Novel double alkoxides of titanium(IV) and iron(II)/(III): synthetic, structural and spectroscopic studies
Nunes, Giovana G.; Reis, Dayane M.; Amorim, Priscila T.; Sá, Eduardo L.; Mangrich, Antonio S.; Evans, David J.; Hitchcock, Peter B.; Jeffery Leigh, G.; Nunes, Fábio S.; Soares, Jaísa F.; New Journal of Chemistry 26 (2002) 519–; doi:10.1039/b111517k

data_7050816
_publ_section_title
;
 Novel double alkoxides of titanium(IV) and iron(II)/(III): synthetic,
 structural and spectroscopic studies
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              519
_journal_paper_doi               10.1039/b111517k
_journal_volume                  26
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H63 Cl1 Fe1 O9 Ti2'
_chemical_formula_structural     'C27 H63 CL1 FE1 O9 TI2'
_chemical_formula_sum            'C27 H63 Cl Fe O9 Ti2'
_chemical_formula_weight         718.87
_chemical_name_common            '[Ti2FeCl(OiPr)9]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-09-21T09:53:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                84.2130(10)
_cell_angle_beta                 83.6270(10)
_cell_angle_gamma                60.7220(10)
_cell_formula_units_Z            2
_cell_length_a                   9.89820(10)
_cell_length_b                   10.1089(2)
_cell_length_c                   21.5840(3)
_cell_measurement_reflns_used    18627
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1869.47(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27583
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.7678
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.7285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                5987
_reflns_number_total             6542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111517k.txt
_cod_data_source_block           sep1899
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050816