Synthesis, characterization, luminescence properties and deciphering the role of a terpyridyl-imidazole based ligand in the dissimilar luminescence sensitization of ternary lanthanide(iii) tris-(β-diketonate) complexes
Ahmed, Toushique; Chakraborty, Amit; Paul, Animesh; Baitalik, Sujoy; Dalton Transactions  (2023) –; doi:10.1039/D3DT01701J

data_7713998
_publ_section_title
;
 Synthesis, characterization, luminescence properties and deciphering the
 role of a terpyridyl-imidazole based ligand in the dissimilar
 luminescence sensitization of ternary lanthanide(iii)
 tris-(\b-diketonate) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01701J
_journal_year                    2023
_chemical_formula_moiety         '(C52 H34 F6 N5 O5 S2 Tb), (Cl)'
_chemical_formula_sum            'C52 H34 Cl F6 N5 O5 S2 Tb'
_chemical_formula_weight         1181.34
_chemical_melting_point          465
_chemical_name_systematic        Monoclinic
_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             2023-04-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-04-10 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.586(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9321(3)
_cell_length_b                   25.1480(7)
_cell_length_c                   40.0049(11)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    108.0
_cell_measurement_theta_max      47.79
_cell_measurement_theta_min      3.52
_cell_volume                     10976.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      108.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1652
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            117779
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.412
_diffrn_reflns_theta_min         2.213
_exptl_absorpt_coefficient_mu    8.086
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             4712
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.854
_refine_diff_density_min         -2.594
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9791
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1276
_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^)+(0.0690P)^2^+413.4437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2638
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8236
_reflns_number_total             9791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01701j2.cif
_cod_data_source_block           17_a
_cod_original_formula_sum        'C52 H34 Cl F6 N5 O5 S2 Tb '
_cod_database_code               7713998
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.358
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Tb1-H5A \\sim Tb1-H5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.002
Uanis(F5) = Uanis(C44)
Uanis(C8) = Uanis(C16)
4.a Free rotating group:
 O5(H5A,H5B)
4.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
4.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C7(H7), C50(H50), C9(H9), C4(H4), C42(H42), C21(H21), C2(H2),
 C18(H18), C20(H20), C37(H37), C29(H29), C38(H38), C3(H3), C15(H15), C1(H1),
 C17(H17), C39(H39), C33(H33), C12(H12), C36(H36), C26(H26), C28(H28), C46(H46),
  C35(H35), C14(H14), C34(H34), C13(H13), C45(H45), C27(H27)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73206
_shelx_fab_checksum              25236
_olex2_submission_special_instructions 'No special instructions were received'