Bright photo- and triboluminescence of centrosymmetric Eu(iii) and Tb(iii) complexes with phosphine oxides containing azaheterocycles
Bryleva, Yuliya A.; Artem’ev, Alexander V.; Glinskaya, Ludmila A.; Rakhmanova, Mariana I.; Samsonenko, Denis G.; Komarov, Vladislav Yu.; Rogovoy, Maxim I.; Davydova, Maria P.; New Journal of Chemistry 45 (2021) 13869–13876; doi:10.1039/D1NJ02441H

data_7060774
_publ_section_title
;
 Bright photo- and triboluminescence of centrosymmetric Eu(iii) and
 Tb(iii) complexes with phosphine oxides containing azaheterocycles
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13869
_journal_page_last               13876
_journal_paper_doi               10.1039/D1NJ02441H
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C49 H31 Eu F18 N2 O8 P2'
_chemical_formula_sum            'C49 H31 Eu F18 N2 O8 P2'
_chemical_formula_weight         1331.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2021-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                81.090(2)
_cell_angle_beta                 88.144(2)
_cell_angle_gamma                88.268(2)
_cell_formula_units_Z            4
_cell_length_a                   12.7089(5)
_cell_length_b                   17.7622(7)
_cell_length_c                   23.0802(10)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      2.70
_cell_volume                     5142.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            94520
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.577
_diffrn_reflns_theta_min         1.604
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0569 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.8604.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         32502
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0279P)^2^+4.9972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24970
_reflns_number_total             32502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02441h3.cif
_cod_data_source_block           eu280_s2_100k
_cod_depositor_comments
'Adding full bibliography for 7060773--7060775.cif.'
_cod_database_code               7060774
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.796
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F21-C21 \\sim F22-C21 \\sim F23-C21 \\sim F1B-C4B \\sim F2B-C4B \\sim F3B-C4B
\\sim F1C-C4C \\sim F2C-C4C
 \\sim F3C-C4C \\sim F1D-C4D \\sim F2D-C4D \\sim F3D-C4D
 with sigma of 0.02
 F21-F22 \\sim F22-F23 \\sim F23-F21 \\sim F1B-F2B \\sim F2B-F3B \\sim F3B-F1B
\\sim F1C-F2C \\sim F2C-F3C
 \\sim F3C-F1C \\sim F1D-F2D \\sim F2D-F3D \\sim F3D-F1D
 with sigma of 0.02
 C4C-C22 \\sim C4D-C22 \\sim C4B-C22 \\sim C22-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C4C) = Uiso(C4D) = Uiso(C4B) = Uiso(C21)
Uiso(F23) = Uiso(F1C) = Uiso(F3C) = Uiso(F3D) = Uiso(F3B) = Uiso(F21) =
Uiso(F1B) = Uiso(F1D) = Uiso(F22) = Uiso(F2B) = Uiso(F2C) = Uiso(F2D)
4. Others
 1*[Sof(F1D)+Sof(F2D)+Sof(F3D)+Sof(C4D)]+1*[Sof(F1C)+Sof(F2C)+Sof(F3C)+
 Sof(C4C)]+1*[Sof(F1B)+Sof(F2B)+Sof(F3B)+Sof(C4B)]+1*[Sof(F21)+Sof(F22)+
 Sof(F23)+Sof(C21)]=1 with esd of 0.001
 Sof(F21)=Sof(F22)=Sof(F23)=Sof(C21)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C4B)=FVAR(2)
 Sof(F1C)=Sof(F2C)=Sof(F3C)=Sof(C4C)=FVAR(3)
 Sof(F1D)=Sof(F2D)=Sof(F3D)=Sof(C4D)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23), C33(H33), C102(H102), C103(H103), C104(H104), C105(H105),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C113(H113),
 C114(H114), C115(H115), C116(H116), C117(H117), C202(H202), C203(H203),
 C204(H204), C205(H205), C207(H207), C208(H208), C209(H209), C210(H210),
 C211(H211), C213(H213), C214(H214), C215(H215), C216(H216), C217(H217),
 C43(H43), C53(H53), C63(H63), C302(H302), C303(H303), C304(H304), C305(H305),
 C307(H307), C308(H308), C309(H309), C310(H310), C311(H311), C313(H313),
 C314(H314), C315(H315), C316(H316), C317(H317), C402(H402), C403(H403),
 C404(H404), C405(H405), C407(H407), C408(H408), C409(H409), C410(H410),
 C411(H411), C413(H413), C414(H414), C415(H415), C416(H416), C417(H417)
;
_shelx_res_checksum              18573
_olex2_submission_special_instructions 'No special instructions were received'