Covert MOF-Based Photoluminescent Tags via Tunable Linker Energetics.
Deneff, Jacob I.; Rohwer, Lauren E. S.; Butler, Kimberly S.; Valdez, Nichole R.; Rodriguez, Mark A.; Luk, Ting S.; Sava Gallis, Dorina F.; ACS applied materials & interfaces 14 (2022) 3038–3047; doi:10.1021/acsami.1c20432

data_4519276
_publ_section_title
;
 Covert MOF-Based Photoluminescent Tags via Tunable Linker Energetics.
;
_journal_issue                   2
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              3038
_journal_page_last               3047
_journal_paper_doi               10.1021/acsami.1c20432
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C132 Nd4.023 O36.571 Yb5.648'
_chemical_formula_sum            'C132 Nd4.17 O36.77 Yb5.9'
_chemical_formula_weight         3796.06
_space_group_crystal_system      trigonal
_space_group_IT_number           156
_space_group_name_Hall           'P 3 -2"'
_space_group_name_H-M_alt        'P 3 m 1'
_audit_creation_date             2021-06-24
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   21.8128(3)
_cell_length_b                   21.8128(3)
_cell_length_c                   16.9894(4)
_cell_measurement_reflns_used    9450
_cell_measurement_temperature    283.0
_cell_measurement_theta_max      74.01
_cell_measurement_theta_min      4.82
_cell_volume                     7000.5(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      283.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1404
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            100611
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.163
_diffrn_reflns_theta_min         4.818
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.551
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.7239.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.900
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1749
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.803
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.495(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         9870
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1427P)^2^+19.7376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2415
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                7891
_reflns_number_total             9870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c20432_si_003.cif
_cod_data_source_block           phase1_tbap_p3ml_b
_cod_original_cell_volume        7000.5(3)
_cod_original_formula_sum        'C132 Nd4.17 O36.77 Yb5.90'
_cod_database_code               4519276
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.251
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(10)
 0.495(10)
2. Restrained distances
 Yb5A-O51A
 2.42 with sigma of 0.02
 Yb4A-O41A \\sim Yb5A-O51A
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma of 0.1
 C7, C71, C72, C73, C74, C75, C76, C77
 with sigma of 0.1
 C8, C81, C82, C83, C84, C85, C86, C87
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uiso(O2A) = Uiso(O2B)
Uiso(O41A) = Uiso(O51A)
Uanis(O3A) = Uanis(O5)
Uanis(O1A) = Uanis(O5)
Uanis(O1A) = Uanis(O3A)
6. Others
 Sof(O78B)=Sof(O79B)=Sof(O88B)=Sof(O89B)=1-FVAR(1)
 Sof(Nd1B)=Sof(Nd2B)=Sof(Nd3B)=0.5*(1-FVAR(2))
 Sof(O2B)=0.125*(1-FVAR(2))
 Sof(O2A)=0.125*FVAR(2)
 Sof(Yb1A)=Sof(O1A)=Sof(Yb2A)=Sof(Yb3A)=Sof(O3A)=0.5*FVAR(2)
 Sof(O78A)=Sof(O79A)=Sof(O88A)=Sof(O89A)=FVAR(1)
 Sof(O41A)=Sof(O51A)=0.125*FVAR(3)
 Sof(Yb4A)=Sof(Yb5A)=0.16667*FVAR(3)
7.a Fitted hexagon refined as free rotating group:
 C71(C72,C73,C74,C75,C76), C81(C82,C83,C84,C85,C86)
;
_olex2_exptl_crystal_mounting_method 'fluorolube on MiTeGen mount'
_olex2_submission_original_sample_id 'Phase 1 TBAP Nd Yb'
_olex2_submission_special_instructions 'No special instructions were received'