Spin Structure of Surface-Supported Single-Molecule Magnets from Isomorphous Replacement and X-ray Magnetic Circular Dichroism
Matteo Mannini; Erik Tancini; Lorenzo Sorace; Philippe Sainctavit; Marie-Anne Arrio; Yu Qian; Edwige Otero; Daniele Chiappe; Ludovica Margheriti; Julio C. Cezar; Roberta Sessoli; Andrea Cornia; Inorganic Chemistry 50 (2011) 2911–2917; doi:10.1021/ic102184n

data_4324759
_publ_contact_author_address
;Department of Chemistry and INSTM Research Unit, 
University of Modena and Reggio Emilia,
Via G. Campi 183, 41100 Modena, Italy
;
_publ_contact_author_email       andrea.cornia@unimore.it
_publ_contact_author_fax         39(059)373543
_publ_contact_author_name        'Cornia, Andrea'
_publ_contact_author_phone       39(059)2055032
_publ_section_title
;
 Spin Structure of Surface-Supported Single-Molecule Magnets from
 Isomorphous Replacement and X-ray Magnetic Circular Dichroism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2911
_journal_page_last               2917
_journal_paper_doi               10.1021/ic102184n
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        synthesis
_chemical_formula_iupac          '[Fe3Cr(C11H19O2)6(C15H27SO4)2]'
_chemical_formula_moiety         'C96 H168 Cr Fe3 O20 S2'
_chemical_formula_sum            'C96 H168 Cr Fe3 O20 S2'
_chemical_formula_weight         1925.97
_chemical_name_common            Fe3CrC9SAc
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.929(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.4032(15)
_cell_length_b                   20.8832(13)
_cell_length_c                   18.9981(12)
_cell_measurement_reflns_used    7828
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.40
_cell_volume                     10768.0(11)
_computing_cell_refinement       'Bruker-Nonius X8APEX package'
_computing_data_collection       'Bruker-Nonius X8APEX package'
_computing_data_reduction        'Bruker-Nonius X8APEX package'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WINGX v1.70.01 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54658
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.8756
_exptl_absorpt_correction_T_min  0.7845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS - Bruker Nonius area detector scaling 
and absorption correction - V2.10'
;
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       prisms
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         12377
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+28.6834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                8635
_reflns_number_total             12377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102184n_si_002.cif
_cod_data_source_block           fe3crc9sac_4_work3
_cod_database_code               4324759