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_4302431
_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_formula_moiety         'C44 H59 N15 Ni O9 Tb W, 0.5(C3 H7 N O) '
_chemical_formula_sum            'C45.5 H62.5 N15.5 Ni O9.5 Tb W'
_chemical_formula_weight         1380.08
_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
_cell_angle_alpha                90
_cell_angle_beta                 106.362(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9038(10)
_cell_length_b                   25.841(2)
_cell_length_c                   19.8029(15)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    180
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     5844.8(8)
_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      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Apex2'
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54522
_diffrn_reflns_theta_full        26.254
_diffrn_reflns_theta_max         26.254
_diffrn_reflns_theta_min         1.330
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.541
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2748
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         8312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001353
_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: 
 0.859 -0.114 0.510 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0431
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0321
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8977
_reflns_number_total             11775
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0316
_oxford_reflns_number_all        11730
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic900003m_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C45.50 H62.5 N15.50 Ni1 O9.50 Tb1 W1'
_cod_database_code               4302431