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_7040471
_publ_section_title
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 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 Ho, 5(C16 H36 N), 8(C2 H3 N)'
_chemical_formula_sum            'C96 H204 Ho Mo16 N13 O52'
_chemical_formula_weight         4072.69
_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                   17.88390(15)
_cell_length_b                   32.8402(2)
_cell_length_c                   47.8961(4)
_cell_measurement_reflns_used    86981
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.1450
_cell_measurement_theta_min      3.3640
_cell_volume                     28129.9(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega  -53.00   11.35   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6917  107.0000   36.0000 117

  2 omega   12.00   79.10   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292 -107.0000  -61.0000 122

  3 omega  -12.00   14.40   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6917  -99.0000  -30.0000 48

  4 omega   36.00   62.40   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292  178.0000  120.0000 48

  5 omega  -10.00   95.05   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   57.0000   90.0000 191

  6 omega  -65.00   47.75   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6917   57.0000 -150.0000 205

  7 omega  -10.00  102.75   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   57.0000 -180.0000 205

  8 omega  -48.00   28.45   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292  -57.0000  -60.0000 139

  9 omega  -10.00  102.75   0.5500   24.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6292   57.0000  -60.0000 205

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0081339000
_diffrn_orient_matrix_UB_12      -0.0051694000
_diffrn_orient_matrix_UB_13      -0.0140544000
_diffrn_orient_matrix_UB_21      -0.0387885000
_diffrn_orient_matrix_UB_22      -0.0002313000
_diffrn_orient_matrix_UB_23      -0.0030931000
_diffrn_orient_matrix_UB_31      0.0015705000
_diffrn_orient_matrix_UB_32      0.0209660000
_diffrn_orient_matrix_UB_33      -0.0035022000
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0267
_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       63
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            296655
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75991
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16208
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.121
_platon_squeeze_details
;
Crystals of HoMo8 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 HoMo8.
;
_refine_diff_density_max         2.257
_refine_diff_density_min         -1.789
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1330
_refine_ls_number_reflns         33161
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+744.4572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1844
_reflns_number_gt                28468
_reflns_number_total             33161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02258h2.cif
_cod_data_source_block           HoMo8
_cod_depositor_comments
'Adding full bibliography for 7040469--7040479.cif.'
_cod_database_code               7040471