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_4329243
_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         'C32 H42 Dy N5 Ni O12, C H4 O'
_chemical_formula_sum            'C33 H46 Dy N5 Ni O13'
_chemical_formula_weight         941.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.876(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1285(3)
_cell_length_b                   22.2252(6)
_cell_length_c                   14.8845(4)
_cell_measurement_reflns_used    15475
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5798
_cell_measurement_theta_min      2.3298
_cell_volume                     3796.47(19)
_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 Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_details
;
  1 omega  -60.00  -33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  114.0000 -138.0000 27

  2 omega  -61.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -77.0000   90.0000 64

  3 omega   14.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269   38.0000   60.0000 51

  4 omega  -49.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -77.0000  -90.0000 75

  5 omega  -87.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -38.0000 -180.0000 102

  6 omega  -28.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332   38.0000  150.0000 65

  7 omega  -73.00  -27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  132.0000    7.0000 46

;
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43779
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87307
_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            turquiose
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_recrystallization_method
'Crashed out of reaction mixture, MeOH solution'
_exptl_crystal_size_max          0.1662
_exptl_crystal_size_mid          0.1007
_exptl_crystal_size_min          0.0613
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9686
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                6960
_reflns_number_total             9686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004596_si_001_10.cif
_cod_data_source_block           9
_cod_original_cell_volume        3796.47(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4329243