#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/96/2219652.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_2219652
loop_
_publ_author_name
'Wang, Yuanlan'
'Wang, Chongchen'
_publ_section_title
Poly[diaqua(μ₂-oxalato-κ⁴O¹,O²:O^1'^,O^2'^)(μ₂-pyrazine-2-carboxylato-κ³N¹,O:O')cerium(III)]
_journal_coeditor_code           LH2687
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1282
_journal_page_last               m1283
_journal_paper_doi               10.1107/S1600536808029164
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ce (C5 H3 N2 O2) (C2 O4) (H2 O)2]'
_chemical_formula_moiety         'C7 H7 Ce N2 O8'
_chemical_formula_sum            'C7 H7 Ce N2 O8'
_chemical_formula_weight         387.27
_chemical_name_systematic
Poly[diaqua(μ₂-oxalato-κ⁴O¹,O²:O^1'^,O^2'^)(μ₂-pyrazine-2-carboxylato-κ³N¹,O:O')cerium(III)]
_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           SHELXL97
_cell_angle_alpha                115.514(2)
_cell_angle_beta                 101.7470(10)
_cell_angle_gamma                95.9990(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0298(7)
_cell_length_b                   8.7161(9)
_cell_length_c                   8.8201(9)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.465
_cell_measurement_theta_min      2.653
_cell_volume                     532.38(9)
_computing_cell_refinement       'SAINT (Bruker, 1996)'
_computing_data_collection       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2790
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  0.6722
_exptl_absorpt_correction_T_min  0.4241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.945
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0274P)²+0.3347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                1760
_reflns_number_total             1858
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2687.cif
_cod_data_source_block           I
_cod_database_code               2219652
_cod_database_fobs_code          2219652
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
Ce Ce1 0.33921(2) 0.58558(2) 1.32325(2) 0.01398(8) Uani d . 1
N N1 0.1921(4) 0.7628(4) 1.5966(4) 0.0211(6) Uani d . 1
N N2 0.1556(4) 1.0173(4) 1.9097(4) 0.0265(7) Uani d . 1
O O1 0.3927(3) 0.5389(3) 1.5971(3) 0.0193(5) Uani d . 1
O O2 0.4946(3) 0.6763(4) 1.8853(3) 0.0287(6) Uani d . 1
O O3 0.5575(3) 0.8498(3) 1.5730(3) 0.0214(5) Uani d . 1
O O4 0.6890(3) 1.1263(3) 1.6700(3) 0.0224(5) Uani d . 1
O O5 0.2132(3) 0.4771(4) 0.9986(3) 0.0257(6) Uani d . 1
O O6 -0.0157(3) 0.4293(4) 0.7792(3) 0.0257(6) Uani d . 1
O O7 0.5757(3) 0.6984(3) 1.2121(3) 0.0251(6) Uani d . 1
H H7A 0.6535 0.6401 1.1878 0.030 Uiso d R 1
H H7B 0.5255 0.7040 1.1205 0.030 Uiso d R 1
O O8 0.2021(3) 0.2812(3) 1.2493(3) 0.0228(5) Uani d . 1
H H8A 0.1736 0.2001 1.1447 0.027 Uiso d R 1
H H8B 0.2566 0.2414 1.3126 0.027 Uiso d R 1
C C1 0.3960(4) 0.6567(4) 1.7474(5) 0.0186(7) Uani d . 1
C C2 0.2763(4) 0.7791(4) 1.7518(5) 0.0194(7) Uani d . 1
C C3 0.2585(5) 0.9048(5) 1.9071(5) 0.0258(8) Uani d . 1
H H3 0.3192 0.9114 2.0122 0.031 Uiso calc R 1
C C4 0.0669(5) 0.9965(5) 1.7544(5) 0.0273(8) Uani d . 1
H H4 -0.0092 1.0689 1.7502 0.033 Uiso calc R 1
C C5 0.0845(5) 0.8704(5) 1.5992(5) 0.0264(8) Uani d . 1
H H5 0.0197 0.8603 1.4939 0.032 Uiso calc R 1
C C6 0.5713(4) 0.9932(4) 1.5705(4) 0.0159(7) Uani d . 1
C C7 0.0567(4) 0.4734(4) 0.9350(4) 0.0187(7) 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'
Ce Ce -0.2486 2.6331 '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
O8 Ce1 O4 . 2_678 149.92(8) n
O8 Ce1 O5 . . 82.87(9) n
O4 Ce1 O5 2_678 . 81.64(8) n
O8 Ce1 O3 . . 139.44(8) n
O4 Ce1 O3 2_678 . 64.55(7) n
O5 Ce1 O3 . . 136.12(8) n
O8 Ce1 O6 . 2_567 76.91(9) n
O4 Ce1 O6 2_678 2_567 73.14(8) n
O5 Ce1 O6 . 2_567 63.80(8) n
O3 Ce1 O6 . 2_567 124.88(8) n
O8 Ce1 O1 . . 68.68(8) n
O4 Ce1 O1 2_678 . 123.57(8) n
O5 Ce1 O1 . . 151.55(9) n
O3 Ce1 O1 . . 71.80(8) n
O6 Ce1 O1 2_567 . 107.92(8) n
O8 Ce1 O7 . . 130.61(8) ?
O4 Ce1 O7 2_678 . 67.79(8) ?
O5 Ce1 O7 . . 72.58(8) ?
O3 Ce1 O7 . . 69.25(8) ?
O6 Ce1 O7 2_567 . 124.39(8) ?
O1 Ce1 O7 . . 126.31(8) ?
O8 Ce1 O1 . 2_668 77.10(8) ?
O4 Ce1 O1 2_678 2_668 132.90(8) ?
O5 Ce1 O1 . 2_668 114.25(8) ?
O3 Ce1 O1 . 2_668 75.86(7) ?
O6 Ce1 O1 2_567 2_668 153.96(9) ?
O1 Ce1 O1 . 2_668 60.35(9) ?
O7 Ce1 O1 . 2_668 75.23(8) ?
O8 Ce1 N1 . . 97.71(9) ?
O4 Ce1 N1 2_678 . 72.66(9) ?
O5 Ce1 N1 . . 128.42(8) ?
O3 Ce1 N1 . . 68.56(9) ?
O6 Ce1 N1 2_567 . 66.20(8) ?
O1 Ce1 N1 . . 58.85(8) ?
O7 Ce1 N1 . . 131.17(9) ?
O1 Ce1 N1 2_668 . 116.07(8) ?
O8 Ce1 O2 . 2_668 66.33(8) ?
O4 Ce1 O2 2_678 2_668 129.05(8) ?
O5 Ce1 O2 . 2_668 67.54(8) ?
O3 Ce1 O2 . 2_668 112.59(8) ?
O6 Ce1 O2 2_567 2_668 121.33(8) ?
O1 Ce1 O2 . 2_668 99.44(7) ?
O7 Ce1 O2 . 2_668 64.80(8) ?
O1 Ce1 O2 2_668 2_668 46.97(7) ?
N1 Ce1 O2 . 2_668 157.52(8) ?
C5 N1 C2 . . 116.2(3) ?
C5 N1 Ce1 . . 126.2(2) ?
C2 N1 Ce1 . . 114.7(2) ?
C4 N2 C3 . . 116.2(3) ?
C1 O1 Ce1 . . 122.9(2) ?
C1 O1 Ce1 . 2_668 100.9(2) ?
Ce1 O1 Ce1 . 2_668 119.65(9) ?
C1 O2 Ce1 . 2_668 88.3(2) ?
C6 O3 Ce1 . . 119.4(2) ?
C6 O4 Ce1 . 2_678 120.1(2) ?
C7 O5 Ce1 . . 121.5(2) ?
C7 O6 Ce1 . 2_567 121.0(2) ?
Ce1 O7 H7A . . 117.4 ?
Ce1 O7 H7B . . 108.6 ?
H7A O7 H7B . . 107.4 ?
Ce1 O8 H8A . . 120.9 ?
Ce1 O8 H8B . . 114.4 ?
H8A O8 H8B . . 106.6 ?
O2 C1 O1 . . 123.3(3) ?
O2 C1 C2 . . 120.1(3) ?
O1 C1 C2 . . 116.6(3) ?
N1 C2 C3 . . 122.0(3) ?
N1 C2 C1 . . 115.8(3) ?
C3 C2 C1 . . 122.2(3) ?
N2 C3 C2 . . 121.6(4) ?
N2 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
N2 C4 C5 . . 122.1(3) ?
N2 C4 H4 . . 119.0 ?
C5 C4 H4 . . 119.0 ?
N1 C5 C4 . . 121.8(3) ?
N1 C5 H5 . . 119.1 ?
C4 C5 H5 . . 119.1 ?
O4 C6 O3 . . 126.0(3) ?
O4 C6 C6 . 2_678 117.0(3) ?
O3 C6 C6 . 2_678 117.0(4) ?
O6 C7 O5 . . 126.5(3) ?
O6 C7 C7 . 2_567 117.4(4) ?
O5 C7 C7 . 2_567 116.1(4) ?
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
Ce1 O8 . 2.506(2) y
Ce1 O4 2_678 2.521(2) y
Ce1 O5 . 2.530(2) y
Ce1 O3 . 2.538(2) y
Ce1 O6 2_567 2.540(2) y
Ce1 O1 . 2.578(2) y
Ce1 O7 . 2.595(3) y
Ce1 O1 2_668 2.614(2) y
Ce1 N1 . 2.815(3) y
Ce1 O2 2_668 2.897(3) y
N1 C5 . 1.337(5) ?
N1 C2 . 1.337(5) ?
N2 C4 . 1.333(5) ?
N2 C3 . 1.343(5) ?
O1 C1 . 1.273(4) ?
O1 Ce1 2_668 2.614(2) ?
O2 C1 . 1.240(4) ?
O2 Ce1 2_668 2.897(3) ?
O3 C6 . 1.254(4) ?
O4 C6 . 1.251(4) ?
O4 Ce1 2_678 2.521(2) ?
O5 C7 . 1.259(4) ?
O6 C7 . 1.244(4) ?
O6 Ce1 2_567 2.540(2) ?
O7 H7A . 0.8500 ?
O7 H7B . 0.8500 ?
O8 H8A . 0.8500 ?
O8 H8B . 0.8500 ?
C1 C2 . 1.502(5) ?
C2 C3 . 1.384(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(5) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C6 2_678 1.564(6) ?
C7 C7 2_567 1.554(7) ?
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
O7 H7A O5 2_667 0.85 2.10 2.836(4) 145.3
O7 H7B O2 1_554 0.85 1.94 2.738(4) 155.7
O8 H8A N2 1_544 0.85 1.96 2.799(4) 169.1
O8 H8B O3 2_668 0.85 2.05 2.873(3) 162.8
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_4
_geom_torsion
O8 Ce1 N1 C5 . . -117.5(3)
O4 Ce1 N1 C5 2_678 . 33.2(3)
O5 Ce1 N1 C5 . . -30.5(4)
O3 Ce1 N1 C5 . . 102.1(3)
O6 Ce1 N1 C5 2_567 . -45.6(3)
O1 Ce1 N1 C5 . . -176.8(3)
O7 Ce1 N1 C5 . . 70.2(3)
O1 Ce1 N1 C5 2_668 . 163.1(3)
O2 Ce1 N1 C5 2_668 . -160.4(3)
O8 Ce1 N1 C2 . . 82.8(3)
O4 Ce1 N1 C2 2_678 . -126.4(3)
O5 Ce1 N1 C2 . . 169.8(2)
O3 Ce1 N1 C2 . . -57.6(2)
O6 Ce1 N1 C2 2_567 . 154.8(3)
O1 Ce1 N1 C2 . . 23.5(2)
O7 Ce1 N1 C2 . . -89.5(3)
O1 Ce1 N1 C2 2_668 . 3.4(3)
O2 Ce1 N1 C2 2_668 . 39.9(4)
O8 Ce1 O1 C1 . . -144.1(3)
O4 Ce1 O1 C1 2_678 . 4.7(3)
O5 Ce1 O1 C1 . . -144.4(2)
O3 Ce1 O1 C1 . . 45.2(2)
O6 Ce1 O1 C1 2_567 . -76.6(3)
O7 Ce1 O1 C1 . . 90.4(3)
O1 Ce1 O1 C1 2_668 . 129.0(3)
N1 Ce1 O1 C1 . . -30.3(2)
O2 Ce1 O1 C1 2_668 . 156.0(3)
O8 Ce1 O1 Ce1 . 2_668 86.94(11)
O4 Ce1 O1 Ce1 2_678 2_668 -124.21(10)
O5 Ce1 O1 Ce1 . 2_668 86.64(18)
O3 Ce1 O1 Ce1 . 2_668 -83.76(11)
O6 Ce1 O1 Ce1 2_567 2_668 154.49(10)
O7 Ce1 O1 Ce1 . 2_668 -38.53(14)
O1 Ce1 O1 Ce1 2_668 2_668 0.0
N1 Ce1 O1 Ce1 . 2_668 -159.23(14)
O2 Ce1 O1 Ce1 2_668 2_668 27.05(11)
O8 Ce1 O3 C6 . . -168.2(2)
O4 Ce1 O3 C6 2_678 . -11.6(2)
O5 Ce1 O3 C6 . . 31.8(3)
O6 Ce1 O3 C6 2_567 . -55.2(3)
O1 Ce1 O3 C6 . . -154.8(3)
O7 Ce1 O3 C6 . . 62.9(2)
O1 Ce1 O3 C6 2_668 . 142.2(3)
N1 Ce1 O3 C6 . . -91.9(2)
O2 Ce1 O3 C6 2_668 . 112.3(2)
O8 Ce1 O5 C7 . . 82.8(3)
O4 Ce1 O5 C7 2_678 . -71.3(3)
O3 Ce1 O5 C7 . . -110.1(3)
O6 Ce1 O5 C7 2_567 . 3.9(3)
O1 Ce1 O5 C7 . . 83.1(3)
O7 Ce1 O5 C7 . . -140.6(3)
O1 Ce1 O5 C7 2_668 . 155.2(3)
N1 Ce1 O5 C7 . . -11.4(3)
O2 Ce1 O5 C7 2_668 . 150.1(3)
Ce1 O2 C1 O1 2_668 . 6.9(3)
Ce1 O2 C1 C2 2_668 . -171.1(3)
Ce1 O1 C1 O2 . . -144.3(3)
Ce1 O1 C1 O2 2_668 . -7.8(4)
Ce1 O1 C1 C2 . . 33.8(4)
Ce1 O1 C1 C2 2_668 . 170.3(3)
C5 N1 C2 C3 . . -2.5(5)
Ce1 N1 C2 C3 . . 159.3(3)
C5 N1 C2 C1 . . 179.6(3)
Ce1 N1 C2 C1 . . -18.6(4)
O2 C1 C2 N1 . . 171.3(3)
O1 C1 C2 N1 . . -6.8(5)
O2 C1 C2 C3 . . -6.6(5)
O1 C1 C2 C3 . . 175.3(3)
C4 N2 C3 C2 . . 2.5(6)
N1 C2 C3 N2 . . -0.1(6)
C1 C2 C3 N2 . . 177.7(3)
C3 N2 C4 C5 . . -2.4(6)
C2 N1 C5 C4 . . 2.6(6)
Ce1 N1 C5 C4 . . -156.8(3)
N2 C4 C5 N1 . . -0.2(6)
Ce1 O4 C6 O3 2_678 . -168.9(3)
Ce1 O4 C6 C6 2_678 2_678 11.3(5)
Ce1 O3 C6 O4 . . -169.0(3)
Ce1 O3 C6 C6 . 2_678 10.8(5)
Ce1 O6 C7 O5 2_567 . 176.2(3)
Ce1 O6 C7 C7 2_567 2_567 -2.7(5)
Ce1 O5 C7 O6 . . 176.9(3)
Ce1 O5 C7 C7 . 2_567 -4.2(5)
