Synthetic Control to Achieve Lanthanide(III)/Pyrimidine-4,6-dicarboxylate Compounds by Preventing Oxalate Formation: Structural, Magnetic, and Luminescent Properties
Javier Cepeda; Rolindes Balda; Garikoitz Beobide; Oscar Castillo; Joaquín Fernández; Antonio Luque; Sonia Pérez-Yáñez; Pascual Román; Inorganic Chemistry 51 (2012) 7875–7888; doi:10.1021/ic3009392

data_4329751
_publ_contact_author
;
Oscar Castillo. Departamento de Quimica Inorganica. 
Facultad de Ciencia y Tecnologia
Universidad del Pais Vasco,  Apdo. 644, 
E-48080 Bilbao, Spain
;
_publ_contact_author_email       oscar.castillo@ehu.es
_publ_contact_author_fax         '+34-946 013 500'
_publ_contact_author_phone       '+34-946 015 991'
_publ_section_title
;
 Synthetic Control to Achieve Lanthanide(III)/Pyrimidine-4,6-dicarboxylate
 Compounds by Preventing Oxalate Formation: Structural, Magnetic, and
 Luminescent Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7875
_journal_page_last               7888
_journal_paper_doi               10.1021/ic3009392
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H30 N6 O18 Tb2, 11(H2 O)'
_chemical_formula_structural     'C18 H30 N6 O18 Tb2, 11(H2 O)'
_chemical_formula_sum            'C18 H52 N6 O29 Tb2'
_chemical_formula_weight         1134.50
_chemical_name_systematic
;
poly-{[tris(mu-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O')-
hexaacuaditerbium(III)]undecahydrate}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.920(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.604(1)
_cell_length_b                   11.847(1)
_cell_length_c                   14.375(1)
_cell_measurement_reflns_used    9458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.45
_cell_measurement_theta_min      3.91
_cell_volume                     3849.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9458
_diffrn_reflns_theta_full        70.45
_diffrn_reflns_theta_max         70.45
_diffrn_reflns_theta_min         3.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.800
_exptl_absorpt_correction_T_max  0.090
_exptl_absorpt_correction_T_min  0.022
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      1.96(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.319
_refine_diff_density_min         -2.348
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9458
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1686P)^2^+42.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2570
_refine_ls_wR_factor_ref         0.2711
_reflns_number_gt                7324
_reflns_number_total             9458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3009392_si_002_4.cif
_cod_data_source_block           1-Tb
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329751
_cell_oxdiff_twin_number         2