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_4324339
_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_moiety         '[Fe8(mu4-O)4(mu-pz)12(NCS)4].2CH2Cl2'
_chemical_formula_sum            'C42 H40 Cl4 Fe8 N28 O4 S4'
_chemical_formula_weight         1717.86
_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                 106.775(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.073(4)
_cell_length_b                   16.004(3)
_cell_length_c                   21.505(4)
_cell_measurement_temperature    298(2)
_cell_volume                     6614(2)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker AXS SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50188
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         14824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0577P)^2^+2.4216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                9114
_reflns_number_total             14824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101691q_si_001_1.cif
_cod_data_source_block           kl026(3a)
_cod_database_code               4324339