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_4336727
_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            'C79 H98 Cl Gd3 N8 Ni2 O20'
_chemical_formula_weight         2104.27
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0447(9)
_cell_length_b                   26.2289(19)
_cell_length_c                   22.8835(17)
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.69
_cell_measurement_theta_min      2.20
_cell_volume                     7829.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1010
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42948
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.705415
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.678
_refine_diff_density_min         -3.601
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.032(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         14537
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                10336
_reflns_number_total             14537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019025_si_001_2.cif
_cod_data_source_block           Ni2Gd3
_cod_database_code               4336727