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_7042651
_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         'Eu0.32 Mo29 O116 Tb3.68, 47(O)'
_chemical_formula_sum            'Eu0.32 Mo29 O163 Tb3.68'
_chemical_formula_weight         6023.75
_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'
_atom_sites_solution_hydrogens   undef
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-24
_audit_creation_method
;
Olex2 1.2
(compiled Nov  7 2016 13:22:42 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                85.8270(10)
_cell_angle_beta                 87.5250(10)
_cell_angle_gamma                65.5430(10)
_cell_formula_units_Z            2
_cell_length_a                   17.1832(2)
_cell_length_b                   19.3527(3)
_cell_length_c                   23.8426(2)
_cell_measurement_reflns_used    53090
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.0820
_cell_measurement_theta_min      2.7550
_cell_volume                     7197.35(16)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.891
_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    -65.00  43.00   1.00   20.00    --   10.17 -76.00-175.00  108
  2  \w    -22.00  86.00   1.00   20.00    --   10.17  76.00 -48.00  108
  3  \w    -14.00  84.00   1.00   20.00    --   10.17  38.00 120.00   98
  4  \w     34.00  97.00   1.00   20.00    --   10.17-178.00 -60.00   63
  5  \w    -70.00  51.00   1.00   20.00    --   10.17 -19.00-150.00  121
  6  \w     34.00  97.00   1.00   20.00    --   10.17-178.00-150.00   63
  7  \w    -86.00 -38.00   1.00   20.00    --  -11.03 153.00 140.59   48
  8  \w    -70.00 -27.00   1.00   20.00    --  -11.03 129.00  69.38   43
  9  \w    -84.00  17.00   1.00   20.00    --  -11.03 -57.00  90.00  101
 10  \w    -63.00 -26.00   1.00   20.00    --   10.17 -57.00   0.00   37
;
_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      -0.0164860000
_diffrn_orient_matrix_UB_12      0.0391209000
_diffrn_orient_matrix_UB_13      -0.0089509000
_diffrn_orient_matrix_UB_21      0.0292501000
_diffrn_orient_matrix_UB_22      -0.0086371000
_diffrn_orient_matrix_UB_23      -0.0230722000
_diffrn_orient_matrix_UB_31      -0.0304871000
_diffrn_orient_matrix_UB_32      -0.0046985000
_diffrn_orient_matrix_UB_33      -0.0166573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            158877
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.696
_diffrn_reflns_theta_min         2.560
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.481
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_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    2.780
_exptl_crystal_description       block
_exptl_crystal_F_000             5562.7
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.087
_refine_diff_density_max         3.751
_refine_diff_density_min         -3.317
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1753
_refine_ls_number_reflns         36369
_refine_ls_number_restraints     1200
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+96.5020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26163
_reflns_number_total             36369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01058c2.cif
_cod_data_source_block           pom69
_cod_database_code               7042651
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Eu0.32 Mo29 O163 Tb3.68'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Tb1, Eu1}
{Tb2, Eu2}
{Tb3, Eu3}
{Eu4, Tb4}
2. Others
 Fixed Sof: Tb1(0.92) Eu1(0.08) Tb2(0.92) Eu2(0.08) Tb3(0.92) Eu3(0.08)
 Tb4(0.92) Eu4(0.08)
 Fixed X: Tb1(0.0684) Eu1(0.0684) Tb2(0.3674) Eu2(0.3674) Tb3(0.2005)
 Eu3(0.2005) Tb4(0.463) Eu4(0.463)
 Fixed Y: Tb1(0.4899) Eu1(0.4899) Tb2(0.5826) Eu2(0.5826) Tb3(0.361)
 Eu3(0.361) Tb4(0.359) Eu4(0.359)
 Fixed Z: Tb1(0.6562) Eu1(0.6562) Tb2(0.8237) Eu2(0.8237) Tb3(0.895)
 Eu3(0.895) Tb4(0.6348) Eu4(0.6348)
;
_shelx_res_checksum              12919
_shelx_hkl_checksum              74231
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.819