#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:29:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179330 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/27/4322711.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_4322711
loop_
_publ_author_name
'Paul D. Moran'
'Clifton E. F. Rickard'
'Graham A. Bowmaker'
'Ralph P. Cooney'
'John R. Bartlett'
'James L. Woolfrey'
_publ_section_title
;
 X-ray Structure and Raman Spectrum of
 [Ti4(μ3-O)2(μ2-OiPr)2(OiPr)8(acac)2]: Presence of a
 Ti4(μ3-O)2(μ2-OiPr)2 Ladder-like Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1417
_journal_page_last               1419
_journal_paper_doi               10.1021/ic970942d
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C20 H42 O8 Ti2'
_chemical_formula_weight         506.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 105.19(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   12.056(4)
_cell_length_b                   15.846(2)
_cell_length_c                   14.758(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      8.5
_cell_volume                     2720.9(11)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software'
_computing_data_reduction        'Local software'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4962
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_obs          0.0671
_refine_ls_shift/esd_max         0.184
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1567P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2431
_refine_ls_wR_factor_obs         0.1928
_reflns_number_observed          2996
_reflns_number_total             4696
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970942d.cif
_cod_data_source_block           C20H42O8Ti2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2720.9(10)
_cod_database_code               4322711
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.06235(9) 0.98070(7) 0.30967(7) 0.0353(3) Uani 1 d . .
Ti2 Ti 0.09173(8) 0.93087(6) 0.52210(7) 0.0307(3) Uani 1 d . .
O1 O 0.1965(4) 1.0674(3) 0.3625(3) 0.0496(11) Uani 1 d . .
O2 O 0.1648(4) 0.9493(3) 0.2263(3) 0.0509(11) Uani 1 d . .
C1 C 0.3492(7) 1.1630(6) 0.3829(6) 0.090(3) Uani 1 d . .
H1A H 0.3050(21) 1.2157(10) 0.3717(38) 0.136 Uiso 1 calc R .
H1B H 0.4186(29) 1.1692(28) 0.3607(34) 0.136 Uiso 1 calc R .
H1C H 0.3709(49) 1.1504(21) 0.4502(8) 0.136 Uiso 1 calc R .
C2 C 0.2767(6) 1.0919(5) 0.3303(5) 0.061(2) Uani 1 d . .
C3 C 0.3015(7) 1.0564(6) 0.2495(6) 0.072(2) Uani 1 d . .
H3 H 0.3589(7) 1.0827(6) 0.2257(6) 0.109 Uiso 1 calc R .
C4 C 0.2468(7) 0.9853(5) 0.2031(5) 0.061(2) Uani 1 d . .
C5 C 0.2855(8) 0.9467(8) 0.1246(7) 0.103(4) Uani 1 d . .
H5A H 0.3368(55) 0.9860(22) 0.1040(37) 0.154 Uiso 1 calc R .
H5B H 0.2186(10) 0.9347(47) 0.0721(22) 0.154 Uiso 1 calc R .
H5C H 0.3267(60) 0.8941(27) 0.1461(18) 0.154 Uiso 1 calc R .
O3 O -0.0318(3) 0.8955(3) 0.2583(3) 0.0416(10) Uani 1 d . .
C6 C -0.0705(8) 0.8502(5) 0.1738(5) 0.074(2) Uani 1 d . .
H6 H 0.0013(8) 0.8400(5) 0.1535(5) 0.110 Uiso 1 calc R 1
C7 C -0.1406(11) 0.8975(7) 0.0984(6) 0.117(4) Uani 1 d . .
H7A H -0.1589(64) 0.8632(21) 0.0412(16) 0.176 Uiso 1 calc R .
H7B H -0.0994(33) 0.9485(30) 0.0882(42) 0.176 Uiso 1 calc R .
H7C H -0.2120(36) 0.9136(49) 0.1138(27) 0.176 Uiso 1 calc R .
C8 C -0.1089(25) 0.7628(22) 0.1919(26) 0.084(8) Uani 0.60 d P 1
H8A H -0.1227(100) 0.7294(31) 0.1342(31) 0.125 Uiso 0.60 calc PR 1
H8B H -0.1800(64) 0.7665(22) 0.2120(90) 0.125 Uiso 0.60 calc PR 1
H8C H -0.0490(53) 0.7358(36) 0.2412(60) 0.125 Uiso 0.60 calc PR 1
C8' C -0.1616(39) 0.7856(33) 0.1987(36) 0.098(16) Uani 0.40 d P 2
H8'1 H -0.1907(137) 0.7473(91) 0.1456(64) 0.147 Uiso 0.40 calc PR 2
H8'2 H -0.2257(94) 0.8175(34) 0.2111(147) 0.147 Uiso 0.40 calc PR 2
H8'3 H -0.1237(59) 0.7527(95) 0.2544(89) 0.147 Uiso 0.40 calc PR 2
O4 O -0.0106(4) 1.0649(3) 0.2367(3) 0.0481(11) Uani 1 d . .
C9 C -0.0071(11) 1.1436(6) 0.1962(8) 0.103(4) Uani 1 d . .
H9 H 0.0726(11) 1.1648(6) 0.2246(8) 0.155 Uiso 1 calc R .
C10 C -0.0150(12) 1.1340(7) 0.0940(6) 0.127(5) Uani 1 d . .
H10A H 0.0326(63) 1.0862(38) 0.0848(9) 0.190 Uiso 1 calc R .
H10B H 0.0123(76) 1.1857(24) 0.0705(16) 0.190 Uiso 1 calc R .
H10C H -0.0952(17) 1.1236(57) 0.0596(11) 0.190 Uiso 1 calc R .
C11 C -0.0786(15) 1.2042(7) 0.2181(9) 0.156(6) Uani 1 d . .
H11A H -0.0682(73) 1.2577(20) 0.1880(67) 0.234 Uiso 1 calc R .
H11B H -0.0594(67) 1.2120(52) 0.2863(11) 0.234 Uiso 1 calc R .
H11C H -0.1587(16) 1.1858(33) 0.1955(70) 0.234 Uiso 1 calc R .
O5 O 0.1592(3) 0.9054(2) 0.4176(3) 0.0381(9) Uani 1 d . .
C12 C 0.2469(6) 0.8406(4) 0.4279(5) 0.048(2) Uani 1 d . .
H12 H 0.2547(6) 0.8114(4) 0.4893(5) 0.072 Uiso 1 calc R .
C13 C 0.3592(6) 0.8813(5) 0.4298(5) 0.064(2) Uani 1 d . .
H13A H 0.4192(10) 0.8380(7) 0.4389(38) 0.096 Uiso 1 calc R .
H13B H 0.3790(23) 0.9220(25) 0.4815(24) 0.096 Uiso 1 calc R .
H13C H 0.3532(14) 0.9105(29) 0.3702(16) 0.096 Uiso 1 calc R .
C14 C 0.2112(7) 0.7762(5) 0.3505(5) 0.065(2) Uani 1 d . .
H14A H 0.2683(24) 0.7308(17) 0.3604(21) 0.098 Uiso 1 calc R .
H14B H 0.2058(43) 0.8033(9) 0.2898(6) 0.098 Uiso 1 calc R .
H14C H 0.1362(22) 0.7526(24) 0.3510(24) 0.098 Uiso 1 calc R .
O6 O 0.0473(4) 0.8264(3) 0.5384(3) 0.0514(12) Uani 1 d . .
C15 C -0.0382(24) 0.7630(16) 0.5177(22) 0.118(12) Uani 0.55 d P 3
H15 H 0.0000 0.7559 0.5797 0.177 Uiso 0.55 d P 3
C15' C -0.0297(28) 0.7675(14) 0.4720(14) 0.059(7) Uani 0.45 d P 4
H15' H 0.0000 0.7759 0.4067 0.089 Uiso 0.45 d P 4
C16 C 0.0176(12) 0.6781(6) 0.5140(10) 0.134(5) Uani 1 d . .
H16A H 0.0000 0.6396 0.4754 0.201 Uiso 1 d . .
H16B H 0.0476 0.6564 0.5763 0.201 Uiso 1 d . .
H16C H 0.0825 0.6842 0.4832 0.201 Uiso 1 d . .
C17 C -0.1429(10) 0.7778(10) 0.4758(13) 0.170(7) Uani 1 d . .
H17A H 0.0000 0.7386 0.4293 0.255 Uiso 1 d . .
H17B H 0.0000 0.8361 0.4553 0.255 Uiso 1 d . .
H17C H 0.0000 0.7671 0.5370 0.255 Uiso 1 d . .
O7 O 0.2211(3) 0.9494(3) 0.6099(3) 0.0514(12) Uani 1 d . .
C18 C 0.2830(6) 1.0062(5) 0.6781(5) 0.056(2) Uani 1 d . .
H18 H 0.2290(6) 1.0507(5) 0.6887(5) 0.084 Uiso 1 calc R .
C19 C 0.3756(9) 1.0478(7) 0.6440(8) 0.106(4) Uani 1 d . .
H19A H 0.4211(45) 1.0844(40) 0.6934(23) 0.159 Uiso 1 calc R .
H19B H 0.3410(9) 1.0816(41) 0.5882(35) 0.159 Uiso 1 calc R .
H19C H 0.4255(41) 1.0046(7) 0.6281(54) 0.159 Uiso 1 calc R .
C20 C 0.3298(8) 0.9603(7) 0.7675(6) 0.086(3) Uani 1 d . .
H20A H 0.3793(48) 0.9982(14) 0.8132(17) 0.129 Uiso 1 calc R .
H20B H 0.3747(49) 0.9117(26) 0.7563(11) 0.129 Uiso 1 calc R .
H20C H 0.2663(9) 0.9407(37) 0.7921(25) 0.129 Uiso 1 calc R .
O8 O 0.0087(3) 1.0031(2) 0.4204(2) 0.0316(9) Uani 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'
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
_geom_angle_publ_flag
O4 Ti1 O3 98.6(2) . . ?
O4 Ti1 O8 98.6(2) . . ?
O3 Ti1 O8 100.3(2) . . ?
O4 Ti1 O2 95.7(2) . . ?
O3 Ti1 O2 88.7(2) . . ?
O8 Ti1 O2 161.6(2) . . ?
O4 Ti1 O5 166.5(2) . . ?
O3 Ti1 O5 93.3(2) . . ?
O8 Ti1 O5 72.8(2) . . ?
O2 Ti1 O5 90.9(2) . . ?
O4 Ti1 O1 86.9(2) . . ?
O3 Ti1 O1 169.3(2) . . ?
O8 Ti1 O1 87.8(2) . . ?
O2 Ti1 O1 81.6(2) . . ?
O5 Ti1 O1 82.5(2) . . ?
O7 Ti2 O6 107.1(2) . . ?
O7 Ti2 O8 130.1(2) . . ?
O6 Ti2 O8 122.7(2) . . ?
O7 Ti2 O8 96.9(2) . 3_576 ?
O6 Ti2 O8 101.4(2) . 3_576 ?
O8 Ti2 O8 76.6(2) . 3_576 ?
O7 Ti2 O5 98.2(2) . . ?
O6 Ti2 O5 96.7(2) . . ?
O8 Ti2 O5 75.5(2) . . ?
O8 Ti2 O5 151.9(2) 3_576 . ?
C2 O1 Ti1 131.1(5) . . ?
C4 O2 Ti1 134.5(5) . . ?
O1 C2 C3 123.6(7) . . ?
O1 C2 C1 116.0(8) . . ?
C3 C2 C1 120.4(8) . . ?
C4 C3 C2 123.9(7) . . ?
O2 C4 C3 122.3(7) . . ?
O2 C4 C5 117.0(8) . . ?
C3 C4 C5 120.7(8) . . ?
C6 O3 Ti1 141.4(5) . . ?
O3 C6 C7 114.5(8) . . ?
O3 C6 C8 110.9(15) . . ?
C7 C6 C8 118.5(15) . . ?
O3 C6 C8' 102.1(17) . . ?
C7 C6 C8' 102.3(20) . . ?
C9 O4 Ti1 149.4(6) . . ?
C11 C9 O4 115.6(9) . . ?
C11 C9 C10 115.3(11) . . ?
O4 C9 C10 110.0(9) . . ?
C12 O5 Ti2 120.2(4) . . ?
C12 O5 Ti1 136.9(4) . . ?
Ti2 O5 Ti1 102.6(2) . . ?
O5 C12 C13 109.2(5) . . ?
O5 C12 C14 110.1(5) . . ?
C13 C12 C14 112.6(6) . . ?
C15 O6 Ti2 149.5(10) . . ?
C15' O6 Ti2 130.9(9) . . ?
C17 C15 O6 123.2(19) . . ?
C17 C15 C16 122.7(23) . . ?
O6 C15 C16 109.5(19) . . ?
C17 C15' O6 110.4(17) . . ?
C17 C15' C16 110.2(16) . . ?
O6 C15' C16 101.8(17) . . ?
C18 O7 Ti2 145.9(4) . . ?
O7 C18 C20 109.2(7) . . ?
O7 C18 C19 110.2(7) . . ?
C20 C18 C19 111.9(7) . . ?
Ti1 O8 Ti2 109.0(2) . . ?
Ti1 O8 Ti2 147.6(2) . 3_576 ?
Ti2 O8 Ti2 103.4(2) . 3_576 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O4 1.793(4) . ?
Ti1 O3 1.798(4) . ?
Ti1 O8 1.941(4) . ?
Ti1 O2 2.020(4) . ?
Ti1 O5 2.086(4) . ?
Ti1 O1 2.110(4) . ?
Ti2 O7 1.771(4) . ?
Ti2 O6 1.775(4) . ?
Ti2 O8 1.943(4) . ?
Ti2 O8 1.955(4) 3_576 ?
Ti2 O5 1.965(4) . ?
O1 C2 1.246(8) . ?
O2 C4 1.264(9) . ?
C1 C2 1.511(11) . ?
C2 C3 1.419(12) . ?
C3 C4 1.392(12) . ?
C4 C5 1.488(11) . ?
O3 C6 1.409(8) . ?
C6 C7 1.423(12) . ?
C6 C8 1.50(4) . ?
C6 C8' 1.61(5) . ?
O4 C9 1.388(9) . ?
C9 C11 1.38(2) . ?
C9 C10 1.495(14) . ?
O5 C12 1.453(7) . ?
C12 C13 1.493(10) . ?
C12 C14 1.508(10) . ?
O6 C15 1.41(3) . ?
O6 C15' 1.49(2) . ?
C15 C17 1.27(3) . ?
C15 C16 1.51(3) . ?
C15' C17 1.39(3) . ?
C15' C16 1.59(3) . ?
O7 C18 1.410(8) . ?
C18 C20 1.483(11) . ?
C18 C19 1.492(12) . ?
O8 Ti2 1.955(4) 3_576 ?
