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_4345124
_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         'Ho Na9 O68 W10, 3(O)'
_chemical_formula_sum            'H70 Ho Na9 O71 W10'
_chemical_formula_weight         3416.90
_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             2015-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
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_cell_formula_units_Z            2
_cell_length_a                   12.7217(5)
_cell_length_b                   13.0494(5)
_cell_length_c                   20.4707(7)
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    90.00(10)
_cell_measurement_theta_max      74.8330
_cell_measurement_theta_min      3.4090
_cell_volume                     3249.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_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 0.971
_diffrn_measurement_details
;
  1 omega    7.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907  -99.0000    0.0000 48

  2 omega   25.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5907 -125.0000  120.0000 63

  3 omega   31.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000   30.0000 73

  4 omega   44.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000   90.0000 97

  5 omega  118.00  159.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   45.0000  150.0000 41

  6 omega  121.00  172.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  111.0000   60.0000 51

  7 omega  134.00  172.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   45.0000   60.0000 38

  8 omega  100.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  111.0000   90.0000 78

  9 omega  101.00  148.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  111.0000  150.0000 47

 10 omega   82.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   45.0000  150.0000 31

 11 omega   81.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   45.0000   60.0000 28

 12 omega   33.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   15.0000  150.0000 81

 13 omega   36.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000   90.0000 79

 14 omega   27.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -77.0000   90.0000 118

 15 omega   73.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000  -90.0000 42

 16 omega   35.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000  -90.0000 26

 17 omega   35.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -94.0000  -90.0000 36

 18 omega  -63.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907   37.0000 -150.0000 104

 19 omega  -93.00  -29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  125.0000 -150.0000 64

 20 omega -123.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000 -180.0000 36

 21 omega -118.00  -83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000  -90.0000 35

 22 omega -123.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000  -30.0000 44

 23 omega -124.00  -99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000 -120.0000 25

 24 omega -123.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5907  -99.0000  120.0000 44
;
_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      0.0632075000
_diffrn_orient_matrix_UB_12      0.1036744000
_diffrn_orient_matrix_UB_13      -0.0195546000
_diffrn_orient_matrix_UB_21      0.0270353000
_diffrn_orient_matrix_UB_22      -0.0159584000
_diffrn_orient_matrix_UB_23      -0.0759742000
_diffrn_orient_matrix_UB_31      -0.1051893000
_diffrn_orient_matrix_UB_32      0.0562043000
_diffrn_orient_matrix_UB_33      -0.0062326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23042
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.158
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    35.676
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    3.493
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.5701
_exptl_crystal_size_mid          0.1036
_exptl_crystal_size_min          0.0067
_refine_diff_density_max         2.242
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         13010
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10964
_reflns_number_total             13010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02312_si_002.cif
_cod_data_source_block           HoW10a
_cod_database_code               4345124
_chemical_oxdiff_formula         'W10 Ho1 Na9 O73 H74'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O31) \\sim Ueq: with sigma of 0.0002 and sigma for terminal atoms of 0.024
;
_shelx_res_checksum              79660
_shelx_hkl_checksum              29296
_shelx_shelxl_version_number     2014/7