#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/21/7202152.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_7202152
loop_
_publ_author_name
'Zheng, Guoli'
'Zhang, Feng'
'Li, Yinyan'
'Zhang, Hongjie'
_publ_section_title
;
 Guest inducing p-sulfonatocalix[4]arene into three-dimensional capsule
 architecture and a mixed A--B double layer framework
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1560
_journal_paper_doi               10.1039/b805628e
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C32 H44 N2 Na2 O28.5 S4 Tb'
_chemical_formula_weight         1245.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 134.057(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.59(3)
_cell_length_b                   17.867(11)
_cell_length_c                   22.10(2)
_cell_measurement_temperature    293(2)
_cell_volume                     8964(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_method       'ω 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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22619
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bolck
_exptl_crystal_F_000             5032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         9.188
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0949P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                5301
_reflns_number_total             8119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805628e.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8966(12)
_cod_original_sg_symbol_H-M      c2/c
_cod_original_formula_sum        'C32 H44 N2 Na2 O28.50 S4 Tb'
_cod_database_code               7202152
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Tb Tb 0.666378(19) -0.27432(2) 0.16867(3) 0.01932(14) Uani 1 1 d . . .
Na1 Na 0.59073(16) 0.2977(2) 0.2196(2) 0.0363(10) Uani 1 1 d . . .
Na2 Na 0.99804(18) -0.0268(3) 0.6485(2) 0.0445(11) Uani 1 1 d . . .
S1 S 0.56313(10) 0.21668(13) 0.03006(15) 0.0304(6) Uani 1 1 d . . .
S2 S 0.60920(12) 0.16554(14) 0.39400(16) 0.0338(6) Uani 1 1 d . . .
S3 S 0.82840(10) -0.10895(13) 0.69230(14) 0.0267(5) Uani 1 1 d . . .
S4 S 0.85956(10) 0.07593(12) 0.42554(14) 0.0245(5) Uani 1 1 d . . .
C1 C 0.6228(4) 0.0084(5) 0.1213(5) 0.024(2) Uani 1 1 d . . .
C2 C 0.6161(4) 0.0796(5) 0.0925(5) 0.0221(19) Uani 1 1 d . . .
H2 H 0.6419 0.0965 0.0883 0.027 Uiso 1 1 calc R . .
C3 C 0.5728(4) 0.1267(5) 0.0697(6) 0.026(2) Uani 1 1 d . . .
C4 C 0.5347(4) 0.1020(5) 0.0776(5) 0.027(2) Uani 1 1 d . . .
H4 H 0.5056 0.1340 0.0632 0.033 Uiso 1 1 calc R . .
C5 C 0.5396(4) 0.0316(5) 0.1061(5) 0.0188(18) Uani 1 1 d . . .
C6 C 0.5845(4) -0.0154(5) 0.1283(5) 0.0203(19) Uani 1 1 d . . .
C7 C 0.5030(4) 0.0066(5) 0.1226(5) 0.025(2) Uani 1 1 d . . .
H7A H 0.4886 -0.0438 0.1011 0.030 Uiso 1 1 calc R . .
H7B H 0.4692 0.0394 0.0935 0.030 Uiso 1 1 calc R . .
C8 C 0.5390(4) 0.0079(5) 0.2159(5) 0.0217(19) Uani 1 1 d . . .
C9 C 0.5555(4) 0.0758(5) 0.2571(5) 0.024(2) Uani 1 1 d . . .
H9 H 0.5430 0.1200 0.2265 0.029 Uiso 1 1 calc R . .
C10 C 0.5902(4) 0.0794(5) 0.3434(6) 0.028(2) Uani 1 1 d . . .
C11 C 0.6089(4) 0.0135(5) 0.3881(6) 0.029(2) Uani 1 1 d . . .
H11 H 0.6333 0.0150 0.4461 0.035 Uiso 1 1 calc R . .
C12 C 0.5915(4) -0.0555(5) 0.3469(6) 0.026(2) Uani 1 1 d . . .
C13 C 0.5558(4) -0.0574(5) 0.2620(5) 0.0211(19) Uani 1 1 d . . .
C14 C 0.6154(4) -0.1283(6) 0.3995(6) 0.030(2) Uani 1 1 d . . .
H14A H 0.6085 -0.1272 0.4359 0.036 Uiso 1 1 calc R . .
H14B H 0.5944 -0.1709 0.3620 0.036 Uiso 1 1 calc R . .
C15 C 0.6803(4) -0.1374(5) 0.4522(5) 0.024(2) Uani 1 1 d . . .
C16 C 0.7212(4) -0.1219(5) 0.5369(6) 0.028(2) Uani 1 1 d . . .
H16 H 0.7085 -0.1078 0.5627 0.034 Uiso 1 1 calc R . .
C17 C 0.7808(4) -0.1270(5) 0.5841(5) 0.023(2) Uani 1 1 d . . .
C18 C 0.8002(4) -0.1489(5) 0.5475(5) 0.024(2) Uani 1 1 d . . .
H18 H 0.8403 -0.1541 0.5801 0.029 Uiso 1 1 calc R . .
C19 C 0.7600(4) -0.1634(5) 0.4618(5) 0.0196(19) Uani 1 1 d . . .
C20 C 0.7004(4) -0.1591(5) 0.4155(5) 0.023(2) Uani 1 1 d . . .
C21 C 0.7811(4) -0.1850(5) 0.4202(6) 0.024(2) Uani 1 1 d . . .
H21A H 0.7579 -0.2267 0.3823 0.029 Uiso 1 1 calc R . .
H21B H 0.8219 -0.2009 0.4629 0.029 Uiso 1 1 calc R . .
C22 C 0.7757(4) -0.1182(5) 0.3700(6) 0.023(2) Uani 1 1 d . . .
C23 C 0.8171(4) -0.0625(5) 0.4132(6) 0.027(2) Uani 1 1 d . . .
H23 H 0.8491 -0.0667 0.4711 0.032 Uiso 1 1 calc R . .
C24 C 0.8113(4) 0.0003(5) 0.3709(6) 0.024(2) Uani 1 1 d . . .
C25 C 0.7649(4) 0.0060(5) 0.2849(5) 0.0230(19) Uani 1 1 d . . .
H25 H 0.7617 0.0479 0.2571 0.028 Uiso 1 1 calc R . .
C26 C 0.7225(4) -0.0503(5) 0.2391(5) 0.0202(19) Uani 1 1 d . . .
C27 C 0.7282(4) -0.1140(4) 0.2829(5) 0.0165(18) Uani 1 1 d . . .
C28 C 0.6711(4) -0.0415(5) 0.1454(5) 0.0216(19) Uani 1 1 d . . .
H28A H 0.6853 -0.0210 0.1216 0.026 Uiso 1 1 calc R . .
H28B H 0.6547 -0.0905 0.1207 0.026 Uiso 1 1 calc R . .
C29 C 0.7781(5) 0.1655(7) 0.4947(7) 0.047(3) Uani 1 1 d . . .
H29 H 0.8038 0.1986 0.5393 0.056 Uiso 1 1 calc R . .
C30 C 0.7391(5) 0.1921(6) 0.4147(7) 0.040(3) Uani 1 1 d . . .
H30 H 0.7370 0.2432 0.4047 0.048 Uiso 1 1 calc R . .
C31 C 0.7406(8) 0.0460(7) 0.4409(13) 0.073(5) Uani 1 1 d . . .
H31 H 0.7401 -0.0051 0.4483 0.088 Uiso 1 1 calc R . .
C32 C 0.7050(7) 0.0731(7) 0.3669(10) 0.059(4) Uani 1 1 d . . .
H32 H 0.6784 0.0409 0.3218 0.071 Uiso 1 1 calc R . .
N1 N 0.7803(5) 0.0916(7) 0.5110(8) 0.063(3) Uani 1 1 d . . .
N2 N 0.7040(4) 0.1451(6) 0.3509(7) 0.050(3) Uani 1 1 d . . .
O1 O 0.5868(3) -0.0851(3) 0.1559(4) 0.0276(15) Uani 1 1 d . . .
H1 H 0.6193 -0.1037 0.1819 0.041 Uiso 1 1 calc R . .
O2 O 0.5369(3) -0.1262(3) 0.2239(4) 0.0302(15) Uani 1 1 d . . .
H2A H 0.5279 -0.1239 0.1791 0.045 Uiso 1 1 calc R . .
O3 O 0.6579(3) -0.1748(4) 0.3316(4) 0.0329(16) Uani 1 1 d . . .
H3 H 0.6723 -0.1993 0.3182 0.049 Uiso 1 1 calc R . .
O4 O 0.6871(3) -0.1673(3) 0.2401(3) 0.0229(13) Uani 1 1 d . . .
O5 O 0.5244(3) 0.2093(4) -0.0604(5) 0.047(2) Uani 1 1 d . . .
O6 O 0.6205(3) 0.2435(4) 0.0705(5) 0.052(2) Uani 1 1 d . . .
O7 O 0.5354(3) 0.2621(4) 0.0502(5) 0.0400(17) Uani 1 1 d . . .
O8 O 0.6039(4) 0.2214(4) 0.3424(5) 0.062(2) Uani 1 1 d . . .
O9 O 0.5679(3) 0.1792(5) 0.4029(5) 0.052(2) Uani 1 1 d . . .
O10 O 0.6692(3) 0.1593(4) 0.4740(5) 0.050(2) Uani 1 1 d . . .
O11 O 0.8873(3) -0.1263(4) 0.7317(4) 0.0414(18) Uani 1 1 d . . .
O12 O 0.8088(3) -0.1601(3) 0.7211(3) 0.0269(15) Uani 1 1 d . . .
O13 O 0.8199(3) -0.0327(4) 0.7023(4) 0.0446(19) Uani 1 1 d . . .
O14 O 0.8219(3) 0.1408(3) 0.4036(4) 0.0343(16) Uani 1 1 d . . .
O15 O 0.9018(3) 0.0571(4) 0.5129(4) 0.046(2) Uani 1 1 d . . .
O16 O 0.8842(3) 0.0935(4) 0.3896(4) 0.0387(17) Uani 1 1 d . . .
O17 O 0.8167(6) 0.0686(7) 0.5882(7) 0.111(5) Uani 1 1 d . . .
O18 O 0.6681(4) 0.1713(6) 0.2743(5) 0.076(3) Uani 1 1 d . . .
O19 O 0.5849(3) -0.2648(4) 0.1560(4) 0.0334(16) Uani 1 1 d . . .
O20 O 0.7004(3) -0.2003(3) 0.1196(4) 0.0296(15) Uani 1 1 d . . .
O21 O 0.5814(3) -0.2384(4) 0.0294(4) 0.0346(16) Uani 1 1 d . . .
O22 O 0.7709(3) -0.2880(4) 0.2655(4) 0.0350(16) Uani 1 1 d . . .
O23 O 0.7993(4) -0.1271(5) 0.1888(7) 0.083(3) Uani 1 1 d . . .
O24 O 0.9916(4) -0.0853(5) 0.5199(6) 0.071(3) Uani 1 1 d . . .
O25 O 1.0775(5) 0.0527(6) 0.6532(6) 0.101(4) Uani 1 1 d . . .
O26 O 0.9410(5) -0.1607(6) 0.6087(7) 0.094(3) Uani 1 1 d . . .
O27 O 0.9275(7) -0.0003(9) 0.6806(10) 0.152(6) Uiso 1 1 d . . .
O28 O 0.4798(5) 0.3365(6) 0.1606(9) 0.117(4) Uani 1 1 d . . .
O29 O 1.0000 -0.2445(18) 0.7500 0.053(15) Uiso 0.38(5) 2 d SP A 1
O30 O 1.0303(14) -0.2285(16) 0.7473(17) 0.061(11) Uiso 0.31(2) 1 d P A 2
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'
Na Na 0.0362 0.0249 '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'
Tb Tb -0.1723 4.1537 '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
_geom_angle_publ_flag
O4 Tb O12 88.4(2) . 7_646 ?
O4 Tb O21 101.2(2) . . ?
O12 Tb O21 139.5(2) 7_646 . ?
O4 Tb O20 81.1(2) . . ?
O12 Tb O20 146.7(2) 7_646 . ?
O21 Tb O20 73.8(2) . . ?
O4 Tb O22 85.0(2) . . ?
O12 Tb O22 76.0(2) 7_646 . ?
O21 Tb O22 143.5(2) . . ?
O20 Tb O22 71.7(2) . . ?
O4 Tb O19 77.8(2) . . ?
O12 Tb O19 72.9(2) 7_646 . ?
O21 Tb O19 71.0(2) . . ?
O20 Tb O19 134.0(2) . . ?
O22 Tb O19 144.6(2) . . ?
O4 Tb O14 152.7(2) . 4_645 ?
O12 Tb O14 106.6(2) 7_646 4_645 ?
O21 Tb O14 82.3(2) . 4_645 ?
O20 Tb O14 73.9(2) . 4_645 ?
O22 Tb O14 77.1(2) . 4_645 ?
O19 Tb O14 127.9(2) . 4_645 ?
O4 Tb O16 151.8(2) . 4_645 ?
O12 Tb O16 72.8(2) 7_646 4_645 ?
O21 Tb O16 81.5(2) . 4_645 ?
O20 Tb O16 125.9(2) . 4_645 ?
O22 Tb O16 109.7(2) . 4_645 ?
O19 Tb O16 76.7(2) . 4_645 ?
O14 Tb O16 55.3(2) 4_645 4_645 ?
O4 Tb S4 178.53(17) . 4_645 ?
O12 Tb S4 90.47(17) 7_646 4_645 ?
O21 Tb S4 80.26(18) . 4_645 ?
O20 Tb S4 99.43(16) . 4_645 ?
O22 Tb S4 93.91(17) . 4_645 ?
O19 Tb S4 102.71(17) . 4_645 ?
O14 Tb S4 27.24(16) 4_645 4_645 ?
O16 Tb S4 28.10(14) 4_645 4_645 ?
O8 Na1 O28 82.4(4) . . ?
O8 Na1 O23 104.7(3) . 4_655 ?
O28 Na1 O23 135.4(3) . 4_655 ?
O8 Na1 O7 134.1(3) . . ?
O28 Na1 O7 91.0(3) . . ?
O23 Na1 O7 111.2(3) 4_655 . ?
O8 Na1 O18 72.7(3) . . ?
O28 Na1 O18 142.4(3) . . ?
O23 Na1 O18 79.3(3) 4_655 . ?
O7 Na1 O18 86.8(2) . . ?
O8 Na1 O25 143.3(3) . 8_455 ?
O28 Na1 O25 81.2(4) . 8_455 ?
O23 Na1 O25 66.9(3) 4_655 8_455 ?
O7 Na1 O25 78.8(3) . 8_455 ?
O18 Na1 O25 134.6(3) . 8_455 ?
O26 Na2 O27 109.4(4) . 2_756 ?
O26 Na2 O15 98.2(3) . . ?
O27 Na2 O15 129.1(4) 2_756 . ?
O26 Na2 O27 76.6(4) . . ?
O27 Na2 O27 72.4(6) 2_756 . ?
O15 Na2 O27 73.6(4) . . ?
O26 Na2 O25 145.0(4) . . ?
O27 Na2 O25 88.5(4) 2_756 . ?
O15 Na2 O25 92.6(3) . . ?
O27 Na2 O25 138.4(4) . . ?
O26 Na2 O24 77.8(3) . . ?
O27 Na2 O24 144.4(4) 2_756 . ?
O15 Na2 O24 81.9(3) . . ?
O27 Na2 O24 141.4(4) . . ?
O25 Na2 O24 70.8(3) . . ?
O6 S1 O5 112.2(5) . . ?
O6 S1 O7 112.8(5) . . ?
O5 S1 O7 110.9(4) . . ?
O6 S1 C3 106.9(4) . . ?
O5 S1 C3 107.0(4) . . ?
O7 S1 C3 106.7(4) . . ?
O8 S2 O10 110.9(5) . . ?
O8 S2 O9 111.6(5) . . ?
O10 S2 O9 112.5(5) . . ?
O8 S2 C10 107.8(5) . . ?
O10 S2 C10 106.9(5) . . ?
O9 S2 C10 106.9(4) . . ?
O13 S3 O11 114.4(5) . . ?
O13 S3 O12 110.1(4) . . ?
O11 S3 O12 111.1(4) . . ?
O13 S3 C17 108.0(4) . . ?
O11 S3 C17 108.0(4) . . ?
O12 S3 C17 104.8(4) . . ?
O15 S4 O16 115.4(5) . . ?
O15 S4 O14 114.2(4) . . ?
O16 S4 O14 105.1(4) . . ?
O15 S4 C24 107.4(4) . . ?
O16 S4 C24 109.0(4) . . ?
O14 S4 C24 105.3(4) . . ?
O15 S4 Tb 131.8(3) . 4_655 ?
O16 S4 Tb 56.9(3) . 4_655 ?
O14 S4 Tb 48.2(3) . 4_655 ?
C24 S4 Tb 120.2(3) . 4_655 ?
C2 C1 C6 118.1(8) . . ?
C2 C1 C28 120.2(8) . . ?
C6 C1 C28 121.7(8) . . ?
C3 C2 C1 122.1(8) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.1(8) . . ?
C2 C3 S1 121.9(7) . . ?
C4 C3 S1 119.1(7) . . ?
C5 C4 C3 121.1(8) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 118.1(8) . . ?
C4 C5 C7 121.8(8) . . ?
C6 C5 C7 119.8(8) . . ?
O1 C6 C1 123.3(8) . . ?
O1 C6 C5 115.1(7) . . ?
C1 C6 C5 121.6(8) . . ?
C5 C7 C8 110.5(7) . . ?
C5 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C5 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C13 118.4(8) . . ?
C9 C8 C7 119.6(8) . . ?
C13 C8 C7 122.0(8) . . ?
C8 C9 C10 121.3(8) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C11 C10 C9 118.7(8) . . ?
C11 C10 S2 120.6(7) . . ?
C9 C10 S2 120.8(7) . . ?
C10 C11 C12 120.5(8) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.5(8) . . ?
C13 C12 C14 121.3(8) . . ?
C11 C12 C14 119.2(8) . . ?
C12 C13 O2 117.3(8) . . ?
C12 C13 C8 121.3(8) . . ?
O2 C13 C8 121.4(7) . . ?
C15 C14 C12 111.3(7) . . ?
C15 C14 H14A 109.4 . . ?
C12 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C12 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 118.4(9) . . ?
C16 C15 C14 121.1(8) . . ?
C20 C15 C14 120.5(8) . . ?
C15 C16 C17 120.8(8) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.4(8) . . ?
C18 C17 S3 123.1(7) . . ?
C16 C17 S3 116.4(7) . . ?
C17 C18 C19 120.0(9) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 C21 120.9(8) . . ?
C18 C19 C21 120.4(8) . . ?
O3 C20 C15 115.9(8) . . ?
O3 C20 C19 122.5(7) . . ?
C15 C20 C19 121.5(8) . . ?
C19 C21 C22 111.3(7) . . ?
C19 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
C19 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 C27 120.8(8) . . ?
C23 C22 C21 118.8(8) . . ?
C27 C22 C21 120.3(8) . . ?
C22 C23 C24 120.2(9) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 120.2(8) . . ?
C25 C24 S4 118.5(7) . . ?
C23 C24 S4 121.1(7) . . ?
C24 C25 C26 120.8(8) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 118.7(8) . . ?
C25 C26 C28 119.7(8) . . ?
C27 C26 C28 121.6(8) . . ?
O4 C27 C22 121.5(7) . . ?
O4 C27 C26 119.3(7) . . ?
C22 C27 C26 119.2(8) . . ?
C1 C28 C26 113.9(7) . . ?
C1 C28 H28A 108.8 . . ?
C26 C28 H28A 108.8 . . ?
C1 C28 H28B 108.8 . . ?
C26 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 N1 121.3(11) . . ?
C30 C29 H29 119.4 . . ?
N1 C29 H29 119.4 . . ?
N2 C30 C29 119.7(11) . . ?
N2 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 N1 121.1(13) . . ?
C32 C31 H31 119.5 . . ?
N1 C31 H31 119.5 . . ?
C31 C32 N2 123.1(14) . . ?
C31 C32 H32 118.4 . . ?
N2 C32 H32 118.4 . . ?
O17 N1 C29 119.6(14) . . ?
O17 N1 C31 124.6(14) . . ?
C29 N1 C31 115.7(12) . . ?
O18 N2 C30 119.0(11) . . ?
O18 N2 C32 122.0(12) . . ?
C30 N2 C32 119.0(11) . . ?
C6 O1 H1 109.5 . . ?
C13 O2 H2A 109.5 . . ?
C20 O3 H3 109.5 . . ?
C27 O4 Tb 139.8(5) . . ?
S1 O7 Na1 124.2(4) . . ?
S2 O8 Na1 165.1(5) . . ?
S3 O12 Tb 147.1(4) . 7_646 ?
S4 O14 Tb 104.6(3) . 4_655 ?
S4 O15 Na2 151.0(5) . . ?
S4 O16 Tb 95.0(3) . 4_655 ?
N2 O18 Na1 122.6(7) . . ?
Na2 O25 Na1 106.9(4) . 8_556 ?
Na2 O27 Na2 104.2(5) 2_756 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb O4 2.267(6) . ?
Tb O12 2.296(6) 7_646 ?
Tb O21 2.367(6) . ?
Tb O20 2.387(6) . ?
Tb O22 2.390(6) . ?
Tb O19 2.393(7) . ?
Tb O14 2.410(6) 4_645 ?
Tb O16 2.631(7) 4_645 ?
Tb S4 3.129(3) 4_645 ?
Na1 O8 2.798(9) . ?
Na1 O28 2.848(13) . ?
Na1 O23 2.862(11) 4_655 ?
Na1 O7 2.894(9) . ?
Na1 O18 2.904(11) . ?
Na1 O25 2.937(12) 8_455 ?
Na2 O26 2.745(12) . ?
Na2 O27 2.769(16) 2_756 ?
Na2 O15 2.793(8) . ?
Na2 O27 2.810(16) . ?
Na2 O25 2.822(14) . ?
Na2 O24 2.901(11) . ?
S1 O6 1.437(7) . ?
S1 O5 1.452(8) . ?
S1 O7 1.471(7) . ?
S1 C3 1.754(9) . ?
S2 O8 1.435(8) . ?
S2 O10 1.439(8) . ?
S2 O9 1.470(7) . ?
S2 C10 1.745(9) . ?
S3 O13 1.434(7) . ?
S3 O11 1.436(7) . ?
S3 O12 1.473(6) . ?
S3 C17 1.755(9) . ?
S4 O15 1.427(7) . ?
S4 O16 1.480(7) . ?
S4 O14 1.480(7) . ?
S4 C24 1.745(9) . ?
S4 Tb 3.129(3) 4_655 ?
C1 C2 1.372(12) . ?
C1 C6 1.388(12) . ?
C1 C28 1.508(12) . ?
C2 C3 1.371(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.401(12) . ?
C4 C5 1.366(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(11) . ?
C5 C7 1.503(11) . ?
C6 O1 1.369(10) . ?
C7 C8 1.510(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.385(12) . ?
C8 C13 1.388(12) . ?
C9 C10 1.391(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(13) . ?
C11 C12 1.399(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.361(12) . ?
C12 C14 1.546(12) . ?
C13 O2 1.371(10) . ?
C14 C15 1.506(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.373(13) . ?
C15 C20 1.386(12) . ?
C16 C17 1.382(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(12) . ?
C18 C19 1.387(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(12) . ?
C19 C21 1.514(11) . ?
C20 O3 1.364(10) . ?
C21 C22 1.555(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.369(13) . ?
C22 C27 1.396(12) . ?
C23 C24 1.389(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(12) . ?
C25 C26 1.394(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.422(11) . ?
C26 C28 1.509(12) . ?
C27 O4 1.333(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.358(15) . ?
C29 N1 1.358(15) . ?
C29 H29 0.9300 . ?
C30 N2 1.322(14) . ?
C30 H30 0.9300 . ?
C31 C32 1.27(2) . ?
C31 N1 1.392(19) . ?
C31 H31 0.9300 . ?
C32 N2 1.330(16) . ?
C32 H32 0.9300 . ?
N1 O17 1.293(14) . ?
N2 O18 1.305(12) . ?
O1 H1 0.8200 . ?
O2 H2A 0.8200 . ?
O3 H3 0.8200 . ?
O12 Tb 2.296(6) 7_646 ?
O14 Tb 2.410(6) 4_655 ?
O16 Tb 2.631(7) 4_655 ?
O23 Na1 2.862(11) 4_645 ?
O25 Na1 2.937(12) 8_556 ?
O27 Na2 2.769(16) 2_756 ?
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
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.9(13) . . . . ?
C28 C1 C2 C3 179.8(8) . . . . ?
C1 C2 C3 C4 1.3(13) . . . . ?
C1 C2 C3 S1 -178.1(7) . . . . ?
O6 S1 C3 C2 -32.7(9) . . . . ?
O5 S1 C3 C2 87.6(8) . . . . ?
O7 S1 C3 C2 -153.6(8) . . . . ?
O6 S1 C3 C4 147.9(8) . . . . ?
O5 S1 C3 C4 -91.7(8) . . . . ?
O7 S1 C3 C4 27.0(9) . . . . ?
C2 C3 C4 C5 -1.1(13) . . . . ?
S1 C3 C4 C5 178.3(7) . . . . ?
C3 C4 C5 C6 0.6(13) . . . . ?
C3 C4 C5 C7 174.2(8) . . . . ?
C2 C1 C6 O1 179.8(8) . . . . ?
C28 C1 C6 O1 -0.9(13) . . . . ?
C2 C1 C6 C5 0.3(13) . . . . ?
C28 C1 C6 C5 179.6(8) . . . . ?
C4 C5 C6 O1 -179.7(7) . . . . ?
C7 C5 C6 O1 6.5(11) . . . . ?
C4 C5 C6 C1 -0.2(12) . . . . ?
C7 C5 C6 C1 -174.0(8) . . . . ?
C4 C5 C7 C8 -102.1(10) . . . . ?
C6 C5 C7 C8 71.4(10) . . . . ?
C5 C7 C8 C9 70.4(10) . . . . ?
C5 C7 C8 C13 -110.5(9) . . . . ?
C13 C8 C9 C10 2.9(13) . . . . ?
C7 C8 C9 C10 -177.9(8) . . . . ?
C8 C9 C10 C11 0.7(13) . . . . ?
C8 C9 C10 S2 -178.5(7) . . . . ?
O8 S2 C10 C11 158.7(8) . . . . ?
O10 S2 C10 C11 39.5(9) . . . . ?
O9 S2 C10 C11 -81.2(8) . . . . ?
O8 S2 C10 C9 -22.0(9) . . . . ?
O10 S2 C10 C9 -141.3(8) . . . . ?
O9 S2 C10 C9 98.0(8) . . . . ?
C9 C10 C11 C12 -2.2(13) . . . . ?
S2 C10 C11 C12 177.1(7) . . . . ?
C10 C11 C12 C13 0.0(13) . . . . ?
C10 C11 C12 C14 177.4(8) . . . . ?
C11 C12 C13 O2 -175.9(7) . . . . ?
C14 C12 C13 O2 6.8(12) . . . . ?
C11 C12 C13 C8 3.8(13) . . . . ?
C14 C12 C13 C8 -173.5(8) . . . . ?
C9 C8 C13 C12 -5.2(12) . . . . ?
C7 C8 C13 C12 175.6(8) . . . . ?
C9 C8 C13 O2 174.5(8) . . . . ?
C7 C8 C13 O2 -4.7(12) . . . . ?
C13 C12 C14 C15 108.5(10) . . . . ?
C11 C12 C14 C15 -68.9(10) . . . . ?
C12 C14 C15 C16 102.5(10) . . . . ?
C12 C14 C15 C20 -75.3(11) . . . . ?
C20 C15 C16 C17 0.8(13) . . . . ?
C14 C15 C16 C17 -177.0(8) . . . . ?
C15 C16 C17 C18 -1.2(13) . . . . ?
C15 C16 C17 S3 -177.8(7) . . . . ?
O13 S3 C17 C18 120.3(8) . . . . ?
O11 S3 C17 C18 -3.9(9) . . . . ?
O12 S3 C17 C18 -122.4(8) . . . . ?
O13 S3 C17 C16 -63.1(8) . . . . ?
O11 S3 C17 C16 172.7(7) . . . . ?
O12 S3 C17 C16 54.2(8) . . . . ?
C16 C17 C18 C19 2.5(13) . . . . ?
S3 C17 C18 C19 178.9(7) . . . . ?
C17 C18 C19 C20 -3.4(13) . . . . ?
C17 C18 C19 C21 177.8(8) . . . . ?
C16 C15 C20 O3 179.2(8) . . . . ?
C14 C15 C20 O3 -3.0(12) . . . . ?
C16 C15 C20 C19 -1.8(13) . . . . ?
C14 C15 C20 C19 176.0(8) . . . . ?
C18 C19 C20 O3 -177.9(8) . . . . ?
C21 C19 C20 O3 0.9(13) . . . . ?
C18 C19 C20 C15 3.1(13) . . . . ?
C21 C19 C20 C15 -178.1(8) . . . . ?
C20 C19 C21 C22 77.5(10) . . . . ?
C18 C19 C21 C22 -103.7(9) . . . . ?
C19 C21 C22 C23 77.7(10) . . . . ?
C19 C21 C22 C27 -99.7(9) . . . . ?
C27 C22 C23 C24 1.8(13) . . . . ?
C21 C22 C23 C24 -175.6(8) . . . . ?
C22 C23 C24 C25 -1.8(13) . . . . ?
C22 C23 C24 S4 174.2(7) . . . . ?
O15 S4 C24 C25 177.8(7) . . . . ?
O16 S4 C24 C25 -56.5(8) . . . . ?
O14 S4 C24 C25 55.7(8) . . . . ?
Tb S4 C24 C25 5.6(8) 4_655 . . . ?
O15 S4 C24 C23 1.8(9) . . . . ?
O16 S4 C24 C23 127.4(8) . . . . ?
O14 S4 C24 C23 -120.3(8) . . . . ?
Tb S4 C24 C23 -170.5(6) 4_655 . . . ?
C23 C24 C25 C26 1.0(13) . . . . ?
S4 C24 C25 C26 -175.1(6) . . . . ?
C24 C25 C26 C27 -0.2(12) . . . . ?
C24 C25 C26 C28 178.1(8) . . . . ?
C23 C22 C27 O4 -179.0(8) . . . . ?
C21 C22 C27 O4 -1.6(12) . . . . ?
C23 C22 C27 C26 -1.0(12) . . . . ?
C21 C22 C27 C26 176.4(7) . . . . ?
C25 C26 C27 O4 178.2(7) . . . . ?
C28 C26 C27 O4 0.0(11) . . . . ?
C25 C26 C27 C22 0.2(11) . . . . ?
C28 C26 C27 C22 -178.1(7) . . . . ?
C2 C1 C28 C26 104.8(9) . . . . ?
C6 C1 C28 C26 -74.5(11) . . . . ?
C25 C26 C28 C1 -79.4(10) . . . . ?
C27 C26 C28 C1 98.9(9) . . . . ?
N1 C29 C30 N2 -2.6(16) . . . . ?
N1 C31 C32 N2 2(2) . . . . ?
C30 C29 N1 O17 -177.7(11) . . . . ?
C30 C29 N1 C31 0.3(16) . . . . ?
C32 C31 N1 O17 178.0(12) . . . . ?
C32 C31 N1 C29 0.1(18) . . . . ?
C29 C30 N2 O18 -177.8(10) . . . . ?
C29 C30 N2 C32 4.4(15) . . . . ?
C31 C32 N2 O18 178.1(12) . . . . ?
C31 C32 N2 C30 -4.2(19) . . . . ?
C22 C27 O4 Tb -93.0(9) . . . . ?
C26 C27 O4 Tb 89.0(9) . . . . ?
O12 Tb O4 C27 106.9(8) 7_646 . . . ?
O21 Tb O4 C27 -112.8(8) . . . . ?
O20 Tb O4 C27 -41.4(8) . . . . ?
O22 Tb O4 C27 30.8(8) . . . . ?
O19 Tb O4 C27 179.8(8) . . . . ?
O14 Tb O4 C27 -17.8(10) 4_645 . . . ?
O16 Tb O4 C27 154.2(7) 4_645 . . . ?
S4 Tb O4 C27 70(6) 4_645 . . . ?
O6 S1 O7 Na1 -52.8(6) . . . . ?
O5 S1 O7 Na1 -179.7(4) . . . . ?
C3 S1 O7 Na1 64.2(5) . . . . ?
O8 Na1 O7 S1 -81.8(6) . . . . ?
O28 Na1 O7 S1 -162.2(5) . . . . ?
O23 Na1 O7 S1 57.4(5) 4_655 . . . ?
O18 Na1 O7 S1 -19.8(5) . . . . ?
O25 Na1 O7 S1 117.0(5) 8_455 . . . ?
O10 S2 O8 Na1 106(2) . . . . ?
O9 S2 O8 Na1 -128(2) . . . . ?
C10 S2 O8 Na1 -11(3) . . . . ?
O28 Na1 O8 S2 110(2) . . . . ?
O23 Na1 O8 S2 -115(2) 4_655 . . . ?
O7 Na1 O8 S2 26(3) . . . . ?
O18 Na1 O8 S2 -41(2) . . . . ?
O25 Na1 O8 S2 174(2) 8_455 . . . ?
O13 S3 O12 Tb -89.5(8) . . . 7_646 ?
O11 S3 O12 Tb 38.3(8) . . . 7_646 ?
C17 S3 O12 Tb 154.6(7) . . . 7_646 ?
O15 S4 O14 Tb 125.4(4) . . . 4_655 ?
O16 S4 O14 Tb -2.1(4) . . . 4_655 ?
C24 S4 O14 Tb -117.1(4) . . . 4_655 ?
O16 S4 O15 Na2 -51.8(10) . . . . ?
O14 S4 O15 Na2 -173.7(8) . . . . ?
C24 S4 O15 Na2 69.9(10) . . . . ?
Tb S4 O15 Na2 -119.1(7) 4_655 . . . ?
O26 Na2 O15 S4 -73.0(9) . . . . ?
O27 Na2 O15 S4 163.8(9) 2_756 . . . ?
O27 Na2 O15 S4 -146.4(10) . . . . ?
O25 Na2 O15 S4 73.6(9) . . . . ?
O24 Na2 O15 S4 3.4(9) . . . . ?
O15 S4 O16 Tb -124.9(4) . . . 4_655 ?
O14 S4 O16 Tb 1.8(4) . . . 4_655 ?
C24 S4 O16 Tb 114.2(4) . . . 4_655 ?
C30 N2 O18 Na1 -50.1(12) . . . . ?
C32 N2 O18 Na1 127.6(10) . . . . ?
O8 Na1 O18 N2 -32.0(8) . . . . ?
O28 Na1 O18 N2 -83.0(10) . . . . ?
O23 Na1 O18 N2 77.3(8) 4_655 . . . ?
O7 Na1 O18 N2 -170.4(8) . . . . ?
O25 Na1 O18 N2 118.9(8) 8_455 . . . ?
O26 Na2 O25 Na1 -179.7(5) . . . 8_556 ?
O27 Na2 O25 Na1 -57.0(5) 2_756 . . 8_556 ?
O15 Na2 O25 Na1 72.0(3) . . . 8_556 ?
O27 Na2 O25 Na1 3.9(7) . . . 8_556 ?
O24 Na2 O25 Na1 152.5(4) . . . 8_556 ?
O26 Na2 O27 Na2 95.5(5) . . . 2_756 ?
O27 Na2 O27 Na2 -20.2(7) 2_756 . . 2_756 ?
O15 Na2 O27 Na2 -161.7(6) . . . 2_756 ?
O25 Na2 O27 Na2 -86.7(7) . . . 2_756 ?
O24 Na2 O27 Na2 145.4(4) . . . 2_756 ?
