#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:45:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179261 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/81/4318183.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_4318183
loop_
_publ_author_name
'William O. Appiah'
'Angela D. DeGreeff'
'Gina L. Razidlo'
'Sarah J. Spessard'
'Maren Pink'
'Victor G. Young,'
'Gretchen E. Hofmeister'
_publ_section_title
;
 Linear Trimer Analogues of Calixarene as Chiral Coordinating Ligands:
 X-ray Crystallographic and NMR Spectroscopic Characterization of Chiral
 and Achiral Trisphenolates Complexed to Titanium(IV) and Aluminum(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3656
_journal_page_last               3667
_journal_paper_doi               10.1021/ic010685j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C116 H184 O15 Ti2'
_chemical_formula_weight         1914.43
_chemical_name_common            99323m_Ti2(trisphenolate)2(O-t-Bu)2
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.3210(10)
_cell_angle_beta                 108.001(2)
_cell_angle_gamma                99.821(2)
_cell_formula_units_Z            1
_cell_length_a                   14.6880(13)
_cell_length_b                   15.4702(14)
_cell_length_c                   15.8721(14)
_cell_measurement_temperature    173(2)
_cell_volume                     2831.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25238
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.200
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         12507
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0705
_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)+(0.1204P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                6526
_reflns_number_total             12507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010685j_1.cif
_cod_data_source_block           99323m_Ti2(trisphenolate)2(O-t-Bu)2
_cod_database_code               4318183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.74859(4) 0.06550(4) 0.09788(4) 0.02975(17) Uani 1 1 d . . .
O1 O 0.85581(16) 0.13418(16) 0.22896(16) 0.0354(5) Uani 1 1 d . . .
O2 O 0.63301(16) 0.03019(16) 0.11108(16) 0.0338(5) Uani 1 1 d . . .
O3 O 0.25209(16) -0.14925(16) -0.04777(17) 0.0354(5) Uani 1 1 d . . .
O4 O 0.76550(17) -0.04886(17) 0.01673(17) 0.0391(6) Uani 1 1 d . . .
C1 C 0.8180(2) 0.2147(2) 0.3756(2) 0.0305(7) Uani 1 1 d . . .
C2 C 0.8794(2) 0.1689(2) 0.3326(2) 0.0310(7) Uani 1 1 d . . .
C3 C 0.9648(2) 0.1579(2) 0.3925(3) 0.0340(7) Uani 1 1 d . . .
C4 C 0.9812(3) 0.1910(3) 0.4961(3) 0.0385(8) Uani 1 1 d . . .
H4 H 1.0375 0.1833 0.5379 0.046 Uiso 1 1 calc R . .
C5 C 0.9198(3) 0.2345(2) 0.5417(3) 0.0378(8) Uani 1 1 d . A .
C6 C 0.8394(2) 0.2473(2) 0.4797(3) 0.0359(8) Uani 1 1 d . . .
H6 H 0.7979 0.2792 0.5093 0.043 Uiso 1 1 calc R . .
C7 C 0.7259(2) 0.2285(2) 0.3132(2) 0.0317(7) Uani 1 1 d . . .
H7A H 0.7336 0.2271 0.2529 0.038 Uiso 1 1 calc R . .
H7B H 0.7241 0.2976 0.3592 0.038 Uiso 1 1 calc R . .
C8 C 0.6248(2) 0.1426(2) 0.2719(2) 0.0298(7) Uani 1 1 d . . .
C9 C 0.5745(2) 0.1558(2) 0.3355(3) 0.0343(7) Uani 1 1 d . . .
H9 H 0.6006 0.2212 0.4006 0.041 Uiso 1 1 calc R . .
C10 C 0.4875(2) 0.0770(2) 0.3074(2) 0.0330(7) Uani 1 1 d . . .
C11 C 0.4496(2) -0.0158(2) 0.2108(2) 0.0311(7) Uani 1 1 d . . .
H11 H 0.3895 -0.0700 0.1898 0.037 Uiso 1 1 calc R . .
C12 C 0.4954(2) -0.0339(2) 0.1421(2) 0.0292(7) Uani 1 1 d . . .
C13 C 0.5838(2) 0.0465(2) 0.1747(2) 0.0282(7) Uani 1 1 d . . .
C14 C 0.4561(2) -0.1385(2) 0.0376(2) 0.0301(7) Uani 1 1 d . . .
H14A H 0.4362 -0.1271 -0.0210 0.036 Uiso 1 1 calc R . .
H14B H 0.5126 -0.1654 0.0376 0.036 Uiso 1 1 calc R . .
C15 C 0.3650(2) -0.2197(2) 0.0178(2) 0.0298(7) Uani 1 1 d . . .
C16 C 0.2650(2) -0.2180(2) -0.0179(2) 0.0284(7) Uani 1 1 d . . .
C17 C 0.1834(2) -0.2813(2) -0.0195(2) 0.0307(7) Uani 1 1 d . . .
C18 C 0.2044(2) -0.3517(2) 0.0084(3) 0.0354(7) Uani 1 1 d . . .
H18 H 0.1496 -0.3964 0.0065 0.042 Uiso 1 1 calc R . .
C19 C 0.3000(3) -0.3608(3) 0.0389(3) 0.0386(8) Uani 1 1 d . B .
C20 C 0.3799(2) -0.2919(2) 0.0447(2) 0.0347(7) Uani 1 1 d . . .
H20 H 0.4468 -0.2941 0.0678 0.042 Uiso 1 1 calc R . .
C21 C 1.0379(3) 0.1139(3) 0.3491(3) 0.0428(8) Uani 1 1 d . . .
C22 C 1.0916(3) 0.1872(4) 0.3243(4) 0.0662(12) Uani 1 1 d . . .
H22A H 1.0405 0.1858 0.2664 0.099 Uiso 1 1 calc R . .
H22B H 1.1435 0.1638 0.3035 0.099 Uiso 1 1 calc R . .
H22C H 1.1252 0.2587 0.3873 0.099 Uiso 1 1 calc R . .
C23 C 1.1220(3) 0.1069(3) 0.4292(3) 0.0555(10) Uani 1 1 d . . .
H23A H 1.1621 0.1766 0.4941 0.083 Uiso 1 1 calc R . .
H23B H 1.1676 0.0802 0.3990 0.083 Uiso 1 1 calc R . .
H23C H 1.0900 0.0594 0.4455 0.083 Uiso 1 1 calc R . .
C24 C 0.9800(3) 0.0033(3) 0.2496(3) 0.0621(12) Uani 1 1 d . . .
H24A H 0.9405 -0.0414 0.2641 0.093 Uiso 1 1 calc R . .
H24B H 1.0295 -0.0254 0.2286 0.093 Uiso 1 1 calc R . .
H24C H 0.9330 0.0058 0.1923 0.093 Uiso 1 1 calc R . .
C25 C 0.9386(3) 0.2668(3) 0.6549(3) 0.0450(9) Uani 1 1 d D . .
C26 C 1.0248(6) 0.2363(6) 0.7051(5) 0.068(2) Uani 0.761(9) 1 d PD A 1
H26A H 1.0909 0.2774 0.7159 0.102 Uiso 0.761(9) 1 calc PR A 1
H26B H 1.0095 0.1616 0.6580 0.102 Uiso 0.761(9) 1 calc PR A 1
H26C H 1.0288 0.2507 0.7733 0.102 Uiso 0.761(9) 1 calc PR A 1
C27 C 0.8389(5) 0.2090(6) 0.6512(5) 0.080(3) Uani 0.761(9) 1 d PD A 1
H27A H 0.8510 0.2274 0.7227 0.120 Uiso 0.761(9) 1 calc PR A 1
H27B H 0.8192 0.1332 0.6050 0.120 Uiso 0.761(9) 1 calc PR A 1
H27C H 0.7833 0.2299 0.6237 0.120 Uiso 0.761(9) 1 calc PR A 1
C28 C 0.9679(6) 0.3824(4) 0.7235(4) 0.072(2) Uani 0.761(9) 1 d PD A 1
H28A H 0.9776 0.4019 0.7946 0.108 Uiso 0.761(9) 1 calc PR A 1
H28B H 0.9132 0.4028 0.6934 0.108 Uiso 0.761(9) 1 calc PR A 1
H28C H 1.0323 0.4185 0.7274 0.108 Uiso 0.761(9) 1 calc PR A 1
C26D C 1.0476(12) 0.3555(15) 0.7300(12) 0.081(8) Uani 0.239(9) 1 d PD A 2
H26D H 1.0498 0.4129 0.7187 0.122 Uiso 0.239(9) 1 calc PR A 2
H26E H 1.0997 0.3277 0.7149 0.122 Uiso 0.239(9) 1 calc PR A 2
H26F H 1.0616 0.3817 0.8037 0.122 Uiso 0.239(9) 1 calc PR A 2
C27D C 0.935(2) 0.1755(14) 0.6651(18) 0.091(10) Uani 0.239(9) 1 d PD A 2
H27D H 0.9841 0.1462 0.6432 0.137 Uiso 0.239(9) 1 calc PR A 2
H27E H 0.8656 0.1220 0.6199 0.137 Uiso 0.239(9) 1 calc PR A 2
H27F H 0.9540 0.1982 0.7389 0.137 Uiso 0.239(9) 1 calc PR A 2
C28D C 0.8640(15) 0.317(2) 0.6888(15) 0.088(10) Uani 0.239(9) 1 d PD A 2
H28D H 0.8716 0.3264 0.7562 0.131 Uiso 0.239(9) 1 calc PR A 2
H28E H 0.7931 0.2718 0.6347 0.131 Uiso 0.239(9) 1 calc PR A 2
H28F H 0.8799 0.3856 0.6970 0.131 Uiso 0.239(9) 1 calc PR A 2
C29 C 0.4397(3) 0.0958(3) 0.3851(3) 0.0405(8) Uani 1 1 d . . .
C30 C 0.4032(3) 0.1871(3) 0.4052(3) 0.0615(11) Uani 1 1 d . . .
H30A H 0.3510 0.1707 0.3384 0.092 Uiso 1 1 calc R . .
H30B H 0.4619 0.2505 0.4351 0.092 Uiso 1 1 calc R . .
H30C H 0.3734 0.1988 0.4550 0.092 Uiso 1 1 calc R . .
C31 C 0.3486(3) -0.0009(3) 0.3440(3) 0.0583(11) Uani 1 1 d . . .
H31A H 0.3208 0.0143 0.3958 0.087 Uiso 1 1 calc R . .
H31B H 0.3717 -0.0594 0.3329 0.087 Uiso 1 1 calc R . .
H31C H 0.2949 -0.0196 0.2769 0.087 Uiso 1 1 calc R . .
C32 C 0.5225(3) 0.1232(3) 0.4904(3) 0.0527(10) Uani 1 1 d . . .
H32A H 0.5784 0.1893 0.5219 0.079 Uiso 1 1 calc R . .
H32B H 0.5501 0.0673 0.4773 0.079 Uiso 1 1 calc R . .
H32C H 0.4919 0.1303 0.5389 0.079 Uiso 1 1 calc R . .
C33 C 0.0775(2) -0.2709(3) -0.0446(3) 0.0369(8) Uani 1 1 d . . .
C34 C 0.0249(3) -0.3041(3) -0.1601(3) 0.0486(9) Uani 1 1 d . . .
H34A H 0.0710 -0.2642 -0.1739 0.073 Uiso 1 1 calc R . .
H34B H -0.0391 -0.2904 -0.1736 0.073 Uiso 1 1 calc R . .
H34C H 0.0092 -0.3791 -0.2067 0.073 Uiso 1 1 calc R . .
C35 C 0.0902(3) -0.1578(3) 0.0311(3) 0.0520(10) Uani 1 1 d . . .
H35A H 0.1237 -0.1387 0.1042 0.078 Uiso 1 1 calc R . .
H35B H 0.0223 -0.1522 0.0160 0.078 Uiso 1 1 calc R . .
H35C H 0.1326 -0.1103 0.0213 0.078 Uiso 1 1 calc R . .
C36 C 0.0045(3) -0.3415(3) -0.0308(3) 0.0526(10) Uani 1 1 d . . .
H36A H -0.0080 -0.4150 -0.0800 0.079 Uiso 1 1 calc R . .
H36B H -0.0610 -0.3307 -0.0455 0.079 Uiso 1 1 calc R . .
H36C H 0.0359 -0.3240 0.0420 0.079 Uiso 1 1 calc R . .
C37 C 0.3178(3) -0.4416(3) 0.0670(3) 0.0576(11) Uani 1 1 d D . .
C38 C 0.4015(8) -0.3751(8) 0.1864(9) 0.129(6) Uani 0.601(12) 1 d PD B 1
H38A H 0.3832 -0.3172 0.2280 0.193 Uiso 0.601(12) 1 calc PR B 1
H38B H 0.4691 -0.3471 0.1909 0.193 Uiso 0.601(12) 1 calc PR B 1
H38C H 0.4041 -0.4200 0.2144 0.193 Uiso 0.601(12) 1 calc PR B 1
C39 C 0.3583(13) -0.5116(10) -0.0010(13) 0.112(6) Uani 0.601(12) 1 d PD B 1
H39A H 0.4238 -0.4695 0.0100 0.169 Uiso 0.601(12) 1 calc PR B 1
H39B H 0.3084 -0.5490 -0.0754 0.169 Uiso 0.601(12) 1 calc PR B 1
H39C H 0.3691 -0.5623 0.0180 0.169 Uiso 0.601(12) 1 calc PR B 1
C40 C 0.2242(5) -0.5023(7) 0.0654(8) 0.062(3) Uani 0.601(12) 1 d PD B 1
H40A H 0.2393 -0.5541 0.0810 0.094 Uiso 0.601(12) 1 calc PR B 1
H40B H 0.1659 -0.5382 -0.0047 0.094 Uiso 0.601(12) 1 calc PR B 1
H40C H 0.2068 -0.4540 0.1188 0.094 Uiso 0.601(12) 1 calc PR B 1
C38D C 0.4143(9) -0.4620(12) 0.0636(12) 0.065(4) Uani 0.399(12) 1 d PD B 2
H38D H 0.4751 -0.4004 0.1230 0.098 Uiso 0.399(12) 1 calc PR B 2
H38E H 0.4148 -0.4762 -0.0031 0.098 Uiso 0.399(12) 1 calc PR B 2
H38F H 0.4153 -0.5227 0.0685 0.098 Uiso 0.399(12) 1 calc PR B 2
C39D C 0.2262(8) -0.5511(8) -0.0239(12) 0.076(6) Uani 0.399(12) 1 d PD B 2
H39D H 0.2362 -0.6048 -0.0094 0.113 Uiso 0.399(12) 1 calc PR B 2
H39E H 0.2257 -0.5710 -0.0922 0.113 Uiso 0.399(12) 1 calc PR B 2
H39F H 0.1604 -0.5449 -0.0258 0.113 Uiso 0.399(12) 1 calc PR B 2
C40D C 0.3163(19) -0.4115(13) 0.1691(13) 0.129(11) Uani 0.399(12) 1 d PD B 2
H40D H 0.2550 -0.3946 0.1696 0.194 Uiso 0.399(12) 1 calc PR B 2
H40E H 0.3783 -0.3502 0.2267 0.194 Uiso 0.399(12) 1 calc PR B 2
H40F H 0.3145 -0.4699 0.1788 0.194 Uiso 0.399(12) 1 calc PR B 2
C41 C 0.7314(3) -0.1534(3) -0.0725(3) 0.0407(8) Uani 1 1 d . . .
C42 C 0.7450(4) -0.2228(3) -0.0295(4) 0.0807(16) Uani 1 1 d . . .
H42A H 0.8176 -0.1978 0.0195 0.121 Uiso 1 1 calc R . .
H42B H 0.7238 -0.2951 -0.0882 0.121 Uiso 1 1 calc R . .
H42C H 0.7025 -0.2203 0.0080 0.121 Uiso 1 1 calc R . .
C43 C 0.6189(3) -0.1856(3) -0.1448(3) 0.0583(11) Uani 1 1 d . . .
H43A H 0.5773 -0.1855 -0.1069 0.087 Uiso 1 1 calc R . .
H43B H 0.5948 -0.2560 -0.2076 0.087 Uiso 1 1 calc R . .
H43C H 0.6121 -0.1360 -0.1662 0.087 Uiso 1 1 calc R . .
C44 C 0.7991(3) -0.1501(3) -0.1270(3) 0.0652(12) Uani 1 1 d . . .
H44A H 0.7847 -0.1087 -0.1577 0.098 Uiso 1 1 calc R . .
H44B H 0.7847 -0.2215 -0.1832 0.098 Uiso 1 1 calc R . .
H44C H 0.8717 -0.1180 -0.0754 0.098 Uiso 1 1 calc R . .
O5 O 0.6977(3) 0.4103(3) 0.5478(3) 0.1064(13) Uani 1 1 d . . .
C50 C 0.6919(7) 0.4501(6) 0.6429(5) 0.146(3) Uani 1 1 d . . .
H50A H 0.6414 0.3951 0.6387 0.175 Uiso 1 1 calc R . .
H50B H 0.7599 0.4713 0.6999 0.175 Uiso 1 1 calc R . .
C51 C 0.6628(8) 0.5345(6) 0.6664(7) 0.155(4) Uani 1 1 d . . .
H51A H 0.7117 0.5948 0.7386 0.186 Uiso 1 1 calc R . .
H51B H 0.5932 0.5174 0.6631 0.186 Uiso 1 1 calc R . .
C52 C 0.6626(6) 0.5605(5) 0.5878(6) 0.122(2) Uani 1 1 d . . .
H52A H 0.5996 0.5735 0.5605 0.147 Uiso 1 1 calc R . .
H52B H 0.7239 0.6229 0.6185 0.147 Uiso 1 1 calc R . .
C53 C 0.6651(5) 0.4668(5) 0.5049(5) 0.1030(19) Uani 1 1 d . . .
H53A H 0.5957 0.4238 0.4445 0.124 Uiso 1 1 calc R . .
H53B H 0.7133 0.4867 0.4792 0.124 Uiso 1 1 calc R . .
O6 O 0.4409(3) -0.4782(3) -0.2770(3) 0.1136(13) Uani 1 1 d D . .
C60 C 0.3691(5) -0.5822(4) -0.3375(5) 0.106(2) Uani 1 1 d D . .
H60A H 0.3999 -0.6257 -0.3167 0.128 Uiso 1 1 calc R . .
H60B H 0.3496 -0.6128 -0.4136 0.128 Uiso 1 1 calc R . .
C61 C 0.2786(4) -0.5803(4) -0.3183(6) 0.133(3) Uani 1 1 d D . .
H61A H 0.2666 -0.6230 -0.2888 0.160 Uiso 1 1 calc R . .
H61B H 0.2168 -0.6087 -0.3850 0.160 Uiso 1 1 calc R . .
C62 C 0.2991(4) -0.4710(4) -0.2429(5) 0.109(2) Uani 1 1 d D . .
H62A H 0.2556 -0.4437 -0.2777 0.131 Uiso 1 1 calc R . .
H62B H 0.2846 -0.4638 -0.1835 0.131 Uiso 1 1 calc R . .
C63 C 0.4076(4) -0.4143(4) -0.2048(5) 0.111(2) Uani 1 1 d D . .
H63A H 0.4172 -0.3473 -0.2005 0.134 Uiso 1 1 calc R . .
H63B H 0.4481 -0.3989 -0.1335 0.134 Uiso 1 1 calc R . .
O7 O 1.3761(6) 0.2259(5) 0.7763(7) 0.102(3) Uiso 0.531(9) 1 d PD C 1
C70 C 1.3476(12) 0.1343(9) 0.6550(10) 0.112(5) Uiso 0.531(9) 1 d PD C 1
H70A H 1.3039 0.1453 0.6022 0.134 Uiso 0.531(9) 1 calc PR C 1
H70B H 1.4098 0.1275 0.6450 0.134 Uiso 0.531(9) 1 calc PR C 1
C71 C 1.2912(11) 0.0461(8) 0.6531(9) 0.098(4) Uiso 0.531(9) 1 d PD C 1
H71A H 1.3307 0.0003 0.6532 0.118 Uiso 0.531(9) 1 calc PR C 1
H71B H 1.2233 0.0041 0.5903 0.118 Uiso 0.531(9) 1 calc PR C 1
C72 C 1.2791(8) 0.0972(7) 0.7523(8) 0.079(3) Uiso 0.531(9) 1 d PD C 1
H72A H 1.2160 0.0539 0.7455 0.095 Uiso 0.531(9) 1 calc PR C 1
H72B H 1.3396 0.1114 0.8132 0.095 Uiso 0.531(9) 1 calc PR C 1
C73 C 1.2716(9) 0.1945(8) 0.7629(11) 0.099(5) Uiso 0.531(9) 1 d PD C 1
H73A H 1.2198 0.1841 0.6982 0.119 Uiso 0.531(9) 1 calc PR C 1
H73B H 1.2626 0.2401 0.8258 0.119 Uiso 0.531(9) 1 calc PR C 1
O7D O 1.3274(8) 0.2228(7) 0.7173(9) 0.120(4) Uiso 0.469(9) 1 d PD C 2
C70D C 1.3948(9) 0.1596(8) 0.6938(10) 0.078(4) Uiso 0.469(9) 1 d PD C 2
H70C H 1.4290 0.1740 0.6543 0.094 Uiso 0.469(9) 1 calc PR C 2
H70D H 1.4470 0.1711 0.7588 0.094 Uiso 0.469(9) 1 calc PR C 2
C71D C 1.3162(8) 0.0577(7) 0.6300(8) 0.066(3) Uiso 0.469(9) 1 d PD C 2
H71C H 1.3442 0.0064 0.6374 0.079 Uiso 0.469(9) 1 calc PR C 2
H71D H 1.2867 0.0344 0.5546 0.079 Uiso 0.469(9) 1 calc PR C 2
C72D C 1.2349(8) 0.0683(7) 0.6705(9) 0.075(3) Uiso 0.469(9) 1 d PD C 2
H72C H 1.1738 0.0683 0.6214 0.090 Uiso 0.469(9) 1 calc PR C 2
H72D H 1.2129 0.0110 0.6806 0.090 Uiso 0.469(9) 1 calc PR C 2
C73D C 1.2896(13) 0.1711(11) 0.7731(11) 0.113(6) Uiso 0.469(9) 1 d PD C 2
H73C H 1.3466 0.1718 0.8271 0.135 Uiso 0.469(9) 1 calc PR C 2
H73D H 1.2432 0.1997 0.8018 0.135 Uiso 0.469(9) 1 calc PR C 2
O8 O 0.8742(4) 0.4819(5) 0.4498(4) 0.0698(16) Uani 0.50 1 d PD D -1
C80 C 0.9403(7) 0.5252(13) 0.5572(5) 0.087(3) Uani 0.50 1 d PD D -1
H80A H 0.9064 0.4934 0.5866 0.105 Uiso 0.50 1 calc PR D -1
H80B H 0.9572 0.6017 0.5991 0.105 Uiso 0.50 1 calc PR D -1
C81 C 1.0338(6) 0.5036(14) 0.5618(7) 0.103(3) Uani 0.50 1 d PD D -1
H81A H 1.0364 0.4497 0.5787 0.123 Uiso 0.50 1 calc PR D -1
H81B H 1.0955 0.5679 0.6167 0.123 Uiso 0.50 1 calc PR D -1
C82 C 1.0302(7) 0.4661(15) 0.4576(8) 0.087(3) Uani 0.50 1 d PD D -1
H82A H 1.0908 0.5120 0.4633 0.105 Uiso 0.50 1 calc PR D -1
H82B H 1.0298 0.3939 0.4246 0.105 Uiso 0.50 1 calc PR D -1
C83 C 0.9356(6) 0.4683(13) 0.3948(6) 0.103(3) Uani 0.50 1 d PD D -1
H83A H 0.9515 0.5268 0.3849 0.123 Uiso 0.50 1 calc PR D -1
H83B H 0.8984 0.4020 0.3243 0.123 Uiso 0.50 1 calc PR D -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'
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
O4 Ti1 O2 109.52(10) . . ?
O4 Ti1 O3 111.21(10) . 2_655 ?
O2 Ti1 O3 112.16(10) . 2_655 ?
O4 Ti1 O1 107.29(10) . . ?
O2 Ti1 O1 106.96(10) . . ?
O3 Ti1 O1 109.49(10) 2_655 . ?
C2 O1 Ti1 142.9(2) . . ?
C13 O2 Ti1 148.8(2) . . ?
C16 O3 Ti1 169.18(19) . 2_655 ?
C41 O4 Ti1 154.5(2) . . ?
C2 C1 C6 118.9(3) . . ?
C2 C1 C7 123.1(3) . . ?
C6 C1 C7 118.0(3) . . ?
O1 C2 C1 118.5(3) . . ?
O1 C2 C3 119.6(3) . . ?
C1 C2 C3 121.9(3) . . ?
C4 C3 C2 116.3(3) . . ?
C4 C3 C21 120.8(3) . . ?
C2 C3 C21 122.9(3) . . ?
C5 C4 C3 123.9(3) . . ?
C6 C5 C4 116.9(3) . . ?
C6 C5 C25 120.9(3) . . ?
C4 C5 C25 122.2(3) . . ?
C5 C6 C1 122.1(3) . . ?
C1 C7 C8 111.6(2) . . ?
C9 C8 C13 117.9(3) . . ?
C9 C8 C7 119.3(3) . . ?
C13 C8 C7 122.6(3) . . ?
C8 C9 C10 122.6(3) . . ?
C11 C10 C9 117.3(3) . . ?
C11 C10 C29 123.3(3) . . ?
C9 C10 C29 119.4(3) . . ?
C10 C11 C12 123.1(3) . . ?
C13 C12 C11 117.4(3) . . ?
C13 C12 C14 119.7(3) . . ?
C11 C12 C14 122.8(3) . . ?
O2 C13 C12 119.0(3) . . ?
O2 C13 C8 119.3(3) . . ?
C12 C13 C8 121.6(3) . . ?
C15 C14 C12 113.1(2) . . ?
C20 C15 C16 118.5(3) . . ?
C20 C15 C14 120.0(3) . . ?
C16 C15 C14 121.2(3) . . ?
O3 C16 C17 121.3(3) . . ?
O3 C16 C15 117.0(3) . . ?
C17 C16 C15 121.6(3) . . ?
C16 C17 C18 116.4(3) . . ?
C16 C17 C33 122.5(3) . . ?
C18 C17 C33 121.1(3) . . ?
C19 C18 C17 124.4(3) . . ?
C18 C19 C20 116.7(3) . . ?
C18 C19 C37 122.0(3) . . ?
C20 C19 C37 121.3(3) . . ?
C19 C20 C15 122.2(3) . . ?
C24 C21 C23 106.6(3) . . ?
C24 C21 C22 109.9(3) . . ?
C23 C21 C22 107.6(3) . . ?
C24 C21 C3 111.6(3) . . ?
C23 C21 C3 112.2(3) . . ?
C22 C21 C3 108.9(3) . . ?
C27D C25 C28 139.3(9) . . ?
C27D C25 C28D 112.2(12) . . ?
C28 C25 C28D 57.0(10) . . ?
C27D C25 C5 110.0(8) . . ?
C28 C25 C5 110.1(3) . . ?
C28D C25 C5 112.4(7) . . ?
C27D C25 C26 48.1(11) . . ?
C28 C25 C26 108.5(4) . . ?
C28D C25 C26 135.4(8) . . ?
C5 C25 C26 112.1(3) . . ?
C27D C25 C27 62.5(11) . . ?
C28 C25 C27 109.8(5) . . ?
C28D C25 C27 54.9(10) . . ?
C5 C25 C27 109.0(3) . . ?
C26 C25 C27 107.1(5) . . ?
C27D C25 C26D 110.6(13) . . ?
C28 C25 C26D 50.2(9) . . ?
C28D C25 C26D 105.1(11) . . ?
C5 C25 C26D 106.3(7) . . ?
C26 C25 C26D 64.0(9) . . ?
C27 C25 C26D 144.1(7) . . ?
C31 C29 C30 108.8(3) . . ?
C31 C29 C32 108.2(3) . . ?
C30 C29 C32 109.0(3) . . ?
C31 C29 C10 112.2(3) . . ?
C30 C29 C10 110.0(3) . . ?
C32 C29 C10 108.5(3) . . ?
C34 C33 C36 106.6(3) . . ?
C34 C33 C35 111.2(3) . . ?
C36 C33 C35 106.8(3) . . ?
C34 C33 C17 109.8(3) . . ?
C36 C33 C17 112.5(3) . . ?
C35 C33 C17 109.9(3) . . ?
C40D C37 C39 135.9(8) . . ?
C40D C37 C40 61.9(9) . . ?
C39 C37 C40 112.4(6) . . ?
C40D C37 C38D 112.2(9) . . ?
C39 C37 C38D 35.8(6) . . ?
C40 C37 C38D 132.0(7) . . ?
C40D C37 C19 111.0(6) . . ?
C39 C37 C19 110.6(5) . . ?
C40 C37 C19 113.3(4) . . ?
C38D C37 C19 112.7(7) . . ?
C40D C37 C38 44.7(9) . . ?
C39 C37 C38 109.5(7) . . ?
C40 C37 C38 105.0(6) . . ?
C38D C37 C38 74.9(7) . . ?
C19 C37 C38 105.5(4) . . ?
C40D C37 C39D 108.9(9) . . ?
C39 C37 C39D 71.0(7) . . ?
C40 C37 C39D 48.4(6) . . ?
C38D C37 C39D 104.3(7) . . ?
C19 C37 C39D 107.4(5) . . ?
C38 C37 C39D 144.3(6) . . ?
O4 C41 C44 106.5(3) . . ?
O4 C41 C43 108.3(3) . . ?
C44 C41 C43 111.4(3) . . ?
O4 C41 C42 106.9(3) . . ?
C44 C41 C42 112.0(3) . . ?
C43 C41 C42 111.6(3) . . ?
C50 O5 C53 108.0(4) . . ?
C51 C50 O5 110.6(6) . . ?
C50 C51 C52 107.5(6) . . ?
C53 C52 C51 103.0(5) . . ?
O5 C53 C52 107.8(5) . . ?
C60 O6 C63 108.1(4) . . ?
O6 C60 C61 108.3(3) . . ?
C60 C61 C62 106.6(2) . . ?
C63 C62 C61 106.0(3) . . ?
O6 C63 C62 107.7(3) . . ?
C73 O7 C70 94.2(8) . . ?
C71 C70 O7 97.7(8) . . ?
C70 C71 C72 103.1(8) . . ?
C73 C72 C71 101.9(8) . . ?
O7 C73 C72 88.7(8) . . ?
C70D O7D C73D 93.0(9) . . ?
C71D C70D O7D 98.0(8) . . ?
C70D C71D C72D 105.4(7) . . ?
C73D C72D C71D 102.7(8) . . ?
C72D C73D O7D 90.2(9) . . ?
C80 O8 C83 107.5(4) . . ?
O8 C80 C81 107.7(4) . . ?
C80 C81 C82 106.5(3) . . ?
C83 C82 C81 106.4(3) . . ?
O8 C83 C82 107.6(4) . . ?
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
Ti1 O4 1.763(2) . ?
Ti1 O2 1.798(2) . ?
Ti1 O3 1.805(2) 2_655 ?
Ti1 O1 1.820(2) . ?
O1 C2 1.373(4) . ?
O2 C13 1.374(3) . ?
O3 C16 1.367(3) . ?
O3 Ti1 1.805(2) 2_655 ?
O4 C41 1.434(4) . ?
C1 C2 1.393(4) . ?
C1 C6 1.395(4) . ?
C1 C7 1.523(4) . ?
C2 C3 1.410(4) . ?
C3 C4 1.402(5) . ?
C3 C21 1.538(4) . ?
C4 C5 1.399(5) . ?
C5 C6 1.393(5) . ?
C5 C25 1.540(5) . ?
C7 C8 1.525(4) . ?
C8 C9 1.389(4) . ?
C8 C13 1.402(4) . ?
C9 C10 1.393(4) . ?
C10 C11 1.379(4) . ?
C10 C29 1.541(4) . ?
C11 C12 1.400(4) . ?
C12 C13 1.393(4) . ?
C12 C14 1.525(4) . ?
C14 C15 1.507(4) . ?
C15 C20 1.394(4) . ?
C15 C16 1.411(4) . ?
C16 C17 1.397(4) . ?
C17 C18 1.398(4) . ?
C17 C33 1.538(4) . ?
C18 C19 1.392(5) . ?
C19 C20 1.392(4) . ?
C19 C37 1.543(5) . ?
C21 C24 1.529(5) . ?
C21 C23 1.534(5) . ?
C21 C22 1.537(5) . ?
C25 C27D 1.489(12) . ?
C25 C28 1.493(6) . ?
C25 C28D 1.539(12) . ?
C25 C26 1.545(6) . ?
C25 C27 1.550(6) . ?
C25 C26D 1.560(13) . ?
C29 C31 1.527(5) . ?
C29 C30 1.528(5) . ?
C29 C32 1.539(5) . ?
C33 C34 1.531(5) . ?
C33 C36 1.536(4) . ?
C33 C35 1.536(5) . ?
C37 C40D 1.476(10) . ?
C37 C39 1.494(9) . ?
C37 C40 1.513(7) . ?
C37 C38D 1.515(11) . ?
C37 C38 1.582(9) . ?
C37 C39D 1.594(10) . ?
C41 C44 1.515(5) . ?
C41 C43 1.522(5) . ?
C41 C42 1.525(5) . ?
O5 C50 1.382(7) . ?
O5 C53 1.395(6) . ?
C50 C51 1.368(8) . ?
C51 C52 1.475(9) . ?
C52 C53 1.460(7) . ?
O6 C60 1.414(4) . ?
O6 C63 1.414(4) . ?
C60 C61 1.454(5) . ?
C61 C62 1.459(7) . ?
C62 C63 1.454(5) . ?
O7 C73 1.444(11) . ?
O7 C70 1.639(11) . ?
C70 C71 1.453(12) . ?
C71 C72 1.487(12) . ?
C72 C73 1.464(12) . ?
O7D C70D 1.516(11) . ?
O7D C73D 1.591(12) . ?
C70D C71D 1.427(11) . ?
C71D C72D 1.520(12) . ?
C72D C73D 1.485(12) . ?
O8 C80 1.415(4) . ?
O8 C83 1.415(4) . ?
C80 C81 1.455(5) . ?
C81 C82 1.459(7) . ?
C82 C83 1.455(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Ti1 O1 C2 -118.3(3) . . . . ?
O2 Ti1 O1 C2 -0.9(3) . . . . ?
O3 Ti1 O1 C2 120.9(3) 2_655 . . . ?
O4 Ti1 O2 C13 136.8(4) . . . . ?
O3 Ti1 O2 C13 -99.3(4) 2_655 . . . ?
O1 Ti1 O2 C13 20.8(4) . . . . ?
O2 Ti1 O4 C41 40.9(5) . . . . ?
O3 Ti1 O4 C41 -83.7(5) 2_655 . . . ?
O1 Ti1 O4 C41 156.6(5) . . . . ?
Ti1 O1 C2 C1 -41.8(5) . . . . ?
Ti1 O1 C2 C3 138.5(3) . . . . ?
C6 C1 C2 O1 178.1(3) . . . . ?
C7 C1 C2 O1 -0.2(4) . . . . ?
C6 C1 C2 C3 -2.3(5) . . . . ?
C7 C1 C2 C3 179.5(3) . . . . ?
O1 C2 C3 C4 -177.3(3) . . . . ?
C1 C2 C3 C4 3.1(5) . . . . ?
O1 C2 C3 C21 3.6(5) . . . . ?
C1 C2 C3 C21 -176.1(3) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
C21 C3 C4 C5 178.1(3) . . . . ?
C3 C4 C5 C6 -1.5(5) . . . . ?
C3 C4 C5 C25 178.2(3) . . . . ?
C4 C5 C6 C1 2.4(5) . . . . ?
C25 C5 C6 C1 -177.3(3) . . . . ?
C2 C1 C6 C5 -0.6(5) . . . . ?
C7 C1 C6 C5 177.7(3) . . . . ?
C2 C1 C7 C8 99.0(3) . . . . ?
C6 C1 C7 C8 -79.2(3) . . . . ?
C1 C7 C8 C9 87.5(3) . . . . ?
C1 C7 C8 C13 -87.6(4) . . . . ?
C13 C8 C9 C10 1.6(5) . . . . ?
C7 C8 C9 C10 -173.7(3) . . . . ?
C8 C9 C10 C11 -2.1(5) . . . . ?
C8 C9 C10 C29 176.7(3) . . . . ?
C9 C10 C11 C12 1.1(5) . . . . ?
C29 C10 C11 C12 -177.6(3) . . . . ?
C10 C11 C12 C13 0.3(5) . . . . ?
C10 C11 C12 C14 177.0(3) . . . . ?
Ti1 O2 C13 C12 -158.3(3) . . . . ?
Ti1 O2 C13 C8 20.2(5) . . . . ?
C11 C12 C13 O2 177.6(3) . . . . ?
C14 C12 C13 O2 0.8(4) . . . . ?
C11 C12 C13 C8 -0.9(4) . . . . ?
C14 C12 C13 C8 -177.7(3) . . . . ?
C9 C8 C13 O2 -178.5(3) . . . . ?
C7 C8 C13 O2 -3.4(4) . . . . ?
C9 C8 C13 C12 -0.1(4) . . . . ?
C7 C8 C13 C12 175.1(3) . . . . ?
C13 C12 C14 C15 175.5(3) . . . . ?
C11 C12 C14 C15 -1.1(4) . . . . ?
C12 C14 C15 C20 -95.4(3) . . . . ?
C12 C14 C15 C16 78.1(4) . . . . ?
Ti1 O3 C16 C17 -142.6(9) 2_655 . . . ?
Ti1 O3 C16 C15 39.4(12) 2_655 . . . ?
C20 C15 C16 O3 -177.4(3) . . . . ?
C14 C15 C16 O3 8.9(4) . . . . ?
C20 C15 C16 C17 4.7(4) . . . . ?
C14 C15 C16 C17 -169.0(3) . . . . ?
O3 C16 C17 C18 177.4(3) . . . . ?
C15 C16 C17 C18 -4.7(4) . . . . ?
O3 C16 C17 C33 -5.8(4) . . . . ?
C15 C16 C17 C33 172.1(3) . . . . ?
C16 C17 C18 C19 1.2(5) . . . . ?
C33 C17 C18 C19 -175.6(3) . . . . ?
C17 C18 C19 C20 2.3(5) . . . . ?
C17 C18 C19 C37 -178.9(3) . . . . ?
C18 C19 C20 C15 -2.4(5) . . . . ?
C37 C19 C20 C15 178.8(3) . . . . ?
C16 C15 C20 C19 -0.9(5) . . . . ?
C14 C15 C20 C19 172.8(3) . . . . ?
C4 C3 C21 C24 122.4(4) . . . . ?
C2 C3 C21 C24 -58.4(4) . . . . ?
C4 C3 C21 C23 2.8(5) . . . . ?
C2 C3 C21 C23 -178.1(3) . . . . ?
C4 C3 C21 C22 -116.2(4) . . . . ?
C2 C3 C21 C22 63.0(4) . . . . ?
C6 C5 C25 C27D 122.9(13) . . . . ?
C4 C5 C25 C27D -56.8(13) . . . . ?
C6 C5 C25 C28 -64.4(5) . . . . ?
C4 C5 C25 C28 115.9(5) . . . . ?
C6 C5 C25 C28D -2.9(12) . . . . ?
C4 C5 C25 C28D 177.5(12) . . . . ?
C6 C5 C25 C26 174.6(4) . . . . ?
C4 C5 C25 C26 -5.1(6) . . . . ?
C6 C5 C25 C27 56.1(5) . . . . ?
C4 C5 C25 C27 -123.5(5) . . . . ?
C6 C5 C25 C26D -117.4(10) . . . . ?
C4 C5 C25 C26D 63.0(10) . . . . ?
C11 C10 C29 C31 1.8(5) . . . . ?
C9 C10 C29 C31 -176.8(3) . . . . ?
C11 C10 C29 C30 -119.5(4) . . . . ?
C9 C10 C29 C30 61.9(4) . . . . ?
C11 C10 C29 C32 121.4(3) . . . . ?
C9 C10 C29 C32 -57.3(4) . . . . ?
C16 C17 C33 C34 67.1(4) . . . . ?
C18 C17 C33 C34 -116.3(3) . . . . ?
C16 C17 C33 C36 -174.4(3) . . . . ?
C18 C17 C33 C36 2.3(4) . . . . ?
C16 C17 C33 C35 -55.6(4) . . . . ?
C18 C17 C33 C35 121.1(3) . . . . ?
C18 C19 C37 C40D -71.5(11) . . . . ?
C20 C19 C37 C40D 107.2(11) . . . . ?
C18 C19 C37 C39 123.1(8) . . . . ?
C20 C19 C37 C39 -58.1(9) . . . . ?
C18 C19 C37 C40 -4.1(6) . . . . ?
C20 C19 C37 C40 174.7(5) . . . . ?
C18 C19 C37 C38D 161.7(7) . . . . ?
C20 C19 C37 C38D -19.5(8) . . . . ?
C18 C19 C37 C38 -118.5(6) . . . . ?
C20 C19 C37 C38 60.3(7) . . . . ?
C18 C19 C37 C39D 47.4(8) . . . . ?
C20 C19 C37 C39D -133.8(7) . . . . ?
Ti1 O4 C41 C44 127.9(4) . . . . ?
Ti1 O4 C41 C43 8.1(6) . . . . ?
Ti1 O4 C41 C42 -112.3(5) . . . . ?
C53 O5 C50 C51 -3.7(9) . . . . ?
O5 C50 C51 C52 -7.8(11) . . . . ?
C50 C51 C52 C53 15.5(10) . . . . ?
C50 O5 C53 C52 13.8(8) . . . . ?
C51 C52 C53 O5 -17.7(8) . . . . ?
C63 O6 C60 C61 11.7(7) . . . . ?
O6 C60 C61 C62 -0.6(8) . . . . ?
C60 C61 C62 C63 -10.3(8) . . . . ?
C60 O6 C63 C62 -18.4(7) . . . . ?
C61 C62 C63 O6 17.7(7) . . . . ?
C73 O7 C70 C71 -50.3(12) . . . . ?
O7 C70 C71 C72 10.1(12) . . . . ?
C70 C71 C72 C73 32.4(13) . . . . ?
C70 O7 C73 C72 67.1(9) . . . . ?
C71 C72 C73 O7 -64.7(10) . . . . ?
C73D O7D C70D C71D 59.9(11) . . . . ?
O7D C70D C71D C72D -29.6(12) . . . . ?
C70D C71D C72D C73D -14.2(14) . . . . ?
C71D C72D C73D O7D 48.6(12) . . . . ?
C70D O7D C73D C72D -66.3(11) . . . . ?
C83 O8 C80 C81 -20.3(13) . . . . ?
O8 C80 C81 C82 11.7(17) . . . . ?
C80 C81 C82 C83 1.0(19) . . . . ?
C80 O8 C83 C82 21.0(12) . . . . ?
C81 C82 C83 O8 -13.4(17) . . . . ?
