#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/91/2019169.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_2019169
loop_
_publ_author_name
'Xiong, Wei-Lu'
'Wang, Yu-Ling'
'Liu, Qing-Yan'
_publ_section_title
;
 A three-dimensional polymeric potassium complex of
 5-sulfonobenzene-1,2,4-tricarboxylic acid:
 poly[μ-aqua-aqua-μ₉-(2,4-dicarboxy-5-sulfonatobenzoato)-dipotassium(I)]
;
_journal_coeditor_code           EM3061
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1132
_journal_page_last               1135
_journal_paper_doi               10.1107/S0108270113024499
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[K2 (C9 H4 O9 S) (H2 O)2]'
_chemical_formula_moiety         'C9 H8 K2 O11 S'
_chemical_formula_sum            'C9 H8 K2 O11 S'
_chemical_formula_weight         402.41
_chemical_name_systematic
;
Poly[μ-aqua-aqua-μ₉-(2,4-dicarboxy-5-sulfonatobenzoato)-dipotassium(I)]
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.7740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4108(6)
_cell_length_b                   7.1795(4)
_cell_length_c                   16.9372(9)
_cell_measurement_reflns_used    6780
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.42
_cell_volume                     1380.52(13)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12572
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.8134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.513
_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     208
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0323
_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)+(0.0544P)²+0.9006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                3056
_reflns_number_total             3411
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            em3061.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019169
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_symmetry_multiplicity
K K1 0.63078(4) 0.34215(8) 0.16439(3) 0.04418(14) Uani d . 1 1
K K2 0.41486(4) -0.15869(5) 0.08872(3) 0.03350(12) Uani d . 1 1
S S1 0.36844(3) 0.36730(5) 0.04779(2) 0.02366(11) Uani d . 1 1
O O1 -0.03680(11) 0.2982(2) -0.10471(7) 0.0360(3) Uani d . 1 1
O O2 -0.17489(11) 0.1925(2) -0.03608(8) 0.0367(3) Uani d . 1 1
O O3 -0.20614(11) 0.1063(2) 0.09568(8) 0.0416(4) Uani d D 1 1
H H3 -0.191(3) 0.139(4) 0.0471(12) 0.062 Uiso d D 1 1
O O4 -0.10690(13) 0.0685(3) 0.21101(8) 0.0519(4) Uani d . 1 1
O O5 0.28766(12) 0.2558(2) 0.28376(7) 0.0374(3) Uani d D 1 1
H H5 0.3474(18) 0.239(4) 0.3156(14) 0.056 Uiso d D 1 1
O O6 0.40340(11) 0.1135(2) 0.20402(8) 0.0346(3) Uani d . 1 1
O O7 0.41622(11) 0.47421(18) 0.11643(8) 0.0332(3) Uani d . 1 1
O O8 0.34166(12) 0.4809(2) -0.02206(8) 0.0400(3) Uani d . 1 1
O O9 0.43865(11) 0.20320(18) 0.03397(8) 0.0324(3) Uani d . 1 1
O O10 0.84463(15) 0.5745(3) 0.19595(11) 0.0579(5) Uani d D 1 1
H H10A 0.871(3) 0.513(4) 0.2340(16) 0.087 Uiso d D 1 1
H H10B 0.904(2) 0.610(5) 0.174(2) 0.087 Uiso d D 1 1
O O11 0.63800(17) -0.1472(3) 0.16637(12) 0.0550(4) Uani d D 1 1
H H11A 0.670(3) -0.237(4) 0.185(2) 0.083 Uiso d D 1 1
H H11B 0.684(3) -0.105(5) 0.1364(18) 0.083 Uiso d D 1 1
C C1 0.02142(13) 0.2350(2) 0.03132(9) 0.0197(3) Uani d . 1 1
C C2 0.00396(13) 0.1757(2) 0.10903(9) 0.0206(3) Uani d . 1 1
C C3 0.10096(14) 0.1725(2) 0.16637(9) 0.0226(3) Uani d . 1 1
H H3A 0.0894 0.1364 0.2178 0.027 Uiso calc R 1 1
C C4 0.21371(13) 0.2209(2) 0.15000(9) 0.0206(3) Uani d . 1 1
C C5 0.23002(13) 0.2838(2) 0.07363(9) 0.0200(3) Uani d . 1 1
C C6 0.13433(13) 0.2908(2) 0.01662(9) 0.0215(3) Uani d . 1 1
H H6 0.1458 0.3346 -0.0337 0.026 Uiso calc R 1 1
C C7 -0.06914(14) 0.2442(2) -0.04115(9) 0.0228(3) Uani d . 1 1
C C8 -0.10917(14) 0.1118(3) 0.14150(10) 0.0271(3) Uani d . 1 1
C C9 0.31274(14) 0.1926(2) 0.21464(9) 0.0234(3) Uani d . 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O7 K1 O4 . 2 82.11(4)
O7 K1 O8 . 3_665 75.74(4)
O4 K1 O8 2 3_665 115.68(6)
O7 K1 O3 . 1_655 134.59(4)
O4 K1 O3 2 1_655 142.99(5)
O8 K1 O3 3_665 1_655 77.36(4)
O7 K1 O10 . . 124.61(5)
O4 K1 O10 2 . 70.47(6)
O8 K1 O10 3_665 . 74.63(5)
O3 K1 O10 1_655 . 81.27(5)
O7 K1 O10 . 2_645 118.08(5)
O4 K1 O10 2 2_645 77.34(6)
O8 K1 O10 3_665 2_645 163.26(5)
O3 K1 O10 1_655 2_645 85.94(5)
O10 K1 O10 . 2_645 101.88(3)
O7 K1 O9 . . 48.76(4)
O4 K1 O9 2 . 128.90(4)
O8 K1 O9 3_665 . 70.33(4)
O3 K1 O9 1_655 . 87.82(4)
O10 K1 O9 . . 144.79(4)
O10 K1 O9 2_645 . 110.65(5)
O7 K1 O6 . . 60.56(4)
O4 K1 O6 2 . 89.84(5)
O8 K1 O6 3_665 . 125.70(4)
O3 K1 O6 1_655 . 110.95(4)
O10 K1 O6 . . 157.36(5)
O10 K1 O6 2_645 . 61.66(4)
O9 K1 O6 . . 57.08(3)
O7 K2 O11 1_545 . 87.52(5)
O7 K2 O6 1_545 . 124.73(4)
O11 K2 O6 . . 75.47(5)
O7 K2 O9 1_545 . 168.30(4)
O11 K2 O9 . . 90.85(5)
O6 K2 O9 . . 65.79(4)
O7 K2 O2 1_545 3 87.63(4)
O11 K2 O2 . 3 169.56(5)
O6 K2 O2 . 3 99.85(4)
O9 K2 O2 . 3 95.73(4)
O7 K2 O9 1_545 3_655 91.39(4)
O11 K2 O9 . 3_655 76.47(5)
O6 K2 O9 . 3_655 132.33(4)
O9 K2 O9 . 3_655 76.97(4)
O2 K2 O9 3 3_655 112.90(4)
O7 K2 O8 1_545 1_545 46.77(4)
O11 K2 O8 . 1_545 118.12(5)
O6 K2 O8 . 1_545 159.68(4)
O9 K2 O8 . 1_545 125.33(4)
O2 K2 O8 3 1_545 64.03(4)
O9 K2 O8 3_655 1_545 67.73(4)
O7 K2 O5 1_545 2_545 72.59(4)
O11 K2 O5 . 2_545 111.13(5)
O6 K2 O5 . 2_545 66.04(4)
O9 K2 O5 . 2_545 118.66(4)
O2 K2 O5 3 2_545 58.53(3)
O9 K2 O5 3_655 2_545 161.48(4)
O8 K2 O5 1_545 2_545 94.11(4)
O8 S1 O7 . . 112.88(9)
O8 S1 O9 . . 113.54(9)
O7 S1 O9 . . 112.81(8)
O8 S1 C5 . . 105.72(7)
O7 S1 C5 . . 104.56(7)
O9 S1 C5 . . 106.41(7)
C7 O2 K2 . 3 154.89(11)
C8 O3 K1 . 1_455 107.01(11)
C8 O3 H3 . . 108(2)
K1 O3 H3 1_455 . 114.7(19)
C8 O4 K1 . 2_545 156.56(16)
C9 O5 K2 . 2 149.09(10)
C9 O5 H5 . . 106.8(19)
K2 O5 H5 2 . 100.4(19)
C9 O6 K2 . . 122.48(11)
C9 O6 K1 . . 120.93(12)
K2 O6 K1 . . 96.73(4)
S1 O7 K1 . . 108.31(7)
S1 O7 K2 . 1_565 112.63(7)
K1 O7 K2 . 1_565 113.03(5)
S1 O8 K1 . 3_665 159.82(8)
S1 O8 K2 . 1_565 87.46(7)
K1 O8 K2 3_665 1_565 95.27(4)
S1 O9 K2 . . 128.91(7)
S1 O9 K2 . 3_655 126.00(7)
K2 O9 K2 . 3_655 103.03(4)
S1 O9 K1 . . 89.21(6)
K2 O9 K1 . . 98.51(4)
K2 O9 K1 3_655 . 97.59(4)
K1 O10 K1 . 2_655 120.46(6)
K1 O10 H10A . . 94(3)
K1 O10 H10A 2_655 . 74(3)
K1 O10 H10B . . 141(3)
K1 O10 H10B 2_655 . 98(3)
H10A O10 H10B . . 105(3)
K2 O11 H11A . . 122(3)
K2 O11 H11B . . 109(3)
H11A O11 H11B . . 104(4)
C6 C1 C2 . . 118.09(13)
C6 C1 C7 . . 114.04(13)
C2 C1 C7 . . 127.87(13)
C3 C2 C1 . . 118.37(13)
C3 C2 C8 . . 112.62(13)
C1 C2 C8 . . 129.00(14)
C4 C3 C2 . . 122.86(14)
C4 C3 H3A . . 118.6
C2 C3 H3A . . 118.6
C3 C4 C5 . . 118.53(13)
C3 C4 C9 . . 117.65(13)
C5 C4 C9 . . 123.74(13)
C6 C5 C4 . . 119.17(13)
C6 C5 S1 . . 118.20(11)
C4 C5 S1 . . 122.55(11)
C5 C6 C1 . . 122.89(14)
C5 C6 H6 . . 118.6
C1 C6 H6 . . 118.6
O1 C7 O2 . . 121.23(14)
O1 C7 C1 . . 118.53(14)
O2 C7 C1 . . 120.22(14)
O4 C8 O3 . . 120.63(16)
O4 C8 C2 . . 119.37(15)
O3 C8 C2 . . 120.00(14)
O6 C9 O5 . . 124.13(15)
O6 C9 C4 . . 123.08(14)
O5 C9 C4 . . 112.73(13)
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
K1 O7 . 2.6745(14) yes
K1 O4 2 2.6990(16) yes
K1 O8 3_665 2.7708(13) yes
K1 O3 1_655 2.8496(16) yes
K1 O10 . 2.960(2) yes
K1 O10 2_645 3.039(2) yes
K1 O9 . 3.1156(15) yes
K1 O6 . 3.1981(15) yes
K2 O7 1_545 2.6768(14) yes
K2 O11 . 2.747(2) yes
K2 O6 . 2.7749(14) yes
K2 O9 . 2.7811(14) yes
K2 O2 3 2.8037(13) yes
K2 O9 3_655 2.8130(13) yes
K2 O8 1_545 3.2558(17) yes
K2 O5 2_545 3.3744(14) yes
S1 O8 . 1.4440(13) ?
S1 O7 . 1.4527(13) ?
S1 O9 . 1.4570(13) ?
S1 C5 . 1.7845(15) ?
O1 C7 . 1.235(2) ?
O2 C7 . 1.274(2) ?
O2 K2 3 2.8037(13) ?
O3 C8 . 1.287(2) ?
O3 K1 1_455 2.8496(16) ?
O3 H3 . 0.890(17) ?
O4 C8 . 1.215(2) ?
O4 K1 2_545 2.6990(16) ?
O5 C9 . 1.313(2) ?
O5 K2 2 3.3744(14) ?
O5 H5 . 0.835(17) ?
O6 C9 . 1.210(2) ?
O7 K2 1_565 2.6768(14) ?
O8 K1 3_665 2.7708(13) ?
O8 K2 1_565 3.2558(17) ?
O9 K2 3_655 2.8130(13) ?
O10 K1 2_655 3.039(2) ?
O10 H10A . 0.815(18) ?
O10 H10B . 0.842(18) ?
O11 H11A . 0.788(18) ?
O11 H11B . 0.823(18) ?
C1 C6 . 1.395(2) ?
C1 C2 . 1.416(2) ?
C1 C7 . 1.524(2) ?
C2 C3 . 1.397(2) ?
C2 C8 . 1.524(2) ?
C3 C4 . 1.387(2) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.400(2) ?
C4 C9 . 1.506(2) ?
C5 C6 . 1.384(2) ?
C6 H6 . 0.9300 ?
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 H3 O2 . 0.890(17) 1.489(18) 2.3771(19) 176(3) yes
O5 H5 O1 4_666 0.835(17) 1.811(18) 2.6400(18) 172(3) yes
O10 H10A O11 2_655 0.815(18) 2.05(2) 2.814(3) 155(3) yes
O10 H10B O1 3_665 0.842(18) 2.116(19) 2.952(2) 172(3) yes
O11 H11A O4 2_545 0.788(18) 2.42(3) 2.958(3) 127(3) yes
O11 H11B O3 1_655 0.823(18) 2.13(2) 2.888(2) 154(4) yes
