Strategy for the Rational Design of Asymmetric Triply Bridged Dinuclear 3d-4f Single-Molecule Magnets.
Enrique Colacio; José Ruiz-Sanchez; Fraser J. White; Euan K. Brechin; Inorganic Chemistry 50 (2011) 7268–7273; doi:10.1021/ic2008599

data_4325816
_publ_contact_author_email       fraser.white@ed.ac.uk
_publ_contact_author_name        'Fraser J. White'
_publ_section_title
;
 Strategy for the Rational Design of Asymmetric Triply Bridged Dinuclear
 3d-4f Single-Molecule Magnets.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7268
_journal_page_last               7273
_journal_paper_doi               10.1021/ic2008599
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'Enrique Colacio'
_chemical_formula_moiety         'C27 H40 Dy N5 O12 Zn'
_chemical_formula_sum            'C27 H40 Dy N5 O12 Zn'
_chemical_formula_weight         854.51
_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                92.6188(11)
_cell_angle_beta                 98.4920(11)
_cell_angle_gamma                90.9853(11)
_cell_formula_units_Z            4
_cell_length_a                   11.44727(16)
_cell_length_b                   14.7621(2)
_cell_length_c                   19.3317(3)
_cell_measurement_reflns_used    46365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5669
_cell_measurement_theta_min      2.2194
_cell_volume                     3226.64(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.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
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CrysAlisPro, Oxford Diffraction Ltd.,
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_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
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_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
  1 omega  -24.00    2.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -77.0000  -30.0000 26

  2 omega  -19.00   87.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269   77.0000  -60.0000 106

  3 omega  -14.00   87.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269   38.0000 -150.0000 101

  4 omega  -59.00   43.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -77.0000   60.0000 102

  5 omega  -87.00   15.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -38.0000    0.0000 102

  6 omega  -68.00  -22.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  124.0000  -85.0000 46

  7 omega  -22.00   66.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269   77.0000    0.0000 88

  8 omega  -67.00   46.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269  -77.0000  -60.0000 113

  9 omega   34.00  102.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269  179.0000 -180.0000 68

 10 omega   34.00  102.00   1.0000   11.6100
omega____ theta____ kappa____ phi______ frames
    -       12.1269  179.0000  -90.0000 68

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72203
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93806
_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.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH solution'
_exptl_crystal_size_max          0.2394
_exptl_crystal_size_mid          0.1998
_exptl_crystal_size_min          0.1444
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         16339
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0332P)^2^+0.0882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                14232
_reflns_number_total             16339
_reflns_threshold_expression     >2sigma(I)
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