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_7040474
_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 Yb, 5(C16 H36 N), 8(C2 H3 N)'
_chemical_formula_sum            'C96 H204 Mo16 N13 O52 Yb'
_chemical_formula_weight         4080.80
_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                   17.8722(3)
_cell_length_b                   32.7932(5)
_cell_length_c                   47.8651(7)
_cell_measurement_reflns_used    35645
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.1364
_cell_measurement_theta_min      3.1284
_cell_volume                     28053.1(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -57.00  -16.80   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6917  100.0000  -75.0000 67

  2 omega  -16.00   10.40   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292 -100.0000  179.0000 44

  3 omega  -62.00   49.00   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6917   57.0000  120.0000 185

  4 omega   41.00  118.40   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292  178.0000  -60.0000 129

  5 omega   89.00  122.00   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292  178.0000 -180.0000 55

  6 omega  -10.00  104.00   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   57.0000    0.0000 190

  7 omega  -10.00  104.00   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   57.0000 -120.0000 190

  8 omega  -57.00    6.00   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292  -77.0000  -90.0000 105

  9 omega  -16.00  110.60   0.6000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   77.0000  120.0000 211

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0211738000
_diffrn_orient_matrix_UB_12      -0.0086605000
_diffrn_orient_matrix_UB_13      -0.0132307000
_diffrn_orient_matrix_UB_21      -0.0254794000
_diffrn_orient_matrix_UB_22      0.0111278000
_diffrn_orient_matrix_UB_23      -0.0033991000
_diffrn_orient_matrix_UB_31      0.0218437000
_diffrn_orient_matrix_UB_32      0.0045788000
_diffrn_orient_matrix_UB_33      -0.0167589000
_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  0.0912
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_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            298597
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16232
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2296
_exptl_crystal_size_mid          0.1783
_exptl_crystal_size_min          0.1755
_platon_squeeze_details
;
Crystals of YbMo8 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 YbMo8.
;
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         32999
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1134
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+1325.6974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2469
_reflns_number_gt                23700
_reflns_number_total             32999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02258h2.cif
_cod_data_source_block           YbMo8
_cod_depositor_comments
'Adding full bibliography for 7040469--7040479.cif.'
_cod_database_code               7040474