Syntheses, Structures, and Magnetic Properties of Acetato- and Diphenolato-Bridged 3d-4f Binuclear Complexes [M(3-MeOsaltn)(MeOH)x(ac)Ln(hfac)2] (M = ZnII, CuII, NiII, CoII; Ln = LaIII, GdIII, TbIII, DyIII; 3-MeOsaltn =N,N'-Bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato; ac = Acetato; hfac = Hexafluoroacetylacetonato;x= 0 or 1)
Masaaki Towatari; Koshiro Nishi; Takeshi Fujinami; Naohide Matsumoto; Yukinari Sunatsuki; Masaaki Kojima; Naotaka Mochida; Takayuki Ishida; Nazzareno Re; Jerzy Mrozinski; Inorganic Chemistry 52 (2013) 6160–6178; doi:10.1021/ic400594u

data_4334968
_publ_contact_author_email       naohide@aster.sci.kumamoto-u.ac.jp
_publ_contact_author_fax         +81-96-342-3390
_publ_contact_author_name        'Naohide Matsumoto'
_publ_contact_author_phone       +81-96-342-3390
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of Acetato- and
 Diphenolato-Bridged 3d-4f Binuclear Complexes
 [M(3-MeOsaltn)(MeOH)x(ac)Ln(hfac)2] (M = ZnII, CuII, NiII, CoII; Ln =
 LaIII, GdIII, TbIII, DyIII; 3-MeOsaltn
 =N,N'-Bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato; ac = Acetato;
 hfac = Hexafluoroacetylacetonato;x= 0 or 1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6160
_journal_page_last               6178
_journal_paper_doi               10.1021/ic400594u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C33 H33 Co F12 N2 O12 Tb'
_chemical_formula_sum            'C33 H33 Co F12 N2 O12 Tb'
_chemical_formula_weight         1095.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.0478(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.1053(6)
_cell_length_b                   12.7743(4)
_cell_length_c                   19.6165(5)
_cell_measurement_reflns_used    29350
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.00
_cell_volume                     4026.6(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36152
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2164.00
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9154
_refine_ls_number_restraints     24
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0369P)^2^+12.7407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                8264
_reflns_number_total             9154
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic400594u_si_002_09.cif
_cod_data_source_block           Co-Tb130107
_cod_original_cell_volume        4026.64(19)
_cod_database_code               4334968