#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/26/2212650.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_2212650
loop_
_publ_author_name
'Bao-Xia Dong'
'Jun Peng'
_publ_section_title
;Poly[[tetraaqua-μ₂-oxalato-bis(μ₃-pyridine-3,4-dicarboxylato-κ⁴O,O':O'':O''')diyttrium(III)]
 trihydrate]
;
_journal_coeditor_code           NG2213
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m689
_journal_page_last               m691
_journal_paper_doi               10.1107/S1600536807005594
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Y2 (C7 H3 N O4)2 (C2 O4) (H2 O)4], 3H2 O'
_chemical_formula_moiety         'C16 H14 N2 O16 Y2, 3(H2 O)'
_chemical_formula_sum            'C16 H20 N2 O19 Y2'
_chemical_formula_weight         722.16
_chemical_name_systematic
;
Poly[[tetraaqua-μ₂-oxalato-bis(μ₃-pyridine-3,4-dicarboxylato-
κ⁴O,O':O'':O''')diyttrium(III)] trihydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.3400(5)
_cell_angle_beta                 99.9260(5)
_cell_angle_gamma                105.2930(5)
_cell_formula_units_Z            1
_cell_length_a                   5.9785(3)
_cell_length_b                   10.1376(5)
_cell_length_c                   11.1811(5)
_cell_measurement_reflns_used    2395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.35
_cell_volume                     612.47(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5250
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.809
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.853
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0353
_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)+(0.0556P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                2225
_reflns_number_total             2395
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2213.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2212650
_cod_database_fobs_code          2212650
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
N N1 0.8166(6) 0.3078(4) 0.4318(2) 0.0342(7) Uani d . 1
Y Y1 0.64874(4) 0.69151(3) 0.93921(2) 0.01842(13) Uani d . 1
O O1 0.6450(4) 0.5797(3) 0.7178(2) 0.0308(6) Uani d . 1
O O1W 0.3979(4) 0.7273(3) 1.0725(2) 0.0306(5) Uani d . 1
H H1B 0.4272 0.8029 1.1345 0.037 Uiso d R 1
H H1A 0.2966 0.6641 1.0909 0.037 Uiso d R 1
O O2 0.8478(4) 0.5210(2) 0.86906(19) 0.0223(5) Uani d . 1
O O2W 0.3918(5) 0.7714(3) 0.8168(2) 0.0419(7) Uani d . 1
H H2A 0.2684 0.7847 0.8389 0.050 Uiso d R 1
H H2B 0.3227 0.7272 0.7384 0.050 Uiso d R 1
O O3W 0.3668(9) -0.0370(5) 0.2501(4) 0.0976(14) Uani d . 1
H H3C 0.2806 0.0025 0.2899 0.117 Uiso d R 1
H H3B 0.4059 0.0359 0.2242 0.117 Uiso d R 1
O O3 1.3356(4) 0.4774(3) 0.8838(2) 0.0341(6) Uani d . 1
O O4W 0.600(3) -0.0389(18) 0.4868(15) 0.157(6) Uani d P 0.50
O O4 1.0782(4) 0.2715(3) 0.8653(2) 0.0286(5) Uani d . 1
O O5 0.9956(4) 0.8355(3) 0.9014(2) 0.0288(5) Uani d . 1
C C1 0.7779(5) 0.5111(4) 0.7525(3) 0.0208(6) Uani d . 1
C C2 0.8570(6) 0.4166(4) 0.6544(3) 0.0221(6) Uani d . 1
C C3 0.7531(6) 0.3869(4) 0.5261(3) 0.0291(7) Uani d . 1
H H3A 0.6314 0.4244 0.5043 0.035 Uiso calc R 1
C C4 0.9912(7) 0.2532(5) 0.4643(3) 0.0411(10) Uani d . 1
H H4A 1.0394 0.1988 0.3999 0.049 Uiso calc R 1
C C5 1.1024(7) 0.2746(5) 0.5900(3) 0.0365(9) Uani d . 1
H H5A 1.2219 0.2345 0.6091 0.044 Uiso calc R 1
C C6 1.0344(5) 0.3560(4) 0.6869(3) 0.0224(6) Uani d . 1
C C7 1.1545(5) 0.3722(4) 0.8220(3) 0.0227(7) Uani d . 1
C C8 1.0724(5) 0.9700(3) 0.9563(3) 0.0213(6) Uani d . 1
O O6 0.7452(4) 0.9426(3) 1.0529(2) 0.0285(5) 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'
Y Y -2.7962 3.5667 '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
C3 N1 C4 . . 117.5(3)
O2W Y1 O3 . 1_455 87.14(10)
O2W Y1 O1W . . 80.49(8)
O3 Y1 O1W 1_455 . 72.80(9)
O2W Y1 O5 . . 93.34(10)
O3 Y1 O5 1_455 . 150.67(8)
O1W Y1 O5 . . 136.21(9)
O2W Y1 O4 . 2_767 149.60(9)
O3 Y1 O4 1_455 2_767 111.21(9)
O1W Y1 O4 . 2_767 82.18(8)
O5 Y1 O4 . 2_767 82.21(8)
O2W Y1 O2 . . 128.56(7)
O3 Y1 O2 1_455 . 79.39(8)
O1W Y1 O2 . . 138.60(8)
O5 Y1 O2 . . 77.48(8)
O4 Y1 O2 2_767 . 80.00(8)
O2W Y1 O6 . . 75.21(9)
O3 Y1 O6 1_455 . 139.64(8)
O1W Y1 O6 . . 68.69(8)
O5 Y1 O6 . . 67.83(7)
O4 Y1 O6 2_767 . 75.28(8)
O2 Y1 O6 . . 139.48(8)
O2W Y1 O1 . . 74.64(7)
O3 Y1 O1 1_455 . 78.25(9)
O1W Y1 O1 . . 142.47(9)
O5 Y1 O1 . . 73.65(9)
O4 Y1 O1 2_767 . 131.34(7)
O2 Y1 O1 . . 54.09(7)
O6 Y1 O1 . . 128.75(8)
O2W Y1 C1 . . 101.55(8)
O3 Y1 C1 1_455 . 77.79(9)
O1W Y1 C1 . . 150.40(10)
O5 Y1 C1 . . 73.38(9)
O4 Y1 C1 2_767 . 105.83(8)
O2 Y1 C1 . . 27.13(8)
O6 Y1 C1 . . 140.71(8)
O1 Y1 C1 . . 26.96(8)
O2W Y1 O3 . 2_767 142.60(9)
O3 Y1 O3 1_455 2_767 64.04(9)
O1W Y1 O3 . 2_767 68.91(7)
O5 Y1 O3 . 2_767 123.58(7)
O4 Y1 O3 2_767 2_767 47.17(8)
O2 Y1 O3 . 2_767 71.55(6)
O6 Y1 O3 . 2_767 110.93(7)
O1 Y1 O3 . 2_767 118.26(8)
C1 Y1 O3 . 2_767 95.31(8)
O2W Y1 C7 . 2_767 153.70(8)
O3 Y1 C7 1_455 2_767 88.18(9)
O1W Y1 C7 . 2_767 73.40(8)
O5 Y1 C7 . 2_767 103.19(8)
O4 Y1 C7 2_767 2_767 23.06(9)
O2 Y1 C7 . 2_767 75.69(7)
O6 Y1 C7 . 2_767 92.09(8)
O1 Y1 C7 . 2_767 129.45(8)
C1 Y1 C7 . 2_767 102.71(8)
O3 Y1 C7 2_767 2_767 24.16(9)
C1 O1 Y1 . . 91.26(17)
Y1 O1W H1B . . 124.7
Y1 O1W H1A . . 127.9
H1B O1W H1A . . 103.2
C1 O2 Y1 . . 93.26(16)
Y1 O2W H2A . . 120.6
Y1 O2W H2B . . 122.9
H2A O2W H2B . . 96.6
H3C O3W H3B . . 88.0
C7 O3 Y1 . 1_655 161.8(2)
C7 O3 Y1 . 2_767 82.1(2)
Y1 O3 Y1 1_655 2_767 115.96(9)
C7 O4 Y1 . 2_767 108.9(2)
C8 O5 Y1 . . 119.88(18)
O1 C1 O2 . . 121.4(3)
O1 C1 C2 . . 119.4(2)
O2 C1 C2 . . 119.2(2)
O1 C1 Y1 . . 61.78(15)
O2 C1 Y1 . . 59.61(14)
C2 C1 Y1 . . 177.9(2)
C3 C2 C6 . . 117.8(3)
C3 C2 C1 . . 119.7(3)
C6 C2 C1 . . 122.6(3)
N1 C3 C2 . . 124.1(3)
N1 C3 H3A . . 117.9
C2 C3 H3A . . 117.9
N1 C4 C5 . . 122.6(3)
N1 C4 H4A . . 118.7
C5 C4 H4A . . 118.7
C6 C5 C4 . . 119.4(3)
C6 C5 H5A . . 120.3
C4 C5 H5A . . 120.3
C5 C6 C2 . . 118.6(3)
C5 C6 C7 . . 117.5(3)
C2 C6 C7 . . 123.9(3)
O3 C7 O4 . . 121.7(3)
O3 C7 C6 . . 120.5(3)
O4 C7 C6 . . 117.6(3)
O3 C7 Y1 . 2_767 73.79(18)
O4 C7 Y1 . 2_767 48.06(15)
C6 C7 Y1 . 2_767 162.9(2)
O6 C8 O5 2_777 . 126.4(3)
O6 C8 C8 2_777 2_777 117.3(4)
O5 C8 C8 . 2_777 116.3(3)
C8 O6 Y1 2_777 . 118.70(18)
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
N1 C3 . 1.334(4) ?
N1 C4 . 1.342(4) ?
Y1 O2W . 2.318(2) y
Y1 O3 1_455 2.322(3) y
Y1 O1W . 2.322(2) y
Y1 O5 . 2.371(2) y
Y1 O4 2_767 2.372(2) y
Y1 O2 . 2.399(2) y
Y1 O6 . 2.408(3) y
Y1 O1 . 2.447(2) y
Y1 C1 . 2.777(3) ?
Y1 O3 2_767 2.925(3) ?
Y1 C7 2_767 3.017(3) ?
O1 C1 . 1.259(4) ?
O1W H1B . 0.8500 ?
O1W H1A . 0.8500 ?
O2 C1 . 1.268(3) ?
O2W H2A . 0.8500 ?
O2W H2B . 0.8500 ?
O3W H3C . 0.8499 ?
O3W H3B . 0.8500 ?
O3 C7 . 1.247(4) ?
O4W O4W 2_656 1.62(3) ?
O4 C7 . 1.249(4) ?
O5 C8 . 1.267(4) ?
C1 C2 . 1.497(4) ?
C2 C3 . 1.384(4) ?
C2 C6 . 1.399(4) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.384(5) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.380(5) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.504(4) ?
C7 Y1 2_767 3.017(3) ?
C8 O6 2_777 1.248(4) ?
C8 C8 2_777 1.534(5) ?
O6 C8 2_777 1.248(4) ?
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
O1W H1A O2 2_667 0.85 2.04 2.849(4) 159(4)
O1W H1B O3W 1_566 0.85 1.97 2.775(5) 158(3)
O2W H2A O5 1_455 0.85 2.02 2.865(4) 175(2)
O2W H2B N1 2_666 0.85 1.84 2.662(3) 161(6)
