#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:14:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179915 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/10/7021036.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_7021036
loop_
_publ_author_name
'Suttil, James A.'
'McGuinness, David S.'
'Gardiner, Michael G.'
'Evans, Stephen J.'
_publ_section_title
;
 Ethylene polymerisation and oligomerisation with arene-substituted
 phenoxy-imine complexes of titanium: investigation of multi-mechanism
 catalytic behaviour.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4185
_journal_page_last               4196
_journal_paper_doi               10.1039/c3dt32183e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C32 H34 Cl4 N2 O2 Ti'
_chemical_formula_weight         668.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   22.5011(13)
_cell_length_b                   22.5011(13)
_cell_length_c                   18.1552(13)
_cell_measurement_reflns_used    24912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.94
_cell_volume                     7960.5(9)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)'
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'ADSC Q315'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  '3-ID1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'Synchrotron ID'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56709
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3114
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Squeeze was used owing to the inability to refine a molecule of DCM
that was badly disordered. Details are below.
It is suspected that the large thermal motion of one of the phenyl
groups is associated with this solvent disorder.
;
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0787
_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)+(0.1293P)²+8.9241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2290
_reflns_number_gt                4234
_reflns_number_total             5600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32183e.txt
_cod_data_source_block           d:\as10js1\squeze
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7021036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.5000 0.0000 0.0000 0.0426(2) Uani 1 2 d S
Cl1 Cl 0.46043(4) 0.07616(4) -0.03010(4) 0.0540(2) Uani 1 1 d .
Cl2 Cl 0.53874(4) 0.05846(4) 0.11429(4) 0.0540(2) Uani 1 1 d .
O1 O 0.41472(11) -0.05804(10) 0.04293(12) 0.0527(5) Uani 1 1 d .
N1 N 0.35195(14) -0.00330(12) 0.12342(13) 0.0467(5) Uani 1 1 d .
H1 H 0.3879(18) 0.0068(18) 0.094(2) 0.053 Uiso 1 1 d .
C1 C 0.36219(14) -0.11957(13) 0.05816(15) 0.0423(5) Uani 1 1 d .
C2 C 0.31013(13) -0.12504(13) 0.10428(14) 0.0404(5) Uani 1 1 d .
C3 C 0.25558(16) -0.19016(15) 0.12282(18) 0.0523(7) Uani 1 1 d .
H3 H 0.2208 -0.1939 0.1553 0.063 Uiso 1 1 calc R
C4 C 0.25195(16) -0.24852(15) 0.0945(2) 0.0565(7) Uani 1 1 d .
H4 H 0.2149 -0.2925 0.1072 0.068 Uiso 1 1 calc R
C5 C 0.30283(18) -0.24259(15) 0.0472(2) 0.0590(8) Uani 1 1 d .
H5 H 0.2997 -0.2829 0.0265 0.071 Uiso 1 1 calc R
C6 C 0.35805(17) -0.17942(15) 0.02952(19) 0.0546(7) Uani 1 1 d .
H6 H 0.3932 -0.1764 -0.0020 0.065 Uiso 1 1 calc R
C7 C 0.30907(15) -0.06632(15) 0.13438(15) 0.0461(6) Uani 1 1 d .
H7 H 0.2718 -0.0759 0.1663 0.055 Uiso 1 1 calc R
C8 C 0.34612(18) 0.05675(16) 0.15211(17) 0.0532(7) Uani 1 1 d .
C9 C 0.3136(3) 0.0408(2) 0.2284(2) 0.0822(13) Uani 1 1 d .
H9A H 0.2665 0.0022 0.2251 0.123 Uiso 1 1 calc R
H9B H 0.3130 0.0812 0.2476 0.123 Uiso 1 1 calc R
H9C H 0.3403 0.0287 0.2615 0.123 Uiso 1 1 calc R
C10 C 0.4185(2) 0.11639(18) 0.1581(2) 0.0661(9) Uani 1 1 d .
H10A H 0.4398 0.1272 0.1092 0.099 Uiso 1 1 calc R
H10B H 0.4451 0.1042 0.1913 0.099 Uiso 1 1 calc R
H10C H 0.4174 0.1565 0.1776 0.099 Uiso 1 1 calc R
C11 C 0.30417(18) 0.06998(15) 0.09335(19) 0.0561(7) Uani 1 1 d .
C12 C 0.2352(3) 0.0327(3) 0.0904(5) 0.130(3) Uani 1 1 d .
H12 H 0.2115 -0.0025 0.1258 0.156 Uiso 1 1 calc R
C13 C 0.1974(3) 0.0441(3) 0.0372(5) 0.145(3) Uani 1 1 d .
H13 H 0.1486 0.0198 0.0390 0.174 Uiso 1 1 calc R
C14 C 0.2310(3) 0.0904(3) -0.0175(3) 0.0943(15) Uani 1 1 d .
H14 H 0.2059 0.0956 -0.0566 0.113 Uiso 1 1 calc R
C15 C 0.2991(3) 0.1285(3) -0.0159(3) 0.0923(14) Uani 1 1 d .
H15 H 0.3225 0.1625 -0.0526 0.111 Uiso 1 1 calc R
C16 C 0.3356(2) 0.1187(3) 0.0386(2) 0.0772(11) Uani 1 1 d .
H16 H 0.3842 0.1463 0.0388 0.093 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'
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(2) . 10_655
O1 Ti1 Cl1 91.40(6) . 10_655
O1 Ti1 Cl1 88.60(6) 10_655 10_655
O1 Ti1 Cl1 88.60(6) . .
O1 Ti1 Cl1 91.40(6) 10_655 .
Cl1 Ti1 Cl1 180.00(3) 10_655 .
O1 Ti1 Cl2 90.75(7) . 10_655
O1 Ti1 Cl2 89.25(7) 10_655 10_655
Cl1 Ti1 Cl2 88.13(3) 10_655 10_655
Cl1 Ti1 Cl2 91.87(3) . 10_655
O1 Ti1 Cl2 89.25(7) . .
O1 Ti1 Cl2 90.75(7) 10_655 .
Cl1 Ti1 Cl2 91.87(3) 10_655 .
Cl1 Ti1 Cl2 88.13(3) . .
Cl2 Ti1 Cl2 180.00(4) 10_655 .
C1 O1 Ti1 152.35(18) . .
C7 N1 C8 125.9(3) . .
C7 N1 H1 117(2) . .
C8 N1 H1 117(2) . .
O1 C1 C2 119.3(2) . .
O1 C1 C6 121.5(2) . .
C2 C1 C6 119.2(2) . .
C1 C2 C3 119.6(2) . .
C1 C2 C7 123.0(2) . .
C3 C2 C7 117.4(2) . .
C4 C3 C2 120.8(3) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C3 C4 C5 119.3(3) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 121.3(3) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
C5 C6 C1 119.8(3) . .
C5 C6 H6 120.1 . .
C1 C6 H6 120.1 . .
N1 C7 C2 127.8(3) . .
N1 C7 H7 116.1 . .
C2 C7 H7 116.1 . .
C10 C8 N1 106.4(3) . .
C10 C8 C9 108.8(3) . .
N1 C8 C9 110.4(3) . .
C10 C8 C11 111.6(3) . .
N1 C8 C11 105.5(2) . .
C9 C8 C11 113.8(3) . .
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 . .
C12 C11 C16 116.1(4) . .
C12 C11 C8 122.1(4) . .
C16 C11 C8 121.8(3) . .
C11 C12 C13 122.2(5) . .
C11 C12 H12 118.9 . .
C13 C12 H12 118.9 . .
C14 C13 C12 119.3(6) . .
C14 C13 H13 120.4 . .
C12 C13 H13 120.4 . .
C15 C14 C13 119.9(5) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C14 C15 C16 120.0(5) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 122.4(5) . .
C15 C16 H16 118.8 . .
C11 C16 H16 118.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.868(2) .
Ti1 O1 1.868(2) 10_655
Ti1 Cl1 2.3567(7) 10_655
Ti1 Cl1 2.3567(7) .
Ti1 Cl2 2.3768(8) 10_655
Ti1 Cl2 2.3768(8) .
O1 C1 1.324(3) .
N1 C7 1.270(4) .
N1 C8 1.514(3) .
N1 H1 0.90(4) .
C1 C2 1.395(4) .
C1 C6 1.402(4) .
C2 C3 1.403(4) .
C2 C7 1.441(4) .
C3 C4 1.374(4) .
C3 H3 0.9500 .
C4 C5 1.383(5) .
C4 H4 0.9500 .
C5 C6 1.379(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C10 1.509(5) .
C8 C9 1.523(5) .
C8 C11 1.549(5) .
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 C12 1.347(6) .
C11 C16 1.383(5) .
C12 C13 1.394(8) .
C12 H12 0.9500 .
C13 C14 1.362(9) .
C13 H13 0.9500 .
C14 C15 1.330(8) .
C14 H14 0.9500 .
C15 C16 1.374(7) .
C15 H15 0.9500 .
C16 H16 0.9500 .
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
O1 Ti1 O1 C1 129(42) 10_655
Cl1 Ti1 O1 C1 -37.9(4) 10_655
Cl1 Ti1 O1 C1 142.1(4) .
Cl2 Ti1 O1 C1 50.3(4) 10_655
Cl2 Ti1 O1 C1 -129.7(4) .
Ti1 O1 C1 C2 175.1(3) .
Ti1 O1 C1 C6 -4.3(6) .
O1 C1 C2 C3 -177.7(3) .
C6 C1 C2 C3 1.7(4) .
O1 C1 C2 C7 2.5(4) .
C6 C1 C2 C7 -178.1(3) .
C1 C2 C3 C4 -1.7(5) .
C7 C2 C3 C4 178.0(3) .
C2 C3 C4 C5 0.0(5) .
C3 C4 C5 C6 1.8(6) .
C4 C5 C6 C1 -1.8(6) .
O1 C1 C6 C5 179.4(3) .
C2 C1 C6 C5 0.0(5) .
C8 N1 C7 C2 175.5(3) .
C1 C2 C7 N1 1.6(5) .
C3 C2 C7 N1 -178.1(3) .
C7 N1 C8 C10 153.5(3) .
C7 N1 C8 C9 35.6(4) .
C7 N1 C8 C11 -87.8(3) .
C10 C8 C11 C12 -163.6(5) .
N1 C8 C11 C12 81.2(5) .
C9 C8 C11 C12 -40.0(6) .
C10 C8 C11 C16 19.5(4) .
N1 C8 C11 C16 -95.6(4) .
C9 C8 C11 C16 143.1(4) .
C16 C11 C12 C13 -2.3(10) .
C8 C11 C12 C13 -179.4(7) .
C11 C12 C13 C14 5.5(13) .
C12 C13 C14 C15 -5.9(12) .
C13 C14 C15 C16 3.2(9) .
C14 C15 C16 C11 -0.1(8) .
C12 C11 C16 C15 -0.4(7) .
C8 C11 C16 C15 176.7(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 407 35 ' '
2 0.667 0.333 0.333 405 35 ' '
3 0.333 0.667 0.167 23 2 ' '
4 0.333 0.667 0.667 405 35 ' '
5 0.000 0.000 0.500 23 2 ' '
6 0.667 0.333 0.833 23 2 ' '
