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_1565655
_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 Er1.38 N2 O12'
_chemical_formula_sum            'C14 H6 Er1.38 N2 O12'
_chemical_formula_weight         624.19
_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     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9510(2)
_cell_length_b                   14.9510(2)
_cell_length_c                   14.6100(3)
_cell_measurement_reflns_used    9084
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      1.9210
_cell_volume                     3265.81(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 0.967
_diffrn_measured_fraction_theta_max 0.922
_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    -61.00  27.00   0.50    8.14    --   10.46 -15.00 170.00  176
  2  \w    -27.00  54.00   0.50    8.14    --   -9.60  57.00   0.00  162
  3  \w    -19.00  44.00   0.50    8.14    --   10.46 -99.00 -60.00  126
  4  \w     -6.00  52.00   0.50    8.14    --   10.46-114.00  58.00  116
  5  \w     -7.00  52.00   0.50    8.14    --   10.46  57.00 150.00  118
;
_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      -0.0459716000
_diffrn_orient_matrix_UB_12      0.0023119000
_diffrn_orient_matrix_UB_13      -0.0117466000
_diffrn_orient_matrix_UB_21      -0.0107967000
_diffrn_orient_matrix_UB_22      0.0092240000
_diffrn_orient_matrix_UB_23      0.0463300000
_diffrn_orient_matrix_UB_31      0.0044414000
_diffrn_orient_matrix_UB_32      0.0464764000
_diffrn_orient_matrix_UB_33      -0.0086025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10109
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         1.926
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44634
_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    2.539
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.655
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Flack x determined using 1348 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3329
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.9257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.849
_reflns_number_gt                3168
_reflns_number_total             3329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-500-119236.cif
_cod_data_source_block           ms20as100918
_cod_original_cell_volume        3265.81(11)
_cod_database_code               1565655
_chemical_oxdiff_formula         'Er1 C7 H3 O4 N1'
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.361
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(2)
 0.48(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Er1-C14B \\sim Er1-N1A
 with sigma of 0.02
 N1B-C14B \\sim C14A-N1A
 with sigma of 0.02
 N1B-C12 \\sim C14A-C12
 with sigma of 0.02
 C14B-C9 \\sim N1A-C9
 with sigma of 0.02
 Er1-N1B \\sim Er1-C14A
 with sigma of 0.04
 N1B-C9 \\sim C14A-C9
 with sigma of 0.04
 C14B-C12 \\sim N1A-C12
 with sigma of 0.04
 Er2-N2B \\sim Er2-C7A
 with sigma of 0.02
 C2-C7B \\sim C2-N2A
 with sigma of 0.02
 N2B-C5 \\sim C7A-C5
 with sigma of 0.02
 N2B-C7B \\sim C7A-N2A
 with sigma of 0.02
 C7B-Er1 \\sim N2A-Er1
 with sigma of 0.02
 Er2-C7B \\sim Er2-N2A
 with sigma of 0.04
 C2-N2B \\sim C2-C7A
 with sigma of 0.04
 N2B-Er1 \\sim C7A-Er1
 with sigma of 0.04
 C5-C7B \\sim C5-N2A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C14B) = Uanis(C14A) =
Uanis(N1B) = Uanis(N1A)
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C7A) = Uanis(N2B) =
Uanis(C7B) = Uanis(N2A)
5. Others
 Sof(Er2)=Sof(N2B)=Sof(C7B)=Sof(H7B)=Sof(N1B)=Sof(C14B)=Sof(H14B)=1-FVAR(1)
 Sof(Er1)=Sof(N1A)=Sof(C14A)=Sof(H14A)=Sof(C7A)=Sof(H7A)=Sof(N2A)=FVAR(1)
 Fixed Sof: Er4(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7B(H7B), C14B(H14B), C11(H11), C10(H10), C14A(H14A), C7A(H7A)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.288
_oxdiff_exptl_absorpt_empirical_full_min 0.643