The Role of Order-Disorder Transitions in the Quest for Molecular Multiferroics: Structural and Magnetic Neutron Studies of a Mixed Valence Iron(II)-Iron(III) Formate Framework
Laura Cañadillas-Delgado; Oscar Fabelo; J. Alberto Rodríguez-Velamazán; Marie-Hélène Lemée-Cailleau; Sax A. Mason; Emilio Pardo; Francesc Lloret; Jiong-Peng Zhao; Xian-He Bu; Virginie Simonet; Claire V. Colin; Juan Rodríguez-Carvajal; Journal of the American Chemical Society 134 (2012) 19772–19781; doi:10.1021/ja3082457

data_4118946
_publ_contact_author_address
;Instituto de Ciencia de Materiales de Arag\'on, CSIC-Universidad de Zaragoza, 
C/ Pedro Cerbuna 12, E-50009, Zaragoza, Spain.
Institut Laue-Langevin, Grenoble, 
6 rue Jules Horowitz, B.P. 156, 38042 Grenoble Cedex 9, France.
;
_publ_contact_author_email       fabelo@ill.fr
_publ_contact_author_name        'Dr. Oscar Fabelo'
_publ_section_title
;
 The Role of Order-Disorder Transitions in the Quest for Molecular
 Multiferroics: Structural and Magnetic Neutron Studies of a Mixed Valence
 Iron(II)-Iron(III) Formate Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19772
_journal_page_last               19781
_journal_paper_doi               10.1021/ja3082457
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C8 H14 Fe2 N O12'
_chemical_formula_weight         427.89
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      163
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.2550(12)
_cell_length_b                   8.2550(12)
_cell_length_c                   13.891(3)
_cell_measurement_temperature    220(2)
_cell_volume                     819.8(2)
_computing_cell_refinement       'lauegen (CCP4)'
_computing_data_collection       'VIVALDI (MAATEL)'
_computing_data_reduction        'argonne_boxes, laue4 (Piltz, 2011)'
_computing_molecular_graphics    'Mercury (McRae, 2006)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 0.7
_diffrn_measurement_device_type  'VIVALDI Laue Instrument'
_diffrn_measurement_method       'Laue patterns at 10 orientations'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL reactor source, thermal guide'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.80-5.20
_diffrn_reflns_av_R_equivalents  0.2526
_diffrn_reflns_av_sigmaI/netI    0.1318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15574
_diffrn_reflns_theta_max         38.64
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             197
_exptl_crystal_size_max          3
_exptl_crystal_size_mid          1
_exptl_crystal_size_min          1
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.513
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.513
_refine_ls_R_factor_all          0.2406
_refine_ls_R_factor_gt           0.1800
_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^)+(0.0454P)^2^+20.4879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2635
_refine_ls_wR_factor_ref         0.2777
_reflns_number_gt                713
_reflns_number_total             838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3082457_si_002.cif
_cod_data_source_block           VIVALDI
_cod_database_code               4118946