Face-Sharing Heterotrinuclear MII-LnIII-MII (M = Mn, Fe, Co, Zn; Ln = La, Gd, Tb, Dy) Complexes: Synthesis, Structures, and Magnetic Properties
Tomoka Yamaguchi; Jean-Pierre Costes; Yukana Kishima; Masaaki Kojima; Yukinari Sunatsuki; Nicolas Bréfuel; Jean-Pierre Tuchagues; Laure Vendier; Wolfgang Wernsdorfer; Inorganic Chemistry 49 (2010) 9125–9135; doi:10.1021/ic100460w

data_4316700
_publ_contact_author             'Costes jean-Pierre'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       jean-pierre.costes@lcc-toulouse.fr
_publ_section_title
;
 Face-Sharing Heterotrinuclear MII-LnIII-MII (M = Mn, Fe, Co, Zn; Ln = La,
 Gd, Tb, Dy) Complexes: Synthesis, Structures, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9125
_journal_page_last               9135
_journal_paper_doi               10.1021/ic100460w
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H60 Co2 Dy N6 O12, C H4 O, N O3'
_chemical_formula_sum            'C59 H64 Co2 Dy N7 O16'
_chemical_formula_weight         1407.53
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7227(10)
_cell_length_b                   15.8241(10)
_cell_length_c                   24.3813(15)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1539
_cell_measurement_theta_min      2.8166
_cell_measurement_wavelength     0.71073
_cell_volume                     6066.0(7)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44289
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.7976
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         11485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                9170
_reflns_number_total             11485
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic100460w_si_002_4.cif
_cod_data_source_block           3
_cod_database_code               4316700