#------------------------------------------------------------------------------
#$Date: 2018-09-27 07:13:35 +0300 (Thu, 27 Sep 2018) $
#$Revision: 211196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/19/4101993.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_4101993
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         'C30 H52 O10 Ti2'
_chemical_formula_sum            'C30 H52 O10 Ti2'
_chemical_formula_weight         668.52
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.0440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1420(7)
_cell_length_b                   13.4738(6)
_cell_length_c                   19.9129(9)
_cell_measurement_reflns_used    348
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      1.59
_cell_volume                     3437.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61749
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         10525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+1.2448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                8356
_reflns_number_total             10525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909600w_si_001.cif
_cod_data_source_block           'data_0m'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4101993
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
C1 C 0.50468(9) 0.28887(9) 0.62433(6) 0.0173(2) Uani 1 1 d . . .
C2 C 0.40586(10) 0.28994(10) 0.56560(7) 0.0225(3) Uani 1 1 d . . .
H2 H 0.3539 0.3344 0.5658 0.027 Uiso 1 1 calc R . .
C3 C 0.38412(10) 0.22475(11) 0.50633(7) 0.0272(3) Uani 1 1 d . . .
H3 H 0.3167 0.2247 0.4662 0.033 Uiso 1 1 calc R . .
C4 C 0.45964(11) 0.16015(11) 0.50529(7) 0.0277(3) Uani 1 1 d . . .
H4 H 0.4432 0.1157 0.4649 0.033 Uiso 1 1 calc R . .
C5 C 0.56011(10) 0.15979(10) 0.56341(7) 0.0217(2) Uani 1 1 d . . .
H5 H 0.6125 0.1165 0.5624 0.026 Uiso 1 1 calc R . .
C6 C 0.58103(9) 0.22380(9) 0.62206(6) 0.0160(2) Uani 1 1 d . . .
C7 C 0.89952(8) 0.27308(8) 0.86693(6) 0.0137(2) Uani 1 1 d . . .
C8 C 0.91437(9) 0.32749(9) 0.92947(6) 0.0168(2) Uani 1 1 d . . .
H8 H 0.8632 0.3736 0.9289 0.020 Uiso 1 1 calc R . .
C9 C 1.00649(10) 0.31318(10) 0.99365(7) 0.0199(2) Uani 1 1 d . . .
H9 H 1.0182 0.3500 1.0371 0.024 Uiso 1 1 calc R . .
C10 C 1.08082(10) 0.24554(10) 0.99420(7) 0.0205(2) Uani 1 1 d . . .
H10 H 1.1429 0.2364 1.0382 0.025 Uiso 1 1 calc R . .
C11 C 1.06541(9) 0.19072(9) 0.93086(7) 0.0184(2) Uani 1 1 d . . .
H11 H 1.1167 0.1446 0.9316 0.022 Uiso 1 1 calc R . .
C12 C 0.97434(9) 0.20438(9) 0.86677(6) 0.0149(2) Uani 1 1 d . . .
C13 C 0.68432(10) 0.51531(9) 0.66368(7) 0.0215(2) Uani 1 1 d . . .
H13 H 0.6309 0.5407 0.6800 0.026 Uiso 1 1 calc R . .
C14 C 0.62936(12) 0.49125(12) 0.58219(8) 0.0336(3) Uani 1 1 d . . .
H14A H 0.6803 0.4673 0.5646 0.050 Uiso 1 1 calc R . .
H14B H 0.5952 0.5511 0.5546 0.050 Uiso 1 1 calc R . .
H14C H 0.5769 0.4397 0.5744 0.050 Uiso 1 1 calc R . .
C15 C 0.76671(11) 0.59518(10) 0.67976(8) 0.0280(3) Uani 1 1 d . . .
H15A H 0.8014 0.6072 0.7333 0.042 Uiso 1 1 calc R . .
H15B H 0.7336 0.6566 0.6543 0.042 Uiso 1 1 calc R . .
H15C H 0.8183 0.5733 0.6621 0.042 Uiso 1 1 calc R . .
C16 C 0.64433(10) 0.51035(10) 0.85427(7) 0.0235(3) Uani 1 1 d . . .
H16 H 0.6505 0.4940 0.9049 0.028 Uiso 1 1 calc R . .
C17 C 0.72442(12) 0.58868(11) 0.86144(9) 0.0330(3) Uani 1 1 d . . .
H17A H 0.7946 0.5624 0.8908 0.049 Uiso 1 1 calc R . .
H17B H 0.7129 0.6473 0.8861 0.049 Uiso 1 1 calc R . .
H17C H 0.7178 0.6072 0.8120 0.049 Uiso 1 1 calc R . .
C18 C 0.53369(11) 0.54357(11) 0.80705(9) 0.0323(3) Uani 1 1 d . . .
H18A H 0.5237 0.5510 0.7555 0.048 Uiso 1 1 calc R . .
H18B H 0.5209 0.6073 0.8254 0.048 Uiso 1 1 calc R . .
H18C H 0.4847 0.4939 0.8096 0.048 Uiso 1 1 calc R . .
C19 C 0.59558(10) 0.20066(10) 0.86341(7) 0.0217(2) Uani 1 1 d . . .
H19 H 0.5877 0.1273 0.8670 0.026 Uiso 1 1 calc R . .
C20 C 0.48814(10) 0.24682(11) 0.83717(8) 0.0273(3) Uani 1 1 d . . .
H20A H 0.4940 0.3192 0.8359 0.041 Uiso 1 1 calc R . .
H20B H 0.4574 0.2287 0.8713 0.041 Uiso 1 1 calc R . .
H20C H 0.4435 0.2224 0.7874 0.041 Uiso 1 1 calc R . .
C21 C 0.67064(11) 0.23749(11) 0.93930(7) 0.0289(3) Uani 1 1 d . . .
H21A H 0.7399 0.2088 0.9523 0.043 Uiso 1 1 calc R . .
H21B H 0.6454 0.2175 0.9762 0.043 Uiso 1 1 calc R . .
H21C H 0.6751 0.3100 0.9385 0.043 Uiso 1 1 calc R . .
C22 C 0.79702(10) -0.00739(9) 0.81992(7) 0.0193(2) Uani 1 1 d . . .
H22 H 0.8635 -0.0234 0.8159 0.023 Uiso 1 1 calc R . .
C23 C 0.82327(12) 0.01507(11) 0.90045(7) 0.0283(3) Uani 1 1 d . . .
H23A H 0.8679 0.0741 0.9160 0.042 Uiso 1 1 calc R . .
H23B H 0.8601 -0.0416 0.9312 0.042 Uiso 1 1 calc R . .
H23C H 0.7588 0.0273 0.9062 0.042 Uiso 1 1 calc R . .
C24 C 0.72447(11) -0.09578(10) 0.79145(8) 0.0270(3) Uani 1 1 d . . .
H24A H 0.6610 -0.0839 0.7987 0.040 Uiso 1 1 calc R . .
H24B H 0.7596 -0.1555 0.8187 0.040 Uiso 1 1 calc R . .
H24C H 0.7059 -0.1051 0.7385 0.040 Uiso 1 1 calc R . .
C25 C 0.85599(11) -0.00853(9) 0.64364(7) 0.0220(2) Uani 1 1 d . . .
H25 H 0.8251 -0.0630 0.6620 0.026 Uiso 1 1 calc R . .
C26 C 0.97419(12) -0.01829(11) 0.68033(9) 0.0324(3) Uani 1 1 d . . .
H26A H 1.0049 0.0299 0.6584 0.049 Uiso 1 1 calc R . .
H26B H 0.9940 -0.0856 0.6726 0.049 Uiso 1 1 calc R . .
H26C H 0.9999 -0.0054 0.7336 0.049 Uiso 1 1 calc R . .
C27 C 0.81232(13) -0.01490(12) 0.56013(8) 0.0332(3) Uani 1 1 d . . .
H27A H 0.7361 -0.0097 0.5389 0.050 Uiso 1 1 calc R . .
H27B H 0.8321 -0.0786 0.5459 0.050 Uiso 1 1 calc R . .
H27C H 0.8405 0.0395 0.5414 0.050 Uiso 1 1 calc R . .
C28 C 0.91768(10) 0.28778(10) 0.63445(7) 0.0197(2) Uani 1 1 d . . .
H28 H 0.8917 0.2343 0.5961 0.024 Uiso 1 1 calc R . .
C29 C 1.03072(10) 0.26675(11) 0.68573(8) 0.0258(3) Uani 1 1 d . . .
H29A H 1.0583 0.3209 0.7217 0.039 Uiso 1 1 calc R . .
H29B H 1.0716 0.2616 0.6566 0.039 Uiso 1 1 calc R . .
H29C H 1.0353 0.2042 0.7120 0.039 Uiso 1 1 calc R . .
C30 C 0.90657(11) 0.38722(11) 0.59577(7) 0.0260(3) Uani 1 1 d . . .
H30A H 0.8328 0.3995 0.5636 0.039 Uiso 1 1 calc R . .
H30B H 0.9466 0.3862 0.5658 0.039 Uiso 1 1 calc R . .
H30C H 0.9332 0.4401 0.6329 0.039 Uiso 1 1 calc R . .
O1 O 0.53277(6) 0.34690(6) 0.68478(5) 0.01859(17) Uani 1 1 d . . .
O2 O 0.67311(6) 0.22885(6) 0.68366(4) 0.01579(16) Uani 1 1 d . . .
O3 O 0.81502(6) 0.28027(6) 0.80036(4) 0.01476(16) Uani 1 1 d . . .
O4 O 0.95103(6) 0.15459(6) 0.80291(4) 0.01640(16) Uani 1 1 d . . .
O5 O 0.73179(7) 0.42792(6) 0.70730(5) 0.01883(17) Uani 1 1 d . . .
H5A H 0.7715 0.4011 0.6910 0.028 Uiso 1 1 calc R . .
O6 O 0.66474(7) 0.42290(6) 0.82264(5) 0.01839(17) Uani 1 1 d . . .
O7 O 0.63749(7) 0.21766(6) 0.81046(5) 0.01780(17) Uani 1 1 d . . .
O8 O 0.75029(7) 0.07811(6) 0.77364(5) 0.01820(17) Uani 1 1 d . . .
H8A H 0.7116 0.1077 0.7895 0.027 Uiso 1 1 calc R . .
O9 O 0.82738(7) 0.08418(6) 0.66362(5) 0.01837(17) Uani 1 1 d . . .
O10 O 0.85585(7) 0.28754(6) 0.67580(5) 0.01758(17) Uani 1 1 d . . .
Ti1 Ti 0.666589(15) 0.325279(15) 0.764896(11) 0.01410(5) Uani 1 1 d . . .
Ti2 Ti 0.820746(16) 0.181925(15) 0.720383(11) 0.01369(5) 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
O1 C1 C2 123.81(11) . . ?
O1 C1 C6 116.79(10) . . ?
C2 C1 C6 119.40(12) . . ?
C1 C2 C3 119.14(12) . . ?
C4 C3 C2 120.83(12) . . ?
C3 C4 C5 120.55(13) . . ?
C6 C5 C4 118.42(12) . . ?
O2 C6 C5 125.09(11) . . ?
O2 C6 C1 113.23(10) . . ?
C5 C6 C1 121.63(11) . . ?
O3 C7 C8 125.13(10) . . ?
O3 C7 C12 113.30(10) . . ?
C8 C7 C12 121.56(10) . . ?
C7 C8 C9 118.51(11) . . ?
C10 C9 C8 120.46(11) . . ?
C9 C10 C11 120.80(11) . . ?
C12 C11 C10 119.28(11) . . ?
O4 C12 C11 124.16(11) . . ?
O4 C12 C7 116.45(10) . . ?
C11 C12 C7 119.39(11) . . ?
O5 C13 C14 111.55(11) . . ?
O5 C13 C15 109.30(10) . . ?
C14 C13 C15 112.30(12) . . ?
O6 C16 C17 109.66(11) . . ?
O6 C16 C18 108.69(10) . . ?
C17 C16 C18 112.91(12) . . ?
O7 C19 C20 110.37(11) . . ?
O7 C19 C21 110.41(10) . . ?
C20 C19 C21 112.71(11) . . ?
O8 C22 C23 110.85(10) . . ?
O8 C22 C24 109.42(10) . . ?
C23 C22 C24 112.11(11) . . ?
O9 C25 C27 109.01(11) . . ?
O9 C25 C26 109.09(11) . . ?
C27 C25 C26 112.20(12) . . ?
O10 C28 C29 109.80(10) . . ?
O10 C28 C30 109.63(10) . . ?
C29 C28 C30 111.07(11) . . ?
C1 O1 Ti1 118.08(7) . . ?
C6 O2 Ti2 139.99(7) . . ?
C6 O2 Ti1 112.75(7) . . ?
Ti2 O2 Ti1 107.00(4) . . ?
C7 O3 Ti1 136.15(7) . . ?
C7 O3 Ti2 113.20(7) . . ?
Ti1 O3 Ti2 107.14(4) . . ?
C12 O4 Ti2 118.39(7) . . ?
C16 O6 Ti1 166.79(8) . . ?
C19 O7 Ti1 137.40(8) . . ?
C25 O9 Ti2 159.18(8) . . ?
C28 O10 Ti2 129.03(8) . . ?
O6 Ti1 O7 101.44(4) . . ?
O6 Ti1 O1 98.54(4) . . ?
O7 Ti1 O1 100.48(4) . . ?
O6 Ti1 O3 107.45(4) . . ?
O7 Ti1 O3 90.42(4) . . ?
O1 Ti1 O3 149.22(4) . . ?
O6 Ti1 O2 169.44(4) . . ?
O7 Ti1 O2 89.10(4) . . ?
O1 Ti1 O2 78.63(3) . . ?
O3 Ti1 O2 72.80(3) . . ?
O6 Ti1 Ti2 144.00(3) . . ?
O7 Ti1 Ti2 88.99(3) . . ?
O1 Ti1 Ti2 113.45(3) . . ?
O3 Ti1 Ti2 37.41(2) . . ?
O2 Ti1 Ti2 35.40(2) . . ?
O9 Ti2 O10 99.71(4) . . ?
O9 Ti2 O4 96.51(4) . . ?
O10 Ti2 O4 101.73(4) . . ?
O9 Ti2 O2 109.40(4) . . ?
O10 Ti2 O2 91.83(4) . . ?
O4 Ti2 O2 148.29(4) . . ?
O9 Ti2 O3 170.75(4) . . ?
O10 Ti2 O3 89.02(4) . . ?
O4 Ti2 O3 78.61(3) . . ?
O2 Ti2 O3 73.04(3) . . ?
O9 Ti2 Ti1 146.00(3) . . ?
O10 Ti2 Ti1 91.18(3) . . ?
O4 Ti2 Ti1 112.76(3) . . ?
O2 Ti2 Ti1 37.60(2) . . ?
O3 Ti2 Ti1 35.45(2) . . ?
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 O1 1.3466(15) . ?
C1 C2 1.3918(16) . ?
C1 C6 1.4064(17) . ?
C2 C3 1.397(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.4022(18) . ?
C5 C6 1.3795(17) . ?
C6 O2 1.3611(13) . ?
C7 O3 1.3614(13) . ?
C7 C8 1.3824(16) . ?
C7 C12 1.4069(16) . ?
C8 C9 1.3993(16) . ?
C9 C10 1.3877(18) . ?
C10 C11 1.3969(17) . ?
C11 C12 1.3891(16) . ?
C12 O4 1.3495(14) . ?
C13 O5 1.4484(14) . ?
C13 C14 1.5083(19) . ?
C13 C15 1.5173(18) . ?
C16 O6 1.4221(14) . ?
C16 C17 1.5100(19) . ?
C16 C18 1.5124(19) . ?
C19 O7 1.4300(14) . ?
C19 C20 1.5153(18) . ?
C19 C21 1.5161(19) . ?
C22 O8 1.4482(14) . ?
C22 C23 1.5155(18) . ?
C22 C24 1.5166(18) . ?
C25 O9 1.4208(14) . ?
C25 C27 1.5116(18) . ?
C25 C26 1.520(2) . ?
C28 O10 1.4325(14) . ?
C28 C29 1.5155(18) . ?
C28 C30 1.5200(18) . ?
O1 Ti1 1.9120(8) . ?
O2 Ti2 2.0003(8) . ?
O2 Ti1 2.1070(8) . ?
O3 Ti1 2.0044(8) . ?
O3 Ti2 2.0995(8) . ?
O4 Ti2 1.9151(8) . ?
O6 Ti1 1.7545(9) . ?
O7 Ti1 1.8469(9) . ?
O9 Ti2 1.7637(8) . ?
O10 Ti2 1.8528(9) . ?
Ti1 Ti2 3.3023(3) . ?
