#------------------------------------------------------------------------------
#$Date: 2021-11-23 10:34:50 +0200 (Tue, 23 Nov 2021) $
#$Revision: 270822 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/19/4101994.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_4101994
loop_
_publ_author_name
'Jason B. Benedict'
'Philip Coppens'
_publ_section_title
;
 The Crystalline Nanocluster Phase as a Medium for Structural and
 Spectroscopic Studies of Light Absorption of Photosensitizer Dyes on
 Semiconductor Surfaces
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2938
_journal_page_last               2944
_journal_paper_doi               10.1021/ja909600w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C36 H28 O12 Ti2, 2/3(C6 H6)'
_chemical_formula_sum            'C40 H32 O12 Ti2'
_chemical_formula_weight         800.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   23.498(8)
_cell_length_b                   23.498(8)
_cell_length_c                   17.407(4)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     8324(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3708
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0553P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                2693
_reflns_number_total             3967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909600w_si_002.cif
_cod_data_source_block           'data_0m'
_cod_depositor_comments
;

2021-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C120 H96 O36 Ti6'
_cod_original_formula_weight         2401.37
_cod_original_formula_moiety         '3(C36 H28 O12 Ti2), 2(C6 H6)'
_cod_original_formula_units_Z            3
_cod_original_cell_volume        8323(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4101994
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_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
C1 C 0.44617(14) 0.02428(14) 0.69273(14) 0.0352(6) Uani 1 1 d . . .
C2 C 0.39505(15) 0.02081(17) 0.73305(17) 0.0486(8) Uani 1 1 d . . .
H2 H 0.3510 -0.0066 0.7166 0.058 Uiso 1 1 calc R . .
C3 C 0.40939(16) 0.05905(17) 0.79978(18) 0.0530(9) Uani 1 1 d . . .
H3 H 0.3747 0.0577 0.8292 0.064 Uiso 1 1 calc R . .
C4 C 0.47358(15) 0.09857(15) 0.82286(17) 0.0461(8) Uani 1 1 d . . .
H4 H 0.4826 0.1245 0.8680 0.055 Uiso 1 1 calc R . .
C5 C 0.52501(14) 0.10116(14) 0.78144(15) 0.0375(6) Uani 1 1 d . . .
H5 H 0.5692 0.1282 0.7978 0.045 Uiso 1 1 calc R . .
C6 C 0.51072(13) 0.06356(13) 0.71592(15) 0.0333(6) Uani 1 1 d . . .
C7 C 0.68079(14) 0.10091(14) 0.55587(15) 0.0358(6) Uani 1 1 d . . .
C8 C 0.71221(15) 0.13000(16) 0.62329(16) 0.0451(8) Uani 1 1 d . . .
H8 H 0.6922 0.1111 0.6711 0.054 Uiso 1 1 calc R . .
C9 C 0.77265(16) 0.18641(18) 0.62179(18) 0.0535(9) Uani 1 1 d . . .
H9 H 0.7942 0.2070 0.6684 0.064 Uiso 1 1 calc R . .
C10 C 0.80180(15) 0.21296(16) 0.55167(18) 0.0475(8) Uani 1 1 d . . .
H10 H 0.8435 0.2520 0.5502 0.057 Uiso 1 1 calc R . .
C11 C 0.77083(15) 0.18320(14) 0.48417(16) 0.0387(7) Uani 1 1 d . . .
H11 H 0.7915 0.2016 0.4365 0.046 Uiso 1 1 calc R . .
C12 C 0.71038(14) 0.12718(14) 0.48504(15) 0.0341(6) Uani 1 1 d . . .
C13 C 0.53665(13) 0.12154(14) 0.48463(15) 0.0343(6) Uani 1 1 d . . .
C14 C 0.57173(14) 0.17383(14) 0.53211(17) 0.0409(7) Uani 1 1 d . . .
H14 H 0.5864 0.1682 0.5808 0.049 Uiso 1 1 calc R . .
C15 C 0.58535(15) 0.23544(15) 0.50748(19) 0.0474(8) Uani 1 1 d . . .
H15 H 0.6091 0.2725 0.5399 0.057 Uiso 1 1 calc R . .
C16 C 0.56452(14) 0.24354(15) 0.43566(19) 0.0459(8) Uani 1 1 d . . .
H16 H 0.5748 0.2862 0.4193 0.055 Uiso 1 1 calc R . .
C17 C 0.52918(14) 0.19070(15) 0.38780(16) 0.0392(7) Uani 1 1 d . . .
H17 H 0.5152 0.1965 0.3387 0.047 Uiso 1 1 calc R . .
C18 C 0.51448(13) 0.12887(14) 0.41282(15) 0.0341(6) Uani 1 1 d . . .
C19 C 0.6622(2) 0.2729(2) 0.7136(2) 0.0723(11) Uani 1 1 d . . .
H19 H 0.6589 0.2310 0.7124 0.087 Uiso 1 1 calc R . .
C20 C 0.6063(2) 0.2780(2) 0.7145(2) 0.0728(11) Uani 1 1 d . . .
H20 H 0.5643 0.2393 0.7157 0.087 Uiso 1 1 calc R . .
O1 O 0.44148(10) -0.01105(10) 0.62622(10) 0.0388(5) Uani 1 1 d . . .
H1 H 0.4017 -0.0356 0.6148 0.058 Uiso 1 1 calc R . .
O2 O 0.55668(9) 0.06212(9) 0.67010(10) 0.0372(5) Uani 1 1 d . . .
O3 O 0.62080(10) 0.04475(10) 0.55558(10) 0.0405(5) Uani 1 1 d . . .
O4 O 0.67761(10) 0.09402(10) 0.41995(10) 0.0432(5) Uani 1 1 d . . .
H4A H 0.7000 0.1137 0.3811 0.065 Uiso 1 1 calc R . .
O5 O 0.51716(10) 0.05717(9) 0.50079(10) 0.0363(5) Uani 1 1 d . . .
O6 O 0.47827(9) 0.07194(10) 0.37265(10) 0.0371(5) Uani 1 1 d . . .
Ti1 Ti 0.53661(3) 0.00973(3) 0.58300(3) 0.03477(17) Uani 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C2 C1 C6 122.1(3) . . ?
C2 C1 O1 126.0(3) . . ?
C6 C1 O1 111.9(2) . . ?
C1 C2 C3 117.9(3) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 121.1(3) . . ?
C6 C5 C4 118.4(3) . . ?
O2 C6 C5 124.1(3) . . ?
O2 C6 C1 115.6(2) . . ?
C5 C6 C1 120.2(2) . . ?
O3 C7 C8 121.5(3) . . ?
O3 C7 C12 117.9(2) . . ?
C8 C7 C12 120.6(3) . . ?
C7 C8 C9 120.2(3) . . ?
C8 C9 C10 119.4(3) . . ?
C11 C10 C9 120.5(3) . . ?
C12 C11 C10 120.6(3) . . ?
C11 C12 O4 123.6(2) . . ?
C11 C12 C7 118.8(3) . . ?
O4 C12 C7 117.6(2) . . ?
C14 C13 O5 126.0(2) . . ?
C14 C13 C18 121.7(3) . . ?
O5 C13 C18 112.3(2) . . ?
C13 C14 C15 118.3(3) . . ?
C14 C15 C16 120.6(3) . . ?
C17 C16 C15 121.1(3) . . ?
C16 C17 C18 118.5(3) . . ?
O6 C18 C17 125.0(3) . . ?
O6 C18 C13 115.2(2) . . ?
C17 C18 C13 119.9(3) . . ?
C20 C19 C20 119.5(5) 2_655 . ?
C19 C20 C19 120.4(5) 3_665 . ?
C6 O2 Ti1 123.67(17) . . ?
C7 O3 Ti1 144.46(18) . . ?
C13 O5 Ti1 135.78(17) . . ?
C13 O5 Ti1 115.92(16) . 10_656 ?
Ti1 O5 Ti1 107.83(9) . 10_656 ?
C18 O6 Ti1 118.91(16) . 10_656 ?
O3 Ti1 O2 93.27(9) . . ?
O3 Ti1 O6 99.96(9) . 10_656 ?
O2 Ti1 O6 101.06(8) . 10_656 ?
O3 Ti1 O5 93.50(8) . . ?
O2 Ti1 O5 105.50(8) . . ?
O6 Ti1 O5 149.38(9) 10_656 . ?
O3 Ti1 O5 106.19(8) . 10_656 ?
O2 Ti1 O5 160.46(8) . 10_656 ?
O6 Ti1 O5 77.68(8) 10_656 10_656 ?
O5 Ti1 O5 72.17(9) . 10_656 ?
O3 Ti1 Ti1 102.24(6) . 10_656 ?
O2 Ti1 Ti1 138.90(6) . 10_656 ?
O6 Ti1 Ti1 113.10(6) 10_656 10_656 ?
O5 Ti1 Ti1 36.60(5) . 10_656 ?
O5 Ti1 Ti1 35.58(5) 10_656 10_656 ?
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 1.358(4) . ?
C1 C6 1.384(4) . ?
C1 O1 1.396(3) . ?
C2 C3 1.403(4) . ?
C3 C4 1.378(4) . ?
C4 C5 1.382(4) . ?
C5 C6 1.377(4) . ?
C6 O2 1.357(3) . ?
C7 O3 1.367(3) . ?
C7 C8 1.373(4) . ?
C7 C12 1.398(4) . ?
C8 C9 1.376(5) . ?
C9 C10 1.386(4) . ?
C10 C11 1.375(4) . ?
C11 C12 1.371(4) . ?
C12 O4 1.372(3) . ?
C13 C14 1.363(4) . ?
C13 O5 1.373(3) . ?
C13 C18 1.398(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.376(4) . ?
C17 C18 1.385(4) . ?
C18 O6 1.365(3) . ?
C19 C20 1.357(5) 2_655 ?
C19 C20 1.378(5) . ?
C20 C19 1.357(5) 3_665 ?
O2 Ti1 1.8589(19) . ?
O3 Ti1 1.786(2) . ?
O5 Ti1 2.0020(18) . ?
O5 Ti1 2.0515(19) 10_656 ?
O6 Ti1 1.931(2) 10_656 ?
Ti1 O6 1.931(2) 10_656 ?
Ti1 O5 2.0515(19) 10_656 ?
Ti1 Ti1 3.2758(11) 10_656 ?
