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_4347395
_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 Dy3 Na11 O103.52 P2 W18, 8.55(O1.46)'
_chemical_formula_sum            'C H84 Dy3 Na11 O116 P2 W18'
_chemical_formula_weight         6064.31
_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             2015-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.38612(11)
_cell_length_b                   26.04781(13)
_cell_length_c                   23.41801(14)
_cell_measurement_reflns_used    36003
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      74.5550
_cell_measurement_theta_min      3.2070
_cell_volume                     9857.69(11)
_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  -36.00   25.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592   37.0000  -60.0000 61

  2 omega  -53.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592  125.0000   60.0000 36

  3 omega   31.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0592 -125.0000 -120.0000 67

  4 omega   40.00   93.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -45.0000 -120.0000 53

  5 omega   97.00  133.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -61.0000  -60.0000 36

  6 omega   76.00  115.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393 -111.0000   30.0000 39

  7 omega   65.00  142.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -77.0000   60.0000 77

  8 omega   78.00  178.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393   30.0000  -60.0000 100

  9 omega  102.00  167.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  111.0000 -150.0000 65

 10 omega   82.00  177.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393   61.0000 -180.0000 95

 11 omega   54.00   90.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000   30.0000 36

 12 omega   62.00   88.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000   60.0000 26

 13 omega   42.00   90.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000  150.0000 48

 14 omega   32.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0592 -125.0000   60.0000 50

 15 omega   33.00   88.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -45.0000  -60.0000 55

 16 omega   29.00  109.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -94.0000 -120.0000 80

 17 omega   87.00  112.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393 -111.0000 -180.0000 25

 18 omega  111.00  142.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  178.0000   90.0000 31

 19 omega   63.00   88.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  178.0000   90.0000 25

 20 omega -110.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592    0.0000  -90.0000 147
;
_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      0.0018484000
_diffrn_orient_matrix_UB_12      -0.0398433000
_diffrn_orient_matrix_UB_13      -0.0331666000
_diffrn_orient_matrix_UB_21      -0.0188021000
_diffrn_orient_matrix_UB_22      -0.0405153000
_diffrn_orient_matrix_UB_23      0.0240401000
_diffrn_orient_matrix_UB_31      -0.0419637000
_diffrn_orient_matrix_UB_32      0.0164338000
_diffrn_orient_matrix_UB_33      -0.0212743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0377
_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       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68519
_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         74.845
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    51.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57040
_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_density_diffrn    4.086
_exptl_crystal_description       'hexagonal-faced rod'
_exptl_crystal_F_000             10796
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.980
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         19888
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0440P)^2^+54.9948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18153
_reflns_number_total             19888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00108_si_002.cif
_cod_data_source_block           mg1dysp
_cod_original_cell_volume        9857.68(11)
_cod_database_code               4347395
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_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
Uiso(O90) = Uiso(O90A)
Uanis(O91) = Uanis(O91A)
Uanis(O92) = Uanis(O92A)
Uanis(O93) = Uanis(O93A)
Uiso(O95) = Uiso(O95A)
Uanis(Na9) = Uanis(Na9A)
Uanis(Na8) = Uanis(Na8A)
2. Others
 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(O95A)=1-FVAR(5)
 Sof(O95)=FVAR(5)
 Sof(Na9A)=1-FVAR(6)
 Sof(Na9)=FVAR(6)
 Sof(Na8A)=1-FVAR(7)
 Sof(Na8)=FVAR(7)
 Sof(O107)=1-FVAR(8)
 Sof(O89)=FVAR(8)
;
_shelx_res_checksum              60023
_shelx_hkl_checksum              51113
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'