#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/48/2214841.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_2214841
loop_
_publ_author_name
'Hao, Lu-Jiang'
'Yu, Tong-Li'
_publ_section_title
;catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)terbium(III)]-μ-pyridine-2,6-dicarboxylato]
 tetrahydrate]
;
_journal_coeditor_code           RK2026
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2182
_journal_page_last               m2183
_journal_paper_doi               10.1107/S1600536807034629
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Tb (C7 H3 N O4) (C7 H4 N O4) (H2 O)2] , 4H2 O'
_chemical_formula_moiety         'C14 H11 N2 O10 Tb , 4H2 O'
_chemical_formula_sum            'C14 H19 N2 O14 Tb'
_chemical_formula_weight         598.24
_chemical_name_systematic
;
catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)terbium(III)]-μ-
pyridine-2,6-dicarboxylato] tetrahydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.0126(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9986(3)
_cell_length_b                   11.3819(2)
_cell_length_c                   12.8982(2)
_cell_measurement_reflns_used    3499
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      1.47
_cell_volume                     2010.08(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, Year?)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7168
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.595
_exptl_absorpt_correction_T_max  0.7150
_exptl_absorpt_correction_T_min  0.7150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.202
_refine_diff_density_min         -2.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0953P)²+13.066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                3237
_reflns_number_total             3499
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rk2026.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214841
_cod_database_fobs_code          2214841
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
C C1 0.5673(6) 0.5764(8) 0.8725(7) 0.0353(9) Uani d U 1
C C2 0.5029(6) 0.6849(8) 0.8698(7) 0.0358(8) Uani d U 1
C C3 0.4056(6) 0.6786(8) 0.8673(7) 0.0363(8) Uani d U 1
H H3 0.3749 0.6062 0.8679 0.044 Uiso calc R 1
C C4 0.3521(7) 0.7840(7) 0.8636(8) 0.0369(8) Uani d U 1
H H4A 0.2852 0.7815 0.8610 0.044 Uiso calc R 1
C C5 0.3989(6) 0.8910(8) 0.8638(7) 0.0364(8) Uani d U 1
H H5 0.3648 0.9614 0.8617 0.044 Uiso calc R 1
C C6 0.4975(6) 0.8894(8) 0.8671(7) 0.0360(8) Uani d U 1
C C7 0.5573(6) 0.9998(8) 0.8682(7) 0.0358(9) Uani d U 1
C C8 0.8806(5) 1.0253(6) 0.8263(5) 0.0179(7) Uani d U 1
C C9 0.8732(5) 1.0388(6) 0.9408(5) 0.0176(6) Uani d U 1
C C10 0.9082(5) 1.1397(6) 1.0001(5) 0.0180(6) Uani d U 1
H H10 0.9344 1.2028 0.9696 0.022 Uiso calc R 1
C C11 0.9018(5) 1.1406(6) 1.1065(5) 0.0182(6) Uani d U 1
H H11 0.9247 1.2050 1.1488 0.022 Uiso calc R 1
C C12 0.8619(5) 1.0469(6) 1.1489(5) 0.0178(6) Uani d U 1
H H12 0.8585 1.0464 1.2201 0.021 Uiso calc R 1
C C13 0.8264(5) 0.9519(6) 1.0829(5) 0.0175(6) Uani d U 1
C C14 0.7743(5) 0.8473(6) 1.1189(5) 0.0173(7) Uani d U 1
H H1W 0.909(4) 0.718(4) 0.987(5) 0.080 Uiso d D 1
H H2W 0.863(3) 0.612(4) 0.952(8) 0.080 Uiso d D 1
H H3W 0.595(6) 0.899(7) 0.672(3) 0.080 Uiso d D 1
H H4W 0.665(8) 0.841(10) 0.629(6) 0.080 Uiso d D 1
H H5W 0.924(8) 0.676(10) 0.190(8) 0.080 Uiso d D 1
H H6W 0.988(9) 0.753(7) 0.158(9) 0.080 Uiso d D 1
H H7W 0.788(10) 0.465(5) 0.888(8) 0.080 Uiso d D 1
H H8W 0.791(12) 0.397(10) 0.977(5) 0.080 Uiso d D 1
H H9W 0.023(10) 0.4869(17) 0.898(8) 0.080 Uiso d D 1
H H10W 0.038(10) 0.589(8) 0.847(5) 0.080 Uiso d D 1
H H11W 0.608(9) 0.300(12) 0.826(4) 0.080 Uiso d D 1
H H12W 0.674(6) 0.238(11) 0.899(9) 0.080 Uiso d D 1
N N1 0.5474(5) 0.7881(5) 0.8674(5) 0.0201(13) Uani d . 1
N N2 0.8315(4) 0.9488(4) 0.9813(4) 0.0111(10) Uani d . 1
O O1 0.5308(4) 0.4780(5) 0.8764(5) 0.0400(15) Uani d . 1
O O2 0.6558(4) 0.5971(4) 0.8704(4) 0.0227(10) Uani d . 1
O O3 0.6432(4) 0.9921(4) 0.8649(4) 0.0257(11) Uani d . 1
O O4 0.5122(5) 1.0991(5) 0.8733(6) 0.0464(16) Uani d . 1
H H4 0.5471 1.1535 0.8619 0.070 Uiso calc R 1
O O5 0.8754(4) 0.6841(5) 0.9368(4) 0.0255(11) Uani d D 1
O O6 0.6333(4) 0.8452(6) 0.6743(4) 0.0372(15) Uani d D 1
O O7 0.8449(4) 0.9295(4) 0.7819(3) 0.0224(10) Uani d . 1
O O8 0.9207(4) 1.1044(5) 0.7853(4) 0.0303(12) Uani d . 1
O O9 0.7268(4) 0.7815(4) 1.0468(4) 0.0175(10) Uani d . 1
O O10 0.7813(4) 0.8336(4) 1.2163(3) 0.0200(10) Uani d . 1
O O11 0.9581(4) 0.6919(5) 0.1491(4) 0.0251(12) Uani d D 1
O O12 0.7991(8) 0.4014(7) 0.9163(9) 0.086(3) Uani d D 1
O O13 0.6236(7) 0.2750(8) 0.8855(10) 0.082(3) Uani d D 1
O O14 0.0299(5) 0.5576(5) 0.9011(4) 0.0338(13) Uani d D 1
Tb Tb1 0.73015(2) 0.79481(3) 0.85156(2) 0.01780(18) Uani 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'
Tb Tb -0.1723 4.1537 '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
O1 C1 O2 . . 125.7(8)
O1 C1 C2 . . 119.1(7)
O2 C1 C2 . . 115.2(7)
N1 C2 C3 . . 121.1(8)
N1 C2 C1 . . 116.0(7)
C3 C2 C1 . . 122.9(8)
C2 C3 C4 . . 118.7(9)
C2 C3 H3 . . 120.6
C4 C3 H3 . . 120.7
C5 C4 C3 . . 120.1(9)
C5 C4 H4A . . 120.0
C3 C4 H4A . . 120.0
C6 C5 C4 . . 117.5(8)
C6 C5 H5 . . 121.3
C4 C5 H5 . . 121.2
N1 C6 C5 . . 121.9(8)
N1 C6 C7 . . 115.3(7)
C5 C6 C7 . . 122.8(8)
O3 C7 O4 . . 123.9(8)
O3 C7 C6 . . 119.4(7)
O4 C7 C6 . . 116.7(7)
O8 C8 O7 . . 126.7(6)
O8 C8 C9 . . 118.3(6)
O7 C8 C9 . . 115.0(6)
N2 C9 C10 . . 122.9(6)
N2 C9 C8 . . 115.4(5)
C10 C9 C8 . . 121.8(6)
C11 C10 C9 . . 117.0(6)
C11 C10 H10 . . 121.5
C9 C10 H10 . . 121.5
C12 C11 C10 . . 120.2(6)
C12 C11 H11 . . 119.9
C10 C11 H11 . . 119.9
C11 C12 C13 . . 118.8(6)
C11 C12 H12 . . 120.6
C13 C12 H12 . . 120.6
N2 C13 C12 . . 122.3(6)
N2 C13 C14 . . 114.2(5)
C12 C13 C14 . . 123.4(6)
O10 C14 O9 . . 125.7(6)
O10 C14 C13 . . 117.6(6)
O9 C14 C13 . . 116.7(6)
C2 N1 C6 . . 120.7(7)
C2 N1 Tb1 . . 119.8(5)
C6 N1 Tb1 . . 119.3(5)
C13 N2 C9 . . 118.9(5)
C13 N2 Tb1 . . 120.9(4)
C9 N2 Tb1 . . 119.0(4)
C1 O2 Tb1 . . 126.5(5)
C7 O3 Tb1 . . 123.3(5)
C7 O4 H4 . . 109.5
Tb1 O5 H1W . . 114(3)
Tb1 O5 H2W . . 114(3)
H1W O5 H2W . . 112(7)
Tb1 O6 H3W . . 116(3)
Tb1 O6 H4W . . 112(8)
H3W O6 H4W . . 119(9)
C8 O7 Tb1 . . 125.2(4)
C14 O9 Tb1 . . 125.3(4)
C14 O10 Tb1 . 4_576 143.4(4)
H5W O11 H6W . . 118(11)
H7W O12 H8W . . 116(11)
H11W O13 H12W . . 116(12)
H9W O14 H10W . . 116(10)
O5 Tb1 O6 . . 141.19(17)
O5 Tb1 O10 . 4_575 71.34(16)
O6 Tb1 O10 . 4_575 70.77(16)
O5 Tb1 O2 . . 79.49(18)
O6 Tb1 O2 . . 98.0(2)
O10 Tb1 O2 4_575 . 74.20(16)
O5 Tb1 O7 . . 86.65(18)
O6 Tb1 O7 . . 78.3(2)
O10 Tb1 O7 4_575 . 79.02(16)
O2 Tb1 O7 . . 152.60(16)
O5 Tb1 O9 . . 73.05(17)
O6 Tb1 O9 . . 144.46(17)
O10 Tb1 O9 4_575 . 136.75(15)
O2 Tb1 O9 . . 75.91(15)
O7 Tb1 O9 . . 122.43(14)
O5 Tb1 O3 . . 141.05(17)
O6 Tb1 O3 . . 71.56(17)
O10 Tb1 O3 4_575 . 140.01(16)
O2 Tb1 O3 . . 124.28(17)
O7 Tb1 O3 . . 80.72(16)
O9 Tb1 O3 . . 83.04(16)
O5 Tb1 N1 . . 133.26(18)
O6 Tb1 N1 . . 73.8(2)
O10 Tb1 N1 4_575 . 117.83(17)
O2 Tb1 N1 . . 62.20(16)
O7 Tb1 N1 . . 139.00(17)
O9 Tb1 N1 . . 72.47(17)
O3 Tb1 N1 . . 62.35(17)
O5 Tb1 N2 . . 76.67(17)
O6 Tb1 N2 . . 123.7(2)
O10 Tb1 N2 4_575 . 129.89(16)
O2 Tb1 N2 . . 135.72(16)
O7 Tb1 N2 . . 61.35(15)
O9 Tb1 N2 . . 61.70(14)
O3 Tb1 N2 . . 64.91(16)
N1 Tb1 N2 . . 112.22(16)
O5 Tb1 H2W . . 15.9(5)
O6 Tb1 H2W . . 139(2)
O10 Tb1 H2W 4_575 . 69(2)
O2 Tb1 H2W . . 63.6(5)
O7 Tb1 H2W . . 101.4(7)
O9 Tb1 H2W . . 70(2)
O3 Tb1 H2W . . 149(2)
N1 Tb1 H2W . . 119.4(9)
N2 Tb1 H2W . . 89.0(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O1 . 1.237(10)
C1 O2 . 1.267(10)
C1 C2 . 1.525(11)
C2 N1 . 1.332(11)
C2 C3 . 1.358(12)
C3 C4 . 1.410(12)
C3 H3 . 0.9300
C4 C5 . 1.382(13)
C4 H4A . 0.9300
C5 C6 . 1.373(11)
C5 H5 . 0.9300
C6 N1 . 1.347(10)
C6 C7 . 1.509(12)
C7 O3 . 1.214(10)
C7 O4 . 1.303(10)
C8 O8 . 1.237(8)
C8 O7 . 1.284(8)
C8 C9 . 1.510(9)
C9 N2 . 1.337(8)
C9 C10 . 1.410(9)
C10 C11 . 1.393(9)
C10 H10 . 0.9300
C11 C12 . 1.369(9)
C11 H11 . 0.9300
C12 C13 . 1.403(9)
C12 H12 . 0.9300
C13 N2 . 1.328(8)
C13 C14 . 1.518(9)
C14 O10 . 1.249(8)
C14 O9 . 1.269(8)
N1 Tb1 . 2.610(6)
N2 Tb1 . 2.626(5)
O2 Tb1 . 2.512(5)
O3 Tb1 . 2.578(5)
O4 H4 . 0.8200
O5 Tb1 . 2.449(5)
O5 H1W . 0.81(6)
O5 H2W . 0.87(5)
O6 Tb1 . 2.470(5)
O6 H3W . 0.81(8)
O6 H4W . 0.81(10)
O7 Tb1 . 2.517(5)
O9 Tb1 . 2.533(5)
O10 Tb1 4_576 2.493(4)
O11 H5W . 0.80(11)
O11 H6W . 0.81(10)
O12 H7W . 0.81(7)
O12 H8W . 0.82(7)
O13 H11W . 0.81(8)
O13 H12W . 0.81(10)
O14 H9W . 0.810(12)
O14 H10W . 0.81(9)
Tb1 O10 4_575 2.493(4)
Tb1 H2W . 2.91(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
O5 H1W O11 1_556 0.81(6) 2.08(5) 2.743(7) 138(7)
O6 H3W O1 2_656 0.81(8) 1.97(4) 2.714(7) 154(9)
O6 H4W O9 4_575 0.81(10) 2.05(7) 2.719(7) 140(11)
O11 H5W O7 4_575 0.80(11) 2.15(11) 2.913(7) 159(11)
O11 H6W O8 3_776 0.81(10) 2.10(10) 2.893(7) 167(13)
O14 H9W O11 3_666 0.810(12) 2.15(4) 2.926(8) 159(11)
O14 H10W O8 2_646 0.81(9) 1.92(9) 2.690(7) 157(11)
O4 H4 O13 1_565 0.82 1.74 2.522(12) 159.7
