#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:53:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178981 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/04/4120411.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_4120411
loop_
_publ_author_name
'Dana Shoken'
'Manab Sharma'
'Mark Botoshansky'
'Matthias Tamm'
'Moris S. Eisen'
_publ_section_title
;
 Mono(imidazolin-2-iminato) Titanium Complexes for Ethylene Polymerization
 at Low Amounts of Methylaluminoxane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12592
_journal_page_last               12595
_journal_paper_doi               10.1021/ja406925z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H40 Cl3 N3 Ti'
_chemical_formula_weight         596.90
_chemical_name_common            'Moris-212 (Manab)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.50(2)
_cell_angle_beta                 95.35(3)
_cell_angle_gamma                112.65(3)
_cell_formula_units_Z            2
_cell_length_a                   9.441(2)
_cell_length_b                   9.489(2)
_cell_length_c                   19.860(4)
_cell_measurement_reflns_used    20370
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.07
_cell_volume                     1628.7(7)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20365
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0950P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                3550
_reflns_number_total             5754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406925z_si_004.cif
_cod_data_source_block           Moris-212
_cod_original_cell_volume        1628.7(6)
_cod_database_code               4120411
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ti1 Ti 0.49962(7) -0.06901(7) 0.26071(3) 0.0403(2) Uani 1 1 d .
Cl1 Cl 0.69641(12) -0.06975(14) 0.33291(6) 0.0734(4) Uani 1 1 d .
Cl2 Cl 0.28199(12) -0.25705(11) 0.28328(6) 0.0683(3) Uani 1 1 d .
Cl3 Cl 0.53869(13) -0.10942(13) 0.15400(6) 0.0749(4) Uani 1 1 d .
N1 N 0.4801(3) 0.1042(3) 0.27200(14) 0.0366(6) Uani 1 1 d .
N2 N 0.4931(3) 0.3340(3) 0.33259(13) 0.0344(6) Uani 1 1 d .
N3 N 0.3917(3) 0.2893(3) 0.22706(13) 0.0341(6) Uani 1 1 d .
C1 C 0.4568(3) 0.2336(3) 0.27717(16) 0.0302(7) Uani 1 1 d .
C2 C 0.4481(4) 0.4530(4) 0.31666(18) 0.0412(8) Uani 1 1 d .
H2 H 0.4594 0.5376 0.3463 0.049 Uiso 1 1 calc R
C3 C 0.3861(4) 0.4262(4) 0.25224(18) 0.0417(8) Uani 1 1 d .
H3 H 0.3459 0.4882 0.2281 0.050 Uiso 1 1 calc R
C4 C 0.5623(4) 0.3152(4) 0.39766(16) 0.0384(8) Uani 1 1 d .
C5 C 0.4658(4) 0.2602(4) 0.44802(18) 0.0446(8) Uani 1 1 d .
C6 C 0.5366(5) 0.2455(5) 0.5105(2) 0.0585(10) Uani 1 1 d .
H6 H 0.4764 0.2099 0.5460 0.070 Uiso 1 1 calc R
C7 C 0.6928(5) 0.2820(5) 0.5210(2) 0.0623(11) Uani 1 1 d .
H7 H 0.7382 0.2715 0.5637 0.075 Uiso 1 1 calc R
C8 C 0.7845(4) 0.3341(5) 0.4696(2) 0.0551(10) Uani 1 1 d .
H8 H 0.8911 0.3574 0.4778 0.066 Uiso 1 1 calc R
C9 C 0.7217(4) 0.3527(4) 0.40609(18) 0.0433(8) Uani 1 1 d .
C10 C 0.2911(4) 0.2132(4) 0.4352(2) 0.0517(9) Uani 1 1 d .
H10 H 0.2697 0.2630 0.3949 0.062 Uiso 1 1 calc R
C11 C 0.2273(5) 0.2666(6) 0.4939(3) 0.0813(15) Uani 1 1 d .
H11A H 0.1166 0.2357 0.4832 0.122 Uiso 1 1 calc R
H11B H 0.2763 0.3774 0.5017 0.122 Uiso 1 1 calc R
H11C H 0.2482 0.2211 0.5344 0.122 Uiso 1 1 calc R
C12 C 0.2096(5) 0.0419(6) 0.4186(3) 0.105(2) Uani 1 1 d .
H12A H 0.0991 0.0147 0.4099 0.157 Uiso 1 1 calc R
H12B H 0.2314 -0.0104 0.4566 0.157 Uiso 1 1 calc R
H12C H 0.2462 0.0115 0.3786 0.157 Uiso 1 1 calc R
C13 C 0.8212(4) 0.4131(4) 0.35017(19) 0.0516(10) Uani 1 1 d .
H13 H 0.7578 0.3643 0.3065 0.062 Uiso 1 1 calc R
C14 C 0.8695(5) 0.5861(5) 0.3489(3) 0.0774(14) Uani 1 1 d .
H14A H 0.9325 0.6217 0.3124 0.116 Uiso 1 1 calc R
H14B H 0.9287 0.6371 0.3919 0.116 Uiso 1 1 calc R
H14C H 0.7781 0.6094 0.3416 0.116 Uiso 1 1 calc R
C15 C 0.9657(5) 0.3759(5) 0.3541(3) 0.0717(13) Uani 1 1 d .
H15A H 1.0233 0.4168 0.3165 0.108 Uiso 1 1 calc R
H15B H 0.9352 0.2656 0.3516 0.108 Uiso 1 1 calc R
H15C H 1.0300 0.4216 0.3966 0.108 Uiso 1 1 calc R
C16 C 0.3458(3) 0.2206(4) 0.15774(16) 0.0342(7) Uani 1 1 d .
C17 C 0.1995(4) 0.1050(4) 0.14220(18) 0.0396(8) Uani 1 1 d .
C18 C 0.1623(4) 0.0414(4) 0.0753(2) 0.0532(10) Uani 1 1 d .
H18 H 0.0641 -0.0362 0.0617 0.064 Uiso 1 1 calc R
C19 C 0.2658(5) 0.0892(5) 0.0284(2) 0.0613(11) Uani 1 1 d .
H19 H 0.2379 0.0431 -0.0164 0.074 Uiso 1 1 calc R
C20 C 0.4091(5) 0.2031(5) 0.0462(2) 0.0559(10) Uani 1 1 d .
H20 H 0.4784 0.2342 0.0135 0.067 Uiso 1 1 calc R
C21 C 0.4536(4) 0.2733(4) 0.11200(18) 0.0424(8) Uani 1 1 d .
C22 C 0.0857(4) 0.0556(4) 0.1938(2) 0.0531(10) Uani 1 1 d .
H22 H 0.1455 0.0789 0.2394 0.064 Uiso 1 1 calc R
C23 C -0.0154(5) 0.1473(5) 0.1908(3) 0.0843(16) Uani 1 1 d .
H23A H -0.0869 0.1158 0.2245 0.126 Uiso 1 1 calc R
H23B H -0.0729 0.1292 0.1460 0.126 Uiso 1 1 calc R
H23C H 0.0492 0.2556 0.2000 0.126 Uiso 1 1 calc R
C24 C -0.0162(5) -0.1159(5) 0.1854(3) 0.0859(16) Uani 1 1 d .
H24A H -0.0850 -0.1404 0.2203 0.129 Uiso 1 1 calc R
H24B H 0.0486 -0.1741 0.1894 0.129 Uiso 1 1 calc R
H24C H -0.0767 -0.1417 0.1410 0.129 Uiso 1 1 calc R
C25 C 0.6111(4) 0.4004(5) 0.1318(2) 0.0626(11) Uani 1 1 d .
H25 H 0.6124 0.4406 0.1788 0.075 Uiso 1 1 calc R
C26 C 0.6398(6) 0.5322(5) 0.0881(3) 0.0937(17) Uani 1 1 d .
H26A H 0.5569 0.5684 0.0893 0.141 Uiso 1 1 calc R
H26B H 0.6434 0.4983 0.0418 0.141 Uiso 1 1 calc R
H26C H 0.7375 0.6147 0.1052 0.141 Uiso 1 1 calc R
C27 C 0.7376(5) 0.3398(7) 0.1331(4) 0.114(2) Uani 1 1 d .
H27A H 0.8371 0.4235 0.1460 0.171 Uiso 1 1 calc R
H27B H 0.7360 0.2934 0.0884 0.171 Uiso 1 1 calc R
H27C H 0.7210 0.2635 0.1657 0.171 Uiso 1 1 calc R
C28 C 0.1854(8) 0.5212(12) 0.0836(4) 0.053(3) Uani 0.50 1 d P
C29 C 0.1430(12) 0.6536(16) 0.0578(5) 0.108(3) Uani 0.50 1 d PD
C30 C 0.0238(6) 0.6331(5) 0.0087(3) 0.0826(15) Uani 1 1 d D
C31 C -0.1021(12) 0.5912(17) -0.0428(5) 0.108(3) Uani 0.50 1 d PD
C32 C 0.0823(18) 0.5033(11) 0.0404(8) 0.122(7) Uani 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ti Ti 0.2776 0.4457 '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'
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'
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
N1 Ti1 Cl3 110.08(10) . .
N1 Ti1 Cl1 110.00(10) . .
Cl3 Ti1 Cl1 110.34(6) . .
N1 Ti1 Cl2 108.70(9) . .
Cl3 Ti1 Cl2 109.34(6) . .
Cl1 Ti1 Cl2 108.36(6) . .
C1 N1 Ti1 175.9(2) . .
C1 N2 C2 108.7(3) . .
C1 N2 C4 124.7(3) . .
C2 N2 C4 126.6(3) . .
C1 N3 C3 108.8(3) . .
C1 N3 C16 124.5(3) . .
C3 N3 C16 126.6(3) . .
N1 C1 N2 127.1(3) . .
N1 C1 N3 125.9(3) . .
N2 C1 N3 107.1(3) . .
C3 C2 N2 108.0(3) . .
C3 C2 H2 126.0 . .
N2 C2 H2 126.0 . .
C2 C3 N3 107.4(3) . .
C2 C3 H3 126.3 . .
N3 C3 H3 126.3 . .
C9 C4 C5 124.2(3) . .
C9 C4 N2 117.8(3) . .
C5 C4 N2 118.0(3) . .
C6 C5 C4 116.5(3) . .
C6 C5 C10 121.3(3) . .
C4 C5 C10 122.2(3) . .
C7 C6 C5 121.1(4) . .
C7 C6 H6 119.4 . .
C5 C6 H6 119.4 . .
C6 C7 C8 120.8(4) . .
C6 C7 H7 119.6 . .
C8 C7 H7 119.6 . .
C7 C8 C9 121.2(4) . .
C7 C8 H8 119.4 . .
C9 C8 H8 119.4 . .
C8 C9 C4 116.2(3) . .
C8 C9 C13 121.6(3) . .
C4 C9 C13 122.2(3) . .
C12 C10 C11 110.9(4) . .
C12 C10 C5 110.8(3) . .
C11 C10 C5 112.4(3) . .
C12 C10 H10 107.5 . .
C11 C10 H10 107.5 . .
C5 C10 H10 107.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C9 C13 C14 111.2(3) . .
C9 C13 C15 113.8(3) . .
C14 C13 C15 109.1(3) . .
C9 C13 H13 107.5 . .
C14 C13 H13 107.5 . .
C15 C13 H13 107.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C21 C16 C17 124.8(3) . .
C21 C16 N3 117.2(3) . .
C17 C16 N3 118.0(3) . .
C18 C17 C16 115.6(3) . .
C18 C17 C22 122.0(3) . .
C16 C17 C22 122.3(3) . .
C19 C18 C17 121.6(3) . .
C19 C18 H18 119.2 . .
C17 C18 H18 119.2 . .
C20 C19 C18 120.7(4) . .
C20 C19 H19 119.6 . .
C18 C19 H19 119.6 . .
C19 C20 C21 120.9(3) . .
C19 C20 H20 119.6 . .
C21 C20 H20 119.6 . .
C16 C21 C20 116.4(3) . .
C16 C21 C25 122.4(3) . .
C20 C21 C25 121.2(3) . .
C17 C22 C23 110.2(3) . .
C17 C22 C24 113.5(3) . .
C23 C22 C24 109.7(3) . .
C17 C22 H22 107.8 . .
C23 C22 H22 107.8 . .
C24 C22 H22 107.8 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 C27 112.2(4) . .
C26 C25 C21 112.2(4) . .
C27 C25 C21 111.2(4) . .
C26 C25 H25 106.9 . .
C27 C25 H25 106.9 . .
C21 C25 H25 106.9 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C31 C28 C29 103.1(10) 2_565 .
C30 C29 C28 123.8(11) . .
C31 C30 C29 172.4(10) . .
C29 C30 C32 133.5(9) . 2_565
C31 C30 C32 121.2(9) . .
C30 C31 C28 139.8(13) . 2_565
C31 C32 C29 144(2) 2_565 .
C28 C32 C30 133.6(10) . 2_565
C29 C32 C30 149.6(13) . 2_565
C31 C32 C30 159.6(18) 2_565 .
C28 C32 C30 128.8(12) . .
C31 C32 C32 114.8(17) 2_565 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.731(3) .
Ti1 Cl3 2.2266(13) .
Ti1 Cl1 2.2411(15) .
Ti1 Cl2 2.2415(14) .
N1 C1 1.329(4) .
N2 C1 1.350(4) .
N2 C2 1.390(4) .
N2 C4 1.442(4) .
N3 C1 1.353(4) .
N3 C3 1.393(4) .
N3 C16 1.449(4) .
C2 C3 1.327(5) .
C2 H2 0.9400 .
C3 H3 0.9400 .
C4 C9 1.398(5) .
C4 C5 1.397(5) .
C5 C6 1.392(5) .
C5 C10 1.526(5) .
C6 C7 1.372(5) .
C6 H6 0.9400 .
C7 C8 1.383(5) .
C7 H7 0.9400 .
C8 C9 1.391(5) .
C8 H8 0.9400 .
C9 C13 1.510(5) .
C10 C12 1.512(6) .
C10 C11 1.515(5) .
C10 H10 0.9900 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 H11C 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 H12C 0.9700 .
C13 C14 1.527(6) .
C13 C15 1.531(5) .
C13 H13 0.9900 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C14 H14C 0.9700 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 H15C 0.9700 .
C16 C21 1.389(4) .
C16 C17 1.390(4) .
C17 C18 1.391(5) .
C17 C22 1.511(5) .
C18 C19 1.376(5) .
C18 H18 0.9400 .
C19 C20 1.369(5) .
C19 H19 0.9400 .
C20 C21 1.391(5) .
C20 H20 0.9400 .
C21 C25 1.513(5) .
C22 C23 1.518(6) .
C22 C24 1.530(5) .
C22 H22 0.9900 .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C23 H23C 0.9700 .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C24 H24C 0.9700 .
C25 C26 1.506(6) .
C25 C27 1.511(6) .
C25 H25 0.9900 .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C26 H26C 0.9700 .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C27 H27C 0.9700 .
C28 C32 1.191(18) .
C28 C31 1.254(16) 2_565
C28 C29 1.552(15) .
C29 C30 1.365(8) .
C29 C32 1.331(17) .
C30 C31 1.412(9) .
C30 C32 1.529(16) 2_565
C30 C32 1.656(12) .
C31 C28 1.254(16) 2_565
C32 C30 1.529(16) 2_565
C32 C32 2.11(4) 2_565
