The effect of terminal N-donor aromatic ligands on the sensitization and emission of lanthanide ions in Zn2Ln (Ln = Eu, Tb) complexes with 4-biphenylcarboxylate anions
Melnikov, Stanislav N.; Evstifeev, Igor S.; Nikolaveskii, Stanislav A.; Ananyev, Ivan V.; Varaksina, Evgenia A.; Taydakov, Ilya V.; Goloveshkin, Alexander S.; Sidorov, Aleksey A.; Kiskin, Mikhail A.; Eremenko, Igor L.; New Journal of Chemistry 45 (2021) 13349–13359; doi:10.1039/D0NJ05994C

data_7060755
_publ_section_title
;
 The effect of terminal N-donor aromatic ligands on the sensitization and
 emission of lanthanide ions in Zn2Ln (Ln = Eu, Tb) complexes with
 4-biphenylcarboxylate anions
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13349
_journal_page_last               13359
_journal_paper_doi               10.1039/D0NJ05994C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C88 H64 Eu N3 O15 Zn2, C2 H3 N'
_chemical_formula_sum            'C90 H67 Eu N4 O15 Zn2'
_chemical_formula_weight         1727.17
_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
_audit_creation_date             2020-09-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                67.158(5)
_cell_angle_beta                 75.572(5)
_cell_angle_gamma                88.289(5)
_cell_formula_units_Z            2
_cell_length_a                   16.666(5)
_cell_length_b                   16.983(5)
_cell_length_c                   17.358(5)
_cell_measurement_reflns_used    4556
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.40
_cell_volume                     4373(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)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.957
_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  0.1304
_diffrn_reflns_av_unetI/netI     0.2083
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35418
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         1.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.6070.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.952
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         15308
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.2358
_refine_ls_R_factor_gt           0.1237
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3014
_refine_ls_wR_factor_ref         0.3815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5971
_reflns_number_total             15308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05994c2.cif
_cod_data_source_block           post
_cod_depositor_comments
'Adding full bibliography for 7060753--7060757.cif.'
_cod_database_code               7060755
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.602
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7986
 0.2014
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
 N3B-O14B
 1.25 with sigma of 0.02
 N3B-O13B
 1.25 with sigma of 0.02
 N3B-O15B
 1.25 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C2 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C60B \\sim C65B \\sim C64B \\sim C63B \\sim C62B \\sim C61B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C50 \\sim C49 \\sim C48 \\sim C47 \\sim C52 \\sim C51: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
N1 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C8 \\sim C13 \\sim C12 \\sim C11 \\sim C10 \\sim C9: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
O14B \\sim N3B \\sim O15B \\sim O13B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C44) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C79) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C87) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C68) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) = Uanis(C8)
Uanis(C86) = Uanis(C87)
5. Others
 Sof(C60B)=Sof(C65B)=Sof(H65B)=Sof(C64B)=Sof(H64B)=Sof(C63B)=Sof(H63B)=
 Sof(C62B)=Sof(H62B)=Sof(C61B)=Sof(H61B)=1-FVAR(1)
 Sof(C62A)=Sof(H62A)=Sof(C61A)=Sof(H61A)=Sof(C60A)=Sof(C65A)=Sof(H65A)=
 Sof(C64A)=Sof(H64A)=Sof(C63A)=Sof(H63A)=FVAR(1)
 Sof(O13B)=Sof(O14B)=Sof(O15B)=Sof(N3B)=1-FVAR(2)
 Sof(O13A)=Sof(N3A)=Sof(O15A)=Sof(O14A)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88), C7(H7), C6(H6), C4(H4), C3(H3), C13(H13),
 C12(H12), C11(H11), C10(H10), C9(H9), C16(H16), C17(H17), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42),
 C43(H43), C45(H45), C46(H46), C50(H50), C49(H49), C48(H48), C52(H52), C51(H51),
  C55(H55), C56(H56), C58(H58), C59(H59), C65B(H65B), C64B(H64B), C63B(H63B),
 C62B(H62B), C61B(H61B), C73(H73), C74(H74), C76(H76), C77(H77), C81(H81),
 C82(H82), C83(H83), C79(H79), C80(H80), C62A(H62A), C61A(H61A), C65A(H65A),
 C64A(H64A), C63A(H63A)
6.b Fitted hexagon refined as free rotating group:
 N1(C66,C67,C68,C69,C70), N2(C84,C85,C86,C87,C88), C2(C7,C6,C5,C4,C3), C8(C13,
 C12,C11,C10,C9), C50(C49,C48,C47,C52,C51), C54(C55,C56,C57,C58,C59), C60B(C65B,
 C64B,C63B,C62B,C61B), C81(C82,C83,C78,C79,C80), C62A(C61A,C60A,C65A,C64A,C63A)
6.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51389
_shelx_fab_checksum              46661
_olex2_submission_special_instructions 'No special instructions were received'