Exploring the luminescent and thermometric potentials of samarium(III) diketonate complexes with extended fluoroalkyl chains.
Metlina, Daria A.; Metlin, Mikhail T.; Korshunov, Vladislav M.; Gontcharenko, Victoria E.; Avetisov, Roman I.; Kiskin, Mikhail A.; Belousov, Yuriy A.; Taydakov, Ilya V.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3812–3826; doi:10.1039/d4dt03262d

data_7717869
_publ_section_title
;
 Exploring the luminescent and thermometric potentials of samarium(III)
 diketonate complexes with extended fluoroalkyl chains.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3812
_journal_page_last               3826
_journal_paper_doi               10.1039/d4dt03262d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C42 H20 F21 N2 O6 S3 Sm'
_chemical_formula_sum            'C42 H20 F21 N2 O6 S3 Sm'
_chemical_formula_weight         1294.13
_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
_audit_creation_date             2024-11-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-05 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9132(3)
_cell_length_b                   18.4956(4)
_cell_length_c                   21.5050(5)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.39
_cell_volume                     4655.80(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.059
_diffrn_source_current           0.9
_diffrn_source_power             0.045
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.6478
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.9188.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         10268
_refine_ls_number_restraints     644
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_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^+20.5895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7854
_reflns_number_total             10268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03262d2.cif
_cod_data_source_block           smp
_cod_depositor_comments
'Adding full bibliography for 7717869--7717871.cif.'
_cod_database_code               7717869
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C27-C24 = C27-C26
 1.43 with sigma of 0.02
 C27-C26 = C27-C24
 1.43 with sigma of 0.02
 C27'-C26' = C27'-C24
 1.43 with sigma of 0.02
 F6A'-C20' = F6B-C20 = F6-C20 = F6B'-C20' = F6'-C20' = F6A-C20 = F5A-C19 = F5-
 C19 = F4-C18 = F4A-C18
 1.34 with sigma of 0.02
 C18-C13 = C18'-C13'
 1.48 with sigma of 0.02
 C20'-C19' = C20-C19 = C19'-C18' = C19-C18 = C18'-C13' = C18-C13
 1.51 with sigma of 0.02
 F4'-C18' = F4A'-C18' = F5A'-C19' = F5'-C19'
 1.34 with sigma of 0.02
 F4A'-F4'
 2.1 with sigma of 0.02
 F5A'-F5'
 2.1 with sigma of 0.02
 F8'-C29' = F8A'-C29'
 1.34 with sigma of 0.02
 F8'-F8A'
 2.1 with sigma of 0.02
 C29'-C28 = C29-C28
 1.51 with sigma of 0.02
 F10-F48
 2.1 with sigma of 0.02
 C29-C28 = C29'-C28
 1.51 with sigma of 0.02
 F48-F10
 2.1 with sigma of 0.01
 F10-C29 = F48-C29
 1.34 with sigma of 0.01
 C29-C30'
 1.52 with sigma of 0.01
 C29'-C30'
 1.52 with sigma of 0.02
 C29-C28 = C30-C29
 1.52 with sigma of 0.02
 F9-C30 = F17-C30 = F16-C30
 1.34 with sigma of 0.02
 F17-F16
 2.1 with sigma of 0.02
 F16-F9
 2.1 with sigma of 0.02
 F17-F9
 2.1 with sigma of 0.02
 C28-C30
 2.47 with sigma of 0.02
 C28-C30'
 2.47 with sigma of 0.02
 F9B'-C30' = F9A'-C30' = F9'-C30'
 1.34 with sigma of 0.02
 F9'-F9B'
 2.1 with sigma of 0.02
 F9B'-F9A'
 2.1 with sigma of 0.02
 F9'-F9A'
 2.1 with sigma of 0.02
 C8-F1 \\sim C8-F1A \\sim C9-F2 \\sim C9-F2A \\sim C10-F3 \\sim C10-F3A \\sim
C10-F3B
 with sigma of 0.02
 C18-F4 \\sim C18-F4A \\sim C19-F5 \\sim C19-F5A \\sim C20-F6 \\sim C20-F6A
\\sim C20-F6B
 with sigma of 0.02
 F1-F1A \\sim F2-F2A \\sim F3-F3A \\sim F3-F3B \\sim F3A-F3B
 with sigma of 0.02
 F4-F4A \\sim F5-F5A \\sim F6-F6A \\sim F6-F6B \\sim F6A-F6B
 with sigma of 0.02
 C8-C9 \\sim C9-C10 \\sim C18-C19 \\sim C19-C20
 with sigma of 0.02
 C8-C10 \\sim C18-C20
 with sigma of 0.02
 C3-C9 \\sim C13-C19
 with sigma of 0.02
 C3-F1 \\sim C3-F1A \\sim C13-F4 \\sim C13-F4A
 with sigma of 0.02
 C9-F1 \\sim C9-F1A \\sim C19-F4 \\sim C19-F4A
 with sigma of 0.02
 C8-F2 \\sim C8-F2A \\sim C18-F5 \\sim C18-F5A
 with sigma of 0.02
 C10-F2 \\sim C10-F2A \\sim C20-F5 \\sim C20-F5A
 with sigma of 0.02
 C8-F3 \\sim C9-F3A \\sim C9-F3B \\sim C19-F6 \\sim C19-F6A \\sim C19-F6B
 with sigma of 0.02
 C24-C27 \\sim C24-C27'
 with sigma of 0.02
 C24-S3 \\sim C24-S3'
 with sigma of 0.02
 C25-C26 \\sim C25'-C26'
 with sigma of 0.02
 C25-S3 \\sim C25'-S3'
 with sigma of 0.02
 C26-C27 \\sim C26'-C27'
 with sigma of 0.02
 C24-C25 \\sim C24-C25'
 with sigma of 0.04
 C24-C26 \\sim C24-C26'
 with sigma of 0.04
 C25-C27 \\sim C25'-C27'
 with sigma of 0.04
 C26-S3 \\sim C26'-S3'
 with sigma of 0.04
 C13-C12 \\sim C12'-C13'
 with sigma of 0.02
 C12-C11 \\sim C12'-C11
 with sigma of 0.02
 O4'-C13' \\sim O4-C13
 with sigma of 0.02
3. Restrained planarity
 C24, C25, C26, C27, S3
 with sigma of 0.1
 C24, S3', C25', C26', C27'
 with sigma of 0.1
 O4', C13', C12', C11, O3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27 \\sim S3' \\sim C25' \\sim C26' \\sim C27' \\sim S3:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(S3)
\\sim Ueq, Uanis(S3') \\sim Ueq, Uanis(C25') \\sim Ueq, Uanis(C26') \\sim Ueq,
Uanis(C27') \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(F4)
\\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq,
Uanis(F6A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(C18')
\\sim Ueq, Uanis(C19') \\sim Ueq, Uanis(C20') \\sim Ueq, Uanis(F6') \\sim Ueq,
Uanis(F6A') \\sim Ueq, Uanis(F6B') \\sim Ueq, Uanis(F4A') \\sim Ueq,
Uanis(F5A') \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F4') \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C13') \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C12') \\sim Ueq:
with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(F8') \\sim Ueq, Uanis(F8A') \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F48)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C29') \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(F8A') \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F48) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C29') \\sim Ueq, Uanis(C30') \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(F9B')
\\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F9A') \\sim Ueq, Uanis(F8') \\sim Ueq:
with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C13) = Uanis(C12) = Uanis(C12') = Uanis(C13') = Uanis(C18') = Uanis(C18)
5. Rigid body (RIGU) restrains
 C18, C19, C19, C20
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C18, F4, C18, F4A, C19, F5, C19, F5A, C20, F6, C20, F6A, C20, F6B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C27, C24, C27, C26
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
6. Others
 Fixed Sof: O4(0.5) C12(0.5) H12(0.5) C13(0.5) C18(0.5) C19(0.5) C20(0.5)
 C25(0.7) H25(0.7) C26(0.7) H26(0.7) C27(0.7) H27(0.7) S3(0.7) F4(0.5) F4A(0.5)
 F5(0.5) F5A(0.5) F6A(0.5) F6(0.5) F6B(0.5) S3'(0.3) C25'(0.3) H25'(0.3)
 C26'(0.3) H26'(0.3) C27'(0.3) H27'(0.3) C18'(0.5) C19'(0.5) C20'(0.5) F6'(0.5)
 F6A'(0.5) F6B'(0.5) C13'(0.5) C12'(0.5) H12'(0.5) F4A'(0.5) F5A'(0.5) F5'(0.5)
 F4'(0.5) O4'(0.5) F8'(0.5) F8A'(0.5) F10(0.5) F48(0.5) C29(0.5) C29'(0.5)
 C30'(0.5) F9(0.5) F16(0.5) F17(0.5) C30(0.5) F9B'(0.5) F9'(0.5) F9A'(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C12(H12), C15(H15), C16(H16), C17(H17),
 C22(H22), C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C36(H36),
  C37(H37), C38(H38), C41(H41), C42(H42), C25'(H25'), C26'(H26'), C27'(H27'),
 C12'(H12')
;
_shelx_res_checksum              22130
_olex2_submission_special_instructions 'No special instructions were received'