Designed cyanide- and phenoxide-bridged FeIIIMnIII single-molecule magnet constructed by highly blocked paramagnetic precursors
Kyung Jin Cho; Dae Won Ryu; Hyun Young Kwak; Jin Wuk Lee; Woo Ram Lee; Kwang Soo Lim; Eui Kwan Koh; Young Wan Kwon; Chang Seop Hong; Chem.Commun. 48 (2012) 7404–; doi:10.1039/c2cc32503a

data_7108004
_publ_section_title
;
 Designed cyanide- and phenoxide-bridged FeIIIMnIII single-molecule magnet
 constructed by highly blocked paramagnetic precursors
;
_journal_name_full               Chem.Commun.
_journal_page_first              7404
_journal_paper_doi               10.1039/c2cc32503a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C92 H104 B2 Br4 Fe2 Mn2 N22 O4'
_chemical_formula_weight         2144.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                98.07(3)
_cell_angle_beta                 105.42(3)
_cell_angle_gamma                98.98(3)
_cell_formula_units_Z            1
_cell_length_a                   12.414(3)
_cell_length_b                   14.003(3)
_cell_length_c                   15.544(3)
_cell_measurement_reflns_used    12392
_cell_measurement_temperature    100(2)
_cell_volume                     2525.5(11)
_computing_cell_refinement       HKL2000
_computing_data_collection       'PAL ADSC Quantum-210'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.797
_diffrn_measured_fraction_theta_max 0.491
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Pt coated Si double crystal'
_diffrn_radiation_source         'Fixed gap multipole wiggler beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.85000
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7063
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.64
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.9379
_exptl_absorpt_correction_T_min  0.8125
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   HKL2000-Scalepack
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The contributions of some 66 electrons were removed from the unit-cell
contents, and as Z = 1 in this case, this could/might correspond with the
removal of solvent such as 1.5(MeOH) and 1.5(MeCN) [some 60 electrons]
from the FeIII2MnIII2 formula unit.
;
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2315
_reflns_number_gt                3313
_reflns_number_total             4889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32503a.txt
_cod_data_source_block           squeezed
_cod_original_cell_volume        2525.6(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108004