Crystal structures and photoluminescent properties of highly disordering lanthanide-2,5-pyridinedicarboxylate frameworks
Yotnoi, Bunlawee; Sinchow, Malee; Ngamjarurojana, Athipong; Rujiwatra, Apinpus; Inorganica Chimica Acta 500 (2020) 119236–; doi:10.1016/j.ica.2019.119236

data_1565653
_publ_section_title
;
 Crystal structures and photoluminescent properties of highly disordering
 lanthanide-2,5-pyridinedicarboxylate frameworks
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119236
_journal_paper_doi               10.1016/j.ica.2019.119236
_journal_volume                  500
_journal_year                    2020
_chemical_formula_moiety         'C14 H6 N2 O12 Tb1.38'
_chemical_formula_sum            'C14 H6 N2 O12 Tb1.38'
_chemical_formula_weight         612.72
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0088(6)
_cell_length_b                   15.0088(6)
_cell_length_c                   14.5806(13)
_cell_measurement_reflns_used    7415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3530
_cell_measurement_theta_min      2.6950
_cell_volume                     3284.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15t (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15t (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15t (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.921
_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     -4.00  59.00   0.50   30.00    --   18.78-112.00  94.00  126
  2  \w     31.00  83.00   0.50   30.00    --   18.78  39.00 -31.00  104
  3  \w     17.00  49.00   0.50   30.00    --  -17.85  30.00-120.00   64
  4  \w    -26.00   9.00   0.50   30.00    --  -17.85  30.00-120.00   70
  5  \w      3.00  28.00   0.50   30.00    --   18.78-125.00   0.00   50
  6  \w     19.00  44.00   0.50   30.00    --   18.78 -77.00 -90.00   50
  7  \w    -40.00  -7.00   0.50   30.00    --   18.78 -77.00 -90.00   66
  8  \w     17.00  60.00   0.50   30.00    --   18.78-125.00-150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0298792000
_diffrn_orient_matrix_UB_12      0.0073479000
_diffrn_orient_matrix_UB_13      -0.0367404000
_diffrn_orient_matrix_UB_21      -0.0297539000
_diffrn_orient_matrix_UB_22      0.0220863000
_diffrn_orient_matrix_UB_23      0.0300576000
_diffrn_orient_matrix_UB_31      0.0213102000
_diffrn_orient_matrix_UB_32      0.0411067000
_diffrn_orient_matrix_UB_33      -0.0095721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5884
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.432
_diffrn_reflns_theta_min         1.919
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15t (Rigaku Oxford Diffraction, 2018)
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    2.478
_exptl_crystal_description       block
_exptl_crystal_F_000             2315
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.601
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 1010 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2918
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0466P)^2^+4.7659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.610
_reflns_Friedel_fraction_full    0.730
_reflns_Friedel_fraction_max     0.611
_reflns_number_gt                2791
_reflns_number_total             2918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-500-119236.cif
_cod_data_source_block           ms80_tb
_cod_original_cell_volume        3284.5(4)
_cod_database_code               1565653
_chemical_oxdiff_formula         'C24 H10 O24 Tb3 N4'
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.468
_reflns_odcompleteness_completeness 67.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(3)
 0.50(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N2B-C7B
 1.4 with sigma of 0.02
 C14A-C12
 1.36 with sigma of 0.02
 N1A-C14A
 1.4 with sigma of 0.02
 N2A-C7A
 1.4 with sigma of 0.02
 N2A-C7A \\sim N2A-C2
 with sigma of 0.02
 C5-C7A \\sim C4-C5 \\sim C3-C4 \\sim C2-C3
 with sigma of 0.02
4. Restrained planarity
 C7A, N2A, C2, C3, C4, C5
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(N1A) = Uanis(C14B) = Uanis(N1B) = Uanis(C14A)
Uanis(C7A) = Uanis(N2B) = Uanis(N2A) = Uanis(C7B)
6. Others
 Sof(N2B)=Sof(Tb2)=Sof(C7B)=Sof(H7B)=Sof(C14B)=Sof(H14B)=Sof(N1B)=1-FVAR(1)
 Sof(Tb1)=Sof(C14A)=Sof(H14A)=Sof(N1A)=Sof(N2A)=Sof(C7A)=Sof(H7A)=FVAR(1)
 Fixed Sof: Tb4(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C4(H4), C3(H3), C7B(H7B), C11(H11), C10(H10), C7A(H7A), C14B(H14B)
;