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_7050817
_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
;
'(C29 H69 O11 Ti3)(C27 H63 Cl4 Fe4 O10 Ti1)'
;
_chemical_formula_sum            'C56 H132 Cl4 Fe4 O21 Ti4'
_chemical_formula_weight         1698.42
_chemical_name_common            '[Ti3(OiPr)9(OMe)2][Fe4TiCl4(O)(OiPr)9]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-09-20T16:09:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.312(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9455(3)
_cell_length_b                   38.1289(12)
_cell_length_c                   16.0638(5)
_cell_measurement_reflns_used    47488
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     8489.8(4)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0962
_diffrn_reflns_av_unetI/netI     0.151
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35844
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         14781
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                7669
_reflns_number_total             14781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111517k.txt
_cod_data_source_block           sep2800
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7050817