# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_2_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 2047325'
loop_
_audit_author_name
_audit_author_address
'David M. Jenkins'
;University of Tennessee
United States of America
;
_audit_update_record             
;
2020-11-30 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 B4 N16 Th'
_chemical_formula_sum            'C36 H48 B4 N16 Th'
_chemical_formula_weight         980.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

# start Validation Reply Form
_vrf_PLAT602_2_a_sqd             
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: Platon SQUEEZE was used to removed disordered toluene.
;
# end Validation Reply Form
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                   18.388(3)
_cell_length_b                   11.1669(16)
_cell_length_c                   22.459(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.007(5)
_cell_angle_gamma                90
_cell_volume                     4600.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_min      2.351
_cell_measurement_theta_max      31.555

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             1944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.732
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.256
_exptl_absorpt_coefficient_mu    3.285
_shelx_estimated_absorpt_T_min   0.197
_shelx_estimated_absorpt_T_max   0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4951
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microsource
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            90914
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.221
_diffrn_reflns_theta_max         31.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15370
_reflns_number_gt                14338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0144P)²+1.9518P] 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         15370
_refine_ls_number_parameters     522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_ref         0.0470
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.010
_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
Th1 Th 0.74742(2) 0.29280(2) 0.67545(2) 0.01036(2) Uani 1 1 d . . . . .
B1 B 0.94057(9) 0.20156(14) 0.58929(8) 0.0171(3) Uani 1 1 d . . . . .
N1 N 0.65997(6) 0.01822(10) 0.62563(6) 0.0157(2) Uani 1 1 d . . . . .
C1 C 0.65092(8) 0.14021(12) 0.62089(7) 0.0154(2) Uani 1 1 d . . . . .
N2 N 0.58725(7) 0.15395(10) 0.58704(6) 0.0157(2) Uani 1 1 d . . . . .
B2 B 0.54921(9) 0.27424(14) 0.56300(8) 0.0158(3) Uani 1 1 d . . . . .
C2 C 0.81716(7) 0.11046(12) 0.62491(7) 0.0148(2) Uani 1 1 d . . . . .
N3 N 0.78937(7) -0.00372(10) 0.62370(6) 0.0167(2) Uani 1 1 d . . . . .
B3 B 0.85735(9) 0.07865(14) 0.80957(8) 0.0169(3) Uani 1 1 d . . . . .
C3 C 0.84092(7) 0.37265(12) 0.59704(6) 0.0152(2) Uani 1 1 d . . . . .
N4 N 0.87926(7) 0.10224(11) 0.59577(6) 0.0165(2) Uani 1 1 d . . . . .
B4 B 0.64521(8) 0.61134(14) 0.73004(8) 0.0165(3) Uani 1 1 d . . . . .
C4 C 0.67412(7) 0.39402(12) 0.58003(6) 0.0147(2) Uani 1 1 d . . . . .
N5 N 0.83099(7) 0.48113(11) 0.56893(6) 0.0162(2) Uani 1 1 d . . . . .
C5 C 0.63478(7) 0.37662(12) 0.73625(6) 0.0150(2) Uani 1 1 d . . . . .
C6 C 0.72501(7) 0.14420(12) 0.76748(7) 0.0150(2) Uani 1 1 d . . . . .
N6 N 0.90105(7) 0.32591(11) 0.57422(6) 0.0161(2) Uani 1 1 d . . . . .
C7 C 0.86468(8) 0.28848(11) 0.75596(7) 0.0149(2) Uani 1 1 d . . . . .
N7 N 0.70133(7) 0.49067(11) 0.55109(6) 0.0163(2) Uani 1 1 d . . . . .
N8 N 0.61176(7) 0.36522(10) 0.54717(6) 0.0153(2) Uani 1 1 d . . . . .
C8 C 0.77516(7) 0.51579(12) 0.71756(7) 0.0152(2) Uani 1 1 d . . . . .
N9 N 0.59125(7) 0.30164(11) 0.76597(6) 0.0172(2) Uani 1 1 d . . . . .
C9 C 0.55731(8) 0.04259(13) 0.57305(8) 0.0212(3) Uani 1 1 d . . . . .
H9 H 0.512285 0.028733 0.550736 0.025 Uiso 1 1 calc R U . . .
C00Q C 0.76636(8) 0.55454(12) 0.57275(7) 0.0179(3) Uani 1 1 d . . . . .
H00A H 0.761892 0.578485 0.614778 0.022 Uiso 1 1 calc R U . . .
H00B H 0.771255 0.628243 0.548858 0.022 Uiso 1 1 calc R U . . .
C00T C 0.91029(7) 0.48657(12) 0.72456(7) 0.0164(3) Uani 1 1 d . . . . .
H00C H 0.953690 0.536933 0.734769 0.020 Uiso 1 1 calc R U . . .
H00D H 0.912619 0.458945 0.682848 0.020 Uiso 1 1 calc R U . . .
C00X C 0.59049(8) 0.17288(13) 0.75756(7) 0.0181(3) Uani 1 1 d . . . . .
H00E H 0.547710 0.138432 0.775820 0.022 Uiso 1 1 calc R U . . .
H00F H 0.585837 0.154552 0.714334 0.022 Uiso 1 1 calc R U . . .
C10 C 0.60277(8) -0.04280(13) 0.59639(7) 0.0199(3) Uani 1 1 d . . . . .
H10 H 0.596686 -0.127113 0.593345 0.024 Uiso 1 1 calc R U . . .
N10 N 0.61840(6) 0.48793(11) 0.75601(6) 0.0165(2) Uani 1 1 d . . . . .
C11 C 0.88951(9) -0.01524(13) 0.57802(8) 0.0227(3) Uani 1 1 d . . . . .
H11 H 0.929082 -0.043962 0.557028 0.027 Uiso 1 1 calc R U . . .
N11 N 0.65648(7) 0.11847(11) 0.78429(6) 0.0174(2) Uani 1 1 d . . . . .
C12 C 0.83355(9) -0.08176(13) 0.59573(8) 0.0236(3) Uani 1 1 d . . . . .
H12 H 0.826282 -0.165312 0.590014 0.028 Uiso 1 1 calc R U . . .
N12 N 0.77072(7) 0.08512(11) 0.80742(6) 0.0176(2) Uani 1 1 d . . . . .
C013 C 0.72492(7) -0.03821(12) 0.65303(7) 0.0166(2) Uani 1 1 d . . . . .
H01A H 0.730949 -0.015121 0.695651 0.020 Uiso 1 1 calc R U . . .
H01B H 0.719203 -0.126302 0.650973 0.020 Uiso 1 1 calc R U . . .
N13 N 0.91145(6) 0.38358(10) 0.76404(6) 0.0155(2) Uani 1 1 d . . . . .
C13 C 0.92771(9) 0.40559(15) 0.53384(8) 0.0242(3) Uani 1 1 d . . . . .
H13 H 0.969892 0.393934 0.512405 0.029 Uiso 1 1 calc R U . . .
C14 C 0.88386(8) 0.50253(14) 0.52998(8) 0.0223(3) Uani 1 1 d . . . . .
H14 H 0.888552 0.571084 0.505499 0.027 Uiso 1 1 calc R U . . .
N14 N 0.88589(7) 0.21143(10) 0.80069(6) 0.0161(2) Uani 1 1 d . . . . .
C15 C 0.60098(9) 0.44395(14) 0.49963(7) 0.0223(3) Uani 1 1 d . . . . .
H15 H 0.561035 0.442675 0.470434 0.027 Uiso 1 1 calc R U . . .
N15 N 0.84492(6) 0.55750(10) 0.72936(6) 0.0157(2) Uani 1 1 d . . . . .
C17 C 0.56604(8) 0.48004(14) 0.79750(8) 0.0227(3) Uani 1 1 d . . . . .
H17 H 0.545857 0.545375 0.817847 0.027 Uiso 1 1 calc R U . . .
C16 C 0.65673(8) 0.52263(14) 0.50182(8) 0.0222(3) Uani 1 1 d . . . . .
H16 H 0.663780 0.586686 0.474988 0.027 Uiso 1 1 calc R U . . .
N16 N 0.73187(6) 0.60710(10) 0.73352(6) 0.0155(2) Uani 1 1 d . . . . .
C18 C 0.54874(9) 0.36333(15) 0.80392(8) 0.0237(3) Uani 1 1 d . . . . .
H18 H 0.514523 0.330623 0.829236 0.028 Uiso 1 1 calc R U . . .
C19 C 0.73043(9) 0.02295(16) 0.84690(9) 0.0293(4) Uani 1 1 d . . . . .
H19 H 0.749833 -0.026435 0.878589 0.035 Uiso 1 1 calc R U . . .
C20 C 0.65899(9) 0.04394(16) 0.83302(9) 0.0287(4) Uani 1 1 d . . . . .
H20 H 0.618865 0.013560 0.852797 0.034 Uiso 1 1 calc R U . . .
C21 C 0.94499(9) 0.25856(14) 0.83487(8) 0.0223(3) Uani 1 1 d . . . . .
H21 H 0.969638 0.221303 0.868540 0.027 Uiso 1 1 calc R U . . .
C22 C 0.96143(8) 0.36639(13) 0.81208(8) 0.0212(3) Uani 1 1 d . . . . .
H22 H 0.999341 0.419200 0.826120 0.025 Uiso 1 1 calc R U . . .
C23 C 0.77443(9) 0.70330(12) 0.75376(8) 0.0212(3) Uani 1 1 d . . . . .
H23 H 0.756788 0.777944 0.767036 0.025 Uiso 1 1 calc R U . . .
C24 C 0.84530(8) 0.67274(12) 0.75137(8) 0.0210(3) Uani 1 1 d . . . . .
H24 H 0.886715 0.720674 0.762524 0.025 Uiso 1 1 calc R U . . .
C25 C 0.98887(10) 0.16566(16) 0.53398(9) 0.0275(3) Uani 1 1 d . . . . .
H25A H 0.957241 0.161872 0.497055 0.041 Uiso 1 1 calc R U . . .
H25B H 1.011661 0.087355 0.541751 0.041 Uiso 1 1 calc R U . . .
H25C H 1.026812 0.226120 0.529816 0.041 Uiso 1 1 calc R U . . .
C26 C 0.99088(9) 0.21184(13) 0.65060(8) 0.0204(3) Uani 1 1 d . . . . .
H26A H 1.019491 0.138306 0.656831 0.031 Uiso 1 1 calc R U . . .
H26B H 0.959921 0.223126 0.683946 0.031 Uiso 1 1 calc R U . . .
H26C H 1.023882 0.280361 0.648380 0.031 Uiso 1 1 calc R U . . .
C27 C 0.49885(9) 0.24321(14) 0.50281(8) 0.0233(3) Uani 1 1 d . . . . .
H27A H 0.477581 0.317213 0.485831 0.035 Uiso 1 1 calc R U . . .
H27B H 0.459730 0.188471 0.512509 0.035 Uiso 1 1 calc R U . . .
H27C H 0.528800 0.205206 0.473730 0.035 Uiso 1 1 calc R U . . .
C28 C 0.50210(8) 0.33338(14) 0.61324(8) 0.0214(3) Uani 1 1 d . . . . .
H28A H 0.481960 0.410054 0.598673 0.032 Uiso 1 1 calc R U . . .
H28B H 0.533500 0.346689 0.649713 0.032 Uiso 1 1 calc R U . . .
H28C H 0.462182 0.279349 0.621893 0.032 Uiso 1 1 calc R U . . .
C29 C 0.88297(8) -0.00641(12) 0.75689(8) 0.0197(3) Uani 1 1 d . . . . .
H29A H 0.882911 0.039560 0.719719 0.030 Uiso 1 1 calc R U . . .
H29B H 0.849305 -0.074167 0.751359 0.030 Uiso 1 1 calc R U . . .
H29C H 0.932269 -0.036310 0.767590 0.030 Uiso 1 1 calc R U . . .
C30 C 0.88789(9) 0.02833(15) 0.87388(8) 0.0261(3) Uani 1 1 d . . . . .
H30A H 0.870003 -0.053401 0.879128 0.039 Uiso 1 1 calc R U . . .
H30B H 0.870906 0.079857 0.905386 0.039 Uiso 1 1 calc R U . . .
H30C H 0.941309 0.027955 0.876169 0.039 Uiso 1 1 calc R U . . .
C31 C 0.61242(8) 0.62520(13) 0.66167(7) 0.0200(3) Uani 1 1 d . . . . .
H31A H 0.635042 0.694202 0.643323 0.030 Uiso 1 1 calc R U . . .
H31B H 0.559580 0.637322 0.660894 0.030 Uiso 1 1 calc R U . . .
H31C H 0.622782 0.552466 0.639354 0.030 Uiso 1 1 calc R U . . .
C32 C 0.62031(9) 0.72170(14) 0.77074(9) 0.0243(3) Uani 1 1 d . . . . .
H32A H 0.635531 0.797466 0.753445 0.036 Uiso 1 1 calc R U . . .
H32B H 0.643172 0.713475 0.811278 0.036 Uiso 1 1 calc R U . . .
H32C H 0.567164 0.720925 0.772145 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 C1 2.6926(14) . ?
Th1 C3 2.6974(14) . ?
Th1 C2 2.6987(14) . ?
Th1 C4 2.6989(14) . ?
Th1 C8 2.6995(14) . ?
Th1 C6 2.7045(14) . ?
Th1 C7 2.7158(15) . ?
Th1 C5 2.7251(14) . ?
B1 N6 1.593(2) . ?
B1 N4 1.595(2) . ?
B1 C26 1.608(3) . ?
B1 C25 1.627(2) . ?
N1 C1 1.3756(17) . ?
N1 C10 1.3804(18) . ?
N1 C013 1.4489(18) . ?
C1 N2 1.3593(18) . ?
N2 C9 1.3871(18) . ?
N2 B2 1.591(2) . ?
B2 N8 1.593(2) . ?
B2 C28 1.611(2) . ?
B2 C27 1.622(2) . ?
C2 N4 1.3584(18) . ?
C2 N3 1.3732(17) . ?
N3 C12 1.3732(19) . ?
N3 C013 1.4477(19) . ?
B3 N14 1.590(2) . ?
B3 N12 1.592(2) . ?
B3 C29 1.613(2) . ?
B3 C30 1.614(2) . ?
C3 N6 1.3552(18) . ?
C3 N5 1.3723(18) . ?
N4 C11 1.3877(18) . ?
B4 N10 1.588(2) . ?
B4 N16 1.591(2) . ?
B4 C31 1.617(2) . ?
B4 C32 1.619(2) . ?
C4 N8 1.3581(18) . ?
C4 N7 1.3722(18) . ?
N5 C14 1.3734(19) . ?
N5 C00Q 1.4511(18) . ?
C5 N10 1.3607(18) . ?
C5 N9 1.3644(18) . ?
C6 N12 1.3567(18) . ?
C6 N11 1.3708(17) . ?
N6 C13 1.384(2) . ?
C7 N14 1.3590(19) . ?
C7 N13 1.3706(17) . ?
N7 C16 1.3776(19) . ?
N7 C00Q 1.4472(19) . ?
N8 C15 1.3865(19) . ?
C8 N16 1.3571(17) . ?
C8 N15 1.3731(17) . ?
N9 C18 1.380(2) . ?
N9 C00X 1.4502(18) . ?
C9 C10 1.350(2) . ?
C9 H9 0.9500 . ?
C00Q H00A 0.9900 . ?
C00Q H00B 0.9900 . ?
C00T N15 1.4499(17) . ?
C00T N13 1.4515(18) . ?
C00T H00C 0.9900 . ?
C00T H00D 0.9900 . ?
C00X N11 1.4492(19) . ?
C00X H00E 0.9900 . ?
C00X H00F 0.9900 . ?
C10 H10 0.9500 . ?
N10 C17 1.3887(19) . ?
C11 C12 1.351(2) . ?
C11 H11 0.9500 . ?
N11 C20 1.373(2) . ?
C12 H12 0.9500 . ?
N12 C19 1.382(2) . ?
C013 H01A 0.9900 . ?
C013 H01B 0.9900 . ?
N13 C22 1.3809(19) . ?
C13 C14 1.349(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
N14 C21 1.3895(19) . ?
C15 C16 1.348(2) . ?
C15 H15 0.9500 . ?
N15 C24 1.3784(18) . ?
C17 C18 1.352(2) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
N16 C23 1.3869(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.349(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.351(2) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.352(2) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
C1 Th1 C3 109.99(5) . . ?
C1 Th1 C2 69.42(4) . . ?
C3 Th1 C2 68.38(4) . . ?
C1 Th1 C4 68.09(4) . . ?
C3 Th1 C4 69.44(4) . . ?
C2 Th1 C4 101.98(4) . . ?
C1 Th1 C8 147.73(4) . . ?
C3 Th1 C8 79.07(4) . . ?
C2 Th1 C8 139.43(4) . . ?
C4 Th1 C8 87.91(4) . . ?
C1 Th1 C6 80.14(4) . . ?
C3 Th1 C6 147.13(4) . . ?
C2 Th1 C6 87.75(4) . . ?
C4 Th1 C6 140.31(4) . . ?
C8 Th1 C6 109.47(4) . . ?
C1 Th1 C7 139.38(4) . . ?
C3 Th1 C7 85.87(5) . . ?
C2 Th1 C7 83.58(4) . . ?
C4 Th1 C7 149.92(4) . . ?
C8 Th1 C7 70.21(4) . . ?
C6 Th1 C7 68.69(4) . . ?
C1 Th1 C5 86.88(4) . . ?
C3 Th1 C5 139.03(4) . . ?
C2 Th1 C5 150.47(4) . . ?
C4 Th1 C5 84.21(4) . . ?
C8 Th1 C5 68.85(4) . . ?
C6 Th1 C5 70.49(4) . . ?
C7 Th1 C5 105.57(4) . . ?
N6 B1 N4 108.11(12) . . ?
N6 B1 C26 110.26(12) . . ?
N4 B1 C26 109.84(13) . . ?
N6 B1 C25 108.54(13) . . ?
N4 B1 C25 108.98(12) . . ?
C26 B1 C25 111.05(14) . . ?
C1 N1 C10 111.59(12) . . ?
C1 N1 C013 123.73(12) . . ?
C10 N1 C013 124.43(12) . . ?
N2 C1 N1 104.48(11) . . ?
N2 C1 Th1 134.23(9) . . ?
N1 C1 Th1 121.27(9) . . ?
C1 N2 C9 109.76(12) . . ?
C1 N2 B2 128.76(12) . . ?
C9 N2 B2 121.45(12) . . ?
N2 B2 N8 107.87(11) . . ?
N2 B2 C28 110.69(13) . . ?
N8 B2 C28 109.07(12) . . ?
N2 B2 C27 108.32(12) . . ?
N8 B2 C27 109.23(13) . . ?
C28 B2 C27 111.57(13) . . ?
N4 C2 N3 104.60(11) . . ?
N4 C2 Th1 133.94(9) . . ?
N3 C2 Th1 121.45(9) . . ?
C12 N3 C2 111.53(12) . . ?
C12 N3 C013 124.66(12) . . ?
C2 N3 C013 123.60(12) . . ?
N14 B3 N12 106.99(11) . . ?
N14 B3 C29 109.96(12) . . ?
N12 B3 C29 110.33(12) . . ?
N14 B3 C30 109.86(13) . . ?
N12 B3 C30 109.14(13) . . ?
C29 B3 C30 110.50(13) . . ?
N6 C3 N5 104.59(12) . . ?
N6 C3 Th1 133.92(10) . . ?
N5 C3 Th1 121.45(9) . . ?
C2 N4 C11 109.75(12) . . ?
C2 N4 B1 128.32(12) . . ?
C11 N4 B1 121.34(12) . . ?
N10 B4 N16 106.95(11) . . ?
N10 B4 C31 109.09(12) . . ?
N16 B4 C31 110.81(12) . . ?
N10 B4 C32 110.22(13) . . ?
N16 B4 C32 108.46(12) . . ?
C31 B4 C32 111.22(12) . . ?
N8 C4 N7 104.53(12) . . ?
N8 C4 Th1 133.48(9) . . ?
N7 C4 Th1 121.81(10) . . ?
C3 N5 C14 111.67(12) . . ?
C3 N5 C00Q 123.69(12) . . ?
C14 N5 C00Q 123.94(12) . . ?
N10 C5 N9 104.49(12) . . ?
N10 C5 Th1 132.11(9) . . ?
N9 C5 Th1 121.78(9) . . ?
N12 C6 N11 104.77(12) . . ?
N12 C6 Th1 133.09(10) . . ?
N11 C6 Th1 122.08(9) . . ?
C3 N6 C13 109.62(13) . . ?
C3 N6 B1 128.88(12) . . ?
C13 N6 B1 121.49(12) . . ?
N14 C7 N13 104.34(12) . . ?
N14 C7 Th1 132.60(9) . . ?
N13 C7 Th1 122.41(9) . . ?
C4 N7 C16 111.59(12) . . ?
C4 N7 C00Q 123.27(12) . . ?
C16 N7 C00Q 125.02(12) . . ?
C4 N8 C15 109.76(12) . . ?
C4 N8 B2 128.68(12) . . ?
C15 N8 B2 120.63(12) . . ?
N16 C8 N15 104.56(11) . . ?
N16 C8 Th1 133.29(9) . . ?
N15 C8 Th1 122.11(9) . . ?
C5 N9 C18 111.88(12) . . ?
C5 N9 C00X 123.05(13) . . ?
C18 N9 C00X 125.06(13) . . ?
C10 C9 N2 108.67(13) . . ?
C10 C9 H9 125.7 . . ?
N2 C9 H9 125.7 . . ?
N7 C00Q N5 111.26(11) . . ?
N7 C00Q H00A 109.4 . . ?
N5 C00Q H00A 109.4 . . ?
N7 C00Q H00B 109.4 . . ?
N5 C00Q H00B 109.4 . . ?
H00A C00Q H00B 108.0 . . ?
N15 C00T N13 111.37(12) . . ?
N15 C00T H00C 109.4 . . ?
N13 C00T H00C 109.4 . . ?
N15 C00T H00D 109.4 . . ?
N13 C00T H00D 109.4 . . ?
H00C C00T H00D 108.0 . . ?
N11 C00X N9 111.20(12) . . ?
N11 C00X H00E 109.4 . . ?
N9 C00X H00E 109.4 . . ?
N11 C00X H00F 109.4 . . ?
N9 C00X H00F 109.4 . . ?
H00E C00X H00F 108.0 . . ?
C9 C10 N1 105.47(12) . . ?
C9 C10 H10 127.3 . . ?
N1 C10 H10 127.3 . . ?
C5 N10 C17 109.91(12) . . ?
C5 N10 B4 126.26(12) . . ?
C17 N10 B4 123.30(12) . . ?
C12 C11 N4 108.28(13) . . ?
C12 C11 H11 125.9 . . ?
N4 C11 H11 125.9 . . ?
C6 N11 C20 111.48(13) . . ?
C6 N11 C00X 123.86(12) . . ?
C20 N11 C00X 124.38(13) . . ?
C11 C12 N3 105.83(13) . . ?
C11 C12 H12 127.1 . . ?
N3 C12 H12 127.1 . . ?
C6 N12 C19 109.48(13) . . ?
C6 N12 B3 127.91(12) . . ?
C19 N12 B3 122.54(13) . . ?
N3 C013 N1 111.57(12) . . ?
N3 C013 H01A 109.3 . . ?
N1 C013 H01A 109.3 . . ?
N3 C013 H01B 109.3 . . ?
N1 C013 H01B 109.3 . . ?
H01A C013 H01B 108.0 . . ?
C7 N13 C22 111.89(12) . . ?
C7 N13 C00T 123.42(12) . . ?
C22 N13 C00T 124.61(12) . . ?
C14 C13 N6 108.69(14) . . ?
C14 C13 H13 125.7 . . ?
N6 C13 H13 125.7 . . ?
C13 C14 N5 105.43(13) . . ?
C13 C14 H14 127.3 . . ?
N5 C14 H14 127.3 . . ?
C7 N14 C21 109.97(12) . . ?
C7 N14 B3 127.08(12) . . ?
C21 N14 B3 122.42(12) . . ?
C16 C15 N8 108.53(14) . . ?
C16 C15 H15 125.7 . . ?
N8 C15 H15 125.7 . . ?
C8 N15 C24 111.54(12) . . ?
C8 N15 C00T 124.65(11) . . ?
C24 N15 C00T 123.59(12) . . ?
C18 C17 N10 108.19(13) . . ?
C18 C17 H17 125.9 . . ?
N10 C17 H17 125.9 . . ?
C15 C16 N7 105.59(13) . . ?
C15 C16 H16 127.2 . . ?
N7 C16 H16 127.2 . . ?
C8 N16 C23 109.91(12) . . ?
C8 N16 B4 127.84(11) . . ?
C23 N16 B4 122.24(11) . . ?
C17 C18 N9 105.52(13) . . ?
C17 C18 H18 127.2 . . ?
N9 C18 H18 127.2 . . ?
C20 C19 N12 108.75(15) . . ?
C20 C19 H19 125.6 . . ?
N12 C19 H19 125.6 . . ?
C19 C20 N11 105.50(14) . . ?
C19 C20 H20 127.2 . . ?
N11 C20 H20 127.2 . . ?
C22 C21 N14 108.38(14) . . ?
C22 C21 H21 125.8 . . ?
N14 C21 H21 125.8 . . ?
C21 C22 N13 105.41(13) . . ?
C21 C22 H22 127.3 . . ?
N13 C22 H22 127.3 . . ?
C24 C23 N16 108.36(12) . . ?
C24 C23 H23 125.8 . . ?
N16 C23 H23 125.8 . . ?
C23 C24 N15 105.61(12) . . ?
C23 C24 H24 127.2 . . ?
N15 C24 H24 127.2 . . ?
B1 C25 H25A 109.5 . . ?
B1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
B1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
B1 C26 H26A 109.5 . . ?
B1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
B1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
B2 C27 H27A 109.5 . . ?
B2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
B2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
B2 C28 H28A 109.5 . . ?
B2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
B2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
B3 C29 H29A 109.5 . . ?
B3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
B3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
B3 C30 H30A 109.5 . . ?
B3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
B3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
B4 C31 H31A 109.5 . . ?
B4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
B4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
B4 C32 H32A 109.5 . . ?
B4 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
B4 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_refine_diff_density_max         0.662
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.103



####################################################################### 
# 
# 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_jd_7_215
_database_code_depnum_ccdc_archive 'CCDC 2047327'
loop_
_audit_author_name
_audit_author_address
'David M. Jenkins'
;University of Tennessee
United States of America
;
_audit_update_record             
;
2020-11-30 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ((BMe2,EtTCH)2)U
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 B4 N16 U [+ pentane/toluene]'
_chemical_formula_sum            'C40 H56 B4 N16 U'
_chemical_formula_weight         1042.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

_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+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   14.118(2)
_cell_length_b                   20.636(3)
_cell_length_c                   37.423(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10903(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5796
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      31.13

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_F_000             4160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.018
_shelx_estimated_absorpt_T_min   0.172
_shelx_estimated_absorpt_T_max   0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_T_max  0.4339
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            19282
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.177
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4166
_reflns_number_gt                3509
_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.
 
 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.
;

_computing_data_collection       'Apex3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          
; 
pentane/toluene solvent SQUEEZED from pore. Very disordered and
could not be modelled with rigid groups.
Q peak near Uranium is due to noise from the heavy metal center.
No other assignments for this peak make reasonable chemical sense.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+36.6887P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4166
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.375000 0.375000 0.375000 0.01824(9) Uani 1 4 d S T P . .
B1 B 0.2588(3) 0.4762(2) 0.46709(11) 0.0217(8) Uani 1 1 d . . . . .
N1 N 0.3560(2) 0.49302(15) 0.44881(8) 0.0216(6) Uani 1 1 d . . . . .
N2 N 0.4731(2) 0.51334(15) 0.41344(8) 0.0226(6) Uani 1 1 d . . . . .
N3 N 0.6052(2) 0.41028(17) 0.41673(8) 0.0244(7) Uani 1 1 d . . . . .
N4 N 0.5478(2) 0.32886(16) 0.44582(8) 0.0226(6) Uani 1 1 d . . . . .
C1 C 0.3945(3) 0.47564(17) 0.41695(9) 0.0221(8) Uani 1 1 d . . . . .
C2 C 0.5282(3) 0.36982(18) 0.41818(9) 0.0231(7) Uani 1 1 d . . . . .
C3 C 0.4131(3) 0.5398(2) 0.46479(10) 0.0279(8) Uani 1 1 d . . . . .
H3 H 0.402274 0.559535 0.487343 0.033 Uiso 1 1 calc R U . . .
C4 C 0.4863(3) 0.55210(18) 0.44284(10) 0.0269(8) Uani 1 1 d . . . . .
H4 H 0.536883 0.581616 0.446848 0.032 Uiso 1 1 calc R U . . .
C5 C 0.5389(3) 0.50620(19) 0.38395(9) 0.0251(8) Uani 1 1 d . . . . .
H5A H 0.560757 0.549711 0.376461 0.030 Uiso 1 1 calc R U . . .
H5B H 0.505129 0.486475 0.363466 0.030 Uiso 1 1 calc R U . . .
C6 C 0.6245(3) 0.4649(2) 0.39284(10) 0.0281(8) Uani 1 1 d . . . . .
H6A H 0.651506 0.447882 0.370299 0.034 Uiso 1 1 calc R U . . .
H6B H 0.673166 0.492852 0.404068 0.034 Uiso 1 1 calc R U . . .
C7 C 0.6716(3) 0.3945(2) 0.44237(10) 0.0279(8) Uani 1 1 d . . . . .
H7 H 0.730386 0.415582 0.446553 0.033 Uiso 1 1 calc R U . . .
C8 C 0.6362(3) 0.3433(2) 0.46024(11) 0.0289(8) Uani 1 1 d . . . . .
H8 H 0.666218 0.321043 0.479330 0.035 Uiso 1 1 calc R U . . .
C9 C 0.1954(3) 0.5417(2) 0.46777(11) 0.0302(9) Uani 1 1 d . . . . .
H9A H 0.136214 0.533430 0.480684 0.045 Uiso 1 1 calc R U . . .
H9B H 0.180913 0.554983 0.443227 0.045 Uiso 1 1 calc R U . . .
H9C H 0.230663 0.576280 0.479812 0.045 Uiso 1 1 calc R U . . .
C10 C 0.2796(3) 0.4482(2) 0.50675(10) 0.0284(8) Uani 1 1 d . . . . .
H10A H 0.219467 0.441705 0.519352 0.043 Uiso 1 1 calc R U . . .
H10B H 0.318650 0.479229 0.520016 0.043 Uiso 1 1 calc R U . . .
H10C H 0.313132 0.406798 0.504876 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 C1 2.618(3) . ?
U1 C1 2.618(3) 4 ?
U1 C1 2.618(3) 2 ?
U1 C1 2.618(3) 3 ?
U1 C2 2.702(4) . ?
U1 C2 2.702(4) 3 ?
U1 C2 2.702(4) 4 ?
U1 C2 2.702(4) 2 ?
B1 N1 1.572(6) . ?
B1 N4 1.601(5) 2 ?
B1 C10 1.620(5) . ?
B1 C9 1.621(6) . ?
N1 C1 1.359(5) . ?
N1 C3 1.392(5) . ?
N2 C1 1.362(5) . ?
N2 C4 1.373(4) . ?
N2 C5 1.450(5) . ?
N3 C2 1.372(5) . ?
N3 C7 1.380(5) . ?
N3 C6 1.465(5) . ?
N4 C2 1.364(5) . ?
N4 C8 1.392(5) . ?
C3 C4 1.345(6) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.516(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.347(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
C1 U1 C1 167.91(18) . 4 ?
C1 U1 C1 106.31(16) . 2 ?
C1 U1 C1 75.01(16) 4 2 ?
C1 U1 C1 75.01(16) . 3 ?
C1 U1 C1 106.31(16) 4 3 ?
C1 U1 C1 167.91(18) 2 3 ?
C1 U1 C2 65.70(12) . . ?
C1 U1 C2 104.06(12) 4 . ?
C1 U1 C2 72.20(12) 2 . ?
C1 U1 C2 118.32(12) 3 . ?
C1 U1 C2 118.32(12) . 3 ?
C1 U1 C2 72.20(12) 4 3 ?
C1 U1 C2 104.06(12) 2 3 ?
C1 U1 C2 65.70(12) 3 3 ?
C2 U1 C2 175.46(16) . 3 ?
C1 U1 C2 104.06(12) . 4 ?
C1 U1 C2 65.70(12) 4 4 ?
C1 U1 C2 118.32(12) 2 4 ?
C1 U1 C2 72.20(12) 3 4 ?
C2 U1 C2 73.65(16) . 4 ?
C2 U1 C2 106.53(16) 3 4 ?
C1 U1 C2 72.20(12) . 2 ?
C1 U1 C2 118.32(12) 4 2 ?
C1 U1 C2 65.70(12) 2 2 ?
C1 U1 C2 104.06(11) 3 2 ?
C2 U1 C2 106.53(16) . 2 ?
C2 U1 C2 73.66(16) 3 2 ?
C2 U1 C2 175.47(16) 4 2 ?
N1 B1 N4 112.1(3) . 2 ?
N1 B1 C10 108.6(3) . . ?
N4 B1 C10 107.0(3) 2 . ?
N1 B1 C9 107.8(3) . . ?
N4 B1 C9 108.9(3) 2 . ?
C10 B1 C9 112.5(3) . . ?
C1 N1 C3 109.1(3) . . ?
C1 N1 B1 132.3(3) . . ?
C3 N1 B1 118.1(3) . . ?
C1 N2 C4 111.5(3) . . ?
C1 N2 C5 122.5(3) . . ?
C4 N2 C5 125.6(3) . . ?
C2 N3 C7 111.6(3) . . ?
C2 N3 C6 129.8(3) . . ?
C7 N3 C6 118.6(4) . . ?
C2 N4 C8 110.0(3) . . ?
C2 N4 B1 135.7(3) . 2 ?
C8 N4 B1 114.0(3) . 2 ?
N1 C1 N2 105.1(3) . . ?
N1 C1 U1 133.9(3) . . ?
N2 C1 U1 118.8(2) . . ?
N4 C2 N3 104.3(3) . . ?
N4 C2 U1 129.8(3) . . ?
N3 C2 U1 125.9(3) . . ?
C4 C3 N1 108.3(3) . . ?
C4 C3 H3 125.8 . . ?
N1 C3 H3 125.8 . . ?
C3 C4 N2 105.9(4) . . ?
C3 C4 H4 127.0 . . ?
N2 C4 H4 127.0 . . ?
N2 C5 C6 113.6(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N3 C6 C5 114.7(3) . . ?
N3 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
N3 C6 H6B 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 N3 106.1(4) . . ?
C8 C7 H7 126.9 . . ?
N3 C7 H7 126.9 . . ?
C7 C8 N4 108.0(4) . . ?
C7 C8 H8 126.0 . . ?
N4 C8 H8 126.0 . . ?
B1 C9 H9A 109.5 . . ?
B1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
B1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
B1 C10 H10A 109.5 . . ?
B1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
B1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 B1 N1 C1 9.1(5) 2 . . . ?
C10 B1 N1 C1 127.1(4) . . . . ?
C9 B1 N1 C1 -110.7(4) . . . . ?
N4 B1 N1 C3 -179.3(3) 2 . . . ?
C10 B1 N1 C3 -61.2(4) . . . . ?
C9 B1 N1 C3 60.9(4) . . . . ?
C3 N1 C1 N2 -1.7(4) . . . . ?
B1 N1 C1 N2 170.5(4) . . . . ?
C3 N1 C1 U1 160.3(3) . . . . ?
B1 N1 C1 U1 -27.5(6) . . . . ?
C4 N2 C1 N1 2.1(4) . . . . ?
C5 N2 C1 N1 175.2(3) . . . . ?
C4 N2 C1 U1 -163.2(3) . . . . ?
C5 N2 C1 U1 9.9(5) . . . . ?
C8 N4 C2 N3 -1.4(4) . . . . ?
B1 N4 C2 N3 172.3(4) 2 . . . ?
C8 N4 C2 U1 179.1(3) . . . . ?
B1 N4 C2 U1 -7.2(6) 2 . . . ?
C7 N3 C2 N4 0.8(4) . . . . ?
C6 N3 C2 N4 -179.1(3) . . . . ?
C7 N3 C2 U1 -179.6(2) . . . . ?
C6 N3 C2 U1 0.4(5) . . . . ?
C1 N1 C3 C4 0.8(5) . . . . ?
B1 N1 C3 C4 -172.7(3) . . . . ?
N1 C3 C4 N2 0.5(5) . . . . ?
C1 N2 C4 C3 -1.7(5) . . . . ?
C5 N2 C4 C3 -174.5(4) . . . . ?
C1 N2 C5 C6 -96.9(4) . . . . ?
C4 N2 C5 C6 75.2(5) . . . . ?
C2 N3 C6 C5 38.1(5) . . . . ?
C7 N3 C6 C5 -141.8(3) . . . . ?
N2 C5 C6 N3 36.0(5) . . . . ?
C2 N3 C7 C8 0.1(4) . . . . ?
C6 N3 C7 C8 -180.0(3) . . . . ?
N3 C7 C8 N4 -1.0(4) . . . . ?
C2 N4 C8 C7 1.6(4) . . . . ?
B1 N4 C8 C7 -173.6(3) 2 . . . ?

_refine_diff_density_max         3.329
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.157




####################################################################### 
# 
# 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_p17064_mono_sqd
_database_code_depnum_ccdc_archive 'CCDC 2047326'
loop_
_audit_author_name
_audit_author_address
'David M. Jenkins'
;University of Tennessee
United States of America
;
_audit_update_record             
;
2020-11-30 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 B4 N16 U'
_chemical_formula_sum            'C36 H48 B4 N16 U'
_chemical_formula_weight         986.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;


# start Validation Reply Form
_vrf_PLAT602_p17064_mono_sqd     
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: Required PLATON SQUEEZE to remove heavily dissordered toluene molecule
;
# end Validation Reply Form

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                   18.5705(2)
_cell_length_b                   11.30970(10)
_cell_length_c                   21.6322(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.3050(10)
_cell_angle_gamma                90
_cell_volume                     4530.52(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    18232
_cell_measurement_theta_min      3.3660
_cell_measurement_theta_max      29.7660

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             1952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.026
_exptl_absorpt_coefficient_mu    3.627
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            80388
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10386
_reflns_number_gt                8885
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+2.1892P] 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         10386
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0553
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.74682(2) 0.28891(2) 0.67490(2) 0.00904(3) Uani 1 1 d . . . . .
N10 N 0.58889(12) 0.1566(2) 0.58653(11) 0.0125(5) Uani 1 1 d . . . . .
N16 N 0.78856(12) -0.0009(2) 0.62509(12) 0.0155(5) Uani 1 1 d . . . . .
N5 N 0.61955(12) 0.4773(2) 0.75497(11) 0.0147(5) Uani 1 1 d . . . . .
N9 N 0.66041(12) 0.0214(2) 0.62586(11) 0.0130(5) Uani 1 1 d . . . . .
N11 N 0.61342(12) 0.3658(2) 0.54621(11) 0.0130(5) Uani 1 1 d . . . . .
N12 N 0.70240(12) 0.4888(2) 0.55104(11) 0.0136(5) Uani 1 1 d . . . . .
N13 N 0.83038(12) 0.4794(2) 0.57234(11) 0.0124(5) Uani 1 1 d . . . . .
N4 N 0.73157(13) 0.59545(19) 0.73198(11) 0.0127(5) Uani 1 1 d . . . . .
N8 N 0.76889(13) 0.0786(2) 0.80540(11) 0.0146(5) Uani 1 1 d . . . . .
N14 N 0.90093(12) 0.3269(2) 0.57947(11) 0.0126(5) Uani 1 1 d . . . . .
N3 N 0.90950(12) 0.3743(2) 0.76306(11) 0.0129(5) Uani 1 1 d . . . . .
N15 N 0.87765(13) 0.1052(2) 0.59726(11) 0.0147(5) Uani 1 1 d . . . . .
N2 N 0.88304(12) 0.2053(2) 0.80109(11) 0.0148(5) Uani 1 1 d . . . . .
N7 N 0.65623(12) 0.1120(2) 0.78072(11) 0.0135(5) Uani 1 1 d . . . . .
C5 C 0.65426(15) 0.1417(2) 0.61914(13) 0.0130(6) Uani 1 1 d . . . . .
N6 N 0.59197(12) 0.2931(2) 0.76336(11) 0.0136(5) Uani 1 1 d . . . . .
C3 C 0.63663(14) 0.3677(3) 0.73448(13) 0.0135(6) Uani 1 1 d . . . . .
C8 C 0.81516(15) 0.1125(2) 0.62695(14) 0.0150(6) Uani 1 1 d . . . . .
C1 C 0.86113(14) 0.2828(2) 0.75554(13) 0.0128(6) Uani 1 1 d . . . . .
C2 C 0.77439(15) 0.5024(2) 0.71812(13) 0.0132(6) Uani 1 1 d . . . . .
C6 C 0.67605(15) 0.3912(2) 0.58030(13) 0.0124(6) Uani 1 1 d . . . . .
C4 C 0.72408(14) 0.1443(2) 0.76678(13) 0.0136(6) Uani 1 1 d . . . . .
C7 C 0.83638(14) 0.3674(2) 0.59678(13) 0.0121(6) Uani 1 1 d . . . . .
C28 C 0.72411(15) -0.0373(3) 0.65370(14) 0.0163(6) Uani 1 1 d . . . . .
H28A H 0.718224 -0.122224 0.649333 0.020 Uiso 1 1 calc R U . . .
H28B H 0.729487 -0.019109 0.697621 0.020 Uiso 1 1 calc R U . . .
C27 C 0.76648(15) 0.5526(2) 0.57354(14) 0.0159(6) Uani 1 1 d . . . . .
H27A H 0.761263 0.578839 0.615650 0.019 Uiso 1 1 calc R U . . .
H27B H 0.771953 0.622013 0.547999 0.019 Uiso 1 1 calc R U . . .
C25 C 0.90874(14) 0.4776(2) 0.72311(14) 0.0136(6) Uani 1 1 d . . . . .
H25A H 0.912051 0.452571 0.680530 0.016 Uiso 1 1 calc R U . . .
H25B H 0.950438 0.526569 0.734837 0.016 Uiso 1 1 calc R U . . .
C26 C 0.59014(15) 0.1668(2) 0.75400(14) 0.0154(6) Uani 1 1 d . . . . .
H26A H 0.584370 0.149890 0.709955 0.019 Uiso 1 1 calc R U . . .
H26B H 0.549039 0.133748 0.773113 0.019 Uiso 1 1 calc R U . . .
C33 C 0.50201(16) 0.3319(3) 0.61133(14) 0.0186(7) Uani 1 1 d . . . . .
H33A H 0.464677 0.276994 0.620077 0.028 Uiso 1 1 calc R U . . .
H33B H 0.531329 0.348599 0.648761 0.028 Uiso 1 1 calc R U . . .
H33C H 0.480538 0.403832 0.595214 0.028 Uiso 1 1 calc R U . . .
C17 C 0.60060(15) -0.0364(3) 0.60029(14) 0.0167(6) Uani 1 1 d . . . . .
H17 H 0.592588 -0.117621 0.599692 0.020 Uiso 1 1 calc R U . . .
C18 C 0.55585(16) 0.0478(3) 0.57626(14) 0.0181(7) Uani 1 1 d . . . . .
H18 H 0.510459 0.035222 0.556155 0.022 Uiso 1 1 calc R U . . .
C34 C 0.50396(17) 0.2434(3) 0.49703(15) 0.0215(7) Uani 1 1 d . . . . .
H34A H 0.466427 0.188820 0.505648 0.032 Uiso 1 1 calc R U . . .
H34B H 0.482781 0.314374 0.479371 0.032 Uiso 1 1 calc R U . . .
H34C H 0.534591 0.208280 0.468286 0.032 Uiso 1 1 calc R U . . .
C9 C 0.94360(17) 0.2492(3) 0.83505(15) 0.0211(7) Uani 1 1 d . . . . .
H9 H 0.968419 0.211818 0.868520 0.025 Uiso 1 1 calc R U . . .
C11 C 0.84344(16) 0.6636(2) 0.74541(14) 0.0172(6) Uani 1 1 d . . . . .
H11 H 0.883533 0.711842 0.753955 0.021 Uiso 1 1 calc R U . . .
C29 C 0.61071(15) 0.6211(3) 0.66014(14) 0.0172(6) Uani 1 1 d . . . . .
H29A H 0.626595 0.695635 0.644900 0.026 Uiso 1 1 calc R U . . .
H29B H 0.625609 0.558626 0.633875 0.026 Uiso 1 1 calc R U . . .
H29C H 0.559018 0.621073 0.660185 0.026 Uiso 1 1 calc R U . . .
B3 B 0.55143(17) 0.2753(3) 0.56094(16) 0.0143(7) Uani 1 1 d . . . . .
C13 C 0.56558(16) 0.4685(3) 0.79594(15) 0.0219(7) Uani 1 1 d . . . . .
H13 H 0.544994 0.531088 0.816186 0.026 Uiso 1 1 calc R U . . .
C12 C 0.77415(16) 0.6934(2) 0.74798(14) 0.0174(6) Uani 1 1 d . . . . .
H12 H 0.757191 0.767417 0.758695 0.021 Uiso 1 1 calc R U . . .
C10 C 0.96030(16) 0.3546(3) 0.81140(14) 0.0188(7) Uani 1 1 d . . . . .
H10 H 0.998316 0.404011 0.824946 0.023 Uiso 1 1 calc R U . . .
C22 C 0.93416(17) 0.4154(3) 0.54758(15) 0.0221(7) Uani 1 1 d . . . . .
H22 H 0.979463 0.410161 0.532150 0.027 Uiso 1 1 calc R U . . .
C14 C 0.54834(16) 0.3537(3) 0.80121(15) 0.0222(7) Uani 1 1 d . . . . .
H14 H 0.513945 0.321750 0.825487 0.027 Uiso 1 1 calc R U . . .
C19 C 0.60197(16) 0.4466(3) 0.49828(14) 0.0198(7) Uani 1 1 d . . . . .
H19 H 0.562617 0.447501 0.469040 0.024 Uiso 1 1 calc R U . . .
C24 C 0.83343(16) -0.0774(3) 0.59678(16) 0.0226(7) Uani 1 1 d . . . . .
H24 H 0.827081 -0.158293 0.590997 0.027 Uiso 1 1 calc R U . . .
C21 C 0.89065(16) 0.5094(3) 0.54261(15) 0.0208(7) Uani 1 1 d . . . . .
H21 H 0.899329 0.580680 0.523037 0.025 Uiso 1 1 calc R U . . .
C23 C 0.88809(16) -0.0112(3) 0.57932(15) 0.0214(7) Uani 1 1 d . . . . .
H23 H 0.926824 -0.038730 0.558523 0.026 Uiso 1 1 calc R U . . .
C35 C 0.99345(15) 0.2038(3) 0.65138(15) 0.0197(7) Uani 1 1 d . . . . .
H35A H 1.030071 0.262271 0.646541 0.030 Uiso 1 1 calc R U . . .
H35B H 0.967437 0.223059 0.686740 0.030 Uiso 1 1 calc R U . . .
H35C H 1.015624 0.127546 0.657340 0.030 Uiso 1 1 calc R U . . .
C31 C 0.88496(16) -0.0146(3) 0.76136(16) 0.0241(8) Uani 1 1 d . . . . .
H31A H 0.867654 -0.093050 0.768407 0.036 Uiso 1 1 calc R U . . .
H31B H 0.868208 0.010771 0.720428 0.036 Uiso 1 1 calc R U . . .
H31C H 0.936793 -0.014402 0.765241 0.036 Uiso 1 1 calc R U . . .
C20 C 0.65716(16) 0.5234(3) 0.50119(14) 0.0199(7) Uani 1 1 d . . . . .
H20 H 0.663496 0.586932 0.474868 0.024 Uiso 1 1 calc R U . . .
C16 C 0.72860(17) 0.0061(3) 0.84123(16) 0.0239(7) Uani 1 1 d . . . . .
H16 H 0.747001 -0.047713 0.870840 0.029 Uiso 1 1 calc R U . . .
B2 B 0.85490(18) 0.0749(3) 0.81207(17) 0.0181(8) Uani 1 1 d . . . . .
C30 C 0.62299(16) 0.7063(3) 0.77529(15) 0.0214(7) Uani 1 1 d . . . . .
H30A H 0.639288 0.780527 0.759952 0.032 Uiso 1 1 calc R U . . .
H30B H 0.571392 0.707695 0.776161 0.032 Uiso 1 1 calc R U . . .
H30C H 0.644632 0.693319 0.816440 0.032 Uiso 1 1 calc R U . . .
C36 C 0.98081(18) 0.1699(3) 0.52885(16) 0.0285(8) Uani 1 1 d . . . . .
H36A H 1.017844 0.227736 0.524077 0.043 Uiso 1 1 calc R U . . .
H36B H 1.002301 0.092956 0.533537 0.043 Uiso 1 1 calc R U . . .
H36C H 0.947249 0.170712 0.492864 0.043 Uiso 1 1 calc R U . . .
B4 B 0.93841(18) 0.2012(3) 0.59010(16) 0.0162(7) Uani 1 1 d . . . . .
B1 B 0.64607(17) 0.6005(3) 0.73026(16) 0.0135(7) Uani 1 1 d . . . . .
C15 C 0.65836(17) 0.0271(3) 0.82578(15) 0.0235(7) Uani 1 1 d . . . . .
H15 H 0.619123 -0.008898 0.842381 0.028 Uiso 1 1 calc R U . . .
C32 C 0.88142(18) 0.0312(3) 0.88134(16) 0.0328(9) Uani 1 1 d . . . . .
H32A H 0.864217 -0.047601 0.887627 0.049 Uiso 1 1 calc R U . . .
H32B H 0.933224 0.031926 0.886290 0.049 Uiso 1 1 calc R U . . .
H32C H 0.862541 0.083392 0.911172 0.049 Uiso 1 1 calc R U . . .
N1 N 0.84323(12) 0.5467(2) 0.72747(11) 0.0125(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 C7 2.614(3) . ?
U1 C6 2.617(3) . ?
U1 C8 2.620(3) . ?
U1 C5 2.621(3) . ?
U1 C2 2.626(3) . ?
U1 C4 2.632(3) . ?
U1 C1 2.645(3) . ?
U1 C3 2.653(3) . ?
N10 C5 1.368(4) . ?
N10 C18 1.386(4) . ?
N10 B3 1.592(4) . ?
N16 C8 1.374(4) . ?
N16 C24 1.376(4) . ?
N16 C28 1.448(4) . ?
N5 C3 1.363(4) . ?
N5 C13 1.390(4) . ?
N5 B1 1.584(4) . ?
N9 C17 1.369(4) . ?
N9 C5 1.373(4) . ?
N9 C28 1.448(4) . ?
N11 C6 1.360(4) . ?
N11 C19 1.387(4) . ?
N11 B3 1.590(4) . ?
N12 C20 1.373(4) . ?
N12 C6 1.380(3) . ?
N12 C27 1.444(4) . ?
N13 C7 1.374(4) . ?
N13 C21 1.375(3) . ?
N13 C27 1.449(3) . ?
N4 C2 1.365(3) . ?
N4 C12 1.390(4) . ?
N4 B1 1.586(4) . ?
N8 C4 1.356(4) . ?
N8 C16 1.386(4) . ?
N8 B2 1.593(4) . ?
N14 C7 1.362(3) . ?
N14 C22 1.387(4) . ?
N14 B4 1.591(4) . ?
N3 C1 1.372(3) . ?
N3 C10 1.373(4) . ?
N3 C25 1.453(4) . ?
N15 C8 1.370(4) . ?
N15 C23 1.391(4) . ?
N15 B4 1.582(4) . ?
N2 C1 1.358(4) . ?
N2 C9 1.388(4) . ?
N2 B2 1.588(4) . ?
N7 C15 1.367(4) . ?
N7 C4 1.367(3) . ?
N7 C26 1.456(4) . ?
N6 C3 1.367(3) . ?
N6 C14 1.377(4) . ?
N6 C26 1.442(4) . ?
C2 N1 1.374(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C25 N1 1.455(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C33 B3 1.609(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C17 C18 1.343(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C34 B3 1.623(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C9 C10 1.344(4) . ?
C9 H9 0.9300 . ?
C11 C12 1.335(4) . ?
C11 N1 1.378(4) . ?
C11 H11 0.9300 . ?
C29 B1 1.624(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C13 C14 1.343(4) . ?
C13 H13 0.9300 . ?
C12 H12 0.9300 . ?
C10 H10 0.9300 . ?
C22 C21 1.335(4) . ?
C22 H22 0.9300 . ?
C14 H14 0.9300 . ?
C19 C20 1.341(4) . ?
C19 H19 0.9300 . ?
C24 C23 1.338(4) . ?
C24 H24 0.9300 . ?
C21 H21 0.9300 . ?
C23 H23 0.9300 . ?
C35 B4 1.612(5) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C31 B2 1.622(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C20 H20 0.9300 . ?
C16 C15 1.343(4) . ?
C16 H16 0.9300 . ?
B2 C32 1.619(5) . ?
C30 B1 1.621(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C36 B4 1.630(4) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C15 H15 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 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
C7 U1 C6 69.57(8) . . ?
C7 U1 C8 69.63(9) . . ?
C6 U1 C8 104.87(9) . . ?
C7 U1 C5 110.20(9) . . ?
C6 U1 C5 69.35(9) . . ?
C8 U1 C5 69.79(9) . . ?
C7 U1 C2 78.54(9) . . ?
C6 U1 C2 86.85(9) . . ?
C8 U1 C2 138.93(9) . . ?
C5 U1 C2 148.38(8) . . ?
C7 U1 C4 147.68(9) . . ?
C6 U1 C4 139.94(8) . . ?
C8 U1 C4 86.32(9) . . ?
C5 U1 C4 79.41(9) . . ?
C2 U1 C4 109.91(9) . . ?
C7 U1 C1 85.24(9) . . ?
C6 U1 C1 149.11(9) . . ?
C8 U1 C1 81.52(9) . . ?
C5 U1 C1 138.85(9) . . ?
C2 U1 C1 70.36(9) . . ?
C4 U1 C1 69.64(9) . . ?
C7 U1 C3 138.73(9) . . ?
C6 U1 C3 82.59(8) . . ?
C8 U1 C3 149.57(9) . . ?
C5 U1 C3 86.20(9) . . ?
C2 U1 C3 69.83(9) . . ?
C4 U1 C3 70.64(9) . . ?
C1 U1 C3 107.37(8) . . ?
C5 N10 C18 109.8(2) . . ?
C5 N10 B3 129.1(2) . . ?
C18 N10 B3 121.1(2) . . ?
C8 N16 C24 111.8(2) . . ?
C8 N16 C28 124.0(2) . . ?
C24 N16 C28 124.0(2) . . ?
C3 N5 C13 109.8(2) . . ?
C3 N5 B1 127.2(2) . . ?
C13 N5 B1 122.4(2) . . ?
C17 N9 C5 111.8(2) . . ?
C17 N9 C28 124.2(2) . . ?
C5 N9 C28 123.9(2) . . ?
C6 N11 C19 110.1(2) . . ?
C6 N11 B3 129.0(2) . . ?
C19 N11 B3 120.1(2) . . ?
C20 N12 C6 111.8(2) . . ?
C20 N12 C27 124.2(2) . . ?
C6 N12 C27 123.8(2) . . ?
C7 N13 C21 111.3(2) . . ?
C7 N13 C27 124.3(2) . . ?
C21 N13 C27 124.3(2) . . ?
C2 N4 C12 109.8(2) . . ?
C2 N4 B1 128.4(2) . . ?
C12 N4 B1 121.8(2) . . ?
C4 N8 C16 109.7(2) . . ?
C4 N8 B2 129.4(2) . . ?
C16 N8 B2 120.9(2) . . ?
C7 N14 C22 109.1(2) . . ?
C7 N14 B4 130.2(2) . . ?
C22 N14 B4 120.7(2) . . ?
C1 N3 C10 112.0(2) . . ?
C1 N3 C25 124.0(2) . . ?
C10 N3 C25 124.0(2) . . ?
C8 N15 C23 109.2(2) . . ?
C8 N15 B4 129.8(2) . . ?
C23 N15 B4 120.5(2) . . ?
C1 N2 C9 109.9(2) . . ?
C1 N2 B2 128.6(2) . . ?
C9 N2 B2 121.0(2) . . ?
C15 N7 C4 111.6(2) . . ?
C15 N7 C26 124.1(2) . . ?
C4 N7 C26 124.2(2) . . ?
N10 C5 N9 103.9(2) . . ?
N10 C5 U1 133.26(19) . . ?
N9 C5 U1 122.31(19) . . ?
C3 N6 C14 111.6(2) . . ?
C3 N6 C26 123.8(2) . . ?
C14 N6 C26 124.6(2) . . ?
N5 C3 N6 104.4(2) . . ?
N5 C3 U1 132.11(19) . . ?
N6 C3 U1 122.10(19) . . ?
N15 C8 N16 104.2(2) . . ?
N15 C8 U1 133.14(19) . . ?
N16 C8 U1 122.60(19) . . ?
N2 C1 N3 104.1(2) . . ?
N2 C1 U1 132.62(19) . . ?
N3 C1 U1 122.97(19) . . ?
N4 C2 N1 103.8(2) . . ?
N4 C2 U1 133.27(19) . . ?
N1 C2 U1 122.82(18) . . ?
N11 C6 N12 103.8(2) . . ?
N11 C6 U1 133.58(19) . . ?
N12 C6 U1 122.51(19) . . ?
N8 C4 N7 104.5(2) . . ?
N8 C4 U1 132.84(19) . . ?
N7 C4 U1 122.37(19) . . ?
N14 C7 N13 104.6(2) . . ?
N14 C7 U1 132.8(2) . . ?
N13 C7 U1 121.65(18) . . ?
N9 C28 N16 111.6(2) . . ?
N9 C28 H28A 109.3 . . ?
N16 C28 H28A 109.3 . . ?
N9 C28 H28B 109.3 . . ?
N16 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
N12 C27 N13 111.3(2) . . ?
N12 C27 H27A 109.4 . . ?
N13 C27 H27A 109.4 . . ?
N12 C27 H27B 109.4 . . ?
N13 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N3 C25 N1 111.4(2) . . ?
N3 C25 H25A 109.4 . . ?
N1 C25 H25A 109.4 . . ?
N3 C25 H25B 109.4 . . ?
N1 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
N6 C26 N7 110.9(2) . . ?
N6 C26 H26A 109.5 . . ?
N7 C26 H26A 109.5 . . ?
N6 C26 H26B 109.5 . . ?
N7 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
B3 C33 H33A 109.5 . . ?
B3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
B3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C18 C17 N9 106.1(3) . . ?
C18 C17 H17 126.9 . . ?
N9 C17 H17 126.9 . . ?
C17 C18 N10 108.3(3) . . ?
C17 C18 H18 125.8 . . ?
N10 C18 H18 125.8 . . ?
B3 C34 H34A 109.5 . . ?
B3 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
B3 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C10 C9 N2 108.5(3) . . ?
C10 C9 H9 125.8 . . ?
N2 C9 H9 125.8 . . ?
C12 C11 N1 105.7(2) . . ?
C12 C11 H11 127.1 . . ?
N1 C11 H11 127.1 . . ?
B1 C29 H29A 109.5 . . ?
B1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
B1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N11 B3 N10 108.0(2) . . ?
N11 B3 C33 109.8(2) . . ?
N10 B3 C33 110.9(2) . . ?
N11 B3 C34 109.1(2) . . ?
N10 B3 C34 107.7(2) . . ?
C33 B3 C34 111.4(2) . . ?
C14 C13 N5 108.2(3) . . ?
C14 C13 H13 125.9 . . ?
N5 C13 H13 125.9 . . ?
C11 C12 N4 108.7(3) . . ?
C11 C12 H12 125.6 . . ?
N4 C12 H12 125.6 . . ?
C9 C10 N3 105.6(3) . . ?
C9 C10 H10 127.2 . . ?
N3 C10 H10 127.2 . . ?
C21 C22 N14 109.0(3) . . ?
C21 C22 H22 125.5 . . ?
N14 C22 H22 125.5 . . ?
C13 C14 N6 106.0(3) . . ?
C13 C14 H14 127.0 . . ?
N6 C14 H14 127.0 . . ?
C20 C19 N11 108.5(3) . . ?
C20 C19 H19 125.7 . . ?
N11 C19 H19 125.7 . . ?
C23 C24 N16 105.8(3) . . ?
C23 C24 H24 127.1 . . ?
N16 C24 H24 127.1 . . ?
C22 C21 N13 105.9(3) . . ?
C22 C21 H21 127.0 . . ?
N13 C21 H21 127.0 . . ?
C24 C23 N15 109.0(3) . . ?
C24 C23 H23 125.5 . . ?
N15 C23 H23 125.5 . . ?
B4 C35 H35A 109.5 . . ?
B4 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
B4 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
B2 C31 H31A 109.5 . . ?
B2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
B2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C19 C20 N12 105.8(3) . . ?
C19 C20 H20 127.1 . . ?
N12 C20 H20 127.1 . . ?
C15 C16 N8 108.2(3) . . ?
C15 C16 H16 125.9 . . ?
N8 C16 H16 125.9 . . ?
N2 B2 N8 107.5(2) . . ?
N2 B2 C32 110.0(3) . . ?
N8 B2 C32 109.0(3) . . ?
N2 B2 C31 110.1(2) . . ?
N8 B2 C31 110.4(3) . . ?
C32 B2 C31 109.8(3) . . ?
B1 C30 H30A 109.5 . . ?
B1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
B1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
B4 C36 H36A 109.5 . . ?
B4 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
B4 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N15 B4 N14 108.6(2) . . ?
N15 B4 C35 110.2(3) . . ?
N14 B4 C35 110.2(2) . . ?
N15 B4 C36 108.8(3) . . ?
N14 B4 C36 108.0(3) . . ?
C35 B4 C36 110.9(3) . . ?
N5 B1 N4 107.2(2) . . ?
N5 B1 C30 110.1(2) . . ?
N4 B1 C30 108.8(2) . . ?
N5 B1 C29 109.1(2) . . ?
N4 B1 C29 111.2(2) . . ?
C30 B1 C29 110.4(2) . . ?
C16 C15 N7 106.1(3) . . ?
C16 C15 H15 127.0 . . ?
N7 C15 H15 127.0 . . ?
B2 C32 H32A 109.5 . . ?
B2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
B2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 N1 C11 112.0(2) . . ?
C2 N1 C25 124.6(2) . . ?
C11 N1 C25 123.3(2) . . ?

_refine_diff_density_max         0.675
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.098


