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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/20/7052097.cif $
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#
# 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_7052097
loop_
_publ_author_name
'Deacon, Glen B.'
'Harika, Rita'
'Junk, Peter C.'
'Skelton, Brian W.'
'White, Allan H.'
_publ_section_title
;
 Structural versatility in hydrated rare earth(iii)
 1,2-benzenedisulfonates
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              634
_journal_paper_doi               10.1039/b614681c
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         'C24 H16 La2 O24 S8, 4(H2 O), 2(H3 O)'
_chemical_formula_sum            'C24 H30 La2 O30 S8'
_chemical_formula_weight         1332.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                64.72(3)
_cell_angle_beta                 84.92(3)
_cell_angle_gamma                76.29(3)
_cell_formula_units_Z            1
_cell_length_a                   9.750(2)
_cell_length_b                   10.216(2)
_cell_length_c                   11.647(2)
_cell_measurement_temperature    123
_cell_volume                     1019.0(4)
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tu'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_av_sigmaI/netI    .052
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13892
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  .82
_exptl_absorpt_correction_T_min  .7822
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_F_000             328
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .16
_refine_diff_density_max         .86
_refine_diff_density_min         -.841
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.013
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .038
_refine_ls_R_factor_gt           .029
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .035
_refine_ls_wR_factor_ref         .033
_reflns_d_resolution_high        .751
_reflns_d_resolution_low         9.453
_reflns_Friedel_coverage         0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                4174
_reflns_number_total             4843
_reflns_threshold_expression     'I > 2.00 sig(I )'
_cod_data_source_file            b614681c.txt
_cod_data_source_block           rh97
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               7052097
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
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_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 .741988(18) .97488(2) .038221(16) .01071(17) Uani ? ? 1.00000 ? ?
S11 .50305(8) .82398(9) .25805(7) .0124(7) Uani ? ? 1.00000 ? ?
O111 .4705(2) .6806(3) .3269(2) .019(2) Uani ? ? 1.00000 ? ?
O112 .4505(2) .9003(3) .1258(2) .017(2) Uani ? ? 1.00000 ? ?
O113 .6543(2) .8211(3) .2562(2) .016(2) Uani ? ? 1.00000 ? ?
S12 .41848(8) 1.20737(9) .12168(7) .0120(7) Uani ? ? 1.00000 ? ?
O121 .5668(2) 1.1482(3) .1054(2) .013(2) Uani ? ? 1.00000 ? ?
O122 .3949(2) 1.3560(3) .1162(2) .015(2) Uani ? ? 1.00000 ? ?
O123 .3238(2) 1.2036(3) .0334(2) .015(2) Uani ? ? 1.00000 ? ?
C11 .4180(3) .9362(4) .3369(3) .013(3) Uani ? ? 1.00000 ? ?
C12 .3788(3) 1.0913(4) .2814(3) .015(3) Uani ? ? 1.00000 ? ?
C13 .3116(3) 1.1661(4) .3541(3) .017(3) Uani ? ? 1.00000 ? ?
C14 .2867(3) 1.0874(4) .4818(3) .021(3) Uani ? ? 1.00000 ? ?
C15 .3275(3) .9356(5) .5381(3) .021(3) Uani ? ? 1.00000 ? ?
C16 .3908(3) .8589(4) .4652(3) .017(3) Uani ? ? 1.00000 ? ?
S21 1.09282(9) .69402(10) .16298(7) .0178(7) Uani ? ? 1.00000 ? ?
O211 1.1338(2) .5444(3) .1734(2) .017(2) Uani ? ? 1.00000 ? ?
O212 .9460(3) .7603(4) .1263(2) .045(3) Uani ? ? 1.00000 ? ?
O213 1.1882(4) .7840(4) .0821(2) .053(4) Uani ? ? 1.00000 ? ?
S22 1.00931(8) .98994(9) .24430(7) .0114(6) Uani ? ? 1.00000 ? ?
O221 .9993(3) 1.0796(3) .3123(2) .022(2) Uani ? ? 1.00000 ? ?
O222 .8734(3) 1.0015(3) .1958(3) .040(3) Uani ? ? 1.00000 ? ?
O223 1.1132(3) 1.0203(3) .1449(3) .044(3) Uani ? ? 1.00000 ? ?
C21 1.1098(3) .6806(4) .3198(3) .014(3) Uani ? ? 1.00000 ? ?
C22 1.0697(3) .8016(4) .3535(3) .012(3) Uani ? ? 1.00000 ? ?
C23 1.0808(3) .7766(4) .4796(3) .015(3) Uani ? ? 1.00000 ? ?
C24 1.1336(3) .6334(4) .5712(3) .019(3) Uani ? ? 1.00000 ? ?
C25 1.1757(4) .5168(4) .5381(3) .021(3) Uani ? ? 1.00000 ? ?
C26 1.1630(3) .5407(4) .4118(3) .019(3) Uani ? ? 1.00000 ? ?
O1 .9925(3) .3705(4) .1281(3) .024(3) Uani ? ? 1.00000 ? ?
O2 .7383(3) .4216(3) .0890(3) .026(3) Uani ? ? 1.00000 ? ?
O3 .5512(3) .4480(3) .2487(3) .026(3) Uani ? ? 1.00000 ? ?
H13 .28300 1.27130 .31570 .02000 Uiso ? ? 1.00000 ? ?
H14 .24170 1.13920 .53090 .02400 Uiso ? ? 1.00000 ? ?
H15 .31200 .88270 .62580 .02600 Uiso ? ? 1.00000 ? ?
H16 .41610 .75360 .50350 .02100 Uiso ? ? 1.00000 ? ?
H23 1.05230 .85670 .50370 .01900 Uiso ? ? 1.00000 ? ?
H24 1.14040 .61730 .65700 .02300 Uiso ? ? 1.00000 ? ?
H25 1.21300 .41980 .60080 .02500 Uiso ? ? 1.00000 ? ?
H26 1.19180 .45970 .38870 .02300 Uiso ? ? 1.00000 ? ?
H1A 1.036(5) .420(6) .143(5) .055(16) Uiso ? ? 1.00000 ? ?
H1B 1.022(4) .284(6) .177(4) .038(14) Uiso ? ? 1.00000 ? ?
H2A .841(6) .406(6) .107(4) .074(18) Uiso ? ? 1.00000 ? ?
H2B .703(4) .492(6) .012(4) .042(13) Uiso ? ? 1.00000 ? ?
H2C .691(4) .428(5) .143(4) .027(13) Uiso ? ? 1.00000 ? ?
H3A .518(5) .515(6) .266(4) .043(15) Uiso ? ? 1.00000 ? ?
H3B .472(4) .442(5) .218(4) .038(12) Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 12 .003296 .001587 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 15 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 15 .01062 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1'
S ? 0 4 .124573 .123413 'Int Tables Vol IV Tables 2.2B and 2.3.1'
La ? 0 1 -.287109 2.4523 'Int Tables Vol IV Tables 2.2B and 2.3.1'
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O121 La1 O212 . . . 139.89(9) ?
O121 La1 O222 . . . 76.35(9) ?
O121 La1 O112 . . '2 675' 73.07(8) ?
O121 La1 O213 . . '2 775' 76.76(10) ?
O121 La1 O223 . . '2 775' 139.27(8) ?
O212 La1 O222 . . . 69.63(11) ?
O212 La1 O112 . . '2 675' 144.84(11) ?
O212 La1 O213 . . '2 775' 113.56(11) ?
O212 La1 O223 . . '2 775' 74.98(9) ?
O222 La1 O112 . . '2 675' 145.00(10) ?
O222 La1 O213 . . '2 775' 76.01(10) ?
O222 La1 O223 . . '2 775' 111.52(11) ?
O112 La1 O213 '2 675' . '2 775' 80.75(10) ?
O112 La1 O223 '2 675' . '2 775' 82.36(9) ?
O213 La1 O223 '2 775' . '2 775' 67.45(11) ?
O111 S11 O112 . . . 113.91(17) ?
O111 S11 O113 . . . 113.60(13) ?
O111 S11 C11 . . . 106.99(15) ?
O112 S11 O113 . . . 107.73(13) ?
O112 S11 C11 . . . 106.98(14) ?
O113 S11 C11 . . . 107.23(18) ?
S11 O112 La1 . . '2 675' 152.81(13) ?
O121 S12 O122 . . . 112.01(15) ?
O121 S12 O123 . . . 113.39(16) ?
O121 S12 C12 . . . 105.21(13) ?
O122 S12 O123 . . . 110.70(14) ?
O122 S12 C12 . . . 105.62(17) ?
O123 S12 C12 . . . 109.45(16) ?
La1 O121 S12 . . . 147.37(18) ?
S11 C11 C12 . . . 125.5(2) ?
S11 C11 C16 . . . 115.3(3) ?
C12 C11 C16 . . . 119.1(4) ?
S12 C12 C11 . . . 124.6(3) ?
S12 C12 C13 . . . 115.5(3) ?
C11 C12 C13 . . . 119.7(3) ?
C12 C13 C14 . . . 120.3(3) ?
C12 C13 H13 . . . 119.6 ?
C14 C13 H13 . . . 120.1 ?
C13 C14 C15 . . . 120.5(4) ?
C13 C14 H14 . . . 119.8 ?
C15 C14 H14 . . . 119.7 ?
C14 C15 C16 . . . 119.7(3) ?
C14 C15 H15 . . . 120.1 ?
C16 C15 H15 . . . 120.2 ?
C11 C16 C15 . . . 120.5(3) ?
C11 C16 H16 . . . 119.7 ?
C15 C16 H16 . . . 119.8 ?
O211 S21 O212 . . . 112.4(2) ?
O211 S21 O213 . . . 111.26(18) ?
O211 S21 C21 . . . 105.96(15) ?
O212 S21 O213 . . . 113.13(17) ?
O212 S21 C21 . . . 106.18(17) ?
O213 S21 C21 . . . 107.4(2) ?
La1 O212 S21 . . . 153.3(2) ?
S21 O213 La1 . . '2 775' 152.4(2) ?
O221 S22 O222 . . . 111.89(18) ?
O221 S22 O223 . . . 112.3(2) ?
O221 S22 C22 . . . 107.47(16) ?
O222 S22 O223 . . . 111.56(18) ?
O222 S22 C22 . . . 107.04(17) ?
O223 S22 C22 . . . 106.17(15) ?
La1 O222 S22 . . . 147.3(2) ?
S22 O223 La1 . . '2 775' 163.4(2) ?
S21 C21 C22 . . . 124.4(2) ?
S21 C21 C26 . . . 116.2(3) ?
C22 C21 C26 . . . 119.4(3) ?
S22 C22 C21 . . . 124.8(2) ?
S22 C22 C23 . . . 115.9(3) ?
C21 C22 C23 . . . 119.3(3) ?
C22 C23 C24 . . . 120.0(4) ?
C22 C23 H23 . . . 120.1 ?
C24 C23 H23 . . . 120.0 ?
C23 C24 C25 . . . 120.7(3) ?
C23 C24 H24 . . . 119.4 ?
C25 C24 H24 . . . 119.8 ?
C24 C25 C26 . . . 119.6(3) ?
C24 C25 H25 . . . 120.2 ?
C26 C25 H25 . . . 120.2 ?
C21 C26 C25 . . . 120.9(4) ?
C21 C26 H26 . . . 119.4 ?
C25 C26 H26 . . . 119.7 ?
H1A O1 H1B . . . 107(5) ?
H1A O1 H2A . . . 125(4) ?
H1B O1 H2A . . . 113(4) ?
H2A O2 H2B . . . 118(4) ?
H2A O2 H2C . . . 113(5) ?
H2B O2 H2C . . . 111(4) ?
H3A O3 H3B . . . 97(5) ?
O1 H2A O2 . . . 173(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
La1 O121 . . 2.486(2) ?
La1 O212 . . 2.488(3) ?
La1 O222 . . 2.468(4) ?
La1 O112 . '2 675' 2.494(2) ?
La1 O213 . '2 775' 2.485(4) ?
La1 O223 . '2 775' 2.440(3) ?
S11 O111 . . 1.436(3) ?
S11 O112 . . 1.472(2) ?
S11 O113 . . 1.466(2) ?
S11 C11 . . 1.778(4) ?
S12 O121 . . 1.459(2) ?
S12 O122 . . 1.455(3) ?
S12 O123 . . 1.460(3) ?
S12 C12 . . 1.795(3) ?
C11 C12 . . 1.398(5) ?
C11 C16 . . 1.396(4) ?
C12 C13 . . 1.396(6) ?
C13 C14 . . 1.388(4) ?
C13 H13 . . .950 ?
C14 C15 . . 1.370(6) ?
C14 H14 . . .950 ?
C15 C16 . . 1.400(6) ?
C15 H15 . . .948 ?
C16 H16 . . .950 ?
S21 O211 . . 1.439(3) ?
S21 O212 . . 1.447(3) ?
S21 O213 . . 1.451(4) ?
S21 C21 . . 1.792(4) ?
S22 O221 . . 1.428(3) ?
S22 O222 . . 1.446(3) ?
S22 O223 . . 1.448(3) ?
S22 C22 . . 1.781(3) ?
C21 C22 . . 1.412(6) ?
C21 C26 . . 1.378(4) ?
C22 C23 . . 1.390(5) ?
C23 C24 . . 1.396(4) ?
C23 H23 . . .948 ?
C24 C25 . . 1.367(6) ?
C24 H24 . . .947 ?
C25 C26 . . 1.396(5) ?
C25 H25 . . .951 ?
C26 H26 . . .951 ?
O1 H1A . . .82(7) ?
O1 H1B . . .82(4) ?
O1 H2A . . 1.45(6) ?
O2 H2A . . 1.00(6) ?
O2 H2B . . .91(4) ?
O2 H2C . . .77(4) ?
O3 H3A . . .79(6) ?
O3 H3B . . .91(5) ?
