#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/27/2212795.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_2212795
loop_
_publ_author_name
'Guo-Ming Wang'
'Zeng-Xin Li'
'Shu-Yun Xue'
'Chun-Sheng Duan'
_publ_section_title
catena-Poly[[diaqua(isonicotinato-κ²O,O')thulium(III)]-μ-di-μ-isonicotinato-κ⁴O:O']
_journal_coeditor_code           BT2294
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1125
_journal_page_last               m1127
_journal_paper_doi               10.1107/S1600536807012457
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Tm (C6 H4 N O2)3 (H2 O)2]'
_chemical_formula_moiety         'C18 H16 N3 O8 Tm'
_chemical_formula_sum            'C18 H16 N3 O8 Tm'
_chemical_formula_weight         571.27
_chemical_name_systematic
;
catena-Poly[[diaqua(isonicotinato-κ²O,O')thulium(III)]-
μ-di-μ₂-isonicotinato-κ⁴O:O']
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.720(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2130(3)
_cell_length_b                   11.5120(6)
_cell_length_c                   9.7830(2)
_cell_measurement_reflns_used    1991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.46
_cell_volume                     2050.89(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SMART (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siemems SMART 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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7729
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.376
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1991
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0305
_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)+(0.046P)²+1.0135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                1796
_reflns_number_total             1991
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2294.cif
_cod_data_source_block           I
_cod_original_cell_volume        2050.89(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2212795
_cod_database_fobs_code          2212795
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Tm Tm 0.0000 0.48653(2) 0.2500 0.03977(15) Uani d S 1
O O1 0.10387(18) 0.5770(3) -0.0366(4) 0.0556(10) Uani d . 1
O O2 0.0800(2) 0.5266(4) 0.1546(6) 0.0656(13) Uani d . 1
O O3 -0.0497(2) 0.6532(3) 0.0988(5) 0.0775(14) Uani d D 1
H H3B -0.0732 0.6577 0.1509 0.093 Uiso d RD 1
H H3A -0.0711 0.6988 0.0238 0.093 Uiso d RD 1
O O4 -0.03166(19) 0.2994(3) 0.3174(4) 0.0488(9) Uani d . 1
C C1 0.1190(3) 0.5709(4) 0.1005(6) 0.0458(13) Uani d . 1
C C2 0.1907(3) 0.6223(6) 0.2091(6) 0.0556(15) Uani d . 1
C C3 0.2232(4) 0.5906(9) 0.3607(8) 0.091(2) Uani d U 1
H H3 0.2003 0.5373 0.3976 0.110 Uiso calc R 1
C C4 0.2896(5) 0.6387(10) 0.4559(10) 0.123(3) Uani d U 1
H H4 0.3119 0.6140 0.5563 0.147 Uiso calc R 1
C C5 0.2926(5) 0.7462(9) 0.2672(11) 0.108(3) Uani d U 1
H H5 0.3163 0.7995 0.2321 0.130 Uiso calc R 1
C C6 0.2276(4) 0.7006(7) 0.1657(9) 0.079(2) Uani d U 1
H H6 0.2083 0.7238 0.0647 0.094 Uiso calc R 1
C C7 0.0000 0.2469(6) 0.2500 0.0473(18) Uani d S 1
C C8 0.0000 0.1167(7) 0.2500 0.062(3) Uani d S 1
C C9 0.0409(6) 0.0559(7) 0.1926(10) 0.098(3) Uani d . 1
H H9 0.0692 0.0950 0.1535 0.117 Uiso calc R 1
C C10 0.0393(8) -0.0651(10) 0.1939(14) 0.143(5) Uani d . 1
H H10 0.0665 -0.1067 0.1545 0.172 Uiso calc R 1
N N1 0.3234(4) 0.7192(9) 0.4110(10) 0.127(3) Uani d U 1
N N2 0.0000 -0.1214(13) 0.2500 0.142(6) Uani d SU 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'
Tm Tm -0.3139 5.2483 '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
O2 Tm O2 . 2 156.2(2) yes
O2 Tm O1 . 5_565 102.87(16) yes
O2 Tm O1 2 5_565 84.58(16) no
O2 Tm O1 . 6_566 84.58(16) yes
O2 Tm O1 2 6_566 102.87(16) no
O1 Tm O1 5_565 6_566 143.65(19) yes
O2 Tm O3 . 2 84.62(18) yes
O2 Tm O3 2 2 76.09(17) yes
O1 Tm O3 5_565 2 141.57(14) yes
O1 Tm O3 6_566 2 73.92(12) no
O2 Tm O3 . . 76.09(17) no
O2 Tm O3 2 . 84.62(18) no
O1 Tm O3 5_565 . 73.92(12) yes
O1 Tm O3 6_566 . 141.57(14) no
O3 Tm O3 2 . 71.5(2) yes
O2 Tm O4 . . 128.43(14) yes
O2 Tm O4 2 . 75.23(14) yes
O1 Tm O4 5_565 . 74.01(13) yes
O1 Tm O4 6_566 . 73.74(13) yes
O3 Tm O4 2 . 130.01(15) yes
O3 Tm O4 . . 143.39(13) yes
O2 Tm O4 . 2 75.23(14) no
O2 Tm O4 2 2 128.43(14) no
O1 Tm O4 5_565 2 73.74(13) no
O1 Tm O4 6_566 2 74.01(13) no
O3 Tm O4 2 2 143.39(13) no
O3 Tm O4 . 2 130.01(15) no
O4 Tm O4 . 2 54.12(17) no
O2 Tm C7 . . 101.88(12) no
O2 Tm C7 2 . 101.88(12) no
O1 Tm C7 5_565 . 71.83(10) no
O1 Tm C7 6_566 . 71.83(10) no
O3 Tm C7 2 . 144.26(10) no
O3 Tm C7 . . 144.26(10) no
O4 Tm C7 . . 27.06(8) no
O4 Tm C7 2 . 27.06(8) no
O2 Tm H3B . . 95.3 no
O2 Tm H3B 2 . 64.5 no
O1 Tm H3B 5_565 . 74.9 no
O1 Tm H3B 6_566 . 140.5 no
O3 Tm H3B 2 . 66.8 no
O3 Tm H3B . . 20.2 no
O4 Tm H3B . . 130.6 no
O4 Tm H3B 2 . 144.1 no
C7 Tm H3B . . 145.1 no
C1 O1 Tm . 5_565 130.5(3) no
C1 O2 Tm . . 167.2(4) no
Tm O3 H3B . . 82.4 no
Tm O3 H3A . . 163.4 no
H3B O3 H3A . . 106.0 no
C7 O4 Tm . . 91.7(3) no
O2 C1 O1 . . 125.7(5) no
O2 C1 C2 . . 117.5(5) no
O1 C1 C2 . . 116.9(5) no
C6 C2 C3 . . 116.3(6) no
C6 C2 C1 . . 122.5(6) no
C3 C2 C1 . . 121.2(6) no
C4 C3 C2 . . 119.3(8) no
C4 C3 H3 . . 120.4 no
C2 C3 H3 . . 120.4 no
N1 C4 C3 . . 123.1(9) no
N1 C4 H4 . . 118.5 no
C3 C4 H4 . . 118.5 no
N1 C5 C6 . . 123.5(8) no
N1 C5 H5 . . 118.3 no
C6 C5 H5 . . 118.3 no
C2 C6 C5 . . 121.2(8) no
C2 C6 H6 . . 119.4 no
C5 C6 H6 . . 119.4 no
O4 C7 O4 2 . 122.4(7) no
O4 C7 C8 2 . 118.8(3) no
O4 C7 C8 . . 118.8(3) no
O4 C7 Tm 2 . 61.2(3) no
O4 C7 Tm . . 61.2(3) no
C8 C7 Tm . . 180.0 no
C9 C8 C9 2 . 118.8(10) no
C9 C8 C7 2 . 120.6(5) no
C9 C8 C7 . . 120.6(5) no
C8 C9 C10 . . 119.0(9) no
C8 C9 H9 . . 120.5 no
C10 C9 H9 . . 120.5 no
N2 C10 C9 . . 121.1(12) no
N2 C10 H10 . . 119.4 no
C9 C10 H10 . . 119.4 no
C5 N1 C4 . . 116.6(7) no
C10 N2 C10 . 2 120.9(15) no
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
Tm O2 . 2.239(5) yes
Tm O2 2 2.239(5) no
Tm O1 5_565 2.345(3) yes
Tm O1 6_566 2.345(3) no
Tm O3 2 2.364(4) no
Tm O3 . 2.364(4) yes
Tm O4 . 2.419(3) yes
Tm O4 2 2.419(3) no
Tm C7 . 2.759(7) no
Tm H3B . 2.4017 no
O1 C1 . 1.241(6) ?
O1 Tm 5_565 2.345(3) no
O2 C1 . 1.234(7) no
O3 H3B . 0.8369 no
O3 H3A . 0.8520 no
O4 C7 . 1.256(5) no
C1 C2 . 1.498(7) no
C2 C6 . 1.350(9) no
C2 C3 . 1.385(9) no
C3 C4 . 1.375(9) no
C3 H3 . 0.9300 no
C4 N1 . 1.335(12) no
C4 H4 . 0.9300 no
C5 N1 . 1.305(10) no
C5 C6 . 1.362(10) no
C5 H5 . 0.9300 no
C6 H6 . 0.9300 no
C7 O4 2 1.256(5) no
C7 C8 . 1.498(11) no
C8 C9 2 1.375(10) no
C8 C9 . 1.375(10) no
C9 C10 . 1.393(15) no
C9 H9 . 0.9300 no
C10 N2 . 1.316(15) no
C10 H10 . 0.9300 no
N2 C10 2 1.316(15) no
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
O3 H3B O2 2 0.84 2.48 3.100(8) 131.8 yes
O3 H3A N1 8_465 0.85 2.15 2.832(8) 137.2 yes
