# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 2179096'
loop_
_audit_author_name
_audit_author_address
'Roberto Diaz-Rodriguez'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H56 Na2 O2 Pb Si2'
_chemical_formula_sum            'C36 H56 Na2 O2 Pb Si2'
_chemical_formula_weight         830.15

#=============================================================
# CRYSTAL DATA

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'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   29.422(2)
_cell_length_b                   10.6642(9)
_cell_length_c                   29.458(2)
_cell_angle_alpha                90
_cell_angle_beta                 111.437(8)
_cell_angle_gamma                90
_cell_volume                     8603.6(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.44

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_F_000             3360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.023
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5232
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?

#=============================================================
# EXPERIMENTAL DATA

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      203(2)
_diffrn_reflns_number            67463
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_av_R_equivalents  0.1933
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.485
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996

#=============================================================
# REFINEMENT DATA

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

_reflns_number_total             7553
_reflns_number_gt                4459
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7553
_refine_ls_number_parameters     398
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0563P)²] where P=(Fo²+2Fc²)/3'
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.133

#=============================================================
# GENERAL COMPUTING 

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#=============================================================
# ATOMIC COORDINATES AND THERMAL PARAMETER

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5024(3) 0.2324(7) 0.6580(3) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.5385(3) 0.1355(7) 0.6711(3) 0.030(2) Uani 1 1 d . . . . .
C3 C 0.5830(3) 0.1497(7) 0.7133(3) 0.028(2) Uani 1 1 d . . . . .
C4 C 0.5915(3) 0.2624(7) 0.7409(3) 0.034(2) Uani 1 1 d . . . . .
C5 C 0.4481(4) 0.4893(8) 0.5721(4) 0.072(4) Uani 1 1 d . . . . .
H5A H 0.476130 0.500132 0.602065 0.108 Uiso 1 1 calc R U . . .
H5B H 0.418674 0.513773 0.577380 0.108 Uiso 1 1 calc R U . . .
H5C H 0.451977 0.541258 0.546714 0.108 Uiso 1 1 calc R U . . .
C6 C 0.3969(5) 0.3384(12) 0.5110(4) 0.108(5) Uani 1 1 d . . . . .
H6A H 0.368620 0.350425 0.520109 0.163 Uiso 1 1 calc R U . . .
H6B H 0.396029 0.254647 0.497869 0.163 Uiso 1 1 calc R U . . .
H6C H 0.396360 0.399790 0.486569 0.163 Uiso 1 1 calc R U . . .
C7 C 0.4876(4) 0.3264(11) 0.5411(4) 0.083(4) Uani 1 1 d . . . . .
H7A H 0.485576 0.378965 0.513562 0.125 Uiso 1 1 calc R U . . .
H7B H 0.486710 0.238889 0.531832 0.125 Uiso 1 1 calc R U . . .
H7C H 0.517955 0.343435 0.568040 0.125 Uiso 1 1 calc R U . . .
C8 C 0.4443(4) 0.3547(7) 0.5568(3) 0.042(2) Uani 1 1 d . . . . .
C9 C 0.4166(3) 0.0866(8) 0.5762(3) 0.052(3) Uani 1 1 d . . . . .
H9A H 0.437858 0.052495 0.560720 0.079 Uiso 1 1 calc R U . . .
H9B H 0.384372 0.100837 0.551803 0.079 Uiso 1 1 calc R U . . .
H9C H 0.414264 0.027713 0.600374 0.079 Uiso 1 1 calc R U . . .
C10 C 0.3961(3) 0.3045(9) 0.6300(3) 0.056(3) Uani 1 1 d . . . . .
H10A H 0.391397 0.246085 0.653085 0.085 Uiso 1 1 calc R U . . .
H10B H 0.365508 0.316260 0.602810 0.085 Uiso 1 1 calc R U . . .
H10C H 0.407255 0.384376 0.645923 0.085 Uiso 1 1 calc R U . . .
C11 C 0.5301(3) 0.0204(7) 0.6400(3) 0.028(2) Uani 1 1 d . . . . .
C12 C 0.5101(3) -0.0892(8) 0.6493(3) 0.045(2) Uani 1 1 d . . . . .
H12 H 0.502517 -0.093067 0.677693 0.054 Uiso 1 1 calc R U . . .
C13 C 0.5005(4) -0.1928(8) 0.6197(4) 0.056(3) Uani 1 1 d . . . . .
H13 H 0.487585 -0.265683 0.628343 0.067 Uiso 1 1 calc R U . . .
C14 C 0.5098(4) -0.1898(9) 0.5770(4) 0.056(3) Uani 1 1 d . . . . .
H14 H 0.502884 -0.258972 0.555832 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5297(4) -0.0816(8) 0.5668(3) 0.050(3) Uani 1 1 d . . . . .
H15 H 0.536188 -0.076903 0.537878 0.060 Uiso 1 1 calc R U . . .
C16 C 0.5402(3) 0.0194(8) 0.5976(3) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.554815 0.090400 0.589780 0.046 Uiso 1 1 calc R U . . .
C17 C 0.6198(3) 0.0448(8) 0.7272(3) 0.033(2) Uani 1 1 d . . . . .
C18 C 0.6632(3) 0.0511(9) 0.7183(3) 0.049(3) Uani 1 1 d . . . . .
H18 H 0.669561 0.122332 0.702726 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6973(4) -0.0461(11) 0.7319(4) 0.062(3) Uani 1 1 d . . . . .
H19 H 0.726006 -0.039788 0.725012 0.074 Uiso 1 1 calc R U . . .
C20 C 0.6898(4) -0.1499(10) 0.7552(3) 0.055(3) Uani 1 1 d . . . . .
H20 H 0.713384 -0.213704 0.765327 0.067 Uiso 1 1 calc R U . . .
C21 C 0.6466(4) -0.1593(9) 0.7634(4) 0.059(3) Uani 1 1 d . . . . .
H21 H 0.640422 -0.231378 0.778607 0.071 Uiso 1 1 calc R U . . .
C22 C 0.6127(4) -0.0647(8) 0.7498(3) 0.045(3) Uani 1 1 d . . . . .
H22 H 0.583670 -0.073959 0.755790 0.054 Uiso 1 1 calc R U . . .
C23 C 0.7024(4) 0.3341(11) 0.7799(4) 0.079(3) Uani 1 1 d . U . . .
H23A H 0.712985 0.251163 0.774379 0.119 Uiso 1 1 calc R U . . .
H23B H 0.727641 0.372577 0.807546 0.119 Uiso 1 1 calc R U . . .
H23C H 0.696578 0.385334 0.751085 0.119 Uiso 1 1 calc R U . . .
C24 C 0.6321(4) 0.4876(10) 0.8046(4) 0.085(3) Uani 1 1 d . U . . .
H24A H 0.622174 0.534650 0.774329 0.128 Uiso 1 1 calc R U . . .
H24B H 0.661523 0.524513 0.827930 0.128 Uiso 1 1 calc R U . . .
H24C H 0.606285 0.489918 0.817629 0.128 Uiso 1 1 calc R U . . .
C25 C 0.6152(5) 0.2005(14) 0.8616(4) 0.112(5) Uani 1 1 d . . . . .
H25A H 0.594380 0.149731 0.834694 0.167 Uiso 1 1 calc R U . . .
H25B H 0.597883 0.275738 0.864256 0.167 Uiso 1 1 calc R U . . .
H25C H 0.624219 0.152937 0.891634 0.167 Uiso 1 1 calc R U . . .
C26 C 0.6920(5) 0.1194(11) 0.8557(5) 0.107(5) Uani 1 1 d . U . . .
H26A H 0.695059 0.071565 0.884631 0.161 Uiso 1 1 calc R U . . .
H26B H 0.724145 0.145903 0.857355 0.161 Uiso 1 1 calc R U . . .
H26C H 0.677089 0.067608 0.826982 0.161 Uiso 1 1 calc R U . . .
C27 C 0.6921(4) 0.3190(11) 0.8960(3) 0.079(4) Uani 1 1 d . . . . .
H27A H 0.672869 0.388752 0.900253 0.119 Uiso 1 1 calc R U . . .
H27B H 0.719868 0.350820 0.889239 0.119 Uiso 1 1 calc R U . . .
H27C H 0.703632 0.269189 0.925623 0.119 Uiso 1 1 calc R U . . .
C28 C 0.6599(3) 0.2357(9) 0.8525(3) 0.047(3) Uani 1 1 d . . . . .
C29 C 0.6091(5) 0.6124(13) 0.6400(6) 0.113(4) Uani 1 1 d . U . . .
H29A H 0.603615 0.631289 0.670118 0.135 Uiso 1 1 calc R U . . .
H29B H 0.577189 0.606564 0.613419 0.135 Uiso 1 1 calc R U . . .
C30 C 0.6373(6) 0.7138(13) 0.6296(6) 0.117(4) Uani 1 1 d . U . . .
H30A H 0.620797 0.746791 0.596566 0.140 Uiso 1 1 calc R U . . .
H30B H 0.642559 0.782444 0.653088 0.140 Uiso 1 1 calc R U . . .
C31 C 0.6829(5) 0.6541(14) 0.6343(6) 0.122(4) Uani 1 1 d . U . . .
H31A H 0.710230 0.698903 0.658377 0.147 Uiso 1 1 calc R U . . .
H31B H 0.687409 0.655636 0.602970 0.147 Uiso 1 1 calc R U . . .
C32 C 0.6814(5) 0.5218(14) 0.6503(6) 0.118(4) Uani 1 1 d . U . . .
H32A H 0.691789 0.463962 0.630115 0.141 Uiso 1 1 calc R U . . .
H32B H 0.703063 0.511073 0.684455 0.141 Uiso 1 1 calc R U . . .
C33 C 0.6191(5) 0.2941(14) 0.5496(5) 0.113(3) Uani 1 1 d . U . . .
H33A H 0.583798 0.304971 0.533354 0.136 Uiso 1 1 calc R U . . .
H33B H 0.634586 0.377012 0.554438 0.136 Uiso 1 1 calc R U . . .
C34 C 0.6379(6) 0.2168(15) 0.5205(5) 0.124(4) Uani 1 1 d . U . . .
H34A H 0.666761 0.256100 0.517530 0.149 Uiso 1 1 calc R U . . .
H34B H 0.613121 0.206757 0.487719 0.149 Uiso 1 1 calc R U . . .
C35 C 0.6508(6) 0.0946(14) 0.5441(5) 0.117(4) Uani 1 1 d . U . . .
H35A H 0.681193 0.063140 0.541904 0.141 Uiso 1 1 calc R U . . .
H35B H 0.624741 0.033227 0.529212 0.141 Uiso 1 1 calc R U . . .
C36 C 0.6567(5) 0.1199(12) 0.5957(4) 0.089(3) Uani 1 1 d . U . . .
H36A H 0.644012 0.049534 0.608894 0.107 Uiso 1 1 calc R U . . .
H36B H 0.691352 0.131045 0.615750 0.107 Uiso 1 1 calc R U . . .
Na1 Na 0.59758(13) 0.3148(4) 0.65252(12) 0.0511(10) Uani 1 1 d . . . . .
Na2 Na 0.50939(14) 0.1311(3) 0.74749(13) 0.0505(10) Uani 1 1 d . . . . .
O1 O 0.6331(3) 0.4989(7) 0.6449(3) 0.082(2) Uani 1 1 d . U . . .
O2 O 0.6301(3) 0.2318(7) 0.5961(3) 0.077(2) Uani 1 1 d . U . . .
Pb Pb 0.52649(2) 0.39407(3) 0.71030(2) 0.03856(13) Uani 1 1 d . . . . .
Si1 Si 0.44265(9) 0.2409(2) 0.60712(9) 0.0373(6) Uani 1 1 d . . . . .
Si2 Si 0.64458(10) 0.3208(3) 0.79269(9) 0.0455(7) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.429(11) . ?
C1 Si1 1.850(9) . ?
C1 Pb 2.247(8) . ?
C1 Na2 2.786(8) . ?
C1 Na1 2.994(9) . ?
C2 C3 1.449(11) . ?
C2 C11 1.498(10) . ?
C2 Na2 2.684(8) . ?
C2 Na1 2.771(8) . ?
C3 C4 1.420(10) . ?
C3 C17 1.505(11) . ?
C3 Na1 2.655(8) . ?
C3 Na2 2.710(8) . ?
C4 Si2 1.848(8) . ?
C4 Pb 2.275(8) . ?
C4 Na1 2.732(8) . ?
C4 Na2 2.859(9) . ?
C5 C8 1.496(11) . ?
C6 C8 1.556(14) . ?
C7 C8 1.537(13) . ?
C8 Si1 1.930(9) . ?
C9 Si1 1.901(8) . ?
C10 Si1 1.860(9) . ?
C11 C12 1.382(11) . ?
C11 C16 1.384(10) . ?
C12 C13 1.373(11) . ?
C13 C14 1.380(12) . ?
C14 C15 1.375(12) . ?
C15 C16 1.370(11) . ?
C17 C18 1.396(11) . ?
C17 C22 1.396(11) . ?
C18 C19 1.397(13) . ?
C19 C20 1.361(13) . ?
C20 C21 1.381(13) . ?
C21 C22 1.371(12) . ?
C23 Si2 1.879(11) . ?
C24 Si2 1.875(11) . ?
C25 C28 1.481(13) . ?
C26 C28 1.541(14) . ?
C27 C28 1.563(12) . ?
C28 Si2 1.885(9) . ?
C29 O1 1.382(14) . ?
C29 C30 1.462(16) . ?
C30 C31 1.445(18) . ?
C31 C32 1.494(17) . ?
C32 O1 1.392(13) . ?
C33 C34 1.437(16) . ?
C33 O2 1.448(13) . ?
C34 C35 1.460(17) . ?
C35 C36 1.490(15) . ?
C36 O2 1.430(12) . ?
Na1 O1 2.274(8) . ?
Na1 O2 2.372(7) . ?
Na1 Pb 3.254(3) . ?
Na2 Pb 3.118(3) . ?
Na2 Pb 3.164(3) 4_546 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Si1 130.2(6) . . ?
C2 C1 Pb 110.7(6) . . ?
Si1 C1 Pb 119.1(4) . . ?
C2 C1 Na2 70.9(4) . . ?
Si1 C1 Na2 120.3(4) . . ?
Pb C1 Na2 75.7(2) . . ?
C2 C1 Na1 67.1(5) . . ?
Si1 C1 Na1 125.0(4) . . ?
Pb C1 Na1 75.3(2) . . ?
Na2 C1 Na1 114.7(3) . . ?
C1 C2 C3 120.4(7) . . ?
C1 C2 C11 119.3(7) . . ?
C3 C2 C11 120.4(7) . . ?
C1 C2 Na2 78.8(5) . . ?
C3 C2 Na2 75.4(4) . . ?
C11 C2 Na2 117.9(5) . . ?
C1 C2 Na1 84.5(5) . . ?
C3 C2 Na1 70.2(4) . . ?
C11 C2 Na1 114.8(5) . . ?
Na2 C2 Na1 126.4(3) . . ?
C4 C3 C2 119.6(7) . . ?
C4 C3 C17 121.1(7) . . ?
C2 C3 C17 119.4(7) . . ?
C4 C3 Na1 77.7(5) . . ?
C2 C3 Na1 79.0(5) . . ?
C17 C3 Na1 113.5(5) . . ?
C4 C3 Na2 81.1(5) . . ?
C2 C3 Na2 73.5(4) . . ?
C17 C3 Na2 116.0(5) . . ?
Na1 C3 Na2 130.3(3) . . ?
C3 C4 Si2 132.5(7) . . ?
C3 C4 Pb 110.5(6) . . ?
Si2 C4 Pb 117.0(4) . . ?
C3 C4 Na1 71.8(4) . . ?
Si2 C4 Na1 112.8(4) . . ?
Pb C4 Na1 80.5(3) . . ?
C3 C4 Na2 69.5(4) . . ?
Si2 C4 Na2 126.1(4) . . ?
Pb C4 Na2 73.8(2) . . ?
Na1 C4 Na2 121.1(3) . . ?
C5 C8 C7 107.5(8) . . ?
C5 C8 C6 108.3(8) . . ?
C7 C8 C6 107.3(9) . . ?
C5 C8 Si1 113.1(6) . . ?
C7 C8 Si1 111.3(6) . . ?
C6 C8 Si1 109.2(7) . . ?
C12 C11 C16 114.9(8) . . ?
C12 C11 C2 123.9(7) . . ?
C16 C11 C2 121.1(7) . . ?
C13 C12 C11 123.8(9) . . ?
C12 C13 C14 119.8(9) . . ?
C15 C14 C13 117.5(9) . . ?
C16 C15 C14 121.7(8) . . ?
C15 C16 C11 122.2(8) . . ?
C18 C17 C22 115.8(8) . . ?
C18 C17 C3 121.9(8) . . ?
C22 C17 C3 122.3(8) . . ?
C17 C18 C19 121.4(9) . . ?
C20 C19 C18 121.1(9) . . ?
C19 C20 C21 118.5(10) . . ?
C22 C21 C20 120.8(9) . . ?
C21 C22 C17 122.4(9) . . ?
C25 C28 C26 110.5(10) . . ?
C25 C28 C27 108.0(9) . . ?
C26 C28 C27 103.5(9) . . ?
C25 C28 Si2 111.4(7) . . ?
C26 C28 Si2 112.0(7) . . ?
C27 C28 Si2 111.1(7) . . ?
O1 C29 C30 111.2(12) . . ?
C31 C30 C29 103.4(12) . . ?
C30 C31 C32 108.3(12) . . ?
O1 C32 C31 105.9(12) . . ?
C34 C33 O2 107.4(12) . . ?
C33 C34 C35 108.5(12) . . ?
C34 C35 C36 103.7(11) . . ?
O2 C36 C35 107.4(10) . . ?
O1 Na1 O2 86.3(3) . . ?
O1 Na1 C3 146.4(3) . . ?
O2 Na1 C3 115.5(3) . . ?
O1 Na1 C4 117.6(3) . . ?
O2 Na1 C4 140.9(3) . . ?
C3 Na1 C4 30.5(2) . . ?
O1 Na1 C2 163.7(3) . . ?
O2 Na1 C2 108.9(3) . . ?
C3 Na1 C2 30.9(2) . . ?
C4 Na1 C2 53.5(2) . . ?
O1 Na1 C1 137.0(3) . . ?
O2 Na1 C1 123.6(3) . . ?
C3 Na1 C1 52.0(2) . . ?
C4 Na1 C1 60.0(2) . . ?
C2 Na1 C1 28.4(2) . . ?
O1 Na1 Pb 103.6(2) . . ?
O2 Na1 Pb 164.7(2) . . ?
C3 Na1 Pb 61.74(18) . . ?
C4 Na1 Pb 43.61(18) . . ?
C2 Na1 Pb 60.40(17) . . ?
C1 Na1 Pb 41.89(15) . . ?
C2 Na2 C3 31.2(2) . . ?
C2 Na2 C1 30.2(2) . . ?
C3 Na2 C1 54.0(3) . . ?
C2 Na2 C4 53.0(2) . . ?
C3 Na2 C4 29.4(2) . . ?
C1 Na2 C4 61.1(2) . . ?
C2 Na2 Pb 63.12(18) . . ?
C3 Na2 Pb 63.25(18) . . ?
C1 Na2 Pb 44.29(17) . . ?
C4 Na2 Pb 44.50(17) . . ?
C2 Na2 Pb 126.7(2) . 4_546 ?
C3 Na2 Pb 129.2(2) . 4_546 ?
C1 Na2 Pb 139.6(2) . 4_546 ?
C4 Na2 Pb 146.0(2) . 4_546 ?
Pb Na2 Pb 167.60(12) . 4_546 ?
C29 O1 C32 108.7(10) . . ?
C29 O1 Na1 122.0(8) . . ?
C32 O1 Na1 128.8(8) . . ?
C36 O2 C33 108.0(9) . . ?
C36 O2 Na1 132.8(6) . . ?
C33 O2 Na1 119.0(7) . . ?
C1 Pb C4 78.8(3) . . ?
C1 Pb Na2 60.0(2) . . ?
C4 Pb Na2 61.7(2) . . ?
C1 Pb Na2 144.7(2) . 4_556 ?
C4 Pb Na2 133.6(2) . 4_556 ?
Na2 Pb Na2 117.431(17) . 4_556 ?
C1 Pb Na1 62.9(2) . . ?
C4 Pb Na1 55.9(2) . . ?
Na2 Pb Na1 99.64(9) . . ?
Na2 Pb Na1 141.59(9) 4_556 . ?
C1 Si1 C10 109.4(4) . . ?
C1 Si1 C9 116.3(4) . . ?
C10 Si1 C9 105.5(4) . . ?
C1 Si1 C8 111.7(4) . . ?
C10 Si1 C8 106.1(4) . . ?
C9 Si1 C8 107.2(4) . . ?
C4 Si2 C24 108.1(4) . . ?
C4 Si2 C23 114.5(4) . . ?
C24 Si2 C23 102.7(5) . . ?
C4 Si2 C28 116.8(4) . . ?
C24 Si2 C28 106.2(5) . . ?
C23 Si2 C28 107.4(5) . . ?

# start Validation Reply Form

_vrf_RINTA01_4a                  
;
RESPONSE: Several crystals of the title compound were carefully
tested on the X-rays (MoKa radiation) at 203 K.
The diffraction quality of the crystals has proven to be moderate
and structure determination was eventually carried out by means of the
best data set collected.
As a necessary compromise between resolution and data completeness
we have used data up to 25 degrees with a completeness of 99.6%. 
;

_vrf_PLAT605_4a                  
;
RESPONSE: The structure contains an area of disordered 
solvent involving one toluene molecule with partial occupancy; attempts 
to model it with a chemically reasonable geometry were unsuccessful. 
Therefore, the SQUEEZE procedure of PLATON (A.L.Spek (2015) Acta Cryst. C71, 
9-18) was employed to remove the contribution of the electron 
density associated with those solvent molecules from the intensity 
data. The solvent-free model and intensity data were used for the 
final results reported here.  
;

_vrf_PLAT869_4a                  
; 
RESPONSE:See comment above.
;

# end Validation Reply Form






_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Alkanes/tetrahydrofuran'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-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_1
_database_code_depnum_ccdc_archive 'CCDC 2179098'
loop_
_audit_author_name
_audit_author_address
'Roberto Diaz-Rodriguez'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H56 K2 O2 Pb Si2'
_chemical_formula_sum            'C36 H56 K2 O2 Pb Si2'
_chemical_formula_weight         862.37

#=============================================================
# CRYSTAL DATA

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'
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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n 21 a'
_space_group_name_Hall           'P -2ac -2n'

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

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

_cell_length_a                   13.9365(3)
_cell_length_b                   19.0723(3)
_cell_length_c                   15.3540(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4081.11(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.05

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.424
_shelx_estimated_absorpt_T_min   0.393
_shelx_estimated_absorpt_T_max   0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?

#=============================================================
# EXPERIMENTAL DATA

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      213(2)
_diffrn_reflns_number            50293
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.973
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.977

#=============================================================
# REFINEMENT DATA

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_reflns_number_total             8719
_reflns_number_gt                6535
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_max     0.935
_reflns_Friedel_fraction_full    0.952
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,Disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.190(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8719
_refine_ls_number_parameters     399
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_ref         0.0434
_refine_ls_wR_factor_gt          0.0387
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+2.8987P] where P=(Fo²+2Fc²)/3'
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.063

#=============================================================
# GENERAL COMPUTING 

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#=============================================================
# ATOMIC COORDINATES AND THERMAL PARAMETER

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2520(5) 0.8917(3) 0.3329(4) 0.0258(16) Uani 1 1 d . . . . .
C2 C 0.1998(5) 0.8560(3) 0.3980(4) 0.0232(15) Uani 1 1 d . . . . .
C3 C 0.2040(6) 0.7808(4) 0.4034(4) 0.0256(16) Uani 1 1 d . . . . .
C4 C 0.2611(5) 0.7429(3) 0.3436(4) 0.0261(15) Uani 1 1 d . . . . .
C5 C 0.1379(6) 0.8938(3) 0.4634(5) 0.0277(16) Uani 1 1 d . . . . .
C6 C 0.0566(5) 0.9306(3) 0.4399(4) 0.0391(16) Uani 1 1 d . . . . .
H6 H 0.037203 0.930752 0.381234 0.047 Uiso 1 1 calc R U . . .
C7 C 0.0026(6) 0.9675(4) 0.5007(6) 0.054(2) Uani 1 1 d . . . . .
H7 H -0.052762 0.991767 0.483134 0.065 Uiso 1 1 calc R U . . .
C8 C 0.0301(7) 0.9685(5) 0.5860(6) 0.055(3) Uani 1 1 d . . . . .
H8 H -0.005700 0.994119 0.626994 0.066 Uiso 1 1 calc R U . . .
C9 C 0.1095(7) 0.9323(4) 0.6116(5) 0.052(2) Uani 1 1 d . . . . .
H9 H 0.127843 0.932448 0.670521 0.062 Uiso 1 1 calc R U . . .
C10 C 0.1630(5) 0.8954(4) 0.5516(4) 0.0379(17) Uani 1 1 d . . . . .
H10 H 0.217535 0.870686 0.570372 0.045 Uiso 1 1 calc R U . . .
C11 C 0.1440(6) 0.7429(4) 0.4690(6) 0.0307(18) Uani 1 1 d . . . . .
C12 C 0.1845(6) 0.7159(4) 0.5440(5) 0.0444(19) Uani 1 1 d . . . . .
H12 H 0.250110 0.722976 0.555133 0.053 Uiso 1 1 calc R U . . .
C13 C 0.1292(8) 0.6783(4) 0.6031(6) 0.060(2) Uani 1 1 d . . . . .
H13 H 0.157984 0.660772 0.653944 0.072 Uiso 1 1 calc R U . . .
C14 C 0.0342(10) 0.6664(5) 0.5889(7) 0.074(4) Uani 1 1 d . . . . .
H14 H -0.001983 0.639563 0.628396 0.089 Uiso 1 1 calc R U . . .
C15 C -0.0074(7) 0.6941(5) 0.5166(7) 0.074(3) Uani 1 1 d . . . . .
H15 H -0.073059 0.686652 0.506025 0.089 Uiso 1 1 calc R U . . .
C16 C 0.0469(6) 0.7334(4) 0.4578(5) 0.0528(19) Uani 1 1 d . . . . .
H16 H 0.016463 0.753944 0.409509 0.063 Uiso 1 1 calc R U . . .
C17 C 0.1537(5) 1.0291(3) 0.2606(4) 0.0551(18) Uani 1 1 d . . . . .
H17A H 0.105640 1.033181 0.305961 0.083 Uiso 1 1 calc R U . . .
H17B H 0.128427 1.001166 0.213043 0.083 Uiso 1 1 calc R U . . .
H17C H 0.170227 1.075457 0.239264 0.083 Uiso 1 1 calc R U . . .
C18 C 0.3543(6) 0.9936(4) 0.2144(5) 0.061(2) Uani 1 1 d . . . . .
H18A H 0.338867 0.959946 0.169171 0.091 Uiso 1 1 calc R U . . .
H18B H 0.418470 0.984513 0.236188 0.091 Uiso 1 1 calc R U . . .
H18C H 0.351426 1.040662 0.190631 0.091 Uiso 1 1 calc R U . . .
C19 C 0.2287(6) 1.0755(4) 0.4519(4) 0.0612(19) Uani 1 1 d . . . . .
H19A H 0.254384 1.102127 0.500433 0.092 Uiso 1 1 calc R U . . .
H19B H 0.188936 1.037696 0.473813 0.092 Uiso 1 1 calc R U . . .
H19C H 0.190273 1.106142 0.415392 0.092 Uiso 1 1 calc R U . . .
C20 C 0.3111(5) 1.0452(3) 0.3985(4) 0.0417(14) Uani 1 1 d . . . . .
C21 C 0.3754(8) 1.0035(5) 0.4591(7) 0.073(3) Uani 1 1 d . . . . .
H21A H 0.337771 0.967784 0.488498 0.109 Uiso 1 1 calc R U . . .
H21B H 0.403487 1.034668 0.502016 0.109 Uiso 1 1 calc R U . . .
H21C H 0.426022 0.981279 0.425683 0.109 Uiso 1 1 calc R U . . .
C22 C 0.3680(8) 1.1067(4) 0.3594(7) 0.074(3) Uani 1 1 d . . . . .
H22A H 0.425749 1.089035 0.331762 0.111 Uiso 1 1 calc R U . . .
H22B H 0.385406 1.139252 0.405324 0.111 Uiso 1 1 calc R U . . .
H22C H 0.328830 1.130641 0.316489 0.111 Uiso 1 1 calc R U . . .
C23 C 0.2802(6) 0.6311(4) 0.2039(4) 0.0544(19) Uani 1 1 d . . . . .
H23A H 0.333913 0.656643 0.179342 0.082 Uiso 1 1 calc R U . . .
H23B H 0.221116 0.646664 0.176693 0.082 Uiso 1 1 calc R U . . .
H23C H 0.288730 0.581295 0.193524 0.082 Uiso 1 1 calc R U . . .
C24 C 0.1724(5) 0.5911(3) 0.3635(5) 0.0580(18) Uani 1 1 d . . . . .
H24A H 0.112009 0.610660 0.343637 0.087 Uiso 1 1 calc R U . . .
H24B H 0.172872 0.589352 0.426647 0.087 Uiso 1 1 calc R U . . .
H24C H 0.179969 0.544143 0.340345 0.087 Uiso 1 1 calc R U . . .
C25 C 0.3903(5) 0.6097(3) 0.3736(4) 0.0443(15) Uani 1 1 d . . . . .
C26 C 0.3888(8) 0.6175(5) 0.4727(6) 0.071(3) Uani 1 1 d . . . . .
H26A H 0.378627 0.666271 0.487875 0.107 Uiso 1 1 calc R U . . .
H26B H 0.449571 0.601761 0.496545 0.107 Uiso 1 1 calc R U . . .
H26C H 0.337210 0.589251 0.496631 0.107 Uiso 1 1 calc R U . . .
C27 C 0.3975(8) 0.5317(4) 0.3521(7) 0.068(3) Uani 1 1 d . . . . .
H27A H 0.453488 0.511931 0.380560 0.102 Uiso 1 1 calc R U . . .
H27B H 0.403368 0.525717 0.289565 0.102 Uiso 1 1 calc R U . . .
H27C H 0.340322 0.507790 0.372465 0.102 Uiso 1 1 calc R U . . .
C28 C 0.4775(5) 0.6464(4) 0.3391(6) 0.072(2) Uani 1 1 d . . . . .
H28A H 0.534615 0.625711 0.364446 0.108 Uiso 1 1 calc R U . . .
H28B H 0.474529 0.695720 0.354150 0.108 Uiso 1 1 calc R U . . .
H28C H 0.479791 0.641440 0.276213 0.108 Uiso 1 1 calc R U . . .
C29 C 0.4241(12) 0.8698(9) 0.6955(8) 0.133(3) Uani 1 1 d D U . . .
H29A H 0.383565 0.907631 0.673034 0.160 Uiso 1 1 calc R U . . .
H29B H 0.488391 0.888715 0.706396 0.160 Uiso 1 1 calc R U . . .
C30 C 0.3837(12) 0.8421(7) 0.7759(7) 0.136(3) Uani 1 1 d D U . . .
H30A H 0.328167 0.870077 0.793893 0.164 Uiso 1 1 calc R U . . .
H30B H 0.431635 0.843492 0.822617 0.164 Uiso 1 1 calc R U . . .
C31 C 0.3542(10) 0.7686(8) 0.7586(7) 0.121(3) Uani 1 1 d D U . . .
H31A H 0.363178 0.738571 0.809805 0.145 Uiso 1 1 calc R U . . .
H31B H 0.287376 0.765644 0.739018 0.145 Uiso 1 1 calc R U . . .
C32 C 0.4225(12) 0.7509(9) 0.6879(8) 0.131(3) Uani 1 1 d D U . . .
H32A H 0.398017 0.712550 0.651662 0.157 Uiso 1 1 calc R U . . .
H32B H 0.485266 0.737523 0.711489 0.157 Uiso 1 1 calc R U . . .
C33 C 0.6430(8) 0.8907(5) 0.4593(7) 0.074(3) Uani 1 1 d D . . . .
H33A H 0.601198 0.922049 0.492697 0.089 Uiso 1 1 calc R U . . .
H33B H 0.663301 0.915138 0.406291 0.089 Uiso 1 1 calc R U . . .
C34 C 0.7268(8) 0.8714(5) 0.5113(8) 0.104(4) Uani 1 1 d D . . . .
H34A H 0.785959 0.879950 0.478490 0.124 Uiso 1 1 calc R U . . .
H34B H 0.728846 0.898933 0.565164 0.124 Uiso 1 1 calc R U . . .
C35 C 0.7166(9) 0.7975(5) 0.5307(9) 0.128(5) Uani 1 1 d D U . . .
H35A H 0.776444 0.772743 0.517411 0.153 Uiso 1 1 calc R U . . .
H35B H 0.702248 0.791037 0.592707 0.153 Uiso 1 1 calc R U . . .
C36 C 0.6396(8) 0.7702(5) 0.4785(7) 0.075(3) Uani 1 1 d D . . . .
H36A H 0.665041 0.737861 0.434535 0.090 Uiso 1 1 calc R U . . .
H36B H 0.594197 0.744406 0.515255 0.090 Uiso 1 1 calc R U . . .
O1 O 0.4289(4) 0.8174(8) 0.6373(3) 0.1120(18) Uani 1 1 d . U . . .
O2 O 0.5921(3) 0.8277(3) 0.4369(2) 0.0457(12) Uani 1 1 d . . . . .
Si1 Si 0.26516(17) 0.98514(10) 0.30646(12) 0.0328(5) Uani 1 1 d . . . . .
Si2 Si 0.27398(17) 0.64778(10) 0.32461(12) 0.0340(5) Uani 1 1 d . . . . .
K1 K 0.39536(8) 0.82722(9) 0.46695(7) 0.0397(3) Uani 1 1 d . . . . .
K2 K 0.08775(7) 0.8086(2) 0.24583(8) 0.0446(6) Uani 1 1 d . . . . .
Pb Pb 0.33408(2) 0.81577(4) 0.24924(2) 0.02682(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.412(9) . ?
C1 Si1 1.836(7) . ?
C1 Pb 2.249(7) . ?
C1 K2 3.089(7) . ?
C1 K1 3.122(7) . ?
C2 C3 1.438(5) . ?
C2 C5 1.508(10) . ?
C2 K2 2.952(7) . ?
C2 K1 2.975(7) . ?
C3 C4 1.414(10) . ?
C3 C11 1.496(11) . ?
C3 K2 2.959(7) . ?
C3 K1 2.974(8) . ?
C4 Si2 1.845(6) . ?
C4 Pb 2.251(6) . ?
C4 K2 3.109(7) . ?
C4 K1 3.110(7) . ?
C5 C6 1.382(11) . ?
C5 C10 1.398(10) . ?
C6 C7 1.390(10) . ?
C6 H6 0.9400 . ?
C7 C8 1.364(13) . ?
C7 H7 0.9400 . ?
C8 C9 1.362(12) . ?
C8 H8 0.9400 . ?
C9 C10 1.379(10) . ?
C9 H9 0.9400 . ?
C10 H10 0.9400 . ?
C11 C16 1.375(12) . ?
C11 C12 1.383(11) . ?
C12 C13 1.389(11) . ?
C12 H12 0.9400 . ?
C13 C14 1.361(15) . ?
C13 H13 0.9400 . ?
C14 C15 1.359(15) . ?
C14 H14 0.9400 . ?
C15 C16 1.397(11) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 Si1 1.900(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 Si1 1.889(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 C20 1.525(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 C21 1.518(10) . ?
C20 C22 1.539(10) . ?
C20 Si1 1.928(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 Si2 1.882(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 Si2 1.878(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 C28 1.499(10) . ?
C25 C27 1.528(9) . ?
C25 C26 1.529(10) . ?
C25 Si2 1.929(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C29 O1 1.341(16) . ?
C29 C30 1.457(13) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 C31 1.485(13) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 C32 1.484(14) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C32 O1 1.490(19) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C33 O2 1.436(11) . ?
C33 C34 1.461(12) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C34 C35 1.448(12) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C35 C36 1.438(12) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C36 O2 1.431(10) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
O1 K1 2.664(5) . ?
O2 K1 2.781(4) . ?
O2 K2 2.831(4) 4 ?
K1 Pb 3.4570(11) . ?
K1 K2 4.2415(16) 4 ?
K2 Pb 3.4361(11) . ?
K2 Pb 3.5388(10) 4_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Si1 132.5(5) . . ?
C2 C1 Pb 110.8(4) . . ?
Si1 C1 Pb 116.6(3) . . ?
C2 C1 K2 71.1(4) . . ?
Si1 C1 K2 118.5(3) . . ?
Pb C1 K2 78.41(19) . . ?
C2 C1 K1 70.9(4) . . ?
Si1 C1 K1 117.7(3) . . ?
Pb C1 K1 78.29(19) . . ?
K2 C1 K1 123.9(2) . . ?
C1 C2 C3 120.1(7) . . ?
C1 C2 C5 122.4(6) . . ?
C3 C2 C5 117.5(7) . . ?
C1 C2 K2 82.0(4) . . ?
C3 C2 K2 76.2(5) . . ?
C5 C2 K2 111.8(5) . . ?
C1 C2 K1 82.5(4) . . ?
C3 C2 K1 76.0(5) . . ?
C5 C2 K1 112.0(5) . . ?
K2 C2 K1 135.2(2) . . ?
C4 C3 C2 119.8(7) . . ?
C4 C3 C11 120.3(6) . . ?
C2 C3 C11 119.8(7) . . ?
C4 C3 K2 82.5(4) . . ?
C2 C3 K2 75.7(5) . . ?
C11 C3 K2 109.3(5) . . ?
C4 C3 K1 82.0(5) . . ?
C2 C3 K1 76.0(5) . . ?
C11 C3 K1 115.1(5) . . ?
K2 C3 K1 134.9(2) . . ?
C3 C4 Si2 131.3(5) . . ?
C3 C4 Pb 110.8(4) . . ?
Si2 C4 Pb 117.5(3) . . ?
C3 C4 K2 70.7(4) . . ?
Si2 C4 K2 113.3(3) . . ?
Pb C4 K2 77.94(19) . . ?
C3 C4 K1 71.3(4) . . ?
Si2 C4 K1 123.1(3) . . ?
Pb C4 K1 78.5(2) . . ?
K2 C4 K1 123.6(2) . . ?
C6 C5 C10 116.6(7) . . ?
C6 C5 C2 122.6(7) . . ?
C10 C5 C2 120.8(7) . . ?
C5 C6 C7 121.7(7) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 120.0(8) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.3(8) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C5 121.5(8) . . ?
C9 C10 H10 119.2 . . ?
C5 C10 H10 119.2 . . ?
C16 C11 C12 117.2(7) . . ?
C16 C11 C3 122.0(7) . . ?
C12 C11 C3 120.8(7) . . ?
C11 C12 C13 120.6(8) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 121.5(8) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 118.7(8) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 120.3(10) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 121.6(8) . . ?
C11 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C19 108.3(7) . . ?
C21 C20 C22 109.5(7) . . ?
C19 C20 C22 107.9(6) . . ?
C21 C20 Si1 109.6(5) . . ?
C19 C20 Si1 111.7(5) . . ?
C22 C20 Si1 109.8(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C25 C27 108.9(6) . . ?
C28 C25 C26 108.6(7) . . ?
C27 C25 C26 108.1(6) . . ?
C28 C25 Si2 111.6(4) . . ?
C27 C25 Si2 109.7(5) . . ?
C26 C25 Si2 109.9(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 C30 108.3(12) . . ?
O1 C29 H29A 110.0 . . ?
C30 C29 H29A 110.0 . . ?
O1 C29 H29B 110.0 . . ?
C30 C29 H29B 110.0 . . ?
H29A C29 H29B 108.4 . . ?
C29 C30 C31 107.3(12) . . ?
C29 C30 H30A 110.2 . . ?
C31 C30 H30A 110.2 . . ?
C29 C30 H30B 110.2 . . ?
C31 C30 H30B 110.2 . . ?
H30A C30 H30B 108.5 . . ?
C32 C31 C30 99.7(12) . . ?
C32 C31 H31A 111.8 . . ?
C30 C31 H31A 111.8 . . ?
C32 C31 H31B 111.8 . . ?
C30 C31 H31B 111.8 . . ?
H31A C31 H31B 109.6 . . ?
C31 C32 O1 103.0(11) . . ?
C31 C32 H32A 111.2 . . ?
O1 C32 H32A 111.2 . . ?
C31 C32 H32B 111.2 . . ?
O1 C32 H32B 111.2 . . ?
H32A C32 H32B 109.1 . . ?
O2 C33 C34 108.4(8) . . ?
O2 C33 H33A 110.0 . . ?
C34 C33 H33A 110.0 . . ?
O2 C33 H33B 110.0 . . ?
C34 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?
C35 C34 C33 106.2(9) . . ?
C35 C34 H34A 110.5 . . ?
C33 C34 H34A 110.5 . . ?
C35 C34 H34B 110.5 . . ?
C33 C34 H34B 110.5 . . ?
H34A C34 H34B 108.7 . . ?
C36 C35 C34 108.1(9) . . ?
C36 C35 H35A 110.1 . . ?
C34 C35 H35A 110.1 . . ?
C36 C35 H35B 110.1 . . ?
C34 C35 H35B 110.1 . . ?
H35A C35 H35B 108.4 . . ?
O2 C36 C35 108.4(8) . . ?
O2 C36 H36A 110.0 . . ?
C35 C36 H36A 110.0 . . ?
O2 C36 H36B 110.0 . . ?
C35 C36 H36B 110.0 . . ?
H36A C36 H36B 108.4 . . ?
C29 O1 C32 106.5(7) . . ?
C29 O1 K1 126.4(10) . . ?
C32 O1 K1 124.1(8) . . ?
C36 O2 C33 107.8(6) . . ?
C36 O2 K1 112.3(5) . . ?
C33 O2 K1 116.7(6) . . ?
C36 O2 K2 110.7(5) . 4 ?
C33 O2 K2 110.8(5) . 4 ?
K1 O2 K2 98.20(12) . 4 ?
C1 Si1 C18 108.3(3) . . ?
C1 Si1 C17 115.4(3) . . ?
C18 Si1 C17 102.9(4) . . ?
C1 Si1 C20 116.6(3) . . ?
C18 Si1 C20 106.2(3) . . ?
C17 Si1 C20 106.3(3) . . ?
C4 Si2 C24 116.2(3) . . ?
C4 Si2 C23 109.1(3) . . ?
C24 Si2 C23 104.5(4) . . ?
C4 Si2 C25 112.9(3) . . ?
C24 Si2 C25 107.0(3) . . ?
C23 Si2 C25 106.4(3) . . ?
O1 K1 O2 89.42(15) . . ?
O1 K1 C3 117.3(2) . . ?
O2 K1 C3 146.17(16) . . ?
O1 K1 C2 121.6(2) . . ?
O2 K1 C2 147.54(16) . . ?
C3 K1 C2 27.98(10) . . ?
O1 K1 C4 131.9(3) . . ?
O2 K1 C4 119.59(17) . . ?
C3 K1 C4 26.75(19) . . ?
C2 K1 C4 47.77(18) . . ?
O1 K1 C1 142.0(3) . . ?
O2 K1 C1 121.37(15) . . ?
C3 K1 C1 47.71(18) . . ?
C2 K1 C1 26.63(18) . . ?
C4 K1 C1 54.37(10) . . ?
O1 K1 Pb 171.3(3) . . ?
O2 K1 Pb 94.80(8) . . ?
C3 K1 Pb 56.10(12) . . ?
C2 K1 Pb 56.02(13) . . ?
C4 K1 Pb 39.65(12) . . ?
C1 K1 Pb 39.56(12) . . ?
O1 K1 K2 129.76(15) . 4 ?
O2 K1 K2 41.34(8) . 4 ?
C3 K1 K2 106.79(13) . 4 ?
C2 K1 K2 108.68(14) . 4 ?
C4 K1 K2 82.40(14) . 4 ?
C1 K1 K2 85.96(13) . 4 ?
Pb K1 K2 53.56(2) . 4 ?
O2 K2 C2 137.2(2) 4_455 . ?
O2 K2 C3 145.25(16) 4_455 . ?
C2 K2 C3 28.16(11) . . ?
O2 K2 C1 110.29(18) 4_455 . ?
C2 K2 C1 26.90(18) . . ?
C3 K2 C1 48.12(18) . . ?
O2 K2 C4 120.93(16) 4_455 . ?
C2 K2 C4 47.95(18) . . ?
C3 K2 C4 26.80(18) . . ?
C1 K2 C4 54.70(11) . . ?
O2 K2 Pb 89.34(8) 4_455 . ?
C2 K2 Pb 56.43(14) . . ?
C3 K2 Pb 56.47(14) . . ?
C1 K2 Pb 39.87(13) . . ?
C4 K2 Pb 39.84(13) . . ?
O2 K2 Pb 92.16(8) 4_455 4_455 ?
C2 K2 Pb 119.99(15) . 4_455 ?
C3 K2 Pb 122.45(15) . 4_455 ?
C1 K2 Pb 135.33(17) . 4_455 ?
C4 K2 Pb 141.43(16) . 4_455 ?
Pb K2 Pb 175.02(14) . 4_455 ?
O2 K2 K1 40.46(8) 4_455 4_455 ?
C2 K2 K1 156.68(19) . 4_455 ?
C3 K2 K1 172.22(18) . 4_455 ?
C1 K2 K1 139.34(17) . 4_455 ?
C4 K2 K1 153.79(16) . 4_455 ?
Pb K2 K1 129.79(4) . 4_455 ?
Pb K2 K1 51.81(2) 4_455 4_455 ?
C1 Pb C4 78.52(14) . . ?
C1 Pb K2 61.72(19) . . ?
C4 Pb K2 62.22(19) . . ?
C1 Pb K1 62.15(17) . . ?
C4 Pb K1 61.85(18) . . ?
K2 Pb K1 105.31(3) . . ?
C1 Pb K2 121.40(19) . 4 ?
C4 Pb K2 114.42(19) . 4 ?
K2 Pb K2 175.47(16) . 4 ?
K1 Pb K2 74.63(3) . 4 ?

# start Validation Reply Form

_vrf_PLAT003_1                   
;
RESPONSE: Soft restraints were used to handle the disorder of 
two tetrahydrofuran (THF) solvent molecules in the structure. 
;

_vrf_PLAT113_1                   
;
RESPONSE: Close examination has shown that the structure is 
pseudo-centrosymmetric and has been successfully refined in 
Pn21a (final R1=2.07%). Attempts to refine it as centrosymmetric 
in Pnma yielded a model with very bad thermal ellipsoids 
(elongated/flat) and distorted geometry (final R1=6.31%). 
The resulting Flack parameter indicates that the macroscopic 
crystal is twinned by inversion in a ratio of approximately 
19:81. 
;

_vrf_PLAT111_1                   
;
RESPONSE: See comment below 'PLAT113'.
;

# end Validation Reply Form



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Alkanes/tetrahydrofuran'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-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_muru412
_database_code_depnum_ccdc_archive 'CCDC 2179099'
loop_
_audit_author_name
_audit_author_address
'Roberto Diaz-Rodriguez'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_audit_creation_date             2022-06-03

loop_
_audit_author_email
rdiaz030@uottawa.ca
thierry.maris@umontreal.ca
_diffrn_source_power             0.1993706
_audit_creation_method           
;
FinalCif V105 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C72 H120 K4 O8 Pb2 Si4'
_chemical_formula_moiety         'C72 H120 K4 O8 Pb2 Si4'
_chemical_formula_weight         1796.81
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_chemical_melting_point          ?
_chemical_absolute_configuration ad
_space_group_crystal_system      monoclinic
_olex2_exptl_crystal_mounting_method 'mounted on  cryoloop'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.930(7)
 0.070(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O1 \\sim C69A \\sim C69B \\sim C70A \\sim C70B \\sim O2: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C69A) = Uanis(C69B)
Uanis(C70A) = Uanis(C70B)
4. Others
 Sof(C69B)=Sof(H69C)=Sof(H69D)=Sof(C70B)=Sof(H70C)=Sof(H70D)=1-FVAR(1)
 Sof(C69A)=Sof(H69A)=Sof(H69B)=Sof(C70A)=Sof(H70A)=Sof(H70B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A,H34B), C65(H65A,
 H65B), C66(H66A,H66B), C69A(H69A,H69B), C70A(H70A,H70B), C69B(H69C,H69D),
 C70B(H70C,H70D)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_olex2_submission_original_sample_id RDA159
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.9985(5)
_cell_length_b                   14.6914(5)
_cell_length_c                   20.5549(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.382(2)
_cell_angle_gamma                90
_cell_volume                     4226.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9749
_cell_measurement_theta_min      3.288
_cell_measurement_theta_max      55.517
_exptl_crystal_description       Plate
_exptl_crystal_colour            'clear light red'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Alkanes/1,2-dimethoxyethane'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    6.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0207
_exptl_absorpt_correction_T_max  0.0927
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1233 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.2233.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.312
_shelx_estimated_absorpt_T_max   0.608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Venture diffractometer equipped with a Photon III CMOS Detector,
a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance 
was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode.
;
_diffrn_ambient_temperature      150
_diffrn_ambient_environment      ?
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_diffrn_radiation_probe          X-ray
_diffrn_source                   'Metal Jet'
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_target            Ga
_diffrn_source_voltage           69.71
_diffrn_source_current           2.86
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_detector_area_resol_mean 10.42
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            65629
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_theta_min         2.617
_diffrn_reflns_theta_max         55.920
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             15909
_reflns_number_gt                14130
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.917
_reflns_Friedel_fraction_full    0.947
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_data_collection       
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_cell_refinement       
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_refine_special_details          
'Refined as a 2-component inversion twin.,Disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+0.3102P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         15909
_refine_ls_number_parameters     847
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.070(7)
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.930(7)
2 0.070(7)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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'
K K 0.3778 0.8310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2153 0.2529 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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 0.48815(2) 0.71768(2) 0.52409(2) 0.04945(8) Uani 1 1 d . . . . .
Pb2 Pb 0.98570(2) 0.76298(2) 0.50033(2) 0.05013(8) Uani 1 1 d . . . . .
K1 K 0.73990(16) 0.73193(19) 0.50936(13) 0.0660(5) Uani 1 1 d . . . . .
K2 K 0.53013(12) 0.48136(10) 0.52408(8) 0.0577(4) Uani 1 1 d . . . . .
K3 K 0.23808(15) 0.74636(18) 0.52827(11) 0.0675(6) Uani 1 1 d . . . . .
K4 K 0.03188(12) 0.99929(10) 0.48950(8) 0.0573(4) Uani 1 1 d . . . . .
Si1 Si 0.95468(15) 0.86047(12) 0.65697(10) 0.0486(4) Uani 1 1 d . . . . .
Si2 Si 0.38920(16) 0.64778(14) 0.67811(10) 0.0544(5) Uani 1 1 d . . . . .
Si3 Si 0.86435(16) 0.79866(14) 0.34920(11) 0.0575(5) Uani 1 1 d . . . . .
Si4 Si 0.45019(15) 0.63116(12) 0.36492(10) 0.0488(4) Uani 1 1 d . . . . .
O1 O 0.7403(6) 0.5356(4) 0.5328(4) 0.0885(12) Uani 1 1 d . U . . .
O2 O 0.6412(5) 0.4397(4) 0.6299(3) 0.0866(12) Uani 1 1 d . U . . .
O3 O 0.6271(5) 0.3675(4) 0.4422(4) 0.090(2) Uani 1 1 d . . . . .
O4 O 0.4940(6) 0.2887(3) 0.5309(4) 0.0733(16) Uani 1 1 d . . . . .
O5 O 0.2350(4) 0.9409(4) 0.5027(3) 0.0679(15) Uani 1 1 d . . . . .
O6 O 0.1230(5) 1.1181(4) 0.5732(3) 0.0790(17) Uani 1 1 d . . . . .
O7 O -0.0061(5) 1.1931(4) 0.4762(3) 0.0740(17) Uani 1 1 d . . . . .
O9 O 0.1659(5) 1.0460(4) 0.3963(3) 0.0720(17) Uani 1 1 d . . . . .
C1 C 0.4098(5) 0.6322(4) 0.4490(3) 0.0476(16) Uani 1 1 d . . . . .
C2 C 0.3433(5) 0.5747(4) 0.4801(3) 0.0455(16) Uani 1 1 d . . . . .
C3 C 0.3376(5) 0.5736(4) 0.5502(3) 0.0446(15) Uani 1 1 d . . . . .
C4 C 0.3957(5) 0.6334(4) 0.5891(3) 0.0464(15) Uani 1 1 d . . . . .
C5 C 0.2655(6) 0.5132(5) 0.5812(4) 0.0523(18) Uani 1 1 d . . . . .
C6 C 0.1689(6) 0.5239(5) 0.5717(4) 0.058(2) Uani 1 1 d . . . . .
H6 H 0.146560 0.568146 0.541236 0.069 Uiso 1 1 calc R U . . .
C7 C 0.1020(7) 0.4725(6) 0.6048(5) 0.074(2) Uani 1 1 d . . . . .
H7 H 0.035589 0.482173 0.597147 0.089 Uiso 1 1 calc R U . . .
C8 C 0.1326(8) 0.4082(6) 0.6482(5) 0.082(3) Uani 1 1 d . . . . .
H8 H 0.087486 0.373958 0.671906 0.099 Uiso 1 1 calc R U . . .
C9 C 0.2316(8) 0.3925(6) 0.6581(5) 0.079(3) Uani 1 1 d . . . . .
H9 H 0.253335 0.346774 0.687580 0.094 Uiso 1 1 calc R U . . .
C10 C 0.2958(7) 0.4438(5) 0.6247(4) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.362255 0.432544 0.630994 0.072 Uiso 1 1 calc R U . . .
C11 C 0.2813(5) 0.5114(5) 0.4404(4) 0.0489(17) Uani 1 1 d . . . . .
C12 C 0.2041(6) 0.5432(5) 0.4025(4) 0.0585(19) Uani 1 1 d . . . . .
H12 H 0.189774 0.606360 0.402661 0.070 Uiso 1 1 calc R U . . .
C13 C 0.1479(7) 0.4851(7) 0.3647(4) 0.078(3) Uani 1 1 d . . . . .
H13 H 0.095813 0.508716 0.339423 0.093 Uiso 1 1 calc R U . . .
C14 C 0.1676(7) 0.3934(6) 0.3637(5) 0.079(3) Uani 1 1 d . . . . .
H14 H 0.130581 0.353678 0.336715 0.095 Uiso 1 1 calc R U . . .
C15 C 0.2416(7) 0.3594(6) 0.4024(5) 0.076(3) Uani 1 1 d . . . . .
H15 H 0.253596 0.295789 0.402996 0.091 Uiso 1 1 calc R U . . .
C16 C 0.2984(6) 0.4167(5) 0.4401(4) 0.0582(19) Uani 1 1 d . . . . .
H16 H 0.349283 0.392128 0.465994 0.070 Uiso 1 1 calc R U . . .
C17 C 0.5850(6) 0.6345(5) 0.3666(4) 0.063(2) Uani 1 1 d . . . . .
H17A H 0.606884 0.692493 0.385175 0.095 Uiso 1 1 calc R U . . .
H17B H 0.608089 0.628515 0.322187 0.095 Uiso 1 1 calc R U . . .
H17C H 0.609903 0.584193 0.393326 0.095 Uiso 1 1 calc R U . . .
C18 C 0.4179(7) 0.5256(5) 0.3158(4) 0.069(2) Uani 1 1 d . . . . .
H18A H 0.454823 0.524693 0.275915 0.103 Uiso 1 1 calc R U . . .
H18B H 0.349539 0.526535 0.304546 0.103 Uiso 1 1 calc R U . . .
H18C H 0.432841 0.471201 0.341704 0.103 Uiso 1 1 calc R U . . .
C19 C 0.4085(6) 0.7338(5) 0.3143(4) 0.0544(18) Uani 1 1 d . . . . .
C20 C 0.4394(8) 0.7233(6) 0.2429(4) 0.077(3) Uani 1 1 d . . . . .
H20A H 0.419578 0.777291 0.217946 0.116 Uiso 1 1 calc R U . . .
H20B H 0.409080 0.669143 0.223738 0.116 Uiso 1 1 calc R U . . .
H20C H 0.508999 0.716960 0.241681 0.116 Uiso 1 1 calc R U . . .
C21 C 0.2998(6) 0.7419(5) 0.3155(4) 0.066(2) Uani 1 1 d . . . . .
H21A H 0.279861 0.751435 0.360392 0.100 Uiso 1 1 calc R U . . .
H21B H 0.270772 0.685901 0.298361 0.100 Uiso 1 1 calc R U . . .
H21C H 0.279033 0.793662 0.288613 0.100 Uiso 1 1 calc R U . . .
C22 C 0.4543(6) 0.8224(5) 0.3411(4) 0.062(2) Uani 1 1 d . . . . .
H22A H 0.424866 0.874989 0.319204 0.093 Uiso 1 1 calc R U . . .
H22B H 0.523046 0.821856 0.333116 0.093 Uiso 1 1 calc R U . . .
H22C H 0.444053 0.826536 0.388014 0.093 Uiso 1 1 calc R U . . .
C23 C 0.2613(6) 0.6416(6) 0.7104(4) 0.069(2) Uani 1 1 d . . . . .
H23A H 0.223546 0.692453 0.692644 0.104 Uiso 1 1 calc R U . . .
H23B H 0.263572 0.645393 0.758014 0.104 Uiso 1 1 calc R U . . .
H23C H 0.231710 0.583959 0.696967 0.104 Uiso 1 1 calc R U . . .
C24 C 0.4627(7) 0.5606(6) 0.7257(4) 0.073(2) Uani 1 1 d . . . . .
H24A H 0.434925 0.499972 0.719043 0.109 Uiso 1 1 calc R U . . .
H24B H 0.462579 0.575859 0.772082 0.109 Uiso 1 1 calc R U . . .
H24C H 0.528487 0.560975 0.710435 0.109 Uiso 1 1 calc R U . . .
C25 C 0.4363(7) 0.7640(5) 0.7087(5) 0.061(2) Uani 1 1 d . . . . .
C26 C 0.4200(7) 0.7714(6) 0.7815(4) 0.073(2) Uani 1 1 d . . . . .
H26A H 0.352856 0.758615 0.790255 0.109 Uiso 1 1 calc R U . . .
H26B H 0.436018 0.833090 0.796360 0.109 Uiso 1 1 calc R U . . .
H26C H 0.460780 0.727338 0.804791 0.109 Uiso 1 1 calc R U . . .
C27 C 0.5422(6) 0.7742(6) 0.6993(4) 0.065(2) Uani 1 1 d . . . . .
H27A H 0.575917 0.722875 0.719894 0.097 Uiso 1 1 calc R U . . .
H27B H 0.564364 0.831245 0.719181 0.097 Uiso 1 1 calc R U . . .
H27C H 0.555197 0.774985 0.652654 0.097 Uiso 1 1 calc R U . . .
C28 C 0.3791(7) 0.8427(5) 0.6742(5) 0.074(3) Uani 1 1 d . . . . .
H28A H 0.382742 0.835664 0.626870 0.112 Uiso 1 1 calc R U . . .
H28B H 0.406531 0.901485 0.687145 0.112 Uiso 1 1 calc R U . . .
H28C H 0.312069 0.840114 0.686835 0.112 Uiso 1 1 calc R U . . .
C29 C 0.2532(8) 0.9218(7) 0.4366(5) 0.088(3) Uani 1 1 d . . . . .
H29A H 0.204939 0.877409 0.420620 0.106 Uiso 1 1 calc R U . . .
H29B H 0.316479 0.891953 0.434542 0.106 Uiso 1 1 calc R U . . .
C30 C 0.2525(8) 0.9984(8) 0.3927(6) 0.094(3) Uani 1 1 d . . . . .
H30A H 0.306236 1.039679 0.404128 0.113 Uiso 1 1 calc R U . . .
H30B H 0.261064 0.976701 0.347619 0.113 Uiso 1 1 calc R U . . .
C31 C 0.1564(8) 1.1144(6) 0.3477(5) 0.083(3) Uani 1 1 d . . . . .
H31A H 0.098629 1.150241 0.355154 0.124 Uiso 1 1 calc R U . . .
H31B H 0.151560 1.085693 0.304696 0.124 Uiso 1 1 calc R U . . .
H31C H 0.212389 1.154411 0.349674 0.124 Uiso 1 1 calc R U . . .
C32 C 0.3070(8) 0.9888(6) 0.5366(6) 0.092(3) Uani 1 1 d . . . . .
H32A H 0.306283 1.052597 0.522651 0.138 Uiso 1 1 calc R U . . .
H32B H 0.369235 0.961804 0.527367 0.138 Uiso 1 1 calc R U . . .
H32C H 0.295836 0.985516 0.583408 0.138 Uiso 1 1 calc R U . . .
C33 C 0.1418(7) 1.1978(7) 0.5354(6) 0.087(3) Uani 1 1 d . . . . .
H33A H 0.174486 1.179714 0.495206 0.104 Uiso 1 1 calc R U . . .
H33B H 0.185377 1.238367 0.560581 0.104 Uiso 1 1 calc R U . . .
C34 C 0.0535(9) 1.2482(6) 0.5176(6) 0.086(3) Uani 1 1 d . . . . .
H34A H 0.018883 1.264254 0.557460 0.104 Uiso 1 1 calc R U . . .
H34B H 0.069951 1.305258 0.494881 0.104 Uiso 1 1 calc R U . . .
C35 C 0.1254(10) 1.1319(8) 0.6397(5) 0.110(4) Uani 1 1 d . . . . .
H35A H 0.076023 1.176026 0.651138 0.166 Uiso 1 1 calc R U . . .
H35B H 0.188320 1.155457 0.653283 0.166 Uiso 1 1 calc R U . . .
H35C H 0.113624 1.074146 0.661946 0.166 Uiso 1 1 calc R U . . .
C36 C -0.0899(8) 1.2405(6) 0.4586(5) 0.081(3) Uani 1 1 d . . . . .
H36A H -0.133760 1.199541 0.435022 0.122 Uiso 1 1 calc R U . . .
H36B H -0.073904 1.292056 0.430662 0.122 Uiso 1 1 calc R U . . .
H36C H -0.120451 1.262941 0.497900 0.122 Uiso 1 1 calc R U . . .
C37 C 0.8839(5) 0.8394(5) 0.4335(3) 0.0499(16) Uani 1 1 d . . . . .
C38 C 0.8319(5) 0.9045(4) 0.4691(3) 0.0462(16) Uani 1 1 d . . . . .
C39 C 0.8454(5) 0.9107(4) 0.5378(3) 0.0457(15) Uani 1 1 d . . . . .
C40 C 0.9152(5) 0.8574(4) 0.5706(3) 0.0468(15) Uani 1 1 d . . . . .
C41 C 0.7562(5) 0.9627(5) 0.4363(4) 0.0494(17) Uani 1 1 d . . . . .
C42 C 0.7779(7) 1.0262(5) 0.3895(4) 0.060(2) Uani 1 1 d . . . . .
H42 H 0.843075 1.035574 0.379586 0.072 Uiso 1 1 calc R U . . .
C43 C 0.7098(8) 1.0767(6) 0.3565(4) 0.075(3) Uani 1 1 d . . . . .
H43 H 0.728305 1.120147 0.325011 0.090 Uiso 1 1 calc R U . . .
C44 C 0.6137(7) 1.0640(5) 0.3694(5) 0.074(3) Uani 1 1 d . . . . .
H44 H 0.565798 1.097388 0.346188 0.089 Uiso 1 1 calc R U . . .
C45 C 0.5894(6) 1.0027(5) 0.4160(4) 0.066(2) Uani 1 1 d . . . . .
H45 H 0.524093 0.993676 0.425799 0.079 Uiso 1 1 calc R U . . .
C46 C 0.6605(6) 0.9530(5) 0.4493(4) 0.057(2) Uani 1 1 d . . . . .
H46 H 0.642218 0.911143 0.481943 0.069 Uiso 1 1 calc R U . . .
C47 C 0.7900(5) 0.9812(4) 0.5737(4) 0.0479(17) Uani 1 1 d . . . . .
C48 C 0.8136(6) 1.0733(5) 0.5728(4) 0.0565(18) Uani 1 1 d . . . . .
H48 H 0.865484 1.092827 0.547274 0.068 Uiso 1 1 calc R U . . .
C49 C 0.7632(6) 1.1379(5) 0.6084(4) 0.067(2) Uani 1 1 d . . . . .
H49 H 0.781568 1.200132 0.607666 0.081 Uiso 1 1 calc R U . . .
C50 C 0.6871(7) 1.1104(6) 0.6443(5) 0.075(3) Uani 1 1 d . . . . .
H50 H 0.652250 1.153853 0.668468 0.090 Uiso 1 1 calc R U . . .
C51 C 0.6611(7) 1.0205(6) 0.6455(5) 0.073(2) Uani 1 1 d . . . . .
H51 H 0.608030 1.001927 0.670174 0.088 Uiso 1 1 calc R U . . .
C52 C 0.7116(6) 0.9571(6) 0.6110(4) 0.062(2) Uani 1 1 d . . . . .
H52 H 0.692567 0.895112 0.612590 0.074 Uiso 1 1 calc R U . . .
C53 C 0.9247(6) 0.9662(5) 0.7049(4) 0.064(2) Uani 1 1 d . . . . .
H53A H 0.939271 1.020305 0.679067 0.095 Uiso 1 1 calc R U . . .
H53B H 0.962771 0.967163 0.745505 0.095 Uiso 1 1 calc R U . . .
H53C H 0.856619 0.965798 0.714821 0.095 Uiso 1 1 calc R U . . .
C54 C 1.0885(6) 0.8542(5) 0.6604(4) 0.059(2) Uani 1 1 d . . . . .
H54A H 1.109142 0.794505 0.644866 0.088 Uiso 1 1 calc R U . . .
H54B H 1.111433 0.863031 0.705404 0.088 Uiso 1 1 calc R U . . .
H54C H 1.114891 0.901955 0.632783 0.088 Uiso 1 1 calc R U . . .
C55 C 0.9109(6) 0.7589(5) 0.7080(4) 0.057(2) Uani 1 1 d . . . . .
C56 C 0.8014(6) 0.7515(6) 0.7020(5) 0.068(2) Uani 1 1 d . . . . .
H56A H 0.779489 0.700141 0.728156 0.103 Uiso 1 1 calc R U . . .
H56B H 0.782445 0.741792 0.656293 0.103 Uiso 1 1 calc R U . . .
H56C H 0.772380 0.807882 0.717637 0.103 Uiso 1 1 calc R U . . .
C57 C 0.9576(6) 0.6694(5) 0.6837(4) 0.067(2) Uani 1 1 d . . . . .
H57A H 1.026327 0.670587 0.694031 0.100 Uiso 1 1 calc R U . . .
H57B H 0.947572 0.664226 0.636471 0.100 Uiso 1 1 calc R U . . .
H57C H 0.928433 0.617175 0.705156 0.100 Uiso 1 1 calc R U . . .
C58 C 0.9379(7) 0.7708(5) 0.7800(4) 0.070(2) Uani 1 1 d . . . . .
H58A H 0.909159 0.826973 0.796318 0.104 Uiso 1 1 calc R U . . .
H58B H 1.007558 0.774394 0.785235 0.104 Uiso 1 1 calc R U . . .
H58C H 0.914219 0.718780 0.804754 0.104 Uiso 1 1 calc R U . . .
C59 C 0.7478(6) 0.8307(5) 0.3085(4) 0.063(2) Uani 1 1 d . . . . .
H59A H 0.697690 0.832795 0.340950 0.094 Uiso 1 1 calc R U . . .
H59B H 0.730943 0.785352 0.275170 0.094 Uiso 1 1 calc R U . . .
H59C H 0.753815 0.890629 0.288087 0.094 Uiso 1 1 calc R U . . .
C60 C 0.8659(7) 0.6692(5) 0.3486(5) 0.074(2) Uani 1 1 d . . . . .
H60A H 0.923179 0.647362 0.372200 0.111 Uiso 1 1 calc R U . . .
H60B H 0.866640 0.647335 0.303596 0.111 Uiso 1 1 calc R U . . .
H60C H 0.808835 0.646092 0.369818 0.111 Uiso 1 1 calc R U . . .
C61 C 0.9612(7) 0.8342(7) 0.2921(4) 0.079(3) Uani 1 1 d . . . . .
C62 C 0.9326(8) 0.8075(8) 0.2203(4) 0.092(3) Uani 1 1 d . . . . .
H62A H 0.918796 0.742180 0.218071 0.138 Uiso 1 1 calc R U . . .
H62B H 0.985459 0.821817 0.191564 0.138 Uiso 1 1 calc R U . . .
H62C H 0.875731 0.841902 0.206331 0.138 Uiso 1 1 calc R U . . .
C63 C 1.0552(7) 0.7839(11) 0.3105(6) 0.115(5) Uani 1 1 d . . . . .
H63A H 1.072391 0.796254 0.356189 0.173 Uiso 1 1 calc R U . . .
H63B H 1.106432 0.805220 0.282698 0.173 Uiso 1 1 calc R U . . .
H63C H 1.046247 0.718224 0.304432 0.173 Uiso 1 1 calc R U . . .
C64 C 0.9757(8) 0.9377(7) 0.2948(5) 0.092(3) Uani 1 1 d . . . . .
H64A H 0.987868 0.956524 0.339975 0.138 Uiso 1 1 calc R U . . .
H64B H 0.918038 0.968190 0.277740 0.138 Uiso 1 1 calc R U . . .
H64C H 1.030291 0.954526 0.268385 0.138 Uiso 1 1 calc R U . . .
C65 C 0.6429(9) 0.2867(8) 0.4804(8) 0.114(4) Uani 1 1 d . . . . .
H65A H 0.672726 0.304011 0.522819 0.136 Uiso 1 1 calc R U . . .
H65B H 0.688365 0.246761 0.457754 0.136 Uiso 1 1 calc R U . . .
C66 C 0.5549(10) 0.2356(7) 0.4921(7) 0.097(4) Uani 1 1 d . . . . .
H66A H 0.522294 0.220966 0.450126 0.117 Uiso 1 1 calc R U . . .
H66B H 0.570507 0.177673 0.514629 0.117 Uiso 1 1 calc R U . . .
C67 C 0.6437(10) 0.3611(9) 0.3761(6) 0.121(4) Uani 1 1 d . . . . .
H67A H 0.609266 0.308513 0.357947 0.181 Uiso 1 1 calc R U . . .
H67B H 0.712370 0.353601 0.369414 0.181 Uiso 1 1 calc R U . . .
H67C H 0.621352 0.416692 0.354205 0.181 Uiso 1 1 calc R U . . .
C68 C 0.4098(8) 0.2393(7) 0.5433(6) 0.089(3) Uani 1 1 d . . . . .
H68A H 0.365277 0.278047 0.566832 0.133 Uiso 1 1 calc R U . . .
H68B H 0.425740 0.185630 0.569798 0.133 Uiso 1 1 calc R U . . .
H68C H 0.379917 0.219824 0.502030 0.133 Uiso 1 1 calc R U . . .
C69A C 0.7430(18) 0.5591(15) 0.5989(11) 0.0882(10) Uani 0.511(15) 1 d . U P A 1
H69A H 0.688504 0.599575 0.608303 0.106 Uiso 0.511(15) 1 calc R U P A 1
H69B H 0.802774 0.592632 0.609305 0.106 Uiso 0.511(15) 1 calc R U P A 1
C70A C 0.7381(18) 0.4751(16) 0.6410(12) 0.0878(10) Uani 0.511(15) 1 d . U P A 1
H70A H 0.786357 0.429773 0.628097 0.105 Uiso 0.511(15) 1 calc R U P A 1
H70B H 0.749125 0.490745 0.687463 0.105 Uiso 0.511(15) 1 calc R U P A 1
C69B C 0.7843(18) 0.5005(16) 0.5970(11) 0.0882(10) Uani 0.489(15) 1 d . U P A 2
H69C H 0.800201 0.434991 0.593823 0.106 Uiso 0.489(15) 1 calc R U P A 2
H69D H 0.842822 0.534852 0.609129 0.106 Uiso 0.489(15) 1 calc R U P A 2
C70B C 0.7068(18) 0.5162(16) 0.6455(12) 0.0878(10) Uani 0.489(15) 1 d . U P A 2
H70C H 0.732088 0.512438 0.690858 0.105 Uiso 0.489(15) 1 calc R U P A 2
H70D H 0.675150 0.575819 0.638709 0.105 Uiso 0.489(15) 1 calc R U P A 2
C71 C 0.6312(9) 0.3678(6) 0.6749(5) 0.093(3) Uani 1 1 d . . . . .
H71A H 0.573802 0.332508 0.663522 0.140 Uiso 1 1 calc R U . . .
H71B H 0.625566 0.392796 0.718804 0.140 Uiso 1 1 calc R U . . .
H71C H 0.687452 0.328145 0.673440 0.140 Uiso 1 1 calc R U . . .
C72 C 0.8140(9) 0.4999(6) 0.4939(8) 0.123(5) Uani 1 1 d . . . . .
H72A H 0.822284 0.434914 0.503229 0.185 Uiso 1 1 calc R U . . .
H72B H 0.873938 0.532097 0.503828 0.185 Uiso 1 1 calc R U . . .
H72C H 0.796725 0.508012 0.447771 0.185 Uiso 1 1 calc R U . . .


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 K1 3.551(2) . ?
Pb1 K2 3.5213(15) . ?
Pb1 K3 3.529(2) . ?
Pb1 C1 2.254(6) . ?
Pb1 C4 2.254(7) . ?
Pb2 K1 3.480(2) . ?
Pb2 K3 3.574(2) 1_655 ?
Pb2 K4 3.5394(15) 1_655 ?
Pb2 C37 2.255(7) . ?
Pb2 C40 2.248(7) . ?
K1 Si3 3.887(4) . ?
K1 O1 2.924(7) . ?
K1 C37 3.023(8) . ?
K1 C38 2.970(7) . ?
K1 C39 3.063(7) . ?
K1 C40 3.295(7) . ?
K2 O1 3.050(8) . ?
K2 O2 2.713(6) . ?
K2 O3 2.753(6) . ?
K2 O4 2.879(5) . ?
K2 C1 3.162(7) . ?
K2 C2 3.070(7) . ?
K2 C3 3.075(7) . ?
K2 C4 3.231(7) . ?
K2 C69A 3.51(2) . ?
K2 C70B 3.51(2) . ?
K3 O5 2.906(6) . ?
K3 C1 3.381(7) . ?
K3 C2 3.095(7) . ?
K3 C3 2.925(7) . ?
K3 C4 3.009(7) . ?
K4 O5 2.976(6) . ?
K4 O6 2.743(6) . ?
K4 O7 2.908(6) . ?
K4 O9 2.798(7) . ?
K4 C37 3.320(7) 1_455 ?
K4 C38 3.146(7) 1_455 ?
K4 C39 3.102(7) 1_455 ?
K4 C40 3.150(7) 1_455 ?
Si1 C40 1.847(7) . ?
Si1 C53 1.891(7) . ?
Si1 C54 1.875(8) . ?
Si1 C55 1.933(8) . ?
Si2 C4 1.846(7) . ?
Si2 C23 1.927(8) . ?
Si2 C24 1.899(8) . ?
Si2 C25 1.931(8) . ?
Si3 C37 1.847(7) . ?
Si3 C59 1.876(8) . ?
Si3 C60 1.903(8) . ?
Si3 C61 1.889(10) . ?
Si4 C1 1.832(7) . ?
Si4 C17 1.887(9) . ?
Si4 C18 1.898(7) . ?
Si4 C19 1.915(8) . ?
O1 C69A 1.40(2) . ?
O1 C69B 1.53(2) . ?
O1 C72 1.421(14) . ?
O2 C70A 1.47(2) . ?
O2 C70B 1.48(2) . ?
O2 C71 1.413(10) . ?
O3 C65 1.438(14) . ?
O3 C67 1.388(13) . ?
O4 C66 1.416(13) . ?
O4 C68 1.414(13) . ?
O5 C29 1.417(11) . ?
O5 C32 1.401(11) . ?
O6 C33 1.432(12) . ?
O6 C35 1.383(12) . ?
O7 C34 1.428(12) . ?
O7 C36 1.404(11) . ?
O9 C30 1.403(11) . ?
O9 C31 1.422(10) . ?
C1 C2 1.419(10) . ?
C2 C3 1.446(10) . ?
C2 C11 1.500(9) . ?
C3 C4 1.428(9) . ?
C3 C5 1.498(10) . ?
C5 C6 1.371(11) . ?
C5 C10 1.416(11) . ?
C6 H6 0.9500 . ?
C6 C7 1.393(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.361(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.415(14) . ?
C9 H9 0.9500 . ?
C9 C10 1.370(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(10) . ?
C11 C16 1.411(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(11) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(11) . ?
C16 H16 0.9500 . ?
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 C20 1.548(12) . ?
C19 C21 1.527(12) . ?
C19 C22 1.546(10) . ?
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 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.523(13) . ?
C25 C27 1.507(12) . ?
C25 C28 1.567(12) . ?
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 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.443(14) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.480(15) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.416(10) . ?
C38 C39 1.425(10) . ?
C38 C41 1.508(9) . ?
C39 C40 1.411(9) . ?
C39 C47 1.497(10) . ?
C41 C42 1.379(11) . ?
C41 C46 1.381(11) . ?
C42 H42 0.9500 . ?
C42 C43 1.373(11) . ?
C43 H43 0.9500 . ?
C43 C44 1.390(13) . ?
C44 H44 0.9500 . ?
C44 C45 1.363(12) . ?
C45 H45 0.9500 . ?
C45 C46 1.400(10) . ?
C46 H46 0.9500 . ?
C47 C48 1.393(10) . ?
C47 C52 1.400(11) . ?
C48 H48 0.9500 . ?
C48 C49 1.399(11) . ?
C49 H49 0.9500 . ?
C49 C50 1.373(12) . ?
C50 H50 0.9500 . ?
C50 C51 1.370(12) . ?
C51 H51 0.9500 . ?
C51 C52 1.376(12) . ?
C52 H52 0.9500 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.540(12) . ?
C55 C57 1.556(11) . ?
C55 C58 1.529(12) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.570(12) . ?
C61 C63 1.548(15) . ?
C61 C64 1.535(14) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.468(18) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69A H69A 0.9900 . ?
C69A H69B 0.9900 . ?
C69A C70A 1.51(3) . ?
C70A H70A 0.9900 . ?
C70A H70B 0.9900 . ?
C69B H69C 0.9900 . ?
C69B H69D 0.9900 . ?
C69B C70B 1.51(4) . ?
C70B H70C 0.9900 . ?
C70B H70D 0.9900 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 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
K2 Pb1 K1 83.81(5) . . ?
K2 Pb1 K3 106.46(5) . . ?
K3 Pb1 K1 169.18(4) . . ?
C1 Pb1 K1 116.24(19) . . ?
C1 Pb1 K2 61.89(16) . . ?
C1 Pb1 K3 67.45(18) . . ?
C1 Pb1 C4 79.8(3) . . ?
C4 Pb1 K1 131.95(17) . . ?
C4 Pb1 K2 63.67(17) . . ?
C4 Pb1 K3 57.79(17) . . ?
K1 Pb2 K3 163.19(4) . 1_655 ?
K1 Pb2 K4 108.31(5) . 1_655 ?
K4 Pb2 K3 84.01(5) 1_655 1_655 ?
C37 Pb2 K1 59.10(19) . . ?
C37 Pb2 K3 137.71(19) . 1_655 ?
C37 Pb2 K4 65.61(17) . 1_655 ?
C40 Pb2 K1 66.22(18) . . ?
C40 Pb2 K3 112.73(18) . 1_655 ?
C40 Pb2 K4 61.23(17) . 1_655 ?
C40 Pb2 C37 78.7(2) . . ?
Pb1 K1 Si3 123.58(8) . . ?
Pb2 K1 Pb1 175.47(8) . . ?
Pb2 K1 Si3 57.18(5) . . ?
O1 K1 Pb1 85.75(18) . . ?
O1 K1 Pb2 98.04(18) . . ?
O1 K1 Si3 112.90(19) . . ?
O1 K1 C37 127.0(2) . . ?
O1 K1 C38 152.7(2) . . ?
O1 K1 C39 144.6(2) . . ?
O1 K1 C40 119.4(2) . . ?
C37 K1 Pb1 138.61(16) . . ?
C37 K1 Pb2 39.81(13) . . ?
C37 K1 Si3 27.55(14) . . ?
C37 K1 C39 47.65(19) . . ?
C37 K1 C40 53.51(18) . . ?
C38 K1 Pb1 120.80(15) . . ?
C38 K1 Pb2 55.77(13) . . ?
C38 K1 Si3 48.89(14) . . ?
C38 K1 C37 27.31(18) . . ?
C38 K1 C39 27.26(19) . . ?
C38 K1 C40 45.98(18) . . ?
C39 K1 Pb1 120.61(15) . . ?
C39 K1 Pb2 54.91(14) . . ?
C39 K1 Si3 73.85(15) . . ?
C39 K1 C40 25.31(16) . . ?
C40 K1 Pb1 137.06(14) . . ?
C40 K1 Pb2 38.64(12) . . ?
C40 K1 Si3 80.66(14) . . ?
O1 K2 Pb1 84.43(13) . . ?
O1 K2 C1 110.33(19) . . ?
O1 K2 C2 135.59(18) . . ?
O1 K2 C3 136.29(19) . . ?
O1 K2 C4 111.46(19) . . ?
O1 K2 C69A 23.3(4) . . ?
O1 K2 C70B 42.1(4) . . ?
O2 K2 Pb1 108.33(14) . . ?
O2 K2 O1 58.6(2) . . ?
O2 K2 O3 94.1(2) . . ?
O2 K2 O4 80.6(2) . . ?
O2 K2 C1 146.85(19) . . ?
O2 K2 C2 143.6(2) . . ?
O2 K2 C3 116.5(2) . . ?
O2 K2 C4 98.7(2) . . ?
O2 K2 C69A 42.1(4) . . ?
O2 K2 C70B 23.4(4) . . ?
O3 K2 Pb1 133.13(16) . . ?
O3 K2 O1 72.9(2) . . ?
O3 K2 O4 61.5(2) . . ?
O3 K2 C1 113.1(2) . . ?
O3 K2 C2 121.3(2) . . ?
O3 K2 C3 145.2(2) . . ?
O3 K2 C4 166.8(2) . . ?
O3 K2 C69A 92.3(5) . . ?
O3 K2 C70B 100.0(5) . . ?
O4 K2 Pb1 160.02(18) . . ?
O4 K2 O1 115.1(2) . . ?
O4 K2 C1 128.3(2) . . ?
O4 K2 C2 107.7(2) . . ?
O4 K2 C3 105.6(2) . . ?
O4 K2 C4 123.7(2) . . ?
O4 K2 C69A 116.5(4) . . ?
O4 K2 C70B 103.3(4) . . ?
C1 K2 Pb1 38.96(12) . . ?
C1 K2 C4 53.76(17) . . ?
C1 K2 C69A 115.0(4) . . ?
C1 K2 C70B 127.1(4) . . ?
C2 K2 Pb1 54.45(11) . . ?
C2 K2 C1 26.27(18) . . ?
C2 K2 C3 27.22(19) . . ?
C2 K2 C4 46.57(17) . . ?
C2 K2 C69A 133.8(4) . . ?
C2 K2 C70B 136.5(5) . . ?
C3 K2 Pb1 54.45(12) . . ?
C3 K2 C1 46.98(18) . . ?
C3 K2 C4 26.03(16) . . ?
C3 K2 C69A 121.2(5) . . ?
C3 K2 C70B 114.6(5) . . ?
C4 K2 Pb1 38.71(12) . . ?
C4 K2 C69A 95.2(5) . . ?
C4 K2 C70B 90.7(5) . . ?
C69A K2 Pb1 79.6(4) . . ?
C70B K2 Pb1 88.3(4) . . ?
Pb1 K3 Pb2 168.98(7) . 1_455 ?
O5 K3 Pb1 97.10(14) . . ?
O5 K3 Pb2 83.88(13) . 1_455 ?
O5 K3 C1 114.13(18) . . ?
O5 K3 C2 138.47(19) . . ?
O5 K3 C3 152.4(2) . . ?
O5 K3 C4 128.72(19) . . ?
C1 K3 Pb1 38.00(11) . . ?
C1 K3 Pb2 131.90(13) . 1_455 ?
C2 K3 Pb1 54.19(13) . . ?
C2 K3 Pb2 118.71(14) . 1_455 ?
C2 K3 C1 24.81(16) . . ?
C3 K3 Pb1 55.32(14) . . ?
C3 K3 Pb2 123.32(15) . 1_455 ?
C3 K3 C1 45.75(18) . . ?
C3 K3 C2 27.61(19) . . ?
C3 K3 C4 27.81(17) . . ?
C4 K3 Pb1 39.34(14) . . ?
C4 K3 Pb2 144.72(16) . 1_455 ?
C4 K3 C1 53.42(18) . . ?
C4 K3 C2 48.23(18) . . ?
O5 K4 Pb2 83.51(12) . 1_455 ?
O5 K4 C37 114.50(17) . 1_455 ?
O5 K4 C38 136.86(17) . 1_455 ?
O5 K4 C39 131.26(18) . 1_455 ?
O5 K4 C40 105.50(18) . 1_455 ?
O6 K4 Pb2 131.88(14) . 1_455 ?
O6 K4 O5 72.38(18) . . ?
O6 K4 O7 61.11(19) . . ?
O6 K4 O9 87.9(2) . . ?
O6 K4 C37 160.8(2) . 1_455 ?
O6 K4 C38 139.8(2) . 1_455 ?
O6 K4 C39 116.6(2) . 1_455 ?
O6 K4 C40 109.2(2) . 1_455 ?
O7 K4 Pb2 158.92(14) . 1_455 ?
O7 K4 O5 117.56(18) . . ?
O7 K4 C37 123.31(18) . 1_455 ?
O7 K4 C38 105.14(18) . 1_455 ?
O7 K4 C39 106.71(18) . 1_455 ?
O7 K4 C40 126.99(19) . 1_455 ?
O9 K4 Pb2 114.21(13) . 1_455 ?
O9 K4 O5 58.56(18) . . ?
O9 K4 O7 79.61(18) . . ?
O9 K4 C37 111.06(19) . 1_455 ?
O9 K4 C38 128.8(2) . 1_455 ?
O9 K4 C39 154.88(19) . 1_455 ?
O9 K4 C40 152.77(18) . 1_455 ?
C37 K4 Pb2 38.22(11) 1_455 1_455 ?
C38 K4 Pb2 53.90(12) 1_455 1_455 ?
C38 K4 C37 25.11(17) 1_455 1_455 ?
C38 K4 C40 46.10(18) 1_455 1_455 ?
C39 K4 Pb2 53.99(12) 1_455 1_455 ?
C39 K4 C37 44.86(18) 1_455 1_455 ?
C39 K4 C38 26.35(18) 1_455 1_455 ?
C39 K4 C40 26.07(16) 1_455 1_455 ?
C40 K4 Pb2 38.73(12) 1_455 1_455 ?
C40 K4 C37 52.28(17) 1_455 1_455 ?
C40 Si1 C53 117.1(3) . . ?
C40 Si1 C54 108.1(3) . . ?
C40 Si1 C55 114.3(3) . . ?
C53 Si1 C55 105.9(4) . . ?
C54 Si1 C53 104.7(4) . . ?
C54 Si1 C55 105.7(4) . . ?
C4 Si2 C23 113.8(4) . . ?
C4 Si2 C24 113.2(4) . . ?
C4 Si2 C25 113.6(4) . . ?
C23 Si2 C25 104.0(4) . . ?
C24 Si2 C23 106.7(4) . . ?
C24 Si2 C25 104.6(4) . . ?
C37 Si3 K1 49.2(2) . . ?
C37 Si3 C59 116.4(4) . . ?
C37 Si3 C60 109.2(4) . . ?
C37 Si3 C61 113.7(4) . . ?
C59 Si3 K1 92.2(3) . . ?
C59 Si3 C60 105.0(4) . . ?
C59 Si3 C61 106.5(4) . . ?
C60 Si3 K1 76.0(3) . . ?
C61 Si3 K1 159.9(3) . . ?
C61 Si3 C60 105.3(4) . . ?
C1 Si4 C17 108.3(4) . . ?
C1 Si4 C18 115.7(3) . . ?
C1 Si4 C19 114.2(3) . . ?
C17 Si4 C18 104.8(4) . . ?
C17 Si4 C19 106.3(4) . . ?
C18 Si4 C19 106.8(4) . . ?
K1 O1 K2 104.5(2) . . ?
C69A O1 K1 85.3(10) . . ?
C69A O1 K2 97.1(11) . . ?
C69A O1 C72 129.3(14) . . ?
C69B O1 K1 118.3(9) . . ?
C69B O1 K2 109.2(10) . . ?
C72 O1 K1 105.7(6) . . ?
C72 O1 K2 125.6(6) . . ?
C72 O1 C69B 94.5(13) . . ?
C70A O2 K2 123.7(10) . . ?
C70B O2 K2 110.1(10) . . ?
C71 O2 K2 129.0(6) . . ?
C71 O2 C70A 105.6(11) . . ?
C71 O2 C70B 119.7(11) . . ?
C65 O3 K2 103.9(7) . . ?
C67 O3 K2 137.5(7) . . ?
C67 O3 C65 116.8(9) . . ?
C66 O4 K2 114.0(6) . . ?
C68 O4 K2 131.5(6) . . ?
C68 O4 C66 109.5(8) . . ?
K3 O5 K4 108.1(2) . . ?
C29 O5 K3 88.7(5) . . ?
C29 O5 K4 99.4(5) . . ?
C32 O5 K3 113.4(5) . . ?
C32 O5 K4 125.1(5) . . ?
C32 O5 C29 115.6(8) . . ?
C33 O6 K4 105.6(5) . . ?
C35 O6 K4 135.5(6) . . ?
C35 O6 C33 114.6(7) . . ?
C34 O7 K4 113.3(6) . . ?
C36 O7 K4 131.2(6) . . ?
C36 O7 C34 110.2(7) . . ?
C30 O9 K4 120.6(6) . . ?
C30 O9 C31 112.4(8) . . ?
C31 O9 K4 127.0(6) . . ?
Pb1 C1 K2 79.15(19) . . ?
Pb1 C1 K3 74.55(18) . . ?
K2 C1 K3 119.3(2) . . ?
Si4 C1 Pb1 119.6(3) . . ?
Si4 C1 K2 106.4(3) . . ?
Si4 C1 K3 134.3(3) . . ?
C2 C1 Pb1 109.7(5) . . ?
C2 C1 K2 73.2(4) . . ?
C2 C1 K3 66.2(4) . . ?
C2 C1 Si4 129.8(5) . . ?
K2 C2 K3 132.7(2) . . ?
C1 C2 K2 80.5(4) . . ?
C1 C2 K3 88.9(4) . . ?
C1 C2 C3 120.5(6) . . ?
C1 C2 C11 120.2(6) . . ?
C3 C2 K2 76.6(4) . . ?
C3 C2 K3 69.6(3) . . ?
C3 C2 C11 119.3(6) . . ?
C11 C2 K2 111.1(4) . . ?
C11 C2 K3 113.9(4) . . ?
K3 C3 K2 140.5(2) . . ?
C2 C3 K2 76.2(4) . . ?
C2 C3 K3 82.8(4) . . ?
C2 C3 C5 119.0(6) . . ?
C4 C3 K2 83.1(4) . . ?
C4 C3 K3 79.3(4) . . ?
C4 C3 C2 120.5(6) . . ?
C4 C3 C5 120.4(6) . . ?
C5 C3 K2 114.6(4) . . ?
C5 C3 K3 104.8(4) . . ?
Pb1 C4 K2 77.6(2) . . ?
Pb1 C4 K3 82.88(19) . . ?
K3 C4 K2 129.6(2) . . ?
Si2 C4 Pb1 124.6(3) . . ?
Si2 C4 K2 122.2(3) . . ?
Si2 C4 K3 107.2(3) . . ?
C3 C4 Pb1 109.4(5) . . ?
C3 C4 K2 70.9(4) . . ?
C3 C4 K3 72.8(4) . . ?
C3 C4 Si2 125.8(5) . . ?
C6 C5 C3 123.0(7) . . ?
C6 C5 C10 116.9(7) . . ?
C10 C5 C3 120.0(7) . . ?
C5 C6 H6 118.6 . . ?
C5 C6 C7 122.7(8) . . ?
C7 C6 H6 118.6 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.5(9) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.9(8) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(9) . . ?
C10 C9 H9 120.3 . . ?
C5 C10 H10 119.3 . . ?
C9 C10 C5 121.5(9) . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C2 121.7(6) . . ?
C12 C11 C16 117.1(7) . . ?
C16 C11 C2 121.2(6) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.9(8) . . ?
C13 C12 H12 119.1 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(9) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.5(8) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(8) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 H16 119.8 . . ?
C15 C16 C11 120.5(8) . . ?
C15 C16 H16 119.8 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 Si4 110.4(5) . . ?
C21 C19 Si4 110.1(5) . . ?
C21 C19 C20 108.9(7) . . ?
C21 C19 C22 109.5(7) . . ?
C22 C19 Si4 110.5(5) . . ?
C22 C19 C20 107.4(7) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 Si2 109.0(6) . . ?
C26 C25 C28 107.8(7) . . ?
C27 C25 Si2 112.0(6) . . ?
C27 C25 C26 106.9(8) . . ?
C27 C25 C28 111.3(8) . . ?
C28 C25 Si2 109.7(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O5 C29 H29A 108.2 . . ?
O5 C29 H29B 108.2 . . ?
O5 C29 C30 116.6(9) . . ?
H29A C29 H29B 107.3 . . ?
C30 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
O9 C30 C29 110.4(9) . . ?
O9 C30 H30A 109.6 . . ?
O9 C30 H30B 109.6 . . ?
C29 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
O9 C31 H31A 109.5 . . ?
O9 C31 H31B 109.5 . . ?
O9 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O5 C32 H32A 109.5 . . ?
O5 C32 H32B 109.5 . . ?
O5 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O6 C33 H33A 109.1 . . ?
O6 C33 H33B 109.1 . . ?
O6 C33 C34 112.3(8) . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
O7 C34 C33 109.6(8) . . ?
O7 C34 H34A 109.7 . . ?
O7 C34 H34B 109.7 . . ?
C33 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
O6 C35 H35A 109.5 . . ?
O6 C35 H35B 109.5 . . ?
O6 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O7 C36 H36A 109.5 . . ?
O7 C36 H36B 109.5 . . ?
O7 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Pb2 C37 K1 81.1(2) . . ?
Pb2 C37 K4 76.17(18) . 1_655 ?
K1 C37 K4 127.5(2) . 1_655 ?
Si3 C37 Pb2 119.1(3) . . ?
Si3 C37 K1 103.3(3) . . ?
Si3 C37 K4 129.2(3) . 1_655 ?
C38 C37 Pb2 110.3(5) . . ?
C38 C37 K1 74.3(4) . . ?
C38 C37 K4 70.6(4) . 1_655 ?
C38 C37 Si3 129.6(5) . . ?
K1 C38 K4 137.0(2) . 1_655 ?
C37 C38 K1 78.4(4) . . ?
C37 C38 K4 84.3(4) . 1_655 ?
C37 C38 C39 119.9(6) . . ?
C37 C38 C41 121.1(6) . . ?
C39 C38 K1 80.0(4) . . ?
C39 C38 K4 75.1(4) . 1_655 ?
C39 C38 C41 118.8(6) . . ?
C41 C38 K1 107.7(4) . . ?
C41 C38 K4 114.9(4) . 1_655 ?
K1 C39 K4 134.8(2) . 1_655 ?
C38 C39 K1 72.7(4) . . ?
C38 C39 K4 78.5(4) . 1_655 ?
C38 C39 C47 118.4(6) . . ?
C40 C39 K1 86.6(4) . . ?
C40 C39 K4 78.9(4) . 1_655 ?
C40 C39 C38 120.8(6) . . ?
C40 C39 C47 120.6(6) . . ?
C47 C39 K1 115.7(5) . . ?
C47 C39 K4 108.5(4) . 1_655 ?
Pb2 C40 K1 75.14(17) . . ?
Pb2 C40 K4 80.0(2) . 1_655 ?
K4 C40 K1 124.0(2) 1_655 . ?
Si1 C40 Pb2 120.5(3) . . ?
Si1 C40 K1 125.7(3) . . ?
Si1 C40 K4 110.2(3) . 1_655 ?
C39 C40 Pb2 110.2(5) . . ?
C39 C40 K1 68.1(4) . . ?
C39 C40 K4 75.1(4) . 1_655 ?
C39 C40 Si1 129.3(5) . . ?
C42 C41 C38 122.2(7) . . ?
C42 C41 C46 115.8(7) . . ?
C46 C41 C38 121.9(7) . . ?
C41 C42 H42 118.4 . . ?
C43 C42 C41 123.2(9) . . ?
C43 C42 H42 118.4 . . ?
C42 C43 H43 120.1 . . ?
C42 C43 C44 119.8(9) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 120.6 . . ?
C45 C44 C43 118.8(7) . . ?
C45 C44 H44 120.6 . . ?
C44 C45 H45 120.0 . . ?
C44 C45 C46 120.1(8) . . ?
C46 C45 H45 120.0 . . ?
C41 C46 C45 122.2(8) . . ?
C41 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?
C48 C47 C39 122.6(7) . . ?
C48 C47 C52 116.2(7) . . ?
C52 C47 C39 121.1(6) . . ?
C47 C48 H48 119.0 . . ?
C47 C48 C49 121.9(8) . . ?
C49 C48 H48 119.0 . . ?
C48 C49 H49 120.3 . . ?
C50 C49 C48 119.3(8) . . ?
C50 C49 H49 120.3 . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.2(8) . . ?
C51 C50 H50 119.9 . . ?
C50 C51 H51 119.9 . . ?
C50 C51 C52 120.3(9) . . ?
C52 C51 H51 119.9 . . ?
C47 C52 H52 119.0 . . ?
C51 C52 C47 122.0(8) . . ?
C51 C52 H52 119.0 . . ?
Si1 C53 H53A 109.5 . . ?
Si1 C53 H53B 109.5 . . ?
Si1 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si1 C54 H54A 109.5 . . ?
Si1 C54 H54B 109.5 . . ?
Si1 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 Si1 109.8(5) . . ?
C56 C55 C57 109.9(7) . . ?
C57 C55 Si1 109.6(6) . . ?
C58 C55 Si1 111.3(5) . . ?
C58 C55 C56 108.0(8) . . ?
C58 C55 C57 108.2(7) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
Si3 C59 H59A 109.5 . . ?
Si3 C59 H59B 109.5 . . ?
Si3 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
Si3 C60 H60A 109.5 . . ?
Si3 C60 H60B 109.5 . . ?
Si3 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 Si3 110.2(7) . . ?
C63 C61 Si3 109.5(8) . . ?
C63 C61 C62 107.9(9) . . ?
C64 C61 Si3 110.3(7) . . ?
C64 C61 C62 108.2(8) . . ?
C64 C61 C63 110.7(9) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O3 C65 H65A 109.0 . . ?
O3 C65 H65B 109.0 . . ?
O3 C65 C66 113.1(10) . . ?
H65A C65 H65B 107.8 . . ?
C66 C65 H65A 109.0 . . ?
C66 C65 H65B 109.0 . . ?
O4 C66 C65 109.2(9) . . ?
O4 C66 H66A 109.8 . . ?
O4 C66 H66B 109.8 . . ?
C65 C66 H66A 109.8 . . ?
C65 C66 H66B 109.8 . . ?
H66A C66 H66B 108.3 . . ?
O3 C67 H67A 109.5 . . ?
O3 C67 H67B 109.5 . . ?
O3 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O4 C68 H68A 109.5 . . ?
O4 C68 H68B 109.5 . . ?
O4 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
K2 C69A H69A 68.3 . . ?
K2 C69A H69B 163.8 . . ?
O1 C69A K2 59.5(9) . . ?
O1 C69A H69A 109.5 . . ?
O1 C69A H69B 109.5 . . ?
O1 C69A C70A 110.8(19) . . ?
H69A C69A H69B 108.1 . . ?
C70A C69A K2 86.3(12) . . ?
C70A C69A H69A 109.5 . . ?
C70A C69A H69B 109.5 . . ?
O2 C70A C69A 104.8(18) . . ?
O2 C70A H70A 110.8 . . ?
O2 C70A H70B 110.8 . . ?
C69A C70A H70A 110.8 . . ?
C69A C70A H70B 110.8 . . ?
H70A C70A H70B 108.9 . . ?
O1 C69B H69C 111.0 . . ?
O1 C69B H69D 111.0 . . ?
H69C C69B H69D 109.0 . . ?
C70B C69B O1 103.8(19) . . ?
C70B C69B H69C 111.0 . . ?
C70B C69B H69D 111.0 . . ?
K2 C70B H70C 153.0 . . ?
K2 C70B H70D 73.9 . . ?
O2 C70B K2 46.6(8) . . ?
O2 C70B C69B 101.1(18) . . ?
O2 C70B H70C 111.6 . . ?
O2 C70B H70D 111.6 . . ?
C69B C70B K2 90.7(13) . . ?
C69B C70B H70C 111.6 . . ?
C69B C70B H70D 111.6 . . ?
H70C C70B H70D 109.4 . . ?
O2 C71 H71A 109.5 . . ?
O2 C71 H71B 109.5 . . ?
O2 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O1 C72 H72A 109.5 . . ?
O1 C72 H72B 109.5 . . ?
O1 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 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 C1 C2 K2 -71.5(3) . . . . ?
Pb1 C1 C2 K3 62.2(3) . . . . ?
Pb1 C1 C2 C3 -3.3(8) . . . . ?
Pb1 C1 C2 C11 179.5(5) . . . . ?
Pb2 C37 C38 K1 -74.0(3) . . . . ?
Pb2 C37 C38 K4 66.4(3) . . . 1_655 ?
Pb2 C37 C38 C39 -2.8(8) . . . . ?
Pb2 C37 C38 C41 -177.9(5) . . . . ?
K1 Si3 C37 Pb2 87.1(4) . . . . ?
K1 Si3 C37 K4 -177.1(5) . . . 1_655 ?
K1 Si3 C37 C38 -80.4(7) . . . . ?
K1 Si3 C61 C62 158.8(7) . . . . ?
K1 Si3 C61 C63 40.3(14) . . . . ?
K1 Si3 C61 C64 -81.8(12) . . . . ?
K1 O1 C69A K2 104.0(3) . . . . ?
K1 O1 C69A C70A 176(2) . . . . ?
K1 O1 C69B C70B 79.7(16) . . . . ?
K1 C37 C38 K4 140.38(19) . . . 1_655 ?
K1 C37 C38 C39 71.2(6) . . . . ?
K1 C37 C38 C41 -103.9(6) . . . . ?
K1 C38 C39 K4 144.60(18) . . . 1_655 ?
K1 C38 C39 C40 75.1(6) . . . . ?
K1 C38 C39 C47 -110.4(6) . . . . ?
K1 C38 C41 C42 -152.3(6) . . . . ?
K1 C38 C41 C46 24.9(8) . . . . ?
K1 C39 C40 Pb2 63.7(3) . . . . ?
K1 C39 C40 K4 136.9(2) . . . 1_655 ?
K1 C39 C40 Si1 -118.9(5) . . . . ?
K1 C39 C47 C48 -159.3(6) . . . . ?
K1 C39 C47 C52 21.5(8) . . . . ?
K2 O1 C69A C70A 72(2) . . . . ?
K2 O1 C69B C70B -39.6(17) . . . . ?
K2 O2 C70A C69A 21(3) . . . . ?
K2 O2 C70B C69B -80.3(18) . . . . ?
K2 O3 C65 C66 69.6(11) . . . . ?
K2 O4 C66 C65 23.1(13) . . . . ?
K2 C1 C2 K3 133.69(19) . . . . ?
K2 C1 C2 C3 68.2(6) . . . . ?
K2 C1 C2 C11 -109.0(6) . . . . ?
K2 C2 C3 K3 146.32(18) . . . . ?
K2 C2 C3 C4 73.2(6) . . . . ?
K2 C2 C3 C5 -110.7(6) . . . . ?
K2 C2 C11 C12 -164.8(6) . . . . ?
K2 C2 C11 C16 15.4(9) . . . . ?
K2 C3 C4 Pb1 68.7(3) . . . . ?
K2 C3 C4 K3 144.4(2) . . . . ?
K2 C3 C4 Si2 -116.4(5) . . . . ?
K2 C3 C5 C6 -150.6(6) . . . . ?
K2 C3 C5 C10 32.3(8) . . . . ?
K2 C69A C70A O2 -13.1(16) . . . . ?
K3 O5 C29 C30 174.9(10) . . . . ?
K3 C1 C2 K2 -133.69(19) . . . . ?
K3 C1 C2 C3 -65.5(5) . . . . ?
K3 C1 C2 C11 117.3(6) . . . . ?
K3 C2 C3 K2 -146.32(18) . . . . ?
K3 C2 C3 C4 -73.1(5) . . . . ?
K3 C2 C3 C5 103.0(6) . . . . ?
K3 C2 C11 C12 29.9(9) . . . . ?
K3 C2 C11 C16 -149.9(6) . . . . ?
K3 C3 C4 Pb1 -75.7(3) . . . . ?
K3 C3 C4 K2 -144.4(2) . . . . ?
K3 C3 C4 Si2 99.2(5) . . . . ?
K3 C3 C5 C6 26.5(8) . . . . ?
K3 C3 C5 C10 -150.6(6) . . . . ?
K4 O5 C29 C30 66.8(10) . . . . ?
K4 O6 C33 C34 69.5(9) . . . . ?
K4 O7 C34 C33 23.0(11) . . . . ?
K4 O9 C30 C29 6.3(13) . . . . ?
K4 C37 C38 K1 -140.38(19) 1_655 . . . ?
K4 C37 C38 C39 -69.2(6) 1_655 . . . ?
K4 C37 C38 C41 115.8(6) 1_655 . . . ?
K4 C38 C39 K1 -144.60(18) 1_655 . . . ?
K4 C38 C39 C40 -69.5(6) 1_655 . . . ?
K4 C38 C39 C47 105.0(6) 1_655 . . . ?
K4 C38 C41 C42 33.5(8) 1_655 . . . ?
K4 C38 C41 C46 -149.4(6) 1_655 . . . ?
K4 C39 C40 Pb2 -73.2(3) 1_655 . . . ?
K4 C39 C40 K1 -136.9(2) 1_655 . . . ?
K4 C39 C40 Si1 104.1(6) 1_655 . . . ?
K4 C39 C47 C48 10.9(8) 1_655 . . . ?
K4 C39 C47 C52 -168.3(6) 1_655 . . . ?
Si3 C37 C38 K1 94.4(6) . . . . ?
Si3 C37 C38 K4 -125.3(6) . . . 1_655 ?
Si3 C37 C38 C39 165.5(5) . . . . ?
Si3 C37 C38 C41 -9.5(10) . . . . ?
Si4 C1 C2 K2 97.6(6) . . . . ?
Si4 C1 C2 K3 -128.7(5) . . . . ?
Si4 C1 C2 C3 165.8(5) . . . . ?
Si4 C1 C2 C11 -11.4(10) . . . . ?
O1 C69A C70A O2 -68(3) . . . . ?
O1 C69B C70B K2 31.5(13) . . . . ?
O1 C69B C70B O2 77.2(19) . . . . ?
O3 C65 C66 O4 -65.2(14) . . . . ?
O5 C29 C30 O9 -54.9(14) . . . . ?
O6 C33 C34 O7 -64.2(12) . . . . ?
C1 C2 C3 K2 -70.3(6) . . . . ?
C1 C2 C3 K3 76.0(6) . . . . ?
C1 C2 C3 C4 3.0(10) . . . . ?
C1 C2 C3 C5 179.0(6) . . . . ?
C1 C2 C11 C12 -73.7(10) . . . . ?
C1 C2 C11 C16 106.5(8) . . . . ?
C2 C3 C4 Pb1 -0.8(7) . . . . ?
C2 C3 C4 K2 -69.5(6) . . . . ?
C2 C3 C4 K3 74.9(6) . . . . ?
C2 C3 C4 Si2 174.1(5) . . . . ?
C2 C3 C5 C6 -63.3(10) . . . . ?
C2 C3 C5 C10 119.6(8) . . . . ?
C2 C11 C12 C13 178.5(8) . . . . ?
C2 C11 C16 C15 -178.8(8) . . . . ?
C3 C2 C11 C12 109.1(8) . . . . ?
C3 C2 C11 C16 -70.7(10) . . . . ?
C3 C5 C6 C7 -174.5(7) . . . . ?
C3 C5 C10 C9 174.4(8) . . . . ?
C4 C3 C5 C6 112.7(8) . . . . ?
C4 C3 C5 C10 -64.4(9) . . . . ?
C5 C3 C4 Pb1 -176.8(5) . . . . ?
C5 C3 C4 K2 114.5(6) . . . . ?
C5 C3 C4 K3 -101.0(6) . . . . ?
C5 C3 C4 Si2 -1.9(9) . . . . ?
C5 C6 C7 C8 -0.5(13) . . . . ?
C6 C5 C10 C9 -2.9(12) . . . . ?
C6 C7 C8 C9 -1.7(14) . . . . ?
C7 C8 C9 C10 1.5(14) . . . . ?
C8 C9 C10 C5 0.9(14) . . . . ?
C10 C5 C6 C7 2.7(12) . . . . ?
C11 C2 C3 K2 106.9(6) . . . . ?
C11 C2 C3 K3 -106.7(6) . . . . ?
C11 C2 C3 C4 -179.8(6) . . . . ?
C11 C2 C3 C5 -3.8(9) . . . . ?
C11 C12 C13 C14 -0.1(14) . . . . ?
C12 C11 C16 C15 1.4(12) . . . . ?
C12 C13 C14 C15 2.2(16) . . . . ?
C13 C14 C15 C16 -2.4(16) . . . . ?
C14 C15 C16 C11 0.6(14) . . . . ?
C16 C11 C12 C13 -1.7(12) . . . . ?
C17 Si4 C1 Pb1 37.8(4) . . . . ?
C17 Si4 C1 K2 -48.8(4) . . . . ?
C17 Si4 C1 K3 135.0(4) . . . . ?
C17 Si4 C1 C2 -130.4(7) . . . . ?
C18 Si4 C1 Pb1 155.1(4) . . . . ?
C18 Si4 C1 K2 68.4(4) . . . . ?
C18 Si4 C1 K3 -107.7(5) . . . . ?
C18 Si4 C1 C2 -13.1(8) . . . . ?
C19 Si4 C1 Pb1 -80.4(4) . . . . ?
C19 Si4 C1 K2 -167.0(3) . . . . ?
C19 Si4 C1 K3 16.8(5) . . . . ?
C19 Si4 C1 C2 111.4(7) . . . . ?
C23 Si2 C4 Pb1 137.2(4) . . . . ?
C23 Si2 C4 K2 -125.6(4) . . . . ?
C23 Si2 C4 K3 44.0(4) . . . . ?
C23 Si2 C4 C3 -36.9(7) . . . . ?
C24 Si2 C4 Pb1 -100.7(5) . . . . ?
C24 Si2 C4 K2 -3.5(5) . . . . ?
C24 Si2 C4 K3 166.1(3) . . . . ?
C24 Si2 C4 C3 85.2(7) . . . . ?
C25 Si2 C4 Pb1 18.4(5) . . . . ?
C25 Si2 C4 K2 115.6(4) . . . . ?
C25 Si2 C4 K3 -74.8(4) . . . . ?
C25 Si2 C4 C3 -155.7(6) . . . . ?
C31 O9 C30 C29 -171.9(9) . . . . ?
C32 O5 C29 C30 -69.7(12) . . . . ?
C35 O6 C33 C34 -90.9(11) . . . . ?
C36 O7 C34 C33 -179.6(9) . . . . ?
C37 Si3 C61 C62 -172.9(7) . . . . ?
C37 Si3 C61 C63 68.6(8) . . . . ?
C37 Si3 C61 C64 -53.5(8) . . . . ?
C37 C38 C39 K1 -70.3(6) . . . . ?
C37 C38 C39 K4 74.3(6) . . . 1_655 ?
C37 C38 C39 C40 4.8(10) . . . . ?
C37 C38 C39 C47 179.2(6) . . . . ?
C37 C38 C41 C42 -65.3(9) . . . . ?
C37 C38 C41 C46 111.8(8) . . . . ?
C38 C39 C40 Pb2 -3.9(8) . . . . ?
C38 C39 C40 K1 -67.6(6) . . . . ?
C38 C39 C40 K4 69.3(6) . . . 1_655 ?
C38 C39 C40 Si1 173.5(5) . . . . ?
C38 C39 C47 C48 -75.8(9) . . . . ?
C38 C39 C47 C52 105.0(8) . . . . ?
C38 C41 C42 C43 176.5(7) . . . . ?
C38 C41 C46 C45 -175.8(7) . . . . ?
C39 C38 C41 C42 119.6(8) . . . . ?
C39 C38 C41 C46 -63.3(9) . . . . ?
C39 C47 C48 C49 -177.7(7) . . . . ?
C39 C47 C52 C51 178.5(8) . . . . ?
C40 C39 C47 C48 98.6(8) . . . . ?
C40 C39 C47 C52 -80.5(9) . . . . ?
C41 C38 C39 K1 104.8(6) . . . . ?
C41 C38 C39 K4 -110.6(6) . . . 1_655 ?
C41 C38 C39 C40 179.9(6) . . . . ?
C41 C38 C39 C47 -5.6(9) . . . . ?
C41 C42 C43 C44 -0.7(13) . . . . ?
C42 C41 C46 C45 1.6(11) . . . . ?
C42 C43 C44 C45 1.5(13) . . . . ?
C43 C44 C45 C46 -0.8(12) . . . . ?
C44 C45 C46 C41 -0.8(12) . . . . ?
C46 C41 C42 C43 -0.9(12) . . . . ?
C47 C39 C40 Pb2 -178.2(5) . . . . ?
C47 C39 C40 K1 118.1(7) . . . . ?
C47 C39 C40 K4 -105.0(6) . . . 1_655 ?
C47 C39 C40 Si1 -0.9(10) . . . . ?
C47 C48 C49 C50 -1.3(13) . . . . ?
C48 C47 C52 C51 -0.7(12) . . . . ?
C48 C49 C50 C51 0.3(14) . . . . ?
C49 C50 C51 C52 0.5(15) . . . . ?
C50 C51 C52 C47 -0.3(15) . . . . ?
C52 C47 C48 C49 1.5(11) . . . . ?
C53 Si1 C40 Pb2 159.0(4) . . . . ?
C53 Si1 C40 K1 -107.7(4) . . . . ?
C53 Si1 C40 K4 68.9(4) . . . 1_655 ?
C53 Si1 C40 C39 -18.0(8) . . . . ?
C54 Si1 C40 Pb2 41.2(4) . . . . ?
C54 Si1 C40 K1 134.4(4) . . . . ?
C54 Si1 C40 K4 -49.0(4) . . . 1_655 ?
C54 Si1 C40 C39 -135.9(6) . . . . ?
C55 Si1 C40 Pb2 -76.3(5) . . . . ?
C55 Si1 C40 K1 17.0(5) . . . . ?
C55 Si1 C40 K4 -166.4(3) . . . 1_655 ?
C55 Si1 C40 C39 106.6(7) . . . . ?
C59 Si3 C37 Pb2 155.2(4) . . . . ?
C59 Si3 C37 K1 68.2(4) . . . . ?
C59 Si3 C37 K4 -109.0(4) . . . 1_655 ?
C59 Si3 C37 C38 -12.2(8) . . . . ?
C59 Si3 C61 C62 -43.4(8) . . . . ?
C59 Si3 C61 C63 -161.9(7) . . . . ?
C59 Si3 C61 C64 75.9(7) . . . . ?
C60 Si3 C37 Pb2 36.7(5) . . . . ?
C60 Si3 C37 K1 -50.4(4) . . . . ?
C60 Si3 C37 K4 132.5(4) . . . 1_655 ?
C60 Si3 C37 C38 -130.8(7) . . . . ?
C60 Si3 C61 C62 67.7(8) . . . . ?
C60 Si3 C61 C63 -50.8(8) . . . . ?
C60 Si3 C61 C64 -173.0(7) . . . . ?
C61 Si3 C37 Pb2 -80.5(5) . . . . ?
C61 Si3 C37 K1 -167.6(4) . . . . ?
C61 Si3 C37 K4 15.3(6) . . . 1_655 ?
C61 Si3 C37 C38 112.0(7) . . . . ?
C67 O3 C65 C66 -97.7(13) . . . . ?
C68 O4 C66 C65 -179.0(11) . . . . ?
C71 O2 C70A C69A -173.0(17) . . . . ?
C71 O2 C70B K2 -168.6(14) . . . . ?
C71 O2 C70B C69B 111.1(17) . . . . ?
C72 O1 C69A K2 -149.5(12) . . . . ?
C72 O1 C69A C70A -77(2) . . . . ?
C72 O1 C69B C70B -169.8(15) . . . . ?

_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-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_4b
_database_code_depnum_ccdc_archive 'CCDC 2179097'
loop_
_audit_author_name
_audit_author_address
'Roberto Diaz-Rodriguez'
;University of Ottawa
Canada
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
#=============================================================
# CHEMICAL DATA
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H72 Na2 O4 Pb Si2'
_chemical_formula_sum            'C44 H72 Na2 O4 Pb Si2'
_chemical_formula_weight         974.36

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'
Na Na 0.0362 0.0249 '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'

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

_cell_length_a                   23.3878(17)
_cell_length_b                   10.5283(8)
_cell_length_c                   20.5795(16)
_cell_angle_alpha                90
_cell_angle_beta                 107.770(2)
_cell_angle_gamma                90
_cell_volume                     4825.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    203.15
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.485
_shelx_estimated_absorpt_T_min   0.318
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0781 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.7519.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.1050
0.00 -1.00 0.00 0.1230
1.00 0.00 0.00 0.1840
-1.00 0.00 0.00 0.1990
-2.00 0.00 1.00 0.2070
2.00 0.00 -1.00 0.1910
0.00 -1.00 2.00 0.0940
1.00 -2.00 2.00 0.1120
0.00 1.00 -1.00 0.1060
1.00 2.00 -2.00 0.1310
-1.00 -2.00 2.00 0.1170
2.00 -1.00 0.00 0.1750
-1.00 2.00 1.00 0.0810
1.00 -2.00 -1.00 0.1360
-1.00 1.00 1.00 0.0770
-2.00 -1.00 0.00 0.1620
0.00 1.00 1.00 0.1150
0.00 -1.00 -1.00 0.1480
2.00 -1.00 -2.00 0.1530
-1.00 -1.00 -1.00 0.1440
-1.00 1.00 2.00 0.0940
1.00 -1.00 -2.00 0.1430
0.00 1.00 2.00 0.1110
-1.00 -1.00 -2.00 0.1390
1.00 0.00 -2.00 0.1120
0.00 0.00 -1.00 0.0840
-1.00 0.00 -2.00 0.1250
1.00 0.00 1.00 0.1610
0.00 0.00 1.00 0.1160
-2.00 1.00 -2.00 0.1190
-1.00 0.00 2.00 0.1290

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Grown via slow diffusion of hexane layered on a solution of compound in toluene/THF mixture at -20 C'
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.235
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            227692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.132
_diffrn_reflns_theta_min         1.829
_diffrn_ambient_temperature      203.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10883
_reflns_number_total             13001
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         13001
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+2.6507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0496
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim C44 \\sim C43 \\sim C42 \\sim C41: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O3 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O2 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O1 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C29(H29A,H29B), C38(H38A,H38B), C33(H33A,H33B), C41(H41A,
 H41B), C36(H36A,H36B), C30(H30A,H30B), C42(H42A,H42B), C34(H34A,H34B),
 C35(H35A,H35B), C32(H32A,H32B), C44(H44A,H44B), C39(H39A,H39B), C31(H31A,H31B),
  C40(H40A,H40B), C43(H43A,H43B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C16(H16), C10(H10), C13(H13), C15(H15), C14(H14), C7(H7),
 C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C18(H18A,H18B,
 H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C21(H21A,
 H21B,H21C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
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 0.73091(2) 0.28562(2) 0.27788(2) 0.03019(3) Uani 1 1 d . . . . .
Si2 Si 0.83922(3) 0.44481(5) 0.40742(3) 0.03035(11) Uani 1 1 d . . . . .
Si1 Si 0.63969(2) 0.37586(6) 0.11690(3) 0.03346(12) Uani 1 1 d . . . . .
Na2 Na 0.81530(4) 0.38220(9) 0.19769(5) 0.0438(2) Uani 1 1 d . . . . .
Na1 Na 0.68101(4) 0.54809(9) 0.30923(5) 0.0438(2) Uani 1 1 d . . . . .
O4 O 0.86492(8) 0.47778(18) 0.12805(9) 0.0531(4) Uani 1 1 d . U . . .
O2 O 0.65678(9) 0.75648(17) 0.32923(10) 0.0560(5) Uani 1 1 d . U . . .
C4 C 0.79232(8) 0.45303(18) 0.31785(10) 0.0276(4) Uani 1 1 d . . . . .
O1 O 0.61810(9) 0.47280(18) 0.36876(11) 0.0647(5) Uani 1 1 d . U . . .
C3 C 0.78027(8) 0.55601(17) 0.27064(10) 0.0265(4) Uani 1 1 d . . . . .
C5 C 0.71781(9) 0.65584(18) 0.15942(10) 0.0305(4) Uani 1 1 d . . . . .
C11 C 0.81804(9) 0.67380(18) 0.28741(9) 0.0278(4) Uani 1 1 d . . . . .
C2 C 0.73164(8) 0.54640(18) 0.20794(9) 0.0269(4) Uani 1 1 d . . . . .
O3 O 0.86146(10) 0.19820(18) 0.18056(14) 0.0775(7) Uani 1 1 d . U . . .
C6 C 0.75898(10) 0.7030(2) 0.12874(11) 0.0372(5) Uani 1 1 d . . . . .
H6 H 0.797335 0.666012 0.139582 0.045 Uiso 1 1 calc R U . . .
C1 C 0.69829(8) 0.43079(18) 0.19325(10) 0.0286(4) Uani 1 1 d . . . . .
C17 C 0.63284(11) 0.4658(3) 0.03548(11) 0.0497(6) Uani 1 1 d . . . . .
H17A H 0.612700 0.546078 0.036203 0.075 Uiso 1 1 calc R U . . .
H17B H 0.609751 0.415906 -0.003281 0.075 Uiso 1 1 calc R U . . .
H17C H 0.672564 0.481594 0.031693 0.075 Uiso 1 1 calc R U . . .
C12 C 0.87981(9) 0.6669(2) 0.29834(11) 0.0371(5) Uani 1 1 d . . . . .
H12 H 0.896717 0.589762 0.290199 0.044 Uiso 1 1 calc R U . . .
C16 C 0.79471(10) 0.79173(19) 0.29661(11) 0.0350(4) Uani 1 1 d . . . . .
H16 H 0.753009 0.801025 0.287341 0.042 Uiso 1 1 calc R U . . .
C24 C 0.86531(12) 0.6011(2) 0.45161(11) 0.0457(6) Uani 1 1 d . . . . .
H24A H 0.897261 0.635470 0.435927 0.069 Uiso 1 1 calc R U . . .
H24B H 0.880072 0.587673 0.500538 0.069 Uiso 1 1 calc R U . . .
H24C H 0.831981 0.660372 0.441052 0.069 Uiso 1 1 calc R U . . .
C10 C 0.66203(11) 0.7157(2) 0.14167(13) 0.0460(5) Uani 1 1 d . . . . .
H10 H 0.632924 0.687316 0.161279 0.055 Uiso 1 1 calc R U . . .
C13 C 0.91681(11) 0.7707(2) 0.32085(13) 0.0461(6) Uani 1 1 d . . . . .
H13 H 0.958372 0.763043 0.328328 0.055 Uiso 1 1 calc R U . . .
C25 C 0.90896(10) 0.3382(2) 0.42310(11) 0.0389(5) Uani 1 1 d . . . . .
C23 C 0.79321(11) 0.3733(3) 0.45955(12) 0.0495(6) Uani 1 1 d . . . . .
H23A H 0.760328 0.429897 0.458910 0.074 Uiso 1 1 calc R U . . .
H23B H 0.818456 0.361361 0.506229 0.074 Uiso 1 1 calc R U . . .
H23C H 0.777266 0.291877 0.440236 0.074 Uiso 1 1 calc R U . . .
C15 C 0.83180(11) 0.8956(2) 0.31918(12) 0.0448(5) Uani 1 1 d . . . . .
H15 H 0.815034 0.973989 0.325555 0.054 Uiso 1 1 calc R U . . .
C18 C 0.65720(13) 0.2083(2) 0.09750(14) 0.0581(7) Uani 1 1 d . . . . .
H18A H 0.692519 0.208130 0.082166 0.087 Uiso 1 1 calc R U . . .
H18B H 0.623384 0.173597 0.061965 0.087 Uiso 1 1 calc R U . . .
H18C H 0.664728 0.156878 0.138347 0.087 Uiso 1 1 calc R U . . .
C14 C 0.89305(11) 0.8852(2) 0.33238(13) 0.0485(6) Uani 1 1 d . . . . .
H14 H 0.918227 0.955206 0.348994 0.058 Uiso 1 1 calc R U . . .
C27 C 0.89097(12) 0.2017(2) 0.40089(15) 0.0552(7) Uani 1 1 d . . . . .
H27A H 0.863511 0.170485 0.424297 0.083 Uiso 1 1 calc R U . . .
H27B H 0.926519 0.148470 0.412274 0.083 Uiso 1 1 calc R U . . .
H27C H 0.871450 0.199337 0.351999 0.083 Uiso 1 1 calc R U . . .
C28 C 0.94435(12) 0.3365(3) 0.49956(13) 0.0579(7) Uani 1 1 d . . . . .
H28A H 0.956519 0.422299 0.514813 0.087 Uiso 1 1 calc R U . . .
H28B H 0.979685 0.283499 0.506924 0.087 Uiso 1 1 calc R U . . .
H28C H 0.919162 0.302645 0.525152 0.087 Uiso 1 1 calc R U . . .
C19 C 0.56058(10) 0.3685(3) 0.12757(13) 0.0475(6) Uani 1 1 d . . . . .
C7 C 0.74493(13) 0.8030(2) 0.08262(12) 0.0486(6) Uani 1 1 d . . . . .
H7 H 0.773558 0.831992 0.062449 0.058 Uiso 1 1 calc R U . . .
C26 C 0.95061(11) 0.3861(3) 0.38400(14) 0.0522(6) Uani 1 1 d . . . . .
H26A H 0.929964 0.382392 0.335379 0.078 Uiso 1 1 calc R U . . .
H26B H 0.986253 0.333294 0.394682 0.078 Uiso 1 1 calc R U . . .
H26C H 0.962094 0.473223 0.397079 0.078 Uiso 1 1 calc R U . . .
C21 C 0.51472(12) 0.3226(3) 0.06074(15) 0.0656(8) Uani 1 1 d . . . . .
H21A H 0.513861 0.381676 0.024293 0.098 Uiso 1 1 calc R U . . .
H21B H 0.475194 0.318045 0.066682 0.098 Uiso 1 1 calc R U . . .
H21C H 0.526250 0.239094 0.049178 0.098 Uiso 1 1 calc R U . . .
C37 C 0.83372(13) 0.0784(3) 0.16544(15) 0.0574(7) Uani 1 1 d . U . . .
H37A H 0.800820 0.081601 0.122449 0.069 Uiso 1 1 calc R U . . .
H37B H 0.817526 0.051377 0.201879 0.069 Uiso 1 1 calc R U . . .
C20 C 0.55966(12) 0.2753(3) 0.18426(15) 0.0693(9) Uani 1 1 d . . . . .
H20A H 0.571798 0.191787 0.173449 0.104 Uiso 1 1 calc R U . . .
H20B H 0.519388 0.270728 0.188077 0.104 Uiso 1 1 calc R U . . .
H20C H 0.587221 0.304150 0.227186 0.104 Uiso 1 1 calc R U . . .
C29 C 0.61500(13) 0.3457(3) 0.39211(16) 0.0638(7) Uani 1 1 d . U . . .
H29A H 0.639121 0.337032 0.440057 0.077 Uiso 1 1 calc R U . . .
H29B H 0.629835 0.285184 0.364806 0.077 Uiso 1 1 calc R U . . .
C8 C 0.68949(13) 0.8598(2) 0.06625(13) 0.0554(7) Uani 1 1 d . . . . .
H8 H 0.680048 0.927696 0.035130 0.067 Uiso 1 1 calc R U . . .
C22 C 0.54097(12) 0.4990(3) 0.14467(18) 0.0738(9) Uani 1 1 d . . . . .
H22A H 0.567060 0.525989 0.188831 0.111 Uiso 1 1 calc R U . . .
H22B H 0.499905 0.494516 0.145969 0.111 Uiso 1 1 calc R U . . .
H22C H 0.543445 0.559489 0.110089 0.111 Uiso 1 1 calc R U . . .
C9 C 0.64822(13) 0.8164(3) 0.09576(15) 0.0593(7) Uani 1 1 d . . . . .
H9 H 0.610195 0.854851 0.084948 0.071 Uiso 1 1 calc R U . . .
C38 C 0.88190(14) -0.0119(3) 0.15964(15) 0.0645(7) Uani 1 1 d . U . . .
H38A H 0.878875 -0.093446 0.181344 0.077 Uiso 1 1 calc R U . . .
H38B H 0.878965 -0.026939 0.111734 0.077 Uiso 1 1 calc R U . . .
C33 C 0.68846(18) 0.8152(3) 0.39356(17) 0.0816(10) Uani 1 1 d . U . . .
H33A H 0.729911 0.784199 0.409833 0.098 Uiso 1 1 calc R U . . .
H33B H 0.668647 0.795393 0.427980 0.098 Uiso 1 1 calc R U . . .
C41 C 0.83279(16) 0.4658(3) 0.05743(15) 0.0714(8) Uani 1 1 d . U . . .
H41A H 0.789756 0.479184 0.049724 0.086 Uiso 1 1 calc R U . . .
H41B H 0.838618 0.380994 0.040915 0.086 Uiso 1 1 calc R U . . .
C36 C 0.62014(16) 0.8514(3) 0.28842(19) 0.0833(10) Uani 1 1 d . U . . .
H36A H 0.577678 0.828613 0.278242 0.100 Uiso 1 1 calc R U . . .
H36B H 0.629297 0.860199 0.245236 0.100 Uiso 1 1 calc R U . . .
C30 C 0.55015(16) 0.3222(4) 0.3838(2) 0.0847(10) Uani 1 1 d . U . . .
H30A H 0.529454 0.287401 0.338583 0.102 Uiso 1 1 calc R U . . .
H30B H 0.545335 0.263559 0.418741 0.102 Uiso 1 1 calc R U . . .
C42 C 0.8567(2) 0.5631(4) 0.02182(18) 0.0897(11) Uani 1 1 d . U . . .
H42A H 0.853803 0.535937 -0.024626 0.108 Uiso 1 1 calc R U . . .
H42B H 0.835335 0.643793 0.019711 0.108 Uiso 1 1 calc R U . . .
C34 C 0.68756(19) 0.9547(3) 0.3812(2) 0.0877(11) Uani 1 1 d . U . . .
H34A H 0.687338 1.002249 0.422078 0.105 Uiso 1 1 calc R U . . .
H34B H 0.722202 0.981217 0.367225 0.105 Uiso 1 1 calc R U . . .
C35 C 0.63267(18) 0.9722(3) 0.3273(3) 0.1068(13) Uani 1 1 d . U . . .
H35A H 0.636701 1.042070 0.297508 0.128 Uiso 1 1 calc R U . . .
H35B H 0.599896 0.992366 0.345956 0.128 Uiso 1 1 calc R U . . .
C32 C 0.56678(15) 0.5398(3) 0.3730(2) 0.0922(11) Uani 1 1 d . U . . .
H32A H 0.545880 0.578576 0.328855 0.111 Uiso 1 1 calc R U . . .
H32B H 0.578836 0.607437 0.407183 0.111 Uiso 1 1 calc R U . . .
C44 C 0.91870(15) 0.5466(4) 0.13467(19) 0.0917(11) Uani 1 1 d . U . . .
H44A H 0.953924 0.495713 0.158600 0.110 Uiso 1 1 calc R U . . .
H44B H 0.919355 0.625613 0.160045 0.110 Uiso 1 1 calc R U . . .
C39 C 0.93934(14) 0.0542(3) 0.19618(19) 0.0772(9) Uani 1 1 d . U . . .
H39A H 0.955700 0.022190 0.242914 0.093 Uiso 1 1 calc R U . . .
H39B H 0.969263 0.041842 0.172219 0.093 Uiso 1 1 calc R U . . .
C31 C 0.52710(18) 0.4502(4) 0.3923(3) 0.1164(14) Uani 1 1 d . U . . .
H31A H 0.485674 0.460218 0.362690 0.140 Uiso 1 1 calc R U . . .
H31B H 0.528095 0.463838 0.439697 0.140 Uiso 1 1 calc R U . . .
C40 C 0.92317(16) 0.1871(4) 0.1962(3) 0.1000(13) Uani 1 1 d . U . . .
H40A H 0.942673 0.224058 0.241252 0.120 Uiso 1 1 calc R U . . .
H40B H 0.936962 0.233433 0.162510 0.120 Uiso 1 1 calc R U . . .
C43 C 0.9182(2) 0.5742(5) 0.0632(2) 0.1216(15) Uani 1 1 d . U . . .
H43A H 0.933298 0.659991 0.059961 0.146 Uiso 1 1 calc R U . . .
H43B H 0.943373 0.513090 0.048502 0.146 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Na2 3.1050(9) . ?
Pb1 Na1 3.1423(9) . ?
Pb1 C4 2.2638(18) . ?
Pb1 C1 2.2672(19) . ?
Si2 C4 1.8369(19) . ?
Si2 C24 1.889(2) . ?
Si2 C25 1.924(2) . ?
Si2 C23 1.892(2) . ?
Si1 C1 1.835(2) . ?
Si1 C17 1.888(2) . ?
Si1 C18 1.881(3) . ?
Si1 C19 1.930(2) . ?
Na2 O4 2.3298(18) . ?
Na2 C4 2.788(2) . ?
Na2 C3 2.650(2) . ?
Na2 C2 2.667(2) . ?
Na2 O3 2.297(2) . ?
Na2 C1 2.758(2) . ?
Na1 O2 2.334(2) . ?
Na1 C4 2.744(2) . ?
Na1 O1 2.3224(19) . ?
Na1 C3 2.674(2) . ?
Na1 C2 2.694(2) . ?
Na1 C1 2.824(2) . ?
O4 C41 1.423(3) . ?
O4 C44 1.422(4) . ?
O2 C33 1.444(4) . ?
O2 C36 1.414(4) . ?
C4 C3 1.425(3) . ?
O1 C29 1.431(3) . ?
O1 C32 1.418(3) . ?
C3 C11 1.501(3) . ?
C3 C2 1.440(3) . ?
C5 C2 1.494(3) . ?
C5 C6 1.394(3) . ?
C5 C10 1.394(3) . ?
C11 C12 1.395(3) . ?
C11 C16 1.392(3) . ?
C2 C1 1.427(3) . ?
O3 C37 1.409(3) . ?
O3 C40 1.384(4) . ?
C6 H6 0.9400 . ?
C6 C7 1.388(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C12 H12 0.9400 . ?
C12 C13 1.383(3) . ?
C16 H16 0.9400 . ?
C16 C15 1.385(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C10 H10 0.9400 . ?
C10 C9 1.390(3) . ?
C13 H13 0.9400 . ?
C13 C14 1.379(3) . ?
C25 C27 1.528(3) . ?
C25 C28 1.538(3) . ?
C25 C26 1.526(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C15 H15 0.9400 . ?
C15 C14 1.378(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C14 H14 0.9400 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C19 C21 1.541(3) . ?
C19 C20 1.530(4) . ?
C19 C22 1.523(4) . ?
C7 H7 0.9400 . ?
C7 C8 1.373(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 C38 1.507(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 C30 1.494(4) . ?
C8 H8 0.9400 . ?
C8 C9 1.367(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C9 H9 0.9400 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 C39 1.496(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 C34 1.489(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 C42 1.465(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 C35 1.484(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 C31 1.481(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 C43 1.435(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 C35 1.430(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 C31 1.460(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 C43 1.496(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 C40 1.449(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 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
Na2 Pb1 Na1 99.05(2) . . ?
C4 Pb1 Na2 60.16(5) . . ?
C4 Pb1 Na1 58.33(5) . . ?
C4 Pb1 C1 77.39(7) . . ?
C1 Pb1 Na2 59.36(5) . . ?
C1 Pb1 Na1 60.39(5) . . ?
C4 Si2 C24 116.63(10) . . ?
C4 Si2 C25 114.31(9) . . ?
C4 Si2 C23 108.60(10) . . ?
C24 Si2 C25 107.14(10) . . ?
C24 Si2 C23 103.28(11) . . ?
C23 Si2 C25 105.80(11) . . ?
C1 Si1 C17 116.15(10) . . ?
C1 Si1 C18 108.86(10) . . ?
C1 Si1 C19 114.00(10) . . ?
C17 Si1 C19 107.24(11) . . ?
C18 Si1 C17 104.28(13) . . ?
C18 Si1 C19 105.36(13) . . ?
O4 Na2 Pb1 170.10(6) . . ?
O4 Na2 C4 134.20(7) . . ?
O4 Na2 C3 110.39(7) . . ?
O4 Na2 C2 106.49(7) . . ?
O4 Na2 C1 125.10(7) . . ?
C4 Na2 Pb1 44.78(4) . . ?
C3 Na2 Pb1 64.44(4) . . ?
C3 Na2 C4 30.26(6) . . ?
C3 Na2 C2 31.42(6) . . ?
C3 Na2 C1 54.23(6) . . ?
C2 Na2 Pb1 64.50(4) . . ?
C2 Na2 C4 53.97(6) . . ?
C2 Na2 C1 30.45(6) . . ?
O3 Na2 Pb1 102.13(6) . . ?
O3 Na2 O4 85.65(8) . . ?
O3 Na2 C4 126.07(9) . . ?
O3 Na2 C3 155.56(9) . . ?
O3 Na2 C2 161.69(8) . . ?
O3 Na2 C1 131.26(8) . . ?
C1 Na2 Pb1 45.02(4) . . ?
C1 Na2 C4 61.43(6) . . ?
O2 Na1 Pb1 171.24(6) . . ?
O2 Na1 C4 127.46(7) . . ?
O2 Na1 C3 107.61(7) . . ?
O2 Na1 C2 109.30(7) . . ?
O2 Na1 C1 131.70(7) . . ?
C4 Na1 Pb1 44.60(4) . . ?
C4 Na1 C1 61.14(6) . . ?
O1 Na1 Pb1 98.22(6) . . ?
O1 Na1 O2 90.05(7) . . ?
O1 Na1 C4 125.64(7) . . ?
O1 Na1 C3 156.11(7) . . ?
O1 Na1 C2 154.81(8) . . ?
O1 Na1 C1 125.01(8) . . ?
C3 Na1 Pb1 63.64(4) . . ?
C3 Na1 C4 30.47(6) . . ?
C3 Na1 C2 31.11(6) . . ?
C3 Na1 C1 53.23(6) . . ?
C2 Na1 Pb1 63.69(4) . . ?
C2 Na1 C4 54.20(6) . . ?
C2 Na1 C1 29.87(5) . . ?
C1 Na1 Pb1 44.27(4) . . ?
C41 O4 Na2 112.53(16) . . ?
C44 O4 Na2 138.88(19) . . ?
C44 O4 C41 108.6(2) . . ?
C33 O2 Na1 118.68(19) . . ?
C36 O2 Na1 134.1(2) . . ?
C36 O2 C33 106.9(2) . . ?
Pb1 C4 Na2 75.06(6) . . ?
Pb1 C4 Na1 77.07(6) . . ?
Si2 C4 Pb1 116.50(9) . . ?
Si2 C4 Na2 131.29(9) . . ?
Si2 C4 Na1 110.26(9) . . ?
Na1 C4 Na2 118.44(7) . . ?
C3 C4 Pb1 111.90(13) . . ?
C3 C4 Si2 130.78(14) . . ?
C3 C4 Na2 69.54(10) . . ?
C3 C4 Na1 72.07(10) . . ?
C29 O1 Na1 126.97(16) . . ?
C32 O1 Na1 123.18(18) . . ?
C32 O1 C29 108.3(2) . . ?
Na2 C3 Na1 126.38(7) . . ?
C4 C3 Na2 80.21(11) . . ?
C4 C3 Na1 77.46(11) . . ?
C4 C3 C11 119.45(16) . . ?
C4 C3 C2 119.69(16) . . ?
C11 C3 Na2 116.03(12) . . ?
C11 C3 Na1 117.45(12) . . ?
C2 C3 Na2 74.93(10) . . ?
C2 C3 Na1 75.17(10) . . ?
C2 C3 C11 120.85(16) . . ?
C6 C5 C2 122.60(18) . . ?
C10 C5 C2 121.24(19) . . ?
C10 C5 C6 116.16(19) . . ?
C12 C11 C3 120.14(18) . . ?
C16 C11 C3 122.73(18) . . ?
C16 C11 C12 117.04(18) . . ?
Na2 C2 Na1 124.88(7) . . ?
C3 C2 Na2 73.65(10) . . ?
C3 C2 Na1 73.71(10) . . ?
C3 C2 C5 119.70(16) . . ?
C5 C2 Na2 117.48(12) . . ?
C5 C2 Na1 117.10(12) . . ?
C1 C2 Na2 78.30(11) . . ?
C1 C2 Na1 80.13(11) . . ?
C1 C2 C3 118.74(16) . . ?
C1 C2 C5 121.56(17) . . ?
C37 O3 Na2 125.64(16) . . ?
C40 O3 Na2 122.8(2) . . ?
C40 O3 C37 110.7(2) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.8(2) . . ?
C7 C6 H6 119.1 . . ?
Pb1 C1 Na2 75.62(6) . . ?
Pb1 C1 Na1 75.34(6) . . ?
Si1 C1 Pb1 115.70(9) . . ?
Si1 C1 Na2 116.37(9) . . ?
Si1 C1 Na1 126.83(9) . . ?
Na2 C1 Na1 116.72(7) . . ?
C2 C1 Pb1 112.22(13) . . ?
C2 C1 Si1 131.84(15) . . ?
C2 C1 Na2 71.25(10) . . ?
C2 C1 Na1 70.00(11) . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.6(2) . . ?
C13 C12 H12 119.2 . . ?
C11 C16 H16 119.4 . . ?
C15 C16 C11 121.2(2) . . ?
C15 C16 H16 119.4 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C5 C10 H10 119.1 . . ?
C9 C10 C5 121.9(2) . . ?
C9 C10 H10 119.1 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.8 . . ?
C27 C25 Si2 110.89(16) . . ?
C27 C25 C28 107.9(2) . . ?
C28 C25 Si2 110.01(17) . . ?
C26 C25 Si2 111.31(16) . . ?
C26 C25 C27 108.4(2) . . ?
C26 C25 C28 108.2(2) . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C16 C15 H15 119.7 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.7 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 H14 120.5 . . ?
C15 C14 C13 119.0(2) . . ?
C15 C14 H14 120.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C21 C19 Si1 109.96(19) . . ?
C20 C19 Si1 110.45(17) . . ?
C20 C19 C21 108.1(2) . . ?
C22 C19 Si1 110.90(17) . . ?
C22 C19 C21 108.2(2) . . ?
C22 C19 C20 109.1(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.5(2) . . ?
C8 C7 H7 119.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C37 H37A 110.5 . . ?
O3 C37 H37B 110.5 . . ?
O3 C37 C38 106.1(2) . . ?
H37A C37 H37B 108.7 . . ?
C38 C37 H37A 110.5 . . ?
C38 C37 H37B 110.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C29 H29A 110.6 . . ?
O1 C29 H29B 110.6 . . ?
O1 C29 C30 105.6(2) . . ?
H29A C29 H29B 108.7 . . ?
C30 C29 H29A 110.6 . . ?
C30 C29 H29B 110.6 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(2) . . ?
C9 C8 H8 120.4 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C10 C9 H9 119.7 . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9 119.7 . . ?
C37 C38 H38A 110.9 . . ?
C37 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
C39 C38 C37 104.2(2) . . ?
C39 C38 H38A 110.9 . . ?
C39 C38 H38B 110.9 . . ?
O2 C33 H33A 110.4 . . ?
O2 C33 H33B 110.4 . . ?
O2 C33 C34 106.8(3) . . ?
H33A C33 H33B 108.6 . . ?
C34 C33 H33A 110.4 . . ?
C34 C33 H33B 110.4 . . ?
O4 C41 H41A 110.4 . . ?
O4 C41 H41B 110.4 . . ?
O4 C41 C42 106.6(3) . . ?
H41A C41 H41B 108.6 . . ?
C42 C41 H41A 110.4 . . ?
C42 C41 H41B 110.4 . . ?
O2 C36 H36A 110.2 . . ?
O2 C36 H36B 110.2 . . ?
O2 C36 C35 107.5(3) . . ?
H36A C36 H36B 108.5 . . ?
C35 C36 H36A 110.2 . . ?
C35 C36 H36B 110.2 . . ?
C29 C30 H30A 111.1 . . ?
C29 C30 H30B 111.1 . . ?
H30A C30 H30B 109.1 . . ?
C31 C30 C29 103.3(3) . . ?
C31 C30 H30A 111.1 . . ?
C31 C30 H30B 111.1 . . ?
C41 C42 H42A 111.1 . . ?
C41 C42 H42B 111.1 . . ?
H42A C42 H42B 109.1 . . ?
C43 C42 C41 103.1(3) . . ?
C43 C42 H42A 111.1 . . ?
C43 C42 H42B 111.1 . . ?
C33 C34 H34A 111.2 . . ?
C33 C34 H34B 111.2 . . ?
H34A C34 H34B 109.1 . . ?
C35 C34 C33 102.9(3) . . ?
C35 C34 H34A 111.2 . . ?
C35 C34 H34B 111.2 . . ?
C36 C35 H35A 110.3 . . ?
C36 C35 H35B 110.3 . . ?
C34 C35 C36 106.9(3) . . ?
C34 C35 H35A 110.3 . . ?
C34 C35 H35B 110.3 . . ?
H35A C35 H35B 108.6 . . ?
O1 C32 H32A 110.0 . . ?
O1 C32 H32B 110.0 . . ?
O1 C32 C31 108.4(3) . . ?
H32A C32 H32B 108.4 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
O4 C44 H44A 110.7 . . ?
O4 C44 H44B 110.7 . . ?
O4 C44 C43 105.3(3) . . ?
H44A C44 H44B 108.8 . . ?
C43 C44 H44A 110.7 . . ?
C43 C44 H44B 110.7 . . ?
C38 C39 H39A 110.8 . . ?
C38 C39 H39B 110.8 . . ?
H39A C39 H39B 108.9 . . ?
C40 C39 C38 104.8(3) . . ?
C40 C39 H39A 110.8 . . ?
C40 C39 H39B 110.8 . . ?
C30 C31 H31A 110.6 . . ?
C30 C31 H31B 110.6 . . ?
C32 C31 C30 105.8(3) . . ?
C32 C31 H31A 110.6 . . ?
C32 C31 H31B 110.6 . . ?
H31A C31 H31B 108.7 . . ?
O3 C40 C39 109.6(3) . . ?
O3 C40 H40A 109.8 . . ?
O3 C40 H40B 109.8 . . ?
C39 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
H40A C40 H40B 108.2 . . ?
C42 C43 C44 105.9(3) . . ?
C42 C43 H43A 110.6 . . ?
C42 C43 H43B 110.6 . . ?
C44 C43 H43A 110.6 . . ?
C44 C43 H43B 110.6 . . ?
H43A C43 H43B 108.7 . . ?

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 C4 C3 Na2 -63.47(9) . . . . ?
Pb1 C4 C3 Na1 67.45(9) . . . . ?
Pb1 C4 C3 C11 -177.93(13) . . . . ?
Pb1 C4 C3 C2 2.8(2) . . . . ?
Si2 C4 C3 Na2 127.46(16) . . . . ?
Si2 C4 C3 Na1 -101.62(16) . . . . ?
Si2 C4 C3 C11 13.0(3) . . . . ?
Si2 C4 C3 C2 -166.25(15) . . . . ?
Na2 O4 C41 C42 161.1(2) . . . . ?
Na2 O4 C44 C43 179.3(3) . . . . ?
Na2 C4 C3 Na1 130.92(6) . . . . ?
Na2 C4 C3 C11 -114.45(16) . . . . ?
Na2 C4 C3 C2 66.30(15) . . . . ?
Na2 C3 C11 C12 -33.3(2) . . . . ?
Na2 C3 C11 C16 150.40(16) . . . . ?
Na2 C3 C2 Na1 134.96(6) . . . . ?
Na2 C3 C2 C5 -112.72(16) . . . . ?
Na2 C3 C2 C1 66.30(16) . . . . ?
Na2 C2 C1 Pb1 65.04(9) . . . . ?
Na2 C2 C1 Si1 -109.01(17) . . . . ?
Na2 C2 C1 Na1 128.97(6) . . . . ?
Na2 O3 C37 C38 -179.33(19) . . . . ?
Na2 O3 C40 C39 165.7(3) . . . . ?
Na1 O2 C33 C34 153.2(2) . . . . ?
Na1 O2 C36 C35 -169.1(2) . . . . ?
Na1 C4 C3 Na2 -130.92(6) . . . . ?
Na1 C4 C3 C11 114.63(16) . . . . ?
Na1 C4 C3 C2 -64.62(15) . . . . ?
Na1 O1 C29 C30 -143.5(2) . . . . ?
Na1 O1 C32 C31 160.4(3) . . . . ?
Na1 C3 C11 C12 150.73(16) . . . . ?
Na1 C3 C11 C16 -25.5(2) . . . . ?
Na1 C3 C2 Na2 -134.96(6) . . . . ?
Na1 C3 C2 C5 112.31(16) . . . . ?
Na1 C3 C2 C1 -68.66(15) . . . . ?
Na1 C2 C1 Pb1 -63.92(9) . . . . ?
Na1 C2 C1 Si1 122.03(17) . . . . ?
Na1 C2 C1 Na2 -128.97(6) . . . . ?
O4 C41 C42 C43 31.2(4) . . . . ?
O4 C44 C43 C42 20.8(5) . . . . ?
O2 C33 C34 C35 29.9(4) . . . . ?
O2 C36 C35 C34 15.8(5) . . . . ?
C4 C3 C11 C12 60.0(3) . . . . ?
C4 C3 C11 C16 -116.2(2) . . . . ?
C4 C3 C2 Na2 -69.13(16) . . . . ?
C4 C3 C2 Na1 65.83(15) . . . . ?
C4 C3 C2 C5 178.14(17) . . . . ?
C4 C3 C2 C1 -2.8(3) . . . . ?
O1 C29 C30 C31 -29.5(4) . . . . ?
O1 C32 C31 C30 -12.7(5) . . . . ?
C3 C11 C12 C13 -173.1(2) . . . . ?
C3 C11 C16 C15 172.99(19) . . . . ?
C3 C2 C1 Pb1 1.2(2) . . . . ?
C3 C2 C1 Si1 -172.81(14) . . . . ?
C3 C2 C1 Na2 -63.80(15) . . . . ?
C3 C2 C1 Na1 65.16(15) . . . . ?
C5 C2 C1 Pb1 -179.76(14) . . . . ?
C5 C2 C1 Si1 6.2(3) . . . . ?
C5 C2 C1 Na2 115.20(17) . . . . ?
C5 C2 C1 Na1 -115.83(17) . . . . ?
C5 C6 C7 C8 0.7(4) . . . . ?
C5 C10 C9 C8 0.1(4) . . . . ?
C11 C3 C2 Na2 111.63(16) . . . . ?
C11 C3 C2 Na1 -113.41(16) . . . . ?
C11 C3 C2 C5 -1.1(3) . . . . ?
C11 C3 C2 C1 177.93(17) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C11 C16 C15 C14 0.8(4) . . . . ?
C2 C3 C11 C12 -120.7(2) . . . . ?
C2 C3 C11 C16 63.0(3) . . . . ?
C2 C5 C6 C7 178.6(2) . . . . ?
C2 C5 C10 C9 -179.0(2) . . . . ?
O3 C37 C38 C39 19.5(3) . . . . ?
C6 C5 C2 Na2 -24.8(2) . . . . ?
C6 C5 C2 Na1 147.20(16) . . . . ?
C6 C5 C2 C3 61.3(3) . . . . ?
C6 C5 C2 C1 -117.7(2) . . . . ?
C6 C5 C10 C9 0.3(4) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
C17 Si1 C1 Pb1 -157.27(11) . . . . ?
C17 Si1 C1 Na2 -71.23(13) . . . . ?
C17 Si1 C1 Na1 112.19(13) . . . . ?
C17 Si1 C1 C2 16.6(2) . . . . ?
C12 C11 C16 C15 -3.4(3) . . . . ?
C12 C13 C14 C15 -1.9(4) . . . . ?
C16 C11 C12 C13 3.4(3) . . . . ?
C16 C15 C14 C13 1.9(4) . . . . ?
C24 Si2 C4 Pb1 -155.68(11) . . . . ?
C24 Si2 C4 Na2 111.20(14) . . . . ?
C24 Si2 C4 Na1 -70.41(12) . . . . ?
C24 Si2 C4 C3 13.0(2) . . . . ?
C10 C5 C2 Na2 154.37(17) . . . . ?
C10 C5 C2 Na1 -33.6(2) . . . . ?
C10 C5 C2 C3 -119.6(2) . . . . ?
C10 C5 C2 C1 61.4(3) . . . . ?
C10 C5 C6 C7 -0.7(3) . . . . ?
C25 Si2 C4 Pb1 78.28(12) . . . . ?
C25 Si2 C4 Na2 -14.84(15) . . . . ?
C25 Si2 C4 Na1 163.55(9) . . . . ?
C25 Si2 C4 C3 -113.05(19) . . . . ?
C23 Si2 C4 Pb1 -39.58(14) . . . . ?
C23 Si2 C4 Na2 -132.70(13) . . . . ?
C23 Si2 C4 Na1 45.69(13) . . . . ?
C23 Si2 C4 C3 129.09(19) . . . . ?
C18 Si1 C1 Pb1 -40.01(15) . . . . ?
C18 Si1 C1 Na2 46.04(14) . . . . ?
C18 Si1 C1 Na1 -130.55(14) . . . . ?
C18 Si1 C1 C2 133.9(2) . . . . ?
C19 Si1 C1 Pb1 77.28(13) . . . . ?
C19 Si1 C1 Na2 163.32(10) . . . . ?
C19 Si1 C1 Na1 -13.26(15) . . . . ?
C19 Si1 C1 C2 -108.8(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C37 O3 C40 C39 -3.6(5) . . . . ?
C37 C38 C39 C40 -21.3(4) . . . . ?
C29 O1 C32 C31 -6.2(5) . . . . ?
C29 C30 C31 C32 25.6(5) . . . . ?
C38 C39 C40 O3 16.0(5) . . . . ?
C33 O2 C36 C35 3.5(4) . . . . ?
C33 C34 C35 C36 -27.4(4) . . . . ?
C41 O4 C44 C43 -1.1(4) . . . . ?
C41 C42 C43 C44 -31.4(5) . . . . ?
C36 O2 C33 C34 -20.7(4) . . . . ?
C32 O1 C29 C30 22.5(4) . . . . ?
C44 O4 C41 C42 -18.7(4) . . . . ?
C40 O3 C37 C38 -10.3(4) . . . . ?

_olex2_date_sample_completion    2021-12-01
_olex2_date_sample_data_collection 2021-05-06
_olex2_date_sample_submission    2021-05-05
_olex2_exptl_crystal_mounting_method 
'Crystal chosen cut from a larger cluster of interpenetrated crystals. Mounted on a 200 uM MicroLoop using Parabar 10312 oil'
_olex2_submission_original_sample_id RDA63-97_S0953
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
