 
data_f60310a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H14 Cl N O2 Ti' 
_chemical_formula_weight          359.65 
 
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' 
 'O'  'O'   0.0106   0.0060 
 '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                    10.1760(19) 
_cell_length_b                    10.457(2) 
_cell_length_c                    15.517(3) 
_cell_angle_alpha                 107.959(3) 
_cell_angle_beta                  94.315(3) 
_cell_angle_gamma                 94.627(3) 
_cell_volume                      1557.0(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     619
_cell_measurement_theta_min       2.568 
_cell_measurement_theta_max       17.252
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.05 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.534 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              736 
_exptl_absorpt_coefficient_mu     0.729 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9645 
_exptl_absorpt_correction_T_max   0.9856 
_exptl_absorpt_process_details    sadabs
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6567 
_diffrn_reflns_av_R_equivalents   0.0505 
_diffrn_reflns_av_sigmaI/netI     0.3046 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.39 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              5410 
_reflns_number_gt                 1649 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0278P)²+0.0000P] where P=(Fo²+2Fc²)/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          5410 
_refine_ls_number_parameters      415 
_refine_ls_number_restraints      11 
_refine_ls_R_factor_all           0.1832 
_refine_ls_R_factor_gt            0.0573 
_refine_ls_wR_factor_ref          0.1073 
_refine_ls_wR_factor_gt           0.0906 
_refine_ls_goodness_of_fit_ref    0.673 
_refine_ls_restrained_S_all       0.727 
_refine_ls_shift/su_max           0.062 
_refine_ls_shift/su_mean          0.004 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ti1 Ti 0.45986(12) 0.78057(13) 0.08191(8) 0.0477(4) Uani 1 1 d . . . 
Ti2 Ti 0.78369(12) 0.78931(13) 0.47183(8) 0.0488(4) Uani 1 1 d . . . 
Cl1 Cl 0.32074(17) 0.8036(2) -0.03661(12) 0.0614(6) Uani 1 1 d . . . 
Cl2 Cl 0.81895(18) 0.66065(19) 0.32508(11) 0.0632(6) Uani 1 1 d . . . 
N1 N 0.5624(9) 0.6104(10) 0.1171(5) 0.129(4) Uani 1 1 d D . . 
N2 N 0.8924(7) 0.9312(8) 0.6030(5) 0.095(3) Uani 1 1 d D . . 
O1 O 0.3347(5) 0.6360(5) 0.0811(3) 0.0702(16) Uani 1 1 d . . . 
O2 O 0.6051(5) 0.7969(5) 0.0170(3) 0.0746(17) Uani 1 1 d . . . 
O3 O 0.9084(4) 0.6953(5) 0.5177(3) 0.0650(16) Uani 1 1 d . . . 
O4 O 0.7972(5) 0.9406(5) 0.4311(3) 0.0676(16) Uani 1 1 d . . . 
C1 C 0.3474(10) 0.5501(8) 0.1288(5) 0.056(2) Uani 1 1 d . . . 
C2 C 0.2437(8) 0.4851(8) 0.1558(5) 0.063(2) Uani 1 1 d . . . 
H2 H 0.1571 0.5010 0.1423 0.075 Uiso 1 1 calc R . . 
C3 C 0.2684(9) 0.3962(8) 0.2028(5) 0.066(3) Uani 1 1 d . . . 
H3 H 0.1975 0.3528 0.2211 0.079 Uiso 1 1 calc R . . 
C4 C 0.3946(10) 0.3696(8) 0.2238(5) 0.070(3) Uani 1 1 d . . . 
H4 H 0.4090 0.3098 0.2562 0.084 Uiso 1 1 calc R . . 
C5 C 0.4974(8) 0.4316(9) 0.1966(5) 0.067(2) Uani 1 1 d . . . 
H5 H 0.5834 0.4126 0.2085 0.080 Uiso 1 1 calc R . . 
C6 C 0.4742(10) 0.5236(8) 0.1507(5) 0.059(3) Uani 1 1 d D . . 
C7 C 0.6676(9) 0.6054(12) 0.1081(6) 0.138(6) Uani 1 1 d D . . 
H7 H 0.7030 0.5355 0.1239 0.165 Uiso 1 1 calc R . . 
C8 C 0.7633(9) 0.6877(9) 0.0757(5) 0.065(3) Uani 1 1 d D . . 
C9 C 0.8936(10) 0.6600(8) 0.0868(5) 0.075(3) Uani 1 1 d . . . 
H9 H 0.9138 0.5977 0.1162 0.090 Uiso 1 1 calc R . . 
C10 C 0.9914(8) 0.7230(9) 0.0550(5) 0.072(3) Uani 1 1 d . . . 
H10 H 1.0780 0.7017 0.0605 0.087 Uiso 1 1 calc R . . 
C11 C 0.9616(8) 0.8188(8) 0.0147(5) 0.058(2) Uani 1 1 d . . . 
H11 H 1.0287 0.8662 -0.0043 0.070 Uiso 1 1 calc R . . 
C12 C 0.8309(8) 0.8441(7) 0.0025(4) 0.052(2) Uani 1 1 d . . . 
H12 H 0.8112 0.9067 -0.0268 0.062 Uiso 1 1 calc R . . 
C13 C 0.7312(8) 0.7800(9) 0.0321(5) 0.054(2) Uani 1 1 d . . . 
C14 C 0.4135(10) 0.8684(8) 0.2334(5) 0.063(2) Uani 1 1 d . . . 
H14 H 0.3723 0.8140 0.2631 0.076 Uiso 1 1 calc R . . 
C15 C 0.5466(9) 0.8920(8) 0.2314(5) 0.063(2) Uani 1 1 d . . . 
H15 H 0.6124 0.8543 0.2574 0.075 Uiso 1 1 calc R . . 
C16 C 0.5657(8) 0.9832(8) 0.1834(5) 0.063(2) Uani 1 1 d . . . 
H16 H 0.6471 1.0192 0.1726 0.075 Uiso 1 1 calc R . . 
C17 C 0.4459(11) 1.0100(8) 0.1551(5) 0.065(2) Uani 1 1 d . . . 
H17 H 0.4307 1.0680 0.1213 0.077 Uiso 1 1 calc R . . 
C18 C 0.3504(8) 0.9385(10) 0.1841(6) 0.072(3) Uani 1 1 d . . . 
H18 H 0.2592 0.9375 0.1726 0.086 Uiso 1 1 calc R . . 
C19 C 0.9627(7) 0.7326(10) 0.6060(5) 0.051(2) Uani 1 1 d . . . 
C20 C 1.0231(7) 0.6420(7) 0.6414(6) 0.054(2) Uani 1 1 d . . . 
H20 H 1.0259 0.5527 0.6059 0.065 Uiso 1 1 calc R . . 
C21 C 1.0787(7) 0.6892(10) 0.7312(6) 0.064(3) Uani 1 1 d . . . 
H21 H 1.1163 0.6295 0.7569 0.077 Uiso 1 1 calc R . . 
C22 C 1.0795(8) 0.8214(10) 0.7830(5) 0.070(3) Uani 1 1 d . . . 
H22 H 1.1200 0.8515 0.8425 0.084 Uiso 1 1 calc R . . 
C23 C 1.0219(8) 0.9077(8) 0.7477(6) 0.069(3) Uani 1 1 d . . . 
H23 H 1.0219 0.9973 0.7833 0.083 Uiso 1 1 calc R . . 
C24 C 0.9628(7) 0.8651(11) 0.6593(6) 0.060(3) Uani 1 1 d D . . 
C25 C 0.8977(10) 1.0481(10) 0.6216(7) 0.115(5) Uani 1 1 d D . . 
H25 H 0.9473 1.0982 0.6761 0.138 Uiso 1 1 calc R . . 
C26 C 0.8347(8) 1.1254(11) 0.5685(7) 0.063(3) Uani 1 1 d D . . 
C27 C 0.8316(8) 1.2595(11) 0.6153(6) 0.072(3) Uani 1 1 d . . . 
H27 H 0.8644 1.2954 0.6764 0.086 Uiso 1 1 calc R . . 
C28 C 0.7784(8) 1.3397(8) 0.5690(7) 0.073(3) Uani 1 1 d . . . 
H28 H 0.7696 1.4295 0.6003 0.088 Uiso 1 1 calc R . . 
C29 C 0.7378(7) 1.2883(9) 0.4767(6) 0.064(2) Uani 1 1 d . . . 
H29 H 0.7065 1.3450 0.4458 0.077 Uiso 1 1 calc R . . 
C30 C 0.7433(7) 1.1550(9) 0.4309(5) 0.053(2) Uani 1 1 d . . . 
H30 H 0.7145 1.1204 0.3691 0.063 Uiso 1 1 calc R . . 
C31 C 0.7921(8) 1.0708(9) 0.4770(7) 0.057(2) Uani 1 1 d . . . 
C32 C 0.6294(9) 0.6635(14) 0.5288(13) 0.087(4) Uani 1 1 d D . . 
H32 H 0.6552 0.5947 0.5504 0.105 Uiso 1 1 calc R . . 
C33 C 0.6314(10) 0.7918(18) 0.5768(6) 0.099(4) Uani 1 1 d D . . 
H33 H 0.6616 0.8289 0.6383 0.118 Uiso 1 1 calc R . . 
C34 C 0.5846(12) 0.8594(11) 0.5250(14) 0.147(8) Uani 1 1 d D . . 
H34 H 0.5723 0.9507 0.5446 0.176 Uiso 1 1 calc R . . 
C35 C 0.5570(13) 0.775(2) 0.4387(10) 0.172(10) Uani 1 1 d D . . 
H35 H 0.5270 0.7973 0.3875 0.207 Uiso 1 1 calc R . . 
C36 C 0.5829(12) 0.6505(14) 0.4426(10) 0.126(6) Uani 1 1 d D . . 
H36 H 0.5705 0.5704 0.3940 0.151 Uiso 1 1 calc R . . 
 
 
_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 O2 1.876(5) . ? 
Ti1 O1 1.893(5) . ? 
Ti1 N1 2.316(9) . ? 
Ti1 C15 2.319(7) . ? 
Ti1 Cl1 2.320(2) . ? 
Ti1 C18 2.331(7) . ? 
Ti1 C16 2.334(7) . ? 
Ti1 C17 2.338(7) . ? 
Ti1 C14 2.344(7) . ? 
Ti2 O4 1.876(5) . ? 
Ti2 O3 1.892(4) . ? 
Ti2 N2 2.259(8) . ? 
Ti2 C35 2.308(13) . ? 
Ti2 C33 2.327(8) . ? 
Ti2 Cl2 2.331(2) . ? 
Ti2 C34 2.333(10) . ? 
Ti2 C36 2.337(10) . ? 
Ti2 C32 2.360(8) . ? 
N1 C7 1.093(7) . ? 
N1 C6 1.461(8) . ? 
N2 C25 1.162(7) . ? 
N2 C24 1.454(7) . ? 
O1 C1 1.336(8) . ? 
O2 C13 1.322(7) . ? 
O3 C19 1.362(7) . ? 
O4 C31 1.335(8) . ? 
C1 C2 1.370(9) . ? 
C1 C6 1.381(9) . ? 
C2 C3 1.374(9) . ? 
C3 C4 1.371(9) . ? 
C4 C5 1.349(9) . ? 
C5 C6 1.387(9) . ? 
C7 C8 1.465(9) . ? 
C8 C13 1.385(10) . ? 
C8 C9 1.389(9) . ? 
C9 C10 1.356(9) . ? 
C10 C11 1.376(9) . ? 
C11 C12 1.388(8) . ? 
C12 C13 1.357(9) . ? 
C14 C15 1.362(9) . ? 
C14 C18 1.372(9) . ? 
C15 C16 1.391(9) . ? 
C16 C17 1.344(9) . ? 
C17 C18 1.365(9) . ? 
C19 C24 1.377(10) . ? 
C19 C20 1.393(8) . ? 
C20 C21 1.385(9) . ? 
C21 C22 1.367(9) . ? 
C22 C23 1.341(9) . ? 
C23 C24 1.377(9) . ? 
C25 C26 1.469(8) . ? 
C26 C27 1.370(10) . ? 
C26 C31 1.378(10) . ? 
C27 C28 1.377(9) . ? 
C28 C29 1.382(9) . ? 
C29 C30 1.364(9) . ? 
C30 C31 1.392(9) . ? 
C32 C33 1.316(8) . ? 
C32 C36 1.346(8) . ? 
C33 C34 1.312(8) . ? 
C34 C35 1.351(9) . ? 
C35 C36 1.370(9) . ? 
 
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 
O2 Ti1 O1 134.6(2) . . ? 
O2 Ti1 N1 85.7(3) . . ? 
O1 Ti1 N1 68.6(3) . . ? 
O2 Ti1 C15 102.4(3) . . ? 
O1 Ti1 C15 108.3(3) . . ? 
N1 Ti1 C15 79.3(3) . . ? 
O2 Ti1 Cl1 89.21(16) . . ? 
O1 Ti1 Cl1 86.35(17) . . ? 
N1 Ti1 Cl1 137.8(2) . . ? 
C15 Ti1 Cl1 142.4(2) . . ? 
O2 Ti1 C18 132.9(3) . . ? 
O1 Ti1 C18 92.2(3) . . ? 
N1 Ti1 C18 124.1(3) . . ? 
C15 Ti1 C18 57.0(3) . . ? 
Cl1 Ti1 C18 88.9(2) . . ? 
O2 Ti1 C16 82.3(2) . . ? 
O1 Ti1 C16 139.4(2) . . ? 
N1 Ti1 C16 105.8(3) . . ? 
C15 Ti1 C16 34.8(2) . . ? 
Cl1 Ti1 C16 115.0(3) . . ? 
C18 Ti1 C16 56.4(3) . . ? 
O2 Ti1 C17 98.9(3) . . ? 
O1 Ti1 C17 125.7(3) . . ? 
N1 Ti1 C17 135.8(3) . . ? 
C15 Ti1 C17 56.7(3) . . ? 
Cl1 Ti1 C17 86.4(2) . . ? 
C18 Ti1 C17 34.0(2) . . ? 
C16 Ti1 C17 33.4(2) . . ? 
O2 Ti1 C14 135.7(3) . . ? 
O1 Ti1 C14 83.0(3) . . ? 
N1 Ti1 C14 90.2(3) . . ? 
C15 Ti1 C14 33.9(2) . . ? 
Cl1 Ti1 C14 120.8(3) . . ? 
C18 Ti1 C14 34.1(2) . . ? 
C16 Ti1 C14 56.5(3) . . ? 
C17 Ti1 C14 56.2(3) . . ? 
O4 Ti2 O3 134.1(2) . . ? 
O4 Ti2 N2 84.8(3) . . ? 
O3 Ti2 N2 71.3(3) . . ? 
O4 Ti2 C35 87.5(5) . . ? 
O3 Ti2 C35 138.4(5) . . ? 
N2 Ti2 C35 122.5(6) . . ? 
O4 Ti2 C33 115.6(5) . . ? 
O3 Ti2 C33 97.1(5) . . ? 
N2 Ti2 C33 77.2(3) . . ? 
C35 Ti2 C33 55.8(4) . . ? 
O4 Ti2 Cl2 87.14(16) . . ? 
O3 Ti2 Cl2 88.36(15) . . ? 
N2 Ti2 Cl2 141.76(19) . . ? 
C35 Ti2 Cl2 94.3(5) . . ? 
C33 Ti2 Cl2 138.8(3) . . ? 
O4 Ti2 C34 86.8(4) . . ? 
O3 Ti2 C34 129.7(5) . . ? 
N2 Ti2 C34 88.8(5) . . ? 
C35 Ti2 C34 33.8(2) . . ? 
C33 Ti2 C34 32.7(2) . . ? 
Cl2 Ti2 C34 128.0(5) . . ? 
O4 Ti2 C36 119.7(6) . . ? 
O3 Ti2 C36 105.3(5) . . ? 
N2 Ti2 C36 131.4(4) . . ? 
C35 Ti2 C36 34.3(2) . . ? 
C33 Ti2 C36 54.7(3) . . ? 
Cl2 Ti2 C36 84.4(3) . . ? 
C34 Ti2 C36 55.2(4) . . ? 
O4 Ti2 C32 140.4(3) . . ? 
O3 Ti2 C32 83.6(3) . . ? 
N2 Ti2 C32 100.8(5) . . ? 
C35 Ti2 C32 56.3(4) . . ? 
C33 Ti2 C32 32.6(2) . . ? 
Cl2 Ti2 C32 109.0(5) . . ? 
C34 Ti2 C32 54.6(3) . . ? 
C36 Ti2 C32 33.3(2) . . ? 
C7 N1 C6 128.4(12) . . ? 
C7 N1 Ti1 118.1(11) . . ? 
C6 N1 Ti1 113.4(6) . . ? 
C25 N2 C24 122.6(10) . . ? 
C25 N2 Ti2 122.6(9) . . ? 
C24 N2 Ti2 114.7(6) . . ? 
C1 O1 Ti1 126.9(5) . . ? 
C13 O2 Ti1 131.3(5) . . ? 
C19 O3 Ti2 124.7(5) . . ? 
C31 O4 Ti2 129.6(5) . . ? 
O1 C1 C2 124.6(9) . . ? 
O1 C1 C6 117.3(8) . . ? 
C2 C1 C6 118.1(8) . . ? 
C1 C2 C3 119.6(8) . . ? 
C4 C3 C2 122.0(8) . . ? 
C5 C4 C3 119.0(8) . . ? 
C4 C5 C6 119.6(8) . . ? 
C1 C6 C5 121.7(8) . . ? 
C1 C6 N1 105.6(8) . . ? 
C5 C6 N1 132.7(10) . . ? 
N1 C7 C8 132.2(14) . . ? 
C13 C8 C9 120.6(8) . . ? 
C13 C8 C7 125.1(10) . . ? 
C9 C8 C7 114.2(10) . . ? 
C10 C9 C8 120.5(8) . . ? 
C9 C10 C11 119.5(8) . . ? 
C10 C11 C12 119.6(7) . . ? 
C13 C12 C11 121.7(7) . . ? 
O2 C13 C12 122.9(9) . . ? 
O2 C13 C8 119.0(8) . . ? 
C12 C13 C8 118.0(8) . . ? 
C15 C14 C18 108.5(8) . . ? 
C15 C14 Ti1 72.0(4) . . ? 
C18 C14 Ti1 72.4(4) . . ? 
C14 C15 C16 107.0(7) . . ? 
C14 C15 Ti1 74.0(5) . . ? 
C16 C15 Ti1 73.2(4) . . ? 
C17 C16 C15 108.0(7) . . ? 
C17 C16 Ti1 73.5(5) . . ? 
C15 C16 Ti1 72.0(4) . . ? 
C16 C17 C18 109.0(8) . . ? 
C16 C17 Ti1 73.1(5) . . ? 
C18 C17 Ti1 72.7(5) . . ? 
C17 C18 C14 107.4(8) . . ? 
C17 C18 Ti1 73.3(4) . . ? 
C14 C18 Ti1 73.5(4) . . ? 
O3 C19 C24 118.5(8) . . ? 
O3 C19 C20 121.6(8) . . ? 
C24 C19 C20 119.9(8) . . ? 
C21 C20 C19 117.8(7) . . ? 
C22 C21 C20 121.6(8) . . ? 
C23 C22 C21 119.8(8) . . ? 
C22 C23 C24 120.8(8) . . ? 
C23 C24 C19 120.0(8) . . ? 
C23 C24 N2 133.9(10) . . ? 
C19 C24 N2 106.1(8) . . ? 
N2 C25 C26 127.2(12) . . ? 
C27 C26 C31 122.3(8) . . ? 
C27 C26 C25 114.7(10) . . ? 
C31 C26 C25 122.8(10) . . ? 
C26 C27 C28 118.0(9) . . ? 
C27 C28 C29 120.9(8) . . ? 
C30 C29 C28 120.2(8) . . ? 
C29 C30 C31 119.8(8) . . ? 
O4 C31 C26 122.3(9) . . ? 
O4 C31 C30 119.1(9) . . ? 
C26 C31 C30 118.6(8) . . ? 
C33 C32 C36 107.2(9) . . ? 
C33 C32 Ti2 72.3(5) . . ? 
C36 C32 Ti2 72.4(6) . . ? 
C34 C33 C32 109.9(10) . . ? 
C34 C33 Ti2 73.9(6) . . ? 
C32 C33 Ti2 75.1(5) . . ? 
C33 C34 C35 109.0(11) . . ? 
C33 C34 Ti2 73.4(6) . . ? 
C35 C34 Ti2 72.1(8) . . ? 
C34 C35 C36 105.3(11) . . ? 
C34 C35 Ti2 74.1(8) . . ? 
C36 C35 Ti2 74.0(8) . . ? 
C32 C36 C35 108.4(10) . . ? 
C32 C36 Ti2 74.3(6) . . ? 
C35 C36 Ti2 71.7(8) . . ? 
 
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.563 
_refine_diff_density_min   -0.277 
_refine_diff_density_rms    0.061 

#===END

  
data_f60525b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C23 H24 Cl N O2 Ti' 
_chemical_formula_weight          429.78 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2776   0.4457 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    12.360(3) 
_cell_length_b                    12.831(3) 
_cell_length_c                    13.710(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.316(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      2097.1(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     735 
_cell_measurement_theta_min       2.332 
_cell_measurement_theta_max       21.781 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.08 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.361 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1344
_exptl_absorpt_coefficient_mu     0.830 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   0.9365	 
_exptl_absorpt_correction_T_max   0.9675
_exptl_absorpt_process_details    sadabs 
  
_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_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10386 
_diffrn_reflns_av_R_equivalents   0.0359 
_diffrn_reflns_av_sigmaI/netI     0.0623 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.97 
_diffrn_reflns_theta_max          27.13 
_reflns_number_total              4577 
_reflns_number_gt                 2749 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/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          4577 
_refine_ls_number_parameters      257 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0891 
_refine_ls_R_factor_gt            0.0482 
_refine_ls_wR_factor_ref          0.1147 
_refine_ls_wR_factor_gt           0.1020 
_refine_ls_goodness_of_fit_ref    0.913 
_refine_ls_restrained_S_all       0.913 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ti1 Ti 0.27792(4) 0.13208(4) 0.19963(4) 0.04414(16) Uani 1 1 d . . . 
Cl1 Cl 0.33770(7) 0.28100(6) 0.12849(7) 0.0721(3) Uani 1 1 d . . . 
O1 O 0.42901(14) 0.09856(13) 0.25949(13) 0.0450(5) Uani 1 1 d . . . 
O2 O 0.18018(15) 0.22306(13) 0.24665(14) 0.0491(5) Uani 1 1 d . . . 
N1 N 0.26562(17) 0.06276(15) 0.34076(16) 0.0392(5) Uani 1 1 d . . . 
C1 C 0.4848(2) 0.01785(19) 0.30971(19) 0.0398(6) Uani 1 1 d . . . 
C2 C 0.5939(2) -0.0069(2) 0.3028(2) 0.0450(7) Uani 1 1 d . . . 
C3 C 0.6416(2) -0.0969(2) 0.3528(2) 0.0477(7) Uani 1 1 d . . . 
H3 H 0.7117 -0.1169 0.3465 0.057 Uiso 1 1 calc R . . 
C4 C 0.5911(2) -0.1590(2) 0.4119(2) 0.0458(7) Uani 1 1 d . . . 
C5 C 0.4900(2) -0.12826(19) 0.4243(2) 0.0426(6) Uani 1 1 d . . . 
H5 H 0.4576 -0.1655 0.4676 0.051 Uiso 1 1 calc R . . 
C6 C 0.4338(2) -0.04079(18) 0.37251(19) 0.0392(6) Uani 1 1 d . . . 
C7 C 0.3321(2) -0.00657(18) 0.3934(2) 0.0413(6) Uani 1 1 d . . . 
H7 H 0.3125 -0.0360 0.4483 0.050 Uiso 1 1 calc R . . 
C8 C 0.1734(2) 0.10336(19) 0.3722(2) 0.0411(6) Uani 1 1 d . . . 
C9 C 0.1306(2) 0.0682(2) 0.4494(2) 0.0491(7) Uani 1 1 d . . . 
H9 H 0.1576 0.0073 0.4841 0.059 Uiso 1 1 calc R . . 
C10 C 0.0464(2) 0.1255(2) 0.4744(2) 0.0560(8) Uani 1 1 d . . . 
H10 H 0.0181 0.1039 0.5276 0.067 Uiso 1 1 calc R . . 
C11 C 0.0042(2) 0.2148(2) 0.4205(2) 0.0555(8) Uani 1 1 d . . . 
H11 H -0.0522 0.2527 0.4379 0.067 Uiso 1 1 calc R . . 
C12 C 0.0448(2) 0.2476(2) 0.3423(2) 0.0507(7) Uani 1 1 d . . . 
H12 H 0.0146 0.3063 0.3052 0.061 Uiso 1 1 calc R . . 
C13 C 0.1312(2) 0.19314(19) 0.3181(2) 0.0438(6) Uani 1 1 d . . . 
C14 C 0.6554(2) 0.0618(2) 0.2434(2) 0.0584(8) Uani 1 1 d . . . 
C15 C 0.5903(3) 0.0671(3) 0.1323(2) 0.0768(10) Uani 1 1 d . . . 
H15A H 0.5775 -0.0022 0.1053 0.115 Uiso 1 1 calc R . . 
H15B H 0.6327 0.1060 0.0953 0.115 Uiso 1 1 calc R . . 
H15C H 0.5195 0.1009 0.1264 0.115 Uiso 1 1 calc R . . 
C16 C 0.6688(3) 0.1711(3) 0.2898(3) 0.0849(11) Uani 1 1 d . . . 
H16A H 0.7103 0.2140 0.2551 0.127 Uiso 1 1 calc R . . 
H16B H 0.7083 0.1667 0.3601 0.127 Uiso 1 1 calc R . . 
H16C H 0.5961 0.2011 0.2833 0.127 Uiso 1 1 calc R . . 
C17 C 0.7729(3) 0.0192(3) 0.2481(3) 0.0812(11) Uani 1 1 d . . . 
H17A H 0.7662 -0.0484 0.2169 0.122 Uiso 1 1 calc R . . 
H17B H 0.8156 0.0136 0.3174 0.122 Uiso 1 1 calc R . . 
H17C H 0.8103 0.0657 0.2128 0.122 Uiso 1 1 calc R . . 
C18 C 0.6475(2) -0.2578(2) 0.4606(3) 0.0624(9) Uani 1 1 d . . . 
H18A H 0.6296 -0.2689 0.5238 0.094 Uiso 1 1 calc R . . 
H18B H 0.7273 -0.2512 0.4724 0.094 Uiso 1 1 calc R . . 
H18C H 0.6214 -0.3159 0.4166 0.094 Uiso 1 1 calc R . . 
C19 C 0.2809(3) -0.0088(3) 0.0895(4) 0.0857(12) Uani 1 1 d . . . 
H19 H 0.3491 -0.0387 0.0883 0.103 Uiso 1 1 calc R . . 
C20 C 0.2167(5) -0.0389(3) 0.1481(3) 0.0888(13) Uani 1 1 d . . . 
H20 H 0.2324 -0.0932 0.1947 0.107 Uiso 1 1 calc R . . 
C21 C 0.1240(4) 0.0230(5) 0.1285(4) 0.1083(18) Uani 1 1 d . . . 
H21 H 0.0652 0.0192 0.1590 0.130 Uiso 1 1 calc R . . 
C22 C 0.1343(4) 0.0923(4) 0.0548(4) 0.1096(19) Uani 1 1 d . . . 
H22 H 0.0833 0.1441 0.0257 0.131 Uiso 1 1 calc R . . 
C23 C 0.2318(5) 0.0713(4) 0.0327(3) 0.0986(14) Uani 1 1 d . . . 
H23 H 0.2603 0.1067 -0.0143 0.118 Uiso 1 1 calc R . . 
  
  
_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 O1 1.8805(18) . ? 
Ti1 O2 1.9103(17) . ? 
Ti1 N1 2.171(2) . ? 
Ti1 C23 2.341(4) . ? 
Ti1 C22 2.343(4) . ? 
Ti1 Cl1 2.3514(10) . ? 
Ti1 C21 2.356(4) . ? 
Ti1 C19 2.362(3) . ? 
Ti1 C20 2.367(3) . ? 
O1 C1 1.331(3) . ? 
O2 C13 1.337(3) . ? 
N1 C7 1.294(3) . ? 
N1 C8 1.420(3) . ? 
C1 C6 1.411(3) . ? 
C1 C2 1.414(3) . ? 
C2 C3 1.391(4) . ? 
C2 C14 1.531(4) . ? 
C3 C4 1.395(4) . ? 
C4 C5 1.364(3) . ? 
C4 C18 1.514(4) . ? 
C5 C6 1.409(3) . ? 
C6 C7 1.430(3) . ? 
C8 C9 1.378(4) . ? 
C8 C13 1.395(3) . ? 
C9 C10 1.390(4) . ? 
C10 C11 1.389(4) . ? 
C11 C12 1.365(4) . ? 
C12 C13 1.388(4) . ? 
C14 C15 1.525(4) . ? 
C14 C16 1.530(4) . ? 
C14 C17 1.537(4) . ? 
C19 C20 1.326(5) . ? 
C19 C23 1.335(5) . ? 
C20 C21 1.361(6) . ? 
C21 C22 1.377(6) . ? 
C22 C23 1.346(6) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1 Ti1 O2 129.51(8) . . ? 
O1 Ti1 N1 79.20(8) . . ? 
O2 Ti1 N1 75.54(8) . . ? 
O1 Ti1 C23 107.91(17) . . ? 
O2 Ti1 C23 121.41(17) . . ? 
N1 Ti1 C23 132.72(12) . . ? 
O1 Ti1 C22 139.70(14) . . ? 
O2 Ti1 C22 90.79(14) . . ? 
N1 Ti1 C22 116.74(19) . . ? 
C23 Ti1 C22 33.40(15) . . ? 
O1 Ti1 Cl1 88.99(6) . . ? 
O2 Ti1 Cl1 86.52(6) . . ? 
N1 Ti1 Cl1 143.73(6) . . ? 
C23 Ti1 Cl1 83.53(11) . . ? 
C22 Ti1 Cl1 94.38(17) . . ? 
O1 Ti1 C21 130.17(19) . . ? 
O2 Ti1 C21 89.38(14) . . ? 
N1 Ti1 C21 83.47(17) . . ? 
C23 Ti1 C21 55.68(16) . . ? 
C22 Ti1 C21 34.08(15) . . ? 
Cl1 Ti1 C21 128.26(19) . . ? 
O1 Ti1 C19 85.54(11) . . ? 
O2 Ti1 C19 143.28(12) . . ? 
N1 Ti1 C19 105.82(15) . . ? 
C23 Ti1 C19 32.98(13) . . ? 
C22 Ti1 C19 55.13(13) . . ? 
Cl1 Ti1 C19 107.30(14) . . ? 
C21 Ti1 C19 55.11(14) . . ? 
O1 Ti1 C20 96.92(14) . . ? 
O2 Ti1 C20 119.11(16) . . ? 
N1 Ti1 C20 78.13(12) . . ? 
C23 Ti1 C20 54.77(14) . . ? 
C22 Ti1 C20 55.55(14) . . ? 
Cl1 Ti1 C20 137.73(12) . . ? 
C21 Ti1 C20 33.51(14) . . ? 
C19 Ti1 C20 32.58(13) . . ? 
C1 O1 Ti1 136.27(16) . . ? 
C13 O2 Ti1 121.40(16) . . ? 
C7 N1 C8 121.7(2) . . ? 
C7 N1 Ti1 126.51(18) . . ? 
C8 N1 Ti1 111.77(16) . . ? 
O1 C1 C6 118.5(2) . . ? 
O1 C1 C2 120.9(2) . . ? 
C6 C1 C2 120.6(2) . . ? 
C3 C2 C1 116.1(2) . . ? 
C3 C2 C14 122.3(2) . . ? 
C1 C2 C14 121.5(2) . . ? 
C2 C3 C4 124.4(3) . . ? 
C5 C4 C3 118.2(2) . . ? 
C5 C4 C18 121.1(3) . . ? 
C3 C4 C18 120.7(3) . . ? 
C4 C5 C6 120.9(3) . . ? 
C5 C6 C1 119.5(2) . . ? 
C5 C6 C7 119.0(2) . . ? 
C1 C6 C7 121.1(2) . . ? 
N1 C7 C6 124.2(2) . . ? 
C9 C8 C13 120.9(3) . . ? 
C9 C8 N1 127.9(2) . . ? 
C13 C8 N1 111.1(2) . . ? 
C8 C9 C10 118.8(3) . . ? 
C11 C10 C9 120.4(3) . . ? 
C12 C11 C10 120.6(3) . . ? 
C11 C12 C13 119.9(3) . . ? 
O2 C13 C12 123.8(2) . . ? 
O2 C13 C8 116.7(2) . . ? 
C12 C13 C8 119.5(3) . . ? 
C15 C14 C16 110.1(3) . . ? 
C15 C14 C2 110.6(2) . . ? 
C16 C14 C2 108.7(2) . . ? 
C15 C14 C17 107.5(3) . . ? 
C16 C14 C17 108.2(3) . . ? 
C2 C14 C17 111.7(3) . . ? 
C20 C19 C23 108.9(4) . . ? 
C20 C19 Ti1 73.9(2) . . ? 
C23 C19 Ti1 72.7(2) . . ? 
C19 C20 C21 108.6(4) . . ? 
C19 C20 Ti1 73.5(2) . . ? 
C21 C20 Ti1 72.8(2) . . ? 
C20 C21 C22 106.5(4) . . ? 
C20 C21 Ti1 73.7(2) . . ? 
C22 C21 Ti1 72.5(2) . . ? 
C23 C22 C21 107.3(4) . . ? 
C23 C22 Ti1 73.2(2) . . ? 
C21 C22 Ti1 73.5(2) . . ? 
C19 C23 C22 108.6(4) . . ? 
C19 C23 Ti1 74.4(2) . . ? 
C22 C23 Ti1 73.4(2) . . ? 
  
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              27.13 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.403 
_refine_diff_density_min   -0.242 
_refine_diff_density_rms    0.057 
  
#===END

  
data_f60516a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H14 Cl N O S Ti' 
_chemical_formula_weight          375.71 
  
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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2776   0.4457 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M    I-4 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 'y, -x, -z' 
 '-y, x, -z' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, -y+1/2, z+1/2' 
 'y+1/2, -x+1/2, -z+1/2' 
 '-y+1/2, x+1/2, -z+1/2' 
  
_cell_length_a                    21.043(4) 
_cell_length_b                    21.043(4) 
_cell_length_c                    7.488(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3315.6(13) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     795 
_cell_measurement_theta_min       2.887 
_cell_measurement_theta_max       22.006 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.505 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1536 
_exptl_absorpt_coefficient_mu     0.805 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8887 
_exptl_absorpt_correction_T_max   0.9384 
_exptl_absorpt_process_details    sadabs 
  
_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_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         3.58 
_diffrn_reflns_number             7656 
_diffrn_reflns_av_R_equivalents   0.0316 
_diffrn_reflns_av_sigmaI/netI     0.0524 
_diffrn_reflns_limit_h_min        -25 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          1.37 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              3214 
_reflns_number_gt                 2649 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0365P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.04(3) 
_refine_ls_number_reflns          3214 
_refine_ls_number_parameters      208 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0520 
_refine_ls_R_factor_gt            0.0419 
_refine_ls_wR_factor_ref          0.0816 
_refine_ls_wR_factor_gt           0.0787 
_refine_ls_goodness_of_fit_ref    0.957 
_refine_ls_restrained_S_all       0.957 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ti1 Ti 0.95083(3) 0.19412(3) 0.16998(7) 0.03756(16) Uani 1 1 d . . . 
S1 S 0.99539(5) 0.29405(5) 0.07883(11) 0.0489(3) Uani 1 1 d . . . 
Cl1 Cl 0.95658(6) 0.17901(5) -0.13946(11) 0.0712(3) Uani 1 1 d . . . 
O1 O 0.86520(12) 0.17196(12) 0.1643(3) 0.0537(7) Uani 1 1 d . . . 
N1 N 0.91830(13) 0.26003(12) 0.3783(4) 0.0387(7) Uani 1 1 d . . . 
C1 C 0.99770(16) 0.33368(16) 0.2844(4) 0.0397(8) Uani 1 1 d . . . 
C2 C 1.03606(16) 0.38666(16) 0.3121(5) 0.0445(9) Uani 1 1 d . . . 
H2A H 1.0617 0.4017 0.2201 0.053 Uiso 1 1 calc R . . 
C3 C 1.03631(17) 0.41662(16) 0.4734(5) 0.0466(9) Uani 1 1 d . . . 
H3A H 1.0615 0.4525 0.4900 0.056 Uiso 1 1 calc R . . 
C4 C 0.99990(17) 0.39440(17) 0.6107(5) 0.0499(10) Uani 1 1 d . . . 
H4A H 1.0011 0.4151 0.7204 0.060 Uiso 1 1 calc R . . 
C5 C 0.96136(16) 0.34199(17) 0.5902(5) 0.0454(9) Uani 1 1 d . . . 
H5A H 0.9374 0.3266 0.6851 0.055 Uiso 1 1 calc R . . 
C6 C 0.95920(16) 0.31236(15) 0.4227(4) 0.0378(8) Uani 1 1 d . . . 
C7 C 0.86608(17) 0.25373(17) 0.4639(5) 0.0502(10) Uani 1 1 d . . . 
H7A H 0.8594 0.2819 0.5578 0.060 Uiso 1 1 calc R . . 
C8 C 0.81675(18) 0.20823(17) 0.4317(5) 0.0496(10) Uani 1 1 d . . . 
C9 C 0.7636(2) 0.2066(2) 0.5452(7) 0.0775(15) Uani 1 1 d . . . 
H9A H 0.7632 0.2318 0.6474 0.093 Uiso 1 1 calc R . . 
C10 C 0.7126(2) 0.1690(2) 0.5082(9) 0.0916(18) Uani 1 1 d . . . 
H10A H 0.6777 0.1683 0.5845 0.110 Uiso 1 1 calc R . . 
C11 C 0.71318(19) 0.13118(19) 0.3543(7) 0.0737(14) Uani 1 1 d . . . 
H11A H 0.6783 0.1058 0.3274 0.088 Uiso 1 1 calc R . . 
C12 C 0.7641(2) 0.1315(2) 0.2450(7) 0.0639(12) Uani 1 1 d . . . 
H12A H 0.7640 0.1055 0.1445 0.077 Uiso 1 1 calc R . . 
C13 C 0.81666(18) 0.16946(17) 0.2786(5) 0.0470(9) Uani 1 1 d . . . 
C14 C 1.0181(2) 0.1695(2) 0.4116(6) 0.0617(12) Uani 1 1 d . . . 
H14A H 1.0298 0.1983 0.5091 0.074 Uiso 1 1 calc R . . 
C15 C 0.9703(2) 0.1260(2) 0.4153(6) 0.0622(11) Uani 1 1 d . . . 
H15A H 0.9412 0.1191 0.5157 0.075 Uiso 1 1 calc R . . 
C16 C 0.9727(3) 0.0910(2) 0.2702(8) 0.0868(17) Uani 1 1 d . . . 
H16A H 0.9463 0.0536 0.2468 0.104 Uiso 1 1 calc R . . 
C17 C 1.0224(3) 0.1097(3) 0.1695(8) 0.109(3) Uani 1 1 d . . . 
H17A H 1.0385 0.0877 0.0633 0.131 Uiso 1 1 calc R . . 
C18 C 1.0522(2) 0.1598(3) 0.2571(10) 0.098(2) Uani 1 1 d . . . 
H18A H 1.0929 0.1794 0.2253 0.117 Uiso 1 1 calc R . . 
  
  
_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 O1 1.862(2) . ? 
Ti1 N1 2.197(3) . ? 
Ti1 C17 2.330(5) . ? 
Ti1 C16 2.342(5) . ? 
Ti1 Cl1 2.3419(11) . ? 
Ti1 C18 2.346(5) . ? 
Ti1 C14 2.355(4) . ? 
Ti1 C15 2.366(4) . ? 
Ti1 S1 2.4014(12) . ? 
S1 C1 1.751(3) . ? 
O1 C13 1.334(4) . ? 
N1 C7 1.279(4) . ? 
N1 C6 1.436(4) . ? 
C1 C6 1.389(5) . ? 
C1 C2 1.392(5) . ? 
C2 C3 1.362(5) . ? 
C3 C4 1.365(5) . ? 
C4 C5 1.377(5) . ? 
C5 C6 1.401(4) . ? 
C7 C8 1.433(5) . ? 
C8 C9 1.405(5) . ? 
C8 C13 1.407(5) . ? 
C9 C10 1.363(6) . ? 
C10 C11 1.400(7) . ? 
C11 C12 1.349(6) . ? 
C12 C13 1.387(5) . ? 
C14 C15 1.361(6) . ? 
C14 C18 1.377(7) . ? 
C15 C16 1.313(6) . ? 
C16 C17 1.348(8) . ? 
C17 C18 1.391(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 
O1 Ti1 N1 82.70(11) . . ? 
O1 Ti1 C17 115.8(2) . . ? 
N1 Ti1 C17 133.17(17) . . ? 
O1 Ti1 C16 88.05(18) . . ? 
N1 Ti1 C16 114.76(18) . . ? 
C17 Ti1 C16 33.53(19) . . ? 
O1 Ti1 Cl1 89.62(9) . . ? 
N1 Ti1 Cl1 143.56(8) . . ? 
C17 Ti1 Cl1 82.04(15) . . ? 
C16 Ti1 Cl1 100.43(16) . . ? 
O1 Ti1 C18 144.07(15) . . ? 
N1 Ti1 C18 106.3(2) . . ? 
C17 Ti1 C18 34.62(19) . . ? 
C16 Ti1 C18 56.4(2) . . ? 
Cl1 Ti1 C18 100.74(19) . . ? 
O1 Ti1 C14 122.98(15) . . ? 
N1 Ti1 C14 77.34(13) . . ? 
C17 Ti1 C14 56.25(17) . . ? 
C16 Ti1 C14 55.35(16) . . ? 
Cl1 Ti1 C14 134.35(13) . . ? 
C18 Ti1 C14 34.05(17) . . ? 
O1 Ti1 C15 91.92(14) . . ? 
N1 Ti1 C15 83.41(13) . . ? 
C17 Ti1 C15 55.04(19) . . ? 
C16 Ti1 C15 32.39(16) . . ? 
Cl1 Ti1 C15 132.60(12) . . ? 
C18 Ti1 C15 55.94(17) . . ? 
C14 Ti1 C15 33.50(14) . . ? 
O1 Ti1 S1 126.21(9) . . ? 
N1 Ti1 S1 76.75(8) . . ? 
C17 Ti1 S1 114.5(2) . . ? 
C16 Ti1 S1 145.64(17) . . ? 
Cl1 Ti1 S1 79.48(4) . . ? 
C18 Ti1 S1 89.63(14) . . ? 
C14 Ti1 S1 100.16(12) . . ? 
C15 Ti1 S1 133.14(12) . . ? 
C1 S1 Ti1 100.25(12) . . ? 
C13 O1 Ti1 137.4(2) . . ? 
C7 N1 C6 118.6(3) . . ? 
C7 N1 Ti1 123.9(2) . . ? 
C6 N1 Ti1 117.5(2) . . ? 
C6 C1 C2 119.0(3) . . ? 
C6 C1 S1 119.0(3) . . ? 
C2 C1 S1 121.9(3) . . ? 
C3 C2 C1 120.3(3) . . ? 
C2 C3 C4 120.5(3) . . ? 
C3 C4 C5 121.4(3) . . ? 
C4 C5 C6 118.4(3) . . ? 
C1 C6 C5 120.3(3) . . ? 
C1 C6 N1 115.1(3) . . ? 
C5 C6 N1 124.6(3) . . ? 
N1 C7 C8 127.4(4) . . ? 
C9 C8 C13 118.5(4) . . ? 
C9 C8 C7 119.4(4) . . ? 
C13 C8 C7 121.7(4) . . ? 
C10 C9 C8 121.2(5) . . ? 
C9 C10 C11 119.4(4) . . ? 
C12 C11 C10 120.3(4) . . ? 
C11 C12 C13 121.7(5) . . ? 
O1 C13 C12 121.1(4) . . ? 
O1 C13 C8 119.9(3) . . ? 
C12 C13 C8 118.9(4) . . ? 
C15 C14 C18 107.7(4) . . ? 
C15 C14 Ti1 73.7(2) . . ? 
C18 C14 Ti1 72.6(3) . . ? 
C16 C15 C14 109.3(5) . . ? 
C16 C15 Ti1 72.8(3) . . ? 
C14 C15 Ti1 72.8(2) . . ? 
C15 C16 C17 109.3(5) . . ? 
C15 C16 Ti1 74.8(3) . . ? 
C17 C16 Ti1 72.7(3) . . ? 
C16 C17 C18 107.9(5) . . ? 
C16 C17 Ti1 73.7(3) . . ? 
C18 C17 Ti1 73.3(3) . . ? 
C14 C18 C17 105.9(5) . . ? 
C14 C18 Ti1 73.4(2) . . ? 
C17 C18 Ti1 72.1(3) . . ? 
  
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.298 
_refine_diff_density_min   -0.204 
_refine_diff_density_rms    0.052 
  
#===END

  
data_f60707b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C23 H24 Cl N O S Ti' 
_chemical_formula_weight          445.84 
  
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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2776   0.4457 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pna2(1) 
  
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' 
  
_cell_length_a                    22.415(11) 
_cell_length_b                    13.398(6) 
_cell_length_c                    7.215(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2166.9(18) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     613
_cell_measurement_theta_min       2.369 
_cell_measurement_theta_max       18.486 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.366 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              464 
_exptl_absorpt_coefficient_mu     0.314 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   0.9693 
_exptl_absorpt_correction_T_max   0.9814 
_exptl_absorpt_process_details    sadabs 
  
_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_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10204 
_diffrn_reflns_av_R_equivalents   0.1033 
_diffrn_reflns_av_sigmaI/netI     0.1884 
_diffrn_reflns_limit_h_min        -28 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          1.77 
_diffrn_reflns_theta_max          27.56 
_reflns_number_total              3768 
_reflns_number_gt                 1793 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0335P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.61(5) 
_refine_ls_number_reflns          3768 
_refine_ls_number_parameters      257 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.1402 
_refine_ls_R_factor_gt            0.0539 
_refine_ls_wR_factor_ref          0.1002 
_refine_ls_wR_factor_gt           0.0855 
_refine_ls_goodness_of_fit_ref    0.805 
_refine_ls_restrained_S_all       0.805 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ti1 Ti 0.32112(4) 0.49089(7) 0.08611(17) 0.0378(3) Uani 1 1 d . . . 
S1 S 0.26968(8) 0.61545(11) 0.2760(2) 0.0462(5) Uani 1 1 d . . . 
Cl1 Cl 0.38491(7) 0.62750(10) 0.0345(2) 0.0489(5) Uani 1 1 d . . . 
O1 O 0.38657(17) 0.4100(2) 0.1410(5) 0.0365(10) Uani 1 1 d . . . 
N1 N 0.2810(2) 0.4027(3) 0.3084(7) 0.0369(14) Uani 1 1 d . . . 
C1 C 0.2135(3) 0.5387(4) 0.3685(8) 0.0389(16) Uani 1 1 d . . . 
C2 C 0.1604(3) 0.5759(4) 0.4503(9) 0.0470(18) Uani 1 1 d . . . 
H2 H 0.1537 0.6444 0.4550 0.056 Uiso 1 1 calc R . . 
C3 C 0.1187(3) 0.5110(5) 0.5228(8) 0.0523(18) Uani 1 1 d . . . 
H3 H 0.0838 0.5369 0.5727 0.063 Uiso 1 1 calc R . . 
C4 C 0.1270(3) 0.4090(4) 0.5240(9) 0.0500(17) Uani 1 1 d . . . 
H4 H 0.0982 0.3667 0.5734 0.060 Uiso 1 1 calc R . . 
C5 C 0.1802(3) 0.3706(4) 0.4483(9) 0.0484(18) Uani 1 1 d . . . 
H5 H 0.1867 0.3021 0.4462 0.058 Uiso 1 1 calc R . . 
C6 C 0.2229(3) 0.4350(4) 0.3769(8) 0.0386(16) Uani 1 1 d . . . 
C7 C 0.3054(3) 0.3262(4) 0.3893(8) 0.0364(16) Uani 1 1 d . . . 
H7 H 0.2829 0.2965 0.4824 0.044 Uiso 1 1 calc R . . 
C8 C 0.3625(3) 0.2814(4) 0.3539(8) 0.0326(15) Uani 1 1 d . . . 
C9 C 0.3794(3) 0.1958(4) 0.4552(7) 0.0347(16) Uani 1 1 d . . . 
H9 H 0.3532 0.1695 0.5422 0.042 Uiso 1 1 calc R . . 
C10 C 0.4336(3) 0.1506(4) 0.4282(9) 0.0381(16) Uani 1 1 d . . . 
C11 C 0.4733(3) 0.1949(4) 0.2989(8) 0.0359(15) Uani 1 1 d . . . 
H11 H 0.5105 0.1654 0.2829 0.043 Uiso 1 1 calc R . . 
C12 C 0.4600(3) 0.2805(4) 0.1932(8) 0.0314(14) Uani 1 1 d . . . 
C13 C 0.4042(3) 0.3248(4) 0.2249(8) 0.0315(15) Uani 1 1 d . . . 
C14 C 0.4523(3) 0.0569(4) 0.5284(9) 0.059(2) Uani 1 1 d . . . 
H14A H 0.4178 0.0245 0.5791 0.089 Uiso 1 1 calc R . . 
H14B H 0.4793 0.0738 0.6267 0.089 Uiso 1 1 calc R . . 
H14C H 0.4718 0.0126 0.4430 0.089 Uiso 1 1 calc R . . 
C15 C 0.5047(2) 0.3209(4) 0.0415(8) 0.0363(14) Uani 1 1 d . . . 
C16 C 0.5636(2) 0.2613(4) 0.0375(10) 0.0568(19) Uani 1 1 d . . . 
H16A H 0.5550 0.1914 0.0244 0.085 Uiso 1 1 calc R . . 
H16B H 0.5850 0.2722 0.1510 0.085 Uiso 1 1 calc R . . 
H16C H 0.5875 0.2831 -0.0652 0.085 Uiso 1 1 calc R . . 
C17 C 0.4747(3) 0.3104(5) -0.1490(9) 0.059(2) Uani 1 1 d . . . 
H17A H 0.5020 0.3310 -0.2440 0.088 Uiso 1 1 calc R . . 
H17B H 0.4396 0.3516 -0.1532 0.088 Uiso 1 1 calc R . . 
H17C H 0.4636 0.2420 -0.1687 0.088 Uiso 1 1 calc R . . 
C18 C 0.5211(3) 0.4317(4) 0.0835(10) 0.0568(18) Uani 1 1 d . . . 
H18A H 0.5345 0.4373 0.2094 0.085 Uiso 1 1 calc R . . 
H18B H 0.4866 0.4731 0.0657 0.085 Uiso 1 1 calc R . . 
H18C H 0.5523 0.4528 0.0012 0.085 Uiso 1 1 calc R . . 
C19 C 0.2700(5) 0.5379(5) -0.1937(12) 0.079(3) Uani 1 1 d . . . 
H19 H 0.2659 0.6050 -0.2249 0.095 Uiso 1 1 calc R . . 
C20 C 0.3177(4) 0.4738(7) -0.2409(10) 0.079(2) Uani 1 1 d . . . 
H20 H 0.3516 0.4910 -0.3077 0.094 Uiso 1 1 calc R . . 
C21 C 0.3045(4) 0.3814(6) -0.1699(12) 0.073(2) Uani 1 1 d . . . 
H21 H 0.3279 0.3245 -0.1829 0.088 Uiso 1 1 calc R . . 
C22 C 0.2518(4) 0.3862(6) -0.0776(11) 0.068(2) Uani 1 1 d . . . 
H22 H 0.2335 0.3337 -0.0155 0.082 Uiso 1 1 calc R . . 
C23 C 0.2304(4) 0.4802(8) -0.0910(13) 0.080(3) Uani 1 1 d . . . 
H23 H 0.1948 0.5027 -0.0398 0.096 Uiso 1 1 calc R . . 
  
  
_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 O1 1.866(4) . ? 
Ti1 N1 2.185(5) . ? 
Ti1 Cl1 2.3522(18) . ? 
Ti1 C20 2.372(7) . ? 
Ti1 C21 2.388(7) . ? 
Ti1 C22 2.403(7) . ? 
Ti1 C19 2.406(8) . ? 
Ti1 C23 2.406(7) . ? 
Ti1 S1 2.448(2) . ? 
S1 C1 1.758(6) . ? 
O1 C13 1.351(6) . ? 
N1 C7 1.300(6) . ? 
N1 C6 1.460(7) . ? 
C1 C6 1.407(7) . ? 
C1 C2 1.418(8) . ? 
C2 C3 1.380(8) . ? 
C3 C4 1.379(7) . ? 
C4 C5 1.408(8) . ? 
C5 C6 1.387(8) . ? 
C7 C8 1.438(7) . ? 
C8 C9 1.411(7) . ? 
C8 C13 1.442(8) . ? 
C9 C10 1.371(7) . ? 
C10 C11 1.419(8) . ? 
C10 C14 1.509(7) . ? 
C11 C12 1.410(7) . ? 
C12 C13 1.403(7) . ? 
C12 C15 1.579(8) . ? 
C15 C17 1.536(8) . ? 
C15 C16 1.545(7) . ? 
C15 C18 1.559(7) . ? 
C19 C23 1.392(10) . ? 
C19 C20 1.413(11) . ? 
C20 C21 1.372(9) . ? 
C21 C22 1.358(9) . ? 
C22 C23 1.350(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 
O1 Ti1 N1 81.59(18) . . ? 
O1 Ti1 Cl1 90.43(12) . . ? 
N1 Ti1 Cl1 141.88(13) . . ? 
O1 Ti1 C20 100.4(3) . . ? 
N1 Ti1 C20 131.6(2) . . ? 
Cl1 Ti1 C20 86.4(2) . . ? 
O1 Ti1 C21 86.0(2) . . ? 
N1 Ti1 C21 99.9(3) . . ? 
Cl1 Ti1 C21 116.8(3) . . ? 
C20 Ti1 C21 33.5(2) . . ? 
O1 Ti1 C22 105.9(3) . . ? 
N1 Ti1 C22 77.3(2) . . ? 
Cl1 Ti1 C22 140.3(2) . . ? 
C20 Ti1 C22 55.5(3) . . ? 
C21 Ti1 C22 32.9(2) . . ? 
O1 Ti1 C19 134.8(3) . . ? 
N1 Ti1 C19 124.2(3) . . ? 
Cl1 Ti1 C19 87.3(2) . . ? 
C20 Ti1 C19 34.4(3) . . ? 
C21 Ti1 C19 55.8(2) . . ? 
C22 Ti1 C19 55.4(3) . . ? 
O1 Ti1 C23 137.9(2) . . ? 
N1 Ti1 C23 90.6(3) . . ? 
Cl1 Ti1 C23 118.4(3) . . ? 
C20 Ti1 C23 55.8(3) . . ? 
C21 Ti1 C23 54.6(3) . . ? 
C22 Ti1 C23 32.6(2) . . ? 
C19 Ti1 C23 33.6(2) . . ? 
O1 Ti1 S1 130.34(14) . . ? 
N1 Ti1 S1 76.35(13) . . ? 
Cl1 Ti1 S1 81.05(7) . . ? 
C20 Ti1 S1 127.4(3) . . ? 
C21 Ti1 S1 141.1(2) . . ? 
C22 Ti1 S1 111.6(3) . . ? 
C19 Ti1 S1 93.8(2) . . ? 
C23 Ti1 S1 86.6(2) . . ? 
C1 S1 Ti1 98.7(2) . . ? 
C13 O1 Ti1 144.7(4) . . ? 
C7 N1 C6 117.1(5) . . ? 
C7 N1 Ti1 125.7(4) . . ? 
C6 N1 Ti1 117.1(3) . . ? 
C6 C1 C2 117.1(6) . . ? 
C6 C1 S1 119.1(5) . . ? 
C2 C1 S1 123.6(5) . . ? 
C3 C2 C1 120.2(6) . . ? 
C4 C3 C2 122.4(6) . . ? 
C3 C4 C5 118.3(6) . . ? 
C6 C5 C4 120.1(6) . . ? 
C5 C6 C1 121.8(6) . . ? 
C5 C6 N1 123.9(5) . . ? 
C1 C6 N1 114.3(5) . . ? 
N1 C7 C8 128.6(6) . . ? 
C9 C8 C7 119.1(5) . . ? 
C9 C8 C13 119.3(5) . . ? 
C7 C8 C13 121.6(5) . . ? 
C10 C9 C8 121.5(5) . . ? 
C9 C10 C11 117.7(5) . . ? 
C9 C10 C14 123.1(6) . . ? 
C11 C10 C14 119.2(5) . . ? 
C12 C11 C10 124.3(5) . . ? 
C13 C12 C11 116.4(5) . . ? 
C13 C12 C15 122.2(5) . . ? 
C11 C12 C15 121.4(5) . . ? 
O1 C13 C12 123.1(5) . . ? 
O1 C13 C8 116.1(5) . . ? 
C12 C13 C8 120.8(5) . . ? 
C17 C15 C16 108.1(5) . . ? 
C17 C15 C18 111.4(5) . . ? 
C16 C15 C18 107.1(4) . . ? 
C17 C15 C12 108.1(4) . . ? 
C16 C15 C12 112.2(5) . . ? 
C18 C15 C12 110.0(5) . . ? 
C23 C19 C20 105.8(7) . . ? 
C23 C19 Ti1 73.2(5) . . ? 
C20 C19 Ti1 71.5(5) . . ? 
C21 C20 C19 107.3(8) . . ? 
C21 C20 Ti1 73.9(5) . . ? 
C19 C20 Ti1 74.1(4) . . ? 
C22 C21 C20 109.1(7) . . ? 
C22 C21 Ti1 74.1(4) . . ? 
C20 C21 Ti1 72.6(4) . . ? 
C23 C22 C21 108.6(8) . . ? 
C23 C22 Ti1 73.8(5) . . ? 
C21 C22 Ti1 72.9(4) . . ? 
C22 C23 C19 109.3(8) . . ? 
C22 C23 Ti1 73.6(5) . . ? 
C19 C23 Ti1 73.2(5) . . ? 
  
_diffrn_measured_fraction_theta_max    0.961 
_diffrn_reflns_theta_full              27.56 
_diffrn_measured_fraction_theta_full   0.961 
_refine_diff_density_max    0.514 
_refine_diff_density_min   -0.306 
_refine_diff_density_rms    0.059 
  
  
#===END


  
data_f60410d 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C22 H22 Cl N O3 Zr' 
_chemical_formula_weight          475.08 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zr'  'Zr'  -2.9673   0.5597 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    8.572(3) 
_cell_length_b                    14.639(4) 
_cell_length_c                    15.940(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.075(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      1997.2(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     712 
_cell_measurement_theta_min       2.559 
_cell_measurement_theta_max       21.131 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.580 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              968 
_exptl_absorpt_coefficient_mu     0.707 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9013 
_exptl_absorpt_correction_T_max   0.9655 
_exptl_absorpt_process_details    sadabs 
  
_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_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         4.07 
_diffrn_reflns_number             8310 
_diffrn_reflns_av_R_equivalents   0.0463 
_diffrn_reflns_av_sigmaI/netI     0.0817 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              3523 
_reflns_number_gt                 2124 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0427P)²+0.0000P] where P=(Fo²+2Fc²)/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          3523 
_refine_ls_number_parameters      272 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0772 
_refine_ls_R_factor_gt            0.0408 
_refine_ls_wR_factor_ref          0.0900 
_refine_ls_wR_factor_gt           0.0834 
_refine_ls_goodness_of_fit_ref    0.842 
_refine_ls_restrained_S_all       0.842 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Zr1 Zr 0.12799(5) 1.01326(2) 0.24954(2) 0.04222(15) Uani 1 1 d . . . 
Cl1 Cl -0.12100(14) 1.07533(7) 0.18364(7) 0.0578(3) Uani 1 1 d . A . 
O1 O 0.2582(4) 1.11399(19) 0.2009(2) 0.0608(9) Uani 1 1 d . A . 
O2 O 0.0350(4) 0.88435(18) 0.24007(19) 0.0572(9) Uani 1 1 d . A . 
O3 O 0.3622(3) 0.93519(17) 0.25347(18) 0.0501(7) Uani 1 1 d . A . 
C1 C 0.138(2) 0.9303(18) 0.0620(15) 0.051(7) Uani 0.41(4) 1 d P A 1 
H1A H 0.1578 0.9305 0.0052 0.061 Uiso 0.41(4) 1 calc PR A 1 
N1 N 0.190(2) 0.9932(15) 0.1089(14) 0.046(5) Uani 0.41(4) 1 d P A 1 
C1' C 0.2082(15) 0.9864(10) 0.0510(10) 0.048(5) Uani 0.59(4) 1 d P A 2 
H1'A H 0.2016 0.9567 -0.0006 0.058 Uiso 0.59(4) 1 calc PR A 2 
N1' N 0.1382(17) 0.9534(11) 0.1123(10) 0.042(4) Uani 0.59(4) 1 d P A 2 
C2 C 0.3214(5) 1.1278(3) 0.1275(3) 0.0479(12) Uani 1 1 d . . . 
C3 C 0.4170(5) 1.2025(3) 0.1158(3) 0.0503(12) Uani 1 1 d . A . 
H3A H 0.4329 1.2450 0.1588 0.060 Uiso 1 1 calc R . . 
C4 C 0.4875(6) 1.2146(3) 0.0426(3) 0.0638(14) Uani 1 1 d . . . 
H4A H 0.5555 1.2634 0.0370 0.077 Uiso 1 1 calc R A . 
C5 C 0.4604(8) 1.1568(4) -0.0221(4) 0.0867(19) Uani 1 1 d . A . 
H5A H 0.5077 1.1665 -0.0725 0.104 Uiso 1 1 calc R . . 
C6 C 0.3634(8) 1.0840(4) -0.0137(4) 0.0832(19) Uani 1 1 d . . . 
H6A H 0.3431 1.0450 -0.0590 0.100 Uiso 1 1 calc R A . 
C7 C 0.2954(6) 1.0673(3) 0.0605(4) 0.0605(14) Uani 1 1 d . A . 
C8 C 0.0518(6) 0.8605(3) 0.0949(3) 0.0588(13) Uani 1 1 d . . . 
C9 C 0.0206(7) 0.8087(4) 0.0244(4) 0.0813(18) Uani 1 1 d . A . 
H9A H 0.0571 0.8270 -0.0269 0.098 Uiso 1 1 calc R . . 
C10 C -0.0639(8) 0.7306(4) 0.0296(4) 0.0869(19) Uani 1 1 d . . . 
H10A H -0.0847 0.6953 -0.0183 0.104 Uiso 1 1 calc R A . 
C11 C -0.1187(6) 0.7032(3) 0.1048(4) 0.0682(15) Uani 1 1 d . A . 
H11A H -0.1777 0.6501 0.1078 0.082 Uiso 1 1 calc R . . 
C12 C -0.0860(5) 0.7548(3) 0.1758(3) 0.0530(12) Uani 1 1 d . . . 
H12A H -0.1222 0.7360 0.2270 0.064 Uiso 1 1 calc R A . 
C13 C 0.0006(5) 0.8346(3) 0.1714(3) 0.0458(11) Uani 1 1 d . A . 
C14 C -0.0100(7) 1.0241(5) 0.3846(3) 0.0780(18) Uani 1 1 d . A . 
H14A H -0.1182 1.0060 0.3927 0.094 Uiso 1 1 calc R . . 
C15 C 0.1209(10) 0.9722(4) 0.4041(3) 0.0773(18) Uani 1 1 d . A . 
H15A H 0.1211 0.9101 0.4270 0.093 Uiso 1 1 calc R . . 
C16 C 0.2491(8) 1.0277(4) 0.3998(3) 0.0765(17) Uani 1 1 d . A . 
H16A H 0.3565 1.0115 0.4182 0.092 Uiso 1 1 calc R . . 
C17 C 0.1970(8) 1.1133(4) 0.3785(3) 0.0693(15) Uani 1 1 d . A . 
H17A H 0.2621 1.1683 0.3784 0.083 Uiso 1 1 calc R . . 
C18 C 0.0413(8) 1.1123(4) 0.3680(3) 0.0719(16) Uani 1 1 d . A . 
H18A H -0.0256 1.1663 0.3616 0.086 Uiso 1 1 calc R . . 
C19 C 0.3798(6) 0.8379(3) 0.2714(4) 0.0775(17) Uani 1 1 d . . . 
H19A H 0.3363 0.8016 0.2249 0.093 Uiso 1 1 calc R A . 
H19B H 0.3275 0.8216 0.3217 0.093 Uiso 1 1 calc R . . 
C20 C 0.5491(7) 0.8232(4) 0.2833(4) 0.101(2) Uani 1 1 d . A . 
H20A H 0.5717 0.7851 0.3322 0.122 Uiso 1 1 calc R . . 
H20B H 0.5877 0.7925 0.2346 0.122 Uiso 1 1 calc R . . 
C21 C 0.6224(7) 0.9081(4) 0.2942(5) 0.110(2) Uani 1 1 d . . . 
H21A H 0.7224 0.9083 0.2684 0.132 Uiso 1 1 calc R A . 
H21B H 0.6397 0.9219 0.3535 0.132 Uiso 1 1 calc R . . 
C22 C 0.5163(6) 0.9761(3) 0.2533(3) 0.0653(14) Uani 1 1 d . A . 
H22A H 0.5194 1.0330 0.2845 0.078 Uiso 1 1 calc R . . 
H22B H 0.5451 0.9881 0.1963 0.078 Uiso 1 1 calc R . . 
  
  
_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 
Zr1 O1 2.029(3) . ? 
Zr1 O2 2.051(3) . ? 
Zr1 O3 2.308(3) . ? 
Zr1 N1 2.35(2) . ? 
Zr1 N1' 2.363(16) . ? 
Zr1 Cl1 2.4988(14) . ? 
Zr1 C14 2.517(5) . ? 
Zr1 C18 2.524(5) . ? 
Zr1 C15 2.540(5) . ? 
Zr1 C17 2.567(5) . ? 
Zr1 C16 2.568(5) . ? 
O1 C2 1.330(5) . ? 
O2 C13 1.334(5) . ? 
O3 C22 1.450(5) . ? 
O3 C19 1.459(5) . ? 
C1 N1 1.25(5) . ? 
C1 C8 1.38(3) . ? 
N1 C7 1.63(2) . ? 
C1' N1' 1.27(4) . ? 
C1' C7 1.405(18) . ? 
N1' C8 1.566(17) . ? 
C2 C3 1.386(5) . ? 
C2 C7 1.395(6) . ? 
C3 C4 1.354(6) . ? 
C4 C5 1.344(7) . ? 
C5 C6 1.364(8) . ? 
C6 C7 1.368(7) . ? 
C8 C9 1.371(7) . ? 
C8 C13 1.372(6) . ? 
C9 C10 1.359(7) . ? 
C10 C11 1.370(8) . ? 
C11 C12 1.377(6) . ? 
C12 C13 1.388(6) . ? 
C14 C15 1.377(8) . ? 
C14 C18 1.393(7) . ? 
C15 C16 1.372(7) . ? 
C16 C17 1.367(7) . ? 
C17 C18 1.336(7) . ? 
C19 C20 1.469(7) . ? 
C20 C21 1.400(7) . ? 
C21 C22 1.476(6) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1 Zr1 O2 149.34(13) . . ? 
O1 Zr1 O3 82.80(11) . . ? 
O2 Zr1 O3 83.13(11) . . ? 
O1 Zr1 N1 64.4(6) . . ? 
O2 Zr1 N1 85.5(6) . . ? 
O3 Zr1 N1 73.9(4) . . ? 
O1 Zr1 N1' 82.3(5) . . ? 
O2 Zr1 N1' 67.9(5) . . ? 
O3 Zr1 N1' 76.5(3) . . ? 
N1 Zr1 N1' 18.0(3) . . ? 
O1 Zr1 Cl1 92.87(10) . . ? 
O2 Zr1 Cl1 89.08(9) . . ? 
O3 Zr1 Cl1 156.00(8) . . ? 
N1 Zr1 Cl1 82.9(4) . . ? 
N1' Zr1 Cl1 79.6(3) . . ? 
O1 Zr1 C14 125.08(16) . . ? 
O2 Zr1 C14 85.56(17) . . ? 
O3 Zr1 C14 117.13(18) . . ? 
N1 Zr1 C14 164.8(6) . . ? 
N1' Zr1 C14 149.1(5) . . ? 
Cl1 Zr1 C14 84.65(17) . . ? 
O1 Zr1 C18 93.38(18) . . ? 
O2 Zr1 C18 117.04(18) . . ? 
O3 Zr1 C18 123.68(16) . . ? 
N1 Zr1 C18 151.2(5) . . ? 
N1' Zr1 C18 158.9(3) . . ? 
Cl1 Zr1 C18 80.02(15) . . ? 
C14 Zr1 C18 32.08(16) . . ? 
O1 Zr1 C15 125.84(18) . . ? 
O2 Zr1 C15 79.86(15) . . ? 
O3 Zr1 C15 85.56(19) . . ? 
N1 Zr1 C15 156.1(4) . . ? 
N1' Zr1 C15 144.5(4) . . ? 
Cl1 Zr1 C15 115.43(19) . . ? 
C14 Zr1 C15 31.59(18) . . ? 
C18 Zr1 C15 52.18(17) . . ? 
O1 Zr1 C17 77.51(16) . . ? 
O2 Zr1 C17 130.98(15) . . ? 
O3 Zr1 C17 95.63(17) . . ? 
N1 Zr1 C17 141.4(6) . . ? 
N1' Zr1 C17 159.2(5) . . ? 
Cl1 Zr1 C17 106.50(15) . . ? 
C14 Zr1 C17 51.49(17) . . ? 
C18 Zr1 C17 30.41(16) . . ? 
C15 Zr1 C17 51.31(17) . . ? 
O1 Zr1 C16 95.38(18) . . ? 
O2 Zr1 C16 106.29(17) . . ? 
O3 Zr1 C16 73.02(15) . . ? 
N1 Zr1 C16 143.1(5) . . ? 
N1' Zr1 C16 149.4(3) . . ? 
Cl1 Zr1 C16 130.97(13) . . ? 
C14 Zr1 C16 51.80(19) . . ? 
C18 Zr1 C16 51.33(18) . . ? 
C15 Zr1 C16 31.15(16) . . ? 
C17 Zr1 C16 30.89(15) . . ? 
C2 O1 Zr1 134.8(3) . . ? 
C13 O2 Zr1 129.1(3) . . ? 
C22 O3 C19 108.6(3) . . ? 
C22 O3 Zr1 125.9(2) . . ? 
C19 O3 Zr1 124.7(3) . . ? 
N1 C1 C8 120(2) . . ? 
C1 N1 C7 113(2) . . ? 
C1 N1 Zr1 125(2) . . ? 
C7 N1 Zr1 121.8(13) . . ? 
N1' C1' C7 120.6(16) . . ? 
C1' N1' C8 115.6(16) . . ? 
C1' N1' Zr1 127.9(16) . . ? 
C8 N1' Zr1 116.5(10) . . ? 
O1 C2 C3 120.6(4) . . ? 
O1 C2 C7 121.4(4) . . ? 
C3 C2 C7 118.0(5) . . ? 
C4 C3 C2 120.9(4) . . ? 
C5 C4 C3 120.9(5) . . ? 
C4 C5 C6 119.8(6) . . ? 
C5 C6 C7 121.0(5) . . ? 
C6 C7 C2 119.4(5) . . ? 
C6 C7 C1' 107.8(8) . . ? 
C2 C7 C1' 132.8(9) . . ? 
C6 C7 N1 143.0(10) . . ? 
C2 C7 N1 97.5(10) . . ? 
C1' C7 N1 35.4(6) . . ? 
C9 C8 C13 121.2(5) . . ? 
C9 C8 C1 100.6(12) . . ? 
C13 C8 C1 138.2(12) . . ? 
C9 C8 N1' 134.1(8) . . ? 
C13 C8 N1' 104.7(7) . . ? 
C1 C8 N1' 33.6(8) . . ? 
C10 C9 C8 119.8(6) . . ? 
C9 C10 C11 120.6(5) . . ? 
C10 C11 C12 119.6(5) . . ? 
C11 C12 C13 120.4(5) . . ? 
O2 C13 C8 120.7(4) . . ? 
O2 C13 C12 120.9(4) . . ? 
C8 C13 C12 118.4(4) . . ? 
C15 C14 C18 107.0(5) . . ? 
C15 C14 Zr1 75.1(3) . . ? 
C18 C14 Zr1 74.3(3) . . ? 
C16 C15 C14 107.9(5) . . ? 
C16 C15 Zr1 75.6(3) . . ? 
C14 C15 Zr1 73.3(3) . . ? 
C17 C16 C15 107.7(6) . . ? 
C17 C16 Zr1 74.5(3) . . ? 
C15 C16 Zr1 73.3(3) . . ? 
C18 C17 C16 109.4(5) . . ? 
C18 C17 Zr1 73.0(3) . . ? 
C16 C17 Zr1 74.6(3) . . ? 
C17 C18 C14 108.1(5) . . ? 
C17 C18 Zr1 76.6(3) . . ? 
C14 C18 Zr1 73.7(3) . . ? 
O3 C19 C20 105.0(4) . . ? 
C21 C20 C19 108.7(5) . . ? 
C20 C21 C22 106.4(5) . . ? 
O3 C22 C21 105.1(4) . . ? 
  
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.706 
_refine_diff_density_min   -0.385 
_refine_diff_density_rms    0.081 
  

