A New Dinuclear Ti(IV)-Peroxo-Citrate Complex from Aqueous Solutions. Synthetic, Structural, and Spectroscopic Studies in Relevance to Aqueous Titanium(IV)-Peroxo-Citrate Speciation
M. Dakanali; E. T. Kefalas; C. P. Raptopoulou; A. Terzis; G. Voyiatzis; I. Kyrikou; T. Mavromoustakos; A. Salifoglou; Inorganic Chemistry 42 (2003) 4632–4639; doi:10.1021/ic0343051

data_4313919
_publ_section_title
;
 A New Dinuclear Ti(IV)-Peroxo-Citrate Complex from Aqueous Solutions.
 Synthetic, Structural, and Spectroscopic Studies in Relevance to Aqueous
 Titanium(IV)-Peroxo-Citrate Speciation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4632
_journal_page_last               4639
_journal_paper_doi               10.1021/ic0343051
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H28 N4 O20 Ti2'
_chemical_formula_weight         644.16
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.99(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.360(4)
_cell_length_b                   10.226(4)
_cell_length_c                   11.478(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      5.3
_cell_volume                     1156.5(9)
_computing_cell_refinement
'Program LEAST (UCLA Cryst.package C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Cryst.pckg C.E.Strouse 1994)'
_computing_data_reduction
' Program REDUCE (UCLA Cryst.package C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta scans'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2269
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        1.7
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_meas      1.75
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.127
_refine_ls_goodness_of_fit_obs   1.148
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_obs          0.0287
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+0.8656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0806
_refine_ls_wR_factor_obs         0.0785
_reflns_number_observed          1995
_reflns_number_total             2159
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0343051.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+0.8656P] 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^)+(0.0145P)^2^+0.8656P] 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        1156.6(9)
_cod_database_code               4313919