##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
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#                                                                            #
#            Copyright International Union of Crystallography                #
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##############################################################################
                                             
data_global
_audit_creation_method     'SHELXL-97'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2005-10-27
_journal_date_accepted     2005-10-31
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2005
_journal_volume     61
_journal_issue     12
_journal_page_first     m2523
_journal_page_last     m2525
_journal_paper_category     EM
_journal_coeditor_code     NG6231
_publ_contact_author_name     'Prof. Shan Gao'
_publ_contact_author_address
;
Laboratory of Functional Materials
School of Chemistry and Materials Science
Heilongjiang University
Harbin 150080
People's Republic of China
;
_publ_contact_author_email     shangao67@yahoo.com
_publ_contact_author_fax     '(86)451 8660 8040'
_publ_contact_author_phone     '(86)451 8660 9148'
_publ_section_title
;\
Diaquatris(nitrato-κ²O,O')bis(4-pyridone-κO)\
lanthanum(III)
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Deng, Zhao-Peng' .
;
Laboratory of Functional Materials
School of Chemistry and Materials Science
Heilongjiang University
Harbin 150080
People's Republic of China
;
    'Gao, Shan' .
;
Laboratory of Functional Materials
School of Chemistry and Materials Science
Heilongjiang University
Harbin 150080
People's Republic of China
;
    'Huo, Li-Hua' .
;
Laboratory of Functional Materials
School of Chemistry and Materials Science
Heilongjiang University
Harbin 150080
People's Republic of China
;
    'Zhao, Hui' .
;
Laboratory of Functional Materials
School of Chemistry and Materials Science
Heilongjiang University
Harbin 150080
People's Republic of China
;
data_I
_chemical_name_systematic
;
Diaquatris(nitrato-κ²O,O')bis(4-pyridone-\kO)lanthanum(III)
;
_chemical_formula_moiety     'C10 H14 La N5 O13'
_chemical_formula_sum     'C10 H14 La N5 O13'
_chemical_formula_iupac     '[La (N O3)3 (C5 H5 N O)2 (H2 O)2]'
_chemical_formula_weight     551.17
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     11.051(2)
_cell_length_b     8.9055(18)
_cell_length_c     19.203(4)
_cell_angle_alpha     90.00
_cell_angle_beta     96.31(3)
_cell_angle_gamma     90.00
_cell_volume     1878.4(7)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     8926
_cell_measurement_theta_min     3.06
_cell_measurement_theta_max     27.46
_cell_measurement_temperature     295(2)
_exptl_crystal_description     Prism
_exptl_crystal_colour     Colorless
_exptl_crystal_size_max     0.36
_exptl_crystal_size_mid     0.25
_exptl_crystal_size_min     0.19
_exptl_crystal_density_diffrn     1.949
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1080
_exptl_absorpt_coefficient_mu     2.352
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_correction_T_min     0.494
_exptl_absorpt_correction_T_max     0.645
_exptl_special_details
;
;
_diffrn_ambient_temperature     295(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku R-AXIS RAPID'
_diffrn_measurement_method     'ω scan'
_diffrn_detector_area_resol_mean     10
_diffrn_reflns_number     8972
_diffrn_reflns_av_R_equivalents     0.0151
_diffrn_reflns_av_sigmaI/netI     0.0117
_diffrn_reflns_theta_min     3.06
_diffrn_reflns_theta_max     27.48
_diffrn_reflns_theta_full     27.48
_diffrn_measured_fraction_theta_max     0.998
_diffrn_measured_fraction_theta_full     0.998
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -24
_diffrn_reflns_limit_l_max     24
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_reflns_number_total     2150
_reflns_number_gt     2106
_reflns_threshold_expression     'I>2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0162
_refine_ls_R_factor_gt     0.0159
_refine_ls_wR_factor_gt     0.0398
_refine_ls_wR_factor_ref     0.0399
_refine_ls_goodness_of_fit_ref     1.242
_refine_ls_restrained_S_all     1.241
_refine_ls_number_reflns     2150
_refine_ls_number_parameters     139
_refine_ls_number_restraints     3
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0228P)²+0.6564P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.343
_refine_diff_density_min     -0.666
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'La' 'La' -0.2871 2.4523
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement     'RAPID-AUTO'
_computing_data_reduction     'CrystalStructure (Rigaku/MSC, 2002)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEPII (Johnson, 1976)'
_computing_publication_material     SHELXL97
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    La1 0.5000 0.298597(13) 0.7500 0.02360(5) Uani d S 1 . . La
    O1W 0.26861(13) 0.31347(16) 0.73382(12) 0.0540(5) Uani d D 1 . . O
    O1 0.48238(15) 0.3808(2) 0.63123(7) 0.0539(4) Uani d . 1 . . O
    O2 0.59694(11) 0.57592(14) 0.74747(8) 0.0424(3) Uani d . 1 . . O
    O3 0.5000 0.7841(2) 0.7500 0.0931(14) Uani d S 1 . . O
    O4 0.40621(13) 0.07622(16) 0.66863(8) 0.0460(3) Uani d . 1 . . O
    O5 0.60148(13) 0.07647(18) 0.68054(8) 0.0505(4) Uani d . 1 . . O
    O6 0.5027(2) -0.0645(3) 0.60190(12) 0.0901(8) Uani d . 1 . . O
    N1 0.27223(18) 0.4560(2) 0.44933(10) 0.0533(5) Uani d . 1 . . N
    N2 0.5000 0.6495(2) 0.7500 0.0383(5) Uani d S 1 . . N
    N3 0.50433(18) 0.0269(2) 0.64929(10) 0.0499(4) Uani d . 1 . . N
    C1 0.2532(2) 0.5356(3) 0.50592(14) 0.0573(6) Uani d . 1 . . C
    C2 0.3222(2) 0.5141(3) 0.56839(12) 0.0493(5) Uani d . 1 . . C
    C3 0.41439(17) 0.4043(2) 0.57403(9) 0.0381(4) Uani d . 1 . . C
    C4 0.4282(2) 0.3218(2) 0.51276(12) 0.0447(4) Uani d . 1 . . C
    C5 0.3573(2) 0.3496(3) 0.45223(11) 0.0504(5) Uani d . 1 . . C
    H1W1 0.227(2) 0.3943(18) 0.7288(17) 0.081 Uiso d D 1 . . H
    H1W2 0.222(2) 0.241(2) 0.7420(18) 0.081 Uiso d D 1 . . H
    H1 0.1916 0.6072 0.5027 0.069 Uiso calc R 1 . . H
    H2 0.3084 0.5717 0.6071 0.059 Uiso calc R 1 . . H
    H4 0.4871 0.2470 0.5140 0.054 Uiso calc R 1 . . H
    H5 0.3680 0.2941 0.4123 0.061 Uiso calc R 1 . . H
    H6 0.2288 0.4737 0.4102 0.064 Uiso calc R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    La1 0.01880(7) 0.02110(7) 0.03051(8) 0.000 0.00102(5) 0.000
    O1W 0.0204(6) 0.0337(7) 0.1075(15) -0.0007(5) 0.0053(8) 0.0087(8)
    O1 0.0548(9) 0.0666(11) 0.0393(7) -0.0012(8) 0.0008(6) 0.0183(7)
    O2 0.0223(6) 0.0285(6) 0.0764(9) 0.0018(5) 0.0055(6) 0.0005(6)
    O3 0.0457(15) 0.0226(11) 0.214(5) 0.000 0.029(2) 0.000
    O4 0.0392(7) 0.0413(7) 0.0555(8) 0.0045(6) -0.0039(6) -0.0149(6)
    O5 0.0394(7) 0.0522(9) 0.0582(8) 0.0095(7) -0.0027(6) -0.0170(7)
    O6 0.0826(14) 0.0916(15) 0.0912(14) 0.0239(12) -0.0119(11) -0.0644(13)
    N1 0.0491(10) 0.0605(12) 0.0468(9) -0.0097(9) -0.0099(8) 0.0074(8)
    N2 0.0250(10) 0.0240(10) 0.0656(14) 0.000 0.0033(9) 0.000
    N3 0.0515(10) 0.0451(10) 0.0504(9) 0.0122(8) -0.0059(8) -0.0181(8)
    C1 0.0448(12) 0.0531(13) 0.0721(16) 0.0089(10) -0.0019(11) 0.0054(12)
    C2 0.0483(11) 0.0507(12) 0.0491(11) 0.0053(10) 0.0064(9) -0.0044(9)
    C3 0.0382(9) 0.0395(9) 0.0371(8) -0.0056(8) 0.0058(7) 0.0094(8)
    C4 0.0461(11) 0.0401(10) 0.0491(11) 0.0010(8) 0.0105(9) 0.0028(8)
    C5 0.0553(13) 0.0533(12) 0.0427(10) -0.0099(10) 0.0056(9) -0.0046(9)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    La1 O1W . 2.5452(15) yes
    La1 O1 . 2.3830(14) yes
    La1 O2 . 2.6946(14) yes
    La1 O4 . 2.6612(14) yes
    La1 O5 . 2.6978(15) yes
    O1 C3 . 1.278(2) yes
    C1 C2 . 1.362(3) yes
    C4 C5 . 1.351(3) yes
    La1 O1W 2_656 2.5452(15) no
    La1 O1 2_656 2.3830(14) no
    La1 O2 2_656 2.6946(14) no
    La1 O4 2_656 2.6612(14) no
    La1 O5 2_656 2.6978(15) no
    O1W H1W1 . 0.854(10) no
    O1W H1W2 . 0.847(10) no
    O2 N2 . 1.2612(17) no
    O3 N2 . 1.199(3) no
    O4 N3 . 1.263(2) no
    O5 N3 . 1.251(2) no
    O6 N3 . 1.219(2) no
    N1 C5 . 1.331(3) no
    N1 C1 . 1.333(3) no
    N1 H6 . 0.8600 no
    N2 O2 2_656 1.2612(17) no
    C1 H1 . 0.9300 no
    C2 C3 . 1.408(3) no
    C2 H2 . 0.9300 no
    C3 C4 . 1.409(3) no
    C4 H4 . 0.9300 no
    C5 H5 . 0.9300 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1W La1 O1W 2_656 . 174.03(7) yes
    O1W La1 O2 . . 110.25(4) yes
    O1W La1 O2 . 2_656 63.80(4) yes
    O1W La1 O4 . 2_656 115.57(5) yes
    O1W La1 O4 . . 69.26(5) yes
    O1W La1 O5 . . 116.39(5) yes
    O1W La1 O5 . 2_656 68.40(5) yes
    O1 La1 O1 2_656 . 144.20(9) yes
    O1 La1 O1W . . 83.79(7) yes
    O1 La1 O1W . 2_656 94.37(7) yes
    O1 La1 O2 . . 72.05(6) yes
    O1 La1 O2 . 2_656 75.21(6) yes
    O1 La1 O4 . 2_656 140.92(6) yes
    O1 La1 O4 . . 71.41(6) yes
    O1 La1 O5 . 2_656 134.74(6) yes
    O1 La1 O5 . . 75.34(6) yes
    O2 La1 O2 . 2_656 47.15(5) yes
    O2 La1 O5 . . 118.39(5) yes
    O2 La1 O5 . 2_656 150.30(5) yes
    O4 La1 O2 . 2_656 124.24(5) yes
    O4 La1 O2 . . 143.27(5) yes
    O4 La1 O4 . 2_656 83.82(7) yes
    O4 La1 O5 . . 47.18(5) yes
    O4 La1 O5 . 2_656 65.69(5) yes
    O5 La1 O5 . 2_656 85.69(8) yes
    La1 O1W H1W1 . . 125.4(18) no
    La1 O1W H1W2 . . 124.0(19) no
    O1W La1 O2 2_656 2_656 110.25(4) no
    O1W La1 O2 2_656 . 63.80(4) no
    O1W La1 O4 2_656 . 115.57(5) no
    O1W La1 O4 2_656 2_656 69.26(5) no
    O1W La1 O5 2_656 2_656 116.39(5) no
    O1W La1 O5 2_656 . 68.40(5) no
    O1 La1 O1W 2_656 2_656 83.79(7) no
    O1 La1 O1W 2_656 . 94.37(7) no
    O1 La1 O2 2_656 2_656 72.05(6) no
    O1 La1 O2 2_656 . 75.21(6) no
    O1 La1 O4 2_656 . 140.92(6) no
    O1 La1 O4 2_656 2_656 71.41(6) no
    O1 La1 O5 2_656 . 134.74(6) no
    O1 La1 O5 2_656 2_656 75.34(6) no
    O1 C3 C2 . . 122.13(19) no
    O1 C3 C4 . . 121.7(2) no
    O2 La1 O5 2_656 2_656 118.39(5) no
    O2 La1 O5 2_656 . 150.30(5) no
    O2 N2 O2 2_656 . 117.4(2) no
    O3 N2 O2 . . 121.30(10) no
    O3 N2 O2 . 2_656 121.30(10) no
    O4 La1 O2 2_656 . 124.24(5) no
    O4 La1 O2 2_656 2_656 143.27(5) no
    O4 La1 O5 2_656 2_656 47.18(5) no
    O4 La1 O5 2_656 . 65.69(5) no
    O5 N3 O4 . . 117.09(16) no
    O6 N3 O4 . . 120.58(19) no
    O6 N3 O5 . . 122.33(19) no
    N1 C1 C2 . . 121.3(2) no
    N1 C1 H1 . . 119.3 no
    N1 C5 C4 . . 120.4(2) no
    N1 C5 H5 . . 119.8 no
    N2 O2 La1 . . 97.73(11) no
    N3 O4 La1 . . 98.04(11) no
    N3 O5 La1 . . 96.57(11) no
    C1 C2 C3 . . 119.7(2) no
    C1 C2 H2 . . 120.1 no
    C1 N1 H6 . . 119.4 no
    C2 C1 H1 . . 119.3 no
    C2 C3 C4 . . 116.20(18) no
    C3 C2 H2 . . 120.1 no
    C3 C4 H4 . . 119.4 no
    C3 O1 La1 . . 148.35(14) no
    C4 C5 H5 . . 119.8 no
    C5 C4 C3 . . 121.1(2) no
    C5 C4 H4 . . 119.4 no
    C5 N1 C1 . . 121.2(2) no
    C5 N1 H6 . . 119.4 no
    H1W1 O1W H1W2 . . 109.3(16) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O1 La1 O1 C3 2_656 . . . -101.4(3) no
    O1W La1 O1 C3 2_656 . . . 173.2(3) no
    O1W La1 O1 C3 . . . . -12.5(3) no
    O4 La1 O1 C3 . . . . 57.7(3) no
    O4 La1 O1 C3 2_656 . . . 111.2(3) no
    O2 La1 O1 C3 . . . . -126.2(3) no
    O2 La1 O1 C3 2_656 . . . -77.0(3) no
    O5 La1 O1 C3 . . . . 106.9(3) no
    O5 La1 O1 C3 2_656 . . . 38.5(3) no
    O1 La1 O2 N2 2_656 . . . -79.06(9) no
    O1 La1 O2 N2 . . . . 86.24(9) no
    O1W La1 O2 N2 2_656 . . . -169.37(11) no
    O1W La1 O2 N2 . . . . 10.16(10) no
    O4 La1 O2 N2 . . . . 92.31(10) no
    O4 La1 O2 N2 2_656 . . . -133.71(8) no
    O2 La1 O2 N2 2_656 . . . 0.0 no
    O5 La1 O2 N2 . . . . 147.72(7) no
    O5 La1 O2 N2 2_656 . . . -71.49(12) no
    O1 La1 O4 N3 2_656 . . . -118.44(13) no
    O1 La1 O4 N3 . . . . 80.96(13) no
    O1W La1 O4 N3 2_656 . . . -4.92(14) no
    O1W La1 O4 N3 . . . . 171.27(14) no
    O4 La1 O4 N3 2_656 . . . -68.38(12) no
    O2 La1 O4 N3 . . . . 74.87(14) no
    O2 La1 O4 N3 2_656 . . . 137.26(12) no
    O5 La1 O4 N3 . . . . -6.04(12) no
    O5 La1 O4 N3 2_656 . . . -113.85(13) no
    O1 La1 O5 N3 2_656 . . . 130.94(13) no
    O1 La1 O5 N3 . . . . -71.99(14) no
    O1W La1 O5 N3 2_656 . . . -172.84(15) no
    O1W La1 O5 N3 . . . . 3.26(15) no
    O4 La1 O5 N3 . . . . 6.07(12) no
    O4 La1 O5 N3 2_656 . . . 110.99(14) no
    O2 La1 O5 N3 . . . . -131.76(13) no
    O2 La1 O5 N3 2_656 . . . -79.56(16) no
    O5 La1 O5 N3 2_656 . . . 66.54(13) no
    La1 O2 N2 O3 . . . . 180.0 no
    La1 O2 N2 O2 . . . 2_656 0.0 no
    La1 O5 N3 O6 . . . . 169.1(2) no
    La1 O5 N3 O4 . . . . -10.6(2) no
    La1 O4 N3 O6 . . . . -168.9(2) no
    La1 O4 N3 O5 . . . . 10.8(2) no
    C5 N1 C1 C2 . . . . 1.9(4) no
    N1 C1 C2 C3 . . . . -1.0(4) no
    La1 O1 C3 C2 . . . . 65.6(4) no
    La1 O1 C3 C4 . . . . -114.7(3) no
    C1 C2 C3 O1 . . . . 179.3(2) no
    C1 C2 C3 C4 . . . . -0.4(3) no
    O1 C3 C4 C5 . . . . -178.7(2) no
    C2 C3 C4 C5 . . . . 0.9(3) no
    C1 N1 C5 C4 . . . . -1.3(3) no
    C3 C4 C5 N1 . . . . -0.1(3) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O1W H1W1 O5 3_455 0.854(10) 2.265(14) 3.087(2) 161(3) yes
    O1W H1W2 O2 3_445 0.847(10) 2.032(12) 2.873(2) 171(3) yes
    O1W H1W2 O3 3_445 0.847(10) 2.51(3) 3.0296(16) 121(2) yes
    N1 H6 O4 7_556 0.86 2.05 2.849(2) 153 yes
