Nickel/Lanthanide Single-Molecule Magnets: {Ni3Ln} "Stars" with a Ligand Derived from the Metal-Promoted Reduction of Di-2-pyridyl Ketone under Solvothermal Conditions
Constantinos G. Efthymiou; Theocharis C. Stamatatos; Constantina Papatriantafyllopoulou; Anastasios J. Tasiopoulos; Wolfgang Wernsdorfer; Spyros P. Perlepes; George Christou; Inorganic Chemistry 49 (2010) 9737–9739; doi:10.1021/ic101504c

data_4316979
_publ_section_title
;
 Nickel/Lanthanide Single-Molecule Magnets: {Ni3Ln} "Stars" with a Ligand
 Derived from the Metal-Promoted Reduction of Di-2-pyridyl Ketone under
 Solvothermal Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9737
_journal_page_last               9739
_journal_paper_doi               10.1021/ic101504c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C66 H54 Gd N12 Ni3 O6 , 3(Cl O4)'
_chemical_formula_sum            'C66 H54 Cl3 Gd N12 Ni3 O18'
_chemical_formula_weight         1742.94
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.145(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.746(2)
_cell_length_b                   20.820(3)
_cell_length_c                   23.728(4)
_cell_measurement_reflns_used    18412
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4112
_cell_measurement_theta_min      3.0552
_cell_volume                     7121.7(19)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics
'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)'
_computing_publication_material  'WINGX (Farrugia, 1999'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method       '\w/\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27889
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.8400
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_crystal_colour            light-pink
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3508
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7753
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                6432
_reflns_number_total             7753
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic101504c_si_001_1.cif
_cod_data_source_block           de268-Gd
_cod_original_cell_volume        7121.7(18)
_cod_database_code               4316979