# Copyright The Royal Society of Chemistry, 1998

# MANUSCRIPT 8/03864C 


# CIF for the paper entitled:
# A novel titanium-oxygen ladder structure supported by calix-4-arene
# ligands, characterised by synchrotron crystallography
#
# by W. Clegg, M. R. J. Elsegood, S. J. Teat, C. Redshaw and V. C. 
# Gibson


data_vcg129

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C102 H120 Cl4 O10 Ti4'
_chemical_formula_weight          1839.38

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'

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    12.5692(14)
_cell_length_b                    13.4268(15)
_cell_length_c                    15.4275(17)
_cell_angle_alpha                 89.299(3)
_cell_angle_beta                  68.935(3)
_cell_angle_gamma                 85.043(3)
_cell_volume                      2420.0(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     8219
_cell_measurement_theta_min       1.69
_cell_measurement_theta_max       26.98

_exptl_crystal_description        plate
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.262
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              968
_exptl_absorpt_coefficient_mu     0.484
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.564
_exptl_absorpt_correction_T_max   0.978

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       160(2)
_diffrn_radiation_wavelength      0.6879
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator   'silicon 111'
_diffrn_measurement_device_type   'Siemens SMART CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         30
_diffrn_reflns_number             11915
_diffrn_reflns_av_R_equivalents   0.0424
_diffrn_reflns_av_sigmaI/netI     0.1058
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.69
_diffrn_reflns_theta_max          27.06
_reflns_number_total              9287
_reflns_number_gt                 6241
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_computing_structure_solution     'Siemens SHELXTL'
_computing_structure_refinement   'Siemens SHELXTL'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'SHELXTL and local programs'

_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is
 not relevant to the choice of reflections for refinement.  R-factors 
based
 on F^2^ are statistically about twice as large as those based on F, and 
R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0040(10)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          9287
_refine_ls_number_parameters      579
_refine_ls_number_restraints      90
_refine_ls_R_factor_all           0.0822
_refine_ls_R_factor_gt            0.0595
_refine_ls_wR_factor_ref          0.1498
_refine_ls_wR_factor_gt           0.1428
_refine_ls_goodness_of_fit_ref    0.925
_refine_ls_restrained_S_all       0.926
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

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_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ti1 Ti 1.09711(5) 0.35386(4) 0.33604(4) 0.01277(16) Uani 1 d . . .
Ti2 Ti 0.96463(5) 0.56453(4) 0.42711(4) 0.01034(15) Uani 1 d . . .
Cl1 Cl 0.98640(8) 0.26282(6) 0.28919(7) 0.0250(2) Uani 1 d . . .
Cl2 Cl 1.26137(8) 0.37721(6) 0.22059(7) 0.0241(2) Uani 1 d . . .
O1 O 1.0379(2) 0.43301(16) 0.44574(15) 0.0148(5) Uani 1 d . . .
O2 O 0.81483(19) 0.57920(16) 0.45093(16) 0.0143(5) Uani 1 d . . .
O3 O 1.0179(2) 0.49007(15) 0.30738(15) 0.0124(5) Uani 1 d . . .
O4 O 1.0402(2) 0.67160(16) 0.38485(16) 0.0142(5) Uani 1 d . . .
O5 O 0.8489(2) 0.74032(16) 0.60569(16) 0.0144(5) Uani 1 d . . .
C1 C 0.7097(3) 0.5896(2) 0.4412(2) 0.0146(7) Uani 1 d . . .
C2 C 0.6205(3) 0.6514(2) 0.5027(2) 0.0154(7) Uani 1 d . . .
C3 C 0.5182(3) 0.6639(2) 0.4870(3) 0.0180(8) Uani 1 d . . .
H3 H 0.4564 0.7055 0.5287 0.022 Uiso 1 calc R . .
C4 C 0.5024(3) 0.6180(3) 0.4124(3) 0.0191(8) Uani 1 d . . .
C5 C 0.5915(3) 0.5523(3) 0.3561(3) 0.0196(8) Uani 1 d . . .
H5 H 0.5811 0.5171 0.3072 0.024 Uiso 1 calc R . .
C6 C 0.6958(3) 0.5366(2) 0.3694(2) 0.0156(7) Uani 1 d . . .
C7 C 0.3966(3) 0.6475(3) 0.3866(3) 0.0228(8) Uani 1 d . . .
C8 C 0.3758(4) 0.5672(3) 0.3273(4) 0.0445(13) Uani 1 d . . .
H8A H 0.4386 0.5617 0.2668 0.067 Uiso 1 calc R . .
H8B H 0.3034 0.5852 0.3182 0.067 Uiso 1 calc R . .
H8C H 0.3721 0.5029 0.3586 0.067 Uiso 1 calc R . .
C9 C 0.4191(4) 0.7440(3) 0.3319(3) 0.0377(11) Uani 1 d . . .
H9A H 0.4850 0.7311 0.2740 0.057 Uiso 1 calc R . .
H9B H 0.4351 0.7951 0.3691 0.057 Uiso 1 calc R . .
H9C H 0.3515 0.7675 0.3173 0.057 Uiso 1 calc R . .
C10 C 0.2874(3) 0.6659(3) 0.4738(3) 0.0331(10) Uani 1 d . . .
H10A H 0.2224 0.6875 0.4551 0.050 Uiso 1 calc R . .
H10B H 0.2981 0.7181 0.5131 0.050 Uiso 1 calc R . .
H10C H 0.2723 0.6040 0.5087 0.050 Uiso 1 calc R . .
C11 C 0.7934(3) 0.4700(2) 0.3026(2) 0.0173(8) Uani 1 d . . .
H11A H 0.8314 0.4277 0.3379 0.021 Uiso 1 calc R . .
H11B H 0.7629 0.4253 0.2683 0.021 Uiso 1 calc R . .
C12 C 0.9875(3) 0.5420(2) 0.2403(2) 0.0135(7) Uani 1 d . . .
C13 C 0.8796(3) 0.5314(2) 0.2346(2) 0.0159(7) Uani 1 d . . .
C14 C 0.8503(3) 0.5854(3) 0.1681(2) 0.0190(8) Uani 1 d . . .
H14 H 0.7782 0.5776 0.1633 0.023 Uiso 1 calc R . .
C15 C 0.9204(3) 0.6500(3) 0.1087(2) 0.0196(8) Uani 1 d . . .
C16 C 1.0248(3) 0.6619(2) 0.1184(2) 0.0191(8) Uani 1 d . . .
H16 H 1.0740 0.7071 0.0792 0.023 Uiso 1 calc R . .
C17 C 1.0587(3) 0.6096(2) 0.1837(2) 0.0153(7) Uani 1 d . . .
C18 C 0.8835(4) 0.7037(3) 0.0341(3) 0.0296(10) Uani 1 d . . .
C19 C 0.7615(4) 0.7561(4) 0.0802(4) 0.0604(16) Uani 1 d . . .
H19A H 0.7372 0.7891 0.0325 0.091 Uiso 1 calc R . .
H19B H 0.7616 0.8061 0.1259 0.091 Uiso 1 calc R . .
H19C H 0.7084 0.7064 0.1113 0.091 Uiso 1 calc R . .
C20 C 0.9627(5) 0.7829(4) -0.0158(4) 0.0613(17) Uani 1 d . . .
H20A H 1.0381 0.7504 -0.0526 0.092 Uiso 1 calc R . .
H20B H 0.9703 0.8288 0.0301 0.092 Uiso 1 calc R . .
H20C H 0.9304 0.8204 -0.0568 0.092 Uiso 1 calc R . .
C21 C 0.8812(6) 0.6263(4) -0.0363(3) 0.0593(16) Uani 1 d . . .
H21A H 0.8549 0.6593 -0.0828 0.089 Uiso 1 calc R . .
H21B H 0.8289 0.5763 -0.0044 0.089 Uiso 1 calc R . .
H21C H 0.9584 0.5934 -0.0669 0.089 Uiso 1 calc R . .
C22 C 1.1714(3) 0.6297(2) 0.1934(2) 0.0161(7) Uani 1 d . . .
H22A H 1.1931 0.5756 0.2296 0.019 Uiso 1 calc R . .
H22B H 1.2319 0.6282 0.1308 0.019 Uiso 1 calc R . .
C23 C 1.1018(3) 0.7459(2) 0.3346(2) 0.0136(7) Uani 1 d . . .
C24 C 1.1661(3) 0.7293(2) 0.2406(2) 0.0152(7) Uani 1 d . . .
C25 C 1.2270(3) 0.8064(3) 0.1917(3) 0.0195(8) Uani 1 d . . .
H25 H 1.2697 0.7967 0.1272 0.023 Uiso 1 calc R . .
C26 C 1.2276(3) 0.8977(3) 0.2341(3) 0.0214(8) Uani 1 d . . .
C27 C 1.1635(3) 0.9105(2) 0.3278(3) 0.0183(8) Uani 1 d . . .
H27 H 1.1633 0.9719 0.3577 0.022 Uiso 1 calc R . .
C28 C 1.0993(3) 0.8366(2) 0.3798(2) 0.0152(7) Uani 1 d . . .
C29 C 1.2987(4) 0.9798(3) 0.1779(3) 0.0326(10) Uani 1 d . . .
C30 C 1.2815(7) 1.0743(4) 0.2323(5) 0.106(3) Uani 1 d . . .
H30A H 1.3162 1.0643 0.2797 0.158 Uiso 1 calc R . .
H30B H 1.1994 1.0935 0.2624 0.158 Uiso 1 calc R . .
H30C H 1.3175 1.1273 0.1906 0.158 Uiso 1 calc R . .
C31 C 1.4243(5) 0.9416(4) 0.1404(4) 0.0630(17) Uani 1 d . . .
H31A H 1.4694 0.9931 0.1025 0.095 Uiso 1 calc R . .
H31B H 1.4348 0.8812 0.1022 0.095 Uiso 1 calc R . .
H31C H 1.4499 0.9257 0.1924 0.095 Uiso 1 calc R . .
C32 C 1.2659(7) 1.0014(5) 0.0910(5) 0.100(3) Uani 1 d . . .
H32A H 1.1864 1.0306 0.1108 0.151 Uiso 1 calc R . .
H32B H 1.2739 0.9389 0.0563 0.151 Uiso 1 calc R . .
H32C H 1.3166 1.0484 0.0512 0.151 Uiso 1 calc R . .
C33 C 1.0229(3) 0.8545(2) 0.4803(2) 0.0169(8) Uani 1 d . . .
H33A H 1.0399 0.9171 0.5040 0.020 Uiso 1 calc R . .
H33B H 1.0371 0.7987 0.5183 0.020 Uiso 1 calc R . .
C34 C 0.8207(3) 0.7990(2) 0.5432(2) 0.0135(7) Uani 1 d . . .
C35 C 0.8988(3) 0.8623(2) 0.4874(2) 0.0148(7) Uani 1 d . . .
C36 C 0.8656(3) 0.9248(2) 0.4279(3) 0.0180(8) Uani 1 d . . .
H36 H 0.9180 0.9691 0.3909 0.022 Uiso 1 calc R . .
C37 C 0.7579(3) 0.9253(2) 0.4201(3) 0.0192(8) Uani 1 d . . .
C38 C 0.6851(3) 0.8577(2) 0.4736(3) 0.0190(8) Uani 1 d . . .
H38 H 0.6124 0.8551 0.4683 0.023 Uiso 1 calc R . .
C39 C 0.7141(3) 0.7936(2) 0.5348(2) 0.0151(7) Uani 1 d . . .
C40 C 0.7266(4) 0.9935(3) 0.3517(3) 0.0343(8) Uani 1 d DU . .
C41 C 0.8233(6) 0.9869(5) 0.2563(4) 0.0509(13) Uani 0.816(5) d PDU A 1
H41A H 0.8015 1.0309 0.2132 0.076 Uiso 0.816(5) calc PR A 1
H41B H 0.8370 0.9178 0.2324 0.076 Uiso 0.816(5) calc PR A 1
H41C H 0.8933 1.0076 0.2622 0.076 Uiso 0.816(5) calc PR A 1
C42 C 0.7107(6) 1.1019(4) 0.3886(5) 0.0466(13) Uani 0.816(5) d PDU A 1
H42A H 0.6901 1.1471 0.3457 0.070 Uiso 0.816(5) calc PR A 1
H42B H 0.7823 1.1197 0.3936 0.070 Uiso 0.816(5) calc PR A 1
H42C H 0.6497 1.1079 0.4499 0.070 Uiso 0.816(5) calc PR A 1
C43 C 0.6162(5) 0.9702(5) 0.3393(5) 0.0516(14) Uani 0.816(5) d PDU A 1
H43A H 0.6007 1.0163 0.2947 0.077 Uiso 0.816(5) calc PR A 1
H43B H 0.5527 0.9780 0.3991 0.077 Uiso 0.816(5) calc PR A 1
H43C H 0.6245 0.9013 0.3159 0.077 Uiso 0.816(5) calc PR A 1
C41A C 0.714(2) 0.9246(16) 0.2772(16) 0.046(3) Uani 0.184(5) d PDU A 2
H41D H 0.6941 0.9652 0.2314 0.069 Uiso 0.184(5) calc PR A 2
H41E H 0.6544 0.8799 0.3067 0.069 Uiso 0.184(5) calc PR A 2
H41F H 0.7873 0.8846 0.2461 0.069 Uiso 0.184(5) calc PR A 2
C42A C 0.8118(19) 1.0696(16) 0.3070(17) 0.043(3) Uani 0.184(5) d PDU A 2
H42D H 0.7855 1.1103 0.2642 0.064 Uiso 0.184(5) calc PR A 2
H42E H 0.8868 1.0347 0.2725 0.064 Uiso 0.184(5) calc PR A 2
H42F H 0.8181 1.1129 0.3553 0.064 Uiso 0.184(5) calc PR A 2
C43A C 0.6044(15) 1.0471(17) 0.4010(16) 0.044(3) Uani 0.184(5) d PDU A 2
H43D H 0.5840 1.0907 0.3570 0.067 Uiso 0.184(5) calc PR A 2
H43E H 0.6037 1.0872 0.4539 0.067 Uiso 0.184(5) calc PR A 2
H43F H 0.5490 0.9969 0.4231 0.067 Uiso 0.184(5) calc PR A 2
C44 C 0.6381(3) 0.7112(2) 0.5788(2) 0.0164(7) Uani 1 d . . .
H44A H 0.5634 0.7405 0.6226 0.020 Uiso 1 calc R . .
H44B H 0.6744 0.6669 0.6140 0.020 Uiso 1 calc R . .
C45 C 1.4999(5) 0.6446(4) 0.0174(5) 0.0678(17) Uani 1 d . . .
H45A H 1.5810 0.6300 -0.0205 0.102 Uiso 1 calc R . .
H45B H 1.4702 0.5849 0.0518 0.102 Uiso 1 calc R . .
H45C H 1.4913 0.6995 0.0614 0.102 Uiso 1 calc R . .
C46 C 1.4347(4) 0.6741(4) -0.0437(4) 0.0456(12) Uani 1 d . . .
C47 C 1.4497(5) 0.7621(4) -0.0925(4) 0.0637(16) Uani 1 d . . .
H47 H 1.5044 0.8043 -0.0878 0.076 Uiso 1 calc R . .
C48 C 1.3868(7) 0.7909(5) -0.1485(5) 0.084(2) Uani 1 d . . .
H48 H 1.3993 0.8514 -0.1819 0.101 Uiso 1 calc R . .
C49 C 1.3072(7) 0.7310(5) -0.1548(4) 0.077(2) Uani 1 d . . .
H49 H 1.2630 0.7505 -0.1918 0.092 Uiso 1 calc R . .
C50 C 1.2908(5) 0.6432(4) -0.1080(4) 0.0577(15) Uani 1 d . . .
H50 H 1.2358 0.6017 -0.1130 0.069 Uiso 1 calc R . .
C51 C 1.3539(5) 0.6146(4) -0.0535(3) 0.0471(13) Uani 1 d . . .
H51 H 1.3420 0.5530 -0.0219 0.057 Uiso 1 calc R . .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ti1 0.0134(4) 0.0091(3) 0.0190(3) -0.0001(2) -0.0098(3) -0.0005(2)
Ti2 0.0091(3) 0.0075(3) 0.0180(3) 0.0013(2) -0.0091(3) -0.0018(2)
Cl1 0.0284(6) 0.0159(4) 0.0417(6) -0.0020(4) -0.0250(5) -0.0046(4)
Cl2 0.0184(5) 0.0218(4) 0.0290(5) 0.0032(4) -0.0055(4) 0.0014(4)
O1 0.0188(14) 0.0114(11) 0.0194(12) 0.0002(9) -0.0137(11) 0.0017(10)
O2 0.0068(13) 0.0149(11) 0.0255(13) -0.0006(10) -0.0108(11) -0.0015(9)
O3 0.0148(13) 0.0101(11) 0.0165(12) 0.0012(9) -0.0107(11) -0.0016(9)
O4 0.0119(13) 0.0109(11) 0.0211(13) 0.0020(9) -0.0066(11) -0.0051(9)
O5 0.0144(13) 0.0088(10) 0.0225(13) 0.0019(9) -0.0102(11) 0.0006(9)
C1 0.0083(19) 0.0110(15) 0.030(2) 0.0071(14) -0.0132(16) -0.0028(13)
C2 0.0131(19) 0.0111(15) 0.0260(19) 0.0047(14) -0.0112(17) -0.0040(13)
C3 0.0089(19) 0.0150(17) 0.030(2) 0.0033(14) -0.0074(17) -0.0006(13)
C4 0.012(2) 0.0187(17) 0.032(2) 0.0092(15) -0.0126(18) -0.0072(14)
C5 0.017(2) 0.0178(17) 0.032(2) 0.0032(15) -0.0183(18) -0.0061(15)
C6 0.0099(19) 0.0149(16) 0.0261(19) 0.0050(14) -0.0109(16) -0.0038(13)
C7 0.018(2) 0.0213(18) 0.037(2) 0.0072(16) -0.0179(19) -0.0039(15)
C8 0.035(3) 0.039(2) 0.079(4) -0.012(2) -0.046(3) 0.005(2)
C9 0.021(2) 0.039(2) 0.061(3) 0.031(2) -0.024(2) -0.0104(19)
C10 0.014(2) 0.042(2) 0.047(3) 0.014(2) -0.016(2) -0.0055(18)
C11 0.016(2) 0.0138(16) 0.0255(19) -0.0003(14) -0.0111(17) -0.0032(14)
C12 0.0137(19) 0.0109(15) 0.0196(18) 0.0014(13) -0.0104(16) -0.0019(13)
C13 0.015(2) 0.0133(16) 0.0220(18) 0.0002(13) -0.0089(16) -0.0032(14)
C14 0.015(2) 0.0213(18) 0.027(2) 0.0008(15) -0.0151(17) -0.0024(15)
C15 0.024(2) 0.0189(17) 0.0226(19) 0.0017(14) -0.0164(18) -0.0014(15)
C16 0.022(2) 0.0159(17) 0.0215(19) 0.0052(14) -0.0096(17) -0.0056(15)
C17 0.015(2) 0.0133(16) 0.0205(18) -0.0011(13) -0.0091(16) -0.0017(13)
C18 0.034(3) 0.029(2) 0.035(2) 0.0113(18) -0.024(2) -0.0040(18)
C19 0.049(4) 0.063(3) 0.074(4) 0.024(3) -0.034(3) 0.016(3)
C20 0.068(4) 0.067(4) 0.074(4) 0.051(3) -0.053(3) -0.027(3)
C21 0.102(5) 0.055(3) 0.042(3) 0.006(2) -0.053(3) -0.002(3)
C22 0.0122(19) 0.0155(16) 0.0226(19) 0.0020(14) -0.0083(16) -0.0038(14)
C23 0.0102(19) 0.0104(15) 0.0234(19) 0.0070(13) -0.0093(16) -0.0051(13)
C24 0.0106(19) 0.0148(16) 0.0254(19) 0.0048(14) -0.0122(17) -0.0041(13)
C25 0.015(2) 0.0192(17) 0.025(2) 0.0064(15) -0.0066(17) -0.0046(14)
C26 0.016(2) 0.0146(17) 0.035(2) 0.0062(15) -0.0101(18) -0.0035(14)
C27 0.014(2) 0.0091(15) 0.034(2) 0.0028(14) -0.0103(18) -0.0038(13)
C28 0.0098(19) 0.0127(15) 0.0273(19) 0.0037(14) -0.0116(16) -0.0023(13)
C29 0.031(3) 0.0149(18) 0.042(3) 0.0098(17) -0.001(2) -0.0078(17)
C30 0.135(7) 0.032(3) 0.084(5) -0.009(3) 0.049(5) -0.048(4)
C31 0.041(4) 0.041(3) 0.092(5) 0.012(3) -0.001(3) -0.021(2)
C32 0.135(7) 0.080(5) 0.113(6) 0.073(4) -0.068(5) -0.056(5)
C33 0.015(2) 0.0110(16) 0.029(2) 0.0017(14) -0.0138(17) -0.0047(14)
C34 0.0123(19) 0.0067(14) 0.0226(18) -0.0008(13) -0.0078(16) 0.0002(13)
C35 0.0137(19) 0.0092(15) 0.0230(19) -0.0037(13) -0.0084(16) -0.0005(13)
C36 0.018(2) 0.0102(15) 0.027(2) 0.0031(14) -0.0088(17) -0.0055(14)
C37 0.020(2) 0.0139(16) 0.029(2) 0.0035(14) -0.0148(18) -0.0026(14)
C38 0.014(2) 0.0153(17) 0.031(2) 0.0027(15) -0.0113(17) -0.0022(14)
C39 0.0126(19) 0.0123(16) 0.0215(18) -0.0009(13) -0.0071(16) -0.0017(13)
C40 0.039(2) 0.0272(16) 0.050(2) 0.0169(16) -0.0315(17) -0.0064(16)
C41 0.057(3) 0.059(3) 0.044(2) 0.018(2) -0.0294(19) 0.001(3)
C42 0.057(3) 0.0235(19) 0.067(3) 0.0179(19) -0.032(3) -0.004(2)
C43 0.055(3) 0.050(3) 0.077(4) 0.035(3) -0.055(3) -0.018(2)
C41A 0.058(6) 0.045(5) 0.053(5) 0.015(4) -0.040(4) -0.014(4)
C42A 0.050(5) 0.035(5) 0.057(6) 0.024(4) -0.033(4) -0.013(4)
C43A 0.042(3) 0.038(5) 0.065(5) 0.021(4) -0.035(5) 0.001(3)
C44 0.0097(19) 0.0172(17) 0.0227(19) 0.0029(14) -0.0061(16) -0.0032(14)
C45 0.053(4) 0.060(4) 0.098(5) -0.007(3) -0.037(4) 0.003(3)
C46 0.034(3) 0.047(3) 0.050(3) -0.004(2) -0.009(3) -0.001(2)
C47 0.059(4) 0.055(3) 0.072(4) 0.010(3) -0.014(3) -0.025(3)
C48 0.118(6) 0.066(4) 0.084(5) 0.044(4) -0.047(5) -0.041(4)
C49 0.106(6) 0.070(4) 0.070(4) 0.019(3) -0.050(4) -0.018(4)
C50 0.081(5) 0.055(3) 0.047(3) 0.002(3) -0.031(3) -0.022(3)
C51 0.058(4) 0.032(2) 0.046(3) -0.001(2) -0.011(3) -0.007(2)

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are 
taken
 into account individually in the estimation of esds in distances, 
angles
 and torsion angles; correlations between esds in cell parameters are 
only
 used when they are defined by crystal symmetry.  An approximate 
(isotropic)
 treatment of cell esds is used for estimating esds involving l.s. 
planes.
;

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 O5 1.769(2) 2_766 ?
Ti1 O1 1.884(2) . ?
Ti1 O3 2.124(2) . ?
Ti1 Cl2 2.2334(12) . ?
Ti1 Cl1 2.2342(10) . ?
Ti1 Ti2 3.2170(8) . ?
Ti2 O2 1.777(2) . ?
Ti2 O4 1.778(2) . ?
Ti2 O1 1.951(2) 2_766 ?
Ti2 O3 1.975(2) . ?
Ti2 O1 1.987(2) . ?
Ti2 Ti2 3.1507(11) 2_766 ?
O1 Ti2 1.951(2) 2_766 ?
O2 C1 1.378(4) . ?
O3 C12 1.387(4) . ?
O4 C23 1.371(4) . ?
O5 C34 1.362(4) . ?
O5 Ti1 1.769(2) 2_766 ?
C1 C2 1.393(5) . ?
C1 C6 1.394(5) . ?
C2 C3 1.388(5) . ?
C2 C44 1.521(5) . ?
C3 C4 1.395(5) . ?
C4 C5 1.391(5) . ?
C4 C7 1.539(5) . ?
C5 C6 1.396(5) . ?
C6 C11 1.514(5) . ?
C7 C8 1.521(5) . ?
C7 C9 1.528(5) . ?
C7 C10 1.542(6) . ?
C11 C13 1.507(5) . ?
C12 C17 1.395(5) . ?
C12 C13 1.409(5) . ?
C13 C14 1.386(5) . ?
C14 C15 1.378(5) . ?
C15 C16 1.396(5) . ?
C15 C18 1.537(5) . ?
C16 C17 1.391(5) . ?
C17 C22 1.523(5) . ?
C18 C21 1.522(6) . ?
C18 C20 1.526(6) . ?
C18 C19 1.547(6) . ?
C22 C24 1.515(4) . ?
C23 C24 1.393(5) . ?
C23 C28 1.402(4) . ?
C24 C25 1.389(5) . ?
C25 C26 1.399(5) . ?
C26 C27 1.383(5) . ?
C26 C29 1.535(5) . ?
C27 C28 1.389(5) . ?
C28 C33 1.511(5) . ?
C29 C30 1.486(7) . ?
C29 C31 1.517(7) . ?
C29 C32 1.555(8) . ?
C33 C35 1.518(5) . ?
C34 C35 1.394(5) . ?
C34 C39 1.399(5) . ?
C35 C36 1.385(5) . ?
C36 C37 1.401(5) . ?
C37 C38 1.387(5) . ?
C37 C40 1.524(5) . ?
C38 C39 1.392(5) . ?
C39 C44 1.515(5) . ?
C40 C42A 1.520(15) . ?
C40 C43 1.525(7) . ?
C40 C41 1.534(7) . ?
C40 C42 1.539(7) . ?
C40 C41A 1.542(16) . ?
C40 C43A 1.561(16) . ?
C45 C46 1.486(8) . ?
C46 C47 1.384(7) . ?
C46 C51 1.395(7) . ?
C47 C48 1.396(9) . ?
C48 C49 1.367(9) . ?
C49 C50 1.367(8) . ?
C50 C51 1.378(7) . ?

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
O5 Ti1 O1 90.44(10) 2_766 . ?
O5 Ti1 O3 161.88(10) 2_766 . ?
O1 Ti1 O3 71.48(9) . . ?
O5 Ti1 Cl2 97.85(8) 2_766 . ?
O1 Ti1 Cl2 123.66(8) . . ?
O3 Ti1 Cl2 91.54(7) . . ?
O5 Ti1 Cl1 98.69(8) 2_766 . ?
O1 Ti1 Cl1 121.90(8) . . ?
O3 Ti1 Cl1 92.11(7) . . ?
Cl2 Ti1 Cl1 111.72(4) . . ?
O5 Ti1 Ti2 125.21(8) 2_766 . ?
O1 Ti1 Ti2 34.81(6) . . ?
O3 Ti1 Ti2 36.68(6) . . ?
Cl2 Ti1 Ti2 110.72(3) . . ?
Cl1 Ti1 Ti2 111.52(3) . . ?
O2 Ti2 O4 116.10(10) . . ?
O2 Ti2 O1 99.04(11) . 2_766 ?
O4 Ti2 O1 99.16(10) . 2_766 ?
O2 Ti2 O3 100.38(10) . . ?
O4 Ti2 O3 96.67(10) . . ?
O1 Ti2 O3 146.28(9) 2_766 . ?
O2 Ti2 O1 119.78(10) . . ?
O4 Ti2 O1 124.10(10) . . ?
O1 Ti2 O1 73.71(10) 2_766 . ?
O3 Ti2 O1 72.75(9) . . ?
O2 Ti2 Ti2 114.24(8) . 2_766 ?
O4 Ti2 Ti2 116.87(8) . 2_766 ?
O1 Ti2 Ti2 37.24(6) 2_766 2_766 ?
O3 Ti2 Ti2 109.15(7) . 2_766 ?
O1 Ti2 Ti2 36.47(6) . 2_766 ?
O2 Ti2 Ti1 116.66(7) . . ?
O4 Ti2 Ti1 115.54(8) . . ?
O1 Ti2 Ti1 106.37(6) 2_766 . ?
O3 Ti2 Ti1 39.99(6) . . ?
O1 Ti2 Ti1 32.78(6) . . ?
Ti2 Ti2 Ti1 69.17(2) 2_766 . ?
Ti1 O1 Ti2 140.99(12) . 2_766 ?
Ti1 O1 Ti2 112.41(11) . . ?
Ti2 O1 Ti2 106.29(10) 2_766 . ?
C1 O2 Ti2 163.0(2) . . ?
C12 O3 Ti2 112.16(18) . . ?
C12 O3 Ti1 144.44(19) . . ?
Ti2 O3 Ti1 103.33(10) . . ?
C23 O4 Ti2 168.2(2) . . ?
C34 O5 Ti1 166.7(2) . 2_766 ?
O2 C1 C2 119.9(3) . . ?
O2 C1 C6 118.4(3) . . ?
C2 C1 C6 121.8(3) . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 C44 120.9(3) . . ?
C1 C2 C44 121.1(3) . . ?
C2 C3 C4 122.6(3) . . ?
C5 C4 C3 117.4(3) . . ?
C5 C4 C7 120.9(3) . . ?
C3 C4 C7 121.3(3) . . ?
C4 C5 C6 122.1(3) . . ?
C1 C6 C5 118.1(3) . . ?
C1 C6 C11 121.4(3) . . ?
C5 C6 C11 120.4(3) . . ?
C8 C7 C9 109.4(4) . . ?
C8 C7 C4 111.9(3) . . ?
C9 C7 C4 107.0(3) . . ?
C8 C7 C10 107.7(4) . . ?
C9 C7 C10 109.3(3) . . ?
C4 C7 C10 111.5(3) . . ?
C13 C11 C6 110.9(3) . . ?
O3 C12 C17 120.6(3) . . ?
O3 C12 C13 119.1(3) . . ?
C17 C12 C13 120.1(3) . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 C11 119.7(3) . . ?
C12 C13 C11 122.0(3) . . ?
C15 C14 C13 123.3(3) . . ?
C14 C15 C16 117.3(3) . . ?
C14 C15 C18 120.0(3) . . ?
C16 C15 C18 122.6(3) . . ?
C17 C16 C15 121.8(3) . . ?
C16 C17 C12 119.2(3) . . ?
C16 C17 C22 119.0(3) . . ?
C12 C17 C22 121.8(3) . . ?
C21 C18 C20 109.5(4) . . ?
C21 C18 C15 108.7(3) . . ?
C20 C18 C15 112.7(3) . . ?
C21 C18 C19 108.6(4) . . ?
C20 C18 C19 107.9(4) . . ?
C15 C18 C19 109.4(4) . . ?
C24 C22 C17 113.2(3) . . ?
O4 C23 C24 119.3(3) . . ?
O4 C23 C28 118.9(3) . . ?
C24 C23 C28 121.7(3) . . ?
C25 C24 C23 117.9(3) . . ?
C25 C24 C22 120.9(3) . . ?
C23 C24 C22 121.3(3) . . ?
C24 C25 C26 122.3(3) . . ?
C27 C26 C25 117.8(3) . . ?
C27 C26 C29 121.7(3) . . ?
C25 C26 C29 120.5(3) . . ?
C26 C27 C28 122.4(3) . . ?
C27 C28 C23 118.0(3) . . ?
C27 C28 C33 121.7(3) . . ?
C23 C28 C33 120.3(3) . . ?
C30 C29 C31 110.5(5) . . ?
C30 C29 C26 113.0(4) . . ?
C31 C29 C26 109.5(3) . . ?
C30 C29 C32 109.1(5) . . ?
C31 C29 C32 105.6(5) . . ?
C26 C29 C32 108.9(4) . . ?
C28 C33 C35 109.0(3) . . ?
O5 C34 C35 119.8(3) . . ?
O5 C34 C39 119.3(3) . . ?
C35 C34 C39 120.9(3) . . ?
C36 C35 C34 118.5(3) . . ?
C36 C35 C33 118.9(3) . . ?
C34 C35 C33 122.0(3) . . ?
C35 C36 C37 122.6(3) . . ?
C38 C37 C36 116.9(3) . . ?
C38 C37 C40 122.4(3) . . ?
C36 C37 C40 120.6(3) . . ?
C37 C38 C39 122.7(3) . . ?
C38 C39 C34 118.2(3) . . ?
C38 C39 C44 119.1(3) . . ?
C34 C39 C44 122.0(3) . . ?
C42A C40 C37 114.6(9) . . ?
C42A C40 C43 132.1(10) . . ?
C37 C40 C43 113.3(4) . . ?
C42A C40 C41 51.8(10) . . ?
C37 C40 C41 110.7(4) . . ?
C43 C40 C41 108.5(4) . . ?
C42A C40 C42 57.4(10) . . ?
C37 C40 C42 108.1(4) . . ?
C43 C40 C42 108.2(4) . . ?
C41 C40 C42 108.0(4) . . ?
C42A C40 C41A 110.6(14) . . ?
C37 C40 C41A 106.4(9) . . ?
C43 C40 C41A 52.7(10) . . ?
C41 C40 C41A 62.5(10) . . ?
C42 C40 C41A 145.2(10) . . ?
C42A C40 C43A 110.4(13) . . ?
C37 C40 C43A 109.4(9) . . ?
C43 C40 C43A 52.9(10) . . ?
C41 C40 C43A 140.0(9) . . ?
C42 C40 C43A 59.2(10) . . ?
C41A C40 C43A 104.9(13) . . ?
C39 C44 C2 109.0(3) . . ?
C47 C46 C51 116.7(5) . . ?
C47 C46 C45 121.9(5) . . ?
C51 C46 C45 121.3(5) . . ?
C46 C47 C48 122.0(6) . . ?
C49 C48 C47 119.2(6) . . ?
C48 C49 C50 120.3(6) . . ?
C49 C50 C51 120.3(6) . . ?
C50 C51 C46 121.5(5) . . ?

_refine_diff_density_max    1.281
_refine_diff_density_min   -1.172
_refine_diff_density_rms    0.108

#===END

# ----------------------------------------------------------------------