A Tetranuclear, Macrocyclic 3d-4f Complex Showing Single-Molecule Magnet Behavior
Humphrey L. C. Feltham; Rodolphe Clérac; Annie K. Powell; Sally Brooker; Inorganic Chemistry 50 (2011) 4232–4234; doi:10.1021/ic2003639

data_4325105
_publ_section_title
;
 A Tetranuclear, Macrocyclic 3d-4f Complex Showing Single-Molecule Magnet
 Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4232
_journal_page_last               4234
_journal_paper_doi               10.1021/ic2003639
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C36 H42 Cu3 N9 O18 Tb'
_chemical_formula_weight         1238.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.687(12)
_cell_angle_beta                 96.526(12)
_cell_angle_gamma                109.584(9)
_cell_formula_units_Z            2
_cell_length_a                   12.286(2)
_cell_length_b                   13.379(3)
_cell_length_c                   14.819(5)
_cell_measurement_reflns_used    4522
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.044
_cell_measurement_theta_min      2.645
_cell_volume                     2089.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker Kappa Apex II area detector'
_diffrn_measurement_method       '\f and \w 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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26932
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    3.269
_exptl_absorpt_correction_T_max  0.8536
_exptl_absorpt_correction_T_min  0.3547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.085
_refine_diff_density_min         -2.994
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7869
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0671P)^2^+31.3761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2134
_reflns_number_gt                4938
_reflns_number_total             7869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003639_si_001.cif
_cod_data_source_block           hf451
_cod_original_cell_volume        2089.1(9)
_cod_database_code               4325105