New 1,4-naphthalenedicarboxylic acid- and 3,5-bis(benzimidazol-2-yl)pyridine-appended d<sup>10</sup>-configuration-based coordination polymers as recoverable turn-off luminescent sensors for tetracycline.
Xiao, Yao; Luo, Jing; Wang, Jun; Lu, Lu; Prakash, Om; Srivastava, Shreya; Muddassir, Mohd; Kumar, Abhinav; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5888–5895; doi:10.1039/d5dt00025d

data_7719018
_publ_section_title
;
 New 1,4-naphthalenedicarboxylic acid- and
 3,5-bis(benzimidazol-2-yl)pyridine-appended
 d<sup>10</sup>-configuration-based coordination polymers as recoverable
 turn-off luminescent sensors for tetracycline.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5888
_journal_page_last               5895
_journal_paper_doi               10.1039/d5dt00025d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C100 H68 Cd2 N20 O10, C50 H33.451 Cd N10 O4.725, C12 H8 O4, 0.275(H2 O)'
_chemical_formula_sum            'C162 H110 Cd3 N30 O19'
_chemical_formula_weight         3117.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-11-24 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   46.521(3)
_cell_length_b                   16.3691(8)
_cell_length_c                   21.6094(11)
_cell_measurement_reflns_used    5232
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.518
_cell_measurement_theta_min      2.573
_cell_volume                     16455.7(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1106
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49546
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.624
_diffrn_reflns_theta_min         2.301
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0604 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.8757.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             6352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         18355
_refine_ls_number_restraints     1026
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1444
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1108P)^2^+28.9294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.2131
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                10644
_reflns_number_total             18355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00025d2.cif
_cod_data_source_block           5_sq
_cod_original_cell_volume        16455.8(15)
_cod_database_code               7719018
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70(4)
 0.30(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 C17A-C24 = C17-C24 = C14-C13 = C14A-C13
 1.49 with sigma of 0.01
 O6-C13 = O5-C13 = O7-C24 = O8-C24
 1.27 with sigma of 0.01
 C29-C29_$1 = C28-C30_$1 = C30-C28_$1
 2.8 with sigma of 0.01
 C27-C26 = C28-C26 = C29-C28 = C30-C29 = C30-C30_$1 = C28-C28_$1 = C27-C27_$1
 1.39 with sigma of 0.01
 C26-C25
 1.48 with sigma of 0.01
 C26-C28_$1 = C28-C27 = C29-C30_$1
 2.4 with sigma of 0.01
 C30-C28
 2.4 with sigma of 0.01
 C26-C26_$1 = C28-C27_$1 = C28_$1-C27
 2.8 with sigma of 0.01
 O8-H23A
 2 with sigma of 0.02
 O12-H12A \\sim O12-H13A
 with sigma of 0.02
 O12-H12B \\sim O12-H13B
 with sigma of 0.02
 C13-C15A \\sim C13-C19A
 with sigma of 0.01
4. Restrained planarity
 C26, C28, C28_$1, C29_$1, C30_$1, C30, C29, C27, C27_$1, C26_$1
 with sigma of 0.01
5. Rigid bond restraints
 O12, O13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, O8, C24, O5, O6, C13, C17, C16, C15, C14, C19, C18, C23, C22, C21, C20,
 C17A, C16A, C15A, C14A, C19A, C18A, C23A, C22A, C21A, C20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, O9, C25, O10, C28, C27, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C65, C66, C67, C68, C63, C64, N8, C62, N7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C87, C82, C83, C84, C85, C86, N15, C81, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C36, N3, C38, C37, C42, C41, C40, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N10, C55, N9, C56, C57, C58, C59, C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cd1, O1, O2, C1, N6, N1, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O12 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O7 \\sim O8 \\sim C24 \\sim O5 \\sim O6 \\sim C13 \\sim C17 \\sim C16 \\sim C15
\\sim C14 \\sim C19 \\sim C18 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim
C17A \\sim C16A \\sim C15A \\sim C14A \\sim C19A \\sim C18A \\sim C23A \\sim
C22A \\sim C21A \\sim C20A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C27 \\sim O9 \\sim C25 \\sim C26 \\sim O10 \\sim C28 \\sim C29 \\sim C30:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N14 \\sim C81 \\sim N15 \\sim C83 \\sim C82 \\sim C87 \\sim C86 \\sim C85 \\sim
C84: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N8 \\sim C62 \\sim N7 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim
C68: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N2 \\sim C36 \\sim N3 \\sim C38 \\sim C37 \\sim C42 \\sim C41 \\sim C40 \\sim
C39: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N10 \\sim C55 \\sim N9 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim
C61: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N6 \\sim Cd1 \\sim O2 \\sim O1 \\sim C1 \\sim N1 \\sim O11: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C17A)
\\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C19A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C23A) \\sim Ueq,
Uanis(C22A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(Cd1) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
7. Others
 Sof(O13)=Sof(H13A)=Sof(H13B)=0.5*(1-FVAR(2))
 Sof(O12)=Sof(H12A)=Sof(H12B)=0.5*FVAR(2)
 Fixed Sof: C17(0.25) C16(0.25) H16(0.25) C15(0.25) H15A(0.25) C14(0.25)
 C19(0.25) C18(0.25) C23(0.25) H23(0.25) C22(0.25) H22(0.25) C21(0.25)
 H21(0.25) C20(0.25) H20(0.25) C17A(0.25) C16A(0.25) H16A(0.25) C15A(0.25)
 H15B(0.25) C14A(0.25) C19A(0.25) C18A(0.25) C23A(0.25) H23A(0.25) C22A(0.25)
 H22A(0.25) C21A(0.25) H21A(0.25) C20A(0.25) H20A(0.25)
8.a Riding coordinates:
 O13(H13A,H13B)
8.b Rotating group:
 O11(H11A,H11B)
8.c Aromatic/amide H refined with riding coordinates:
 N13(H13), N7(H7), N5(H5), N15(H15), N2(H2), C50(H50), C52(H52), C58(H58),
 C59(H59), C60(H60), C61(H61), N10(H10), C33(H33), C54(H54), C71(H71), C3(H3),
 C8(H8), C73(H73), C39(H39), C40(H40), C41(H41), C42(H42), C87(H87), C86(H86),
 C85(H85), C84(H84), C35(H35), C31(H31), C4(H4), C11(H11), C46(H46), C77(H77),
 C65(H65), C68(H68), C67(H67), C66(H66), C9(H9), C69(H69), C49(H49), C78(H78),
 C80(H80), C47(H47), C79(H79), C48(H48), C10(H10A), C16(H16), C15(H15A),
 C23(H23), C22(H22), C21(H21), C20(H20), C29(H29), C27(H27), C30(H30),
 C16A(H16A), C15A(H15B), C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A)
8.d Fitted hexagon refined as free rotating group:
 C56(C57,C58,C59,C60,C61), C37(C38,C39,C40,C41,C42), C82(C87,C86,C85,C84,C83),
 C65(C64,C63,C68,C67,C66)
8.e Tetrahedral OH refined with riding coordinates:
 O10(H10B)
8.f X=CH2 refined with riding coordinates:
 O12(H12A,H12B)
8.g Naphthalene refined as free rotating group:
 C17(C16,C15,C14,C19,C18,C23,C22,C21,C20), C17A(C16A,C15A,C14A,C19A,C18A,C23A,
 C22A,C21A,C20A)
;
_shelx_res_checksum              75093
_shelx_hkl_checksum              55312
_shelx_fab_checksum              69721
_olex2_submission_special_instructions 'No special instructions were received'