data_2005src1012
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C22 H18 Cl2 N4 Ti'
_chemical_formula_sum
 'C22 H18 Cl2 N4 Ti'
_chemical_formula_weight          457.20
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
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                    11.5255(6)
_cell_length_b                    14.0330(7)
_cell_length_c                    14.1939(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  113.615(2)
_cell_angle_gamma                 90.00
_cell_volume                      2103.44(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4871
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        blade
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.34
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.444
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              936
_exptl_absorpt_coefficient_mu     0.677
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8025
_exptl_absorpt_correction_T_max   0.9933
_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   '10cm confocal mirrors'
_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             24418
_diffrn_reflns_av_R_equivalents   0.0997
_diffrn_reflns_av_sigmaI/netI     0.0835
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.13
_diffrn_reflns_theta_max          27.50
_reflns_number_total              4806
_reflns_number_gt                 3374
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_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)+(0.0217P)²+3.0625P] 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          4806
_refine_ls_number_parameters      262
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0948
_refine_ls_R_factor_gt            0.0571
_refine_ls_wR_factor_ref          0.1117
_refine_ls_wR_factor_gt           0.0986
_refine_ls_goodness_of_fit_ref    1.030
_refine_ls_restrained_S_all       1.030
_refine_ls_shift/su_max           0.010
_refine_ls_shift/su_mean          0.001
 
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
C1 C 0.6197(3) 0.7563(2) -0.1757(2) 0.0237(7) Uani 1 1 d . . .
H1 H 0.5763 0.6978 -0.1991 0.028 Uiso 1 1 calc R . .
C2 C 0.5755(3) 0.8443(3) -0.2191(2) 0.0298(8) Uani 1 1 d . . .
H2 H 0.4984 0.8566 -0.2765 0.036 Uiso 1 1 calc R . .
C3 C 0.6661(3) 0.9118(2) -0.1624(2) 0.0260(7) Uani 1 1 d . . .
H3 H 0.6625 0.9787 -0.1740 0.031 Uiso 1 1 calc R . .
C4 C 0.7620(3) 0.8621(2) -0.0863(2) 0.0215(7) Uani 1 1 d . . .
C5 C 0.8773(3) 0.8866(2) -0.0067(2) 0.0214(7) Uani 1 1 d . . .
H5 H 0.9030 0.9513 0.0063 0.026 Uiso 1 1 calc R . .
C6 C 1.0638(3) 0.8430(2) 0.1335(2) 0.0210(7) Uani 1 1 d . . .
C7 C 1.0635(3) 0.9069(2) 0.2079(2) 0.0264(7) Uani 1 1 d . . .
H7 H 0.9864 0.9357 0.2024 0.032 Uiso 1 1 calc R . .
C8 C 1.1752(4) 0.9288(2) 0.2900(3) 0.0312(8) Uani 1 1 d . . .
H8 H 1.1749 0.9730 0.3405 0.037 Uiso 1 1 calc R . .
C9 C 1.2873(3) 0.8868(2) 0.2988(3) 0.0332(8) Uani 1 1 d . . .
H9 H 1.3641 0.9013 0.3555 0.040 Uiso 1 1 calc R . .
C10 C 1.2869(3) 0.8231(3) 0.2240(3) 0.0339(8) Uani 1 1 d . . .
H10 H 1.3641 0.7946 0.2294 0.041 Uiso 1 1 calc R . .
C11 C 1.1762(3) 0.8004(2) 0.1420(3) 0.0273(7) Uani 1 1 d . . .
H11 H 1.1767 0.7560 0.0917 0.033 Uiso 1 1 calc R . .
C12 C 1.1049(3) 0.5911(2) 0.1878(2) 0.0238(7) Uani 1 1 d . . .
H12 H 1.1425 0.5620 0.1465 0.029 Uiso 1 1 calc R . .
C13 C 1.1613(3) 0.5978(2) 0.2938(2) 0.0260(7) Uani 1 1 d . . .
H13 H 1.2429 0.5749 0.3372 0.031 Uiso 1 1 calc R . .
C14 C 1.0748(3) 0.6450(2) 0.3251(2) 0.0247(7) Uani 1 1 d . . .
H14 H 1.0866 0.6598 0.3936 0.030 Uiso 1 1 calc R . .
C15 C 0.9695(3) 0.6658(2) 0.2367(2) 0.0203(7) Uani 1 1 d . . .
C16 C 0.8558(3) 0.7141(2) 0.2150(2) 0.0200(7) Uani 1 1 d . . .
H16 H 0.8345 0.7379 0.2687 0.024 Uiso 1 1 calc R . .
C17 C 0.6657(3) 0.7789(2) 0.0956(2) 0.0201(7) Uani 1 1 d . . .
C18 C 0.5509(3) 0.7425(2) 0.0277(2) 0.0264(7) Uani 1 1 d . . .
H18 H 0.5480 0.6826 -0.0044 0.032 Uiso 1 1 calc R . .
C19 C 0.4406(3) 0.7932(3) 0.0066(3) 0.0306(8) Uani 1 1 d . . .
H19 H 0.3618 0.7672 -0.0386 0.037 Uiso 1 1 calc R . .
C20 C 0.4441(3) 0.8814(3) 0.0509(3) 0.0303(8) Uani 1 1 d . . .
H20 H 0.3682 0.9165 0.0354 0.036 Uiso 1 1 calc R . .
C21 C 0.5584(3) 0.9183(2) 0.1175(3) 0.0288(8) Uani 1 1 d . . .
H21 H 0.5609 0.9787 0.1484 0.035 Uiso 1 1 calc R . .
C22 C 0.6701(3) 0.8678(2) 0.1399(2) 0.0235(7) Uani 1 1 d . . .
H22 H 0.7488 0.8939 0.1851 0.028 Uiso 1 1 calc R . .
N1 N 0.7336(2) 0.76512(18) -0.09498(19) 0.0200(6) Uani 1 1 d . . .
N2 N 0.9485(2) 0.81848(18) 0.04901(18) 0.0189(5) Uani 1 1 d . . .
N3 N 0.9878(2) 0.63217(18) 0.15072(18) 0.0195(5) Uani 1 1 d . . .
N4 N 0.7794(2) 0.72556(18) 0.11849(19) 0.0186(5) Uani 1 1 d . . .
Cl1 Cl 0.98862(8) 0.63454(6) -0.06559(6) 0.02448(19) Uani 1 1 d . . .
Cl2 Cl 0.72101(8) 0.55331(6) -0.04537(6) 0.02577(19) Uani 1 1 d . . .
Ti1 Ti 0.85897(5) 0.67606(4) 0.01122(4) 0.01816(14) Uani 1 1 d . . .
 
 
_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 1.359(4) . ?
C1 C2 1.382(5) . ?
C2 C3 1.401(5) . ?
C3 C4 1.385(4) . ?
C4 N1 1.394(4) . ?
C4 C5 1.399(5) . ?
C5 N2 1.301(4) . ?
C6 C7 1.387(4) . ?
C6 C11 1.386(4) . ?
C6 N2 1.430(4) . ?
C7 C8 1.381(5) . ?
C8 C9 1.380(5) . ?
C9 C10 1.386(5) . ?
C10 C11 1.375(5) . ?
C12 N3 1.364(4) . ?
C12 C13 1.382(4) . ?
C13 C14 1.409(5) . ?
C14 C15 1.383(4) . ?
C15 C16 1.396(4) . ?
C15 N3 1.400(4) . ?
C16 N4 1.309(4) . ?
C17 C18 1.385(4) . ?
C17 C22 1.389(4) . ?
C17 N4 1.429(4) . ?
C18 C19 1.381(5) . ?
C19 C20 1.382(5) . ?
C20 C21 1.378(5) . ?
C21 C22 1.390(5) . ?
N1 Ti1 2.044(3) . ?
N2 Ti1 2.214(3) . ?
N3 Ti1 2.037(3) . ?
N4 Ti1 2.182(2) . ?
Cl1 Ti1 2.2509(9) . ?
Cl2 Ti1 2.2622(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
N1 C1 C2 110.7(3) . . ?
C1 C2 C3 106.9(3) . . ?
C4 C3 C2 106.6(3) . . ?
C3 C4 N1 109.7(3) . . ?
C3 C4 C5 135.2(3) . . ?
N1 C4 C5 115.1(3) . . ?
N2 C5 C4 118.3(3) . . ?
C7 C6 C11 119.9(3) . . ?
C7 C6 N2 120.6(3) . . ?
C11 C6 N2 119.5(3) . . ?
C8 C7 C6 120.0(3) . . ?
C9 C8 C7 120.3(3) . . ?
C8 C9 C10 119.4(3) . . ?
C11 C10 C9 120.9(3) . . ?
C10 C11 C6 119.5(3) . . ?
N3 C12 C13 110.7(3) . . ?
C12 C13 C14 106.9(3) . . ?
C15 C14 C13 106.7(3) . . ?
C14 C15 C16 135.0(3) . . ?
C14 C15 N3 109.6(3) . . ?
C16 C15 N3 115.3(3) . . ?
N4 C16 C15 117.9(3) . . ?
C18 C17 C22 119.8(3) . . ?
C18 C17 N4 120.0(3) . . ?
C22 C17 N4 120.2(3) . . ?
C19 C18 C17 120.1(3) . . ?
C20 C19 C18 120.4(3) . . ?
C21 C20 C19 119.6(3) . . ?
C20 C21 C22 120.6(3) . . ?
C21 C22 C17 119.4(3) . . ?
C1 N1 C4 106.0(3) . . ?
C1 N1 Ti1 136.5(2) . . ?
C4 N1 Ti1 117.4(2) . . ?
C5 N2 C6 118.7(3) . . ?
C5 N2 Ti1 113.4(2) . . ?
C6 N2 Ti1 127.33(19) . . ?
C12 N3 C15 106.1(2) . . ?
C12 N3 Ti1 136.6(2) . . ?
C15 N3 Ti1 116.1(2) . . ?
C16 N4 C17 118.3(2) . . ?
C16 N4 Ti1 113.4(2) . . ?
C17 N4 Ti1 127.69(18) . . ?
N3 Ti1 N1 157.90(10) . . ?
N3 Ti1 N4 76.37(10) . . ?
N1 Ti1 N4 87.11(9) . . ?
N3 Ti1 N2 87.13(10) . . ?
N1 Ti1 N2 75.51(10) . . ?
N4 Ti1 N2 80.14(9) . . ?
N3 Ti1 Cl1 91.47(7) . . ?
N1 Ti1 Cl1 102.20(7) . . ?
N4 Ti1 Cl1 165.15(7) . . ?
N2 Ti1 Cl1 90.90(7) . . ?
N3 Ti1 Cl2 104.48(8) . . ?
N1 Ti1 Cl2 90.86(8) . . ?
N4 Ti1 Cl2 93.34(7) . . ?
N2 Ti1 Cl2 165.08(7) . . ?
Cl1 Ti1 Cl2 98.02(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.357
_refine_diff_density_min   -0.420
_refine_diff_density_rms    0.084
