Multi-temperature X-ray diffraction, Mössbauer spectroscopy and magnetic susceptibility studies of a solvated mixed-valence trinuclear iron formate, [Fe3O(HCO2)6(NC5H4CH3)3]·1.3(NC5H4CH3)
Overgaard, Jacob; Rentschler, Eva; Timco, Grigore A.; Gerbeleu, Nicolae V.; Arion, Vladimir; Bousseksou, Azzedine; Tuchagues, Jean Pierre; Larsen, Finn K.; Journal of the Chemical Society, Dalton Transactions  (2002) 2981–; doi:10.1039/b202851d

data_7011685
_publ_section_title
;
 Multi-temperature X-ray diffraction, M\"ossbauer spectroscopy and
 magnetic susceptibility studies of a solvated mixed-valence trinuclear
 iron formate, [Fe3O(HCO2)6(NC5H4CH3)3]&#x00B7;1.3(NC5H4CH3)
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2981
_journal_paper_doi               10.1039/b202851d
_journal_year                    2002
_chemical_formula_sum            'C29.64 H27 Fe3 N3.94 O13'
_chemical_formula_weight         813.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.000(12)
_cell_angle_beta                 96.221(9)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            8
_cell_length_a                   24.495(5)
_cell_length_b                   27.532(6)
_cell_length_c                   12.685(3)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.098
_cell_measurement_theta_min      2.260
_cell_volume                     8504(3)
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT+ V5.01 (Bruker, 1998)'
_computing_molecular_graphics    'XP (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       \w-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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42046
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Sheldrick 1996)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             3315
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         9983
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+18.6138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2984
_reflns_number_gt                5596
_reflns_number_total             9983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202851d.txt
_cod_data_source_block           p87_295
_cod_original_cell_volume        8505(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7011685