# 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_compound12
_database_code_depnum_ccdc_archive 'CCDC 1514274'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2015-04-20
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H40 Cl6 Si3'
_chemical_formula_sum            'C34 H40 Cl6 Si3'
_chemical_formula_weight         745.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c6 h6 Cl f si'
_chemical_oxdiff_usercomment     'C40 H34 Si3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.7815(4)
_cell_length_b                   17.1132(5)
_cell_length_c                   17.4795(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.751(3)
_cell_angle_gamma                90
_cell_volume                     3713.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4807
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.9450
_cell_measurement_theta_min      3.5590
_exptl_absorpt_coefficient_mu    5.324
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1552
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 4 -4 0.0508
5 -2 -10 0.0309
-5 2 10 0.0082
2 5 9 0.0579
4 -2 8 0.0568
3 -10 3 0.0431
0 -10 -5 0.0492
-4 1 -9 0.0336
-2 11 0 0.0315
6 -7 -4 0.0244
-7 -6 2 0.0492

_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.043
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.5809 4.3230 -3.7651 0.9222 0.1718 0.3466
5.1564 -1.5380 -10.1709 0.8293 0.1535 -0.5373
-4.6627 2.0919 10.3885 -0.7816 -0.1445 0.6069
2.4376 4.9854 8.5055 0.0282 -0.1476 0.9887
3.7459 -2.0332 8.4063 0.1334 -0.7152 0.6861
2.9371 -9.7247 2.6794 0.1802 -0.9704 -0.1608
-0.0889 -9.8918 -4.9819 0.0892 -0.4838 -0.8706
-3.6946 1.4439 -8.5614 -0.1264 0.6771 -0.7250
-1.9645 10.7878 0.2688 -0.1603 0.8649 0.4757
5.9893 -6.9951 -4.0013 0.7082 -0.5802 -0.3376
-7.0133 -5.9950 2.0039 -0.8193 -0.2345 -0.5291

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.313
_diffrn_reflns_theta_min         3.560
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -92.00 -23.00   1.00   17.50    --  -38.50 -38.00 150.00   69
  2  ω    -97.00 -47.00   1.00   17.50    --  -38.50-178.00-180.00   50
  3  ω   -122.00 -43.00   1.00   17.50    --  -38.50-178.00 -90.00   79
  4  ω      6.00  66.00   1.00   17.50    --   43.20 -99.00 150.00   60
  5  ω     40.00  75.00   1.00   70.00    --  109.03-125.00 120.00   35
  6  ω     39.00 122.00   1.00   70.00    --  109.03-125.00-120.00   83
  7  ω     79.00 127.00   1.00   70.00    --  109.03  77.00 -60.00   48
  8  ω    102.00 156.00   1.00   70.00    --  109.03  30.00   0.00   54
  9  ω     50.00 120.00   1.00   70.00    --  109.03-125.00  90.00   70
 10  ω     53.00 126.00   1.00   70.00    --  109.03 -15.00 -60.00   73
 11  ω     57.00 116.00   1.00   70.00    --  109.03 -77.00-150.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1042652000
_diffrn_orient_matrix_UB_12      0.0048557000
_diffrn_orient_matrix_UB_13      -0.0294126000
_diffrn_orient_matrix_UB_21      -0.0431361000
_diffrn_orient_matrix_UB_22      0.0735126000
_diffrn_orient_matrix_UB_23      -0.0480743000
_diffrn_orient_matrix_UB_31      0.0515640000
_diffrn_orient_matrix_UB_32      0.0517159000
_diffrn_orient_matrix_UB_33      0.0711470000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5606
_reflns_number_total             7396
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7396
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0676
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1217P)²+3.9325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2055
_refine_special_details          
;
One SiCl2 Me group (Si3, Cl5+6, C34)  disordered at three positions  
by rotation of approx. 120 deg about the Si3-C33 axis, ratio 46:38:16.
The C34 atom of the part with an occupancy of 38% shows a non-classical 
hydrogen bridgeto Cl4b of the neighbouring SiCl2Me-group introducing 
a disorder at Cl4 with ratio 38:62.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cl1 Cl 0.34349(8) 0.35555(6) 0.28648(6) 0.0443(3) Uani 1 1 d . . . . .
Cl2 Cl 0.34767(9) 0.43834(7) 0.11805(7) 0.0494(3) Uani 1 1 d . . . . .
Cl3 Cl 0.40658(11) 0.08527(10) 0.00639(8) 0.0656(4) Uani 1 1 d . . . A 1
Cl4A Cl 0.4443(4) 0.1830(2) 0.1623(2) 0.0902(13) Uani 0.619(3) 1 d . . P A 1
Cl4B Cl 0.4118(4) 0.1637(3) 0.1898(4) 0.0623(12) Uani 0.381(3) 1 d . . P A 2
Cl5A Cl 0.65032(11) 0.26784(10) 0.50908(14) 0.0735(6) Uani 0.842(3) 1 d . . P A
3
Cl6A Cl 0.5898(2) 0.14503(18) 0.36586(15) 0.0671(7) Uani 0.619(3) 1 d . . P A 1
Cl6B Cl 0.5927(2) 0.0860(2) 0.54275(19) 0.0689(8) Uani 0.539(3) 1 d . . P A 4
Si1 Si 0.24576(8) 0.39329(6) 0.18164(6) 0.0298(2) Uani 1 1 d . . . . .
Si2 Si 0.47292(12) 0.07422(8) 0.12493(8) 0.0528(4) Uani 1 1 d . . . . .
Si3 Si 0.55348(9) 0.17278(7) 0.46924(8) 0.0432(3) Uani 1 1 d . . . . .
C1 C 0.1469(3) 0.09217(19) 0.25710(18) 0.0229(6) Uani 1 1 d . . . . .
H1 H 0.2123 0.1171 0.2487 0.028 Uiso 1 1 calc R U . . .
C2 C 0.0454(3) 0.1201(2) 0.19318(19) 0.0250(7) Uani 1 1 d . . . . .
C3 C 0.0025(3) 0.0452(2) 0.1503(2) 0.0280(7) Uani 1 1 d . . . . .
C4 C -0.0865(3) 0.0370(2) 0.0867(2) 0.0355(8) Uani 1 1 d . . . . .
H4 H -0.1259 0.0806 0.0650 0.043 Uiso 1 1 calc R U . . .
C5 C -0.1154(3) -0.0368(3) 0.0563(2) 0.0408(9) Uani 1 1 d . . . . .
H5 H -0.1745 -0.0426 0.0138 0.049 Uiso 1 1 calc R U . . .
C6 C -0.0564(4) -0.1024(3) 0.0889(3) 0.0442(10) Uani 1 1 d . . . . .
H6 H -0.0770 -0.1517 0.0684 0.053 Uiso 1 1 calc R U . . .
C7 C 0.0326(4) -0.0945(2) 0.1514(2) 0.0385(9) Uani 1 1 d . . . . .
H7 H 0.0726 -0.1380 0.1728 0.046 Uiso 1 1 calc R U . . .
C8 C 0.0613(3) -0.0198(2) 0.1819(2) 0.0295(7) Uani 1 1 d . . . . .
C9 C 0.1547(3) 0.0011(2) 0.25072(19) 0.0256(7) Uani 1 1 d . . . . .
C10 C 0.1386(3) -0.0276(2) 0.3294(2) 0.0252(7) Uani 1 1 d . . . . .
C11 C 0.1345(3) -0.1050(2) 0.3537(2) 0.0286(7) Uani 1 1 d . . . . .
H11 H 0.1393 -0.1459 0.3198 0.034 Uiso 1 1 calc R U . . .
C12 C 0.1230(3) -0.1201(2) 0.4295(2) 0.0308(7) Uani 1 1 d . . . . .
H12 H 0.1197 -0.1714 0.4463 0.037 Uiso 1 1 calc R U . . .
C13 C 0.1165(3) -0.0586(2) 0.4802(2) 0.0307(7) Uani 1 1 d . . . . .
H13 H 0.1103 -0.0690 0.5312 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1191(3) 0.0183(2) 0.4552(2) 0.0277(7) Uani 1 1 d . . . . .
H14 H 0.1142 0.0592 0.4892 0.033 Uiso 1 1 calc R U . . .
C15 C 0.1293(3) 0.03369(19) 0.37933(19) 0.0237(6) Uani 1 1 d . . . . .
C16 C 0.1301(3) 0.1129(2) 0.34023(19) 0.0238(7) Uani 1 1 d . . . . .
C17 C 0.0191(3) 0.15006(19) 0.3223(2) 0.0241(7) Uani 1 1 d . . . . .
C18 C -0.0359(3) 0.1794(2) 0.3758(2) 0.0286(7) Uani 1 1 d . . . . .
H18 H -0.0035 0.1791 0.4294 0.034 Uiso 1 1 calc R U . . .
C19 C -0.1396(3) 0.2094(2) 0.3491(2) 0.0337(8) Uani 1 1 d . . . . .
H19 H -0.1772 0.2280 0.3848 0.040 Uiso 1 1 calc R U . . .
C20 C -0.1866(3) 0.2112(2) 0.2686(2) 0.0340(8) Uani 1 1 d . . . . .
H20 H -0.2558 0.2312 0.2508 0.041 Uiso 1 1 calc R U . . .
C21 C -0.1312(3) 0.1834(2) 0.2145(2) 0.0309(8) Uani 1 1 d . . . . .
H21 H -0.1627 0.1853 0.1608 0.037 Uiso 1 1 calc R U . . .
C22 C -0.0280(3) 0.15283(19) 0.2417(2) 0.0256(7) Uani 1 1 d . . . . .
C23 C 0.0735(3) 0.1812(2) 0.1367(2) 0.0278(7) Uani 1 1 d . . . . .
H23A H 0.1245 0.1585 0.1098 0.033 Uiso 1 1 calc R U . . .
H23B H 0.0088 0.1943 0.0971 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1216(3) 0.2558(2) 0.1783(2) 0.0287(7) Uani 1 1 d . . . . .
H24A H 0.1739 0.2419 0.2263 0.034 Uiso 1 1 calc R U . . .
H24B H 0.0648 0.2856 0.1930 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1765(3) 0.3073(2) 0.1278(2) 0.0296(7) Uani 1 1 d . . . . .
H25A H 0.1228 0.3253 0.0822 0.035 Uiso 1 1 calc R U . . .
H25B H 0.2287 0.2761 0.1091 0.035 Uiso 1 1 calc R U . . .
C26 C 0.1546(4) 0.4690(3) 0.2010(3) 0.0457(10) Uani 1 1 d . . . . .
H26A H 0.1959 0.5115 0.2289 0.068 Uiso 1 1 calc R U . . .
H26B H 0.1109 0.4878 0.1520 0.068 Uiso 1 1 calc R U . . .
H26C H 0.1092 0.4477 0.2323 0.068 Uiso 1 1 calc R U . . .
C27 C 0.2654(3) -0.0268(2) 0.2397(2) 0.0335(8) Uani 1 1 d . . . . .
H27A H 0.3213 -0.0071 0.2831 0.040 Uiso 1 1 calc R U . . .
H27B H 0.2677 -0.0834 0.2424 0.040 Uiso 1 1 calc R U . . .
C28 C 0.2906(4) -0.0012(4) 0.1627(3) 0.0582(15) Uani 1 1 d . . . . .
H28A H 0.2683 0.0527 0.1522 0.070 Uiso 1 1 calc R U . . .
H28B H 0.2494 -0.0330 0.1201 0.070 Uiso 1 1 calc R U . . .
C29 C 0.4120(4) -0.0085(4) 0.1645(3) 0.0591(14) Uani 1 1 d . . . . .
H29A H 0.4220 -0.0549 0.1351 0.071 Uiso 1 1 calc R U . . .
H29B H 0.4511 -0.0166 0.2187 0.071 Uiso 1 1 calc R U . . .
C30 C 0.6193(4) 0.0694(4) 0.1444(4) 0.0733(19) Uani 1 1 d . . . B 1
H30A H 0.6458 0.1144 0.1221 0.110 Uiso 1 1 calc R U . B 1
H30B H 0.6492 0.0683 0.2002 0.110 Uiso 1 1 calc R U . B 1
H30C H 0.6400 0.0229 0.1211 0.110 Uiso 1 1 calc R U . B 1
C31 C 0.2144(3) 0.16892(19) 0.3892(2) 0.0252(7) Uani 1 1 d . . . . .
H31A H 0.2095 0.2185 0.3617 0.030 Uiso 1 1 calc R U . . .
H31B H 0.1961 0.1783 0.4391 0.030 Uiso 1 1 calc R U . . .
C32 C 0.3313(3) 0.1407(2) 0.4057(2) 0.0300(7) Uani 1 1 d . . . . .
H32A H 0.3502 0.1299 0.3562 0.036 Uiso 1 1 calc R U . . .
H32B H 0.3382 0.0924 0.4356 0.036 Uiso 1 1 calc R U . . .
C33 C 0.4097(3) 0.2016(2) 0.4520(2) 0.0373(9) Uani 1 1 d . . . . .
H33A H 0.3925 0.2103 0.5025 0.045 Uiso 1 1 calc R U . . .
H33B H 0.3992 0.2506 0.4234 0.045 Uiso 1 1 calc R U . . .
C34A C 0.5845(12) 0.1197(10) 0.5705(10) 0.0689(8) Uani 0.461(3) 1 d . . P A 3
H34A H 0.6583 0.1028 0.5836 0.103 Uiso 0.461(3) 1 calc R U P A 3
H34B H 0.5724 0.1549 0.6103 0.103 Uiso 0.461(3) 1 calc R U P A 3
H34C H 0.5381 0.0751 0.5676 0.103 Uiso 0.461(3) 1 calc R U P A 3
C34B C 0.5979(15) 0.1764(14) 0.3870(12) 0.0671(7) Uani 0.381(3) 1 d . . P A 2
H34D H 0.6723 0.1611 0.3984 0.101 Uiso 0.381(3) 1 calc R U P A 2
H34E H 0.5563 0.1415 0.3486 0.101 Uiso 0.381(3) 1 calc R U P A 2
H34F H 0.5908 0.2287 0.3666 0.101 Uiso 0.381(3) 1 calc R U P A 2
C34C C 0.629(3) 0.243(2) 0.565(3) 0.0735(6) Uani 0.158(3) 1 d . . P A 4
H34G H 0.7047 0.2325 0.5783 0.110 Uiso 0.158(3) 1 calc R U P A 4
H34H H 0.6172 0.2973 0.5504 0.110 Uiso 0.158(3) 1 calc R U P A 4
H34I H 0.5990 0.2322 0.6090 0.110 Uiso 0.158(3) 1 calc R U P A 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Si1 2.0609(13) . ?
Cl2 Si1 2.0530(14) . ?
Cl3 Si2 2.0525(19) . ?
Cl4A Si2 2.034(4) . ?
Cl4B Si2 2.159(5) . ?
Cl5A Si3 2.0624(18) . ?
Cl6A Si3 2.026(3) . ?
Cl6B Si3 1.950(3) . ?
Si1 C25 1.854(4) . ?
Si1 C26 1.827(4) . ?
Si2 C29 1.829(6) . ?
Si2 C30 1.822(6) . ?
Si3 C33 1.857(4) . ?
Si3 C34A 1.946(15) . ?
Si3 C34B 1.668(19) . ?
Si3 C34C 2.10(4) . ?
C1 H1 0.9800 . ?
C1 C2 1.572(4) . ?
C1 C9 1.567(5) . ?
C1 C16 1.559(5) . ?
C2 C3 1.520(5) . ?
C2 C22 1.513(5) . ?
C2 C23 1.538(5) . ?
C3 C4 1.395(5) . ?
C3 C8 1.382(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.386(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.399(5) . ?
C8 C9 1.522(5) . ?
C9 C10 1.519(5) . ?
C9 C27 1.549(5) . ?
C10 C11 1.396(5) . ?
C10 C15 1.388(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.391(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.391(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.389(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(5) . ?
C15 C16 1.519(4) . ?
C16 C17 1.519(4) . ?
C16 C31 1.541(4) . ?
C17 C18 1.391(5) . ?
C17 C22 1.395(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.394(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.393(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.393(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.393(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.526(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.530(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.520(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.550(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.531(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.536(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
C34C H34G 0.9600 . ?
C34C H34H 0.9600 . ?
C34C H34I 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Si1 Cl1 105.70(6) . . ?
C25 Si1 Cl1 108.52(12) . . ?
C25 Si1 Cl2 108.14(13) . . ?
C26 Si1 Cl1 109.64(17) . . ?
C26 Si1 Cl2 110.37(17) . . ?
C26 Si1 C25 114.11(19) . . ?
Cl4A Si2 Cl3 100.20(12) . . ?
C29 Si2 Cl3 110.0(2) . . ?
C29 Si2 Cl4A 117.5(2) . . ?
C29 Si2 Cl4B 96.4(2) . . ?
C30 Si2 Cl3 110.6(2) . . ?
C30 Si2 Cl4A 103.7(3) . . ?
C30 Si2 C29 113.9(2) . . ?
Cl6B Si3 C34C 85.2(15) . . ?
C33 Si3 Cl5A 109.67(14) . . ?
C33 Si3 Cl6A 110.21(16) . . ?
C33 Si3 Cl6B 113.49(17) . . ?
C33 Si3 C34A 104.6(5) . . ?
C33 Si3 C34C 103.0(10) . . ?
C34A Si3 Cl5A 94.9(5) . . ?
C34B Si3 C33 112.2(7) . . ?
C2 C1 H1 110.5 . . ?
C9 C1 H1 110.5 . . ?
C9 C1 C2 107.9(3) . . ?
C16 C1 H1 110.5 . . ?
C16 C1 C2 108.7(3) . . ?
C16 C1 C9 108.5(3) . . ?
C3 C2 C1 103.5(3) . . ?
C3 C2 C23 111.6(3) . . ?
C22 C2 C1 103.3(3) . . ?
C22 C2 C3 112.9(3) . . ?
C22 C2 C23 112.3(3) . . ?
C23 C2 C1 112.6(3) . . ?
C4 C3 C2 127.4(3) . . ?
C8 C3 C2 112.6(3) . . ?
C8 C3 C4 120.0(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.5(4) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.6 . . ?
C6 C7 C8 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C3 C8 C7 121.0(3) . . ?
C3 C8 C9 112.1(3) . . ?
C7 C8 C9 126.9(3) . . ?
C8 C9 C1 103.8(3) . . ?
C8 C9 C27 113.4(3) . . ?
C10 C9 C1 103.5(3) . . ?
C10 C9 C8 112.9(3) . . ?
C10 C9 C27 109.7(3) . . ?
C27 C9 C1 113.0(3) . . ?
C11 C10 C9 127.3(3) . . ?
C15 C10 C9 112.0(3) . . ?
C15 C10 C11 120.7(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.2(3) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.1(3) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.7(3) . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C14 119.9(3) . . ?
C10 C15 C16 112.4(3) . . ?
C14 C15 C16 127.7(3) . . ?
C15 C16 C1 103.5(3) . . ?
C15 C16 C31 112.6(3) . . ?
C17 C16 C1 103.4(3) . . ?
C17 C16 C15 111.1(3) . . ?
C17 C16 C31 110.5(3) . . ?
C31 C16 C1 115.2(3) . . ?
C18 C17 C16 127.6(3) . . ?
C18 C17 C22 120.1(3) . . ?
C22 C17 C16 112.3(3) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(4) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.3(3) . . ?
C22 C21 H21 120.3 . . ?
C17 C22 C2 112.2(3) . . ?
C21 C22 C2 127.6(3) . . ?
C21 C22 C17 120.2(3) . . ?
C2 C23 H23A 109.0 . . ?
C2 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C24 C23 C2 113.1(3) . . ?
C24 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C23 C24 C25 113.3(3) . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
Si1 C25 H25A 108.9 . . ?
Si1 C25 H25B 108.9 . . ?
C24 C25 Si1 113.2(2) . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.8 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C9 C27 H27A 108.7 . . ?
C9 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 C9 114.4(3) . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
C27 C28 C29 112.4(4) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.1 . . ?
C29 C28 H28B 109.1 . . ?
Si2 C29 H29A 108.2 . . ?
Si2 C29 H29B 108.2 . . ?
C28 C29 Si2 116.4(4) . . ?
C28 C29 H29A 108.2 . . ?
C28 C29 H29B 108.2 . . ?
H29A C29 H29B 107.3 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C16 C31 H31A 108.4 . . ?
C16 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 C16 115.5(3) . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C31 C32 C33 111.7(3) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
Si3 C33 H33A 108.8 . . ?
Si3 C33 H33B 108.8 . . ?
C32 C33 Si3 113.7(3) . . ?
C32 C33 H33A 108.8 . . ?
C32 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
Si3 C34A H34A 109.5 . . ?
Si3 C34A H34B 109.5 . . ?
Si3 C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
Si3 C34B H34D 109.5 . . ?
Si3 C34B H34E 109.5 . . ?
Si3 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
Si3 C34C H34G 109.5 . . ?
Si3 C34C H34H 109.5 . . ?
Si3 C34C H34I 109.5 . . ?
H34G C34C H34H 109.5 . . ?
H34G C34C H34I 109.5 . . ?
H34H C34C H34I 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 Si1 C25 C24 50.5(3) . . . . ?
Cl2 Si1 C25 C24 164.7(2) . . . . ?
Cl3 Si2 C29 C28 -65.4(5) . . . . ?
Cl4A Si2 C29 C28 48.3(5) . . . . ?
Cl4B Si2 C29 C28 49.2(5) . . . . ?
Cl5A Si3 C33 C32 167.5(3) . . . . ?
Cl6A Si3 C33 C32 53.7(3) . . . . ?
Cl6B Si3 C33 C32 -69.3(3) . . . . ?
C1 C2 C3 C4 -178.8(4) . . . . ?
C1 C2 C3 C8 2.2(4) . . . . ?
C1 C2 C22 C17 2.4(4) . . . . ?
C1 C2 C22 C21 -177.8(3) . . . . ?
C1 C2 C23 C24 -61.5(4) . . . . ?
C1 C9 C10 C11 177.6(3) . . . . ?
C1 C9 C10 C15 -3.4(4) . . . . ?
C1 C9 C27 C28 -65.0(5) . . . . ?
C1 C16 C17 C18 180.0(3) . . . . ?
C1 C16 C17 C22 0.1(4) . . . . ?
C1 C16 C31 C32 -58.8(4) . . . . ?
C2 C1 C9 C8 2.3(4) . . . . ?
C2 C1 C9 C10 -115.9(3) . . . . ?
C2 C1 C9 C27 125.6(3) . . . . ?
C2 C1 C16 C15 117.4(3) . . . . ?
C2 C1 C16 C17 1.4(3) . . . . ?
C2 C1 C16 C31 -119.2(3) . . . . ?
C2 C3 C4 C5 -178.4(4) . . . . ?
C2 C3 C8 C7 178.5(4) . . . . ?
C2 C3 C8 C9 -0.8(4) . . . . ?
C2 C23 C24 C25 164.9(3) . . . . ?
C3 C2 C22 C17 113.5(3) . . . . ?
C3 C2 C22 C21 -66.6(4) . . . . ?
C3 C2 C23 C24 -177.4(3) . . . . ?
C3 C4 C5 C6 0.1(7) . . . . ?
C3 C8 C9 C1 -1.0(4) . . . . ?
C3 C8 C9 C10 110.4(4) . . . . ?
C3 C8 C9 C27 -124.1(3) . . . . ?
C4 C3 C8 C7 -0.6(6) . . . . ?
C4 C3 C8 C9 -179.9(3) . . . . ?
C4 C5 C6 C7 -0.8(7) . . . . ?
C5 C6 C7 C8 0.8(7) . . . . ?
C6 C7 C8 C3 -0.1(6) . . . . ?
C6 C7 C8 C9 179.1(4) . . . . ?
C7 C8 C9 C1 179.7(4) . . . . ?
C7 C8 C9 C10 -68.9(5) . . . . ?
C7 C8 C9 C27 56.7(5) . . . . ?
C8 C3 C4 C5 0.6(6) . . . . ?
C8 C9 C10 C11 66.0(4) . . . . ?
C8 C9 C10 C15 -115.0(3) . . . . ?
C8 C9 C27 C28 52.9(5) . . . . ?
C9 C1 C2 C3 -2.7(3) . . . . ?
C9 C1 C2 C22 115.2(3) . . . . ?
C9 C1 C2 C23 -123.4(3) . . . . ?
C9 C1 C16 C15 0.3(3) . . . . ?
C9 C1 C16 C17 -115.7(3) . . . . ?
C9 C1 C16 C31 123.6(3) . . . . ?
C9 C10 C11 C12 177.7(3) . . . . ?
C9 C10 C15 C14 -177.0(3) . . . . ?
C9 C10 C15 C16 3.8(4) . . . . ?
C9 C27 C28 C29 163.0(4) . . . . ?
C10 C9 C27 C28 -179.9(4) . . . . ?
C10 C11 C12 C13 -0.4(5) . . . . ?
C10 C15 C16 C1 -2.5(3) . . . . ?
C10 C15 C16 C17 107.9(3) . . . . ?
C10 C15 C16 C31 -127.6(3) . . . . ?
C11 C10 C15 C14 2.0(5) . . . . ?
C11 C10 C15 C16 -177.1(3) . . . . ?
C11 C12 C13 C14 1.3(5) . . . . ?
C12 C13 C14 C15 -0.6(5) . . . . ?
C13 C14 C15 C10 -1.1(5) . . . . ?
C13 C14 C15 C16 177.9(3) . . . . ?
C14 C15 C16 C1 178.5(3) . . . . ?
C14 C15 C16 C17 -71.1(4) . . . . ?
C14 C15 C16 C31 53.4(5) . . . . ?
C15 C10 C11 C12 -1.2(5) . . . . ?
C15 C16 C17 C18 69.5(4) . . . . ?
C15 C16 C17 C22 -110.4(3) . . . . ?
C15 C16 C31 C32 59.6(4) . . . . ?
C16 C1 C2 C3 -120.2(3) . . . . ?
C16 C1 C2 C22 -2.2(3) . . . . ?
C16 C1 C2 C23 119.1(3) . . . . ?
C16 C1 C9 C8 119.9(3) . . . . ?
C16 C1 C9 C10 1.7(3) . . . . ?
C16 C1 C9 C27 -116.8(3) . . . . ?
C16 C17 C18 C19 -177.8(3) . . . . ?
C16 C17 C22 C2 -1.6(4) . . . . ?
C16 C17 C22 C21 178.5(3) . . . . ?
C16 C31 C32 C33 177.8(3) . . . . ?
C17 C16 C31 C32 -175.5(3) . . . . ?
C17 C18 C19 C20 -1.4(5) . . . . ?
C18 C17 C22 C2 178.5(3) . . . . ?
C18 C17 C22 C21 -1.4(5) . . . . ?
C18 C19 C20 C21 0.0(6) . . . . ?
C19 C20 C21 C22 0.7(5) . . . . ?
C20 C21 C22 C2 -179.8(3) . . . . ?
C20 C21 C22 C17 0.0(5) . . . . ?
C22 C2 C3 C4 70.1(5) . . . . ?
C22 C2 C3 C8 -108.9(3) . . . . ?
C22 C2 C23 C24 54.6(4) . . . . ?
C22 C17 C18 C19 2.1(5) . . . . ?
C23 C2 C3 C4 -57.5(5) . . . . ?
C23 C2 C3 C8 123.5(3) . . . . ?
C23 C2 C22 C17 -119.2(3) . . . . ?
C23 C2 C22 C21 60.7(4) . . . . ?
C23 C24 C25 Si1 -174.7(2) . . . . ?
C26 Si1 C25 C24 -72.0(3) . . . . ?
C27 C9 C10 C11 -61.5(4) . . . . ?
C27 C9 C10 C15 117.5(3) . . . . ?
C27 C28 C29 Si2 -135.1(4) . . . . ?
C30 Si2 C29 C28 169.8(5) . . . . ?
C31 C16 C17 C18 -56.2(4) . . . . ?
C31 C16 C17 C22 123.9(3) . . . . ?
C31 C32 C33 Si3 -176.9(3) . . . . ?
C34A Si3 C33 C32 -91.8(7) . . . . ?
C34B Si3 C33 C32 71.6(9) . . . . ?
C34C Si3 C33 C32 -159.7(16) . . . . ?

_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.885
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1514268'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-10-21
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H22'
_chemical_formula_sum            'C25 H22'
_chemical_formula_weight         322.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25 H22'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'

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

_cell_length_a                   8.75501(19)
_cell_length_b                   12.8417(2)
_cell_length_c                   16.3598(3)
_cell_angle_alpha                99.9308(15)
_cell_angle_beta                 94.5032(15)
_cell_angle_gamma                97.3754(16)
_cell_volume                     1787.22(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16180
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.0400
_cell_measurement_theta_min      3.5280
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.3178
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31757
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.994
_diffrn_reflns_theta_min         2.757
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -38.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
  2 omega  -64.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega   14.00   50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega   14.00  115.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   90.0000 101

#__ type_ start__ end____ width___ exp.time_
  5 omega   20.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 48

#__ type_ start__ end____ width___ exp.time_
  6 omega   14.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega   13.00   45.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
  8 omega   55.00  101.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -30.0000 46

#__ type_ start__ end____ width___ exp.time_
  9 omega   14.00   80.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
 10 omega   82.00  124.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000   60.0000 42

#__ type_ start__ end____ width___ exp.time_
 11 omega   87.00  113.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 12 omega    2.00   67.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  -99.0000   90.0000 65

#__ type_ start__ end____ width___ exp.time_
 13 omega   18.00   53.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -30.0000 35

#__ type_ start__ end____ width___ exp.time_
 14 omega   57.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -120.0000 32

#__ type_ start__ end____ width___ exp.time_
 15 omega   83.00  113.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
 16 omega   96.00  126.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00  115.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 58

#__ type_ start__ end____ width___ exp.time_
 18 omega   54.00   81.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 19 omega   24.00   99.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000 -150.0000 75

#__ type_ start__ end____ width___ exp.time_
 20 omega   81.00  172.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
 21 omega   37.00  102.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 65

#__ type_ start__ end____ width___ exp.time_
 22 omega  132.00  166.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000  -76.2844 34

#__ type_ start__ end____ width___ exp.time_
 23 omega   42.00   97.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 55

#__ type_ start__ end____ width___ exp.time_
 24 omega   31.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 77

#__ type_ start__ end____ width___ exp.time_
 25 omega   82.00  107.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   85.00  112.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   81.00  109.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 28 omega   41.00   97.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
 29 omega   81.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
 30 omega   81.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 31 omega   86.00  111.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 32 omega   81.00  109.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000  -76.2844 28

#__ type_ start__ end____ width___ exp.time_
 33 omega   82.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   74.0000 -173.6747 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   85.00  112.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 35 omega   86.00  111.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 36 omega  153.00  178.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 37 omega   81.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 38 omega   85.00  124.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 39

#__ type_ start__ end____ width___ exp.time_
 39 omega   85.00  111.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 40 omega   83.00  108.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000   -3.0671 25

#__ type_ start__ end____ width___ exp.time_
 41 omega   81.00  177.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
 42 omega   74.00  119.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
 43 omega   81.00  159.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 78

#__ type_ start__ end____ width___ exp.time_
 44 omega   81.00  178.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
 45 omega   85.00  116.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 31

#__ type_ start__ end____ width___ exp.time_
 46 omega   81.00  107.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 47 omega  140.00  166.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 48 omega   81.00  107.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 49 omega   85.00  164.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 79

#__ type_ start__ end____ width___ exp.time_
 50 omega   89.00  152.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 63

#__ type_ start__ end____ width___ exp.time_
 51 omega   44.00  122.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 78

#__ type_ start__ end____ width___ exp.time_
 52 omega   85.00  169.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
 53 omega   49.00  105.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 56

#__ type_ start__ end____ width___ exp.time_
 54 omega  128.00  156.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
 55 omega   85.00  111.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 56 omega   33.00   90.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 57

#__ type_ start__ end____ width___ exp.time_
 57 omega   81.00  112.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000 -167.5388 31

#__ type_ start__ end____ width___ exp.time_
 58 omega   84.00  157.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   64.0000  126.6685 73

#__ type_ start__ end____ width___ exp.time_
 59 omega   81.00  178.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   55.2604 97

#__ type_ start__ end____ width___ exp.time_
 60 omega   86.00  160.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   58.0000 -169.7303 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0171970000
_diffrn_orient_matrix_UB_12      0.0808854000
_diffrn_orient_matrix_UB_13      -0.0593058000
_diffrn_orient_matrix_UB_21      0.0984885000
_diffrn_orient_matrix_UB_22      0.0823050000
_diffrn_orient_matrix_UB_23      0.0702649000
_diffrn_orient_matrix_UB_31      0.1477297000
_diffrn_orient_matrix_UB_32      -0.0428091000
_diffrn_orient_matrix_UB_33      -0.0279827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6211
_reflns_number_total             7020
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         7020
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0463P)²+0.5065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0920
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.95318(12) 0.23885(8) 0.13467(6) 0.0184(2) Uani 1 1 d . . . . .
H1 H 0.9952(15) 0.1935(11) 0.1727(8) 0.021(3) Uiso 1 1 d . . . . .
C2 C 1.03532(12) 0.22860(8) 0.05286(6) 0.0200(2) Uani 1 1 d . . . . .
C3 C 0.90186(12) 0.19120(8) -0.01572(7) 0.0200(2) Uani 1 1 d . . . . .
C4 C 0.91035(14) 0.17204(9) -0.10154(7) 0.0253(2) Uani 1 1 d . . . . .
H4 H 1.0119(18) 0.1850(12) -0.1238(9) 0.033(4) Uiso 1 1 d . . . . .
C5 C 0.77482(14) 0.13606(9) -0.15475(7) 0.0264(2) Uani 1 1 d . . . . .
H5 H 0.7795(17) 0.1223(12) -0.2161(10) 0.032(4) Uiso 1 1 d . . . . .
C6 C 0.63343(14) 0.11781(9) -0.12297(7) 0.0253(2) Uani 1 1 d . . . . .
H6 H 0.5387(18) 0.0907(12) -0.1618(9) 0.032(4) Uiso 1 1 d . . . . .
C7 C 0.62495(13) 0.13729(9) -0.03721(7) 0.0235(2) Uani 1 1 d . . . . .
H7 H 0.5234(17) 0.1251(12) -0.0150(9) 0.028(3) Uiso 1 1 d . . . . .
C8 C 0.76016(13) 0.17542(8) 0.01608(6) 0.0194(2) Uani 1 1 d . . . . .
C9 C 0.77549(12) 0.20475(8) 0.11063(6) 0.0192(2) Uani 1 1 d . . . . .
C10 C 0.70696(12) 0.30535(9) 0.14128(6) 0.0195(2) Uani 1 1 d . . . . .
C11 C 0.55190(13) 0.31919(10) 0.13462(7) 0.0245(2) Uani 1 1 d . . . . .
H11 H 0.4720(18) 0.2601(12) 0.1066(9) 0.031(4) Uiso 1 1 d . . . . .
C12 C 0.51027(14) 0.41744(10) 0.16792(7) 0.0278(2) Uani 1 1 d . . . . .
H12 H 0.4013(19) 0.4269(12) 0.1638(9) 0.033(4) Uiso 1 1 d . . . . .
C13 C 0.62305(15) 0.50058(10) 0.20795(8) 0.0293(3) Uani 1 1 d . . . . .
H13 H 0.5914(19) 0.5703(14) 0.2322(10) 0.040(4) Uiso 1 1 d . . . . .
C14 C 0.77812(14) 0.48717(9) 0.21455(7) 0.0257(2) Uani 1 1 d . . . . .
H14 H 0.8596(18) 0.5459(13) 0.2430(10) 0.034(4) Uiso 1 1 d . . . . .
C15 C 0.81995(12) 0.38925(9) 0.18026(6) 0.0197(2) Uani 1 1 d . . . . .
C16 C 0.98152(12) 0.35875(8) 0.17867(6) 0.0189(2) Uani 1 1 d . . . . .
C17 C 1.07708(12) 0.41388(9) 0.12052(6) 0.0194(2) Uani 1 1 d . . . . .
C18 C 1.13110(13) 0.52253(9) 0.12958(7) 0.0239(2) Uani 1 1 d . . . . .
H18 H 1.1041(17) 0.5747(12) 0.1761(9) 0.030(4) Uiso 1 1 d . . . . .
C19 C 1.22149(14) 0.55818(10) 0.07092(8) 0.0278(2) Uani 1 1 d . . . . .
H19 H 1.2599(18) 0.6344(13) 0.0773(10) 0.035(4) Uiso 1 1 d . . . . .
C20 C 1.25826(14) 0.48623(10) 0.00418(8) 0.0287(3) Uani 1 1 d . . . . .
H20 H 1.3240(19) 0.5127(13) -0.0359(10) 0.038(4) Uiso 1 1 d . . . . .
C21 C 1.20279(13) 0.37803(10) -0.00540(7) 0.0259(2) Uani 1 1 d . . . . .
H21 H 1.2307(17) 0.3261(12) -0.0539(10) 0.033(4) Uiso 1 1 d . . . . .
C22 C 1.11121(12) 0.34213(9) 0.05291(7) 0.0205(2) Uani 1 1 d . . . . .
C23 C 1.15143(13) 0.14849(10) 0.04897(8) 0.0260(2) Uani 1 1 d . . . . .
H23A H 1.2064(18) 0.1471(12) -0.0025(10) 0.035(4) Uiso 1 1 d . . . . .
H23B H 1.2318(18) 0.1683(12) 0.0983(10) 0.032(4) Uiso 1 1 d . . . . .
H23C H 1.0973(18) 0.0745(13) 0.0491(9) 0.034(4) Uiso 1 1 d . . . . .
C24 C 0.70684(14) 0.11105(9) 0.14993(7) 0.0256(2) Uani 1 1 d . . . . .
H24A H 0.7220(16) 0.1313(11) 0.2107(9) 0.027(3) Uiso 1 1 d . . . . .
H24B H 0.5934(18) 0.0931(12) 0.1326(9) 0.032(4) Uiso 1 1 d . . . . .
H24C H 0.7588(17) 0.0437(12) 0.1315(9) 0.030(4) Uiso 1 1 d . . . . .
C25 C 1.06652(14) 0.37742(9) 0.26693(7) 0.0255(2) Uani 1 1 d . . . . .
H25A H 1.0822(17) 0.4549(13) 0.2918(9) 0.031(4) Uiso 1 1 d . . . . .
H25B H 1.0050(18) 0.3379(13) 0.3048(10) 0.036(4) Uiso 1 1 d . . . . .
H25C H 1.172(2) 0.3540(13) 0.2654(10) 0.038(4) Uiso 1 1 d . . . . .
C26 C 0.56054(13) 0.67352(8) 0.49238(6) 0.0196(2) Uani 1 1 d . . . . .
H26 H 0.5246(15) 0.5967(11) 0.4938(8) 0.019(3) Uiso 1 1 d . . . . .
C27 C 0.47324(12) 0.70802(8) 0.41638(6) 0.0198(2) Uani 1 1 d . . . . .
C28 C 0.39850(12) 0.80178(8) 0.45617(7) 0.0200(2) Uani 1 1 d . . . . .
C29 C 0.30800(13) 0.86296(9) 0.41605(7) 0.0241(2) Uani 1 1 d . . . . .
H29 H 0.2851(17) 0.8455(12) 0.3545(10) 0.031(4) Uiso 1 1 d . . . . .
C30 C 0.25418(13) 0.94935(9) 0.46252(8) 0.0264(2) Uani 1 1 d . . . . .
H30 H 0.1892(18) 0.9913(12) 0.4338(9) 0.032(4) Uiso 1 1 d . . . . .
C31 C 0.29169(13) 0.97462(9) 0.54855(8) 0.0259(2) Uani 1 1 d . . . . .
H31 H 0.2540(17) 1.0361(13) 0.5808(10) 0.034(4) Uiso 1 1 d . . . . .
C32 C 0.38047(13) 0.91270(9) 0.58882(7) 0.0234(2) Uani 1 1 d . . . . .
H32 H 0.4064(16) 0.9300(11) 0.6509(9) 0.023(3) Uiso 1 1 d . . . . .
C33 C 0.43297(12) 0.82551(8) 0.54232(7) 0.0194(2) Uani 1 1 d . . . . .
C34 C 0.52792(13) 0.74687(8) 0.57415(6) 0.0196(2) Uani 1 1 d . . . . .
C35 C 0.68793(13) 0.80012(8) 0.61317(6) 0.0200(2) Uani 1 1 d . . . . .
C36 C 0.72618(14) 0.86935(9) 0.68983(7) 0.0236(2) Uani 1 1 d . . . . .
H36 H 0.6431(16) 0.8869(11) 0.7271(9) 0.025(3) Uiso 1 1 d . . . . .
C37 C 0.88037(14) 0.91372(9) 0.71341(7) 0.0252(2) Uani 1 1 d . . . . .
H37 H 0.9071(17) 0.9614(12) 0.7683(9) 0.029(4) Uiso 1 1 d . . . . .
C38 C 0.99413(14) 0.89006(9) 0.66142(7) 0.0246(2) Uani 1 1 d . . . . .
H38 H 1.1032(17) 0.9226(11) 0.6782(9) 0.027(3) Uiso 1 1 d . . . . .
C39 C 0.95663(13) 0.81923(9) 0.58582(7) 0.0224(2) Uani 1 1 d . . . . .
H39 H 1.0405(17) 0.8016(11) 0.5499(9) 0.025(3) Uiso 1 1 d . . . . .
C40 C 0.80286(13) 0.77412(8) 0.56252(6) 0.0197(2) Uani 1 1 d . . . . .
C41 C 0.73814(13) 0.69301(8) 0.48436(6) 0.0200(2) Uani 1 1 d . . . . .
C42 C 0.74821(13) 0.73779(8) 0.40456(6) 0.0198(2) Uani 1 1 d . . . . .
C43 C 0.88176(13) 0.76954(9) 0.36900(7) 0.0243(2) Uani 1 1 d . . . . .
H43 H 0.9868(17) 0.7652(11) 0.3956(9) 0.028(4) Uiso 1 1 d . . . . .
C44 C 0.86796(14) 0.80820(10) 0.29489(7) 0.0281(2) Uani 1 1 d . . . . .
H44 H 0.9620(18) 0.8319(12) 0.2693(10) 0.035(4) Uiso 1 1 d . . . . .
C45 C 0.72272(15) 0.81392(10) 0.25614(7) 0.0282(3) Uani 1 1 d . . . . .
H45 H 0.7134(17) 0.8395(12) 0.2027(10) 0.032(4) Uiso 1 1 d . . . . .
C46 C 0.58941(14) 0.78200(9) 0.29180(7) 0.0247(2) Uani 1 1 d . . . . .
H46 H 0.4865(18) 0.7841(12) 0.2637(9) 0.031(4) Uiso 1 1 d . . . . .
C47 C 0.60286(13) 0.74418(8) 0.36647(6) 0.0203(2) Uani 1 1 d . . . . .
C48 C 0.35310(14) 0.61880(9) 0.36437(7) 0.0252(2) Uani 1 1 d . . . . .
H48A H 0.4021(17) 0.5549(12) 0.3430(9) 0.031(4) Uiso 1 1 d . . . . .
H48B H 0.2693(18) 0.5969(12) 0.3998(9) 0.031(4) Uiso 1 1 d . . . . .
H48C H 0.3035(17) 0.6438(12) 0.3160(10) 0.032(4) Uiso 1 1 d . . . . .
C49 C 0.43976(15) 0.68594(10) 0.63301(7) 0.0273(2) Uani 1 1 d . . . . .
H49A H 0.4220(18) 0.7356(13) 0.6848(10) 0.036(4) Uiso 1 1 d . . . . .
H49B H 0.5011(19) 0.6290(13) 0.6505(10) 0.039(4) Uiso 1 1 d . . . . .
H49C H 0.3339(19) 0.6521(13) 0.6066(10) 0.036(4) Uiso 1 1 d . . . . .
C50 C 0.81539(14) 0.59156(9) 0.47931(8) 0.0265(2) Uani 1 1 d . . . . .
H50A H 0.7699(18) 0.5373(12) 0.4291(10) 0.034(4) Uiso 1 1 d . . . . .
H50B H 0.8001(18) 0.5604(12) 0.5308(10) 0.034(4) Uiso 1 1 d . . . . .
H50C H 0.9295(19) 0.6089(12) 0.4750(9) 0.032(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 1.002(14) . ?
C1 C2 1.5622(14) . ?
C1 C9 1.5608(14) . ?
C1 C16 1.5627(14) . ?
C2 C3 1.5228(14) . ?
C2 C22 1.5224(15) . ?
C2 C23 1.5336(15) . ?
C3 C4 1.3925(16) . ?
C3 C8 1.3870(16) . ?
C4 H4 0.992(16) . ?
C4 C5 1.3920(16) . ?
C5 H5 0.994(15) . ?
C5 C6 1.3879(18) . ?
C6 H6 0.990(15) . ?
C6 C7 1.3916(16) . ?
C7 H7 0.991(15) . ?
C7 C8 1.3940(15) . ?
C8 C9 1.5186(14) . ?
C9 C10 1.5177(15) . ?
C9 C24 1.5376(15) . ?
C10 C11 1.3900(16) . ?
C10 C15 1.3915(15) . ?
C11 H11 0.984(15) . ?
C11 C12 1.3904(18) . ?
C12 H12 0.976(16) . ?
C12 C13 1.3894(18) . ?
C13 H13 0.997(17) . ?
C13 C14 1.3885(18) . ?
C14 H14 0.992(16) . ?
C14 C15 1.3919(16) . ?
C15 C16 1.5164(15) . ?
C16 C17 1.5204(14) . ?
C16 C25 1.5368(14) . ?
C17 C18 1.3931(15) . ?
C17 C22 1.3901(16) . ?
C18 H18 0.989(15) . ?
C18 C19 1.3909(17) . ?
C19 H19 0.978(16) . ?
C19 C20 1.3903(19) . ?
C20 H20 0.981(17) . ?
C20 C21 1.3895(18) . ?
C21 H21 1.012(16) . ?
C21 C22 1.3937(16) . ?
C23 H23A 1.002(16) . ?
C23 H23B 1.002(16) . ?
C23 H23C 1.006(16) . ?
C24 H24A 0.978(15) . ?
C24 H24B 0.997(16) . ?
C24 H24C 1.039(15) . ?
C25 H25A 0.995(16) . ?
C25 H25B 1.011(16) . ?
C25 H25C 1.006(17) . ?
C26 H26 1.001(13) . ?
C26 C27 1.5667(14) . ?
C26 C34 1.5662(14) . ?
C26 C41 1.5623(15) . ?
C27 C28 1.5168(15) . ?
C27 C47 1.5202(15) . ?
C27 C48 1.5352(14) . ?
C28 C29 1.3899(16) . ?
C28 C33 1.3899(15) . ?
C29 H29 0.991(15) . ?
C29 C30 1.3893(17) . ?
C30 H30 0.979(16) . ?
C30 C31 1.3915(17) . ?
C31 H31 0.981(16) . ?
C31 C32 1.3890(17) . ?
C32 H32 1.003(14) . ?
C32 C33 1.3918(16) . ?
C33 C34 1.5201(15) . ?
C34 C35 1.5168(15) . ?
C34 C49 1.5352(15) . ?
C35 C36 1.3958(15) . ?
C35 C40 1.3902(16) . ?
C36 H36 1.008(15) . ?
C36 C37 1.3931(17) . ?
C37 H37 0.988(15) . ?
C37 C38 1.3890(18) . ?
C38 H38 0.989(15) . ?
C38 C39 1.3916(16) . ?
C39 H39 0.999(15) . ?
C39 C40 1.3915(16) . ?
C40 C41 1.5219(14) . ?
C41 C42 1.5188(14) . ?
C41 C50 1.5360(15) . ?
C42 C43 1.3921(16) . ?
C42 C47 1.3909(16) . ?
C43 H43 0.998(15) . ?
C43 C44 1.3897(17) . ?
C44 H44 0.990(16) . ?
C44 C45 1.3920(18) . ?
C45 H45 0.986(15) . ?
C45 C46 1.3918(17) . ?
C46 H46 0.984(15) . ?
C46 C47 1.3923(16) . ?
C48 H48A 0.998(16) . ?
C48 H48B 1.011(16) . ?
C48 H48C 0.994(16) . ?
C49 H49A 1.005(16) . ?
C49 H49B 1.026(17) . ?
C49 H49C 1.002(17) . ?
C50 H50A 1.000(16) . ?
C50 H50B 1.004(16) . ?
C50 H50C 1.006(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 110.5(8) . . ?
C2 C1 C16 108.35(8) . . ?
C9 C1 H1 111.1(8) . . ?
C9 C1 C2 108.45(8) . . ?
C9 C1 C16 108.35(8) . . ?
C16 C1 H1 110.0(8) . . ?
C3 C2 C1 103.45(8) . . ?
C3 C2 C23 110.94(9) . . ?
C22 C2 C1 103.81(8) . . ?
C22 C2 C3 112.23(9) . . ?
C22 C2 C23 112.88(9) . . ?
C23 C2 C1 112.98(9) . . ?
C4 C3 C2 127.40(10) . . ?
C8 C3 C2 112.22(9) . . ?
C8 C3 C4 120.38(10) . . ?
C3 C4 H4 119.8(9) . . ?
C5 C4 C3 119.01(11) . . ?
C5 C4 H4 121.2(9) . . ?
C4 C5 H5 119.7(9) . . ?
C6 C5 C4 120.67(10) . . ?
C6 C5 H5 119.6(9) . . ?
C5 C6 H6 119.4(9) . . ?
C5 C6 C7 120.29(10) . . ?
C7 C6 H6 120.3(9) . . ?
C6 C7 H7 119.8(8) . . ?
C6 C7 C8 119.09(11) . . ?
C8 C7 H7 121.1(8) . . ?
C3 C8 C7 120.54(10) . . ?
C3 C8 C9 112.05(9) . . ?
C7 C8 C9 127.41(10) . . ?
C8 C9 C1 103.76(8) . . ?
C8 C9 C24 111.51(9) . . ?
C10 C9 C1 103.74(8) . . ?
C10 C9 C8 112.42(9) . . ?
C10 C9 C24 111.35(9) . . ?
C24 C9 C1 113.63(9) . . ?
C11 C10 C9 127.54(10) . . ?
C11 C10 C15 120.40(10) . . ?
C15 C10 C9 112.05(9) . . ?
C10 C11 H11 120.4(9) . . ?
C10 C11 C12 119.43(11) . . ?
C12 C11 H11 120.1(9) . . ?
C11 C12 H12 119.4(9) . . ?
C13 C12 C11 120.06(11) . . ?
C13 C12 H12 120.5(9) . . ?
C12 C13 H13 119.2(10) . . ?
C14 C13 C12 120.68(11) . . ?
C14 C13 H13 120.1(10) . . ?
C13 C14 H14 121.4(9) . . ?
C13 C14 C15 119.24(11) . . ?
C15 C14 H14 119.4(9) . . ?
C10 C15 C14 120.17(10) . . ?
C10 C15 C16 112.10(9) . . ?
C14 C15 C16 127.72(10) . . ?
C15 C16 C1 103.71(8) . . ?
C15 C16 C17 112.72(9) . . ?
C15 C16 C25 111.52(9) . . ?
C17 C16 C1 103.65(8) . . ?
C17 C16 C25 111.35(9) . . ?
C25 C16 C1 113.44(9) . . ?
C18 C17 C16 127.38(10) . . ?
C22 C17 C16 112.26(9) . . ?
C22 C17 C18 120.35(10) . . ?
C17 C18 H18 121.1(9) . . ?
C19 C18 C17 119.25(11) . . ?
C19 C18 H18 119.6(9) . . ?
C18 C19 H19 119.4(9) . . ?
C20 C19 C18 120.45(11) . . ?
C20 C19 H19 120.2(9) . . ?
C19 C20 H20 119.3(9) . . ?
C21 C20 C19 120.28(11) . . ?
C21 C20 H20 120.4(9) . . ?
C20 C21 H21 119.8(9) . . ?
C20 C21 C22 119.42(11) . . ?
C22 C21 H21 120.8(9) . . ?
C17 C22 C2 111.83(9) . . ?
C17 C22 C21 120.23(10) . . ?
C21 C22 C2 127.92(10) . . ?
C2 C23 H23A 110.9(9) . . ?
C2 C23 H23B 110.9(9) . . ?
C2 C23 H23C 110.7(9) . . ?
H23A C23 H23B 107.6(12) . . ?
H23A C23 H23C 108.8(12) . . ?
H23B C23 H23C 107.9(12) . . ?
C9 C24 H24A 109.7(9) . . ?
C9 C24 H24B 110.0(9) . . ?
C9 C24 H24C 111.0(8) . . ?
H24A C24 H24B 108.2(12) . . ?
H24A C24 H24C 109.3(11) . . ?
H24B C24 H24C 108.7(12) . . ?
C16 C25 H25A 110.1(9) . . ?
C16 C25 H25B 111.2(9) . . ?
C16 C25 H25C 110.9(9) . . ?
H25A C25 H25B 107.9(12) . . ?
H25A C25 H25C 107.4(13) . . ?
H25B C25 H25C 109.2(13) . . ?
C27 C26 H26 110.4(7) . . ?
C34 C26 H26 110.5(7) . . ?
C34 C26 C27 108.21(8) . . ?
C41 C26 H26 111.1(7) . . ?
C41 C26 C27 108.35(8) . . ?
C41 C26 C34 108.23(8) . . ?
C28 C27 C26 103.71(8) . . ?
C28 C27 C47 111.21(9) . . ?
C28 C27 C48 111.77(9) . . ?
C47 C27 C26 103.56(8) . . ?
C47 C27 C48 112.31(9) . . ?
C48 C27 C26 113.71(9) . . ?
C29 C28 C27 127.40(10) . . ?
C29 C28 C33 120.40(10) . . ?
C33 C28 C27 112.18(9) . . ?
C28 C29 H29 119.5(9) . . ?
C30 C29 C28 119.54(10) . . ?
C30 C29 H29 120.9(9) . . ?
C29 C30 H30 118.9(9) . . ?
C29 C30 C31 120.07(11) . . ?
C31 C30 H30 121.0(9) . . ?
C30 C31 H31 119.5(9) . . ?
C32 C31 C30 120.42(11) . . ?
C32 C31 H31 120.1(9) . . ?
C31 C32 H32 120.6(8) . . ?
C31 C32 C33 119.46(10) . . ?
C33 C32 H32 119.9(8) . . ?
C28 C33 C32 120.09(10) . . ?
C28 C33 C34 112.18(9) . . ?
C32 C33 C34 127.73(10) . . ?
C33 C34 C26 103.53(8) . . ?
C33 C34 C49 111.10(9) . . ?
C35 C34 C26 103.62(8) . . ?
C35 C34 C33 112.06(8) . . ?
C35 C34 C49 112.42(9) . . ?
C49 C34 C26 113.60(9) . . ?
C36 C35 C34 127.46(10) . . ?
C40 C35 C34 112.27(9) . . ?
C40 C35 C36 120.26(10) . . ?
C35 C36 H36 120.2(8) . . ?
C37 C36 C35 118.85(11) . . ?
C37 C36 H36 120.9(8) . . ?
C36 C37 H37 118.5(9) . . ?
C38 C37 C36 120.67(10) . . ?
C38 C37 H37 120.8(9) . . ?
C37 C38 H38 120.3(8) . . ?
C37 C38 C39 120.51(11) . . ?
C39 C38 H38 119.2(8) . . ?
C38 C39 H39 119.4(8) . . ?
C40 C39 C38 118.87(11) . . ?
C40 C39 H39 121.7(8) . . ?
C35 C40 C39 120.80(10) . . ?
C35 C40 C41 111.90(9) . . ?
C39 C40 C41 127.30(10) . . ?
C40 C41 C26 103.77(8) . . ?
C40 C41 C50 110.98(9) . . ?
C42 C41 C26 103.76(8) . . ?
C42 C41 C40 113.37(8) . . ?
C42 C41 C50 110.90(9) . . ?
C50 C41 C26 113.73(9) . . ?
C43 C42 C41 127.24(10) . . ?
C47 C42 C41 112.13(9) . . ?
C47 C42 C43 120.63(10) . . ?
C42 C43 H43 121.4(8) . . ?
C44 C43 C42 119.04(11) . . ?
C44 C43 H43 119.5(8) . . ?
C43 C44 H44 119.9(9) . . ?
C43 C44 C45 120.56(11) . . ?
C45 C44 H44 119.6(9) . . ?
C44 C45 H45 120.3(9) . . ?
C46 C45 C44 120.26(11) . . ?
C46 C45 H45 119.5(9) . . ?
C45 C46 H46 120.4(9) . . ?
C45 C46 C47 119.34(11) . . ?
C47 C46 H46 120.2(9) . . ?
C42 C47 C27 112.17(9) . . ?
C42 C47 C46 120.17(10) . . ?
C46 C47 C27 127.65(10) . . ?
C27 C48 H48A 111.0(9) . . ?
C27 C48 H48B 109.8(8) . . ?
C27 C48 H48C 110.6(9) . . ?
H48A C48 H48B 108.7(12) . . ?
H48A C48 H48C 108.5(12) . . ?
H48B C48 H48C 108.1(12) . . ?
C34 C49 H49A 111.2(9) . . ?
C34 C49 H49B 110.5(9) . . ?
C34 C49 H49C 111.4(9) . . ?
H49A C49 H49B 108.2(13) . . ?
H49A C49 H49C 105.3(12) . . ?
H49B C49 H49C 110.2(13) . . ?
C41 C50 H50A 110.8(9) . . ?
C41 C50 H50B 109.4(9) . . ?
C41 C50 H50C 110.3(9) . . ?
H50A C50 H50B 109.2(12) . . ?
H50A C50 H50C 107.9(12) . . ?
H50B C50 H50C 109.1(12) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 1 0.0150 0.0000 -1.0001 0.9997 -0.1402 -0.0121 0.0148
0 1 -1 0.0150 -0.0000 1.0001 -0.9997 0.1402 0.0121 -0.0148
0 3 5 0.0755 -0.0015 2.9981 5.0012 -0.0541 0.5980 -0.2685
0 -3 -5 0.0755 0.0015 -2.9981 -5.0012 0.0541 -0.5980 0.2685
4 1 5 0.0661 3.9999 0.9974 5.0006 -0.1471 0.8274 0.4083
-4 -1 -5 0.0661 -3.9999 -0.9974 -5.0006 0.1471 -0.8274 -0.4083

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound17
_database_code_depnum_ccdc_archive 'CCDC 1514278'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-11-24
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C55 H52 Si3'
_chemical_formula_sum            'C55 H52 Si3'
_chemical_formula_weight         797.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C55 H52 Si3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_H-M_alt        'I a -3'
_space_group_name_Hall           '-I 2b 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y, -z+1/2, x'
'z, -x, -y+1/2'
'-y+1/2, z, -x'
'-z, -x+1/2, y'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1, z+1/2, -x+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y, z-1/2, -x'
'-z, x, y-1/2'
'y-1/2, -z, x'
'z, x-1/2, -y'
'z-1/2, -x, y'
'-y, z, x-1/2'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x+1/2, y'
'y, -z+1/2, x+1/2'
'z+1/2, x, -y+1/2'
'z, -x+1/2, y+1/2'
'-y+1/2, z+1/2, x'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'

_cell_length_a                   27.0972(2)
_cell_length_b                   27.0972(2)
_cell_length_c                   27.0972(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19896.3(5)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    24928
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.7470
_cell_measurement_theta_min      3.2500
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.2015
_exptl_crystal_size_mid          0.1664
_exptl_crystal_size_min          0.1295
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            82503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.36
_diffrn_reflns_theta_min         2.31
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00   14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   60.0000 61

#__ type_ start__ end____ width___ exp.time_
  2 omega  -47.00   29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega -106.00  -10.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000 -150.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega    2.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000  120.0000 70

#__ type_ start__ end____ width___ exp.time_
  6 omega   65.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega   38.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -125.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
  8 omega   13.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
  9 omega   14.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
 10 omega   62.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  -30.0000 49

#__ type_ start__ end____ width___ exp.time_
 11 omega   14.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 31

#__ type_ start__ end____ width___ exp.time_
 12 omega   18.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  -30.0000 41

#__ type_ start__ end____ width___ exp.time_
 13 omega   13.00   80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 67

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000   60.0000 39

#__ type_ start__ end____ width___ exp.time_
 15 omega   20.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000   90.0000 92

#__ type_ start__ end____ width___ exp.time_
 16 omega   16.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   41.00   98.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 57

#__ type_ start__ end____ width___ exp.time_
 18 omega   85.00  162.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 77

#__ type_ start__ end____ width___ exp.time_
 19 omega   83.00  162.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000  172.8209 79

#__ type_ start__ end____ width___ exp.time_
 20 omega   85.00  176.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 91

#__ type_ start__ end____ width___ exp.time_
 21 omega   85.00  112.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   31.00   83.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 52

#__ type_ start__ end____ width___ exp.time_
 23 omega  137.00  176.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   49.0000   10.2334 39

#__ type_ start__ end____ width___ exp.time_
 24 omega   44.00  109.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 65

#__ type_ start__ end____ width___ exp.time_
 25 omega   85.00  110.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   66.0000   -1.0687 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   81.00   99.00   1.0000   33.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0281191000
_diffrn_orient_matrix_UB_12      0.0483751000
_diffrn_orient_matrix_UB_13      -0.0102055000
_diffrn_orient_matrix_UB_21      0.0207253000
_diffrn_orient_matrix_UB_22      -0.0221599000
_diffrn_orient_matrix_UB_23      -0.0481012000
_diffrn_orient_matrix_UB_31      -0.0449094000
_diffrn_orient_matrix_UB_32      0.0200350000
_diffrn_orient_matrix_UB_33      -0.0284457000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2483
_reflns_number_total             3279
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0866
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1681P)²+14.8482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2836
_refine_ls_wR_factor_ref         0.2981
_refine_special_details          
;Disorder of C(17), C(18) and C(19) on three positions  (53:32:15)

 The crystal contains a highly disordered solvent molecule, which could not be 
 refined reliabally, so the squeeze algorithm of Olex2 was applied. 
 (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
 J. Appl. Cryst. (2009), 42, 339-341.)
 The sum formular and further calculations disregard this electron density.
 
mask.log:

Miller array info: D:/Data/toma19/struct/olex2_toma19/toma19.hkl:Iobs,SigIobs
Observation type: xray.intensity
Type of data: double, size=82503
Type of sigmas: double, size=82503
Number of Miller indices: 82503
Anomalous flag: False
Unit cell: (27.0972, 27.0972, 27.0972, 90, 90, 90)
Space group: I a -3 (No. 206)
Systematic absences: 3015
Systematic absences not included in following:
Centric reflections: 79488
Resolution range: 13.5486 0.808961

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
    C     H    Si
 1.70  1.09  2.10

Total solvent accessible volume / cell = 2101.7 Ang^3 [10.6%]
Total electron count / cell = 482.5

gridding: (144,144,144)
Void #Grid points Vol/A^3 Vol/%  Centre of mass (frac)   Eigenvectors (frac)
   1        10697    71.3   0.4  ( 0.000,-0.000,-0.000)  1  ( 0.577, 0.577, 0.577)
                                                         2  ( 0.707,-0.707, 0.000)
                                                         3  (-0.408,-0.408, 0.816)
   2        10697    71.3   0.4  ( 0.000, 0.000, 0.500)  1  ( 0.577,-0.577,-0.577)
                                                         2  ( 0.707, 0.707, 0.000)
                                                         3  ( 0.408,-0.408, 0.816)
   3        10697    71.3   0.4  ( 0.000, 0.500, 0.500)  1  ( 0.577,-0.577, 0.577)
                                                         2  (-0.408, 0.408, 0.816)
                                                         3  ( 0.707, 0.707, 0.000)
   4        10697    71.3   0.4  ( 0.000, 0.500, 1.000)  1  ( 0.577, 0.577,-0.577)
                                                         2  ( 0.408, 0.408, 0.816)
                                                         3  ( 0.707,-0.707, 0.000)
   5        28731   191.4   1.0  ( 0.250, 0.250, 0.250)  1  (-0.707, 0.707, 0.000)
                                                         2  (-0.408,-0.408, 0.816)
                                                         3  ( 0.577, 0.577, 0.577)
   6        28731   191.4   1.0  ( 0.250, 0.250, 0.750)  1  ( 0.707, 0.707, 0.000)
                                                         2  (-0.408, 0.408, 0.816)
                                                         3  ( 0.577,-0.577, 0.577)
   7        28731   191.4   1.0  ( 0.250, 0.750, 0.750)  1  ( 0.408, 0.408, 0.816)
                                                         2  ( 0.707,-0.707, 0.000)
                                                         3  ( 0.577, 0.577,-0.577)
   8        28731   191.4   1.0  ( 0.250, 0.750, 0.250)  1  ( 0.408,-0.408, 0.816)
                                                         2  ( 0.707, 0.707, 0.000)
                                                         3  (-0.577, 0.577, 0.577)
   9        10697    71.3   0.4  ( 0.500,-0.000, 0.500)  1  ( 0.577, 0.577,-0.577)
                                                         2  (-0.707, 0.707, 0.000)
                                                         3  ( 0.408, 0.408, 0.816)
  10        10697    71.3   0.4  ( 0.500, 0.500,-0.000)  1  ( 0.577,-0.577,-0.577)
                                                         2  ( 0.707, 0.707, 0.000)
                                                         3  ( 0.408,-0.408, 0.816)
  11        10697    71.3   0.4  ( 0.500, 0.500, 0.500)  1  ( 0.577, 0.577, 0.577)
                                                         2  ( 0.707,-0.707,-0.000)
                                                         3  (-0.408,-0.408, 0.816)
  12        10697    71.3   0.4  ( 0.500, 0.000, 1.000)  1  (-0.577, 0.577,-0.577)
                                                         2  ( 0.707, 0.707, 0.000)
                                                         3  (-0.408, 0.408, 0.816)
  13        28731   191.4   1.0  ( 0.750, 0.250, 0.250)  1  (-0.707, 0.707, 0.000)
                                                         2  ( 0.408, 0.408, 0.816)
                                                         3  ( 0.577, 0.577,-0.577)
  14        28731   191.4   1.0  ( 0.750, 0.250, 0.750)  1  ( 0.707, 0.707, 0.000)
                                                         2  ( 0.408,-0.408, 0.816)
                                                         3  ( 0.577,-0.577,-0.577)
  15        28731   191.4   1.0  ( 0.750, 0.750, 0.750)  1  (-0.707, 0.707, 0.000)
                                                         2  (-0.408,-0.408, 0.816)
                                                         3  ( 0.577, 0.577, 0.577)
  16        28731   191.4   1.0  ( 0.750, 0.750, 0.250)  1  ( 0.707, 0.707, 0.000)
                                                         2  (-0.408, 0.408, 0.816)
                                                         3  (-0.577, 0.577,-0.577)

Void  Vol/Ang^3  #Electrons
   1       71.3          0.0
   2       71.3          0.0
   3       71.3          0.0
   4       71.3          0.0
   5      191.4         60.3
   6      191.4         60.3
   7      191.4         60.3
   8      191.4         60.3
   9       71.3          0.0
  10       71.3          0.0
  11       71.3          0.0
  12       71.3          0.0
  13      191.4         60.3
  14      191.4         60.3
  15      191.4         60.3
  16      191.4         60.3, SQUEEZE
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.36705(4) 0.40346(5) -0.20589(4) 0.0998(5) Uani 1 1 d D . . . .
C1 C 0.41631(11) 0.58369(11) 0.08369(11) 0.0694(12) Uani 1 3 d S T P . .
H1 H 0.4372 0.5628 0.0628 0.083 Uiso 1 3 calc R U P . .
C2 C 0.36302(11) 0.58801(12) 0.06134(12) 0.0745(8) Uani 1 1 d . . . . .
C3 C 0.33020(13) 0.56871(14) 0.10265(13) 0.0839(10) Uani 1 1 d . . . . .
C4 C 0.27865(14) 0.56602(17) 0.10199(17) 0.1012(12) Uani 1 1 d . . . . .
H4 H 0.2607 0.5759 0.0745 0.121 Uiso 1 1 calc R U . . .
C5 C 0.25481(19) 0.5478(2) 0.1445(2) 0.1232(17) Uani 1 1 d . . . . .
H5 H 0.2206 0.5445 0.1449 0.148 Uiso 1 1 calc R U . . .
C6 C 0.2815(2) 0.5349(2) 0.1851(2) 0.1220(16) Uani 1 1 d . . . . .
H6 H 0.2652 0.5241 0.2133 0.146 Uiso 1 1 calc R U . . .
C7 C 0.33150(18) 0.53747(16) 0.18500(17) 0.1059(13) Uani 1 1 d . . . . .
H7 H 0.3492 0.5278 0.2128 0.127 Uiso 1 1 calc R U . . .
C8 C 0.35640(14) 0.55450(13) 0.14347(13) 0.0830(9) Uani 1 1 d . . . . .
C9 C 0.35848(11) 0.55852(13) 0.01376(12) 0.0741(8) Uani 1 1 d . . . . .
C10 C 0.36826(14) 0.57896(14) -0.03164(13) 0.0880(10) Uani 1 1 d . . . . .
H10 H 0.3746 0.6126 -0.0338 0.106 Uiso 1 1 calc R U . . .
C11 C 0.36894(14) 0.55081(15) -0.07427(14) 0.0885(10) Uani 1 1 d . . . . .
H11 H 0.3758 0.5659 -0.1043 0.106 Uiso 1 1 calc R U . . .
C12 C 0.35969(11) 0.50103(13) -0.07289(12) 0.0730(8) Uani 1 1 d . . . . .
C13 C 0.34893(14) 0.47936(14) -0.02724(12) 0.0828(9) Uani 1 1 d . . . . .
H13 H 0.3422 0.4458 -0.0253 0.099 Uiso 1 1 calc R U . . .
C14 C 0.34841(14) 0.50823(14) 0.01503(13) 0.0835(9) Uani 1 1 d . . . . .
H14 H 0.3411 0.4935 0.0451 0.100 Uiso 1 1 calc R U . . .
C15 C 0.36132(11) 0.47042(13) -0.11728(14) 0.0766(9) Uani 1 1 d . . . . .
C16 C 0.36424(13) 0.44534(16) -0.15184(14) 0.0880(10) Uani 1 1 d . . . . .
C17A C 0.4318(3) 0.4061(4) -0.2303(4) 0.1256(17) Uani 0.525(3) 1 d D . P A 1
H17A H 0.4543 0.3951 -0.2052 0.188 Uiso 0.525(3) 1 calc R U P A 1
H17B H 0.4346 0.3852 -0.2587 0.188 Uiso 0.525(3) 1 calc R U P A 1
H17C H 0.4397 0.4395 -0.2393 0.188 Uiso 0.525(3) 1 calc R U P A 1
C17B C 0.4106(7) 0.4259(7) -0.2504(5) 0.1256(17) Uani 0.323(3) 1 d D . P A 2
H17D H 0.4116 0.4038 -0.2781 0.188 Uiso 0.323(3) 1 calc R U P A 2
H17E H 0.4008 0.4581 -0.2613 0.188 Uiso 0.323(3) 1 calc R U P A 2
H17F H 0.4428 0.4277 -0.2356 0.188 Uiso 0.323(3) 1 calc R U P A 2
C17C C 0.3692(15) 0.4390(11) -0.2652(7) 0.1256(17) Uani 0.152(3) 1 d D . P A 3
H17G H 0.3500 0.4686 -0.2619 0.188 Uiso 0.152(3) 1 calc R U P A 3
H17H H 0.4028 0.4475 -0.2727 0.188 Uiso 0.152(3) 1 calc R U P A 3
H17I H 0.3560 0.4192 -0.2914 0.188 Uiso 0.152(3) 1 calc R U P A 3
C18A C 0.3230(4) 0.4239(4) -0.2516(3) 0.1256(17) Uani 0.525(3) 1 d D . P A 1
H18A H 0.3314 0.4567 -0.2623 0.188 Uiso 0.525(3) 1 calc R U P A 1
H18B H 0.3237 0.4020 -0.2794 0.188 Uiso 0.525(3) 1 calc R U P A 1
H18C H 0.2905 0.4241 -0.2375 0.188 Uiso 0.525(3) 1 calc R U P A 1
C18B C 0.3014(5) 0.4008(8) -0.2284(8) 0.1256(17) Uani 0.323(3) 1 d D . P A 2
H18D H 0.2805 0.3884 -0.2025 0.188 Uiso 0.323(3) 1 calc R U P A 2
H18E H 0.2907 0.4332 -0.2377 0.188 Uiso 0.323(3) 1 calc R U P A 2
H18F H 0.2994 0.3792 -0.2564 0.188 Uiso 0.323(3) 1 calc R U P A 2
C18C C 0.3063(8) 0.3803(15) -0.2284(15) 0.1256(17) Uani 0.152(3) 1 d D . P A 3
H18G H 0.2840 0.4075 -0.2322 0.188 Uiso 0.152(3) 1 calc R U P A 3
H18H H 0.3107 0.3642 -0.2597 0.188 Uiso 0.152(3) 1 calc R U P A 3
H18I H 0.2931 0.3573 -0.2050 0.188 Uiso 0.152(3) 1 calc R U P A 3
C19A C 0.3565(4) 0.3410(4) -0.1813(4) 0.1256(17) Uani 0.525(3) 1 d D . P A 1
H19A H 0.3815 0.3333 -0.1574 0.188 Uiso 0.525(3) 1 calc R U P A 1
H19B H 0.3246 0.3396 -0.1659 0.188 Uiso 0.525(3) 1 calc R U P A 1
H19C H 0.3578 0.3175 -0.2078 0.188 Uiso 0.525(3) 1 calc R U P A 1
C19B C 0.3827(7) 0.3397(5) -0.1866(6) 0.1256(17) Uani 0.323(3) 1 d D . P A 2
H19D H 0.3590 0.3283 -0.1629 0.188 Uiso 0.323(3) 1 calc R U P A 2
H19E H 0.3822 0.3183 -0.2149 0.188 Uiso 0.323(3) 1 calc R U P A 2
H19F H 0.4151 0.3393 -0.1722 0.188 Uiso 0.323(3) 1 calc R U P A 2
C19C C 0.4009(13) 0.3451(9) -0.2024(13) 0.1256(17) Uani 0.152(3) 1 d D . P A 3
H19G H 0.3985 0.3282 -0.2334 0.188 Uiso 0.152(3) 1 calc R U P A 3
H19H H 0.4349 0.3517 -0.1950 0.188 Uiso 0.152(3) 1 calc R U P A 3
H19I H 0.3870 0.3249 -0.1768 0.188 Uiso 0.152(3) 1 calc R U P A 3


_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 C16 1.854(4) . ?
Si1 C17A 1.877(9) . ?
Si1 C17B 1.794(12) . ?
Si1 C17C 1.875(15) . ?
Si1 C18A 1.808(9) . ?
Si1 C18B 1.883(12) . ?
Si1 C18C 1.863(15) . ?
Si1 C19A 1.842(10) . ?
Si1 C19B 1.855(13) . ?
Si1 C19C 1.829(15) . ?
C1 H1 0.9800 . ?
C1 C2 1.570(4) . ?
C1 C2 1.570(4) 19_554 ?
C1 C2 1.570(4) 18 ?
C2 C3 1.522(5) . ?
C2 C8 1.528(5) 19_554 ?
C2 C9 1.522(5) . ?
C3 C4 1.399(5) . ?
C3 C8 1.370(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.411(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.362(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.356(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.391(5) . ?
C8 C2 1.528(5) 18 ?
C9 C10 1.375(5) . ?
C9 C14 1.390(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.384(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.373(5) . ?
C12 C13 1.400(5) . ?
C12 C15 1.462(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.387(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.160(5) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17C H17G 0.9600 . ?
C17C H17H 0.9600 . ?
C17C H17I 0.9600 . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18C H18G 0.9600 . ?
C18C H18H 0.9600 . ?
C18C H18I 0.9600 . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
C19C H19G 0.9600 . ?
C19C H19H 0.9600 . ?
C19C H19I 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 Si1 C17A 107.0(3) . . ?
C16 Si1 C17C 111.3(10) . . ?
C16 Si1 C18B 103.9(5) . . ?
C16 Si1 C18C 115.4(11) . . ?
C16 Si1 C19B 111.0(6) . . ?
C17B Si1 C16 110.5(5) . . ?
C17B Si1 C18B 114.7(10) . . ?
C17B Si1 C19B 110.7(9) . . ?
C18A Si1 C16 109.1(3) . . ?
C18A Si1 C17A 111.4(5) . . ?
C18A Si1 C19A 115.3(5) . . ?
C18C Si1 C17C 85.4(19) . . ?
C19A Si1 C16 105.7(3) . . ?
C19A Si1 C17A 108.0(5) . . ?
C19B Si1 C18B 105.7(9) . . ?
C19C Si1 C16 120.5(11) . . ?
C19C Si1 C17C 118.2(16) . . ?
C19C Si1 C18C 99.7(17) . . ?
C2 C1 H1 110.6 19_554 . ?
C2 C1 H1 110.6 18 . ?
C2 C1 H1 110.6 . . ?
C2 C1 C2 108.3(2) 19_554 18 ?
C2 C1 C2 108.3(2) 19_554 . ?
C2 C1 C2 108.3(2) 18 . ?
C3 C2 C1 103.2(3) . . ?
C3 C2 C8 111.1(3) . 19_554 ?
C8 C2 C1 103.1(3) 19_554 . ?
C9 C2 C1 111.2(3) . . ?
C9 C2 C3 113.3(3) . . ?
C9 C2 C8 113.9(3) . 19_554 ?
C4 C3 C2 126.3(4) . . ?
C8 C3 C2 112.8(3) . . ?
C8 C3 C4 120.9(3) . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.7(5) . . ?
C5 C4 H4 121.1 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.0(5) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.3(5) . . ?
C8 C7 H7 119.9 . . ?
C3 C8 C2 112.6(3) . 18 ?
C3 C8 C7 119.7(4) . . ?
C7 C8 C2 127.7(4) . 18 ?
C10 C9 C2 122.1(3) . . ?
C10 C9 C14 117.1(3) . . ?
C14 C9 C2 120.6(3) . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.8(3) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 C15 122.0(3) . . ?
C13 C12 C15 119.7(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.7(3) . . ?
C14 C13 H13 120.2 . . ?
C9 C14 H14 119.0 . . ?
C13 C14 C9 122.0(3) . . ?
C13 C14 H14 119.0 . . ?
C16 C15 C12 177.4(4) . . ?
C15 C16 Si1 177.6(4) . . ?
Si1 C17A H17A 109.5 . . ?
Si1 C17A H17B 109.5 . . ?
Si1 C17A H17C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
Si1 C17B H17D 109.5 . . ?
Si1 C17B H17E 109.5 . . ?
Si1 C17B H17F 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
Si1 C17C H17G 109.5 . . ?
Si1 C17C H17H 109.5 . . ?
Si1 C17C H17I 109.5 . . ?
H17G C17C H17H 109.5 . . ?
H17G C17C H17I 109.5 . . ?
H17H C17C H17I 109.5 . . ?
Si1 C18A H18A 109.5 . . ?
Si1 C18A H18B 109.5 . . ?
Si1 C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
Si1 C18B H18D 109.5 . . ?
Si1 C18B H18E 109.5 . . ?
Si1 C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
Si1 C18C H18G 109.5 . . ?
Si1 C18C H18H 109.5 . . ?
Si1 C18C H18I 109.5 . . ?
H18G C18C H18H 109.5 . . ?
H18G C18C H18I 109.5 . . ?
H18H C18C H18I 109.5 . . ?
Si1 C19A H19A 109.5 . . ?
Si1 C19A H19B 109.5 . . ?
Si1 C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
Si1 C19B H19D 109.5 . . ?
Si1 C19B H19E 109.5 . . ?
Si1 C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
Si1 C19C H19G 109.5 . . ?
Si1 C19C H19H 109.5 . . ?
Si1 C19C H19I 109.5 . . ?
H19G C19C H19H 109.5 . . ?
H19G C19C H19I 109.5 . . ?
H19H C19C H19I 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 71.3 0.0 ?
2 0.000 0.000 0.500 71.3 0.0 ?
3 0.000 0.500 0.500 71.3 0.0 ?
4 0.000 0.500 1.000 71.3 0.0 ?
5 0.250 0.250 0.250 191.4 60.3 ?
6 0.250 0.250 0.750 191.4 60.3 ?
7 0.250 0.750 0.750 191.4 60.3 ?
8 0.250 0.750 0.250 191.4 60.3 ?
9 0.500 0.000 0.500 71.3 0.0 ?
10 0.500 0.500 0.000 71.3 0.0 ?
11 0.500 0.500 0.500 71.3 0.0 ?
12 0.500 0.000 1.000 71.3 0.0 ?
13 0.750 0.250 0.250 191.4 60.3 ?
14 0.750 0.250 0.750 191.4 60.3 ?
15 0.750 0.750 0.750 191.4 60.3 ?
16 0.750 0.750 0.250 191.4 60.3 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 -5 0.0514 -0.0043 -0.9994 -5.0022 0.0026 0.2627 0.1225
5 -3 0 0.0756 4.9838 -3.0225 0.0006 -0.0061 0.1702 -0.2844
2 0 5 0.0829 1.9986 -0.0096 5.0026 0.0047 -0.1990 -0.2323
-5 0 -2 0.0829 -4.9964 0.0236 -2.0042 -0.1189 -0.0077 0.2819
0 5 -2 0.0682 0.0208 4.9983 -1.9952 0.2627 -0.0144 0.1560
1 1 0 0.0695 1.0034 0.9949 0.0018 0.0763 -0.0013 -0.0252
5 -5 4 0.0726 4.9756 -5.0219 3.9994 -0.1438 0.0220 -0.4378
0 -5 2 0.0763 -0.0208 -4.9983 1.9952 -0.2627 0.0144 -0.1560
-2 2 5 0.0608 -1.9901 2.0085 5.0017 -0.0098 -0.3263 -0.0127
-5 3 2 0.0777 -4.9838 3.0224 1.9998 -0.0143 -0.2665 0.2275

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound10
_database_code_depnum_ccdc_archive 'CCDC 1514273'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2015-02-11
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H31 Cl3 Si3'
_chemical_formula_sum            'C28 H31 Cl3 Si3'
_chemical_formula_weight         558.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H31 Cl3 Si3'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   10.1259(3)
_cell_length_b                   10.1259(3)
_cell_length_c                   15.3317(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1361.41(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    42178
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      38.4920
_cell_measurement_theta_min      2.6450
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3349
_exptl_crystal_size_mid          0.2532
_exptl_crystal_size_min          0.1438
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86809
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.483
_diffrn_reflns_theta_min         2.657
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9883
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   68.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 87

#__ type_ start__ end____ width___ exp.time_
  2 omega    6.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   87.0000  156.5345 28

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -99.0000 -180.0000 101

#__ type_ start__ end____ width___ exp.time_
  4 omega    5.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   89.0000 -129.5473 28

#__ type_ start__ end____ width___ exp.time_
  5 omega    8.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   83.0000   -8.5917 32

#__ type_ start__ end____ width___ exp.time_
  6 omega  -30.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -38.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
  7 omega    6.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   87.0000   36.6002 28

#__ type_ start__ end____ width___ exp.time_
  8 omega   22.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   57.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
  9 omega  -32.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -19.0000 -120.0000 110

#__ type_ start__ end____ width___ exp.time_
 10 omega  -20.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -99.0000  -60.0000 101

#__ type_ start__ end____ width___ exp.time_
 11 omega  -28.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -57.0000   60.0000 87

#__ type_ start__ end____ width___ exp.time_
 12 omega  -20.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -99.0000   30.0000 101

#__ type_ start__ end____ width___ exp.time_
 13 omega   17.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   67.0000   47.3890 91

#__ type_ start__ end____ width___ exp.time_
 14 omega   22.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   57.0000 -150.0000 87

#__ type_ start__ end____ width___ exp.time_
 15 omega   12.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   77.0000  120.0000 97

#__ type_ start__ end____ width___ exp.time_
 16 omega   15.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   71.0000  -78.7486 93

#__ type_ start__ end____ width___ exp.time_
 17 omega  -20.00   40.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 18 omega   22.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   57.0000  -90.0000 87

#__ type_ start__ end____ width___ exp.time_
 19 omega  -29.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -77.0000   60.0000 96

#__ type_ start__ end____ width___ exp.time_
 20 omega  -30.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485  -38.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
 21 omega   15.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   70.0000 -169.4027 93

#__ type_ start__ end____ width___ exp.time_
 22 omega   22.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   57.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
 23 omega    7.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   86.0000   78.4468 28

#__ type_ start__ end____ width___ exp.time_
 24 omega    6.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2485   87.0000  -93.1556 28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0077494000
_diffrn_orient_matrix_UB_12      -0.0594034000
_diffrn_orient_matrix_UB_13      0.0194198000
_diffrn_orient_matrix_UB_21      0.0607405000
_diffrn_orient_matrix_UB_22      0.0543539000
_diffrn_orient_matrix_UB_23      0.0261555000
_diffrn_orient_matrix_UB_31      -0.0529056000
_diffrn_orient_matrix_UB_32      -0.0081754000
_diffrn_orient_matrix_UB_33      0.0328556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4491
_reflns_number_total             4796
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Disorder of Me2ClSi group over three positions with a 74:17:9 distribution.

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0263P)²+0.5502P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0838
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cl1 Cl 0.78047(11) 0.60436(12) 0.43742(7) 0.02007(10) Uani 0.7372(12) 1 d . . P
A 1
Cl1B Cl 0.7517(9) 0.8255(8) 0.2842(5) 0.0230(9) Uani 0.1756(12) 1 d . . P A 2
Cl1C Cl 0.4542(17) 0.536(2) 0.3692(11) 0.0154(13) Uani 0.0872(12) 1 d . . P A 3
C11 C 0.774(2) 0.614(2) 0.4301(10) 0.041(5) Uani 0.2628(12) 1 d . . P A 2
H11A H 0.7311 0.5117 0.4525 0.062 Uiso 0.2628(12) 1 calc R U P A 2
H11B H 0.7672 0.6779 0.4737 0.062 Uiso 0.2628(12) 1 calc R U P A 2
H11C H 0.8789 0.6518 0.4151 0.062 Uiso 0.2628(12) 1 calc R U P A 2
C10 C 0.7576(7) 0.8185(7) 0.2981(4) 0.0204(7) Uani 0.8244(12) 1 d . . P A 1
H10A H 0.7042 0.8303 0.2497 0.031 Uiso 0.8244(12) 1 calc R U P A 1
H10B H 0.8617 0.8544 0.2820 0.031 Uiso 0.8244(12) 1 calc R U P A 1
H10C H 0.7547 0.8766 0.3468 0.031 Uiso 0.8244(12) 1 calc R U P A 1
C9 C 0.4641(7) 0.5470(8) 0.3607(5) 0.0187(8) Uani 0.9128(12) 1 d . . P A 1
H9A H 0.4121 0.5622 0.3128 0.028 Uiso 0.9128(12) 1 calc R U P A 1
H9B H 0.4630 0.6045 0.4102 0.028 Uiso 0.9128(12) 1 calc R U P A 1
H9C H 0.4137 0.4406 0.3755 0.028 Uiso 0.9128(12) 1 calc R U P A 1
Si1 Si 0.66426(3) 0.61190(3) 0.32922(2) 0.01191(5) Uani 1 1 d . . . . .
C1 C 0.6667 0.3333 0.27828(8) 0.00917(17) Uani 1 3 d S T P . .
H1 H 0.6667 0.3333 0.3422 0.011 Uiso 1 3 calc R U P . .
C2 C 0.67316(8) 0.48207(8) 0.24096(4) 0.01000(10) Uani 1 1 d . . . . .
C3 C 0.81687(8) 0.55498(8) 0.18543(5) 0.01093(11) Uani 1 1 d . . . . .
C4 C 0.87332(9) 0.68630(9) 0.13416(5) 0.01448(12) Uani 1 1 d . . . . .
H4 H 0.8243 0.7433 0.1337 0.017 Uiso 1 1 calc R U . . .
C5 C 1.00375(10) 0.73142(10) 0.08368(5) 0.01636(13) Uani 1 1 d . . . . .
H5 H 1.0418 0.8191 0.0498 0.020 Uiso 1 1 calc R U . . .
C6 C 1.07736(9) 0.64656(10) 0.08354(5) 0.01663(13) Uani 1 1 d . . . . .
H6 H 1.1642 0.6776 0.0497 0.020 Uiso 1 1 calc R U . . .
C7 C 1.02074(9) 0.51471(9) 0.13422(5) 0.01508(13) Uani 1 1 d . . . . .
H7 H 1.0697 0.4577 0.1344 0.018 Uiso 1 1 calc R U . . .
C8 C 0.89013(8) 0.46905(8) 0.18469(5) 0.01100(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Si1 2.0573(13) . ?
Cl1B Si1 2.006(7) . ?
Cl1C Si1 1.964(15) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 Si1 1.899(16) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 Si1 1.876(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 Si1 1.855(6) . ?
Si1 C2 1.9199(7) . ?
C1 H1 0.9800 . ?
C1 C2 1.5815(8) 2_655 ?
C1 C2 1.5814(8) 3_665 ?
C1 C2 1.5815(8) . ?
C2 C3 1.5208(10) . ?
C2 C8 1.5198(10) 2_655 ?
C3 C4 1.3974(11) . ?
C3 C8 1.3976(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.3959(12) . ?
C5 H5 0.9300 . ?
C5 C6 1.3908(13) . ?
C6 H6 0.9300 . ?
C6 C7 1.3963(12) . ?
C7 H7 0.9300 . ?
C7 C8 1.3964(10) . ?
C8 C2 1.5198(10) 3_665 ?

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
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
C11 Si1 Cl1B 109.3(6) . . ?
C11 Si1 C2 110.6(5) . . ?
C10 Si1 Cl1 105.51(19) . . ?
C10 Si1 C2 114.50(19) . . ?
C9 Si1 Cl1 108.7(2) . . ?
C9 Si1 C10 108.3(3) . . ?
C9 Si1 C2 111.0(2) . . ?
C2 Si1 Cl1 108.62(4) . . ?
C2 Si1 Cl1B 110.4(2) . . ?
C2 Si1 Cl1C 111.3(5) . . ?
C2 C1 H1 111.2 . . ?
C2 C1 H1 111.2 2_655 . ?
C2 C1 H1 111.2 3_665 . ?
C2 C1 C2 107.67(5) 2_655 . ?
C2 C1 C2 107.67(5) 3_665 . ?
C2 C1 C2 107.68(5) 3_665 2_655 ?
C1 C2 Si1 113.78(6) . . ?
C3 C2 Si1 115.04(5) . . ?
C3 C2 C1 103.82(5) . . ?
C8 C2 Si1 108.60(5) 2_655 . ?
C8 C2 C1 103.81(5) 2_655 . ?
C8 C2 C3 111.21(6) 2_655 . ?
C4 C3 C2 127.85(7) . . ?
C4 C3 C8 119.73(7) . . ?
C8 C3 C2 112.29(6) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.56(7) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.68(7) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 119.95(7) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.54(8) . . ?
C8 C7 H7 120.2 . . ?
C3 C8 C2 112.39(6) . 3_665 ?
C7 C8 C2 127.05(7) . 3_665 ?
C7 C8 C3 120.54(7) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5 -1 0 0.0974 5.0000 -1.0000 0.0002 0.0982 0.2494 -0.2563
5 0 4 0.0847 5.0000 0.0000 4.0002 0.1164 0.4083 -0.1331
-5 0 -4 0.0847 -5.0000 -0.0000 -4.0002 -0.1164 -0.4083 0.1331
0 1 5 0.0955 -0.0000 1.0000 5.0000 0.0377 0.1851 0.1561
0 -1 -5 0.0955 0.0000 -1.0000 -5.0000 -0.0377 -0.1851 -0.1561
1 2 5 0.0719 1.0000 2.0000 5.0000 -0.0140 0.3002 0.0950
-1 -2 -5 0.0719 -1.0000 -2.0000 -5.0000 0.0140 -0.3002 -0.0950
5 1 0 0.0751 5.0000 1.0000 0.0002 -0.0207 0.3581 -0.2727
-4 -2 -5 0.0744 -4.0000 -2.0000 -5.0002 -0.0093 -0.4825 0.0637
0 -3 5 0.1301 -0.0000 -3.0000 5.0001 0.2753 -0.0323 0.1888
4 -5 -1 0.1528 4.0000 -5.0000 -0.9997 0.3086 -0.0550 -0.2036
-4 5 -1 0.0986 -3.9999 5.0000 -1.0003 -0.3474 0.0026 0.1379
-5 4 3 0.1437 -5.0000 4.0000 2.9997 -0.2181 -0.0078 0.3304
5 -4 -3 0.1437 5.0000 -4.0000 -2.9997 0.2181 0.0078 -0.3304
-5 4 -4 0.0724 -4.9999 4.0000 -4.0003 -0.3540 -0.1909 0.1004
1 -5 1 0.1099 1.0000 -5.0000 1.0002 0.3242 -0.1849 0.0208

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_compound16
_database_code_depnum_ccdc_archive 'CCDC 1514277'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;

_vrf_CHEMW03_compound16          
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The crystal includes 3 highly disordered chloroform in the asymmetric 
          unit. They were treated with the SQUEEZE procedure of Olex2 
          program (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; 
          Puschmann, H., J. Appl. Cryst. (2009). 42, 339-341.),
          but added in the sum formula for further calculations.
;
_vrf_PLAT051_compound16          
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      13.19 %     
RESPONSE: The crystal includes 3 highly disordered chloroform in the asymmetric 
          unit. They were treated with the SQUEEZE procedure of Olex2 
          program (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; 
          Puschmann, H., J. Appl. Cryst. (2009). 42, 339-341.),
          but added in the sum formula for further calculations.
;


_audit_creation_date             2015-01-14
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H25 I3, 1.5(CHCl3)'
_chemical_formula_sum            'C41.50 H26.50 Cl4.50 I3'
_chemical_formula_weight         1065.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C83 H53 Cl9 I6 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   15.4391(2)
_cell_length_b                   18.7068(3)
_cell_length_c                   26.9918(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.9936(16)
_cell_angle_gamma                90
_cell_volume                     7596.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    55933
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.2830
_cell_measurement_theta_min      3.6560
_exptl_absorpt_coefficient_mu    22.530
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.1575
_exptl_crystal_size_mid          0.0843
_exptl_crystal_size_min          0.0246
_exptl_special_details           
;

Miller array info: 
D:/Data/toma23/struct/olex2_toma23_twin1_hklf4/toma23_twin1_hklf4.hkl:Iobs,SigIobs
Observation type: xray.intensity
Type of data: double, size=130209
Type of sigmas: double, size=130209
Number of Miller indices: 130209
Anomalous flag: False
Unit cell: (15.4391, 18.7068, 26.9918, 90, 102.994, 90)
Space group: P 1 21/n 1 (No. 14)
Systematic absences: 0
Centric reflections: 130209
Resolution range: 15.2441 0.838114

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
    C     H     I
 1.70  1.09  1.98

Total solvent accessible volume / cell = 1901.5 Ang^3 [25.0%]
Total electron count / cell = 733.0

gridding: (80,90,144)
Void #Grid points Vol/A^3 Vol/%  Centre of mass (frac)   Eigenvectors (frac)
   1       129769   950.7  12.5  ( 0.000,-0.827,-0.000)  1  ( 0.860, 0.071, 0.505)
                                                         2  (-0.499,-0.085, 0.862)
                                                         3  (-0.104, 0.994, 0.038)
   2       129769   950.7  12.5  ( 0.500,-0.487, 0.500)  1  ( 0.879, 0.113, 0.463)
                                                         2  (-0.443,-0.166, 0.881)
                                                         3  (-0.176, 0.980, 0.096)

Void  Vol/Ang^3  #Electrons
   1      950.7        366.5
   2      950.7        366.5


;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            130209
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.90
_diffrn_reflns_theta_min         2.90
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.9474
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    8.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  120.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   28.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   30.0000 76

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -41.00   13.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 54

#__ type_ start__ end____ width___ exp.time_
  6 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega   54.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega   10.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   19.0000  -30.0000 110

#__ type_ start__ end____ width___ exp.time_
  9 omega   23.00   82.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000   60.0000 59

#__ type_ start__ end____ width___ exp.time_
 10 omega   14.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
 11 omega   14.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega   13.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 66

#__ type_ start__ end____ width___ exp.time_
 13 omega   23.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -125.0000 -180.0000 74

#__ type_ start__ end____ width___ exp.time_
 14 omega   71.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -30.0000 42

#__ type_ start__ end____ width___ exp.time_
 15 omega   18.00   83.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000   90.0000 65

#__ type_ start__ end____ width___ exp.time_
 16 omega   13.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 64

#__ type_ start__ end____ width___ exp.time_
 17 omega   13.00   47.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 34

#__ type_ start__ end____ width___ exp.time_
 18 omega   14.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
 19 omega   30.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000  -30.0000 51

#__ type_ start__ end____ width___ exp.time_
 20 omega   81.00  166.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
 21 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   84.00  110.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000   77.6263 26

#__ type_ start__ end____ width___ exp.time_
 23 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 24 omega   83.00  109.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000  117.6535 26

#__ type_ start__ end____ width___ exp.time_
 25 omega   42.00   99.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 57

#__ type_ start__ end____ width___ exp.time_
 26 omega   85.00  156.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 71

#__ type_ start__ end____ width___ exp.time_
 27 omega   41.00  121.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 80

#__ type_ start__ end____ width___ exp.time_
 28 omega   89.00  117.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
 29 omega  146.00  172.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 30 omega   44.00  129.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 31 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000 -130.4059 26

#__ type_ start__ end____ width___ exp.time_
 33 omega   83.00  164.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   70.0000 -135.1860 81

#__ type_ start__ end____ width___ exp.time_
 34 omega   87.00  115.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   54.0000   74.9292 28

#__ type_ start__ end____ width___ exp.time_
 35 omega  110.00  177.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 67

#__ type_ start__ end____ width___ exp.time_
 36 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   87.00  157.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   53.0000   -8.7378 70

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 39 omega   43.00   89.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 46

#__ type_ start__ end____ width___ exp.time_
 40 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 41 omega  116.00  142.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 42 omega  143.00  171.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 28

#__ type_ start__ end____ width___ exp.time_
 43 omega   41.00  140.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 99

#__ type_ start__ end____ width___ exp.time_
 44 omega   82.00  178.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000   -5.7297 96

#__ type_ start__ end____ width___ exp.time_
 45 omega   84.00  152.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   65.0000  103.2402 68

#__ type_ start__ end____ width___ exp.time_
 46 omega   85.00  177.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 92

#__ type_ start__ end____ width___ exp.time_
 47 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 48 omega  123.00  168.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 45

#__ type_ start__ end____ width___ exp.time_
 49 omega   81.00  118.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 37

#__ type_ start__ end____ width___ exp.time_
 50 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 52 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   82.00  108.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000  174.8904 26

#__ type_ start__ end____ width___ exp.time_
 54 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 55 omega   81.00  178.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
 56 omega   31.00  109.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 78

#__ type_ start__ end____ width___ exp.time_
 57 omega  118.00  174.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 56

#__ type_ start__ end____ width___ exp.time_
 58 omega   86.00  122.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
 59 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 60 omega   81.00  176.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 61 omega   85.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   85.00  160.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 75

#__ type_ start__ end____ width___ exp.time_
 63 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  -72.2663 26

#__ type_ start__ end____ width___ exp.time_
 64 omega   81.00  107.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000   82.4911 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   84.00  110.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000   56.8401 26

#__ type_ start__ end____ width___ exp.time_
 66 omega   94.00  122.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
 67 omega   84.00  111.00   1.0000   72.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000  158.1195 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0094743000
_diffrn_orient_matrix_UB_12      -0.0765352000
_diffrn_orient_matrix_UB_13      -0.0188674000
_diffrn_orient_matrix_UB_21      0.0979840000
_diffrn_orient_matrix_UB_22      0.0147915000
_diffrn_orient_matrix_UB_23      0.0000139000
_diffrn_orient_matrix_UB_31      0.0278579000
_diffrn_orient_matrix_UB_32      -0.0259952000
_diffrn_orient_matrix_UB_33      0.0555596000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.9065 99594 56264
2 0.0935 99398 56264

_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10614
_reflns_number_total             13060
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13060
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0814P)²+11.5323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1466
_refine_special_details          ', SQUEEZE'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
I1 I -0.20755(3) 0.69103(3) 0.16608(2) 0.06523(16) Uani 1 1 d . . . . .
I2 I -0.39479(3) 0.40425(3) 0.41645(2) 0.05443(13) Uani 1 1 d . . . . .
I3 I -0.21489(3) 0.17989(3) 0.13095(2) 0.06231(15) Uani 1 1 d . . . . .
C1 C 0.0035(3) 0.4137(3) 0.3238(2) 0.0294(11) Uani 1 1 d . . . . .
H1 H -0.0573 0.4160 0.3030 0.035 Uiso 1 1 calc R U . . .
C2 C 0.0570(4) 0.4830(3) 0.3165(2) 0.0315(11) Uani 1 1 d . . . . .
C3 C 0.0865(4) 0.5124(3) 0.3705(2) 0.0357(12) Uani 1 1 d . . . . .
C4 C 0.1394(4) 0.5715(3) 0.3859(3) 0.0423(14) Uani 1 1 d . . . . .
H4 H 0.1626 0.5977 0.3626 0.051 Uiso 1 1 calc R U . . .
C5 C 0.1573(5) 0.5908(4) 0.4370(3) 0.0586(19) Uani 1 1 d . . . . .
H5 H 0.1919 0.6310 0.4478 0.070 Uiso 1 1 calc R U . . .
C6 C 0.1243(5) 0.5512(5) 0.4719(3) 0.062(2) Uani 1 1 d . . . . .
H6 H 0.1364 0.5652 0.5059 0.074 Uiso 1 1 calc R U . . .
C7 C 0.0740(5) 0.4913(4) 0.4568(3) 0.0548(17) Uani 1 1 d . . . . .
H7 H 0.0536 0.4639 0.4805 0.066 Uiso 1 1 calc R U . . .
C8 C 0.0535(4) 0.4719(3) 0.4055(2) 0.0388(13) Uani 1 1 d . . . . .
C9 C 0.0026(4) 0.4068(3) 0.3820(2) 0.0364(12) Uani 1 1 d . . . . .
C10 C 0.0553(4) 0.3396(3) 0.3982(2) 0.0360(12) Uani 1 1 d . . . . .
C11 C 0.0803(5) 0.3109(4) 0.4475(3) 0.0515(16) Uani 1 1 d . . . . .
H11 H 0.0631 0.3331 0.4746 0.062 Uiso 1 1 calc R U . . .
C12 C 0.1302(5) 0.2500(4) 0.4550(3) 0.0586(19) Uani 1 1 d . . . . .
H12 H 0.1454 0.2302 0.4874 0.070 Uiso 1 1 calc R U . . .
C13 C 0.1590(5) 0.2167(4) 0.4154(3) 0.0526(17) Uani 1 1 d . . . . .
H13 H 0.1936 0.1756 0.4212 0.063 Uiso 1 1 calc R U . . .
C14 C 0.1352(4) 0.2458(3) 0.3678(3) 0.0442(14) Uani 1 1 d . . . . .
H14 H 0.1541 0.2242 0.3411 0.053 Uiso 1 1 calc R U . . .
C15 C 0.0834(4) 0.3070(3) 0.3587(2) 0.0360(12) Uani 1 1 d . . . . .
C16 C 0.0535(3) 0.3470(3) 0.3090(2) 0.0313(11) Uani 1 1 d . . . . .
C17 C 0.1327(3) 0.3802(3) 0.2929(2) 0.0272(10) Uani 1 1 d . . . . .
C18 C 0.2004(4) 0.3439(3) 0.2765(2) 0.0348(12) Uani 1 1 d . . . . .
H18 H 0.1990 0.2944 0.2735 0.042 Uiso 1 1 calc R U . A 1
C19 C 0.2689(4) 0.3823(3) 0.2650(2) 0.0367(12) Uani 1 1 d . . . B 1
H19 H 0.3135 0.3586 0.2534 0.044 Uiso 1 1 calc R U . B 1
C20 C 0.2726(4) 0.4561(3) 0.2704(2) 0.0378(13) Uani 1 1 d . . . . .
H20 H 0.3209 0.4811 0.2638 0.045 Uiso 1 1 calc R U . B 1
C21 C 0.2042(4) 0.4935(3) 0.2855(2) 0.0363(13) Uani 1 1 d . . . . .
H21 H 0.2050 0.5431 0.2876 0.044 Uiso 1 1 calc R U . . .
C22 C 0.1348(4) 0.4540(3) 0.2974(2) 0.0314(11) Uani 1 1 d . . . . .
C23 C -0.0006(4) 0.5357(3) 0.2807(2) 0.0321(11) Uani 1 1 d . . . . .
C24 C -0.0093(4) 0.5319(3) 0.2279(2) 0.0388(13) Uani 1 1 d . . . . .
H24 H 0.0249 0.4994 0.2145 0.047 Uiso 1 1 calc R U . . .
C25 C -0.0680(4) 0.5759(3) 0.1955(3) 0.0450(14) Uani 1 1 d . . . . .
H25 H -0.0723 0.5737 0.1606 0.054 Uiso 1 1 calc R U . . .
C26 C -0.1200(4) 0.6233(3) 0.2151(3) 0.0465(15) Uani 1 1 d . . . . .
C27 C -0.1124(4) 0.6282(3) 0.2666(3) 0.0438(15) Uani 1 1 d . . . . .
H27 H -0.1470 0.6607 0.2797 0.053 Uiso 1 1 calc R U . . .
C28 C -0.0537(4) 0.5850(3) 0.2986(2) 0.0369(13) Uani 1 1 d . . . . .
H28 H -0.0491 0.5887 0.3335 0.044 Uiso 1 1 calc R U . . .
C29 C -0.0928(4) 0.4041(4) 0.3904(2) 0.0418(14) Uani 1 1 d . . . . .
C30 C -0.1428(5) 0.4646(4) 0.3846(4) 0.071(3) Uani 1 1 d . . . . .
H30 H -0.1179 0.5072 0.3767 0.085 Uiso 1 1 calc R U . . .
C31 C -0.2299(5) 0.4644(4) 0.3900(3) 0.065(2) Uani 1 1 d . . . . .
H31 H -0.2639 0.5058 0.3841 0.078 Uiso 1 1 calc R U . . .
C32 C -0.2656(4) 0.4024(4) 0.4042(2) 0.0457(15) Uani 1 1 d . . . . .
C33 C -0.2170(4) 0.3405(4) 0.4122(3) 0.0477(15) Uani 1 1 d . . . . .
H33 H -0.2408 0.2989 0.4224 0.057 Uiso 1 1 calc R U . . .
C34 C -0.1291(4) 0.3417(4) 0.4043(2) 0.0431(14) Uani 1 1 d . . . . .
H34 H -0.0955 0.3000 0.4085 0.052 Uiso 1 1 calc R U . . .
C35 C -0.0058(3) 0.3038(3) 0.2667(2) 0.0333(12) Uani 1 1 d . . . . .
C36 C -0.0566(4) 0.2469(3) 0.2775(3) 0.0419(14) Uani 1 1 d . . . . .
H36 H -0.0513 0.2324 0.3111 0.050 Uiso 1 1 calc R U . . .
C37 C -0.1155(4) 0.2115(3) 0.2384(3) 0.0438(15) Uani 1 1 d . . . . .
H37 H -0.1498 0.1740 0.2461 0.053 Uiso 1 1 calc R U . . .
C38 C -0.1230(4) 0.2311(3) 0.1895(3) 0.0429(14) Uani 1 1 d . . . . .
C39 C -0.0732(5) 0.2873(4) 0.1775(3) 0.0516(16) Uani 1 1 d . . . . .
H39 H -0.0793 0.3010 0.1438 0.062 Uiso 1 1 calc R U . . .
C40 C -0.0144(4) 0.3230(3) 0.2154(3) 0.0436(14) Uani 1 1 d . . . . .
H40 H 0.0198 0.3601 0.2070 0.052 Uiso 1 1 calc R U . . .
I4 I 0.62609(3) 0.32090(2) 0.63770(2) 0.05703(14) Uani 1 1 d . . . . .
I5 I 1.01943(3) 0.54182(4) 0.92059(2) 0.0792(2) Uani 1 1 d . . . . .
I6 I 0.64299(3) 0.85246(2) 0.65855(2) 0.04870(13) Uani 1 1 d . . . . .
C41 C 0.5536(3) 0.5737(3) 0.8192(2) 0.0287(11) Uani 1 1 d . . . . .
H41 H 0.5995 0.5747 0.7994 0.034 Uiso 1 1 calc R U . . .
C42 C 0.4892(3) 0.5090(3) 0.8030(2) 0.0304(11) Uani 1 1 d . . . . .
C43 C 0.4926(4) 0.4707(3) 0.8531(2) 0.0319(11) Uani 1 1 d . . . . .
C44 C 0.4411(4) 0.4115(3) 0.8606(3) 0.0403(14) Uani 1 1 d . . . . .
H44 H 0.4030 0.3893 0.8333 0.048 Uiso 1 1 calc R U . . .
C45 C 0.4486(4) 0.3875(3) 0.9092(3) 0.0429(15) Uani 1 1 d . . . . .
H45 H 0.4154 0.3480 0.9147 0.051 Uiso 1 1 calc R U . . .
C46 C 0.5043(5) 0.4203(4) 0.9509(3) 0.0541(18) Uani 1 1 d . . . . .
H46 H 0.5081 0.4028 0.9835 0.065 Uiso 1 1 calc R U . . .
C47 C 0.5537(4) 0.4790(3) 0.9431(3) 0.0433(14) Uani 1 1 d . . . . .
H47 H 0.5901 0.5019 0.9707 0.052 Uiso 1 1 calc R U . . .
C48 C 0.5491(4) 0.5039(3) 0.8938(2) 0.0349(12) Uani 1 1 d . . . . .
C49 C 0.5969(4) 0.5665(3) 0.8776(2) 0.0341(12) Uani 1 1 d . . . . .
C50 C 0.5693(4) 0.6360(3) 0.8997(2) 0.0371(13) Uani 1 1 d . . . . .
C51 C 0.5939(5) 0.6597(3) 0.9498(3) 0.0456(15) Uani 1 1 d . . . . .
H51 H 0.6334 0.6334 0.9741 0.055 Uiso 1 1 calc R U . . .
C52 C 0.5585(6) 0.7234(4) 0.9630(3) 0.0547(18) Uani 1 1 d . . . . .
H52 H 0.5748 0.7401 0.9963 0.066 Uiso 1 1 calc R U . . .
C53 C 0.4993(6) 0.7619(4) 0.9269(3) 0.058(2) Uani 1 1 d . . . . .
H53 H 0.4759 0.8043 0.9363 0.069 Uiso 1 1 calc R U . . .
C54 C 0.4744(5) 0.7388(3) 0.8775(3) 0.0495(17) Uani 1 1 d . . . . .
H54 H 0.4337 0.7651 0.8538 0.059 Uiso 1 1 calc R U . . .
C55 C 0.5107(4) 0.6753(3) 0.8629(3) 0.0388(13) Uani 1 1 d . . . . .
C56 C 0.4969(4) 0.6443(3) 0.8109(2) 0.0344(12) Uani 1 1 d . . . . .
C57 C 0.4037(4) 0.6177(3) 0.7891(3) 0.0391(14) Uani 1 1 d . . . . .
C58 C 0.3267(4) 0.6577(3) 0.7750(3) 0.0525(18) Uani 1 1 d . . . . .
H58 H 0.3291 0.7072 0.7775 0.063 Uiso 1 1 calc R U . . .
C59 C 0.2455(5) 0.6235(4) 0.7572(4) 0.081(3) Uani 1 1 d . . . . .
H59 H 0.1935 0.6500 0.7480 0.097 Uiso 1 1 calc R U . . .
C60 C 0.2429(4) 0.5490(4) 0.7531(4) 0.083(3) Uani 1 1 d . . . . .
H60 H 0.1886 0.5259 0.7422 0.099 Uiso 1 1 calc R U . . .
C61 C 0.3197(4) 0.5094(4) 0.7652(4) 0.064(2) Uani 1 1 d . . . . .
H61 H 0.3182 0.4601 0.7607 0.077 Uiso 1 1 calc R U . . .
C62 C 0.3988(4) 0.5439(3) 0.7840(3) 0.0401(14) Uani 1 1 d . . . . .
C63 C 0.5179(3) 0.4612(3) 0.7635(2) 0.0284(11) Uani 1 1 d . . . . .
C64 C 0.4829(4) 0.4715(3) 0.7116(2) 0.0396(13) Uani 1 1 d . . . . .
H64 H 0.4389 0.5056 0.7009 0.048 Uiso 1 1 calc R U . . .
C65 C 0.5137(4) 0.4309(3) 0.6756(2) 0.0424(13) Uani 1 1 d . . . . .
H65 H 0.4897 0.4373 0.6411 0.051 Uiso 1 1 calc R U . . .
C66 C 0.5799(4) 0.3812(3) 0.6918(2) 0.0374(13) Uani 1 1 d . . . . .
C67 C 0.6146(4) 0.3708(3) 0.7426(2) 0.0361(12) Uani 1 1 d . . . . .
H67 H 0.6583 0.3362 0.7531 0.043 Uiso 1 1 calc R U . . .
C68 C 0.5852(4) 0.4113(3) 0.7783(2) 0.0325(11) Uani 1 1 d . . . . .
H68 H 0.6108 0.4050 0.8127 0.039 Uiso 1 1 calc R U . . .
C69 C 0.6973(4) 0.5587(3) 0.8888(2) 0.0345(12) Uani 1 1 d . . . . .
C70 C 0.7433(4) 0.5006(3) 0.9162(2) 0.0436(14) Uani 1 1 d . . . . .
H70 H 0.7112 0.4648 0.9280 0.052 Uiso 1 1 calc R U . . .
C71 C 0.8341(5) 0.4961(4) 0.9259(3) 0.0499(16) Uani 1 1 d . . . . .
H71 H 0.8638 0.4588 0.9453 0.060 Uiso 1 1 calc R U . . .
C72 C 0.8813(4) 0.5486(4) 0.9062(3) 0.0515(16) Uani 1 1 d . . . . .
C73 C 0.8387(4) 0.6052(4) 0.8781(3) 0.0492(15) Uani 1 1 d . . . . .
H73 H 0.8712 0.6392 0.8648 0.059 Uiso 1 1 calc R U . . .
C74 C 0.7481(4) 0.6110(3) 0.8700(2) 0.0409(13) Uani 1 1 d . . . . .
H74 H 0.7195 0.6498 0.8519 0.049 Uiso 1 1 calc R U . . .
C75 C 0.5283(3) 0.6964(3) 0.7737(2) 0.0318(12) Uani 1 1 d . . . . .
C76 C 0.5915(4) 0.7481(3) 0.7926(2) 0.0343(12) Uani 1 1 d . . . . .
H76 H 0.6119 0.7535 0.8275 0.041 Uiso 1 1 calc R U . . .
C77 C 0.6246(4) 0.7923(3) 0.7592(2) 0.0390(13) Uani 1 1 d . . . . .
H77 H 0.6667 0.8272 0.7719 0.047 Uiso 1 1 calc R U . . .
C78 C 0.5947(4) 0.7839(3) 0.7077(2) 0.0388(13) Uani 1 1 d . . . . .
C79 C 0.5322(4) 0.7317(3) 0.6886(3) 0.0423(14) Uani 1 1 d . . . . .
H79 H 0.5119 0.7260 0.6537 0.051 Uiso 1 1 calc R U . . .
C80 C 0.5004(4) 0.6886(3) 0.7216(2) 0.0366(12) Uani 1 1 d . . . . .
H80 H 0.4590 0.6533 0.7087 0.044 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
I1 C26 2.093(6) . ?
I2 C32 2.094(6) . ?
I3 C38 2.103(6) . ?
C1 H1 0.9800 . ?
C1 C2 1.574(7) . ?
C1 C9 1.577(8) . ?
C1 C16 1.566(7) . ?
C2 C3 1.529(8) . ?
C2 C22 1.511(7) . ?
C2 C23 1.519(8) . ?
C3 C4 1.381(8) . ?
C3 C8 1.393(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.372(11) . ?
C7 H7 0.9300 . ?
C7 C8 1.397(9) . ?
C8 C9 1.510(9) . ?
C9 C10 1.508(8) . ?
C9 C29 1.541(8) . ?
C10 C11 1.406(9) . ?
C10 C15 1.378(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.364(11) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.367(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.386(8) . ?
C15 C16 1.515(8) . ?
C16 C17 1.519(7) . ?
C16 C35 1.525(8) . ?
C17 C18 1.398(7) . ?
C17 C22 1.386(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.371(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.389(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.401(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.398(8) . ?
C23 C24 1.404(8) . ?
C23 C28 1.391(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.381(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(9) . ?
C26 C27 1.372(10) . ?
C27 H27 0.9300 . ?
C27 C28 1.368(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.359(10) . ?
C29 C34 1.382(9) . ?
C30 H30 0.9300 . ?
C30 C31 1.385(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.376(10) . ?
C32 C33 1.370(10) . ?
C33 H33 0.9300 . ?
C33 C34 1.420(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.393(8) . ?
C35 C40 1.407(9) . ?
C36 H36 0.9300 . ?
C36 C37 1.396(9) . ?
C37 H37 0.9300 . ?
C37 C38 1.351(10) . ?
C38 C39 1.381(9) . ?
C39 H39 0.9300 . ?
C39 C40 1.378(10) . ?
C40 H40 0.9300 . ?
I4 C66 2.094(6) . ?
I5 C72 2.084(7) . ?
I6 C78 2.098(6) . ?
C41 H41 0.9800 . ?
C41 C42 1.566(7) . ?
C41 C49 1.574(8) . ?
C41 C56 1.573(7) . ?
C42 C43 1.523(8) . ?
C42 C62 1.521(7) . ?
C42 C63 1.530(7) . ?
C43 C44 1.404(8) . ?
C43 C48 1.386(8) . ?
C44 H44 0.9300 . ?
C44 C45 1.367(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.395(11) . ?
C46 H46 0.9300 . ?
C46 C47 1.379(9) . ?
C47 H47 0.9300 . ?
C47 C48 1.397(9) . ?
C48 C49 1.500(7) . ?
C49 C50 1.529(7) . ?
C49 C69 1.518(8) . ?
C50 C51 1.395(9) . ?
C50 C55 1.393(9) . ?
C51 H51 0.9300 . ?
C51 C52 1.390(9) . ?
C52 H52 0.9300 . ?
C52 C53 1.380(11) . ?
C53 H53 0.9300 . ?
C53 C54 1.372(10) . ?
C54 H54 0.9300 . ?
C54 C55 1.408(8) . ?
C55 C56 1.490(9) . ?
C56 C57 1.512(8) . ?
C56 C75 1.554(7) . ?
C57 C58 1.384(8) . ?
C57 C62 1.388(8) . ?
C58 H58 0.9300 . ?
C58 C59 1.392(10) . ?
C59 H59 0.9300 . ?
C59 C60 1.398(11) . ?
C60 H60 0.9300 . ?
C60 C61 1.373(10) . ?
C61 H61 0.9300 . ?
C61 C62 1.373(9) . ?
C63 C64 1.396(8) . ?
C63 C68 1.388(8) . ?
C64 H64 0.9300 . ?
C64 C65 1.397(9) . ?
C65 H65 0.9300 . ?
C65 C66 1.378(9) . ?
C66 C67 1.370(9) . ?
C67 H67 0.9300 . ?
C67 C68 1.380(8) . ?
C68 H68 0.9300 . ?
C69 C70 1.413(9) . ?
C69 C74 1.416(8) . ?
C70 H70 0.9300 . ?
C70 C71 1.370(10) . ?
C71 H71 0.9300 . ?
C71 C72 1.398(11) . ?
C72 C73 1.380(10) . ?
C73 H73 0.9300 . ?
C73 C74 1.371(9) . ?
C74 H74 0.9300 . ?
C75 C76 1.386(8) . ?
C75 C80 1.381(9) . ?
C76 H76 0.9300 . ?
C76 C77 1.402(8) . ?
C77 H77 0.9300 . ?
C77 C78 1.372(9) . ?
C78 C79 1.388(9) . ?
C79 H79 0.9300 . ?
C79 C80 1.373(8) . ?
C80 H80 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 110.7 . . ?
C2 C1 C9 108.3(4) . . ?
C9 C1 H1 110.7 . . ?
C16 C1 H1 110.7 . . ?
C16 C1 C2 108.7(4) . . ?
C16 C1 C9 107.7(4) . . ?
C3 C2 C1 103.2(4) . . ?
C22 C2 C1 103.1(4) . . ?
C22 C2 C3 111.4(5) . . ?
C22 C2 C23 114.4(5) . . ?
C23 C2 C1 111.4(4) . . ?
C23 C2 C3 112.3(4) . . ?
C4 C3 C2 127.1(5) . . ?
C4 C3 C8 120.9(6) . . ?
C8 C3 C2 112.0(5) . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.5(6) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(7) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.3(7) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.7(7) . . ?
C8 C7 H7 120.2 . . ?
C3 C8 C7 119.6(6) . . ?
C3 C8 C9 112.9(5) . . ?
C7 C8 C9 127.4(6) . . ?
C8 C9 C1 103.4(4) . . ?
C8 C9 C29 112.8(5) . . ?
C10 C9 C1 103.4(4) . . ?
C10 C9 C8 110.8(5) . . ?
C10 C9 C29 113.7(5) . . ?
C29 C9 C1 111.9(5) . . ?
C11 C10 C9 127.4(6) . . ?
C15 C10 C9 112.8(5) . . ?
C15 C10 C11 119.7(6) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.0(7) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 119.1 . . ?
C11 C12 C13 121.7(7) . . ?
C13 C12 H12 119.1 . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(6) . . ?
C14 C13 H13 120.7 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(7) . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C14 119.9(6) . . ?
C10 C15 C16 112.3(5) . . ?
C14 C15 C16 127.8(6) . . ?
C15 C16 C1 103.7(5) . . ?
C15 C16 C17 110.5(4) . . ?
C15 C16 C35 114.4(4) . . ?
C17 C16 C1 102.9(4) . . ?
C17 C16 C35 112.8(5) . . ?
C35 C16 C1 111.5(4) . . ?
C18 C17 C16 126.8(5) . . ?
C22 C17 C16 112.7(4) . . ?
C22 C17 C18 120.4(5) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.2(5) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.8(5) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.7(5) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 121.0 . . ?
C22 C21 C20 118.0(5) . . ?
C22 C21 H21 121.0 . . ?
C17 C22 C2 112.6(4) . . ?
C17 C22 C21 120.7(5) . . ?
C21 C22 C2 126.7(5) . . ?
C24 C23 C2 121.5(5) . . ?
C28 C23 C2 121.0(5) . . ?
C28 C23 C24 117.2(5) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.8(5) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.7(6) . . ?
C26 C25 H25 120.1 . . ?
C25 C26 I1 119.7(5) . . ?
C27 C26 I1 119.7(5) . . ?
C27 C26 C25 120.6(6) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.6(6) . . ?
C28 C27 H27 120.2 . . ?
C23 C28 H28 118.9 . . ?
C27 C28 C23 122.1(6) . . ?
C27 C28 H28 118.9 . . ?
C30 C29 C9 119.5(6) . . ?
C30 C29 C34 118.7(6) . . ?
C34 C29 C9 121.8(5) . . ?
C29 C30 H30 119.2 . . ?
C29 C30 C31 121.6(7) . . ?
C31 C30 H30 119.2 . . ?
C30 C31 H31 120.3 . . ?
C32 C31 C30 119.5(7) . . ?
C32 C31 H31 120.3 . . ?
C31 C32 I2 119.0(5) . . ?
C33 C32 I2 119.8(5) . . ?
C33 C32 C31 121.1(6) . . ?
C32 C33 H33 120.9 . . ?
C32 C33 C34 118.1(6) . . ?
C34 C33 H33 120.9 . . ?
C29 C34 C33 120.9(6) . . ?
C29 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C16 121.2(5) . . ?
C36 C35 C40 118.0(6) . . ?
C40 C35 C16 120.7(5) . . ?
C35 C36 H36 119.8 . . ?
C35 C36 C37 120.3(6) . . ?
C37 C36 H36 119.8 . . ?
C36 C37 H37 119.7 . . ?
C38 C37 C36 120.6(6) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 I3 120.3(5) . . ?
C37 C38 C39 120.4(6) . . ?
C39 C38 I3 119.2(5) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 C38 120.3(7) . . ?
C40 C39 H39 119.9 . . ?
C35 C40 H40 119.8 . . ?
C39 C40 C35 120.4(6) . . ?
C39 C40 H40 119.8 . . ?
C42 C41 H41 110.7 . . ?
C42 C41 C49 108.3(4) . . ?
C42 C41 C56 108.1(4) . . ?
C49 C41 H41 110.7 . . ?
C56 C41 H41 110.7 . . ?
C56 C41 C49 108.2(4) . . ?
C43 C42 C41 102.8(4) . . ?
C43 C42 C63 112.7(4) . . ?
C62 C42 C41 103.9(4) . . ?
C62 C42 C43 110.3(4) . . ?
C62 C42 C63 113.8(5) . . ?
C63 C42 C41 112.4(4) . . ?
C44 C43 C42 126.2(6) . . ?
C48 C43 C42 112.5(5) . . ?
C48 C43 C44 121.1(6) . . ?
C43 C44 H44 121.1 . . ?
C45 C44 C43 117.9(6) . . ?
C45 C44 H44 121.1 . . ?
C44 C45 H45 118.9 . . ?
C44 C45 C46 122.2(5) . . ?
C46 C45 H45 118.9 . . ?
C45 C46 H46 120.3 . . ?
C47 C46 C45 119.3(6) . . ?
C47 C46 H46 120.3 . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 119.9(6) . . ?
C48 C47 H47 120.0 . . ?
C43 C48 C47 119.5(5) . . ?
C43 C48 C49 112.6(5) . . ?
C47 C48 C49 127.9(6) . . ?
C48 C49 C41 103.4(5) . . ?
C48 C49 C50 110.6(4) . . ?
C48 C49 C69 114.5(5) . . ?
C50 C49 C41 102.9(5) . . ?
C69 C49 C41 113.0(4) . . ?
C69 C49 C50 111.5(5) . . ?
C51 C50 C49 127.6(6) . . ?
C55 C50 C49 111.4(5) . . ?
C55 C50 C51 120.9(5) . . ?
C50 C51 H51 120.5 . . ?
C52 C51 C50 119.0(7) . . ?
C52 C51 H51 120.5 . . ?
C51 C52 H52 119.9 . . ?
C53 C52 C51 120.1(7) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 119.3 . . ?
C54 C53 C52 121.3(6) . . ?
C54 C53 H53 119.3 . . ?
C53 C54 H54 120.2 . . ?
C53 C54 C55 119.6(7) . . ?
C55 C54 H54 120.2 . . ?
C50 C55 C54 118.9(6) . . ?
C50 C55 C56 113.5(5) . . ?
C54 C55 C56 127.6(6) . . ?
C55 C56 C41 103.6(5) . . ?
C55 C56 C57 114.7(5) . . ?
C55 C56 C75 111.5(5) . . ?
C57 C56 C41 103.2(4) . . ?
C57 C56 C75 111.3(5) . . ?
C75 C56 C41 112.0(4) . . ?
C58 C57 C56 127.8(5) . . ?
C58 C57 C62 119.1(6) . . ?
C62 C57 C56 113.1(5) . . ?
C57 C58 H58 120.1 . . ?
C57 C58 C59 119.8(6) . . ?
C59 C58 H58 120.1 . . ?
C58 C59 H59 120.2 . . ?
C58 C59 C60 119.5(6) . . ?
C60 C59 H59 120.2 . . ?
C59 C60 H60 119.6 . . ?
C61 C60 C59 120.7(7) . . ?
C61 C60 H60 119.6 . . ?
C60 C61 H61 120.6 . . ?
C60 C61 C62 118.9(6) . . ?
C62 C61 H61 120.6 . . ?
C57 C62 C42 111.6(5) . . ?
C61 C62 C42 126.5(5) . . ?
C61 C62 C57 121.9(5) . . ?
C64 C63 C42 120.7(5) . . ?
C68 C63 C42 120.5(5) . . ?
C68 C63 C64 118.5(5) . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.5(5) . . ?
C65 C64 H64 119.7 . . ?
C64 C65 H65 120.4 . . ?
C66 C65 C64 119.3(6) . . ?
C66 C65 H65 120.4 . . ?
C65 C66 I4 119.1(5) . . ?
C67 C66 I4 120.2(4) . . ?
C67 C66 C65 120.6(5) . . ?
C66 C67 H67 119.9 . . ?
C66 C67 C68 120.3(5) . . ?
C68 C67 H67 119.9 . . ?
C63 C68 H68 119.6 . . ?
C67 C68 C63 120.8(5) . . ?
C67 C68 H68 119.6 . . ?
C70 C69 C49 123.2(5) . . ?
C70 C69 C74 117.8(5) . . ?
C74 C69 C49 119.0(5) . . ?
C69 C70 H70 119.4 . . ?
C71 C70 C69 121.3(6) . . ?
C71 C70 H70 119.4 . . ?
C70 C71 H71 120.6 . . ?
C70 C71 C72 118.9(6) . . ?
C72 C71 H71 120.6 . . ?
C71 C72 I5 119.1(5) . . ?
C73 C72 I5 119.4(5) . . ?
C73 C72 C71 121.5(6) . . ?
C72 C73 H73 120.3 . . ?
C74 C73 C72 119.4(6) . . ?
C74 C73 H73 120.3 . . ?
C69 C74 H74 119.5 . . ?
C73 C74 C69 121.0(6) . . ?
C73 C74 H74 119.5 . . ?
C76 C75 C56 119.7(5) . . ?
C80 C75 C56 121.3(5) . . ?
C80 C75 C76 118.8(5) . . ?
C75 C76 H76 119.9 . . ?
C75 C76 C77 120.2(6) . . ?
C77 C76 H76 119.9 . . ?
C76 C77 H77 120.1 . . ?
C78 C77 C76 119.7(5) . . ?
C78 C77 H77 120.1 . . ?
C77 C78 I6 118.9(4) . . ?
C77 C78 C79 120.2(5) . . ?
C79 C78 I6 120.8(5) . . ?
C78 C79 H79 120.2 . . ?
C80 C79 C78 119.6(6) . . ?
C80 C79 H79 120.2 . . ?
C75 C80 H80 119.3 . . ?
C79 C80 C75 121.5(6) . . ?
C79 C80 H80 119.3 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.827 0.000 950.7 366.5 ?
2 0.500 -0.487 0.500 950.7 366.5 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 1 0.0143 -0.0008 -0.0007 0.9988 -0.0188 -0.0001 0.0555
0 0 -1 0.0103 0.0008 0.0007 -0.9988 0.0188 0.0001 -0.0555
1 2 5 0.0239 0.9963 1.9997 4.9894 -0.2377 0.1273 0.2530
-1 -2 -5 0.0159 -0.9963 -1.9997 -4.9894 0.2377 -0.1273 -0.2530
5 -1 -1 0.0495 5.0070 -0.9986 -1.0142 0.1430 0.4758 0.1091
-5 1 1 0.0315 -5.0070 0.9986 1.0142 -0.1430 -0.4758 -0.1091

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound13
_database_code_depnum_ccdc_archive 'CCDC 1514275'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-07-20
_audit_creation_method           
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H40 F6 Si3, Cl3 Sb'
_chemical_formula_sum            'C34 H40 Cl3 F6 Sb Si3'
_chemical_formula_weight         875.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H40 Cl3 F6 Sb1 Si3'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.27399(19)
_cell_length_b                   26.8362(6)
_cell_length_c                   14.2421(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.165(2)
_cell_angle_gamma                90
_cell_volume                     3790.02(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    57901
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0400
_cell_measurement_theta_min      2.9310
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0248
0 1 0 0.0248
0 0 1 0.1168
0 0 -1 0.1168
0 0 0 0.1897
0 0 0 0.1897

_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0012 -1.0025 -0.0011 -0.0263 -0.0008 0.0027
-0.0012 1.0025 0.0011 0.0263 0.0008 -0.0027
-0.0002 -0.0022 1.0032 -0.0054 0.0030 -0.0514
0.0002 0.0022 -1.0032 0.0054 -0.0030 0.0514
0.3350 0.0011 -0.0009 -0.0013 0.0234 -0.0048
-0.3350 -0.0011 0.0009 0.0013 -0.0234 0.0048

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            222083
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         2.554
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00 -24.00   1.00   16.50    --  -17.08 126.00-131.72   48
  2  ω    -72.00 -24.00   1.00   16.50    --  -17.08 126.00 122.74   48
  3  ω    -75.00 -27.00   1.00   16.50    --  -17.08 131.00  37.75   48
  4  ω     -8.00  86.00   1.00   16.50    --   17.39  57.00 -60.00   94
  5  ω    -13.00  89.00   1.00   16.50    --   17.39  77.00 150.00  102
  6  ω    -51.00  43.00   1.00   16.50    --   17.39 -57.00   0.00   94
  7  ω     35.00 101.00   1.00   16.50    --   17.39 178.00-180.00   66
  8  ω     -8.00  86.00   1.00   16.50    --   17.39  57.00  60.00   94
  9  ω    -54.00  38.00   1.00   16.50    --   17.39 -37.00-120.00   92
 10  ω    -51.00  43.00   1.00   16.50    --   17.39 -57.00 150.00   94
 11  ω    -85.00   8.00   1.00   16.50    --  -17.08 -57.00-150.00   93
 12  ω    -91.00 -39.00   1.00   16.50    --  -17.08 154.00 149.93   52
 13  ω    -88.00  13.00   1.00   16.50    --  -17.08 -77.00 -60.00  101
 14  ω    -75.00 -27.00   1.00   16.50    --  -17.08 131.00 -13.33   48
 15  ω    -69.00 -20.00   1.00   16.50    --  -17.08 121.00 -91.07   49
 16  ω    -88.00   3.00   1.00   16.50    --  -17.08 -37.00-150.00   91
 17  ω    -76.00 -29.00   1.00   16.50    --  -17.08 133.00  65.82   47
 18  ω    -75.00 -27.00   1.00   16.50    --  -17.08 131.00 -45.22   48
 19  ω    -42.00  51.00   1.00   16.50    --  -17.08  57.00-120.00   93
 20  ω   -101.00 -55.00   1.00   16.50    --  -17.08 178.00 -30.00   46
 21  ω    -50.00  15.00   1.00   16.50    --  -17.08  85.00 -96.69   65
 22  ω    -51.00  43.00   1.00   16.50    --   17.39 -57.00  60.00   94
 23  ω    -20.00  56.00   1.00   16.50    --   17.39 -99.00  60.00   76
 24  ω    -68.00 103.00   1.00   16.50    --   17.39   0.00-180.00  171
 25  ω     35.00 101.00   1.00   16.50    --   17.39 178.00  90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038738000
_diffrn_orient_matrix_UB_12      0.0262813000
_diffrn_orient_matrix_UB_13      -0.0053597000
_diffrn_orient_matrix_UB_21      0.0699687000
_diffrn_orient_matrix_UB_22      0.0009113000
_diffrn_orient_matrix_UB_23      0.0030241000
_diffrn_orient_matrix_UB_31      -0.0143088000
_diffrn_orient_matrix_UB_32      -0.0026959000
_diffrn_orient_matrix_UB_33      -0.0512289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9358
_reflns_number_total             11143
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0395P)²+2.9446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0931
_refine_special_details          
;
 Disorder of SbCl3 over two sites (50:50).
 Disorder of Si(3), F(5), F(6), C(31), C(32), C(33), C(34) over two sites (50:50).
 Disorder of F(1), F(2), C(26) over tow sites (83:17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.18018(5) 0.16739(2) 0.14923(4) 0.03055(10) Uani 1 1 d . . . . .
Si2 Si 0.32529(5) 0.45126(2) 0.43840(4) 0.03095(10) Uani 1 1 d . . . . .
F3 F 0.25526(14) 0.39863(5) 0.43750(11) 0.0518(3) Uani 1 1 d . . . . .
F4 F 0.46412(13) 0.44532(5) 0.51919(9) 0.0470(3) Uani 1 1 d . . . . .
C1 C 0.50441(15) 0.34743(5) 0.11985(12) 0.0238(3) Uani 1 1 d . . . . .
H1 H 0.4101 0.3470 0.1226 0.029 Uiso 1 1 calc R U . . .
C2 C 0.58656(14) 0.30420(5) 0.18250(11) 0.0206(3) Uani 1 1 d . . . . .
C3 C 0.69919(14) 0.33086(5) 0.25568(11) 0.0222(3) Uani 1 1 d . . . . .
C4 C 0.80366(16) 0.30955(6) 0.32710(13) 0.0292(3) Uani 1 1 d . . . . .
H4 H 0.8071 0.2752 0.3365 0.035 Uiso 1 1 calc R U . . .
C5 C 0.90267(18) 0.34002(7) 0.38414(16) 0.0389(4) Uani 1 1 d . . . . .
H5 H 0.9732 0.3260 0.4315 0.047 Uiso 1 1 calc R U . . .
C6 C 0.89671(19) 0.39153(7) 0.37064(17) 0.0433(5) Uani 1 1 d . . . . .
H6 H 0.9629 0.4117 0.4094 0.052 Uiso 1 1 calc R U . . .
C7 C 0.79298(18) 0.41279(6) 0.29993(15) 0.0351(4) Uani 1 1 d . . . . .
H7 H 0.7892 0.4471 0.2909 0.042 Uiso 1 1 calc R U . . .
C8 C 0.69389(15) 0.38213(6) 0.24217(12) 0.0248(3) Uani 1 1 d . . . . .
C9 C 0.57445(15) 0.39800(5) 0.15995(12) 0.0240(3) Uani 1 1 d . . . . .
C10 C 0.62082(15) 0.41872(6) 0.07501(12) 0.0249(3) Uani 1 1 d . . . . .
C11 C 0.68882(18) 0.46345(6) 0.07114(14) 0.0314(3) Uani 1 1 d . . . . .
H11 H 0.7080 0.4850 0.1241 0.038 Uiso 1 1 calc R U . . .
C12 C 0.72752(18) 0.47532(6) -0.01251(14) 0.0333(4) Uani 1 1 d . . . . .
H12 H 0.7740 0.5048 -0.0153 0.040 Uiso 1 1 calc R U . . .
C13 C 0.6974(2) 0.44362(7) -0.09167(13) 0.0357(4) Uani 1 1 d . . . . .
H13 H 0.7235 0.4520 -0.1475 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6283(2) 0.39936(7) -0.08856(13) 0.0356(4) Uani 1 1 d . . . . .
H14 H 0.6073 0.3782 -0.1422 0.043 Uiso 1 1 calc R U . . .
C15 C 0.59100(16) 0.38705(6) -0.00457(12) 0.0270(3) Uani 1 1 d . . . . .
C16 C 0.51513(16) 0.34091(6) 0.01275(12) 0.0263(3) Uani 1 1 d . . . . .
C17 C 0.60099(16) 0.29429(6) 0.01687(11) 0.0247(3) Uani 1 1 d . . . . .
C18 C 0.64112(19) 0.27148(7) -0.05878(13) 0.0324(3) Uani 1 1 d . . . . .
H18 H 0.6124 0.2840 -0.1217 0.039 Uiso 1 1 calc R U . . .
C19 C 0.72433(19) 0.22993(7) -0.03947(14) 0.0349(4) Uani 1 1 d . . . . .
H19 H 0.7511 0.2145 -0.0898 0.042 Uiso 1 1 calc R U . . .
C20 C 0.76776(17) 0.21127(6) 0.05432(13) 0.0311(3) Uani 1 1 d . . . . .
H20 H 0.8239 0.1835 0.0667 0.037 Uiso 1 1 calc R U . . .
C21 C 0.72769(16) 0.23387(6) 0.12976(12) 0.0257(3) Uani 1 1 d . . . . .
H21 H 0.7574 0.2215 0.1928 0.031 Uiso 1 1 calc R U . . .
C22 C 0.64294(14) 0.27507(5) 0.11062(11) 0.0214(3) Uani 1 1 d . . . . .
C23 C 0.50314(15) 0.27077(5) 0.23265(11) 0.0226(3) Uani 1 1 d . . . . .
H23A H 0.5639 0.2479 0.2756 0.027 Uiso 1 1 calc R U . . .
H23B H 0.4622 0.2916 0.2727 0.027 Uiso 1 1 calc R U . . .
C24 C 0.39194(15) 0.24050(6) 0.16395(11) 0.0235(3) Uani 1 1 d . . . . .
H24A H 0.4308 0.2208 0.1209 0.028 Uiso 1 1 calc R U . . .
H24B H 0.3263 0.2630 0.1242 0.028 Uiso 1 1 calc R U . . .
C25 C 0.32091(17) 0.20578(6) 0.22027(12) 0.0289(3) Uani 1 1 d . . . . .
H25A H 0.2869 0.2260 0.2651 0.035 Uiso 1 1 calc R U . . .
H25B H 0.3882 0.1835 0.2591 0.035 Uiso 1 1 calc R U . . .
C27 C 0.48354(17) 0.43558(6) 0.19491(12) 0.0272(3) Uani 1 1 d . . . . .
H27A H 0.5302 0.4673 0.2066 0.033 Uiso 1 1 calc R U . . .
H27B H 0.4022 0.4405 0.1429 0.033 Uiso 1 1 calc R U . . .
C28 C 0.44295(17) 0.42069(6) 0.28673(13) 0.0299(3) Uani 1 1 d . . . . .
H28A H 0.5234 0.4136 0.3383 0.036 Uiso 1 1 calc R U . . .
H28B H 0.3892 0.3905 0.2741 0.036 Uiso 1 1 calc R U . . .
C29 C 0.36160(17) 0.46205(6) 0.32038(12) 0.0290(3) Uani 1 1 d . . . . .
H29A H 0.2767 0.4661 0.2714 0.035 Uiso 1 1 calc R U . . .
H29B H 0.4110 0.4931 0.3239 0.035 Uiso 1 1 calc R U . . .
C30 C 0.2223(3) 0.49866(9) 0.47764(18) 0.0500(5) Uani 1 1 d . . . . .
H30A H 0.2626 0.5309 0.4764 0.075 Uiso 1 1 calc R U . . .
H30B H 0.2173 0.4914 0.5426 0.075 Uiso 1 1 calc R U . . .
H30C H 0.1332 0.4986 0.4345 0.075 Uiso 1 1 calc R U . . .
Si3A Si 0.09646(10) 0.42044(3) -0.26058(7) 0.02883(19) Uani 0.5 1 d D . P A 1
F1A F 0.2278(5) 0.11092(17) 0.1594(7) 0.0785(18) Uani 0.83(2) 1 d . . P B 1
F2A F 0.0590(5) 0.16943(17) 0.1976(4) 0.0486(9) Uani 0.83(2) 1 d . . P B 1
F5A F 0.0087(4) 0.40137(13) -0.3631(2) 0.0586(10) Uani 0.5 1 d D . P A 1
F6A F 0.2033(12) 0.4630(3) -0.2673(9) 0.086(3) Uani 0.5 1 d D . P A 1
C26A C 0.1130(7) 0.1809(3) 0.0174(4) 0.0477(14) Uani 0.83(2) 1 d . . P B 1
H26A H 0.1837 0.1772 -0.0147 0.072 Uiso 0.83(2) 1 calc R U P B 1
H26B H 0.0793 0.2145 0.0091 0.072 Uiso 0.83(2) 1 calc R U P B 1
H26C H 0.0412 0.1582 -0.0104 0.072 Uiso 0.83(2) 1 calc R U P B 1
C31A C 0.3920(9) 0.3325(3) -0.0736(6) 0.0231(13) Uani 0.5 1 d . . P A 1
H31A H 0.4229 0.3214 -0.1289 0.028 Uiso 0.5 1 calc R U P A 1
H31B H 0.3378 0.3060 -0.0571 0.028 Uiso 0.5 1 calc R U P A 1
C32A C 0.3030(4) 0.37830(12) -0.1036(3) 0.0255(6) Uani 0.5 1 d . . P A 1
H32A H 0.3584 0.4068 -0.1092 0.031 Uiso 0.5 1 calc R U P A 1
H32B H 0.2559 0.3857 -0.0545 0.031 Uiso 0.5 1 calc R U P A 1
C33A C 0.2003(3) 0.36851(12) -0.2019(2) 0.0263(6) Uani 0.5 1 d . . P A 1
H33A H 0.1405 0.3421 -0.1923 0.032 Uiso 0.5 1 calc R U P A 1
H33B H 0.2493 0.3560 -0.2466 0.032 Uiso 0.5 1 calc R U P A 1
C34A C -0.0128(4) 0.44995(17) -0.1943(3) 0.0435(9) Uani 0.5 1 d . . P A 1
H34A H 0.0407 0.4614 -0.1324 0.065 Uiso 0.5 1 calc R U P A 1
H34B H -0.0584 0.4777 -0.2312 0.065 Uiso 0.5 1 calc R U P A 1
H34C H -0.0780 0.4262 -0.1846 0.065 Uiso 0.5 1 calc R U P A 1
Si3B Si 0.18801(11) 0.40509(4) -0.26860(7) 0.0317(2) Uani 0.5 1 d D . P A 2
F1B F 0.196(3) 0.1145(11) 0.1987(19) 0.074(8) Uani 0.17(2) 1 d . . P B 2
F2B F 0.0604(19) 0.188(2) 0.1961(18) 0.080(9) Uani 0.17(2) 1 d . . P B 2
F5B F 0.3276(2) 0.38260(11) -0.27958(17) 0.0497(6) Uani 0.5 1 d D . P A 2
F6B F 0.2010(9) 0.4617(3) -0.2818(8) 0.066(2) Uani 0.5 1 d D . P A 2
C26B C 0.135(3) 0.1686(9) 0.033(2) 0.037(5) Uani 0.17(2) 1 d . . P B 2
H26D H 0.1967 0.1493 0.0075 0.055 Uiso 0.17(2) 1 calc R U P B 2
H26E H 0.1345 0.2024 0.0106 0.055 Uiso 0.17(2) 1 calc R U P B 2
H26F H 0.0457 0.1549 0.0100 0.055 Uiso 0.17(2) 1 calc R U P B 2
C31B C 0.3684(9) 0.3386(4) -0.0577(7) 0.0247(13) Uani 0.5 1 d . . P A 2
H31C H 0.3766 0.3312 -0.1226 0.030 Uiso 0.5 1 calc R U P A 2
H31D H 0.3216 0.3108 -0.0377 0.030 Uiso 0.5 1 calc R U P A 2
C32B C 0.2796(3) 0.38500(14) -0.0641(3) 0.0250(6) Uani 0.5 1 d . . P A 2
H32C H 0.3332 0.4144 -0.0670 0.030 Uiso 0.5 1 calc R U P A 2
H32D H 0.2479 0.3873 -0.0058 0.030 Uiso 0.5 1 calc R U P A 2
C33B C 0.1568(3) 0.38394(14) -0.1542(2) 0.0298(7) Uani 0.5 1 d . . P A 2
H33C H 0.0863 0.4045 -0.1407 0.036 Uiso 0.5 1 calc R U P A 2
H33D H 0.1229 0.3501 -0.1632 0.036 Uiso 0.5 1 calc R U P A 2
C34B C 0.0569(5) 0.3909(2) -0.3769(4) 0.0387(10) Uani 0.5 1 d . . P A 2
H34D H 0.0374 0.3559 -0.3787 0.058 Uiso 0.5 1 calc R U P A 2
H34E H -0.0230 0.4094 -0.3765 0.058 Uiso 0.5 1 calc R U P A 2
H34F H 0.0864 0.3999 -0.4333 0.058 Uiso 0.5 1 calc R U P A 2
Sb1A Sb -0.05445(10) 0.35398(5) 0.12273(5) 0.04274(17) Uani 0.5 1 d D . P C 1
Cl1A Cl 0.1393(2) 0.31890(10) 0.22115(19) 0.0713(7) Uani 0.5 1 d D . P C 1
Cl2A Cl 0.0550(4) 0.42593(11) 0.1013(4) 0.0524(7) Uani 0.5 1 d D . P C 1
Cl3A Cl -0.0260(4) 0.32983(13) -0.0330(3) 0.0825(10) Uani 0.5 1 d D . P C 1
Sb1B Sb -0.07104(10) 0.35562(4) 0.09603(5) 0.04080(17) Uani 0.5 1 d D . P D 2
Cl1B Cl 0.0843(2) 0.30786(11) 0.21022(19) 0.0697(6) Uani 0.5 1 d D . P D 2
Cl2B Cl 0.0620(4) 0.43005(15) 0.1211(4) 0.0731(13) Uani 0.5 1 d D . P D 2
Cl3B Cl 0.0091(4) 0.31354(11) -0.0188(2) 0.0696(7) Uani 0.5 1 d D . P D 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
Si1 C25 1.8467(17) . ?
Si1 F1A 1.587(4) . ?
Si1 F2A 1.573(5) . ?
Si1 C26A 1.859(7) . ?
Si1 F1B 1.573(18) . ?
Si1 F2B 1.65(3) . ?
Si1 C26B 1.60(3) . ?
Si2 F3 1.5835(13) . ?
Si2 F4 1.5890(13) . ?
Si2 C29 1.8375(18) . ?
Si2 C30 1.833(2) . ?
C1 H1 0.9800 . ?
C1 C2 1.568(2) . ?
C1 C9 1.572(2) . ?
C1 C16 1.568(2) . ?
C2 C3 1.518(2) . ?
C2 C22 1.518(2) . ?
C2 C23 1.540(2) . ?
C3 C4 1.394(2) . ?
C3 C8 1.388(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.383(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.397(2) . ?
C8 C9 1.519(2) . ?
C9 C10 1.517(2) . ?
C9 C27 1.543(2) . ?
C10 C11 1.397(2) . ?
C10 C15 1.385(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.388(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(2) . ?
C15 C16 1.518(2) . ?
C16 C17 1.523(2) . ?
C16 C31A 1.533(10) . ?
C16 C31B 1.578(11) . ?
C17 C18 1.392(2) . ?
C17 C22 1.390(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.386(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.387(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.389(2) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.529(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.533(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.526(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.539(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
Si3A F5A 1.587(3) . ?
Si3A F6A 1.604(8) . ?
Si3A C33A 1.820(3) . ?
Si3A C34A 1.825(4) . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C31A C32A 1.524(9) . ?
C32A H32A 0.9700 . ?
C32A H32B 0.9700 . ?
C32A C33A 1.539(5) . ?
C33A H33A 0.9700 . ?
C33A H33B 0.9700 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
Si3B F5B 1.601(3) . ?
Si3B F6B 1.541(7) . ?
Si3B C33B 1.831(4) . ?
Si3B C34B 1.804(5) . ?
C26B H26D 0.9600 . ?
C26B H26E 0.9600 . ?
C26B H26F 0.9600 . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C31B C32B 1.532(9) . ?
C32B H32C 0.9700 . ?
C32B H32D 0.9700 . ?
C32B C33B 1.547(5) . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
Sb1A Cl1A 2.314(2) . ?
Sb1A Cl2A 2.295(4) . ?
Sb1A Cl3A 2.400(4) . ?
Sb1B Cl1B 2.341(2) . ?
Sb1B Cl2B 2.394(4) . ?
Sb1B Cl3B 2.310(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C25 Si1 C26A 118.4(2) . . ?
F1A Si1 C25 107.70(15) . . ?
F1A Si1 C26A 107.6(2) . . ?
F2A Si1 C25 109.7(2) . . ?
F2A Si1 F1A 104.7(3) . . ?
F2A Si1 C26A 107.9(3) . . ?
F1B Si1 C25 106.5(6) . . ?
F1B Si1 F2B 97.3(10) . . ?
F1B Si1 C26B 116.7(13) . . ?
F2B Si1 C25 98.5(13) . . ?
C26B Si1 C25 122.0(9) . . ?
C26B Si1 F2B 111.5(12) . . ?
F3 Si2 F4 103.66(8) . . ?
F3 Si2 C29 109.49(8) . . ?
F3 Si2 C30 108.92(10) . . ?
F4 Si2 C29 108.64(8) . . ?
F4 Si2 C30 109.22(10) . . ?
C30 Si2 C29 116.17(9) . . ?
C2 C1 H1 111.1 . . ?
C2 C1 C9 107.74(12) . . ?
C9 C1 H1 111.1 . . ?
C16 C1 H1 111.1 . . ?
C16 C1 C2 107.85(12) . . ?
C16 C1 C9 107.94(12) . . ?
C3 C2 C1 104.01(11) . . ?
C3 C2 C23 111.89(12) . . ?
C22 C2 C1 103.93(12) . . ?
C22 C2 C3 110.41(12) . . ?
C22 C2 C23 111.69(12) . . ?
C23 C2 C1 114.39(12) . . ?
C4 C3 C2 127.64(13) . . ?
C8 C3 C2 112.12(13) . . ?
C8 C3 C4 120.17(14) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.43(15) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.24(17) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.45(17) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C8 119.32(16) . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C7 120.39(15) . . ?
C3 C8 C9 112.28(13) . . ?
C7 C8 C9 127.31(14) . . ?
C8 C9 C1 103.82(12) . . ?
C8 C9 C27 111.70(13) . . ?
C10 C9 C1 103.66(13) . . ?
C10 C9 C8 111.02(12) . . ?
C10 C9 C27 111.14(12) . . ?
C27 C9 C1 115.05(12) . . ?
C11 C10 C9 127.65(15) . . ?
C15 C10 C9 112.29(13) . . ?
C15 C10 C11 120.05(15) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.30(16) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.38(16) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.50(17) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 120.4 . . ?
C15 C14 C13 119.27(17) . . ?
C15 C14 H14 120.4 . . ?
C10 C15 C14 120.49(15) . . ?
C10 C15 C16 112.38(14) . . ?
C14 C15 C16 127.13(15) . . ?
C1 C16 C31B 108.9(3) . . ?
C15 C16 C1 103.70(12) . . ?
C15 C16 C17 111.08(14) . . ?
C15 C16 C31A 109.9(4) . . ?
C15 C16 C31B 112.0(4) . . ?
C17 C16 C1 103.98(12) . . ?
C17 C16 C31A 105.0(3) . . ?
C17 C16 C31B 116.1(3) . . ?
C31A C16 C1 122.9(3) . . ?
C18 C17 C16 128.11(15) . . ?
C22 C17 C16 111.89(14) . . ?
C22 C17 C18 119.99(15) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.45(16) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.48(16) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.17(16) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.58(16) . . ?
C22 C21 H21 120.2 . . ?
C17 C22 C2 112.28(13) . . ?
C21 C22 C2 127.41(14) . . ?
C21 C22 C17 120.31(14) . . ?
C2 C23 H23A 108.5 . . ?
C2 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
C24 C23 C2 115.24(12) . . ?
C24 C23 H23A 108.5 . . ?
C24 C23 H23B 108.5 . . ?
C23 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C23 C24 C25 111.50(13) . . ?
H24A C24 H24B 108.0 . . ?
C25 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
Si1 C25 H25A 107.9 . . ?
Si1 C25 H25B 107.9 . . ?
C24 C25 Si1 117.65(11) . . ?
C24 C25 H25A 107.9 . . ?
C24 C25 H25B 107.9 . . ?
H25A C25 H25B 107.2 . . ?
C9 C27 H27A 108.4 . . ?
C9 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
C28 C27 C9 115.44(13) . . ?
C28 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
C27 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C27 C28 C29 111.74(13) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.3 . . ?
C29 C28 H28B 109.3 . . ?
Si2 C29 H29A 108.4 . . ?
Si2 C29 H29B 108.4 . . ?
C28 C29 Si2 115.33(11) . . ?
C28 C29 H29A 108.4 . . ?
C28 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
F5A Si3A F6A 114.0(5) . . ?
F5A Si3A C33A 107.44(16) . . ?
F5A Si3A C34A 109.7(2) . . ?
F6A Si3A C33A 104.2(5) . . ?
F6A Si3A C34A 104.2(4) . . ?
C33A Si3A C34A 117.43(19) . . ?
Si1 C26A H26A 109.5 . . ?
Si1 C26A H26B 109.5 . . ?
Si1 C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C16 C31A H31A 108.6 . . ?
C16 C31A H31B 108.6 . . ?
H31A C31A H31B 107.6 . . ?
C32A C31A C16 114.6(6) . . ?
C32A C31A H31A 108.6 . . ?
C32A C31A H31B 108.6 . . ?
C31A C32A H32A 109.7 . . ?
C31A C32A H32B 109.7 . . ?
C31A C32A C33A 109.6(4) . . ?
H32A C32A H32B 108.2 . . ?
C33A C32A H32A 109.7 . . ?
C33A C32A H32B 109.7 . . ?
Si3A C33A H33A 107.8 . . ?
Si3A C33A H33B 107.8 . . ?
C32A C33A Si3A 117.9(2) . . ?
C32A C33A H33A 107.8 . . ?
C32A C33A H33B 107.8 . . ?
H33A C33A H33B 107.2 . . ?
Si3A C34A H34A 109.5 . . ?
Si3A C34A H34B 109.5 . . ?
Si3A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
F5B Si3B C33B 109.87(15) . . ?
F5B Si3B C34B 108.94(19) . . ?
F6B Si3B F5B 104.5(3) . . ?
F6B Si3B C33B 117.1(4) . . ?
F6B Si3B C34B 100.0(5) . . ?
C34B Si3B C33B 115.5(2) . . ?
Si1 C26B H26D 109.5 . . ?
Si1 C26B H26E 109.5 . . ?
Si1 C26B H26F 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C16 C31B H31C 107.9 . . ?
C16 C31B H31D 107.9 . . ?
H31C C31B H31D 107.2 . . ?
C32B C31B C16 117.5(6) . . ?
C32B C31B H31C 107.9 . . ?
C32B C31B H31D 107.9 . . ?
C31B C32B H32C 109.2 . . ?
C31B C32B H32D 109.2 . . ?
C31B C32B C33B 112.2(5) . . ?
H32C C32B H32D 107.9 . . ?
C33B C32B H32C 109.2 . . ?
C33B C32B H32D 109.2 . . ?
Si3B C33B H33C 108.3 . . ?
Si3B C33B H33D 108.3 . . ?
C32B C33B Si3B 116.0(2) . . ?
C32B C33B H33C 108.3 . . ?
C32B C33B H33D 108.3 . . ?
H33C C33B H33D 107.4 . . ?
Si3B C34B H34D 109.5 . . ?
Si3B C34B H34E 109.5 . . ?
Si3B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
Cl1A Sb1A Cl3A 99.00(11) . . ?
Cl2A Sb1A Cl1A 92.80(12) . . ?
Cl2A Sb1A Cl3A 85.53(16) . . ?
Cl1B Sb1B Cl2B 95.40(14) . . ?
Cl3B Sb1B Cl1B 85.39(11) . . ?
Cl3B Sb1B Cl2B 102.60(16) . . ?

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
F3 Si2 C29 C28 -53.59(15) . . . . ?
F4 Si2 C29 C28 58.99(15) . . . . ?
C1 C2 C3 C4 -178.04(16) . . . . ?
C1 C2 C3 C8 -1.18(16) . . . . ?
C1 C2 C22 C17 -2.15(16) . . . . ?
C1 C2 C22 C21 177.44(14) . . . . ?
C1 C2 C23 C24 65.02(17) . . . . ?
C1 C9 C10 C11 179.65(15) . . . . ?
C1 C9 C10 C15 -1.70(17) . . . . ?
C1 C9 C27 C28 68.62(19) . . . . ?
C1 C16 C17 C18 179.59(15) . . . . ?
C1 C16 C17 C22 -1.98(16) . . . . ?
C1 C16 C31A C32A 72.3(6) . . . . ?
C1 C16 C31B C32B 63.4(7) . . . . ?
C2 C1 C9 C8 0.77(16) . . . . ?
C2 C1 C9 C10 116.87(13) . . . . ?
C2 C1 C9 C27 -121.59(14) . . . . ?
C2 C1 C16 C15 -115.67(13) . . . . ?
C2 C1 C16 C17 0.58(15) . . . . ?
C2 C1 C16 C31A 119.2(4) . . . . ?
C2 C1 C16 C31B 125.0(4) . . . . ?
C2 C3 C4 C5 176.25(17) . . . . ?
C2 C3 C8 C7 -177.13(15) . . . . ?
C2 C3 C8 C9 1.80(18) . . . . ?
C2 C23 C24 C25 176.11(13) . . . . ?
C3 C2 C22 C17 -113.16(14) . . . . ?
C3 C2 C22 C21 66.43(19) . . . . ?
C3 C2 C23 C24 -177.03(12) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C3 C8 C9 C1 -1.57(17) . . . . ?
C3 C8 C9 C10 -112.36(15) . . . . ?
C3 C8 C9 C27 122.98(14) . . . . ?
C4 C3 C8 C7 0.0(2) . . . . ?
C4 C3 C8 C9 178.92(14) . . . . ?
C4 C5 C6 C7 -0.5(3) . . . . ?
C5 C6 C7 C8 0.1(3) . . . . ?
C6 C7 C8 C3 0.1(3) . . . . ?
C6 C7 C8 C9 -178.61(18) . . . . ?
C7 C8 C9 C1 177.27(17) . . . . ?
C7 C8 C9 C10 66.5(2) . . . . ?
C7 C8 C9 C27 -58.2(2) . . . . ?
C8 C3 C4 C5 -0.4(3) . . . . ?
C8 C9 C10 C11 -69.5(2) . . . . ?
C8 C9 C10 C15 109.20(15) . . . . ?
C8 C9 C27 C28 -49.39(18) . . . . ?
C9 C1 C2 C3 0.17(15) . . . . ?
C9 C1 C2 C22 -115.44(13) . . . . ?
C9 C1 C2 C23 122.52(13) . . . . ?
C9 C1 C16 C15 0.49(16) . . . . ?
C9 C1 C16 C17 116.73(13) . . . . ?
C9 C1 C16 C31A -124.6(4) . . . . ?
C9 C1 C16 C31B -118.9(4) . . . . ?
C9 C10 C11 C12 177.67(16) . . . . ?
C9 C10 C15 C14 -178.71(15) . . . . ?
C9 C10 C15 C16 2.17(19) . . . . ?
C9 C27 C28 C29 175.68(14) . . . . ?
C10 C9 C27 C28 -173.99(14) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C10 C15 C16 C1 -1.61(18) . . . . ?
C10 C15 C16 C17 -112.74(16) . . . . ?
C10 C15 C16 C31A 131.5(3) . . . . ?
C10 C15 C16 C31B 115.7(3) . . . . ?
C11 C10 C15 C14 0.1(2) . . . . ?
C11 C10 C15 C16 -179.06(14) . . . . ?
C11 C12 C13 C14 -0.2(3) . . . . ?
C12 C13 C14 C15 -0.6(3) . . . . ?
C13 C14 C15 C10 0.7(3) . . . . ?
C13 C14 C15 C16 179.68(17) . . . . ?
C14 C15 C16 C1 179.34(17) . . . . ?
C14 C15 C16 C17 68.2(2) . . . . ?
C14 C15 C16 C31A -47.5(3) . . . . ?
C14 C15 C16 C31B -63.4(3) . . . . ?
C15 C10 C11 C12 -0.9(2) . . . . ?
C15 C16 C17 C18 -69.5(2) . . . . ?
C15 C16 C17 C22 108.97(15) . . . . ?
C15 C16 C31A C32A -50.1(5) . . . . ?
C15 C16 C31B C32B -50.7(6) . . . . ?
C16 C1 C2 C3 116.45(12) . . . . ?
C16 C1 C2 C22 0.84(15) . . . . ?
C16 C1 C2 C23 -121.20(13) . . . . ?
C16 C1 C9 C8 -115.46(13) . . . . ?
C16 C1 C9 C10 0.64(15) . . . . ?
C16 C1 C9 C27 122.19(14) . . . . ?
C16 C17 C18 C19 177.55(16) . . . . ?
C16 C17 C22 C2 2.70(17) . . . . ?
C16 C17 C22 C21 -176.93(14) . . . . ?
C16 C31A C32A C33A 168.9(4) . . . . ?
C16 C31B C32B C33B 164.0(5) . . . . ?
C17 C16 C31A C32A -169.6(4) . . . . ?
C17 C16 C31B C32B -179.7(4) . . . . ?
C17 C18 C19 C20 -0.2(3) . . . . ?
C18 C17 C22 C2 -178.73(14) . . . . ?
C18 C17 C22 C21 1.6(2) . . . . ?
C18 C19 C20 C21 0.4(3) . . . . ?
C19 C20 C21 C22 0.5(2) . . . . ?
C20 C21 C22 C2 178.93(14) . . . . ?
C20 C21 C22 C17 -1.5(2) . . . . ?
C22 C2 C3 C4 -67.1(2) . . . . ?
C22 C2 C3 C8 109.78(14) . . . . ?
C22 C2 C23 C24 -52.67(17) . . . . ?
C22 C17 C18 C19 -0.8(2) . . . . ?
C23 C2 C3 C4 58.0(2) . . . . ?
C23 C2 C3 C8 -125.16(14) . . . . ?
C23 C2 C22 C17 121.66(14) . . . . ?
C23 C2 C22 C21 -58.7(2) . . . . ?
C23 C24 C25 Si1 178.40(11) . . . . ?
C27 C9 C10 C11 55.5(2) . . . . ?
C27 C9 C10 C15 -125.83(15) . . . . ?
C27 C28 C29 Si2 -172.84(12) . . . . ?
C30 Si2 C29 C28 -177.45(14) . . . . ?
F1A Si1 C25 C24 111.5(4) . . . . ?
F2A Si1 C25 C24 -135.13(19) . . . . ?
F5A Si3A C33A C32A 175.8(3) . . . . ?
F6A Si3A C33A C32A 54.5(5) . . . . ?
C26A Si1 C25 C24 -10.8(3) . . . . ?
C31A C16 C17 C18 49.3(4) . . . . ?
C31A C16 C17 C22 -132.3(3) . . . . ?
C31A C16 C31B C32B -136(3) . . . . ?
C31A C32A C33A Si3A -172.4(4) . . . . ?
C34A Si3A C33A C32A -60.1(4) . . . . ?
F1B Si1 C25 C24 139.2(18) . . . . ?
F2B Si1 C25 C24 -120.5(17) . . . . ?
F5B Si3B C33B C32B 43.1(3) . . . . ?
F6B Si3B C33B C32B -75.9(5) . . . . ?
C26B Si1 C25 C24 1.6(11) . . . . ?
C31B C16 C17 C18 60.0(4) . . . . ?
C31B C16 C17 C22 -121.6(4) . . . . ?
C31B C16 C31A C32A 51(2) . . . . ?
C31B C32B C33B Si3B -83.0(5) . . . . ?
C34B Si3B C33B C32B 166.7(3) . . . . ?

_olex2_date_sample_data_collection 2016-05-03
_olex2_date_sample_submission    1461189600
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.539
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound18
_database_code_depnum_ccdc_archive 'CCDC 1514279'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2015-04-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H28'
_chemical_formula_sum            'C46 H28'
_chemical_formula_weight         580.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H48'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'

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

_cell_length_a                   23.7889(10)
_cell_length_b                   10.4654(4)
_cell_length_c                   27.3953(16)
_cell_angle_alpha                90
_cell_angle_beta                 107.901(5)
_cell_angle_gamma                90
_cell_volume                     6490.2(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.0450
_cell_measurement_theta_min      3.3450
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.0211
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28358
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         75.46
_diffrn_reflns_theta_min         2.95
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9672
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega -114.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega   -7.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 40

#__ type_ start__ end____ width___ exp.time_
  4 omega   57.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   43.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -30.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
  6 omega   41.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -45.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
  7 omega   65.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -45.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
  8 omega   87.00  173.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343   45.0000  -30.0000 86

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   74.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -30.0000  150.0000 36

#__ type_ start__ end____ width___ exp.time_
 10 omega   63.00  133.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -77.0000  -90.0000 70

#__ type_ start__ end____ width___ exp.time_
 11 omega   94.00  176.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  125.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 12 omega   40.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343 -125.0000  120.0000 73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0436630000
_diffrn_orient_matrix_UB_12      -0.1127231000
_diffrn_orient_matrix_UB_13      -0.0143006000
_diffrn_orient_matrix_UB_21      -0.0450740000
_diffrn_orient_matrix_UB_22      0.0768781000
_diffrn_orient_matrix_UB_23      0.0182109000
_diffrn_orient_matrix_UB_31      -0.0263547000
_diffrn_orient_matrix_UB_32      0.0553874000
_diffrn_orient_matrix_UB_33      -0.0543382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          Squeezed
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7493
_reflns_number_total             11464
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         11464
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0711
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1235P)²+0.2845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2171
_refine_special_details          
;Crystal contains highly disordered solvent, which was squeezed using Olex2.
Total solvent accessible volume / cell = 537.7 Ang^3, i.e. 8.3% of cell volume., SQUEEZE
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.38960(12) -0.0031(3) 0.84829(11) 0.0406(6) Uani 1 1 d . . . . .
H1 H 0.3523 -0.0224 0.8217 0.049 Uiso 1 1 calc R . . . .
C2 C 0.43328(12) 0.0695(3) 0.82461(12) 0.0434(7) Uani 1 1 d . . . . .
C3 C 0.48860(13) -0.0142(3) 0.83993(12) 0.0470(7) Uani 1 1 d . . . . .
C4 C 0.54261(14) 0.0113(3) 0.83168(14) 0.0556(8) Uani 1 1 d . . . . .
H4 H 0.5470 0.0825 0.8129 0.067 Uiso 1 1 calc R . . . .
C5 C 0.58949(14) -0.0710(3) 0.85192(17) 0.0655(10) Uani 1 1 d . . . . .
H5 H 0.6256 -0.0546 0.8467 0.079 Uiso 1 1 calc R . . . .
C6 C 0.58329(15) -0.1793(3) 0.88041(18) 0.0697(11) Uani 1 1 d . . . . .
H6 H 0.6153 -0.2330 0.8946 0.084 Uiso 1 1 calc R . . . .
C7 C 0.52886(14) -0.2050(3) 0.88699(16) 0.0617(9) Uani 1 1 d . . . . .
H7 H 0.5239 -0.2775 0.9049 0.074 Uiso 1 1 calc R . . . .
C8 C 0.48147(13) -0.1219(3) 0.86678(13) 0.0482(7) Uani 1 1 d . . . . .
C9 C 0.42082(12) -0.1301(3) 0.87422(12) 0.0431(7) Uani 1 1 d . . . . .
C10 C 0.42514(12) -0.1131(3) 0.92976(12) 0.0435(7) Uani 1 1 d . . . . .
C11 C 0.44755(14) -0.2004(3) 0.96990(13) 0.0530(8) Uani 1 1 d . . . . .
H11 H 0.4617 -0.2797 0.9637 0.064 Uiso 1 1 calc R . . . .
C12 C 0.44823(13) -0.1667(3) 1.01874(13) 0.0548(9) Uani 1 1 d . . . . .
H12 H 0.4628 -0.2243 1.0455 0.066 Uiso 1 1 calc R . . . .
C13 C 0.42799(13) -0.0502(3) 1.02860(13) 0.0546(8) Uani 1 1 d . . . . .
H13 H 0.4289 -0.0293 1.0618 0.065 Uiso 1 1 calc R . . . .
C14 C 0.40607(13) 0.0367(3) 0.98914(12) 0.0480(7) Uani 1 1 d . . . . .
H14 H 0.3926 0.1163 0.9958 0.058 Uiso 1 1 calc R . . . .
C15 C 0.40436(12) 0.0043(3) 0.93948(11) 0.0420(6) Uani 1 1 d . . . . .
C16 C 0.37860(12) 0.0827(3) 0.89115(11) 0.0408(6) Uani 1 1 d . . . . .
C17 C 0.41424(12) 0.2028(3) 0.88954(11) 0.0421(6) Uani 1 1 d . . . . .
C18 C 0.41942(14) 0.3124(3) 0.91962(13) 0.0500(7) Uani 1 1 d . . . . .
H18 H 0.3997 0.3178 0.9440 0.060 Uiso 1 1 calc R . . . .
C19 C 0.45420(15) 0.4132(3) 0.91294(15) 0.0580(9) Uani 1 1 d . . . . .
H19 H 0.4579 0.4862 0.9331 0.070 Uiso 1 1 calc R . . . .
C20 C 0.48347(14) 0.4057(3) 0.87633(13) 0.0526(8) Uani 1 1 d . . . . .
H20 H 0.5060 0.4743 0.8714 0.063 Uiso 1 1 calc R . . . .
C21 C 0.47912(13) 0.2962(3) 0.84709(13) 0.0491(7) Uani 1 1 d . . . . .
H21 H 0.4994 0.2902 0.8231 0.059 Uiso 1 1 calc R . . . .
C22 C 0.44421(12) 0.1952(3) 0.85387(11) 0.0410(6) Uani 1 1 d . . . . .
C23 C 0.40722(13) 0.0906(3) 0.76667(12) 0.0459(7) Uani 1 1 d . . . . .
C24 C 0.41821(15) 0.0098(3) 0.73052(13) 0.0551(8) Uani 1 1 d . . . . .
H24 H 0.4439 -0.0587 0.7415 0.066 Uiso 1 1 calc R . . . .
C25 C 0.39162(16) 0.0289(4) 0.67836(14) 0.0599(9) Uani 1 1 d . . . . .
H25 H 0.3991 -0.0273 0.6548 0.072 Uiso 1 1 calc R . . . .
C26 C 0.35397(15) 0.1315(4) 0.66139(13) 0.0574(8) Uani 1 1 d . . . . .
C27 C 0.34236(16) 0.2125(4) 0.69694(13) 0.0604(9) Uani 1 1 d . . . . .
H27 H 0.3169 0.2813 0.6859 0.072 Uiso 1 1 calc R . . . .
C28 C 0.36822(14) 0.1922(3) 0.74865(13) 0.0541(8) Uani 1 1 d . . . . .
H28 H 0.3596 0.2471 0.7720 0.065 Uiso 1 1 calc R . . . .
C29 C 0.32630(18) 0.1562(4) 0.60488(18) 0.0688(10) Uani 1 1 d D . . . .
C30 C 0.3054(3) 0.1786(5) 0.5662(2) 0.0925(15) Uani 1 1 d D . . . .
H30 H 0.2868 0.1985 0.5319 0.111 Uiso 1 1 calc R . . . .
C31 C 0.38629(12) -0.2487(3) 0.84916(12) 0.0422(7) Uani 1 1 d . . . . .
C32 C 0.34536(12) -0.3078(3) 0.86895(12) 0.0440(7) Uani 1 1 d . . . . .
H32 H 0.3421 -0.2812 0.9004 0.053 Uiso 1 1 calc R . . . .
C33 C 0.30955(12) -0.4054(3) 0.84244(12) 0.0450(7) Uani 1 1 d . . . . .
H33 H 0.2822 -0.4430 0.8560 0.054 Uiso 1 1 calc R . . . .
C34 C 0.31425(12) -0.4479(3) 0.79563(12) 0.0436(7) Uani 1 1 d . . . . .
C35 C 0.35633(14) -0.3928(3) 0.77624(13) 0.0501(7) Uani 1 1 d . . . . .
H35 H 0.3608 -0.4221 0.7456 0.060 Uiso 1 1 calc R . . . .
C36 C 0.39160(13) -0.2937(3) 0.80293(13) 0.0500(7) Uani 1 1 d . . . . .
H36 H 0.4193 -0.2567 0.7896 0.060 Uiso 1 1 calc R . . . .
C37 C 0.27305(15) -0.5478(3) 0.76592(12) 0.0466(7) Uani 1 1 d D . . . .
C38 C 0.24518(15) -0.6224(4) 0.74515(14) 0.0592(9) Uani 1 1 d D . . . .
H38 H 0.2209 -0.6874 0.7271 0.071 Uiso 1 1 calc R . . . .
C39 C 0.31260(12) 0.1082(3) 0.88315(11) 0.0413(6) Uani 1 1 d . . . . .
C40 C 0.27823(13) 0.0160(3) 0.89727(13) 0.0503(7) Uani 1 1 d . . . . .
H40 H 0.2956 -0.0602 0.9118 0.060 Uiso 1 1 calc R . . . .
C41 C 0.21911(14) 0.0359(3) 0.89014(13) 0.0537(8) Uani 1 1 d . . . . .
H41 H 0.1967 -0.0278 0.8989 0.064 Uiso 1 1 calc R . . . .
C42 C 0.19261(13) 0.1511(3) 0.86979(12) 0.0504(7) Uani 1 1 d . . . . .
C43 C 0.22645(14) 0.2422(3) 0.85511(14) 0.0563(8) Uani 1 1 d . . . . .
H43 H 0.2092 0.3187 0.8407 0.068 Uiso 1 1 calc R . . . .
C44 C 0.28553(14) 0.2206(3) 0.86169(13) 0.0509(7) Uani 1 1 d . . . . .
H44 H 0.3075 0.2827 0.8515 0.061 Uiso 1 1 calc R . . . .
C45 C 0.1264(2) 0.1731(4) 0.86211(16) 0.0613(9) Uani 1 1 d D . . . .
C46 C 0.0849(3) 0.1882(5) 0.8570(2) 0.1044(19) Uani 1 1 d D . . . .
H46 H 0.0449 0.2027 0.8521 0.125 Uiso 1 1 calc R . . . .
C47 C 0.27895(13) 0.1014(3) 0.39324(12) 0.0442(7) Uani 1 1 d . . . . .
H47 H 0.2735 0.0836 0.3570 0.053 Uiso 1 1 calc R . . . .
C48 C 0.33477(13) 0.1893(3) 0.41658(12) 0.0447(7) Uani 1 1 d . . . . .
C49 C 0.30934(14) 0.3053(3) 0.43579(12) 0.0471(7) Uani 1 1 d . . . . .
C50 C 0.33957(17) 0.4121(3) 0.46123(14) 0.0597(9) Uani 1 1 d . . . . .
H50 H 0.3801 0.4190 0.4674 0.072 Uiso 1 1 calc R . . . .
C51 C 0.30920(18) 0.5078(4) 0.47729(16) 0.0674(10) Uani 1 1 d . . . . .
H51 H 0.3295 0.5786 0.4945 0.081 Uiso 1 1 calc R . . . .
C52 C 0.24831(17) 0.4987(3) 0.46771(15) 0.0626(9) Uani 1 1 d . . . . .
H52 H 0.2279 0.5638 0.4781 0.075 Uiso 1 1 calc R . . . .
C53 C 0.21826(15) 0.3925(3) 0.44274(12) 0.0524(8) Uani 1 1 d . . . . .
H53 H 0.1777 0.3855 0.4367 0.063 Uiso 1 1 calc R . . . .
C54 C 0.24887(13) 0.2965(3) 0.42678(11) 0.0446(7) Uani 1 1 d . . . . .
C55 C 0.22329(13) 0.1728(3) 0.39995(12) 0.0458(7) Uani 1 1 d . . . . .
C56 C 0.20365(15) 0.0852(3) 0.43605(13) 0.0519(7) Uani 1 1 d . . . . .
C57 C 0.15679(17) 0.1047(4) 0.45589(16) 0.0640(9) Uani 1 1 d . . . . .
H57 H 0.1319 0.1747 0.4455 0.077 Uiso 1 1 calc R . . . .
C58 C 0.1478(2) 0.0186(4) 0.49108(18) 0.0771(12) Uani 1 1 d . . . . .
H58 H 0.1166 0.0306 0.5044 0.093 Uiso 1 1 calc R . . . .
C59 C 0.1857(2) -0.0872(4) 0.50688(18) 0.0804(12) Uani 1 1 d . . . . .
H59 H 0.1801 -0.1433 0.5313 0.097 Uiso 1 1 calc R . . . .
C60 C 0.23082(18) -0.1076(4) 0.48624(16) 0.0657(10) Uani 1 1 d . . . . .
H60 H 0.2551 -0.1787 0.4959 0.079 Uiso 1 1 calc R . . . .
C61 C 0.23978(15) -0.0210(3) 0.45087(13) 0.0514(7) Uani 1 1 d . . . . .
C62 C 0.28828(14) -0.0262(3) 0.42515(13) 0.0487(7) Uani 1 1 d . . . . .
C63 C 0.34892(14) -0.0089(3) 0.46509(12) 0.0483(7) Uani 1 1 d . . . . .
C64 C 0.37885(16) -0.0930(3) 0.50355(13) 0.0580(8) Uani 1 1 d . . . . .
H64 H 0.3627 -0.1725 0.5065 0.070 Uiso 1 1 calc R . . . .
C65 C 0.43256(17) -0.0579(4) 0.53723(14) 0.0648(10) Uani 1 1 d . . . . .
H65 H 0.4525 -0.1141 0.5631 0.078 Uiso 1 1 calc R . . . .
C66 C 0.45730(17) 0.0600(4) 0.53317(14) 0.0657(10) Uani 1 1 d . . . . .
H66 H 0.4935 0.0827 0.5563 0.079 Uiso 1 1 calc R . . . .
C67 C 0.42789(15) 0.1442(4) 0.49452(13) 0.0576(8) Uani 1 1 d . . . . .
H67 H 0.4444 0.2232 0.4914 0.069 Uiso 1 1 calc R . . . .
C68 C 0.37348(14) 0.1088(3) 0.46052(12) 0.0476(7) Uani 1 1 d . . . . .
C69 C 0.36596(12) 0.2198(3) 0.37690(12) 0.0444(7) Uani 1 1 d . . . . .
C70 C 0.40132(14) 0.1283(3) 0.36424(13) 0.0520(7) Uani 1 1 d . . . . .
H70 H 0.4075 0.0507 0.3816 0.062 Uiso 1 1 calc R . . . .
C71 C 0.42753(15) 0.1498(3) 0.32644(14) 0.0557(8) Uani 1 1 d . . . . .
H71 H 0.4509 0.0869 0.3184 0.067 Uiso 1 1 calc R . . . .
C72 C 0.41878(14) 0.2660(3) 0.30045(12) 0.0514(8) Uani 1 1 d . . . . .
C73 C 0.38352(15) 0.3572(4) 0.31242(15) 0.0594(9) Uani 1 1 d . . . . .
H73 H 0.3771 0.4345 0.2948 0.071 Uiso 1 1 calc R . . . .
C74 C 0.35766(15) 0.3349(3) 0.35024(14) 0.0575(8) Uani 1 1 d . . . . .
H74 H 0.3342 0.3980 0.3581 0.069 Uiso 1 1 calc R . . . .
C75 C 0.44817(19) 0.2917(4) 0.25907(19) 0.0629(10) Uani 1 1 d D . . . .
C76 C 0.4676(2) 0.3115(6) 0.2338(2) 0.0938(17) Uani 1 1 d D . . . .
H76 H 0.4864 0.3305 0.2095 0.113 Uiso 1 1 calc R . . . .
C77 C 0.17627(13) 0.1961(3) 0.34845(12) 0.0472(7) Uani 1 1 d . . . . .
C78 C 0.18106(14) 0.3004(3) 0.31797(12) 0.0502(7) Uani 1 1 d . . . . .
H78 H 0.2127 0.3563 0.3301 0.060 Uiso 1 1 calc R . . . .
C79 C 0.14023(15) 0.3234(4) 0.27027(14) 0.0576(8) Uani 1 1 d . . . . .
H79 H 0.1449 0.3934 0.2510 0.069 Uiso 1 1 calc R . . . .
C80 C 0.09228(15) 0.2417(4) 0.25135(13) 0.0553(8) Uani 1 1 d . . . . .
C81 C 0.08740(14) 0.1366(4) 0.28052(14) 0.0595(9) Uani 1 1 d . . . . .
H81 H 0.0562 0.0798 0.2679 0.071 Uiso 1 1 calc R . . . .
C82 C 0.12847(14) 0.1144(3) 0.32862(14) 0.0524(8) Uani 1 1 d . . . . .
H82 H 0.1238 0.0439 0.3477 0.063 Uiso 1 1 calc R . . . .
C83 C 0.04491(16) 0.2688(4) 0.20080(16) 0.0607(9) Uani 1 1 d D . . . .
C84 C 0.0118(2) 0.2892(5) 0.1661(2) 0.0934(14) Uani 1 1 d D . . . .
H84 H -0.0174 0.3072 0.1354 0.112 Uiso 1 1 calc R . . . .
C85 C 0.28250(13) -0.1416(3) 0.39051(12) 0.0460(7) Uani 1 1 d . . . . .
C86 C 0.22596(14) -0.1837(3) 0.36133(14) 0.0549(8) Uani 1 1 d . . . . .
H86 H 0.1928 -0.1478 0.3672 0.066 Uiso 1 1 calc R . . . .
C87 C 0.21852(14) -0.2765(3) 0.32443(14) 0.0554(8) Uani 1 1 d . . . . .
H87 H 0.1806 -0.3014 0.3054 0.066 Uiso 1 1 calc R . . . .
C88 C 0.26721(14) -0.3338(3) 0.31516(12) 0.0476(7) Uani 1 1 d . . . . .
C89 C 0.32347(14) -0.2956(3) 0.34478(13) 0.0487(7) Uani 1 1 d . . . . .
H89 H 0.3565 -0.3338 0.3396 0.058 Uiso 1 1 calc R . . . .
C90 C 0.33090(14) -0.2015(3) 0.38172(13) 0.0494(7) Uani 1 1 d . . . . .
H90 H 0.3689 -0.1777 0.4011 0.059 Uiso 1 1 calc R . . . .
C91 C 0.25869(14) -0.4300(3) 0.27307(16) 0.0527(8) Uani 1 1 d D . . . .
C92 C 0.25248(17) -0.4999(4) 0.24500(15) 0.0624(9) Uani 1 1 d D . . . .
H92 H 0.2469 -0.5624 0.2199 0.075 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.579(4) . ?
C1 C9 1.581(4) . ?
C1 C16 1.563(4) . ?
C2 C3 1.528(4) . ?
C2 C22 1.521(4) . ?
C2 C23 1.532(4) . ?
C3 C4 1.397(5) . ?
C3 C8 1.384(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.410(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.396(4) . ?
C8 C9 1.520(4) . ?
C9 C10 1.504(5) . ?
C9 C31 1.530(4) . ?
C10 C11 1.403(4) . ?
C10 C15 1.381(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.379(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.386(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.390(4) . ?
C15 C16 1.518(4) . ?
C16 C17 1.524(4) . ?
C16 C39 1.540(4) . ?
C17 C18 1.395(4) . ?
C17 C22 1.377(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.384(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.391(4) . ?
C23 C24 1.388(5) . ?
C23 C28 1.397(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.388(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.384(5) . ?
C26 C27 1.382(5) . ?
C26 C29 1.507(6) . ?
C27 H27 0.9300 . ?
C27 C28 1.376(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.050(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.396(4) . ?
C31 C36 1.393(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.385(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.394(5) . ?
C34 C35 1.394(5) . ?
C34 C37 1.492(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.392(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.068(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.394(4) . ?
C39 C44 1.382(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.375(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.395(5) . ?
C42 C43 1.385(5) . ?
C42 C45 1.541(5) . ?
C43 H43 0.9300 . ?
C43 C44 1.380(5) . ?
C44 H44 0.9300 . ?
C45 C46 0.967(6) . ?
C46 H46 0.9300 . ?
C47 H47 0.9800 . ?
C47 C48 1.580(4) . ?
C47 C55 1.579(4) . ?
C47 C62 1.574(4) . ?
C48 C49 1.521(4) . ?
C48 C68 1.524(4) . ?
C48 C69 1.526(5) . ?
C49 C50 1.395(5) . ?
C49 C54 1.386(4) . ?
C50 H50 0.9300 . ?
C50 C51 1.383(5) . ?
C51 H51 0.9300 . ?
C51 C52 1.394(6) . ?
C52 H52 0.9300 . ?
C52 C53 1.383(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.388(4) . ?
C54 C55 1.520(4) . ?
C55 C56 1.523(5) . ?
C55 C77 1.527(4) . ?
C56 C57 1.397(5) . ?
C56 C61 1.387(5) . ?
C57 H57 0.9300 . ?
C57 C58 1.383(5) . ?
C58 H58 0.9300 . ?
C58 C59 1.409(6) . ?
C59 H59 0.9300 . ?
C59 C60 1.376(6) . ?
C60 H60 0.9300 . ?
C60 C61 1.390(5) . ?
C61 C62 1.527(5) . ?
C62 C63 1.530(5) . ?
C62 C85 1.516(5) . ?
C63 C64 1.390(5) . ?
C63 C68 1.386(5) . ?
C64 H64 0.9300 . ?
C64 C65 1.376(5) . ?
C65 H65 0.9300 . ?
C65 C66 1.386(6) . ?
C66 H66 0.9300 . ?
C66 C67 1.390(5) . ?
C67 H67 0.9300 . ?
C67 C68 1.392(5) . ?
C69 C70 1.387(4) . ?
C69 C74 1.392(5) . ?
C70 H70 0.9300 . ?
C70 C71 1.382(5) . ?
C71 H71 0.9300 . ?
C71 C72 1.392(5) . ?
C72 C73 1.375(5) . ?
C72 C75 1.528(6) . ?
C73 H73 0.9300 . ?
C73 C74 1.378(5) . ?
C74 H74 0.9300 . ?
C75 C76 0.965(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.401(5) . ?
C77 C82 1.392(5) . ?
C78 H78 0.9300 . ?
C78 C79 1.389(5) . ?
C79 H79 0.9300 . ?
C79 C80 1.392(5) . ?
C80 C81 1.385(5) . ?
C80 C83 1.520(5) . ?
C81 H81 0.9300 . ?
C81 C82 1.398(5) . ?
C82 H82 0.9300 . ?
C83 C84 1.054(6) . ?
C84 H84 0.9300 . ?
C85 C86 1.408(5) . ?
C85 C90 1.396(4) . ?
C86 H86 0.9300 . ?
C86 C87 1.374(5) . ?
C87 H87 0.9300 . ?
C87 C88 1.395(5) . ?
C88 C89 1.394(4) . ?
C88 C91 1.497(5) . ?
C89 H89 0.9300 . ?
C89 C90 1.384(5) . ?
C90 H90 0.9300 . ?
C91 C92 1.038(5) . ?
C92 H92 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 110.7 . . ?
C2 C1 C9 108.2(2) . . ?
C9 C1 H1 110.7 . . ?
C16 C1 H1 110.7 . . ?
C16 C1 C2 108.4(2) . . ?
C16 C1 C9 108.0(2) . . ?
C3 C2 C1 103.4(2) . . ?
C3 C2 C23 114.0(3) . . ?
C22 C2 C1 103.1(2) . . ?
C22 C2 C3 111.0(2) . . ?
C22 C2 C23 111.7(2) . . ?
C23 C2 C1 112.8(2) . . ?
C4 C3 C2 127.1(3) . . ?
C8 C3 C2 112.1(3) . . ?
C8 C3 C4 120.7(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C3 C8 C7 120.1(3) . . ?
C3 C8 C9 113.2(3) . . ?
C7 C8 C9 126.6(3) . . ?
C8 C9 C1 103.1(2) . . ?
C8 C9 C31 112.7(3) . . ?
C10 C9 C1 103.4(2) . . ?
C10 C9 C8 110.9(2) . . ?
C10 C9 C31 114.2(2) . . ?
C31 C9 C1 111.6(2) . . ?
C11 C10 C9 127.4(3) . . ?
C15 C10 C9 112.5(2) . . ?
C15 C10 C11 120.0(3) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 C10 118.8(3) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.3(3) . . ?
C13 C12 H12 119.3 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.6(3) . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C14 120.1(3) . . ?
C10 C15 C16 112.7(3) . . ?
C14 C15 C16 127.1(3) . . ?
C15 C16 C1 103.2(2) . . ?
C15 C16 C17 113.1(2) . . ?
C15 C16 C39 109.8(2) . . ?
C17 C16 C1 103.2(2) . . ?
C17 C16 C39 113.9(2) . . ?
C39 C16 C1 113.0(2) . . ?
C18 C17 C16 127.5(3) . . ?
C22 C17 C16 112.8(3) . . ?
C22 C17 C18 119.7(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.3(3) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.6(3) . . ?
C22 C21 H21 120.2 . . ?
C17 C22 C2 112.5(3) . . ?
C17 C22 C21 120.7(3) . . ?
C21 C22 C2 126.8(3) . . ?
C24 C23 C2 123.1(3) . . ?
C24 C23 C28 117.5(3) . . ?
C28 C23 C2 119.3(3) . . ?
C23 C24 H24 119.3 . . ?
C23 C24 C25 121.4(3) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C29 120.7(3) . . ?
C27 C26 C25 119.2(3) . . ?
C27 C26 C29 120.0(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 H27 119.8 . . ?
C23 C28 H28 119.3 . . ?
C27 C28 C23 121.3(3) . . ?
C27 C28 H28 119.3 . . ?
C30 C29 C26 176.0(5) . . ?
C29 C30 H30 180.0 . . ?
C32 C31 C9 121.8(3) . . ?
C36 C31 C9 119.7(3) . . ?
C36 C31 C32 118.2(3) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 C31 120.9(3) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.5(3) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C35 119.3(3) . . ?
C33 C34 C37 120.0(3) . . ?
C35 C34 C37 120.7(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.7(3) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 H36 119.3 . . ?
C35 C36 C31 121.4(3) . . ?
C35 C36 H36 119.3 . . ?
C38 C37 C34 177.4(3) . . ?
C37 C38 H38 180.0 . . ?
C40 C39 C16 120.0(3) . . ?
C44 C39 C16 122.0(3) . . ?
C44 C39 C40 118.1(3) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 C39 121.2(3) . . ?
C41 C40 H40 119.4 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C42 120.3(3) . . ?
C42 C41 H41 119.9 . . ?
C41 C42 C45 120.1(3) . . ?
C43 C42 C41 118.7(3) . . ?
C43 C42 C45 121.2(3) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 C42 120.6(3) . . ?
C44 C43 H43 119.7 . . ?
C39 C44 H44 119.4 . . ?
C43 C44 C39 121.2(3) . . ?
C43 C44 H44 119.4 . . ?
C46 C45 C42 179.1(6) . . ?
C45 C46 H46 180.0 . . ?
C48 C47 H47 110.7 . . ?
C55 C47 H47 110.7 . . ?
C55 C47 C48 108.0(2) . . ?
C62 C47 H47 110.7 . . ?
C62 C47 C48 108.1(2) . . ?
C62 C47 C55 108.5(2) . . ?
C49 C48 C47 103.3(2) . . ?
C49 C48 C68 112.1(3) . . ?
C49 C48 C69 114.3(3) . . ?
C68 C48 C47 103.1(2) . . ?
C68 C48 C69 111.7(2) . . ?
C69 C48 C47 111.4(2) . . ?
C50 C49 C48 127.9(3) . . ?
C54 C49 C48 112.8(3) . . ?
C54 C49 C50 119.3(3) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 C49 120.0(3) . . ?
C51 C50 H50 120.0 . . ?
C50 C51 H51 119.9 . . ?
C50 C51 C52 120.3(3) . . ?
C52 C51 H51 119.9 . . ?
C51 C52 H52 120.1 . . ?
C53 C52 C51 119.9(3) . . ?
C53 C52 H52 120.1 . . ?
C52 C53 H53 120.1 . . ?
C52 C53 C54 119.7(3) . . ?
C54 C53 H53 120.1 . . ?
C49 C54 C53 120.8(3) . . ?
C49 C54 C55 112.5(3) . . ?
C53 C54 C55 126.7(3) . . ?
C54 C55 C47 103.5(2) . . ?
C54 C55 C56 110.8(3) . . ?
C54 C55 C77 112.4(2) . . ?
C56 C55 C47 103.1(2) . . ?
C56 C55 C77 114.3(3) . . ?
C77 C55 C47 111.7(2) . . ?
C57 C56 C55 127.3(3) . . ?
C61 C56 C55 112.7(3) . . ?
C61 C56 C57 120.0(3) . . ?
C56 C57 H57 120.3 . . ?
C58 C57 C56 119.3(3) . . ?
C58 C57 H57 120.3 . . ?
C57 C58 H58 119.9 . . ?
C57 C58 C59 120.3(3) . . ?
C59 C58 H58 119.9 . . ?
C58 C59 H59 119.9 . . ?
C60 C59 C58 120.2(4) . . ?
C60 C59 H59 119.9 . . ?
C59 C60 H60 120.3 . . ?
C59 C60 C61 119.4(4) . . ?
C61 C60 H60 120.3 . . ?
C56 C61 C60 120.8(3) . . ?
C56 C61 C62 112.4(3) . . ?
C60 C61 C62 126.7(3) . . ?
C61 C62 C47 103.2(2) . . ?
C61 C62 C63 110.2(3) . . ?
C63 C62 C47 103.8(2) . . ?
C85 C62 C47 111.0(3) . . ?
C85 C62 C61 112.4(3) . . ?
C85 C62 C63 115.2(3) . . ?
C64 C63 C62 128.2(3) . . ?
C68 C63 C62 111.8(3) . . ?
C68 C63 C64 120.0(3) . . ?
C63 C64 H64 120.2 . . ?
C65 C64 C63 119.5(3) . . ?
C65 C64 H64 120.2 . . ?
C64 C65 H65 119.6 . . ?
C64 C65 C66 120.9(3) . . ?
C66 C65 H65 119.6 . . ?
C65 C66 H66 120.0 . . ?
C65 C66 C67 119.9(3) . . ?
C67 C66 H66 120.0 . . ?
C66 C67 H67 120.4 . . ?
C66 C67 C68 119.2(4) . . ?
C68 C67 H67 120.4 . . ?
C63 C68 C48 113.1(3) . . ?
C63 C68 C67 120.5(3) . . ?
C67 C68 C48 126.4(3) . . ?
C70 C69 C48 119.9(3) . . ?
C70 C69 C74 117.8(3) . . ?
C74 C69 C48 122.2(3) . . ?
C69 C70 H70 119.2 . . ?
C71 C70 C69 121.5(3) . . ?
C71 C70 H70 119.2 . . ?
C70 C71 H71 120.2 . . ?
C70 C71 C72 119.6(3) . . ?
C72 C71 H71 120.2 . . ?
C71 C72 C75 120.2(3) . . ?
C73 C72 C71 119.4(3) . . ?
C73 C72 C75 120.4(3) . . ?
C72 C73 H73 119.7 . . ?
C72 C73 C74 120.5(3) . . ?
C74 C73 H73 119.7 . . ?
C69 C74 H74 119.4 . . ?
C73 C74 C69 121.1(3) . . ?
C73 C74 H74 119.4 . . ?
C76 C75 C72 177.3(6) . . ?
C75 C76 H76 180.0 . . ?
C78 C77 C55 120.3(3) . . ?
C82 C77 C55 122.8(3) . . ?
C82 C77 C78 116.9(3) . . ?
C77 C78 H78 118.8 . . ?
C79 C78 C77 122.3(3) . . ?
C79 C78 H78 118.8 . . ?
C78 C79 H79 120.0 . . ?
C78 C79 C80 120.0(3) . . ?
C80 C79 H79 120.0 . . ?
C79 C80 C83 121.2(3) . . ?
C81 C80 C79 118.5(3) . . ?
C81 C80 C83 120.3(3) . . ?
C80 C81 H81 119.4 . . ?
C80 C81 C82 121.2(3) . . ?
C82 C81 H81 119.4 . . ?
C77 C82 C81 121.1(3) . . ?
C77 C82 H82 119.5 . . ?
C81 C82 H82 119.5 . . ?
C84 C83 C80 178.9(5) . . ?
C83 C84 H84 180.0 . . ?
C86 C85 C62 119.5(3) . . ?
C90 C85 C62 123.0(3) . . ?
C90 C85 C86 117.2(3) . . ?
C85 C86 H86 119.2 . . ?
C87 C86 C85 121.6(3) . . ?
C87 C86 H86 119.2 . . ?
C86 C87 H87 119.6 . . ?
C86 C87 C88 120.8(3) . . ?
C88 C87 H87 119.6 . . ?
C87 C88 C91 120.4(3) . . ?
C89 C88 C87 118.2(3) . . ?
C89 C88 C91 121.3(3) . . ?
C88 C89 H89 119.5 . . ?
C90 C89 C88 120.9(3) . . ?
C90 C89 H89 119.5 . . ?
C85 C90 H90 119.4 . . ?
C89 C90 C85 121.3(3) . . ?
C89 C90 H90 119.4 . . ?
C92 C91 C88 177.4(4) . . ?
C91 C92 H92 180.0 . . ?

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
C1 C2 C3 C4 -175.1(3) . . . . ?
C1 C2 C3 C8 1.6(3) . . . . ?
C1 C2 C22 C17 0.4(3) . . . . ?
C1 C2 C22 C21 -178.7(3) . . . . ?
C1 C2 C23 C24 -96.0(3) . . . . ?
C1 C2 C23 C28 80.9(3) . . . . ?
C1 C9 C10 C11 177.6(3) . . . . ?
C1 C9 C10 C15 -3.1(3) . . . . ?
C1 C9 C31 C32 -94.7(3) . . . . ?
C1 C9 C31 C36 79.6(3) . . . . ?
C1 C16 C17 C18 179.1(3) . . . . ?
C1 C16 C17 C22 -1.7(3) . . . . ?
C1 C16 C39 C40 80.1(3) . . . . ?
C1 C16 C39 C44 -99.3(3) . . . . ?
C2 C1 C9 C8 2.7(3) . . . . ?
C2 C1 C9 C10 118.3(2) . . . . ?
C2 C1 C9 C31 -118.5(3) . . . . ?
C2 C1 C16 C15 -116.1(2) . . . . ?
C2 C1 C16 C17 1.9(3) . . . . ?
C2 C1 C16 C39 125.4(2) . . . . ?
C2 C3 C4 C5 174.8(3) . . . . ?
C2 C3 C8 C7 -175.5(3) . . . . ?
C2 C3 C8 C9 0.1(4) . . . . ?
C2 C23 C24 C25 177.0(3) . . . . ?
C2 C23 C28 C27 -178.0(3) . . . . ?
C3 C2 C22 C17 -109.7(3) . . . . ?
C3 C2 C22 C21 71.2(4) . . . . ?
C3 C2 C23 C24 21.5(4) . . . . ?
C3 C2 C23 C28 -161.6(3) . . . . ?
C3 C4 C5 C6 0.1(6) . . . . ?
C3 C8 C9 C1 -1.8(3) . . . . ?
C3 C8 C9 C10 -111.9(3) . . . . ?
C3 C8 C9 C31 118.7(3) . . . . ?
C4 C3 C8 C7 1.5(5) . . . . ?
C4 C3 C8 C9 177.1(3) . . . . ?
C4 C5 C6 C7 1.6(6) . . . . ?
C5 C6 C7 C8 -1.9(6) . . . . ?
C6 C7 C8 C3 0.3(6) . . . . ?
C6 C7 C8 C9 -174.6(3) . . . . ?
C7 C8 C9 C1 173.5(3) . . . . ?
C7 C8 C9 C10 63.4(4) . . . . ?
C7 C8 C9 C31 -66.0(4) . . . . ?
C8 C3 C4 C5 -1.7(5) . . . . ?
C8 C9 C10 C11 -72.5(4) . . . . ?
C8 C9 C10 C15 106.8(3) . . . . ?
C8 C9 C31 C32 149.8(3) . . . . ?
C8 C9 C31 C36 -35.8(4) . . . . ?
C9 C1 C2 C3 -2.7(3) . . . . ?
C9 C1 C2 C22 -118.3(2) . . . . ?
C9 C1 C2 C23 121.0(3) . . . . ?
C9 C1 C16 C15 0.9(3) . . . . ?
C9 C1 C16 C17 118.9(2) . . . . ?
C9 C1 C16 C39 -117.6(3) . . . . ?
C9 C10 C11 C12 179.4(3) . . . . ?
C9 C10 C15 C14 -178.9(2) . . . . ?
C9 C10 C15 C16 3.9(3) . . . . ?
C9 C31 C32 C33 172.2(3) . . . . ?
C9 C31 C36 C35 -173.1(3) . . . . ?
C10 C9 C31 C32 22.1(4) . . . . ?
C10 C9 C31 C36 -163.6(3) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C10 C15 C16 C1 -2.9(3) . . . . ?
C10 C15 C16 C17 -113.7(3) . . . . ?
C10 C15 C16 C39 117.9(3) . . . . ?
C11 C10 C15 C14 0.6(4) . . . . ?
C11 C10 C15 C16 -176.6(2) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C15 0.5(4) . . . . ?
C13 C14 C15 C10 -0.9(4) . . . . ?
C13 C14 C15 C16 175.9(3) . . . . ?
C14 C15 C16 C1 -179.9(3) . . . . ?
C14 C15 C16 C17 69.3(4) . . . . ?
C14 C15 C16 C39 -59.1(4) . . . . ?
C15 C10 C11 C12 0.1(4) . . . . ?
C15 C16 C17 C18 -70.1(4) . . . . ?
C15 C16 C17 C22 109.1(3) . . . . ?
C15 C16 C39 C40 -34.5(4) . . . . ?
C15 C16 C39 C44 146.1(3) . . . . ?
C16 C1 C2 C3 114.2(2) . . . . ?
C16 C1 C2 C22 -1.4(3) . . . . ?
C16 C1 C2 C23 -122.1(3) . . . . ?
C16 C1 C9 C8 -114.4(2) . . . . ?
C16 C1 C9 C10 1.2(3) . . . . ?
C16 C1 C9 C31 124.3(3) . . . . ?
C16 C17 C18 C19 179.8(3) . . . . ?
C16 C17 C22 C2 0.9(3) . . . . ?
C16 C17 C22 C21 -180.0(2) . . . . ?
C16 C39 C40 C41 -179.4(3) . . . . ?
C16 C39 C44 C43 -179.6(3) . . . . ?
C17 C16 C39 C40 -162.5(3) . . . . ?
C17 C16 C39 C44 18.1(4) . . . . ?
C17 C18 C19 C20 0.4(5) . . . . ?
C18 C17 C22 C2 -179.9(3) . . . . ?
C18 C17 C22 C21 -0.7(4) . . . . ?
C18 C19 C20 C21 -1.4(5) . . . . ?
C19 C20 C21 C22 1.4(5) . . . . ?
C20 C21 C22 C2 178.7(3) . . . . ?
C20 C21 C22 C17 -0.3(4) . . . . ?
C22 C2 C3 C4 -65.2(4) . . . . ?
C22 C2 C3 C8 111.6(3) . . . . ?
C22 C2 C23 C24 148.4(3) . . . . ?
C22 C2 C23 C28 -34.8(4) . . . . ?
C22 C17 C18 C19 0.7(4) . . . . ?
C23 C2 C3 C4 62.1(4) . . . . ?
C23 C2 C3 C8 -121.2(3) . . . . ?
C23 C2 C22 C17 121.8(3) . . . . ?
C23 C2 C22 C21 -57.3(4) . . . . ?
C23 C24 C25 C26 1.1(5) . . . . ?
C24 C23 C28 C27 -1.0(5) . . . . ?
C24 C25 C26 C27 -1.4(5) . . . . ?
C24 C25 C26 C29 178.0(3) . . . . ?
C25 C26 C27 C28 0.5(5) . . . . ?
C26 C27 C28 C23 0.7(6) . . . . ?
C28 C23 C24 C25 0.1(5) . . . . ?
C29 C26 C27 C28 -178.9(3) . . . . ?
C31 C9 C10 C11 56.1(4) . . . . ?
C31 C9 C10 C15 -124.5(3) . . . . ?
C31 C32 C33 C34 0.8(4) . . . . ?
C32 C31 C36 C35 1.5(4) . . . . ?
C32 C33 C34 C35 1.3(4) . . . . ?
C32 C33 C34 C37 -176.4(3) . . . . ?
C33 C34 C35 C36 -2.1(4) . . . . ?
C34 C35 C36 C31 0.7(5) . . . . ?
C36 C31 C32 C33 -2.2(4) . . . . ?
C37 C34 C35 C36 175.6(3) . . . . ?
C39 C16 C17 C18 56.2(4) . . . . ?
C39 C16 C17 C22 -124.7(3) . . . . ?
C39 C40 C41 C42 -1.8(5) . . . . ?
C40 C39 C44 C43 1.0(5) . . . . ?
C40 C41 C42 C43 2.6(5) . . . . ?
C40 C41 C42 C45 -179.7(3) . . . . ?
C41 C42 C43 C44 -1.6(5) . . . . ?
C42 C43 C44 C39 -0.2(5) . . . . ?
C44 C39 C40 C41 0.0(5) . . . . ?
C45 C42 C43 C44 -179.3(3) . . . . ?
C47 C48 C49 C50 178.2(3) . . . . ?
C47 C48 C49 C54 -0.3(3) . . . . ?
C47 C48 C68 C63 0.7(3) . . . . ?
C47 C48 C68 C67 -178.5(3) . . . . ?
C47 C48 C69 C70 -76.7(3) . . . . ?
C47 C48 C69 C74 99.5(3) . . . . ?
C47 C55 C56 C57 178.2(4) . . . . ?
C47 C55 C56 C61 1.0(4) . . . . ?
C47 C55 C77 C78 -81.9(3) . . . . ?
C47 C55 C77 C82 95.7(3) . . . . ?
C47 C62 C63 C64 179.5(3) . . . . ?
C47 C62 C63 C68 1.1(3) . . . . ?
C47 C62 C85 C86 -77.7(4) . . . . ?
C47 C62 C85 C90 95.4(3) . . . . ?
C48 C47 C55 C54 -0.4(3) . . . . ?
C48 C47 C55 C56 -115.9(3) . . . . ?
C48 C47 C55 C77 120.8(3) . . . . ?
C48 C47 C62 C61 114.4(3) . . . . ?
C48 C47 C62 C63 -0.7(3) . . . . ?
C48 C47 C62 C85 -125.0(3) . . . . ?
C48 C49 C50 C51 -178.2(3) . . . . ?
C48 C49 C54 C53 178.6(3) . . . . ?
C48 C49 C54 C55 0.0(4) . . . . ?
C48 C69 C70 C71 176.3(3) . . . . ?
C48 C69 C74 C73 -176.1(3) . . . . ?
C49 C48 C68 C63 111.2(3) . . . . ?
C49 C48 C68 C67 -68.0(4) . . . . ?
C49 C48 C69 C70 166.7(3) . . . . ?
C49 C48 C69 C74 -17.1(4) . . . . ?
C49 C50 C51 C52 -0.6(6) . . . . ?
C49 C54 C55 C47 0.2(3) . . . . ?
C49 C54 C55 C56 110.1(3) . . . . ?
C49 C54 C55 C77 -120.5(3) . . . . ?
C50 C49 C54 C53 0.0(5) . . . . ?
C50 C49 C54 C55 -178.5(3) . . . . ?
C50 C51 C52 C53 1.0(6) . . . . ?
C51 C52 C53 C54 -0.8(5) . . . . ?
C52 C53 C54 C49 0.3(5) . . . . ?
C52 C53 C54 C55 178.7(3) . . . . ?
C53 C54 C55 C47 -178.2(3) . . . . ?
C53 C54 C55 C56 -68.3(4) . . . . ?
C53 C54 C55 C77 61.0(4) . . . . ?
C54 C49 C50 C51 0.1(5) . . . . ?
C54 C55 C56 C57 68.0(4) . . . . ?
C54 C55 C56 C61 -109.2(3) . . . . ?
C54 C55 C77 C78 33.9(4) . . . . ?
C54 C55 C77 C82 -148.4(3) . . . . ?
C55 C47 C48 C49 0.4(3) . . . . ?
C55 C47 C48 C68 117.2(3) . . . . ?
C55 C47 C48 C69 -122.8(3) . . . . ?
C55 C47 C62 C61 -2.5(3) . . . . ?
C55 C47 C62 C63 -117.5(3) . . . . ?
C55 C47 C62 C85 118.2(3) . . . . ?
C55 C56 C57 C58 -175.7(4) . . . . ?
C55 C56 C61 C60 176.1(3) . . . . ?
C55 C56 C61 C62 -2.7(4) . . . . ?
C55 C77 C78 C79 178.2(3) . . . . ?
C55 C77 C82 C81 -177.8(3) . . . . ?
C56 C55 C77 C78 161.4(3) . . . . ?
C56 C55 C77 C82 -21.0(4) . . . . ?
C56 C57 C58 C59 0.3(7) . . . . ?
C56 C61 C62 C47 3.2(4) . . . . ?
C56 C61 C62 C63 113.5(3) . . . . ?
C56 C61 C62 C85 -116.5(3) . . . . ?
C57 C56 C61 C60 -1.4(6) . . . . ?
C57 C56 C61 C62 179.8(3) . . . . ?
C57 C58 C59 C60 -1.9(8) . . . . ?
C58 C59 C60 C61 1.9(7) . . . . ?
C59 C60 C61 C56 -0.3(6) . . . . ?
C59 C60 C61 C62 178.3(4) . . . . ?
C60 C61 C62 C47 -175.5(4) . . . . ?
C60 C61 C62 C63 -65.2(5) . . . . ?
C60 C61 C62 C85 64.8(5) . . . . ?
C61 C56 C57 C58 1.3(6) . . . . ?
C61 C62 C63 C64 69.5(4) . . . . ?
C61 C62 C63 C68 -108.8(3) . . . . ?
C61 C62 C85 C86 37.3(4) . . . . ?
C61 C62 C85 C90 -149.6(3) . . . . ?
C62 C47 C48 C49 -116.8(3) . . . . ?
C62 C47 C48 C68 0.1(3) . . . . ?
C62 C47 C48 C69 120.0(3) . . . . ?
C62 C47 C55 C54 116.6(3) . . . . ?
C62 C47 C55 C56 1.0(3) . . . . ?
C62 C47 C55 C77 -122.2(3) . . . . ?
C62 C63 C64 C65 -177.6(3) . . . . ?
C62 C63 C68 C48 -1.2(4) . . . . ?
C62 C63 C68 C67 178.0(3) . . . . ?
C62 C85 C86 C87 171.2(3) . . . . ?
C62 C85 C90 C89 -171.3(3) . . . . ?
C63 C62 C85 C86 164.7(3) . . . . ?
C63 C62 C85 C90 -22.2(4) . . . . ?
C63 C64 C65 C66 -0.3(6) . . . . ?
C64 C63 C68 C48 -179.7(3) . . . . ?
C64 C63 C68 C67 -0.5(5) . . . . ?
C64 C65 C66 C67 -0.3(6) . . . . ?
C65 C66 C67 C68 0.5(6) . . . . ?
C66 C67 C68 C48 179.0(3) . . . . ?
C66 C67 C68 C63 0.0(5) . . . . ?
C68 C48 C49 C50 67.8(4) . . . . ?
C68 C48 C49 C54 -110.6(3) . . . . ?
C68 C48 C69 C70 38.1(4) . . . . ?
C68 C48 C69 C74 -145.7(3) . . . . ?
C68 C63 C64 C65 0.7(5) . . . . ?
C69 C48 C49 C50 -60.6(4) . . . . ?
C69 C48 C49 C54 121.0(3) . . . . ?
C69 C48 C68 C63 -119.1(3) . . . . ?
C69 C48 C68 C67 61.8(4) . . . . ?
C69 C70 C71 C72 0.4(5) . . . . ?
C70 C69 C74 C73 0.2(5) . . . . ?
C70 C71 C72 C73 -0.8(5) . . . . ?
C70 C71 C72 C75 179.2(3) . . . . ?
C71 C72 C73 C74 0.9(5) . . . . ?
C72 C73 C74 C69 -0.6(6) . . . . ?
C74 C69 C70 C71 -0.1(5) . . . . ?
C75 C72 C73 C74 -179.0(3) . . . . ?
C77 C55 C56 C57 -60.3(5) . . . . ?
C77 C55 C56 C61 122.5(3) . . . . ?
C77 C78 C79 C80 0.4(5) . . . . ?
C78 C77 C82 C81 -0.1(5) . . . . ?
C78 C79 C80 C81 -1.6(5) . . . . ?
C78 C79 C80 C83 176.2(3) . . . . ?
C79 C80 C81 C82 1.9(5) . . . . ?
C80 C81 C82 C77 -1.1(5) . . . . ?
C82 C77 C78 C79 0.5(5) . . . . ?
C83 C80 C81 C82 -175.9(3) . . . . ?
C85 C62 C63 C64 -59.0(4) . . . . ?
C85 C62 C63 C68 122.7(3) . . . . ?
C85 C86 C87 C88 1.0(5) . . . . ?
C86 C85 C90 C89 1.9(5) . . . . ?
C86 C87 C88 C89 0.8(5) . . . . ?
C86 C87 C88 C91 -176.8(3) . . . . ?
C87 C88 C89 C90 -1.3(5) . . . . ?
C88 C89 C90 C85 -0.1(5) . . . . ?
C90 C85 C86 C87 -2.3(5) . . . . ?
C91 C88 C89 C90 176.4(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 268.8 51.5 ?
2 0.500 0.500 0.500 268.8 51.5 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4 0 -15 0.0457 -3.8235 0.2208 -15.0395 0.3571 -0.0846 0.9302
-6 -6 -2 0.0805 -5.9579 -6.0458 -1.9900 0.9701 -0.2325 -0.0697
3 -1 15 0.0394 3.4525 -0.6797 15.1918 -0.2914 0.0688 -0.9541
4 6 -7 0.0571 3.5996 6.1604 -7.2138 -0.7484 0.1800 0.6383
1 0 -1 0.0105 1.0006 -0.0007 -0.9995 -0.0293 -0.0634 0.0279
-1 0 1 0.0105 -1.0006 0.0007 0.9995 0.0293 0.0634 -0.0279

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 1428583816.21
_olex2_exptl_crystal_mounting_method mounted
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C84-C83 \\sim C76-C75 \\sim C92-C91 \\sim C38-C37 \\sim C46-C45 \\sim C30-C29
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C47(H47)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27), C28(H28),
  C32(H32), C33(H33), C35(H35), C36(H36), C40(H40), C41(H41), C43(H43),
 C44(H44), C50(H50), C51(H51), C52(H52), C53(H53), C57(H57), C58(H58), C59(H59),
  C60(H60), C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71),
 C73(H73), C74(H74), C78(H78), C79(H79), C81(H81), C82(H82), C86(H86), C87(H87),
  C89(H89), C90(H90)
3.c :
 C30(H30), C38(H38), C46(H46), C76(H76), C84(H84), C92(H92)
;
_olex2_submission_special_instructions 'No special instructions were received'

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_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.
;
####################################################################### 
# 
# 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_compound7
_database_code_depnum_ccdc_archive 'CCDC 1514270'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-08-08
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H34 Si3'
_chemical_formula_sum            'C28 H34 Si3'
_chemical_formula_weight         454.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H34 Si3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Si Si 0.2541 0.3302 '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'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3175(3)
_cell_length_b                   10.0431(4)
_cell_length_c                   15.1272(6)
_cell_angle_alpha                78.521(4)
_cell_angle_beta                 84.931(3)
_cell_angle_gamma                66.031(4)
_cell_volume                     1267.56(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8776
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.0840
_cell_measurement_theta_min      2.9570
_exptl_absorpt_coefficient_mu    1.807
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.2569
_exptl_crystal_size_mid          0.1754
_exptl_crystal_size_min          0.0286
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17086
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.591
_diffrn_reflns_theta_min         2.981
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -124.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000    0.0000 -120.0000 171

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
  3 omega -123.00  -34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  178.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
  4 omega   76.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   57.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega   21.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   38.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   16.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   57.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   38.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  8 omega   16.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   77.0000    0.0000 62

#__ type_ start__ end____ width___ exp.time_
  9 omega   62.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488  178.0000 -180.0000 61

#__ type_ start__ end____ width___ exp.time_
 10 omega   11.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   77.0000   90.0000 36

#__ type_ start__ end____ width___ exp.time_
 11 omega   11.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   77.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
 12 omega   59.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488  178.0000  -60.0000 64

#__ type_ start__ end____ width___ exp.time_
 13 omega   13.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   77.0000  150.0000 54

#__ type_ start__ end____ width___ exp.time_
 14 omega   11.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9488   77.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 15 omega   89.00  138.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   45.0000  -30.0000 49

#__ type_ start__ end____ width___ exp.time_
 16 omega   85.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
 17 omega   49.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093 -125.0000  -60.0000 63

#__ type_ start__ end____ width___ exp.time_
 18 omega   31.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093  -94.0000  -30.0000 59

#__ type_ start__ end____ width___ exp.time_
 19 omega   85.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 20 omega  122.00  150.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000   90.0000 28

#__ type_ start__ end____ width___ exp.time_
 21 omega   86.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   62.0000 -171.9260 90

#__ type_ start__ end____ width___ exp.time_
 22 omega   90.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   45.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 23 omega   86.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 24 omega   81.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000    0.0000 28

#__ type_ start__ end____ width___ exp.time_
 25 omega  130.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
 26 omega   85.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   81.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  -90.0000 28

#__ type_ start__ end____ width___ exp.time_
 28 omega   85.00  138.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
 29 omega   85.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
 30 omega   84.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
 31 omega   81.00  151.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000   30.0000 70

#__ type_ start__ end____ width___ exp.time_
 32 omega   81.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   81.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 34 omega  116.00  148.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
 35 omega   89.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   45.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
 36 omega   31.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093  -94.0000 -180.0000 64

#__ type_ start__ end____ width___ exp.time_
 37 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   85.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 39 omega   32.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093  -94.0000  120.0000 61

#__ type_ start__ end____ width___ exp.time_
 40 omega   86.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 41 omega   85.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
 42 omega   56.00   83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093  -45.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 43 omega   81.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000   60.0000 96

#__ type_ start__ end____ width___ exp.time_
 44 omega   81.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 45 omega   83.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 46 omega  115.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  120.0000 63

#__ type_ start__ end____ width___ exp.time_
 47 omega   85.00  120.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
 48 omega   85.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000 -180.0000 31

#__ type_ start__ end____ width___ exp.time_
 49 omega   86.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   61.0000   30.0000 38

#__ type_ start__ end____ width___ exp.time_
 50 omega   81.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 51 omega  112.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   77.0000  -30.0000 64

#__ type_ start__ end____ width___ exp.time_
 52 omega   32.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093  -94.0000   30.0000 73

#__ type_ start__ end____ width___ exp.time_
 53 omega   84.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   64.0000  -81.8243 92

#__ type_ start__ end____ width___ exp.time_
 54 omega   86.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.9093   65.0000  -24.3058 28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0668248000
_diffrn_orient_matrix_UB_12      -0.0476076000
_diffrn_orient_matrix_UB_13      0.0961540000
_diffrn_orient_matrix_UB_21      0.1673276000
_diffrn_orient_matrix_UB_22      -0.0385513000
_diffrn_orient_matrix_UB_23      -0.0394173000
_diffrn_orient_matrix_UB_31      -0.0167120000
_diffrn_orient_matrix_UB_32      0.1592593000
_diffrn_orient_matrix_UB_33      -0.0007522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3919
_reflns_number_total             4457
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0497
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0669P)²+1.4721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1360
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.42489(8) 1.35186(7) 0.19117(4) 0.02138(18) Uani 1 1 d . . . . .
H1 H 0.4493 1.4092 0.2303 0.026 Uiso 1 1 calc R U . . .
Si2 Si 0.09070(7) 1.08577(8) 0.13961(4) 0.02187(18) Uani 1 1 d . . . . .
H2 H -0.0094 1.0753 0.1612 0.026 Uiso 1 1 calc R U . . .
Si3 Si 0.64273(7) 0.82977(7) 0.17011(4) 0.01936(18) Uani 1 1 d . . . . .
H3 H 0.6119 0.8994 0.1112 0.023 Uiso 1 1 calc R U . . .
C1 C 0.3677(3) 1.0788(2) 0.21884(15) 0.0166(5) Uani 1 1 d . . . . .
H1A H 0.3823 1.1029 0.1522 0.020 Uiso 1 1 calc R U . . .
C2 C 0.3739(3) 1.2016(2) 0.26745(16) 0.0170(5) Uani 1 1 d . . . . .
C3 C 0.2107(3) 1.2663(3) 0.30859(15) 0.0180(5) Uani 1 1 d . . . . .
C4 C 0.1504(3) 1.3841(3) 0.35497(17) 0.0225(5) Uani 1 1 d . . . . .
H4 H 0.2134 1.4344 0.3642 0.027 Uiso 1 1 calc R U . . .
C5 C -0.0039(3) 1.4281(3) 0.38795(17) 0.0252(5) Uani 1 1 d . . . . .
H5 H -0.0457 1.5085 0.4198 0.030 Uiso 1 1 calc R U . . .
C6 C -0.0964(3) 1.3548(3) 0.37441(17) 0.0251(5) Uani 1 1 d . . . . .
H6 H -0.2010 1.3851 0.3972 0.030 Uiso 1 1 calc R U . . .
C7 C -0.0364(3) 1.2375(3) 0.32766(17) 0.0227(5) Uani 1 1 d . . . . .
H7 H -0.0997 1.1875 0.3184 0.027 Uiso 1 1 calc R U . . .
C8 C 0.1174(3) 1.1934(3) 0.29429(15) 0.0182(5) Uani 1 1 d . . . . .
C9 C 0.2043(3) 1.0690(3) 0.24235(15) 0.0166(5) Uani 1 1 d . . . . .
C10 C 0.2452(3) 0.9167(3) 0.29942(15) 0.0176(5) Uani 1 1 d . . . . .
C11 C 0.1403(3) 0.8565(3) 0.34217(16) 0.0209(5) Uani 1 1 d . . . . .
H11 H 0.0302 0.9118 0.3362 0.025 Uiso 1 1 calc R U . . .
C12 C 0.1989(3) 0.7151(3) 0.39335(17) 0.0230(5) Uani 1 1 d . . . . .
H12 H 0.1284 0.6729 0.4222 0.028 Uiso 1 1 calc R U . . .
C13 C 0.3602(3) 0.6346(3) 0.40271(17) 0.0235(5) Uani 1 1 d . . . . .
H13 H 0.3992 0.5379 0.4381 0.028 Uiso 1 1 calc R U . . .
C14 C 0.4649(3) 0.6950(3) 0.36042(16) 0.0211(5) Uani 1 1 d . . . . .
H14 H 0.5749 0.6399 0.3670 0.025 Uiso 1 1 calc R U . . .
C15 C 0.4071(3) 0.8363(3) 0.30856(15) 0.0171(5) Uani 1 1 d . . . . .
C16 C 0.5000(3) 0.9253(3) 0.26079(15) 0.0165(5) Uani 1 1 d . . . . .
C17 C 0.5766(3) 0.9659(3) 0.33022(15) 0.0176(5) Uani 1 1 d . . . . .
C18 C 0.6989(3) 0.8708(3) 0.38847(16) 0.0209(5) Uani 1 1 d . . . . .
H18 H 0.7483 0.7686 0.3849 0.025 Uiso 1 1 calc R U . . .
C19 C 0.7484(3) 0.9257(3) 0.45163(16) 0.0236(5) Uani 1 1 d . . . . .
H19 H 0.8324 0.8612 0.4909 0.028 Uiso 1 1 calc R U . . .
C20 C 0.6750(3) 1.0756(3) 0.45769(17) 0.0236(5) Uani 1 1 d . . . . .
H20 H 0.7083 1.1127 0.5014 0.028 Uiso 1 1 calc R U . . .
C21 C 0.5536(3) 1.1699(3) 0.39985(17) 0.0224(5) Uani 1 1 d . . . . .
H21 H 0.5036 1.2720 0.4037 0.027 Uiso 1 1 calc R U . . .
C22 C 0.5048(3) 1.1148(3) 0.33597(16) 0.0186(5) Uani 1 1 d . . . . .
C23 C 0.6024(3) 1.2662(3) 0.1229(2) 0.0437(8) Uani 1 1 d . . . . .
H23A H 0.5775 1.2190 0.0791 0.066 Uiso 1 1 calc R U . . .
H23B H 0.6862 1.1916 0.1627 0.066 Uiso 1 1 calc R U . . .
H23C H 0.6375 1.3428 0.0909 0.066 Uiso 1 1 calc R U . . .
C24 C 0.2614(4) 1.4836(3) 0.1152(2) 0.0411(7) Uani 1 1 d . . . . .
H24A H 0.2471 1.4331 0.0697 0.062 Uiso 1 1 calc R U . . .
H24B H 0.2866 1.5676 0.0853 0.062 Uiso 1 1 calc R U . . .
H24C H 0.1644 1.5196 0.1506 0.062 Uiso 1 1 calc R U . . .
C25 C 0.0395(4) 1.2698(3) 0.0653(2) 0.0359(7) Uani 1 1 d . . . . .
H25A H 0.1353 1.2776 0.0372 0.054 Uiso 1 1 calc R U . . .
H25B H -0.0114 1.3480 0.1012 0.054 Uiso 1 1 calc R U . . .
H25C H -0.0324 1.2806 0.0183 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2048(3) 0.9326(3) 0.07703(19) 0.0320(6) Uani 1 1 d . . . . .
H26A H 0.2196 0.8374 0.1157 0.048 Uiso 1 1 calc R U . . .
H26B H 0.3075 0.9355 0.0596 0.048 Uiso 1 1 calc R U . . .
H26C H 0.1474 0.9444 0.0228 0.048 Uiso 1 1 calc R U . . .
C27 C 0.6313(4) 0.6534(3) 0.1567(2) 0.0352(7) Uani 1 1 d . . . . .
H27A H 0.6765 0.5772 0.2097 0.053 Uiso 1 1 calc R U . . .
H27B H 0.6902 0.6206 0.1026 0.053 Uiso 1 1 calc R U . . .
H27C H 0.5212 0.6698 0.1507 0.053 Uiso 1 1 calc R U . . .
C28 C 0.8515(3) 0.7916(3) 0.1900(2) 0.0336(6) Uani 1 1 d . . . . .
H28A H 0.8931 0.7076 0.2397 0.050 Uiso 1 1 calc R U . . .
H28B H 0.8576 0.8793 0.2057 0.050 Uiso 1 1 calc R U . . .
H28C H 0.9135 0.7680 0.1352 0.050 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 H1 1.0000 . ?
Si1 C2 1.905(2) . ?
Si1 C23 1.854(3) . ?
Si1 C24 1.860(3) . ?
Si2 H2 1.0000 . ?
Si2 C9 1.899(2) . ?
Si2 C25 1.860(3) . ?
Si2 C26 1.862(3) . ?
Si3 H3 1.0000 . ?
Si3 C16 1.933(2) . ?
Si3 C27 1.869(3) . ?
Si3 C28 1.864(3) . ?
C1 H1A 1.0000 . ?
C1 C2 1.578(3) . ?
C1 C9 1.571(3) . ?
C1 C16 1.582(3) . ?
C2 C3 1.521(3) . ?
C2 C22 1.524(3) . ?
C3 C4 1.389(3) . ?
C3 C8 1.397(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.398(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.396(3) . ?
C8 C9 1.513(3) . ?
C9 C10 1.513(3) . ?
C10 C11 1.397(3) . ?
C10 C15 1.396(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.395(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(3) . ?
C15 C16 1.527(3) . ?
C16 C17 1.522(3) . ?
C17 C18 1.395(3) . ?
C17 C22 1.386(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.396(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.393(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Si1 H1 108.1 . . ?
C23 Si1 H1 108.1 . . ?
C23 Si1 C2 109.92(12) . . ?
C23 Si1 C24 109.56(15) . . ?
C24 Si1 H1 108.1 . . ?
C24 Si1 C2 112.90(12) . . ?
C9 Si2 H2 107.9 . . ?
C25 Si2 H2 107.9 . . ?
C25 Si2 C9 111.57(12) . . ?
C25 Si2 C26 111.32(14) . . ?
C26 Si2 H2 107.9 . . ?
C26 Si2 C9 109.98(11) . . ?
C16 Si3 H3 107.1 . . ?
C27 Si3 H3 107.1 . . ?
C27 Si3 C16 113.37(11) . . ?
C28 Si3 H3 107.1 . . ?
C28 Si3 C16 113.25(11) . . ?
C28 Si3 C27 108.45(14) . . ?
C2 C1 H1A 111.2 . . ?
C2 C1 C16 107.95(17) . . ?
C9 C1 H1A 111.2 . . ?
C9 C1 C2 107.27(17) . . ?
C9 C1 C16 107.88(17) . . ?
C16 C1 H1A 111.2 . . ?
C1 C2 Si1 115.11(16) . . ?
C3 C2 Si1 111.22(15) . . ?
C3 C2 C1 103.93(18) . . ?
C3 C2 C22 114.53(19) . . ?
C22 C2 Si1 108.49(15) . . ?
C22 C2 C1 103.45(18) . . ?
C4 C3 C2 127.7(2) . . ?
C4 C3 C8 120.2(2) . . ?
C8 C3 C2 112.0(2) . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C3 C8 C9 112.0(2) . . ?
C7 C8 C3 120.1(2) . . ?
C7 C8 C9 127.9(2) . . ?
C1 C9 Si2 113.69(15) . . ?
C8 C9 Si2 111.82(15) . . ?
C8 C9 C1 104.42(18) . . ?
C8 C9 C10 113.27(19) . . ?
C10 C9 Si2 109.31(15) . . ?
C10 C9 C1 104.09(18) . . ?
C11 C10 C9 126.9(2) . . ?
C15 C10 C9 112.4(2) . . ?
C15 C10 C11 120.6(2) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.2(2) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.4(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.5(2) . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C16 112.2(2) . . ?
C14 C15 C10 119.9(2) . . ?
C14 C15 C16 127.9(2) . . ?
C1 C16 Si3 112.27(15) . . ?
C15 C16 Si3 112.63(16) . . ?
C15 C16 C1 103.39(17) . . ?
C17 C16 Si3 114.41(15) . . ?
C17 C16 C1 103.39(18) . . ?
C17 C16 C15 109.82(18) . . ?
C18 C17 C16 127.6(2) . . ?
C22 C17 C16 112.6(2) . . ?
C22 C17 C18 119.7(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 119.9(2) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.8(2) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C2 112.5(2) . . ?
C17 C22 C21 120.4(2) . . ?
C21 C22 C2 127.0(2) . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si3 C27 H27A 109.5 . . ?
Si3 C27 H27B 109.5 . . ?
Si3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si3 C28 H28A 109.5 . . ?
Si3 C28 H28B 109.5 . . ?
Si3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 C2 C3 C4 -51.8(3) . . . . ?
Si1 C2 C3 C8 127.47(18) . . . . ?
Si1 C2 C22 C17 -119.87(18) . . . . ?
Si1 C2 C22 C21 60.6(3) . . . . ?
Si2 C9 C10 C11 -62.3(3) . . . . ?
Si2 C9 C10 C15 119.21(18) . . . . ?
Si3 C16 C17 C18 -59.1(3) . . . . ?
Si3 C16 C17 C22 124.73(18) . . . . ?
C1 C2 C3 C4 -176.2(2) . . . . ?
C1 C2 C3 C8 3.0(3) . . . . ?
C1 C2 C22 C17 2.8(2) . . . . ?
C1 C2 C22 C21 -176.7(2) . . . . ?
C1 C9 C10 C11 175.9(2) . . . . ?
C1 C9 C10 C15 -2.6(2) . . . . ?
C1 C16 C17 C18 178.5(2) . . . . ?
C1 C16 C17 C22 2.3(2) . . . . ?
C2 C1 C9 Si2 127.57(16) . . . . ?
C2 C1 C9 C8 5.4(2) . . . . ?
C2 C1 C9 C10 -113.58(19) . . . . ?
C2 C1 C16 Si3 -124.30(16) . . . . ?
C2 C1 C16 C15 114.03(19) . . . . ?
C2 C1 C16 C17 -0.5(2) . . . . ?
C2 C3 C4 C5 179.9(2) . . . . ?
C2 C3 C8 C7 179.8(2) . . . . ?
C2 C3 C8 C9 0.4(3) . . . . ?
C3 C2 C22 C17 115.2(2) . . . . ?
C3 C2 C22 C21 -64.3(3) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C3 C8 C9 Si2 -127.10(18) . . . . ?
C3 C8 C9 C1 -3.7(2) . . . . ?
C3 C8 C9 C10 108.8(2) . . . . ?
C4 C3 C8 C7 -0.9(3) . . . . ?
C4 C3 C8 C9 179.8(2) . . . . ?
C4 C5 C6 C7 -0.2(4) . . . . ?
C5 C6 C7 C8 0.0(4) . . . . ?
C6 C7 C8 C3 0.5(4) . . . . ?
C6 C7 C8 C9 179.8(2) . . . . ?
C7 C8 C9 Si2 53.6(3) . . . . ?
C7 C8 C9 C1 177.0(2) . . . . ?
C7 C8 C9 C10 -70.4(3) . . . . ?
C8 C3 C4 C5 0.6(4) . . . . ?
C8 C9 C10 C11 63.1(3) . . . . ?
C8 C9 C10 C15 -115.4(2) . . . . ?
C9 C1 C2 Si1 -127.06(16) . . . . ?
C9 C1 C2 C3 -5.2(2) . . . . ?
C9 C1 C2 C22 114.76(19) . . . . ?
C9 C1 C16 Si3 120.08(16) . . . . ?
C9 C1 C16 C15 -1.6(2) . . . . ?
C9 C1 C16 C17 -116.10(19) . . . . ?
C9 C10 C11 C12 -178.9(2) . . . . ?
C9 C10 C15 C14 178.8(2) . . . . ?
C9 C10 C15 C16 1.7(3) . . . . ?
C10 C11 C12 C13 0.6(4) . . . . ?
C10 C15 C16 Si3 -121.41(18) . . . . ?
C10 C15 C16 C1 0.0(2) . . . . ?
C10 C15 C16 C17 109.8(2) . . . . ?
C11 C10 C15 C14 0.2(3) . . . . ?
C11 C10 C15 C16 -176.9(2) . . . . ?
C11 C12 C13 C14 -0.2(4) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C13 C14 C15 C10 0.2(3) . . . . ?
C13 C14 C15 C16 176.7(2) . . . . ?
C14 C15 C16 Si3 61.8(3) . . . . ?
C14 C15 C16 C1 -176.8(2) . . . . ?
C14 C15 C16 C17 -67.0(3) . . . . ?
C15 C10 C11 C12 -0.6(3) . . . . ?
C15 C16 C17 C18 68.7(3) . . . . ?
C15 C16 C17 C22 -107.5(2) . . . . ?
C16 C1 C2 Si1 116.92(17) . . . . ?
C16 C1 C2 C3 -121.20(18) . . . . ?
C16 C1 C2 C22 -1.3(2) . . . . ?
C16 C1 C9 Si2 -116.36(17) . . . . ?
C16 C1 C9 C8 121.50(19) . . . . ?
C16 C1 C9 C10 2.5(2) . . . . ?
C16 C17 C18 C19 -176.1(2) . . . . ?
C16 C17 C22 C2 -3.4(3) . . . . ?
C16 C17 C22 C21 176.2(2) . . . . ?
C17 C18 C19 C20 0.7(4) . . . . ?
C18 C17 C22 C2 -179.9(2) . . . . ?
C18 C17 C22 C21 -0.3(3) . . . . ?
C18 C19 C20 C21 -0.7(4) . . . . ?
C19 C20 C21 C22 0.2(4) . . . . ?
C20 C21 C22 C2 179.8(2) . . . . ?
C20 C21 C22 C17 0.3(4) . . . . ?
C22 C2 C3 C4 71.6(3) . . . . ?
C22 C2 C3 C8 -109.1(2) . . . . ?
C22 C17 C18 C19 -0.2(3) . . . . ?
C25 Si2 C9 C1 -63.2(2) . . . . ?
C25 Si2 C9 C8 54.7(2) . . . . ?
C25 Si2 C9 C10 -179.01(17) . . . . ?
C26 Si2 C9 C1 60.83(19) . . . . ?
C26 Si2 C9 C8 178.77(17) . . . . ?
C26 Si2 C9 C10 -54.98(19) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0033 0.0005 0.0010 -1.0004 -0.0962 0.0395 0.0009
0 0 1 0.0253 -0.0005 -0.0010 1.0004 0.0962 -0.0395 -0.0009
1 5 1 0.1265 1.0020 4.9987 1.0047 -0.0744 -0.0646 0.7786
4 5 2 0.1247 4.0003 4.9986 2.0071 0.2223 0.3975 0.7277
5 0 2 0.0903 4.9970 -0.0004 2.0042 0.5267 0.7571 -0.0851
0 -5 -1 0.0919 -0.0024 -4.9983 -1.0040 0.1413 0.2319 -0.7952
-3 -5 -2 0.1232 -3.0007 -4.9983 -2.0064 -0.1555 -0.2303 -0.7444
-5 2 -1 0.0706 -4.9963 1.9991 -1.0023 -0.5254 -0.8736 0.4026
-3 1 5 0.0534 -3.0007 0.9939 5.0009 0.2330 -0.7375 0.2047

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?

_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound8
_database_code_depnum_ccdc_archive 'CCDC 1514271'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-04-17
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C31 H40 Si3'
_chemical_formula_sum            'C31 H40 Si3'
_chemical_formula_weight         496.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H40 Si3 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   10.20063(12)
_cell_length_b                   10.20063(12)
_cell_length_c                   46.3518(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4176.87(11)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    12139
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.6300
_cell_measurement_theta_min      5.0740
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.1512
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0227
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            16974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.833
_diffrn_reflns_theta_min         5.097
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9938
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   30.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 158

#__ type_ start__ end____ width___ exp.time_
  2 omega   51.00   78.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega   13.00   60.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   64.00  111.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega   55.00  125.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -178.0000   90.0000 140

#__ type_ start__ end____ width___ exp.time_
  6 omega   57.00  103.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  7 omega   73.00  114.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  8 omega   13.00   68.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 110

#__ type_ start__ end____ width___ exp.time_
  9 omega   25.00   65.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 80

#__ type_ start__ end____ width___ exp.time_
 10 omega   13.00   50.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega   18.00   54.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  120.0000 72

#__ type_ start__ end____ width___ exp.time_
 12 omega   18.00   56.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000    0.0000 76

#__ type_ start__ end____ width___ exp.time_
 13 omega   86.00  113.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
 14 omega   84.00  113.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   71.0000 -148.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega    1.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000 -180.0000 140

#__ type_ start__ end____ width___ exp.time_
 16 omega   17.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   71.0000 -148.0000 108

#__ type_ start__ end____ width___ exp.time_
 17 omega   79.00  106.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 54

#__ type_ start__ end____ width___ exp.time_
 18 omega   89.00  115.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
 19 omega   23.00   59.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -30.0000 72

#__ type_ start__ end____ width___ exp.time_
 20 omega   13.00  115.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 204

#__ type_ start__ end____ width___ exp.time_
 21 omega   37.00  138.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843  -77.0000 -150.0000 202

#__ type_ start__ end____ width___ exp.time_
 22 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000    0.0000 50

#__ type_ start__ end____ width___ exp.time_
 23 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   74.0000  -93.6977 50

#__ type_ start__ end____ width___ exp.time_
 24 omega   78.00  163.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   90.0000 170

#__ type_ start__ end____ width___ exp.time_
 25 omega   39.00  106.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843 -125.0000  120.0000 134

#__ type_ start__ end____ width___ exp.time_
 26 omega   82.00  134.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000 -120.0000 104

#__ type_ start__ end____ width___ exp.time_
 27 omega   82.00  143.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000 -180.0000 122

#__ type_ start__ end____ width___ exp.time_
 28 omega   78.00  178.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000  -60.0000 200

#__ type_ start__ end____ width___ exp.time_
 29 omega   82.00  112.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
 30 omega   79.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   71.0000 -148.0000 52

#__ type_ start__ end____ width___ exp.time_
 31 omega   78.00  177.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   35.5414 198

#__ type_ start__ end____ width___ exp.time_
 32 omega   83.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   56.0000 -105.1524 52

#__ type_ start__ end____ width___ exp.time_
 33 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   75.0000  -38.9174 50

#__ type_ start__ end____ width___ exp.time_
 34 omega   82.00  141.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000  -60.0000 118

#__ type_ start__ end____ width___ exp.time_
 35 omega   80.00  163.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   66.0000   87.1822 166

#__ type_ start__ end____ width___ exp.time_
 36 omega   38.00  122.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843 -125.0000   60.0000 168

#__ type_ start__ end____ width___ exp.time_
 37 omega   78.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
 38 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000  150.0000 50

#__ type_ start__ end____ width___ exp.time_
 39 omega   79.00  102.50   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   70.0000  134.8234 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0541730000
_diffrn_orient_matrix_UB_12      0.1296943000
_diffrn_orient_matrix_UB_13      0.0221108000
_diffrn_orient_matrix_UB_21      -0.0988079000
_diffrn_orient_matrix_UB_22      0.0553739000
_diffrn_orient_matrix_UB_23      -0.0147683000
_diffrn_orient_matrix_UB_31      -0.1331041000
_diffrn_orient_matrix_UB_32      -0.1025502000
_diffrn_orient_matrix_UB_33      0.0199461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1854
_reflns_number_total             1914
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0642P)²+5.8983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1050
_refine_special_details          
;Refined as merohdral twin, ratio 66:34
(TWIN LAW:  0.0, 1.0, 0.0, 1.0, 0.0, 0.0, 0.0, 0.0, 1.0), Twin
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.61290(4) 0.66760(5) 0.39099(2) 0.01317(16) Uani 1 1 d . . . . .
C1 C 0.3333 0.6667 0.40814(5) 0.0115(5) Uani 1 3 d S T P . .
H1 H 0.3333 0.6667 0.3868(7) 0.015(8) Uiso 1 3 d S T P . .
C2 C 0.47756(17) 0.66539(18) 0.42029(3) 0.0120(3) Uani 1 1 d . . . . .
C3 C 0.41064(18) 0.52413(18) 0.43910(3) 0.0133(3) Uani 1 1 d . . . . .
C4 C 0.25268(18) 0.44462(18) 0.43857(3) 0.0134(3) Uani 1 1 d . . . . .
C5 C 0.17175(19) 0.31176(19) 0.45447(3) 0.0171(3) Uani 1 1 d . . . . .
H5 H 0.059(3) 0.255(3) 0.4532(5) 0.030(6) Uiso 1 1 d . . . . .
C6 C 0.2497(2) 0.26098(19) 0.47150(3) 0.0185(3) Uani 1 1 d . . . . .
H6 H 0.192(3) 0.171(3) 0.4828(4) 0.027(6) Uiso 1 1 d . . . . .
C7 C 0.4065(2) 0.3425(2) 0.47305(3) 0.0186(3) Uani 1 1 d . . . . .
H7 H 0.460(2) 0.309(3) 0.4848(4) 0.023(5) Uiso 1 1 d . . . . .
C8 C 0.48771(19) 0.47431(19) 0.45682(3) 0.0165(3) Uani 1 1 d . . . . .
H8 H 0.591(3) 0.526(2) 0.4579(4) 0.020(5) Uiso 1 1 d . . . . .
C9 C 0.7260(2) 0.5800(2) 0.40343(4) 0.0225(4) Uani 1 1 d . . . . .
H9A H 0.784(3) 0.583(3) 0.3873(5) 0.030(6) Uiso 1 1 d . . . . .
H9B H 0.660(3) 0.473(3) 0.4091(5) 0.032(6) Uiso 1 1 d . . . . .
H9C H 0.793(3) 0.632(3) 0.4197(5) 0.038(7) Uiso 1 1 d . . . . .
C10 C 0.5064(2) 0.5588(2) 0.35839(4) 0.0264(4) Uani 1 1 d . . . . .
H10A H 0.443(4) 0.597(4) 0.3494(6) 0.059(9) Uiso 1 1 d . . . . .
H10B H 0.446(4) 0.447(4) 0.3630(6) 0.057(8) Uiso 1 1 d . . . . .
H10C H 0.575(3) 0.561(3) 0.3438(5) 0.041(7) Uiso 1 1 d . . . . .
C11 C 0.7496(2) 0.8660(2) 0.38015(5) 0.0247(4) Uani 1 1 d . . . . .
H11A H 0.820(4) 0.865(3) 0.3662(6) 0.057(8) Uiso 1 1 d . . . . .
H11B H 0.808(4) 0.916(4) 0.3960(7) 0.063(9) Uiso 1 1 d . . . . .
H11C H 0.697(5) 0.917(5) 0.3732(8) 0.097(13) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C2 1.9286(15) . ?
Si1 C9 1.8688(18) . ?
Si1 C10 1.8681(19) . ?
Si1 C11 1.8629(19) . ?
C1 H1 0.99(3) . ?
C1 C2 1.5814(16) . ?
C1 C2 1.5814(16) 3_565 ?
C1 C2 1.5814(16) 2_665 ?
C2 C3 1.523(2) . ?
C2 C4 1.520(2) 2_665 ?
C3 C4 1.396(2) . ?
C3 C8 1.397(2) . ?
C4 C2 1.520(2) 3_565 ?
C4 C5 1.394(2) . ?
C5 H5 1.00(2) . ?
C5 C6 1.391(2) . ?
C6 H6 0.96(2) . ?
C6 C7 1.387(3) . ?
C7 H7 0.95(2) . ?
C7 C8 1.395(2) . ?
C8 H8 0.92(2) . ?
C9 H9A 0.94(2) . ?
C9 H9B 0.99(3) . ?
C9 H9C 0.98(3) . ?
C10 H10A 1.00(3) . ?
C10 H10B 1.01(3) . ?
C10 H10C 0.97(3) . ?
C11 H11A 0.97(3) . ?
C11 H11B 0.92(3) . ?
C11 H11C 0.96(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Si1 C2 112.75(7) . . ?
C10 Si1 C2 111.24(7) . . ?
C10 Si1 C9 106.29(9) . . ?
C11 Si1 C2 110.19(8) . . ?
C11 Si1 C9 107.27(9) . . ?
C11 Si1 C10 108.91(9) . . ?
C2 C1 H1 110.86(9) 2_665 . ?
C2 C1 H1 110.86(9) 3_565 . ?
C2 C1 H1 110.86(9) . . ?
C2 C1 C2 108.05(10) 2_665 3_565 ?
C2 C1 C2 108.05(10) 2_665 . ?
C2 C1 C2 108.05(10) 3_565 . ?
C1 C2 Si1 114.37(11) . . ?
C3 C2 Si1 113.19(10) . . ?
C3 C2 C1 103.47(11) . . ?
C4 C2 Si1 110.68(10) 2_665 . ?
C4 C2 C1 103.49(11) 2_665 . ?
C4 C2 C3 111.05(11) 2_665 . ?
C4 C3 C2 112.40(14) . . ?
C4 C3 C8 119.68(15) . . ?
C8 C3 C2 127.84(14) . . ?
C3 C4 C2 112.56(14) . 3_565 ?
C5 C4 C2 126.99(15) . 3_565 ?
C5 C4 C3 120.42(15) . . ?
C4 C5 H5 118.8(13) . . ?
C6 C5 C4 119.41(16) . . ?
C6 C5 H5 121.8(13) . . ?
C5 C6 H6 118.4(14) . . ?
C7 C6 C5 120.58(16) . . ?
C7 C6 H6 120.9(14) . . ?
C6 C7 H7 120.7(14) . . ?
C6 C7 C8 120.02(15) . . ?
C8 C7 H7 119.3(14) . . ?
C3 C8 H8 121.4(13) . . ?
C7 C8 C3 119.81(15) . . ?
C7 C8 H8 118.8(13) . . ?
Si1 C9 H9A 105.3(14) . . ?
Si1 C9 H9B 111.5(14) . . ?
Si1 C9 H9C 114.1(15) . . ?
H9A C9 H9B 108.5(19) . . ?
H9A C9 H9C 110(2) . . ?
H9B C9 H9C 107.5(19) . . ?
Si1 C10 H10A 113.7(18) . . ?
Si1 C10 H10B 110.1(16) . . ?
Si1 C10 H10C 110.8(15) . . ?
H10A C10 H10B 112(2) . . ?
H10A C10 H10C 107(2) . . ?
H10B C10 H10C 102(2) . . ?
Si1 C11 H11A 109.1(18) . . ?
Si1 C11 H11B 108(2) . . ?
Si1 C11 H11C 111(3) . . ?
H11A C11 H11B 105(3) . . ?
H11A C11 H11C 113(3) . . ?
H11B C11 H11C 110(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
Si1 C2 C3 C4 -122.46(13) . . . . ?
Si1 C2 C3 C8 60.89(19) . . . . ?
C1 C2 C3 C4 1.88(17) . . . . ?
C1 C2 C3 C8 -174.76(15) . . . . ?
C2 C1 C2 Si1 -120.69(15) 2_665 . . . ?
C2 C1 C2 Si1 122.64(15) 3_565 . . . ?
C2 C1 C2 C3 115.74(10) 2_665 . . . ?
C2 C1 C2 C3 -0.93(17) 3_565 . . . ?
C2 C1 C2 C4 -0.20(17) 2_665 . . 2_665 ?
C2 C1 C2 C4 -116.87(10) 3_565 . . 2_665 ?
C2 C3 C4 C2 -2.17(18) . . . 3_565 ?
C2 C3 C4 C5 179.78(13) . . . . ?
C2 C3 C8 C7 178.77(14) . . . . ?
C2 C4 C5 C6 -176.09(14) 3_565 . . . ?
C3 C4 C5 C6 1.6(2) . . . . ?
C4 C2 C3 C4 112.33(16) 2_665 . . . ?
C4 C2 C3 C8 -64.32(19) 2_665 . . . ?
C4 C3 C8 C7 2.3(2) . . . . ?
C4 C5 C6 C7 0.9(2) . . . . ?
C5 C6 C7 C8 -1.8(3) . . . . ?
C6 C7 C8 C3 0.2(2) . . . . ?
C8 C3 C4 C2 174.78(13) . . . 3_565 ?
C8 C3 C4 C5 -3.3(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0089 -0.0003 0.0002 -0.9998 -0.0221 0.0148 -0.0199
0 1 0 0.0574 -0.0015 1.0005 0.0012 0.1297 0.0555 -0.1024
-1 0 0 0.0742 -0.9995 -0.0001 -0.0009 -0.0542 0.0988 0.1330
0 0 1 0.0139 0.0003 -0.0002 0.9998 0.0221 -0.0148 0.0199
0 -1 0 0.0725 0.0015 -1.0005 -0.0012 -0.1297 -0.0555 0.1024
1 -1 0 0.0697 1.0010 -1.0004 -0.0002 -0.0755 -0.1543 -0.0306
-6 2 0 0.0614 -6.0001 2.0006 -0.0034 -0.0657 0.7037 0.5934
2 -1 0 0.0777 2.0005 -1.0003 0.0007 -0.0213 -0.2531 -0.1637

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_refinement_description    
;
;

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-1
####################################################################### 
# 
# 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_compound9
_database_code_depnum_ccdc_archive 'CCDC 1514272'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2015-01-06
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H31 F3 Si3'
_chemical_formula_sum            'C28 H31 F3 Si3'
_chemical_formula_weight         508.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H29 F3 Si3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   28.66207(14)
_cell_length_b                   9.64548(4)
_cell_length_c                   19.37370(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.7173(5)
_cell_angle_gamma                90
_cell_volume                     5155.78(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    84437
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.1130
_cell_measurement_theta_min      3.1870
_exptl_absorpt_coefficient_mu    2.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.2905
_exptl_crystal_size_mid          0.1772
_exptl_crystal_size_min          0.0558
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            145084
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.986
_diffrn_reflns_theta_min         3.204
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -116.00   -5.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  120.0000 111

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  120.0000 83

#__ type_ start__ end____ width___ exp.time_
  3 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 102

#__ type_ start__ end____ width___ exp.time_
  5 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 102

#__ type_ start__ end____ width___ exp.time_
  6 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -30.0000 102

#__ type_ start__ end____ width___ exp.time_
  7 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 102

#__ type_ start__ end____ width___ exp.time_
  8 omega  -28.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -77.0000  -90.0000 102

#__ type_ start__ end____ width___ exp.time_
  9 omega   23.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -30.0000 91

#__ type_ start__ end____ width___ exp.time_
 10 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   30.0000 102

#__ type_ start__ end____ width___ exp.time_
 11 omega    1.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000 -180.0000 81

#__ type_ start__ end____ width___ exp.time_
 12 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -150.0000 102

#__ type_ start__ end____ width___ exp.time_
 13 omega   23.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -125.0000   30.0000 74

#__ type_ start__ end____ width___ exp.time_
 14 omega   82.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000   41.2091 96

#__ type_ start__ end____ width___ exp.time_
 15 omega   82.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000   52.4514 96

#__ type_ start__ end____ width___ exp.time_
 16 omega   83.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -160.6146 95

#__ type_ start__ end____ width___ exp.time_
 17 omega   83.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000    0.8018 95

#__ type_ start__ end____ width___ exp.time_
 18 omega   87.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   50.0000 -159.1968 91

#__ type_ start__ end____ width___ exp.time_
 19 omega   84.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   64.0000  -58.1894 94

#__ type_ start__ end____ width___ exp.time_
 20 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   96.6165 93

#__ type_ start__ end____ width___ exp.time_
 21 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 93

#__ type_ start__ end____ width___ exp.time_
 22 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 93

#__ type_ start__ end____ width___ exp.time_
 23 omega   31.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 78

#__ type_ start__ end____ width___ exp.time_
 24 omega   31.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 78

#__ type_ start__ end____ width___ exp.time_
 25 omega   31.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 78

#__ type_ start__ end____ width___ exp.time_
 26 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

#__ type_ start__ end____ width___ exp.time_
 27 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 97

#__ type_ start__ end____ width___ exp.time_
 28 omega   41.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 81

#__ type_ start__ end____ width___ exp.time_
 29 omega   83.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000  -45.3478 95

#__ type_ start__ end____ width___ exp.time_
 30 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
 31 omega   41.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 81

#__ type_ start__ end____ width___ exp.time_
 32 omega   82.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000 -134.8651 96

#__ type_ start__ end____ width___ exp.time_
 33 omega   87.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   52.0000  -52.0910 91

#__ type_ start__ end____ width___ exp.time_
 34 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 93

#__ type_ start__ end____ width___ exp.time_
 35 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

#__ type_ start__ end____ width___ exp.time_
 36 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 97

#__ type_ start__ end____ width___ exp.time_
 37 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000  -44.3568 97

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 97

#__ type_ start__ end____ width___ exp.time_
 39 omega   85.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
 40 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

#__ type_ start__ end____ width___ exp.time_
 41 omega   81.00  171.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
 42 omega   82.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000  113.7660 26

#__ type_ start__ end____ width___ exp.time_
 43 omega   85.00  111.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   81.00  107.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 45 omega  111.00  177.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 66

#__ type_ start__ end____ width___ exp.time_
 46 omega   81.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
 47 omega   42.00  120.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 78

#__ type_ start__ end____ width___ exp.time_
 48 omega   81.00  107.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 49 omega   84.00  114.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   65.0000 -144.4198 30

#__ type_ start__ end____ width___ exp.time_
 50 omega   85.00  140.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -180.0000 55

#__ type_ start__ end____ width___ exp.time_
 51 omega   43.00  137.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
 52 omega   81.00  107.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   82.00  115.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000  -87.0027 33

#__ type_ start__ end____ width___ exp.time_
 54 omega   85.00  113.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   62.0000 -112.7481 28

#__ type_ start__ end____ width___ exp.time_
 55 omega   85.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   37.4105 38

#__ type_ start__ end____ width___ exp.time_
 56 omega   88.00  114.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   46.0000 -167.7726 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0371801000
_diffrn_orient_matrix_UB_12      -0.0165796000
_diffrn_orient_matrix_UB_13      -0.0438684000
_diffrn_orient_matrix_UB_21      -0.0329641000
_diffrn_orient_matrix_UB_22      -0.1084171000
_diffrn_orient_matrix_UB_23      -0.0479227000
_diffrn_orient_matrix_UB_31      -0.0254780000
_diffrn_orient_matrix_UB_32      0.1160831000
_diffrn_orient_matrix_UB_33      -0.0510164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9609
_reflns_number_total             10125
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0465
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0631P)²+5.9475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1239
_refine_special_details          
;
 Disorder of Me2FSi-group Si(2), F(2), C(25), C(26) on two positions (91:9).
 Disorder of Si(5), F(5), C(54), F(6), C(56) over two sites with a 50:50
 distribution.
 Because of low resolution the disordered positions of F(6) and C(56) 
 were refined on the same site.
 All thermal displacement parameters of disordered atoms were constrained with 
 EADP to become equal. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.07273(2) 0.76226(6) 0.25214(3) 0.02527(12) Uani 1 1 d . . . . .
Si2A Si 0.13567(4) 0.31937(7) 0.23487(4) 0.02636(19) Uani 0.911(3) 1 d . . P A
1
Si2B Si 0.1515(4) 0.3065(8) 0.2234(5) 0.02636(19) Uani 0.089(3) 1 d . . P A 2
Si3 Si 0.22310(2) 0.72654(5) 0.18113(3) 0.02423(12) Uani 1 1 d . . . . .
F1 F 0.02477(5) 0.85982(15) 0.22715(7) 0.0411(3) Uani 1 1 d . . . . .
F2A F 0.16532(9) 0.40755(19) 0.30369(10) 0.0678(7) Uani 0.911(3) 1 d . . P A 1
F2B F 0.1960(9) 0.368(2) 0.2737(10) 0.0678(7) Uani 0.089(3) 1 d . . P A 2
F3 F 0.21180(4) 0.83579(13) 0.23765(7) 0.0346(3) Uani 1 1 d . . . . .
C1 C 0.13159(6) 0.60346(18) 0.17958(10) 0.0203(3) Uani 1 1 d . . . . .
H1 H 0.1506 0.6086 0.2299 0.024 Uiso 1 1 calc R U . . .
C2 C 0.08353(6) 0.69042(19) 0.16651(10) 0.0210(4) Uani 1 1 d . . . . .
C3 C 0.04398(6) 0.5865(2) 0.13239(9) 0.0217(4) Uani 1 1 d . . . . .
C4 C -0.00561(7) 0.6122(2) 0.10637(10) 0.0264(4) Uani 1 1 d . . . . .
H4 H -0.0180 0.6999 0.1107 0.032 Uiso 1 1 calc R U . . .
C5 C -0.03638(7) 0.5054(2) 0.07387(10) 0.0291(4) Uani 1 1 d . . . . .
H5 H -0.0694 0.5220 0.0560 0.035 Uiso 1 1 calc R U . . .
C6 C -0.01800(7) 0.3747(2) 0.06801(10) 0.0295(4) Uani 1 1 d . . . . .
H6 H -0.0388 0.3040 0.0459 0.035 Uiso 1 1 calc R U . . .
C7 C 0.03136(7) 0.3480(2) 0.09489(10) 0.0272(4) Uani 1 1 d . . . . .
H7 H 0.0435 0.2597 0.0914 0.033 Uiso 1 1 calc R U . . .
C8 C 0.06236(7) 0.4550(2) 0.12706(10) 0.0228(4) Uani 1 1 d . . . . .
C9 C 0.11744(7) 0.44847(19) 0.15646(10) 0.0230(4) Uani 1 1 d . . . . .
C10 C 0.14100(6) 0.42367(19) 0.09595(10) 0.0236(4) Uani 1 1 d . . . . .
C11 C 0.13879(7) 0.3041(2) 0.05471(12) 0.0292(4) Uani 1 1 d . . . . .
H11 H 0.1237 0.2248 0.0655 0.035 Uiso 1 1 calc R U . . .
C12 C 0.15933(7) 0.3040(2) -0.00256(12) 0.0327(5) Uani 1 1 d . . . . .
H12 H 0.1578 0.2243 -0.0301 0.039 Uiso 1 1 calc R U . . .
C13 C 0.18202(7) 0.4215(2) -0.01904(11) 0.0305(4) Uani 1 1 d . . . . .
H13 H 0.1954 0.4206 -0.0578 0.037 Uiso 1 1 calc R U . . .
C14 C 0.18482(7) 0.5406(2) 0.02230(11) 0.0268(4) Uani 1 1 d . . . . .
H14 H 0.2004 0.6191 0.0117 0.032 Uiso 1 1 calc R U . . .
C15 C 0.16415(6) 0.54157(19) 0.07960(10) 0.0227(4) Uani 1 1 d . . . . .
C16 C 0.16110(6) 0.66253(19) 0.12824(10) 0.0208(4) Uani 1 1 d . . . . .
C17 C 0.12971(6) 0.77978(18) 0.08872(10) 0.0210(4) Uani 1 1 d . . . . .
C18 C 0.13722(7) 0.8599(2) 0.03307(10) 0.0253(4) Uani 1 1 d . . . . .
H18 H 0.1644 0.8454 0.0165 0.030 Uiso 1 1 calc R U . . .
C19 C 0.10368(7) 0.9619(2) 0.00246(10) 0.0275(4) Uani 1 1 d . . . . .
H19 H 0.1081 1.0142 -0.0356 0.033 Uiso 1 1 calc R U . . .
C20 C 0.06388(7) 0.9862(2) 0.02821(11) 0.0279(4) Uani 1 1 d . . . . .
H20 H 0.0423 1.0568 0.0084 0.033 Uiso 1 1 calc R U . . .
C21 C 0.05598(7) 0.9056(2) 0.08356(10) 0.0258(4) Uani 1 1 d . . . . .
H21 H 0.0292 0.9219 0.1009 0.031 Uiso 1 1 calc R U . . .
C22 C 0.08855(6) 0.80013(19) 0.11276(10) 0.0213(4) Uani 1 1 d . . . . .
C23 C 0.12153(8) 0.8750(2) 0.30210(12) 0.0364(5) Uani 1 1 d . . . . .
H23A H 0.1129 0.9133 0.3427 0.055 Uiso 1 1 calc R U . . .
H23B H 0.1264 0.9488 0.2715 0.055 Uiso 1 1 calc R U . . .
H23C H 0.1509 0.8221 0.3183 0.055 Uiso 1 1 calc R U . . .
C24 C 0.05940(11) 0.6225(3) 0.30783(13) 0.0444(6) Uani 1 1 d . . . . .
H24A H 0.0322 0.5699 0.2806 0.067 Uiso 1 1 calc R U . . .
H24B H 0.0519 0.6614 0.3492 0.067 Uiso 1 1 calc R U . . .
H24C H 0.0871 0.5629 0.3230 0.067 Uiso 1 1 calc R U . . .
C25A C 0.08449(10) 0.2435(3) 0.26169(15) 0.0374(6) Uani 0.911(3) 1 d . . P A 1
H25A H 0.0962 0.1981 0.3072 0.056 Uiso 0.911(3) 1 calc R U P A 1
H25B H 0.0683 0.1772 0.2263 0.056 Uiso 0.911(3) 1 calc R U P A 1
H25C H 0.0622 0.3154 0.2655 0.056 Uiso 0.911(3) 1 calc R U P A 1
C26A C 0.17764(12) 0.1831(4) 0.2212(2) 0.0650(12) Uani 0.911(3) 1 d . . P A 1
H26A H 0.1617 0.1272 0.1806 0.097 Uiso 0.911(3) 1 calc R U P A 1
H26B H 0.2059 0.2255 0.2126 0.097 Uiso 0.911(3) 1 calc R U P A 1
H26C H 0.1871 0.1258 0.2632 0.097 Uiso 0.911(3) 1 calc R U P A 1
C25B C 0.1125(11) 0.280(3) 0.2809(16) 0.0374(6) Uani 0.089(3) 1 d . . P A 2
H25D H 0.1298 0.2301 0.3230 0.056 Uiso 0.089(3) 1 calc R U P A 2
H25E H 0.0847 0.2270 0.2558 0.056 Uiso 0.089(3) 1 calc R U P A 2
H25F H 0.1022 0.3679 0.2946 0.056 Uiso 0.089(3) 1 calc R U P A 2
C26B C 0.1572(14) 0.130(4) 0.193(3) 0.0650(12) Uani 0.089(3) 1 d . . P A 2
H26D H 0.1269 0.1013 0.1615 0.097 Uiso 0.089(3) 1 calc R U P A 2
H26E H 0.1820 0.1273 0.1684 0.097 Uiso 0.089(3) 1 calc R U P A 2
H26F H 0.1658 0.0695 0.2339 0.097 Uiso 0.089(3) 1 calc R U P A 2
C27 C 0.25850(7) 0.5832(2) 0.23344(12) 0.0333(5) Uani 1 1 d . . . . .
H27A H 0.2852 0.6205 0.2699 0.050 Uiso 1 1 calc R U . . .
H27B H 0.2706 0.5246 0.2022 0.050 Uiso 1 1 calc R U . . .
H27C H 0.2381 0.5300 0.2554 0.050 Uiso 1 1 calc R U . . .
C28 C 0.25748(8) 0.8211(3) 0.12823(13) 0.0388(5) Uani 1 1 d . . . . .
H28A H 0.2882 0.8496 0.1591 0.058 Uiso 1 1 calc R U . . .
H28B H 0.2395 0.9014 0.1068 0.058 Uiso 1 1 calc R U . . .
H28C H 0.2627 0.7617 0.0913 0.058 Uiso 1 1 calc R U . . .
Si4 Si 0.64753(2) 0.69815(6) 0.55482(3) 0.02906(13) Uani 1 1 d . . . . .
Si5A Si 0.5708(11) 0.246(4) 0.5153(18) 0.0381(4) Uani 0.5 1 d . . P B 1
Si5B Si 0.5712(11) 0.244(4) 0.5144(18) 0.0381(4) Uani 0.5 1 d . . P B 2
Si6 Si 0.53977(2) 0.57213(6) 0.32300(3) 0.03165(14) Uani 1 1 d . . . . .
F4 F 0.60938(7) 0.80466(18) 0.50712(8) 0.0635(5) Uani 1 1 d . . . . .
F5A F 0.5621(2) 0.3716(4) 0.5725(3) 0.0638(13) Uani 0.5 1 d . . P B 1
F6A F 0.49611(8) 0.4627(3) 0.33574(13) 0.0642(4) Uani 0.5 1 d . . P C 1
F5B F 0.54262(15) 0.3656(4) 0.5315(3) 0.0527(10) Uani 0.5 1 d . . P B 2
F6B F 0.53630(8) 0.5815(3) 0.23425(13) 0.0642(4) Uani 0.5 1 d . . P C 2
C29 C 0.60941(7) 0.4801(2) 0.45254(10) 0.0233(4) Uani 1 1 d . . . . .
H29 H 0.5817 0.5163 0.4675 0.028 Uiso 1 1 calc R U . . .
C30 C 0.65741(6) 0.5612(2) 0.49013(10) 0.0229(4) Uani 1 1 d . . . . .
C31 C 0.69174(7) 0.4486(2) 0.52850(10) 0.0242(4) Uani 1 1 d . . . . .
C32 C 0.74033(7) 0.4630(2) 0.56583(10) 0.0286(4) Uani 1 1 d . . . . .
H32 H 0.7549 0.5499 0.5708 0.034 Uiso 1 1 calc R U . . .
C33 C 0.76689(8) 0.3467(2) 0.59560(11) 0.0326(4) Uani 1 1 d . . . . .
H33 H 0.7993 0.3559 0.6208 0.039 Uiso 1 1 calc R U . . .
C34 C 0.74519(8) 0.2171(2) 0.58793(11) 0.0338(5) Uani 1 1 d . . . . .
H34 H 0.7631 0.1398 0.6084 0.041 Uiso 1 1 calc R U . . .
C35 C 0.69687(8) 0.2021(2) 0.54981(11) 0.0306(4) Uani 1 1 d . . . . .
H35 H 0.6825 0.1149 0.5441 0.037 Uiso 1 1 calc R U . . .
C36 C 0.66999(7) 0.3181(2) 0.52019(10) 0.0254(4) Uani 1 1 d . . . . .
C37 C 0.61822(7) 0.3216(2) 0.47237(11) 0.0261(4) Uani 1 1 d . . . . .
C38 C 0.61539(7) 0.2525(2) 0.40086(11) 0.0281(4) Uani 1 1 d . . . . .
C39 C 0.62248(8) 0.1129(2) 0.38847(13) 0.0366(5) Uani 1 1 d . . . . .
H39 H 0.6284 0.0495 0.4260 0.044 Uiso 1 1 calc R U . . .
C40 C 0.62057(9) 0.0692(3) 0.31923(14) 0.0434(6) Uani 1 1 d . . . . .
H40 H 0.6256 -0.0237 0.3105 0.052 Uiso 1 1 calc R U . . .
C41 C 0.61129(9) 0.1635(3) 0.26337(13) 0.0413(5) Uani 1 1 d . . . . .
H41 H 0.6099 0.1334 0.2172 0.050 Uiso 1 1 calc R U . . .
C42 C 0.60404(8) 0.3028(2) 0.27559(12) 0.0332(5) Uani 1 1 d . . . . .
H42 H 0.5978 0.3657 0.2378 0.040 Uiso 1 1 calc R U . . .
C43 C 0.60621(7) 0.3473(2) 0.34456(11) 0.0271(4) Uani 1 1 d . . . . .
C44 C 0.60110(7) 0.4946(2) 0.36904(10) 0.0238(4) Uani 1 1 d . . . . .
C45 C 0.64223(6) 0.5880(2) 0.36172(10) 0.0233(4) Uani 1 1 d . . . . .
C46 C 0.65206(7) 0.6336(2) 0.29906(11) 0.0288(4) Uani 1 1 d . . . . .
H46 H 0.6317 0.6092 0.2546 0.035 Uiso 1 1 calc R U . . .
C47 C 0.69250(8) 0.7160(2) 0.30314(11) 0.0322(4) Uani 1 1 d . . . . .
H47 H 0.6990 0.7474 0.2613 0.039 Uiso 1 1 calc R U . . .
C48 C 0.72327(7) 0.7516(2) 0.36918(12) 0.0306(4) Uani 1 1 d . . . . .
H48 H 0.7503 0.8065 0.3715 0.037 Uiso 1 1 calc R U . . .
C49 C 0.71379(7) 0.7053(2) 0.43190(11) 0.0271(4) Uani 1 1 d . . . . .
H49 H 0.7346 0.7285 0.4762 0.033 Uiso 1 1 calc R U . . .
C50 C 0.67315(7) 0.6241(2) 0.42820(10) 0.0229(4) Uani 1 1 d . . . . .
C51 C 0.70159(9) 0.8016(3) 0.59948(13) 0.0403(5) Uani 1 1 d . . . . .
H51A H 0.7137 0.8476 0.5639 0.060 Uiso 1 1 calc R U . . .
H51B H 0.7262 0.7414 0.6276 0.060 Uiso 1 1 calc R U . . .
H51C H 0.6930 0.8693 0.6302 0.060 Uiso 1 1 calc R U . . .
C52 C 0.62108(11) 0.6220(4) 0.62313(15) 0.0614(9) Uani 1 1 d . . . . .
H52A H 0.6105 0.6949 0.6490 0.092 Uiso 1 1 calc R U . . .
H52B H 0.6451 0.5668 0.6558 0.092 Uiso 1 1 calc R U . . .
H52C H 0.5939 0.5647 0.6001 0.092 Uiso 1 1 calc R U . . .
C53 C 0.59479(11) 0.1171(3) 0.58558(16) 0.0560(7) Uani 1 1 d . . . . .
H53A H 0.6215 0.1564 0.6213 0.084 Uiso 1 1 calc R U . B 1
H53B H 0.6057 0.0371 0.5649 0.084 Uiso 1 1 calc R U . B 1
H53C H 0.5698 0.0904 0.6073 0.084 Uiso 1 1 calc R U . B 1
C54A C 0.5129(3) 0.2061(10) 0.4546(5) 0.067(2) Uani 0.5 1 d . . P B 1
H54A H 0.4989 0.2891 0.4302 0.100 Uiso 0.5 1 calc R U P B 1
H54B H 0.4918 0.1691 0.4810 0.100 Uiso 0.5 1 calc R U P B 1
H54C H 0.5170 0.1390 0.4201 0.100 Uiso 0.5 1 calc R U P B 1
C54B C 0.5261(3) 0.1293(10) 0.4457(5) 0.067(2) Uani 0.5 1 d . . P B 2
H54D H 0.5137 0.1803 0.4020 0.100 Uiso 0.5 1 calc R U P B 2
H54E H 0.4998 0.1030 0.4648 0.100 Uiso 0.5 1 calc R U P B 2
H54F H 0.5424 0.0476 0.4360 0.100 Uiso 0.5 1 calc R U P B 2
C55 C 0.53228(9) 0.7448(3) 0.35711(18) 0.0550(7) Uani 1 1 d . . . . .
H55A H 0.5012 0.7812 0.3319 0.082 Uiso 1 1 calc R U . . .
H55B H 0.5573 0.8049 0.3500 0.082 Uiso 1 1 calc R U . . .
H55C H 0.5345 0.7392 0.4074 0.082 Uiso 1 1 calc R U . . .
C56A C 0.53630(8) 0.5815(3) 0.23425(13) 0.0642(4) Uani 0.5 1 d . . P C 1
H56A H 0.5609 0.6431 0.2272 0.096 Uiso 0.5 1 calc R U P C 1
H56B H 0.5411 0.4909 0.2168 0.096 Uiso 0.5 1 calc R U P C 1
H56C H 0.5050 0.6157 0.2085 0.096 Uiso 0.5 1 calc R U P C 1
C56B C 0.49611(8) 0.4627(3) 0.33574(13) 0.0642(4) Uani 0.5 1 d . . P C 2
H56D H 0.4981 0.4575 0.3859 0.096 Uiso 0.5 1 calc R U P C 2
H56E H 0.4647 0.4968 0.3101 0.096 Uiso 0.5 1 calc R U P C 2
H56F H 0.5009 0.3720 0.3184 0.096 Uiso 0.5 1 calc R U P C 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
Si1 F1 1.6276(13) . ?
Si1 C2 1.8990(19) . ?
Si1 C23 1.828(2) . ?
Si1 C24 1.830(2) . ?
Si2A F2A 1.6154(18) . ?
Si2A C9 1.924(2) . ?
Si2A C25A 1.836(3) . ?
Si2A C26A 1.849(3) . ?
Si2B F2B 1.50(2) . ?
Si2B C9 1.955(8) . ?
Si2B C25B 1.80(3) . ?
Si2B C26B 1.82(5) . ?
Si3 F3 1.6144(13) . ?
Si3 C16 1.8979(18) . ?
Si3 C27 1.847(2) . ?
Si3 C28 1.844(2) . ?
C1 H1 0.9800 . ?
C1 C2 1.574(2) . ?
C1 C9 1.582(2) . ?
C1 C16 1.577(2) . ?
C2 C3 1.523(2) . ?
C2 C22 1.519(2) . ?
C3 C4 1.396(3) . ?
C3 C8 1.388(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.393(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.394(3) . ?
C8 C9 1.528(2) . ?
C9 C10 1.522(3) . ?
C10 C11 1.395(3) . ?
C10 C15 1.396(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.390(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.386(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.393(3) . ?
C15 C16 1.517(3) . ?
C16 C17 1.517(2) . ?
C17 C18 1.390(3) . ?
C17 C22 1.394(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.391(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.393(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25A H25A 0.9600 . ?
C25A H25B 0.9600 . ?
C25A H25C 0.9600 . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C25B H25D 0.9600 . ?
C25B H25E 0.9600 . ?
C25B H25F 0.9600 . ?
C26B H26D 0.9600 . ?
C26B H26E 0.9600 . ?
C26B H26F 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Si4 F4 1.5993(16) . ?
Si4 C30 1.894(2) . ?
Si4 C51 1.849(2) . ?
Si4 C52 1.846(3) . ?
Si5A F5A 1.71(4) . ?
Si5A C37 1.92(4) . ?
Si5A C53 1.83(3) . ?
Si5A C54A 1.80(3) . ?
Si5B F5B 1.52(4) . ?
Si5B C37 1.91(4) . ?
Si5B C53 1.83(3) . ?
Si5B C54B 1.93(3) . ?
Si6 F6A 1.705(2) . ?
Si6 F6B 1.698(2) . ?
Si6 C44 1.8962(19) . ?
Si6 C55 1.826(3) . ?
C29 H29 0.9800 . ?
C29 C30 1.579(2) . ?
C29 C37 1.581(3) . ?
C29 C44 1.576(3) . ?
C30 C31 1.518(3) . ?
C30 C50 1.518(2) . ?
C31 C32 1.391(3) . ?
C31 C36 1.394(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.391(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.386(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.389(3) . ?
C35 H35 0.9300 . ?
C35 C36 1.391(3) . ?
C36 C37 1.522(3) . ?
C37 C38 1.519(3) . ?
C38 C39 1.393(3) . ?
C38 C43 1.393(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.393(3) . ?
C40 H40 0.9300 . ?
C40 C41 1.383(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.389(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.389(3) . ?
C43 C44 1.517(3) . ?
C44 C45 1.520(3) . ?
C45 C46 1.390(3) . ?
C45 C50 1.395(3) . ?
C46 H46 0.9300 . ?
C46 C47 1.389(3) . ?
C47 H47 0.9300 . ?
C47 C48 1.386(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.389(3) . ?
C49 H49 0.9300 . ?
C49 C50 1.389(3) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Si1 C2 105.99(8) . . ?
F1 Si1 C23 106.08(9) . . ?
F1 Si1 C24 107.87(11) . . ?
C23 Si1 C2 113.40(10) . . ?
C23 Si1 C24 112.20(12) . . ?
C24 Si1 C2 110.83(10) . . ?
F2A Si2A C9 106.29(9) . . ?
F2A Si2A C25A 104.98(13) . . ?
F2A Si2A C26A 106.00(18) . . ?
C25A Si2A C9 114.49(11) . . ?
C25A Si2A C26A 110.98(14) . . ?
C26A Si2A C9 113.25(13) . . ?
F2B Si2B C9 109.8(8) . . ?
F2B Si2B C25B 102.4(15) . . ?
F2B Si2B C26B 116.1(17) . . ?
C25B Si2B C9 103.3(10) . . ?
C25B Si2B C26B 101.0(15) . . ?
C26B Si2B C9 120.9(14) . . ?
F3 Si3 C16 104.37(7) . . ?
F3 Si3 C27 107.32(9) . . ?
F3 Si3 C28 106.82(10) . . ?
C27 Si3 C16 110.34(9) . . ?
C28 Si3 C16 115.09(9) . . ?
C28 Si3 C27 112.23(11) . . ?
C2 C1 H1 111.1 . . ?
C2 C1 C9 108.19(14) . . ?
C2 C1 C16 107.56(14) . . ?
C9 C1 H1 111.1 . . ?
C16 C1 H1 111.1 . . ?
C16 C1 C9 107.65(14) . . ?
C1 C2 Si1 113.37(12) . . ?
C3 C2 Si1 109.93(12) . . ?
C3 C2 C1 103.60(14) . . ?
C22 C2 Si1 114.39(13) . . ?
C22 C2 C1 103.90(14) . . ?
C22 C2 C3 111.01(14) . . ?
C4 C3 C2 127.26(18) . . ?
C8 C3 C2 112.38(15) . . ?
C8 C3 C4 120.35(17) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.42(19) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.21(18) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.59(18) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C8 119.36(19) . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C7 120.06(17) . . ?
C3 C8 C9 112.63(16) . . ?
C7 C8 C9 127.26(18) . . ?
C1 C9 Si2A 113.22(12) . . ?
C1 C9 Si2B 115.5(3) . . ?
C8 C9 Si2A 110.69(13) . . ?
C8 C9 Si2B 123.8(3) . . ?
C8 C9 C1 103.09(14) . . ?
C10 C9 Si2A 115.10(13) . . ?
C10 C9 Si2B 98.9(4) . . ?
C10 C9 C1 103.50(14) . . ?
C10 C9 C8 110.40(15) . . ?
C11 C10 C9 127.62(17) . . ?
C11 C10 C15 119.64(18) . . ?
C15 C10 C9 112.59(16) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.63(19) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.67(19) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.02(19) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.62(19) . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C16 112.01(16) . . ?
C14 C15 C10 120.42(18) . . ?
C14 C15 C16 127.51(17) . . ?
C1 C16 Si3 111.15(12) . . ?
C15 C16 Si3 112.49(12) . . ?
C15 C16 C1 104.18(14) . . ?
C15 C16 C17 112.70(15) . . ?
C17 C16 Si3 111.75(12) . . ?
C17 C16 C1 103.98(14) . . ?
C18 C17 C16 127.63(17) . . ?
C18 C17 C22 120.24(17) . . ?
C22 C17 C16 112.09(16) . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.32(18) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.54(18) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.36(18) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.32(18) . . ?
C22 C21 H21 120.3 . . ?
C17 C22 C2 112.14(16) . . ?
C21 C22 C2 127.56(17) . . ?
C21 C22 C17 120.12(17) . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2A C25A H25A 109.5 . . ?
Si2A C25A H25B 109.5 . . ?
Si2A C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
Si2A C26A H26A 109.5 . . ?
Si2A C26A H26B 109.5 . . ?
Si2A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
Si2B C25B H25D 109.5 . . ?
Si2B C25B H25E 109.5 . . ?
Si2B C25B H25F 109.5 . . ?
H25D C25B H25E 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
Si2B C26B H26D 109.5 . . ?
Si2B C26B H26E 109.5 . . ?
Si2B C26B H26F 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
Si3 C27 H27A 109.5 . . ?
Si3 C27 H27B 109.5 . . ?
Si3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si3 C28 H28A 109.5 . . ?
Si3 C28 H28B 109.5 . . ?
Si3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
F4 Si4 C30 105.49(8) . . ?
F4 Si4 C51 106.21(12) . . ?
F4 Si4 C52 108.69(14) . . ?
C51 Si4 C30 115.42(10) . . ?
C52 Si4 C30 111.16(13) . . ?
C52 Si4 C51 109.51(12) . . ?
F5A Si5A C37 104.9(17) . . ?
F5A Si5A C53 95.2(17) . . ?
F5A Si5A C54A 107.7(18) . . ?
C53 Si5A C37 114.4(16) . . ?
C54A Si5A C37 115.8(18) . . ?
C54A Si5A C53 115.8(19) . . ?
F5B Si5B C37 106.0(19) . . ?
F5B Si5B C53 118(2) . . ?
F5B Si5B C54B 107.0(16) . . ?
C37 Si5B C54B 110.4(18) . . ?
C53 Si5B C37 115.1(16) . . ?
C53 Si5B C54B 100.3(16) . . ?
F6A Si6 C44 108.11(10) . . ?
F6A Si6 C55 110.47(13) . . ?
F6B Si6 C44 106.84(10) . . ?
F6B Si6 C55 109.74(14) . . ?
C55 Si6 C44 111.98(11) . . ?
C30 C29 H29 111.2 . . ?
C30 C29 C37 107.79(15) . . ?
C37 C29 H29 111.2 . . ?
C44 C29 H29 111.2 . . ?
C44 C29 C30 107.47(14) . . ?
C44 C29 C37 107.76(15) . . ?
C29 C30 Si4 112.52(12) . . ?
C31 C30 Si4 111.60(13) . . ?
C31 C30 C29 103.86(15) . . ?
C31 C30 C50 112.42(15) . . ?
C50 C30 Si4 111.95(13) . . ?
C50 C30 C29 103.99(14) . . ?
C32 C31 C30 127.43(18) . . ?
C32 C31 C36 120.21(18) . . ?
C36 C31 C30 112.29(16) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 C31 119.6(2) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.26(19) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.3(2) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.8(2) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 C37 112.47(17) . . ?
C35 C36 C31 119.88(18) . . ?
C35 C36 C37 127.46(18) . . ?
C29 C37 Si5A 112.9(10) . . ?
C29 C37 Si5B 113.5(10) . . ?
C36 C37 Si5A 114.6(9) . . ?
C36 C37 Si5B 114.6(9) . . ?
C36 C37 C29 103.54(15) . . ?
C38 C37 Si5A 111.1(10) . . ?
C38 C37 Si5B 110.4(10) . . ?
C38 C37 C29 103.69(15) . . ?
C38 C37 C36 110.36(16) . . ?
C39 C38 C37 127.4(2) . . ?
C43 C38 C37 112.26(18) . . ?
C43 C38 C39 120.4(2) . . ?
C38 C39 H39 120.4 . . ?
C40 C39 C38 119.3(2) . . ?
C40 C39 H39 120.4 . . ?
C39 C40 H40 119.9 . . ?
C41 C40 C39 120.3(2) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.5(2) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 120.2 . . ?
C43 C42 C41 119.6(2) . . ?
C43 C42 H42 120.2 . . ?
C38 C43 C44 112.55(17) . . ?
C42 C43 C38 120.0(2) . . ?
C42 C43 C44 127.41(19) . . ?
C29 C44 Si6 112.38(12) . . ?
C43 C44 Si6 112.20(13) . . ?
C43 C44 C29 103.73(15) . . ?
C43 C44 C45 112.48(15) . . ?
C45 C44 Si6 111.48(13) . . ?
C45 C44 C29 104.05(15) . . ?
C46 C45 C44 127.94(18) . . ?
C46 C45 C50 119.90(18) . . ?
C50 C45 C44 112.12(16) . . ?
C45 C46 H46 120.2 . . ?
C47 C46 C45 119.65(19) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 H47 119.8 . . ?
C48 C47 C46 120.43(19) . . ?
C48 C47 H47 119.8 . . ?
C47 C48 H48 119.9 . . ?
C47 C48 C49 120.10(19) . . ?
C49 C48 H48 119.9 . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.74(19) . . ?
C50 C49 H49 120.1 . . ?
C45 C50 C30 112.29(16) . . ?
C49 C50 C30 127.51(17) . . ?
C49 C50 C45 120.17(17) . . ?
Si4 C51 H51A 109.5 . . ?
Si4 C51 H51B 109.5 . . ?
Si4 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
Si4 C52 H52A 109.5 . . ?
Si4 C52 H52B 109.5 . . ?
Si4 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
Si5A C53 H53A 109.5 . . ?
Si5A C53 H53B 109.5 . . ?
Si5A C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si5A C54A H54A 109.5 . . ?
Si5A C54A H54B 109.5 . . ?
Si5A C54A H54C 109.5 . . ?
H54A C54A H54B 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
Si5B C54B H54D 109.5 . . ?
Si5B C54B H54E 109.5 . . ?
Si5B C54B H54F 109.5 . . ?
H54D C54B H54E 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
Si6 C55 H55A 109.5 . . ?
Si6 C55 H55B 109.5 . . ?
Si6 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 -4 4 0.1137 -4.9341 -3.9956 4.0259 -0.2938 0.4029 -0.5435
5 4 -4 0.1137 4.9341 3.9956 -4.0259 0.2938 -0.4029 0.5435
5 0 1 0.0812 5.0037 0.0120 0.9886 0.1425 -0.2136 -0.1765
-5 0 -1 0.0759 -5.0037 -0.0120 -0.9886 -0.1425 0.2136 0.1765
-2 0 5 0.0314 -1.9757 0.0097 4.9922 -0.2926 -0.1752 -0.2032
2 0 -5 0.0244 1.9757 -0.0097 -4.9922 0.2926 0.1752 0.2032
5 -3 0 0.1256 5.0332 -2.9885 0.0103 0.2362 0.1576 -0.4757
-5 3 0 0.1256 -5.0332 2.9885 -0.0103 -0.2362 -0.1576 0.4757

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound15
_database_code_depnum_ccdc_archive 'CCDC 1514276'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-07-21
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C31 H31 F9 Si3, Cl3 Sb'
_chemical_formula_sum            'C31 H31 Cl3 F9 Sb Si3'
_chemical_formula_weight         886.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H31 Cl3 F9 Sb Si3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   14.3167(4)
_cell_length_b                   14.3167(4)
_cell_length_c                   10.44916(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1854.80(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25281
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      71.7310
_cell_measurement_theta_min      3.5320
_exptl_absorpt_coefficient_mu    9.426
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             884
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0614
3 -5 3 0.0912
5 4 1 0.0785
-1 0 0 0.0614
-2 4 5 0.1312
2 -4 -5 0.1312
-3 5 -3 0.0912
-4 5 0 0.0952
5 -3 1 0.0641
4 -5 0 0.0952
-5 -4 -1 0.0785

_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.123
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9994 -0.0028 -0.0008 0.0126 0.0437 0.1154
3.0058 -5.0256 2.9743 0.0372 0.6711 -0.1911
5.0165 3.9642 1.0167 0.4624 0.0538 0.8622
-0.9994 0.0028 0.0008 -0.0126 -0.0437 -0.1154
-1.9485 3.9414 5.0245 0.8436 0.0627 -0.1152
1.9485 -3.9414 -5.0245 -0.8436 -0.0627 0.1152
-3.0058 5.0256 -2.9743 -0.0372 -0.6711 0.1911
-3.9823 4.9968 0.0282 0.3023 -0.4788 -0.0516
4.9953 -3.0158 0.9816 -0.0313 0.4795 0.2885
3.9823 -4.9968 -0.0282 -0.3023 0.4788 0.0516
-5.0165 -3.9642 -1.0167 -0.4624 -0.0538 -0.8622

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            65175
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         3.565
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  30.00   1.00    3.50    --  -38.50  57.00  60.00   94
  2  ω    -64.00  30.00   1.00    3.50    --  -38.50  57.00-180.00   94
  3  ω    -64.00  30.00   1.00    3.50    --  -38.50  57.00 -60.00   94
  4  ω     13.00 115.00   1.00    3.50    --   43.45  77.00 -30.00  102
  5  ω     13.00 115.00   1.00    3.50    --   43.45  77.00  30.00  102
  6  ω     13.00 115.00   1.00    3.50    --   43.45  77.00-150.00  102
  7  ω     23.00 114.00   1.00    3.50    --   43.45  38.00 -60.00   91
  8  ω     13.00 115.00   1.00    3.50    --   43.45  77.00 -90.00  102
  9  ω     13.00 115.00   1.00    3.50    --   43.45  77.00 150.00  102
 10  ω     23.00  97.00   1.00    3.50    --   43.45-125.00 -90.00   74
 11  ω     23.00 114.00   1.00    3.50    --   43.45  38.00-180.00   91
 12  ω     23.00  97.00   1.00    3.50    --   43.45-125.00  90.00   74
 13  ω     13.00 115.00   1.00    3.50    --   43.45  77.00  90.00  102
 14  ω     23.00 114.00   1.00    3.50    --   43.45  38.00  60.00   91
 15  ω     31.00 109.00   1.00   33.00    --  111.00 -94.00 -60.00   78
 16  ω     85.00 178.00   1.00   33.00    --  111.00  61.00 150.00   93
 17  ω     40.00 141.00   1.00   33.00    --  111.00 -77.00  60.00  101
 18  ω     81.00 178.00   1.00   33.00    --  111.00  77.00-150.00   97
 19  ω     41.00 122.00   1.00   33.00    --  111.00-125.00-120.00   81
 20  ω     41.00 133.00   1.00   33.00    --  111.00 -45.00  60.00   92
 21  ω     81.00 178.00   1.00   33.00    --  111.00  77.00  90.00   97
 22  ω     85.00 178.00   1.00   33.00    --  111.00  61.00  60.00   93
 23  ω     31.00 109.00   1.00   33.00    --  111.00 -94.00-120.00   78
 24  ω     81.00 178.00   1.00   33.00    --  111.00  77.00  30.00   97
 25  ω     85.00 178.00   1.00   33.00    --  111.00  61.00 -90.00   93
 26  ω     82.00 178.00   1.00   33.00    --  111.00  72.00  76.59   96
 27  ω     81.00 178.00   1.00   33.00    --  111.00  77.00-120.00   97
 28  ω     31.00 109.00   1.00   33.00    --  111.00 -94.00  30.00   78
 29  ω     85.00 178.00   1.00   33.00    --  111.00  61.00  30.00   93
 30  ω     85.00 178.00   1.00   33.00    --  111.00  61.00 -60.00   93
 31  ω     85.00 178.00   1.00   33.00    --  111.00  61.00-150.00   93
 32  ω     85.00 178.00   1.00   33.00    --  111.00  61.00 120.00   93
 33  ω     81.00 178.00   1.00   33.00    --  111.00  77.00  60.00   97
 34  ω     81.00 178.00   1.00   33.00    --  111.00  77.00 -90.00   97
 35  ω     81.00 178.00   1.00   33.00    --  111.00  77.00-180.00   97
 36  ω     81.00 178.00   1.00   33.00    --  111.00  77.00 150.00   97
 37  ω     81.00 178.00   1.00   33.00    --  111.00  77.00   0.00   97
 38  ω     85.00 178.00   1.00   33.00    --  111.00  61.00   0.00   93
 39  ω     81.00 178.00   1.00   33.00    --  111.00  77.00 120.00   97
 40  ω     85.00 178.00   1.00   33.00    --  111.00  61.00-120.00   93
 41  ω     85.00 178.00   1.00   33.00    --  111.00  61.00-180.00   93
 42  ω     41.00 122.00   1.00   33.00    --  111.00-125.00  30.00   81
 43  ω     81.00 178.00   1.00   33.00    --  111.00  77.00 -30.00   97
 44  ω     85.00 178.00   1.00   33.00    --  111.00  61.00 -30.00   93
 45  ω     41.00 122.00   1.00   33.00    --  111.00-125.00 150.00   81
 46  ω     84.00 178.00   1.00   33.00    --  111.00  64.00 -48.37   94
 47  ω     82.00 178.00   1.00   33.00    --  111.00  72.00 120.40   96
 48  ω   -110.00  -8.00   1.00    3.50    --  -38.50 -77.00-180.00  102
 49  ω   -107.00 -13.00   1.00    3.50    --  -38.50 -57.00-180.00   94
 50  ω     23.00 114.00   1.00    3.50    --   43.45  38.00  90.00   91
 51  ω     18.00 112.00   1.00    3.50    --   43.45  57.00-120.00   94
 52  ω     21.00 117.00   1.00    3.50    --   43.45  28.00 -24.00   96
 53  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00-180.00  171
 54  ω     18.00 112.00   1.00    3.50    --   43.45  57.00-150.00   94
 55  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00-150.00  171
 56  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00-120.00  171
 57  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00 -90.00  171
 58  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00 -60.00  171
 59  ω    -42.00 129.00   1.00    3.50    --   43.45   0.00 -30.00  171
 60  ω     23.00 114.00   1.00    3.50    --   43.45  38.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0128807000
_diffrn_orient_matrix_UB_12      0.0700936000
_diffrn_orient_matrix_UB_13      0.1179166000
_diffrn_orient_matrix_UB_21      0.0436051000
_diffrn_orient_matrix_UB_22      -0.0615123000
_diffrn_orient_matrix_UB_23      0.0776425000
_diffrn_orient_matrix_UB_31      0.1156281000
_diffrn_orient_matrix_UB_32      0.0820560000
_diffrn_orient_matrix_UB_33      -0.0424581000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1785
_reflns_number_total             2286
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0683
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1800P)²+0.1423P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2470
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.26416(13) 0.13964(15) 0.68664(16) 0.1476(7) Uani 1 1 d . . . . .
F1A F 0.1943(10) 0.0411(12) 0.5980(14) 0.208(6) Uani 0.5 1 d . . . A 1
F1B F 0.2581(16) 0.0508(7) 0.635(2) 0.274(12) Uani 0.5 1 d . . . A 2
F2A F 0.2010(14) 0.1365(6) 0.7988(16) 0.223(7) Uani 0.5 1 d . . . A 1
F2B F 0.1555(5) 0.1500(9) 0.7013(13) 0.191(4) Uani 0.5 1 d . . . A 2
F3A F 0.3233(12) 0.0782(10) 0.7652(15) 0.222(5) Uani 0.5 1 d . . . A 1
F3B F 0.2935(13) 0.1581(11) 0.8259(10) 0.212(5) Uani 0.5 1 d . . . A 2
C1 C 0.6667 0.3333 0.3809(5) 0.0895(12) Uani 1 3 d S T P . .
H1 H 0.6667 0.3333 0.4746 0.107 Uiso 1 3 calc RS T P . .
C2 C 0.5713(3) 0.3464(3) 0.3277(3) 0.0916(8) Uani 1 1 d . . . . .
C3 C 0.6275(3) 0.4469(3) 0.2454(3) 0.0972(8) Uani 1 1 d . . . . .
C4 C 0.5806(4) 0.4940(4) 0.1729(4) 0.1141(11) Uani 1 1 d . . . . .
H4 H 0.5060 0.4637 0.1722 0.137 Uiso 1 1 calc R . . . .
C5 C 0.6439(5) 0.5850(4) 0.1024(4) 0.1278(14) Uani 1 1 d . . . . .
H5 H 0.6120 0.6164 0.0547 0.153 Uiso 1 1 calc R . . . .
C6 C 0.7545(5) 0.6304(3) 0.1018(4) 0.1239(13) Uani 1 1 d . . . . .
H6 H 0.7969 0.6921 0.0536 0.149 Uiso 1 1 calc R . . . .
C7 C 0.8024(4) 0.5840(3) 0.1732(4) 0.1130(10) Uani 1 1 d . . . . .
H7 H 0.8769 0.6144 0.1735 0.136 Uiso 1 1 calc R . . . .
C8 C 0.7377(3) 0.4917(3) 0.2445(3) 0.0981(9) Uani 1 1 d . . . . .
C9 C 0.4996(3) 0.3553(3) 0.4314(3) 0.1010(9) Uani 1 1 d . . . . .
H9A H 0.5454 0.4127 0.4900 0.121 Uiso 1 1 calc R . . . .
H9B H 0.4516 0.3758 0.3907 0.121 Uiso 1 1 calc R . . . .
C10 C 0.4322(3) 0.2529(3) 0.5081(4) 0.1087(10) Uani 1 1 d . . . . .
H10A H 0.4799 0.2330 0.5506 0.130 Uiso 1 1 calc R . . . .
H10B H 0.3868 0.1950 0.4499 0.130 Uiso 1 1 calc R . . . .
C11 C 0.3609(4) 0.2646(4) 0.6085(4) 0.1222(12) Uani 1 1 d . . . . .
H11A H 0.3218 0.2956 0.5677 0.147 Uiso 1 1 calc R . . . .
H11B H 0.4070 0.3150 0.6734 0.147 Uiso 1 1 calc R . . . .
Sb1 Sb 0.6734(16) 0.3186(9) 0.93151(8) 0.169(2) Uani 0.3333 1 d . . . B -1
Cl1 Cl 0.8225(6) 0.3697(7) 0.7927(9) 0.1367(19) Uani 0.3333 1 d . . . B -1
Cl2 Cl 0.585(2) 0.1858(14) 0.801(3) 0.316(13) Uani 0.3333 1 d . . . B -1
Cl3 Cl 0.6223(16) 0.4302(12) 0.8397(14) 0.215(6) Uani 0.3333 1 d . . . B -1


_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 F1A 1.561(12) . ?
Si1 F1B 1.344(8) . ?
Si1 F2A 1.467(7) . ?
Si1 F2B 1.642(8) . ?
Si1 F3A 1.706(13) . ?
Si1 F3B 1.501(11) . ?
Si1 C11 1.819(5) . ?
C1 H1 0.9800 . ?
C1 C2 1.570(4) . ?
C1 C2 1.570(4) 3_665 ?
C1 C2 1.570(4) 2_655 ?
C2 C3 1.516(5) . ?
C2 C8 1.529(4) 2_655 ?
C2 C9 1.540(4) . ?
C3 C4 1.391(5) . ?
C3 C8 1.373(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.378(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.392(5) . ?
C8 C2 1.529(4) 3_665 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.519(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.529(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
Sb1 Cl1 2.374(18) . ?
Sb1 Cl2 2.16(3) . ?
Sb1 Cl3 2.275(14) . ?

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
F1A Si1 F3A 94.5(8) . . ?
F1A Si1 C11 116.8(6) . . ?
F1B Si1 F2B 120.5(11) . . ?
F1B Si1 F3B 116.0(13) . . ?
F1B Si1 C11 114.0(5) . . ?
F2A Si1 F1A 109.9(8) . . ?
F2A Si1 F3A 93.3(9) . . ?
F2A Si1 C11 122.9(4) . . ?
F2B Si1 C11 104.1(4) . . ?
F3A Si1 C11 113.1(5) . . ?
F3B Si1 F2B 95.0(7) . . ?
F3B Si1 C11 104.7(5) . . ?
C2 C1 H1 110.7 3_665 . ?
C2 C1 H1 110.7 . . ?
C2 C1 H1 110.7 2_655 . ?
C2 C1 C2 108.2(2) 2_655 3_665 ?
C2 C1 C2 108.2(2) 2_655 . ?
C2 C1 C2 108.2(2) 3_665 . ?
C3 C2 C1 103.4(2) . . ?
C3 C2 C8 110.7(2) . 2_655 ?
C3 C2 C9 112.4(3) . . ?
C8 C2 C1 103.2(2) 2_655 . ?
C8 C2 C9 112.0(3) 2_655 . ?
C9 C2 C1 114.6(3) . . ?
C4 C3 C2 127.8(4) . . ?
C8 C3 C2 112.8(3) . . ?
C8 C3 C4 119.4(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C8 119.3(4) . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C2 112.4(3) . 3_665 ?
C3 C8 C7 120.7(3) . . ?
C7 C8 C2 127.0(3) . 3_665 ?
C2 C9 H9A 108.6 . . ?
C2 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
C10 C9 C2 114.8(3) . . ?
C10 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C9 C10 H10A 108.9 . . ?
C9 C10 H10B 108.9 . . ?
C9 C10 C11 113.2(3) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
Si1 C11 H11A 108.5 . . ?
Si1 C11 H11B 108.5 . . ?
C10 C11 Si1 115.0(3) . . ?
C10 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
Cl2 Sb1 Cl1 85.6(6) . . ?
Cl2 Sb1 Cl3 95.8(11) . . ?
Cl3 Sb1 Cl1 94.7(6) . . ?

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
F1A Si1 C11 C10 -48.6(9) . . . . ?
F1B Si1 C11 C10 -8.1(15) . . . . ?
F2A Si1 C11 C10 170.1(11) . . . . ?
F2B Si1 C11 C10 -141.2(6) . . . . ?
F3A Si1 C11 C10 59.5(8) . . . . ?
F3B Si1 C11 C10 119.7(7) . . . . ?
C1 C2 C3 C4 178.5(3) . . . . ?
C1 C2 C3 C8 -0.2(4) . . . . ?
C1 C2 C9 C10 -68.3(4) . . . . ?
C2 C1 C2 C3 0.7(4) 3_665 . . . ?
C2 C1 C2 C3 -116.3(2) 2_655 . . . ?
C2 C1 C2 C8 116.1(2) 3_665 . . 2_655 ?
C2 C1 C2 C8 -0.9(4) 2_655 . . 2_655 ?
C2 C1 C2 C9 121.1(4) 2_655 . . . ?
C2 C1 C2 C9 -121.9(4) 3_665 . . . ?
C2 C3 C4 C5 -179.4(4) . . . . ?
C2 C3 C8 C2 -0.3(4) . . . 3_665 ?
C2 C3 C8 C7 179.6(3) . . . . ?
C2 C9 C10 C11 -179.0(3) . . . . ?
C3 C2 C9 C10 174.0(3) . . . . ?
C3 C4 C5 C6 0.4(7) . . . . ?
C4 C3 C8 C2 -179.2(3) . . . 3_665 ?
C4 C3 C8 C7 0.8(5) . . . . ?
C4 C5 C6 C7 -0.2(7) . . . . ?
C5 C6 C7 C8 0.2(7) . . . . ?
C6 C7 C8 C2 179.4(4) . . . 3_665 ?
C6 C7 C8 C3 -0.5(6) . . . . ?
C8 C2 C3 C4 68.5(4) 2_655 . . . ?
C8 C2 C3 C8 -110.1(3) 2_655 . . . ?
C8 C2 C9 C10 48.7(4) 2_655 . . . ?
C8 C3 C4 C5 -0.7(6) . . . . ?
C9 C2 C3 C4 -57.5(4) . . . . ?
C9 C2 C3 C8 123.9(3) . . . . ?
C9 C10 C11 Si1 171.3(3) . . . . ?

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: F1A(0.5) F1B(0.5) F2A(0.5) F2B(0.5) F3A(0.5) F3B(0.5) Sb1(0.33333)
 Cl1(0.33333) Cl2(0.33333) Cl3(0.33333)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.531
_oxdiff_exptl_absorpt_empirical_full_min 0.590

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1514269'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2014-05-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H16 Br6'
_chemical_formula_sum            'C25 H16 Br6'
_chemical_formula_weight         795.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25H16Br6 '
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.4708(4)
_cell_length_b                   9.3343(2)
_cell_length_c                   18.9329(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.806(3)
_cell_angle_gamma                90
_cell_volume                     2377.77(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15779
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      25.8770
_cell_measurement_theta_min      1.8100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.144
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.0815
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101948
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.814
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000  -90.0000 98

#__ type_ start__ end____ width___ exp.time_
  2 omega    3.00   95.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   38.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000   30.0000 87

#__ type_ start__ end____ width___ exp.time_
  4 omega    6.00   83.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -130.0000   22.5926 77

#__ type_ start__ end____ width___ exp.time_
  5 omega  -46.00   47.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -38.0000   30.0000 93

#__ type_ start__ end____ width___ exp.time_
  6 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  7 omega  -46.00   47.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -38.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
  8 omega  -44.00   43.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -57.0000 -120.0000 87

#__ type_ start__ end____ width___ exp.time_
  9 omega   35.00   99.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  178.0000   60.0000 64

#__ type_ start__ end____ width___ exp.time_
 10 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
 11 omega   -2.00   77.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -120.0000 -159.4549 79

#__ type_ start__ end____ width___ exp.time_
 12 omega  -85.00   -8.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  135.0000   27.8271 77

#__ type_ start__ end____ width___ exp.time_
 13 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

#__ type_ start__ end____ width___ exp.time_
 14 omega  -20.00   65.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -99.0000   60.0000 85

#__ type_ start__ end____ width___ exp.time_
 15 omega  -20.00   65.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -99.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 16 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000  120.0000 98

#__ type_ start__ end____ width___ exp.time_
 17 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000  -30.0000 87

#__ type_ start__ end____ width___ exp.time_
 18 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
 19 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000   60.0000 87

#__ type_ start__ end____ width___ exp.time_
 20 omega   35.00   99.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  178.0000  -30.0000 64

#__ type_ start__ end____ width___ exp.time_
 21 omega   34.00  100.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -178.0000  150.0000 66

#__ type_ start__ end____ width___ exp.time_
 22 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

#__ type_ start__ end____ width___ exp.time_
 23 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 143

#__ type_ start__ end____ width___ exp.time_
 24 omega  -95.00   23.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -60.0000 118

#__ type_ start__ end____ width___ exp.time_
 25 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0025697000
_diffrn_orient_matrix_UB_12      0.0636870000
_diffrn_orient_matrix_UB_13      0.0202831000
_diffrn_orient_matrix_UB_21      0.0467921000
_diffrn_orient_matrix_UB_22      0.0217228000
_diffrn_orient_matrix_UB_23      -0.0118876000
_diffrn_orient_matrix_UB_31      -0.0241285000
_diffrn_orient_matrix_UB_32      0.0353337000
_diffrn_orient_matrix_UB_33      -0.0292329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3834
_reflns_number_total             4684
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0217P)²+4.1154P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0561
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.94236(3) 0.03032(4) 0.08640(2) 0.02042(10) Uani 1 1 d . . . . .
Br2 Br 0.78717(3) 0.23967(4) -0.00970(2) 0.02257(10) Uani 1 1 d . . . . .
Br3 Br 0.35906(3) 0.59876(4) 0.13901(2) 0.01835(9) Uani 1 1 d . . . . .
Br4 Br 0.31768(3) 0.57337(4) 0.31145(2) 0.01978(9) Uani 1 1 d . . . . .
Br5 Br 0.71155(3) 0.24221(4) 0.51922(2) 0.01967(9) Uani 1 1 d . . . . .
Br6 Br 0.89818(3) 0.06403(4) 0.44627(2) 0.02075(10) Uani 1 1 d . . . . .
C1 C 0.5122(3) -0.0443(4) 0.22963(18) 0.0134(8) Uani 1 1 d . . . . .
H1 H 0.4693 -0.1284 0.2226 0.016 Uiso 1 1 calc R . . . .
C2 C 0.6235(3) -0.0908(4) 0.24135(18) 0.0125(8) Uani 1 1 d . . . . .
C3 C 0.6738(3) -0.0218(4) 0.17956(18) 0.0117(7) Uani 1 1 d . . . . .
C4 C 0.7718(3) -0.0363(4) 0.16229(19) 0.0150(8) Uani 1 1 d . . . . .
H4 H 0.8141 -0.0975 0.1882 0.018 Uiso 1 1 calc R . . . .
C5 C 0.8064(3) 0.0413(4) 0.10593(18) 0.0122(7) Uani 1 1 d . . . . .
C6 C 0.7421(3) 0.1306(4) 0.06716(19) 0.0149(8) Uani 1 1 d . . . . .
C7 C 0.6431(3) 0.1424(4) 0.08285(18) 0.0139(8) Uani 1 1 d . . . . .
H7 H 0.6002 0.2007 0.0558 0.017 Uiso 1 1 calc R . . . .
C8 C 0.6090(3) 0.0660(4) 0.13957(18) 0.0124(8) Uani 1 1 d . . . . .
C9 C 0.5033(3) 0.0562(4) 0.16345(18) 0.0122(8) Uani 1 1 d . . . . .
C10 C 0.4613(3) 0.1935(4) 0.19234(18) 0.0117(7) Uani 1 1 d . . . . .
C11 C 0.4343(3) 0.3173(4) 0.15534(19) 0.0133(8) Uani 1 1 d . . . . .
H11 H 0.4436 0.3234 0.1071 0.016 Uiso 1 1 calc R . . . .
C12 C 0.3936(3) 0.4315(4) 0.19065(19) 0.0123(8) Uani 1 1 d . . . . .
C13 C 0.3774(3) 0.4215(4) 0.26283(19) 0.0144(8) Uani 1 1 d . . . . .
C14 C 0.4037(3) 0.2980(4) 0.30021(19) 0.0146(8) Uani 1 1 d . . . . .
H14 H 0.3925 0.2909 0.3482 0.018 Uiso 1 1 calc R . . . .
C15 C 0.4470(3) 0.1851(4) 0.26479(18) 0.0118(7) Uani 1 1 d . . . . .
C16 C 0.4819(3) 0.0430(4) 0.29595(19) 0.0120(7) Uani 1 1 d . . . . .
C17 C 0.5791(3) 0.0574(4) 0.33991(18) 0.0117(7) Uani 1 1 d . . . . .
C18 C 0.5953(3) 0.1328(4) 0.40257(18) 0.0140(8) Uani 1 1 d . . . . .
H18 H 0.5435 0.1820 0.4224 0.017 Uiso 1 1 calc R . . . .
C19 C 0.6897(3) 0.1338(4) 0.43523(18) 0.0144(8) Uani 1 1 d . . . . .
C20 C 0.7666(3) 0.0586(4) 0.40596(19) 0.0135(8) Uani 1 1 d . . . . .
C21 C 0.7508(3) -0.0193(4) 0.34396(19) 0.0150(8) Uani 1 1 d . . . . .
H21 H 0.8021 -0.0712 0.3251 0.018 Uiso 1 1 calc R . . . .
C22 C 0.6564(3) -0.0180(4) 0.31069(18) 0.0116(7) Uani 1 1 d . . . . .
C23 C 0.6373(3) -0.2532(4) 0.2445(2) 0.0193(9) Uani 1 1 d . . . . .
H23A H 0.5991 -0.2918 0.2816 0.029 Uiso 1 1 calc GR . . . .
H23B H 0.7063 -0.2750 0.2539 0.029 Uiso 1 1 calc GR . . . .
H23C H 0.6151 -0.2946 0.2001 0.029 Uiso 1 1 calc GR . . . .
C24 C 0.4351(3) -0.0061(4) 0.10299(19) 0.0168(8) Uani 1 1 d . . . . .
H24A H 0.3695 -0.0197 0.1194 0.025 Uiso 1 1 calc GR . . . .
H24B H 0.4612 -0.0964 0.0883 0.025 Uiso 1 1 calc GR . . . .
H24C H 0.4324 0.0592 0.0637 0.025 Uiso 1 1 calc GR . . . .
C25 C 0.4033(3) -0.0325(4) 0.33842(19) 0.0164(8) Uani 1 1 d . . . . .
H25A H 0.4281 -0.1240 0.3543 0.025 Uiso 1 1 calc GR . . . .
H25B H 0.3439 -0.0459 0.3090 0.025 Uiso 1 1 calc GR . . . .
H25C H 0.3885 0.0251 0.3786 0.025 Uiso 1 1 calc GR . . . .


_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 C5 1.888(4) . ?
Br2 C6 1.900(4) . ?
Br3 C12 1.888(3) . ?
Br4 C13 1.892(4) . ?
Br5 C19 1.896(3) . ?
Br6 C20 1.896(3) . ?
C1 H1 0.9800 . ?
C1 C2 1.566(5) . ?
C1 C9 1.565(5) . ?
C1 C16 1.567(5) . ?
C2 C3 1.524(5) . ?
C2 C22 1.525(5) . ?
C2 C23 1.527(5) . ?
C3 C4 1.381(5) . ?
C3 C8 1.394(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(5) . ?
C5 C6 1.386(5) . ?
C6 C7 1.385(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.386(5) . ?
C8 C9 1.518(5) . ?
C9 C10 1.514(5) . ?
C9 C24 1.546(5) . ?
C10 C11 1.390(5) . ?
C10 C15 1.397(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(5) . ?
C12 C13 1.398(5) . ?
C13 C14 1.389(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(5) . ?
C15 C16 1.518(5) . ?
C16 C17 1.523(5) . ?
C16 C25 1.532(5) . ?
C17 C18 1.387(5) . ?
C17 C22 1.393(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.387(5) . ?
C19 C20 1.388(5) . ?
C20 C21 1.388(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.391(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 110.5 . . ?
C2 C1 C16 108.4(3) . . ?
C9 C1 H1 110.5 . . ?
C9 C1 C2 108.4(3) . . ?
C9 C1 C16 108.5(3) . . ?
C16 C1 H1 110.5 . . ?
C3 C2 C1 103.5(3) . . ?
C3 C2 C22 110.6(3) . . ?
C3 C2 C23 113.1(3) . . ?
C22 C2 C1 103.5(3) . . ?
C22 C2 C23 112.3(3) . . ?
C23 C2 C1 113.2(3) . . ?
C4 C3 C2 127.3(3) . . ?
C4 C3 C8 120.6(3) . . ?
C8 C3 C2 112.1(3) . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 Br1 119.2(3) . . ?
C6 C5 Br1 121.1(3) . . ?
C6 C5 C4 119.7(3) . . ?
C5 C6 Br2 120.8(3) . . ?
C7 C6 Br2 117.9(3) . . ?
C7 C6 C5 121.2(3) . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C8 119.0(3) . . ?
C8 C7 H7 120.5 . . ?
C3 C8 C9 112.0(3) . . ?
C7 C8 C3 120.1(3) . . ?
C7 C8 C9 127.8(3) . . ?
C8 C9 C1 103.8(3) . . ?
C8 C9 C24 109.5(3) . . ?
C10 C9 C1 103.5(3) . . ?
C10 C9 C8 115.4(3) . . ?
C10 C9 C24 111.5(3) . . ?
C24 C9 C1 112.8(3) . . ?
C11 C10 C9 127.9(3) . . ?
C11 C10 C15 119.7(3) . . ?
C15 C10 C9 112.3(3) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 Br3 118.7(3) . . ?
C11 C12 C13 120.3(3) . . ?
C13 C12 Br3 121.0(3) . . ?
C12 C13 Br4 121.1(3) . . ?
C14 C13 Br4 118.5(3) . . ?
C14 C13 C12 120.4(3) . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 119.0(3) . . ?
C15 C14 H14 120.5 . . ?
C10 C15 C16 112.1(3) . . ?
C14 C15 C10 120.8(3) . . ?
C14 C15 C16 127.1(3) . . ?
C15 C16 C1 103.3(3) . . ?
C15 C16 C17 112.1(3) . . ?
C15 C16 C25 113.4(3) . . ?
C17 C16 C1 103.5(3) . . ?
C17 C16 C25 110.6(3) . . ?
C25 C16 C1 113.3(3) . . ?
C18 C17 C16 127.4(3) . . ?
C18 C17 C22 120.4(3) . . ?
C22 C17 C16 112.2(3) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.2(3) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 Br5 118.6(3) . . ?
C18 C19 C20 120.3(3) . . ?
C20 C19 Br5 121.1(3) . . ?
C19 C20 Br6 121.8(3) . . ?
C19 C20 C21 121.1(3) . . ?
C21 C20 Br6 117.1(3) . . ?
C20 C21 H21 120.8 . . ?
C20 C21 C22 118.5(3) . . ?
C22 C21 H21 120.8 . . ?
C17 C22 C2 112.1(3) . . ?
C21 C22 C2 127.3(3) . . ?
C21 C22 C17 120.6(3) . . ?
C2 C23 H23A 109.5 . . ?
C2 C23 H23B 109.5 . . ?
C2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C9 C24 H24A 109.5 . . ?
C9 C24 H24B 109.5 . . ?
C9 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C16 C25 H25A 109.5 . . ?
C16 C25 H25B 109.5 . . ?
C16 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C5 C6 Br2 2.5(4) . . . . ?
Br1 C5 C6 C7 -177.9(3) . . . . ?
Br2 C6 C7 C8 -178.7(3) . . . . ?
Br3 C12 C13 Br4 1.3(4) . . . . ?
Br3 C12 C13 C14 -179.7(3) . . . . ?
Br4 C13 C14 C15 179.5(3) . . . . ?
Br5 C19 C20 Br6 -1.9(4) . . . . ?
Br5 C19 C20 C21 -179.2(3) . . . . ?
Br6 C20 C21 C22 -176.0(3) . . . . ?
C1 C2 C3 C4 -175.8(3) . . . . ?
C1 C2 C3 C8 5.5(4) . . . . ?
C1 C2 C22 C17 2.0(4) . . . . ?
C1 C2 C22 C21 -177.1(3) . . . . ?
C1 C9 C10 C11 -176.8(3) . . . . ?
C1 C9 C10 C15 0.9(4) . . . . ?
C1 C16 C17 C18 176.1(3) . . . . ?
C1 C16 C17 C22 -4.8(4) . . . . ?
C2 C1 C9 C8 -0.6(4) . . . . ?
C2 C1 C9 C10 -121.5(3) . . . . ?
C2 C1 C9 C24 117.8(3) . . . . ?
C2 C1 C16 C15 122.9(3) . . . . ?
C2 C1 C16 C17 5.8(4) . . . . ?
C2 C1 C16 C25 -114.0(3) . . . . ?
C2 C3 C4 C5 -176.4(3) . . . . ?
C2 C3 C8 C7 177.3(3) . . . . ?
C2 C3 C8 C9 -6.3(4) . . . . ?
C3 C2 C22 C17 112.2(3) . . . . ?
C3 C2 C22 C21 -66.8(4) . . . . ?
C3 C4 C5 Br1 176.0(3) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C3 C8 C9 C1 4.2(4) . . . . ?
C3 C8 C9 C10 116.7(3) . . . . ?
C3 C8 C9 C24 -116.5(3) . . . . ?
C4 C3 C8 C7 -1.5(5) . . . . ?
C4 C3 C8 C9 174.9(3) . . . . ?
C4 C5 C6 Br2 179.4(3) . . . . ?
C4 C5 C6 C7 -0.9(5) . . . . ?
C5 C6 C7 C8 1.6(5) . . . . ?
C6 C7 C8 C3 -0.4(5) . . . . ?
C6 C7 C8 C9 -176.1(3) . . . . ?
C7 C8 C9 C1 -179.8(3) . . . . ?
C7 C8 C9 C10 -67.3(5) . . . . ?
C7 C8 C9 C24 59.5(5) . . . . ?
C8 C3 C4 C5 2.2(5) . . . . ?
C8 C9 C10 C11 70.5(5) . . . . ?
C8 C9 C10 C15 -111.8(3) . . . . ?
C9 C1 C2 C3 -2.7(4) . . . . ?
C9 C1 C2 C22 112.7(3) . . . . ?
C9 C1 C2 C23 -125.5(3) . . . . ?
C9 C1 C16 C15 5.4(4) . . . . ?
C9 C1 C16 C17 -111.7(3) . . . . ?
C9 C1 C16 C25 128.5(3) . . . . ?
C9 C10 C11 C12 177.7(3) . . . . ?
C9 C10 C15 C14 -176.4(3) . . . . ?
C9 C10 C15 C16 2.7(4) . . . . ?
C10 C11 C12 Br3 179.3(3) . . . . ?
C10 C11 C12 C13 -1.6(5) . . . . ?
C10 C15 C16 C1 -5.1(4) . . . . ?
C10 C15 C16 C17 105.8(3) . . . . ?
C10 C15 C16 C25 -128.1(3) . . . . ?
C11 C10 C15 C14 1.5(5) . . . . ?
C11 C10 C15 C16 -179.4(3) . . . . ?
C11 C12 C13 Br4 -177.8(3) . . . . ?
C11 C12 C13 C14 1.2(5) . . . . ?
C12 C13 C14 C15 0.5(5) . . . . ?
C13 C14 C15 C10 -1.8(5) . . . . ?
C13 C14 C15 C16 179.2(3) . . . . ?
C14 C15 C16 C1 174.0(3) . . . . ?
C14 C15 C16 C17 -75.2(5) . . . . ?
C14 C15 C16 C25 51.0(5) . . . . ?
C15 C10 C11 C12 0.2(5) . . . . ?
C15 C16 C17 C18 65.4(5) . . . . ?
C15 C16 C17 C22 -115.5(3) . . . . ?
C16 C1 C2 C3 -120.3(3) . . . . ?
C16 C1 C2 C22 -4.9(4) . . . . ?
C16 C1 C2 C23 117.0(3) . . . . ?
C16 C1 C9 C8 116.9(3) . . . . ?
C16 C1 C9 C10 -4.0(4) . . . . ?
C16 C1 C9 C24 -124.7(3) . . . . ?
C16 C17 C18 C19 -179.9(3) . . . . ?
C16 C17 C22 C2 1.8(4) . . . . ?
C16 C17 C22 C21 -179.1(3) . . . . ?
C17 C18 C19 Br5 178.0(3) . . . . ?
C17 C18 C19 C20 -0.9(5) . . . . ?
C18 C17 C22 C2 -178.9(3) . . . . ?
C18 C17 C22 C21 0.2(5) . . . . ?
C18 C19 C20 Br6 177.0(3) . . . . ?
C18 C19 C20 C21 -0.3(5) . . . . ?
C19 C20 C21 C22 1.4(5) . . . . ?
C20 C21 C22 C2 177.6(3) . . . . ?
C20 C21 C22 C17 -1.4(5) . . . . ?
C22 C2 C3 C4 73.9(4) . . . . ?
C22 C2 C3 C8 -104.8(3) . . . . ?
C22 C17 C18 C19 0.9(5) . . . . ?
C23 C2 C3 C4 -52.9(5) . . . . ?
C23 C2 C3 C8 128.4(3) . . . . ?
C23 C2 C22 C17 -120.5(3) . . . . ?
C23 C2 C22 C21 60.4(5) . . . . ?
C24 C9 C10 C11 -55.3(5) . . . . ?
C24 C9 C10 C15 122.4(3) . . . . ?
C25 C16 C17 C18 -62.3(5) . . . . ?
C25 C16 C17 C22 116.9(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7 11 8 0.0033 7.0249 11.4242 8.3238 0.8784 0.4779 -0.0092
-4 -13 0 0.0633 -3.6901 -12.9020 -0.4431 -0.8212 -0.4477 -0.3539
-15 6 -8 0.0118 -15.4551 6.1859 -8.0547 0.2703 -0.4930 0.8269
-12 -2 -20 0.0128 -11.9969 -2.0033 -20.0042 -0.5025 -0.3671 0.8035
10 1 -23 0.0037 10.4164 1.0480 -22.9081 -0.4247 0.7825 0.4554
-10 -1 23 0.0073 -10.4164 -1.0480 22.9081 0.4247 -0.7825 -0.4554
10 1 22 0.0096 10.3738 0.5437 21.5879 0.4458 0.2406 -0.8622

_olex2_exptl_crystal_mounting_method mounted
