#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/80/2018057.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018057
loop_
_publ_author_name
'Martín, Avelino'
'Mena, Miguel'
'Pérez-Redondo, Adrián'
'Yélamos, Carlos'
_publ_section_title
;
 A new double-cube nitride complex containing titanium and potassium
;
_journal_coeditor_code           DT3001
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m157
_journal_page_last               m159
_journal_paper_doi               10.1107/S0108270111012686
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[K2 Ti6 (C10 H15)6 I2 N2 (N H)6 (C5 H5 N)2]'
_chemical_formula_moiety         'C70 H106 I2 K2 N10 Ti6'
_chemical_formula_sum            'C70 H106 I2 K2 N10 Ti6'
_chemical_formula_weight         1707.05
_chemical_name_systematic
;
di-μ-iodido-1:1'κ⁴I-bis[tri-μ₃-imido-1:2:3κ³N;
1:2:4κ³N;1:3:4κ³N-μ₃-nitrido-2:3:4κ³N-
tris[2,3,4(η⁵)-pentamethylcyclopentadienyl](pyridine-1κN)-
tetrahedro-potassiumtrititanium(IV)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.660(10)
_cell_angle_beta                 93.460(10)
_cell_angle_gamma                115.550(10)
_cell_formula_units_Z            1
_cell_length_a                   11.298(2)
_cell_length_b                   11.346(2)
_cell_length_c                   18.391(3)
_cell_measurement_reflns_used    82
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      3
_cell_volume                     2053.8(7)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34701
_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        25
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.45
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0609P)²+0.0977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                6034
_reflns_number_total             9150
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dt3001.cif
_cod_data_source_block           II
_cod_original_cell_volume        2053.8(6)
_cod_database_code               2018057
_cod_database_fobs_code          2018057
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
C C11 0.6813(3) 0.4029(4) 0.7540(2) 0.0320(8) Uani d . 1 1 . .
C C12 0.7232(3) 0.5237(4) 0.8121(2) 0.0318(8) Uani d . 1 1 . .
C C13 0.7454(3) 0.6325(4) 0.7784(2) 0.0372(9) Uani d . 1 1 . .
C C14 0.7148(4) 0.5777(5) 0.6979(2) 0.0409(10) Uani d . 1 1 . .
C C15 0.6754(4) 0.4365(5) 0.6832(2) 0.0387(10) Uani d . 1 1 . .
C C16 0.6534(4) 0.2661(4) 0.7661(3) 0.0461(10) Uani d . 1 1 . .
H H16A 0.5974 0.1969 0.7222 0.069 Uiso calc R 1 1 . .
H H16B 0.6095 0.2531 0.809 0.069 Uiso calc R 1 1 . .
H H16C 0.7358 0.2614 0.7747 0.069 Uiso calc R 1 1 . .
C C17 0.7442(4) 0.5378(5) 0.8963(2) 0.0449(10) Uani d . 1 1 . .
H H17A 0.6839 0.4552 0.907 0.067 Uiso calc R 1 1 . .
H H17B 0.7279 0.6105 0.922 0.067 Uiso calc R 1 1 . .
H H17C 0.8341 0.5565 0.913 0.067 Uiso calc R 1 1 . .
C C18 0.7979(4) 0.7789(4) 0.8214(3) 0.0557(13) Uani d . 1 1 . .
H H18A 0.7801 0.8284 0.7893 0.084 Uiso calc R 1 1 . .
H H18B 0.8921 0.8172 0.8377 0.084 Uiso calc R 1 1 . .
H H18C 0.7547 0.7837 0.8645 0.084 Uiso calc R 1 1 . .
C C19 0.7303(5) 0.6565(6) 0.6384(3) 0.0693(16) Uani d . 1 1 . .
H H19A 0.7254 0.7386 0.6591 0.104 Uiso calc R 1 1 . .
H H19B 0.6605 0.603 0.596 0.104 Uiso calc R 1 1 . .
H H19C 0.815 0.6776 0.6225 0.104 Uiso calc R 1 1 . .
C C20 0.6413(5) 0.3402(6) 0.6067(3) 0.0648(15) Uani d . 1 1 . .
H H20A 0.5839 0.2502 0.6097 0.097 Uiso calc R 1 1 . .
H H20B 0.7214 0.3432 0.5903 0.097 Uiso calc R 1 1 . .
H H20C 0.5968 0.3658 0.5714 0.097 Uiso calc R 1 1 . .
C C21 0.2430(4) 0.6774(4) 0.6522(2) 0.0345(9) Uani d . 1 1 . .
C C22 0.3768(4) 0.7727(4) 0.6849(3) 0.0402(10) Uani d . 1 1 . .
C C23 0.3836(4) 0.8151(4) 0.7622(3) 0.0453(11) Uani d . 1 1 . .
C C24 0.2547(5) 0.7484(5) 0.7798(2) 0.0482(11) Uani d . 1 1 . .
C C25 0.1666(4) 0.6633(4) 0.7118(3) 0.0411(10) Uani d . 1 1 . .
C C26 0.1911(6) 0.6104(6) 0.5688(3) 0.0729(16) Uani d . 1 1 . .
H H26A 0.1 0.5438 0.562 0.109 Uiso calc R 1 1 . .
H H26B 0.2437 0.5676 0.549 0.109 Uiso calc R 1 1 . .
H H26C 0.197 0.6773 0.5426 0.109 Uiso calc R 1 1 . .
C C27 0.4903(5) 0.8189(6) 0.6401(4) 0.0812(19) Uani d . 1 1 . .
H H27A 0.487 0.7419 0.6051 0.122 Uiso calc R 1 1 . .
H H27B 0.5738 0.8644 0.6739 0.122 Uiso calc R 1 1 . .
H H27C 0.4816 0.8796 0.613 0.122 Uiso calc R 1 1 . .
C C28 0.5051(6) 0.9221(5) 0.8196(4) 0.089(2) Uani d . 1 1 . .
H H28A 0.5033 0.8964 0.8664 0.133 Uiso calc R 1 1 . .
H H28B 0.5035 1.0076 0.8277 0.133 Uiso calc R 1 1 . .
H H28C 0.5849 0.9294 0.8009 0.133 Uiso calc R 1 1 . .
C C29 0.2150(8) 0.7675(7) 0.8581(3) 0.098(2) Uani d . 1 1 . .
H H29A 0.1258 0.6999 0.8562 0.147 Uiso calc R 1 1 . .
H H29B 0.2193 0.8555 0.8735 0.147 Uiso calc R 1 1 . .
H H29C 0.2749 0.7589 0.8936 0.147 Uiso calc R 1 1 . .
C C30 0.0164(5) 0.5809(6) 0.7021(4) 0.082(2) Uani d . 1 1 . .
H H30A -0.008 0.5628 0.7492 0.124 Uiso calc R 1 1 . .
H H30B -0.0115 0.4972 0.665 0.124 Uiso calc R 1 1 . .
H H30C -0.026 0.6308 0.686 0.124 Uiso calc R 1 1 . .
C C31 0.1070(4) 0.0565(4) 0.6827(2) 0.0396(10) Uani d . 1 1 . .
C C32 0.1903(4) 0.0680(4) 0.6273(2) 0.0351(9) Uani d . 1 1 . .
C C33 0.1578(4) 0.1316(4) 0.5758(2) 0.0429(10) Uani d . 1 1 . .
C C34 0.0503(4) 0.1561(4) 0.5985(3) 0.0485(12) Uani d . 1 1 . .
C C35 0.0190(4) 0.1097(4) 0.6646(3) 0.0466(11) Uani d . 1 1 . .
C C36 0.1103(6) -0.0070(5) 0.7477(3) 0.0707(16) Uani d . 1 1 . .
H H36A 0.0706 0.0247 0.7868 0.106 Uiso calc R 1 1 . .
H H36B 0.2009 0.0177 0.7671 0.106 Uiso calc R 1 1 . .
H H36C 0.0615 -0.1035 0.7301 0.106 Uiso calc R 1 1 . .
C C37 0.2952(5) 0.0175(5) 0.6239(3) 0.0650(15) Uani d . 1 1 . .
H H37A 0.3373 0.0348 0.5807 0.098 Uiso calc R 1 1 . .
H H37B 0.2537 -0.0778 0.6199 0.098 Uiso calc R 1 1 . .
H H37C 0.3608 0.0637 0.6688 0.098 Uiso calc R 1 1 . .
C C38 0.2226(7) 0.1628(5) 0.5072(3) 0.083(2) Uani d . 1 1 . .
H H38A 0.3011 0.1498 0.5092 0.124 Uiso calc R 1 1 . .
H H38B 0.2463 0.2548 0.507 0.124 Uiso calc R 1 1 . .
H H38C 0.1611 0.1036 0.4622 0.124 Uiso calc R 1 1 . .
C C39 -0.0204(7) 0.2174(5) 0.5573(4) 0.106(3) Uani d . 1 1 . .
H H39A -0.0533 0.2654 0.5928 0.159 Uiso calc R 1 1 . .
H H39B -0.0934 0.1468 0.5206 0.159 Uiso calc R 1 1 . .
H H39C 0.041 0.2786 0.5325 0.159 Uiso calc R 1 1 . .
C C40 -0.0917(5) 0.1113(6) 0.7073(4) 0.090(2) Uani d . 1 1 . .
H H40A -0.0654 0.1221 0.7598 0.134 Uiso calc R 1 1 . .
H H40B -0.1711 0.0278 0.6879 0.134 Uiso calc R 1 1 . .
H H40C -0.1086 0.1851 0.7013 0.134 Uiso calc R 1 1 . .
N N1 0.3709(3) 0.4524(3) 0.66719(16) 0.0276(6) Uani d . 1 1 . .
N N12 0.4739(3) 0.6157(3) 0.80365(17) 0.0267(6) Uani d . 1 1 . .
N N13 0.3862(3) 0.3109(3) 0.76297(18) 0.0295(7) Uani d . 1 1 . .
N N23 0.1795(3) 0.4169(3) 0.74969(17) 0.0295(7) Uani d . 1 1 . .
Ti Ti1 0.51229(6) 0.47830(6) 0.74308(3) 0.02487(15) Uani d . 1 1 . .
Ti Ti2 0.32196(6) 0.57712(6) 0.73130(3) 0.02383(15) Uani d . 1 1 . .
Ti Ti3 0.24024(6) 0.29469(6) 0.69314(4) 0.02655(15) Uani d . 1 1 . .
K K1 0.33000(8) 0.44731(9) 0.90362(5) 0.0383(2) Uani d . 1 1 . .
I I1 0.43572(3) 0.23225(3) 0.973406(16) 0.04420(11) Uani d . 1 1 . .
H H12 0.527(4) 0.689(4) 0.839(2) 0.028(10) Uiso d . 1 1 . .
H H13 0.404(4) 0.259(5) 0.778(2) 0.044(14) Uiso d . 1 1 . .
H H23 0.105(4) 0.397(4) 0.757(2) 0.047(14) Uiso d . 1 1 . .
C C102 -0.0438(5) 0.3309(5) 0.9240(3) 0.0583(13) Uani d . 1 1 . .
H H102 -0.0299 0.4113 0.9122 0.07 Uiso calc R 1 1 . .
C C103 -0.1669(5) 0.2515(6) 0.9407(3) 0.0642(15) Uani d . 1 1 . .
H H103 -0.2333 0.2791 0.9402 0.077 Uiso calc R 1 1 . .
C C104 -0.1901(5) 0.1318(5) 0.9579(3) 0.0577(13) Uani d . 1 1 . .
H H104 -0.2722 0.0772 0.969 0.069 Uiso calc R 1 1 . .
C C105 -0.0890(5) 0.0945(5) 0.9583(3) 0.0568(13) Uani d . 1 1 . .
H H105 -0.102 0.0141 0.9698 0.068 Uiso calc R 1 1 . .
C C106 0.0319(5) 0.1780(5) 0.9414(3) 0.0556(12) Uani d . 1 1 . .
H H106 0.099 0.1513 0.9417 0.067 Uiso calc R 1 1 . .
N N101 0.0579(4) 0.2964(4) 0.9243(2) 0.0526(10) Uani d . 1 1 . .
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
-3 -16 4 0.066
1 -1 0 0.068
15 -2 -3 0.079
1 10 -2 0.156
-8 -1 2 0.148
-1 1 0 0.2
-1 1 -10 0.05
1 -1 16 0.115
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N12 K1 N13 . . 62.09(9) y
N12 K1 N23 . . 60.70(9) y
N13 K1 N23 . . 60.71(9) y
N12 K1 I1 . . 123.11(6) y
N12 K1 I1 . 2_667 74.18(6) y
N12 K1 N101 . . 138.20(10) y
N13 K1 I1 . . 79.45(7) y
N13 K1 I1 . 2_667 124.46(7) y
N13 K1 N101 . . 111.30(10) y
N23 K1 I1 . . 132.43(7) y
N23 K1 I1 . 2_667 123.68(6) y
N23 K1 N101 . . 79.80(10) y
N101 K1 I1 . . 92.89(9) y
N101 K1 I1 . 2_667 124.17(8) y
I1 K1 I1 . 2_667 99.39(3) y
K1 I1 K1 . 2_667 80.61(3) y
N12 Ti1 N13 . . 104.00(10) y
N12 Ti2 N23 . . 103.90(10) y
N13 Ti3 N23 . . 104.10(10) y
N1 Ti1 N12 . . 85.80(10) y
N1 Ti1 N13 . . 86.40(10) y
N1 Ti2 N12 . . 86.00(10) y
N1 Ti2 N23 . . 85.90(10) y
N1 Ti3 N13 . . 86.30(10) y
N1 Ti3 N23 . . 86.00(10) y
Ti1 N1 Ti2 . . 94.00(10) y
Ti1 N1 Ti3 . . 93.70(10) y
Ti2 N1 Ti3 . . 94.10(10) y
Ti1 N12 Ti2 . . 93.80(10) y
Ti1 N12 K1 . . 95.20(10) y
Ti1 N12 H12 . . 130(2) ?
Ti2 N12 K1 . . 98.30(10) y
Ti2 N12 H12 . . 132(2) ?
K1 N12 H12 . . 98(2) ?
Ti1 N13 Ti3 . . 93.20(10) y
Ti1 N13 K1 . . 94.50(10) y
Ti1 N13 H13 . . 126(3) ?
Ti3 N13 K1 . . 97.90(10) y
Ti3 N13 H13 . . 134(3) ?
K1 N13 H13 . . 101(3) ?
Ti2 N23 Ti3 . . 93.60(10) y
Ti2 N23 K1 . . 94.00(10) y
Ti2 N23 H23 . . 134(3) ?
Ti3 N23 K1 . . 94.60(10) y
Ti3 N23 H23 . . 126(3) ?
K1 N23 H23 . . 103(3) ?
C12 C11 C15 . . 107.6(3) ?
C12 C11 C16 . . 125.4(4) ?
C15 C11 C16 . . 127.0(4) ?
C12 C11 Ti1 . . 73.0(2) ?
C15 C11 Ti1 . . 70.7(2) ?
C16 C11 Ti1 . . 123.4(3) ?
C11 C12 C13 . . 108.7(3) ?
C11 C12 C17 . . 126.7(4) ?
C13 C12 C17 . . 124.6(4) ?
C11 C12 Ti1 . . 72.76(19) ?
C13 C12 Ti1 . . 72.1(2) ?
C17 C12 Ti1 . . 122.1(2) ?
C12 C13 C14 . . 107.5(4) ?
C12 C13 C18 . . 124.7(4) ?
C14 C13 C18 . . 127.7(4) ?
C12 C13 Ti1 . . 73.5(2) ?
C14 C13 Ti1 . . 70.8(2) ?
C18 C13 Ti1 . . 123.3(3) ?
C15 C14 C13 . . 107.9(3) ?
C15 C14 C19 . . 125.3(4) ?
C13 C14 C19 . . 126.6(4) ?
C15 C14 Ti1 . . 72.8(2) ?
C13 C14 Ti1 . . 74.0(2) ?
C19 C14 Ti1 . . 122.2(3) ?
C14 C15 C11 . . 108.2(3) ?
C14 C15 C20 . . 126.1(4) ?
C11 C15 C20 . . 125.6(4) ?
C14 C15 Ti1 . . 72.1(2) ?
C11 C15 Ti1 . . 74.4(2) ?
C20 C15 Ti1 . . 122.1(3) ?
C11 C16 H16A . . 109.5 ?
C11 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C11 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C12 C17 H17A . . 109.5 ?
C12 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C12 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C13 C18 H18A . . 109.5 ?
C13 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C13 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C14 C19 H19A . . 109.5 ?
C14 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C14 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C15 C20 H20A . . 109.5 ?
C15 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C15 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C25 C21 C22 . . 107.1(4) ?
C25 C21 C26 . . 126.8(4) ?
C22 C21 C26 . . 126.0(4) ?
C25 C21 Ti2 . . 73.4(2) ?
C22 C21 Ti2 . . 73.2(2) ?
C26 C21 Ti2 . . 121.5(3) ?
C23 C22 C21 . . 108.9(4) ?
C23 C22 C27 . . 127.2(5) ?
C21 C22 C27 . . 123.9(4) ?
C23 C22 Ti2 . . 74.2(2) ?
C21 C22 Ti2 . . 71.9(2) ?
C27 C22 Ti2 . . 120.6(3) ?
C22 C23 C24 . . 108.4(4) ?
C22 C23 C28 . . 127.4(5) ?
C24 C23 C28 . . 124.1(5) ?
C22 C23 Ti2 . . 72.1(2) ?
C24 C23 Ti2 . . 72.9(2) ?
C28 C23 Ti2 . . 124.0(3) ?
C23 C24 C25 . . 108.1(4) ?
C23 C24 C29 . . 126.4(5) ?
C25 C24 C29 . . 125.5(5) ?
C23 C24 Ti2 . . 72.9(2) ?
C25 C24 Ti2 . . 72.0(2) ?
C29 C24 Ti2 . . 122.3(3) ?
C24 C25 C21 . . 107.6(3) ?
C24 C25 C30 . . 126.9(5) ?
C21 C25 C30 . . 125.4(5) ?
C24 C25 Ti2 . . 73.5(2) ?
C21 C25 Ti2 . . 71.6(2) ?
C30 C25 Ti2 . . 124.3(3) ?
C21 C26 H26A . . 109.5 ?
C21 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C21 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C22 C27 H27A . . 109.5 ?
C22 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C22 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C23 C28 H28A . . 109.5 ?
C23 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
C23 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
C24 C29 H29A . . 109.5 ?
C24 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
C24 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C25 C30 H30A . . 109.5 ?
C25 C30 H30B . . 109.5 ?
H30A C30 H30B . . 109.5 ?
C25 C30 H30C . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
C32 C31 C35 . . 107.8(4) ?
C32 C31 C36 . . 124.9(4) ?
C35 C31 C36 . . 127.3(4) ?
C32 C31 Ti3 . . 72.6(2) ?
C35 C31 Ti3 . . 72.4(2) ?
C36 C31 Ti3 . . 122.4(3) ?
C31 C32 C33 . . 108.7(4) ?
C31 C32 C37 . . 124.8(4) ?
C33 C32 C37 . . 126.4(4) ?
C31 C32 Ti3 . . 73.3(2) ?
C33 C32 Ti3 . . 71.1(2) ?
C37 C32 Ti3 . . 122.4(3) ?
C32 C33 C34 . . 107.4(4) ?
C32 C33 C38 . . 126.1(5) ?
C34 C33 C38 . . 126.4(5) ?
C32 C33 Ti3 . . 74.4(2) ?
C34 C33 Ti3 . . 72.8(2) ?
C38 C33 Ti3 . . 120.3(3) ?
C33 C34 C35 . . 108.1(4) ?
C33 C34 C39 . . 125.4(5) ?
C35 C34 C39 . . 126.5(5) ?
C33 C34 Ti3 . . 72.2(2) ?
C35 C34 Ti3 . . 73.9(2) ?
C39 C34 Ti3 . . 121.0(3) ?
C31 C35 C34 . . 107.9(4) ?
C31 C35 C40 . . 125.4(5) ?
C34 C35 C40 . . 126.6(5) ?
C31 C35 Ti3 . . 73.3(2) ?
C34 C35 Ti3 . . 71.4(2) ?
C40 C35 Ti3 . . 122.7(3) ?
C31 C36 H36A . . 109.5 ?
C31 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C31 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C32 C37 H37A . . 109.5 ?
C32 C37 H37B . . 109.5 ?
H37A C37 H37B . . 109.5 ?
C32 C37 H37C . . 109.5 ?
H37A C37 H37C . . 109.5 ?
H37B C37 H37C . . 109.5 ?
C33 C38 H38A . . 109.5 ?
C33 C38 H38B . . 109.5 ?
H38A C38 H38B . . 109.5 ?
C33 C38 H38C . . 109.5 ?
H38A C38 H38C . . 109.5 ?
H38B C38 H38C . . 109.5 ?
C34 C39 H39A . . 109.5 ?
C34 C39 H39B . . 109.5 ?
H39A C39 H39B . . 109.5 ?
C34 C39 H39C . . 109.5 ?
H39A C39 H39C . . 109.5 ?
H39B C39 H39C . . 109.5 ?
C35 C40 H40A . . 109.5 ?
C35 C40 H40B . . 109.5 ?
H40A C40 H40B . . 109.5 ?
C35 C40 H40C . . 109.5 ?
H40A C40 H40C . . 109.5 ?
H40B C40 H40C . . 109.5 ?
N1 Ti1 C14 . . 107.54(13) ?
N13 Ti1 C14 . . 142.90(15) ?
N12 Ti1 C14 . . 111.06(15) ?
N1 Ti1 C15 . . 109.24(13) ?
N13 Ti1 C15 . . 108.10(15) ?
N12 Ti1 C15 . . 145.14(14) ?
C14 Ti1 C15 . . 35.07(15) ?
N1 Ti1 C13 . . 134.66(13) ?
N13 Ti1 C13 . . 138.27(14) ?
N12 Ti1 C13 . . 88.70(13) ?
C14 Ti1 C13 . . 35.19(14) ?
C15 Ti1 C13 . . 58.10(14) ?
N1 Ti1 C11 . . 137.95(13) ?
N13 Ti1 C11 . . 88.39(13) ?
N12 Ti1 C11 . . 135.74(13) ?
C14 Ti1 C11 . . 57.97(14) ?
C15 Ti1 C11 . . 34.83(13) ?
C13 Ti1 C11 . . 57.46(13) ?
N1 Ti1 C12 . . 165.05(12) ?
N13 Ti1 C12 . . 103.92(13) ?
N12 Ti1 C12 . . 101.79(13) ?
C14 Ti1 C12 . . 57.79(13) ?
C15 Ti1 C12 . . 57.57(13) ?
C13 Ti1 C12 . . 34.39(13) ?
C11 Ti1 C12 . . 34.26(13) ?
N1 Ti1 Ti3 . . 43.20(9) ?
N13 Ti1 Ti3 . . 43.43(10) ?
N12 Ti1 Ti3 . . 93.33(9) ?
C14 Ti1 Ti3 . . 141.62(11) ?
C15 Ti1 Ti3 . . 119.41(11) ?
C13 Ti1 Ti3 . . 176.81(11) ?
C11 Ti1 Ti3 . . 121.97(10) ?
C12 Ti1 Ti3 . . 146.96(10) ?
N1 Ti1 Ti2 . . 43.09(9) ?
N13 Ti1 Ti2 . . 93.70(10) ?
N12 Ti1 Ti2 . . 42.92(9) ?
C14 Ti1 Ti2 . . 120.24(11) ?
C15 Ti1 Ti2 . . 144.51(10) ?
C13 Ti1 Ti2 . . 120.33(10) ?
C11 Ti1 Ti2 . . 177.79(10) ?
C12 Ti1 Ti2 . . 144.08(10) ?
Ti3 Ti1 Ti2 . . 60.22(3) ?
N1 Ti1 K1 . . 98.39(9) ?
N13 Ti1 K1 . . 53.79(10) ?
N12 Ti1 K1 . . 53.10(9) ?
C14 Ti1 K1 . . 148.83(11) ?
C15 Ti1 K1 . . 146.36(10) ?
C13 Ti1 K1 . . 113.64(10) ?
C11 Ti1 K1 . . 111.70(9) ?
C12 Ti1 K1 . . 96.44(9) ?
Ti3 Ti1 K1 . . 69.54(3) ?
Ti2 Ti1 K1 . . 69.09(2) ?
N12 Ti2 C21 . . 141.77(13) ?
N1 Ti2 C21 . . 107.24(13) ?
N23 Ti2 C21 . . 112.55(14) ?
N12 Ti2 C22 . . 106.91(14) ?
N1 Ti2 C22 . . 110.02(14) ?
N23 Ti2 C22 . . 146.05(14) ?
C21 Ti2 C22 . . 34.96(14) ?
N12 Ti2 C25 . . 139.28(15) ?
N1 Ti2 C25 . . 133.84(15) ?
N23 Ti2 C25 . . 89.61(14) ?
C21 Ti2 C25 . . 34.94(14) ?
C22 Ti2 C25 . . 57.50(13) ?
N12 Ti2 C23 . . 88.62(14) ?
N1 Ti2 C23 . . 138.12(15) ?
N23 Ti2 C23 . . 135.51(15) ?
C21 Ti2 C23 . . 57.35(14) ?
C22 Ti2 C23 . . 33.73(15) ?
C25 Ti2 C23 . . 57.17(14) ?
N12 Ti2 C24 . . 104.82(15) ?
N1 Ti2 C24 . . 164.61(14) ?
N23 Ti2 C24 . . 101.76(15) ?
C21 Ti2 C24 . . 57.55(14) ?
C22 Ti2 C24 . . 56.71(15) ?
C25 Ti2 C24 . . 34.46(15) ?
C23 Ti2 C24 . . 34.17(16) ?
N12 Ti2 Ti1 . . 43.28(9) ?
N1 Ti2 Ti1 . . 42.90(9) ?
N23 Ti2 Ti1 . . 93.21(10) ?
C21 Ti2 Ti1 . . 140.46(10) ?
C22 Ti2 Ti1 . . 119.09(10) ?
C25 Ti2 Ti1 . . 175.37(11) ?
C23 Ti2 Ti1 . . 122.22(11) ?
C24 Ti2 Ti1 . . 147.69(12) ?
N12 Ti2 Ti3 . . 93.17(9) ?
N1 Ti2 Ti3 . . 42.90(9) ?
N23 Ti2 Ti3 . . 43.21(10) ?
C21 Ti2 Ti3 . . 121.19(10) ?
C22 Ti2 Ti3 . . 145.85(11) ?
C25 Ti2 Ti3 . . 120.88(10) ?
C23 Ti2 Ti3 . . 178.05(10) ?
C24 Ti2 Ti3 . . 144.27(12) ?
Ti1 Ti2 Ti3 . . 59.72(2) ?
N12 Ti2 K1 . . 51.09(9) ?
N1 Ti2 K1 . . 95.81(9) ?
N23 Ti2 K1 . . 54.90(9) ?
C21 Ti2 K1 . . 153.33(10) ?
C22 Ti2 K1 . . 145.50(11) ?
C25 Ti2 K1 . . 118.42(11) ?
C23 Ti2 K1 . . 112.49(11) ?
C24 Ti2 K1 . . 99.51(11) ?
Ti1 Ti2 K1 . . 66.19(2) ?
Ti3 Ti2 K1 . . 68.20(3) ?
N1 Ti3 C33 . . 102.49(13) ?
N13 Ti3 C33 . . 121.54(15) ?
N23 Ti3 C33 . . 133.87(15) ?
N1 Ti3 C34 . . 114.67(15) ?
N13 Ti3 C34 . . 149.01(14) ?
N23 Ti3 C34 . . 100.17(15) ?
C33 Ti3 C34 . . 35.00(16) ?
N1 Ti3 C32 . . 122.40(13) ?
N13 Ti3 C32 . . 92.55(14) ?
N23 Ti3 C32 . . 148.31(14) ?
C33 Ti3 C32 . . 34.56(14) ?
C34 Ti3 C32 . . 57.28(14) ?
N1 Ti3 C35 . . 148.16(15) ?
N13 Ti3 C35 . . 124.88(16) ?
N23 Ti3 C35 . . 91.74(14) ?
C33 Ti3 C35 . . 57.79(16) ?
C34 Ti3 C35 . . 34.66(16) ?
C32 Ti3 C35 . . 56.85(14) ?
N1 Ti3 C31 . . 156.50(14) ?
N13 Ti3 C31 . . 94.16(14) ?
N23 Ti3 C31 . . 116.50(14) ?
C33 Ti3 C31 . . 57.55(14) ?
C34 Ti3 C31 . . 57.37(14) ?
C32 Ti3 C31 . . 34.10(14) ?
C35 Ti3 C31 . . 34.26(15) ?
N1 Ti3 Ti1 . . 43.11(9) ?
N13 Ti3 Ti1 . . 43.35(10) ?
N23 Ti3 Ti1 . . 93.52(10) ?
C33 Ti3 Ti1 . . 123.62(12) ?
C34 Ti3 Ti1 . . 153.18(13) ?
C32 Ti3 Ti1 . . 116.55(10) ?
C35 Ti3 Ti1 . . 168.10(12) ?
C31 Ti3 Ti1 . . 134.54(11) ?
N1 Ti3 Ti2 . . 43.00(9) ?
N13 Ti3 Ti2 . . 93.50(10) ?
N23 Ti3 Ti2 . . 43.22(10) ?
C33 Ti3 Ti2 . . 131.53(10) ?
C34 Ti3 Ti2 . . 117.45(11) ?
C32 Ti3 Ti2 . . 163.59(10) ?
C35 Ti3 Ti2 . . 129.35(11) ?
C31 Ti3 Ti2 . . 159.66(11) ?
Ti1 Ti3 Ti2 . . 60.06(2) ?
N1 Ti3 K1 . . 95.36(9) ?
N13 Ti3 K1 . . 51.42(10) ?
N23 Ti3 K1 . . 54.48(9) ?
C33 Ti3 K1 . . 160.53(10) ?
C34 Ti3 K1 . . 140.15(13) ?
C32 Ti3 K1 . . 127.31(10) ?
C35 Ti3 K1 . . 109.04(12) ?
C31 Ti3 K1 . . 103.25(10) ?
Ti1 Ti3 K1 . . 66.02(3) ?
Ti2 Ti3 K1 . . 67.58(3) ?
N101 K1 Ti1 . . 136.19(8) ?
N12 K1 Ti1 . . 31.75(6) ?
N13 K1 Ti1 . . 31.69(6) ?
N23 K1 Ti1 . . 62.05(6) ?
I1 K1 Ti1 . . 97.43(3) ?
I1 K1 Ti1 2_667 . 95.95(3) ?
N101 K1 Ti2 . . 107.91(8) ?
N12 K1 Ti2 . . 30.57(6) ?
N13 K1 Ti2 . . 61.99(7) ?
N23 K1 Ti2 . . 31.09(6) ?
I1 K1 Ti2 . . 140.55(3) ?
I1 K1 Ti2 2_667 . 95.99(3) ?
Ti1 K1 Ti2 . . 44.717(18) ?
N101 K1 Ti3 . . 91.75(8) ?
N12 K1 Ti3 . . 61.62(6) ?
N13 K1 Ti3 . . 30.64(6) ?
N23 K1 Ti3 . . 30.90(6) ?
I1 K1 Ti3 . . 103.91(3) ?
I1 K1 Ti3 2_667 . 135.79(3) ?
Ti1 K1 Ti3 . . 44.441(19) ?
Ti2 K1 Ti3 . . 44.217(19) ?
N101 K1 K1 . 2_667 118.42(8) ?
N12 K1 K1 . 2_667 101.95(7) ?
N13 K1 K1 . 2_667 107.45(7) ?
N23 K1 K1 . 2_667 161.73(7) ?
I1 K1 K1 . 2_667 50.19(2) ?
I1 K1 K1 2_667 2_667 49.21(2) ?
Ti1 K1 K1 . 2_667 100.37(3) ?
Ti2 K1 K1 . 2_667 132.37(3) ?
Ti3 K1 K1 . 2_667 137.95(4) ?
N101 C102 C103 . . 123.0(5) ?
N101 C102 H102 . . 118.5 ?
C103 C102 H102 . . 118.5 ?
C104 C103 C102 . . 119.6(5) ?
C104 C103 H103 . . 120.2 ?
C102 C103 H103 . . 120.2 ?
C103 C104 C105 . . 118.5(4) ?
C103 C104 H104 . . 120.7 ?
C105 C104 H104 . . 120.7 ?
C106 C105 C104 . . 119.3(5) ?
C106 C105 H105 . . 120.4 ?
C104 C105 H105 . . 120.4 ?
N101 C106 C105 . . 123.6(5) ?
N101 C106 H106 . . 118.2 ?
C105 C106 H106 . . 118.2 ?
C106 N101 C102 . . 116.0(4) ?
C106 N101 K1 . . 114.1(3) ?
C102 N101 K1 . . 129.7(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K1 N12 . 2.962(3) y
K1 N13 . 2.986(3) y
K1 N23 . 3.089(3) y
K1 N101 . 2.896(4) y
K1 I1 . 3.5530(10) y
K1 I1 2_667 3.6050(10) y
Ti1 N12 . 1.949(3) y
Ti1 N13 . 1.944(3) y
Ti2 N12 . 1.936(3) y
Ti2 N23 . 1.950(3) y
Ti3 N13 . 1.947(3) y
Ti3 N23 . 1.949(3) y
Ti1 N1 . 1.936(3) y
Ti2 N1 . 1.943(3) y
Ti3 N1 . 1.939(3) y
I1 K1 2_667 3.6046(12) ?
C11 C12 . 1.426(5) ?
C11 C15 . 1.434(5) ?
C11 C16 . 1.511(6) ?
C11 Ti1 . 2.420(3) ?
C12 C13 . 1.427(6) ?
C12 C17 . 1.516(5) ?
C12 Ti1 . 2.423(3) ?
C13 C14 . 1.441(6) ?
C13 C18 . 1.516(6) ?
C13 Ti1 . 2.404(4) ?
C14 C15 . 1.426(6) ?
C14 C19 . 1.520(6) ?
C14 Ti1 . 2.362(4) ?
C15 C20 . 1.507(6) ?
C15 Ti1 . 2.371(4) ?
C16 H16A . 0.96 ?
C16 H16B . 0.96 ?
C16 H16C . 0.96 ?
C17 H17A . 0.96 ?
C17 H17B . 0.96 ?
C17 H17C . 0.96 ?
C18 H18A . 0.96 ?
C18 H18B . 0.96 ?
C18 H18C . 0.96 ?
C19 H19A . 0.96 ?
C19 H19B . 0.96 ?
C19 H19C . 0.96 ?
C20 H20A . 0.96 ?
C20 H20B . 0.96 ?
C20 H20C . 0.96 ?
C21 C25 . 1.428(6) ?
C21 C22 . 1.426(6) ?
C21 C26 . 1.520(6) ?
C21 Ti2 . 2.366(4) ?
C22 C23 . 1.391(6) ?
C22 C27 . 1.524(6) ?
C22 Ti2 . 2.383(4) ?
C23 C24 . 1.416(6) ?
C23 C28 . 1.531(6) ?
C23 Ti2 . 2.410(4) ?
C24 C25 . 1.422(6) ?
C24 C29 . 1.535(7) ?
C24 Ti2 . 2.410(4) ?
C25 C30 . 1.521(6) ?
C25 Ti2 . 2.390(4) ?
C26 H26A . 0.96 ?
C26 H26B . 0.96 ?
C26 H26C . 0.96 ?
C27 H27A . 0.96 ?
C27 H27B . 0.96 ?
C27 H27C . 0.96 ?
C28 H28A . 0.96 ?
C28 H28B . 0.96 ?
C28 H28C . 0.96 ?
C29 H29A . 0.96 ?
C29 H29B . 0.96 ?
C29 H29C . 0.96 ?
C30 H30A . 0.96 ?
C30 H30B . 0.96 ?
C30 H30C . 0.96 ?
C31 C32 . 1.416(6) ?
C31 C35 . 1.422(6) ?
C31 C36 . 1.521(6) ?
C31 Ti3 . 2.419(4) ?
C32 C33 . 1.419(6) ?
C32 C37 . 1.523(6) ?
C32 Ti3 . 2.410(4) ?
C33 C34 . 1.426(6) ?
C33 C38 . 1.524(7) ?
C33 Ti3 . 2.367(4) ?
C34 C35 . 1.425(7) ?
C34 C39 . 1.521(6) ?
C34 Ti3 . 2.375(4) ?
C35 C40 . 1.522(7) ?
C35 Ti3 . 2.408(4) ?
C36 H36A . 0.96 ?
C36 H36B . 0.96 ?
C36 H36C . 0.96 ?
C37 H37A . 0.96 ?
C37 H37B . 0.96 ?
C37 H37C . 0.96 ?
C38 H38A . 0.96 ?
C38 H38B . 0.96 ?
C38 H38C . 0.96 ?
C39 H39A . 0.96 ?
C39 H39B . 0.96 ?
C39 H39C . 0.96 ?
C40 H40A . 0.96 ?
C40 H40B . 0.96 ?
C40 H40C . 0.96 ?
C102 N101 . 1.364(6) ?
C102 C103 . 1.386(7) ?
C102 H102 . 0.93 ?
C103 C104 . 1.375(8) ?
C103 H103 . 0.93 ?
C104 C105 . 1.378(7) ?
C104 H104 . 0.93 ?
C105 C106 . 1.384(7) ?
C105 H105 . 0.93 ?
C106 N101 . 1.353(6) ?
C106 H106 . 0.93 ?
