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_4325511
_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_formula_moiety
'C23 H28 Ce N7 Ni O14,C21 H29 CeN5NiO13,2(C2H3N),NO3 '
_chemical_formula_sum            'C48 H63 Ce2 N15 Ni2 O30'
_chemical_formula_weight         1727.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             09-07-15
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90.983(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9538(6)
_cell_length_b                   11.3152(4)
_cell_length_c                   32.2403(11)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    180
_cell_measurement_theta_max      35
_cell_measurement_theta_min      3
_cell_volume                     6548.7(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_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  0.035
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            100925
_diffrn_reflns_theta_full        32.010
_diffrn_reflns_theta_max         35.567
_diffrn_reflns_theta_min         1.683
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.028
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.12
_refine_diff_density_min         -1.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         20002
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.003213
_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: 
 0.844 0.354 0.629 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0448
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0381
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              52
_reflns_limit_l_min              0
_reflns_number_gt                21892
_reflns_number_total             28044
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0429
_oxford_reflns_number_all        27991
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'cpd 2 - jps0916'
_cod_data_source_file            ic2004276_si_007.cif
_cod_data_source_block           cpd2
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4325511