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_4329234
_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
;
;
_chemical_formula_moiety         'C27 H40 Gd N5 Ni O12'
_chemical_formula_sum            'C27 H40 Gd N5 Ni O12'
_chemical_formula_weight         842.60
_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                92.4072(12)
_cell_angle_beta                 98.2605(12)
_cell_angle_gamma                91.0646(11)
_cell_formula_units_Z            4
_cell_length_a                   11.42261(15)
_cell_length_b                   14.71446(19)
_cell_length_c                   19.4020(3)
_cell_measurement_reflns_used    43399
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4663
_cell_measurement_theta_min      2.2156
_cell_volume                     3223.36(8)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
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_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 0.999
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
  1 omega  -67.00  -31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  125.0000   26.0000 36

  2 omega  -24.00   15.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -38.0000   60.0000 39

  3 omega  -98.00  -59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  179.0000  150.0000 39

  4 omega  -65.00  -38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -38.0000   60.0000 27

  5 omega  -22.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269   77.0000  -30.0000 87

  6 omega  -72.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269    0.0000  150.0000 172

  7 omega  -87.00  -41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -38.0000 -180.0000 46

  8 omega  -90.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -77.0000  -30.0000 113

  9 omega  -67.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -77.0000  -90.0000 113

 10 omega   34.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  179.0000 -120.0000 68

 11 omega  -64.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -38.0000    0.0000 103

;
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_measurement_method       '\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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
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empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH solution'
_exptl_crystal_size_max          0.1700
_exptl_crystal_size_mid          0.1628
_exptl_crystal_size_min          0.1204
_refine_diff_density_max         2.693
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         16355
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.7699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                13592
_reflns_number_total             16355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004596_si_001_01.cif
_cod_data_source_block           1
_cod_original_cell_volume        3223.37(8)
_cod_database_code               4329234