Single-Molecule Magnets Constructed from Cyanometalates: {[Tp*FeIII(CN)3MII(DMF)4]2[OTf]2}.2DMF (MII= Co, Ni)
Dongfeng Li; Sean Parkin; Guangbin Wang; Gordon T. Yee; Andrey V. Prosvirin; Stephen M. Holmes; Inorganic Chemistry 44 (2005) 4903–4905; doi:10.1021/ic048367i

data_4309156
_publ_contact_author_name        'Stephen M. Holmes'
_publ_section_title
;
Single-Molecule Magnets Constructed from Cyanometalates:
{[Tp*FeIII(CN)3MII(DMF)4]2[OTf]2}.2DMF (MII= Co, Ni)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4905
_journal_paper_doi               10.1021/ic048367i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         ((Tp*FeIII(CN)3-MII(DMF)4)2-(OTf)2.2DMF
_chemical_formula_sum            'C68 H114 B2 F6 Fe2 Mn2 N28 O16 S2'
_chemical_formula_weight         2001.19
_chemical_name_systematic
;
?
;
_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                 107.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.295(3)
_cell_length_b                   13.194(3)
_cell_length_c                   24.321(5)
_cell_measurement_reflns_used    25457
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     4691.3(19)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1995)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c == 55\%'
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31439
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.9336
_exptl_absorpt_correction_T_min  0.8733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         8252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1178P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                5393
_reflns_number_total             8252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048367isi20041124_115151_2.cif
_cod_data_source_block           k04010
_cod_original_cell_volume        4691.3(16)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4309156