#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/34/2223433.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_2223433
loop_
_publ_author_name
'Guo, Hai-Fu'
'Qin, Liang'
'Hao, Xiang-Ying'
_publ_section_title
Poly[diaqua(μ₂-5-carboxypyridine-3-carboxylato-κ²N:O³)hemi(μ₂-oxalato-κ⁴O¹,O²:O^1'^,O^2'^)(μ₄-pyridine-3,5-dicarboxylato-κ⁴N:O³:O^3'^:O⁵)silver(I)terbium(III)]
_journal_coeditor_code           HY2227
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1214
_journal_page_last               m1215
_journal_paper_doi               10.1107/S1600536809036393
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Ag Tb (C7 H3 N O4) (C7 H4 N O4) (C2 O4)0.5 (H2 O)2]'
_chemical_formula_moiety         'C15 H11 Ag N2 O12 Tb'
_chemical_formula_sum            'C15 H11 Ag N2 O12 Tb'
_chemical_formula_weight         678.05
_chemical_name_systematic
;
\
Poly[diaqua(μ₂-3-carboxypyridine-5-carboxylato-κ²N:O⁵)\
(hemi-μ₂-oxalato-κ⁴O¹,O²:O^1'^,O^2'^)\
(μ₄-pyridine-3,5-dicarboxylato-κ⁴N:O³:O^3'^:\
O⁵)silver(I)terbium(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           SHELXL-97
_cell_angle_alpha                98.956(4)
_cell_angle_beta                 99.556(4)
_cell_angle_gamma                95.839(5)
_cell_formula_units_Z            2
_cell_length_a                   7.592(3)
_cell_length_b                   8.249(3)
_cell_length_c                   14.241(6)
_cell_measurement_reflns_used    3600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1.36
_cell_volume                     861.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4416
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.287
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.793
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0323P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                2862
_reflns_number_total             3032
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            hy2227.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2223433
_cod_database_fobs_code          2223433
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb Tb1 0.80756(3) 0.29706(2) 0.080761(13) 0.01369(8) Uani d . 1 . .
Ag Ag1 0.17209(6) 0.40250(5) 0.53284(3) 0.03343(12) Uani d . 1 . .
O O1 0.4372(5) 0.2187(4) 0.2009(2) 0.0305(8) Uani d . 1 . .
O O1W 0.7121(5) 0.5291(4) 0.0096(2) 0.0278(8) Uani d . 1 . .
H H1W 0.7742 0.5573 -0.0302 0.042 Uiso d R 1 . .
H H2W 0.6316 0.5904 0.0165 0.042 Uiso d R 1 . .
O O2 0.6205(4) 0.4300(4) 0.1747(2) 0.0255(7) Uani d . 1 . .
O O2W 1.0914(4) 0.1769(4) 0.0759(2) 0.0253(7) Uani d . 1 . .
H H3W 1.1070 0.1393 0.0200 0.038 Uiso d R 1 . .
H H4W 1.1876 0.1905 0.1166 0.038 Uiso d R 1 . .
O O3 0.4778(6) 0.9748(5) 0.2896(3) 0.0449(10) Uani d . 1 . .
O O4 0.3416(5) 1.0334(4) 0.4169(2) 0.0346(8) Uani d . 1 . .
O O5 1.0531(4) 0.5114(3) 0.1239(2) 0.0203(7) Uani d . 1 . .
O O9 0.5031(4) 0.2064(3) -0.0119(2) 0.0209(7) Uani d . 1 . .
N N1 0.3034(5) 0.5246(4) 0.4335(3) 0.0234(8) Uani d . 1 . .
N N2 0.8987(5) 0.7556(4) 0.3678(2) 0.0192(8) Uani d . 1 . .
C C1 0.3576(6) 0.4244(5) 0.3627(3) 0.0231(10) Uani d . 1 . .
H H1 0.3377 0.3106 0.3601 0.028 Uiso calc R 1 . .
C C2 0.4420(6) 0.4845(5) 0.2934(3) 0.0188(9) Uani d . 1 . .
C C3 0.4629(6) 0.6531(5) 0.2942(3) 0.0204(9) Uani d . 1 . .
H H3 0.5162 0.6965 0.2476 0.025 Uiso calc R 1 . .
C C4 0.4032(6) 0.7568(5) 0.3654(3) 0.0200(9) Uani d . 1 . .
C C5 0.3273(6) 0.6886(5) 0.4347(3) 0.0208(10) Uani d . 1 . .
H H5 0.2917 0.7587 0.4838 0.025 Uiso calc R 1 . .
C C6 0.5041(6) 0.3688(5) 0.2177(3) 0.0216(10) Uani d . 1 . .
C C7 0.4047(6) 0.9388(6) 0.3621(3) 0.0246(10) Uani d . 1 . .
C C8 0.9565(6) 0.6777(5) 0.2901(3) 0.0165(9) Uani d . 1 . .
H H8 0.9658 0.5652 0.2849 0.020 Uiso calc R 1 . .
C C9 1.0023(6) 0.7592(5) 0.2182(3) 0.0169(9) Uani d . 1 . .
C C10 0.9849(6) 0.9277(5) 0.2249(3) 0.0168(9) Uani d . 1 . .
H H10 1.0142 0.9848 0.1770 0.020 Uiso calc R 1 . .
C C11 0.9234(6) 1.0091(5) 0.3038(3) 0.0166(9) Uani d . 1 . .
C C12 0.8845(6) 0.9188(5) 0.3740(3) 0.0201(9) Uani d . 1 . .
H H12 0.8469 0.9732 0.4279 0.024 Uiso calc R 1 . .
C C13 1.0667(6) 0.6684(5) 0.1333(3) 0.0151(9) Uani d . 1 . .
C C15 0.4376(6) 0.0595(5) -0.0196(3) 0.0168(9) Uani d . 1 . .
O O6 1.1310(4) 0.7500(3) 0.0780(2) 0.0211(7) Uani d . 1 . .
C C14 0.9003(6) 1.1915(5) 0.3113(3) 0.0202(10) Uani d . 1 . .
O O7 0.8768(5) 1.2673(4) 0.3899(2) 0.0328(8) Uani d . 1 . .
O O10 0.2771(4) -0.0028(3) -0.0543(2) 0.0219(7) Uani d . 1 . .
O O8 0.9101(5) 1.2520(4) 0.2359(2) 0.0262(8) Uani d . 1 . .
H H3A 0.461(9) 1.076(8) 0.276(4) 0.056(18) Uiso 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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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 Tb1 O2 1_545 . 75.61(11) ?
O8 Tb1 O6 1_545 2_765 141.96(11) ?
O2 Tb1 O6 . 2_765 142.34(10) ?
O8 Tb1 O5 1_545 . 82.16(11) ?
O2 Tb1 O5 . . 96.02(11) ?
O6 Tb1 O5 2_765 . 89.03(10) ?
O8 Tb1 O10 1_545 2_655 81.37(10) ?
O2 Tb1 O10 . 2_655 109.81(11) ?
O6 Tb1 O10 2_765 2_655 85.00(10) ?
O5 Tb1 O10 . 2_655 144.60(10) ?
O8 Tb1 O1W 1_545 . 135.70(10) ?
O2 Tb1 O1W . . 71.23(11) ?
O6 Tb1 O1W 2_765 . 74.71(10) ?
O5 Tb1 O1W . . 73.14(11) ?
O10 Tb1 O1W 2_655 . 137.38(11) ?
O8 Tb1 O9 1_545 . 125.23(12) ?
O2 Tb1 O9 . . 75.56(11) ?
O6 Tb1 O9 2_765 . 79.71(11) ?
O5 Tb1 O9 . . 146.28(10) ?
O10 Tb1 O9 2_655 . 66.38(9) ?
O1W Tb1 O9 . . 73.25(11) ?
O8 Tb1 O2W 1_545 . 73.67(11) ?
O2 Tb1 O2W . . 147.82(10) ?
O6 Tb1 O2W 2_765 . 68.50(10) ?
O5 Tb1 O2W . . 70.60(11) ?
O10 Tb1 O2W 2_655 . 74.76(11) ?
O1W Tb1 O2W . . 127.82(11) ?
O9 Tb1 O2W . . 131.32(10) ?
N2 Ag1 N1 2_666 . 164.83(14) ?
N2 Ag1 Ag1 2_666 2_566 108.80(10) ?
N1 Ag1 Ag1 . 2_566 86.10(10) ?
N2 Ag1 O7 2_666 1_445 93.85(11) ?
N1 Ag1 O7 . 1_445 92.40(13) ?
N1 Ag1 O7 . 2_676 83.19(11) ?
N2 Ag1 O7 2_666 2_676 107.77(11) ?
O7 Ag1 O7 1_445 2_676 108.60(9) ?
Tb1 O1W H1W . . 113.8 ?
Tb1 O1W H2W . . 134.5 ?
H1W O1W H2W . . 111.6 ?
C6 O2 Tb1 . . 129.6(3) ?
Tb1 O2W H3W . . 114.5 ?
Tb1 O2W H4W . . 131.1 ?
H3W O2W H4W . . 111.7 ?
C7 O3 H3A . . 113(4) ?
C13 O5 Tb1 . . 133.9(3) ?
C15 O9 Tb1 . . 118.8(3) ?
C5 N1 C1 . . 118.3(4) ?
C5 N1 Ag1 . . 125.6(3) ?
C1 N1 Ag1 . . 116.1(3) ?
C8 N2 C12 . . 118.2(4) ?
C8 N2 Ag1 . 2_666 114.8(3) ?
C12 N2 Ag1 . 2_666 127.0(3) ?
N1 C1 C2 . . 122.6(4) ?
N1 C1 H1 . . 118.7 ?
C2 C1 H1 . . 118.7 ?
C3 C2 C1 . . 118.6(4) ?
C3 C2 C6 . . 120.7(4) ?
C1 C2 C6 . . 120.7(4) ?
C2 C3 C4 . . 119.1(4) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 C3 . . 119.0(4) ?
C5 C4 C7 . . 120.2(4) ?
C3 C4 C7 . . 120.6(4) ?
N1 C5 C4 . . 122.3(4) ?
N1 C5 H5 . . 118.9 ?
C4 C5 H5 . . 118.9 ?
O1 C6 O2 . . 124.7(4) ?
O1 C6 C2 . . 118.4(4) ?
O2 C6 C2 . . 116.9(4) ?
O4 C7 O3 . . 126.2(4) ?
O4 C7 C4 . . 124.1(4) ?
O3 C7 C4 . . 109.6(4) ?
N2 C8 C9 . . 122.3(4) ?
N2 C8 H8 . . 118.8 ?
C9 C8 H8 . . 118.8 ?
C8 C9 C10 . . 118.9(4) ?
C8 C9 C13 . . 120.7(4) ?
C10 C9 C13 . . 120.4(4) ?
C11 C10 C9 . . 119.4(4) ?
C11 C10 H10 . . 120.3 ?
C9 C10 H10 . . 120.3 ?
C12 C11 C10 . . 117.9(4) ?
C12 C11 C14 . . 122.0(4) ?
C10 C11 C14 . . 120.1(4) ?
N2 C12 C11 . . 123.2(4) ?
N2 C12 H12 . . 118.4 ?
C11 C12 H12 . . 118.4 ?
O6 C13 O5 . . 124.4(4) ?
O6 C13 C9 . . 118.5(3) ?
O5 C13 C9 . . 117.1(4) ?
O9 C15 O10 . . 126.9(4) ?
O9 C15 C15 . 2_655 117.3(5) ?
O10 C15 C15 . 2_655 115.7(4) ?
C13 O6 Tb1 . 2_765 137.7(3) ?
O7 C14 O8 . . 126.2(4) ?
O7 C14 C11 . . 118.2(4) ?
O8 C14 C11 . . 115.6(4) ?
C15 O10 Tb1 . 2_655 120.5(2) ?
C14 O8 Tb1 . 1_565 155.4(3) ?
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
Tb1 O2 . 2.346(3) y
Tb1 O5 . 2.364(3) y
Tb1 O6 2_765 2.365(3) y
Tb1 O8 1_545 2.317(3) y
Tb1 O9 . 2.444(3) y
Tb1 O10 2_655 2.401(3) y
Tb1 O1W . 2.421(3) y
Tb1 O2W . 2.468(3) y
Ag1 N1 . 2.172(4) y
Ag1 N2 2_666 2.162(4) y
Ag1 O7 1_445 2.772(3) y
Ag1 O7 2_676 2.859(3) y
Ag1 Ag1 2_566 3.2867(12) ?
O1 C6 . 1.260(5) ?
O1W H1W . 0.8401 ?
O1W H2W . 0.8400 ?
O2 C6 . 1.263(6) ?
O2W H3W . 0.8402 ?
O2W H4W . 0.8400 ?
O3 C7 . 1.309(6) ?
O3 H3A . 0.90(6) ?
O4 C7 . 1.207(5) ?
O5 C13 . 1.273(5) ?
O9 C15 . 1.244(5) ?
N1 C5 . 1.343(6) ?
N1 C1 . 1.348(5) ?
N2 C8 . 1.352(5) ?
N2 C12 . 1.351(5) ?
N2 Ag1 2_666 2.162(4) ?
C1 C2 . 1.388(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.382(6) ?
C2 C6 . 1.494(6) ?
C3 C4 . 1.388(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.386(6) ?
C4 C7 . 1.508(6) ?
C5 H5 . 0.9300 ?
C8 C9 . 1.381(6) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.400(6) ?
C9 C13 . 1.500(6) ?
C10 C11 . 1.391(6) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.388(6) ?
C11 C14 . 1.522(6) ?
C12 H12 . 0.9300 ?
C13 O6 . 1.241(5) ?
C15 O10 . 1.260(5) ?
C15 C15 2_655 1.535(8) ?
C14 O7 . 1.244(5) ?
C14 O8 . 1.262(5) ?
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 H1W O5 2_765 0.84 2.08 2.820(5) 147 y
O1W H1W O2W 2_765 0.84 2.55 3.221(5) 138 y
O1W H2W O9 2_665 0.84 2.05 2.855(4) 159 y
O2W H3W O10 1_655 0.84 2.13 2.839(4) 142 y
O2W H4W O1 1_655 0.84 2.04 2.873(5) 173 y
O3 H3A O1 1_565 0.90(6) 1.71(7) 2.554(5) 154(6) y
C10 H10 O2W 1_565 0.93 2.40 3.314(6) 169 y
