#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340234.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_4340234
loop_
_publ_author_name
'Davidson, Matthew G.'
'Jones, Matthew D.'
'Lunn, Matthew D.'
'Mahon, Mary F.'
_publ_section_title
;
 Synthesis and X-ray structures of new titanium(IV) aryloxides and their
 exploitation for the ring opening polymerization of epsilon-caprolactone.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2282
_journal_page_last               2287
_journal_paper_doi               10.1021/ic051708n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C32 H56 O12 Ti2, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H60 Cl4 O12 Ti2'
_chemical_formula_weight         898.42
_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                111.2650(10)
_cell_angle_beta                 93.1220(10)
_cell_angle_gamma                102.4000(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8280(2)
_cell_length_b                   10.5980(2)
_cell_length_c                   13.2650(3)
_cell_measurement_reflns_used    16705
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      5.04
_cell_volume                     1117.58(4)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'nonius kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16606
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         5.04
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.9380
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0313
_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)+(0.0359P)²+0.4433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                4389
_reflns_number_total             5021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051708nsi20051004_093209.cif
_cod_data_source_block           5a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340234
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 0.05933(3) 0.61965(2) 0.12443(2) 0.01672(8) Uani 1 1 d .
Cl1 Cl 0.05208(6) 0.16922(6) 0.42466(4) 0.05113(14) Uani 1 1 d .
Cl2 Cl 0.35950(6) 0.28524(6) 0.55836(5) 0.05518(15) Uani 1 1 d .
O3 O -0.08041(12) 0.71751(10) 0.10304(9) 0.0237(2) Uani 1 1 d .
O4 O 0.10098(11) 0.57042(10) -0.03049(8) 0.0183(2) Uani 1 1 d .
O5 O 0.02444(11) 0.43569(10) -0.23645(8) 0.0212(2) Uani 1 1 d .
O2 O 0.21599(11) 0.75987(11) 0.20885(8) 0.0224(2) Uani 1 1 d .
O1 O 0.20477(13) 0.47214(13) 0.10975(10) 0.0280(2) Uani 1 1 d .
O6 O 0.14369(13) 0.53663(12) -0.38566(9) 0.0293(2) Uani 1 1 d .
C10 C 0.16797(15) 0.64012(15) -0.09193(12) 0.0187(3) Uani 1 1 d .
C12 C 0.18993(17) 0.61980(16) -0.27717(12) 0.0228(3) Uani 1 1 d .
C11 C 0.12555(15) 0.56330(15) -0.20402(12) 0.0191(3) Uani 1 1 d .
C4 C 0.33668(16) 0.84803(16) 0.29670(12) 0.0242(3) Uani 1 1 d .
H4 H 0.4272 0.8044 0.2916 0.029 Uiso 1 1 calc R
C15 C 0.27078(17) 0.77176(15) -0.05008(13) 0.0242(3) Uani 1 1 d .
H15 H 0.2979 0.8230 0.0265 0.029 Uiso 1 1 calc R
C14 C 0.33312(19) 0.82654(17) -0.12423(14) 0.0304(3) Uani 1 1 d .
H14 H 0.4037 0.9168 -0.0976 0.036 Uiso 1 1 calc R
C13 C 0.29402(18) 0.75181(17) -0.23613(14) 0.0284(3) Uani 1 1 d .
H13 H 0.3386 0.7910 -0.2851 0.034 Uiso 1 1 calc R
C1 C 0.31852(18) 0.46253(17) 0.18669(13) 0.0279(3) Uani 1 1 d .
H1A H 0.3346 0.5470 0.2559 0.033 Uiso 1 1 calc R
C7 C -0.09285(18) 0.85418(15) 0.16965(13) 0.0242(3) Uani 1 1 d .
H7 H -0.0242 0.8864 0.2413 0.029 Uiso 1 1 calc R
C17 C 0.1572(2) 0.2214(2) 0.55575(15) 0.0407(4) Uani 1 1 d .
H17B H 0.1403 0.1406 0.5783 0.049 Uiso 1 1 calc R
H17A H 0.1171 0.2953 0.6088 0.049 Uiso 1 1 calc R
C5 C 0.3903(2) 0.98862(17) 0.28800(14) 0.0340(4) Uani 1 1 d .
H5B H 0.4291 0.9758 0.2180 0.051 Uiso 1 1 calc R
H5A H 0.4746 1.0492 0.3481 0.051 Uiso 1 1 calc R
H5C H 0.3021 1.0320 0.2922 0.051 Uiso 1 1 calc R
C9 C -0.2606(2) 0.8470(2) 0.19058(17) 0.0405(4) Uani 1 1 d .
H9C H -0.3284 0.8214 0.1216 0.061 Uiso 1 1 calc R
H9A H -0.2678 0.9385 0.2420 0.061 Uiso 1 1 calc R
H9B H -0.2943 0.7765 0.2218 0.061 Uiso 1 1 calc R
C16 C 0.2185(2) 0.5843(2) -0.46243(15) 0.0386(4) Uani 1 1 d .
H16A H 0.1969 0.6737 -0.4555 0.058 Uiso 1 1 calc R
H16B H 0.1781 0.5151 -0.5367 0.058 Uiso 1 1 calc R
H16C H 0.3319 0.5967 -0.4479 0.058 Uiso 1 1 calc R
C6 C 0.2746(2) 0.8596(2) 0.40328(14) 0.0390(4) Uani 1 1 d .
H6B H 0.1917 0.9096 0.4120 0.059 Uiso 1 1 calc R
H6C H 0.3600 0.9111 0.4645 0.059 Uiso 1 1 calc R
H6A H 0.2319 0.7657 0.4022 0.059 Uiso 1 1 calc R
C2 C 0.4722(2) 0.4645(3) 0.1431(2) 0.0528(5) Uani 1 1 d .
H2A H 0.4603 0.3807 0.0766 0.079 Uiso 1 1 calc R
H2B H 0.5519 0.4661 0.1983 0.079 Uiso 1 1 calc R
H2C H 0.5046 0.5481 0.1261 0.079 Uiso 1 1 calc R
C8 C -0.0371(2) 0.9541(2) 0.11516(18) 0.0429(4) Uani 1 1 d .
H8A H 0.0727 0.9575 0.1051 0.064 Uiso 1 1 calc R
H8B H -0.0461 1.0476 0.1610 0.064 Uiso 1 1 calc R
H8C H -0.1015 0.9223 0.0438 0.064 Uiso 1 1 calc R
C3 C 0.2572(3) 0.3350(3) 0.2124(2) 0.0577(6) Uani 1 1 d .
H3C H 0.1563 0.3386 0.2391 0.087 Uiso 1 1 calc R
H26B H 0.3322 0.3331 0.2688 0.087 Uiso 1 1 calc R
H3A H 0.2434 0.2505 0.1462 0.087 Uiso 1 1 calc R
H1 H 0.188(3) 0.413(2) 0.0570(19) 0.039(6) Uiso 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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 O3 100.06(5) . .
O2 Ti1 O5 97.65(4) . 2_565
O3 Ti1 O5 100.43(5) . 2_565
O2 Ti1 O4 107.75(4) . .
O3 Ti1 O4 90.69(4) . .
O5 Ti1 O4 150.05(4) 2_565 .
O2 Ti1 O4 169.10(4) . 2_565
O3 Ti1 O4 90.78(4) . 2_565
O5 Ti1 O4 79.01(4) 2_565 2_565
O4 Ti1 O4 73.07(4) . 2_565
O2 Ti1 O1 90.52(5) . .
O3 Ti1 O1 166.60(5) . .
O5 Ti1 O1 86.16(5) 2_565 .
O4 Ti1 O1 78.16(4) . .
O4 Ti1 O1 78.95(4) 2_565 .
O2 Ti1 Ti1 144.06(4) . 2_565
O3 Ti1 Ti1 90.91(3) . 2_565
O5 Ti1 Ti1 113.98(3) 2_565 2_565
O4 Ti1 Ti1 37.44(3) . 2_565
O4 Ti1 Ti1 35.62(3) 2_565 2_565
O1 Ti1 Ti1 75.72(3) . 2_565
C7 O3 Ti1 129.30(9) . .
C10 O4 Ti1 136.81(9) . .
C10 O4 Ti1 112.96(8) . 2_565
Ti1 O4 Ti1 106.93(4) . 2_565
C11 O5 Ti1 117.10(9) . 2_565
C4 O2 Ti1 162.50(10) . .
C1 O1 Ti1 132.43(10) . .
C1 O1 H1 112.9(18) . .
Ti1 O1 H1 114.4(17) . .
C12 O6 C16 117.04(13) . .
O4 C10 C15 124.85(13) . .
O4 C10 C11 112.92(12) . .
C15 C10 C11 122.21(13) . .
O6 C12 C13 125.47(13) . .
O6 C12 C11 115.40(13) . .
C13 C12 C11 119.13(14) . .
O5 C11 C10 117.58(12) . .
O5 C11 C12 123.20(13) . .
C10 C11 C12 119.22(13) . .
O2 C4 C5 109.39(12) . .
O2 C4 C6 108.46(12) . .
C5 C4 C6 112.45(14) . .
O2 C4 H4 108.8 . .
C5 C4 H4 108.8 . .
C6 C4 H4 108.8 . .
C10 C15 C14 117.72(14) . .
C10 C15 H15 121.1 . .
C14 C15 H15 121.1 . .
C13 C14 C15 121.25(14) . .
C13 C14 H14 119.4 . .
C15 C14 H14 119.4 . .
C14 C13 C12 120.46(14) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
O1 C1 C2 109.55(15) . .
O1 C1 C3 110.14(15) . .
C2 C1 C3 113.17(17) . .
O1 C1 H1A 107.9 . .
C2 C1 H1A 107.9 . .
C3 C1 H1A 107.9 . .
O3 C7 C8 109.75(13) . .
O3 C7 C9 109.13(13) . .
C8 C7 C9 112.18(14) . .
O3 C7 H7 108.6 . .
C8 C7 H7 108.6 . .
C9 C7 H7 108.6 . .
Cl1 C17 Cl2 111.56(11) . .
Cl1 C17 H17B 109.3 . .
Cl2 C17 H17B 109.3 . .
Cl1 C17 H17A 109.3 . .
Cl2 C17 H17A 109.3 . .
H17B C17 H17A 108.0 . .
C4 C5 H5B 109.5 . .
C4 C5 H5A 109.5 . .
H5B C5 H5A 109.5 . .
C4 C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
C7 C9 H9C 109.5 . .
C7 C9 H9A 109.5 . .
H9C C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9C C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O6 C16 H16A 109.5 . .
O6 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O6 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C4 C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C4 C6 H6A 109.5 . .
H6B C6 H6A 109.5 . .
H6C C6 H6A 109.5 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C1 C3 H3C 109.5 . .
C1 C3 H26B 109.5 . .
H3C C3 H26B 109.5 . .
C1 C3 H3A 109.5 . .
H3C C3 H3A 109.5 . .
H26B C3 H3A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O2 1.7654(10) .
Ti1 O3 1.8447(10) .
Ti1 O5 1.9142(10) 2_565
Ti1 O4 2.0043(10) .
Ti1 O4 2.0920(9) 2_565
Ti1 O1 2.1906(11) .
Ti1 Ti1 3.2919(5) 2_565
Cl1 C17 1.760(2) .
Cl2 C17 1.763(2) .
O3 C7 1.4287(17) .
O4 C10 1.3643(16) .
O4 Ti1 2.0920(9) 2_565
O5 C11 1.3522(17) .
O5 Ti1 1.9142(10) 2_565
O2 C4 1.4190(17) .
O1 C1 1.4380(18) .
O1 H1 0.73(2) .
O6 C12 1.3697(19) .
O6 C16 1.4249(18) .
C10 C15 1.385(2) .
C10 C11 1.394(2) .
C12 C13 1.393(2) .
C12 C11 1.3995(19) .
C4 C5 1.512(2) .
C4 C6 1.517(2) .
C4 H4 1.0000 .
C15 C14 1.394(2) .
C15 H15 0.9500 .
C14 C13 1.387(2) .
C14 H14 0.9500 .
C13 H13 0.9500 .
C1 C2 1.502(3) .
C1 C3 1.509(3) .
C1 H1A 1.0000 .
C7 C8 1.502(2) .
C7 C9 1.512(2) .
C7 H7 1.0000 .
C17 H17B 0.9900 .
C17 H17A 0.9900 .
C5 H5B 0.9800 .
C5 H5A 0.9800 .
C5 H5C 0.9800 .
C9 H9C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C6 H6A 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C3 H3C 0.9800 .
C3 H26B 0.9800 .
C3 H3A 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O3 0.73(2) 2.10(2) 2.7949(16) 159(2) 2_565
