#------------------------------------------------------------------------------
#$Date: 2017-01-01 07:02:42 +0200 (Sun, 01 Jan 2017) $
#$Revision: 189683 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/68/4086893.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_4086893
loop_
_publ_author_name
'Kilpatrick, Alexander F. R.'
'Green, Jennifer C.'
'Cloke, F. Geoffrey N.'
_publ_section_title
;
 Reactivity of a Dititanium Bis(pentalene) Complex toward Heteroallenes
 and Main-Group Element--Element Bonds
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00791
_journal_year                    2016
_chemical_formula_moiety         'C67 H106 N2 Si4 Ti2'
_chemical_formula_sum            'C67 H106 N2 Si4 Ti2'
_chemical_formula_weight         1147.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 121.30(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.872(5)
_cell_length_b                   15.032(3)
_cell_length_c                   19.626(4)
_cell_measurement_reflns_used    7976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1.6
_cell_volume                     6522(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
DIRDIF-2008 (Beurskens et al., University of Nijmegen, The Netherlands, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32498
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.307
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DTABSCOR
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0733P)²+6.1802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6538
_reflns_number_total             7312
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00791_si_003.cif
_cod_data_source_block           Compound3
_cod_database_code               4086893
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.11659(8) 0.06402(11) 0.88906(11) 0.0182(4) Uani 1 1 d . . .
C2 C 0.12541(8) 0.14724(11) 0.86057(11) 0.0188(3) Uani 1 1 d . . .
H2 H 0.1611 0.1622 0.8605 0.023 Uiso 1 1 calc R U .
C3 C 0.07542(8) 0.20388(11) 0.83284(11) 0.0186(3) Uani 1 1 d . . .
H3 H 0.0702 0.2598 0.8075 0.022 Uiso 1 1 calc R U .
C5 C 0.05810(8) 0.07462(11) 0.88249(11) 0.0170(3) Uani 1 1 d . . .
C9 C 0.24511(9) 0.01904(14) 0.93429(13) 0.0273(4) Uani 1 1 d . . .
H9 H 0.2499 0.0850 0.9335 0.033 Uiso 1 1 calc R U .
C10 C 0.22635(10) -0.01505(14) 0.85092(14) 0.0307(5) Uani 1 1 d . . .
H10A H 0.1865 0.0091 0.8118 0.046 Uiso 1 1 calc R U .
H10B H 0.2244 -0.0802 0.8503 0.046 Uiso 1 1 calc R U .
H10C H 0.2561 0.0042 0.8374 0.046 Uiso 1 1 calc R U .
C11 C 0.30774(10) -0.01851(19) 0.99563(17) 0.0440(6) Uani 1 1 d . . .
H11A H 0.3199 0.0036 1.0489 0.066 Uiso 1 1 calc R U .
H11B H 0.3374 0.0006 0.9818 0.066 Uiso 1 1 calc R U .
H11C H 0.3059 -0.0836 0.9953 0.066 Uiso 1 1 calc R U .
C12 C 0.17411(9) -0.12488(12) 0.96649(12) 0.0253(4) Uani 1 1 d . . .
H12 H 0.1765 -0.1532 0.9221 0.030 Uiso 1 1 calc R U .
C13 C 0.22375(10) -0.16811(15) 1.04442(14) 0.0352(5) Uani 1 1 d . . .
H13A H 0.2636 -0.1530 1.0531 0.053 Uiso 1 1 calc R U .
H13B H 0.2186 -0.2329 1.0406 0.053 Uiso 1 1 calc R U .
H13C H 0.2207 -0.1460 1.0892 0.053 Uiso 1 1 calc R U .
C14 C 0.11194(9) -0.14884(13) 0.95336(13) 0.0275(4) Uani 1 1 d . . .
H14A H 0.0802 -0.1215 0.9038 0.041 Uiso 1 1 calc R U .
H14B H 0.1090 -0.1267 0.9982 0.041 Uiso 1 1 calc R U .
H14C H 0.1069 -0.2136 0.9497 0.041 Uiso 1 1 calc R U .
C15 C 0.21396(9) 0.05246(13) 1.06261(13) 0.0272(4) Uani 1 1 d . . .
H15 H 0.2532 0.0232 1.1013 0.033 Uiso 1 1 calc R U .
C16 C 0.22693(12) 0.15251(15) 1.06208(14) 0.0388(5) Uani 1 1 d . . .
H16A H 0.2543 0.1609 1.0421 0.058 Uiso 1 1 calc R U .
H16B H 0.2458 0.1761 1.1164 0.058 Uiso 1 1 calc R U .
H16C H 0.1889 0.1841 1.0274 0.058 Uiso 1 1 calc R U .
C17 C 0.17108(10) 0.03862(16) 1.09409(14) 0.0341(5) Uani 1 1 d . . .
H17A H 0.1631 -0.0251 1.0945 0.051 Uiso 1 1 calc R U .
H17B H 0.1329 0.0698 1.0594 0.051 Uiso 1 1 calc R U .
H17C H 0.1899 0.0623 1.1484 0.051 Uiso 1 1 calc R U .
C30 C -0.03360(8) 0.16171(11) 0.65012(11) 0.0175(3) Uani 1 1 d . . .
C32 C -0.01557(8) 0.03233(11) 0.60157(11) 0.0181(3) Uani 1 1 d . . .
H32 H -0.0182 -0.0267 0.5828 0.022 Uiso 1 1 calc R U .
C33 C 0.03029(8) 0.09353(11) 0.61864(11) 0.0188(4) Uani 1 1 d . . .
H33 H 0.0627 0.0825 0.6101 0.023 Uiso 1 1 calc R U .
C34 C 0.02260(8) 0.17579(11) 0.65088(11) 0.0179(3) Uani 1 1 d . . .
C44 C 0.14062(9) 0.28614(12) 0.71838(12) 0.0238(4) Uani 1 1 d . . .
H44 H 0.1463 0.2963 0.7722 0.029 Uiso 1 1 calc R U .
C45 C 0.17126(9) 0.19798(14) 0.72177(13) 0.0276(4) Uani 1 1 d . . .
H45A H 0.1504 0.1493 0.7309 0.041 Uiso 1 1 calc R U .
H45B H 0.2136 0.1998 0.7654 0.041 Uiso 1 1 calc R U .
H45C H 0.1694 0.1883 0.6712 0.041 Uiso 1 1 calc R U .
C46 C 0.17517(10) 0.36040(14) 0.70427(14) 0.0320(5) Uani 1 1 d . . .
H46A H 0.1566 0.4180 0.7018 0.048 Uiso 1 1 calc R U .
H46B H 0.1734 0.3495 0.6539 0.048 Uiso 1 1 calc R U .
H46C H 0.2175 0.3608 0.7482 0.048 Uiso 1 1 calc R U .
C47 C 0.04503(10) 0.28941(13) 0.54023(13) 0.0279(4) Uani 1 1 d . . .
H47 H 0.0791 0.2543 0.5436 0.033 Uiso 1 1 calc R U .
C48 C 0.05074(11) 0.38340(15) 0.51364(15) 0.0360(5) Uani 1 1 d . . .
H48A H 0.0876 0.4118 0.5561 0.054 Uiso 1 1 calc R U .
H48B H 0.0155 0.4190 0.5026 0.054 Uiso 1 1 calc R U .
H48C H 0.0528 0.3793 0.4653 0.054 Uiso 1 1 calc R U .
C49 C -0.01261(11) 0.24701(16) 0.47342(14) 0.0367(5) Uani 1 1 d . . .
H49A H -0.0171 0.1871 0.4895 0.055 Uiso 1 1 calc R U .
H49B H -0.0104 0.2432 0.4252 0.055 Uiso 1 1 calc R U .
H49C H -0.0475 0.2834 0.4626 0.055 Uiso 1 1 calc R U .
C50 C 0.01487(9) 0.37452(12) 0.66316(13) 0.0270(4) Uani 1 1 d . . .
H50 H 0.0096 0.3514 0.7070 0.032 Uiso 1 1 calc R U .
C51 C 0.04829(12) 0.46296(14) 0.69373(17) 0.0407(6) Uani 1 1 d . . .
H51A H 0.0892 0.4519 0.7389 0.061 Uiso 1 1 calc R U .
H51B H 0.0264 0.5011 0.7109 0.061 Uiso 1 1 calc R U .
H51C H 0.0507 0.4926 0.6509 0.061 Uiso 1 1 calc R U .
C52 C -0.04958(10) 0.39121(15) 0.59230(15) 0.0362(5) Uani 1 1 d . . .
H52A H -0.0708 0.3343 0.5731 0.054 Uiso 1 1 calc R U .
H52B H -0.0475 0.4206 0.5492 0.054 Uiso 1 1 calc R U .
H52C H -0.0715 0.4294 0.6094 0.054 Uiso 1 1 calc R U .
C53 C 0.0000 -0.04876(16) 0.7500 0.0185(5) Uani 1 2 d S T P
C54 C 0.07595(8) -0.14952(11) 0.74706(11) 0.0200(4) Uani 1 1 d . . .
C55 C 0.11090(8) -0.14479(12) 0.71206(12) 0.0227(4) Uani 1 1 d . . .
H55 H 0.1143 -0.0900 0.6906 0.027 Uiso 1 1 calc R U .
C56 C 0.14079(9) -0.21945(12) 0.70835(13) 0.0269(4) Uani 1 1 d . . .
H56 H 0.1645 -0.2149 0.6844 0.032 Uiso 1 1 calc R U .
C57 C 0.13683(9) -0.30076(12) 0.73896(13) 0.0270(4) Uani 1 1 d . . .
C58 C 0.10196(9) -0.30523(12) 0.77355(13) 0.0275(4) Uani 1 1 d . . .
H58 H 0.0986 -0.3603 0.7947 0.033 Uiso 1 1 calc R U .
C59 C 0.07173(9) -0.23084(12) 0.77806(12) 0.0240(4) Uani 1 1 d . . .
H59 H 0.0482 -0.2355 0.8023 0.029 Uiso 1 1 calc R U .
C60 C 0.16836(10) -0.38201(14) 0.73239(17) 0.0390(6) Uani 1 1 d . . .
H60A H 0.1907 -0.3657 0.7064 0.058 Uiso 1 1 calc R U .
H60B H 0.1383 -0.4276 0.7007 0.058 Uiso 1 1 calc R U .
H60C H 0.1966 -0.4054 0.7858 0.058 Uiso 1 1 calc R U .
N1 N 0.04936(7) -0.06954(9) 0.75146(9) 0.0168(3) Uani 1 1 d . . .
Si1 Si 0.18573(2) -0.00096(3) 0.96138(3) 0.01912(13) Uani 1 1 d . . .
Si4 Si 0.05565(2) 0.28355(3) 0.64320(3) 0.01928(13) Uani 1 1 d . . .
Ti1 Ti 0.04641(2) 0.07114(2) 0.74829(2) 0.01590(10) 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 0.0000 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'
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_
_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
C2 C1 C5 103.74(14) . .
C2 C1 Si1 117.75(13) . .
C5 C1 Si1 131.30(13) . .
C2 C1 Ti1 71.96(10) . .
C5 C1 Ti1 76.30(11) . .
Si1 C1 Ti1 138.49(9) . .
C3 C2 C1 112.31(15) . .
C3 C2 Ti1 75.93(11) . .
C1 C2 Ti1 73.03(10) . .
C3 C2 H2 123.8 . .
C1 C2 H2 123.8 . .
Ti1 C2 H2 118.7 . .
C2 C3 C30 107.25(15) . 2_556
C2 C3 Ti1 70.39(10) . .
C30 C3 Ti1 78.20(10) 2_556 .
C2 C3 H3 126.4 . .
C30 C3 H3 126.4 2_556 .
Ti1 C3 H3 117.1 . .
C32 C5 C30 106.64(14) 2_556 2_556
C32 C5 C1 143.86(16) 2_556 .
C30 C5 C1 109.46(14) 2_556 .
C32 C5 Ti1 122.28(13) 2_556 .
C30 C5 Ti1 76.54(10) 2_556 .
C1 C5 Ti1 69.00(10) . .
C32 C5 Ti1 71.55(10) 2_556 2_556
C30 C5 Ti1 65.69(10) 2_556 2_556
C1 C5 Ti1 125.94(12) . 2_556
Ti1 C5 Ti1 57.34(5) . 2_556
C10 C9 C11 109.47(18) . .
C10 C9 Si1 113.18(14) . .
C11 C9 Si1 113.62(16) . .
C10 C9 H9 106.7 . .
C11 C9 H9 106.7 . .
Si1 C9 H9 106.7 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C14 C12 C13 109.19(17) . .
C14 C12 Si1 113.75(13) . .
C13 C12 Si1 113.18(15) . .
C14 C12 H12 106.8 . .
C13 C12 H12 106.8 . .
Si1 C12 H12 106.8 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C17 C15 C16 109.83(18) . .
C17 C15 Si1 113.37(15) . .
C16 C15 Si1 111.81(15) . .
C17 C15 H15 107.2 . .
C16 C15 H15 107.2 . .
Si1 C15 H15 107.2 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C3 C30 C5 106.97(14) 2_556 2_556
C3 C30 C34 143.12(16) 2_556 .
C5 C30 C34 109.85(14) 2_556 .
C3 C30 Ti1 120.40(12) 2_556 .
C5 C30 Ti1 80.70(10) 2_556 .
C34 C30 Ti1 68.52(10) . .
C3 C30 Ti1 68.72(10) 2_556 2_556
C5 C30 Ti1 70.23(9) 2_556 2_556
C34 C30 Ti1 126.62(12) . 2_556
Ti1 C30 Ti1 58.69(4) . 2_556
C33 C32 C5 107.88(15) . 2_556
C33 C32 Ti1 67.56(11) . .
C5 C32 Ti1 75.81(11) 2_556 .
C33 C32 H32 126.1 . .
C5 C32 H32 126.1 2_556 .
Ti1 C32 H32 122.2 . .
C32 C33 C34 111.97(15) . .
C32 C33 Ti1 79.54(11) . .
C34 C33 Ti1 68.98(10) . .
C32 C33 H33 124.0 . .
C34 C33 H33 124.0 . .
Ti1 C33 H33 118.9 . .
C33 C34 C30 103.51(14) . .
C33 C34 Si4 122.05(12) . .
C30 C34 Si4 128.13(13) . .
C33 C34 Ti1 74.98(10) . .
C30 C34 Ti1 75.21(10) . .
Si4 C34 Ti1 136.22(10) . .
C45 C44 C46 107.43(16) . .
C45 C44 Si4 112.29(13) . .
C46 C44 Si4 114.72(14) . .
C45 C44 H44 107.4 . .
C46 C44 H44 107.4 . .
Si4 C44 H44 107.4 . .
C44 C45 H45A 109.5 . .
C44 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C44 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C44 C46 H46A 109.5 . .
C44 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C44 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C49 C47 C48 108.41(18) . .
C49 C47 Si4 115.69(15) . .
C48 C47 Si4 114.70(15) . .
C49 C47 H47 105.7 . .
C48 C47 H47 105.7 . .
Si4 C47 H47 105.7 . .
C47 C48 H48A 109.5 . .
C47 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
C47 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C47 C49 H49A 109.5 . .
C47 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
C47 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C51 C50 C52 109.84(18) . .
C51 C50 Si4 116.62(14) . .
C52 C50 Si4 112.98(15) . .
C51 C50 H50 105.5 . .
C52 C50 H50 105.5 . .
Si4 C50 H50 105.5 . .
C50 C51 H51A 109.5 . .
C50 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C50 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
C50 C52 H52A 109.5 . .
C50 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C50 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
N1 C53 N1 152.2(2) . 2_556
N1 C53 Ti1 69.87(9) . .
N1 C53 Ti1 137.92(15) 2_556 .
N1 C53 Ti1 137.92(15) . 2_556
N1 C53 Ti1 69.86(9) 2_556 2_556
Ti1 C53 Ti1 68.13(7) . 2_556
C55 C54 C59 118.55(16) . .
C55 C54 N1 116.69(16) . .
C59 C54 N1 124.70(16) . .
C56 C55 C54 120.50(17) . .
C56 C55 H55 119.8 . .
C54 C55 H55 119.8 . .
C55 C56 C57 121.41(18) . .
C55 C56 H56 119.3 . .
C57 C56 H56 119.3 . .
C58 C57 C56 117.92(17) . .
C58 C57 C60 121.40(19) . .
C56 C57 C60 120.66(19) . .
C57 C58 C59 121.51(18) . .
C57 C58 H58 119.2 . .
C59 C58 H58 119.2 . .
C58 C59 C54 120.12(17) . .
C58 C59 H59 119.9 . .
C54 C59 H59 119.9 . .
C57 C60 H60A 109.5 . .
C57 C60 H60B 109.5 . .
H60A C60 H60B 109.5 . .
C57 C60 H60C 109.5 . .
H60A C60 H60C 109.5 . .
H60B C60 H60C 109.5 . .
C53 N1 C54 135.10(17) . .
C53 N1 Ti1 74.89(12) . .
C54 N1 Ti1 149.51(12) . .
C1 Si1 C9 107.36(9) . .
C1 Si1 C12 115.81(9) . .
C9 Si1 C12 110.17(9) . .
C1 Si1 C15 105.54(9) . .
C9 Si1 C15 107.40(10) . .
C12 Si1 C15 110.16(9) . .
C34 Si4 C50 106.36(8) . .
C34 Si4 C47 107.85(9) . .
C50 Si4 C47 113.61(9) . .
C34 Si4 C44 110.24(8) . .
C50 Si4 C44 111.61(9) . .
C47 Si4 C44 107.11(9) . .
N1 Ti1 C53 35.24(5) . .
N1 Ti1 C34 134.30(6) . .
C53 Ti1 C34 131.92(5) . .
N1 Ti1 C33 99.00(6) . .
C53 Ti1 C33 110.01(5) . .
C34 Ti1 C33 36.04(6) . .
N1 Ti1 C2 116.92(6) . .
C53 Ti1 C2 126.82(5) . .
C34 Ti1 C2 99.87(7) . .
C33 Ti1 C2 120.77(6) . .
N1 Ti1 C30 126.60(6) . .
C53 Ti1 C30 103.33(5) . .
C34 Ti1 C30 36.27(6) . .
C33 Ti1 C30 57.30(6) . .
C2 Ti1 C30 116.13(7) . .
N1 Ti1 C1 85.82(6) . .
C53 Ti1 C1 92.23(5) . .
C34 Ti1 C1 134.86(6) . .
C33 Ti1 C1 147.92(6) . .
C2 Ti1 C1 35.01(6) . .
C30 Ti1 C1 140.92(6) . .
N1 Ti1 Ti1 91.15(4) . 2_556
C53 Ti1 Ti1 55.94(4) . 2_556
C34 Ti1 Ti1 100.41(5) . 2_556
C33 Ti1 Ti1 113.69(6) . 2_556
C2 Ti1 Ti1 111.04(5) . 2_556
C30 Ti1 Ti1 64.46(5) . 2_556
C1 Ti1 Ti1 97.79(5) . 2_556
N1 Ti1 C3 143.16(6) . .
C53 Ti1 C3 129.90(5) . .
C34 Ti1 C3 82.04(6) . .
C33 Ti1 C3 115.53(6) . .
C2 Ti1 C3 33.68(6) . .
C30 Ti1 C3 85.08(7) . .
C1 Ti1 C3 58.20(6) . .
Ti1 Ti1 C3 86.60(4) 2_556 .
N1 Ti1 C5 90.41(6) . .
C53 Ti1 C5 76.46(4) . .
C34 Ti1 C5 134.25(6) . .
C33 Ti1 C5 170.27(6) . .
C2 Ti1 C5 55.70(6) . .
C30 Ti1 C5 114.78(6) . .
C1 Ti1 C5 34.69(6) . .
Ti1 Ti1 C5 63.31(5) 2_556 .
C3 Ti1 C5 55.98(6) . .
N1 Ti1 C32 78.17(6) . .
C53 Ti1 C32 78.35(4) . .
C34 Ti1 C32 58.26(6) . .
C33 Ti1 C32 32.89(6) . .
C2 Ti1 C32 153.66(6) . .
C30 Ti1 C32 56.11(6) . .
C1 Ti1 C32 162.79(6) . .
Ti1 Ti1 C32 88.87(5) 2_556 .
C3 Ti1 C32 138.44(6) . .
C5 Ti1 C32 149.88(6) . .
N1 Ti1 C30 121.53(6) . 2_556
C53 Ti1 C30 97.58(5) . 2_556
C34 Ti1 C30 101.28(6) . 2_556
C33 Ti1 C30 137.07(6) . 2_556
C2 Ti1 C30 54.74(6) . 2_556
C30 Ti1 C30 85.23(8) . 2_556
C1 Ti1 C30 57.00(6) . 2_556
Ti1 Ti1 C30 56.86(4) 2_556 2_556
C3 Ti1 C30 33.08(5) . 2_556
C5 Ti1 C30 33.23(5) . 2_556
C32 Ti1 C30 137.96(6) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.436(2) .
C1 C5 1.459(2) .
C1 Si1 1.879(2) .
C1 Ti1 2.394(2) .
C2 C3 1.401(2) .
C2 Ti1 2.380(2) .
C2 H2 0.9500 .
C3 C30 1.435(2) 2_556
C3 Ti1 2.4504(18) .
C3 H3 0.9500 .
C5 C32 1.439(2) 2_556
C5 C30 1.450(2) 2_556
C5 Ti1 2.4909(18) .
C5 Ti1 2.587(2) 2_556
C9 C10 1.533(3) .
C9 C11 1.538(3) .
C9 Si1 1.893(2) .
C9 H9 1.0000 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C14 1.534(3) .
C12 C13 1.539(3) .
C12 Si1 1.898(2) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.539(3) .
C15 C16 1.542(3) .
C15 Si1 1.902(2) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C30 C3 1.435(2) 2_556
C30 C5 1.450(2) 2_556
C30 C34 1.462(2) .
C30 Ti1 2.3888(19) .
C30 Ti1 2.5742(18) 2_556
C32 C33 1.398(2) .
C32 C5 1.439(2) 2_556
C32 Ti1 2.531(2) .
C32 H32 0.9500 .
C33 C34 1.449(2) .
C33 Ti1 2.3788(19) .
C33 H33 0.9500 .
C34 Si4 1.8740(18) .
C34 Ti1 2.2990(18) .
C44 C45 1.528(3) .
C44 C46 1.542(3) .
C44 Si4 1.908(2) .
C44 H44 1.0000 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 C49 1.523(3) .
C47 C48 1.540(3) .
C47 Si4 1.895(2) .
C47 H47 1.0000 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C50 C51 1.528(3) .
C50 C52 1.539(3) .
C50 Si4 1.8885(19) .
C50 H50 1.0000 .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C53 N1 1.3004(15) .
C53 N1 1.3004(15) 2_556
C53 Ti1 2.176(2) .
C53 Ti1 2.176(2) 2_556
C54 C55 1.393(2) .
C54 C59 1.395(2) .
C54 N1 1.410(2) .
C55 C56 1.386(3) .
C55 H55 0.9500 .
C56 C57 1.389(3) .
C56 H56 0.9500 .
C57 C58 1.384(3) .
C57 C60 1.511(3) .
C58 C59 1.393(3) .
C58 H58 0.9500 .
C59 H59 0.9500 .
C60 H60A 0.9800 .
C60 H60B 0.9800 .
C60 H60C 0.9800 .
N1 Ti1 2.1159(15) .
Ti1 Ti1 2.4374(8) 2_556
Ti1 C30 2.5741(18) 2_556
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_4
C5 C1 C2 C3 -3.9(2) . .
Si1 C1 C2 C3 -157.63(13) . .
Ti1 C1 C2 C3 66.43(14) . .
C5 C1 C2 Ti1 -70.36(12) . .
Si1 C1 C2 Ti1 135.94(12) . .
C1 C2 C3 C30 5.6(2) . 2_556
Ti1 C2 C3 C30 70.24(13) . 2_556
C1 C2 C3 Ti1 -64.65(13) . .
C2 C1 C5 C32 -176.4(2) . 2_556
Si1 C1 C5 C32 -27.9(4) . 2_556
Ti1 C1 C5 C32 116.4(3) . 2_556
C2 C1 C5 C30 0.8(2) . 2_556
Si1 C1 C5 C30 149.30(14) . 2_556
Ti1 C1 C5 C30 -66.42(13) . 2_556
C2 C1 C5 Ti1 67.18(12) . .
Si1 C1 C5 Ti1 -144.28(16) . .
C2 C1 C5 Ti1 74.32(17) . 2_556
Si1 C1 C5 Ti1 -137.14(13) . 2_556
Ti1 C1 C5 Ti1 7.13(11) . 2_556
C5 C32 C33 C34 3.6(2) 2_556 .
Ti1 C32 C33 C34 -62.10(13) . .
C5 C32 C33 Ti1 65.68(13) 2_556 .
C32 C33 C34 C30 -1.7(2) . .
Ti1 C33 C34 C30 -70.36(12) . .
C32 C33 C34 Si4 -155.84(14) . .
Ti1 C33 C34 Si4 135.56(14) . .
C32 C33 C34 Ti1 68.61(14) . .
C3 C30 C34 C33 -177.4(2) 2_556 .
C5 C30 C34 C33 -0.7(2) 2_556 .
Ti1 C30 C34 C33 70.18(12) . .
Ti1 C30 C34 C33 78.90(17) 2_556 .
C3 C30 C34 Si4 -25.5(4) 2_556 .
C5 C30 C34 Si4 151.16(14) 2_556 .
Ti1 C30 C34 Si4 -137.91(16) . .
Ti1 C30 C34 Si4 -129.19(13) 2_556 .
C3 C30 C34 Ti1 112.4(3) 2_556 .
C5 C30 C34 Ti1 -70.93(13) 2_556 .
Ti1 C30 C34 Ti1 8.72(11) 2_556 .
C59 C54 C55 C56 -0.1(3) . .
N1 C54 C55 C56 177.24(18) . .
C54 C55 C56 C57 0.2(3) . .
C55 C56 C57 C58 0.0(3) . .
C55 C56 C57 C60 178.3(2) . .
C56 C57 C58 C59 -0.2(3) . .
C60 C57 C58 C59 -178.5(2) . .
C57 C58 C59 C54 0.3(3) . .
C55 C54 C59 C58 -0.1(3) . .
N1 C54 C59 C58 -177.21(18) . .
N1 C53 N1 C54 5.06(17) 2_556 .
Ti1 C53 N1 C54 -173.5(2) . .
Ti1 C53 N1 C54 -176.99(13) 2_556 .
N1 C53 N1 Ti1 178.53(4) 2_556 .
Ti1 C53 N1 Ti1 -3.53(10) 2_556 .
C55 C54 N1 C53 148.96(17) . .
C59 C54 N1 C53 -33.9(3) . .
C55 C54 N1 Ti1 -18.5(3) . .
C59 C54 N1 Ti1 158.61(19) . .
C2 C1 Si1 C9 -33.68(16) . .
C5 C1 Si1 C9 -178.73(17) . .
Ti1 C1 Si1 C9 60.13(15) . .
C2 C1 Si1 C12 -157.21(13) . .
C5 C1 Si1 C12 57.74(19) . .
Ti1 C1 Si1 C12 -63.40(15) . .
C2 C1 Si1 C15 80.66(15) . .
C5 C1 Si1 C15 -64.39(18) . .
Ti1 C1 Si1 C15 174.47(13) . .
C10 C9 Si1 C1 -62.93(17) . .
C11 C9 Si1 C1 171.41(16) . .
C10 C9 Si1 C12 64.00(17) . .
C11 C9 Si1 C12 -61.66(19) . .
C10 C9 Si1 C15 -176.02(15) . .
C11 C9 Si1 C15 58.33(19) . .
C14 C12 Si1 C1 -33.90(18) . .
C13 C12 Si1 C1 -159.28(14) . .
C14 C12 Si1 C9 -155.96(15) . .
C13 C12 Si1 C9 78.67(16) . .
C14 C12 Si1 C15 85.74(16) . .
C13 C12 Si1 C15 -39.63(17) . .
C33 C34 Si4 C50 162.89(15) . .
C30 C34 Si4 C50 15.58(19) . .
Ti1 C34 Si4 C50 -94.91(14) . .
C33 C34 Si4 C47 40.67(18) . .
C30 C34 Si4 C47 -106.63(17) . .
Ti1 C34 Si4 C47 142.88(12) . .
C33 C34 Si4 C44 -75.96(17) . .
C30 C34 Si4 C44 136.74(16) . .
Ti1 C34 Si4 C44 26.25(15) . .
C51 C50 Si4 C34 155.87(17) . .
C52 C50 Si4 C34 -75.45(15) . .
C51 C50 Si4 C47 -85.6(2) . .
C52 C50 Si4 C47 43.04(16) . .
C51 C50 Si4 C44 35.6(2) . .
C52 C50 Si4 C44 164.27(13) . .
C49 C47 Si4 C34 34.22(18) . .
C48 C47 Si4 C34 161.59(15) . .
C49 C47 Si4 C50 -83.42(18) . .
C48 C47 Si4 C50 43.96(19) . .
C49 C47 Si4 C44 152.87(16) . .
C48 C47 Si4 C44 -79.76(17) . .
