Single ion magnets based on lanthanoid polyoxomolybdate complexes.
Baldoví, José J; Duan, Yan; Bustos, Carlos; Cardona-Serra, Salvador; Gouzerh, Pierre; Villanneau, Richard; Gontard, Geoffrey; Clemente-Juan, Juan M; Gaita-Ariño, Alejandro; Giménez-Saiz, Carlos; Proust, Anna; Coronado, Eugenio; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16653–16660; doi:10.1039/c6dt02258h

data_7040472
_publ_section_title
;
 Single ion magnets based on lanthanoid polyoxomolybdate complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16653
_journal_page_last               16660
_journal_paper_doi               10.1039/c6dt02258h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'Mo16 O52 Er, 5(C16 H36 N), 8(C2 H3 N)'
_chemical_formula_sum            'C96 H204 Er Mo16 N13 O52'
_chemical_formula_weight         4075.02
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Moisture-sensitive, Efflorescent'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-16 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.8110(3)
_cell_length_b                   33.1580(5)
_cell_length_c                   48.1554(8)
_cell_measurement_reflns_used    15212
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.0630
_cell_measurement_theta_min      3.2090
_cell_volume                     28439.5(8)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            135509
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16216
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Crystals of ErMo8 are extremely efflorescent and solvent loss occurs 
immediately after they are separated from their mother solutions. Therefore, 
although the crystals were quickly covered with Paratone-N oil and placed in a 
stream of cooled nitrogen (120 K), some partial loss of solvent from the 
crystal could not be avoided. This fact causes a lowering in the quality of 
the single crystals as well as a large disorder in some of the organic cations 
present in the crystals. The structure solution reveals that some 
tetrabutylammonium (TBA) cations are extremely disordered, exhibiting 
unusually high isotropic thermal parameters. This fact was attributed to 
thermal libration caused by the loss of solvent molecules from the crystal, 
which creates voids in the surroundings of these TBA cations. In particular,  
one of the TBA cations was so disordered that some carbon atoms could not be 
found in difference maps and, then, the whole cation was removed from the 
experimental structure factors and modeled using the SQUEEZE procedure.
In addition, some acetonitrile molecules were found in difference maps 
exhibiting large disorder and very high isotropic thermal factors. As they 
could not be modeled satisfactorily using atomic sites, they were also 
removed from the atomic list and their diffuse contribution  treated with 
the SQUEEZE program. This procedure gave void volumes and electron numbers 
per unit cell which correspond to one TBA cation and 8 acetonitrile molecules, 
which were added to the formula unit of compound ErMo8.
;
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.462
_refine_ls_extinction_coef       0.00124(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         31298
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2688
_refine_ls_wR_factor_ref         0.3039
_reflns_number_gt                14582
_reflns_number_total             31298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02258h2.cif
_cod_data_source_block           ErMo8
_cod_depositor_comments
'Adding full bibliography for 7040469--7040479.cif.'
_cod_database_code               7040472