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_7062457
_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_formula_moiety         'C43 H25 F18 N2 O8 P2 Tb'
_chemical_formula_sum            'C43 H25 F18 N2 O8 P2 Tb'
_chemical_formula_weight         1260.51
_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     dual
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.503(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8954(6)
_cell_length_b                   19.2681(7)
_cell_length_c                   18.7132(8)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.70
_cell_measurement_theta_min      2.28
_cell_volume                     4778.3(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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  0.0988
_diffrn_reflns_av_unetI/netI     0.0464
_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       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            119113
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.8960.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         11403
_refine_ls_number_restraints     2282
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0606P)^2^+9.0690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8496
_reflns_number_total             11403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01119d3.cif
_cod_data_source_block           tb414_s1_mp_150k
_cod_depositor_comments
'Adding full bibliography for 7062455--7062458.cif.'
_cod_database_code               7062457
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1_1-F1_1 \\sim C1_1-F2_1 \\sim C1_1-F3_1 \\sim C5_1-F4_1 \\sim C5_1-F5_1
\\sim C5_1-F6_1
 C1_2-F1_2 \\sim C1_2-F2_2 \\sim C1_2-F3_2 \\sim C5_2-F4_2 \\sim C5_2-F5_2
\\sim C5_2-F6_2
 C1_3-F1_3 \\sim C1_3-F2_3 \\sim C1_3-F3_3 \\sim C5_3-F4_3 \\sim C5_3-F5_3
\\sim C5_3-F6_3
 C1_4-F1_4 \\sim C1_4-F2_4 \\sim C1_4-F3_4 \\sim C5_4-F4_4 \\sim C5_4-F5_4
\\sim C5_4-F6_4
 C1_5-F1_5 \\sim C1_5-F2_5 \\sim C1_5-F3_5 \\sim C5_5-F4_5 \\sim C5_5-F5_5
\\sim C5_5-F6_5
 with sigma of 0.01
 C2_1-F1_1 \\sim C2_1-F2_1 \\sim C2_1-F3_1 \\sim C4_1-F4_1 \\sim C4_1-F5_1
\\sim C4_1-F6_1
 C2_2-F1_2 \\sim C2_2-F2_2 \\sim C2_2-F3_2 \\sim C4_2-F4_2 \\sim C4_2-F5_2
\\sim C4_2-F6_2
 C2_3-F1_3 \\sim C2_3-F2_3 \\sim C2_3-F3_3 \\sim C4_3-F4_3 \\sim C4_3-F5_3
\\sim C4_3-F6_3
 C2_4-F1_4 \\sim C2_4-F2_4 \\sim C2_4-F3_4 \\sim C4_4-F4_4 \\sim C4_4-F5_4
\\sim C4_4-F6_4
 C2_5-F1_5 \\sim C2_5-F2_5 \\sim C2_5-F3_5 \\sim C4_5-F4_5 \\sim C4_5-F5_5
\\sim C4_5-F6_5
 with sigma of 0.03
 F1_1-F2_1 \\sim F2_1-F3_1 \\sim F3_1-F1_1 \\sim F4_1-F5_1 \\sim F5_1-F6_1
\\sim F6_1-F4_1
 F1_2-F2_2 \\sim F2_2-F3_2 \\sim F3_2-F1_2 \\sim F4_2-F5_2 \\sim F5_2-F6_2
\\sim F6_2-F4_2
 F1_3-F2_3 \\sim F2_3-F3_3 \\sim F3_3-F1_3 \\sim F4_3-F5_3 \\sim F5_3-F6_3
\\sim F6_3-F4_3
 F1_4-F2_4 \\sim F2_4-F3_4 \\sim F3_4-F1_4 \\sim F4_4-F5_4 \\sim F5_4-F6_4
\\sim F6_4-F4_4
 F1_5-F2_5 \\sim F2_5-F3_5 \\sim F3_5-F1_5 \\sim F4_5-F5_5 \\sim F5_5-F6_5
\\sim F6_5-F4_5
 with sigma of 0.03
 C2_1-C3_1 \\sim C4_1-C3_1
 C2_2-C3_2 \\sim C4_2-C3_2
 C2_3-C3_3 \\sim C4_3-C3_3
 C2_4-C3_4 \\sim C4_4-C3_4
 C2_5-C3_5 \\sim C4_5-C3_5
 with sigma of 0.01
 C2_1-O1_1 \\sim C4_1-O2_1
 C2_2-O1_2 \\sim C4_2-O2_2
 C2_3-O1_3 \\sim C4_3-O2_3
 C2_4-O1_4 \\sim C4_4-O2_4
 C2_5-O1_5 \\sim C4_5-O2_5
 with sigma of 0.01
 C1_1-O1_1 \\sim C5_1-O2_1
 C1_2-O1_2 \\sim C5_2-O2_2
 C1_3-O1_3 \\sim C5_3-O2_3
 C1_4-O1_4 \\sim C5_4-O2_4
 C1_5-O1_5 \\sim C5_5-O2_5
 with sigma of 0.03
 C3_1-O1_1 \\sim C3_1-O2_1
 C3_2-O1_2 \\sim C3_2-O2_2
 C3_3-O1_3 \\sim C3_3-O2_3
 C3_4-O1_4 \\sim C3_4-O2_4
 C3_5-O1_5 \\sim C3_5-O2_5
 with sigma of 0.03
3. Restrained planarity
 C5_1, C4_1, O2_1, C3_1, C2_1, O1_1, C1_1
 C5_2, C4_2, O2_2, C3_2, C2_2, O1_2, C1_2
 C5_3, C4_3, O2_3, C3_3, C2_3, O1_3, C1_3
 C5_4, C4_4, O2_4, C3_4, C2_4, O1_4, C1_4
 C5_5, C4_5, O2_5, C3_5, C2_5, O1_5, C1_5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(F2_2) \\sim Ueq, Uanis(C1_2) \\sim Ueq, Uanis(F1_2) \\sim Ueq,
Uanis(F3_2) \\sim Ueq, Uanis(C2_2) \\sim Ueq, Uanis(C3_2) \\sim Ueq,
Uanis(F5_2) \\sim Ueq, Uanis(F2_3) \\sim Ueq, Uanis(C1_3) \\sim Ueq,
Uanis(F1_3) \\sim Ueq, Uanis(F3_3) \\sim Ueq, Uanis(C3_3) \\sim Ueq,
Uanis(C4_3) \\sim Ueq, Uanis(C5_3) \\sim Ueq, Uanis(F5_3) \\sim Ueq,
Uanis(F6_3) \\sim Ueq, Uanis(F4_3) \\sim Ueq, Uanis(O1_2) \\sim Ueq,
Uanis(C4_2) \\sim Ueq, Uanis(O2_2) \\sim Ueq, Uanis(C5_2) \\sim Ueq,
Uanis(F6_2) \\sim Ueq, Uanis(F4_2) \\sim Ueq, Uanis(O1_3) \\sim Ueq,
Uanis(C2_3) \\sim Ueq, Uanis(O2_3) \\sim Ueq, Uanis(O1_4) \\sim Ueq,
Uanis(F2_4) \\sim Ueq, Uanis(C1_4) \\sim Ueq, Uanis(F1_4) \\sim Ueq,
Uanis(F3_4) \\sim Ueq, Uanis(C2_4) \\sim Ueq, Uanis(C3_4) \\sim Ueq,
Uanis(C4_4) \\sim Ueq, Uanis(O2_4) \\sim Ueq, Uanis(C5_4) \\sim Ueq,
Uanis(F5_4) \\sim Ueq, Uanis(F6_4) \\sim Ueq, Uanis(F4_4) \\sim Ueq,
Uanis(O1_5) \\sim Ueq, Uanis(F2_5) \\sim Ueq, Uanis(C1_5) \\sim Ueq,
Uanis(F1_5) \\sim Ueq, Uanis(F3_5) \\sim Ueq, Uanis(C2_5) \\sim Ueq,
Uanis(C3_5) \\sim Ueq, Uanis(C4_5) \\sim Ueq, Uanis(O2_5) \\sim Ueq,
Uanis(C5_5) \\sim Ueq, Uanis(F5_5) \\sim Ueq, Uanis(F6_5) \\sim Ueq,
Uanis(F4_5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C4_1, C5_1, F5_1, F4_1, F6_1
 C4_2, C5_2, F5_2, F4_2, F6_2
 C4_3, C5_3, F5_3, F4_3, F6_3
 C4_4, C5_4, F5_4, F4_4, F6_4
 C4_5, C5_5, F5_5, F4_5, F6_5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F2_1, C1_1, F3_1, F1_1, C2_1
 F2_2, C1_2, F3_2, F1_2, C2_2
 F2_3, C1_3, F3_3, F1_3, C2_3
 F2_4, C1_4, F3_4, F1_4, C2_4
 F2_5, C1_5, F3_5, F1_5, C2_5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1_1, O2_1, C1_1, C2_1, C3_1, C4_1, C5_1
 O1_2, O2_2, C1_2, C2_2, C3_2, C4_2, C5_2
 O1_3, O2_3, C1_3, C2_3, C3_3, C4_3, C5_3
 O1_4, O2_4, C1_4, C2_4, C3_4, C4_4, C5_4
 O1_5, O2_5, C1_5, C2_5, C3_5, C4_5, C5_5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(O1)=Sof(F2)=Sof(C1)=Sof(F1)=Sof(F3)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(O2)=Sof(C5)=Sof(F5)=Sof(F6)=Sof(F4)=1-FVAR(1)
 Sof(O1)=Sof(F2)=Sof(C1)=Sof(F1)=Sof(F3)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(O2)=Sof(C5)=Sof(F5)=Sof(F6)=Sof(F4)=FVAR(1)
 Sof(O1)=Sof(F2)=Sof(C1)=Sof(F1)=Sof(F3)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(O2)=Sof(C5)=Sof(F5)=Sof(F6)=Sof(F4)=1-FVAR(2)
 Sof(O1)=Sof(F2)=Sof(C1)=Sof(F1)=Sof(F3)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(O2)=Sof(C5)=Sof(F5)=Sof(F6)=Sof(F4)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C2C(H2C), C3C(H3C), C2D(H2D), C3D(H3D), C4D(H4D),
  C5D(H5D), C6D(H6D), C2E(H2E), C3E(H3E), C4E(H4E), C5E(H5E), C6E(H6E), C3(H3),
 C3(H3), C3(H3), C3(H3), C3(H3)
;
_shelx_res_checksum              77468
_olex2_submission_special_instructions 'No special instructions were received'