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_7040473
_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 Tm, 5(C16 H36 N), 8(C2 H3 N)'
_chemical_formula_sum            'C96 H204 Mo16 N13 O52 Tm'
_chemical_formula_weight         4076.69
_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                   17.8375(2)
_cell_length_b                   32.8499(4)
_cell_length_c                   47.7986(8)
_cell_measurement_reflns_used    29754
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.6020
_cell_measurement_theta_min      3.1770
_cell_volume                     28008.1(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 0.996
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega  -63.00  -39.00   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.8479  111.0000  109.0000 32

  2 omega   28.00   64.00   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.7073 -111.0000 -109.0000 48

  3 omega   50.50   73.75   0.7500    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.4297 -178.0000 -120.0000 31

  4 omega  -47.75   49.75   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.7073  -38.0000  -30.0000 130

  5 omega   80.25  101.25   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.7073   57.0000  120.0000 28

  6 omega  -75.25   37.25   0.7500    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.4297  -57.0000  -90.0000 150

  7 omega -111.25  -87.25   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.8479  -77.0000   90.0000 32

  8 omega  -14.25  109.50   0.7500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.7073   77.0000  -30.0000 165

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0011596000
_diffrn_orient_matrix_UB_12      0.0193307000
_diffrn_orient_matrix_UB_13      0.0065907000
_diffrn_orient_matrix_UB_21      -0.0094568000
_diffrn_orient_matrix_UB_22      -0.0091984000
_diffrn_orient_matrix_UB_23      0.0129587000
_diffrn_orient_matrix_UB_31      0.0386134000
_diffrn_orient_matrix_UB_32      -0.0028510000
_diffrn_orient_matrix_UB_33      0.0029678000
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            164439
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    2.087
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.685
_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    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16224
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2591
_exptl_crystal_size_mid          0.1485
_exptl_crystal_size_min          0.0678
_platon_squeeze_details
;
Crystals of TmMo8 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 8 acetonitrile molecules, 
which were added to the formula unit of compound TmMo8.
;
_refine_diff_density_max         1.965
_refine_diff_density_min         -1.796
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1295
_refine_ls_number_reflns         32083
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.1116
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+1232.7322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                22110
_reflns_number_total             32083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02258h2.cif
_cod_data_source_block           TmMo8
_cod_depositor_comments
'Adding full bibliography for 7040469--7040479.cif.'
_cod_database_code               7040473