data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. P. G. Taylor
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C104 H96 Cl40 O28 Si8'
_chemical_formula_weight          3436.53
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.7863(9)
_cell_length_b                    18.4652(15)
_cell_length_c                    19.0801(19)
_cell_angle_alpha                 68.711(4)
_cell_angle_beta                  81.679(5)
_cell_angle_gamma                 82.351(7)
_cell_volume                      3490.2(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     9507
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.635
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1736
_exptl_absorpt_coefficient_mu     0.910
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8832
_exptl_absorpt_correction_T_max   0.9732
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             32442
_diffrn_reflns_av_R_equivalents   0.2458
_diffrn_reflns_av_sigmaI/netI     0.5300
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.55
_reflns_number_total              12068
_reflns_number_gt                 3235
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_computing_publication_material   ? 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0320P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          12068
_refine_ls_number_parameters      819
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.3570
_refine_ls_R_factor_gt            0.0794
_refine_ls_wR_factor_ref          0.1680
_refine_ls_wR_factor_gt           0.1098
_refine_ls_goodness_of_fit_ref    0.859
_refine_ls_restrained_S_all       0.859
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Si1 Si 0.7819(3) 0.44005(18) 0.50518(15) 0.0353(9) Uani 1 1 d . . .
Si2 Si 0.8167(3) 0.55474(18) 0.58629(15) 0.0340(8) Uani 1 1 d . . .
Si3 Si 1.0680(3) 0.45691(18) 0.64133(15) 0.0338(8) Uani 1 1 d . . .
Si4 Si 1.0328(3) 0.34245(18) 0.56036(15) 0.0338(8) Uani 1 1 d . . .
Cl9 Cl 0.6310(3) 0.1519(2) 0.45894(18) 0.0759(11) Uani 1 1 d . . .
Cl10 Cl 0.7390(3) 0.0053(2) 0.41829(18) 0.0812(12) Uani 1 1 d . . .
Cl11 Cl 0.7143(3) -0.1617(2) 0.53918(19) 0.0807(11) Uani 1 1 d . . .
Cl12 Cl 0.5697(3) -0.1802(2) 0.69840(18) 0.0763(11) Uani 1 1 d . . .
Cl13 Cl 0.4555(3) -0.0307(2) 0.73493(17) 0.0747(11) Uani 1 1 d . . .
Cl22 Cl 0.4377(3) 0.32645(18) 0.96566(15) 0.0534(9) Uani 1 1 d . . .
Cl23 Cl 0.5505(3) 0.18708(18) 1.09787(16) 0.0581(9) Uani 1 1 d . . .
Cl24 Cl 0.7694(3) 0.21152(18) 1.17592(15) 0.0590(9) Uani 1 1 d . . .
Cl25 Cl 0.8713(3) 0.37574(18) 1.12190(15) 0.0542(9) Uani 1 1 d . . .
Cl26 Cl 0.7550(3) 0.51317(17) 0.99069(14) 0.0509(8) Uani 1 1 d . . .
Cl35 Cl 0.6198(3) 0.22678(19) 0.84164(16) 0.0679(10) Uani 1 1 d . . .
Cl36 Cl 0.5320(3) 0.0662(2) 0.85130(16) 0.0728(11) Uani 1 1 d . . .
Cl37 Cl 0.6359(3) -0.0887(2) 0.97030(16) 0.0718(10) Uani 1 1 d . . .
Cl38 Cl 0.8239(3) -0.08231(19) 1.07629(17) 0.0730(10) Uani 1 1 d . . .
Cl39 Cl 0.8996(3) 0.0771(2) 1.06901(16) 0.0678(10) Uani 1 1 d . . .
Cl48 Cl 1.0331(3) -0.11614(19) 0.55073(16) 0.0677(10) Uani 1 1 d . . .
Cl49 Cl 1.0524(3) -0.3003(2) 0.60995(18) 0.0775(11) Uani 1 1 d . . .
Cl50 Cl 0.9223(3) -0.39046(18) 0.76948(17) 0.0665(10) Uani 1 1 d . . .
Cl51 Cl 0.7812(3) -0.29932(19) 0.87008(17) 0.0718(10) Uani 1 1 d . . .
Cl52 Cl 0.7771(3) -0.11808(19) 0.81190(18) 0.0715(10) Uani 1 1 d . . .
O1 O 0.7575(6) 0.5001(4) 0.5521(3) 0.0362(19) Uani 1 1 d . . .
O2 O 0.9322(6) 0.5045(4) 0.6343(3) 0.0365(18) Uani 1 1 d . . .
O3 O 1.0659(6) 0.3798(4) 0.6201(3) 0.0326(18) Uani 1 1 d . . .
O4 O 0.8900(6) 0.3724(4) 0.5401(3) 0.0350(18) Uani 1 1 d . . .
O5 O 0.8283(6) 0.4884(4) 0.4183(3) 0.0362(18) Uani 1 1 d . . .
O6 O 0.8733(6) 0.6271(4) 0.5169(3) 0.0338(18) Uani 1 1 d . . .
O7 O 0.6722(9) 0.1307(5) 0.6470(5) 0.073(3) Uani 1 1 d . . .
O8 O 0.4923(7) 0.1159(5) 0.6116(4) 0.061(2) Uani 1 1 d . . .
O9 O 0.7058(8) 0.4600(5) 0.8454(4) 0.057(2) Uani 1 1 d . . .
O10 O 0.5486(6) 0.4748(4) 0.9315(4) 0.044(2) Uani 1 1 d . . .
O11 O 0.9544(7) 0.2026(4) 0.8749(4) 0.048(2) Uani 1 1 d . . .
O12 O 0.7861(8) 0.2122(5) 0.9557(4) 0.047(2) Uani 1 1 d . . .
O13 O 1.0695(8) -0.0622(5) 0.7258(5) 0.063(3) Uani 1 1 d . . .
O14 O 0.9027(7) -0.0476(5) 0.6600(4) 0.053(2) Uani 1 1 d . . .
C1 C 0.6367(10) 0.3962(6) 0.5133(5) 0.047(3) Uani 1 1 d . . .
H1A H 0.5649 0.4351 0.5152 0.056 Uiso 1 1 calc R . .
H1B H 0.6350 0.3837 0.4672 0.056 Uiso 1 1 calc R . .
C2 C 0.6182(10) 0.3202(7) 0.5841(6) 0.048(3) Uani 1 1 d . . .
H2A H 0.6748 0.2770 0.5750 0.057 Uiso 1 1 calc R . .
H2B H 0.6448 0.3282 0.6282 0.057 Uiso 1 1 calc R . .
C3 C 0.4841(11) 0.2951(7) 0.6047(6) 0.050(3) Uani 1 1 d . . .
C4 C 0.4050(11) 0.3477(7) 0.6429(6) 0.063(4) Uani 1 1 d . . .
H4A H 0.4028 0.4019 0.6079 0.095 Uiso 1 1 calc R . .
H4B H 0.4421 0.3436 0.6883 0.095 Uiso 1 1 calc R . .
H4C H 0.3193 0.3316 0.6571 0.095 Uiso 1 1 calc R . .
C5 C 0.4276(11) 0.2963(7) 0.5359(6) 0.071(4) Uani 1 1 d . . .
H5A H 0.4152 0.3503 0.5012 0.107 Uiso 1 1 calc R . .
H5B H 0.3465 0.2738 0.5518 0.107 Uiso 1 1 calc R . .
H5C H 0.4847 0.2657 0.5102 0.107 Uiso 1 1 calc R . .
C6 C 0.4863(11) 0.2147(8) 0.6661(7) 0.060(4) Uani 1 1 d . . .
H6A H 0.5223 0.2170 0.7100 0.072 Uiso 1 1 calc R . .
H6B H 0.3988 0.2005 0.6830 0.072 Uiso 1 1 calc R . .
C7 C 0.5604(15) 0.1523(8) 0.6414(7) 0.067(4) Uani 1 1 d . . .
C8 C 0.5551(12) 0.0504(9) 0.5962(8) 0.057(4) Uani 1 1 d . . .
C9 C 0.6170(12) 0.0563(8) 0.5267(7) 0.060(4) Uani 1 1 d . . .
C10 C 0.6680(11) -0.0093(10) 0.5081(7) 0.059(4) Uani 1 1 d . . .
C11 C 0.6510(12) -0.0831(8) 0.5628(8) 0.058(4) Uani 1 1 d . . .
C12 C 0.5927(12) -0.0887(7) 0.6327(7) 0.053(3) Uani 1 1 d . . .
C13 C 0.5375(11) -0.0231(9) 0.6487(7) 0.056(4) Uani 1 1 d . . .
C14 C 0.6942(9) 0.5908(6) 0.6460(5) 0.040(3) Uani 1 1 d . . .
H14A H 0.7347 0.6025 0.6836 0.048 Uiso 1 1 calc R . .
H14B H 0.6519 0.6402 0.6139 0.048 Uiso 1 1 calc R . .
C15 C 0.5931(9) 0.5329(6) 0.6887(5) 0.039(3) Uani 1 1 d . . .
H15A H 0.5499 0.5234 0.6508 0.046 Uiso 1 1 calc R . .
H15B H 0.6363 0.4825 0.7182 0.046 Uiso 1 1 calc R . .
C16 C 0.4932(10) 0.5595(7) 0.7425(6) 0.043(3) Uani 1 1 d . . .
C17 C 0.3992(10) 0.4968(7) 0.7764(6) 0.055(4) Uani 1 1 d . . .
H17A H 0.4443 0.4463 0.8019 0.083 Uiso 1 1 calc R . .
H17B H 0.3566 0.4931 0.7360 0.083 Uiso 1 1 calc R . .
H17C H 0.3369 0.5110 0.8131 0.083 Uiso 1 1 calc R . .
C18 C 0.4171(10) 0.6385(7) 0.6997(5) 0.056(4) Uani 1 1 d . . .
H18A H 0.3482 0.6503 0.7345 0.084 Uiso 1 1 calc R . .
H18B H 0.3826 0.6338 0.6569 0.084 Uiso 1 1 calc R . .
H18C H 0.4732 0.6807 0.6810 0.084 Uiso 1 1 calc R . .
C19 C 0.5477(10) 0.5717(6) 0.8064(5) 0.044(3) Uani 1 1 d . . .
H19A H 0.6102 0.6108 0.7842 0.053 Uiso 1 1 calc R . .
H19B H 0.4793 0.5932 0.8357 0.053 Uiso 1 1 calc R . .
C20 C 0.6089(12) 0.4996(8) 0.8586(7) 0.048(3) Uani 1 1 d . . .
C21 C 0.6035(11) 0.4109(8) 0.9864(6) 0.037(3) Uani 1 1 d . . .
C22 C 0.5576(10) 0.3399(9) 1.0115(6) 0.041(3) Uani 1 1 d . . .
C23 C 0.6050(10) 0.2778(7) 1.0681(6) 0.038(3) Uani 1 1 d . . .
C24 C 0.7005(12) 0.2881(7) 1.1043(5) 0.049(3) Uani 1 1 d . . .
C25 C 0.7495(10) 0.3603(8) 1.0804(6) 0.041(3) Uani 1 1 d . . .
C26 C 0.6989(9) 0.4223(6) 1.0210(5) 0.031(3) Uani 1 1 d . . .
C27 C 1.1077(9) 0.4281(6) 0.7387(5) 0.032(3) Uani 1 1 d . . .
H27A H 1.1907 0.3976 0.7430 0.038 Uiso 1 1 calc R . .
H27B H 1.1147 0.4756 0.7498 0.038 Uiso 1 1 calc R . .
C28 C 1.0119(9) 0.3800(6) 0.7970(5) 0.038(3) Uani 1 1 d . . .
H28A H 1.0016 0.3346 0.7831 0.046 Uiso 1 1 calc R . .
H28B H 0.9302 0.4120 0.7933 0.046 Uiso 1 1 calc R . .
C29 C 1.0391(10) 0.3491(6) 0.8804(5) 0.032(3) Uani 1 1 d . . .
C30 C 1.1643(10) 0.2964(6) 0.8902(5) 0.051(3) Uani 1 1 d . . .
H30A H 1.2340 0.3276 0.8619 0.076 Uiso 1 1 calc R . .
H30B H 1.1608 0.2543 0.8710 0.076 Uiso 1 1 calc R . .
H30C H 1.1773 0.2740 0.9440 0.076 Uiso 1 1 calc R . .
C31 C 1.0503(10) 0.4159(6) 0.9065(5) 0.053(3) Uani 1 1 d . . .
H31A H 0.9744 0.4521 0.8973 0.079 Uiso 1 1 calc R . .
H31B H 1.1239 0.4433 0.8785 0.079 Uiso 1 1 calc R . .
H31C H 1.0600 0.3954 0.9608 0.079 Uiso 1 1 calc R . .
C32 C 0.9306(10) 0.3045(7) 0.9290(5) 0.041(3) Uani 1 1 d . . .
H32A H 0.9491 0.2861 0.9823 0.049 Uiso 1 1 calc R . .
H32B H 0.8547 0.3418 0.9244 0.049 Uiso 1 1 calc R . .
C33 C 0.8983(12) 0.2370(7) 0.9139(6) 0.041(3) Uani 1 1 d . . .
C34 C 0.7545(11) 0.1399(8) 0.9584(6) 0.045(3) Uani 1 1 d . . .
C35 C 0.6735(13) 0.1413(8) 0.9070(6) 0.060(4) Uani 1 1 d . . .
C36 C 0.6319(11) 0.0701(9) 0.9114(6) 0.053(4) Uani 1 1 d . . .
C37 C 0.6795(11) 0.0017(7) 0.9634(7) 0.042(3) Uani 1 1 d . . .
C38 C 0.7632(12) 0.0021(7) 1.0116(6) 0.051(3) Uani 1 1 d . . .
C39 C 0.8000(11) 0.0732(9) 1.0089(6) 0.048(3) Uani 1 1 d . . .
C40 C 1.0539(10) 0.2363(6) 0.5989(6) 0.042(3) Uani 1 1 d . . .
H40A H 1.0360 0.2161 0.5603 0.051 Uiso 1 1 calc R . .
H40B H 1.1434 0.2206 0.6076 0.051 Uiso 1 1 calc R . .
C41 C 0.9726(10) 0.1968(6) 0.6728(5) 0.041(3) Uani 1 1 d . . .
H41A H 0.8835 0.2065 0.6623 0.050 Uiso 1 1 calc R . .
H41B H 0.9815 0.2222 0.7092 0.050 Uiso 1 1 calc R . .
C42 C 1.0033(11) 0.1071(7) 0.7113(6) 0.045(3) Uani 1 1 d . . .
C43 C 0.9083(10) 0.0797(6) 0.7827(5) 0.050(3) Uani 1 1 d . . .
H43A H 0.9230 0.0231 0.8078 0.075 Uiso 1 1 calc R . .
H43B H 0.8224 0.0927 0.7681 0.075 Uiso 1 1 calc R . .
H43C H 0.9194 0.1060 0.8175 0.075 Uiso 1 1 calc R . .
C44 C 1.1355(10) 0.0905(6) 0.7298(5) 0.047(3) Uani 1 1 d . . .
H44A H 1.1542 0.1277 0.7519 0.071 Uiso 1 1 calc R . .
H44B H 1.1923 0.0955 0.6836 0.071 Uiso 1 1 calc R . .
H44C H 1.1474 0.0373 0.7663 0.071 Uiso 1 1 calc R . .
C45 C 0.9758(10) 0.0686(7) 0.6550(5) 0.041(3) Uani 1 1 d . . .
H45A H 0.8880 0.0847 0.6425 0.050 Uiso 1 1 calc R . .
H45B H 1.0321 0.0878 0.6076 0.050 Uiso 1 1 calc R . .
C46 C 0.9942(13) -0.0185(9) 0.6868(7) 0.051(4) Uani 1 1 d . . .
C47 C 0.9097(11) -0.1290(8) 0.6869(7) 0.046(3) Uani 1 1 d . . .
C48 C 0.9679(10) -0.1692(8) 0.6388(6) 0.044(3) Uani 1 1 d . . .
C49 C 0.9733(11) -0.2505(7) 0.6671(7) 0.049(3) Uani 1 1 d . . .
C50 C 0.9171(11) -0.2899(6) 0.7384(7) 0.045(3) Uani 1 1 d . . .
C51 C 0.8564(11) -0.2511(8) 0.7850(6) 0.047(3) Uani 1 1 d . . .
C52 C 0.8526(10) -0.1709(8) 0.7577(7) 0.043(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Si1 O5 1.612(6) . ?
Si1 O4 1.612(7) . ?
Si1 O1 1.637(6) . ?
Si1 C1 1.819(11) . ?
Si2 O6 1.615(6) . ?
Si2 O1 1.618(6) . ?
Si2 O2 1.630(7) . ?
Si2 C14 1.836(9) . ?
Si3 O2 1.601(7) . ?
Si3 O3 1.618(7) . ?
Si3 O5 1.632(7) 2_766 ?
Si3 C27 1.836(9) . ?
Si4 O4 1.617(7) . ?
Si4 O6 1.623(6) 2_766 ?
Si4 O3 1.631(6) . ?
Si4 C40 1.821(10) . ?
Cl9 C9 1.781(13) . ?
Cl10 C10 1.713(12) . ?
Cl11 C11 1.703(12) . ?
Cl12 C12 1.724(12) . ?
Cl13 C13 1.719(12) . ?
Cl22 C22 1.752(11) . ?
Cl23 C23 1.716(11) . ?
Cl24 C24 1.740(11) . ?
Cl25 C25 1.731(11) . ?
Cl26 C26 1.726(11) . ?
Cl35 C35 1.708(13) . ?
Cl36 C36 1.708(11) . ?
Cl37 C37 1.749(11) . ?
Cl38 C38 1.717(11) . ?
Cl39 C39 1.707(12) . ?
Cl48 C48 1.710(10) . ?
Cl49 C49 1.737(11) . ?
Cl50 C50 1.728(11) . ?
Cl51 C51 1.687(12) . ?
Cl52 C52 1.721(11) . ?
O5 Si3 1.632(7) 2_766 ?
O6 Si4 1.623(6) 2_766 ?
O7 C7 1.226(14) . ?
O8 C7 1.358(14) . ?
O8 C8 1.412(13) . ?
O9 C20 1.242(12) . ?
O10 C20 1.386(12) . ?
O10 C21 1.392(11) . ?
O11 C33 1.198(12) . ?
O12 C33 1.383(12) . ?
O12 C34 1.402(13) . ?
O13 C46 1.195(13) . ?
O14 C47 1.396(13) . ?
O14 C46 1.418(13) . ?
C1 C2 1.567(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.531(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.517(13) . ?
C3 C6 1.521(14) . ?
C3 C4 1.522(13) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.492(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C9 1.368(15) . ?
C8 C13 1.381(16) . ?
C9 C10 1.405(16) . ?
C10 C11 1.400(15) . ?
C11 C12 1.363(14) . ?
C12 C13 1.392(15) . ?
C14 C15 1.555(13) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.536(12) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C19 1.526(13) . ?
C16 C17 1.538(13) . ?
C16 C18 1.576(14) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.481(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C21 C22 1.357(15) . ?
C21 C26 1.377(13) . ?
C22 C23 1.359(14) . ?
C23 C24 1.391(14) . ?
C24 C25 1.393(14) . ?
C25 C26 1.401(14) . ?
C27 C28 1.512(12) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.541(12) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C31 1.513(13) . ?
C29 C32 1.515(13) . ?
C29 C30 1.548(13) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.469(14) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C34 C39 1.343(14) . ?
C34 C35 1.397(14) . ?
C35 C36 1.415(15) . ?
C36 C37 1.381(15) . ?
C37 C38 1.380(14) . ?
C38 C39 1.404(15) . ?
C40 C41 1.535(12) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.560(14) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C44 1.485(13) . ?
C42 C43 1.548(13) . ?
C42 C45 1.566(13) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.495(16) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C47 C52 1.390(14) . ?
C47 C48 1.410(14) . ?
C48 C49 1.395(14) . ?
C49 C50 1.381(14) . ?
C50 C51 1.379(14) . ?
C51 C52 1.377(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
O5 Si1 O4 109.0(3) . . ?
O5 Si1 O1 108.4(3) . . ?
O4 Si1 O1 109.8(3) . . ?
O5 Si1 C1 111.6(4) . . ?
O4 Si1 C1 109.3(4) . . ?
O1 Si1 C1 108.8(4) . . ?
O6 Si2 O1 108.7(3) . . ?
O6 Si2 O2 108.0(3) . . ?
O1 Si2 O2 109.1(4) . . ?
O6 Si2 C14 110.1(4) . . ?
O1 Si2 C14 109.8(4) . . ?
O2 Si2 C14 111.1(4) . . ?
O2 Si3 O3 109.4(4) . . ?
O2 Si3 O5 109.1(4) . 2_766 ?
O3 Si3 O5 108.5(3) . 2_766 ?
O2 Si3 C27 109.3(4) . . ?
O3 Si3 C27 109.6(4) . . ?
O5 Si3 C27 110.8(4) 2_766 . ?
O4 Si4 O6 108.3(3) . 2_766 ?
O4 Si4 O3 109.2(3) . . ?
O6 Si4 O3 108.9(3) 2_766 . ?
O4 Si4 C40 111.0(4) . . ?
O6 Si4 C40 108.6(4) 2_766 . ?
O3 Si4 C40 110.8(4) . . ?
Si2 O1 Si1 147.9(4) . . ?
Si3 O2 Si2 152.6(4) . . ?
Si3 O3 Si4 148.0(4) . . ?
Si1 O4 Si4 152.2(4) . . ?
Si1 O5 Si3 147.6(4) . 2_766 ?
Si2 O6 Si4 148.6(4) . 2_766 ?
C7 O8 C8 115.9(10) . . ?
C20 O10 C21 118.8(9) . . ?
C33 O12 C34 116.2(9) . . ?
C47 O14 C46 112.7(9) . . ?
C2 C1 Si1 114.6(7) . . ?
C2 C1 H1A 108.6 . . ?
Si1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
Si1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C1 115.4(9) . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C5 C3 C6 111.8(10) . . ?
C5 C3 C4 111.8(10) . . ?
C6 C3 C4 104.0(9) . . ?
C5 C3 C2 111.5(9) . . ?
C6 C3 C2 108.7(9) . . ?
C4 C3 C2 108.8(10) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C3 113.7(10) . . ?
C7 C6 H6A 108.8 . . ?
C3 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
C3 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O7 C7 O8 118.8(14) . . ?
O7 C7 C6 126.8(14) . . ?
O8 C7 C6 114.3(12) . . ?
C9 C8 C13 118.5(13) . . ?
C9 C8 O8 122.1(14) . . ?
C13 C8 O8 118.7(12) . . ?
C8 C9 C10 122.6(12) . . ?
C8 C9 Cl9 117.1(12) . . ?
C10 C9 Cl9 120.3(11) . . ?
C11 C10 C9 117.8(11) . . ?
C11 C10 Cl10 123.7(11) . . ?
C9 C10 Cl10 118.3(12) . . ?
C12 C11 C10 119.3(11) . . ?
C12 C11 Cl11 123.6(12) . . ?
C10 C11 Cl11 117.0(11) . . ?
C11 C12 C13 121.7(11) . . ?
C11 C12 Cl12 118.4(11) . . ?
C13 C12 Cl12 119.4(11) . . ?
C8 C13 C12 119.6(12) . . ?
C8 C13 Cl13 118.6(11) . . ?
C12 C13 Cl13 121.6(11) . . ?
C15 C14 Si2 114.1(7) . . ?
C15 C14 H14A 108.7 . . ?
Si2 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
Si2 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C16 C15 C14 115.4(8) . . ?
C16 C15 H15A 108.4 . . ?
C14 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C19 C16 C15 113.5(9) . . ?
C19 C16 C17 109.2(9) . . ?
C15 C16 C17 107.8(8) . . ?
C19 C16 C18 106.8(8) . . ?
C15 C16 C18 111.9(9) . . ?
C17 C16 C18 107.5(9) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C16 113.8(9) . . ?
C20 C19 H19A 108.8 . . ?
C16 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C16 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
O9 C20 O10 117.3(11) . . ?
O9 C20 C19 128.5(11) . . ?
O10 C20 C19 114.2(10) . . ?
C22 C21 C26 119.4(10) . . ?
C22 C21 O10 121.7(11) . . ?
C26 C21 O10 118.6(11) . . ?
C21 C22 C23 122.8(11) . . ?
C21 C22 Cl22 118.5(10) . . ?
C23 C22 Cl22 118.6(11) . . ?
C22 C23 C24 118.8(11) . . ?
C22 C23 Cl23 122.9(10) . . ?
C24 C23 Cl23 118.3(10) . . ?
C23 C24 C25 120.0(10) . . ?
C23 C24 Cl24 122.0(11) . . ?
C25 C24 Cl24 117.8(10) . . ?
C24 C25 C26 119.1(10) . . ?
C24 C25 Cl25 122.0(10) . . ?
C26 C25 Cl25 119.0(10) . . ?
C21 C26 C25 119.9(10) . . ?
C21 C26 Cl26 119.5(8) . . ?
C25 C26 Cl26 120.6(9) . . ?
C28 C27 Si3 113.3(7) . . ?
C28 C27 H27A 108.9 . . ?
Si3 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
Si3 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 C29 117.8(8) . . ?
C27 C28 H28A 107.9 . . ?
C29 C28 H28A 107.9 . . ?
C27 C28 H28B 107.9 . . ?
C29 C28 H28B 107.9 . . ?
H28A C28 H28B 107.2 . . ?
C31 C29 C32 107.9(8) . . ?
C31 C29 C28 110.6(9) . . ?
C32 C29 C28 109.0(8) . . ?
C31 C29 C30 108.1(9) . . ?
C32 C29 C30 110.9(9) . . ?
C28 C29 C30 110.3(8) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C29 118.7(9) . . ?
C33 C32 H32A 107.6 . . ?
C29 C32 H32A 107.6 . . ?
C33 C32 H32B 107.6 . . ?
C29 C32 H32B 107.6 . . ?
H32A C32 H32B 107.1 . . ?
O11 C33 O12 120.1(11) . . ?
O11 C33 C32 130.3(11) . . ?
O12 C33 C32 109.6(11) . . ?
C39 C34 C35 122.4(12) . . ?
C39 C34 O12 120.7(11) . . ?
C35 C34 O12 116.9(12) . . ?
C34 C35 C36 118.7(11) . . ?
C34 C35 Cl35 121.6(11) . . ?
C36 C35 Cl35 119.7(11) . . ?
C37 C36 C35 118.4(11) . . ?
C37 C36 Cl36 119.6(11) . . ?
C35 C36 Cl36 121.9(11) . . ?
C36 C37 C38 121.5(11) . . ?
C36 C37 Cl37 120.9(10) . . ?
C38 C37 Cl37 117.6(11) . . ?
C37 C38 C39 119.8(10) . . ?
C37 C38 Cl38 122.1(11) . . ?
C39 C38 Cl38 118.0(11) . . ?
C34 C39 C38 119.1(11) . . ?
C34 C39 Cl39 119.1(11) . . ?
C38 C39 Cl39 121.7(11) . . ?
C41 C40 Si4 116.1(7) . . ?
C41 C40 H40A 108.3 . . ?
Si4 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
Si4 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C40 C41 C42 116.0(8) . . ?
C40 C41 H41A 108.3 . . ?
C42 C41 H41A 108.3 . . ?
C40 C41 H41B 108.3 . . ?
C42 C41 H41B 108.3 . . ?
H41A C41 H41B 107.4 . . ?
C44 C42 C43 112.1(9) . . ?
C44 C42 C41 109.9(9) . . ?
C43 C42 C41 107.0(9) . . ?
C44 C42 C45 113.2(9) . . ?
C43 C42 C45 107.7(9) . . ?
C41 C42 C45 106.6(9) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C42 112.4(9) . . ?
C46 C45 H45A 109.1 . . ?
C42 C45 H45A 109.1 . . ?
C46 C45 H45B 109.1 . . ?
C42 C45 H45B 109.1 . . ?
H45A C45 H45B 107.9 . . ?
O13 C46 O14 120.5(13) . . ?
O13 C46 C45 132.1(12) . . ?
O14 C46 C45 107.4(11) . . ?
C52 C47 O14 121.5(11) . . ?
C52 C47 C48 119.2(12) . . ?
O14 C47 C48 119.1(11) . . ?
C49 C48 C47 117.9(10) . . ?
C49 C48 Cl48 123.6(10) . . ?
C47 C48 Cl48 118.5(10) . . ?
C50 C49 C48 120.8(10) . . ?
C50 C49 Cl49 121.2(10) . . ?
C48 C49 Cl49 118.0(10) . . ?
C51 C50 C49 121.8(11) . . ?
C51 C50 Cl50 119.3(11) . . ?
C49 C50 Cl50 118.9(11) . . ?
C52 C51 C50 117.5(11) . . ?
C52 C51 Cl51 120.9(11) . . ?
C50 C51 Cl51 121.5(11) . . ?
C51 C52 C47 122.6(11) . . ?
C51 C52 Cl52 120.4(10) . . ?
C47 C52 Cl52 116.9(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.749
_diffrn_reflns_theta_full              27.55
_diffrn_measured_fraction_theta_full   0.749
_refine_diff_density_max    0.395
_refine_diff_density_min   -0.443
_refine_diff_density_rms    0.093
