Hierarchical lanthanide-based self-assembly complexes that undergo reversible luminescent response to both temperature changes and chemical reactions within competitive media.
Gorai, Tumpa; Lovitt, June I.; Twamley, Brendan; Luis, Ena T.; Gunnlaugsson, Thorfinnur; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10022–10029; doi:10.1039/d5dt00831j

data_7718781
_publ_section_title
;
 Hierarchical lanthanide-based self-assembly complexes that undergo
 reversible luminescent response to both temperature changes and chemical
 reactions within competitive media.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10022
_journal_page_last               10029
_journal_paper_doi               10.1039/d5dt00831j
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C2 H7 O S), 2(C31 H27 N3 O3)'
_chemical_formula_sum            'C66 H69 N6 O8 S2'
_chemical_formula_weight         1138.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2792(4)
_cell_length_b                   16.8732(6)
_cell_length_c                   26.4228(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      59.85
_cell_measurement_theta_min      3.11
_cell_volume                     5920.4(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Apex Kappa Duo Imus CuKa'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       APEX2
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1631
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            106332
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        62.736
_diffrn_reflns_theta_max         62.736
_diffrn_reflns_theta_min         3.107
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.59
_diffrn_source_power             0.0293053
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           49.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1286 before and 0.0946 after correction. The Ratio of minimum to maximum transmission is 0.8208. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(16)
_refine_ls_extinction_coef       0.00200(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         9355
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0882P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                6939
_reflns_number_total             9355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00831j2.cif
_cod_data_source_block           jil117
_cod_depositor_comments
'Adding full bibliography for 7718781--7718783.cif.'
_cod_database_code               7718781
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H65-H42
 2.2 with sigma of 0.02
 H5-H60
 2.2 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C71(H71), C26(H26), C48(H48), C11(H11)
3.b Aromatic/amide H refined with riding coordinates:
 N70(H70), N10(H10), N25(H25), N47(H47), C74(H74), C40(H40), C75(H75),
 C19(H19), C6(H6), C43(H43), C82(H82), C76(H76), C31(H31), C30(H30), C79(H79),
 C3(H3), C14(H14), C29(H29), C34(H34), C15(H15), C81(H81), C22(H22), C20(H20),
 C51(H51), C21(H21), C35(H35), C57(H57), C52(H52), C53(H53), C56(H56), C16(H16),
  C37(H37), C80(H80), C59(H59), C36(H36), C58(H58)
3.c Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C27(H27A,H27B,H27C), C12(H12A,H12B,H12C), C49(H49A,H49B,
 H49C), C67(H67A,H67B,H67C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C66(H66A,
 H66B,H66C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O42(H42), O60(H60), O65(H65)
;
_shelx_res_checksum              35781
_shelx_hkl_checksum              73952
_olex2_submission_special_instructions 'No special instructions were received'