#------------------------------------------------------------------------------
#$Date: 2025-08-21 22:04:39 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301851 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052103.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_7052103
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         '2(C6 H16 Tb O12 S2), C6 H4 O6 S2,4(H2 O)'
_chemical_formula_sum            'C18 H44 O34 S6 Tb2'
_chemical_formula_weight         1314.76
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 111.3270(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   7.7246(4)
_cell_length_b                   34.366(2)
_cell_length_c                   8.5388(4)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    150
_cell_measurement_theta_max      37.4
_cell_measurement_theta_min      2.3
_cell_volume                     2111.51(19)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_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      150
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .040
_diffrn_reflns_av_sigmaI/netI    .039
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43562
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.725
_exptl_absorpt_correction_T_max  .79
_exptl_absorpt_correction_T_min  .63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          .16
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .14
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.236
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     286
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .044
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w=1/(sig^2(F) + .0006F^2)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .054
_refine_ls_wR_factor_ref         .051
_reflns_d_resolution_high        .583
_reflns_d_resolution_low         17.124
_reflns_Friedel_coverage         0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              58
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -14
_reflns_number_gt                9838
_reflns_number_total             11240
_reflns_threshold_expression     'F > 4.00 sig(F )'
_cod_data_source_file            b614681c.txt
_cod_data_source_block           rh239
_cod_original_cell_volume        2111.5(2)
_cod_original_sg_symbol_Hall     -p_2yb
_cod_original_sg_symbol_H-M      P_1_21/m_1
_cod_database_code               7052103
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,-z
-x,-y,-z
+x,1/2-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
Tb .66569(2) .116740(6) .450950(10) .00910(4) Uani ? ? 1.00000 ? ?
C11 .2447(4) .05503(8) .0527(3) .0128(9) Uani ? ? 1.00000 ? ?
S11 .23168(9) .10696(2) .05518(8) .0120(2) Uani ? ? 1.00000 ? ?
O111 .3887(3) .11997(6) .2025(3) .0137(7) Uani ? ? 1.00000 ? ?
O112 .2473(3) .11983(7) -.1020(3) .0183(9) Uani ? ? 1.00000 ? ?
O113 .0527(3) .11776(7) .0633(3) .0174(8) Uani ? ? 1.00000 ? ?
C12 .2670(4) .03096(8) .1934(3) .0117(9) Uani ? ? 1.00000 ? ?
S12 .28842(9) .04799(2) .39725(8) .0105(2) Uani ? ? 1.00000 ? ?
O121 .4747(3) .06538(6) .4673(3) .0134(7) Uani ? ? 1.00000 ? ?
O122 .2738(4) .01423(7) .4934(3) .0179(8) Uani ? ? 1.00000 ? ?
O123 .1415(3) .07621(7) .3766(3) .0178(8) Uani ? ? 1.00000 ? ?
C13 .2801(5) -.00907(9) .1769(4) .0188(11) Uani ? ? 1.00000 ? ?
C14 .2691(6) -.02555(10) .0244(5) .0250(13) Uani ? ? 1.00000 ? ?
C15 .2446(6) -.00191(11) -.1144(4) .0265(14) Uani ? ? 1.00000 ? ?
C16 .2341(5) .03836(10) -.0995(4) .0210(12) Uani ? ? 1.00000 ? ?
C21 .9878(6) .25000 -.0364(5) .0153(14) Uani ? ? 1.00000 ? ?
S21 .87986(14) .25000 .11673(12) .0135(3) Uani ? ? 1.00000 ? ?
O211 .7715(4) .21451(8) .0946(3) .0255(11) Uani ? ? 1.00000 ? ?
O212 1.0347(5) .25000 .2800(4) .0177(12) Uani ? ? 1.00000 ? ?
C22 .8917(6) .25000 -.2133(5) .0143(13) Uani ? ? 1.00000 ? ?
S22 .64619(14) .25000 -.31541(12) .0112(3) Uani ? ? 1.00000 ? ?
O221 .5785(3) .21480(7) -.2634(3) .0180(8) Uani ? ? 1.00000 ? ?
O222 .6095(5) .25000 -.4962(4) .0163(11) Uani ? ? 1.00000 ? ?
C23 .9936(7) .25000 -.3186(7) .027(2) Uani ? ? 1.00000 ? ?
C24 1.1866(8) .25000 -.2532(8) .036(3) Uani ? ? 1.00000 ? ?
C25 1.2811(7) .25000 -.0814(8) .043(3) Uani ? ? 1.00000 ? ?
C26 1.1819(7) .25000 .0263(7) .030(2) Uani ? ? 1.00000 ? ?
O01 .6655(4) .18178(6) .3453(3) .0171(8) Uani ? ? 1.00000 ? ?
O02 .7727(3) .10873(7) .2261(3) .0163(8) Uani ? ? 1.00000 ? ?
O03 .8602(3) .05971(6) .5120(3) .0167(8) Uani ? ? 1.00000 ? ?
O04 .4609(3) .15229(7) .5392(3) .0165(8) Uani ? ? 1.00000 ? ?
O05 .7548(3) .11090(7) .7474(3) .0177(8) Uani ? ? 1.00000 ? ?
O06 .9763(3) .13970(7) .5748(3) .0179(8) Uani ? ? 1.00000 ? ?
O07 .1148(3) .17087(7) .3476(3) .0179(8) Uani ? ? 1.00000 ? ?
O08 .5947(3) .14669(7) .9405(3) .0171(8) Uani ? ? 1.00000 ? ?
H13 .29996 -.02538 .27269 .02400 Uiso ? ? 1.00000 ? ?
H14 .27849 -.05304 .01461 .03000 Uiso ? ? 1.00000 ? ?
H15 .23218 -.01334 -.21950 .03100 Uiso ? ? 1.00000 ? ?
H16 .21938 .05466 -.19448 .02500 Uiso ? ? 1.00000 ? ?
H23 .93017 .25000 -.43725 .03300 Uiso ? ? 1.00000 ? ?
H24 1.25494 .25000 -.32590 .04400 Uiso ? ? 1.00000 ? ?
H25 1.41364 .25000 -.03610 .05100 Uiso ? ? 1.00000 ? ?
H26 1.24864 .25000 .14574 .03800 Uiso ? ? 1.00000 ? ?
H01a .70659 .19252 .25681 .02500 Uiso ? ? 1.00000 ? ?
H01b .63913 .20000 .38763 .02500 Uiso ? ? 1.00000 ? ?
H02a .71992 .12132 .14180 .02500 Uiso ? ? 1.00000 ? ?
H02b .87817 .09981 .22231 .02500 Uiso ? ? 1.00000 ? ?
H03a .95815 .05820 .49738 .02400 Uiso ? ? 1.00000 ? ?
H03b .81372 .03456 .49891 .02400 Uiso ? ? 1.00000 ? ?
H04a .34196 .14951 .55002 .02400 Uiso ? ? 1.00000 ? ?
H04b .50682 .17175 .60058 .02400 Uiso ? ? 1.00000 ? ?
H05a .87674 .10599 .85166 .02600 Uiso ? ? 1.00000 ? ?
H05b .67161 .12656 .78311 .02600 Uiso ? ? 1.00000 ? ?
H06a 1.02410 .15826 .52976 .02600 Uiso ? ? 1.00000 ? ?
H06b 1.05847 .13168 .67773 .02600 Uiso ? ? 1.00000 ? ?
H07a .00000 .14967 .35109 .02700 Uiso ? ? 1.00000 ? ?
H07b .09436 .19789 .32976 .02700 Uiso ? ? 1.00000 ? ?
H08a .47840 .14337 .91052 .02500 Uiso ? ? 1.00000 ? ?
H08b .62220 .17857 .94430 .02500 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 36 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 68 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
S ? 0 12 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Tb ? 0 4 -.591 4.151 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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
O111 Tb O121 . . . 73.10(7) ?
O111 Tb O01 . . . 75.40(7) ?
O111 Tb O02 . . . 75.57(8) ?
O111 Tb O03 . . . 120.85(7) ?
O111 Tb O04 . . . 76.75(8) ?
O111 Tb O05 . . . 139.72(9) ?
O111 Tb O06 . . . 143.78(8) ?
O121 Tb O01 . . . 143.94(8) ?
O121 Tb O02 . . . 112.02(8) ?
O121 Tb O03 . . . 74.34(8) ?
O121 Tb O04 . . . 81.90(8) ?
O121 Tb O05 . . . 79.47(8) ?
O121 Tb O06 . . . 141.36(7) ?
O01 Tb O02 . . . 75.93(9) ?
O01 Tb O03 . . . 138.68(9) ?
O01 Tb O04 . . . 74.16(9) ?
O01 Tb O05 . . . 115.94(8) ?
O01 Tb O06 . . . 73.84(8) ?
O02 Tb O03 . . . 72.92(9) ?
O02 Tb O04 . . . 143.32(8) ?
O02 Tb O05 . . . 143.39(8) ?
O02 Tb O06 . . . 78.80(8) ?
O03 Tb O04 . . . 143.14(9) ?
O03 Tb O05 . . . 77.57(9) ?
O03 Tb O06 . . . 74.02(8) ?
O04 Tb O05 . . . 70.58(8) ?
O04 Tb O06 . . . 112.09(8) ?
O05 Tb O06 . . . 72.54(9) ?
S11 C11 C12 . . . 124.3(2) ?
S11 C11 C16 . . . 115.9(2) ?
C12 C11 C16 . . . 119.9(3) ?
C11 S11 O111 . . . 106.39(12) ?
C11 S11 O112 . . . 105.54(15) ?
C11 S11 O113 . . . 108.24(15) ?
O111 S11 O112 . . . 112.20(14) ?
O111 S11 O113 . . . 112.69(15) ?
O112 S11 O113 . . . 111.33(14) ?
Tb O111 S11 . . . 159.51(13) ?
C11 C12 S12 . . . 125.1(2) ?
C11 C12 C13 . . . 118.9(3) ?
S12 C12 C13 . . . 116.0(2) ?
C12 S12 O121 . . . 105.06(14) ?
C12 S12 O122 . . . 106.93(14) ?
C12 S12 O123 . . . 108.00(13) ?
O121 S12 O122 . . . 111.21(13) ?
O121 S12 O123 . . . 112.57(13) ?
O122 S12 O123 . . . 112.57(17) ?
Tb O121 S12 . . . 145.99(12) ?
C12 C13 C14 . . . 121.0(3) ?
C12 C13 H13 . . . 119.2 ?
C14 C13 H13 . . . 119.8 ?
C13 C14 C15 . . . 120.1(3) ?
C13 C14 H14 . . . 120.3 ?
C15 C14 H14 . . . 119.7 ?
C14 C15 C16 . . . 119.7(4) ?
C14 C15 H15 . . . 119.9 ?
C16 C15 H15 . . . 120.4 ?
C11 C16 C15 . . . 120.4(3) ?
C11 C16 H16 . . . 119.8 ?
C15 C16 H16 . . . 119.7 ?
S21 C21 C22 . . . 125.1(3) ?
S21 C21 C26 . . . 116.1(4) ?
C22 C21 C26 . . . 118.7(5) ?
C21 S21 O211 . . . 107.73(15) ?
C21 S21 O212 . . . 105.0(2) ?
C21 S21 O211 . . 4 107.73(15) ?
O211 S21 O212 . . . 110.81(12) ?
O211 S21 O211 . . 4 114.27(18) ?
O212 S21 O211 . . 4 110.81(12) ?
C21 C22 S22 . . . 125.0(4) ?
C21 C22 C23 . . . 119.1(4) ?
S22 C22 C23 . . . 115.8(3) ?
C22 S22 O221 . . . 106.81(12) ?
C22 S22 O222 . . . 106.3(2) ?
C22 S22 O221 . . 4 106.81(12) ?
O221 S22 O222 . . . 111.69(12) ?
O221 S22 O221 . . 4 113.08(18) ?
O222 S22 O221 . . 4 111.69(12) ?
C22 C23 C24 . . . 121.1(5) ?
C22 C23 H23 . . . 119.6 ?
C24 C23 H23 . . . 119.4 ?
C23 C24 C25 . . . 120.2(7) ?
C23 C24 H24 . . . 120.5 ?
C25 C24 H24 . . . 119.3 ?
C24 C25 C26 . . . 119.7(5) ?
C24 C25 H25 . . . 120.4 ?
C26 C25 H25 . . . 119.9 ?
C21 C26 C25 . . . 121.2(5) ?
C21 C26 H26 . . . 119.6 ?
C25 C26 H26 . . . 119.2 ?
Tb O01 H01a . . . 132.40 ?
Tb O01 H01b . . . 122.1 ?
H01a O01 H01b . . . 105.2 ?
Tb O02 H02a . . . 116.5 ?
Tb O02 H02b . . . 132.06 ?
H02a O02 H02b . . . 109.0 ?
Tb O03 H03a . . . 124.2 ?
Tb O03 H03b . . . 123.31 ?
H03a O03 H03b . . . 105.3 ?
Tb O04 H04a . . . 139.82 ?
Tb O04 H04b . . . 115.8 ?
H04a O04 H04b . . . 102.7 ?
Tb O05 H05a . . . 137.8 ?
Tb O05 H05b . . . 108.67 ?
H05a O05 H05b . . . 108.4 ?
Tb O06 H06a . . . 123.71 ?
Tb O06 H06b . . . 124.0 ?
H06a O06 H06b . . . 112.1 ?
H07a O07 H07b . . . 122.6 ?
H08a O08 H08b . . . 108.1 ?
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
Tb O111 . . 2.4061(19) ?
Tb O121 . . 2.337(2) ?
Tb O01 . . 2.410(2) ?
Tb O02 . . 2.367(3) ?
Tb O03 . . 2.408(2) ?
Tb O04 . . 2.330(3) ?
Tb O05 . . 2.378(2) ?
Tb O06 . . 2.377(2) ?
C11 S11 . . 1.788(3) ?
C11 C12 . . 1.417(4) ?
C11 C16 . . 1.395(5) ?
S11 O111 . . 1.464(2) ?
S11 O112 . . 1.459(3) ?
S11 O113 . . 1.458(3) ?
C12 S12 . . 1.786(3) ?
C12 C13 . . 1.390(4) ?
S12 O121 . . 1.469(2) ?
S12 O122 . . 1.449(3) ?
S12 O123 . . 1.454(3) ?
C13 C14 . . 1.394(5) ?
C13 H13 . . .957 ?
C14 C15 . . 1.392(5) ?
C14 H14 . . .953 ?
C15 C16 . . 1.395(5) ?
C15 H15 . . .952 ?
C16 H16 . . .958 ?
C21 S21 . . 1.788(5) ?
C21 C22 . . 1.420(6) ?
C21 C26 . . 1.397(7) ?
S21 O211 . . 1.452(3) ?
S21 O212 . . 1.470(3) ?
S21 O211 . 4 1.452(3) ?
C22 S22 . . 1.776(4) ?
C22 C23 . . 1.395(8) ?
S22 O221 . . 1.450(3) ?
S22 O222 . . 1.465(3) ?
S22 O221 . 4 1.450(3) ?
C23 C24 . . 1.388(8) ?
C23 H23 . . .951 ?
C24 C25 . . 1.381(9) ?
C24 H24 . . .950 ?
C25 C26 . . 1.395(10) ?
C25 H25 . . .954 ?
C26 H26 . . .961 ?
O01 H01a . . .991 ?
O01 H01b . . .786 ?
O02 H02a . . .811 ?
O02 H02b . . .882 ?
O03 H03a . . .812 ?
O03 H03b . . .927 ?
O04 H04a . . .961 ?
O04 H04b . . .844 ?
O05 H05a . . 1.048 ?
O05 H05b . . .968 ?
O06 H06a . . .891 ?
O06 H06b . . .920 ?
O07 H07a . . 1.156 ?
O07 H07b . . .945 ?
O08 H08a . . .848 ?
O08 H08b . . 1.114 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168349068
