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_7718783
_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         '0.35(C1 H2 Cl2), C33 H29 N3 O4, 0.15(C2 H3 N)'
_chemical_formula_sum            'C33.65 H30.15 Cl0.7 N3.15 O4'
_chemical_formula_weight         567.47
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-18 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            8
_cell_length_a                   12.173(2)
_cell_length_b                   17.814(3)
_cell_length_c                   25.973(5)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      69.862
_cell_measurement_theta_min      3.011
_cell_volume                     5632.2(17)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            139091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         3.008
_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    1.303
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.8492.
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    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 4274 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10631
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                9984
_reflns_number_total             10631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00831j2.cif
_cod_data_source_block           etl146
_cod_depositor_comments
'Adding full bibliography for 7718781--7718783.cif.'
_cod_original_cell_volume        5632.3(18)
_cod_original_formula_sum        'C33.65 H30.15 Cl0.70 N3.15 O4'
_cod_database_code               7718783
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.676
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C68
 1.14 with sigma of 0.02
 C68-N7
 1.137 with sigma of 0.01
 C68-C69
 1.456 with sigma of 0.01
 C69-N7
 2.593 with sigma of 0.02
 N7-C69
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N7 \\sim C68 \\sim C69: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(N7) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N7, C68, C69
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.1
5. Others
 Fixed Sof: Cl1(0.7) Cl2(0.7) C67(0.7) H67A(0.7) H67B(0.7) N7(0.3) C68(0.3)
 C69(0.3) H69A(0.3) H69B(0.3) H69C(0.3)
6.a Ternary CH refined with riding coordinates:
 C53(H53), C44(H44), C11(H11), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C42(H42), C56(H56), C4(H4), C3(H3A), C63(H63), C50(H50),
 C57(H57), C58(H58), C48(H48), C25(H25), C2(H2), C35(H35), C28(H28), C41(H41),
 C30(H30), C62(H62), C36(H36), C24(H24), C9(H9), C60(H60), C23(H23), C27(H27),
 C29(H29), C61(H61), C6(H6), C7(H7), C37(H37), C8(H8), C39(H39), C40(H40)
6.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C54(H54A,H54B,
 H54C), C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              92646
_shelx_hkl_checksum              95064
_olex2_date_sample_data_collection 2022-04-12
_olex2_submission_original_sample_id TGG2021
_olex2_submission_special_instructions 'No special instructions were received'