#------------------------------------------------------------------------------
#$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005086.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005086
loop_
_publ_author_name
'Gibson, D. H.'
'Ding, Y.'
'Richardson, J. F.'
'Mashuta, M. S.'
_publ_contact_author
; Dorothy H. Gibson
Department of Chemistry and Center for Chemical Catalysis
University of Louisville
Louisville
KY  40292
USA
;
_publ_section_title
;
 Bis(\h^5^-cyclopentadienyl)bis(formato-<i>O</i>)titanium
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1614
_journal_page_last               1616
_journal_paper_doi               10.1107/S0108270196002715
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ti (C5 H5)2 (C H O2)2]'
_chemical_formula_moiety         'C12 H12 O4 Ti '
_chemical_formula_sum            'C12 H12 O4 Ti'
_chemical_formula_weight         268.12
_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'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 99.71(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.210(2)
_cell_length_b                   12.076(5)
_cell_length_c                   11.949(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     1167.7(6)
_computing_cell_refinement       'Diffractometer Control Software'
_computing_data_collection
'Diffractometer Control Software (Enraf-Nonius, 1988)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1993)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'DIRDIF92 (PATTY) (Beurskens et al., 1992)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2856
_diffrn_reflns_theta_max         26.94
_diffrn_standards_decay_%        <2.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type
'empirical, \y scans (North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             552.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.24
_refine_ls_extinction_coef       '3.1(2) x 10^-6^'
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.88
_refine_ls_hydrogen_treatment
'H atoms refined with isotropic thermal parameters'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1933
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.038
_refine_ls_shift/esd_max         0.0240
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s^2^(F)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.038
_reflns_number_observed          1933
_reflns_number_total             2689
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            bk1212.cif
_cod_data_source_block           Ticp
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C12 H12 O4 Ti '
_cod_database_code               2005086
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,1/2+y,1/2-z'
'   -x,   -y,   -z'
'   +x,1/2-y,1/2+z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ti 0.0293(2) 0.0294(3) 0.0417(3) -0.0027(2) 0.0093(2) -0.0032(2)
O(1) 0.0340(10) 0.0500(10) 0.110(2) -0.0049(10) 0.0260(10) -0.0100(10)
O(2) 0.069(2) 0.091(2) 0.205(4) -0.002(2) 0.064(2) -0.057(2)
O(3) 0.0410(10) 0.0420(10) 0.0530(10) 0.0101(9) 0.0016(9) -0.0124(9)
O(4) 0.0470(10) 0.085(2) 0.086(2) 0.0150(10) 0.0180(10) 0.0010(10)
C(1) 0.039(2) 0.061(2) 0.120(3) -0.007(2) 0.026(2) -0.020(2)
C(2) 0.057(2) 0.042(2) 0.045(2) 0.010(2) 0.0060(10) -0.0020(10)
C(3) 0.081(3) 0.055(2) 0.065(2) -0.015(2) -0.020(2) 0.022(2)
C(4) 0.078(3) 0.060(2) 0.060(2) -0.004(2) 0.028(2) 0.015(2)
C(5) 0.055(2) 0.067(2) 0.066(2) -0.026(2) 0.003(2) 0.020(2)
C(6) 0.136(4) 0.030(2) 0.071(3) -0.018(2) 0.028(3) -0.007(2)
C(7) 0.056(3) 0.054(3) 0.164(5) 0.018(2) 0.023(3) 0.050(3)
C(8) 0.131(4) 0.066(3) 0.052(2) -0.009(3) 0.038(2) -0.019(2)
C(9) 0.097(3) 0.061(2) 0.056(2) -0.022(2) 0.034(2) -0.002(2)
C(10) 0.098(3) 0.067(3) 0.046(2) 0.011(2) 0.011(2) 0.011(2)
C(11) 0.053(3) 0.212(8) 0.035(2) 0.025(4) 0.002(2) 0.026(3)
C(12) 0.136(5) 0.093(4) 0.036(2) -0.067(3) -0.010(2) 0.008(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ti .18682(5) .05394(4) .22452(4) .03310(10) Uij
O(1) -.0493(2) .0223(2) .2077(2) .0630(7) Uij
O(2) -0.2162(3) .1435(2) .2675(3) .1170(10) Uij
O(3) .2186(2) -.0764(2) .1343(2) .0462(5) Uij
O(4) .4748(3) -0.1259(2) .1242(2) .0717(8) Uij
C(1) -0.1892(4) .0590(3) .2233(4) .0720(10) Uij
C(2) .3288(4) -0.1403(3) .1059(3) .0485(9) Uij
C(3) .1280(5) .1450(3) .0467(3) .0710(10) Uij
C(4) .2953(5) .1366(3) .0732(3) .0640(10) Uij
C(5) .3500(5) .1966(3) .1681(3) .0640(10) Uij
C(6) .2167(7) .2452(3) .2025(4) .078(2) Uij
C(7) .0777(6) .2139(4) .1265(6) .091(2) Uij
C(8) .1998(7) .0830(4) .4206(3) .0800(10) Uij
C(9) .1684(6) -.0274(3) .4042(3) .0690(10) Uij
C(10) .2950(6) -.0763(4) .3685(3) .0700(10) Uij
C(11) .4131(6) .0066(7) .3623(4) .101(2) Uij
C(12) .3527(8) .1042(4) .3972(3) .091(2) Uij
H(1) -0.278(4) .009(3) .186(3) .080(10) Uij
H(2) .283(3) -0.205(2) .068(2) .057(9) Uij
H(3) .064(4) .110(3) -.010(3) .090(10) Uij
H(4) .363(4) .094(3) .041(3) .090(10) Uij
H(5) .457(4) .205(3) .200(3) .080(10) Uij
H(6) .224(4) .277(3) .260(3) .070(10) Uij
H(7) -.024(5) .235(3) .129(4) .10(2) Uij
H(8) .132(5) .134(4) .439(4) .13(2) Uij
H(9) .067(5) -.066(3) .401(3) .110(10) Uij
H(10) .294(5) -0.148(3) .344(3) .090(10) Uij
H(11) .504(4) -.019(3) .340(3) .024(9) Uij
H(12) .384(5) .172(4) .401(3) .110(10) Uij
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ti 0.278 0.446 'International Tables'
C 0.003 0.002 'International Tables'
H 0.000 0.000 'International Tables'
O 0.011 0.006 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) Ti O(3) 90.56(8) yes
O(1) Ti C(3) 87.10(10) no
O(1) Ti C(4) 119.90(10) no
O(1) Ti C(5) 135.80(10) no
O(1) Ti C(6) 107.5(2) no
O(1) Ti C(7) 79.60(10) no
O(1) Ti C(8) 90.50(10) no
O(1) Ti C(9) 78.50(10) no
O(1) Ti C(10) 100.90(10) no
O(1) Ti C(11) 133.1(2) no
O(1) Ti C(12) 123.9(2) no
O(3) Ti C(3) 84.60(10) no
O(3) Ti C(4) 79.30(10) no
O(3) Ti C(5) 107.30(10) no
O(3) Ti C(6) 135.10(10) no
O(3) Ti C(7) 117.6(2) no
O(3) Ti C(8) 133.00(10) no
O(3) Ti C(9) 101.50(10) no
O(3) Ti C(10) 78.30(10) no
O(3) Ti C(11) 91.5(2) no
O(3) Ti C(12) 125.5(2) no
C(3) Ti C(4) 33.40(10) no
C(3) Ti C(5) 56.10(10) no
C(3) Ti C(6) 56.70(10) no
C(3) Ti C(7) 34.0(2) no
C(3) Ti C(8) 142.3(2) no
C(3) Ti C(9) 164.3(2) no
C(3) Ti C(10) 161.2(2) no
C(3) Ti C(11) 139.8(2) no
C(3) Ti C(12) 131.90(10) no
C(4) Ti C(5) 33.40(10) no
C(4) Ti C(6) 55.90(10) no
C(4) Ti C(7) 55.6(2) no
C(4) Ti C(8) 137.6(2) no
C(4) Ti C(9) 161.60(10) no
C(4) Ti C(10) 133.3(2) no
C(4) Ti C(11) 106.5(2) no
C(4) Ti C(12) 109.0(2) no
C(5) Ti C(6) 33.90(10) no
C(5) Ti C(7) 56.20(10) no
C(5) Ti C(8) 104.2(2) no
C(5) Ti C(9) 133.20(10) no
C(5) Ti C(10) 121.9(2) no
C(5) Ti C(11) 87.6(2) no
C(5) Ti C(12) 77.90(10) no
C(6) Ti C(7) 34.3(2) no
C(6) Ti C(8) 88.70(10) no
C(6) Ti C(9) 122.00(10) no
C(6) Ti C(10) 134.2(2) no
C(6) Ti C(11) 103.6(2) no
C(6) Ti C(12) 77.8(2) no
C(7) Ti C(8) 108.8(2) no
C(7) Ti C(9) 135.0(2) no
C(7) Ti C(10) 164.1(2) no
C(7) Ti C(11) 137.9(3) no
C(7) Ti C(12) 109.9(2) no
C(8) Ti C(9) 33.50(10) no
C(8) Ti C(10) 55.4(2) no
C(8) Ti C(11) 55.8(2) no
C(8) Ti C(12) 33.5(2) no
C(9) Ti C(10) 32.30(10) no
C(9) Ti C(11) 55.2(2) no
C(9) Ti C(12) 55.40(10) no
C(10) Ti C(11) 34.5(2) no
C(10) Ti C(12) 56.5(2) no
C(11) Ti C(12) 34.0(2) no
Ti O(1) C(1) 145.2(2) yes
Ti O(3) C(2) 143.3(2) yes
O(1) C(1) O(2) 127.2(3) no
O(3) C(2) O(4) 126.7(3) no
Ti C(3) C(4) 73.2(2) no
Ti C(3) C(7) 72.6(2) no
C(4) C(3) C(7) 107.1(4) no
Ti C(4) C(3) 73.4(2) no
Ti C(4) C(5) 72.6(2) no
C(3) C(4) C(5) 109.4(4) no
Ti C(5) C(4) 74.0(2) no
Ti C(5) C(6) 72.8(2) no
C(4) C(5) C(6) 108.2(4) no
Ti C(6) C(5) 73.3(2) no
Ti C(6) C(7) 73.5(2) no
C(5) C(6) C(7) 107.4(4) no
Ti C(7) C(3) 73.5(2) no
Ti C(7) C(6) 72.2(2) no
C(3) C(7) C(6) 107.9(4) no
Ti C(8) C(9) 74.7(2) no
Ti C(8) C(12) 73.2(2) no
C(9) C(8) C(12) 108.2(4) no
Ti C(9) C(8) 71.9(2) no
Ti C(9) C(10) 74.0(2) no
C(8) C(9) C(10) 110.1(4) no
Ti C(10) C(9) 73.8(2) no
Ti C(10) C(11) 70.6(2) no
C(9) C(10) C(11) 106.5(4) no
Ti C(11) C(10) 74.8(2) no
Ti C(11) C(12) 73.6(3) no
C(10) C(11) C(12) 107.9(4) no
Ti C(12) C(8) 73.3(2) no
Ti C(12) C(11) 72.4(2) no
C(8) C(12) C(11) 107.3(4) no
O(1) C(1) H(1) 110(2) no
O(2) C(1) H(1) 123(2) no
O(3) C(2) H(2) 113(2) no
O(4) C(2) H(2) 121(2) no
C(4) C(3) H(3) 126(2) no
C(7) C(3) H(3) 127(2) no
C(3) C(4) H(4) 129(2) no
C(5) C(4) H(4) 122(2) no
C(4) C(5) H(5) 125(2) no
C(6) C(5) H(5) 126(2) no
C(5) C(6) H(6) 122(3) no
C(7) C(6) H(6) 130(3) no
C(3) C(7) H(7) 126.8(4) no
C(6) C(7) H(7) 125.1(3) no
C(9) C(8) H(8) 128(3) no
C(12) C(8) H(8) 124(3) no
C(8) C(9) H(9) 129(3) no
C(10) C(9) H(9) 120(3) no
C(9) C(10) H(10) 124(2) no
C(11) C(10) H(10) 129(2) no
C(10) C(11) H(11) 112.8(4) no
C(12) C(11) H(11) 138.6(4) no
C(8) C(12) H(12) 117(3) no
C(11) C(12) H(12) 136(3) no
M(1) Ti M(2) 132.0 yes
O(1) Ti M(1) 107.2 yes
O(1) Ti M(2) 106.4 yes
O(3) Ti M(1) 105.8 yes
O(3) Ti M(2) 107.0 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ti O(1) 1.952(2) yes
Ti O(3) 1.951(2) yes
Ti C(3) 2.369(3) no
Ti C(4) 2.367(3) no
Ti C(5) 2.349(3) no
Ti C(6) 2.342(3) no
Ti C(7) 2.357(4) no
Ti C(8) 2.353(4) no
Ti C(9) 2.388(3) no
Ti C(10) 2.391(4) no
Ti C(11) 2.337(4) no
Ti C(12) 2.352(4) no
O(1) C(1) 1.275(4) yes
O(2) C(1) 1.188(4) yes
O(3) C(2) 1.279(3) yes
O(4) C(2) 1.194(4) yes
C(3) C(4) 1.361(5) no
C(3) C(7) 1.380(7) no
C(4) C(5) 1.356(5) no
C(5) C(6) 1.367(6) no
C(6) C(7) 1.386(6) no
C(8) C(9) 1.365(5) no
C(8) C(12) 1.355(6) no
C(9) C(10) 1.327(5) no
C(10) C(11) 1.404(7) no
C(11) C(12) 1.371(8) no
C(1) H(1) 0.99(3) no
C(2) H(2) 0.94(3) no
C(3) H(3) 0.89(4) no
C(4) H(4) 0.89(3) no
C(5) H(5) 0.90(3) no
C(6) H(6) 0.78(3) no
C(7) H(7) 0.88(3) no
C(8) H(8) 0.89(4) no
C(9) H(9) 0.94(4) no
C(10) H(10) 0.92(4) no
C(11) H(11) 0.89(4) no
C(12) H(12) 0.85(4) no
Ti M(1) 2.049 yes
Ti M(2) 2.059 yes