# Copyright The Royal Society of Chemistry, 1998

data_global
#========================================================

# 1. SUBMISSION DETAILS

_publ_contact_author           # Name and address of author for correspondence
;
        Dr. W. Edward Lindsell 
        Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
;
_publ_contact_author_phone        '0131 449-5111 ext-4118'
_publ_contact_author_fax          '0131 451 3180'
_publ_contact_author_email        W.E.Lindsell@hw.ac.uk
   
_publ_requested_journal           'J. Chem. Soc., Dalton Trans.'
_publ_requested_coeditor_name     ?

_publ_contact_letter
;

;

#==============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ?

_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?

_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
    
_journal_coeditor_name            ?
_journal_coeditor_code            ?
_journal_coeditor_notes
; ?
;

_journal_techeditor_code          ?
_journal_techeditor_notes
; ?
;

_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?

_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title
;
Synthesis and Characterisation of Derivatives of Monocyclopentadienyl-bis
(arene-1,2-dithiolato)titanium(IV); Crystal Structures of M[Ti{\n~5~-
C~5~(CH~3~)~5~}(1,2-S~2~C~6~H~4~)~2~] (M = Tl and N(PPh~3~)~2~)
;

# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary.

loop_
        _publ_author_name
        _publ_author_address
'Lindsell, W. Edward'            #<--'Last name, first name' 
;       Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
; 
'Rosair, Georgina M.'            
;       Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
; 
'Spence, Malcolm A.'
;       Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
;


#==============================================================================
  
data_1
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C22 H23 S4 Ti Tl' 
_chemical_formula_weight          667.91 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
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' 
 'S'  'S'   0.1246   0.1234 
 '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' 
 'Tl'  'Tl'  -2.8358   9.6688 
 '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                    12.2824(9) 
_cell_length_b                    13.9012(10) 
_cell_length_c                    15.6661(12) 
_cell_angle_alpha                 70.396(5) 
_cell_angle_beta                  68.067(8) 
_cell_angle_gamma                 84.155(6) 
_cell_volume                      2336.6(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     27 
_cell_measurement_theta_min       4.67 
_cell_measurement_theta_max       12.43 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             dark_red 
_exptl_crystal_size_max           0.42 
_exptl_crystal_size_mid           0.24 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.899 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1288 
_exptl_absorpt_coefficient_mu     7.594 
_exptl_absorpt_correction_type    'semi-empirical via \y scans'
_exptl_absorpt_correction_T_min   0.289
_exptl_absorpt_correction_T_max   0.474 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(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        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         4.37 
_diffrn_reflns_number             9248 
_diffrn_reflns_av_R_equivalents   0.0440 
_diffrn_reflns_av_sigmaI/netI     0.0876 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.56 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              8019 
_reflns_number_observed           5095 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0330P)^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          8014 
_refine_ls_number_parameters      505 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0991 
_refine_ls_R_factor_obs           0.0470 
_refine_ls_wR_factor_all          0.1274 
_refine_ls_wR_factor_obs          0.0839 
_refine_ls_goodness_of_fit_all    1.009 
_refine_ls_goodness_of_fit_obs    1.058 
_refine_ls_restrained_S_all       1.259 
_refine_ls_restrained_S_obs       1.058 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Tl1 Tl 0.02860(5) 0.67464(4) 0.40664(4) 0.0602(2) Uani 1 d . . 
Tl2 Tl 0.08466(4) 0.94071(4) 0.09933(3) 0.04967(13) Uani 1 d . . 
Ti1 Ti 0.23303(15) 0.55240(12) 0.24824(11) 0.0326(4) Uani 1 d . . 
Ti2 Ti -0.13277(14) 1.02161(13) 0.28763(12) 0.0326(3) Uani 1 d . . 
S1 S 0.3243(3) 0.6805(2) 0.2747(2) 0.0501(6) Uani 1 d . . 
S2 S 0.2149(3) 0.4647(3) 0.4163(2) 0.0589(8) Uani 1 d . . 
S3 S 0.1469(2) 0.7074(2) 0.1718(2) 0.0416(5) Uani 1 d . . 
S4 S 0.0281(2) 0.4967(2) 0.3238(2) 0.0437(6) Uani 1 d . . 
S5 S 0.0261(3) 1.1452(2) 0.1821(2) 0.0533(7) Uani 1 d . . 
S6 S 0.0096(2) 0.9471(2) 0.3629(2) 0.0486(6) Uani 1 d . . 
S7 S -0.1364(2) 0.8477(2) 0.2900(2) 0.0430(6) Uani 1 d . . 
S8 S -0.1574(2) 1.0509(2) 0.1308(2) 0.0408(5) Uani 1 d . . 
C10 C 0.4092(11) 0.4678(10) 0.1917(9) 0.058(3) Uani 1 d . . 
C11 C 0.4099(9) 0.5532(9) 0.1138(8) 0.053(3) Uani 1 d . . 
C12 C 0.3162(10) 0.5417(9) 0.0854(8) 0.047(3) Uani 1 d . . 
C13 C 0.2599(10) 0.4499(8) 0.1440(8) 0.046(2) Uani 1 d . . 
C14 C 0.3131(11) 0.4032(8) 0.2119(7) 0.051(3) Uani 1 d . . 
C15 C 0.4924(14) 0.4473(17) 0.2433(13) 0.105(7) Uani 1 d . . 
H15A H 0.4722(14) 0.3828(17) 0.2943(13) 0.158 Uiso 1 calc R . 
H15B H 0.4884(14) 0.5004(17) 0.2707(13) 0.158 Uiso 1 calc R . 
H15C H 0.5707(14) 0.4454(17) 0.1984(13) 0.158 Uiso 1 calc R . 
C16 C 0.4993(12) 0.6412(12) 0.0610(11) 0.088(6) Uani 1 d . . 
H16A H 0.4782(12) 0.6900(12) 0.0099(11) 0.133 Uiso 1 calc R . 
H16B H 0.5756(12) 0.6157(12) 0.0337(11) 0.133 Uiso 1 calc R . 
H16C H 0.5006(12) 0.6735(12) 0.1060(11) 0.133 Uiso 1 calc R . 
C17 C 0.2975(15) 0.6130(12) -0.0062(9) 0.083(5) Uani 1 d . . 
H17A H 0.3484(15) 0.6723(12) -0.0334(9) 0.125 Uiso 1 calc R . 
H17B H 0.2172(15) 0.6337(12) 0.0102(9) 0.125 Uiso 1 calc R . 
H17C H 0.3150(15) 0.5779(12) -0.0530(9) 0.125 Uiso 1 calc R . 
C18 C 0.1654(15) 0.3996(12) 0.1329(13) 0.090(5) Uani 1 d . . 
H18A H 0.1415(15) 0.3356(12) 0.1843(13) 0.134 Uiso 1 calc R . 
H18B H 0.1951(15) 0.3879(12) 0.0713(13) 0.134 Uiso 1 calc R . 
H18C H 0.0992(15) 0.4433(12) 0.1360(13) 0.134 Uiso 1 calc R . 
C19 C 0.2843(18) 0.2986(9) 0.2856(12) 0.095(6) Uani 1 d . . 
H19A H 0.3338(18) 0.2851(9) 0.3232(12) 0.143 Uiso 1 calc R . 
H19B H 0.2972(18) 0.2488(9) 0.2529(12) 0.143 Uiso 1 calc R . 
H19C H 0.2036(18) 0.2950(9) 0.3278(12) 0.143 Uiso 1 calc R . 
C20 C -0.3313(9) 1.0784(9) 0.3308(8) 0.047(3) Uani 1 d . . 
C21 C -0.3279(10) 0.9909(9) 0.4073(8) 0.053(3) Uani 1 d . . 
C22 C -0.2516(9) 1.0145(8) 0.4474(7) 0.042(2) Uani 1 d . . 
C23 C -0.2117(10) 1.1151(7) 0.3986(7) 0.043(2) Uani 1 d . . 
C24 C -0.2575(9) 1.1561(8) 0.3228(8) 0.046(2) Uani 1 d . . 
C25 C -0.4148(11) 1.0950(14) 0.2774(11) 0.081(5) Uani 1 d . . 
H25A H -0.3991(11) 1.1609(14) 0.2283(11) 0.122 Uiso 1 calc R . 
H25B H -0.4941(11) 1.0915(14) 0.3224(11) 0.122 Uiso 1 calc R . 
H25C H -0.4046(11) 1.0430(14) 0.2474(11) 0.122 Uiso 1 calc R . 
C26 C -0.3979(12) 0.8944(12) 0.4463(10) 0.078(4) Uani 1 d . . 
H26A H -0.3776(12) 0.8475(12) 0.4987(10) 0.118 Uiso 1 calc R . 
H26B H -0.3814(12) 0.8648(12) 0.3957(10) 0.118 Uiso 1 calc R . 
H26C H -0.4800(12) 0.9085(12) 0.4698(10) 0.118 Uiso 1 calc R . 
C27 C -0.2286(13) 0.9437(11) 0.5360(8) 0.069(4) Uani 1 d . . 
H27A H -0.2659(13) 0.8783(11) 0.5557(8) 0.104 Uiso 1 calc R . 
H27B H -0.2599(13) 0.9723(11) 0.5880(8) 0.104 Uiso 1 calc R . 
H27C H -0.1456(13) 0.9356(11) 0.5203(8) 0.104 Uiso 1 calc R . 
C28 C -0.1353(12) 1.1740(10) 0.4197(10) 0.063(3) Uani 1 d . . 
H28A H -0.1217(12) 1.2420(10) 0.3741(10) 0.094 Uiso 1 calc R . 
H28B H -0.0617(12) 1.1408(10) 0.4140(10) 0.094 Uiso 1 calc R . 
H28C H -0.1735(12) 1.1771(10) 0.4845(10) 0.094 Uiso 1 calc R . 
C29 C -0.2375(13) 1.2620(9) 0.2513(10) 0.067(4) Uani 1 d . . 
H29A H -0.1840(13) 1.2991(9) 0.2612(10) 0.100 Uiso 1 calc R . 
H29B H -0.3108(13) 1.2963(9) 0.2604(10) 0.100 Uiso 1 calc R . 
H29C H -0.2048(13) 1.2585(9) 0.1864(10) 0.100 Uiso 1 calc R . 
C30 C 0.1445(10) 0.9945(9) 0.2720(8) 0.047(3) Uani 1 d . . 
C31 C 0.2473(11) 0.9448(11) 0.2797(10) 0.062(3) Uani 1 d . . 
H31A H 0.2412(11) 0.8845(11) 0.3307(10) 0.075 Uiso 1 calc R . 
C32 C 0.3578(12) 0.9830(13) 0.2137(12) 0.079(4) Uani 1 d . . 
H32A H 0.4254(12) 0.9490(13) 0.2189(12) 0.095 Uiso 1 calc R . 
C33 C 0.3636(12) 1.0770(15) 0.1369(13) 0.087(5) Uani 1 d . . 
H33A H 0.4363(12) 1.1063(15) 0.0927(13) 0.105 Uiso 1 calc R . 
C34 C 0.2667(10) 1.1222(10) 0.1284(10) 0.062(3) Uani 1 d . . 
H34A H 0.2730(10) 1.1817(10) 0.0767(10) 0.074 Uiso 1 calc R . 
C35 C 0.1540(9) 1.0838(8) 0.1949(7) 0.041(2) Uani 1 d . . 
C40 C -0.2297(9) 0.8504(8) 0.2257(7) 0.045(2) Uani 1 d . . 
C41 C -0.2409(8) 0.9408(8) 0.1574(7) 0.041(2) Uani 1 d . . 
C42 C -0.3153(10) 0.9433(11) 0.1078(9) 0.058(3) Uani 1 d . . 
H42A H -0.3248(10) 1.0035(11) 0.0622(9) 0.070 Uiso 1 calc R . 
C43 C -0.3765(10) 0.8514(13) 0.1288(10) 0.067(4) Uani 1 d . . 
H43A H -0.4274(10) 0.8513(13) 0.0973(10) 0.081 Uiso 1 calc R . 
C44 C -0.3602(14) 0.7626(13) 0.1957(11) 0.080(4) Uani 1 d . . 
H44A H -0.3991(14) 0.7027(13) 0.2080(11) 0.096 Uiso 1 calc R . 
C45 C -0.2894(13) 0.7612(12) 0.2432(11) 0.074(4) Uani 1 d . . 
H45A H -0.2796(13) 0.7006(12) 0.2882(11) 0.088 Uiso 1 calc R . 
C50 C 0.3389(9) 0.6320(9) 0.3887(8) 0.048(3) Uani 1 d . . 
C51 C 0.2904(10) 0.5357(11) 0.4521(8) 0.056(3) Uani 1 d . . 
C52 C 0.3026(12) 0.4981(13) 0.5417(9) 0.074(4) Uani 1 d . . 
H52A H 0.2685(12) 0.4352(13) 0.5851(9) 0.089 Uiso 1 calc R . 
C53 C 0.3651(13) 0.5537(17) 0.5664(11) 0.095(6) Uani 1 d . . 
H53A H 0.3769(13) 0.5259(17) 0.6251(11) 0.114 Uiso 1 calc R . 
C54 C 0.4117(12) 0.6512(15) 0.5057(11) 0.085(5) Uani 1 d . . 
H54A H 0.4507(12) 0.6900(15) 0.5242(11) 0.102 Uiso 1 calc R . 
C55 C 0.3974(11) 0.6875(11) 0.4170(9) 0.062(3) Uani 1 d . . 
H55A H 0.4285(11) 0.7519(11) 0.3750(9) 0.074 Uiso 1 calc R . 
C60 C -0.0170(9) 0.5584(8) 0.2247(8) 0.043(2) Uani 1 d . . 
C61 C -0.1075(10) 0.5162(9) 0.2124(9) 0.054(3) Uani 1 d . . 
H61A H -0.1449(10) 0.4556(9) 0.2584(9) 0.065 Uiso 1 calc R . 
C62 C -0.1417(12) 0.5618(11) 0.1350(11) 0.066(3) Uani 1 d . . 
H62A H -0.2019(12) 0.5327(11) 0.1286(11) 0.079 Uiso 1 calc R . 
C63 C -0.0853(12) 0.6526(11) 0.0656(9) 0.065(3) Uani 1 d . . 
H63A H -0.1064(12) 0.6831(11) 0.0115(9) 0.078 Uiso 1 calc R . 
C64 C 0.0018(11) 0.6975(9) 0.0768(8) 0.054(3) Uani 1 d . . 
H64A H 0.0373(11) 0.7591(9) 0.0315(8) 0.065 Uiso 1 calc R . 
C65 C 0.0361(9) 0.6504(7) 0.1557(7) 0.039(2) Uani 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 
Tl1 0.0597(3) 0.0649(3) 0.0594(3) -0.0319(3) -0.0161(3) 0.0077(2) 
Tl2 0.0502(3) 0.0512(3) 0.0447(2) -0.0222(2) -0.0083(2) 0.0025(2) 
Ti1 0.0359(9) 0.0323(8) 0.0290(8) -0.0100(6) -0.0108(7) 0.0003(7) 
Ti2 0.0303(8) 0.0355(8) 0.0317(8) -0.0118(7) -0.0102(7) 0.0021(7) 
S1 0.060(2) 0.0475(14) 0.0523(15) -0.0178(12) -0.0275(13) -0.0064(13) 
S2 0.071(2) 0.066(2) 0.0354(13) -0.0005(13) -0.0239(14) -0.020(2) 
S3 0.0444(14) 0.0322(11) 0.0498(14) -0.0100(10) -0.0215(12) 0.0014(10) 
S4 0.0426(14) 0.0460(14) 0.0354(12) -0.0052(11) -0.0108(11) -0.0096(12) 
S5 0.045(2) 0.0467(15) 0.061(2) -0.0008(13) -0.0228(13) -0.0091(12) 
S6 0.0433(14) 0.0531(15) 0.0478(14) -0.0054(12) -0.0238(12) -0.0015(12) 
S7 0.0461(14) 0.0352(12) 0.0442(13) -0.0122(10) -0.0132(11) 0.0014(11) 
S8 0.0388(13) 0.0468(13) 0.0346(12) -0.0111(10) -0.0115(10) -0.0026(11) 
C10 0.051(7) 0.070(8) 0.062(7) -0.038(7) -0.021(6) 0.030(6) 
C11 0.033(5) 0.072(7) 0.052(6) -0.043(6) 0.007(5) -0.002(5) 
C12 0.056(6) 0.056(6) 0.040(5) -0.027(5) -0.019(5) 0.008(5) 
C13 0.049(6) 0.043(6) 0.057(6) -0.030(5) -0.020(5) 0.006(5) 
C14 0.075(8) 0.033(5) 0.038(5) -0.009(4) -0.019(5) 0.018(5) 
C15 0.073(10) 0.187(20) 0.113(13) -0.101(15) -0.066(10) 0.071(12) 
C16 0.062(8) 0.108(12) 0.083(10) -0.061(9) 0.026(8) -0.043(8) 
C17 0.109(13) 0.092(11) 0.038(6) -0.024(7) -0.020(7) 0.035(10) 
C18 0.096(12) 0.091(11) 0.121(14) -0.073(11) -0.049(11) 0.009(9) 
C19 0.153(18) 0.035(6) 0.092(11) -0.013(7) -0.046(12) 0.005(9) 
C20 0.034(5) 0.060(7) 0.059(7) -0.042(6) -0.012(5) 0.011(5) 
C21 0.037(6) 0.061(7) 0.051(6) -0.028(6) 0.003(5) -0.001(5) 
C22 0.047(6) 0.050(6) 0.032(5) -0.017(4) -0.016(4) 0.009(5) 
C23 0.052(6) 0.036(5) 0.042(5) -0.014(4) -0.017(5) 0.002(5) 
C24 0.042(6) 0.045(6) 0.056(6) -0.023(5) -0.020(5) 0.015(5) 
C25 0.037(6) 0.139(14) 0.087(10) -0.064(10) -0.023(7) 0.019(8) 
C26 0.056(8) 0.094(10) 0.074(9) -0.039(8) 0.008(7) -0.028(8) 
C27 0.081(9) 0.073(8) 0.042(6) -0.009(6) -0.020(6) 0.011(7) 
C28 0.072(8) 0.062(7) 0.070(8) -0.035(6) -0.033(7) 0.004(6) 
C29 0.083(9) 0.048(7) 0.075(8) -0.026(6) -0.034(8) 0.022(7) 
C30 0.048(6) 0.057(6) 0.053(6) -0.027(5) -0.028(5) 0.004(5) 
C31 0.048(7) 0.081(9) 0.071(8) -0.041(7) -0.025(6) 0.022(6) 
C32 0.043(7) 0.106(12) 0.090(10) -0.049(10) -0.016(7) 0.028(8) 
C33 0.035(7) 0.132(15) 0.100(12) -0.066(12) -0.009(7) 0.020(8) 
C34 0.046(7) 0.069(8) 0.068(8) -0.031(6) -0.008(6) -0.005(6) 
C35 0.035(5) 0.054(6) 0.041(5) -0.026(5) -0.013(4) 0.001(4) 
C40 0.037(5) 0.054(6) 0.043(5) -0.026(5) -0.003(4) -0.006(5) 
C41 0.032(5) 0.056(6) 0.042(5) -0.031(5) -0.008(4) 0.001(4) 
C42 0.037(6) 0.096(9) 0.045(6) -0.033(6) -0.012(5) 0.009(6) 
C43 0.029(5) 0.127(13) 0.067(8) -0.063(9) -0.009(5) -0.014(7) 
C44 0.076(10) 0.095(11) 0.079(10) -0.041(9) -0.022(8) -0.017(9) 
C45 0.072(9) 0.076(9) 0.080(9) -0.040(8) -0.015(8) -0.022(7) 
C50 0.035(5) 0.070(7) 0.047(6) -0.035(6) -0.011(5) 0.004(5) 
C51 0.039(6) 0.093(9) 0.038(6) -0.021(6) -0.017(5) 0.004(6) 
C52 0.060(8) 0.117(12) 0.038(6) -0.008(7) -0.022(6) -0.009(8) 
C53 0.062(9) 0.187(20) 0.051(8) -0.051(11) -0.018(7) -0.020(11) 
C54 0.053(8) 0.157(16) 0.076(10) -0.067(11) -0.027(7) -0.012(9) 
C55 0.049(7) 0.092(9) 0.057(7) -0.046(7) -0.013(6) -0.002(6) 
C60 0.036(5) 0.050(6) 0.045(6) -0.018(5) -0.015(5) 0.002(5) 
C61 0.052(7) 0.060(7) 0.058(7) -0.019(6) -0.026(6) -0.003(5) 
C62 0.055(7) 0.077(9) 0.085(9) -0.032(8) -0.042(7) 0.006(7) 
C63 0.077(9) 0.079(9) 0.053(7) -0.011(6) -0.048(7) 0.002(7) 
C64 0.064(7) 0.054(6) 0.049(6) -0.018(5) -0.027(6) 0.006(6) 
C65 0.041(5) 0.037(5) 0.046(5) -0.013(4) -0.021(5) -0.004(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 
Tl1 S4 3.157(3) . ? 
Tl1 S3 3.296(3) . ? 
Tl1 S1 3.436(3) . ? 
Tl1 S2 3.518(4) . ? 
Tl1 Ti1 3.557(2) . ? 
Tl2 S8 3.148(3) . ? 
Tl2 S7 3.167(3) . ? 
Tl2 S5 3.412(3) . ? 
Tl2 Ti2 3.581(2) . ? 
Tl2 S6 3.910(3) . ? 
Ti1 C14 2.356(10) . ? 
Ti1 C10 2.366(10) . ? 
Ti1 C11 2.393(9) . ? 
Ti1 S1 2.418(3) . ? 
Ti1 C12 2.419(10) . ? 
Ti1 C13 2.422(9) . ? 
Ti1 S4 2.427(3) . ? 
Ti1 S2 2.436(3) . ? 
Ti1 S3 2.438(3) . ? 
Ti2 C22 2.353(9) . ? 
Ti2 C24 2.371(9) . ? 
Ti2 C23 2.377(9) . ? 
Ti2 C21 2.399(10) . ? 
Ti2 C20 2.400(10) . ? 
Ti2 S7 2.410(3) . ? 
Ti2 S5 2.421(3) . ? 
Ti2 S6 2.423(3) . ? 
Ti2 S8 2.480(3) . ? 
S1 C50 1.757(12) . ? 
S2 C51 1.759(12) . ? 
S3 C65 1.777(10) . ? 
S4 C60 1.763(11) . ? 
S5 C35 1.756(11) . ? 
S6 C30 1.743(12) . ? 
S7 C40 1.777(11) . ? 
S8 C41 1.773(10) . ? 
C10 C11 1.39(2) . ? 
C10 C14 1.43(2) . ? 
C10 C15 1.48(2) . ? 
C11 C12 1.42(2) . ? 
C11 C16 1.52(2) . ? 
C12 C13 1.37(2) . ? 
C12 C17 1.53(2) . ? 
C13 C14 1.40(2) . ? 
C13 C18 1.51(2) . ? 
C14 C19 1.50(2) . ? 
C20 C21 1.40(2) . ? 
C20 C24 1.42(2) . ? 
C20 C25 1.51(2) . ? 
C21 C22 1.42(2) . ? 
C21 C26 1.48(2) . ? 
C22 C23 1.386(15) . ? 
C22 C27 1.51(2) . ? 
C23 C24 1.43(2) . ? 
C23 C28 1.49(2) . ? 
C24 C29 1.50(2) . ? 
C30 C35 1.39(2) . ? 
C30 C31 1.40(2) . ? 
C31 C32 1.39(2) . ? 
C32 C33 1.44(2) . ? 
C33 C34 1.32(2) . ? 
C34 C35 1.41(2) . ? 
C40 C41 1.38(2) . ? 
C40 C45 1.40(2) . ? 
C41 C42 1.39(2) . ? 
C42 C43 1.43(2) . ? 
C43 C44 1.38(2) . ? 
C44 C45 1.33(2) . ? 
C50 C55 1.37(2) . ? 
C50 C51 1.40(2) . ? 
C51 C52 1.38(2) . ? 
C52 C53 1.37(2) . ? 
C53 C54 1.40(3) . ? 
C54 C55 1.38(2) . ? 
C60 C65 1.394(15) . ? 
C60 C61 1.41(2) . ? 
C61 C62 1.36(2) . ? 
C62 C63 1.40(2) . ? 
C63 C64 1.38(2) . ? 
C64 C65 1.39(2) . ? 
  
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 
S4 Tl1 S3 58.55(6) . . ? 
S4 Tl1 S1 82.22(6) . . ? 
S3 Tl1 S1 54.55(7) . . ? 
S4 Tl1 S2 54.38(7) . . ? 
S3 Tl1 S2 81.69(6) . . ? 
S1 Tl1 S2 53.65(7) . . ? 
S4 Tl1 Ti1 41.86(6) . . ? 
S3 Tl1 Ti1 41.45(5) . . ? 
S1 Tl1 Ti1 40.41(5) . . ? 
S2 Tl1 Ti1 40.27(5) . . ? 
S8 Tl2 S7 59.67(7) . . ? 
S8 Tl2 S5 57.80(7) . . ? 
S7 Tl2 S5 81.32(7) . . ? 
S8 Tl2 Ti2 42.64(5) . . ? 
S7 Tl2 Ti2 41.27(5) . . ? 
S5 Tl2 Ti2 40.41(6) . . ? 
S8 Tl2 S6 80.07(6) . . ? 
S7 Tl2 S6 50.35(7) . . ? 
S5 Tl2 S6 50.88(7) . . ? 
Ti2 Tl2 S6 37.42(5) . . ? 
C14 Ti1 C10 35.3(5) . . ? 
C14 Ti1 C11 56.9(4) . . ? 
C10 Ti1 C11 33.9(4) . . ? 
C14 Ti1 S1 129.2(4) . . ? 
C10 Ti1 S1 95.1(3) . . ? 
C11 Ti1 S1 88.3(3) . . ? 
C14 Ti1 C12 56.0(4) . . ? 
C10 Ti1 C12 56.7(4) . . ? 
C11 Ti1 C12 34.3(4) . . ? 
S1 Ti1 C12 114.9(3) . . ? 
C14 Ti1 C13 33.9(4) . . ? 
C10 Ti1 C13 57.0(4) . . ? 
C11 Ti1 C13 56.0(4) . . ? 
S1 Ti1 C13 144.2(3) . . ? 
C12 Ti1 C13 32.8(4) . . ? 
C14 Ti1 S4 98.0(3) . . ? 
C10 Ti1 S4 132.8(4) . . ? 
C11 Ti1 S4 143.2(3) . . ? 
S1 Ti1 S4 127.19(11) . . ? 
C12 Ti1 S4 110.6(3) . . ? 
C13 Ti1 S4 87.9(3) . . ? 
C14 Ti1 S2 88.5(3) . . ? 
C10 Ti1 S2 91.0(3) . . ? 
C11 Ti1 S2 122.5(3) . . ? 
S1 Ti1 S2 80.58(11) . . ? 
C12 Ti1 S2 143.9(3) . . ? 
C13 Ti1 S2 118.1(3) . . ? 
S4 Ti1 S2 78.19(11) . . ? 
C14 Ti1 S3 136.7(3) . . ? 
C10 Ti1 S3 133.2(3) . . ? 
C11 Ti1 S3 99.3(3) . . ? 
S1 Ti1 S3 78.96(11) . . ? 
C12 Ti1 S3 83.6(3) . . ? 
C13 Ti1 S3 103.2(3) . . ? 
S4 Ti1 S3 80.94(10) . . ? 
S2 Ti1 S3 132.44(12) . . ? 
C14 Ti1 Tl1 150.7(3) . . ? 
C10 Ti1 Tl1 154.6(3) . . ? 
C11 Ti1 Tl1 151.6(3) . . ? 
S1 Ti1 Tl1 67.10(8) . . ? 
C12 Ti1 Tl1 146.5(3) . . ? 
C13 Ti1 Tl1 146.2(3) . . ? 
S4 Ti1 Tl1 60.20(7) . . ? 
S2 Ti1 Tl1 68.99(9) . . ? 
S3 Ti1 Tl1 63.53(7) . . ? 
C22 Ti2 C24 57.6(4) . . ? 
C22 Ti2 C23 34.1(4) . . ? 
C24 Ti2 C23 34.9(4) . . ? 
C22 Ti2 C21 34.8(4) . . ? 
C24 Ti2 C21 57.6(4) . . ? 
C23 Ti2 C21 57.2(4) . . ? 
C22 Ti2 C20 57.0(4) . . ? 
C24 Ti2 C20 34.7(4) . . ? 
C23 Ti2 C20 57.2(4) . . ? 
C21 Ti2 C20 34.0(4) . . ? 
C22 Ti2 S7 103.6(3) . . ? 
C24 Ti2 S7 142.2(3) . . ? 
C23 Ti2 S7 137.7(3) . . ? 
C21 Ti2 S7 87.9(3) . . ? 
C20 Ti2 S7 107.7(3) . . ? 
C22 Ti2 S5 124.2(3) . . ? 
C24 Ti2 S5 89.5(3) . . ? 
C23 Ti2 S5 92.9(3) . . ? 
C21 Ti2 S5 146.6(3) . . ? 
C20 Ti2 S5 119.3(3) . . ? 
S7 Ti2 S5 125.34(12) . . ? 
C22 Ti2 S6 82.8(3) . . ? 
C24 Ti2 S6 124.3(3) . . ? 
C23 Ti2 S6 90.4(3) . . ? 
C21 Ti2 S6 110.2(3) . . ? 
C20 Ti2 S6 139.8(3) . . ? 
S7 Ti2 S6 79.32(11) . . ? 
S5 Ti2 S6 81.99(11) . . ? 
C22 Ti2 S8 137.8(3) . . ? 
C24 Ti2 S8 93.6(3) . . ? 
C23 Ti2 S8 128.5(3) . . ? 
C21 Ti2 S8 105.1(3) . . ? 
C20 Ti2 S8 81.5(3) . . ? 
S7 Ti2 S8 79.96(10) . . ? 
S5 Ti2 S8 80.88(11) . . ? 
S6 Ti2 S8 137.99(11) . . ? 
C22 Ti2 Tl2 157.2(3) . . ? 
C24 Ti2 Tl2 145.0(3) . . ? 
C23 Ti2 Tl2 157.3(3) . . ? 
C21 Ti2 Tl2 145.3(3) . . ? 
C20 Ti2 Tl2 139.9(3) . . ? 
S7 Ti2 Tl2 60.10(7) . . ? 
S5 Ti2 Tl2 66.04(8) . . ? 
S6 Ti2 Tl2 78.67(8) . . ? 
S8 Ti2 Tl2 59.32(7) . . ? 
C50 S1 Ti1 109.9(4) . . ? 
C50 S1 Tl1 84.9(3) . . ? 
Ti1 S1 Tl1 72.49(8) . . ? 
C51 S2 Ti1 109.6(4) . . ? 
C51 S2 Tl1 83.6(4) . . ? 
Ti1 S2 Tl1 70.74(9) . . ? 
C65 S3 Ti1 98.8(3) . . ? 
C65 S3 Tl1 100.7(3) . . ? 
Ti1 S3 Tl1 75.02(8) . . ? 
C60 S4 Ti1 99.0(4) . . ? 
C60 S4 Tl1 102.7(3) . . ? 
Ti1 S4 Tl1 77.94(8) . . ? 
C35 S5 Ti2 105.5(4) . . ? 
C35 S5 Tl2 67.9(3) . . ? 
Ti2 S5 Tl2 73.56(8) . . ? 
C30 S6 Ti2 104.1(4) . . ? 
C30 S6 Tl2 59.3(3) . . ? 
Ti2 S6 Tl2 63.91(7) . . ? 
C40 S7 Ti2 103.8(4) . . ? 
C40 S7 Tl2 94.2(3) . . ? 
Ti2 S7 Tl2 78.62(8) . . ? 
C41 S8 Ti2 101.6(4) . . ? 
C41 S8 Tl2 95.4(3) . . ? 
Ti2 S8 Tl2 78.04(8) . . ? 
C11 C10 C14 106.8(11) . . ? 
C11 C10 C15 126.5(15) . . ? 
C14 C10 C15 126.7(14) . . ? 
C11 C10 Ti1 74.1(6) . . ? 
C14 C10 Ti1 72.0(6) . . ? 
C15 C10 Ti1 119.6(8) . . ? 
C10 C11 C12 108.2(11) . . ? 
C10 C11 C16 127.2(13) . . ? 
C12 C11 C16 124.5(13) . . ? 
C10 C11 Ti1 72.0(6) . . ? 
C12 C11 Ti1 73.8(6) . . ? 
C16 C11 Ti1 123.6(7) . . ? 
C13 C12 C11 108.5(11) . . ? 
C13 C12 C17 126.8(12) . . ? 
C11 C12 C17 124.0(12) . . ? 
C13 C12 Ti1 73.7(6) . . ? 
C11 C12 Ti1 71.8(5) . . ? 
C17 C12 Ti1 128.0(8) . . ? 
C12 C13 C14 108.6(10) . . ? 
C12 C13 C18 127.1(12) . . ? 
C14 C13 C18 124.0(12) . . ? 
C12 C13 Ti1 73.5(5) . . ? 
C14 C13 Ti1 70.5(6) . . ? 
C18 C13 Ti1 127.0(8) . . ? 
C13 C14 C10 107.9(10) . . ? 
C13 C14 C19 126.3(13) . . ? 
C10 C14 C19 125.4(13) . . ? 
C13 C14 Ti1 75.6(5) . . ? 
C10 C14 Ti1 72.8(6) . . ? 
C19 C14 Ti1 122.8(9) . . ? 
C21 C20 C24 108.8(10) . . ? 
C21 C20 C25 125.8(12) . . ? 
C24 C20 C25 124.5(12) . . ? 
C21 C20 Ti2 73.0(6) . . ? 
C24 C20 Ti2 71.5(6) . . ? 
C25 C20 Ti2 129.8(7) . . ? 
C20 C21 C22 107.0(10) . . ? 
C20 C21 C26 127.4(13) . . ? 
C22 C21 C26 125.4(12) . . ? 
C20 C21 Ti2 73.0(6) . . ? 
C22 C21 Ti2 70.8(6) . . ? 
C26 C21 Ti2 125.4(8) . . ? 
C23 C22 C21 109.2(10) . . ? 
C23 C22 C27 125.9(11) . . ? 
C21 C22 C27 124.7(11) . . ? 
C23 C22 Ti2 73.9(6) . . ? 
C21 C22 Ti2 74.4(5) . . ? 
C27 C22 Ti2 122.9(7) . . ? 
C22 C23 C24 108.2(9) . . ? 
C22 C23 C28 127.6(10) . . ? 
C24 C23 C28 124.1(10) . . ? 
C22 C23 Ti2 72.0(5) . . ? 
C24 C23 Ti2 72.3(5) . . ? 
C28 C23 Ti2 122.1(8) . . ? 
C20 C24 C23 106.7(10) . . ? 
C20 C24 C29 126.1(11) . . ? 
C23 C24 C29 127.1(11) . . ? 
C20 C24 Ti2 73.7(5) . . ? 
C23 C24 Ti2 72.7(5) . . ? 
C29 C24 Ti2 121.1(8) . . ? 
C35 C30 C31 118.8(11) . . ? 
C35 C30 S6 121.9(8) . . ? 
C31 C30 S6 119.2(10) . . ? 
C32 C31 C30 122.0(14) . . ? 
C31 C32 C33 117.3(13) . . ? 
C34 C33 C32 120.5(15) . . ? 
C33 C34 C35 122.5(15) . . ? 
C30 C35 C34 118.8(11) . . ? 
C30 C35 S5 119.4(8) . . ? 
C34 C35 S5 121.8(9) . . ? 
C41 C40 C45 120.6(12) . . ? 
C41 C40 S7 119.4(8) . . ? 
C45 C40 S7 119.9(11) . . ? 
C40 C41 C42 119.5(10) . . ? 
C40 C41 S8 119.9(8) . . ? 
C42 C41 S8 120.6(10) . . ? 
C41 C42 C43 118.4(13) . . ? 
C44 C43 C42 120.0(12) . . ? 
C45 C44 C43 121.1(14) . . ? 
C44 C45 C40 120.4(16) . . ? 
C55 C50 C51 119.3(12) . . ? 
C55 C50 S1 120.8(10) . . ? 
C51 C50 S1 119.9(8) . . ? 
C52 C51 C50 119.4(12) . . ? 
C52 C51 S2 121.1(12) . . ? 
C50 C51 S2 119.4(9) . . ? 
C53 C52 C51 119.9(15) . . ? 
C52 C53 C54 121.7(14) . . ? 
C55 C54 C53 117.2(13) . . ? 
C50 C55 C54 122.3(14) . . ? 
C65 C60 C61 117.9(10) . . ? 
C65 C60 S4 121.0(8) . . ? 
C61 C60 S4 121.1(9) . . ? 
C62 C61 C60 121.8(12) . . ? 
C61 C62 C63 119.3(12) . . ? 
C64 C63 C62 120.3(11) . . ? 
C63 C64 C65 119.9(11) . . ? 
C64 C65 C60 120.7(10) . . ? 
C64 C65 S3 120.5(8) . . ? 
C60 C65 S3 118.7(8) . . ? 
  
_refine_diff_density_max    0.707 
_refine_diff_density_min   -0.891 
_refine_diff_density_rms    0.161 


#=END
 
data_7 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C61 H59 Cl6 N P2 S4 Ti' 
_chemical_formula_weight          1256.87 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
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' 
 'P'  'P'   0.1023   0.0942 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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                    11.473(3) 
_cell_length_b                    15.545(4) 
_cell_length_c                    16.778(6) 
_cell_angle_alpha                 89.08(2) 
_cell_angle_beta                  88.04(2) 
_cell_angle_gamma                 89.859(14) 
_cell_volume                      2990.2(15) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     160(2) 
_cell_measurement_reflns_used     27 
_cell_measurement_theta_min       3.58 
_cell_measurement_theta_max       13.16 
  
_exptl_crystal_description        needle 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.22 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.396 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1300 
_exptl_absorpt_coefficient_mu     0.644 
_exptl_absorpt_correction_type    'semi-empirical via \y scans'
_exptl_absorpt_correction_T_min   0.516
_exptl_absorpt_correction_T_max   0.621
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       160(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        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         8.5
_diffrn_reflns_number             12059 
_diffrn_reflns_av_R_equivalents   0.0681 
_diffrn_reflns_av_sigmaI/netI     0.1073 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        1 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.77 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              10398 
_reflns_number_observed           6296 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 21 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+6.0023P] 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          10377 
_refine_ls_number_parameters      676 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1267 
_refine_ls_R_factor_obs           0.0646 
_refine_ls_wR_factor_all          0.1893 
_refine_ls_wR_factor_obs          0.1451 
_refine_ls_goodness_of_fit_all    1.058 
_refine_ls_goodness_of_fit_obs    1.123 
_refine_ls_restrained_S_all       1.122 
_refine_ls_restrained_S_obs       1.123 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ti1 Ti 0.44238(8) 0.84551(6) 0.24746(6) 0.0197(2) Uani 1 d . . 
N1 N 0.9972(4) 0.4139(3) 0.2149(3) 0.0266(11) Uani 1 d . . 
P1 P 0.89000(11) 0.47723(9) 0.20372(9) 0.0202(3) Uani 1 d . . 
P2 P 1.02865(11) 0.31540(9) 0.21040(9) 0.0203(3) Uani 1 d . . 
S1 S 0.53822(13) 0.72766(10) 0.17742(9) 0.0285(3) Uani 1 d . . 
S2 S 0.44040(14) 0.74258(10) 0.35715(9) 0.0311(4) Uani 1 d . . 
S3 S 0.24417(12) 0.86112(10) 0.29822(9) 0.0262(3) Uani 1 d . . 
S4 S 0.34249(12) 0.85991(10) 0.12142(9) 0.0258(3) Uani 1 d . . 
C10 C 0.6325(5) 0.8968(4) 0.2758(4) 0.0278(13) Uani 1 d . . 
C11 C 0.5563(5) 0.9265(4) 0.3375(4) 0.0294(14) Uani 1 d . . 
C12 C 0.4759(5) 0.9843(4) 0.3027(4) 0.0271(13) Uani 1 d . . 
C13 C 0.5016(5) 0.9907(4) 0.2205(4) 0.0250(13) Uani 1 d . . 
C14 C 0.5994(5) 0.9358(4) 0.2025(4) 0.0264(13) Uani 1 d . . 
C15 C 0.7368(5) 0.8400(5) 0.2869(5) 0.046(2) Uani 1 d . . 
H15A H 0.7748(5) 0.8288(5) 0.2349(5) 0.069 Uiso 1 calc R . 
H15B H 0.7119(5) 0.7855(5) 0.3121(5) 0.069 Uiso 1 calc R . 
H15C H 0.7919(5) 0.8687(5) 0.3210(5) 0.069 Uiso 1 calc R . 
C16 C 0.5659(6) 0.9072(5) 0.4258(4) 0.044(2) Uani 1 d . . 
H16A H 0.5020(6) 0.9357(5) 0.4554(4) 0.066 Uiso 1 calc R . 
H16B H 0.6407(6) 0.9285(5) 0.4439(4) 0.066 Uiso 1 calc R . 
H16C H 0.5612(6) 0.8449(5) 0.4353(4) 0.066 Uiso 1 calc R . 
C17 C 0.3872(6) 1.0363(4) 0.3498(4) 0.040(2) Uani 1 d . . 
H17A H 0.3876(6) 1.0184(4) 0.4061(4) 0.061 Uiso 1 calc R . 
H17B H 0.3095(6) 1.0268(4) 0.3291(4) 0.061 Uiso 1 calc R . 
H17C H 0.4068(6) 1.0975(4) 0.3449(4) 0.061 Uiso 1 calc R . 
C18 C 0.4429(5) 1.0508(4) 0.1640(4) 0.0330(15) Uani 1 d . . 
H18A H 0.4760(5) 1.0431(4) 0.1100(4) 0.050 Uiso 1 calc R . 
H18B H 0.4549(5) 1.1103(4) 0.1804(4) 0.050 Uiso 1 calc R . 
H18C H 0.3591(5) 1.0384(4) 0.1647(4) 0.050 Uiso 1 calc R . 
C19 C 0.6589(5) 0.9230(4) 0.1226(4) 0.038(2) Uani 1 d . . 
H19A H 0.6189(5) 0.9571(4) 0.0821(4) 0.057 Uiso 1 calc R . 
H19B H 0.6563(5) 0.8620(4) 0.1090(4) 0.057 Uiso 1 calc R . 
H19C H 0.7403(5) 0.9416(4) 0.1245(4) 0.057 Uiso 1 calc R . 
C20 C 0.4610(5) 0.6422(4) 0.2236(3) 0.0246(13) Uani 1 d . . 
C21 C 0.4481(5) 0.5638(4) 0.1845(4) 0.0313(14) Uani 1 d . . 
H21 H 0.4793(5) 0.5579(4) 0.1317(4) 0.038 Uiso 1 calc R . 
C22 C 0.3913(6) 0.4958(4) 0.2213(5) 0.045(2) Uani 1 d . . 
H22 H 0.3832(6) 0.4433(4) 0.1938(5) 0.054 Uiso 1 calc R . 
C23 C 0.3453(6) 0.5032(4) 0.2989(5) 0.046(2) Uani 1 d . . 
H23 H 0.3057(6) 0.4559(4) 0.3241(5) 0.055 Uiso 1 calc R . 
C24 C 0.3571(5) 0.5786(4) 0.3387(4) 0.036(2) Uani 1 d . . 
H24 H 0.3252(5) 0.5835(4) 0.3914(4) 0.043 Uiso 1 calc R . 
C25 C 0.4160(5) 0.6490(4) 0.3024(3) 0.0260(13) Uani 1 d . . 
C30 C 0.1714(5) 0.9185(4) 0.2242(4) 0.0276(13) Uani 1 d . . 
C31 C 0.0645(5) 0.9600(4) 0.2412(4) 0.036(2) Uani 1 d . . 
H31 H 0.0325(5) 0.9589(4) 0.2942(4) 0.043 Uiso 1 calc R . 
C32 C 0.0060(6) 1.0022(4) 0.1822(5) 0.044(2) Uani 1 d . . 
H32 H -0.0669(6) 1.0287(4) 0.1947(5) 0.053 Uiso 1 calc R . 
C33 C 0.0512(6) 1.0066(4) 0.1056(5) 0.044(2) Uani 1 d . . 
H33 H 0.0106(6) 1.0373(4) 0.0657(5) 0.053 Uiso 1 calc R . 
C34 C 0.1561(6) 0.9664(4) 0.0863(4) 0.035(2) Uani 1 d . . 
H34 H 0.1870(6) 0.9693(4) 0.0331(4) 0.042 Uiso 1 calc R . 
C35 C 0.2171(5) 0.9211(4) 0.1451(4) 0.0259(13) Uani 1 d . . 
C40 C 0.7902(4) 0.4416(4) 0.1299(3) 0.0219(12) Uani 1 d . . 
C41 C 0.6838(5) 0.4052(4) 0.1530(4) 0.0316(14) Uani 1 d . . 
H41 H 0.6593(5) 0.4049(4) 0.2077(4) 0.038 Uiso 1 calc R . 
C42 C 0.6125(5) 0.3692(5) 0.0970(4) 0.038(2) Uani 1 d . . 
H42 H 0.5412(5) 0.3422(5) 0.1133(4) 0.046 Uiso 1 calc R . 
C43 C 0.6474(6) 0.3734(4) 0.0160(4) 0.036(2) Uani 1 d . . 
H43 H 0.5991(6) 0.3500(4) -0.0230(4) 0.043 Uiso 1 calc R . 
C44 C 0.7515(6) 0.4113(4) -0.0067(4) 0.037(2) Uani 1 d . . 
H44 H 0.7743(6) 0.4147(4) -0.0617(4) 0.044 Uiso 1 calc R . 
C45 C 0.8234(6) 0.4447(4) 0.0495(4) 0.0334(15) Uani 1 d . . 
H45 H 0.8959(6) 0.4698(4) 0.0332(4) 0.040 Uiso 1 calc R . 
C50 C 0.8055(4) 0.4905(4) 0.2958(3) 0.0241(13) Uani 1 d . . 
C51 C 0.8051(5) 0.4264(4) 0.3540(3) 0.0281(13) Uani 1 d . . 
H51 H 0.8509(5) 0.3761(4) 0.3456(3) 0.034 Uiso 1 calc R . 
C52 C 0.7399(5) 0.4341(4) 0.4235(4) 0.037(2) Uani 1 d . . 
H52 H 0.7392(5) 0.3891(4) 0.4626(4) 0.044 Uiso 1 calc R . 
C53 C 0.6743(5) 0.5091(5) 0.4362(4) 0.038(2) Uani 1 d . . 
H53 H 0.6299(5) 0.5155(5) 0.4846(4) 0.046 Uiso 1 calc R . 
C54 C 0.6738(5) 0.5723(4) 0.3802(4) 0.036(2) Uani 1 d . . 
H54 H 0.6285(5) 0.6226(4) 0.3893(4) 0.044 Uiso 1 calc R . 
C55 C 0.7400(5) 0.5642(4) 0.3082(4) 0.0333(15) Uani 1 d . . 
H55 H 0.7395(5) 0.6088(4) 0.2689(4) 0.040 Uiso 1 calc R . 
C60 C 0.9448(5) 0.5813(4) 0.1717(3) 0.0231(12) Uani 1 d . . 
C61 C 1.0579(5) 0.6055(4) 0.1905(4) 0.0323(14) Uani 1 d . . 
H61 H 1.1067(5) 0.5660(4) 0.2174(4) 0.039 Uiso 1 calc R . 
C62 C 1.0985(5) 0.6857(4) 0.1702(4) 0.036(2) Uani 1 d . . 
H62 H 1.1752(5) 0.7020(4) 0.1833(4) 0.043 Uiso 1 calc R . 
C63 C 1.0271(6) 0.7435(4) 0.1301(4) 0.040(2) Uani 1 d . . 
H63 H 1.0549(6) 0.7996(4) 0.1167(4) 0.048 Uiso 1 calc R . 
C64 C 0.9158(6) 0.7197(4) 0.1099(4) 0.036(2) Uani 1 d . . 
H64 H 0.8681(6) 0.7587(4) 0.0813(4) 0.044 Uiso 1 calc R . 
C65 C 0.8744(5) 0.6386(4) 0.1314(4) 0.0319(14) Uani 1 d . . 
H65 H 0.7976(5) 0.6223(4) 0.1186(4) 0.038 Uiso 1 calc R . 
C70 C 0.9120(4) 0.2462(3) 0.1795(4) 0.0233(13) Uani 1 d . . 
C71 C 0.8962(5) 0.2387(4) 0.0984(4) 0.0277(13) Uani 1 d . . 
H71 H 0.9497(5) 0.2646(4) 0.0608(4) 0.033 Uiso 1 calc R . 
C72 C 0.8010(6) 0.1926(4) 0.0726(5) 0.041(2) Uani 1 d . . 
H72 H 0.7883(6) 0.1880(4) 0.0171(5) 0.049 Uiso 1 calc R . 
C73 C 0.7253(6) 0.1539(4) 0.1273(5) 0.045(2) Uani 1 d . . 
H73 H 0.6608(6) 0.1222(4) 0.1093(5) 0.054 Uiso 1 calc R . 
C74 C 0.7419(5) 0.1605(4) 0.2073(5) 0.045(2) Uani 1 d . . 
H74 H 0.6895(5) 0.1328(4) 0.2445(5) 0.054 Uiso 1 calc R . 
C75 C 0.8363(5) 0.2080(4) 0.2346(4) 0.0311(14) Uani 1 d . . 
H75 H 0.8475(5) 0.2137(4) 0.2901(4) 0.037 Uiso 1 calc R . 
C80 C 1.0773(4) 0.2768(4) 0.3054(3) 0.0232(12) Uani 1 d . . 
C81 C 1.0934(5) 0.1894(4) 0.3208(4) 0.0325(14) Uani 1 d . . 
H81 H 1.0738(5) 0.1484(4) 0.2821(4) 0.039 Uiso 1 calc R . 
C82 C 1.1383(5) 0.1621(5) 0.3930(4) 0.039(2) Uani 1 d . . 
H82 H 1.1502(5) 0.1025(5) 0.4033(4) 0.047 Uiso 1 calc R . 
C83 C 1.1649(5) 0.2206(5) 0.4487(4) 0.044(2) Uani 1 d . . 
H83 H 1.1957(5) 0.2011(5) 0.4977(4) 0.053 Uiso 1 calc R . 
C84 C 1.1483(6) 0.3084(5) 0.4359(4) 0.043(2) Uani 1 d . . 
H84 H 1.1666(6) 0.3485(5) 0.4757(4) 0.051 Uiso 1 calc R . 
C85 C 1.1041(5) 0.3365(4) 0.3633(4) 0.0309(14) Uani 1 d . . 
H85 H 1.0922(5) 0.3962(4) 0.3534(4) 0.037 Uiso 1 calc R . 
C90 C 1.1479(4) 0.2995(4) 0.1383(3) 0.0243(13) Uani 1 d . . 
C91 C 1.2013(5) 0.3701(4) 0.1017(3) 0.0275(13) Uani 1 d . . 
H91 H 1.1751(5) 0.4265(4) 0.1137(3) 0.033 Uiso 1 calc R . 
C92 C 1.2945(5) 0.3578(4) 0.0467(4) 0.0338(15) Uani 1 d . . 
H92 H 1.3310(5) 0.4060(4) 0.0209(4) 0.041 Uiso 1 calc R . 
C93 C 1.3328(5) 0.2759(4) 0.0300(4) 0.0334(15) Uani 1 d . . 
H93 H 1.3971(5) 0.2677(4) -0.0063(4) 0.040 Uiso 1 calc R . 
C94 C 1.2780(5) 0.2051(5) 0.0661(4) 0.035(2) Uani 1 d . . 
H94 H 1.3034(5) 0.1486(5) 0.0533(4) 0.042 Uiso 1 calc R . 
C95 C 1.1865(5) 0.2170(4) 0.1205(4) 0.0293(14) Uani 1 d . . 
H95 H 1.1499(5) 0.1685(4) 0.1458(4) 0.035 Uiso 1 calc R . 
C100 C 0.5172(7) 0.3163(6) 0.3355(4) 0.054(2) Uani 1 d . . 
H10A H 0.5959(7) 0.2937(6) 0.3215(4) 0.065 Uiso 1 calc R . 
H10B H 0.5184(7) 0.3793(6) 0.3264(4) 0.065 Uiso 1 calc R . 
C101 C 0.0862(6) 0.6817(4) 0.3894(5) 0.050(2) Uani 1 d . . 
H10C H 0.1209(6) 0.7086(4) 0.4361(5) 0.060 Uiso 1 calc R . 
H10D H 0.1464(6) 0.6807(4) 0.3457(5) 0.060 Uiso 1 calc R . 
C102 C 0.8589(7) 0.1033(5) 0.4904(5) 0.055(2) Uani 1 d . . 
H10E H 0.8407(7) 0.0857(5) 0.5464(5) 0.067 Uiso 1 calc R . 
H10F H 0.9353(7) 0.1329(5) 0.4887(5) 0.067 Uiso 1 calc R . 
Cl1 Cl 0.4141(2) 0.26947(13) 0.27275(13) 0.0628(6) Uani 1 d . . 
Cl2 Cl 0.4841(2) 0.2940(2) 0.43760(13) 0.0690(6) Uani 1 d . . 
Cl3 Cl 0.0454(2) 0.57502(12) 0.41492(12) 0.0512(5) Uani 1 d . . 
Cl4 Cl -0.0319(2) 0.74369(13) 0.35924(12) 0.0529(5) Uani 1 d . . 
Cl5 Cl 0.7525(2) 0.1746(2) 0.45869(15) 0.0845(8) Uani 1 d . . 
Cl6 Cl 0.8694(2) 0.0114(2) 0.4318(2) 0.0782(7) Uani 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 
Ti1 0.0185(5) 0.0195(5) 0.0211(5) -0.0017(4) -0.0015(4) -0.0006(4) 
N1 0.019(2) 0.028(3) 0.033(3) -0.001(2) -0.005(2) 0.000(2) 
P1 0.0169(6) 0.0186(8) 0.0250(8) 0.0007(6) -0.0016(6) -0.0022(6) 
P2 0.0167(6) 0.0218(8) 0.0223(8) -0.0006(6) -0.0008(6) -0.0010(6) 
S1 0.0337(8) 0.0240(8) 0.0272(8) -0.0009(6) 0.0084(6) 0.0029(6) 
S2 0.0417(8) 0.0291(9) 0.0223(8) 0.0011(7) 0.0000(7) 0.0087(7) 
S3 0.0209(7) 0.0303(8) 0.0273(8) 0.0004(6) 0.0006(6) -0.0011(6) 
S4 0.0278(7) 0.0273(8) 0.0225(8) -0.0029(6) -0.0041(6) -0.0028(6) 
C10 0.022(3) 0.025(3) 0.037(4) -0.005(3) -0.006(3) 0.000(2) 
C11 0.027(3) 0.030(3) 0.031(3) -0.006(3) -0.008(3) -0.005(3) 
C12 0.022(3) 0.022(3) 0.038(4) -0.010(3) -0.002(3) -0.005(2) 
C13 0.021(3) 0.018(3) 0.037(4) 0.000(3) -0.008(2) -0.007(2) 
C14 0.021(3) 0.026(3) 0.033(3) -0.007(3) 0.003(2) -0.007(2) 
C15 0.024(3) 0.046(4) 0.068(5) -0.004(4) -0.016(3) 0.001(3) 
C16 0.051(4) 0.049(4) 0.033(4) -0.009(3) -0.012(3) -0.006(3) 
C17 0.039(4) 0.031(4) 0.051(4) -0.014(3) 0.007(3) -0.001(3) 
C18 0.028(3) 0.017(3) 0.054(4) 0.003(3) -0.001(3) -0.004(2) 
C19 0.035(3) 0.036(4) 0.043(4) -0.003(3) 0.010(3) -0.007(3) 
C20 0.023(3) 0.024(3) 0.026(3) 0.001(3) -0.004(2) 0.006(2) 
C21 0.041(3) 0.028(3) 0.025(3) -0.002(3) -0.010(3) 0.003(3) 
C22 0.055(4) 0.025(4) 0.055(5) -0.002(3) -0.023(4) -0.005(3) 
C23 0.043(4) 0.027(4) 0.066(5) 0.015(4) -0.004(4) -0.009(3) 
C24 0.029(3) 0.039(4) 0.038(4) 0.012(3) 0.009(3) 0.002(3) 
C25 0.021(3) 0.028(3) 0.029(3) 0.004(3) -0.003(2) 0.006(2) 
C30 0.029(3) 0.022(3) 0.033(4) -0.002(3) -0.011(3) -0.007(2) 
C31 0.020(3) 0.035(4) 0.053(4) -0.014(3) -0.004(3) -0.005(3) 
C32 0.033(3) 0.038(4) 0.064(5) -0.016(4) -0.022(4) 0.013(3) 
C33 0.049(4) 0.023(3) 0.064(5) -0.006(3) -0.036(4) 0.001(3) 
C34 0.047(4) 0.020(3) 0.040(4) -0.001(3) -0.019(3) 0.001(3) 
C35 0.027(3) 0.023(3) 0.029(3) -0.007(3) -0.007(2) -0.007(2) 
C40 0.021(3) 0.020(3) 0.025(3) 0.000(2) -0.003(2) 0.000(2) 
C41 0.026(3) 0.045(4) 0.023(3) -0.001(3) -0.001(3) -0.008(3) 
C42 0.025(3) 0.051(4) 0.040(4) -0.004(3) -0.006(3) -0.013(3) 
C43 0.040(4) 0.039(4) 0.030(4) -0.004(3) -0.013(3) -0.010(3) 
C44 0.046(4) 0.040(4) 0.024(3) -0.002(3) -0.001(3) -0.006(3) 
C45 0.039(3) 0.028(3) 0.033(4) -0.002(3) 0.007(3) -0.004(3) 
C50 0.015(2) 0.030(3) 0.027(3) -0.007(3) -0.005(2) -0.002(2) 
C51 0.029(3) 0.031(3) 0.025(3) 0.003(3) -0.004(3) 0.002(3) 
C52 0.039(3) 0.044(4) 0.026(3) 0.007(3) 0.001(3) 0.002(3) 
C53 0.031(3) 0.056(5) 0.027(4) -0.009(3) 0.001(3) 0.006(3) 
C54 0.028(3) 0.044(4) 0.037(4) -0.005(3) -0.003(3) 0.011(3) 
C55 0.029(3) 0.035(4) 0.036(4) -0.001(3) -0.002(3) 0.004(3) 
C60 0.025(3) 0.020(3) 0.024(3) -0.006(2) 0.002(2) -0.007(2) 
C61 0.027(3) 0.037(4) 0.033(4) -0.003(3) -0.004(3) -0.008(3) 
C62 0.031(3) 0.034(4) 0.042(4) -0.003(3) 0.000(3) -0.013(3) 
C63 0.061(4) 0.031(4) 0.029(4) 0.000(3) 0.006(3) -0.021(3) 
C64 0.048(4) 0.025(3) 0.036(4) -0.001(3) -0.007(3) 0.001(3) 
C65 0.029(3) 0.029(4) 0.037(4) 0.003(3) -0.006(3) -0.006(3) 
C70 0.020(3) 0.016(3) 0.034(3) -0.007(2) 0.001(2) 0.004(2) 
C71 0.027(3) 0.024(3) 0.032(4) -0.001(3) -0.003(3) -0.001(2) 
C72 0.040(4) 0.032(4) 0.053(5) -0.011(3) -0.016(3) 0.001(3) 
C73 0.030(3) 0.035(4) 0.070(6) -0.013(4) -0.008(3) -0.008(3) 
C74 0.023(3) 0.034(4) 0.076(6) 0.001(4) 0.009(3) -0.008(3) 
C75 0.024(3) 0.028(3) 0.041(4) -0.001(3) 0.001(3) 0.001(3) 
C80 0.017(2) 0.027(3) 0.025(3) 0.004(3) 0.002(2) 0.003(2) 
C81 0.030(3) 0.036(4) 0.031(4) 0.003(3) 0.008(3) 0.002(3) 
C82 0.037(3) 0.046(4) 0.034(4) 0.020(3) 0.008(3) 0.014(3) 
C83 0.028(3) 0.071(6) 0.032(4) 0.014(4) -0.001(3) 0.013(3) 
C84 0.035(3) 0.068(5) 0.026(4) -0.009(3) -0.006(3) -0.001(3) 
C85 0.024(3) 0.039(4) 0.031(3) -0.003(3) -0.003(3) 0.000(3) 
C90 0.019(3) 0.032(3) 0.022(3) -0.001(3) 0.001(2) -0.001(2) 
C91 0.027(3) 0.029(3) 0.027(3) 0.002(3) 0.000(2) -0.004(3) 
C92 0.027(3) 0.046(4) 0.029(3) 0.006(3) -0.002(3) -0.015(3) 
C93 0.023(3) 0.054(4) 0.023(3) -0.003(3) 0.001(2) 0.003(3) 
C94 0.032(3) 0.045(4) 0.026(3) -0.005(3) -0.001(3) 0.012(3) 
C95 0.029(3) 0.031(4) 0.028(3) 0.000(3) 0.002(3) 0.005(3) 
C100 0.048(4) 0.064(5) 0.049(5) 0.017(4) -0.002(4) -0.004(4) 
C101 0.038(4) 0.033(4) 0.079(6) 0.004(4) -0.015(4) 0.001(3) 
C102 0.057(5) 0.055(5) 0.054(5) -0.009(4) 0.004(4) -0.010(4) 
Cl1 0.091(2) 0.0408(11) 0.0572(13) 0.0009(10) -0.0078(11) -0.0101(11) 
Cl2 0.0685(13) 0.090(2) 0.0479(12) 0.0204(11) -0.0002(10) -0.0153(12) 
Cl3 0.0518(10) 0.0422(11) 0.0596(12) 0.0010(9) -0.0019(9) -0.0034(8) 
Cl4 0.0414(9) 0.0645(13) 0.0520(11) 0.0118(10) 0.0039(8) 0.0188(9) 
Cl5 0.100(2) 0.092(2) 0.0606(15) -0.0007(13) 0.0022(13) 0.032(2) 
Cl6 0.085(2) 0.0667(15) 0.083(2) -0.0263(13) 0.0097(13) -0.0103(13) 
  
_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 C14 2.381(6) . ? 
Ti1 C10 2.390(6) . ? 
Ti1 C13 2.390(6) . ? 
Ti1 C12 2.399(6) . ? 
Ti1 C11 2.404(6) . ? 
Ti1 S3 2.414(2) . ? 
Ti1 S2 2.419(2) . ? 
Ti1 S1 2.432(2) . ? 
Ti1 S4 2.446(2) . ? 
N1 P2 1.575(5) . ? 
N1 P1 1.588(5) . ? 
P1 C60 1.804(6) . ? 
P1 C40 1.809(6) . ? 
P1 C50 1.810(6) . ? 
P2 C80 1.800(6) . ? 
P2 C70 1.814(6) . ? 
P2 C90 1.814(5) . ? 
S1 C20 1.755(6) . ? 
S2 C25 1.761(6) . ? 
S3 C30 1.750(6) . ? 
S4 C35 1.760(6) . ? 
C10 C11 1.414(8) . ? 
C10 C14 1.426(9) . ? 
C10 C15 1.500(8) . ? 
C11 C12 1.418(8) . ? 
C11 C16 1.515(9) . ? 
C12 C13 1.403(8) . ? 
C12 C17 1.509(8) . ? 
C13 C14 1.435(8) . ? 
C13 C18 1.496(8) . ? 
C14 C19 1.499(8) . ? 
C20 C21 1.403(8) . ? 
C20 C25 1.408(8) . ? 
C21 C22 1.371(9) . ? 
C22 C23 1.394(10) . ? 
C23 C24 1.368(10) . ? 
C24 C25 1.407(8) . ? 
C30 C31 1.407(8) . ? 
C30 C35 1.411(8) . ? 
C31 C32 1.372(10) . ? 
C32 C33 1.369(11) . ? 
C33 C34 1.386(9) . ? 
C34 C35 1.407(8) . ? 
C40 C41 1.387(8) . ? 
C40 C45 1.389(8) . ? 
C41 C42 1.392(8) . ? 
C42 C43 1.404(9) . ? 
C43 C44 1.373(9) . ? 
C44 C45 1.383(9) . ? 
C50 C55 1.384(8) . ? 
C50 C51 1.384(8) . ? 
C51 C52 1.371(9) . ? 
C52 C53 1.402(9) . ? 
C53 C54 1.349(9) . ? 
C54 C55 1.411(9) . ? 
C60 C65 1.385(8) . ? 
C60 C61 1.400(8) . ? 
C61 C62 1.365(9) . ? 
C62 C63 1.396(10) . ? 
C63 C64 1.386(9) . ? 
C64 C65 1.386(9) . ? 
C70 C75 1.375(8) . ? 
C70 C71 1.386(8) . ? 
C71 C72 1.393(8) . ? 
C72 C73 1.374(10) . ? 
C73 C74 1.368(10) . ? 
C74 C75 1.407(9) . ? 
C80 C81 1.393(8) . ? 
C80 C85 1.397(8) . ? 
C81 C82 1.391(9) . ? 
C82 C83 1.357(10) . ? 
C83 C84 1.393(10) . ? 
C84 C85 1.398(9) . ? 
C90 C91 1.382(8) . ? 
C90 C95 1.391(8) . ? 
C91 C92 1.403(8) . ? 
C92 C93 1.376(9) . ? 
C93 C94 1.388(9) . ? 
C94 C95 1.381(8) . ? 
C100 Cl2 1.770(8) . ? 
C100 Cl1 1.775(8) . ? 
C101 Cl4 1.745(7) . ? 
C101 Cl3 1.765(7) . ? 
C102 Cl5 1.739(9) . ? 
C102 Cl6 1.747(8) . ? 
  
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 
C14 Ti1 C10 34.8(2) . . ? 
C14 Ti1 C13 35.0(2) . . ? 
C10 Ti1 C13 57.5(2) . . ? 
C14 Ti1 C12 57.4(2) . . ? 
C10 Ti1 C12 57.1(2) . . ? 
C13 Ti1 C12 34.1(2) . . ? 
C14 Ti1 C11 57.6(2) . . ? 
C10 Ti1 C11 34.3(2) . . ? 
C13 Ti1 C11 57.2(2) . . ? 
C12 Ti1 C11 34.4(2) . . ? 
C14 Ti1 S3 138.10(15) . . ? 
C10 Ti1 S3 138.6(2) . . ? 
C13 Ti1 S3 103.14(14) . . ? 
C12 Ti1 S3 86.05(14) . . ? 
C11 Ti1 S3 104.4(2) . . ? 
C14 Ti1 S2 127.5(2) . . ? 
C10 Ti1 S2 93.1(2) . . ? 
C13 Ti1 S2 138.6(2) . . ? 
C12 Ti1 S2 106.9(2) . . ? 
C11 Ti1 S2 82.0(2) . . ? 
S3 Ti1 S2 79.33(6) . . ? 
C14 Ti1 S1 88.15(14) . . ? 
C10 Ti1 S1 87.32(15) . . ? 
C13 Ti1 S1 120.22(15) . . ? 
C12 Ti1 S1 143.05(14) . . ? 
C11 Ti1 S1 117.63(15) . . ? 
S3 Ti1 S1 130.86(7) . . ? 
S2 Ti1 S1 82.33(6) . . ? 
C14 Ti1 S4 93.0(2) . . ? 
C10 Ti1 S4 127.2(2) . . ? 
C13 Ti1 S4 84.44(15) . . ? 
C12 Ti1 S4 110.5(2) . . ? 
C11 Ti1 S4 141.5(2) . . ? 
S3 Ti1 S4 80.41(6) . . ? 
S2 Ti1 S4 135.62(7) . . ? 
S1 Ti1 S4 81.84(6) . . ? 
P2 N1 P1 140.4(3) . . ? 
N1 P1 C60 108.8(3) . . ? 
N1 P1 C40 113.3(3) . . ? 
C60 P1 C40 107.6(3) . . ? 
N1 P1 C50 111.8(3) . . ? 
C60 P1 C50 108.2(3) . . ? 
C40 P1 C50 107.0(2) . . ? 
N1 P2 C80 110.1(3) . . ? 
N1 P2 C70 115.3(2) . . ? 
C80 P2 C70 108.4(3) . . ? 
N1 P2 C90 109.8(3) . . ? 
C80 P2 C90 107.1(2) . . ? 
C70 P2 C90 105.6(3) . . ? 
C20 S1 Ti1 98.3(2) . . ? 
C25 S2 Ti1 98.2(2) . . ? 
C30 S3 Ti1 105.5(2) . . ? 
C35 S4 Ti1 104.5(2) . . ? 
C11 C10 C14 108.5(5) . . ? 
C11 C10 C15 125.6(6) . . ? 
C14 C10 C15 125.7(6) . . ? 
C11 C10 Ti1 73.4(3) . . ? 
C14 C10 Ti1 72.3(3) . . ? 
C15 C10 Ti1 124.3(4) . . ? 
C10 C11 C12 107.7(5) . . ? 
C10 C11 C16 126.2(6) . . ? 
C12 C11 C16 125.9(6) . . ? 
C10 C11 Ti1 72.3(3) . . ? 
C12 C11 Ti1 72.6(3) . . ? 
C16 C11 Ti1 125.2(4) . . ? 
C13 C12 C11 108.7(5) . . ? 
C13 C12 C17 126.9(6) . . ? 
C11 C12 C17 124.1(6) . . ? 
C13 C12 Ti1 72.6(3) . . ? 
C11 C12 Ti1 73.0(3) . . ? 
C17 C12 Ti1 125.4(4) . . ? 
C12 C13 C14 108.1(5) . . ? 
C12 C13 C18 124.9(5) . . ? 
C14 C13 C18 126.8(6) . . ? 
C12 C13 Ti1 73.3(3) . . ? 
C14 C13 Ti1 72.2(3) . . ? 
C18 C13 Ti1 124.5(4) . . ? 
C10 C14 C13 107.0(5) . . ? 
C10 C14 C19 125.8(5) . . ? 
C13 C14 C19 127.2(6) . . ? 
C10 C14 Ti1 72.9(3) . . ? 
C13 C14 Ti1 72.8(3) . . ? 
C19 C14 Ti1 120.9(4) . . ? 
C21 C20 C25 118.4(6) . . ? 
C21 C20 S1 120.7(5) . . ? 
C25 C20 S1 120.7(4) . . ? 
C22 C21 C20 121.1(6) . . ? 
C21 C22 C23 120.3(6) . . ? 
C24 C23 C22 119.9(6) . . ? 
C23 C24 C25 120.7(6) . . ? 
C24 C25 C20 119.5(6) . . ? 
C24 C25 S2 120.1(5) . . ? 
C20 C25 S2 120.3(5) . . ? 
C31 C30 C35 118.5(6) . . ? 
C31 C30 S3 121.2(5) . . ? 
C35 C30 S3 120.3(4) . . ? 
C32 C31 C30 120.8(7) . . ? 
C33 C32 C31 121.0(6) . . ? 
C32 C33 C34 120.0(6) . . ? 
C33 C34 C35 120.4(7) . . ? 
C34 C35 C30 119.3(5) . . ? 
C34 C35 S4 121.9(5) . . ? 
C30 C35 S4 118.6(4) . . ? 
C41 C40 C45 119.3(5) . . ? 
C41 C40 P1 120.6(4) . . ? 
C45 C40 P1 120.0(4) . . ? 
C40 C41 C42 120.7(6) . . ? 
C41 C42 C43 119.1(6) . . ? 
C44 C43 C42 119.9(6) . . ? 
C43 C44 C45 120.6(6) . . ? 
C44 C45 C40 120.3(6) . . ? 
C55 C50 C51 119.6(6) . . ? 
C55 C50 P1 120.4(5) . . ? 
C51 C50 P1 120.1(4) . . ? 
C52 C51 C50 121.2(6) . . ? 
C51 C52 C53 119.1(6) . . ? 
C54 C53 C52 120.4(6) . . ? 
C53 C54 C55 120.6(6) . . ? 
C50 C55 C54 119.1(6) . . ? 
C65 C60 C61 119.8(6) . . ? 
C65 C60 P1 120.5(4) . . ? 
C61 C60 P1 119.7(5) . . ? 
C62 C61 C60 120.4(6) . . ? 
C61 C62 C63 119.8(6) . . ? 
C64 C63 C62 120.4(6) . . ? 
C63 C64 C65 119.6(6) . . ? 
C60 C65 C64 120.1(6) . . ? 
C75 C70 C71 121.1(5) . . ? 
C75 C70 P2 121.1(5) . . ? 
C71 C70 P2 117.6(4) . . ? 
C70 C71 C72 119.2(6) . . ? 
C73 C72 C71 120.0(7) . . ? 
C74 C73 C72 120.7(6) . . ? 
C73 C74 C75 120.2(6) . . ? 
C70 C75 C74 118.8(6) . . ? 
C81 C80 C85 119.6(6) . . ? 
C81 C80 P2 121.4(5) . . ? 
C85 C80 P2 118.9(4) . . ? 
C82 C81 C80 120.0(6) . . ? 
C83 C82 C81 120.1(6) . . ? 
C82 C83 C84 121.6(6) . . ? 
C83 C84 C85 118.8(6) . . ? 
C80 C85 C84 120.0(6) . . ? 
C91 C90 C95 120.0(5) . . ? 
C91 C90 P2 119.7(4) . . ? 
C95 C90 P2 120.3(4) . . ? 
C90 C91 C92 119.7(6) . . ? 
C93 C92 C91 119.9(6) . . ? 
C92 C93 C94 120.3(6) . . ? 
C95 C94 C93 119.9(6) . . ? 
C94 C95 C90 120.2(6) . . ? 
Cl2 C100 Cl1 111.9(4) . . ? 
Cl4 C101 Cl3 112.3(4) . . ? 
Cl5 C102 Cl6 112.7(5) . . ? 
  
_refine_diff_density_max    0.556 
_refine_diff_density_min   -0.551 
_refine_diff_density_rms    0.095