#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:08:14 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178936 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/65/4116502.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_4116502
loop_
_publ_author_name
'Oleg V. Ozerov'
'Folami T. Ladipo'
'Brian O. Patrick'
_publ_section_title
;
 Highly Regioselective Alkyne Cyclotrimerization Catalyzed by Titanium
 Complexes Supported by Proximally Bridged p-tert-Butylcalix[4]arene
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7941
_journal_page_last               7942
_journal_paper_doi               10.1021/ja990740b
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C54 H76 Cl2 O4 Si Ti'
_chemical_formula_weight         936.04
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 124.79(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.750(1)
_cell_length_b                   17.0434(9)
_cell_length_c                   17.1877(9)
_cell_measurement_reflns_used    22618
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.39
_cell_volume                     4991.9(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7735
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.347
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.194
_refine_ls_goodness_of_fit_obs   1.258
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.256
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_obs          0.1231
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0685P)²+42.4482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2649
_refine_ls_wR_factor_obs         0.2505
_reflns_number_observed          3542
_reflns_number_total             4382
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990740b.cif
_cod_data_source_block           k99013
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+42.4482P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+42.4482P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4991.9(4)
_cod_database_code               4116502
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.02621(8) 0.11177(8) 0.10898(9) 0.0346(4) Uani 0.50 d P 1
Cl1 Cl -0.0906(4) 0.1668(5) 0.0031(6) 0.0514(15) Uani 0.50 d P 1
Cl2 Cl 0.0817(4) 0.1862(3) 0.2360(4) 0.0629(14) Uani 0.50 d P 1
Si1 Si 0.02621(8) 0.11177(8) 0.10898(9) 0.0346(4) Uani 0.50 d P 2
C23 C -0.0651(19) 0.1476(18) 0.0186(28) 0.065(9) Uani 0.50 d P 2
H23A H -0.0987 0.1523 0.0414 0.098 Uiso 0.50 calc P 2
H23B H -0.0892 0.1114 -0.0353 0.098 Uiso 0.50 calc P 2
H23C H -0.0588 0.1992 -0.0013 0.098 Uiso 0.50 calc P 2
C24 C 0.0833(18) 0.1541(11) 0.2327(26) 0.112(14) Uani 0.50 d P 2
H24A H 0.0492 0.1575 0.2550 0.168 Uiso 0.50 calc P 2
H24B H 0.1021 0.2067 0.2320 0.168 Uiso 0.50 calc P 2
H24C H 0.1282 0.1202 0.2753 0.168 Uiso 0.50 calc P 2
O1 O 0.0140(2) 0.0181(2) 0.1345(3) 0.0383(11) Uani 1 d . .
O2 O 0.0829(2) 0.1046(2) 0.0664(3) 0.0375(10) Uani 1 d . .
C1 C -0.0010(3) -0.1189(3) 0.1433(4) 0.0310(13) Uani 1 d . .
C2 C 0.0336(4) -0.1927(3) 0.1744(4) 0.0353(14) Uani 1 d . .
H2 H 0.0006 -0.2368 0.1599 0.042 Uiso 1 calc . .
C3 C 0.1139(4) -0.2043(4) 0.2254(4) 0.043(2) Uani 1 d . .
C4 C 0.1601(3) -0.1382(4) 0.2437(4) 0.038(2) Uani 1 d . .
H4 H 0.2154 -0.1444 0.2789 0.045 Uiso 1 calc . .
C5 C 0.1285(3) -0.0638(3) 0.2125(4) 0.0322(13) Uani 1 d . .
C6 C 0.1821(3) 0.0032(4) 0.2277(4) 0.0353(14) Uani 1 d . .
H6A H 0.1614 0.0527 0.2356 0.042 Uiso 1 calc . .
H6B H 0.2349 -0.0060 0.2865 0.042 Uiso 1 calc . .
C7 C 0.1887(3) 0.0112(3) 0.1452(4) 0.0312(13) Uani 1 d . .
C8 C 0.2444(3) -0.0318(4) 0.1438(4) 0.0339(14) Uani 1 d . .
H8 H 0.2806 -0.0624 0.1978 0.041 Uiso 1 calc . .
C9 C 0.2500(3) -0.0325(4) 0.0672(4) 0.0332(13) Uani 1 d . .
C10 C 0.1955(3) 0.0135(4) -0.0108(4) 0.0348(14) Uani 1 d . .
H10 H 0.1972 0.0137 -0.0649 0.042 Uiso 1 calc . .
C11 C 0.1393(3) 0.0585(3) -0.0126(4) 0.0277(12) Uani 1 d . .
C12 C 0.0885(3) 0.1131(4) -0.0970(4) 0.0359(14) Uani 1 d . .
H12A H 0.1104 0.1666 -0.0765 0.043 Uiso 1 calc . .
H12B H 0.0960 0.0975 -0.1468 0.043 Uiso 1 calc . .
C13 C 0.0474(3) -0.0551(3) 0.1633(4) 0.0294(13) Uani 1 d . .
C14 C 0.1364(3) 0.0573(3) 0.0666(4) 0.0276(12) Uani 1 d . .
C15 C 0.1520(4) -0.2852(4) 0.2607(5) 0.055(2) Uani 1 d D .
C16A C 0.0939(9) -0.3470(8) 0.2483(13) 0.086(3) Uani 0.65(2) d PD 3
H16A H 0.1199(19) -0.3982(14) 0.2686(74) 0.129 Uiso 0.65(2) calc PR 3
H16B H 0.0497(33) -0.3497(46) 0.1815(18) 0.129 Uiso 0.65(2) calc PR 3
H16C H 0.0745(50) -0.3329(35) 0.2868(62) 0.129 Uiso 0.65(2) calc PR 3
C17A C 0.2139(11) -0.2797(10) 0.3685(11) 0.086(3) Uani 0.65(2) d PD 3
H17A H 0.1887(16) -0.2621(60) 0.3994(13) 0.129 Uiso 0.65(2) calc PR 3
H17B H 0.2547(35) -0.2422(48) 0.3816(11) 0.129 Uiso 0.65(2) calc PR 3
H17C H 0.2376(45) -0.3314(17) 0.3932(16) 0.129 Uiso 0.65(2) calc PR 3
C18A C 0.1973(16) -0.3008(16) 0.2164(17) 0.086(3) Uani 0.65(2) d PD 3
H18A H 0.2327(46) -0.2568(35) 0.2304(64) 0.129 Uiso 0.65(2) calc PR 3
H18B H 0.1602(16) -0.3064(63) 0.1477(20) 0.129 Uiso 0.65(2) calc PR 3
H18C H 0.2279(54) -0.3491(39) 0.2430(62) 0.129 Uiso 0.65(2) calc PR 3
C16B C 0.0931(15) -0.3519(13) 0.2005(21) 0.086(3) Uani 0.35(2) d PD 4
H16D H 0.0819(92) -0.3515(75) 0.1369(49) 0.129 Uiso 0.35(2) calc PR 4
H16E H 0.0443(45) -0.3437(65) 0.1959(118) 0.129 Uiso 0.35(2) calc PR 4
H16F H 0.1159(49) -0.4026(16) 0.2308(78) 0.129 Uiso 0.35(2) calc PR 4
C17B C 0.1857(21) -0.2985(20) 0.3616(19) 0.086(3) Uani 0.35(2) d PD 4
H17D H 0.1433(22) -0.3062(117) 0.3701(26) 0.129 Uiso 0.35(2) calc PR 4
H17E H 0.2171(96) -0.2528(53) 0.3984(25) 0.129 Uiso 0.35(2) calc PR 4
H17F H 0.2192(96) -0.3452(70) 0.3835(41) 0.129 Uiso 0.35(2) calc PR 4
C18B C 0.2076(29) -0.3085(30) 0.2362(33) 0.086(3) Uani 0.35(2) d PD 4
H18D H 0.1861(61) -0.2929(110) 0.1708(56) 0.129 Uiso 0.35(2) calc PR 4
H18E H 0.2151(94) -0.3655(31) 0.2424(140) 0.129 Uiso 0.35(2) calc PR 4
H18F H 0.2581(46) -0.2823(93) 0.2792(95) 0.129 Uiso 0.35(2) calc PR 4
C19 C 0.3117(4) -0.0826(4) 0.0682(5) 0.048(2) Uani 1 d D .
C20A C 0.3086(7) -0.1674(7) 0.0973(9) 0.080(2) Uani 0.747(9) d PD 5
H20A H 0.2597(24) -0.1924(18) 0.0467(27) 0.121 Uiso 0.747(9) calc PR 5
H20B H 0.3106(50) -0.1666(8) 0.1557(34) 0.121 Uiso 0.747(9) calc PR 5
H20C H 0.3534(28) -0.1970(16) 0.1080(59) 0.121 Uiso 0.747(9) calc PR 5
C21A C 0.3929(7) -0.0532(8) 0.1457(9) 0.080(2) Uani 0.747(9) d PD 5
H21A H 0.4006(21) -0.0004(23) 0.1298(33) 0.121 Uiso 0.747(9) calc PR 5
H21B H 0.4326(7) -0.0886(30) 0.1512(45) 0.121 Uiso 0.747(9) calc PR 5
H21C H 0.3982(20) -0.0517(51) 0.2060(15) 0.121 Uiso 0.747(9) calc PR 5
C22A C 0.3027(8) -0.0862(9) -0.0249(9) 0.080(2) Uani 0.747(9) d PD 5
H22A H 0.3058(51) -0.0331(11) -0.0444(31) 0.121 Uiso 0.747(9) calc PR 5
H22B H 0.2517(24) -0.1094(47) -0.0730(17) 0.121 Uiso 0.747(9) calc PR 5
H22C H 0.3447(32) -0.1186(43) -0.0180(18) 0.121 Uiso 0.747(9) calc PR 5
C20B C 0.2712(20) -0.1295(23) -0.0237(21) 0.080(2) Uani 0.253(9) d PD 6
H20D H 0.2360(117) -0.0949(41) -0.0773(27) 0.121 Uiso 0.253(9) calc PR 6
H20E H 0.2407(126) -0.1722(96) -0.0214(79) 0.121 Uiso 0.253(9) calc PR 6
H20F H 0.3108(22) -0.1514(130) -0.0316(95) 0.121 Uiso 0.253(9) calc PR 6
C21B C 0.3607(20) -0.0232(19) 0.0512(28) 0.080(2) Uani 0.253(9) d PD 6
H21D H 0.3249(20) 0.0110(105) -0.0025(123) 0.121 Uiso 0.253(9) calc PR 6
H21E H 0.3938(118) -0.0524(19) 0.0375(189) 0.121 Uiso 0.253(9) calc PR 6
H21F H 0.3939(118) 0.0089(108) 0.1081(73) 0.121 Uiso 0.253(9) calc PR 6
C22B C 0.3724(20) -0.1209(25) 0.1613(21) 0.080(2) Uani 0.253(9) d PD 6
H22D H 0.3502(56) -0.1683(89) 0.1696(90) 0.121 Uiso 0.253(9) calc PR 6
H22E H 0.3883(117) -0.0843(61) 0.2132(25) 0.121 Uiso 0.253(9) calc PR 6
H22F H 0.4183(69) -0.1351(146) 0.1614(78) 0.121 Uiso 0.253(9) calc PR 6
C25 C 0.0216(22) 0.4638(17) 0.0244(25) 0.338(18) Uiso 1 d D .
H25A H 0.0663 0.4778 0.0212 0.406 Uiso 1 calc . .
H25B H -0.0118 0.4312 -0.0329 0.406 Uiso 1 calc . .
C26 C 0.0632(11) 0.3939(11) 0.0861(14) 0.188(7) Uiso 1 d D .
H26A H 0.0288 0.3749 0.1048 0.225 Uiso 1 calc . .
H26B H 0.1104 0.4155 0.1445 0.225 Uiso 1 calc . .
C27 C 0.0911(10) 0.3212(10) 0.0647(13) 0.173(7) Uiso 1 d D .
H27A H 0.1315 0.2938 0.1238 0.207 Uiso 1 calc . .
H27B H 0.0470 0.2847 0.0245 0.207 Uiso 1 calc . .
C28 C 0.1249(13) 0.3508(13) 0.0133(15) 0.213(9) Uiso 1 d D .
H28A H 0.1447 0.3065 -0.0036 0.320 Uiso 1 calc . .
H28B H 0.1680 0.3871 0.0541 0.320 Uiso 1 calc . .
H28C H 0.0841 0.3781 -0.0445 0.320 Uiso 1 calc . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
O2 Ti1 O1 106.4(2) . .
O2 Ti1 Cl2 111.6(2) . .
O1 Ti1 Cl2 110.7(2) . .
O2 Ti1 Cl1 111.8(3) . .
O1 Ti1 Cl1 110.4(3) . .
Cl2 Ti1 Cl1 106.0(3) . .
O2 Si1 O1 106.4(2) . .
O2 Si1 C23 107.9(12) . .
O1 Si1 C23 108.2(12) . .
O2 Si1 C24 111.5(10) . .
O1 Si1 C24 99.0(9) . .
C23 Si1 C24 122.4(13) . .
Si1 C23 H23A 109.5(30) . .
Si1 C23 H23B 109.5(18) . .
H23A C23 H23B 109.5(34) . .
Si1 C23 H23C 109.5(27) . .
H23A C23 H23C 109.5(23) . .
H23B C23 H23C 109.5(38) . .
Si1 C24 H24A 109.5(22) . .
Si1 C24 H24B 109.5(29) . .
H24A C24 H24B 109.5(20) . .
Si1 C24 H24C 109.5(17) . .
H24A C24 H24C 109.5(37) . .
H24B C24 H24C 109.5(28) . .
C13 O1 Ti1 145.1(4) . .
C13 O1 Si1 145.1(4) . .
C14 O2 Ti1 142.8(4) . .
C14 O2 Si1 142.8(4) . .
C13 C1 C2 118.1(5) . .
C13 C1 C12 124.2(5) . 5
C2 C1 C12 117.4(5) . 5
C3 C2 C1 122.8(6) . .
C3 C2 H2 118.6(6) . .
C1 C2 H2 118.6(6) . .
C2 C3 C4 116.8(6) . .
C2 C3 C15 122.9(6) . .
C4 C3 C15 120.3(6) . .
C5 C4 C3 122.6(5) . .
C5 C4 H4 118.7(6) . .
C3 C4 H4 118.7(6) . .
C4 C5 C13 118.2(6) . .
C4 C5 C6 119.0(5) . .
C13 C5 C6 122.6(5) . .
C7 C6 C5 111.0(5) . .
C7 C6 H6A 109.4(5) . .
C5 C6 H6A 109.4(5) . .
C7 C6 H6B 109.4(5) . .
C5 C6 H6B 109.4(5) . .
H6A C6 H6B 108.0(5) . .
C8 C7 C14 118.6(5) . .
C8 C7 C6 119.7(5) . .
C14 C7 C6 121.5(5) . .
C7 C8 C9 123.1(5) . .
C7 C8 H8 118.5(6) . .
C9 C8 H8 118.5(6) . .
C8 C9 C10 116.5(5) . .
C8 C9 C19 121.1(5) . .
C10 C9 C19 122.4(5) . .
C11 C10 C9 122.9(5) . .
C11 C10 H10 118.6(6) . .
C9 C10 H10 118.6(6) . .
C10 C11 C14 118.4(5) . .
C10 C11 C12 118.4(5) . .
C14 C11 C12 123.0(5) . .
C1 C12 C11 120.6(5) 5 .
C1 C12 H12A 107.2(5) 5 .
C11 C12 H12A 107.2(5) . .
C1 C12 H12B 107.2(5) 5 .
C11 C12 H12B 107.2(5) . .
H12A C12 H12B 106.8(5) . .
O1 C13 C1 118.5(5) . .
O1 C13 C5 120.1(5) . .
C1 C13 C5 121.4(5) . .
O2 C14 C7 121.0(5) . .
O2 C14 C11 118.4(5) . .
C7 C14 C11 120.6(5) . .
C17B C15 C18B 111.6(19) . .
C16A C15 C18A 118.2(15) . .
C17B C15 C3 113.3(13) . .
C18B C15 C3 115.8(15) . .
C16A C15 C3 112.2(7) . .
C18A C15 C3 106.5(9) . .
C16A C15 C17A 105.1(9) . .
C18A C15 C17A 106.3(13) . .
C3 C15 C17A 108.0(8) . .
C17B C15 C16B 109.7(16) . .
C18B C15 C16B 93.4(29) . .
C3 C15 C16B 111.3(10) . .
C15 C16A H16A 109.5(5) . .
C15 C16A H16B 109.5(7) . .
H16A C16A H16B 109.5 . .
C15 C16A H16C 109.5(7) . .
H16A C16A H16C 109.5 . .
H16B C16A H16C 109.5 . .
C15 C17A H17A 109.5(7) . .
C15 C17A H17B 109.5(8) . .
H17A C17A H17B 109.5 . .
C15 C17A H17C 109.5(7) . .
H17A C17A H17C 109.5 . .
H17B C17A H17C 109.5 . .
C15 C18A H18A 109.5(13) . .
C15 C18A H18B 109.5(11) . .
H18A C18A H18B 109.5 . .
C15 C18A H18C 109.5(7) . .
H18A C18A H18C 109.5 . .
H18B C18A H18C 109.5 . .
C15 C16B H16D 109.5(12) . .
C15 C16B H16E 109.5(11) . .
H16D C16B H16E 109.5 . .
C15 C16B H16F 109.5(9) . .
H16D C16B H16F 109.5 . .
H16E C16B H16F 109.5 . .
C15 C17B H17D 109.5(15) . .
C15 C17B H17E 109.5(15) . .
H17D C17B H17E 109.47(7) . .
C15 C17B H17F 109.5(12) . .
H17D C17B H17F 109.5 . .
H17E C17B H17F 109.47(7) . .
C15 C18B H18D 109.5(14) . .
C15 C18B H18E 109.5(19) . .
H18D C18B H18E 109.5 . .
C15 C18B H18F 109.5(25) . .
H18D C18B H18F 109.5 . .
H18E C18B H18F 109.47(6) . .
C22A C19 C21A 110.4(9) . .
C22B C19 C20B 120.3(22) . .
C22A C19 C9 114.6(6) . .
C22B C19 C9 116.2(13) . .
C21A C19 C9 109.3(6) . .
C20B C19 C9 108.5(14) . .
C22A C19 C20A 107.7(9) . .
C21A C19 C20A 104.8(8) . .
C9 C19 C20A 109.7(6) . .
C22B C19 C21B 103.7(22) . .
C20B C19 C21B 100.2(22) . .
C9 C19 C21B 105.3(13) . .
C19 C20A H20A 109.5(6) . .
C19 C20A H20B 109.5(5) . .
H20A C20A H20B 109.5 . .
C19 C20A H20C 109.5(5) . .
H20A C20A H20C 109.5 . .
H20B C20A H20C 109.5 . .
C19 C21A H21A 109.5(6) . .
C19 C21A H21B 109.5(5) . .
H21A C21A H21B 109.5 . .
C19 C21A H21C 109.5(5) . .
H21A C21A H21C 109.5 . .
H21B C21A H21C 109.5 . .
C19 C22A H22A 109.5(7) . .
C19 C22A H22B 109.5(7) . .
H22A C22A H22B 109.5 . .
C19 C22A H22C 109.5(5) . .
H22A C22A H22C 109.5 . .
H22B C22A H22C 109.5 . .
C19 C20B H20D 109.5(15) . .
C19 C20B H20E 109.5(18) . .
H20D C20B H20E 109.5 . .
C19 C20B H20F 109.5(14) . .
H20D C20B H20F 109.5 . .
H20E C20B H20F 109.47(5) . .
C19 C21B H21D 109.5(13) . .
C19 C21B H21E 109.5(12) . .
H21D C21B H21E 109.5 . .
C19 C21B H21F 109.5(14) . .
H21D C21B H21F 109.47(7) . .
H21E C21B H21F 109.5 . .
C19 C22B H22D 109.5(18) . .
C19 C22B H22E 109.5(16) . .
H22D C22B H22E 109.5 . .
C19 C22B H22F 109.5(13) . .
H22D C22B H22F 109.5 . .
H22E C22B H22F 109.47(5) . .
C25 C25 C26 170.6(49) 5_565 .
C25 C25 H25A 92.9(34) 5_565 .
C26 C25 H25A 92.9(23) . .
C25 C25 H25B 92.9(33) 5_565 .
C26 C25 H25B 92.9(23) . .
H25A C25 H25B 103.0(37) . .
C25 C26 C27 129.1(24) . .
C25 C26 H26A 105.0(23) . .
C27 C26 H26A 105.0(16) . .
C25 C26 H26B 105.0(23) . .
C27 C26 H26B 105.0(17) . .
H26A C26 H26B 105.9(18) . .
C28 C27 C26 104.1(16) . .
C28 C27 H27A 110.9(17) . .
C26 C27 H27A 110.9(17) . .
C28 C27 H27B 110.9(17) . .
C26 C27 H27B 110.9(17) . .
H27A C27 H27B 109.0(17) . .
C27 C28 H28A 109.5(18) . .
C27 C28 H28B 109.5(18) . .
H28A C28 H28B 109.5(20) . .
C27 C28 H28C 109.5(18) . .
H28A C28 H28C 109.5(20) . .
H28B C28 H28C 109.5(20) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O2 1.706(4) .
Ti1 O1 1.713(4) .
Ti1 Cl2 2.198(5) .
Ti1 Cl1 2.243(6) .
Si1 O2 1.706(4) .
Si1 O1 1.713(4) .
Si1 C23 1.74(3) .
Si1 C24 1.89(3) .
C23 H23A 0.98(3) .
C23 H23B 0.98(4) .
C23 H23C 0.98(3) .
C24 H24A 0.98(3) .
C24 H24B 0.98(2) .
C24 H24C 0.98(3) .
O1 C13 1.374(7) .
O2 C14 1.371(6) .
C1 C13 1.383(8) .
C1 C2 1.395(8) .
C1 C12 1.514(8) 5
C2 C3 1.384(9) .
C2 H2 0.950(6) .
C3 C4 1.394(9) .
C3 C15 1.532(9) .
C4 C5 1.387(8) .
C4 H4 0.950(6) .
C5 C13 1.394(8) .
C5 C6 1.511(8) .
C6 C7 1.507(8) .
C6 H6A 0.990(6) .
C6 H6B 0.990(6) .
C7 C8 1.380(8) .
C7 C14 1.396(8) .
C8 C9 1.385(8) .
C8 H8 0.950(5) .
C9 C10 1.400(8) .
C9 C19 1.530(8) .
C10 C11 1.381(8) .
C10 H10 0.950(6) .
C11 C14 1.397(7) .
C11 C12 1.528(8) .
C12 C1 1.514(8) 5
C12 H12A 0.990(6) .
C12 H12B 0.990(6) .
C15 C17B 1.47(2) .
C15 C18B 1.49(3) .
C15 C16A 1.52(2) .
C15 C18A 1.53(2) .
C15 C17A 1.54(2) .
C15 C16B 1.55(2) .
C16A H16A 0.98 .
C16A H16B 0.98 .
C16A H16C 0.98 .
C17A H17A 0.98 .
C17A H17B 0.98 .
C17A H17C 0.98 .
C18A H18A 0.98 .
C18A H18B 0.98 .
C18A H18C 0.98 .
C16B H16D 0.98 .
C16B H16E 0.98 .
C16B H16F 0.98 .
C17B H17D 0.98 .
C17B H17E 0.98 .
C17B H17F 0.98 .
C18B H18D 0.98 .
C18B H18E 0.98 .
C18B H18F 0.98 .
C19 C22A 1.503(12) .
C19 C22B 1.51(3) .
C19 C21A 1.518(13) .
C19 C20B 1.53(3) .
C19 C20A 1.543(13) .
C19 C21B 1.58(3) .
C20A H20A 0.98 .
C20A H20B 0.98 .
C20A H20C 0.98 .
C21A H21A 0.98 .
C21A H21B 0.98 .
C21A H21C 0.98 .
C22A H22A 0.98 .
C22A H22B 0.98 .
C22A H22C 0.98 .
C20B H20D 0.98 .
C20B H20E 0.98 .
C20B H20F 0.98 .
C21B H21D 0.98 .
C21B H21E 0.98 .
C21B H21F 0.98 .
C22B H22D 0.98 .
C22B H22E 0.98 .
C22B H22F 0.98 .
C25 C25 1.47(4) 5_565
C25 C26 1.498(5) .
C25 H25A 0.99(4) .
C25 H25B 0.99(4) .
C26 C27 1.500(5) .
C26 H26A 0.99(2) .
C26 H26B 0.99(2) .
C27 C28 1.495(5) .
C27 H27A 0.99(2) .
C27 H27B 0.99(2) .
C28 H28A 0.98(2) .
C28 H28B 0.98(2) .
C28 H28C 0.98(2) .
