#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320692.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_4320692
_publ_author_name                'Udo Radius'
_publ_contact_author
;
  Udo Radius
  Institut für Anorganische Chemie der Universität
  Engesserstrasse, Gebäude 30.45
  D-76128 Karlsruhe
  Deutschland
;
_publ_contact_author_email       uradius@achibm6.chemie.uni_karlsruhe.de
_publ_contact_author_fax         'Int + 721 661921'
_publ_contact_author_phone       'Int + 721 608 2855'
_publ_section_title
;
 Shaping the Cavity of the Macrocyclic Ligand in Metallocalix[4]arenes:
 The Role of the Ligand Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6637
_journal_page_last               6642
_journal_paper_doi               10.1021/ic010482v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C60 H71 Cl2 O4 Ti'
_chemical_formula_weight         974.97
_chemical_name_systematic
;
?
;
_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                 95.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.639(4)
_cell_length_b                   20.152(4)
_cell_length_c                   12.750(3)
_cell_measurement_temperature    190(2)
_cell_volume                     5533(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46404
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.295
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          1.353
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1117P)²+1.5960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                7655
_reflns_number_total             9554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010482v_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5532.6(19)
_cod_database_code               4320692
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
Ti1 Ti 0.168432(19) 0.45602(2) 0.54942(3) 0.01782(14) Uani 1 1 d . . .
Cl1 Cl 0.10343(3) 0.51686(4) 0.65029(5) 0.03593(19) Uani 1 1 d . . .
Cl2 Cl 0.16834(4) 0.37013(4) 0.67538(6) 0.0456(2) Uani 1 1 d . . .
O1 O 0.09634(7) 0.41184(8) 0.45095(13) 0.0214(4) Uani 1 1 d . . .
O2 O 0.16413(8) 0.52404(8) 0.45681(13) 0.0219(4) Uani 1 1 d . . .
O3 O 0.24827(8) 0.50390(8) 0.62667(12) 0.0210(4) Uani 1 1 d . . .
O4 O 0.22120(8) 0.40837(8) 0.48125(14) 0.0239(4) Uani 1 1 d . . .
C1 C 0.04932(11) 0.52552(12) 0.3280(2) 0.0252(5) Uani 1 1 d . . .
H1A H 0.0126 0.5382 0.2797 0.030 Uiso 1 1 calc R . .
H1B H 0.0341 0.5114 0.3952 0.030 Uiso 1 1 calc R . .
C2 C 0.16401(12) 0.30286(12) 0.3639(2) 0.0254(5) Uani 1 1 d . . .
H2A H 0.1451 0.3008 0.4314 0.031 Uiso 1 1 calc R . .
H2B H 0.1545 0.2606 0.3261 0.031 Uiso 1 1 calc R . .
C3 C 0.22877(12) 0.63675(12) 0.5419(2) 0.0245(5) Uani 1 1 d . . .
H3A H 0.2448 0.6821 0.5571 0.029 Uiso 1 1 calc R . .
H3B H 0.2118 0.6201 0.6062 0.029 Uiso 1 1 calc R . .
C4 C 0.34468(12) 0.41550(12) 0.5690(2) 0.0245(5) Uani 1 1 d . . .
H4A H 0.3890 0.4068 0.5919 0.029 Uiso 1 1 calc R . .
H4B H 0.3212 0.4099 0.6312 0.029 Uiso 1 1 calc R . .
C5 C 0.04089(12) 0.37907(14) 0.4802(2) 0.0295(6) Uani 1 1 d . . .
H5A H 0.0041 0.4010 0.4449 0.044 Uiso 1 1 calc R . .
H5B H 0.0398 0.3817 0.5567 0.044 Uiso 1 1 calc R . .
H5C H 0.0413 0.3324 0.4586 0.044 Uiso 1 1 calc R . .
C6 C 0.26371(14) 0.51647(14) 0.7386(2) 0.0318(6) Uani 1 1 d . . .
H6A H 0.3071 0.5044 0.7586 0.048 Uiso 1 1 calc R . .
H6B H 0.2367 0.4899 0.7793 0.048 Uiso 1 1 calc R . .
H6C H 0.2577 0.5637 0.7532 0.048 Uiso 1 1 calc R . .
C10 C 0.10281(11) 0.41201(12) 0.34069(19) 0.0206(5) Uani 1 1 d . . .
C11 C 0.08004(11) 0.46611(12) 0.2807(2) 0.0223(5) Uani 1 1 d . . .
C12 C 0.13414(11) 0.35943(12) 0.2981(2) 0.0221(5) Uani 1 1 d . . .
C13 C 0.08540(12) 0.46432(13) 0.1726(2) 0.0265(5) Uani 1 1 d . . .
H13 H 0.0693 0.5003 0.1301 0.032 Uiso 1 1 calc R . .
C14 C 0.13806(12) 0.36038(13) 0.1899(2) 0.0262(5) Uani 1 1 d . . .
H14 H 0.1583 0.3246 0.1589 0.031 Uiso 1 1 calc R . .
C15 C 0.11361(12) 0.41148(14) 0.1247(2) 0.0279(6) Uani 1 1 d . . .
C16 C 0.11599(15) 0.40763(16) 0.0044(2) 0.0385(7) Uani 1 1 d . . .
C17 C 0.06674(19) 0.3585(2) -0.0413(3) 0.0663(12) Uani 1 1 d . . .
H17A H 0.0732 0.3156 -0.0057 0.100 Uiso 1 1 calc R . .
H17B H 0.0701 0.3529 -0.1169 0.100 Uiso 1 1 calc R . .
H17C H 0.0254 0.3754 -0.0308 0.100 Uiso 1 1 calc R . .
C18 C 0.1045(2) 0.4755(2) -0.0488(3) 0.0648(11) Uani 1 1 d . . .
H18A H 0.0627 0.4910 -0.0379 0.097 Uiso 1 1 calc R . .
H18B H 0.1081 0.4713 -0.1245 0.097 Uiso 1 1 calc R . .
H18C H 0.1353 0.5074 -0.0181 0.097 Uiso 1 1 calc R . .
C19 C 0.17953(17) 0.3823(2) -0.0205(3) 0.0551(9) Uani 1 1 d . . .
H19A H 0.2121 0.4114 0.0125 0.083 Uiso 1 1 calc R . .
H19B H 0.1813 0.3821 -0.0970 0.083 Uiso 1 1 calc R . .
H19C H 0.1859 0.3371 0.0069 0.083 Uiso 1 1 calc R . .
C20 C 0.14348(11) 0.58383(12) 0.42061(18) 0.0204(5) Uani 1 1 d . . .
C21 C 0.17626(11) 0.64065(12) 0.45383(19) 0.0224(5) Uani 1 1 d . . .
C22 C 0.08949(11) 0.58684(12) 0.34953(19) 0.0219(5) Uani 1 1 d . . .
C23 C 0.15655(12) 0.70155(12) 0.4098(2) 0.0264(5) Uani 1 1 d . . .
H23 H 0.1788 0.7406 0.4316 0.032 Uiso 1 1 calc R . .
C24 C 0.07194(12) 0.64831(13) 0.3076(2) 0.0267(6) Uani 1 1 d . . .
H24 H 0.0360 0.6510 0.2585 0.032 Uiso 1 1 calc R . .
C25 C 0.10523(12) 0.70679(13) 0.3350(2) 0.0285(6) Uani 1 1 d . . .
C26 C 0.08475(14) 0.77341(14) 0.2841(2) 0.0381(7) Uani 1 1 d . . .
C27 C 0.1214(3) 0.83139(18) 0.3359(5) 0.0926(19) Uani 1 1 d . . .
H27A H 0.1655 0.8258 0.3272 0.139 Uiso 1 1 calc R . .
H27B H 0.1157 0.8326 0.4112 0.139 Uiso 1 1 calc R . .
H27C H 0.1064 0.8730 0.3027 0.139 Uiso 1 1 calc R . .
C28 C 0.01569(19) 0.78511(19) 0.2928(4) 0.0640(11) Uani 1 1 d . . .
H28A H 0.0033 0.8277 0.2600 0.096 Uiso 1 1 calc R . .
H28B H 0.0080 0.7859 0.3672 0.096 Uiso 1 1 calc R . .
H28C H -0.0085 0.7493 0.2566 0.096 Uiso 1 1 calc R . .
C29 C 0.0951(2) 0.77098(19) 0.1673(3) 0.0627(11) Uani 1 1 d . . .
H29A H 0.0848 0.8142 0.1349 0.094 Uiso 1 1 calc R . .
H29B H 0.0684 0.7367 0.1320 0.094 Uiso 1 1 calc R . .
H29C H 0.1387 0.7605 0.1601 0.094 Uiso 1 1 calc R . .
C30 C 0.29133(11) 0.52891(12) 0.55936(19) 0.0208(5) Uani 1 1 d . . .
C31 C 0.28265(11) 0.59266(12) 0.51845(19) 0.0224(5) Uani 1 1 d . . .
C32 C 0.33806(11) 0.48704(12) 0.53145(19) 0.0225(5) Uani 1 1 d . . .
C33 C 0.32549(12) 0.61542(13) 0.4522(2) 0.0275(6) Uani 1 1 d . . .
H33 H 0.3209 0.6590 0.4242 0.033 Uiso 1 1 calc R . .
C34 C 0.37942(12) 0.51220(13) 0.4648(2) 0.0270(6) Uani 1 1 d . . .
H34 H 0.4119 0.4845 0.4454 0.032 Uiso 1 1 calc R . .
C35 C 0.37489(12) 0.57668(13) 0.4255(2) 0.0286(6) Uani 1 1 d . . .
C36 C 0.42283(13) 0.60594(16) 0.3566(3) 0.0394(7) Uani 1 1 d . . .
C37 C 0.46940(18) 0.5539(2) 0.3274(4) 0.0648(11) Uani 1 1 d . . .
H37A H 0.4472 0.5173 0.2897 0.097 Uiso 1 1 calc R . .
H37B H 0.4927 0.5369 0.3916 0.097 Uiso 1 1 calc R . .
H37C H 0.4982 0.5741 0.2820 0.097 Uiso 1 1 calc R . .
C38 C 0.45794(18) 0.6615(2) 0.4200(3) 0.0642(11) Uani 1 1 d . . .
H38A H 0.4901 0.6797 0.3793 0.096 Uiso 1 1 calc R . .
H38B H 0.4773 0.6436 0.4868 0.096 Uiso 1 1 calc R . .
H38C H 0.4288 0.6968 0.4345 0.096 Uiso 1 1 calc R . .
C39 C 0.38975(18) 0.6347(2) 0.2550(3) 0.0598(10) Uani 1 1 d . . .
H39A H 0.4204 0.6548 0.2130 0.090 Uiso 1 1 calc R . .
H39B H 0.3599 0.6685 0.2725 0.090 Uiso 1 1 calc R . .
H39C H 0.3678 0.5991 0.2143 0.090 Uiso 1 1 calc R . .
C40 C 0.25905(11) 0.36044(11) 0.45209(18) 0.0201(5) Uani 1 1 d . . .
C41 C 0.23404(12) 0.30899(12) 0.38752(19) 0.0226(5) Uani 1 1 d . . .
C42 C 0.32200(12) 0.36422(12) 0.48676(19) 0.0224(5) Uani 1 1 d . . .
C43 C 0.27492(12) 0.26307(13) 0.3519(2) 0.0275(6) Uani 1 1 d . . .
H43 H 0.2591 0.2282 0.3068 0.033 Uiso 1 1 calc R . .
C44 C 0.36124(12) 0.31713(13) 0.4491(2) 0.0264(6) Uani 1 1 d . . .
H44 H 0.4045 0.3194 0.4706 0.032 Uiso 1 1 calc R . .
C45 C 0.33899(13) 0.26684(13) 0.3808(2) 0.0300(6) Uani 1 1 d . . .
C46 C 0.38235(14) 0.21635(16) 0.3349(3) 0.0424(8) Uani 1 1 d . . .
C47 C 0.44970(18) 0.2233(3) 0.3860(4) 0.0869(18) Uani 1 1 d . . .
H47A H 0.4505 0.2181 0.4625 0.130 Uiso 1 1 calc R . .
H47B H 0.4657 0.2673 0.3699 0.130 Uiso 1 1 calc R . .
H47C H 0.4757 0.1891 0.3579 0.130 Uiso 1 1 calc R . .
C48 C 0.38142(19) 0.23022(19) 0.2170(3) 0.0596(10) Uani 1 1 d . . .
H48A H 0.4103 0.2002 0.1863 0.089 Uiso 1 1 calc R . .
H48B H 0.3940 0.2763 0.2064 0.089 Uiso 1 1 calc R . .
H48C H 0.3394 0.2231 0.1828 0.089 Uiso 1 1 calc R . .
C49 C 0.3594(2) 0.14593(16) 0.3522(3) 0.0566(10) Uani 1 1 d . . .
H49A H 0.3171 0.1409 0.3178 0.085 Uiso 1 1 calc R . .
H49B H 0.3594 0.1376 0.4279 0.085 Uiso 1 1 calc R . .
H49C H 0.3869 0.1140 0.3221 0.085 Uiso 1 1 calc R . .
C50 C 0.2050(4) 0.6062(4) 0.1522(7) 0.079(2) Uiso 0.70 1 d P A 1
C51 C 0.2499(3) 0.5466(3) 0.1427(4) 0.0512(12) Uiso 0.70 1 d P A 1
C52 C 0.2615(3) 0.4953(3) 0.2231(4) 0.0511(13) Uiso 0.70 1 d P A 1
H52 H 0.2394 0.4966 0.2838 0.061 Uiso 0.70 1 calc PR A 1
C53 C 0.2990(3) 0.4504(4) 0.2144(5) 0.0627(16) Uiso 0.70 1 d P A 1
H53 H 0.3046 0.4187 0.2696 0.075 Uiso 0.70 1 calc PR A 1
C54 C 0.3345(3) 0.4427(3) 0.1276(5) 0.0616(14) Uiso 0.70 1 d P A 1
H54 H 0.3634 0.4075 0.1241 0.074 Uiso 0.70 1 calc PR A 1
C55 C 0.3249(3) 0.4890(3) 0.0492(5) 0.0563(13) Uiso 0.70 1 d P A 1
H55 H 0.3476 0.4857 -0.0106 0.068 Uiso 0.70 1 calc PR A 1
C56 C 0.2821(3) 0.5412(4) 0.0548(5) 0.0493(14) Uiso 0.70 1 d P A 1
H56 H 0.2755 0.5724 -0.0011 0.059 Uiso 0.70 1 calc PR A 1
C50 C 0.3161(7) 0.4275(7) 0.1997(11) 0.052(3) Uiso 0.30 1 d P B 2
C51 C 0.2877(9) 0.4887(9) 0.1551(15) 0.084(5) Uiso 0.30 1 d P B 2
C52 C 0.2992(7) 0.5175(8) 0.0578(9) 0.042(3) Uiso 0.30 1 d P B 2
H52A H 0.3264 0.4974 0.0131 0.050 Uiso 0.30 1 calc PR B 2
C53 C 0.2682(9) 0.5780(10) 0.0302(15) 0.084(5) Uiso 0.30 1 d P B 2
H53A H 0.2755 0.5967 -0.0358 0.101 Uiso 0.30 1 calc PR B 2
C54 C 0.2290(9) 0.6123(10) 0.0879(16) 0.090(5) Uiso 0.30 1 d P B 2
H54A H 0.2093 0.6527 0.0652 0.108 Uiso 0.30 1 calc PR B 2
C55 C 0.2214(8) 0.5826(8) 0.1815(13) 0.066(4) Uiso 0.30 1 d P B 2
H55A H 0.1954 0.6043 0.2266 0.079 Uiso 0.30 1 calc PR B 2
C56 C 0.2486(4) 0.5225(5) 0.2169(8) 0.029(2) Uiso 0.30 1 d P B 2
H56A H 0.2404 0.5049 0.2832 0.034 Uiso 0.30 1 calc PR B 2
C60 C 0.4758(11) 0.5765(11) 0.909(2) 0.407(14) Uiso 1 1 d D . .
H60A H 0.5055 0.6034 0.9542 0.610 Uiso 1 1 calc R . .
H60B H 0.4982 0.5496 0.8615 0.610 Uiso 1 1 calc R . .
H60C H 0.4531 0.5473 0.9536 0.610 Uiso 1 1 calc R . .
C61 C 0.3698(4) 0.6744(4) 0.7454(8) 0.143(3) Uiso 1 1 d D . .
H61 H 0.3633 0.6913 0.6756 0.171 Uiso 1 1 calc R . .
C62 C 0.3246(6) 0.7009(6) 0.7978(10) 0.192(4) Uiso 1 1 d D . .
H62 H 0.2901 0.7260 0.7679 0.230 Uiso 1 1 calc R . .
C63 C 0.3380(6) 0.6848(6) 0.9037(11) 0.209(5) Uiso 1 1 d D . .
H63 H 0.3127 0.6977 0.9571 0.250 Uiso 1 1 calc R . .
C64 C 0.3957(5) 0.6453(5) 0.9247(8) 0.153(3) Uiso 1 1 d D . .
H64 H 0.4094 0.6361 0.9963 0.183 Uiso 1 1 calc R . .
C65 C 0.4320(10) 0.6200(10) 0.8480(17) 0.285(8) Uiso 1 1 d D . .
C66 C 0.4169(6) 0.6371(6) 0.7473(11) 0.188(4) Uiso 1 1 d D . .
H66 H 0.4376 0.6237 0.6884 0.226 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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 94.82(8) . . ?
O4 Ti1 O1 87.36(7) . . ?
O2 Ti1 O1 86.77(7) . . ?
O4 Ti1 O3 86.57(7) . . ?
O2 Ti1 O3 86.88(7) . . ?
O1 Ti1 O3 170.81(7) . . ?
O4 Ti1 Cl1 175.90(6) . . ?
O2 Ti1 Cl1 88.10(6) . . ?
O1 Ti1 Cl1 95.69(5) . . ?
O3 Ti1 Cl1 90.73(5) . . ?
O4 Ti1 Cl2 88.88(7) . . ?
O2 Ti1 Cl2 176.21(6) . . ?
O1 Ti1 Cl2 92.59(5) . . ?
O3 Ti1 Cl2 94.17(5) . . ?
Cl1 Ti1 Cl2 88.24(4) . . ?
C10 O1 C5 114.74(18) . . ?
C10 O1 Ti1 116.64(13) . . ?
C5 O1 Ti1 128.59(15) . . ?
C20 O2 Ti1 153.48(16) . . ?
C30 O3 C6 115.48(18) . . ?
C30 O3 Ti1 115.56(13) . . ?
C6 O3 Ti1 128.93(15) . . ?
C40 O4 Ti1 163.82(16) . . ?
C22 C1 C11 116.5(2) . . ?
C41 C2 C12 114.2(2) . . ?
C31 C3 C21 114.7(2) . . ?
C42 C4 C32 114.5(2) . . ?
C11 C10 C12 122.7(2) . . ?
C11 C10 O1 118.6(2) . . ?
C12 C10 O1 118.7(2) . . ?
C10 C11 C13 117.5(2) . . ?
C10 C11 C1 122.9(2) . . ?
C13 C11 C1 119.6(2) . . ?
C14 C12 C10 117.0(2) . . ?
C14 C12 C2 119.5(2) . . ?
C10 C12 C2 123.4(2) . . ?
C11 C13 C15 122.3(2) . . ?
C12 C14 C15 123.0(2) . . ?
C14 C15 C13 117.3(2) . . ?
C14 C15 C16 120.5(2) . . ?
C13 C15 C16 122.2(2) . . ?
C17 C16 C19 108.1(3) . . ?
C17 C16 C18 109.4(3) . . ?
C19 C16 C18 108.4(3) . . ?
C17 C16 C15 108.8(3) . . ?
C19 C16 C15 110.1(2) . . ?
C18 C16 C15 112.0(3) . . ?
O2 C20 C21 119.3(2) . . ?
O2 C20 C22 119.0(2) . . ?
C21 C20 C22 121.8(2) . . ?
C20 C21 C23 118.3(2) . . ?
C20 C21 C3 120.3(2) . . ?
C23 C21 C3 121.2(2) . . ?
C24 C22 C20 117.7(2) . . ?
C24 C22 C1 121.8(2) . . ?
C20 C22 C1 120.3(2) . . ?
C25 C23 C21 122.1(2) . . ?
C22 C24 C25 122.6(2) . . ?
C23 C25 C24 117.4(2) . . ?
C23 C25 C26 122.1(2) . . ?
C24 C25 C26 120.5(2) . . ?
C27 C26 C29 109.1(4) . . ?
C27 C26 C28 108.7(3) . . ?
C29 C26 C28 108.3(3) . . ?
C27 C26 C25 111.8(3) . . ?
C29 C26 C25 108.6(3) . . ?
C28 C26 C25 110.3(3) . . ?
C32 C30 C31 122.6(2) . . ?
C32 C30 O3 118.5(2) . . ?
C31 C30 O3 118.8(2) . . ?
C33 C31 C30 117.3(2) . . ?
C33 C31 C3 119.8(2) . . ?
C30 C31 C3 122.9(2) . . ?
C34 C32 C30 117.6(2) . . ?
C34 C32 C4 119.5(2) . . ?
C30 C32 C4 122.9(2) . . ?
C31 C33 C35 122.5(2) . . ?
C32 C34 C35 122.3(2) . . ?
C34 C35 C33 117.6(2) . . ?
C34 C35 C36 122.3(2) . . ?
C33 C35 C36 120.1(2) . . ?
C37 C36 C39 108.5(3) . . ?
C37 C36 C38 109.0(3) . . ?
C39 C36 C38 109.6(3) . . ?
C37 C36 C35 112.0(3) . . ?
C39 C36 C35 110.0(2) . . ?
C38 C36 C35 107.7(3) . . ?
O4 C40 C42 118.5(2) . . ?
O4 C40 C41 119.0(2) . . ?
C42 C40 C41 122.5(2) . . ?
C43 C41 C40 117.7(2) . . ?
C43 C41 C2 122.4(2) . . ?
C40 C41 C2 119.8(2) . . ?
C44 C42 C40 117.7(2) . . ?
C44 C42 C4 122.4(2) . . ?
C40 C42 C4 119.7(2) . . ?
C41 C43 C45 121.6(2) . . ?
C42 C44 C45 121.9(2) . . ?
C44 C45 C43 118.4(2) . . ?
C44 C45 C46 122.3(2) . . ?
C43 C45 C46 119.3(2) . . ?
C48 C46 C49 109.9(3) . . ?
C48 C46 C45 107.7(3) . . ?
C49 C46 C45 109.9(3) . . ?
C48 C46 C47 108.6(4) . . ?
C49 C46 C47 109.3(3) . . ?
C45 C46 C47 111.4(2) . . ?
C56 C51 C52 116.7(5) . . ?
C56 C51 C50 119.5(6) . . ?
C52 C51 C50 123.8(6) . . ?
C53 C52 C51 121.9(6) . . ?
C52 C53 C54 124.4(7) . . ?
C55 C54 C53 116.2(6) . . ?
C54 C55 C56 121.8(6) . . ?
C51 C56 C55 119.1(6) . . ?
C56 C51 C52 117.7(16) . . ?
C56 C51 C50 116.5(16) . . ?
C52 C51 C50 125.7(16) . . ?
C53 C52 C51 116.8(16) . . ?
C54 C53 C52 127.3(19) . . ?
C53 C54 C55 112.7(19) . . ?
C54 C55 C56 125.4(16) . . ?
C55 C56 C51 120.1(13) . . ?
C66 C61 C62 148.1(13) . . ?
C66 C61 C65 37.7(8) . . ?
C62 C61 C65 110.6(10) . . ?
C61 C62 C63 107.3(12) . . ?
C62 C63 C64 113.0(13) . . ?
C65 C64 C63 125.9(14) . . ?
C64 C65 C66 118.2(18) . . ?
C64 C65 C60 102.8(19) . . ?
C66 C65 C60 139(2) . . ?
C64 C65 C61 82.8(12) . . ?
C66 C65 C61 35.3(9) . . ?
C60 C65 C61 173.2(18) . . ?
C61 C66 C65 106.9(15) . . ?
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 1.7828(17) . ?
Ti1 O2 1.8055(17) . ?
Ti1 O1 2.1010(17) . ?
Ti1 O3 2.1327(17) . ?
Ti1 Cl1 2.3439(9) . ?
Ti1 Cl2 2.3613(8) . ?
O1 C10 1.427(3) . ?
O1 C5 1.450(3) . ?
O2 C20 1.350(3) . ?
O3 C30 1.420(3) . ?
O3 C6 1.455(3) . ?
O4 C40 1.342(3) . ?
C1 C22 1.520(4) . ?
C1 C11 1.523(3) . ?
C2 C41 1.521(4) . ?
C2 C12 1.521(4) . ?
C3 C31 1.519(4) . ?
C3 C21 1.518(3) . ?
C4 C42 1.518(3) . ?
C4 C32 1.521(3) . ?
C10 C11 1.393(4) . ?
C10 C12 1.396(3) . ?
C11 C13 1.396(4) . ?
C12 C14 1.392(4) . ?
C13 C15 1.398(4) . ?
C14 C15 1.394(4) . ?
C15 C16 1.541(4) . ?
C16 C17 1.528(5) . ?
C16 C19 1.530(5) . ?
C16 C18 1.536(5) . ?
C20 C21 1.391(4) . ?
C20 C22 1.407(3) . ?
C21 C23 1.398(4) . ?
C22 C24 1.387(4) . ?
C23 C25 1.395(4) . ?
C24 C25 1.407(4) . ?
C25 C26 1.537(4) . ?
C26 C27 1.525(5) . ?
C26 C29 1.529(5) . ?
C26 C28 1.528(5) . ?
C30 C32 1.390(4) . ?
C30 C31 1.392(3) . ?
C31 C33 1.392(4) . ?
C32 C34 1.390(4) . ?
C33 C35 1.393(4) . ?
C34 C35 1.393(4) . ?
C35 C36 1.541(4) . ?
C36 C37 1.526(5) . ?
C36 C39 1.531(5) . ?
C36 C38 1.538(5) . ?
C40 C42 1.392(4) . ?
C40 C41 1.399(3) . ?
C41 C43 1.387(4) . ?
C42 C44 1.390(4) . ?
C43 C45 1.401(4) . ?
C44 C45 1.391(4) . ?
C45 C46 1.538(4) . ?
C46 C48 1.526(5) . ?
C46 C49 1.527(5) . ?
C46 C47 1.543(5) . ?
C50 C51 1.557(10) . ?
C51 C56 1.381(8) . ?
C51 C52 1.460(8) . ?
C52 C53 1.227(9) . ?
C53 C54 1.417(9) . ?
C54 C55 1.367(8) . ?
C55 C56 1.408(8) . ?
C50 C51 1.47(2) . ?
C51 C56 1.39(2) . ?
C51 C52 1.41(2) . ?
C52 C53 1.42(2) . ?
C53 C54 1.36(3) . ?
C54 C55 1.36(3) . ?
C55 C56 1.40(2) . ?
C60 C65 1.46(2) . ?
C61 C66 1.265(12) . ?
C61 C62 1.347(13) . ?
C61 C65 2.09(2) . ?
C62 C63 1.392(14) . ?
C63 C64 1.483(14) . ?
C64 C65 1.409(18) . ?
C65 C66 1.339(19) . ?
