#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/24/2222437.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2222437
loop_
_publ_author_name
'Xia, Jun'
'Wei, Jun-Fu'
_publ_section_title
Poly[diaqua(μ₄-3,5-dicarboxylatopyrazol-1-ido-κ⁶N¹,O⁵:N²,O³:O^3'^:O⁵,O^5'^)lanthanum(III)]
_journal_coeditor_code           RZ2328
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m732
_journal_paper_doi               10.1107/S1600536809020479
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[La (C5 H N2 O4) (H2 O)2]'
_chemical_formula_moiety         'C5 H5 La N2 O6'
_chemical_formula_sum            'C5 H5 La N2 O6'
_chemical_formula_weight         328.02
_chemical_name_systematic
;
Poly[diaqua(μ₄-3,5-dicarboxylatopyrazol-1-ido-
κ⁶N¹,O⁵:N²,O³:O^3'^:
O⁵,O^5'^)lanthanum(III)]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5712(8)
_cell_length_b                   8.4350(6)
_cell_length_c                   16.0070(10)
_cell_measurement_reflns_used    3962
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.54
_cell_volume                     1697.35(19)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8554
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    5.041
_exptl_absorpt_correction_T_max  0.365
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.502
_refine_ls_extinction_coef       0.00271(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0162
_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)+(0.0185P)²+2.3502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0406
_reflns_number_gt                1316
_reflns_number_total             1496
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rz2328.cif
_cod_data_source_block           I
_cod_database_code               2222437
_cod_database_fobs_code          2222437
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_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
La La1 0.968426(12) 0.009678(17) 0.662201(9) 0.01104(9) Uani d . 1 . .
O O1 0.80247(17) 0.1816(2) 0.67873(12) 0.0212(5) Uani d . 1 . .
O O2 0.68279(17) 0.3455(3) 0.62560(14) 0.0274(5) Uani d . 1 . .
O O3 0.9060(2) 0.5049(2) 0.31256(13) 0.0222(5) Uani d . 1 . .
O O4 0.98606(16) 0.2761(2) 0.29004(12) 0.0170(4) Uani d . 1 . .
O O5 1.0936(2) 0.2221(3) 0.60343(15) 0.0325(6) Uani d . 1 . .
H H5A 1.0942 0.1442 0.6371 0.049 Uiso d R 1 . .
H H5B 1.0973 0.3066 0.6322 0.049 Uiso d R 1 . .
O O6 1.15184(19) -0.0151(2) 0.73037(16) 0.0338(6) Uani d . 1 . .
H H6A 1.1780 -0.1047 0.7434 0.051 Uiso d R 1 . .
H H6B 1.1851 0.0664 0.7475 0.051 Uiso d R 1 . .
N N1 0.89277(19) 0.1436(3) 0.52362(14) 0.0162(5) Uani d . 1 . .
N N2 0.93750(19) 0.1715(3) 0.44839(14) 0.0165(5) Uani d . 1 . .
C C1 0.7644(2) 0.2632(3) 0.61947(19) 0.0153(6) Uani d . 1 . .
C C2 0.8238(2) 0.2624(3) 0.53938(17) 0.0155(6) Uani d . 1 . .
C C3 0.8237(2) 0.3719(3) 0.47460(18) 0.0190(7) Uani d . 1 . .
H H3 0.7841 0.4646 0.4698 0.023 Uiso calc R 1 . .
C C4 0.8967(2) 0.3099(3) 0.41903(17) 0.0160(6) Uani d . 1 . .
C C5 0.9322(2) 0.3675(3) 0.33671(17) 0.0154(6) Uani d . 1 . .
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'
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
O2 La1 O3 8_755 7_566 87.64(7) ?
O2 La1 O1 8_755 . 73.08(8) ?
O3 La1 O1 7_566 . 71.11(7) ?
O2 La1 O6 8_755 . 139.71(7) ?
O3 La1 O6 7_566 . 82.55(8) ?
O1 La1 O6 . . 137.56(7) ?
O2 La1 O5 8_755 . 142.39(7) ?
O3 La1 O5 7_566 . 124.93(7) ?
O1 La1 O5 . . 98.20(7) ?
O6 La1 O5 . . 70.16(8) ?
O2 La1 O4 8_755 5_756 73.32(7) ?
O3 La1 O4 7_566 5_756 75.12(6) ?
O1 La1 O4 . 5_756 132.65(6) ?
O6 La1 O4 . 5_756 66.39(6) ?
O5 La1 O4 . 5_756 128.50(7) ?
O2 La1 N2 8_755 5_756 81.81(8) ?
O3 La1 N2 7_566 5_756 138.85(7) ?
O1 La1 N2 . 5_756 140.31(7) ?
O6 La1 N2 . 5_756 80.43(8) ?
O5 La1 N2 . 5_756 83.25(7) ?
O4 La1 N2 5_756 5_756 63.74(7) ?
O2 La1 N1 8_755 . 76.18(7) ?
O3 La1 N1 7_566 . 134.47(7) ?
O1 La1 N1 . . 63.52(7) ?
O6 La1 N1 . . 135.32(8) ?
O5 La1 N1 . . 67.51(8) ?
O4 La1 N1 5_756 . 135.91(6) ?
N2 La1 N1 5_756 . 81.13(7) ?
O2 La1 O4 8_755 7_566 128.39(7) ?
O3 La1 O4 7_566 7_566 49.28(6) ?
O1 La1 O4 . 7_566 67.31(6) ?
O6 La1 O4 . 7_566 70.28(7) ?
O5 La1 O4 . 7_566 76.32(6) ?
O4 La1 O4 5_756 7_566 112.04(2) ?
N2 La1 O4 5_756 7_566 148.53(7) ?
N1 La1 O4 . 7_566 111.79(6) ?
O2 La1 C5 8_755 7_566 107.57(8) ?
O3 La1 C5 7_566 7_566 24.47(7) ?
O1 La1 C5 . 7_566 65.50(7) ?
O6 La1 C5 . 7_566 76.66(8) ?
O5 La1 C5 . 7_566 101.11(7) ?
O4 La1 C5 5_756 7_566 94.58(7) ?
N2 La1 C5 5_756 7_566 153.48(8) ?
N1 La1 C5 . 7_566 124.88(7) ?
O4 La1 C5 7_566 7_566 24.90(7) ?
O2 La1 H5A 8_755 . 154.3 ?
O3 La1 H5A 7_566 . 117.8 ?
O1 La1 H5A . . 110.3 ?
O6 La1 H5A . . 54.3 ?
O5 La1 H5A . . 15.9 ?
O4 La1 H5A 5_756 . 114.5 ?
N2 La1 H5A 5_756 . 80.6 ?
N1 La1 H5A . . 82.7 ?
O4 La1 H5A 7_566 . 73.1 ?
C5 La1 H5A 7_566 . 96.4 ?
C1 O1 La1 . . 122.68(18) ?
C1 O2 La1 . 8_765 170.3(2) ?
C5 O3 La1 . 7_565 99.48(17) ?
C5 O4 La1 . 5_756 120.58(17) ?
C5 O4 La1 . 7_565 89.78(16) ?
La1 O4 La1 5_756 7_565 148.37(8) ?
La1 O5 H5B . . 114.9 ?
H5A O5 H5B . . 107.7 ?
La1 O6 H6A . . 121.7 ?
La1 O6 H6B . . 120.9 ?
H6A O6 H6B . . 116.7 ?
C2 N1 N2 . . 107.8(2) ?
C2 N1 La1 . . 112.86(17) ?
N2 N1 La1 . . 131.91(17) ?
N1 N2 C4 . . 107.5(2) ?
N1 N2 La1 . 5_756 133.56(17) ?
C4 N2 La1 . 5_756 115.97(17) ?
O2 C1 O1 . . 123.8(3) ?
O2 C1 C2 . . 119.1(3) ?
O1 C1 C2 . . 117.0(2) ?
N1 C2 C3 . . 110.8(3) ?
N1 C2 C1 . . 119.2(2) ?
C3 C2 C1 . . 129.9(3) ?
C4 C3 C2 . . 103.2(2) ?
C4 C3 H3 . . 128.4 ?
C2 C3 H3 . . 128.4 ?
N2 C4 C3 . . 110.7(2) ?
N2 C4 C5 . . 118.5(2) ?
C3 C4 C5 . . 130.8(3) ?
O3 C5 O4 . . 121.0(3) ?
O3 C5 C4 . . 119.7(3) ?
O4 C5 C4 . . 119.2(2) ?
O3 C5 La1 . 7_565 56.04(14) ?
O4 C5 La1 . 7_565 65.32(14) ?
C4 C5 La1 . 7_565 171.1(2) ?
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 O2 8_755 2.424(2) ?
La1 O3 7_566 2.535(2) ?
La1 O1 . 2.554(2) ?
La1 O6 . 2.559(2) ?
La1 O5 . 2.564(2) ?
La1 O4 5_756 2.5929(19) ?
La1 N2 5_756 2.620(2) ?
La1 N1 . 2.665(2) ?
La1 O4 7_566 2.7388(19) ?
La1 C5 7_566 3.014(3) ?
La1 H5A . 1.9874 ?
O1 C1 . 1.266(4) ?
O2 C1 . 1.242(3) ?
O2 La1 8_765 2.424(2) ?
O3 C5 . 1.266(3) ?
O3 La1 7_565 2.535(2) ?
O4 C5 . 1.269(3) ?
O4 La1 5_756 2.5929(19) ?
O4 La1 7_565 2.7388(19) ?
O5 H5A . 0.8500 ?
O5 H5B . 0.8500 ?
O6 H6A . 0.8500 ?
O6 H6B . 0.8499 ?
N1 C2 . 1.349(4) ?
N1 N2 . 1.350(3) ?
N2 C4 . 1.360(4) ?
N2 La1 5_756 2.620(2) ?
C1 C2 . 1.483(4) ?
C2 C3 . 1.389(4) ?
C3 C4 . 1.380(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.474(4) ?
C5 La1 7_565 3.014(3) ?
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
O5 H5A O6 . 0.85 2.14 2.944(3) 159
O5 H5B O3 5_766 0.85 1.82 2.667(3) 174
O6 H6A O1 3_746 0.85 2.20 2.999(3) 155
O6 H6B O1 6_657 0.85 2.12 2.908(3) 153
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
O2 La1 O1 C1 8_755 . . . -89.3(2) ?
O3 La1 O1 C1 7_566 . . . 177.3(2) ?
O6 La1 O1 C1 . . . . 122.6(2) ?
O5 La1 O1 C1 . . . . 53.1(2) ?
O4 La1 O1 C1 5_756 . . . -135.8(2) ?
N2 La1 O1 C1 5_756 . . . -36.2(3) ?
N1 La1 O1 C1 . . . . -6.6(2) ?
O4 La1 O1 C1 7_566 . . . 124.5(2) ?
C5 La1 O1 C1 7_566 . . . 151.7(2) ?
O2 La1 N1 C2 8_755 . . . 93.7(2) ?
O3 La1 N1 C2 7_566 . . . 21.3(2) ?
O1 La1 N1 C2 . . . . 15.99(18) ?
O6 La1 N1 C2 . . . . -115.99(19) ?
O5 La1 N1 C2 . . . . -96.26(19) ?
O4 La1 N1 C2 5_756 . . . 141.00(17) ?
N2 La1 N1 C2 5_756 . . . 177.4(2) ?
O4 La1 N1 C2 7_566 . . . -32.5(2) ?
C5 La1 N1 C2 7_566 . . . -8.2(2) ?
O2 La1 N1 N2 8_755 . . . -120.8(2) ?
O3 La1 N1 N2 7_566 . . . 166.70(19) ?
O1 La1 N1 N2 . . . . 161.4(2) ?
O6 La1 N1 N2 . . . . 29.5(3) ?
O5 La1 N1 N2 . . . . 49.2(2) ?
O4 La1 N1 N2 5_756 . . . -73.6(2) ?
N2 La1 N1 N2 5_756 . . . -37.1(2) ?
O4 La1 N1 N2 7_566 . . . 113.0(2) ?
C5 La1 N1 N2 7_566 . . . 137.2(2) ?
C2 N1 N2 C4 . . . . 1.1(3) ?
La1 N1 N2 C4 . . . . -145.6(2) ?
C2 N1 N2 La1 . . . 5_756 -157.9(2) ?
La1 N1 N2 La1 . . . 5_756 55.4(3) ?
La1 O1 C1 O2 . . . . 178.7(2) ?
La1 O1 C1 C2 . . . . -3.1(3) ?
N2 N1 C2 C3 . . . . -0.9(3) ?
La1 N1 C2 C3 . . . . 152.7(2) ?
N2 N1 C2 C1 . . . . -178.8(2) ?
La1 N1 C2 C1 . . . . -25.2(3) ?
O2 C1 C2 N1 . . . . -161.5(3) ?
O1 C1 C2 N1 . . . . 20.3(4) ?
O2 C1 C2 C3 . . . . 21.1(5) ?
O1 C1 C2 C3 . . . . -157.2(3) ?
N1 C2 C3 C4 . . . . 0.4(3) ?
C1 C2 C3 C4 . . . . 178.0(3) ?
N1 N2 C4 C3 . . . . -0.9(3) ?
La1 N2 C4 C3 5_756 . . . 162.30(19) ?
N1 N2 C4 C5 . . . . -179.6(2) ?
La1 N2 C4 C5 5_756 . . . -16.4(3) ?
C2 C3 C4 N2 . . . . 0.3(3) ?
C2 C3 C4 C5 . . . . 178.8(3) ?
La1 O3 C5 O4 7_565 . . . 7.1(3) ?
La1 O3 C5 C4 7_565 . . . -170.7(2) ?
La1 O4 C5 O3 5_756 . . . -177.2(2) ?
La1 O4 C5 O3 7_565 . . . -6.5(3) ?
La1 O4 C5 C4 5_756 . . . 0.7(3) ?
La1 O4 C5 C4 7_565 . . . 171.4(2) ?
La1 O4 C5 La1 5_756 . . 7_565 -170.65(16) ?
N2 C4 C5 O3 . . . . -171.1(3) ?
C3 C4 C5 O3 . . . . 10.5(5) ?
N2 C4 C5 O4 . . . . 11.0(4) ?
C3 C4 C5 O4 . . . . -167.4(3) ?
