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_4302434
_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 Ho1 N15 Ni1 O9 W1'
_chemical_formula_sum            'C44 H59 Ho N15 Ni O9 W'
_chemical_formula_weight         1349.54
_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                 106.4670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0236(4)
_cell_length_b                   26.0618(8)
_cell_length_c                   19.6674(6)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     5910.1(3)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.047
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            70157
_diffrn_reflns_theta_full        27.019
_diffrn_reflns_theta_max         28.743
_diffrn_reflns_theta_min         1.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.641
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Blessing, acta cryst. (1995), a51, 33-38
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         10836
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001176
_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: 
 0.980 -0.979E-01 0.714 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0371
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0315
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11706
_reflns_number_total             15205
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0333
_oxford_reflns_number_all        15158
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic900003m_si_006.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        'C44 H59 Ho1 N15 Ni1 O9 W1'
_cod_database_code               4302434