#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/63/2016361.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_2016361
loop_
_publ_author_name
'Wang, Jingen'
'Huang, Xihe'
'Huang, Changcang'
'Song, Haiyan'
'Yang, Duoping'
_publ_section_title
;
 A new three-dimensional neutral framework of lanthanum oxalate:
 [La₂(C₂O₄)₃(DMF)(H₂O)₃]ₙ
;
_journal_coeditor_code           SQ3099
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m583
_journal_page_last               m585
_journal_paper_doi               10.1107/S0108270107053292
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[La2 (C2 O4)3 (C3 H7 N O) (H2 O)3]'
_chemical_formula_moiety         'C9 H13 La2 N O16'
_chemical_formula_sum            'C9 H13 La2 N O16'
_chemical_formula_weight         669.02
_chemical_name_systematic
;
poly[triaquabis(dimethylformamide)di-μ₃-oxalato-μ₂-oxalato-\
dilanthanum(III)]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.392(2)
_cell_length_b                   10.224(2)
_cell_length_c                   8.7073(17)
_cell_measurement_reflns_used    7311
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.18
_cell_volume                     872.4(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1993)'
_computing_publication_material  'SHELXL97-2 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8351
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.18
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.918
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0261
_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)+(0.0157P)²+1.7609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                1779
_reflns_number_total             2011
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3099.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2016361
_cod_database_fobs_code          2016361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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
La La1 0.0000 0.43195(3) 0.7500 0.01358(9) Uani d S 1
La La2 0.5000 0.23575(3) 0.7500 0.01326(9) Uani d S 1
O O2 0.0753(2) 0.4019(3) 0.4929(3) 0.0176(5) Uani d . 1
O O3 0.2023(3) 0.4179(3) 0.2753(3) 0.0220(6) Uani d . 1
O O4 0.2542(3) 0.3054(3) 0.6688(3) 0.0211(6) Uani d . 1
O O5 0.3917(3) 0.3333(3) 0.4536(3) 0.0246(6) Uani d . 1
O O6 0.6121(3) 0.1322(3) 0.5644(3) 0.0219(6) Uani d . 1
O O7 0.6213(3) -0.0386(3) 0.4094(3) 0.0276(6) Uani d . 1
C C1 0.2714(4) 0.3709(3) 0.4111(4) 0.0171(7) Uani d . 1
C C2 0.1953(4) 0.3574(3) 0.5353(4) 0.0151(7) Uani d . 1
C C3 0.5676(4) 0.0273(4) 0.4920(4) 0.0195(7) Uani d . 1
O O1 0.0000 0.1954(4) 0.7500 0.0492(13) Uani d S 1
C C4 0.0542(9) 0.0987(9) 0.7277(12) 0.034(2) Uani d P 0.50
H H4A 0.1331 0.1051 0.6942 0.041 Uiso d PR 0.50
N N1 0.0000 -0.0212(5) 0.7500 0.0544(19) Uani d SD 1
C C5 -0.1175(9) -0.0462(12) 0.7838(14) 0.050 Uiso d PD 0.50
H H5D -0.1638 0.0310 0.8003 0.060 Uiso d PR 0.50
H H5E -0.1775 -0.0962 0.6955 0.060 Uiso d PR 0.50
H H5F -0.0909 -0.0981 0.8812 0.060 Uiso d PR 0.50
C C6 0.0886(11) -0.1238(10) 0.7164(13) 0.050 Uiso d PD 0.50
H H6A 0.0513 -0.2082 0.7256 0.060 Uiso d PR 0.50
H H6B 0.0932 -0.1134 0.6088 0.060 Uiso d PR 0.50
H H6C 0.1786 -0.1167 0.7949 0.060 Uiso d PR 0.50
O OW1 0.2120(3) 0.3442(4) 0.9791(3) 0.0350(8) Uani d D 1
H H1W1 0.225(6) 0.358(5) 1.076(2) 0.052 Uiso d D 1
H H2W1 0.251(6) 0.276(3) 0.973(6) 0.052 Uiso d D 1
O OW2 0.5000 0.4956(4) 0.7500 0.0317(9) Uani d SD 1
H H1W2 0.531(5) 0.544(3) 0.695(5) 0.048 Uiso d 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
O1 La1 O3 . 4_566 126.96(7) y
O1 La1 O3 . 3_566 126.96(7) ?
O3 La1 O3 4_566 3_566 106.07(13) ?
O1 La1 OW1 . 2_556 69.74(8) ?
O3 La1 OW1 4_566 2_556 137.69(9) ?
O3 La1 OW1 3_566 2_556 71.14(11) ?
O1 La1 OW1 . . 69.74(8) ?
O3 La1 OW1 4_566 . 71.14(11) y
O3 La1 OW1 3_566 . 137.69(9) ?
OW1 La1 OW1 2_556 . 139.49(17) y
O1 La1 O2 . 4_566 130.39(6) ?
O3 La1 O2 4_566 4_566 61.59(8) ?
O3 La1 O2 3_566 4_566 72.33(8) ?
OW1 La1 O2 2_556 4_566 142.65(10) ?
OW1 La1 O2 . 4_566 69.75(9) ?
O1 La1 O2 . 3_566 130.39(6) y
O3 La1 O2 4_566 3_566 72.33(8) ?
O3 La1 O2 3_566 3_566 61.59(8) y
OW1 La1 O2 2_556 3_566 69.75(9) ?
OW1 La1 O2 . 3_566 142.65(10) ?
O2 La1 O2 4_566 3_566 99.21(11) ?
O1 La1 O2 . . 83.28(6) y
O3 La1 O2 4_566 . 70.93(8) y
O3 La1 O2 3_566 . 117.87(8) ?
OW1 La1 O2 2_556 . 73.80(9) ?
OW1 La1 O2 . . 101.42(9) y
O2 La1 O2 4_566 . 132.11(8) y
O2 La1 O2 3_566 . 58.74(10) ?
O1 La1 O2 . 2_556 83.28(6) ?
O3 La1 O2 4_566 2_556 117.87(8) ?
O3 La1 O2 3_566 2_556 70.93(8) ?
OW1 La1 O2 2_556 2_556 101.42(9) ?
OW1 La1 O2 . 2_556 73.80(9) ?
O2 La1 O2 4_566 2_556 58.74(10) ?
O2 La1 O2 3_566 2_556 132.11(8) ?
O2 La1 O2 . 2_556 166.57(12) ?
O4 La2 O4 2_656 . 147.13(13) ?
O4 La2 O6 2_656 . 69.89(8) ?
O4 La2 O6 . . 125.57(8) ?
O4 La2 O6 2_656 2_656 125.57(8) ?
O4 La2 O6 . 2_656 69.89(8) ?
O6 La2 O6 . 2_656 130.28(12) ?
O4 La2 O7 2_656 3_656 130.78(9) ?
O4 La2 O7 . 3_656 78.30(9) ?
O6 La2 O7 . 3_656 64.28(9) y
O6 La2 O7 2_656 3_656 76.39(9) ?
O4 La2 O7 2_656 4_556 78.30(9) ?
O4 La2 O7 . 4_556 130.78(9) ?
O6 La2 O7 . 4_556 76.39(9) y
O6 La2 O7 2_656 4_556 64.28(9) ?
O7 La2 O7 3_656 4_556 74.54(14) ?
O4 La2 O5 2_656 2_656 63.66(8) ?
O4 La2 O5 . 2_656 103.31(9) y
O6 La2 O5 . 2_656 130.36(8) ?
O6 La2 O5 2_656 2_656 70.71(9) ?
O7 La2 O5 3_656 2_656 143.88(9) ?
O7 La2 O5 4_556 2_656 78.03(10) ?
O4 La2 O5 2_656 . 103.31(9) ?
O4 La2 O5 . . 63.66(8) y
O6 La2 O5 . . 70.71(9) ?
O6 La2 O5 2_656 . 130.36(8) ?
O7 La2 O5 3_656 . 78.03(10) ?
O7 La2 O5 4_556 . 143.88(9) ?
O5 La2 O5 2_656 . 135.67(14) ?
O4 La2 OW2 2_656 . 73.57(7) ?
O4 La2 OW2 . . 73.57(7) y
O6 La2 OW2 . . 114.86(6) y
O6 La2 OW2 2_656 . 114.86(6) ?
O7 La2 OW2 3_656 . 142.73(7) ?
O7 La2 OW2 4_556 . 142.73(7) ?
O5 La2 OW2 2_656 . 67.83(7) ?
O5 La2 OW2 . . 67.83(7) y
C2 O2 La1 . 3_566 118.1(2) ?
C2 O2 La1 . . 109.8(2) ?
La1 O2 La1 3_566 . 121.26(10) ?
C1 O3 La1 . 3_566 120.5(2) ?
C2 O4 La2 . . 121.6(2) ?
C1 O5 La2 . . 117.9(2) ?
C3 O6 La2 . . 120.8(2) ?
C3 O7 La2 . 3_656 120.7(2) ?
O5 C1 O3 . . 127.0(3) ?
O5 C1 C2 . . 117.6(3) ?
O3 C1 C2 . . 115.3(3) ?
O4 C2 O2 . . 124.2(3) ?
O4 C2 C1 . . 119.1(3) ?
O2 C2 C1 . . 116.7(3) ?
O7 C3 O6 . . 126.4(4) ?
O7 C3 C3 . 3_656 116.6(4) ?
O6 C3 C3 . 3_656 117.0(4) ?
C4 O1 C4 . 2_556 67.0(10) ?
C4 O1 La1 . . 146.5(5) ?
C4 O1 La1 2_556 . 146.5(5) ?
O1 C4 C4 . 2_556 56.5(5) ?
O1 C4 N1 . . 118.4(8) ?
C4 C4 N1 2_556 . 61.9(4) ?
O1 C4 C5 . 2_556 170.8(9) ?
C4 C4 C5 2_556 2_556 114.9(5) ?
N1 C4 C5 . 2_556 53.1(5) ?
O1 C4 H4A . . 119.6 ?
C4 C4 H4A 2_556 . 176.1 ?
N1 C4 H4A . . 121.9 ?
C5 C4 H4A 2_556 . 69.0 ?
C5 N1 C5 2_556 . 158.5(12) ?
C5 N1 C4 2_556 . 72.8(7) ?
C5 N1 C4 . . 128.7(7) ?
C5 N1 C4 2_556 2_556 128.7(7) ?
C5 N1 C4 . 2_556 72.8(6) ?
C4 N1 C4 . 2_556 56.1(8) ?
C5 N1 C6 2_556 . 34.2(6) ?
C5 N1 C6 . . 124.3(9) ?
C4 N1 C6 . . 106.8(6) ?
C4 N1 C6 2_556 . 162.9(7) ?
C5 N1 C6 2_556 2_556 124.3(9) ?
C5 N1 C6 . 2_556 34.2(6) ?
C4 N1 C6 . 2_556 162.9(7) ?
C4 N1 C6 2_556 2_556 106.8(6) ?
C6 N1 C6 . 2_556 90.3(10) ?
C6 C5 N1 2_556 . 80.4(9) ?
C6 C5 C4 2_556 2_556 134.1(11) ?
N1 C5 C4 . 2_556 54.1(5) ?
C6 C5 H5D 2_556 . 164.7 ?
N1 C5 H5D . . 113.9 ?
C4 C5 H5D 2_556 . 59.7 ?
C6 C5 H5E 2_556 . 68.7 ?
N1 C5 H5E . . 108.4 ?
C4 C5 H5E 2_556 . 126.8 ?
H5D C5 H5E . . 109.5 ?
C6 C5 H5F 2_556 . 59.2 ?
N1 C5 H5F . . 106.1 ?
C4 C5 H5F 2_556 . 123.4 ?
H5D C5 H5F . . 109.5 ?
H5E C5 H5F . . 109.5 ?
C5 C6 N1 2_556 . 65.4(7) ?
C5 C6 H6A 2_556 . 173.4 ?
N1 C6 H6A . . 108.9 ?
C5 C6 H6B 2_556 . 76.2 ?
N1 C6 H6B . . 110.4 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C 2_556 . 70.7 ?
N1 C6 H6C . . 109.1 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
La1 OW1 H1W1 . . 123(4) ?
La1 OW1 H2W1 . . 124(4) ?
H1W1 OW1 H2W1 . . 107(4) ?
La2 OW2 H1W2 . . 127(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 O1 . 2.418(5) y
La1 O3 4_566 2.553(3) y
La1 O3 3_566 2.553(3) n
La1 OW1 2_556 2.591(3) n
La1 OW1 . 2.591(3) y
La1 O2 4_566 2.621(2) y
La1 O2 3_566 2.621(2) n
La1 O2 . 2.624(2) y
La1 O2 2_556 2.624(2) n
La2 O4 2_656 2.516(3) n
La2 O4 . 2.516(3) y
La2 O6 . 2.518(3) y
La2 O6 2_656 2.518(3) n
La2 O7 3_656 2.532(3) y
La2 O7 4_556 2.532(3) n
La2 O5 2_656 2.644(3) n
La2 O5 . 2.644(3) y
La2 OW2 . 2.657(4) y
O2 C2 . 1.262(4) ?
O2 La1 3_566 2.621(2) ?
O3 C1 . 1.257(4) ?
O3 La1 3_566 2.553(3) ?
O4 C2 . 1.239(4) ?
O5 C1 . 1.242(4) ?
O6 C3 . 1.252(5) ?
O7 C3 . 1.246(5) ?
O7 La2 3_656 2.532(3) ?
C1 C2 . 1.544(5) ?
C3 C3 3_656 1.562(7) ?
O1 C4 . 1.185(9) ?
O1 C4 2_556 1.185(9) ?
C4 C4 2_556 1.308(19) ?
C4 N1 . 1.389(10) ?
C4 C5 2_556 1.638(14) ?
C4 H4A . 0.9600 ?
N1 C5 2_556 1.372(8) ?
N1 C5 . 1.372(8) ?
N1 C4 2_556 1.389(10) ?
N1 C6 . 1.488(8) ?
N1 C6 2_556 1.488(8) ?
C5 C6 2_556 0.848(14) ?
C5 C4 2_556 1.638(14) ?
C5 H5D . 0.9601 ?
C5 H5E . 0.9600 ?
C5 H5F . 0.9601 ?
C6 C5 2_556 0.848(14) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9601 ?
C6 H6C . 0.9600 ?
OW1 H1W1 . 0.818(10) ?
OW1 H2W1 . 0.818(10) ?
OW2 H1W2 . 0.818(10) ?
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
OW1 H1W1 O3 1_556 0.818(10) 1.931(18) 2.721(4) 162(5)
OW1 H2W1 O6 2_656 0.818(10) 2.15(2) 2.940(4) 164(6)
OW2 H1W2 O5 3_666 0.818(10) 2.148(11) 2.966(4) 178(5)
