#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007955.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_7007955
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         'C21 H21 Cl3 F5 N O2 Ti'
_chemical_formula_structural     '[TiCl3(thf)(OC6H3tBu-6,-CHNC6F5-2)]'
_chemical_formula_sum            'C21 H21 Cl3 F5 N O2 Ti'
_chemical_formula_weight         568.64
_chemical_name_common            'Complex 5e'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.5740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2176(2)
_cell_length_b                   34.4138(9)
_cell_length_c                   9.3904(2)
_cell_measurement_reflns_used    18362
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2317.10(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25995
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_correction_T_min  0.8358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0015(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   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0438
_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)+(0.0317P)²+0.6385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3410
_reflns_number_total             5294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414229b.txt
_cod_data_source_block           03src0743
_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_sg_symbol_H-M      P2(1)/c
_cod_database_code               7007955
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'
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 0.2381(3) 0.11079(8) 0.3496(3) 0.0209(6) Uani 1 1 d . . .
C2 C 0.2159(4) 0.12887(8) 0.2183(3) 0.0243(7) Uani 1 1 d . . .
C3 C 0.1355(4) 0.11074(9) 0.0958(3) 0.0321(8) Uani 1 1 d . . .
C4 C 0.0672(4) 0.07372(10) 0.1063(3) 0.0341(8) Uani 1 1 d . . .
C5 C 0.0856(4) 0.05508(9) 0.2356(4) 0.0295(7) Uani 1 1 d . . .
C6 C 0.1716(4) 0.07306(8) 0.3559(3) 0.0238(7) Uani 1 1 d . . .
C7 C 0.2337(4) 0.15923(8) 0.5159(3) 0.0187(6) Uani 1 1 d . . .
H7 H 0.1148 0.1636 0.4637 0.022 Uiso 1 1 calc R . .
C8 C 0.2871(3) 0.18514(7) 0.6324(3) 0.0178(6) Uani 1 1 d . . .
C9 C 0.1686(4) 0.21643(7) 0.6533(3) 0.0206(6) Uani 1 1 d . . .
H9 H 0.0580 0.2204 0.5898 0.025 Uiso 1 1 calc R . .
C10 C 0.2141(4) 0.24124(8) 0.7666(3) 0.0233(6) Uani 1 1 d . . .
H10 H 0.1381 0.2632 0.7794 0.028 Uiso 1 1 calc R . .
C11 C 0.3723(4) 0.23407(8) 0.8629(3) 0.0221(6) Uani 1 1 d . . .
H11 H 0.3994 0.2514 0.9413 0.026 Uiso 1 1 calc R . .
C12 C 0.4923(4) 0.20303(7) 0.8506(3) 0.0187(6) Uani 1 1 d . . .
C13 C 0.4495(3) 0.17948(7) 0.7291(3) 0.0166(6) Uani 1 1 d . . .
C14 C 0.6640(4) 0.19598(8) 0.9585(3) 0.0214(6) Uani 1 1 d . . .
C15 C 0.8393(4) 0.20492(8) 0.8864(3) 0.0252(7) Uani 1 1 d . . .
H15A H 0.8440 0.1877 0.8037 0.038 Uiso 1 1 calc R . .
H15B H 0.9503 0.2007 0.9552 0.038 Uiso 1 1 calc R . .
H15C H 0.8359 0.2320 0.8544 0.038 Uiso 1 1 calc R . .
C16 C 0.6712(4) 0.15391(8) 1.0145(3) 0.0247(7) Uani 1 1 d . . .
H16A H 0.5512 0.1472 1.0474 0.037 Uiso 1 1 calc R . .
H16B H 0.7704 0.1515 1.0945 0.037 Uiso 1 1 calc R . .
H16C H 0.6966 0.1362 0.9373 0.037 Uiso 1 1 calc R . .
C17 C 0.6653(4) 0.22292(8) 1.0884(3) 0.0284(7) Uani 1 1 d . . .
H17A H 0.6635 0.2500 1.0564 0.043 Uiso 1 1 calc R . .
H17B H 0.7782 0.2182 1.1546 0.043 Uiso 1 1 calc R . .
H17C H 0.5550 0.2178 1.1375 0.043 Uiso 1 1 calc R . .
C18 C 0.6109(4) 0.03349(8) 0.6714(4) 0.0351(8) Uani 1 1 d . . .
H18A H 0.7482 0.0341 0.6726 0.042 Uiso 1 1 calc R . .
H18B H 0.5566 0.0187 0.5864 0.042 Uiso 1 1 calc R . .
C19 C 0.5573(4) 0.01582(9) 0.8058(4) 0.0377(8) Uani 1 1 d . . .
H19A H 0.6506 0.0218 0.8887 0.045 Uiso 1 1 calc R . .
H19B H 0.5436 -0.0127 0.7964 0.045 Uiso 1 1 calc R . .
C20 C 0.3730(4) 0.03494(9) 0.8215(4) 0.0446(9) Uani 1 1 d . . .
H20A H 0.2706 0.0226 0.7580 0.054 Uiso 1 1 calc R . .
H20B H 0.3436 0.0336 0.9218 0.054 Uiso 1 1 calc R . .
C21 C 0.4036(4) 0.07620(8) 0.7773(3) 0.0271(7) Uani 1 1 d . . .
H21A H 0.2851 0.0883 0.7357 0.033 Uiso 1 1 calc R . .
H21B H 0.4575 0.0920 0.8601 0.033 Uiso 1 1 calc R . .
N1 N 0.3295(3) 0.13042(6) 0.4733(2) 0.0187(5) Uani 1 1 d . . .
O1 O 0.5617(2) 0.15016(5) 0.70045(19) 0.0183(4) Uani 1 1 d . . .
O2 O 0.5348(2) 0.07286(5) 0.6697(2) 0.0225(4) Uani 1 1 d . . .
F1 F 0.2770(2) 0.16563(5) 0.20592(17) 0.0311(4) Uani 1 1 d . . .
F2 F 0.1229(3) 0.12878(6) -0.03054(19) 0.0442(5) Uani 1 1 d . . .
F3 F -0.0164(3) 0.05567(6) -0.0108(2) 0.0504(6) Uani 1 1 d . . .
F4 F 0.0195(2) 0.01892(5) 0.2458(2) 0.0433(5) Uani 1 1 d . . .
F5 F 0.1932(2) 0.05363(4) 0.47989(18) 0.0317(4) Uani 1 1 d . . .
Cl1 Cl 0.63686(9) 0.07814(2) 0.36360(8) 0.02882(19) Uani 1 1 d . . .
Cl2 Cl 0.92246(9) 0.10675(2) 0.65712(8) 0.02579(18) Uani 1 1 d . . .
Cl3 Cl 0.70850(9) 0.17256(2) 0.42886(8) 0.02631(18) Uani 1 1 d . . .
Ti1 Ti 0.63001(6) 0.119965(14) 0.55626(5) 0.01816(13) 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'
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'
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'
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
C2 C1 C6 117.2(3) . . ?
C2 C1 N1 120.5(2) . . ?
C6 C1 N1 122.3(3) . . ?
F1 C2 C1 119.8(2) . . ?
F1 C2 C3 117.6(3) . . ?
C1 C2 C3 122.6(3) . . ?
F2 C3 C4 120.5(3) . . ?
F2 C3 C2 120.8(3) . . ?
C4 C3 C2 118.7(3) . . ?
F3 C4 C5 119.9(3) . . ?
F3 C4 C3 120.1(3) . . ?
C5 C4 C3 120.0(3) . . ?
F4 C5 C4 120.0(3) . . ?
F4 C5 C6 119.4(3) . . ?
C4 C5 C6 120.6(3) . . ?
F5 C6 C5 119.2(3) . . ?
F5 C6 C1 119.9(2) . . ?
C5 C6 C1 120.9(3) . . ?
N1 C7 C8 127.2(2) . . ?
N1 C7 H7 116.4 . . ?
C8 C7 H7 116.4 . . ?
C9 C8 C13 119.4(2) . . ?
C9 C8 C7 118.0(2) . . ?
C13 C8 C7 122.5(2) . . ?
C10 C9 C8 119.3(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 119.8(3) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 123.7(3) . . ?
C12 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
C11 C12 C13 115.5(2) . . ?
C11 C12 C14 122.3(2) . . ?
C13 C12 C14 122.2(2) . . ?
O1 C13 C12 121.0(2) . . ?
O1 C13 C8 116.8(2) . . ?
C12 C13 C8 122.1(2) . . ?
C12 C14 C17 111.3(2) . . ?
C12 C14 C15 108.9(2) . . ?
C17 C14 C15 107.5(2) . . ?
C12 C14 C16 111.7(2) . . ?
C17 C14 C16 107.5(2) . . ?
C15 C14 C16 110.0(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 C19 104.7(2) . . ?
O2 C18 H18A 110.8 . . ?
C19 C18 H18A 110.8 . . ?
O2 C18 H18B 110.8 . . ?
C19 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C18 C19 C20 102.8(3) . . ?
C18 C19 H19A 111.2 . . ?
C20 C19 H19A 111.2 . . ?
C18 C19 H19B 111.2 . . ?
C20 C19 H19B 111.2 . . ?
H19A C19 H19B 109.1 . . ?
C21 C20 C19 103.1(2) . . ?
C21 C20 H20A 111.1 . . ?
C19 C20 H20A 111.1 . . ?
C21 C20 H20B 111.1 . . ?
C19 C20 H20B 111.1 . . ?
H20A C20 H20B 109.1 . . ?
O2 C21 C20 104.1(2) . . ?
O2 C21 H21A 110.9 . . ?
C20 C21 H21A 110.9 . . ?
O2 C21 H21B 110.9 . . ?
C20 C21 H21B 110.9 . . ?
H21A C21 H21B 109.0 . . ?
C7 N1 C1 113.4(2) . . ?
C7 N1 Ti1 122.87(17) . . ?
C1 N1 Ti1 122.68(16) . . ?
C13 O1 Ti1 143.21(17) . . ?
C18 O2 C21 109.7(2) . . ?
C18 O2 Ti1 125.26(17) . . ?
C21 O2 Ti1 124.35(16) . . ?
O1 Ti1 O2 86.04(8) . . ?
O1 Ti1 N1 80.41(8) . . ?
O2 Ti1 N1 86.59(8) . . ?
O1 Ti1 Cl2 97.06(6) . . ?
O2 Ti1 Cl2 88.63(5) . . ?
N1 Ti1 Cl2 174.73(6) . . ?
O1 Ti1 Cl3 92.40(6) . . ?
O2 Ti1 Cl3 175.31(6) . . ?
N1 Ti1 Cl3 88.80(6) . . ?
Cl2 Ti1 Cl3 95.95(3) . . ?
O1 Ti1 Cl1 165.45(6) . . ?
O2 Ti1 Cl1 87.36(6) . . ?
N1 Ti1 Cl1 86.28(6) . . ?
Cl2 Ti1 Cl1 95.73(3) . . ?
Cl3 Ti1 Cl1 93.14(3) . . ?
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 C2 1.373(4) . ?
C1 C6 1.388(4) . ?
C1 N1 1.437(3) . ?
C2 F1 1.349(3) . ?
C2 C3 1.377(4) . ?
C3 F2 1.333(4) . ?
C3 C4 1.374(4) . ?
C4 F3 1.344(3) . ?
C4 C5 1.366(4) . ?
C5 F4 1.340(3) . ?
C5 C6 1.372(4) . ?
C6 F5 1.337(3) . ?
C7 N1 1.297(3) . ?
C7 C8 1.430(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(4) . ?
C8 C13 1.411(4) . ?
C9 C10 1.375(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.405(4) . ?
C12 C14 1.528(4) . ?
C13 O1 1.340(3) . ?
C14 C17 1.532(4) . ?
C14 C15 1.533(4) . ?
C14 C16 1.540(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O2 1.462(3) . ?
C18 C19 1.492(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.506(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.503(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O2 1.466(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
N1 Ti1 2.248(2) . ?
O1 Ti1 1.8191(18) . ?
O2 Ti1 2.0981(19) . ?
Cl1 Ti1 2.3169(8) . ?
Cl2 Ti1 2.2587(8) . ?
Cl3 Ti1 2.2768(8) . ?
