#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:03:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179275 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319531.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_4319531
loop_
_publ_author_name
'Joseph M. Tanski'
'Peter T. Wolczanski'
_publ_section_title
;
 Covalent Titanium Aryldioxy One-, Two-, and Three-Dimensional Networks
 and Their Examination as Ziegler-Natta Catalysts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2026
_journal_page_last               2033
_journal_paper_doi               10.1021/ic000763n
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C70 H59 N5 O8 Ti2'
_chemical_formula_weight         1194.02
_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                93.88(3)
_cell_angle_beta                 107.31(3)
_cell_angle_gamma                108.77(3)
_cell_formula_units_Z            2
_cell_length_a                   10.814(2)
_cell_length_b                   16.785(3)
_cell_length_c                   18.020(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2907.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.678
_diffrn_measured_fraction_theta_max 0.678
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90900
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5658
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.626
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         5658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.626
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          2.236
_refine_ls_shift/su_mean         0.422
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                4787
_reflns_number_total             19034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000763n_2.cif
_cod_data_source_block           jmt233
_cod_original_cell_volume        2907.8(10)
_cod_database_code               4319531
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 0.58063(9) 0.28840(5) 0.46516(5) 0.0562(4) Uani 1 1 d . . .
Ti2 Ti 0.17200(9) -0.21114(5) -0.03544(5) 0.0566(4) Uani 1 1 d . . .
O1 O 0.4377(3) 0.19687(18) 0.39448(18) 0.0654(9) Uani 1 1 d . . .
O2 O 0.2247(3) -0.12289(17) 0.04965(17) 0.0583(8) Uani 1 1 d . . .
O3 O 0.5991(3) 0.35732(17) 0.39012(18) 0.0620(9) Uani 1 1 d . . .
O4 O 0.0066(4) 0.25701(19) 0.03145(18) 0.0635(9) Uani 1 1 d . . .
O5 O 0.7010(3) 0.37696(17) 0.55035(18) 0.0582(8) Uani 1 1 d . . .
O6 O 1.1533(3) 0.69750(17) 0.89353(18) 0.0645(9) Uani 1 1 d . . .
O7 O 0.7170(3) 0.24258(18) 0.46847(17) 0.0613(9) Uani 1 1 d . . .
O8 O 0.8519(3) 0.14219(17) 0.11032(18) 0.0636(9) Uani 1 1 d . . .
N1 N 0.4094(5) 0.3330(2) 0.4821(2) 0.0626(11) Uani 1 1 d . . .
N1S N 0.885(2) -0.1844(18) 0.324(2) 0.077(8) Uani 0.40 1 d P . .
N2 N 0.5330(4) 0.2081(2) 0.5576(2) 0.0564(10) Uani 1 1 d . . .
N2S N 0.7368(15) -0.3160(8) 0.1771(11) 0.090(4) Uani 0.60 1 d P . .
N3 N 0.4049(4) -0.1659(2) -0.0192(2) 0.0639(11) Uani 1 1 d . . .
N4 N 0.2326(5) -0.2921(2) 0.0567(2) 0.0573(11) Uani 1 1 d . . .
C1 C 0.3616(5) 0.1169(3) 0.3529(3) 0.0567(12) Uani 1 1 d . . .
C1S C 0.8084(8) -0.2716(5) 0.3216(5) 0.101(2) Uani 1 1 d . . .
H1SA H 0.8010 -0.2883 0.3716 0.121 Uiso 1 1 calc R . .
C2 C 0.3602(5) 0.0942(3) 0.2785(3) 0.0591(13) Uani 1 1 d . . .
H2A H 0.4111 0.1349 0.2558 0.071 Uiso 1 1 calc R . .
C2S C 0.7427(7) -0.3327(4) 0.2560(5) 0.096(2) Uani 1 1 d . . .
H2SA H 0.7045 -0.3922 0.2624 0.116 Uiso 1 1 calc R . .
C3 C 0.2833(5) 0.0104(2) 0.2349(3) 0.0504(11) Uani 1 1 d . . .
C3S C 0.686(2) -0.3111(16) 0.1882(17) 0.068(6) Uani 0.40 1 d P . .
C4 C 0.2863(5) -0.0159(2) 0.1596(3) 0.0563(12) Uani 1 1 d . . .
H4B H 0.3362 0.0238 0.1358 0.068 Uiso 1 1 calc R . .
C4S C 0.7578(7) -0.2280(4) 0.1794(5) 0.100(2) Uani 1 1 d . . .
H4SA H 0.7213 -0.2100 0.1294 0.120 Uiso 1 1 calc R . .
C5 C 0.2167(5) -0.0990(2) 0.1211(2) 0.0528(11) Uani 1 1 d . . .
C5S C 0.8213(8) -0.1676(4) 0.2449(5) 0.093(2) Uani 1 1 d . . .
H5SA H 0.8296 -0.1085 0.2396 0.112 Uiso 1 1 calc R . .
C6 C 0.1396(5) -0.1591(3) 0.1554(3) 0.0569(12) Uani 1 1 d . . .
H6B H 0.0915 -0.2152 0.1286 0.068 Uiso 1 1 calc R . .
C6S C 0.819(2) -0.1910(15) 0.3128(17) 0.081(6) Uani 0.60 1 d P . .
C7 C 0.1345(5) -0.1357(3) 0.2281(3) 0.0635(13) Uani 1 1 d . . .
H7A H 0.0829 -0.1764 0.2504 0.076 Uiso 1 1 calc R . .
C7S C 0.8554(15) -0.1270(8) 0.3823(7) 0.110(4) Uani 0.60 1 d P . .
C8 C 0.2062(5) -0.0507(2) 0.2702(3) 0.0555(12) Uani 1 1 d . . .
C8S C 0.5987(14) -0.3744(8) 0.1181(7) 0.068(3) Uani 0.40 1 d P . .
C9 C 0.2057(5) -0.0254(3) 0.3462(3) 0.0626(13) Uani 1 1 d . . .
H9A H 0.1536 -0.0648 0.3693 0.075 Uiso 1 1 calc R . .
C10 C 0.2809(5) 0.0566(3) 0.3864(3) 0.0616(13) Uani 1 1 d . . .
H10A H 0.2787 0.0725 0.4363 0.074 Uiso 1 1 calc R . .
C11 C 0.5392(6) 0.3596(3) 0.3127(3) 0.0630(14) Uani 1 1 d . . .
C12 C 0.6291(6) 0.4063(3) 0.2745(3) 0.0644(13) Uani 1 1 d . . .
H12A H 0.7242 0.4318 0.3010 0.077 Uiso 1 1 calc R . .
C13 C 0.5713(6) 0.4126(3) 0.1969(3) 0.0691(15) Uani 1 1 d . . .
H13A H 0.6296 0.4427 0.1712 0.083 Uiso 1 1 calc R . .
C14 C 0.4286(6) 0.3757(3) 0.1549(3) 0.0638(14) Uani 1 1 d . . .
C15 C 0.3681(6) 0.3820(3) 0.0750(3) 0.0700(15) Uani 1 1 d . . .
H15A H 0.4245 0.4133 0.0490 0.084 Uiso 1 1 calc R . .
C16 C 0.2302(6) 0.3433(3) 0.0358(3) 0.0642(14) Uani 1 1 d . . .
H16A H 0.1929 0.3479 -0.0166 0.077 Uiso 1 1 calc R . .
C17 C 0.1430(6) 0.2960(3) 0.0747(3) 0.0583(13) Uani 1 1 d . . .
C18 C 0.1961(5) 0.2877(3) 0.1509(3) 0.0563(13) Uani 1 1 d . . .
H18A H 0.1379 0.2557 0.1756 0.068 Uiso 1 1 calc R . .
C19 C 0.3393(5) 0.3276(3) 0.1925(3) 0.0566(13) Uani 1 1 d . . .
C20 C 0.4008(6) 0.3215(3) 0.2742(3) 0.0604(13) Uani 1 1 d . . .
H20A H 0.3444 0.2910 0.3006 0.072 Uiso 1 1 calc R . .
C21 C 0.8034(5) 0.4009(2) 0.6204(3) 0.0542(12) Uani 1 1 d . . .
C22 C 0.8586(5) 0.3411(3) 0.6558(3) 0.0571(12) Uani 1 1 d . . .
H22A H 0.8260 0.2851 0.6290 0.069 Uiso 1 1 calc R . .
C23 C 0.9571(5) 0.3645(3) 0.7274(3) 0.0630(13) Uani 1 1 d . . .
H23A H 0.9892 0.3236 0.7499 0.076 Uiso 1 1 calc R . .
C24 C 1.0138(5) 0.4496(3) 0.7697(3) 0.0544(12) Uani 1 1 d . . .
C25 C 1.1157(5) 0.4753(3) 0.8452(3) 0.0621(13) Uani 1 1 d . . .
H25A H 1.1520 0.4360 0.8680 0.074 Uiso 1 1 calc R . .
C26 C 1.1626(5) 0.5570(3) 0.8860(3) 0.0602(12) Uani 1 1 d . . .
H26A H 1.2299 0.5729 0.9360 0.072 Uiso 1 1 calc R . .
C27 C 1.1077(5) 0.6175(3) 0.8515(3) 0.0575(13) Uani 1 1 d . . .
C28 C 1.0126(5) 0.5948(3) 0.7782(3) 0.0563(12) Uani 1 1 d . . .
H28A H 0.9795 0.6354 0.7558 0.068 Uiso 1 1 calc R . .
C29 C 0.9617(5) 0.5105(2) 0.7344(3) 0.0548(12) Uani 1 1 d . . .
C30 C 0.8577(5) 0.4843(3) 0.6594(3) 0.0568(12) Uani 1 1 d . . .
H30A H 0.8248 0.5244 0.6356 0.068 Uiso 1 1 calc R . .
C31 C 0.7725(5) 0.2040(3) 0.4263(3) 0.0581(13) Uani 1 1 d . . .
C32 C 0.7579(5) 0.2119(2) 0.3498(3) 0.0560(12) Uani 1 1 d . . .
H32A H 0.7069 0.2440 0.3254 0.067 Uiso 1 1 calc R . .
C33 C 0.8189(5) 0.1722(3) 0.3071(3) 0.0585(12) Uani 1 1 d . . .
C34 C 0.8040(5) 0.1782(3) 0.2267(3) 0.0587(12) Uani 1 1 d . . .
H34A H 0.7508 0.2082 0.2004 0.070 Uiso 1 1 calc R . .
C35 C 0.8681(5) 0.1397(3) 0.1873(3) 0.0596(13) Uani 1 1 d . . .
C36 C 0.9466(6) 0.0934(3) 0.2258(3) 0.0672(14) Uani 1 1 d . . .
H36A H 0.9888 0.0674 0.1989 0.081 Uiso 1 1 calc R . .
C37 C 0.9617(6) 0.0861(3) 0.3027(3) 0.0699(14) Uani 1 1 d . . .
H37A H 1.0152 0.0556 0.3276 0.084 Uiso 1 1 calc R . .
C38 C 0.8981(5) 0.1239(3) 0.3454(3) 0.0622(13) Uani 1 1 d . . .
C39 C 0.9105(6) 0.1173(3) 0.4244(3) 0.0707(14) Uani 1 1 d . . .
H39A H 0.9622 0.0863 0.4504 0.085 Uiso 1 1 calc R . .
C40 C 0.8481(6) 0.1554(3) 0.4637(3) 0.0665(14) Uani 1 1 d . . .
H40A H 0.8559 0.1491 0.5156 0.080 Uiso 1 1 calc R . .
C41 C 0.4421(6) 0.4068(3) 0.5318(3) 0.0687(14) Uani 1 1 d . . .
H41A H 0.5353 0.4380 0.5597 0.082 Uiso 1 1 calc R . .
C42 C 0.3449(6) 0.4377(3) 0.5430(3) 0.0706(15) Uani 1 1 d . . .
H42A H 0.3731 0.4886 0.5779 0.085 Uiso 1 1 calc R . .
C43 C 0.2060(6) 0.3940(3) 0.5031(3) 0.0628(13) Uani 1 1 d . . .
C44 C 0.0957(6) 0.4257(3) 0.5144(3) 0.0785(15) Uani 1 1 d . . .
H44A H 0.1389 0.4781 0.5521 0.118 Uiso 1 1 calc R . .
H44B H 0.0344 0.3835 0.5333 0.118 Uiso 1 1 calc R . .
H44C H 0.0437 0.4355 0.4648 0.118 Uiso 1 1 calc R . .
C45 C 0.1722(6) 0.3192(3) 0.4519(3) 0.0679(14) Uani 1 1 d . . .
H45A H 0.0797 0.2880 0.4225 0.081 Uiso 1 1 calc R . .
C46 C 0.2740(6) 0.2907(3) 0.4439(3) 0.0690(15) Uani 1 1 d . . .
H46A H 0.2473 0.2392 0.4101 0.083 Uiso 1 1 calc R . .
C47 C 0.5407(5) 0.1309(3) 0.5550(3) 0.0631(13) Uani 1 1 d . . .
H47A H 0.5716 0.1126 0.5164 0.076 Uiso 1 1 calc R . .
C48 C 0.5065(5) 0.0757(3) 0.6049(3) 0.0654(13) Uani 1 1 d . . .
H48A H 0.5175 0.0231 0.6002 0.078 Uiso 1 1 calc R . .
C49 C 0.4575(6) 0.0974(3) 0.6603(4) 0.0751(15) Uani 1 1 d . . .
C50 C 0.4203(7) 0.0412(4) 0.7179(4) 0.101(2) Uani 1 1 d . . .
H50A H 0.4330 -0.0118 0.7066 0.151 Uiso 1 1 calc R . .
H50B H 0.3252 0.0299 0.7131 0.151 Uiso 1 1 calc R . .
H50C H 0.4791 0.0696 0.7708 0.151 Uiso 1 1 calc R . .
C51 C 0.4543(12) 0.1781(5) 0.6646(6) 0.181(5) Uani 1 1 d . . .
H51A H 0.4274 0.1986 0.7041 0.217 Uiso 1 1 calc R . .
C52 C 0.4893(9) 0.2302(4) 0.6129(5) 0.129(3) Uani 1 1 d . . .
H52A H 0.4814 0.2837 0.6175 0.155 Uiso 1 1 calc R . .
C53 C 0.4602(6) -0.2079(3) -0.0576(3) 0.0660(14) Uani 1 1 d . . .
H53A H 0.4016 -0.2589 -0.0921 0.079 Uiso 1 1 calc R . .
C54 C 0.5973(6) -0.1803(3) -0.0492(3) 0.0667(14) Uani 1 1 d . . .
H54A H 0.6283 -0.2117 -0.0792 0.080 Uiso 1 1 calc R . .
C55 C 0.6926(5) -0.1059(3) 0.0035(3) 0.0658(14) Uani 1 1 d . . .
C56 C 0.8430(5) -0.0739(3) 0.0150(4) 0.0787(16) Uani 1 1 d . . .
H56A H 0.8891 -0.0222 0.0538 0.118 Uiso 1 1 calc R . .
H56B H 0.8561 -0.0624 -0.0341 0.118 Uiso 1 1 calc R . .
H56C H 0.8811 -0.1163 0.0327 0.118 Uiso 1 1 calc R . .
C57 C 0.6341(6) -0.0626(3) 0.0436(3) 0.0694(15) Uani 1 1 d . . .
H57A H 0.6905 -0.0120 0.0792 0.083 Uiso 1 1 calc R . .
C58 C 0.4962(5) -0.0934(3) 0.0313(3) 0.0639(14) Uani 1 1 d . . .
H58A H 0.4619 -0.0625 0.0595 0.077 Uiso 1 1 calc R . .
C59 C 0.1433(5) -0.3691(3) 0.0547(3) 0.0669(14) Uani 1 1 d . . .
H59A H 0.0544 -0.3867 0.0177 0.080 Uiso 1 1 calc R . .
C60 C 0.1744(7) -0.4241(3) 0.1037(3) 0.0686(15) Uani 1 1 d . . .
H60A H 0.1068 -0.4771 0.0987 0.082 Uiso 1 1 calc R . .
C61 C 0.2987(7) -0.4034(3) 0.1582(4) 0.0774(16) Uani 1 1 d . . .
C62 C 0.3371(7) -0.4598(4) 0.2160(4) 0.103(2) Uani 1 1 d . . .
H62A H 0.2579 -0.5107 0.2075 0.155 Uiso 1 1 calc R . .
H62B H 0.3665 -0.4295 0.2690 0.155 Uiso 1 1 calc R . .
H62C H 0.4113 -0.4749 0.2082 0.155 Uiso 1 1 calc R . .
C63 C 0.3916(8) -0.3236(5) 0.1624(7) 0.182(5) Uani 1 1 d . . .
H63A H 0.4806 -0.3048 0.1994 0.219 Uiso 1 1 calc R . .
C64 C 0.3523(8) -0.2709(4) 0.1110(5) 0.137(4) Uani 1 1 d . . .
H64A H 0.4168 -0.2166 0.1163 0.164 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'
N N 0.0061 0.0033 '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 Ti1 O3 94.63(14) . . ?
O1 Ti1 O7 95.05(14) . . ?
O3 Ti1 O7 101.08(14) . . ?
O1 Ti1 O5 167.60(15) . . ?
O3 Ti1 O5 93.76(13) . . ?
O7 Ti1 O5 92.27(14) . . ?
O1 Ti1 N2 83.90(14) . . ?
O3 Ti1 N2 172.37(14) . . ?
O7 Ti1 N2 86.51(13) . . ?
O5 Ti1 N2 86.57(13) . . ?
O1 Ti1 N1 85.72(14) . . ?
O3 Ti1 N1 89.88(14) . . ?
O7 Ti1 N1 168.90(14) . . ?
O5 Ti1 N1 85.19(14) . . ?
N2 Ti1 N1 82.55(14) . . ?
O6 Ti2 O8 94.48(14) 1_444 2_655 ?
O6 Ti2 O4 95.25(14) 1_444 2 ?
O8 Ti2 O4 101.37(15) 2_655 2 ?
O6 Ti2 O2 167.64(15) 1_444 . ?
O8 Ti2 O2 93.79(13) 2_655 . ?
O4 Ti2 O2 92.10(14) 2 . ?
O6 Ti2 N4 83.70(14) 1_444 . ?
O8 Ti2 N4 171.93(15) 2_655 . ?
O4 Ti2 N4 86.65(15) 2 . ?
O2 Ti2 N4 86.83(13) . . ?
O6 Ti2 N3 85.74(14) 1_444 . ?
O8 Ti2 N3 89.52(14) 2_655 . ?
O4 Ti2 N3 168.94(14) 2 . ?
O2 Ti2 N3 85.16(14) . . ?
N4 Ti2 N3 82.51(15) . . ?
C1 O1 Ti1 161.4(3) . . ?
C5 O2 Ti2 147.3(3) . . ?
C11 O3 Ti1 141.6(3) . . ?
C17 O4 Ti2 145.2(3) . 2 ?
C21 O5 Ti1 147.3(3) . . ?
C27 O6 Ti2 161.3(3) . 1_666 ?
C31 O7 Ti1 146.2(3) . . ?
C35 O8 Ti2 142.0(3) . 2_655 ?
C46 N1 C41 115.7(4) . . ?
C46 N1 Ti1 123.7(3) . . ?
C41 N1 Ti1 120.6(4) . . ?
C6S N1S C1S 70(4) . . ?
C6S N1S C5S 64(5) . . ?
C1S N1S C5S 105(2) . . ?
C6S N1S C7S 70(4) . . ?
C1S N1S C7S 108.9(17) . . ?
C5S N1S C7S 105.6(18) . . ?
C52 N2 C47 114.6(4) . . ?
C52 N2 Ti1 124.7(3) . . ?
C47 N2 Ti1 120.5(3) . . ?
C3S N2S C4S 76(3) . . ?
C3S N2S C2S 66(4) . . ?
C4S N2S C2S 106.6(11) . . ?
C3S N2S C8S 71(4) . . ?
C4S N2S C8S 113.4(12) . . ?
C2S N2S C8S 109.1(9) . . ?
C58 N3 C53 115.1(4) . . ?
C58 N3 Ti2 121.2(3) . . ?
C53 N3 Ti2 123.7(3) . . ?
C64 N4 C59 114.6(4) . . ?
C64 N4 Ti2 125.1(3) . . ?
C59 N4 Ti2 120.3(4) . . ?
O1 C1 C2 121.0(4) . . ?
O1 C1 C10 119.5(4) . . ?
C2 C1 C10 119.5(4) . . ?
C6S C1S C2S 117.3(14) . . ?
C6S C1S N1S 26.9(15) . . ?
C2S C1S N1S 125.2(17) . . ?
C1 C2 C3 121.6(4) . . ?
C1S C2S C3S 118.6(13) . . ?
C1S C2S N2S 123.4(8) . . ?
C3S C2S N2S 27.3(6) . . ?
C4 C3 C2 122.6(4) . . ?
C4 C3 C8 118.8(4) . . ?
C2 C3 C8 118.5(4) . . ?
N2S C3S C4S 77(3) . . ?
N2S C3S C2S 87(4) . . ?
C4S C3S C2S 115(2) . . ?
N2S C3S C8S 83(4) . . ?
C4S C3S C8S 118.6(19) . . ?
C2S C3S C8S 121.7(19) . . ?
C5 C4 C3 121.0(4) . . ?
C5S C4S C3S 117.0(13) . . ?
C5S C4S N2S 125.1(10) . . ?
C3S C4S N2S 27.4(6) . . ?
O2 C5 C4 119.6(4) . . ?
O2 C5 C6 120.1(3) . . ?
C4 C5 C6 120.3(4) . . ?
C4S C5S C6S 118.0(12) . . ?
C4S C5S N1S 123.6(13) . . ?
C6S C5S N1S 26.2(10) . . ?
C7 C6 C5 120.2(4) . . ?
N1S C6S C1S 83(5) . . ?
N1S C6S C5S 90(5) . . ?
C1S C6S C5S 119.2(19) . . ?
N1S C6S C7S 86(5) . . ?
C1S C6S C7S 119(2) . . ?
C5S C6S C7S 120.2(18) . . ?
C6 C7 C8 121.3(4) . . ?
C6S C7S N1S 24.6(15) . . ?
C9 C8 C7 122.4(4) . . ?
C9 C8 C3 119.1(4) . . ?
C7 C8 C3 118.5(4) . . ?
C3S C8S N2S 25.9(6) . . ?
C10 C9 C8 120.7(4) . . ?
C9 C10 C1 120.6(4) . . ?
C20 C11 O3 122.2(5) . . ?
C20 C11 C12 121.4(5) . . ?
O3 C11 C12 116.4(5) . . ?
C13 C12 C11 118.0(5) . . ?
C12 C13 C14 122.8(5) . . ?
C13 C14 C19 119.1(5) . . ?
C13 C14 C15 123.2(5) . . ?
C19 C14 C15 117.6(5) . . ?
C16 C15 C14 121.5(5) . . ?
C15 C16 C17 119.9(5) . . ?
O4 C17 C18 122.3(4) . . ?
O4 C17 C16 116.9(4) . . ?
C18 C17 C16 120.7(5) . . ?
C17 C18 C19 120.0(5) . . ?
C18 C19 C14 120.2(4) . . ?
C18 C19 C20 122.1(4) . . ?
C14 C19 C20 117.7(5) . . ?
C11 C20 C19 121.0(5) . . ?
O5 C21 C30 120.5(4) . . ?
O5 C21 C22 121.0(4) . . ?
C30 C21 C22 118.6(4) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C24 122.0(4) . . ?
C25 C24 C29 119.1(4) . . ?
C25 C24 C23 123.0(4) . . ?
C29 C24 C23 117.8(4) . . ?
C26 C25 C24 121.3(4) . . ?
C25 C26 C27 119.6(4) . . ?
C28 C27 O6 121.3(4) . . ?
C28 C27 C26 120.1(4) . . ?
O6 C27 C26 118.7(4) . . ?
C27 C28 C29 121.7(4) . . ?
C30 C29 C24 119.1(4) . . ?
C30 C29 C28 122.7(4) . . ?
C24 C29 C28 118.1(4) . . ?
C21 C30 C29 121.7(4) . . ?
O7 C31 C32 121.8(4) . . ?
O7 C31 C40 118.0(4) . . ?
C32 C31 C40 120.2(4) . . ?
C31 C32 C33 120.9(4) . . ?
C32 C33 C38 119.1(4) . . ?
C32 C33 C34 122.3(4) . . ?
C38 C33 C34 118.6(4) . . ?
C35 C34 C33 120.6(5) . . ?
O8 C35 C34 121.7(5) . . ?
O8 C35 C36 118.0(4) . . ?
C34 C35 C36 120.2(4) . . ?
C37 C36 C35 120.4(5) . . ?
C36 C37 C38 121.5(5) . . ?
C39 C38 C33 118.2(4) . . ?
C39 C38 C37 123.1(5) . . ?
C33 C38 C37 118.7(4) . . ?
C40 C39 C38 121.2(5) . . ?
C39 C40 C31 120.4(5) . . ?
N1 C41 C42 123.3(5) . . ?
C43 C42 C41 120.6(5) . . ?
C42 C43 C45 116.3(5) . . ?
C42 C43 C44 122.1(5) . . ?
C45 C43 C44 121.6(5) . . ?
C46 C45 C43 120.6(5) . . ?
N1 C46 C45 123.5(5) . . ?
N2 C47 C48 125.0(4) . . ?
C49 C48 C47 120.4(4) . . ?
C48 C49 C51 114.4(5) . . ?
C48 C49 C50 123.5(5) . . ?
C51 C49 C50 122.0(5) . . ?
C52 C51 C49 122.5(6) . . ?
N2 C52 C51 123.0(5) . . ?
C54 C53 N3 123.7(4) . . ?
C53 C54 C55 121.5(5) . . ?
C57 C55 C54 114.3(5) . . ?
C57 C55 C56 122.4(5) . . ?
C54 C55 C56 123.3(5) . . ?
C58 C57 C55 120.8(5) . . ?
N3 C58 C57 124.5(5) . . ?
N4 C59 C60 124.0(5) . . ?
C61 C60 C59 121.5(5) . . ?
C60 C61 C63 115.5(5) . . ?
C60 C61 C62 123.8(5) . . ?
C63 C61 C62 120.6(6) . . ?
C64 C63 C61 119.9(7) . . ?
N4 C64 C63 124.5(6) . . ?
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 O1 1.846(3) . ?
Ti1 O3 1.852(3) . ?
Ti1 O7 1.859(3) . ?
Ti1 O5 1.875(3) . ?
Ti1 N2 2.287(4) . ?
Ti1 N1 2.298(4) . ?
Ti2 O6 1.847(3) 1_444 ?
Ti2 O8 1.850(3) 2_655 ?
Ti2 O4 1.861(4) 2 ?
Ti2 O2 1.871(3) . ?
Ti2 N4 2.294(4) . ?
Ti2 N3 2.303(4) . ?
O1 C1 1.351(5) . ?
O2 C5 1.358(5) . ?
O3 C11 1.362(6) . ?
O4 C17 1.355(6) . ?
O4 Ti2 1.861(4) 2 ?
O5 C21 1.339(5) . ?
O6 C27 1.355(5) . ?
O6 Ti2 1.847(3) 1_666 ?
O7 C31 1.346(5) . ?
O8 C35 1.350(5) . ?
O8 Ti2 1.850(3) 2_655 ?
N1 C46 1.336(6) . ?
N1 C41 1.358(6) . ?
N1S C6S 0.65(3) . ?
N1S C1S 1.42(3) . ?
N1S C5S 1.47(4) . ?
N1S C7S 1.55(3) . ?
N2 C52 1.302(7) . ?
N2 C47 1.322(5) . ?
N2S C3S 0.667(13) . ?
N2S C4S 1.415(14) . ?
N2S C2S 1.455(18) . ?
N2S C8S 1.51(2) . ?
N3 C58 1.352(6) . ?
N3 C53 1.337(6) . ?
N4 C64 1.289(7) . ?
N4 C59 1.333(6) . ?
C1 C2 1.363(6) . ?
C1 C10 1.407(6) . ?
C1S C6S 1.34(2) . ?
C1S C2S 1.350(9) . ?
C2 C3 1.412(6) . ?
C2S C3S 1.33(3) . ?
C3 C4 1.412(6) . ?
C3 C8 1.416(6) . ?
C3S C4S 1.41(2) . ?
C3S C8S 1.44(3) . ?
C4 C5 1.370(6) . ?
C4S C5S 1.343(9) . ?
C5 C6 1.394(6) . ?
C5S C6S 1.32(3) . ?
C6 C7 1.364(6) . ?
C6S C7S 1.46(3) . ?
C7 C8 1.416(6) . ?
C8 C9 1.408(6) . ?
C9 C10 1.369(6) . ?
C11 C20 1.355(7) . ?
C11 C12 1.419(7) . ?
C12 C13 1.378(7) . ?
C13 C14 1.402(7) . ?
C14 C19 1.416(7) . ?
C14 C15 1.420(7) . ?
C15 C16 1.353(7) . ?
C16 C17 1.413(7) . ?
C17 C18 1.358(7) . ?
C18 C19 1.408(7) . ?
C19 C20 1.449(7) . ?
C21 C30 1.376(6) . ?
C21 C22 1.419(6) . ?
C22 C23 1.340(6) . ?
C23 C24 1.418(6) . ?
C24 C25 1.405(6) . ?
C24 C29 1.419(6) . ?
C25 C26 1.368(6) . ?
C26 C27 1.422(7) . ?
C27 C28 1.348(6) . ?
C28 C29 1.421(6) . ?
C29 C30 1.407(6) . ?
C31 C32 1.361(6) . ?
C31 C40 1.402(7) . ?
C32 C33 1.411(6) . ?
C33 C38 1.428(7) . ?
C33 C34 1.423(6) . ?
C34 C35 1.387(7) . ?
C35 C36 1.398(7) . ?
C36 C37 1.364(7) . ?
C37 C38 1.413(7) . ?
C38 C39 1.406(7) . ?
C39 C40 1.367(7) . ?
C41 C42 1.370(7) . ?
C42 C43 1.374(7) . ?
C43 C45 1.382(7) . ?
C43 C44 1.511(7) . ?
C45 C46 1.374(7) . ?
C47 C48 1.377(7) . ?
C48 C49 1.341(7) . ?
C49 C51 1.364(8) . ?
C49 C50 1.506(7) . ?
C51 C52 1.372(9) . ?
C53 C54 1.360(7) . ?
C54 C55 1.398(7) . ?
C55 C57 1.395(7) . ?
C55 C56 1.482(7) . ?
C57 C58 1.353(7) . ?
C59 C60 1.370(7) . ?
C60 C61 1.327(7) . ?
C61 C63 1.372(8) . ?
C61 C62 1.510(8) . ?
C63 C64 1.392(10) . ?
