# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Darrin Richeson'
'Tiow-Gan Ong'
'Glenn P. A. Yap'

_publ_contact_author_name        'Prof Darrin Richeson'
_publ_contact_author_address     
;
Department of Chemistry
University of Ottawa
Center for Catalysis Research & Inn
Ottawa
Ontario
K1N 6N5
CANADA
;

_publ_contact_author_email       DARRIN@SCIENCE.UOTTAWA.CA

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Catalytic C=N bond metathesis of carbodiimides by
group 4 and 5 imido complexes supported by guanidinate ligands
;

data_dr2106
_database_code_CSD               216357

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H62 F5 N9 Ti'
_chemical_formula_weight         775.86

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'
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'

_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                   11.0583(13)
_cell_length_b                   12.7145(15)
_cell_length_c                   14.9289(18)
_cell_angle_alpha                88.106(2)
_cell_angle_beta                 83.591(2)
_cell_angle_gamma                82.446(2)
_cell_volume                     2067.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    2755
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.24

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9486
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'

_exptl_special_details           
;
Data collection is performed with three batch runs at phi = 0.00 deg
(606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames)
A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal
and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged,
corrected for decay (if any), and treated with multi-scan absorption corrections
(if required). All symmetry-equivalent reflections are merged for
centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data.
;

_diffrn_ambient_temperature      203(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            12027
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         28.81
_reflns_number_total             8660
_reflns_number_gt                4832
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, Bruker (2000)'
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'

_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.
;

_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^)+(0.0787P)^2^+0.0529P] 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         8660
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1730
_refine_ls_wR_factor_gt          0.1441
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
Ti Ti 0.28871(5) 0.24434(5) 0.24944(4) 0.02667(18) Uani 1 1 d . . .
F1 F 0.4570(2) -0.01863(18) 0.16429(16) 0.0513(6) Uani 1 1 d . . .
F2 F 0.5672(2) -0.2015(2) 0.2271(2) 0.0789(9) Uani 1 1 d . . .
F3 F 0.4620(3) -0.30122(19) 0.3757(2) 0.0780(9) Uani 1 1 d . . .
F4 F 0.2449(2) -0.20882(19) 0.46232(17) 0.0599(7) Uani 1 1 d . . .
F5 F 0.13873(18) -0.02205(17) 0.40556(15) 0.0439(6) Uani 1 1 d . . .
N1 N 0.2454(2) 0.0913(2) 0.25516(19) 0.0276(7) Uani 1 1 d . . .
N2 N 0.1213(2) 0.2328(2) 0.2227(2) 0.0318(7) Uani 1 1 d . . .
N3 N 0.0376(2) 0.0728(2) 0.2122(2) 0.0333(7) Uani 1 1 d . . .
N4 N 0.4796(2) 0.1945(2) 0.2516(2) 0.0304(7) Uani 1 1 d . . .
N5 N 0.3941(2) 0.2439(2) 0.12649(19) 0.0287(7) Uani 1 1 d . . .
N6 N 0.6138(3) 0.1950(3) 0.1125(2) 0.0430(9) Uani 1 1 d . . .
N7 N 0.2765(3) 0.4050(2) 0.2770(2) 0.0309(7) Uani 1 1 d . . .
N8 N 0.2548(3) 0.2857(2) 0.3881(2) 0.0363(8) Uani 1 1 d . . .
N9 N 0.2170(4) 0.4697(3) 0.4281(3) 0.0579(11) Uani 1 1 d . . .
C1 C 0.4038(3) -0.0612(3) 0.2403(3) 0.0381(9) Uani 1 1 d . . .
C2 C 0.4603(4) -0.1571(3) 0.2709(3) 0.0502(11) Uani 1 1 d . . .
C3 C 0.4079(4) -0.2074(3) 0.3457(3) 0.0505(12) Uani 1 1 d . . .
C4 C 0.2984(4) -0.1603(3) 0.3891(3) 0.0400(10) Uani 1 1 d . . .
C5 C 0.2450(3) -0.0643(3) 0.3589(3) 0.0327(8) Uani 1 1 d . . .
C6 C 0.2946(3) -0.0098(3) 0.2834(2) 0.0294(8) Uani 1 1 d . . .
C7 C 0.0335(4) 0.3910(4) 0.1395(3) 0.0597(14) Uani 1 1 d . . .
H7A H 0.0910 0.3709 0.0862 0.072 Uiso 1 1 calc R . .
H7B H 0.0725 0.4365 0.1763 0.072 Uiso 1 1 calc R . .
C8 C -0.0838(4) 0.4537(4) 0.1094(3) 0.0565(13) Uani 1 1 d . . .
H8A H -0.0638 0.5186 0.0772 0.068 Uiso 1 1 calc R . .
H8B H -0.1190 0.4109 0.0680 0.068 Uiso 1 1 calc R . .
C9 C -0.1767(4) 0.4821(4) 0.1898(4) 0.0639(14) Uani 1 1 d . . .
H9A H -0.1447 0.5309 0.2279 0.077 Uiso 1 1 calc R . .
H9B H -0.2525 0.5185 0.1689 0.077 Uiso 1 1 calc R . .
C10 C -0.2043(4) 0.3862(4) 0.2436(3) 0.0620(14) Uani 1 1 d . . .
H10A H -0.2465 0.3421 0.2079 0.074 Uiso 1 1 calc R . .
H10B H -0.2596 0.4078 0.2976 0.074 Uiso 1 1 calc R . .
C11 C -0.0878(3) 0.3202(3) 0.2721(3) 0.0425(10) Uani 1 1 d . . .
H11A H -0.0528 0.3602 0.3156 0.051 Uiso 1 1 calc R . .
H11B H -0.1097 0.2545 0.3020 0.051 Uiso 1 1 calc R . .
C12 C 0.0075(3) 0.2929(3) 0.1930(3) 0.0414(10) Uani 1 1 d . . .
H12A H -0.0269 0.2465 0.1531 0.050 Uiso 1 1 calc R . .
C13 C -0.0544(3) -0.0840(3) 0.2709(3) 0.0401(10) Uani 1 1 d . . .
H13A H -0.0432 -0.0684 0.3331 0.048 Uiso 1 1 calc R . .
H13B H -0.1345 -0.0479 0.2578 0.048 Uiso 1 1 calc R . .
C14 C -0.0513(4) -0.2038(3) 0.2614(3) 0.0491(11) Uani 1 1 d . . .
H14A H 0.0261 -0.2402 0.2797 0.059 Uiso 1 1 calc R . .
H14B H -0.1187 -0.2283 0.3016 0.059 Uiso 1 1 calc R . .
C15 C -0.0631(4) -0.2322(4) 0.1653(3) 0.0543(12) Uani 1 1 d . . .
H15A H -0.1450 -0.2036 0.1498 0.065 Uiso 1 1 calc R . .
H15B H -0.0545 -0.3096 0.1606 0.065 Uiso 1 1 calc R . .
C16 C 0.0335(4) -0.1886(4) 0.0987(3) 0.0523(11) Uani 1 1 d . . .
H16A H 0.1147 -0.2259 0.1079 0.063 Uiso 1 1 calc R . .
H16B H 0.0175 -0.2020 0.0371 0.063 Uiso 1 1 calc R . .
C17 C 0.0334(3) -0.0706(3) 0.1097(3) 0.0421(10) Uani 1 1 d . . .
H17A H -0.0435 -0.0328 0.0918 0.051 Uiso 1 1 calc R . .
H17B H 0.1010 -0.0469 0.0692 0.051 Uiso 1 1 calc R . .
C18 C 0.0470(3) -0.0419(3) 0.2062(2) 0.0297(8) Uani 1 1 d . . .
H18A H 0.1282 -0.0743 0.2225 0.036 Uiso 1 1 calc R . .
C19 C 0.1262(3) 0.1222(3) 0.2305(2) 0.0306(8) Uani 1 1 d . . .
C20 C 0.3798(3) 0.2225(3) 0.0317(2) 0.0369(9) Uani 1 1 d . . .
H20A H 0.4597 0.1883 0.0031 0.044 Uiso 1 1 calc R . .
C21 C 0.2850(4) 0.1463(3) 0.0263(3) 0.0488(11) Uani 1 1 d . . .
H21A H 0.3086 0.0813 0.0595 0.073 Uiso 1 1 calc R . .
H21B H 0.2810 0.1301 -0.0362 0.073 Uiso 1 1 calc R . .
H21C H 0.2052 0.1791 0.0523 0.073 Uiso 1 1 calc R . .
C22 C 0.3444(4) 0.3257(3) -0.0212(3) 0.0504(11) Uani 1 1 d . . .
H22A H 0.4057 0.3731 -0.0178 0.076 Uiso 1 1 calc R . .
H22B H 0.2651 0.3596 0.0046 0.076 Uiso 1 1 calc R . .
H22C H 0.3403 0.3096 -0.0837 0.076 Uiso 1 1 calc R . .
C23 C 0.5781(3) 0.1866(3) 0.3120(3) 0.0381(9) Uani 1 1 d . . .
H23A H 0.6561 0.1961 0.2749 0.046 Uiso 1 1 calc R . .
C24 C 0.5941(4) 0.0768(3) 0.3591(3) 0.0521(12) Uani 1 1 d . . .
H24A H 0.6111 0.0220 0.3141 0.078 Uiso 1 1 calc R . .
H24B H 0.5194 0.0669 0.3973 0.078 Uiso 1 1 calc R . .
H24C H 0.6619 0.0725 0.3957 0.078 Uiso 1 1 calc R . .
C25 C 0.5528(4) 0.2725(3) 0.3832(3) 0.0498(11) Uani 1 1 d . . .
H25A H 0.5437 0.3418 0.3537 0.075 Uiso 1 1 calc R . .
H25B H 0.6207 0.2671 0.4196 0.075 Uiso 1 1 calc R . .
H25C H 0.4779 0.2631 0.4213 0.075 Uiso 1 1 calc R . .
C26 C 0.6459(4) 0.2628(4) 0.0352(3) 0.0563(13) Uani 1 1 d . . .
H26A H 0.5799 0.3204 0.0302 0.084 Uiso 1 1 calc R . .
H26B H 0.6583 0.2214 -0.0192 0.084 Uiso 1 1 calc R . .
H26C H 0.7207 0.2918 0.0432 0.084 Uiso 1 1 calc R . .
C27 C 0.7062(3) 0.1052(3) 0.1272(3) 0.0534(12) Uani 1 1 d . . .
H27A H 0.6779 0.0643 0.1796 0.080 Uiso 1 1 calc R . .
H27B H 0.7823 0.1309 0.1372 0.080 Uiso 1 1 calc R . .
H27C H 0.7199 0.0606 0.0746 0.080 Uiso 1 1 calc R . .
C28 C 0.4999(3) 0.2100(3) 0.1630(3) 0.0315(8) Uani 1 1 d . . .
C29 C 0.3242(3) 0.5045(3) 0.2428(3) 0.0391(10) Uani 1 1 d . . .
H29A H 0.3201 0.5515 0.2950 0.047 Uiso 1 1 calc R . .
C30 C 0.4573(4) 0.4844(4) 0.2033(4) 0.0766(17) Uani 1 1 d . . .
H30A H 0.5058 0.4465 0.2473 0.115 Uiso 1 1 calc R . .
H30B H 0.4876 0.5516 0.1877 0.115 Uiso 1 1 calc R . .
H30C H 0.4638 0.4422 0.1496 0.115 Uiso 1 1 calc R . .
C31 C 0.2500(5) 0.5635(4) 0.1747(4) 0.0826(19) Uani 1 1 d . . .
H31A H 0.1648 0.5771 0.1998 0.124 Uiso 1 1 calc R . .
H31B H 0.2561 0.5213 0.1210 0.124 Uiso 1 1 calc R . .
H31C H 0.2810 0.6304 0.1590 0.124 Uiso 1 1 calc R . .
C32 C 0.1948(4) 0.2458(3) 0.4739(3) 0.0424(10) Uani 1 1 d . . .
H32A H 0.1855 0.3028 0.5187 0.051 Uiso 1 1 calc R . .
C33 C 0.2762(4) 0.1506(3) 0.5089(3) 0.0483(11) Uani 1 1 d . . .
H33A H 0.3561 0.1708 0.5161 0.072 Uiso 1 1 calc R . .
H33B H 0.2856 0.0934 0.4662 0.072 Uiso 1 1 calc R . .
H33C H 0.2387 0.1270 0.5666 0.072 Uiso 1 1 calc R . .
C34 C 0.0667(4) 0.2184(3) 0.4617(3) 0.0473(11) Uani 1 1 d . . .
H34A H 0.0169 0.2810 0.4409 0.071 Uiso 1 1 calc R . .
H34B H 0.0285 0.1939 0.5189 0.071 Uiso 1 1 calc R . .
H34C H 0.0738 0.1629 0.4177 0.071 Uiso 1 1 calc R . .
C35 C 0.1287(5) 0.5603(3) 0.4093(4) 0.0764(17) Uani 1 1 d . . .
H35A H 0.0982 0.5510 0.3520 0.115 Uiso 1 1 calc R . .
H35B H 0.1680 0.6244 0.4065 0.115 Uiso 1 1 calc R . .
H35C H 0.0609 0.5662 0.4567 0.115 Uiso 1 1 calc R . .
C36 C 0.2738(6) 0.4703(5) 0.5112(4) 0.092(2) Uani 1 1 d . . .
H36A H 0.3318 0.4066 0.5154 0.137 Uiso 1 1 calc R . .
H36B H 0.2111 0.4725 0.5622 0.137 Uiso 1 1 calc R . .
H36C H 0.3166 0.5322 0.5114 0.137 Uiso 1 1 calc R . .
C37 C 0.2495(3) 0.3889(3) 0.3668(3) 0.0365(9) Uani 1 1 d . . .

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
Ti 0.0283(3) 0.0209(3) 0.0280(4) 0.0028(3) 0.0031(3) 0.0011(2)
F1 0.0464(13) 0.0437(14) 0.0568(16) -0.0020(12) 0.0131(11) 0.0046(10)
F2 0.0635(17) 0.0573(17) 0.103(2) -0.0094(16) 0.0030(16) 0.0332(13)
F3 0.099(2) 0.0349(14) 0.097(2) 0.0103(15) -0.0361(18) 0.0208(14)
F4 0.0790(18) 0.0476(15) 0.0582(17) 0.0265(13) -0.0268(14) -0.0175(13)
F5 0.0401(12) 0.0475(13) 0.0420(14) 0.0109(11) 0.0009(10) -0.0059(10)
N1 0.0255(14) 0.0219(15) 0.0333(18) 0.0032(13) -0.0009(12) 0.0017(11)
N2 0.0276(15) 0.0268(16) 0.0374(19) 0.0076(14) 0.0037(13) 0.0024(12)
N3 0.0263(15) 0.0339(17) 0.039(2) 0.0064(15) -0.0031(13) -0.0041(13)
N4 0.0256(14) 0.0340(17) 0.0311(19) 0.0020(14) -0.0048(13) -0.0012(12)
N5 0.0264(14) 0.0315(16) 0.0267(18) 0.0037(13) 0.0000(12) -0.0017(12)
N6 0.0296(16) 0.047(2) 0.046(2) 0.0060(17) 0.0095(14) 0.0041(14)
N7 0.0353(16) 0.0188(15) 0.0357(19) 0.0040(13) 0.0026(13) 0.0010(12)
N8 0.0457(18) 0.0301(17) 0.0280(18) -0.0016(14) 0.0084(14) 0.0033(14)
N9 0.091(3) 0.038(2) 0.041(2) -0.0162(18) 0.007(2) -0.0025(19)
C1 0.039(2) 0.030(2) 0.043(3) -0.0018(18) -0.0008(18) 0.0014(16)
C2 0.042(2) 0.035(2) 0.070(3) -0.008(2) -0.012(2) 0.0121(18)
C3 0.068(3) 0.022(2) 0.062(3) 0.003(2) -0.029(2) 0.0084(19)
C4 0.056(2) 0.030(2) 0.039(3) 0.0106(18) -0.0211(19) -0.0129(18)
C5 0.0344(19) 0.031(2) 0.034(2) 0.0037(17) -0.0106(16) -0.0058(15)
C6 0.0302(18) 0.0241(18) 0.035(2) 0.0026(16) -0.0088(15) -0.0036(14)
C7 0.039(2) 0.058(3) 0.074(4) 0.024(3) 0.008(2) 0.007(2)
C8 0.045(2) 0.065(3) 0.052(3) 0.027(2) 0.000(2) 0.008(2)
C9 0.041(2) 0.054(3) 0.089(4) 0.021(3) 0.000(2) 0.013(2)
C10 0.040(2) 0.071(3) 0.064(3) 0.017(3) 0.010(2) 0.018(2)
C11 0.037(2) 0.043(2) 0.043(3) 0.009(2) 0.0004(18) 0.0062(17)
C12 0.0288(19) 0.031(2) 0.060(3) 0.009(2) 0.0018(18) 0.0037(15)
C13 0.042(2) 0.043(2) 0.035(2) 0.0069(19) 0.0010(18) -0.0107(17)
C14 0.057(3) 0.044(3) 0.047(3) 0.005(2) 0.000(2) -0.016(2)
C15 0.063(3) 0.046(3) 0.057(3) -0.005(2) -0.008(2) -0.018(2)
C16 0.053(3) 0.059(3) 0.045(3) -0.009(2) -0.004(2) -0.005(2)
C17 0.037(2) 0.053(3) 0.033(3) 0.007(2) 0.0031(17) -0.0031(18)
C18 0.0243(16) 0.0298(19) 0.034(2) 0.0065(17) -0.0044(15) -0.0001(14)
C19 0.0303(18) 0.032(2) 0.025(2) 0.0073(16) 0.0041(15) 0.0046(15)
C20 0.037(2) 0.046(2) 0.025(2) 0.0014(18) 0.0029(16) 0.0016(17)
C21 0.059(3) 0.055(3) 0.033(3) -0.005(2) -0.006(2) -0.009(2)
C22 0.054(3) 0.057(3) 0.037(3) 0.011(2) -0.001(2) -0.001(2)
C23 0.037(2) 0.037(2) 0.041(3) -0.0006(19) -0.0119(17) 0.0022(16)
C24 0.054(3) 0.044(3) 0.057(3) 0.010(2) -0.019(2) 0.005(2)
C25 0.053(2) 0.052(3) 0.048(3) -0.002(2) -0.024(2) -0.003(2)
C26 0.040(2) 0.070(3) 0.055(3) 0.005(3) 0.015(2) -0.010(2)
C27 0.033(2) 0.050(3) 0.071(3) -0.011(2) 0.002(2) 0.0118(18)
C28 0.0284(17) 0.0277(19) 0.036(2) -0.0019(17) 0.0034(15) -0.0009(14)
C29 0.043(2) 0.0219(19) 0.050(3) 0.0009(18) 0.0031(18) -0.0042(16)
C30 0.039(2) 0.063(3) 0.123(5) 0.037(3) 0.007(3) -0.011(2)
C31 0.067(3) 0.060(3) 0.123(5) 0.048(3) -0.026(3) -0.020(3)
C32 0.064(3) 0.033(2) 0.025(2) 0.0000(17) 0.0120(19) 0.0013(18)
C33 0.053(2) 0.054(3) 0.035(3) 0.015(2) -0.0018(19) -0.005(2)
C34 0.047(2) 0.051(3) 0.035(3) 0.012(2) 0.0130(18) 0.0099(19)
C35 0.095(4) 0.034(3) 0.087(4) -0.015(3) 0.038(3) 0.006(2)
C36 0.144(6) 0.084(4) 0.055(4) -0.028(3) 0.000(4) -0.045(4)
C37 0.040(2) 0.032(2) 0.034(2) -0.0024(18) 0.0030(17) -0.0002(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
Ti N2 1.962(3) . ?
Ti N5 2.061(3) . ?
Ti N1 2.061(3) . ?
Ti N7 2.081(3) . ?
Ti N4 2.127(3) . ?
Ti N8 2.132(3) . ?
Ti C28 2.531(3) . ?
Ti C37 2.543(4) . ?
Ti C19 2.569(4) . ?
F1 C1 1.350(4) . ?
F2 C2 1.349(5) . ?
F3 C3 1.349(4) . ?
F4 C4 1.354(4) . ?
F5 C5 1.353(4) . ?
N1 C6 1.400(4) . ?
N1 C19 1.411(4) . ?
N2 C19 1.402(4) . ?
N2 C12 1.488(4) . ?
N3 C19 1.289(5) . ?
N3 C18 1.454(4) . ?
N4 C28 1.330(4) . ?
N4 C23 1.481(4) . ?
N5 C28 1.359(4) . ?
N5 C20 1.479(5) . ?
N6 C28 1.387(4) . ?
N6 C27 1.457(5) . ?
N6 C26 1.458(5) . ?
N7 C37 1.355(5) . ?
N7 C29 1.487(4) . ?
N8 C37 1.335(4) . ?
N8 C32 1.481(4) . ?
N9 C37 1.384(5) . ?
N9 C35 1.450(6) . ?
N9 C36 1.453(7) . ?
C1 C2 1.384(5) . ?
C1 C6 1.395(5) . ?
C2 C3 1.376(6) . ?
C3 C4 1.381(6) . ?
C4 C5 1.369(5) . ?
C5 C6 1.400(5) . ?
C7 C12 1.501(5) . ?
C7 C8 1.534(5) . ?
C8 C9 1.510(6) . ?
C9 C10 1.485(6) . ?
C10 C11 1.535(5) . ?
C11 C12 1.510(5) . ?
C13 C14 1.531(5) . ?
C13 C18 1.535(5) . ?
C14 C15 1.514(6) . ?
C15 C16 1.523(6) . ?
C16 C17 1.515(6) . ?
C17 C18 1.526(5) . ?
C20 C21 1.528(5) . ?
C20 C22 1.538(5) . ?
C23 C25 1.527(6) . ?
C23 C24 1.540(5) . ?
C29 C31 1.499(6) . ?
C29 C30 1.516(5) . ?
C32 C33 1.525(5) . ?
C32 C34 1.534(6) . ?

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
N2 Ti N5 105.91(12) . . ?
N2 Ti N1 65.91(11) . . ?
N5 Ti N1 100.50(12) . . ?
N2 Ti N7 101.55(12) . . ?
N5 Ti N7 98.75(11) . . ?
N1 Ti N7 159.34(11) . . ?
N2 Ti N4 155.88(12) . . ?
N5 Ti N4 64.09(11) . . ?
N1 Ti N4 93.41(11) . . ?
N7 Ti N4 101.71(11) . . ?
N2 Ti N8 100.43(12) . . ?
N5 Ti N8 151.01(12) . . ?
N1 Ti N8 101.14(11) . . ?
N7 Ti N8 63.75(11) . . ?
N4 Ti N8 95.53(12) . . ?
N2 Ti C28 134.95(13) . . ?
N5 Ti C28 32.41(11) . . ?
N1 Ti C28 98.55(11) . . ?
N7 Ti C28 101.71(11) . . ?
N4 Ti C28 31.69(11) . . ?
N8 Ti C28 124.45(13) . . ?
N2 Ti C37 101.34(12) . . ?
N5 Ti C37 128.23(12) . . ?
N1 Ti C37 130.86(12) . . ?
N7 Ti C37 32.16(11) . . ?
N4 Ti C37 101.73(12) . . ?
N8 Ti C37 31.66(11) . . ?
C28 Ti C37 118.50(12) . . ?
N2 Ti C19 32.69(11) . . ?
N5 Ti C19 105.08(12) . . ?
N1 Ti C19 33.24(10) . . ?
N7 Ti C19 132.63(11) . . ?
N4 Ti C19 125.46(11) . . ?
N8 Ti C19 103.61(12) . . ?
C28 Ti C19 120.21(11) . . ?
C37 Ti C19 120.97(11) . . ?
C6 N1 C19 127.0(3) . . ?
C6 N1 Ti 138.8(2) . . ?
C19 N1 Ti 93.6(2) . . ?
C19 N2 C12 117.2(3) . . ?
C19 N2 Ti 98.2(2) . . ?
C12 N2 Ti 144.4(2) . . ?
C19 N3 C18 123.7(3) . . ?
C28 N4 C23 122.9(3) . . ?
C28 N4 Ti 91.2(2) . . ?
C23 N4 Ti 141.7(2) . . ?
C28 N5 C20 121.5(3) . . ?
C28 N5 Ti 93.2(2) . . ?
C20 N5 Ti 137.2(2) . . ?
C28 N6 C27 122.8(3) . . ?
C28 N6 C26 122.3(3) . . ?
C27 N6 C26 114.7(3) . . ?
C37 N7 C29 120.0(3) . . ?
C37 N7 Ti 93.0(2) . . ?
C29 N7 Ti 142.0(2) . . ?
C37 N8 C32 122.7(3) . . ?
C37 N8 Ti 91.4(2) . . ?
C32 N8 Ti 139.3(3) . . ?
C37 N9 C35 120.8(4) . . ?
C37 N9 C36 121.8(4) . . ?
C35 N9 C36 117.3(4) . . ?
F1 C1 C2 117.3(3) . . ?
F1 C1 C6 120.0(3) . . ?
C2 C1 C6 122.7(4) . . ?
F2 C2 C3 120.0(4) . . ?
F2 C2 C1 119.7(4) . . ?
C3 C2 C1 120.3(4) . . ?
F3 C3 C2 120.8(4) . . ?
F3 C3 C4 120.5(4) . . ?
C2 C3 C4 118.8(3) . . ?
F4 C4 C5 120.2(4) . . ?
F4 C4 C3 119.7(3) . . ?
C5 C4 C3 120.1(4) . . ?
F5 C5 C4 116.9(3) . . ?
F5 C5 C6 119.7(3) . . ?
C4 C5 C6 123.4(4) . . ?
C1 C6 N1 121.1(3) . . ?
C1 C6 C5 114.7(3) . . ?
N1 C6 C5 124.0(3) . . ?
C12 C7 C8 111.9(3) . . ?
C9 C8 C7 110.6(4) . . ?
C10 C9 C8 111.3(4) . . ?
C9 C10 C11 112.2(4) . . ?
C12 C11 C10 112.3(3) . . ?
N2 C12 C7 111.8(3) . . ?
N2 C12 C11 111.3(3) . . ?
C7 C12 C11 110.7(3) . . ?
C14 C13 C18 110.8(3) . . ?
C15 C14 C13 111.4(3) . . ?
C14 C15 C16 111.8(4) . . ?
C17 C16 C15 111.7(4) . . ?
C16 C17 C18 112.6(3) . . ?
N3 C18 C17 109.1(3) . . ?
N3 C18 C13 109.9(3) . . ?
C17 C18 C13 109.6(3) . . ?
N3 C19 N2 122.5(3) . . ?
N3 C19 N1 135.1(3) . . ?
N2 C19 N1 102.3(3) . . ?
N3 C19 Ti 170.7(3) . . ?
N2 C19 Ti 49.10(16) . . ?
N1 C19 Ti 53.19(17) . . ?
N5 C20 C21 111.1(3) . . ?
N5 C20 C22 111.4(3) . . ?
C21 C20 C22 110.2(3) . . ?
N4 C23 C25 111.6(3) . . ?
N4 C23 C24 111.2(3) . . ?
C25 C23 C24 109.2(3) . . ?
N4 C28 N5 111.5(3) . . ?
N4 C28 N6 125.4(3) . . ?
N5 C28 N6 123.1(3) . . ?
N4 C28 Ti 57.13(17) . . ?
N5 C28 Ti 54.39(17) . . ?
N6 C28 Ti 177.1(3) . . ?
N7 C29 C31 113.3(3) . . ?
N7 C29 C30 111.9(3) . . ?
C31 C29 C30 109.2(4) . . ?
N8 C32 C33 109.7(3) . . ?
N8 C32 C34 110.8(3) . . ?
C33 C32 C34 111.7(3) . . ?
N8 C37 N7 111.6(3) . . ?
N8 C37 N9 124.4(3) . . ?
N7 C37 N9 124.0(3) . . ?
N8 C37 Ti 57.0(2) . . ?
N7 C37 Ti 54.82(18) . . ?
N9 C37 Ti 174.5(3) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ti N1 C6 -169.8(4) . . . . ?
N5 Ti N1 C6 87.4(4) . . . . ?
N7 Ti N1 C6 -114.1(4) . . . . ?
N4 Ti N1 C6 23.1(4) . . . . ?
N8 Ti N1 C6 -73.2(4) . . . . ?
C28 Ti N1 C6 54.5(4) . . . . ?
C37 Ti N1 C6 -85.6(4) . . . . ?
C19 Ti N1 C6 -171.1(5) . . . . ?
N2 Ti N1 C19 1.33(19) . . . . ?
N5 Ti N1 C19 -101.5(2) . . . . ?
N7 Ti N1 C19 57.0(4) . . . . ?
N4 Ti N1 C19 -165.8(2) . . . . ?
N8 Ti N1 C19 97.9(2) . . . . ?
C28 Ti N1 C19 -134.3(2) . . . . ?
C37 Ti N1 C19 85.5(2) . . . . ?
N5 Ti N2 C19 93.3(2) . . . . ?
N1 Ti N2 C19 -1.3(2) . . . . ?
N7 Ti N2 C19 -164.1(2) . . . . ?
N4 Ti N2 C19 31.6(4) . . . . ?
N8 Ti N2 C19 -99.0(2) . . . . ?
C28 Ti N2 C19 76.2(2) . . . . ?
C37 Ti N2 C19 -131.2(2) . . . . ?
N5 Ti N2 C12 -80.0(4) . . . . ?
N1 Ti N2 C12 -174.6(5) . . . . ?
N7 Ti N2 C12 22.7(4) . . . . ?
N4 Ti N2 C12 -141.7(4) . . . . ?
N8 Ti N2 C12 87.7(4) . . . . ?
C28 Ti N2 C12 -97.1(4) . . . . ?
C37 Ti N2 C12 55.5(4) . . . . ?
C19 Ti N2 C12 -173.3(6) . . . . ?
N2 Ti N4 C28 70.9(4) . . . . ?
N5 Ti N4 C28 0.8(2) . . . . ?
N1 Ti N4 C28 100.8(2) . . . . ?
N7 Ti N4 C28 -93.4(2) . . . . ?
N8 Ti N4 C28 -157.7(2) . . . . ?
C37 Ti N4 C28 -126.2(2) . . . . ?
C19 Ti N4 C28 91.3(2) . . . . ?
N2 Ti N4 C23 -134.4(4) . . . . ?
N5 Ti N4 C23 155.4(4) . . . . ?
N1 Ti N4 C23 -104.6(4) . . . . ?
N7 Ti N4 C23 61.3(4) . . . . ?
N8 Ti N4 C23 -3.0(4) . . . . ?
C28 Ti N4 C23 154.6(5) . . . . ?
C37 Ti N4 C23 28.4(4) . . . . ?
C19 Ti N4 C23 -114.1(4) . . . . ?
N2 Ti N5 C28 -157.2(2) . . . . ?
N1 Ti N5 C28 -89.4(2) . . . . ?
N7 Ti N5 C28 98.1(2) . . . . ?
N4 Ti N5 C28 -0.7(2) . . . . ?
N8 Ti N5 C28 48.3(3) . . . . ?
C37 Ti N5 C28 83.8(2) . . . . ?
C19 Ti N5 C28 -123.2(2) . . . . ?
N2 Ti N5 C20 -10.9(4) . . . . ?
N1 Ti N5 C20 56.8(3) . . . . ?
N7 Ti N5 C20 -115.7(3) . . . . ?
N4 Ti N5 C20 145.5(4) . . . . ?
N8 Ti N5 C20 -165.5(3) . . . . ?
C28 Ti N5 C20 146.2(4) . . . . ?
C37 Ti N5 C20 -129.9(3) . . . . ?
C19 Ti N5 C20 23.0(3) . . . . ?
N2 Ti N7 C37 93.0(2) . . . . ?
N5 Ti N7 C37 -158.7(2) . . . . ?
N1 Ti N7 C37 42.7(4) . . . . ?
N4 Ti N7 C37 -93.5(2) . . . . ?
N8 Ti N7 C37 -3.0(2) . . . . ?
C28 Ti N7 C37 -125.9(2) . . . . ?
C19 Ti N7 C37 81.4(2) . . . . ?
N2 Ti N7 C29 -115.2(4) . . . . ?
N5 Ti N7 C29 -6.8(4) . . . . ?
N1 Ti N7 C29 -165.4(4) . . . . ?
N4 Ti N7 C29 58.4(4) . . . . ?
N8 Ti N7 C29 148.8(4) . . . . ?
C28 Ti N7 C29 26.0(4) . . . . ?
C37 Ti N7 C29 151.8(5) . . . . ?
C19 Ti N7 C29 -126.8(4) . . . . ?
N2 Ti N8 C37 -94.7(2) . . . . ?
N5 Ti N8 C37 60.4(3) . . . . ?
N1 Ti N8 C37 -162.0(2) . . . . ?
N7 Ti N8 C37 3.1(2) . . . . ?
N4 Ti N8 C37 103.4(2) . . . . ?
C28 Ti N8 C37 89.4(2) . . . . ?
C19 Ti N8 C37 -128.0(2) . . . . ?
N2 Ti N8 C32 54.2(4) . . . . ?
N5 Ti N8 C32 -150.6(3) . . . . ?
N1 Ti N8 C32 -13.0(4) . . . . ?
N7 Ti N8 C32 152.0(4) . . . . ?
N4 Ti N8 C32 -107.6(4) . . . . ?
C28 Ti N8 C32 -121.6(4) . . . . ?
C37 Ti N8 C32 149.0(5) . . . . ?
C19 Ti N8 C32 20.9(4) . . . . ?
F1 C1 C2 F2 3.0(6) . . . . ?
C6 C1 C2 F2 -178.7(4) . . . . ?
F1 C1 C2 C3 -176.9(4) . . . . ?
C6 C1 C2 C3 1.4(7) . . . . ?
F2 C2 C3 F3 -0.3(7) . . . . ?
C1 C2 C3 F3 179.7(4) . . . . ?
F2 C2 C3 C4 -179.9(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
F3 C3 C4 F4 -0.2(6) . . . . ?
C2 C3 C4 F4 179.5(4) . . . . ?
F3 C3 C4 C5 179.1(4) . . . . ?
C2 C3 C4 C5 -1.2(7) . . . . ?
F4 C4 C5 F5 0.2(5) . . . . ?
C3 C4 C5 F5 -179.0(4) . . . . ?
F4 C4 C5 C6 -179.6(3) . . . . ?
C3 C4 C5 C6 1.2(6) . . . . ?
F1 C1 C6 N1 -7.2(6) . . . . ?
C2 C1 C6 N1 174.5(4) . . . . ?
F1 C1 C6 C5 176.8(3) . . . . ?
C2 C1 C6 C5 -1.5(6) . . . . ?
C19 N1 C6 C1 125.4(4) . . . . ?
Ti N1 C6 C1 -65.8(5) . . . . ?
C19 N1 C6 C5 -59.0(5) . . . . ?
Ti N1 C6 C5 109.9(4) . . . . ?
F5 C5 C6 C1 -179.6(3) . . . . ?
C4 C5 C6 C1 0.2(6) . . . . ?
F5 C5 C6 N1 4.5(5) . . . . ?
C4 C5 C6 N1 -175.7(3) . . . . ?
C12 C7 C8 C9 56.6(6) . . . . ?
C7 C8 C9 C10 -55.9(6) . . . . ?
C8 C9 C10 C11 54.4(6) . . . . ?
C9 C10 C11 C12 -53.2(6) . . . . ?
C19 N2 C12 C7 -148.3(4) . . . . ?
Ti N2 C12 C7 24.2(6) . . . . ?
C19 N2 C12 C11 87.3(4) . . . . ?
Ti N2 C12 C11 -100.1(4) . . . . ?
C8 C7 C12 N2 -179.6(4) . . . . ?
C8 C7 C12 C11 -54.9(5) . . . . ?
C10 C11 C12 N2 177.7(4) . . . . ?
C10 C11 C12 C7 52.8(5) . . . . ?
C18 C13 C14 C15 -56.8(5) . . . . ?
C13 C14 C15 C16 54.6(5) . . . . ?
C14 C15 C16 C17 -53.0(5) . . . . ?
C15 C16 C17 C18 54.1(5) . . . . ?
C19 N3 C18 C17 -115.6(4) . . . . ?
C19 N3 C18 C13 124.2(4) . . . . ?
C16 C17 C18 N3 -176.1(3) . . . . ?
C16 C17 C18 C13 -55.7(4) . . . . ?
C14 C13 C18 N3 176.4(3) . . . . ?
C14 C13 C18 C17 56.5(4) . . . . ?
C18 N3 C19 N2 170.2(3) . . . . ?
C18 N3 C19 N1 -5.3(6) . . . . ?
C18 N3 C19 Ti 145.6(15) . . . . ?
C12 N2 C19 N3 0.7(5) . . . . ?
Ti N2 C19 N3 -174.9(3) . . . . ?
C12 N2 C19 N1 177.4(3) . . . . ?
Ti N2 C19 N1 1.8(3) . . . . ?
C12 N2 C19 Ti 175.6(4) . . . . ?
C6 N1 C19 N3 -13.0(6) . . . . ?
Ti N1 C19 N3 174.3(4) . . . . ?
C6 N1 C19 N2 170.9(3) . . . . ?
Ti N1 C19 N2 -1.7(3) . . . . ?
C6 N1 C19 Ti 172.7(4) . . . . ?
N2 Ti C19 N3 27.7(16) . . . . ?
N5 Ti C19 N3 -68.4(17) . . . . ?
N1 Ti C19 N3 -154.6(18) . . . . ?
N7 Ti C19 N3 49.1(17) . . . . ?
N4 Ti C19 N3 -137.1(16) . . . . ?
N8 Ti C19 N3 115.8(17) . . . . ?
C28 Ti C19 N3 -99.7(17) . . . . ?
C37 Ti C19 N3 87.0(17) . . . . ?
N5 Ti C19 N2 -96.1(2) . . . . ?
N1 Ti C19 N2 177.8(3) . . . . ?
N7 Ti C19 N2 21.5(3) . . . . ?
N4 Ti C19 N2 -164.7(2) . . . . ?
N8 Ti C19 N2 88.1(2) . . . . ?
C28 Ti C19 N2 -127.3(2) . . . . ?
C37 Ti C19 N2 59.3(2) . . . . ?
N2 Ti C19 N1 -177.8(3) . . . . ?
N5 Ti C19 N1 86.2(2) . . . . ?
N7 Ti C19 N1 -156.3(2) . . . . ?
N4 Ti C19 N1 17.5(2) . . . . ?
N8 Ti C19 N1 -89.6(2) . . . . ?
C28 Ti C19 N1 54.9(2) . . . . ?
C37 Ti C19 N1 -118.4(2) . . . . ?
C28 N5 C20 C21 112.9(4) . . . . ?
Ti N5 C20 C21 -26.5(5) . . . . ?
C28 N5 C20 C22 -123.8(3) . . . . ?
Ti N5 C20 C22 96.8(4) . . . . ?
C28 N4 C23 C25 120.1(4) . . . . ?
Ti N4 C23 C25 -29.2(5) . . . . ?
C28 N4 C23 C24 -117.7(4) . . . . ?
Ti N4 C23 C24 93.0(4) . . . . ?
C23 N4 C28 N5 -162.7(3) . . . . ?
Ti N4 C28 N5 -1.1(3) . . . . ?
C23 N4 C28 N6 16.7(6) . . . . ?
Ti N4 C28 N6 178.3(3) . . . . ?
C23 N4 C28 Ti -161.6(4) . . . . ?
C20 N5 C28 N4 -152.6(3) . . . . ?
Ti N5 C28 N4 1.1(3) . . . . ?
C20 N5 C28 N6 28.0(5) . . . . ?
Ti N5 C28 N6 -178.3(3) . . . . ?
C20 N5 C28 Ti -153.7(3) . . . . ?
C27 N6 C28 N4 41.5(6) . . . . ?
C26 N6 C28 N4 -144.3(4) . . . . ?
C27 N6 C28 N5 -139.2(4) . . . . ?
C26 N6 C28 N5 35.0(6) . . . . ?
C27 N6 C28 Ti -168(6) . . . . ?
C26 N6 C28 Ti 6(6) . . . . ?
N2 Ti C28 N4 -146.9(2) . . . . ?
N5 Ti C28 N4 -178.7(3) . . . . ?
N1 Ti C28 N4 -82.6(2) . . . . ?
N7 Ti C28 N4 93.4(2) . . . . ?
N8 Ti C28 N4 27.3(3) . . . . ?
C37 Ti C28 N4 64.0(2) . . . . ?
C19 Ti C28 N4 -109.6(2) . . . . ?
N2 Ti C28 N5 31.8(3) . . . . ?
N1 Ti C28 N5 96.2(2) . . . . ?
N7 Ti C28 N5 -87.9(2) . . . . ?
N4 Ti C28 N5 178.7(3) . . . . ?
N8 Ti C28 N5 -154.0(2) . . . . ?
C37 Ti C28 N5 -117.3(2) . . . . ?
C19 Ti C28 N5 69.2(2) . . . . ?
N2 Ti C28 N6 62(6) . . . . ?
N5 Ti C28 N6 30(6) . . . . ?
N1 Ti C28 N6 126(6) . . . . ?
N7 Ti C28 N6 -58(6) . . . . ?
N4 Ti C28 N6 -151(6) . . . . ?
N8 Ti C28 N6 -124(6) . . . . ?
C37 Ti C28 N6 -87(6) . . . . ?
C19 Ti C28 N6 99(6) . . . . ?
C37 N7 C29 C31 -125.0(4) . . . . ?
Ti N7 C29 C31 88.0(5) . . . . ?
C37 N7 C29 C30 111.0(4) . . . . ?
Ti N7 C29 C30 -36.0(6) . . . . ?
C37 N8 C32 C33 -142.0(4) . . . . ?
Ti N8 C32 C33 75.8(5) . . . . ?
C37 N8 C32 C34 94.2(4) . . . . ?
Ti N8 C32 C34 -48.0(5) . . . . ?
C32 N8 C37 N7 -161.0(3) . . . . ?
Ti N8 C37 N7 -4.6(3) . . . . ?
C32 N8 C37 N9 17.2(6) . . . . ?
Ti N8 C37 N9 173.6(4) . . . . ?
C32 N8 C37 Ti -156.4(4) . . . . ?
C29 N7 C37 N8 -155.7(3) . . . . ?
Ti N7 C37 N8 4.7(3) . . . . ?
C29 N7 C37 N9 26.1(5) . . . . ?
Ti N7 C37 N9 -173.5(4) . . . . ?
C29 N7 C37 Ti -160.4(3) . . . . ?
C35 N9 C37 N8 -132.8(4) . . . . ?
C36 N9 C37 N8 50.4(6) . . . . ?
C35 N9 C37 N7 45.2(6) . . . . ?
C36 N9 C37 N7 -131.6(4) . . . . ?
C35 N9 C37 Ti -30(3) . . . . ?
C36 N9 C37 Ti 153(3) . . . . ?
N2 Ti C37 N8 91.5(2) . . . . ?
N5 Ti C37 N8 -147.6(2) . . . . ?
N1 Ti C37 N8 23.7(3) . . . . ?
N7 Ti C37 N8 -174.8(3) . . . . ?
N4 Ti C37 N8 -81.4(2) . . . . ?
C28 Ti C37 N8 -110.2(2) . . . . ?
C19 Ti C37 N8 63.2(2) . . . . ?
N2 Ti C37 N7 -93.7(2) . . . . ?
N5 Ti C37 N7 27.2(3) . . . . ?
N1 Ti C37 N7 -161.55(19) . . . . ?
N4 Ti C37 N7 93.4(2) . . . . ?
N8 Ti C37 N7 174.8(3) . . . . ?
C28 Ti C37 N7 64.6(2) . . . . ?
C19 Ti C37 N7 -122.0(2) . . . . ?
N2 Ti C37 N9 -15(3) . . . . ?
N5 Ti C37 N9 106(3) . . . . ?
N1 Ti C37 N9 -83(3) . . . . ?
N7 Ti C37 N9 79(3) . . . . ?
N4 Ti C37 N9 172(3) . . . . ?
N8 Ti C37 N9 -106(3) . . . . ?
C28 Ti C37 N9 143(3) . . . . ?
C19 Ti C37 N9 -43(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.803
_diffrn_reflns_theta_full        28.81
_diffrn_measured_fraction_theta_full 0.803
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.060

data_dr2124
_database_code_CSD               216358

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H71 Cl N7 O3 Ta'
_chemical_formula_weight         866.40

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.002(3)
_cell_length_b                   22.236(5)
_cell_length_c                   21.629(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.98(3)
_cell_angle_gamma                90.00
_cell_volume                     4306(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    208(2)
_cell_measurement_reflns_used    46
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      19.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6916
_exptl_absorpt_correction_T_max  0.7772
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'

_exptl_special_details           
;
Data collection is performed with three batch runs at phi = 0.00 deg
(606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames)
A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal
and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged,
corrected for decay (if any), and treated with multi-scan absorption corrections
(if required). All symmetry-equivalent reflections are merged for
centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data.
;

_diffrn_ambient_temperature      208(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            6906
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         19.99
_reflns_number_total             3540
_reflns_number_gt                2507
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, Bruker (2000)'
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'

_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.
;

_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^)+(0.2000P)^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         3540
_refine_ls_number_parameters     433
_refine_ls_number_restraints     400
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0993
_refine_ls_wR_factor_ref         0.2689
_refine_ls_wR_factor_gt          0.2398
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_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
Ta Ta 0.22063(9) 0.18791(3) 0.66732(4) 0.0274(5) Uani 1 1 d U . .
Cl Cl -0.0474(6) 0.1840(2) 0.6242(3) 0.0422(15) Uani 1 1 d U . .
N1 N 0.1992(18) 0.2842(6) 0.6377(8) 0.032(3) Uani 1 1 d U . .
N2 N 0.4118(17) 0.2411(6) 0.6592(8) 0.034(3) Uani 1 1 d U . .
N3 N 0.4124(17) 0.1335(6) 0.6718(8) 0.033(3) Uani 1 1 d U . .
N4 N 0.2006(18) 0.0881(7) 0.6635(8) 0.041(3) Uani 1 1 d U . .
N5 N 0.4147(19) 0.3414(7) 0.6184(8) 0.041(4) Uani 1 1 d U . .
H5A H 0.3641 0.3635 0.5904 0.050 Uiso 1 1 calc R . .
N6 N 0.4156(18) 0.0253(6) 0.6548(8) 0.038(4) Uani 1 1 d U . .
H6A H 0.3682 -0.0011 0.6305 0.045 Uiso 1 1 calc R . .
N7 N 0.195(2) 0.1957(6) 0.7485(8) 0.034(3) Uani 1 1 d U . .
O1 O 0.2443(17) 0.1745(6) 0.5560(6) 0.045(3) Uani 1 1 d U . .
O2 O 0.2648(18) 0.9043(6) 0.5928(8) 0.060(4) Uani 1 1 d U . .
C1 C 0.099(2) 0.3362(9) 0.6397(10) 0.045(4) Uani 1 1 d U . .
H1A H 0.1591 0.3733 0.6467 0.054 Uiso 1 1 calc R . .
C2 C -0.007(3) 0.3303(10) 0.6911(12) 0.057(6) Uani 1 1 d U . .
H2A H 0.0515 0.3276 0.7313 0.086 Uiso 1 1 calc R . .
H2B H -0.0672 0.2943 0.6841 0.086 Uiso 1 1 calc R . .
H2C H -0.0717 0.3652 0.6903 0.086 Uiso 1 1 calc R . .
C3 C 0.000(2) 0.3411(9) 0.5765(11) 0.055(6) Uani 1 1 d U . .
H3A H 0.0640 0.3461 0.5433 0.083 Uiso 1 1 calc R . .
H3B H -0.0656 0.3755 0.5773 0.083 Uiso 1 1 calc R . .
H3C H -0.0585 0.3048 0.5694 0.083 Uiso 1 1 calc R . .
C4 C 0.345(2) 0.2923(8) 0.6377(9) 0.032(3) Uani 1 1 d U . .
C5 C 0.558(2) 0.2184(8) 0.6401(10) 0.037(4) Uani 1 1 d U . .
H5B H 0.6416 0.2366 0.6661 0.044 Uiso 1 1 calc R . .
H5C H 0.5669 0.2289 0.5966 0.044 Uiso 1 1 calc R . .
C6 C 0.560(2) 0.1506(8) 0.6481(10) 0.038(4) Uani 1 1 d U . .
H6B H 0.6437 0.1385 0.6780 0.046 Uiso 1 1 calc R . .
H6C H 0.5699 0.1308 0.6083 0.046 Uiso 1 1 calc R . .
C7 C 0.351(2) 0.0783(8) 0.6632(9) 0.033(3) Uani 1 1 d U . .
C8 C 0.098(2) 0.0397(8) 0.6807(11) 0.044(4) Uani 1 1 d U . .
H8A H 0.1607 0.0054 0.6966 0.053 Uiso 1 1 calc R . .
C9 C 0.009(3) 0.0582(10) 0.7304(12) 0.068(6) Uani 1 1 d U . .
H9A H 0.0755 0.0717 0.7659 0.102 Uiso 1 1 calc R . .
H9B H -0.0493 0.0244 0.7425 0.102 Uiso 1 1 calc R . .
H9C H -0.0570 0.0908 0.7157 0.102 Uiso 1 1 calc R . .
C10 C 0.003(3) 0.0181(10) 0.6219(13) 0.075(7) Uani 1 1 d U . .
H10A H 0.0684 0.0057 0.5912 0.112 Uiso 1 1 calc R . .
H10B H -0.0608 0.0505 0.6052 0.112 Uiso 1 1 calc R . .
H10C H -0.0578 -0.0157 0.6321 0.112 Uiso 1 1 calc R . .
C11 C 0.565(2) 0.3616(8) 0.6393(11) 0.046(5) Uani 1 1 d U . .
H11A H 0.6351 0.3298 0.6285 0.055 Uiso 1 1 calc R . .
C12 C 0.585(3) 0.3693(11) 0.7085(12) 0.078(7) Uani 1 1 d U . .
H12A H 0.5589 0.3322 0.7283 0.117 Uiso 1 1 calc R . .
H12B H 0.5216 0.4016 0.7203 0.117 Uiso 1 1 calc R . .
H12C H 0.6889 0.3791 0.7217 0.117 Uiso 1 1 calc R . .
C13 C 0.602(3) 0.4164(9) 0.6069(15) 0.088(8) Uani 1 1 d U . .
H13A H 0.5866 0.4098 0.5624 0.132 Uiso 1 1 calc R . .
H13B H 0.7052 0.4270 0.6189 0.132 Uiso 1 1 calc R . .
H13C H 0.5375 0.4489 0.6180 0.132 Uiso 1 1 calc R . .
C14 C 0.566(2) 0.0101(8) 0.6858(11) 0.044(4) Uani 1 1 d U . .
H14A H 0.6375 0.0398 0.6719 0.053 Uiso 1 1 calc R . .
C15 C 0.575(3) 0.0133(10) 0.7547(11) 0.074(7) Uani 1 1 d U . .
H15A H 0.5467 0.0533 0.7671 0.111 Uiso 1 1 calc R . .
H15B H 0.6765 0.0049 0.7721 0.111 Uiso 1 1 calc R . .
H15C H 0.5078 -0.0161 0.7697 0.111 Uiso 1 1 calc R . .
C16 C 0.608(3) -0.0508(9) 0.6625(11) 0.058(6) Uani 1 1 d U . .
H16A H 0.6027 -0.0501 0.6175 0.087 Uiso 1 1 calc R . .
H16B H 0.5390 -0.0809 0.6753 0.087 Uiso 1 1 calc R . .
H16C H 0.7087 -0.0608 0.6797 0.087 Uiso 1 1 calc R . .
C17 C 0.335(3) 0.1923(8) 0.8504(11) 0.046(4) Uani 1 1 d U . .
C18 C 0.325(3) 0.1911(9) 0.9157(11) 0.056(5) Uani 1 1 d U . .
H18A H 0.4131 0.1884 0.9431 0.067 Uiso 1 1 calc R . .
C19 C 0.187(3) 0.1941(9) 0.9395(12) 0.060(5) Uani 1 1 d U . .
H19A H 0.1832 0.1935 0.9827 0.072 Uiso 1 1 calc R . .
C20 C 0.071(3) 0.1976(9) 0.9048(11) 0.053(5) Uani 1 1 d U . .
H20A H -0.0187 0.1989 0.9233 0.064 Uiso 1 1 calc R . .
C21 C 0.061(3) 0.1998(9) 0.8402(11) 0.044(4) Uani 1 1 d U . .
C22 C 0.198(3) 0.1970(8) 0.8126(11) 0.040(4) Uani 1 1 d U . .
C23 C 0.480(3) 0.1890(9) 0.8243(11) 0.054(6) Uani 1 1 d U . .
H23A H 0.4634 0.1892 0.7793 0.081 Uiso 1 1 calc R . .
H23B H 0.5312 0.1523 0.8382 0.081 Uiso 1 1 calc R . .
H23C H 0.5406 0.2235 0.8383 0.081 Uiso 1 1 calc R . .
C24 C -0.079(3) 0.2063(11) 0.8012(11) 0.067(6) Uani 1 1 d U . .
H24A H -0.0597 0.2057 0.7578 0.101 Uiso 1 1 calc R . .
H24B H -0.1249 0.2442 0.8104 0.101 Uiso 1 1 calc R . .
H24C H -0.1447 0.1734 0.8091 0.101 Uiso 1 1 calc R . .
C25 C 0.241(4) 0.2207(11) 0.5114(10) 0.080(5) Uani 1 1 d U . .
H25A H 0.3319 0.2449 0.5182 0.096 Uiso 1 1 calc R . .
H25B H 0.1550 0.2471 0.5154 0.096 Uiso 1 1 calc R . .
C26 C 0.229(4) 0.1943(11) 0.4495(12) 0.091(6) Uani 1 1 d U . .
H26A H 0.1636 0.2181 0.4197 0.109 Uiso 1 1 calc R . .
H26B H 0.3269 0.1898 0.4342 0.109 Uiso 1 1 calc R . .
C27 C 0.165(4) 0.1376(12) 0.4611(12) 0.096(6) Uani 1 1 d U . .
H27A H 0.0555 0.1402 0.4543 0.115 Uiso 1 1 calc R . .
H27B H 0.1982 0.1073 0.4327 0.115 Uiso 1 1 calc R . .
C28 C 0.209(3) 0.1217(10) 0.5218(11) 0.075(5) Uani 1 1 d U . .
H28A H 0.2961 0.0952 0.5236 0.090 Uiso 1 1 calc R . .
H28B H 0.1279 0.1001 0.5393 0.090 Uiso 1 1 calc R . .
C29 C 0.258(3) 0.8488(10) 0.6270(13) 0.068(6) Uani 1 1 d U . .
H29A H 0.3588 0.8330 0.6374 0.082 Uiso 1 1 calc R . .
H29B H 0.2000 0.8190 0.6012 0.082 Uiso 1 1 calc R . .
C30 C 0.187(3) 0.8592(11) 0.6846(13) 0.076(7) Uani 1 1 d U . .
H30A H 0.1846 0.8218 0.7076 0.114 Uiso 1 1 calc R . .
H30B H 0.0857 0.8736 0.6742 0.114 Uiso 1 1 calc R . .
H30C H 0.2437 0.8889 0.7099 0.114 Uiso 1 1 calc R . .
C31 C 0.313(3) 0.8943(10) 0.5346(12) 0.067(6) Uani 1 1 d U . .
H31A H 0.2458 0.8660 0.5111 0.081 Uiso 1 1 calc R . .
H31B H 0.4135 0.8766 0.5396 0.081 Uiso 1 1 calc R . .
C32 C 0.316(3) 0.9544(10) 0.4990(11) 0.075(7) Uani 1 1 d U . .
H32A H 0.3486 0.9472 0.4583 0.112 Uiso 1 1 calc R . .
H32B H 0.3848 0.9819 0.5220 0.112 Uiso 1 1 calc R . .
H32C H 0.2167 0.9718 0.4944 0.112 Uiso 1 1 calc R . .
O3 O -0.254(3) 0.0385(9) 1.0405(11) 0.105(6) Uani 1 1 d U . .
C36 C -0.283(5) -0.0186(14) 1.1275(18) 0.139(12) Uani 1 1 d U . .
H36A H -0.3006 -0.0600 1.1390 0.208 Uiso 1 1 calc R . .
H36B H -0.3633 0.0065 1.1399 0.208 Uiso 1 1 calc R . .
H36C H -0.1887 -0.0050 1.1484 0.208 Uiso 1 1 calc R . .
C34 C -0.240(5) 0.0897(17) 0.9456(16) 0.143(12) Uani 1 1 d U . .
H34A H -0.2538 0.0768 0.9025 0.214 Uiso 1 1 calc R . .
H34B H -0.1402 0.1054 0.9552 0.214 Uiso 1 1 calc R . .
H34C H -0.3125 0.1209 0.9520 0.214 Uiso 1 1 calc R . .
C35 C -0.280(5) -0.0150(15) 1.0675(17) 0.126(9) Uani 1 1 d U . .
H35A H -0.3762 -0.0300 1.0480 0.151 Uiso 1 1 calc R . .
H35B H -0.2035 -0.0432 1.0563 0.151 Uiso 1 1 calc R . .
C33 C -0.261(5) 0.0425(16) 0.9830(17) 0.125(8) Uani 1 1 d U . .
H33A H -0.3609 0.0275 0.9684 0.150 Uiso 1 1 calc R . .
H33B H -0.1913 0.0118 0.9710 0.150 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
Ta 0.0095(9) 0.0145(6) 0.0556(8) -0.0016(4) -0.0085(5) -0.0012(3)
Cl 0.013(3) 0.027(3) 0.083(4) -0.005(3) -0.013(3) -0.0024(19)
N1 0.018(5) 0.015(3) 0.061(7) -0.002(4) -0.006(6) 0.003(3)
N2 0.013(4) 0.013(4) 0.073(7) 0.001(5) -0.008(5) -0.005(3)
N3 0.010(4) 0.013(3) 0.075(7) -0.002(5) 0.004(5) -0.001(3)
N4 0.014(5) 0.015(3) 0.092(8) -0.001(4) -0.005(7) -0.006(3)
N5 0.026(8) 0.014(6) 0.081(10) 0.010(7) -0.010(8) -0.001(5)
N6 0.023(8) 0.012(5) 0.075(9) -0.003(7) -0.009(7) 0.002(5)
N7 0.016(8) 0.026(7) 0.058(3) 0.001(5) -0.001(4) 0.007(6)
O1 0.045(7) 0.029(6) 0.060(3) -0.011(4) 0.000(5) -0.003(6)
O2 0.044(10) 0.039(7) 0.098(10) -0.001(7) 0.004(8) 0.008(7)
C1 0.026(8) 0.014(6) 0.089(10) -0.018(8) -0.013(7) 0.005(6)
C2 0.029(15) 0.042(13) 0.099(12) -0.028(12) -0.005(11) 0.020(10)
C3 0.019(14) 0.037(12) 0.105(11) 0.018(12) -0.019(10) 0.002(9)
C4 0.020(5) 0.015(4) 0.061(8) -0.001(5) -0.003(7) -0.002(3)
C5 0.013(6) 0.019(6) 0.075(11) 0.002(8) -0.005(8) -0.005(5)
C6 0.015(6) 0.019(6) 0.080(11) -0.002(8) 0.007(9) -0.002(5)
C7 0.016(6) 0.016(4) 0.068(9) -0.008(7) 0.008(8) -0.001(3)
C8 0.012(8) 0.021(6) 0.099(11) 0.009(8) 0.001(8) -0.001(6)
C9 0.040(16) 0.051(14) 0.117(15) 0.013(12) 0.023(11) 0.001(11)
C10 0.034(16) 0.048(15) 0.139(15) -0.022(14) -0.010(13) -0.027(11)
C11 0.023(9) 0.013(8) 0.100(11) 0.005(8) -0.006(11) -0.003(6)
C12 0.041(17) 0.080(17) 0.108(11) -0.030(13) -0.010(12) -0.032(14)
C13 0.049(16) 0.030(12) 0.184(19) 0.038(13) 0.006(17) -0.010(9)
C14 0.029(10) 0.013(8) 0.087(10) 0.008(9) -0.015(10) 0.001(7)
C15 0.09(2) 0.040(13) 0.087(10) -0.007(11) -0.038(12) 0.015(13)
C16 0.035(15) 0.034(11) 0.100(15) -0.003(10) -0.017(14) 0.022(8)
C17 0.044(8) 0.032(10) 0.059(6) 0.002(9) -0.010(5) 0.003(9)
C18 0.060(12) 0.045(11) 0.058(6) -0.001(10) -0.013(7) 0.001(10)
C19 0.074(13) 0.050(11) 0.056(9) 0.013(10) 0.000(7) 0.002(12)
C20 0.058(12) 0.041(10) 0.061(7) 0.000(10) 0.009(7) -0.014(10)
C21 0.042(8) 0.036(10) 0.056(7) -0.007(9) 0.004(6) -0.008(9)
C22 0.034(8) 0.028(9) 0.057(4) -0.008(8) -0.004(5) 0.001(8)
C23 0.038(9) 0.052(14) 0.066(12) -0.017(11) -0.016(9) 0.021(11)
C24 0.033(9) 0.093(17) 0.076(12) 0.006(14) 0.009(9) 0.009(14)
C25 0.125(15) 0.053(8) 0.058(5) -0.001(6) -0.004(11) -0.027(11)
C26 0.136(17) 0.070(12) 0.059(5) -0.006(7) -0.030(13) -0.018(12)
C27 0.141(17) 0.070(11) 0.069(8) -0.019(8) -0.017(12) -0.024(12)
C28 0.115(14) 0.043(7) 0.066(6) -0.022(5) 0.000(11) -0.007(11)
C29 0.049(15) 0.041(10) 0.112(13) 0.004(9) -0.003(11) -0.004(11)
C30 0.062(19) 0.042(15) 0.125(17) 0.022(12) 0.016(15) 0.005(13)
C31 0.054(15) 0.049(11) 0.098(12) -0.013(9) 0.003(11) -0.001(11)
C32 0.08(2) 0.064(13) 0.074(13) -0.004(10) -0.011(14) 0.010(14)
O3 0.123(16) 0.075(11) 0.117(13) 0.025(11) 0.007(15) 0.009(11)
C36 0.19(3) 0.07(2) 0.148(18) 0.055(17) -0.03(3) -0.03(2)
C34 0.18(3) 0.13(2) 0.13(2) 0.032(17) 0.06(2) 0.00(2)
C35 0.14(2) 0.082(14) 0.149(17) 0.036(14) -0.008(19) -0.010(15)
C33 0.16(2) 0.098(16) 0.119(14) 0.020(14) 0.01(2) 0.004(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
Ta N7 1.804(17) . ?
Ta N3 2.102(15) . ?
Ta N2 2.111(15) . ?
Ta N4 2.227(15) . ?
Ta N1 2.237(14) . ?
Ta O1 2.459(14) . ?
Ta Cl 2.496(6) . ?
Ta C4 2.685(19) . ?
N1 C4 1.33(2) . ?
N1 C1 1.47(2) . ?
N2 C4 1.35(2) . ?
N2 C5 1.51(2) . ?
N3 C7 1.35(2) . ?
N3 C6 1.52(2) . ?
N4 C7 1.37(2) . ?
N4 C8 1.49(2) . ?
N5 C4 1.35(2) . ?
N5 C11 1.45(2) . ?
N6 C7 1.33(2) . ?
N6 C14 1.49(3) . ?
N7 C22 1.38(3) . ?
O1 C25 1.41(3) . ?
O1 C28 1.41(2) . ?
O2 C31 1.39(3) . ?
O2 C29 1.44(3) . ?
C1 C2 1.54(3) . ?
C1 C3 1.55(3) . ?
C5 C6 1.52(3) . ?
C8 C9 1.46(3) . ?
C8 C10 1.53(3) . ?
C11 C13 1.46(3) . ?
C11 C12 1.50(3) . ?
C14 C15 1.48(3) . ?
C14 C16 1.51(3) . ?
C17 C22 1.41(4) . ?
C17 C18 1.42(3) . ?
C17 C23 1.48(4) . ?
C18 C19 1.40(4) . ?
C19 C20 1.22(3) . ?
C20 C21 1.39(3) . ?
C21 C22 1.42(3) . ?
C21 C24 1.45(3) . ?
C25 C26 1.46(3) . ?
C26 C27 1.42(3) . ?
C27 C28 1.38(3) . ?
C29 C30 1.48(3) . ?
C31 C32 1.54(3) . ?
O3 C33 1.24(3) . ?
O3 C35 1.36(3) . ?
C36 C35 1.30(4) . ?
C34 C33 1.35(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
_geom_angle_publ_flag
N7 Ta N3 101.5(7) . . ?
N7 Ta N2 102.5(7) . . ?
N3 Ta N2 69.7(6) . . ?
N7 Ta N4 96.5(6) . . ?
N3 Ta N4 59.4(6) . . ?
N2 Ta N4 128.2(6) . . ?
N7 Ta N1 99.8(6) . . ?
N3 Ta N1 127.5(6) . . ?
N2 Ta N1 59.1(6) . . ?
N4 Ta N1 159.8(6) . . ?
N7 Ta O1 177.1(6) . . ?
N3 Ta O1 79.7(6) . . ?
N2 Ta O1 80.3(6) . . ?
N4 Ta O1 81.8(5) . . ?
N1 Ta O1 81.3(5) . . ?
N7 Ta Cl 98.5(6) . . ?
N3 Ta Cl 139.0(4) . . ?
N2 Ta Cl 138.9(4) . . ?
N4 Ta Cl 83.1(4) . . ?
N1 Ta Cl 82.9(4) . . ?
O1 Ta Cl 79.0(4) . . ?
N7 Ta C4 104.4(6) . . ?
N3 Ta C4 98.5(6) . . ?
N2 Ta C4 29.7(6) . . ?
N4 Ta C4 152.5(6) . . ?
N1 Ta C4 29.5(5) . . ?
O1 Ta C4 77.9(5) . . ?
Cl Ta C4 110.6(5) . . ?
C4 N1 C1 120.3(16) . . ?
C4 N1 Ta 94.3(11) . . ?
C1 N1 Ta 141.1(14) . . ?
C4 N2 C5 124.0(16) . . ?
C4 N2 Ta 99.5(13) . . ?
C5 N2 Ta 125.3(11) . . ?
C7 N3 C6 122.6(15) . . ?
C7 N3 Ta 101.3(12) . . ?
C6 N3 Ta 125.6(11) . . ?
C7 N4 C8 121.6(15) . . ?
C7 N4 Ta 94.8(10) . . ?
C8 N4 Ta 139.5(13) . . ?
C4 N5 C11 127.0(16) . . ?
C7 N6 C14 121.8(16) . . ?
C22 N7 Ta 170.2(15) . . ?
C25 O1 C28 105.2(16) . . ?
C25 O1 Ta 125.7(13) . . ?
C28 O1 Ta 125.3(13) . . ?
C31 O2 C29 111.2(17) . . ?
N1 C1 C2 112.4(17) . . ?
N1 C1 C3 108.9(16) . . ?
C2 C1 C3 107.6(18) . . ?
N1 C4 N5 127.1(18) . . ?
N1 C4 N2 106.9(16) . . ?
N5 C4 N2 126(2) . . ?
N1 C4 Ta 56.2(9) . . ?
N5 C4 Ta 174.0(15) . . ?
N2 C4 Ta 50.8(9) . . ?
N2 C5 C6 107.6(14) . . ?
C5 C6 N3 106.7(14) . . ?
N6 C7 N3 130.2(19) . . ?
N6 C7 N4 125.7(16) . . ?
N3 C7 N4 104.0(15) . . ?
C9 C8 N4 112.3(17) . . ?
C9 C8 C10 114(2) . . ?
N4 C8 C10 109.0(19) . . ?
N5 C11 C13 110.9(18) . . ?
N5 C11 C12 111.0(19) . . ?
C13 C11 C12 112(2) . . ?
C15 C14 N6 113(2) . . ?
C15 C14 C16 112.9(18) . . ?
N6 C14 C16 107.5(16) . . ?
C22 C17 C18 116(2) . . ?
C22 C17 C23 122(2) . . ?
C18 C17 C23 122(2) . . ?
C19 C18 C17 121(3) . . ?
C20 C19 C18 121(3) . . ?
C19 C20 C21 125(3) . . ?
C20 C21 C22 117(2) . . ?
C20 C21 C24 123(2) . . ?
C22 C21 C24 120(2) . . ?
N7 C22 C17 120(2) . . ?
N7 C22 C21 119(2) . . ?
C17 C22 C21 120(2) . . ?
O1 C25 C26 109(2) . . ?
C27 C26 C25 101(2) . . ?
C28 C27 C26 108(2) . . ?
C27 C28 O1 108(2) . . ?
O2 C29 C30 110.2(19) . . ?
O2 C31 C32 109.6(19) . . ?
C33 O3 C35 120(3) . . ?
C36 C35 O3 120(3) . . ?
O3 C33 C34 131(4) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N7 Ta N1 C4 101.9(13) . . . . ?
N3 Ta N1 C4 -11.0(15) . . . . ?
N2 Ta N1 C4 3.1(11) . . . . ?
N4 Ta N1 C4 -114.4(19) . . . . ?
O1 Ta N1 C4 -80.7(12) . . . . ?
Cl Ta N1 C4 -160.6(12) . . . . ?
N7 Ta N1 C1 -52(2) . . . . ?
N3 Ta N1 C1 -165.0(19) . . . . ?
N2 Ta N1 C1 -151(2) . . . . ?
N4 Ta N1 C1 92(3) . . . . ?
O1 Ta N1 C1 125(2) . . . . ?
Cl Ta N1 C1 45(2) . . . . ?
C4 Ta N1 C1 -154(3) . . . . ?
N7 Ta N2 C4 -97.2(13) . . . . ?
N3 Ta N2 C4 165.0(13) . . . . ?
N4 Ta N2 C4 153.9(12) . . . . ?
N1 Ta N2 C4 -3.1(11) . . . . ?
O1 Ta N2 C4 82.5(12) . . . . ?
Cl Ta N2 C4 21.9(16) . . . . ?
N7 Ta N2 C5 118.5(15) . . . . ?
N3 Ta N2 C5 20.6(15) . . . . ?
N4 Ta N2 C5 9.6(18) . . . . ?
N1 Ta N2 C5 -147.5(17) . . . . ?
O1 Ta N2 C5 -61.8(15) . . . . ?
Cl Ta N2 C5 -122.4(13) . . . . ?
C4 Ta N2 C5 -144(2) . . . . ?
N7 Ta N3 C7 95.3(13) . . . . ?
N2 Ta N3 C7 -165.4(14) . . . . ?
N4 Ta N3 C7 4.5(12) . . . . ?
N1 Ta N3 C7 -152.5(12) . . . . ?
O1 Ta N3 C7 -82.0(13) . . . . ?
Cl Ta N3 C7 -22.4(16) . . . . ?
C4 Ta N3 C7 -158.0(13) . . . . ?
N7 Ta N3 C6 -119.7(16) . . . . ?
N2 Ta N3 C6 -20.4(15) . . . . ?
N4 Ta N3 C6 149.5(18) . . . . ?
N1 Ta N3 C6 -7.5(19) . . . . ?
O1 Ta N3 C6 63.0(15) . . . . ?
Cl Ta N3 C6 122.6(14) . . . . ?
C4 Ta N3 C6 -13.0(16) . . . . ?
N7 Ta N4 C7 -104.0(13) . . . . ?
N3 Ta N4 C7 -4.4(12) . . . . ?
N2 Ta N4 C7 7.6(15) . . . . ?
N1 Ta N4 C7 112.0(19) . . . . ?
O1 Ta N4 C7 78.4(12) . . . . ?
Cl Ta N4 C7 158.2(12) . . . . ?
C4 Ta N4 C7 36(2) . . . . ?
N7 Ta N4 C8 51(2) . . . . ?
N3 Ta N4 C8 151(2) . . . . ?
N2 Ta N4 C8 162.7(19) . . . . ?
N1 Ta N4 C8 -93(3) . . . . ?
O1 Ta N4 C8 -127(2) . . . . ?
Cl Ta N4 C8 -47(2) . . . . ?
C4 Ta N4 C8 -169.2(18) . . . . ?
N3 Ta N7 C22 8(8) . . . . ?
N2 Ta N7 C22 -63(8) . . . . ?
N4 Ta N7 C22 68(8) . . . . ?
N1 Ta N7 C22 -123(8) . . . . ?
O1 Ta N7 C22 123(12) . . . . ?
Cl Ta N7 C22 152(8) . . . . ?
C4 Ta N7 C22 -94(8) . . . . ?
N7 Ta O1 C25 115(11) . . . . ?
N3 Ta O1 C25 -130.3(19) . . . . ?
N2 Ta O1 C25 -59.4(19) . . . . ?
N4 Ta O1 C25 169.4(19) . . . . ?
N1 Ta O1 C25 0.5(18) . . . . ?
Cl Ta O1 C25 84.9(18) . . . . ?
C4 Ta O1 C25 -29.3(19) . . . . ?
N7 Ta O1 C28 -40(12) . . . . ?
N3 Ta O1 C28 74.7(18) . . . . ?
N2 Ta O1 C28 145.7(19) . . . . ?
N4 Ta O1 C28 14.5(18) . . . . ?
N1 Ta O1 C28 -154.4(19) . . . . ?
Cl Ta O1 C28 -70.0(18) . . . . ?
C4 Ta O1 C28 175.8(19) . . . . ?
C4 N1 C1 C2 -129(2) . . . . ?
Ta N1 C1 C2 20(3) . . . . ?
C4 N1 C1 C3 112(2) . . . . ?
Ta N1 C1 C3 -99(2) . . . . ?
C1 N1 C4 N5 -25(3) . . . . ?
Ta N1 C4 N5 173.9(19) . . . . ?
C1 N1 C4 N2 157.0(17) . . . . ?
Ta N1 C4 N2 -4.4(16) . . . . ?
C1 N1 C4 Ta 161(2) . . . . ?
C11 N5 C4 N1 154(2) . . . . ?
C11 N5 C4 N2 -28(3) . . . . ?
C11 N5 C4 Ta -85(15) . . . . ?
C5 N2 C4 N1 149.7(17) . . . . ?
Ta N2 C4 N1 4.7(17) . . . . ?
C5 N2 C4 N5 -29(3) . . . . ?
Ta N2 C4 N5 -173.6(17) . . . . ?
C5 N2 C4 Ta 145(2) . . . . ?
N7 Ta C4 N1 -84.5(13) . . . . ?
N3 Ta C4 N1 171.2(12) . . . . ?
N2 Ta C4 N1 -175(2) . . . . ?
N4 Ta C4 N1 137.1(15) . . . . ?
O1 Ta C4 N1 93.8(12) . . . . ?
Cl Ta C4 N1 20.6(12) . . . . ?
N7 Ta C4 N5 150(15) . . . . ?
N3 Ta C4 N5 46(15) . . . . ?
N2 Ta C4 N5 60(14) . . . . ?
N4 Ta C4 N5 12(15) . . . . ?
N1 Ta C4 N5 -126(15) . . . . ?
O1 Ta C4 N5 -32(15) . . . . ?
Cl Ta C4 N5 -105(15) . . . . ?
N7 Ta C4 N2 90.1(13) . . . . ?
N3 Ta C4 N2 -14.2(13) . . . . ?
N4 Ta C4 N2 -48(2) . . . . ?
N1 Ta C4 N2 175(2) . . . . ?
O1 Ta C4 N2 -91.7(12) . . . . ?
Cl Ta C4 N2 -164.8(11) . . . . ?
C4 N2 C5 C6 -153.9(18) . . . . ?
Ta N2 C5 C6 -18(2) . . . . ?
N2 C5 C6 N3 0(2) . . . . ?
C7 N3 C6 C5 155.4(18) . . . . ?
Ta N3 C6 C5 17(2) . . . . ?
C14 N6 C7 N3 35(3) . . . . ?
C14 N6 C7 N4 -147(2) . . . . ?
C6 N3 C7 N6 26(3) . . . . ?
Ta N3 C7 N6 172(2) . . . . ?
C6 N3 C7 N4 -152.9(17) . . . . ?
Ta N3 C7 N4 -6.5(17) . . . . ?
C8 N4 C7 N6 26(3) . . . . ?
Ta N4 C7 N6 -172.6(19) . . . . ?
C8 N4 C7 N3 -155.2(18) . . . . ?
Ta N4 C7 N3 6.0(16) . . . . ?
C7 N4 C8 C9 126(2) . . . . ?
Ta N4 C8 C9 -24(3) . . . . ?
C7 N4 C8 C10 -107(2) . . . . ?
Ta N4 C8 C10 102(2) . . . . ?
C4 N5 C11 C13 179(2) . . . . ?
C4 N5 C11 C12 -56(3) . . . . ?
C7 N6 C14 C15 58(2) . . . . ?
C7 N6 C14 C16 -176.1(18) . . . . ?
C22 C17 C18 C19 0(3) . . . . ?
C23 C17 C18 C19 -179.9(19) . . . . ?
C17 C18 C19 C20 0(3) . . . . ?
C18 C19 C20 C21 -1(4) . . . . ?
C19 C20 C21 C22 1(3) . . . . ?
C19 C20 C21 C24 -177(2) . . . . ?
Ta N7 C22 C17 21(9) . . . . ?
Ta N7 C22 C21 -155(7) . . . . ?
C18 C17 C22 N7 -177.1(17) . . . . ?
C23 C17 C22 N7 3(3) . . . . ?
C18 C17 C22 C21 -1(3) . . . . ?
C23 C17 C22 C21 179.9(18) . . . . ?
C20 C21 C22 N7 176.6(17) . . . . ?
C24 C21 C22 N7 -5(3) . . . . ?
C20 C21 C22 C17 0(3) . . . . ?
C24 C21 C22 C17 178.3(19) . . . . ?
C28 O1 C25 C26 -10(3) . . . . ?
Ta O1 C25 C26 -169(2) . . . . ?
O1 C25 C26 C27 23(3) . . . . ?
C25 C26 C27 C28 -29(4) . . . . ?
C26 C27 C28 O1 24(4) . . . . ?
C25 O1 C28 C27 -8(3) . . . . ?
Ta O1 C28 C27 151(2) . . . . ?
C31 O2 C29 C30 -172(2) . . . . ?
C29 O2 C31 C32 179(2) . . . . ?
C33 O3 C35 C36 -175(4) . . . . ?
C35 O3 C33 C34 180(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.881
_diffrn_reflns_theta_full        19.99
_diffrn_measured_fraction_theta_full 0.881
_refine_diff_density_max         2.399
_refine_diff_density_min         -4.440
_refine_diff_density_rms         0.249