#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/85/4068548.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4068548
loop_
_publ_author_name
'Krempner, Clemens'
'Jäger-Fiedler, Ulrike'
'Köckerling, Martin'
'Reinke, Helmut'
_publ_section_title
;
 Synthesis and Structures of Titanium and Zirconium Trisiloxides
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              382
_journal_paper_doi               10.1021/om800930s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C50 H152 O6 Si26 Zr1'
_chemical_formula_sum            'C50 H152 O6 Si26 Zr'
_chemical_formula_weight         1671.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'ct.exe (M. Köckerling, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 115.082(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6636(7)
_cell_length_b                   26.479(2)
_cell_length_c                   14.9466(7)
_cell_measurement_reflns_used    5813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.15
_cell_volume                     5256.2(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            58667
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.8666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.023
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         12670
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0945P)²+4.5341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                8493
_reflns_number_total             12670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800930s_si_002.cif
_cod_data_source_block           CK1010-C50H152O6Si26Zr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C50 H152 O6 Si26 Zr1'
_cod_database_code               4068548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Zr1 Zr 0.51818(5) 0.99413(4) 0.00195(10) 0.0499(2) Uani 0.50 1 d P . .
O1 O 0.41332(17) 0.94113(8) -0.08371(16) 0.0382(5) Uani 1 1 d . . .
O2 O 0.41219(15) 1.00136(8) 0.08177(16) 0.0355(5) Uani 1 1 d . . .
H1 H 0.3845 1.0295 0.0535 0.053 Uiso 0.50 1 d PR . .
O3 O 0.59846(16) 0.94719(9) 0.10393(17) 0.0429(5) Uani 1 1 d . . .
H2 H 0.6449 0.9662 0.1485 0.064 Uiso 0.50 1 d PR . .
Si1 Si 0.30512(8) 0.86088(4) -0.31839(7) 0.0470(2) Uani 1 1 d . . .
C1 C 0.2365(4) 0.92211(15) -0.3560(3) 0.0640(11) Uani 1 1 d . . .
H1A H 0.2404 0.9345 -0.4161 0.096 Uiso 1 1 calc R . .
H1B H 0.2672 0.9469 -0.3029 0.096 Uiso 1 1 calc R . .
H1C H 0.1658 0.9171 -0.3688 0.096 Uiso 1 1 calc R . .
C2 C 0.4405(4) 0.8739(2) -0.2892(4) 0.0784(14) Uani 1 1 d . . .
H2A H 0.4457 0.8867 -0.3484 0.118 Uiso 1 1 calc R . .
H2B H 0.4794 0.8426 -0.2677 0.118 Uiso 1 1 calc R . .
H2C H 0.4671 0.8991 -0.2364 0.118 Uiso 1 1 calc R . .
C3 C 0.2515(4) 0.81424(17) -0.4225(3) 0.0714(13) Uani 1 1 d . . .
H3A H 0.2559 0.8281 -0.4813 0.107 Uiso 1 1 calc R . .
H3B H 0.1809 0.8076 -0.4370 0.107 Uiso 1 1 calc R . .
H3C H 0.2898 0.7827 -0.4034 0.107 Uiso 1 1 calc R . .
Si2 Si 0.29727(7) 0.83028(3) -0.17481(7) 0.0392(2) Uani 1 1 d . . .
C4 C 0.3893(3) 0.77581(15) -0.1228(3) 0.0653(12) Uani 1 1 d . . .
H4A H 0.3695 0.7480 -0.1705 0.098 Uiso 1 1 calc R . .
H4B H 0.3885 0.7642 -0.0609 0.098 Uiso 1 1 calc R . .
H4C H 0.4572 0.7872 -0.1103 0.098 Uiso 1 1 calc R . .
Si3 Si 0.33365(6) 0.90079(3) -0.06941(6) 0.03256(18) Uani 1 1 d . . .
C5 C 0.2107(2) 0.93480(13) -0.1057(2) 0.0422(8) Uani 1 1 d . . .
H5A H 0.1801 0.9408 -0.1772 0.063 Uiso 1 1 calc R . .
H5B H 0.2226 0.9672 -0.0708 0.063 Uiso 1 1 calc R . .
H5C H 0.1653 0.9141 -0.0882 0.063 Uiso 1 1 calc R . .
Si4 Si 0.41924(6) 0.88272(3) 0.10093(6) 0.03202(18) Uani 1 1 d . . .
C6 C 0.3766(3) 0.82533(14) 0.1477(3) 0.0531(9) Uani 1 1 d . . .
H6A H 0.3053 0.8289 0.1335 0.080 Uiso 1 1 calc R . .
H6B H 0.4166 0.8222 0.2191 0.080 Uiso 1 1 calc R . .
H6C H 0.3859 0.7951 0.1146 0.080 Uiso 1 1 calc R . .
Si5 Si 0.40423(6) 0.96182(3) 0.16573(6) 0.03288(19) Uani 1 1 d . . .
C7 C 0.5105(3) 0.97969(15) 0.2866(2) 0.0477(8) Uani 1 1 d . . .
H7A H 0.4971 1.0130 0.3071 0.072 Uiso 1 1 calc R . .
H7B H 0.5735 0.9808 0.2789 0.072 Uiso 1 1 calc R . .
H7C H 0.5161 0.9546 0.3369 0.072 Uiso 1 1 calc R . .
Si6 Si 0.25446(7) 0.96827(4) 0.18695(7) 0.0443(2) Uani 1 1 d . A .
C8 C 0.1509(3) 0.92366(18) 0.1058(3) 0.0601(11) Uani 1 1 d . . .
H8A H 0.0912 0.9284 0.1186 0.090 Uiso 1 1 calc R . .
H8B H 0.1743 0.8887 0.1208 0.090 Uiso 1 1 calc R . .
H8C H 0.1337 0.9308 0.0361 0.090 Uiso 1 1 calc R . .
Si7 Si 0.19279(9) 1.05014(6) 0.15567(13) 0.0824(5) Uani 1 1 d . . .
C9 C 0.1520(5) 1.0643(3) 0.0191(6) 0.121(2) Uani 1 1 d . A .
H9A H 0.1257 1.0988 0.0047 0.182 Uiso 1 1 calc R . .
H9B H 0.0993 1.0404 -0.0208 0.182 Uiso 1 1 calc R . .
H9C H 0.2099 1.0609 0.0030 0.182 Uiso 1 1 calc R . .
C10 C 0.0816(4) 1.0576(3) 0.1837(6) 0.134(3) Uani 1 1 d . A .
H10A H 0.0570 1.0924 0.1700 0.201 Uiso 1 1 calc R . .
H10B H 0.1009 1.0499 0.2536 0.201 Uiso 1 1 calc R . .
H10C H 0.0283 1.0344 0.1425 0.201 Uiso 1 1 calc R . .
C11A C 0.2880(8) 1.0930(4) 0.2483(9) 0.096(4) Uiso 0.619(18) 1 d P A 1
H11A H 0.2631 1.1278 0.2367 0.143 Uiso 0.619(18) 1 calc PR A 1
H11B H 0.3516 1.0909 0.2417 0.143 Uiso 0.619(18) 1 calc PR A 1
H11C H 0.2991 1.0826 0.3151 0.143 Uiso 0.619(18) 1 calc PR A 1
C11B C 0.2946(11) 1.0995(6) 0.1969(13) 0.080(5) Uiso 0.381(18) 1 d P A 2
H11D H 0.2639 1.1332 0.1811 0.121 Uiso 0.381(18) 1 calc PR A 2
H11E H 0.3379 1.0944 0.1626 0.121 Uiso 0.381(18) 1 calc PR A 2
H11F H 0.3349 1.0968 0.2683 0.121 Uiso 0.381(18) 1 calc PR A 2
Si8 Si 0.58867(6) 0.88580(4) 0.12385(7) 0.0402(2) Uani 1 1 d . B .
C12 C 0.6166(3) 0.85187(16) 0.0280(3) 0.0614(11) Uani 1 1 d . . .
H12A H 0.5701 0.8635 -0.0379 0.092 Uiso 1 1 calc R . .
H12B H 0.6084 0.8154 0.0334 0.092 Uiso 1 1 calc R . .
H12C H 0.6860 0.8590 0.0385 0.092 Uiso 1 1 calc R . .
Si9 Si 0.70378(8) 0.85581(5) 0.28009(9) 0.0586(3) Uani 1 1 d . . .
C13 C 0.6511(5) 0.8610(3) 0.3779(4) 0.115(2) Uani 1 1 d . B .
H13A H 0.7010 0.8482 0.4413 0.173 Uiso 1 1 calc R . .
H13B H 0.5892 0.8410 0.3569 0.173 Uiso 1 1 calc R . .
H13C H 0.6362 0.8965 0.3852 0.173 Uiso 1 1 calc R . .
Si1A Si 0.85266(15) 0.90122(8) 0.35326(18) 0.0564(6) Uani 0.631(5) 1 d PD B 3
C14A C 0.9662(6) 0.8629(3) 0.4099(6) 0.070(2) Uiso 0.631(5) 1 d PD B 3
H14A H 1.0251 0.8850 0.4398 0.105 Uiso 0.631(5) 1 calc PR B 3
H14B H 0.9732 0.8418 0.3594 0.105 Uiso 0.631(5) 1 calc PR B 3
H14C H 0.9614 0.8413 0.4610 0.105 Uiso 0.631(5) 1 calc PR B 3
C15A C 0.8634(6) 0.9463(3) 0.2605(6) 0.077(2) Uiso 0.631(5) 1 d PD B 3
H15A H 0.9260 0.9656 0.2918 0.116 Uiso 0.631(5) 1 calc PR B 3
H15B H 0.8059 0.9694 0.2369 0.116 Uiso 0.631(5) 1 calc PR B 3
H15C H 0.8639 0.9271 0.2046 0.116 Uiso 0.631(5) 1 calc PR B 3
C16A C 0.8575(8) 0.9393(4) 0.4601(7) 0.107(3) Uiso 0.631(5) 1 d PD B 3
H16A H 0.9212 0.9579 0.4890 0.160 Uiso 0.631(5) 1 calc PR B 3
H16B H 0.8527 0.9168 0.5099 0.160 Uiso 0.631(5) 1 calc PR B 3
H16C H 0.8012 0.9632 0.4375 0.160 Uiso 0.631(5) 1 calc PR B 3
Si1B Si 0.8666(3) 0.88903(17) 0.3040(4) 0.0721(15) Uani 0.369(5) 1 d PD B 4
C14B C 0.9661(8) 0.8487(5) 0.3912(8) 0.054(3) Uiso 0.369(5) 1 d PD B 4
H14D H 1.0320 0.8627 0.4025 0.081 Uiso 0.369(5) 1 calc PR B 4
H14E H 0.9597 0.8146 0.3638 0.081 Uiso 0.369(5) 1 calc PR B 4
H14F H 0.9600 0.8473 0.4539 0.081 Uiso 0.369(5) 1 calc PR B 4
C15B C 0.8936(19) 0.8916(11) 0.1953(13) 0.177(11) Uiso 0.369(5) 1 d PD B 4
H15D H 0.9610 0.9057 0.2140 0.266 Uiso 0.369(5) 1 calc PR B 4
H15E H 0.8436 0.9130 0.1448 0.266 Uiso 0.369(5) 1 calc PR B 4
H15F H 0.8906 0.8574 0.1690 0.266 Uiso 0.369(5) 1 calc PR B 4
C16B C 0.865(3) 0.9553(6) 0.342(3) 0.217(15) Uiso 0.369(5) 1 d PD B 4
H16D H 0.9297 0.9713 0.3534 0.325 Uiso 0.369(5) 1 calc PR B 4
H16E H 0.8557 0.9562 0.4028 0.325 Uiso 0.369(5) 1 calc PR B 4
H16F H 0.8103 0.9735 0.2895 0.325 Uiso 0.369(5) 1 calc PR B 4
Si11 Si 0.13536(8) 0.79916(4) -0.21148(9) 0.0567(3) Uani 1 1 d . . .
C17 C 0.1265(5) 0.7333(2) -0.2624(6) 0.115(2) Uani 1 1 d . . .
H17A H 0.0594 0.7195 -0.2783 0.173 Uiso 1 1 calc R . .
H17B H 0.1776 0.7119 -0.2130 0.173 Uiso 1 1 calc R . .
H17C H 0.1380 0.7344 -0.3223 0.173 Uiso 1 1 calc R . .
C18 C 0.0359(3) 0.8397(2) -0.3062(3) 0.0699(13) Uani 1 1 d . . .
H18A H -0.0309 0.8259 -0.3202 0.105 Uiso 1 1 calc R . .
H18B H 0.0457 0.8401 -0.3671 0.105 Uiso 1 1 calc R . .
H18C H 0.0409 0.8742 -0.2808 0.105 Uiso 1 1 calc R . .
C19 C 0.1080(4) 0.7959(2) -0.0998(4) 0.0758(14) Uani 1 1 d . . .
H19A H 0.0398 0.7827 -0.1189 0.114 Uiso 1 1 calc R . .
H19B H 0.1130 0.8297 -0.0716 0.114 Uiso 1 1 calc R . .
H19C H 0.1568 0.7734 -0.0505 0.114 Uiso 1 1 calc R . .
Si12 Si 0.28761(9) 0.94323(8) 0.34913(9) 0.0840(5) Uani 1 1 d . . .
C20 C 0.1633(4) 0.9288(4) 0.3511(4) 0.135(3) Uani 1 1 d . A .
H20A H 0.1742 0.9183 0.4177 0.202 Uiso 1 1 calc R . .
H20B H 0.1299 0.9016 0.3042 0.202 Uiso 1 1 calc R . .
H20C H 0.1209 0.9591 0.3324 0.202 Uiso 1 1 calc R . .
C21 C 0.3471(5) 0.9960(3) 0.4390(4) 0.138(3) Uani 1 1 d . A .
H21A H 0.3601 0.9847 0.5058 0.206 Uiso 1 1 calc R . .
H21B H 0.3015 1.0251 0.4211 0.206 Uiso 1 1 calc R . .
H21C H 0.4107 1.0057 0.4371 0.206 Uiso 1 1 calc R . .
C22 C 0.3677(5) 0.8860(3) 0.3889(5) 0.127(3) Uani 1 1 d . A .
H22A H 0.3792 0.8772 0.4566 0.190 Uiso 1 1 calc R . .
H22B H 0.4325 0.8926 0.3867 0.190 Uiso 1 1 calc R . .
H22C H 0.3339 0.8579 0.3446 0.190 Uiso 1 1 calc R . .
Si13 Si 0.72440(12) 0.76892(6) 0.26715(15) 0.0976(6) Uani 1 1 d . B .
C23 C 0.8045(5) 0.7550(3) 0.2002(7) 0.137(3) Uani 1 1 d . . .
H23A H 0.8115 0.7184 0.1962 0.205 Uiso 1 1 calc R B .
H23B H 0.8711 0.7702 0.2360 0.205 Uiso 1 1 calc R . .
H23C H 0.7726 0.7692 0.1334 0.205 Uiso 1 1 calc R . .
C24 C 0.6015(6) 0.7377(2) 0.1974(8) 0.164(4) Uani 1 1 d . . .
H24A H 0.6119 0.7014 0.1929 0.245 Uiso 1 1 calc R B .
H24B H 0.5693 0.7521 0.1308 0.245 Uiso 1 1 calc R . .
H24C H 0.5581 0.7431 0.2316 0.245 Uiso 1 1 calc R . .
C25 C 0.7939(7) 0.7420(3) 0.3941(7) 0.178(4) Uani 1 1 d . . .
H25A H 0.8029 0.7056 0.3894 0.267 Uiso 1 1 calc R B .
H25B H 0.7552 0.7481 0.4328 0.267 Uiso 1 1 calc R . .
H25C H 0.8599 0.7583 0.4266 0.267 Uiso 1 1 calc R . .
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Zr1 Zr1 O2 126.9(3) 3_675 3_675
Zr1 Zr1 O3 129.1(3) 3_675 .
O2 Zr1 O3 103.83(10) 3_675 .
Zr1 Zr1 O1 84.0(2) 3_675 .
O2 Zr1 O1 95.70(10) 3_675 .
O3 Zr1 O1 95.51(10) . .
Zr1 Zr1 O1 79.6(2) 3_675 3_675
O2 Zr1 O1 94.19(9) 3_675 3_675
O3 Zr1 O1 94.88(11) . 3_675
O1 Zr1 O1 163.52(3) . 3_675
Zr1 Zr1 O2 41.2(2) 3_675 .
O2 Zr1 O2 168.18(5) 3_675 .
O3 Zr1 O2 87.97(10) . .
O1 Zr1 O2 83.74(8) . .
O1 Zr1 O2 83.87(9) 3_675 .
Zr1 Zr1 O3 39.5(2) 3_675 3_675
O2 Zr1 O3 87.51(10) 3_675 3_675
O3 Zr1 O3 168.63(6) . 3_675
O1 Zr1 O3 83.95(9) . 3_675
O1 Zr1 O3 83.36(9) 3_675 3_675
O2 Zr1 O3 80.68(8) . 3_675
Si3 O1 Zr1 137.12(13) . .
Si3 O1 Zr1 129.73(12) . 3_675
Zr1 O1 Zr1 16.48(3) . 3_675
Si5 O2 Zr1 138.59(13) . 3_675
Si5 O2 Zr1 127.18(12) . .
Zr1 O2 Zr1 11.83(5) 3_675 .
Si8 O3 Zr1 134.21(14) . .
Si8 O3 Zr1 132.00(12) . 3_675
Zr1 O3 Zr1 11.37(6) . 3_675
C1 Si1 C2 107.1(2) . .
C1 Si1 C3 109.8(2) . .
C2 Si1 C3 110.1(2) . .
C1 Si1 Si2 110.32(14) . .
C2 Si1 Si2 108.00(17) . .
C3 Si1 Si2 111.45(17) . .
C4 Si2 Si1 109.57(16) . .
C4 Si2 Si11 107.54(15) . .
Si1 Si2 Si11 110.19(5) . .
C4 Si2 Si3 114.08(14) . .
Si1 Si2 Si3 104.69(5) . .
Si11 Si2 Si3 110.76(5) . .
O1 Si3 C5 107.19(15) . .
O1 Si3 Si2 113.32(9) . .
C5 Si3 Si2 105.63(11) . .
O1 Si3 Si4 100.81(9) . .
C5 Si3 Si4 114.54(11) . .
Si2 Si3 Si4 115.28(5) . .
C6 Si4 Si5 117.42(14) . .
C6 Si4 Si8 117.87(13) . .
Si5 Si4 Si8 100.69(4) . .
C6 Si4 Si3 117.02(13) . .
Si5 Si4 Si3 99.41(4) . .
Si8 Si4 Si3 101.25(4) . .
O2 Si5 C7 105.68(14) . .
O2 Si5 Si6 114.87(9) . .
C7 Si5 Si6 107.02(12) . .
O2 Si5 Si4 101.49(8) . .
C7 Si5 Si4 115.81(13) . .
Si6 Si5 Si4 112.01(5) . .
C8 Si6 Si7 108.33(15) . .
C8 Si6 Si5 114.06(14) . .
Si7 Si6 Si5 110.30(6) . .
C8 Si6 Si12 104.03(14) . .
Si7 Si6 Si12 111.30(8) . .
Si5 Si6 Si12 108.71(5) . .
C10 Si7 C11A 102.6(5) . .
C10 Si7 C11B 120.2(6) . .
C11A Si7 C11B 25.6(5) . .
C10 Si7 C9 108.3(3) . .
C11A Si7 C9 118.1(5) . .
C11B Si7 C9 93.4(6) . .
C10 Si7 Si6 111.0(3) . .
C11A Si7 Si6 108.2(3) . .
C11B Si7 Si6 113.4(5) . .
C9 Si7 Si6 108.5(2) . .
O3 Si8 C12 105.45(17) . .
O3 Si8 Si4 99.93(9) . .
C12 Si8 Si4 115.44(14) . .
O3 Si8 Si9 115.07(9) . .
C12 Si8 Si9 107.32(14) . .
Si4 Si8 Si9 113.48(5) . .
C13 Si9 Si1A 101.8(2) . .
C13 Si9 Si13 103.9(2) . .
Si1A Si9 Si13 114.83(8) . .
C13 Si9 Si8 112.16(18) . .
Si1A Si9 Si8 115.26(7) . .
Si13 Si9 Si8 108.17(7) . .
C13 Si9 Si1B 123.3(3) . .
Si1A Si9 Si1B 21.81(12) . .
Si13 Si9 Si1B 102.44(13) . .
Si8 Si9 Si1B 105.65(12) . .
C14A Si1A C16A 102.0(4) . .
C14A Si1A C15A 110.4(4) . .
C16A Si1A C15A 107.6(4) . .
C14A Si1A Si9 115.0(3) . .
C16A Si1A Si9 111.8(4) . .
C15A Si1A Si9 109.7(3) . .
C15B Si1B C14B 104.2(10) . .
C15B Si1B C16B 105.7(14) . .
C14B Si1B C16B 116.3(12) . .
C15B Si1B Si9 117.0(9) . .
C14B Si1B Si9 109.4(5) . .
C16B Si1B Si9 104.7(11) . .
C19 Si11 C18 107.8(2) . .
C19 Si11 C17 108.2(3) . .
C18 Si11 C17 109.0(3) . .
C19 Si11 Si2 112.65(16) . .
C18 Si11 Si2 111.12(15) . .
C17 Si11 Si2 108.0(2) . .
C22 Si12 C20 108.4(4) . .
C22 Si12 C21 109.9(3) . .
C20 Si12 C21 107.5(3) . .
C22 Si12 Si6 112.7(2) . .
C20 Si12 Si6 107.17(19) . .
C21 Si12 Si6 110.9(3) . .
C24 Si13 C25 112.5(4) . .
C24 Si13 C23 107.0(5) . .
C25 Si13 C23 105.8(4) . .
C24 Si13 Si9 110.9(2) . .
C25 Si13 Si9 108.9(3) . .
C23 Si13 Si9 111.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 Zr1 0.5984(11) 3_675
Zr1 O2 1.925(2) 3_675
Zr1 O3 1.932(2) .
Zr1 O1 2.075(2) .
Zr1 O1 2.098(2) 3_675
Zr1 O2 2.334(2) .
Zr1 O3 2.356(2) 3_675
O1 Si3 1.662(2) .
O1 Zr1 2.098(2) 3_675
O2 Si5 1.676(2) .
O2 Zr1 1.925(2) 3_675
O3 Si8 1.670(2) .
O3 Zr1 2.356(2) 3_675
Si1 C1 1.865(4) .
Si1 C2 1.875(5) .
Si1 C3 1.878(4) .
Si1 Si2 2.3421(14) .
Si2 C4 1.901(4) .
Si2 Si11 2.3479(14) .
Si2 Si3 2.3537(12) .
Si3 C5 1.878(3) .
Si3 Si4 2.3616(12) .
Si4 C6 1.886(4) .
Si4 Si5 2.3567(12) .
Si4 Si8 2.3612(12) .
Si5 C7 1.878(3) .
Si5 Si6 2.3546(12) .
Si6 C8 1.901(4) .
Si6 Si7 2.3189(18) .
Si6 Si12 2.3563(16) .
Si7 C10 1.858(6) .
Si7 C11A 1.875(10) .
Si7 C11B 1.881(15) .
Si7 C9 1.905(8) .
Si8 C12 1.878(4) .
Si8 Si9 2.3644(14) .
Si9 C13 1.927(6) .
Si9 Si1A 2.320(2) .
Si9 Si13 2.339(2) .
Si9 Si1B 2.424(4) .
Si1A C14A 1.823(7) .
Si1A C16A 1.864(8) .
Si1A C15A 1.885(7) .
Si1B C15B 1.829(11) .
Si1B C14B 1.832(8) .
Si1B C16B 1.846(11) .
Si11 C19 1.877(5) .
Si11 C18 1.881(5) .
Si11 C17 1.884(6) .
Si12 C22 1.855(8) .
Si12 C20 1.874(5) .
Si12 C21 1.877(7) .
Si13 C24 1.851(7) .
Si13 C25 1.873(8) .
Si13 C23 1.874(8) .
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_4
Zr1 Zr1 O1 Si3 -70.8(3) 3_675 .
O2 Zr1 O1 Si3 162.55(19) 3_675 .
O3 Zr1 O1 Si3 58.0(2) . .
O1 Zr1 O1 Si3 -70.8(3) 3_675 .
O2 Zr1 O1 Si3 -29.32(19) . .
O3 Zr1 O1 Si3 -110.6(2) 3_675 .
O2 Zr1 O1 Zr1 -126.6(3) 3_675 3_675
O3 Zr1 O1 Zr1 128.8(3) . 3_675
O1 Zr1 O1 Zr1 0.0 3_675 3_675
O2 Zr1 O1 Zr1 41.5(2) . 3_675
O3 Zr1 O1 Zr1 -39.8(2) 3_675 3_675
Zr1 Zr1 O2 Si5 166.1(3) 3_675 .
O2 Zr1 O2 Si5 166.0(3) 3_675 .
O3 Zr1 O2 Si5 -17.67(16) . .
O1 Zr1 O2 Si5 78.10(15) . .
O1 Zr1 O2 Si5 -112.79(15) 3_675 .
O3 Zr1 O2 Si5 162.96(15) 3_675 .
O2 Zr1 O2 Zr1 -0.013(4) 3_675 3_675
O3 Zr1 O2 Zr1 176.3(4) . 3_675
O1 Zr1 O2 Zr1 -88.0(3) . 3_675
O1 Zr1 O2 Zr1 81.1(3) 3_675 3_675
O3 Zr1 O2 Zr1 -3.1(3) 3_675 3_675
Zr1 Zr1 O3 Si8 84.1(4) 3_675 .
O2 Zr1 O3 Si8 -99.8(2) 3_675 .
O1 Zr1 O3 Si8 -2.6(2) . .
O1 Zr1 O3 Si8 164.62(19) 3_675 .
O2 Zr1 O3 Si8 80.9(2) . .
O3 Zr1 O3 Si8 84.1(4) 3_675 .
O2 Zr1 O3 Zr1 176.0(4) 3_675 3_675
O1 Zr1 O3 Zr1 -86.7(3) . 3_675
O1 Zr1 O3 Zr1 80.5(3) 3_675 3_675
O2 Zr1 O3 Zr1 -3.2(3) . 3_675
O3 Zr1 O3 Zr1 0.000(2) 3_675 3_675
C1 Si1 Si2 C4 -168.3(2) . .
C2 Si1 Si2 C4 -51.5(2) . .
C3 Si1 Si2 C4 69.5(2) . .
C1 Si1 Si2 Si11 73.61(17) . .
C2 Si1 Si2 Si11 -169.67(18) . .
C3 Si1 Si2 Si11 -48.66(18) . .
C1 Si1 Si2 Si3 -45.52(17) . .
C2 Si1 Si2 Si3 71.20(19) . .
C3 Si1 Si2 Si3 -167.79(17) . .
Zr1 O1 Si3 C5 90.6(2) . .
Zr1 O1 Si3 C5 70.2(2) 3_675 .
Zr1 O1 Si3 Si2 -153.25(15) . .
Zr1 O1 Si3 Si2 -173.64(12) 3_675 .
Zr1 O1 Si3 Si4 -29.5(2) . .
Zr1 O1 Si3 Si4 -49.88(16) 3_675 .
C4 Si2 Si3 O1 87.5(2) . .
Si1 Si2 Si3 O1 -32.31(11) . .
Si11 Si2 Si3 O1 -151.05(10) . .
C4 Si2 Si3 C5 -155.5(2) . .
Si1 Si2 Si3 C5 84.74(13) . .
Si11 Si2 Si3 C5 -34.00(13) . .
C4 Si2 Si3 Si4 -27.97(19) . .
Si1 Si2 Si3 Si4 -147.73(5) . .
Si11 Si2 Si3 Si4 93.52(6) . .
O1 Si3 Si4 C6 -164.06(17) . .
C5 Si3 Si4 C6 81.2(2) . .
Si2 Si3 Si4 C6 -41.66(16) . .
O1 Si3 Si4 Si5 68.46(9) . .
C5 Si3 Si4 Si5 -46.24(13) . .
Si2 Si3 Si4 Si5 -169.14(5) . .
O1 Si3 Si4 Si8 -34.52(9) . .
C5 Si3 Si4 Si8 -149.22(13) . .
Si2 Si3 Si4 Si8 87.88(5) . .
Zr1 O2 Si5 C7 85.9(2) 3_675 .
Zr1 O2 Si5 C7 81.65(19) . .
Zr1 O2 Si5 Si6 -156.34(16) 3_675 .
Zr1 O2 Si5 Si6 -160.62(10) . .
Zr1 O2 Si5 Si4 -35.3(2) 3_675 .
Zr1 O2 Si5 Si4 -39.58(14) . .
C6 Si4 Si5 O2 -162.15(15) . .
Si8 Si4 Si5 O2 68.50(9) . .
Si3 Si4 Si5 O2 -34.94(9) . .
C6 Si4 Si5 C7 83.98(19) . .
Si8 Si4 Si5 C7 -45.36(14) . .
Si3 Si4 Si5 C7 -148.81(13) . .
C6 Si4 Si5 Si6 -39.12(15) . .
Si8 Si4 Si5 Si6 -168.47(5) . .
Si3 Si4 Si5 Si6 88.09(5) . .
O2 Si5 Si6 C8 92.03(18) . .
C7 Si5 Si6 C8 -151.0(2) . .
Si4 Si5 Si6 C8 -23.07(17) . .
O2 Si5 Si6 Si7 -30.13(11) . .
C7 Si5 Si6 Si7 86.83(15) . .
Si4 Si5 Si6 Si7 -145.24(6) . .
O2 Si5 Si6 Si12 -152.42(10) . .
C7 Si5 Si6 Si12 -35.45(15) . .
Si4 Si5 Si6 Si12 92.48(7) . .
C8 Si6 Si7 C10 60.0(3) . .
Si5 Si6 Si7 C10 -174.5(3) . .
Si12 Si6 Si7 C10 -53.8(3) . .
C8 Si6 Si7 C11A 171.9(5) . .
Si5 Si6 Si7 C11A -62.6(5) . .
Si12 Si6 Si7 C11A 58.1(5) . .
C8 Si6 Si7 C11B -161.2(7) . .
Si5 Si6 Si7 C11B -35.7(7) . .
Si12 Si6 Si7 C11B 85.0(7) . .
C8 Si6 Si7 C9 -58.9(3) . .
Si5 Si6 Si7 C9 66.6(2) . .
Si12 Si6 Si7 C9 -172.7(2) . .
Zr1 O3 Si8 C12 71.2(2) . .
Zr1 O3 Si8 C12 86.5(2) 3_675 .
Zr1 O3 Si8 Si4 -48.9(2) . .
Zr1 O3 Si8 Si4 -33.59(19) 3_675 .
Zr1 O3 Si8 Si9 -170.79(15) . .
Zr1 O3 Si8 Si9 -155.49(13) 3_675 .
C6 Si4 Si8 O3 -163.94(18) . .
Si5 Si4 Si8 O3 -34.90(10) . .
Si3 Si4 Si8 O3 67.06(10) . .
C6 Si4 Si8 C12 83.6(2) . .
Si5 Si4 Si8 C12 -147.40(16) . .
Si3 Si4 Si8 C12 -45.45(16) . .
C6 Si4 Si8 Si9 -40.92(17) . .
Si5 Si4 Si8 Si9 88.13(6) . .
Si3 Si4 Si8 Si9 -169.92(5) . .
O3 Si8 Si9 C13 89.9(3) . .
C12 Si8 Si9 C13 -153.1(3) . .
Si4 Si8 Si9 C13 -24.4(3) . .
O3 Si8 Si9 Si1A -26.05(15) . .
C12 Si8 Si9 Si1A 90.95(17) . .
Si4 Si8 Si9 Si1A -140.30(10) . .
O3 Si8 Si9 Si13 -156.10(11) . .
C12 Si8 Si9 Si13 -39.10(16) . .
Si4 Si8 Si9 Si13 89.65(8) . .
O3 Si8 Si9 Si1B -46.99(19) . .
C12 Si8 Si9 Si1B 70.0(2) . .
Si4 Si8 Si9 Si1B -161.24(16) . .
C13 Si9 Si1A C14A 101.8(4) . .
Si13 Si9 Si1A C14A -9.7(4) . .
Si8 Si9 Si1A C14A -136.5(3) . .
Si1B Si9 Si1A C14A -68.6(4) . .
C13 Si9 Si1A C16A -13.8(4) . .
Si13 Si9 Si1A C16A -125.4(4) . .
Si8 Si9 Si1A C16A 107.9(4) . .
Si1B Si9 Si1A C16A 175.8(5) . .
C13 Si9 Si1A C15A -133.0(4) . .
Si13 Si9 Si1A C15A 115.4(3) . .
Si8 Si9 Si1A C15A -11.4(3) . .
Si1B Si9 Si1A C15A 56.5(4) . .
C13 Si9 Si1B C15B -168.5(10) . .
Si1A Si9 Si1B C15B -157.2(11) . .
Si13 Si9 Si1B C15B 75.5(10) . .
Si8 Si9 Si1B C15B -37.7(10) . .
C13 Si9 Si1B C14B 73.4(6) . .
Si1A Si9 Si1B C14B 84.7(6) . .
Si13 Si9 Si1B C14B -42.7(5) . .
Si8 Si9 Si1B C14B -155.8(5) . .
C13 Si9 Si1B C16B -51.9(12) . .
Si1A Si9 Si1B C16B -40.7(12) . .
Si13 Si9 Si1B C16B -168.0(12) . .
Si8 Si9 Si1B C16B 78.8(12) . .
C4 Si2 Si11 C19 81.3(2) . .
Si1 Si2 Si11 C19 -159.29(18) . .
Si3 Si2 Si11 C19 -43.93(19) . .
C4 Si2 Si11 C18 -157.5(2) . .
Si1 Si2 Si11 C18 -38.16(18) . .
Si3 Si2 Si11 C18 77.20(18) . .
C4 Si2 Si11 C17 -38.1(3) . .
Si1 Si2 Si11 C17 81.3(3) . .
Si3 Si2 Si11 C17 -163.3(3) . .
C8 Si6 Si12 C22 79.0(3) . .
Si7 Si6 Si12 C22 -164.6(3) . .
Si5 Si6 Si12 C22 -42.9(3) . .
C8 Si6 Si12 C20 -40.3(4) . .
Si7 Si6 Si12 C20 76.2(3) . .
Si5 Si6 Si12 C20 -162.1(3) . .
C8 Si6 Si12 C21 -157.3(3) . .
Si7 Si6 Si12 C21 -40.8(2) . .
Si5 Si6 Si12 C21 80.8(2) . .
C13 Si9 Si13 C24 75.0(4) . .
Si1A Si9 Si13 C24 -174.7(4) . .
Si8 Si9 Si13 C24 -44.4(4) . .
Si1B Si9 Si13 C24 -155.7(4) . .
C13 Si9 Si13 C25 -49.3(4) . .
Si1A Si9 Si13 C25 61.1(4) . .
Si8 Si9 Si13 C25 -168.7(4) . .
Si1B Si9 Si13 C25 80.0(4) . .
C13 Si9 Si13 C23 -165.8(3) . .
Si1A Si9 Si13 C23 -55.4(3) . .
Si8 Si9 Si13 C23 74.9(3) . .
Si1B Si9 Si13 C23 -36.4(3) . .
