#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340230.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_4340230
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         'C30 H32 O10 Ti2, 2(C3 H8 O), 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H52 Cl4 O12 Ti2'
_chemical_formula_weight         938.40
_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                116.6880(10)
_cell_angle_beta                 98.5910(10)
_cell_angle_gamma                102.9490(10)
_cell_formula_units_Z            1
_cell_length_a                   8.51300(10)
_cell_length_b                   12.4810(2)
_cell_length_c                   12.6270(2)
_cell_measurement_reflns_used    12809
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      3.59
_cell_volume                     1119.02(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12809
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.8386
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0327
_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)+(0.0382P)²+0.6013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                3571
_reflns_number_total             3921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051708nsi20051004_093209.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340230
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 0.68423(4) 0.52072(3) -0.03046(3) 0.01903(11) Uani 1 1 d .
O3 O 0.56405(15) 0.54126(11) 0.10718(11) 0.0210(3) Uani 1 1 d .
O4 O 0.77697(15) 0.52808(11) -0.15377(11) 0.0223(3) Uani 1 1 d .
O2 O 0.86146(15) 0.55772(12) 0.10118(11) 0.0232(3) Uani 1 1 d .
O5 O 0.71061(16) 0.69557(11) 0.01454(11) 0.0248(3) Uani 1 1 d .
O1 O 0.66219(18) 0.33298(13) -0.10947(13) 0.0242(3) Uani 1 1 d .
C15 C 0.7682(2) 0.73269(17) -0.06242(16) 0.0228(4) Uani 1 1 d .
C9 C 0.6686(2) 0.56618(16) 0.21525(16) 0.0206(4) Uani 1 1 d .
C10 C 0.8061(2) 0.63821(17) -0.15767(17) 0.0225(4) Uani 1 1 d .
C4 C 0.8342(2) 0.57536(16) 0.20997(16) 0.0215(4) Uani 1 1 d .
C8 C 0.6231(2) 0.58400(18) 0.32047(17) 0.0258(4) Uani 1 1 d .
H8 H 0.5104 0.5775 0.3229 0.031 Uiso 1 1 calc R
C7 C 0.7471(3) 0.6119(2) 0.42367(18) 0.0322(5) Uani 1 1 d .
H7 H 0.7189 0.6250 0.4976 0.039 Uiso 1 1 calc R
C5 C 0.9565(2) 0.60269(18) 0.31220(17) 0.0267(4) Uani 1 1 d .
H5 H 1.0690 0.6090 0.3097 0.032 Uiso 1 1 calc R
C1 C 0.7836(2) 0.27637(18) -0.07989(19) 0.0295(4) Uani 1 1 d .
H1A H 0.8960 0.3443 -0.0336 0.035 Uiso 1 1 calc R
C13 C 0.8529(3) 0.87166(19) -0.1402(2) 0.0371(5) Uani 1 1 d .
H13 H 0.8698 0.9519 -0.1350 0.045 Uiso 1 1 calc R
C3 C 0.7296(3) 0.2275(2) 0.0031(2) 0.0414(5) Uani 1 1 d .
H3C H 0.7207 0.2971 0.0775 0.062 Uiso 1 1 calc R
H3B H 0.8130 0.1935 0.0269 0.062 Uiso 1 1 calc R
H3A H 0.6200 0.1601 -0.0411 0.062 Uiso 1 1 calc R
C6 C 0.9111(3) 0.6207(2) 0.41919(18) 0.0317(4) Uani 1 1 d .
H6 H 0.9938 0.6394 0.4901 0.038 Uiso 1 1 calc R
C2 C 0.7984(3) 0.1752(2) -0.1978(2) 0.0440(6) Uani 1 1 d .
H2C H 0.6921 0.1042 -0.2409 0.066 Uiso 1 1 calc R
H2B H 0.8893 0.1449 -0.1783 0.066 Uiso 1 1 calc R
H2A H 0.8233 0.2106 -0.2511 0.066 Uiso 1 1 calc R
C14 C 0.7909(3) 0.85036(19) -0.05215(19) 0.0319(4) Uani 1 1 d .
H15 H 0.7654 0.9148 0.0125 0.038 Uiso 1 1 calc R
C11 C 0.8659(2) 0.65930(19) -0.24489(18) 0.0298(4) Uani 1 1 d .
H11 H 0.8901 0.5946 -0.3103 0.036 Uiso 1 1 calc R
C12 C 0.8897(3) 0.7785(2) -0.23392(19) 0.0359(5) Uani 1 1 d .
H12 H 0.9321 0.7956 -0.2922 0.043 Uiso 1 1 calc R
Cl2 Cl 0.58773(10) 0.12367(7) 0.20964(7) 0.0640(2) Uani 1 1 d .
Cl1 Cl 0.62173(10) 0.32189(9) 0.45733(7) 0.0710(2) Uani 1 1 d .
C19 C 0.5918(4) 0.2801(2) 0.3013(2) 0.0513(6) Uani 1 1 d .
H19A H 0.4844 0.2889 0.2700 0.062 Uiso 1 1 calc R
H19B H 0.6839 0.3391 0.2947 0.062 Uiso 1 1 calc R
O6 O 0.62972(17) 0.84141(13) 0.21812(13) 0.0308(3) Uani 1 1 d .
C16 C 0.7509(2) 0.90028(18) 0.33748(18) 0.0298(4) Uani 1 1 d .
H16 H 0.8015 0.8370 0.3422 0.036 Uiso 1 1 calc R
C17 C 0.8881(3) 1.0117(2) 0.3541(2) 0.0409(5) Uani 1 1 d .
H17B H 0.9453 0.9818 0.2900 0.061 Uiso 1 1 calc R
H17C H 0.9694 1.0528 0.4359 0.061 Uiso 1 1 calc R
H17A H 0.8386 1.0729 0.3473 0.061 Uiso 1 1 calc R
C18 C 0.6557(3) 0.9375(3) 0.4316(2) 0.0528(6) Uani 1 1 d .
H18A H 0.6050 0.9989 0.4267 0.079 Uiso 1 1 calc R
H18B H 0.7329 0.9759 0.5145 0.079 Uiso 1 1 calc R
H18C H 0.5670 0.8619 0.4150 0.079 Uiso 1 1 calc R
H1 H 0.582(3) 0.284(2) -0.146(2) 0.024(6) Uiso 1 1 d .
H6A H 0.674(3) 0.810(2) 0.167(2) 0.046(8) 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 O4 107.54(5) . .
O2 Ti1 O5 96.34(6) . .
O4 Ti1 O5 80.67(5) . .
O2 Ti1 O3 147.60(5) . 2_665
O4 Ti1 O3 104.37(5) . 2_665
O5 Ti1 O3 94.18(5) . 2_665
O2 Ti1 O1 89.76(6) . .
O4 Ti1 O1 88.73(5) . .
O5 Ti1 O1 168.95(5) . .
O3 Ti1 O1 85.42(5) 2_665 .
O2 Ti1 O3 78.32(5) . .
O4 Ti1 O3 168.64(5) . .
O5 Ti1 O3 89.09(5) . .
O3 Ti1 O3 71.29(5) 2_665 .
O1 Ti1 O3 101.19(5) . .
O2 Ti1 Ti1 112.31(4) . 2_665
O4 Ti1 Ti1 140.03(4) . 2_665
O5 Ti1 Ti1 91.94(4) . 2_665
O3 Ti1 Ti1 36.62(3) 2_665 2_665
O1 Ti1 Ti1 94.26(4) . 2_665
O3 Ti1 Ti1 34.68(3) . 2_665
C9 O3 Ti1 136.06(11) . 2_665
C9 O3 Ti1 113.36(10) . .
Ti1 O3 Ti1 108.71(5) 2_665 .
C10 O4 Ti1 117.35(11) . .
C4 O2 Ti1 120.39(11) . .
C15 O5 Ti1 115.42(11) . .
C1 O1 Ti1 127.94(12) . .
C1 O1 H1 109.6(18) . .
Ti1 O1 H1 120.8(18) . .
O5 C15 C14 125.94(17) . .
O5 C15 C10 113.18(15) . .
C14 C15 C10 120.88(17) . .
O3 C9 C8 125.67(16) . .
O3 C9 C4 112.57(15) . .
C8 C9 C4 121.75(16) . .
O4 C10 C11 125.70(17) . .
O4 C10 C15 113.21(15) . .
C11 C10 C15 121.09(17) . .
O2 C4 C5 124.68(16) . .
O2 C4 C9 115.33(15) . .
C5 C4 C9 119.98(16) . .
C9 C8 C7 118.10(17) . .
C9 C8 H8 120.9 . .
C7 C8 H8 120.9 . .
C6 C7 C8 120.56(17) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C4 C5 C6 118.56(17) . .
C4 C5 H5 120.7 . .
C6 C5 H5 120.7 . .
O1 C1 C2 109.57(17) . .
O1 C1 C3 108.82(16) . .
C2 C1 C3 113.27(18) . .
O1 C1 H1A 108.4 . .
C2 C1 H1A 108.4 . .
C3 C1 H1A 108.4 . .
C12 C13 C14 121.19(18) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C1 C3 H3C 109.5 . .
C1 C3 H3B 109.5 . .
H3C C3 H3B 109.5 . .
C1 C3 H3A 109.5 . .
H3C C3 H3A 109.5 . .
H3B C3 H3A 109.5 . .
C7 C6 C5 121.05(17) . .
C7 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C1 C2 H2C 109.5 . .
C1 C2 H2B 109.5 . .
H2C C2 H2B 109.5 . .
C1 C2 H2A 109.5 . .
H2C C2 H2A 109.5 . .
H2B C2 H2A 109.5 . .
C15 C14 C13 117.83(19) . .
C15 C14 H15 121.1 . .
C13 C14 H15 121.1 . .
C10 C11 C12 117.94(19) . .
C10 C11 H11 121.0 . .
C12 C11 H11 121.0 . .
C13 C12 C11 121.07(18) . .
C13 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
Cl2 C19 Cl1 111.68(14) . .
Cl2 C19 H19A 109.3 . .
Cl1 C19 H19A 109.3 . .
Cl2 C19 H19B 109.3 . .
Cl1 C19 H19B 109.3 . .
H19A C19 H19B 107.9 . .
C16 O6 H6A 108.0(19) . .
O6 C16 C18 106.56(17) . .
O6 C16 C17 109.43(16) . .
C18 C16 C17 113.13(19) . .
O6 C16 H16 109.2 . .
C18 C16 H16 109.2 . .
C17 C16 H16 109.2 . .
C16 C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C17 H17A 109.5 . .
H17B C17 H17A 109.5 . .
H17C C17 H17A 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 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 1.8712(12) .
Ti1 O4 1.8761(12) .
Ti1 O5 1.9401(12) .
Ti1 O3 1.9967(12) 2_665
Ti1 O1 2.0416(14) .
Ti1 O3 2.0931(12) .
Ti1 Ti1 3.3240(6) 2_665
O3 C9 1.372(2) .
O3 Ti1 1.9967(12) 2_665
O4 C10 1.366(2) .
O2 C4 1.355(2) .
O5 C15 1.358(2) .
O1 C1 1.468(2) .
O1 H1 0.72(2) .
C15 C14 1.380(3) .
C15 C10 1.398(3) .
C9 C8 1.376(2) .
C9 C4 1.402(3) .
C10 C11 1.382(3) .
C4 C5 1.382(3) .
C8 C7 1.397(3) .
C8 H8 0.9500 .
C7 C6 1.387(3) .
C7 H7 0.9500 .
C5 C6 1.395(3) .
C5 H5 0.9500 .
C1 C2 1.506(3) .
C1 C3 1.508(3) .
C1 H1A 1.0000 .
C13 C12 1.375(3) .
C13 C14 1.400(3) .
C13 H13 0.9500 .
C3 H3C 0.9800 .
C3 H3B 0.9800 .
C3 H3A 0.9800 .
C6 H6 0.9500 .
C2 H2C 0.9800 .
C2 H2B 0.9800 .
C2 H2A 0.9800 .
C14 H15 0.9500 .
C11 C12 1.394(3) .
C11 H11 0.9500 .
C12 H12 0.9500 .
Cl2 C19 1.755(3) .
Cl1 C19 1.756(3) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
O6 C16 1.441(2) .
O6 H6A 0.78(3) .
C16 C18 1.498(3) .
C16 C17 1.510(3) .
C16 H16 1.0000 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C17 H17A 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 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
O6 H6A O5 0.78(3) 1.94(3) 2.6987(19) 162(3) .
O1 H1 O6 0.72(2) 1.87(2) 2.583(2) 171(2) 2_665
