Highly photo- and triboluminescent lanthanide(iii) coordination polymers based on diphosphine dioxides containing azaheterocyclic linkers
Bryleva, Yuliya A.; Komarov, Vladislav Yu.; Glinskaya, Ludmila A.; Artem'ev, Alexander V.; Davydova, Maria P.; Rakhmanova, Mariana I.; Samsonenko, Denis G.; New Journal of Chemistry 47 (2023) 10446–10454; doi:10.1039/D3NJ01119D

data_7062458
_publ_section_title
;
 Highly photo- and triboluminescent lanthanide(iii) coordination polymers
 based on diphosphine dioxides containing azaheterocyclic linkers
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10446
_journal_page_last               10454
_journal_paper_doi               10.1039/D3NJ01119D
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C43 H25 Eu F18 N2 O8 P2'
_chemical_formula_sum            'C43 H25 Eu F18 N2 O8 P2'
_chemical_formula_weight         1253.55
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                103.866(3)
_cell_angle_beta                 97.437(3)
_cell_angle_gamma                96.554(3)
_cell_formula_units_Z            6
_cell_length_a                   13.1593(10)
_cell_length_b                   18.8395(15)
_cell_length_c                   30.990(2)
_cell_measurement_reflns_used    9019
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.24
_cell_volume                     7311.7(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            203402
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_description       plank
_exptl_crystal_F_000             3696
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.045(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4183
_refine_ls_number_reflns         80176
_refine_ls_number_restraints     822
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+1.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.893
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                65184
_reflns_number_total             80176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01119d3.cif
_cod_data_source_block           eu464_rem1_150k
_cod_depositor_comments
'Adding full bibliography for 7062455--7062458.cif.'
_cod_original_cell_volume        7311.8(10)
_cod_database_code               7062458
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.640
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.955(6)
 0.045(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{P2R3, P3}
{C6, C235}
4. Restrained distances
 C1_31-C2_31 = C4_31-C5_31
 1.54 with sigma of 0.02
 C1_35-F1_35 = C1_35-F2_35 = C1_35-F3_35
 1.315 with sigma of 0.005
 C2_31-C3_31 = C3_31-C4_31
 1.41 with sigma of 0.02
 O1_31-C2_31 = O2_31-C4_31
 1.25 with sigma of 0.02
 C135-F135 = C135-F235 = C135-F335
 1.315 with sigma of 0.005
 C1_31-F1_31 = C1_31-F2_31 = C1_31-F3_31 = C5_31-F4_31 = C5_31-F5_31 = C5_31-
 F6_31
 1.315 with sigma of 0.02
 C1_29-C2_29 = C4_29-C5_29
 1.54 with sigma of 0.02
 C2_29-C3_29 = C3_29-C4_29
 1.41 with sigma of 0.02
 O1_29-C2_29 = O2_29-C4_29
 1.25 with sigma of 0.02
 C1_29-F1_29 = C1_29-F2_29 = C1_29-F3_29 = C5_29-F4_29 = C5_29-F5_29 = C5_29-
 F6_29
 1.315 with sigma of 0.02
 C1A-C2A = C4A-C5A
 1.54 with sigma of 0.02
 C2A-C3A = C3A-C4A
 1.41 with sigma of 0.02
 O1A-C2A = O2A-C4A
 1.25 with sigma of 0.02
 C1A-F1A = C1A-F2A = C1A-F3A = C5A-F4A = C5A-F5A = C5A-F6A
 1.315 with sigma of 0.02
 C1B-C2B = C4B-C5B
 1.54 with sigma of 0.02
 C2B-C3B = C3B-C4B
 1.41 with sigma of 0.02
 O1B-C2B = O2B-C4B
 1.25 with sigma of 0.02
 C1B-F1B = C1B-F2B = C1B-F3B = C5B-F4B = C5B-F5B = C5B-F6B
 1.315 with sigma of 0.02
 F1_35-F2_35 = F1_35-F3_35 = F2_35-F3_35
 2.105 with sigma of 0.01
 C6_35-F1_35 = C6_35-F2_35 = C6_35-F3_35
 2.36 with sigma of 0.01
 O1_31-C3_31 = O2_31-C3_31
 2.4 with sigma of 0.05
 F135-F235 = F135-F335 = F235-F335
 2.105 with sigma of 0.01
 O1_31-C1_31 = O2_31-C5_31
 2.34 with sigma of 0.05
 C235-F135 = C235-F235 = C235-F335
 2.36 with sigma of 0.01
 F1_31-F2_31 = F1_31-F3_31 = F2_31-F3_31 = F4_31-F5_31 = F4_31-F6_31 = F5_31-
 F6_31
 2.105 with sigma of 0.05
 C2_31-F1_31 = C2_31-F2_31 = C2_31-F3_31 = C4_31-F4_31 = C4_31-F5_31 = C4_31-
 F6_31
 2.36 with sigma of 0.05
 O1_29-C3_29 = O2_29-C3_29
 2.4 with sigma of 0.05
 O1_29-C1_29 = O2_29-C5_29
 2.34 with sigma of 0.05
 F1_29-F2_29 = F1_29-F3_29 = F2_29-F3_29 = F4_29-F5_29 = F4_29-F6_29 = F5_29-
 F6_29
 2.105 with sigma of 0.05
 C2_29-F1_29 = C2_29-F2_29 = C2_29-F3_29 = C4_29-F4_29 = C4_29-F5_29 = C4_29-
 F6_29
 2.36 with sigma of 0.05
 O1A-C3A = O2A-C3A
 2.4 with sigma of 0.05
 O1A-C1A = O2A-C5A
 2.34 with sigma of 0.05
 F1A-F2A = F1A-F3A = F2A-F3A = F4A-F5A = F4A-F6A = F5A-F6A
 2.105 with sigma of 0.05
 C2A-F1A = C2A-F2A = C2A-F3A = C4A-F4A = C4A-F5A = C4A-F6A
 2.36 with sigma of 0.05
 O1B-C3B = O2B-C3B
 2.4 with sigma of 0.05
 O1B-C1B = O2B-C5B
 2.34 with sigma of 0.05
 F1B-F2B = F1B-F3B = F2B-F3B = F4B-F5B = F4B-F6B = F5B-F6B
 2.105 with sigma of 0.05
 C2B-F1B = C2B-F2B = C2B-F3B = C4B-F4B = C4B-F5B = C4B-F6B
 2.36 with sigma of 0.05
5. Restrained planarity
 C1E3, C2E3, C3E3, C4E3, C5E3, C6E3
 with sigma of 0.1
 C1D_3, C2D_3, C3D_3, C4D_3, C5D_3, C6D_3
 with sigma of 0.1
 C1E_3, C2E_3, C3E_3, C4E_3, C5E_3, C6E_3
 with sigma of 0.1
 C1D3, C2D3, C3D3, C4D3, C5D3, C6D3
 with sigma of 0.1
 O1_30, O2_30, C2_30, C1_30, C3_30, C4_30, C5_30
 with sigma of 0.1
 C1_29, C2_29, O1_29, C3_29, C4_29, O2_29, C5_29
 with sigma of 0.1
 O1A, O2A, C2A, C4A, C1A, C3A, C5A
 with sigma of 0.1
 O1B, O2B, C2B, C3B, C4B, C5B, C1B
 with sigma of 0.1
6. Uiso/Uaniso restraints and constraints
F1_31 \\sim F3_31 \\sim F4_31 \\sim F5_31 \\sim F6_31 \\sim O1_31 \\sim O2_31
\\sim C1_31 \\sim C2_31 \\sim C3_31 \\sim C4_31 \\sim C5_31 \\sim F2_31: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1D3 \\sim C2D3 \\sim C3D3 \\sim C4D3 \\sim C5D3 \\sim C6D3: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F1_29 \\sim F2_29 \\sim F3_29 \\sim F4_29 \\sim F5_29 \\sim F6_29 \\sim O1_29
\\sim O2_29 \\sim C1_29 \\sim C2_29 \\sim C3_29 \\sim C4_29 \\sim C5_29: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F1B \\sim F2B \\sim F3B \\sim F4B \\sim F5B \\sim F6B \\sim O1B \\sim O2B \\sim
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim O1A \\sim O2A \\sim
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C1E3) \\sim Ueq, Uanis(C1E_3) \\sim Ueq, Uanis(C6E3) \\sim Ueq,
Uanis(C6E_3) \\sim Ueq, Uanis(C5E3) \\sim Ueq, Uanis(C5E_3) \\sim Ueq,
Uanis(C4E3) \\sim Ueq, Uanis(C4E_3) \\sim Ueq, Uanis(C3E3) \\sim Ueq,
Uanis(C3E_3) \\sim Ueq, Uanis(C2E3) \\sim Ueq, Uanis(C2E_3) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C135) \\sim Ueq, Uanis(C1_35) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C235) \\sim Ueq, Uanis(C6_35) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O2A) \\sim Ueq, Uanis(O1_31) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C1E3) \\sim Ueq, Uanis(C1E_3) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.02
Uanis(O2_29) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C6D3) \\sim Ueq, Uanis(C6D_3) \\sim Ueq, Uanis(C5D3) \\sim Ueq,
Uanis(C5D_3) \\sim Ueq, Uanis(C4D3) \\sim Ueq, Uanis(C4D_3) \\sim Ueq,
Uanis(C3D3) \\sim Ueq, Uanis(C3D_3) \\sim Ueq, Uanis(C2D3) \\sim Ueq,
Uanis(C2D_3) \\sim Ueq, Uanis(C1D3) \\sim Ueq, Uanis(C1D_3) \\sim Ueq,
Uanis(C1D_3) \\sim Ueq, Uanis(C2D_3) \\sim Ueq, Uanis(C3D_3) \\sim Ueq,
Uanis(C4D_3) \\sim Ueq, Uanis(C5D3) \\sim Ueq, Uanis(C6D3) \\sim Ueq,
Uanis(C1D3) \\sim Ueq, Uanis(C6D_3) \\sim Ueq, Uanis(C5D_3) \\sim Ueq,
Uanis(C4D3) \\sim Ueq, Uanis(C3D3) \\sim Ueq, Uanis(C2D3) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6_35) = Uanis(C235)
Uanis(P2R3) = Uanis(P3_3)
Uanis(O2B) = Uanis(O2_31)
Uanis(O2A) = Uanis(O1_31)
Uanis(C1E3) = Uanis(C1E_3)
Uiso(F6A) = Uiso(F3_31)
Uiso(F6B) = Uiso(F6_31)
Uanis(O1B) = Uanis(O2_29)
Uanis(O1A) = Uanis(O1_29)
7. Rigid body (RIGU) restrains
 C1E3, C2E3, C3E3, C4E3, C5E3, C6E3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F335, F135, C135, F235
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1_35, C1_35, F2_35, F3_35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1_31, C2_31, C3_31, C4_31, O2_31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.005
 C1D_3, C2D_3, C3D_3, C4D_3, C5D_3, C6D_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1E_3, C2E_3, C3E_3, C4E_3, C5E_3, C6E_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1D3, C2D3, C3D3, C4D3, C5D3, C6D3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2_29, C4_29, C3_29, C2_29, O1_29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C2A, C3A, C4A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, C4B, C3B, C2B, O1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(P2R3)=Sof(C1D3)=Sof(C2D3)=Sof(H2D3)=Sof(C3D3)=Sof(H3D3)=Sof(C4D3)=
 Sof(H4D3)=Sof(C5D3)=Sof(H5D3)=Sof(C6D3)=Sof(H6D3)=1-FVAR(1)
 Sof(P3)=Sof(C1D)=Sof(C2D)=Sof(H2D)=Sof(C3D)=Sof(H3D)=Sof(C4D)=Sof(H4D)=
 Sof(C5D)=Sof(H5D)=Sof(C6D)=Sof(H6D)=FVAR(1)
 Sof(C1E3)=Sof(C2E3)=Sof(H2E3)=Sof(C3E3)=Sof(H3E3)=Sof(C4E3)=Sof(H4E3)=
 Sof(C5E3)=Sof(H5E3)=Sof(C6E3)=Sof(H6E3)=1-FVAR(2)
 Sof(C1E)=Sof(C2E)=Sof(H2E)=Sof(C3E)=Sof(H3E)=Sof(C4E)=Sof(H4E)=Sof(C5E)=
 Sof(H5E)=Sof(C6E)=Sof(H6E)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O1A)=Sof(O2A)=
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(F1B)=Sof(F2B)=
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O1B)=Sof(O2B)=Sof(C1B)=Sof(C2B)=
 Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(C5B)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O1)=Sof(O2)=Sof(C1)=
 Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=
 Sof(F5)=Sof(F6)=Sof(O1)=Sof(O2)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(C5)=FVAR(3)
 Sof(F135)=Sof(F235)=Sof(F335)=Sof(C135)=Sof(C235)=1-FVAR(4)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C1)=Sof(C6)=FVAR(4)
9.a Riding coordinates:
 C3(H3)
9.b Aromatic/amide H refined with riding coordinates:
 C2D3(H2D3), C3D3(H3D3), C4D3(H4D3), C5D3(H5D3), C6D3(H6D3), C2E3(H2E3),
 C3E3(H3E3), C4E3(H4E3), C5E3(H5E3), C6E3(H6E3), C3A(H3A), C3B(H3B), C2A(H2A),
 C2B(H2B), C2C(H2C), C2D(H2D), C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E),
  C4A(H4A), C4B(H4B), C4C(H4C), C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B),
 C5D(H5D), C5E(H5E), C6A(H6A), C6B(H6B), C6D(H6D), C6E(H6E), C2A(H2A), C2B(H2B),
  C2C(H2C), C2D(H2D), C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E),
 C4A(H4A), C4B(H4B), C4C(H4C), C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B), C5D(H5D),
  C5E(H5E), C6A(H6A), C6B(H6B), C6D(H6D), C6E(H6E), C2A(H2A), C2B(H2B),
 C2C(H2C), C2D(H2D), C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E), C4A(H4A),
  C4B(H4B), C4C(H4C), C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B), C5D(H5D),
 C5E(H5E), C6A(H6A), C6B(H6B), C6D(H6D), C6E(H6E), C2A(H2A), C2B(H2B), C2C(H2C),
  C2D(H2D), C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E), C4A(H4A),
 C4B(H4B), C4C(H4C), C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B), C5D(H5D), C5E(H5E),
  C6A(H6A), C6B(H6B), C6D(H6D), C6E(H6E), C2B(H2B), C2C(H2C), C2D(H2D),
 C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E), C4A(H4A), C4B(H4B), C4C(H4C),
  C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B), C5D(H5D), C5E(H5E), C6A(H6A),
 C6B(H6B), C6D(H6D), C6E(H6E), C8(H8), C2A(H2A), C2B(H2B), C2C(H2C), C2D(H2D),
 C2E(H2E), C3A(H3A), C3B(H3B), C3D(H3D), C3E(H3E), C4A(H4A), C4B(H4B), C4C(H4C),
  C4D(H4D), C4E(H4E), C5A(H5A), C5B(H5B), C5D(H5D), C5E(H5E), C6A(H6A),
 C6B(H6B), C6D(H6D), C6E(H6E), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3),
 C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3), C3(H3),
  C3(H3)
;
_shelx_res_checksum              72486
_olex2_submission_special_instructions 'No special instructions were received'