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_4329240
_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         'C25 H37 N6 Ni O13 Tb, 2(C H4 O)'
_chemical_formula_sum            'C27 H45 N6 Ni O15 Tb'
_chemical_formula_weight         911.32
_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                 105.4273(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.58073(16)
_cell_length_b                   21.0969(3)
_cell_length_c                   16.4567(2)
_cell_measurement_reflns_used    26217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4550
_cell_measurement_theta_min      2.2134
_cell_volume                     3541.11(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega  -70.00  -26.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  128.0000  -66.0000 44

  2 omega    2.00   33.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -       12.1269   77.0000 -120.0000 31

  3 omega  -72.00   53.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -       12.1269    0.0000 -150.0000 125

  4 omega -100.00  -75.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  179.0000 -180.0000 25

  5 omega  -14.00   88.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -       12.1269   38.0000  -90.0000 102

  6 omega  -64.00   39.00   1.0000   19.6300
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -38.0000  120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40901
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            cyan
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8831
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+2.6449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                7786
_reflns_number_total             8831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004596_si_001_07.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329240