#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:05:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178594 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/05/4070595.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_4070595
loop_
_publ_author_name
'Ye, Wei-Ping'
'Zhan, Jie'
'Pan, Li'
'Hu, Ning-Hai'
'Li, Yue-Sheng'
_publ_section_title
;
 Synthesis and Characterization of Titanium Complexes Bearing Two
 β-Enaminoketonato Ligands with Electron-Withdrawing Groups and Their
 Behavior in Ethylene Polymerization
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3642
_journal_paper_doi               10.1021/om700803u
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C30 H28 Cl2 F12 N2 O2 Ti'
_chemical_formula_weight         795.34
_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                 102.9830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6966(9)
_cell_length_b                   8.6009(8)
_cell_length_c                   20.8763(19)
_cell_measurement_reflns_used    2230
_cell_measurement_temperature    187(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.57
_cell_volume                     1696.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      187(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9112
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.9688
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.063
_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     226
_refine_ls_number_reflns         3322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0550P)²+0.6785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                2626
_reflns_number_total             3322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700803u-file001.cif
_cod_data_source_block           q383
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4070595
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
Ti1 Ti 1.0000 0.5000 0.0000 0.02053(17) Uani 1 2 d S
Cl1 Cl 1.19264(7) 0.34117(8) 0.03335(3) 0.03311(19) Uani 1 1 d .
F1 F 1.3909(2) 0.4300(2) 0.18248(9) 0.0597(5) Uani 1 1 d .
F2 F 1.17347(18) 0.39069(18) 0.18423(8) 0.0449(4) Uani 1 1 d .
F3 F 1.3130(2) 0.4992(2) 0.26599(8) 0.0558(5) Uani 1 1 d .
F4 F 0.8998(2) 0.8041(2) 0.18194(10) 0.0706(6) Uani 1 1 d .
F5 F 1.0169(2) 0.6284(3) 0.24077(9) 0.0713(6) Uani 1 1 d .
F6 F 0.7926(2) 0.6200(3) 0.21622(10) 0.0735(7) Uani 1 1 d .
N1 N 1.0104(2) 0.5868(2) 0.09876(9) 0.0231(4) Uani 1 1 d .
O1 O 0.87876(17) 0.34749(19) 0.02381(8) 0.0253(4) Uani 1 1 d .
C1 C 1.1233(3) 0.6948(3) 0.12558(11) 0.0261(6) Uani 1 1 d .
C2 C 1.2460(3) 0.6525(3) 0.17097(12) 0.0315(6) Uani 1 1 d .
C3 C 1.3482(3) 0.7669(4) 0.19371(13) 0.0438(8) Uani 1 1 d .
H3 H 1.4327 0.7395 0.2245 0.053 Uiso 1 1 calc R
C4 C 1.3286(4) 0.9175(4) 0.17236(15) 0.0499(8) Uani 1 1 d .
H4 H 1.3985 0.9938 0.1888 0.060 Uiso 1 1 calc R
C5 C 1.2077(4) 0.9585(3) 0.12713(15) 0.0444(8) Uani 1 1 d .
H5 H 1.1941 1.0631 0.1124 0.053 Uiso 1 1 calc R
C6 C 1.1061(3) 0.8479(3) 0.10318(12) 0.0318(6) Uani 1 1 d .
H6 H 1.0238 0.8762 0.0712 0.038 Uiso 1 1 calc R
C7 C 1.2781(3) 0.4936(4) 0.19990(13) 0.0399(7) Uani 1 1 d .
C8 C 0.9087(3) 0.5608(3) 0.12998(12) 0.0279(6) Uani 1 1 d .
C9 C 0.9045(3) 0.6534(4) 0.19290(14) 0.0407(7) Uani 1 1 d .
C10 C 0.7978(3) 0.4542(3) 0.11080(12) 0.0311(6) Uani 1 1 d .
H10 H 0.7244 0.4555 0.1342 0.037 Uiso 1 1 calc R
C11 C 0.7870(2) 0.3479(3) 0.06075(12) 0.0247(5) Uani 1 1 d .
C12 C 0.6726(3) 0.2249(3) 0.04500(13) 0.0306(6) Uani 1 1 d .
C13 C 0.5751(3) 0.2254(4) 0.09372(15) 0.0438(7) Uani 1 1 d .
H13A H 0.6318 0.2101 0.1384 0.066 Uiso 1 1 calc R
H13B H 0.5057 0.1412 0.0827 0.066 Uiso 1 1 calc R
H13C H 0.5255 0.3253 0.0911 0.066 Uiso 1 1 calc R
C14 C 0.5844(3) 0.2611(4) -0.02404(14) 0.0427(7) Uani 1 1 d .
H14A H 0.5359 0.3609 -0.0234 0.064 Uiso 1 1 calc R
H14B H 0.5142 0.1788 -0.0379 0.064 Uiso 1 1 calc R
H14C H 0.6468 0.2669 -0.0550 0.064 Uiso 1 1 calc R
C15 C 0.7456(3) 0.0668(3) 0.04671(17) 0.0475(8) Uani 1 1 d .
H15A H 0.8106 0.0683 0.0169 0.071 Uiso 1 1 calc R
H15B H 0.6742 -0.0144 0.0328 0.071 Uiso 1 1 calc R
H15C H 0.7989 0.0451 0.0916 0.071 Uiso 1 1 calc R
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
O1 Ti1 O1 180.0 . 3_765
O1 Ti1 N1 96.39(7) . 3_765
O1 Ti1 N1 83.61(7) 3_765 3_765
O1 Ti1 N1 83.61(7) . .
O1 Ti1 N1 96.39(7) 3_765 .
N1 Ti1 N1 180.00(10) 3_765 .
O1 Ti1 Cl1 88.91(5) . 3_765
O1 Ti1 Cl1 91.09(5) 3_765 3_765
N1 Ti1 Cl1 93.18(5) 3_765 3_765
N1 Ti1 Cl1 86.82(5) . 3_765
O1 Ti1 Cl1 91.09(5) . .
O1 Ti1 Cl1 88.91(5) 3_765 .
N1 Ti1 Cl1 86.82(5) 3_765 .
N1 Ti1 Cl1 93.18(5) . .
Cl1 Ti1 Cl1 180.0 3_765 .
C8 N1 C1 120.2(2) . .
C8 N1 Ti1 122.02(16) . .
C1 N1 Ti1 117.18(14) . .
C11 O1 Ti1 134.28(15) . .
C2 C1 C6 119.6(2) . .
C2 C1 N1 123.4(2) . .
C6 C1 N1 116.9(2) . .
C1 C2 C3 118.6(3) . .
C1 C2 C7 125.5(2) . .
C3 C2 C7 115.9(2) . .
C4 C3 C2 121.2(3) . .
C3 C4 C5 120.0(3) . .
C6 C5 C4 120.0(3) . .
C5 C6 C1 120.5(3) . .
F2 C7 F3 106.1(2) . .
F2 C7 F1 106.5(2) . .
F3 C7 F1 105.1(2) . .
F2 C7 C2 115.5(2) . .
F3 C7 C2 111.2(2) . .
F1 C7 C2 111.7(2) . .
N1 C8 C10 125.6(2) . .
N1 C8 C9 119.9(2) . .
C10 C8 C9 114.5(2) . .
F4 C9 F6 106.3(3) . .
F4 C9 F5 106.4(3) . .
F6 C9 F5 107.1(2) . .
F4 C9 C8 111.5(2) . .
F6 C9 C8 112.6(2) . .
F5 C9 C8 112.6(2) . .
C11 C10 C8 125.1(2) . .
O1 C11 C10 120.5(2) . .
O1 C11 C12 115.7(2) . .
C10 C11 C12 123.8(2) . .
C11 C12 C15 107.7(2) . .
C11 C12 C14 106.8(2) . .
C15 C12 C14 111.1(2) . .
C11 C12 C13 112.6(2) . .
C15 C12 C13 109.7(2) . .
C14 C12 C13 109.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.9006(15) .
Ti1 O1 1.9006(15) 3_765
Ti1 N1 2.1736(19) 3_765
Ti1 N1 2.1736(19) .
Ti1 Cl1 2.2926(6) 3_765
Ti1 Cl1 2.2926(6) .
F1 C7 1.344(3) .
F2 C7 1.330(3) .
F3 C7 1.345(3) .
F4 C9 1.316(3) .
F5 C9 1.321(4) .
F6 C9 1.317(3) .
N1 C8 1.318(3) .
N1 C1 1.449(3) .
O1 C11 1.302(3) .
C1 C2 1.392(4) .
C1 C6 1.394(4) .
C2 C3 1.402(4) .
C2 C7 1.499(4) .
C3 C4 1.369(5) .
C4 C5 1.376(5) .
C5 C6 1.380(4) .
C8 C10 1.402(4) .
C8 C9 1.545(4) .
C10 C11 1.374(3) .
C11 C12 1.515(3) .
C12 C15 1.530(4) .
C12 C14 1.534(4) .
C12 C13 1.536(4) .
