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_4347396
_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 Ho3 Na11 O104.16 P2 W18, 9.84(O)'
_chemical_formula_sum            'C H84 Ho3 Na11 O116 P2 W18'
_chemical_formula_weight         6071.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-15
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_length_b                   25.97724(15)
_cell_length_c                   23.3379(2)
_cell_measurement_reflns_used    36944
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      74.6030
_cell_measurement_theta_min      3.9420
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_diffrn_detector_area_resol_mean 10.2273
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_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega -120.00   -9.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592  -77.0000  120.0000 111

  2 omega  -58.00  -12.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592  -57.0000    0.0000 46

  3 omega -107.00  -20.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592  -57.0000 -180.0000 87

  4 omega  -93.00  -22.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0592  125.0000 -120.0000 71

  5 omega  -22.00    8.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000   90.0000 30

  6 omega -132.00  -79.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000 -150.0000 53

  7 omega   35.00  114.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393 -111.0000  120.0000 79

  8 omega   48.00   74.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -45.0000  -30.0000 26

  9 omega   87.00  134.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -77.0000  150.0000 47

 10 omega   49.00   99.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -45.0000   60.0000 50

 11 omega   30.00   88.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000  150.0000 58

 12 omega   56.00   89.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000 -180.0000 33

 13 omega   49.00  107.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393 -111.0000  -30.0000 58

 14 omega   25.00  109.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -94.0000 -180.0000 84

 15 omega   44.00   87.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000  -60.0000 43

 16 omega   77.00  177.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393   30.0000  -30.0000 100

 17 omega   25.00  102.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -94.0000    0.0000 77

 18 omega  136.00  175.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  111.0000 -180.0000 39

 19 omega   26.00  117.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -15.0000  -30.0000 91
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0465527000
_diffrn_orient_matrix_UB_12      0.0475437000
_diffrn_orient_matrix_UB_13      -0.0355166000
_diffrn_orient_matrix_UB_21      -0.0247873000
_diffrn_orient_matrix_UB_22      -0.0303277000
_diffrn_orient_matrix_UB_23      -0.0608262000
_diffrn_orient_matrix_UB_31      -0.0797222000
_diffrn_orient_matrix_UB_32      -0.0183471000
_diffrn_orient_matrix_UB_33      0.0084948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.645
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    44.350
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            yellow-pink
_exptl_crystal_density_diffrn    4.128
_exptl_crystal_description       'Hexagonal-faced Rods'
_exptl_crystal_F_000             10808
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.0404
_exptl_crystal_size_min          0.0331
_refine_diff_density_max         1.940
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         19743
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+49.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18625
_reflns_number_total             19743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00108_si_002.cif
_cod_data_source_block           mg195ho
_cod_original_cell_volume        9769.70(15)
_cod_database_code               4347396
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Others
 1*[Sof(Na6C)]+1*[Sof(Na6B)]+1*[Sof(Na6)+Sof(O1B)+Sof(O117)]=1 with esd of 0.001
 Sof(O108)=1-FVAR(1)
 Sof(O109)=FVAR(1)
 Sof(O116)=1-FVAR(2)
 Sof(O81)=FVAR(2)
 Sof(O117)=1-FVAR(5)
 Sof(Na6)=Sof(O1B)=FVAR(5)
 Sof(O201)=1-FVAR(6)
 Sof(O101)=FVAR(6)
 Sof(O200)=1-FVAR(7)
 Sof(O100)=FVAR(7)
;
_shelx_res_checksum              76903
_shelx_hkl_checksum              15348
_shelx_shelxl_version_number     2014/7
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'