#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336315.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_4336315
loop_
_publ_author_name
'Jorge Caballo'
'Mariano González-Moreiras'
'Miguel Mena'
'Adrián Pérez-Redondo'
'Carlos Yélamos'
_publ_contact_author_address
;
Departamento de Química Orgánica y Química Inorgánica
Universidad de Alcalá
28871, Alcalá de Henares
Madrid, Spain
;
_publ_contact_author_email       adrian.perez@uah.es
_publ_contact_author_fax         '+34 91 8854683'
_publ_contact_author_name        'Pérez-Redondo, Adrián'
_publ_contact_author_phone       '+34 91 8854677'
_publ_section_title
;
 Reactivity with Electrophiles of Imido Groups Supported on Trinuclear
 Titanium Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11519
_journal_page_last               11529
_journal_paper_doi               10.1021/ic4018294
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H55 K N4 Si Ti3'
_chemical_formula_sum            'C33 H55 K N4 Si Ti3'
_chemical_formula_weight         718.7
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2013-07-04T15:40:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 115.38(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.918(9)
_cell_length_b                   16.303(8)
_cell_length_c                   22.856(11)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3676(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.125
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73443
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.035
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+0.7340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1552
_reflns_number_gt                4692
_reflns_number_total             8449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018294_si_002_1.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336315
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
C1 C 0.3568(5) -0.1459(3) -0.1912(2) 0.0527(13) Uani 1 1 d .
H1A H 0.4064 -0.1479 -0.2182 0.079 Uiso 1 1 calc R
H1B H 0.4188 -0.1301 -0.147 0.079 Uiso 1 1 calc R
H1C H 0.2836 -0.1054 -0.2091 0.079 Uiso 1 1 calc R
C2 C 0.4261(5) -0.3173(3) -0.1381(2) 0.0565(14) Uani 1 1 d .
H2A H 0.3898 -0.3635 -0.1231 0.085 Uiso 1 1 calc R
H2B H 0.4901 -0.2865 -0.1007 0.085 Uiso 1 1 calc R
H2C H 0.473 -0.3381 -0.1633 0.085 Uiso 1 1 calc R
C3 C 0.1767(6) -0.2308(3) -0.1453(2) 0.0553(14) Uani 1 1 d .
H3A H 0.142 -0.1745 -0.1527 0.083 Uiso 1 1 calc R
H3B H 0.2318 -0.2394 -0.0989 0.083 Uiso 1 1 calc R
H3C H 0.1005 -0.2694 -0.1609 0.083 Uiso 1 1 calc R
C11 C -0.0996(4) -0.4805(2) -0.32264(18) 0.0294(9) Uani 1 1 d .
C12 C -0.0868(4) -0.4504(2) -0.26275(19) 0.0303(9) Uani 1 1 d .
C13 C 0.0530(4) -0.4536(3) -0.21874(17) 0.0305(10) Uani 1 1 d .
C14 C 0.1246(4) -0.4864(3) -0.25254(19) 0.0310(9) Uani 1 1 d .
C15 C 0.0285(4) -0.5022(2) -0.31724(18) 0.0298(9) Uani 1 1 d .
C16 C -0.2284(4) -0.4875(3) -0.3841(2) 0.0428(12) Uani 1 1 d .
H16A H -0.3057 -0.4714 -0.3756 0.064 Uiso 1 1 calc R
H16B H -0.2402 -0.5443 -0.3996 0.064 Uiso 1 1 calc R
H16C H -0.2231 -0.4512 -0.4171 0.064 Uiso 1 1 calc R
C17 C -0.1994(5) -0.4216(3) -0.2466(2) 0.0470(12) Uani 1 1 d .
H17A H -0.2721 -0.3979 -0.2853 0.07 Uiso 1 1 calc R
H17B H -0.1646 -0.38 -0.2124 0.07 Uiso 1 1 calc R
H17C H -0.235 -0.4682 -0.2315 0.07 Uiso 1 1 calc R
C18 C 0.1080(5) -0.4395(3) -0.14688(19) 0.0484(13) Uani 1 1 d .
H18A H 0.0546 -0.3968 -0.1383 0.073 Uiso 1 1 calc R
H18B H 0.2028 -0.4219 -0.1301 0.073 Uiso 1 1 calc R
H18C H 0.1025 -0.4905 -0.1255 0.073 Uiso 1 1 calc R
C19 C 0.2727(4) -0.5063(3) -0.2246(2) 0.0463(12) Uani 1 1 d .
H19A H 0.2844 -0.5652 -0.2291 0.07 Uiso 1 1 calc R
H19B H 0.3153 -0.4914 -0.1786 0.07 Uiso 1 1 calc R
H19C H 0.3153 -0.4754 -0.2477 0.07 Uiso 1 1 calc R
C20 C 0.0604(5) -0.5389(3) -0.3697(2) 0.0440(12) Uani 1 1 d .
H20A H -0.0013 -0.5848 -0.39 0.066 Uiso 1 1 calc R
H20B H 0.1542 -0.5588 -0.3507 0.066 Uiso 1 1 calc R
H20C H 0.0491 -0.4971 -0.4024 0.066 Uiso 1 1 calc R
C21 C 0.2705(4) -0.2988(3) -0.4263(2) 0.0343(10) Uani 1 1 d .
C22 C 0.2679(4) -0.2121(3) -0.42745(19) 0.0312(10) Uani 1 1 d .
C23 C 0.3588(4) -0.1828(3) -0.3656(2) 0.0331(10) Uani 1 1 d .
C24 C 0.4213(4) -0.2519(3) -0.32687(19) 0.0325(10) Uani 1 1 d .
C25 C 0.3658(4) -0.3235(3) -0.3635(2) 0.0334(10) Uani 1 1 d .
C26 C 0.1953(5) -0.3564(3) -0.4806(2) 0.0427(11) Uani 1 1 d .
H26A H 0.1382 -0.3925 -0.4685 0.064 Uiso 1 1 calc R
H26B H 0.26 -0.3895 -0.4897 0.064 Uiso 1 1 calc R
H26C H 0.1382 -0.325 -0.5193 0.064 Uiso 1 1 calc R
C27 C 0.1915(5) -0.1580(3) -0.4848(2) 0.0448(12) Uani 1 1 d .
H27A H 0.2557 -0.1297 -0.4974 0.067 Uiso 1 1 calc R
H27B H 0.1391 -0.1175 -0.4734 0.067 Uiso 1 1 calc R
H27C H 0.1299 -0.1916 -0.5211 0.067 Uiso 1 1 calc R
C28 C 0.3878(5) -0.0939(3) -0.3483(2) 0.0453(12) Uani 1 1 d .
H28A H 0.4568 -0.0891 -0.3035 0.068 Uiso 1 1 calc R
H28B H 0.3045 -0.0664 -0.3526 0.068 Uiso 1 1 calc R
H28C H 0.421 -0.0681 -0.3774 0.068 Uiso 1 1 calc R
C29 C 0.5453(4) -0.2504(3) -0.2626(2) 0.0507(13) Uani 1 1 d .
H29A H 0.5395 -0.2951 -0.2352 0.076 Uiso 1 1 calc R
H29B H 0.5499 -0.1977 -0.2411 0.076 Uiso 1 1 calc R
H29C H 0.6268 -0.2575 -0.2698 0.076 Uiso 1 1 calc R
C30 C 0.4058(5) -0.4102(3) -0.3427(2) 0.0449(12) Uani 1 1 d .
H30A H 0.4657 -0.4302 -0.3615 0.067 Uiso 1 1 calc R
H30B H 0.3244 -0.4447 -0.3576 0.067 Uiso 1 1 calc R
H30C H 0.4534 -0.4127 -0.2954 0.067 Uiso 1 1 calc R
C31 C -0.2433(4) -0.1668(3) -0.50550(18) 0.0340(10) Uani 1 1 d .
C32 C -0.2178(4) -0.2396(3) -0.53181(17) 0.0294(9) Uani 1 1 d .
C33 C -0.2828(4) -0.3049(3) -0.51546(18) 0.0317(10) Uani 1 1 d .
C34 C -0.3488(4) -0.2726(3) -0.47905(18) 0.0311(10) Uani 1 1 d .
C35 C -0.3225(4) -0.1867(3) -0.47252(19) 0.0362(10) Uani 1 1 d .
C36 C -0.2027(5) -0.0828(3) -0.5158(2) 0.0510(13) Uani 1 1 d .
H36A H -0.2657 -0.0629 -0.5586 0.077 Uiso 1 1 calc R
H36B H -0.1106 -0.0844 -0.513 0.077 Uiso 1 1 calc R
H36C H -0.205 -0.0459 -0.4824 0.077 Uiso 1 1 calc R
C37 C -0.1541(5) -0.2456(3) -0.5776(2) 0.0473(12) Uani 1 1 d .
H37A H -0.0982 -0.2953 -0.5681 0.071 Uiso 1 1 calc R
H37B H -0.0971 -0.1974 -0.5728 0.071 Uiso 1 1 calc R
H37C H -0.225 -0.2483 -0.6221 0.071 Uiso 1 1 calc R
C38 C -0.2885(5) -0.3915(3) -0.5397(2) 0.0450(12) Uani 1 1 d .
H38A H -0.3245 -0.3911 -0.587 0.068 Uiso 1 1 calc R
H38B H -0.3477 -0.4246 -0.5267 0.068 Uiso 1 1 calc R
H38C H -0.1971 -0.415 -0.5211 0.068 Uiso 1 1 calc R
C39 C -0.4414(4) -0.3157(3) -0.4569(2) 0.0517(13) Uani 1 1 d .
H39A H -0.4007 -0.3169 -0.4094 0.078 Uiso 1 1 calc R
H39B H -0.4562 -0.372 -0.4735 0.078 Uiso 1 1 calc R
H39C H -0.5283 -0.2868 -0.4731 0.078 Uiso 1 1 calc R
C40 C -0.3789(5) -0.1299(4) -0.4394(2) 0.0614(16) Uani 1 1 d .
H40A H -0.3222 -0.0806 -0.4255 0.092 Uiso 1 1 calc R
H40B H -0.3802 -0.1573 -0.4015 0.092 Uiso 1 1 calc R
H40C H -0.4715 -0.1144 -0.4693 0.092 Uiso 1 1 calc R
K1 K 0.00050(11) -0.13486(6) -0.27748(5) 0.0432(3) Uani 1 1 d .
N1 N 0.0369(3) -0.33805(19) -0.38685(13) 0.0232(7) Uani 1 1 d .
N12 N 0.1879(3) -0.2829(2) -0.26729(14) 0.0269(8) Uani 1 1 d .
N13 N -0.1201(3) -0.2808(2) -0.33622(15) 0.0276(8) Uani 1 1 d .
N23 N 0.0395(3) -0.1764(2) -0.38607(15) 0.0258(7) Uani 1 1 d .
Si1 Si 0.28379(12) -0.24840(8) -0.19022(5) 0.0348(3) Uani 1 1 d .
Ti1 Ti 0.02517(7) -0.35359(4) -0.30633(3) 0.02470(18) Uani 1 1 d .
Ti2 Ti 0.17772(7) -0.25839(4) -0.35327(3) 0.02462(18) Uani 1 1 d .
Ti3 Ti -0.10641(7) -0.25512(4) -0.41352(3) 0.02503(18) Uani 1 1 d .
H23 H 0.036(5) -0.137(3) -0.413(2) 0.053(15) Uiso 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'
K K 0.2009 0.2494 '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'
Si Si 0.0817 0.0704 '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
-1 0 -5 0.058
1 0 4 0.04
-1 0 1 0.169
1 0 -1 0.149
0 -1 0 0.117
0 1 0 0.014
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
C15 C11 C12 109.0(3) . .
C15 C11 C16 124.2(4) . .
C12 C11 C16 126.8(4) . .
C15 C11 Ti1 74.1(2) . .
C12 C11 Ti1 74.7(2) . .
C16 C11 Ti1 116.6(3) . .
C15 C11 K1 74.0(2) . 2_544
C12 C11 K1 73.8(2) . 2_544
C16 C11 K1 119.5(3) . 2_544
Ti1 C11 K1 123.87(15) . 2_544
C11 C12 C13 107.8(4) . .
C11 C12 C17 126.8(4) . .
C13 C12 C17 125.4(4) . .
C11 C12 Ti1 71.8(2) . .
C13 C12 Ti1 75.0(2) . .
C17 C12 Ti1 120.1(3) . .
C11 C12 K1 81.0(2) . 2_544
C13 C12 K1 70.4(2) . 2_544
C17 C12 K1 113.5(3) . 2_544
Ti1 C12 K1 126.20(15) . 2_544
C14 C13 C12 107.7(3) . .
C14 C13 C18 126.6(4) . .
C12 C13 C18 124.8(4) . .
C14 C13 Ti1 73.4(2) . .
C12 C13 Ti1 71.6(2) . .
C18 C13 Ti1 129.0(3) . .
C14 C13 K1 76.1(2) . 2_544
C12 C13 K1 83.1(2) . 2_544
C18 C13 K1 99.4(3) . 2_544
Ti1 C13 K1 131.56(15) . 2_544
C13 C14 C15 107.5(4) . .
C13 C14 C19 126.6(4) . .
C15 C14 C19 125.8(4) . .
C13 C14 Ti1 73.6(2) . .
C15 C14 Ti1 71.0(2) . .
C19 C14 Ti1 124.1(3) . .
C13 C14 K1 76.5(2) . 2_544
C15 C14 K1 83.5(2) . 2_544
C19 C14 K1 104.0(3) . 2_544
Ti1 C14 K1 131.89(17) . 2_544
C11 C15 C14 108.1(3) . .
C11 C15 C20 126.5(4) . .
C14 C15 C20 125.4(4) . .
C11 C15 Ti1 72.5(2) . .
C14 C15 Ti1 75.5(2) . .
C20 C15 Ti1 119.7(3) . .
C11 C15 K1 81.0(2) . 2_544
C14 C15 K1 70.1(2) . 2_544
C20 C15 K1 113.4(3) . 2_544
Ti1 C15 K1 126.72(15) . 2_544
C22 C21 C25 107.5(4) . .
C22 C21 C26 127.9(4) . .
C25 C21 C26 124.5(4) . .
C22 C21 Ti2 74.1(2) . .
C25 C21 Ti2 73.6(2) . .
C26 C21 Ti2 120.6(3) . .
C21 C22 C23 108.6(4) . .
C21 C22 C27 127.0(4) . .
C23 C22 C27 124.2(4) . .
C21 C22 Ti2 71.7(2) . .
C23 C22 Ti2 74.2(2) . .
C27 C22 Ti2 123.7(3) . .
C24 C23 C22 107.4(4) . .
C24 C23 C28 127.9(4) . .
C22 C23 C28 124.6(4) . .
C24 C23 Ti2 73.9(2) . .
C22 C23 Ti2 71.9(2) . .
C28 C23 Ti2 123.1(3) . .
C25 C24 C23 108.6(3) . .
C25 C24 C29 124.5(4) . .
C23 C24 C29 125.9(4) . .
C25 C24 Ti2 71.1(2) . .
C23 C24 Ti2 72.6(2) . .
C29 C24 Ti2 131.4(3) . .
C24 C25 C21 107.9(4) . .
C24 C25 C30 126.9(4) . .
C21 C25 C30 125.1(4) . .
C24 C25 Ti2 75.3(2) . .
C21 C25 Ti2 71.9(2) . .
C30 C25 Ti2 122.0(3) . .
C35 C31 C32 108.2(4) . .
C35 C31 C36 126.2(4) . .
C32 C31 C36 125.4(4) . .
C35 C31 Ti3 72.2(2) . .
C32 C31 Ti3 73.3(2) . .
C36 C31 Ti3 124.1(3) . .
C31 C32 C33 107.9(4) . .
C31 C32 C37 126.4(4) . .
C33 C32 C37 125.0(4) . .
C31 C32 Ti3 73.3(2) . .
C33 C32 Ti3 72.5(2) . .
C37 C32 Ti3 127.4(3) . .
C34 C33 C32 108.3(4) . .
C34 C33 C38 127.8(4) . .
C32 C33 C38 123.6(4) . .
C34 C33 Ti3 73.0(2) . .
C32 C33 Ti3 73.9(2) . .
C38 C33 Ti3 123.6(3) . .
C33 C34 C35 107.3(4) . .
C33 C34 C39 128.0(4) . .
C35 C34 C39 124.4(4) . .
C33 C34 Ti3 73.3(2) . .
C35 C34 Ti3 72.8(2) . .
C39 C34 Ti3 124.3(3) . .
C31 C35 C34 108.3(4) . .
C31 C35 C40 127.8(5) . .
C34 C35 C40 123.9(5) . .
C31 C35 Ti3 74.3(2) . .
C34 C35 Ti3 73.2(2) . .
C40 C35 Ti3 121.3(3) . .
N13 K1 N23 65.20(10) . .
N13 K1 C14 129.44(12) . 2_554
N23 K1 C14 131.34(11) . 2_554
N13 K1 C13 141.62(11) . 2_554
N23 K1 C13 108.44(11) . 2_554
C14 K1 C13 27.32(11) 2_554 2_554
N13 K1 N12 61.97(10) . .
N23 K1 N12 61.92(9) . .
C14 K1 N12 163.60(10) 2_554 .
C13 K1 N12 151.54(11) 2_554 .
N13 K1 C12 167.43(11) . 2_554
N23 K1 C12 110.52(11) . 2_554
C14 K1 C12 43.57(11) 2_554 2_554
C13 K1 C12 26.50(11) 2_554 2_554
N12 K1 C12 127.69(11) . 2_554
N13 K1 C15 138.64(11) . 2_554
N23 K1 C15 151.09(11) . 2_554
C14 K1 C15 26.48(10) 2_554 2_554
C13 K1 C15 43.46(10) 2_554 2_554
N12 K1 C15 137.22(10) . 2_554
C12 K1 C15 42.14(10) 2_554 2_554
N13 K1 C11 161.62(10) . 2_554
N23 K1 C11 133.17(11) . 2_554
C14 K1 C11 42.52(11) 2_554 2_554
C13 K1 C11 42.53(10) 2_554 2_554
N12 K1 C11 122.51(10) . 2_554
C12 K1 C11 25.18(10) 2_554 2_554
C15 K1 C11 25.04(10) 2_554 2_554
N13 K1 Si1 86.61(9) . .
N23 K1 Si1 86.71(9) . .
C14 K1 Si1 133.66(9) 2_554 .
C13 K1 Si1 131.69(9) 2_554 .
N12 K1 Si1 29.96(6) . .
C12 K1 Si1 105.23(9) 2_554 .
C15 K1 Si1 107.54(9) 2_554 .
C11 K1 Si1 93.63(9) 2_554 .
N13 K1 Ti3 33.25(7) . .
N23 K1 Ti3 34.21(7) . .
C14 K1 Ti3 131.08(9) 2_554 .
C13 K1 Ti3 123.32(8) 2_554 .
N12 K1 Ti3 65.24(7) . .
C12 K1 Ti3 138.52(8) 2_554 .
C15 K1 Ti3 156.08(9) 2_554 .
C11 K1 Ti3 163.68(8) 2_554 .
Si1 K1 Ti3 95.20(5) . .
N13 K1 Ti1 29.77(7) . .
N23 K1 Ti1 63.24(8) . .
C14 K1 Ti1 154.68(9) 2_554 .
C13 K1 Ti1 169.01(8) 2_554 .
N12 K1 Ti1 32.77(7) . .
C12 K1 Ti1 160.44(8) 2_554 .
C15 K1 Ti1 145.57(8) 2_554 .
C11 K1 Ti1 148.39(8) 2_554 .
Si1 K1 Ti1 57.25(4) . .
N13 K1 Ti2 62.66(8) . .
N23 K1 Ti2 30.32(7) . .
C14 K1 Ti2 158.06(9) 2_554 .
C13 K1 Ti2 131.00(9) 2_554 .
N12 K1 Ti2 32.03(6) . .
C12 K1 Ti2 120.19(9) 2_554 .
C15 K1 Ti2 156.47(9) 2_554 .
C11 K1 Ti2 131.81(9) 2_554 .
Si1 K1 Ti2 56.91(5) . .
Ti2 N1 Ti1 94.46(13) . .
Ti2 N1 Ti3 93.09(15) . .
Ti1 N1 Ti3 90.96(13) . .
Si1 N12 Ti2 135.3(2) . .
Si1 N12 Ti1 133.58(19) . .
Ti2 N12 Ti1 90.73(13) . .
Si1 N12 K1 85.08(13) . .
Ti2 N12 K1 90.78(12) . .
Ti1 N12 K1 89.05(12) . .
Ti1 N13 Ti3 95.09(15) . .
Ti1 N13 K1 102.49(14) . .
Ti3 N13 K1 92.92(13) . .
Ti2 N23 Ti3 93.73(16) . .
Ti2 N23 K1 102.57(14) . .
Ti3 N23 K1 91.80(13) . .
N12 Si1 C1 111.07(19) . .
N12 Si1 C2 115.5(2) . .
C1 Si1 C2 107.7(2) . .
N12 Si1 C3 111.3(2) . .
C1 Si1 C3 103.9(2) . .
C2 Si1 C3 106.6(2) . .
N12 Si1 K1 64.96(12) . .
C1 Si1 K1 77.93(17) . .
C2 Si1 K1 172.94(19) . .
C3 Si1 K1 67.48(17) . .
N13 Ti1 N1 87.73(14) . .
N13 Ti1 N12 104.70(15) . .
N1 Ti1 N12 86.52(13) . .
N13 Ti1 C11 98.84(16) . .
N1 Ti1 C11 103.32(13) . .
N12 Ti1 C11 154.85(13) . .
N13 Ti1 C15 130.10(15) . .
N1 Ti1 C15 91.32(13) . .
N12 Ti1 C15 125.05(14) . .
C11 Ti1 C15 33.43(14) . .
N13 Ti1 C12 93.71(15) . .
N1 Ti1 C12 136.48(14) . .
N12 Ti1 C12 134.28(13) . .
C11 Ti1 C12 33.48(13) . .
C15 Ti1 C12 55.54(13) . .
N13 Ti1 C14 148.90(14) . .
N1 Ti1 C14 113.18(14) . .
N12 Ti1 C14 99.53(14) . .
C11 Ti1 C14 55.33(14) . .
C15 Ti1 C14 33.50(13) . .
C12 Ti1 C14 55.22(14) . .
N13 Ti1 C13 120.15(15) . .
N1 Ti1 C13 145.20(14) . .
N12 Ti1 C13 103.97(14) . .
C11 Ti1 C13 55.35(13) . .
C15 Ti1 C13 55.32(13) . .
C12 Ti1 C13 33.40(13) . .
C14 Ti1 C13 33.00(13) . .
N13 Ti1 Ti3 42.78(10) . .
N1 Ti1 Ti3 45.12(10) . .
N12 Ti1 Ti3 94.97(10) . .
C11 Ti1 Ti3 108.44(10) . .
C15 Ti1 Ti3 120.80(10) . .
C12 Ti1 Ti3 125.02(11) . .
C14 Ti1 Ti3 153.14(10) . .
C13 Ti1 Ti3 158.27(10) . .
N13 Ti1 Ti2 93.40(12) . .
N1 Ti1 Ti2 42.62(10) . .
N12 Ti1 Ti2 44.37(10) . .
C11 Ti1 Ti2 143.39(10) . .
C15 Ti1 Ti2 118.26(10) . .
C12 Ti1 Ti2 172.77(10) . .
C14 Ti1 Ti2 117.64(11) . .
C13 Ti1 Ti2 141.25(11) . .
Ti3 Ti1 Ti2 60.48(5) . .
N13 Ti1 K1 47.74(11) . .
N1 Ti1 K1 94.86(10) . .
N12 Ti1 K1 58.18(10) . .
C11 Ti1 K1 141.48(11) . .
C15 Ti1 K1 173.27(10) . .
C12 Ti1 K1 117.78(10) . .
C14 Ti1 K1 143.78(10) . .
C13 Ti1 K1 119.03(10) . .
Ti3 Ti1 K1 62.78(4) . .
Ti2 Ti1 K1 68.35(4) . .
N1 Ti2 N23 87.34(15) . .
N1 Ti2 N12 87.36(13) . .
N23 Ti2 N12 103.40(14) . .
N1 Ti2 C21 92.35(14) . .
N23 Ti2 C21 114.77(15) . .
N12 Ti2 C21 141.79(15) . .
N1 Ti2 C25 103.58(15) . .
N23 Ti2 C25 146.29(15) . .
N12 Ti2 C25 108.81(14) . .
C21 Ti2 C25 34.52(14) . .
N1 Ti2 C22 115.54(13) . .
N23 Ti2 C22 89.84(15) . .
N12 Ti2 C22 154.31(14) . .
C21 Ti2 C22 34.22(15) . .
C25 Ti2 C22 56.59(15) . .
N1 Ti2 C23 148.19(13) . .
N23 Ti2 C23 98.25(16) . .
N12 Ti2 C23 121.10(14) . .
C21 Ti2 C23 56.82(15) . .
C25 Ti2 C23 56.40(15) . .
C22 Ti2 C23 33.89(13) . .
N1 Ti2 C24 136.72(15) . .
N23 Ti2 C24 130.80(16) . .
N12 Ti2 C24 99.89(14) . .
C21 Ti2 C24 56.38(14) . .
C25 Ti2 C24 33.66(14) . .
C22 Ti2 C24 55.74(14) . .
C23 Ti2 C24 33.48(14) . .
N1 Ti2 Ti3 44.19(10) . .
N23 Ti2 Ti3 43.37(11) . .
N12 Ti2 Ti3 94.10(11) . .
C21 Ti2 Ti3 111.93(11) . .
C25 Ti2 Ti3 140.37(11) . .
C22 Ti2 Ti3 110.31(11) . .
C23 Ti2 Ti3 135.44(11) . .
C24 Ti2 Ti3 165.99(10) . .
N1 Ti2 Ti1 42.92(9) . .
N23 Ti2 Ti1 92.21(12) . .
N12 Ti2 Ti1 44.90(10) . .
C21 Ti2 Ti1 127.90(11) . .
C25 Ti2 Ti1 117.63(11) . .
C22 Ti2 Ti1 158.15(10) . .
C23 Ti2 Ti1 164.71(10) . .
C24 Ti2 Ti1 133.29(11) . .
Ti3 Ti2 Ti1 59.00(5) . .
N1 Ti2 K1 93.79(11) . .
N23 Ti2 K1 47.11(10) . .
N12 Ti2 K1 57.19(10) . .
C21 Ti2 K1 160.42(11) . .
C25 Ti2 K1 157.49(11) . .
C22 Ti2 K1 127.65(11) . .
C23 Ti2 K1 112.97(11) . .
C24 Ti2 K1 126.04(11) . .
Ti3 Ti2 K1 61.88(5) . .
Ti1 Ti2 K1 66.82(5) . .
N13 Ti3 N23 103.27(15) . .
N13 Ti3 N1 85.88(14) . .
N23 Ti3 N1 85.41(15) . .
N13 Ti3 C35 100.04(15) . .
N23 Ti3 C35 110.19(16) . .
N1 Ti3 C35 161.19(14) . .
N13 Ti3 C34 92.80(15) . .
N23 Ti3 C34 143.71(15) . .
N1 Ti3 C34 128.58(14) . .
C35 Ti3 C34 34.05(15) . .
N13 Ti3 C33 118.32(15) . .
N23 Ti3 C33 137.39(15) . .
N1 Ti3 C33 105.43(14) . .
C35 Ti3 C33 56.03(15) . .
C34 Ti3 C33 33.75(14) . .
N13 Ti3 C32 148.73(14) . .
N23 Ti3 C32 103.86(14) . .
N1 Ti3 C32 111.50(13) . .
C35 Ti3 C32 55.73(14) . .
C34 Ti3 C32 55.96(14) . .
C33 Ti3 C32 33.63(14) . .
N13 Ti3 C31 132.05(15) . .
N23 Ti3 C31 90.17(15) . .
N1 Ti3 C31 141.58(14) . .
C35 Ti3 C31 33.48(15) . .
C34 Ti3 C31 55.95(14) . .
C33 Ti3 C31 55.67(15) . .
C32 Ti3 C31 33.39(13) . .
N13 Ti3 Ti1 42.13(10) . .
N23 Ti3 Ti1 93.17(11) . .
N1 Ti3 Ti1 43.92(9) . .
C35 Ti3 Ti1 140.49(12) . .
C34 Ti3 Ti1 119.51(11) . .
C33 Ti3 Ti1 123.46(11) . .
C32 Ti3 Ti1 149.34(10) . .
C31 Ti3 Ti1 173.94(11) . .
N13 Ti3 Ti2 92.92(11) . .
N23 Ti3 Ti2 42.90(11) . .
N1 Ti3 Ti2 42.72(10) . .
C35 Ti3 Ti2 152.66(12) . .
C34 Ti3 Ti2 169.05(11) . .
C33 Ti3 Ti2 135.82(11) . .
C32 Ti3 Ti2 117.65(11) . .
C31 Ti3 Ti2 124.81(11) . .
Ti1 Ti3 Ti2 60.52(4) . .
N13 Ti3 K1 53.83(11) . .
N23 Ti3 K1 53.99(10) . .
N1 Ti3 K1 101.34(10) . .
C35 Ti3 K1 96.49(11) . .
C34 Ti3 K1 118.85(11) . .
C33 Ti3 K1 151.50(11) . .
C32 Ti3 K1 138.98(11) . .
C31 Ti3 K1 106.65(11) . .
Ti1 Ti3 K1 71.49(5) . .
Ti2 Ti3 K1 71.98(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Si1 1.856(5) .
C2 Si1 1.874(5) .
C3 Si1 1.879(5) .
C11 C15 1.396(6) .
C11 C12 1.404(5) .
C11 C16 1.507(5) .
C11 Ti1 2.417(4) .
C11 K1 3.258(4) 2_544
C12 C13 1.423(6) .
C12 C17 1.503(6) .
C12 Ti1 2.454(4) .
C12 K1 3.168(4) 2_544
C13 C14 1.419(6) .
C13 C18 1.505(5) .
C13 Ti1 2.498(4) .
C13 K1 3.006(4) 2_544
C14 C15 1.423(6) .
C14 C19 1.497(6) .
C14 Ti1 2.496(4) .
C14 K1 3.000(4) 2_544
C15 C20 1.507(6) .
C15 Ti1 2.437(4) .
C15 K1 3.171(4) 2_544
C21 C22 1.414(6) .
C21 C25 1.424(6) .
C21 C26 1.490(6) .
C21 Ti2 2.387(4) .
C22 C23 1.418(6) .
C22 C27 1.502(6) .
C22 Ti2 2.418(4) .
C23 C24 1.415(6) .
C23 C28 1.499(6) .
C23 Ti2 2.447(4) .
C24 C25 1.412(6) .
C24 C29 1.513(6) .
C24 Ti2 2.464(4) .
C25 C30 1.496(6) .
C25 Ti2 2.410(4) .
C31 C35 1.407(6) .
C31 C32 1.411(6) .
C31 C36 1.488(6) .
C31 Ti3 2.456(4) .
C32 C33 1.416(6) .
C32 C37 1.488(6) .
C32 Ti3 2.457(4) .
C33 C34 1.415(6) .
C33 C38 1.507(6) .
C33 Ti3 2.439(4) .
C34 C35 1.424(6) .
C34 C39 1.488(6) .
C34 Ti3 2.435(4) .
C35 C40 1.487(6) .
C35 Ti3 2.429(4) .
K1 N13 2.772(4) .
K1 N23 2.776(4) .
K1 C14 3.000(4) 2_554
K1 C13 3.006(4) 2_554
K1 N12 3.108(4) .
K1 C12 3.168(4) 2_554
K1 C15 3.171(4) 2_554
K1 C11 3.258(4) 2_554
K1 Si1 3.418(3) .
K1 Ti3 3.4297(18) .
K1 Ti1 3.657(2) .
K1 Ti2 3.6977(19) .
N1 Ti2 1.905(3) .
N1 Ti1 1.916(3) .
N1 Ti3 1.957(3) .
N12 Si1 1.713(3) .
N12 Ti2 1.961(3) .
N12 Ti1 1.980(3) .
N13 Ti1 1.860(3) .
N13 Ti3 1.883(3) .
N23 Ti2 1.913(4) .
N23 Ti3 1.929(4) .
Ti1 Ti3 2.7615(15) .
Ti1 Ti2 2.8045(16) .
Ti2 Ti3 2.804(3) .
