#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/48/1514873.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_1514873
loop_
_publ_author_name
'Seisenbaeva, Gulaim A.'
'Daniel, Geoffrey'
'Nedelec, Jean-Marie'
'Kessler, Vadim G.'
_publ_section_title
;
 Solution equilibrium behind the room-temperature synthesis of
 nanocrystalline titanium dioxide.
;
_journal_issue                   8
_journal_name_full               Nanoscale
_journal_page_first              3330
_journal_page_last               3336
_journal_paper_doi               10.1039/c3nr34068f
_journal_volume                  5
_journal_year                    2013
_chemical_formula_sum            'C9 H26 N2 O12 Ti'
_chemical_formula_weight         402.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           143
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.3040(15)
_cell_length_b                   15.3040(15)
_cell_length_c                   6.6658(13)
_cell_measurement_reflns_used    5298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.66
_cell_volume                     1352.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Apex-II CCD'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9275
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.8518
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.120
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      5.959
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0219
_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)+(0.0286P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                2640
_reflns_number_total             2772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nr34068f.txt
_cod_data_source_block           tilac1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1352.0(3)
_cod_original_sg_symbol_H-M      P3
_cod_database_code               1514873
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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 0.3333 0.6667 0.8779(5) 0.0258(10) Uani 1 3 d S
Ti2 Ti 0.0000 1.0000 -0.1171(5) 0.0257(10) Uani 1 3 d S
Ti3 Ti 0.6667 0.3333 0.6998(5) 0.0241(9) Uani 1 3 d S
O2 O -0.1002(7) 0.8939(7) 0.0805(14) 0.032(2) Uani 1 1 d .
O1 O 0.4235(7) 0.7756(7) 0.6798(15) 0.038(2) Uani 1 1 d .
O3 O 0.6385(7) 0.2152(6) 0.8348(13) 0.033(2) Uani 1 1 d .
O8 O -0.2027(8) 0.7286(7) 0.1248(15) 0.042(2) Uani 1 1 d .
C1 C 0.5464(10) 0.1341(11) 0.540(2) 0.033(3) Uani 1 1 d .
O7 O 0.5006(9) 0.0651(8) 0.4234(16) 0.060(3) Uani 1 1 d .
C8 C 0.5411(10) 0.8162(10) 0.941(2) 0.032(3) Uani 1 1 d .
H8A H 0.5552 0.8738 1.0270 0.039 Uiso 1 1 calc R
C2 C 0.5774(10) 0.1188(9) 0.749(2) 0.032(3) Uani 1 1 d .
H2A H 0.6179 0.0859 0.7345 0.039 Uiso 1 1 calc R
O9 O 0.5772(9) 0.9043(9) 0.6300(17) 0.059(3) Uani 1 1 d .
C7 C 0.5153(10) 0.8357(10) 0.735(2) 0.033(3) Uani 1 1 d .
C9 C 0.6328(11) 0.8039(14) 0.939(3) 0.053(4) Uani 1 1 d .
H9A H 0.6475 0.7923 1.0733 0.079 Uiso 1 1 calc R
H9B H 0.6894 0.8640 0.8868 0.079 Uiso 1 1 calc R
H9C H 0.6200 0.7475 0.8560 0.079 Uiso 1 1 calc R
C4 C -0.1459(9) 0.8021(10) 0.021(2) 0.028(3) Uani 1 1 d .
O6 O 0.5732(7) 0.2266(7) 0.5006(13) 0.035(2) Uani 1 1 d .
O5 O -0.0418(7) 0.8810(6) -0.2594(13) 0.032(2) Uani 1 1 d .
O4 O 0.4552(6) 0.7288(7) 1.0186(13) 0.034(2) Uani 1 1 d .
O10 O 0.0444(10) 0.8594(9) -0.6084(18) 0.049(3) Uani 1 1 d D
O11 O -0.3125(10) 0.7507(10) 0.4484(19) 0.057(3) Uani 1 1 d D
O12 O 0.6735(10) 1.0125(9) 0.2872(18) 0.051(3) Uani 1 1 d D
N1 N 0.3687(10) 0.8568(10) 0.3535(18) 0.044(3) Uani 1 1 d D
H1A H 0.341(2) 0.816(3) 0.201(10) 0.09(7) Uiso 1 1 d RD
H1B H 0.3722(11) 0.818(3) 0.429(5) 0.07(6) Uiso 1 1 d RD
H1C H 0.319(3) 0.8736(14) 0.392(3) 0.08(7) Uiso 1 1 d RD
H1D H 0.440(5) 0.936(5) 0.340(2) 0.10(7) Uiso 1 1 d RD
N2 N 0.4623(10) 0.2496(10) 0.1826(19) 0.036(3) Uani 1 1 d D
C3 C 0.4865(12) 0.0525(12) 0.877(2) 0.051(4) Uani 1 1 d .
H3A H 0.5084 0.0440 1.0064 0.076 Uiso 1 1 calc R
H3B H 0.4476 -0.0121 0.8134 0.076 Uiso 1 1 calc R
H3C H 0.4457 0.0836 0.8912 0.076 Uiso 1 1 calc R
C6 C -0.1132(15) 0.7014(11) -0.238(3) 0.060(5) Uani 1 1 d .
H6A H -0.1023 0.6979 -0.3787 0.090 Uiso 1 1 calc R
H6B H -0.1725 0.6406 -0.1965 0.090 Uiso 1 1 calc R
H6C H -0.0559 0.7089 -0.1641 0.090 Uiso 1 1 calc R
C5 C -0.1269(10) 0.7902(10) -0.198(2) 0.034(3) Uani 1 1 d .
H5A H -0.1852 0.7813 -0.2754 0.041 Uiso 1 1 calc R
H2AA H 0.499(10) 0.283(10) 0.065(18) 0.04(4) Uiso 1 1 d D
H2BA H 0.429(12) 0.286(12) 0.22(3) 0.07(6) Uiso 1 1 d D
H11A H -0.280(16) 0.815(9) 0.46(3) 0.09(8) Uiso 1 1 d D
H2CA H 0.501(12) 0.247(14) 0.29(2) 0.07(6) Uiso 1 1 d D
H2DA H 0.407(11) 0.185(9) 0.14(3) 0.07(6) Uiso 1 1 d D
H10A H 0.050(15) 0.897(13) -0.70(3) 0.08(7) Uiso 1 1 d D
H12A H 0.724(11) 1.002(14) 0.31(3) 0.07(6) Uiso 1 1 d D
H10B H 0.019(13) 0.874(13) -0.51(2) 0.06(6) Uiso 1 1 d D
H11B H -0.282(14) 0.737(16) 0.35(2) 0.08(7) Uiso 1 1 d D
H12B H 0.633(14) 0.980(14) 0.38(2) 0.07(7) Uiso 1 1 d 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'
N N 0.0061 0.0033 '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
O4 Ti1 O4 97.0(4) 2_665 .
O4 Ti1 O4 97.0(4) 2_665 3_565
O4 Ti1 O4 97.0(4) . 3_565
O4 Ti1 O1 79.2(4) 2_665 2_665
O4 Ti1 O1 159.8(4) . 2_665
O4 Ti1 O1 103.2(4) 3_565 2_665
O4 Ti1 O1 103.2(4) 2_665 .
O4 Ti1 O1 79.2(4) . .
O4 Ti1 O1 159.8(4) 3_565 .
O1 Ti1 O1 82.3(4) 2_665 .
O4 Ti1 O1 159.8(4) 2_665 3_565
O4 Ti1 O1 103.2(4) . 3_565
O4 Ti1 O1 79.2(4) 3_565 3_565
O1 Ti1 O1 82.3(4) 2_665 3_565
O1 Ti1 O1 82.3(4) . 3_565
O5 Ti2 O5 96.3(4) . 3_465
O5 Ti2 O5 96.3(4) . 2_675
O5 Ti2 O5 96.3(4) 3_465 2_675
O5 Ti2 O2 159.1(4) . 3_465
O5 Ti2 O2 78.3(3) 3_465 3_465
O5 Ti2 O2 104.3(4) 2_675 3_465
O5 Ti2 O2 104.3(4) . 2_675
O5 Ti2 O2 159.1(4) 3_465 2_675
O5 Ti2 O2 78.3(4) 2_675 2_675
O2 Ti2 O2 83.4(4) 3_465 2_675
O5 Ti2 O2 78.3(3) . .
O5 Ti2 O2 104.3(4) 3_465 .
O5 Ti2 O2 159.1(4) 2_675 .
O2 Ti2 O2 83.4(4) 3_465 .
O2 Ti2 O2 83.4(4) 2_675 .
O3 Ti3 O3 98.7(4) . 2_655
O3 Ti3 O3 98.7(4) . 3_665
O3 Ti3 O3 98.7(4) 2_655 3_665
O3 Ti3 O6 101.3(4) . 2_655
O3 Ti3 O6 78.9(4) 2_655 2_655
O3 Ti3 O6 159.9(4) 3_665 2_655
O3 Ti3 O6 78.9(4) . .
O3 Ti3 O6 159.9(4) 2_655 .
O3 Ti3 O6 101.3(4) 3_665 .
O6 Ti3 O6 82.0(4) 2_655 .
O3 Ti3 O6 159.9(4) . 3_665
O3 Ti3 O6 101.3(4) 2_655 3_665
O3 Ti3 O6 78.9(4) 3_665 3_665
O6 Ti3 O6 82.0(4) 2_655 3_665
O6 Ti3 O6 82.0(4) . 3_665
C4 O2 Ti2 116.8(8) . .
C7 O1 Ti1 116.8(9) . .
C2 O3 Ti3 121.8(8) . .
O7 C1 O6 123.5(13) . .
O7 C1 C2 122.7(13) . .
O6 C1 C2 113.8(11) . .
O4 C8 C7 107.9(10) . .
O4 C8 C9 111.5(11) . .
C7 C8 C9 111.8(12) . .
O4 C8 H8A 108.5 . .
C7 C8 H8A 108.5 . .
C9 C8 H8A 108.5 . .
O3 C2 C3 112.2(11) . .
O3 C2 C1 107.7(10) . .
C3 C2 C1 111.4(12) . .
O3 C2 H2A 108.5 . .
C3 C2 H2A 108.5 . .
C1 C2 H2A 108.5 . .
O9 C7 O1 123.3(13) . .
O9 C7 C8 121.8(13) . .
O1 C7 C8 114.9(11) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O8 C4 O2 125.1(12) . .
O8 C4 C5 121.4(12) . .
O2 C4 C5 113.5(11) . .
C1 O6 Ti3 117.2(8) . .
C5 O5 Ti2 120.8(8) . .
C8 O4 Ti1 121.0(8) . .
H10A O10 H10B 106(10) . .
H11A O11 H11B 105(10) . .
H12A O12 H12B 104(10) . .
H1A N1 H1B 107.1 . .
H1A N1 H1C 104.3 . .
H1B N1 H1C 113.4 . .
H1A N1 H1D 113.1 . .
H1B N1 H1D 116.5 . .
H1C N1 H1D 101.8 . .
H2AA N2 H2BA 104(10) . .
H2AA N2 H2CA 117(10) . .
H2BA N2 H2CA 110(10) . .
H2AA N2 H2DA 107(10) . .
H2BA N2 H2DA 102(10) . .
H2CA N2 H2DA 115(10) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
O5 C5 C6 111.2(11) . .
O5 C5 C4 107.5(11) . .
C6 C5 C4 113.8(12) . .
O5 C5 H5A 108.1 . .
C6 C5 H5A 108.1 . .
C4 C5 H5A 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O4 1.868(9) 2_665
Ti1 O4 1.868(9) .
Ti1 O4 1.868(9) 3_565
Ti1 O1 2.032(10) 2_665
Ti1 O1 2.032(10) .
Ti1 O1 2.032(10) 3_565
Ti2 O5 1.860(9) .
Ti2 O5 1.860(9) 3_465
Ti2 O5 1.860(9) 2_675
Ti2 O2 2.057(9) 3_465
Ti2 O2 2.057(9) 2_675
Ti2 O2 2.057(9) .
Ti3 O3 1.866(8) .
Ti3 O3 1.866(8) 2_655
Ti3 O3 1.866(8) 3_665
Ti3 O6 2.035(9) 2_655
Ti3 O6 2.035(9) .
Ti3 O6 2.035(9) 3_665
O2 C4 1.280(16) .
O1 C7 1.289(17) .
O3 C2 1.414(15) .
O8 C4 1.234(16) .
C1 O7 1.215(17) .
C1 O6 1.289(17) .
C1 C2 1.523(19) .
C8 O4 1.424(16) .
C8 C7 1.50(2) .
C8 C9 1.51(2) .
C8 H8A 0.9800 .
C2 C3 1.51(2) .
C2 H2A 0.9800 .
O9 C7 1.223(16) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C4 C5 1.514(19) .
O5 C5 1.410(16) .
O10 H10A 0.79(13) .
O10 H10B 0.84(10) .
O11 H11A 0.86(11) .
O11 H11B 0.87(11) .
O12 H12A 0.88(11) .
O12 H12B 0.86(11) .
N1 H1A 1.1538 .
N1 H1B 0.8053 .
N1 H1C 0.9461 .
N1 H1D 1.1613 .
N2 H2AA 0.95(9) .
N2 H2BA 0.96(10) .
N2 H2CA 0.96(10) .
N2 H2DA 0.97(10) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C6 C5 1.50(2) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C5 H5A 0.9800 .
