#------------------------------------------------------------------------------
#$Date: 2016-11-11 08:38:39 +0200 (Fri, 11 Nov 2016) $
#$Revision: 188395 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/70/7227083.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_7227083
loop_
_publ_author_name
'D'Vries, Richard Fernando'
'Gómez, Germán'
'Lionello, Diego E.'
'Fuertes, Cecilia'
'Soler-Illia, Galo'
'Ellena, Javier A.'
_publ_section_title
;
 Luminescence, Chemical Sensing and Mechanical Properties of Crystalline
 Materials Based on Lanthanide-Sulfonate Coordination Polymers
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23516F
_journal_year                    2016
_chemical_formula_moiety         'C44 H28 N4 O15 S4 Tb2, 3(H2 O)'
_chemical_formula_sum            'C44 H34 N4 O18 S4 Tb2'
_chemical_formula_weight         1352.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.088(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2636(6)
_cell_length_b                   17.0354(7)
_cell_length_c                   18.9491(7)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.28
_cell_volume                     4546.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            140387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.493
_diffrn_reflns_theta_min         1.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.354
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1206 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8208.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       needle
_exptl_crystal_F_000             2656
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0325P)²+14.2315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6857
_reflns_number_total             9363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra23516f2.cif
_cod_data_source_block           Phase3-Tb
_cod_database_code               7227083
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B,O17,H17A,H17B,O18,H18A,H18B)
2.b Rotating group:
 O15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
C1 C -0.2375(4) 0.2606(3) 0.2539(3) 0.0231(12) Uani 1 1 d .
C2 C -0.2089(4) 0.2680(3) 0.3256(3) 0.0260(12) Uani 1 1 d .
H2 H -0.1936 0.3171 0.3456 0.031 Uiso 1 1 calc R
C3 C -0.2028(4) 0.2007(3) 0.3693(3) 0.0253(12) Uani 1 1 d .
C4 C -0.6752(4) 0.2934(4) -0.0554(3) 0.0300(13) Uani 1 1 d .
H4 H -0.6637 0.2445 -0.0341 0.036 Uiso 1 1 calc R
C5 C -0.6657(4) 0.3596(4) -0.0144(3) 0.0289(13) Uani 1 1 d .
C6 C -0.6797(5) 0.4342(4) -0.0464(3) 0.0361(15) Uani 1 1 d .
H6 H -0.6700 0.4791 -0.0182 0.043 Uiso 1 1 calc R
C7 C -0.2072(5) 0.0588(4) 0.3818(3) 0.0364(15) Uani 1 1 d .
H7 H -0.2171 0.0092 0.3615 0.044 Uiso 1 1 calc R
C8 C -0.2210(4) 0.1263(3) 0.3375(3) 0.0284(13) Uani 1 1 d .
C9 C -0.2555(4) 0.1199(3) 0.2630(3) 0.0287(13) Uani 1 1 d .
H9 H -0.2695 0.0709 0.2423 0.034 Uiso 1 1 calc R
C10 C -0.2680(4) 0.1865(3) 0.2221(3) 0.0224(12) Uani 1 1 d .
C11 C -0.4111(4) 0.2852(3) -0.0385(3) 0.0237(12) Uani 1 1 d .
C12 C -0.4125(4) 0.3537(3) -0.0768(3) 0.0297(13) Uani 1 1 d .
H12 H -0.3954 0.4005 -0.0530 0.036 Uiso 1 1 calc R
C13 C -0.4392(4) 0.3541(3) -0.1514(3) 0.0276(13) Uani 1 1 d .
C14 C 0.0690(5) 0.0774(4) 0.3072(3) 0.0369(15) Uani 1 1 d .
H14 H 0.0843 0.0298 0.3301 0.044 Uiso 1 1 calc R
C15 C 0.0548(5) 0.0805(4) 0.2340(3) 0.0355(15) Uani 1 1 d .
H15 H 0.0633 0.0357 0.2076 0.043 Uiso 1 1 calc R
C16 C 0.0273(4) 0.1512(4) 0.1990(3) 0.0299(13) Uani 1 1 d .
C17 C 0.0130(4) 0.2176(4) 0.2367(3) 0.0300(13) Uani 1 1 d .
H17 H -0.0082 0.2634 0.2126 0.036 Uiso 1 1 calc R
C18 C -0.4697(4) 0.2834(4) -0.1875(3) 0.0271(13) Uani 1 1 d .
C19 C -0.4787(4) 0.2153(3) -0.1465(3) 0.0255(12) Uani 1 1 d .
H19 H -0.5042 0.1697 -0.1687 0.031 Uiso 1 1 calc R
C20 C -0.4501(4) 0.2163(3) -0.0748(3) 0.0234(12) Uani 1 1 d .
C21 C -0.4681(5) 0.3695(4) 0.2746(3) 0.0427(17) Uani 1 1 d .
H21 H -0.4716 0.4098 0.2412 0.051 Uiso 1 1 calc R
C22 C -0.4573(6) 0.3890(5) 0.3472(4) 0.054(2) Uani 1 1 d .
H22 H -0.4548 0.4412 0.3614 0.065 Uiso 1 1 calc R
C23 C -0.4505(5) 0.3303(5) 0.3967(4) 0.056(2) Uani 1 1 d .
H23 H -0.4434 0.3426 0.4450 0.067 Uiso 1 1 calc R
C24 C -0.4542(5) 0.2517(4) 0.3750(3) 0.0410(16) Uani 1 1 d .
C25 C -0.4476(5) 0.1874(5) 0.4235(4) 0.053(2) Uani 1 1 d .
H25 H -0.4382 0.1970 0.4724 0.064 Uiso 1 1 calc R
C26 C -0.4546(5) 0.1124(5) 0.3996(4) 0.0485(19) Uani 1 1 d .
H26 H -0.4484 0.0713 0.4323 0.058 Uiso 1 1 calc R
C27 C -0.4713(5) 0.0954(4) 0.3251(3) 0.0385(15) Uani 1 1 d .
C28 C -0.4860(5) 0.0190(4) 0.2974(4) 0.0501(19) Uani 1 1 d .
H28 H -0.4843 -0.0237 0.3282 0.060 Uiso 1 1 calc R
C29 C -0.5027(6) 0.0077(4) 0.2256(4) 0.054(2) Uani 1 1 d .
H29 H -0.5121 -0.0427 0.2069 0.065 Uiso 1 1 calc R
C30 C -0.5056(5) 0.0720(4) 0.1801(4) 0.0414(16) Uani 1 1 d .
H30 H -0.5169 0.0631 0.1310 0.050 Uiso 1 1 calc R
C31 C -0.4772(4) 0.1573(4) 0.2754(3) 0.0280(13) Uani 1 1 d .
C32 C -0.4686(4) 0.2367(4) 0.3001(3) 0.0289(13) Uani 1 1 d .
C33 C -0.1745(5) 0.3859(4) -0.0066(3) 0.0370(15) Uani 1 1 d .
H33 H -0.1656 0.3973 0.0419 0.044 Uiso 1 1 calc R
C34 C -0.1729(5) 0.4472(4) -0.0547(4) 0.0432(17) Uani 1 1 d .
H34 H -0.1629 0.4984 -0.0381 0.052 Uiso 1 1 calc R
C35 C -0.1863(5) 0.4323(4) -0.1267(4) 0.0431(17) Uani 1 1 d .
H35 H -0.1873 0.4732 -0.1594 0.052 Uiso 1 1 calc R
C36 C -0.1984(4) 0.3542(4) -0.1501(3) 0.0323(14) Uani 1 1 d .
C37 C -0.2107(5) 0.3337(4) -0.2243(3) 0.0430(17) Uani 1 1 d .
H37 H -0.2110 0.3730 -0.2584 0.052 Uiso 1 1 calc R
C38 C -0.2219(5) 0.2588(5) -0.2452(4) 0.0481(18) Uani 1 1 d .
H38 H -0.2307 0.2468 -0.2936 0.058 Uiso 1 1 calc R
C39 C -0.2206(5) 0.1966(4) -0.1937(3) 0.0379(15) Uani 1 1 d .
C40 C -0.2307(6) 0.1173(4) -0.2131(4) 0.052(2) Uani 1 1 d .
H40 H -0.2373 0.1028 -0.2609 0.063 Uiso 1 1 calc R
C41 C -0.2306(6) 0.0619(5) -0.1617(4) 0.053(2) Uani 1 1 d .
H41 H -0.2358 0.0090 -0.1739 0.064 Uiso 1 1 calc R
C42 C -0.2226(5) 0.0850(4) -0.0906(3) 0.0422(16) Uani 1 1 d .
H42 H -0.2244 0.0463 -0.0561 0.051 Uiso 1 1 calc R
C43 C -0.2108(4) 0.2153(4) -0.1210(3) 0.0305(13) Uani 1 1 d .
C44 C -0.1984(4) 0.2956(4) -0.0980(3) 0.0311(14) Uani 1 1 d .
O1 O -0.1866(3) 0.3105(2) 0.1379(2) 0.0308(9) Uani 1 1 d .
O2 O -0.1906(3) 0.4052(2) 0.2329(2) 0.0364(10) Uani 1 1 d .
O3 O -0.3380(3) 0.3553(2) 0.16637(19) 0.0279(9) Uani 1 1 d .
O4 O -0.5309(3) 0.3817(2) 0.0937(2) 0.0375(10) Uani 1 1 d .
O5 O -0.6279(3) 0.2701(2) 0.0983(2) 0.0298(9) Uani 1 1 d .
O6 O -0.6954(3) 0.4005(3) 0.1119(2) 0.0465(12) Uani 1 1 d .
O7 O -0.3111(3) 0.1865(2) 0.15263(18) 0.0250(8) Uani 1 1 d .
O8 O -0.3602(3) 0.1143(2) 0.0101(2) 0.0296(9) Uani 1 1 d .
O9 O -0.5062(3) 0.0729(2) -0.0631(2) 0.0313(9) Uani 1 1 d .
O10 O -0.5096(3) 0.1615(2) 0.03651(19) 0.0299(9) Uani 1 1 d .
O11 O 0.1048(3) 0.1945(3) 0.0897(2) 0.0464(12) Uani 1 1 d .
O12 O -0.0634(3) 0.2046(3) 0.0798(2) 0.0347(10) Uani 1 1 d .
O13 O 0.0086(3) 0.0760(3) 0.0790(2) 0.0422(11) Uani 1 1 d .
O14 O -0.3718(3) 0.2793(2) 0.03096(18) 0.0257(9) Uani 1 1 d .
O15 O -0.1853(3) 0.0727(2) 0.0841(2) 0.0418(11) Uani 1 1 d .
H15A H -0.1826 0.0642 0.1298 0.063 Uiso 1 1 d GR
H15B H -0.1294 0.0634 0.0728 0.063 Uiso 1 1 d GR
O16 O 0.0906(3) 0.3706(3) 0.1075(5) 0.147(4) Uani 1 1 d .
H16A H 0.0948 0.3764 0.1526 0.220 Uiso 1 1 d G
H16B H 0.1344 0.3968 0.0925 0.220 Uiso 1 1 d G
O17 O 0.7114(4) 0.9411(2) 0.0635(4) 0.0764(18) Uani 1 1 d G
H17A H 0.6875 0.9563 0.0998 0.115 Uiso 1 1 d G
H17B H 0.6910 0.9701 0.0278 0.115 Uiso 1 1 d G
O18 O 0.2730(4) 0.1149(2) 0.0735(4) 0.087(2) Uani 1 1 d G
H18A H 0.2180 0.1312 0.0786 0.130 Uiso 1 1 d G
H18B H 0.3092 0.1539 0.0700 0.130 Uiso 1 1 d G
S1 S -0.23770(10) 0.34003(8) 0.19510(7) 0.0267(3) Uani 1 1 d .
S2 S -0.63085(11) 0.35409(9) 0.07874(7) 0.0309(3) Uani 1 1 d .
S3 S -0.45735(10) 0.13365(8) -0.02012(7) 0.0251(3) Uani 1 1 d .
S4 S 0.01985(11) 0.15591(10) 0.10514(8) 0.0317(3) Uani 1 1 d .
Tb1 Tb -0.22952(2) 0.20327(2) 0.05644(2) 0.02546(8) Uani 1 1 d .
Tb2 Tb -0.45368(2) 0.25787(2) 0.12557(2) 0.02489(8) Uani 1 1 d .
N1 N -0.4735(3) 0.2953(3) 0.2515(2) 0.0275(11) Uani 1 1 d .
N2 N -0.4931(3) 0.1455(3) 0.2031(2) 0.0294(11) Uani 1 1 d .
N3 N -0.1882(3) 0.3113(3) -0.0271(2) 0.0274(11) Uani 1 1 d .
N4 N -0.2126(4) 0.1595(3) -0.0691(3) 0.0355(12) 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'
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
C2 C1 C10 121.6(5) . .
C2 C1 S1 122.2(4) . .
C10 C1 S1 116.2(4) . .
C1 C2 H2 120.3 . .
C1 C2 C3 119.5(5) . .
C3 C2 H2 120.3 . .
C2 C3 C4 120.9(5) . 4_666
C8 C3 C2 119.4(5) . .
C8 C3 C4 119.6(5) . 4_666
C3 C4 H4 120.0 4_565 .
C5 C4 C3 120.0(5) . 4_565
C5 C4 H4 120.0 . .
C4 C5 C6 120.4(5) . .
C4 C5 S2 121.0(5) . .
C6 C5 S2 118.6(4) . .
C5 C6 H6 119.7 . .
C7 C6 C5 120.6(6) 4_565 .
C7 C6 H6 119.7 4_565 .
C6 C7 H7 119.6 4_666 .
C6 C7 C8 120.7(6) 4_666 .
C8 C7 H7 119.6 . .
C3 C8 C7 118.5(5) . .
C3 C8 C9 120.2(5) . .
C7 C8 C9 121.2(5) . .
C8 C9 H9 120.3 . .
C10 C9 C8 119.5(5) . .
C10 C9 H9 120.3 . .
C9 C10 C1 119.1(5) . .
O7 C10 C1 117.7(5) . .
O7 C10 C9 123.2(5) . .
C12 C11 C20 118.2(5) . .
O14 C11 C12 123.3(5) . .
O14 C11 C20 118.5(5) . .
C11 C12 H12 119.5 . .
C11 C12 C13 121.1(5) . .
C13 C12 H12 119.5 . .
C12 C13 C14 121.8(5) . 4_565
C12 C13 C18 119.6(5) . .
C18 C13 C14 118.5(5) . 4_565
C13 C14 H14 119.5 4_666 .
C15 C14 C13 121.0(6) . 4_666
C15 C14 H14 119.5 . .
C14 C15 H15 120.1 . .
C14 C15 C16 119.9(6) . .
C16 C15 H15 120.1 . .
C15 C16 S4 118.9(4) . .
C17 C16 C15 121.0(5) . .
C17 C16 S4 119.9(5) . .
C16 C17 H17 120.0 . .
C16 C17 C18 120.1(5) . 4_666
C18 C17 H17 120.0 4_666 .
C17 C18 C13 119.4(5) 4_565 .
C19 C18 C13 118.6(5) . .
C19 C18 C17 122.0(5) . 4_565
C18 C19 H19 119.9 . .
C20 C19 C18 120.2(5) . .
C20 C19 H19 119.9 . .
C11 C20 S3 115.4(4) . .
C19 C20 C11 121.7(5) . .
C19 C20 S3 122.9(4) . .
C22 C21 H21 118.7 . .
N1 C21 H21 118.7 . .
N1 C21 C22 122.6(7) . .
C21 C22 H22 120.4 . .
C23 C22 C21 119.2(7) . .
C23 C22 H22 120.4 . .
C22 C23 H23 119.9 . .
C22 C23 C24 120.3(6) . .
C24 C23 H23 119.9 . .
C23 C24 C25 123.6(6) . .
C23 C24 C32 117.2(6) . .
C25 C24 C32 119.2(7) . .
C24 C25 H25 119.4 . .
C26 C25 C24 121.2(6) . .
C26 C25 H25 119.4 . .
C25 C26 H26 119.5 . .
C25 C26 C27 121.0(6) . .
C27 C26 H26 119.5 . .
C28 C27 C26 123.4(6) . .
C28 C27 C31 117.0(6) . .
C31 C27 C26 119.6(6) . .
C27 C28 H28 120.1 . .
C29 C28 C27 119.8(6) . .
C29 C28 H28 120.1 . .
C28 C29 H29 120.2 . .
C28 C29 C30 119.6(7) . .
C30 C29 H29 120.2 . .
C29 C30 H30 118.4 . .
N2 C30 C29 123.3(6) . .
N2 C30 H30 118.4 . .
C27 C31 C32 119.8(5) . .
N2 C31 C27 122.9(6) . .
N2 C31 C32 117.3(5) . .
C24 C32 C31 119.2(6) . .
N1 C32 C24 122.0(6) . .
N1 C32 C31 118.9(5) . .
C34 C33 H33 118.5 . .
N3 C33 H33 118.5 . .
N3 C33 C34 122.9(6) . .
C33 C34 H34 120.0 . .
C35 C34 C33 120.0(6) . .
C35 C34 H34 120.0 . .
C34 C35 H35 120.6 . .
C34 C35 C36 118.7(6) . .
C36 C35 H35 120.6 . .
C35 C36 C37 122.1(6) . .
C44 C36 C35 117.7(6) . .
C44 C36 C37 120.3(6) . .
C36 C37 H37 119.6 . .
C38 C37 C36 120.9(6) . .
C38 C37 H37 119.6 . .
C37 C38 H38 119.5 . .
C37 C38 C39 120.9(6) . .
C39 C38 H38 119.5 . .
C40 C39 C38 122.9(6) . .
C43 C39 C38 119.2(6) . .
C43 C39 C40 117.9(6) . .
C39 C40 H40 120.2 . .
C41 C40 C39 119.6(6) . .
C41 C40 H40 120.2 . .
C40 C41 H41 120.3 . .
C40 C41 C42 119.3(7) . .
C42 C41 H41 120.3 . .
C41 C42 H42 118.2 . .
N4 C42 C41 123.5(6) . .
N4 C42 H42 118.2 . .
C39 C43 C44 120.2(6) . .
N4 C43 C39 122.6(6) . .
N4 C43 C44 117.2(5) . .
C36 C44 C43 118.4(5) . .
N3 C44 C36 123.0(6) . .
N3 C44 C43 118.5(5) . .
S1 O1 Tb1 128.3(2) . .
S1 O3 Tb2 125.5(2) . .
S2 O4 Tb2 99.0(2) . .
S2 O5 Tb2 97.0(2) . .
C10 O7 Tb1 123.5(3) . .
C10 O7 Tb2 117.0(3) . .
Tb1 O7 Tb2 106.70(14) . .
S3 O8 Tb1 128.6(2) . .
S3 O10 Tb2 125.5(2) . .
S4 O12 Tb1 143.1(3) . .
C11 O14 Tb1 116.5(3) . .
C11 O14 Tb2 125.7(3) . .
Tb2 O14 Tb1 105.89(14) . .
H15A O15 H15B 108.3 . .
Tb1 O15 H15A 110.3 . .
Tb1 O15 H15B 109.9 . .
H16A O16 H16B 109.6 . .
H17A O17 H17B 109.5 . .
H18A O18 H18B 109.6 . .
O1 S1 C1 104.5(2) . .
O2 S1 C1 109.1(3) . .
O2 S1 O1 112.5(2) . .
O2 S1 O3 113.6(3) . .
O3 S1 C1 106.0(2) . .
O3 S1 O1 110.5(2) . .
C5 S2 Tb2 114.4(2) . .
O4 S2 C5 106.6(3) . .
O4 S2 Tb2 51.97(17) . .
O5 S2 C5 107.2(3) . .
O5 S2 O4 105.7(2) . .
O5 S2 Tb2 54.02(16) . .
O6 S2 C5 108.2(3) . .
O6 S2 O4 113.9(3) . .
O6 S2 O5 114.7(3) . .
O6 S2 Tb2 137.34(19) . .
O8 S3 C20 105.8(2) . .
O8 S3 O10 110.3(2) . .
O9 S3 C20 108.2(2) . .
O9 S3 O8 114.1(2) . .
O9 S3 O10 113.0(2) . .
O10 S3 C20 104.7(2) . .
O11 S4 C16 107.7(3) . .
O11 S4 O12 109.7(3) . .
O12 S4 C16 105.8(3) . .
O13 S4 C16 106.8(3) . .
O13 S4 O11 114.1(3) . .
O13 S4 O12 112.3(3) . .
O1 Tb1 O8 143.12(13) . .
O1 Tb1 Tb2 74.51(9) . .
O1 Tb1 N3 77.91(14) . .
O1 Tb1 N4 140.44(15) . .
O7 Tb1 O1 72.48(13) . .
O7 Tb1 O8 76.10(13) . .
O7 Tb1 O12 117.95(13) . .
O7 Tb1 O14 73.22(12) . .
O7 Tb1 O15 81.91(15) . .
O7 Tb1 Tb2 36.88(9) . .
O7 Tb1 N3 139.92(14) . .
O7 Tb1 N4 146.07(15) . .
O8 Tb1 Tb2 68.78(9) . .
O8 Tb1 N3 117.35(14) . .
O8 Tb1 N4 70.28(15) . .
O12 Tb1 O1 73.97(14) . .
O12 Tb1 O8 139.67(14) . .
O12 Tb1 O14 146.55(14) . .
O12 Tb1 O15 74.85(15) . .
O12 Tb1 Tb2 145.37(10) . .
O12 Tb1 N3 77.56(15) . .
O12 Tb1 N4 86.41(15) . .
O14 Tb1 O1 80.82(13) . .
O14 Tb1 O8 71.94(13) . .
O14 Tb1 Tb2 36.38(9) . .
O14 Tb1 N3 75.92(14) . .
O14 Tb1 N4 99.95(15) . .
O15 Tb1 O1 122.91(14) . .
O15 Tb1 O8 69.94(14) . .
O15 Tb1 O14 138.36(14) . .
O15 Tb1 Tb2 111.71(11) . .
O15 Tb1 N3 137.72(15) . .
O15 Tb1 N4 82.49(17) . .
N3 Tb1 Tb2 109.26(10) . .
N4 Tb1 Tb2 127.64(12) . .
N4 Tb1 N3 64.29(16) . .
O3 Tb2 O4 74.76(13) . .
O3 Tb2 O5 129.25(13) . .
O3 Tb2 O10 147.32(13) . .
O3 Tb2 S2 102.79(10) . .
O3 Tb2 Tb1 72.65(9) . .
O3 Tb2 N1 72.12(14) . .
O3 Tb2 N2 123.02(14) . .
O4 Tb2 O5 57.90(14) . .
O4 Tb2 S2 29.02(10) . .
O4 Tb2 Tb1 120.60(11) . .
O4 Tb2 N1 84.31(15) . .
O4 Tb2 N2 132.28(15) . .
O5 Tb2 S2 28.99(10) . .
O5 Tb2 Tb1 146.37(9) . .
O5 Tb2 N1 85.23(14) . .
O5 Tb2 N2 82.90(14) . .
O7 Tb2 O3 76.04(13) . .
O7 Tb2 O4 148.23(14) . .
O7 Tb2 O5 153.67(13) . .
O7 Tb2 O10 88.85(13) . .
O7 Tb2 S2 174.92(9) . .
O7 Tb2 Tb1 36.42(8) . .
O7 Tb2 N1 98.41(13) . .
O7 Tb2 N2 75.32(14) . .
O10 Tb2 O4 109.54(13) . .
O10 Tb2 O5 72.44(13) . .
O10 Tb2 S2 89.70(10) . .
O10 Tb2 Tb1 78.00(9) . .
O10 Tb2 N1 139.65(14) . .
O10 Tb2 N2 79.11(14) . .
O14 Tb2 O3 74.55(13) . .
O14 Tb2 O4 86.25(14) . .
O14 Tb2 O5 116.04(13) . .
O14 Tb2 O7 74.12(12) . .
O14 Tb2 O10 73.48(13) . .
O14 Tb2 S2 100.80(10) . .
O14 Tb2 Tb1 37.73(9) . .
O14 Tb2 N1 146.66(14) . .
O14 Tb2 N2 138.90(14) . .
S2 Tb2 Tb1 138.51(3) . .
N1 Tb2 S2 85.83(11) . .
N1 Tb2 Tb1 128.28(11) . .
N1 Tb2 N2 64.82(15) . .
N2 Tb2 S2 109.17(11) . .
N2 Tb2 Tb1 107.12(11) . .
C21 N1 C32 118.8(5) . .
C21 N1 Tb2 122.6(4) . .
C32 N1 Tb2 117.0(4) . .
C30 N2 C31 117.4(5) . .
C30 N2 Tb2 123.6(4) . .
C31 N2 Tb2 117.0(4) . .
C33 N3 C44 117.6(5) . .
C33 N3 Tb1 122.9(4) . .
C44 N3 Tb1 118.2(4) . .
C42 N4 C43 117.0(5) . .
C42 N4 Tb1 122.9(4) . .
C43 N4 Tb1 118.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.360(7) .
C1 C10 1.438(7) .
C1 S1 1.753(5) .
C2 H2 0.9300 .
C2 C3 1.409(8) .
C3 C4 1.424(7) 4_666
C3 C8 1.409(8) .
C4 C3 1.424(7) 4_565
C4 H4 0.9300 .
C4 C5 1.363(8) .
C5 C6 1.410(8) .
C5 S2 1.759(6) .
C6 H6 0.9300 .
C6 C7 1.360(8) 4_565
C7 C6 1.360(8) 4_666
C7 H7 0.9300 .
C7 C8 1.419(8) .
C8 C9 1.424(7) .
C9 H9 0.9300 .
C9 C10 1.369(8) .
C10 O7 1.362(6) .
C11 C12 1.372(8) .
C11 C20 1.428(8) .
C11 O14 1.350(6) .
C12 H12 0.9300 .
C12 C13 1.405(7) .
C13 C14 1.421(8) 4_565
C13 C18 1.419(8) .
C14 C13 1.421(8) 4_666
C14 H14 0.9300 .
C14 C15 1.371(8) .
C15 H15 0.9300 .
C15 C16 1.402(8) .
C16 C17 1.371(8) .
C16 S4 1.766(5) .
C17 H17 0.9300 .
C17 C18 1.417(7) 4_666
C18 C17 1.417(7) 4_565
C18 C19 1.415(8) .
C19 H19 0.9300 .
C19 C20 1.355(7) .
C20 S3 1.760(5) .
C21 H21 0.9300 .
C21 C22 1.399(9) .
C21 N1 1.335(8) .
C22 H22 0.9300 .
C22 C23 1.363(11) .
C23 H23 0.9300 .
C23 C24 1.399(10) .
C24 C25 1.423(10) .
C24 C32 1.425(8) .
C25 H25 0.9300 .
C25 C26 1.354(11) .
C26 H26 0.9300 .
C26 C27 1.423(9) .
C27 C28 1.407(10) .
C27 C31 1.408(8) .
C28 H28 0.9300 .
C28 C29 1.358(10) .
C29 H29 0.9300 .
C29 C30 1.390(9) .
C30 H30 0.9300 .
C30 N2 1.329(8) .
C31 C32 1.430(8) .
C31 N2 1.368(7) .
C32 N1 1.353(7) .
C33 H33 0.9300 .
C33 C34 1.389(9) .
C33 N3 1.333(8) .
C34 H34 0.9300 .
C34 C35 1.370(9) .
C35 H35 0.9300 .
C35 C36 1.406(9) .
C36 C37 1.431(9) .
C36 C44 1.405(8) .
C37 H37 0.9300 .
C37 C38 1.338(10) .
C38 H38 0.9300 .
C38 C39 1.439(9) .
C39 C40 1.401(10) .
C39 C43 1.399(8) .
C40 H40 0.9300 .
C40 C41 1.356(10) .
C41 H41 0.9300 .
C41 C42 1.391(9) .
C42 H42 0.9300 .
C42 N4 1.334(8) .
C43 C44 1.438(9) .
C43 N4 1.370(8) .
C44 N3 1.355(7) .
O1 S1 1.486(4) .
O1 Tb1 2.408(4) .
O2 S1 1.430(4) .
O3 S1 1.471(4) .
O3 Tb2 2.381(4) .
O4 S2 1.486(4) .
O4 Tb2 2.413(4) .
O5 S2 1.477(4) .
O5 Tb2 2.466(4) .
O6 S2 1.432(4) .
O7 Tb1 2.330(4) .
O7 Tb2 2.355(4) .
O8 S3 1.451(4) .
O8 Tb1 2.455(4) .
O9 S3 1.430(4) .
O10 S3 1.478(4) .
O10 Tb2 2.399(4) .
O11 S4 1.449(5) .
O12 S4 1.466(4) .
O12 Tb1 2.340(4) .
O13 S4 1.449(5) .
O14 Tb1 2.392(4) .
O14 Tb2 2.318(4) .
O15 H15A 0.8733 .
O15 H15B 0.8715 .
O15 Tb1 2.349(4) .
O16 H16A 0.8530 .
O16 H16B 0.8522 .
O17 H17A 0.8537 .
O17 H17B 0.8515 .
O18 H18A 0.8516 .
O18 H18B 0.8512 .
S2 Tb2 3.0252(15) .
Tb1 Tb2 3.7587(4) .
Tb1 N3 2.556(5) .
Tb1 N4 2.541(5) .
Tb2 N1 2.529(4) .
Tb2 N2 2.530(5) .
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_4
C1 C2 C3 C4 -178.6(5) . 4_666
C1 C2 C3 C8 3.7(8) . .
C1 C10 O7 Tb1 75.0(5) . .
C1 C10 O7 Tb2 -61.3(5) . .
C2 C1 C10 C9 -9.3(8) . .
C2 C1 C10 O7 168.6(5) . .
C2 C1 S1 O1 129.6(5) . .
C2 C1 S1 O2 9.1(6) . .
C2 C1 S1 O3 -113.6(5) . .
C2 C3 C8 C7 175.1(6) . .
C2 C3 C8 C9 -7.0(9) . .
C3 C4 C5 C6 -2.3(9) 4_565 .
C3 C4 C5 S2 -179.5(4) 4_565 .
C3 C8 C9 C10 2.0(9) . .
C4 C3 C8 C7 -2.7(9) 4_666 .
C4 C3 C8 C9 175.3(5) 4_666 .
C4 C5 C6 C7 3.1(10) . 4_565
C4 C5 S2 O4 106.3(5) . .
C4 C5 S2 O5 -6.6(6) . .
C4 C5 S2 O6 -130.8(5) . .
C4 C5 S2 Tb2 51.1(5) . .
C6 C5 S2 O4 -71.0(5) . .
C6 C5 S2 O5 176.1(5) . .
C6 C5 S2 O6 51.9(6) . .
C6 C5 S2 Tb2 -126.2(5) . .
C6 C7 C8 C3 1.9(10) 4_666 .
C6 C7 C8 C9 -176.0(6) 4_666 .
C7 C8 C9 C10 180.0(6) . .
C8 C9 C10 C1 5.9(8) . .
C8 C9 C10 O7 -171.9(5) . .
C9 C10 O7 Tb1 -107.2(5) . .
C9 C10 O7 Tb2 116.5(5) . .
C10 C1 C2 C3 4.4(8) . .
C10 C1 S1 O1 -49.6(5) . .
C10 C1 S1 O2 -170.1(4) . .
C10 C1 S1 O3 67.2(5) . .
C11 C12 C13 C14 -172.9(6) . 4_565
C11 C12 C13 C18 3.0(9) . .
C11 C20 S3 O8 -63.0(5) . .
C11 C20 S3 O9 174.2(4) . .
C11 C20 S3 O10 53.5(5) . .
C12 C11 C20 C19 6.9(8) . .
C12 C11 C20 S3 -173.5(4) . .
C12 C11 O14 Tb1 -110.6(5) . .
C12 C11 O14 Tb2 112.2(5) . .
C12 C13 C18 C17 -173.4(5) . 4_565
C12 C13 C18 C19 4.4(8) . .
C13 C14 C15 C16 -3.0(10) 4_666 .
C13 C18 C19 C20 -6.1(8) . .
C14 C13 C18 C17 2.6(8) 4_565 4_565
C14 C13 C18 C19 -179.5(5) 4_565 .
C14 C15 C16 C17 -1.0(10) . .
C14 C15 C16 S4 174.4(5) . .
C15 C16 C17 C18 3.1(9) . 4_666
C15 C16 S4 O11 -101.0(5) . .
C15 C16 S4 O12 141.7(5) . .
C15 C16 S4 O13 21.9(6) . .
C17 C16 S4 O11 74.4(6) . .
C17 C16 S4 O12 -42.9(6) . .
C17 C16 S4 O13 -162.6(5) . .
C17 C18 C19 C20 171.7(5) 4_565 .
C18 C19 C20 C11 0.5(8) . .
C18 C19 C20 S3 -179.1(4) . .
C19 C20 S3 O8 116.6(5) . .
C19 C20 S3 O9 -6.1(6) . .
C19 C20 S3 O10 -126.9(5) . .
C20 C11 C12 C13 -8.6(8) . .
C20 C11 O14 Tb1 67.0(5) . .
C20 C11 O14 Tb2 -70.3(6) . .
C21 C22 C23 C24 0.1(12) . .
C22 C21 N1 C32 0.1(10) . .
C22 C21 N1 Tb2 -165.0(5) . .
C22 C23 C24 C25 180.0(7) . .
C22 C23 C24 C32 -2.2(11) . .
C23 C24 C25 C26 177.9(7) . .
C23 C24 C32 C31 -177.2(6) . .
C23 C24 C32 N1 3.5(10) . .
C24 C25 C26 C27 -1.6(11) . .
C24 C32 N1 C21 -2.5(9) . .
C24 C32 N1 Tb2 163.5(5) . .
C25 C24 C32 C31 0.7(9) . .
C25 C24 C32 N1 -178.6(6) . .
C25 C26 C27 C28 -175.2(7) . .
C25 C26 C27 C31 2.3(10) . .
C26 C27 C28 C29 179.2(7) . .
C26 C27 C31 C32 -1.5(9) . .
C26 C27 C31 N2 -180.0(6) . .
C27 C28 C29 C30 -0.4(12) . .
C27 C31 C32 C24 0.0(9) . .
C27 C31 C32 N1 179.3(5) . .
C27 C31 N2 C30 1.7(9) . .
C27 C31 N2 Tb2 -162.6(4) . .
C28 C27 C31 C32 176.2(6) . .
C28 C27 C31 N2 -2.2(9) . .
C28 C29 C30 N2 -0.2(12) . .
C29 C30 N2 C31 -0.4(10) . .
C29 C30 N2 Tb2 162.7(5) . .
C31 C27 C28 C29 1.5(10) . .
C31 C32 N1 C21 178.2(6) . .
C31 C32 N1 Tb2 -15.8(7) . .
C32 C24 C25 C26 0.1(11) . .
C32 C31 N2 C30 -176.8(5) . .
C32 C31 N2 Tb2 18.9(6) . .
C33 C34 C35 C36 -1.9(10) . .
C34 C33 N3 C44 1.7(9) . .
C34 C33 N3 Tb1 -165.3(5) . .
C34 C35 C36 C37 -178.7(6) . .
C34 C35 C36 C44 1.5(9) . .
C35 C36 C37 C38 179.8(6) . .
C35 C36 C44 C43 180.0(6) . .
C35 C36 C44 N3 0.6(9) . .
C36 C37 C38 C39 -0.8(11) . .
C36 C44 N3 C33 -2.2(9) . .
C36 C44 N3 Tb1 165.5(4) . .
C37 C36 C44 C43 0.1(9) . .
C37 C36 C44 N3 -179.2(6) . .
C37 C38 C39 C40 -179.0(7) . .
C37 C38 C39 C43 2.2(10) . .
C38 C39 C40 C41 -178.7(7) . .
C38 C39 C43 C44 -2.4(9) . .
C38 C39 C43 N4 177.4(6) . .
C39 C40 C41 C42 1.4(12) . .
C39 C43 C44 C36 1.3(9) . .
C39 C43 C44 N3 -179.3(5) . .
C39 C43 N4 C42 1.2(9) . .
C39 C43 N4 Tb1 -167.0(5) . .
C40 C39 C43 C44 178.8(6) . .
C40 C39 C43 N4 -1.4(10) . .
C40 C41 C42 N4 -1.7(12) . .
C41 C42 N4 C43 0.3(10) . .
C41 C42 N4 Tb1 168.0(5) . .
C43 C39 C40 C41 0.0(11) . .
C43 C44 N3 C33 178.5(5) . .
C43 C44 N3 Tb1 -13.9(7) . .
C44 C36 C37 C38 -0.4(10) . .
C44 C43 N4 C42 -179.0(6) . .
C44 C43 N4 Tb1 12.8(7) . .
O14 C11 C12 C13 169.0(5) . .
O14 C11 C20 C19 -170.8(5) . .
O14 C11 C20 S3 8.9(7) . .
S1 C1 C2 C3 -174.7(4) . .
S1 C1 C10 C9 169.8(4) . .
S1 C1 C10 O7 -12.3(6) . .
S2 C5 C6 C7 -179.6(5) . 4_565
S4 C16 C17 C18 -172.2(4) . 4_666
Tb1 O1 S1 C1 61.8(3) . .
Tb1 O1 S1 O2 -180.0(3) . .
Tb1 O1 S1 O3 -51.8(3) . .
Tb1 O8 S3 C20 41.2(3) . .
Tb1 O8 S3 O9 160.1(2) . .
Tb1 O8 S3 O10 -71.5(3) . .
Tb1 O12 S4 C16 -77.1(4) . .
Tb1 O12 S4 O11 166.9(4) . .
Tb1 O12 S4 O13 39.0(5) . .
Tb2 O3 S1 C1 -44.3(3) . .
Tb2 O3 S1 O1 68.4(3) . .
Tb2 O3 S1 O2 -164.1(2) . .
Tb2 O4 S2 C5 -108.4(2) . .
Tb2 O4 S2 O5 5.5(2) . .
Tb2 O4 S2 O6 132.4(2) . .
Tb2 O5 S2 C5 108.1(2) . .
Tb2 O5 S2 O4 -5.3(2) . .
Tb2 O5 S2 O6 -131.8(2) . .
Tb2 O10 S3 C20 -65.7(3) . .
Tb2 O10 S3 O8 47.7(3) . .
Tb2 O10 S3 O9 176.8(2) . .
N1 C21 C22 C23 1.1(12) . .
N2 C31 C32 C24 178.6(5) . .
N2 C31 C32 N1 -2.1(8) . .
N3 C33 C34 C35 0.3(10) . .
N4 C43 C44 C36 -178.6(5) . .
N4 C43 C44 N3 0.8(8) . .
