Magnetic Excitations in Polyoxotungstate-Supported Lanthanoid Single-Molecule Magnets: An Inelastic Neutron Scattering and ab Initio Study.
Vonci, Michele; Giansiracusa, Marcus J.; Van den Heuvel, Willem; Gable, Robert W.; Moubaraki, Boujemaa; Murray, Keith S.; Yu, Dehong; Mole, Richard A.; Soncini, Alessandro; Boskovic, Colette; Inorganic chemistry 56 (2017) 378–394; doi:10.1021/acs.inorgchem.6b02312

data_4345123
_publ_section_title
;
 Magnetic Excitations in Polyoxotungstate-Supported Lanthanoid
 Single-Molecule Magnets: An Inelastic Neutron Scattering and ab Initio
 Study.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              378
_journal_page_last               394
_journal_paper_doi               10.1021/acs.inorgchem.6b02312
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'Dy Na9 O68 W10, 3(O)'
_chemical_formula_sum            'Dy H70 Na9 O71 W10'
_chemical_formula_weight         3414.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                82.865(3)
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_cell_angle_gamma                88.920(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7318(6)
_cell_length_b                   13.0746(4)
_cell_length_c                   20.4722(8)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    90.00(10)
_cell_measurement_theta_max      74.9350
_cell_measurement_theta_min      3.5880
_cell_volume                     3257.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega    3.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907  -99.0000    0.0000 79

  2 omega   23.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907 -125.0000 -120.0000 63

  3 omega   14.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907  -57.0000 -150.0000 54

  4 omega   33.00  109.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -61.0000  -30.0000 76

  5 omega   75.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -94.0000   60.0000 29

  6 omega   93.00  129.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -77.0000  120.0000 36

  7 omega   71.00  142.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -45.0000   90.0000 71

  8 omega  123.00  159.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249   30.0000  -30.0000 36

  9 omega   61.00  104.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000  -60.0000 43

 10 omega   47.00  137.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -45.0000  -30.0000 90

 11 omega   74.00  113.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000 -180.0000 39

 12 omega   33.00  132.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -45.0000 -150.0000 99

 13 omega   48.00  115.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000    0.0000 67

 14 omega   27.00   80.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -77.0000  120.0000 53

 15 omega   25.00  178.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249    0.0000  -60.0000 153

 16 omega   30.00   56.00   1.0000    1.2900
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000 -180.0000 26

 17 omega  -36.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907  -57.0000 -150.0000 26

 18 omega -118.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -37.0000    0.0000 101

 19 omega  -59.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907   57.0000  150.0000 95

 20 omega -114.00  -83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000  150.0000 31

 21 omega -121.00  -85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000   90.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1111241000
_diffrn_orient_matrix_UB_12      0.0002930000
_diffrn_orient_matrix_UB_13      -0.0165722000
_diffrn_orient_matrix_UB_21      0.0430453000
_diffrn_orient_matrix_UB_22      -0.0771992000
_diffrn_orient_matrix_UB_23      -0.0517009000
_diffrn_orient_matrix_UB_31      -0.0396744000
_diffrn_orient_matrix_UB_32      -0.0902468000
_diffrn_orient_matrix_UB_33      0.0569852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.327
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    39.451
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.481
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3086
_exptl_crystal_size_max          0.1153
_exptl_crystal_size_mid          0.0572
_exptl_crystal_size_min          0.0152
_refine_diff_density_max         1.957
_refine_diff_density_min         -2.640
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         13019
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11331
_reflns_number_total             13019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02312_si_002.cif
_cod_data_source_block           DyW10a
_cod_database_code               4345123
_chemical_oxdiff_formula         'Dy1 W10 Na9 O71'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
;
_shelx_res_checksum              11583
_shelx_hkl_checksum              93004
_shelx_shelxl_version_number     2014/7