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_4345121
_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         '9(Na), Nd O67 W10, 3.5(O)'
_chemical_formula_sum            'H69 Na9 Nd O70.5 W10'
_chemical_formula_weight         3387.20
_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             2016-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                113.503(2)
_cell_angle_beta                 97.778(2)
_cell_angle_gamma                90.3643(19)
_cell_formula_units_Z            4
_cell_length_a                   18.2697(5)
_cell_length_b                   18.4818(4)
_cell_length_c                   20.8278(6)
_cell_measurement_reflns_used    17209
_cell_measurement_temperature    90.00(10)
_cell_measurement_theta_max      74.8220
_cell_measurement_theta_min      3.4380
_cell_volume                     6375.8(3)
_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 0.968
_diffrn_measurement_details
;
  1 omega  -47.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657   37.0000  -90.0000 82

  2 omega    3.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657   37.0000 -180.0000 37

  3 omega  -12.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657  -57.0000  -90.0000 83

  4 omega   39.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000  -90.0000 34

  5 omega   41.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000 -180.0000 45

  6 omega   31.00   89.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000 -150.0000 58

  7 omega  136.00  174.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249   45.0000  -60.0000 38

  8 omega   64.00  177.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -15.0000  120.0000 113

  9 omega   90.00  115.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000  -60.0000 25

 10 omega   61.00   86.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -45.0000    0.0000 25

 11 omega   56.00  102.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -94.0000   30.0000 46

 12 omega   60.00  113.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000  120.0000 53

 13 omega   50.00   82.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000    0.0000 32

 14 omega   30.00   83.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000  -30.0000 53

 15 omega   30.00   91.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000  -90.0000 61

 16 omega   39.00  134.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -77.0000 -150.0000 95

 17 omega   50.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000   30.0000 43

 18 omega   45.00   71.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -94.0000  150.0000 26

 19 omega   34.00   87.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -45.0000   60.0000 53

 20 omega   32.00   58.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -30.0000  150.0000 26

 21 omega   29.00   56.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -15.0000  120.0000 27

 22 omega   31.00   91.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249 -111.0000   30.0000 60

 23 omega   36.00  106.00   1.0000    2.1000
omega____ theta____ kappa____ phi______ frames
    -      111.4249  -94.0000 -180.0000 70

 24 omega  -43.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657   37.0000  150.0000 81

 25 omega  -98.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657  -37.0000    0.0000 77
;
_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      0.0779164000
_diffrn_orient_matrix_UB_12      -0.0257289000
_diffrn_orient_matrix_UB_13      0.0162313000
_diffrn_orient_matrix_UB_21      -0.0263236000
_diffrn_orient_matrix_UB_22      -0.0234392000
_diffrn_orient_matrix_UB_23      0.0567113000
_diffrn_orient_matrix_UB_31      -0.0226122000
_diffrn_orient_matrix_UB_32      -0.0841865000
_diffrn_orient_matrix_UB_33      -0.0563605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.226
_diffrn_reflns_theta_min         3.121
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    40.248
_exptl_absorpt_correction_T_max  0.250
_exptl_absorpt_correction_T_min  0.034
_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    3.529
_exptl_crystal_description
;
;
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.1759
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_exptl_crystal_size_min          0.0765
_refine_diff_density_max         3.568
_refine_diff_density_min         -2.726
_refine_diff_density_rms         0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1630
_refine_ls_number_reflns         25518
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21977
_reflns_number_total             25518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02312_si_002.cif
_cod_data_source_block           Nd2W20
_cod_depositor_comments
;

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H138 Na18 Nd2 O141 W20'
_cod_original_formula_weight         6774.40
_cod_original_formula_moiety         'Na18 Nd2 O134 W20, 7(O)'
_cod_original_formula_units_Z            2
_cod_database_code               4345121
_chemical_oxdiff_formula         'Nd1 W10 O71 Na9'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.026
Uanis(O20') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.026
Uanis(O35') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.026
;
_shelx_res_checksum              57398
_shelx_hkl_checksum              37816
_shelx_shelxl_version_number     2014/7