#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007959.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_7007959
loop_
_publ_author_name
'Pennington, Dale A.'
'Clegg, William'
'Coles, Simon J.'
'Harrington, Ross W.'
'Hursthouse, Michael B.'
'Hughes, David L.'
'Light, Mark E.'
'Schormann, Mark'
'Bochmann, Manfred'
'Lancaster, Simon J.'
_publ_section_title
;
 The synthesis, structure and ethene polymerisation catalysis of
 mono(salicylaldiminato) titanium and zirconium complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              561
_journal_page_last               571
_journal_paper_doi               10.1039/b414229b
_journal_year                    2005
_chemical_formula_moiety         'C15 H21 Cl3 O3 Ti'
_chemical_formula_structural     '[TiCl3(thf)(OC6H3tBu-6,-CHO-2)]'
_chemical_formula_sum            'C15 H21 Cl3 O3 Ti'
_chemical_formula_weight         403.57
_chemical_name_common            'Complex 7'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.350(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5359(4)
_cell_length_b                   8.3775(4)
_cell_length_c                   20.2839(10)
_cell_measurement_reflns_used    55955
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.91
_cell_volume                     1755.34(14)
_computing_cell_refinement       'DENZO (Otwinowski and MInor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO, COLLECT, MAXUS (Mackay et al., 1998)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '9.091 pixels mm^1^'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Nonius Kappa CCD Area detector'
_diffrn_measurement_method       'φ and ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19393
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.7633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.032
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       0.024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.1491
_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)+(0.0000P)²+100.6789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3535
_refine_ls_wR_factor_ref         0.3641
_reflns_number_gt                3016
_reflns_number_total             3826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414229b.txt
_cod_data_source_block           03src0767
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1755.33(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7007959
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'
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 0.3650(12) -0.0154(16) 0.2532(6) 0.018(3) Uani 1 1 d . . .
H1 H 0.3483 -0.0937 0.2843 0.021 Uiso 1 1 calc R . .
C2 C 0.4541(13) 0.1090(15) 0.2790(6) 0.019(3) Uani 1 1 d . . .
C3 C 0.5253(13) 0.0965(15) 0.3456(6) 0.020(3) Uani 1 1 d . . .
H3 H 0.5170 0.0049 0.3720 0.024 Uiso 1 1 calc R . .
C4 C 0.6057(12) 0.2179(16) 0.3711(6) 0.020(3) Uani 1 1 d . . .
H4 H 0.6565 0.2090 0.4151 0.023 Uiso 1 1 calc R . .
C5 C 0.6149(13) 0.3561(18) 0.3332(6) 0.024(3) Uani 1 1 d . . .
H5 H 0.6715 0.4388 0.3529 0.029 Uiso 1 1 calc R . .
C6 C 0.5441(11) 0.3778(15) 0.2674(6) 0.015(2) Uani 1 1 d . . .
C7 C 0.4655(14) 0.2512(17) 0.2415(7) 0.025(3) Uani 1 1 d . . .
C8 C 0.5547(13) 0.5276(16) 0.2265(7) 0.023(3) Uani 1 1 d . . .
C9 C 0.4171(13) 0.5974(16) 0.2018(7) 0.024(3) Uani 1 1 d . . .
H9A H 0.3638 0.5197 0.1725 0.037 Uiso 1 1 calc R . .
H9B H 0.4232 0.6960 0.1766 0.037 Uiso 1 1 calc R . .
H9C H 0.3775 0.6205 0.2406 0.037 Uiso 1 1 calc R . .
C10 C 0.6378(15) 0.6551(17) 0.2688(8) 0.031(3) Uani 1 1 d . . .
H10A H 0.5981 0.6847 0.3069 0.047 Uiso 1 1 calc R . .
H10B H 0.6435 0.7494 0.2410 0.047 Uiso 1 1 calc R . .
H10C H 0.7248 0.6126 0.2856 0.047 Uiso 1 1 calc R . .
C11 C 0.6160(13) 0.4850(16) 0.1654(6) 0.022(3) Uani 1 1 d . . .
H11A H 0.7049 0.4476 0.1812 0.033 Uiso 1 1 calc R . .
H11B H 0.6168 0.5798 0.1372 0.033 Uiso 1 1 calc R . .
H11C H 0.5651 0.4006 0.1390 0.033 Uiso 1 1 calc R . .
C12 C 0.1510(13) -0.1824(18) 0.0634(7) 0.026(3) Uani 1 1 d . . .
H12A H 0.0706 -0.1245 0.0435 0.031 Uiso 1 1 calc R . .
H12B H 0.1506 -0.2040 0.1113 0.031 Uiso 1 1 calc R . .
C13 C 0.1605(14) -0.3346(17) 0.0264(7) 0.028(3) Uani 1 1 d . . .
H13A H 0.0738 -0.3763 0.0060 0.034 Uiso 1 1 calc R . .
H13B H 0.2086 -0.4169 0.0564 0.034 Uiso 1 1 calc R . .
C14 C 0.2350(15) -0.2827(19) -0.0274(7) 0.031(3) Uani 1 1 d . . .
H14A H 0.2751 -0.3751 -0.0458 0.038 Uiso 1 1 calc R . .
H14B H 0.1782 -0.2255 -0.0646 0.038 Uiso 1 1 calc R . .
C15 C 0.3344(15) -0.1749(19) 0.0111(7) 0.030(3) Uani 1 1 d . . .
H15A H 0.4081 -0.2364 0.0368 0.036 Uiso 1 1 calc R . .
H15B H 0.3671 -0.0993 -0.0192 0.036 Uiso 1 1 calc R . .
O1 O 0.3068(9) -0.0305(11) 0.1932(5) 0.023(2) Uani 1 1 d . . .
O2 O 0.3977(8) 0.2562(10) 0.1789(4) 0.0169(18) Uani 1 1 d . . .
O3 O 0.2637(9) -0.0899(11) 0.0568(5) 0.023(2) Uani 1 1 d . . .
Cl1 Cl 0.5337(3) -0.0062(4) 0.12706(16) 0.0223(8) Uani 1 1 d . . .
Cl2 Cl 0.1174(3) 0.1860(4) 0.10483(17) 0.0252(8) Uani 1 1 d . . .
Cl3 Cl 0.3602(3) 0.2608(4) 0.02330(16) 0.0264(8) Uani 1 1 d . . .
Ti1 Ti 0.3325(2) 0.1140(3) 0.11268(11) 0.0173(6) 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'
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'
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 C1 C2 126.0(11) . . ?
O1 C1 H1 117.0 . . ?
C2 C1 H1 117.0 . . ?
C3 C2 C1 118.8(11) . . ?
C3 C2 C7 119.1(12) . . ?
C1 C2 C7 122.0(11) . . ?
C4 C3 C2 118.8(12) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 120.9(11) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 123.0(13) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C7 C6 C5 115.3(12) . . ?
C7 C6 C8 121.9(11) . . ?
C5 C6 C8 122.8(12) . . ?
O2 C7 C6 120.5(12) . . ?
O2 C7 C2 116.6(12) . . ?
C6 C7 C2 122.9(12) . . ?
C6 C8 C10 111.5(11) . . ?
C6 C8 C11 109.5(11) . . ?
C10 C8 C11 109.1(11) . . ?
C6 C8 C9 108.8(10) . . ?
C10 C8 C9 108.2(11) . . ?
C11 C8 C9 109.7(11) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 C13 105.9(11) . . ?
O3 C12 H12A 110.6 . . ?
C13 C12 H12A 110.6 . . ?
O3 C12 H12B 110.6 . . ?
C13 C12 H12B 110.6 . . ?
H12A C12 H12B 108.7 . . ?
C12 C13 C14 102.2(11) . . ?
C12 C13 H13A 111.3 . . ?
C14 C13 H13A 111.3 . . ?
C12 C13 H13B 111.3 . . ?
C14 C13 H13B 111.3 . . ?
H13A C13 H13B 109.2 . . ?
C15 C14 C13 102.0(11) . . ?
C15 C14 H14A 111.4 . . ?
C13 C14 H14A 111.4 . . ?
C15 C14 H14B 111.4 . . ?
C13 C14 H14B 111.4 . . ?
H14A C14 H14B 109.2 . . ?
O3 C15 C14 103.3(11) . . ?
O3 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
O3 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C1 O1 Ti1 125.7(9) . . ?
C7 O2 Ti1 137.4(8) . . ?
C12 O3 C15 108.9(10) . . ?
C12 O3 Ti1 126.1(8) . . ?
C15 O3 Ti1 124.5(8) . . ?
O2 Ti1 O1 83.7(4) . . ?
O2 Ti1 O3 165.6(4) . . ?
O1 Ti1 O3 82.4(4) . . ?
O2 Ti1 Cl3 98.4(3) . . ?
O1 Ti1 Cl3 177.7(3) . . ?
O3 Ti1 Cl3 95.4(3) . . ?
O2 Ti1 Cl1 89.3(3) . . ?
O1 Ti1 Cl1 84.6(3) . . ?
O3 Ti1 Cl1 85.7(3) . . ?
Cl3 Ti1 Cl1 94.52(15) . . ?
O2 Ti1 Cl2 95.9(3) . . ?
O1 Ti1 Cl2 85.9(3) . . ?
O3 Ti1 Cl2 86.9(3) . . ?
Cl3 Ti1 Cl2 94.70(15) . . ?
Cl1 Ti1 Cl2 168.64(17) . . ?
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 O1 1.257(15) . ?
C1 C2 1.431(18) . ?
C1 H1 0.9500 . ?
C2 C3 1.413(17) . ?
C2 C7 1.431(18) . ?
C3 C4 1.359(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(19) . ?
C6 C8 1.520(18) . ?
C7 O2 1.330(16) . ?
C8 C10 1.532(18) . ?
C8 C11 1.549(18) . ?
C8 C9 1.552(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 O3 1.446(16) . ?
C12 C13 1.49(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.53(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.48(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O3 1.481(16) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O1 Ti1 2.094(9) . ?
O2 Ti1 1.825(9) . ?
O3 Ti1 2.100(9) . ?
Cl1 Ti1 2.312(4) . ?
Cl2 Ti1 2.321(4) . ?
Cl3 Ti1 2.256(4) . ?
