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#$Date: 2022-09-21 12:21:21 +0300 (Wed, 21 Sep 2022) $
#$Revision: 278034 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/58/8105820.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_8105820
loop_
_publ_author_name
'Xi-Shi, Tai'
'Li-Li, Liu'
'Xiao-Jing, Zhou'
_publ_section_title
;
 The crystal structure of
 poly[m2-aqua-tetraaqua-bis(m9-4-formylbenzene-1,3-disulfonato)tetrasodium(I)
 hydrate, C14H18O19S4Na4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              685
_journal_page_last               686
_journal_paper_doi               10.1515/ncrs-2019-0035
_journal_volume                  234
_journal_year                    2019
_chemical_formula_sum            'C14 H18 Na4 O19 S4'
_chemical_formula_weight         710.48
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.14(3)
_cell_angle_beta                 90.46(3)
_cell_angle_gamma                106.53(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0769(14)
_cell_length_b                   9.5622(19)
_cell_length_c                   10.952(2)
_cell_measurement_reflns_used    2128
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7843
_cell_measurement_theta_min      2.2234
_cell_volume                     636.1(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  bruker-CCD
_diffrn_measurement_method       'phi and omega 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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4997
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9057
_exptl_absorpt_correction_T_min  0.8965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0759P)²+0.6411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                2128
_reflns_number_total             2246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2019-0035_suppl.cif
_cod_data_source_block           ww
_cod_original_cell_volume        636.1(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C14 H18 Na4 O19 S4 '
_cod_database_code               8105820
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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.07669(8) -0.68903(6) 0.29435(5) 0.0184(2) Uani 1 1 d . . .
S2 S -0.24073(8) -1.33612(6) 0.16300(6) 0.0183(2) Uani 1 1 d . . .
Na1 Na -0.25680(16) -0.35031(14) 0.43253(11) 0.0348(3) Uani 1 1 d . . .
Na2 Na -0.22474(15) -1.62759(12) -0.19927(10) 0.0272(3) Uani 1 1 d . . .
C1 C -0.1633(3) -0.8975(3) 0.1675(2) 0.0177(5) Uani 1 1 d . . .
C2 C -0.1629(3) -1.0170(3) 0.2079(2) 0.0189(5) Uani 1 1 d . . .
H2A H -0.1132 -0.9882 0.2971 0.023 Uiso 1 1 calc R . .
C3 C -0.2380(3) -1.1805(3) 0.1132(2) 0.0176(5) Uani 1 1 d . . .
C4 C -0.3142(3) -1.2257(3) -0.0199(2) 0.0205(5) Uani 1 1 d . . .
H4A H -0.3679 -1.3352 -0.0814 0.025 Uiso 1 1 calc R . .
C5 C -0.3094(3) -1.1060(3) -0.0602(2) 0.0204(5) Uani 1 1 d . . .
H5A H -0.3574 -1.1357 -0.1500 0.024 Uiso 1 1 calc R . .
C6 C -0.2332(3) -0.9409(3) 0.0321(2) 0.0182(5) Uani 1 1 d . . .
C7 C -0.2353(4) -0.8193(3) -0.0177(2) 0.0237(5) Uani 1 1 d . . .
H7A H -0.2005 -0.7103 0.0457 0.028 Uiso 1 1 calc R . .
O1 O -0.0144(3) -0.6955(2) 0.41816(17) 0.0285(4) Uani 1 1 d . . .
O1W O -0.2952(3) -0.0887(3) 0.5752(2) 0.0432(5) Uani 1 1 d . . .
H1WB H -0.2919 -0.0486 0.6619 0.065 Uiso 1 1 d R . .
H1WA H -0.2786 -0.0083 0.5559 0.065 Uiso 1 1 d R . .
O2 O 0.0871(3) -0.6030(2) 0.24795(19) 0.0320(5) Uani 1 1 d . . .
O2W O -0.5558(8) -0.5381(7) 0.4310(5) 0.0584(13) Uiso 0.50 1 d P . .
H2WA H -0.5690 -0.4527 0.4879 0.088 Uiso 1 1 d R . .
O3 O -0.2486(3) -0.6335(2) 0.30245(19) 0.0319(5) Uani 1 1 d . . .
O3W O -0.3076(3) -1.8041(3) -0.4411(2) 0.0393(5) Uani 1 1 d . . .
H3WA H -0.2192 -1.7738 -0.4860 0.059 Uiso 1 1 d R . .
H3WB H -0.4228 -1.8298 -0.4858 0.059 Uiso 1 1 d R . .
O4 O -0.0710(3) -1.2698(2) 0.2689(2) 0.0321(4) Uani 1 1 d . . .
O5 O -0.4261(3) -1.3706(2) 0.21709(19) 0.0291(4) Uani 1 1 d . . .
O6 O -0.2264(4) -1.4712(2) 0.0404(2) 0.0401(5) Uani 1 1 d . . .
O7 O -0.2797(3) -0.8543(2) -0.13607(17) 0.0288(4) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O3 S1 O2 113.28(12) . .
O3 S1 O1 113.15(12) . .
O2 S1 O1 112.61(12) . .
O3 S1 C1 104.68(11) . .
O2 S1 C1 107.42(11) . .
O1 S1 C1 104.84(11) . .
O6 S2 O4 113.08(13) . .
O6 S2 O5 113.99(13) . .
O4 S2 O5 110.51(12) . .
O6 S2 C3 105.10(11) . .
O4 S2 C3 107.01(11) . .
O5 S2 C3 106.53(11) . .
O6 S2 Na1 121.92(8) . 1_545
O4 S2 Na1 54.99(8) . 1_545
O5 S2 Na1 57.40(8) . 1_545
C3 S2 Na1 132.95(8) . 1_545
O1 Na1 O2W 115.50(14) 2_546 .
O1 Na1 O2W 83.42(13) 2_546 2_446
O2W Na1 O2W 36.1(2) . 2_446
O1 Na1 O1W 92.57(9) 2_546 .
O2W Na1 O1W 103.66(16) . .
O2W Na1 O1W 89.73(15) 2_446 .
O1 Na1 O4 98.42(8) 2_546 1_565
O2W Na1 O4 138.85(14) . 1_565
O2W Na1 O4 172.90(15) 2_446 1_565
O1W Na1 O4 97.02(8) . 1_565
O1 Na1 O3 87.68(8) 2_546 .
O2W Na1 O3 69.62(15) . .
O2W Na1 O3 82.89(15) 2_446 .
O1W Na1 O3 172.54(9) . .
O4 Na1 O3 90.31(8) 1_565 .
O1 Na1 O5 154.94(8) 2_546 1_565
O2W Na1 O5 86.62(14) . 1_565
O2W Na1 O5 120.92(13) 2_446 1_565
O1W Na1 O5 93.36(8) . 1_565
O4 Na1 O5 56.68(6) 1_565 1_565
O3 Na1 O5 89.52(8) . 1_565
O1 Na1 S2 126.18(7) 2_546 1_565
O2W Na1 S2 111.53(13) . 1_565
O2W Na1 S2 147.56(13) 2_446 1_565
O1W Na1 S2 100.55(7) . 1_565
O4 Na1 S2 28.61(5) 1_565 1_565
O3 Na1 S2 85.25(6) . 1_565
O5 Na1 S2 28.77(4) 1_565 1_565
O1 Na1 H2WA 114.7 2_546 .
O2W Na1 H2WA 20.2 . .
O2W Na1 H2WA 31.7 2_446 .
O1W Na1 H2WA 83.6 . .
O4 Na1 H2WA 146.8 1_565 .
O3 Na1 H2WA 89.5 . .
O5 Na1 H2WA 90.2 1_565 .
S2 Na1 H2WA 118.5 1_565 .
O6 Na2 O3W 166.40(9) . .
O6 Na2 O2 96.49(8) . 2_535
O3W Na2 O2 89.30(8) . 2_535
O6 Na2 O5 82.87(9) . 2_425
O3W Na2 O5 84.30(8) . 2_425
O2 Na2 O5 95.92(8) 2_535 2_425
O6 Na2 O7 83.04(7) . 1_545
O3W Na2 O7 94.24(8) . 1_545
O2 Na2 O7 166.17(8) 2_535 1_545
O5 Na2 O7 97.73(7) 2_425 1_545
O6 Na2 O4 117.73(8) . 2_525
O3W Na2 O4 74.13(8) . 2_525
O2 Na2 O4 92.35(7) 2_535 2_525
O5 Na2 O4 156.79(8) 2_425 2_525
O7 Na2 O4 75.85(7) 1_545 2_525
C2 C1 C6 120.3(2) . .
C2 C1 S1 117.90(17) . .
C6 C1 S1 121.79(17) . .
C1 C2 C3 119.3(2) . .
C1 C2 H2A 120.4 . .
C3 C2 H2A 120.4 . .
C4 C3 C2 121.1(2) . .
C4 C3 S2 118.81(17) . .
C2 C3 S2 120.04(18) . .
C5 C4 C3 119.2(2) . .
C5 C4 H4A 120.4 . .
C3 C4 H4A 120.4 . .
C4 C5 C6 120.9(2) . .
C4 C5 H5A 119.5 . .
C6 C5 H5A 119.5 . .
C5 C6 C1 119.0(2) . .
C5 C6 C7 118.0(2) . .
C1 C6 C7 122.9(2) . .
O7 C7 C6 123.5(2) . .
O7 C7 H7A 118.3 . .
C6 C7 H7A 118.3 . .
S1 O1 Na1 145.25(12) . 2_546
Na1 O1W H1WB 124.9 . .
Na1 O1W H1WA 127.0 . .
H1WB O1W H1WA 105.6 . .
S1 O2 Na2 146.51(12) . 2_535
O2W O2W Na1 73.5(4) 2_446 .
O2W O2W Na1 70.4(4) 2_446 2_446
Na1 O2W Na1 143.9(2) . 2_446
O2W O2W H2WA 61.4 2_446 .
Na1 O2W H2WA 79.7 . .
Na1 O2W H2WA 83.2 2_446 .
S1 O3 Na1 127.10(11) . .
Na2 O3W H3WA 112.1 . .
Na2 O3W H3WB 122.2 . .
H3WA O3W H3WB 107.4 . .
S2 O4 Na1 96.40(10) . 1_545
S2 O4 Na2 116.37(12) . 2_525
Na1 O4 Na2 116.39(8) 1_545 2_525
S2 O5 Na2 143.31(11) . 2_425
S2 O5 Na1 93.82(9) . 1_545
Na2 O5 Na1 120.59(8) 2_425 1_545
S2 O6 Na2 157.57(12) . .
C7 O7 Na2 117.49(16) . 1_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O3 1.4489(19) .
S1 O2 1.4494(19) .
S1 O1 1.4541(18) .
S1 C1 1.793(2) .
S2 O6 1.444(2) .
S2 O4 1.452(2) .
S2 O5 1.4538(18) .
S2 C3 1.785(2) .
S2 Na1 3.0137(13) 1_545
Na1 O1 2.326(2) 2_546
Na1 O2W 2.348(5) .
Na1 O2W 2.390(5) 2_446
Na1 O1W 2.418(3) .
Na1 O4 2.484(2) 1_565
Na1 O3 2.486(2) .
Na1 O5 2.545(2) 1_565
Na1 S2 3.0137(13) 1_565
Na1 H2WA 2.3453 .
Na2 O6 2.408(2) .
Na2 O3W 2.413(2) .
Na2 O2 2.424(2) 2_535
Na2 O5 2.471(2) 2_425
Na2 O7 2.475(2) 1_545
Na2 O4 2.546(2) 2_525
C1 C2 1.391(3) .
C1 C6 1.402(3) .
C2 C3 1.394(3) .
C2 H2A 0.9300 .
C3 C4 1.386(3) .
C4 C5 1.383(3) .
C4 H4A 0.9300 .
C5 C6 1.398(3) .
C5 H5A 0.9300 .
C6 C7 1.482(3) .
C7 O7 1.207(3) .
C7 H7A 0.9300 .
O1 Na1 2.326(2) 2_546
O1W H1WB 0.8577 .
O1W H1WA 0.8582 .
O2 Na2 2.424(2) 2_535
O2W O2W 1.468(10) 2_446
O2W Na1 2.390(5) 2_446
O2W H2WA 0.8221 .
O3W H3WA 0.8606 .
O3W H3WB 0.8614 .
O4 Na1 2.484(2) 1_545
O4 Na2 2.546(2) 2_525
O5 Na2 2.471(2) 2_425
O5 Na1 2.545(2) 1_545
O7 Na2 2.475(2) 1_565
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O3 S1 C1 C2 -116.97(19) . . . .
O2 S1 C1 C2 122.35(19) . . . .
O1 S1 C1 C2 2.4(2) . . . .
O3 S1 C1 C6 61.8(2) . . . .
O2 S1 C1 C6 -58.8(2) . . . .
O1 S1 C1 C6 -178.84(18) . . . .
C6 C1 C2 C3 -1.8(3) . . . .
S1 C1 C2 C3 177.06(17) . . . .
C1 C2 C3 C4 -0.5(3) . . . .
C1 C2 C3 S2 -179.53(17) . . . .
O6 S2 C3 C4 29.4(2) . . . .
O4 S2 C3 C4 149.84(19) . . . .
O5 S2 C3 C4 -91.9(2) . . . .
Na1 S2 C3 C4 -152.49(14) 1_545 . . .
O6 S2 C3 C2 -151.6(2) . . . .
O4 S2 C3 C2 -31.1(2) . . . .
O5 S2 C3 C2 87.1(2) . . . .
Na1 S2 C3 C2 26.5(2) 1_545 . . .
C2 C3 C4 C5 2.2(3) . . . .
S2 C3 C4 C5 -178.82(17) . . . .
C3 C4 C5 C6 -1.5(4) . . . .
C4 C5 C6 C1 -0.7(3) . . . .
C4 C5 C6 C7 -179.2(2) . . . .
C2 C1 C6 C5 2.4(3) . . . .
S1 C1 C6 C5 -176.38(17) . . . .
C2 C1 C6 C7 -179.3(2) . . . .
S1 C1 C6 C7 2.0(3) . . . .
C5 C6 C7 O7 -7.9(4) . . . .
C1 C6 C7 O7 173.7(2) . . . .
O3 S1 O1 Na1 -141.24(18) . . . 2_546
O2 S1 O1 Na1 -11.2(2) . . . 2_546
C1 S1 O1 Na1 105.29(19) . . . 2_546
O3 S1 O2 Na2 11.7(3) . . . 2_535
O1 S1 O2 Na2 -118.3(2) . . . 2_535
C1 S1 O2 Na2 126.8(2) . . . 2_535
O1 Na1 O2W O2W 29.6(5) 2_546 . . 2_446
O1W Na1 O2W O2W -70.0(4) . . . 2_446
O4 Na1 O2W O2W 172.0(3) 1_565 . . 2_446
O3 Na1 O2W O2W 106.6(4) . . . 2_446
O5 Na1 O2W O2W -162.7(4) 1_565 . . 2_446
S2 Na1 O2W O2W -177.4(4) 1_565 . . 2_446
O1 Na1 O2W Na1 29.6(5) 2_546 . . 2_446
O2W Na1 O2W Na1 0.0 2_446 . . 2_446
O1W Na1 O2W Na1 -70.0(4) . . . 2_446
O4 Na1 O2W Na1 172.0(3) 1_565 . . 2_446
O3 Na1 O2W Na1 106.6(4) . . . 2_446
O5 Na1 O2W Na1 -162.7(4) 1_565 . . 2_446
S2 Na1 O2W Na1 -177.4(4) 1_565 . . 2_446
O2 S1 O3 Na1 -55.65(17) . . . .
O1 S1 O3 Na1 74.06(16) . . . .
C1 S1 O3 Na1 -172.37(12) . . . .
O1 Na1 O3 S1 -27.45(15) 2_546 . . .
O2W Na1 O3 S1 -145.8(2) . . . .
O2W Na1 O3 S1 -111.11(18) 2_446 . . .
O1W Na1 O3 S1 -119.5(6) . . . .
O4 Na1 O3 S1 70.96(15) 1_565 . . .
O5 Na1 O3 S1 127.64(15) 1_565 . . .
S2 Na1 O3 S1 99.15(14) 1_565 . . .
O6 S2 O4 Na1 -113.79(11) . . . 1_545
O5 S2 O4 Na1 15.36(12) . . . 1_545
C3 S2 O4 Na1 130.96(9) . . . 1_545
O6 S2 O4 Na2 9.91(15) . . . 2_525
O5 S2 O4 Na2 139.06(11) . . . 2_525
C3 S2 O4 Na2 -105.34(11) . . . 2_525
Na1 S2 O4 Na2 123.70(12) 1_545 . . 2_525
O6 S2 O5 Na2 -85.7(2) . . . 2_425
O4 S2 O5 Na2 145.69(18) . . . 2_425
C3 S2 O5 Na2 29.8(2) . . . 2_425
Na1 S2 O5 Na2 160.6(2) 1_545 . . 2_425
O6 S2 O5 Na1 113.73(11) . . . 1_545
O4 S2 O5 Na1 -14.92(11) . . . 1_545
C3 S2 O5 Na1 -130.83(10) . . . 1_545
O4 S2 O6 Na2 -126.6(4) . . . .
O5 S2 O6 Na2 106.1(4) . . . .
C3 S2 O6 Na2 -10.2(4) . . . .
Na1 S2 O6 Na2 171.4(3) 1_545 . . .
O3W Na2 O6 S2 -82.9(6) . . . .
O2 Na2 O6 S2 31.9(4) 2_535 . . .
O5 Na2 O6 S2 -63.3(4) 2_425 . . .
O7 Na2 O6 S2 -162.1(4) 1_545 . . .
O4 Na2 O6 S2 128.0(4) 2_525 . . .
C6 C7 O7 Na2 -171.22(17) . . . 1_565
