Synthesis and luminescence studies of lanthanide complexes (Gd, Tb, Dy) with phenyl- and 2-pyridylthiolates supported by a bulky β-diketiminate ligand. Impact of the ligand environment on terbium(iii) emission
Mironova, Olga A.; Ryadun, Aleksey A.; Sukhikh, Taisiya S.; Konchenko, Sergey N.; Pushkarevsky, Nikolay A.; New Journal of Chemistry 44 (2020) 19769–19779; doi:10.1039/D0NJ04201C

data_7060080
_publ_section_title
;
 Synthesis and luminescence studies of lanthanide complexes (Gd, Tb, Dy)
 with phenyl- and 2-pyridylthiolates supported by a bulky \b-diketiminate
 ligand. Impact of the ligand environment on terbium(iii) emission
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19769
_journal_page_last               19779
_journal_paper_doi               10.1039/D0NJ04201C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C39 H49 Dy N4 S2, 0.34(C4 H8 O)'
_chemical_formula_sum            'C40.38 H51.76 Dy N4 O0.34 S2'
_chemical_formula_weight         825.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-01 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.257(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8956(5)
_cell_length_b                   19.6998(7)
_cell_length_c                   15.2240(7)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.26
_cell_volume                     3861.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29367
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.728
_diffrn_reflns_theta_min         1.692
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0565 before and 0.0419 after correction. The Ratio of minimum to maximum transmission is 0.8817. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             1691
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7362
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0156P)^2^+3.4001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6282
_reflns_number_total             7362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04201c2.cif
_cod_data_source_block           moa44
_cod_depositor_comments
'Adding full bibliography for 7060074--7060081.cif.'
_cod_database_code               7060080
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.604
_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
 C1S-C2S \\sim C2S-C3S \\sim C3S-C4S
 with sigma of 0.02
 C2S-C4S \\sim C1S-C3S
 with sigma of 0.04
 O1S-C1S \\sim O1S-C4S
 with sigma of 0.02
 O1S-C2S \\sim O1S-C3S
 with sigma of 0.04
3. Others
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              43119
_olex2_submission_special_instructions 'No special instructions were received'