Isotypic lanthanide-organic frameworks and scintillating films with colour-tunable X-ray radioluminescence for imaging applications.
Gu, Qi; Wang, Wenqian; Lu, Hao; Chen, Xi; Wang, Shuaihua; Wu, Shaofan; Dalton transactions (Cambridge, England : 2003) 51 (2021) 257–263; doi:10.1039/d1dt03059k

data_7708923
_publ_section_title
;
 Isotypic lanthanide-organic frameworks and scintillating films with
 colour-tunable X-ray radioluminescence for imaging applications.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              257
_journal_page_last               263
_journal_paper_doi               10.1039/d1dt03059k
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C42 H27 N6 O6 Tb, H2 O'
_chemical_formula_sum            'C42 H29 N6 O7 Tb'
_chemical_formula_weight         888.64
_chemical_name_common            '[Tb(bmb)3]H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-07 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6637(2)
_cell_length_b                   22.0021(2)
_cell_length_c                   9.57190(10)
_cell_measurement_reflns_used    25670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.7740
_cell_measurement_theta_min      2.2200
_cell_volume                     3708.75(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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     -3.00  22.00   0.50    0.11    --   72.03 -19.00   0.00   50
  2  \w     27.00 106.00   0.50    0.11    --   72.03 -99.00 -30.00  158
  3  \w     33.00 106.00   0.50    0.11    --   72.03-125.00 -30.00  146
  4  \w     36.00  64.00   0.50    0.11    --   72.03 -57.00 120.00   56
  5  \w    -96.00 -33.00   0.50    0.11    --  -75.46 125.00-150.00  126
  6  \w    -59.00 -28.00   0.50    0.11    --  -75.46  57.00-120.00   62
  7  \w    -97.00 -39.00   0.50    0.11    --  -75.46 125.00  90.00  116
  8  \w   -107.00 -21.00   0.50    0.11    --  -75.46 125.00 120.00  172
  9  \w    -89.00  -2.00   0.50    0.11    --  -75.46  77.00  90.00  174
 10  \w    -65.00  -3.00   0.50    0.11    --  -75.46  57.00  90.00  124
 11  \w    -42.00  -5.00   0.50    0.11    --  -75.46  38.00 150.00   74
 12  \w    -13.00  70.00   0.50    0.60    --   -1.72  38.00 120.00  166
 13  \w    -57.00  -5.00   0.50    0.11    --  -75.46  57.00  30.00  104
 14  \w    -31.00  -4.00   0.50    0.11    --  -75.46  38.00   0.00   54
 15  \w    -43.00  -3.00   0.50    0.11    --  -75.46  38.00  30.00   80
 16  \w    -26.00  -1.00   0.50    0.11    --  -75.46  19.00   0.00   50
 17  \w    -26.00  -1.00   0.50    0.11    --  -75.46  19.00 -90.00   50
 18  \w    -42.00  -6.00   0.50    0.11    --  -75.46  38.00-120.00   72
 19  \w    -37.00 -10.00   0.50    0.11    --  -75.46  38.00-150.00   54
 20  \w    -25.00   0.00   0.50    0.11    --  -75.46  19.00-150.00   50
 21  \w   -123.00  -2.00   0.50    0.11    --  -75.46   0.00-180.00  242
 22  \w    -72.00  15.00   0.50    0.60    --   -1.72 -57.00 -30.00  174
 23  \w    -60.00 -34.00   0.50    0.60    --   -1.72 -38.00 150.00   52
 24  \w    -24.00   7.00   0.50    0.60    --   -1.72 -38.00 150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0530073000
_diffrn_orient_matrix_UB_12      0.0388805000
_diffrn_orient_matrix_UB_13      -0.0532331000
_diffrn_orient_matrix_UB_21      -0.0415767000
_diffrn_orient_matrix_UB_22      -0.0467112000
_diffrn_orient_matrix_UB_23      -0.0527252000
_diffrn_orient_matrix_UB_31      -0.0352602000
_diffrn_orient_matrix_UB_32      -0.0033817000
_diffrn_orient_matrix_UB_33      0.1186735000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            46785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.604
_diffrn_reflns_theta_min         2.794
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    10.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+1.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7264
_reflns_number_total             8420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03059k2.cif
_cod_data_source_block           LnOF-1
_cod_depositor_comments
'Adding full bibliography for 7708923--7708924.cif.'
_cod_database_code               7708923
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_usercomment     'C H O N Tb'
_diffrn_oxdiff_digest_frames
;
012b79df8ddd20844afc8fd1478abb370200038de23
;
_diffrn_oxdiff_digest_hkl
;
011858c4278286b431ea2c905491bf5ef5861c
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O56(H56a,H56b)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C31(H31), C15(H15), C27(H27), C40(H40), C46(H46), C36(H36),
 C42(H42), C11(H11), C34(H34), C8(H8), C29(H29), C43(H43), C35(H35), C28(H28),
 C13(H13), C49(H49), C44(H44), C7(H7), C2(H2), C12(H12), C6(H6), C5(H5),
 C55(H55), C51(H51), C52(H52), C50(H50)
;
_shelx_res_checksum              24398
_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 2.485
_oxdiff_exptl_absorpt_empirical_full_min 0.624