#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051827.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_7051827
loop_
_publ_author_name
'Nogai, Stefan D.'
'Schuster, Oliver'
'Bruce, Jocelyn'
'Raubenheimer, Helgard G.'
_publ_section_title
;
 Titanoxycarbene complexes of Ti(iv) with O- and N-donor ligands
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              540
_journal_paper_doi               10.1039/b715075j
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         'C32 H48 O18 Ti2 W2'
_chemical_formula_sum            'C32 H48 O18 Ti2 W2'
_chemical_formula_weight         1184.20
_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                108.787(1)
_cell_angle_beta                 107.558(1)
_cell_angle_gamma                91.644(1)
_cell_formula_units_Z            1
_cell_length_a                   9.6870(5)
_cell_length_b                   10.6893(6)
_cell_length_c                   11.7611(6)
_cell_measurement_reflns_used    4962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.23
_cell_measurement_theta_min      26.77
_cell_volume                     1088.50(10)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6461
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    5.687
_exptl_absorpt_correction_T_max  0.6001
_exptl_absorpt_correction_T_min  0.4248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.352
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0250
_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)+(0.0326P)²+2.5027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                4311
_reflns_number_total             4503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715075j.txt
_cod_data_source_block           '[{(OC)5W=C(Me)OTi(OiPr)2}(OiPr)]2'
_cod_original_cell_volume        1088.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051827
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.274353(15) 0.265491(14) 0.543583(13) 0.01866(6) Uani 1 1 d . . .
C3 C 0.0625(4) 0.3043(4) 0.4921(4) 0.0264(8) Uani 1 1 d . . .
O3 O -0.0551(3) 0.3257(4) 0.4614(3) 0.0403(8) Uani 1 1 d . . .
Ti1 Ti 0.00769(7) 0.15392(6) 0.08043(6) 0.01521(13) Uani 1 1 d . . .
O4 O 0.1704(4) -0.0197(3) 0.5447(3) 0.0373(7) Uani 1 1 d . . .
C4 C 0.2059(4) 0.0822(4) 0.5427(4) 0.0239(8) Uani 1 1 d . . .
C5 C 0.4813(4) 0.2182(4) 0.5827(4) 0.0248(8) Uani 1 1 d . . .
O5 O 0.5962(3) 0.1886(3) 0.6049(3) 0.0376(7) Uani 1 1 d . . .
C6 C 0.3432(4) 0.4496(4) 0.5461(4) 0.0238(8) Uani 1 1 d . . .
O6 O 0.3797(4) 0.5537(3) 0.5494(3) 0.0345(7) Uani 1 1 d . . .
C2 C 0.2996(4) 0.3512(4) 0.7306(4) 0.0230(8) Uani 1 1 d . . .
O2 O 0.3137(3) 0.4031(3) 0.8358(3) 0.0309(6) Uani 1 1 d . . .
O11 O 0.1234(3) 0.1888(3) 0.2566(3) 0.0259(6) Uani 1 1 d . . .
C11 C 0.2407(4) 0.1829(4) 0.3394(4) 0.0208(7) Uani 1 1 d . . .
C12 C 0.3534(5) 0.1188(5) 0.2822(4) 0.0312(9) Uani 1 1 d . . .
H12A H 0.3128 0.0892 0.1893 0.047 Uiso 1 1 calc R . .
H12B H 0.3789 0.0419 0.3084 0.047 Uiso 1 1 calc R . .
H12C H 0.4412 0.1839 0.3121 0.047 Uiso 1 1 calc R . .
O41 O 0.0803(3) 0.3113(3) 0.0902(3) 0.0264(6) Uani 1 1 d . . .
C41 C 0.1530(6) 0.4454(5) 0.1498(6) 0.0508(15) Uani 1 1 d . . .
H41 H 0.1193 0.4902 0.0856 0.061 Uiso 1 1 calc R . .
C42 C 0.3075(6) 0.4494(6) 0.1776(6) 0.0583(16) Uani 1 1 d . . .
H42A H 0.3455 0.4035 0.2381 0.088 Uiso 1 1 calc R . .
H42B H 0.3542 0.5425 0.2146 0.088 Uiso 1 1 calc R . .
H42C H 0.3288 0.4049 0.0990 0.088 Uiso 1 1 calc R . .
C43 C 0.0995(5) 0.5165(4) 0.2586(4) 0.0334(10) Uani 1 1 d . . .
H43A H -0.0044 0.5242 0.2251 0.050 Uiso 1 1 calc R . .
H43B H 0.1556 0.6058 0.3050 0.050 Uiso 1 1 calc R . .
H43C H 0.1124 0.4656 0.3162 0.050 Uiso 1 1 calc R . .
O31 O -0.1766(3) 0.1726(3) 0.0685(3) 0.0222(5) Uani 1 1 d . . .
C31 C -0.2743(4) 0.2711(4) 0.0718(4) 0.0285(9) Uani 1 1 d . . .
H31 H -0.2154 0.3617 0.1091 0.034 Uiso 1 1 calc R . .
C32 C -0.3602(6) 0.2598(6) 0.1554(5) 0.0485(13) Uani 1 1 d . . .
H32A H -0.4159 0.1702 0.1210 0.073 Uiso 1 1 calc R . .
H32B H -0.4277 0.3264 0.1586 0.073 Uiso 1 1 calc R . .
H32C H -0.2932 0.2753 0.2414 0.073 Uiso 1 1 calc R . .
C33 C -0.3682(7) 0.2502(8) -0.0612(6) 0.067(2) Uani 1 1 d . . .
H33A H -0.3062 0.2503 -0.1133 0.100 Uiso 1 1 calc R . .
H33B H -0.4285 0.3223 -0.0611 0.100 Uiso 1 1 calc R . .
H33C H -0.4316 0.1644 -0.0964 0.100 Uiso 1 1 calc R . .
O21 O -0.0250(3) -0.0419(2) 0.0774(2) 0.0165(5) Uani 1 1 d . . .
C21 C -0.0780(4) -0.0700(4) 0.1721(4) 0.0206(7) Uani 1 1 d . . .
H21 H -0.0601 0.0150 0.2458 0.025 Uiso 1 1 calc R . .
C22 C 0.0079(5) -0.1693(4) 0.2194(4) 0.0263(8) Uani 1 1 d . . .
H22A H 0.1126 -0.1356 0.2515 0.039 Uiso 1 1 calc R . .
H22B H -0.0112 -0.2547 0.1494 0.039 Uiso 1 1 calc R . .
H22C H -0.0217 -0.1819 0.2880 0.039 Uiso 1 1 calc R . .
C23 C -0.2409(4) -0.1145(4) 0.1153(4) 0.0256(8) Uani 1 1 d . . .
H23A H -0.2610 -0.1995 0.0445 0.038 Uiso 1 1 calc R . .
H23B H -0.2890 -0.0469 0.0840 0.038 Uiso 1 1 calc R . .
H23C H -0.2785 -0.1260 0.1804 0.038 Uiso 1 1 calc R . .
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'
W W -0.8490 6.8722 '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
C2 W1 C5 92.10(15) . . ?
C2 W1 C4 91.62(15) . . ?
C5 W1 C4 88.00(16) . . ?
C2 W1 C6 87.88(15) . . ?
C5 W1 C6 91.99(16) . . ?
C4 W1 C6 179.50(14) . . ?
C2 W1 C3 91.55(16) . . ?
C5 W1 C3 176.20(15) . . ?
C4 W1 C3 90.85(16) . . ?
C6 W1 C3 89.19(16) . . ?
C2 W1 C11 176.58(14) . . ?
C5 W1 C11 90.37(15) . . ?
C4 W1 C11 90.82(14) . . ?
C6 W1 C11 89.68(14) . . ?
C3 W1 C11 86.02(15) . . ?
O3 C3 W1 178.8(4) . . ?
O41 Ti1 O31 102.87(13) . . ?
O41 Ti1 O21 101.20(11) . 2 ?
O31 Ti1 O21 111.92(12) . 2 ?
O41 Ti1 O11 90.37(13) . . ?
O31 Ti1 O11 109.71(13) . . ?
O21 Ti1 O11 132.71(12) 2 . ?
O41 Ti1 O21 165.84(12) . . ?
O31 Ti1 O21 91.20(11) . . ?
O21 Ti1 O21 74.43(11) 2 . ?
O11 Ti1 O21 83.33(11) . . ?
O41 Ti1 Ti1 138.75(10) . 2 ?
O31 Ti1 Ti1 103.75(9) . 2 ?
O21 Ti1 Ti1 39.14(7) 2 2 ?
O11 Ti1 Ti1 109.31(9) . 2 ?
O21 Ti1 Ti1 35.29(6) . 2 ?
O4 C4 W1 178.4(4) . . ?
O5 C5 W1 178.2(4) . . ?
O6 C6 W1 178.4(3) . . ?
O2 C2 W1 178.1(3) . . ?
C11 O11 Ti1 150.2(3) . . ?
O11 C11 C12 113.3(3) . . ?
O11 C11 W1 122.0(3) . . ?
C12 C11 W1 124.6(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C41 O41 Ti1 157.3(3) . . ?
O41 C41 C42 111.1(5) . . ?
O41 C41 C43 109.1(4) . . ?
C42 C41 C43 117.1(5) . . ?
O41 C41 H41 106.3 . . ?
C42 C41 H41 106.3 . . ?
C43 C41 H41 106.3 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C31 O31 Ti1 141.2(3) . . ?
O31 C31 C33 108.6(4) . . ?
O31 C31 C32 108.4(4) . . ?
C33 C31 C32 113.1(4) . . ?
O31 C31 H31 108.9 . . ?
C33 C31 H31 108.9 . . ?
C32 C31 H31 108.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C21 O21 Ti1 132.7(2) . 2 ?
C21 O21 Ti1 120.7(2) . . ?
Ti1 O21 Ti1 105.57(11) 2 . ?
O21 C21 C23 109.0(3) . . ?
O21 C21 C22 109.6(3) . . ?
C23 C21 C22 114.0(3) . . ?
O21 C21 H21 108.0 . . ?
C23 C21 H21 108.0 . . ?
C22 C21 H21 108.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
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
W1 C2 2.025(4) . ?
W1 C5 2.034(4) . ?
W1 C4 2.046(4) . ?
W1 C6 2.047(4) . ?
W1 C3 2.052(4) . ?
W1 C11 2.190(4) . ?
C3 O3 1.140(5) . ?
Ti1 O41 1.760(3) . ?
Ti1 O31 1.770(3) . ?
Ti1 O21 1.917(2) 2 ?
Ti1 O11 1.941(3) . ?
Ti1 O21 2.095(2) . ?
Ti1 Ti1 3.1971(12) 2 ?
O4 C4 1.142(5) . ?
C5 O5 1.142(5) . ?
C6 O6 1.144(5) . ?
C2 O2 1.145(5) . ?
O11 C11 1.273(5) . ?
C11 C12 1.518(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O41 C41 1.427(5) . ?
C41 C42 1.429(8) . ?
C41 C43 1.509(6) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O31 C31 1.435(4) . ?
C31 C33 1.493(7) . ?
C31 C32 1.496(6) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O21 C21 1.465(4) . ?
O21 Ti1 1.917(2) 2 ?
C21 C23 1.510(5) . ?
C21 C22 1.510(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 W1 C3 O3 160(19) . . . . ?
C5 W1 C3 O3 -36(20) . . . . ?
C4 W1 C3 O3 -109(19) . . . . ?
C6 W1 C3 O3 72(19) . . . . ?
C11 W1 C3 O3 -18(19) . . . . ?
C2 W1 C4 O4 -49(13) . . . . ?
C5 W1 C4 O4 43(13) . . . . ?
C6 W1 C4 O4 -45(25) . . . . ?
C3 W1 C4 O4 -140(13) . . . . ?
C11 W1 C4 O4 134(13) . . . . ?
C2 W1 C5 O5 88(12) . . . . ?
C4 W1 C5 O5 -4(12) . . . . ?
C6 W1 C5 O5 176(100) . . . . ?
C3 W1 C5 O5 -76(12) . . . . ?
C11 W1 C5 O5 -94(12) . . . . ?
C2 W1 C6 O6 -41(13) . . . . ?
C5 W1 C6 O6 -133(13) . . . . ?
C4 W1 C6 O6 -44(25) . . . . ?
C3 W1 C6 O6 51(13) . . . . ?
C11 W1 C6 O6 137(13) . . . . ?
C5 W1 C2 O2 113(10) . . . . ?
C4 W1 C2 O2 -159(10) . . . . ?
C6 W1 C2 O2 21(10) . . . . ?
C3 W1 C2 O2 -68(10) . . . . ?
C11 W1 C2 O2 -23(12) . . . . ?
O41 Ti1 O11 C11 -90.4(5) . . . . ?
O31 Ti1 O11 C11 165.8(5) . . . . ?
O21 Ti1 O11 C11 15.3(6) 2 . . . ?
O21 Ti1 O11 C11 76.9(5) . . . . ?
Ti1 Ti1 O11 C11 52.6(5) 2 . . . ?
Ti1 O11 C11 C12 0.2(7) . . . . ?
Ti1 O11 C11 W1 178.0(3) . . . . ?
C2 W1 C11 O11 -40(2) . . . . ?
C5 W1 C11 O11 -176.4(3) . . . . ?
C4 W1 C11 O11 95.6(3) . . . . ?
C6 W1 C11 O11 -84.4(3) . . . . ?
C3 W1 C11 O11 4.8(3) . . . . ?
C2 W1 C11 C12 137(2) . . . . ?
C5 W1 C11 C12 1.2(3) . . . . ?
C4 W1 C11 C12 -86.8(3) . . . . ?
C6 W1 C11 C12 93.2(3) . . . . ?
C3 W1 C11 C12 -177.6(3) . . . . ?
O31 Ti1 O41 C41 93.2(8) . . . . ?
O21 Ti1 O41 C41 -151.0(8) 2 . . . ?
O11 Ti1 O41 C41 -17.2(8) . . . . ?
O21 Ti1 O41 C41 -80.5(9) . . . . ?
Ti1 Ti1 O41 C41 -137.7(8) 2 . . . ?
Ti1 O41 C41 C42 87.1(8) . . . . ?
Ti1 O41 C41 C43 -43.4(11) . . . . ?
O41 Ti1 O31 C31 -4.8(4) . . . . ?
O21 Ti1 O31 C31 -112.7(4) 2 . . . ?
O11 Ti1 O31 C31 90.3(4) . . . . ?
O21 Ti1 O31 C31 173.6(4) . . . . ?
Ti1 Ti1 O31 C31 -153.0(4) 2 . . . ?
Ti1 O31 C31 C33 102.7(5) . . . . ?
Ti1 O31 C31 C32 -134.1(4) . . . . ?
O41 Ti1 O21 C21 116.6(5) . . . . ?
O31 Ti1 O21 C21 -57.2(2) . . . . ?
O21 Ti1 O21 C21 -169.6(3) 2 . . . ?
O11 Ti1 O21 C21 52.5(2) . . . . ?
Ti1 Ti1 O21 C21 -169.6(3) 2 . . . ?
O41 Ti1 O21 Ti1 -73.7(5) . . . 2 ?
O31 Ti1 O21 Ti1 112.44(13) . . . 2 ?
O21 Ti1 O21 Ti1 0.0 2 . . 2 ?
O11 Ti1 O21 Ti1 -137.86(14) . . . 2 ?
Ti1 O21 C21 C23 -68.4(4) 2 . . . ?
Ti1 O21 C21 C23 98.0(3) . . . . ?
Ti1 O21 C21 C22 57.1(4) 2 . . . ?
Ti1 O21 C21 C22 -136.6(3) . . . . ?
