# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-Eu
_database_code_depnum_ccdc_archive 'CCDC 1016547'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':k2O,O'':kO''')europium(III)]
_chemical_formula_moiety         'C6 H4 Eu N3 O8'
_chemical_formula_structural     'C6 H4 Eu N3 O8'
_chemical_formula_sum            'C6 H4 Eu N3 O8'
_chemical_formula_weight         398.08
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5841(2)
_cell_length_b                   12.0772(2)
_cell_length_c                   9.4047(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.127(2)
_cell_angle_gamma                90.00
_cell_volume                     967.47(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7007
_cell_measurement_theta_min      5.99
_cell_measurement_theta_max      73.14

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      2.74(1)
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    46.924
_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_absorpt_correction_T_min  0.063
_exptl_absorpt_correction_T_max  0.304

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7007
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         5.99
_diffrn_reflns_theta_max         73.14
_reflns_number_total             1922
_reflns_number_gt                1841
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections. The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement. R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0256P)²+0.2786P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1922
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0487
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.365273(18) 0.638565(13) 0.902569(17) 0.01021(7) Uani 1 1 d . . .
N11 N 0.2394(3) 0.6661(2) 1.1518(3) 0.0150(5) Uani 1 1 d . . .
C12 C 0.1329(3) 0.7369(2) 1.1887(3) 0.0157(6) Uani 1 1 d . . .
H12 H 0.0726 0.7743 1.1149 0.019 Uiso 1 1 calc R . .
N13 N 0.1048(3) 0.7592(2) 1.3218(3) 0.0135(5) Uani 1 1 d . . .
C14 C 0.2021(3) 0.7120(2) 1.4284(3) 0.0145(6) Uani 1 1 d . . .
C15 C 0.3149(4) 0.6348(2) 1.4017(4) 0.0156(6) Uani 1 1 d . . .
H15 H 0.3804 0.6009 1.4753 0.019 Uiso 1 1 calc R . .
C16 C 0.3239(3) 0.6116(2) 1.2601(3) 0.0142(6) Uani 1 1 d . . .
C17 C 0.4224(3) 0.5195(2) 1.2128(3) 0.0142(6) Uani 1 1 d . . .
O171 O 0.3938(2) 0.49118(17) 1.0811(2) 0.0150(4) Uani 1 1 d . . .
O172 O 0.5235(3) 0.47309(18) 1.2974(2) 0.0186(4) Uani 1 1 d . . .
C18 C 0.1770(3) 0.7454(2) 1.5789(3) 0.0132(5) Uani 1 1 d . . .
O181 O 0.0550(2) 0.79929(18) 1.5929(2) 0.0155(4) Uani 1 1 d . . .
O182 O 0.2818(2) 0.71721(18) 1.6769(2) 0.0154(4) Uani 1 1 d . . .
O21 O 0.0630(3) 0.6395(2) 0.8649(3) 0.0233(5) Uani 1 1 d . . .
N22 N 0.0530(3) 0.5583(2) 0.7813(3) 0.0209(6) Uani 1 1 d . . .
O23 O 0.1753(3) 0.4977(2) 0.7832(3) 0.0240(5) Uani 1 1 d . . .
O24 O -0.0658(3) 0.5380(2) 0.6980(3) 0.0308(6) Uani 1 1 d . . .
O1W O 0.3093(3) 0.83447(19) 0.9400(2) 0.0188(4) Uani 1 1 d . . .
H11W H 0.3094 0.8806 0.8715 0.028 Uiso 1 1 d . . .
H12W H 0.3400 0.8722 1.0149 0.028 Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O182 2.354(2) 1_554 ?
Eu1 O181 2.387(2) 4_675 ?
Eu1 O171 2.438(2) . ?
Eu1 O1W 2.448(2) . ?
Eu1 O23 2.522(2) . ?
Eu1 O21 2.575(2) . ?
Eu1 O171 2.584(2) 3_667 ?
Eu1 O172 2.590(2) 3_667 ?
Eu1 N13 2.592(2) 4_675 ?
Eu1 N11 2.721(3) . ?
Eu1 C17 2.938(3) 3_667 ?
Eu1 N22 2.944(3) . ?
N11 C12 1.328(4) . ?
N11 C16 1.347(4) . ?
C12 N13 1.331(4) . ?
C12 H12 0.9300 . ?
N13 C14 1.349(4) . ?
N13 Eu1 2.592(2) 4_576 ?
C14 C15 1.389(4) . ?
C14 C18 1.513(4) . ?
C15 C16 1.373(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.498(4) . ?
C17 O172 1.236(4) . ?
C17 O171 1.279(4) . ?
C17 Eu1 2.938(3) 3_667 ?
O171 Eu1 2.584(2) 3_667 ?
O172 Eu1 2.590(2) 3_667 ?
C18 O182 1.253(4) . ?
C18 O181 1.253(4) . ?
O181 Eu1 2.387(2) 4_576 ?
O182 Eu1 2.354(2) 1_556 ?
O21 N22 1.253(4) . ?
N22 O24 1.231(4) . ?
N22 O23 1.279(4) . ?
O1W H11W 0.8517 . ?
O1W H12W 0.8532 . ?

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
_geom_angle_publ_flag
O182 Eu1 O181 130.71(8) 1_554 4_675 ?
O182 Eu1 O171 155.31(7) 1_554 . ?
O181 Eu1 O171 73.28(7) 4_675 . ?
O182 Eu1 O1W 72.33(8) 1_554 . ?
O181 Eu1 O1W 73.51(8) 4_675 . ?
O171 Eu1 O1W 127.67(7) . . ?
O182 Eu1 O23 76.30(8) 1_554 . ?
O181 Eu1 O23 152.80(8) 4_675 . ?
O171 Eu1 O23 79.52(8) . . ?
O1W Eu1 O23 126.04(8) . . ?
O182 Eu1 O21 71.66(8) 1_554 . ?
O181 Eu1 O21 133.16(7) 4_675 . ?
O171 Eu1 O21 96.38(7) . . ?
O1W Eu1 O21 78.65(8) . . ?
O23 Eu1 O21 49.98(8) . . ?
O182 Eu1 O171 116.75(7) 1_554 3_667 ?
O181 Eu1 O171 71.30(7) 4_675 3_667 ?
O171 Eu1 O171 60.35(8) . 3_667 ?
O1W Eu1 O171 138.36(7) . 3_667 ?
O23 Eu1 O171 94.92(7) . 3_667 ?
O21 Eu1 O171 142.77(7) . 3_667 ?
O182 Eu1 O172 69.76(7) 1_554 3_667 ?
O181 Eu1 O172 115.43(7) 4_675 3_667 ?
O171 Eu1 O172 96.04(7) . 3_667 ?
O1W Eu1 O172 134.75(7) . 3_667 ?
O23 Eu1 O172 66.52(8) . 3_667 ?
O21 Eu1 O172 110.98(7) . 3_667 ?
O171 Eu1 O172 50.45(7) 3_667 3_667 ?
O182 Eu1 N13 72.99(8) 1_554 4_675 ?
O181 Eu1 N13 65.01(8) 4_675 4_675 ?
O171 Eu1 N13 122.29(7) . 4_675 ?
O1W Eu1 N13 76.03(8) . 4_675 ?
O23 Eu1 N13 133.13(8) . 4_675 ?
O21 Eu1 N13 141.28(8) . 4_675 ?
O171 Eu1 N13 69.40(7) 3_667 4_675 ?
O172 Eu1 N13 70.02(7) 3_667 4_675 ?
O182 Eu1 N11 128.19(8) 1_554 . ?
O181 Eu1 N11 67.82(7) 4_675 . ?
O171 Eu1 N11 60.84(7) . . ?
O1W Eu1 N11 69.63(8) . . ?
O23 Eu1 N11 99.34(8) . . ?
O21 Eu1 N11 67.47(8) . . ?
O171 Eu1 N11 115.06(7) 3_667 . ?
O172 Eu1 N11 155.59(8) 3_667 . ?
N13 Eu1 N11 127.48(8) 4_675 . ?
O182 Eu1 C17 93.59(8) 1_554 3_667 ?
O181 Eu1 C17 94.84(8) 4_675 3_667 ?
O171 Eu1 C17 76.48(7) . 3_667 ?
O1W Eu1 C17 145.35(8) . 3_667 ?
O23 Eu1 C17 78.09(8) . 3_667 ?
O21 Eu1 C17 127.78(8) . 3_667 ?
O171 Eu1 C17 25.78(8) 3_667 3_667 ?
O172 Eu1 C17 24.83(8) 3_667 3_667 ?
N13 Eu1 C17 69.54(8) 4_675 3_667 ?
N11 Eu1 C17 136.77(8) . 3_667 ?
O182 Eu1 N22 67.84(8) 1_554 . ?
O181 Eu1 N22 153.89(7) 4_675 . ?
O171 Eu1 N22 92.02(8) . . ?
O1W Eu1 N22 100.85(8) . . ?
O23 Eu1 N22 25.59(8) . . ?
O21 Eu1 N22 25.12(8) . . ?
O171 Eu1 N22 120.46(7) 3_667 . ?
O172 Eu1 N22 86.97(7) 3_667 . ?
N13 Eu1 N22 139.52(8) 4_675 . ?
N11 Eu1 N22 86.23(8) . . ?
C17 Eu1 N22 102.69(8) 3_667 . ?
C12 N11 C16 116.2(3) . . ?
C12 N11 Eu1 131.6(2) . . ?
C16 N11 Eu1 110.93(18) . . ?
N11 C12 N13 125.9(3) . . ?
N11 C12 H12 117.1 . . ?
N13 C12 H12 117.1 . . ?
C12 N13 C14 116.5(3) . . ?
C12 N13 Eu1 127.9(2) . 4_576 ?
C14 N13 Eu1 115.09(18) . 4_576 ?
N13 C14 C15 122.0(3) . . ?
N13 C14 C18 115.8(3) . . ?
C15 C14 C18 122.1(3) . . ?
C16 C15 C14 115.9(3) . . ?
C16 C15 H15 122.1 . . ?
C14 C15 H15 122.1 . . ?
N11 C16 C15 123.0(3) . . ?
N11 C16 C17 114.2(3) . . ?
C15 C16 C17 122.8(3) . . ?
O172 C17 O171 122.5(3) . . ?
O172 C17 C16 121.5(3) . . ?
O171 C17 C16 116.0(3) . . ?
O172 C17 Eu1 61.64(15) . 3_667 ?
O171 C17 Eu1 61.46(15) . 3_667 ?
C16 C17 Eu1 172.30(19) . 3_667 ?
O172 C17 Eu1 142.9(2) . . ?
O171 C17 Eu1 41.92(14) . . ?
C16 C17 Eu1 84.80(17) . . ?
Eu1 C17 Eu1 89.27(8) 3_667 . ?
C17 O171 Eu1 117.56(18) . . ?
C17 O171 Eu1 92.76(17) . 3_667 ?
Eu1 O171 Eu1 119.65(8) . 3_667 ?
C17 O172 Eu1 93.53(18) . 3_667 ?
O182 C18 O181 126.7(3) . . ?
O182 C18 C14 116.3(3) . . ?
O181 C18 C14 117.1(3) . . ?
C18 O181 Eu1 125.85(19) . 4_576 ?
C18 O182 Eu1 152.08(19) . 1_556 ?
N22 O21 Eu1 94.15(18) . . ?
O24 N22 O21 122.8(3) . . ?
O24 N22 O23 120.6(3) . . ?
O21 N22 O23 116.6(3) . . ?
O24 N22 Eu1 162.7(2) . . ?
O21 N22 Eu1 60.72(16) . . ?
O23 N22 Eu1 58.43(15) . . ?
N22 O23 Eu1 95.98(18) . . ?
Eu1 O1W H11W 120.3 . . ?
Eu1 O1W H12W 126.1 . . ?
H11W O1W H12W 104.2 . . ?

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 O23 0.85 2.04 2.894(3) 175.3 2_556
O1W H12W O24 0.85 2.11 2.960(4) 175.5 4_676

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        73.14
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.100

_exptl_crystal_preparation       'Magnetic properties, Luminescent'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-La
_database_code_depnum_ccdc_archive 'CCDC 1016548'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':k2O,O'':kO''')lanthanum(III)]
_chemical_formula_moiety         'C6 H4 La N3 O8'
_chemical_formula_structural     'C6 H4 La N3 O8'
_chemical_formula_sum            'C6 H4 La N3 O8'
_chemical_formula_weight         385.03
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7220(2)
_cell_length_b                   12.2820(2)
_cell_length_c                   9.5780(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.640(2)
_cell_angle_gamma                90.00
_cell_volume                     1019.15(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7144
_cell_measurement_theta_min      5.88
_cell_measurement_theta_max      73.07

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      2.51(1)
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    32.887
_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_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_T_max  0.396

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7144
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         5.88
_diffrn_reflns_theta_max         73.07
_reflns_number_total             2015
_reflns_number_gt                1964
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections. The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement. R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0276P)²+0.2136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2015
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0170
_refine_ls_wR_factor_ref         0.0443
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.360888(14) 0.636462(10) 0.900562(13) 0.00991(6) Uani 1 1 d . . .
N11 N 0.2395(2) 0.66355(17) 1.1560(2) 0.0125(4) Uani 1 1 d . . .
C12 C 0.1348(3) 0.73376(19) 1.1922(3) 0.0143(5) Uani 1 1 d . . .
H12 H 0.0741 0.7690 1.1197 0.017 Uiso 1 1 calc R . .
N13 N 0.1092(2) 0.75794(16) 1.3230(2) 0.0128(4) Uani 1 1 d . . .
C14 C 0.2047(3) 0.71244(19) 1.4281(3) 0.0126(4) Uani 1 1 d . . .
C15 C 0.3154(3) 0.63700(18) 1.4025(3) 0.0132(5) Uani 1 1 d . . .
H15 H 0.3805 0.6051 1.4749 0.016 Uiso 1 1 calc R . .
C16 C 0.3241(3) 0.6115(2) 1.2628(3) 0.0127(5) Uani 1 1 d . . .
C17 C 0.4232(3) 0.52094(19) 1.2183(3) 0.0125(5) Uani 1 1 d . . .
O171 O 0.39733(19) 0.49237(13) 1.08908(17) 0.0133(3) Uani 1 1 d . . .
O172 O 0.5218(2) 0.47630(15) 1.30305(18) 0.0168(4) Uani 1 1 d . . .
C18 C 0.1796(3) 0.74709(19) 1.5757(3) 0.0124(4) Uani 1 1 d . . .
O181 O 0.05964(19) 0.79918(14) 1.59015(18) 0.0143(3) Uani 1 1 d . . .
O182 O 0.28259(19) 0.71983(14) 1.67119(17) 0.0143(3) Uani 1 1 d . . .
O21 O 0.0529(2) 0.63479(15) 0.8618(2) 0.0239(4) Uani 1 1 d . . .
N22 N 0.0441(3) 0.55736(19) 0.7751(2) 0.0214(5) Uani 1 1 d . . .
O23 O 0.1633(2) 0.49740(16) 0.7739(2) 0.0249(4) Uani 1 1 d . . .
O24 O -0.0727(2) 0.53968(19) 0.6932(2) 0.0328(5) Uani 1 1 d . . .
O1W O 0.3090(2) 0.83788(15) 0.9424(2) 0.0192(4) Uani 1 1 d . . .
H11W H 0.3045 0.8859 0.8781 0.029 Uiso 1 1 d . . .
H12W H 0.3547 0.8701 1.0147 0.029 Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O182 2.4483(16) 1_554 ?
La1 O181 2.4898(17) 4_675 ?
La1 O171 2.5220(16) . ?
La1 O1W 2.5548(19) . ?
La1 O23 2.6218(19) . ?
La1 O171 2.6291(16) 3_667 ?
La1 O21 2.669(2) . ?
La1 O172 2.6887(17) 3_667 ?
La1 N13 2.701(2) 4_675 ?
La1 N11 2.796(2) . ?
La1 C17 3.013(2) 3_667 ?
La1 N22 3.042(2) . ?
N11 C12 1.331(3) . ?
N11 C16 1.350(3) . ?
C12 N13 1.331(3) . ?
C12 H12 0.9300 . ?
N13 C14 1.351(3) . ?
N13 La1 2.701(2) 4_576 ?
C14 C15 1.381(3) . ?
C14 C18 1.516(3) . ?
C15 C16 1.384(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.501(3) . ?
C17 O172 1.240(3) . ?
C17 O171 1.281(3) . ?
C17 La1 3.013(2) 3_667 ?
O171 La1 2.6291(16) 3_667 ?
O172 La1 2.6887(17) 3_667 ?
C18 O181 1.248(3) . ?
C18 O182 1.251(3) . ?
O181 La1 2.4898(17) 4_576 ?
O182 La1 2.4483(16) 1_556 ?
O21 N22 1.260(3) . ?
N22 O24 1.231(3) . ?
N22 O23 1.275(3) . ?
O1W H11W 0.8509 . ?
O1W H12W 0.8550 . ?

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
_geom_angle_publ_flag
O182 La1 O181 128.32(6) 1_554 4_675 ?
O182 La1 O171 159.21(6) 1_554 . ?
O181 La1 O171 71.41(5) 4_675 . ?
O182 La1 O1W 72.53(6) 1_554 . ?
O181 La1 O1W 72.50(6) 4_675 . ?
O171 La1 O1W 125.24(6) . . ?
O182 La1 O23 75.94(6) 1_554 . ?
O181 La1 O23 155.38(6) 4_675 . ?
O171 La1 O23 84.02(6) . . ?
O1W La1 O23 125.77(6) . . ?
O182 La1 O171 115.14(5) 1_554 3_667 ?
O181 La1 O171 71.08(5) 4_675 3_667 ?
O171 La1 O171 61.09(6) . 3_667 ?
O1W La1 O171 137.12(6) . 3_667 ?
O23 La1 O171 96.13(6) . 3_667 ?
O182 La1 O21 72.94(6) 1_554 . ?
O181 La1 O21 135.11(6) 4_675 . ?
O171 La1 O21 97.80(6) . . ?
O1W La1 O21 80.53(6) . . ?
O23 La1 O21 48.21(6) . . ?
O171 La1 O21 142.24(5) 3_667 . ?
O182 La1 O172 69.79(5) 1_554 3_667 ?
O181 La1 O172 113.66(5) 4_675 3_667 ?
O171 La1 O172 97.52(5) . 3_667 ?
O1W La1 O172 134.57(6) . 3_667 ?
O23 La1 O172 67.28(6) . 3_667 ?
O171 La1 O172 49.20(5) 3_667 3_667 ?
O21 La1 O172 110.88(6) . 3_667 ?
O182 La1 N13 72.64(6) 1_554 4_675 ?
O181 La1 N13 62.32(6) 4_675 4_675 ?
O171 La1 N13 119.68(6) . 4_675 ?
O1W La1 N13 74.96(6) . 4_675 ?
O23 La1 N13 133.66(6) . 4_675 ?
O171 La1 N13 68.55(6) 3_667 4_675 ?
O21 La1 N13 142.32(6) . 4_675 ?
O172 La1 N13 70.33(6) 3_667 4_675 ?
O182 La1 N11 129.87(6) 1_554 . ?
O181 La1 N11 68.04(6) 4_675 . ?
O171 La1 N11 59.07(6) . . ?
O1W La1 N11 69.85(6) . . ?
O23 La1 N11 100.80(6) . . ?
O171 La1 N11 114.94(6) 3_667 . ?
O21 La1 N11 69.26(6) . . ?
O172 La1 N11 155.55(6) 3_667 . ?
N13 La1 N11 125.47(6) 4_675 . ?
O182 La1 C17 92.92(6) 1_554 3_667 ?
O181 La1 C17 93.80(6) 4_675 3_667 ?
O171 La1 C17 77.74(6) . 3_667 ?
O1W La1 C17 144.14(6) . 3_667 ?
O23 La1 C17 79.24(6) . 3_667 ?
O171 La1 C17 25.08(6) 3_667 3_667 ?
O21 La1 C17 127.28(6) . 3_667 ?
O172 La1 C17 24.29(6) 3_667 3_667 ?
N13 La1 C17 69.39(6) 4_675 3_667 ?
N11 La1 C17 136.34(6) . 3_667 ?
O182 La1 N22 68.45(6) 1_554 . ?
O181 La1 N22 156.00(6) 4_675 . ?
O171 La1 N22 95.30(6) . . ?
O1W La1 N22 101.65(6) . . ?
O23 La1 N22 24.61(6) . . ?
O171 La1 N22 120.70(6) 3_667 . ?
O21 La1 N22 24.37(6) . . ?
O172 La1 N22 87.32(6) 3_667 . ?
N13 La1 N22 139.91(6) 4_675 . ?
N11 La1 N22 88.02(6) . . ?
C17 La1 N22 102.98(6) 3_667 . ?
C12 N11 C16 116.2(2) . . ?
C12 N11 La1 130.19(16) . . ?
C16 N11 La1 112.20(15) . . ?
N11 C12 N13 125.7(2) . . ?
N11 C12 H12 117.1 . . ?
N13 C12 H12 117.1 . . ?
C12 N13 C14 116.9(2) . . ?
C12 N13 La1 126.37(15) . 4_576 ?
C14 N13 La1 116.01(15) . 4_576 ?
N13 C14 C15 121.9(2) . . ?
N13 C14 C18 115.8(2) . . ?
C15 C14 C18 122.2(2) . . ?
C14 C15 C16 116.1(2) . . ?
C14 C15 H15 121.9 . . ?
C16 C15 H15 121.9 . . ?
N11 C16 C15 122.6(2) . . ?
N11 C16 C17 114.7(2) . . ?
C15 C16 C17 122.7(2) . . ?
O172 C17 O171 122.9(2) . . ?
O172 C17 C16 121.4(2) . . ?
O171 C17 C16 115.8(2) . . ?
O172 C17 La1 63.06(13) . 3_667 ?
O171 C17 La1 60.46(12) . 3_667 ?
C16 C17 La1 171.45(16) . 3_667 ?
C17 O171 La1 119.54(14) . . ?
C17 O171 La1 94.46(13) . 3_667 ?
La1 O171 La1 118.91(6) . 3_667 ?
C17 O172 La1 92.65(14) . 3_667 ?
O181 C18 O182 126.6(2) . . ?
O181 C18 C14 117.4(2) . . ?
O182 C18 C14 116.0(2) . . ?
C18 O181 La1 127.15(15) . 4_576 ?
C18 O182 La1 150.46(16) . 1_556 ?
N22 O21 La1 94.63(15) . . ?
O24 N22 O21 122.4(2) . . ?
O24 N22 O23 120.6(2) . . ?
O21 N22 O23 117.0(2) . . ?
O24 N22 La1 162.77(17) . . ?
O21 N22 La1 60.99(13) . . ?
O23 N22 La1 58.91(12) . . ?
N22 O23 La1 96.47(14) . . ?
La1 O1W H11W 123.5 . . ?
La1 O1W H12W 120.1 . . ?
H11W O1W H12W 104.1 . . ?

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 O23 0.85 2.04 2.882(3) 169.4 2_556
O1W H12W O24 0.85 2.07 2.919(3) 169.8 4_676

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        73.07
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.091

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-Nd
_database_code_depnum_ccdc_archive 'CCDC 1016549'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':k2O,O'':kO''')neodymium(III)]
_chemical_formula_moiety         'C6 H4 N3 Nd O8'
_chemical_formula_structural     'C6 H4 N3 Nd O8'
_chemical_formula_sum            'C6 H4 N3 Nd O8'
_chemical_formula_weight         390.36
_chemical_compound_source        'synthesis as described'


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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6320(2)
_cell_length_b                   12.1470(3)
_cell_length_c                   9.4520(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8790(10)
_cell_angle_gamma                90.00
_cell_volume                     983.94(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6236
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.06
_cell_oxdiff_twin_number         2

loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.9490 0.2342 -0.0447 0.4744 0.9404 0.1403 0.0806 0.0366 -0.9880

loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.8696 6464 128
2 0.1304 6382 128

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      2.64(1)
_exptl_crystal_density_diffrn    2.635
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    5.322
_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_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_T_max  0.820

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6236
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         27.06
_reflns_number_total             2147
_reflns_number_gt                1858
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          Twin

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2147
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0426
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.36344(2) 0.637518(16) 0.901876(18) 0.00642(6) Uani 1 1 d . . .
N11 N 0.2396(4) 0.6646(2) 1.1531(3) 0.0090(7) Uani 1 1 d . . .
C12 C 0.1333(4) 0.7347(3) 1.1898(4) 0.0102(8) Uani 1 1 d . . .
H12 H 0.0721 0.7708 1.1164 0.012 Uiso 1 1 calc R . .
N13 N 0.1065(3) 0.7580(2) 1.3229(3) 0.0092(7) Uani 1 1 d . . .
C14 C 0.2034(4) 0.7120(3) 1.4276(3) 0.0083(7) Uani 1 1 d . . .
C15 C 0.3143(4) 0.6359(3) 1.4020(3) 0.0084(7) Uani 1 1 d . . .
H15 H 0.3795 0.6032 1.4756 0.010 Uiso 1 1 calc R . .
C16 C 0.3235(4) 0.6108(3) 1.2603(3) 0.0072(7) Uani 1 1 d . . .
C17 C 0.4224(4) 0.5196(3) 1.2153(4) 0.0096(8) Uani 1 1 d . . .
O171 O 0.3952(3) 0.4909(2) 1.0841(2) 0.0098(5) Uani 1 1 d . . .
O172 O 0.5229(3) 0.4740(2) 1.3001(2) 0.0130(6) Uani 1 1 d . . .
C18 C 0.1778(4) 0.7465(3) 1.5781(3) 0.0067(7) Uani 1 1 d . . .
O181 O 0.0565(3) 0.7988(2) 1.5918(2) 0.0094(5) Uani 1 1 d . . .
O182 O 0.2819(3) 0.7183(2) 1.6748(2) 0.0095(5) Uani 1 1 d . . .
O21 O 0.0584(3) 0.6374(2) 0.8646(3) 0.0183(6) Uani 1 1 d . . .
N22 N 0.0495(4) 0.5576(3) 0.7788(3) 0.0167(8) Uani 1 1 d . . .
O23 O 0.1711(3) 0.4976(2) 0.7786(3) 0.0190(6) Uani 1 1 d . . .
O24 O -0.0684(4) 0.5392(3) 0.6967(3) 0.0294(8) Uani 1 1 d . . .
O1W O 0.3090(3) 0.8359(2) 0.9418(2) 0.0137(6) Uani 1 1 d . . .
H11W H 0.3111 0.8804 0.8716 0.021 Uiso 1 1 d . . .
H12W H 0.3395 0.8758 1.0147 0.021 Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O182 2.388(2) 1_554 ?
Nd1 O181 2.425(2) 4_675 ?
Nd1 O171 2.470(2) . ?
Nd1 O1W 2.493(2) . ?
Nd1 O23 2.558(3) . ?
Nd1 O171 2.594(2) 3_667 ?
Nd1 O21 2.614(3) . ?
Nd1 O172 2.626(2) 3_667 ?
Nd1 N13 2.636(3) 4_675 ?
Nd1 N11 2.738(3) . ?
Nd1 C17 2.962(4) 3_667 ?
Nd1 N22 2.981(3) . ?
N11 C12 1.328(4) . ?
N11 C16 1.343(4) . ?
C12 N13 1.336(4) . ?
C12 H12 0.9300 . ?
N13 C14 1.339(5) . ?
N13 Nd1 2.636(3) 4_576 ?
C14 C15 1.373(5) . ?
C14 C18 1.525(4) . ?
C15 C16 1.386(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.491(5) . ?
C17 O172 1.238(4) . ?
C17 O171 1.283(4) . ?
C17 Nd1 2.962(4) 3_667 ?
O171 Nd1 2.594(2) 3_667 ?
O172 Nd1 2.626(2) 3_667 ?
C18 O181 1.245(4) . ?
C18 O182 1.250(4) . ?
O181 Nd1 2.425(2) 4_576 ?
O182 Nd1 2.388(2) 1_556 ?
N22 O24 1.224(4) . ?
N22 O21 1.260(4) . ?
N22 O23 1.278(4) . ?
O1W H11W 0.8575 . ?
O1W H12W 0.8576 . ?

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
_geom_angle_publ_flag
O182 Nd1 O181 129.54(8) 1_554 4_675 ?
O182 Nd1 O171 156.82(8) 1_554 . ?
O181 Nd1 O171 72.82(8) 4_675 . ?
O182 Nd1 O1W 72.42(8) 1_554 . ?
O181 Nd1 O1W 72.84(9) 4_675 . ?
O171 Nd1 O1W 126.77(7) . . ?
O182 Nd1 O23 76.02(9) 1_554 . ?
O181 Nd1 O23 154.20(8) 4_675 . ?
O171 Nd1 O23 81.40(8) . . ?
O1W Nd1 O23 125.98(9) . . ?
O182 Nd1 O171 116.21(7) 1_554 3_667 ?
O181 Nd1 O171 71.18(8) 4_675 3_667 ?
O171 Nd1 O171 60.62(8) . 3_667 ?
O1W Nd1 O171 137.62(8) . 3_667 ?
O23 Nd1 O171 95.58(8) . 3_667 ?
O182 Nd1 O21 72.27(8) 1_554 . ?
O181 Nd1 O21 133.76(8) 4_675 . ?
O171 Nd1 O21 96.85(8) . . ?
O1W Nd1 O21 79.39(9) . . ?
O23 Nd1 O21 49.43(8) . . ?
O171 Nd1 O21 142.79(8) 3_667 . ?
O182 Nd1 O172 69.78(8) 1_554 3_667 ?
O181 Nd1 O172 114.79(8) 4_675 3_667 ?
O171 Nd1 O172 96.62(8) . 3_667 ?
O1W Nd1 O172 134.65(7) . 3_667 ?
O23 Nd1 O172 66.70(8) . 3_667 ?
O171 Nd1 O172 50.11(7) 3_667 3_667 ?
O21 Nd1 O172 111.09(8) . 3_667 ?
O182 Nd1 N13 72.92(9) 1_554 4_675 ?
O181 Nd1 N13 63.67(8) 4_675 4_675 ?
O171 Nd1 N13 121.28(9) . 4_675 ?
O1W Nd1 N13 75.42(9) . 4_675 ?
O23 Nd1 N13 133.35(8) . 4_675 ?
O171 Nd1 N13 69.03(8) 3_667 4_675 ?
O21 Nd1 N13 141.75(9) . 4_675 ?
O172 Nd1 N13 70.30(8) 3_667 4_675 ?
O182 Nd1 N11 128.77(9) 1_554 . ?
O181 Nd1 N11 67.97(8) 4_675 . ?
O171 Nd1 N11 60.26(8) . . ?
O1W Nd1 N11 69.66(8) . . ?
O23 Nd1 N11 100.09(8) . . ?
O171 Nd1 N11 115.01(8) 3_667 . ?
O21 Nd1 N11 68.00(8) . . ?
O172 Nd1 N11 155.69(8) 3_667 . ?
N13 Nd1 N11 126.50(9) 4_675 . ?
O182 Nd1 C17 93.37(9) 1_554 3_667 ?
O181 Nd1 C17 94.47(9) 4_675 3_667 ?
O171 Nd1 C17 76.96(9) . 3_667 ?
O1W Nd1 C17 144.77(9) . 3_667 ?
O23 Nd1 C17 78.56(9) . 3_667 ?
O171 Nd1 C17 25.60(8) 3_667 3_667 ?
O21 Nd1 C17 127.78(9) . 3_667 ?
O172 Nd1 C17 24.67(9) 3_667 3_667 ?
N13 Nd1 C17 69.55(9) 4_675 3_667 ?
N11 Nd1 C17 136.68(9) . 3_667 ?
O182 Nd1 N22 68.09(8) 1_554 . ?
O181 Nd1 N22 154.79(8) 4_675 . ?
O171 Nd1 N22 93.27(9) . . ?
O1W Nd1 N22 101.23(9) . . ?
O23 Nd1 N22 25.23(9) . . ?
O171 Nd1 N22 120.76(9) 3_667 . ?
O21 Nd1 N22 24.94(8) . . ?
O172 Nd1 N22 87.12(8) 3_667 . ?
N13 Nd1 N22 139.79(8) 4_675 . ?
N11 Nd1 N22 86.92(9) . . ?
C17 Nd1 N22 102.89(10) 3_667 . ?
C12 N11 C16 116.2(3) . . ?
C12 N11 Nd1 131.1(2) . . ?
C16 N11 Nd1 111.4(2) . . ?
N11 C12 N13 125.8(3) . . ?
N11 C12 H12 117.1 . . ?
N13 C12 H12 117.1 . . ?
C12 N13 C14 116.4(3) . . ?
C12 N13 Nd1 127.0(2) . 4_576 ?
C14 N13 Nd1 116.1(2) . 4_576 ?
N13 C14 C15 122.5(3) . . ?
N13 C14 C18 115.3(3) . . ?
C15 C14 C18 122.1(3) . . ?
C14 C15 C16 116.2(3) . . ?
C14 C15 H15 121.9 . . ?
C16 C15 H15 121.9 . . ?
N11 C16 C15 122.3(3) . . ?
N11 C16 C17 115.0(3) . . ?
C15 C16 C17 122.7(3) . . ?
O172 C17 O171 122.5(3) . . ?
O172 C17 C16 121.9(3) . . ?
O171 C17 C16 115.6(3) . . ?
O172 C17 Nd1 62.26(18) . 3_667 ?
O171 C17 Nd1 60.92(18) . 3_667 ?
C16 C17 Nd1 171.6(2) . 3_667 ?
C17 O171 Nd1 118.1(2) . . ?
C17 O171 Nd1 93.5(2) . 3_667 ?
Nd1 O171 Nd1 119.38(8) . 3_667 ?
C17 O172 Nd1 93.1(2) . 3_667 ?
O181 C18 O182 127.1(3) . . ?
O181 C18 C14 117.0(3) . . ?
O182 C18 C14 115.8(3) . . ?
C18 O181 Nd1 126.7(2) . 4_576 ?
C18 O182 Nd1 151.4(2) . 1_556 ?
O24 N22 O21 122.0(4) . . ?
O24 N22 O23 121.0(3) . . ?
O21 N22 O23 116.9(3) . . ?
O24 N22 Nd1 162.7(2) . . ?
O21 N22 Nd1 61.03(18) . . ?
O23 N22 Nd1 58.53(18) . . ?
N22 O21 Nd1 94.0(2) . . ?
N22 O23 Nd1 96.2(2) . . ?
Nd1 O1W H11W 118.0 . . ?
Nd1 O1W H12W 128.5 . . ?
H11W O1W H12W 103.5 . . ?

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 O23 0.86 2.03 2.883(3) 173.5 2_556
O1W H12W O24 0.86 2.08 2.935(4) 174.1 4_676

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.06
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.139


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Gd
_database_code_depnum_ccdc_archive 'CCDC 1016550'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97


_chemical_name_systematic        
Poly{[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':kO'':kO''')gadolinium(III)]hydrate}
_chemical_formula_moiety         'C6 H4 Gd N3 O8, H2 O'
_chemical_formula_structural     'C6 H4 Gd N3 O8, H2 O'
_chemical_formula_sum            'C6 H6 Gd N3 O9'
_chemical_formula_weight         421.39
_chemical_compound_source        'synthesis as described'


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_Int_Tables_number      173

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'

_cell_length_a                   15.8956(4)
_cell_length_b                   15.8956(4)
_cell_length_c                   7.6028(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1663.64(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11658
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      73.12

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      2.53(1)
_exptl_crystal_density_diffrn    2.524
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             1194
_exptl_absorpt_coefficient_mu    39.239
_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_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_T_max  0.396

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11658
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         73.12
_reflns_number_total             1895
_reflns_number_gt                1760
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          Pseudosymmetry

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0075P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_number_reflns         1895
_refine_ls_number_parameters     173
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_ref         0.0338
_refine_ls_wR_factor_gt          0.0330
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.370211(10) 0.185107(10) 0.25515(4) 0.00838(5) Uani 1 1 d . . .
N11 N 0.5012(2) 0.1524(2) 0.4014(4) 0.0106(5) Uani 1 1 d . . .
C12 C 0.5934(2) 0.1866(2) 0.3507(4) 0.0121(6) Uani 1 1 d . . .
H12 H 0.6195 0.2388 0.2730 0.014 Uiso 1 1 calc R . .
N13 N 0.6513(2) 0.1524(2) 0.4017(4) 0.0104(5) Uani 1 1 d . . .
C14 C 0.6124(2) 0.0760(2) 0.5114(5) 0.0114(6) Uani 1 1 d . . .
C15 C 0.5179(3) 0.0354(3) 0.5708(5) 0.0148(7) Uani 1 1 d . . .
H15 H 0.4916 -0.0172 0.6476 0.018 Uiso 1 1 calc R . .
C16 C 0.4636(2) 0.0764(2) 0.5108(5) 0.0124(7) Uani 1 1 d . . .
C17 C 0.3570(3) 0.0334(3) 0.5581(5) 0.0131(7) Uani 1 1 d . . .
O171 O 0.31327(18) 0.07236(19) 0.4925(4) 0.0174(5) Uani 1 1 d . . .
O172 O 0.32137(18) -0.03986(19) 0.6556(4) 0.0196(6) Uani 1 1 d . . .
C18 C 0.6763(3) 0.0328(3) 0.5576(5) 0.0133(7) Uani 1 1 d . . .
O181 O 0.75941(18) 0.07272(19) 0.4923(4) 0.0176(5) Uani 1 1 d . . .
O182 O 0.63888(19) -0.03946(19) 0.6554(4) 0.0188(5) Uani 1 1 d . . .
O21 O 0.3745(2) 0.1870(2) -0.0764(4) 0.0291(7) Uani 1 1 d . . .
N22 N 0.4657(3) 0.2330(3) -0.0865(5) 0.0275(8) Uani 1 1 d . . .
O23 O 0.51105(19) 0.2553(2) 0.0618(4) 0.0200(5) Uani 1 1 d . . .
O24 O 0.5083(3) 0.2540(4) -0.2259(6) 0.0534(13) Uani 1 1 d . . .
O1W O 0.20275(17) 0.10117(18) 0.1720(4) 0.0172(5) Uani 1 1 d . . .
O2W O 0.09129(18) -0.09146(18) 0.2614(7) 0.0192(6) Uani 1 1 d . . .
H11W H 0.1687 0.0436 0.2128 0.029 Uiso 1 1 d . . .
H12W H 0.1725 0.1301 0.2075 0.029 Uiso 1 1 d . . .
H21W H 0.1147 -0.1171 0.3390 0.029 Uiso 1 1 d . . .
H22W H 0.1111 -0.1110 0.1596 0.029 Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O172 2.365(2) 5_554 ?
Gd1 O182 2.371(2) 2_654 ?
Gd1 O181 2.376(3) 4_665 ?
Gd1 O171 2.380(3) . ?
Gd1 O1W 2.390(2) . ?
Gd1 O23 2.433(3) . ?
Gd1 O21 2.521(3) . ?
Gd1 N13 2.631(3) 4_665 ?
Gd1 N11 2.632(3) . ?
Gd1 N22 2.911(4) . ?
N11 C16 1.336(5) . ?
N11 C12 1.339(4) . ?
C12 N13 1.339(4) . ?
C12 H12 0.9300 . ?
N13 C14 1.342(5) . ?
N13 Gd1 2.631(3) 3_655 ?
C14 C15 1.381(5) . ?
C14 C18 1.524(5) . ?
C15 C16 1.394(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.520(5) . ?
C17 O171 1.244(5) . ?
C17 O172 1.251(5) . ?
O172 Gd1 2.365(2) 6 ?
C18 O182 1.242(5) . ?
C18 O181 1.248(5) . ?
O181 Gd1 2.376(3) 3_655 ?
O182 Gd1 2.371(2) 2_655 ?
O21 N22 1.258(5) . ?
N22 O24 1.212(6) . ?
N22 O23 1.289(5) . ?
O1W H11W 0.8556 . ?
O1W H12W 0.8580 . ?
O2W H21W 0.8967 . ?
O2W H22W 0.9446 . ?

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
_geom_angle_publ_flag
O172 Gd1 O182 142.16(11) 5_554 2_654 ?
O172 Gd1 O181 72.20(11) 5_554 4_665 ?
O182 Gd1 O181 139.17(10) 2_654 4_665 ?
O172 Gd1 O171 139.27(10) 5_554 . ?
O182 Gd1 O171 72.11(10) 2_654 . ?
O181 Gd1 O171 68.42(9) 4_665 . ?
O172 Gd1 O1W 82.32(9) 5_554 . ?
O182 Gd1 O1W 82.14(9) 2_654 . ?
O181 Gd1 O1W 83.31(9) 4_665 . ?
O171 Gd1 O1W 83.23(9) . . ?
O172 Gd1 O23 81.35(10) 5_554 . ?
O182 Gd1 O23 81.23(10) 2_654 . ?
O181 Gd1 O23 136.22(9) 4_665 . ?
O171 Gd1 O23 136.03(9) . . ?
O1W Gd1 O23 127.50(10) . . ?
O172 Gd1 O21 71.52(11) 5_554 . ?
O182 Gd1 O21 71.32(11) 2_654 . ?
O181 Gd1 O21 140.11(11) 4_665 . ?
O171 Gd1 O21 139.87(11) . . ?
O1W Gd1 O21 75.99(10) . . ?
O23 Gd1 O21 51.50(9) . . ?
O172 Gd1 N13 67.08(9) 5_554 4_665 ?
O182 Gd1 N13 137.09(9) 2_654 4_665 ?
O181 Gd1 N13 64.63(9) 4_665 4_665 ?
O171 Gd1 N13 103.77(10) . 4_665 ?
O1W Gd1 N13 140.67(9) . 4_665 ?
O23 Gd1 N13 73.19(9) . 4_665 ?
O21 Gd1 N13 114.11(10) . 4_665 ?
O172 Gd1 N11 137.06(9) 5_554 . ?
O182 Gd1 N11 67.07(9) 2_654 . ?
O181 Gd1 N11 103.79(10) 4_665 . ?
O171 Gd1 N11 64.63(9) . . ?
O1W Gd1 N11 140.53(9) . . ?
O23 Gd1 N11 73.04(9) . . ?
O21 Gd1 N11 113.92(10) . . ?
N13 Gd1 N11 72.73(8) 4_665 . ?
O172 Gd1 N22 74.77(11) 5_554 . ?
O182 Gd1 N22 74.88(11) 2_654 . ?
O181 Gd1 N22 145.64(10) 4_665 . ?
O171 Gd1 N22 145.65(10) . . ?
O1W Gd1 N22 101.50(10) . . ?
O23 Gd1 N22 26.00(10) . . ?
O21 Gd1 N22 25.50(10) . . ?
N13 Gd1 N22 93.92(10) 4_665 . ?
N11 Gd1 N22 93.91(10) . . ?
C16 N11 C12 116.8(3) . . ?
C16 N11 Gd1 113.6(2) . . ?
C12 N11 Gd1 127.7(2) . . ?
N13 C12 N11 125.9(3) . . ?
N13 C12 H12 117.1 . . ?
N11 C12 H12 117.1 . . ?
C12 N13 C14 116.6(3) . . ?
C12 N13 Gd1 127.5(2) . 3_655 ?
C14 N13 Gd1 113.8(2) . 3_655 ?
N13 C14 C15 121.8(3) . . ?
N13 C14 C18 116.2(3) . . ?
C15 C14 C18 121.9(3) . . ?
C14 C15 C16 117.2(3) . . ?
C14 C15 H15 121.4 . . ?
C16 C15 H15 121.4 . . ?
N11 C16 C15 121.6(3) . . ?
N11 C16 C17 116.7(3) . . ?
C15 C16 C17 121.6(3) . . ?
O171 C17 O172 126.5(3) . . ?
O171 C17 C16 117.1(3) . . ?
O172 C17 C16 116.3(3) . . ?
C17 O171 Gd1 125.6(2) . . ?
C17 O172 Gd1 149.9(2) . 6 ?
O182 C18 O181 127.1(3) . . ?
O182 C18 C14 115.8(3) . . ?
O181 C18 C14 117.0(3) . . ?
C18 O181 Gd1 125.8(2) . 3_655 ?
C18 O182 Gd1 149.5(3) . 2_655 ?
N22 O21 Gd1 94.8(2) . . ?
O24 N22 O21 122.5(4) . . ?
O24 N22 O23 122.0(4) . . ?
O21 N22 O23 115.5(3) . . ?
O24 N22 Gd1 177.8(3) . . ?
O21 N22 Gd1 59.7(2) . . ?
O23 N22 Gd1 55.82(18) . . ?
N22 O23 Gd1 98.2(2) . . ?
Gd1 O1W H11W 115.7 . . ?
Gd1 O1W H12W 112.5 . . ?
H11W O1W H12W 103.6 . . ?
H21W O2W H22W 96.1 . . ?

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 O2W 0.86 1.90 2.748(4) 169.9 .
O1W H12W O2W 0.86 1.90 2.751(4) 171.5 3
O2W H21W O21 0.90 2.07 2.913(4) 156.9 6
O2W H22W O171 0.94 2.23 3.033(5) 142.0 6_554
O2W H22W O181 0.94 2.23 3.033(5) 142.3 2_654

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        73.12
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.073

# start Validation Reply Form
_vrf_PLAT113_2-Gd                
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space group. P63mc Check 
RESPONSE: 2-Gd presents high pseudo-symmetry, but the inclusion of the additional 
symmetry elements (P63mc) gives rise to extremely elongated anisotropic displacement 
parameters (ADP) indicating that these symmetry elements are not eventually present 
in the crystal structure. 
;
# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties'
