# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Arkadi Vigalok'
'Israel Goldberg'
'Ella Tzadka'

_publ_contact_author_name        'Arkadi Vigalok'
_publ_contact_author_email       AVIGAL@POST.TAU.AC.IL

_publ_section_title              
;
Entry to new N,O-ligands from oxygen-depleted
calixarenes
;

# Attachment 'ar26.cif'

data_ar26
_database_code_depnum_ccdc_archive 'CCDC 702763'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H70 N6 O2'
_chemical_formula_sum            'C62 H70 N6 O2'
_chemical_formula_weight         931.24

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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'

_cell_length_a                   11.6844(5)
_cell_length_b                   41.4198(15)
_cell_length_c                   10.9193(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.280(2)
_cell_angle_gamma                90.00
_cell_volume                     5229.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5570
_cell_measurement_theta_min      1.41
_cell_measurement_theta_max      25.06

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.4 deg. \w scans'
_diffrn_detector_area_resol_mean 12.8
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18124
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         23.00
_reflns_number_total             6705
_reflns_number_gt                4505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Nonius B.V.'
_computing_cell_refinement       Denzo
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The crystals are characterized by high mosaicity and very poor diffraction.
In addition, they don't seem to be entirely single.
Some of the t-Bu groups exhibit partial orientational disorder, which
could not be resolved.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+7.9388P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6705
_refine_ls_number_parameters     643
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.1923
_refine_ls_wR_factor_gt          0.1661
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.1159(4) 0.15454(10) 0.3867(4) 0.0327(11) Uani 1 1 d . . .
H1A H 1.1042 0.1774 0.3619 0.039 Uiso 1 1 calc R . .
H1B H 1.1988 0.1514 0.4187 0.039 Uiso 1 1 calc R . .
C2 C 1.0808(4) 0.13274(10) 0.2759(4) 0.0300(11) Uani 1 1 d . . .
C3 C 1.1455(4) 0.10546(10) 0.2579(4) 0.0348(11) Uani 1 1 d . . .
H3 H 1.2179 0.1027 0.3090 0.042 Uiso 1 1 calc R . .
C4 C 1.1104(4) 0.08192(10) 0.1692(4) 0.0331(11) Uani 1 1 d . . .
C5 C 1.0067(4) 0.08817(10) 0.0918(4) 0.0336(11) Uani 1 1 d . . .
H5 H 0.9807 0.0730 0.0287 0.040 Uiso 1 1 calc R . .
C6 C 0.9403(4) 0.11522(10) 0.1024(4) 0.0306(11) Uani 1 1 d . . .
C7 C 0.9766(4) 0.13732(10) 0.1962(4) 0.0310(11) Uani 1 1 d . . .
C8 C 0.8247(4) 0.12098(10) 0.0223(4) 0.0302(11) Uani 1 1 d . . .
H8A H 0.8194 0.1077 -0.0538 0.036 Uiso 1 1 calc R . .
H8B H 0.8177 0.1440 -0.0022 0.036 Uiso 1 1 calc R . .
C9 C 0.7270(4) 0.11191(10) 0.0950(4) 0.0303(11) Uani 1 1 d . . .
C10 C 0.7210(4) 0.07980(10) 0.1289(4) 0.0317(11) Uani 1 1 d . . .
H10 H 0.7697 0.0647 0.0962 0.038 Uiso 1 1 calc R . .
C11 C 0.6462(4) 0.06860(11) 0.2095(4) 0.0337(11) Uani 1 1 d . . .
C12 C 0.5776(4) 0.09173(11) 0.2550(4) 0.0327(11) Uani 1 1 d . . .
H12 H 0.5273 0.0851 0.3112 0.039 Uiso 1 1 calc R . .
C13 C 0.5788(4) 0.12422(10) 0.2223(4) 0.0294(11) Uani 1 1 d . . .
C14 C 0.6517(4) 0.13441(10) 0.1372(4) 0.0302(11) Uani 1 1 d . . .
C15 C 0.5027(4) 0.14677(11) 0.2870(4) 0.0333(11) Uani 1 1 d . . .
H15A H 0.5087 0.1691 0.2558 0.040 Uiso 1 1 calc R . .
H15B H 0.4209 0.1399 0.2682 0.040 Uiso 1 1 calc R . .
C16 C 0.5407(4) 0.14609(10) 0.4258(4) 0.0300(11) Uani 1 1 d . . .
C17 C 0.4868(4) 0.12483(10) 0.4986(4) 0.0332(11) Uani 1 1 d . . .
H17 H 0.4194 0.1138 0.4616 0.040 Uiso 1 1 calc R . .
C18 C 0.5274(4) 0.11903(11) 0.6236(4) 0.0350(11) Uani 1 1 d . . .
C19 C 0.6254(4) 0.13629(10) 0.6739(4) 0.0341(11) Uani 1 1 d . . .
H19 H 0.6554 0.1328 0.7585 0.041 Uiso 1 1 calc R . .
C20 C 0.6809(4) 0.15810(10) 0.6075(4) 0.0298(11) Uani 1 1 d . . .
C21 C 0.6373(4) 0.16316(10) 0.4810(4) 0.0295(11) Uani 1 1 d . . .
C22 C 0.7935(4) 0.17400(10) 0.6610(4) 0.0328(11) Uani 1 1 d . . .
H22A H 0.8015 0.1739 0.7525 0.039 Uiso 1 1 calc R . .
H22B H 0.7943 0.1967 0.6327 0.039 Uiso 1 1 calc R . .
C23 C 0.8934(4) 0.15556(10) 0.6188(4) 0.0294(11) Uani 1 1 d . . .
C24 C 0.9070(4) 0.12353(10) 0.6560(4) 0.0329(11) Uani 1 1 d . . .
H24 H 0.8607 0.1158 0.7145 0.040 Uiso 1 1 calc R . .
C25 C 0.9830(4) 0.10222(10) 0.6136(4) 0.0326(11) Uani 1 1 d . . .
C26 C 1.0493(4) 0.11464(10) 0.5286(4) 0.0326(11) Uani 1 1 d . . .
H26 H 1.1025 0.1007 0.4968 0.039 Uiso 1 1 calc R . .
C27 C 1.0416(4) 0.14625(10) 0.4884(4) 0.0320(11) Uani 1 1 d . . .
C28 C 0.9643(4) 0.16759(10) 0.5345(4) 0.0288(11) Uani 1 1 d . . .
O29 O 0.9037(2) 0.16261(7) 0.2048(3) 0.0343(8) Uani 1 1 d . . .
H29 H 0.9317 0.1748 0.2631 0.051 Uiso 1 1 calc R . .
O30 O 0.6976(2) 0.18508(7) 0.4230(3) 0.0365(8) Uani 1 1 d . . .
H30 H 0.6678 0.1867 0.3485 0.055 Uiso 1 1 calc R . .
C31 C 0.6480(4) 0.16845(10) 0.0938(4) 0.0302(11) Uani 1 1 d . . .
C32 C 0.6241(4) 0.18058(11) -0.0242(4) 0.0342(11) Uani 1 1 d . . .
H32 H 0.6077 0.1686 -0.0988 0.041 Uiso 1 1 calc R . .
N33 N 0.6285(3) 0.21271(9) -0.0124(3) 0.0369(10) Uani 1 1 d . . .
N34 N 0.6530(3) 0.22150(9) 0.1081(3) 0.0392(10) Uani 1 1 d . . .
N35 N 0.6647(3) 0.19447(9) 0.1715(3) 0.0353(10) Uani 1 1 d . . .
C36 C 0.6024(4) 0.23751(11) -0.1096(4) 0.0428(13) Uani 1 1 d . . .
H36A H 0.6635 0.2376 -0.1637 0.051 Uiso 1 1 calc R . .
H36B H 0.6003 0.2591 -0.0712 0.051 Uiso 1 1 calc R . .
C37 C 0.4860(4) 0.23015(11) -0.1860(4) 0.0404(13) Uani 1 1 d . . .
C38 C 0.3833(5) 0.23514(12) -0.1380(5) 0.0503(14) Uani 1 1 d . . .
H38 H 0.3843 0.2451 -0.0595 0.060 Uiso 1 1 calc R . .
C39 C 0.2789(5) 0.22541(14) -0.2063(6) 0.0623(16) Uani 1 1 d . . .
H39 H 0.2086 0.2288 -0.1742 0.075 Uiso 1 1 calc R . .
C40 C 0.2770(5) 0.21074(13) -0.3208(6) 0.0608(17) Uani 1 1 d . . .
H40 H 0.2058 0.2038 -0.3663 0.073 Uiso 1 1 calc R . .
C41 C 0.3780(5) 0.20633(13) -0.3676(5) 0.0587(16) Uani 1 1 d . . .
H41 H 0.3766 0.1967 -0.4467 0.070 Uiso 1 1 calc R . .
C42 C 0.4818(5) 0.21573(11) -0.3013(5) 0.0488(14) Uani 1 1 d . . .
H42 H 0.5514 0.2123 -0.3349 0.059 Uiso 1 1 calc R . .
C43 C 0.9553(3) 0.20180(10) 0.4950(4) 0.0280(11) Uani 1 1 d . . .
C44 C 0.9513(4) 0.22963(10) 0.5619(4) 0.0334(11) Uani 1 1 d . . .
H44 H 0.9551 0.2315 0.6491 0.040 Uiso 1 1 calc R . .
N45 N 0.9476(3) 0.21059(8) 0.3737(3) 0.0328(9) Uani 1 1 d . . .
N46 N 0.9389(3) 0.24228(9) 0.3633(3) 0.0351(9) Uani 1 1 d . . .
N47 N 0.9411(3) 0.25379(8) 0.4783(3) 0.0322(9) Uani 1 1 d . . .
C48 C 0.9379(4) 0.28843(10) 0.4989(4) 0.0392(12) Uani 1 1 d . . .
H48A H 0.9050 0.2926 0.5761 0.047 Uiso 1 1 calc R . .
H48B H 0.8863 0.2986 0.4298 0.047 Uiso 1 1 calc R . .
C49 C 1.0557(4) 0.30380(10) 0.5091(4) 0.0347(12) Uani 1 1 d . . .
C50 C 1.1470(4) 0.29339(11) 0.5967(4) 0.0424(13) Uani 1 1 d . . .
H50 H 1.1354 0.2759 0.6500 0.051 Uiso 1 1 calc R . .
C51 C 1.2525(4) 0.30793(11) 0.6069(4) 0.0431(13) Uani 1 1 d . . .
H51 H 1.3138 0.3001 0.6661 0.052 Uiso 1 1 calc R . .
C52 C 1.2723(4) 0.33386(12) 0.5330(5) 0.0471(13) Uani 1 1 d . . .
H52 H 1.3459 0.3440 0.5413 0.057 Uiso 1 1 calc R . .
C53 C 1.1822(4) 0.34455(11) 0.4465(5) 0.0458(13) Uani 1 1 d . . .
H53 H 1.1940 0.3623 0.3948 0.055 Uiso 1 1 calc R . .
C54 C 1.0752(4) 0.32981(11) 0.4342(4) 0.0404(12) Uani 1 1 d . . .
H54 H 1.0144 0.3375 0.3741 0.048 Uiso 1 1 calc R . .
C55 C 1.1836(4) 0.05188(11) 0.1564(4) 0.0375(12) Uani 1 1 d . . .
C56 C 1.2347(5) 0.03881(12) 0.2855(4) 0.0540(15) Uani 1 1 d . . .
H56A H 1.2884 0.0547 0.3281 0.081 Uiso 1 1 calc R . .
H56B H 1.2761 0.0186 0.2760 0.081 Uiso 1 1 calc R . .
H56C H 1.1720 0.0348 0.3343 0.081 Uiso 1 1 calc R . .
C57 C 1.1129(4) 0.02425(11) 0.0900(4) 0.0453(13) Uani 1 1 d . . .
H57A H 1.0486 0.0189 0.1348 0.068 Uiso 1 1 calc R . .
H57B H 1.1626 0.0053 0.0871 0.068 Uiso 1 1 calc R . .
H57C H 1.0824 0.0309 0.0055 0.068 Uiso 1 1 calc R . .
C58 C 1.2831(4) 0.06071(12) 0.0847(4) 0.0491(14) Uani 1 1 d . . .
H58A H 1.2513 0.0686 0.0021 0.074 Uiso 1 1 calc R . .
H58B H 1.3308 0.0416 0.0769 0.074 Uiso 1 1 calc R . .
H58C H 1.3307 0.0777 0.1293 0.074 Uiso 1 1 calc R . .
C59 C 0.6488(4) 0.03287(10) 0.2453(4) 0.0383(12) Uani 1 1 d . . .
C60 C 0.5692(5) 0.02543(12) 0.3414(5) 0.0647(17) Uani 1 1 d . . .
H60A H 0.5953 0.0375 0.4175 0.097 Uiso 1 1 calc R . .
H60B H 0.5714 0.0022 0.3594 0.097 Uiso 1 1 calc R . .
H60C H 0.4899 0.0318 0.3088 0.097 Uiso 1 1 calc R . .
C61 C 0.7713(5) 0.02301(13) 0.2996(6) 0.079(2) Uani 1 1 d . . .
H61A H 0.7967 0.0358 0.3742 0.118 Uiso 1 1 calc R . .
H61B H 0.8235 0.0269 0.2385 0.118 Uiso 1 1 calc R . .
H61C H 0.7725 0.0000 0.3210 0.118 Uiso 1 1 calc R . .
C62 C 0.6111(6) 0.01254(12) 0.1321(5) 0.0691(18) Uani 1 1 d . . .
H62A H 0.6167 -0.0104 0.1546 0.104 Uiso 1 1 calc R . .
H62B H 0.6613 0.0170 0.0695 0.104 Uiso 1 1 calc R . .
H62C H 0.5309 0.0178 0.0985 0.104 Uiso 1 1 calc R . .
C63 C 0.9947(4) 0.06711(11) 0.6569(4) 0.0388(12) Uani 1 1 d . . .
C64 C 0.8808(5) 0.05455(12) 0.6898(6) 0.0695(18) Uani 1 1 d . . .
H64A H 0.8197 0.0576 0.6193 0.104 Uiso 1 1 calc R . .
H64B H 0.8610 0.0664 0.7615 0.104 Uiso 1 1 calc R . .
H64C H 0.8882 0.0315 0.7098 0.104 Uiso 1 1 calc R . .
C65 C 1.0862(5) 0.06579(13) 0.7726(4) 0.0591(16) Uani 1 1 d . . .
H65A H 1.0980 0.0433 0.7997 0.089 Uiso 1 1 calc R . .
H65B H 1.0599 0.0785 0.8389 0.089 Uiso 1 1 calc R . .
H65C H 1.1592 0.0747 0.7531 0.089 Uiso 1 1 calc R . .
C66 C 1.0336(4) 0.04520(11) 0.5585(4) 0.0485(14) Uani 1 1 d . . .
H66A H 1.0344 0.0227 0.5868 0.073 Uiso 1 1 calc R . .
H66B H 1.1115 0.0514 0.5443 0.073 Uiso 1 1 calc R . .
H66C H 0.9799 0.0473 0.4813 0.073 Uiso 1 1 calc R . .
C67 C 0.4694(4) 0.09512(12) 0.7032(4) 0.0449(13) Uani 1 1 d . . .
C68 C 0.3781(4) 0.07484(12) 0.6255(5) 0.0522(14) Uani 1 1 d . . .
H68A H 0.3463 0.0591 0.6787 0.078 Uiso 1 1 calc R . .
H68B H 0.4132 0.0634 0.5617 0.078 Uiso 1 1 calc R . .
H68C H 0.3160 0.0889 0.5861 0.078 Uiso 1 1 calc R . .
C69 C 0.4196(6) 0.11303(15) 0.8029(6) 0.091(3) Uani 1 1 d . . .
H69A H 0.3599 0.1280 0.7650 0.137 Uiso 1 1 calc R . .
H69B H 0.4811 0.1252 0.8536 0.137 Uiso 1 1 calc R . .
H69C H 0.3853 0.0976 0.8552 0.137 Uiso 1 1 calc R . .
C70 C 0.5622(5) 0.07087(15) 0.7660(6) 0.082(2) Uani 1 1 d . . .
H70A H 0.5250 0.0550 0.8139 0.124 Uiso 1 1 calc R . .
H70B H 0.6213 0.0827 0.8213 0.124 Uiso 1 1 calc R . .
H70C H 0.5984 0.0598 0.7023 0.124 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.030(3) 0.042(3) 0.025(3) 0.003(2) 0.001(2) -0.003(2)
C2 0.034(3) 0.036(3) 0.019(3) 0.001(2) 0.000(2) -0.004(2)
C3 0.031(3) 0.046(3) 0.025(3) -0.001(2) -0.002(2) 0.001(2)
C4 0.041(3) 0.041(3) 0.018(3) 0.002(2) 0.006(2) 0.000(2)
C5 0.044(3) 0.041(3) 0.014(3) 0.000(2) 0.001(2) -0.007(2)
C6 0.038(3) 0.037(3) 0.017(3) 0.003(2) 0.001(2) 0.001(2)
C7 0.037(3) 0.038(3) 0.019(3) 0.004(2) 0.006(2) 0.002(2)
C8 0.038(3) 0.040(3) 0.012(2) -0.003(2) 0.003(2) 0.003(2)
C9 0.035(3) 0.041(3) 0.011(2) -0.001(2) -0.010(2) 0.003(2)
C10 0.032(3) 0.039(3) 0.021(3) -0.006(2) -0.005(2) 0.002(2)
C11 0.028(3) 0.046(3) 0.024(3) -0.001(2) -0.006(2) -0.004(2)
C12 0.032(3) 0.047(3) 0.017(3) -0.002(2) -0.004(2) -0.003(2)
C13 0.031(3) 0.035(3) 0.019(3) -0.007(2) -0.008(2) 0.003(2)
C14 0.032(3) 0.040(3) 0.015(3) -0.001(2) -0.006(2) -0.001(2)
C15 0.031(3) 0.044(3) 0.023(3) -0.002(2) -0.004(2) -0.001(2)
C16 0.035(3) 0.035(3) 0.018(3) -0.007(2) -0.003(2) 0.002(2)
C17 0.031(3) 0.042(3) 0.026(3) -0.004(2) 0.002(2) -0.006(2)
C18 0.035(3) 0.047(3) 0.024(3) -0.002(2) 0.008(2) -0.003(2)
C19 0.036(3) 0.046(3) 0.019(3) -0.005(2) -0.002(2) -0.002(2)
C20 0.033(3) 0.035(3) 0.020(3) 0.000(2) 0.001(2) -0.001(2)
C21 0.033(3) 0.033(2) 0.022(3) 0.003(2) 0.005(2) 0.000(2)
C22 0.041(3) 0.037(3) 0.019(3) -0.001(2) -0.001(2) 0.001(2)
C23 0.033(3) 0.037(3) 0.015(3) -0.002(2) -0.006(2) -0.003(2)
C24 0.037(3) 0.044(3) 0.016(3) 0.001(2) -0.005(2) -0.006(2)
C25 0.031(3) 0.041(3) 0.023(3) -0.001(2) -0.004(2) 0.001(2)
C26 0.033(3) 0.039(3) 0.025(3) -0.001(2) 0.000(2) 0.001(2)
C27 0.036(3) 0.038(3) 0.019(3) 0.001(2) -0.008(2) -0.003(2)
C28 0.033(3) 0.036(3) 0.014(3) -0.001(2) -0.006(2) -0.004(2)
O29 0.0389(18) 0.0399(18) 0.0215(18) -0.0069(14) -0.0040(14) 0.0018(14)
O30 0.0402(19) 0.0443(18) 0.0218(18) 0.0034(15) -0.0068(14) -0.0041(15)
C31 0.029(3) 0.038(3) 0.022(3) -0.001(2) -0.004(2) -0.001(2)
C32 0.042(3) 0.039(3) 0.019(3) -0.004(2) -0.005(2) 0.000(2)
N33 0.044(2) 0.041(2) 0.022(2) 0.0046(19) -0.0090(18) -0.0030(18)
N34 0.043(2) 0.044(2) 0.028(3) 0.002(2) -0.0045(18) 0.0022(18)
N35 0.038(2) 0.036(2) 0.029(2) 0.001(2) -0.0029(18) 0.0034(17)
C36 0.050(3) 0.039(3) 0.036(3) 0.009(2) -0.007(2) 0.001(2)
C37 0.056(4) 0.035(3) 0.026(3) 0.006(2) -0.008(2) 0.001(2)
C38 0.059(4) 0.067(4) 0.027(3) 0.007(3) 0.012(3) 0.005(3)
C39 0.048(4) 0.082(4) 0.054(4) 0.027(4) 0.001(3) 0.008(3)
C40 0.059(4) 0.067(4) 0.049(4) 0.013(3) -0.019(3) -0.012(3)
C41 0.065(4) 0.059(4) 0.047(4) -0.002(3) -0.011(3) 0.005(3)
C42 0.054(4) 0.051(3) 0.038(3) 0.005(3) -0.006(3) 0.004(3)
C43 0.027(3) 0.040(3) 0.015(3) -0.006(2) -0.0010(19) -0.0002(19)
C44 0.035(3) 0.041(3) 0.022(3) 0.000(2) -0.003(2) -0.002(2)
N45 0.041(2) 0.039(2) 0.017(2) 0.0004(18) -0.0031(17) -0.0005(17)
N46 0.048(2) 0.037(2) 0.018(2) -0.0013(19) -0.0026(17) -0.0011(18)
N47 0.035(2) 0.037(2) 0.022(2) -0.004(2) -0.0022(16) -0.0019(17)
C48 0.047(3) 0.034(3) 0.033(3) -0.001(2) -0.006(2) 0.001(2)
C49 0.044(3) 0.033(3) 0.025(3) -0.007(2) 0.000(2) 0.001(2)
C50 0.057(3) 0.041(3) 0.026(3) 0.001(2) -0.003(2) -0.007(2)
C51 0.046(3) 0.050(3) 0.029(3) 0.001(2) -0.009(2) -0.008(2)
C52 0.049(3) 0.052(3) 0.038(3) -0.007(3) -0.003(3) -0.012(3)
C53 0.057(4) 0.044(3) 0.039(3) 0.004(2) 0.015(3) -0.007(3)
C54 0.043(3) 0.043(3) 0.033(3) 0.004(2) 0.003(2) 0.002(2)
C55 0.040(3) 0.046(3) 0.025(3) -0.003(2) 0.002(2) 0.004(2)
C56 0.070(4) 0.056(3) 0.032(3) -0.006(3) -0.008(3) 0.018(3)
C57 0.049(3) 0.046(3) 0.040(3) -0.004(2) 0.001(2) 0.001(2)
C58 0.041(3) 0.066(3) 0.040(3) -0.006(3) 0.006(3) 0.006(3)
C59 0.038(3) 0.037(3) 0.037(3) 0.001(2) -0.001(2) -0.002(2)
C60 0.080(4) 0.047(3) 0.073(4) 0.009(3) 0.031(3) 0.001(3)
C61 0.058(4) 0.062(4) 0.110(5) 0.036(4) -0.008(4) 0.005(3)
C62 0.102(5) 0.046(3) 0.058(4) -0.005(3) 0.006(3) -0.009(3)
C63 0.045(3) 0.044(3) 0.029(3) 0.005(2) 0.010(2) 0.002(2)
C64 0.073(4) 0.047(3) 0.094(5) 0.023(3) 0.031(4) 0.008(3)
C65 0.088(4) 0.063(4) 0.025(3) 0.014(3) 0.002(3) 0.014(3)
C66 0.063(4) 0.044(3) 0.037(3) 0.004(2) 0.001(3) 0.005(2)
C67 0.046(3) 0.059(3) 0.029(3) -0.001(3) 0.003(2) -0.013(3)
C68 0.054(3) 0.062(3) 0.039(3) 0.004(3) 0.003(3) -0.013(3)
C69 0.135(6) 0.085(5) 0.073(5) -0.038(4) 0.079(5) -0.057(4)
C70 0.069(4) 0.096(5) 0.074(5) 0.042(4) -0.017(3) -0.033(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(6) . ?
C1 C27 1.543(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.389(6) . ?
C2 C7 1.404(6) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(6) . ?
C4 C55 1.527(6) . ?
C5 C6 1.377(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(6) . ?
C6 C8 1.519(6) . ?
C7 O29 1.363(5) . ?
C8 C9 1.528(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.385(6) . ?
C9 C14 1.404(6) . ?
C10 C11 1.406(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(6) . ?
C11 C59 1.530(6) . ?
C12 C13 1.393(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.413(6) . ?
C13 C15 1.531(6) . ?
C14 C31 1.486(6) . ?
C15 C16 1.517(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C21 1.393(6) . ?
C16 C17 1.396(6) . ?
C17 C18 1.400(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(6) . ?
C18 C67 1.537(6) . ?
C19 C20 1.378(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.417(6) . ?
C20 C22 1.511(6) . ?
C21 O30 1.360(5) . ?
C22 C23 1.521(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.390(6) . ?
C23 C28 1.415(6) . ?
C24 C25 1.378(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(6) . ?
C25 C63 1.529(6) . ?
C26 C27 1.380(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.407(6) . ?
C28 C43 1.480(6) . ?
O29 H29 0.8400 . ?
O30 H30 0.8400 . ?
C31 N35 1.368(5) . ?
C31 C32 1.374(6) . ?
C32 N33 1.337(5) . ?
C32 H32 0.9500 . ?
N33 N34 1.356(5) . ?
N33 C36 1.477(5) . ?
N34 N35 1.313(5) . ?
C36 C37 1.521(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C42 1.388(7) . ?
C37 C38 1.392(7) . ?
C38 C39 1.394(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.364(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.376(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 N45 1.364(5) . ?
C43 C44 1.369(6) . ?
C44 N47 1.349(5) . ?
C44 H44 0.9500 . ?
N45 N46 1.320(5) . ?
N46 N47 1.340(5) . ?
N47 C48 1.454(5) . ?
C48 C49 1.506(6) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C54 1.391(6) . ?
C49 C50 1.395(6) . ?
C50 C51 1.363(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.383(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.382(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.380(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C57 1.532(6) . ?
C55 C58 1.537(7) . ?
C55 C56 1.548(6) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C62 1.508(7) . ?
C59 C61 1.525(7) . ?
C59 C60 1.530(7) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.519(7) . ?
C63 C66 1.525(6) . ?
C63 C65 1.534(6) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C69 1.503(7) . ?
C67 C68 1.517(6) . ?
C67 C70 1.562(7) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C27 109.0(3) . . ?
C2 C1 H1A 109.9 . . ?
C27 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
C27 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C3 C2 C7 117.6(4) . . ?
C3 C2 C1 120.4(4) . . ?
C7 C2 C1 121.6(4) . . ?
C2 C3 C4 123.7(4) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C3 C4 C5 115.7(4) . . ?
C3 C4 C55 121.4(4) . . ?
C5 C4 C55 122.9(4) . . ?
C6 C5 C4 123.4(4) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C5 C6 C7 118.7(4) . . ?
C5 C6 C8 123.0(4) . . ?
C7 C6 C8 118.1(4) . . ?
O29 C7 C6 115.4(4) . . ?
O29 C7 C2 123.8(4) . . ?
C6 C7 C2 120.8(4) . . ?
C6 C8 C9 109.4(3) . . ?
C6 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
C6 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C10 C9 C14 119.5(4) . . ?
C10 C9 C8 116.4(4) . . ?
C14 C9 C8 123.9(4) . . ?
C9 C10 C11 123.0(4) . . ?
C9 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C12 C11 C10 116.1(4) . . ?
C12 C11 C59 124.7(4) . . ?
C10 C11 C59 119.2(4) . . ?
C11 C12 C13 123.3(4) . . ?
C11 C12 H12 118.3 . . ?
C13 C12 H12 118.3 . . ?
C12 C13 C14 119.1(4) . . ?
C12 C13 C15 116.4(4) . . ?
C14 C13 C15 124.5(4) . . ?
C9 C14 C13 118.9(4) . . ?
C9 C14 C31 121.1(4) . . ?
C13 C14 C31 120.0(4) . . ?
C16 C15 C13 110.1(3) . . ?
C16 C15 H15A 109.6 . . ?
C13 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C13 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
C21 C16 C17 118.5(4) . . ?
C21 C16 C15 121.6(4) . . ?
C17 C16 C15 119.4(4) . . ?
C16 C17 C18 123.2(4) . . ?
C16 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C19 C18 C17 116.1(4) . . ?
C19 C18 C67 120.8(4) . . ?
C17 C18 C67 123.1(4) . . ?
C20 C19 C18 123.5(4) . . ?
C20 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
C19 C20 C21 118.6(4) . . ?
C19 C20 C22 122.1(4) . . ?
C21 C20 C22 118.9(4) . . ?
O30 C21 C16 125.4(4) . . ?
O30 C21 C20 114.5(4) . . ?
C16 C21 C20 120.1(4) . . ?
C20 C22 C23 109.1(3) . . ?
C20 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
C20 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C24 C23 C28 118.3(4) . . ?
C24 C23 C22 116.8(4) . . ?
C28 C23 C22 124.6(4) . . ?
C25 C24 C23 124.4(4) . . ?
C25 C24 H24 117.8 . . ?
C23 C24 H24 117.8 . . ?
C24 C25 C26 115.8(4) . . ?
C24 C25 C63 122.6(4) . . ?
C26 C25 C63 121.6(4) . . ?
C27 C26 C25 123.1(4) . . ?
C27 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C26 C27 C28 119.9(4) . . ?
C26 C27 C1 115.0(4) . . ?
C28 C27 C1 125.0(4) . . ?
C27 C28 C23 118.5(4) . . ?
C27 C28 C43 121.3(4) . . ?
C23 C28 C43 120.2(4) . . ?
C7 O29 H29 109.5 . . ?
C21 O30 H30 109.5 . . ?
N35 C31 C32 106.5(4) . . ?
N35 C31 C14 123.7(4) . . ?
C32 C31 C14 129.7(4) . . ?
N33 C32 C31 105.9(4) . . ?
N33 C32 H32 127.0 . . ?
C31 C32 H32 127.0 . . ?
C32 N33 N34 111.1(3) . . ?
C32 N33 C36 128.5(4) . . ?
N34 N33 C36 120.2(4) . . ?
N35 N34 N33 105.9(3) . . ?
N34 N35 C31 110.5(3) . . ?
N33 C36 C37 109.3(4) . . ?
N33 C36 H36A 109.8 . . ?
C37 C36 H36A 109.8 . . ?
N33 C36 H36B 109.8 . . ?
C37 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
C42 C37 C38 119.1(5) . . ?
C42 C37 C36 119.7(5) . . ?
C38 C37 C36 121.0(5) . . ?
C39 C38 C37 119.4(5) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C40 C39 C38 120.5(6) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C41 C40 C39 119.6(5) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C40 C41 C42 120.6(6) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C41 C42 C37 120.8(5) . . ?
C41 C42 H42 119.6 . . ?
C37 C42 H42 119.6 . . ?
N45 C43 C44 106.9(4) . . ?
N45 C43 C28 122.0(4) . . ?
C44 C43 C28 131.1(4) . . ?
N47 C44 C43 105.7(4) . . ?
N47 C44 H44 127.2 . . ?
C43 C44 H44 127.2 . . ?
N46 N45 C43 110.0(3) . . ?
N45 N46 N47 106.4(3) . . ?
N46 N47 C44 111.0(3) . . ?
N46 N47 C48 120.0(4) . . ?
C44 N47 C48 129.0(4) . . ?
N47 C48 C49 112.6(4) . . ?
N47 C48 H48A 109.1 . . ?
C49 C48 H48A 109.1 . . ?
N47 C48 H48B 109.1 . . ?
C49 C48 H48B 109.1 . . ?
H48A C48 H48B 107.8 . . ?
C54 C49 C50 117.9(4) . . ?
C54 C49 C48 120.7(4) . . ?
C50 C49 C48 121.4(4) . . ?
C51 C50 C49 120.9(4) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C52 121.4(4) . . ?
C50 C51 H51 119.3 . . ?
C52 C51 H51 119.3 . . ?
C51 C52 C53 118.2(5) . . ?
C51 C52 H52 120.9 . . ?
C53 C52 H52 120.9 . . ?
C54 C53 C52 121.0(5) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C53 C54 C49 120.6(4) . . ?
C53 C54 H54 119.7 . . ?
C49 C54 H54 119.7 . . ?
C4 C55 C57 112.4(4) . . ?
C4 C55 C58 109.1(4) . . ?
C57 C55 C58 109.4(4) . . ?
C4 C55 C56 110.4(4) . . ?
C57 C55 C56 106.3(4) . . ?
C58 C55 C56 109.1(4) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C62 C59 C61 108.4(5) . . ?
C62 C59 C11 109.8(4) . . ?
C61 C59 C11 109.9(4) . . ?
C62 C59 C60 108.4(4) . . ?
C61 C59 C60 108.0(4) . . ?
C11 C59 C60 112.2(4) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 C66 108.9(4) . . ?
C64 C63 C25 110.9(4) . . ?
C66 C63 C25 111.7(4) . . ?
C64 C63 C65 108.9(4) . . ?
C66 C63 C65 108.4(4) . . ?
C25 C63 C65 108.0(4) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C69 C67 C68 111.3(5) . . ?
C69 C67 C18 109.8(4) . . ?
C68 C67 C18 111.9(4) . . ?
C69 C67 C70 108.4(5) . . ?
C68 C67 C70 106.1(4) . . ?
C18 C67 C70 109.2(4) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.923
_diffrn_reflns_theta_full        23.00
_diffrn_measured_fraction_theta_full 0.923
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.053

# Attachment 'ar38sq.cif'

data_ar38sq
_database_code_depnum_ccdc_archive 'CCDC 702764'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cl2 N6 O2 Ti, 1.721(C H Cl3)'
_chemical_formula_sum            'C63.72 H69.72 Cl7.16 N6 O2 Ti'
_chemical_formula_weight         1253.44

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3623(4)
_cell_length_b                   16.3201(4)
_cell_length_c                   19.1318(7)
_cell_angle_alpha                83.9380(19)
_cell_angle_beta                 75.0364(13)
_cell_angle_gamma                71.1954(17)
_cell_volume                     3528.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    8546
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1307.6
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_detector_area_resol_mean 12.8
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31509
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.46
_reflns_number_total             15836
_reflns_number_gt                10522
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Nonius B.V.'
_computing_cell_refinement       Denzo
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The crystal contains molecules of partly disordered chloroform solvent.
It also contains additional crystallization solvent, which could not be
modeled by discrete atoms.
Two of the t-butyl substituents also exhibit rotational disorder.
Distance constraints were used in their crystallographic refinement.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15836
_refine_ls_number_parameters     745
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.2349
_refine_ls_wR_factor_gt          0.2135
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.13589(5) 0.25055(3) 0.91674(3) 0.01997(16) Uani 1 1 d . . .
Cl2 Cl -0.05339(7) 0.33637(5) 0.98442(4) 0.0271(2) Uani 1 1 d . . .
Cl3 Cl 0.17015(7) 0.16658(4) 1.02458(4) 0.02474(19) Uani 1 1 d . . .
O4 O 0.27693(18) 0.18182(12) 0.86742(12) 0.0229(5) Uani 1 1 d . . .
O5 O 0.10301(19) 0.32068(13) 0.83869(12) 0.0248(5) Uani 1 1 d . . .
C6 C -0.0506(3) 0.28224(19) 0.76452(19) 0.0297(8) Uani 1 1 d . . .
H6A H -0.1115 0.2858 0.7384 0.036 Uiso 1 1 calc R . .
H6B H -0.0813 0.2698 0.8163 0.036 Uiso 1 1 calc R . .
C7 C -0.0242(3) 0.36702(19) 0.75642(18) 0.0254(7) Uani 1 1 d . . .
C8 C -0.0703(3) 0.42955(19) 0.70757(18) 0.0273(7) Uani 1 1 d . . .
H8 H -0.1225 0.4188 0.6835 0.033 Uiso 1 1 calc R . .
C9 C -0.0436(3) 0.50714(19) 0.69225(17) 0.0265(7) Uani 1 1 d . . .
C10 C 0.0332(3) 0.51993(19) 0.72935(18) 0.0268(7) Uani 1 1 d . . .
H10 H 0.0535 0.5721 0.7201 0.032 Uiso 1 1 calc R . .
C11 C 0.0811(3) 0.46044(19) 0.77879(17) 0.0253(7) Uani 1 1 d . . .
C12 C 0.0528(3) 0.38255(18) 0.79275(17) 0.0236(7) Uani 1 1 d . . .
C13 C 0.1610(3) 0.48302(19) 0.81674(19) 0.0281(7) Uani 1 1 d . . .
H13A H 0.1316 0.4778 0.8698 0.034 Uiso 1 1 calc R . .
H13B H 0.1596 0.5438 0.8047 0.034 Uiso 1 1 calc R . .
C14 C 0.2871(3) 0.4232(2) 0.79405(19) 0.0292(8) Uani 1 1 d . . .
C15 C 0.3515(4) 0.4225(2) 0.7223(2) 0.0365(9) Uani 1 1 d . . .
H15 H 0.3186 0.4634 0.6883 0.044 Uiso 1 1 calc R . .
C16 C 0.4626(4) 0.3633(2) 0.6992(2) 0.0389(9) Uani 1 1 d . A .
C17 C 0.5043(3) 0.2996(2) 0.7482(2) 0.0358(9) Uani 1 1 d . . .
H17 H 0.5766 0.2554 0.7321 0.043 Uiso 1 1 calc R . .
C18 C 0.4430(3) 0.2985(2) 0.82033(19) 0.0274(7) Uani 1 1 d . . .
C19 C 0.3375(3) 0.36514(19) 0.84418(17) 0.0228(7) Uani 1 1 d . . .
C20 C 0.4847(3) 0.2241(2) 0.8714(2) 0.0305(8) Uani 1 1 d . . .
H20A H 0.5646 0.2203 0.8752 0.037 Uiso 1 1 calc R . .
H20B H 0.4314 0.2350 0.9202 0.037 Uiso 1 1 calc R . .
C21 C 0.4873(3) 0.13932(19) 0.84477(18) 0.0269(7) Uani 1 1 d . . .
C22 C 0.5957(3) 0.0776(2) 0.81852(19) 0.0303(8) Uani 1 1 d . . .
H22 H 0.6653 0.0889 0.8211 0.036 Uiso 1 1 calc R . .
C23 C 0.6064(3) 0.0006(2) 0.78891(19) 0.0287(7) Uani 1 1 d . . .
C24 C 0.5023(3) -0.0143(2) 0.78844(19) 0.0289(8) Uani 1 1 d . . .
H24 H 0.5070 -0.0673 0.7698 0.035 Uiso 1 1 calc R . .
C25 C 0.3914(3) 0.04421(19) 0.81385(18) 0.0245(7) Uani 1 1 d . . .
C26 C 0.3840(3) 0.12202(19) 0.84270(17) 0.0236(7) Uani 1 1 d . . .
C27 C 0.2826(3) 0.02345(19) 0.80863(18) 0.0254(7) Uani 1 1 d . . .
H27A H 0.3052 -0.0366 0.7923 0.030 Uiso 1 1 calc R . .
H27B H 0.2275 0.0279 0.8569 0.030 Uiso 1 1 calc R . .
C28 C 0.2224(3) 0.08573(19) 0.75566(18) 0.0251(7) Uani 1 1 d . . .
C29 C 0.2848(3) 0.0950(2) 0.68448(19) 0.0324(8) Uani 1 1 d . . .
H29 H 0.3618 0.0566 0.6679 0.039 Uiso 1 1 calc R . .
C30 C 0.2370(4) 0.1589(2) 0.63766(19) 0.0371(9) Uani 1 1 d . B .
C31 C 0.1271(3) 0.2170(2) 0.66377(19) 0.0354(9) Uani 1 1 d . . .
H31 H 0.0957 0.2632 0.6330 0.042 Uiso 1 1 calc R . .
C32 C 0.0612(3) 0.2098(2) 0.73395(18) 0.0277(7) Uani 1 1 d . . .
C33 C 0.1074(3) 0.14025(18) 0.77789(17) 0.0230(7) Uani 1 1 d . . .
N34 N 0.2031(2) 0.33610(15) 0.95937(14) 0.0218(6) Uani 1 1 d . . .
N35 N 0.1651(2) 0.36082(16) 1.02704(14) 0.0241(6) Uani 1 1 d . . .
N36 N 0.2187(2) 0.41719(15) 1.03286(14) 0.0231(6) Uani 1 1 d . . .
C37 C 0.2917(3) 0.42969(19) 0.96917(17) 0.0240(7) Uani 1 1 d . . .
H37 H 0.3394 0.4669 0.9594 0.029 Uiso 1 1 calc R . .
C38 C 0.2813(3) 0.37686(18) 0.92230(17) 0.0227(7) Uani 1 1 d . . .
C39 C 0.1832(3) 0.46341(19) 1.10126(18) 0.0250(7) Uani 1 1 d . . .
H39A H 0.1464 0.4292 1.1404 0.030 Uiso 1 1 calc R . .
H39B H 0.1231 0.5197 1.0966 0.030 Uiso 1 1 calc R . .
C40 C 0.2831(3) 0.4795(2) 1.12234(17) 0.0246(7) Uani 1 1 d . . .
C41 C 0.3508(3) 0.4185(2) 1.16331(19) 0.0308(8) Uani 1 1 d . . .
H41 H 0.3362 0.3646 1.1760 0.037 Uiso 1 1 calc R . .
C42 C 0.4388(3) 0.4357(3) 1.1857(2) 0.0403(9) Uani 1 1 d . . .
H42 H 0.4844 0.3936 1.2135 0.048 Uiso 1 1 calc R . .
C43 C 0.4606(3) 0.5142(3) 1.1676(2) 0.0382(9) Uani 1 1 d . . .
H43 H 0.5197 0.5266 1.1842 0.046 Uiso 1 1 calc R . .
C44 C 0.3967(3) 0.5744(2) 1.1255(2) 0.0391(9) Uani 1 1 d . . .
H44 H 0.4138 0.6273 1.1114 0.047 Uiso 1 1 calc R . .
C45 C 0.3077(3) 0.5576(2) 1.1037(2) 0.0317(8) Uani 1 1 d . . .
H45 H 0.2628 0.5998 1.0756 0.038 Uiso 1 1 calc R . .
N46 N 0.0381(2) 0.16275(15) 0.91111(14) 0.0222(6) Uani 1 1 d . . .
N47 N -0.0326(2) 0.13877(15) 0.96906(15) 0.0244(6) Uani 1 1 d . . .
N48 N -0.0803(2) 0.08913(15) 0.94451(15) 0.0243(6) Uani 1 1 d . . .
C49 C -0.0421(3) 0.08028(19) 0.87264(18) 0.0251(7) Uani 1 1 d . . .
H49 H -0.0642 0.0482 0.8431 0.030 Uiso 1 1 calc R . .
C50 C 0.0353(3) 0.12689(18) 0.85064(18) 0.0237(7) Uani 1 1 d . . .
C51 C -0.1640(3) 0.05217(19) 0.99618(19) 0.0273(7) Uani 1 1 d . . .
H51A H -0.1396 0.0391 1.0425 0.033 Uiso 1 1 calc R . .
H51B H -0.1600 -0.0032 0.9773 0.033 Uiso 1 1 calc R . .
C52 C -0.2886(3) 0.10970(19) 1.01049(18) 0.0259(7) Uani 1 1 d . . .
C53 C -0.3789(3) 0.0734(2) 1.01902(19) 0.0300(8) Uani 1 1 d . . .
H53 H -0.3605 0.0135 1.0110 0.036 Uiso 1 1 calc R . .
C54 C -0.4963(3) 0.1244(2) 1.0393(2) 0.0358(8) Uani 1 1 d . . .
H54 H -0.5575 0.0993 1.0450 0.043 Uiso 1 1 calc R . .
C55 C -0.5230(3) 0.2111(2) 1.0508(2) 0.0381(9) Uani 1 1 d . . .
H55 H -0.6030 0.2455 1.0651 0.046 Uiso 1 1 calc R . .
C56 C -0.4346(3) 0.2489(2) 1.0417(2) 0.0362(9) Uani 1 1 d . . .
H56 H -0.4538 0.3091 1.0490 0.043 Uiso 1 1 calc R . .
C57 C -0.3180(3) 0.1984(2) 1.02180(19) 0.0311(8) Uani 1 1 d . . .
H57 H -0.2573 0.2243 1.0158 0.037 Uiso 1 1 calc R . .
C58 C -0.0879(3) 0.57314(19) 0.63498(18) 0.0301(8) Uani 1 1 d . . .
C59 C -0.1371(4) 0.6650(2) 0.6659(2) 0.0383(9) Uani 1 1 d . . .
H59A H -0.2012 0.6667 0.7090 0.057 Uiso 1 1 calc R . .
H59B H -0.1669 0.7067 0.6294 0.057 Uiso 1 1 calc R . .
H59C H -0.0744 0.6799 0.6792 0.057 Uiso 1 1 calc R . .
C60 C -0.1848(4) 0.5540(2) 0.6096(2) 0.0397(9) Uani 1 1 d . . .
H60A H -0.1513 0.5006 0.5821 0.060 Uiso 1 1 calc R . .
H60B H -0.2188 0.6021 0.5787 0.060 Uiso 1 1 calc R . .
H60C H -0.2463 0.5471 0.6517 0.060 Uiso 1 1 calc R . .
C61 C 0.0163(4) 0.5704(2) 0.5702(2) 0.0393(9) Uani 1 1 d . . .
H61A H 0.0765 0.5861 0.5857 0.059 Uiso 1 1 calc R . .
H61B H -0.0107 0.6115 0.5324 0.059 Uiso 1 1 calc R . .
H61C H 0.0498 0.5118 0.5510 0.059 Uiso 1 1 calc R . .
C62 C 0.5389(3) 0.3739(2) 0.62159(18) 0.0626(14) Uani 1 1 d D . .
C63A C 0.6424(6) 0.2940(4) 0.5940(4) 0.061(3) Uiso 0.664(11) 1 d PD A 1
H63A H 0.6132 0.2450 0.5934 0.091 Uiso 0.664(11) 1 calc PR A 1
H63B H 0.6967 0.2797 0.6260 0.091 Uiso 0.664(11) 1 calc PR A 1
H63C H 0.6838 0.3059 0.5449 0.091 Uiso 0.664(11) 1 calc PR A 1
C64A C 0.4611(5) 0.4005(4) 0.5673(3) 0.051(2) Uiso 0.664(11) 1 d PD A 1
H64A H 0.3991 0.4550 0.5819 0.077 Uiso 0.664(11) 1 calc PR A 1
H64B H 0.4253 0.3553 0.5660 0.077 Uiso 0.664(11) 1 calc PR A 1
H64C H 0.5091 0.4082 0.5190 0.077 Uiso 0.664(11) 1 calc PR A 1
C65A C 0.5867(8) 0.4482(4) 0.6268(5) 0.062(3) Uiso 0.664(11) 1 d PD A 1
H65A H 0.6285 0.4626 0.5785 0.093 Uiso 0.664(11) 1 calc PR A 1
H65B H 0.6409 0.4306 0.6589 0.093 Uiso 0.664(11) 1 calc PR A 1
H65C H 0.5211 0.4991 0.6463 0.093 Uiso 0.664(11) 1 calc PR A 1
C63B C 0.5800(12) 0.2820(4) 0.5930(7) 0.064(5) Uiso 0.336(11) 1 d PD A 2
H63D H 0.5125 0.2601 0.6016 0.097 Uiso 0.336(11) 1 calc PR A 2
H63E H 0.6383 0.2442 0.6181 0.097 Uiso 0.336(11) 1 calc PR A 2
H63F H 0.6156 0.2829 0.5409 0.097 Uiso 0.336(11) 1 calc PR A 2
C64B C 0.4858(13) 0.4375(7) 0.5658(7) 0.064(8) Uiso 0.336(11) 1 d PD A 2
H64D H 0.4561 0.4963 0.5845 0.096 Uiso 0.336(11) 1 calc PR A 2
H64E H 0.4210 0.4217 0.5563 0.096 Uiso 0.336(11) 1 calc PR A 2
H64F H 0.5464 0.4354 0.5207 0.096 Uiso 0.336(11) 1 calc PR A 2
C65B C 0.6454(8) 0.3953(9) 0.6320(7) 0.068(5) Uiso 0.336(11) 1 d PD A 2
H65D H 0.7117 0.3758 0.5902 0.103 Uiso 0.336(11) 1 calc PR A 2
H65E H 0.6671 0.3658 0.6760 0.103 Uiso 0.336(11) 1 calc PR A 2
H65F H 0.6256 0.4580 0.6365 0.103 Uiso 0.336(11) 1 calc PR A 2
C66 C 0.7251(3) -0.0658(2) 0.7575(2) 0.0351(8) Uani 1 1 d . . .
C67 C 0.8273(3) -0.0416(3) 0.7718(3) 0.0499(11) Uani 1 1 d . . .
H67A H 0.8290 0.0145 0.7482 0.075 Uiso 1 1 calc R . .
H67B H 0.9017 -0.0860 0.7523 0.075 Uiso 1 1 calc R . .
H67C H 0.8167 -0.0377 0.8240 0.075 Uiso 1 1 calc R . .
C68 C 0.7300(3) -0.1554(2) 0.7919(2) 0.0410(9) Uani 1 1 d . . .
H68A H 0.7264 -0.1543 0.8436 0.061 Uiso 1 1 calc R . .
H68B H 0.8036 -0.1979 0.7683 0.061 Uiso 1 1 calc R . .
H68C H 0.6632 -0.1715 0.7859 0.061 Uiso 1 1 calc R . .
C69 C 0.7390(4) -0.0692(3) 0.6747(2) 0.0485(11) Uani 1 1 d . . .
H69A H 0.6747 -0.0864 0.6660 0.073 Uiso 1 1 calc R . .
H69B H 0.8144 -0.1116 0.6535 0.073 Uiso 1 1 calc R . .
H69C H 0.7368 -0.0120 0.6525 0.073 Uiso 1 1 calc R . .
C70 C 0.3129(3) 0.1641(2) 0.56012(18) 0.0584(13) Uani 1 1 d D . .
C71A C 0.2620(6) 0.2460(3) 0.5176(4) 0.056(2) Uiso 0.591(8) 1 d PD B 1
H71A H 0.2577 0.2971 0.5422 0.084 Uiso 0.591(8) 1 calc PR B 1
H71B H 0.1829 0.2490 0.5145 0.084 Uiso 0.591(8) 1 calc PR B 1
H71C H 0.3127 0.2446 0.4687 0.084 Uiso 0.591(8) 1 calc PR B 1
C72A C 0.4353(4) 0.1617(4) 0.5660(4) 0.062(2) Uiso 0.591(8) 1 d PD B 1
H72A H 0.4778 0.1031 0.5804 0.093 Uiso 0.591(8) 1 calc PR B 1
H72B H 0.4271 0.2026 0.6025 0.093 Uiso 0.591(8) 1 calc PR B 1
H72C H 0.4791 0.1778 0.5191 0.093 Uiso 0.591(8) 1 calc PR B 1
C73A C 0.3258(6) 0.0849(3) 0.5187(4) 0.058(2) Uiso 0.591(8) 1 d PD B 1
H73A H 0.3718 0.0886 0.4690 0.087 Uiso 0.591(8) 1 calc PR B 1
H73B H 0.2477 0.0831 0.5177 0.087 Uiso 0.591(8) 1 calc PR B 1
H73C H 0.3662 0.0321 0.5427 0.087 Uiso 0.591(8) 1 calc PR B 1
C71B C 0.3023(10) 0.2597(3) 0.5429(7) 0.060(3) Uiso 0.409(8) 1 d PD B 2
H71D H 0.3343 0.2810 0.5766 0.090 Uiso 0.409(8) 1 calc PR B 2
H71E H 0.2194 0.2933 0.5478 0.090 Uiso 0.409(8) 1 calc PR B 2
H71F H 0.3466 0.2661 0.4932 0.090 Uiso 0.409(8) 1 calc PR B 2
C72B C 0.4395(5) 0.1092(6) 0.5289(7) 0.054(6) Uiso 0.409(8) 1 d PD B 2
H72D H 0.4717 0.1359 0.4833 0.081 Uiso 0.409(8) 1 calc PR B 2
H72E H 0.4406 0.0509 0.5198 0.081 Uiso 0.409(8) 1 calc PR B 2
H72F H 0.4873 0.1056 0.5634 0.081 Uiso 0.409(8) 1 calc PR B 2
C73B C 0.2375(10) 0.1652(10) 0.5078(7) 0.049(6) Uiso 0.409(8) 1 d PD B 2
H73D H 0.2881 0.1517 0.4591 0.074 Uiso 0.409(8) 1 calc PR B 2
H73E H 0.1799 0.2226 0.5069 0.074 Uiso 0.409(8) 1 calc PR B 2
H73F H 0.1964 0.1218 0.5238 0.074 Uiso 0.409(8) 1 calc PR B 2
C74 C -0.1153(3) 0.2423(2) 1.1481(2) 0.0323(8) Uani 1 1 d . . .
H74 H -0.0668 0.2424 1.0974 0.039 Uiso 1 1 calc R . .
Cl75 Cl -0.25540(8) 0.31990(5) 1.15285(5) 0.0382(2) Uani 1 1 d . . .
Cl76 Cl -0.13044(9) 0.13820(5) 1.17000(6) 0.0443(3) Uani 1 1 d . . .
Cl77 Cl -0.04417(11) 0.26878(6) 1.20582(8) 0.0625(4) Uani 1 1 d . . .
C78 C -0.3988(6) 0.2257(4) 1.3241(4) 0.061(2) Uani 0.721(4) 1 d P . .
H78 H -0.3460 0.2337 1.2763 0.073 Uiso 0.721(4) 1 calc PR . .
Cl79 Cl -0.3362(2) 0.12296(13) 1.35776(12) 0.1009(10) Uani 0.721(4) 1 d P . .
Cl80 Cl -0.5310(2) 0.23281(14) 1.30915(14) 0.0937(9) Uani 0.721(4) 1 d P . .
Cl81 Cl -0.4139(3) 0.30723(16) 1.37832(17) 0.1264(12) Uani 0.721(4) 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0221(3) 0.0176(3) 0.0221(3) 0.0007(2) -0.0070(2) -0.0077(2)
Cl2 0.0244(4) 0.0237(4) 0.0311(5) 0.0004(3) -0.0065(3) -0.0047(3)
Cl3 0.0286(4) 0.0219(4) 0.0268(4) 0.0042(3) -0.0114(3) -0.0097(3)
O4 0.0207(11) 0.0218(10) 0.0257(12) -0.0013(8) -0.0060(9) -0.0054(8)
O5 0.0295(13) 0.0217(10) 0.0251(12) 0.0025(8) -0.0100(10) -0.0087(9)
C6 0.0333(19) 0.0271(16) 0.0314(19) 0.0030(13) -0.0151(15) -0.0080(14)
C7 0.0211(17) 0.0262(16) 0.0247(17) 0.0007(12) -0.0054(14) -0.0020(12)
C8 0.0275(18) 0.0250(16) 0.0287(19) -0.0006(13) -0.0123(15) -0.0026(13)
C9 0.0281(18) 0.0243(16) 0.0203(17) 0.0010(12) -0.0031(14) -0.0015(13)
C10 0.037(2) 0.0215(15) 0.0224(17) -0.0006(12) -0.0075(15) -0.0086(13)
C11 0.0307(18) 0.0227(15) 0.0208(17) -0.0012(12) -0.0077(14) -0.0044(13)
C12 0.0291(18) 0.0204(15) 0.0197(16) 0.0010(11) -0.0064(14) -0.0055(12)
C13 0.036(2) 0.0220(15) 0.0286(19) 0.0023(12) -0.0121(15) -0.0093(13)
C14 0.035(2) 0.0298(17) 0.0309(19) 0.0018(13) -0.0117(15) -0.0190(14)
C15 0.050(2) 0.043(2) 0.027(2) 0.0060(15) -0.0130(17) -0.0270(18)
C16 0.044(2) 0.051(2) 0.025(2) -0.0078(16) 0.0012(17) -0.0246(18)
C17 0.031(2) 0.0375(19) 0.040(2) -0.0108(16) -0.0011(17) -0.0146(15)
C18 0.0276(18) 0.0259(16) 0.034(2) -0.0047(13) -0.0069(15) -0.0143(13)
C19 0.0263(17) 0.0240(15) 0.0229(17) -0.0036(12) -0.0053(13) -0.0134(13)
C20 0.0250(18) 0.0272(16) 0.042(2) -0.0065(14) -0.0140(15) -0.0044(13)
C21 0.0269(18) 0.0266(16) 0.0295(19) -0.0029(13) -0.0098(14) -0.0084(13)
C22 0.0265(19) 0.0326(18) 0.035(2) -0.0052(14) -0.0122(15) -0.0076(14)
C23 0.0248(18) 0.0273(16) 0.0321(19) -0.0006(13) -0.0099(15) -0.0032(13)
C24 0.034(2) 0.0213(15) 0.0314(19) -0.0032(13) -0.0112(15) -0.0052(13)
C25 0.0258(18) 0.0246(15) 0.0249(18) 0.0027(12) -0.0103(14) -0.0077(13)
C26 0.0251(17) 0.0232(15) 0.0209(17) 0.0032(12) -0.0072(13) -0.0054(12)
C27 0.0272(18) 0.0201(15) 0.0278(18) -0.0017(12) -0.0060(14) -0.0058(12)
C28 0.0299(18) 0.0241(15) 0.0257(18) -0.0010(12) -0.0102(14) -0.0116(13)
C29 0.037(2) 0.0270(17) 0.032(2) -0.0035(14) -0.0082(16) -0.0073(14)
C30 0.054(2) 0.0338(18) 0.0213(18) 0.0010(14) -0.0088(17) -0.0110(17)
C31 0.054(2) 0.0270(17) 0.0247(19) 0.0016(13) -0.0171(17) -0.0057(16)
C32 0.036(2) 0.0269(16) 0.0238(18) -0.0020(13) -0.0130(15) -0.0091(14)
C33 0.0290(18) 0.0197(14) 0.0250(17) -0.0012(12) -0.0123(14) -0.0092(12)
N34 0.0245(14) 0.0199(12) 0.0229(14) 0.0011(10) -0.0073(11) -0.0087(10)
N35 0.0263(15) 0.0243(13) 0.0246(15) -0.0023(10) -0.0059(12) -0.0113(11)
N36 0.0231(14) 0.0222(13) 0.0245(15) -0.0014(10) -0.0043(11) -0.0083(10)
C37 0.0218(17) 0.0243(15) 0.0252(17) -0.0002(12) -0.0030(13) -0.0082(12)
C38 0.0233(17) 0.0200(14) 0.0258(18) 0.0007(12) -0.0059(13) -0.0085(12)
C39 0.0264(18) 0.0233(15) 0.0255(18) -0.0062(12) -0.0060(14) -0.0064(12)
C40 0.0221(17) 0.0302(16) 0.0201(17) -0.0071(12) 0.0001(13) -0.0079(13)
C41 0.0312(19) 0.0286(17) 0.033(2) 0.0007(14) -0.0083(16) -0.0098(14)
C42 0.034(2) 0.054(2) 0.035(2) 0.0025(17) -0.0154(17) -0.0118(17)
C43 0.032(2) 0.059(2) 0.033(2) -0.0065(17) -0.0093(17) -0.0222(18)
C44 0.038(2) 0.039(2) 0.046(2) 0.0013(16) -0.0091(18) -0.0215(16)
C45 0.038(2) 0.0275(17) 0.035(2) 0.0009(14) -0.0150(16) -0.0120(14)
N46 0.0227(14) 0.0233(13) 0.0233(14) 0.0001(10) -0.0066(11) -0.0099(10)
N47 0.0220(14) 0.0233(13) 0.0289(16) 0.0034(11) -0.0073(12) -0.0086(10)
N48 0.0256(15) 0.0197(12) 0.0305(16) 0.0010(10) -0.0107(12) -0.0082(10)
C49 0.0258(18) 0.0209(15) 0.0313(19) -0.0019(12) -0.0115(14) -0.0068(12)
C50 0.0269(18) 0.0176(14) 0.0302(18) 0.0022(12) -0.0152(14) -0.0059(12)
C51 0.0272(18) 0.0213(15) 0.036(2) 0.0050(13) -0.0075(15) -0.0129(13)
C52 0.0289(18) 0.0248(15) 0.0251(18) 0.0038(12) -0.0098(14) -0.0085(13)
C53 0.0305(19) 0.0316(17) 0.0307(19) 0.0067(14) -0.0096(15) -0.0137(14)
C54 0.029(2) 0.049(2) 0.033(2) 0.0028(16) -0.0088(16) -0.0160(16)
C55 0.028(2) 0.042(2) 0.036(2) 0.0027(16) -0.0065(16) -0.0021(15)
C56 0.036(2) 0.0293(18) 0.036(2) -0.0002(14) -0.0066(17) -0.0022(15)
C57 0.031(2) 0.0307(17) 0.036(2) -0.0008(14) -0.0110(16) -0.0122(14)
C58 0.039(2) 0.0206(15) 0.0262(18) 0.0009(12) -0.0099(15) -0.0018(13)
C59 0.050(2) 0.0217(16) 0.039(2) 0.0041(14) -0.0185(18) -0.0021(15)
C60 0.049(2) 0.0346(19) 0.037(2) 0.0068(15) -0.0214(18) -0.0084(17)
C61 0.046(2) 0.0368(19) 0.030(2) 0.0030(15) -0.0082(17) -0.0075(16)
C62 0.075(3) 0.091(3) 0.029(2) -0.010(2) 0.006(2) -0.046(3)
C66 0.030(2) 0.0323(18) 0.043(2) -0.0128(15) -0.0114(17) -0.0037(14)
C67 0.026(2) 0.042(2) 0.077(3) -0.020(2) -0.014(2) 0.0024(16)
C68 0.034(2) 0.0321(19) 0.050(3) -0.0091(16) -0.0127(18) 0.0031(15)
C69 0.033(2) 0.057(2) 0.047(3) -0.0127(19) -0.0006(19) -0.0050(18)
C70 0.077(3) 0.062(3) 0.031(2) 0.0049(19) -0.003(2) -0.023(2)
C74 0.0301(19) 0.0290(17) 0.037(2) 0.0038(14) -0.0086(16) -0.0093(14)
Cl75 0.0288(5) 0.0387(5) 0.0426(6) 0.0004(4) -0.0084(4) -0.0047(4)
Cl76 0.0501(6) 0.0300(4) 0.0532(6) 0.0013(4) -0.0075(5) -0.0174(4)
Cl77 0.0674(8) 0.0328(5) 0.1024(10) -0.0074(5) -0.0579(7) -0.0043(5)
C78 0.067(4) 0.042(3) 0.059(4) 0.003(3) 0.008(3) -0.015(3)
Cl79 0.138(2) 0.0639(12) 0.0707(14) 0.0182(9) -0.0106(13) -0.0081(12)
Cl80 0.1017(18) 0.0768(14) 0.114(2) -0.0010(12) -0.0260(14) -0.0431(12)
Cl81 0.160(3) 0.0930(17) 0.130(2) -0.0588(16) -0.022(2) -0.0354(16)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O4 1.817(2) . ?
Ti1 O5 1.832(2) . ?
Ti1 N34 2.155(3) . ?
Ti1 N46 2.177(3) . ?
Ti1 Cl3 2.4070(9) . ?
Ti1 Cl2 2.4122(9) . ?
O4 C26 1.367(4) . ?
O5 C12 1.367(4) . ?
C6 C7 1.505(4) . ?
C6 C32 1.525(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.392(4) . ?
C7 C12 1.410(5) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(5) . ?
C9 C58 1.530(4) . ?
C10 C11 1.383(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.406(4) . ?
C11 C13 1.516(5) . ?
C13 C14 1.527(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.393(5) . ?
C14 C15 1.398(5) . ?
C15 C16 1.391(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(5) . ?
C16 C62 1.565(5) . ?
C17 C18 1.394(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.406(4) . ?
C18 C20 1.517(5) . ?
C19 C38 1.480(4) . ?
C20 C21 1.513(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.398(5) . ?
C21 C26 1.404(5) . ?
C22 C23 1.387(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(5) . ?
C23 C66 1.531(5) . ?
C24 C25 1.392(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(4) . ?
C25 C27 1.518(5) . ?
C27 C28 1.516(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C33 1.395(5) . ?
C28 C29 1.400(5) . ?
C29 C30 1.385(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(5) . ?
C30 C70 1.548(5) . ?
C31 C32 1.394(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.396(4) . ?
C33 C50 1.483(4) . ?
N34 N35 1.317(4) . ?
N34 C38 1.357(4) . ?
N35 N36 1.323(4) . ?
N36 C37 1.356(4) . ?
N36 C39 1.474(4) . ?
C37 C38 1.363(5) . ?
C37 H37 0.9500 . ?
C39 C40 1.499(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C45 1.393(4) . ?
C40 C41 1.393(5) . ?
C41 C42 1.381(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.383(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.378(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
N46 N47 1.333(3) . ?
N46 C50 1.363(4) . ?
N47 N48 1.325(4) . ?
N48 C49 1.341(4) . ?
N48 C51 1.470(4) . ?
C49 C50 1.365(4) . ?
C49 H49 0.9500 . ?
C51 C52 1.494(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.391(5) . ?
C52 C57 1.401(4) . ?
C53 C54 1.396(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.373(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.385(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.385(5) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C60 1.531(5) . ?
C58 C61 1.533(5) . ?
C58 C59 1.544(4) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C64B 1.5290(10) . ?
C62 C63A 1.5294(10) . ?
C62 C65B 1.5300(10) . ?
C62 C64A 1.5316(10) . ?
C62 C63B 1.5317(10) . ?
C62 C65A 1.5320(10) . ?
C63A H63A 0.9800 . ?
C63A H63B 0.9800 . ?
C63A H63C 0.9800 . ?
C64A H64A 0.9800 . ?
C64A H64B 0.9800 . ?
C64A H64C 0.9800 . ?
C65A H65A 0.9800 . ?
C65A H65B 0.9800 . ?
C65A H65C 0.9800 . ?
C63B H63D 0.9800 . ?
C63B H63E 0.9800 . ?
C63B H63F 0.9800 . ?
C64B H64D 0.9891 . ?
C64B H64E 0.9892 . ?
C64B H64F 0.9891 . ?
C65B H65D 0.9800 . ?
C65B H65E 0.9800 . ?
C65B H65F 0.9800 . ?
C66 C68 1.528(5) . ?
C66 C67 1.534(5) . ?
C66 C69 1.553(6) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 C72B 1.5282(10) . ?
C70 C71A 1.5293(10) . ?
C70 C73B 1.5300(10) . ?
C70 C71B 1.5301(10) . ?
C70 C73A 1.5321(10) . ?
C70 C72A 1.5328(10) . ?
C71A H71A 0.9800 . ?
C71A H71B 0.9800 . ?
C71A H71C 0.9800 . ?
C72A H72A 0.9800 . ?
C72A H72B 0.9800 . ?
C72A H72C 0.9800 . ?
C73A H73A 0.9800 . ?
C73A H73B 0.9800 . ?
C73A H73C 0.9800 . ?
C71B H71D 0.9800 . ?
C71B H71E 0.9800 . ?
C71B H71F 0.9800 . ?
C72B H72D 0.9800 . ?
C72B H72E 0.9800 . ?
C72B H72F 0.9800 . ?
C73B H73D 0.9800 . ?
C73B H73E 0.9800 . ?
C73B H73F 0.9800 . ?
C74 Cl77 1.740(4) . ?
C74 Cl76 1.765(3) . ?
C74 Cl75 1.772(3) . ?
C74 H74 1.0000 . ?
C78 Cl80 1.695(8) . ?
C78 Cl81 1.708(7) . ?
C78 Cl79 1.737(6) . ?
C78 H78 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ti1 O5 95.24(10) . . ?
O4 Ti1 N34 96.95(10) . . ?
O5 Ti1 N34 95.26(10) . . ?
O4 Ti1 N46 95.29(10) . . ?
O5 Ti1 N46 98.01(10) . . ?
N34 Ti1 N46 161.02(10) . . ?
O4 Ti1 Cl3 88.38(7) . . ?
O5 Ti1 Cl3 176.03(7) . . ?
N34 Ti1 Cl3 82.66(7) . . ?
N46 Ti1 Cl3 83.25(7) . . ?
O4 Ti1 Cl2 177.58(7) . . ?
O5 Ti1 Cl2 86.42(7) . . ?
N34 Ti1 Cl2 84.64(7) . . ?
N46 Ti1 Cl2 82.72(7) . . ?
Cl3 Ti1 Cl2 90.01(3) . . ?
C26 O4 Ti1 169.1(2) . . ?
C12 O5 Ti1 165.6(2) . . ?
C7 C6 C32 109.7(3) . . ?
C7 C6 H6A 109.7 . . ?
C32 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
C32 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C12 118.9(3) . . ?
C8 C7 C6 119.0(3) . . ?
C12 C7 C6 122.0(3) . . ?
C7 C8 C9 123.2(3) . . ?
C7 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C8 C9 C10 116.1(3) . . ?
C8 C9 C58 123.1(3) . . ?
C10 C9 C58 120.7(3) . . ?
C11 C10 C9 123.3(3) . . ?
C11 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 C13 118.2(3) . . ?
C12 C11 C13 122.7(3) . . ?
O5 C12 C11 120.6(3) . . ?
O5 C12 C7 120.0(3) . . ?
C11 C12 C7 119.3(3) . . ?
C11 C13 C14 111.0(3) . . ?
C11 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C11 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.0 . . ?
C19 C14 C15 119.0(3) . . ?
C19 C14 C13 120.1(3) . . ?
C15 C14 C13 120.8(3) . . ?
C16 C15 C14 121.7(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 117.9(3) . . ?
C17 C16 C62 122.3(3) . . ?
C15 C16 C62 119.6(3) . . ?
C16 C17 C18 121.8(3) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C19 118.8(3) . . ?
C17 C18 C20 121.0(3) . . ?
C19 C18 C20 120.1(3) . . ?
C14 C19 C18 119.8(3) . . ?
C14 C19 C38 119.3(3) . . ?
C18 C19 C38 120.8(3) . . ?
C21 C20 C18 110.8(3) . . ?
C21 C20 H20A 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C22 C21 C26 118.7(3) . . ?
C22 C21 C20 119.2(3) . . ?
C26 C21 C20 122.0(3) . . ?
C23 C22 C21 123.0(3) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C24 C23 C22 116.4(3) . . ?
C24 C23 C66 120.3(3) . . ?
C22 C23 C66 123.3(3) . . ?
C23 C24 C25 123.6(3) . . ?
C23 C24 H24 118.2 . . ?
C25 C24 H24 118.2 . . ?
C24 C25 C26 118.4(3) . . ?
C24 C25 C27 119.7(3) . . ?
C26 C25 C27 121.8(3) . . ?
O4 C26 C21 119.8(3) . . ?
O4 C26 C25 120.4(3) . . ?
C21 C26 C25 119.8(3) . . ?
C28 C27 C25 110.2(2) . . ?
C28 C27 H27A 109.6 . . ?
C25 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
C25 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C33 C28 C29 118.3(3) . . ?
C33 C28 C27 121.1(3) . . ?
C29 C28 C27 120.4(3) . . ?
C30 C29 C28 121.7(3) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C31 C30 C29 118.4(3) . . ?
C31 C30 C70 123.7(3) . . ?
C29 C30 C70 117.8(3) . . ?
C30 C31 C32 122.0(3) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 118.3(3) . . ?
C33 C32 C6 121.0(3) . . ?
C31 C32 C6 120.3(3) . . ?
C32 C33 C28 120.8(3) . . ?
C32 C33 C50 119.5(3) . . ?
C28 C33 C50 119.6(3) . . ?
N35 N34 C38 109.9(3) . . ?
N35 N34 Ti1 122.65(18) . . ?
C38 N34 Ti1 127.3(2) . . ?
N34 N35 N36 106.3(2) . . ?
N35 N36 C37 111.7(3) . . ?
N35 N36 C39 118.4(2) . . ?
C37 N36 C39 129.5(3) . . ?
N36 C37 C38 104.6(3) . . ?
N36 C37 H37 127.7 . . ?
C38 C37 H37 127.7 . . ?
N34 C38 C37 107.5(3) . . ?
N34 C38 C19 123.3(3) . . ?
C37 C38 C19 129.2(3) . . ?
N36 C39 C40 113.7(3) . . ?
N36 C39 H39A 108.8 . . ?
C40 C39 H39A 108.8 . . ?
N36 C39 H39B 108.8 . . ?
C40 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C45 C40 C41 118.3(3) . . ?
C45 C40 C39 120.5(3) . . ?
C41 C40 C39 121.1(3) . . ?
C42 C41 C40 120.7(3) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C43 120.1(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 120.0(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 119.9(3) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C40 120.9(3) . . ?
C44 C45 H45 119.6 . . ?
C40 C45 H45 119.5 . . ?
N47 N46 C50 110.0(3) . . ?
N47 N46 Ti1 122.8(2) . . ?
C50 N46 Ti1 127.2(2) . . ?
N48 N47 N46 105.7(3) . . ?
N47 N48 C49 112.0(3) . . ?
N47 N48 C51 118.8(3) . . ?
C49 N48 C51 129.2(3) . . ?
N48 C49 C50 105.8(3) . . ?
N48 C49 H49 127.1 . . ?
C50 C49 H49 127.1 . . ?
N46 C50 C49 106.5(3) . . ?
N46 C50 C33 122.5(3) . . ?
C49 C50 C33 131.0(3) . . ?
N48 C51 C52 114.2(2) . . ?
N48 C51 H51A 108.7 . . ?
C52 C51 H51A 108.7 . . ?
N48 C51 H51B 108.7 . . ?
C52 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?
C53 C52 C57 118.7(3) . . ?
C53 C52 C51 119.4(3) . . ?
C57 C52 C51 121.7(3) . . ?
C52 C53 C54 120.5(3) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C55 C54 C53 119.8(3) . . ?
C55 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C54 C55 C56 120.7(3) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C57 C56 C55 119.7(3) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C56 C57 C52 120.7(3) . . ?
C56 C57 H57 119.7 . . ?
C52 C57 H57 119.7 . . ?
C60 C58 C9 112.1(3) . . ?
C60 C58 C61 109.3(3) . . ?
C9 C58 C61 108.2(3) . . ?
C60 C58 C59 108.5(3) . . ?
C9 C58 C59 109.9(3) . . ?
C61 C58 C59 108.8(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C64B C62 C63A 118.1(7) . . ?
C64B C62 C65B 109.01(10) . . ?
C63A C62 C65B 76.3(5) . . ?
C64B C62 C64A 28.5(5) . . ?
C63A C62 C64A 108.90(10) . . ?
C65B C62 C64A 135.7(6) . . ?
C64B C62 C63B 108.88(10) . . ?
C63A C62 C63B 32.6(5) . . ?
C65B C62 C63B 108.79(10) . . ?
C64A C62 C63B 87.5(5) . . ?
C64B C62 C65A 80.1(5) . . ?
C63A C62 C65A 108.84(10) . . ?
C65B C62 C65A 36.1(4) . . ?
C64A C62 C65A 108.62(10) . . ?
C63B C62 C65A 140.7(5) . . ?
C64B C62 C16 121.0(6) . . ?
C63A C62 C16 115.1(4) . . ?
C65B C62 C16 106.4(6) . . ?
C64A C62 C16 110.0(4) . . ?
C63B C62 C16 102.1(5) . . ?
C65A C62 C16 105.2(4) . . ?
C62 C63A H63A 109.5 . . ?
C62 C63A H63B 109.5 . . ?
C62 C63A H63C 109.5 . . ?
C62 C64A H64A 109.5 . . ?
C62 C64A H64B 109.5 . . ?
C62 C64A H64C 109.5 . . ?
C62 C65A H65A 109.5 . . ?
C62 C65A H65B 109.5 . . ?
C62 C65A H65C 109.5 . . ?
C62 C63B H63D 109.4 . . ?
C62 C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C62 C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
C62 C64B H64D 110.3 . . ?
C62 C64B H64E 110.4 . . ?
H64D C64B H64E 108.6 . . ?
C62 C64B H64F 110.4 . . ?
H64D C64B H64F 108.6 . . ?
H64E C64B H64F 108.6 . . ?
C62 C65B H65D 109.4 . . ?
C62 C65B H65E 109.4 . . ?
H65D C65B H65E 109.5 . . ?
C62 C65B H65F 109.5 . . ?
H65D C65B H65F 109.5 . . ?
H65E C65B H65F 109.5 . . ?
C68 C66 C23 110.6(3) . . ?
C68 C66 C67 107.5(3) . . ?
C23 C66 C67 111.4(3) . . ?
C68 C66 C69 109.4(3) . . ?
C23 C66 C69 108.1(3) . . ?
C67 C66 C69 109.9(3) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C66 C69 H69A 109.5 . . ?
C66 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C66 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C72B C70 C71A 117.5(5) . . ?
C72B C70 C73B 109.05(10) . . ?
C71A C70 C73B 58.1(6) . . ?
C72B C70 C71B 109.03(9) . . ?
C71A C70 C71B 33.0(5) . . ?
C73B C70 C71B 91.1(8) . . ?
C72B C70 C73A 64.8(5) . . ?
C71A C70 C73A 108.86(10) . . ?
C73B C70 C73A 56.3(6) . . ?
C71B C70 C73A 137.0(5) . . ?
C72B C70 C72A 44.1(5) . . ?
C71A C70 C72A 108.81(10) . . ?
C73B C70 C72A 144.8(6) . . ?
C71B C70 C72A 81.4(5) . . ?
C73A C70 C72A 108.54(10) . . ?
C72B C70 C30 127.6(6) . . ?
C71A C70 C30 113.5(3) . . ?
C73B C70 C30 107.0(6) . . ?
C71B C70 C30 107.0(5) . . ?
C73A C70 C30 109.0(3) . . ?
C72A C70 C30 108.0(4) . . ?
C70 C71A H71A 109.5 . . ?
C70 C71A H71B 109.5 . . ?
C70 C71A H71C 109.5 . . ?
C70 C72A H72A 109.5 . . ?
C70 C72A H72B 109.5 . . ?
C70 C72A H72C 109.5 . . ?
C70 C73A H73A 109.5 . . ?
C70 C73A H73B 109.5 . . ?
C70 C73A H73C 109.5 . . ?
C70 C71B H71D 109.5 . . ?
C70 C71B H71E 109.5 . . ?
H71D C71B H71E 109.5 . . ?
C70 C71B H71F 109.5 . . ?
H71D C71B H71F 109.5 . . ?
H71E C71B H71F 109.5 . . ?
C70 C72B H72D 109.5 . . ?
C70 C72B H72E 109.5 . . ?
H72D C72B H72E 109.5 . . ?
C70 C72B H72F 109.5 . . ?
H72D C72B H72F 109.5 . . ?
H72E C72B H72F 109.5 . . ?
C70 C73B H73D 109.5 . . ?
C70 C73B H73E 109.5 . . ?
H73D C73B H73E 109.5 . . ?
C70 C73B H73F 109.5 . . ?
H73D C73B H73F 109.5 . . ?
H73E C73B H73F 109.5 . . ?
Cl77 C74 Cl76 110.6(2) . . ?
Cl77 C74 Cl75 110.5(2) . . ?
Cl76 C74 Cl75 109.99(19) . . ?
Cl77 C74 H74 108.6 . . ?
Cl76 C74 H74 108.6 . . ?
Cl75 C74 H74 108.6 . . ?
Cl80 C78 Cl81 110.1(4) . . ?
Cl80 C78 Cl79 109.9(4) . . ?
Cl81 C78 Cl79 113.7(5) . . ?
Cl80 C78 H78 107.6 . . ?
Cl81 C78 H78 107.6 . . ?
Cl79 C78 H78 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.648
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.095