Multi-Temperature Crystallographic Studies of Mixed-Valence Polynuclear Complexes; Valence Trapping Process in the Trinuclear Oxo-Bridged Iron Compound, [Fe3O(O2CC(CH3)3)6(C5H5N)3]
Claire Wilson; Bo B. Iversen; Jacob Overgaard; Finn K. Larsen; Guang Wu; Sergiu P. Palii; Grigore A. Timco; Nicolae V. Gerbeleu; Journal of the American Chemical Society 122 (2000) 11370–11379; doi:10.1021/ja994162a

data_4116249
_publ_section_title
;
 Multi-Temperature Crystallographic Studies of Mixed-Valence Polynuclear
 Complexes; Valence Trapping Process in the Trinuclear Oxo-Bridged Iron
 Compound, [Fe3O(O2CC(CH3)3)6(C5H5N)3]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11370
_journal_page_last               11379
_journal_paper_doi               10.1021/ja994162a
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C45 H69 Fe3 N3 O13'
_chemical_formula_weight         1027.58
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.786(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6670(10)
_cell_length_b                   19.918(2)
_cell_length_c                   11.9810(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2665.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34002
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.864
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_F_000             1084
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         14491
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          1.642
_refine_ls_shift/su_mean         0.048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+2.3436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                10742
_reflns_number_total             14491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja994162a_08.cif
_cod_data_source_block           fe160m
_cod_database_code               4116249