#------------------------------------------------------------------------------
#$Date: 2022-07-01 01:54:34 +0300 (Fri, 01 Jul 2022) $
#$Revision: 276460 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/06/7710647.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_7710647
loop_
_publ_author_name
'Varbanov, Hristo Plamenov'
'Glasnov, Toma N.'
'Belaj, Ferdinand'
'Herbert, Simon'
'Brumby, Thomas'
'Moesch-Zanetti, Nadia Carmen'
_publ_section_title
;
 New strategies towards advanced CT contrast agents. Development of
 neutral and monoanionic sulfur-bridged W(V) dimeric complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01470J
_journal_year                    2022
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         '3(C6 H14 N4 O6 S2 W2), 4(K2 S4 W), 14(H2 O)'
_chemical_formula_sum            'C18 H70 K8 N12 O32 S22 W10'
_chemical_formula_weight         3823.48
_chemical_name_common
'tris[bis(mu2-sulfido)-bis(2,3-diaminopropionato-N,N',O)-dioxo-di-tungsten(V)]-tetrakis[potassium tetrasulfido-tungsten(VI)]-tetradecaaqua adduct'
_chemical_name_systematic
'tris[bis(mu2-sulfido)-bis(2,3-diaminopropionato-N,N',O)-dioxo-di-tungsten(V)]-tetrakis[potassium tetrasulfido-tungsten(VI)]-tetradecaaqua adduct'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2022-03-19 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.0697(7)
_cell_length_b                   18.0697(7)
_cell_length_c                   45.2783(18)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.55
_cell_measurement_theta_min      2.63
_cell_volume                     12803.3(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            48598
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        35.0
_diffrn_reflns_theta_max         35.0
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    14.416
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.975
_exptl_crystal_description       plate
_exptl_crystal_F_000             10572
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.052
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12558
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0128P)²+2.6029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11195
_reflns_number_total             12558
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01470j2.cif
_cod_data_source_block           HV25B
_cod_original_cell_volume        12803.3(13)
_cod_database_code               7710647
_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.
;
_shelx_estimated_absorpt_t_min   0.098
_shelx_estimated_absorpt_t_max   0.300
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.53888(2) 0.57680(2) 0.35505(2) 0.00878(2) Uani 1 1 d D . . . .
W2 W 0.63642(2) 0.61013(2) 0.40661(2) 0.00902(2) Uani 1 1 d D . . . .
O1 O 0.60593(10) 0.57069(10) 0.32933(3) 0.0160(3) Uani 1 1 d . . . . .
O2 O 0.72737(10) 0.61410(10) 0.39301(3) 0.0159(3) Uani 1 1 d . . . . .
S1 S 0.52613(3) 0.47856(3) 0.39083(2) 0.01282(8) Uani 1 1 d . . . . .
S2 S 0.62234(3) 0.70899(3) 0.37766(2) 0.01113(8) Uani 1 1 d . . . . .
N13 N 0.4986(4) 0.6414(6) 0.3236(3) 0.0098(10) Uani 0.637(3) 1 d D . P A 1
H131 H 0.4894 0.6797 0.3337 0.021(3) Uiso 0.637(3) 1 calc R U P A 1
H132 H 0.5421 0.6714 0.3107 0.021(3) Uiso 0.637(3) 1 calc R U P A 1
C14 C 0.42003(19) 0.58403(18) 0.30643(7) 0.0116(4) Uani 0.637(3) 1 d D . P A 1
H141 H 0.4352 0.5672 0.2876 0.020(4) Uiso 0.637(3) 1 calc R U P A 1
H142 H 0.3872 0.6132 0.3020 0.020(4) Uiso 0.637(3) 1 calc R U P A 1
C17 C 0.36755(19) 0.50565(18) 0.32579(6) 0.0122(5) Uani 0.637(3) 1 d D . P A 1
H17 H 0.3121 0.4640 0.3163 0.020(4) Uiso 0.637(3) 1 calc R U P A 1
N17 N 0.4217(4) 0.4672(3) 0.33208(15) 0.0090(10) Uani 0.637(3) 1 d D . P A 1
H171 H 0.4368 0.4512 0.3151 0.021(3) Uiso 0.637(3) 1 calc R U P A 1
H172 H 0.3943 0.4210 0.3442 0.021(3) Uiso 0.637(3) 1 calc R U P A 1
C18 C 0.3546(2) 0.5364(2) 0.35550(6) 0.0111(5) Uani 0.637(3) 1 d D . P A 1
O18 O 0.2901(3) 0.5392(4) 0.36176(18) 0.0128(8) Uani 0.637(3) 1 d D . P A 1
O19 O 0.41913(19) 0.5596(4) 0.37293(8) 0.0090(8) Uani 0.637(3) 1 d D . P A 1
N83 N 0.4349(8) 0.4751(6) 0.3295(3) 0.0090(10) Uani 0.363(3) 1 d D . P A 2
H831 H 0.4563 0.4479 0.3185 0.021(3) Uiso 0.363(3) 1 calc R U P A 2
H832 H 0.3957 0.4362 0.3422 0.021(3) Uiso 0.363(3) 1 calc R U P A 2
C84 C 0.3909(3) 0.5062(3) 0.30936(11) 0.0122(5) Uani 0.363(3) 1 d D . P A 2
H841 H 0.3291 0.4639 0.3081 0.020(4) Uiso 0.363(3) 1 calc R U P A 2
H842 H 0.4157 0.5161 0.2893 0.020(4) Uiso 0.363(3) 1 calc R U P A 2
C87 C 0.4048(3) 0.5898(3) 0.32282(10) 0.0116(4) Uani 0.363(3) 1 d D . P A 2
H87 H 0.3755 0.6140 0.3108 0.020(4) Uiso 0.363(3) 1 calc R U P A 2
N87 N 0.4980(7) 0.6506(11) 0.3243(6) 0.0098(10) Uani 0.363(3) 1 d D . P A 2
H871 H 0.5097 0.7017 0.3322 0.021(3) Uiso 0.363(3) 1 calc R U P A 2
H872 H 0.5231 0.6594 0.3062 0.021(3) Uiso 0.363(3) 1 calc R U P A 2
C88 C 0.3697(4) 0.5706(4) 0.35402(10) 0.0111(5) Uani 0.363(3) 1 d D . P A 2
O88 O 0.2965(6) 0.5559(9) 0.3584(4) 0.0128(8) Uani 0.363(3) 1 d D . P A 2
O89 O 0.4255(4) 0.5749(8) 0.37281(14) 0.0090(8) Uani 0.363(3) 1 d D . P A 2
N23 N 0.6358(14) 0.5415(9) 0.44653(14) 0.0128(6) Uani 0.642(3) 1 d D . P B 3
H231 H 0.5805 0.5047 0.4516 0.021(3) Uiso 0.642(3) 1 calc R U P B 3
H232 H 0.6607 0.5098 0.4423 0.021(3) Uiso 0.642(3) 1 calc R U P B 3
C24 C 0.6807(2) 0.5973(2) 0.47274(7) 0.0144(5) Uani 0.642(3) 1 d D . P B 3
H241 H 0.7409 0.6106 0.4735 0.020(4) Uiso 0.642(3) 1 calc R U P B 3
H242 H 0.6520 0.5684 0.4913 0.020(4) Uiso 0.642(3) 1 calc R U P B 3
C27 C 0.6762(2) 0.6781(2) 0.46837(7) 0.0145(5) Uani 0.642(3) 1 d D . P B 3
H27 H 0.7029 0.7191 0.4851 0.020(4) Uiso 0.642(3) 1 calc R U P B 3
N27 N 0.7177(13) 0.7164(5) 0.4395(2) 0.0113(13) Uani 0.642(3) 1 d D . P B 3
H271 H 0.7731 0.7288 0.4391 0.021(3) Uiso 0.642(3) 1 calc R U P B 3
H272 H 0.7157 0.7648 0.4356 0.021(3) Uiso 0.642(3) 1 calc R U P B 3
C28 C 0.58097(19) 0.6486(2) 0.46485(7) 0.0125(5) Uani 0.642(3) 1 d D . P B 3
O28 O 0.5366(2) 0.6437(2) 0.48589(8) 0.0177(7) Uani 0.642(3) 1 d D . P B 3
O29 O 0.5509(14) 0.622(2) 0.43817(7) 0.0135(3) Uani 0.642(3) 1 d D . P B 3
N93 N 0.718(2) 0.7090(9) 0.4381(4) 0.0113(13) Uani 0.358(3) 1 d D . P B 4
H931 H 0.7729 0.7341 0.4314 0.021(3) Uiso 0.358(3) 1 calc R U P B 4
H932 H 0.7026 0.7497 0.4384 0.021(3) Uiso 0.358(3) 1 calc R U P B 4
C94 C 0.7167(3) 0.6798(3) 0.46936(12) 0.0145(5) Uani 0.358(3) 1 d D . P B 4
H941 H 0.7174 0.7218 0.4836 0.020(4) Uiso 0.358(3) 1 calc R U P B 4
H942 H 0.7669 0.6730 0.4732 0.020(4) Uiso 0.358(3) 1 calc R U P B 4
C97 C 0.6347(3) 0.5948(3) 0.47234(12) 0.0144(5) Uani 0.358(3) 1 d D . P B 4
H97 H 0.6302 0.5692 0.4923 0.020(4) Uiso 0.358(3) 1 calc R U P B 4
N97 N 0.632(3) 0.5365(16) 0.4484(2) 0.0128(6) Uani 0.358(3) 1 d D . P B 4
H971 H 0.5835 0.4848 0.4493 0.021(3) Uiso 0.358(3) 1 calc R U P B 4
H972 H 0.6782 0.5287 0.4495 0.021(3) Uiso 0.358(3) 1 calc R U P B 4
C98 C 0.5590(3) 0.6088(4) 0.46650(13) 0.0125(5) Uani 0.358(3) 1 d D . P B 4
O98 O 0.5178(5) 0.6153(4) 0.48659(16) 0.0177(7) Uani 0.358(3) 1 d D . P B 4
O99 O 0.552(2) 0.622(4) 0.43842(11) 0.0135(3) Uani 0.358(3) 1 d D . P B 4
W3 W 0.3333 0.6667 0.56336(2) 0.01525(3) Uani 1 3 d S T P . .
S31 S 0.3333 0.6667 0.61082(3) 0.0562(4) Uani 1 3 d S T P . .
S32 S 0.45920(3) 0.69537(4) 0.54669(2) 0.02160(11) Uani 1 1 d . . . . .
W4 W 0.58857(2) 0.71143(2) 0.23979(2) 0.01698(2) Uani 0.9574(3) 1 d . . P C 5
S41 S 0.49420(5) 0.74416(5) 0.25526(2) 0.02532(15) Uani 0.9574(3) 1 d . . P C 5
S42 S 0.66913(4) 0.80403(4) 0.20632(2) 0.01921(12) Uani 0.9574(3) 1 d . . P C 5
S43 S 0.52865(5) 0.58182(5) 0.22174(2) 0.03926(18) Uani 0.9574(3) 1 d . . P C 5
S44 S 0.66974(4) 0.71870(5) 0.27772(2) 0.02766(13) Uani 0.9574(3) 1 d . . P C 5
W5 W 0.54769(14) 0.68761(13) 0.22801(5) 0.01698(2) Uani 0.0426(3) 1 d D . P C 6
S51 S 0.4793(8) 0.7272(9) 0.2581(3) 0.02532(15) Uani 0.0426(3) 1 d D . P C 6
S52 S 0.6629(5) 0.7989(6) 0.2112(3) 0.01921(12) Uani 0.0426(3) 1 d D . P C 6
S53 S 0.4639(7) 0.6136(7) 0.1916(2) 0.03926(18) Uani 0.0426(3) 1 d D . P C 6
S54 S 0.5843(7) 0.6048(6) 0.2528(2) 0.02766(13) Uani 0.0426(3) 1 d D . P C 6
K1 K 0.3333 0.6667 0.45101(3) 0.0453(3) Uani 1 3 d S T P . .
O11 O 0.35760(8) 0.57497(10) 0.48196(3) 0.0222(3) Uani 1 1 d D . . . .
H111 H 0.40587(14) 0.5923(8) 0.48960(12) 0.046(7) Uiso 1 1 d D U . . .
H112 H 0.32717(19) 0.5733(4) 0.49626(6) 0.046(7) Uiso 1 1 d D U . . .
O12 O 0.45028(8) 0.70048(9) 0.42056(3) 0.0148(3) Uani 1 1 d D . . . .
H121 H 0.4459(6) 0.7107(5) 0.40275(5) 0.058(8) Uiso 1 1 d D U . . .
H122 H 0.49308(12) 0.6947(2) 0.4233(3) 0.058(8) Uiso 1 1 d D U . . .
K2 K 0.37236(3) 0.50284(3) 0.43090(2) 0.01521(8) Uani 1 1 d . . . . .
O21 O 0.44260(10) 0.41818(10) 0.45991(3) 0.0239(3) Uani 1 1 d D . . . .
H211 H 0.4575(3) 0.4119(4) 0.47686(5) 0.034(6) Uiso 1 1 d D U . . .
H212 H 0.4090(6) 0.37079(18) 0.45215(12) 0.034(6) Uiso 1 1 d D U . . .
K3 K 0.83858(6) 0.56040(7) 0.39178(2) 0.0291(3) Uani 0.788(3) 1 d . . P D 7
K4 K 0.8033(2) 0.5171(3) 0.37912(10) 0.0369(11) Uani 0.212(3) 1 d . . P D 8
O41 O 0.7247(6) 0.49203(16) 0.34346(5) 0.0415(14) Uani 0.1667 1 d D . P E 9
H411 H 0.7320(9) 0.4925(17) 0.36180(5) 0.062 Uiso 0.1667 1 d D U P F 9
H412 H 0.752(3) 0.54136(17) 0.33619(13) 0.062 Uiso 0.1667 1 d D U P G 9
O42 O 0.6732(2) 0.46121(16) 0.33485(5) 0.0415(14) Uani 0.1667 1 d D . P H 10
H421 H 0.6480(2) 0.4596(5) 0.35063(6) 0.062 Uiso 0.1667 1 d D U P I 10
H422 H 0.6749(4) 0.49681(17) 0.32254(8) 0.062 Uiso 0.1667 1 d D U P J 10
O43 O 0.6359(2) 0.43543(16) 0.32935(5) 0.0415(14) Uani 0.1667 1 d D . P K 11
H431 H 0.6658(4) 0.4638(4) 0.31490(7) 0.062 Uiso 0.1667 1 d D U P L 11
H432 H 0.6241(2) 0.46432(18) 0.34096(8) 0.062 Uiso 0.1667 1 d D U P M 11
O44 O 0.60576(19) 0.41949(12) 0.32828(6) 0.0415(14) Uani 0.1667 1 d D . P N 12
H441 H 0.6216(3) 0.4047(3) 0.31307(6) 0.062 Uiso 0.1667 1 d D U P O 12
H442 H 0.6089(3) 0.46732(13) 0.3269(6) 0.062 Uiso 0.1667 1 d D U P P 12
O45 O 0.57566(13) 0.40096(13) 0.32906(6) 0.0415(14) Uani 0.1667 1 d D . P Q 13
H451 H 0.60117(16) 0.37695(16) 0.32191(13) 0.062 Uiso 0.1667 1 d D U P R 13
H452 H 0.5613(2) 0.42562(19) 0.31650(8) 0.062 Uiso 0.1667 1 d D U P S 13
O46 O 0.54498(12) 0.3648(2) 0.32101(7) 0.0415(14) Uani 0.1667 1 d D . P T 14
H461 H 0.49483(13) 0.3547(4) 0.3182(3) 0.062 Uiso 0.1667 1 d D U P U 14
H462 H 0.5615(2) 0.3465(2) 0.30692(7) 0.062 Uiso 0.1667 1 d D U P V 14
K5 K 0.3333 0.6667 0.20714(6) 0.0570(8) Uani 0.5 3 d S T P W 15
O51 O 0.18806(11) 0.5933(2) 0.17243(8) 0.028(3) Uani 0.1667 1 d D . P X 16
H511 H 0.15592(17) 0.6034(2) 0.16185(9) 0.042 Uiso 0.1667 1 d D U P Y 16
H512 H 0.23882(15) 0.618(4) 0.16641(15) 0.042 Uiso 0.1667 1 d D U P Z 16
K6 K 0.2676(3) 0.6151(3) 0.19844(10) 0.0406(9) Uani 0.1667 1 d . . P A 17
O61 O 0.42776(12) 0.76630(18) 0.19062(6) 0.070(5) Uani 0.1667 1 d D . P B 18
H611 H 0.47262(13) 0.7635(2) 0.1891(6) 0.105 Uiso 0.1667 1 d D U P C 18
H612 H 0.4153(3) 0.7819(3) 0.17482(6) 0.105 Uiso 0.1667 1 d D U P D 18
O62 O 0.35222(16) 0.55296(19) 0.16806(6) 0.080(6) Uani 0.1667 1 d D . P E 19
H621 H 0.3541(4) 0.52236(19) 0.15445(7) 0.120 Uiso 0.1667 1 d D U P F 19
H622 H 0.39837(18) 0.578(2) 0.17749(10) 0.120 Uiso 0.1667 1 d D U P G 19
O63 O 0.2241(2) 0.70927(13) 0.16955(9) 0.092(8) Uani 0.1667 1 d D . P H 20
H631 H 0.2411(6) 0.76184(13) 0.1700(15) 0.138 Uiso 0.1667 1 d D U P I 20
H632 H 0.1818(2) 0.6815(9) 0.15845(9) 0.138 Uiso 0.1667 1 d D U P J 20
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'
K K 0.2009 0.2494 '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'
W W -0.8490 6.8722 '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
O1 W1 O19 156.97(11) . . yes
O1 W1 N13 91.5(4) . . ?
O19 W1 N13 75.3(3) . . ?
O1 W1 O89 158.64(18) . . ?
O1 W1 N83 85.7(5) . . ?
O89 W1 N83 77.1(5) . . ?
O1 W1 N87 93.9(7) . . ?
O89 W1 N87 70.2(6) . . ?
N83 W1 N87 77.0(4) . . ?
O1 W1 N17 90.8(2) . . ?
O19 W1 N17 67.9(2) . . ?
N13 W1 N17 75.89(18) . . ?
O1 W1 S1 103.06(5) . . ?
O19 W1 S1 85.43(14) . . ?
N13 W1 S1 158.26(18) . . yes
O89 W1 S1 89.8(3) . . ?
N83 W1 S1 90.7(3) . . ?
N87 W1 S1 158.3(3) . . ?
N17 W1 S1 87.75(17) . . ?
O1 W1 S2 104.32(5) . . ?
O19 W1 S2 94.05(14) . . ?
N13 W1 S2 87.5(3) . . ?
O89 W1 S2 88.6(3) . . ?
N83 W1 S2 159.5(4) . . ?
N87 W1 S2 84.4(6) . . ?
N17 W1 S2 157.9(2) . . yes
S1 W1 S2 104.040(18) . . yes
O1 W1 W2 100.95(5) . . ?
O19 W1 W2 101.18(9) . . ?
N13 W1 W2 140.3(4) . . ?
O89 W1 W2 100.41(17) . . ?
N83 W1 W2 143.5(3) . . ?
N87 W1 W2 137.1(7) . . ?
N17 W1 W2 140.41(17) . . ?
S1 W1 W2 52.858(13) . . ?
S2 W1 W2 53.019(12) . . ?
O2 W2 N93 87.6(13) . . ?
O2 W2 N23 93.1(5) . . ?
O2 W2 O99 158.5(6) . . ?
N93 W2 O99 73.2(18) . . ?
O2 W2 O29 159.0(4) . . yes
N23 W2 O29 73.4(7) . . ?
O2 W2 N27 89.9(7) . . ?
N23 W2 N27 76.0(3) . . ?
O29 W2 N27 71.5(10) . . ?
O2 W2 N97 94.2(9) . . ?
N93 W2 N97 75.4(5) . . ?
O99 W2 N97 72.1(12) . . ?
O2 W2 S1 104.19(6) . . ?
N93 W2 S1 157.1(6) . . ?
N23 W2 S1 85.1(5) . . ?
O99 W2 S1 91.1(16) . . ?
O29 W2 S1 90.9(9) . . ?
N27 W2 S1 157.1(4) . . yes
N97 W2 S1 84.1(9) . . ?
O2 W2 S2 103.57(5) . . ?
N93 W2 S2 91.7(7) . . ?
N23 W2 S2 158.0(3) . . yes
O99 W2 S2 86.8(11) . . ?
O29 W2 S2 86.4(6) . . ?
N27 W2 S2 89.6(3) . . ?
N97 W2 S2 157.6(5) . . ?
S1 W2 S2 104.186(17) . . yes
O2 W2 W1 101.28(5) . . ?
N93 W2 W1 144.6(7) . . ?
N23 W2 W1 137.9(5) . . ?
O99 W2 W1 100.0(4) . . ?
O29 W2 W1 99.5(2) . . ?
N27 W2 W1 142.4(4) . . ?
N97 W2 W1 136.7(9) . . ?
S1 W2 W1 53.020(12) . . ?
S2 W2 W1 53.009(12) . . ?
W2 S1 W1 74.122(14) . . yes
W1 S2 W2 73.972(14) . . yes
C14 N13 W1 115.1(4) . . yes
C14 N13 H131 108.5 . . ?
W1 N13 H131 108.5 . . ?
C14 N13 H132 108.5 . . ?
W1 N13 H132 108.5 . . ?
H131 N13 H132 107.5 . . ?
N13 C14 C17 106.2(3) . . ?
N13 C14 H141 110.5 . . ?
C17 C14 H141 110.5 . . ?
N13 C14 H142 110.5 . . ?
C17 C14 H142 110.5 . . ?
H141 C14 H142 108.7 . . ?
N17 C17 C18 105.0(3) . . ?
N17 C17 C14 107.2(3) . . ?
C18 C17 C14 107.9(2) . . ?
N17 C17 H17 112.1 . . ?
C18 C17 H17 112.1 . . ?
C14 C17 H17 112.1 . . ?
C17 N17 W1 102.9(3) . . yes
C17 N17 H171 111.2 . . ?
W1 N17 H171 111.2 . . ?
C17 N17 H172 111.2 . . ?
W1 N17 H172 111.2 . . ?
H171 N17 H172 109.1 . . ?
O18 C18 O19 124.6(5) . . ?
O18 C18 C17 123.0(5) . . ?
O19 C18 C17 112.4(3) . . ?
C18 O19 W1 119.3(2) . . yes
C84 N83 W1 113.7(6) . . ?
C84 N83 H831 108.8 . . ?
W1 N83 H831 108.8 . . ?
C84 N83 H832 108.8 . . ?
W1 N83 H832 108.8 . . ?
H831 N83 H832 107.7 . . ?
N83 C84 C87 105.9(6) . . ?
N83 C84 H841 110.6 . . ?
C87 C84 H841 110.6 . . ?
N83 C84 H842 110.6 . . ?
C87 C84 H842 110.6 . . ?
H841 C84 H842 108.7 . . ?
N87 C87 C88 108.6(11) . . ?
N87 C87 C84 108.4(11) . . ?
C88 C87 C84 107.6(4) . . ?
N87 C87 H87 110.7 . . ?
C88 C87 H87 110.7 . . ?
C84 C87 H87 110.7 . . ?
C87 N87 W1 99.9(4) . . ?
C87 N87 H871 111.8 . . ?
W1 N87 H871 111.8 . . ?
C87 N87 H872 111.8 . . ?
W1 N87 H872 111.8 . . ?
H871 N87 H872 109.5 . . ?
O88 C88 O89 129.1(8) . . ?
O88 C88 C87 118.9(9) . . ?
O89 C88 C87 112.0(5) . . ?
C88 O89 W1 117.1(4) . . ?
C24 N23 W2 115.1(6) . . yes
C24 N23 H231 108.5 . . ?
W2 N23 H231 108.5 . . ?
C24 N23 H232 108.5 . . ?
W2 N23 H232 108.5 . . ?
H231 N23 H232 107.5 . . ?
N23 C24 C27 105.7(3) . . ?
N23 C24 H241 110.6 . . ?
C27 C24 H241 110.6 . . ?
N23 C24 H242 110.6 . . ?
C27 C24 H242 110.6 . . ?
H241 C24 H242 108.7 . . ?
N27 C27 C24 107.7(8) . . ?
N27 C27 C28 106.6(8) . . ?
C24 C27 C28 105.7(3) . . ?
N27 C27 H27 112.2 . . ?
C24 C27 H27 112.2 . . ?
C28 C27 H27 112.2 . . ?
C27 N27 W2 102.6(5) . . yes
C27 N27 H271 111.3 . . ?
W2 N27 H271 111.3 . . ?
C27 N27 H272 111.3 . . ?
W2 N27 H272 111.3 . . ?
H271 N27 H272 109.2 . . ?
O28 C28 O29 123.7(7) . . ?
O28 C28 C27 121.8(3) . . ?
O29 C28 C27 114.2(5) . . ?
C28 O29 W2 116.8(6) . . yes
C94 N93 W2 116.2(8) . . ?
C94 N93 H931 108.2 . . ?
W2 N93 H931 108.2 . . ?
C94 N93 H932 108.2 . . ?
W2 N93 H932 108.2 . . ?
H931 N93 H932 107.4 . . ?
N93 C94 C97 106.0(9) . . ?
N93 C94 H941 110.5 . . ?
C97 C94 H941 110.5 . . ?
N93 C94 H942 110.5 . . ?
C97 C94 H942 110.5 . . ?
H941 C94 H942 108.7 . . ?
N97 C97 C94 108.6(15) . . ?
N97 C97 C98 106.1(14) . . ?
C94 C97 C98 108.6(5) . . ?
N97 C97 H97 111.1 . . ?
C94 C97 H97 111.1 . . ?
C98 C97 H97 111.1 . . ?
C97 N97 W2 102.0(6) . . ?
C97 N97 H971 111.4 . . ?
W2 N97 H971 111.4 . . ?
C97 N97 H972 111.4 . . ?
W2 N97 H972 111.4 . . ?
H971 N97 H972 109.2 . . ?
O98 C98 O99 125.6(7) . . ?
O98 C98 C97 121.7(6) . . ?
O99 C98 C97 112.2(5) . . ?
C98 O99 W2 118.6(7) . . ?
S31 W3 S32 110.091(17) . 2_665 ?
S31 W3 S32 110.091(17) . 3_565 ?
S32 W3 S32 108.844(18) 2_665 3_565 ?
S31 W3 S32 110.090(17) . . ?
S32 W3 S32 108.845(18) 2_665 . ?
S32 W3 S32 108.844(18) 3_565 . ?
S41 W4 S42 109.07(3) . . ?
S41 W4 S43 112.00(3) . . ?
S42 W4 S43 110.12(3) . . ?
S41 W4 S44 108.58(3) . . ?
S42 W4 S44 108.88(3) . . ?
S43 W4 S44 108.12(3) . . ?
S52 W5 S51 110.5(3) . . ?
S52 W5 S53 110.5(3) . . ?
S51 W5 S53 109.7(3) . . ?
S52 W5 S54 109.2(3) . . ?
S51 W5 S54 108.3(3) . . ?
S53 W5 S54 108.5(3) . . ?
H111 O11 H112 103.6(6) . . ?
H121 O12 H122 111.4(11) . . ?
H211 O21 H212 111.2(6) . . ?
H411 O41 H412 112(2) . . ?
H421 O42 H422 113.8(7) . . ?
H431 O43 H432 113.2(7) . . ?
H441 O44 H442 114.1(19) . . ?
H451 O45 H452 114.1(6) . . ?
H461 O46 H462 110.9(11) . . ?
H511 O51 H512 113(3) . . ?
H611 O61 H612 112.3(17) . . ?
H621 O62 H622 112(2) . . ?
H631 O63 H632 113(3) . . ?
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
W1 O1 1.7236(15) . yes
W1 O19 2.1820(19) . yes
W1 N13 2.184(4) . yes
W1 N17 2.301(4) . yes
W1 O89 2.185(3) . ?
W1 N83 2.190(5) . ?
W1 N87 2.292(5) . ?
W1 S1 2.3280(5) . yes
W1 S2 2.3294(5) . yes
W2 O2 1.7225(14) . yes
W2 O29 2.1942(19) . yes
W2 N23 2.189(4) . yes
W2 N27 2.288(4) . yes
W2 O99 2.192(3) . ?
W2 N93 2.184(5) . ?
W2 N97 2.295(5) . ?
W2 S1 2.3230(5) . yes
W2 S2 2.3297(5) . yes
W1 W2 2.80301(15) . yes
N13 C14 1.492(10) . yes
N13 H131 0.91 . ?
N13 H132 0.91 . ?
C14 C17 1.527(4) . yes
C14 H141 0.99 . ?
C14 H142 0.99 . ?
C17 N17 1.483(8) . yes
C17 C18 1.517(4) . yes
C17 H17 1.00 . ?
N17 H171 0.91 . ?
N17 H172 0.91 . ?
C18 O18 1.227(3) . yes
C18 O19 1.292(3) . yes
N83 C84 1.491(11) . ?
N83 H831 0.91 . ?
N83 H832 0.91 . ?
C84 C87 1.528(4) . ?
C84 H841 0.99 . ?
C84 H842 0.99 . ?
C87 N87 1.483(9) . ?
C87 C88 1.516(4) . ?
C87 H87 1.00 . ?
N87 H871 0.91 . ?
N87 H872 0.91 . ?
C88 O88 1.227(4) . ?
C88 O89 1.292(4) . ?
N23 C24 1.505(14) . yes
N23 H231 0.91 . ?
N23 H232 0.91 . ?
C24 C27 1.516(4) . yes
C24 H241 0.99 . ?
C24 H242 0.99 . ?
C27 N27 1.496(15) . yes
C27 C28 1.535(4) . yes
C27 H27 1.00 . ?
N27 H271 0.91 . ?
N27 H272 0.91 . ?
C28 O28 1.220(3) . yes
C28 O29 1.313(12) . yes
N93 C94 1.505(14) . ?
N93 H931 0.91 . ?
N93 H932 0.91 . ?
C94 C97 1.516(5) . ?
C94 H941 0.99 . ?
C94 H942 0.99 . ?
C97 N97 1.495(15) . ?
C97 C98 1.533(5) . ?
C97 H97 1.00 . ?
N97 H971 0.91 . ?
N97 H972 0.91 . ?
C98 O98 1.218(4) . ?
C98 O99 1.313(12) . ?
W3 S31 2.1489(13) . yes
W3 S32 2.1982(6) . yes
W3 S32 2.1982(6) 2_665 ?
W3 S32 2.1982(6) 3_565 ?
W4 S41 2.1810(6) . yes
W4 S42 2.1863(6) . yes
W4 S43 2.1885(8) . yes
W4 S44 2.2190(7) . yes
W5 S52 2.1847(7) . ?
W5 S51 2.1850(7) . ?
W5 S53 2.1851(7) . ?
W5 S54 2.2190(7) . ?
O11 H111 0.84 . ?
O11 H112 0.84 . ?
O12 H121 0.84 . ?
O12 H122 0.84 . ?
O21 H211 0.84 . ?
O21 H212 0.84 . ?
O41 H411 0.84 . ?
O41 H412 0.84 . ?
O42 H421 0.84 . ?
O42 H422 0.84 . ?
O43 H431 0.84 . ?
O43 H432 0.84 . ?
O44 H441 0.84 . ?
O44 H442 0.84 . ?
O45 H451 0.84 . ?
O45 H452 0.84 . ?
O46 H461 0.84 . ?
O46 H462 0.84 . ?
O51 H511 0.84 . ?
O51 H512 0.84 . ?
O61 H611 0.84 . ?
O61 H612 0.84 . ?
O62 H621 0.84 . ?
O62 H622 0.84 . ?
O63 H631 0.84 . ?
O63 H632 0.84 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N13 H131 O18 0.91 2.05 2.951(17) 170.4 2_665
N17 H171 O2 0.91 2.19 3.089(8) 168.8 18_545
N17 H172 O1 0.91 2.50 3.158(6) 129.3 18_545
N83 H831 O2 0.91 2.22 2.982(15) 140.6 18_545
N87 H871 O88 0.91 2.04 2.75(3) 134.4 2_665
N23 H231 O21 0.91 2.21 3.12(2) 174.5 .
N23 H232 S32 0.91 2.50 3.332(15) 151.9 12_656
N97 H971 O21 0.91 2.26 3.04(4) 144.3 .
O11 H111 O28 0.84 2.068(4) 2.831(4) 150.9(5) .
O11 H111 O98 0.84 1.855(9) 2.616(8) 150.0(8) .
O12 H121 O18 0.84 1.961(8) 2.789(8) 168.4(9) 2_665
O12 H121 O88 0.84 2.084(15) 2.923(15) 176.1(10) 2_665
O12 H122 O29 0.84 2.151(18) 2.918(14) 151.6(10) .
O12 H122 O99 0.84 2.17(3) 2.93(2) 151.8(15) .
O21 H211 O28 0.84 1.993(5) 2.799(5) 160.6(6) 10_666
O21 H211 O98 0.84 1.843(9) 2.679(9) 173.4(7) 10_666
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
S1 W1 S2 W2 14.67(3) . . . . yes
S2 W1 S1 W2 -14.70(3) . . . . yes
S1 W2 S2 W1 -14.71(4) . . . . yes
S2 W2 S1 W1 14.71(4) . . . . yes
O1 W1 W2 O2 1.18(9) . . . . yes
O19 W1 W2 O29 -8.4(10) . . . . yes
W1 N13 C14 C17 27.7(9) . . . . yes
N13 C14 C17 N17 -58.6(7) . . . . ?
N13 C14 C17 C18 54.1(6) . . . . ?
C14 C17 N17 W1 58.8(4) . . . . yes
C18 C17 N17 W1 -55.8(4) . . . . yes
N17 C17 C18 O18 -149.5(4) . . . . ?
C14 C17 C18 O18 96.4(4) . . . . ?
N17 C17 C18 O19 31.2(5) . . . . ?
C14 C17 C18 O19 -82.9(4) . . . . ?
C17 C18 O19 W1 12.7(5) . . . . yes
O18 C18 O19 W1 -166.6(4) . . . . yes
W1 N83 C84 C87 -25.0(10) . . . . ?
N83 C84 C87 N87 60.1(10) . . . . ?
N83 C84 C87 C88 -57.2(8) . . . . ?
C88 C87 N87 W1 55.0(13) . . . . ?
C84 C87 N87 W1 -61.6(13) . . . . ?
N87 C87 C88 O88 147.6(12) . . . . ?
C84 C87 C88 O88 -95.3(10) . . . . ?
N87 C87 C88 O89 -30.5(11) . . . . ?
C84 C87 C88 O89 86.6(8) . . . . ?
O88 C88 O89 W1 167.8(10) . . . . ?
C87 C88 O89 W1 -14.3(11) . . . . ?
W2 N23 C24 C27 26.4(12) . . . . yes
N23 C24 C27 N27 -58.1(11) . . . . ?
N23 C24 C27 C28 55.5(8) . . . . ?
C24 C27 N27 W2 59.7(10) . . . . yes
C28 C27 N27 W2 -53.3(10) . . . . yes
N27 C27 C28 O28 -153.1(6) . . . . ?
C24 C27 C28 O28 92.5(4) . . . . ?
N27 C27 C28 O29 32.9(18) . . . . ?
C24 C27 C28 O29 -81.5(17) . . . . ?
C27 C28 O29 W2 7.6(23) . . . . yes
O28 C28 O29 W2 -166.3(9) . . . . yes
W2 N93 C94 C97 -20(3) . . . . ?
N93 C94 C97 N97 54(2) . . . . ?
N93 C94 C97 C98 -60.7(19) . . . . ?
C94 C97 N97 W2 -60.3(17) . . . . ?
C98 C97 N97 W2 56.2(17) . . . . ?
N97 C97 C98 O98 143.8(11) . . . . ?
C94 C97 C98 O98 -99.7(7) . . . . ?
N97 C97 C98 O99 -43(3) . . . . ?
C94 C97 C98 O99 73(3) . . . . ?
O98 C98 O99 W2 178.0(16) . . . . ?
C97 C98 O99 W2 6(5) . . . . ?
