Tuning the luminescence efficiency by perfluorination of side chains in Eu3+ complexes with β-diketones of the thiophene series
Varaksina, Evgeniya A.; Kiskin, Mikhail A.; Lyssenko, Konstantin A.; Puntus, Lada N.; Korshunov, Vladislav M.; Silva, Gustavo S.; Freire, Ricardo O.; Taydakov, Ilya V.; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP02951G

data_7243900
_publ_section_title
;
 Tuning the luminescence efficiency by perfluorination of side chains in
 Eu3+ complexes with \b-diketones of the thiophene series
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP02951G
_journal_year                    2021
_chemical_formula_moiety
'0.5(C36 H20 Eu F9 N2 O6 S2.78), 0.5(C36 H19 Eu F9 N2 O6 S2.614), C3 H6 O, 0.303(S)'
_chemical_formula_sum            'C39 H26 Eu F9 N2 O7 S3'
_chemical_formula_weight         1053.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.992(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8914(5)
_cell_length_b                   10.6986(5)
_cell_length_c                   38.1886(18)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.18
_cell_volume                     4041.3(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            42018
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.600
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0980 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.7865.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2088
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.291
_refine_diff_density_min         -2.857
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         19911
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0556
_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^)+7.3898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                16463
_reflns_number_total             19911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp02951g2.cif
_cod_data_source_block           3_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7243900
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.982(12)
 0.018(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S2-C12 = S2-C15
 1.7 with sigma of 0.01
 S2A-C12 = S2A-C14
 1.7 with sigma of 0.01
 S5-C48 = S5-C51
 1.7 with sigma of 0.01
 S5A-C48 = S5A-C50
 1.7 with sigma of 0.01
 S4-C40 = S4-C43
 1.7 with sigma of 0.01
 S4A-C40 = S4A-C42
 1.7 with sigma of 0.01
 C41-C42 = C42-C43
 1.39 with sigma of 0.01
 C40-C41
 1.34 with sigma of 0.01
 C13-C14 = C14-C15
 1.39 with sigma of 0.01
 C12-C13
 1.34 with sigma of 0.01
 C49-C50 = C50-C51
 1.39 with sigma of 0.01
 C48-C49
 1.34 with sigma of 0.01
4. Restrained planarity
 S4, C40, C41, C42, C43
 with sigma of 0.01
 S5, C48, C49, C50, C51
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C41) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C49) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(S2) = Uanis(S2A)
Uanis(S4) = Uanis(S4A)
Uanis(S5) = Uanis(S5A)
6. Rigid body (RIGU) restrains
 C21, C20, C21, C22
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C41, C42, C41, C40
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C16, F4, C16, F5, C16, F6
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C26, C25, C26, C27
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C52, F13, C52, F14, C52, F15
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C44, F10, C44, F11, C44, F12
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C24, F7, C24, F8, C24, F9
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C13, C12, C13, C14
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C48, C49, C49, C50
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
 C63, C62, C63, C64
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.016
7. Others
 Sof(S5A)=1-FVAR(1)
 Sof(S5)=FVAR(1)
 Sof(S4A)=1-FVAR(2)
 Sof(S4)=FVAR(2)
 Sof(S2A)=1-FVAR(3)
 Sof(S2)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C38(H38), C43(H43), C62(H62), C57(H57), C21(H21), C54(H54),
 C78(H78), C23(H23), C61(H61), C25(H25), C15(H15), C2(H2), C36(H36), C32(H32),
 C02D(H02D), C51(H51), C67(H67), C35(H35), C66(H66), C7(H7), C6(H6), C30(H30),
 C63(H63), C59(H59), C27(H27), C31(H31), C71(H71), C46(H46), C58(H58), C42(H42),
  C41(H41), C50(H50), C72(H72), C13(H13), C22(H22), C18(H18), C10(H10), C14(H14)
8.b Idealised Me refined as rotating group:
 C5S(H5SA,H5SB,H5SC), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C6S(H6SA,H6SB,
 H6SC)
;
_shelx_res_checksum              89704
_olex2_submission_special_instructions 'No special instructions were received'