Dual emissive Ln(iii)–Ag(i) heterometallic chains based on tris(2-pyridyl)phosphine oxide
Bryleva, Yuliya A.; Rakhmanova, Mariana I.; Artem'ev, Alexander V.; Baranov, Andrey Yu.; Glinskaya, Ludmila A.; New Journal of Chemistry 48 (2024) 6430–6437; doi:10.1039/D4NJ00617H

data_7063081
_publ_section_title
;
 Dual emissive Ln(iii)--Ag(i) heterometallic chains based on
 tris(2-pyridyl)phosphine oxide
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6430
_journal_page_last               6437
_journal_paper_doi               10.1039/D4NJ00617H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         '2(C15 H12 Ag0.5 Eu0.5 N5 O7 P), 3(C2 H3 N)'
_chemical_formula_sum            'C36 H33 Ag Eu N13 O14 P2'
_chemical_formula_weight         1193.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-29 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.0607(4)
_cell_length_b                   28.9999(9)
_cell_length_c                   38.8996(9)
_cell_measurement_reflns_used    9689
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.51
_cell_volume                     18117.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_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 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            172059
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.891
_diffrn_reflns_theta_min         1.404
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.954
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0934 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.9020.
The \l/2 correction factor is Not present.
;
_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    1.750
_exptl_crystal_description       plank
_exptl_crystal_F_000             9472
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.412
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.207(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1277
_refine_ls_number_reflns         21623
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+72.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                19512
_reflns_number_total             21623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00617h2.cif
_cod_data_source_block           euag575
_cod_depositor_comments
'Adding full bibliography for 7063081--7063082.cif.'
_cod_database_code               7063081
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.793(12)
 0.207(12)
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
 N11-O13
 1.24 with sigma of 0.02
 N4S-C41S
 1.14 with sigma of 0.01
 C42S-C41S
 1.42 with sigma of 0.01
 N11-O12
 1.2459 with sigma of 0.02
 N11-O11
 1.2459 with sigma of 0.02
 O11-O12
 2.1579 with sigma of 0.02
 O13-O11 = O13-O12
 2.16 with sigma of 0.04
 C42S-N4S
 2.56 with sigma of 0.01
 Eu1-O32 \\sim Eu1-O32'
 with sigma of 0.02
 Eu1-O31 \\sim Eu1-O31'
 with sigma of 0.02
 N31-O32 \\sim N31-O32'
 with sigma of 0.02
 N31-O31 \\sim N31-O31'
 with sigma of 0.02
 Eu2-O62' \\sim Eu2-O62
 with sigma of 0.02
 Eu2-O61' \\sim Eu2-O61
 with sigma of 0.02
 N61-O62' \\sim N61-O62
 with sigma of 0.02
 N61-O61' \\sim N61-O61
 with sigma of 0.02
 Eu2-O71 \\sim Eu2-O71'
 with sigma of 0.02
 Eu2-O72 \\sim Eu2-O72'
 with sigma of 0.02
 O71-N71 \\sim O71'-N71
 with sigma of 0.02
 O72-N71 \\sim O72'-N71
 with sigma of 0.02
4. Restrained planarity
 O81, N81', O83', O82
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O13') \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C41S) = Uanis(C42S)
Uanis(O31') = Uanis(O32')
Uanis(O83) = Uanis(O83')
Uanis(N81) = Uanis(N81')
6. Rigid body (RIGU) restrains
 O71, N71, O73, O72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O71', N71, O73, O72'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O32')=Sof(O31')=1-FVAR(1)
 Sof(O32)=Sof(O31)=FVAR(1)
 Sof(O61)=Sof(O62)=1-FVAR(2)
 Sof(O62')=Sof(O61')=FVAR(2)
 Sof(O72')=Sof(O71')=1-FVAR(3)
 Sof(O71)=Sof(O72)=FVAR(3)
 Sof(O83')=Sof(N81')=1-FVAR(4)
 Sof(N81)=Sof(O83)=FVAR(4)
 Sof(O13)=1-FVAR(5)
 Sof(O13')=FVAR(5)
8.a Aromatic/amide H refined with riding coordinates:
 C4C(H4C), C2I(H2I), C3F(H3F), C4F(H4F), C2C(H2C), C3I(H3I), C3C(H3C),
 C5J(H5J), C4E(H4E), C2A(H2A), C2H(H2H), C2K(H2K), C3B(H3B), C4K(H4K), C4A(H4A),
  C5I(H5I), C2D(H2D), C4G(H4G), C5K(H5K), C2F(H2F), C2O(H2O), C2E(H2E),
 C4H(H4H), C3K(H3K), C3O(H3O), C5G(H5G), C3D(H3D), C5O(H5O), C4B(H4B), C4J(H4J),
  C2B(H2B), C4I(H4I), C5D(H5D), C5F(H5F), C4D(H4D), C5C(H5C), C5E(H5E),
 C3A(H3A), C2J(H2J), C3E(H3E), C2G(H2G), C3H(H3H), C4O(H4O), C5A(H5A), C5B(H5B),
  C5H(H5H), C3G(H3G), C3J(H3J)
8.b Idealised Me refined as rotating group:
 C22S(H22A,H22B,H22C), C12S(H12A,H12B,H12C), C32S(H32A,H32B,H32C), C52S(H52A,
 H52B,H52C), C42S(H42A,H42B,H42C), C62S(H62A,H62B,H62C)
;
_shelx_res_checksum              85498
_olex2_submission_special_instructions 'No special instructions were received'