data_2005src0377
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C22 H8 Cl2 F10 N4 Ti'
_chemical_formula_sum
 'C22 H8 Cl2 F10 N4 Ti'
_chemical_formula_weight          637.12
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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    C2/c
_symmetry_space_group_name_hall   '-C 2yc'
 
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                    14.034(3)
_cell_length_b                    7.5893(15)
_cell_length_c                    22.296(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  104.38(3)
_cell_angle_gamma                 90.00
_cell_volume                      2300.3(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     2813
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.840
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1256
_exptl_absorpt_coefficient_mu     0.707
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8158
_exptl_absorpt_correction_T_max   0.9326
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             16052
_diffrn_reflns_av_R_equivalents   0.0319
_diffrn_reflns_av_sigmaI/netI     0.0229
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          3.41
_diffrn_reflns_theta_max          27.50
_reflns_number_total              2637
_reflns_number_gt                 2229
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'DENZO, COLLECT'
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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)+(0.0631P)²+1.5443P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0
_refine_ls_number_reflns          2637
_refine_ls_number_parameters      194
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0404
_refine_ls_R_factor_gt            0.0315
_refine_ls_wR_factor_ref          0.0953
_refine_ls_wR_factor_gt           0.0879
_refine_ls_goodness_of_fit_ref    1.012
_refine_ls_restrained_S_all       1.012
_refine_ls_shift/su_max           0.018
_refine_ls_shift/su_mean          0.002
 
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
H5 H 0.2904(14) 0.416(2) 0.7629(9) 0.020(5) Uiso 1 1 d . . .
H2 H 0.6795(16) 0.346(3) 0.6015(9) 0.029(5) Uiso 1 1 d . . .
H3 H 0.5537(16) 0.152(3) 0.5299(10) 0.039(6) Uiso 1 1 d . . .
H4 H 0.4526(16) 0.000(3) 0.5964(10) 0.033(5) Uiso 1 1 d . . .
C1 C 0.61537(11) 0.2516(2) 0.67152(7) 0.0190(3) Uani 1 1 d . . .
C2 C 0.63092(13) 0.2726(2) 0.61265(8) 0.0242(4) Uani 1 1 d . . .
C3 C 0.56158(13) 0.1659(2) 0.57345(8) 0.0254(4) Uani 1 1 d . . .
C4 C 0.50699(13) 0.0836(2) 0.60901(8) 0.0236(4) Uani 1 1 d . . .
C5 C 0.34644(11) 0.3318(2) 0.77080(7) 0.0187(3) Uani 1 1 d . . .
C6 C 0.34694(12) 0.3575(2) 0.66601(7) 0.0185(3) Uani 1 1 d . . .
C7 C 0.39693(12) 0.4786(2) 0.63856(8) 0.0221(3) Uani 1 1 d . . .
C8 C 0.35953(14) 0.5349(2) 0.57859(9) 0.0290(4) Uani 1 1 d . . .
C9 C 0.27118(15) 0.4700(3) 0.54457(8) 0.0310(4) Uani 1 1 d . . .
C10 C 0.21957(13) 0.3505(2) 0.57029(8) 0.0285(4) Uani 1 1 d . . .
C11 C 0.25697(12) 0.2968(2) 0.63099(8) 0.0225(4) Uani 1 1 d . . .
N1 N 0.53872(9) 0.13394(18) 0.66941(6) 0.0187(3) Uani 1 1 d . . .
N2 N 0.38835(9) 0.29162(17) 0.72639(6) 0.0175(3) Uani 1 1 d . . .
F1 F 0.48269(7) 0.54454(14) 0.67080(5) 0.0286(3) Uani 1 1 d . . .
F2 F 0.40900(9) 0.65279(17) 0.55334(6) 0.0442(3) Uani 1 1 d . . .
F3 F 0.23456(10) 0.52458(18) 0.48598(5) 0.0452(3) Uani 1 1 d . . .
F4 F 0.13404(8) 0.28621(16) 0.53732(5) 0.0393(3) Uani 1 1 d . . .
F5 F 0.20465(7) 0.18282(14) 0.65545(5) 0.0310(3) Uani 1 1 d . . .
Cl1 Cl 0.38500(3) -0.10876(5) 0.70127(2) 0.02694(15) Uani 1 1 d . . .
Ti1 Ti 0.5000 0.08449(5) 0.7500 0.01653(14) Uani 1 2 d S . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N1 1.390(2) . ?
C1 C2 1.392(2) . ?
C1 C5 1.404(2) 2_656 ?
C2 C3 1.394(3) . ?
C3 C4 1.381(3) . ?
C4 N1 1.364(2) . ?
C5 N2 1.307(2) . ?
C5 C1 1.404(2) 2_656 ?
C6 C7 1.387(2) . ?
C6 C11 1.388(2) . ?
C6 N2 1.418(2) . ?
C7 F1 1.336(2) . ?
C7 C8 1.377(3) . ?
C8 F2 1.339(2) . ?
C8 C9 1.374(3) . ?
C9 F3 1.345(2) . ?
C9 C10 1.372(3) . ?
C10 F4 1.335(2) . ?
C10 C11 1.386(2) . ?
C11 F5 1.336(2) . ?
N1 Ti1 2.0372(14) . ?
N2 Ti1 2.1895(14) . ?
Cl1 Ti1 2.2505(7) . ?
Ti1 N1 2.0372(14) 2_656 ?
Ti1 N2 2.1895(14) 2_656 ?
Ti1 Cl1 2.2505(7) 2_656 ?
 
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
N1 C1 C2 110.05(14) . . ?
N1 C1 C5 115.21(14) . 2_656 ?
C2 C1 C5 134.49(15) . 2_656 ?
C1 C2 C3 106.03(15) . . ?
C4 C3 C2 107.65(16) . . ?
N1 C4 C3 110.38(15) . . ?
N2 C5 C1 116.85(14) . 2_656 ?
C7 C6 C11 117.44(15) . . ?
C7 C6 N2 121.29(14) . . ?
C11 C6 N2 121.20(15) . . ?
F1 C7 C8 118.75(15) . . ?
F1 C7 C6 119.83(15) . . ?
C8 C7 C6 121.41(16) . . ?
F2 C8 C9 119.88(16) . . ?
F2 C8 C7 120.20(18) . . ?
C9 C8 C7 119.92(17) . . ?
F3 C9 C10 119.70(18) . . ?
F3 C9 C8 120.05(18) . . ?
C10 C9 C8 120.25(16) . . ?
F4 C10 C9 120.50(16) . . ?
F4 C10 C11 120.07(17) . . ?
C9 C10 C11 119.44(17) . . ?
F5 C11 C10 118.43(15) . . ?
F5 C11 C6 120.05(14) . . ?
C10 C11 C6 121.51(16) . . ?
C4 N1 C1 105.88(13) . . ?
C4 N1 Ti1 136.56(12) . . ?
C1 N1 Ti1 117.54(11) . . ?
C5 N2 C6 118.78(13) . . ?
C5 N2 Ti1 114.54(11) . . ?
C6 N2 Ti1 125.54(10) . . ?
N1 Ti1 N1 158.77(8) . 2_656 ?
N1 Ti1 N2 75.41(5) . 2_656 ?
N1 Ti1 N2 89.28(5) 2_656 2_656 ?
N1 Ti1 N2 89.28(5) . . ?
N1 Ti1 N2 75.41(5) 2_656 . ?
N2 Ti1 N2 88.22(7) 2_656 . ?
N1 Ti1 Cl1 90.61(4) . . ?
N1 Ti1 Cl1 103.27(4) 2_656 . ?
N2 Ti1 Cl1 165.59(4) 2_656 . ?
N2 Ti1 Cl1 88.12(4) . . ?
N1 Ti1 Cl1 103.27(4) . 2_656 ?
N1 Ti1 Cl1 90.61(4) 2_656 2_656 ?
N2 Ti1 Cl1 88.12(4) 2_656 2_656 ?
N2 Ti1 Cl1 165.59(4) . 2_656 ?
Cl1 Ti1 Cl1 98.67(4) . 2_656 ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.273
_refine_diff_density_min   -0.465
_refine_diff_density_rms    0.059
