#------------------------------------------------------------------------------ #$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100329.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_2100329 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2005 _journal_volume 61 _journal_page_first 663 _journal_page_last 668 _chemical_formula_moiety 'H4 Br1 Na9 O20 S4' _chemical_formula_sum 'Br1 H4 Na9 O20 S4' _chemical_formula_weight 739.09 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n' _symmetry_space_group_name_Hall '-P 4a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 14.9126(5) _cell_length_b 14.9126(5) _cell_length_c 8.4052(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1869.20(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 2.626 _diffrn_ambient_temperature 150(2) loop_ _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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Br1 0.75 0.25 1 0.01417(12) Uani d S 1 . . Br Br11 0.25 0.25 0.48695(5) 0.01273(12) Uani d S 1 . . Br Na1 0.64723(7) 0.37337(6) 0.81685(12) 0.0146(2) Uani d . 1 . . Na Na2 0.75 0.25 0.5 0.0163(4) Uani d S 1 . . Na Na3 0.62673(7) 0.39174(7) 0.20464(12) 0.0163(2) Uani d . 1 . . Na Na11 0.35448(6) 0.37461(7) 0.68522(11) 0.0142(2) Uani d . 1 . . Na Na12 0.25 0.25 1.0196(2) 0.0161(4) Uani d S 1 . . Na Na13 0.37149(7) 0.38946(7) 1.29937(12) 0.0163(2) Uani d . 1 . . Na O1 0.48432(12) 0.18355(12) 0.50326(18) 0.0144(4) Uani d . 1 . . O O2 0.59709(11) 0.26609(11) 0.3582(2) 0.0149(3) Uani d . 1 . . O O3 0.48255(12) 0.34608(11) 0.50464(18) 0.0140(4) Uani d . 1 . . O O4 0.59943(11) 0.26410(11) 0.6435(2) 0.0142(3) Uani d . 1 . . O O5 0.54143(12) 0.47531(12) 0.7030(2) 0.0166(4) Uani d . 1 . . O O11 0.51614(12) 0.18381(12) 1.00036(18) 0.0150(4) Uani d . 1 . . O O12 0.40253(11) 0.26427(11) 1.1447(2) 0.0149(3) Uani d . 1 . . O O13 0.51716(12) 0.34647(12) 1.00146(17) 0.0146(4) Uani d . 1 . . O O14 0.40122(11) 0.26533(11) 0.8598(2) 0.0140(3) Uani d . 1 . . O O15 0.46047(12) 0.47460(12) 0.8003(2) 0.0167(4) Uani d . 1 . . O S1 0.54035(4) 0.26441(4) 0.50241(6) 0.01007(13) Uani d . 1 . . S S11 0.45972(4) 0.26436(4) 1.00141(6) 0.01007(13) Uani d . 1 . . S H5 0.527(2) 0.440(2) 0.628(4) 0.032(9) Uiso d . 1 . . H H15 0.477(3) 0.443(3) 0.881(5) 0.055(12) Uiso d . 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01358(15) 0.01358(15) 0.0153(2) 0 0 0 Br11 0.01265(14) 0.01265(14) 0.0129(2) 0 0 0 Na1 0.0153(5) 0.0151(5) 0.0134(5) -0.0012(4) 0.0002(4) -0.0014(4) Na2 0.0133(6) 0.0133(6) 0.0223(11) 0 0 0 Na3 0.0161(5) 0.0160(5) 0.0167(5) -0.0020(4) -0.0017(4) 0.0030(4) Na11 0.0141(5) 0.0144(5) 0.0140(5) 0.0002(4) 0.0000(4) 0.0022(4) Na12 0.0139(6) 0.0139(6) 0.0204(10) 0 0 0 Na13 0.0164(5) 0.0167(5) 0.0158(5) 0.0013(4) -0.0013(4) -0.0035(4) O1 0.0137(8) 0.0151(8) 0.0145(9) -0.0051(6) 0.0018(6) 0.0000(6) O2 0.0157(8) 0.0147(8) 0.0145(8) -0.0013(7) 0.0036(7) 0.0017(7) O3 0.0136(8) 0.0131(8) 0.0152(9) 0.0041(6) -0.0009(6) -0.0008(6) O4 0.0158(8) 0.0140(8) 0.0130(8) 0.0015(7) -0.0035(7) -0.0001(6) O5 0.0141(8) 0.0181(9) 0.0175(9) -0.0010(7) 0.0032(7) -0.0009(7) O11 0.0144(8) 0.0155(8) 0.0151(9) 0.0043(6) -0.0019(6) -0.0015(6) O12 0.0149(8) 0.0164(8) 0.0135(8) -0.0003(7) 0.0020(7) -0.0016(7) O13 0.0152(8) 0.0143(8) 0.0142(9) -0.0034(6) -0.0016(6) 0.0020(6) O14 0.0136(8) 0.0151(8) 0.0133(8) -0.0003(6) -0.0039(6) 0.0008(6) O15 0.0150(8) 0.0181(9) 0.0169(9) 0.0005(7) 0.0028(7) 0.0022(7) S1 0.0105(2) 0.0102(2) 0.0095(3) 0.00005(19) -0.00022(19) -0.00019(19) S11 0.0101(2) 0.0104(2) 0.0097(3) -0.00001(19) -0.00067(19) -0.00026(19) 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 Br1 Na1 7_667 2.8466(10) ? Br1 Na1 8_657 2.8466(10) ? Br1 Na1 2_655 2.8466(10) ? Br1 Na1 . 2.8466(10) ? Br1 Na3 8_656 3.2872(10) ? Br1 Na3 1_556 3.2872(10) ? Br1 Na3 7_666 3.2872(10) ? Br1 Na3 2_656 3.2872(10) ? Br11 Na11 . 2.9424(10) ? Br11 Na11 2 2.9424(10) ? Br11 Na11 4 2.9424(10) ? Br11 Na11 3 2.9424(10) ? Br11 Na13 2_554 3.1770(11) ? Br11 Na13 1_554 3.1770(11) ? Br11 Na13 3_554 3.1770(11) ? Br11 Na13 4_554 3.1770(11) ? Na1 O4 . 2.2993(19) ? Na1 O11 7_667 2.3179(19) ? Na1 O2 7_666 2.345(2) ? Na1 O5 . 2.391(2) ? Na1 O13 . 2.516(2) ? Na1 Na3 1_556 3.2852(15) ? Na1 Na2 . 3.5813(10) ? Na1 Na3 7_666 3.6507(14) ? Na1 Na13 5_667 3.6798(14) ? Na1 Na3 8_656 3.7281(14) ? Na1 H5 . 2.59(3) ? Na2 O4 8_656 2.5574(17) ? Na2 O4 2_655 2.5574(17) ? Na2 O4 . 2.5574(17) ? Na2 O4 7_666 2.5574(17) ? Na2 O2 . 2.5842(18) ? Na2 O2 8_656 2.5842(18) ? Na2 O2 7_666 2.5842(18) ? Na2 O2 2_655 2.5842(18) ? Na2 S1 8_656 3.1339(6) ? Na2 S1 . 3.1339(6) ? Na2 S1 7_666 3.1339(6) ? Na2 S1 2_655 3.1339(6) ? Na3 O2 . 2.3178(19) ? Na3 O11 7_666 2.3623(19) ? Na3 O15 5_666 2.380(2) ? Na3 O4 7_666 2.4173(19) ? Na3 O13 1_554 2.458(2) ? Na3 Na1 1_554 3.2852(15) ? Na3 Br1 1_554 3.2872(10) ? Na3 S1 7_666 3.3621(11) ? Na3 Na11 5_666 3.6161(14) ? Na3 Na1 8_656 3.6507(14) ? Na3 Na1 7_666 3.7281(14) ? Na11 O14 . 2.3009(19) ? Na11 O1 3 2.3103(19) ? Na11 O14 3 2.3457(19) ? Na11 O15 . 2.379(2) ? Na11 O3 . 2.4764(19) ? Na11 Na13 1_554 3.2606(15) ? Na11 Na11 4 3.4294(14) ? Na11 Na11 3 3.4294(14) ? Na11 Na3 5_666 3.6161(14) ? Na11 Na12 . 3.7121(18) ? Na11 H15 . 2.66(4) ? Na12 O12 . 2.5147(19) ? Na12 O12 4 2.5147(19) ? Na12 O12 3 2.5147(19) ? Na12 O12 2 2.5147(19) ? Na12 O14 2 2.635(2) ? Na12 O14 4 2.635(2) ? Na12 O14 3 2.635(2) ? Na12 O14 . 2.635(2) ? Na12 S11 2 3.1385(6) ? Na12 S11 4 3.1385(6) ? Na12 S11 3 3.1385(6) ? Na12 S11 . 3.1385(6) ? Na13 O12 . 2.322(2) ? Na13 O1 3_556 2.3689(19) ? Na13 O5 5_667 2.399(2) ? Na13 O12 3 2.414(2) ? Na13 O3 1_556 2.4777(19) ? Na13 Br11 1_556 3.1770(11) ? Na13 Na11 1_556 3.2606(15) ? Na13 S11 3 3.3872(11) ? Na13 S11 . 3.3888(11) ? Na13 Na1 5_667 3.6798(14) ? Na13 Na3 1_556 3.8889(15) ? O1 S1 . 1.4670(18) ? O1 Na11 4 2.3103(19) ? O1 Na13 4_554 2.3689(19) ? O2 S1 . 1.4786(17) ? O2 Na1 8_656 2.3452(19) ? O3 S1 . 1.4921(17) ? O3 Na13 1_554 2.4777(19) ? O4 S1 . 1.4773(17) ? O4 Na3 8_656 2.4173(19) ? O5 O15 . 1.458(2) ? O5 Na13 5_667 2.399(2) ? O5 H5 . 0.85(3) ? O11 S11 . 1.4666(18) ? O11 Na1 8_657 2.3179(19) ? O11 Na3 8_656 2.3623(19) ? O12 S11 . 1.4755(18) ? O12 Na13 4 2.414(2) ? O13 S11 . 1.4945(18) ? O13 Na3 1_556 2.458(2) ? O14 S11 . 1.4759(17) ? O14 Na11 4 2.3457(19) ? O15 Na3 5_666 2.380(2) ? O15 H15 . 0.86(4) ? S1 Na3 8_656 3.3621(11) ? S11 Na13 4 3.3872(11) ?