#------------------------------------------------------------------------------
#$Date: 2019-11-24 12:59:58 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/90/4089069.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_4089069
loop_
_publ_author_name
'Adler, Christian'
'Frerichs, Nils'
'Schmidtmann, Marc'
'Beckhaus, Rüdiger'
_publ_section_title
;
 Zwitterionic d0Metal Complexes [(Cy2N)3M]+[(μ-Me)B(C6F5)3]−(M =
 Ti, Zr, Hf) Derived from Tris(dicyclohexylamido)methyl Metal Precursors
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3728
_journal_paper_doi               10.1021/acs.organomet.6b00688
_journal_volume                  35
_journal_year                    2016
_chemical_formula_structural     '[Ti(N(C6H11)2)3] [B(CH3)(C6F5)3] *2.5C7H8'
_chemical_formula_sum            'C72.5 H89 B F15 N3 Ti'
_chemical_formula_weight         1346.17
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.9270(4)
_cell_length_b                   16.9270(4)
_cell_length_c                   39.8167(12)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.41
_cell_volume                     9880.0(4)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            69469
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.026
_diffrn_reflns_theta_min         1.480
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             4242
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4840
_reflns_number_total             6420
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00688_si_002.cif
_cod_data_source_block           '[(Cy2N)3Ti][MeB(C6F5)3_(3-Ti)'
_cod_original_cell_volume        9879.9(5)
_cod_original_formula_sum        'C72.50 H89 B F15 N3 Ti'
_cod_database_code               4089069
_shelx_shelxl_version_number     2014/7
_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   0.968
_shelx_estimated_absorpt_t_max   0.968
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.6667 0.3333 0.52308(2) 0.01725(11) Uani 1 3 d S T P . .
N1 N 0.57093(9) 0.22206(10) 0.53958(3) 0.0222(3) Uani 1 1 d . . . . .
C1 C 0.48088(11) 0.19989(11) 0.52573(4) 0.0232(3) Uani 1 1 d . . . . .
H1 H 0.4908 0.2570 0.5145 0.028 Uiso 1 1 calc R U . . .
C2 C 0.44473(11) 0.12661(12) 0.49806(4) 0.0263(3) Uani 1 1 d . . . . .
H2A H 0.4930 0.1419 0.4811 0.032 Uiso 1 1 calc R U . . .
H2B H 0.4286 0.0668 0.5080 0.032 Uiso 1 1 calc R U . . .
C3 C 0.36074(12) 0.12042(14) 0.48110(5) 0.0343(4) Uani 1 1 d . . . . .
H3A H 0.3782 0.1788 0.4697 0.041 Uiso 1 1 calc R U . . .
H3B H 0.3376 0.0717 0.4639 0.041 Uiso 1 1 calc R U . . .
C4 C 0.28525(13) 0.09982(15) 0.50653(6) 0.0404(5) Uani 1 1 d . . . . .
H4A H 0.2336 0.1005 0.4951 0.048 Uiso 1 1 calc R U . . .
H4B H 0.2627 0.0383 0.5161 0.048 Uiso 1 1 calc R U . . .
C5 C 0.32074(14) 0.17005(16) 0.53449(6) 0.0415(5) Uani 1 1 d . . . . .
H5A H 0.2720 0.1537 0.5514 0.050 Uiso 1 1 calc R U . . .
H5B H 0.3372 0.2306 0.5251 0.050 Uiso 1 1 calc R U . . .
C6 C 0.40423(13) 0.17555(13) 0.55154(5) 0.0312(4) Uani 1 1 d . . . . .
H6A H 0.3871 0.1162 0.5621 0.037 Uiso 1 1 calc R U . . .
H6B H 0.4263 0.2225 0.5694 0.037 Uiso 1 1 calc R U . . .
C7 C 0.58150(13) 0.16328(12) 0.56450(4) 0.0281(4) Uani 1 1 d . . . . .
H7 H 0.6487 0.1871 0.5657 0.034 Uiso 1 1 calc R U . . .
C8 C 0.54000(14) 0.06262(13) 0.55518(5) 0.0326(4) Uani 1 1 d . . . . .
H8A H 0.5600 0.0574 0.5323 0.039 Uiso 1 1 calc R U . . .
H8B H 0.4726 0.0330 0.5551 0.039 Uiso 1 1 calc R U . . .
C9 C 0.56990(16) 0.01424(15) 0.58038(5) 0.0417(5) Uani 1 1 d . . . . .
H9A H 0.5401 -0.0514 0.5748 0.050 Uiso 1 1 calc R U . . .
H9B H 0.6367 0.0400 0.5788 0.050 Uiso 1 1 calc R U . . .
C10 C 0.54481(19) 0.02528(17) 0.61613(6) 0.0509(6) Uani 1 1 d . . . . .
H10B H 0.4776 -0.0064 0.6183 0.061 Uiso 1 1 calc R U . . .
H10A H 0.5680 -0.0035 0.6320 0.061 Uiso 1 1 calc R U . . .
C11 C 0.58436(19) 0.12489(17) 0.62527(5) 0.0496(6) Uani 1 1 d . . . . .
H11B H 0.6518 0.1553 0.6253 0.060 Uiso 1 1 calc R U . . .
H11A H 0.5643 0.1296 0.6482 0.060 Uiso 1 1 calc R U . . .
C12 C 0.55398(16) 0.17333(15) 0.60040(4) 0.0378(5) Uani 1 1 d . . . . .
H12A H 0.5828 0.2388 0.6063 0.045 Uiso 1 1 calc R U . . .
H12B H 0.4870 0.1465 0.6016 0.045 Uiso 1 1 calc R U . . .
F1 F 0.84176(7) 0.47783(7) 0.44885(2) 0.0288(2) Uani 1 1 d . . . . .
F2 F 0.94165(8) 0.64768(8) 0.42673(3) 0.0474(3) Uani 1 1 d . . . . .
F3 F 0.88563(11) 0.70714(8) 0.37316(4) 0.0628(5) Uani 1 1 d . . . . .
F4 F 0.72526(8) 0.59113(8) 0.34227(3) 0.0363(3) Uani 1 1 d . . . . .
F5 F 0.62521(7) 0.42251(7) 0.36304(2) 0.0263(2) Uani 1 1 d . . . . .
C13 C 0.72532(10) 0.43985(10) 0.40807(3) 0.0154(3) Uani 1 1 d . . . . .
C14 C 0.80832(11) 0.50247(10) 0.42228(4) 0.0210(3) Uani 1 1 d . . . . .
C15 C 0.86262(12) 0.59084(12) 0.41122(4) 0.0300(4) Uani 1 1 d . . . . .
C16 C 0.83438(14) 0.62142(12) 0.38421(5) 0.0347(4) Uani 1 1 d . . . . .
C17 C 0.75343(12) 0.56285(12) 0.36887(4) 0.0261(3) Uani 1 1 d . . . . .
C18 C 0.70144(10) 0.47503(11) 0.38075(4) 0.0192(3) Uani 1 1 d . . . . .
C19 C 0.6667 0.3333 0.46334(6) 0.0169(5) Uani 1 3 d S T P . .
H19 H 0.6628(14) 0.3856(13) 0.4712(5) 0.026(5) Uiso 1 1 d . . . . .
B1 B 0.6667 0.3333 0.42123(7) 0.0139(5) Uani 1 3 d S T P . .
C20 C 0.2728(5) 0.1797(4) 0.64099(17) 0.0445(14) Uani 0.5 1 d . U P A -1
C21 C 0.3079(6) 0.2268(5) 0.6703(2) 0.0525(17) Uani 0.5 1 d . U P A -1
H21 H 0.2983 0.2757 0.6763 0.063 Uiso 0.5 1 calc R U P A -1
C22 C 0.3578(6) 0.2018(5) 0.69133(18) 0.0615(19) Uani 0.5 1 d . U P A -1
H22 H 0.3851 0.2356 0.7112 0.074 Uiso 0.5 1 calc R U P A -1
C23 C 0.3674(5) 0.1271(5) 0.6830(2) 0.0492(16) Uani 0.5 1 d . U P A -1
H23 H 0.4001 0.1086 0.6973 0.059 Uiso 0.5 1 calc R U P A -1
C24 C 0.3286(4) 0.0806(4) 0.65358(17) 0.0436(14) Uani 0.5 1 d . U P A -1
H24 H 0.3347 0.0294 0.6480 0.052 Uiso 0.5 1 calc R U P A -1
C25 C 0.2822(5) 0.1053(4) 0.63248(15) 0.0430(12) Uani 0.5 1 d . U P A -1
H25 H 0.2566 0.0724 0.6123 0.052 Uiso 0.5 1 calc R U P A -1
C26 C 0.2268(6) 0.2075(5) 0.61986(15) 0.084(2) Uani 0.5 1 d . U P A -1
H26A H 0.1750 0.2049 0.6319 0.126 Uiso 0.5 1 calc R U P A -1
H26B H 0.2045 0.1672 0.6003 0.126 Uiso 0.5 1 calc R U P A -1
H26C H 0.2681 0.2702 0.6125 0.126 Uiso 0.5 1 calc R U P A -1
C27 C 0.6667 0.3333 0.72085(11) 0.0522(10) Uani 1 3 d S TU P . .
C28 C 0.6204(6) 0.3713(6) 0.73178(18) 0.0506(18) Uani 0.3333 1 d . U P B -1
H28 H 0.6010 0.3998 0.7158 0.061 Uiso 0.3333 1 calc R U P B -1
C29 C 0.5982(7) 0.3725(7) 0.7646(2) 0.062(2) Uani 0.3333 1 d . U P B -1
H29 H 0.5616 0.3980 0.7710 0.074 Uiso 0.3333 1 calc R U P B -1
C30 C 0.6294(13) 0.3370(14) 0.7877(3) 0.076(5) Uani 0.3333 1 d . U P B -1
H30 H 0.6177 0.3412 0.8107 0.091 Uiso 0.3333 1 calc R U P B -1
C31 C 0.679(2) 0.293(2) 0.7787(4) 0.136(10) Uani 0.3333 1 d . U P B -1
H31 H 0.6970 0.2644 0.7950 0.164 Uiso 0.3333 1 calc R U P B -1
C32 C 0.7003(11) 0.2955(12) 0.7453(2) 0.109(5) Uani 0.3333 1 d . U P B -1
H32 H 0.7377 0.2714 0.7383 0.131 Uiso 0.3333 1 calc R U P B -1
C33 C 0.6971(10) 0.341(2) 0.68422(18) 0.063(3) Uani 0.3333 1 d . U P B -1
H33A H 0.7285 0.3063 0.6810 0.095 Uiso 0.3333 1 calc R U P B -1
H33B H 0.7388 0.4055 0.6787 0.095 Uiso 0.3333 1 calc R U P B -1
H33C H 0.6437 0.3169 0.6695 0.095 Uiso 0.3333 1 calc R U P B -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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Ti1 N1 108.53(4) 2_655 .
N1 Ti1 N1 108.52(4) 2_655 3_665
N1 Ti1 N1 108.53(4) . 3_665
N1 Ti1 H19 119.1(5) 2_655 .
N1 Ti1 H19 122.1(5) . .
N1 Ti1 H19 86.4(5) 3_665 .
C7 N1 C1 122.32(13) . .
C7 N1 Ti1 125.01(11) . .
C1 N1 Ti1 112.63(10) . .
N1 C1 C2 114.50(14) . .
N1 C1 C6 116.20(14) . .
C2 C1 C6 108.64(14) . .
N1 C1 H1 105.5 . .
C2 C1 H1 105.5 . .
C6 C1 H1 105.5 . .
C3 C2 C1 110.65(15) . .
C3 C2 H2A 109.5 . .
C1 C2 H2A 109.5 . .
C3 C2 H2B 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C4 C3 C2 111.46(16) . .
C4 C3 H3A 109.3 . .
C2 C3 H3A 109.3 . .
C4 C3 H3B 109.3 . .
C2 C3 H3B 109.3 . .
H3A C3 H3B 108.0 . .
C5 C4 C3 110.45(16) . .
C5 C4 H4A 109.6 . .
C3 C4 H4A 109.6 . .
C5 C4 H4B 109.6 . .
C3 C4 H4B 109.6 . .
H4A C4 H4B 108.1 . .
C4 C5 C6 111.45(17) . .
C4 C5 H5A 109.3 . .
C6 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
C6 C5 H5B 109.3 . .
H5A C5 H5B 108.0 . .
C5 C6 C1 110.47(15) . .
C5 C6 H6A 109.6 . .
C1 C6 H6A 109.6 . .
C5 C6 H6B 109.6 . .
C1 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
N1 C7 C8 116.38(14) . .
N1 C7 C12 113.83(15) . .
C8 C7 C12 110.67(15) . .
N1 C7 H7 104.9 . .
C8 C7 H7 104.9 . .
C12 C7 H7 104.9 . .
C7 C8 C9 110.24(17) . .
C7 C8 H8A 109.6 . .
C9 C8 H8A 109.6 . .
C7 C8 H8B 109.6 . .
C9 C8 H8B 109.6 . .
H8A C8 H8B 108.1 . .
C10 C9 C8 111.07(18) . .
C10 C9 H9A 109.4 . .
C8 C9 H9A 109.4 . .
C10 C9 H9B 109.4 . .
C8 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
C11 C10 C9 111.46(18) . .
C11 C10 H10B 109.3 . .
C9 C10 H10B 109.3 . .
C11 C10 H10A 109.3 . .
C9 C10 H10A 109.3 . .
H10B C10 H10A 108.0 . .
C10 C11 C12 111.18(19) . .
C10 C11 H11B 109.4 . .
C12 C11 H11B 109.4 . .
C10 C11 H11A 109.4 . .
C12 C11 H11A 109.4 . .
H11B C11 H11A 108.0 . .
C11 C12 C7 109.91(18) . .
C11 C12 H12A 109.7 . .
C7 C12 H12A 109.7 . .
C11 C12 H12B 109.7 . .
C7 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
C14 C13 C18 113.01(13) . .
C14 C13 B1 122.08(13) . .
C18 C13 B1 124.78(13) . .
F1 C14 C15 115.29(14) . .
F1 C14 C13 120.01(13) . .
C15 C14 C13 124.69(14) . .
F2 C15 C16 119.80(15) . .
F2 C15 C14 120.96(15) . .
C16 C15 C14 119.23(16) . .
F3 C16 C17 120.64(17) . .
F3 C16 C15 120.32(17) . .
C17 C16 C15 119.04(15) . .
F4 C17 C16 119.89(15) . .
F4 C17 C18 120.37(15) . .
C16 C17 C18 119.74(15) . .
F5 C18 C17 114.69(13) . .
F5 C18 C13 120.97(13) . .
C17 C18 C13 124.29(14) . .
B1 C19 Ti1 180.0 . .
B1 C19 H19 108.8(12) . .
Ti1 C19 H19 71.2(12) . .
C13 B1 C13 110.41(9) 3_665 2_655
C13 B1 C13 110.40(9) 3_665 .
C13 B1 C13 110.41(9) 2_655 .
C13 B1 C19 108.52(10) 3_665 .
C13 B1 C19 108.52(10) 2_655 .
C13 B1 C19 108.52(10) . .
C21 C20 C26 118.4(6) . .
C21 C20 C25 121.6(7) . .
C26 C20 C25 120.1(6) . .
C20 C21 C22 119.1(6) . .
C20 C21 H21 120.5 . .
C22 C21 H21 120.5 . .
C23 C22 C21 119.7(6) . .
C23 C22 H22 120.2 . .
C21 C22 H22 120.2 . .
C24 C23 C22 118.8(7) . .
C24 C23 H23 120.6 . .
C22 C23 H23 120.6 . .
C25 C24 C23 122.4(7) . .
C25 C24 H24 118.8 . .
C23 C24 H24 118.8 . .
C24 C25 C20 118.4(6) . .
C24 C25 H25 120.8 . .
C20 C25 H25 120.8 . .
C20 C26 H26A 109.5 . .
C20 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C20 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C28 C27 C32 117.6(6) . .
C28 C27 C33 122.1(8) . .
C32 C27 C33 119.7(7) . .
C27 C28 C29 124.1(7) . .
C27 C28 H28 117.9 . .
C29 C28 H28 117.9 . .
C30 C29 C28 118.5(9) . .
C30 C29 H29 120.8 . .
C28 C29 H29 120.8 . .
C29 C30 C31 122.1(14) . .
C29 C30 H30 118.9 . .
C31 C30 H30 118.9 . .
C32 C31 C30 116.5(16) . .
C32 C31 H31 121.7 . .
C30 C31 H31 121.7 . .
C31 C32 C27 120.8(10) . .
C31 C32 H32 119.6 . .
C27 C32 H32 119.6 . .
C27 C33 H33A 109.5 . .
C27 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C27 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.8850(14) 2_655
Ti1 N1 1.8850(14) .
Ti1 N1 1.8850(14) 3_665
Ti1 H19 2.260(19) .
N1 C7 1.478(2) .
N1 C1 1.482(2) .
C1 C2 1.539(2) .
C1 C6 1.541(2) .
C1 H1 1.0000 .
C2 C3 1.529(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.528(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.516(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.528(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.529(3) .
C7 C12 1.539(2) .
C7 H7 1.0000 .
C8 C9 1.533(3) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.523(3) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.515(4) .
C10 H10B 0.9900 .
C10 H10A 0.9900 .
C11 C12 1.529(3) .
C11 H11B 0.9900 .
C11 H11A 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
F1 C14 1.3599(17) .
F2 C15 1.345(2) .
F3 C16 1.3389(19) .
F4 C17 1.3442(18) .
F5 C18 1.3436(18) .
C13 C14 1.389(2) .
C13 C18 1.394(2) .
C13 B1 1.6496(16) .
C14 C15 1.379(2) .
C15 C16 1.379(3) .
C16 C17 1.369(3) .
C17 C18 1.378(2) .
C19 B1 1.677(4) .
C19 H19 0.972(19) .
B1 C13 1.6495(16) 3_665
B1 C13 1.6496(16) 2_655
C20 C21 1.371(9) .
C20 C26 1.380(10) .
C20 C25 1.388(8) .
C21 C22 1.396(11) .
C21 H21 0.9500 .
C22 C23 1.392(10) .
C22 H22 0.9500 .
C23 C24 1.381(8) .
C23 H23 0.9500 .
C24 C25 1.351(9) .
C24 H24 0.9500 .
C25 H25 0.9500 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 C28 1.312(7) .
C27 C32 1.430(9) .
C27 C33 1.530(8) .
C28 C29 1.363(11) .
C28 H28 0.9500 .
C29 C30 1.342(14) .
C29 H29 0.9500 .
C30 C31 1.413(16) .
C30 H30 0.9500 .
C31 C32 1.374(17) .
C31 H31 0.9500 .
C32 H32 0.9500 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
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
N1 Ti1 N1 C7 6.76(15) 2_655 .
N1 Ti1 N1 C7 -110.99(10) 3_665 .
N1 Ti1 N1 C1 -175.31(9) 2_655 .
N1 Ti1 N1 C1 66.94(14) 3_665 .
C7 N1 C1 C2 -78.72(18) . .
Ti1 N1 C1 C2 103.28(13) . .
C7 N1 C1 C6 49.3(2) . .
Ti1 N1 C1 C6 -128.72(13) . .
N1 C1 C2 C3 -169.99(13) . .
C6 C1 C2 C3 58.27(18) . .
C1 C2 C3 C4 -57.4(2) . .
C2 C3 C4 C5 55.3(2) . .
C3 C4 C5 C6 -55.8(2) . .
C4 C5 C6 C1 58.4(2) . .
N1 C1 C6 C5 170.52(16) . .
C2 C1 C6 C5 -58.7(2) . .
C1 N1 C7 C8 53.4(2) . .
Ti1 N1 C7 C8 -128.86(15) . .
C1 N1 C7 C12 -77.1(2) . .
Ti1 N1 C7 C12 100.62(17) . .
N1 C7 C8 C9 170.55(16) . .
C12 C7 C8 C9 -57.5(2) . .
C7 C8 C9 C10 56.2(2) . .
C8 C9 C10 C11 -55.8(3) . .
C9 C10 C11 C12 56.2(3) . .
C10 C11 C12 C7 -56.8(3) . .
N1 C7 C12 C11 -169.02(17) . .
C8 C7 C12 C11 57.7(2) . .
C18 C13 C14 F1 -178.89(14) . .
B1 C13 C14 F1 -2.9(2) . .
C18 C13 C14 C15 0.4(2) . .
B1 C13 C14 C15 176.42(16) . .
F1 C14 C15 F2 -1.6(3) . .
C13 C14 C15 F2 179.04(17) . .
F1 C14 C15 C16 179.47(17) . .
C13 C14 C15 C16 0.1(3) . .
F2 C15 C16 F3 0.6(3) . .
C14 C15 C16 F3 179.54(19) . .
F2 C15 C16 C17 -179.53(18) . .
C14 C15 C16 C17 -0.6(3) . .
F3 C16 C17 F4 0.6(3) . .
C15 C16 C17 F4 -179.27(18) . .
F3 C16 C17 C18 -179.65(18) . .
C15 C16 C17 C18 0.5(3) . .
F4 C17 C18 F5 2.2(2) . .
C16 C17 C18 F5 -177.56(16) . .
F4 C17 C18 C13 179.86(15) . .
C16 C17 C18 C13 0.1(3) . .
C14 C13 C18 F5 176.98(13) . .
B1 C13 C18 F5 1.1(2) . .
C14 C13 C18 C17 -0.6(2) . .
B1 C13 C18 C17 -176.41(15) . .
C14 C13 B1 C13 -74.6(2) . 3_665
C18 C13 B1 C13 100.87(12) . 3_665
C14 C13 B1 C13 163.00(14) . 2_655
C18 C13 B1 C13 -21.5(2) . 2_655
C14 C13 B1 C19 44.18(14) . .
C18 C13 B1 C19 -140.32(12) . .
C26 C20 C21 C22 -177.4(7) . .
C25 C20 C21 C22 3.1(10) . .
C20 C21 C22 C23 -3.1(11) . .
C21 C22 C23 C24 1.4(11) . .
C22 C23 C24 C25 0.5(10) . .
C23 C24 C25 C20 -0.6(9) . .
C21 C20 C25 C24 -1.2(9) . .
C26 C20 C25 C24 179.3(6) . .
C32 C27 C28 C29 -3.7(12) . .
C33 C27 C28 C29 -174.4(13) . .
C27 C28 C29 C30 3.6(18) . .
C28 C29 C30 C31 -4(3) . .
C29 C30 C31 C32 5(4) . .
C30 C31 C32 C27 -5(4) . .
C28 C27 C32 C31 4(2) . .
C33 C27 C32 C31 175(2) . .
