#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/72/1507235.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1507235
loop_
_publ_author_name
'Liguori, Dario'
'Centore, Roberto'
'Tuzi, Angela'
'Grisi, Fabia'
'Sessa, Irene'
'Zambelli, Adolfo'
_publ_section_title
;
 Titanium Monoamidinate−MAO Catalysts:  Some Information
 about Active Species and Stereochemical Polymerization Mechanisms
;
_journal_issue                   15
_journal_name_full               Macromolecules
_journal_page_first              5451
_journal_paper_doi               10.1021/ma034249n
_journal_volume                  36
_journal_year                    2003
_chemical_formula_moiety         'C14 H21 Cl3 N2 Ti'
_chemical_formula_sum            'C14 H21 Cl3 N2 Ti'
_chemical_formula_weight         371.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 110.65(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.679(9)
_cell_length_b                   10.317(6)
_cell_length_c                   14.490(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.79
_cell_measurement_theta_min      12.21
_cell_volume                     1774(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia,!997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.003569
_diffrn_orient_matrix_UB_12      0.029434
_diffrn_orient_matrix_UB_13      -0.066948
_diffrn_orient_matrix_UB_21      -0.053014
_diffrn_orient_matrix_UB_22      -0.072747
_diffrn_orient_matrix_UB_23      -0.030903
_diffrn_orient_matrix_UB_31      -0.065573
_diffrn_orient_matrix_UB_32      0.057230
_diffrn_orient_matrix_UB_33      -0.004825
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4399
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.50
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.8300
_exptl_absorpt_correction_T_min  0.7171
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   2
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0366P)²+0.7716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                2968
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma034249nsi20030226_100911.cif
_cod_data_source_block           precatalyst(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value ' psi-scan ' changed to
'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               1507235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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
C1 C 0.04952(19) 0.8847(2) 0.27421(17) 0.0319(5) Uani 1 1 d .
C2 C 0.0701(2) 1.1200(3) 0.2756(2) 0.0449(7) Uani 1 1 d .
H2 H 0.0635 1.1089 0.2067 0.054 Uiso 1 1 calc R
C3 C 0.1924(3) 1.1478(3) 0.3356(2) 0.0591(9) Uani 1 1 d .
H3A H 0.2015 1.1550 0.4041 0.059 Uiso 1 1 calc R
H3B H 0.2146 1.2276 0.3137 0.059 Uiso 1 1 calc R
H3C H 0.2386 1.0784 0.3271 0.059 Uiso 1 1 calc R
C4 C -0.0056(3) 1.2278(3) 0.2803(3) 0.0742(11) Uani 1 1 d .
H4A H -0.0823 1.2051 0.2429 0.074 Uiso 1 1 calc R
H4B H 0.0145 1.3050 0.2533 0.074 Uiso 1 1 calc R
H4C H 0.0020 1.2430 0.3477 0.074 Uiso 1 1 calc R
C5 C 0.0158(2) 0.6501(2) 0.2974(2) 0.0370(6) Uani 1 1 d .
H5 H 0.0677 0.6404 0.2612 0.037 Uiso 1 1 calc R
C6 C 0.0663(3) 0.5798(3) 0.3951(2) 0.0522(8) Uani 1 1 d .
H6A H 0.1356 0.6212 0.4340 0.052 Uiso 1 1 calc R
H6B H 0.0810 0.4913 0.3833 0.052 Uiso 1 1 calc R
H6C H 0.0144 0.5825 0.4298 0.052 Uiso 1 1 calc R
C7 C -0.0978(2) 0.5949(3) 0.2338(2) 0.0522(8) Uani 1 1 d .
H7A H -0.1486 0.5979 0.2697 0.052 Uiso 1 1 calc R
H7B H -0.0885 0.5067 0.2170 0.052 Uiso 1 1 calc R
H7C H -0.1281 0.6454 0.1746 0.052 Uiso 1 1 calc R
C8 C 0.0988(2) 0.8600(3) 0.19498(19) 0.0402(6) Uani 1 1 d .
H8A H 0.1550 0.7919 0.2165 0.040 Uiso 1 1 calc R
H8B H 0.1360 0.9380 0.1847 0.040 Uiso 1 1 calc R
C9 C 0.0088(2) 0.8206(3) 0.09884(19) 0.0423(6) Uani 1 1 d .
C10 C 0.0244(4) 0.7156(4) 0.0467(2) 0.0704(10) Uani 1 1 d .
H10 H 0.0917 0.6695 0.0701 0.070 Uiso 1 1 calc R
C11 C -0.0588(5) 0.6776(4) -0.0403(3) 0.0986(16) Uani 1 1 d .
H11 H -0.0475 0.6062 -0.0749 0.099 Uiso 1 1 calc R
C12 C -0.1562(4) 0.7442(5) -0.0746(3) 0.0979(16) Uani 1 1 d .
H12 H -0.2122 0.7181 -0.1327 0.098 Uiso 1 1 calc R
C13 C -0.1734(3) 0.8497(5) -0.0248(3) 0.0862(13) Uani 1 1 d .
H13 H -0.2409 0.8953 -0.0490 0.086 Uiso 1 1 calc R
C14 C -0.0906(3) 0.8884(4) 0.0615(2) 0.0620(9) Uani 1 1 d .
H14 H -0.1021 0.9610 0.0948 0.062 Uiso 1 1 calc R
Cl1 Cl -0.15482(6) 0.75272(7) 0.43083(5) 0.04839(19) Uani 1 1 d .
Cl2 Cl -0.22559(5) 0.96813(7) 0.24775(5) 0.04598(18) Uani 1 1 d .
Cl3 Cl 0.10022(5) 0.90188(6) 0.53119(4) 0.04018(16) Uani 1 1 d .
N1 N 0.03540(17) 0.99765(19) 0.30933(15) 0.0337(5) Uani 1 1 d .
N2 N 0.00452(16) 0.78991(19) 0.31405(14) 0.0314(4) Uani 1 1 d .
Ti1 Ti -0.06774(4) 0.91063(4) 0.37707(3) 0.03120(12) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-5 -4 -1
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 N2 109.9(2) . . no
N1 C1 C8 126.6(2) . . no
N2 C1 C8 123.4(2) . . no
N1 C1 Ti1 58.23(13) . . no
N2 C1 Ti1 52.25(12) . . no
C8 C1 Ti1 168.11(17) . . no
N1 C2 C4 110.6(3) . . no
N1 C2 C3 109.7(2) . . no
C4 C2 C3 112.3(3) . . no
N1 C2 H2 108.0 . . no
C4 C2 H2 108.0 . . no
C3 C2 H2 108.0 . . no
C2 C3 H3A 109.5 . . no
C2 C3 H3B 109.5 . . no
H3A C3 H3B 109.5 . . no
C2 C3 H3C 109.5 . . no
H3A C3 H3C 109.5 . . no
H3B C3 H3C 109.5 . . no
C2 C4 H4A 109.5 . . no
C2 C4 H4B 109.5 . . no
H4A C4 H4B 109.5 . . no
C2 C4 H4C 109.5 . . no
H4A C4 H4C 109.5 . . no
H4B C4 H4C 109.5 . . no
N2 C5 C6 110.3(2) . . no
N2 C5 C7 109.8(2) . . no
C6 C5 C7 112.6(2) . . no
N2 C5 H5 108.0 . . no
C6 C5 H5 108.0 . . no
C7 C5 H5 108.0 . . no
C5 C6 H6A 109.5 . . no
C5 C6 H6B 109.5 . . no
H6A C6 H6B 109.5 . . no
C5 C6 H6C 109.5 . . no
H6A C6 H6C 109.5 . . no
H6B C6 H6C 109.5 . . no
C5 C7 H7A 109.5 . . no
C5 C7 H7B 109.5 . . no
H7A C7 H7B 109.5 . . no
C5 C7 H7C 109.5 . . no
H7A C7 H7C 109.5 . . no
H7B C7 H7C 109.5 . . no
C1 C8 C9 111.4(2) . . no
C1 C8 H8A 109.3 . . no
C9 C8 H8A 109.3 . . no
C1 C8 H8B 109.3 . . no
C9 C8 H8B 109.3 . . no
H8A C8 H8B 108.0 . . no
C10 C9 C14 118.3(3) . . no
C10 C9 C8 120.7(3) . . no
C14 C9 C8 121.0(3) . . no
C9 C10 C11 120.8(4) . . no
C9 C10 H10 119.6 . . no
C11 C10 H10 119.6 . . no
C12 C11 C10 119.8(4) . . no
C12 C11 H11 120.1 . . no
C10 C11 H11 120.1 . . no
C11 C12 C13 120.6(4) . . no
C11 C12 H12 119.7 . . no
C13 C12 H12 119.7 . . no
C12 C13 C14 119.8(4) . . no
C12 C13 H13 120.1 . . no
C14 C13 H13 120.1 . . no
C9 C14 C13 120.6(4) . . no
C9 C14 H14 119.7 . . no
C13 C14 H14 119.7 . . no
Ti1 Cl3 Ti1 101.72(4) 3_576 . no
C1 N1 C2 122.4(2) . . no
C1 N1 Ti1 89.66(15) . . no
C2 N1 Ti1 146.12(18) . . no
C1 N2 C5 123.6(2) . . no
C1 N2 Ti1 94.37(15) . . no
C5 N2 Ti1 141.93(17) . . no
N2 Ti1 N1 65.21(9) . . no
N2 Ti1 Cl1 93.92(8) . . no
N1 Ti1 Cl1 159.11(6) . . no
N2 Ti1 Cl2 101.64(8) . . no
N1 Ti1 Cl2 90.89(8) . . no
Cl1 Ti1 Cl2 94.41(5) . . no
N2 Ti1 Cl3 161.55(6) . 3_576 no
N1 Ti1 Cl3 99.63(7) . 3_576 no
Cl1 Ti1 Cl3 100.69(5) . 3_576 no
Cl2 Ti1 Cl3 88.50(5) . 3_576 no
N2 Ti1 C1 33.38(8) . . no
N1 Ti1 C1 32.10(8) . . no
Cl1 Ti1 C1 127.16(7) . . no
Cl2 Ti1 C1 94.19(8) . . no
Cl3 Ti1 C1 131.57(6) 3_576 . no
N2 Ti1 Cl3 90.13(8) . . no
N1 Ti1 Cl3 87.59(8) . . no
Cl1 Ti1 Cl3 91.84(5) . . no
Cl2 Ti1 Cl3 166.24(3) . . no
Cl3 Ti1 Cl3 78.28(4) 3_576 . no
C1 Ti1 Cl3 91.78(8) . . no
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 1.309(3) . no
C1 N2 1.359(3) . no
C1 C8 1.510(4) . no
C1 Ti1 2.463(3) . no
C2 N1 1.475(3) . no
C2 C4 1.486(4) . no
C2 C3 1.513(4) . no
C2 H2 0.9800 . no
C3 H3A 0.9600 . no
C3 H3B 0.9600 . no
C3 H3C 0.9600 . no
C4 H4A 0.9600 . no
C4 H4B 0.9600 . no
C4 H4C 0.9600 . no
C5 N2 1.478(3) . no
C5 C6 1.517(4) . no
C5 C7 1.521(4) . no
C5 H5 0.9800 . no
C6 H6A 0.9600 . no
C6 H6B 0.9600 . no
C6 H6C 0.9600 . no
C7 H7A 0.9600 . no
C7 H7B 0.9600 . no
C7 H7C 0.9600 . no
C8 C9 1.513(4) . no
C8 H8A 0.9700 . no
C8 H8B 0.9700 . no
C9 C10 1.375(4) . no
C9 C14 1.375(4) . no
C10 C11 1.385(5) . no
C10 H10 0.9300 . no
C11 C12 1.345(6) . no
C11 H11 0.9300 . no
C12 C13 1.366(6) . no
C12 H12 0.9300 . no
C13 C14 1.378(5) . no
C13 H13 0.9300 . no
C14 H14 0.9300 . no
Cl1 Ti1 2.2553(12) . no
Cl2 Ti1 2.2855(17) . no
Cl3 Ti1 2.4625(13) 3_576 no
Cl3 Ti1 2.4852(19) . no
N1 Ti1 2.094(2) . no
N2 Ti1 1.953(2) . no
Ti1 Cl3 2.4625(13) 3_576 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C8 C9 -106.9(3) . . no
N2 C1 C8 C9 67.6(3) . . no
Ti1 C1 C8 C9 3.0(10) . . no
C1 C8 C9 C10 -132.7(3) . . no
C1 C8 C9 C14 47.1(4) . . no
C14 C9 C10 C11 -1.3(5) . . no
C8 C9 C10 C11 178.6(3) . . no
C9 C10 C11 C12 0.2(7) . . no
C10 C11 C12 C13 0.5(7) . . no
C11 C12 C13 C14 -0.1(7) . . no
C10 C9 C14 C13 1.6(5) . . no
C8 C9 C14 C13 -178.3(3) . . no
C12 C13 C14 C9 -0.9(6) . . no
N2 C1 N1 C2 -176.6(2) . . no
C8 C1 N1 C2 -1.5(4) . . no
Ti1 C1 N1 C2 -168.4(2) . . no
N2 C1 N1 Ti1 -8.27(18) . . no
C8 C1 N1 Ti1 166.8(2) . . no
C4 C2 N1 C1 148.6(3) . . no
C3 C2 N1 C1 -87.0(3) . . no
C4 C2 N1 Ti1 -10.2(4) . . no
C3 C2 N1 Ti1 114.2(3) . . no
N1 C1 N2 C5 -173.9(2) . . no
C8 C1 N2 C5 10.8(3) . . no
Ti1 C1 N2 C5 177.2(3) . . no
N1 C1 N2 Ti1 8.9(2) . . no
C8 C1 N2 Ti1 -166.4(2) . . no
C6 C5 N2 C1 124.8(3) . . no
C7 C5 N2 C1 -110.5(3) . . no
C6 C5 N2 Ti1 -59.7(3) . . no
C7 C5 N2 Ti1 65.0(4) . . no
C1 N2 Ti1 N1 -5.74(13) . . no
C5 N2 Ti1 N1 178.0(3) . . no
C1 N2 Ti1 Cl1 175.12(13) . . no
C5 N2 Ti1 Cl1 -1.1(3) . . no
C1 N2 Ti1 Cl2 79.80(14) . . no
C5 N2 Ti1 Cl2 -96.5(3) . . no
C1 N2 Ti1 Cl3 -42.4(3) . 3_576 no
C5 N2 Ti1 Cl3 141.3(2) . 3_576 no
C5 N2 Ti1 C1 -176.3(3) . . no
C1 N2 Ti1 Cl3 -93.02(13) . . no
C5 N2 Ti1 Cl3 90.7(3) . . no
C1 N1 Ti1 N2 5.95(13) . . no
C2 N1 Ti1 N2 168.1(3) . . no
C1 N1 Ti1 Cl1 8.4(3) . . no
C2 N1 Ti1 Cl1 170.6(2) . . no
C1 N1 Ti1 Cl2 -96.47(14) . . no
C2 N1 Ti1 Cl2 65.7(3) . . no
C1 N1 Ti1 Cl3 174.90(13) . 3_576 no
C2 N1 Ti1 Cl3 -22.9(3) . 3_576 no
C2 N1 Ti1 C1 162.2(4) . . no
C1 N1 Ti1 Cl3 97.21(14) . . no
C2 N1 Ti1 Cl3 -100.6(3) . . no
N1 C1 Ti1 N2 -170.2(2) . . no
C8 C1 Ti1 N2 72.5(9) . . no
N2 C1 Ti1 N1 170.2(2) . . no
C8 C1 Ti1 N1 -117.4(9) . . no
N1 C1 Ti1 Cl1 -176.26(12) . . no
N2 C1 Ti1 Cl1 -6.11(16) . . no
C8 C1 Ti1 Cl1 66.4(9) . . no
N1 C1 Ti1 Cl2 84.98(14) . . no
N2 C1 Ti1 Cl2 -104.86(13) . . no
C8 C1 Ti1 Cl2 -32.4(9) . . no
N1 C1 Ti1 Cl3 -6.73(17) . 3_576 no
N2 C1 Ti1 Cl3 163.42(11) . 3_576 no
C8 C1 Ti1 Cl3 -124.1(9) . 3_576 no
N1 C1 Ti1 Cl3 -82.60(13) . . no
N2 C1 Ti1 Cl3 87.55(13) . . no
C8 C1 Ti1 Cl3 160.0(9) . . no
Ti1 Cl3 Ti1 N2 165.53(7) 3_576 . no
Ti1 Cl3 Ti1 N1 100.35(7) 3_576 . no
Ti1 Cl3 Ti1 Cl1 -100.54(6) 3_576 . no
Ti1 Cl3 Ti1 Cl2 16.50(15) 3_576 . no
Ti1 Cl3 Ti1 Cl3 0.0 3_576 3_576 no
Ti1 Cl3 Ti1 C1 132.19(6) 3_576 . no
