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

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

data_X224
_database_code_depnum_ccdc_archive 'CCDC 981990'
_audit_update_record             
;
2014-01-17 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            (NCN)Th(CH2SiMe3)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H72 N2 Si3 Th'
_chemical_formula_weight         933.33

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'
Si Si 0.0817 0.0704 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   11.6853(6)
_cell_length_b                   14.4818(7)
_cell_length_c                   16.2987(8)
_cell_angle_alpha                99.2960(10)
_cell_angle_beta                 91.7080(10)
_cell_angle_gamma                92.4610(10)
_cell_volume                     2717.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   0.269
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.834
_shelx_estimated_absorpt_T_min   0.538
_shelx_estimated_absorpt_T_max   0.727
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13466
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.747
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             9336
_reflns_number_gt                8006
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2013)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2013)'

_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)+(0.0507P)²]
 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         9336
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1009
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
C1 C 0.2827(6) 0.1278(5) 0.0973(3) 0.0433(15) Uani 1 1 d . . . . .
H1A H 0.3000 0.0607 0.0874 0.052 Uiso 1 1 calc R U . . .
H1B H 0.2127 0.1340 0.0633 0.052 Uiso 1 1 calc R U . . .
C2 C 0.1991(5) 0.0122(4) 0.2839(4) 0.0371(14) Uani 1 1 d . . . . .
H2A H 0.1997 0.0217 0.3454 0.045 Uiso 1 1 calc R U . . .
H2B H 0.1199 -0.0090 0.2642 0.045 Uiso 1 1 calc R U . . .
C3 C 0.4054(5) 0.2149(4) 0.3349(4) 0.0387(14) Uani 1 1 d . . . . .
H3A H 0.4641 0.1716 0.3119 0.046 Uiso 1 1 calc R U . . .
H3B H 0.4302 0.2771 0.3220 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5400(6) 0.1504(7) 0.0903(6) 0.095(3) Uani 1 1 d . . . . .
H4A H 0.6030 0.1850 0.0685 0.143 Uiso 1 1 calc R U . . .
H4B H 0.5442 0.0833 0.0693 0.143 Uiso 1 1 calc R U . . .
H4C H 0.5463 0.1610 0.1512 0.143 Uiso 1 1 calc R U . . .
C5 C 0.3947(8) 0.3181(6) 0.0995(6) 0.095(3) Uani 1 1 d . . . . .
H5A H 0.4574 0.3533 0.0780 0.142 Uiso 1 1 calc R U . . .
H5B H 0.4027 0.3263 0.1603 0.142 Uiso 1 1 calc R U . . .
H5C H 0.3212 0.3414 0.0834 0.142 Uiso 1 1 calc R U . . .
C6 C 0.3957(8) 0.1794(6) -0.0592(4) 0.080(3) Uani 1 1 d . . . . .
H6A H 0.4605 0.2156 -0.0769 0.120 Uiso 1 1 calc R U . . .
H6B H 0.3237 0.2027 -0.0783 0.120 Uiso 1 1 calc R U . . .
H6C H 0.4004 0.1132 -0.0833 0.120 Uiso 1 1 calc R U . . .
C7 C 0.2472(7) -0.1502(5) 0.1442(5) 0.069(2) Uani 1 1 d . . . . .
H7A H 0.2984 -0.2015 0.1285 0.103 Uiso 1 1 calc R U . . .
H7B H 0.2525 -0.1066 0.1042 0.103 Uiso 1 1 calc R U . . .
H7C H 0.1682 -0.1756 0.1442 0.103 Uiso 1 1 calc R U . . .
C8 C 0.2887(8) -0.1729(5) 0.3245(5) 0.076(3) Uani 1 1 d . . . . .
H8A H 0.3393 -0.2235 0.3051 0.113 Uiso 1 1 calc R U . . .
H8B H 0.2104 -0.1990 0.3272 0.113 Uiso 1 1 calc R U . . .
H8C H 0.3155 -0.1414 0.3800 0.113 Uiso 1 1 calc R U . . .
C9 C 0.4441(6) -0.0428(5) 0.2473(5) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.4921 -0.0957 0.2297 0.092 Uiso 1 1 calc R U . . .
H9B H 0.4705 -0.0109 0.3027 0.092 Uiso 1 1 calc R U . . .
H9C H 0.4496 0.0012 0.2076 0.092 Uiso 1 1 calc R U . . .
C10 C 0.4107(7) 0.1106(5) 0.4836(4) 0.070(2) Uani 1 1 d . . . . .
H10A H 0.3352 0.0817 0.4647 0.105 Uiso 1 1 calc R U . . .
H10B H 0.4176 0.1189 0.5444 0.105 Uiso 1 1 calc R U . . .
H10C H 0.4705 0.0701 0.4597 0.105 Uiso 1 1 calc R U . . .
C11 C 0.3190(8) 0.3057(6) 0.5035(5) 0.081(3) Uani 1 1 d . . . . .
H11A H 0.2415 0.2811 0.4848 0.121 Uiso 1 1 calc R U . . .
H11B H 0.3310 0.3688 0.4899 0.121 Uiso 1 1 calc R U . . .
H11C H 0.3282 0.3083 0.5638 0.121 Uiso 1 1 calc R U . . .
C12 C 0.5741(7) 0.2768(7) 0.4860(5) 0.087(3) Uani 1 1 d . . . . .
H12A H 0.5818 0.2816 0.5466 0.130 Uiso 1 1 calc R U . . .
H12B H 0.5850 0.3393 0.4708 0.130 Uiso 1 1 calc R U . . .
H12C H 0.6321 0.2360 0.4599 0.130 Uiso 1 1 calc R U . . .
C13 C 0.1337(5) 0.3954(4) 0.2193(3) 0.0341(14) Uani 1 1 d . . . . .
C14 C 0.2097(6) 0.4673(4) 0.2607(4) 0.0406(15) Uani 1 1 d . . . . .
C15 C 0.2772(5) 0.4580(4) 0.3394(4) 0.0390(15) Uani 1 1 d . . . . .
H15 H 0.2661 0.3917 0.3487 0.047 Uiso 1 1 calc R U . . .
C16 C 0.2320(6) 0.5219(6) 0.4157(4) 0.067(2) Uani 1 1 d . . . . .
H16A H 0.2773 0.5146 0.4656 0.100 Uiso 1 1 calc R U . . .
H16B H 0.1514 0.5042 0.4227 0.100 Uiso 1 1 calc R U . . .
H16C H 0.2387 0.5873 0.4071 0.100 Uiso 1 1 calc R U . . .
C17 C 0.4067(5) 0.4793(5) 0.3345(5) 0.0532(18) Uani 1 1 d . . . . .
H17A H 0.4455 0.4707 0.3867 0.080 Uiso 1 1 calc R U . . .
H17B H 0.4201 0.5441 0.3255 0.080 Uiso 1 1 calc R U . . .
H17C H 0.4368 0.4365 0.2882 0.080 Uiso 1 1 calc R U . . .
C18 C 0.2243(6) 0.5497(4) 0.2279(5) 0.0541(19) Uani 1 1 d . . . . .
H18 H 0.2748 0.5988 0.2555 0.065 Uiso 1 1 calc R U . . .
C19 C 0.1655(7) 0.5609(5) 0.1547(5) 0.069(2) Uani 1 1 d . . . . .
H19 H 0.1760 0.6176 0.1331 0.082 Uiso 1 1 calc R U . . .
C20 C 0.0914(6) 0.4895(5) 0.1133(4) 0.0564(19) Uani 1 1 d . . . . .
H20 H 0.0515 0.4974 0.0634 0.068 Uiso 1 1 calc R U . . .
C21 C 0.0761(5) 0.4066(4) 0.1451(4) 0.0345(13) Uani 1 1 d . . . . .
C22 C -0.0038(5) 0.3300(4) 0.0939(4) 0.0404(15) Uani 1 1 d . . . . .
H22 H -0.0088 0.2755 0.1245 0.048 Uiso 1 1 calc R U . . .
C23 C -0.1248(6) 0.3616(5) 0.0812(4) 0.0536(18) Uani 1 1 d . . . . .
H23A H -0.1570 0.3830 0.1355 0.080 Uiso 1 1 calc R U . . .
H23B H -0.1728 0.3091 0.0511 0.080 Uiso 1 1 calc R U . . .
H23C H -0.1224 0.4131 0.0489 0.080 Uiso 1 1 calc R U . . .
C24 C 0.0450(7) 0.2962(5) 0.0085(4) 0.066(2) Uani 1 1 d . . . . .
H24A H 0.1226 0.2749 0.0159 0.099 Uiso 1 1 calc R U . . .
H24B H 0.0479 0.3479 -0.0236 0.099 Uiso 1 1 calc R U . . .
H24C H -0.0041 0.2443 -0.0214 0.099 Uiso 1 1 calc R U . . .
C26 C 0.0226(5) 0.2718(4) 0.2734(3) 0.0276(12) Uani 1 1 d . . . . .
C27 C -0.0798(5) 0.3284(4) 0.2924(3) 0.0309(13) Uani 1 1 d . . . . .
C28 C -0.0664(5) 0.4212(4) 0.3305(4) 0.0400(15) Uani 1 1 d . . . . .
H28 H 0.0087 0.4479 0.3447 0.048 Uiso 1 1 calc R U . . .
C29 C -0.1590(7) 0.4758(5) 0.3483(5) 0.058(2) Uani 1 1 d . . . . .
H29 H -0.1474 0.5391 0.3747 0.069 Uiso 1 1 calc R U . . .
C30 C -0.2692(7) 0.4381(5) 0.3277(5) 0.065(2) Uani 1 1 d . . . . .
H30 H -0.3333 0.4757 0.3393 0.078 Uiso 1 1 calc R U . . .
C31 C -0.2853(5) 0.3461(5) 0.2906(4) 0.0477(17) Uani 1 1 d . . . . .
H31 H -0.3607 0.3199 0.2766 0.057 Uiso 1 1 calc R U . . .
C32 C -0.1910(6) 0.2912(4) 0.2734(4) 0.0428(15) Uani 1 1 d . . . . .
H32 H -0.2029 0.2274 0.2483 0.051 Uiso 1 1 calc R U . . .
C33 C -0.0618(4) 0.1247(4) 0.3051(3) 0.0297(12) Uani 1 1 d . . . . .
C34 C -0.0876(5) 0.1340(4) 0.3895(4) 0.0342(13) Uani 1 1 d . . . . .
C35 C -0.0140(5) 0.1971(4) 0.4574(4) 0.0423(15) Uani 1 1 d . . . . .
H35 H 0.0492 0.2281 0.4301 0.051 Uiso 1 1 calc R U . . .
C36 C -0.0865(7) 0.2742(5) 0.5042(4) 0.068(2) Uani 1 1 d . . . . .
H36A H -0.0383 0.3141 0.5473 0.102 Uiso 1 1 calc R U . . .
H36B H -0.1502 0.2450 0.5302 0.102 Uiso 1 1 calc R U . . .
H36C H -0.1169 0.3124 0.4649 0.102 Uiso 1 1 calc R U . . .
C37 C 0.0399(7) 0.1388(6) 0.5177(5) 0.067(2) Uani 1 1 d . . . . .
H37A H 0.0869 0.1801 0.5605 0.101 Uiso 1 1 calc R U . . .
H37B H 0.0880 0.0924 0.4870 0.101 Uiso 1 1 calc R U . . .
H37C H -0.0209 0.1067 0.5441 0.101 Uiso 1 1 calc R U . . .
C38 C -0.1805(6) 0.0769(5) 0.4089(4) 0.0505(18) Uani 1 1 d . . . . .
H38 H -0.2020 0.0818 0.4651 0.061 Uiso 1 1 calc R U . . .
C39 C -0.2405(7) 0.0151(5) 0.3497(4) 0.057(2) Uani 1 1 d . . . . .
H39 H -0.3042 -0.0210 0.3644 0.069 Uiso 1 1 calc R U . . .
C40 C -0.2081(6) 0.0054(5) 0.2687(4) 0.0523(18) Uani 1 1 d . . . . .
H40 H -0.2501 -0.0383 0.2278 0.063 Uiso 1 1 calc R U . . .
C41 C -0.1161(5) 0.0574(4) 0.2443(4) 0.0382(14) Uani 1 1 d . . . . .
C42 C -0.0794(6) 0.0415(5) 0.1541(4) 0.0479(17) Uani 1 1 d . . . . .
H42 H -0.0041 0.0764 0.1519 0.058 Uiso 1 1 calc R U . . .
C43 C -0.1665(7) 0.0805(5) 0.0975(4) 0.062(2) Uani 1 1 d . . . . .
H43A H -0.1415 0.0693 0.0400 0.093 Uiso 1 1 calc R U . . .
H43B H -0.1715 0.1480 0.1160 0.093 Uiso 1 1 calc R U . . .
H43C H -0.2419 0.0491 0.1004 0.093 Uiso 1 1 calc R U . . .
C44 C -0.0639(7) -0.0607(5) 0.1207(5) 0.070(2) Uani 1 1 d . . . . .
H44A H -0.0412 -0.0672 0.0627 0.106 Uiso 1 1 calc R U . . .
H44B H -0.1363 -0.0967 0.1236 0.106 Uiso 1 1 calc R U . . .
H44C H -0.0042 -0.0845 0.1542 0.106 Uiso 1 1 calc R U . . .
N1 N 0.1215(4) 0.3088(3) 0.2509(3) 0.0272(10) Uani 1 1 d . . . . .
N2 N 0.0308(3) 0.1815(3) 0.2792(3) 0.0252(10) Uani 1 1 d . . . . .
Si1 Si 0.40008(16) 0.19186(14) 0.05566(11) 0.0465(5) Uani 1 1 d . . . . .
Si2 Si 0.29066(16) -0.08684(12) 0.25079(11) 0.0407(4) Uani 1 1 d . . . . .
Si3 Si 0.42768(16) 0.22630(13) 0.44931(11) 0.0434(4) Uani 1 1 d . . . . .
Th1 Th 0.23442(2) 0.16793(2) 0.24424(2) 0.02747(8) 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 Si1 1.831(6) . ?
C1 Th1 2.460(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 Si2 1.846(6) . ?
C2 Th1 2.466(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 Si3 1.855(6) . ?
C3 Th1 2.453(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 Si1 1.869(9) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Si1 1.857(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si1 1.850(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Si2 1.873(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 Si2 1.866(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 Si2 1.883(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 Si3 1.854(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si3 1.891(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 Si3 1.874(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C21 1.402(8) . ?
C13 C14 1.410(8) . ?
C13 N1 1.434(6) . ?
C14 C18 1.391(8) . ?
C14 C15 1.512(9) . ?
C15 C17 1.538(8) . ?
C15 C16 1.546(8) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.393(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.389(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.539(8) . ?
C22 C23 1.524(9) . ?
C22 C24 1.534(9) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 N2 1.333(7) . ?
C26 N1 1.339(6) . ?
C26 C27 1.491(8) . ?
C26 Th1 2.962(6) . ?
C27 C28 1.387(8) . ?
C27 C32 1.392(8) . ?
C28 C29 1.378(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.374(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.396(9) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C41 1.390(8) . ?
C33 C34 1.403(8) . ?
C33 N2 1.446(6) . ?
C34 C38 1.411(8) . ?
C34 C35 1.532(8) . ?
C35 C37 1.533(9) . ?
C35 C36 1.547(9) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.359(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.372(9) . ?
C39 H39 0.9500 . ?
C40 C41 1.391(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.527(8) . ?
C42 C44 1.513(9) . ?
C42 C43 1.539(9) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N1 Th1 2.466(4) . ?
N2 Th1 2.472(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1 C1 Th1 120.4(3) . . ?
Si1 C1 H1A 107.2 . . ?
Th1 C1 H1A 107.2 . . ?
Si1 C1 H1B 107.2 . . ?
Th1 C1 H1B 107.2 . . ?
H1A C1 H1B 106.9 . . ?
Si2 C2 Th1 122.6(3) . . ?
Si2 C2 H2A 106.7 . . ?
Th1 C2 H2A 106.7 . . ?
Si2 C2 H2B 106.7 . . ?
Th1 C2 H2B 106.7 . . ?
H2A C2 H2B 106.6 . . ?
Si3 C3 Th1 131.2(3) . . ?
Si3 C3 H3A 104.5 . . ?
Th1 C3 H3A 104.5 . . ?
Si3 C3 H3B 104.5 . . ?
Th1 C3 H3B 104.5 . . ?
H3A C3 H3B 105.6 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C13 C14 120.1(5) . . ?
C21 C13 N1 120.5(5) . . ?
C14 C13 N1 119.3(5) . . ?
C18 C14 C13 118.9(6) . . ?
C18 C14 C15 118.6(6) . . ?
C13 C14 C15 122.5(5) . . ?
C14 C15 C17 113.5(5) . . ?
C14 C15 C16 111.2(5) . . ?
C17 C15 C16 108.9(5) . . ?
C14 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C19 120.6(6) . . ?
C14 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 120.5(6) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 119.6(7) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C13 120.2(6) . . ?
C20 C21 C22 116.4(5) . . ?
C13 C21 C22 123.4(5) . . ?
C23 C22 C24 108.8(5) . . ?
C23 C22 C21 113.1(5) . . ?
C24 C22 C21 110.9(5) . . ?
C23 C22 H22 108.0 . . ?
C24 C22 H22 108.0 . . ?
C21 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C26 N1 111.3(5) . . ?
N2 C26 C27 126.1(5) . . ?
N1 C26 C27 122.5(5) . . ?
N2 C26 Th1 55.8(3) . . ?
N1 C26 Th1 55.6(3) . . ?
C27 C26 Th1 176.3(4) . . ?
C28 C27 C32 117.6(5) . . ?
C28 C27 C26 120.3(5) . . ?
C32 C27 C26 122.2(5) . . ?
C29 C28 C27 121.9(6) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C30 119.8(6) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C31 C30 C29 119.7(6) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.0(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 121.0(6) . . ?
C27 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C41 C33 C34 122.8(5) . . ?
C41 C33 N2 117.0(5) . . ?
C34 C33 N2 120.0(5) . . ?
C33 C34 C38 116.1(5) . . ?
C33 C34 C35 122.0(5) . . ?
C38 C34 C35 121.8(5) . . ?
C34 C35 C37 110.5(5) . . ?
C34 C35 C36 110.4(6) . . ?
C37 C35 C36 111.0(5) . . ?
C34 C35 H35 108.3 . . ?
C37 C35 H35 108.3 . . ?
C36 C35 H35 108.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C34 122.2(6) . . ?
C39 C38 H38 118.9 . . ?
C34 C38 H38 118.9 . . ?
C38 C39 C40 119.4(6) . . ?
C38 C39 H39 120.3 . . ?
C40 C39 H39 120.3 . . ?
C39 C40 C41 122.3(6) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C33 C41 C40 116.9(5) . . ?
C33 C41 C42 122.4(5) . . ?
C40 C41 C42 120.7(6) . . ?
C44 C42 C41 112.6(6) . . ?
C44 C42 C43 109.3(6) . . ?
C41 C42 C43 110.9(6) . . ?
C44 C42 H42 108.0 . . ?
C41 C42 H42 108.0 . . ?
C43 C42 H42 108.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C26 N1 C13 124.9(5) . . ?
C26 N1 Th1 97.8(3) . . ?
C13 N1 Th1 135.0(3) . . ?
C26 N2 C33 123.3(4) . . ?
C26 N2 Th1 97.8(3) . . ?
C33 N2 Th1 138.8(3) . . ?
C1 Si1 C6 114.1(3) . . ?
C1 Si1 C5 108.6(3) . . ?
C6 Si1 C5 108.5(4) . . ?
C1 Si1 C4 109.3(4) . . ?
C6 Si1 C4 108.4(4) . . ?
C5 Si1 C4 107.8(5) . . ?
C2 Si2 C8 112.2(3) . . ?
C2 Si2 C7 111.8(3) . . ?
C8 Si2 C7 108.6(4) . . ?
C2 Si2 C9 110.0(3) . . ?
C8 Si2 C9 106.7(4) . . ?
C7 Si2 C9 107.3(4) . . ?
C10 Si3 C3 110.9(3) . . ?
C10 Si3 C12 107.3(4) . . ?
C3 Si3 C12 112.4(3) . . ?
C10 Si3 C11 108.3(4) . . ?
C3 Si3 C11 109.9(3) . . ?
C12 Si3 C11 107.9(4) . . ?
C3 Th1 C1 111.9(2) . . ?
C3 Th1 C2 97.14(19) . . ?
C1 Th1 C2 102.1(2) . . ?
C3 Th1 N1 106.04(17) . . ?
C1 Th1 N1 104.99(19) . . ?
C2 Th1 N1 134.00(16) . . ?
C3 Th1 N2 128.38(17) . . ?
C1 Th1 N2 118.86(18) . . ?
C2 Th1 N2 81.34(16) . . ?
N1 Th1 N2 53.08(13) . . ?
C3 Th1 C26 119.75(17) . . ?
C1 Th1 C26 114.89(19) . . ?
C2 Th1 C26 107.60(17) . . ?
N1 Th1 C26 26.60(13) . . ?
N2 Th1 C26 26.49(13) . . ?

_refine_diff_density_max         1.178
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.127


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.500 0.500 1.000 600 104 ' '
_platon_squeeze_details          
;
One disordered Toluene molecule per formual unit of (NCN)Th(CH2SiMe3)3

was not modelled and the disordered density was taken into account

using the SQUEEZE/PLATON procedure.(Sluis, P. van der; Spek, A. L. Acta Crystallogr.

1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta

Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3.

PLATON - a multipurpose crystallographic tool.  Utrecht University,

Utrecht, The Netherlands). 
;
####################################################################### 
# 
# 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_Y031
_database_code_depnum_ccdc_archive 'CCDC 981993'
_audit_update_record             
;
2014-01-17 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[NP]Th(CH2C6H4CH3)3'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H54 N P Th'
_chemical_formula_weight         907.93

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'
P P 0.1023 0.0942 '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/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                   14.2747(7)
_cell_length_b                   16.5427(8)
_cell_length_c                   17.8960(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.0030(10)
_cell_angle_gamma                90
_cell_volume                     4161.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             1816
_exptl_transmission_factor_min   0.763
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    3.654
_shelx_estimated_absorpt_T_min   0.309
_shelx_estimated_absorpt_T_max   0.487
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23821
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7290
_reflns_number_gt                6111
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2013)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2013)'

_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)+(0.0409P)²]
 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         7290
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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 0.7847(3) 0.8071(3) 0.0000(3) 0.0361(11) Uani 1 1 d . . . . .
H1A H 0.7568 0.8613 0.0047 0.043 Uiso 1 1 calc R U . . .
H1B H 0.8074 0.8010 -0.0490 0.043 Uiso 1 1 calc R U . . .
C2 C 0.7266(3) 0.7406(3) 0.0186(3) 0.0316(11) Uani 1 1 d . . . . .
C3 C 0.6943(3) 0.7393(3) 0.0883(3) 0.0349(11) Uani 1 1 d . . . . .
H3 H 0.7049 0.7852 0.1206 0.042 Uiso 1 1 calc R U . . .
C4 C 0.6473(3) 0.6727(3) 0.1115(3) 0.0368(12) Uani 1 1 d . . . . .
H4 H 0.6255 0.6753 0.1587 0.044 Uiso 1 1 calc R U . . .
C5 C 0.6310(3) 0.6030(3) 0.0688(3) 0.0380(12) Uani 1 1 d . . . . .
C6 C 0.5805(4) 0.5308(3) 0.0947(3) 0.0517(14) Uani 1 1 d . . . . .
H6A H 0.5760 0.4881 0.0563 0.078 Uiso 1 1 calc R U . . .
H6B H 0.5164 0.5466 0.1016 0.078 Uiso 1 1 calc R U . . .
H6C H 0.6162 0.5108 0.1428 0.078 Uiso 1 1 calc R U . . .
C7 C 0.6635(3) 0.6035(3) -0.0010(3) 0.0402(12) Uani 1 1 d . . . . .
H7 H 0.6532 0.5571 -0.0326 0.048 Uiso 1 1 calc R U . . .
C8 C 0.7097(3) 0.6692(3) -0.0248(3) 0.0367(12) Uani 1 1 d . . . . .
H8 H 0.7310 0.6664 -0.0721 0.044 Uiso 1 1 calc R U . . .
C9 C 0.9481(3) 0.8606(3) 0.2279(3) 0.0368(12) Uani 1 1 d . . . . .
H9A H 0.9698 0.8338 0.2773 0.044 Uiso 1 1 calc R U . . .
H9B H 0.9928 0.9038 0.2189 0.044 Uiso 1 1 calc R U . . .
C10 C 0.8481(3) 0.8865(3) 0.2161(3) 0.0344(11) Uani 1 1 d . . . . .
C11 C 0.8113(3) 0.9378(3) 0.1557(3) 0.0362(11) Uani 1 1 d . . . . .
H11 H 0.8533 0.9608 0.1258 0.043 Uiso 1 1 calc R U . . .
C12 C 0.7150(3) 0.9556(3) 0.1387(3) 0.0477(14) Uani 1 1 d . . . . .
H12 H 0.6925 0.9907 0.0974 0.057 Uiso 1 1 calc R U . . .
C13 C 0.6509(4) 0.9237(3) 0.1803(3) 0.0507(15) Uani 1 1 d . . . . .
C14 C 0.5454(4) 0.9424(4) 0.1598(4) 0.079(2) Uani 1 1 d . . . . .
H14A H 0.5111 0.9148 0.1953 0.118 Uiso 1 1 calc R U . . .
H14B H 0.5214 0.9236 0.1080 0.118 Uiso 1 1 calc R U . . .
H14C H 0.5356 1.0009 0.1627 0.118 Uiso 1 1 calc R U . . .
C15 C 0.6859(4) 0.8726(3) 0.2399(3) 0.0502(15) Uani 1 1 d . . . . .
H15 H 0.6431 0.8494 0.2691 0.060 Uiso 1 1 calc R U . . .
C16 C 0.7814(4) 0.8545(3) 0.2580(3) 0.0451(13) Uani 1 1 d . . . . .
H16 H 0.8029 0.8197 0.2996 0.054 Uiso 1 1 calc R U . . .
C17 C 0.9211(4) 0.6123(3) 0.1399(3) 0.0386(12) Uani 1 1 d . . . . .
H17A H 0.8624 0.5815 0.1209 0.046 Uiso 1 1 calc R U . . .
H17B H 0.9771 0.5876 0.1229 0.046 Uiso 1 1 calc R U . . .
C18 C 0.9353(3) 0.6303(3) 0.2207(3) 0.0317(11) Uani 1 1 d . . . . .
C19 C 1.0239(3) 0.6575(3) 0.2610(3) 0.0403(12) Uani 1 1 d . . . . .
H19 H 1.0768 0.6596 0.2354 0.048 Uiso 1 1 calc R U . . .
C20 C 1.0362(3) 0.6809(3) 0.3358(3) 0.0440(13) Uani 1 1 d . . . . .
H20 H 1.0977 0.6964 0.3610 0.053 Uiso 1 1 calc R U . . .
C21 C 0.9611(4) 0.6824(3) 0.3753(3) 0.0473(14) Uani 1 1 d . . . . .
C22 C 0.9739(5) 0.7080(5) 0.4575(3) 0.078(2) Uani 1 1 d . . . . .
H22A H 0.9126 0.7050 0.4750 0.117 Uiso 1 1 calc R U . . .
H22B H 0.9977 0.7636 0.4625 0.117 Uiso 1 1 calc R U . . .
H22C H 1.0196 0.6719 0.4882 0.117 Uiso 1 1 calc R U . . .
C23 C 0.8727(3) 0.6590(3) 0.3362(3) 0.0454(13) Uani 1 1 d . . . . .
H23 H 0.8197 0.6596 0.3618 0.054 Uiso 1 1 calc R U . . .
C24 C 0.8592(3) 0.6349(3) 0.2614(3) 0.0379(12) Uani 1 1 d . . . . .
H24 H 0.7970 0.6209 0.2365 0.045 Uiso 1 1 calc R U . . .
C25 C 1.0987(3) 0.6891(2) 0.0278(2) 0.0230(9) Uani 1 1 d . . . . .
C26 C 1.1960(3) 0.6742(3) 0.0556(2) 0.0264(10) Uani 1 1 d . . . . .
C27 C 1.2449(3) 0.7009(3) 0.1338(2) 0.0296(10) Uani 1 1 d . . . . .
H27 H 1.2005 0.7374 0.1552 0.036 Uiso 1 1 calc R U . . .
C28 C 1.3383(3) 0.7470(3) 0.1338(3) 0.0433(14) Uani 1 1 d . . . . .
H28A H 1.3657 0.7627 0.1858 0.065 Uiso 1 1 calc R U . . .
H28B H 1.3256 0.7955 0.1022 0.065 Uiso 1 1 calc R U . . .
H28C H 1.3833 0.7122 0.1132 0.065 Uiso 1 1 calc R U . . .
C29 C 1.2631(4) 0.6261(3) 0.1855(3) 0.0456(13) Uani 1 1 d . . . . .
H29A H 1.2944 0.6428 0.2363 0.068 Uiso 1 1 calc R U . . .
H29B H 1.3042 0.5881 0.1643 0.068 Uiso 1 1 calc R U . . .
H29C H 1.2024 0.5999 0.1888 0.068 Uiso 1 1 calc R U . . .
C30 C 1.2473(3) 0.6272(3) 0.0116(3) 0.0334(11) Uani 1 1 d . . . . .
H30 H 1.3132 0.6185 0.0290 0.040 Uiso 1 1 calc R U . . .
C31 C 1.2049(3) 0.5935(3) -0.0561(3) 0.0359(11) Uani 1 1 d . . . . .
H31 H 1.2418 0.5644 -0.0864 0.043 Uiso 1 1 calc R U . . .
C32 C 1.1082(3) 0.6023(3) -0.0793(3) 0.0319(11) Uani 1 1 d . . . . .
H32 H 1.0783 0.5760 -0.1244 0.038 Uiso 1 1 calc R U . . .
C33 C 1.0532(3) 0.6485(3) -0.0385(2) 0.0259(10) Uani 1 1 d . . . . .
C34 C 0.9459(3) 0.6499(3) -0.0666(2) 0.0287(10) Uani 1 1 d . . . . .
H34 H 0.9161 0.6815 -0.0292 0.034 Uiso 1 1 calc R U . . .
C35 C 0.9201(3) 0.6915(3) -0.1440(3) 0.0369(11) Uani 1 1 d . . . . .
H35A H 0.8509 0.6915 -0.1598 0.055 Uiso 1 1 calc R U . . .
H35B H 0.9495 0.6622 -0.1815 0.055 Uiso 1 1 calc R U . . .
H35C H 0.9435 0.7473 -0.1401 0.055 Uiso 1 1 calc R U . . .
C36 C 0.9054(3) 0.5641(3) -0.0697(3) 0.0374(12) Uani 1 1 d . . . . .
H36A H 0.8365 0.5660 -0.0872 0.056 Uiso 1 1 calc R U . . .
H36B H 0.9189 0.5399 -0.0190 0.056 Uiso 1 1 calc R U . . .
H36C H 0.9350 0.5314 -0.1049 0.056 Uiso 1 1 calc R U . . .
C37 C 1.1580(3) 0.8941(2) 0.0963(2) 0.0261(10) Uani 1 1 d . . . . .
C38 C 1.2145(3) 0.9432(3) 0.0590(3) 0.0358(11) Uani 1 1 d . . . . .
H38 H 1.2013 0.9473 0.0052 0.043 Uiso 1 1 calc R U . . .
C39 C 1.2900(3) 0.9863(3) 0.0998(3) 0.0428(13) Uani 1 1 d . . . . .
H39 H 1.3280 1.0196 0.0737 0.051 Uiso 1 1 calc R U . . .
C40 C 1.3102(3) 0.9812(3) 0.1776(3) 0.0457(14) Uani 1 1 d . . . . .
H40 H 1.3619 1.0109 0.2051 0.055 Uiso 1 1 calc R U . . .
C41 C 1.2550(3) 0.9329(3) 0.2160(3) 0.0383(12) Uani 1 1 d . . . . .
H41 H 1.2690 0.9291 0.2698 0.046 Uiso 1 1 calc R U . . .
C42 C 1.1792(3) 0.8900(3) 0.1756(3) 0.0325(11) Uani 1 1 d . . . . .
H42 H 1.1411 0.8573 0.2021 0.039 Uiso 1 1 calc R U . . .
C43 C 1.0468(3) 0.8651(3) -0.0506(2) 0.0258(10) Uani 1 1 d . . . . .
C44 C 0.9733(3) 0.9119(2) -0.0894(2) 0.0278(10) Uani 1 1 d . . . . .
H44 H 0.9278 0.9347 -0.0626 0.033 Uiso 1 1 calc R U . . .
C45 C 0.9653(3) 0.9258(3) -0.1663(3) 0.0354(11) Uani 1 1 d . . . . .
H45 H 0.9150 0.9583 -0.1920 0.042 Uiso 1 1 calc R U . . .
C46 C 1.0304(3) 0.8924(3) -0.2057(3) 0.0365(11) Uani 1 1 d . . . . .
H46 H 1.0244 0.9014 -0.2588 0.044 Uiso 1 1 calc R U . . .
C47 C 1.1044(3) 0.8458(3) -0.1685(3) 0.0352(11) Uani 1 1 d . . . . .
H47 H 1.1493 0.8230 -0.1959 0.042 Uiso 1 1 calc R U . . .
C48 C 1.1132(3) 0.8324(3) -0.0910(2) 0.0287(10) Uani 1 1 d . . . . .
H48 H 1.1645 0.8009 -0.0654 0.034 Uiso 1 1 calc R U . . .
N1 N 1.0450(2) 0.74557(19) 0.0646(2) 0.0235(8) Uani 1 1 d . . . . .
P1 P 1.04786(8) 0.84606(7) 0.04948(6) 0.0239(3) Uani 1 1 d . . . . .
Th1 Th 0.90603(2) 0.76247(2) 0.11715(2) 0.02449(7) 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 C2 1.451(6) . ?
C1 Th1 2.585(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.404(7) . ?
C2 C8 1.410(6) . ?
C2 Th1 2.869(5) . ?
C3 C4 1.390(6) . ?
C3 Th1 3.001(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(7) . ?
C4 H4 0.9500 . ?
C5 C7 1.406(6) . ?
C5 C6 1.509(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.378(7) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.469(6) . ?
C9 Th1 2.552(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.402(6) . ?
C10 C16 1.413(7) . ?
C10 Th1 2.921(4) . ?
C11 C12 1.388(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(7) . ?
C12 H12 0.9500 . ?
C13 C15 1.385(8) . ?
C13 C14 1.519(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.378(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.456(6) . ?
C17 Th1 2.520(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C24 1.410(6) . ?
C18 C19 1.416(6) . ?
C18 Th1 2.850(4) . ?
C19 C20 1.376(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(7) . ?
C20 H20 0.9500 . ?
C21 C23 1.387(7) . ?
C21 C22 1.509(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.379(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.413(5) . ?
C25 C33 1.419(6) . ?
C25 N1 1.438(5) . ?
C26 C30 1.401(6) . ?
C26 C27 1.517(6) . ?
C27 C28 1.537(6) . ?
C27 C29 1.539(6) . ?
C27 H27 1.0000 . ?
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 C31 1.374(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.379(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.526(6) . ?
C34 C36 1.530(6) . ?
C34 C35 1.533(6) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.395(6) . ?
C37 C42 1.401(6) . ?
C37 P1 1.829(4) . ?
C38 C39 1.389(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.375(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.386(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.388(6) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.389(6) . ?
C43 C48 1.397(6) . ?
C43 P1 1.816(4) . ?
C44 C45 1.380(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.376(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.388(6) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 P1 1.686(3) . ?
N1 Th1 2.355(3) . ?
P1 Th1 2.8859(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
C2 C1 Th1 85.8(3) . . ?
C2 C1 H1A 114.4 . . ?
Th1 C1 H1A 114.4 . . ?
C2 C1 H1B 114.4 . . ?
Th1 C1 H1B 114.4 . . ?
H1A C1 H1B 111.5 . . ?
C3 C2 C8 115.2(4) . . ?
C3 C2 C1 120.3(4) . . ?
C8 C2 C1 124.0(4) . . ?
C3 C2 Th1 81.5(3) . . ?
C8 C2 Th1 119.5(3) . . ?
C1 C2 Th1 64.0(2) . . ?
C4 C3 C2 121.9(4) . . ?
C4 C3 Th1 125.0(3) . . ?
C2 C3 Th1 71.0(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
Th1 C3 H3 75.2 . . ?
C5 C4 C3 122.7(5) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C4 C5 C7 116.0(5) . . ?
C4 C5 C6 122.4(5) . . ?
C7 C5 C6 121.7(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C5 121.9(5) . . ?
C8 C7 H7 119.0 . . ?
C5 C7 H7 119.0 . . ?
C7 C8 C2 122.4(4) . . ?
C7 C8 H8 118.8 . . ?
C2 C8 H8 118.8 . . ?
C10 C9 Th1 89.0(3) . . ?
C10 C9 H9A 113.8 . . ?
Th1 C9 H9A 113.8 . . ?
C10 C9 H9B 113.8 . . ?
Th1 C9 H9B 113.8 . . ?
H9A C9 H9B 111.0 . . ?
C11 C10 C16 116.0(5) . . ?
C11 C10 C9 120.8(4) . . ?
C16 C10 C9 122.8(5) . . ?
C11 C10 Th1 93.8(3) . . ?
C16 C10 Th1 110.3(3) . . ?
C9 C10 Th1 60.9(2) . . ?
C12 C11 C10 121.5(5) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C13 C12 C11 121.6(5) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C15 117.7(5) . . ?
C12 C13 C14 120.8(6) . . ?
C15 C13 C14 121.4(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C13 121.5(5) . . ?
C16 C15 H15 119.2 . . ?
C13 C15 H15 119.2 . . ?
C15 C16 C10 121.7(5) . . ?
C15 C16 H16 119.2 . . ?
C10 C16 H16 119.2 . . ?
C18 C17 Th1 87.3(3) . . ?
C18 C17 H17A 114.1 . . ?
Th1 C17 H17A 114.1 . . ?
C18 C17 H17B 114.1 . . ?
Th1 C17 H17B 114.1 . . ?
H17A C17 H17B 111.3 . . ?
C24 C18 C19 114.8(4) . . ?
C24 C18 C17 122.5(4) . . ?
C19 C18 C17 121.9(4) . . ?
C24 C18 Th1 104.8(3) . . ?
C19 C18 Th1 96.0(3) . . ?
C17 C18 Th1 62.0(2) . . ?
C20 C19 C18 122.4(4) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C19 C20 C21 121.6(5) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C23 117.0(5) . . ?
C20 C21 C22 121.9(5) . . ?
C23 C21 C22 121.0(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C21 122.2(5) . . ?
C24 C23 H23 118.9 . . ?
C21 C23 H23 118.9 . . ?
C23 C24 C18 121.8(5) . . ?
C23 C24 H24 119.1 . . ?
C18 C24 H24 119.1 . . ?
C26 C25 C33 119.4(4) . . ?
C26 C25 N1 121.4(4) . . ?
C33 C25 N1 119.2(4) . . ?
C30 C26 C25 118.5(4) . . ?
C30 C26 C27 118.6(4) . . ?
C25 C26 C27 122.7(4) . . ?
C26 C27 C28 113.9(4) . . ?
C26 C27 C29 108.9(4) . . ?
C28 C27 C29 110.1(4) . . ?
C26 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C26 121.9(4) . . ?
C31 C30 H30 119.1 . . ?
C26 C30 H30 119.1 . . ?
C30 C31 C32 119.2(4) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C31 C32 C33 121.8(4) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C32 C33 C25 118.8(4) . . ?
C32 C33 C34 117.5(4) . . ?
C25 C33 C34 123.7(4) . . ?
C33 C34 C36 110.4(4) . . ?
C33 C34 C35 111.9(4) . . ?
C36 C34 C35 110.7(4) . . ?
C33 C34 H34 107.9 . . ?
C36 C34 H34 107.9 . . ?
C35 C34 H34 107.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 118.2(4) . . ?
C38 C37 P1 123.8(3) . . ?
C42 C37 P1 117.4(3) . . ?
C39 C38 C37 120.6(5) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 C38 120.5(5) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C39 C40 C41 120.1(5) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 C42 119.7(5) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C41 C42 C37 121.0(5) . . ?
C41 C42 H42 119.5 . . ?
C37 C42 H42 119.5 . . ?
C44 C43 C48 118.6(4) . . ?
C44 C43 P1 117.8(3) . . ?
C48 C43 P1 123.6(3) . . ?
C45 C44 C43 121.0(4) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C46 C45 C44 119.9(4) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C47 120.3(4) . . ?
C45 C46 H46 119.9 . . ?
C47 C46 H46 119.9 . . ?
C46 C47 C48 120.0(4) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 C43 120.2(4) . . ?
C47 C48 H48 119.9 . . ?
C43 C48 H48 119.9 . . ?
C25 N1 P1 122.5(3) . . ?
C25 N1 Th1 144.3(3) . . ?
P1 N1 Th1 89.57(15) . . ?
N1 P1 C43 109.46(19) . . ?
N1 P1 C37 113.42(19) . . ?
C43 P1 C37 103.6(2) . . ?
N1 P1 Th1 54.69(12) . . ?
C43 P1 Th1 127.65(14) . . ?
C37 P1 Th1 128.72(15) . . ?
N1 Th1 C17 83.86(13) . . ?
N1 Th1 C9 106.54(14) . . ?
C17 Th1 C9 119.97(15) . . ?
N1 Th1 C1 101.66(13) . . ?
C17 Th1 C1 116.06(15) . . ?
C9 Th1 C1 118.85(14) . . ?
N1 Th1 C18 97.48(12) . . ?
C17 Th1 C18 30.69(13) . . ?
C9 Th1 C18 89.69(15) . . ?
C1 Th1 C18 138.49(14) . . ?
N1 Th1 C2 117.60(13) . . ?
C17 Th1 C2 90.98(14) . . ?
C9 Th1 C2 128.50(14) . . ?
C1 Th1 C2 30.29(13) . . ?
C18 Th1 C2 108.51(13) . . ?
N1 Th1 P1 35.74(8) . . ?
C17 Th1 P1 119.56(11) . . ?
C9 Th1 P1 86.19(12) . . ?
C1 Th1 P1 86.71(10) . . ?
C18 Th1 P1 127.32(9) . . ?
C2 Th1 P1 114.75(10) . . ?
N1 Th1 C10 132.22(12) . . ?
C17 Th1 C10 128.28(14) . . ?
C9 Th1 C10 30.19(13) . . ?
C1 Th1 C10 94.06(14) . . ?
C18 Th1 C10 99.76(14) . . ?
C2 Th1 C10 98.35(13) . . ?
P1 Th1 C10 102.17(10) . . ?
N1 Th1 C3 144.03(13) . . ?
C17 Th1 C3 87.55(14) . . ?
C9 Th1 C3 108.00(14) . . ?
C1 Th1 C3 51.99(14) . . ?
C18 Th1 C3 92.48(13) . . ?
C2 Th1 C3 27.57(13) . . ?
P1 Th1 C3 138.42(10) . . ?
C10 Th1 C3 79.13(13) . . ?

_refine_diff_density_max         1.265
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.168



####################################################################### 
# 
# 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_X219
_database_code_depnum_ccdc_archive 'CCDC 981991'
_audit_update_record             
;
2014-01-17 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (NPN)Th(CH2SiMe3)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H77 N2 P Si3 Th'
_chemical_formula_weight         1029.39

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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. 
;

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                   12.1409(5)
_cell_length_b                   21.1710(9)
_cell_length_c                   20.5445(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.5670(10)
_cell_angle_gamma                90
_cell_volume                     5221.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    8811
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             2104
_exptl_transmission_factor_min   0.872
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.986
_shelx_estimated_absorpt_T_min   0.522
_shelx_estimated_absorpt_T_max   0.663
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25594
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.696
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_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             9173
_reflns_number_gt                7658
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2013)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2013)'

_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)+(0.0343P)²] 
 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         9173
_refine_ls_number_parameters     509
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.2140(3) 0.08116(18) 0.12916(18) 0.0399(9) Uani 1 1 d . . . . .
H1A H 0.2126 0.0536 0.0901 0.048 Uiso 1 1 calc R U . . .
H1B H 0.1442 0.1060 0.1220 0.048 Uiso 1 1 calc R U . . .
C2 C 0.0023(3) 0.02298(17) 0.23307(18) 0.0375(9) Uani 1 1 d . . . . .
H2A H -0.0363 -0.0139 0.2106 0.045 Uiso 1 1 calc R U . . .
H2B H -0.0029 0.0180 0.2804 0.045 Uiso 1 1 calc R U . . .
C3 C 0.2738(4) 0.07487(19) 0.31997(19) 0.0495(11) Uani 1 1 d D . . . .
H3A H 0.3510 0.0590 0.3312 0.059 Uiso 1 1 calc R U . A 1
H3B H 0.2815 0.1170 0.3002 0.059 Uiso 1 1 calc R U . A 1
C4 C 0.4647(4) 0.1055(2) 0.1653(2) 0.0658(14) Uani 1 1 d . . . . .
H4A H 0.5233 0.1369 0.1632 0.099 Uiso 1 1 calc R U . . .
H4B H 0.4815 0.0672 0.1419 0.099 Uiso 1 1 calc R U . . .
H4C H 0.4609 0.0951 0.2114 0.099 Uiso 1 1 calc R U . . .
C5 C 0.3030(5) 0.2108(2) 0.1726(3) 0.0776(17) Uani 1 1 d . . . . .
H5A H 0.3644 0.2406 0.1714 0.116 Uiso 1 1 calc R U . . .
H5B H 0.2980 0.1998 0.2185 0.116 Uiso 1 1 calc R U . . .
H5C H 0.2330 0.2304 0.1524 0.116 Uiso 1 1 calc R U . . .
C6 C 0.3423(4) 0.1638(2) 0.0407(2) 0.0674(14) Uani 1 1 d . . . . .
H6A H 0.4044 0.1936 0.0422 0.101 Uiso 1 1 calc R U . . .
H6B H 0.2732 0.1844 0.0206 0.101 Uiso 1 1 calc R U . . .
H6C H 0.3565 0.1268 0.0144 0.101 Uiso 1 1 calc R U . . .
C7 C -0.2142(4) 0.0961(2) 0.2431(3) 0.0652(13) Uani 1 1 d . . . . .
H7A H -0.2573 0.1336 0.2269 0.098 Uiso 1 1 calc R U . . .
H7B H -0.1948 0.0986 0.2911 0.098 Uiso 1 1 calc R U . . .
H7C H -0.2588 0.0581 0.2313 0.098 Uiso 1 1 calc R U . . .
C8 C -0.1261(5) 0.0897(3) 0.1144(2) 0.0839(17) Uani 1 1 d . . . . .
H8A H -0.1715 0.1268 0.1000 0.126 Uiso 1 1 calc R U . . .
H8B H -0.1696 0.0513 0.1025 0.126 Uiso 1 1 calc R U . . .
H8C H -0.0594 0.0894 0.0928 0.126 Uiso 1 1 calc R U . . .
C9 C -0.0063(4) 0.1670(2) 0.2264(3) 0.0795(17) Uani 1 1 d . . . . .
H9A H -0.0534 0.2031 0.2109 0.119 Uiso 1 1 calc R U . . .
H9B H 0.0610 0.1674 0.2053 0.119 Uiso 1 1 calc R U . . .
H9C H 0.0147 0.1696 0.2743 0.119 Uiso 1 1 calc R U . . .
Si3 Si 0.2359(3) 0.09512(18) 0.40297(17) 0.0512(8) Uani 0.787(6) 1 d D . P B 1
C10 C 0.3065(8) 0.1636(4) 0.4410(5) 0.0884(18) Uani 0.787(6) 1 d D . P B 1
H10A H 0.3872 0.1569 0.4460 0.133 Uiso 0.787(6) 1 calc R U P B 1
H10B H 0.2841 0.1704 0.4843 0.133 Uiso 0.787(6) 1 calc R U P B 1
H10C H 0.2866 0.2007 0.4132 0.133 Uiso 0.787(6) 1 calc R U P B 1
C11 C 0.0898(6) 0.1222(3) 0.4011(3) 0.0884(18) Uani 0.787(6) 1 d D . P B 1
H11A H 0.0387 0.0894 0.3809 0.133 Uiso 0.787(6) 1 calc R U P B 1
H11B H 0.0780 0.1611 0.3752 0.133 Uiso 0.787(6) 1 calc R U P B 1
H11C H 0.0758 0.1302 0.4461 0.133 Uiso 0.787(6) 1 calc R U P B 1
C12 C 0.2547(8) 0.0259(3) 0.4598(3) 0.0884(18) Uani 0.787(6) 1 d D . P B 1
H12A H 0.2151 -0.0106 0.4385 0.133 Uiso 0.787(6) 1 calc R U P B 1
H12B H 0.2247 0.0360 0.5003 0.133 Uiso 0.787(6) 1 calc R U P B 1
H12C H 0.3342 0.0161 0.4706 0.133 Uiso 0.787(6) 1 calc R U P B 1
Si3' Si 0.2765(10) 0.0833(6) 0.4069(6) 0.044(3) Uani 0.213(6) 1 d D . P B 2
C10' C 0.353(2) 0.1526(12) 0.4432(15) 0.065(5) Uani 0.213(6) 1 d D . P B 2
H10D H 0.3505 0.1536 0.4907 0.097 Uiso 0.213(6) 1 calc R U P B 2
H10E H 0.3190 0.1910 0.4227 0.097 Uiso 0.213(6) 1 calc R U P B 2
H10F H 0.4308 0.1500 0.4357 0.097 Uiso 0.213(6) 1 calc R U P B 2
C11' C 0.1460(18) 0.0480(10) 0.4270(10) 0.065(5) Uani 0.213(6) 1 d D . P B 2
H11D H 0.1447 0.0515 0.4745 0.097 Uiso 0.213(6) 1 calc R U P B 2
H11E H 0.1423 0.0034 0.4142 0.097 Uiso 0.213(6) 1 calc R U P B 2
H11F H 0.0819 0.0706 0.4031 0.097 Uiso 0.213(6) 1 calc R U P B 2
C12' C 0.3987(18) 0.0429(10) 0.4513(9) 0.065(5) Uani 0.213(6) 1 d D . P B 2
H12D H 0.3989 0.0473 0.4988 0.097 Uiso 0.213(6) 1 calc R U P B 2
H12E H 0.4666 0.0617 0.4394 0.097 Uiso 0.213(6) 1 calc R U P B 2
H12F H 0.3959 -0.0020 0.4396 0.097 Uiso 0.213(6) 1 calc R U P B 2
C13 C 0.3019(3) -0.20425(16) 0.19523(16) 0.0320(9) Uani 1 1 d . . . . .
C14 C 0.4138(3) -0.22075(17) 0.19751(18) 0.0407(10) Uani 1 1 d . . . . .
H14 H 0.4701 -0.1947 0.2208 0.049 Uiso 1 1 calc R U . . .
C15 C 0.4436(4) -0.27479(19) 0.1660(2) 0.0513(12) Uani 1 1 d . . . . .
H15 H 0.5199 -0.2855 0.1676 0.062 Uiso 1 1 calc R U . . .
C16 C 0.3625(5) -0.31251(19) 0.1327(2) 0.0570(13) Uani 1 1 d . . . . .
H16 H 0.3830 -0.3494 0.1111 0.068 Uiso 1 1 calc R U . . .
C17 C 0.2512(5) -0.29754(19) 0.13021(19) 0.0553(13) Uani 1 1 d . . . . .
H17 H 0.1954 -0.3238 0.1067 0.066 Uiso 1 1 calc R U . . .
C18 C 0.2214(4) -0.24373(17) 0.16238(17) 0.0412(10) Uani 1 1 d . . . . .
H18 H 0.1449 -0.2340 0.1618 0.049 Uiso 1 1 calc R U . . .
C19 C 0.3072(3) -0.16401(16) 0.32522(16) 0.0302(8) Uani 1 1 d . . . . .
C20 C 0.3123(3) -0.12140(17) 0.37727(17) 0.0349(9) Uani 1 1 d . . . . .
H20 H 0.2956 -0.0781 0.3684 0.042 Uiso 1 1 calc R U . . .
C21 C 0.3413(4) -0.14121(19) 0.44146(18) 0.0439(10) Uani 1 1 d . . . . .
H21 H 0.3467 -0.1115 0.4764 0.053 Uiso 1 1 calc R U . . .
C22 C 0.3625(4) -0.2047(2) 0.45493(19) 0.0500(11) Uani 1 1 d . . . . .
H22 H 0.3813 -0.2185 0.4992 0.060 Uiso 1 1 calc R U . . .
C23 C 0.3562(4) -0.24690(19) 0.40477(18) 0.0463(11) Uani 1 1 d . . . . .
H23 H 0.3712 -0.2903 0.4141 0.056 Uiso 1 1 calc R U . . .
C24 C 0.3282(3) -0.22714(17) 0.33990(18) 0.0386(9) Uani 1 1 d . . . . .
H24 H 0.3234 -0.2572 0.3053 0.046 Uiso 1 1 calc R U . . .
C25 C 0.4470(3) -0.07110(15) 0.20487(17) 0.0300(8) Uani 1 1 d . . . . .
C26 C 0.4542(3) -0.07536(16) 0.13728(17) 0.0323(8) Uani 1 1 d . . . . .
C27 C 0.3538(3) -0.08000(17) 0.08328(17) 0.0381(9) Uani 1 1 d . . . . .
H27 H 0.2848 -0.0762 0.1042 0.046 Uiso 1 1 calc R U . . .
C28 C 0.3537(4) -0.02610(19) 0.0329(2) 0.0534(12) Uani 1 1 d . . . . .
H28A H 0.2880 -0.0299 -0.0009 0.080 Uiso 1 1 calc R U . . .
H28B H 0.4212 -0.0287 0.0121 0.080 Uiso 1 1 calc R U . . .
H28C H 0.3520 0.0146 0.0554 0.080 Uiso 1 1 calc R U . . .
C29 C 0.3486(4) -0.14321(17) 0.04539(18) 0.0472(11) Uani 1 1 d . . . . .
H29A H 0.2824 -0.1437 0.0117 0.071 Uiso 1 1 calc R U . . .
H29B H 0.3447 -0.1782 0.0761 0.071 Uiso 1 1 calc R U . . .
H29C H 0.4155 -0.1478 0.0243 0.071 Uiso 1 1 calc R U . . .
C30 C 0.5592(4) -0.07345(18) 0.1180(2) 0.0448(10) Uani 1 1 d . . . . .
H30 H 0.5651 -0.0765 0.0725 0.054 Uiso 1 1 calc R U . . .
C31 C 0.6542(4) -0.0673(2) 0.1627(2) 0.0525(11) Uani 1 1 d . . . . .
H31 H 0.7252 -0.0674 0.1484 0.063 Uiso 1 1 calc R U . . .
C32 C 0.6461(3) -0.0611(2) 0.2280(2) 0.0478(11) Uani 1 1 d . . . . .
H32 H 0.7122 -0.0559 0.2587 0.057 Uiso 1 1 calc R U . . .
C33 C 0.5439(3) -0.06207(16) 0.25108(18) 0.0346(9) Uani 1 1 d . . . . .
C34 C 0.5418(3) -0.05422(17) 0.32373(18) 0.0388(9) Uani 1 1 d . . . . .
H34 H 0.4620 -0.0506 0.3301 0.047 Uiso 1 1 calc R U . . .
C35 C 0.5908(4) -0.1121(2) 0.3629(2) 0.0567(12) Uani 1 1 d . . . . .
H35A H 0.5873 -0.1056 0.4098 0.085 Uiso 1 1 calc R U . . .
H35B H 0.6685 -0.1179 0.3565 0.085 Uiso 1 1 calc R U . . .
H35C H 0.5477 -0.1498 0.3475 0.085 Uiso 1 1 calc R U . . .
C36 C 0.6009(4) 0.0063(2) 0.3510(2) 0.0597(13) Uani 1 1 d . . . . .
H36A H 0.5969 0.0097 0.3981 0.090 Uiso 1 1 calc R U . . .
H36B H 0.5644 0.0430 0.3280 0.090 Uiso 1 1 calc R U . . .
H36C H 0.6790 0.0049 0.3442 0.090 Uiso 1 1 calc R U . . .
C37 C 0.0399(3) -0.13622(16) 0.22025(17) 0.0316(8) Uani 1 1 d . . . . .
C38 C -0.0176(3) -0.14688(16) 0.27316(17) 0.0331(9) Uani 1 1 d . . . . .
C39 C 0.0260(3) -0.12698(18) 0.34365(18) 0.0389(9) Uani 1 1 d . . . . .
H39 H 0.0967 -0.1029 0.3431 0.047 Uiso 1 1 calc R U . . .
C40 C -0.0562(4) -0.0835(2) 0.3726(2) 0.0535(12) Uani 1 1 d . . . . .
H40A H -0.0248 -0.0718 0.4177 0.080 Uiso 1 1 calc R U . . .
H40B H -0.1269 -0.1057 0.3728 0.080 Uiso 1 1 calc R U . . .
H40C H -0.0690 -0.0452 0.3456 0.080 Uiso 1 1 calc R U . . .
C41 C 0.0525(4) -0.1840(2) 0.38883(19) 0.0563(12) Uani 1 1 d . . . . .
H41A H 0.0804 -0.1695 0.4335 0.084 Uiso 1 1 calc R U . . .
H41B H 0.1093 -0.2101 0.3726 0.084 Uiso 1 1 calc R U . . .
H41C H -0.0152 -0.2091 0.3894 0.084 Uiso 1 1 calc R U . . .
C42 C -0.1219(3) -0.17554(18) 0.2615(2) 0.0432(10) Uani 1 1 d . . . . .
H42 H -0.1609 -0.1832 0.2975 0.052 Uiso 1 1 calc R U . . .
C43 C -0.1696(3) -0.19298(19) 0.1997(2) 0.0479(11) Uani 1 1 d . . . . .
H43 H -0.2400 -0.2135 0.1931 0.058 Uiso 1 1 calc R U . . .
C44 C -0.1151(3) -0.18071(18) 0.1471(2) 0.0454(11) Uani 1 1 d . . . . .
H44 H -0.1492 -0.1924 0.1041 0.054 Uiso 1 1 calc R U . . .
C45 C -0.0121(3) -0.15189(16) 0.15512(17) 0.0338(9) Uani 1 1 d . . . . .
C46 C 0.0404(3) -0.13454(17) 0.09468(17) 0.0401(10) Uani 1 1 d . . . . .
H46 H 0.1230 -0.1343 0.1084 0.048 Uiso 1 1 calc R U . . .
C47 C 0.0153(4) -0.1817(2) 0.03782(19) 0.0554(12) Uani 1 1 d . . . . .
H47A H 0.0519 -0.1678 0.0009 0.083 Uiso 1 1 calc R U . . .
H47B H -0.0654 -0.1839 0.0237 0.083 Uiso 1 1 calc R U . . .
H47C H 0.0432 -0.2235 0.0525 0.083 Uiso 1 1 calc R U . . .
C48 C 0.0067(4) -0.06823(19) 0.07105(19) 0.0538(12) Uani 1 1 d . . . . .
H48A H 0.0415 -0.0581 0.0323 0.081 Uiso 1 1 calc R U . . .
H48B H 0.0314 -0.0378 0.1062 0.081 Uiso 1 1 calc R U . . .
H48C H -0.0745 -0.0661 0.0595 0.081 Uiso 1 1 calc R U . . .
N1 N 0.3396(2) -0.07320(12) 0.22684(13) 0.0281(7) Uani 1 1 d . . . . .
N2 N 0.1466(2) -0.10547(13) 0.22764(13) 0.0275(6) Uani 1 1 d . . . . .
Si1 Si 0.32857(10) 0.13810(5) 0.12634(5) 0.0384(3) Uani 1 1 d . . . . .
Si2 Si -0.08435(10) 0.09249(5) 0.20498(6) 0.0415(3) Uani 1 1 d . . . . .
P1 P 0.26923(8) -0.13554(4) 0.24099(4) 0.0271(2) Uani 1 1 d . . . . .
Th1 Th 0.19938(2) 0.00993(2) 0.22341(2) 0.02916(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 Si1 1.848(4) . ?
C1 Th1 2.481(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 Si2 1.851(4) . ?
C2 Th1 2.445(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 Si3' 1.790(12) . ?
C3 Si3 1.881(5) . ?
C3 Th1 2.471(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 Si1 1.858(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Si1 1.860(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si1 1.873(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Si2 1.863(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 Si2 1.856(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 Si2 1.858(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
Si3 C10 1.802(8) . ?
Si3 C11 1.858(8) . ?
Si3 C12 1.866(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
Si3' C12' 1.833(18) . ?
Si3' C10' 1.835(19) . ?
Si3' C11' 1.853(18) . ?
C10' H10D 0.9800 . ?
C10' H10E 0.9800 . ?
C10' H10F 0.9800 . ?
C11' H11D 0.9800 . ?
C11' H11E 0.9800 . ?
C11' H11F 0.9800 . ?
C12' H12D 0.9800 . ?
C12' H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C13 C18 1.383(5) . ?
C13 C14 1.397(5) . ?
C13 P1 1.808(4) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.369(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.386(5) . ?
C19 C20 1.393(5) . ?
C19 P1 1.826(3) . ?
C20 C21 1.379(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.358(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.407(5) . ?
C25 C33 1.410(5) . ?
C25 N1 1.443(4) . ?
C26 C30 1.391(5) . ?
C26 C27 1.524(5) . ?
C27 C28 1.540(5) . ?
C27 C29 1.545(5) . ?
C27 H27 1.0000 . ?
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 C31 1.370(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.367(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.506(5) . ?
C34 C36 1.533(5) . ?
C34 C35 1.537(5) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.395(5) . ?
C37 C45 1.431(5) . ?
C37 N2 1.438(4) . ?
C38 C42 1.392(5) . ?
C38 C39 1.525(5) . ?
C39 C41 1.528(5) . ?
C39 C40 1.541(5) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.366(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.373(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.523(5) . ?
C46 C48 1.521(5) . ?
C46 C47 1.533(5) . ?
C46 H46 1.0000 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N1 P1 1.622(3) . ?
N1 Th1 2.442(3) . ?
N2 P1 1.604(3) . ?
N2 Th1 2.530(3) . ?
P1 Th1 3.2004(9) . ?

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
Si1 C1 Th1 124.22(19) . . ?
Si1 C1 H1A 106.3 . . ?
Th1 C1 H1A 106.3 . . ?
Si1 C1 H1B 106.3 . . ?
Th1 C1 H1B 106.3 . . ?
H1A C1 H1B 106.4 . . ?
Si2 C2 Th1 125.62(19) . . ?
Si2 C2 H2A 105.9 . . ?
Th1 C2 H2A 105.9 . . ?
Si2 C2 H2B 105.9 . . ?
Th1 C2 H2B 105.9 . . ?
H2A C2 H2B 106.2 . . ?
Si3' C3 Th1 143.7(5) . . ?
Si3 C3 Th1 138.2(3) . . ?
Si3 C3 H3A 102.6 . . ?
Th1 C3 H3A 102.6 . . ?
Si3 C3 H3B 102.6 . . ?
Th1 C3 H3B 102.6 . . ?
H3A C3 H3B 104.9 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 Si3 C11 98.8(4) . . ?
C10 Si3 C12 110.8(4) . . ?
C11 Si3 C12 106.4(4) . . ?
C10 Si3 C3 114.3(4) . . ?
C11 Si3 C3 114.4(3) . . ?
C12 Si3 C3 111.4(3) . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 Si3' C12' 110.1(9) . . ?
C3 Si3' C10' 114.7(12) . . ?
C12' Si3' C10' 81.2(12) . . ?
C3 Si3' C11' 107.1(9) . . ?
C12' Si3' C11' 110.9(13) . . ?
C10' Si3' C11' 129.0(13) . . ?
Si3' C10' H10D 109.5 . . ?
Si3' C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
Si3' C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
Si3' C11' H11D 109.5 . . ?
Si3' C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
Si3' C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
Si3' C12' H12D 109.5 . . ?
Si3' C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
Si3' C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C18 C13 C14 118.6(3) . . ?
C18 C13 P1 123.1(3) . . ?
C14 C13 P1 118.1(3) . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 120.8(4) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C13 C18 C17 120.8(4) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C24 C19 C20 118.2(3) . . ?
C24 C19 P1 122.5(3) . . ?
C20 C19 P1 119.3(3) . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 119.9(4) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.9(4) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.5(4) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.7 . . ?
C19 C24 C23 120.7(4) . . ?
C19 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C33 120.3(3) . . ?
C26 C25 N1 119.9(3) . . ?
C33 C25 N1 119.7(3) . . ?
C30 C26 C25 118.2(4) . . ?
C30 C26 C27 117.5(3) . . ?
C25 C26 C27 124.2(3) . . ?
C26 C27 C28 111.2(3) . . ?
C26 C27 C29 113.0(3) . . ?
C28 C27 C29 107.9(3) . . ?
C26 C27 H27 108.2 . . ?
C28 C27 H27 108.2 . . ?
C29 C27 H27 108.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C26 121.9(4) . . ?
C31 C30 H30 119.0 . . ?
C26 C30 H30 119.0 . . ?
C32 C31 C30 119.3(4) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 122.1(4) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
C32 C33 C25 118.0(4) . . ?
C32 C33 C34 118.9(3) . . ?
C25 C33 C34 123.1(3) . . ?
C33 C34 C36 112.2(3) . . ?
C33 C34 C35 111.6(3) . . ?
C36 C34 C35 110.6(3) . . ?
C33 C34 H34 107.4 . . ?
C36 C34 H34 107.4 . . ?
C35 C34 H34 107.4 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C45 119.3(3) . . ?
C38 C37 N2 122.6(3) . . ?
C45 C37 N2 118.0(3) . . ?
C42 C38 C37 119.0(3) . . ?
C42 C38 C39 117.5(3) . . ?
C37 C38 C39 123.5(3) . . ?
C38 C39 C41 111.7(3) . . ?
C38 C39 C40 112.2(3) . . ?
C41 C39 C40 109.2(3) . . ?
C38 C39 H39 107.8 . . ?
C41 C39 H39 107.8 . . ?
C40 C39 H39 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C38 121.8(4) . . ?
C43 C42 H42 119.1 . . ?
C38 C42 H42 119.1 . . ?
C42 C43 C44 119.5(4) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C45 121.6(4) . . ?
C43 C44 H44 119.2 . . ?
C45 C44 H44 119.2 . . ?
C44 C45 C37 118.7(4) . . ?
C44 C45 C46 119.4(3) . . ?
C37 C45 C46 121.8(3) . . ?
C48 C46 C45 110.9(3) . . ?
C48 C46 C47 110.1(3) . . ?
C45 C46 C47 113.8(3) . . ?
C48 C46 H46 107.2 . . ?
C45 C46 H46 107.2 . . ?
C47 C46 H46 107.2 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C25 N1 P1 127.3(2) . . ?
C25 N1 Th1 128.9(2) . . ?
P1 N1 Th1 102.02(14) . . ?
C37 N2 P1 129.6(2) . . ?
C37 N2 Th1 131.5(2) . . ?
P1 N2 Th1 98.97(13) . . ?
C1 Si1 C4 111.7(2) . . ?
C1 Si1 C5 109.9(2) . . ?
C4 Si1 C5 107.0(2) . . ?
C1 Si1 C6 113.1(2) . . ?
C4 Si1 C6 108.3(2) . . ?
C5 Si1 C6 106.6(2) . . ?
C2 Si2 C8 110.2(2) . . ?
C2 Si2 C9 110.7(2) . . ?
C8 Si2 C9 108.6(3) . . ?
C2 Si2 C7 112.3(2) . . ?
C8 Si2 C7 107.5(2) . . ?
C9 Si2 C7 107.4(2) . . ?
N2 P1 N1 98.42(15) . . ?
N2 P1 C13 120.01(16) . . ?
N1 P1 C13 113.55(16) . . ?
N2 P1 C19 112.93(16) . . ?
N1 P1 C19 111.93(16) . . ?
C13 P1 C19 100.57(16) . . ?
N2 P1 Th1 51.35(10) . . ?
N1 P1 Th1 48.27(10) . . ?
C13 P1 Th1 142.24(11) . . ?
C19 P1 Th1 116.73(11) . . ?
N1 Th1 C2 139.93(11) . . ?
N1 Th1 C3 102.00(12) . . ?
C2 Th1 C3 96.72(14) . . ?
N1 Th1 C1 109.27(11) . . ?
C2 Th1 C1 100.31(12) . . ?
C3 Th1 C1 103.19(13) . . ?
N1 Th1 N2 58.81(9) . . ?
C2 Th1 N2 81.42(11) . . ?
C3 Th1 N2 125.01(11) . . ?
C1 Th1 N2 131.41(11) . . ?
N1 Th1 P1 29.71(7) . . ?
C2 Th1 P1 110.22(9) . . ?
C3 Th1 P1 112.69(10) . . ?
C1 Th1 P1 128.63(9) . . ?
N2 Th1 P1 29.68(7) . . ?

_refine_diff_density_max         1.089
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_X263
_database_code_depnum_ccdc_archive 'CCDC 981992'
_audit_update_record             
;
2014-01-17 deposited with the CCDC.	2019-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (TpMe2)Th(CH2SiMe3)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H55 B N6 Si3 Th'
_chemical_formula_weight         790.89

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'
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'
Si Si 0.0817 0.0704 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   10.8929(8)
_cell_length_b                   12.6477(10)
_cell_length_c                   13.5582(10)
_cell_angle_alpha                97.6860(10)
_cell_angle_beta                 91.2190(10)
_cell_angle_gamma                90.2440(10)
_cell_volume                     1850.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    5495
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   0.404
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.150
_shelx_estimated_absorpt_T_min   0.491
_shelx_estimated_absorpt_T_max   0.658
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9121
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.516
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             6322
_reflns_number_gt                5714
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2013)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2013)'

_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)+(0.0524P)²] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6322
_refine_ls_number_parameters     347
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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 0.9248(6) 0.6684(5) 0.3568(4) 0.0422(14) Uani 1 1 d . . . . .
H1A H 0.8707 0.6269 0.3954 0.051 Uiso 1 1 calc R U . . .
H1B H 0.9610 0.6144 0.3063 0.051 Uiso 1 1 calc R U . . .
C2 C 0.5908(5) 0.7633(5) 0.3639(4) 0.0460(15) Uani 1 1 d . . . . .
H2A H 0.5405 0.8232 0.3459 0.055 Uiso 1 1 calc R U . . .
H2B H 0.5426 0.6975 0.3424 0.055 Uiso 1 1 calc R U . . .
C3 C 0.8246(5) 0.9459(4) 0.2745(4) 0.0340(12) Uani 1 1 d . . . . .
H3A H 0.7559 0.9787 0.3139 0.041 Uiso 1 1 calc R U . . .
H3B H 0.8960 0.9513 0.3213 0.041 Uiso 1 1 calc R U . . .
C5 C 1.0916(7) 0.8448(5) 0.4689(5) 0.0583(18) Uani 1 1 d . . . . .
H5A H 1.1623 0.8570 0.5151 0.087 Uiso 1 1 calc R U . . .
H5B H 1.0204 0.8831 0.4982 0.087 Uiso 1 1 calc R U . . .
H5C H 1.1110 0.8708 0.4061 0.087 Uiso 1 1 calc R U . . .
C6 C 1.1967(7) 0.6276(6) 0.3960(8) 0.090(3) Uani 1 1 d . . . . .
H6A H 1.2658 0.6455 0.4429 0.135 Uiso 1 1 calc R U . . .
H6B H 1.2165 0.6491 0.3314 0.135 Uiso 1 1 calc R U . . .
H6C H 1.1815 0.5505 0.3882 0.135 Uiso 1 1 calc R U . . .
C7 C 1.0226(9) 0.6544(6) 0.5682(5) 0.080(3) Uani 1 1 d . . . . .
H7A H 1.0929 0.6714 0.6140 0.119 Uiso 1 1 calc R U . . .
H7B H 1.0078 0.5772 0.5587 0.119 Uiso 1 1 calc R U . . .
H7C H 0.9495 0.6911 0.5961 0.119 Uiso 1 1 calc R U . . .
C8 C 0.6181(8) 0.6469(6) 0.5462(5) 0.070(2) Uani 1 1 d . . . . .
H8A H 0.6219 0.6568 0.6191 0.106 Uiso 1 1 calc R U . . .
H8B H 0.6947 0.6148 0.5204 0.106 Uiso 1 1 calc R U . . .
H8C H 0.5489 0.5999 0.5226 0.106 Uiso 1 1 calc R U . . .
C9 C 0.4551(7) 0.8424(8) 0.5596(6) 0.085(3) Uani 1 1 d . . . . .
H9A H 0.4635 0.8482 0.6322 0.128 Uiso 1 1 calc R U . . .
H9B H 0.3831 0.7983 0.5370 0.128 Uiso 1 1 calc R U . . .
H9C H 0.4451 0.9136 0.5398 0.128 Uiso 1 1 calc R U . . .
C10 C 0.7279(7) 0.8691(6) 0.5489(5) 0.065(2) Uani 1 1 d . . . . .
H10A H 0.7315 0.8764 0.6218 0.097 Uiso 1 1 calc R U . . .
H10B H 0.7157 0.9393 0.5275 0.097 Uiso 1 1 calc R U . . .
H10C H 0.8050 0.8387 0.5224 0.097 Uiso 1 1 calc R U . . .
C11 C 0.7571(6) 1.1637(5) 0.2161(5) 0.0463(15) Uani 1 1 d . . . . .
H11A H 0.7767 1.2157 0.1711 0.069 Uiso 1 1 calc R U . . .
H11B H 0.7684 1.1970 0.2852 0.069 Uiso 1 1 calc R U . . .
H11C H 0.6717 1.1400 0.2045 0.069 Uiso 1 1 calc R U . . .
C12 C 0.8393(6) 0.9951(5) 0.0565(4) 0.0449(14) Uani 1 1 d . . . . .
H12A H 0.8584 1.0517 0.0164 0.067 Uiso 1 1 calc R U . . .
H12B H 0.7539 0.9716 0.0433 0.067 Uiso 1 1 calc R U . . .
H12C H 0.8943 0.9347 0.0391 0.067 Uiso 1 1 calc R U . . .
C13 C 1.0217(6) 1.0997(5) 0.2114(5) 0.0530(16) Uani 1 1 d . . . . .
H13A H 1.0365 1.1526 0.1662 0.079 Uiso 1 1 calc R U . . .
H13B H 1.0796 1.0407 0.1977 0.079 Uiso 1 1 calc R U . . .
H13C H 1.0333 1.1333 0.2804 0.079 Uiso 1 1 calc R U . . .
C14 C 0.6330(5) 0.4114(4) -0.0862(4) 0.0416(14) Uani 1 1 d . . . . .
H14A H 0.6576 0.4643 -0.1288 0.062 Uiso 1 1 calc R U . . .
H14B H 0.5456 0.3941 -0.0979 0.062 Uiso 1 1 calc R U . . .
H14C H 0.6816 0.3466 -0.1020 0.062 Uiso 1 1 calc R U . . .
C15 C 0.6544(5) 0.4559(4) 0.0204(4) 0.0306(11) Uani 1 1 d . . . . .
C16 C 0.6324(5) 0.4090(4) 0.1047(4) 0.0350(12) Uani 1 1 d . . . . .
H16 H 0.5989 0.3399 0.1070 0.042 Uiso 1 1 calc R U . . .
C17 C 0.6688(5) 0.4821(4) 0.1853(4) 0.0311(11) Uani 1 1 d . . . . .
C18 C 0.6639(6) 0.4712(5) 0.2940(4) 0.0434(14) Uani 1 1 d . . . . .
H18A H 0.6962 0.5365 0.3333 0.065 Uiso 1 1 calc R U . . .
H18B H 0.7138 0.4103 0.3077 0.065 Uiso 1 1 calc R U . . .
H18C H 0.5787 0.4598 0.3120 0.065 Uiso 1 1 calc R U . . .
C19 C 0.9768(6) 0.5852(6) -0.1481(4) 0.0567(18) Uani 1 1 d . . . . .
H19A H 0.8920 0.5633 -0.1663 0.085 Uiso 1 1 calc R U . . .
H19B H 1.0280 0.5217 -0.1478 0.085 Uiso 1 1 calc R U . . .
H19C H 1.0081 0.6289 -0.1967 0.085 Uiso 1 1 calc R U . . .
C20 C 0.9803(5) 0.6491(4) -0.0465(4) 0.0366(13) Uani 1 1 d . . . . .
C21 C 1.0804(5) 0.6972(5) 0.0060(4) 0.0388(13) Uani 1 1 d . . . . .
H21 H 1.1625 0.6990 -0.0161 0.047 Uiso 1 1 calc R U . . .
C22 C 1.0367(5) 0.7422(4) 0.0973(4) 0.0323(12) Uani 1 1 d . . . . .
C23 C 1.1068(5) 0.8029(5) 0.1821(5) 0.0478(15) Uani 1 1 d . . . . .
H23A H 1.0511 0.8244 0.2369 0.072 Uiso 1 1 calc R U . . .
H23B H 1.1436 0.8666 0.1605 0.072 Uiso 1 1 calc R U . . .
H23C H 1.1717 0.7578 0.2047 0.072 Uiso 1 1 calc R U . . .
C24 C 0.6204(6) 0.7616(5) -0.1730(4) 0.0425(14) Uani 1 1 d . . . . .
H24A H 0.6812 0.7048 -0.1859 0.064 Uiso 1 1 calc R U . . .
H24B H 0.6498 0.8259 -0.1986 0.064 Uiso 1 1 calc R U . . .
H24C H 0.5424 0.7382 -0.2063 0.064 Uiso 1 1 calc R U . . .
C25 C 0.6018(5) 0.7860(4) -0.0631(4) 0.0295(11) Uani 1 1 d . . . . .
C26 C 0.5236(5) 0.8595(4) -0.0137(4) 0.0326(12) Uani 1 1 d . . . . .
H26 H 0.4675 0.9042 -0.0429 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5432(5) 0.8552(4) 0.0870(4) 0.0274(11) Uani 1 1 d . . . . .
C28 C 0.4815(5) 0.9176(5) 0.1732(4) 0.0403(13) Uani 1 1 d . . . . .
H28A H 0.5149 0.8968 0.2355 0.060 Uiso 1 1 calc R U . . .
H28B H 0.3930 0.9029 0.1685 0.060 Uiso 1 1 calc R U . . .
H28C H 0.4961 0.9939 0.1723 0.060 Uiso 1 1 calc R U . . .
B1 B 0.7444(6) 0.6378(5) -0.0134(5) 0.0312(13) Uani 1 1 d . . . . .
N1 N 0.7015(4) 0.5542(3) 0.0503(3) 0.0273(9) Uani 1 1 d . . . . .
N2 N 0.7110(4) 0.5722(3) 0.1532(3) 0.0294(9) Uani 1 1 d . . . . .
N3 N 0.8822(4) 0.6667(3) 0.0107(3) 0.0301(10) Uani 1 1 d . . . . .
N4 N 0.9163(4) 0.7236(4) 0.1013(3) 0.0312(10) Uani 1 1 d . . . . .
N5 N 0.6637(4) 0.7383(3) 0.0050(3) 0.0267(9) Uani 1 1 d . . . . .
N6 N 0.6307(4) 0.7810(3) 0.0995(3) 0.0282(9) Uani 1 1 d . . . . .
Si1 Si 1.05613(17) 0.69962(14) 0.44498(13) 0.0460(4) Uani 1 1 d . . . . .
Si2 Si 0.59708(16) 0.77880(15) 0.50123(12) 0.0443(4) Uani 1 1 d . . . . .
Si3 Si 0.86063(13) 1.04730(12) 0.19201(11) 0.0317(3) Uani 1 1 d . . . . .
Th1 Th 0.77289(2) 0.75411(2) 0.25480(2) 0.02663(8) Uani 1 1 d . . . . .
H1B1 H 0.731(5) 0.614(4) -0.088(4) 0.036(15) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Si1 1.851(6) . ?
C1 Th1 2.480(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 Si2 1.846(6) . ?
C2 Th1 2.493(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 Si3 1.856(5) . ?
C3 Th1 2.466(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 Si1 1.859(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si1 1.874(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Si1 1.879(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 Si2 1.864(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 Si2 1.885(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 Si2 1.871(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si3 1.857(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 Si3 1.876(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 Si3 1.874(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.492(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N1 1.351(6) . ?
C15 C16 1.381(7) . ?
C16 C17 1.384(7) . ?
C16 H16 0.9500 . ?
C17 N2 1.354(6) . ?
C17 C18 1.501(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.501(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N3 1.335(7) . ?
C20 C21 1.382(8) . ?
C21 C22 1.387(8) . ?
C21 H21 0.9500 . ?
C22 N4 1.334(7) . ?
C22 C23 1.489(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.499(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N5 1.340(6) . ?
C25 C26 1.379(8) . ?
C26 C27 1.386(7) . ?
C26 H26 0.9500 . ?
C27 N6 1.364(6) . ?
C27 C28 1.494(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
B1 N1 1.530(7) . ?
B1 N5 1.544(7) . ?
B1 N3 1.561(8) . ?
B1 H1B1 1.02(5) . ?
N1 N2 1.385(5) . ?
N2 Th1 2.597(4) . ?
N3 N4 1.381(6) . ?
N4 Th1 2.618(4) . ?
N5 N6 1.378(5) . ?
N6 Th1 2.647(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1 C1 Th1 141.9(3) . . ?
Si1 C1 H1A 101.5 . . ?
Th1 C1 H1A 101.5 . . ?
Si1 C1 H1B 101.5 . . ?
Th1 C1 H1B 101.5 . . ?
H1A C1 H1B 104.6 . . ?
Si2 C2 Th1 125.2(3) . . ?
Si2 C2 H2A 106.0 . . ?
Th1 C2 H2A 106.0 . . ?
Si2 C2 H2B 106.0 . . ?
Th1 C2 H2B 106.0 . . ?
H2A C2 H2B 106.3 . . ?
Si3 C3 Th1 137.1(3) . . ?
Si3 C3 H3A 102.9 . . ?
Th1 C3 H3A 102.9 . . ?
Si3 C3 H3B 102.9 . . ?
Th1 C3 H3B 102.9 . . ?
H3A C3 H3B 105.0 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C16 107.6(5) . . ?
N1 C15 C14 123.5(5) . . ?
C16 C15 C14 128.9(5) . . ?
C15 C16 C17 106.7(5) . . ?
C15 C16 H16 126.7 . . ?
C17 C16 H16 126.7 . . ?
N2 C17 C16 109.9(5) . . ?
N2 C17 C18 121.7(5) . . ?
C16 C17 C18 128.3(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 C21 107.8(5) . . ?
N3 C20 C19 123.8(5) . . ?
C21 C20 C19 128.3(5) . . ?
C20 C21 C22 106.0(5) . . ?
C20 C21 H21 127.0 . . ?
C22 C21 H21 127.0 . . ?
N4 C22 C21 109.9(5) . . ?
N4 C22 C23 122.0(5) . . ?
C21 C22 C23 128.1(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 C26 108.1(4) . . ?
N5 C25 C24 123.8(5) . . ?
C26 C25 C24 128.1(5) . . ?
C25 C26 C27 106.4(5) . . ?
C25 C26 H26 126.8 . . ?
C27 C26 H26 126.8 . . ?
N6 C27 C26 109.4(5) . . ?
N6 C27 C28 122.1(5) . . ?
C26 C27 C28 128.5(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 B1 N5 110.1(4) . . ?
N1 B1 N3 110.0(4) . . ?
N5 B1 N3 110.6(4) . . ?
N1 B1 H1B1 113(3) . . ?
N5 B1 H1B1 103(3) . . ?
N3 B1 H1B1 111(3) . . ?
C15 N1 N2 110.0(4) . . ?
C15 N1 B1 128.7(4) . . ?
N2 N1 B1 121.3(4) . . ?
C17 N2 N1 105.9(4) . . ?
C17 N2 Th1 129.6(3) . . ?
N1 N2 Th1 124.2(3) . . ?
C20 N3 N4 109.9(4) . . ?
C20 N3 B1 129.8(5) . . ?
N4 N3 B1 120.2(4) . . ?
C22 N4 N3 106.4(4) . . ?
C22 N4 Th1 128.9(3) . . ?
N3 N4 Th1 123.9(3) . . ?
C25 N5 N6 110.1(4) . . ?
C25 N5 B1 127.4(4) . . ?
N6 N5 B1 121.7(4) . . ?
C27 N6 N5 105.9(4) . . ?
C27 N6 Th1 131.3(3) . . ?
N5 N6 Th1 120.1(3) . . ?
C1 Si1 C5 112.6(3) . . ?
C1 Si1 C6 110.3(4) . . ?
C5 Si1 C6 108.6(4) . . ?
C1 Si1 C7 110.4(3) . . ?
C5 Si1 C7 107.4(3) . . ?
C6 Si1 C7 107.4(4) . . ?
C2 Si2 C8 110.7(3) . . ?
C2 Si2 C10 109.7(3) . . ?
C8 Si2 C10 109.2(4) . . ?
C2 Si2 C9 113.1(3) . . ?
C8 Si2 C9 108.2(4) . . ?
C10 Si2 C9 105.9(4) . . ?
C3 Si3 C11 110.7(3) . . ?
C3 Si3 C13 112.4(3) . . ?
C11 Si3 C13 106.9(3) . . ?
C3 Si3 C12 112.7(3) . . ?
C11 Si3 C12 106.0(3) . . ?
C13 Si3 C12 107.7(3) . . ?
C3 Th1 C1 106.92(18) . . ?
C3 Th1 C2 98.5(2) . . ?
C1 Th1 C2 100.9(2) . . ?
C3 Th1 N2 154.21(16) . . ?
C1 Th1 N2 91.93(16) . . ?
C2 Th1 N2 94.87(18) . . ?
C3 Th1 N4 89.30(16) . . ?
C1 Th1 N4 90.60(18) . . ?
C2 Th1 N4 163.43(16) . . ?
N2 Th1 N4 72.70(13) . . ?
C3 Th1 N6 89.02(15) . . ?
C1 Th1 N6 158.43(17) . . ?
C2 Th1 N6 90.65(16) . . ?
N2 Th1 N6 68.80(13) . . ?
N4 Th1 N6 74.81(13) . . ?

_refine_diff_density_max         0.853
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.191
