#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210479.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7210479
loop_
_publ_author_name
'Yang, Ai-Hong'
'Gao, Hong-Ling'
'Cui, Jian-Zhong'
'Zhao, Bin'
_publ_section_title
;
 Syntheses, structures, and photoluminescence of lanthanide coordination
 polymers with pyridine-2,3,5,6-tetracarboxylic acid
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1870
_journal_paper_doi               10.1039/c0ce00397b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C9 H10 N O12 Pr'
_chemical_formula_weight         465.09
_chemical_name_systematic
;
?
;
_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                95.53(3)
_cell_angle_beta                 115.45(3)
_cell_angle_gamma                95.45(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4864(17)
_cell_length_b                   8.9615(18)
_cell_length_c                   9.4369(19)
_cell_measurement_reflns_used    2208
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.872
_cell_measurement_theta_min      2.360
_cell_volume                     637.6(3)
_computing_cell_refinement       crystalclear
_computing_data_collection       'crystalclear(Rigaku/MSC Inc., 2005)'
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'rigaku saturn CCD area detector'
_diffrn_measurement_method       'ω and φ 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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5531
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_T_max  0.6967
_exptl_absorpt_correction_T_min  0.5406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.960
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0275
_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)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                2557
_reflns_number_total             2910
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7210475
_cod_data_source_file            c0ce00397b.txt
_cod_data_source_block           r91002f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        637.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pr1 Pr 0.67971(2) 0.30371(2) 0.30549(2) 0.00600(7) Uani 1 1 d .
O1 O 0.4128(3) 0.0971(3) 0.1586(3) 0.0088(6) Uani 1 1 d .
O2 O 0.1631(3) -0.0686(3) 0.0312(3) 0.0111(6) Uani 1 1 d .
H2A H 0.1759 -0.0513 -0.0495 0.017 Uiso 1 1 calc R
O3 O 0.3715(4) -0.2517(3) 0.2372(3) 0.0206(7) Uani 1 1 d .
O4 O 0.3611(3) -0.3333(3) 0.4508(3) 0.0108(6) Uani 1 1 d .
O5 O 0.2212(3) -0.0764(3) 0.7880(3) 0.0092(6) Uani 1 1 d .
O6 O 0.1854(4) 0.1681(3) 0.7943(3) 0.0168(7) Uani 1 1 d .
O7 O -0.0199(3) 0.3246(3) 0.5165(3) 0.0095(6) Uani 1 1 d .
O8 O 0.2643(3) 0.4243(3) 0.6084(3) 0.0122(6) Uani 1 1 d .
O9 O 0.4041(3) 0.4150(3) 0.2403(3) 0.0158(6) Uani 1 1 d .
H9A H 0.3959 0.4839 0.3046 0.024 Uiso 1 1 d R
H9B H 0.3153 0.3965 0.1501 0.024 Uiso 1 1 d R
O10 O 0.9217(3) 0.4252(3) 0.2283(3) 0.0142(6) Uani 1 1 d .
H10A H 0.9001 0.4691 0.1476 0.021 Uiso 1 1 d R
H10B H 0.9765 0.4895 0.3124 0.021 Uiso 1 1 d R
O11 O 0.5518(4) 0.3297(4) 0.0130(3) 0.0258(8) Uani 1 1 d .
H11A H 0.6020 0.3337 -0.0481 0.039 Uiso 1 1 d R
H11B H 0.4542 0.2701 -0.0282 0.039 Uiso 1 1 d R
N1 N 0.2750(4) -0.0748(4) 0.5343(3) 0.0064(6) Uani 1 1 d .
C1 C 0.3461(5) -0.2366(4) 0.3574(4) 0.0090(8) Uani 1 1 d .
C2 C 0.2900(5) -0.0899(4) 0.3977(4) 0.0053(7) Uani 1 1 d .
C3 C 0.2569(5) 0.0259(4) 0.3042(4) 0.0069(8) Uani 1 1 d .
C4 C 0.2055(4) 0.1553(4) 0.3519(4) 0.0078(8) Uani 1 1 d .
H4 H 0.1828 0.2347 0.2892 0.009 Uiso 1 1 calc R
C5 C 0.1866(4) 0.1698(4) 0.4926(4) 0.0059(8) Uani 1 1 d .
C6 C 0.2232(5) 0.0495(4) 0.5798(4) 0.0057(7) Uani 1 1 d .
C7 C 0.2085(5) 0.0501(4) 0.7338(4) 0.0080(8) Uani 1 1 d .
C8 C 0.2863(5) 0.0183(4) 0.1569(4) 0.0073(8) Uani 1 1 d U
C9 C 0.1386(5) 0.3163(4) 0.5448(4) 0.0065(8) Uani 1 1 d .
O12 O 0.9149(3) 0.6516(3) 0.0281(3) 0.0158(6) Uani 1 1 d .
H12A H 0.8773 0.7106 0.0789 0.024 Uiso 1 1 d R
H12B H 1.0191 0.6873 0.0455 0.024 Uiso 1 1 d R
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'
Pr Pr -0.2180 2.8214 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O8 Pr1 O7 81.19(10) 2_666 1_655
O8 Pr1 O4 75.38(9) 2_666 2_656
O7 Pr1 O4 76.80(9) 1_655 2_656
O8 Pr1 O9 67.32(9) 2_666 .
O7 Pr1 O9 140.81(9) 1_655 .
O4 Pr1 O9 73.21(9) 2_656 .
O8 Pr1 O5 147.73(8) 2_666 2_656
O7 Pr1 O5 79.27(9) 1_655 2_656
O4 Pr1 O5 123.91(8) 2_656 2_656
O9 Pr1 O5 139.03(9) . 2_656
O8 Pr1 O11 93.53(10) 2_666 .
O7 Pr1 O11 133.85(9) 1_655 .
O4 Pr1 O11 146.18(9) 2_656 .
O9 Pr1 O11 73.03(10) . .
O5 Pr1 O11 82.01(10) 2_656 .
O8 Pr1 O1 137.54(8) 2_666 .
O7 Pr1 O1 137.02(9) 1_655 .
O4 Pr1 O1 93.83(8) 2_656 .
O9 Pr1 O1 70.24(9) . .
O5 Pr1 O1 71.59(9) 2_656 .
O11 Pr1 O1 72.75(9) . .
O8 Pr1 N1 131.49(9) 2_666 2_656
O7 Pr1 N1 67.28(9) 1_655 2_656
O4 Pr1 N1 62.49(9) 2_656 2_656
O9 Pr1 N1 117.51(9) . 2_656
O5 Pr1 N1 61.53(9) 2_656 2_656
O11 Pr1 N1 134.92(10) . 2_656
O1 Pr1 N1 71.20(9) . 2_656
O8 Pr1 O10 71.50(9) 2_666 .
O7 Pr1 O10 66.85(8) 1_655 .
O4 Pr1 O10 133.58(9) 2_656 .
O9 Pr1 O10 120.04(9) . .
O5 Pr1 O10 77.28(8) 2_656 .
O11 Pr1 O10 68.03(9) . .
O1 Pr1 O10 132.47(8) . .
N1 Pr1 O10 122.36(9) 2_656 .
C8 O1 Pr1 149.1(2) . .
C8 O2 H2A 109.5 . .
C1 O4 Pr1 127.3(2) . 2_656
C7 O5 Pr1 126.8(2) . 2_656
C9 O7 Pr1 144.1(2) . 1_455
C9 O8 Pr1 140.5(2) . 2_666
Pr1 O9 H9A 121.9 . .
Pr1 O9 H9B 123.9 . .
H9A O9 H9B 113.8 . .
Pr1 O10 H10A 124.7 . .
Pr1 O10 H10B 96.3 . .
H10A O10 H10B 109.7 . .
Pr1 O11 H11A 129.9 . .
Pr1 O11 H11B 103.8 . .
H11A O11 H11B 113.3 . .
C6 N1 C2 120.2(3) . .
C6 N1 Pr1 120.8(2) . 2_656
C2 N1 Pr1 118.8(2) . 2_656
O3 C1 O4 126.6(4) . .
O3 C1 C2 117.5(3) . .
O4 C1 C2 116.0(3) . .
N1 C2 C3 120.6(3) . .
N1 C2 C1 115.3(3) . .
C3 C2 C1 124.2(3) . .
C4 C3 C2 119.4(3) . .
C4 C3 C8 118.5(3) . .
C2 C3 C8 122.0(3) . .
C3 C4 C5 120.1(3) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C6 C5 C4 117.1(4) . .
C6 C5 C9 124.4(3) . .
C4 C5 C9 118.4(3) . .
N1 C6 C5 122.7(3) . .
N1 C6 C7 114.6(3) . .
C5 C6 C7 122.7(3) . .
O6 C7 O5 126.4(3) . .
O6 C7 C6 118.3(3) . .
O5 C7 C6 115.3(3) . .
O1 C8 O2 124.6(3) . .
O1 C8 C3 119.9(3) . .
O2 C8 C3 115.3(3) . .
O8 C9 O7 125.3(4) . .
O8 C9 C5 114.7(3) . .
O7 C9 C5 119.9(3) . .
H12A O12 H12B 110.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O8 2.428(3) 2_666
Pr1 O7 2.444(3) 1_655
Pr1 O4 2.463(3) 2_656
Pr1 O9 2.484(3) .
Pr1 O5 2.500(3) 2_656
Pr1 O11 2.539(3) .
Pr1 O1 2.548(3) .
Pr1 N1 2.625(3) 2_656
Pr1 O10 2.636(3) .
O1 C8 1.220(4) .
O2 C8 1.307(4) .
O2 H2A 0.8400 .
O3 C1 1.239(4) .
O4 C1 1.271(4) .
O4 Pr1 2.463(3) 2_656
O5 C7 1.283(4) .
O5 Pr1 2.500(3) 2_656
O6 C7 1.226(5) .
O7 C9 1.265(4) .
O7 Pr1 2.444(3) 1_455
O8 C9 1.256(4) .
O8 Pr1 2.428(3) 2_666
O9 H9A 0.8519 .
O9 H9B 0.8475 .
O10 H10A 0.8487 .
O10 H10B 0.8493 .
O11 H11A 0.8528 .
O11 H11B 0.8491 .
N1 C6 1.336(5) .
N1 C2 1.344(4) .
N1 Pr1 2.625(3) 2_656
C1 C2 1.509(5) .
C2 C3 1.397(5) .
C3 C4 1.379(5) .
C3 C8 1.511(5) .
C4 C5 1.400(5) .
C4 H4 0.9500 .
C5 C6 1.396(5) .
C5 C9 1.510(5) .
C6 C7 1.511(5) .
O12 H12A 0.8529 .
O12 H12B 0.8503 .
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
_geom_torsion_site_symmetry_1
O8 Pr1 O1 C8 -70.2(5) 2_666
O7 Pr1 O1 C8 77.0(5) 1_655
O4 Pr1 O1 C8 2.3(5) 2_656
O9 Pr1 O1 C8 -68.3(5) .
O5 Pr1 O1 C8 126.8(5) 2_656
O11 Pr1 O1 C8 -146.0(5) .
N1 Pr1 O1 C8 61.5(5) 2_656
O10 Pr1 O1 C8 178.6(4) .
Pr1 O4 C1 O3 178.0(3) 2_656
Pr1 O4 C1 C2 -2.6(4) 2_656
C6 N1 C2 C3 2.0(5) .
Pr1 N1 C2 C3 176.3(2) 2_656
C6 N1 C2 C1 -178.8(3) .
Pr1 N1 C2 C1 -4.5(4) 2_656
O3 C1 C2 N1 -176.0(3) .
O4 C1 C2 N1 4.6(5) .
O3 C1 C2 C3 3.2(5) .
O4 C1 C2 C3 -176.2(3) .
N1 C2 C3 C4 -1.1(5) .
C1 C2 C3 C4 179.7(3) .
N1 C2 C3 C8 175.1(3) .
C1 C2 C3 C8 -4.1(5) .
C2 C3 C4 C5 -0.1(5) .
C8 C3 C4 C5 -176.4(3) .
C3 C4 C5 C6 0.5(5) .
C3 C4 C5 C9 177.1(3) .
C2 N1 C6 C5 -1.6(5) .
Pr1 N1 C6 C5 -175.8(3) 2_656
C2 N1 C6 C7 178.8(3) .
Pr1 N1 C6 C7 4.6(4) 2_656
C4 C5 C6 N1 0.3(5) .
C9 C5 C6 N1 -176.1(3) .
C4 C5 C6 C7 179.9(3) .
C9 C5 C6 C7 3.5(5) .
Pr1 O5 C7 O6 -168.4(3) 2_656
Pr1 O5 C7 C6 11.9(4) 2_656
N1 C6 C7 O6 170.2(3) .
C5 C6 C7 O6 -9.5(5) .
N1 C6 C7 O5 -10.1(5) .
C5 C6 C7 O5 170.3(3) .
Pr1 O1 C8 O2 170.4(3) .
Pr1 O1 C8 C3 -4.9(7) .
C4 C3 C8 O1 70.2(5) .
C2 C3 C8 O1 -106.0(4) .
C4 C3 C8 O2 -105.5(4) .
C2 C3 C8 O2 78.2(4) .
Pr1 O8 C9 O7 -7.5(6) 2_666
Pr1 O8 C9 C5 169.1(2) 2_666
Pr1 O7 C9 O8 115.8(4) 1_455
Pr1 O7 C9 C5 -60.7(5) 1_455
C6 C5 C9 O8 98.5(4) .
C4 C5 C9 O8 -77.8(4) .
C6 C5 C9 O7 -84.6(4) .
C4 C5 C9 O7 99.0(4) .
