Fine-Tuning the Single-Molecule Magnet Properties of a [Dy(III)-Radical]2 Pair
Elisabeth M. Fatila; Mathieu Rouzières; Michael C. Jennings; Alan J. Lough; Rodolphe Clérac; Kathryn E. Preuss; Journal of the American Chemical Society 135 (2013) 9596–9599; doi:10.1021/ja403794d

data_4120031
_publ_section_title
;
 Fine-Tuning the Single-Molecule Magnet Properties of a [Dy(III)-Radical]2
 Pair
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9596
_journal_page_last               9599
_journal_paper_doi               10.1021/ja403794d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C23 H7 Dy F18 N3 O7 S2'
_chemical_formula_sum            'C23 H7 Dy F18 N3 O7 S2'
_chemical_formula_weight         1005.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.733(3)
_cell_length_b                   28.590(6)
_cell_length_c                   15.682(3)
_cell_measurement_reflns_used    87154
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     6606(2)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.1065
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            81622
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.782
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         11666
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1175P)^2^+21.1616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.2072
_reflns_number_gt                7426
_reflns_number_total             11666
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja403794d_si_002.cif
_cod_data_source_block           k11119m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4120031