Designing water-quenching resistant highly luminescent europium complexes by regulating the orthogonal arrangement of bis-β-diketone ligands.
Li, Mei; Zhou, Yanyan; Yao, Yuan; Gao, Ting; Yan, Pengfei; Li, Hongfeng; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9914–9922; doi:10.1039/d1dt00155h

data_7707677
_publ_section_title
;
 Designing water-quenching resistant highly luminescent europium complexes
 by regulating the orthogonal arrangement of bis-\b-diketone ligands.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9914
_journal_page_last               9922
_journal_paper_doi               10.1039/d1dt00155h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C56 H20 Eu F12 N8 O8, 2(C4 H8 O), C6 H16 N, 0.5(C6 H12)'
_chemical_formula_sum            'C73 H58 Eu F12 N9 O10'
_chemical_formula_weight         1601.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-07 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.442(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0646(11)
_cell_length_b                   13.3266(7)
_cell_length_c                   26.5837(12)
_cell_measurement_reflns_used    9341
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.69
_cell_volume                     7361.5(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            184773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.760
_diffrn_reflns_theta_min         2.694
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.890
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0604P)^2^+31.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7585
_reflns_number_total             7807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00155h2.cif
_cod_data_source_block           mo_gt_1211_0m
_cod_depositor_comments          'Adding full bibliography for 7707677.cif.'
_cod_database_code               7707677
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5B-C38B = C38B-C39B = N5B-C40B = C40B-C41B = N5B-C36B = C37B-C36B
 1.5 with sigma of 0.001
 N5A-C41A = N5A-C39A = N5A-C37A
 2.7 with sigma of 0.05
 N5B-C39B = N5B-C41B = C37B-N5B
 2.75 with sigma of 0.01
 N5A-C38A = C39A-C38A = N5A-C36A = C37A-C36A = N5A-C40A = C40A-C41A
 1.5 with sigma of 0.001
 C38B-C36B
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N5B \\sim C41B \\sim C40B \\sim C38B \\sim C36B \\sim C39B \\sim C37B \\sim N5A
\\sim C37A \\sim C36A \\sim C40A \\sim C38A \\sim C39A \\sim C41A: within 2.4A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2.4A
4. Others
 Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(N5A)=Sof(H5A)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=
 Sof(C39A)=Sof(H39D)=Sof(H39F)=Sof(H39E)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=0.5*(1-FVAR(2))
 Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C40B)=Sof(H40B)=Sof(H40A)=
 Sof(N5B)=Sof(H5B)=Sof(C38B)=Sof(H38A)=Sof(H38B)=Sof(C36B)=Sof(H36A)=Sof(H36B)=
 Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C37B)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=0.5*FVAR(2)
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C30(0.5) H30A(0.5) H30B(0.5) C29(0.5)
 H29A(0.5) H29B(0.5)
5.a Riding coordinates:
 C37A(H37D,H37E,H37F), C39B(H39A,H39B,H39C)
5.b Ternary CH refined with riding coordinates:
 C11(H11), C18(H18), N5A(H5A), N5B(H5B)
5.c Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C33(H33A,H33B), C35(H35A,H35B), C32(H32A,H32B), C40A(H40C,
 H40D), C36A(H36C,H36D), C40B(H40B,H40A), C38B(H38A,H38B), C36B(H36A,H36B),
 C38A(H38C,H38D), C31(H31A,H31B), C30(H30A,H30B), C29(H29A,H29B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C23(H23), C26(H26), C21(H21), C8(H8), C22(H22), C7(H7)
5.e Idealised Me refined as rotating group:
 C41B(H41A,H41B,H41C), C37B(H37A,H37B,H37C), C39A(H39D,H39F,H39E), C41A(H41D,
 H41E,H41F)
;
_shelx_res_checksum              99514
_shelx_hkl_checksum              43592
_olex2_submission_special_instructions 'No special instructions were received'