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_7249595
_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 N4 Na O15 Tm, 8(H2 O)'
_chemical_formula_sum            'C28 H46 N4 Na O23 Tm'
_chemical_formula_weight         998.61
_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)thulium(III)] 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             2024-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-16 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                   18.7780(6)
_cell_length_b                   22.8484(6)
_cell_length_c                   18.0407(6)
_cell_measurement_reflns_used    14641
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.2800
_cell_measurement_theta_min      1.7730
_cell_volume                     7740.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      130.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -24.00   1.00   1.00    5.00    --  -23.50 -95.00-176.00   25
  2  \w    -66.00 -41.00   1.00    5.00    --  -23.50-178.00 -30.00   25
  3  \w    -42.00 -10.00   1.00    5.00    --   24.74 -57.00 -30.00   32
  4  \w     30.00  59.00   1.00    5.00    --   24.74 -57.00 -30.00   29
  5  \w     44.00 105.00   1.00    5.00    --   24.74  77.00 -90.00   61
  6  \w    -14.00  30.00   1.00    5.00    --   24.74  77.00 -90.00   44
  7  \w    -11.00  15.00   1.00    5.00    --  -23.50 -99.00 -60.00   26
  8  \w    -37.00 -11.00   1.00    5.00    --  -23.50  38.00  30.00   26
  9  \w     39.00 115.00   1.00    5.00    --   24.74 178.00  90.00   76
 10  \w      9.00  65.00   1.00    5.00    --   24.74 -77.00  60.00   56
 11  \w     38.00  64.00   1.00    5.00    --   24.74 -38.00  60.00   26
 12  \w    -52.00 -15.00   1.00    5.00    --   24.74 -38.00  60.00   37
 13  \w    -54.00 -25.00   1.00    5.00    --   24.74 -77.00  60.00   29
 14  \w     10.00  99.00   1.00    5.00    --   24.74  57.00-180.00   89
 15  \w     28.00  54.00   1.00    5.00    --   24.74  77.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0327233000
_diffrn_orient_matrix_UB_12      -0.0039094000
_diffrn_orient_matrix_UB_13      -0.0189989000
_diffrn_orient_matrix_UB_21      -0.0187090000
_diffrn_orient_matrix_UB_22      -0.0106446000
_diffrn_orient_matrix_UB_23      -0.0313915000
_diffrn_orient_matrix_UB_31      -0.0024402000
_diffrn_orient_matrix_UB_32      0.0288985000
_diffrn_orient_matrix_UB_33      -0.0141213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64038
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.783
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             4048
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0140P)^2^+11.2497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6072
_reflns_number_total             8284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00881b2.cif
_cod_data_source_block           5Tm
_cod_depositor_comments
'Adding full bibliography for 7249595--7249597.cif.'
_cod_database_code               7249595
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
2.a Everything fixed:
 H1WA, H1WB, H2WA, H2WB, H3WA, H3WB, H4WA, H4WB, H5WA, H5WB, H6WA, H6WB, H7WA,
 H7WB, H8WA, H8WB, H9WA, H9WB, H10A, H10B, H11A, H11B
2.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), C4A(H4A), C5A(H5A), N1B(H1B), C4B(H4B), C5B(H5B), N1C(H1C),
 C4C(H4C), C5C(H5C), N1D(H1D), C4D(H4D), C5D(H5D)
2.c Idealised Me refined as rotating group:
 C61A(H61A,H61B,H61C), C61B(H61D,H61E,H61F), C61C(H61G,H61H,H61I), C61D(H61J,
 H61K,H61L)
;
_shelx_res_checksum              67010
_shelx_hkl_checksum              49455
_olex2_submission_special_instructions 'No special instructions were received'