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_1565654
_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 Ho1.38 N2 O12'
_chemical_formula_sum            'C14 H6 Ho1.38 N2 O12'
_chemical_formula_weight         620.99
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9801(2)
_cell_length_b                   14.9801(2)
_cell_length_c                   14.6127(3)
_cell_measurement_reflns_used    5723
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3240
_cell_measurement_theta_min      2.7090
_cell_volume                     3279.14(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.938
_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    -33.00  13.00   0.50   40.89    --   -9.60 102.00  15.00   92
  2  \w     26.00  78.00   0.50   40.89    --   10.46  26.00-100.00  104
  3  \w    -44.00  -3.00   0.50   40.89    --   -9.60 125.00  30.00   82
  4  \w    -56.00  -7.00   0.50   40.89    --   -9.60 125.00 120.00   98
  5  \w    -21.00   5.00   0.50   40.89    --   10.46 -26.00  95.00   52
;
_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      -0.0251518000
_diffrn_orient_matrix_UB_12      -0.0160280000
_diffrn_orient_matrix_UB_13      0.0377121000
_diffrn_orient_matrix_UB_21      -0.0392075000
_diffrn_orient_matrix_UB_22      0.0006810000
_diffrn_orient_matrix_UB_23      -0.0271769000
_diffrn_orient_matrix_UB_31      0.0084426000
_diffrn_orient_matrix_UB_32      -0.0445629000
_diffrn_orient_matrix_UB_33      -0.0139648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6513
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.386
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_description       block
_exptl_crystal_F_000             2337
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.793
_refine_diff_density_min         -2.639
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Flack x determined using 1068 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2960
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0512P)^2^+19.8646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.622
_reflns_Friedel_fraction_full    0.701
_reflns_Friedel_fraction_max     0.634
_reflns_number_gt                2890
_reflns_number_total             2960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-500-119236.cif
_cod_data_source_block           ms72
_cod_original_cell_volume        3279.14(11)
_cod_database_code               1565654
_chemical_oxdiff_formula         'C11 H10 N O Ho1'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C5-C7B
 1.37 with sigma of 0.02
 N2B-C7B
 1.4 with sigma of 0.02
 Ho1-N1A \\sim Ho1-C14B
 with sigma of 0.02
 C12-C14A \\sim C12-N1B
 with sigma of 0.02
 C9-N1A \\sim C9-C14B
 with sigma of 0.02
 Ho2-C14A \\sim Ho2-N1B
 with sigma of 0.02
 N1A-C14A \\sim C14B-N1B
 with sigma of 0.02
 Ho1-C14A \\sim Ho1-N1B
 with sigma of 0.04
 C12-N1A \\sim C12-C14B
 with sigma of 0.04
 C9-C14A \\sim C9-N1B
 with sigma of 0.04
 Ho2-N1A \\sim Ho2-C14B
 with sigma of 0.04
4. Restrained planarity
 N2A, C7A, C2, C3, C4, C5
 with sigma of 0.1
 N2B, C7B, C5, C4, C3, C2
 with sigma of 0.1
 C5, C7B, N2B, C2, C3, C4
 with sigma of 0.1
 C9, C10, C11, C12, C14A, N1A
 with sigma of 0.1
 N1B, C14B, C9, C10, C11, C12
 with sigma of 0.1
 C2, C7A, N2A, C5, C4, C3
 with sigma of 0.1
 C5, C4, C3, C2, N2B, C7B
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(N1B) = Uanis(C14A) = Uanis(N1A) = Uanis(C14B) = Uanis(C9) = Uanis(C10) =
Uanis(C11) = Uanis(C12)
Uanis(C7A) = Uanis(C7B) = Uanis(N2B) = Uanis(N2A) = Uanis(C5) = Uanis(C4) =
Uanis(C3) = Uanis(C2)
6. Others
 Sof(C7B)=Sof(H7B)=Sof(N2B)=Sof(Ho2)=Sof(C14B)=Sof(H14B)=Sof(N1B)=1-FVAR(1)
 Sof(Ho1)=Sof(N2A)=Sof(C7A)=Sof(H7A)=Sof(N1A)=Sof(C14A)=Sof(H14A)=FVAR(1)
 Fixed Sof: Ho4(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C3(H3), C4(H4), C7B(H7B), C7A(H7A), C14A(H14A), C14B(H14B)
;
_shelx_hkl_checksum              20087