Cryogenic Luminescent Thermometers Based on Multinuclear Eu3+/Tb3+ Mixed Lanthanide Polyoxometalates
Kaczmarek, Anna M. Marta; Liu, Jing; Laforce, Brecht; Vincze, Laszlo; Van Hecke, Kristof; Van Deun, Rik; Dalton Trans.  (2017) –; doi:10.1039/C7DT01058C

data_7042652
_publ_section_title
;
 Cryogenic Luminescent Thermometers Based on Multinuclear Eu3+/Tb3+ Mixed
 Lanthanide Polyoxometalates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01058C
_journal_year                    2017
_chemical_formula_moiety         '3(Eu0.06 Mo29 O116 Tb3.94), 124(O)'
_chemical_formula_sum            'Eu0.19 Mo87 O472 Tb11.81'
_chemical_formula_weight         17804.60
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2017-01-25
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:38:10 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                86.5448(4)
_cell_angle_beta                 88.2388(5)
_cell_angle_gamma                86.4840(5)
_cell_formula_units_Z            2
_cell_length_a                   18.62032(13)
_cell_length_b                   29.59902(16)
_cell_length_c                   36.28676(17)
_cell_measurement_reflns_used    185764
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.6130
_cell_measurement_theta_min      2.7220
_cell_volume                     19917.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -45.00  43.50   0.75   35.00    --   10.33 -82.00 165.00  118
  2  \w    -45.00  22.50   0.75   35.00    --  -11.19 -82.00 165.00   90
  3  \w    -45.00  22.50   0.75   35.00    --  -11.19  82.00 -73.00   90
  4  \w    -63.00  37.50   0.75   35.00    --   10.33 -57.00  60.00  134
  5  \w    -20.00  50.50   0.75   35.00    --   10.33 -99.00  60.00   94
  6  \w    -20.00  50.50   0.75   35.00    --   10.33 -99.00 -60.00   94
  7  \w    -85.00  12.50   0.75   35.00    --  -11.19 -38.00-150.00  130
  8  \w    -88.00 -40.00   0.75   35.00    --  -11.19 156.00  75.55   64
  9  \w    -85.00  12.50   0.75   35.00    --  -11.19 -38.00 -60.00  130
 10  \w    -87.00  -3.75   0.75   35.00    --  -11.19 -77.00  90.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0259849000
_diffrn_orient_matrix_UB_12      -0.0111146000
_diffrn_orient_matrix_UB_13      0.0113574000
_diffrn_orient_matrix_UB_21      0.0272841000
_diffrn_orient_matrix_UB_22      -0.0081391000
_diffrn_orient_matrix_UB_23      0.0123550000
_diffrn_orient_matrix_UB_31      -0.0061622000
_diffrn_orient_matrix_UB_32      0.0197135000
_diffrn_orient_matrix_UB_33      0.0101058000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            447068
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.772
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.868
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.969
_exptl_crystal_description       needle
_exptl_crystal_F_000             16419.2
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.083
_refine_diff_density_max         5.338
_refine_diff_density_min         -3.661
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5105
_refine_ls_number_reflns         101627
_refine_ls_number_restraints     3498
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+582.4562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                83777
_reflns_number_total             101627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01058c3.cif
_cod_data_source_block           POM70_Moredo
_cod_database_code               7042652
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Eu0.19 Mo87 O472 Tb11.81'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(Tb1)
Uanis(Tb2)
Uanis(Tb3)
Uanis(Tb4)
Uanis(Tb5)
Uanis(Tb6)
Uanis(Tb7)
Uanis(Tb8)
Uanis(Tb9)
Uanis(Tb10)
Uanis(Tb11)
Uanis(Tb12)
2. Others
 Fixed Sof: Tb1(0.984) Eu1(0.016) Tb2(0.984) Eu2(0.016) Tb3(0.984) Eu3(0.016)
 Tb4(0.984) Eu4(0.016) Tb5(0.984) Eu5(0.016) Tb6(0.984) Eu6(0.016) Tb7(0.984)
 Eu7(0.016) Tb8(0.984) Eu8(0.016) Tb9(0.984) Eu9(0.016) Tb10(0.984) Eu10(0.016)
 Tb11(0.984) Eu11(0.016) Tb12(0.984) Eu12(0.016)
 Fixed X: Tb1(0.525517) Eu1(0.525517) Tb2(0.701176) Eu2(0.701176)
 Tb3(0.449031) Eu3(0.449031) Tb4(0.470901) Eu4(0.470901) Tb5(0.853251)
 Eu5(0.853251) Tb6(0.872252) Eu6(0.872252) Tb7(0.790174) Eu7(0.790174)
 Tb8(0.620938) Eu8(0.620938) Tb9(0.856112) Eu9(0.856112) Tb10(1.039021)
 Eu10(1.039021) Tb11(0.78972) Eu11(0.78972) Tb12(0.801208) Eu12(0.801208)
 Fixed Y: Tb1(0.788013) Eu1(0.788013) Tb2(0.713027) Eu2(0.713027)
 Tb3(0.856009) Eu3(0.856009) Tb4(0.617146) Eu4(0.617146) Tb5(0.730412)
 Eu5(0.730412) Tb6(0.49052) Eu6(0.49052) Tb7(0.562827) Eu7(0.562827)
 Tb8(0.632051) Eu8(0.632051) Tb9(0.144625) Eu9(0.144625) Tb10(0.05585)
 Eu10(0.05585) Tb11(0.202868) Eu11(0.202868) Tb12(-0.032825) Eu12(-0.032825)
 Fixed Z: Tb1(0.614903) Eu1(0.614903) Tb2(0.437545) Eu2(0.437545)
 Tb3(0.455316) Eu3(0.455316) Tb4(0.534122) Eu4(0.534122) Tb5(0.130287)
 Eu5(0.130287) Tb6(0.20365) Eu6(0.20365) Tb7(0.04635) Eu7(0.04635)
 Tb8(0.225307) Eu8(0.225307) Tb9(0.272882) Eu9(0.272882) Tb10(0.102528)
 Eu10(0.102528) Tb11(0.110738) Eu11(0.110738) Tb12(0.200086) Eu12(0.200086)
;
_shelx_res_checksum              49965
_shelx_hkl_checksum              23966
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.724