Eu3+/Tb3+ and Dy3+ POM@MOFs and 2D coordination polymers based on pyridine-2,6-dicarboxylic acid for ratiometric optical temperature sensing
Kaczmarek, Anna M.; Journal of Materials Chemistry C 6 (2018) 5916–; doi:10.1039/C8TC01062E

data_7237303
_publ_section_title
;
 Eu3+/Tb3+ and Dy3+ POM@MOFs and 2D coordination polymers based on
 pyridine-2,6-dicarboxylic acid for ratiometric optical temperature
 sensing
;
_journal_issue                   22
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              5916
_journal_paper_doi               10.1039/C8TC01062E
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C21 H9 Eu0.88 N3 O16 Tb1.12, 6(O)'
_chemical_formula_sum            'C21 H9 Eu0.88 N3 O22 Tb1.12'
_chemical_formula_weight         967.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.515(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9877(2)
_cell_length_b                   14.3607(4)
_cell_length_c                   24.6049(7)
_cell_measurement_reflns_used    11793
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.9540
_cell_measurement_theta_min      3.5260
_cell_volume                     3148.47(14)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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   -114.00 -15.00   1.00    2.00    --  -41.68 -52.00-136.00   99
  2  \w    -69.00  30.00   1.00    2.00    --  -41.68  52.00   8.00   99
  3  \w     15.00 114.00   1.00    2.00    --   41.68  52.00   8.00   99
  4  \w     82.00 178.00   1.00   10.00    --  109.13  52.00   8.00   96
  5  \w     37.00 136.00   1.00   10.00    --  109.13 -52.00-136.00   99
  6  \w    -96.00  -2.00   1.00    2.00    --  -41.68 125.00   0.00   94
  7  \w    -30.00  69.00   1.00    2.00    --   41.68 -52.00-136.00   99
  8  \w     23.00  98.00   1.00    2.00    --   41.68-125.00-180.00   75
  9  \w     81.00 178.00   1.00   10.00    --  109.13  30.00 -60.00   97
 10  \w     37.00 138.00   1.00   10.00    --  109.13 -61.00  90.00  101
 11  \w     80.00 178.00   1.00   10.00    --  109.13  61.00  30.00   98
 12  \w     36.00 121.00   1.00   10.00    --  109.13-125.00-150.00   85
 13  \w   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00 120.00  101
 14  \w    -66.00  33.00   1.00    2.00    --  -41.68  38.00 150.00   99
 15  \w   -118.00  -9.00   1.00    2.00    --  -41.68 -77.00  30.00  109
 16  \w   -118.00  -9.00   1.00    2.00    --  -41.68 -77.00 120.00  109
 17  \w      9.00 100.00   1.00    2.00    --   41.68  77.00   0.00   91
 18  \w      9.00 118.00   1.00    2.00    --   41.68  77.00-120.00  109
;
_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      0.0170506000
_diffrn_orient_matrix_UB_12      0.0303753000
_diffrn_orient_matrix_UB_13      -0.0589382000
_diffrn_orient_matrix_UB_21      0.1415990000
_diffrn_orient_matrix_UB_22      -0.0607705000
_diffrn_orient_matrix_UB_23      0.0015877000
_diffrn_orient_matrix_UB_31      -0.0977431000
_diffrn_orient_matrix_UB_32      -0.0829740000
_diffrn_orient_matrix_UB_33      -0.0227074000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29446
_diffrn_reflns_theta_full        75.33
_diffrn_reflns_theta_max         75.33
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.506
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.540
_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    2.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1841.0
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.062
_refine_diff_density_max         3.086
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6270
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+8.0627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1556
_reflns_number_gt                5292
_reflns_number_total             6270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8tc01062e2.cif
_cod_data_source_block           eutbpom_mof
_cod_database_code               7237303
_chemical_oxdiff_formula         'C21 H9 Eu0.88 N3 O22 Tb1.12'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.003 and
sigma for terminal atoms of 0.006
Uanis(Tb1)
Uanis(Tb2)
3. Others
 Fixed Sof: Tb1(0.561) Tb2(0.561) Eu1(0.439) Eu2(0.439)
 Fixed X: Tb1(0.24656) Tb2(-0.218511) Eu1(0.24656) Eu2(-0.218511)
 Fixed Y: Tb1(0.455404) Tb2(0.207949) Eu1(0.455404) Eu2(0.207949)
 Fixed Z: Tb1(0.747682) Tb2(0.834075) Eu1(0.747682) Eu2(0.834075)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19)
;
_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 2.917
_oxdiff_exptl_absorpt_empirical_full_min 0.457