Hetero-Metallic {3d-4f-5d} Complexes: Preparation and Magnetic Behavior of Trinuclear [(LMe2Ni-Ln){W(CN)8}] Compounds (Ln = Gd, Tb, Dy, Ho, Er, Y; LMe2= Schiff base) and Variable SMM Characteristics for the Tb Derivative
Jean-Pascal Sutter; Sébastien Dhers; Jean-Pierre Costes; Carine Duhayon; Laure Vendier; Raghunathan Rajamani; S. Ramasesha; Inorganic Chemistry 48 (2009) 5820–5828; doi:10.1021/ic900003m

data_4302430
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       jean-pascal.sutter@lcc-toulouse.fr
_publ_contact_author_name        'J.-P. Sutter'
_publ_section_title
;
Hetero-Metallic {3d-4f-5d} Complexes: Preparation and Magnetic Behavior of
Trinuclear [(LMe2Ni-Ln){W(CN)8}] Compounds (Ln = Gd, Tb, Dy, Ho, Er, Y;
LMe2= Schiff base) and Variable SMM Characteristics for the Tb Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5820
_journal_page_last               5828
_journal_paper_doi               10.1021/ic900003m
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'2(C41 H54 Gd N14 Ni O9 W), C7 H15 N O2, 2(H2 O)'
_chemical_formula_sum            'C89 H127 Gd2 N29 Ni2 O22 W2'
_chemical_formula_weight         2754.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.256(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.6930(4)
_cell_length_b                   10.9040(2)
_cell_length_c                   22.1400(4)
_cell_measurement_reflns_used    20432
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.133
_cell_measurement_theta_min      2.6924
_cell_measurement_wavelength     0.71073
_cell_volume                     5455.39(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0155423148
_diffrn_orient_matrix_UB_12      0.0400372894
_diffrn_orient_matrix_UB_13      0.0181884192
_diffrn_orient_matrix_UB_21      0.0170807728
_diffrn_orient_matrix_UB_22      -0.0214491037
_diffrn_orient_matrix_UB_23      0.0263079317
_diffrn_orient_matrix_UB_31      0.0212924783
_diffrn_orient_matrix_UB_32      0.0465527085
_diffrn_orient_matrix_UB_33      -0.003554627
_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  0.036
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20555
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         9651
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                9294
_reflns_number_total             9651
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic900003m_si_002.cif
_cod_data_source_block           jps0816
_cod_database_code               4302430