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_4329236
_publ_contact_author_email       fraser.white@ed.ac.uk
_publ_contact_author_name        'Fraser J. White'
_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_compound_source        'Enrique Colacio'
_chemical_formula_moiety         'C27 H40 N5 Ni O12 Tb'
_chemical_formula_sum            'C27 H40 N5 Ni O12 Tb'
_chemical_formula_weight         844.27
_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                92.451(6)
_cell_angle_beta                 98.325(6)
_cell_angle_gamma                91.234(6)
_cell_formula_units_Z            4
_cell_length_a                   11.4079(13)
_cell_length_b                   14.7065(17)
_cell_length_c                   19.389(2)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.396
_cell_measurement_theta_min      2.3975
_cell_volume                     3214.4(6)
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Apex II CCD on D8'
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41847
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            cyan
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH solution'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         13106
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0250P)^2^+0.1972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                10803
_reflns_number_total             13106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004596_si_001_03.cif
_cod_data_source_block           2
_cod_database_code               4329236