# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_028TAQA12
_database_code_depnum_ccdc_archive 'CCDC 1001294'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_audit_creation_date             2015-08-27
_audit_creation_method           CRYSTALS_ver_14.43

_chemical_name_systematic        ?
_chemical_melting_point          ?

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.2291(7)
_cell_length_b                   9.7804(7)
_cell_length_c                   15.8873(12)
_cell_angle_alpha                89.600(6)
_cell_angle_beta                 81.392(6)
_cell_angle_gamma                73.234(6)
_cell_volume                     1356.64(18)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Si 0.2541 0.3302 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C32 H44 Si1 
# Dc =      1.12 Fooo =    500.00 Mu =      8.66 M =    456.79
# Found Formula = C32 H44 Si1 
# Dc =      1.12 FOOO =    500.00 Mu =      8.66 M =    456.79

_chemical_formula_sum            'C32 H44 Si1'
_chemical_formula_moiety         'C32 H44 Si1'
_chemical_compound_source        ?
_chemical_formula_weight         456.79


_cell_measurement_reflns_used    7359
_cell_measurement_theta_min      5
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.030
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             500
_exptl_absorpt_coefficient_mu    0.866

# Sheldrick geometric approximatio 0.96 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.97
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            5617
_reflns_number_total             5617
_diffrn_reflns_av_R_equivalents  0.081
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5617 
# Theoretical number of reflections is about 11414 


_diffrn_reflns_theta_min         4.725
_diffrn_reflns_theta_max         76.569
_diffrn_measured_fraction_theta_max 0.983

_diffrn_reflns_theta_full        73.506
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -12
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      0.03

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.39
_refine_diff_density_max         0.57


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     0
_refine_ls_number_parameters     301
_oxford_refine_ls_R_factor_ref   0.1117
_refine_ls_wR_factor_ref         0.2790
_refine_ls_goodness_of_fit_ref   0.9647
_refine_ls_shift/su_max          0.0000972
_refine_ls_shift/su_mean         0.0000097


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5597
_refine_ls_R_factor_all          0.1118
_refine_ls_wR_factor_all         0.2791

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4511
_refine_ls_R_factor_gt           0.0970
_refine_ls_wR_factor_gt          0.2717

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.537E+04 0.877E+04 0.586E+04 0.268E+04 815. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.4434(4) 0.9499(5) 0.3424(2) 0.0233 1.0000 Uani . . . . . .
C2 C 0.2803(5) 1.0015(5) 0.3265(2) 0.0265 1.0000 Uani . . . . . .
C3 C 0.1930(5) 0.9312(5) 0.3737(3) 0.0269 1.0000 Uani . . . . . .
C4 C 0.2475(5) 0.7472(5) 0.4946(3) 0.0299 1.0000 Uani . . . . . .
C5 C 0.3570(5) 0.6858(5) 0.5474(3) 0.0298 1.0000 Uani . . . . . .
C6 C 0.5018(5) 0.7117(5) 0.5362(3) 0.0288 1.0000 Uani . . . . . .
C7 C 0.5406(5) 0.7976(5) 0.4710(3) 0.0258 1.0000 Uani . . . . . .
C8 C 0.4330(5) 0.8566(4) 0.4178(2) 0.0236 1.0000 Uani . . . . . .
C9 C 0.2858(4) 0.8373(5) 0.4313(3) 0.0247 1.0000 Uani . . . . . .
C10 C 0.2299(5) 1.1139(5) 0.2632(3) 0.0338 1.0000 Uani . . . . . .
C11 C 0.0269(5) 0.9502(6) 0.3685(3) 0.0383 1.0000 Uani . . . . . .
C12 C 0.0970(6) 0.7118(6) 0.5047(3) 0.0412 1.0000 Uani . . . . . .
C13 C 0.3218(7) 0.5891(6) 0.6173(3) 0.0425 1.0000 Uani . . . . . .
C14 C 0.6171(6) 0.6422(5) 0.5936(3) 0.0388 1.0000 Uani . . . . . .
C15 C 0.6918(5) 0.8298(5) 0.4604(3) 0.0297 1.0000 Uani . . . . . .
C16 C 0.5963(5) 0.9442(5) 0.1481(2) 0.0235 1.0000 Uani . . . . . .
C17 C 0.7293(5) 0.9956(5) 0.1622(3) 0.0266 1.0000 Uani . . . . . .
C18 C 0.8586(5) 0.9233(5) 0.1118(3) 0.0276 1.0000 Uani . . . . . .
C19 C 0.9086(5) 0.7320(5) -0.0146(3) 0.0300 1.0000 Uani . . . . . .
C20 C 0.8334(6) 0.6647(5) -0.0644(3) 0.0332 1.0000 Uani . . . . . .
C21 C 0.6750(6) 0.6925(5) -0.0497(3) 0.0304 1.0000 Uani . . . . . .
C22 C 0.5848(5) 0.7848(5) 0.0187(3) 0.0254 1.0000 Uani . . . . . .
C23 C 0.6604(5) 0.8475(4) 0.0703(2) 0.0223 1.0000 Uani . . . . . .
C24 C 0.8198(5) 0.8266(5) 0.0523(3) 0.0256 1.0000 Uani . . . . . .
C25 C 0.7143(5) 1.1087(5) 0.2296(3) 0.0324 1.0000 Uani . . . . . .
C26 C 1.0155(5) 0.9356(6) 0.1172(3) 0.0371 1.0000 Uani . . . . . .
C27 C 1.0820(6) 0.6984(6) -0.0314(4) 0.0440 1.0000 Uani . . . . . .
C28 C 0.9290(7) 0.5631(6) -0.1378(3) 0.0473 1.0000 Uani . . . . . .
C29 C 0.5967(7) 0.6186(6) -0.1048(3) 0.0433 1.0000 Uani . . . . . .
C30 C 0.4138(5) 0.8208(5) 0.0333(3) 0.0291 1.0000 Uani . . . . . .
C31 C 0.7524(5) 0.7171(5) 0.2615(3) 0.0331 1.0000 Uani . . . . . .
C32 C 0.4488(6) 0.7020(5) 0.2242(3) 0.0362 1.0000 Uani . . . . . .
Si1 Si 0.55900(13) 0.82931(12) 0.24445(7) 0.0230 1.0000 Uani . . . . . .
H11 H 0.4843 1.0293 0.3522 0.0282 1.0000 Uiso R . . . . .
H103 H 0.1236 1.1680 0.2794 0.0511 1.0000 Uiso R . . . . .
H101 H 0.2925 1.1787 0.2586 0.0508 1.0000 Uiso R . . . . .
H102 H 0.2433 1.0687 0.2078 0.0510 1.0000 Uiso R . . . . .
H111 H -0.0128 1.0319 0.3347 0.0591 1.0000 Uiso R . . . . .
H112 H -0.0335 0.9655 0.4249 0.0587 1.0000 Uiso R . . . . .
H113 H 0.0180 0.8654 0.3427 0.0591 1.0000 Uiso R . . . . .
H152 H 0.7743 0.7430 0.4452 0.0451 1.0000 Uiso R . . . . .
H151 H 0.7072 0.8697 0.5125 0.0452 1.0000 Uiso R . . . . .
H153 H 0.6993 0.8962 0.4153 0.0448 1.0000 Uiso R . . . . .
H143 H 0.7137 0.6604 0.5733 0.0592 1.0000 Uiso R . . . . .
H141 H 0.5805 0.6823 0.6503 0.0592 1.0000 Uiso R . . . . .
H142 H 0.6317 0.5405 0.5935 0.0590 1.0000 Uiso R . . . . .
H133 H 0.3640 0.6033 0.6667 0.0642 1.0000 Uiso R . . . . .
H132 H 0.2131 0.6110 0.6334 0.0643 1.0000 Uiso R . . . . .
H131 H 0.3631 0.4899 0.5987 0.0640 1.0000 Uiso R . . . . .
H121 H 0.0258 0.7713 0.5493 0.0612 1.0000 Uiso R . . . . .
H123 H 0.0525 0.7270 0.4536 0.0613 1.0000 Uiso R . . . . .
H122 H 0.1115 0.6143 0.5187 0.0608 1.0000 Uiso R . . . . .
H161 H 0.5049 1.0230 0.1413 0.0282 1.0000 Uiso R . . . . .
H251 H 0.7925 1.1571 0.2152 0.0490 1.0000 Uiso R . . . . .
H252 H 0.6140 1.1775 0.2359 0.0489 1.0000 Uiso R . . . . .
H253 H 0.7287 1.0629 0.2828 0.0489 1.0000 Uiso R . . . . .
H263 H 1.0069 1.0132 0.1563 0.0563 1.0000 Uiso R . . . . .
H261 H 1.0638 0.9537 0.0620 0.0556 1.0000 Uiso R . . . . .
H262 H 1.0770 0.8478 0.1365 0.0558 1.0000 Uiso R . . . . .
H301 H 0.3869 0.7351 0.0463 0.0437 1.0000 Uiso R . . . . .
H303 H 0.3733 0.8579 -0.0170 0.0442 1.0000 Uiso R . . . . .
H302 H 0.3705 0.8888 0.0797 0.0443 1.0000 Uiso R . . . . .
H293 H 0.4882 0.6430 -0.0843 0.0662 1.0000 Uiso R . . . . .
H291 H 0.6133 0.6498 -0.1616 0.0664 1.0000 Uiso R . . . . .
H292 H 0.6427 0.5162 -0.1049 0.0661 1.0000 Uiso R . . . . .
H281 H 0.8837 0.5826 -0.1892 0.0724 1.0000 Uiso R . . . . .
H282 H 1.0317 0.5711 -0.1497 0.0724 1.0000 Uiso R . . . . .
H283 H 0.9380 0.4648 -0.1244 0.0723 1.0000 Uiso R . . . . .
H272 H 1.1270 0.5969 -0.0376 0.0647 1.0000 Uiso R . . . . .
H273 H 1.1165 0.7408 -0.0817 0.0651 1.0000 Uiso R . . . . .
H271 H 1.1166 0.7318 0.0158 0.0655 1.0000 Uiso R . . . . .
H311 H 0.8098 0.7750 0.2792 0.0485 1.0000 Uiso R . . . . .
H313 H 0.7419 0.6477 0.3032 0.0490 1.0000 Uiso R . . . . .
H312 H 0.8062 0.6658 0.2094 0.0492 1.0000 Uiso R . . . . .
H322 H 0.3475 0.7526 0.2135 0.0534 1.0000 Uiso R . . . . .
H321 H 0.4390 0.6443 0.2735 0.0541 1.0000 Uiso R . . . . .
H323 H 0.5026 0.6378 0.1763 0.0541 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          9.5(11)

loop_
_oxford_twin_element_scale_factors
0.389(5)
0.195(6)
0.208(6)
0.208(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.502(5) yes
C1 . C8 . 1.510(6) yes
C1 . Si1 . 1.937(4) yes
C1 . H11 . 0.978 no
C2 . C3 . 1.347(6) yes
C2 . C10 . 1.505(6) yes
C3 . C9 . 1.477(6) yes
C3 . C11 . 1.504(6) yes
C4 . C5 . 1.407(6) yes
C4 . C9 . 1.406(6) yes
C4 . C12 . 1.511(6) yes
C5 . C6 . 1.416(6) yes
C5 . C13 . 1.513(6) yes
C6 . C7 . 1.399(6) yes
C6 . C14 . 1.512(6) yes
C7 . C8 . 1.395(6) yes
C7 . C15 . 1.503(6) yes
C8 . C9 . 1.410(5) yes
C10 . H103 . 0.967 no
C10 . H101 . 0.969 no
C10 . H102 . 0.964 no
C11 . H111 . 0.971 no
C11 . H112 . 0.970 no
C11 . H113 . 0.957 no
C12 . H121 . 0.958 no
C12 . H123 . 0.955 no
C12 . H122 . 0.954 no
C13 . H133 . 0.954 no
C13 . H132 . 0.958 no
C13 . H131 . 0.965 no
C14 . H143 . 0.967 no
C14 . H141 . 0.958 no
C14 . H142 . 0.965 no
C15 . H152 . 0.966 no
C15 . H151 . 0.964 no
C15 . H153 . 0.972 no
C16 . C17 . 1.500(6) yes
C16 . C23 . 1.498(5) yes
C16 . Si1 . 1.941(4) yes
C16 . H161 . 0.984 no
C17 . C18 . 1.341(6) yes
C17 . C25 . 1.508(6) yes
C18 . C24 . 1.492(6) yes
C18 . C26 . 1.502(6) yes
C19 . C20 . 1.406(7) yes
C19 . C24 . 1.404(6) yes
C19 . C27 . 1.520(7) yes
C20 . C21 . 1.391(7) yes
C20 . C28 . 1.527(6) yes
C21 . C22 . 1.413(6) yes
C21 . C29 . 1.520(6) yes
C22 . C23 . 1.400(6) yes
C22 . C30 . 1.497(6) yes
C23 . C24 . 1.410(6) yes
C25 . H251 . 0.971 no
C25 . H252 . 0.966 no
C25 . H253 . 0.963 no
C26 . H263 . 0.962 no
C26 . H261 . 0.962 no
C26 . H262 . 0.959 no
C27 . H272 . 0.958 no
C27 . H273 . 0.954 no
C27 . H271 . 0.952 no
C28 . H281 . 0.966 no
C28 . H282 . 0.964 no
C28 . H283 . 0.966 no
C29 . H293 . 0.965 no
C29 . H291 . 0.956 no
C29 . H292 . 0.969 no
C30 . H301 . 0.954 no
C30 . H303 . 0.958 no
C30 . H302 . 0.955 no
C31 . Si1 . 1.864(5) yes
C31 . H311 . 0.948 no
C31 . H313 . 0.960 no
C31 . H312 . 0.961 no
C32 . Si1 . 1.876(5) yes
C32 . H322 . 0.963 no
C32 . H321 . 0.972 no
C32 . H323 . 0.966 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 102.6(3) yes
C2 . C1 . Si1 . 106.7(3) yes
C8 . C1 . Si1 . 108.4(3) yes
C2 . C1 . H11 . 111.9 no
C8 . C1 . H11 . 114.3 no
Si1 . C1 . H11 . 112.3 no
C1 . C2 . C3 . 111.0(4) yes
C1 . C2 . C10 . 122.1(4) yes
C3 . C2 . C10 . 126.9(4) yes
C2 . C3 . C9 . 108.9(4) yes
C2 . C3 . C11 . 124.4(4) yes
C9 . C3 . C11 . 126.6(4) yes
C5 . C4 . C9 . 117.7(4) yes
C5 . C4 . C12 . 120.4(4) yes
C9 . C4 . C12 . 121.9(4) yes
C4 . C5 . C6 . 121.3(4) yes
C4 . C5 . C13 . 120.2(4) yes
C6 . C5 . C13 . 118.5(4) yes
C5 . C6 . C7 . 120.5(4) yes
C5 . C6 . C14 . 119.7(4) yes
C7 . C6 . C14 . 119.8(4) yes
C6 . C7 . C8 . 118.2(4) yes
C6 . C7 . C15 . 120.9(4) yes
C8 . C7 . C15 . 120.8(4) yes
C1 . C8 . C7 . 130.0(4) yes
C1 . C8 . C9 . 108.4(3) yes
C7 . C8 . C9 . 121.6(4) yes
C3 . C9 . C8 . 108.0(4) yes
C3 . C9 . C4 . 131.4(4) yes
C8 . C9 . C4 . 120.5(4) yes
C2 . C10 . H103 . 111.1 no
C2 . C10 . H101 . 110.6 no
H103 . C10 . H101 . 109.2 no
C2 . C10 . H102 . 109.3 no
H103 . C10 . H102 . 109.3 no
H101 . C10 . H102 . 107.2 no
C3 . C11 . H111 . 110.3 no
C3 . C11 . H112 . 110.7 no
H111 . C11 . H112 . 108.6 no
C3 . C11 . H113 . 108.8 no
H111 . C11 . H113 . 109.8 no
H112 . C11 . H113 . 108.7 no
C4 . C12 . H121 . 109.9 no
C4 . C12 . H123 . 111.6 no
H121 . C12 . H123 . 108.0 no
C4 . C12 . H122 . 110.5 no
H121 . C12 . H122 . 108.7 no
H123 . C12 . H122 . 108.1 no
C5 . C13 . H133 . 111.1 no
C5 . C13 . H132 . 109.4 no
H133 . C13 . H132 . 107.7 no
C5 . C13 . H131 . 111.0 no
H133 . C13 . H131 . 108.4 no
H132 . C13 . H131 . 109.2 no
C6 . C14 . H143 . 109.5 no
C6 . C14 . H141 . 109.2 no
H143 . C14 . H141 . 109.0 no
C6 . C14 . H142 . 110.0 no
H143 . C14 . H142 . 109.3 no
H141 . C14 . H142 . 109.7 no
C7 . C15 . H152 . 109.9 no
C7 . C15 . H151 . 111.2 no
H152 . C15 . H151 . 108.0 no
C7 . C15 . H153 . 111.5 no
H152 . C15 . H153 . 107.4 no
H151 . C15 . H153 . 108.7 no
C17 . C16 . C23 . 102.6(3) yes
C17 . C16 . Si1 . 106.3(3) yes
C23 . C16 . Si1 . 108.7(3) yes
C17 . C16 . H161 . 112.7 no
C23 . C16 . H161 . 113.7 no
Si1 . C16 . H161 . 112.2 no
C16 . C17 . C18 . 111.6(4) yes
C16 . C17 . C25 . 121.9(4) yes
C18 . C17 . C25 . 126.4(4) yes
C17 . C18 . C24 . 108.4(4) yes
C17 . C18 . C26 . 125.2(4) yes
C24 . C18 . C26 . 126.4(4) yes
C20 . C19 . C24 . 118.2(4) yes
C20 . C19 . C27 . 120.4(4) yes
C24 . C19 . C27 . 121.4(4) yes
C19 . C20 . C21 . 121.5(4) yes
C19 . C20 . C28 . 118.4(5) yes
C21 . C20 . C28 . 120.0(5) yes
C20 . C21 . C22 . 120.8(4) yes
C20 . C21 . C29 . 120.3(4) yes
C22 . C21 . C29 . 118.8(4) yes
C21 . C22 . C23 . 117.7(4) yes
C21 . C22 . C30 . 121.6(4) yes
C23 . C22 . C30 . 120.7(4) yes
C16 . C23 . C22 . 129.5(4) yes
C16 . C23 . C24 . 109.0(3) yes
C22 . C23 . C24 . 121.5(4) yes
C18 . C24 . C23 . 107.5(4) yes
C18 . C24 . C19 . 132.3(4) yes
C23 . C24 . C19 . 120.1(4) yes
C17 . C25 . H251 . 110.4 no
C17 . C25 . H252 . 110.6 no
H251 . C25 . H252 . 109.7 no
C17 . C25 . H253 . 108.4 no
H251 . C25 . H253 . 108.4 no
H252 . C25 . H253 . 109.3 no
C18 . C26 . H263 . 109.3 no
C18 . C26 . H261 . 110.1 no
H263 . C26 . H261 . 109.2 no
C18 . C26 . H262 . 109.5 no
H263 . C26 . H262 . 109.9 no
H261 . C26 . H262 . 108.9 no
C19 . C27 . H272 . 109.3 no
C19 . C27 . H273 . 112.1 no
H272 . C27 . H273 . 108.6 no
C19 . C27 . H271 . 109.8 no
H272 . C27 . H271 . 108.0 no
H273 . C27 . H271 . 109.0 no
C20 . C28 . H281 . 111.2 no
C20 . C28 . H282 . 111.5 no
H281 . C28 . H282 . 108.1 no
C20 . C28 . H283 . 111.1 no
H281 . C28 . H283 . 108.0 no
H282 . C28 . H283 . 106.8 no
C21 . C29 . H293 . 110.7 no
C21 . C29 . H291 . 107.8 no
H293 . C29 . H291 . 109.7 no
C21 . C29 . H292 . 109.5 no
H293 . C29 . H292 . 110.6 no
H291 . C29 . H292 . 108.7 no
C22 . C30 . H301 . 108.0 no
C22 . C30 . H303 . 110.6 no
H301 . C30 . H303 . 108.5 no
C22 . C30 . H302 . 110.8 no
H301 . C30 . H302 . 109.2 no
H303 . C30 . H302 . 109.6 no
Si1 . C31 . H311 . 110.5 no
Si1 . C31 . H313 . 109.6 no
H311 . C31 . H313 . 110.6 no
Si1 . C31 . H312 . 109.6 no
H311 . C31 . H312 . 109.1 no
H313 . C31 . H312 . 107.5 no
Si1 . C32 . H322 . 111.2 no
Si1 . C32 . H321 . 109.9 no
H322 . C32 . H321 . 108.2 no
Si1 . C32 . H323 . 110.3 no
H322 . C32 . H323 . 109.7 no
H321 . C32 . H323 . 107.5 no
C16 . Si1 . C1 . 110.69(18) yes
C16 . Si1 . C32 . 114.01(19) yes
C1 . Si1 . C32 . 106.8(2) yes
C16 . Si1 . C31 . 105.15(19) yes
C1 . Si1 . C31 . 114.00(19) yes
C32 . Si1 . C31 . 106.3(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C12 . H123 . C11 . 123.89(16) 0.955 2.531 3.165(7) yes
C27 . H271 . C26 . 135.01(17) 0.952 2.441 3.186(7) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 27/08/15 at 10:49:17
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (  10,X'S) H   ( 103,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 123,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 263,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 273,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 293,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 303,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 313,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) H   ( 323,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 27/08/15 at 10:49:17
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_201TAQA13
_database_code_depnum_ccdc_archive 'CCDC 1001295'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H42 Cl2 Si Zr'
_chemical_formula_sum            'C32 H42 Cl2 Si Zr'
_chemical_formula_weight         616.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0820 0.0700 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9670 0.5600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   14.10780(10)
_cell_length_b                   14.2840(2)
_cell_length_c                   14.3753(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.8940(10)
_cell_angle_gamma                90
_cell_volume                     2875.91(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6774
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.630
_shelx_estimated_absorpt_T_min   0.810
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.85
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log  

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12519
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0134
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         5.126
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6559
_reflns_number_gt                5817
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    
;
Palatinus, L.; Chapuis, G. J. Appl. Cryst. 2007, 40, 786-790.
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+2.0780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6559
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.09271(12) 0.40948(12) 0.90916(12) 0.0181(3) Uani 1 1 d . . . . .
C2 C 0.05073(12) 0.36603(12) 0.98594(12) 0.0191(3) Uani 1 1 d . . . . .
C3 C 0.09637(12) 0.39767(12) 1.07294(12) 0.0198(3) Uani 1 1 d . . . . .
C4 C 0.23726(13) 0.51403(13) 1.11666(12) 0.0213(3) Uani 1 1 d . . . . .
C5 C 0.29464(13) 0.57798(13) 1.07821(13) 0.0243(4) Uani 1 1 d . . . . .
C6 C 0.28385(13) 0.59568(13) 0.97927(13) 0.0236(4) Uani 1 1 d . . . . .
C7 C 0.21851(12) 0.54726(12) 0.91774(12) 0.0205(3) Uani 1 1 d . . . . .
C8 C 0.16323(12) 0.47439(12) 0.95433(12) 0.0180(3) Uani 1 1 d . . . . .
C9 C 0.16869(12) 0.46345(12) 1.05469(12) 0.0187(3) Uani 1 1 d . . . . .
C10 C -0.03120(13) 0.29767(13) 0.97814(14) 0.0253(4) Uani 1 1 d . . . . .
H10A H -0.0381 0.2720 1.0402 0.038 Uiso 1 1 calc R U . . .
H10B H -0.0186 0.2466 0.9357 0.038 Uiso 1 1 calc R U . . .
H10C H -0.0902 0.3299 0.9534 0.038 Uiso 1 1 calc R U . . .
C11 C 0.06378(14) 0.37524(15) 1.16644(13) 0.0283(4) Uani 1 1 d . . . . .
H11A H 0.0084 0.3334 1.1573 0.042 Uiso 1 1 calc R U . . .
H11B H 0.0461 0.4333 1.1964 0.042 Uiso 1 1 calc R U . . .
H11C H 0.1157 0.3444 1.2065 0.042 Uiso 1 1 calc R U . . .
C12 C 0.25132(14) 0.49009(15) 1.21978(13) 0.0285(4) Uani 1 1 d . . . . .
H12A H 0.3071 0.5237 1.2504 0.043 Uiso 1 1 calc R U . . .
H12B H 0.2615 0.4225 1.2274 0.043 Uiso 1 1 calc R U . . .
H12C H 0.1945 0.5085 1.2484 0.043 Uiso 1 1 calc R U . . .
C13 C 0.37080(17) 0.63170(17) 1.13914(16) 0.0391(5) Uani 1 1 d . . . . .
H13A H 0.3652 0.6189 1.2052 0.059 Uiso 1 1 calc R U . . .
H13B H 0.3626 0.6989 1.1270 0.059 Uiso 1 1 calc R U . . .
H13C H 0.4340 0.6121 1.1247 0.059 Uiso 1 1 calc R U . . .
C14 C 0.34508(15) 0.67047(15) 0.94178(16) 0.0335(5) Uani 1 1 d . . . . .
H14A H 0.3310 0.6736 0.8734 0.050 Uiso 1 1 calc R U . . .
H14B H 0.4126 0.6551 0.9587 0.050 Uiso 1 1 calc R U . . .
H14C H 0.3313 0.7312 0.9689 0.050 Uiso 1 1 calc R U . . .
C15 C 0.19658(14) 0.57890(14) 0.81762(13) 0.0273(4) Uani 1 1 d . . . . .
H15A H 0.1877 0.6469 0.8159 0.041 Uiso 1 1 calc R U . . .
H15B H 0.1380 0.5483 0.7890 0.041 Uiso 1 1 calc R U . . .
H15C H 0.2497 0.5620 0.7828 0.041 Uiso 1 1 calc R U . . .
C16 C 0.16979(12) 0.25596(12) 0.81953(11) 0.0185(3) Uani 1 1 d . . . . .
C17 C 0.27094(12) 0.27856(13) 0.83109(12) 0.0198(3) Uani 1 1 d . . . . .
C18 C 0.32334(12) 0.20889(12) 0.88461(12) 0.0195(3) Uani 1 1 d . . . . .
C19 C 0.27070(12) 0.05669(12) 0.96471(12) 0.0199(3) Uani 1 1 d . . . . .
C20 C 0.19573(13) -0.00477(13) 0.96354(12) 0.0218(3) Uani 1 1 d . . . . .
C21 C 0.10588(12) 0.01367(12) 0.90756(12) 0.0205(3) Uani 1 1 d . . . . .
C22 C 0.08962(12) 0.09661(12) 0.85860(12) 0.0193(3) Uani 1 1 d . . . . .
C23 C 0.16414(12) 0.16516(12) 0.86418(11) 0.0172(3) Uani 1 1 d . . . . .
C24 C 0.25701(12) 0.14022(12) 0.90972(11) 0.0178(3) Uani 1 1 d . . . . .
C25 C 0.31820(14) 0.36049(14) 0.78943(14) 0.0280(4) Uani 1 1 d . . . . .
H25A H 0.3836 0.3672 0.8204 0.042 Uiso 1 1 calc R U . . .
H25B H 0.2822 0.4177 0.7986 0.042 Uiso 1 1 calc R U . . .
H25C H 0.3196 0.3499 0.7223 0.042 Uiso 1 1 calc R U . . .
C26 C 0.43064(13) 0.20124(14) 0.89652(15) 0.0269(4) Uani 1 1 d . . . . .
H26A H 0.4565 0.2396 0.8490 0.040 Uiso 1 1 calc R U . . .
H26B H 0.4491 0.1358 0.8892 0.040 Uiso 1 1 calc R U . . .
H26C H 0.4561 0.2234 0.9591 0.040 Uiso 1 1 calc R U . . .
C27 C 0.36344(13) 0.04194(14) 1.02823(13) 0.0256(4) Uani 1 1 d . . . . .
H27A H 0.3501 0.0104 1.0858 0.038 Uiso 1 1 calc R U . . .
H27B H 0.3935 0.1027 1.0439 0.038 Uiso 1 1 calc R U . . .
H27C H 0.4066 0.0032 0.9959 0.038 Uiso 1 1 calc R U . . .
C28 C 0.20656(16) -0.09532(14) 1.01845(16) 0.0330(4) Uani 1 1 d . . . . .
H28A H 0.2738 -0.1045 1.0427 0.050 Uiso 1 1 calc R U . . .
H28B H 0.1847 -0.1477 0.9773 0.050 Uiso 1 1 calc R U . . .
H28C H 0.1682 -0.0923 1.0708 0.050 Uiso 1 1 calc R U . . .
C29 C 0.02854(14) -0.05990(14) 0.90153(15) 0.0281(4) Uani 1 1 d . . . . .
H29A H -0.0325 -0.0319 0.8760 0.042 Uiso 1 1 calc R U . . .
H29B H 0.0233 -0.0848 0.9642 0.042 Uiso 1 1 calc R U . . .
H29C H 0.0446 -0.1108 0.8605 0.042 Uiso 1 1 calc R U . . .
C30 C 0.00238(13) 0.10821(14) 0.78772(14) 0.0272(4) Uani 1 1 d . . . . .
H30A H -0.0105 0.0494 0.7534 0.041 Uiso 1 1 calc R U . . .
H30B H 0.0137 0.1582 0.7437 0.041 Uiso 1 1 calc R U . . .
H30C H -0.0526 0.1245 0.8201 0.041 Uiso 1 1 calc R U . . .
C31 C -0.05243(14) 0.32357(15) 0.75555(15) 0.0303(4) Uani 1 1 d . . . . .
H31A H -0.0894 0.3818 0.7515 0.045 Uiso 1 1 calc R U . . .
H31B H -0.0752 0.2825 0.8027 0.045 Uiso 1 1 calc R U . . .
H31C H -0.0604 0.2921 0.6945 0.045 Uiso 1 1 calc R U . . .
C32 C 0.10154(16) 0.41306(15) 0.68045(13) 0.0303(4) Uani 1 1 d . . . . .
H32A H 0.0926 0.3696 0.6274 0.045 Uiso 1 1 calc R U . . .
H32B H 0.1674 0.4362 0.6882 0.045 Uiso 1 1 calc R U . . .
H32C H 0.0574 0.4659 0.6686 0.045 Uiso 1 1 calc R U . . .
Cl1 Cl 0.18672(4) 0.19450(3) 1.11039(3) 0.02777(11) Uani 1 1 d . . . . .
Cl2 Cl 0.37101(3) 0.35502(3) 1.04949(3) 0.02791(11) Uani 1 1 d . . . . .
Si1 Si 0.07702(3) 0.35094(3) 0.78973(3) 0.01999(11) Uani 1 1 d . . . . .
Zr1 Zr 0.21367(2) 0.30095(2) 0.98530(2) 0.01494(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.453(2) . ?
C1 C8 1.455(2) . ?
C1 Si1 1.8986(18) . ?
C1 Zr1 2.4628(16) . ?
C2 C3 1.411(2) . ?
C2 C10 1.507(2) . ?
C2 Zr1 2.4807(17) . ?
C3 C9 1.434(2) . ?
C3 C11 1.506(2) . ?
C3 Zr1 2.5952(17) . ?
C4 C5 1.379(3) . ?
C4 C9 1.430(2) . ?
C4 C12 1.511(2) . ?
C5 C6 1.435(3) . ?
C5 C13 1.511(3) . ?
C6 C7 1.384(3) . ?
C6 C14 1.513(3) . ?
C7 C8 1.438(2) . ?
C7 C15 1.505(2) . ?
C8 C9 1.444(2) . ?
C8 Zr1 2.6012(17) . ?
C9 Zr1 2.6339(17) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.453(2) . ?
C16 C23 1.454(2) . ?
C16 Si1 1.8979(18) . ?
C16 Zr1 2.4740(16) . ?
C17 C18 1.411(3) . ?
C17 C25 1.506(2) . ?
C17 Zr1 2.4697(17) . ?
C18 C24 1.431(2) . ?
C18 C26 1.507(2) . ?
C18 Zr1 2.5992(17) . ?
C19 C20 1.373(3) . ?
C19 C24 1.431(2) . ?
C19 C27 1.518(2) . ?
C20 C21 1.442(3) . ?
C20 C28 1.513(3) . ?
C21 C22 1.383(3) . ?
C21 C29 1.510(2) . ?
C22 C23 1.432(2) . ?
C22 C30 1.510(2) . ?
C23 C24 1.438(2) . ?
C23 Zr1 2.6439(17) . ?
C24 Zr1 2.6428(17) . ?
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 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Si1 1.875(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 Si1 1.872(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Cl1 Zr1 2.4195(5) . ?
Cl2 Zr1 2.4255(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
C2 C1 C8 104.62(14) . . ?
C2 C1 Si1 119.00(12) . . ?
C8 C1 Si1 133.13(13) . . ?
C2 C1 Zr1 73.58(9) . . ?
C8 C1 Zr1 78.61(9) . . ?
Si1 C1 Zr1 97.12(7) . . ?
C3 C2 C1 110.64(15) . . ?
C3 C2 C10 122.54(16) . . ?
C1 C2 C10 126.81(16) . . ?
C3 C2 Zr1 78.39(10) . . ?
C1 C2 Zr1 72.24(9) . . ?
C10 C2 Zr1 117.37(12) . . ?
C2 C3 C9 107.86(15) . . ?
C2 C3 C11 124.57(16) . . ?
C9 C3 C11 127.05(16) . . ?
C2 C3 Zr1 69.44(10) . . ?
C9 C3 Zr1 75.57(10) . . ?
C11 C3 Zr1 126.92(12) . . ?
C5 C4 C9 118.08(16) . . ?
C5 C4 C12 121.92(17) . . ?
C9 C4 C12 119.75(16) . . ?
C4 C5 C6 121.10(16) . . ?
C4 C5 C13 120.96(18) . . ?
C6 C5 C13 117.94(17) . . ?
C7 C6 C5 121.93(16) . . ?
C7 C6 C14 119.36(17) . . ?
C5 C6 C14 118.71(17) . . ?
C6 C7 C8 118.49(16) . . ?
C6 C7 C15 120.39(16) . . ?
C8 C7 C15 120.61(15) . . ?
C7 C8 C9 118.54(15) . . ?
C7 C8 C1 132.07(16) . . ?
C9 C8 C1 109.18(15) . . ?
C7 C8 Zr1 127.08(11) . . ?
C9 C8 Zr1 75.24(10) . . ?
C1 C8 Zr1 68.15(9) . . ?
C4 C9 C3 131.30(16) . . ?
C4 C9 C8 121.24(15) . . ?
C3 C9 C8 107.45(15) . . ?
C4 C9 Zr1 120.36(11) . . ?
C3 C9 Zr1 72.60(10) . . ?
C8 C9 Zr1 72.75(9) . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 C12 H12A 109.5 . . ?
C4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C13 H13A 109.5 . . ?
C5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C23 104.65(14) . . ?
C17 C16 Si1 120.54(13) . . ?
C23 C16 Si1 131.65(13) . . ?
C17 C16 Zr1 72.74(9) . . ?
C23 C16 Zr1 80.04(9) . . ?
Si1 C16 Zr1 96.77(7) . . ?
C18 C17 C16 110.40(15) . . ?
C18 C17 C25 122.46(16) . . ?
C16 C17 C25 127.06(16) . . ?
C18 C17 Zr1 78.95(10) . . ?
C16 C17 Zr1 73.07(9) . . ?
C25 C17 Zr1 117.67(12) . . ?
C17 C18 C24 107.77(15) . . ?
C17 C18 C26 124.50(16) . . ?
C24 C18 C26 126.85(16) . . ?
C17 C18 Zr1 68.84(10) . . ?
C24 C18 Zr1 75.84(9) . . ?
C26 C18 Zr1 129.08(12) . . ?
C20 C19 C24 118.26(16) . . ?
C20 C19 C27 121.72(17) . . ?
C24 C19 C27 119.83(16) . . ?
C19 C20 C21 120.95(16) . . ?
C19 C20 C28 120.71(17) . . ?
C21 C20 C28 118.31(17) . . ?
C22 C21 C20 121.44(16) . . ?
C22 C21 C29 119.50(16) . . ?
C20 C21 C29 119.06(16) . . ?
C21 C22 C23 118.78(15) . . ?
C21 C22 C30 120.63(16) . . ?
C23 C22 C30 119.76(16) . . ?
C22 C23 C24 118.63(15) . . ?
C22 C23 C16 131.62(15) . . ?
C24 C23 C16 109.08(14) . . ?
C22 C23 Zr1 132.29(11) . . ?
C24 C23 Zr1 74.18(9) . . ?
C16 C23 Zr1 67.17(9) . . ?
C19 C24 C18 131.41(16) . . ?
C19 C24 C23 120.88(15) . . ?
C18 C24 C23 107.64(15) . . ?
C19 C24 Zr1 121.31(11) . . ?
C18 C24 Zr1 72.48(9) . . ?
C23 C24 Zr1 74.26(9) . . ?
C17 C25 H25A 109.5 . . ?
C17 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C17 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C18 C26 H26A 109.5 . . ?
C18 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C18 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 H27A 109.5 . . ?
C19 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C19 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C20 C28 H28A 109.5 . . ?
C20 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C20 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C21 C29 H29A 109.5 . . ?
C21 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C21 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si1 C32 H32A 109.5 . . ?
Si1 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si1 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C32 Si1 C31 98.70(10) . . ?
C32 Si1 C16 109.66(9) . . ?
C31 Si1 C16 122.26(9) . . ?
C32 Si1 C1 122.46(9) . . ?
C31 Si1 C1 109.45(9) . . ?
C16 Si1 C1 96.22(7) . . ?
Cl1 Zr1 Cl2 97.797(19) . . ?
Cl1 Zr1 C1 124.30(4) . . ?
Cl2 Zr1 C1 121.49(4) . . ?
Cl1 Zr1 C17 133.10(5) . . ?
Cl2 Zr1 C17 89.98(4) . . ?
C1 Zr1 C17 88.08(6) . . ?
Cl1 Zr1 C16 120.61(4) . . ?
Cl2 Zr1 C16 124.12(4) . . ?
C1 Zr1 C16 69.85(6) . . ?
C17 Zr1 C16 34.19(5) . . ?
Cl1 Zr1 C2 90.25(4) . . ?
Cl2 Zr1 C2 133.27(4) . . ?
C1 Zr1 C2 34.18(5) . . ?
C17 Zr1 C2 117.06(6) . . ?
C16 Zr1 C2 88.62(6) . . ?
Cl1 Zr1 C3 78.90(4) . . ?
Cl2 Zr1 C3 104.69(4) . . ?
C1 Zr1 C3 55.42(6) . . ?
C17 Zr1 C3 143.23(6) . . ?
C16 Zr1 C3 120.36(6) . . ?
C2 Zr1 C3 32.17(6) . . ?
Cl1 Zr1 C18 104.66(4) . . ?
Cl2 Zr1 C18 78.13(4) . . ?
C1 Zr1 C18 119.86(6) . . ?
C17 Zr1 C18 32.21(6) . . ?
C16 Zr1 C18 55.18(5) . . ?
C2 Zr1 C18 143.65(6) . . ?
C3 Zr1 C18 175.25(5) . . ?
Cl1 Zr1 C8 131.42(4) . . ?
Cl2 Zr1 C8 88.91(4) . . ?
C1 Zr1 C8 33.25(5) . . ?
C17 Zr1 C8 94.70(6) . . ?
C16 Zr1 C8 92.91(6) . . ?
C2 Zr1 C8 53.78(5) . . ?
C3 Zr1 C8 53.04(5) . . ?
C18 Zr1 C8 123.74(5) . . ?
Cl1 Zr1 C9 101.88(4) . . ?
Cl2 Zr1 C9 80.00(4) . . ?
C1 Zr1 C9 55.11(5) . . ?
C17 Zr1 C9 125.01(6) . . ?
C16 Zr1 C9 123.36(6) . . ?
C2 Zr1 C9 53.33(5) . . ?
C3 Zr1 C9 31.83(5) . . ?
C18 Zr1 C9 147.50(5) . . ?
C8 Zr1 C9 32.01(5) . . ?
Cl1 Zr1 C24 79.88(4) . . ?
Cl2 Zr1 C24 100.76(4) . . ?
C1 Zr1 C24 123.11(5) . . ?
C17 Zr1 C24 53.25(6) . . ?
C16 Zr1 C24 54.68(5) . . ?
C2 Zr1 C24 125.96(5) . . ?
C3 Zr1 C24 148.70(5) . . ?
C18 Zr1 C24 31.68(5) . . ?
C8 Zr1 C24 146.00(5) . . ?
C9 Zr1 C24 178.00(5) . . ?
Cl1 Zr1 C23 88.61(4) . . ?
Cl2 Zr1 C23 129.91(4) . . ?
C1 Zr1 C23 93.14(5) . . ?
C17 Zr1 C23 53.34(5) . . ?
C16 Zr1 C23 32.79(5) . . ?
C2 Zr1 C23 96.06(5) . . ?
C3 Zr1 C23 125.22(5) . . ?
C18 Zr1 C23 52.41(5) . . ?
C8 Zr1 C23 122.74(5) . . ?
C9 Zr1 C23 147.06(5) . . ?
C24 Zr1 C23 31.56(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
C8 C1 C2 C3 -3.43(19) . . . . ?
Si1 C1 C2 C3 158.84(12) . . . . ?
Zr1 C1 C2 C3 69.73(13) . . . . ?
C8 C1 C2 C10 175.54(16) . . . . ?
Si1 C1 C2 C10 -22.2(2) . . . . ?
Zr1 C1 C2 C10 -111.30(17) . . . . ?
C8 C1 C2 Zr1 -73.16(11) . . . . ?
Si1 C1 C2 Zr1 89.11(11) . . . . ?
C1 C2 C3 C9 0.6(2) . . . . ?
C10 C2 C3 C9 -178.41(16) . . . . ?
Zr1 C2 C3 C9 66.39(12) . . . . ?
C1 C2 C3 C11 172.84(16) . . . . ?
C10 C2 C3 C11 -6.2(3) . . . . ?
Zr1 C2 C3 C11 -121.38(17) . . . . ?
C1 C2 C3 Zr1 -65.78(12) . . . . ?
C10 C2 C3 Zr1 115.19(16) . . . . ?
C9 C4 C5 C6 2.1(3) . . . . ?
C12 C4 C5 C6 176.26(17) . . . . ?
C9 C4 C5 C13 -178.03(18) . . . . ?
C12 C4 C5 C13 -3.8(3) . . . . ?
C4 C5 C6 C7 -2.6(3) . . . . ?
C13 C5 C6 C7 177.52(19) . . . . ?
C4 C5 C6 C14 176.63(18) . . . . ?
C13 C5 C6 C14 -3.3(3) . . . . ?
C5 C6 C7 C8 -2.8(3) . . . . ?
C14 C6 C7 C8 178.00(17) . . . . ?
C5 C6 C7 C15 169.06(17) . . . . ?
C14 C6 C7 C15 -10.1(3) . . . . ?
C6 C7 C8 C9 8.3(2) . . . . ?
C15 C7 C8 C9 -163.52(16) . . . . ?
C6 C7 C8 C1 -177.47(18) . . . . ?
C15 C7 C8 C1 10.7(3) . . . . ?
C6 C7 C8 Zr1 -84.4(2) . . . . ?
C15 C7 C8 Zr1 103.76(18) . . . . ?
C2 C1 C8 C7 -169.65(18) . . . . ?
Si1 C1 C8 C7 31.8(3) . . . . ?
Zr1 C1 C8 C7 120.87(19) . . . . ?
C2 C1 C8 C9 4.96(18) . . . . ?
Si1 C1 C8 C9 -153.64(14) . . . . ?
Zr1 C1 C8 C9 -64.52(12) . . . . ?
C2 C1 C8 Zr1 69.48(11) . . . . ?
Si1 C1 C8 Zr1 -89.12(15) . . . . ?
C5 C4 C9 C3 -175.87(18) . . . . ?
C12 C4 C9 C3 9.8(3) . . . . ?
C5 C4 C9 C8 3.7(3) . . . . ?
C12 C4 C9 C8 -170.59(16) . . . . ?
C5 C4 C9 Zr1 91.07(18) . . . . ?
C12 C4 C9 Zr1 -83.26(18) . . . . ?
C2 C3 C9 C4 -177.82(18) . . . . ?
C11 C3 C9 C4 10.2(3) . . . . ?
Zr1 C3 C9 C4 -115.46(19) . . . . ?
C2 C3 C9 C8 2.53(19) . . . . ?
C11 C3 C9 C8 -169.45(17) . . . . ?
Zr1 C3 C9 C8 64.89(11) . . . . ?
C2 C3 C9 Zr1 -62.36(12) . . . . ?
C11 C3 C9 Zr1 125.66(18) . . . . ?
C7 C8 C9 C4 -9.0(2) . . . . ?
C1 C8 C9 C4 175.56(15) . . . . ?
Zr1 C8 C9 C4 115.51(16) . . . . ?
C7 C8 C9 C3 170.70(15) . . . . ?
C1 C8 C9 C3 -4.74(19) . . . . ?
Zr1 C8 C9 C3 -64.79(12) . . . . ?
C7 C8 C9 Zr1 -124.50(15) . . . . ?
C1 C8 C9 Zr1 60.05(11) . . . . ?
C23 C16 C17 C18 -3.52(19) . . . . ?
Si1 C16 C17 C18 158.63(12) . . . . ?
Zr1 C16 C17 C18 70.92(12) . . . . ?
C23 C16 C17 C25 173.33(17) . . . . ?
Si1 C16 C17 C25 -24.5(2) . . . . ?
Zr1 C16 C17 C25 -112.23(18) . . . . ?
C23 C16 C17 Zr1 -74.44(11) . . . . ?
Si1 C16 C17 Zr1 87.71(11) . . . . ?
C16 C17 C18 C24 -0.64(19) . . . . ?
C25 C17 C18 C24 -177.66(16) . . . . ?
Zr1 C17 C18 C24 66.46(12) . . . . ?
C16 C17 C18 C26 169.25(16) . . . . ?
C25 C17 C18 C26 -7.8(3) . . . . ?
Zr1 C17 C18 C26 -123.66(17) . . . . ?
C16 C17 C18 Zr1 -67.10(12) . . . . ?
C25 C17 C18 Zr1 115.88(17) . . . . ?
C24 C19 C20 C21 0.7(2) . . . . ?
C27 C19 C20 C21 175.70(16) . . . . ?
C24 C19 C20 C28 178.58(16) . . . . ?
C27 C19 C20 C28 -6.5(3) . . . . ?
C19 C20 C21 C22 -4.7(3) . . . . ?
C28 C20 C21 C22 177.35(17) . . . . ?
C19 C20 C21 C29 174.49(16) . . . . ?
C28 C20 C21 C29 -3.4(2) . . . . ?
C20 C21 C22 C23 0.0(2) . . . . ?
C29 C21 C22 C23 -179.25(16) . . . . ?
C20 C21 C22 C30 169.49(16) . . . . ?
C29 C21 C22 C30 -9.7(3) . . . . ?
C21 C22 C23 C24 8.4(2) . . . . ?
C30 C22 C23 C24 -161.22(16) . . . . ?
C21 C22 C23 C16 177.88(17) . . . . ?
C30 C22 C23 C16 8.3(3) . . . . ?
C21 C22 C23 Zr1 -86.0(2) . . . . ?
C30 C22 C23 Zr1 104.39(18) . . . . ?
C17 C16 C23 C22 -163.87(17) . . . . ?
Si1 C16 C23 C22 36.8(3) . . . . ?
Zr1 C16 C23 C22 127.05(18) . . . . ?
C17 C16 C23 C24 6.37(18) . . . . ?
Si1 C16 C23 C24 -152.93(13) . . . . ?
Zr1 C16 C23 C24 -62.70(12) . . . . ?
C17 C16 C23 Zr1 69.07(11) . . . . ?
Si1 C16 C23 Zr1 -90.23(14) . . . . ?
C20 C19 C24 C18 -168.66(17) . . . . ?
C27 C19 C24 C18 16.3(3) . . . . ?
C20 C19 C24 C23 7.9(2) . . . . ?
C27 C19 C24 C23 -167.18(15) . . . . ?
C20 C19 C24 Zr1 97.53(17) . . . . ?
C27 C19 C24 Zr1 -77.54(18) . . . . ?
C17 C18 C24 C19 -178.47(17) . . . . ?
C26 C18 C24 C19 11.9(3) . . . . ?
Zr1 C18 C24 C19 -116.62(18) . . . . ?
C17 C18 C24 C23 4.64(19) . . . . ?
C26 C18 C24 C23 -164.94(17) . . . . ?
Zr1 C18 C24 C23 66.50(11) . . . . ?
C17 C18 C24 Zr1 -61.85(12) . . . . ?
C26 C18 C24 Zr1 128.57(18) . . . . ?
C22 C23 C24 C19 -12.5(2) . . . . ?
C16 C23 C24 C19 175.77(15) . . . . ?
Zr1 C23 C24 C19 117.42(15) . . . . ?
C22 C23 C24 C18 164.75(15) . . . . ?
C16 C23 C24 C18 -6.95(18) . . . . ?
Zr1 C23 C24 C18 -65.30(11) . . . . ?
C22 C23 C24 Zr1 -129.95(15) . . . . ?
C16 C23 C24 Zr1 58.35(11) . . . . ?
C17 C16 Si1 C32 55.61(15) . . . . ?
C23 C16 Si1 C32 -147.78(16) . . . . ?
Zr1 C16 Si1 C32 129.54(8) . . . . ?
C17 C16 Si1 C31 170.15(13) . . . . ?
C23 C16 Si1 C31 -33.2(2) . . . . ?
Zr1 C16 Si1 C31 -115.92(9) . . . . ?
C17 C16 Si1 C1 -72.14(14) . . . . ?
C23 C16 Si1 C1 84.47(16) . . . . ?
Zr1 C16 Si1 C1 1.79(7) . . . . ?
C2 C1 Si1 C32 165.00(13) . . . . ?
C8 C1 Si1 C32 -38.8(2) . . . . ?
Zr1 C1 Si1 C32 -119.85(9) . . . . ?
C2 C1 Si1 C31 50.50(15) . . . . ?
C8 C1 Si1 C31 -153.32(17) . . . . ?
Zr1 C1 Si1 C31 125.64(8) . . . . ?
C2 C1 Si1 C16 -76.94(14) . . . . ?
C8 C1 Si1 C16 79.24(17) . . . . ?
Zr1 C1 Si1 C16 -1.80(7) . . . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.066

_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_002TAQA13
_database_code_depnum_ccdc_archive 'CCDC 1419346'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H66 Cl6 Si2 Zr2'
_chemical_formula_sum            'C42 H66 Cl6 Si2 Zr2'
_chemical_formula_weight         1022.26

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.52710(10)
_cell_length_b                   11.12740(10)
_cell_length_c                   11.36160(10)
_cell_angle_alpha                78.1650(10)
_cell_angle_beta                 87.3400(10)
_cell_angle_gamma                77.9020(10)
_cell_volume                     1152.67(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5228
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.881
_shelx_estimated_absorpt_T_min   0.742
_shelx_estimated_absorpt_T_max   0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.82
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9971
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0130
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         5.123
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5248
_reflns_number_gt                4851
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-86, Sheldrick, G. M.'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+0.7042P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5248
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.12505(17) 0.83562(14) 0.35009(14) 0.0161(3) Uani 1 1 d . . . . .
C2 C 0.00860(18) 0.87933(15) 0.32759(15) 0.0188(3) Uani 1 1 d . . . . .
C3 C 0.08490(18) 0.86027(15) 0.43554(16) 0.0197(3) Uani 1 1 d . . . . .
C4 C 0.0300(2) 0.76516(16) 0.65769(16) 0.0227(4) Uani 1 1 d . . . . .
C5 C -0.0771(2) 0.72668(16) 0.73180(16) 0.0242(4) Uani 1 1 d . . . . .
C6 C -0.2096(2) 0.71628(16) 0.68327(16) 0.0227(4) Uani 1 1 d . . . . .
C7 C -0.23583(18) 0.74390(15) 0.56071(15) 0.0184(3) Uani 1 1 d . . . . .
C8 C -0.13007(17) 0.79231(14) 0.48102(14) 0.0159(3) Uani 1 1 d . . . . .
C9 C 0.00121(18) 0.80398(15) 0.53146(15) 0.0176(3) Uani 1 1 d . . . . .
C10 C 0.0688(2) 0.93707(18) 0.20907(17) 0.0269(4) Uani 1 1 d . . . . .
H10A H 0.0333 1.0281 0.1928 0.040 Uiso 1 1 calc R U . . .
H10B H 0.0383 0.9019 0.1445 0.040 Uiso 1 1 calc R U . . .
H10C H 0.1739 0.9186 0.2130 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2175(2) 0.91086(18) 0.4452(2) 0.0289(4) Uani 1 1 d . . . . .
H11A H 0.3025 0.8432 0.4481 0.043 Uiso 1 1 calc R U . . .
H11B H 0.2124 0.9449 0.5187 0.043 Uiso 1 1 calc R U . . .
H11C H 0.2241 0.9775 0.3751 0.043 Uiso 1 1 calc R U . . .
C12 C 0.1780(2) 0.7581(2) 0.7048(2) 0.0367(5) Uani 1 1 d . . . . .
H12A H 0.1831 0.8387 0.7246 0.055 Uiso 1 1 calc R U . . .
H12B H 0.2500 0.7391 0.6432 0.055 Uiso 1 1 calc R U . . .
H12C H 0.1968 0.6919 0.7771 0.055 Uiso 1 1 calc R U . . .
C13 C -0.0562(3) 0.6908(2) 0.86682(18) 0.0383(5) Uani 1 1 d . . . . .
H13A H -0.0364 0.5992 0.8918 0.057 Uiso 1 1 calc R U . . .
H13B H -0.1435 0.7267 0.9070 0.057 Uiso 1 1 calc R U . . .
H13C H 0.0248 0.7232 0.8889 0.057 Uiso 1 1 calc R U . . .
C14 C -0.3223(2) 0.6720(2) 0.77006(18) 0.0335(4) Uani 1 1 d . . . . .
H14A H -0.4034 0.6633 0.7248 0.050 Uiso 1 1 calc R U . . .
H14B H -0.3557 0.7334 0.8212 0.050 Uiso 1 1 calc R U . . .
H14C H -0.2807 0.5908 0.8203 0.050 Uiso 1 1 calc R U . . .
C15 C -0.37551(19) 0.72883(17) 0.51445(17) 0.0238(4) Uani 1 1 d . . . . .
H15A H -0.3877 0.6424 0.5432 0.036 Uiso 1 1 calc R U . . .
H15B H -0.3745 0.7477 0.4263 0.036 Uiso 1 1 calc R U . . .
H15C H -0.4552 0.7866 0.5438 0.036 Uiso 1 1 calc R U . . .
C16 C -0.4278(2) 0.98776(18) 0.28807(19) 0.0292(4) Uani 1 1 d . . . . .
H16A H -0.3999 1.0689 0.2811 0.044 Uiso 1 1 calc R U . . .
H16B H -0.4496 0.9554 0.3723 0.044 Uiso 1 1 calc R U . . .
H16C H -0.5129 0.9984 0.2387 0.044 Uiso 1 1 calc R U . . .
C17 C -0.2254(2) 0.9604(2) 0.08413(17) 0.0319(4) Uani 1 1 d . . . . .
H17A H -0.1527 0.9041 0.0461 0.048 Uiso 1 1 calc R U . . .
H17B H -0.1866 1.0322 0.0949 0.048 Uiso 1 1 calc R U . . .
H17C H -0.3107 0.9900 0.0329 0.048 Uiso 1 1 calc R U . . .
C18 C -0.3347(2) 0.73341(17) 0.19970(17) 0.0245(4) Uani 1 1 d . . . . .
H18A H -0.2532 0.6826 0.1629 0.029 Uiso 1 1 calc R U . . .
H18B H -0.3594 0.6809 0.2760 0.029 Uiso 1 1 calc R U . . .
C19 C -0.4639(2) 0.76685(17) 0.11497(17) 0.0247(4) Uani 1 1 d . . . . .
H19A H -0.5487 0.8094 0.1552 0.030 Uiso 1 1 calc R U . . .
H19B H -0.4435 0.8263 0.0418 0.030 Uiso 1 1 calc R U . . .
C20 C -0.4988(2) 0.65201(18) 0.07868(17) 0.0259(4) Uani 1 1 d . . . . .
H20A H -0.5217 0.5936 0.1518 0.031 Uiso 1 1 calc R U . . .
H20B H -0.4131 0.6082 0.0405 0.031 Uiso 1 1 calc R U . . .
C21 C -0.6247(2) 0.6850(2) -0.00809(18) 0.0307(4) Uani 1 1 d . . . . .
H21A H -0.7106 0.7263 0.0300 0.046 Uiso 1 1 calc R U . . .
H21B H -0.6423 0.6082 -0.0288 0.046 Uiso 1 1 calc R U . . .
H21C H -0.6022 0.7416 -0.0813 0.046 Uiso 1 1 calc R U . . .
Cl1 Cl 0.06032(5) 0.63818(4) 0.18034(4) 0.02620(10) Uani 1 1 d . . . . .
Cl2 Cl 0.32107(5) 0.62750(4) 0.38291(4) 0.02750(10) Uani 1 1 d . . . . .
Cl3 Cl -0.11930(4) 0.50519(4) 0.40753(3) 0.01884(9) Uani 1 1 d . . . . .
Si1 Si -0.27573(5) 0.87358(4) 0.23444(4) 0.01954(10) Uani 1 1 d . . . . .
Zr1 Zr 0.06463(2) 0.64887(2) 0.38879(2) 0.01572(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.450(2) . ?
C1 C8 1.469(2) . ?
C1 Si1 1.9128(17) . ?
C1 Zr1 2.4294(16) . ?
C2 C3 1.410(2) . ?
C2 C10 1.511(2) . ?
C2 Zr1 2.4645(16) . ?
C3 C9 1.437(2) . ?
C3 C11 1.504(2) . ?
C3 Zr1 2.5623(16) . ?
C4 C5 1.374(3) . ?
C4 C9 1.432(2) . ?
C4 C12 1.513(3) . ?
C5 C6 1.436(3) . ?
C5 C13 1.515(3) . ?
C6 C7 1.386(2) . ?
C6 C14 1.514(3) . ?
C7 C8 1.438(2) . ?
C7 C15 1.507(2) . ?
C8 C9 1.440(2) . ?
C8 Zr1 2.5201(16) . ?
C9 Zr1 2.5673(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 Si1 1.883(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si1 1.876(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.533(2) . ?
C18 Si1 1.8829(18) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.523(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.524(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Cl1 Zr1 2.3982(4) . ?
Cl2 Zr1 2.4037(4) . ?
Cl3 Zr1 2.5831(4) . ?
Cl3 Zr1 2.5837(4) 2_566 ?
Zr1 Cl3 2.5837(4) 2_566 ?

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 C8 104.89(14) . . ?
C2 C1 Si1 123.58(12) . . ?
C8 C1 Si1 129.49(12) . . ?
C2 C1 Zr1 74.10(9) . . ?
C8 C1 Zr1 76.16(9) . . ?
Si1 C1 Zr1 127.15(8) . . ?
C3 C2 C1 110.73(15) . . ?
C3 C2 C10 120.78(16) . . ?
C1 C2 C10 128.48(16) . . ?
C3 C2 Zr1 77.56(10) . . ?
C1 C2 Zr1 71.45(9) . . ?
C10 C2 Zr1 117.66(11) . . ?
C2 C3 C9 107.70(14) . . ?
C2 C3 C11 123.67(16) . . ?
C9 C3 C11 127.94(16) . . ?
C2 C3 Zr1 69.93(9) . . ?
C9 C3 Zr1 73.93(9) . . ?
C11 C3 Zr1 128.88(12) . . ?
C5 C4 C9 117.97(16) . . ?
C5 C4 C12 121.78(17) . . ?
C9 C4 C12 120.09(17) . . ?
C4 C5 C6 120.98(16) . . ?
C4 C5 C13 120.58(18) . . ?
C6 C5 C13 118.42(18) . . ?
C7 C6 C5 122.15(16) . . ?
C7 C6 C14 119.66(17) . . ?
C5 C6 C14 118.18(16) . . ?
C6 C7 C8 118.31(16) . . ?
C6 C7 C15 119.98(16) . . ?
C8 C7 C15 121.64(15) . . ?
C7 C8 C9 118.66(15) . . ?
C7 C8 C1 132.86(15) . . ?
C9 C8 C1 108.48(14) . . ?
C7 C8 Zr1 121.32(11) . . ?
C9 C8 Zr1 75.36(9) . . ?
C1 C8 Zr1 69.39(8) . . ?
C4 C9 C3 130.30(16) . . ?
C4 C9 C8 121.60(15) . . ?
C3 C9 C8 108.09(14) . . ?
C4 C9 Zr1 121.33(11) . . ?
C3 C9 Zr1 73.54(9) . . ?
C8 C9 Zr1 71.76(9) . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 C12 H12A 109.5 . . ?
C4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C13 H13A 109.5 . . ?
C5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 Si1 114.03(12) . . ?
C19 C18 H18A 108.7 . . ?
Si1 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
Si1 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C18 112.50(15) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 C21 112.75(16) . . ?
C19 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Zr1 Cl3 Zr1 105.285(14) . 2_566 ?
C17 Si1 C18 104.22(9) . . ?
C17 Si1 C16 104.25(10) . . ?
C18 Si1 C16 112.75(9) . . ?
C17 Si1 C1 112.82(8) . . ?
C18 Si1 C1 115.19(8) . . ?
C16 Si1 C1 107.16(8) . . ?
Cl1 Zr1 Cl2 91.233(17) . . ?
Cl1 Zr1 C1 89.05(4) . . ?
Cl2 Zr1 C1 130.30(4) . . ?
Cl1 Zr1 C2 88.19(4) . . ?
Cl2 Zr1 C2 95.88(4) . . ?
C1 Zr1 C2 34.45(5) . . ?
Cl1 Zr1 C8 121.54(4) . . ?
Cl2 Zr1 C8 131.58(4) . . ?
C1 Zr1 C8 34.46(5) . . ?
C2 Zr1 C8 55.29(5) . . ?
Cl1 Zr1 C3 116.57(4) . . ?
Cl2 Zr1 C3 79.97(4) . . ?
C1 Zr1 C3 56.18(5) . . ?
C2 Zr1 C3 32.52(6) . . ?
C8 Zr1 C3 54.54(5) . . ?
Cl1 Zr1 C9 141.73(4) . . ?
Cl2 Zr1 C9 99.31(4) . . ?
C1 Zr1 C9 56.30(5) . . ?
C2 Zr1 C9 54.33(5) . . ?
C8 Zr1 C9 32.88(5) . . ?
C3 Zr1 C9 32.53(5) . . ?
Cl1 Zr1 Cl3 82.776(15) . . ?
Cl2 Zr1 Cl3 137.879(15) . . ?
C1 Zr1 Cl3 91.41(4) . . ?
C2 Zr1 Cl3 125.36(4) . . ?
C8 Zr1 Cl3 84.89(4) . . ?
C3 Zr1 Cl3 139.43(4) . . ?
C9 Zr1 Cl3 111.04(4) . . ?
Cl1 Zr1 Cl3 137.682(15) . 2_566 ?
Cl2 Zr1 Cl3 82.663(15) . 2_566 ?
C1 Zr1 Cl3 126.22(4) . 2_566 ?
C2 Zr1 Cl3 134.01(4) . 2_566 ?
C8 Zr1 Cl3 91.95(4) . 2_566 ?
C3 Zr1 Cl3 103.56(4) . 2_566 ?
C9 Zr1 Cl3 80.40(4) . 2_566 ?
Cl3 Zr1 Cl3 74.715(14) . 2_566 ?

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
C8 C1 C2 C3 2.25(18) . . . . ?
Si1 C1 C2 C3 167.35(12) . . . . ?
Zr1 C1 C2 C3 -68.28(12) . . . . ?
C8 C1 C2 C10 -178.43(16) . . . . ?
Si1 C1 C2 C10 -13.3(2) . . . . ?
Zr1 C1 C2 C10 111.03(17) . . . . ?
C8 C1 C2 Zr1 70.54(10) . . . . ?
Si1 C1 C2 Zr1 -124.37(12) . . . . ?
C1 C2 C3 C9 -0.37(19) . . . . ?
C10 C2 C3 C9 -179.74(15) . . . . ?
Zr1 C2 C3 C9 -64.78(11) . . . . ?
C1 C2 C3 C11 -171.56(15) . . . . ?
C10 C2 C3 C11 9.1(3) . . . . ?
Zr1 C2 C3 C11 124.02(16) . . . . ?
C1 C2 C3 Zr1 64.41(11) . . . . ?
C10 C2 C3 Zr1 -114.96(15) . . . . ?
C9 C4 C5 C6 4.8(3) . . . . ?
C12 C4 C5 C6 -170.58(17) . . . . ?
C9 C4 C5 C13 -176.88(16) . . . . ?
C12 C4 C5 C13 7.7(3) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C13 C5 C6 C7 -178.20(17) . . . . ?
C4 C5 C6 C14 179.39(17) . . . . ?
C13 C5 C6 C14 1.0(2) . . . . ?
C5 C6 C7 C8 -4.2(2) . . . . ?
C14 C6 C7 C8 176.60(16) . . . . ?
C5 C6 C7 C15 178.74(16) . . . . ?
C14 C6 C7 C15 -0.5(2) . . . . ?
C6 C7 C8 C9 3.1(2) . . . . ?
C15 C7 C8 C9 -179.89(15) . . . . ?
C6 C7 C8 C1 -177.05(16) . . . . ?
C15 C7 C8 C1 0.0(3) . . . . ?
C6 C7 C8 Zr1 92.80(17) . . . . ?
C15 C7 C8 Zr1 -90.15(17) . . . . ?
C2 C1 C8 C7 176.82(17) . . . . ?
Si1 C1 C8 C7 12.9(3) . . . . ?
Zr1 C1 C8 C7 -114.12(18) . . . . ?
C2 C1 C8 C9 -3.28(17) . . . . ?
Si1 C1 C8 C9 -167.16(12) . . . . ?
Zr1 C1 C8 C9 65.77(11) . . . . ?
C2 C1 C8 Zr1 -69.05(10) . . . . ?
Si1 C1 C8 Zr1 127.07(13) . . . . ?
C5 C4 C9 C3 172.69(17) . . . . ?
C12 C4 C9 C3 -11.8(3) . . . . ?
C5 C4 C9 C8 -5.8(2) . . . . ?
C12 C4 C9 C8 169.64(16) . . . . ?
C5 C4 C9 Zr1 -92.64(18) . . . . ?
C12 C4 C9 Zr1 82.83(19) . . . . ?
C2 C3 C9 C4 179.57(17) . . . . ?
C11 C3 C9 C4 -9.7(3) . . . . ?
Zr1 C3 C9 C4 117.41(18) . . . . ?
C2 C3 C9 C8 -1.75(18) . . . . ?
C11 C3 C9 C8 168.96(16) . . . . ?
Zr1 C3 C9 C8 -63.91(11) . . . . ?
C2 C3 C9 Zr1 62.17(11) . . . . ?
C11 C3 C9 Zr1 -127.13(18) . . . . ?
C7 C8 C9 C4 1.9(2) . . . . ?
C1 C8 C9 C4 -178.01(15) . . . . ?
Zr1 C8 C9 C4 -116.11(15) . . . . ?
C7 C8 C9 C3 -176.92(14) . . . . ?
C1 C8 C9 C3 3.17(17) . . . . ?
Zr1 C8 C9 C3 65.08(11) . . . . ?
C7 C8 C9 Zr1 118.00(14) . . . . ?
C1 C8 C9 Zr1 -61.91(10) . . . . ?
Si1 C18 C19 C20 174.08(13) . . . . ?
C18 C19 C20 C21 -178.51(16) . . . . ?
C19 C18 Si1 C17 -60.76(16) . . . . ?
C19 C18 Si1 C16 51.67(16) . . . . ?
C19 C18 Si1 C1 175.10(13) . . . . ?

_refine_diff_density_max         0.398
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3



