Heterotetranuclear Oxalato-Bridged ReIV3MII (M = Mn, Fe, Co, Ni, Cu) Complexes: A New Example of a Single-Molecule Magnet (M = Ni)
José Martínez-Lillo; Donatella Armentano; Giovanni De Munno; Wolfgang Wernsdorfer; Juan Modesto Clemente-Juan; J. Krzystek; Francesc Lloret; Miguel Julve; Juan Faus; Inorganic Chemistry 48 (2009) 3027–3038; doi:10.1021/ic8021497

data_4301816
_publ_contact_author_address
;Departament de Qu\'imica Inorg\`anica
Facultat de Qu\'imica de la Universitat de Val\`encia
Avda. Dr. Moliner 50
46100 Burjassot, Val\`encia 
Spain
;
_publ_contact_author_email       juan.faus@uv.es
_publ_contact_author_name        'Juan Faus'
_publ_contact_author_phone       0034963544856
_publ_section_title
;
Heterotetranuclear Oxalato-Bridged ReIV3MII (M = Mn, Fe, Co, Ni, Cu)
Complexes: A New Example of a Single-Molecule Magnet (M = Ni)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3027
_journal_page_last               3038
_journal_paper_doi               10.1021/ic8021497
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C70 H144 Cl12 Fe N4 O12 Re3'
_chemical_formula_weight         2273.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.783(3)
_cell_angle_beta                 83.403(3)
_cell_angle_gamma                80.960(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0050(8)
_cell_length_b                   19.4680(17)
_cell_length_c                   25.580(2)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.35
_cell_volume                     4867.2(7)
_computing_cell_refinement       'Bruker-Nonius X8 APEX'
_computing_data_collection       'Bruker-Nonius X8 APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            97090
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         0.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  0.6978
_exptl_absorpt_correction_T_min  0.5186
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brownish-orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             2286
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.334
_refine_diff_density_min         -3.570
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         20920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                14703
_reflns_number_total             20920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8021497_si_001_1.cif
_cod_data_source_block           2
_cod_database_code               4301816