Family of Carboxylate- and Nitrate-diphenoxo Triply Bridged Dinuclear NiIILnIII Complexes (Ln = Eu, Gd, Tb, Ho, Er, Y): Synthesis, Experimental and Theoretical Magneto-Structural Studies, and Single-Molecule Magnet Behavior
Enrique Colacio; José Ruiz; Antonio J. Mota; María A. Palacios; Eduard Cremades; Eliseo Ruiz; Fraser J. White; Euan K. Brechin; Inorganic Chemistry 51 (2012) 5857–5868; doi:10.1021/ic3004596

data_4329242
_publ_section_title
;
 Family of Carboxylate- and Nitrate-diphenoxo Triply Bridged Dinuclear
 NiIILnIII Complexes (Ln = Eu, Gd, Tb, Ho, Er, Y): Synthesis, Experimental
 and Theoretical Magneto-Structural Studies, and Single-Molecule Magnet
 Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5857
_journal_page_last               5868
_journal_paper_doi               10.1021/ic3004596
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C27 H47 Eu N6 Ni O16'
_chemical_formula_weight         922.38
_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                 102.5480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6262(5)
_cell_length_b                   17.6724(9)
_cell_length_c                   20.0285(10)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.003
_cell_measurement_theta_min      2.2765
_cell_volume                     3671.3(3)
_computing_cell_refinement       'Bruker smart'
_computing_data_collection       'Bruker smart'
_computing_data_reduction        'Bruker smart'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19229
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.724844
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       Block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+8.6105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                5606
_reflns_number_total             6451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004596_si_001_09.cif
_cod_data_source_block           8a
_cod_database_code               4329242