Autoluminescent Metal-Organic Frameworks (MOFs): Self-Photoemission of a Highly Stable Thorium MOF.
Andreo, Jacopo; Priola, Emanuele; Alberto, Gabriele; Benzi, Paola; Marabello, Domenica; Proserpio, Davide M.; Lamberti, Carlo; Diana, Eliano; Journal of the American Chemical Society 140 (2018) 14144–14149; doi:10.1021/jacs.8b07113

data_4132883
_publ_section_title
;
 Autoluminescent Metal-Organic Frameworks (MOFs): Self-Photoemission of a
 Highly Stable Thorium MOF.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14144
_journal_page_last               14149
_journal_paper_doi               10.1021/jacs.8b07113
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C24 H12 O8 Th'
_chemical_formula_sum            'C24 H12 O8 Th'
_chemical_formula_weight         660.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.913(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7914(5)
_cell_length_b                   22.1948(6)
_cell_length_c                   12.5214(3)
_cell_measurement_reflns_used    6290
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      61.8390
_cell_measurement_theta_min      4.2990
_cell_volume                     4677.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2890
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -59.00  18.00   1.00   10.00    --    0.00 -37.00  90.00   77
  2  \w    -20.00  74.00   1.00   10.00    --    0.00  37.00 -90.00   94
  3  \w   -102.00 -59.00   1.00   30.00    --  -72.00  80.00  15.38   43
  4  \w    -95.00 -70.00   1.00   30.00    --  -72.00  80.00 -97.22   25
  5  \w    -92.00 -51.00   1.00   30.00    --  -72.00  80.00  95.25   41
  6  \w    -84.00 -58.00   1.00   30.00    --  -72.00  80.00 126.40   26
  7  \w    -97.00 -64.00   1.00   30.00    --  -72.00  80.00 174.09   33
  8  \w   -103.00 -77.00   1.00   30.00    --  -72.00  77.00 -60.00   26
  9  \w      9.00  35.00   1.00   30.00    --   82.02 -65.00-172.83   26
 10  \w     64.00  98.00   1.00   30.00    --   82.02 -61.00 -60.00   34
 11  \w     55.00 111.00   1.00   30.00    --   82.02 -68.00 103.38   56
 12  \w     62.00 157.00   1.00   30.00    --   82.02  30.00 -90.00   95
 13  \w     49.00 106.00   1.00   30.00    --   82.02 -61.00   0.00   57
 14  \w     81.00 156.00   1.00   30.00    --   82.02  77.00 -60.00   75
 15  \w     57.00  83.00   1.00   30.00    --   82.02 -61.00  60.00   26
 16  \w    128.00 154.00   1.00   30.00    --   82.02  77.00-120.00   26
 17  \w     49.00  81.00   1.00   30.00    --   82.02  77.00-120.00   32
 18  \w     45.00 134.00   1.00   30.00    --   82.02 -15.00 -90.00   89
 19  \w     51.00 107.00   1.00   30.00    --   82.02  77.00 120.00   56
 20  \w     49.00 111.00   1.00   30.00    --   82.02 -61.00-120.00   62
 21  \w     65.00 102.00   1.00   30.00    --   82.02 -65.00-172.83   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0086565000
_diffrn_orient_matrix_UB_12      0.0658644000
_diffrn_orient_matrix_UB_13      -0.0332208000
_diffrn_orient_matrix_UB_21      0.0322119000
_diffrn_orient_matrix_UB_22      -0.0219017000
_diffrn_orient_matrix_UB_23      -0.0936056000
_diffrn_orient_matrix_UB_31      -0.0851894000
_diffrn_orient_matrix_UB_32      -0.0016022000
_diffrn_orient_matrix_UB_33      -0.0839646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14439
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        57.902
_diffrn_reflns_theta_max         57.902
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0237P)^2^+2.5825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2216
_reflns_number_total             3230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07113_si_001.cif
_cod_data_source_block           th2
_cod_database_code               4132883
_chemical_oxdiff_formula         Th(C12H6O4)2
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C6A(H6A), C8A(H8A), C9A(H9A), C3B(H3B), C5B(H5B),
 C6B(H6B), C3C(H3C), C5C(H5C), C6C(H6C), C11A(H11A)
;
_shelx_res_checksum              85710
_shelx_hkl_checksum              76142
_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 2.897
_oxdiff_exptl_absorpt_empirical_full_min 0.694