Lanthanide MOF-based luminescent sensor arrays for the detection of castration-resistant prostate cancer curing drugs and biomarkers.
Wang, Xinrui; Gopalsamy, Karuppasamy; Clavier, Gilles; Maurin, Guillaume; Ding, Bin; Tissot, Antoine; Serre, Christian; Chemical science 15 (2024) 6488–6499; doi:10.1039/d3sc06899d

data_1571302
_publ_section_title
;
 Lanthanide MOF-based luminescent sensor arrays for the detection of
 castration-resistant prostate cancer curing drugs and biomarkers.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              6488
_journal_page_last               6499
_journal_paper_doi               10.1039/d3sc06899d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C49.35 H33.25 Eu2 N9.45 O14'
_chemical_formula_sum            'C49.35 H33.25 Eu2 N9.45 O14'
_chemical_formula_weight         1286.52
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.363(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6951(13)
_cell_length_b                   13.7413(6)
_cell_length_c                   35.681(3)
_cell_measurement_reflns_used    7086
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2430
_cell_measurement_theta_min      3.0300
_cell_volume                     10909.4(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5479
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -6.00  23.00   1.00   14.15    --  -10.77 -99.00-120.00   29
  2  \w    -55.00  40.00   1.00   14.15    --   11.63 -57.00 -30.00   95
  3  \w     -2.00  75.00   1.00   14.15    --   11.63  38.00 150.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0050171000
_diffrn_orient_matrix_UB_12      -0.0508751000
_diffrn_orient_matrix_UB_13      -0.0007251000
_diffrn_orient_matrix_UB_21      -0.0257949000
_diffrn_orient_matrix_UB_22      -0.0045993000
_diffrn_orient_matrix_UB_23      -0.0147651000
_diffrn_orient_matrix_UB_31      0.0180272000
_diffrn_orient_matrix_UB_32      0.0076085000
_diffrn_orient_matrix_UB_33      -0.0138741000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25053
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.742
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             5068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.296
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9600
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0397P)^2^+115.8661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7813
_reflns_number_total             9600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06899d2.cif
_cod_data_source_block           a221012d_sq
_cod_depositor_comments
'Adding full bibliography for 1571301--1571302.cif.'
_cod_original_cell_volume        10909.4(11)
_cod_database_code               1571302
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N7A-C35 = N7-C35
 1.45 with sigma of 0.01
 O13-C49
 1.15 with sigma of 0.01
 C51-C50
 2.2 with sigma of 0.01
 N10-C51 = N10-C50
 1.5 with sigma of 0.01
 N10-C49
 1.32 with sigma of 0.01
 O13-C49 \\sim O13A-C49
 with sigma of 0.02
 Eu2-O13 \\sim Eu2-O13A
 with sigma of 0.02
 C51-C49 \\sim C49-C50
 with sigma of 0.001
3. Restrained planarity
 N10, C49, C50, C51
 with sigma of 0.001
 N7, N8, N9, C33, C34
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
O13 \\sim N10 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C28 \\sim C29 \\sim C30 \\sim C25 \\sim C26 \\sim C27: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(N9A) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C34A) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(O13) = Uanis(O13A)
Uanis(N7A) = Uanis(N7)
Uanis(N8A) = Uanis(N8)
Uanis(C33A) = Uanis(C33)
Uanis(N9) = Uanis(N9A)
Uanis(C34) = Uanis(C34A)
5. Others
 Sof(N7A)=Sof(C34A)=Sof(H34A)=Sof(N9A)=Sof(C33A)=Sof(H33A)=Sof(N8A)=1-FVAR(1)
 Sof(N7)=Sof(N8)=Sof(C33)=Sof(H33)=Sof(N9)=Sof(C34)=Sof(H34)=FVAR(1)
 Fixed Sof: O13(0.45) N10(0.45) C49(0.45) H49(0.45) C50(0.45) H50A(0.45)
 H50B(0.45) H50C(0.45) C51(0.45) H51A(0.45) H51B(0.45) H51C(0.45) O13A(0.55)
 H13A(0.55) H13B(0.55)
6.a Riding coordinates:
 O14(H14A,H14B), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), O13A(H13A,H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C28(H28),
  C30(H30), C36(H36), C37(H37), C39(H39), C40(H40), C42(H42), C44(H44),
 C46(H46), C33(H33), C34(H34), C49(H49), C34A(H34A), C33A(H33A)
6.c Fitted pentagon refined as free rotating group:
 N7(N8,C33,N9,C34), N7A(C34A,N9A,C33A,N8A)
;
_shelx_res_checksum              53178
_shelx_fab_checksum              39538
_platon_squeeze_void_probe_radius 1.20
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.594