#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/32/2233296.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_2233296
loop_
_publ_author_name
'Eshtiagh-Hosseini, H.'
'Mirzaei, M.'
'Mousavinezhad, A.'
'Necas, M.'
'Mague, J. T.'
_publ_section_title
;
 Bis(μ-pyridine-2,3-dicarboxylato)bis[aqua(3-carboxypyridine-2-carboxylato)indium(III)]
 tetrahydrate
;
_journal_coeditor_code           SU2349
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m71
_journal_page_last               m72
_journal_paper_doi               10.1107/S1600536811053566
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[In2 (C7 H3 N O4)2 (C7 H4 N O4)2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C28 H18 In2 N4 O18, 4(H2 O)'
_chemical_formula_sum            'C28 H26 In2 N4 O22'
_chemical_formula_weight         1000.17
_chemical_name_systematic
;
bis(μ-pyridine-2,3-dicarboxylato)bis[aqua(3-carboxypyridine-2-
carboxylato)indium(III)] tetrahydrate
;
_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                110.069(4)
_cell_angle_beta                 96.236(3)
_cell_angle_gamma                109.076(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0166(3)
_cell_length_b                   10.0890(4)
_cell_length_c                   11.9838(5)
_cell_measurement_reflns_used    8569
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1860
_cell_measurement_theta_min      2.8404
_cell_volume                     833.36(7)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_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      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with a Sapphire2
detector
;
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10774
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.6640
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.308
_refine_ls_extinction_coef       0.0083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0155
_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)+(0.0197P)²+0.3217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0389
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                3168
_reflns_number_total             3373
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2349.cif
_cod_data_source_block           I
_cod_original_cell_volume        833.36(6)
_cod_database_code               2233296
_cod_database_fobs_code          2233296
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_symmetry_multiplicity
In In1 0.716069(17) 0.792788(13) 0.730349(10) 0.00941(5) Uani d . 1 1
O O1 0.81082(17) 0.78122(15) 0.57022(11) 0.0132(3) Uani d . 1 1
O O2 0.77166(18) 0.81433(15) 0.39645(11) 0.0165(3) Uani d . 1 1
O O3 0.43118(19) 0.60530(14) 0.22385(11) 0.0154(3) Uani d . 1 1
O O4 0.38691(19) 0.80920(15) 0.21595(11) 0.0179(3) Uani d . 1 1
H H4O 0.3870 0.7721 0.1416 0.021 Uiso d R 1 1
O O5 0.64775(17) 0.86624(14) 0.90207(10) 0.0127(3) Uani d . 1 1
O O6 0.73152(19) 1.05169(15) 1.08983(11) 0.0171(3) Uani d . 1 1
O O7 0.92356(19) 1.40964(15) 1.17662(11) 0.0165(3) Uani d . 1 1
O O8 1.10615(18) 1.31541(14) 1.24362(11) 0.0144(3) Uani d . 1 1
O O9 0.50749(18) 0.56958(14) 0.66940(11) 0.0168(3) Uani d . 1 1
H H91 0.3972 0.5539 0.6473 0.020 Uiso d R 1 1
H H92 0.5325 0.5180 0.7057 0.020 Uiso d R 1 1
N N1 0.5111(2) 0.83155(16) 0.61329(13) 0.0105(3) Uani d . 1 1
N N2 0.9159(2) 1.03454(17) 0.83361(13) 0.0104(3) Uani d . 1 1
C C1 0.5347(2) 0.80161(19) 0.49914(15) 0.0101(4) Uani d . 1 1
C C2 0.4018(3) 0.78340(19) 0.40403(16) 0.0120(4) Uani d . 1 1
C C3 0.2455(3) 0.8044(2) 0.43128(17) 0.0159(4) Uani d . 1 1
H H3 0.1527 0.7938 0.3685 0.019 Uiso calc R 1 1
C C4 0.2254(3) 0.8406(2) 0.54992(17) 0.0165(4) Uani d . 1 1
H H4 0.1209 0.8583 0.5699 0.020 Uiso calc R 1 1
C C5 0.3595(3) 0.8508(2) 0.63908(16) 0.0135(4) Uani d . 1 1
H H5 0.3442 0.8717 0.7200 0.016 Uiso calc R 1 1
C C6 0.7195(2) 0.79807(19) 0.48430(15) 0.0107(4) Uani d . 1 1
C C7 0.4120(3) 0.7255(2) 0.27281(16) 0.0124(4) Uani d . 1 1
C C8 0.9017(3) 1.0999(2) 0.94915(15) 0.0100(3) Uani d . 1 1
C C9 1.0201(3) 1.2475(2) 1.02728(15) 0.0113(4) Uani d . 1 1
C C10 1.1540(3) 1.3289(2) 0.98329(16) 0.0153(4) Uani d . 1 1
H H10 1.2361 1.4305 1.0348 0.018 Uiso calc R 1 1
C C11 1.1667(3) 1.2612(2) 0.86462(16) 0.0158(4) Uani d . 1 1
H H11 1.2570 1.3154 0.8335 0.019 Uiso calc R 1 1
C C12 1.0452(3) 1.1130(2) 0.79220(16) 0.0131(4) Uani d . 1 1
H H12 1.0537 1.0655 0.7107 0.016 Uiso calc R 1 1
C C13 0.7493(3) 1.0014(2) 0.98602(15) 0.0113(4) Uani d . 1 1
C C14 1.0119(3) 1.3270(2) 1.15813(15) 0.0121(4) Uani d . 1 1
O O10 0.39345(18) 0.69562(15) -0.00496(11) 0.0167(3) Uani d . 1 1
H H101 0.4704 0.7512 -0.0293 0.020 Uiso d R 1 1
H H102 0.2944 0.6616 -0.0572 0.020 Uiso d R 1 1
O O11 0.83456(19) 0.48403(16) 0.39983(12) 0.0217(3) Uani d . 1 1
H H111 0.8943 0.5668 0.4609 0.026 Uiso d R 1 1
H H112 0.8849 0.4755 0.3413 0.026 Uiso d R 1 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'
In In -0.7276 1.3100 '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
O8 In1 O1 2_777 . 83.58(5)
O8 In1 O9 2_777 . 84.44(5)
O1 In1 O9 . . 101.63(5)
O8 In1 O5 2_777 . 104.07(5)
O1 In1 O5 . . 165.16(5)
O9 In1 O5 . . 91.87(5)
O8 In1 N2 2_777 . 97.32(5)
O1 In1 N2 . . 91.20(5)
O9 In1 N2 . . 167.17(5)
O5 In1 N2 . . 75.36(5)
O8 In1 N1 2_777 . 153.16(5)
O1 In1 N1 . . 75.34(5)
O9 In1 N1 . . 83.75(5)
O5 In1 N1 . . 100.33(5)
N2 In1 N1 . . 99.52(5)
C6 O1 In1 . . 119.19(11)
C7 O4 H4O . . 112.4
C13 O5 In1 . . 118.93(11)
C14 O8 In1 . 2_777 140.24(11)
In1 O9 H91 . . 121.2
In1 O9 H92 . . 112.4
H91 O9 H92 . . 117.5
C5 N1 C1 . . 120.12(15)
C5 N1 In1 . . 126.80(11)
C1 N1 In1 . . 111.76(11)
C12 N2 C8 . . 119.97(16)
C12 N2 In1 . . 126.11(11)
C8 N2 In1 . . 113.89(12)
N1 C1 C2 . . 121.65(16)
N1 C1 C6 . . 115.19(15)
C2 C1 C6 . . 123.09(15)
C1 C2 C3 . . 118.00(16)
C1 C2 C7 . . 122.31(16)
C3 C2 C7 . . 119.33(16)
C4 C3 C2 . . 119.91(17)
C4 C3 H3 . . 120.0
C2 C3 H3 . . 120.0
C5 C4 C3 . . 119.06(17)
C5 C4 H4 . . 120.5
C3 C4 H4 . . 120.5
N1 C5 C4 . . 121.17(16)
N1 C5 H5 . . 119.4
C4 C5 H5 . . 119.4
O2 C6 O1 . . 125.21(17)
O2 C6 C1 . . 119.13(15)
O1 C6 C1 . . 115.64(14)
O3 C7 O4 . . 124.16(16)
O3 C7 C2 . . 121.80(15)
O4 C7 C2 . . 113.89(15)
N2 C8 C9 . . 121.27(16)
N2 C8 C13 . . 115.55(15)
C9 C8 C13 . . 123.18(15)
C8 C9 C10 . . 118.45(16)
C8 C9 C14 . . 123.82(16)
C10 C9 C14 . . 117.73(16)
C11 C10 C9 . . 119.83(18)
C11 C10 H10 . . 120.1
C9 C10 H10 . . 120.1
C10 C11 C12 . . 118.58(18)
C10 C11 H11 . . 120.7
C12 C11 H11 . . 120.7
N2 C12 C11 . . 121.89(16)
N2 C12 H12 . . 119.1
C11 C12 H12 . . 119.1
O6 C13 O5 . . 124.90(17)
O6 C13 C8 . . 119.05(16)
O5 C13 C8 . . 116.05(14)
O7 C14 O8 . . 123.27(15)
O7 C14 C9 . . 117.88(15)
O8 C14 C9 . . 118.63(15)
H101 O10 H102 . . 105.0
H111 O11 H112 . . 111.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
In1 O8 2_777 2.1153(12)
In1 O1 . 2.1199(12)
In1 O9 . 2.1319(13)
In1 O5 . 2.1324(11)
In1 N2 . 2.2339(15)
In1 N1 . 2.2618(14)
O1 C6 . 1.289(2)
O2 C6 . 1.216(2)
O3 C7 . 1.221(2)
O4 C7 . 1.302(2)
O4 H4O . 0.8401
O5 C13 . 1.300(2)
O6 C13 . 1.216(2)
O7 C14 . 1.240(2)
O8 C14 . 1.268(2)
O8 In1 2_777 2.1152(12)
O9 H91 . 0.8400
O9 H92 . 0.8400
N1 C5 . 1.343(2)
N1 C1 . 1.345(2)
N2 C12 . 1.339(2)
N2 C8 . 1.350(2)
C1 C2 . 1.390(2)
C1 C6 . 1.522(2)
C2 C3 . 1.392(3)
C2 C7 . 1.500(2)
C3 C4 . 1.383(3)
C3 H3 . 0.9500
C4 C5 . 1.383(3)
C4 H4 . 0.9500
C5 H5 . 0.9500
C8 C9 . 1.386(3)
C8 C13 . 1.517(3)
C9 C10 . 1.396(3)
C9 C14 . 1.517(2)
C10 C11 . 1.382(2)
C10 H10 . 0.9500
C11 C12 . 1.383(3)
C11 H11 . 0.9500
C12 H12 . 0.9500
O10 H101 . 0.8400
O10 H102 . 0.8400
O11 H111 . 0.8400
O11 H112 . 0.8400
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
O9 H91 O11 2_666 0.84 1.75 2.5938(19) 178
O9 H92 O3 2_666 0.84 1.80 2.6402(17) 175
O11 H112 O7 1_544 0.84 1.95 2.7595(18) 162
O10 H101 O5 1_554 0.84 1.97 2.8065(18) 175
O10 H102 O7 2_676 0.84 1.88 2.7237(19) 178
O4 H4O O10 . 0.84 1.67 2.5124(17) 178
C4 H4 O1 1_455 0.95 2.35 3.231(2) 154
C5 H5 O6 2_677 0.95 2.36 3.293(2) 168
C11 H11 O3 2_776 0.95 2.61 3.495(2) 156
C12 H12 O2 2_776 0.95 2.33 2.993(2) 126
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
O8 In1 O1 C6 2_777 162.67(13)
O9 In1 O1 C6 . 79.72(13)
O5 In1 O1 C6 . -75.3(2)
N2 In1 O1 C6 . -100.10(13)
N1 In1 O1 C6 . -0.57(12)
O8 In1 O5 C13 2_777 89.72(12)
O1 In1 O5 C13 . -30.0(2)
O9 In1 O5 C13 . 174.45(12)
N2 In1 O5 C13 . -4.31(11)
N1 In1 O5 C13 . -101.56(12)
O8 In1 N1 C5 2_777 138.04(14)
O1 In1 N1 C5 . 177.42(15)
O9 In1 N1 C5 . 73.64(15)
O5 In1 N1 C5 . -17.12(15)
N2 In1 N1 C5 . -93.83(15)
O8 In1 N1 C1 2_777 -28.73(19)
O1 In1 N1 C1 . 10.65(11)
O9 In1 N1 C1 . -93.12(12)
O5 In1 N1 C1 . 176.11(12)
N2 In1 N1 C1 . 99.40(12)
O8 In1 N2 C12 2_777 78.74(14)
O1 In1 N2 C12 . -4.94(14)
O9 In1 N2 C12 . 175.85(19)
O5 In1 N2 C12 . -178.56(15)
N1 In1 N2 C12 . -80.27(14)
O8 In1 N2 C8 2_777 -99.18(12)
O1 In1 N2 C8 . 177.14(12)
O9 In1 N2 C8 . -2.1(3)
O5 In1 N2 C8 . 3.52(11)
N1 In1 N2 C8 . 101.80(12)
C5 N1 C1 C2 . -2.7(3)
In1 N1 C1 C2 . 165.07(13)
C5 N1 C1 C6 . 174.13(15)
In1 N1 C1 C6 . -18.10(17)
N1 C1 C2 C3 . 3.0(3)
C6 C1 C2 C3 . -173.52(16)
N1 C1 C2 C7 . -169.95(16)
C6 C1 C2 C7 . 13.5(3)
C1 C2 C3 C4 . -0.7(3)
C7 C2 C3 C4 . 172.56(17)
C2 C3 C4 C5 . -2.0(3)
C1 N1 C5 C4 . -0.1(3)
In1 N1 C5 C4 . -165.89(13)
C3 C4 C5 N1 . 2.5(3)
In1 O1 C6 O2 . 169.57(14)
In1 O1 C6 C1 . -8.69(19)
N1 C1 C6 O2 . -159.83(16)
C2 C1 C6 O2 . 16.9(3)
N1 C1 C6 O1 . 18.5(2)
C2 C1 C6 O1 . -164.68(16)
C1 C2 C7 O3 . 53.6(3)
C3 C2 C7 O3 . -119.3(2)
C1 C2 C7 O4 . -130.59(18)
C3 C2 C7 O4 . 56.5(2)
C12 N2 C8 C9 . -0.6(2)
In1 N2 C8 C9 . 177.46(12)
C12 N2 C8 C13 . 179.38(15)
In1 N2 C8 C13 . -2.56(18)
N2 C8 C9 C10 . 0.9(2)
C13 C8 C9 C10 . -179.06(16)
N2 C8 C9 C14 . -179.73(16)
C13 C8 C9 C14 . 0.3(3)
C8 C9 C10 C11 . -0.5(3)
C14 C9 C10 C11 . -179.94(16)
C9 C10 C11 C12 . -0.1(3)
C8 N2 C12 C11 . -0.1(3)
In1 N2 C12 C11 . -177.90(13)
C10 C11 C12 N2 . 0.4(3)
In1 O5 C13 O6 . -174.77(13)
In1 O5 C13 C8 . 4.34(18)
N2 C8 C13 O6 . 178.18(15)
C9 C8 C13 O6 . -1.8(3)
N2 C8 C13 O5 . -1.0(2)
C9 C8 C13 O5 . 179.00(15)
In1 O8 C14 O7 2_777 -176.98(13)
In1 O8 C14 C9 2_777 -2.6(3)
C8 C9 C14 O7 . -93.8(2)
C10 C9 C14 O7 . 85.6(2)
C8 C9 C14 O8 . 91.5(2)
C10 C9 C14 O8 . -89.1(2)
