Eu(tta)<sub>3</sub>DPPZ-based organic light-emitting diodes: spin-coating <i>vs</i>. vacuum-deposition.
Kuznetsov, Kirill M.; Kozlov, Makarii I.; Aslandukov, Andrey N.; Vashchenko, Andrey A.; Medved'ko, Aleksei V.; Latipov, Egor V.; Goloveshkin, Alexander S.; Tsymbarenko, Dmitry M.; Utochnikova, Valentina V.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9685–9689; doi:10.1039/d1dt01316e

data_7707715
_publ_section_title
;
 Eu(tta)<sub>3</sub>DPPZ-based organic light-emitting diodes: spin-coating
 <i>vs</i>. vacuum-deposition.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9685
_journal_page_last               9689
_journal_paper_doi               10.1039/d1dt01316e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C42 H22 Eu F9 N4 O6 S3, C2 H3 N'
_chemical_formula_sum            'C44 H25 Eu F9 N5 O6 S3'
_chemical_formula_weight         1138.83
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.444(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7467(3)
_cell_length_b                   20.2118(6)
_cell_length_c                   21.5322(7)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.20
_cell_measurement_theta_min      2.18
_cell_volume                     4584.0(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0688
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55622
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.553
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11382
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+29.3102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1869
_reflns_number_gt                7623
_reflns_number_total             11382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt01316e2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7707715.cif.'
_cod_database_code               7707715
_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
 C19-F1
 1.55 with sigma of 0.01
 C42B-C40 = C42B-C39 = C42A-C39 = C42A-C41
 1.45 with sigma of 0.01
 S3B-C39 = S3B-C41 = S3A-C39 = S3A-C40
 1.7 with sigma of 0.01
 F7A-C35 = F8A-C35 = F9A-C35
 1.27 with sigma of 0.01
 F7B-C35 = F8B-C35 = F9B-C35
 1.27 with sigma of 0.01
3. Restrained planarity
 S3B, C42A, C39, C42B, C41, C40, S3A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim C28 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C35: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F8B \\sim F9A \\sim F9B \\sim F8A \\sim F7B \\sim F7A \\sim C35: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C2S) = Uanis(C3S) = Uanis(N1S)
Uanis(S3A) = Uanis(C42B) = Uanis(C39) = Uanis(S3B) = Uanis(C42A)
5. Others
 Sof(C42B)=Sof(H42B)=Sof(S3B)=Sof(H40)=Sof(H41)=1-FVAR(1)
 Sof(H40A)=Sof(H41A)=Sof(S3A)=Sof(C42A)=Sof(H42A)=FVAR(1)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(2)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C42B(H42B), C21(H21), C37(H37), C16(H16), C17(H17), C34(H34), C15(H15),
 C29(H29), C24(H24), C33(H33), C2(H2), C3(H3), C40(H40), C40(H40A), C8(H8),
 C11(H11), C10(H10), C9(H9), C26(H26), C41(H41), C41(H41A), C25(H25), C32(H32),
 C4(H4), C42A(H42A)
6.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC)
;
_olex2_submission_special_instructions 'No special instructions were received'