Carbonate-Bridged Lanthanoid Triangles: Single-Molecule Magnet Behavior, Inelastic Neutron Scattering, and Ab Initio Studies.
Giansiracusa, Marcus J.; Vonci, Michele; Van den Heuvel, Willem; Gable, Robert W.; Moubaraki, Boujemaa; Murray, Keith S.; Yu, Dehong; Mole, Richard A.; Soncini, Alessandro; Boskovic, Colette; Inorganic chemistry 55 (2016) 5201–5214; doi:10.1021/acs.inorgchem.6b00108

data_4347394
_publ_section_title
;
 Carbonate-Bridged Lanthanoid Triangles: Single-Molecule Magnet Behavior,
 Inelastic Neutron Scattering, and Ab Initio Studies.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5201
_journal_page_last               5214
_journal_paper_doi               10.1021/acs.inorgchem.6b00108
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C Na11 O104.25 P2 Tb3 W18, 10.63(O)'
_chemical_formula_sum            'C H84 Na11 O116 P2 Tb3 W18'
_chemical_formula_weight         6053.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_creation_date             2015-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.6016(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.38631(15)
_cell_length_b                   26.04125(18)
_cell_length_c                   23.4293(2)
_cell_measurement_reflns_used    23422
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      73.4620
_cell_measurement_theta_min      3.9240
_cell_volume                     9862.85(15)
_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, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(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 0.982
_diffrn_measurement_details
;
  1 omega  -44.00   12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.1173   37.0000  -90.0000 56

  2 omega  -31.00   10.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.1173   37.0000   90.0000 41

  3 omega   32.00   84.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.1173 -125.0000   30.0000 52

  4 omega   31.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -77.0000  -60.0000 96

  5 omega   94.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158 -125.0000   60.0000 28

  6 omega   51.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -94.0000  -90.0000 46

  7 omega   34.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       42.1173 -125.0000 -150.0000 49

  8 omega   29.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -94.0000 -150.0000 73

  9 omega   29.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -30.0000  -60.0000 54

 10 omega   54.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158   15.0000    0.0000 84

 11 omega   76.00  166.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158   30.0000 -150.0000 90

 12 omega   94.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  125.0000 -150.0000 81

 13 omega   28.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -30.0000    0.0000 40

 14 omega   30.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -30.0000   60.0000 57

 15 omega   47.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -94.0000  150.0000 50

 16 omega   28.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.6158  -30.0000 -180.0000 61

 17 omega -117.00   24.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.1173    0.0000 -120.0000 141
;
_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      -0.0152321000
_diffrn_orient_matrix_UB_12      0.0425053000
_diffrn_orient_matrix_UB_13      -0.0486833000
_diffrn_orient_matrix_UB_21      -0.0638367000
_diffrn_orient_matrix_UB_22      -0.0344873000
_diffrn_orient_matrix_UB_23      -0.0477136000
_diffrn_orient_matrix_UB_31      -0.0690713000
_diffrn_orient_matrix_UB_32      0.0224865000
_diffrn_orient_matrix_UB_33      0.0188637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.630
_diffrn_reflns_theta_min         3.955
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    50.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47886
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.077
_exptl_crystal_description       'Hexagonal faceted rod'
_exptl_crystal_F_000             10784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.623
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1346
_refine_ls_number_reflns         19554
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+21.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17245
_reflns_number_total             19554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00108_si_002.cif
_cod_data_source_block           mjg1_138_tb_abs
_cod_original_cell_volume        9862.84(15)
_cod_database_code               4347394
_chemical_oxdiff_formula         'Tb3 W18 O74 P2 Na11'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O26) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(W3A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(O90) = Uiso(O90A) = Uiso(O89)
Uanis(O91) = Uanis(O91A)
Uanis(O92) = Uanis(O92A)
Uanis(O93) = Uanis(O93A)
Uanis(Na8) = Uanis(Na8A)
Uanis(Na9) = Uanis(O9A)
2. Others
 1*[Sof(Na8)]+1*[Sof(Na8A)]+1*[Sof(Na9)]+1*[Sof(Na1)]=2 with esd of 0.001
 1*[Sof(Na8)]+1*[Sof(Na9)]=1 with esd of 0.001
 1*[Sof(O121)]+1*[Sof(O107)]+1*[Sof(O9A)]+1*[Sof(O89)]=2 with esd of 0.001
 Sof(O90A)=1-FVAR(1)
 Sof(O90)=FVAR(1)
 Sof(O91A)=1-FVAR(2)
 Sof(O91)=FVAR(2)
 Sof(O92A)=1-FVAR(3)
 Sof(O92)=FVAR(3)
 Sof(O93A)=1-FVAR(4)
 Sof(O93)=FVAR(4)
 Sof(W1A)=Sof(W2A)=Sof(W3A)=1-FVAR(6)
 Sof(W1)=Sof(W2)=Sof(W3)=Sof(O70)=Sof(O72)=Sof(O74)=FVAR(6)
;
_shelx_res_checksum              14704
_shelx_hkl_checksum              73019
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'