Lanthanide(III)/Pyrimidine-4,6-dicarboxylate/Oxalate Extended Frameworks: A Detailed Study Based on the Lanthanide Contraction and Temperature Effects
Javier Cepeda; Rolindes Balda; Garikoitz Beobide; Oscar Castillo; Joaquín Fernández; Antonio Luque; Sonia Pérez-Yáñez; Pascual Román; Daniel Vallejo-Sánchez; Inorganic Chemistry 50 (2011) 8437–8451; doi:10.1021/ic201013v

data_4326095
_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
;
 Lanthanide(III)/Pyrimidine-4,6-dicarboxylate/Oxalate Extended Frameworks:
 A Detailed Study Based on the Lanthanide Contraction and Temperature
 Effects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8437
_journal_page_last               8451
_journal_paper_doi               10.1021/ic201013v
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H10 N4 Nd2 O15, 5(H2 O)'
_chemical_formula_structural     'C14 H10 N4 Nd2 O15, 5(H2 O)'
_chemical_formula_sum            'C14 H20 N4 Nd2 O20'
_chemical_formula_weight         852.8
_chemical_name_systematic
;
poly-{[(mu-oxalato)(mu3-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O':kO''
(mu4-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O':kO'':kO''')-
triacuadineodymium(III)]pentahydrate}
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9460(2)
_cell_length_b                   10.9890(2)
_cell_length_c                   19.4020(3)
_cell_measurement_reflns_used    24000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      3.28
_cell_volume                     2546.99(7)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24000
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.134
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      2.28(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.241
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6563
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                5926
_reflns_number_total             6563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201013v_si_002_15.cif
_cod_data_source_block           4-Nd
_cod_database_code               4326095