Octanuclear {Ln(III)8} (Ln = Gd, Tb, Dy, Ho) Macrocyclic Complexes in a Cyclooctadiene-like Conformation: Manifestation of Slow Relaxation of Magnetization in the Dy(III) Derivative
Vadapalli Chandrasekhar; Prasenjit Bag; Enrique Colacio; Inorganic Chemistry 52 (2013) 4562–4570; doi:10.1021/ic400091j

data_4334509
_publ_section_title
;
 Octanuclear {Ln(III)8} (Ln = Gd, Tb, Dy, Ho) Macrocyclic Complexes in a
 Cyclooctadiene-like Conformation: Manifestation of Slow Relaxation of
 Magnetization in the Dy(III) Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4562
_journal_page_last               4570
_journal_paper_doi               10.1021/ic400091j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C112 H192 Ho8 N16 O48'
_chemical_formula_weight         3850.26
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   18.183(3)
_cell_length_b                   18.183(3)
_cell_length_c                   44.626(9)
_cell_measurement_reflns_used    7047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.42
_cell_volume                     14754(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            41387
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    4.318
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.718030
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.095
_refine_diff_density_max         2.218
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7231
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0621P)^2^+211.9633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                5701
_reflns_number_total             7223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400091j_si_001_4.cif
_cod_data_source_block           Ho8
_cod_original_cell_volume        14755(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4334509