Ratiometric fluorescent detection of dipicolinic acid as an anthrax biomarker based on a high-nuclearity Yb18 nanoring
Ma, Yanan; Yang, Xiaoping; Hao, Wenxin; Zhu, Ting; Wang, Chengri; Schipper, Desmond; Dalton Transactions  (2021) –; doi:10.1039/D1DT01731D

data_7708140
_publ_section_title
;
 Ratiometric fluorescent detection of dipicolinic acid as an anthrax
 biomarker based on a high-nuclearity Yb18 nanoring
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01731D
_journal_year                    2021
_chemical_formula_moiety         'C21 H25 Al Li N3 O'
_chemical_formula_sum            'C21 H25 Al Li N3 O'
_chemical_formula_weight         369.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-11 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                81.015(6)
_cell_angle_beta                 76.374(7)
_cell_angle_gamma                60.358(7)
_cell_formula_units_Z            2
_cell_length_a                   10.0339(8)
_cell_length_b                   10.0431(6)
_cell_length_c                   15.9941(12)
_cell_measurement_reflns_used    2865
_cell_measurement_temperature    220.0(4)
_cell_measurement_theta_max      74.1030
_cell_measurement_theta_min      5.0490
_cell_volume                     1359.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -64.00  33.00   1.00    5.24    --  -41.06  37.00-150.00   97
  2  \w   -107.00 -17.00   1.00    5.24    --  -41.06 -37.00  30.00   90
  3  \w    -64.00  -8.00   1.00    5.24    --  -41.06  77.00 -60.00   56
  4  \w      1.00  29.00   1.00    5.24    --  -41.06  77.00 -60.00   28
  5  \w     97.00 130.00   1.00    5.24    --   41.06 178.00-180.00   33
  6  \w     56.00  85.00   1.00    5.24    --   41.06-178.00  60.00   29
  7  \w     91.00 121.00   1.00    5.24    --   41.06 178.00 -90.00   30
  8  \w     97.00 175.00   1.00   20.97    --  110.01  30.00 -30.00   78
  9  \w    129.00 166.00   1.00   20.97    --  110.01  30.00   0.00   37
 10  \w     49.00 138.00   1.00   20.97    --  110.01 -30.00 150.00   89
 11  \w     85.00 110.00   1.00   20.97    --  110.01 -94.00  30.00   25
 12  \w     41.00 137.00   1.00   20.97    --  110.01 -61.00-120.00   96
 13  \w     30.00  55.00   1.00   20.97    --  110.01 -94.00  30.00   25
 14  \w     85.00 152.00   1.00   20.97    --  110.01  77.00  30.00   67
 15  \w     84.00 116.00   1.00   20.97    --  110.01-125.00 -30.00   32
 16  \w     50.00 138.00   1.00   20.97    --  110.01 -30.00   0.00   88
 17  \w     47.00  99.00   1.00   20.97    --  110.01 -94.00 120.00   52
 18  \w     27.00  89.00   1.00   20.97    --  110.01 -94.00-150.00   62
 19  \w    125.00 152.00   1.00   20.97    --  110.01 125.00 -90.00   27
 20  \w     90.00 118.00   1.00   20.97    --  110.01-125.00-180.00   28
 21  \w     85.00 135.00   1.00   20.97    --  110.01 -77.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1410485000
_diffrn_orient_matrix_UB_12      -0.0715721000
_diffrn_orient_matrix_UB_13      0.0457784000
_diffrn_orient_matrix_UB_21      -0.0953472000
_diffrn_orient_matrix_UB_22      0.1189903000
_diffrn_orient_matrix_UB_23      0.0698300000
_diffrn_orient_matrix_UB_31      -0.0576200000
_diffrn_orient_matrix_UB_32      -0.1092577000
_diffrn_orient_matrix_UB_33      0.0535968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         5.073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_recrystallization_method THF/toluene
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.051
_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     256
_refine_ls_number_reflns         4778
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1679P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3543
_reflns_number_total             4778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01731d2.cif
_cod_data_source_block           agr2977
_cod_original_cell_volume        1359.90(19)
_cod_database_code               7708140
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H25 Al Li N3 O'
_chemical_oxdiff_usercomment     'white block'
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.728
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
O1S \\sim C3S \\sim C2S \\sim C5S \\sim C4S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Others
 Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1(H1BC,H1BD), C5S(H5SA,H5SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 86 electrons were found in a volume of 376 cubic angstroms in 1 void per unit cell. 
The crystallization solvent was THF/toluene and this is consistent with the presence of 2THF per Unit Cell which account for 80 electrons per unit cell and is also consistent with the NMR data.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24620
_shelx_hkl_checksum              54898
_shelx_fab_checksum              3064
_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 1.669
_oxdiff_exptl_absorpt_empirical_full_min 0.729