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_2022780
_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          'Na3 [Sm (C7 H3 N O4)3], 14H2 O'
_chemical_formula_moiety         '3(Na +), C21 H9 N3 O12 Sm 3-, 14(H2 O)'
_chemical_formula_sum            'C21 H37 N3 Na3 O26 Sm'
_chemical_formula_weight         966.85
_chemical_name_systematic
;Trisodium tris(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)samarate(III)
tetradecahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_cell_angle_alpha                73.835(3)
_cell_angle_beta                 77.573(3)
_cell_angle_gamma                72.894(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2674(10)
_cell_length_b                   10.9688(10)
_cell_length_c                   17.1570(16)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      2.44
_cell_volume                     1754.9(3)
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107477
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.237
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.776
_exptl_crystal_size_mid          0.579
_exptl_crystal_size_min          0.264
_refine_diff_density_max         3.318
_refine_diff_density_min         -1.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         13465
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0210P)^2^+2.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                12700
_reflns_number_total             13465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5678sup1.cif
_cod_data_source_block           I
_cod_database_code               2022780
_shelx_estimated_absorpt_t_min   0.333
_shelx_estimated_absorpt_t_max   0.646
_shelx_hkl_checksum              64161
_shelx_res_checksum              7619
_cod_database_fobs_code 2022780