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_4347397
_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 Er3 Na11 O103.55 P2 W18, 12.45(O)'
_chemical_formula_sum            'C H84 Er3 Na11 O116 P2 W18'
_chemical_formula_weight         6078.59
_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
_cell_angle_beta                 111.6682(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.37028(19)
_cell_length_b                   26.0440(2)
_cell_length_c                   23.4126(3)
_cell_measurement_reflns_used    35551
_cell_measurement_temperature    135(7)
_cell_measurement_theta_max      75.6510
_cell_measurement_theta_min      3.2080
_cell_volume                     9843.2(2)
_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
;
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)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      135(7)
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -94.00  -13.00   1.0000    5.6400
omega____ theta____ kappa____ phi______ frames
    -      -40.9342  125.0000 -150.0000 81

  2 omega  -42.00   27.00   1.0000    5.6400
omega____ theta____ kappa____ phi______ frames
    -      -40.9342   37.0000 -150.0000 69

  3 omega -120.00   -7.00   1.0000    5.6400
omega____ theta____ kappa____ phi______ frames
    -      -40.9342  -77.0000   90.0000 113

  4 omega  -10.00   16.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000 -120.0000 26

  5 omega  -55.00  -27.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   45.0000   90.0000 28

  6 omega  -34.00   14.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   77.0000  -30.0000 48

  7 omega -109.00  -83.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000 -180.0000 26

  8 omega -108.00  -82.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -94.0000  -30.0000 26

  9 omega   82.00  178.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063   30.0000  150.0000 96

 10 omega   27.00  103.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -94.0000   30.0000 76

 11 omega   42.00   90.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000  -30.0000 48

 12 omega   80.00  177.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063   30.0000 -120.0000 97

 13 omega   36.00   78.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -45.0000 -150.0000 42

 14 omega   40.00   67.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063 -111.0000  120.0000 27

 15 omega   54.00  106.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -94.0000  -60.0000 52

 16 omega   58.00   84.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000 -150.0000 26

 17 omega   37.00   79.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000 -120.0000 42

 18 omega   81.00  115.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063 -111.0000  120.0000 34

 19 omega   54.00  108.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -94.0000 -150.0000 54

 20 omega   38.00   81.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -45.0000  120.0000 43

 21 omega   39.00   80.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000  150.0000 41

 22 omega   38.00   85.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063 -111.0000    0.0000 47

 23 omega   49.00  116.00   1.0000   22.5500
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -61.0000   60.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0411228000
_diffrn_orient_matrix_UB_12      -0.0330458000
_diffrn_orient_matrix_UB_13      0.0354054000
_diffrn_orient_matrix_UB_21      -0.0632700000
_diffrn_orient_matrix_UB_22      0.0431418000
_diffrn_orient_matrix_UB_23      -0.0060858000
_diffrn_orient_matrix_UB_31      -0.0584343000
_diffrn_orient_matrix_UB_32      -0.0235435000
_diffrn_orient_matrix_UB_33      -0.0609192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71768
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.864
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    44.262
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.271
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    4.102
_exptl_crystal_description       'Hexagonal-faced rod'
_exptl_crystal_F_000             10820
_exptl_crystal_size_max          0.0919
_exptl_crystal_size_mid          0.0377
_exptl_crystal_size_min          0.0171
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1304
_refine_ls_number_reflns         20109
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0313P)^2^+115.5597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19115
_reflns_number_total             20109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00108_si_002.cif
_cod_data_source_block           mg1_er_p_na5absspheerical
_cod_original_cell_volume        9843.25(19)
_cod_database_code               4347397
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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(O91) = Uanis(O91A)
Uanis(O92) = Uanis(O92A)
Uanis(O93) = Uanis(O93A)
Uiso(O95) = Uiso(O95A)
Uiso(Na9) = Uiso(Na9A)
Uiso(Na8) = Uiso(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              47428
_shelx_hkl_checksum              90280
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'