A family of luminescent heterometallic coordination polymers based on lanthanide(iii) ions and 6-methyl-2-oxonicotinate: near-infrared/visible emitters and colour fine-tuning
Razquin-Bobillo, Laura; García, Jose Angel; Hernández, Ricardo; Rodríguez-Diéguez, Antonio; Cepeda, Javier; CrystEngComm 26 (2024) 6707–6718; doi:10.1039/D4CE00881B

data_7249596
_publ_section_title
;
 A family of luminescent heterometallic coordination polymers based on
 lanthanide(iii) ions and 6-methyl-2-oxonicotinate: near-infrared/visible
 emitters and colour fine-tuning
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6707
_journal_page_last               6718
_journal_paper_doi               10.1039/D4CE00881B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C28 H30 Dy0.77 Eu0.12 N4 Na O15 Y0.11, 8(H2 O)'
_chemical_formula_sum            'C28 H46 Dy0.77 Eu0.12 N4 Na O23 Y0.11'
_chemical_formula_weight         982.82
_chemical_name_systematic
'Poly{[bis(2-oxo-6-methyl-1H-pyridine-3-carboxylato-kO,kO')(mu-2-oxo-6-methyl-1H-pyridine-3-carboxylato-kO,kO':kO'')(mu-2-oxo-6-methyl-1H-pyridine-3-carboxylato-kO,kO':kO',kO'')triaquasodium(I)dysprosium(III)/europium(III)/yttrium(III) (0.77/0.12/0.11] octahydrate}'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-14 deposited with the CCDC.	2024-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.937(5)
_cell_length_b                   18.160(4)
_cell_length_c                   18.791(4)
_cell_measurement_reflns_used    96067
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.388
_cell_measurement_theta_min      2.343
_cell_volume                     7827(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            96067
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.343
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.929
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1146 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.7530.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             3989
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.597
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0445
_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^)+84.3869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5842
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00881b2.cif
_cod_data_source_block           DyEuY6m2onic
_cod_depositor_comments
'Adding full bibliography for 7249595--7249597.cif.'
_cod_database_code               7249596
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1C,H1B} of C61C, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, {H61A,H61B,H61C} of C61D, {H61D,H61E,H61F} of C61B,
  {H61J,H61K,H61L} of C61C, {H61G,H61H,H61I} of C61A
2. Shared sites
{Eu1, Dy1, Y1}
3. Uiso/Uaniso restraints and constraints
Uanis(Eu1) = Uanis(Dy1) = Uanis(Y1)
4. Others
 Fixed Sof: Eu1(0.12) Dy1(0.77) Y1(0.11)
5.a Everything fixed:
 H1A, H1C, H1B
5.b Riding coordinates:
 O5W(H5WA,H5WB)
5.c Free rotating group:
 O10W(H10A,H10B), O7W(H7WA,H7WB), O4W(H4WA,H4WB), O9W(H9WA,H9WB,O8W,H8WA,H8WB),
  O6W(H6WA,H6WB,O11W,H11A,H11B)
5.d Rotating group:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.e Aromatic/amide H refined with riding coordinates:
 N1D(H1D), C4A(H4A), C4B(H4B), C5A(H5A), C4C(H4C), C5B(H5B), C5D(H5D),
 C5C(H5C), C4D(H4D)
5.f Idealised Me refined as rotating group:
 C61D(H61A,H61B,H61C), C61B(H61D,H61E,H61F), C61A(H61G,H61H,H61I), C61C(H61J,
 H61K,H61L)
;
_shelx_res_checksum              53961
_shelx_hkl_checksum              9153
_olex2_submission_special_instructions 'No special instructions were received'