0.0974(3) 0.4403(3) 0.0246(12) Uani 1 1 d . . . . .
H25 H -0.0523 0.0747 0.4422 0.029 Uiso 1 1 calc R . . . .
C40 C 0.2415(2) 0.1991(2) 0.5943(3) 0.0225(12) Uani 1 1 d . . . . .
C86 C 0.5112(3) 0.0490(3) 0.3465(3) 0.0302(14) Uani 1 1 d . . . . .
H86 H 0.4765 0.0275 0.3360 0.036 Uiso 1 1 calc R . . . .
C23 C -0.0414(3) 0.0875(3) 0.5543(3) 0.0281(14) Uani 1 1 d . . . . .
H23 H -0.0291 0.0508 0.5417 0.034 Uiso 1 1 calc R . . . .
C104 C 0.7389(2) 0.2519(3) 0.6153(2) 0.0228(12) Uani 1 1 d . . . . .
C107 C 0.7342(2) 0.3758(3) 0.6423(3) 0.0257(13) Uani 1 1 d . . . . .
C114 C 0.7029(3) 0.3627(3) 0.3981(3) 0.0288(14) Uani 1 1 d . . . . .
C32 C 0.1181(3) 0.2297(3) 0.3330(3) 0.0403(17) Uani 1 1 d . . . . .
H32A H 0.1093 0.2650 0.3107 0.060 Uiso 1 1 calc GR . . . .
H32B H 0.1517 0.2373 0.3605 0.060 Uiso 1 1 calc GR . . . .
H32C H 0.0845 0.2194 0.3512 0.060 Uiso 1 1 calc GR . . . .
C542 C 0.6641(3) 0.0201(3) 0.6034(3) 0.0352(15) Uani 1 1 d . . . . .
H54C H 0.6882 0.0317 0.6378 0.042 Uiso 1 1 calc R . . . .
H54D H 0.6417 -0.0157 0.6100 0.042 Uiso 1 1 calc R . . . .
C81 C 0.4321(3) 0.0926(3) 0.5989(3) 0.0312(14) Uani 1 1 d . . . . .
H81 H 0.4273 0.0581 0.6195 0.037 Uiso 1 1 calc R . . . .
C75 C 0.4258(2) 0.3022(2) 0.5164(3) 0.0228(12) Uani 1 1 d . . . . .
C70 C 0.4293(2) 0.3566(2) 0.4856(3) 0.0233(12) Uani 1 1 d . . . . .
C103 C 0.7546(2) 0.2726(3) 0.6720(2) 0.0264(13) Uani 1 1 d . . . . .
C68 C 0.4623(3) 0.3867(3) 0.3439(3) 0.0354(15) Uani 1 1 d . . . . .
C402 C 0.1623(3) 0.0277(3) 0.5986(3) 0.0344(15) Uani 1 1 d . . . . .
H40C H 0.1406 -0.0084 0.6054 0.041 Uiso 1 1 calc R . . . .
H40D H 0.1864 0.0396 0.6329 0.041 Uiso 1 1 calc R . . . .
C65 C 0.5358(3) 0.3995(3) 0.2955(3) 0.0323(15) Uani 1 1 d . . . . .
C45 C 0.2364(2) 0.2611(3) 0.6079(3) 0.0254(13) Uani 1 1 d . . . . .
C99 C 0.7447(2) 0.1903(3) 0.6023(3) 0.0260(13) Uani 1 1 d . . . . .
C39 C 0.2636(3) 0.1726(3) 0.5075(3) 0.0289(14) Uani 1 1 d . . . . .
H39 H 0.3030 0.1786 0.5224 0.035 Uiso 1 1 calc R . . . .
C7 C -0.0420(3) 0.4060(3) 0.2675(3) 0.0443(18) Uani 1 1 d . . . . .
H7 H -0.0485 0.4157 0.2298 0.053 Uiso 1 1 calc R . . . .
C52 C 0.2006(3) 0.4700(3) 0.5538(3) 0.0315(14) Uani 1 1 d . . . . .
H52 H 0.1890 0.4987 0.5265 0.038 Uiso 1 1 calc R . . . .
C44 C 0.2558(2) 0.2808(3) 0.6647(2) 0.0232(12) Uani 1 1 d . . . . .
C12 C -0.0998(3) 0.4086(2) 0.5194(3) 0.0283(14) Uani 1 1 d . . . . .
H12 H -0.1004 0.4437 0.4985 0.034 Uiso 1 1 calc R . . . .
C91 C 0.6338(3) 0.2234(3) 0.3399(3) 0.0410(17) Uani 1 1 d . . . . .
H91A H 0.6299 0.2604 0.3194 0.062 Uiso 1 1 calc GR . . . .
H91B H 0.6651 0.2270 0.3704 0.062 Uiso 1 1 calc GR . . . .
H91C H 0.5972 0.2147 0.3540 0.062 Uiso 1 1 calc GR . . . .
C404 C 0.1559(3) 0.0261(3) 0.5015(3) 0.0320(14) Uani 1 1 d . . . . .
H40E H 0.1753 0.0374 0.4697 0.038 Uiso 1 1 calc R . . . .
H40F H 0.1335 -0.0105 0.4926 0.038 Uiso 1 1 calc R . . . .
C49 C 0.2541(3) 0.3408(3) 0.6776(3) 0.0271(13) Uani 1 1 d . . . . .
H49 H 0.2658 0.3529 0.7142 0.032 Uiso 1 1 calc R . . . .
C82 C 0.4614(2) 0.0891(3) 0.5506(3) 0.0263(13) Uani 1 1 d . . . . .
H82 H 0.4755 0.0522 0.5400 0.032 Uiso 1 1 calc R . . . .
C56 C 0.2198(3) 0.3614(3) 0.3466(3) 0.0332(15) Uani 1 1 d . . . . .
H56 H 0.2590 0.3491 0.3477 0.040 Uiso 1 1 calc R . . . .
C301 C 0.0519(3) 0.4360(3) 0.5785(3) 0.0421(15) Uani 1 1 d . U . . .
H30C H 0.0854 0.4632 0.5803 0.050 Uiso 1 1 calc R . . . .
H30D H 0.0165 0.4567 0.5619 0.050 Uiso 1 1 calc R . . . .
C92 C 0.6796(3) 0.0670(3) 0.2878(3) 0.0292(14) Uani 1 1 d . . . . .
H92A H 0.6488 0.0660 0.2560 0.035 Uiso 1 1 calc R . . . .
H92B H 0.7151 0.0829 0.2750 0.035 Uiso 1 1 calc R . . . .
C543 C 0.7019(3) 0.0101(3) 0.5570(3) 0.0341(15) Uani 1 1 d . . . . .
H54E H 0.7337 0.0393 0.5587 0.041 Uiso 1 1 calc R . . . .
H54F H 0.7187 -0.0300 0.5587 0.041 Uiso 1 1 calc R . . . .
O55 O 0.8722(3) 0.1703(3) 0.2896(3) 0.0788(19) Uani 1 1 d . U . . .
C27 C 0.0014(3) 0.0512(3) 0.3488(3) 0.0305(14) Uani 1 1 d . . . . .
H27 H -0.0327 0.0282 0.3401 0.037 Uiso 1 1 calc R . . . .
C90 C 0.6480(3) 0.1733(2) 0.3019(3) 0.0297(14) Uani 1 1 d . . . . .
H90A H 0.6828 0.1845 0.2850 0.036 Uiso 1 1 calc R . . . .
H90B H 0.6153 0.1689 0.2722 0.036 Uiso 1 1 calc R . . . .
C22 C -0.0679(3) 0.0901(3) 0.6042(3) 0.0331(15) Uani 1 1 d . . . . .
H22 H -0.0725 0.0550 0.6239 0.040 Uiso 1 1 calc R . . . .
C79 C 0.3921(2) 0.2535(3) 0.5962(3) 0.0294(14) Uani 1 1 d . . . . .
H79 H 0.3728 0.2554 0.6278 0.035 Uiso 1 1 calc R . . . .
C87 C 0.5592(3) 0.0536(2) 0.3173(3) 0.0278(13) Uani 1 1 d . . . . .
H87 H 0.5626 0.0361 0.2830 0.033 Uiso 1 1 calc R . . . .
C95 C 0.7711(3) 0.1243(3) 0.3717(3) 0.0347(16) Uani 1 1 d . . . . .
H95 H 0.7875 0.1179 0.3390 0.042 Uiso 1 1 calc R . . . .
C69 C 0.4334(3) 0.3751(3) 0.3919(3) 0.0327(15) Uani 1 1 d . . . . .
H69 H 0.3924 0.3790 0.3890 0.039 Uiso 1 1 calc R . . . .
C544 C 0.6582(3) 0.0183(3) 0.5059(3) 0.0329(15) Uani 1 1 d . . . . .
H54G H 0.6780 0.0289 0.4741 0.039 Uiso 1 1 calc R . . . .
H54H H 0.6352 -0.0179 0.4972 0.039 Uiso 1 1 calc R . . . .
C111 C 0.6989(3) 0.4596(3) 0.5580(3) 0.0330(15) Uani 1 1 d . . . . .
H111 H 0.6866 0.4877 0.5304 0.040 Uiso 1 1 calc R . . . .
C1 C 0.0717(3) 0.4153(3) 0.2817(3) 0.0281(13) Uani 1 1 d . . . . .
C98 C 0.7704(3) 0.1624(2) 0.5167(3) 0.0270(13) Uani 1 1 d . . . . .
H98 H 0.8094 0.1680 0.5330 0.032 Uiso 1 1 calc R . . . .
C72 C 0.3699(2) 0.4094(3) 0.5456(3) 0.0293(15) Uani 1 1 d . . . . .
H72 H 0.3513 0.4446 0.5544 0.035 Uiso 1 1 calc R . . . .
C28 C 0.0475(3) 0.0569(3) 0.3171(3) 0.0292(14) Uani 1 1 d . . . . .
H28 H 0.0498 0.0391 0.2826 0.035 Uiso 1 1 calc R . . . .
C109 C 0.7322(3) 0.4383(3) 0.6535(3) 0.0313(14) Uani 1 1 d . . . . .
H109 H 0.7419 0.4514 0.6901 0.038 Uiso 1 1 calc R . . . .
C48 C 0.2352(2) 0.3846(3) 0.6370(2) 0.0232(12) Uani 1 1 d . . . . .
C108 C 0.7520(3) 0.3328(3) 0.6839(3) 0.0264(13) Uani 1 1 d . . . . .
H108 H 0.7623 0.3456 0.7205 0.032 Uiso 1 1 calc R . . . .
C60 C 0.5966(3) 0.4074(3) 0.2788(3) 0.0361(16) Uani 1 1 d . . . . .
C34 C 0.1819(3) 0.0097(3) 0.3044(3) 0.0405(17) Uani 1 1 d . . . . .
H34A H 0.1954 -0.0136 0.2752 0.061 Uiso 1 1 calc GR . . . .
H34B H 0.1480 -0.0093 0.3165 0.061 Uiso 1 1 calc GR . . . .
H34C H 0.2131 0.0126 0.3353 0.061 Uiso 1 1 calc GR . . . .
C19 C -0.0814(2) 0.1967(3) 0.5928(3) 0.0240(13) Uani 1 1 d . . . . .
C57 C 0.1796(3) 0.3714(3) 0.2997(3) 0.0334(15) Uani 1 1 d . . . . .
H57 H 0.1869 0.3671 0.2630 0.040 Uiso 1 1 calc R . . . .
C20 C -0.1042(2) 0.2507(3) 0.6105(3) 0.0282(13) Uani 1 1 d . . . . .
H20 H -0.1209 0.2514 0.6436 0.034 Uiso 1 1 calc R . . . .
C80 C 0.4113(3) 0.1456(3) 0.6149(3) 0.0295(14) Uani 1 1 d . . . . .
H80 H 0.3929 0.1477 0.6469 0.035 Uiso 1 1 calc R . . . .
C37 C 0.2914(3) 0.1468(3) 0.4122(3) 0.0378(16) Uani 1 1 d . . . . .
H37 H 0.3323 0.1513 0.4193 0.045 Uiso 1 1 calc R . . . .
C31 C 0.1322(3) 0.1782(3) 0.2959(3) 0.0308(14) Uani 1 1 d . . . . .
H31A H 0.1661 0.1895 0.2777 0.037 Uiso 1 1 calc R . . . .
H31B H 0.0988 0.1726 0.2670 0.037 Uiso 1 1 calc R . . . .
C8 C -0.0853(3) 0.3957(4) 0.3022(3) 0.051(2) Uani 1 1 d . . . . .
H8 H -0.1262 0.3970 0.2924 0.061 Uiso 1 1 calc R . . . .
C78 C 0.4174(2) 0.1987(3) 0.5827(2) 0.0236(12) Uani 1 1 d . . . . .
C96 C 0.8016(3) 0.1396(3) 0.4231(3) 0.0371(16) Uani 1 1 d . . . . .
H96 H 0.8423 0.1452 0.4313 0.045 Uiso 1 1 calc R . . . .
C115 C 0.7371(3) 0.3502(3) 0.3559(3) 0.0371(16) Uani 1 1 d . . . . .
H115 H 0.7761 0.3367 0.3602 0.044 Uiso 1 1 calc R . . . .
C531 C 0.5476(3) 0.4275(3) 0.5735(3) 0.0440(16) Uani 1 1 d . U . . .
H53C H 0.5807 0.4551 0.5784 0.053 Uiso 1 1 calc R . . . .
H53D H 0.5130 0.4481 0.5547 0.053 Uiso 1 1 calc R . . . .
C73 C 0.3665(2) 0.3587(3) 0.5781(3) 0.0322(15) Uani 1 1 d . . . . .
H73 H 0.3459 0.3599 0.6089 0.039 Uiso 1 1 calc R . . . .
C403 C 0.2002(3) 0.0180(3) 0.5524(3) 0.0323(14) Uani 1 1 d . . . . .
H40G H 0.2318 0.0474 0.5539 0.039 Uiso 1 1 calc R . . . .
H40H H 0.2172 -0.0220 0.5540 0.039 Uiso 1 1 calc R . . . .
C4 C 0.0715(3) 0.3990(3) 0.2194(3) 0.0367(16) Uani 1 1 d . . . . .
H4A H 0.0398 0.4212 0.1977 0.044 Uiso 1 1 calc R . . . .
H4B H 0.1086 0.4126 0.2079 0.044 Uiso 1 1 calc R . . . .
C101 C 0.7794(3) 0.1711(3) 0.7008(3) 0.0351(15) Uani 1 1 d . . . . .
H101 H 0.7927 0.1437 0.7287 0.042 Uiso 1 1 calc R . . . .
C21 C -0.0863(3) 0.1420(3) 0.6234(3) 0.0318(14) Uani 1 1 d . . . . .
H21 H -0.1024 0.1428 0.6568 0.038 Uiso 1 1 calc R . . . .
C15 C -0.1026(2) 0.3030(3) 0.5802(2) 0.0233(12) Uani 1 1 d . . . . .
C10 C -0.0773(3) 0.3721(3) 0.4044(3) 0.0311(14) Uani 1 1 d . . . . .
H10 H -0.1183 0.3723 0.4040 0.037 Uiso 1 1 calc R . . . .
C71 C 0.4012(3) 0.4078(3) 0.4997(3) 0.0333(15) Uani 1 1 d . . . . .
H71 H 0.4030 0.4422 0.4783 0.040 Uiso 1 1 calc R . . . .
C93 C 0.6920(3) 0.0029(3) 0.3083(3) 0.0404(17) Uani 1 1 d . . . . .
H93A H 0.7079 -0.0198 0.2800 0.061 Uiso 1 1 calc GR . . . .
H93B H 0.6557 -0.0153 0.3161 0.061 Uiso 1 1 calc GR . . . .
H93C H 0.7201 0.0035 0.3416 0.061 Uiso 1 1 calc GR . . . .
C33 C 0.1650(3) 0.0728(3) 0.2827(3) 0.0318(14) Uani 1 1 d . . . . .
H33A H 0.1326 0.0693 0.2524 0.038 Uiso 1 1 calc R . . . .
H33B H 0.1986 0.0899 0.2673 0.038 Uiso 1 1 calc R . . . .
C43 C 0.2773(3) 0.2359(3) 0.7055(3) 0.0293(14) Uani 1 1 d . . . . .
H43 H 0.2887 0.2474 0.7424 0.035 Uiso 1 1 calc R . . . .
C50 C 0.2371(3) 0.4466(3) 0.6497(3) 0.0310(14) Uani 1 1 d . . . . .
H50 H 0.2490 0.4590 0.6861 0.037 Uiso 1 1 calc R . . . .
C41 C 0.2637(3) 0.1584(3) 0.6342(3) 0.0297(14) Uani 1 1 d . . . . .
H41 H 0.2675 0.1183 0.6248 0.036 Uiso 1 1 calc R . . . .
C102 C 0.7744(3) 0.2291(3) 0.7139(3) 0.0318(14) Uani 1 1 d . . . . .
H102 H 0.7840 0.2413 0.7508 0.038 Uiso 1 1 calc R . . . .
C116 C 0.7014(3) 0.3620(3) 0.3061(3) 0.0422(18) Uani 1 1 d . . . . .
H116 H 0.7119 0.3580 0.2704 0.051 Uiso 1 1 calc R . . . .
C100 C 0.7644(3) 0.1503(3) 0.6444(3) 0.0335(15) Uani 1 1 d . . . . .
H100 H 0.7681 0.1098 0.6362 0.040 Uiso 1 1 calc R . . . .
C14 C -0.1278(3) 0.3573(3) 0.5984(3) 0.0333(15) Uani 1 1 d . . . . .
H14 H -0.1454 0.3575 0.6309 0.040 Uiso 1 1 calc R . . . .
C74 C 0.3948(2) 0.3045(2) 0.5643(3) 0.0229(12) Uani 1 1 d . . . . .
C36 C 0.2586(3) 0.1312(3) 0.3620(3) 0.0356(16) Uani 1 1 d . . . . .
H36 H 0.2733 0.1242 0.3285 0.043 Uiso 1 1 calc R . . . .
C67 C 0.4369(4) 0.4054(4) 0.2915(3) 0.056(2) Uani 1 1 d . . . . .
H67 H 0.3969 0.4119 0.2797 0.067 Uiso 1 1 calc R . . . .
C61 C 0.6092(4) 0.4776(3) 0.2754(3) 0.049(2) Uani 1 1 d . . . . .
H61A H 0.6480 0.4832 0.2637 0.059 Uiso 1 1 calc R . . . .
H61B H 0.5802 0.4949 0.2469 0.059 Uiso 1 1 calc R . . . .
C42 C 0.2812(3) 0.1781(3) 0.6913(3) 0.0341(15) Uani 1 1 d . . . . .
H42 H 0.2953 0.1501 0.7184 0.041 Uiso 1 1 calc R . . . .
C2 C 0.0765(3) 0.4851(3) 0.2888(3) 0.0371(16) Uani 1 1 d . . . . .
H2A H 0.0421 0.5031 0.2671 0.045 Uiso 1 1 calc R . . . .
H2B H 0.0744 0.4945 0.3277 0.045 Uiso 1 1 calc R . . . .
C110 C 0.7170(3) 0.4793(3) 0.6134(3) 0.0381(16) Uani 1 1 d . . . . .
H110 H 0.7182 0.5200 0.6219 0.046 Uiso 1 1 calc R . . . .
C51 C 0.2216(3) 0.4886(3) 0.6090(3) 0.0363(16) Uani 1 1 d . . . . .
H51 H 0.2248 0.5292 0.6175 0.044 Uiso 1 1 calc R . . . .
C13 C -0.1261(3) 0.4087(3) 0.5682(3) 0.0358(16) Uani 1 1 d . . . . .
H13 H -0.1424 0.4438 0.5802 0.043 Uiso 1 1 calc R . . . .
C62 C 0.6074(3) 0.5106(3) 0.3274(3) 0.053(2) Uani 1 1 d . . . . .
H62A H 0.6163 0.5521 0.3218 0.079 Uiso 1 1 calc GR . . . .
H62B H 0.6361 0.4941 0.3560 0.079 Uiso 1 1 calc GR . . . .
H62C H 0.5685 0.5073 0.3385 0.079 Uiso 1 1 calc GR . . . .
C66 C 0.4828(3) 0.4122(3) 0.2604(3) 0.048(2) Uani 1 1 d . . . . .
H66 H 0.4795 0.4233 0.2231 0.058 Uiso 1 1 calc R . . . .
C63 C 0.5985(4) 0.3833(3) 0.2190(3) 0.0467(19) Uani 1 1 d . . . . .
H63A H 0.5699 0.4058 0.1937 0.056 Uiso 1 1 calc R . . . .
H63B H 0.6374 0.3917 0.2087 0.056 Uiso 1 1 calc R . . . .
C551 C 0.9088(4) 0.1621(4) 0.2487(5) 0.072(2) Uani 1 1 d . U . . .
H55A H 0.8865 0.1656 0.2117 0.087 Uiso 1 1 calc R . . . .
H55B H 0.9277 0.1230 0.2522 0.087 Uiso 1 1 calc R . . . .
C5 C 0.0637(4) 0.3325(3) 0.2047(3) 0.048(2) Uani 1 1 d . . . . .
H5A H 0.0616 0.3275 0.1650 0.072 Uiso 1 1 calc GR . . . .
H5B H 0.0278 0.3179 0.2167 0.072 Uiso 1 1 calc GR . . . .
H5C H 0.0969 0.3103 0.2229 0.072 Uiso 1 1 calc GR . . . .
O5 O 0.3838(4) 0.1748(4) 0.2973(4) 0.122(3) Uani 1 1 d . U . . .
C3 C 0.1300(3) 0.5144(3) 0.2728(4) 0.061(2) Uani 1 1 d . . . . .
H3A H 0.1312 0.5086 0.2336 0.091 Uiso 1 1 calc GR . . . .
H3B H 0.1647 0.4970 0.2936 0.091 Uiso 1 1 calc GR . . . .
H3C H 0.1288 0.5566 0.2807 0.091 Uiso 1 1 calc GR . . . .
C501 C 0.4130(6) 0.1698(5) 0.2524(6) 0.100(3) Uani 1 1 d . U . . .
H50A H 0.3882 0.1838 0.2192 0.120 Uiso 1 1 calc R . . . .
H50B H 0.4234 0.1282 0.2468 0.120 Uiso 1 1 calc R . . . .
C553 C 0.9546(4) 0.2263(5) 0.3181(5) 0.087(3) Uani 1 1 d . U . . .
H55C H 0.9840 0.2023 0.3410 0.104 Uiso 1 1 calc R . . . .
H55D H 0.9631 0.2684 0.3255 0.104 Uiso 1 1 calc R . . . .
C533 C 0.5667(5) 0.3462(4) 0.6361(3) 0.069(2) Uani 1 1 d . U . . .
H53E H 0.5455 0.3189 0.6578 0.083 Uiso 1 1 calc R . . . .
H53F H 0.6063 0.3522 0.6556 0.083 Uiso 1 1 calc R . . . .
C64 C 0.5859(4) 0.3171(3) 0.2098(3) 0.068(3) Uani 1 1 d . . . . .
H64A H 0.5847 0.3079 0.1709 0.101 Uiso 1 1 calc GR . . . .
H64B H 0.5484 0.3074 0.2216 0.101 Uiso 1 1 calc GR . . . .
H64C H 0.6166 0.2940 0.2310 0.101 Uiso 1 1 calc GR . . . .
C552 C 0.9551(5) 0.2129(5) 0.2594(5) 0.092(3) Uani 1 1 d . U . . .
H55E H 0.9939 0.1994 0.2523 0.111 Uiso 1 1 calc R . . . .
H55F H 0.9435 0.2476 0.2363 0.111 Uiso 1 1 calc R . . . .
C532 C 0.5356(5) 0.4028(5) 0.6279(4) 0.077(3) Uani 1 1 d . U . . .
H53G H 0.5496 0.4305 0.6577 0.093 Uiso 1 1 calc R . . . .
H53H H 0.4934 0.3968 0.6277 0.093 Uiso 1 1 calc R . . . .
C303 C 0.0677(5) 0.3535(4) 0.6416(4) 0.077(3) Uani 1 1 d . U . . .
H30E H 0.0424 0.3288 0.6617 0.092 Uiso 1 1 calc R . . . .
H30F H 0.1072 0.3541 0.6623 0.092 Uiso 1 1 calc R . . . .
C302 C 0.0446(5) 0.4127(5) 0.6348(4) 0.083(3) Uani 1 1 d . U . . .
H30G H 0.0653 0.4387 0.6632 0.100 Uiso 1 1 calc R . . . .
H30H H 0.0029 0.4126 0.6394 0.100 Uiso 1 1 calc R . . . .
C554 C 0.8971(4) 0.2119(5) 0.3294(5) 0.088(3) Uani 1 1 d . U . . .
H55G H 0.8989 0.1950 0.3665 0.105 Uiso 1 1 calc R . . . .
H55H H 0.8729 0.2479 0.3277 0.105 Uiso 1 1 calc R . . . .
C503 C 0.4665(6) 0.2285(6) 0.3202(6) 0.123(4) Uani 1 1 d . U . . .
H50C H 0.4956 0.2068 0.3456 0.148 Uiso 1 1 calc R . . . .
H50D H 0.4762 0.2709 0.3225 0.148 Uiso 1 1 calc R . . . .
C502 C 0.4674(6) 0.2070(6) 0.2632(6) 0.120(4) Uani 1 1 d . U . . .
H50E H 0.5026 0.1832 0.2603 0.144 Uiso 1 1 calc R . . . .
H50F H 0.4661 0.2402 0.2371 0.144 Uiso 1 1 calc R . . . .
C504 C 0.4115(6) 0.2193(6) 0.3339(6) 0.125(4) Uani 1 1 d . U . . .
H50G H 0.3889 0.2563 0.3300 0.150 Uiso 1 1 calc R . . . .
H50H H 0.4139 0.2059 0.3723 0.150 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 O1 1.780(4) . ?
U1 O2 1.760(4) . ?
U1 O3 2.457(4) . ?
U1 N4 2.435(5) . ?
U1 N3 2.513(5) . ?
U1 N1 2.435(5) . ?
U1 N2 2.550(5) . ?
U2 O51 1.767(4) . ?
U2 O52 1.764(4) . ?
U2 O53 2.460(4) . ?
U2 N00H 2.454(5) . ?
U2 N00K 2.506(4) . ?
U2 N00L 2.447(5) . ?
U2 N00S 2.549(5) . ?
Pb1 O4 2.469(4) . ?
Pb1 N5 2.324(5) . ?
Pb1 N8 2.346(5) . ?
Pb2 O54 2.488(4) . ?
Pb2 N00D 2.343(5) . ?
Pb2 N00F 2.780(5) . ?
Pb2 N00M 2.319(4) . ?
O3 C304 1.461(7) . ?
O3 C301 1.496(8) . ?
O54 C541 1.450(7) . ?
O54 C544 1.453(7) . ?
O53 C534 1.457(7) . ?
O53 C531 1.493(8) . ?
O4 C401 1.456(7) . ?
O4 C404 1.455(7) . ?
N00D C94 1.356(8) . ?
N00D C97 1.398(7) . ?
N4 C55 1.398(7) . ?
N4 C58 1.360(7) . ?
N00F C84 1.295(7) . ?
N00F C83 1.412(7) . ?
N7 C40 1.402(8) . ?
N7 C39 1.286(8) . ?
N00H C117 1.344(8) . ?
N00H C114 1.392(7) . ?
N5 C26 1.377(7) . ?
N5 C29 1.355(7) . ?
N00J C99 1.404(8) . ?
N00J C98 1.286(8) . ?
N00K C112 1.432(7) . ?
N00K C113 1.319(7) . ?
N00L C68 1.381(8) . ?
N00L C65 1.351(8) . ?
N00M C88 1.352(7) . ?
N00M C85 1.371(7) . ?
N8 C35 1.355(8) . ?
N8 C38 1.378(7) . ?
N3 C54 1.327(8) . ?
N3 C53 1.420(8) . ?
N6 C24 1.400(7) . ?
N6 C25 1.285(7) . ?
N1 C6 1.364(8) . ?
N1 C9 1.385(8) . ?
N2 C11 1.430(7) . ?
N2 C10 1.313(8) . ?
N00S C70 1.436(7) . ?
N00S C69 1.295(8) . ?
C6 C7 1.409(9) . ?
C6 C1 1.499(9) . ?
C84 H84 0.9300 . ?
C84 C85 1.405(8) . ?
C54 H54 0.9300 . ?
C54 C55 1.394(9) . ?
C55 C56 1.398(9) . ?
C46 H46 0.9300 . ?
C46 C47 1.398(7) . ?
C46 C45 1.399(8) . ?
C26 C25 1.422(8) . ?
C26 C27 1.393(8) . ?
C112 C106 1.432(8) . ?
C112 C111 1.363(8) . ?
C11 C16 1.435(8) . ?
C11 C12 1.398(8) . ?
C88 C89 1.508(8) . ?
C88 C87 1.410(8) . ?
C76 H76 0.9300 . ?
C76 C77 1.400(7) . ?
C76 C75 1.406(8) . ?
C534 H53A 0.9700 . ?
C534 H53B 0.9700 . ?
C534 C533 1.498(10) . ?
C47 C53 1.441(8) . ?
C47 C48 1.420(8) . ?
C94 C89 1.518(8) . ?
C94 C95 1.395(8) . ?
C18 C17 1.384(8) . ?
C18 C24 1.442(8) . ?
C18 C19 1.430(8) . ?
C17 H17 0.9300 . ?
C17 C16 1.402(8) . ?
C58 C1 1.526(8) . ?
C58 C57 1.399(8) . ?
C24 C23 1.375(8) . ?
C30 C35 1.525(8) . ?
C30 C29 1.503(8) . ?
C30 C31 1.575(8) . ?
C30 C33 1.542(8) . ?
C53 C52 1.380(8) . ?
C113 H113 0.9300 . ?
C113 C114 1.394(9) . ?
C117 C60 1.526(9) . ?
C117 C116 1.402(9) . ?
C83 C77 1.436(7) . ?
C83 C82 1.362(8) . ?
C97 C98 1.413(9) . ?
C97 C96 1.387(9) . ?
C89 C92 1.554(8) . ?
C89 C90 1.577(7) . ?
C77 C78 1.429(8) . ?
C35 C36 1.398(8) . ?
C105 H105 0.9300 . ?
C105 C106 1.398(8) . ?
C105 C104 1.400(8) . ?
C541 H54A 0.9700 . ?
C541 H54B 0.9700 . ?
C541 C542 1.519(9) . ?
C106 C107 1.427(8) . ?
C29 C28 1.408(8) . ?
C85 C86 1.401(8) . ?
C401 H40A 0.9700 . ?
C401 H40B 0.9700 . ?
C401 C402 1.507(8) . ?
C38 C39 1.438(9) . ?
C38 C37 1.390(9) . ?
C9 C8 1.406(9) . ?
C9 C10 1.386(9) . ?
C304 H30A 0.9700 . ?
C304 H30B 0.9700 . ?
C304 C303 1.487(10) . ?
C16 C15 1.430(8) . ?
C25 H25 0.9300 . ?
C40 C45 1.428(8) . ?
C40 C41 1.371(8) . ?
C86 H86 0.9300 . ?
C86 C87 1.380(9) . ?
C23 H23 0.9300 . ?
C23 C22 1.420(9) . ?
C104 C103 1.446(8) . ?
C104 C99 1.418(8) . ?
C107 C109 1.420(8) . ?
C107 C108 1.410(8) . ?
C114 C115 1.391(9) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 C31 1.517(8) . ?
C542 H54C 0.9700 . ?
C542 H54D 0.9700 . ?
C542 C543 1.517(9) . ?
C81 H81 0.9300 . ?
C81 C82 1.421(9) . ?
C81 C80 1.349(9) . ?
C75 C70 1.430(8) . ?
C75 C74 1.436(8) . ?
C70 C71 1.373(8) . ?
C103 C108 1.377(8) . ?
C103 C102 1.432(8) . ?
C68 C69 1.431(9) . ?
C68 C67 1.386(10) . ?
C402 H40C 0.9700 . ?
C402 H40D 0.9700 . ?
C402 C403 1.516(9) . ?
C65 C60 1.502(9) . ?
C65 C66 1.408(9) . ?
C45 C44 1.454(8) . ?
C99 C100 1.383(9) . ?
C39 H39 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.396(10) . ?
C52 H52 0.9300 . ?
C52 C51 1.418(9) . ?
C44 C49 1.374(8) . ?
C44 C43 1.445(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(9) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C91 C90 1.508(8) . ?
C404 H40E 0.9700 . ?
C404 H40F 0.9700 . ?
C404 C403 1.496(9) . ?
C49 H49 0.9300 . ?
C49 C48 1.410(8) . ?
C82 H82 0.9300 . ?
C56 H56 0.9300 . ?
C56 C57 1.378(9) . ?
C301 H30C 0.9700 . ?
C301 H30D 0.9700 . ?
C301 C302 1.487(11) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C92 C93 1.526(8) . ?
C543 H54E 0.9700 . ?
C543 H54F 0.9700 . ?
C543 C544 1.492(9) . ?
O55 C551 1.386(12) . ?
O55 C554 1.401(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.386(9) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
C22 H22 0.9300 . ?
C22 C21 1.333(9) . ?
C79 H79 0.9300 . ?
C79 C78 1.407(8) . ?
C79 C74 1.379(8) . ?
C87 H87 0.9300 . ?
C95 H95 0.9300 . ?
C95 C96 1.384(9) . ?
C69 H69 0.9300 . ?
C544 H54G 0.9700 . ?
C544 H54H 0.9700 . ?
C111 H111 0.9300 . ?
C111 C110 1.418(9) . ?
C1 C4 1.550(8) . ?
C1 C2 1.567(8) . ?
C98 H98 0.9300 . ?
C72 H72 0.9300 . ?
C72 C73 1.385(9) . ?
C72 C71 1.395(9) . ?
C28 H28 0.9300 . ?
C109 H109 0.9300 . ?
C109 C110 1.344(9) . ?
C48 C50 1.414(8) . ?
C108 H108 0.9300 . ?
C60 C61 1.593(8) . ?
C60 C63 1.549(9) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C34 C33 1.531(8) . ?
C19 C20 1.401(8) . ?
C19 C21 1.438(8) . ?
C57 H57 0.9300 . ?
C20 H20 0.9300 . ?
C20 C15 1.381(8) . ?
C80 H80 0.9300 . ?
C80 C78 1.433(8) . ?
C37 H37 0.9300 . ?
C37 C36 1.384(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C8 H8 0.9300 . ?
C96 H96 0.9300 . ?
C115 H115 0.9300 . ?
C115 C116 1.385(10) . ?
C531 H53C 0.9700 . ?
C531 H53D 0.9700 . ?
C531 C532 1.483(11) . ?
C73 H73 0.9300 . ?
C73 C74 1.428(8) . ?
C403 H40G 0.9700 . ?
C403 H40H 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.528(9) . ?
C101 H101 0.9300 . ?
C101 C102 1.340(9) . ?
C101 C100 1.439(9) . ?
C21 H21 0.9300 . ?
C15 C14 1.433(8) . ?
C10 H10 0.9300 . ?
C71 H71 0.9300 . ?
C93 H93A 0.9600 . ?
C93 H93B 0.9600 . ?
C93 H93C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C43 H43 0.9300 . ?
C43 C42 1.340(9) . ?
C50 H50 0.9300 . ?
C50 C51 1.371(9) . ?
C41 H41 0.9300 . ?
C41 C42 1.454(9) . ?
C102 H102 0.9300 . ?
C116 H116 0.9300 . ?
C100 H100 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.360(9) . ?
C36 H36 0.9300 . ?
C67 H67 0.9300 . ?
C67 C66 1.372(11) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 C62 1.463(10) . ?
C42 H42 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.476(9) . ?
C110 H110 0.9300 . ?
C51 H51 0.9300 . ?
C13 H13 0.9300 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C66 H66 0.9300 . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.513(9) . ?
C551 H55A 0.9700 . ?
C551 H55B 0.9700 . ?
C551 C552 1.544(13) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
O5 C501 1.350(14) . ?
O5 C504 1.422(13) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C501 H50A 0.9700 . ?
C501 H50B 0.9700 . ?
C501 C502 1.483(14) . ?
C553 H55C 0.9700 . ?
C553 H55D 0.9700 . ?
C553 C552 1.453(15) . ?
C553 C554 1.407(13) . ?
C533 H53E 0.9700 . ?
C533 H53F 0.9700 . ?
C533 C532 1.447(13) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C552 H55E 0.9700 . ?
C552 H55F 0.9700 . ?
C532 H53G 0.9700 . ?
C532 H53H 0.9700 . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C302 1.422(13) . ?
C302 H30G 0.9700 . ?
C302 H30H 0.9700 . ?
C554 H55G 0.9700 . ?
C554 H55H 0.9700 . ?
C503 H50C 0.9700 . ?
C503 H50D 0.9700 . ?
C503 C502 1.462(17) . ?
C503 C504 1.352(16) . ?
C502 H50E 0.9700 . ?
C502 H50F 0.9700 . ?
C504 H50G 0.9700 . ?
C504 H50H 0.9700 . ?

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 90.03(17) . . ?
O1 U1 N4 89.44(17) . . ?
O1 U1 N3 88.58(17) . . ?
O1 U1 N1 95.99(18) . . ?
O1 U1 N2 87.74(16) . . ?
O2 U1 O1 175.1(2) . . ?
O2 U1 O3 85.12(17) . . ?
O2 U1 N4 94.67(17) . . ?
O2 U1 N3 90.66(17) . . ?
O2 U1 N1 87.81(17) . . ?
O2 U1 N2 90.86(17) . . ?
O3 U1 N3 77.10(16) . . ?
O3 U1 N2 77.27(15) . . ?
N4 U1 O3 144.09(15) . . ?
N4 U1 N3 66.99(16) . . ?
N4 U1 N1 70.89(16) . . ?
N4 U1 N2 138.56(16) . . ?
N3 U1 N2 154.10(17) . . ?
N1 U1 O3 144.74(15) . . ?
N1 U1 N3 137.57(17) . . ?
N1 U1 N2 68.33(16) . . ?
O51 U2 O53 90.04(17) . . ?
O51 U2 N00H 87.99(17) . . ?
O51 U2 N00K 88.37(17) . . ?
O51 U2 N00L 96.00(18) . . ?
O51 U2 N00S 87.42(17) . . ?
O52 U2 O51 174.62(19) . . ?
O52 U2 O53 84.59(17) . . ?
O52 U2 N00H 96.53(17) . . ?
O52 U2 N00K 90.73(17) . . ?
O52 U2 N00L 88.32(17) . . ?
O52 U2 N00S 91.16(17) . . ?
O53 U2 N00K 77.77(15) . . ?
O53 U2 N00S 77.50(15) . . ?
N00H U2 O53 144.60(15) . . ?
N00H U2 N00K 66.85(17) . . ?
N00H U2 N00S 137.63(16) . . ?
N00K U2 N00S 154.90(17) . . ?
N00L U2 O53 145.69(16) . . ?
N00L U2 N00H 69.55(17) . . ?
N00L U2 N00K 135.97(17) . . ?
N00L U2 N00S 69.11(17) . . ?
N5 Pb1 O4 81.37(15) . . ?
N5 Pb1 N8 76.73(16) . . ?
N8 Pb1 O4 88.85(14) . . ?
O54 Pb2 N00F 73.53(13) . . ?
N00D Pb2 O54 88.55(15) . . ?
N00D Pb2 N00F 140.68(15) . . ?
N00M Pb2 O54 82.07(15) . . ?
N00M Pb2 N00D 76.37(16) . . ?
N00M Pb2 N00F 66.84(15) . . ?
C304 O3 U1 128.4(4) . . ?
C304 O3 C301 109.0(5) . . ?
C301 O3 U1 122.6(4) . . ?
C541 O54 Pb2 115.3(4) . . ?
C541 O54 C544 109.9(5) . . ?
C544 O54 Pb2 120.1(4) . . ?
C534 O53 U2 127.5(4) . . ?
C534 O53 C531 109.4(5) . . ?
C531 O53 U2 123.1(4) . . ?
C401 O4 Pb1 115.0(3) . . ?
C404 O4 Pb1 121.2(4) . . ?
C404 O4 C401 109.9(4) . . ?
C94 N00D Pb2 131.0(4) . . ?
C94 N00D C97 107.0(5) . . ?
C97 N00D Pb2 118.1(4) . . ?
C55 N4 U1 113.5(4) . . ?
C58 N4 U1 137.2(4) . . ?
C58 N4 C55 105.8(5) . . ?
C84 N00F Pb2 107.1(4) . . ?
C84 N00F C83 118.4(5) . . ?
C83 N00F Pb2 129.2(3) . . ?
C39 N7 C40 117.8(5) . . ?
C117 N00H U2 138.4(4) . . ?
C117 N00H C114 105.6(5) . . ?
C114 N00H U2 113.3(4) . . ?
C26 N5 Pb1 120.0(4) . . ?
C29 N5 Pb1 132.0(4) . . ?
C29 N5 C26 107.9(5) . . ?
C98 N00J C99 118.3(5) . . ?
C112 N00K U2 127.5(4) . . ?
C113 N00K U2 113.8(4) . . ?
C113 N00K C112 118.6(5) . . ?
C68 N00L U2 113.1(4) . . ?
C65 N00L U2 138.8(4) . . ?
C65 N00L C68 106.1(5) . . ?
C88 N00M Pb2 132.1(4) . . ?
C88 N00M C85 108.1(5) . . ?
C85 N00M Pb2 119.8(4) . . ?
C35 N8 Pb1 131.6(4) . . ?
C35 N8 C38 106.8(5) . . ?
C38 N8 Pb1 119.4(4) . . ?
C54 N3 U1 113.2(4) . . ?
C54 N3 C53 118.2(5) . . ?
C53 N3 U1 128.6(4) . . ?
C25 N6 C24 118.4(5) . . ?
C6 N1 U1 138.4(4) . . ?
C6 N1 C9 105.8(5) . . ?
C9 N1 U1 114.6(4) . . ?
C11 N2 U1 128.4(4) . . ?
C10 N2 U1 112.5(4) . . ?
C10 N2 C11 116.5(5) . . ?
C70 N00S U2 127.7(4) . . ?
C69 N00S U2 112.2(4) . . ?
C69 N00S C70 116.0(5) . . ?
N1 C6 C7 110.5(6) . . ?
N1 C6 C1 124.3(5) . . ?
C7 C6 C1 124.3(6) . . ?
N00F C84 H84 119.2 . . ?
N00F C84 C85 121.6(5) . . ?
C85 C84 H84 119.2 . . ?
N3 C54 H54 119.6 . . ?
N3 C54 C55 120.8(5) . . ?
C55 C54 H54 119.6 . . ?
N4 C55 C56 109.8(6) . . ?
C54 C55 N4 117.8(5) . . ?
C54 C55 C56 131.7(6) . . ?
C47 C46 H46 119.6 . . ?
C47 C46 C45 120.9(5) . . ?
C45 C46 H46 119.6 . . ?
N5 C26 C25 122.4(5) . . ?
N5 C26 C27 109.1(5) . . ?
C27 C26 C25 128.5(5) . . ?
C106 C112 N00K 120.8(5) . . ?
C111 C112 N00K 118.5(6) . . ?
C111 C112 C106 120.7(6) . . ?
N2 C11 C16 121.5(5) . . ?
C12 C11 N2 119.7(5) . . ?
C12 C11 C16 118.8(6) . . ?
N00M C88 C89 124.5(5) . . ?
N00M C88 C87 108.7(5) . . ?
C87 C88 C89 126.6(5) . . ?
C77 C76 H76 119.6 . . ?
C77 C76 C75 120.9(5) . . ?
C75 C76 H76 119.6 . . ?
O53 C534 H53A 110.6 . . ?
O53 C534 H53B 110.6 . . ?
O53 C534 C533 105.6(6) . . ?
H53A C534 H53B 108.7 . . ?
C533 C534 H53A 110.6 . . ?
C533 C534 H53B 110.6 . . ?
C46 C47 C53 121.1(5) . . ?
C46 C47 C48 120.8(5) . . ?
C48 C47 C53 118.2(5) . . ?
N00D C94 C89 123.8(5) . . ?
N00D C94 C95 109.6(5) . . ?
C95 C94 C89 126.4(6) . . ?
C17 C18 C24 123.2(5) . . ?
C17 C18 C19 119.2(5) . . ?
C19 C18 C24 117.5(5) . . ?
C18 C17 H17 119.3 . . ?
C18 C17 C16 121.3(5) . . ?
C16 C17 H17 119.3 . . ?
N4 C58 C1 121.2(5) . . ?
N4 C58 C57 110.2(5) . . ?
C57 C58 C1 127.7(6) . . ?
N6 C24 C18 118.4(5) . . ?
C23 C24 N6 121.1(5) . . ?
C23 C24 C18 120.4(6) . . ?
C35 C30 C31 106.1(5) . . ?
C35 C30 C33 109.0(5) . . ?
C29 C30 C35 116.8(5) . . ?
C29 C30 C31 107.9(5) . . ?
C29 C30 C33 110.0(5) . . ?
C33 C30 C31 106.6(5) . . ?
N3 C53 C47 121.4(5) . . ?
C52 C53 N3 118.4(6) . . ?
C52 C53 C47 120.2(6) . . ?
N00K C113 H113 119.5 . . ?
N00K C113 C114 120.9(5) . . ?
C114 C113 H113 119.5 . . ?
N00H C117 C60 123.6(6) . . ?
N00H C117 C116 111.1(6) . . ?
C116 C117 C60 124.8(6) . . ?
N00F C83 C77 118.6(5) . . ?
C82 C83 N00F 120.7(5) . . ?
C82 C83 C77 120.7(6) . . ?
N00D C97 C98 123.6(6) . . ?
C96 C97 N00D 108.7(6) . . ?
C96 C97 C98 127.7(6) . . ?
C88 C89 C94 117.0(5) . . ?
C88 C89 C92 109.4(5) . . ?
C88 C89 C90 107.4(5) . . ?
C94 C89 C92 109.3(5) . . ?
C94 C89 C90 106.6(5) . . ?
C92 C89 C90 106.7(5) . . ?
C76 C77 C83 122.9(5) . . ?
C76 C77 C78 119.8(5) . . ?
C78 C77 C83 117.3(5) . . ?
N8 C35 C30 124.0(5) . . ?
N8 C35 C36 109.6(5) . . ?
C36 C35 C30 126.1(6) . . ?
C106 C105 H105 118.7 . . ?
C106 C105 C104 122.6(6) . . ?
C104 C105 H105 118.7 . . ?
O54 C541 H54A 110.7 . . ?
O54 C541 H54B 110.7 . . ?
O54 C541 C542 105.2(5) . . ?
H54A C541 H54B 108.8 . . ?
C542 C541 H54A 110.7 . . ?
C542 C541 H54B 110.7 . . ?
C105 C106 C112 122.9(6) . . ?
C105 C106 C107 118.9(5) . . ?
C107 C106 C112 118.2(5) . . ?
N5 C29 C30 125.0(5) . . ?
N5 C29 C28 108.8(5) . . ?
C28 C29 C30 126.0(5) . . ?
N00M C85 C84 122.9(5) . . ?
N00M C85 C86 109.1(5) . . ?
C86 C85 C84 127.8(5) . . ?
O4 C401 H40A 110.8 . . ?
O4 C401 H40B 110.8 . . ?
O4 C401 C402 104.7(5) . . ?
H40A C401 H40B 108.9 . . ?
C402 C401 H40A 110.8 . . ?
C402 C401 H40B 110.8 . . ?
N8 C38 C39 122.9(5) . . ?
N8 C38 C37 109.8(6) . . ?
C37 C38 C39 127.2(6) . . ?
N1 C9 C8 110.9(6) . . ?
N1 C9 C10 120.9(6) . . ?
C10 C9 C8 128.1(6) . . ?
O3 C304 H30A 110.3 . . ?
O3 C304 H30B 110.3 . . ?
O3 C304 C303 107.0(6) . . ?
H30A C304 H30B 108.6 . . ?
C303 C304 H30A 110.3 . . ?
C303 C304 H30B 110.3 . . ?
C17 C16 C11 122.7(5) . . ?
C17 C16 C15 119.5(5) . . ?
C15 C16 C11 117.9(5) . . ?
N6 C25 C26 122.2(5) . . ?
N6 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
N7 C40 C45 118.4(5) . . ?
C41 C40 N7 120.8(5) . . ?
C41 C40 C45 120.8(6) . . ?
C85 C86 H86 126.7 . . ?
C87 C86 C85 106.6(5) . . ?
C87 C86 H86 126.7 . . ?
C24 C23 H23 119.8 . . ?
C24 C23 C22 120.5(6) . . ?
C22 C23 H23 119.8 . . ?
C105 C104 C103 117.8(5) . . ?
C105 C104 C99 122.1(6) . . ?
C99 C104 C103 120.0(5) . . ?
C109 C107 C106 118.3(6) . . ?
C108 C107 C106 118.9(5) . . ?
C108 C107 C109 122.8(6) . . ?
N00H C114 C113 118.1(5) . . ?
C115 C114 N00H 110.3(6) . . ?
C115 C114 C113 131.0(6) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
C541 C542 H54C 111.2 . . ?
C541 C542 H54D 111.2 . . ?
H54C C542 H54D 109.1 . . ?
C543 C542 C541 102.7(5) . . ?
C543 C542 H54C 111.2 . . ?
C543 C542 H54D 111.2 . . ?
C82 C81 H81 119.9 . . ?
C80 C81 H81 119.9 . . ?
C80 C81 C82 120.3(6) . . ?
C76 C75 C70 123.4(6) . . ?
C76 C75 C74 119.4(5) . . ?
C70 C75 C74 117.3(5) . . ?
C75 C70 N00S 121.0(5) . . ?
C71 C70 N00S 118.0(5) . . ?
C71 C70 C75 120.9(6) . . ?
C108 C103 C104 119.8(5) . . ?
C108 C103 C102 121.9(6) . . ?
C102 C103 C104 118.2(6) . . ?
N00L C68 C69 121.3(6) . . ?
N00L C68 C67 110.5(7) . . ?
C67 C68 C69 128.0(7) . . ?
C401 C402 H40C 110.9 . . ?
C401 C402 H40D 110.9 . . ?
C401 C402 C403 104.1(5) . . ?
H40C C402 H40D 109.0 . . ?
C403 C402 H40C 110.9 . . ?
C403 C402 H40D 110.9 . . ?
N00L C65 C60 126.1(6) . . ?
N00L C65 C66 109.6(6) . . ?
C66 C65 C60 124.1(6) . . ?
C46 C45 C40 122.2(6) . . ?
C46 C45 C44 118.6(5) . . ?
C40 C45 C44 119.1(5) . . ?
N00J C99 C104 119.3(5) . . ?
C100 C99 N00J 121.2(5) . . ?
C100 C99 C104 119.4(6) . . ?
N7 C39 C38 123.4(5) . . ?
N7 C39 H39 118.3 . . ?
C38 C39 H39 118.3 . . ?
C6 C7 H7 126.4 . . ?
C8 C7 C6 107.2(6) . . ?
C8 C7 H7 126.4 . . ?
C53 C52 H52 119.7 . . ?
C53 C52 C51 120.6(6) . . ?
C51 C52 H52 119.7 . . ?
C49 C44 C45 119.6(5) . . ?
C49 C44 C43 122.4(6) . . ?
C43 C44 C45 118.0(5) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 C11 122.5(6) . . ?
C13 C12 H12 118.7 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
O4 C404 H40E 110.9 . . ?
O4 C404 H40F 110.9 . . ?
O4 C404 C403 104.1(5) . . ?
H40E C404 H40F 109.0 . . ?
C403 C404 H40E 110.9 . . ?
C403 C404 H40F 110.9 . . ?
C44 C49 H49 119.0 . . ?
C44 C49 C48 122.0(6) . . ?
C48 C49 H49 119.0 . . ?
C83 C82 C81 121.3(6) . . ?
C83 C82 H82 119.4 . . ?
C81 C82 H82 119.4 . . ?
C55 C56 H56 126.8 . . ?
C57 C56 C55 106.4(6) . . ?
C57 C56 H56 126.8 . . ?
O3 C301 H30C 111.1 . . ?
O3 C301 H30D 111.1 . . ?
H30C C301 H30D 109.0 . . ?
C302 C301 O3 103.5(6) . . ?
C302 C301 H30C 111.1 . . ?
C302 C301 H30D 111.1 . . ?
C89 C92 H92A 108.5 . . ?
C89 C92 H92B 108.5 . . ?
H92A C92 H92B 107.5 . . ?
C93 C92 C89 115.1(5) . . ?
C93 C92 H92A 108.5 . . ?
C93 C92 H92B 108.5 . . ?
C542 C543 H54E 111.3 . . ?
C542 C543 H54F 111.3 . . ?
H54E C543 H54F 109.2 . . ?
C544 C543 C542 102.4(5) . . ?
C544 C543 H54E 111.3 . . ?
C544 C543 H54F 111.3 . . ?
C551 O55 C554 110.7(7) . . ?
C26 C27 H27 126.5 . . ?
C28 C27 C26 106.9(5) . . ?
C28 C27 H27 126.5 . . ?
C89 C90 H90A 108.7 . . ?
C89 C90 H90B 108.7 . . ?
C91 C90 C89 114.3(5) . . ?
C91 C90 H90A 108.7 . . ?
C91 C90 H90B 108.7 . . ?
H90A C90 H90B 107.6 . . ?
C23 C22 H22 119.3 . . ?
C21 C22 C23 121.3(6) . . ?
C21 C22 H22 119.3 . . ?
C78 C79 H79 118.8 . . ?
C74 C79 H79 118.8 . . ?
C74 C79 C78 122.3(6) . . ?
C88 C87 H87 126.3 . . ?
C86 C87 C88 107.5(5) . . ?
C86 C87 H87 126.3 . . ?
C94 C95 H95 126.3 . . ?
C96 C95 C94 107.3(6) . . ?
C96 C95 H95 126.3 . . ?
N00S C69 C68 121.9(6) . . ?
N00S C69 H69 119.0 . . ?
C68 C69 H69 119.0 . . ?
O54 C544 C543 103.8(5) . . ?
O54 C544 H54G 111.0 . . ?
O54 C544 H54H 111.0 . . ?
C543 C544 H54G 111.0 . . ?
C543 C544 H54H 111.0 . . ?
H54G C544 H54H 109.0 . . ?
C112 C111 H111 119.5 . . ?
C112 C111 C110 121.0(6) . . ?
C110 C111 H111 119.5 . . ?
C6 C1 C58 114.8(5) . . ?
C6 C1 C4 110.3(5) . . ?
C6 C1 C2 105.2(5) . . ?
C58 C1 C4 110.8(5) . . ?
C58 C1 C2 106.1(5) . . ?
C4 C1 C2 109.4(5) . . ?
N00J C98 C97 123.7(5) . . ?
N00J C98 H98 118.1 . . ?
C97 C98 H98 118.1 . . ?
C73 C72 H72 119.8 . . ?
C73 C72 C71 120.3(5) . . ?
C71 C72 H72 119.8 . . ?
C29 C28 H28 126.4 . . ?
C27 C28 C29 107.2(5) . . ?
C27 C28 H28 126.4 . . ?
C107 C109 H109 118.7 . . ?
C110 C109 C107 122.7(6) . . ?
C110 C109 H109 118.7 . . ?
C49 C48 C47 118.2(5) . . ?
C49 C48 C50 121.8(6) . . ?
C50 C48 C47 120.0(6) . . ?
C107 C108 H108 119.0 . . ?
C103 C108 C107 121.9(6) . . ?
C103 C108 H108 119.0 . . ?
C117 C60 C61 106.8(5) . . ?
C117 C60 C63 111.5(6) . . ?
C65 C60 C117 114.3(5) . . ?
C65 C60 C61 107.9(6) . . ?
C65 C60 C63 110.5(6) . . ?
C63 C60 C61 105.4(5) . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
C18 C19 C21 119.9(5) . . ?
C20 C19 C18 119.2(5) . . ?
C20 C19 C21 120.9(6) . . ?
C58 C57 H57 126.1 . . ?
C56 C57 C58 107.8(6) . . ?
C56 C57 H57 126.1 . . ?
C19 C20 H20 119.2 . . ?
C15 C20 C19 121.7(6) . . ?
C15 C20 H20 119.2 . . ?
C81 C80 H80 119.9 . . ?
C81 C80 C78 120.3(6) . . ?
C78 C80 H80 119.9 . . ?
C38 C37 H37 126.8 . . ?
C36 C37 C38 106.4(6) . . ?
C36 C37 H37 126.8 . . ?
C30 C31 H31A 108.4 . . ?
C30 C31 H31B 108.4 . . ?
C32 C31 C30 115.3(5) . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C9 C8 H8 127.1 . . ?
C7 C8 C9 105.7(6) . . ?
C7 C8 H8 127.1 . . ?
C77 C78 C80 120.2(5) . . ?
C79 C78 C77 118.5(5) . . ?
C79 C78 C80 121.2(6) . . ?
C97 C96 H96 126.3 . . ?
C95 C96 C97 107.4(6) . . ?
C95 C96 H96 126.3 . . ?
C114 C115 H115 126.8 . . ?
C116 C115 C114 106.4(6) . . ?
C116 C115 H115 126.8 . . ?
O53 C531 H53C 111.0 . . ?
O53 C531 H53D 111.0 . . ?
H53C C531 H53D 109.0 . . ?
C532 C531 O53 103.7(6) . . ?
C532 C531 H53C 111.0 . . ?
C532 C531 H53D 111.0 . . ?
C72 C73 H73 120.1 . . ?
C72 C73 C74 119.7(6) . . ?
C74 C73 H73 120.1 . . ?
C402 C403 H40G 111.4 . . ?
C402 C403 H40H 111.4 . . ?
C404 C403 C402 101.7(5) . . ?
C404 C403 H40G 111.4 . . ?
C404 C403 H40H 111.4 . . ?
H40G C403 H40H 109.3 . . ?
C1 C4 H4A 108.3 . . ?
C1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C5 C4 C1 116.1(5) . . ?
C5 C4 H4A 108.3 . . ?
C5 C4 H4B 108.3 . . ?
C102 C101 H101 119.4 . . ?
C102 C101 C100 121.3(6) . . ?
C100 C101 H101 119.4 . . ?
C22 C21 C19 120.4(6) . . ?
C22 C21 H21 119.8 . . ?
C19 C21 H21 119.8 . . ?
C16 C15 C14 120.3(5) . . ?
C20 C15 C16 119.1(5) . . ?
C20 C15 C14 120.6(6) . . ?
N2 C10 C9 122.3(6) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C70 C71 C72 121.5(6) . . ?
C70 C71 H71 119.3 . . ?
C72 C71 H71 119.3 . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C30 C33 H33A 108.5 . . ?
C30 C33 H33B 108.5 . . ?
C34 C33 C30 115.0(5) . . ?
C34 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C44 C43 H43 119.4 . . ?
C42 C43 C44 121.2(6) . . ?
C42 C43 H43 119.4 . . ?
C48 C50 H50 119.6 . . ?
C51 C50 C48 120.8(6) . . ?
C51 C50 H50 119.6 . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 119.9(6) . . ?
C42 C41 H41 120.0 . . ?
C103 C102 H102 119.6 . . ?
C101 C102 C103 120.9(6) . . ?
C101 C102 H102 119.6 . . ?
C117 C116 H116 126.7 . . ?
C115 C116 C117 106.7(6) . . ?
C115 C116 H116 126.7 . . ?
C99 C100 C101 120.3(6) . . ?
C99 C100 H100 119.9 . . ?
C101 C100 H100 119.9 . . ?
C15 C14 H14 119.8 . . ?
C13 C14 C15 120.3(6) . . ?
C13 C14 H14 119.8 . . ?
C79 C74 C75 119.1(5) . . ?
C79 C74 C73 120.7(6) . . ?
C73 C74 C75 120.2(5) . . ?
C35 C36 H36 126.3 . . ?
C37 C36 C35 107.3(6) . . ?
C37 C36 H36 126.3 . . ?
C68 C67 H67 126.9 . . ?
C66 C67 C68 106.2(7) . . ?
C66 C67 H67 126.9 . . ?
C60 C61 H61A 108.5 . . ?
C60 C61 H61B 108.5 . . ?
H61A C61 H61B 107.5 . . ?
C62 C61 C60 115.1(6) . . ?
C62 C61 H61A 108.5 . . ?
C62 C61 H61B 108.5 . . ?
C43 C42 C41 121.0(6) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C1 C2 H2A 108.0 . . ?
C1 C2 H2B 108.0 . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 C1 117.3(6) . . ?
C3 C2 H2A 108.0 . . ?
C3 C2 H2B 108.0 . . ?
C111 C110 H110 120.4 . . ?
C109 C110 C111 119.1(6) . . ?
C109 C110 H110 120.4 . . ?
C52 C51 H51 120.0 . . ?
C50 C51 C52 120.0(6) . . ?
C50 C51 H51 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(6) . . ?
C14 C13 H13 120.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C65 C66 H66 126.2 . . ?
C67 C66 C65 107.5(6) . . ?
C67 C66 H66 126.2 . . ?
C60 C63 H63A 108.1 . . ?
C60 C63 H63B 108.1 . . ?
H63A C63 H63B 107.3 . . ?
C64 C63 C60 116.6(6) . . ?
C64 C63 H63A 108.1 . . ?
C64 C63 H63B 108.1 . . ?
O55 C551 H55A 110.9 . . ?
O55 C551 H55B 110.9 . . ?
O55 C551 C552 104.1(8) . . ?
H55A C551 H55B 109.0 . . ?
C552 C551 H55A 110.9 . . ?
C552 C551 H55B 110.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C501 O5 C504 109.5(10) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O5 C501 H50A 110.2 . . ?
O5 C501 H50B 110.2 . . ?
O5 C501 C502 107.5(11) . . ?
H50A C501 H50B 108.5 . . ?
C502 C501 H50A 110.2 . . ?
C502 C501 H50B 110.2 . . ?
H55C C553 H55D 108.7 . . ?
C552 C553 H55C 110.6 . . ?
C552 C553 H55D 110.6 . . ?
C554 C553 H55C 110.6 . . ?
C554 C553 H55D 110.6 . . ?
C554 C553 C552 105.7(9) . . ?
C534 C533 H53E 110.6 . . ?
C534 C533 H53F 110.6 . . ?
H53E C533 H53F 108.8 . . ?
C532 C533 C534 105.6(7) . . ?
C532 C533 H53E 110.6 . . ?
C532 C533 H53F 110.6 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C551 C552 H55E 111.2 . . ?
C551 C552 H55F 111.2 . . ?
C553 C552 C551 102.8(9) . . ?
C553 C552 H55E 111.2 . . ?
C553 C552 H55F 111.2 . . ?
H55E C552 H55F 109.1 . . ?
C531 C532 H53G 110.2 . . ?
C531 C532 H53H 110.2 . . ?
C533 C532 C531 107.6(7) . . ?
C533 C532 H53G 110.2 . . ?
C533 C532 H53H 110.2 . . ?
H53G C532 H53H 108.5 . . ?
C304 C303 H30E 110.5 . . ?
C304 C303 H30F 110.5 . . ?
H30E C303 H30F 108.7 . . ?
C302 C303 C304 106.3(7) . . ?
C302 C303 H30E 110.5 . . ?
C302 C303 H30F 110.5 . . ?
C301 C302 H30G 109.6 . . ?
C301 C302 H30H 109.6 . . ?
C303 C302 C301 110.2(8) . . ?
C303 C302 H30G 109.6 . . ?
C303 C302 H30H 109.6 . . ?
H30G C302 H30H 108.1 . . ?
O55 C554 C553 108.5(10) . . ?
O55 C554 H55G 110.0 . . ?
O55 C554 H55H 110.0 . . ?
C553 C554 H55G 110.0 . . ?
C553 C554 H55H 110.0 . . ?
H55G C554 H55H 108.4 . . ?
H50C C503 H50D 108.4 . . ?
C502 C503 H50C 110.1 . . ?
C502 C503 H50D 110.1 . . ?
C504 C503 H50C 110.1 . . ?
C504 C503 H50D 110.1 . . ?
C504 C503 C502 108.1(12) . . ?
C501 C502 H50E 111.1 . . ?
C501 C502 H50F 111.1 . . ?
C503 C502 C501 103.5(11) . . ?
C503 C502 H50E 111.1 . . ?
C503 C502 H50F 111.1 . . ?
H50E C502 H50F 109.0 . . ?
O5 C504 H50G 110.2 . . ?
O5 C504 H50H 110.2 . . ?
C503 C504 O5 107.5(13) . . ?
C503 C504 H50G 110.2 . . ?
C503 C504 H50H 110.2 . . ?
H50G C504 H50H 108.5 . . ?

_shelx_SHELXL_version_number     2014/7
_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 2.629
_oxdiff_exptl_absorpt_empirical_full_min 0.665
