# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/2175
 
data_CC9902 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C54 H36 N3 F35 S7 Ti'
_chemical_formula_weight          1664.18 
_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'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0727   0.0534 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.3331   0.5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2191   1.8069 
 '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)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    9.9531(9) 
_cell_length_b                    31.429(2) 
_cell_length_c                    21.014(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.577(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      6571.2(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     183(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       11.10 
_cell_measurement_theta_max       27.89 
  
_exptl_crystal_description        'platy needles' 
_exptl_crystal_colour             'Deep red' 
_exptl_crystal_size_max           0.57 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.682 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              3320 
_exptl_absorpt_coefficient_mu     4.475 
_exptl_absorpt_correction_type    Empirical 
_exptl_absorpt_correction_T_min   0.2859 
_exptl_absorpt_correction_T_max   0.7312 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       183(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\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_%         ? 
_diffrn_reflns_number             10236 
_diffrn_reflns_av_R_equivalents   0.0313 
_diffrn_reflns_av_sigmaI/netI     0.0612 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -27 
_diffrn_reflns_limit_k_max        35 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.53 
_diffrn_reflns_theta_max          60.01 
_reflns_number_total              9610 
_reflns_number_observed           6536 
_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 940 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^)+(0.0751P)^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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00007(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          8670 
_refine_ls_number_parameters      902 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0933 
_refine_ls_R_factor_obs           0.0536 
_refine_ls_wR_factor_all          0.1477 
_refine_ls_wR_factor_obs          0.1227 
_refine_ls_goodness_of_fit_all    1.041 
_refine_ls_goodness_of_fit_obs    1.111 
_refine_ls_restrained_S_all       1.080 
_refine_ls_restrained_S_obs       1.111 
_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 
Ti Ti 0.25003(8) 0.72281(3) 0.85231(3) 0.0350(2) Uani 1 d . . 
S1 S 0.29968(11) 0.72203(4) 0.74189(5) 0.0371(3) Uani 1 d . . 
S2 S 0.17206(12) 0.72043(5) 0.95961(5) 0.0447(3) Uani 1 d . . 
S3 S 0.02119(13) 0.71742(6) 0.82294(6) 0.0558(4) Uani 1 d . . 
S4 S 0.36202(14) 0.65772(4) 0.87050(5) 0.0448(3) Uani 1 d . . 
S5 S 0.36624(14) 0.78545(5) 0.88173(5) 0.0498(3) Uani 1 d . . 
C1 C 0.1801(5) 0.7908(2) 0.6817(2) 0.0407(11) Uani 1 d . . 
F1 F 0.2756(4) 0.81560(11) 0.7096(2) 0.0630(9) Uani 1 d . . 
C2 C 0.0904(6) 0.8104(2) 0.6394(2) 0.0531(15) Uani 1 d . . 
F2 F 0.1005(5) 0.85229(12) 0.6273(2) 0.0801(11) Uani 1 d . . 
C3 C -0.0074(6) 0.7868(2) 0.6085(2) 0.0534(15) Uani 1 d . . 
F3 F -0.0933(4) 0.80555(15) 0.5680(2) 0.0782(12) Uani 1 d . . 
C4 C -0.0131(6) 0.7446(2) 0.6199(2) 0.0569(15) Uani 1 d . . 
F4 F -0.1074(4) 0.7206(2) 0.5898(2) 0.0842(12) Uani 1 d . . 
C5 C 0.0781(5) 0.7251(2) 0.6617(2) 0.0456(12) Uani 1 d . . 
F5 F 0.0692(4) 0.68305(11) 0.6697(2) 0.0696(10) Uani 1 d . . 
C6 C 0.1776(5) 0.7482(2) 0.6941(2) 0.0333(10) Uani 1 d . . 
C7 C 0.3907(5) 0.7149(2) 1.0427(2) 0.0423(12) Uani 1 d . . 
F7 F 0.4016(4) 0.67399(11) 1.0266(2) 0.0739(11) Uani 1 d . . 
C8 C 0.4829(5) 0.7309(2) 1.0867(2) 0.0516(15) Uani 1 d . . 
F8 F 0.5803(4) 0.7057(2) 1.1115(2) 0.0901(14) Uani 1 d . . 
C9 C 0.4804(6) 0.7722(2) 1.1031(2) 0.061(2) Uani 1 d . . 
F9 F 0.5735(4) 0.7885(2) 1.1435(2) 0.097(2) Uani 1 d . . 
C10 C 0.3830(8) 0.7981(2) 1.0778(3) 0.063(2) Uani 1 d . . 
F10 F 0.3754(7) 0.83905(14) 1.0934(2) 0.112(2) Uani 1 d . . 
C11 C 0.2883(6) 0.7817(2) 1.0352(2) 0.0464(12) Uani 1 d . . 
F11 F 0.1892(5) 0.80685(13) 1.0133(2) 0.0824(13) Uani 1 d . . 
C12 C 0.2923(5) 0.7403(2) 1.0150(2) 0.0352(10) Uani 1 d . . 
C13 C -0.0722(6) 0.7939(2) 0.8681(3) 0.0542(14) Uani 1 d . . 
F13 F 0.0143(5) 0.8128(2) 0.8292(2) 0.0935(14) Uani 1 d . . 
C14 C -0.1538(7) 0.8194(2) 0.9030(3) 0.070(2) Uani 1 d . . 
F14 F -0.1475(6) 0.8619(2) 0.8979(3) 0.116(2) Uani 1 d . . 
C15 C -0.2429(7) 0.8013(3) 0.9433(3) 0.071(2) Uani 1 d . . 
F15 F -0.3241(5) 0.8253(2) 0.9779(2) 0.122(2) Uani 1 d . . 
C16 C -0.2509(6) 0.7576(3) 0.9477(3) 0.061(2) Uani 1 d . . 
F16 F -0.3372(4) 0.7395(2) 0.9862(2) 0.106(2) Uani 1 d . . 
C17 C -0.1679(5) 0.7328(2) 0.9110(2) 0.0477(13) Uani 1 d . . 
F17 F -0.1793(4) 0.69080(13) 0.9167(2) 0.0747(10) Uani 1 d . . 
C18 C -0.0760(5) 0.7503(2) 0.8712(2) 0.0406(11) Uani 1 d . . 
C19 C 0.2946(6) 0.6179(2) 0.7575(3) 0.0497(13) Uani 1 d . . 
F19 F 0.1665(3) 0.62202(11) 0.7746(2) 0.0571(8) Uani 1 d . . 
C20 C 0.3178(7) 0.5988(2) 0.7004(3) 0.059(2) Uani 1 d . . 
F20 F 0.2162(5) 0.58494(13) 0.6632(2) 0.0851(12) Uani 1 d . . 
C21 C 0.4453(8) 0.5941(2) 0.6805(3) 0.068(2) Uani 1 d . . 
F21 F 0.4725(6) 0.57643(14) 0.6247(2) 0.102(2) Uani 1 d . . 
C22 C 0.5498(7) 0.6088(2) 0.7187(3) 0.070(2) Uani 1 d . . 
F22 F 0.6776(5) 0.6047(2) 0.7000(2) 0.108(2) Uani 1 d . . 
C23 C 0.5259(6) 0.6280(2) 0.7763(3) 0.0537(14) Uani 1 d . . 
F23 F 0.6306(4) 0.64142(15) 0.8126(2) 0.0783(11) Uani 1 d . . 
C24 C 0.3963(5) 0.6337(2) 0.7975(2) 0.0417(11) Uani 1 d . . 
C25 C 0.5783(5) 0.7722(2) 0.7994(2) 0.0402(11) Uani 1 d . . 
F25 F 0.5764(3) 0.73068(10) 0.81620(14) 0.0508(7) Uani 1 d . . 
C26 C 0.6754(5) 0.7848(2) 0.7582(2) 0.0455(12) Uani 1 d . . 
F26 F 0.7606(3) 0.75666(13) 0.7346(2) 0.0635(9) Uani 1 d . . 
C27 C 0.6832(6) 0.8271(2) 0.7420(2) 0.057(2) Uani 1 d . . 
F27 F 0.7784(4) 0.83956(14) 0.7017(2) 0.0768(11) Uani 1 d . . 
C28 C 0.5972(7) 0.8556(2) 0.7674(3) 0.058(2) Uani 1 d . . 
F28 F 0.6059(5) 0.89695(13) 0.7516(2) 0.0917(14) Uani 1 d . . 
C29 C 0.4991(6) 0.8422(2) 0.8072(2) 0.0524(14) Uani 1 d . . 
F29 F 0.4146(5) 0.87165(12) 0.8294(2) 0.0797(12) Uani 1 d . . 
C30 C 0.4872(5) 0.8000(2) 0.8260(2) 0.0406(11) Uani 1 d . . 
S6 S 0.04255(13) 0.48111(4) 0.89887(5) 0.0434(3) Uani 1 d . . 
C41 C 0.2942(6) 0.5090(2) 0.8693(2) 0.0461(12) Uani 1 d . . 
F41 F 0.2410(3) 0.54797(10) 0.8609(2) 0.0567(8) Uani 1 d . . 
C42 C 0.4310(6) 0.5050(2) 0.8606(2) 0.0529(14) Uani 1 d . . 
F42 F 0.5042(4) 0.53869(13) 0.8440(2) 0.0712(10) Uani 1 d . . 
C43 C 0.4897(6) 0.4659(2) 0.8675(3) 0.060(2) Uani 1 d . . 
F43 F 0.6232(4) 0.4617(2) 0.8570(2) 0.0845(12) Uani 1 d . . 
C44 C 0.4149(7) 0.4314(2) 0.8836(3) 0.061(2) Uani 1 d . . 
F44 F 0.4727(5) 0.39331(14) 0.8898(2) 0.0869(13) Uani 1 d . . 
C45 C 0.2794(7) 0.4360(2) 0.8929(2) 0.0531(14) Uani 1 d . . 
F45 F 0.2092(4) 0.40169(10) 0.9092(2) 0.0642(9) Uani 1 d . . 
C46 C 0.2144(5) 0.4751(2) 0.8867(2) 0.0404(11) Uani 1 d . . 
S7 S 0.05485(12) 0.48563(4) 0.60782(5) 0.0394(3) Uani 1 d . . 
C51 C 0.3034(5) 0.4858(2) 0.6697(2) 0.0379(11) Uani 1 d . . 
F51 F 0.2402(3) 0.49579(12) 0.72360(12) 0.0550(8) Uani 1 d . . 
C52 C 0.4418(5) 0.4830(2) 0.6737(2) 0.0432(12) Uani 1 d . . 
F52 F 0.5094(3) 0.49044(13) 0.72811(14) 0.0633(9) Uani 1 d . . 
C53 C 0.5114(5) 0.4725(2) 0.6204(2) 0.0462(12) Uani 1 d . . 
F53 F 0.6471(3) 0.47088(14) 0.6234(2) 0.0697(10) Uani 1 d . . 
C54 C 0.4430(6) 0.4650(2) 0.5644(3) 0.0544(14) Uani 1 d . . 
F54 F 0.5101(4) 0.4551(2) 0.5116(2) 0.0810(13) Uani 1 d . . 
C55 C 0.3058(5) 0.4694(2) 0.5616(2) 0.0476(13) Uani 1 d . . 
F55 F 0.2440(3) 0.46382(14) 0.50419(14) 0.0704(11) Uani 1 d . . 
C56 C 0.2297(5) 0.4798(2) 0.6133(2) 0.0356(10) Uani 1 d . . 
N60 N 0.0431(4) 0.57264(14) 0.5201(2) 0.0405(9) Uani 1 d . . 
H60A H 0.0423(4) 0.55169(14) 0.5493(2) 0.049 Uiso 1 calc R . 
H60B H -0.0148(4) 0.56538(14) 0.4883(2) 0.049 Uiso 1 calc R . 
C61 C 0.1807(5) 0.5758(2) 0.4943(3) 0.0542(14) Uani 1 d . . 
H61A H 0.2113(5) 0.5470(2) 0.4818(3) 0.065 Uiso 1 calc R . 
H61B H 0.2434(5) 0.5865(2) 0.5280(3) 0.065 Uiso 1 calc R . 
C62 C 0.1849(7) 0.6048(2) 0.4377(3) 0.071(2) Uani 1 d . . 
H62A H 0.2767(7) 0.6060(2) 0.4222(3) 0.106 Uiso 1 calc R . 
H62B H 0.1563(7) 0.6334(2) 0.4501(3) 0.106 Uiso 1 calc R . 
H62C H 0.1243(7) 0.5939(2) 0.4039(3) 0.106 Uiso 1 calc R . 
C63 C -0.0048(6) 0.6127(2) 0.5500(3) 0.0508(13) Uani 1 d . . 
H63A H -0.0226(6) 0.6341(2) 0.5163(3) 0.061 Uiso 1 calc R . 
H63B H 0.0671(6) 0.6240(2) 0.5788(3) 0.061 Uiso 1 calc R . 
C64 C -0.1294(7) 0.6065(2) 0.5870(3) 0.069(2) Uani 1 d . . 
H64A H -0.1565(7) 0.6336(2) 0.6055(3) 0.103 Uiso 1 calc R . 
H64B H -0.1119(7) 0.5857(2) 0.6211(3) 0.103 Uiso 1 calc R . 
H64C H -0.2017(7) 0.5959(2) 0.5586(3) 0.103 Uiso 1 calc R . 
N70 N -0.0602(4) 0.48039(14) 0.7517(2) 0.0406(9) Uani 1 d . . 
H70A H -0.0049(4) 0.48300(14) 0.7187(2) 0.049 Uiso 1 calc R . 
H70B H -0.0088(4) 0.48049(14) 0.7876(2) 0.049 Uiso 1 calc R . 
C71 C -0.1287(6) 0.4384(2) 0.7465(3) 0.0546(14) Uani 1 d . . 
H71A H -0.1856(6) 0.4376(2) 0.7071(3) 0.066 Uiso 1 calc R . 
H71B H -0.1876(6) 0.4345(2) 0.7833(3) 0.066 Uiso 1 calc R . 
C72 C -0.0279(9) 0.4035(2) 0.7452(3) 0.077(2) Uani 1 d . . 
H72A H -0.0744(9) 0.3760(2) 0.7418(3) 0.115 Uiso 1 calc R . 
H72B H 0.0276(9) 0.4041(2) 0.7845(3) 0.115 Uiso 1 calc R . 
H72C H 0.0296(9) 0.4072(2) 0.7085(3) 0.115 Uiso 1 calc R . 
C73 C -0.1495(5) 0.5184(2) 0.7525(3) 0.0514(13) Uani 1 d . . 
H73A H -0.2139(5) 0.5156(2) 0.7873(3) 0.062 Uiso 1 calc R . 
H73B H -0.2014(5) 0.5203(2) 0.7117(3) 0.062 Uiso 1 calc R . 
C74 C -0.0664(7) 0.5576(2) 0.7621(3) 0.065(2) Uani 1 d . . 
H74A H -0.1253(7) 0.5826(2) 0.7626(3) 0.097 Uiso 1 calc R . 
H74B H -0.0035(7) 0.5603(2) 0.7272(3) 0.097 Uiso 1 calc R . 
H74C H -0.0160(7) 0.5557(2) 0.8027(3) 0.097 Uiso 1 calc R . 
N80 N 0.0054(6) 0.57396(15) 0.9715(2) 0.0573(13) Uani 1 d . . 
H80A H 0.0255(6) 0.55210(15) 0.9458(2) 0.069 Uiso 1 calc R . 
H80B H -0.0163(6) 0.56300(15) 1.0094(2) 0.069 Uiso 1 calc R . 
C81 C 0.1274(9) 0.6011(2) 0.9805(3) 0.085(3) Uani 1 d . . 
H81A H 0.1565(9) 0.6115(2) 0.9386(3) 0.101 Uiso 1 calc R . 
H81B H 0.1050(9) 0.6262(2) 1.0067(3) 0.101 Uiso 1 calc R . 
C82 C 0.2390(9) 0.5770(3) 1.0123(4) 0.092(3) Uani 1 d . . 
H82A H 0.3177(9) 0.5956(3) 1.0176(4) 0.137 Uiso 1 calc R . 
H82B H 0.2622(9) 0.5525(3) 0.9860(4) 0.137 Uiso 1 calc R . 
H82C H 0.2108(9) 0.5672(3) 1.0541(4) 0.137 Uiso 1 calc R . 
C83 C -0.1138(9) 0.5967(2) 0.9439(3) 0.083(3) Uani 1 d . . 
H83A H -0.1390(9) 0.6200(2) 0.9730(3) 0.099 Uiso 1 calc R . 
H83B H -0.0897(9) 0.6096(2) 0.9028(3) 0.099 Uiso 1 calc R . 
C84 C -0.2314(9) 0.5681(3) 0.9334(4) 0.100(3) Uani 1 d . . 
H84A H -0.3071(9) 0.5844(3) 0.9153(4) 0.150 Uiso 1 calc R . 
H84B H -0.2570(9) 0.5556(3) 0.9741(4) 0.150 Uiso 1 calc R . 
H84C H -0.2077(9) 0.5453(3) 0.9039(4) 0.150 Uiso 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 
Ti 0.0329(4) 0.0395(5) 0.0327(4) 0.0026(3) 0.0011(3) -0.0027(4) 
S1 0.0378(6) 0.0406(7) 0.0328(5) 0.0020(4) -0.0006(4) 0.0043(5) 
S2 0.0366(6) 0.0632(8) 0.0344(5) 0.0027(5) 0.0012(4) -0.0077(6) 
S3 0.0353(7) 0.0852(11) 0.0467(6) -0.0150(6) -0.0032(5) 0.0029(7) 
S4 0.0515(7) 0.0390(7) 0.0437(6) 0.0071(5) -0.0007(5) 0.0018(6) 
S5 0.0589(8) 0.0500(8) 0.0411(6) -0.0094(5) 0.0114(5) -0.0151(7) 
C1 0.046(3) 0.040(3) 0.035(2) 0.000(2) -0.006(2) 0.002(2) 
F1 0.081(2) 0.042(2) 0.066(2) 0.0060(14) -0.018(2) -0.013(2) 
C2 0.073(4) 0.048(3) 0.039(2) 0.010(2) 0.007(3) 0.022(3) 
F2 0.119(3) 0.050(2) 0.071(2) 0.014(2) -0.008(2) 0.021(2) 
C3 0.051(3) 0.068(4) 0.040(2) 0.003(2) -0.001(2) 0.027(3) 
F3 0.071(2) 0.106(3) 0.057(2) 0.010(2) -0.013(2) 0.041(2) 
C4 0.044(3) 0.078(5) 0.048(3) -0.008(3) -0.009(2) 0.003(3) 
F4 0.065(2) 0.107(3) 0.078(2) 0.000(2) -0.036(2) -0.014(2) 
C5 0.044(3) 0.049(3) 0.043(2) 0.000(2) -0.004(2) 0.000(3) 
F5 0.081(2) 0.048(2) 0.078(2) 0.003(2) -0.029(2) -0.014(2) 
C6 0.033(2) 0.036(3) 0.030(2) -0.001(2) -0.001(2) 0.002(2) 
C7 0.047(3) 0.039(3) 0.042(2) 0.002(2) 0.001(2) 0.001(2) 
F7 0.109(3) 0.043(2) 0.069(2) 0.002(2) -0.020(2) 0.023(2) 
C8 0.040(3) 0.077(5) 0.038(2) 0.006(3) -0.002(2) 0.009(3) 
F8 0.070(2) 0.133(4) 0.066(2) 0.009(2) -0.020(2) 0.038(3) 
C9 0.055(3) 0.091(5) 0.036(2) -0.013(3) 0.003(2) -0.023(4) 
F9 0.077(3) 0.155(5) 0.058(2) -0.029(2) -0.006(2) -0.052(3) 
C10 0.103(5) 0.042(3) 0.045(3) -0.013(2) 0.012(3) -0.010(4) 
F10 0.200(6) 0.059(3) 0.076(2) -0.031(2) 0.003(3) -0.017(3) 
C11 0.063(3) 0.039(3) 0.037(2) 0.004(2) 0.000(2) 0.018(3) 
F11 0.122(3) 0.064(2) 0.061(2) -0.005(2) -0.003(2) 0.050(3) 
C12 0.035(2) 0.043(3) 0.028(2) 0.006(2) 0.003(2) 0.005(2) 
C13 0.050(3) 0.055(4) 0.057(3) 0.010(3) -0.003(3) -0.010(3) 
F13 0.088(3) 0.084(3) 0.109(3) 0.029(2) 0.014(2) -0.031(3) 
C14 0.069(4) 0.052(4) 0.086(4) -0.013(3) -0.024(4) -0.002(3) 
F14 0.126(4) 0.055(3) 0.166(5) -0.020(3) -0.030(4) 0.005(3) 
C15 0.049(4) 0.094(6) 0.068(4) -0.034(4) -0.013(3) 0.022(4) 
F15 0.081(3) 0.164(6) 0.119(4) -0.076(4) -0.009(3) 0.048(3) 
C16 0.039(3) 0.096(6) 0.048(3) 0.002(3) 0.010(2) 0.000(3) 
F16 0.064(2) 0.171(5) 0.084(3) 0.024(3) 0.037(2) -0.002(3) 
C17 0.038(3) 0.056(4) 0.048(3) 0.011(2) -0.004(2) 0.000(3) 
F17 0.065(2) 0.061(2) 0.098(3) 0.029(2) 0.004(2) -0.007(2) 
C18 0.029(2) 0.053(3) 0.040(2) 0.003(2) -0.002(2) -0.004(2) 
C19 0.062(4) 0.030(3) 0.057(3) 0.005(2) 0.006(3) 0.002(3) 
F19 0.048(2) 0.049(2) 0.074(2) -0.0034(15) 0.0016(15) -0.009(2) 
C20 0.091(5) 0.030(3) 0.055(3) -0.001(2) -0.002(3) 0.004(3) 
F20 0.132(4) 0.052(2) 0.070(2) -0.010(2) -0.015(2) -0.012(2) 
C21 0.104(6) 0.042(4) 0.058(3) 0.013(3) 0.015(4) 0.022(4) 
F21 0.181(5) 0.061(3) 0.067(2) 0.001(2) 0.043(3) 0.037(3) 
C22 0.070(4) 0.062(4) 0.080(4) 0.030(3) 0.038(4) 0.038(4) 
F22 0.087(3) 0.122(4) 0.117(3) 0.039(3) 0.050(3) 0.055(3) 
C23 0.041(3) 0.057(4) 0.063(3) 0.024(3) -0.001(3) 0.011(3) 
F23 0.045(2) 0.087(3) 0.103(3) 0.025(2) 0.000(2) 0.013(2) 
C24 0.045(3) 0.030(3) 0.050(2) 0.010(2) 0.004(2) 0.005(2) 
C25 0.039(3) 0.039(3) 0.042(2) 0.003(2) -0.011(2) -0.009(2) 
F25 0.050(2) 0.041(2) 0.061(2) 0.0083(13) -0.0064(13) 0.0002(14) 
C26 0.034(3) 0.060(4) 0.042(2) -0.003(2) -0.005(2) -0.003(3) 
F26 0.042(2) 0.082(3) 0.067(2) -0.007(2) 0.0027(14) 0.006(2) 
C27 0.056(3) 0.072(4) 0.044(3) -0.001(3) 0.006(2) -0.029(3) 
F27 0.076(2) 0.092(3) 0.064(2) -0.002(2) 0.021(2) -0.038(2) 
C28 0.082(4) 0.040(3) 0.053(3) -0.004(2) 0.004(3) -0.020(3) 
F28 0.147(4) 0.046(2) 0.083(2) 0.006(2) 0.025(3) -0.030(2) 
C29 0.069(4) 0.042(3) 0.046(3) -0.006(2) 0.006(3) -0.007(3) 
F29 0.117(3) 0.044(2) 0.080(2) -0.006(2) 0.033(2) 0.009(2) 
C30 0.044(3) 0.039(3) 0.039(2) -0.002(2) -0.004(2) -0.014(2) 
S6 0.0515(7) 0.0395(7) 0.0392(5) 0.0039(5) 0.0004(5) -0.0020(6) 
C41 0.058(3) 0.040(3) 0.041(2) 0.004(2) 0.000(2) 0.004(3) 
F41 0.067(2) 0.033(2) 0.071(2) 0.0095(14) 0.010(2) 0.002(2) 
C42 0.056(4) 0.053(4) 0.049(3) 0.010(2) 0.004(2) -0.002(3) 
F42 0.066(2) 0.061(2) 0.087(2) 0.017(2) 0.010(2) -0.016(2) 
C43 0.050(4) 0.072(4) 0.060(3) 0.009(3) 0.013(3) 0.010(3) 
F43 0.058(2) 0.098(3) 0.098(3) 0.024(2) 0.018(2) 0.021(2) 
C44 0.073(4) 0.048(4) 0.061(3) 0.012(3) 0.007(3) 0.029(3) 
F44 0.090(3) 0.060(3) 0.112(3) 0.020(2) 0.016(2) 0.032(2) 
C45 0.075(4) 0.035(3) 0.050(3) 0.001(2) 0.008(3) 0.004(3) 
F45 0.086(2) 0.032(2) 0.074(2) 0.0074(14) 0.012(2) -0.001(2) 
C46 0.057(3) 0.031(3) 0.033(2) 0.005(2) 0.000(2) 0.002(2) 
S7 0.0330(6) 0.0461(7) 0.0389(5) -0.0004(5) 0.0005(4) -0.0040(5) 
C51 0.039(3) 0.036(3) 0.039(2) 0.001(2) 0.003(2) 0.002(2) 
F51 0.047(2) 0.081(2) 0.0373(13) -0.0047(14) 0.0027(12) 0.003(2) 
C52 0.042(3) 0.043(3) 0.044(2) 0.002(2) -0.005(2) -0.001(2) 
F52 0.043(2) 0.097(3) 0.049(2) -0.005(2) -0.0130(13) 0.002(2) 
C53 0.036(3) 0.051(3) 0.051(3) -0.002(2) -0.001(2) 0.008(2) 
F53 0.033(2) 0.099(3) 0.077(2) -0.009(2) -0.0008(14) 0.009(2) 
C54 0.044(3) 0.067(4) 0.052(3) -0.017(3) 0.010(2) 0.001(3) 
F54 0.051(2) 0.130(4) 0.063(2) -0.030(2) 0.014(2) 0.009(2) 
C55 0.042(3) 0.060(4) 0.042(2) -0.011(2) 0.002(2) 0.001(3) 
F55 0.050(2) 0.116(3) 0.045(2) -0.028(2) 0.0001(13) -0.002(2) 
C56 0.033(2) 0.035(3) 0.039(2) -0.001(2) -0.001(2) -0.001(2) 
N60 0.035(2) 0.044(3) 0.042(2) 0.000(2) 0.000(2) -0.005(2) 
C61 0.039(3) 0.059(4) 0.065(3) -0.010(3) 0.011(2) -0.008(3) 
C62 0.088(5) 0.054(4) 0.073(4) -0.014(3) 0.041(3) -0.021(4) 
C63 0.055(3) 0.042(3) 0.056(3) -0.007(2) 0.011(2) -0.003(3) 
C64 0.065(4) 0.058(4) 0.085(4) -0.014(3) 0.034(3) -0.002(3) 
N70 0.034(2) 0.050(3) 0.038(2) 0.001(2) 0.005(2) 0.002(2) 
C71 0.059(4) 0.049(3) 0.056(3) -0.005(2) 0.006(3) -0.008(3) 
C72 0.111(6) 0.048(4) 0.073(4) 0.001(3) 0.015(4) 0.006(4) 
C73 0.040(3) 0.057(4) 0.057(3) -0.007(3) -0.005(2) 0.006(3) 
C74 0.072(4) 0.052(4) 0.069(3) 0.002(3) -0.015(3) 0.000(3) 
N80 0.092(4) 0.039(3) 0.042(2) 0.006(2) 0.014(2) 0.000(3) 
C81 0.136(7) 0.045(4) 0.074(4) -0.011(3) 0.030(5) -0.043(5) 
C82 0.095(6) 0.105(7) 0.075(4) -0.013(4) -0.002(4) -0.050(6) 
C83 0.133(7) 0.067(5) 0.049(3) 0.015(3) 0.009(4) 0.046(5) 
C84 0.094(6) 0.125(8) 0.079(5) -0.007(5) -0.019(4) 0.048(6) 
  
_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 S3 2.350(2) . ? 
Ti S4 2.356(2) . ? 
Ti S5 2.357(2) . ? 
Ti S1 2.3860(13) . ? 
Ti S2 2.4058(13) . ? 
S1 C6 1.760(5) . ? 
S2 C12 1.762(5) . ? 
S3 C18 1.757(5) . ? 
S4 C24 1.751(5) . ? 
S5 C30 1.763(5) . ? 
C1 F1 1.351(6) . ? 
C1 C6 1.364(7) . ? 
C1 C2 1.386(7) . ? 
C2 F2 1.345(7) . ? 
C2 C3 1.372(9) . ? 
C3 F3 1.328(6) . ? 
C3 C4 1.348(10) . ? 
C4 F4 1.349(7) . ? 
C4 C5 1.388(8) . ? 
C5 F5 1.336(7) . ? 
C5 C6 1.392(7) . ? 
C7 F7 1.334(6) . ? 
C7 C8 1.380(8) . ? 
C7 C12 1.381(7) . ? 
C8 F8 1.345(7) . ? 
C8 C9 1.344(10) . ? 
C9 F9 1.341(7) . ? 
C9 C10 1.363(10) . ? 
C10 F10 1.332(8) . ? 
C10 C11 1.381(9) . ? 
C11 F11 1.336(6) . ? 
C11 C12 1.369(8) . ? 
C13 F13 1.343(7) . ? 
C13 C14 1.368(10) . ? 
C13 C18 1.371(8) . ? 
C14 F14 1.344(9) . ? 
C14 C15 1.368(11) . ? 
C15 F15 1.337(7) . ? 
C15 C16 1.378(11) . ? 
C16 F16 1.325(7) . ? 
C16 C17 1.386(9) . ? 
C17 F17 1.329(7) . ? 
C17 C18 1.373(7) . ? 
C19 F19 1.341(7) . ? 
C19 C20 1.367(8) . ? 
C19 C24 1.391(8) . ? 
C20 F20 1.333(8) . ? 
C20 C21 1.355(10) . ? 
C21 F21 1.333(7) . ? 
C21 C22 1.375(11) . ? 
C22 F22 1.348(7) . ? 
C22 C23 1.379(10) . ? 
C23 F23 1.343(7) . ? 
C23 C24 1.389(8) . ? 
C25 F25 1.352(6) . ? 
C25 C26 1.374(7) . ? 
C25 C30 1.388(8) . ? 
C26 F26 1.330(6) . ? 
C26 C27 1.375(9) . ? 
C27 F27 1.345(6) . ? 
C27 C28 1.359(9) . ? 
C28 F28 1.344(7) . ? 
C28 C29 1.370(8) . ? 
C29 F29 1.344(7) . ? 
C29 C30 1.388(8) . ? 
S6 C46 1.746(6) . ? 
C41 F41 1.344(6) . ? 
C41 C42 1.385(8) . ? 
C41 C46 1.385(8) . ? 
C42 F42 1.337(7) . ? 
C42 C43 1.366(9) . ? 
C43 F43 1.359(7) . ? 
C43 C44 1.362(10) . ? 
C44 F44 1.333(7) . ? 
C44 C45 1.375(9) . ? 
C45 F45 1.334(7) . ? 
C45 C46 1.394(8) . ? 
S7 C56 1.751(5) . ? 
C51 F51 1.348(5) . ? 
C51 C52 1.380(7) . ? 
C51 C56 1.389(7) . ? 
C52 F52 1.331(6) . ? 
C52 C53 1.373(7) . ? 
C53 F53 1.352(6) . ? 
C53 C54 1.363(8) . ? 
C54 F54 1.347(6) . ? 
C54 C55 1.373(8) . ? 
C55 F55 1.350(6) . ? 
C55 C56 1.381(7) . ? 
N60 C61 1.491(6) . ? 
N60 C63 1.491(7) . ? 
C61 C62 1.499(9) . ? 
C63 C64 1.495(8) . ? 
N70 C71 1.487(7) . ? 
N70 C73 1.488(7) . ? 
C71 C72 1.489(9) . ? 
C73 C74 1.496(9) . ? 
N80 C83 1.489(9) . ? 
N80 C81 1.492(9) . ? 
C81 C82 1.487(12) . ? 
C83 C84 1.488(13) . ? 
  
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 
S3 Ti S4 115.52(7) . . ? 
S3 Ti S5 126.47(7) . . ? 
S4 Ti S5 117.14(6) . . ? 
S3 Ti S1 88.22(5) . . ? 
S4 Ti S1 92.24(5) . . ? 
S5 Ti S1 98.65(5) . . ? 
S3 Ti S2 84.76(5) . . ? 
S4 Ti S2 89.10(5) . . ? 
S5 Ti S2 87.07(5) . . ? 
S1 Ti S2 172.73(6) . . ? 
C6 S1 Ti 113.05(14) . . ? 
C12 S2 Ti 112.21(14) . . ? 
C18 S3 Ti 110.5(2) . . ? 
C24 S4 Ti 109.6(2) . . ? 
C30 S5 Ti 112.5(2) . . ? 
F1 C1 C6 119.9(4) . . ? 
F1 C1 C2 117.2(5) . . ? 
C6 C1 C2 122.9(5) . . ? 
F2 C2 C3 119.7(5) . . ? 
F2 C2 C1 120.3(6) . . ? 
C3 C2 C1 119.9(5) . . ? 
F3 C3 C4 121.4(6) . . ? 
F3 C3 C2 119.9(6) . . ? 
C4 C3 C2 118.7(5) . . ? 
C3 C4 F4 120.0(5) . . ? 
C3 C4 C5 121.1(6) . . ? 
F4 C4 C5 118.9(6) . . ? 
F5 C5 C4 118.2(5) . . ? 
F5 C5 C6 120.3(4) . . ? 
C4 C5 C6 121.6(6) . . ? 
C1 C6 C5 115.8(4) . . ? 
C1 C6 S1 123.6(4) . . ? 
C5 C6 S1 120.4(4) . . ? 
F7 C7 C8 117.7(5) . . ? 
F7 C7 C12 120.9(5) . . ? 
C8 C7 C12 121.5(5) . . ? 
F8 C8 C9 119.2(6) . . ? 
F8 C8 C7 120.2(6) . . ? 
C9 C8 C7 120.5(5) . . ? 
F9 C9 C8 120.9(7) . . ? 
F9 C9 C10 119.4(7) . . ? 
C8 C9 C10 119.6(5) . . ? 
F10 C10 C9 121.7(6) . . ? 
F10 C10 C11 118.6(7) . . ? 
C9 C10 C11 119.7(6) . . ? 
F11 C11 C12 118.8(5) . . ? 
F11 C11 C10 119.2(5) . . ? 
C12 C11 C10 122.0(5) . . ? 
C11 C12 C7 116.5(5) . . ? 
C11 C12 S2 121.2(4) . . ? 
C7 C12 S2 122.2(4) . . ? 
F13 C13 C14 117.8(6) . . ? 
F13 C13 C18 119.3(6) . . ? 
C14 C13 C18 122.9(6) . . ? 
F14 C14 C13 120.7(7) . . ? 
F14 C14 C15 119.8(7) . . ? 
C13 C14 C15 119.5(7) . . ? 
F15 C15 C14 121.0(8) . . ? 
F15 C15 C16 119.3(8) . . ? 
C14 C15 C16 119.7(6) . . ? 
F16 C16 C15 120.6(6) . . ? 
F16 C16 C17 120.2(7) . . ? 
C15 C16 C17 119.1(6) . . ? 
F17 C17 C18 120.9(5) . . ? 
F17 C17 C16 117.1(5) . . ? 
C18 C17 C16 122.0(6) . . ? 
C13 C18 C17 116.7(5) . . ? 
C13 C18 S3 123.0(4) . . ? 
C17 C18 S3 120.2(5) . . ? 
F19 C19 C20 117.6(6) . . ? 
F19 C19 C24 119.0(5) . . ? 
C20 C19 C24 123.4(6) . . ? 
F20 C20 C21 119.1(6) . . ? 
F20 C20 C19 120.9(6) . . ? 
C21 C20 C19 120.0(7) . . ? 
F21 C21 C20 122.1(8) . . ? 
F21 C21 C22 118.9(7) . . ? 
C20 C21 C22 119.0(6) . . ? 
F22 C22 C21 120.2(7) . . ? 
F22 C22 C23 118.9(8) . . ? 
C21 C22 C23 120.8(6) . . ? 
F23 C23 C22 119.2(6) . . ? 
F23 C23 C24 119.3(5) . . ? 
C22 C23 C24 121.6(6) . . ? 
C23 C24 C19 115.2(5) . . ? 
C23 C24 S4 122.9(4) . . ? 
C19 C24 S4 121.9(4) . . ? 
F25 C25 C26 117.2(5) . . ? 
F25 C25 C30 119.3(4) . . ? 
C26 C25 C30 123.4(5) . . ? 
F26 C26 C25 120.7(5) . . ? 
F26 C26 C27 120.6(5) . . ? 
C25 C26 C27 118.7(5) . . ? 
F27 C27 C28 121.1(6) . . ? 
F27 C27 C26 118.9(6) . . ? 
C28 C27 C26 120.0(5) . . ? 
F28 C28 C27 119.7(5) . . ? 
F28 C28 C29 120.0(6) . . ? 
C27 C28 C29 120.3(6) . . ? 
F29 C29 C28 117.6(5) . . ? 
F29 C29 C30 120.0(5) . . ? 
C28 C29 C30 122.4(6) . . ? 
C29 C30 C25 115.1(5) . . ? 
C29 C30 S5 120.2(4) . . ? 
C25 C30 S5 124.7(4) . . ? 
F41 C41 C42 116.8(5) . . ? 
F41 C41 C46 120.6(5) . . ? 
C42 C41 C46 122.5(5) . . ? 
F42 C42 C43 120.4(5) . . ? 
F42 C42 C41 120.4(5) . . ? 
C43 C42 C41 119.2(6) . . ? 
F43 C43 C44 120.5(6) . . ? 
F43 C43 C42 119.1(6) . . ? 
C44 C43 C42 120.4(6) . . ? 
F44 C44 C43 120.1(6) . . ? 
F44 C44 C45 120.1(6) . . ? 
C43 C44 C45 119.8(6) . . ? 
F45 C45 C44 118.4(5) . . ? 
F45 C45 C46 119.4(5) . . ? 
C44 C45 C46 122.2(6) . . ? 
C41 C46 C45 115.8(5) . . ? 
C41 C46 S6 121.7(4) . . ? 
C45 C46 S6 122.4(4) . . ? 
F51 C51 C52 116.9(4) . . ? 
F51 C51 C56 120.0(4) . . ? 
C52 C51 C56 123.1(4) . . ? 
F52 C52 C53 119.3(5) . . ? 
F52 C52 C51 121.4(4) . . ? 
C53 C52 C51 119.4(4) . . ? 
F53 C53 C54 120.6(4) . . ? 
F53 C53 C52 119.8(5) . . ? 
C54 C53 C52 119.6(5) . . ? 
F54 C54 C53 120.2(5) . . ? 
F54 C54 C55 120.2(5) . . ? 
C53 C54 C55 119.5(5) . . ? 
F55 C55 C54 117.0(4) . . ? 
F55 C55 C56 119.2(5) . . ? 
C54 C55 C56 123.8(5) . . ? 
C55 C56 C51 114.6(4) . . ? 
C55 C56 S7 122.5(4) . . ? 
C51 C56 S7 122.9(4) . . ? 
C61 N60 C63 113.9(4) . . ? 
N60 C61 C62 112.0(5) . . ? 
N60 C63 C64 112.8(5) . . ? 
C71 N70 C73 116.1(4) . . ? 
N70 C71 C72 110.4(5) . . ? 
N70 C73 C74 109.6(5) . . ? 
C83 N80 C81 114.3(6) . . ? 
C82 C81 N80 111.2(6) . . ? 
C84 C83 N80 112.6(6) . . ? 
  
_refine_diff_density_max    0.557 
_refine_diff_density_min   -0.320 
_refine_diff_density_rms    0.065 
  

 
data_CC0001 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C32 H22 N2 F20 S4 Ti'
_chemical_formula_weight          990.66 
_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'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0727   0.0534 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.3331   0.5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2191   1.8069 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    15.2002(12) 
_cell_length_b                    17.6154(12) 
_cell_length_c                    14.117(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.179(12) 
_cell_angle_gamma                 90.00 
_cell_volume                      3779.1(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     193(2) 
_cell_measurement_reflns_used     24 
_cell_measurement_theta_min       10.59 
_cell_measurement_theta_max       27.91 
  
_exptl_crystal_description        blocks 
_exptl_crystal_colour             'Deep red' 
_exptl_crystal_size_max           0.43 
_exptl_crystal_size_mid           0.37 
_exptl_crystal_size_min           0.23 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.741 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1976 
_exptl_absorpt_coefficient_mu     5.184 
_exptl_absorpt_correction_type    Ellipsoidal 
_exptl_absorpt_correction_T_min   0.0844 
_exptl_absorpt_correction_T_max   0.2352 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       193(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\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_%         ? 
_diffrn_reflns_number             3219 
_diffrn_reflns_av_R_equivalents   0.0494 
_diffrn_reflns_av_sigmaI/netI     0.0285 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          3.84 
_diffrn_reflns_theta_max          63.59 
_reflns_number_total              3093 
_reflns_number_observed           2598 
_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 114 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^)+(0.1123P)^2^+0.7417P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00018(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          2979 
_refine_ls_number_parameters      291 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0684 
_refine_ls_R_factor_obs           0.0552 
_refine_ls_wR_factor_all          0.1595 
_refine_ls_wR_factor_obs          0.1427 
_refine_ls_goodness_of_fit_all    1.061 
_refine_ls_goodness_of_fit_obs    1.088 
_refine_ls_restrained_S_all       1.108 
_refine_ls_restrained_S_obs       1.089 
_refine_ls_shift/esd_max          0.004 
_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 
Ti Ti 0.0000 0.26647(4) 0.7500 0.0400(3) Uani 1 d S . 
S1 S 0.06773(5) 0.33478(5) 0.88081(6) 0.0501(3) Uani 1 d . . 
S2 S 0.13183(5) 0.30423(5) 0.66804(6) 0.0476(3) Uani 1 d . . 
N N 0.0000 0.1615(2) 0.7500 0.0537(10) Uani 1 d S . 
C1 C 0.1836(2) 0.3362(2) 0.8813(2) 0.0475(7) Uani 1 d . . 
C2 C 0.2282(2) 0.4047(2) 0.8845(3) 0.0531(8) Uani 1 d . . 
F2 F 0.1826(2) 0.47029(15) 0.8793(2) 0.0713(7) Uani 1 d . . 
C3 C 0.3187(2) 0.4092(3) 0.8909(3) 0.0583(9) Uani 1 d . . 
F3 F 0.3596(2) 0.4767(2) 0.8901(2) 0.0816(8) Uani 1 d . . 
C4 C 0.3675(2) 0.3437(3) 0.8937(3) 0.0585(9) Uani 1 d . . 
F4 F 0.4554(2) 0.3480(2) 0.8990(2) 0.0848(9) Uani 1 d . . 
C5 C 0.3264(3) 0.2746(3) 0.8905(3) 0.0567(9) Uani 1 d . . 
F5 F 0.3736(2) 0.2108(2) 0.8926(2) 0.0770(8) Uani 1 d . . 
C6 C 0.2359(3) 0.2713(2) 0.8849(3) 0.0521(8) Uani 1 d . . 
F6 F 0.1980(2) 0.20315(14) 0.8822(2) 0.0665(6) Uani 1 d . . 
C7 C 0.1378(2) 0.2511(2) 0.5630(3) 0.0478(7) Uani 1 d . . 
C8 C 0.1754(2) 0.1784(2) 0.5616(3) 0.0491(7) Uani 1 d . . 
F8 F 0.2061(2) 0.14747(14) 0.6418(2) 0.0615(6) Uani 1 d . . 
C9 C 0.1831(2) 0.1374(2) 0.4781(3) 0.0556(8) Uani 1 d . . 
F9 F 0.2212(2) 0.0690(2) 0.4795(2) 0.0765(7) Uani 1 d . . 
C10 C 0.1537(2) 0.1676(3) 0.3947(3) 0.0582(9) Uani 1 d . . 
F10 F 0.1585(2) 0.1272(2) 0.3145(2) 0.0774(8) Uani 1 d . . 
C11 C 0.1194(2) 0.2398(3) 0.3924(3) 0.0577(9) Uani 1 d . . 
F11 F 0.0916(2) 0.2703(2) 0.3101(2) 0.0778(8) Uani 1 d . . 
C12 C 0.1127(2) 0.2806(2) 0.4753(3) 0.0523(8) Uani 1 d . . 
F12 F 0.0819(2) 0.3519(2) 0.4686(2) 0.0677(6) Uani 1 d . . 
C13 C 0.0166(3) 0.1183(2) 0.8371(3) 0.0574(9) Uani 1 d . . 
H13A H -0.0382(3) 0.0919(2) 0.8545(3) 0.069 Uiso 1 calc R . 
H13B H 0.0319(3) 0.1542(2) 0.8888(3) 0.069 Uiso 1 calc R . 
C14 C 0.0900(3) 0.0600(3) 0.8295(4) 0.0735(12) Uani 1 d . . 
H14A H 0.0974(3) 0.0334(3) 0.8901(4) 0.110 Uiso 1 calc R . 
H14B H 0.1450(3) 0.0857(3) 0.8140(4) 0.110 Uiso 1 calc R . 
H14C H 0.0748(3) 0.0233(3) 0.7796(4) 0.110 Uiso 1 calc R . 
N20 N -0.0080(17) 0.4920(5) 0.7684(16) 0.099(6) Uani 0.50 d PD -1 
H20A H -0.0452(17) 0.4638(5) 0.7300(16) 0.119 Uiso 0.50 calc PR -1 
H20B H 0.0354(17) 0.4599(5) 0.7910(16) 0.119 Uiso 0.50 calc PR -1 
C21 C -0.0579(12) 0.5198(18) 0.8488(14) 0.166(15) Uani 0.50 d PD -1 
H21A H -0.0300(12) 0.5674(18) 0.8713(14) 0.199 Uiso 0.50 calc PR -1 
H21B H -0.0516(12) 0.4822(18) 0.9007(14) 0.199 Uiso 0.50 calc PR -1 
C22 C -0.1529(10) 0.5347(9) 0.8333(13) 0.113(5) Uani 0.50 d PD -1 
H22A H -0.1784(10) 0.5530(9) 0.8923(13) 0.169 Uiso 0.50 calc PR -1 
H22B H -0.1825(10) 0.4877(9) 0.8135(13) 0.169 Uiso 0.50 calc PR -1 
H22C H -0.1609(10) 0.5732(9) 0.7838(13) 0.169 Uiso 0.50 calc PR -1 
C23 C 0.0334(14) 0.5506(6) 0.7101(11) 0.138(8) Uani 0.50 d PD -1 
H23A H 0.0725(14) 0.5820(6) 0.7511(11) 0.166 Uiso 0.50 calc PR -1 
H23B H -0.0130(14) 0.5842(6) 0.6833(11) 0.166 Uiso 0.50 calc PR -1 
C24 C 0.0863(13) 0.5184(11) 0.6301(13) 0.099(5) Uani 0.50 d PD -1 
H24A H 0.1121(13) 0.5601(11) 0.5940(13) 0.148 Uiso 0.50 calc PR -1 
H24B H 0.0477(13) 0.4883(11) 0.5882(13) 0.148 Uiso 0.50 calc PR -1 
H24C H 0.1333(13) 0.4861(11) 0.6561(13) 0.148 Uiso 0.50 calc PR -1 
  
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 0.0299(4) 0.0429(4) 0.0474(4) 0.000 0.0075(3) 0.000 
S1 0.0337(4) 0.0643(5) 0.0525(5) -0.0086(3) 0.0071(3) -0.0008(3) 
S2 0.0342(4) 0.0586(5) 0.0505(5) -0.0025(3) 0.0106(3) -0.0069(3) 
N 0.040(2) 0.044(2) 0.077(3) 0.000 0.018(2) 0.000 
C1 0.0342(15) 0.060(2) 0.048(2) -0.0058(14) 0.0046(12) 0.0031(13) 
C2 0.040(2) 0.058(2) 0.062(2) -0.007(2) 0.0106(14) 0.0029(14) 
F2 0.0501(12) 0.0591(13) 0.105(2) -0.0092(13) 0.0093(12) 0.0049(9) 
C3 0.042(2) 0.070(2) 0.063(2) -0.008(2) 0.0100(15) -0.011(2) 
F3 0.0538(13) 0.077(2) 0.115(2) -0.016(2) 0.0206(14) -0.0186(12) 
C4 0.032(2) 0.086(3) 0.058(2) -0.003(2) 0.0063(13) 0.003(2) 
F4 0.0328(11) 0.118(2) 0.103(2) -0.008(2) 0.0083(11) 0.0025(12) 
C5 0.045(2) 0.073(2) 0.052(2) 0.004(2) 0.0067(14) 0.014(2) 
F5 0.0628(15) 0.086(2) 0.082(2) 0.0117(14) 0.0047(12) 0.0291(13) 
C6 0.048(2) 0.061(2) 0.048(2) -0.0002(14) 0.0052(14) 0.0014(15) 
F6 0.0640(14) 0.0546(12) 0.081(2) 0.0015(11) 0.0073(11) -0.0014(10) 
C7 0.0307(13) 0.061(2) 0.053(2) 0.0007(14) 0.0116(12) -0.0092(13) 
C8 0.0372(15) 0.060(2) 0.051(2) 0.0022(14) 0.0123(13) -0.0075(13) 
F8 0.0587(12) 0.0666(13) 0.0595(12) 0.0062(10) 0.0106(9) 0.0051(10) 
C9 0.046(2) 0.057(2) 0.065(2) -0.005(2) 0.0197(15) -0.0106(15) 
F9 0.084(2) 0.0602(13) 0.087(2) -0.0067(12) 0.0274(14) 0.0014(12) 
C10 0.046(2) 0.077(2) 0.052(2) -0.013(2) 0.0151(14) -0.020(2) 
F10 0.075(2) 0.097(2) 0.0611(14) -0.0236(13) 0.0183(12) -0.0259(14) 
C11 0.040(2) 0.083(3) 0.050(2) 0.004(2) 0.0052(14) -0.016(2) 
F11 0.069(2) 0.113(2) 0.0512(12) 0.0089(13) 0.0019(11) -0.0016(14) 
C12 0.036(2) 0.068(2) 0.053(2) 0.004(2) 0.0094(13) -0.0040(14) 
F12 0.0605(13) 0.076(2) 0.0666(13) 0.0146(11) 0.0125(10) 0.0080(11) 
C13 0.050(2) 0.053(2) 0.070(2) 0.002(2) 0.015(2) 0.0029(15) 
C14 0.069(3) 0.064(2) 0.088(3) 0.007(2) 0.005(2) 0.014(2) 
N20 0.095(10) 0.083(5) 0.120(19) 0.002(6) -0.024(10) 0.020(7) 
C21 0.109(14) 0.091(14) 0.301(43) -0.040(20) 0.063(19) 0.003(12) 
C22 0.120(12) 0.087(8) 0.132(12) -0.005(8) 0.026(10) -0.009(8) 
C23 0.223(25) 0.038(5) 0.154(16) 0.007(6) -0.030(14) 0.018(8) 
C24 0.127(15) 0.058(7) 0.112(10) -0.011(7) 0.000(10) -0.004(9) 
  
_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 N 1.849(4) . ? 
Ti S1 2.4166(9) . ? 
Ti S1 2.4166(9) 2_556 ? 
Ti S2 2.4273(8) 2_556 ? 
Ti S2 2.4273(8) . ? 
S1 C1 1.761(3) . ? 
S2 C7 1.758(4) . ? 
N C13 1.463(5) 2_556 ? 
N C13 1.463(5) . ? 
C1 C2 1.384(5) . ? 
C1 C6 1.392(5) . ? 
C2 F2 1.349(5) . ? 
C2 C3 1.380(5) . ? 
C3 F3 1.342(5) . ? 
C3 C4 1.372(6) . ? 
C4 F4 1.338(4) . ? 
C4 C5 1.368(6) . ? 
C5 F5 1.332(5) . ? 
C5 C6 1.378(6) . ? 
C6 F6 1.332(5) . ? 
C7 C12 1.388(5) . ? 
C7 C8 1.403(5) . ? 
C8 F8 1.332(5) . ? 
C8 C9 1.389(5) . ? 
C9 F9 1.337(5) . ? 
C9 C10 1.360(6) . ? 
C10 F10 1.340(5) . ? 
C10 C11 1.376(7) . ? 
C11 F11 1.340(5) . ? 
C11 C12 1.379(6) . ? 
C12 F12 1.342(5) . ? 
C13 C14 1.522(6) . ? 
N20 C21 1.463(10) . ? 
N20 C23 1.470(9) . ? 
C21 C22 1.481(10) . ? 
C23 C24 1.510(10) . ? 
  
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 
N Ti S1 119.86(3) . . ? 
N Ti S1 119.86(3) . 2_556 ? 
S1 Ti S1 120.27(6) . 2_556 ? 
N Ti S2 105.90(3) . 2_556 ? 
S1 Ti S2 80.92(3) . 2_556 ? 
S1 Ti S2 83.39(3) 2_556 2_556 ? 
N Ti S2 105.90(3) . . ? 
S1 Ti S2 83.39(3) . . ? 
S1 Ti S2 80.92(3) 2_556 . ? 
S2 Ti S2 148.20(5) 2_556 . ? 
C1 S1 Ti 114.83(12) . . ? 
C7 S2 Ti 108.31(11) . . ? 
C13 N C13 117.3(4) 2_556 . ? 
C13 N Ti 121.3(2) 2_556 . ? 
C13 N Ti 121.3(2) . . ? 
C2 C1 C6 115.8(3) . . ? 
C2 C1 S1 120.1(3) . . ? 
C6 C1 S1 124.0(3) . . ? 
F2 C2 C3 117.7(4) . . ? 
F2 C2 C1 119.7(3) . . ? 
C3 C2 C1 122.7(4) . . ? 
F3 C3 C4 119.7(3) . . ? 
F3 C3 C2 120.8(4) . . ? 
C4 C3 C2 119.4(4) . . ? 
F4 C4 C5 120.5(4) . . ? 
F4 C4 C3 119.4(4) . . ? 
C5 C4 C3 120.1(3) . . ? 
F5 C5 C4 120.3(4) . . ? 
F5 C5 C6 120.2(4) . . ? 
C4 C5 C6 119.5(4) . . ? 
F6 C6 C5 118.0(4) . . ? 
F6 C6 C1 119.5(3) . . ? 
C5 C6 C1 122.5(4) . . ? 
C12 C7 C8 115.7(3) . . ? 
C12 C7 S2 122.3(3) . . ? 
C8 C7 S2 121.7(3) . . ? 
F8 C8 C9 118.3(4) . . ? 
F8 C8 C7 119.8(3) . . ? 
C9 C8 C7 121.9(4) . . ? 
F9 C9 C10 120.0(4) . . ? 
F9 C9 C8 120.1(4) . . ? 
C10 C9 C8 120.0(4) . . ? 
F10 C10 C9 120.1(4) . . ? 
F10 C10 C11 119.9(4) . . ? 
C9 C10 C11 120.0(4) . . ? 
F11 C11 C10 120.2(4) . . ? 
F11 C11 C12 120.0(4) . . ? 
C10 C11 C12 119.8(4) . . ? 
F12 C12 C11 117.3(4) . . ? 
F12 C12 C7 120.1(3) . . ? 
C11 C12 C7 122.6(4) . . ? 
N C13 C14 114.0(3) . . ? 
C21 N20 C23 115.7(15) . . ? 
N20 C21 C22 117.7(18) . . ? 
N20 C23 C24 113.3(10) . . ? 
  
_refine_diff_density_max    0.598 
_refine_diff_density_min   -0.378 
_refine_diff_density_rms    0.086