#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:41:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180049 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/43/7034314.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_7034314
loop_
_publ_author_name
'Cepeda, Javier'
'Pérez-Yáñez, Sonia'
'Beobide, Garikoitz'
'Castillo, Oscar'
'García, José Ángel'
'Lanchas, Mónica'
'Luque, Antonio'
_publ_section_title
;
 Enhancing luminescence properties of
 lanthanide(iii)/pyrimidine-4,6-dicarboxylato system by solvent-free
 approach.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6972
_journal_page_last               6986
_journal_paper_doi               10.1039/c4dt03797a
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_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_name_systematic
Poly[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':k2O,O'':kO''')europium(III)]
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_audit_update_record
;
2015-02-06 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.127(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5841(2)
_cell_length_b                   12.0772(2)
_cell_length_c                   9.4047(2)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.14
_cell_measurement_theta_min      5.99
_cell_volume                     967.47(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       ω
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7007
_diffrn_reflns_theta_full        73.14
_diffrn_reflns_theta_max         73.14
_diffrn_reflns_theta_min         5.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    46.924
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.063
_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    2.733
_exptl_crystal_density_meas      2.74(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             752
_exptl_crystal_preparation       'Magnetic properties, Luminescent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0256P)²+0.2786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                1841
_reflns_number_total             1922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03797a2.cif
_cod_data_source_block           1-Eu
_cod_depositor_comments
'Adding full bibliography for 7034314--7034317.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7034314
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'
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
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 .
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
