#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:08:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179363 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/60/4326095.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4326095
loop_
_publ_author_name
'Javier Cepeda'
'Rolindes Balda'
'Garikoitz Beobide'
'Oscar Castillo'
'Joaquín Fernández'
'Antonio Luque'
'Sonia Pérez-Yáñez'
'Pascual Román'
'Daniel Vallejo-Sánchez'
_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       ω
_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/[σ²(Fo²)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nd1 Nd 0.65819(2) 0.863284(19) 0.985619(13) 0.00433(5) Uani 1 1 d .
Nd2 Nd 0.475999(18) 0.382028(19) 0.771455(13) 0.00459(5) Uani 1 1 d .
N11 N 0.6212(4) 0.7724(4) 0.8600(2) 0.0081(8) Uani 1 1 d .
C12 C 0.5617(4) 0.6721(4) 0.8466(2) 0.0065(9) Uani 1 1 d .
H12 H 0.5067 0.6507 0.8782 0.008 Uiso 1 1 calc R
N13 N 0.5743(3) 0.6001(3) 0.7918(2) 0.0081(8) Uani 1 1 d .
C14 C 0.6482(4) 0.6358(4) 0.7442(3) 0.0083(9) Uani 1 1 d .
C15 C 0.7104(4) 0.7423(4) 0.7519(2) 0.0067(9) Uani 1 1 d .
H15 H 0.7597 0.7682 0.7179 0.008 Uiso 1 1 calc R
C16 C 0.6960(4) 0.8070(4) 0.8113(2) 0.0067(9) Uani 1 1 d .
C17 C 0.7706(4) 0.9138(4) 0.8296(3) 0.0076(9) Uani 1 1 d .
O171 O 0.7613(3) 0.9553(3) 0.88994(18) 0.0091(7) Uani 1 1 d .
O172 O 0.8378(3) 0.9497(3) 0.78412(18) 0.0077(7) Uani 1 1 d .
C18 C 0.6674(4) 0.5527(4) 0.6833(3) 0.0112(10) Uani 1 1 d .
O181 O 0.6081(3) 0.4571(3) 0.68093(18) 0.0117(7) Uani 1 1 d .
O182 O 0.7383(4) 0.5852(4) 0.6419(2) 0.0294(11) Uani 1 1 d .
N21 N 0.5091(3) 0.9995(3) 0.9113(2) 0.0070(7) Uani 1 1 d .
C22 C 0.5283(4) 1.1018(4) 0.8760(3) 0.0088(9) Uani 1 1 d .
H22 H 0.6017 1.1299 0.8743 0.011 Uiso 1 1 calc R
N23 N 0.4508(3) 1.1671(4) 0.8429(2) 0.0073(8) Uani 1 1 d .
C24 C 0.3451(4) 1.1264(4) 0.8463(3) 0.0071(9) Uani 1 1 d .
C25 C 0.3173(4) 1.0214(4) 0.8820(3) 0.0096(9) Uani 1 1 d .
H25 H 0.2436 0.9946 0.8852 0.012 Uiso 1 1 calc R
C26 C 0.4039(4) 0.9587(4) 0.9124(3) 0.0073(9) Uani 1 1 d .
C27 C 0.3840(4) 0.8395(4) 0.9499(2) 0.0068(9) Uani 1 1 d .
O271 O 0.4655(2) 0.7916(3) 0.9814(2) 0.0080(6) Uani 1 1 d .
O272 O 0.2886(3) 0.7943(3) 0.94334(17) 0.0088(7) Uani 1 1 d .
C28 C 0.2554(4) 1.2040(4) 0.8121(2) 0.0076(9) Uani 1 1 d .
O281 O 0.2869(3) 1.2995(3) 0.78349(19) 0.0114(7) Uani 1 1 d .
O282 O 0.1573(3) 1.1659(3) 0.8162(2) 0.0109(7) Uani 1 1 d .
O31 O 0.5790(3) 0.8893(3) 1.10240(18) 0.0107(7) Uani 1 1 d .
C32 C 0.5649(4) 0.7992(4) 1.1401(3) 0.0085(9) Uani 1 1 d .
O33 O 0.5109(3) 0.7952(3) 1.1956(2) 0.0106(7) Uani 1 1 d .
O34 O 0.6515(3) 0.6741(3) 1.05542(19) 0.0111(7) Uani 1 1 d .
C35 C 0.6174(4) 0.6774(4) 1.1163(3) 0.0077(9) Uani 1 1 d .
O36 O 0.6204(3) 0.5918(3) 1.15991(18) 0.0091(7) Uani 1 1 d .
O1W O 0.6779(3) 1.0798(3) 1.01348(19) 0.0138(8) Uani 1 1 d .
O2W O 0.8385(3) 0.8845(3) 1.0470(2) 0.0127(8) Uani 1 1 d .
O3W O 0.4569(3) 0.4201(3) 0.89683(18) 0.0131(7) Uani 1 1 d .
O4W O 0.5057(4) 0.2536(4) 1.0031(3) 0.0359(12) Uani 1 1 d .
O5W O 0.3408(5) 1.1029(6) 1.0520(4) 0.0586(18) Uani 1 1 d .
O6W O 0.3945(6) 0.6481(5) 0.6134(3) 0.0569(19) Uani 1 1 d .
O7W O 0.9562(4) 0.6547(4) 0.6970(3) 0.0392(13) Uani 1 1 d .
O8W O 0.6370(3) 0.0093(3) 0.6878(3) 0.0238(10) Uani 1 1 d .
H11W H 0.6344 1.1425 1.0136 0.036 Uiso 1 1 d .
H12W H 0.6948 1.0674 1.0569 0.036 Uiso 1 1 d .
H21W H 0.8593 0.8851 1.0909 0.036 Uiso 1 1 d .
H22W H 0.8684 0.8142 1.0336 0.036 Uiso 1 1 d .
H31W H 0.3873 0.4452 0.8986 0.036 Uiso 1 1 d .
H32W H 0.4615 0.3695 0.9307 0.036 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O271 Nd1 O171 125.73(12) . .
O271 Nd1 O1W 114.37(11) . .
O171 Nd1 O1W 73.61(12) . .
O271 Nd1 O272 110.99(11) . 4_565
O171 Nd1 O272 73.76(11) . 4_565
O1W Nd1 O272 133.88(12) . 4_565
O271 Nd1 O31 72.93(13) . .
O171 Nd1 O31 147.19(11) . .
O1W Nd1 O31 73.88(12) . .
O272 Nd1 O31 128.83(11) 4_565 .
O271 Nd1 O2W 150.52(13) . .
O171 Nd1 O2W 83.59(13) . .
O1W Nd1 O2W 73.64(11) . .
O272 Nd1 O2W 71.14(11) 4_565 .
O31 Nd1 O2W 83.16(13) . .
O271 Nd1 O34 73.57(11) . .
O171 Nd1 O34 140.91(11) . .
O1W Nd1 O34 134.07(12) . .
O272 Nd1 O34 67.30(11) 4_565 .
O31 Nd1 O34 65.45(11) . .
O2W Nd1 O34 81.02(12) . .
O271 Nd1 N11 72.04(13) . .
O171 Nd1 N11 62.95(12) . .
O1W Nd1 N11 125.46(12) . .
O272 Nd1 N11 62.55(12) 4_565 .
O31 Nd1 N11 144.72(13) . .
O2W Nd1 N11 128.26(12) . .
O34 Nd1 N11 100.34(12) . .
O271 Nd1 N21 62.87(11) . .
O171 Nd1 N21 72.64(12) . .
O1W Nd1 N21 69.39(11) . .
O272 Nd1 N21 128.24(12) 4_565 .
O31 Nd1 N21 99.83(12) . .
O2W Nd1 N21 140.27(11) . .
O34 Nd1 N21 136.44(12) . .
N11 Nd1 N21 67.42(12) . .
O282 Nd2 O33 89.16(11) 4_565 2_664
O282 Nd2 O281 136.06(12) 4_565 1_545
O33 Nd2 O281 79.70(12) 2_664 1_545
O282 Nd2 O36 140.02(13) 4_565 2_664
O33 Nd2 O36 66.12(11) 2_664 2_664
O281 Nd2 O36 72.31(12) 1_545 2_664
O282 Nd2 O3W 76.35(12) 4_565 .
O33 Nd2 O3W 136.94(12) 2_664 .
O281 Nd2 O3W 83.34(13) 1_545 .
O36 Nd2 O3W 142.93(12) 2_664 .
O282 Nd2 O172 136.68(11) 4_565 4_465
O33 Nd2 O172 133.85(11) 2_664 4_465
O281 Nd2 O172 69.73(10) 1_545 4_465
O36 Nd2 O172 71.99(11) 2_664 4_465
O3W Nd2 O172 73.55(11) . 4_465
O282 Nd2 O181 75.89(13) 4_565 .
O33 Nd2 O181 78.45(12) 2_664 .
O281 Nd2 O181 140.56(12) 1_545 .
O36 Nd2 O181 68.91(12) 2_664 .
O3W Nd2 O181 133.74(12) . .
O172 Nd2 O181 104.05(11) 4_465 .
O282 Nd2 N13 75.42(12) 4_565 .
O33 Nd2 N13 140.12(12) 2_664 .
O281 Nd2 N13 135.86(11) 1_545 .
O36 Nd2 N13 103.15(12) 2_664 .
O3W Nd2 N13 75.32(12) . .
O172 Nd2 N13 67.34(11) 4_465 .
O181 Nd2 N13 62.29(12) . .
O282 Nd2 N23 74.19(12) 4_565 1_545
O33 Nd2 N23 68.11(12) 2_664 1_545
O281 Nd2 N23 62.18(12) 1_545 1_545
O36 Nd2 N23 119.37(12) 2_664 1_545
O3W Nd2 N23 68.95(12) . 1_545
O172 Nd2 N23 120.95(12) 4_465 1_545
O181 Nd2 N23 134.82(12) . 1_545
N13 Nd2 N23 137.35(13) . 1_545
C12 N11 C16 116.5(4) . .
C12 N11 Nd1 125.1(3) . .
C16 N11 Nd1 115.0(3) . .
N13 C12 N11 125.8(5) . .
N13 C12 H12 117.1 . .
N11 C12 H12 117.1 . .
C12 N13 C14 116.8(4) . .
C12 N13 Nd2 126.5(3) . .
C14 N13 Nd2 116.6(3) . .
N13 C14 C15 121.6(4) . .
N13 C14 C18 117.6(4) . .
C15 C14 C18 120.7(4) . .
C16 C15 C14 117.5(4) . .
C16 C15 H15 121.3 . .
C14 C15 H15 121.3 . .
N11 C16 C15 121.7(4) . .
N11 C16 C17 116.2(4) . .
C15 C16 C17 121.8(4) . .
O172 C17 O171 126.5(4) . .
O172 C17 C16 117.1(4) . .
O171 C17 C16 116.4(4) . .
C17 O171 Nd1 126.8(3) . .
C17 O172 Nd2 136.6(3) . 4_565
O182 C18 O181 127.3(5) . .
O182 C18 C14 116.3(4) . .
O181 C18 C14 116.4(4) . .
C18 O181 Nd2 126.9(3) . .
C26 N21 C22 116.9(4) . .
C26 N21 Nd1 114.9(3) . .
C22 N21 Nd1 128.2(3) . .
N23 C22 N21 125.4(5) . .
N23 C22 H22 117.3 . .
N21 C22 H22 117.3 . .
C22 N23 C24 116.7(4) . .
C22 N23 Nd2 128.8(3) . 1_565
C24 N23 Nd2 114.4(3) . 1_565
N23 C24 C25 121.9(4) . .
N23 C24 C28 117.1(4) . .
C25 C24 C28 121.0(4) . .
C26 C25 C24 116.8(4) . .
C26 C25 H25 121.6 . .
C24 C25 H25 121.6 . .
N21 C26 C25 122.2(4) . .
N21 C26 C27 116.4(4) . .
C25 C26 C27 121.3(4) . .
O272 C27 O271 125.9(4) . .
O272 C27 C26 115.9(4) . .
O271 C27 C26 118.1(4) . .
C27 O271 Nd1 127.6(3) . .
C27 O272 Nd1 145.1(3) . 4_465
O281 C28 O282 126.6(4) . .
O281 C28 C24 117.0(4) . .
O282 C28 C24 116.4(4) . .
C28 O281 Nd2 129.4(3) . 1_565
C28 O282 Nd2 154.3(3) . 4_465
C32 O31 Nd1 119.9(3) . .
O31 C32 O33 127.0(4) . .
O31 C32 C35 117.3(4) . .
O33 C32 C35 115.7(4) . .
C32 O33 Nd2 120.7(3) . 2_665
C35 O34 Nd1 120.1(3) . .
O34 C35 O36 126.9(5) . .
O34 C35 C32 116.0(4) . .
O36 C35 C32 117.1(4) . .
C35 O36 Nd2 119.1(3) . 2_665
Nd1 O1W H11W 135.8 . .
Nd1 O1W H12W 94.8 . .
H11W O1W H12W 105.0 . .
Nd1 O2W H21W 135.0 . .
Nd1 O2W H22W 97.2 . .
H21W O2W H22W 100.1 . .
Nd2 O3W H31W 100.3 . .
Nd2 O3W H32W 129.2 . .
H31W O3W H32W 103.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd1 O271 2.434(3) .
Nd1 O171 2.446(3) .
Nd1 O1W 2.451(3) .
Nd1 O272 2.470(3) 4_565
Nd1 O31 2.472(3) .
Nd1 O2W 2.473(4) .
Nd1 O34 2.482(3) .
Nd1 N11 2.670(4) .
Nd1 N21 2.737(4) .
Nd2 O282 2.392(3) 4_565
Nd2 O33 2.446(3) 2_664
Nd2 O281 2.446(3) 1_545
Nd2 O36 2.468(4) 2_664
Nd2 O3W 2.479(4) .
Nd2 O172 2.491(3) 4_465
Nd2 O181 2.501(4) .
Nd2 N13 2.698(4) .
Nd2 N23 2.755(4) 1_545
N11 C12 1.337(6) .
N11 C16 1.355(6) .
C12 N13 1.334(6) .
C12 H12 0.9300 .
N13 C14 1.336(6) .
C14 C15 1.394(6) .
C14 C18 1.511(7) .
C15 C16 1.366(6) .
C15 H15 0.9300 .
C16 C17 1.515(7) .
C17 O172 1.257(6) .
C17 O171 1.261(6) .
O172 Nd2 2.491(3) 4_565
C18 O182 1.220(6) .
C18 O181 1.268(6) .
N21 C26 1.334(6) .
N21 C22 1.336(6) .
C22 N23 1.335(6) .
C22 H22 0.9300 .
N23 C24 1.341(6) .
N23 Nd2 2.755(4) 1_565
C24 C25 1.386(7) .
C24 C28 1.522(6) .
C25 C26 1.376(6) .
C25 H25 0.9300 .
C26 C27 1.517(6) .
C27 O272 1.250(6) .
C27 O271 1.264(6) .
O272 Nd1 2.470(3) 4_465
C28 O281 1.245(5) .
C28 O282 1.248(6) .
O281 Nd2 2.446(3) 1_565
O282 Nd2 2.392(3) 4_465
O31 C32 1.242(6) .
C32 O33 1.257(6) .
C32 C35 1.548(7) .
O33 Nd2 2.446(3) 2_665
O34 C35 1.251(6) .
C35 O36 1.266(6) .
O36 Nd2 2.468(4) 2_665
O1W H11W 0.8633 .
O1W H12W 0.8776 .
O2W H21W 0.8859 .
O2W H22W 0.8904 .
O3W H31W 0.8772 .
O3W H32W 0.8624 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O4W 0.86 1.97 2.814(6) 164.3 1_565
O1W H12W O182 0.88 1.84 2.686(6) 160.5 3_655
O2W H21W O181 0.89 1.96 2.791(5) 156.3 3_655
O2W H22W O271 0.89 1.93 2.769(4) 156.6 4_565
O3W H31W O171 0.88 1.87 2.712(5) 160.9 4_465
O3W H32W O4W 0.86 1.97 2.818(6) 168.0 .
