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_7040469
_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 Tb, 5(C16 H36 N), 6(C2 H3 N)'
_chemical_formula_sum            'C92 H198 Mo16 N11 O52 Tb'
_chemical_formula_weight         3984.57
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Moisture-sensitive, Efflorescent'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.419(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0421(7)
_cell_length_b                   17.1885(5)
_cell_length_c                   31.9702(9)
_cell_measurement_reflns_used    15611
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.1400
_cell_measurement_theta_min      3.2890
_cell_volume                     13756.9(7)
_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 0.982
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega  -96.60  -72.80   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9495 -178.0000  -60.0000 34

  2 omega  -84.60  -44.00   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9495 -178.0000  120.0000 58

  3 omega  -34.60   95.60   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       23.7307  -19.0000  -60.0000 186

  4 omega   41.40   89.70   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       23.7307 -178.0000 -120.0000 69

  5 omega    2.70    5.50   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9495  -57.0000   90.0000 4

  6 omega  -58.60    6.50   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9495   77.0000  120.0000 93

  7 omega -108.60  -37.20   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9495  178.0000 -180.0000 102

  8 omega  -15.00   37.50   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       23.7307   83.0000  -95.0000 75

  9 omega  -13.00   99.00   0.7000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       23.7307   77.0000    0.0000 160

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0129343000
_diffrn_orient_matrix_UB_12      0.0328656000
_diffrn_orient_matrix_UB_13      -0.0085341000
_diffrn_orient_matrix_UB_21      -0.0047278000
_diffrn_orient_matrix_UB_22      -0.0148909000
_diffrn_orient_matrix_UB_23      -0.0204559000
_diffrn_orient_matrix_UB_31      -0.0247628000
_diffrn_orient_matrix_UB_32      0.0200124000
_diffrn_orient_matrix_UB_33      -0.0011501000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            126269
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7920
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2985
_exptl_crystal_size_mid          0.1639
_exptl_crystal_size_min          0.0691
_platon_squeeze_details
;
Crystals of TbMo8 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. 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 removed from the atomic list and their diffuse contribution was 
treated with the SQUEEZE program. This procedure gave void volumes and 
electron numbers per unit cell which correspond to 6 acetonitrile molecules, 
which were added to the formula unit of compound TbMo8.
;
_refine_diff_density_max         4.487
_refine_diff_density_min         -2.452
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         32334
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.1205
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1438P)^2^+325.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3127
_refine_ls_wR_factor_ref         0.3448
_reflns_number_gt                18162
_reflns_number_total             32334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02258h2.cif
_cod_data_source_block           TbMo8
_cod_depositor_comments
'Adding full bibliography for 7040469--7040479.cif.'
_cod_database_code               7040469