#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:04:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180371 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/40/7204072.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_7204072
loop_
_publ_author_name
'Jones, Anthony C.'
'Williams, Paul A.'
'Bickley, Jamie F.'
'Steiner, Alexander'
'Davies, Hywel O.'
'Leedham, Timothy J.'
'Awaluddin, Amir'
'Pemble, Martyn E.'
'Critchlow, Gary W.'
_publ_section_title
;
 Synthesis and crystal structures of two new titanium alkoxy--diolate
 complexes. Potential precursors for oxide ceramics
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1428
_journal_paper_doi               10.1039/b100411p
_journal_volume                  11
_journal_year                    2001
_chemical_formula_sum            'C28 H64 N4 O8 Ti2'
_chemical_formula_weight         680.76
_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                110.358(17)
_cell_angle_beta                 107.365(18)
_cell_angle_gamma                99.353(18)
_cell_formula_units_Z            1
_cell_length_a                   9.3358(14)
_cell_length_b                   10.0168(16)
_cell_length_c                   11.4403(18)
_cell_measurement_temperature    213(2)
_cell_volume                     913.9(3)
_computing_data_collection       'IPDS (STOE, 1997)'
_computing_data_reduction        'X-RED (STOE, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Image plate'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5798
_diffrn_reflns_theta_full        24.25
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                2219
_reflns_number_total             2692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100411p.txt
_cod_data_source_block           tony33
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0549P)^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^)+(0.0549P)^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        913.9(2)
_cod_database_code               7204072
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3654(3) 0.1933(2) 0.6181(2) 0.0303(5) Uani 1 d . . .
C2 C 0.2886(3) 0.0327(3) 0.5118(3) 0.0471(6) Uani 1 d . . .
H2A H 0.2243 -0.0226 0.5423 0.057 Uiso 1 calc R . .
H2B H 0.3695 -0.0132 0.4977 0.057 Uiso 1 calc R . .
H2C H 0.2231 0.0318 0.4276 0.057 Uiso 1 calc R . .
C3 C 0.4722(3) 0.1965(3) 0.7495(3) 0.0471(6) Uani 1 d . . .
H3A H 0.4104 0.1426 0.7826 0.056 Uiso 1 calc R . .
H3B H 0.5223 0.2991 0.8160 0.056 Uiso 1 calc R . .
H3C H 0.5521 0.1500 0.7336 0.056 Uiso 1 calc R . .
C4 C 0.2471(3) 0.2834(2) 0.6392(2) 0.0319(5) Uani 1 d . . .
C5 C 0.1724(3) 0.2590(3) 0.7345(3) 0.0492(7) Uani 1 d . . .
H5A H 0.1081 0.1561 0.6951 0.059 Uiso 1 calc R . .
H5B H 0.1072 0.3244 0.7489 0.059 Uiso 1 calc R . .
H5C H 0.2542 0.2810 0.8202 0.059 Uiso 1 calc R . .
C6 C 0.1187(3) 0.2534(3) 0.5059(3) 0.0440(6) Uani 1 d . . .
H6A H 0.0531 0.1506 0.4643 0.053 Uiso 1 calc R . .
H6B H 0.1665 0.2708 0.4459 0.053 Uiso 1 calc R . .
H6C H 0.0548 0.3196 0.5225 0.053 Uiso 1 calc R . .
C7 C 0.8310(3) 0.5172(3) 0.8276(2) 0.0390(6) Uani 1 d . . .
H7A H 0.8215 0.4154 0.7684 0.047 Uiso 1 calc R . .
H7B H 0.8542 0.5234 0.9191 0.047 Uiso 1 calc R . .
C8 C 0.9644(3) 0.6254(3) 0.8283(2) 0.0407(6) Uani 1 d . . .
H8A H 1.0594 0.5942 0.8512 0.049 Uiso 1 calc R . .
H8B H 0.9388 0.6210 0.7372 0.049 Uiso 1 calc R . .
C9 C 1.1041(3) 0.8787(3) 0.8981(3) 0.0512(7) Uani 1 d . . .
H9A H 1.1254 0.9807 0.9615 0.061 Uiso 1 calc R . .
H9B H 1.0560 0.8692 0.8066 0.061 Uiso 1 calc R . .
H9C H 1.2017 0.8533 0.9097 0.061 Uiso 1 calc R . .
C10 C 1.0655(4) 0.7999(3) 1.0622(2) 0.0589(7) Uani 1 d . . .
H10A H 1.0856 0.9033 1.1216 0.071 Uiso 1 calc R . .
H10B H 1.1634 0.7746 1.0783 0.071 Uiso 1 calc R . .
H10C H 0.9928 0.7361 1.0799 0.071 Uiso 1 calc R . .
C11 C 0.3002(2) 0.6459(2) 0.5265(2) 0.0275(5) Uani 1 d . . .
H11A H 0.1877 0.5954 0.4732 0.033 Uiso 1 calc R . .
H11B H 0.3323 0.7266 0.5013 0.033 Uiso 1 calc R . .
C12 C 0.3295(3) 0.7106(2) 0.6762(2) 0.0303(5) Uani 1 d . . .
H12A H 0.3200 0.8120 0.7052 0.036 Uiso 1 calc R . .
H12B H 0.2508 0.6495 0.6922 0.036 Uiso 1 calc R . .
C13 C 0.5074(3) 0.7477(3) 0.8959(2) 0.0427(6) Uani 1 d . . .
H13A H 0.6123 0.7495 0.9460 0.051 Uiso 1 calc R . .
H13B H 0.4304 0.6715 0.8977 0.051 Uiso 1 calc R . .
H13C H 0.4924 0.8442 0.9368 0.051 Uiso 1 calc R . .
C14 C 0.6098(3) 0.8260(2) 0.7531(2) 0.0350(5) Uani 1 d . . .
H14A H 0.7127 0.8258 0.8054 0.042 Uiso 1 calc R . .
H14B H 0.5970 0.9240 0.7922 0.042 Uiso 1 calc R . .
H14C H 0.6000 0.8022 0.6608 0.042 Uiso 1 calc R . .
N1 N 0.9976(2) 0.7784(2) 0.92268(18) 0.0371(4) Uani 1 d . . .
N2 N 0.4875(2) 0.71395(18) 0.75450(16) 0.0287(4) Uani 1 d . . .
O1 O 0.45949(16) 0.27333(14) 0.57191(13) 0.0256(3) Uani 1 d . . .
O2 O 0.34084(17) 0.43397(15) 0.69728(14) 0.0297(3) Uani 1 d . . .
O3 O 0.68836(17) 0.54780(16) 0.78272(14) 0.0337(4) Uani 1 d . . .
O4 O 0.38728(15) 0.54216(14) 0.49801(13) 0.0223(3) Uani 1 d . . .
Ti1 Ti 0.50306(4) 0.48029(4) 0.63971(3) 0.02143(13) 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 0.0020 0.0020 '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 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2480 0.4460 '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 C3 108.14(18) . . ?
O1 C1 C2 108.89(17) . . ?
C3 C1 C2 110.00(19) . . ?
O1 C1 C4 102.95(15) . . ?
C3 C1 C4 112.31(18) . . ?
C2 C1 C4 114.12(19) . . ?
O2 C4 C5 109.27(18) . . ?
O2 C4 C6 108.15(17) . . ?
C5 C4 C6 109.6(2) . . ?
O2 C4 C1 103.57(16) . . ?
C5 C4 C1 113.89(18) . . ?
C6 C4 C1 112.07(18) . . ?
O3 C7 C8 111.40(18) . . ?
N1 C8 C7 113.63(19) . . ?
O4 C11 C12 110.02(15) . . ?
N2 C12 C11 109.68(15) . . ?
C8 N1 C10 112.2(2) . . ?
C8 N1 C9 110.08(19) . . ?
C10 N1 C9 109.3(2) . . ?
C12 N2 C14 111.26(16) . . ?
C12 N2 C13 110.64(17) . . ?
C14 N2 C13 109.07(17) . . ?
C12 N2 Ti1 103.77(12) . . ?
C14 N2 Ti1 108.66(12) . . ?
C13 N2 Ti1 113.38(12) . . ?
C1 O1 Ti1 118.88(11) . . ?
C4 O2 Ti1 118.31(12) . . ?
C7 O3 Ti1 142.44(14) . . ?
C11 O4 Ti1 121.10(11) . . ?
C11 O4 Ti1 123.94(11) . 2_666 ?
Ti1 O4 Ti1 108.93(6) . 2_666 ?
O3 Ti1 O1 103.43(7) . . ?
O3 Ti1 O2 107.98(7) . . ?
O1 Ti1 O2 80.05(6) . . ?
O3 Ti1 O4 139.26(6) . . ?
O1 Ti1 O4 111.22(6) . . ?
O2 Ti1 O4 98.69(6) . . ?
O3 Ti1 O4 92.96(6) . 2_666 ?
O1 Ti1 O4 83.37(6) . 2_666 ?
O2 Ti1 O4 155.75(6) . 2_666 ?
O4 Ti1 O4 71.07(6) . 2_666 ?
O3 Ti1 N2 81.88(7) . . ?
O1 Ti1 N2 158.50(6) . . ?
O2 Ti1 N2 78.51(6) . . ?
O4 Ti1 N2 73.79(6) . . ?
O4 Ti1 N2 117.47(6) 2_666 . ?
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 1.427(2) . ?
C1 C3 1.522(3) . ?
C1 C2 1.524(3) . ?
C1 C4 1.558(3) . ?
C4 O2 1.417(3) . ?
C4 C5 1.522(3) . ?
C4 C6 1.526(3) . ?
C7 O3 1.402(3) . ?
C7 C8 1.508(4) . ?
C8 N1 1.451(3) . ?
C9 N1 1.455(3) . ?
C10 N1 1.452(3) . ?
C11 O4 1.430(2) . ?
C11 C12 1.523(3) . ?
C12 N2 1.468(3) . ?
C13 N2 1.478(3) . ?
C14 N2 1.473(3) . ?
N2 Ti1 2.3041(17) . ?
O1 Ti1 1.8665(14) . ?
O2 Ti1 1.8768(14) . ?
O3 Ti1 1.8131(15) . ?
O4 Ti1 2.0128(13) . ?
O4 Ti1 2.0909(13) 2_666 ?
Ti1 O4 2.0909(13) 2_666 ?
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
O1 C1 C4 O2 -40.33(19) . . . . ?
C3 C1 C4 O2 75.8(2) . . . . ?
C2 C1 C4 O2 -158.17(17) . . . . ?
O1 C1 C4 C5 -158.9(2) . . . . ?
C3 C1 C4 C5 -42.8(3) . . . . ?
C2 C1 C4 C5 83.3(3) . . . . ?
O1 C1 C4 C6 76.0(2) . . . . ?
C3 C1 C4 C6 -167.91(19) . . . . ?
C2 C1 C4 C6 -41.8(2) . . . . ?
O3 C7 C8 N1 64.3(2) . . . . ?
O4 C11 C12 N2 29.6(2) . . . . ?
C7 C8 N1 C10 69.5(3) . . . . ?
C7 C8 N1 C9 -168.46(19) . . . . ?
C11 C12 N2 C14 69.8(2) . . . . ?
C11 C12 N2 C13 -168.76(17) . . . . ?
C11 C12 N2 Ti1 -46.84(17) . . . . ?
C3 C1 O1 Ti1 -84.60(18) . . . . ?
C2 C1 O1 Ti1 155.89(14) . . . . ?
C4 C1 O1 Ti1 34.43(19) . . . . ?
C5 C4 O2 Ti1 157.22(15) . . . . ?
C6 C4 O2 Ti1 -83.56(18) . . . . ?
C1 C4 O2 Ti1 35.51(18) . . . . ?
C8 C7 O3 Ti1 106.4(2) . . . . ?
C12 C11 O4 Ti1 7.5(2) . . . . ?
C12 C11 O4 Ti1 -142.12(14) . . . 2_666 ?
C7 O3 Ti1 O1 35.5(2) . . . . ?
C7 O3 Ti1 O2 119.2(2) . . . . ?
C7 O3 Ti1 O4 -112.5(2) . . . . ?
C7 O3 Ti1 O4 -48.4(2) . . . 2_666 ?
C7 O3 Ti1 N2 -165.7(2) . . . . ?
C1 O1 Ti1 O3 92.53(14) . . . . ?
C1 O1 Ti1 O2 -13.75(13) . . . . ?
C1 O1 Ti1 O4 -109.29(13) . . . . ?
C1 O1 Ti1 O4 -175.99(14) . . . 2_666 ?
C1 O1 Ti1 N2 -9.6(2) . . . . ?
C4 O2 Ti1 O3 -115.88(14) . . . . ?
C4 O2 Ti1 O1 -14.88(13) . . . . ?
C4 O2 Ti1 O4 95.30(13) . . . . ?
C4 O2 Ti1 O4 32.7(2) . . . 2_666 ?
C4 O2 Ti1 N2 166.69(14) . . . . ?
C11 O4 Ti1 O3 -81.98(16) . . . . ?
Ti1 O4 Ti1 O3 71.67(10) 2_666 . . . ?
C11 O4 Ti1 O1 131.66(14) . . . . ?
Ti1 O4 Ti1 O1 -74.69(7) 2_666 . . . ?
C11 O4 Ti1 O2 49.02(14) . . . . ?
Ti1 O4 Ti1 O2 -157.32(7) 2_666 . . . ?
C11 O4 Ti1 O4 -153.66(17) . . . 2_666 ?
Ti1 O4 Ti1 O4 0.0 2_666 . . 2_666 ?
C11 O4 Ti1 N2 -26.24(14) . . . . ?
Ti1 O4 Ti1 N2 127.41(8) 2_666 . . . ?
C12 N2 Ti1 O3 -174.09(13) . . . . ?
C14 N2 Ti1 O3 67.44(13) . . . . ?
C13 N2 Ti1 O3 -54.01(16) . . . . ?
C12 N2 Ti1 O1 -68.0(2) . . . . ?
C14 N2 Ti1 O1 173.56(15) . . . . ?
C13 N2 Ti1 O1 52.1(2) . . . . ?
C12 N2 Ti1 O2 -63.77(12) . . . . ?
C14 N2 Ti1 O2 177.76(13) . . . . ?
C13 N2 Ti1 O2 56.31(15) . . . . ?
C12 N2 Ti1 O4 38.92(12) . . . . ?
C14 N2 Ti1 O4 -79.55(13) . . . . ?
C13 N2 Ti1 O4 159.00(16) . . . . ?
C12 N2 Ti1 O4 96.79(13) . . . 2_666 ?
C14 N2 Ti1 O4 -21.68(14) . . . 2_666 ?
C13 N2 Ti1 O4 -143.13(15) . . . 2_666 ?
