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_4329753
_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 H10 La2 N6 O14, H2 O'
_chemical_formula_structural     'C18 H10 La2 N6 O14, H2 O'
_chemical_formula_sum            'C18 H12 La2 N6 O15'
_chemical_formula_weight         830.1
_chemical_name_systematic
;
poly-{[(mu-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O'-bis-
(mu4-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O':kO'':kO''')-
diacuadilanthanum(III)]hydrate}
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 106.632(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3759(2)
_cell_length_b                   10.4558(2)
_cell_length_c                   12.5447(2)
_cell_measurement_reflns_used    7532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      1.95
_cell_volume                     1178.34(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'DIAMOND 3 (K. & Putz, 2005))'
_computing_publication_material  'Jana 2006 (Petricek et al., 2006)'
_computing_structure_refinement  'Jana 2006 (Petricek et al., 2006)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.053
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7532
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.669
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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    2.339
_exptl_crystal_density_meas      2.34(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details
'  2214 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   -0.008(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     176
_refine_ls_number_reflns         4623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.96
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.0097
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                3925
_reflns_number_total             4623
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ic3009392_si_002_6.cif
_cod_data_source_block           2-La
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4329753