#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:41:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180049 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/43/7034315.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_7034315
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 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_name_systematic
Poly[aqua(nitrato-k2O,O')(mu4-pyrimidine-4,6-dicarboxylato-k2N,O:k2N',O':k2O,O'':kO''')lanthanum(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                 96.640(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7220(2)
_cell_length_b                   12.2820(2)
_cell_length_c                   9.5780(2)
_cell_measurement_reflns_used    7144
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.07
_cell_measurement_theta_min      5.88
_cell_volume                     1019.15(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7144
_diffrn_reflns_theta_full        73.07
_diffrn_reflns_theta_max         73.07
_diffrn_reflns_theta_min         5.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    32.887
_exptl_absorpt_correction_T_max  0.396
_exptl_absorpt_correction_T_min  0.078
_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    2.509
_exptl_crystal_density_meas      2.51(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0276P)²+0.2136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                1964
_reflns_number_total             2015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03797a2.cif
_cod_data_source_block           1-La
_cod_depositor_comments
'Adding full bibliography for 7034314--7034317.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7034315
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
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 .
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'
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 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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
