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_4347393
_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 O106.22 P2 W18 Y3, 9.78(O)'
_chemical_formula_sum            'C H84 Na11 O116 P2 W18 Y3'
_chemical_formula_weight         5843.54
_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'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_angle_alpha                90
_cell_angle_beta                 111.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3425(4)
_cell_length_b                   25.9777(4)
_cell_length_c                   23.4294(4)
_cell_measurement_reflns_used    20004
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      28.6950
_cell_measurement_theta_min      2.9890
_cell_volume                     9808.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (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 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
  1 omega    1.75   58.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4933  -99.0000  -90.0000 75

  2 omega  -64.00   20.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4933  -57.0000  -30.0000 112

  3 omega   34.00   75.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4933 -178.0000  -60.0000 55

  4 omega  -17.00   93.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4933   38.0000  120.0000 147

  5 omega -101.00  -62.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.6496 -178.0000   60.0000 52

  6 omega  -14.00   27.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.6496  -99.0000  120.0000 55
;
_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      -0.0075019000
_diffrn_orient_matrix_UB_12      0.0262870000
_diffrn_orient_matrix_UB_13      -0.0083562000
_diffrn_orient_matrix_UB_21      -0.0427973000
_diffrn_orient_matrix_UB_22      -0.0035102000
_diffrn_orient_matrix_UB_23      -0.0057018000
_diffrn_orient_matrix_UB_31      0.0071665000
_diffrn_orient_matrix_UB_32      0.0064359000
_diffrn_orient_matrix_UB_33      0.0309545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.057
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.985
_exptl_absorpt_correction_T_max  0.437
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.957
_exptl_crystal_description       'Hexagonal faceted rod'
_exptl_crystal_F_000             10472
_exptl_crystal_size_max          0.2519
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.04
_refine_diff_density_max         7.007
_refine_diff_density_min         -5.231
_refine_diff_density_rms         0.669
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         23420
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0973P)^2^+76.8166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17112
_reflns_number_total             23420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00108_si_002.cif
_cod_data_source_block           mg1_p_y_na3gau
_cod_database_code               4347393
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 1*[Sof(O202)]+1*[Sof(O203)]+1*[Sof(O204)]=1 with esd of 0.001
 Fixed Uiso: O93(0.15) O201(0.15) O202(0.15) O203(0.15) O204(0.15)
;
_shelx_res_checksum              16038
_shelx_hkl_checksum              61049
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'