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

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

data_xbic
_database_code_depnum_ccdc_archive 'CCDC 1922351'
loop_
_audit_author_name
_audit_author_address
'Allen G. Oliver'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dihydroxy-benzaldimine)
_chemical_name_common            XbicH4
_chemical_melting_point          .
_chemical_formula_moiety         'C45 H56 N2 O5'
_chemical_formula_sum            'C45 H56 N2 O5'
_chemical_formula_weight         704.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8219(5)
_cell_length_b                   14.8289(8)
_cell_length_c                   15.3393(8)
_cell_angle_alpha                68.6189(17)
_cell_angle_beta                 80.0462(18)
_cell_angle_gamma                73.9409(17)
_cell_volume                     1992.71(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7625
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25.84

_exptl_crystal_description       'polyhedron block'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   0.6597
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.111
_exptl_absorpt_coefficient_mu    0.076
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6597
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_recrystallization_method 
'Crystals were deposited by slow evaporationof XbicH4 in acetone.'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            49269
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.430
_diffrn_reflns_theta_max         28.600
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10186
_reflns_number_gt                6747
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;All hydrogens were found on the difference Fourier map and refined 
isotropically.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0675P)²+0.2363P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10186
_refine_ls_number_parameters     693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.48938(12) 0.21640(8) 0.40787(8) 0.0259(3) Uani 1 1 d . . . . .
H1 H 0.441(2) 0.1872(17) 0.4606(16) 0.053(7) Uiso 1 1 d . . . . .
O2 O 0.22425(12) 0.24595(8) 0.47367(7) 0.0225(2) Uani 1 1 d . . . . .
H2 H 0.123(3) 0.2624(18) 0.4905(16) 0.073(8) Uiso 1 1 d . . . . .
O3 O 0.24565(12) 0.23273(9) 0.21100(9) 0.0311(3) Uani 1 1 d . . . . .
H3 H 0.216(3) 0.2459(18) 0.2671(17) 0.065(7) Uiso 1 1 d . . . . .
O4 O 0.05795(12) 0.18471(8) 0.35007(8) 0.0251(3) Uani 1 1 d . . . . .
H4 H -0.013(2) 0.1559(16) 0.3995(15) 0.050(6) Uiso 1 1 d . . . . .
O5 O -0.19307(10) 0.21538(7) 0.52557(7) 0.0201(2) Uani 1 1 d . . . . .
N1 N -0.02937(13) 0.34543(9) 0.46256(9) 0.0197(3) Uani 1 1 d . . . . .
N2 N -0.12081(13) 0.08569(9) 0.43847(8) 0.0188(3) Uani 1 1 d . . . . .
C11 C 0.39563(15) 0.29699(11) 0.35503(10) 0.0195(3) Uani 1 1 d . . . . .
C12 C 0.25346(16) 0.31213(11) 0.38921(10) 0.0188(3) Uani 1 1 d . . . . .
C13 C 0.15031(15) 0.39224(11) 0.33899(10) 0.0180(3) Uani 1 1 d . . . . .
C14 C 0.19237(16) 0.45656(11) 0.25066(11) 0.0214(3) Uani 1 1 d . . . . .
C15 C 0.33559(16) 0.43907(12) 0.22131(11) 0.0216(3) Uani 1 1 d . . . . .
H15 H 0.3681(17) 0.4841(12) 0.1633(11) 0.019(4) Uiso 1 1 d . . . . .
C16 C 0.44090(15) 0.36133(11) 0.27140(10) 0.0197(3) Uani 1 1 d . . . . .
C17 C 0.59769(16) 0.34943(12) 0.23493(11) 0.0234(3) Uani 1 1 d . . . . .
C171 C 0.6515(2) 0.25044(15) 0.21628(16) 0.0362(4) Uani 1 1 d . . . . .
H17C H 0.642(2) 0.1904(17) 0.2769(16) 0.055(6) Uiso 1 1 d . . . . .
H17B H 0.601(2) 0.2501(16) 0.1664(15) 0.049(6) Uiso 1 1 d . . . . .
H17A H 0.754(2) 0.2438(15) 0.1924(13) 0.043(5) Uiso 1 1 d . . . . .
C172 C 0.68430(19) 0.35041(15) 0.30806(13) 0.0295(4) Uani 1 1 d . . . . .
H17F H 0.659(2) 0.4137(16) 0.3194(14) 0.046(6) Uiso 1 1 d . . . . .
H17E H 0.668(2) 0.3018(15) 0.3688(14) 0.038(5) Uiso 1 1 d . . . . .
H17D H 0.782(2) 0.3454(14) 0.2837(13) 0.041(5) Uiso 1 1 d . . . . .
C173 C 0.62191(19) 0.43283(16) 0.14406(13) 0.0352(4) Uani 1 1 d . . . . .
H17I H 0.571(2) 0.4349(14) 0.0909(14) 0.040(5) Uiso 1 1 d . . . . .
H17H H 0.589(2) 0.5019(16) 0.1517(14) 0.045(6) Uiso 1 1 d . . . . .
H17G H 0.721(2) 0.4250(14) 0.1250(13) 0.041(5) Uiso 1 1 d . . . . .
C18 C 0.08687(17) 0.54171(13) 0.18590(12) 0.0311(4) Uani 1 1 d . . . . .
C181 C 0.1605(2) 0.59021(19) 0.09005(15) 0.0508(6) Uani 1 1 d . . . . .
H18C H 0.090(2) 0.6420(16) 0.0493(15) 0.050(6) Uiso 1 1 d . . . . .
H18B H 0.231(2) 0.6247(15) 0.0942(14) 0.047(6) Uiso 1 1 d . . . . .
H18A H 0.211(3) 0.5370(18) 0.0545(16) 0.064(7) Uiso 1 1 d . . . . .
C182 C 0.0211(2) 0.62445(14) 0.22833(18) 0.0446(5) Uani 1 1 d . . . . .
H18F H -0.044(3) 0.685(2) 0.1826(18) 0.077(8) Uiso 1 1 d . . . . .
H18E H -0.039(2) 0.6052(17) 0.2950(16) 0.058(6) Uiso 1 1 d . . . . .
H18D H 0.094(3) 0.6540(18) 0.2381(16) 0.064(7) Uiso 1 1 d . . . . .
C183 C -0.0263(2) 0.50021(17) 0.16559(14) 0.0384(5) Uani 1 1 d . . . . .
H18I H 0.020(3) 0.444(2) 0.1359(18) 0.081(8) Uiso 1 1 d . . . . .
H18H H -0.089(2) 0.4707(16) 0.2210(15) 0.052(6) Uiso 1 1 d . . . . .
H18G H -0.087(2) 0.5534(17) 0.1184(15) 0.054(6) Uiso 1 1 d . . . . .
C19 C 0.00632(16) 0.40698(11) 0.38413(11) 0.0194(3) Uani 1 1 d . . . . .
H19 H -0.0623(17) 0.4646(12) 0.3531(10) 0.015(4) Uiso 1 1 d . . . . .
C21 C 0.17555(16) 0.16471(11) 0.21210(11) 0.0209(3) Uani 1 1 d . . . . .
C22 C 0.07549(16) 0.13765(11) 0.28714(10) 0.0202(3) Uani 1 1 d . . . . .
C23 C -0.00173(15) 0.06834(11) 0.29425(10) 0.0184(3) Uani 1 1 d . . . . .
C24 C 0.02476(15) 0.02453(11) 0.22262(10) 0.0186(3) Uani 1 1 d . . . . .
C25 C 0.12442(15) 0.05455(11) 0.14992(11) 0.0201(3) Uani 1 1 d . . . . .
H25 H 0.1420(17) 0.0259(12) 0.1011(12) 0.024(4) Uiso 1 1 d . . . . .
C26 C 0.20203(15) 0.12372(11) 0.14144(10) 0.0202(3) Uani 1 1 d . . . . .
C27 C 0.31090(16) 0.15289(12) 0.05869(11) 0.0238(3) Uani 1 1 d . . . . .
C271 C 0.3183(2) 0.10034(18) -0.01154(13) 0.0375(5) Uani 1 1 d . . . . .
H27C H 0.347(2) 0.0235(16) 0.0205(13) 0.040(5) Uiso 1 1 d . . . . .
H27B H 0.388(2) 0.1256(15) -0.0637(15) 0.049(6) Uiso 1 1 d . . . . .
H27A H 0.222(2) 0.1214(16) -0.0417(15) 0.058(6) Uiso 1 1 d . . . . .
C272 C 0.45841(18) 0.12223(15) 0.09478(13) 0.0298(4) Uani 1 1 d . . . . .
H27F H 0.484(2) 0.0482(17) 0.1267(14) 0.047(6) Uiso 1 1 d . . . . .
H27E H 0.4623(19) 0.1482(14) 0.1425(13) 0.035(5) Uiso 1 1 d . . . . .
H27D H 0.528(2) 0.1480(14) 0.0408(14) 0.040(5) Uiso 1 1 d . . . . .
C273 C 0.2726(2) 0.26500(15) 0.00757(15) 0.0420(5) Uani 1 1 d . . . . .
H27I H 0.178(3) 0.2849(18) -0.0142(16) 0.070(8) Uiso 1 1 d . . . . .
H27H H 0.274(2) 0.3040(16) 0.0501(15) 0.050(6) Uiso 1 1 d . . . . .
H27G H 0.341(2) 0.2868(15) -0.0477(15) 0.047(6) Uiso 1 1 d . . . . .
C28 C -0.05429(15) -0.05136(11) 0.22172(10) 0.0195(3) Uani 1 1 d . . . . .
C281 C -0.21167(17) -0.00065(13) 0.20483(13) 0.0260(4) Uani 1 1 d . . . . .
H28C H -0.2665(19) 0.0226(13) 0.2584(13) 0.034(5) Uiso 1 1 d . . . . .
H28B H -0.2598(18) -0.0519(13) 0.1994(12) 0.029(5) Uiso 1 1 d . . . . .
H28A H -0.2175(18) 0.0578(14) 0.1451(13) 0.029(5) Uiso 1 1 d . . . . .
C282 C -0.0396(2) -0.14220(13) 0.31164(12) 0.0269(4) Uani 1 1 d . . . . .
H28F H 0.062(2) -0.1800(15) 0.3178(13) 0.042(5) Uiso 1 1 d . . . . .
H28E H -0.0686(19) -0.1236(14) 0.3706(13) 0.037(5) Uiso 1 1 d . . . . .
H28D H -0.097(2) -0.1880(15) 0.3111(13) 0.041(5) Uiso 1 1 d . . . . .
C283 C 0.00410(18) -0.09219(13) 0.14086(12) 0.0246(3) Uani 1 1 d . . . . .
H28I H 0.108(2) -0.1246(14) 0.1431(13) 0.041(5) Uiso 1 1 d . . . . .
H28H H -0.0058(17) -0.0408(13) 0.0772(12) 0.023(4) Uiso 1 1 d . . . . .
H28G H -0.0488(19) -0.1417(13) 0.1452(12) 0.029(5) Uiso 1 1 d . . . . .
C29 C -0.10908(16) 0.05029(11) 0.37189(10) 0.0197(3) Uani 1 1 d . . . . .
H29 H -0.1763(18) 0.0128(13) 0.3714(11) 0.027(4) Uiso 1 1 d . . . . .
C31 C -0.16353(15) 0.37112(11) 0.50945(10) 0.0195(3) Uani 1 1 d . . . . .
C32 C -0.24454(15) 0.30032(11) 0.54910(10) 0.0177(3) Uani 1 1 d . . . . .
C33 C -0.36712(15) 0.31524(11) 0.60702(10) 0.0197(3) Uani 1 1 d . . . . .
C34 C -0.41132(18) 0.40725(13) 0.62037(12) 0.0277(4) Uani 1 1 d . . . . .
H34 H -0.499(2) 0.4217(15) 0.6598(14) 0.044(5) Uiso 1 1 d . . . . .
C35 C -0.33646(18) 0.47988(13) 0.57885(13) 0.0309(4) Uani 1 1 d . . . . .
H35 H -0.369(2) 0.5451(15) 0.5907(12) 0.036(5) Uiso 1 1 d . . . . .
C36 C -0.21160(18) 0.46159(12) 0.52427(12) 0.0262(4) Uani 1 1 d . . . . .
H36 H -0.1543(17) 0.5108(13) 0.4970(11) 0.023(4) Uiso 1 1 d . . . . .
C41 C -0.23138(15) 0.07345(11) 0.51052(10) 0.0180(3) Uani 1 1 d . . . . .
C42 C -0.29983(17) -0.00348(12) 0.53938(11) 0.0226(3) Uani 1 1 d . . . . .
H42 H -0.2687(19) -0.0581(14) 0.5127(12) 0.033(5) Uiso 1 1 d . . . . .
C43 C -0.41316(18) -0.00517(13) 0.60685(11) 0.0266(4) Uani 1 1 d . . . . .
H43 H -0.4598(18) -0.0587(13) 0.6285(12) 0.025(4) Uiso 1 1 d . . . . .
C44 C -0.45920(17) 0.07090(12) 0.64382(11) 0.0247(3) Uani 1 1 d . . . . .
H44 H -0.539(2) 0.0682(13) 0.6908(12) 0.032(5) Uiso 1 1 d . . . . .
C45 C -0.39159(15) 0.14867(11) 0.61789(10) 0.0195(3) Uani 1 1 d . . . . .
C46 C -0.27406(15) 0.14609(11) 0.55374(10) 0.0170(3) Uani 1 1 d . . . . .
C1 C -0.44435(16) 0.23283(12) 0.65857(11) 0.0219(3) Uani 1 1 d . . . . .
C2 C -0.4128(2) 0.19146(16) 0.76231(12) 0.0355(4) Uani 1 1 d . . . . .
H2C H -0.444(2) 0.2421(15) 0.7912(14) 0.045(6) Uiso 1 1 d . . . . .
H2B H -0.304(3) 0.1655(17) 0.7653(15) 0.060(7) Uiso 1 1 d . . . . .
H2A H -0.465(2) 0.1353(15) 0.7997(14) 0.043(6) Uiso 1 1 d . . . . .
C3 C -0.60474(19) 0.27281(16) 0.65126(18) 0.0386(5) Uani 1 1 d . . . . .
H3C H -0.625(2) 0.2980(17) 0.5830(17) 0.060(7) Uiso 1 1 d . . . . .
H3B H -0.657(2) 0.2205(16) 0.6840(14) 0.046(6) Uiso 1 1 d . . . . .
H3A H -0.641(2) 0.3254(17) 0.6821(15) 0.054(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C11 1.3697(18) . ?
O1 H1 0.89(2) . ?
O2 C12 1.3506(18) . ?
O2 H2 0.97(3) . ?
O3 C21 1.3636(18) . ?
O3 H3 0.93(2) . ?
O4 C22 1.3474(18) . ?
O4 H4 1.00(2) . ?
O5 C46 1.3730(17) . ?
O5 C32 1.3741(17) . ?
N1 C19 1.2782(19) . ?
N1 C31 1.4118(18) . ?
N2 C29 1.2840(19) . ?
N2 C41 1.4077(18) . ?
C11 C16 1.378(2) . ?
C11 C12 1.391(2) . ?
C12 C13 1.403(2) . ?
C13 C14 1.414(2) . ?
C13 C19 1.459(2) . ?
C14 C15 1.383(2) . ?
C14 C18 1.540(2) . ?
C15 C16 1.399(2) . ?
C15 H15 0.963(16) . ?
C16 C17 1.530(2) . ?
C17 C173 1.523(2) . ?
C17 C172 1.527(2) . ?
C17 C171 1.530(2) . ?
C171 H17C 1.04(2) . ?
C171 H17B 0.98(2) . ?
C171 H17A 1.00(2) . ?
C172 H17F 0.97(2) . ?
C172 H17E 0.97(2) . ?
C172 H17D 0.96(2) . ?
C173 H17I 1.02(2) . ?
C173 H17H 1.03(2) . ?
C173 H17G 0.95(2) . ?
C18 C182 1.531(3) . ?
C18 C183 1.533(3) . ?
C18 C181 1.533(3) . ?
C181 H18C 0.98(2) . ?
C181 H18B 0.99(2) . ?
C181 H18A 1.08(2) . ?
C182 H18F 1.04(3) . ?
C182 H18E 1.07(2) . ?
C182 H18D 0.99(2) . ?
C183 H18I 1.05(3) . ?
C183 H18H 1.00(2) . ?
C183 H18G 0.99(2) . ?
C19 H19 0.952(16) . ?
C21 C26 1.381(2) . ?
C21 C22 1.394(2) . ?
C22 C23 1.402(2) . ?
C23 C24 1.423(2) . ?
C23 C29 1.446(2) . ?
C24 C25 1.379(2) . ?
C24 C28 1.539(2) . ?
C25 C26 1.397(2) . ?
C25 H25 0.957(17) . ?
C26 C27 1.526(2) . ?
C27 C273 1.525(3) . ?
C27 C271 1.525(2) . ?
C27 C272 1.530(2) . ?
C271 H27C 1.04(2) . ?
C271 H27B 0.99(2) . ?
C271 H27A 1.04(2) . ?
C272 H27F 1.00(2) . ?
C272 H27E 0.95(2) . ?
C272 H27D 1.01(2) . ?
C273 H27I 0.98(3) . ?
C273 H27H 1.02(2) . ?
C273 H27G 1.00(2) . ?
C28 C283 1.531(2) . ?
C28 C282 1.531(2) . ?
C28 C281 1.541(2) . ?
C281 H28C 1.018(19) . ?
C281 H28B 1.033(18) . ?
C281 H28A 1.003(18) . ?
C282 H28F 1.00(2) . ?
C282 H28E 1.013(19) . ?
C282 H28D 1.00(2) . ?
C283 H28I 1.00(2) . ?
C283 H28H 0.996(17) . ?
C283 H28G 0.988(18) . ?
C29 H29 0.977(18) . ?
C31 C36 1.382(2) . ?
C31 C32 1.391(2) . ?
C32 C33 1.384(2) . ?
C33 C34 1.392(2) . ?
C33 C1 1.515(2) . ?
C34 C35 1.372(2) . ?
C34 H34 0.98(2) . ?
C35 C36 1.380(2) . ?
C35 H35 1.00(2) . ?
C36 H36 0.973(17) . ?
C41 C42 1.379(2) . ?
C41 C46 1.397(2) . ?
C42 C43 1.382(2) . ?
C42 H42 0.990(19) . ?
C43 C44 1.376(2) . ?
C43 H43 0.952(18) . ?
C44 C45 1.388(2) . ?
C44 H44 0.969(18) . ?
C45 C46 1.383(2) . ?
C45 C1 1.521(2) . ?
C1 C3 1.530(2) . ?
C1 C2 1.536(2) . ?
C2 H2C 0.96(2) . ?
C2 H2B 1.03(2) . ?
C2 H2A 1.04(2) . ?
C3 H3C 1.01(2) . ?
C3 H3B 0.98(2) . ?
C3 H3A 1.01(2) . ?

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
C11 O1 H1 107.2(14) . . ?
C12 O2 H2 108.6(14) . . ?
C21 O3 H3 106.3(14) . . ?
C22 O4 H4 104.8(12) . . ?
C46 O5 C32 118.28(11) . . ?
C19 N1 C31 119.38(13) . . ?
C29 N2 C41 121.22(13) . . ?
O1 C11 C16 121.12(13) . . ?
O1 C11 C12 117.67(13) . . ?
C16 C11 C12 121.21(13) . . ?
O2 C12 C11 115.23(13) . . ?
O2 C12 C13 123.46(13) . . ?
C11 C12 C13 121.30(14) . . ?
C12 C13 C14 118.77(13) . . ?
C12 C13 C19 117.30(13) . . ?
C14 C13 C19 123.85(13) . . ?
C15 C14 C13 117.25(14) . . ?
C15 C14 C18 119.42(14) . . ?
C13 C14 C18 123.31(13) . . ?
C14 C15 C16 124.93(15) . . ?
C14 C15 H15 119.1(9) . . ?
C16 C15 H15 116.0(9) . . ?
C11 C16 C15 116.43(14) . . ?
C11 C16 C17 122.18(14) . . ?
C15 C16 C17 121.39(14) . . ?
C173 C17 C172 107.82(14) . . ?
C173 C17 C16 112.37(13) . . ?
C172 C17 C16 109.66(13) . . ?
C173 C17 C171 108.22(15) . . ?
C172 C17 C171 109.44(15) . . ?
C16 C17 C171 109.28(13) . . ?
C17 C171 H17C 111.5(12) . . ?
C17 C171 H17B 110.6(13) . . ?
H17C C171 H17B 110.3(17) . . ?
C17 C171 H17A 108.3(11) . . ?
H17C C171 H17A 109.3(17) . . ?
H17B C171 H17A 106.7(16) . . ?
C17 C172 H17F 113.0(12) . . ?
C17 C172 H17E 111.8(11) . . ?
H17F C172 H17E 104.7(16) . . ?
C17 C172 H17D 109.2(12) . . ?
H17F C172 H17D 102.6(16) . . ?
H17E C172 H17D 115.2(16) . . ?
C17 C173 H17I 112.4(11) . . ?
C17 C173 H17H 112.4(11) . . ?
H17I C173 H17H 107.4(16) . . ?
C17 C173 H17G 110.2(12) . . ?
H17I C173 H17G 108.6(16) . . ?
H17H C173 H17G 105.4(16) . . ?
C182 C18 C183 112.07(16) . . ?
C182 C18 C181 106.50(17) . . ?
C183 C18 C181 105.83(17) . . ?
C182 C18 C14 110.99(15) . . ?
C183 C18 C14 109.76(14) . . ?
C181 C18 C14 111.55(14) . . ?
C18 C181 H18C 109.8(12) . . ?
C18 C181 H18B 112.8(12) . . ?
H18C C181 H18B 105.2(17) . . ?
C18 C181 H18A 111.9(12) . . ?
H18C C181 H18A 107.0(17) . . ?
H18B C181 H18A 109.7(18) . . ?
C18 C182 H18F 111.6(14) . . ?
C18 C182 H18E 117.5(12) . . ?
H18F C182 H18E 107.1(18) . . ?
C18 C182 H18D 112.1(14) . . ?
H18F C182 H18D 103.1(19) . . ?
H18E C182 H18D 104.2(18) . . ?
C18 C183 H18I 111.2(15) . . ?
C18 C183 H18H 115.6(12) . . ?
H18I C183 H18H 106.1(19) . . ?
C18 C183 H18G 109.4(12) . . ?
H18I C183 H18G 105.9(18) . . ?
H18H C183 H18G 108.2(17) . . ?
N1 C19 C13 122.23(14) . . ?
N1 C19 H19 119.9(9) . . ?
C13 C19 H19 117.8(9) . . ?
O3 C21 C26 121.48(14) . . ?
O3 C21 C22 117.79(13) . . ?
C26 C21 C22 120.73(14) . . ?
O4 C22 C21 114.65(13) . . ?
O4 C22 C23 123.51(13) . . ?
C21 C22 C23 121.83(13) . . ?
C22 C23 C24 118.37(13) . . ?
C22 C23 C29 117.23(13) . . ?
C24 C23 C29 124.31(13) . . ?
C25 C24 C23 117.19(14) . . ?
C25 C24 C28 119.45(13) . . ?
C23 C24 C28 123.34(13) . . ?
C24 C25 C26 125.27(14) . . ?
C24 C25 H25 117.7(10) . . ?
C26 C25 H25 117.1(10) . . ?
C21 C26 C25 116.60(14) . . ?
C21 C26 C27 121.32(13) . . ?
C25 C26 C27 122.08(14) . . ?
C273 C27 C271 108.38(16) . . ?
C273 C27 C26 110.21(14) . . ?
C271 C27 C26 111.74(13) . . ?
C273 C27 C272 109.73(15) . . ?
C271 C27 C272 107.45(14) . . ?
C26 C27 C272 109.28(13) . . ?
C27 C271 H27C 110.6(11) . . ?
C27 C271 H27B 106.2(12) . . ?
H27C C271 H27B 112.6(16) . . ?
C27 C271 H27A 111.3(12) . . ?
H27C C271 H27A 110.6(16) . . ?
H27B C271 H27A 105.5(16) . . ?
C27 C272 H27F 109.2(12) . . ?
C27 C272 H27E 113.4(11) . . ?
H27F C272 H27E 103.8(16) . . ?
C27 C272 H27D 108.9(11) . . ?
H27F C272 H27D 114.1(16) . . ?
H27E C272 H27D 107.5(15) . . ?
C27 C273 H27I 109.8(14) . . ?
C27 C273 H27H 111.7(12) . . ?
H27I C273 H27H 108.6(19) . . ?
C27 C273 H27G 112.6(12) . . ?
H27I C273 H27G 108.4(18) . . ?
H27H C273 H27G 105.7(17) . . ?
C283 C28 C282 105.84(13) . . ?
C283 C28 C24 111.98(12) . . ?
C282 C28 C24 112.07(12) . . ?
C283 C28 C281 105.21(13) . . ?
C282 C28 C281 111.28(13) . . ?
C24 C28 C281 110.19(12) . . ?
C28 C281 H28C 113.1(10) . . ?
C28 C281 H28B 108.3(10) . . ?
H28C C281 H28B 106.9(14) . . ?
C28 C281 H28A 109.3(10) . . ?
H28C C281 H28A 109.2(14) . . ?
H28B C281 H28A 109.9(13) . . ?
C28 C282 H28F 111.0(11) . . ?
C28 C282 H28E 112.8(10) . . ?
H28F C282 H28E 104.7(15) . . ?
C28 C282 H28D 110.4(11) . . ?
H28F C282 H28D 108.3(16) . . ?
H28E C282 H28D 109.5(15) . . ?
C28 C283 H28I 112.3(11) . . ?
C28 C283 H28H 114.3(10) . . ?
H28I C283 H28H 105.2(14) . . ?
C28 C283 H28G 108.1(10) . . ?
H28I C283 H28G 109.2(15) . . ?
H28H C283 H28G 107.5(14) . . ?
N2 C29 C23 121.53(14) . . ?
N2 C29 H29 120.0(10) . . ?
C23 C29 H29 118.4(10) . . ?
C36 C31 C32 118.71(14) . . ?
C36 C31 N1 121.90(14) . . ?
C32 C31 N1 119.15(13) . . ?
O5 C32 C33 123.23(13) . . ?
O5 C32 C31 114.50(12) . . ?
C33 C32 C31 122.27(14) . . ?
C32 C33 C34 117.01(14) . . ?
C32 C33 C1 121.43(13) . . ?
C34 C33 C1 121.44(13) . . ?
C35 C34 C33 121.77(15) . . ?
C35 C34 H34 118.5(12) . . ?
C33 C34 H34 119.7(12) . . ?
C34 C35 C36 119.97(16) . . ?
C34 C35 H35 120.6(10) . . ?
C36 C35 H35 119.3(11) . . ?
C35 C36 C31 120.16(15) . . ?
C35 C36 H36 121.2(10) . . ?
C31 C36 H36 118.6(10) . . ?
C42 C41 C46 118.95(13) . . ?
C42 C41 N2 124.60(14) . . ?
C46 C41 N2 116.44(13) . . ?
C41 C42 C43 119.94(15) . . ?
C41 C42 H42 120.9(10) . . ?
C43 C42 H42 119.1(10) . . ?
C44 C43 C42 119.91(15) . . ?
C44 C43 H43 119.3(10) . . ?
C42 C43 H43 120.8(10) . . ?
C43 C44 C45 121.88(15) . . ?
C43 C44 H44 118.3(11) . . ?
C45 C44 H44 119.7(11) . . ?
C46 C45 C44 117.10(14) . . ?
C46 C45 C1 121.52(13) . . ?
C44 C45 C1 121.38(13) . . ?
O5 C46 C45 123.20(13) . . ?
O5 C46 C41 114.85(12) . . ?
C45 C46 C41 121.92(13) . . ?
C33 C1 C45 110.22(12) . . ?
C33 C1 C3 110.45(14) . . ?
C45 C1 C3 109.62(13) . . ?
C33 C1 C2 108.66(13) . . ?
C45 C1 C2 108.39(14) . . ?
C3 C1 C2 109.46(15) . . ?
C1 C2 H2C 111.6(12) . . ?
C1 C2 H2B 107.9(12) . . ?
H2C C2 H2B 108.4(17) . . ?
C1 C2 H2A 110.6(11) . . ?
H2C C2 H2A 107.4(16) . . ?
H2B C2 H2A 111.1(16) . . ?
C1 C3 H3C 109.0(13) . . ?
C1 C3 H3B 111.8(12) . . ?
H3C C3 H3B 106.7(17) . . ?
C1 C3 H3A 110.0(12) . . ?
H3C C3 H3A 113.0(18) . . ?
H3B C3 H3A 106.4(17) . . ?

_refine_diff_density_max         0.310
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_sina
_database_code_depnum_ccdc_archive 'CCDC 1922354'
loop_
_audit_author_name
_audit_author_address
'Allen G. Oliver'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT390_sina                
;
PROBLEM: Deviating Methyl C182....X-C-H Bond Angle....119 Degree
RESPONSE: Hydrogens were found on the difference map and refined
isotropically. Deviations are due to small disorder around the 
tertbutyls that was not modeled.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'(Tetrahydrofuran)sodium(9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dioxybenzaldimine)(phenyl)silicate) bis(tetrahydrofuran) solvate'
_chemical_name_common            '(THF)Na[(Xbic)SiPh] . 2 THF'
_chemical_melting_point          .
_chemical_formula_moiety         'C55 H65 N2 Na O6 Si, 2(C4 H8 O)'
_chemical_formula_sum            'C63 H81 N2 Na O8 Si'
_chemical_formula_weight         1045.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.104(2)
_cell_length_b                   19.806(3)
_cell_length_c                   17.777(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.068(2)
_cell_angle_gamma                90
_cell_volume                     5656.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9971
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.72

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   0.696000
_exptl_transmission_factor_max   0.795700
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.196
_exptl_absorpt_coefficient_mu    0.106
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_recrystallization_method 
'Crystals were deposited by diffusion of acetonitrile into a solution of the compound in THF.'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            129520
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.268
_diffrn_reflns_theta_max         28.452
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14183
_reflns_number_gt                10326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
 All hydrogens except for the ones on THF solvate were found
on the difference map and refined isotropically. 
 Hydrogens on THF solvates were placed in calculated positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0721P)²+5.5303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14183
_refine_ls_number_parameters     936
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.1616
_refine_ls_wR_factor_gt          0.1440
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.32241(3) 0.63576(3) 0.41379(3) 0.01589(12) Uani 1 1 d . . . . .
Na Na 0.14822(5) 0.56245(4) 0.35534(5) 0.02042(18) Uani 1 1 d . . . . .
O1 O 0.33102(8) 0.72352(7) 0.42195(8) 0.0192(3) Uani 1 1 d . . . . .
O2 O 0.21519(8) 0.64619(7) 0.41932(8) 0.0172(3) Uani 1 1 d . . . . .
O3 O 0.39258(8) 0.63982(7) 0.34562(8) 0.0185(3) Uani 1 1 d . . . . .
O4 O 0.29152(8) 0.55534(7) 0.37516(8) 0.0182(3) Uani 1 1 d . . . . .
O5 O 0.02808(8) 0.49441(7) 0.34906(8) 0.0181(3) Uani 1 1 d . . . . .
N1 N 0.04482(10) 0.61830(9) 0.41874(9) 0.0175(3) Uani 1 1 d . . . . .
N2 N 0.18340(10) 0.45197(8) 0.32111(9) 0.0178(3) Uani 1 1 d . . . . .
C11 C 0.25693(12) 0.75572(10) 0.42363(10) 0.0163(4) Uani 1 1 d . . . . .
C12 C 0.18963(12) 0.71115(10) 0.42294(10) 0.0161(4) Uani 1 1 d . . . . .
C13 C 0.10639(12) 0.73188(10) 0.42323(11) 0.0170(4) Uani 1 1 d . . . . .
C14 C 0.09212(12) 0.80370(10) 0.42300(11) 0.0178(4) Uani 1 1 d . . . . .
C15 C 0.16073(13) 0.84599(10) 0.42221(11) 0.0181(4) Uani 1 1 d . . . . .
H15 H 0.1503(14) 0.8936(12) 0.4232(12) 0.014(5) Uiso 1 1 d . . . . .
C16 C 0.24463(12) 0.82472(10) 0.42220(10) 0.0171(4) Uani 1 1 d . . . . .
C17 C 0.31703(13) 0.87400(10) 0.41723(11) 0.0193(4) Uani 1 1 d . . . . .
C171 C 0.37992(14) 0.86446(13) 0.48596(12) 0.0243(4) Uani 1 1 d . . . . .
H17C H 0.3533(16) 0.8738(13) 0.5327(15) 0.030(7) Uiso 1 1 d . . . . .
H17B H 0.4277(16) 0.8961(13) 0.4830(14) 0.023(6) Uiso 1 1 d . . . . .
H17A H 0.4006(16) 0.8217(14) 0.4879(15) 0.028(7) Uiso 1 1 d . . . . .
C172 C 0.35962(15) 0.85957(13) 0.34398(12) 0.0253(5) Uani 1 1 d . . . . .
H17F H 0.3199(17) 0.8620(13) 0.3014(16) 0.030(7) Uiso 1 1 d . . . . .
H17E H 0.3998(17) 0.8927(14) 0.3370(15) 0.029(7) Uiso 1 1 d . . . . .
H17D H 0.3818(17) 0.8150(14) 0.3434(15) 0.030(7) Uiso 1 1 d . . . . .
C173 C 0.28919(15) 0.94756(12) 0.41578(14) 0.0267(5) Uani 1 1 d . . . . .
H17I H 0.2630(17) 0.9616(14) 0.4594(16) 0.033(7) Uiso 1 1 d . . . . .
H17H H 0.2511(19) 0.9575(14) 0.3720(17) 0.039(8) Uiso 1 1 d . . . . .
H17G H 0.3366(16) 0.9762(13) 0.4122(14) 0.026(6) Uiso 1 1 d . . . . .
C18 C 0.00433(13) 0.83568(11) 0.42011(12) 0.0210(4) Uani 1 1 d . . . . .
C181 C 0.00690(16) 0.91307(12) 0.41559(16) 0.0319(5) Uani 1 1 d . . . . .
H18C H 0.0336(18) 0.9298(14) 0.3715(17) 0.036(7) Uiso 1 1 d . . . . .
H18B H -0.0485(18) 0.9293(14) 0.4128(15) 0.034(7) Uiso 1 1 d . . . . .
H18A H 0.0383(19) 0.9344(15) 0.4590(17) 0.041(8) Uiso 1 1 d . . . . .
C182 C -0.04715(15) 0.81255(14) 0.34808(14) 0.0300(5) Uani 1 1 d . . . . .
H18F H -0.0167(19) 0.8264(15) 0.3032(17) 0.042(8) Uiso 1 1 d . . . . .
H18E H -0.1012(19) 0.8338(15) 0.3445(17) 0.043(8) Uiso 1 1 d . . . . .
H18D H -0.060(2) 0.7657(19) 0.342(2) 0.061(10) Uiso 1 1 d . . . . .
C183 C -0.04051(15) 0.82020(13) 0.49167(14) 0.0278(5) Uani 1 1 d . . . . .
H18I H -0.0106(17) 0.8395(14) 0.5357(16) 0.032(7) Uiso 1 1 d . . . . .
H18H H -0.0960(18) 0.8441(14) 0.4886(15) 0.034(7) Uiso 1 1 d . . . . .
H18G H -0.0460(16) 0.7734(14) 0.5026(15) 0.028(7) Uiso 1 1 d . . . . .
C19 C 0.03851(12) 0.68238(11) 0.42507(11) 0.0187(4) Uani 1 1 d . . . . .
H19 H -0.0133(16) 0.6995(13) 0.4328(14) 0.026(6) Uiso 1 1 d . . . . .
C21 C 0.39101(12) 0.58605(10) 0.29771(11) 0.0175(4) Uani 1 1 d . . . . .
C22 C 0.33101(12) 0.53807(10) 0.31378(11) 0.0175(4) Uani 1 1 d . . . . .
C23 C 0.31411(12) 0.48091(10) 0.26899(11) 0.0180(4) Uani 1 1 d . . . . .
C24 C 0.36343(12) 0.47198(10) 0.20557(11) 0.0179(4) Uani 1 1 d . . . . .
C25 C 0.42328(12) 0.52055(11) 0.19275(11) 0.0190(4) Uani 1 1 d . . . . .
H25 H 0.4545(16) 0.5132(12) 0.1499(14) 0.024(6) Uiso 1 1 d . . . . .
C26 C 0.43938(12) 0.57859(10) 0.23676(11) 0.0188(4) Uani 1 1 d . . . . .
C27 C 0.50415(13) 0.63158(11) 0.21837(12) 0.0221(4) Uani 1 1 d . . . . .
H27F H 0.4218(18) 0.6971(14) 0.1579(16) 0.034(7) Uiso 1 1 d . . . . .
C271 C 0.55144(15) 0.61187(14) 0.14983(14) 0.0292(5) Uani 1 1 d . . . . .
H27C H 0.5161(17) 0.6039(13) 0.1062(16) 0.031(7) Uiso 1 1 d . . . . .
H27B H 0.5813(17) 0.5708(14) 0.1577(15) 0.028(7) Uiso 1 1 d . . . . .
H27A H 0.5914(17) 0.6475(14) 0.1415(15) 0.031(7) Uiso 1 1 d . . . . .
C272 C 0.46049(17) 0.69912(13) 0.20089(15) 0.0314(5) Uani 1 1 d . . . . .
H27E H 0.4986(18) 0.7331(15) 0.1899(16) 0.037(7) Uiso 1 1 d . . . . .
H27D H 0.4314(18) 0.7149(15) 0.2429(17) 0.041(8) Uiso 1 1 d . . . . .
C273 C 0.56799(15) 0.64055(14) 0.28613(13) 0.0294(5) Uani 1 1 d . . . . .
H27I H 0.6062(19) 0.6752(15) 0.2742(17) 0.041(8) Uiso 1 1 d . . . . .
H27H H 0.5958(17) 0.5990(14) 0.2966(15) 0.029(7) Uiso 1 1 d . . . . .
H27G H 0.5400(17) 0.6550(14) 0.3296(16) 0.032(7) Uiso 1 1 d . . . . .
C28 C 0.35100(13) 0.41180(11) 0.15051(12) 0.0224(4) Uani 1 1 d . . . . .
H28I H 0.3433(19) 0.3314(16) 0.2340(18) 0.047(8) Uiso 1 1 d . . . . .
C281 C 0.26050(15) 0.40806(14) 0.11576(15) 0.0300(5) Uani 1 1 d . . . . .
H28C H 0.2541(18) 0.3696(15) 0.0826(17) 0.042(8) Uiso 1 1 d . . . . .
H28B H 0.2459(19) 0.4480(16) 0.0849(18) 0.046(9) Uiso 1 1 d . . . . .
H28A H 0.2216(18) 0.4035(14) 0.1528(17) 0.039(8) Uiso 1 1 d . . . . .
C282 C 0.40442(15) 0.41886(14) 0.08251(14) 0.0298(5) Uani 1 1 d . . . . .
H28F H 0.3934(18) 0.3815(15) 0.0485(17) 0.041(8) Uiso 1 1 d . . . . .
H28E H 0.3908(18) 0.4606(15) 0.0542(16) 0.037(8) Uiso 1 1 d . . . . .
H28D H 0.4623(17) 0.4211(13) 0.0983(14) 0.025(6) Uiso 1 1 d . . . . .
C283 C 0.37807(18) 0.34553(13) 0.18979(16) 0.0335(5) Uani 1 1 d . . . . .
H28H H 0.435(2) 0.3467(16) 0.2077(18) 0.047(9) Uiso 1 1 d . . . . .
H28G H 0.3705(19) 0.3075(16) 0.1569(18) 0.048(9) Uiso 1 1 d . . . . .
C29 C 0.24726(13) 0.43448(11) 0.28616(11) 0.0197(4) Uani 1 1 d . . . . .
H29 H 0.2522(14) 0.3894(12) 0.2699(12) 0.014(5) Uiso 1 1 d . . . . .
C31 C -0.02747(12) 0.57871(10) 0.42849(11) 0.0184(4) Uani 1 1 d . . . . .
C32 C -0.03525(12) 0.51510(10) 0.39376(11) 0.0173(4) Uani 1 1 d . . . . .
C33 C -0.10474(12) 0.47386(11) 0.40020(11) 0.0190(4) Uani 1 1 d . . . . .
C34 C -0.16580(13) 0.49512(12) 0.44648(12) 0.0233(4) Uani 1 1 d . . . . .
H34 H -0.2133(15) 0.4667(12) 0.4541(13) 0.019(6) Uiso 1 1 d . . . . .
C35 C -0.15797(13) 0.55652(12) 0.48349(12) 0.0244(4) Uani 1 1 d . . . . .
H35 H -0.1974(17) 0.5679(14) 0.5166(16) 0.034(7) Uiso 1 1 d . . . . .
C36 C -0.09010(13) 0.59797(11) 0.47472(12) 0.0211(4) Uani 1 1 d . . . . .
H36 H -0.0847(14) 0.6390(12) 0.4979(13) 0.015(5) Uiso 1 1 d . . . . .
C41 C 0.12211(12) 0.40254(10) 0.33360(11) 0.0180(4) Uani 1 1 d . . . . .
C42 C 0.13790(14) 0.33341(11) 0.33861(11) 0.0214(4) Uani 1 1 d . . . . .
H42 H 0.1933(16) 0.3158(13) 0.3362(14) 0.025(6) Uiso 1 1 d . . . . .
C43 C 0.07452(14) 0.28845(11) 0.35154(12) 0.0240(4) Uani 1 1 d . . . . .
H43 H 0.0868(16) 0.2405(13) 0.3544(14) 0.027(7) Uiso 1 1 d . . . . .
C44 C -0.00606(14) 0.31152(11) 0.35702(12) 0.0237(4) Uani 1 1 d . . . . .
H44 H -0.0483(17) 0.2788(14) 0.3628(15) 0.032(7) Uiso 1 1 d . . . . .
C45 C -0.02434(13) 0.38020(11) 0.35292(11) 0.0200(4) Uani 1 1 d . . . . .
C46 C 0.04145(12) 0.42498(10) 0.34525(11) 0.0179(4) Uani 1 1 d . . . . .
C51 C 0.37137(12) 0.60728(10) 0.50670(11) 0.0188(4) Uani 1 1 d . . . . .
C52 C 0.39837(15) 0.54051(12) 0.51800(13) 0.0273(5) Uani 1 1 d . . . . .
H52 H 0.3935(16) 0.5078(14) 0.4754(15) 0.030(7) Uiso 1 1 d . . . . .
C53 C 0.43388(17) 0.51859(13) 0.58734(14) 0.0344(6) Uani 1 1 d . . . . .
H53 H 0.4563(18) 0.4731(15) 0.5920(16) 0.040(8) Uiso 1 1 d . . . . .
C54 C 0.44155(16) 0.56287(13) 0.64770(13) 0.0331(5) Uani 1 1 d . . . . .
H54 H 0.4672(17) 0.5486(14) 0.6968(16) 0.034(7) Uiso 1 1 d . . . . .
C55 C 0.41519(15) 0.62874(13) 0.63848(13) 0.0290(5) Uani 1 1 d . . . . .
H55 H 0.4210(17) 0.6608(15) 0.6773(17) 0.038(8) Uiso 1 1 d . . . . .
C56 C 0.38181(13) 0.65115(12) 0.56854(12) 0.0236(4) Uani 1 1 d . . . . .
H56 H 0.3646(14) 0.6984(12) 0.5624(12) 0.014(5) Uiso 1 1 d . . . . .
C1 C -0.11151(13) 0.40951(11) 0.35317(11) 0.0202(4) Uani 1 1 d . . . . .
C2 C -0.17371(15) 0.35943(12) 0.38244(14) 0.0276(5) Uani 1 1 d . . . . .
H2C H -0.1565(17) 0.3448(14) 0.4344(16) 0.033(7) Uiso 1 1 d . . . . .
H2B H -0.2305(18) 0.3802(14) 0.3756(15) 0.036(7) Uiso 1 1 d . . . . .
H2A H -0.1782(16) 0.3192(14) 0.3484(15) 0.030(7) Uiso 1 1 d . . . . .
C3 C -0.14128(15) 0.42900(13) 0.27180(13) 0.0266(5) Uani 1 1 d . . . . .
H3C H -0.1428(17) 0.3894(14) 0.2401(16) 0.034(7) Uiso 1 1 d . . . . .
H3B H -0.1976(18) 0.4511(14) 0.2732(15) 0.036(7) Uiso 1 1 d . . . . .
H3 H -0.1054(17) 0.4641(14) 0.2506(15) 0.035(7) Uiso 1 1 d . . . . .
O6 O 0.14519(11) 0.61564(9) 0.23911(9) 0.0326(4) Uani 1 1 d . . . . .
C61 C 0.18836(19) 0.67623(14) 0.22091(14) 0.0345(5) Uani 1 1 d . . . . .
H61B H 0.242(2) 0.6780(15) 0.2504(17) 0.045(8) Uiso 1 1 d . . . . .
H61A H 0.156(2) 0.7127(16) 0.2362(18) 0.048(9) Uiso 1 1 d . . . . .
C62 C 0.20146(19) 0.67288(14) 0.13719(15) 0.0363(6) Uani 1 1 d . . . . .
H62B H 0.255(2) 0.6946(16) 0.1286(18) 0.053(9) Uiso 1 1 d . . . . .
H62A H 0.151(2) 0.6944(16) 0.1066(18) 0.048(9) Uiso 1 1 d . . . . .
C63 C 0.19870(19) 0.59771(14) 0.12190(15) 0.0372(6) Uani 1 1 d . . . . .
H63B H 0.2501(19) 0.5775(15) 0.1398(17) 0.041(8) Uiso 1 1 d . . . . .
H63A H 0.182(2) 0.5866(17) 0.066(2) 0.060(10) Uiso 1 1 d . . . . .
C64 C 0.13327(17) 0.57466(14) 0.17238(14) 0.0343(5) Uani 1 1 d . . . . .
H64B H 0.076(2) 0.5847(16) 0.1528(18) 0.048(9) Uiso 1 1 d . . . . .
H64A H 0.1410(18) 0.5274(16) 0.1878(17) 0.041(8) Uiso 1 1 d . . . . .
O7 O 0.08096(14) 0.37702(11) 0.84197(12) 0.0505(5) Uani 1 1 d . . . . .
C71 C 0.07074(19) 0.37360(16) 0.76213(16) 0.0455(7) Uani 1 1 d . . . . .
H71A H 0.0469 0.4163 0.7411 0.055 Uiso 1 1 calc R U . . .
H71B H 0.0332 0.3359 0.7460 0.055 Uiso 1 1 calc R U . . .
C72 C 0.1577(2) 0.3620(2) 0.7357(2) 0.0586(9) Uani 1 1 d . . . . .
H72A H 0.1674 0.3135 0.7260 0.070 Uiso 1 1 calc R U . . .
H72B H 0.1659 0.3878 0.6891 0.070 Uiso 1 1 calc R U . . .
C73 C 0.2142(2) 0.3870(2) 0.8003(2) 0.0684(10) Uani 1 1 d . . . . .
H73A H 0.2474 0.4260 0.7847 0.082 Uiso 1 1 calc R U . . .
H73B H 0.2525 0.3509 0.8195 0.082 Uiso 1 1 calc R U . . .
C74 C 0.1568(3) 0.4076(2) 0.8594(2) 0.0723(12) Uani 1 1 d . . . . .
H74A H 0.1798 0.3931 0.9099 0.087 Uiso 1 1 calc R U . . .
H74B H 0.1502 0.4573 0.8597 0.087 Uiso 1 1 calc R U . . .
O8 O 0.32410(16) 0.27593(16) 0.39526(16) 0.0731(7) Uani 1 1 d . . . . .
C81 C 0.3853(3) 0.3214(4) 0.4142(3) 0.108(2) Uani 1 1 d . . . . .
H81A H 0.3747 0.3625 0.3832 0.130 Uiso 1 1 calc R U . . .
H81B H 0.4389 0.3021 0.4005 0.130 Uiso 1 1 calc R U . . .
C82 C 0.3938(4) 0.3402(4) 0.4883(3) 0.130(3) Uani 1 1 d . . . . .
H82A H 0.3815 0.3889 0.4937 0.155 Uiso 1 1 calc R U . . .
H82B H 0.4511 0.3313 0.5099 0.155 Uiso 1 1 calc R U . . .
C83 C 0.3345(5) 0.2998(4) 0.5256(3) 0.141(3) Uani 1 1 d . . . . .
H83A H 0.2926 0.3288 0.5478 0.169 Uiso 1 1 calc R U . . .
H83B H 0.3629 0.2723 0.5663 0.169 Uiso 1 1 calc R U . . .
C84 C 0.2939(3) 0.2549(3) 0.4645(3) 0.108(2) Uani 1 1 d . . . . .
H84A H 0.3084 0.2070 0.4746 0.130 Uiso 1 1 calc R U . . .
H84B H 0.2325 0.2596 0.4627 0.130 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
Si O3 1.7164(14) . ?
Si O2 1.7487(15) . ?
Si O1 1.7488(15) . ?
Si O4 1.7910(15) . ?
Si C51 1.866(2) . ?
Na O2 2.2437(16) . ?
Na O4 2.3140(16) . ?
Na O6 2.3167(18) . ?
Na N2 2.3511(19) . ?
Na N1 2.3522(18) . ?
Na O5 2.3539(16) . ?
O1 C11 1.355(2) . ?
O2 C12 1.354(2) . ?
O3 C21 1.363(2) . ?
O4 C22 1.346(2) . ?
O5 C46 1.394(2) . ?
O5 C32 1.398(2) . ?
N1 C19 1.279(3) . ?
N1 C31 1.424(2) . ?
N2 C29 1.286(3) . ?
N2 C41 1.419(2) . ?
C11 C16 1.381(3) . ?
C11 C12 1.397(3) . ?
C12 C13 1.402(3) . ?
C13 C14 1.441(3) . ?
C13 C19 1.470(3) . ?
C14 C15 1.387(3) . ?
C14 C18 1.547(3) . ?
C15 C16 1.415(3) . ?
C15 H15 0.96(2) . ?
C16 C17 1.528(3) . ?
C17 C173 1.524(3) . ?
C17 C172 1.541(3) . ?
C17 C171 1.542(3) . ?
C171 H17C 0.98(3) . ?
C171 H17B 1.00(3) . ?
C171 H17A 0.91(3) . ?
C172 H17F 0.96(3) . ?
C172 H17E 0.94(3) . ?
C172 H17D 0.95(3) . ?
C173 H17I 0.95(3) . ?
C173 H17H 0.98(3) . ?
C173 H17G 0.96(3) . ?
C18 C181 1.536(3) . ?
C18 C183 1.538(3) . ?
C18 C182 1.545(3) . ?
C181 H18C 0.98(3) . ?
C181 H18B 0.95(3) . ?
C181 H18A 0.99(3) . ?
C182 H18F 1.00(3) . ?
C182 H18E 0.96(3) . ?
C182 H18D 0.95(4) . ?
C183 H18I 0.97(3) . ?
C183 H18H 1.01(3) . ?
C183 H18G 0.95(3) . ?
C19 H19 0.92(3) . ?
C21 C26 1.386(3) . ?
C21 C22 1.399(3) . ?
C22 C23 1.400(3) . ?
C23 C24 1.435(3) . ?
C23 C29 1.464(3) . ?
C24 C25 1.392(3) . ?
C24 C28 1.546(3) . ?
C25 C26 1.404(3) . ?
C25 H25 0.95(3) . ?
C26 C27 1.531(3) . ?
C27 C272 1.533(3) . ?
C27 C271 1.533(3) . ?
C27 C273 1.537(3) . ?
C271 H27C 0.94(3) . ?
C271 H27B 0.95(3) . ?
C271 H27A 0.97(3) . ?
C272 H27F 0.95(3) . ?
C272 H27E 0.94(3) . ?
C272 H27D 0.96(3) . ?
C273 H27I 0.96(3) . ?
C273 H27H 0.95(3) . ?
C273 H27G 0.97(3) . ?
C28 C283 1.535(3) . ?
C28 C282 1.539(3) . ?
C28 C281 1.544(3) . ?
C281 H28C 0.96(3) . ?
C281 H28B 0.98(3) . ?
C281 H28A 0.95(3) . ?
C282 H28F 0.96(3) . ?
C282 H28E 0.99(3) . ?
C282 H28D 0.95(3) . ?
C283 H28I 1.04(3) . ?
C283 H28H 0.95(3) . ?
C283 H28G 0.96(3) . ?
C29 H29 0.94(2) . ?
C31 C36 1.399(3) . ?
C31 C32 1.405(3) . ?
C32 C33 1.397(3) . ?
C33 C34 1.391(3) . ?
C33 C1 1.524(3) . ?
C34 C35 1.384(3) . ?
C34 H34 0.97(2) . ?
C35 C36 1.385(3) . ?
C35 H35 0.92(3) . ?
C36 H36 0.91(2) . ?
C41 C42 1.394(3) . ?
C41 C46 1.402(3) . ?
C42 C43 1.386(3) . ?
C42 H42 0.96(3) . ?
C43 C44 1.386(3) . ?
C43 H43 0.97(3) . ?
C44 C45 1.393(3) . ?
C44 H44 0.95(3) . ?
C45 C46 1.396(3) . ?
C45 C1 1.519(3) . ?
C51 C56 1.402(3) . ?
C51 C52 1.402(3) . ?
C52 C53 1.391(3) . ?
C52 H52 1.00(3) . ?
C53 C54 1.385(4) . ?
C53 H53 0.97(3) . ?
C54 C55 1.378(4) . ?
C54 H54 0.98(3) . ?
C55 C56 1.392(3) . ?
C55 H55 0.94(3) . ?
C56 H56 0.98(2) . ?
C1 C2 1.527(3) . ?
C1 C3 1.541(3) . ?
C2 H2C 0.99(3) . ?
C2 H2B 1.00(3) . ?
C2 H2A 1.00(3) . ?
C3 H3C 0.97(3) . ?
C3 H3B 1.01(3) . ?
C3 H3 1.00(3) . ?
O6 C61 1.435(3) . ?
O6 C64 1.439(3) . ?
C61 C62 1.519(3) . ?
C61 H61B 0.98(3) . ?
C61 H61A 0.94(3) . ?
C62 C63 1.514(4) . ?
C62 H62B 0.98(3) . ?
C62 H62A 1.04(3) . ?
C63 C64 1.503(4) . ?
C63 H63B 0.95(3) . ?
C63 H63A 1.03(4) . ?
C64 H64B 0.98(3) . ?
C64 H64A 0.98(3) . ?
O7 C74 1.378(4) . ?
O7 C71 1.419(3) . ?
C71 C72 1.526(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.498(5) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.504(6) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
O8 C81 1.360(5) . ?
O8 C84 1.418(6) . ?
C81 C82 1.367(7) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 C83 1.442(8) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.517(8) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Si O2 137.42(7) . . ?
O3 Si O1 87.69(7) . . ?
O2 Si O1 87.18(7) . . ?
O3 Si O4 87.12(7) . . ?
O2 Si O4 83.00(7) . . ?
O1 Si O4 159.06(7) . . ?
O3 Si C51 112.40(8) . . ?
O2 Si C51 110.04(8) . . ?
O1 Si C51 101.59(8) . . ?
O4 Si C51 99.14(8) . . ?
O2 Na O4 61.93(5) . . ?
O2 Na O6 95.45(6) . . ?
O4 Na O6 96.96(6) . . ?
O2 Na N2 134.69(7) . . ?
O4 Na N2 74.14(6) . . ?
O6 Na N2 100.52(7) . . ?
O2 Na N1 74.96(6) . . ?
O4 Na N1 133.46(6) . . ?
O6 Na N1 104.04(7) . . ?
N2 Na N1 138.89(7) . . ?
O2 Na O5 144.21(6) . . ?
O4 Na O5 141.25(6) . . ?
O6 Na O5 104.64(6) . . ?
N2 Na O5 70.57(6) . . ?
N1 Na O5 71.61(6) . . ?
C11 O1 Si 113.88(12) . . ?
C12 O2 Si 114.82(12) . . ?
C12 O2 Na 126.15(12) . . ?
Si O2 Na 108.98(7) . . ?
C21 O3 Si 114.89(12) . . ?
C22 O4 Si 113.74(12) . . ?
C22 O4 Na 114.56(12) . . ?
Si O4 Na 104.55(7) . . ?
C46 O5 C32 115.98(15) . . ?
C46 O5 Na 115.95(11) . . ?
C32 O5 Na 115.82(11) . . ?
C19 N1 C31 117.70(17) . . ?
C19 N1 Na 124.91(13) . . ?
C31 N1 Na 114.32(13) . . ?
C29 N2 C41 118.60(17) . . ?
C29 N2 Na 126.25(14) . . ?
C41 N2 Na 114.75(12) . . ?
O1 C11 C16 126.21(18) . . ?
O1 C11 C12 112.72(17) . . ?
C16 C11 C12 120.99(18) . . ?
O2 C12 C11 111.25(17) . . ?
O2 C12 C13 124.91(17) . . ?
C11 C12 C13 123.80(18) . . ?
C12 C13 C14 116.18(17) . . ?
C12 C13 C19 121.15(18) . . ?
C14 C13 C19 122.66(17) . . ?
C15 C14 C13 117.98(18) . . ?
C15 C14 C18 118.63(18) . . ?
C13 C14 C18 123.34(17) . . ?
C14 C15 C16 125.54(19) . . ?
C14 C15 H15 116.9(14) . . ?
C16 C15 H15 117.5(14) . . ?
C11 C16 C15 115.48(18) . . ?
C11 C16 C17 121.62(18) . . ?
C15 C16 C17 122.84(18) . . ?
C173 C17 C16 112.76(17) . . ?
C173 C17 C172 108.11(18) . . ?
C16 C17 C172 108.52(17) . . ?
C173 C17 C171 107.84(18) . . ?
C16 C17 C171 109.70(16) . . ?
C172 C17 C171 109.88(18) . . ?
C17 C171 H17C 110.3(16) . . ?
C17 C171 H17B 110.3(14) . . ?
H17C C171 H17B 108(2) . . ?
C17 C171 H17A 111.3(17) . . ?
H17C C171 H17A 109(2) . . ?
H17B C171 H17A 108(2) . . ?
C17 C172 H17F 110.3(16) . . ?
C17 C172 H17E 109.6(16) . . ?
H17F C172 H17E 107(2) . . ?
C17 C172 H17D 111.7(16) . . ?
H17F C172 H17D 106(2) . . ?
H17E C172 H17D 113(2) . . ?
C17 C173 H17I 114.4(16) . . ?
C17 C173 H17H 111.9(17) . . ?
H17I C173 H17H 107(2) . . ?
C17 C173 H17G 109.4(15) . . ?
H17I C173 H17G 106(2) . . ?
H17H C173 H17G 107(2) . . ?
C181 C18 C183 104.98(19) . . ?
C181 C18 C182 105.5(2) . . ?
C183 C18 C182 111.76(19) . . ?
C181 C18 C14 112.49(18) . . ?
C183 C18 C14 111.89(17) . . ?
C182 C18 C14 109.97(17) . . ?
C18 C181 H18C 113.3(17) . . ?
C18 C181 H18B 108.2(17) . . ?
H18C C181 H18B 108(2) . . ?
C18 C181 H18A 113.6(17) . . ?
H18C C181 H18A 105(2) . . ?
H18B C181 H18A 109(2) . . ?
C18 C182 H18F 108.3(17) . . ?
C18 C182 H18E 110.7(18) . . ?
H18F C182 H18E 108(2) . . ?
C18 C182 H18D 119(2) . . ?
H18F C182 H18D 107(3) . . ?
H18E C182 H18D 104(3) . . ?
C18 C183 H18I 110.8(16) . . ?
C18 C183 H18H 109.2(16) . . ?
H18I C183 H18H 104(2) . . ?
C18 C183 H18G 114.8(16) . . ?
H18I C183 H18G 106(2) . . ?
H18H C183 H18G 112(2) . . ?
N1 C19 C13 126.57(18) . . ?
N1 C19 H19 117.3(16) . . ?
C13 C19 H19 116.1(16) . . ?
O3 C21 C26 125.83(18) . . ?
O3 C21 C22 112.68(17) . . ?
C26 C21 C22 121.43(18) . . ?
O4 C22 C21 111.46(17) . . ?
O4 C22 C23 125.65(18) . . ?
C21 C22 C23 122.86(18) . . ?
C22 C23 C24 116.77(18) . . ?
C22 C23 C29 120.37(17) . . ?
C24 C23 C29 122.84(18) . . ?
C25 C24 C23 118.14(18) . . ?
C25 C24 C28 119.29(17) . . ?
C23 C24 C28 122.56(18) . . ?
C24 C25 C26 125.25(18) . . ?
C24 C25 H25 115.8(15) . . ?
C26 C25 H25 118.9(15) . . ?
C21 C26 C25 115.53(18) . . ?
C21 C26 C27 121.50(18) . . ?
C25 C26 C27 122.95(18) . . ?
C26 C27 C272 109.38(18) . . ?
C26 C27 C271 112.30(18) . . ?
C272 C27 C271 107.93(19) . . ?
C26 C27 C273 109.87(18) . . ?
C272 C27 C273 109.2(2) . . ?
C271 C27 C273 108.05(18) . . ?
C27 C271 H27C 113.1(16) . . ?
C27 C271 H27B 112.1(16) . . ?
H27C C271 H27B 104(2) . . ?
C27 C271 H27A 107.9(16) . . ?
H27C C271 H27A 111(2) . . ?
H27B C271 H27A 108(2) . . ?
C27 C272 H27F 113.0(17) . . ?
C27 C272 H27E 111.7(18) . . ?
H27F C272 H27E 105(2) . . ?
C27 C272 H27D 111.7(18) . . ?
H27F C272 H27D 108(2) . . ?
H27E C272 H27D 107(2) . . ?
C27 C273 H27I 108.3(18) . . ?
C27 C273 H27H 109.5(16) . . ?
H27I C273 H27H 111(2) . . ?
C27 C273 H27G 109.7(16) . . ?
H27I C273 H27G 108(2) . . ?
H27H C273 H27G 110(2) . . ?
C283 C28 C282 106.18(19) . . ?
C283 C28 C281 111.7(2) . . ?
C282 C28 C281 104.75(19) . . ?
C283 C28 C24 110.57(19) . . ?
C282 C28 C24 111.88(18) . . ?
C281 C28 C24 111.49(17) . . ?
C28 C281 H28C 109.8(18) . . ?
C28 C281 H28B 111.5(18) . . ?
H28C C281 H28B 106(2) . . ?
C28 C281 H28A 112.3(18) . . ?
H28C C281 H28A 108(2) . . ?
H28B C281 H28A 109(2) . . ?
C28 C282 H28F 109.6(17) . . ?
C28 C282 H28E 111.2(17) . . ?
H28F C282 H28E 107(2) . . ?
C28 C282 H28D 111.2(15) . . ?
H28F C282 H28D 111(2) . . ?
H28E C282 H28D 107(2) . . ?
C28 C283 H28I 115.2(17) . . ?
C28 C283 H28H 111.5(19) . . ?
H28I C283 H28H 108(3) . . ?
C28 C283 H28G 112.0(19) . . ?
H28I C283 H28G 102(2) . . ?
H28H C283 H28G 108(3) . . ?
N2 C29 C23 123.80(19) . . ?
N2 C29 H29 119.4(14) . . ?
C23 C29 H29 116.8(14) . . ?
C36 C31 C32 117.22(18) . . ?
C36 C31 N1 123.44(18) . . ?
C32 C31 N1 119.24(17) . . ?
C33 C32 O5 119.75(18) . . ?
C33 C32 C31 122.38(18) . . ?
O5 C32 C31 117.82(17) . . ?
C34 C33 C32 118.39(19) . . ?
C34 C33 C1 123.46(18) . . ?
C32 C33 C1 118.08(17) . . ?
C35 C34 C33 120.17(19) . . ?
C35 C34 H34 119.4(14) . . ?
C33 C34 H34 120.4(14) . . ?
C34 C35 C36 120.89(19) . . ?
C34 C35 H35 118.3(17) . . ?
C36 C35 H35 120.7(17) . . ?
C35 C36 C31 120.8(2) . . ?
C35 C36 H36 121.8(14) . . ?
C31 C36 H36 117.3(14) . . ?
C42 C41 C46 117.94(18) . . ?
C42 C41 N2 124.18(18) . . ?
C46 C41 N2 117.81(18) . . ?
C43 C42 C41 120.6(2) . . ?
C43 C42 H42 118.0(15) . . ?
C41 C42 H42 121.3(15) . . ?
C44 C43 C42 120.3(2) . . ?
C44 C43 H43 120.5(15) . . ?
C42 C43 H43 119.2(15) . . ?
C43 C44 C45 120.9(2) . . ?
C43 C44 H44 117.7(16) . . ?
C45 C44 H44 121.4(16) . . ?
C44 C45 C46 117.82(19) . . ?
C44 C45 C1 124.39(19) . . ?
C46 C45 C1 117.75(18) . . ?
O5 C46 C45 120.06(18) . . ?
O5 C46 C41 117.88(17) . . ?
C45 C46 C41 122.06(19) . . ?
C56 C51 C52 116.97(19) . . ?
C56 C51 Si 121.75(16) . . ?
C52 C51 Si 121.28(16) . . ?
C53 C52 C51 121.7(2) . . ?
C53 C52 H52 118.5(15) . . ?
C51 C52 H52 119.8(15) . . ?
C54 C53 C52 119.8(2) . . ?
C54 C53 H53 120.6(17) . . ?
C52 C53 H53 119.5(17) . . ?
C55 C54 C53 119.8(2) . . ?
C55 C54 H54 119.1(16) . . ?
C53 C54 H54 121.1(16) . . ?
C54 C55 C56 120.3(2) . . ?
C54 C55 H55 122.6(18) . . ?
C56 C55 H55 117.0(18) . . ?
C55 C56 C51 121.3(2) . . ?
C55 C56 H56 119.5(13) . . ?
C51 C56 H56 119.1(13) . . ?
C45 C1 C33 106.91(16) . . ?
C45 C1 C2 112.43(18) . . ?
C33 C1 C2 112.30(17) . . ?
C45 C1 C3 108.60(17) . . ?
C33 C1 C3 108.11(18) . . ?
C2 C1 C3 108.35(18) . . ?
C1 C2 H2C 111.1(16) . . ?
C1 C2 H2B 107.8(16) . . ?
H2C C2 H2B 115(2) . . ?
C1 C2 H2A 109.5(15) . . ?
H2C C2 H2A 110(2) . . ?
H2B C2 H2A 103(2) . . ?
C1 C3 H3C 109.8(16) . . ?
C1 C3 H3B 107.8(16) . . ?
H3C C3 H3B 112(2) . . ?
C1 C3 H3 112.3(16) . . ?
H3C C3 H3 110(2) . . ?
H3B C3 H3 105(2) . . ?
C61 O6 C64 108.91(18) . . ?
C61 O6 Na 126.97(15) . . ?
C64 O6 Na 118.16(15) . . ?
O6 C61 C62 106.7(2) . . ?
O6 C61 H61B 109.5(18) . . ?
C62 C61 H61B 110.3(18) . . ?
O6 C61 H61A 106.9(19) . . ?
C62 C61 H61A 115.8(19) . . ?
H61B C61 H61A 108(3) . . ?
C63 C62 C61 102.4(2) . . ?
C63 C62 H62B 114.7(19) . . ?
C61 C62 H62B 108.4(19) . . ?
C63 C62 H62A 107.4(17) . . ?
C61 C62 H62A 109.8(17) . . ?
H62B C62 H62A 114(3) . . ?
C64 C63 C62 101.8(2) . . ?
C64 C63 H63B 107.6(18) . . ?
C62 C63 H63B 109.8(18) . . ?
C64 C63 H63A 111.4(19) . . ?
C62 C63 H63A 112.7(19) . . ?
H63B C63 H63A 113(3) . . ?
O6 C64 C63 105.2(2) . . ?
O6 C64 H64B 104.1(18) . . ?
C63 C64 H64B 114.1(18) . . ?
O6 C64 H64A 107.5(17) . . ?
C63 C64 H64A 112.1(17) . . ?
H64B C64 H64A 113(3) . . ?
C74 O7 C71 106.5(2) . . ?
O7 C71 C72 105.8(2) . . ?
O7 C71 H71A 110.6 . . ?
C72 C71 H71A 110.6 . . ?
O7 C71 H71B 110.6 . . ?
C72 C71 H71B 110.6 . . ?
H71A C71 H71B 108.7 . . ?
C73 C72 C71 103.5(3) . . ?
C73 C72 H72A 111.1 . . ?
C71 C72 H72A 111.1 . . ?
C73 C72 H72B 111.1 . . ?
C71 C72 H72B 111.1 . . ?
H72A C72 H72B 109.0 . . ?
C72 C73 C74 104.8(3) . . ?
C72 C73 H73A 110.8 . . ?
C74 C73 H73A 110.8 . . ?
C72 C73 H73B 110.8 . . ?
C74 C73 H73B 110.8 . . ?
H73A C73 H73B 108.9 . . ?
O7 C74 C73 107.6(3) . . ?
O7 C74 H74A 110.2 . . ?
C73 C74 H74A 110.2 . . ?
O7 C74 H74B 110.2 . . ?
C73 C74 H74B 110.2 . . ?
H74A C74 H74B 108.5 . . ?
C81 O8 C84 105.5(3) . . ?
O8 C81 C82 116.1(4) . . ?
O8 C81 H81A 108.3 . . ?
C82 C81 H81A 108.3 . . ?
O8 C81 H81B 108.3 . . ?
C82 C81 H81B 108.3 . . ?
H81A C81 H81B 107.4 . . ?
C81 C82 C83 105.6(5) . . ?
C81 C82 H82A 110.6 . . ?
C83 C82 H82A 110.6 . . ?
C81 C82 H82B 110.6 . . ?
C83 C82 H82B 110.6 . . ?
H82A C82 H82B 108.8 . . ?
C82 C83 C84 105.2(5) . . ?
C82 C83 H83A 110.7 . . ?
C84 C83 H83A 110.7 . . ?
C82 C83 H83B 110.7 . . ?
C84 C83 H83B 110.7 . . ?
H83A C83 H83B 108.8 . . ?
O8 C84 C83 107.0(4) . . ?
O8 C84 H84A 110.3 . . ?
C83 C84 H84A 110.3 . . ?
O8 C84 H84B 110.3 . . ?
C83 C84 H84B 110.3 . . ?
H84A C84 H84B 108.6 . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_SiLi
_database_code_depnum_ccdc_archive 'CCDC 1922353'
loop_
_audit_author_name
_audit_author_address
'Allen G. Oliver'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'(Tetrahydrofuran)lithium((9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dioxybenzaldimine)(phenyl)silicate) bis(tetrahydrofuran) solvate'
_chemical_name_common            '(THF)Li[(Xbic)SiPh] . 2 THF'
_chemical_melting_point          .
_chemical_formula_moiety         'C55 H65 Li N2 O6 Si, 2(C4 H8 O)'
_chemical_formula_sum            'C63 H81 Li N2 O8 Si'
_chemical_formula_weight         1029.32

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.0349(9)
_cell_length_b                   19.6695(12)
_cell_length_c                   17.5883(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.404(2)
_cell_angle_gamma                90
_cell_volume                     5537.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9948
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.90

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             2216
_exptl_transmission_factor_min   0.7073
_exptl_transmission_factor_max   0.7458
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.248
_exptl_absorpt_coefficient_mu    0.100
_shelx_estimated_absorpt_T_min   0.967
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.99841
_exptl_absorpt_correction_T_max  0.99899
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_recrystallization_method 
'Crystals were deposited by diffusion of acetonitrile into a solution of the compound in THF.'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            124873
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.555
_diffrn_reflns_theta_max         28.928
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14612
_reflns_number_gt                10816
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

 The 1 0 0 reflection was omitted since it was obscured by the
beamstop.
;

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
C63 on the THF molecule bound to lithium was found to be split,
so it was modeled as C63A and C63B, with their thermal parameters
constrained to be equal.
Hydrogens on the Xbic ligand were found on the difference map
and refined isotropically. Hydrogens on the THF ligand and lattice 
THF molecules were placed in calculated positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0886P)²+5.8443P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14612
_refine_ls_number_parameters     908
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1826
_refine_ls_wR_factor_gt          0.1625
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
SI1 Si 0.31950(3) 0.63607(3) 0.91311(3) 0.01755(12) Uani 1 1 d . . . . .
LI1 Li 0.1544(2) 0.56293(18) 0.8599(2) 0.0249(7) Uani 1 1 d . . . . .
O1 O 0.32685(8) 0.72353(7) 0.92430(8) 0.0207(3) Uani 1 1 d . . . . .
O2 O 0.21124(8) 0.64499(7) 0.91592(8) 0.0187(3) Uani 1 1 d . . . . .
O3 O 0.39104(8) 0.64225(7) 0.84503(8) 0.0213(3) Uani 1 1 d . . . . .
O4 O 0.28888(8) 0.55656(7) 0.87217(8) 0.0195(3) Uani 1 1 d . . . . .
O5 O 0.03124(8) 0.49298(7) 0.84580(8) 0.0196(3) Uani 1 1 d . . . . .
O6 O 0.14303(10) 0.60248(8) 0.75408(9) 0.0288(3) Uani 1 1 d . . . . .
N1 N 0.04610(10) 0.61443(9) 0.91555(9) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.18710(10) 0.45444(8) 0.82313(9) 0.0192(3) Uani 1 1 d . . . . .
C11 C 0.25221(11) 0.75514(10) 0.92534(11) 0.0185(4) Uani 1 1 d . . . . .
C12 C 0.18531(11) 0.71000(10) 0.92163(10) 0.0175(4) Uani 1 1 d . . . . .
C13 C 0.10197(11) 0.73002(10) 0.92097(10) 0.0180(4) Uani 1 1 d . . . . .
C14 C 0.08653(12) 0.80160(10) 0.92311(11) 0.0190(4) Uani 1 1 d . . . . .
C15 C 0.15466(12) 0.84467(10) 0.92486(11) 0.0194(4) Uani 1 1 d . . . . .
H15 H 0.1430(14) 0.8897(12) 0.9255(12) 0.015(5) Uiso 1 1 d . . . . .
C16 C 0.23856(12) 0.82422(10) 0.92530(10) 0.0182(4) Uani 1 1 d . . . . .
C17 C 0.31104(12) 0.87429(10) 0.92196(11) 0.0206(4) Uani 1 1 d . . . . .
C171 C 0.37226(14) 0.86423(12) 0.99095(12) 0.0254(4) Uani 1 1 d . . . . .
H17A H 0.4190(16) 0.8955(13) 0.9896(14) 0.026(6) Uiso 1 1 d . . . . .
H17B H 0.3954(17) 0.8175(15) 0.9909(16) 0.036(7) Uiso 1 1 d . . . . .
H17C H 0.3451(16) 0.8721(13) 1.0366(16) 0.028(6) Uiso 1 1 d . . . . .
C172 C 0.35496(14) 0.86137(13) 0.84810(12) 0.0268(4) Uani 1 1 d . . . . .
H17D H 0.3974(16) 0.8971(13) 0.8422(14) 0.027(6) Uiso 1 1 d . . . . .
H17E H 0.3786(16) 0.8197(14) 0.8489(14) 0.024(6) Uiso 1 1 d . . . . .
H17F H 0.3171(17) 0.8657(14) 0.8040(16) 0.034(7) Uiso 1 1 d . . . . .
C173 C 0.28155(15) 0.94784(12) 0.92119(14) 0.0291(5) Uani 1 1 d . . . . .
H17G H 0.3298(16) 0.9757(13) 0.9207(14) 0.028(6) Uiso 1 1 d . . . . .
H17H H 0.2538(18) 0.9588(14) 0.9673(17) 0.039(8) Uiso 1 1 d . . . . .
H17I H 0.2438(17) 0.9588(14) 0.8736(16) 0.034(7) Uiso 1 1 d . . . . .
C18 C -0.00216(12) 0.83276(11) 0.92050(12) 0.0222(4) Uani 1 1 d . . . . .
C181 C -0.04845(15) 0.81398(13) 0.99140(14) 0.0300(5) Uani 1 1 d . . . . .
H18A H -0.1050(18) 0.8364(15) 0.9869(16) 0.040(8) Uiso 1 1 d . . . . .
H18B H -0.0184(17) 0.8345(14) 1.0389(16) 0.032(7) Uiso 1 1 d . . . . .
H18C H -0.0543(18) 0.7661(16) 0.9984(16) 0.038(7) Uiso 1 1 d . . . . .
C182 C -0.00058(15) 0.91040(12) 0.91916(15) 0.0304(5) Uani 1 1 d . . . . .
H18D H 0.0264(17) 0.9317(14) 0.9643(16) 0.031(7) Uiso 1 1 d . . . . .
H18E H -0.057(2) 0.9266(15) 0.9182(17) 0.046(8) Uiso 1 1 d . . . . .
H18F H 0.0246(17) 0.9287(14) 0.8766(17) 0.036(7) Uiso 1 1 d . . . . .
C183 C -0.05179(14) 0.81100(13) 0.84715(14) 0.0293(5) Uani 1 1 d . . . . .
H18G H -0.1079(18) 0.8295(14) 0.8452(16) 0.036(7) Uiso 1 1 d . . . . .
H18H H -0.0626(18) 0.7618(16) 0.8395(17) 0.041(8) Uiso 1 1 d . . . . .
H18I H -0.0225(19) 0.8227(15) 0.8052(18) 0.045(8) Uiso 1 1 d . . . . .
C19 C 0.03647(12) 0.67891(10) 0.92083(11) 0.0194(4) Uani 1 1 d . . . . .
H19 H -0.0152(15) 0.6937(12) 0.9261(13) 0.020(6) Uiso 1 1 d . . . . .
C21 C 0.39103(11) 0.58893(10) 0.79611(11) 0.0189(4) Uani 1 1 d . . . . .
C22 C 0.33099(11) 0.54061(10) 0.81105(11) 0.0181(4) Uani 1 1 d . . . . .
C23 C 0.31575(11) 0.48369(10) 0.76549(11) 0.0181(4) Uani 1 1 d . . . . .
C24 C 0.36605(11) 0.47522(10) 0.70188(11) 0.0186(4) Uani 1 1 d . . . . .
C25 C 0.42573(12) 0.52428(10) 0.68980(11) 0.0200(4) Uani 1 1 d . . . . .
H25 H 0.4563(15) 0.5184(12) 0.6464(14) 0.024(6) Uiso 1 1 d . . . . .
C26 C 0.44062(11) 0.58223(10) 0.73479(11) 0.0197(4) Uani 1 1 d . . . . .
C27 C 0.50520(13) 0.63589(11) 0.71686(12) 0.0238(4) Uani 1 1 d . . . . .
C271 C 0.46076(16) 0.70348(13) 0.69998(16) 0.0338(5) Uani 1 1 d . . . . .
H27A H 0.5008(18) 0.7395(15) 0.6883(16) 0.040(8) Uiso 1 1 d . . . . .
H27B H 0.4331(18) 0.7191(15) 0.7429(18) 0.041(8) Uiso 1 1 d . . . . .
H27C H 0.4231(19) 0.7004(15) 0.6537(18) 0.044(8) Uiso 1 1 d . . . . .
C272 C 0.56775(15) 0.64480(14) 0.78535(14) 0.0321(5) Uani 1 1 d . . . . .
H27D H 0.5964(18) 0.6026(15) 0.7959(16) 0.034(7) Uiso 1 1 d . . . . .
H27E H 0.6093(18) 0.6800(14) 0.7728(15) 0.035(7) Uiso 1 1 d . . . . .
H27F H 0.5386(18) 0.6622(14) 0.8305(17) 0.038(7) Uiso 1 1 d . . . . .
C273 C 0.55359(15) 0.61711(14) 0.64779(14) 0.0319(5) Uani 1 1 d . . . . .
H27G H 0.5868(18) 0.5759(15) 0.6594(16) 0.038(7) Uiso 1 1 d . . . . .
H27H H 0.5170(17) 0.6120(14) 0.5998(16) 0.034(7) Uiso 1 1 d . . . . .
H27I H 0.5945(17) 0.6554(14) 0.6398(16) 0.036(7) Uiso 1 1 d . . . . .
C28 C 0.35599(12) 0.41456(11) 0.64666(12) 0.0228(4) Uani 1 1 d . . . . .
C281 C 0.41191(15) 0.42150(13) 0.57947(13) 0.0303(5) Uani 1 1 d . . . . .
H28A H 0.4705(18) 0.4210(14) 0.5966(15) 0.034(7) Uiso 1 1 d . . . . .
H28B H 0.3992(18) 0.4643(16) 0.5495(17) 0.043(8) Uiso 1 1 d . . . . .
H28C H 0.4012(17) 0.3849(15) 0.5470(16) 0.037(7) Uiso 1 1 d . . . . .
C282 C 0.38178(16) 0.34831(13) 0.68757(16) 0.0327(5) Uani 1 1 d . . . . .
H28D H 0.439(2) 0.3517(15) 0.7070(17) 0.043(8) Uiso 1 1 d . . . . .
H28E H 0.3477(19) 0.3363(15) 0.7290(18) 0.043(8) Uiso 1 1 d . . . . .
H28F H 0.379(2) 0.3147(17) 0.6545(19) 0.051(9) Uiso 1 1 d . . . . .
C283 C 0.26651(14) 0.41025(13) 0.61034(14) 0.0294(5) Uani 1 1 d . . . . .
H28G H 0.2247(17) 0.4036(13) 0.6449(16) 0.033(7) Uiso 1 1 d . . . . .
H28H H 0.2533(19) 0.4484(16) 0.5785(18) 0.046(8) Uiso 1 1 d . . . . .
H28I H 0.2595(19) 0.3730(16) 0.5763(18) 0.046(8) Uiso 1 1 d . . . . .
C29 C 0.24849(12) 0.43788(11) 0.78319(11) 0.0205(4) Uani 1 1 d . . . . .
H29 H 0.2513(14) 0.3957(12) 0.7624(13) 0.018(6) Uiso 1 1 d . . . . .
C31 C -0.02575(11) 0.57467(10) 0.92646(11) 0.0195(4) Uani 1 1 d . . . . .
C32 C -0.03334(11) 0.51199(10) 0.89063(11) 0.0190(4) Uani 1 1 d . . . . .
C33 C -0.10209(12) 0.46957(10) 0.89729(11) 0.0197(4) Uani 1 1 d . . . . .
C34 C -0.16379(12) 0.49031(11) 0.94431(12) 0.0241(4) Uani 1 1 d . . . . .
H34 H -0.2118(16) 0.4628(13) 0.9504(14) 0.027(6) Uiso 1 1 d . . . . .
C35 C -0.15671(13) 0.55133(12) 0.98244(12) 0.0260(4) Uani 1 1 d . . . . .
H35 H -0.1988(17) 0.5614(14) 1.0175(16) 0.036(7) Uiso 1 1 d . . . . .
C36 C -0.08863(12) 0.59354(11) 0.97388(11) 0.0224(4) Uani 1 1 d . . . . .
H36 H -0.0836(14) 0.6345(12) 1.0011(13) 0.017(5) Uiso 1 1 d . . . . .
C41 C 0.12779(12) 0.40316(10) 0.83401(11) 0.0202(4) Uani 1 1 d . . . . .
C42 C 0.14618(13) 0.33422(11) 0.83972(12) 0.0231(4) Uani 1 1 d . . . . .
H42 H 0.2013(16) 0.3186(12) 0.8387(14) 0.024(6) Uiso 1 1 d . . . . .
C43 C 0.08345(14) 0.28790(11) 0.85133(12) 0.0265(4) Uani 1 1 d . . . . .
H43 H 0.0986(17) 0.2382(14) 0.8557(15) 0.033(7) Uiso 1 1 d . . . . .
C44 C 0.00174(14) 0.30922(11) 0.85529(12) 0.0259(4) Uani 1 1 d . . . . .
H44 H -0.0412(17) 0.2744(14) 0.8638(15) 0.034(7) Uiso 1 1 d . . . . .
C45 C -0.01871(12) 0.37757(11) 0.85040(11) 0.0217(4) Uani 1 1 d . . . . .
C46 C 0.04569(12) 0.42370(10) 0.84325(11) 0.0197(4) Uani 1 1 d . . . . .
C51 C 0.36727(11) 0.60595(10) 1.00605(11) 0.0197(4) Uani 1 1 d . . . . .
C52 C 0.39474(14) 0.53898(11) 1.01582(13) 0.0281(5) Uani 1 1 d . . . . .
H52 H 0.3879(16) 0.5060(14) 0.9743(15) 0.032(7) Uiso 1 1 d . . . . .
C53 C 0.43014(17) 0.51624(13) 1.08494(14) 0.0360(5) Uani 1 1 d . . . . .
H53 H 0.4504(19) 0.4704(16) 1.0865(17) 0.045(8) Uiso 1 1 d . . . . .
C54 C 0.43744(16) 0.55955(13) 1.14645(14) 0.0347(5) Uani 1 1 d . . . . .
H54 H 0.4626(19) 0.5459(15) 1.1942(18) 0.047(8) Uiso 1 1 d . . . . .
C55 C 0.41086(15) 0.62552(13) 1.13868(13) 0.0309(5) Uani 1 1 d . . . . .
H55 H 0.4158(18) 0.6563(15) 1.1775(17) 0.038(7) Uiso 1 1 d . . . . .
C56 C 0.37744(13) 0.64887(11) 1.06907(12) 0.0256(4) Uani 1 1 d . . . . .
H56 H 0.3586(15) 0.6950(13) 1.0645(13) 0.020(6) Uiso 1 1 d . . . . .
C61 C 0.17922(17) 0.66526(13) 0.73106(13) 0.0348(5) Uani 1 1 d . . . . .
H61A H 0.234410 0.672136 0.758263 0.042 Uiso 1 1 calc R U . . .
H61B H 0.142593 0.703886 0.742911 0.042 Uiso 1 1 calc R U . . .
C62 C 0.1886(2) 0.66093(17) 0.64649(16) 0.0560(8) Uani 1 1 d . . . . .
H62A H 0.144580 0.687775 0.618344 0.067 Uiso 0.781(7) 1 calc R U P A 1
H62B H 0.243912 0.678179 0.633375 0.067 Uiso 0.781(7) 1 calc R U P A 1
H62C H 0.167379 0.702523 0.620198 0.067 Uiso 0.219(7) 1 calc R U P A 2
H62D H 0.247603 0.653712 0.634954 0.067 Uiso 0.219(7) 1 calc R U P A 2
C63A C 0.1802(3) 0.58885(19) 0.62812(18) 0.0393(9) Uani 0.781(7) 1 d . . P A 1
H63A H 0.234666 0.565231 0.634257 0.047 Uiso 0.781(7) 1 calc R U P A 1
H63B H 0.156363 0.582135 0.575421 0.047 Uiso 0.781(7) 1 calc R U P A 1
C63B C 0.1372(11) 0.6018(7) 0.6248(7) 0.0393(9) Uani 0.219(7) 1 d . . P A 2
H63C H 0.084147 0.617279 0.598766 0.047 Uiso 0.219(7) 1 calc R U P A 2
H63D H 0.166899 0.573423 0.588582 0.047 Uiso 0.219(7) 1 calc R U P A 2
C64 C 0.12023(17) 0.56387(14) 0.68639(14) 0.0392(6) Uani 1 1 d . . . . .
H64A H 0.061486 0.572770 0.668679 0.047 Uiso 0.781(7) 1 calc R U P A 1
H64B H 0.127369 0.514538 0.695837 0.047 Uiso 0.781(7) 1 calc R U P A 1
H64C H 0.152373 0.520897 0.686495 0.047 Uiso 0.219(7) 1 calc R U P A 2
H64D H 0.059989 0.552559 0.684739 0.047 Uiso 0.219(7) 1 calc R U P A 2
C1 C -0.10698(12) 0.40517(11) 0.85005(12) 0.0223(4) Uani 1 1 d . . . . .
C2 C -0.16819(15) 0.35393(12) 0.87988(15) 0.0306(5) Uani 1 1 d . . . . .
H2A H -0.1534(14) 0.3414(12) 0.9347(14) 0.020(6) Uiso 1 1 d . . . . .
H2B H -0.1725(17) 0.3169(14) 0.8438(16) 0.034(7) Uiso 1 1 d . . . . .
H2C H -0.2221(19) 0.3735(15) 0.8777(17) 0.042(8) Uiso 1 1 d . . . . .
C3 C -0.13577(15) 0.42404(13) 0.76794(13) 0.0294(5) Uani 1 1 d . . . . .
H3A H -0.192(2) 0.4462(16) 0.7703(17) 0.048(8) Uiso 1 1 d . . . . .
H3B H -0.0995(17) 0.4596(14) 0.7452(15) 0.034(7) Uiso 1 1 d . . . . .
H3C H -0.1373(16) 0.3838(14) 0.7334(15) 0.030(7) Uiso 1 1 d . . . . .
O7 O 0.08264(15) 0.37684(12) 0.34016(12) 0.0584(6) Uani 1 1 d . . . . .
C71 C 0.1556(3) 0.4092(2) 0.3575(2) 0.0814(13) Uani 1 1 d . . . . .
H71A H 0.178321 0.395342 0.408689 0.098 Uiso 1 1 calc R U . . .
H71B H 0.146530 0.459014 0.357698 0.098 Uiso 1 1 calc R U . . .
C72 C 0.2147(3) 0.3911(2) 0.2998(3) 0.0828(12) Uani 1 1 d . . . . .
H72A H 0.254701 0.356283 0.320018 0.099 Uiso 1 1 calc R U . . .
H72B H 0.246482 0.431660 0.284911 0.099 Uiso 1 1 calc R U . . .
C73 C 0.1640(2) 0.3642(2) 0.2338(2) 0.0651(9) Uani 1 1 d . . . . .
H73A H 0.177594 0.316029 0.223975 0.078 Uiso 1 1 calc R U . . .
H73B H 0.171987 0.391250 0.187355 0.078 Uiso 1 1 calc R U . . .
C74 C 0.0747(2) 0.37170(18) 0.25983(18) 0.0527(7) Uani 1 1 d . . . . .
H74A H 0.047884 0.412969 0.237376 0.063 Uiso 1 1 calc R U . . .
H74B H 0.040539 0.331638 0.244123 0.063 Uiso 1 1 calc R U . . .
O8 O 0.33037(15) 0.27683(14) 0.89413(14) 0.0648(6) Uani 1 1 d . . . . .
C81 C 0.3016(3) 0.2494(2) 0.9597(2) 0.0756(11) Uani 1 1 d . . . . .
H81A H 0.330304 0.205766 0.971488 0.091 Uiso 1 1 calc R U . . .
H81B H 0.240894 0.240511 0.952693 0.091 Uiso 1 1 calc R U . . .
C82 C 0.3177(7) 0.2962(4) 1.0210(4) 0.198(5) Uani 1 1 d . . . . .
H82A H 0.333159 0.272268 1.069353 0.238 Uiso 1 1 calc R U . . .
H82B H 0.268913 0.325874 1.028136 0.238 Uiso 1 1 calc R U . . .
C83 C 0.3940(5) 0.3378(4) 0.9915(3) 0.137(3) Uani 1 1 d . . . . .
H83A H 0.391127 0.386338 1.006058 0.164 Uiso 1 1 calc R U . . .
H83B H 0.448090 0.318648 1.011404 0.164 Uiso 1 1 calc R U . . .
C84 C 0.3833(3) 0.3298(3) 0.9150(3) 0.1052(18) Uani 1 1 d . . . . .
H84A H 0.438322 0.321533 0.894010 0.126 Uiso 1 1 calc R U . . .
H84B H 0.360420 0.372415 0.892211 0.126 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
SI1 O3 1.7111(14) . ?
SI1 O1 1.7346(15) . ?
SI1 O2 1.7483(14) . ?
SI1 O4 1.7786(15) . ?
SI1 C51 1.860(2) . ?
LI1 O6 2.016(4) . ?
LI1 O2 2.074(4) . ?
LI1 O4 2.158(4) . ?
LI1 N1 2.280(4) . ?
LI1 N2 2.300(4) . ?
LI1 O5 2.408(4) . ?
O1 C11 1.350(2) . ?
O2 C12 1.350(2) . ?
O3 C21 1.356(2) . ?
O4 C22 1.340(2) . ?
O5 C46 1.383(2) . ?
O5 C32 1.389(2) . ?
O6 C61 1.433(3) . ?
O6 C64 1.441(3) . ?
N1 C19 1.282(3) . ?
N1 C31 1.415(2) . ?
N2 C29 1.285(3) . ?
N2 C41 1.407(2) . ?
C11 C16 1.376(3) . ?
C11 C12 1.391(3) . ?
C12 C13 1.393(3) . ?
C13 C14 1.430(3) . ?
C13 C19 1.454(3) . ?
C14 C15 1.381(3) . ?
C14 C18 1.547(3) . ?
C15 C16 1.404(3) . ?
C15 H15 0.91(2) . ?
C16 C17 1.527(3) . ?
C17 C173 1.522(3) . ?
C17 C171 1.528(3) . ?
C17 C172 1.535(3) . ?
C171 H17A 0.97(3) . ?
C171 H17B 0.99(3) . ?
C171 H17C 0.95(3) . ?
C172 H17D 0.99(3) . ?
C172 H17E 0.90(3) . ?
C172 H17F 0.96(3) . ?
C173 H17G 0.95(3) . ?
C173 H17H 0.97(3) . ?
C173 H17I 1.03(3) . ?
C18 C182 1.528(3) . ?
C18 C181 1.534(3) . ?
C18 C183 1.536(3) . ?
C181 H18A 1.01(3) . ?
C181 H18B 1.02(3) . ?
C181 H18C 0.96(3) . ?
C182 H18D 0.98(3) . ?
C182 H18E 0.96(3) . ?
C182 H18F 0.94(3) . ?
C183 H18G 0.97(3) . ?
C183 H18H 0.99(3) . ?
C183 H18I 0.93(3) . ?
C19 H19 0.89(2) . ?
C21 C26 1.384(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.390(3) . ?
C23 C24 1.427(3) . ?
C23 C29 1.453(3) . ?
C24 C25 1.384(3) . ?
C24 C28 1.541(3) . ?
C25 C26 1.400(3) . ?
C25 H25 0.94(3) . ?
C26 C27 1.525(3) . ?
C27 C273 1.525(3) . ?
C27 C271 1.529(3) . ?
C27 C272 1.531(3) . ?
C271 H27A 0.99(3) . ?
C271 H27B 0.95(3) . ?
C271 H27C 0.99(3) . ?
C272 H27D 0.96(3) . ?
C272 H27E 0.99(3) . ?
C272 H27F 1.01(3) . ?
C273 H27G 0.98(3) . ?
C273 H27H 1.00(3) . ?
C273 H27I 1.01(3) . ?
C28 C281 1.531(3) . ?
C28 C282 1.533(3) . ?
C28 C283 1.538(3) . ?
C281 H28A 0.97(3) . ?
C281 H28B 1.01(3) . ?
C281 H28C 0.93(3) . ?
C282 H28D 0.96(3) . ?
C282 H28E 0.97(3) . ?
C282 H28F 0.88(3) . ?
C283 H28G 0.94(3) . ?
C283 H28H 0.95(3) . ?
C283 H28I 0.95(3) . ?
C29 H29 0.91(2) . ?
C31 C32 1.387(3) . ?
C31 C36 1.396(3) . ?
C32 C33 1.393(3) . ?
C33 C34 1.388(3) . ?
C33 C1 1.515(3) . ?
C34 C35 1.376(3) . ?
C34 H34 0.95(3) . ?
C35 C36 1.387(3) . ?
C35 H35 0.96(3) . ?
C36 H36 0.94(2) . ?
C41 C42 1.390(3) . ?
C41 C46 1.396(3) . ?
C42 C43 1.381(3) . ?
C42 H42 0.94(3) . ?
C43 C44 1.381(3) . ?
C43 H43 1.01(3) . ?
C44 C45 1.385(3) . ?
C44 H44 0.99(3) . ?
C45 C46 1.386(3) . ?
C45 C1 1.516(3) . ?
C51 C56 1.395(3) . ?
C51 C52 1.396(3) . ?
C52 C53 1.385(3) . ?
C52 H52 0.98(3) . ?
C53 C54 1.377(4) . ?
C53 H53 0.96(3) . ?
C54 C55 1.370(4) . ?
C54 H54 0.95(3) . ?
C55 C56 1.385(3) . ?
C55 H55 0.91(3) . ?
C56 H56 0.96(2) . ?
C61 C62 1.506(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63A 1.459(5) . ?
C62 C63B 1.463(15) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 H62C 0.9900 . ?
C62 H62D 0.9900 . ?
C63A C64 1.527(5) . ?
C63A H63A 0.9900 . ?
C63A H63B 0.9900 . ?
C63B C64 1.356(13) . ?
C63B H63C 0.9900 . ?
C63B H63D 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C64 H64C 0.9900 . ?
C64 H64D 0.9900 . ?
C1 C2 1.522(3) . ?
C1 C3 1.535(3) . ?
C2 H2A 1.01(2) . ?
C2 H2B 0.96(3) . ?
C2 H2C 0.95(3) . ?
C3 H3A 1.01(3) . ?
C3 H3B 1.01(3) . ?
C3 H3C 1.00(3) . ?
O7 C71 1.350(4) . ?
O7 C74 1.415(4) . ?
C71 C72 1.473(6) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.475(6) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.535(5) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
O8 C81 1.378(5) . ?
O8 C84 1.379(5) . ?
C81 C82 1.428(9) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 C83 1.586(11) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.356(7) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 SI1 O1 88.00(7) . . ?
O3 SI1 O2 136.12(7) . . ?
O1 SI1 O2 87.60(6) . . ?
O3 SI1 O4 87.68(7) . . ?
O1 SI1 O4 158.94(7) . . ?
O2 SI1 O4 81.32(6) . . ?
O3 SI1 C51 112.29(8) . . ?
O1 SI1 C51 101.21(8) . . ?
O2 SI1 C51 111.39(8) . . ?
O4 SI1 C51 99.49(8) . . ?
O6 LI1 O2 98.70(16) . . ?
O6 LI1 O4 98.60(16) . . ?
O2 LI1 O4 65.75(11) . . ?
O6 LI1 N1 101.26(16) . . ?
O2 LI1 N1 77.00(13) . . ?
O4 LI1 N1 139.90(18) . . ?
O6 LI1 N2 96.18(15) . . ?
O2 LI1 N2 139.01(18) . . ?
O4 LI1 N2 74.39(12) . . ?
N1 LI1 N2 136.48(17) . . ?
O6 LI1 O5 95.54(15) . . ?
O2 LI1 O5 145.97(18) . . ?
O4 LI1 O5 141.79(18) . . ?
N1 LI1 O5 69.96(11) . . ?
N2 LI1 O5 68.90(11) . . ?
C11 O1 SI1 113.83(12) . . ?
C12 O2 SI1 114.07(12) . . ?
C12 O2 LI1 130.08(15) . . ?
SI1 O2 LI1 108.53(12) . . ?
C21 O3 SI1 114.47(12) . . ?
C22 O4 SI1 112.98(12) . . ?
C22 O4 LI1 118.79(15) . . ?
SI1 O4 LI1 103.86(12) . . ?
C46 O5 C32 114.55(15) . . ?
C46 O5 LI1 115.36(14) . . ?
C32 O5 LI1 114.95(14) . . ?
C61 O6 C64 107.93(18) . . ?
C61 O6 LI1 125.28(17) . . ?
C64 O6 LI1 124.35(18) . . ?
C19 N1 C31 115.75(17) . . ?
C19 N1 LI1 124.67(16) . . ?
C31 N1 LI1 117.36(16) . . ?
C29 N2 C41 116.02(17) . . ?
C29 N2 LI1 125.74(16) . . ?
C41 N2 LI1 117.36(15) . . ?
O1 C11 C16 126.58(17) . . ?
O1 C11 C12 112.78(17) . . ?
C16 C11 C12 120.53(17) . . ?
O2 C12 C11 111.59(16) . . ?
O2 C12 C13 124.54(17) . . ?
C11 C12 C13 123.83(18) . . ?
C12 C13 C14 116.47(17) . . ?
C12 C13 C19 119.82(18) . . ?
C14 C13 C19 123.68(17) . . ?
C15 C14 C13 117.80(17) . . ?
C15 C14 C18 118.83(17) . . ?
C13 C14 C18 123.34(17) . . ?
C14 C15 C16 125.51(18) . . ?
C14 C15 H15 115.9(14) . . ?
C16 C15 H15 118.6(14) . . ?
C11 C16 C15 115.80(17) . . ?
C11 C16 C17 121.02(17) . . ?
C15 C16 C17 123.11(17) . . ?
C173 C17 C16 112.13(17) . . ?
C173 C17 C171 108.35(18) . . ?
C16 C17 C171 109.91(16) . . ?
C173 C17 C172 107.92(18) . . ?
C16 C17 C172 108.31(16) . . ?
C171 C17 C172 110.19(17) . . ?
C17 C171 H17A 111.1(15) . . ?
C17 C171 H17B 110.1(16) . . ?
H17A C171 H17B 107(2) . . ?
C17 C171 H17C 110.2(16) . . ?
H17A C171 H17C 108(2) . . ?
H17B C171 H17C 110(2) . . ?
C17 C172 H17D 108.9(15) . . ?
C17 C172 H17E 110.5(16) . . ?
H17D C172 H17E 111(2) . . ?
C17 C172 H17F 111.7(16) . . ?
H17D C172 H17F 105(2) . . ?
H17E C172 H17F 110(2) . . ?
C17 C173 H17G 107.3(16) . . ?
C17 C173 H17H 111.2(17) . . ?
H17G C173 H17H 107(2) . . ?
C17 C173 H17I 112.1(15) . . ?
H17G C173 H17I 108(2) . . ?
H17H C173 H17I 111(2) . . ?
C182 C18 C181 105.22(18) . . ?
C182 C18 C183 105.89(18) . . ?
C181 C18 C183 111.36(19) . . ?
C182 C18 C14 112.36(17) . . ?
C181 C18 C14 111.65(17) . . ?
C183 C18 C14 110.13(17) . . ?
C18 C181 H18A 107.9(17) . . ?
C18 C181 H18B 110.0(15) . . ?
H18A C181 H18B 106(2) . . ?
C18 C181 H18C 113.5(17) . . ?
H18A C181 H18C 110(2) . . ?
H18B C181 H18C 109(2) . . ?
C18 C182 H18D 115.1(16) . . ?
C18 C182 H18E 108.5(18) . . ?
H18D C182 H18E 104(2) . . ?
C18 C182 H18F 113.7(17) . . ?
H18D C182 H18F 107(2) . . ?
H18E C182 H18F 108(2) . . ?
C18 C183 H18G 111.0(17) . . ?
C18 C183 H18H 117.6(17) . . ?
H18G C183 H18H 102(2) . . ?
C18 C183 H18I 109.8(19) . . ?
H18G C183 H18I 113(2) . . ?
H18H C183 H18I 103(2) . . ?
N1 C19 C13 126.46(18) . . ?
N1 C19 H19 116.7(16) . . ?
C13 C19 H19 116.8(15) . . ?
O3 C21 C26 126.13(18) . . ?
O3 C21 C22 112.52(16) . . ?
C26 C21 C22 121.27(18) . . ?
O4 C22 C21 112.30(17) . . ?
O4 C22 C23 124.83(17) . . ?
C21 C22 C23 122.83(17) . . ?
C22 C23 C24 117.24(17) . . ?
C22 C23 C29 118.90(17) . . ?
C24 C23 C29 123.83(18) . . ?
C25 C24 C23 117.84(18) . . ?
C25 C24 C28 119.38(17) . . ?
C23 C24 C28 122.78(17) . . ?
C24 C25 C26 125.23(18) . . ?
C24 C25 H25 116.0(15) . . ?
C26 C25 H25 118.7(15) . . ?
C21 C26 C25 115.57(18) . . ?
C21 C26 C27 121.60(18) . . ?
C25 C26 C27 122.80(17) . . ?
C26 C27 C273 112.40(18) . . ?
C26 C27 C271 109.12(17) . . ?
C273 C27 C271 108.01(19) . . ?
C26 C27 C272 109.74(17) . . ?
C273 C27 C272 108.29(18) . . ?
C271 C27 C272 109.2(2) . . ?
C27 C271 H27A 111.4(17) . . ?
C27 C271 H27B 111.2(18) . . ?
H27A C271 H27B 106(2) . . ?
C27 C271 H27C 111.2(18) . . ?
H27A C271 H27C 104(2) . . ?
H27B C271 H27C 113(2) . . ?
C27 C272 H27D 109.6(17) . . ?
C27 C272 H27E 108.8(16) . . ?
H27D C272 H27E 109(2) . . ?
C27 C272 H27F 110.3(16) . . ?
H27D C272 H27F 112(2) . . ?
H27E C272 H27F 107(2) . . ?
C27 C273 H27G 109.2(17) . . ?
C27 C273 H27H 113.2(16) . . ?
H27G C273 H27H 112(2) . . ?
C27 C273 H27I 107.1(16) . . ?
H27G C273 H27I 107(2) . . ?
H27H C273 H27I 108(2) . . ?
C281 C28 C282 106.49(18) . . ?
C281 C28 C283 105.01(18) . . ?
C282 C28 C283 111.54(19) . . ?
C281 C28 C24 111.91(17) . . ?
C282 C28 C24 110.31(18) . . ?
C283 C28 C24 111.39(17) . . ?
C28 C281 H28A 111.2(16) . . ?
C28 C281 H28B 111.6(17) . . ?
H28A C281 H28B 109(2) . . ?
C28 C281 H28C 108.1(18) . . ?
H28A C281 H28C 109(2) . . ?
H28B C281 H28C 108(2) . . ?
C28 C282 H28D 109.5(18) . . ?
C28 C282 H28E 114.4(18) . . ?
H28D C282 H28E 109(3) . . ?
C28 C282 H28F 109(2) . . ?
H28D C282 H28F 107(3) . . ?
H28E C282 H28F 108(3) . . ?
C28 C283 H28G 115.0(17) . . ?
C28 C283 H28H 111.7(19) . . ?
H28G C283 H28H 110(2) . . ?
C28 C283 H28I 112.2(19) . . ?
H28G C283 H28I 104(2) . . ?
H28H C283 H28I 103(3) . . ?
N2 C29 C23 124.23(19) . . ?
N2 C29 H29 120.6(15) . . ?
C23 C29 H29 115.1(15) . . ?
C32 C31 C36 117.44(17) . . ?
C32 C31 N1 118.68(17) . . ?
C36 C31 N1 123.83(18) . . ?
C31 C32 O5 116.68(16) . . ?
C31 C32 C33 122.88(17) . . ?
O5 C32 C33 120.44(17) . . ?
C34 C33 C32 118.02(19) . . ?
C34 C33 C1 123.87(17) . . ?
C32 C33 C1 118.05(17) . . ?
C35 C34 C33 120.37(19) . . ?
C35 C34 H34 119.0(15) . . ?
C33 C34 H34 120.6(15) . . ?
C34 C35 C36 120.79(19) . . ?
C34 C35 H35 116.8(17) . . ?
C36 C35 H35 122.3(17) . . ?
C35 C36 C31 120.4(2) . . ?
C35 C36 H36 120.2(14) . . ?
C31 C36 H36 119.3(14) . . ?
C42 C41 C46 118.12(18) . . ?
C42 C41 N2 124.53(18) . . ?
C46 C41 N2 117.27(18) . . ?
C43 C42 C41 120.1(2) . . ?
C43 C42 H42 118.8(15) . . ?
C41 C42 H42 121.0(15) . . ?
C42 C43 C44 120.6(2) . . ?
C42 C43 H43 118.4(15) . . ?
C44 C43 H43 121.0(15) . . ?
C43 C44 C45 120.89(19) . . ?
C43 C44 H44 117.9(16) . . ?
C45 C44 H44 121.2(16) . . ?
C44 C45 C46 117.79(19) . . ?
C44 C45 C1 124.43(18) . . ?
C46 C45 C1 117.76(18) . . ?
O5 C46 C45 120.99(17) . . ?
O5 C46 C41 116.73(17) . . ?
C45 C46 C41 122.28(19) . . ?
C56 C51 C52 116.86(19) . . ?
C56 C51 SI1 121.87(16) . . ?
C52 C51 SI1 121.27(16) . . ?
C53 C52 C51 121.5(2) . . ?
C53 C52 H52 117.6(16) . . ?
C51 C52 H52 120.8(16) . . ?
C54 C53 C52 120.1(2) . . ?
C54 C53 H53 123.2(18) . . ?
C52 C53 H53 116.7(18) . . ?
C55 C54 C53 119.8(2) . . ?
C55 C54 H54 118.1(19) . . ?
C53 C54 H54 122.1(19) . . ?
C54 C55 C56 120.3(2) . . ?
C54 C55 H55 122.8(18) . . ?
C56 C55 H55 116.9(18) . . ?
C55 C56 C51 121.5(2) . . ?
C55 C56 H56 119.5(14) . . ?
C51 C56 H56 119.0(14) . . ?
O6 C61 C62 107.2(2) . . ?
O6 C61 H61A 110.3 . . ?
C62 C61 H61A 110.3 . . ?
O6 C61 H61B 110.3 . . ?
C62 C61 H61B 110.3 . . ?
H61A C61 H61B 108.5 . . ?
C63A C62 C61 105.1(2) . . ?
C63B C62 C61 102.4(5) . . ?
C63A C62 H62A 110.7 . . ?
C61 C62 H62A 110.7 . . ?
C63A C62 H62B 110.7 . . ?
C61 C62 H62B 110.7 . . ?
H62A C62 H62B 108.8 . . ?
C63B C62 H62C 111.3 . . ?
C61 C62 H62C 111.3 . . ?
C63B C62 H62D 111.3 . . ?
C61 C62 H62D 111.3 . . ?
H62C C62 H62D 109.2 . . ?
C62 C63A C64 102.6(3) . . ?
C62 C63A H63A 111.3 . . ?
C64 C63A H63A 111.3 . . ?
C62 C63A H63B 111.3 . . ?
C64 C63A H63B 111.3 . . ?
H63A C63A H63B 109.2 . . ?
C64 C63B C62 111.5(9) . . ?
C64 C63B H63C 109.3 . . ?
C62 C63B H63C 109.3 . . ?
C64 C63B H63D 109.3 . . ?
C62 C63B H63D 109.3 . . ?
H63C C63B H63D 108.0 . . ?
C63B C64 O6 108.5(6) . . ?
O6 C64 C63A 104.2(2) . . ?
O6 C64 H64A 110.9 . . ?
C63A C64 H64A 110.9 . . ?
O6 C64 H64B 110.9 . . ?
C63A C64 H64B 110.9 . . ?
H64A C64 H64B 108.9 . . ?
C63B C64 H64C 110.0 . . ?
O6 C64 H64C 110.0 . . ?
C63B C64 H64D 110.0 . . ?
O6 C64 H64D 110.0 . . ?
H64C C64 H64D 108.4 . . ?
C33 C1 C45 106.22(16) . . ?
C33 C1 C2 112.22(17) . . ?
C45 C1 C2 112.50(18) . . ?
C33 C1 C3 108.47(18) . . ?
C45 C1 C3 108.61(17) . . ?
C2 C1 C3 108.69(18) . . ?
C1 C2 H2A 111.8(13) . . ?
C1 C2 H2B 107.2(16) . . ?
H2A C2 H2B 117(2) . . ?
C1 C2 H2C 108.8(18) . . ?
H2A C2 H2C 107(2) . . ?
H2B C2 H2C 105(2) . . ?
C1 C3 H3A 106.7(18) . . ?
C1 C3 H3B 113.1(16) . . ?
H3A C3 H3B 105(2) . . ?
C1 C3 H3C 112.1(15) . . ?
H3A C3 H3C 112(2) . . ?
H3B C3 H3C 108(2) . . ?
C71 O7 C74 106.5(3) . . ?
O7 C71 C72 108.4(3) . . ?
O7 C71 H71A 110.0 . . ?
C72 C71 H71A 110.0 . . ?
O7 C71 H71B 110.0 . . ?
C72 C71 H71B 110.0 . . ?
H71A C71 H71B 108.4 . . ?
C71 C72 C73 106.3(3) . . ?
C71 C72 H72A 110.5 . . ?
C73 C72 H72A 110.5 . . ?
C71 C72 H72B 110.5 . . ?
C73 C72 H72B 110.5 . . ?
H72A C72 H72B 108.7 . . ?
C72 C73 C74 102.2(3) . . ?
C72 C73 H73A 111.3 . . ?
C74 C73 H73A 111.3 . . ?
C72 C73 H73B 111.3 . . ?
C74 C73 H73B 111.3 . . ?
H73A C73 H73B 109.2 . . ?
O7 C74 C73 106.0(3) . . ?
O7 C74 H74A 110.5 . . ?
C73 C74 H74A 110.5 . . ?
O7 C74 H74B 110.5 . . ?
C73 C74 H74B 110.5 . . ?
H74A C74 H74B 108.7 . . ?
C81 O8 C84 107.7(3) . . ?
O8 C81 C82 109.0(4) . . ?
O8 C81 H81A 109.9 . . ?
C82 C81 H81A 109.9 . . ?
O8 C81 H81B 109.9 . . ?
C82 C81 H81B 109.9 . . ?
H81A C81 H81B 108.3 . . ?
C81 C82 C83 101.1(4) . . ?
C81 C82 H82A 111.5 . . ?
C83 C82 H82A 111.5 . . ?
C81 C82 H82B 111.5 . . ?
C83 C82 H82B 111.5 . . ?
H82A C82 H82B 109.4 . . ?
C84 C83 C82 102.1(5) . . ?
C84 C83 H83A 111.3 . . ?
C82 C83 H83A 111.3 . . ?
C84 C83 H83B 111.3 . . ?
C82 C83 H83B 111.3 . . ?
H83A C83 H83B 109.2 . . ?
C83 C84 O8 113.1(5) . . ?
C83 C84 H84A 109.0 . . ?
O8 C84 H84A 109.0 . . ?
C83 C84 H84B 109.0 . . ?
O8 C84 H84B 109.0 . . ?
H84A C84 H84B 107.8 . . ?

_refine_diff_density_max         0.924
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_sixbic_sq_final
_database_code_depnum_ccdc_archive 'CCDC 1922352'
loop_
_audit_author_name
_audit_author_address
'Allen G. Oliver'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT934_sixbic_sq_sq        
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....2 Check 
RESPONSE: These are not low angle reflections, so there is no reason to
OMIT them. SQUEEZE was ran on this structure, so the poor agreement between
Fobs and Fcalc could be due to the solvent that was SQUEEZEd. The esd's
are also not much higher than 10 (11.93 and 10.33).
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'(9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dioxybenzaldiminium)-(phenyl)silicon(IV) bichloride tri-chloroform solvate'
_chemical_name_common            '[(XbicH2)SiPh][HCl2] . 3 CHCl3'
_chemical_melting_point          .
_chemical_formula_moiety         'C51 H59 N2 O5 Si, H Cl2, 3(C H Cl3)'
_chemical_formula_sum            'C54 H63 Cl11 N2 O5 Si'
_chemical_formula_weight         1238.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.3173(8)
_cell_length_b                   17.8374(8)
_cell_length_c                   21.3223(11)
_cell_angle_alpha                89.6599(17)
_cell_angle_beta                 81.8824(17)
_cell_angle_gamma                84.0998(16)
_cell_volume                     6111.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9319
_cell_measurement_theta_min      2.296
_cell_measurement_theta_max      28.462

_exptl_crystal_description       'arrowhead block'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             2568
_exptl_transmission_factor_min   0.6797
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.686
_exptl_crystal_size_mid          0.503
_exptl_crystal_size_min          0.398
_exptl_absorpt_coefficient_mu    0.565
_shelx_estimated_absorpt_T_min   0.6797
_shelx_estimated_absorpt_T_max   0.7457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_recrystallization_method 
'Crystals deposited from a reaction mixture ofSiPhCl3 with an equivalent of XbicH4 in CHCl3layered with hexanes'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            123098
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         0.965
_diffrn_reflns_theta_max         28.528
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             30965
_reflns_number_gt                24316
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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


_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
The asymmetric unit contains two molecules of the complex and its 
bichloride counterion, as well as four ordered chloroform molecules.  
There was additional, disordered, electron density, which was treated
with the program SQUEEZE. The total amount of electron density found 
in the void spaces was 256 electrons/unit cell, corresponding to
approximately 4 CHCl3 molecules, for a total of 12 in the unit cell 
(3 per formula unit). 

The hydrogens bonded to N1-N4 and C19, C29, C69, and C79 were found on 
the difference map and refined isotropically. The hydrogens in the
HCl2 anions were also found on the difference map and refined 
isotropically. All other hydrogens were placed in calculated positions.

One of the bichloride anions (containing Cl3A and Cl3B) was disordered, 
with the occupancy of Cl3A refining to 89.3(2)% occupancy.  The two sites  
were constrained to have equal thermal parameters. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0583P)²+8.1181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         30965
_refine_ls_number_parameters     1287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
SI1 Si 0.77634(3) 0.24754(3) 0.15261(2) 0.01723(10) Uani 1 1 d . . . . .
O1 O 0.73241(9) 0.29112(7) 0.22349(6) 0.0203(3) Uani 1 1 d . . . . .
O2 O 0.80871(9) 0.16927(7) 0.19702(6) 0.0203(3) Uani 1 1 d . . . . .
O3 O 0.69629(9) 0.29312(7) 0.11917(6) 0.0197(3) Uani 1 1 d . . . . .
O4 O 0.78229(9) 0.17583(7) 0.09205(6) 0.0192(3) Uani 1 1 d . . . . .
O5 O 0.89645(8) -0.03351(7) 0.11425(6) 0.0185(3) Uani 1 1 d . . . . .
N1 N 0.89150(10) 0.04380(9) 0.22583(8) 0.0182(3) Uani 1 1 d . . . . .
H1 H 0.8778(15) 0.0687(14) 0.2000(12) 0.018(6) Uiso 1 1 d . . . . .
N2 N 0.83039(10) 0.05347(9) 0.02251(8) 0.0182(3) Uani 1 1 d . . . . .
H2 H 0.8352(16) 0.0773(15) 0.0528(13) 0.026(6) Uiso 1 1 d . . . . .
SI2 Si 0.22950(4) 0.25042(3) 0.60232(3) 0.02217(11) Uani 1 1 d . . . . .
O6 O 0.27302(10) 0.20442(9) 0.66333(7) 0.0277(3) Uani 1 1 d . . . . .
O7 O 0.19952(9) 0.32764(8) 0.65374(7) 0.0243(3) Uani 1 1 d . . . . .
O8 O 0.31081(9) 0.20831(8) 0.55194(7) 0.0256(3) Uani 1 1 d . . . . .
O9 O 0.21950(9) 0.32267(8) 0.54256(7) 0.0235(3) Uani 1 1 d . . . . .
O10 O 0.10779(9) 0.53015(7) 0.58972(6) 0.0198(3) Uani 1 1 d . . . . .
N3 N 0.11758(11) 0.45232(10) 0.70097(8) 0.0224(3) Uani 1 1 d . . . . .
H3 H 0.1344(16) 0.4259(15) 0.6685(13) 0.027(6) Uiso 1 1 d . . . . .
N4 N 0.16778(11) 0.44437(9) 0.48267(8) 0.0194(3) Uani 1 1 d . . . . .
H4 H 0.1658(17) 0.4251(15) 0.5124(13) 0.026(7) Uiso 1 1 d . . . . .
C11 C 0.74617(12) 0.25057(10) 0.27534(9) 0.0176(3) Uani 1 1 d . . . . .
C12 C 0.78939(12) 0.18065(10) 0.25973(9) 0.0173(3) Uani 1 1 d . . . . .
C13 C 0.81009(12) 0.12763(10) 0.30494(9) 0.0170(3) Uani 1 1 d . . . . .
C14 C 0.78136(11) 0.14582(10) 0.37025(9) 0.0170(3) Uani 1 1 d . . . . .
C15 C 0.73887(12) 0.21610(11) 0.38340(9) 0.0182(4) Uani 1 1 d . . . . .
H15 H 0.719835 0.228548 0.426623 0.022 Uiso 1 1 calc R U . . .
C16 C 0.72131(11) 0.27114(10) 0.33788(9) 0.0173(3) Uani 1 1 d . . . . .
C17 C 0.67628(12) 0.34876(11) 0.35582(9) 0.0206(4) Uani 1 1 d . . . . .
C171 C 0.59285(13) 0.35596(13) 0.33006(12) 0.0304(5) Uani 1 1 d . . . . .
H17A H 0.563173 0.405704 0.341272 0.046 Uiso 1 1 calc R U . . .
H17B H 0.602775 0.350038 0.283863 0.046 Uiso 1 1 calc R U . . .
H17C H 0.559227 0.316753 0.348568 0.046 Uiso 1 1 calc R U . . .
C172 C 0.72934(14) 0.40946(11) 0.32635(11) 0.0258(4) Uani 1 1 d . . . . .
H17D H 0.700479 0.459440 0.337837 0.039 Uiso 1 1 calc R U . . .
H17E H 0.783136 0.404166 0.342223 0.039 Uiso 1 1 calc R U . . .
H17F H 0.738352 0.403585 0.280144 0.039 Uiso 1 1 calc R U . . .
C173 C 0.66002(16) 0.36177(13) 0.42748(11) 0.0332(5) Uani 1 1 d . . . . .
H17G H 0.631060 0.412222 0.436743 0.050 Uiso 1 1 calc R U . . .
H17H H 0.625468 0.323885 0.447265 0.050 Uiso 1 1 calc R U . . .
H17I H 0.713111 0.357559 0.444380 0.050 Uiso 1 1 calc R U . . .
C18 C 0.79464(13) 0.08975(11) 0.42399(9) 0.0210(4) Uani 1 1 d . . . . .
C181 C 0.75226(16) 0.12195(14) 0.48817(10) 0.0345(5) Uani 1 1 d . . . . .
H18A H 0.775357 0.168748 0.496952 0.052 Uiso 1 1 calc R U . . .
H18B H 0.692300 0.132413 0.487244 0.052 Uiso 1 1 calc R U . . .
H18C H 0.761986 0.085301 0.521435 0.052 Uiso 1 1 calc R U . . .
C182 C 0.88753(13) 0.07252(12) 0.43080(10) 0.0254(4) Uani 1 1 d . . . . .
H18D H 0.918158 0.051580 0.390837 0.038 Uiso 1 1 calc R U . . .
H18E H 0.909935 0.119112 0.441144 0.038 Uiso 1 1 calc R U . . .
H18F H 0.893509 0.035932 0.464732 0.038 Uiso 1 1 calc R U . . .
C183 C 0.75574(15) 0.01689(12) 0.41326(12) 0.0311(5) Uani 1 1 d . . . . .
H18G H 0.781230 -0.005715 0.372441 0.047 Uiso 1 1 calc R U . . .
H18H H 0.765424 -0.018612 0.447335 0.047 Uiso 1 1 calc R U . . .
H18I H 0.695738 0.028500 0.413144 0.047 Uiso 1 1 calc R U . . .
C19 C 0.86264(12) 0.06166(10) 0.28456(9) 0.0188(4) Uani 1 1 d . . . . .
H19 H 0.8812(14) 0.0276(13) 0.3135(11) 0.014(5) Uiso 1 1 d . . . . .
C21 C 0.67860(12) 0.26022(10) 0.06634(8) 0.0171(3) Uani 1 1 d . . . . .
C22 C 0.72850(12) 0.19292(10) 0.05136(9) 0.0170(3) Uani 1 1 d . . . . .
C23 C 0.72042(12) 0.14720(10) -0.00031(9) 0.0177(4) Uani 1 1 d . . . . .
C24 C 0.65689(12) 0.17216(11) -0.03869(9) 0.0203(4) Uani 1 1 d . . . . .
C25 C 0.60937(12) 0.23920(11) -0.02132(9) 0.0215(4) Uani 1 1 d . . . . .
H25 H 0.567745 0.255961 -0.046657 0.026 Uiso 1 1 calc R U . . .
C26 C 0.61716(12) 0.28525(11) 0.03091(9) 0.0185(4) Uani 1 1 d . . . . .
C27 C 0.55946(13) 0.35689(11) 0.04844(9) 0.0217(4) Uani 1 1 d . . . . .
C271 C 0.50030(15) 0.37677(14) -0.00013(11) 0.0331(5) Uani 1 1 d . . . . .
H27A H 0.464603 0.423108 0.013215 0.050 Uiso 1 1 calc R U . . .
H27B H 0.532690 0.384406 -0.041576 0.050 Uiso 1 1 calc R U . . .
H27C H 0.465680 0.335539 -0.003152 0.050 Uiso 1 1 calc R U . . .
C272 C 0.60998(15) 0.42341(12) 0.05437(11) 0.0295(5) Uani 1 1 d . . . . .
H27D H 0.572060 0.469058 0.065651 0.044 Uiso 1 1 calc R U . . .
H27E H 0.645598 0.412961 0.087404 0.044 Uiso 1 1 calc R U . . .
H27F H 0.644680 0.430871 0.013859 0.044 Uiso 1 1 calc R U . . .
C273 C 0.50710(14) 0.34470(13) 0.11274(10) 0.0291(5) Uani 1 1 d . . . . .
H27G H 0.469461 0.390279 0.124898 0.044 Uiso 1 1 calc R U . . .
H27H H 0.474452 0.302107 0.109440 0.044 Uiso 1 1 calc R U . . .
H27I H 0.544002 0.333934 0.144883 0.044 Uiso 1 1 calc R U . . .
C28 C 0.64176(14) 0.12789(13) -0.09680(10) 0.0284(5) Uani 1 1 d . . . . .
C281 C 0.71829(16) 0.12317(14) -0.14750(10) 0.0333(5) Uani 1 1 d . . . . .
H28A H 0.766262 0.097889 -0.130134 0.050 Uiso 1 1 calc R U . . .
H28B H 0.707736 0.094467 -0.184066 0.050 Uiso 1 1 calc R U . . .
H28C H 0.729985 0.174119 -0.160830 0.050 Uiso 1 1 calc R U . . .
C282 C 0.57039(18) 0.16799(18) -0.12811(13) 0.0480(8) Uani 1 1 d . . . . .
H28D H 0.519197 0.172694 -0.097618 0.072 Uiso 1 1 calc R U . . .
H28E H 0.584323 0.218258 -0.141740 0.072 Uiso 1 1 calc R U . . .
H28F H 0.562074 0.138606 -0.164976 0.072 Uiso 1 1 calc R U . . .
C283 C 0.61580(16) 0.04963(15) -0.07778(13) 0.0392(6) Uani 1 1 d . . . . .
H28G H 0.566661 0.055123 -0.045280 0.059 Uiso 1 1 calc R U . . .
H28H H 0.602596 0.023884 -0.115005 0.059 Uiso 1 1 calc R U . . .
H28I H 0.661588 0.019936 -0.060902 0.059 Uiso 1 1 calc R U . . .
C29 C 0.77334(12) 0.07931(11) -0.01189(9) 0.0187(4) Uani 1 1 d . . . . .
H29 H 0.7678(14) 0.0503(13) -0.0472(11) 0.015(5) Uiso 1 1 d . . . . .
C31 C 0.95286(12) -0.01737(10) 0.20951(9) 0.0188(4) Uani 1 1 d . . . . .
C32 C 0.95282(12) -0.05898(10) 0.15480(9) 0.0179(4) Uani 1 1 d . . . . .
C33 C 1.00655(12) -0.12454(10) 0.14213(9) 0.0194(4) Uani 1 1 d . . . . .
C34 C 1.06492(13) -0.14321(11) 0.18254(10) 0.0225(4) Uani 1 1 d . . . . .
H34 H 1.102377 -0.187593 0.174461 0.027 Uiso 1 1 calc R U . . .
C35 C 1.06961(13) -0.09838(12) 0.23445(10) 0.0249(4) Uani 1 1 d . . . . .
H35 H 1.111983 -0.110551 0.260240 0.030 Uiso 1 1 calc R U . . .
C36 C 1.01276(13) -0.03608(11) 0.24868(10) 0.0224(4) Uani 1 1 d . . . . .
H36 H 1.014580 -0.006157 0.285067 0.027 Uiso 1 1 calc R U . . .
C41 C 0.88688(12) -0.01148(10) 0.00522(9) 0.0182(4) Uani 1 1 d . . . . .
C42 C 0.90957(13) -0.03090(11) -0.05828(9) 0.0209(4) Uani 1 1 d . . . . .
H42 H 0.888784 -0.000033 -0.090160 0.025 Uiso 1 1 calc R U . . .
C43 C 0.96252(13) -0.09533(11) -0.07485(10) 0.0228(4) Uani 1 1 d . . . . .
H43 H 0.978300 -0.108738 -0.118247 0.027 Uiso 1 1 calc R U . . .
C44 C 0.99262(13) -0.14036(11) -0.02854(10) 0.0221(4) Uani 1 1 d . . . . .
H44 H 1.029128 -0.184479 -0.040521 0.027 Uiso 1 1 calc R U . . .
C45 C 0.97039(12) -0.12215(10) 0.03524(9) 0.0197(4) Uani 1 1 d . . . . .
C46 C 0.91882(12) -0.05622(10) 0.05148(9) 0.0183(4) Uani 1 1 d . . . . .
C51 C 0.87273(13) 0.29188(11) 0.12586(9) 0.0217(4) Uani 1 1 d . . . . .
C52 C 0.94601(14) 0.26804(12) 0.15120(11) 0.0271(4) Uani 1 1 d . . . . .
H52 H 0.943936 0.233240 0.185144 0.033 Uiso 1 1 calc R U . . .
C53 C 1.02102(15) 0.29430(15) 0.12764(12) 0.0356(5) Uani 1 1 d . . . . .
H53 H 1.070162 0.276407 0.144549 0.043 Uiso 1 1 calc R U . . .
C54 C 1.02449(17) 0.34617(15) 0.07987(13) 0.0411(6) Uani 1 1 d . . . . .
H54 H 1.076067 0.364082 0.063573 0.049 Uiso 1 1 calc R U . . .
C55 C 0.95307(18) 0.37233(14) 0.05548(12) 0.0383(6) Uani 1 1 d . . . . .
H55 H 0.955380 0.409225 0.023143 0.046 Uiso 1 1 calc R U . . .
C56 C 0.87797(15) 0.34509(12) 0.07790(11) 0.0293(5) Uani 1 1 d . . . . .
H56 H 0.829401 0.363005 0.060256 0.035 Uiso 1 1 calc R U . . .
C1 C 0.99339(13) -0.17401(11) 0.08805(10) 0.0217(4) Uani 1 1 d . . . . .
C2 C 0.91817(14) -0.21756(12) 0.11058(11) 0.0283(4) Uani 1 1 d . . . . .
H2A H 0.908290 -0.250214 0.076197 0.043 Uiso 1 1 calc R U . . .
H2B H 0.929496 -0.248422 0.147162 0.043 Uiso 1 1 calc R U . . .
H2C H 0.868802 -0.181795 0.122727 0.043 Uiso 1 1 calc R U . . .
C3 C 1.06916(15) -0.23019(12) 0.06730(11) 0.0293(5) Uani 1 1 d . . . . .
H3A H 1.058180 -0.261172 0.032210 0.044 Uiso 1 1 calc R U . . .
H3B H 1.117530 -0.202835 0.053398 0.044 Uiso 1 1 calc R U . . .
H3C H 1.080463 -0.262682 0.102960 0.044 Uiso 1 1 calc R U . . .
C61 C 0.26025(13) 0.24334(11) 0.71818(10) 0.0224(4) Uani 1 1 d . . . . .
C62 C 0.21835(13) 0.31421(11) 0.71236(10) 0.0224(4) Uani 1 1 d . . . . .
C63 C 0.19834(14) 0.36613(11) 0.76211(10) 0.0238(4) Uani 1 1 d . . . . .
C64 C 0.22633(15) 0.34648(12) 0.82147(11) 0.0292(5) Uani 1 1 d . . . . .
C65 C 0.26769(15) 0.27524(12) 0.82500(11) 0.0289(5) Uani 1 1 d . . . . .
H65 H 0.285923 0.261313 0.864230 0.035 Uiso 1 1 calc R U . . .
C66 C 0.28519(13) 0.22136(12) 0.77532(10) 0.0243(4) Uani 1 1 d . . . . .
C67 C 0.33044(15) 0.14307(13) 0.78255(11) 0.0303(5) Uani 1 1 d . . . . .
C671 C 0.3474(2) 0.12934(15) 0.85061(13) 0.0454(7) Uani 1 1 d . . . . .
H67A H 0.294542 0.133549 0.879233 0.068 Uiso 1 1 calc R U . . .
H67B H 0.376187 0.078740 0.853676 0.068 Uiso 1 1 calc R U . . .
H67C H 0.382314 0.166923 0.862539 0.068 Uiso 1 1 calc R U . . .
C672 C 0.27653(17) 0.08284(13) 0.76520(12) 0.0355(5) Uani 1 1 d . . . . .
H67D H 0.223563 0.087421 0.793683 0.053 Uiso 1 1 calc R U . . .
H67E H 0.265833 0.089972 0.721360 0.053 Uiso 1 1 calc R U . . .
H67F H 0.305775 0.032668 0.769466 0.053 Uiso 1 1 calc R U . . .
C673 C 0.41280(17) 0.13640(17) 0.73858(15) 0.0466(7) Uani 1 1 d . . . . .
H67G H 0.442301 0.086349 0.742878 0.070 Uiso 1 1 calc R U . . .
H67H H 0.402300 0.143510 0.694699 0.070 Uiso 1 1 calc R U . . .
H67I H 0.446870 0.175050 0.749837 0.070 Uiso 1 1 calc R U . . .
C68 C 0.2126(2) 0.40226(13) 0.87880(13) 0.0443(7) Uani 1 1 d . . . . .
C681 C 0.2585(3) 0.36874(18) 0.93247(17) 0.0823(15) Uani 1 1 d . . . . .
H68A H 0.317788 0.357207 0.916514 0.123 Uiso 1 1 calc R U . . .
H68B H 0.251912 0.405264 0.967433 0.123 Uiso 1 1 calc R U . . .
H68C H 0.235073 0.322423 0.947624 0.123 Uiso 1 1 calc R U . . .
C682 C 0.2524(2) 0.47496(15) 0.85858(17) 0.0545(8) Uani 1 1 d . . . . .
H68D H 0.311111 0.462235 0.841448 0.082 Uiso 1 1 calc R U . . .
H68E H 0.223149 0.500393 0.826035 0.082 Uiso 1 1 calc R U . . .
H68F H 0.248203 0.508467 0.895404 0.082 Uiso 1 1 calc R U . . .
C683 C 0.1209(2) 0.41923(15) 0.90588(13) 0.0506(8) Uani 1 1 d . . . . .
H68G H 0.089901 0.440722 0.872725 0.076 Uiso 1 1 calc R U . . .
H68H H 0.098541 0.372515 0.921238 0.076 Uiso 1 1 calc R U . . .
H68I H 0.115380 0.455356 0.941047 0.076 Uiso 1 1 calc R U . . .
C69 C 0.14686(14) 0.43304(11) 0.75329(10) 0.0241(4) Uani 1 1 d . . . . .
H69 H 0.1306(15) 0.4685(14) 0.7886(12) 0.023(6) Uiso 1 1 d . . . . .
C71 C 0.32344(13) 0.23954(11) 0.49385(10) 0.0219(4) Uani 1 1 d . . . . .
C72 C 0.27019(12) 0.30533(11) 0.48929(9) 0.0206(4) Uani 1 1 d . . . . .
C73 C 0.27402(12) 0.34908(11) 0.43422(9) 0.0199(4) Uani 1 1 d . . . . .
C74 C 0.33252(12) 0.32168(11) 0.38010(9) 0.0212(4) Uani 1 1 d . . . . .
C75 C 0.38404(13) 0.25743(12) 0.38838(10) 0.0235(4) Uani 1 1 d . . . . .
H75 H 0.423370 0.239838 0.353056 0.028 Uiso 1 1 calc R U . . .
C76 C 0.38370(13) 0.21529(11) 0.44464(10) 0.0233(4) Uani 1 1 d . . . . .
C77 C 0.44643(14) 0.14727(12) 0.45183(11) 0.0287(5) Uani 1 1 d . . . . .
C771 C 0.40108(16) 0.07795(13) 0.47196(13) 0.0347(5) Uani 1 1 d . . . . .
H77A H 0.442015 0.034739 0.476401 0.052 Uiso 1 1 calc R U . . .
H77B H 0.365462 0.088338 0.512599 0.052 Uiso 1 1 calc R U . . .
H77C H 0.366784 0.066489 0.439751 0.052 Uiso 1 1 calc R U . . .
C772 C 0.50488(17) 0.12788(15) 0.39001(14) 0.0436(6) Uani 1 1 d . . . . .
H77D H 0.544037 0.084065 0.396612 0.065 Uiso 1 1 calc R U . . .
H77E H 0.472142 0.116204 0.356837 0.065 Uiso 1 1 calc R U . . .
H77F H 0.535832 0.170985 0.377056 0.065 Uiso 1 1 calc R U . . .
C773 C 0.49865(16) 0.16633(15) 0.50291(14) 0.0402(6) Uani 1 1 d . . . . .
H77G H 0.539470 0.123357 0.508357 0.060 Uiso 1 1 calc R U . . .
H77H H 0.527737 0.210525 0.489951 0.060 Uiso 1 1 calc R U . . .
H77I H 0.462110 0.177276 0.543062 0.060 Uiso 1 1 calc R U . . .
C78 C 0.33647(13) 0.35970(13) 0.31517(10) 0.0264(4) Uani 1 1 d . . . . .
C781 C 0.39683(15) 0.31346(16) 0.26449(11) 0.0370(6) Uani 1 1 d . . . . .
H78A H 0.379411 0.262752 0.261804 0.055 Uiso 1 1 calc R U . . .
H78B H 0.396419 0.338244 0.223381 0.055 Uiso 1 1 calc R U . . .
H78C H 0.453171 0.309902 0.275976 0.055 Uiso 1 1 calc R U . . .
C782 C 0.25143(14) 0.36357(14) 0.29151(11) 0.0313(5) Uani 1 1 d . . . . .
H78D H 0.233601 0.312808 0.290801 0.047 Uiso 1 1 calc R U . . .
H78E H 0.210428 0.395999 0.319972 0.047 Uiso 1 1 calc R U . . .
H78F H 0.256033 0.384387 0.248662 0.047 Uiso 1 1 calc R U . . .
C783 C 0.36694(15) 0.43802(14) 0.31708(12) 0.0343(5) Uani 1 1 d . . . . .
H78G H 0.368776 0.460780 0.275021 0.051 Uiso 1 1 calc R U . . .
H78H H 0.328736 0.469968 0.347873 0.051 Uiso 1 1 calc R U . . .
H78I H 0.422774 0.433373 0.329548 0.051 Uiso 1 1 calc R U . . .
C79 C 0.22206(12) 0.41769(11) 0.43494(9) 0.0195(4) Uani 1 1 d . . . . .
H79 H 0.2257(14) 0.4448(13) 0.3993(11) 0.018(6) Uiso 1 1 d . . . . .
C81 C 0.05752(13) 0.51480(11) 0.69874(10) 0.0220(4) Uani 1 1 d . . . . .
C82 C 0.05540(12) 0.55663(11) 0.64372(9) 0.0198(4) Uani 1 1 d . . . . .
C83 C 0.00365(12) 0.62374(11) 0.64428(10) 0.0212(4) Uani 1 1 d . . . . .
C84 C -0.04923(13) 0.64473(11) 0.69931(11) 0.0254(4) Uani 1 1 d . . . . .
H84 H -0.083932 0.691002 0.700527 0.031 Uiso 1 1 calc R U . . .
C85 C -0.05274(15) 0.60002(12) 0.75250(11) 0.0286(4) Uani 1 1 d . . . . .
H85 H -0.092043 0.613826 0.788863 0.034 Uiso 1 1 calc R U . . .
C86 C 0.00114(14) 0.53520(12) 0.75253(10) 0.0267(4) Uani 1 1 d . . . . .
H86 H -0.000255 0.504575 0.789196 0.032 Uiso 1 1 calc R U . . .
C91 C 0.11276(12) 0.51053(11) 0.47894(9) 0.0198(4) Uani 1 1 d . . . . .
C92 C 0.08749(13) 0.53146(11) 0.42125(10) 0.0219(4) Uani 1 1 d . . . . .
H92 H 0.105648 0.500673 0.384721 0.026 Uiso 1 1 calc R U . . .
C93 C 0.03594(13) 0.59708(11) 0.41715(10) 0.0240(4) Uani 1 1 d . . . . .
H93 H 0.018938 0.611612 0.377636 0.029 Uiso 1 1 calc R U . . .
C94 C 0.00904(13) 0.64158(11) 0.46999(10) 0.0237(4) Uani 1 1 d . . . . .
H94 H -0.026363 0.686681 0.466475 0.028 Uiso 1 1 calc R U . . .
C95 C 0.03278(12) 0.62169(11) 0.52848(10) 0.0204(4) Uani 1 1 d . . . . .
C96 C 0.08334(12) 0.55463(10) 0.53261(9) 0.0188(4) Uani 1 1 d . . . . .
C101 C 0.13354(14) 0.20578(11) 0.59647(10) 0.0253(4) Uani 1 1 d . . . . .
C102 C 0.06284(15) 0.22388(14) 0.64059(11) 0.0329(5) Uani 1 1 d . . . . .
H102 H 0.066312 0.255245 0.675778 0.039 Uiso 1 1 calc R U . . .
C103 C -0.01251(17) 0.19718(16) 0.63433(14) 0.0431(6) Uani 1 1 d . . . . .
H103 H -0.060325 0.211235 0.664370 0.052 Uiso 1 1 calc R U . . .
C104 C -0.01763(19) 0.15022(16) 0.58439(15) 0.0466(7) Uani 1 1 d . . . . .
H104 H -0.069102 0.131806 0.579857 0.056 Uiso 1 1 calc R U . . .
C105 C 0.05237(19) 0.12974(14) 0.54061(14) 0.0427(6) Uani 1 1 d . . . . .
H105 H 0.049021 0.096477 0.506644 0.051 Uiso 1 1 calc R U . . .
C106 C 0.12687(16) 0.15760(12) 0.54633(11) 0.0322(5) Uani 1 1 d . . . . .
H106 H 0.174246 0.143859 0.515796 0.039 Uiso 1 1 calc R U . . .
C4 C 0.01200(13) 0.67308(11) 0.58620(10) 0.0219(4) Uani 1 1 d . . . . .
C5 C -0.06561(14) 0.72784(12) 0.58381(12) 0.0295(5) Uani 1 1 d . . . . .
H5A H -0.057782 0.758673 0.545656 0.044 Uiso 1 1 calc R U . . .
H5B H -0.113748 0.699460 0.582807 0.044 Uiso 1 1 calc R U . . .
H5C H -0.075180 0.760588 0.621427 0.044 Uiso 1 1 calc R U . . .
C6 C 0.08641(14) 0.71864(12) 0.58894(12) 0.0289(5) Uani 1 1 d . . . . .
H6A H 0.093188 0.751148 0.551750 0.043 Uiso 1 1 calc R U . . .
H6B H 0.076466 0.749781 0.627513 0.043 Uiso 1 1 calc R U . . .
H6C H 0.137042 0.684039 0.589319 0.043 Uiso 1 1 calc R U . . .
CL1 Cl 0.19962(5) 0.07493(4) 0.17796(3) 0.04334(15) Uani 1 1 d . . . . .
H12S H 0.106(3) 0.143(2) 0.2274(19) 0.082(12) Uiso 1 1 d . . . . .
CL2 Cl 0.04461(4) 0.15301(3) 0.26535(3) 0.04214(15) Uani 1 1 d . . . . .
CL3A Cl 0.19828(8) 0.57619(6) 0.28103(4) 0.0559(3) Uani 0.893(2) 1 d . . P A 1
CL3B Cl 0.1525(7) 0.5575(5) 0.2713(3) 0.0559(3) Uani 0.107(2) 1 d . . P A 2
CL4 Cl 0.04241(5) 0.65420(4) 0.22930(4) 0.05153(18) Uani 1 1 d . . . . .
H43S H 0.0983(18) 0.6262(16) 0.2436(13) 0.035(7) Uiso 1 1 d . . . . .
C10 C 0.52297(18) 0.13576(15) 0.16954(16) 0.0475(7) Uani 1 1 d . . . . .
H10 H 0.502237 0.184081 0.150334 0.057 Uiso 1 1 calc R U . . .
CL11 Cl 0.57130(5) 0.07577(5) 0.10842(4) 0.05652(19) Uani 1 1 d . . . . .
CL12 Cl 0.59148(6) 0.15639(6) 0.22101(5) 0.0670(2) Uani 1 1 d . . . . .
CL13 Cl 0.43773(7) 0.09678(8) 0.20994(6) 0.1097(5) Uani 1 1 d . . . . .
C20 C 0.2164(2) 0.55101(17) 0.12252(13) 0.0476(7) Uani 1 1 d . . . . .
H20 H 0.194184 0.555963 0.168649 0.057 Uiso 1 1 calc R U . . .
CL21 Cl 0.24933(6) 0.63759(5) 0.09627(4) 0.0670(3) Uani 1 1 d . . . . .
CL22 Cl 0.30052(7) 0.48031(5) 0.11318(5) 0.0793(3) Uani 1 1 d . . . . .
CL23 Cl 0.13660(9) 0.52637(9) 0.08216(6) 0.1026(4) Uani 1 1 d . . . . .
C30 C 0.29139(18) 0.19300(17) 0.07188(14) 0.0437(6) Uani 1 1 d . . . . .
H30 H 0.280439 0.158574 0.108621 0.052 Uiso 1 1 calc R U . . .
CL31 Cl 0.39525(5) 0.17348(5) 0.03689(6) 0.0710(3) Uani 1 1 d . . . . .
CL32 Cl 0.27382(5) 0.28662(5) 0.09943(5) 0.0635(2) Uani 1 1 d . . . . .
CL33 Cl 0.22402(5) 0.17819(5) 0.01755(4) 0.0591(2) Uani 1 1 d . . . . .
C40 C 0.22332(19) 0.04794(16) 0.33143(13) 0.0433(6) Uani 1 1 d . . . . .
H40 H 0.204907 0.053759 0.288722 0.052 Uiso 1 1 calc R U . . .
CL41 Cl 0.14255(6) 0.01595(7) 0.38353(5) 0.0788(3) Uani 1 1 d . . . . .
CL42 Cl 0.24890(5) 0.13482(4) 0.35483(4) 0.0567(2) Uani 1 1 d . . . . .
CL43 Cl 0.31144(7) -0.01860(5) 0.32498(5) 0.0704(3) 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
Si1 O3 1.7068(14) . ?
Si1 O1 1.7307(14) . ?
Si1 O2 1.7604(14) . ?
Si1 O4 1.8089(14) . ?
Si1 C51 1.850(2) . ?
O1 C11 1.350(2) . ?
O2 C12 1.341(2) . ?
O3 C21 1.353(2) . ?
O4 C22 1.332(2) . ?
O5 C46 1.388(2) . ?
O5 C32 1.391(2) . ?
N1 C19 1.303(3) . ?
N1 C31 1.413(2) . ?
N1 H1 0.75(3) . ?
N2 C29 1.311(2) . ?
N2 C41 1.420(2) . ?
N2 H2 0.79(3) . ?
Si2 O8 1.6972(15) . ?
Si2 O6 1.7316(15) . ?
Si2 O7 1.7511(15) . ?
Si2 O9 1.8186(14) . ?
Si2 C101 1.848(2) . ?
O6 C61 1.343(3) . ?
O7 C62 1.343(2) . ?
O8 C71 1.353(2) . ?
O9 C72 1.325(2) . ?
O10 C82 1.388(2) . ?
O10 C96 1.388(2) . ?
N3 C69 1.305(3) . ?
N3 C81 1.412(3) . ?
N3 H3 0.84(3) . ?
N4 C79 1.308(3) . ?
N4 C91 1.416(2) . ?
N4 H4 0.72(3) . ?
C11 C16 1.378(3) . ?
C11 C12 1.386(3) . ?
C12 C13 1.398(3) . ?
C13 C19 1.415(3) . ?
C13 C14 1.433(3) . ?
C14 C15 1.379(3) . ?
C14 C18 1.540(3) . ?
C15 C16 1.413(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.524(3) . ?
C17 C173 1.528(3) . ?
C17 C171 1.532(3) . ?
C17 C172 1.532(3) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C18 C181 1.530(3) . ?
C18 C183 1.536(3) . ?
C18 C182 1.542(3) . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C19 H19 0.92(2) . ?
C21 C26 1.376(3) . ?
C21 C22 1.391(3) . ?
C22 C23 1.404(3) . ?
C23 C29 1.415(3) . ?
C23 C24 1.443(3) . ?
C24 C25 1.379(3) . ?
C24 C28 1.536(3) . ?
C25 C26 1.415(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.523(3) . ?
C27 C272 1.528(3) . ?
C27 C271 1.529(3) . ?
C27 C273 1.536(3) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C28 C281 1.528(3) . ?
C28 C282 1.535(3) . ?
C28 C283 1.536(4) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C29 H29 0.94(2) . ?
C31 C32 1.386(3) . ?
C31 C36 1.387(3) . ?
C32 C33 1.391(3) . ?
C33 C34 1.387(3) . ?
C33 C1 1.508(3) . ?
C34 C35 1.385(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.389(3) . ?
C41 C46 1.390(3) . ?
C42 C43 1.381(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.381(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.389(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(3) . ?
C45 C1 1.517(3) . ?
C51 C56 1.391(3) . ?
C51 C52 1.406(3) . ?
C52 C53 1.382(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.371(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.386(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C1 C3 1.525(3) . ?
C1 C2 1.538(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C61 C66 1.380(3) . ?
C61 C62 1.388(3) . ?
C62 C63 1.393(3) . ?
C63 C69 1.415(3) . ?
C63 C64 1.435(3) . ?
C64 C65 1.383(3) . ?
C64 C68 1.558(3) . ?
C65 C66 1.413(3) . ?
C65 H65 0.9500 . ?
C66 C67 1.529(3) . ?
C67 C673 1.520(4) . ?
C67 C671 1.529(3) . ?
C67 C672 1.535(3) . ?
C671 H67A 0.9800 . ?
C671 H67B 0.9800 . ?
C671 H67C 0.9800 . ?
C672 H67D 0.9800 . ?
C672 H67E 0.9800 . ?
C672 H67F 0.9800 . ?
C673 H67G 0.9800 . ?
C673 H67H 0.9800 . ?
C673 H67I 0.9800 . ?
C68 C683 1.526(5) . ?
C68 C681 1.539(4) . ?
C68 C682 1.541(4) . ?
C681 H68A 0.9800 . ?
C681 H68B 0.9800 . ?
C681 H68C 0.9800 . ?
C682 H68D 0.9800 . ?
C682 H68E 0.9800 . ?
C682 H68F 0.9800 . ?
C683 H68G 0.9800 . ?
C683 H68H 0.9800 . ?
C683 H68I 0.9800 . ?
C69 H69 0.98(3) . ?
C71 C76 1.372(3) . ?
C71 C72 1.398(3) . ?
C72 C73 1.404(3) . ?
C73 C79 1.414(3) . ?
C73 C74 1.443(3) . ?
C74 C75 1.376(3) . ?
C74 C78 1.534(3) . ?
C75 C76 1.412(3) . ?
C75 H75 0.9500 . ?
C76 C77 1.526(3) . ?
C77 C772 1.533(3) . ?
C77 C771 1.534(3) . ?
C77 C773 1.534(4) . ?
C771 H77A 0.9800 . ?
C771 H77B 0.9800 . ?
C771 H77C 0.9800 . ?
C772 H77D 0.9800 . ?
C772 H77E 0.9800 . ?
C772 H77F 0.9800 . ?
C773 H77G 0.9800 . ?
C773 H77H 0.9800 . ?
C773 H77I 0.9800 . ?
C78 C783 1.533(3) . ?
C78 C781 1.537(3) . ?
C78 C782 1.537(3) . ?
C781 H78A 0.9800 . ?
C781 H78B 0.9800 . ?
C781 H78C 0.9800 . ?
C782 H78D 0.9800 . ?
C782 H78E 0.9800 . ?
C782 H78F 0.9800 . ?
C783 H78G 0.9800 . ?
C783 H78H 0.9800 . ?
C783 H78I 0.9800 . ?
C79 H79 0.90(2) . ?
C81 C82 1.389(3) . ?
C81 C86 1.390(3) . ?
C82 C83 1.391(3) . ?
C83 C84 1.384(3) . ?
C83 C4 1.513(3) . ?
C84 C85 1.381(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.379(3) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C91 C92 1.389(3) . ?
C91 C96 1.392(3) . ?
C92 C93 1.379(3) . ?
C92 H92 0.9500 . ?
C93 C94 1.375(3) . ?
C93 H93 0.9500 . ?
C94 C95 1.391(3) . ?
C94 H94 0.9500 . ?
C95 C96 1.391(3) . ?
C95 C4 1.517(3) . ?
C101 C102 1.393(3) . ?
C101 C106 1.399(3) . ?
C102 C103 1.387(4) . ?
C102 H102 0.9500 . ?
C103 C104 1.376(4) . ?
C103 H103 0.9500 . ?
C104 C105 1.388(4) . ?
C104 H104 0.9500 . ?
C105 C106 1.381(4) . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C4 C5 1.524(3) . ?
C4 C6 1.537(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Cl2 H12S 1.20(4) . ?
Cl3B H43S 1.60(3) . ?
Cl4 H43S 1.08(3) . ?
C10 Cl13 1.736(3) . ?
C10 Cl11 1.737(3) . ?
C10 Cl12 1.739(3) . ?
C10 H10 1.0000 . ?
C20 Cl21 1.750(3) . ?
C20 Cl23 1.751(3) . ?
C20 Cl22 1.757(3) . ?
C20 H20 1.0000 . ?
C30 Cl33 1.744(3) . ?
C30 Cl31 1.753(3) . ?
C30 Cl32 1.755(3) . ?
C30 H30 1.0000 . ?
C40 Cl42 1.740(3) . ?
C40 Cl41 1.741(3) . ?
C40 Cl43 1.758(3) . ?
C40 H40 1.0000 . ?

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
O3 Si1 O1 87.60(7) . . ?
O3 Si1 O2 145.83(8) . . ?
O1 Si1 O2 87.73(6) . . ?
O3 Si1 O4 87.00(6) . . ?
O1 Si1 O4 152.61(8) . . ?
O2 Si1 O4 81.85(6) . . ?
O3 Si1 C51 109.21(8) . . ?
O1 Si1 C51 106.50(8) . . ?
O2 Si1 C51 104.58(8) . . ?
O4 Si1 C51 100.64(8) . . ?
C11 O1 Si1 114.08(11) . . ?
C12 O2 Si1 112.93(11) . . ?
C21 O3 Si1 115.43(11) . . ?
C22 O4 Si1 112.35(11) . . ?
C46 O5 C32 115.15(14) . . ?
C19 N1 C31 122.08(17) . . ?
C19 N1 H1 118.9(19) . . ?
C31 N1 H1 118.8(19) . . ?
C29 N2 C41 122.86(17) . . ?
C29 N2 H2 117.5(19) . . ?
C41 N2 H2 119.4(19) . . ?
O8 Si2 O6 87.47(7) . . ?
O8 Si2 O7 142.88(9) . . ?
O6 Si2 O7 87.81(7) . . ?
O8 Si2 O9 87.10(7) . . ?
O6 Si2 O9 155.47(8) . . ?
O7 Si2 O9 82.22(7) . . ?
O8 Si2 C101 110.80(9) . . ?
O6 Si2 C101 105.45(9) . . ?
O7 Si2 C101 105.95(9) . . ?
O9 Si2 C101 98.83(8) . . ?
C61 O6 Si2 114.13(12) . . ?
C62 O7 Si2 112.91(12) . . ?
C71 O8 Si2 115.38(12) . . ?
C72 O9 Si2 111.92(12) . . ?
C82 O10 C96 115.55(15) . . ?
C69 N3 C81 121.59(18) . . ?
C69 N3 H3 118.2(18) . . ?
C81 N3 H3 120.2(18) . . ?
C79 N4 C91 123.11(17) . . ?
C79 N4 H4 119(2) . . ?
C91 N4 H4 118(2) . . ?
O1 C11 C16 127.47(17) . . ?
O1 C11 C12 112.09(16) . . ?
C16 C11 C12 120.43(17) . . ?
O2 C12 C11 113.04(16) . . ?
O2 C12 C13 123.80(16) . . ?
C11 C12 C13 123.16(17) . . ?
C12 C13 C19 118.74(17) . . ?
C12 C13 C14 117.69(16) . . ?
C19 C13 C14 123.42(17) . . ?
C15 C14 C13 116.92(17) . . ?
C15 C14 C18 120.58(17) . . ?
C13 C14 C18 122.48(16) . . ?
C14 C15 C16 125.38(17) . . ?
C14 C15 H15 117.3 . . ?
C16 C15 H15 117.3 . . ?
C11 C16 C15 116.28(17) . . ?
C11 C16 C17 121.02(17) . . ?
C15 C16 C17 122.69(17) . . ?
C16 C17 C173 112.36(16) . . ?
C16 C17 C171 108.59(16) . . ?
C173 C17 C171 108.86(18) . . ?
C16 C17 C172 109.34(16) . . ?
C173 C17 C172 108.11(17) . . ?
C171 C17 C172 109.55(17) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C181 C18 C183 106.75(19) . . ?
C181 C18 C14 111.23(16) . . ?
C183 C18 C14 110.27(17) . . ?
C181 C18 C182 105.68(18) . . ?
C183 C18 C182 110.80(17) . . ?
C14 C18 C182 111.91(16) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
N1 C19 C13 125.34(18) . . ?
N1 C19 H19 113.8(14) . . ?
C13 C19 H19 120.8(14) . . ?
O3 C21 C26 126.81(17) . . ?
O3 C21 C22 112.10(16) . . ?
C26 C21 C22 121.03(17) . . ?
O4 C22 C21 113.01(16) . . ?
O4 C22 C23 124.08(16) . . ?
C21 C22 C23 122.88(17) . . ?
C22 C23 C29 119.22(17) . . ?
C22 C23 C24 117.44(17) . . ?
C29 C23 C24 123.34(17) . . ?
C25 C24 C23 116.91(17) . . ?
C25 C24 C28 120.25(17) . . ?
C23 C24 C28 122.83(17) . . ?
C24 C25 C26 125.76(18) . . ?
C24 C25 H25 117.1 . . ?
C26 C25 H25 117.1 . . ?
C21 C26 C25 115.97(17) . . ?
C21 C26 C27 121.68(17) . . ?
C25 C26 C27 122.32(17) . . ?
C26 C27 C272 110.41(17) . . ?
C26 C27 C271 112.58(17) . . ?
C272 C27 C271 108.42(18) . . ?
C26 C27 C273 108.19(16) . . ?
C272 C27 C273 108.82(18) . . ?
C271 C27 C273 108.34(18) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C281 C28 C282 105.7(2) . . ?
C281 C28 C24 110.55(18) . . ?
C282 C28 C24 111.17(18) . . ?
C281 C28 C283 112.04(19) . . ?
C282 C28 C283 106.2(2) . . ?
C24 C28 C283 110.93(19) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
N2 C29 C23 125.49(17) . . ?
N2 C29 H29 116.7(14) . . ?
C23 C29 H29 117.8(14) . . ?
C32 C31 C36 120.09(17) . . ?
C32 C31 N1 120.12(17) . . ?
C36 C31 N1 119.78(17) . . ?
C31 C32 O5 117.64(16) . . ?
C31 C32 C33 120.55(17) . . ?
O5 C32 C33 121.80(17) . . ?
C34 C33 C32 118.21(18) . . ?
C34 C33 C1 123.90(17) . . ?
C32 C33 C1 117.72(17) . . ?
C35 C34 C33 121.25(18) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C36 C35 C34 119.94(19) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 119.56(19) . . ?
C35 C36 H36 120.2 . . ?
C31 C36 H36 120.2 . . ?
C42 C41 C46 119.77(17) . . ?
C42 C41 N2 119.78(17) . . ?
C46 C41 N2 120.44(17) . . ?
C43 C42 C41 119.64(18) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 120.24(18) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C45 121.05(18) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C44 C45 C46 118.38(18) . . ?
C44 C45 C1 123.13(17) . . ?
C46 C45 C1 118.26(17) . . ?
O5 C46 C45 121.28(17) . . ?
O5 C46 C41 117.86(16) . . ?
C45 C46 C41 120.85(17) . . ?
C56 C51 C52 117.4(2) . . ?
C56 C51 Si1 122.62(17) . . ?
C52 C51 Si1 119.79(16) . . ?
C53 C52 C51 121.2(2) . . ?
C53 C52 H52 119.4 . . ?
C51 C52 H52 119.4 . . ?
C54 C53 C52 120.0(2) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.0(2) . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C54 C55 C56 120.4(2) . . ?
C54 C55 H55 119.8 . . ?
C56 C55 H55 119.8 . . ?
C55 C56 C51 120.9(2) . . ?
C55 C56 H56 119.5 . . ?
C51 C56 H56 119.5 . . ?
C33 C1 C45 107.07(15) . . ?
C33 C1 C3 111.96(17) . . ?
C45 C1 C3 113.05(17) . . ?
C33 C1 C2 107.87(17) . . ?
C45 C1 C2 107.67(17) . . ?
C3 C1 C2 109.01(17) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O6 C61 C66 127.91(19) . . ?
O6 C61 C62 111.99(17) . . ?
C66 C61 C62 120.1(2) . . ?
O7 C62 C61 112.99(18) . . ?
O7 C62 C63 123.57(18) . . ?
C61 C62 C63 123.44(18) . . ?
C62 C63 C69 118.80(18) . . ?
C62 C63 C64 118.02(19) . . ?
C69 C63 C64 123.0(2) . . ?
C65 C64 C63 116.3(2) . . ?
C65 C64 C68 121.32(19) . . ?
C63 C64 C68 122.33(19) . . ?
C64 C65 C66 125.67(19) . . ?
C64 C65 H65 117.2 . . ?
C66 C65 H65 117.2 . . ?
C61 C66 C65 116.34(19) . . ?
C61 C66 C67 120.6(2) . . ?
C65 C66 C67 123.09(18) . . ?
C673 C67 C66 108.9(2) . . ?
C673 C67 C671 109.0(2) . . ?
C66 C67 C671 111.5(2) . . ?
C673 C67 C672 109.9(2) . . ?
C66 C67 C672 109.49(18) . . ?
C671 C67 C672 108.1(2) . . ?
C67 C671 H67A 109.5 . . ?
C67 C671 H67B 109.5 . . ?
H67A C671 H67B 109.5 . . ?
C67 C671 H67C 109.5 . . ?
H67A C671 H67C 109.5 . . ?
H67B C671 H67C 109.5 . . ?
C67 C672 H67D 109.5 . . ?
C67 C672 H67E 109.5 . . ?
H67D C672 H67E 109.5 . . ?
C67 C672 H67F 109.5 . . ?
H67D C672 H67F 109.5 . . ?
H67E C672 H67F 109.5 . . ?
C67 C673 H67G 109.5 . . ?
C67 C673 H67H 109.5 . . ?
H67G C673 H67H 109.5 . . ?
C67 C673 H67I 109.5 . . ?
H67G C673 H67I 109.5 . . ?
H67H C673 H67I 109.5 . . ?
C683 C68 C681 107.5(3) . . ?
C683 C68 C682 111.4(2) . . ?
C681 C68 C682 106.0(3) . . ?
C683 C68 C64 112.5(2) . . ?
C681 C68 C64 110.1(2) . . ?
C682 C68 C64 109.1(2) . . ?
C68 C681 H68A 109.5 . . ?
C68 C681 H68B 109.5 . . ?
H68A C681 H68B 109.5 . . ?
C68 C681 H68C 109.5 . . ?
H68A C681 H68C 109.5 . . ?
H68B C681 H68C 109.5 . . ?
C68 C682 H68D 109.5 . . ?
C68 C682 H68E 109.5 . . ?
H68D C682 H68E 109.5 . . ?
C68 C682 H68F 109.5 . . ?
H68D C682 H68F 109.5 . . ?
H68E C682 H68F 109.5 . . ?
C68 C683 H68G 109.5 . . ?
C68 C683 H68H 109.5 . . ?
H68G C683 H68H 109.5 . . ?
C68 C683 H68I 109.5 . . ?
H68G C683 H68I 109.5 . . ?
H68H C683 H68I 109.5 . . ?
N3 C69 C63 125.4(2) . . ?
N3 C69 H69 115.5(14) . . ?
C63 C69 H69 119.1(14) . . ?
O8 C71 C76 126.57(18) . . ?
O8 C71 C72 112.06(17) . . ?
C76 C71 C72 121.25(18) . . ?
O9 C72 C71 112.99(17) . . ?
O9 C72 C73 124.68(17) . . ?
C71 C72 C73 122.28(18) . . ?
C72 C73 C79 118.79(18) . . ?
C72 C73 C74 117.54(17) . . ?
C79 C73 C74 123.65(18) . . ?
C75 C74 C73 116.91(18) . . ?
C75 C74 C78 120.43(18) . . ?
C73 C74 C78 122.63(18) . . ?
C74 C75 C76 125.86(19) . . ?
C74 C75 H75 117.1 . . ?
C76 C75 H75 117.1 . . ?
C71 C76 C75 115.90(18) . . ?
C71 C76 C77 121.03(19) . . ?
C75 C76 C77 123.07(19) . . ?
C76 C77 C772 112.04(19) . . ?
C76 C77 C771 110.31(18) . . ?
C772 C77 C771 108.2(2) . . ?
C76 C77 C773 108.02(19) . . ?
C772 C77 C773 108.7(2) . . ?
C771 C77 C773 109.5(2) . . ?
C77 C771 H77A 109.5 . . ?
C77 C771 H77B 109.5 . . ?
H77A C771 H77B 109.5 . . ?
C77 C771 H77C 109.5 . . ?
H77A C771 H77C 109.5 . . ?
H77B C771 H77C 109.5 . . ?
C77 C772 H77D 109.5 . . ?
C77 C772 H77E 109.5 . . ?
H77D C772 H77E 109.5 . . ?
C77 C772 H77F 109.5 . . ?
H77D C772 H77F 109.5 . . ?
H77E C772 H77F 109.5 . . ?
C77 C773 H77G 109.5 . . ?
C77 C773 H77H 109.5 . . ?
H77G C773 H77H 109.5 . . ?
C77 C773 H77I 109.5 . . ?
H77G C773 H77I 109.5 . . ?
H77H C773 H77I 109.5 . . ?
C783 C78 C74 111.42(18) . . ?
C783 C78 C781 106.94(19) . . ?
C74 C78 C781 111.49(18) . . ?
C783 C78 C782 111.33(19) . . ?
C74 C78 C782 110.45(17) . . ?
C781 C78 C782 104.98(19) . . ?
C78 C781 H78A 109.5 . . ?
C78 C781 H78B 109.5 . . ?
H78A C781 H78B 109.5 . . ?
C78 C781 H78C 109.5 . . ?
H78A C781 H78C 109.5 . . ?
H78B C781 H78C 109.5 . . ?
C78 C782 H78D 109.5 . . ?
C78 C782 H78E 109.5 . . ?
H78D C782 H78E 109.5 . . ?
C78 C782 H78F 109.5 . . ?
H78D C782 H78F 109.5 . . ?
H78E C782 H78F 109.5 . . ?
C78 C783 H78G 109.5 . . ?
C78 C783 H78H 109.5 . . ?
H78G C783 H78H 109.5 . . ?
C78 C783 H78I 109.5 . . ?
H78G C783 H78I 109.5 . . ?
H78H C783 H78I 109.5 . . ?
N4 C79 C73 125.70(18) . . ?
N4 C79 H79 117.0(15) . . ?
C73 C79 H79 117.3(15) . . ?
C82 C81 C86 119.97(18) . . ?
C82 C81 N3 120.55(18) . . ?
C86 C81 N3 119.47(18) . . ?
O10 C82 C81 117.77(17) . . ?
O10 C82 C83 122.04(18) . . ?
C81 C82 C83 120.16(19) . . ?
C84 C83 C82 118.52(19) . . ?
C84 C83 C4 122.89(18) . . ?
C82 C83 C4 118.45(18) . . ?
C85 C84 C83 121.55(19) . . ?
C85 C84 H84 119.2 . . ?
C83 C84 H84 119.2 . . ?
C86 C85 C84 119.6(2) . . ?
C86 C85 H85 120.2 . . ?
C84 C85 H85 120.2 . . ?
C85 C86 C81 119.8(2) . . ?
C85 C86 H86 120.1 . . ?
C81 C86 H86 120.1 . . ?
C92 C91 C96 119.58(17) . . ?
C92 C91 N4 119.76(18) . . ?
C96 C91 N4 120.66(17) . . ?
C93 C92 C91 119.81(19) . . ?
C93 C92 H92 120.1 . . ?
C91 C92 H92 120.1 . . ?
C94 C93 C92 120.31(18) . . ?
C94 C93 H93 119.8 . . ?
C92 C93 H93 119.8 . . ?
C93 C94 C95 121.14(18) . . ?
C93 C94 H94 119.4 . . ?
C95 C94 H94 119.4 . . ?
C94 C95 C96 118.29(19) . . ?
C94 C95 C4 122.67(17) . . ?
C96 C95 C4 118.82(17) . . ?
O10 C96 C95 121.54(18) . . ?
O10 C96 C91 117.66(16) . . ?
C95 C96 C91 120.78(17) . . ?
C102 C101 C106 117.7(2) . . ?
C102 C101 Si2 119.87(18) . . ?
C106 C101 Si2 122.25(18) . . ?
C103 C102 C101 121.5(2) . . ?
C103 C102 H102 119.2 . . ?
C101 C102 H102 119.2 . . ?
C104 C103 C102 119.7(3) . . ?
C104 C103 H103 120.2 . . ?
C102 C103 H103 120.2 . . ?
C103 C104 C105 120.0(3) . . ?
C103 C104 H104 120.0 . . ?
C105 C104 H104 120.0 . . ?
C106 C105 C104 120.1(3) . . ?
C106 C105 H105 119.9 . . ?
C104 C105 H105 119.9 . . ?
C105 C106 C101 120.9(2) . . ?
C105 C106 H106 119.5 . . ?
C101 C106 H106 119.5 . . ?
C83 C4 C95 107.72(15) . . ?
C83 C4 C5 111.95(18) . . ?
C95 C4 C5 112.84(17) . . ?
C83 C4 C6 107.84(17) . . ?
C95 C4 C6 107.62(17) . . ?
C5 C4 C6 108.67(17) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Cl13 C10 Cl11 109.91(15) . . ?
Cl13 C10 Cl12 111.0(2) . . ?
Cl11 C10 Cl12 111.94(16) . . ?
Cl13 C10 H10 108.0 . . ?
Cl11 C10 H10 108.0 . . ?
Cl12 C10 H10 108.0 . . ?
Cl21 C20 Cl23 110.98(17) . . ?
Cl21 C20 Cl22 110.37(18) . . ?
Cl23 C20 Cl22 110.52(17) . . ?
Cl21 C20 H20 108.3 . . ?
Cl23 C20 H20 108.3 . . ?
Cl22 C20 H20 108.3 . . ?
Cl33 C30 Cl31 110.50(17) . . ?
Cl33 C30 Cl32 109.93(17) . . ?
Cl31 C30 Cl32 109.79(15) . . ?
Cl33 C30 H30 108.9 . . ?
Cl31 C30 H30 108.9 . . ?
Cl32 C30 H30 108.9 . . ?
Cl42 C40 Cl41 111.98(17) . . ?
Cl42 C40 Cl43 109.91(16) . . ?
Cl41 C40 Cl43 110.08(15) . . ?
Cl42 C40 H40 108.3 . . ?
Cl41 C40 H40 108.3 . . ?
Cl43 C40 H40 108.3 . . ?

_refine_diff_density_max         1.127
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.065



####################################################################### 
# 
# 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_siag
_database_code_depnum_ccdc_archive 'CCDC 1922355'
loop_
_audit_author_name
_audit_author_address
'Allen G. Oliver'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'Silver((9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dioxybenzaldimine)(phenyl)silicate) tris(deuteriodichloromethane) solvate'
_chemical_name_common            'Ag[(Xbic)SiPh] . 3 CD2Cl2'
_chemical_melting_point          .
_chemical_formula_moiety         'C51 H57 Ag N2 O5 Si, 3(C D2 Cl2)'
_chemical_formula_sum            'C54 H57 Ag Cl6 D6 N2 O5 Si'
_chemical_formula_weight         1174.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.9942(18)
_cell_length_b                   19.485(2)
_cell_length_c                   17.562(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.0777(16)
_cell_angle_gamma                90
_cell_volume                     5469.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9694
_cell_measurement_theta_min      2.391
_cell_measurement_theta_max      29.047

_exptl_crystal_description       block
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   0.6804
_exptl_transmission_factor_max   0.7279
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.208
_exptl_absorpt_coefficient_mu    0.731
_shelx_estimated_absorpt_T_min   0.804
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_T_max  0.7279
_exptl_absorpt_process_details   
;
Blessing, R.H. (1995)Acta Cryst. A51, 33-38.

Shledrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc.
Madison, WI USA.
;
_exptl_crystal_recrystallization_method 
'Crystals deposited from the reaction mixture of [(XbicH2)SiPh][HCl2]with excess Ag2O in CD2Cl2.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            154871
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.274
_diffrn_reflns_theta_max         29.145
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14700
_reflns_number_gt                13067
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
One dichloromethane of crystallization was found to be positionally disordered
with the two chlorine atoms oscillating. The chlorines were constrained to 
have the same thermal parameters using EADP. The molecule was modeled with the 
chlorine atoms refined with occupancies summed to unity yielding an 
approximately 0.71:0.39 ratio.

The hydrogen atoms on the dichloromethanes were placed in calculated
positions. The hydrogens on the tert-butyl carbons and methyl carbons
were also placed in calculated positions. All other hydrogens were found
on the difference map and refined isotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0844P)²+20.8558P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14700
_refine_ls_number_parameters     691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1702
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.32747(5) 0.14141(4) 0.41765(5) 0.01469(16) Uani 1 1 d . . . . .
Ag Ag 0.15859(2) 0.03637(2) 0.43024(2) 0.01652(8) Uani 1 1 d . . . . .
O1 O 0.33236(14) 0.23024(11) 0.42613(13) 0.0179(4) Uani 1 1 d . . . . .
O2 O 0.21862(14) 0.14913(11) 0.42344(14) 0.0181(4) Uani 1 1 d . . . . .
O3 O 0.40026(14) 0.14492(12) 0.34813(13) 0.0182(4) Uani 1 1 d . . . . .
O4 O 0.29890(14) 0.05885(12) 0.38097(13) 0.0180(4) Uani 1 1 d . . . . .
O5 O 0.02865(14) -0.00464(11) 0.34867(12) 0.0156(4) Uani 1 1 d . . . . .
N1 N 0.04506(16) 0.11536(13) 0.42788(14) 0.0151(5) Uani 1 1 d . . . . .
N2 N 0.18767(17) -0.04600(13) 0.33356(15) 0.0158(5) Uani 1 1 d . . . . .
C11 C 0.25676(19) 0.26099(16) 0.43015(17) 0.0155(5) Uani 1 1 d . . . . .
C12 C 0.19035(19) 0.21391(15) 0.42946(17) 0.0155(5) Uani 1 1 d . . . . .
C13 C 0.10584(19) 0.23257(15) 0.42988(17) 0.0154(5) Uani 1 1 d . . . . .
C14 C 0.0886(2) 0.30539(15) 0.43281(17) 0.0161(5) Uani 1 1 d . . . . .
C15 C 0.1563(2) 0.34986(16) 0.43428(17) 0.0166(6) Uani 1 1 d . . . . .
H15 H 0.146(3) 0.394(3) 0.435(3) 0.025(11) Uiso 1 1 d . . . . .
C16 C 0.2411(2) 0.33068(15) 0.43192(16) 0.0159(5) Uani 1 1 d . . . . .
C17 C 0.3118(2) 0.38310(16) 0.42777(18) 0.0182(6) Uani 1 1 d . . . . .
C171 C 0.3567(2) 0.37237(19) 0.35264(19) 0.0245(7) Uani 1 1 d . . . . .
H17A H 0.4023 0.4057 0.3493 0.037 Uiso 1 1 calc R U . . .
H17B H 0.3168 0.3788 0.3095 0.037 Uiso 1 1 calc R U . . .
H17C H 0.3797 0.3258 0.3513 0.037 Uiso 1 1 calc R U . . .
C172 C 0.2791(2) 0.45705(17) 0.4290(2) 0.0260(7) Uani 1 1 d . . . . .
H17D H 0.3262 0.4890 0.4263 0.039 Uiso 1 1 calc R U . . .
H17E H 0.2499 0.4650 0.4763 0.039 Uiso 1 1 calc R U . . .
H17F H 0.2404 0.4645 0.3853 0.039 Uiso 1 1 calc R U . . .
C173 C 0.3732(2) 0.37312(18) 0.4963(2) 0.0231(6) Uani 1 1 d . . . . .
H17G H 0.4186 0.4067 0.4937 0.035 Uiso 1 1 calc R U . . .
H17H H 0.3966 0.3266 0.4951 0.035 Uiso 1 1 calc R U . . .
H17I H 0.3437 0.3796 0.5436 0.035 Uiso 1 1 calc R U . . .
C18 C -0.0007(2) 0.33627(16) 0.43193(18) 0.0182(6) Uani 1 1 d . . . . .
C181 C 0.0006(2) 0.41511(18) 0.4391(2) 0.0277(7) Uani 1 1 d . . . . .
H18A H 0.0311 0.4348 0.3969 0.042 Uiso 1 1 calc R U . . .
H18B H 0.0283 0.4281 0.4876 0.042 Uiso 1 1 calc R U . . .
H18C H -0.0570 0.4325 0.4373 0.042 Uiso 1 1 calc R U . . .
C182 C -0.0470(2) 0.32065(19) 0.3554(2) 0.0251(7) Uani 1 1 d . . . . .
H18D H -0.0137 0.3372 0.3135 0.038 Uiso 1 1 calc R U . . .
H18E H -0.1014 0.3438 0.3538 0.038 Uiso 1 1 calc R U . . .
H18F H -0.0554 0.2710 0.3504 0.038 Uiso 1 1 calc R U . . .
C183 C -0.0497(2) 0.31156(19) 0.5005(2) 0.0241(7) Uani 1 1 d . . . . .
H18G H -0.0532 0.2614 0.4999 0.036 Uiso 1 1 calc R U . . .
H18H H -0.1063 0.3310 0.4976 0.036 Uiso 1 1 calc R U . . .
H18I H -0.0210 0.3266 0.5478 0.036 Uiso 1 1 calc R U . . .
C19 C 0.03885(19) 0.18175(16) 0.42565(17) 0.0158(5) Uani 1 1 d . . . . .
H19 H -0.012(3) 0.199(2) 0.413(2) 0.016(10) Uiso 1 1 d . . . . .
C21 C 0.39877(19) 0.09044(15) 0.29952(17) 0.0156(5) Uani 1 1 d . . . . .
C22 C 0.33743(19) 0.04225(15) 0.31714(17) 0.0152(5) Uani 1 1 d . . . . .
C23 C 0.31754(18) -0.01421(15) 0.27126(17) 0.0148(5) Uani 1 1 d . . . . .
C24 C 0.36711(19) -0.02399(16) 0.20478(17) 0.0152(5) Uani 1 1 d . . . . .
C25 C 0.4298(2) 0.02364(17) 0.19191(18) 0.0170(5) Uani 1 1 d . . . . .
H25 H 0.461(3) 0.020(2) 0.150(3) 0.028(12) Uiso 1 1 d . . . . .
C26 C 0.44788(19) 0.08178(16) 0.23713(17) 0.0169(5) Uani 1 1 d . . . . .
C27 C 0.5161(2) 0.13361(17) 0.21841(19) 0.0206(6) Uani 1 1 d . . . . .
C271 C 0.4753(3) 0.20262(19) 0.1992(2) 0.0295(8) Uani 1 1 d . . . . .
H27A H 0.5186 0.2361 0.1871 0.044 Uiso 1 1 calc R U . . .
H27B H 0.4445 0.2189 0.2430 0.044 Uiso 1 1 calc R U . . .
H27C H 0.4365 0.1972 0.1551 0.044 Uiso 1 1 calc R U . . .
C272 C 0.5773(2) 0.1422(2) 0.2871(2) 0.0288(7) Uani 1 1 d . . . . .
H27D H 0.6035 0.0979 0.2994 0.043 Uiso 1 1 calc R U . . .
H27E H 0.5469 0.1586 0.3310 0.043 Uiso 1 1 calc R U . . .
H27F H 0.6206 0.1756 0.2747 0.043 Uiso 1 1 calc R U . . .
C273 C 0.5667(3) 0.1110(2) 0.1500(2) 0.0323(8) Uani 1 1 d . . . . .
H27G H 0.5934 0.0667 0.1613 0.048 Uiso 1 1 calc R U . . .
H27H H 0.6097 0.1454 0.1403 0.048 Uiso 1 1 calc R U . . .
H27I H 0.5292 0.1064 0.1049 0.048 Uiso 1 1 calc R U . . .
C28 C 0.3516(2) -0.08296(17) 0.14779(18) 0.0184(6) Uani 1 1 d . . . . .
C281 C 0.4102(2) -0.0788(2) 0.0803(2) 0.0263(7) Uani 1 1 d . . . . .
H28A H 0.3984 -0.1171 0.0453 0.040 Uiso 1 1 calc R U . . .
H28B H 0.4685 -0.0813 0.0993 0.040 Uiso 1 1 calc R U . . .
H28C H 0.4009 -0.0353 0.0533 0.040 Uiso 1 1 calc R U . . .
C282 C 0.2619(2) -0.0794(2) 0.1117(2) 0.0257(7) Uani 1 1 d . . . . .
H28D H 0.2535 -0.1174 0.0756 0.038 Uiso 1 1 calc R U . . .
H28E H 0.2543 -0.0357 0.0847 0.038 Uiso 1 1 calc R U . . .
H28F H 0.2211 -0.0829 0.1518 0.038 Uiso 1 1 calc R U . . .
C283 C 0.3699(3) -0.15312(18) 0.1858(2) 0.0285(7) Uani 1 1 d . . . . .
H28G H 0.3596 -0.1899 0.1485 0.043 Uiso 1 1 calc R U . . .
H28H H 0.3333 -0.1594 0.2288 0.043 Uiso 1 1 calc R U . . .
H28I H 0.4285 -0.1546 0.2041 0.043 Uiso 1 1 calc R U . . .
C29 C 0.2467(2) -0.05824(16) 0.28678(17) 0.0159(5) Uani 1 1 d . . . . .
H29 H 0.242(3) -0.097(2) 0.259(3) 0.026(11) Uiso 1 1 d . . . . .
C31 C -0.03219(19) 0.07869(15) 0.42844(17) 0.0152(5) Uani 1 1 d . . . . .
C32 C -0.10007(19) 0.10044(16) 0.46998(17) 0.0172(6) Uani 1 1 d . . . . .
H32 H -0.098(3) 0.142(2) 0.501(2) 0.018(10) Uiso 1 1 d . . . . .
C33 C -0.1734(2) 0.06187(17) 0.47032(18) 0.0187(6) Uani 1 1 d . . . . .
H33 H -0.221(3) 0.080(2) 0.494(3) 0.025(11) Uiso 1 1 d . . . . .
C34 C -0.17919(19) -0.00056(17) 0.43086(17) 0.0178(6) Uani 1 1 d . . . . .
H34 H -0.227(3) -0.023(2) 0.429(2) 0.009(8) Uiso 1 1 d . . . . .
C35 C -0.1109(2) -0.02489(16) 0.39060(17) 0.0167(5) Uani 1 1 d . . . . .
C36 C -0.03930(19) 0.01566(16) 0.38984(16) 0.0150(5) Uani 1 1 d . . . . .
C41 C 0.12432(19) -0.09677(16) 0.33645(16) 0.0155(5) Uani 1 1 d . . . . .
C42 C 0.0413(2) -0.07525(15) 0.34376(16) 0.0154(5) Uani 1 1 d . . . . .
C43 C -0.0254(2) -0.12026(16) 0.34564(17) 0.0178(6) Uani 1 1 d . . . . .
C44 C -0.0078(2) -0.19042(17) 0.34490(19) 0.0217(6) Uani 1 1 d . . . . .
H44 H -0.058(3) -0.222(2) 0.347(2) 0.015(9) Uiso 1 1 d . . . . .
C45 C 0.0740(2) -0.21330(17) 0.34051(19) 0.0221(6) Uani 1 1 d . . . . .
H45 H 0.089(3) -0.258(2) 0.343(3) 0.025(11) Uiso 1 1 d . . . . .
C46 C 0.1397(2) -0.16718(16) 0.33567(18) 0.0188(6) Uani 1 1 d . . . . .
H46 H 0.196(2) -0.183(2) 0.338(2) 0.010(8) Uiso 1 1 d . . . . .
C51 C 0.37489(19) 0.11235(16) 0.51122(17) 0.0164(5) Uani 1 1 d . . . . .
C52 C 0.3826(2) 0.15595(18) 0.57444(19) 0.0209(6) Uani 1 1 d . . . . .
H52 H 0.365(3) 0.202(3) 0.567(3) 0.026(11) Uiso 1 1 d . . . . .
C53 C 0.4133(2) 0.1323(2) 0.6446(2) 0.0258(7) Uani 1 1 d . . . . .
H53 H 0.416(3) 0.164(3) 0.684(3) 0.034(13) Uiso 1 1 d . . . . .
C54 C 0.4387(2) 0.0645(2) 0.6534(2) 0.0285(7) Uani 1 1 d . . . . .
H54 H 0.455(4) 0.051(3) 0.710(4) 0.061(19) Uiso 1 1 d . . . . .
C55 C 0.4336(2) 0.0206(2) 0.5913(2) 0.0274(7) Uani 1 1 d . . . . .
H55 H 0.453(3) -0.027(3) 0.595(3) 0.031(13) Uiso 1 1 d . . . . .
C56 C 0.4014(2) 0.04408(18) 0.5212(2) 0.0222(6) Uani 1 1 d . . . . .
H56 H 0.397(3) 0.009(2) 0.477(2) 0.016(9) Uiso 1 1 d . . . . .
C1 C -0.1135(2) -0.09026(18) 0.34329(18) 0.0195(6) Uani 1 1 d . . . . .
C2 C -0.1783(2) -0.1411(2) 0.3708(2) 0.0301(8) Uani 1 1 d . . . . .
H2A H -0.2336 -0.1195 0.3688 0.045 Uiso 1 1 calc R U . . .
H2B H -0.1637 -0.1548 0.4233 0.045 Uiso 1 1 calc R U . . .
H2C H -0.1792 -0.1817 0.3378 0.045 Uiso 1 1 calc R U . . .
C3 C -0.1368(2) -0.0700(2) 0.2598(2) 0.0281(7) Uani 1 1 d . . . . .
H3A H -0.0966 -0.0361 0.2421 0.042 Uiso 1 1 calc R U . . .
H3B H -0.1931 -0.0502 0.2572 0.042 Uiso 1 1 calc R U . . .
H3C H -0.1353 -0.1108 0.2273 0.042 Uiso 1 1 calc R U . . .
C4 C 0.6097(6) 0.2022(4) 0.5170(4) 0.085(3) Uani 1 1 d . . . . .
D4A D 0.5643 0.2316 0.5356 0.102 Uiso 1 1 calc R U . . .
D4B D 0.5928 0.1855 0.4654 0.102 Uiso 1 1 calc R U . . .
Cl1 Cl 0.62573(9) 0.13298(8) 0.57792(10) 0.0602(4) Uani 1 1 d . . . . .
Cl2 Cl 0.70514(18) 0.25118(12) 0.51280(16) 0.1096(9) Uani 1 1 d . . . . .
C5 C 0.1885(8) 0.6158(6) 0.2309(6) 0.122(4) Uani 1 1 d . . . . .
D5A D 0.1340 0.5974 0.2116 0.146 Uiso 1 1 calc R U . . .
D5B D 0.2329 0.5848 0.2134 0.146 Uiso 1 1 calc R U . . .
Cl3 Cl 0.20323(14) 0.69708(12) 0.19222(18) 0.1004(8) Uani 1 1 d . . . . .
Cl4 Cl 0.1903(2) 0.61620(15) 0.32801(19) 0.1283(12) Uani 1 1 d . . . . .
C6 C 0.1427(5) 0.3860(4) 0.7399(4) 0.0654(17) Uani 1 1 d . . . . .
D6A D 0.1639 0.4338 0.7410 0.078 Uiso 0.705(4) 1 calc R U P A 1
D6B D 0.1422 0.3695 0.7932 0.078 Uiso 0.705(4) 1 calc R U P A 1
D6C D 0.0947 0.3698 0.7691 0.078 Uiso 0.295(4) 1 calc R U P A 2
D6D D 0.1710 0.4225 0.7704 0.078 Uiso 0.295(4) 1 calc R U P A 2
Cl5A Cl 0.2076(4) 0.3382(4) 0.6925(6) 0.228(5) Uani 0.705(4) 1 d . . P A 1
Cl6A Cl 0.0385(2) 0.38641(16) 0.7017(2) 0.1014(13) Uani 0.705(4) 1 d . . P A 1
Cl5B Cl 0.1055(7) 0.4207(9) 0.6593(12) 0.228(5) Uani 0.295(4) 1 d . . P A 2
Cl6B Cl 0.2130(8) 0.3173(6) 0.7312(6) 0.1014(13) Uani 0.295(4) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si O3 1.719(2) . ?
Si O1 1.739(2) . ?
Si O2 1.754(2) . ?
Si O4 1.786(2) . ?
Si C51 1.872(3) . ?
Ag N1 2.379(3) . ?
Ag N2 2.394(3) . ?
Ag O2 2.402(2) . ?
Ag O4 2.473(2) . ?
Ag C34 2.547(3) 3_556 ?
Ag C33 2.596(3) 3_556 ?
Ag O5 2.606(2) . ?
O1 C11 1.353(4) . ?
O2 C12 1.346(4) . ?
O3 C21 1.362(4) . ?
O4 C22 1.338(4) . ?
O5 C36 1.385(3) . ?
O5 C42 1.394(4) . ?
N1 C19 1.298(4) . ?
N1 C31 1.428(4) . ?
N2 C29 1.297(4) . ?
N2 C41 1.418(4) . ?
C11 C16 1.381(4) . ?
C11 C12 1.403(4) . ?
C12 C13 1.400(4) . ?
C13 C14 1.447(4) . ?
C13 C19 1.459(4) . ?
C14 C15 1.386(4) . ?
C14 C18 1.549(4) . ?
C15 C16 1.409(4) . ?
C15 H15 0.87(5) . ?
C16 C17 1.527(4) . ?
C17 C172 1.533(5) . ?
C17 C173 1.538(5) . ?
C17 C171 1.540(5) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C18 C183 1.538(4) . ?
C18 C182 1.541(5) . ?
C18 C181 1.541(5) . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C19 H19 0.90(4) . ?
C21 C26 1.381(4) . ?
C21 C22 1.401(4) . ?
C22 C23 1.394(4) . ?
C23 C24 1.447(4) . ?
C23 C29 1.454(4) . ?
C24 C25 1.391(4) . ?
C24 C28 1.538(4) . ?
C25 C26 1.407(4) . ?
C25 H25 0.91(5) . ?
C26 C27 1.531(4) . ?
C27 C271 1.527(5) . ?
C27 C272 1.535(5) . ?
C27 C273 1.537(5) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C28 C281 1.540(4) . ?
C28 C283 1.545(5) . ?
C28 C282 1.549(5) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C29 H29 0.91(5) . ?
C31 C32 1.396(4) . ?
C31 C36 1.405(4) . ?
C32 C33 1.394(4) . ?
C32 H32 0.97(4) . ?
C33 C34 1.401(5) . ?
C33 Ag 2.596(3) 3_556 ?
C33 H33 0.95(5) . ?
C34 C35 1.405(4) . ?
C34 Ag 2.547(3) 3_556 ?
C34 H34 0.88(4) . ?
C35 C36 1.392(4) . ?
C35 C1 1.520(4) . ?
C41 C46 1.394(4) . ?
C41 C42 1.403(4) . ?
C42 C43 1.383(4) . ?
C43 C44 1.396(5) . ?
C43 C1 1.523(5) . ?
C44 C45 1.387(5) . ?
C44 H44 1.01(4) . ?
C45 C46 1.388(5) . ?
C45 H45 0.91(5) . ?
C46 H46 0.95(4) . ?
C51 C52 1.400(4) . ?
C51 C56 1.405(4) . ?
C52 C53 1.388(5) . ?
C52 H52 0.95(5) . ?
C53 C54 1.389(5) . ?
C53 H53 0.93(5) . ?
C54 C55 1.386(6) . ?
C54 H54 1.04(7) . ?
C55 C56 1.395(5) . ?
C55 H55 0.99(5) . ?
C56 H56 1.02(4) . ?
C1 C2 1.525(5) . ?
C1 C3 1.552(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 Cl1 1.735(7) . ?
C4 Cl2 1.805(10) . ?
C4 D4A 0.9900 . ?
C4 D4B 0.9900 . ?
C5 Cl4 1.705(11) . ?
C5 Cl3 1.742(11) . ?
C5 D5A 0.9900 . ?
C5 D5B 0.9900 . ?
C6 Cl5A 1.645(8) . ?
C6 Cl5B 1.66(3) . ?
C6 Cl6B 1.759(13) . ?
C6 Cl6A 1.773(7) . ?
C6 D6A 0.9900 . ?
C6 D6B 0.9900 . ?
C6 D6C 0.9900 . ?
C6 D6D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Si O1 89.53(11) . . ?
O3 Si O2 137.48(12) . . ?
O1 Si O2 87.20(11) . . ?
O3 Si O4 87.17(11) . . ?
O1 Si O4 159.64(12) . . ?
O2 Si O4 81.76(11) . . ?
O3 Si C51 111.86(13) . . ?
O1 Si C51 102.14(13) . . ?
O2 Si C51 110.26(13) . . ?
O4 Si C51 97.72(13) . . ?
N1 Ag N2 126.09(9) . . ?
N1 Ag O2 73.36(8) . . ?
N2 Ag O2 119.31(8) . . ?
N1 Ag O4 125.51(8) . . ?
N2 Ag O4 70.65(8) . . ?
O2 Ag O4 56.73(7) . . ?
N1 Ag C34 105.43(9) . 3_556 ?
N2 Ag C34 118.28(10) . 3_556 ?
O2 Ag C34 105.07(9) . 3_556 ?
O4 Ag C34 107.22(9) . 3_556 ?
N1 Ag C33 122.66(9) . 3_556 ?
N2 Ag C33 88.13(10) . 3_556 ?
O2 Ag C33 132.90(9) . 3_556 ?
O4 Ag C33 107.69(9) . 3_556 ?
C34 Ag C33 31.60(10) 3_556 3_556 ?
N1 Ag O5 66.17(8) . . ?
N2 Ag O5 64.93(8) . . ?
O2 Ag O5 124.42(7) . . ?
O4 Ag O5 125.28(7) . . ?
C34 Ag O5 121.01(8) 3_556 . ?
C33 Ag O5 101.26(9) 3_556 . ?
C11 O1 Si 114.06(19) . . ?
C12 O2 Si 114.96(19) . . ?
C12 O2 Ag 135.86(19) . . ?
Si O2 Ag 108.88(11) . . ?
C21 O3 Si 114.67(19) . . ?
C22 O4 Si 113.59(19) . . ?
C22 O4 Ag 134.54(19) . . ?
Si O4 Ag 104.88(10) . . ?
C36 O5 C42 115.6(2) . . ?
C36 O5 Ag 104.53(17) . . ?
C42 O5 Ag 102.84(17) . . ?
C19 N1 C31 115.7(3) . . ?
C19 N1 Ag 134.6(2) . . ?
C31 N1 Ag 109.65(18) . . ?
C29 N2 C41 115.6(3) . . ?
C29 N2 Ag 137.5(2) . . ?
C41 N2 Ag 106.54(18) . . ?
O1 C11 C16 126.8(3) . . ?
O1 C11 C12 112.8(3) . . ?
C16 C11 C12 120.3(3) . . ?
O2 C12 C13 124.8(3) . . ?
O2 C12 C11 110.9(3) . . ?
C13 C12 C11 124.1(3) . . ?
C12 C13 C14 116.1(3) . . ?
C12 C13 C19 122.1(3) . . ?
C14 C13 C19 121.8(3) . . ?
C15 C14 C13 117.7(3) . . ?
C15 C14 C18 118.4(3) . . ?
C13 C14 C18 123.9(3) . . ?
C14 C15 C16 125.8(3) . . ?
C14 C15 H15 117(3) . . ?
C16 C15 H15 117(3) . . ?
C11 C16 C15 115.9(3) . . ?
C11 C16 C17 121.4(3) . . ?
C15 C16 C17 122.6(3) . . ?
C16 C17 C172 112.0(3) . . ?
C16 C17 C173 109.3(3) . . ?
C172 C17 C173 108.4(3) . . ?
C16 C17 C171 108.6(3) . . ?
C172 C17 C171 108.0(3) . . ?
C173 C17 C171 110.4(3) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C183 C18 C182 112.2(3) . . ?
C183 C18 C181 104.7(3) . . ?
C182 C18 C181 105.8(3) . . ?
C183 C18 C14 111.5(3) . . ?
C182 C18 C14 110.2(3) . . ?
C181 C18 C14 112.2(3) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
N1 C19 C13 128.3(3) . . ?
N1 C19 H19 117(3) . . ?
C13 C19 H19 114(3) . . ?
O3 C21 C26 126.5(3) . . ?
O3 C21 C22 112.4(3) . . ?
C26 C21 C22 121.1(3) . . ?
O4 C22 C23 124.9(3) . . ?
O4 C22 C21 111.7(3) . . ?
C23 C22 C21 123.3(3) . . ?
C22 C23 C24 116.7(3) . . ?
C22 C23 C29 121.4(3) . . ?
C24 C23 C29 121.8(3) . . ?
C25 C24 C23 117.5(3) . . ?
C25 C24 C28 119.6(3) . . ?
C23 C24 C28 122.9(3) . . ?
C24 C25 C26 125.5(3) . . ?
C24 C25 H25 120(3) . . ?
C26 C25 H25 115(3) . . ?
C21 C26 C25 115.8(3) . . ?
C21 C26 C27 121.3(3) . . ?
C25 C26 C27 122.9(3) . . ?
C271 C27 C26 109.0(3) . . ?
C271 C27 C272 109.5(3) . . ?
C26 C27 C272 110.0(3) . . ?
C271 C27 C273 108.2(3) . . ?
C26 C27 C273 112.2(3) . . ?
C272 C27 C273 107.8(3) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C24 C28 C281 111.9(3) . . ?
C24 C28 C283 110.9(3) . . ?
C281 C28 C283 105.5(3) . . ?
C24 C28 C282 111.0(3) . . ?
C281 C28 C282 105.2(3) . . ?
C283 C28 C282 112.0(3) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
N2 C29 C23 126.9(3) . . ?
N2 C29 H29 117(3) . . ?
C23 C29 H29 116(3) . . ?
C32 C31 C36 117.8(3) . . ?
C32 C31 N1 122.8(3) . . ?
C36 C31 N1 119.3(3) . . ?
C33 C32 C31 120.6(3) . . ?
C33 C32 H32 117(3) . . ?
C31 C32 H32 122(3) . . ?
C32 C33 C34 120.4(3) . . ?
C32 C33 Ag 110.1(2) . 3_556 ?
C34 C33 Ag 72.26(18) . 3_556 ?
C32 C33 H33 120(3) . . ?
C34 C33 H33 120(3) . . ?
Ag C33 H33 92(3) 3_556 . ?
C33 C34 C35 120.2(3) . . ?
C33 C34 Ag 76.14(18) . 3_556 ?
C35 C34 Ag 108.3(2) . 3_556 ?
C33 C34 H34 119(3) . . ?
C35 C34 H34 120(3) . . ?
Ag C34 H34 88(2) 3_556 . ?
C36 C35 C34 117.9(3) . . ?
C36 C35 C1 118.4(3) . . ?
C34 C35 C1 123.5(3) . . ?
O5 C36 C35 120.3(3) . . ?
O5 C36 C31 116.7(3) . . ?
C35 C36 C31 122.9(3) . . ?
C46 C41 C42 117.6(3) . . ?
C46 C41 N2 124.0(3) . . ?
C42 C41 N2 118.3(3) . . ?
C43 C42 O5 120.7(3) . . ?
C43 C42 C41 123.1(3) . . ?
O5 C42 C41 116.1(3) . . ?
C42 C43 C44 117.7(3) . . ?
C42 C43 C1 118.0(3) . . ?
C44 C43 C1 124.2(3) . . ?
C45 C44 C43 120.4(3) . . ?
C45 C44 H44 124(2) . . ?
C43 C44 H44 116(2) . . ?
C44 C45 C46 120.9(3) . . ?
C44 C45 H45 124(3) . . ?
C46 C45 H45 115(3) . . ?
C45 C46 C41 120.2(3) . . ?
C45 C46 H46 120(2) . . ?
C41 C46 H46 120(2) . . ?
C52 C51 C56 117.3(3) . . ?
C52 C51 Si 122.3(2) . . ?
C56 C51 Si 120.4(2) . . ?
C53 C52 C51 121.4(3) . . ?
C53 C52 H52 122(3) . . ?
C51 C52 H52 117(3) . . ?
C52 C53 C54 120.5(3) . . ?
C52 C53 H53 116(3) . . ?
C54 C53 H53 123(3) . . ?
C55 C54 C53 119.4(3) . . ?
C55 C54 H54 127(4) . . ?
C53 C54 H54 114(4) . . ?
C54 C55 C56 120.1(3) . . ?
C54 C55 H55 121(3) . . ?
C56 C55 H55 119(3) . . ?
C55 C56 C51 121.3(3) . . ?
C55 C56 H56 117(2) . . ?
C51 C56 H56 121(2) . . ?
C35 C1 C43 107.5(2) . . ?
C35 C1 C2 112.1(3) . . ?
C43 C1 C2 112.4(3) . . ?
C35 C1 C3 107.7(3) . . ?
C43 C1 C3 108.3(3) . . ?
C2 C1 C3 108.8(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Cl1 C4 Cl2 109.2(4) . . ?
Cl1 C4 D4A 109.8 . . ?
Cl2 C4 D4A 109.8 . . ?
Cl1 C4 D4B 109.8 . . ?
Cl2 C4 D4B 109.8 . . ?
D4A C4 D4B 108.3 . . ?
Cl4 C5 Cl3 112.9(5) . . ?
Cl4 C5 D5A 109.0 . . ?
Cl3 C5 D5A 109.0 . . ?
Cl4 C5 D5B 109.0 . . ?
Cl3 C5 D5B 109.0 . . ?
D5A C5 D5B 107.8 . . ?
Cl5B C6 Cl6B 116.5(6) . . ?
Cl5A C6 Cl6A 114.4(4) . . ?
Cl5A C6 D6A 108.7 . . ?
Cl6A C6 D6A 108.7 . . ?
Cl5A C6 D6B 108.7 . . ?
Cl6A C6 D6B 108.7 . . ?
D6A C6 D6B 107.6 . . ?
Cl5B C6 D6C 108.2 . . ?
Cl6B C6 D6C 108.2 . . ?
Cl5B C6 D6D 108.2 . . ?
Cl6B C6 D6D 108.2 . . ?
D6C C6 D6D 107.3 . . ?

_refine_diff_density_max         2.037
_refine_diff_density_min         -2.350
_refine_diff_density_rms         0.148

_shelxl_version_number           2013-4

