#------------------------------------------------------------------------------
#$Date: 2016-10-01 08:32:39 +0300 (Sat, 01 Oct 2016) $
#$Revision: 186873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/57/7055793.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_7055793
loop_
_publ_author_name
'Mandal, Mrinmay'
'Monkowius, Uwe'
'Chakraborty, Debashis'
_publ_section_title
;
 Synthesis and structural characterization of titanium and zirconium
 complexes containing half-salen ligands as catalysts for polymerization
 reactions
;
_journal_name_full               'New J. Chem.'
_journal_paper_doi               10.1039/C6NJ02148D
_journal_year                    2016
_chemical_formula_moiety         'C36 H50 N2 O4 Ti'
_chemical_formula_sum            'C36 H50 N2 O4 Ti'
_chemical_formula_weight         622.68
_chemical_name_systematic        Ti1
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.1-2'
_audit_update_record
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.720(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4864(9)
_cell_length_b                   17.4311(13)
_cell_length_c                   16.5711(16)
_cell_measurement_reflns_used    7841
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.34
_cell_volume                     4047.1(6)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19126
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0451
_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)+(0.0754P)²+0.6354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3664
_reflns_number_total             5037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02148d2.cif
_cod_data_source_block           Ti1
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7055793
_publcif_datablock.id            {1ca9f957-dee2-423c-8aa0-77e1010ccb34}
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.2500 0.01259(2) 0.0000 0.04692(15) Uani 1 2 d S
O2 O 0.30253(10) -0.05784(8) 0.08246(9) 0.0777(4) Uani 1 1 d .
C13 C 0.30626(18) -0.13523(13) 0.20492(15) 0.0848(7) Uani 1 1 d .
H13A H 0.3754 -0.1379 0.2204 0.102 Uiso 1 1 calc R
H13B H 0.2821 -0.1794 0.1704 0.102 Uiso 1 1 calc R
C4 C 0.00507(12) 0.25282(11) -0.07150(11) 0.0598(4) Uani 1 1 d .
H4 H -0.0117 0.2973 -0.1028 0.072 Uiso 1 1 calc R
C10 C 0.11072(18) 0.16044(17) -0.22328(14) 0.0921(7) Uani 1 1 d .
H10A H 0.0440 0.1524 -0.2483 0.138 Uiso 1 1 calc R
H10B H 0.1380 0.1144 -0.1953 0.138 Uiso 1 1 calc R
H10C H 0.1424 0.1732 -0.2658 0.138 Uiso 1 1 calc R
C16 C 0.12930(16) -0.05388(13) 0.21063(12) 0.0752(6) Uani 1 1 d .
H16A H 0.0601 -0.0523 0.1944 0.090 Uiso 1 1 calc R
H16B H 0.1521 -0.0083 0.2432 0.090 Uiso 1 1 calc R
C15 C 0.16300(19) -0.12550(15) 0.26282(14) 0.0903(7) Uani 1 1 d .
H15A H 0.1437 -0.1219 0.3146 0.108 Uiso 1 1 calc R
H15B H 0.1319 -0.1701 0.2328 0.108 Uiso 1 1 calc R
C14 C 0.26961(18) -0.13659(15) 0.28262(14) 0.0885(7) Uani 1 1 d .
H14A H 0.2860 -0.1853 0.3109 0.106 Uiso 1 1 calc R
H14B H 0.3007 -0.0963 0.3202 0.106 Uiso 1 1 calc R
C1 C 0.05324(9) 0.12204(9) 0.02208(9) 0.0435(3) Uani 1 1 d .
C7 C -0.11360(17) 0.29275(16) 0.00952(15) 0.0920(8) Uani 1 1 d .
H7A H -0.1762 0.2775 -0.0216 0.138 Uiso 1 1 calc R
H7B H -0.1005 0.3436 -0.0067 0.138 Uiso 1 1 calc R
H7C H -0.1106 0.2921 0.0681 0.138 Uiso 1 1 calc R
C8 C 0.12305(13) 0.22670(12) -0.15976(11) 0.0639(5) Uani 1 1 d .
C9 C 0.22843(15) 0.23949(16) -0.12136(15) 0.0928(8) Uani 1 1 d .
H9A H 0.2596 0.2511 -0.1645 0.139 Uiso 1 1 calc R
H9B H 0.2558 0.1939 -0.0924 0.139 Uiso 1 1 calc R
H9C H 0.2366 0.2816 -0.0828 0.139 Uiso 1 1 calc R
C12 C 0.27445(13) -0.06279(11) 0.15660(12) 0.0616(5) Uani 1 1 d .
H12 H 0.3017 -0.0190 0.1918 0.074 Uiso 1 1 calc R
C2 C 0.09912(9) 0.13884(9) -0.04178(9) 0.0452(4) Uani 1 1 d .
C3 C 0.07342(10) 0.20579(10) -0.09055(10) 0.0516(4) Uani 1 1 d .
C5 C -0.04043(12) 0.23771(11) -0.00812(10) 0.0578(4) Uani 1 1 d .
C6 C -0.01665(10) 0.17204(10) 0.03677(9) 0.0502(4) Uani 1 1 d .
H6 H -0.0474 0.1600 0.0781 0.060 Uiso 1 1 calc R
C11 C 0.08082(19) 0.29811(16) -0.20791(16) 0.1030(9) Uani 1 1 d .
H11A H 0.0142 0.2899 -0.2332 0.154 Uiso 1 1 calc R
H11B H 0.1133 0.3085 -0.2505 0.154 Uiso 1 1 calc R
H11C H 0.0883 0.3410 -0.1704 0.154 Uiso 1 1 calc R
C17 C 0.07815(10) 0.05599(10) 0.07491(9) 0.0470(4) Uani 1 1 d .
H17 H 0.0408 0.0458 0.1118 0.056 Uiso 1 1 calc R
C18 C 0.16707(11) -0.05559(10) 0.13440(10) 0.0509(4) Uani 1 1 d .
H18 H 0.1410 -0.1016 0.1027 0.061 Uiso 1 1 calc R
N1 N 0.14724(9) 0.00981(7) 0.07582(8) 0.0438(3) Uani 1 1 d .
O1 O 0.16482(8) 0.09134(7) -0.05460(7) 0.0580(3) 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'
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'
H H 0.0000 0.0000 '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
O2 Ti1 O2 96.89(10) 2 .
O2 Ti1 O1 156.95(5) 2 2
O2 Ti1 O1 91.83(7) . 2
O2 Ti1 O1 91.83(7) 2 .
O2 Ti1 O1 156.95(5) . .
O1 Ti1 O1 88.27(8) 2 .
O2 Ti1 N1 76.85(5) 2 2
O2 Ti1 N1 101.42(5) . 2
O1 Ti1 N1 80.53(4) 2 2
O1 Ti1 N1 101.33(4) . 2
O2 Ti1 N1 101.42(5) 2 .
O2 Ti1 N1 76.85(5) . .
O1 Ti1 N1 101.33(4) 2 .
O1 Ti1 N1 80.53(4) . .
N1 Ti1 N1 177.45(7) 2 .
C12 O2 Ti1 122.38(11) . .
C12 C13 C14 109.89(19) . .
C12 C13 H13A 109.7 . .
C14 C13 H13A 109.7 . .
C12 C13 H13B 109.7 . .
C14 C13 H13B 109.7 . .
H13A C13 H13B 108.2 . .
C3 C4 C5 124.13(16) . .
C3 C4 H4 117.9 . .
C5 C4 H4 117.9 . .
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 . .
C18 C16 C15 109.18(18) . .
C18 C16 H16A 109.8 . .
C15 C16 H16A 109.8 . .
C18 C16 H16B 109.8 . .
C15 C16 H16B 109.8 . .
H16A C16 H16B 108.3 . .
C14 C15 C16 112.99(19) . .
C14 C15 H15A 109.0 . .
C16 C15 H15A 109.0 . .
C14 C15 H15B 109.0 . .
C16 C15 H15B 109.0 . .
H15A C15 H15B 107.8 . .
C15 C14 C13 111.99(18) . .
C15 C14 H14A 109.2 . .
C13 C14 H14A 109.2 . .
C15 C14 H14B 109.2 . .
C13 C14 H14B 109.2 . .
H14A C14 H14B 107.9 . .
C6 C1 C2 119.84(14) . .
C6 C1 C17 118.22(13) . .
C2 C1 C17 121.91(13) . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 C11 109.16(19) . .
C9 C8 C10 109.07(18) . .
C11 C8 C10 107.06(18) . .
C9 C8 C3 109.43(15) . .
C11 C8 C3 112.45(15) . .
C10 C8 C3 109.59(16) . .
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 . .
O2 C12 C13 113.81(17) . .
O2 C12 C18 107.10(14) . .
C13 C12 C18 110.91(16) . .
O2 C12 H12 108.3 . .
C13 C12 H12 108.3 . .
C18 C12 H12 108.3 . .
O1 C2 C3 121.46(12) . .
O1 C2 C1 119.05(14) . .
C3 C2 C1 119.49(13) . .
C4 C3 C2 117.30(14) . .
C4 C3 C8 121.69(15) . .
C2 C3 C8 120.96(14) . .
C6 C5 C4 117.80(15) . .
C6 C5 C7 121.36(16) . .
C4 C5 C7 120.84(17) . .
C5 C6 C1 121.41(14) . .
C5 C6 H6 119.3 . .
C1 C6 H6 119.3 . .
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 . .
N1 C17 C1 125.83(12) . .
N1 C17 H17 117.1 . .
C1 C17 H17 117.1 . .
N1 C18 C16 119.12(15) . .
N1 C18 C12 103.92(12) . .
C16 C18 C12 111.74(15) . .
N1 C18 H18 107.1 . .
C16 C18 H18 107.1 . .
C12 C18 H18 107.1 . .
C17 N1 C18 120.89(12) . .
C17 N1 Ti1 128.69(10) . .
C18 N1 Ti1 110.41(9) . .
C2 O1 Ti1 141.23(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O2 1.8506(13) 2
Ti1 O2 1.8507(13) .
Ti1 O1 1.9126(11) 2
Ti1 O1 1.9127(11) .
Ti1 N1 2.1789(12) 2
Ti1 N1 2.1789(12) .
O2 C12 1.391(2) .
C13 C12 1.503(3) .
C13 C14 1.512(3) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C4 C3 1.382(2) .
C4 C5 1.399(2) .
C4 H4 0.9300 .
C10 C8 1.542(3) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C16 C18 1.499(2) .
C16 C15 1.526(3) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C15 C14 1.508(3) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C1 C6 1.403(2) .
C1 C2 1.4159(18) .
C1 C17 1.436(2) .
C7 C5 1.512(2) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.514(3) .
C8 C11 1.521(3) .
C8 C3 1.544(2) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C12 C18 1.510(2) .
C12 H12 0.9800 .
C2 O1 1.3188(18) .
C2 C3 1.414(2) .
C5 C6 1.361(2) .
C6 H6 0.9300 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C17 N1 1.282(2) .
C17 H17 0.9300 .
C18 N1 1.477(2) .
C18 H18 0.9800 .
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
O2 Ti1 O2 C12 -117.64(17) 2
O1 Ti1 O2 C12 83.74(15) 2
O1 Ti1 O2 C12 -6.2(3) .
N1 Ti1 O2 C12 164.45(15) 2
N1 Ti1 O2 C12 -17.47(14) .
C18 C16 C15 C14 53.2(3) .
C16 C15 C14 C13 -53.3(3) .
C12 C13 C14 C15 54.2(3) .
Ti1 O2 C12 C13 165.22(15) .
Ti1 O2 C12 C18 42.3(2) .
C14 C13 C12 O2 -178.06(18) .
C14 C13 C12 C18 -57.2(2) .
C6 C1 C2 O1 179.82(13) .
C17 C1 C2 O1 1.9(2) .
C6 C1 C2 C3 -0.4(2) .
C17 C1 C2 C3 -178.36(14) .
C5 C4 C3 C2 -0.8(3) .
C5 C4 C3 C8 -178.33(17) .
O1 C2 C3 C4 -178.85(15) .
C1 C2 C3 C4 1.4(2) .
O1 C2 C3 C8 -1.3(2) .
C1 C2 C3 C8 178.98(15) .
C9 C8 C3 C4 115.6(2) .
C11 C8 C3 C4 -5.9(3) .
C10 C8 C3 C4 -124.88(19) .
C9 C8 C3 C2 -61.9(2) .
C11 C8 C3 C2 176.59(19) .
C10 C8 C3 C2 57.6(2) .
C3 C4 C5 C6 -0.9(3) .
C3 C4 C5 C7 179.16(19) .
C4 C5 C6 C1 1.9(2) .
C7 C5 C6 C1 -178.12(18) .
C2 C1 C6 C5 -1.3(2) .
C17 C1 C6 C5 176.70(15) .
C6 C1 C17 N1 -171.78(15) .
C2 C1 C17 N1 6.2(2) .
C15 C16 C18 N1 -177.36(16) .
C15 C16 C18 C12 -56.1(2) .
O2 C12 C18 N1 -45.78(18) .
C13 C12 C18 N1 -170.50(16) .
O2 C12 C18 C16 -175.47(15) .
C13 C12 C18 C16 59.8(2) .
C1 C17 N1 C18 178.78(14) .
C1 C17 N1 Ti1 -0.4(2) .
C16 C18 N1 C17 -20.2(2) .
C12 C18 N1 C17 -145.29(15) .
C16 C18 N1 Ti1 159.10(14) .
C12 C18 N1 Ti1 34.01(15) .
O2 Ti1 N1 C17 -98.33(14) 2
O2 Ti1 N1 C17 167.17(15) .
O1 Ti1 N1 C17 77.93(14) 2
O1 Ti1 N1 C17 -8.36(13) .
N1 Ti1 N1 C17 -145.38(13) 2
O2 Ti1 N1 C18 82.44(11) 2
O2 Ti1 N1 C18 -12.06(10) .
O1 Ti1 N1 C18 -101.30(10) 2
O1 Ti1 N1 C18 172.40(11) .
N1 Ti1 N1 C18 35.39(9) 2
C3 C2 O1 Ti1 159.40(13) .
C1 C2 O1 Ti1 -20.8(3) .
O2 Ti1 O1 C2 122.07(17) 2
O2 Ti1 O1 C2 9.6(3) .
O1 Ti1 O1 C2 -80.99(17) 2
N1 Ti1 O1 C2 -160.98(16) 2
N1 Ti1 O1 C2 20.79(17) .
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 -0.015 0.500 0.000 471 102 ' '
2 0.049 0.000 0.500 471 102 ' '
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
