#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:30:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179848 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/44/7014451.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_7014451
loop_
_publ_author_name
'Darwish, Wael'
'Seikel, Elisabeth'
'Käsmarker, Ralf'
'Harms, Klaus'
'Sundermeyer, Jörg'
_publ_section_title
;
 Synthesis and X-ray crystal structures of imido and ureato derivatives
 of titanium(iv) phthalocyanine and their application in the catalytic
 formation of carbodiimides by metathesis from isocyanates.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1787
_journal_page_last               1794
_journal_paper_doi               10.1039/c0dt00867b
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H33 N8 Ti1'
_chemical_formula_sum            'C44 H33 N9 Ti'
_chemical_formula_weight         735.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-04-18T16:02:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.568(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9544(9)
_cell_length_b                   17.0865(9)
_cell_length_c                   19.5582(15)
_cell_measurement_reflns_used    11975
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1.5
_cell_measurement_wavelength     0.71073
_cell_volume                     3543.1(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29449
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
a grid of 8 x 8 x 8 = 512 sampling points was used
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0342P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                3550
_reflns_number_total             6229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00867B.TXT
_cod_data_source_block           2a
_cod_original_cell_volume        3543.1(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7014451
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
C2 C 0.3357(3) 0.19479(16) 0.44585(14) 0.0328(7) Uani 1 1 d . . .
C3 C 0.2798(3) 0.26090(16) 0.47342(14) 0.0345(7) Uani 1 1 d . . .
C4 C 0.1704(3) 0.30393(17) 0.44628(16) 0.0411(8) Uani 1 1 d . . .
H4 H 0.1143 0.2911 0.4022 0.049 Uiso 1 1 calc R . .
C5 C 0.1470(3) 0.36597(19) 0.48617(17) 0.0506(9) Uani 1 1 d . . .
H5 H 0.0743 0.3974 0.4685 0.061 Uiso 1 1 calc R . .
C6 C 0.2278(3) 0.3839(2) 0.55212(16) 0.0499(8) Uani 1 1 d . . .
H6 H 0.2082 0.4266 0.5786 0.06 Uiso 1 1 calc R . .
C7 C 0.3344(3) 0.34078(18) 0.57894(16) 0.0417(8) Uani 1 1 d . . .
H7 H 0.3888 0.3527 0.6238 0.05 Uiso 1 1 calc R . .
C8 C 0.3604(3) 0.27943(16) 0.53892(14) 0.0328(7) Uani 1 1 d . . .
C9 C 0.4653(3) 0.22437(17) 0.55065(14) 0.0337(7) Uani 1 1 d . . .
C11 C 0.6588(3) 0.17654(17) 0.61780(13) 0.0328(7) Uani 1 1 d . . .
C13 C 0.7901(3) 0.08151(17) 0.60228(13) 0.0319(7) Uani 1 1 d . . .
C14 C 0.8477(3) 0.11881(17) 0.66951(12) 0.0319(6) Uani 1 1 d . . .
C15 C 0.9635(3) 0.10585(17) 0.71725(13) 0.0371(7) Uani 1 1 d . . .
H15 H 1.019 0.0658 0.7099 0.045 Uiso 1 1 calc R . .
C16 C 0.9940(3) 0.15395(18) 0.77591(14) 0.0428(8) Uani 1 1 d . . .
H16 H 1.073 0.1474 0.8093 0.051 Uiso 1 1 calc R . .
C17 C 0.9119(3) 0.21162(19) 0.78711(14) 0.0439(8) Uani 1 1 d . . .
H17 H 0.9355 0.2431 0.8284 0.053 Uiso 1 1 calc R . .
C18 C 0.7960(3) 0.22452(17) 0.73962(14) 0.0411(8) Uani 1 1 d . . .
H18 H 0.7398 0.2637 0.7478 0.049 Uiso 1 1 calc R . .
C19 C 0.7656(3) 0.17762(16) 0.67954(13) 0.0325(7) Uani 1 1 d . . .
C21 C 0.7928(3) -0.01112(16) 0.51413(13) 0.0314(7) Uani 1 1 d . . .
C23 C 0.6650(3) -0.04106(16) 0.40947(13) 0.0320(7) Uani 1 1 d . . .
C24 C 0.7709(3) -0.09427(16) 0.42073(13) 0.0318(7) Uani 1 1 d . . .
C25 C 0.8014(3) -0.15391(17) 0.37960(14) 0.0371(7) Uani 1 1 d . . .
H25 H 0.747 -0.167 0.3351 0.045 Uiso 1 1 calc R . .
C26 C 0.9132(3) -0.19345(18) 0.40545(14) 0.0404(8) Uani 1 1 d . . .
H26 H 0.9366 -0.234 0.3781 0.049 Uiso 1 1 calc R . .
C27 C 0.9926(3) -0.17491(18) 0.47111(14) 0.0395(7) Uani 1 1 d . . .
H27 H 1.0688 -0.2033 0.4877 0.047 Uiso 1 1 calc R . .
C28 C 0.9626(3) -0.11602(18) 0.51245(13) 0.0367(7) Uani 1 1 d . . .
H28 H 1.0166 -0.1037 0.5573 0.044 Uiso 1 1 calc R . .
C29 C 0.8516(3) -0.07583(16) 0.48638(13) 0.0323(7) Uani 1 1 d . . .
C31 C 0.4706(3) 0.00659(17) 0.34297(13) 0.0321(7) Uani 1 1 d . . .
C33 C 0.3366(3) 0.10106(17) 0.35766(13) 0.0327(7) Uani 1 1 d . . .
C34 C 0.2799(3) 0.06333(17) 0.29015(13) 0.0322(7) Uani 1 1 d . . .
C35 C 0.1673(3) 0.07610(18) 0.23957(14) 0.0381(7) Uani 1 1 d . . .
H35 H 0.1097 0.1155 0.2457 0.046 Uiso 1 1 calc R . .
C36 C 0.1426(3) 0.02941(19) 0.18029(15) 0.0456(8) Uani 1 1 d . . .
H36 H 0.0669 0.0376 0.1446 0.055 Uiso 1 1 calc R . .
C37 C 0.2249(3) -0.02935(19) 0.17115(14) 0.0435(8) Uani 1 1 d . . .
H37 H 0.2042 -0.0607 0.1297 0.052 Uiso 1 1 calc R . .
C38 C 0.3363(3) -0.04269(18) 0.22141(14) 0.0395(8) Uani 1 1 d . . .
H38 H 0.3929 -0.0827 0.2154 0.047 Uiso 1 1 calc R . .
C39 C 0.3628(3) 0.00476(17) 0.28127(13) 0.0339(7) Uani 1 1 d . . .
C42 C 0.7345(3) 0.23622(18) 0.39597(13) 0.0364(7) Uani 1 1 d . . .
C43 C 0.7590(3) 0.3129(2) 0.42427(15) 0.0449(8) Uani 1 1 d . . .
C44 C 0.8183(3) 0.3654(2) 0.38864(18) 0.0584(10) Uani 1 1 d . . .
H44 H 0.8342 0.4173 0.406 0.07 Uiso 1 1 calc R . .
C45 C 0.8546(3) 0.3437(3) 0.32835(19) 0.0663(12) Uani 1 1 d . . .
H45 H 0.8931 0.3808 0.3043 0.08 Uiso 1 1 calc R . .
C46 C 0.8350(3) 0.2683(3) 0.30352(18) 0.0622(11) Uani 1 1 d . . .
H46 H 0.8638 0.2535 0.2635 0.075 Uiso 1 1 calc R . .
C47 C 0.7743(3) 0.2135(2) 0.33521(15) 0.0474(9) Uani 1 1 d . . .
C48 C 0.7192(4) 0.3364(2) 0.49030(16) 0.0541(10) Uani 1 1 d . . .
H48 H 0.6979 0.2873 0.5125 0.065 Uiso 1 1 calc R . .
C49 C 0.6029(4) 0.3869(3) 0.4739(2) 0.0816(12) Uani 1 1 d . . .
H49A H 0.6209 0.4362 0.4528 0.122 Uiso 1 1 calc R . .
H49B H 0.5775 0.3978 0.5175 0.122 Uiso 1 1 calc R . .
H49C H 0.5345 0.3595 0.4405 0.122 Uiso 1 1 calc R . .
C50 C 0.8267(4) 0.3770(3) 0.5451(2) 0.0835(13) Uani 1 1 d . . .
H50A H 0.8414 0.4291 0.528 0.125 Uiso 1 1 calc R . .
H50B H 0.9039 0.3457 0.5521 0.125 Uiso 1 1 calc R . .
H50C H 0.8031 0.3818 0.59 0.125 Uiso 1 1 calc R . .
C51 C 0.7487(4) 0.1320(2) 0.30593(16) 0.0607(11) Uani 1 1 d . . .
H51 H 0.7353 0.098 0.345 0.073 Uiso 1 1 calc R . .
C52 C 0.6265(4) 0.1305(2) 0.2473(2) 0.0722(12) Uani 1 1 d . . .
H52A H 0.5572 0.1507 0.2655 0.108 Uiso 1 1 calc R . .
H52B H 0.6078 0.0766 0.2308 0.108 Uiso 1 1 calc R . .
H52C H 0.6363 0.1632 0.2079 0.108 Uiso 1 1 calc R . .
C53 C 0.8542(4) 0.0953(3) 0.27897(19) 0.0977(18) Uani 1 1 d . . .
H53A H 0.8311 0.0415 0.2635 0.147 Uiso 1 1 calc R . .
H53B H 0.932 0.0948 0.3169 0.147 Uiso 1 1 calc R . .
H53C H 0.8674 0.1259 0.2391 0.147 Uiso 1 1 calc R . .
N1 N 0.4482(2) 0.17538(13) 0.49268(11) 0.0332(6) Uani 1 1 d . . .
N10 N 0.5616(2) 0.22523(14) 0.60796(11) 0.0356(6) Uani 1 1 d . . .
N12 N 0.6782(2) 0.11840(14) 0.57211(10) 0.0309(5) Uani 1 1 d . . .
N20 N 0.8431(2) 0.02239(13) 0.57663(11) 0.0320(6) Uani 1 1 d . . .
N22 N 0.6817(2) 0.00951(13) 0.46649(10) 0.0312(6) Uani 1 1 d . . .
N30 N 0.5682(2) -0.04172(14) 0.35229(11) 0.0343(6) Uani 1 1 d . . .
N32 N 0.4519(2) 0.06620(13) 0.38702(10) 0.0314(6) Uani 1 1 d . . .
N40 N 0.2835(2) 0.16048(14) 0.38369(11) 0.0337(6) Uani 1 1 d . . .
N41 N 0.6698(2) 0.18258(14) 0.42742(11) 0.0327(6) Uani 1 1 d . . .
Ti1 Ti 0.59215(5) 0.11540(3) 0.46591(2) 0.03033(14) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 8 11 0.062
0 -11 7 0.031
1 -3 -6 0.049
0 10 4 0.021
0 -13 -5 0.035
9 -4 -2 0.161
0 1 7 0.042
2 7 -8 0.058
-2 -7 7 0.067
-10 2 11 0.147
0 0 -1 0.033
0 7 -4 0.012
4 11 -9 0.08
-3 -6 -11 0.083
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
N40 C2 N1 127.1(3) . . ?
N40 C2 C3 123.6(3) . . ?
N1 C2 C3 109.3(2) . . ?
C4 C3 C8 121.0(3) . . ?
C4 C3 C2 132.2(3) . . ?
C8 C3 C2 106.8(2) . . ?
C5 C4 C3 117.1(3) . . ?
C5 C4 H4 121.5 . . ?
C3 C4 H4 121.5 . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 121.0(3) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 118.0(3) . . ?
C6 C7 H7 121 . . ?
C8 C7 H7 121 . . ?
C7 C8 C3 121.3(3) . . ?
C7 C8 C9 131.9(3) . . ?
C3 C8 C9 106.8(2) . . ?
N10 C9 N1 127.7(3) . . ?
N10 C9 C8 123.5(2) . . ?
N1 C9 C8 108.8(2) . . ?
N10 C11 N12 127.1(2) . . ?
N10 C11 C19 124.1(2) . . ?
N12 C11 C19 108.8(2) . . ?
N20 C13 N12 128.1(2) . . ?
N20 C13 C14 123.0(3) . . ?
N12 C13 C14 108.9(2) . . ?
C15 C14 C19 122.1(2) . . ?
C15 C14 C13 130.7(3) . . ?
C19 C14 C13 107.1(2) . . ?
C16 C15 C14 116.9(3) . . ?
C16 C15 H15 121.6 . . ?
C14 C15 H15 121.6 . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C18 121.8(3) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C19 117.2(3) . . ?
C17 C18 H18 121.4 . . ?
C19 C18 H18 121.4 . . ?
C18 C19 C14 120.5(3) . . ?
C18 C19 C11 132.8(3) . . ?
C14 C19 C11 106.6(2) . . ?
N20 C21 N22 126.8(3) . . ?
N20 C21 C29 123.2(3) . . ?
N22 C21 C29 109.9(2) . . ?
N30 C23 N22 126.6(3) . . ?
N30 C23 C24 124.1(2) . . ?
N22 C23 C24 109.3(2) . . ?
C25 C24 C29 120.5(3) . . ?
C25 C24 C23 132.3(3) . . ?
C29 C24 C23 107.2(2) . . ?
C26 C25 C24 117.9(3) . . ?
C26 C25 H25 121.1 . . ?
C24 C25 H25 121.1 . . ?
C25 C26 C27 121.1(3) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 121.3(3) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C29 C28 C27 117.7(3) . . ?
C29 C28 H28 121.2 . . ?
C27 C28 H28 121.2 . . ?
C28 C29 C24 121.5(3) . . ?
C28 C29 C21 132.4(3) . . ?
C24 C29 C21 106.1(2) . . ?
N30 C31 N32 127.9(2) . . ?
N30 C31 C39 123.8(2) . . ?
N32 C31 C39 108.3(3) . . ?
N40 C33 N32 127.5(2) . . ?
N40 C33 C34 123.7(3) . . ?
N32 C33 C34 108.7(2) . . ?
C35 C34 C39 120.9(3) . . ?
C35 C34 C33 132.3(3) . . ?
C39 C34 C33 106.8(2) . . ?
C36 C35 C34 117.4(3) . . ?
C36 C35 H35 121.3 . . ?
C34 C35 H35 121.3 . . ?
C35 C36 C37 122.0(3) . . ?
C35 C36 H36 119 . . ?
C37 C36 H36 119 . . ?
C38 C37 C36 120.9(3) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C37 C38 C39 117.5(3) . . ?
C37 C38 H38 121.2 . . ?
C39 C38 H38 121.2 . . ?
C34 C39 C38 121.3(3) . . ?
C34 C39 C31 107.4(2) . . ?
C38 C39 C31 131.3(3) . . ?
N41 C42 C47 119.2(3) . . ?
N41 C42 C43 120.1(3) . . ?
C47 C42 C43 120.7(3) . . ?
C44 C43 C42 117.7(3) . . ?
C44 C43 C48 121.6(3) . . ?
C42 C43 C48 120.6(3) . . ?
C45 C44 C43 121.5(4) . . ?
C45 C44 H44 119.2 . . ?
C43 C44 H44 119.2 . . ?
C46 C45 C44 119.9(3) . . ?
C46 C45 H45 120.1 . . ?
C44 C45 H45 120.1 . . ?
C45 C46 C47 121.8(4) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C46 C47 C42 118.3(3) . . ?
C46 C47 C51 121.4(3) . . ?
C42 C47 C51 120.3(3) . . ?
C49 C48 C43 112.3(3) . . ?
C49 C48 C50 110.4(3) . . ?
C43 C48 C50 112.2(3) . . ?
C49 C48 H48 107.2 . . ?
C43 C48 H48 107.2 . . ?
C50 C48 H48 107.2 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 C53 115.3(4) . . ?
C47 C51 C52 110.2(3) . . ?
C53 C51 C52 109.3(3) . . ?
C47 C51 H51 107.2 . . ?
C53 C51 H51 107.2 . . ?
C52 C51 H51 107.2 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C2 N1 C9 108.2(2) . . ?
C2 N1 Ti1 124.45(18) . . ?
C9 N1 Ti1 123.78(19) . . ?
C11 N10 C9 123.5(2) . . ?
C13 N12 C11 108.5(2) . . ?
C13 N12 Ti1 123.78(17) . . ?
C11 N12 Ti1 124.30(18) . . ?
C13 N20 C21 123.6(2) . . ?
C21 N22 C23 107.4(2) . . ?
C21 N22 Ti1 124.54(17) . . ?
C23 N22 Ti1 125.30(18) . . ?
C31 N30 C23 123.6(2) . . ?
C31 N32 C33 108.8(2) . . ?
C31 N32 Ti1 124.53(19) . . ?
C33 N32 Ti1 124.44(18) . . ?
C33 N40 C2 123.5(2) . . ?
C42 N41 Ti1 179.0(2) . . ?
N41 Ti1 N12 105.99(10) . . ?
N41 Ti1 N1 105.99(10) . . ?
N12 Ti1 N1 85.19(9) . . ?
N41 Ti1 N22 107.65(11) . . ?
N12 Ti1 N22 85.39(9) . . ?
N1 Ti1 N22 146.36(10) . . ?
N41 Ti1 N32 107.67(10) . . ?
N12 Ti1 N32 146.34(10) . . ?
N1 Ti1 N32 85.34(9) . . ?
N22 Ti1 N32 84.85(9) . . ?
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
C2 N40 1.341(3) . ?
C2 N1 1.379(3) . ?
C2 C3 1.452(4) . ?
C3 C4 1.392(4) . ?
C3 C8 1.397(4) . ?
C4 C5 1.378(4) . ?
C4 H4 0.95 . ?
C5 C6 1.402(4) . ?
C5 H5 0.95 . ?
C6 C7 1.368(4) . ?
C6 H6 0.95 . ?
C7 C8 1.380(4) . ?
C7 H7 0.95 . ?
C8 C9 1.458(4) . ?
C9 N10 1.332(4) . ?
C9 N1 1.384(3) . ?
C11 N10 1.327(4) . ?
C11 N12 1.388(3) . ?
C11 C19 1.455(4) . ?
C13 N20 1.325(4) . ?
C13 N12 1.373(4) . ?
C13 C14 1.455(4) . ?
C14 C15 1.391(4) . ?
C14 C19 1.395(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.95 . ?
C16 C17 1.389(4) . ?
C16 H16 0.95 . ?
C17 C18 1.389(4) . ?
C17 H17 0.95 . ?
C18 C19 1.392(4) . ?
C18 H18 0.95 . ?
C21 N20 1.337(3) . ?
C21 N22 1.379(3) . ?
C21 C29 1.452(4) . ?
C23 N30 1.334(3) . ?
C23 N22 1.386(3) . ?
C23 C24 1.447(4) . ?
C24 C25 1.390(4) . ?
C24 C29 1.399(4) . ?
C25 C26 1.378(4) . ?
C25 H25 0.95 . ?
C26 C27 1.394(4) . ?
C26 H26 0.95 . ?
C27 C28 1.381(4) . ?
C27 H27 0.95 . ?
C28 C29 1.378(4) . ?
C28 H28 0.95 . ?
C31 N30 1.326(4) . ?
C31 N32 1.382(3) . ?
C31 C39 1.461(4) . ?
C33 N40 1.333(4) . ?
C33 N32 1.384(4) . ?
C33 C34 1.460(4) . ?
C34 C35 1.391(4) . ?
C34 C39 1.391(4) . ?
C35 C36 1.377(4) . ?
C35 H35 0.95 . ?
C36 C37 1.391(4) . ?
C36 H36 0.95 . ?
C37 C38 1.380(4) . ?
C37 H37 0.95 . ?
C38 C39 1.393(4) . ?
C38 H38 0.95 . ?
C42 N41 1.393(4) . ?
C42 C47 1.419(4) . ?
C42 C43 1.421(4) . ?
C43 C44 1.393(4) . ?
C43 C48 1.518(4) . ?
C44 C45 1.387(5) . ?
C44 H44 0.95 . ?
C45 C46 1.374(5) . ?
C45 H45 0.95 . ?
C46 C47 1.382(5) . ?
C46 H46 0.95 . ?
C47 C51 1.505(5) . ?
C48 C49 1.504(5) . ?
C48 C50 1.543(5) . ?
C48 H48 1 . ?
C49 H49A 0.98 . ?
C49 H49B 0.98 . ?
C49 H49C 0.98 . ?
C50 H50A 0.98 . ?
C50 H50B 0.98 . ?
C50 H50C 0.98 . ?
C51 C53 1.521(5) . ?
C51 C52 1.528(5) . ?
C51 H51 1 . ?
C52 H52A 0.98 . ?
C52 H52B 0.98 . ?
C52 H52C 0.98 . ?
C53 H53A 0.98 . ?
C53 H53B 0.98 . ?
C53 H53C 0.98 . ?
N1 Ti1 2.056(2) . ?
N12 Ti1 2.054(2) . ?
N22 Ti1 2.057(2) . ?
N32 Ti1 2.063(2) . ?
N41 Ti1 1.712(2) . ?
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
N40 C2 C3 C4 -1.3(5) . . . . ?
N1 C2 C3 C4 177.8(3) . . . . ?
N40 C2 C3 C8 179.5(3) . . . . ?
N1 C2 C3 C8 -1.4(3) . . . . ?
C8 C3 C4 C5 1.2(4) . . . . ?
C2 C3 C4 C5 -177.9(3) . . . . ?
C3 C4 C5 C6 -1.7(5) . . . . ?
C4 C5 C6 C7 0.9(5) . . . . ?
C5 C6 C7 C8 0.4(5) . . . . ?
C6 C7 C8 C3 -0.9(5) . . . . ?
C6 C7 C8 C9 178.1(3) . . . . ?
C4 C3 C8 C7 0.1(4) . . . . ?
C2 C3 C8 C7 179.4(3) . . . . ?
C4 C3 C8 C9 -179.1(3) . . . . ?
C2 C3 C8 C9 0.2(3) . . . . ?
C7 C8 C9 N10 0.2(5) . . . . ?
C3 C8 C9 N10 179.3(3) . . . . ?
C7 C8 C9 N1 -178.0(3) . . . . ?
C3 C8 C9 N1 1.1(3) . . . . ?
N20 C13 C14 C15 3.2(5) . . . . ?
N12 C13 C14 C15 -175.7(3) . . . . ?
N20 C13 C14 C19 -179.5(3) . . . . ?
N12 C13 C14 C19 1.5(3) . . . . ?
C19 C14 C15 C16 0.3(4) . . . . ?
C13 C14 C15 C16 177.2(3) . . . . ?
C14 C15 C16 C17 1.1(4) . . . . ?
C15 C16 C17 C18 -0.9(5) . . . . ?
C16 C17 C18 C19 -0.6(5) . . . . ?
C17 C18 C19 C14 2.0(4) . . . . ?
C17 C18 C19 C11 -176.3(3) . . . . ?
C15 C14 C19 C18 -1.8(4) . . . . ?
C13 C14 C19 C18 -179.4(3) . . . . ?
C15 C14 C19 C11 176.9(3) . . . . ?
C13 C14 C19 C11 -0.7(3) . . . . ?
N10 C11 C19 C18 -0.6(5) . . . . ?
N12 C11 C19 C18 178.1(3) . . . . ?
N10 C11 C19 C14 -179.1(3) . . . . ?
N12 C11 C19 C14 -0.3(3) . . . . ?
N30 C23 C24 C25 1.4(5) . . . . ?
N22 C23 C24 C25 -178.1(3) . . . . ?
N30 C23 C24 C29 -179.5(3) . . . . ?
N22 C23 C24 C29 0.9(3) . . . . ?
C29 C24 C25 C26 -0.4(4) . . . . ?
C23 C24 C25 C26 178.6(3) . . . . ?
C24 C25 C26 C27 0.7(4) . . . . ?
C25 C26 C27 C28 -0.4(5) . . . . ?
C26 C27 C28 C29 -0.3(4) . . . . ?
C27 C28 C29 C24 0.7(4) . . . . ?
C27 C28 C29 C21 -178.7(3) . . . . ?
C25 C24 C29 C28 -0.3(4) . . . . ?
C23 C24 C29 C28 -179.5(3) . . . . ?
C25 C24 C29 C21 179.2(3) . . . . ?
C23 C24 C29 C21 0.0(3) . . . . ?
N20 C21 C29 C28 -0.7(5) . . . . ?
N22 C21 C29 C28 178.6(3) . . . . ?
N20 C21 C29 C24 179.9(3) . . . . ?
N22 C21 C29 C24 -0.9(3) . . . . ?
N40 C33 C34 C35 -0.6(5) . . . . ?
N32 C33 C34 C35 -179.1(3) . . . . ?
N40 C33 C34 C39 179.7(3) . . . . ?
N32 C33 C34 C39 1.2(3) . . . . ?
C39 C34 C35 C36 -1.0(4) . . . . ?
C33 C34 C35 C36 179.4(3) . . . . ?
C34 C35 C36 C37 1.1(5) . . . . ?
C35 C36 C37 C38 -0.6(5) . . . . ?
C36 C37 C38 C39 0.0(5) . . . . ?
C35 C34 C39 C38 0.4(4) . . . . ?
C33 C34 C39 C38 -179.9(3) . . . . ?
C35 C34 C39 C31 -180.0(3) . . . . ?
C33 C34 C39 C31 -0.3(3) . . . . ?
C37 C38 C39 C34 0.1(4) . . . . ?
C37 C38 C39 C31 -179.4(3) . . . . ?
N30 C31 C39 C34 179.8(3) . . . . ?
N32 C31 C39 C34 -0.8(3) . . . . ?
N30 C31 C39 C38 -0.6(5) . . . . ?
N32 C31 C39 C38 178.9(3) . . . . ?
N41 C42 C43 C44 -176.8(3) . . . . ?
C47 C42 C43 C44 2.7(4) . . . . ?
N41 C42 C43 C48 2.1(4) . . . . ?
C47 C42 C43 C48 -178.5(3) . . . . ?
C42 C43 C44 C45 -1.2(5) . . . . ?
C48 C43 C44 C45 179.9(3) . . . . ?
C43 C44 C45 C46 -1.5(5) . . . . ?
C44 C45 C46 C47 2.9(6) . . . . ?
C45 C46 C47 C42 -1.4(5) . . . . ?
C45 C46 C47 C51 177.5(3) . . . . ?
N41 C42 C47 C46 178.1(3) . . . . ?
C43 C42 C47 C46 -1.4(4) . . . . ?
N41 C42 C47 C51 -0.9(4) . . . . ?
C43 C42 C47 C51 179.6(3) . . . . ?
C44 C43 C48 C49 75.4(4) . . . . ?
C42 C43 C48 C49 -103.4(4) . . . . ?
C44 C43 C48 C50 -49.7(4) . . . . ?
C42 C43 C48 C50 131.5(3) . . . . ?
C46 C47 C51 C53 39.9(4) . . . . ?
C42 C47 C51 C53 -141.2(3) . . . . ?
C46 C47 C51 C52 -84.5(4) . . . . ?
C42 C47 C51 C52 94.5(3) . . . . ?
N40 C2 N1 C9 -178.8(3) . . . . ?
C3 C2 N1 C9 2.1(3) . . . . ?
N40 C2 N1 Ti1 21.8(4) . . . . ?
C3 C2 N1 Ti1 -157.24(19) . . . . ?
N10 C9 N1 C2 179.9(3) . . . . ?
C8 C9 N1 C2 -2.0(3) . . . . ?
N10 C9 N1 Ti1 -20.5(4) . . . . ?
C8 C9 N1 Ti1 157.52(18) . . . . ?
N12 C11 N10 C9 0.4(5) . . . . ?
C19 C11 N10 C9 178.9(3) . . . . ?
N1 C9 N10 C11 -0.3(5) . . . . ?
C8 C9 N10 C11 -178.1(3) . . . . ?
N20 C13 N12 C11 179.4(3) . . . . ?
C14 C13 N12 C11 -1.7(3) . . . . ?
N20 C13 N12 Ti1 -20.9(4) . . . . ?
C14 C13 N12 Ti1 157.97(18) . . . . ?
N10 C11 N12 C13 180.0(3) . . . . ?
C19 C11 N12 C13 1.3(3) . . . . ?
N10 C11 N12 Ti1 20.4(4) . . . . ?
C19 C11 N12 Ti1 -158.28(18) . . . . ?
N12 C13 N20 C21 0.5(5) . . . . ?
C14 C13 N20 C21 -178.3(3) . . . . ?
N22 C21 N20 C13 0.8(4) . . . . ?
C29 C21 N20 C13 179.9(3) . . . . ?
N20 C21 N22 C23 -179.3(3) . . . . ?
C29 C21 N22 C23 1.4(3) . . . . ?
N20 C21 N22 Ti1 18.6(4) . . . . ?
C29 C21 N22 Ti1 -160.59(18) . . . . ?
N30 C23 N22 C21 179.0(3) . . . . ?
C24 C23 N22 C21 -1.5(3) . . . . ?
N30 C23 N22 Ti1 -19.2(4) . . . . ?
C24 C23 N22 Ti1 160.41(19) . . . . ?
N32 C31 N30 C23 2.3(5) . . . . ?
C39 C31 N30 C23 -178.4(3) . . . . ?
N22 C23 N30 C31 -1.5(4) . . . . ?
C24 C23 N30 C31 179.0(3) . . . . ?
N30 C31 N32 C33 -179.0(3) . . . . ?
C39 C31 N32 C33 1.6(3) . . . . ?
N30 C31 N32 Ti1 17.5(4) . . . . ?
C39 C31 N32 Ti1 -161.91(18) . . . . ?
N40 C33 N32 C31 179.8(3) . . . . ?
C34 C33 N32 C31 -1.7(3) . . . . ?
N40 C33 N32 Ti1 -16.7(4) . . . . ?
C34 C33 N32 Ti1 161.76(17) . . . . ?
N32 C33 N40 C2 -2.0(4) . . . . ?
C34 C33 N40 C2 179.7(3) . . . . ?
N1 C2 N40 C33 -0.7(4) . . . . ?
C3 C2 N40 C33 178.2(3) . . . . ?
C47 C42 N41 Ti1 43(12) . . . . ?
C43 C42 N41 Ti1 -137(12) . . . . ?
C42 N41 Ti1 N12 89(12) . . . . ?
C42 N41 Ti1 N1 18E1(10) . . . . ?
C42 N41 Ti1 N22 -1(12) . . . . ?
C42 N41 Ti1 N32 -91(12) . . . . ?
C13 N12 Ti1 N41 -79.5(2) . . . . ?
C11 N12 Ti1 N41 77.0(2) . . . . ?
C13 N12 Ti1 N1 175.2(2) . . . . ?
C11 N12 Ti1 N1 -28.3(2) . . . . ?
C13 N12 Ti1 N22 27.5(2) . . . . ?
C11 N12 Ti1 N22 -175.9(2) . . . . ?
C13 N12 Ti1 N32 101.1(3) . . . . ?
C11 N12 Ti1 N32 -102.4(3) . . . . ?
C2 N1 Ti1 N41 79.2(2) . . . . ?
C9 N1 Ti1 N41 -77.1(2) . . . . ?
C2 N1 Ti1 N12 -175.5(2) . . . . ?
C9 N1 Ti1 N12 28.2(2) . . . . ?
C2 N1 Ti1 N22 -101.3(2) . . . . ?
C9 N1 Ti1 N22 102.4(2) . . . . ?
C2 N1 Ti1 N32 -27.9(2) . . . . ?
C9 N1 Ti1 N32 175.8(2) . . . . ?
C21 N22 Ti1 N41 78.6(2) . . . . ?
C23 N22 Ti1 N41 -80.3(2) . . . . ?
C21 N22 Ti1 N12 -26.7(2) . . . . ?
C23 N22 Ti1 N12 174.4(2) . . . . ?
C21 N22 Ti1 N1 -100.9(3) . . . . ?
C23 N22 Ti1 N1 100.2(2) . . . . ?
C21 N22 Ti1 N32 -174.5(2) . . . . ?
C23 N22 Ti1 N32 26.7(2) . . . . ?
C31 N32 Ti1 N41 81.2(2) . . . . ?
C33 N32 Ti1 N41 -79.7(2) . . . . ?
C31 N32 Ti1 N12 -99.4(3) . . . . ?
C33 N32 Ti1 N12 99.7(3) . . . . ?
C31 N32 Ti1 N1 -173.5(2) . . . . ?
C33 N32 Ti1 N1 25.6(2) . . . . ?
C31 N32 Ti1 N22 -25.7(2) . . . . ?
C33 N32 Ti1 N22 173.4(2) . . . . ?
