Ab initio calculations as a quantitative tool in the inelastic neutron scattering study of a single-molecule magnet analogue.
Vonci, Michele; Giansiracusa, Marcus J.; Gable, Robert W.; Van den Heuvel, Willem; Latham, Kay; Moubaraki, Boujemaa; Murray, Keith S.; Yu, Dehong; Mole, Richard A.; Soncini, Alessandro; Boskovic, Colette; Chemical communications (Cambridge, England) 52 (2016) 2091–2094; doi:10.1039/c5cc07541f

data_7118630
_publ_section_title
;
 Ab initio calculations as a quantitative tool in the inelastic neutron
 scattering study of a single-molecule magnet analogue.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2091
_journal_page_last               2094
_journal_paper_doi               10.1039/c5cc07541f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'Na9 O71.5 Tb W10, 0.5(O)'
_chemical_formula_sum            'H72 Na9 O72 Tb W10'
_chemical_formula_weight         3428.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                76.956(3)
_cell_angle_beta                 83.954(3)
_cell_angle_gamma                77.348(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8949(5)
_cell_length_b                   13.1098(5)
_cell_length_c                   20.9057(7)
_cell_measurement_reflns_used    9545
_cell_measurement_temperature    131.10(10)
_cell_measurement_theta_max      71.2540
_cell_measurement_theta_min      3.4960
_cell_volume                     3353.5(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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      131.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega   28.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000  -30.0000 43

  2 omega   28.00   58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000 -120.0000 30

  3 omega   41.00  133.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -61.0000  -30.0000 92

  4 omega   66.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -30.0000    0.0000 25

  5 omega   74.00  173.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966   45.0000   60.0000 99

  6 omega  135.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  111.0000  -30.0000 41

  7 omega  123.00  149.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  178.0000 -150.0000 26

  8 omega   94.00  138.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  178.0000 -120.0000 44

  9 omega   74.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966   45.0000    0.0000 104

 10 omega  115.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966   45.0000  -60.0000 62

 11 omega   65.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -30.0000  150.0000 26

 12 omega   27.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -30.0000   60.0000 49

 13 omega   26.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -94.0000  -30.0000 82

 14 omega   58.00   85.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -30.0000 -150.0000 27

 15 omega   29.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966  -94.0000  -90.0000 62

 16 omega   27.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0966 -111.0000 -150.0000 88

 17 omega   28.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4657 -125.0000   60.0000 35

 18 omega  -96.00  -27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657  125.0000   60.0000 69

 19 omega -130.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4657    0.0000   30.0000 183
;
_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      -0.0041509000
_diffrn_orient_matrix_UB_12      0.1062301000
_diffrn_orient_matrix_UB_13      -0.0505259000
_diffrn_orient_matrix_UB_21      0.0974229000
_diffrn_orient_matrix_UB_22      0.0186708000
_diffrn_orient_matrix_UB_23      0.0291666000
_diffrn_orient_matrix_UB_31      0.0744045000
_diffrn_orient_matrix_UB_32      -0.0594378000
_diffrn_orient_matrix_UB_33      -0.0483541000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22609
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.499
_diffrn_reflns_theta_min         3.519
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    37.561
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.134
_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    3.396
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.1477
_exptl_crystal_size_mid          0.0402
_exptl_crystal_size_min          0.0344
_refine_diff_density_max         4.488
_refine_diff_density_min         -2.607
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         12708
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10916
_reflns_number_total             12708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07541f2.cif
_cod_data_source_block           mv_2_38Tb_B
_cod_database_code               7118630
_chemical_oxdiff_formula         'W10 O72 Tb1 Na9 H72'
_cell_oxdiff_angle_alpha         76.956(3)
_cell_oxdiff_angle_beta          83.954(3)
_cell_oxdiff_angle_gamma         77.348(3)
_cell_oxdiff_length_a            12.8949(5)
_cell_oxdiff_length_b            13.1098(5)
_cell_oxdiff_length_c            20.9057(7)
_cell_oxdiff_measurement_reflns_used 9545
_cell_oxdiff_volume              3353.5(2)
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Others
 1*[Sof(Na2)]+1*[Sof(Na1)]+1*[Sof(Na15)]+1*[Sof(Na14)]+1*[Sof(Na4)]+1*
 [Sof(Na3)]=1.5 with esd of 0.001
 Sof(Na5)=1-FVAR(1)
 Sof(Na6)=FVAR(1)
 Sof(O40)=1-FVAR(6)
 Sof(O41)=FVAR(6)
 Sof(O62)=1-FVAR(7)
 Sof(O63)=FVAR(7)
 Fixed Sof: O76(0.5) O67(0.5) O69(0.5) O72(0.5) O71(0.5) O68(0.5) O70(0.5)
 O74(0.5)
;
_shelx_res_checksum              53409
_shelx_hkl_checksum              31146
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'