#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:15:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180130 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/28/7102890.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_7102890
loop_
_publ_author_name
'Rohe, Markus'
'Merz, Klaus'
_publ_section_title
;
 Active peroxo titanium complexes: syntheses, characterization and
 their potential in the photooxidation of 2-propanol.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              862
_journal_page_last               864
_journal_paper_doi               10.1039/b716199a
_journal_year                    2008
_chemical_formula_sum            'C18 H23 Li2 O25 Ti'
_chemical_formula_weight         701.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 115.474(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.731(7)
_cell_length_b                   14.940(9)
_cell_length_c                   14.911(9)
_cell_measurement_temperature    213(2)
_cell_volume                     2762(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_diffrn_measurement_method       'omega scan'
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15219
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.9592
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0219(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0521
_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)+(0.0755P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                3126
_reflns_number_total             4836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716199a.txt
_cod_data_source_block           070621t
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7102890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ti1 Ti 0.19505(5) 0.23528(4) 0.17269(5) 0.0166(2) Uani 1 1 d . . .
Li1 Li 0.0992(5) 0.3014(4) 0.3345(5) 0.0298(16) Uani 1 1 d . . .
Li2 Li 0.4954(5) 0.2016(5) 0.5877(5) 0.0321(17) Uani 1 1 d . . .
O1 O -0.1918(2) 0.17473(18) 0.2480(2) 0.0333(7) Uani 1 1 d . . .
C1 C -0.1146(3) 0.2093(2) 0.2416(3) 0.0187(8) Uani 1 1 d . . .
O2 O -0.0556(2) 0.26976(17) 0.3053(2) 0.0246(6) Uani 1 1 d . . .
C2 C -0.0824(3) 0.1831(2) 0.1607(3) 0.0211(9) Uani 1 1 d . . .
H2A H -0.1464 0.1598 0.1046 0.025 Uiso 1 1 calc R . .
H2B H -0.0301 0.1340 0.1854 0.025 Uiso 1 1 calc R . .
O3 O 0.07256(19) 0.20686(16) 0.04054(19) 0.0213(6) Uani 1 1 d . . .
C3 C -0.0332(3) 0.2573(2) 0.1218(3) 0.0178(8) Uani 1 1 d . . .
O4 O -0.1062(2) 0.21103(17) -0.05051(19) 0.0220(6) Uani 1 1 d . . .
C4 C -0.0249(3) 0.2228(2) 0.0279(3) 0.0191(8) Uani 1 1 d . . .
O5 O -0.0237(3) 0.39779(18) -0.0053(3) 0.0477(9) Uani 1 1 d . . .
C5 C -0.0578(3) 0.4128(2) 0.0552(3) 0.0243(9) Uani 1 1 d . . .
O6 O -0.0589(3) 0.49269(19) 0.0898(3) 0.0448(9) Uani 1 1 d . . .
H6 H -0.025(4) 0.525(3) 0.063(4) 0.063(17) Uiso 1 1 d . . .
C6 C -0.1027(3) 0.3418(2) 0.0970(3) 0.0211(9) Uani 1 1 d . . .
H6A H -0.1762 0.3271 0.0487 0.025 Uiso 1 1 calc R . .
H6B H -0.1062 0.3642 0.1573 0.025 Uiso 1 1 calc R . .
O7 O 0.07363(19) 0.27692(15) 0.19217(19) 0.0186(6) Uani 1 1 d . . .
C7 C 0.5029(3) 0.3372(3) 0.2995(3) 0.0247(9) Uani 1 1 d . . .
O8 O 0.5647(3) 0.2892(2) 0.3767(2) 0.0390(8) Uani 1 1 d . . .
H8 H 0.599(6) 0.248(4) 0.363(6) 0.11(3) Uiso 1 1 d . . .
C8 C 0.4387(3) 0.4072(3) 0.3211(3) 0.0245(9) Uani 1 1 d . . .
H8A H 0.4598 0.4664 0.3071 0.029 Uiso 1 1 calc R . .
H8B H 0.4546 0.4051 0.3917 0.029 Uiso 1 1 calc R . .
O9 O 0.4981(2) 0.3241(2) 0.2174(2) 0.0356(7) Uani 1 1 d . . .
C9 C 0.3175(3) 0.3938(2) 0.2586(3) 0.0183(8) Uani 1 1 d . . .
O10 O 0.3086(2) 0.47001(17) 0.1132(2) 0.0277(7) Uani 1 1 d . . .
C10 C 0.2470(3) 0.4644(2) 0.2792(3) 0.0231(9) Uani 1 1 d . . .
H10A H 0.2726 0.5245 0.2737 0.028 Uiso 1 1 calc R . .
H10B H 0.1722 0.4589 0.2290 0.028 Uiso 1 1 calc R . .
O11 O 0.2282(2) 0.33694(16) 0.09564(19) 0.0214(6) Uani 1 1 d . . .
C11 C 0.2507(3) 0.4530(2) 0.3802(3) 0.0198(8) Uani 1 1 d . . .
O12 O 0.3255(2) 0.50169(18) 0.4493(2) 0.0324(7) Uani 1 1 d . . .
C12 C 0.2856(3) 0.4018(2) 0.1478(3) 0.0214(9) Uani 1 1 d . . .
O13 O 0.1909(2) 0.40246(17) 0.3969(2) 0.0251(6) Uani 1 1 d . . .
C13 C 0.1210(3) -0.0191(2) 0.1238(3) 0.0234(9) Uani 1 1 d . . .
O14 O 0.28907(19) 0.30598(15) 0.27523(19) 0.0189(6) Uani 1 1 d . . .
C14 C 0.2203(3) -0.0275(2) 0.2197(3) 0.0246(9) Uani 1 1 d . . .
H14A H 0.2651 -0.0767 0.2152 0.030 Uiso 1 1 calc R . .
H14B H 0.2001 -0.0408 0.2738 0.030 Uiso 1 1 calc R . .
O15 O 0.1276(2) 0.00092(18) 0.0471(2) 0.0330(7) Uani 1 1 d . . .
C15 C 0.2842(3) 0.0602(2) 0.2416(3) 0.0196(8) Uani 1 1 d . . .
O16 O 0.0297(2) -0.03347(19) 0.1292(2) 0.0332(7) Uani 1 1 d . . .
H16 H -0.028(4) -0.029(3) 0.063(4) 0.071(18) Uiso 1 1 d . . .
C16 C 0.3913(3) 0.0578(3) 0.3355(3) 0.0258(9) Uani 1 1 d . . .
H16A H 0.4300 0.0034 0.3330 0.031 Uiso 1 1 calc R . .
H16B H 0.4348 0.1089 0.3330 0.031 Uiso 1 1 calc R . .
O17 O 0.3030(2) 0.01901(19) 0.4377(2) 0.0316(7) Uani 1 1 d . . .
C17 C 0.3862(3) 0.0597(2) 0.4336(3) 0.0244(9) Uani 1 1 d . . .
O18 O 0.4555(2) 0.09631(18) 0.5056(2) 0.0326(7) Uani 1 1 d . . .
C18 C 0.3145(3) 0.0840(2) 0.1575(3) 0.0219(9) Uani 1 1 d . . .
O19 O 0.3662(2) 0.03081(17) 0.1317(2) 0.0278(7) Uani 1 1 d . . .
O20 O 0.28692(19) 0.16344(16) 0.12262(19) 0.0200(6) Uani 1 1 d . . .
O21 O 0.21725(19) 0.13088(15) 0.24705(19) 0.0178(6) Uani 1 1 d . . .
O22 O 0.1606(3) 0.1928(2) 0.3946(3) 0.0441(10) Uani 1 1 d . . .
H22A H 0.177(3) 0.160(3) 0.367(3) 0.020(13) Uiso 1 1 d . . .
H22B H 0.186(6) 0.174(4) 0.449(5) 0.10(3) Uiso 1 1 d . . .
O23 O 0.3889(3) 0.2828(2) 0.5056(3) 0.0374(8) Uani 1 1 d . . .
H23B H 0.342(4) 0.307(3) 0.534(4) 0.066(17) Uiso 1 1 d . . .
H23A H 0.342(5) 0.277(4) 0.445(5) 0.08(2) Uiso 1 1 d . . .
O24 O 0.6270(3) 0.2497(3) 0.5870(3) 0.0538(10) Uani 1 1 d . . .
H24A H 0.667(5) 0.287(4) 0.634(5) 0.062(19) Uiso 1 1 d . . .
H24B H 0.590(7) 0.278(5) 0.518(7) 0.14(3) Uiso 1 1 d . . .
O25 O 0.6767(3) 0.1602(2) 0.3511(3) 0.0512(11) Uani 1 1 d . . .
H25A H 0.727(5) 0.175(4) 0.346(5) 0.09(3) Uiso 1 1 d . . .
H25B H 0.665(7) 0.097(6) 0.355(6) 0.14(3) 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'
Li Li -0.0003 0.0001 '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
O14 Ti1 O21 96.25(12) . . ?
O14 Ti1 O7 91.88(11) . . ?
O21 Ti1 O7 96.44(10) . . ?
O14 Ti1 O3 157.37(11) . . ?
O21 Ti1 O3 105.10(11) . . ?
O7 Ti1 O3 78.54(11) . . ?
O14 Ti1 O20 106.44(11) . . ?
O21 Ti1 O20 78.89(11) . . ?
O7 Ti1 O20 161.43(11) . . ?
O3 Ti1 O20 85.30(11) . . ?
O14 Ti1 O11 78.33(11) . . ?
O21 Ti1 O11 157.93(10) . . ?
O7 Ti1 O11 105.05(11) . . ?
O3 Ti1 O11 84.38(11) . . ?
O20 Ti1 O11 82.16(10) . . ?
O14 Ti1 Li1 65.66(14) . . ?
O21 Ti1 Li1 80.36(14) . . ?
O7 Ti1 Li1 32.77(14) . . ?
O3 Ti1 Li1 110.21(14) . . ?
O20 Ti1 Li1 156.79(14) . . ?
O11 Ti1 Li1 115.55(14) . . ?
O22 Li1 O13 112.5(4) . . ?
O22 Li1 O7 100.6(3) . . ?
O13 Li1 O7 115.4(4) . . ?
O22 Li1 O2 96.6(3) . . ?
O13 Li1 O2 133.6(4) . . ?
O7 Li1 O2 92.3(3) . . ?
O22 Li1 Ti1 81.6(3) . . ?
O13 Li1 Ti1 101.6(3) . . ?
O7 Li1 Ti1 30.71(13) . . ?
O2 Li1 Ti1 118.3(3) . . ?
O23 Li2 O18 100.6(4) . . ?
O23 Li2 O24 102.8(4) . . ?
O18 Li2 O24 107.9(4) . . ?
O23 Li2 O9 116.6(4) . 4_566 ?
O18 Li2 O9 110.4(4) . 4_566 ?
O24 Li2 O9 117.0(4) . 4_566 ?
O1 C1 O2 121.5(3) . . ?
O1 C1 C2 121.2(3) . . ?
O2 C1 C2 117.3(3) . . ?
C1 O2 Li1 125.4(3) . . ?
C1 C2 C3 116.3(3) . . ?
C4 O3 Ti1 118.8(2) . . ?
O7 C3 C6 110.4(3) . . ?
O7 C3 C2 110.6(3) . . ?
C6 C3 C2 110.9(3) . . ?
O7 C3 C4 106.5(3) . . ?
C6 C3 C4 109.9(3) . . ?
C2 C3 C4 108.5(3) . . ?
O4 C4 O3 124.8(4) . . ?
O4 C4 C3 121.2(3) . . ?
O3 C4 C3 114.0(3) . . ?
O5 C5 O6 122.9(4) . . ?
O5 C5 C6 123.0(4) . . ?
O6 C5 C6 114.1(4) . . ?
C5 C6 C3 111.1(3) . . ?
C3 O7 Ti1 120.7(2) . . ?
C3 O7 Li1 118.0(3) . . ?
Ti1 O7 Li1 116.5(2) . . ?
O9 C7 O8 122.1(4) . . ?
O9 C7 C8 123.5(4) . . ?
O8 C7 C8 114.4(4) . . ?
C7 C8 C9 111.5(3) . . ?
C7 O9 Li2 177.3(4) . 4_565 ?
O14 C9 C12 106.8(3) . . ?
O14 C9 C8 108.8(3) . . ?
C12 C9 C8 112.4(3) . . ?
O14 C9 C10 110.6(3) . . ?
C12 C9 C10 104.5(3) . . ?
C8 C9 C10 113.5(3) . . ?
C11 C10 C9 111.7(3) . . ?
C12 O11 Ti1 116.3(2) . . ?
O13 C11 O12 123.3(4) . . ?
O13 C11 C10 122.9(3) . . ?
O12 C11 C10 113.7(3) . . ?
O10 C12 O11 124.7(4) . . ?
O10 C12 C9 120.6(3) . . ?
O11 C12 C9 114.5(3) . . ?
C11 O13 Li1 138.1(3) . . ?
O15 C13 O16 123.8(4) . . ?
O15 C13 C14 120.6(4) . . ?
O16 C13 C14 115.6(4) . . ?
C9 O14 Ti1 122.0(2) . . ?
C13 C14 C15 109.6(3) . . ?
O21 C15 C18 106.6(3) . . ?
O21 C15 C14 108.8(3) . . ?
C18 C15 C14 111.0(3) . . ?
O21 C15 C16 110.7(3) . . ?
C18 C15 C16 105.2(3) . . ?
C14 C15 C16 114.3(3) . . ?
C17 C16 C15 117.5(3) . . ?
O18 C17 O17 122.2(4) . . ?
O18 C17 C16 121.6(4) . . ?
O17 C17 C16 116.3(4) . . ?
C17 O18 Li2 146.1(3) . . ?
O19 C18 O20 125.3(4) . . ?
O19 C18 C15 120.3(3) . . ?
O20 C18 C15 114.3(3) . . ?
C18 O20 Ti1 117.4(2) . . ?
C15 O21 Ti1 122.1(2) . . ?
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 O14 1.850(3) . ?
Ti1 O21 1.861(3) . ?
Ti1 O7 1.915(3) . ?
Ti1 O3 2.010(3) . ?
Ti1 O20 2.028(3) . ?
Ti1 O11 2.070(3) . ?
Ti1 Li1 3.356(7) . ?
Li1 O22 1.869(8) . ?
Li1 O13 1.930(7) . ?
Li1 O7 2.030(8) . ?
Li1 O2 2.033(7) . ?
Li2 O23 1.889(8) . ?
Li2 O18 1.923(8) . ?
Li2 O24 1.949(8) . ?
Li2 O9 1.955(8) 4_566 ?
O1 C1 1.220(4) . ?
C1 O2 1.308(4) . ?
C1 C2 1.505(5) . ?
C2 C3 1.536(5) . ?
O3 C4 1.291(4) . ?
C3 O7 1.419(4) . ?
C3 C6 1.528(5) . ?
C3 C4 1.541(5) . ?
O4 C4 1.234(5) . ?
O5 C5 1.203(5) . ?
C5 O6 1.303(5) . ?
C5 C6 1.493(5) . ?
C7 O9 1.213(5) . ?
C7 O8 1.311(5) . ?
C7 C8 1.489(5) . ?
C8 C9 1.532(5) . ?
O9 Li2 1.955(8) 4_565 ?
C9 O14 1.421(4) . ?
C9 C12 1.520(5) . ?
C9 C10 1.548(5) . ?
O10 C12 1.243(4) . ?
C10 C11 1.495(5) . ?
O11 C12 1.280(4) . ?
C11 O13 1.217(4) . ?
C11 O12 1.318(5) . ?
C13 O15 1.224(5) . ?
C13 O16 1.307(5) . ?
C13 C14 1.498(6) . ?
C14 C15 1.531(5) . ?
C15 O21 1.425(4) . ?
C15 C18 1.523(5) . ?
C15 C16 1.534(5) . ?
C16 C17 1.496(5) . ?
O17 C17 1.319(5) . ?
C17 O18 1.216(5) . ?
C18 O19 1.233(4) . ?
C18 O20 1.285(4) . ?
