#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:39:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179255 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/75/4317599.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_4317599
loop_
_publ_author_name
'Timothy J. Boyle'
'Cecilia A. Zechmann'
'Todd M. Alam'
'Mark A. Rodriguez'
'Cybele A. Hijar'
'Brian L. Scott'
_publ_section_title
;
 From Clusters to Ionic Complexes: Structurally Characterized Thallium
 Titanium Double Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              946
_journal_page_last               957
_journal_paper_doi               10.1021/ic0110833
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H45 O5 Ti Tl'
_chemical_formula_weight         858.03
_chemical_name_common            Tl[Ti(DMP)5]
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1148(12)
_cell_length_b                   10.5537(7)
_cell_length_c                   19.6490(13)
_cell_measurement_temperature    168(2)
_cell_volume                     3549.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  '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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21462
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    4.802
_exptl_absorpt_correction_type   emperical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1712
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.411(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7633
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          1.021
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                6406
_reflns_number_total             7633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110833_6.cif
_cod_data_source_block           cz037m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317599
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1331(4) 0.5477(6) 0.1132(3) 0.0226(13) Uani 1 1 d . . .
C2 C 0.1936(4) 0.4789(6) 0.0797(3) 0.0249(13) Uani 1 1 d . . .
C3 C 0.2168(4) 0.5183(7) 0.0151(3) 0.0313(15) Uani 1 1 d . . .
H3 H 0.2577 0.4738 -0.0072 0.038 Uiso 1 1 calc R . .
C4 C 0.1825(4) 0.6197(7) -0.0180(4) 0.0381(16) Uani 1 1 d . . .
H4 H 0.1988 0.6433 -0.0624 0.046 Uiso 1 1 calc R . .
C5 C 0.1238(5) 0.6865(6) 0.0153(3) 0.0360(17) Uani 1 1 d . . .
H5 H 0.1013 0.7583 -0.0063 0.043 Uiso 1 1 calc R . .
C6 C 0.0968(4) 0.6508(6) 0.0798(3) 0.0270(13) Uani 1 1 d . . .
C7 C 0.2337(4) 0.3682(7) 0.1130(4) 0.0301(14) Uani 1 1 d . . .
H7A H 0.1990 0.2944 0.1122 0.045 Uiso 1 1 calc R . .
H7B H 0.2463 0.3898 0.1603 0.045 Uiso 1 1 calc R . .
H7C H 0.2819 0.3484 0.0884 0.045 Uiso 1 1 calc R . .
C8 C 0.0332(4) 0.7220(7) 0.1154(4) 0.0338(15) Uani 1 1 d . . .
H8A H -0.0069 0.6623 0.1311 0.051 Uiso 1 1 calc R . .
H8B H 0.0096 0.7829 0.0839 0.051 Uiso 1 1 calc R . .
H8C H 0.0550 0.7672 0.1546 0.051 Uiso 1 1 calc R . .
C9 C 0.2600(4) 0.5315(6) 0.2678(3) 0.0238(12) Uani 1 1 d . . .
C10 C 0.2836(4) 0.6322(7) 0.2260(3) 0.0260(14) Uani 1 1 d . . .
C11 C 0.3580(4) 0.6230(7) 0.1970(4) 0.0306(16) Uani 1 1 d . . .
H11 H 0.3747 0.6879 0.1668 0.037 Uiso 1 1 calc R . .
C12 C 0.4085(4) 0.5231(7) 0.2105(3) 0.0335(15) Uani 1 1 d . . .
H12 H 0.4580 0.5182 0.1888 0.040 Uiso 1 1 calc R . .
C13 C 0.3852(4) 0.4314(6) 0.2559(4) 0.0309(15) Uani 1 1 d . . .
H13 H 0.4200 0.3641 0.2667 0.037 Uiso 1 1 calc R . .
C14 C 0.3114(4) 0.4351(6) 0.2865(3) 0.0273(14) Uani 1 1 d . . .
C15 C 0.2344(4) 0.7469(6) 0.2150(4) 0.0314(15) Uani 1 1 d . . .
H15A H 0.2220 0.7857 0.2590 0.047 Uiso 1 1 calc R . .
H15B H 0.1859 0.7227 0.1919 0.047 Uiso 1 1 calc R . .
H15C H 0.2631 0.8078 0.1868 0.047 Uiso 1 1 calc R . .
C16 C 0.2902(4) 0.3437(6) 0.3418(3) 0.0334(15) Uani 1 1 d . . .
H16A H 0.3291 0.2756 0.3436 0.050 Uiso 1 1 calc R . .
H16B H 0.2386 0.3075 0.3325 0.050 Uiso 1 1 calc R . .
H16C H 0.2891 0.3881 0.3856 0.050 Uiso 1 1 calc R . .
C17 C 0.0988(4) 0.4191(6) 0.4179(3) 0.0256(13) Uani 1 1 d . . .
C18 C 0.0870(4) 0.2936(7) 0.4363(4) 0.0352(16) Uani 1 1 d . . .
C19 C 0.1288(6) 0.2481(9) 0.4939(4) 0.062(3) Uani 1 1 d . . .
H19 H 0.1221 0.1621 0.5070 0.075 Uiso 1 1 calc R . .
C20 C 0.1776(6) 0.3219(12) 0.5308(4) 0.060(3) Uani 1 1 d . . .
H20 H 0.2059 0.2869 0.5679 0.072 Uiso 1 1 calc R . .
C21 C 0.1860(5) 0.4466(11) 0.5144(4) 0.057(3) Uani 1 1 d . . .
H21 H 0.2187 0.4989 0.5415 0.068 Uiso 1 1 calc R . .
C22 C 0.1468(4) 0.4995(8) 0.4577(3) 0.0389(19) Uani 1 1 d . . .
C23 C 0.0311(5) 0.2123(8) 0.3968(4) 0.050(2) Uani 1 1 d . . .
H23A H -0.0185 0.2575 0.3910 0.075 Uiso 1 1 calc R . .
H23B H 0.0219 0.1331 0.4215 0.075 Uiso 1 1 calc R . .
H23C H 0.0535 0.1933 0.3520 0.075 Uiso 1 1 calc R . .
C24 C 0.1568(5) 0.6386(9) 0.4399(4) 0.050(2) Uani 1 1 d . . .
H24A H 0.1810 0.6831 0.4783 0.075 Uiso 1 1 calc R . .
H24B H 0.1055 0.6760 0.4304 0.075 Uiso 1 1 calc R . .
H24C H 0.1902 0.6465 0.3996 0.075 Uiso 1 1 calc R . .
C25 C -0.0376(4) 0.6735(6) 0.3131(3) 0.0248(14) Uani 1 1 d . . .
C26 C -0.1112(4) 0.6232(6) 0.3298(3) 0.0280(14) Uani 1 1 d . . .
C27 C -0.1592(4) 0.6907(6) 0.3744(3) 0.0293(14) Uani 1 1 d . . .
H27 H -0.2097 0.6587 0.3849 0.035 Uiso 1 1 calc R . .
C28 C -0.1347(4) 0.8040(7) 0.4039(3) 0.0340(15) Uani 1 1 d . . .
H28 H -0.1676 0.8486 0.4346 0.041 Uiso 1 1 calc R . .
C29 C -0.0622(5) 0.8495(7) 0.3878(4) 0.0349(16) Uani 1 1 d . . .
H29 H -0.0449 0.9258 0.4086 0.042 Uiso 1 1 calc R . .
C30 C -0.0125(5) 0.7884(7) 0.3418(4) 0.0324(17) Uani 1 1 d . . .
C31 C -0.1377(4) 0.5004(7) 0.2979(4) 0.0346(16) Uani 1 1 d . . .
H31A H -0.1409 0.5106 0.2485 0.052 Uiso 1 1 calc R . .
H31B H -0.1892 0.4775 0.3159 0.052 Uiso 1 1 calc R . .
H31C H -0.1002 0.4332 0.3088 0.052 Uiso 1 1 calc R . .
C32 C 0.0639(4) 0.8463(7) 0.3198(4) 0.0399(17) Uani 1 1 d . . .
H32A H 0.0585 0.8804 0.2736 0.060 Uiso 1 1 calc R . .
H32B H 0.1048 0.7813 0.3202 0.060 Uiso 1 1 calc R . .
H32C H 0.0781 0.9147 0.3511 0.060 Uiso 1 1 calc R . .
C33 C 0.0561(4) 0.2447(6) 0.1902(3) 0.0239(13) Uani 1 1 d . . .
C34 C 0.1104(4) 0.1457(6) 0.1860(3) 0.0287(14) Uani 1 1 d . . .
C35 C 0.1094(5) 0.0668(6) 0.1297(4) 0.0364(17) Uani 1 1 d . . .
H35 H 0.1462 -0.0003 0.1266 0.044 Uiso 1 1 calc R . .
C36 C 0.0562(5) 0.0834(7) 0.0780(5) 0.042(2) Uani 1 1 d . . .
H36 H 0.0568 0.0296 0.0393 0.051 Uiso 1 1 calc R . .
C37 C 0.0013(5) 0.1809(7) 0.0834(4) 0.0368(18) Uani 1 1 d . . .
H37 H -0.0361 0.1920 0.0481 0.044 Uiso 1 1 calc R . .
C38 C 0.0000(5) 0.2612(6) 0.1387(4) 0.0312(15) Uani 1 1 d . . .
C39 C 0.1733(5) 0.1281(7) 0.2393(4) 0.040(2) Uani 1 1 d . . .
H39A H 0.2133 0.1937 0.2338 0.061 Uiso 1 1 calc R . .
H39B H 0.1972 0.0444 0.2340 0.061 Uiso 1 1 calc R . .
H39C H 0.1501 0.1349 0.2848 0.061 Uiso 1 1 calc R . .
C40 C -0.0625(5) 0.3599(7) 0.1447(4) 0.0389(17) Uani 1 1 d . . .
H40A H -0.0936 0.3615 0.1028 0.058 Uiso 1 1 calc R . .
H40B H -0.0385 0.4430 0.1519 0.058 Uiso 1 1 calc R . .
H40C H -0.0965 0.3396 0.1833 0.058 Uiso 1 1 calc R . .
O1 O 0.1103(3) 0.5157(4) 0.1751(2) 0.0238(10) Uani 1 1 d . . .
O2 O 0.1866(2) 0.5319(4) 0.2945(2) 0.0249(9) Uani 1 1 d . . .
O3 O 0.0610(3) 0.4676(4) 0.3636(2) 0.0247(9) Uani 1 1 d . . .
O4 O 0.0071(3) 0.6139(4) 0.2671(2) 0.0265(9) Uani 1 1 d . . .
O5 O 0.0561(3) 0.3224(4) 0.2461(2) 0.0261(10) Uani 1 1 d . . .
Ti1 Ti 0.08606(6) 0.48890(10) 0.26735(5) 0.0188(2) Uani 1 1 d . . .
Tl1 Tl 0.456410(12) 0.929055(19) 0.47562(2) 0.02942(8) 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'
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'
Tl Tl -2.8358 9.6688 '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
O1 C1 C6 119.5(6) . . ?
O1 C1 C2 120.6(6) . . ?
C6 C1 C2 119.8(6) . . ?
C3 C2 C1 118.3(6) . . ?
C3 C2 C7 120.0(6) . . ?
C1 C2 C7 121.6(6) . . ?
C4 C3 C2 122.6(7) . . ?
C3 C4 C5 118.6(7) . . ?
C4 C5 C6 121.8(7) . . ?
C5 C6 C1 118.7(6) . . ?
C5 C6 C8 121.9(6) . . ?
C1 C6 C8 119.3(6) . . ?
O2 C9 C14 118.8(6) . . ?
O2 C9 C10 119.2(6) . . ?
C14 C9 C10 121.8(6) . . ?
C11 C10 C9 116.6(6) . . ?
C11 C10 C15 120.7(7) . . ?
C9 C10 C15 122.6(6) . . ?
C12 C11 C10 122.8(7) . . ?
C13 C12 C11 118.5(6) . . ?
C12 C13 C14 121.4(6) . . ?
C9 C14 C13 118.4(6) . . ?
C9 C14 C16 120.6(6) . . ?
C13 C14 C16 120.8(6) . . ?
O3 C17 C18 120.0(6) . . ?
O3 C17 C22 119.2(6) . . ?
C18 C17 C22 120.7(6) . . ?
C17 C18 C19 117.2(8) . . ?
C17 C18 C23 120.1(7) . . ?
C19 C18 C23 122.6(8) . . ?
C20 C19 C18 122.9(9) . . ?
C19 C20 C21 119.6(8) . . ?
C20 C21 C22 121.1(9) . . ?
C21 C22 C17 118.3(8) . . ?
C21 C22 C24 120.6(7) . . ?
C17 C22 C24 121.1(6) . . ?
O4 C25 C30 120.1(6) . . ?
O4 C25 C26 119.4(6) . . ?
C30 C25 C26 120.4(6) . . ?
C27 C26 C25 118.7(6) . . ?
C27 C26 C31 121.4(6) . . ?
C25 C26 C31 119.8(6) . . ?
C28 C27 C26 121.5(6) . . ?
C29 C28 C27 118.5(6) . . ?
C28 C29 C30 122.7(7) . . ?
C29 C30 C25 118.1(7) . . ?
C29 C30 C32 121.8(7) . . ?
C25 C30 C32 120.0(7) . . ?
O5 C33 C34 119.5(6) . . ?
O5 C33 C38 120.2(6) . . ?
C34 C33 C38 120.3(6) . . ?
C35 C34 C33 119.1(7) . . ?
C35 C34 C39 119.3(6) . . ?
C33 C34 C39 121.5(6) . . ?
C36 C35 C34 121.5(7) . . ?
C35 C36 C37 118.9(7) . . ?
C38 C37 C36 121.5(8) . . ?
C37 C38 C33 118.7(7) . . ?
C37 C38 C40 120.1(7) . . ?
C33 C38 C40 121.2(6) . . ?
C1 O1 Ti1 172.2(4) . . ?
C9 O2 Ti1 137.9(4) . . ?
C17 O3 Ti1 134.8(4) . . ?
C25 O4 Ti1 137.2(4) . . ?
C33 O5 Ti1 137.6(4) . . ?
O2 Ti1 O5 123.0(2) . . ?
O2 Ti1 O1 92.05(19) . . ?
O5 Ti1 O1 89.3(2) . . ?
O2 Ti1 O4 119.5(2) . . ?
O5 Ti1 O4 117.3(2) . . ?
O1 Ti1 O4 92.9(2) . . ?
O2 Ti1 O3 87.32(19) . . ?
O5 Ti1 O3 92.7(2) . . ?
O1 Ti1 O3 178.0(2) . . ?
O4 Ti1 O3 85.73(19) . . ?
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
C1 O1 1.320(7) . ?
C1 C6 1.415(9) . ?
C1 C2 1.426(9) . ?
C2 C3 1.393(9) . ?
C2 C7 1.505(9) . ?
C3 C4 1.382(11) . ?
C4 C5 1.391(10) . ?
C5 C6 1.401(9) . ?
C6 C8 1.496(10) . ?
C9 O2 1.362(7) . ?
C9 C14 1.394(9) . ?
C9 C10 1.402(9) . ?
C10 C11 1.399(9) . ?
C10 C15 1.490(9) . ?
C11 C12 1.389(11) . ?
C12 C13 1.375(10) . ?
C13 C14 1.401(9) . ?
C14 C16 1.497(9) . ?
C17 O3 1.348(8) . ?
C17 C18 1.388(10) . ?
C17 C22 1.417(10) . ?
C18 C19 1.421(11) . ?
C18 C23 1.502(12) . ?
C19 C20 1.353(14) . ?
C20 C21 1.363(13) . ?
C21 C22 1.415(11) . ?
C22 C24 1.519(13) . ?
C25 O4 1.341(7) . ?
C25 C30 1.405(10) . ?
C25 C26 1.406(9) . ?
C26 C27 1.397(9) . ?
C26 C31 1.509(10) . ?
C27 C28 1.393(10) . ?
C28 C29 1.368(10) . ?
C29 C30 1.398(10) . ?
C30 C32 1.506(10) . ?
C33 O5 1.372(7) . ?
C33 C34 1.401(9) . ?
C33 C38 1.406(9) . ?
C34 C35 1.385(9) . ?
C34 C39 1.514(11) . ?
C35 C36 1.374(12) . ?
C36 C37 1.397(12) . ?
C37 C38 1.378(10) . ?
C38 C40 1.498(10) . ?
O1 Ti1 1.882(4) . ?
O2 Ti1 1.857(4) . ?
O3 Ti1 1.953(4) . ?
O4 Ti1 1.888(4) . ?
O5 Ti1 1.877(4) . ?
