# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1832389'
_audit_update_record             
;
2018-03-26 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H76 B2 O2 Pb Si8'
_chemical_formula_sum            'C28 H76 B2 O2 Pb Si8'
_chemical_formula_weight         898.41
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.147(6)
_cell_length_b                   18.137(4)
_cell_length_c                   23.271(6)
_cell_angle_alpha                90
_cell_angle_beta                 118.845(8)
_cell_angle_gamma                90
_cell_volume                     9297(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9776
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.52
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.490
_exptl_crystal_size_min          0.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3712
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_T_max  0.259

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0673
_diffrn_reflns_av_uneti/neti     0.0750
_diffrn_reflns_number            30996
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.974
_reflns_number_total             10368
_reflns_number_gt                7238
_reflns_threshold_expression     >2sigma(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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+325.6818P] 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         10368
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1494
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         4.689
_refine_diff_density_min         -4.867
_refine_diff_density_rms         0.184

#...............................................................................
# .RES SHELXL file: job.res
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file .............................................
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.32173(2) 0.26352(2) 0.31791(2) 0.04189(14) Uani 1 1 d . . . . .
Si1 Si 0.26088(10) 0.35939(15) 0.13927(12) 0.0297(6) Uani 1 1 d . . . . .
Si2 Si 0.25650(10) 0.49953(14) 0.36028(12) 0.0257(5) Uani 1 1 d . . . . .
Si3 Si 0.14399(9) 0.41633(13) 0.24705(12) 0.0244(5) Uani 1 1 d . . . . .
Si4 Si 0.31747(10) 0.51620(14) 0.19827(12) 0.0276(5) Uani 1 1 d . . . . .
O1 O 0.3004(2) 0.3736(3) 0.2956(3) 0.0250(13) Uani 1 1 d . . . . .
B2 B 0.2611(3) 0.4244(5) 0.2541(4) 0.0194(19) Uani 1 1 d . . . . .
C3 C 0.2174(3) 0.4670(4) 0.2731(4) 0.0201(16) Uani 1 1 d . . . . .
H3 H 0.206056 0.512066 0.246562 0.024 Uiso 1 1 calc R U . . .
C4 C 0.2540(5) 0.4315(7) 0.4185(5) 0.046(3) Uani 1 1 d . . . . .
H4A H 0.212532 0.423067 0.407924 0.069 Uiso 1 1 calc R U . . .
H4B H 0.276218 0.450289 0.462438 0.069 Uiso 1 1 calc R U . . .
H4C H 0.271827 0.385954 0.415350 0.069 Uiso 1 1 calc R U . . .
C5 C 0.3390(4) 0.5188(6) 0.3901(5) 0.038(2) Uani 1 1 d . . . . .
H5A H 0.357956 0.533875 0.435180 0.057 Uiso 1 1 calc R U . . .
H5B H 0.342916 0.557341 0.364084 0.057 Uiso 1 1 calc R U . . .
H5C H 0.358448 0.474920 0.386173 0.057 Uiso 1 1 calc R U . . .
C6 C 0.2199(5) 0.5873(6) 0.3650(6) 0.048(3) Uani 1 1 d . . . . .
H6A H 0.180146 0.576867 0.359161 0.072 Uiso 1 1 calc R U . . .
H6B H 0.216610 0.620293 0.331251 0.072 Uiso 1 1 calc R U . . .
H6C H 0.244141 0.609687 0.407175 0.072 Uiso 1 1 calc R U . . .
C7 C 0.0944(4) 0.4612(6) 0.2756(5) 0.041(3) Uani 1 1 d . . . . .
H7A H 0.085988 0.510925 0.259624 0.061 Uiso 1 1 calc R U . . .
H7B H 0.114633 0.461471 0.322699 0.061 Uiso 1 1 calc R U . . .
H7C H 0.057030 0.434264 0.259264 0.061 Uiso 1 1 calc R U . . .
C8 C 0.0989(4) 0.4154(6) 0.1557(5) 0.041(2) Uani 1 1 d . . . . .
H8A H 0.061672 0.388891 0.142425 0.061 Uiso 1 1 calc R U . . .
H8B H 0.121858 0.391615 0.137909 0.061 Uiso 1 1 calc R U . . .
H8C H 0.089811 0.465069 0.139661 0.061 Uiso 1 1 calc R U . . .
C9 C 0.1568(4) 0.3185(5) 0.2767(5) 0.040(2) Uani 1 1 d . . . . .
H9A H 0.180068 0.317841 0.323674 0.059 Uiso 1 1 calc R U . . .
H9B H 0.178589 0.292701 0.258464 0.059 Uiso 1 1 calc R U . . .
H9C H 0.118413 0.294903 0.263020 0.059 Uiso 1 1 calc R U . . .
C10 C 0.2606(3) 0.4423(5) 0.1872(4) 0.0229(17) Uani 1 1 d . . . . .
H10 H 0.221029 0.465413 0.159849 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3381(4) 0.3175(6) 0.1720(5) 0.039(2) Uani 1 1 d . . . . .
H11A H 0.335016 0.271657 0.149966 0.059 Uiso 1 1 calc R U . . .
H11B H 0.354915 0.308667 0.218233 0.059 Uiso 1 1 calc R U . . .
H11C H 0.364017 0.350590 0.164699 0.059 Uiso 1 1 calc R U . . .
C12 C 0.2086(4) 0.2859(6) 0.1383(6) 0.048(3) Uani 1 1 d . . . . .
H12A H 0.167288 0.301910 0.112356 0.071 Uiso 1 1 calc R U . . .
H12B H 0.216604 0.276174 0.182304 0.071 Uiso 1 1 calc R U . . .
H12C H 0.214862 0.241675 0.119649 0.071 Uiso 1 1 calc R U . . .
C13 C 0.2320(5) 0.3817(8) 0.0516(5) 0.059(4) Uani 1 1 d . . . . .
H13A H 0.193446 0.405986 0.034746 0.089 Uiso 1 1 calc R U . . .
H13B H 0.227315 0.337020 0.027477 0.089 Uiso 1 1 calc R U . . .
H13C H 0.260276 0.413559 0.047185 0.089 Uiso 1 1 calc R U . . .
C14 C 0.3210(6) 0.5373(7) 0.1226(6) 0.058(3) Uani 1 1 d . . . . .
H14A H 0.280897 0.547953 0.087757 0.087 Uiso 1 1 calc R U . . .
H14B H 0.337136 0.495617 0.110704 0.087 Uiso 1 1 calc R U . . .
H14C H 0.346701 0.579303 0.129912 0.087 Uiso 1 1 calc R U . . .
C15 C 0.2943(4) 0.6048(5) 0.2214(5) 0.035(2) Uani 1 1 d . . . . .
H15A H 0.322912 0.642737 0.226675 0.053 Uiso 1 1 calc R U . . .
H15B H 0.293421 0.598266 0.261875 0.053 Uiso 1 1 calc R U . . .
H15C H 0.254644 0.618749 0.187471 0.053 Uiso 1 1 calc R U . . .
C16 C 0.3958(4) 0.4921(6) 0.2631(5) 0.039(2) Uani 1 1 d . . . . .
H16A H 0.412121 0.454621 0.246875 0.058 Uiso 1 1 calc R U . . .
H16B H 0.394515 0.474097 0.301179 0.058 Uiso 1 1 calc R U . . .
H16C H 0.421086 0.535147 0.274514 0.058 Uiso 1 1 calc R U . . .
Si11 Si 0.53518(9) 0.33432(13) 0.42332(11) 0.0221(5) Uani 1 1 d . . . . .
Si12 Si 0.51714(10) 0.16201(13) 0.40569(13) 0.0279(5) Uani 1 1 d . . . . .
Si13 Si 0.46936(11) 0.29535(14) 0.57840(12) 0.0286(5) Uani 1 1 d . . . . .
Si14 Si 0.38278(10) 0.16250(13) 0.49810(13) 0.0272(5) Uani 1 1 d . . . . .
O21 O 0.4035(2) 0.2825(3) 0.4036(3) 0.0234(12) Uani 1 1 d . . . . .
B22 B 0.4529(4) 0.2505(5) 0.4533(4) 0.0200(18) Uani 1 1 d . . . . .
C23 C 0.5144(3) 0.2461(4) 0.4498(4) 0.0206(17) Uani 1 1 d . . . . .
H23 H 0.546193 0.238792 0.495332 0.025 Uiso 1 1 calc R U . . .
C24 C 0.4461(4) 0.1511(6) 0.3252(5) 0.043(3) Uani 1 1 d . . . . .
H24A H 0.413052 0.138235 0.332866 0.065 Uiso 1 1 calc R U . . .
H24B H 0.451850 0.112743 0.300225 0.065 Uiso 1 1 calc R U . . .
H24C H 0.437139 0.196574 0.301251 0.065 Uiso 1 1 calc R U . . .
C25 C 0.5813(5) 0.1591(6) 0.3877(6) 0.048(3) Uani 1 1 d . . . . .
H25A H 0.575320 0.195829 0.355427 0.072 Uiso 1 1 calc R U . . .
H25B H 0.583242 0.111257 0.371279 0.072 Uiso 1 1 calc R U . . .
H25C H 0.618532 0.168862 0.427185 0.072 Uiso 1 1 calc R U . . .
C26 C 0.5279(5) 0.0797(5) 0.4584(6) 0.046(3) Uani 1 1 d . . . . .
H26A H 0.567537 0.081451 0.496211 0.069 Uiso 1 1 calc R U . . .
H26B H 0.524206 0.035636 0.433859 0.069 Uiso 1 1 calc R U . . .
H26C H 0.497610 0.079662 0.472216 0.069 Uiso 1 1 calc R U . . .
C27 C 0.6202(4) 0.3415(5) 0.4660(5) 0.034(2) Uani 1 1 d . . . . .
H27A H 0.636525 0.302525 0.451232 0.051 Uiso 1 1 calc R U . . .
H27B H 0.635882 0.337519 0.512494 0.051 Uiso 1 1 calc R U . . .
H27C H 0.631751 0.388270 0.455948 0.051 Uiso 1 1 calc R U . . .
C28 C 0.5052(4) 0.4177(5) 0.4446(5) 0.035(2) Uani 1 1 d . . . . .
H28A H 0.517192 0.460960 0.430001 0.052 Uiso 1 1 calc R U . . .
H28B H 0.521193 0.419943 0.491265 0.052 Uiso 1 1 calc R U . . .
H28C H 0.461682 0.415149 0.423481 0.052 Uiso 1 1 calc R U . . .
C29 C 0.5059(4) 0.3392(5) 0.3332(4) 0.036(2) Uani 1 1 d . . . . .
H29A H 0.462459 0.335625 0.310983 0.054 Uiso 1 1 calc R U . . .
H29B H 0.522489 0.299211 0.319826 0.054 Uiso 1 1 calc R U . . .
H29C H 0.517774 0.385214 0.322410 0.054 Uiso 1 1 calc R U . . .
C30 C 0.4508(3) 0.2200(4) 0.5163(4) 0.0209(17) Uani 1 1 d . . . . .
H30 H 0.485213 0.185826 0.536713 0.025 Uiso 1 1 calc R U . . .
C31 C 0.4208(4) 0.3774(5) 0.5427(5) 0.040(2) Uani 1 1 d . . . . .
H31A H 0.421961 0.392138 0.503780 0.060 Uiso 1 1 calc R U . . .
H31B H 0.435322 0.416913 0.574035 0.060 Uiso 1 1 calc R U . . .
H31C H 0.379750 0.365614 0.531919 0.060 Uiso 1 1 calc R U . . .
C32 C 0.5513(4) 0.3209(6) 0.6119(5) 0.041(2) Uani 1 1 d . . . . .
H32A H 0.576235 0.278333 0.631468 0.062 Uiso 1 1 calc R U . . .
H32B H 0.561789 0.358802 0.644384 0.062 Uiso 1 1 calc R U . . .
H32C H 0.557810 0.338686 0.576900 0.062 Uiso 1 1 calc R U . . .
C33 C 0.4610(6) 0.2657(7) 0.6497(5) 0.057(3) Uani 1 1 d . . . . .
H33A H 0.418692 0.260017 0.636574 0.086 Uiso 1 1 calc R U . . .
H33B H 0.478514 0.302127 0.683725 0.086 Uiso 1 1 calc R U . . .
H33C H 0.481424 0.219434 0.665825 0.086 Uiso 1 1 calc R U . . .
C34 C 0.3977(5) 0.1042(6) 0.5698(6) 0.046(3) Uani 1 1 d . . . . .
H34A H 0.438220 0.085011 0.589010 0.069 Uiso 1 1 calc R U . . .
H34B H 0.369220 0.064141 0.555870 0.069 Uiso 1 1 calc R U . . .
H34C H 0.393254 0.133376 0.601703 0.069 Uiso 1 1 calc R U . . .
C35 C 0.3122(4) 0.2175(6) 0.4744(7) 0.051(3) Uani 1 1 d . . . . .
H35A H 0.279179 0.184675 0.465734 0.077 Uiso 1 1 calc R U . . .
H35B H 0.302650 0.245753 0.435794 0.077 Uiso 1 1 calc R U . . .
H35C H 0.318575 0.250104 0.509668 0.077 Uiso 1 1 calc R U . . .
C36 C 0.3655(4) 0.0947(5) 0.4308(5) 0.036(2) Uani 1 1 d . . . . .
H36A H 0.399802 0.062754 0.443207 0.054 Uiso 1 1 calc R U . . .
H36B H 0.357226 0.120661 0.391391 0.054 Uiso 1 1 calc R U . . .
H36C H 0.330737 0.065905 0.423280 0.054 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.067(6) . ?
Pb1 O21 2.089(5) . ?
Si1 C13 1.850(11) . ?
Si1 C12 1.865(11) . ?
Si1 C11 1.872(9) . ?
Si1 C10 1.874(9) . ?
Si2 C4 1.857(11) . ?
Si2 C6 1.868(10) . ?
Si2 C3 1.872(8) . ?
Si2 C5 1.877(9) . ?
Si3 C7 1.859(10) . ?
Si3 C8 1.866(10) . ?
Si3 C9 1.874(9) . ?
Si3 C3 1.882(8) . ?
Si4 C14 1.846(13) . ?
Si4 C16 1.865(9) . ?
Si4 C15 1.874(10) . ?
Si4 C10 1.885(8) . ?
O1 B2 1.356(10) . ?
B2 C3 1.573(12) . ?
B2 C10 1.584(13) . ?
C3 H3 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
Si11 C28 1.860(9) . ?
Si11 C29 1.859(9) . ?
Si11 C27 1.878(8) . ?
Si11 C23 1.878(8) . ?
Si12 C25 1.852(11) . ?
Si12 C23 1.858(8) . ?
Si12 C26 1.867(10) . ?
Si12 C24 1.873(9) . ?
Si13 C31 1.848(10) . ?
Si13 C33 1.851(12) . ?
Si13 C32 1.876(9) . ?
Si13 C30 1.877(9) . ?
Si14 C34 1.855(11) . ?
Si14 C30 1.870(8) . ?
Si14 C35 1.872(10) . ?
Si14 C36 1.870(10) . ?
O21 B22 1.353(10) . ?
B22 C23 1.590(11) . ?
B22 C30 1.591(12) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O21 95.6(2) . . ?
C13 Si1 C12 104.1(6) . . ?
C13 Si1 C11 108.4(5) . . ?
C12 Si1 C11 107.6(5) . . ?
C13 Si1 C10 111.6(5) . . ?
C12 Si1 C10 112.1(4) . . ?
C11 Si1 C10 112.6(4) . . ?
C4 Si2 C6 109.4(6) . . ?
C4 Si2 C3 113.4(4) . . ?
C6 Si2 C3 108.4(4) . . ?
C4 Si2 C5 106.0(5) . . ?
C6 Si2 C5 108.0(5) . . ?
C3 Si2 C5 111.6(4) . . ?
C7 Si3 C8 105.5(5) . . ?
C7 Si3 C9 108.0(5) . . ?
C8 Si3 C9 108.2(5) . . ?
C7 Si3 C3 113.2(4) . . ?
C8 Si3 C3 109.6(4) . . ?
C9 Si3 C3 112.1(4) . . ?
C14 Si4 C16 107.6(5) . . ?
C14 Si4 C15 105.1(5) . . ?
C16 Si4 C15 108.8(5) . . ?
C14 Si4 C10 113.5(5) . . ?
C16 Si4 C10 112.3(4) . . ?
C15 Si4 C10 109.2(4) . . ?
B2 O1 Pb1 147.9(5) . . ?
O1 B2 C3 120.2(8) . . ?
O1 B2 C10 119.8(7) . . ?
C3 B2 C10 120.0(7) . . ?
B2 C3 Si2 112.7(5) . . ?
B2 C3 Si3 112.3(5) . . ?
Si2 C3 Si3 115.1(4) . . ?
B2 C3 H3 105.2 . . ?
Si2 C3 H3 105.2 . . ?
Si3 C3 H3 105.2 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si3 C7 H7A 109.5 . . ?
Si3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si3 C8 H8A 109.5 . . ?
Si3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
B2 C10 Si1 114.8(6) . . ?
B2 C10 Si4 111.4(5) . . ?
Si1 C10 Si4 115.6(4) . . ?
B2 C10 H10 104.5 . . ?
Si1 C10 H10 104.5 . . ?
Si4 C10 H10 104.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C28 Si11 C29 105.7(4) . . ?
C28 Si11 C27 107.9(4) . . ?
C29 Si11 C27 108.8(4) . . ?
C28 Si11 C23 113.1(4) . . ?
C29 Si11 C23 112.9(4) . . ?
C27 Si11 C23 108.2(4) . . ?
C25 Si12 C23 114.6(4) . . ?
C25 Si12 C26 105.0(5) . . ?
C23 Si12 C26 109.0(5) . . ?
C25 Si12 C24 106.6(5) . . ?
C23 Si12 C24 111.6(4) . . ?
C26 Si12 C24 109.8(5) . . ?
C31 Si13 C33 107.5(6) . . ?
C31 Si13 C32 110.1(5) . . ?
C33 Si13 C32 106.1(5) . . ?
C31 Si13 C30 112.1(4) . . ?
C33 Si13 C30 112.7(5) . . ?
C32 Si13 C30 108.3(4) . . ?
C34 Si14 C30 110.4(4) . . ?
C34 Si14 C35 108.6(6) . . ?
C30 Si14 C35 113.8(4) . . ?
C34 Si14 C36 104.1(5) . . ?
C30 Si14 C36 111.9(4) . . ?
C35 Si14 C36 107.5(5) . . ?
B22 O21 Pb1 145.1(5) . . ?
O21 B22 C23 119.5(7) . . ?
O21 B22 C30 120.8(7) . . ?
C23 B22 C30 119.6(7) . . ?
B22 C23 Si12 111.5(5) . . ?
B22 C23 Si11 113.9(5) . . ?
Si12 C23 Si11 115.3(4) . . ?
B22 C23 H23 105.0 . . ?
Si12 C23 H23 105.0 . . ?
Si11 C23 H23 105.0 . . ?
Si12 C24 H24A 109.5 . . ?
Si12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si12 C25 H25A 109.5 . . ?
Si12 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si12 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si12 C26 H26A 109.5 . . ?
Si12 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si12 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si11 C27 H27A 109.5 . . ?
Si11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si11 C28 H28A 109.5 . . ?
Si11 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si11 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si11 C29 H29A 109.5 . . ?
Si11 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si11 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
B22 C30 Si14 114.7(5) . . ?
B22 C30 Si13 110.5(5) . . ?
Si14 C30 Si13 116.1(4) . . ?
B22 C30 H30 104.7 . . ?
Si14 C30 H30 104.7 . . ?
Si13 C30 H30 104.7 . . ?
Si13 C31 H31A 109.5 . . ?
Si13 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si13 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si13 C32 H32A 109.5 . . ?
Si13 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si13 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si13 C33 H33A 109.5 . . ?
Si13 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si13 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si14 C34 H34A 109.5 . . ?
Si14 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si14 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si14 C35 H35A 109.5 . . ?
Si14 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si14 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si14 C36 H36A 109.5 . . ?
Si14 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si14 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 B2 C3 103.8(11) . . . . ?
Pb1 O1 B2 C10 -77.8(12) . . . . ?
O1 B2 C3 Si2 44.0(9) . . . . ?
C10 B2 C3 Si2 -134.3(6) . . . . ?
O1 B2 C3 Si3 -88.0(7) . . . . ?
C10 B2 C3 Si3 93.7(7) . . . . ?
C4 Si2 C3 B2 -90.0(7) . . . . ?
C6 Si2 C3 B2 148.3(6) . . . . ?
C5 Si2 C3 B2 29.5(7) . . . . ?
C4 Si2 C3 Si3 40.6(6) . . . . ?
C6 Si2 C3 Si3 -81.1(6) . . . . ?
C5 Si2 C3 Si3 160.1(5) . . . . ?
C7 Si3 C3 B2 174.7(6) . . . . ?
C8 Si3 C3 B2 -67.8(7) . . . . ?
C9 Si3 C3 B2 52.3(7) . . . . ?
C7 Si3 C3 Si2 43.9(6) . . . . ?
C8 Si3 C3 Si2 161.4(5) . . . . ?
C9 Si3 C3 Si2 -78.5(6) . . . . ?
O1 B2 C10 Si1 46.6(8) . . . . ?
C3 B2 C10 Si1 -135.0(6) . . . . ?
O1 B2 C10 Si4 -87.2(8) . . . . ?
C3 B2 C10 Si4 91.2(7) . . . . ?
C13 Si1 C10 B2 158.8(6) . . . . ?
C12 Si1 C10 B2 42.5(7) . . . . ?
C11 Si1 C10 B2 -79.0(7) . . . . ?
C13 Si1 C10 Si4 -69.4(6) . . . . ?
C12 Si1 C10 Si4 174.3(5) . . . . ?
C11 Si1 C10 Si4 52.9(6) . . . . ?
C14 Si4 C10 B2 178.0(6) . . . . ?
C16 Si4 C10 B2 55.7(7) . . . . ?
C15 Si4 C10 B2 -65.1(6) . . . . ?
C14 Si4 C10 Si1 44.5(6) . . . . ?
C16 Si4 C10 Si1 -77.8(6) . . . . ?
C15 Si4 C10 Si1 161.4(4) . . . . ?
Pb1 O21 B22 C23 98.4(10) . . . . ?
Pb1 O21 B22 C30 -83.8(11) . . . . ?
O21 B22 C23 Si12 -87.3(8) . . . . ?
C30 B22 C23 Si12 94.9(7) . . . . ?
O21 B22 C23 Si11 45.3(9) . . . . ?
C30 B22 C23 Si11 -132.5(6) . . . . ?
C25 Si12 C23 B22 170.9(6) . . . . ?
C26 Si12 C23 B22 -71.8(6) . . . . ?
C24 Si12 C23 B22 49.6(7) . . . . ?
C25 Si12 C23 Si11 39.0(6) . . . . ?
C26 Si12 C23 Si11 156.4(4) . . . . ?
C24 Si12 C23 Si11 -82.2(5) . . . . ?
C28 Si11 C23 B22 27.9(7) . . . . ?
C29 Si11 C23 B22 -92.2(6) . . . . ?
C27 Si11 C23 B22 147.3(6) . . . . ?
C28 Si11 C23 Si12 158.6(4) . . . . ?
C29 Si11 C23 Si12 38.6(5) . . . . ?
C27 Si11 C23 Si12 -81.9(5) . . . . ?
O21 B22 C30 Si14 47.0(10) . . . . ?
C23 B22 C30 Si14 -135.2(6) . . . . ?
O21 B22 C30 Si13 -86.5(8) . . . . ?
C23 B22 C30 Si13 91.2(7) . . . . ?
C34 Si14 C30 B22 159.9(6) . . . . ?
C35 Si14 C30 B22 -77.6(8) . . . . ?
C36 Si14 C30 B22 44.5(7) . . . . ?
C34 Si14 C30 Si13 -69.2(6) . . . . ?
C35 Si14 C30 Si13 53.2(7) . . . . ?
C36 Si14 C30 Si13 175.3(4) . . . . ?
C31 Si13 C30 B22 53.5(7) . . . . ?
C33 Si13 C30 B22 174.8(6) . . . . ?
C32 Si13 C30 B22 -68.2(6) . . . . ?
C31 Si13 C30 Si14 -79.4(6) . . . . ?
C33 Si13 C30 Si14 41.9(6) . . . . ?
C32 Si13 C30 Si14 159.0(5) . . . . ?

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR SAA9                                                   #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1832390'
_audit_update_record             
;
2018-03-26 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;


#----------------------------------------------------------------------------#
#                              CHEMICAL_INFORMATION                          #
#----------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H76 B2 O2 Si8 Sn'
_chemical_formula_sum            'C28 H76 B2 O2 Si8 Sn'
_chemical_formula_weight         809.91
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                             UNIT CELL INFORMATION                          #
#----------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.1738(8)
_cell_length_b                   18.1907(6)
_cell_length_c                   24.6824(7)
_cell_angle_alpha                90
_cell_angle_beta                 123.9170(10)
_cell_angle_gamma                90
_cell_volume                     9379.6(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.46
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                              CRYSTAL INFORMATION                           #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3456
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                             ABSORPTION CORRECTION                          #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  0.775

#----------------------------------------------------------------------------#
#                                DATA COLLECTION                             #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0617
_diffrn_reflns_av_uneti/neti     0.0488
_diffrn_reflns_number            42335
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.970
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             10742
_reflns_number_gt                8081
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                             COMPUTER PROGRAMS USED                         #
#----------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2014)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2016)'

#----------------------------------------------------------------------------#
#                             REFINEMENT INFORMATION                         #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+26.9267P] 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         10742
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.423
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.082

#...............................................................................
# .RES SHELXL file: SAA24.res
# .HKL SHELXL file: SAA24.hkl
#...............................................................................



# ............... End of .HKL file .............................................
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS            #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Sn1 Sn 0.74837(2) 0.51816(2) 0.32213(2) 0.02990(7) Uani 1 1 d . . . . .
O1 O 0.75013(9) 0.53314(10) 0.40263(8) 0.0195(4) Uani 1 1 d . . . . .
O2 O 0.74447(8) 0.62242(10) 0.29819(8) 0.0189(4) Uani 1 1 d . . . . .
B1 B 0.75085(14) 0.50091(15) 0.45308(14) 0.0155(6) Uani 1 1 d . . . . .
B2 B 0.74233(14) 0.67300(16) 0.25631(13) 0.0148(6) Uani 1 1 d . . . . .
Si1 Si 0.63764(3) 0.58371(4) 0.42321(3) 0.01763(15) Uani 1 1 d . . . . .
Si2 Si 0.63948(4) 0.41103(4) 0.40642(4) 0.02367(17) Uani 1 1 d . . . . .
Si3 Si 0.86623(4) 0.41185(4) 0.49830(4) 0.02259(17) Uani 1 1 d . . . . .
Si4 Si 0.85918(4) 0.54494(5) 0.57824(4) 0.02402(17) Uani 1 1 d . . . . .
Si5 Si 0.63090(4) 0.76535(4) 0.20136(4) 0.02307(17) Uani 1 1 d . . . . .
Si6 Si 0.62829(4) 0.60931(5) 0.14067(4) 0.02477(18) Uani 1 1 d . . . . .
Si7 Si 0.85501(4) 0.74781(4) 0.36320(4) 0.02194(16) Uani 1 1 d . . . . .
Si8 Si 0.85256(4) 0.66581(4) 0.24814(4) 0.02109(16) Uani 1 1 d . . . . .
C1 C 0.68608(12) 0.49641(14) 0.45015(12) 0.0161(5) Uani 1 1 d . . . . .
H1 H 0.700013 0.489295 0.496478 0.019 Uiso 1 1 calc R U . . .
C2 C 0.68839(14) 0.66734(16) 0.44429(14) 0.0282(6) Uani 1 1 d . . . . .
H2A H 0.712760 0.664032 0.424312 0.042 Uiso 1 1 calc R U . . .
H2B H 0.718064 0.670868 0.491816 0.042 Uiso 1 1 calc R U . . .
H2C H 0.661034 0.711086 0.427809 0.042 Uiso 1 1 calc R U . . .
C3 C 0.59591(14) 0.59016(18) 0.46664(14) 0.0286(7) Uani 1 1 d . . . . .
H3A H 0.627586 0.587426 0.513884 0.043 Uiso 1 1 calc R U . . .
H3B H 0.565492 0.549434 0.452896 0.043 Uiso 1 1 calc R U . . .
H3C H 0.572872 0.636983 0.455812 0.043 Uiso 1 1 calc R U . . .
C4 C 0.57636(14) 0.58719(17) 0.33296(13) 0.0287(7) Uani 1 1 d . . . . .
H4A H 0.553513 0.634194 0.321529 0.043 Uiso 1 1 calc R U . . .
H4B H 0.545855 0.546759 0.320251 0.043 Uiso 1 1 calc R U . . .
H4C H 0.597675 0.582447 0.309887 0.043 Uiso 1 1 calc R U . . .
C5 C 0.55695(14) 0.40777(19) 0.38932(17) 0.0371(8) Uani 1 1 d . . . . .
H5A H 0.530009 0.444984 0.356541 0.056 Uiso 1 1 calc R U . . .
H5B H 0.559324 0.417678 0.429645 0.056 Uiso 1 1 calc R U . . .
H5C H 0.538400 0.358945 0.372830 0.056 Uiso 1 1 calc R U . . .
C6 C 0.68258(16) 0.32953(17) 0.45967(18) 0.0404(8) Uani 1 1 d . . . . .
H6A H 0.662579 0.284255 0.434994 0.061 Uiso 1 1 calc R U . . .
H6B H 0.680183 0.330868 0.497944 0.061 Uiso 1 1 calc R U . . .
H6C H 0.727529 0.330828 0.473917 0.061 Uiso 1 1 calc R U . . .
C7 C 0.62958(17) 0.39957(19) 0.32563(15) 0.0402(8) Uani 1 1 d . . . . .
H7A H 0.613394 0.445450 0.300746 0.060 Uiso 1 1 calc R U . . .
H7B H 0.599141 0.359772 0.301072 0.060 Uiso 1 1 calc R U . . .
H7C H 0.671042 0.387518 0.332910 0.060 Uiso 1 1 calc R U . . .
C8 C 0.81552(12) 0.47033(14) 0.51525(12) 0.0169(5) Uani 1 1 d . . . . .
H8 H 0.800984 0.435669 0.535917 0.020 Uiso 1 1 calc R U . . .
C9 C 0.92128(15) 0.35249(18) 0.57053(16) 0.0384(8) Uani 1 1 d . . . . .
H9A H 0.936645 0.311687 0.556843 0.058 Uiso 1 1 calc R U . . .
H9B H 0.898181 0.332934 0.588794 0.058 Uiso 1 1 calc R U . . .
H9C H 0.957814 0.381777 0.603741 0.058 Uiso 1 1 calc R U . . .
C10 C 0.91529(17) 0.46619(18) 0.47681(19) 0.0414(8) Uani 1 1 d . . . . .
H10A H 0.886890 0.495828 0.437810 0.062 Uiso 1 1 calc R U . . .
H10B H 0.940094 0.432532 0.468119 0.062 Uiso 1 1 calc R U . . .
H10C H 0.944526 0.498622 0.513272 0.062 Uiso 1 1 calc R U . . .
C11 C 0.81678(15) 0.34498(16) 0.43040(14) 0.0295(7) Uani 1 1 d . . . . .
H11A H 0.784385 0.371753 0.391098 0.044 Uiso 1 1 calc R U . . .
H11B H 0.795596 0.310749 0.443221 0.044 Uiso 1 1 calc R U . . .
H11C H 0.844478 0.317451 0.421363 0.044 Uiso 1 1 calc R U . . .
C12 C 0.87216(15) 0.62790(17) 0.54288(16) 0.0345(7) Uani 1 1 d . . . . .
H12A H 0.831004 0.644966 0.505148 0.052 Uiso 1 1 calc R U . . .
H12B H 0.900735 0.615553 0.528996 0.052 Uiso 1 1 calc R U . . .
H12C H 0.891581 0.666861 0.575883 0.052 Uiso 1 1 calc R U . . .
C13 C 0.93937(16) 0.5150(2) 0.65004(16) 0.0480(9) Uani 1 1 d . . . . .
H13A H 0.968325 0.506285 0.635956 0.072 Uiso 1 1 calc R U . . .
H13B H 0.934491 0.469626 0.668217 0.072 Uiso 1 1 calc R U . . .
H13C H 0.957173 0.553598 0.683451 0.072 Uiso 1 1 calc R U . . .
C14 C 0.81155(15) 0.57008(19) 0.61251(14) 0.0352(7) Uani 1 1 d . . . . .
H14A H 0.833195 0.609870 0.644336 0.053 Uiso 1 1 calc R U . . .
H14B H 0.807678 0.527116 0.634035 0.053 Uiso 1 1 calc R U . . .
H14C H 0.768804 0.586420 0.577111 0.053 Uiso 1 1 calc R U . . .
C16 C 0.67616(12) 0.69157(15) 0.18941(12) 0.0187(5) Uani 1 1 d . . . . .
H16 H 0.689016 0.715545 0.161932 0.022 Uiso 1 1 calc R U . . .
C17 C 0.67700(16) 0.85361(16) 0.22477(15) 0.0331(7) Uani 1 1 d . . . . .
H17A H 0.653970 0.891624 0.231961 0.050 Uiso 1 1 calc R U . . .
H17B H 0.681701 0.869103 0.189626 0.050 Uiso 1 1 calc R U . . .
H17C H 0.719428 0.846287 0.264962 0.050 Uiso 1 1 calc R U . . .
C18 C 0.61673(16) 0.74070(18) 0.26574(16) 0.0365(8) Uani 1 1 d . . . . .
H18A H 0.657073 0.724797 0.305227 0.055 Uiso 1 1 calc R U . . .
H18B H 0.585424 0.700669 0.249952 0.055 Uiso 1 1 calc R U . . .
H18C H 0.600259 0.783677 0.275820 0.055 Uiso 1 1 calc R U . . .
C19 C 0.55096(15) 0.7863(2) 0.12509(17) 0.0479(9) Uani 1 1 d . . . . .
H19A H 0.521796 0.744978 0.114855 0.072 Uiso 1 1 calc R U . . .
H19B H 0.555939 0.793994 0.088856 0.072 Uiso 1 1 calc R U . . .
H19C H 0.533331 0.830830 0.131674 0.072 Uiso 1 1 calc R U . . .
C20 C 0.58286(15) 0.56690(19) 0.17234(15) 0.0345(7) Uani 1 1 d . . . . .
H20A H 0.612064 0.557774 0.219299 0.052 Uiso 1 1 calc R U . . .
H20B H 0.563942 0.520311 0.149691 0.052 Uiso 1 1 calc R U . . .
H20C H 0.548814 0.600431 0.164603 0.052 Uiso 1 1 calc R U . . .
C21 C 0.57040(16) 0.6339(2) 0.05271(14) 0.0475(10) Uani 1 1 d . . . . .
H21A H 0.537224 0.666369 0.048476 0.071 Uiso 1 1 calc R U . . .
H21B H 0.550491 0.589011 0.027261 0.071 Uiso 1 1 calc R U . . .
H21C H 0.593185 0.659090 0.036372 0.071 Uiso 1 1 calc R U . . .
C22 C 0.67997(16) 0.53517(18) 0.13988(16) 0.0370(8) Uani 1 1 d . . . . .
H22A H 0.697448 0.552176 0.115171 0.055 Uiso 1 1 calc R U . . .
H22B H 0.654202 0.490884 0.119260 0.055 Uiso 1 1 calc R U . . .
H22C H 0.715188 0.523840 0.184784 0.055 Uiso 1 1 calc R U . . .
C23 C 0.80574(12) 0.71541(14) 0.27561(12) 0.0159(5) Uani 1 1 d . . . . .
H23 H 0.790418 0.761516 0.249049 0.019 Uiso 1 1 calc R U . . .
C24 C 0.80401(15) 0.76734(19) 0.39483(15) 0.0332(7) Uani 1 1 d . . . . .
H24A H 0.779141 0.723412 0.389925 0.050 Uiso 1 1 calc R U . . .
H24B H 0.774796 0.808009 0.370043 0.050 Uiso 1 1 calc R U . . .
H24C H 0.831382 0.780813 0.441084 0.050 Uiso 1 1 calc R U . . .
C25 C 0.91579(14) 0.6790(2) 0.42004(14) 0.0365(8) Uani 1 1 d . . . . .
H25A H 0.940595 0.699125 0.464414 0.055 Uiso 1 1 calc R U . . .
H25B H 0.944590 0.667776 0.406201 0.055 Uiso 1 1 calc R U . . .
H25C H 0.894105 0.633911 0.419365 0.055 Uiso 1 1 calc R U . . .
C26 C 0.89646(17) 0.83547(19) 0.36775(17) 0.0416(8) Uani 1 1 d . . . . .
H26A H 0.864806 0.871168 0.336833 0.062 Uiso 1 1 calc R U . . .
H26B H 0.927609 0.825639 0.356682 0.062 Uiso 1 1 calc R U . . .
H26C H 0.918650 0.855437 0.412115 0.062 Uiso 1 1 calc R U . . .
C27 C 0.86973(16) 0.56803(16) 0.27659(16) 0.0325(7) Uani 1 1 d . . . . .
H27A H 0.829427 0.540659 0.256109 0.049 Uiso 1 1 calc R U . . .
H27B H 0.891672 0.566548 0.324157 0.049 Uiso 1 1 calc R U . . .
H27C H 0.897073 0.545698 0.264406 0.049 Uiso 1 1 calc R U . . .
C28 C 0.93047(14) 0.71188(19) 0.27648(15) 0.0345(7) Uani 1 1 d . . . . .
H28A H 0.958278 0.710428 0.324264 0.052 Uiso 1 1 calc R U . . .
H28B H 0.922546 0.763136 0.261735 0.052 Uiso 1 1 calc R U . . .
H28C H 0.951354 0.686200 0.258270 0.052 Uiso 1 1 calc R U . . .
C29 C 0.80632(15) 0.66680(19) 0.15680(14) 0.0342(7) Uani 1 1 d . . . . .
H29A H 0.829884 0.639242 0.142532 0.051 Uiso 1 1 calc R U . . .
H29B H 0.800530 0.717694 0.141432 0.051 Uiso 1 1 calc R U . . .
H29C H 0.764366 0.643999 0.138660 0.051 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                               MOLECULAR GEOMETRY                           #
#----------------------------------------------------------------------------#

_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
Sn1 O2 1.9724(18) . ?
Sn1 O1 1.9812(17) . ?
O1 B1 1.367(3) . ?
O2 B2 1.362(3) . ?
B1 C8 1.589(4) . ?
B1 C1 1.593(4) . ?
B2 C23 1.588(4) . ?
B2 C16 1.596(4) . ?
Si1 C2 1.864(3) . ?
Si1 C4 1.874(3) . ?
Si1 C3 1.877(3) . ?
Si1 C1 1.883(3) . ?
Si2 C6 1.874(3) . ?
Si2 C5 1.876(3) . ?
Si2 C7 1.878(3) . ?
Si2 C1 1.882(3) . ?
Si3 C9 1.873(3) . ?
Si3 C11 1.874(3) . ?
Si3 C10 1.875(3) . ?
Si3 C8 1.879(3) . ?
Si4 C12 1.861(3) . ?
Si4 C14 1.869(3) . ?
Si4 C13 1.876(3) . ?
Si4 C8 1.887(3) . ?
Si5 C18 1.867(3) . ?
Si5 C17 1.873(3) . ?
Si5 C19 1.874(3) . ?
Si5 C16 1.887(3) . ?
Si6 C21 1.872(3) . ?
Si6 C20 1.874(3) . ?
Si6 C16 1.876(3) . ?
Si6 C22 1.882(3) . ?
Si7 C25 1.866(3) . ?
Si7 C24 1.871(3) . ?
Si7 C26 1.874(3) . ?
Si7 C23 1.889(3) . ?
Si8 C27 1.872(3) . ?
Si8 C28 1.873(3) . ?
Si8 C29 1.873(3) . ?
Si8 C23 1.886(3) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Sn1 O1 97.92(7) . . ?
B1 O1 Sn1 146.71(17) . . ?
B2 O2 Sn1 148.32(17) . . ?
O1 B1 C8 121.0(2) . . ?
O1 B1 C1 119.2(2) . . ?
C8 B1 C1 119.8(2) . . ?
O2 B2 C23 119.5(2) . . ?
O2 B2 C16 120.3(2) . . ?
C23 B2 C16 120.1(2) . . ?
C2 Si1 C4 106.59(14) . . ?
C2 Si1 C3 107.72(14) . . ?
C4 Si1 C3 108.96(13) . . ?
C2 Si1 C1 112.44(12) . . ?
C4 Si1 C1 112.93(13) . . ?
C3 Si1 C1 108.04(13) . . ?
C6 Si2 C5 105.55(15) . . ?
C6 Si2 C7 109.80(16) . . ?
C5 Si2 C7 106.46(16) . . ?
C6 Si2 C1 108.61(13) . . ?
C5 Si2 C1 114.39(14) . . ?
C7 Si2 C1 111.80(13) . . ?
C9 Si3 C11 104.27(15) . . ?
C9 Si3 C10 108.60(16) . . ?
C11 Si3 C10 107.64(15) . . ?
C9 Si3 C8 110.38(14) . . ?
C11 Si3 C8 111.83(13) . . ?
C10 Si3 C8 113.64(13) . . ?
C12 Si4 C14 109.79(15) . . ?
C12 Si4 C13 107.47(17) . . ?
C14 Si4 C13 105.50(16) . . ?
C12 Si4 C8 111.77(13) . . ?
C14 Si4 C8 108.84(13) . . ?
C13 Si4 C8 113.26(15) . . ?
C18 Si5 C17 108.84(15) . . ?
C18 Si5 C19 107.20(16) . . ?
C17 Si5 C19 105.60(16) . . ?
C18 Si5 C16 112.38(13) . . ?
C17 Si5 C16 109.49(13) . . ?
C19 Si5 C16 113.03(15) . . ?
C21 Si6 C20 108.70(15) . . ?
C21 Si6 C16 111.04(15) . . ?
C20 Si6 C16 112.57(13) . . ?
C21 Si6 C22 104.73(16) . . ?
C20 Si6 C22 107.21(15) . . ?
C16 Si6 C22 112.20(13) . . ?
C25 Si7 C24 106.22(15) . . ?
C25 Si7 C26 109.28(16) . . ?
C24 Si7 C26 107.59(16) . . ?
C25 Si7 C23 112.98(13) . . ?
C24 Si7 C23 111.81(13) . . ?
C26 Si7 C23 108.79(14) . . ?
C27 Si8 C28 108.10(15) . . ?
C27 Si8 C29 108.60(15) . . ?
C28 Si8 C29 105.26(14) . . ?
C27 Si8 C23 112.30(13) . . ?
C28 Si8 C23 112.71(14) . . ?
C29 Si8 C23 109.56(13) . . ?
B1 C1 Si2 111.30(17) . . ?
B1 C1 Si1 114.67(17) . . ?
Si2 C1 Si1 114.83(13) . . ?
B1 C1 H1 104.9 . . ?
Si2 C1 H1 104.9 . . ?
Si1 C1 H1 104.9 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 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 . . ?
B1 C8 Si3 116.12(17) . . ?
B1 C8 Si4 110.83(17) . . ?
Si3 C8 Si4 115.77(13) . . ?
B1 C8 H8 104.1 . . ?
Si3 C8 H8 104.1 . . ?
Si4 C8 H8 104.1 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si3 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 . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
B2 C16 Si6 114.88(18) . . ?
B2 C16 Si5 111.20(17) . . ?
Si6 C16 Si5 116.08(13) . . ?
B2 C16 H16 104.4 . . ?
Si6 C16 H16 104.4 . . ?
Si5 C16 H16 104.4 . . ?
Si5 C17 H17A 109.5 . . ?
Si5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si5 C18 H18A 109.5 . . ?
Si5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si5 C19 H19A 109.5 . . ?
Si5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si6 C20 H20A 109.5 . . ?
Si6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si6 C21 H21A 109.5 . . ?
Si6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si6 C22 H22A 109.5 . . ?
Si6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
B2 C23 Si8 112.65(17) . . ?
B2 C23 Si7 113.78(17) . . ?
Si8 C23 Si7 114.71(13) . . ?
B2 C23 H23 104.8 . . ?
Si8 C23 H23 104.8 . . ?
Si7 C23 H23 104.8 . . ?
Si7 C24 H24A 109.5 . . ?
Si7 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si7 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si7 C25 H25A 109.5 . . ?
Si7 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si7 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si7 C26 H26A 109.5 . . ?
Si7 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si7 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si8 C27 H27A 109.5 . . ?
Si8 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si8 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si8 C28 H28A 109.5 . . ?
Si8 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si8 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sn1 O1 B1 C8 81.1(4) . . . . ?
Sn1 O1 B1 C1 -100.8(3) . . . . ?
Sn1 O2 B2 C23 -100.6(3) . . . . ?
Sn1 O2 B2 C16 81.5(4) . . . . ?
O1 B1 C1 Si2 87.7(3) . . . . ?
C8 B1 C1 Si2 -94.2(2) . . . . ?
O1 B1 C1 Si1 -44.8(3) . . . . ?
C8 B1 C1 Si1 133.3(2) . . . . ?
C6 Si2 C1 B1 71.2(2) . . . . ?
C5 Si2 C1 B1 -171.21(18) . . . . ?
C7 Si2 C1 B1 -50.1(2) . . . . ?
C6 Si2 C1 Si1 -156.43(15) . . . . ?
C5 Si2 C1 Si1 -38.83(19) . . . . ?
C7 Si2 C1 Si1 82.27(18) . . . . ?
C2 Si1 C1 B1 -28.4(2) . . . . ?
C4 Si1 C1 B1 92.2(2) . . . . ?
C3 Si1 C1 B1 -147.19(19) . . . . ?
C2 Si1 C1 Si2 -159.21(14) . . . . ?
C4 Si1 C1 Si2 -38.54(18) . . . . ?
C3 Si1 C1 Si2 82.05(16) . . . . ?
O1 B1 C8 Si3 -47.4(3) . . . . ?
C1 B1 C8 Si3 134.6(2) . . . . ?
O1 B1 C8 Si4 87.5(3) . . . . ?
C1 B1 C8 Si4 -90.6(2) . . . . ?
C9 Si3 C8 B1 -158.4(2) . . . . ?
C11 Si3 C8 B1 -42.8(2) . . . . ?
C10 Si3 C8 B1 79.3(2) . . . . ?
C9 Si3 C8 Si4 69.01(18) . . . . ?
C11 Si3 C8 Si4 -175.39(14) . . . . ?
C10 Si3 C8 Si4 -53.3(2) . . . . ?
C12 Si4 C8 B1 -53.6(2) . . . . ?
C14 Si4 C8 B1 67.8(2) . . . . ?
C13 Si4 C8 B1 -175.2(2) . . . . ?
C12 Si4 C8 Si3 81.37(17) . . . . ?
C14 Si4 C8 Si3 -157.19(15) . . . . ?
C13 Si4 C8 Si3 -40.2(2) . . . . ?
O2 B2 C16 Si6 -47.9(3) . . . . ?
C23 B2 C16 Si6 134.2(2) . . . . ?
O2 B2 C16 Si5 86.5(3) . . . . ?
C23 B2 C16 Si5 -91.4(2) . . . . ?
C21 Si6 C16 B2 -158.4(2) . . . . ?
C20 Si6 C16 B2 79.5(2) . . . . ?
C22 Si6 C16 B2 -41.5(2) . . . . ?
C21 Si6 C16 Si5 69.50(19) . . . . ?
C20 Si6 C16 Si5 -52.63(19) . . . . ?
C22 Si6 C16 Si5 -173.67(15) . . . . ?
C18 Si5 C16 B2 -55.8(2) . . . . ?
C17 Si5 C16 B2 65.3(2) . . . . ?
C19 Si5 C16 B2 -177.3(2) . . . . ?
C18 Si5 C16 Si6 78.00(18) . . . . ?
C17 Si5 C16 Si6 -160.92(14) . . . . ?
C19 Si5 C16 Si6 -43.5(2) . . . . ?
O2 B2 C23 Si8 89.4(2) . . . . ?
C16 B2 C23 Si8 -92.7(2) . . . . ?
O2 B2 C23 Si7 -43.3(3) . . . . ?
C16 B2 C23 Si7 134.6(2) . . . . ?
C27 Si8 C23 B2 -53.1(2) . . . . ?
C28 Si8 C23 B2 -175.53(18) . . . . ?
C29 Si8 C23 B2 67.6(2) . . . . ?
C27 Si8 C23 Si7 79.16(18) . . . . ?
C28 Si8 C23 Si7 -43.23(18) . . . . ?
C29 Si8 C23 Si7 -160.07(15) . . . . ?
C25 Si7 C23 B2 90.5(2) . . . . ?
C24 Si7 C23 B2 -29.3(2) . . . . ?
C26 Si7 C23 B2 -147.9(2) . . . . ?
C25 Si7 C23 Si8 -41.25(19) . . . . ?
C24 Si7 C23 Si8 -161.02(15) . . . . ?
C26 Si7 C23 Si8 80.30(18) . . . . ?

#----------------------------------------------------------------------------#
#===END OF CIF FILE FOR SAA24                                                #
#----------------------------------------------------------------------------#
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1832391'
_audit_update_record             
;
2018-03-26 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H6 F36 O7 Pb4'
_chemical_formula_sum            'C18 H6 F36 O7 Pb4'
_chemical_formula_weight         1846.99
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.8700(8)
_cell_length_b                   10.1801(4)
_cell_length_c                   19.4987(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.176(2)
_cell_angle_gamma                90
_cell_volume                     3745.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.55
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.275
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3288
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    18.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_T_max  0.234

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0556
_diffrn_reflns_av_uneti/neti     0.0640
_diffrn_reflns_number            23053
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total             8505
_reflns_number_gt                6619
_reflns_threshold_expression     >2sigma(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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1124P)²+63.4153P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00080(8)
_refine_ls_number_reflns         8505
_refine_ls_number_parameters     575
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1260
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         3.570
_refine_diff_density_min         -4.045
_refine_diff_density_rms         0.422

#...............................................................................
# .RES SHELXL file: job.res
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ...........................................
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.65493(2) 0.55852(4) 0.26397(2) 0.01562(14) Uani 1 1 d . . . . .
O1 O 0.6672(5) 0.5264(9) 0.3889(5) 0.022(2) Uani 1 1 d . . . . .
C2 C 0.6556(7) 0.6109(13) 0.4409(7) 0.022(3) Uani 1 1 d . . . . .
H2 H 0.700288 0.656916 0.450027 0.026 Uiso 1 1 calc R U . . .
C3 C 0.6008(7) 0.7137(15) 0.4219(7) 0.027(3) Uani 1 1 d . . . . .
F4 F 0.6252(5) 0.7829(9) 0.3681(5) 0.043(2) Uani 1 1 d . . . . .
F5 F 0.5403(5) 0.6611(9) 0.4022(6) 0.041(2) Uani 1 1 d . . . . .
F6 F 0.5875(6) 0.7973(10) 0.4716(6) 0.049(3) Uani 1 1 d . . . . .
C7 C 0.6343(8) 0.5375(17) 0.5078(7) 0.031(3) Uani 1 1 d . . . . .
F8 F 0.6278(7) 0.6162(14) 0.5607(5) 0.064(3) Uani 1 1 d . . . . .
F9 F 0.5732(5) 0.4734(11) 0.4987(5) 0.043(2) Uani 1 1 d . . . . .
F10 F 0.6832(5) 0.4454(11) 0.5219(5) 0.043(3) Uani 1 1 d . . . . .
O11 O 0.8354(5) 0.4642(10) 0.3954(5) 0.026(2) Uani 1 1 d . . . . .
C12 C 0.8915(7) 0.4538(15) 0.4426(7) 0.026(3) Uani 1 1 d . . . . .
H12 H 0.926693 0.520787 0.430850 0.032 Uiso 1 1 calc R U . . .
C13 C 0.8664(8) 0.4813(17) 0.5148(8) 0.034(3) Uani 1 1 d . . . . .
F14 F 0.8293(6) 0.5916(10) 0.5170(5) 0.045(2) Uani 1 1 d . . . . .
F15 F 0.8218(5) 0.3848(11) 0.5371(5) 0.045(2) Uani 1 1 d . . . . .
F16 F 0.9189(5) 0.4900(13) 0.5589(5) 0.049(3) Uani 1 1 d . . . . .
C17 C 0.9264(8) 0.3200(18) 0.4343(10) 0.040(4) Uani 1 1 d . . . . .
F18 F 0.8801(6) 0.2198(10) 0.4401(7) 0.058(3) Uani 1 1 d . . . . .
F19 F 0.9771(6) 0.2996(12) 0.4840(6) 0.057(3) Uani 1 1 d . . . . .
F20 F 0.9573(7) 0.3114(14) 0.3750(6) 0.070(4) Uani 1 1 d . . . . .
Pb2 Pb 0.72916(3) 0.33644(5) 0.38178(2) 0.02066(15) Uani 1 1 d . . . . .
O21 O 0.6366(5) 0.3171(9) 0.2825(5) 0.0213(19) Uani 1 1 d . . . . .
C22 C 0.5742(7) 0.2495(14) 0.2803(7) 0.021(3) Uani 1 1 d . . . . .
H22 H 0.547567 0.279084 0.239926 0.025 Uiso 1 1 calc R U . . .
C23 C 0.5296(8) 0.2769(15) 0.3431(7) 0.028(3) Uani 1 1 d . . . . .
F24 F 0.5182(5) 0.4048(9) 0.3493(5) 0.037(2) Uani 1 1 d . . . . .
F25 F 0.5606(6) 0.2386(10) 0.4013(5) 0.048(3) Uani 1 1 d . . . . .
F26 F 0.4648(5) 0.2194(10) 0.3400(6) 0.046(3) Uani 1 1 d . . . . .
C27 C 0.5890(7) 0.1018(17) 0.2721(8) 0.034(4) Uani 1 1 d . . . . .
F28 F 0.6330(6) 0.0589(9) 0.3211(6) 0.046(3) Uani 1 1 d . . . . .
F29 F 0.5311(5) 0.0299(10) 0.2713(6) 0.045(3) Uani 1 1 d . . . . .
F30 F 0.6223(6) 0.0819(10) 0.2130(5) 0.049(3) Uani 1 1 d . . . . .
O41 O 0.6949(5) 0.4767(10) 0.1522(5) 0.026(2) Uani 1 1 d . . . . .
C42 C 0.6632(6) 0.4959(12) 0.0895(6) 0.015(2) Uani 1 1 d . . . . .
H42 H 0.645611 0.586476 0.087822 0.018 Uiso 1 1 calc R U . . .
C43 C 0.5997(7) 0.4031(13) 0.0796(7) 0.023(3) Uani 1 1 d . . . . .
F44 F 0.5554(4) 0.4181(10) 0.1326(5) 0.036(2) Uani 1 1 d . . . . .
F45 F 0.6198(5) 0.2757(10) 0.0794(6) 0.051(3) Uani 1 1 d . . . . .
F46 F 0.5636(5) 0.4237(11) 0.0229(5) 0.044(2) Uani 1 1 d . . . . .
C47 C 0.7181(7) 0.4791(16) 0.0326(7) 0.029(3) Uani 1 1 d . . . . .
F48 F 0.7566(5) 0.3713(10) 0.0393(5) 0.042(2) Uani 1 1 d . . . . .
F49 F 0.6890(5) 0.4768(11) -0.0302(4) 0.043(2) Uani 1 1 d . . . . .
Pb3 Pb 0.75104(2) 0.29394(4) 0.19127(2) 0.01752(14) Uani 1 1 d . . . . .
F50 F 0.7632(5) 0.5797(11) 0.0341(5) 0.047(3) Uani 1 1 d . . . . .
O51 O 0.8559(5) 0.4067(9) 0.1821(5) 0.026(2) Uani 1 1 d . . . . .
C52 C 0.9115(7) 0.3688(15) 0.1393(8) 0.028(3) Uani 1 1 d . . . . .
H52 H 0.891523 0.328136 0.097941 0.034 Uiso 1 1 calc R U . . .
C53 C 0.9569(8) 0.2654(19) 0.1777(8) 0.038(4) Uani 1 1 d . . . . .
F54 F 0.9146(6) 0.1643(10) 0.1960(6) 0.053(3) Uani 1 1 d . . . . .
F55 F 1.0080(5) 0.2158(11) 0.1382(5) 0.044(2) Uani 1 1 d . . . . .
F56 F 0.9858(5) 0.3095(11) 0.2346(5) 0.047(3) Uani 1 1 d . . . . .
C57 C 0.9543(9) 0.487(2) 0.1185(9) 0.045(4) Uani 1 1 d . . . . .
F58 F 0.9145(7) 0.5685(13) 0.0816(7) 0.073(4) Uani 1 1 d . . . . .
F59 F 1.0104(5) 0.4558(11) 0.0806(6) 0.050(3) Uani 1 1 d . . . . .
F60 F 0.9786(6) 0.5542(12) 0.1728(6) 0.063(4) Uani 1 1 d . . . . .
Pb4 Pb 0.85519(2) 0.55310(5) 0.28398(2) 0.01677(14) Uani 1 1 d . . . . .
O61 O 0.7581(4) 0.6969(9) 0.2753(5) 0.0201(19) Uani 1 1 d . . . . .
C62 C 0.7574(8) 0.8261(13) 0.2594(8) 0.0274(18) Uani 1 1 d . . . . .
H62 H 0.708037 0.855802 0.261599 0.033 Uiso 1 1 calc R U . . .
C63 C 0.7828(8) 0.8468(13) 0.1857(8) 0.0274(18) Uani 1 1 d . . . . .
F64 F 0.7385(8) 0.7854(12) 0.1442(5) 0.066(4) Uani 1 1 d . . . . .
F65 F 0.8472(7) 0.7998(10) 0.1765(6) 0.057(3) Uani 1 1 d . . . . .
F66 F 0.7834(7) 0.9723(9) 0.1665(5) 0.054(3) Uani 1 1 d . . . . .
C67 C 0.8003(8) 0.9083(13) 0.3120(8) 0.0274(18) Uani 1 1 d . . . . .
F68 F 0.8694(5) 0.8752(11) 0.3090(6) 0.053(3) Uani 1 1 d . . . . .
F69 F 0.7981(6) 1.0361(10) 0.3001(6) 0.052(3) Uani 1 1 d . . . . .
F70 F 0.7781(7) 0.8855(12) 0.3738(5) 0.062(3) Uani 1 1 d . . . . .
O101 O 0.7564(4) 0.4325(8) 0.2801(4) 0.0144(17) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O101 2.325(8) . ?
Pb1 O61 2.413(9) . ?
Pb1 O41 2.455(9) . ?
Pb1 O1 2.468(9) . ?
Pb1 O21 2.508(9) . ?
Pb1 Pb2 3.5113(7) . ?
Pb1 Pb3 3.5452(6) . ?
O1 C2 1.348(15) . ?
O1 Pb2 2.265(8) . ?
C2 C3 1.517(19) . ?
C2 C7 1.558(19) . ?
C2 H2 0.9800 . ?
C3 F6 1.315(16) . ?
C3 F5 1.316(17) . ?
C3 F4 1.345(17) . ?
C7 F8 1.313(18) . ?
C7 F9 1.337(18) . ?
C7 F10 1.343(18) . ?
O11 C12 1.406(16) . ?
O11 Pb4 2.384(9) . ?
O11 Pb2 2.403(10) . ?
C12 C13 1.51(2) . ?
C12 C17 1.52(2) . ?
C12 H12 0.9800 . ?
C13 F16 1.314(17) . ?
C13 F14 1.324(18) . ?
C13 F15 1.364(19) . ?
C17 F20 1.30(2) . ?
C17 F18 1.35(2) . ?
C17 F19 1.374(19) . ?
Pb2 O101 2.272(7) . ?
Pb2 O21 2.611(9) . ?
O21 C22 1.365(15) . ?
C22 C23 1.513(17) . ?
C22 C27 1.54(2) . ?
C22 H22 0.9800 . ?
C23 F24 1.326(17) . ?
C23 F25 1.334(18) . ?
C23 F26 1.356(16) . ?
C27 F29 1.315(16) . ?
C27 F30 1.330(17) . ?
C27 F28 1.34(2) . ?
O41 C42 1.373(14) . ?
O41 Pb3 2.272(10) . ?
C42 C47 1.531(17) . ?
C42 C43 1.537(18) . ?
C42 H42 0.9800 . ?
C43 F46 1.315(16) . ?
C43 F44 1.339(15) . ?
C43 F45 1.351(16) . ?
C47 F48 1.322(17) . ?
C47 F50 1.332(18) . ?
C47 F49 1.340(17) . ?
Pb3 O101 2.235(9) . ?
Pb3 O51 2.295(9) . ?
O51 C52 1.397(15) . ?
O51 Pb4 2.483(9) . ?
C52 C57 1.51(2) . ?
C52 C53 1.55(2) . ?
C52 H52 0.9800 . ?
C53 F56 1.31(2) . ?
C53 F55 1.335(17) . ?
C53 F54 1.351(19) . ?
C57 F58 1.33(2) . ?
C57 F59 1.332(18) . ?
C57 F60 1.34(2) . ?
Pb4 O101 2.233(8) . ?
Pb4 O61 2.351(9) . ?
O61 C62 1.351(16) . ?
C62 C63 1.53(2) . ?
C62 C67 1.55(2) . ?
C62 H62 0.9800 . ?
C63 F64 1.319(19) . ?
C63 F65 1.319(18) . ?
C63 F66 1.331(15) . ?
C67 F70 1.299(17) . ?
C67 F69 1.322(16) . ?
C67 F68 1.348(17) . ?

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
O101 Pb1 O61 69.3(3) . . ?
O101 Pb1 O41 71.2(3) . . ?
O61 Pb1 O41 91.7(3) . . ?
O101 Pb1 O1 73.7(3) . . ?
O61 Pb1 O1 85.1(3) . . ?
O41 Pb1 O1 143.5(3) . . ?
O101 Pb1 O21 63.5(3) . . ?
O61 Pb1 O21 132.1(3) . . ?
O41 Pb1 O21 80.7(3) . . ?
O1 Pb1 O21 75.0(3) . . ?
O101 Pb1 Pb2 39.64(18) . . ?
O61 Pb1 Pb2 89.8(2) . . ?
O41 Pb1 Pb2 103.9(2) . . ?
O1 Pb1 Pb2 39.92(19) . . ?
O21 Pb1 Pb2 47.9(2) . . ?
O101 Pb1 Pb3 38.1(2) . . ?
O61 Pb1 Pb3 93.8(2) . . ?
O41 Pb1 Pb3 39.5(2) . . ?
O1 Pb1 Pb3 104.34(19) . . ?
O21 Pb1 Pb3 52.0(2) . . ?
Pb2 Pb1 Pb3 64.464(13) . . ?
C2 O1 Pb2 132.5(8) . . ?
C2 O1 Pb1 130.0(8) . . ?
Pb2 O1 Pb1 95.7(3) . . ?
O1 C2 C3 111.6(11) . . ?
O1 C2 C7 111.5(11) . . ?
C3 C2 C7 111.0(11) . . ?
O1 C2 H2 107.5 . . ?
C3 C2 H2 107.5 . . ?
C7 C2 H2 107.5 . . ?
F6 C3 F5 108.1(11) . . ?
F6 C3 F4 107.5(12) . . ?
F5 C3 F4 106.6(13) . . ?
F6 C3 C2 113.4(13) . . ?
F5 C3 C2 112.4(12) . . ?
F4 C3 C2 108.5(11) . . ?
F8 C7 F9 108.6(12) . . ?
F8 C7 F10 109.4(13) . . ?
F9 C7 F10 106.2(14) . . ?
F8 C7 C2 113.0(14) . . ?
F9 C7 C2 110.3(12) . . ?
F10 C7 C2 109.1(10) . . ?
C12 O11 Pb4 120.4(8) . . ?
C12 O11 Pb2 131.2(8) . . ?
Pb4 O11 Pb2 103.8(3) . . ?
O11 C12 C13 111.0(11) . . ?
O11 C12 C17 108.9(12) . . ?
C13 C12 C17 113.7(13) . . ?
O11 C12 H12 107.7 . . ?
C13 C12 H12 107.7 . . ?
C17 C12 H12 107.7 . . ?
F16 C13 F14 108.6(14) . . ?
F16 C13 F15 107.7(14) . . ?
F14 C13 F15 105.9(12) . . ?
F16 C13 C12 112.5(12) . . ?
F14 C13 C12 110.7(14) . . ?
F15 C13 C12 111.0(13) . . ?
F20 C17 F18 108.4(16) . . ?
F20 C17 F19 107.7(13) . . ?
F18 C17 F19 106.0(15) . . ?
F20 C17 C12 110.6(15) . . ?
F18 C17 C12 112.8(13) . . ?
F19 C17 C12 111.2(14) . . ?
O1 Pb2 O101 78.7(3) . . ?
O1 Pb2 O11 87.8(3) . . ?
O101 Pb2 O11 70.9(3) . . ?
O1 Pb2 O21 76.4(3) . . ?
O101 Pb2 O21 62.5(3) . . ?
O11 Pb2 O21 132.7(3) . . ?
O1 Pb2 Pb1 44.4(2) . . ?
O101 Pb2 Pb1 40.8(2) . . ?
O11 Pb2 Pb1 93.1(2) . . ?
O21 Pb2 Pb1 45.5(2) . . ?
C22 O21 Pb1 127.5(8) . . ?
C22 O21 Pb2 129.5(8) . . ?
Pb1 O21 Pb2 86.6(3) . . ?
O21 C22 C23 111.4(11) . . ?
O21 C22 C27 109.8(11) . . ?
C23 C22 C27 111.5(11) . . ?
O21 C22 H22 108.0 . . ?
C23 C22 H22 108.0 . . ?
C27 C22 H22 108.0 . . ?
F24 C23 F25 106.3(12) . . ?
F24 C23 F26 106.4(12) . . ?
F25 C23 F26 107.7(12) . . ?
F24 C23 C22 110.2(11) . . ?
F25 C23 C22 113.0(12) . . ?
F26 C23 C22 112.8(12) . . ?
F29 C27 F30 107.5(13) . . ?
F29 C27 F28 109.9(14) . . ?
F30 C27 F28 106.0(13) . . ?
F29 C27 C22 113.2(12) . . ?
F30 C27 C22 109.1(13) . . ?
F28 C27 C22 111.0(12) . . ?
C42 O41 Pb3 128.1(8) . . ?
C42 O41 Pb1 127.4(7) . . ?
Pb3 O41 Pb1 97.1(3) . . ?
O41 C42 C47 109.6(10) . . ?
O41 C42 C43 111.2(10) . . ?
C47 C42 C43 111.6(10) . . ?
O41 C42 H42 108.1 . . ?
C47 C42 H42 108.1 . . ?
C43 C42 H42 108.1 . . ?
F46 C43 F44 107.9(11) . . ?
F46 C43 F45 107.1(11) . . ?
F44 C43 F45 106.7(12) . . ?
F46 C43 C42 114.2(12) . . ?
F44 C43 C42 108.7(10) . . ?
F45 C43 C42 111.9(11) . . ?
F48 C47 F50 106.6(12) . . ?
F48 C47 F49 107.5(12) . . ?
F50 C47 F49 107.0(13) . . ?
F48 C47 C42 113.2(12) . . ?
F50 C47 C42 109.4(11) . . ?
F49 C47 C42 112.8(11) . . ?
O101 Pb3 O41 76.3(3) . . ?
O101 Pb3 O51 73.0(3) . . ?
O41 Pb3 O51 88.0(4) . . ?
O101 Pb3 Pb1 39.9(2) . . ?
O41 Pb3 Pb1 43.4(2) . . ?
O51 Pb3 Pb1 95.4(2) . . ?
C52 O51 Pb3 123.9(8) . . ?
C52 O51 Pb4 130.5(9) . . ?
Pb3 O51 Pb4 103.4(3) . . ?
O51 C52 C57 110.1(12) . . ?
O51 C52 C53 108.3(12) . . ?
C57 C52 C53 112.1(13) . . ?
O51 C52 H52 108.7 . . ?
C57 C52 H52 108.7 . . ?
C53 C52 H52 108.7 . . ?
F56 C53 F55 108.6(13) . . ?
F56 C53 F54 106.4(14) . . ?
F55 C53 F54 107.0(15) . . ?
F56 C53 C52 113.8(15) . . ?
F55 C53 C52 112.2(13) . . ?
F54 C53 C52 108.5(12) . . ?
F58 C57 F59 107.3(14) . . ?
F58 C57 F60 107.6(17) . . ?
F59 C57 F60 106.8(15) . . ?
F58 C57 C52 110.0(15) . . ?
F59 C57 C52 112.7(15) . . ?
F60 C57 C52 112.2(14) . . ?
O101 Pb4 O61 71.9(3) . . ?
O101 Pb4 O11 71.9(3) . . ?
O61 Pb4 O11 100.2(3) . . ?
O101 Pb4 O51 69.5(3) . . ?
O61 Pb4 O51 108.8(3) . . ?
O11 Pb4 O51 120.1(3) . . ?
C62 O61 Pb4 129.1(9) . . ?
C62 O61 Pb1 122.7(9) . . ?
Pb4 O61 Pb1 105.8(4) . . ?
O61 C62 C63 110.2(11) . . ?
O61 C62 C67 111.7(12) . . ?
C63 C62 C67 112.4(12) . . ?
O61 C62 H62 107.4 . . ?
C63 C62 H62 107.4 . . ?
C67 C62 H62 107.4 . . ?
F64 C63 F65 109.1(13) . . ?
F64 C63 F66 106.8(14) . . ?
F65 C63 F66 107.5(12) . . ?
F64 C63 C62 108.1(12) . . ?
F65 C63 C62 111.7(13) . . ?
F66 C63 C62 113.5(11) . . ?
F70 C67 F69 109.1(12) . . ?
F70 C67 F68 108.1(14) . . ?
F69 C67 F68 105.6(12) . . ?
F70 C67 C62 110.3(12) . . ?
F69 C67 C62 113.6(13) . . ?
F68 C67 C62 109.9(11) . . ?
Pb4 O101 Pb3 114.2(3) . . ?
Pb4 O101 Pb2 113.4(3) . . ?
Pb3 O101 Pb2 113.2(3) . . ?
Pb4 O101 Pb1 112.8(3) . . ?
Pb3 O101 Pb1 102.0(3) . . ?
Pb2 O101 Pb1 99.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb2 O1 C2 C3 -171.3(8) . . . . ?
Pb1 O1 C2 C3 27.6(16) . . . . ?
Pb2 O1 C2 C7 -46.6(16) . . . . ?
Pb1 O1 C2 C7 152.4(9) . . . . ?
O1 C2 C3 F6 179.3(11) . . . . ?
C7 C2 C3 F6 54.3(16) . . . . ?
O1 C2 C3 F5 56.3(15) . . . . ?
C7 C2 C3 F5 -68.7(15) . . . . ?
O1 C2 C3 F4 -61.3(15) . . . . ?
C7 C2 C3 F4 173.7(12) . . . . ?
O1 C2 C7 F8 175.3(12) . . . . ?
C3 C2 C7 F8 -59.6(16) . . . . ?
O1 C2 C7 F9 -62.9(16) . . . . ?
C3 C2 C7 F9 62.2(16) . . . . ?
O1 C2 C7 F10 53.4(16) . . . . ?
C3 C2 C7 F10 178.5(12) . . . . ?
Pb4 O11 C12 C13 143.5(10) . . . . ?
Pb2 O11 C12 C13 -65.1(16) . . . . ?
Pb4 O11 C12 C17 -90.7(13) . . . . ?
Pb2 O11 C12 C17 60.8(15) . . . . ?
O11 C12 C13 F16 -171.3(13) . . . . ?
C17 C12 C13 F16 65.5(18) . . . . ?
O11 C12 C13 F14 -49.5(17) . . . . ?
C17 C12 C13 F14 -172.7(13) . . . . ?
O11 C12 C13 F15 67.8(16) . . . . ?
C17 C12 C13 F15 -55.3(17) . . . . ?
O11 C12 C17 F20 66.6(17) . . . . ?
C13 C12 C17 F20 -169.1(14) . . . . ?
O11 C12 C17 F18 -54.9(18) . . . . ?
C13 C12 C17 F18 69.3(18) . . . . ?
O11 C12 C17 F19 -173.9(12) . . . . ?
C13 C12 C17 F19 -49.6(18) . . . . ?
Pb1 O21 C22 C23 -73.6(13) . . . . ?
Pb2 O21 C22 C23 48.8(15) . . . . ?
Pb1 O21 C22 C27 162.4(8) . . . . ?
Pb2 O21 C22 C27 -75.2(13) . . . . ?
O21 C22 C23 F24 56.4(16) . . . . ?
C27 C22 C23 F24 179.4(12) . . . . ?
O21 C22 C23 F25 -62.4(16) . . . . ?
C27 C22 C23 F25 60.7(16) . . . . ?
O21 C22 C23 F26 175.1(12) . . . . ?
C27 C22 C23 F26 -61.9(16) . . . . ?
O21 C22 C27 F29 178.4(12) . . . . ?
C23 C22 C27 F29 54.5(18) . . . . ?
O21 C22 C27 F30 -62.0(16) . . . . ?
C23 C22 C27 F30 174.1(12) . . . . ?
O21 C22 C27 F28 54.3(14) . . . . ?
C23 C22 C27 F28 -69.5(15) . . . . ?
Pb3 O41 C42 C47 -60.0(14) . . . . ?
Pb1 O41 C42 C47 157.1(9) . . . . ?
Pb3 O41 C42 C43 63.9(12) . . . . ?
Pb1 O41 C42 C43 -79.0(12) . . . . ?
O41 C42 C43 F46 174.9(10) . . . . ?
C47 C42 C43 F46 -62.4(14) . . . . ?
O41 C42 C43 F44 54.4(14) . . . . ?
C47 C42 C43 F44 177.1(11) . . . . ?
O41 C42 C43 F45 -63.2(14) . . . . ?
C47 C42 C43 F45 59.5(15) . . . . ?
O41 C42 C47 F48 48.2(16) . . . . ?
C43 C42 C47 F48 -75.4(14) . . . . ?
O41 C42 C47 F50 -70.5(15) . . . . ?
C43 C42 C47 F50 165.9(11) . . . . ?
O41 C42 C47 F49 170.6(12) . . . . ?
C43 C42 C47 F49 46.9(17) . . . . ?
Pb3 O51 C52 C57 152.6(11) . . . . ?
Pb4 O51 C52 C57 -47.3(18) . . . . ?
Pb3 O51 C52 C53 -84.4(13) . . . . ?
Pb4 O51 C52 C53 75.7(15) . . . . ?
O51 C52 C53 F56 -61.4(16) . . . . ?
C57 C52 C53 F56 60.3(17) . . . . ?
O51 C52 C53 F55 174.9(12) . . . . ?
C57 C52 C53 F55 -63.4(18) . . . . ?
O51 C52 C53 F54 56.8(16) . . . . ?
C57 C52 C53 F54 178.5(13) . . . . ?
O51 C52 C57 F58 -63.7(18) . . . . ?
C53 C52 C57 F58 175.6(14) . . . . ?
O51 C52 C57 F59 176.6(14) . . . . ?
C53 C52 C57 F59 55.9(19) . . . . ?
O51 C52 C57 F60 55.9(19) . . . . ?
C53 C52 C57 F60 -64.7(18) . . . . ?
Pb4 O61 C62 C63 64.8(16) . . . . ?
Pb1 O61 C62 C63 -94.6(12) . . . . ?
Pb4 O61 C62 C67 -61.0(14) . . . . ?
Pb1 O61 C62 C67 139.7(9) . . . . ?
O61 C62 C63 F64 61.7(16) . . . . ?
C67 C62 C63 F64 -173.0(12) . . . . ?
O61 C62 C63 F65 -58.3(16) . . . . ?
C67 C62 C63 F65 67.0(15) . . . . ?
O61 C62 C63 F66 180.0(13) . . . . ?
C67 C62 C63 F66 -54.7(18) . . . . ?
O61 C62 C67 F70 -54.0(16) . . . . ?
C63 C62 C67 F70 -178.6(13) . . . . ?
O61 C62 C67 F69 -176.9(12) . . . . ?
C63 C62 C67 F69 58.6(16) . . . . ?
O61 C62 C67 F68 65.1(15) . . . . ?
C63 C62 C67 F68 -59.4(16) . . . . ?

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR SAA36                                                  #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1832392'
_audit_update_record             
;
2018-03-26 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;


#----------------------------------------------------------------------------#
#                            CHEMICAL INFORMATION                            #
#----------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H30 N2 Pb Si2'
_chemical_formula_sum            'C15 H30 N2 Pb Si2'
_chemical_formula_weight         501.78
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                           UNIT CELL INFORMATION                            #
#----------------------------------------------------------------------------#


_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9054(10)
_cell_length_b                   10.6022(11)
_cell_length_c                   12.4223(14)
_cell_angle_alpha                103.574(4)
_cell_angle_beta                 110.985(4)
_cell_angle_gamma                103.843(4)
_cell_volume                     994.66(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9436
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.66
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                            CRYSTAL INFORMATION                             #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             488
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                           ABSORPTION CORRECTION                            #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    8.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.025
_exptl_absorpt_correction_T_max  0.054

#----------------------------------------------------------------------------#
#                              DATA COLLECTION                               #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_r_equivalents  0.0475
_diffrn_reflns_av_uneti/neti     0.0489
_diffrn_reflns_number            12673
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.067
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_reflns_number_total             4523
_reflns_number_gt                4268
_reflns_threshold_expression     >2sigma(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.
;

#----------------------------------------------------------------------------#
#                           COMPUTER PROGRAMS USED                           #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'

#----------------------------------------------------------------------------#
#                           REFINEMENT INFORMATION                           #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0130P)²+0.4658P] 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         4523
_refine_ls_number_parameters     189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.668
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.165

#...............................................................................
# .RES SHELXL file: job.res
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file .............................................
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#              ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS              #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.39142(2) 0.60331(2) 0.91556(2) 0.01398(6) Uani 1 1 d . . . . .
C1 C 0.5187(5) 0.7523(4) 0.8386(4) 0.0151(8) Uani 1 1 d . . . . .
C2 C 0.6926(5) 0.8027(4) 0.8659(4) 0.0212(9) Uani 1 1 d . . . . .
H2 H 0.769552 0.768921 0.915953 0.025 Uiso 1 1 calc R U . . .
C3 C 0.7555(6) 0.9013(4) 0.8215(4) 0.0262(10) Uani 1 1 d . . . . .
H3 H 0.874101 0.932930 0.839694 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6457(6) 0.9531(4) 0.7508(4) 0.0279(10) Uani 1 1 d . . . . .
H4 H 0.688400 1.020604 0.720212 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4731(6) 0.9066(4) 0.7246(4) 0.0234(9) Uani 1 1 d . . . . .
H5 H 0.397370 0.942662 0.676184 0.028 Uiso 1 1 calc R U . . .
C6 C 0.4108(5) 0.8083(4) 0.7684(4) 0.0169(8) Uani 1 1 d . . . . .
C7 C 0.2227(5) 0.7539(4) 0.7352(4) 0.0195(8) Uani 1 1 d . . . . .
H7A H 0.172091 0.823586 0.714680 0.023 Uiso 1 1 calc R U . . .
H7B H 0.165286 0.668503 0.660972 0.023 Uiso 1 1 calc R U . . .
N8 N 0.1889(4) 0.7220(3) 0.8363(3) 0.0159(7) Uani 1 1 d . . . . .
C9 C 0.2423(6) 0.8511(4) 0.9390(4) 0.0253(9) Uani 1 1 d . . . . .
H9A H 0.176149 0.908097 0.910364 0.038 Uiso 1 1 calc R U . . .
H9B H 0.365251 0.902528 0.969523 0.038 Uiso 1 1 calc R U . . .
H9C H 0.221016 0.828590 1.005617 0.038 Uiso 1 1 calc R U . . .
C10 C 0.0060(5) 0.6439(4) 0.7926(4) 0.0237(9) Uani 1 1 d . . . . .
H10A H -0.014512 0.628630 0.861700 0.036 Uiso 1 1 calc R U . . .
H10B H -0.027329 0.554115 0.729120 0.036 Uiso 1 1 calc R U . . .
H10C H -0.062457 0.696637 0.757689 0.036 Uiso 1 1 calc R U . . .
N11 N 0.2527(4) 0.4110(3) 0.7452(3) 0.0155(7) Uani 1 1 d . . . . .
Si1 Si 0.09398(14) 0.28237(11) 0.74602(10) 0.0163(2) Uani 1 1 d . . . . .
C12 C -0.1126(6) 0.2211(5) 0.6025(4) 0.0294(10) Uani 1 1 d . . . . .
H12A H -0.149502 0.299790 0.594674 0.044 Uiso 1 1 calc R U . . .
H12B H -0.201370 0.150518 0.607292 0.044 Uiso 1 1 calc R U . . .
H12C H -0.094677 0.180973 0.530585 0.044 Uiso 1 1 calc R U . . .
C13 C 0.0422(6) 0.3419(4) 0.8781(4) 0.0250(9) Uani 1 1 d . . . . .
H13A H 0.145432 0.371471 0.955914 0.037 Uiso 1 1 calc R U . . .
H13B H -0.048769 0.265364 0.874638 0.037 Uiso 1 1 calc R U . . .
H13C H 0.002885 0.420023 0.873076 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1521(6) 0.1270(4) 0.7637(5) 0.0291(10) Uani 1 1 d . . . . .
H14A H 0.177163 0.086481 0.695635 0.044 Uiso 1 1 calc R U . . .
H14B H 0.055647 0.057955 0.762611 0.044 Uiso 1 1 calc R U . . .
H14C H 0.253901 0.155615 0.842178 0.044 Uiso 1 1 calc R U . . .
Si2 Si 0.34284(14) 0.38335(11) 0.64413(10) 0.0178(2) Uani 1 1 d . . . . .
C15 C 0.2506(8) 0.2015(5) 0.5328(5) 0.0456(15) Uani 1 1 d . . . . .
H15A H 0.273182 0.138547 0.578012 0.068 Uiso 1 1 calc R U . . .
H15B H 0.303961 0.194980 0.476110 0.068 Uiso 1 1 calc R U . . .
H15C H 0.126055 0.175487 0.485921 0.068 Uiso 1 1 calc R U . . .
C16 C 0.5785(6) 0.4195(5) 0.7284(4) 0.0299(10) Uani 1 1 d . . . . .
H16A H 0.638187 0.518684 0.777803 0.045 Uiso 1 1 calc R U . . .
H16B H 0.624085 0.393563 0.668932 0.045 Uiso 1 1 calc R U . . .
H16C H 0.596539 0.365279 0.782742 0.045 Uiso 1 1 calc R U . . .
C17 C 0.3086(6) 0.4892(5) 0.5438(4) 0.0284(10) Uani 1 1 d . . . . .
H17A H 0.188542 0.483877 0.511937 0.043 Uiso 1 1 calc R U . . .
H17B H 0.334369 0.453495 0.474872 0.043 Uiso 1 1 calc R U . . .
H17C H 0.384826 0.586096 0.591851 0.043 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                             MOLECULAR GEOMETRY                             #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N11 2.249(3) . ?
Pb1 C1 2.308(4) . ?
Pb1 N8 2.490(3) . ?
C1 C2 1.393(5) . ?
C1 C6 1.397(5) . ?
C2 C3 1.386(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.496(5) . ?
C7 N8 1.484(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C10 1.464(5) . ?
N8 C9 1.470(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N11 Si1 1.718(3) . ?
N11 Si2 1.723(3) . ?
Si1 C13 1.871(4) . ?
Si1 C12 1.876(5) . ?
Si1 C14 1.877(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Si2 C17 1.858(5) . ?
Si2 C15 1.866(5) . ?
Si2 C16 1.871(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Pb1 C1 99.02(12) . . ?
N11 Pb1 N8 94.18(11) . . ?
C1 Pb1 N8 73.25(12) . . ?
C2 C1 C6 117.6(3) . . ?
C2 C1 Pb1 126.9(3) . . ?
C6 C1 Pb1 115.0(3) . . ?
C3 C2 C1 121.3(4) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 C7 120.0(4) . . ?
C1 C6 C7 118.8(3) . . ?
N8 C7 C6 112.5(3) . . ?
N8 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N8 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C10 N8 C9 109.4(3) . . ?
C10 N8 C7 110.8(3) . . ?
C9 N8 C7 110.3(3) . . ?
C10 N8 Pb1 116.2(2) . . ?
C9 N8 Pb1 105.6(2) . . ?
C7 N8 Pb1 104.4(2) . . ?
N8 C9 H9A 109.5 . . ?
N8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N8 C10 H10A 109.5 . . ?
N8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 N11 Si2 123.26(19) . . ?
Si1 N11 Pb1 115.67(17) . . ?
Si2 N11 Pb1 118.93(16) . . ?
N11 Si1 C13 112.43(18) . . ?
N11 Si1 C12 111.52(19) . . ?
C13 Si1 C12 106.2(2) . . ?
N11 Si1 C14 114.01(19) . . ?
C13 Si1 C14 103.9(2) . . ?
C12 Si1 C14 108.2(2) . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N11 Si2 C17 112.38(19) . . ?
N11 Si2 C15 114.2(2) . . ?
C17 Si2 C15 103.8(3) . . ?
N11 Si2 C16 111.06(19) . . ?
C17 Si2 C16 109.5(2) . . ?
C15 Si2 C16 105.3(3) . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.3(6) . . . . ?
Pb1 C1 C2 C3 -174.5(3) . . . . ?
C1 C2 C3 C4 1.3(7) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C3 C4 C5 C6 -0.3(7) . . . . ?
C4 C5 C6 C1 -0.8(7) . . . . ?
C4 C5 C6 C7 -177.3(4) . . . . ?
C2 C1 C6 C5 2.0(6) . . . . ?
Pb1 C1 C6 C5 175.1(3) . . . . ?
C2 C1 C6 C7 178.6(4) . . . . ?
Pb1 C1 C6 C7 -8.3(5) . . . . ?
C5 C6 C7 N8 -145.7(4) . . . . ?
C1 C6 C7 N8 37.7(5) . . . . ?
C6 C7 N8 C10 -168.7(3) . . . . ?
C6 C7 N8 C9 70.1(4) . . . . ?
C6 C7 N8 Pb1 -42.9(3) . . . . ?
Si2 N11 Si1 C13 173.5(2) . . . . ?
Pb1 N11 Si1 C13 10.3(2) . . . . ?
Si2 N11 Si1 C12 -67.3(3) . . . . ?
Pb1 N11 Si1 C12 129.5(2) . . . . ?
Si2 N11 Si1 C14 55.6(3) . . . . ?
Pb1 N11 Si1 C14 -107.6(2) . . . . ?
Si1 N11 Si2 C17 119.0(3) . . . . ?
Pb1 N11 Si2 C17 -78.4(2) . . . . ?
Si1 N11 Si2 C15 1.1(4) . . . . ?
Pb1 N11 Si2 C15 163.7(3) . . . . ?
Si1 N11 Si2 C16 -117.9(3) . . . . ?
Pb1 N11 Si2 C16 44.7(2) . . . . ?

#----------------------------------------------------------------------------#
#===END OF CIF FILE FOR SAA2                                                 #
#----------------------------------------------------------------------------#
#                                                                            #
##############################################################################
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl Ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1832393'
_audit_update_record             
;
2018-03-26 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C23 H50 B N O Pb Si4'
_chemical_formula_sum            'C23 H50 B N O Pb Si4'
_chemical_formula_weight         687.00
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
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                   9.1319(9)
_cell_length_b                   18.6282(17)
_cell_length_c                   18.929(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.613(4)
_cell_angle_gamma                90
_cell_volume                     3142.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9295
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.49
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1384
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    5.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.122
_exptl_absorpt_correction_T_max  0.296

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0394
_diffrn_reflns_av_uneti/neti     0.0292
_diffrn_reflns_number            35346
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.014
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             7187
_reflns_number_gt                6456
_reflns_threshold_expression     >2sigma(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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0245P)²+2.6997P] 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         7187
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.107

#...............................................................................
# .RES SHELXL file: job.res
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file .............................................
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.50009(2) 0.68552(2) 0.30865(2) 0.01545(4) Uani 1 1 d . . . . .
Si1 Si 0.70446(8) 0.43723(4) 0.27064(4) 0.01377(15) Uani 1 1 d . . . . .
Si2 Si 0.36165(8) 0.39919(4) 0.21071(4) 0.01212(15) Uani 1 1 d . . . . .
Si3 Si 0.57854(9) 0.61809(4) 0.09064(4) 0.01434(15) Uani 1 1 d . . . . .
Si4 Si 0.24315(9) 0.63615(4) 0.11151(4) 0.01497(16) Uani 1 1 d . . . . .
C1 C 0.6899(3) 0.65243(16) 0.40309(16) 0.0172(6) Uani 1 1 d . . . . .
C2 C 0.8404(4) 0.67358(18) 0.41691(19) 0.0248(7) Uani 1 1 d . . . . .
H2 H 0.873509 0.705695 0.384660 0.030 Uiso 1 1 calc R U . . .
C3 C 0.9425(3) 0.6480(2) 0.4776(2) 0.0291(8) Uani 1 1 d . . . . .
H3 H 1.044128 0.663259 0.486580 0.035 Uiso 1 1 calc R U . . .
C4 C 0.8969(4) 0.6008(2) 0.5244(2) 0.0324(8) Uani 1 1 d . . . . .
H4 H 0.967286 0.582565 0.564892 0.039 Uiso 1 1 calc R U . . .
C5 C 0.7471(4) 0.58004(18) 0.51209(18) 0.0256(7) Uani 1 1 d . . . . .
H5 H 0.714718 0.547966 0.544592 0.031 Uiso 1 1 calc R U . . .
C6 C 0.6454(3) 0.60616(16) 0.45242(16) 0.0168(6) Uani 1 1 d . . . . .
C7 C 0.4829(3) 0.58267(16) 0.43879(17) 0.0184(6) Uani 1 1 d . . . . .
H7A H 0.468605 0.540001 0.406843 0.022 Uiso 1 1 calc R U . . .
H7B H 0.458099 0.568798 0.485288 0.022 Uiso 1 1 calc R U . . .
N8 N 0.3803(3) 0.64026(13) 0.40479(14) 0.0164(5) Uani 1 1 d . . . . .
C9 C 0.3788(4) 0.69972(17) 0.45651(18) 0.0240(7) Uani 1 1 d . . . . .
H9A H 0.308547 0.736907 0.433398 0.036 Uiso 1 1 calc R U . . .
H9B H 0.479738 0.720244 0.471010 0.036 Uiso 1 1 calc R U . . .
H9C H 0.347184 0.681375 0.499356 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2281(3) 0.61088(18) 0.37990(18) 0.0228(7) Uani 1 1 d . . . . .
H10A H 0.227912 0.575877 0.341242 0.034 Uiso 1 1 calc R U . . .
H10B H 0.158248 0.649942 0.361461 0.034 Uiso 1 1 calc R U . . .
H10C H 0.196671 0.587282 0.420444 0.034 Uiso 1 1 calc R U . . .
O11 O 0.4882(2) 0.57493(10) 0.26897(10) 0.0143(4) Uani 1 1 d . . . . .
B12 B 0.4764(3) 0.54243(16) 0.20483(17) 0.0093(5) Uani 1 1 d . . . . .
C13 C 0.5242(3) 0.45937(14) 0.20536(14) 0.0106(5) Uani 1 1 d . . . . .
H13 H 0.544582 0.450429 0.156318 0.013 Uiso 1 1 calc R U . . .
C14 C 0.8391(3) 0.51425(17) 0.28924(19) 0.0233(7) Uani 1 1 d . . . . .
H14A H 0.859490 0.531804 0.243546 0.035 Uiso 1 1 calc R U . . .
H14B H 0.932972 0.498276 0.321016 0.035 Uiso 1 1 calc R U . . .
H14C H 0.795206 0.552998 0.312910 0.035 Uiso 1 1 calc R U . . .
C15 C 0.6779(4) 0.4064(2) 0.36179(18) 0.0267(7) Uani 1 1 d . . . . .
H15A H 0.636329 0.445835 0.385595 0.040 Uiso 1 1 calc R U . . .
H15B H 0.774864 0.391849 0.391738 0.040 Uiso 1 1 calc R U . . .
H15C H 0.608591 0.365588 0.355457 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8013(4) 0.36373(17) 0.2300(2) 0.0274(7) Uani 1 1 d . . . . .
H16A H 0.736061 0.321445 0.221031 0.041 Uiso 1 1 calc R U . . .
H16B H 0.895445 0.351084 0.263639 0.041 Uiso 1 1 calc R U . . .
H16C H 0.822875 0.380419 0.184253 0.041 Uiso 1 1 calc R U . . .
C17 C 0.2790(3) 0.42009(17) 0.29021(17) 0.0216(6) Uani 1 1 d . . . . .
H17A H 0.255448 0.471410 0.290339 0.032 Uiso 1 1 calc R U . . .
H17B H 0.351251 0.407761 0.334928 0.032 Uiso 1 1 calc R U . . .
H17C H 0.187001 0.392089 0.287124 0.032 Uiso 1 1 calc R U . . .
C18 C 0.4170(4) 0.30169(16) 0.2139(2) 0.0232(7) Uani 1 1 d . . . . .
H18A H 0.499797 0.293325 0.255615 0.035 Uiso 1 1 calc R U . . .
H18B H 0.448969 0.289031 0.169286 0.035 Uiso 1 1 calc R U . . .
H18C H 0.330885 0.271955 0.218284 0.035 Uiso 1 1 calc R U . . .
C19 C 0.2075(3) 0.40918(18) 0.12778(18) 0.0239(7) Uani 1 1 d . . . . .
H19A H 0.126609 0.375304 0.130156 0.036 Uiso 1 1 calc R U . . .
H19B H 0.246967 0.399131 0.084636 0.036 Uiso 1 1 calc R U . . .
H19C H 0.168367 0.458316 0.125202 0.036 Uiso 1 1 calc R U . . .
C20 C 0.4193(3) 0.57995(14) 0.12714(14) 0.0106(5) Uani 1 1 d . . . . .
H20 H 0.387418 0.537862 0.094625 0.013 Uiso 1 1 calc R U . . .
C21 C 0.1252(3) 0.61375(18) 0.17803(19) 0.0250(7) Uani 1 1 d . . . . .
H21A H 0.178729 0.627456 0.226826 0.037 Uiso 1 1 calc R U . . .
H21B H 0.104994 0.562036 0.176658 0.037 Uiso 1 1 calc R U . . .
H21C H 0.030072 0.640036 0.165380 0.037 Uiso 1 1 calc R U . . .
C22 C 0.1270(4) 0.6150(2) 0.01880(19) 0.0310(8) Uani 1 1 d . . . . .
H22A H 0.108540 0.563195 0.014606 0.047 Uiso 1 1 calc R U . . .
H22B H 0.181085 0.630293 -0.018013 0.047 Uiso 1 1 calc R U . . .
H22C H 0.031063 0.640524 0.011546 0.047 Uiso 1 1 calc R U . . .
C23 C 0.2711(4) 0.73594(17) 0.11542(19) 0.0257(7) Uani 1 1 d . . . . .
H23A H 0.174098 0.759786 0.111866 0.039 Uiso 1 1 calc R U . . .
H23B H 0.315156 0.751257 0.075082 0.039 Uiso 1 1 calc R U . . .
H23C H 0.338634 0.748922 0.161341 0.039 Uiso 1 1 calc R U . . .
C24 C 0.5112(4) 0.65811(19) -0.00167(19) 0.0302(8) Uani 1 1 d . . . . .
H24A H 0.596125 0.679736 -0.017819 0.045 Uiso 1 1 calc R U . . .
H24B H 0.435867 0.695073 0.000335 0.045 Uiso 1 1 calc R U . . .
H24C H 0.466496 0.620441 -0.035750 0.045 Uiso 1 1 calc R U . . .
C25 C 0.6843(4) 0.68845(17) 0.1521(2) 0.0280(7) Uani 1 1 d . . . . .
H25A H 0.727246 0.667156 0.199429 0.042 Uiso 1 1 calc R U . . .
H25B H 0.615877 0.727410 0.157989 0.042 Uiso 1 1 calc R U . . .
H25C H 0.765191 0.707576 0.130996 0.042 Uiso 1 1 calc R U . . .
C26 C 0.7129(3) 0.54520(17) 0.07803(17) 0.0207(6) Uani 1 1 d . . . . .
H26A H 0.659988 0.509438 0.043808 0.031 Uiso 1 1 calc R U . . .
H26B H 0.753833 0.522116 0.124686 0.031 Uiso 1 1 calc R U . . .
H26C H 0.795037 0.566054 0.059016 0.031 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O11 2.1874(19) . ?
Pb1 C1 2.286(3) . ?
Pb1 N8 2.467(2) . ?
Si1 C14 1.872(3) . ?
Si1 C13 1.876(3) . ?
Si1 C16 1.883(3) . ?
Si1 C15 1.884(3) . ?
Si2 C17 1.866(3) . ?
Si2 C19 1.875(3) . ?
Si2 C13 1.880(3) . ?
Si2 C18 1.883(3) . ?
Si3 C25 1.875(3) . ?
Si3 C24 1.876(3) . ?
Si3 C26 1.880(3) . ?
Si3 C20 1.880(3) . ?
Si4 C21 1.874(3) . ?
Si4 C23 1.876(3) . ?
Si4 C22 1.883(3) . ?
Si4 C20 1.888(3) . ?
C1 C6 1.395(4) . ?
C1 C2 1.398(4) . ?
C2 C3 1.395(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.514(4) . ?
C7 N8 1.477(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C10 1.472(4) . ?
N8 C9 1.480(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O11 B12 1.340(4) . ?
B12 C13 1.607(4) . ?
B12 C20 1.609(4) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
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 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Pb1 C1 89.25(9) . . ?
O11 Pb1 N8 86.24(8) . . ?
C1 Pb1 N8 73.37(9) . . ?
C14 Si1 C13 113.65(13) . . ?
C14 Si1 C16 106.64(15) . . ?
C13 Si1 C16 108.30(14) . . ?
C14 Si1 C15 105.77(16) . . ?
C13 Si1 C15 113.59(13) . . ?
C16 Si1 C15 108.58(16) . . ?
C17 Si2 C19 107.02(15) . . ?
C17 Si2 C13 112.45(13) . . ?
C19 Si2 C13 110.66(13) . . ?
C17 Si2 C18 109.20(15) . . ?
C19 Si2 C18 105.62(15) . . ?
C13 Si2 C18 111.56(13) . . ?
C25 Si3 C24 108.65(17) . . ?
C25 Si3 C26 108.75(15) . . ?
C24 Si3 C26 105.01(15) . . ?
C25 Si3 C20 111.79(14) . . ?
C24 Si3 C20 111.72(15) . . ?
C26 Si3 C20 110.64(13) . . ?
C21 Si4 C23 106.70(15) . . ?
C21 Si4 C22 106.87(16) . . ?
C23 Si4 C22 106.74(16) . . ?
C21 Si4 C20 111.50(13) . . ?
C23 Si4 C20 116.07(13) . . ?
C22 Si4 C20 108.49(14) . . ?
C6 C1 C2 117.8(3) . . ?
C6 C1 Pb1 114.1(2) . . ?
C2 C1 Pb1 128.1(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.4(3) . . ?
C5 C6 C7 119.7(3) . . ?
C1 C6 C7 118.8(3) . . ?
N8 C7 C6 111.7(2) . . ?
N8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
N8 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C10 N8 C7 109.6(2) . . ?
C10 N8 C9 110.2(2) . . ?
C7 N8 C9 110.6(2) . . ?
C10 N8 Pb1 115.52(19) . . ?
C7 N8 Pb1 103.20(16) . . ?
C9 N8 Pb1 107.55(18) . . ?
N8 C9 H9A 109.5 . . ?
N8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N8 C10 H10A 109.5 . . ?
N8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
B12 O11 Pb1 136.46(18) . . ?
O11 B12 C13 117.5(2) . . ?
O11 B12 C20 125.3(2) . . ?
C13 B12 C20 117.2(2) . . ?
B12 C13 Si1 114.44(18) . . ?
B12 C13 Si2 110.98(17) . . ?
Si1 C13 Si2 115.02(14) . . ?
B12 C13 H13 105.1 . . ?
Si1 C13 H13 105.1 . . ?
Si2 C13 H13 105.1 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
B12 C20 Si3 112.20(17) . . ?
B12 C20 Si4 118.63(18) . . ?
Si3 C20 Si4 115.71(14) . . ?
B12 C20 H20 102.4 . . ?
Si3 C20 H20 102.4 . . ?
Si4 C20 H20 102.4 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si4 C23 H23A 109.5 . . ?
Si4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si3 C24 H24A 109.5 . . ?
Si3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si3 C25 H25A 109.5 . . ?
Si3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si3 C26 H26A 109.5 . . ?
Si3 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si3 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.1(5) . . . . ?
Pb1 C1 C2 C3 -179.9(2) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C2 C3 C4 C5 -1.7(5) . . . . ?
C3 C4 C5 C6 0.8(5) . . . . ?
C4 C5 C6 C1 1.0(5) . . . . ?
C4 C5 C6 C7 179.3(3) . . . . ?
C2 C1 C6 C5 -1.9(4) . . . . ?
Pb1 C1 C6 C5 178.9(2) . . . . ?
C2 C1 C6 C7 179.8(3) . . . . ?
Pb1 C1 C6 C7 0.7(3) . . . . ?
C5 C6 C7 N8 147.0(3) . . . . ?
C1 C6 C7 N8 -34.7(4) . . . . ?
C6 C7 N8 C10 169.1(2) . . . . ?
C6 C7 N8 C9 -69.2(3) . . . . ?
C6 C7 N8 Pb1 45.6(3) . . . . ?
Pb1 O11 B12 C13 160.78(17) . . . . ?
Pb1 O11 B12 C20 -18.8(4) . . . . ?
O11 B12 C13 Si1 -44.7(3) . . . . ?
C20 B12 C13 Si1 134.9(2) . . . . ?
O11 B12 C13 Si2 87.5(2) . . . . ?
C20 B12 C13 Si2 -92.9(2) . . . . ?
C14 Si1 C13 B12 -28.0(2) . . . . ?
C16 Si1 C13 B12 -146.3(2) . . . . ?
C15 Si1 C13 B12 93.0(2) . . . . ?
C14 Si1 C13 Si2 -158.21(15) . . . . ?
C16 Si1 C13 Si2 83.48(18) . . . . ?
C15 Si1 C13 Si2 -37.2(2) . . . . ?
C17 Si2 C13 B12 -55.4(2) . . . . ?
C19 Si2 C13 B12 64.2(2) . . . . ?
C18 Si2 C13 B12 -178.5(2) . . . . ?
C17 Si2 C13 Si1 76.49(18) . . . . ?
C19 Si2 C13 Si1 -163.88(15) . . . . ?
C18 Si2 C13 Si1 -46.6(2) . . . . ?
O11 B12 C20 Si3 92.2(3) . . . . ?
C13 B12 C20 Si3 -87.4(2) . . . . ?
O11 B12 C20 Si4 -47.0(3) . . . . ?
C13 B12 C20 Si4 133.4(2) . . . . ?
C25 Si3 C20 B12 -60.4(2) . . . . ?
C24 Si3 C20 B12 177.5(2) . . . . ?
C26 Si3 C20 B12 60.9(2) . . . . ?
C25 Si3 C20 Si4 79.98(19) . . . . ?
C24 Si3 C20 Si4 -42.0(2) . . . . ?
C26 Si3 C20 Si4 -158.65(15) . . . . ?
C21 Si4 C20 B12 -20.0(2) . . . . ?
C23 Si4 C20 B12 102.4(2) . . . . ?
C22 Si4 C20 B12 -137.4(2) . . . . ?
C21 Si4 C20 Si3 -157.80(16) . . . . ?
C23 Si4 C20 Si3 -35.3(2) . . . . ?
C22 Si4 C20 Si3 84.77(19) . . . . ?

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR SAA29                                                  #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_chemical_melting_point          414
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
