Pentanuclear Heterometallic {Ni2Ln3} (Ln = Gd, Dy, Tb, Ho) Assemblies. Single-Molecule Magnet Behavior and Multistep Relaxation in the Dysprosium Derivative
Vadapalli Chandrasekhar; Prasenjit Bag; Wolfgang Kroener; Klaus Gieb; Paul Müller; Inorganic Chemistry 52 (2013) 13078–13086; doi:10.1021/ic4019025

data_4336728
_publ_section_title
;
 Pentanuclear Heterometallic {Ni2Ln3} (Ln = Gd, Dy, Tb, Ho) Assemblies.
 Single-Molecule Magnet Behavior and Multistep Relaxation in the
 Dysprosium Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13078
_journal_page_last               13086
_journal_paper_doi               10.1021/ic4019025
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C78 H92 Cl5 N8 Ni2 O18 Tb3'
_chemical_formula_weight         2201.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.198(3)
_cell_length_b                   26.420(5)
_cell_length_c                   23.571(5)
_cell_measurement_reflns_used    4005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.32
_cell_volume                     8219(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_sigmaI/netI    0.1370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43569
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    3.233
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.576264
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.295
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         15220
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+216.8225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2408
_reflns_number_gt                9235
_reflns_number_total             15220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019025_si_001_3.cif
_cod_data_source_block           Ni2Tb3
_cod_database_code               4336728