Preparation, Crystal Structures, and Magnetic Features for a Series of Dinuclear [NiIILnIII] Schiff-Base Complexes: Evidence for Slow Relaxation of the Magnetization for the DyIII Derivative
Traian D. Pasatoiu; Jean-Pascal Sutter; Augustin M. Madalan; Fatima Zohra Chiboub Fellah; Carine Duhayon; Marius Andruh; Inorganic Chemistry 50 (2011) 5890–5898; doi:10.1021/ic2004276

data_4325508
_publ_contact_author_email       'jean-pascal.sutter@lcc-toulouse.fr '
_publ_contact_author_fax         '(33) 5 61 55 30 03'
_publ_contact_author_name        'JP Sutter'
_publ_contact_author_phone       '(33) 5 61 33 31 57'
_publ_section_title
;
 Preparation, Crystal Structures, and Magnetic Features for a Series of
 Dinuclear [NiIILnIII] Schiff-Base Complexes: Evidence for Slow Relaxation
 of the Magnetization for the DyIII Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5898
_journal_paper_doi               10.1021/ic2004276
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H26 N7 Ni O13 Sm, C2 H3 N, H2 O'
_chemical_formula_sum            'C25 H31 N8 Ni O14 Sm'
_chemical_formula_weight         876.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_audit_creation_date             08-03-18
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5639(5)
_cell_length_b                   14.7667(6)
_cell_length_c                   19.3364(9)
_cell_measurement_reflns_used    9264
_cell_measurement_temperature    295
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     3587.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            99802
_diffrn_reflns_theta_full        33.209
_diffrn_reflns_theta_max         34.957
_diffrn_reflns_theta_min         1.933
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.88
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_details 'Flack (1983), 6400 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.022(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000988
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.01 1.22 1.75 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0391
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0357
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                10376
_reflns_number_total             14487
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            ic2004276_si_004.cif
_cod_data_source_block           CRYSTALS_cif_cpd5
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C25 H31 N8 Ni1 O14 Sm1'
_cod_database_code               4325508