#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:40:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179983 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/77/7027716.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027716
loop_
_publ_author_name
'Crocker, Mark'
'Herold, Ruud H. M.'
'Orpen, A. Guy'
'Overgaag, Martijn T. A.'
_publ_section_title
;
 Synthesis and characterisation of titanium silasesquioxane complexes:
 soluble models for the active site in titanium silicate epoxidation
 catalysts †
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3791
_journal_paper_doi               10.1039/a905887g
_journal_year                    1999
_chemical_formula_sum            'C45 H86 O13 Si8 Ti'
_chemical_formula_weight         1107.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.955(4)
_cell_length_b                   16.955(4)
_cell_length_c                   17.853(6)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      7.5
_cell_volume                     4445(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       R3m
_diffrn_measurement_method       'wyckoff w scan'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1448
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  .936
_exptl_absorpt_correction_T_min  .828
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          .42
_exptl_crystal_size_mid          .42
_exptl_crystal_size_min          .42
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.397
_refine_ls_goodness_of_fit_obs   1.655
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1190
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.446
_refine_ls_restrained_S_obs      1.676
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_obs          0.1071
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3075
_refine_ls_wR_factor_obs         0.2692
_reflns_number_observed          775
_reflns_number_total             1296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905887gsup1.cif
_cod_data_source_block           tresetti
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] 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^)+(0.1000P)^2^+10.0000P] 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        4444.6(21)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7027716
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Si1 Si 0.0000 0.0000 0.3446(2) 0.137(2) Uani 0.50 d SP 1
Ti1 Ti 0.0000 0.0000 0.3446(2) 0.137(2) Uani 0.50 d SP 2
Si2 Si 0.1601(2) 0.0175(2) 0.44873(13) 0.1053(11) Uani 1 d . .
O1 O 0.0961(4) 0.0110(4) 0.3785(3) 0.120(2) Uani 1 d . .
O2 O 0.1037(4) -0.0754(4) 0.4991(3) 0.125(2) Uani 1 d . .
C1 C 0.2705(8) 0.0333(9) 0.4155(7) 0.163(4) Uani 1 d DU .
H1 H 0.3026(8) 0.0900(9) 0.3867(7) 0.195 Uiso 1 calc R .
C2 C 0.2617(12) -0.0443(11) 0.3692(9) 0.230(6) Uani 1 d DU .
H2A H 0.2363(12) -0.0995(11) 0.3990(9) 0.275 Uiso 1 calc R .
H2B H 0.2219(12) -0.0548(11) 0.3268(9) 0.275 Uiso 1 calc R .
C3 C 0.3527(17) -0.0191(28) 0.3437(14) 0.468(24) Uani 1 d DU .
H3A H 0.3500(17) -0.0585(28) 0.3031(14) 0.562 Uiso 1 calc R .
H3B H 0.3849(17) 0.0435(28) 0.3264(14) 0.562 Uiso 1 calc R .
C4 C 0.3964(19) -0.0301(23) 0.4066(17) 0.405(15) Uani 1 d DU .
H4A H 0.4510(19) -0.0311(23) 0.3923(17) 0.485 Uiso 1 calc R .
H4B H 0.3561(19) -0.0857(23) 0.4334(17) 0.485 Uiso 1 calc R .
C5 C 0.4183(11) 0.0498(19) 0.4515(15) 0.397(15) Uani 1 d DU .
H5A H 0.4493(11) 0.1044(19) 0.4212(15) 0.477 Uiso 1 calc R .
H5B H 0.4578(11) 0.0549(19) 0.4928(15) 0.477 Uiso 1 calc R .
C6 C 0.3268(11) 0.0379(14) 0.4818(9) 0.270(9) Uani 1 d DU .
H6A H 0.2951(11) -0.0176(14) 0.5111(9) 0.324 Uiso 1 calc R .
H6B H 0.3382(11) 0.0889(14) 0.5136(9) 0.324 Uiso 1 calc R .
C7 C 0.0000 0.0000 0.2413(8) 0.188(7) Uani 0.50 d SP 1
H7 H 0.0251 -0.0373 0.2227(8) 0.225 Uiso 0.17 calc PR 1
C8 C 0.0563(23) 0.0942(19) 0.2153(12) 0.143(11) Uani 0.33 d P 1
H8A H 0.1140(23) 0.1224(19) 0.2419(12) 0.171 Uiso 0.33 calc PR 1
H8B H 0.0258(23) 0.1282(19) 0.2270(12) 0.171 Uiso 0.33 calc PR 1
O3 O 0.0000 0.0000 0.2413(8) 0.188(7) Uani 0.50 d SP 2
Si4 Si 0.0000 0.0000 0.1409(11) 0.209(6) Uani 0.50 d SP 2
C9 C 0.0229(24) -0.0773(20) 0.1180(13) 0.280(12) Uani 0.50 d P 2
H9A H -0.0261(24) -0.1357(20) 0.1334(13) 0.336 Uiso 0.50 calc PR 2
H9B H 0.0782(24) -0.0659(20) 0.1423(13) 0.336 Uiso 0.50 calc PR 2
H9C H 0.0304(24) -0.0769(20) 0.0647(13) 0.336 Uiso 0.50 calc PR 2
C10 C 0.0229(24) -0.0773(20) 0.1180(13) 0.280(12) Uani 0.33 d P 1
H10A H 0.0522(48) -0.1099(61) 0.0990(33) 0.336 Uiso 0.33 calc PR 1
H10B H -0.0404(48) -0.1070(61) 0.1025(33) 0.336 Uiso 0.33 calc PR 1
C11 C 0.0725(48) 0.0188(61) 0.1014(33) 0.118(16) Uiso 0.17 d P 1
H11A H 0.1346(48) 0.0333(61) 0.1111(33) 0.141 Uiso 0.17 calc PR 1
H11B H 0.0680(48) 0.0181(61) 0.0472(33) 0.141 Uiso 0.17 calc PR 1
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'
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
O1 Si1 O1 107.4(2) 2 .
O1 Si1 O1 107.4(2) 2 3
O1 Si1 O1 107.4(2) . 3
O1 Si1 C7 111.4(2) 2 .
O1 Si1 C7 111.4(2) . .
O1 Si1 C7 111.4(2) 3 .
O1 Ti1 O1 107.4(2) 2 .
O1 Ti1 O1 107.4(2) 2 3
O1 Ti1 O1 107.4(2) . 3
O1 Ti1 O3 111.4(2) 2 .
O1 Ti1 O3 111.4(2) . .
O1 Ti1 O3 111.4(2) 3 .
O2 Si2 O1 109.1(3) 12_556 .
O2 Si2 O2 107.9(2) 12_556 .
O1 Si2 O2 108.0(3) . .
O2 Si2 C1 108.8(4) 12_556 .
O1 Si2 C1 110.8(4) . .
O2 Si2 C1 112.1(5) . .
Si2 O1 Si1 151.0(4) . .
Si2 O1 Ti1 151.0(4) . .
Si2 O2 Si2 151.0(4) 11_556 .
C2 C1 C6 105.2(10) . .
C2 C1 Si2 113.6(10) . .
C6 C1 Si2 109.0(9) . .
C3 C2 C1 106.9(16) . .
C4 C3 C2 105.2(24) . .
C3 C4 C5 102.9(23) . .
C4 C5 C6 107.3(17) . .
C1 C6 C5 107.4(13) . .
C8 C7 C8 110.5(11) 2 .
C8 C7 Si1 108.4(11) 2 .
C8 C7 Si1 108.4(11) . .
C7 C8 C10 112.1(21) . 2
Si4 O3 Ti1 180.0 . .
C9 Si4 C9 113.7(9) 2 3
C9 Si4 C9 113.7(9) 2 .
C9 Si4 C9 113.7(9) 3 .
C9 Si4 O3 104.8(11) 2 .
C9 Si4 O3 104.8(11) 3 .
C9 Si4 O3 104.8(11) . .
C11 C10 C8 91.8(30) . 3
C10 C11 C10 143.0(54) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.658(6) 2
Si1 O1 1.658(6) .
Si1 O1 1.658(6) 3
Si1 C7 1.84(2) .
Ti1 O1 1.658(6) 2
Ti1 O1 1.658(6) .
Ti1 O1 1.658(6) 3
Ti1 O3 1.84(2) .
Si2 O2 1.625(6) 12_556
Si2 O1 1.625(6) .
Si2 O2 1.641(6) .
Si2 C1 1.851(11) .
O2 Si2 1.624(6) 11_556
C1 C2 1.496(15) .
C1 C6 1.50(2) .
C2 C3 1.45(2) .
C3 C4 1.41(3) .
C4 C5 1.45(3) .
C5 C6 1.56(2) .
C7 C8 1.47(3) 2
C7 C8 1.47(3) .
C8 C10 1.77(3) 2
O3 Si4 1.79(2) .
Si4 C9 1.60(2) 2
Si4 C9 1.60(2) 3
Si4 C9 1.60(2) .
C10 C11 1.44(8) .
C10 C8 1.77(3) 3
C11 C10 1.37(7) 2
