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_7050340
_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)(C7 H8)'
_chemical_formula_sum            'C31 H64 Cl5 Fe5 O9'
_chemical_formula_weight         1037.32
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab -1ab'
_symmetry_space_group_name_H-M   'P 4/n :1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4622(3)
_cell_length_b                   15.4621(3)
_cell_length_c                   19.2214(4)
_cell_measurement_reflns_used    21425
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4595.42(16)
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_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      -0.47186E-1
_diffrn_orient_matrix_UB_12      0.288966E-1
_diffrn_orient_matrix_UB_13      0.269355E-1
_diffrn_orient_matrix_UB_21      -0.257326E-1
_diffrn_orient_matrix_UB_22      0.218864E-1
_diffrn_orient_matrix_UB_23      -0.443642E-1
_diffrn_orient_matrix_UB_31      -0.359725E-1
_diffrn_orient_matrix_UB_32      -0.535606E-1
_diffrn_orient_matrix_UB_33      -0.35964E-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  0.1549
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33048
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.874
_exptl_absorpt_correction_T_max  0.8728
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3164
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.066
_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^)+(0.0590P)^2^+23.7302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.15
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                2397
_reflns_number_total             3164
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7050340