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_7060077
_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         'C37 H57 Gd I2 N2 O2, C4 H8 O'
_chemical_formula_sum            'C41 H65 Gd I2 N2 O3'
_chemical_formula_weight         1045.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.955(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2426(4)
_cell_length_b                   20.0490(9)
_cell_length_c                   10.6372(7)
_cell_measurement_reflns_used    3295
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.55
_cell_measurement_theta_min      2.79
_cell_volume                     2181.49(19)
_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 0.689
_diffrn_measured_fraction_theta_max 0.689
_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  0.0195
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.689
_diffrn_reflns_Laue_measured_fraction_max 0.689
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5152
_diffrn_reflns_point_group_measured_fraction_full 0.689
_diffrn_reflns_point_group_measured_fraction_max 0.689
_diffrn_reflns_theta_full        24.614
_diffrn_reflns_theta_max         24.614
_diffrn_reflns_theta_min         1.991
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.971
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0486 before and 0.0318 after correction. The Ratio of minimum to maximum transmission is 0.8116. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+4.7511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2366
_reflns_number_total             2613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04201c2.cif
_cod_data_source_block           moa74
_cod_depositor_comments
'Adding full bibliography for 7060074--7060081.cif.'
_cod_database_code               7060077
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4S-C3S \\sim C3S-C2S \\sim C2S-C1S
 with sigma of 0.02
 O1S-C4S \\sim O1S-C1S
 with sigma of 0.02
 O1S-C3S \\sim O1S-C2S
 with sigma of 0.04
 C3S-C1S \\sim C4S-C2S
 with sigma of 0.04
 C19-C18A \\sim C19-C18 \\sim C18A-C17A \\sim C18-C17 \\sim C17-C16 \\sim
C17A-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C18A) = Uiso(C17A)
4. Others
 Sof(H16C)=Sof(H16D)=Sof(H19C)=Sof(H19D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=
 Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H19A)=Sof(H19B)=FVAR(1)
 Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
 C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C16(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C19(H19C,H19D), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB),
 C4S(H4SA,H4SB), C18A(H18C,H18D), C17A(H17C,H17D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              40454
_olex2_submission_special_instructions 'No special instructions were received'