#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:04:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180371 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/40/7204071.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_7204071
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            'C20 H48 N4 O8 Ti2'
_chemical_formula_weight         568.52
_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                104.70(2)
_cell_angle_beta                 104.99(2)
_cell_angle_gamma                96.58(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2993(17)
_cell_length_b                   9.3651(19)
_cell_length_c                   9.7070(19)
_cell_measurement_temperature    213(2)
_cell_volume                     691.7(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 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3807
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0355
_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)+(0.0429P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                1548
_reflns_number_total             2063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100411p.txt
_cod_data_source_block           tony27
_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^)+(0.0429P)^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^)+(0.0429P)^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        691.7(2)
_cod_database_code               7204071
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 0.7040(4) 0.5274(3) 0.4549(3) 0.0300(7) Uani 1 d . . .
H1A H 0.6791 0.5368 0.5498 0.036 Uiso 1 calc R . .
H1B H 0.8224 0.5763 0.4763 0.036 Uiso 1 calc R . .
C2 C 0.6769(4) 0.3638(3) 0.3686(3) 0.0304(7) Uani 1 d . . .
H2A H 0.7719 0.3197 0.4119 0.036 Uiso 1 calc R . .
H2B H 0.5720 0.3087 0.3738 0.036 Uiso 1 calc R . .
C3 C 0.8348(4) 0.4036(4) 0.1998(4) 0.0346(8) Uani 1 d . . .
H3A H 0.8263 0.3953 0.0964 0.042 Uiso 1 calc R . .
H3B H 0.9126 0.3420 0.2355 0.042 Uiso 1 calc R . .
H3C H 0.8769 0.5078 0.2598 0.042 Uiso 1 calc R . .
C4 C 0.6049(4) 0.1931(3) 0.1212(4) 0.0374(8) Uani 1 d . . .
H4A H 0.5971 0.1844 0.0178 0.045 Uiso 1 calc R . .
H4B H 0.4938 0.1571 0.1280 0.045 Uiso 1 calc R . .
H4C H 0.6842 0.1332 0.1581 0.045 Uiso 1 calc R . .
C5 C 0.2746(4) 0.7403(3) 0.2750(3) 0.0277(7) Uani 1 d . . .
H5A H 0.3469 0.7543 0.3766 0.033 Uiso 1 calc R . .
H5B H 0.1671 0.6738 0.2590 0.033 Uiso 1 calc R . .
C6 C 0.2412(4) 0.8903(3) 0.2561(3) 0.0270(7) Uani 1 d . . .
H6A H 0.3499 0.9579 0.2784 0.032 Uiso 1 calc R . .
H6B H 0.1772 0.8761 0.1519 0.032 Uiso 1 calc R . .
C7 C 0.2523(5) 1.0200(3) 0.5078(4) 0.0446(9) Uani 1 d . . .
H7A H 0.1857 1.0654 0.5694 0.054 Uiso 1 calc R . .
H7B H 0.3468 1.0954 0.5146 0.054 Uiso 1 calc R . .
H7C H 0.2953 0.9391 0.5421 0.054 Uiso 1 calc R . .
C8 C 0.0784(5) 1.0813(3) 0.3046(4) 0.0461(9) Uani 1 d . . .
H8A H 0.0153 1.1268 0.3698 0.055 Uiso 1 calc R . .
H8B H 0.0034 1.0417 0.2031 0.055 Uiso 1 calc R . .
H8C H 0.1714 1.1566 0.3085 0.055 Uiso 1 calc R . .
C9 C 0.1745(4) 0.2998(4) 0.0327(4) 0.0371(8) Uani 1 d . . .
H9A H 0.0899 0.3637 0.0177 0.044 Uiso 1 calc R . .
H9B H 0.1178 0.2040 0.0370 0.044 Uiso 1 calc R . .
C10 C 0.2510(4) 0.2723(3) -0.0951(3) 0.0279(7) Uani 1 d . . .
H10A H 0.3003 0.1814 -0.1037 0.033 Uiso 1 calc R . .
H10B H 0.1649 0.2612 -0.1898 0.033 Uiso 1 calc R . .
O1 O 0.5927(2) 0.59590(19) 0.3658(2) 0.0260(5) Uani 1 d . . .
O2 O 0.3561(3) 0.6747(2) 0.1707(2) 0.0310(5) Uani 1 d . . .
O3 O 0.3063(2) 0.3714(2) 0.1677(2) 0.0296(5) Uani 1 d . . .
O4 O 0.3797(2) 0.40298(18) -0.0572(2) 0.0211(4) Uani 1 d . . .
N1 N 0.6651(3) 0.3516(2) 0.2115(3) 0.0243(6) Uani 1 d . . .
N2 N 0.1457(3) 0.9600(2) 0.3532(3) 0.0305(6) Uani 1 d . . .
Ti1 Ti 0.47410(6) 0.52137(5) 0.16656(6) 0.02046(16) 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'
O O 0.0080 0.0060 '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'
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 C2 107.6(3) . . ?
N1 C2 C1 109.1(2) . . ?
O2 C5 C6 109.2(2) . . ?
N2 C6 C5 112.3(2) . . ?
O3 C9 C10 108.7(2) . . ?
O4 C10 C9 104.5(2) . . ?
C1 O1 Ti1 128.19(18) . . ?
C5 O2 Ti1 129.90(17) . . ?
C9 O3 Ti1 117.81(16) . . ?
C10 O4 Ti1 133.53(16) . 2_665 ?
C10 O4 Ti1 116.04(15) . . ?
Ti1 O4 Ti1 109.14(8) 2_665 . ?
C4 N1 C2 109.2(2) . . ?
C4 N1 C3 108.5(2) . . ?
C2 N1 C3 109.8(2) . . ?
C4 N1 Ti1 116.68(18) . . ?
C2 N1 Ti1 99.73(16) . . ?
C3 N1 Ti1 112.52(16) . . ?
C8 N2 C7 108.9(2) . . ?
C8 N2 C6 110.1(2) . . ?
C7 N2 C6 111.3(2) . . ?
O2 Ti1 O1 93.42(9) . . ?
O2 Ti1 O3 99.34(9) . . ?
O1 Ti1 O3 101.43(9) . . ?
O2 Ti1 O4 93.74(8) . 2_665 ?
O1 Ti1 O4 106.52(9) . 2_665 ?
O3 Ti1 O4 148.28(9) . 2_665 ?
O2 Ti1 O4 99.88(9) . . ?
O1 Ti1 O4 166.56(8) . . ?
O3 Ti1 O4 78.46(8) . . ?
O4 Ti1 O4 70.86(8) 2_665 . ?
O2 Ti1 N1 168.15(9) . . ?
O1 Ti1 N1 74.98(8) . . ?
O3 Ti1 N1 85.61(8) . . ?
O4 Ti1 N1 87.38(7) 2_665 . ?
O4 Ti1 N1 91.64(8) . . ?
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 1.420(3) . ?
C1 C2 1.507(4) . ?
C2 N1 1.476(4) . ?
C3 N1 1.479(3) . ?
C4 N1 1.471(4) . ?
C5 O2 1.411(3) . ?
C5 C6 1.510(4) . ?
C6 N2 1.462(3) . ?
C7 N2 1.456(4) . ?
C8 N2 1.451(4) . ?
C9 O3 1.417(4) . ?
C9 C10 1.514(4) . ?
C10 O4 1.429(3) . ?
O1 Ti1 1.836(2) . ?
O2 Ti1 1.8263(18) . ?
O3 Ti1 1.8653(19) . ?
O4 Ti1 1.9880(17) 2_665 ?
O4 Ti1 2.064(2) . ?
N1 Ti1 2.409(2) . ?
Ti1 O4 1.9880(17) 2_665 ?
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 C2 N1 43.3(3) . . . . ?
O2 C5 C6 N2 175.8(2) . . . . ?
O3 C9 C10 O4 -38.1(3) . . . . ?
C2 C1 O1 Ti1 -14.0(3) . . . . ?
C6 C5 O2 Ti1 163.2(2) . . . . ?
C10 C9 O3 Ti1 40.9(3) . . . . ?
C9 C10 O4 Ti1 -171.40(19) . . . 2_665 ?
C9 C10 O4 Ti1 23.2(3) . . . . ?
C1 C2 N1 C4 -168.8(2) . . . . ?
C1 C2 N1 C3 72.4(3) . . . . ?
C1 C2 N1 Ti1 -45.9(2) . . . . ?
C5 C6 N2 C8 -165.0(3) . . . . ?
C5 C6 N2 C7 74.1(3) . . . . ?
C5 O2 Ti1 O1 -44.9(2) . . . . ?
C5 O2 Ti1 O3 57.2(2) . . . . ?
C5 O2 Ti1 O4 -151.8(2) . . . 2_665 ?
C5 O2 Ti1 O4 137.0(2) . . . . ?
C5 O2 Ti1 N1 -56.7(5) . . . . ?
C1 O1 Ti1 O2 172.7(2) . . . . ?
C1 O1 Ti1 O3 72.5(2) . . . . ?
C1 O1 Ti1 O4 -92.3(2) . . . 2_665 ?
C1 O1 Ti1 O4 -15.7(5) . . . . ?
C1 O1 Ti1 N1 -9.7(2) . . . . ?
C9 O3 Ti1 O2 76.7(2) . . . . ?
C9 O3 Ti1 O1 172.1(2) . . . . ?
C9 O3 Ti1 O4 -36.4(3) . . . 2_665 ?
C9 O3 Ti1 O4 -21.6(2) . . . . ?
C9 O3 Ti1 N1 -114.2(2) . . . . ?
C10 O4 Ti1 O2 -100.63(17) . . . . ?
Ti1 O4 Ti1 O2 90.55(9) 2_665 . . . ?
C10 O4 Ti1 O1 87.9(4) . . . . ?
Ti1 O4 Ti1 O1 -80.9(3) 2_665 . . . ?
C10 O4 Ti1 O3 -3.01(17) . . . . ?
Ti1 O4 Ti1 O3 -171.83(10) 2_665 . . . ?
C10 O4 Ti1 O4 168.8(2) . . . 2_665 ?
Ti1 O4 Ti1 O4 0.0 2_665 . . 2_665 ?
C10 O4 Ti1 N1 82.16(17) . . . . ?
Ti1 O4 Ti1 N1 -86.65(9) 2_665 . . . ?
C4 N1 Ti1 O2 160.0(4) . . . . ?
C2 N1 Ti1 O2 42.7(4) . . . . ?
C3 N1 Ti1 O2 -73.7(4) . . . . ?
C4 N1 Ti1 O1 147.8(2) . . . . ?
C2 N1 Ti1 O1 30.51(16) . . . . ?
C3 N1 Ti1 O1 -85.8(2) . . . . ?
C4 N1 Ti1 O3 44.7(2) . . . . ?
C2 N1 Ti1 O3 -72.57(17) . . . . ?
C3 N1 Ti1 O3 171.1(2) . . . . ?
C4 N1 Ti1 O4 -104.3(2) . . . 2_665 ?
C2 N1 Ti1 O4 138.38(16) . . . 2_665 ?
C3 N1 Ti1 O4 22.0(2) . . . 2_665 ?
C4 N1 Ti1 O4 -33.5(2) . . . . ?
C2 N1 Ti1 O4 -150.87(16) . . . . ?
C3 N1 Ti1 O4 92.8(2) . . . . ?
