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_7063082
_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 N5 O7 P Tb0.5), 3(C2 H3 N)'
_chemical_formula_sum            'C36 H33 Ag N13 O14 P2 Tb'
_chemical_formula_weight         1200.48
_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                   16.0444(4)
_cell_length_b                   28.8706(9)
_cell_length_c                   38.8302(10)
_cell_measurement_reflns_used    9095
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.92
_cell_measurement_theta_min      2.52
_cell_volume                     17986.6(9)
_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 2014/5 (Sheldrick, 2014)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            231949
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.585
_diffrn_reflns_theta_min         1.544
_exptl_absorpt_coefficient_mu    2.146
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0996 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.8771.
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    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             9504
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.422(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         30129
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+51.6233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                26043
_reflns_number_total             30129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00617h2.cif
_cod_data_source_block           tbag573
_cod_depositor_comments
'Adding full bibliography for 7063081--7063082.cif.'
_cod_database_code               7063082
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.578(8)
 0.422(8)
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
 N2S-C21S
 1.11 with sigma of 0.005
 C22S-C21S
 1.44 with sigma of 0.005
 C22S-N2S
 2.55 with sigma of 0.005
 Tb2-O61 \\sim Tb2-O61'
 with sigma of 0.02
 Tb2-O62 \\sim Tb2-O62'
 with sigma of 0.02
 N61-O61 \\sim N61-O61'
 with sigma of 0.02
 N61-O62 \\sim N61-O62'
 with sigma of 0.02
 Tb1-O32 \\sim Tb1-O32'
 with sigma of 0.02
 Tb1-O31 \\sim Tb1-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
 Tb2-O51 \\sim Tb2-O51'
 with sigma of 0.02
 Tb2-O52 \\sim Tb2-O52'
 with sigma of 0.02
 O51-N51 \\sim O51'-N51
 with sigma of 0.02
 N51-O52 \\sim N51-O52'
 with sigma of 0.02
 Tb1-O42 \\sim Tb1-O42'
 with sigma of 0.02
 Tb1-O41 \\sim Tb1-O41'
 with sigma of 0.02
 N41-O42 \\sim N41-O42'
 with sigma of 0.02
 N41-O41 \\sim N41-O41'
 with sigma of 0.02
4. Others
 Sof(O61')=Sof(O62')=1-FVAR(1)
 Sof(O61)=Sof(O62)=FVAR(1)
 Sof(O31')=Sof(O32')=1-FVAR(2)
 Sof(O32)=Sof(O31)=FVAR(2)
 Sof(O52')=Sof(O51')=1-FVAR(3)
 Sof(O51)=Sof(O52)=FVAR(3)
 Sof(O41')=Sof(O42')=1-FVAR(4)
 Sof(O42)=Sof(O41)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C3H(HR), C2B(H2B), C4C(H4C), C2F(H2F), C4F(H4F), C2O(HS), C3F(H3F), C4J(HT),
 C4H(HU), C2C(H2C), C5O(HV), C3C(H3C), C4O(HW), C3O(HX), C2K(HY), C5C(H5C),
 C3E(H3E), C3A(H3A), C2I(HZ), C5H(H1), C3J(H2), C2H(H3), C3G(H4), C2E(H2E),
 C2G(H5), C2A(H2A), C4B(H4B), C4D(H4D), C5F(H5F), C4I(H6), C5G(H7), C4G(H8),
 C5B(H5B), C5I(H9), C3D(H3D), C3K(H10), C4A(H4A), C2D(H2D), C4K(H11), C2J(H12),
 C5J(H13), C3I(H14), C5A(H5A), C4E(H4E), C5E(H5E), C3B(H3B), C5D(H5D), C5K(H15)
5.b Idealised Me refined as rotating group:
 C52S(H,HA,HB), C42S(HC,HD,HE), C32S(HF,HG,HH), C12S(HI,HJ,HK), C62S(HL,HM,HN),
  C22S(HO,HP,HQ)
;
_shelx_res_checksum              73464
_olex2_submission_special_instructions 'No special instructions were received'