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#$Date: 2025-08-23 02:36:08 +0300 (Sat, 23 Aug 2025) $
#$Revision: 301880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/00/8000086.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_8000086
loop_
_publ_author_name
'Hirotsu, Masakazu'
'Taruno, Shinsuke'
'Yoshimura, Takashi'
'Ueno, Keiji'
'Unno, Masafumi'
'Matsumoto, Hideyuki'
_publ_section_title
;
 Synthesis and Structures of the First Titanium(IV) Complexes with Cyclic
 Tetrasiloxide Ligands: Incomplete and Complete Cage Titanosiloxanes
;
_journal_issue                   11
_journal_name_full               'Chemistry Letters'
_journal_page_first              1542
_journal_paper_doi               10.1246/cl.2005.1542
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C31 H39 O10.5 Si5 Ti'
_chemical_formula_weight         767.97
_space_group_IT_number           18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4561(9)
_cell_length_b                   18.1710(9)
_cell_length_c                   14.1250(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3710.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20382
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.445
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1604
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0755P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                9347
_reflns_number_total             10318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            34-1542sup1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C31 H39 O10.50 Si5 Ti'
_cod_database_code               8000086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
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
Ti1 Ti 0.55839(3) 0.92703(2) 0.69930(3) 0.01321(8) Uani 1 1 d .
Si1 Si 0.39963(4) 0.81032(3) 0.76243(5) 0.01426(12) Uani 1 1 d .
Si2 Si 0.30927(4) 0.90385(3) 0.92515(5) 0.01504(12) Uani 1 1 d .
Si3 Si 0.24178(4) 1.01351(3) 0.77157(5) 0.01467(12) Uani 1 1 d .
Si4 Si 0.33327(4) 0.92069(3) 0.62771(5) 0.01411(12) Uani 1 1 d .
Si5 Si 0.65323(5) 0.83449(4) 0.51436(5) 0.02050(14) Uani 1 1 d .
O1 O 0.50225(11) 0.84635(9) 0.75689(12) 0.0170(3) Uani 1 1 d .
O2 O 0.40217(12) 0.94635(9) 0.96238(13) 0.0188(3) Uani 1 1 d .
O3 O 0.33204(10) 1.06695(9) 0.76736(12) 0.0172(3) Uani 1 1 d .
O4 O 0.42750(11) 0.96361(8) 0.65890(12) 0.0143(3) Uani 1 1 d .
O5 O 0.59707(12) 0.88831(9) 0.59042(13) 0.0204(3) Uani 1 1 d .
O6 O 0.34709(12) 0.83842(9) 0.85751(13) 0.0201(3) Uani 1 1 d .
O7 O 0.24607(11) 0.96158(9) 0.86594(13) 0.0195(3) Uani 1 1 d .
O8 O 0.24440(11) 0.96134(9) 0.67705(12) 0.0175(3) Uani 1 1 d .
O9 O 0.34114(11) 0.83702(9) 0.66969(12) 0.0173(3) Uani 1 1 d .
O10 O 0.5000 1.0000 0.81981(17) 0.0136(4) Uani 1 2 d S
C31 C 0.13160(16) 1.06493(13) 0.7778(2) 0.0223(5) Uani 1 1 d .
C32 C 0.1035(2) 1.09567(18) 0.8641(3) 0.0376(7) Uani 1 1 d .
H32 H 0.1408 1.0906 0.9173 0.045 Uiso 1 1 calc R
C33 C 0.0198(3) 1.1339(2) 0.8709(4) 0.0559(11) Uani 1 1 d .
H33 H 0.0024 1.1549 0.9283 0.067 Uiso 1 1 calc R
C34 C -0.0371(2) 1.14053(18) 0.7933(4) 0.0605(14) Uani 1 1 d .
H34 H -0.0933 1.1650 0.7986 0.073 Uiso 1 1 calc R
C35 C -0.0108(2) 1.11118(18) 0.7085(4) 0.0546(12) Uani 1 1 d .
H35 H -0.0494 1.1159 0.6562 0.066 Uiso 1 1 calc R
C36 C 0.0747(2) 1.07366(16) 0.6993(3) 0.0369(7) Uani 1 1 d .
H36 H 0.0926 1.0549 0.6409 0.044 Uiso 1 1 calc R
C21 C 0.24371(16) 0.86147(12) 1.02333(17) 0.0168(4) Uani 1 1 d .
C22 C 0.15727(16) 0.88759(13) 1.05315(18) 0.0190(4) Uani 1 1 d .
H22 H 0.1313 0.9285 1.0237 0.023 Uiso 1 1 calc R
C23 C 0.10975(17) 0.85283(14) 1.1266(2) 0.0230(5) Uani 1 1 d .
H23 H 0.0527 0.8710 1.1462 0.028 Uiso 1 1 calc R
C24 C 0.14707(18) 0.79142(14) 1.17037(19) 0.0228(5) Uani 1 1 d .
H24 H 0.1145 0.7678 1.2183 0.027 Uiso 1 1 calc R
C25 C 0.23373(18) 0.76496(14) 1.14248(18) 0.0224(5) Uani 1 1 d .
H25 H 0.2594 0.7241 1.1722 0.027 Uiso 1 1 calc R
C26 C 0.28114(17) 0.80021(13) 1.07000(18) 0.0198(5) Uani 1 1 d .
H26 H 0.3390 0.7828 1.0520 0.024 Uiso 1 1 calc R
C11 C 0.39764(15) 0.70803(13) 0.76634(18) 0.0171(4) Uani 1 1 d .
C12 C 0.42876(19) 0.66602(13) 0.6901(2) 0.0244(5) Uani 1 1 d .
H12 H 0.4524 0.6895 0.6369 0.029 Uiso 1 1 calc R
C13 C 0.4249(2) 0.58903(14) 0.6926(2) 0.0307(6) Uani 1 1 d .
H13 H 0.4464 0.5616 0.6416 0.037 Uiso 1 1 calc R
C14 C 0.38895(19) 0.55395(14) 0.7711(2) 0.0306(6) Uani 1 1 d .
H14 H 0.3874 0.5028 0.7732 0.037 Uiso 1 1 calc R
C15 C 0.3554(2) 0.59420(14) 0.8464(2) 0.0312(6) Uani 1 1 d .
H15 H 0.3293 0.5703 0.8981 0.037 Uiso 1 1 calc R
C16 C 0.36054(19) 0.67058(14) 0.8448(2) 0.0260(5) Uani 1 1 d .
H16 H 0.3391 0.6974 0.8965 0.031 Uiso 1 1 calc R
C41 C 0.31771(16) 0.91850(12) 0.49845(17) 0.0182(4) Uani 1 1 d .
C42 C 0.39470(18) 0.92150(15) 0.43781(18) 0.0243(5) Uani 1 1 d .
H42 H 0.4537 0.9263 0.4633 0.029 Uiso 1 1 calc R
C43 C 0.3837(2) 0.91737(16) 0.3398(2) 0.0308(6) Uani 1 1 d .
H43 H 0.4352 0.9186 0.3003 0.037 Uiso 1 1 calc R
C44 C 0.2945(2) 0.91129(15) 0.3011(2) 0.0295(6) Uani 1 1 d .
H44 H 0.2866 0.9099 0.2357 0.035 Uiso 1 1 calc R
C45 C 0.2193(2) 0.90743(15) 0.3594(2) 0.0282(6) Uani 1 1 d .
H45 H 0.1606 0.9020 0.3335 0.034 Uiso 1 1 calc R
C46 C 0.22984(18) 0.91148(13) 0.45734(19) 0.0228(5) Uani 1 1 d .
H46 H 0.1778 0.9095 0.4960 0.027 Uiso 1 1 calc R
C51 C 0.6793(3) 0.88821(18) 0.4065(2) 0.0420(8) Uani 1 1 d .
H51A H 0.7200 0.9281 0.4223 0.063 Uiso 1 1 calc R
H51B H 0.6229 0.9075 0.3807 0.063 Uiso 1 1 calc R
H51C H 0.7085 0.8569 0.3607 0.063 Uiso 1 1 calc R
C52 C 0.7604(2) 0.79929(19) 0.5715(3) 0.0456(9) Uani 1 1 d .
H52A H 0.7444 0.7720 0.6273 0.068 Uiso 1 1 calc R
H52B H 0.7994 0.8399 0.5885 0.068 Uiso 1 1 calc R
H52C H 0.7927 0.7678 0.5281 0.068 Uiso 1 1 calc R
C53 C 0.5767(3) 0.75619(19) 0.4818(3) 0.0479(9) Uani 1 1 d .
H53A H 0.5210 0.7747 0.4537 0.072 Uiso 1 1 calc R
H53B H 0.5617 0.7284 0.5375 0.072 Uiso 1 1 calc R
H53C H 0.6081 0.7250 0.4373 0.072 Uiso 1 1 calc R
O11 O 0.36822(14) 1.06616(11) 1.05899(14) 0.0285(4) Uani 1 1 d .
C61 C 0.3624(2) 1.13125(15) 1.0000(2) 0.0277(6) Uani 1 1 d .
H61A H 0.2987 1.1473 0.9941 0.033 Uiso 1 1 calc R
H61B H 0.3865 1.1211 0.9372 0.033 Uiso 1 1 calc R
C62 C 0.4198(2) 1.18939(16) 1.0485(2) 0.0329(6) Uani 1 1 d .
H62A H 0.3942 1.2381 1.0381 0.039 Uiso 1 1 calc R
H62B H 0.4833 1.1884 1.0264 0.039 Uiso 1 1 calc R
C63 C 0.4136(3) 1.16757(17) 1.1525(2) 0.0414(8) Uani 1 1 d .
H63A H 0.4663 1.1858 1.1881 0.050 Uiso 1 1 calc R
H63B H 0.3570 1.1856 1.1813 0.050 Uiso 1 1 calc R
C64 C 0.4142(3) 1.08470(16) 1.1466(2) 0.0454(9) Uani 1 1 d .
H64A H 0.4772 1.0663 1.1465 0.054 Uiso 1 1 calc R
H64B H 0.3816 1.0635 1.2000 0.054 Uiso 1 1 calc R
H1 H 0.466(2) 0.9790(18) 0.866(3) 0.033(9) Uiso 1 1 d .
H2 H 0.397(3) 0.987(2) 1.006(3) 0.053(12) Uiso 1 1 d .
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'
Ti Ti 0.2776 0.4457 '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'
O O 0.0106 0.0060 '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
O5 Ti1 O3 101.68(8) . 2_675
O5 Ti1 O1 101.71(8) . .
O3 Ti1 O1 101.07(7) 2_675 .
O5 Ti1 O4 96.30(7) . 2_675
O3 Ti1 O4 90.12(7) 2_675 2_675
O1 Ti1 O4 156.29(7) . 2_675
O5 Ti1 O4 100.05(8) . .
O3 Ti1 O4 153.82(7) 2_675 .
O1 Ti1 O4 88.57(7) . .
O4 Ti1 O4 73.08(7) 2_675 .
O5 Ti1 O10 167.09(7) . .
O3 Ti1 O10 84.07(6) 2_675 .
O1 Ti1 O10 88.33(6) . .
O4 Ti1 O10 71.95(6) 2_675 .
O4 Ti1 O10 71.82(6) . .
O5 Ti1 Ti1 120.12(6) . 2_675
O3 Ti1 Ti1 114.11(5) 2_675 2_675
O1 Ti1 Ti1 115.47(5) . 2_675
O4 Ti1 Ti1 41.05(4) 2_675 2_675
O4 Ti1 Ti1 40.87(4) . 2_675
O10 Ti1 Ti1 47.28(4) . 2_675
O1 Si1 O6 109.89(9) . .
O1 Si1 O9 108.34(9) . .
O6 Si1 O9 109.13(9) . .
O1 Si1 C11 114.74(9) . .
O6 Si1 C11 106.40(10) . .
O9 Si1 C11 108.22(10) . .
O6 Si2 O7 111.11(10) . .
O6 Si2 O2 105.00(9) . .
O7 Si2 O2 108.82(9) . .
O6 Si2 C21 108.06(10) . .
O7 Si2 C21 111.55(10) . .
O2 Si2 C21 112.12(10) . .
O3 Si3 O7 110.11(9) . .
O3 Si3 O8 107.28(9) . .
O7 Si3 O8 109.26(9) . .
O3 Si3 C31 113.01(10) . .
O7 Si3 C31 106.61(11) . .
O8 Si3 C31 110.55(11) . .
O4 Si4 O9 106.77(8) . .
O4 Si4 O8 108.95(8) . .
O9 Si4 O8 108.63(9) . .
O4 Si4 C41 112.37(10) . .
O9 Si4 C41 110.36(10) . .
O8 Si4 C41 109.64(10) . .
O5 Si5 C51 108.73(12) . .
O5 Si5 C52 109.17(13) . .
C51 Si5 C52 111.67(19) . .
O5 Si5 C53 108.62(14) . .
C51 Si5 C53 108.75(19) . .
C52 Si5 C53 109.84(18) . .
Si1 O1 Ti1 137.44(10) . .
Si3 O3 Ti1 137.58(11) . 2_675
Si4 O4 Ti1 127.87(9) . 2_675
Si4 O4 Ti1 132.82(9) . .
Ti1 O4 Ti1 98.08(7) 2_675 .
Si5 O5 Ti1 160.49(12) . .
Si2 O6 Si1 151.12(12) . .
Si2 O7 Si3 144.57(12) . .
Si4 O8 Si3 128.76(10) . .
Si1 O9 Si4 127.08(10) . .
Ti1 O10 Ti1 85.44(8) 2_675 .
C36 C31 C32 118.4(3) . .
C36 C31 Si3 122.1(2) . .
C32 C31 Si3 119.5(2) . .
C33 C32 C31 120.6(4) . .
C34 C33 C32 120.4(4) . .
C35 C34 C33 119.9(3) . .
C34 C35 C36 120.7(4) . .
C31 C36 C35 119.9(4) . .
C22 C21 C26 118.1(2) . .
C22 C21 Si2 122.81(18) . .
C26 C21 Si2 119.06(18) . .
C23 C22 C21 120.6(2) . .
C24 C23 C22 120.3(2) . .
C23 C24 C25 120.0(2) . .
C26 C25 C24 119.4(2) . .
C25 C26 C21 121.5(2) . .
C12 C11 C16 117.8(2) . .
C12 C11 Si1 121.29(19) . .
C16 C11 Si1 120.83(19) . .
C11 C12 C13 121.0(3) . .
C14 C13 C12 119.8(3) . .
C15 C14 C13 120.5(2) . .
C14 C15 C16 119.9(3) . .
C15 C16 C11 121.1(3) . .
C46 C41 C42 117.9(2) . .
C46 C41 Si4 121.57(19) . .
C42 C41 Si4 120.46(18) . .
C43 C42 C41 120.8(2) . .
C42 C43 C44 119.6(3) . .
C45 C44 C43 120.0(3) . .
C44 C45 C46 120.6(3) . .
C45 C46 C41 121.0(3) . .
C64 O11 C61 109.2(2) . .
O11 C61 C62 106.2(2) . .
C61 C62 C63 102.9(2) . .
C64 C63 C62 101.9(3) . .
O11 C64 C63 106.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O5 1.7813(18) .
Ti1 O3 1.8561(17) 2_675
Ti1 O1 1.8628(17) .
Ti1 O4 2.0774(16) 2_675
Ti1 O4 2.0851(16) .
Ti1 O10 2.3169(18) .
Ti1 Ti1 3.1435(8) 2_675
Si1 O1 1.6234(17) .
Si1 O6 1.6251(19) .
Si1 O9 1.6328(18) .
Si1 C11 1.860(2) .
Si2 O6 1.6203(18) .
Si2 O7 1.6232(18) .
Si2 O2 1.6360(18) .
Si2 C21 1.848(2) .
Si3 O3 1.6276(17) .
Si3 O7 1.6343(19) .
Si3 O8 1.6378(18) .
Si3 C31 1.849(2) .
Si4 O4 1.6303(17) .
Si4 O9 1.6361(17) .
Si4 O8 1.6376(18) .
Si4 C41 1.840(3) .
Si5 O5 1.6643(19) .
Si5 C51 1.848(3) .
Si5 C52 1.860(3) .
Si5 C53 1.860(3) .
O3 Ti1 1.8561(17) 2_675
O4 Ti1 2.0774(16) 2_675
O10 Ti1 2.3169(18) 2_675
C31 C36 1.389(4) .
C31 C32 1.402(4) .
C32 C33 1.398(4) .
C33 C34 1.375(7) .
C34 C35 1.365(7) .
C35 C36 1.417(4) .
C21 C22 1.401(3) .
C21 C26 1.402(3) .
C22 C23 1.395(3) .
C23 C24 1.385(4) .
C24 C25 1.399(4) .
C25 C26 1.389(3) .
C11 C12 1.394(3) .
C11 C16 1.407(3) .
C12 C13 1.401(3) .
C13 C14 1.380(4) .
C14 C15 1.379(4) .
C15 C16 1.390(3) .
C41 C46 1.402(3) .
C41 C42 1.405(3) .
C42 C43 1.396(4) .
C43 C44 1.406(4) .
C44 C45 1.365(4) .
C45 C46 1.394(4) .
O11 C64 1.444(4) .
O11 C61 1.449(3) .
C61 C62 1.508(4) .
C62 C63 1.524(5) .
C63 C64 1.508(4) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139205841
