Iron(III) and Titanium(IV) Oxoalkoxide Chemistry: Synthetic, Structural, Magnetochemical and Spectroscopic Studies of [Ti3(m3-OPri)2(m-OPri)3(OPri)6][FeCl4] and [Fe5(m5-O)(m-OPri)8Cl5]
Jaisa Fernandes Soares; David J. Evans; Geraldo R. Friedermann; Peter B. Hitchcock; G. Jeffery Leigh; Giovana G. Nunes; Dayane M. Reis; Eduardo L. Sa; New J.Chem.(Nouv.J.Chim.)  (2004) –; doi:

data_7050339
_publ_section_title
;
Iron(III) and Titanium(IV) Oxoalkoxide Chemistry:
Synthetic, Structural, Magnetochemical and Spectroscopic Studies of
[Ti3(m3-OPri)2(m-OPri)3(OPri)6][FeCl4] and [Fe5(m5-O)(m-OPri)8Cl5]
;
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H56 Cl5 Fe5 O9'
_chemical_formula_sum            'C24 H56 Cl5 Fe5 O9'
_chemical_formula_weight         945.19
_chemical_name_common            '[Fe5Cl5(O){OiPr}8]'
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 91.861(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0547(3)
_cell_length_b                   9.9251(2)
_cell_length_c                   16.7734(5)
_cell_measurement_reflns_used    12217
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2005.78(9)
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.645144E-1
_diffrn_orient_matrix_UB_12      0.128418E-1
_diffrn_orient_matrix_UB_13      0.352249E-1
_diffrn_orient_matrix_UB_21      -0.493596E-1
_diffrn_orient_matrix_UB_22      0.171993E-1
_diffrn_orient_matrix_UB_23      -0.479889E-1
_diffrn_orient_matrix_UB_31      -0.170398E-1
_diffrn_orient_matrix_UB_32      -0.984417E-1
_diffrn_orient_matrix_UB_33      -0.37893E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20515
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.96
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.7479
_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    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+4.1745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2532
_reflns_number_total             3527
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7050339