# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_mj661
_database_code_depnum_ccdc_archive 'CCDC 1456557'
_audit_update_record             
;
2016-06-20 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          411
_chemical_formula_moiety         'C80 H96 N8 O12 Si8'
_chemical_formula_sum            'C80 H96 N8 O12 Si8'
_chemical_formula_weight         1586.37
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'
Si Si 0.0817 0.0704 '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                   9.982(3)
_cell_length_b                   13.141(4)
_cell_length_c                   16.763(5)
_cell_angle_alpha                82.27(3)
_cell_angle_beta                 82.12(3)
_cell_angle_gamma                77.37(3)
_cell_volume                     2112.9(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3414
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      30.7

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.190
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            15995
_diffrn_reflns_av_unetI/netI     0.1040
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.8
_diffrn_reflns_theta_max         30.7
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             11237
_reflns_number_gt                6986
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.6, CCDC 2015'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11237
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1128
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Si1 Si 0.81633(7) 0.67819(5) 0.46050(4) 0.01546(15) Uani 1 1 d . . . . .
Si2 Si 1.07004(7) 0.66319(5) 0.55419(4) 0.01545(15) Uani 1 1 d . . . . .
Si3 Si 0.99971(7) 0.46428(5) 0.66264(4) 0.01545(15) Uani 1 1 d . . . . .
Si4 Si 0.74565(7) 0.47908(5) 0.56881(4) 0.01591(15) Uani 1 1 d . . . . .
O1 O 0.87912(17) 0.62345(12) 0.37820(10) 0.0193(4) Uani 1 1 d . . . . .
O2 O 0.94181(17) 0.70519(12) 0.50043(10) 0.0202(4) Uani 1 1 d . . . . .
O3 O 1.02725(17) 0.58036(12) 0.62873(10) 0.0197(4) Uani 1 1 d . . . . .
O4 O 0.85271(16) 0.45462(12) 0.63723(10) 0.0196(4) Uani 1 1 d . . . . .
O5 O 0.74315(17) 0.59714(12) 0.52422(10) 0.0189(4) Uani 1 1 d . . . . .
O6 O 0.79838(17) 0.39567(12) 0.50219(10) 0.0197(4) Uani 1 1 d . . . . .
N1A N 0.3428(2) 0.86827(16) 0.34910(13) 0.0242(5) Uani 1 1 d . . . . .
N1B N 1.3100(2) 0.91495(16) 0.59629(14) 0.0251(5) Uani 1 1 d . . . . .
N1C N 0.8701(2) 0.63813(16) 0.93411(12) 0.0227(5) Uani 1 1 d . . . . .
N1D N 0.3658(2) 0.53939(17) 0.81749(13) 0.0237(5) Uani 1 1 d . . . . .
C1A C 0.6916(2) 0.79987(18) 0.43475(15) 0.0183(5) Uani 1 1 d . . . . .
H1AA H 0.6606 0.8363 0.4841 0.022 Uiso 1 1 calc R U . . .
H1AB H 0.7392 0.8464 0.3946 0.022 Uiso 1 1 calc R U . . .
C2A C 0.5641(3) 0.78365(18) 0.40015(16) 0.0224(6) Uani 1 1 d . . . . .
H2AA H 0.5943 0.7476 0.3506 0.027 Uiso 1 1 calc R U . . .
H2AB H 0.5153 0.7379 0.4402 0.027 Uiso 1 1 calc R U . . .
C3A C 0.4648(3) 0.88705(19) 0.37973(17) 0.0257(6) Uani 1 1 d . . . . .
H3AA H 0.4359 0.9242 0.4288 0.031 Uiso 1 1 calc R U . . .
H3AB H 0.5121 0.9322 0.3383 0.031 Uiso 1 1 calc R U . . .
C4A C 0.2948(3) 0.93189(19) 0.29150(16) 0.0239(6) Uani 1 1 d . . . . .
H4A H 0.3399 0.9879 0.2702 0.029 Uiso 1 1 calc R U . . .
C5A C 0.1707(3) 0.92249(19) 0.25593(15) 0.0226(6) Uani 1 1 d . . . . .
C6A C 0.0934(3) 0.84694(19) 0.28807(15) 0.0224(6) Uani 1 1 d . . . . .
H6A H 0.1196 0.7999 0.3341 0.027 Uiso 1 1 calc R U . . .
C7A C -0.0213(3) 0.8407(2) 0.25278(16) 0.0249(6) Uani 1 1 d . . . . .
H7A H -0.0732 0.7888 0.2746 0.030 Uiso 1 1 calc R U . . .
C8A C -0.0619(3) 0.9096(2) 0.18552(16) 0.0273(6) Uani 1 1 d . . . . .
H8A H -0.1414 0.9051 0.1618 0.033 Uiso 1 1 calc R U . . .
C9A C 0.0147(3) 0.9844(2) 0.15372(17) 0.0332(7) Uani 1 1 d . . . . .
H9A H -0.0116 1.0312 0.1075 0.040 Uiso 1 1 calc R U . . .
C10A C 0.1294(3) 0.9914(2) 0.18884(17) 0.0314(7) Uani 1 1 d . . . . .
H10A H 0.1806 1.0438 0.1671 0.038 Uiso 1 1 calc R U . . .
C1B C 1.1126(3) 0.77470(17) 0.59392(14) 0.0185(5) Uani 1 1 d . . . . .
H1BA H 1.0355 0.8031 0.6339 0.022 Uiso 1 1 calc R U . . .
H1BB H 1.1959 0.7493 0.6226 0.022 Uiso 1 1 calc R U . . .
C2B C 1.1389(3) 0.86291(18) 0.52825(15) 0.0220(6) Uani 1 1 d . . . . .
H2BA H 1.0542 0.8904 0.5010 0.026 Uiso 1 1 calc R U . . .
H2BB H 1.2135 0.8340 0.4871 0.026 Uiso 1 1 calc R U . . .
C3B C 1.1798(3) 0.95360(19) 0.56155(17) 0.0274(6) Uani 1 1 d . . . . .
H3BA H 1.1901 1.0104 0.5174 0.033 Uiso 1 1 calc R U . . .
H3BB H 1.1069 0.9824 0.6036 0.033 Uiso 1 1 calc R U . . .
C4B C 1.3041(3) 0.90460(18) 0.67299(16) 0.0238(6) Uani 1 1 d . . . . .
H4B H 1.2175 0.9264 0.7036 0.029 Uiso 1 1 calc R U . . .
C5B C 1.4260(3) 0.86016(18) 0.71648(16) 0.0215(6) Uani 1 1 d . . . . .
C6B C 1.4129(3) 0.8559(2) 0.80024(16) 0.0282(6) Uani 1 1 d . . . . .
H6B H 1.3257 0.8814 0.8289 0.034 Uiso 1 1 calc R U . . .
C7B C 1.5266(3) 0.8146(2) 0.84255(18) 0.0327(7) Uani 1 1 d . . . . .
H7B H 1.5170 0.8114 0.9000 0.039 Uiso 1 1 calc R U . . .
C8B C 1.6527(3) 0.7784(2) 0.80104(19) 0.0331(7) Uani 1 1 d . . . . .
H8B H 1.7309 0.7519 0.8299 0.040 Uiso 1 1 calc R U . . .
C9B C 1.6673(3) 0.7802(2) 0.71764(19) 0.0342(7) Uani 1 1 d . . . . .
H9B H 1.7545 0.7534 0.6895 0.041 Uiso 1 1 calc R U . . .
C10B C 1.5539(3) 0.8214(2) 0.67515(17) 0.0285(6) Uani 1 1 d . . . . .
H10B H 1.5637 0.8230 0.6178 0.034 Uiso 1 1 calc R U . . .
C1C C 1.0005(3) 0.44787(18) 0.77371(14) 0.0184(5) Uani 1 1 d . . . . .
H1CA H 0.9633 0.3849 0.7967 0.022 Uiso 1 1 calc R U . . .
H1CB H 1.0970 0.4360 0.7865 0.022 Uiso 1 1 calc R U . . .
C2C C 0.9154(3) 0.54254(19) 0.81381(14) 0.0206(5) Uani 1 1 d . . . . .
H2CA H 0.9413 0.6071 0.7842 0.025 Uiso 1 1 calc R U . . .
H2CB H 0.8164 0.5468 0.8094 0.025 Uiso 1 1 calc R U . . .
C3C C 0.9357(3) 0.53808(19) 0.90277(15) 0.0218(6) Uani 1 1 d . . . . .
H3CA H 0.8949 0.4810 0.9346 0.026 Uiso 1 1 calc R U . . .
H3CB H 1.0357 0.5226 0.9087 0.026 Uiso 1 1 calc R U . . .
C4C C 0.7887(3) 0.63631(19) 0.99913(15) 0.0212(6) Uani 1 1 d . . . . .
H4C H 0.7726 0.5704 1.0248 0.025 Uiso 1 1 calc R U . . .
C5C C 0.7184(3) 0.73137(19) 1.03651(15) 0.0215(6) Uani 1 1 d . . . . .
C6C C 0.6284(3) 0.7223(2) 1.10635(16) 0.0293(6) Uani 1 1 d . . . . .
H6C H 0.6156 0.6548 1.1302 0.035 Uiso 1 1 calc R U . . .
C7C C 0.5564(3) 0.8111(2) 1.14201(19) 0.0410(8) Uani 1 1 d . . . . .
H7C H 0.4954 0.8042 1.1903 0.049 Uiso 1 1 calc R U . . .
C8C C 0.5739(3) 0.9089(2) 1.1070(2) 0.0398(8) Uani 1 1 d . . . . .
H8C H 0.5229 0.9696 1.1305 0.048 Uiso 1 1 calc R U . . .
C9C C 0.6656(3) 0.9195(2) 1.03764(18) 0.0335(7) Uani 1 1 d . . . . .
H9C H 0.6789 0.9870 1.0144 0.040 Uiso 1 1 calc R U . . .
C10C C 0.7372(3) 0.8313(2) 1.00276(16) 0.0281(6) Uani 1 1 d . . . . .
H10C H 0.8000 0.8384 0.9553 0.034 Uiso 1 1 calc R U . . .
C1D C 0.5720(3) 0.46799(19) 0.61757(15) 0.0203(5) Uani 1 1 d . . . . .
H1DA H 0.5035 0.5021 0.5796 0.024 Uiso 1 1 calc R U . . .
H1DB H 0.5672 0.3928 0.6282 0.024 Uiso 1 1 calc R U . . .
C2D C 0.5323(3) 0.5175(2) 0.69702(15) 0.0242(6) Uani 1 1 d . . . . .
H2DA H 0.5974 0.4808 0.7361 0.029 Uiso 1 1 calc R U . . .
H2DB H 0.5417 0.5917 0.6871 0.029 Uiso 1 1 calc R U . . .
C3D C 0.3857(3) 0.5129(2) 0.73424(15) 0.0239(6) Uani 1 1 d . . . . .
H3DA H 0.3189 0.5629 0.7020 0.029 Uiso 1 1 calc R U . . .
H3DB H 0.3689 0.4415 0.7337 0.029 Uiso 1 1 calc R U . . .
C4D C 0.2801(3) 0.6213(2) 0.83550(16) 0.0240(6) Uani 1 1 d . . . . .
H4D H 0.2269 0.6615 0.7950 0.029 Uiso 1 1 calc R U . . .
C5D C 0.2594(3) 0.65708(19) 0.91654(16) 0.0232(6) Uani 1 1 d . . . . .
C6D C 0.1459(3) 0.7339(2) 0.93847(17) 0.0310(7) Uani 1 1 d . . . . .
H6D H 0.0811 0.7635 0.9009 0.037 Uiso 1 1 calc R U . . .
C7D C 0.1262(3) 0.7678(2) 1.01495(18) 0.0352(7) Uani 1 1 d . . . . .
H7D H 0.0477 0.8200 1.0296 0.042 Uiso 1 1 calc R U . . .
C8D C 0.2200(3) 0.7262(2) 1.06955(18) 0.0371(7) Uani 1 1 d . . . . .
H8D H 0.2068 0.7504 1.1215 0.044 Uiso 1 1 calc R U . . .
C9D C 0.3341(3) 0.6487(2) 1.04880(18) 0.0362(7) Uani 1 1 d . . . . .
H9D H 0.3983 0.6190 1.0868 0.043 Uiso 1 1 calc R U . . .
C10D C 0.3536(3) 0.6150(2) 0.97241(17) 0.0307(7) Uani 1 1 d . . . . .
H10D H 0.4320 0.5627 0.9580 0.037 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 O5 1.6215(18) . ?
Si1 O2 1.6220(18) . ?
Si1 O1 1.6267(18) . ?
Si1 C1A 1.839(2) . ?
Si2 O3 1.6185(18) . ?
Si2 O6 1.6212(19) 2_766 ?
Si2 O2 1.6213(18) . ?
Si2 C1B 1.839(2) . ?
Si3 O4 1.6180(18) . ?
Si3 O3 1.6226(17) . ?
Si3 O1 1.6237(19) 2_766 ?
Si3 C1C 1.846(2) . ?
Si4 O6 1.6253(18) . ?
Si4 O5 1.6256(17) . ?
Si4 O4 1.6271(18) . ?
Si4 C1D 1.840(3) . ?
O1 Si3 1.6237(19) 2_766 ?
O6 Si2 1.6213(19) 2_766 ?
N1A C4A 1.263(3) . ?
N1A C3A 1.464(3) . ?
N1B C4B 1.269(3) . ?
N1B C3B 1.458(3) . ?
N1C C4C 1.268(3) . ?
N1C C3C 1.466(3) . ?
N1D C4D 1.263(3) . ?
N1D C3D 1.460(3) . ?
C1A C2A 1.535(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A C3A 1.525(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A C5A 1.482(4) . ?
C4A H4A 0.9500 . ?
C5A C10A 1.395(3) . ?
C5A C6A 1.396(4) . ?
C6A C7A 1.381(4) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.395(3) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.383(4) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.383(4) . ?
C9A H9A 0.9500 . ?
C10A H10A 0.9500 . ?
C1B C2B 1.528(3) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B C3B 1.534(3) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B C5B 1.474(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.387(4) . ?
C5B C10B 1.392(4) . ?
C6B C7B 1.391(4) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.372(4) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.383(4) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.390(4) . ?
C9B H9B 0.9500 . ?
C10B H10B 0.9500 . ?
C1C C2C 1.525(3) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.524(3) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C C5C 1.467(4) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.383(4) . ?
C5C C10C 1.399(3) . ?
C6C C7C 1.393(4) . ?
C6C H6C 0.9500 . ?
C7C C8C 1.376(4) . ?
C7C H7C 0.9500 . ?
C8C C9C 1.389(4) . ?
C8C H8C 0.9500 . ?
C9C C10C 1.379(4) . ?
C9C H9C 0.9500 . ?
C10C H10C 0.9500 . ?
C1D C2D 1.526(3) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D C3D 1.521(3) . ?
C2D H2DA 0.9900 . ?
C2D H2DB 0.9900 . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4D C5D 1.470(4) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.386(4) . ?
C5D C10D 1.394(4) . ?
C6D C7D 1.389(4) . ?
C6D H6D 0.9500 . ?
C7D C8D 1.375(4) . ?
C7D H7D 0.9500 . ?
C8D C9D 1.391(4) . ?
C8D H8D 0.9500 . ?
C9D C10D 1.385(4) . ?
C9D H9D 0.9500 . ?
C10D H10D 0.9500 . ?

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
O5 Si1 O2 108.97(9) . . ?
O5 Si1 O1 109.31(9) . . ?
O2 Si1 O1 108.84(9) . . ?
O5 Si1 C1A 110.98(11) . . ?
O2 Si1 C1A 109.67(10) . . ?
O1 Si1 C1A 109.05(10) . . ?
O3 Si2 O6 108.94(9) . 2_766 ?
O3 Si2 O2 109.34(10) . . ?
O6 Si2 O2 108.96(9) 2_766 . ?
O3 Si2 C1B 109.62(10) . . ?
O6 Si2 C1B 110.55(11) 2_766 . ?
O2 Si2 C1B 109.41(10) . . ?
O4 Si3 O3 108.46(9) . . ?
O4 Si3 O1 109.01(9) . 2_766 ?
O3 Si3 O1 109.40(10) . 2_766 ?
O4 Si3 C1C 111.66(11) . . ?
O3 Si3 C1C 108.03(10) . . ?
O1 Si3 C1C 110.23(10) 2_766 . ?
O6 Si4 O5 109.16(9) . . ?
O6 Si4 O4 108.99(9) . . ?
O5 Si4 O4 108.98(9) . . ?
O6 Si4 C1D 110.37(10) . . ?
O5 Si4 C1D 109.96(11) . . ?
O4 Si4 C1D 109.34(10) . . ?
Si3 O1 Si1 145.48(11) 2_766 . ?
Si2 O2 Si1 147.75(11) . . ?
Si2 O3 Si3 150.07(12) . . ?
Si3 O4 Si4 148.16(12) . . ?
Si1 O5 Si4 149.60(12) . . ?
Si2 O6 Si4 145.71(11) 2_766 . ?
C4A N1A C3A 117.2(2) . . ?
C4B N1B C3B 116.8(2) . . ?
C4C N1C C3C 118.2(2) . . ?
C4D N1D C3D 119.2(2) . . ?
C2A C1A Si1 114.45(16) . . ?
C2A C1A H1AA 108.6 . . ?
Si1 C1A H1AA 108.6 . . ?
C2A C1A H1AB 108.6 . . ?
Si1 C1A H1AB 108.6 . . ?
H1AA C1A H1AB 107.6 . . ?
C3A C2A C1A 112.1(2) . . ?
C3A C2A H2AA 109.2 . . ?
C1A C2A H2AA 109.2 . . ?
C3A C2A H2AB 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?
N1A C3A C2A 110.6(2) . . ?
N1A C3A H3AA 109.5 . . ?
C2A C3A H3AA 109.5 . . ?
N1A C3A H3AB 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 108.1 . . ?
N1A C4A C5A 122.5(2) . . ?
N1A C4A H4A 118.8 . . ?
C5A C4A H4A 118.8 . . ?
C10A C5A C6A 119.1(2) . . ?
C10A C5A C4A 119.1(2) . . ?
C6A C5A C4A 121.8(2) . . ?
C7A C6A C5A 119.8(2) . . ?
C7A C6A H6A 120.1 . . ?
C5A C6A H6A 120.1 . . ?
C6A C7A C8A 120.9(3) . . ?
C6A C7A H7A 119.6 . . ?
C8A C7A H7A 119.6 . . ?
C9A C8A C7A 119.3(3) . . ?
C9A C8A H8A 120.4 . . ?
C7A C8A H8A 120.4 . . ?
C8A C9A C10A 120.3(3) . . ?
C8A C9A H9A 119.9 . . ?
C10A C9A H9A 119.9 . . ?
C9A C10A C5A 120.7(3) . . ?
C9A C10A H10A 119.7 . . ?
C5A C10A H10A 119.7 . . ?
C2B C1B Si2 113.38(17) . . ?
C2B C1B H1BA 108.9 . . ?
Si2 C1B H1BA 108.9 . . ?
C2B C1B H1BB 108.9 . . ?
Si2 C1B H1BB 108.9 . . ?
H1BA C1B H1BB 107.7 . . ?
C1B C2B C3B 113.0(2) . . ?
C1B C2B H2BA 109.0 . . ?
C3B C2B H2BA 109.0 . . ?
C1B C2B H2BB 109.0 . . ?
C3B C2B H2BB 109.0 . . ?
H2BA C2B H2BB 107.8 . . ?
N1B C3B C2B 109.1(2) . . ?
N1B C3B H3BA 109.9 . . ?
C2B C3B H3BA 109.9 . . ?
N1B C3B H3BB 109.9 . . ?
C2B C3B H3BB 109.9 . . ?
H3BA C3B H3BB 108.3 . . ?
N1B C4B C5B 122.7(3) . . ?
N1B C4B H4B 118.6 . . ?
C5B C4B H4B 118.6 . . ?
C6B C5B C10B 119.3(2) . . ?
C6B C5B C4B 119.4(3) . . ?
C10B C5B C4B 121.3(2) . . ?
C5B C6B C7B 120.4(3) . . ?
C5B C6B H6B 119.8 . . ?
C7B C6B H6B 119.8 . . ?
C8B C7B C6B 119.7(3) . . ?
C8B C7B H7B 120.1 . . ?
C6B C7B H7B 120.1 . . ?
C7B C8B C9B 120.7(3) . . ?
C7B C8B H8B 119.7 . . ?
C9B C8B H8B 119.7 . . ?
C8B C9B C10B 119.8(3) . . ?
C8B C9B H9B 120.1 . . ?
C10B C9B H9B 120.1 . . ?
C9B C10B C5B 120.1(3) . . ?
C9B C10B H10B 120.0 . . ?
C5B C10B H10B 120.0 . . ?
C2C C1C Si3 112.87(16) . . ?
C2C C1C H1CA 109.0 . . ?
Si3 C1C H1CA 109.0 . . ?
C2C C1C H1CB 109.0 . . ?
Si3 C1C H1CB 109.0 . . ?
H1CA C1C H1CB 107.8 . . ?
C3C C2C C1C 113.13(19) . . ?
C3C C2C H2CA 109.0 . . ?
C1C C2C H2CA 109.0 . . ?
C3C C2C H2CB 109.0 . . ?
C1C C2C H2CB 109.0 . . ?
H2CA C2C H2CB 107.8 . . ?
N1C C3C C2C 110.47(19) . . ?
N1C C3C H3CA 109.6 . . ?
C2C C3C H3CA 109.6 . . ?
N1C C3C H3CB 109.6 . . ?
C2C C3C H3CB 109.6 . . ?
H3CA C3C H3CB 108.1 . . ?
N1C C4C C5C 123.0(2) . . ?
N1C C4C H4C 118.5 . . ?
C5C C4C H4C 118.5 . . ?
C6C C5C C10C 118.9(2) . . ?
C6C C5C C4C 119.1(2) . . ?
C10C C5C C4C 122.0(2) . . ?
C5C C6C C7C 120.6(3) . . ?
C5C C6C H6C 119.7 . . ?
C7C C6C H6C 119.7 . . ?
C8C C7C C6C 119.7(3) . . ?
C8C C7C H7C 120.1 . . ?
C6C C7C H7C 120.1 . . ?
C7C C8C C9C 120.5(3) . . ?
C7C C8C H8C 119.8 . . ?
C9C C8C H8C 119.8 . . ?
C10C C9C C8C 119.6(3) . . ?
C10C C9C H9C 120.2 . . ?
C8C C9C H9C 120.2 . . ?
C9C C10C C5C 120.7(3) . . ?
C9C C10C H10C 119.7 . . ?
C5C C10C H10C 119.7 . . ?
C2D C1D Si4 113.74(17) . . ?
C2D C1D H1DA 108.8 . . ?
Si4 C1D H1DA 108.8 . . ?
C2D C1D H1DB 108.8 . . ?
Si4 C1D H1DB 108.8 . . ?
H1DA C1D H1DB 107.7 . . ?
C3D C2D C1D 113.1(2) . . ?
C3D C2D H2DA 109.0 . . ?
C1D C2D H2DA 109.0 . . ?
C3D C2D H2DB 109.0 . . ?
C1D C2D H2DB 109.0 . . ?
H2DA C2D H2DB 107.8 . . ?
N1D C3D C2D 109.8(2) . . ?
N1D C3D H3DA 109.7 . . ?
C2D C3D H3DA 109.7 . . ?
N1D C3D H3DB 109.7 . . ?
C2D C3D H3DB 109.7 . . ?
H3DA C3D H3DB 108.2 . . ?
N1D C4D C5D 122.7(2) . . ?
N1D C4D H4D 118.6 . . ?
C5D C4D H4D 118.6 . . ?
C6D C5D C10D 118.9(3) . . ?
C6D C5D C4D 120.4(2) . . ?
C10D C5D C4D 120.7(2) . . ?
C5D C6D C7D 120.5(3) . . ?
C5D C6D H6D 119.7 . . ?
C7D C6D H6D 119.7 . . ?
C8D C7D C6D 120.2(3) . . ?
C8D C7D H7D 119.9 . . ?
C6D C7D H7D 119.9 . . ?
C7D C8D C9D 120.1(3) . . ?
C7D C8D H8D 119.9 . . ?
C9D C8D H8D 119.9 . . ?
C10D C9D C8D 119.5(3) . . ?
C10D C9D H9D 120.2 . . ?
C8D C9D H9D 120.2 . . ?
C9D C10D C5D 120.8(3) . . ?
C9D C10D H10D 119.6 . . ?
C5D C10D H10D 119.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2B H2BB N1A 0.99 2.53 3.391(4) 145.9 1_655

_refine_diff_density_max         0.514
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.070


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method methanol
####################################################################### 
# 
# 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_mj487
_database_code_depnum_ccdc_archive 'CCDC 1456558'
_audit_update_record             
;
2016-06-20 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          124
_chemical_formula_moiety         'C80 H96 N8 O20 Si8'
_chemical_formula_sum            'C80 H96 N8 O20 Si8'
_chemical_formula_weight         1714.37
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'
Si Si 0.0817 0.0704 '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                   9.381(3)
_cell_length_b                   14.034(4)
_cell_length_c                   16.112(5)
_cell_angle_alpha                91.48(3)
_cell_angle_beta                 94.07(3)
_cell_angle_gamma                90.06(3)
_cell_volume                     2115.1(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    7550
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      30.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.20
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            19597
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.8
_diffrn_reflns_theta_max         30.6
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11718
_reflns_number_gt                8613
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+0.6340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11718
_refine_ls_number_parameters     527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Si4 Si 0.97095(5) 0.15818(3) 0.09681(3) 0.01429(10) Uani 1 1 d . . . . .
Si1 Si 0.81283(5) 0.11814(3) -0.07960(3) 0.01493(10) Uani 1 1 d . . . . .
Si3 Si 1.25543(5) 0.08888(3) 0.03011(3) 0.01458(10) Uani 1 1 d . . . . .
Si2 Si 1.09659(5) 0.04860(3) -0.14623(3) 0.01452(10) Uani 1 1 d . . . . .
O4 O 1.14041(12) 0.14187(8) 0.08630(7) 0.0176(2) Uani 1 1 d . . . . .
O3 O 1.19714(12) 0.08914(8) -0.06718(7) 0.0183(2) Uani 1 1 d . . . . .
O2 O 0.93604(13) 0.09067(9) -0.14213(7) 0.0186(3) Uani 1 1 d . . . . .
O5 O 0.88702(13) 0.16549(9) 0.00559(7) 0.0191(3) Uani 1 1 d . . . . .
O1 O 0.72739(13) 0.02141(8) -0.05874(7) 0.0181(2) Uani 1 1 d . . . . .
O6 O 0.90996(13) 0.06685(8) 0.14327(7) 0.0180(2) Uani 1 1 d . . . . .
O1B O 1.55965(15) 0.01627(10) -0.34749(9) 0.0292(3) Uani 1 1 d . . . . .
H1B H 1.4758 0.0371 -0.3544 0.044 Uiso 1 1 calc R U . . .
N1B N 1.29481(17) 0.01891(11) -0.40176(9) 0.0231(3) Uani 1 1 d . . . . .
O1D O 0.86434(17) 0.25578(12) 0.52635(9) 0.0372(4) Uani 1 1 d . . . . .
H1D H 0.8595 0.2680 0.4755 0.056 Uiso 1 1 calc R U . . .
N1D N 0.93389(18) 0.33405(11) 0.39065(10) 0.0250(3) Uani 1 1 d . . . . .
O1A O 0.20966(16) 0.31219(10) -0.07486(10) 0.0344(3) Uani 1 1 d . . . . .
H1A H 0.2615 0.2832 -0.1075 0.052 Uiso 1 1 calc R U . . .
N1A N 0.40748(17) 0.29278(11) -0.18276(10) 0.0236(3) Uani 1 1 d . . . . .
O1C O 1.25010(16) 0.37382(11) 0.18592(10) 0.0360(4) Uani 1 1 d . . . . .
H1C H 1.2957 0.3240 0.1753 0.054 Uiso 1 1 calc R U . . .
C1B C 1.16985(18) 0.08092(13) -0.24455(10) 0.0186(3) Uani 1 1 d . . . . .
H1BA H 1.1732 0.1513 -0.2474 0.022 Uiso 1 1 calc R U . . .
H1BB H 1.2691 0.0571 -0.2449 0.022 Uiso 1 1 calc R U . . .
N1C N 1.42958(17) 0.23596(12) 0.21494(10) 0.0259(3) Uani 1 1 d . . . . .
C5B C 1.4576(2) -0.09864(13) -0.44781(11) 0.0220(4) Uani 1 1 d . . . . .
C2B C 1.08296(19) 0.04078(14) -0.32229(11) 0.0208(4) Uani 1 1 d . . . . .
H2BA H 1.0719 -0.0289 -0.3171 0.025 Uiso 1 1 calc R U . . .
H2BB H 0.9863 0.0693 -0.3248 0.025 Uiso 1 1 calc R U . . .
C1C C 1.42971(18) 0.15121(13) 0.04103(11) 0.0199(4) Uani 1 1 d . . . . .
H1CA H 1.4774 0.1398 -0.0112 0.024 Uiso 1 1 calc R U . . .
H1CB H 1.4105 0.2205 0.0454 0.024 Uiso 1 1 calc R U . . .
C5A C 0.3643(2) 0.44065(13) -0.11006(12) 0.0235(4) Uani 1 1 d . . . . .
C2A C 0.5816(2) 0.16354(13) -0.19619(12) 0.0226(4) Uani 1 1 d . . . . .
H2AA H 0.5175 0.1191 -0.1698 0.027 Uiso 1 1 calc R U . . .
H2AB H 0.6335 0.1264 -0.2375 0.027 Uiso 1 1 calc R U . . .
C3D C 0.9203(2) 0.34700(13) 0.30053(11) 0.0251(4) Uani 1 1 d . . . . .
H3DA H 0.9829 0.4001 0.2862 0.030 Uiso 1 1 calc R U . . .
H3DB H 0.8205 0.3640 0.2831 0.030 Uiso 1 1 calc R U . . .
C4A C 0.4379(2) 0.38086(13) -0.16803(12) 0.0238(4) Uani 1 1 d . . . . .
H4A H 0.5125 0.4084 -0.1965 0.029 Uiso 1 1 calc R U . . .
C3A C 0.4913(2) 0.23954(14) -0.24119(12) 0.0245(4) Uani 1 1 d . . . . .
H3AA H 0.5546 0.2839 -0.2683 0.029 Uiso 1 1 calc R U . . .
H3AB H 0.4263 0.2087 -0.2850 0.029 Uiso 1 1 calc R U . . .
C1A C 0.68957(18) 0.20523(12) -0.12962(11) 0.0182(3) Uani 1 1 d . . . . .
H1AA H 0.6365 0.2375 -0.0860 0.022 Uiso 1 1 calc R U . . .
H1AB H 0.7468 0.2544 -0.1553 0.022 Uiso 1 1 calc R U . . .
C5D C 1.0536(2) 0.37172(13) 0.52433(12) 0.0239(4) Uani 1 1 d . . . . .
C1D C 0.93637(19) 0.26634(12) 0.15940(11) 0.0185(3) Uani 1 1 d . . . . .
H1DA H 0.9982 0.3183 0.1419 0.022 Uiso 1 1 calc R U . . .
H1DB H 0.8359 0.2858 0.1467 0.022 Uiso 1 1 calc R U . . .
C4D C 1.0301(2) 0.38240(13) 0.43416(12) 0.0235(4) Uani 1 1 d . . . . .
H4D H 1.0874 0.4262 0.4072 0.028 Uiso 1 1 calc R U . . .
C2D C 0.9617(2) 0.25626(13) 0.25382(11) 0.0220(4) Uani 1 1 d . . . . .
H2DA H 0.9046 0.2021 0.2717 0.026 Uiso 1 1 calc R U . . .
H2DB H 1.0638 0.2423 0.2679 0.026 Uiso 1 1 calc R U . . .
C10B C 1.4792(2) -0.17970(14) -0.49877(12) 0.0281(4) Uani 1 1 d . . . . .
H10B H 1.4030 -0.2036 -0.5355 0.034 Uiso 1 1 calc R U . . .
C2C C 1.53586(19) 0.12619(14) 0.11341(12) 0.0238(4) Uani 1 1 d . . . . .
H2CA H 1.5655 0.0590 0.1059 0.029 Uiso 1 1 calc R U . . .
H2CB H 1.6220 0.1665 0.1111 0.029 Uiso 1 1 calc R U . . .
C6B C 1.5730(2) -0.06301(13) -0.39541(12) 0.0236(4) Uani 1 1 d . . . . .
C4B C 1.3178(2) -0.05253(14) -0.45007(11) 0.0234(4) Uani 1 1 d . . . . .
H4B H 1.2428 -0.0759 -0.4879 0.028 Uiso 1 1 calc R U . . .
C6D C 0.9694(2) 0.30876(14) 0.56681(12) 0.0274(4) Uani 1 1 d . . . . .
C10D C 1.1623(2) 0.42364(14) 0.56928(13) 0.0286(4) Uani 1 1 d . . . . .
H10D H 1.2202 0.4658 0.5409 0.034 Uiso 1 1 calc R U . . .
C6A C 0.2535(2) 0.40401(14) -0.06505(13) 0.0268(4) Uani 1 1 d . . . . .
C3B C 1.1519(2) 0.06029(15) -0.40346(11) 0.0258(4) Uani 1 1 d . . . . .
H3BA H 1.0919 0.0324 -0.4511 0.031 Uiso 1 1 calc R U . . .
H3BB H 1.1581 0.1299 -0.4110 0.031 Uiso 1 1 calc R U . . .
C10A C 0.4051(2) 0.53611(14) -0.09627(13) 0.0285(4) Uani 1 1 d . . . . .
H10A H 0.4804 0.5611 -0.1257 0.034 Uiso 1 1 calc R U . . .
C9A C 0.3387(2) 0.59462(15) -0.04113(13) 0.0319(5) Uani 1 1 d . . . . .
H9A H 0.3674 0.6593 -0.0328 0.038 Uiso 1 1 calc R U . . .
C5C C 1.4291(2) 0.37817(14) 0.30038(12) 0.0269(4) Uani 1 1 d . . . . .
C4C C 1.4819(2) 0.28295(14) 0.27873(12) 0.0265(4) Uani 1 1 d . . . . .
H4C H 1.5569 0.2557 0.3131 0.032 Uiso 1 1 calc R U . . .
C7C C 1.2599(2) 0.50726(16) 0.27852(15) 0.0358(5) Uani 1 1 d . . . . .
H7C H 1.1805 0.5344 0.2479 0.043 Uiso 1 1 calc R U . . .
C8B C 1.7216(2) -0.18959(15) -0.44186(13) 0.0324(5) Uani 1 1 d . . . . .
H8B H 1.8112 -0.2213 -0.4393 0.039 Uiso 1 1 calc R U . . .
C6C C 1.3129(2) 0.41841(15) 0.25403(13) 0.0285(4) Uani 1 1 d . . . . .
C9B C 1.6103(2) -0.22475(15) -0.49585(14) 0.0329(5) Uani 1 1 d . . . . .
H9B H 1.6243 -0.2793 -0.5304 0.039 Uiso 1 1 calc R U . . .
C9D C 1.1862(2) 0.41443(15) 0.65418(13) 0.0328(5) Uani 1 1 d . . . . .
H9D H 1.2607 0.4497 0.6840 0.039 Uiso 1 1 calc R U . . .
C7A C 0.1870(2) 0.46323(16) -0.00914(14) 0.0330(5) Uani 1 1 d . . . . .
H7A H 0.1126 0.4388 0.0213 0.040 Uiso 1 1 calc R U . . .
C3C C 1.4798(2) 0.13871(14) 0.19955(12) 0.0269(4) Uani 1 1 d . . . . .
H3CA H 1.4002 0.0934 0.2048 0.032 Uiso 1 1 calc R U . . .
H3CB H 1.5569 0.1234 0.2423 0.032 Uiso 1 1 calc R U . . .
C7B C 1.7043(2) -0.10943(15) -0.39195(13) 0.0288(4) Uani 1 1 d . . . . .
H7B H 1.7814 -0.0862 -0.3556 0.035 Uiso 1 1 calc R U . . .
C7D C 0.9937(2) 0.30067(15) 0.65308(13) 0.0327(5) Uani 1 1 d . . . . .
H7D H 0.9365 0.2589 0.6823 0.039 Uiso 1 1 calc R U . . .
C8C C 1.3237(3) 0.55543(16) 0.34765(15) 0.0369(5) Uani 1 1 d . . . . .
H8C H 1.2870 0.6155 0.3641 0.044 Uiso 1 1 calc R U . . .
C8D C 1.1013(2) 0.35361(15) 0.69581(13) 0.0333(5) Uani 1 1 d . . . . .
H8D H 1.1171 0.3481 0.7544 0.040 Uiso 1 1 calc R U . . .
C9C C 1.4395(3) 0.51767(16) 0.39289(14) 0.0381(5) Uani 1 1 d . . . . .
H9C H 1.4834 0.5519 0.4396 0.046 Uiso 1 1 calc R U . . .
C10C C 1.4912(2) 0.42902(16) 0.36952(13) 0.0344(5) Uani 1 1 d . . . . .
H10C H 1.5702 0.4025 0.4010 0.041 Uiso 1 1 calc R U . . .
C8A C 0.2288(2) 0.55756(16) 0.00243(14) 0.0359(5) Uani 1 1 d . . . . .
H8A H 0.1820 0.5975 0.0404 0.043 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si4 O5 1.6231(14) . ?
Si4 O6 1.6245(14) . ?
Si4 O4 1.6265(13) . ?
Si4 C1D 1.8425(18) . ?
Si1 O5 1.6206(14) . ?
Si1 O2 1.6265(13) . ?
Si1 O1 1.6302(14) . ?
Si1 C1A 1.8444(19) . ?
Si3 O3 1.6232(14) . ?
Si3 O4 1.6255(13) . ?
Si3 O1 1.6314(14) 2_755 ?
Si3 C1C 1.8486(18) . ?
Si2 O3 1.6206(14) . ?
Si2 O6 1.6233(13) 2_755 ?
Si2 O2 1.6234(14) . ?
Si2 C1B 1.8381(18) . ?
O1 Si3 1.6313(14) 2_755 ?
O6 Si2 1.6234(13) 2_755 ?
O1B C6B 1.349(2) . ?
O1B H1B 0.8400 . ?
N1B C4B 1.281(2) . ?
N1B C3B 1.460(2) . ?
O1D C6D 1.353(2) . ?
O1D H1D 0.8400 . ?
N1D C4D 1.285(2) . ?
N1D C3D 1.465(2) . ?
O1A C6A 1.354(2) . ?
O1A H1A 0.8400 . ?
N1A C4A 1.281(2) . ?
N1A C3A 1.461(2) . ?
O1C C6C 1.347(2) . ?
O1C H1C 0.8400 . ?
C1B C2B 1.539(2) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
N1C C4C 1.275(2) . ?
N1C C3C 1.465(3) . ?
C5B C6B 1.408(3) . ?
C5B C10B 1.409(3) . ?
C5B C4B 1.462(3) . ?
C2B C3B 1.530(3) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C1C C2C 1.527(3) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C5A C10A 1.401(3) . ?
C5A C6A 1.412(3) . ?
C5A C4A 1.451(3) . ?
C2A C1A 1.526(2) . ?
C2A C3A 1.528(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3D C2D 1.527(2) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4A H4A 0.9500 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C5D C10D 1.400(3) . ?
C5D C6D 1.407(3) . ?
C5D C4D 1.465(3) . ?
C1D C2D 1.533(2) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C4D H4D 0.9500 . ?
C2D H2DA 0.9900 . ?
C2D H2DB 0.9900 . ?
C10B C9B 1.381(3) . ?
C10B H10B 0.9500 . ?
C2C C3C 1.524(3) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C6B C7B 1.392(3) . ?
C4B H4B 0.9500 . ?
C6D C7D 1.400(3) . ?
C10D C9D 1.380(3) . ?
C10D H10D 0.9500 . ?
C6A C7A 1.391(3) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C10A C9A 1.376(3) . ?
C10A H10A 0.9500 . ?
C9A C8A 1.396(3) . ?
C9A H9A 0.9500 . ?
C5C C10C 1.398(3) . ?
C5C C6C 1.405(3) . ?
C5C C4C 1.468(3) . ?
C4C H4C 0.9500 . ?
C7C C8C 1.386(3) . ?
C7C C6C 1.400(3) . ?
C7C H7C 0.9500 . ?
C8B C7B 1.382(3) . ?
C8B C9B 1.392(3) . ?
C8B H8B 0.9500 . ?
C9B H9B 0.9500 . ?
C9D C8D 1.384(3) . ?
C9D H9D 0.9500 . ?
C7A C8A 1.384(3) . ?
C7A H7A 0.9500 . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C7B H7B 0.9500 . ?
C7D C8D 1.385(3) . ?
C7D H7D 0.9500 . ?
C8C C9C 1.378(4) . ?
C8C H8C 0.9500 . ?
C8D H8D 0.9500 . ?
C9C C10C 1.389(3) . ?
C9C H9C 0.9500 . ?
C10C H10C 0.9500 . ?
C8A H8A 0.9500 . ?

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
O5 Si4 O6 108.82(7) . . ?
O5 Si4 O4 109.43(7) . . ?
O6 Si4 O4 108.39(7) . . ?
O5 Si4 C1D 109.38(8) . . ?
O6 Si4 C1D 108.35(8) . . ?
O4 Si4 C1D 112.39(8) . . ?
O5 Si1 O2 109.20(7) . . ?
O5 Si1 O1 109.76(7) . . ?
O2 Si1 O1 108.86(7) . . ?
O5 Si1 C1A 109.06(8) . . ?
O2 Si1 C1A 109.28(8) . . ?
O1 Si1 C1A 110.66(8) . . ?
O3 Si3 O4 109.50(7) . . ?
O3 Si3 O1 108.60(7) . 2_755 ?
O4 Si3 O1 108.86(7) . 2_755 ?
O3 Si3 C1C 108.30(8) . . ?
O4 Si3 C1C 110.86(8) . . ?
O1 Si3 C1C 110.70(8) 2_755 . ?
O3 Si2 O6 109.13(7) . 2_755 ?
O3 Si2 O2 109.74(7) . . ?
O6 Si2 O2 108.95(7) 2_755 . ?
O3 Si2 C1B 110.85(8) . . ?
O6 Si2 C1B 108.12(8) 2_755 . ?
O2 Si2 C1B 110.01(8) . . ?
Si3 O4 Si4 144.30(8) . . ?
Si2 O3 Si3 152.46(9) . . ?
Si2 O2 Si1 143.90(9) . . ?
Si1 O5 Si4 152.16(9) . . ?
Si1 O1 Si3 144.98(8) . 2_755 ?
Si2 O6 Si4 145.93(8) 2_755 . ?
C6B O1B H1B 109.5 . . ?
C4B N1B C3B 119.24(17) . . ?
C6D O1D H1D 109.5 . . ?
C4D N1D C3D 118.16(17) . . ?
C6A O1A H1A 109.5 . . ?
C4A N1A C3A 118.15(17) . . ?
C6C O1C H1C 109.5 . . ?
C2B C1B Si2 113.55(12) . . ?
C2B C1B H1BA 108.9 . . ?
Si2 C1B H1BA 108.9 . . ?
C2B C1B H1BB 108.9 . . ?
Si2 C1B H1BB 108.9 . . ?
H1BA C1B H1BB 107.7 . . ?
C4C N1C C3C 119.10(18) . . ?
C6B C5B C10B 118.76(18) . . ?
C6B C5B C4B 120.99(16) . . ?
C10B C5B C4B 120.25(18) . . ?
C3B C2B C1B 113.23(15) . . ?
C3B C2B H2BA 108.9 . . ?
C1B C2B H2BA 108.9 . . ?
C3B C2B H2BB 108.9 . . ?
C1B C2B H2BB 108.9 . . ?
H2BA C2B H2BB 107.7 . . ?
C2C C1C Si3 118.64(13) . . ?
C2C C1C H1CA 107.7 . . ?
Si3 C1C H1CA 107.7 . . ?
C2C C1C H1CB 107.7 . . ?
Si3 C1C H1CB 107.7 . . ?
H1CA C1C H1CB 107.1 . . ?
C10A C5A C6A 118.66(18) . . ?
C10A C5A C4A 120.00(18) . . ?
C6A C5A C4A 121.32(18) . . ?
C1A C2A C3A 113.07(15) . . ?
C1A C2A H2AA 109.0 . . ?
C3A C2A H2AA 109.0 . . ?
C1A C2A H2AB 109.0 . . ?
C3A C2A H2AB 109.0 . . ?
H2AA C2A H2AB 107.8 . . ?
N1D C3D C2D 110.98(15) . . ?
N1D C3D H3DA 109.4 . . ?
C2D C3D H3DA 109.4 . . ?
N1D C3D H3DB 109.4 . . ?
C2D C3D H3DB 109.4 . . ?
H3DA C3D H3DB 108.0 . . ?
N1A C4A C5A 123.27(18) . . ?
N1A C4A H4A 118.4 . . ?
C5A C4A H4A 118.4 . . ?
N1A C3A C2A 110.62(15) . . ?
N1A C3A H3AA 109.5 . . ?
C2A C3A H3AA 109.5 . . ?
N1A C3A H3AB 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 108.1 . . ?
C2A C1A Si1 115.15(12) . . ?
C2A C1A H1AA 108.5 . . ?
Si1 C1A H1AA 108.5 . . ?
C2A C1A H1AB 108.5 . . ?
Si1 C1A H1AB 108.5 . . ?
H1AA C1A H1AB 107.5 . . ?
C10D C5D C6D 119.06(18) . . ?
C10D C5D C4D 120.03(19) . . ?
C6D C5D C4D 120.90(18) . . ?
C2D C1D Si4 115.23(12) . . ?
C2D C1D H1DA 108.5 . . ?
Si4 C1D H1DA 108.5 . . ?
C2D C1D H1DB 108.5 . . ?
Si4 C1D H1DB 108.5 . . ?
H1DA C1D H1DB 107.5 . . ?
N1D C4D C5D 121.70(19) . . ?
N1D C4D H4D 119.1 . . ?
C5D C4D H4D 119.1 . . ?
C3D C2D C1D 111.40(15) . . ?
C3D C2D H2DA 109.3 . . ?
C1D C2D H2DA 109.3 . . ?
C3D C2D H2DB 109.3 . . ?
C1D C2D H2DB 109.3 . . ?
H2DA C2D H2DB 108.0 . . ?
C9B C10B C5B 120.6(2) . . ?
C9B C10B H10B 119.7 . . ?
C5B C10B H10B 119.7 . . ?
C3C C2C C1C 115.05(16) . . ?
C3C C2C H2CA 108.5 . . ?
C1C C2C H2CA 108.5 . . ?
C3C C2C H2CB 108.5 . . ?
C1C C2C H2CB 108.5 . . ?
H2CA C2C H2CB 107.5 . . ?
O1B C6B C7B 118.41(18) . . ?
O1B C6B C5B 121.24(17) . . ?
C7B C6B C5B 120.35(17) . . ?
N1B C4B C5B 120.99(18) . . ?
N1B C4B H4B 119.5 . . ?
C5B C4B H4B 119.5 . . ?
O1D C6D C7D 118.83(19) . . ?
O1D C6D C5D 121.59(18) . . ?
C7D C6D C5D 119.58(19) . . ?
C9D C10D C5D 120.9(2) . . ?
C9D C10D H10D 119.6 . . ?
C5D C10D H10D 119.6 . . ?
O1A C6A C7A 118.70(19) . . ?
O1A C6A C5A 121.72(18) . . ?
C7A C6A C5A 119.59(19) . . ?
N1B C3B C2B 110.31(15) . . ?
N1B C3B H3BA 109.6 . . ?
C2B C3B H3BA 109.6 . . ?
N1B C3B H3BB 109.6 . . ?
C2B C3B H3BB 109.6 . . ?
H3BA C3B H3BB 108.1 . . ?
C9A C10A C5A 121.6(2) . . ?
C9A C10A H10A 119.2 . . ?
C5A C10A H10A 119.2 . . ?
C10A C9A C8A 119.0(2) . . ?
C10A C9A H9A 120.5 . . ?
C8A C9A H9A 120.5 . . ?
C10C C5C C6C 118.9(2) . . ?
C10C C5C C4C 120.20(19) . . ?
C6C C5C C4C 120.86(18) . . ?
N1C C4C C5C 121.53(19) . . ?
N1C C4C H4C 119.2 . . ?
C5C C4C H4C 119.2 . . ?
C8C C7C C6C 119.8(2) . . ?
C8C C7C H7C 120.1 . . ?
C6C C7C H7C 120.1 . . ?
C7B C8B C9B 121.28(19) . . ?
C7B C8B H8B 119.4 . . ?
C9B C8B H8B 119.4 . . ?
O1C C6C C7C 118.5(2) . . ?
O1C C6C C5C 121.75(19) . . ?
C7C C6C C5C 119.7(2) . . ?
C10B C9B C8B 119.49(19) . . ?
C10B C9B H9B 120.3 . . ?
C8B C9B H9B 120.3 . . ?
C10D C9D C8D 119.7(2) . . ?
C10D C9D H9D 120.1 . . ?
C8D C9D H9D 120.1 . . ?
C8A C7A C6A 120.4(2) . . ?
C8A C7A H7A 119.8 . . ?
C6A C7A H7A 119.8 . . ?
N1C C3C C2C 112.04(16) . . ?
N1C C3C H3CA 109.2 . . ?
C2C C3C H3CA 109.2 . . ?
N1C C3C H3CB 109.2 . . ?
C2C C3C H3CB 109.2 . . ?
H3CA C3C H3CB 107.9 . . ?
C8B C7B C6B 119.5(2) . . ?
C8B C7B H7B 120.3 . . ?
C6B C7B H7B 120.3 . . ?
C8D C7D C6D 119.9(2) . . ?
C8D C7D H7D 120.0 . . ?
C6D C7D H7D 120.0 . . ?
C9C C8C C7C 121.2(2) . . ?
C9C C8C H8C 119.4 . . ?
C7C C8C H8C 119.4 . . ?
C9D C8D C7D 120.8(2) . . ?
C9D C8D H8D 119.6 . . ?
C7D C8D H8D 119.6 . . ?
C8C C9C C10C 119.3(2) . . ?
C8C C9C H9C 120.4 . . ?
C10C C9C H9C 120.4 . . ?
C9C C10C C5C 121.1(2) . . ?
C9C C10C H10C 119.4 . . ?
C5C C10C H10C 119.4 . . ?
C7A C8A C9A 120.7(2) . . ?
C7A C8A H8A 119.6 . . ?
C9A C8A H8A 119.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1A H1A N1A 0.84 1.90 2.641(2) 146.6 .
O1B H1B N1B 0.84 1.83 2.575(2) 147.6 .
O1C H1C N1C 0.84 1.86 2.596(2) 146.1 .
O1D H1D N1D 0.84 1.85 2.596(2) 147.6 .
C2A H2AB O1B 0.99 2.39 3.150(2) 133.6 1_455

_refine_diff_density_max         0.413
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.063


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method methanol
####################################################################### 
# 
# 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_mj488a
_database_code_depnum_ccdc_archive 'CCDC 1456559'
_audit_update_record             
;
2016-06-20 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          442
_chemical_formula_moiety         'C80 H88 Br8 N8 O12 Si8'
_chemical_formula_sum            'C80 H88 Br8 N8 O12 Si8'
_chemical_formula_weight         2217.51

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'
Br Br -0.2901 2.4595 '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'
_symmetry_space_group_name_hall  '-P 1'

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

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

_cell_length_a                   11.895(3)
_cell_length_b                   14.061(4)
_cell_length_c                   15.763(4)
_cell_angle_alpha                66.17(5)
_cell_angle_beta                 85.35(5)
_cell_angle_gamma                68.70(5)
_cell_volume                     2240.3(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    7874
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      28.0

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.370
_exptl_absorpt_coefficient_mu    3.750
_shelx_estimated_absorpt_T_min   0.251
_shelx_estimated_absorpt_T_max   0.338
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_T_max  0.366
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_diffrn_ambient_temperature      80(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  'Xcalibur PX with Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            20253
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.8
_diffrn_reflns_theta_max         28.1
_diffrn_reflns_theta_full        26.0
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10851
_reflns_number_gt                8358
_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       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.6, CCDC 2015'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+1.7250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10851
_refine_ls_number_parameters     598
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Br1 Br 0.18927(4) 0.54409(4) 0.49559(3) 0.04266(13) Uani 1 1 d . . . . .
Br2 Br 0.38973(4) -0.07389(3) 0.82673(2) 0.02700(10) Uani 1 1 d . . . . .
Br3 Br 0.10983(4) -0.05960(4) 0.43501(3) 0.03781(12) Uani 1 1 d . . . . .
Br4 Br -0.03663(5) 0.50711(4) 0.30112(3) 0.04649(14) Uani 1 1 d . . . . .
O1 O 1.1020(2) 0.10145(19) 0.05637(16) 0.0178(5) Uani 1 1 d . . . . .
O2 O 0.9587(2) 0.00392(19) 0.16185(15) 0.0180(5) Uani 1 1 d . . . . .
O3 O 0.8655(2) -0.11304(19) 0.11470(15) 0.0171(5) Uani 1 1 d . . . . .
O4 O 0.7673(2) 0.07966(18) -0.02827(16) 0.0170(5) Uani 1 1 d . . . . .
O5 O 0.8649(2) 0.19511(18) 0.01675(16) 0.0173(5) Uani 1 1 d . . . . .
O6 O 0.8982(2) 0.1802(2) -0.14585(16) 0.0204(5) Uani 1 1 d . . . . .
Si1 Si 0.97148(9) 0.12325(7) 0.09982(6) 0.01377(19) Uani 1 1 d . . . . .
Si2 Si 0.97220(9) -0.12132(7) 0.17776(6) 0.01416(19) Uani 1 1 d . . . . .
Si3 Si 0.80266(9) -0.05394(7) 0.00930(6) 0.01296(19) Uani 1 1 d . . . . .
Si4 Si 0.80220(9) 0.19062(7) -0.06862(6) 0.01380(19) Uani 1 1 d . . . . .
C1A C 0.9590(3) 0.1972(3) 0.1758(2) 0.0178(7) Uani 1 1 d . . . . .
H1AA H 1.0211 0.1492 0.2287 0.021 Uiso 1 1 calc R U . . .
H1AB H 0.9764 0.2659 0.1403 0.021 Uiso 1 1 calc R U . . .
C2A C 0.8346(3) 0.2286(3) 0.2138(3) 0.0223(8) Uani 1 1 d . . . . .
H2AA H 0.7736 0.2852 0.1619 0.027 Uiso 1 1 calc R U . . .
H2AB H 0.8119 0.1618 0.2422 0.027 Uiso 1 1 calc R U . . .
C3A C 0.8337(4) 0.2748(3) 0.2861(3) 0.0250(8) Uani 1 1 d . . . . .
H3AA H 0.8953 0.2187 0.3378 0.030 Uiso 1 1 calc R U . . .
H3AB H 0.8550 0.3423 0.2576 0.030 Uiso 1 1 calc R U . . .
C4A C 0.6679(4) 0.3983(3) 0.3230(2) 0.0225(8) Uani 1 1 d . . . . .
H4A H 0.7102 0.4483 0.2988 0.027 Uiso 1 1 calc R U . . .
C5A C 0.5496(4) 0.4356(3) 0.3595(2) 0.0227(8) Uani 1 1 d . . . . .
C6A C 0.5058(4) 0.5391(3) 0.3651(3) 0.0293(9) Uani 1 1 d . . . . .
H6A H 0.5508 0.5869 0.3422 0.035 Uiso 1 1 calc R U . . .
C7A C 0.3974(4) 0.5732(3) 0.4038(3) 0.0324(10) Uani 1 1 d . . . . .
H7A H 0.3676 0.6438 0.4074 0.039 Uiso 1 1 calc R U . . .
C8A C 0.3341(4) 0.5029(3) 0.4366(3) 0.0283(9) Uani 1 1 d . . . . .
C9A C 0.3726(4) 0.4012(4) 0.4298(3) 0.0347(10) Uani 1 1 d . . . . .
H9A H 0.3264 0.3544 0.4519 0.042 Uiso 1 1 calc R U . . .
C10A C 0.4800(4) 0.3694(3) 0.3900(3) 0.0314(9) Uani 1 1 d . . . . .
H10A H 0.5067 0.3005 0.3835 0.038 Uiso 1 1 calc R U . . .
N1A N 0.7149(3) 0.3029(3) 0.3228(2) 0.0251(7) Uani 1 1 d . . . . .
C1B C 0.9678(3) -0.2051(3) 0.3019(2) 0.0184(7) Uani 1 1 d . . . . .
H1BA H 0.9679 -0.2780 0.3078 0.022 Uiso 1 1 calc R U . . .
H1BB H 1.0439 -0.2199 0.3345 0.022 Uiso 1 1 calc R U . . .
C2B C 0.8639(3) -0.1585(3) 0.3530(2) 0.0183(7) Uani 1 1 d . . . . .
H2BA H 0.7866 -0.1455 0.3231 0.022 Uiso 1 1 calc R U . . .
H2BB H 0.8624 -0.0859 0.3489 0.022 Uiso 1 1 calc R U . . .
C3B C 0.8756(4) -0.2381(3) 0.4548(2) 0.0237(8) Uani 1 1 d . . . . .
H3BA H 0.8863 -0.3129 0.4588 0.028 Uiso 1 1 calc R U . . .
H3BB H 0.9485 -0.2446 0.4863 0.028 Uiso 1 1 calc R U . . .
C4B C 0.7876(4) -0.1862(3) 0.5740(3) 0.0296(9) Uani 1 1 d . . . . .
H4B H 0.8675 -0.1976 0.5915 0.035 Uiso 1 1 calc R U . . .
C5B C 0.6909(4) -0.1533(3) 0.6309(2) 0.0251(8) Uani 1 1 d . . . . .
C6B C 0.5685(4) -0.1222(3) 0.6045(2) 0.0218(8) Uani 1 1 d . . . . .
H6B H 0.5471 -0.1173 0.5458 0.026 Uiso 1 1 calc R U . . .
C7B C 0.4799(3) -0.0988(3) 0.6612(2) 0.0204(8) Uani 1 1 d . . . . .
H7B H 0.3976 -0.0784 0.6425 0.024 Uiso 1 1 calc R U . . .
C8B C 0.5113(4) -0.1050(3) 0.7473(2) 0.0224(8) Uani 1 1 d . . . . .
C9B C 0.6309(4) -0.1342(4) 0.7748(3) 0.0331(10) Uani 1 1 d . . . . .
H9B H 0.6517 -0.1379 0.8333 0.040 Uiso 1 1 calc R U . . .
C10B C 0.7196(4) -0.1578(4) 0.7169(3) 0.0369(11) Uani 1 1 d . . . . .
H10B H 0.8017 -0.1775 0.7357 0.044 Uiso 1 1 calc R U . . .
N1B N 0.7705(3) -0.2003(3) 0.5023(2) 0.0235(7) Uani 1 1 d . . . . .
C1C C 0.6652(3) -0.0833(3) 0.0054(2) 0.0172(7) Uani 1 1 d . . . . .
H1CA H 0.6068 -0.0525 0.0446 0.021 Uiso 1 1 calc R U . . .
H1CB H 0.6282 -0.0432 -0.0593 0.021 Uiso 1 1 calc R U . . .
C2C C 0.6838(4) -0.2074(3) 0.0379(2) 0.0232(8) Uani 1 1 d . . . . .
H2CA H 0.6152 -0.2133 0.0114 0.028 Uiso 1 1 calc R U . . .
H2CB H 0.7586 -0.2446 0.0137 0.028 Uiso 1 1 calc R U . . .
C3C C 0.6929(4) -0.2679(3) 0.1435(3) 0.0277(9) Uani 1 1 d . . . . .
H3CA H 0.7178 -0.3490 0.1609 0.033 Uiso 1 1 calc R U . . .
H3CB H 0.7555 -0.2555 0.1710 0.033 Uiso 1 1 calc R U . . .
C4C C 0.5771(4) -0.2033(3) 0.2491(3) 0.0269(9) Uani 1 1 d . . . . .
H4C H 0.6511 -0.2100 0.2739 0.032 Uiso 1 1 calc R U . . .
C5C C 0.4655(4) -0.1647(3) 0.2916(2) 0.0253(9) Uani 1 1 d . . . . .
C6C C 0.3528(4) -0.1368(3) 0.2502(3) 0.0243(8) Uani 1 1 d . . . . .
H6C H 0.3484 -0.1401 0.1916 0.029 Uiso 1 1 calc R U . . .
C7C C 0.2481(4) -0.1049(3) 0.2909(2) 0.0249(9) Uani 1 1 d . . . . .
H7C H 0.1720 -0.0851 0.2608 0.030 Uiso 1 1 calc R U . . .
C8C C 0.2548(4) -0.1018(3) 0.3770(3) 0.0288(9) Uani 1 1 d . . . . .
C9C C 0.3648(4) -0.1287(4) 0.4207(3) 0.0394(11) Uani 1 1 d . . . . .
H9C H 0.3681 -0.1263 0.4798 0.047 Uiso 1 1 calc R U . . .
C10C C 0.4700(4) -0.1591(4) 0.3780(3) 0.0350(10) Uani 1 1 d . . . . .
H10C H 0.5457 -0.1762 0.4074 0.042 Uiso 1 1 calc R U . . .
N1C N 0.5785(3) -0.2282(3) 0.1802(2) 0.0249(7) Uani 1 1 d . . . . .
C1D C 0.6658(3) 0.3157(3) -0.1195(2) 0.0184(7) Uani 1 1 d . . . . .
H1DA H 0.6903 0.3809 -0.1525 0.022 Uiso 1 1 calc R U . . .
H1DB H 0.6237 0.3070 -0.1660 0.022 Uiso 1 1 calc R U . . .
C2D C 0.5777(3) 0.3392(3) -0.0487(2) 0.0207(8) Uani 1 1 d . . . . .
H2D1 H 0.5564 0.2722 -0.0153 0.025 Uiso 1 1 calc R U . A 1
H2D2 H 0.6220 0.3464 -0.0025 0.025 Uiso 1 1 calc R U . A 1
C3D C 0.462(2) 0.438(2) -0.0799(11) 0.016(2) Uani 0.5 1 d D . P B 1
H3DA H 0.4810 0.5065 -0.1113 0.019 Uiso 0.5 1 calc R U P B 1
H3DB H 0.4157 0.4325 -0.1261 0.019 Uiso 0.5 1 calc R U P B 1
C4D C 0.2769(7) 0.4625(5) -0.0100(5) 0.0191(15) Uani 0.5 1 d D . P B 1
H4D H 0.2420 0.4688 -0.0650 0.023 Uiso 0.5 1 calc R U P B 1
C5D C 0.2002(7) 0.4696(7) 0.0662(6) 0.0226(17) Uani 0.5 1 d D . P B 1
C6D C 0.0760(7) 0.4960(6) 0.0548(5) 0.0255(17) Uani 0.5 1 d D . P B 1
H6D H 0.0414 0.5079 -0.0026 0.031 Uiso 0.5 1 calc R U P B 1
C7D C 0.0029(7) 0.5049(6) 0.1256(5) 0.0258(17) Uani 0.5 1 d D . P B 1
H7D H -0.0818 0.5247 0.1160 0.031 Uiso 0.5 1 calc R U P B 1
C8D C 0.0504(10) 0.4856(9) 0.2091(7) 0.026(3) Uani 0.5 1 d D . P B 1
C9D C 0.1709(11) 0.4631(9) 0.2198(6) 0.031(3) Uani 0.5 1 d D . P B 1
H9D H 0.2029 0.4554 0.2766 0.037 Uiso 0.5 1 calc R U P B 1
C10D C 0.2501(8) 0.4508(7) 0.1506(6) 0.0273(19) Uani 0.5 1 d D . P B 1
H10D H 0.3348 0.4304 0.1613 0.033 Uiso 0.5 1 calc R U P B 1
N1D N 0.3866(9) 0.4485(7) -0.0055(6) 0.021(2) Uani 0.5 1 d . . P B 1
C3E C 0.464(2) 0.439(2) -0.1051(11) 0.016(2) Uani 0.5 1 d D . P B 2
H3EA H 0.4884 0.5041 -0.1399 0.019 Uiso 0.5 1 calc R U P B 2
H3EB H 0.4353 0.4204 -0.1514 0.019 Uiso 0.5 1 calc R U P B 2
C4E C 0.3777(11) 0.4232(9) 0.0367(7) 0.023(2) Uani 0.5 1 d D . P B 2
H4E H 0.4538 0.3674 0.0653 0.028 Uiso 0.5 1 calc R U P B 2
C5E C 0.2779(8) 0.4517(6) 0.0953(5) 0.0223(16) Uani 0.5 1 d D . P B 2
C6E C 0.1637(8) 0.5312(7) 0.0592(6) 0.0269(18) Uani 0.5 1 d D . P B 2
H6E H 0.1474 0.5694 -0.0063 0.032 Uiso 0.5 1 calc R U P B 2
C7E C 0.0721(7) 0.5565(6) 0.1164(5) 0.0290(18) Uani 0.5 1 d D . P B 2
H7E H -0.0039 0.6141 0.0902 0.035 Uiso 0.5 1 calc R U P B 2
C8E C 0.0927(10) 0.4977(8) 0.2104(6) 0.019(2) Uani 0.5 1 d D . P B 2
C9E C 0.2072(9) 0.4252(8) 0.2497(6) 0.020(2) Uani 0.5 1 d D . P B 2
H9E H 0.2231 0.3917 0.3154 0.024 Uiso 0.5 1 calc R U P B 2
C10E C 0.3012(8) 0.4006(7) 0.1920(6) 0.0268(18) Uani 0.5 1 d D . P B 2
H10E H 0.3799 0.3494 0.2189 0.032 Uiso 0.5 1 calc R U P B 2
N1E N 0.3625(8) 0.4721(7) -0.0504(6) 0.0245(19) Uani 0.5 1 d . . P B 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
Br1 C8A 1.903(4) . ?
Br2 C8B 1.881(4) . ?
Br3 C8C 1.898(5) . ?
Br4 C8D 1.776(11) . ?
Br4 C8E 2.020(10) . ?
O1 Si3 1.619(3) 2_755 ?
O1 Si1 1.620(3) . ?
O2 Si1 1.622(3) . ?
O2 Si2 1.623(2) . ?
O3 Si2 1.617(2) . ?
O3 Si3 1.626(2) . ?
O4 Si3 1.620(2) . ?
O4 Si4 1.624(2) . ?
O5 Si1 1.616(3) . ?
O5 Si4 1.624(2) . ?
O6 Si2 1.612(3) 2_755 ?
O6 Si4 1.614(3) . ?
Si1 C1A 1.845(3) . ?
Si2 O6 1.612(3) 2_755 ?
Si2 C1B 1.839(4) . ?
Si3 O1 1.619(3) 2_755 ?
Si3 C1C 1.837(3) . ?
Si4 C1D 1.835(4) . ?
C1A C2A 1.529(5) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A C3A 1.520(4) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A N1A 1.461(5) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A N1A 1.254(5) . ?
C4A C5A 1.469(6) . ?
C4A H4A 0.9500 . ?
C5A C10A 1.386(5) . ?
C5A C6A 1.394(5) . ?
C6A C7A 1.387(6) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.369(6) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.380(5) . ?
C9A C10A 1.381(6) . ?
C9A H9A 0.9500 . ?
C10A H10A 0.9500 . ?
C1B C2B 1.512(5) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B C3B 1.523(5) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B N1B 1.447(5) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B N1B 1.266(4) . ?
C4B C5B 1.457(6) . ?
C4B H4B 0.9500 . ?
C5B C10B 1.396(5) . ?
C5B C6B 1.404(5) . ?
C6B C7B 1.360(5) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.396(5) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.384(6) . ?
C9B C10B 1.375(6) . ?
C9B H9B 0.9500 . ?
C10B H10B 0.9500 . ?
C1C C2C 1.540(5) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.524(5) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C N1C 1.442(5) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C N1C 1.266(5) . ?
C4C C5C 1.460(6) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.390(5) . ?
C5C C10C 1.403(5) . ?
C6C C7C 1.364(6) . ?
C6C H6C 0.9500 . ?
C7C C8C 1.383(5) . ?
C7C H7C 0.9500 . ?
C8C C9C 1.381(6) . ?
C9C C10C 1.381(6) . ?
C9C H9C 0.9500 . ?
C10C H10C 0.9500 . ?
C1D C2D 1.519(5) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D C3D 1.50(3) . ?
C2D C3E 1.55(3) . ?
C2D H2D1 0.9900 . ?
C2D H2D2 0.9900 . ?
C3D N1D 1.439(18) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4D N1D 1.251(12) . ?
C4D C5D 1.462(10) . ?
C4D H4D 0.9500 . ?
C5D C10D 1.386(10) . ?
C5D C6D 1.394(10) . ?
C6D C7D 1.377(10) . ?
C6D H6D 0.9500 . ?
C7D C8D 1.358(11) . ?
C7D H7D 0.9500 . ?
C8D C9D 1.360(12) . ?
C9D C10D 1.406(12) . ?
C9D H9D 0.9500 . ?
C10D H10D 0.9500 . ?
C3E N1E 1.47(2) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C4E N1E 1.256(11) . ?
C4E C5E 1.483(12) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.388(10) . ?
C5E C10E 1.398(10) . ?
C6E C7E 1.394(10) . ?
C6E H6E 0.9500 . ?
C7E C8E 1.364(11) . ?
C7E H7E 0.9500 . ?
C8E C9E 1.377(11) . ?
C9E C10E 1.416(10) . ?
C9E H9E 0.9500 . ?
C10E H10E 0.9500 . ?

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
Si3 O1 Si1 150.86(15) 2_755 . ?
Si1 O2 Si2 151.76(16) . . ?
Si2 O3 Si3 143.04(16) . . ?
Si3 O4 Si4 152.03(17) . . ?
Si1 O5 Si4 143.18(16) . . ?
Si2 O6 Si4 152.45(17) 2_755 . ?
O5 Si1 O1 109.68(14) . . ?
O5 Si1 O2 109.24(13) . . ?
O1 Si1 O2 108.78(14) . . ?
O5 Si1 C1A 110.25(15) . . ?
O1 Si1 C1A 110.44(15) . . ?
O2 Si1 C1A 108.41(14) . . ?
O6 Si2 O3 109.48(13) 2_755 . ?
O6 Si2 O2 108.83(14) 2_755 . ?
O3 Si2 O2 108.68(14) . . ?
O6 Si2 C1B 107.69(16) 2_755 . ?
O3 Si2 C1B 111.84(15) . . ?
O2 Si2 C1B 110.26(14) . . ?
O1 Si3 O4 109.79(14) 2_755 . ?
O1 Si3 O3 108.87(14) 2_755 . ?
O4 Si3 O3 108.95(13) . . ?
O1 Si3 C1C 108.97(14) 2_755 . ?
O4 Si3 C1C 109.06(15) . . ?
O3 Si3 C1C 111.19(15) . . ?
O6 Si4 O5 109.35(13) . . ?
O6 Si4 O4 108.14(13) . . ?
O5 Si4 O4 108.20(13) . . ?
O6 Si4 C1D 110.75(16) . . ?
O5 Si4 C1D 110.20(15) . . ?
O4 Si4 C1D 110.13(15) . . ?
C2A C1A Si1 113.6(2) . . ?
C2A C1A H1AA 108.8 . . ?
Si1 C1A H1AA 108.8 . . ?
C2A C1A H1AB 108.8 . . ?
Si1 C1A H1AB 108.8 . . ?
H1AA C1A H1AB 107.7 . . ?
C3A C2A C1A 111.7(3) . . ?
C3A C2A H2AA 109.3 . . ?
C1A C2A H2AA 109.3 . . ?
C3A C2A H2AB 109.3 . . ?
C1A C2A H2AB 109.3 . . ?
H2AA C2A H2AB 107.9 . . ?
N1A C3A C2A 111.1(3) . . ?
N1A C3A H3AA 109.4 . . ?
C2A C3A H3AA 109.4 . . ?
N1A C3A H3AB 109.4 . . ?
C2A C3A H3AB 109.4 . . ?
H3AA C3A H3AB 108.0 . . ?
N1A C4A C5A 122.4(4) . . ?
N1A C4A H4A 118.8 . . ?
C5A C4A H4A 118.8 . . ?
C10A C5A C6A 118.4(4) . . ?
C10A C5A C4A 121.5(3) . . ?
C6A C5A C4A 120.1(4) . . ?
C7A C6A C5A 120.9(4) . . ?
C7A C6A H6A 119.6 . . ?
C5A C6A H6A 119.6 . . ?
C8A C7A C6A 118.6(4) . . ?
C8A C7A H7A 120.7 . . ?
C6A C7A H7A 120.7 . . ?
C7A C8A C9A 122.3(4) . . ?
C7A C8A Br1 119.6(3) . . ?
C9A C8A Br1 118.1(3) . . ?
C8A C9A C10A 118.1(4) . . ?
C8A C9A H9A 120.9 . . ?
C10A C9A H9A 120.9 . . ?
C9A C10A C5A 121.6(4) . . ?
C9A C10A H10A 119.2 . . ?
C5A C10A H10A 119.2 . . ?
C4A N1A C3A 117.4(3) . . ?
C2B C1B Si2 118.4(2) . . ?
C2B C1B H1BA 107.7 . . ?
Si2 C1B H1BA 107.7 . . ?
C2B C1B H1BB 107.7 . . ?
Si2 C1B H1BB 107.7 . . ?
H1BA C1B H1BB 107.1 . . ?
C1B C2B C3B 111.2(3) . . ?
C1B C2B H2BA 109.4 . . ?
C3B C2B H2BA 109.4 . . ?
C1B C2B H2BB 109.4 . . ?
C3B C2B H2BB 109.4 . . ?
H2BA C2B H2BB 108.0 . . ?
N1B C3B C2B 111.8(3) . . ?
N1B C3B H3BA 109.3 . . ?
C2B C3B H3BA 109.3 . . ?
N1B C3B H3BB 109.3 . . ?
C2B C3B H3BB 109.3 . . ?
H3BA C3B H3BB 107.9 . . ?
N1B C4B C5B 123.4(4) . . ?
N1B C4B H4B 118.3 . . ?
C5B C4B H4B 118.3 . . ?
C10B C5B C6B 118.0(4) . . ?
C10B C5B C4B 119.7(4) . . ?
C6B C5B C4B 122.2(3) . . ?
C7B C6B C5B 121.5(3) . . ?
C7B C6B H6B 119.2 . . ?
C5B C6B H6B 119.2 . . ?
C6B C7B C8B 119.3(4) . . ?
C6B C7B H7B 120.4 . . ?
C8B C7B H7B 120.4 . . ?
C9B C8B C7B 120.6(4) . . ?
C9B C8B Br2 119.7(3) . . ?
C7B C8B Br2 119.7(3) . . ?
C10B C9B C8B 119.5(3) . . ?
C10B C9B H9B 120.2 . . ?
C8B C9B H9B 120.2 . . ?
C9B C10B C5B 121.0(4) . . ?
C9B C10B H10B 119.5 . . ?
C5B C10B H10B 119.5 . . ?
C4B N1B C3B 117.5(3) . . ?
C2C C1C Si3 115.6(3) . . ?
C2C C1C H1CA 108.4 . . ?
Si3 C1C H1CA 108.4 . . ?
C2C C1C H1CB 108.4 . . ?
Si3 C1C H1CB 108.4 . . ?
H1CA C1C H1CB 107.4 . . ?
C3C C2C C1C 112.7(3) . . ?
C3C C2C H2CA 109.0 . . ?
C1C C2C H2CA 109.0 . . ?
C3C C2C H2CB 109.0 . . ?
C1C C2C H2CB 109.0 . . ?
H2CA C2C H2CB 107.8 . . ?
N1C C3C C2C 110.8(3) . . ?
N1C C3C H3CA 109.5 . . ?
C2C C3C H3CA 109.5 . . ?
N1C C3C H3CB 109.5 . . ?
C2C C3C H3CB 109.5 . . ?
H3CA C3C H3CB 108.1 . . ?
N1C C4C C5C 122.1(4) . . ?
N1C C4C H4C 119.0 . . ?
C5C C4C H4C 119.0 . . ?
C6C C5C C10C 118.0(4) . . ?
C6C C5C C4C 121.6(3) . . ?
C10C C5C C4C 120.3(4) . . ?
C7C C6C C5C 122.2(4) . . ?
C7C C6C H6C 118.9 . . ?
C5C C6C H6C 118.9 . . ?
C6C C7C C8C 118.8(4) . . ?
C6C C7C H7C 120.6 . . ?
C8C C7C H7C 120.6 . . ?
C9C C8C C7C 121.0(4) . . ?
C9C C8C Br3 119.8(3) . . ?
C7C C8C Br3 119.1(3) . . ?
C8C C9C C10C 119.6(4) . . ?
C8C C9C H9C 120.2 . . ?
C10C C9C H9C 120.2 . . ?
C9C C10C C5C 120.3(4) . . ?
C9C C10C H10C 119.9 . . ?
C5C C10C H10C 119.9 . . ?
C4C N1C C3C 118.6(3) . . ?
C2D C1D Si4 113.9(2) . . ?
C2D C1D H1DA 108.8 . . ?
Si4 C1D H1DA 108.8 . . ?
C2D C1D H1DB 108.8 . . ?
Si4 C1D H1DB 108.8 . . ?
H1DA C1D H1DB 107.7 . . ?
C3D C2D C1D 120.0(6) . . ?
C1D C2D C3E 106.2(6) . . ?
C3D C2D H2D1 107.3 . . ?
C1D C2D H2D1 107.3 . . ?
C3D C2D H2D2 107.3 . . ?
C1D C2D H2D2 107.3 . . ?
H2D1 C2D H2D2 106.9 . . ?
N1D C3D C2D 113.8(13) . . ?
N1D C3D H3DA 108.8 . . ?
C2D C3D H3DA 108.8 . . ?
N1D C3D H3DB 108.8 . . ?
C2D C3D H3DB 108.8 . . ?
H3DA C3D H3DB 107.7 . . ?
N1D C4D C5D 122.5(7) . . ?
N1D C4D H4D 118.7 . . ?
C5D C4D H4D 118.7 . . ?
C10D C5D C6D 119.2(7) . . ?
C10D C5D C4D 120.3(8) . . ?
C6D C5D C4D 120.5(7) . . ?
C7D C6D C5D 120.8(7) . . ?
C7D C6D H6D 119.6 . . ?
C5D C6D H6D 119.6 . . ?
C8D C7D C6D 120.8(8) . . ?
C8D C7D H7D 119.6 . . ?
C6D C7D H7D 119.6 . . ?
C7D C8D C9D 118.7(10) . . ?
C7D C8D Br4 124.4(8) . . ?
C9D C8D Br4 116.2(8) . . ?
C8D C9D C10D 122.8(9) . . ?
C8D C9D H9D 118.6 . . ?
C10D C9D H9D 118.6 . . ?
C5D C10D C9D 117.5(8) . . ?
C5D C10D H10D 121.2 . . ?
C9D C10D H10D 121.2 . . ?
C4D N1D C3D 121.9(11) . . ?
N1E C3E C2D 115.7(12) . . ?
N1E C3E H3EA 108.3 . . ?
C2D C3E H3EA 108.3 . . ?
N1E C3E H3EB 108.3 . . ?
C2D C3E H3EB 108.3 . . ?
H3EA C3E H3EB 107.4 . . ?
N1E C4E C5E 120.6(10) . . ?
N1E C4E H4E 119.7 . . ?
C5E C4E H4E 119.7 . . ?
C6E C5E C10E 117.9(8) . . ?
C6E C5E C4E 123.4(8) . . ?
C10E C5E C4E 118.6(8) . . ?
C5E C6E C7E 121.9(7) . . ?
C5E C6E H6E 119.0 . . ?
C7E C6E H6E 119.0 . . ?
C8E C7E C6E 119.3(8) . . ?
C8E C7E H7E 120.3 . . ?
C6E C7E H7E 120.3 . . ?
C7E C8E C9E 120.6(9) . . ?
C7E C8E Br4 124.3(7) . . ?
C9E C8E Br4 115.2(7) . . ?
C8E C9E C10E 119.8(8) . . ?
C8E C9E H9E 120.1 . . ?
C10E C9E H9E 120.1 . . ?
C5E C10E C9E 119.9(9) . . ?
C5E C10E H10E 120.1 . . ?
C9E C10E H10E 120.1 . . ?
C4E N1E C3E 118.2(12) . . ?

_refine_diff_density_max         1.065
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.105


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method methanol
####################################################################### 
# 
# 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_MJ491b
_database_code_depnum_ccdc_archive 'CCDC 1456560'
_audit_update_record             
;
2016-06-20 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
_audit_creation_date             2015-09-26
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C112 H112 N8 O20 Si8, 6.1(C H4 O)'
_chemical_formula_sum            'C118.10 H136.40 N8 O26.10 Si8'
_chemical_formula_weight         2310.28
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'

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


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

_cell_length_a                   14.292(6)
_cell_length_b                   14.663(7)
_cell_length_c                   15.109(7)
_cell_angle_alpha                97.14(4)
_cell_angle_beta                 97.17(4)
_cell_angle_gamma                110.39(4)
_cell_volume                     2896(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    2981
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      30.6

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_F_000             1222
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.170
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(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  'Xcalibur PX with Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            18913
_diffrn_reflns_av_unetI/netI     0.1430
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.8
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10761
_reflns_number_gt                5889
_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       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.6, CCDC 2015'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0686P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10761
_refine_ls_number_parameters     772
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1799
_refine_ls_wR_factor_gt          0.1444
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.001
_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 0.6350(2) 0.1784(2) 0.51191(19) 0.0213(7) Uani 1 1 d . . . . .
O2 O 0.4793(2) 0.1077(2) 0.37613(19) 0.0223(7) Uani 1 1 d . . . . .
O3 O 0.3523(2) 0.0703(2) 0.49278(18) 0.0227(7) Uani 1 1 d . . . . .
O4 O 0.5090(2) 0.1442(2) 0.62890(19) 0.0220(7) Uani 1 1 d . . . . .
O5 O 0.6263(2) 0.0359(2) 0.38252(19) 0.0237(7) Uani 1 1 d . . . . .
O6 O 0.3443(2) -0.0733(2) 0.36297(19) 0.0222(7) Uani 1 1 d . . . . .
Si1 Si 0.60048(9) 0.13493(9) 0.40390(8) 0.0201(3) Uani 1 1 d . . . . .
Si2 Si 0.36462(9) 0.04401(9) 0.38803(8) 0.0197(3) Uani 1 1 d . . . . .
Si3 Si 0.38948(9) 0.07455(9) 0.59936(8) 0.0192(3) Uani 1 1 d . . . . .
Si4 Si 0.62538(9) 0.16563(9) 0.61564(8) 0.0191(3) Uani 1 1 d . . . . .
C1A C 0.6689(3) 0.2287(3) 0.3402(3) 0.0227(10) Uani 1 1 d . . . . .
H1AA H 0.6491 0.2003 0.2746 0.027 Uiso 1 1 calc R U . . .
H1AB H 0.6475 0.2860 0.3503 0.027 Uiso 1 1 calc R U . . .
C2A C 0.7849(3) 0.2655(3) 0.3665(3) 0.0329(12) Uani 1 1 d . . . . .
H2AA H 0.8047 0.2906 0.4327 0.039 Uiso 1 1 calc R U . . .
H2AB H 0.8068 0.2090 0.3530 0.039 Uiso 1 1 calc R U . . .
C3A C 0.8403(4) 0.3471(4) 0.3171(4) 0.0399(13) Uani 1 1 d . . . . .
H3AA H 0.9143 0.3628 0.3315 0.048 Uiso 1 1 calc R U . . .
H3AB H 0.8179 0.3245 0.2507 0.048 Uiso 1 1 calc R U . . .
C4A C 0.8849(4) 0.5254(4) 0.3723(3) 0.0371(13) Uani 1 1 d . . . . .
H4A H 0.9535 0.5377 0.3667 0.045 Uiso 1 1 calc R U . . .
C5A C 0.8596(4) 0.6052(4) 0.4097(4) 0.0357(13) Uani 1 1 d . . . . .
C6A C 0.7591(4) 0.5862(4) 0.4266(4) 0.0472(15) Uani 1 1 d . . . . .
C7A C 0.7378(4) 0.6637(4) 0.4753(4) 0.0531(16) Uani 1 1 d . . . . .
H7A H 0.6717 0.6508 0.4886 0.064 Uiso 1 1 calc R U . . .
C8A C 0.8089(4) 0.7550(4) 0.5032(4) 0.0469(15) Uani 1 1 d . . . . .
H8A H 0.7920 0.8050 0.5356 0.056 Uiso 1 1 calc R U . . .
C9A C 0.9099(4) 0.7783(4) 0.4849(3) 0.0398(13) Uani 1 1 d . . . . .
C10A C 0.9355(4) 0.7043(4) 0.4385(4) 0.0364(13) Uani 1 1 d . . . . .
C11A C 1.0351(4) 0.7305(4) 0.4198(4) 0.0507(16) Uani 1 1 d . . . . .
H11A H 1.0538 0.6825 0.3861 0.061 Uiso 1 1 calc R U . . .
C12A C 1.1056(4) 0.8257(4) 0.4504(4) 0.0574(17) Uani 1 1 d . . . . .
H12A H 1.1723 0.8419 0.4375 0.069 Uiso 1 1 calc R U . . .
C13A C 1.0807(5) 0.8974(4) 0.4991(4) 0.0558(17) Uani 1 1 d . . . . .
H13A H 1.1303 0.9618 0.5212 0.067 Uiso 1 1 calc R U . . .
C14A C 0.9833(4) 0.8743(4) 0.5152(4) 0.0481(15) Uani 1 1 d . . . . .
H14A H 0.9653 0.9239 0.5472 0.058 Uiso 1 1 calc R U . . .
N1A N 0.8184(3) 0.4356(3) 0.3450(3) 0.0456(12) Uani 1 1 d . . . . .
H1A H 0.7542 0.4276 0.3432 0.055 Uiso 1 1 calc R U . . .
O1A O 0.6874(3) 0.4989(3) 0.4006(3) 0.0685(13) Uani 1 1 d . . . . .
C1B C 0.2706(3) 0.0734(3) 0.3144(3) 0.0244(11) Uani 1 1 d . . . . .
H1BA H 0.2066 0.0541 0.3386 0.029 Uiso 1 1 calc R U . . .
H1BB H 0.2954 0.1458 0.3170 0.029 Uiso 1 1 calc R U . . .
C2B C 0.2478(3) 0.0222(3) 0.2147(3) 0.0257(11) Uani 1 1 d . . . . .
H2BA H 0.3122 0.0354 0.1916 0.031 Uiso 1 1 calc R U . . .
H2BB H 0.2148 -0.0502 0.2106 0.031 Uiso 1 1 calc R U . . .
C3B C 0.1783(3) 0.0592(3) 0.1561(3) 0.0291(11) Uani 1 1 d . . . . .
H3BA H 0.1124 0.0427 0.1770 0.035 Uiso 1 1 calc R U . . .
H3BB H 0.2095 0.1320 0.1627 0.035 Uiso 1 1 calc R U . . .
C4B C 0.0803(3) -0.0616(3) 0.0207(3) 0.0278(11) Uani 1 1 d . . . . .
H4B H 0.0296 -0.0881 0.0555 0.033 Uiso 1 1 calc R U . . .
C5B C 0.0629(3) -0.1069(3) -0.0714(3) 0.0268(11) Uani 1 1 d . . . . .
C6B C 0.1352(4) -0.0639(3) -0.1275(3) 0.0303(11) Uani 1 1 d . . . . .
C7B C 0.1082(4) -0.1049(4) -0.2227(3) 0.0397(13) Uani 1 1 d . . . . .
H7B H 0.1523 -0.0753 -0.2619 0.048 Uiso 1 1 calc R U . . .
C8B C 0.0230(4) -0.1835(4) -0.2583(3) 0.0395(13) Uani 1 1 d . . . . .
H8B H 0.0083 -0.2075 -0.3218 0.047 Uiso 1 1 calc R U . . .
C9B C -0.0461(3) -0.2318(3) -0.2028(3) 0.0298(11) Uani 1 1 d . . . . .
C10B C -0.0258(3) -0.1947(3) -0.1087(3) 0.0254(11) Uani 1 1 d . . . . .
C11B C -0.0921(3) -0.2486(4) -0.0556(4) 0.0349(12) Uani 1 1 d . . . . .
H11B H -0.0789 -0.2270 0.0082 0.042 Uiso 1 1 calc R U . . .
C12B C -0.1753(4) -0.3317(4) -0.0945(4) 0.0407(14) Uani 1 1 d . . . . .
H12B H -0.2183 -0.3672 -0.0572 0.049 Uiso 1 1 calc R U . . .
C13B C -0.1977(4) -0.3650(4) -0.1882(4) 0.0445(14) Uani 1 1 d . . . . .
H13B H -0.2568 -0.4213 -0.2146 0.053 Uiso 1 1 calc R U . . .
C14B C -0.1342(4) -0.3162(4) -0.2417(4) 0.0446(14) Uani 1 1 d . . . . .
H14B H -0.1492 -0.3389 -0.3054 0.054 Uiso 1 1 calc R U . . .
N1B N 0.1614(3) 0.0141(3) 0.0610(2) 0.0297(9) Uani 1 1 d . . . . .
H1B H 0.2085 0.0393 0.0290 0.036 Uiso 1 1 calc R U . . .
O1B O 0.2188(3) 0.0080(2) -0.0960(2) 0.0404(9) Uani 1 1 d . . . . .
C1C C 0.3165(3) 0.1280(3) 0.6671(3) 0.0201(10) Uani 1 1 d . . . . .
H1CA H 0.3222 0.1928 0.6508 0.024 Uiso 1 1 calc R U . . .
H1CB H 0.2440 0.0840 0.6515 0.024 Uiso 1 1 calc R U . . .
C2C C 0.3517(3) 0.1422(3) 0.7691(3) 0.0223(10) Uani 1 1 d . . . . .
H2CA H 0.3392 0.0768 0.7869 0.027 Uiso 1 1 calc R U . . .
H2CB H 0.4257 0.1807 0.7844 0.027 Uiso 1 1 calc R U . . .
C3C C 0.2968(3) 0.1958(3) 0.8221(3) 0.0253(11) Uani 1 1 d . . . . .
H3CA H 0.3069 0.2600 0.8025 0.030 Uiso 1 1 calc R U . . .
H3CB H 0.2231 0.1559 0.8089 0.030 Uiso 1 1 calc R U . . .
C4C C 0.3670(3) 0.2987(3) 0.9725(3) 0.0268(11) Uani 1 1 d . . . . .
H4C H 0.3666 0.3539 0.9457 0.032 Uiso 1 1 calc R U . . .
C5C C 0.4036(3) 0.3169(3) 1.0669(3) 0.0217(10) Uani 1 1 d . . . . .
C6C C 0.4093(3) 0.2365(3) 1.1092(3) 0.0274(11) Uani 1 1 d . . . . .
C7C C 0.4492(3) 0.2591(3) 1.2050(3) 0.0292(11) Uani 1 1 d . . . . .
H7C H 0.4564 0.2079 1.2347 0.035 Uiso 1 1 calc R U . . .
C8C C 0.4763(3) 0.3500(4) 1.2536(3) 0.0317(12) Uani 1 1 d . . . . .
H8C H 0.5003 0.3606 1.3170 0.038 Uiso 1 1 calc R U . . .
C9C C 0.4706(3) 0.4319(3) 1.2135(3) 0.0262(11) Uani 1 1 d . . . . .
C10C C 0.4339(3) 0.4161(3) 1.1198(3) 0.0224(10) Uani 1 1 d . . . . .
C11C C 0.4266(3) 0.4979(3) 1.0827(3) 0.0283(11) Uani 1 1 d . . . . .
H11C H 0.4039 0.4903 1.0195 0.034 Uiso 1 1 calc R U . . .
C12C C 0.4522(3) 0.5885(3) 1.1373(3) 0.0277(11) Uani 1 1 d . . . . .
H12C H 0.4463 0.6424 1.1113 0.033 Uiso 1 1 calc R U . . .
C13C C 0.4867(3) 0.6023(3) 1.2302(3) 0.0325(12) Uani 1 1 d . . . . .
H13C H 0.5037 0.6652 1.2672 0.039 Uiso 1 1 calc R U . . .
C14C C 0.4960(3) 0.5257(4) 1.2681(3) 0.0338(12) Uani 1 1 d . . . . .
H14C H 0.5196 0.5352 1.3314 0.041 Uiso 1 1 calc R U . . .
N1C N 0.3339(3) 0.2129(3) 0.9190(2) 0.0257(9) Uani 1 1 d . . . . .
H1C H 0.3339 0.1614 0.9435 0.031 Uiso 1 1 calc R U . . .
O1C O 0.3813(2) 0.1493(2) 1.0645(2) 0.0322(8) Uani 1 1 d . . . . .
C1D C 0.7100(3) 0.2785(3) 0.6951(3) 0.0223(10) Uani 1 1 d . . . . .
H1DA H 0.7810 0.2900 0.6883 0.027 Uiso 1 1 calc R U . . .
H1DB H 0.6944 0.3355 0.6783 0.027 Uiso 1 1 calc R U . . .
C2D C 0.7013(3) 0.2748(3) 0.7942(3) 0.0255(11) Uani 1 1 d . . . . .
H2DA H 0.7189 0.2190 0.8115 0.031 Uiso 1 1 calc R U . . .
H2DB H 0.6298 0.2613 0.8006 0.031 Uiso 1 1 calc R U . . .
C3D C 0.7693(3) 0.3698(3) 0.8600(3) 0.0306(12) Uani 1 1 d . . . . .
H3DA H 0.7567 0.4272 0.8407 0.037 Uiso 1 1 calc R U . . .
H3DB H 0.7536 0.3657 0.9217 0.037 Uiso 1 1 calc R U . . .
C4D C 0.9534(3) 0.4665(4) 0.8763(3) 0.0300(11) Uani 1 1 d . . . . .
H4D H 0.9422 0.5266 0.8890 0.036 Uiso 1 1 calc R U . . .
C5D C 1.0539(3) 0.4705(3) 0.8747(3) 0.0253(11) Uani 1 1 d . . . . .
C6D C 1.0693(3) 0.3816(4) 0.8491(3) 0.0315(12) Uani 1 1 d . . . . .
C7D C 1.1698(4) 0.3868(4) 0.8375(3) 0.0369(13) Uani 1 1 d . . . . .
H7D H 1.1810 0.3280 0.8177 0.044 Uiso 1 1 calc R U . . .
C8D C 1.2479(4) 0.4750(4) 0.8546(3) 0.0338(12) Uani 1 1 d . . . . .
H8D H 1.3131 0.4765 0.8464 0.041 Uiso 1 1 calc R U . . .
C9D C 1.2367(3) 0.5661(4) 0.8846(3) 0.0287(11) Uani 1 1 d . . . . .
C10D C 1.1384(3) 0.5654(3) 0.8951(3) 0.0269(11) Uani 1 1 d . . . . .
C11D C 1.1316(3) 0.6570(3) 0.9246(3) 0.0309(12) Uani 1 1 d . . . . .
H11D H 1.0669 0.6589 0.9310 0.037 Uiso 1 1 calc R U . . .
C12D C 1.2152(4) 0.7449(4) 0.9447(3) 0.0365(13) Uani 1 1 d . . . . .
H12D H 1.2079 0.8053 0.9661 0.044 Uiso 1 1 calc R U . . .
C13D C 1.3106(4) 0.7438(4) 0.9334(4) 0.0403(13) Uani 1 1 d . . . . .
H13D H 1.3681 0.8038 0.9454 0.048 Uiso 1 1 calc R U . . .
C14D C 1.3203(4) 0.6559(4) 0.9050(3) 0.0391(13) Uani 1 1 d . . . . .
H14D H 1.3856 0.6557 0.8989 0.047 Uiso 1 1 calc R U . . .
N1D N 0.8758(3) 0.3826(3) 0.8608(2) 0.0288(9) Uani 1 1 d . . . . .
H1D H 0.8889 0.3284 0.8498 0.035 Uiso 1 1 calc R U . . .
O1D O 0.9968(2) 0.2961(2) 0.8339(2) 0.0431(10) Uani 1 1 d . . . . .
O1M O 1.0391(3) 0.1314(3) 0.8116(3) 0.0515(10) Uani 1 1 d . . . . .
H1M H 1.0220 0.1807 0.8191 0.077 Uiso 1 1 calc R U . . .
C1M C 1.0236(4) 0.0947(4) 0.7198(4) 0.0533(16) Uani 1 1 d . . . . .
H1MA H 1.0660 0.1454 0.6900 0.080 Uiso 1 1 calc R U . . .
H1MB H 0.9520 0.0768 0.6932 0.080 Uiso 1 1 calc R U . . .
H1MC H 1.0417 0.0360 0.7111 0.080 Uiso 1 1 calc R U . . .
O2M O 0.3995(8) -0.0331(7) 1.0580(7) 0.088(3) Uani 0.5 1 d D . P A 1
H2M H 0.3941 0.0230 1.0595 0.133 Uiso 0.5 1 d R U P A 1
C2M C 0.487(3) -0.0187(17) 1.121(4) 0.086(3) Uani 0.5 1 d D . P A 1
H2MA H 0.4800 0.0100 1.1814 0.128 Uiso 0.5 1 calc R U P A 1
H2MB H 0.5466 0.0262 1.1030 0.128 Uiso 0.5 1 calc R U P A 1
H2MC H 0.4938 -0.0824 1.1242 0.128 Uiso 0.5 1 calc R U P A 1
O3M O 0.5074(9) 0.0590(8) 1.1429(9) 0.110(4) Uani 0.5 1 d D . P B 2
H3M H 0.5004 0.0865 1.0984 0.165 Uiso 0.5 1 d R U P B 2
C3M C 0.475(4) -0.0427(16) 1.112(4) 0.086(3) Uani 0.5 1 d D . P B 2
H3MA H 0.4648 -0.0774 1.1636 0.128 Uiso 0.5 1 calc R U P B 2
H3MB H 0.5260 -0.0573 1.0818 0.128 Uiso 0.5 1 calc R U P B 2
H3MC H 0.4106 -0.0649 1.0690 0.128 Uiso 0.5 1 calc R U P B 2
O4M O 0.5360(6) 0.4418(5) 0.4977(6) 0.055(2) Uani 0.5 1 d D . P C 3
H4M H 0.5943 0.4728 0.4878 0.083 Uiso 0.5 1 d R U P C 3
C4M C 0.5304(8) 0.3497(7) 0.5157(9) 0.033(3) Uani 0.5 1 d D . P C 3
H4MA H 0.5991 0.3494 0.5301 0.050 Uiso 0.5 1 calc R U P C 3
H4MB H 0.4923 0.2989 0.4624 0.050 Uiso 0.5 1 calc R U P C 3
H4MC H 0.4960 0.3358 0.5674 0.050 Uiso 0.5 1 calc R U P C 3
O5M O 0.6349(16) 0.4058(16) 0.5244(15) 0.070(6) Uiso 0.2 1 d D . P D 4
H5M H 0.6405 0.3514 0.5079 0.104 Uiso 0.2 1 d R U P D 4
C5M C 0.5327(19) 0.392(4) 0.511(4) 0.084(19) Uiso 0.2 1 d D . P D 4
H5MA H 0.4926 0.3250 0.5182 0.127 Uiso 0.2 1 calc R U P D 4
H5MB H 0.5116 0.4026 0.4505 0.127 Uiso 0.2 1 calc R U P D 4
H5MC H 0.5219 0.4400 0.5566 0.127 Uiso 0.2 1 calc R U P D 4
C6M C 0.100(4) 0.493(4) 0.420(3) 0.041(11) Uiso 0.1 1 d D . P E 5
H6MA H 0.0623 0.4227 0.4198 0.061 Uiso 0.1 1 calc R U P E 5
H6MB H 0.0713 0.5331 0.4565 0.061 Uiso 0.1 1 calc R U P E 5
H6MC H 0.1713 0.5102 0.4459 0.061 Uiso 0.1 1 calc R U P E 5
O6M O 0.091(3) 0.511(3) 0.331(2) 0.071(13) Uiso 0.1 1 d D . P E 5
H6M H 0.0623 0.4567 0.2948 0.106 Uiso 0.1 1 calc R U P E 5
C7M C 0.170(4) 0.516(5) 0.404(4) 0.041(11) Uiso 0.1 1 d D . P F 6
H7MA H 0.1302 0.5138 0.3455 0.061 Uiso 0.1 1 d R U P F 6
H7MB H 0.1765 0.5747 0.4465 0.061 Uiso 0.1 1 d R U P F 6
H7MC H 0.1364 0.4564 0.4282 0.061 Uiso 0.1 1 d R U P F 6
O7M O 0.264(4) 0.516(5) 0.386(4) 0.13(2) Uiso 0.1 1 d D . P F 6
H7M H 0.2633 0.4578 0.3777 0.192 Uiso 0.1 1 d R U P F 6
C8M C 0.137(3) 0.489(2) 0.376(3) 0.050(12) Uiso 0.15 1 d D . P G 7
H8MA H 0.1091 0.4954 0.3158 0.075 Uiso 0.15 1 calc R U P G 7
H8MB H 0.0876 0.4329 0.3956 0.075 Uiso 0.15 1 calc R U P G 7
H8MC H 0.2003 0.4779 0.3750 0.075 Uiso 0.15 1 calc R U P G 7
O8M O 0.1550(19) 0.5753(18) 0.4374(16) 0.053(7) Uiso 0.15 1 d D . P G 7
H8M H 0.1717 0.6238 0.4104 0.080 Uiso 0.15 1 d R U P G 7


_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 Si4 1.619(3) . ?
O1 Si1 1.623(3) . ?
O2 Si1 1.622(3) . ?
O2 Si2 1.625(3) . ?
O3 Si3 1.618(3) . ?
O3 Si2 1.628(3) . ?
O4 Si3 1.625(3) . ?
O4 Si4 1.625(3) . ?
O5 Si3 1.619(3) 2_656 ?
O5 Si1 1.623(3) . ?
O6 Si4 1.615(3) 2_656 ?
O6 Si2 1.627(3) . ?
Si1 C1A 1.844(4) . ?
Si2 C1B 1.837(4) . ?
Si3 O5 1.619(3) 2_656 ?
Si3 C1C 1.841(4) . ?
Si4 O6 1.615(3) 2_656 ?
Si4 C1D 1.842(4) . ?
C1A C2A 1.535(6) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A C3A 1.526(6) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A N1A 1.463(6) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A N1A 1.304(6) . ?
C4A C5A 1.414(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.428(7) . ?
C5A C10A 1.451(6) . ?
C6A O1A 1.305(6) . ?
C6A C7A 1.419(7) . ?
C7A C8A 1.344(7) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.433(7) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.398(7) . ?
C9A C14A 1.409(7) . ?
C10A C11A 1.413(7) . ?
C11A C12A 1.386(7) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.380(8) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.374(7) . ?
C13A H13A 0.9500 . ?
C14A H14A 0.9500 . ?
N1A H1A 0.8800 . ?
C1B C2B 1.538(6) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B C3B 1.530(6) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B N1B 1.458(5) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B N1B 1.306(5) . ?
C4B C5B 1.417(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.443(6) . ?
C5B C10B 1.445(6) . ?
C6B O1B 1.273(5) . ?
C6B C7B 1.436(6) . ?
C7B C8B 1.344(6) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.430(7) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.413(6) . ?
C9B C14B 1.419(6) . ?
C10B C11B 1.411(6) . ?
C11B C12B 1.372(6) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.398(7) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.364(7) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?
N1B H1B 0.8800 . ?
C1C C2C 1.524(6) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.519(5) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C N1C 1.454(5) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C N1C 1.303(5) . ?
C4C C5C 1.415(6) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.430(6) . ?
C5C C10C 1.458(6) . ?
C6C O1C 1.270(5) . ?
C6C C7C 1.440(6) . ?
C7C C8C 1.338(6) . ?
C7C H7C 0.9500 . ?
C8C C9C 1.432(6) . ?
C8C H8C 0.9500 . ?
C9C C10C 1.408(6) . ?
C9C C14C 1.414(6) . ?
C10C C11C 1.416(6) . ?
C11C C12C 1.375(6) . ?
C11C H11C 0.9500 . ?
C12C C13C 1.393(6) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.362(7) . ?
C13C H13C 0.9500 . ?
C14C H14C 0.9500 . ?
N1C H1C 0.8800 . ?
C1D C2D 1.524(6) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D C3D 1.531(6) . ?
C2D H2DA 0.9900 . ?
C2D H2DB 0.9900 . ?
C3D N1D 1.466(5) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4D N1D 1.307(5) . ?
C4D C5D 1.421(6) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.411(6) . ?
C5D C10D 1.456(6) . ?
C6D O1D 1.289(5) . ?
C6D C7D 1.446(6) . ?
C7D C8D 1.351(6) . ?
C7D H7D 0.9500 . ?
C8D C9D 1.425(6) . ?
C8D H8D 0.9500 . ?
C9D C14D 1.403(6) . ?
C9D C10D 1.429(6) . ?
C10D C11D 1.402(6) . ?
C11D C12D 1.386(6) . ?
C11D H11D 0.9500 . ?
C12D C13D 1.400(6) . ?
C12D H12D 0.9500 . ?
C13D C14D 1.366(7) . ?
C13D H13D 0.9500 . ?
C14D H14D 0.9500 . ?
N1D H1D 0.8800 . ?
O1M C1M 1.385(6) . ?
O1M H1M 0.8400 . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
O2M C2M 1.408(10) . ?
O2M H2M 0.8509 . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
O3M C3M 1.395(10) . ?
O3M H3M 0.8397 . ?
C3M H3MA 0.9800 . ?
C3M H3MB 0.9800 . ?
C3M H3MC 0.9800 . ?
O4M C4M 1.387(9) . ?
O4M H4M 0.8407 . ?
C4M H4MA 0.9800 . ?
C4M H4MB 0.9800 . ?
C4M H4MC 0.9800 . ?
O5M C5M 1.389(10) . ?
O5M H5M 0.8397 . ?
C5M H5MA 0.9800 . ?
C5M H5MB 0.9800 . ?
C5M H5MC 0.9800 . ?
C6M O6M 1.399(10) . ?
C6M H6MA 0.9800 . ?
C6M H6MB 0.9800 . ?
C6M H6MC 0.9800 . ?
O6M H6M 0.8400 . ?
C7M O7M 1.406(10) . ?
C7M H7MA 0.9802 . ?
C7M H7MB 0.9798 . ?
C7M H7MC 0.9799 . ?
O7M H7M 0.8400 . ?
C8M O8M 1.392(10) . ?
C8M H8MA 0.9800 . ?
C8M H8MB 0.9800 . ?
C8M H8MC 0.9800 . ?
O8M H8M 0.8400 . ?

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
Si4 O1 Si1 150.1(2) . . ?
Si1 O2 Si2 149.0(2) . . ?
Si3 O3 Si2 148.82(19) . . ?
Si3 O4 Si4 148.52(19) . . ?
Si3 O5 Si1 148.37(19) 2_656 . ?
Si4 O6 Si2 148.5(2) 2_656 . ?
O2 Si1 O5 109.76(16) . . ?
O2 Si1 O1 108.79(16) . . ?
O5 Si1 O1 108.56(16) . . ?
O2 Si1 C1A 109.66(18) . . ?
O5 Si1 C1A 110.37(18) . . ?
O1 Si1 C1A 109.66(19) . . ?
O2 Si2 O6 109.01(16) . . ?
O2 Si2 O3 109.42(16) . . ?
O6 Si2 O3 109.20(16) . . ?
O2 Si2 C1B 111.08(19) . . ?
O6 Si2 C1B 109.77(19) . . ?
O3 Si2 C1B 108.34(18) . . ?
O3 Si3 O5 109.48(16) . 2_656 ?
O3 Si3 O4 109.64(16) . . ?
O5 Si3 O4 109.15(16) 2_656 . ?
O3 Si3 C1C 109.59(17) . . ?
O5 Si3 C1C 110.37(18) 2_656 . ?
O4 Si3 C1C 108.60(18) . . ?
O6 Si4 O1 109.11(15) 2_656 . ?
O6 Si4 O4 109.26(16) 2_656 . ?
O1 Si4 O4 109.39(16) . . ?
O6 Si4 C1D 109.39(18) 2_656 . ?
O1 Si4 C1D 110.67(18) . . ?
O4 Si4 C1D 109.00(18) . . ?
C2A C1A Si1 113.9(3) . . ?
C2A C1A H1AA 108.8 . . ?
Si1 C1A H1AA 108.8 . . ?
C2A C1A H1AB 108.8 . . ?
Si1 C1A H1AB 108.8 . . ?
H1AA C1A H1AB 107.7 . . ?
C3A C2A C1A 113.3(4) . . ?
C3A C2A H2AA 108.9 . . ?
C1A C2A H2AA 108.9 . . ?
C3A C2A H2AB 108.9 . . ?
C1A C2A H2AB 108.9 . . ?
H2AA C2A H2AB 107.7 . . ?
N1A C3A C2A 109.6(4) . . ?
N1A C3A H3AA 109.7 . . ?
C2A C3A H3AA 109.7 . . ?
N1A C3A H3AB 109.7 . . ?
C2A C3A H3AB 109.7 . . ?
H3AA C3A H3AB 108.2 . . ?
N1A C4A C5A 123.1(5) . . ?
N1A C4A H4A 118.5 . . ?
C5A C4A H4A 118.5 . . ?
C4A C5A C6A 119.2(4) . . ?
C4A C5A C10A 121.6(4) . . ?
C6A C5A C10A 119.1(5) . . ?
O1A C6A C7A 119.5(5) . . ?
O1A C6A C5A 121.6(5) . . ?
C7A C6A C5A 118.9(5) . . ?
C8A C7A C6A 121.7(5) . . ?
C8A C7A H7A 119.2 . . ?
C6A C7A H7A 119.2 . . ?
C7A C8A C9A 121.3(5) . . ?
C7A C8A H8A 119.3 . . ?
C9A C8A H8A 119.3 . . ?
C10A C9A C14A 120.2(5) . . ?
C10A C9A C8A 119.4(5) . . ?
C14A C9A C8A 120.3(5) . . ?
C9A C10A C11A 117.9(5) . . ?
C9A C10A C5A 119.5(5) . . ?
C11A C10A C5A 122.6(5) . . ?
C12A C11A C10A 120.5(5) . . ?
C12A C11A H11A 119.8 . . ?
C10A C11A H11A 119.8 . . ?
C13A C12A C11A 121.2(6) . . ?
C13A C12A H12A 119.4 . . ?
C11A C12A H12A 119.4 . . ?
C14A C13A C12A 119.2(5) . . ?
C14A C13A H13A 120.4 . . ?
C12A C13A H13A 120.4 . . ?
C13A C14A C9A 120.9(5) . . ?
C13A C14A H14A 119.5 . . ?
C9A C14A H14A 119.5 . . ?
C4A N1A C3A 126.3(4) . . ?
C4A N1A H1A 116.9 . . ?
C3A N1A H1A 116.9 . . ?
C2B C1B Si2 114.4(3) . . ?
C2B C1B H1BA 108.7 . . ?
Si2 C1B H1BA 108.7 . . ?
C2B C1B H1BB 108.7 . . ?
Si2 C1B H1BB 108.7 . . ?
H1BA C1B H1BB 107.6 . . ?
C3B C2B C1B 111.2(4) . . ?
C3B C2B H2BA 109.4 . . ?
C1B C2B H2BA 109.4 . . ?
C3B C2B H2BB 109.4 . . ?
C1B C2B H2BB 109.4 . . ?
H2BA C2B H2BB 108.0 . . ?
N1B C3B C2B 110.7(4) . . ?
N1B C3B H3BA 109.5 . . ?
C2B C3B H3BA 109.5 . . ?
N1B C3B H3BB 109.5 . . ?
C2B C3B H3BB 109.5 . . ?
H3BA C3B H3BB 108.1 . . ?
N1B C4B C5B 124.4(4) . . ?
N1B C4B H4B 117.8 . . ?
C5B C4B H4B 117.8 . . ?
C4B C5B C6B 119.0(4) . . ?
C4B C5B C10B 120.6(4) . . ?
C6B C5B C10B 120.4(4) . . ?
O1B C6B C7B 120.4(4) . . ?
O1B C6B C5B 122.7(4) . . ?
C7B C6B C5B 116.9(4) . . ?
C8B C7B C6B 122.4(5) . . ?
C8B C7B H7B 118.8 . . ?
C6B C7B H7B 118.8 . . ?
C7B C8B C9B 121.5(5) . . ?
C7B C8B H8B 119.3 . . ?
C9B C8B H8B 119.3 . . ?
C10B C9B C14B 120.1(5) . . ?
C10B C9B C8B 119.5(4) . . ?
C14B C9B C8B 120.5(5) . . ?
C11B C10B C9B 117.5(4) . . ?
C11B C10B C5B 123.6(4) . . ?
C9B C10B C5B 118.9(4) . . ?
C12B C11B C10B 121.2(5) . . ?
C12B C11B H11B 119.4 . . ?
C10B C11B H11B 119.4 . . ?
C11B C12B C13B 120.9(5) . . ?
C11B C12B H12B 119.6 . . ?
C13B C12B H12B 119.6 . . ?
C14B C13B C12B 119.7(5) . . ?
C14B C13B H13B 120.2 . . ?
C12B C13B H13B 120.2 . . ?
C13B C14B C9B 120.5(5) . . ?
C13B C14B H14B 119.8 . . ?
C9B C14B H14B 119.8 . . ?
C4B N1B C3B 123.6(4) . . ?
C4B N1B H1B 118.2 . . ?
C3B N1B H1B 118.2 . . ?
C2C C1C Si3 113.4(3) . . ?
C2C C1C H1CA 108.9 . . ?
Si3 C1C H1CA 108.9 . . ?
C2C C1C H1CB 108.9 . . ?
Si3 C1C H1CB 108.9 . . ?
H1CA C1C H1CB 107.7 . . ?
C3C C2C C1C 111.5(3) . . ?
C3C C2C H2CA 109.3 . . ?
C1C C2C H2CA 109.3 . . ?
C3C C2C H2CB 109.3 . . ?
C1C C2C H2CB 109.3 . . ?
H2CA C2C H2CB 108.0 . . ?
N1C C3C C2C 111.3(3) . . ?
N1C C3C H3CA 109.4 . . ?
C2C C3C H3CA 109.4 . . ?
N1C C3C H3CB 109.4 . . ?
C2C C3C H3CB 109.4 . . ?
H3CA C3C H3CB 108.0 . . ?
N1C C4C C5C 125.7(4) . . ?
N1C C4C H4C 117.2 . . ?
C5C C4C H4C 117.2 . . ?
C4C C5C C6C 118.9(4) . . ?
C4C C5C C10C 120.1(4) . . ?
C6C C5C C10C 121.0(4) . . ?
O1C C6C C5C 121.8(4) . . ?
O1C C6C C7C 121.3(4) . . ?
C5C C6C C7C 116.9(4) . . ?
C8C C7C C6C 122.1(4) . . ?
C8C C7C H7C 119.0 . . ?
C6C C7C H7C 119.0 . . ?
C7C C8C C9C 122.4(4) . . ?
C7C C8C H8C 118.8 . . ?
C9C C8C H8C 118.8 . . ?
C10C C9C C14C 120.6(4) . . ?
C10C C9C C8C 118.9(4) . . ?
C14C C9C C8C 120.4(4) . . ?
C9C C10C C11C 117.5(4) . . ?
C9C C10C C5C 118.7(4) . . ?
C11C C10C C5C 123.8(4) . . ?
C12C C11C C10C 120.7(5) . . ?
C12C C11C H11C 119.6 . . ?
C10C C11C H11C 119.6 . . ?
C11C C12C C13C 121.0(4) . . ?
C11C C12C H12C 119.5 . . ?
C13C C12C H12C 119.5 . . ?
C14C C13C C12C 119.9(4) . . ?
C14C C13C H13C 120.0 . . ?
C12C C13C H13C 120.0 . . ?
C13C C14C C9C 120.3(5) . . ?
C13C C14C H14C 119.9 . . ?
C9C C14C H14C 119.9 . . ?
C4C N1C C3C 124.8(4) . . ?
C4C N1C H1C 117.6 . . ?
C3C N1C H1C 117.6 . . ?
C2D C1D Si4 114.0(3) . . ?
C2D C1D H1DA 108.7 . . ?
Si4 C1D H1DA 108.7 . . ?
C2D C1D H1DB 108.7 . . ?
Si4 C1D H1DB 108.7 . . ?
H1DA C1D H1DB 107.6 . . ?
C1D C2D C3D 114.0(4) . . ?
C1D C2D H2DA 108.7 . . ?
C3D C2D H2DA 108.7 . . ?
C1D C2D H2DB 108.7 . . ?
C3D C2D H2DB 108.7 . . ?
H2DA C2D H2DB 107.6 . . ?
N1D C3D C2D 109.2(4) . . ?
N1D C3D H3DA 109.8 . . ?
C2D C3D H3DA 109.8 . . ?
N1D C3D H3DB 109.8 . . ?
C2D C3D H3DB 109.8 . . ?
H3DA C3D H3DB 108.3 . . ?
N1D C4D C5D 122.0(4) . . ?
N1D C4D H4D 119.0 . . ?
C5D C4D H4D 119.0 . . ?
C6D C5D C4D 118.8(4) . . ?
C6D C5D C10D 121.0(4) . . ?
C4D C5D C10D 120.1(4) . . ?
O1D C6D C5D 122.6(4) . . ?
O1D C6D C7D 118.7(4) . . ?
C5D C6D C7D 118.7(4) . . ?
C8D C7D C6D 120.2(5) . . ?
C8D C7D H7D 119.9 . . ?
C6D C7D H7D 119.9 . . ?
C7D C8D C9D 123.0(4) . . ?
C7D C8D H8D 118.5 . . ?
C9D C8D H8D 118.5 . . ?
C14D C9D C8D 121.2(4) . . ?
C14D C9D C10D 119.6(5) . . ?
C8D C9D C10D 119.2(4) . . ?
C11D C10D C9D 116.9(4) . . ?
C11D C10D C5D 125.3(4) . . ?
C9D C10D C5D 117.9(4) . . ?
C12D C11D C10D 122.7(4) . . ?
C12D C11D H11D 118.7 . . ?
C10D C11D H11D 118.7 . . ?
C11D C12D C13D 119.4(5) . . ?
C11D C12D H12D 120.3 . . ?
C13D C12D H12D 120.3 . . ?
C14D C13D C12D 119.6(5) . . ?
C14D C13D H13D 120.2 . . ?
C12D C13D H13D 120.2 . . ?
C13D C14D C9D 121.8(5) . . ?
C13D C14D H14D 119.1 . . ?
C9D C14D H14D 119.1 . . ?
C4D N1D C3D 126.6(4) . . ?
C4D N1D H1D 116.7 . . ?
C3D N1D H1D 116.7 . . ?
C1M O1M H1M 109.5 . . ?
O1M C1M H1MA 109.5 . . ?
O1M C1M H1MB 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
O1M C1M H1MC 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
C2M O2M H2M 106.8 . . ?
O2M C2M H2MA 109.5 . . ?
O2M C2M H2MB 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
O2M C2M H2MC 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C3M O3M H3M 108.7 . . ?
O3M C3M H3MA 109.5 . . ?
O3M C3M H3MB 109.5 . . ?
H3MA C3M H3MB 109.5 . . ?
O3M C3M H3MC 109.5 . . ?
H3MA C3M H3MC 109.5 . . ?
H3MB C3M H3MC 109.5 . . ?
C4M O4M H4M 109.4 . . ?
O4M C4M H4MA 109.5 . . ?
O4M C4M H4MB 109.5 . . ?
H4MA C4M H4MB 109.5 . . ?
O4M C4M H4MC 109.5 . . ?
H4MA C4M H4MC 109.5 . . ?
H4MB C4M H4MC 109.5 . . ?
C5M O5M H5M 109.1 . . ?
O5M C5M H5MA 109.5 . . ?
O5M C5M H5MB 109.5 . . ?
H5MA C5M H5MB 109.5 . . ?
O5M C5M H5MC 109.5 . . ?
H5MA C5M H5MC 109.5 . . ?
H5MB C5M H5MC 109.5 . . ?
O6M C6M H6MA 109.5 . . ?
O6M C6M H6MB 109.5 . . ?
H6MA C6M H6MB 109.5 . . ?
O6M C6M H6MC 109.5 . . ?
H6MA C6M H6MC 109.5 . . ?
H6MB C6M H6MC 109.5 . . ?
C6M O6M H6M 109.5 . . ?
O7M C7M H7MA 106.3 . . ?
O7M C7M H7MB 112.9 . . ?
H7MA C7M H7MB 109.5 . . ?
O7M C7M H7MC 109.1 . . ?
H7MA C7M H7MC 109.5 . . ?
H7MB C7M H7MC 109.5 . . ?
C7M O7M H7M 109.9 . . ?
O8M C8M H8MA 109.5 . . ?
O8M C8M H8MB 109.5 . . ?
H8MA C8M H8MB 109.5 . . ?
O8M C8M H8MC 109.5 . . ?
H8MA C8M H8MC 109.5 . . ?
H8MB C8M H8MC 109.5 . . ?
C8M O8M H8M 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si2 O2 Si1 O5 58.5(4) . . . . ?
Si2 O2 Si1 O1 -60.2(4) . . . . ?
Si2 O2 Si1 C1A 179.9(3) . . . . ?
Si3 O5 Si1 O2 -60.1(4) 2_656 . . . ?
Si3 O5 Si1 O1 58.7(4) 2_656 . . . ?
Si3 O5 Si1 C1A 178.9(4) 2_656 . . . ?
Si4 O1 Si1 O2 57.9(4) . . . . ?
Si4 O1 Si1 O5 -61.5(4) . . . . ?
Si4 O1 Si1 C1A 177.9(4) . . . . ?
Si1 O2 Si2 O6 -58.5(4) . . . . ?
Si1 O2 Si2 O3 60.8(4) . . . . ?
Si1 O2 Si2 C1B -179.6(4) . . . . ?
Si4 O6 Si2 O2 61.2(4) 2_656 . . . ?
Si4 O6 Si2 O3 -58.3(4) 2_656 . . . ?
Si4 O6 Si2 C1B -176.9(3) 2_656 . . . ?
Si3 O3 Si2 O2 -58.2(4) . . . . ?
Si3 O3 Si2 O6 61.0(4) . . . . ?
Si3 O3 Si2 C1B -179.4(4) . . . . ?
Si2 O3 Si3 O5 -61.4(4) . . . 2_656 ?
Si2 O3 Si3 O4 58.3(4) . . . . ?
Si2 O3 Si3 C1C 177.4(4) . . . . ?
Si4 O4 Si3 O3 -59.9(4) . . . . ?
Si4 O4 Si3 O5 60.1(4) . . . 2_656 ?
Si4 O4 Si3 C1C -179.6(4) . . . . ?
Si1 O1 Si4 O6 61.5(4) . . . 2_656 ?
Si1 O1 Si4 O4 -58.0(4) . . . . ?
Si1 O1 Si4 C1D -178.1(4) . . . . ?
Si3 O4 Si4 O6 -60.2(4) . . . 2_656 ?
Si3 O4 Si4 O1 59.2(4) . . . . ?
Si3 O4 Si4 C1D -179.6(4) . . . . ?
O2 Si1 C1A C2A 175.8(3) . . . . ?
O5 Si1 C1A C2A -63.2(4) . . . . ?
O1 Si1 C1A C2A 56.4(4) . . . . ?
Si1 C1A C2A C3A -176.8(3) . . . . ?
C1A C2A C3A N1A 65.5(5) . . . . ?
N1A C4A C5A C6A 6.1(8) . . . . ?
N1A C4A C5A C10A -179.4(5) . . . . ?
C4A C5A C6A O1A -6.7(8) . . . . ?
C10A C5A C6A O1A 178.6(5) . . . . ?
C4A C5A C6A C7A 171.5(5) . . . . ?
C10A C5A C6A C7A -3.2(8) . . . . ?
O1A C6A C7A C8A -179.6(6) . . . . ?
C5A C6A C7A C8A 2.2(9) . . . . ?
C6A C7A C8A C9A 0.0(9) . . . . ?
C7A C8A C9A C10A -1.1(8) . . . . ?
C7A C8A C9A C14A -179.6(5) . . . . ?
C14A C9A C10A C11A -2.8(8) . . . . ?
C8A C9A C10A C11A 178.6(5) . . . . ?
C14A C9A C10A C5A 178.5(5) . . . . ?
C8A C9A C10A C5A -0.1(8) . . . . ?
C4A C5A C10A C9A -172.4(5) . . . . ?
C6A C5A C10A C9A 2.2(8) . . . . ?
C4A C5A C10A C11A 9.0(8) . . . . ?
C6A C5A C10A C11A -176.4(5) . . . . ?
C9A C10A C11A C12A 2.7(8) . . . . ?
C5A C10A C11A C12A -178.7(5) . . . . ?
C10A C11A C12A C13A -0.4(9) . . . . ?
C11A C12A C13A C14A -1.9(9) . . . . ?
C12A C13A C14A C9A 1.8(9) . . . . ?
C10A C9A C14A C13A 0.6(8) . . . . ?
C8A C9A C14A C13A 179.2(5) . . . . ?
C5A C4A N1A C3A -171.3(5) . . . . ?
C2A C3A N1A C4A 130.1(5) . . . . ?
O2 Si2 C1B C2B 79.1(3) . . . . ?
O6 Si2 C1B C2B -41.5(4) . . . . ?
O3 Si2 C1B C2B -160.7(3) . . . . ?
Si2 C1B C2B C3B -173.6(3) . . . . ?
C1B C2B C3B N1B 177.0(4) . . . . ?
N1B C4B C5B C6B -4.3(7) . . . . ?
N1B C4B C5B C10B 175.6(4) . . . . ?
C4B C5B C6B O1B 6.3(7) . . . . ?
C10B C5B C6B O1B -173.6(4) . . . . ?
C4B C5B C6B C7B -172.5(4) . . . . ?
C10B C5B C6B C7B 7.6(7) . . . . ?
O1B C6B C7B C8B 177.0(5) . . . . ?
C5B C6B C7B C8B -4.1(7) . . . . ?
C6B C7B C8B C9B -0.5(8) . . . . ?
C7B C8B C9B C10B 1.7(7) . . . . ?
C7B C8B C9B C14B -178.4(5) . . . . ?
C14B C9B C10B C11B 4.3(7) . . . . ?
C8B C9B C10B C11B -175.7(4) . . . . ?
C14B C9B C10B C5B -178.1(4) . . . . ?
C8B C9B C10B C5B 1.8(7) . . . . ?
C4B C5B C10B C11B -9.0(7) . . . . ?
C6B C5B C10B C11B 170.8(4) . . . . ?
C4B C5B C10B C9B 173.6(4) . . . . ?
C6B C5B C10B C9B -6.6(6) . . . . ?
C9B C10B C11B C12B -2.5(7) . . . . ?
C5B C10B C11B C12B -179.9(4) . . . . ?
C10B C11B C12B C13B -0.8(7) . . . . ?
C11B C12B C13B C14B 2.2(8) . . . . ?
C12B C13B C14B C9B -0.3(8) . . . . ?
C10B C9B C14B C13B -3.0(7) . . . . ?
C8B C9B C14B C13B 177.0(5) . . . . ?
C5B C4B N1B C3B -179.6(4) . . . . ?
C2B C3B N1B C4B 99.2(5) . . . . ?
O3 Si3 C1C C2C -175.6(3) . . . . ?
O5 Si3 C1C C2C 63.7(3) 2_656 . . . ?
O4 Si3 C1C C2C -55.9(3) . . . . ?
Si3 C1C C2C C3C 174.2(3) . . . . ?
C1C C2C C3C N1C -177.6(3) . . . . ?
N1C C4C C5C C6C 2.5(7) . . . . ?
N1C C4C C5C C10C -176.9(4) . . . . ?
C4C C5C C6C O1C -0.8(6) . . . . ?
C10C C5C C6C O1C 178.6(4) . . . . ?
C4C C5C C6C C7C 178.6(4) . . . . ?
C10C C5C C6C C7C -2.0(6) . . . . ?
O1C C6C C7C C8C -178.1(4) . . . . ?
C5C C6C C7C C8C 2.5(7) . . . . ?
C6C C7C C8C C9C -1.9(7) . . . . ?
C7C C8C C9C C10C 0.9(7) . . . . ?
C7C C8C C9C C14C 177.3(4) . . . . ?
C14C C9C C10C C11C 2.0(6) . . . . ?
C8C C9C C10C C11C 178.3(4) . . . . ?
C14C C9C C10C C5C -176.8(4) . . . . ?
C8C C9C C10C C5C -0.4(6) . . . . ?
C4C C5C C10C C9C -179.6(4) . . . . ?
C6C C5C C10C C9C 1.1(6) . . . . ?
C4C C5C C10C C11C 1.7(6) . . . . ?
C6C C5C C10C C11C -177.6(4) . . . . ?
C9C C10C C11C C12C -1.7(6) . . . . ?
C5C C10C C11C C12C 177.0(4) . . . . ?
C10C C11C C12C C13C 0.6(7) . . . . ?
C11C C12C C13C C14C 0.4(7) . . . . ?
C12C C13C C14C C9C -0.1(7) . . . . ?
C10C C9C C14C C13C -1.1(7) . . . . ?
C8C C9C C14C C13C -177.4(4) . . . . ?
C5C C4C N1C C3C -179.8(4) . . . . ?
C2C C3C N1C C4C 126.3(4) . . . . ?
O6 Si4 C1D C2D -62.9(3) 2_656 . . . ?
O1 Si4 C1D C2D 176.8(3) . . . . ?
O4 Si4 C1D C2D 56.5(4) . . . . ?
Si4 C1D C2D C3D -178.3(3) . . . . ?
C1D C2D C3D N1D -66.7(5) . . . . ?
N1D C4D C5D C6D 4.7(7) . . . . ?
N1D C4D C5D C10D -178.1(4) . . . . ?
C4D C5D C6D O1D -5.4(7) . . . . ?
C10D C5D C6D O1D 177.4(4) . . . . ?
C4D C5D C6D C7D 173.0(4) . . . . ?
C10D C5D C6D C7D -4.2(7) . . . . ?
O1D C6D C7D C8D -178.7(5) . . . . ?
C5D C6D C7D C8D 2.8(7) . . . . ?
C6D C7D C8D C9D 0.1(8) . . . . ?
C7D C8D C9D C14D 177.6(5) . . . . ?
C7D C8D C9D C10D -1.6(7) . . . . ?
C14D C9D C10D C11D 0.9(7) . . . . ?
C8D C9D C10D C11D -179.9(4) . . . . ?
C14D C9D C10D C5D -179.0(4) . . . . ?
C8D C9D C10D C5D 0.2(7) . . . . ?
C6D C5D C10D C11D -177.2(4) . . . . ?
C4D C5D C10D C11D 5.7(7) . . . . ?
C6D C5D C10D C9D 2.7(7) . . . . ?
C4D C5D C10D C9D -174.5(4) . . . . ?
C9D C10D C11D C12D -1.2(7) . . . . ?
C5D C10D C11D C12D 178.6(5) . . . . ?
C10D C11D C12D C13D 1.7(8) . . . . ?
C11D C12D C13D C14D -1.8(8) . . . . ?
C12D C13D C14D C9D 1.5(8) . . . . ?
C8D C9D C14D C13D 179.7(5) . . . . ?
C10D C9D C14D C13D -1.1(8) . . . . ?
C5D C4D N1D C3D -179.5(4) . . . . ?
C2D C3D N1D C4D 150.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2A H2AA O8M 0.99 2.45 3.35(2) 150.1 2_666
C4B H4B O1M 0.95 2.40 3.299(6) 157.3 2_656
N1B H1B O1C 0.88 2.38 3.066(5) 134.9 1_554
C3C H3CB O1M 0.99 2.53 3.446(6) 153.1 1_455
N1C H1C O1B 0.88 2.23 2.842(5) 126.6 1_556
C4A H4A O6M 0.95 2.26 3.16(4) 159.9 1_655
N1A H1A O1A 0.88 1.85 2.546(6) 134.1 .
N1B H1B O1B 0.88 1.92 2.606(5) 133.2 .
N1C H1C O1C 0.88 1.92 2.595(5) 132.2 .
N1D H1D O1D 0.88 1.80 2.519(5) 137.6 .
O1M H1M O1D 0.84 1.84 2.679(5) 174.4 .
O2M H2M O1C 0.85 1.92 2.767(9) 179.1 .
O3M H3M O1C 0.84 2.24 2.815(12) 126.3 .
O4M H4M O1A 0.84 1.96 2.715(9) 148.0 .
O5M H5M O1 0.84 2.52 3.32(2) 159.0 .

_refine_diff_density_max         0.461
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.072


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method methanol
####################################################################### 
# 
# 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_mj517a
_database_code_depnum_ccdc_archive 'CCDC 1456561'
_audit_update_record             
;
2016-06-20 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H86 N16 O28 Si8, 4(C H Cl3)'
_chemical_formula_sum            'C84 H90 Cl12 N16 O28 Si8'
_chemical_formula_weight         2421.84
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'
Cl Cl 0.1484 0.1585 '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      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                   9.578(4)
_cell_length_b                   16.150(7)
_cell_length_c                   18.867(7)
_cell_angle_alpha                108.08(4)
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                92.53(3)
_cell_volume                     2729(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    5631
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      30.8

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1246
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.471
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            22452
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.9
_diffrn_reflns_theta_max         30.8
_diffrn_reflns_theta_full        25.5
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             14558
_reflns_number_gt                10431
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.6, CCDC 2015'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0902P)²+3.3624P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14558
_refine_ls_number_parameters     830
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1889
_refine_ls_wR_factor_gt          0.1684
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.005
_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 0.76135(7) 0.55345(4) 0.05265(4) 0.01628(14) Uani 1 1 d . . . . .
Si2 Si 1.04770(7) 0.66850(4) 0.09067(4) 0.01632(14) Uani 1 1 d . . . . .
Si3 Si 1.07943(7) 0.60073(4) -0.08118(4) 0.01700(14) Uani 1 1 d . . . . .
Si4 Si 0.79310(7) 0.48541(4) -0.11951(4) 0.01662(14) Uani 1 1 d . . . . .
O1 O 0.88768(18) 0.63259(12) 0.09255(10) 0.0208(4) Uani 1 1 d . . . . .
O2 O 1.06323(19) 0.65787(12) 0.00423(10) 0.0219(4) Uani 1 1 d . . . . .
O3 O 0.92798(18) 0.54620(12) -0.12524(10) 0.0214(4) Uani 1 1 d . . . . .
O4 O 0.74295(18) 0.53007(12) -0.03876(10) 0.0201(4) Uani 1 1 d . . . . .
O5 O 0.80455(19) 0.46822(12) 0.07556(10) 0.0224(4) Uani 1 1 d . . . . .
O6 O 0.84075(18) 0.38887(12) -0.12390(10) 0.0213(4) Uani 1 1 d . . . . .
C1A C 0.5945(2) 0.58382(16) 0.08586(14) 0.0195(5) Uani 1 1 d . . . . .
H1AA H 0.5278 0.5301 0.0696 0.023 Uiso 1 1 calc R U . . .
H1AB H 0.6143 0.6044 0.1419 0.023 Uiso 1 1 calc R U . . .
C2A C 0.5180(3) 0.65395(18) 0.05998(15) 0.0247(5) Uani 1 1 d . . . . .
H2A H 0.5115 0.6393 0.0045 0.030 Uiso 1 1 calc R U . . .
H2B H 0.4200 0.6529 0.0707 0.030 Uiso 1 1 calc R U . . .
C3A C 0.5923(3) 0.74598(18) 0.09863(16) 0.0269(6) Uani 1 1 d . . . . .
H3AA H 0.6916 0.7473 0.0900 0.032 Uiso 1 1 calc R U . . .
H3AB H 0.5435 0.7875 0.0767 0.032 Uiso 1 1 calc R U . . .
N1A N 0.5906(2) 0.77224(15) 0.17970(14) 0.0257(5) Uani 1 1 d . . . . .
C4A C 0.7084(3) 0.79773(18) 0.22470(16) 0.0262(6) Uani 1 1 d . . . . .
H4A H 0.7937 0.7950 0.2045 0.031 Uiso 1 1 calc R U . . .
C5A C 0.7162(3) 0.83139(18) 0.30725(16) 0.0268(6) Uani 1 1 d . . . . .
C6A C 0.5939(3) 0.83050(19) 0.33966(17) 0.0297(6) Uani 1 1 d . . . . .
H6A H 0.5066 0.8022 0.3085 0.036 Uiso 1 1 calc R U . . .
C7A C 0.5991(3) 0.8701(2) 0.41610(18) 0.0336(7) Uani 1 1 d . . . . .
H7A H 0.5160 0.8705 0.4379 0.040 Uiso 1 1 calc R U . . .
C8A C 0.7286(3) 0.9095(2) 0.46064(18) 0.0337(6) Uani 1 1 d . . . . .
C9A C 0.8527(3) 0.9090(2) 0.43109(18) 0.0321(6) Uani 1 1 d . . . . .
H9A H 0.9405 0.9348 0.4630 0.039 Uiso 1 1 calc R U . . .
C10A C 0.8455(3) 0.87010(19) 0.35391(17) 0.0300(6) Uani 1 1 d . . . . .
H10A H 0.9291 0.8697 0.3325 0.036 Uiso 1 1 calc R U . . .
N2A N 0.7344(3) 0.9553(2) 0.54190(17) 0.0441(7) Uani 1 1 d . . . . .
O1A O 0.6271(3) 0.9500(2) 0.56834(15) 0.0624(8) Uani 1 1 d . . . . .
O2A O 0.8463(3) 0.9963(2) 0.57953(14) 0.0518(7) Uani 1 1 d . . . . .
C1B C 1.0847(3) 0.78460(16) 0.14792(15) 0.0199(5) Uani 1 1 d . . . . .
H1BA H 1.0160 0.8186 0.1268 0.024 Uiso 1 1 calc R U . . .
H1BB H 1.0700 0.7913 0.2002 0.024 Uiso 1 1 calc R U . . .
C2B C 1.2361(3) 0.82291(17) 0.15089(16) 0.0245(5) Uani 1 1 d . . . . .
H2BA H 1.3051 0.7933 0.1769 0.029 Uiso 1 1 calc R U . . .
H2BB H 1.2545 0.8115 0.0986 0.029 Uiso 1 1 calc R U . . .
C3B C 1.2576(3) 0.92118(19) 0.1925(2) 0.0349(7) Uani 1 1 d . . . . .
H3B H 1.234(4) 0.934(2) 0.245(2) 0.042 Uiso 1 1 d . U . . .
N1B N 1.4056(3) 0.95433(16) 0.19681(16) 0.0340(6) Uani 1 1 d . . . . .
C4B C 1.4788(3) 0.98279(18) 0.26254(18) 0.0307(6) Uani 1 1 d . . . . .
H4B H 1.4340 0.9829 0.3041 0.037 Uiso 1 1 calc R U . . .
C5B C 1.6302(3) 1.01601(19) 0.27839(19) 0.0321(6) Uani 1 1 d . . . . .
C6B C 1.7112(3) 1.0057(2) 0.2216(2) 0.0370(7) Uani 1 1 d . . . . .
H6B H 1.6697 0.9756 0.1703 0.044 Uiso 1 1 calc R U . . .
C7B C 1.8537(4) 1.0395(2) 0.2399(2) 0.0408(8) Uani 1 1 d . . . . .
H7B H 1.9113 1.0319 0.2020 0.049 Uiso 1 1 calc R U . . .
C8B C 1.9087(4) 1.0849(2) 0.3159(2) 0.0413(8) Uani 1 1 d . . . . .
C9B C 1.8320(4) 1.0943(2) 0.3732(2) 0.0382(7) Uani 1 1 d . . . . .
H9B H 1.8738 1.1241 0.4244 0.046 Uiso 1 1 calc R U . . .
C10B C 1.6926(3) 1.0593(2) 0.35421(19) 0.0354(7) Uani 1 1 d . . . . .
H10B H 1.6377 1.0644 0.3930 0.043 Uiso 1 1 calc R U . . .
N2B N 2.0576(3) 1.1264(2) 0.33552(19) 0.0488(8) Uani 1 1 d . . . . .
O1B O 2.1299(3) 1.10859(19) 0.28625(18) 0.0586(8) Uani 1 1 d . . . . .
O2B O 2.0984(3) 1.1761(2) 0.40020(18) 0.0688(9) Uani 1 1 d . . . . .
C1C C 1.1336(11) 0.6789(7) -0.1307(6) 0.0199(17) Uani 0.68 1 d . . P A 1
H1CA H 1.1457 0.6449 -0.1826 0.024 Uiso 0.68 1 calc R U P A 1
H1CB H 1.0566 0.7169 -0.1350 0.024 Uiso 0.68 1 calc R U P A 1
C2C C 1.2703(6) 0.7360(4) -0.0897(3) 0.0295(11) Uani 0.68 1 d . . P A 1
H2CA H 1.3511 0.6997 -0.0947 0.035 Uiso 0.68 1 calc R U P A 1
H2CB H 1.2660 0.7608 -0.0352 0.035 Uiso 0.68 1 calc R U P A 1
C3C C 1.2948(6) 0.8105(3) -0.1217(3) 0.0363(11) Uani 0.68 1 d . . P A 1
H3CA H 1.3874 0.8442 -0.0961 0.044 Uiso 0.68 1 calc R U P A 1
H3CB H 1.2196 0.8505 -0.1118 0.044 Uiso 0.68 1 calc R U P A 1
N1C N 1.2932(6) 0.7730(3) -0.2103(3) 0.0400(10) Uani 0.68 1 d . . P A 1
C4C C 1.4015(6) 0.7939(3) -0.2332(3) 0.0419(11) Uani 0.68 1 d . . P A 1
H4C H 1.4779 0.8315 -0.1984 0.050 Uiso 0.68 1 calc R U P A 1
C5C C 1.4095(4) 0.7601(2) -0.31431(14) 0.0365(11) Uani 0.68 1 d G . P A 1
C6C C 1.2974(3) 0.7055(2) -0.36543(19) 0.0407(12) Uani 0.68 1 d G . P A 1
H6C H 1.2165 0.6884 -0.3479 0.049 Uiso 0.68 1 calc R U P A 1
C7C C 1.3037(4) 0.6759(3) -0.44225(17) 0.0377(16) Uani 0.68 1 d G . P A 1
H7C H 1.2271 0.6386 -0.4772 0.045 Uiso 0.68 1 calc R U P A 1
C8C C 1.4221(4) 0.7008(3) -0.46795(14) 0.0387(12) Uani 0.68 1 d G . P A 1
C9C C 1.5342(3) 0.7554(2) -0.41682(19) 0.0393(11) Uani 0.68 1 d G . P A 1
H9C H 1.6151 0.7725 -0.4344 0.047 Uiso 0.68 1 calc R U P A 1
C10C C 1.5279(3) 0.7850(2) -0.34000(17) 0.0357(10) Uani 0.68 1 d G . P A 1
H10C H 1.6045 0.8223 -0.3051 0.043 Uiso 0.68 1 calc R U P A 1
N2C N 1.4348(5) 0.6719(3) -0.5451(4) 0.0323(10) Uani 0.68 1 d . . P A 1
O1C O 1.3291(5) 0.6258(3) -0.5910(2) 0.0448(9) Uani 0.68 1 d . . P A 1
O2C O 1.5425(4) 0.6909(3) -0.5637(3) 0.0554(11) Uani 0.68 1 d . . P A 1
C1D C 0.6485(3) 0.47801(17) -0.19806(14) 0.0210(5) Uani 1 1 d . . . B 1
H1DA H 0.6848 0.4588 -0.2464 0.025 Uiso 1 1 calc R U . B 1
H1DB H 0.5722 0.4335 -0.2001 0.025 Uiso 1 1 calc R U . B 1
C2D C 0.5867(3) 0.56655(19) -0.18912(17) 0.0281(6) Uani 1 1 d . . . B 1
H2DA H 0.5451 0.5834 -0.1423 0.034 Uiso 1 1 calc R U . B 1
H2DB H 0.6651 0.6117 -0.1829 0.034 Uiso 1 1 calc R U . B 1
C3D C 0.4732(3) 0.5660(2) -0.25573(18) 0.0322(6) Uani 1 1 d . . . B 1
H3DA H 0.4465 0.6262 -0.2487 0.039 Uiso 1 1 calc R U . B 1
H3DB H 0.5122 0.5463 -0.3032 0.039 Uiso 1 1 calc R U . B 1
N1D N 0.3476(3) 0.50832(17) -0.26189(14) 0.0299(5) Uani 1 1 d . . . B 1
C4D C 0.3008(3) 0.4528(2) -0.32617(18) 0.0322(6) Uani 1 1 d . . . B 1
H4D H 0.3502 0.4500 -0.3667 0.039 Uiso 1 1 calc R U . B 1
C5D C 0.1721(3) 0.3922(2) -0.34041(17) 0.0301(6) Uani 1 1 d . . . B 1
C6D C 0.0957(3) 0.3926(2) -0.28288(17) 0.0335(7) Uani 1 1 d . . . B 1
H6D H 0.1276 0.4319 -0.2331 0.040 Uiso 1 1 calc R U . B 1
C7D C -0.0257(3) 0.3364(2) -0.29770(17) 0.0320(6) Uani 1 1 d . . . B 1
H7D H -0.0772 0.3360 -0.2586 0.038 Uiso 1 1 calc R U . B 1
C8D C -0.0709(3) 0.2803(2) -0.37113(17) 0.0310(6) Uani 1 1 d . . . B 1
C9D C 0.0014(3) 0.2793(2) -0.42950(17) 0.0345(7) Uani 1 1 d . . . B 1
H9D H -0.0326 0.2410 -0.4794 0.041 Uiso 1 1 calc R U . B 1
C10D C 0.1234(3) 0.3348(2) -0.41373(17) 0.0339(7) Uani 1 1 d . . . B 1
H10D H 0.1751 0.3342 -0.4530 0.041 Uiso 1 1 calc R U . B 1
N2D N -0.1970(3) 0.21823(19) -0.38625(16) 0.0365(6) Uani 1 1 d . . . B 1
O1D O -0.2499(3) 0.2122(2) -0.33280(15) 0.0499(7) Uani 1 1 d . . . B 1
O2D O -0.2437(3) 0.17423(17) -0.45299(14) 0.0447(6) Uani 1 1 d . . . B 1
C1E C 1.138(3) 0.6649(14) -0.1303(15) 0.022(5) Uiso 0.32 1 d . . P A 2
H1EA H 1.1875 0.6278 -0.1694 0.026 Uiso 0.32 1 calc R U P A 2
H1EB H 1.0540 0.6826 -0.1573 0.026 Uiso 0.32 1 calc R U P A 2
C2E C 1.234(4) 0.744(2) -0.088(2) 0.134(14) Uiso 0.32 1 d . . P A 2
H2EA H 1.3331 0.7300 -0.0891 0.161 Uiso 0.32 1 calc R U P A 2
H2EB H 1.2203 0.7632 -0.0348 0.161 Uiso 0.32 1 calc R U P A 2
C3E C 1.210(3) 0.830(2) -0.1221(17) 0.134(10) Uiso 0.32 1 d . . P A 2
H3EA H 1.2309 0.8882 -0.0827 0.161 Uiso 0.32 1 calc R U P A 2
H3EB H 1.1173 0.8252 -0.1552 0.161 Uiso 0.32 1 calc R U P A 2
N1E N 1.3500(14) 0.7969(8) -0.1716(8) 0.054(3) Uiso 0.32 1 d . . P A 2
C4E C 1.2568(17) 0.7754(10) -0.2414(9) 0.047(4) Uiso 0.32 1 d . . P A 2
H4E H 1.1570 0.7767 -0.2447 0.057 Uiso 0.32 1 calc R U P A 2
C5E C 1.3239(7) 0.7510(4) -0.3082(3) 0.0207(15) Uiso 0.32 1 d G . P A 2
C6E C 1.2331(6) 0.7053(5) -0.3754(4) 0.025(2) Uiso 0.32 1 d G . P A 2
H6E H 1.1373 0.6883 -0.3746 0.030 Uiso 0.32 1 calc R U P A 2
C7E C 1.2825(8) 0.6845(7) -0.4438(3) 0.039(4) Uiso 0.32 1 d G . P A 2
H7E H 1.2204 0.6533 -0.4896 0.047 Uiso 0.32 1 calc R U P A 2
C8E C 1.4227(9) 0.7094(7) -0.4450(3) 0.032(3) Uiso 0.32 1 d G . P A 2
C9E C 1.5135(6) 0.7551(5) -0.3778(4) 0.035(2) Uiso 0.32 1 d G . P A 2
H9E H 1.6093 0.7721 -0.3786 0.042 Uiso 0.32 1 calc R U P A 2
C10E C 1.4641(7) 0.7759(5) -0.3094(3) 0.034(3) Uiso 0.32 1 d G . P A 2
H10E H 1.5261 0.8071 -0.2635 0.041 Uiso 0.32 1 calc R U P A 2
N2E N 1.4869(18) 0.6912(9) -0.5156(9) 0.060(4) Uiso 0.32 1 d . . P A 2
O1E O 1.3929(19) 0.6563(11) -0.5699(9) 0.065(5) Uiso 0.32 1 d . . P A 2
O2E O 1.6070(19) 0.7073(11) -0.5072(10) 0.110(5) Uiso 0.32 1 d . . P A 2
C1 C 0.8033(8) 0.5739(5) -0.3603(5) 0.0407(16) Uiso 0.5 1 d . . P C 3
H1 H 0.7600 0.5365 -0.3343 0.049 Uiso 0.5 1 calc R U P C 3
Cl1 Cl 0.6773(6) 0.5574(3) -0.4453(2) 0.0622(14) Uani 0.5 1 d . . P C 3
Cl2 Cl 0.8210(4) 0.6779(2) -0.2957(2) 0.0521(7) Uani 0.5 1 d . . P C 3
Cl3 Cl 0.9666(4) 0.5365(3) -0.3700(5) 0.147(3) Uani 0.5 1 d . . P C 3
C2 C 0.8143(15) 0.5429(12) -0.3843(8) 0.053(4) Uiso 0.25 1 d D . P D 4
H2 H 0.7806 0.4875 -0.3763 0.064 Uiso 0.25 1 calc R U P D 4
Cl4 Cl 0.723(2) 0.5670(13) -0.4550(8) 0.195(12) Uani 0.25 1 d D . P D 4
Cl5 Cl 0.9622(10) 0.5414(8) -0.4211(5) 0.074(3) Uani 0.25 1 d D . P D 4
Cl6 Cl 0.885(2) 0.6259(15) -0.3062(6) 0.204(11) Uani 0.25 1 d D . P D 4
C3 C 0.8305(16) 0.5982(13) -0.4010(10) 0.073(5) Uiso 0.25 1 d D . P E 5
H3 H 0.8253 0.6492 -0.4205 0.087 Uiso 0.25 1 calc R U P E 5
Cl7 Cl 0.6617(8) 0.5430(7) -0.4364(7) 0.086(4) Uani 0.25 1 d D . P E 5
Cl8 Cl 0.9572(11) 0.5359(8) -0.4518(5) 0.073(3) Uani 0.25 1 d D . P E 5
Cl9 Cl 0.840(2) 0.6462(11) -0.3067(8) 0.120(7) Uani 0.25 1 d D . P E 5
C4 C 0.7026(19) 0.8411(10) -0.0787(8) 0.088(5) Uiso 0.35 1 d D . P F -6
H4 H 0.6072 0.8107 -0.1059 0.105 Uiso 0.35 1 calc R U P F -6
Cl10 Cl 0.7865(5) 0.8713(3) -0.1407(2) 0.0713(11) Uani 0.35 1 d D . P F -6
Cl11 Cl 0.7978(4) 0.7693(2) -0.04396(19) 0.0495(8) Uani 0.35 1 d D . P F -6
Cl12 Cl 0.6784(6) 0.9329(3) -0.0011(3) 0.1079(17) Uani 0.35 1 d D . P F -6
C5 C 0.8230(10) 0.8797(6) -0.0527(5) 0.032(2) Uiso 0.3 1 d D . P G -7
H5 H 0.7644 0.9293 -0.0348 0.038 Uiso 0.3 1 calc R U P G -7
Cl13 Cl 0.8589(4) 0.8714(3) -0.1408(2) 0.0408(7) Uani 0.3 1 d D . P G -7
Cl14 Cl 0.7248(9) 0.7777(3) -0.0682(3) 0.0809(18) Uani 0.3 1 d D . P G -7
Cl15 Cl 0.9891(11) 0.8981(6) 0.0068(5) 0.168(5) Uani 0.3 1 d D . P G -7
C6 C 0.701(2) 0.8882(13) -0.0258(12) 0.050(6) Uiso 0.15 1 d D . P H -8
H6 H 0.6141 0.8746 -0.0067 0.060 Uiso 0.15 1 calc R U P H -8
Cl16 Cl 0.759(3) 0.7927(17) -0.0870(15) 0.194(13) Uiso 0.15 1 d D . P H -8
Cl17 Cl 0.6737(6) 0.9611(3) -0.0773(3) 0.0343(10) Uiso 0.15 1 d D . P H -8
Cl18 Cl 0.8359(14) 0.9327(8) 0.0436(7) 0.089(3) Uiso 0.15 1 d D . P H -8
C7 C 0.406(4) 1.0741(17) 0.003(2) 0.100 Uiso 0.1 1 d D U P I -9
H7 H 0.3122 1.0626 -0.0319 0.120 Uiso 0.1 1 calc R U P I -9
Cl19 Cl 0.535(2) 1.0596(14) -0.0564(11) 0.125(7) Uiso 0.1 1 d D . P I -9
Cl20 Cl 0.4009(18) 0.9958(10) 0.0504(9) 0.091(4) Uiso 0.1 1 d D . P I -9
Cl21 Cl 0.411(4) 1.1852(13) 0.0634(18) 0.200 Uiso 0.1 1 d D U P I -9
C8 C 0.889(2) 1.0094(16) -0.0151(13) 0.031(6) Uiso 0.1 1 d D . P J -10
H8 H 0.8571 1.0611 0.0215 0.037 Uiso 0.1 1 calc R U P J -10
Cl22 Cl 0.8886(11) 0.9317(6) 0.0369(5) 0.0357(18) Uiso 0.1 1 d D . P J -10
Cl23 Cl 1.0470(15) 1.0523(10) -0.0211(9) 0.079(4) Uiso 0.1 1 d D . P J -10
Cl24 Cl 0.740(2) 0.978(2) -0.0857(16) 0.200 Uiso 0.1 1 d D U P J -10


_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 O5 1.618(2) . ?
Si1 O4 1.626(2) . ?
Si1 O1 1.628(2) . ?
Si1 C1A 1.836(2) . ?
Si2 O2 1.617(2) . ?
Si2 O6 1.624(2) 2_765 ?
Si2 O1 1.6241(19) . ?
Si2 C1B 1.837(3) . ?
Si3 O5 1.623(2) 2_765 ?
Si3 O3 1.623(2) . ?
Si3 O2 1.624(2) . ?
Si3 C1E 1.72(2) . ?
Si3 C1C 1.886(10) . ?
Si4 O6 1.625(2) . ?
Si4 O3 1.6251(19) . ?
Si4 O4 1.626(2) . ?
Si4 C1D 1.837(3) . ?
O5 Si3 1.623(2) 2_765 ?
O6 Si2 1.624(2) 2_765 ?
C1A C2A 1.538(4) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A C3A 1.524(4) . ?
C2A H2A 0.9900 . ?
C2A H2B 0.9900 . ?
C3A N1A 1.458(4) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
N1A C4A 1.270(4) . ?
C4A C5A 1.471(4) . ?
C4A H4A 0.9500 . ?
C5A C10A 1.399(4) . ?
C5A C6A 1.403(4) . ?
C6A C7A 1.376(4) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.388(4) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.387(4) . ?
C8A N2A 1.472(4) . ?
C9A C10A 1.385(4) . ?
C9A H9A 0.9500 . ?
C10A H10A 0.9500 . ?
N2A O1A 1.220(4) . ?
N2A O2A 1.226(4) . ?
C1B C2B 1.538(3) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C2B C3B 1.525(4) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B N1B 1.474(4) . ?
C3B H3B 1.01(4) . ?
N1B C4B 1.262(4) . ?
C4B C5B 1.476(4) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.391(5) . ?
C5B C10B 1.405(5) . ?
C6B C7B 1.398(5) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.397(5) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.372(5) . ?
C8B N2B 1.490(4) . ?
C9B C10B 1.375(4) . ?
C9B H9B 0.9500 . ?
C10B H10B 0.9500 . ?
N2B O1B 1.214(4) . ?
N2B O2B 1.227(4) . ?
C1C C2C 1.518(11) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.529(6) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C N1C 1.589(8) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
N1C C4C 1.254(7) . ?
C4C C5C 1.472(6) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.3900 . ?
C5C C10C 1.3900 . ?
C6C C7C 1.3900 . ?
C6C H6C 0.9500 . ?
C7C C8C 1.3900 . ?
C7C H7C 0.9500 . ?
C8C C9C 1.3900 . ?
C8C N2C 1.411(7) . ?
C9C C10C 1.3900 . ?
C9C H9C 0.9500 . ?
C10C H10C 0.9500 . ?
N2C O2C 1.196(6) . ?
N2C O1C 1.263(7) . ?
C1D C2D 1.542(4) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D C3D 1.529(4) . ?
C2D H2DA 0.9900 . ?
C2D H2DB 0.9900 . ?
C3D N1D 1.456(4) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
N1D C4D 1.265(4) . ?
C4D C5D 1.475(4) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.398(4) . ?
C5D C10D 1.400(4) . ?
C6D C7D 1.381(4) . ?
C6D H6D 0.9500 . ?
C7D C8D 1.389(4) . ?
C7D H7D 0.9500 . ?
C8D C9D 1.383(4) . ?
C8D N2D 1.469(4) . ?
C9D C10D 1.377(4) . ?
C9D H9D 0.9500 . ?
C10D H10D 0.9500 . ?
N2D O1D 1.223(4) . ?
N2D O2D 1.239(4) . ?
C1E C2E 1.47(4) . ?
C1E H1EA 0.9900 . ?
C1E H1EB 0.9900 . ?
C2E C3E 1.70(4) . ?
C2E H2EA 0.9900 . ?
C2E H2EB 0.9900 . ?
C3E N1E 1.76(3) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
N1E C4E 1.408(18) . ?
C4E C5E 1.455(16) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.3900 . ?
C5E C10E 1.3900 . ?
C6E C7E 1.3900 . ?
C6E H6E 0.9500 . ?
C7E C8E 1.3900 . ?
C7E H7E 0.9500 . ?
C8E C9E 1.3900 . ?
C8E N2E 1.505(15) . ?
C9E C10E 1.3900 . ?
C9E H9E 0.9500 . ?
C10E H10E 0.9500 . ?
N2E O2E 1.14(2) . ?
N2E O1E 1.221(18) . ?
C1 Cl3 1.717(9) . ?
C1 Cl2 1.725(9) . ?
C1 Cl1 1.794(9) . ?
C1 H1 1.0000 . ?
C2 Cl4 1.641(16) . ?
C2 Cl5 1.668(15) . ?
C2 Cl6 1.677(16) . ?
C2 H2 1.0000 . ?
Cl4 Cl5 2.37(2) . ?
Cl5 Cl6 2.42(2) . ?
C3 Cl9 1.693(16) . ?
C3 Cl7 1.739(15) . ?
C3 Cl8 1.807(15) . ?
C3 H3 1.0000 . ?
Cl8 Cl8 2.135(19) 2_764 ?
C4 Cl10 1.691(14) . ?
C4 Cl11 1.727(14) . ?
C4 Cl12 1.785(14) . ?
C4 H4 1.0000 . ?
C5 Cl13 1.715(10) . ?
C5 Cl15 1.756(11) . ?
C5 Cl14 1.778(10) . ?
C5 H5 1.0000 . ?
C6 Cl18 1.648(17) . ?
C6 Cl17 1.748(16) . ?
C6 Cl16 1.783(19) . ?
C6 H6 1.0000 . ?
C7 Cl20 1.76(2) . ?
C7 Cl19 1.77(2) . ?
C7 Cl21 1.79(2) . ?
C7 H7 1.0000 . ?
C8 Cl23 1.666(16) . ?
C8 Cl24 1.737(17) . ?
C8 Cl22 1.817(16) . ?
C8 H8 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
O5 Si1 O4 109.26(11) . . ?
O5 Si1 O1 109.06(10) . . ?
O4 Si1 O1 108.78(10) . . ?
O5 Si1 C1A 107.70(11) . . ?
O4 Si1 C1A 111.11(11) . . ?
O1 Si1 C1A 110.89(11) . . ?
O2 Si2 O6 109.45(10) . 2_765 ?
O2 Si2 O1 109.31(10) . . ?
O6 Si2 O1 108.79(10) 2_765 . ?
O2 Si2 C1B 109.06(12) . . ?
O6 Si2 C1B 110.00(11) 2_765 . ?
O1 Si2 C1B 110.21(11) . . ?
O5 Si3 O3 108.62(11) 2_765 . ?
O5 Si3 O2 108.28(11) 2_765 . ?
O3 Si3 O2 108.99(10) . . ?
O5 Si3 C1E 107.8(8) 2_765 . ?
O3 Si3 C1E 110.8(9) . . ?
O2 Si3 C1E 112.2(8) . . ?
O5 Si3 C1C 112.7(3) 2_765 . ?
O3 Si3 C1C 110.2(3) . . ?
O2 Si3 C1C 108.0(3) . . ?
O6 Si4 O3 109.15(10) . . ?
O6 Si4 O4 109.32(11) . . ?
O3 Si4 O4 108.68(10) . . ?
O6 Si4 C1D 110.59(12) . . ?
O3 Si4 C1D 108.80(11) . . ?
O4 Si4 C1D 110.28(11) . . ?
Si2 O1 Si1 144.77(12) . . ?
Si2 O2 Si3 152.96(13) . . ?
Si3 O3 Si4 145.41(13) . . ?
Si4 O4 Si1 152.17(13) . . ?
Si1 O5 Si3 148.60(12) . 2_765 ?
Si2 O6 Si4 147.36(12) 2_765 . ?
C2A C1A Si1 117.90(18) . . ?
C2A C1A H1AA 107.8 . . ?
Si1 C1A H1AA 107.8 . . ?
C2A C1A H1AB 107.8 . . ?
Si1 C1A H1AB 107.8 . . ?
H1AA C1A H1AB 107.2 . . ?
C3A C2A C1A 113.1(2) . . ?
C3A C2A H2A 109.0 . . ?
C1A C2A H2A 109.0 . . ?
C3A C2A H2B 109.0 . . ?
C1A C2A H2B 109.0 . . ?
H2A C2A H2B 107.8 . . ?
N1A C3A C2A 109.9(2) . . ?
N1A C3A H3AA 109.7 . . ?
C2A C3A H3AA 109.7 . . ?
N1A C3A H3AB 109.7 . . ?
C2A C3A H3AB 109.7 . . ?
H3AA C3A H3AB 108.2 . . ?
C4A N1A C3A 117.9(2) . . ?
N1A C4A C5A 121.7(2) . . ?
N1A C4A H4A 119.2 . . ?
C5A C4A H4A 119.2 . . ?
C10A C5A C6A 119.3(3) . . ?
C10A C5A C4A 119.6(3) . . ?
C6A C5A C4A 120.9(3) . . ?
C7A C6A C5A 120.7(3) . . ?
C7A C6A H6A 119.7 . . ?
C5A C6A H6A 119.7 . . ?
C6A C7A C8A 118.6(3) . . ?
C6A C7A H7A 120.7 . . ?
C8A C7A H7A 120.7 . . ?
C9A C8A C7A 122.4(3) . . ?
C9A C8A N2A 118.5(3) . . ?
C7A C8A N2A 119.1(3) . . ?
C10A C9A C8A 118.4(3) . . ?
C10A C9A H9A 120.8 . . ?
C8A C9A H9A 120.8 . . ?
C9A C10A C5A 120.6(3) . . ?
C9A C10A H10A 119.7 . . ?
C5A C10A H10A 119.7 . . ?
O1A N2A O2A 123.4(3) . . ?
O1A N2A C8A 117.9(3) . . ?
O2A N2A C8A 118.7(3) . . ?
C2B C1B Si2 113.40(17) . . ?
C2B C1B H1BA 108.9 . . ?
Si2 C1B H1BA 108.9 . . ?
C2B C1B H1BB 108.9 . . ?
Si2 C1B H1BB 108.9 . . ?
H1BA C1B H1BB 107.7 . . ?
C3B C2B C1B 111.6(2) . . ?
C3B C2B H2BA 109.3 . . ?
C1B C2B H2BA 109.3 . . ?
C3B C2B H2BB 109.3 . . ?
C1B C2B H2BB 109.3 . . ?
H2BA C2B H2BB 108.0 . . ?
N1B C3B C2B 109.7(2) . . ?
N1B C3B H3B 111(2) . . ?
C2B C3B H3B 110(2) . . ?
C4B N1B C3B 115.5(3) . . ?
N1B C4B C5B 123.6(3) . . ?
N1B C4B H4B 118.2 . . ?
C5B C4B H4B 118.2 . . ?
C6B C5B C10B 119.8(3) . . ?
C6B C5B C4B 122.5(3) . . ?
C10B C5B C4B 117.7(3) . . ?
C5B C6B C7B 119.9(3) . . ?
C5B C6B H6B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
C8B C7B C6B 117.8(3) . . ?
C8B C7B H7B 121.1 . . ?
C6B C7B H7B 121.1 . . ?
C9B C8B C7B 123.4(3) . . ?
C9B C8B N2B 118.3(3) . . ?
C7B C8B N2B 118.3(3) . . ?
C8B C9B C10B 118.0(3) . . ?
C8B C9B H9B 121.0 . . ?
C10B C9B H9B 121.0 . . ?
C9B C10B C5B 121.1(3) . . ?
C9B C10B H10B 119.5 . . ?
C5B C10B H10B 119.5 . . ?
O1B N2B O2B 124.7(3) . . ?
O1B N2B C8B 117.6(3) . . ?
O2B N2B C8B 117.7(3) . . ?
C2C C1C Si3 113.0(6) . . ?
C2C C1C H1CA 109.0 . . ?
Si3 C1C H1CA 109.0 . . ?
C2C C1C H1CB 109.0 . . ?
Si3 C1C H1CB 109.0 . . ?
H1CA C1C H1CB 107.8 . . ?
C1C C2C C3C 111.4(6) . . ?
C1C C2C H2CA 109.3 . . ?
C3C C2C H2CA 109.3 . . ?
C1C C2C H2CB 109.3 . . ?
C3C C2C H2CB 109.3 . . ?
H2CA C2C H2CB 108.0 . . ?
C2C C3C N1C 110.6(4) . . ?
C2C C3C H3CA 109.5 . . ?
N1C C3C H3CA 109.5 . . ?
C2C C3C H3CB 109.5 . . ?
N1C C3C H3CB 109.5 . . ?
H3CA C3C H3CB 108.1 . . ?
C4C N1C C3C 116.4(5) . . ?
N1C C4C C5C 119.7(5) . . ?
N1C C4C H4C 120.2 . . ?
C5C C4C H4C 120.2 . . ?
C6C C5C C10C 120.0 . . ?
C6C C5C C4C 120.3(3) . . ?
C10C C5C C4C 119.7(3) . . ?
C7C C6C C5C 120.0 . . ?
C7C C6C H6C 120.0 . . ?
C5C C6C H6C 120.0 . . ?
C8C C7C C6C 120.0 . . ?
C8C C7C H7C 120.0 . . ?
C6C C7C H7C 120.0 . . ?
C7C C8C C9C 120.0 . . ?
C7C C8C N2C 122.4(3) . . ?
C9C C8C N2C 117.6(3) . . ?
C10C C9C C8C 120.0 . . ?
C10C C9C H9C 120.0 . . ?
C8C C9C H9C 120.0 . . ?
C9C C10C C5C 120.0 . . ?
C9C C10C H10C 120.0 . . ?
C5C C10C H10C 120.0 . . ?
O2C N2C O1C 123.7(6) . . ?
O2C N2C C8C 119.7(6) . . ?
O1C N2C C8C 116.6(4) . . ?
C2D C1D Si4 111.71(18) . . ?
C2D C1D H1DA 109.3 . . ?
Si4 C1D H1DA 109.3 . . ?
C2D C1D H1DB 109.3 . . ?
Si4 C1D H1DB 109.3 . . ?
H1DA C1D H1DB 107.9 . . ?
C3D C2D C1D 114.0(2) . . ?
C3D C2D H2DA 108.7 . . ?
C1D C2D H2DA 108.7 . . ?
C3D C2D H2DB 108.7 . . ?
C1D C2D H2DB 108.7 . . ?
H2DA C2D H2DB 107.6 . . ?
N1D C3D C2D 111.2(2) . . ?
N1D C3D H3DA 109.4 . . ?
C2D C3D H3DA 109.4 . . ?
N1D C3D H3DB 109.4 . . ?
C2D C3D H3DB 109.4 . . ?
H3DA C3D H3DB 108.0 . . ?
C4D N1D C3D 117.0(3) . . ?
N1D C4D C5D 122.3(3) . . ?
N1D C4D H4D 118.8 . . ?
C5D C4D H4D 118.8 . . ?
C6D C5D C10D 119.3(3) . . ?
C6D C5D C4D 121.5(3) . . ?
C10D C5D C4D 119.2(3) . . ?
C7D C6D C5D 120.6(3) . . ?
C7D C6D H6D 119.7 . . ?
C5D C6D H6D 119.7 . . ?
C6D C7D C8D 118.5(3) . . ?
C6D C7D H7D 120.8 . . ?
C8D C7D H7D 120.8 . . ?
C9D C8D C7D 122.3(3) . . ?
C9D C8D N2D 119.2(3) . . ?
C7D C8D N2D 118.4(3) . . ?
C10D C9D C8D 118.6(3) . . ?
C10D C9D H9D 120.7 . . ?
C8D C9D H9D 120.7 . . ?
C9D C10D C5D 120.7(3) . . ?
C9D C10D H10D 119.7 . . ?
C5D C10D H10D 119.7 . . ?
O1D N2D O2D 123.5(3) . . ?
O1D N2D C8D 118.7(3) . . ?
O2D N2D C8D 117.8(3) . . ?
C2E C1E Si3 119(2) . . ?
C2E C1E H1EA 107.6 . . ?
Si3 C1E H1EA 107.6 . . ?
C2E C1E H1EB 107.6 . . ?
Si3 C1E H1EB 107.6 . . ?
H1EA C1E H1EB 107.1 . . ?
C1E C2E C3E 115(3) . . ?
C1E C2E H2EA 108.6 . . ?
C3E C2E H2EA 108.6 . . ?
C1E C2E H2EB 108.6 . . ?
C3E C2E H2EB 108.6 . . ?
H2EA C2E H2EB 107.5 . . ?
C2E C3E N1E 87.3(19) . . ?
C2E C3E H3EA 114.1 . . ?
N1E C3E H3EA 114.1 . . ?
C2E C3E H3EB 114.1 . . ?
N1E C3E H3EB 114.1 . . ?
H3EA C3E H3EB 111.3 . . ?
C4E N1E C3E 91.0(14) . . ?
N1E C4E C5E 115.3(13) . . ?
N1E C4E H4E 122.3 . . ?
C5E C4E H4E 122.3 . . ?
C6E C5E C10E 120.0 . . ?
C6E C5E C4E 114.8(8) . . ?
C10E C5E C4E 125.0(8) . . ?
C5E C6E C7E 120.0 . . ?
C5E C6E H6E 120.0 . . ?
C7E C6E H6E 120.0 . . ?
C8E C7E C6E 120.0 . . ?
C8E C7E H7E 120.0 . . ?
C6E C7E H7E 120.0 . . ?
C7E C8E C9E 120.0 . . ?
C7E C8E N2E 124.5(8) . . ?
C9E C8E N2E 115.5(8) . . ?
C8E C9E C10E 120.0 . . ?
C8E C9E H9E 120.0 . . ?
C10E C9E H9E 120.0 . . ?
C9E C10E C5E 120.0 . . ?
C9E C10E H10E 120.0 . . ?
C5E C10E H10E 120.0 . . ?
O2E N2E O1E 135.3(19) . . ?
O2E N2E C8E 116.6(16) . . ?
O1E N2E C8E 108.0(15) . . ?
Cl3 C1 Cl2 110.7(5) . . ?
Cl3 C1 Cl1 117.3(6) . . ?
Cl2 C1 Cl1 115.1(5) . . ?
Cl3 C1 H1 104.0 . . ?
Cl2 C1 H1 104.0 . . ?
Cl1 C1 H1 104.0 . . ?
Cl4 C2 Cl5 91.5(11) . . ?
Cl4 C2 Cl6 117.8(14) . . ?
Cl5 C2 Cl6 92.6(11) . . ?
Cl4 C2 H2 116.5 . . ?
Cl5 C2 H2 116.5 . . ?
Cl6 C2 H2 116.5 . . ?
C2 Cl4 Cl5 44.7(7) . . ?
C2 Cl5 Cl4 43.8(6) . . ?
C2 Cl5 Cl6 43.9(6) . . ?
Cl4 Cl5 Cl6 72.8(6) . . ?
C2 Cl6 Cl5 43.6(7) . . ?
Cl9 C3 Cl7 107.0(11) . . ?
Cl9 C3 Cl8 129.5(14) . . ?
Cl7 C3 Cl8 109.3(10) . . ?
Cl9 C3 H3 102.6 . . ?
Cl7 C3 H3 102.6 . . ?
Cl8 C3 H3 102.6 . . ?
C3 Cl8 Cl8 156.8(10) . 2_764 ?
Cl10 C4 Cl11 110.4(9) . . ?
Cl10 C4 Cl12 111.9(9) . . ?
Cl11 C4 Cl12 108.9(8) . . ?
Cl10 C4 H4 108.5 . . ?
Cl11 C4 H4 108.5 . . ?
Cl12 C4 H4 108.5 . . ?
Cl13 C5 Cl15 105.6(6) . . ?
Cl13 C5 Cl14 102.9(5) . . ?
Cl15 C5 Cl14 115.7(6) . . ?
Cl13 C5 H5 110.7 . . ?
Cl15 C5 H5 110.7 . . ?
Cl14 C5 H5 110.7 . . ?
Cl18 C6 Cl17 107.0(12) . . ?
Cl18 C6 Cl16 106.6(16) . . ?
Cl17 C6 Cl16 106.7(16) . . ?
Cl18 C6 H6 112.0 . . ?
Cl17 C6 H6 112.0 . . ?
Cl16 C6 H6 112.0 . . ?
Cl20 C7 Cl19 113.6(16) . . ?
Cl20 C7 Cl21 114.3(17) . . ?
Cl19 C7 Cl21 112.8(16) . . ?
Cl20 C7 H7 105.0 . . ?
Cl19 C7 H7 105.0 . . ?
Cl21 C7 H7 105.0 . . ?
Cl23 C8 Cl24 126.7(15) . . ?
Cl23 C8 Cl22 117.3(12) . . ?
Cl24 C8 Cl22 106.5(12) . . ?
Cl23 C8 H8 100.3 . . ?
Cl24 C8 H8 100.3 . . ?
Cl22 C8 H8 100.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Si2 O1 Si1 45.4(3) . . . . ?
O6 Si2 O1 Si1 -74.0(2) 2_765 . . . ?
C1B Si2 O1 Si1 165.3(2) . . . . ?
O5 Si1 O1 Si2 73.3(2) . . . . ?
O4 Si1 O1 Si2 -45.8(3) . . . . ?
C1A Si1 O1 Si2 -168.3(2) . . . . ?
O6 Si2 O2 Si3 44.5(3) 2_765 . . . ?
O1 Si2 O2 Si3 -74.6(3) . . . . ?
C1B Si2 O2 Si3 164.8(3) . . . . ?
O5 Si3 O2 Si2 -43.8(3) 2_765 . . . ?
O3 Si3 O2 Si2 74.2(3) . . . . ?
C1E Si3 O2 Si2 -162.7(10) . . . . ?
C1C Si3 O2 Si2 -166.1(4) . . . . ?
O5 Si3 O3 Si4 72.8(2) 2_765 . . . ?
O2 Si3 O3 Si4 -45.0(3) . . . . ?
C1E Si3 O3 Si4 -168.9(9) . . . . ?
C1C Si3 O3 Si4 -163.3(4) . . . . ?
O6 Si4 O3 Si3 -73.6(2) . . . . ?
O4 Si4 O3 Si3 45.6(3) . . . . ?
C1D Si4 O3 Si3 165.7(2) . . . . ?
O6 Si4 O4 Si1 42.9(3) . . . . ?
O3 Si4 O4 Si1 -76.1(3) . . . . ?
C1D Si4 O4 Si1 164.7(3) . . . . ?
O5 Si1 O4 Si4 -42.7(3) . . . . ?
O1 Si1 O4 Si4 76.3(3) . . . . ?
C1A Si1 O4 Si4 -161.3(3) . . . . ?
O4 Si1 O5 Si3 67.0(3) . . . 2_765 ?
O1 Si1 O5 Si3 -51.8(3) . . . 2_765 ?
C1A Si1 O5 Si3 -172.2(2) . . . 2_765 ?
O3 Si4 O6 Si2 52.9(3) . . . 2_765 ?
O4 Si4 O6 Si2 -65.8(2) . . . 2_765 ?
C1D Si4 O6 Si2 172.6(2) . . . 2_765 ?
O5 Si1 C1A C2A -170.39(18) . . . . ?
O4 Si1 C1A C2A -50.8(2) . . . . ?
O1 Si1 C1A C2A 70.3(2) . . . . ?
Si1 C1A C2A C3A -72.9(3) . . . . ?
C1A C2A C3A N1A -64.2(3) . . . . ?
C2A C3A N1A C4A 125.6(3) . . . . ?
C3A N1A C4A C5A 175.6(2) . . . . ?
N1A C4A C5A C10A -171.0(3) . . . . ?
N1A C4A C5A C6A 4.8(4) . . . . ?
C10A C5A C6A C7A 2.5(5) . . . . ?
C4A C5A C6A C7A -173.3(3) . . . . ?
C5A C6A C7A C8A -1.2(5) . . . . ?
C6A C7A C8A C9A -1.1(5) . . . . ?
C6A C7A C8A N2A 177.5(3) . . . . ?
C7A C8A C9A C10A 2.0(5) . . . . ?
N2A C8A C9A C10A -176.5(3) . . . . ?
C8A C9A C10A C5A -0.7(5) . . . . ?
C6A C5A C10A C9A -1.5(4) . . . . ?
C4A C5A C10A C9A 174.3(3) . . . . ?
C9A C8A N2A O1A -174.9(3) . . . . ?
C7A C8A N2A O1A 6.5(5) . . . . ?
C9A C8A N2A O2A 4.8(5) . . . . ?
C7A C8A N2A O2A -173.8(3) . . . . ?
O2 Si2 C1B C2B -61.6(2) . . . . ?
O6 Si2 C1B C2B 58.4(2) 2_765 . . . ?
O1 Si2 C1B C2B 178.34(18) . . . . ?
Si2 C1B C2B C3B 174.5(2) . . . . ?
C1B C2B C3B N1B 177.6(3) . . . . ?
C2B C3B N1B C4B -114.1(3) . . . . ?
C3B N1B C4B C5B 178.0(3) . . . . ?
N1B C4B C5B C6B -10.8(5) . . . . ?
N1B C4B C5B C10B 169.4(3) . . . . ?
C10B C5B C6B C7B -1.0(5) . . . . ?
C4B C5B C6B C7B 179.2(3) . . . . ?
C5B C6B C7B C8B -1.5(5) . . . . ?
C6B C7B C8B C9B 3.1(5) . . . . ?
C6B C7B C8B N2B -176.0(3) . . . . ?
C7B C8B C9B C10B -1.9(5) . . . . ?
N2B C8B C9B C10B 177.1(3) . . . . ?
C8B C9B C10B C5B -0.7(5) . . . . ?
C6B C5B C10B C9B 2.1(5) . . . . ?
C4B C5B C10B C9B -178.0(3) . . . . ?
C9B C8B N2B O1B 171.0(4) . . . . ?
C7B C8B N2B O1B -9.9(5) . . . . ?
C9B C8B N2B O2B -9.1(5) . . . . ?
C7B C8B N2B O2B 170.0(4) . . . . ?
O5 Si3 C1C C2C -61.9(7) 2_765 . . . ?
O3 Si3 C1C C2C 176.6(6) . . . . ?
O2 Si3 C1C C2C 57.6(7) . . . . ?
Si3 C1C C2C C3C -168.3(5) . . . . ?
C1C C2C C3C N1C -55.7(7) . . . . ?
C2C C3C N1C C4C -123.6(5) . . . . ?
C3C N1C C4C C5C 178.5(4) . . . . ?
N1C C4C C5C C6C 0.3(6) . . . . ?
N1C C4C C5C C10C 178.4(4) . . . . ?
C10C C5C C6C C7C 0.0 . . . . ?
C4C C5C C6C C7C 178.0(4) . . . . ?
C5C C6C C7C C8C 0.0 . . . . ?
C6C C7C C8C C9C 0.0 . . . . ?
C6C C7C C8C N2C 179.2(4) . . . . ?
C7C C8C C9C C10C 0.0 . . . . ?
N2C C8C C9C C10C -179.3(4) . . . . ?
C8C C9C C10C C5C 0.0 . . . . ?
C6C C5C C10C C9C 0.0 . . . . ?
C4C C5C C10C C9C -178.0(4) . . . . ?
C7C C8C N2C O2C -175.4(4) . . . . ?
C9C C8C N2C O2C 3.9(6) . . . . ?
C7C C8C N2C O1C 4.0(5) . . . . ?
C9C C8C N2C O1C -176.8(3) . . . . ?
O6 Si4 C1D C2D 171.90(18) . . . . ?
O3 Si4 C1D C2D -68.2(2) . . . . ?
O4 Si4 C1D C2D 50.9(2) . . . . ?
Si4 C1D C2D C3D 175.8(2) . . . . ?
C1D C2D C3D N1D 65.4(3) . . . . ?
C2D C3D N1D C4D -129.4(3) . . . . ?
C3D N1D C4D C5D -178.3(3) . . . . ?
N1D C4D C5D C6D -0.6(5) . . . . ?
N1D C4D C5D C10D 177.5(3) . . . . ?
C10D C5D C6D C7D 0.8(5) . . . . ?
C4D C5D C6D C7D 178.9(3) . . . . ?
C5D C6D C7D C8D -0.8(5) . . . . ?
C6D C7D C8D C9D -0.1(5) . . . . ?
C6D C7D C8D N2D 177.7(3) . . . . ?
C7D C8D C9D C10D 1.1(5) . . . . ?
N2D C8D C9D C10D -176.8(3) . . . . ?
C8D C9D C10D C5D -1.1(5) . . . . ?
C6D C5D C10D C9D 0.2(5) . . . . ?
C4D C5D C10D C9D -178.0(3) . . . . ?
C9D C8D N2D O1D 171.1(3) . . . . ?
C7D C8D N2D O1D -6.8(4) . . . . ?
C9D C8D N2D O2D -8.5(4) . . . . ?
C7D C8D N2D O2D 173.6(3) . . . . ?
O5 Si3 C1E C2E -88(2) 2_765 . . . ?
O3 Si3 C1E C2E 154(2) . . . . ?
O2 Si3 C1E C2E 32(2) . . . . ?
Si3 C1E C2E C3E -145(2) . . . . ?
C1E C2E C3E N1E -97(3) . . . . ?
C2E C3E N1E C4E 114.1(18) . . . . ?
C3E N1E C4E C5E 173.3(14) . . . . ?
N1E C4E C5E C6E 161.4(10) . . . . ?
N1E C4E C5E C10E -23.9(15) . . . . ?
C10E C5E C6E C7E 0.0 . . . . ?
C4E C5E C6E C7E 174.9(8) . . . . ?
C5E C6E C7E C8E 0.0 . . . . ?
C6E C7E C8E C9E 0.0 . . . . ?
C6E C7E C8E N2E -179.4(11) . . . . ?
C7E C8E C9E C10E 0.0 . . . . ?
N2E C8E C9E C10E 179.4(10) . . . . ?
C8E C9E C10E C5E 0.0 . . . . ?
C6E C5E C10E C9E 0.0 . . . . ?
C4E C5E C10E C9E -174.4(9) . . . . ?
C7E C8E N2E O2E -172.0(12) . . . . ?
C9E C8E N2E O2E 8.6(18) . . . . ?
C7E C8E N2E O1E 3.9(17) . . . . ?
C9E C8E N2E O1E -175.5(12) . . . . ?
Cl6 C2 Cl4 Cl5 93.7(14) . . . . ?
Cl6 C2 Cl5 Cl4 -117.9(15) . . . . ?
Cl4 C2 Cl5 Cl6 117.9(15) . . . . ?
Cl4 C2 Cl6 Cl5 -93.1(14) . . . . ?
Cl9 C3 Cl8 Cl8 -176(2) . . . 2_764 ?
Cl7 C3 Cl8 Cl8 50(4) . . . 2_764 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4B H4B O1A 0.95 2.48 3.365(4) 154.1 2_776
C3A H3AB Cl19 0.99 2.73 3.68(2) 161.1 2_675
C4B H4B O1A 0.95 2.48 3.365(4) 154.1 2_776
C7B H7B Cl18 0.95 2.88 3.541(13) 127.8 1_655

_refine_diff_density_max         1.003
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.087


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method chloroform
