Luminescence "Turn-On" Detection of Gossypol using Ln3±Based Metal-Organic Frameworks and Ln Salts.
Luo, Tian-Yi; White, David L.; Liu, Chong; Star, Alexander; Rosi, Nathaniel L.; Das, Prasenjit; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11429

data_4134111
_publ_section_title
;
 Luminescence &quot;Turn-On&quot; Detection of Gossypol using Ln3+-Based
 Metal-Organic Frameworks and Ln Salts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11429
_journal_year                    2020
_chemical_formula_moiety         '0.5(C240 H144 N24 O67.76 Yb12)'
_chemical_formula_sum            'C120 H72 N12 O33.88 Yb6'
_chemical_formula_weight         3262.21
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.4692(14)
_cell_length_b                   33.4692(14)
_cell_length_c                   33.4692(14)
_cell_measurement_reflns_used    9223
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      51.18
_cell_measurement_theta_min      2.29
_cell_volume                     37492(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.619
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1353
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.619
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16692
_diffrn_reflns_point_group_measured_fraction_full 0.619
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.173
_diffrn_reflns_theta_min         2.286
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.5304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1224 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.7071. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.578
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             6268
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1076
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0983
_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^)+(0.1569P)^2^+617.4092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2754
_refine_ls_wR_factor_ref         0.2831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                929
_reflns_number_total             1076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11429_si_002.cif
_cod_data_source_block           lty_5_62_4_0m_a
_cod_original_cell_volume        37492(5)
_cod_database_code               4134111
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C3-C2 = C4-C3 = C5-C4 = C7-C6
 1.38 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.25) H1A(0.25) H1B(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'