Experimental and Theoretical Mössbauer Study of an Extended Family of [Fe8(μ4-O)4(μ-4-R-px)12X4] Clusters
Ekaterina M. Zueva; W. M. C. Sameera; Dalice M. Piñero; Indranil Chakraborty; Eamonn Devlin; Peter Baran; Katarina Lebruskova; Yiannis Sanakis; John E. McGrady; Raphael G. Raptis; Inorganic Chemistry 50 (2011) 1021–1029; doi:10.1021/ic101691q

data_4324340
_publ_section_title
;
 Experimental and Theoretical M\"ossbauer Study of an Extended Family of
 [Fe8(\m4-O)4(\m-4-R-px)12X4] Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1021
_journal_page_last               1029
_journal_paper_doi               10.1021/ic101691q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H24 Cl12 Fe8 N28 O4 S4'
_chemical_formula_weight         1961.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.528(3)
_cell_length_b                   22.157(4)
_cell_length_c                   27.626(6)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.35
_cell_measurement_theta_min      4.74
_cell_volume                     8167(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1060
_diffrn_reflns_av_sigmaI/netI    0.1145
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            59650
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.485
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         18580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+28.9875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2293
_reflns_number_gt                8976
_reflns_number_total             18580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101691q_si_001_2.cif
_cod_data_source_block           ic034(3c)
_cod_database_code               4324340