Crystal structures of two SmIII complexes with dipicolinate [DPA]2− ligands: comparison of luminescent properties of products obtained at different pH values
Mortensen, Sabina Svava; Sørensen, Thomas Just; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S2056989023004814

data_2022781
_publ_section_title
;
 Crystal structures of two SmIII complexes with dipicolinate
 [DPA]2&#x2212; ligands: comparison of luminescent properties of products
 obtained at different pH values
;
_journal_issue                   7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989023004814
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Sm (C7 H3 N O4) (C7 H4 N O4) (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C14 H11 N2 O10 Sm, 4H2 O'
_chemical_formula_sum            'C14 H19 N2 O14 Sm'
_chemical_formula_weight         589.66
_chemical_name_systematic
'<i>catena</i>-Poly[[[diaqua(6-carboxypyridine-2-carboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)samarium(III)]-\m-pyridine-2,6-dicarboxylato-\k^4^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^:<i>O</i>^2^] tetrahydrate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 103.049(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9292(8)
_cell_length_b                   11.1969(7)
_cell_length_c                   12.8086(7)
_cell_measurement_reflns_used    9554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.07
_cell_measurement_theta_min      2.44
_cell_volume                     1946.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX2 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74345
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.444
_exptl_absorpt_coefficient_mu    3.097
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.726
_refine_diff_density_min         -1.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7424
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+2.2391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                6679
_reflns_number_total             7424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5678sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022781
_shelx_estimated_absorpt_t_min   0.318
_shelx_estimated_absorpt_t_max   0.650
_shelx_hkl_checksum              74091
_shelx_res_checksum              61540
_cod_database_fobs_code 2022781