# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-W
_database_code_depnum_ccdc_archive 'CCDC 1413124'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_audit_creation_date             2011-08-17
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
(NEt4)2[WO(S2C6H3CONH-t-Bu)2] 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H66 N4 O3 S4 W'
_chemical_formula_sum            'C38 H66 N4 O3 S4 W'
_chemical_formula_weight         939.04

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   8.865(2)
_cell_length_b                   16.289(3)
_cell_length_c                   29.929(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4321.8(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    27666
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      25.36

_exptl_crystal_description       column
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            28811
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         24.99
_reflns_number_total             7323
_reflns_number_gt                6972
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'

_refine_special_details          Twin

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+64.7205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3157 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.002(12)
_refine_ls_number_reflns         7323
_refine_ls_number_parameters     454
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1526
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
W1 W 0.61013(8) 0.59975(3) 0.256307(17) 0.03686(16) Uani 1 1 d D . .
S11 S 0.3461(4) 0.6007(2) 0.26052(10) 0.0400(8) Uani 1 1 d D . .
S12 S 0.5634(4) 0.6671(2) 0.18750(11) 0.0367(9) Uani 1 1 d D . .
S21 S 0.8239(4) 0.6843(2) 0.26463(12) 0.0427(9) Uani 1 1 d D . .
S22 S 0.6064(5) 0.6102(2) 0.33532(9) 0.0375(8) Uani 1 1 d . . .
O1 O 0.3212(15) 0.7210(9) 0.0575(4) 0.069(4) Uani 1 1 d . . .
O2 O 0.792(2) 0.6415(13) 0.4771(5) 0.125(8) Uani 1 1 d . . .
O3 O 0.6691(11) 0.5026(5) 0.2430(4) 0.050(3) Uani 1 1 d . . .
N1 N 0.5429(15) 0.6796(7) 0.0865(4) 0.039(3) Uani 1 1 d . . .
H1 H 0.5856 0.6533 0.1088 0.047 Uiso 1 1 calc R . .
N2 N 0.6019(18) 0.6053(10) 0.4359(3) 0.056(3) Uani 1 1 d . . .
H2 H 0.5688 0.6002 0.4083 0.067 Uiso 1 1 calc R . .
N3 N 0.9997(13) 0.4012(8) 0.3263(4) 0.038(3) Uani 1 1 d . . .
N4 N 0.5114(17) 0.8974(9) 0.3707(4) 0.052(3) Uani 1 1 d . . .
C11 C 0.2727(16) 0.6206(8) 0.2066(4) 0.037(3) Uani 1 1 d DU . .
C12 C 0.3712(15) 0.6485(7) 0.1733(4) 0.036(3) Uani 1 1 d D . .
C13 C 0.3083(18) 0.6601(8) 0.1291(5) 0.038(3) Uani 1 1 d . . .
C14 C 0.1560(16) 0.6442(9) 0.1211(5) 0.036(4) Uani 1 1 d . . .
H3 H 0.1148 0.6522 0.0921 0.043 Uiso 1 1 calc R . .
C15 C 0.0680(17) 0.6175(9) 0.1547(6) 0.047(4) Uani 1 1 d . . .
H4 H -0.0341 0.6045 0.1481 0.057 Uiso 1 1 calc R . .
C16 C 0.117(2) 0.6079(9) 0.1977(4) 0.045(3) Uani 1 1 d . . .
H5 H 0.0487 0.5932 0.2209 0.054 Uiso 1 1 calc R . .
C17 C 0.395(2) 0.6905(9) 0.0884(5) 0.048(4) Uani 1 1 d . . .
C18 C 0.640(2) 0.7074(9) 0.0507(4) 0.043(4) Uani 1 1 d . . .
C21 C 0.884(2) 0.6766(8) 0.3209(4) 0.035(3) Uani 1 1 d . . .
C22 C 0.7838(19) 0.6490(8) 0.3538(5) 0.037(4) Uani 1 1 d . . .
C23 C 0.8345(18) 0.6515(8) 0.3987(5) 0.036(4) Uani 1 1 d . . .
C24 C 0.982(2) 0.6777(10) 0.4077(6) 0.051(5) Uani 1 1 d . . .
H6 H 1.0141 0.6799 0.4380 0.062 Uiso 1 1 calc R . .
C25 C 1.082(3) 0.7000(11) 0.3755(6) 0.070(6) Uani 1 1 d . . .
H7 H 1.1829 0.7142 0.3824 0.084 Uiso 1 1 calc R . .
C26 C 1.027(2) 0.7011(10) 0.3317(5) 0.048(4) Uani 1 1 d . . .
H8 H 1.0914 0.7196 0.3085 0.057 Uiso 1 1 calc R . .
C27 C 0.742(2) 0.6332(11) 0.4398(5) 0.054(5) Uani 1 1 d . . .
C28 C 0.493(2) 0.5814(12) 0.4713(5) 0.063(5) Uani 1 1 d . . .
C31 C 0.9878(19) 0.4641(10) 0.3622(5) 0.048(4) Uani 1 1 d . . .
H9 H 0.8925 0.4947 0.3579 0.058 Uiso 1 1 calc R . .
H10 H 1.0718 0.5036 0.3585 0.058 Uiso 1 1 calc R . .
C32 C 0.991(3) 0.4317(14) 0.4093(6) 0.088(7) Uani 1 1 d . . .
H11 H 1.0870 0.4030 0.4144 0.105 Uiso 1 1 calc R . .
H12 H 0.9074 0.3936 0.4137 0.105 Uiso 1 1 calc R . .
H13 H 0.9824 0.4776 0.4303 0.105 Uiso 1 1 calc R . .
C33 C 0.875(2) 0.3393(10) 0.3306(7) 0.068(5) Uani 1 1 d . . .
H14 H 0.8901 0.3079 0.3585 0.082 Uiso 1 1 calc R . .
H15 H 0.8822 0.3002 0.3054 0.082 Uiso 1 1 calc R . .
C34 C 0.718(2) 0.3755(15) 0.3311(9) 0.101(10) Uani 1 1 d . . .
H16 H 0.7005 0.4063 0.3034 0.121 Uiso 1 1 calc R . .
H17 H 0.7071 0.4124 0.3568 0.121 Uiso 1 1 calc R . .
H18 H 0.6432 0.3311 0.3334 0.121 Uiso 1 1 calc R . .
C35 C 0.9916(19) 0.4475(9) 0.2821(5) 0.044(4) Uani 1 1 d . . .
H19 H 0.8994 0.4818 0.2821 0.052 Uiso 1 1 calc R . .
H20 H 1.0794 0.4849 0.2801 0.052 Uiso 1 1 calc R . .
C36 C 0.990(3) 0.3945(13) 0.2418(6) 0.093(7) Uani 1 1 d . . .
H21 H 0.9011 0.3586 0.2428 0.111 Uiso 1 1 calc R . .
H22 H 1.0815 0.3610 0.2411 0.111 Uiso 1 1 calc R . .
H23 H 0.9854 0.4289 0.2150 0.111 Uiso 1 1 calc R . .
C37 C 1.1483(15) 0.3542(9) 0.3302(5) 0.040(4) Uani 1 1 d . . .
H24 H 1.1471 0.3242 0.3590 0.048 Uiso 1 1 calc R . .
H25 H 1.1504 0.3125 0.3062 0.048 Uiso 1 1 calc R . .
C38 C 1.290(2) 0.4006(16) 0.3280(7) 0.079(6) Uani 1 1 d . . .
H26 H 1.2930 0.4410 0.3522 0.094 Uiso 1 1 calc R . .
H27 H 1.2965 0.4290 0.2992 0.094 Uiso 1 1 calc R . .
H28 H 1.3755 0.3628 0.3310 0.094 Uiso 1 1 calc R . .
C41 C 0.661(2) 0.9355(11) 0.3587(8) 0.074(6) Uani 1 1 d . . .
H29 H 0.6709 0.9876 0.3756 0.089 Uiso 1 1 calc R . .
H30 H 0.6585 0.9498 0.3266 0.089 Uiso 1 1 calc R . .
C42 C 0.806(3) 0.8845(15) 0.3672(9) 0.102(9) Uani 1 1 d . . .
H31 H 0.7990 0.8324 0.3509 0.122 Uiso 1 1 calc R . .
H32 H 0.8157 0.8735 0.3992 0.122 Uiso 1 1 calc R . .
H33 H 0.8939 0.9153 0.3567 0.122 Uiso 1 1 calc R . .
C43 C 0.485(3) 0.8193(11) 0.3430(9) 0.103(10) Uani 1 1 d . . .
H34 H 0.5643 0.7787 0.3504 0.123 Uiso 1 1 calc R . .
H35 H 0.3865 0.7952 0.3513 0.123 Uiso 1 1 calc R . .
C44 C 0.487(4) 0.8354(15) 0.2924(8) 0.151(16) Uani 1 1 d . . .
H36 H 0.5872 0.8548 0.2835 0.181 Uiso 1 1 calc R . .
H37 H 0.4115 0.8772 0.2850 0.181 Uiso 1 1 calc R . .
H38 H 0.4634 0.7844 0.2765 0.181 Uiso 1 1 calc R . .
C45 C 0.392(3) 0.9577(10) 0.3629(6) 0.073(6) Uani 1 1 d . . .
H39 H 0.3961 0.9753 0.3312 0.088 Uiso 1 1 calc R . .
H40 H 0.4115 1.0066 0.3816 0.088 Uiso 1 1 calc R . .
C46 C 0.234(2) 0.9254(17) 0.3730(10) 0.110(11) Uani 1 1 d . . .
H41 H 0.2116 0.8787 0.3535 0.132 Uiso 1 1 calc R . .
H42 H 0.1598 0.9690 0.3678 0.132 Uiso 1 1 calc R . .
H43 H 0.2288 0.9078 0.4043 0.132 Uiso 1 1 calc R . .
C47 C 0.515(3) 0.8687(13) 0.4183(7) 0.087(7) Uani 1 1 d . . .
H44 H 0.5962 0.8273 0.4216 0.105 Uiso 1 1 calc R . .
H45 H 0.4181 0.8417 0.4255 0.105 Uiso 1 1 calc R . .
C48 C 0.542(3) 0.9386(19) 0.4517(7) 0.129(13) Uani 1 1 d . . .
H46 H 0.4647 0.9808 0.4478 0.154 Uiso 1 1 calc R . .
H47 H 0.6421 0.9627 0.4464 0.154 Uiso 1 1 calc R . .
H48 H 0.5379 0.9169 0.4822 0.154 Uiso 1 1 calc R . .
C101 C 0.803(2) 0.6852(11) 0.0635(6) 0.057(5) Uani 1 1 d . . .
H49 H 0.8118 0.6255 0.0670 0.069 Uiso 1 1 calc R . .
H50 H 0.8296 0.7121 0.0917 0.069 Uiso 1 1 calc R . .
H51 H 0.8719 0.7037 0.0399 0.069 Uiso 1 1 calc R . .
C102 C 0.630(2) 0.7997(9) 0.0440(5) 0.050(4) Uani 1 1 d . . .
H52 H 0.6607 0.8277 0.0715 0.060 Uiso 1 1 calc R . .
H53 H 0.5262 0.8148 0.0366 0.060 Uiso 1 1 calc R . .
H54 H 0.6973 0.8161 0.0195 0.060 Uiso 1 1 calc R . .
C103 C 0.597(2) 0.6631(9) 0.0058(4) 0.049(4) Uani 1 1 d . . .
H55 H 0.4923 0.6757 -0.0018 0.059 Uiso 1 1 calc R . .
H56 H 0.6090 0.6037 0.0095 0.059 Uiso 1 1 calc R . .
H57 H 0.6639 0.6824 -0.0181 0.059 Uiso 1 1 calc R . .
C201 C 0.363(3) 0.549(2) 0.4484(7) 0.131(12) Uani 1 1 d . . .
H58 H 0.3922 0.5002 0.4313 0.157 Uiso 1 1 calc R . .
H59 H 0.3225 0.5906 0.4280 0.157 Uiso 1 1 calc R . .
H60 H 0.2856 0.5339 0.4703 0.157 Uiso 1 1 calc R . .
C202 C 0.560(3) 0.5138(14) 0.4996(8) 0.094(8) Uani 1 1 d . . .
H61 H 0.6546 0.5327 0.5128 0.113 Uiso 1 1 calc R . .
H62 H 0.5788 0.4655 0.4809 0.113 Uiso 1 1 calc R . .
H63 H 0.4887 0.4993 0.5234 0.113 Uiso 1 1 calc R . .
C203 C 0.457(4) 0.6554(15) 0.4982(11) 0.151(16) Uani 1 1 d . . .
H64 H 0.4109 0.6971 0.4789 0.181 Uiso 1 1 calc R . .
H65 H 0.5495 0.6773 0.5114 0.181 Uiso 1 1 calc R . .
H66 H 0.3859 0.6406 0.5220 0.181 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O3 1.714(8) . ?
W1 S11 2.344(3) . ?
W1 S21 2.356(4) . ?
W1 S12 2.370(3) . ?
W1 S22 2.371(3) . ?
S11 C11 1.770(12) . ?
S12 C12 1.783(13) . ?
S21 C21 1.770(13) . ?
S22 C22 1.783(17) . ?
O1 C17 1.235(18) . ?
O2 C27 1.21(2) . ?
N1 C17 1.33(2) . ?
N1 C18 1.447(19) . ?
N1 H1 0.8800 . ?
N2 C27 1.33(2) . ?
N2 C28 1.48(2) . ?
N2 H2 0.8800 . ?
N3 C31 1.487(19) . ?
N3 C33 1.50(2) . ?
N3 C35 1.526(17) . ?
N3 C37 1.527(17) . ?
N4 C45 1.46(2) . ?
N4 C47 1.50(2) . ?
N4 C41 1.51(2) . ?
N4 C43 1.54(2) . ?
C11 C12 1.40(2) . ?
C11 C16 1.42(2) . ?
C12 C13 1.448(19) . ?
C13 C14 1.40(2) . ?
C13 C17 1.52(2) . ?
C14 C15 1.34(2) . ?
C14 H3 0.9500 . ?
C15 C16 1.37(2) . ?
C15 H4 0.9500 . ?
C16 H5 0.9500 . ?
C18 C102 1.52(2) . ?
C18 C101 1.54(3) . ?
C18 C103 1.571(19) . ?
C21 C26 1.37(2) . ?
C21 C22 1.40(2) . ?
C22 C23 1.42(2) . ?
C23 C24 1.40(2) . ?
C23 C27 1.51(2) . ?
C24 C25 1.35(3) . ?
C24 H6 0.9500 . ?
C25 C26 1.40(2) . ?
C25 H7 0.9500 . ?
C26 H8 0.9500 . ?
C28 C201 1.44(3) . ?
C28 C203 1.49(3) . ?
C28 C202 1.51(3) . ?
C31 C32 1.50(2) . ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9800 . ?
C32 H12 0.9800 . ?
C32 H13 0.9800 . ?
C33 C34 1.51(3) . ?
C33 H14 0.9900 . ?
C33 H15 0.9900 . ?
C34 H16 0.9800 . ?
C34 H17 0.9800 . ?
C34 H18 0.9800 . ?
C35 C36 1.48(2) . ?
C35 H19 0.9900 . ?
C35 H20 0.9900 . ?
C36 H21 0.9800 . ?
C36 H22 0.9800 . ?
C36 H23 0.9800 . ?
C37 C38 1.47(2) . ?
C37 H24 0.9900 . ?
C37 H25 0.9900 . ?
C38 H26 0.9800 . ?
C38 H27 0.9800 . ?
C38 H28 0.9800 . ?
C41 C42 1.55(3) . ?
C41 H29 0.9900 . ?
C41 H30 0.9900 . ?
C42 H31 0.9800 . ?
C42 H32 0.9800 . ?
C42 H33 0.9800 . ?
C43 C44 1.54(3) . ?
C43 H34 0.9900 . ?
C43 H35 0.9900 . ?
C44 H36 0.9800 . ?
C44 H37 0.9800 . ?
C44 H38 0.9800 . ?
C45 C46 1.53(3) . ?
C45 H39 0.9900 . ?
C45 H40 0.9900 . ?
C46 H41 0.9800 . ?
C46 H42 0.9800 . ?
C46 H43 0.9800 . ?
C47 C48 1.53(3) . ?
C47 H44 0.9900 . ?
C47 H45 0.9900 . ?
C48 H46 0.9800 . ?
C48 H47 0.9800 . ?
C48 H48 0.9800 . ?
C101 H49 0.9800 . ?
C101 H50 0.9800 . ?
C101 H51 0.9800 . ?
C102 H52 0.9800 . ?
C102 H53 0.9800 . ?
C102 H54 0.9800 . ?
C103 H55 0.9800 . ?
C103 H56 0.9800 . ?
C103 H57 0.9800 . ?
C201 H58 0.9800 . ?
C201 H59 0.9800 . ?
C201 H60 0.9800 . ?
C202 H61 0.9800 . ?
C202 H62 0.9800 . ?
C202 H63 0.9800 . ?
C203 H64 0.9800 . ?
C203 H65 0.9800 . ?
C203 H66 0.9800 . ?

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
O3 W1 S11 108.8(4) . . ?
O3 W1 S21 108.6(4) . . ?
S11 W1 S21 142.55(14) . . ?
O3 W1 S12 106.1(4) . . ?
S11 W1 S12 82.50(12) . . ?
S21 W1 S12 87.81(13) . . ?
O3 W1 S22 107.6(4) . . ?
S11 W1 S22 86.09(13) . . ?
S21 W1 S22 82.18(13) . . ?
S12 W1 S22 146.22(13) . . ?
C11 S11 W1 108.6(5) . . ?
C12 S12 W1 107.2(4) . . ?
C21 S21 W1 107.5(6) . . ?
C22 S22 W1 108.8(5) . . ?
C17 N1 C18 125.3(12) . . ?
C17 N1 H1 117.3 . . ?
C18 N1 H1 117.3 . . ?
C27 N2 C28 129.5(13) . . ?
C27 N2 H2 115.3 . . ?
C28 N2 H2 115.3 . . ?
C31 N3 C33 110.4(13) . . ?
C31 N3 C35 106.4(11) . . ?
C33 N3 C35 111.8(12) . . ?
C31 N3 C37 110.5(11) . . ?
C33 N3 C37 107.1(12) . . ?
C35 N3 C37 110.8(11) . . ?
C45 N4 C47 112.3(15) . . ?
C45 N4 C41 108.8(15) . . ?
C47 N4 C41 109.5(17) . . ?
C45 N4 C43 111.1(15) . . ?
C47 N4 C43 104.9(16) . . ?
C41 N4 C43 110.2(16) . . ?
C12 C11 C16 121.4(9) . . ?
C12 C11 S11 118.6(9) . . ?
C16 C11 S11 120.0(11) . . ?
C11 C12 C13 116.9(10) . . ?
C11 C12 S12 118.8(8) . . ?
C13 C12 S12 124.3(11) . . ?
C14 C13 C12 120.3(13) . . ?
C14 C13 C17 114.2(14) . . ?
C12 C13 C17 125.5(14) . . ?
C15 C14 C13 119.6(14) . . ?
C15 C14 H3 120.2 . . ?
C13 C14 H3 120.2 . . ?
C14 C15 C16 123.9(15) . . ?
C14 C15 H4 118.0 . . ?
C16 C15 H4 118.0 . . ?
C15 C16 C11 117.7(14) . . ?
C15 C16 H5 121.1 . . ?
C11 C16 H5 121.1 . . ?
O1 C17 N1 123.0(16) . . ?
O1 C17 C13 117.7(18) . . ?
N1 C17 C13 119.2(13) . . ?
N1 C18 C102 112.0(13) . . ?
N1 C18 C101 107.6(12) . . ?
C102 C18 C101 108.7(14) . . ?
N1 C18 C103 110.2(13) . . ?
C102 C18 C103 109.1(12) . . ?
C101 C18 C103 109.3(14) . . ?
C26 C21 C22 120.9(14) . . ?
C26 C21 S21 118.8(12) . . ?
C22 C21 S21 120.2(13) . . ?
C21 C22 C23 117.2(15) . . ?
C21 C22 S22 117.0(11) . . ?
C23 C22 S22 125.8(12) . . ?
C24 C23 C22 119.2(15) . . ?
C24 C23 C27 114.2(15) . . ?
C22 C23 C27 126.5(15) . . ?
C25 C24 C23 123.5(16) . . ?
C25 C24 H6 118.2 . . ?
C23 C24 H6 118.2 . . ?
C24 C25 C26 116(2) . . ?
C24 C25 H7 121.9 . . ?
C26 C25 H7 121.9 . . ?
C21 C26 C25 122.7(17) . . ?
C21 C26 H8 118.6 . . ?
C25 C26 H8 118.6 . . ?
O2 C27 N2 117.5(17) . . ?
O2 C27 C23 122.3(18) . . ?
N2 C27 C23 120.3(14) . . ?
C201 C28 N2 106.2(14) . . ?
C201 C28 C203 112(2) . . ?
N2 C28 C203 108.3(17) . . ?
C201 C28 C202 108(2) . . ?
N2 C28 C202 109.7(18) . . ?
C203 C28 C202 112(2) . . ?
N3 C31 C32 115.7(14) . . ?
N3 C31 H9 108.4 . . ?
C32 C31 H9 108.4 . . ?
N3 C31 H10 108.4 . . ?
C32 C31 H10 108.4 . . ?
H9 C31 H10 107.4 . . ?
C31 C32 H11 109.5 . . ?
C31 C32 H12 109.5 . . ?
H11 C32 H12 109.5 . . ?
C31 C32 H13 109.5 . . ?
H11 C32 H13 109.5 . . ?
H12 C32 H13 109.5 . . ?
N3 C33 C34 114.8(14) . . ?
N3 C33 H14 108.6 . . ?
C34 C33 H14 108.6 . . ?
N3 C33 H15 108.6 . . ?
C34 C33 H15 108.6 . . ?
H14 C33 H15 107.6 . . ?
C33 C34 H16 109.5 . . ?
C33 C34 H17 109.5 . . ?
H16 C34 H17 109.5 . . ?
C33 C34 H18 109.5 . . ?
H16 C34 H18 109.5 . . ?
H17 C34 H18 109.5 . . ?
C36 C35 N3 114.7(13) . . ?
C36 C35 H19 108.6 . . ?
N3 C35 H19 108.6 . . ?
C36 C35 H20 108.6 . . ?
N3 C35 H20 108.6 . . ?
H19 C35 H20 107.6 . . ?
C35 C36 H21 109.5 . . ?
C35 C36 H22 109.5 . . ?
H21 C36 H22 109.5 . . ?
C35 C36 H23 109.5 . . ?
H21 C36 H23 109.5 . . ?
H22 C36 H23 109.5 . . ?
C38 C37 N3 118.5(15) . . ?
C38 C37 H24 107.7 . . ?
N3 C37 H24 107.7 . . ?
C38 C37 H25 107.7 . . ?
N3 C37 H25 107.7 . . ?
H24 C37 H25 107.1 . . ?
C37 C38 H26 109.5 . . ?
C37 C38 H27 109.5 . . ?
H26 C38 H27 109.5 . . ?
C37 C38 H28 109.5 . . ?
H26 C38 H28 109.5 . . ?
H27 C38 H28 109.5 . . ?
N4 C41 C42 118.0(17) . . ?
N4 C41 H29 107.8 . . ?
C42 C41 H29 107.8 . . ?
N4 C41 H30 107.8 . . ?
C42 C41 H30 107.8 . . ?
H29 C41 H30 107.1 . . ?
C41 C42 H31 109.5 . . ?
C41 C42 H32 109.5 . . ?
H31 C42 H32 109.5 . . ?
C41 C42 H33 109.5 . . ?
H31 C42 H33 109.5 . . ?
H32 C42 H33 109.5 . . ?
C44 C43 N4 112.9(17) . . ?
C44 C43 H34 109.0 . . ?
N4 C43 H34 109.0 . . ?
C44 C43 H35 109.0 . . ?
N4 C43 H35 109.0 . . ?
H34 C43 H35 107.8 . . ?
C43 C44 H36 109.5 . . ?
C43 C44 H37 109.5 . . ?
H36 C44 H37 109.5 . . ?
C43 C44 H38 109.5 . . ?
H36 C44 H38 109.5 . . ?
H37 C44 H38 109.5 . . ?
N4 C45 C46 113.6(16) . . ?
N4 C45 H39 108.8 . . ?
C46 C45 H39 108.8 . . ?
N4 C45 H40 108.8 . . ?
C46 C45 H40 108.8 . . ?
H39 C45 H40 107.7 . . ?
C45 C46 H41 109.5 . . ?
C45 C46 H42 109.5 . . ?
H41 C46 H42 109.5 . . ?
C45 C46 H43 109.5 . . ?
H41 C46 H43 109.5 . . ?
H42 C46 H43 109.5 . . ?
N4 C47 C48 113.0(16) . . ?
N4 C47 H44 109.0 . . ?
C48 C47 H44 109.0 . . ?
N4 C47 H45 109.0 . . ?
C48 C47 H45 109.0 . . ?
H44 C47 H45 107.8 . . ?
C47 C48 H46 109.5 . . ?
C47 C48 H47 109.5 . . ?
H46 C48 H47 109.5 . . ?
C47 C48 H48 109.5 . . ?
H46 C48 H48 109.5 . . ?
H47 C48 H48 109.5 . . ?
C18 C101 H49 109.5 . . ?
C18 C101 H50 109.5 . . ?
H49 C101 H50 109.5 . . ?
C18 C101 H51 109.5 . . ?
H49 C101 H51 109.5 . . ?
H50 C101 H51 109.5 . . ?
C18 C102 H52 109.5 . . ?
C18 C102 H53 109.5 . . ?
H52 C102 H53 109.5 . . ?
C18 C102 H54 109.5 . . ?
H52 C102 H54 109.5 . . ?
H53 C102 H54 109.5 . . ?
C18 C103 H55 109.5 . . ?
C18 C103 H56 109.5 . . ?
H55 C103 H56 109.5 . . ?
C18 C103 H57 109.5 . . ?
H55 C103 H57 109.5 . . ?
H56 C103 H57 109.5 . . ?
C28 C201 H58 109.5 . . ?
C28 C201 H59 109.5 . . ?
H58 C201 H59 109.5 . . ?
C28 C201 H60 109.5 . . ?
H58 C201 H60 109.5 . . ?
H59 C201 H60 109.5 . . ?
C28 C202 H61 109.5 . . ?
C28 C202 H62 109.5 . . ?
H61 C202 H62 109.5 . . ?
C28 C202 H63 109.5 . . ?
H61 C202 H63 109.5 . . ?
H62 C202 H63 109.5 . . ?
C28 C203 H64 109.5 . . ?
C28 C203 H65 109.5 . . ?
H64 C203 H65 109.5 . . ?
C28 C203 H66 109.5 . . ?
H64 C203 H66 109.5 . . ?
H65 C203 H66 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 W1 S11 C11 -87.8(6) . . . . ?
S21 W1 S11 C11 93.1(5) . . . . ?
S12 W1 S11 C11 16.7(5) . . . . ?
S22 W1 S11 C11 164.9(5) . . . . ?
O3 W1 S12 C12 89.8(6) . . . . ?
S11 W1 S12 C12 -17.7(5) . . . . ?
S21 W1 S12 C12 -161.4(5) . . . . ?
S22 W1 S12 C12 -89.0(5) . . . . ?
O3 W1 S21 C21 -88.1(6) . . . . ?
S11 W1 S21 C21 91.0(5) . . . . ?
S12 W1 S21 C21 165.6(5) . . . . ?
S22 W1 S21 C21 18.0(5) . . . . ?
O3 W1 S22 C22 92.1(6) . . . . ?
S11 W1 S22 C22 -159.4(5) . . . . ?
S21 W1 S22 C22 -15.0(5) . . . . ?
S12 W1 S22 C22 -89.1(5) . . . . ?
W1 S11 C11 C12 -12.7(11) . . . . ?
W1 S11 C11 C16 167.0(10) . . . . ?
C16 C11 C12 C13 -2.7(18) . . . . ?
S11 C11 C12 C13 176.9(10) . . . . ?
C16 C11 C12 S12 177.5(10) . . . . ?
S11 C11 C12 S12 -2.9(15) . . . . ?
W1 S12 C12 C11 16.7(11) . . . . ?
W1 S12 C12 C13 -163.1(10) . . . . ?
C11 C12 C13 C14 0.4(19) . . . . ?
S12 C12 C13 C14 -179.8(11) . . . . ?
C11 C12 C13 C17 179.5(13) . . . . ?
S12 C12 C13 C17 -1(2) . . . . ?
C12 C13 C14 C15 0(2) . . . . ?
C17 C13 C14 C15 -179.6(13) . . . . ?
C13 C14 C15 C16 3(2) . . . . ?
C14 C15 C16 C11 -5(2) . . . . ?
C12 C11 C16 C15 5(2) . . . . ?
S11 C11 C16 C15 -174.6(11) . . . . ?
C18 N1 C17 O1 6(3) . . . . ?
C18 N1 C17 C13 -178.0(13) . . . . ?
C14 C13 C17 O1 21(2) . . . . ?
C12 C13 C17 O1 -158.2(15) . . . . ?
C14 C13 C17 N1 -155.7(14) . . . . ?
C12 C13 C17 N1 25(2) . . . . ?
C17 N1 C18 C102 58(2) . . . . ?
C17 N1 C18 C101 177.4(14) . . . . ?
C17 N1 C18 C103 -63.5(19) . . . . ?
W1 S21 C21 C26 162.3(10) . . . . ?
W1 S21 C21 C22 -20.2(11) . . . . ?
C26 C21 C22 C23 3.1(19) . . . . ?
S21 C21 C22 C23 -174.3(10) . . . . ?
C26 C21 C22 S22 -174.6(11) . . . . ?
S21 C21 C22 S22 7.9(15) . . . . ?
W1 S22 C22 C21 8.4(11) . . . . ?
W1 S22 C22 C23 -169.2(11) . . . . ?
C21 C22 C23 C24 -3(2) . . . . ?
S22 C22 C23 C24 174.8(12) . . . . ?
C21 C22 C23 C27 173.4(14) . . . . ?
S22 C22 C23 C27 -9(2) . . . . ?
C22 C23 C24 C25 -1(3) . . . . ?
C27 C23 C24 C25 -177.5(17) . . . . ?
C23 C24 C25 C26 4(3) . . . . ?
C22 C21 C26 C25 0(2) . . . . ?
S21 C21 C26 C25 177.6(13) . . . . ?
C24 C25 C26 C21 -4(3) . . . . ?
C28 N2 C27 O2 0(3) . . . . ?
C28 N2 C27 C23 178.2(17) . . . . ?
C24 C23 C27 O2 1(3) . . . . ?
C22 C23 C27 O2 -175.6(19) . . . . ?
C24 C23 C27 N2 -177.8(16) . . . . ?
C22 C23 C27 N2 6(3) . . . . ?
C27 N2 C28 C201 -175(2) . . . . ?
C27 N2 C28 C203 64(3) . . . . ?
C27 N2 C28 C202 -58(3) . . . . ?
C33 N3 C31 C32 58(2) . . . . ?
C35 N3 C31 C32 179.3(16) . . . . ?
C37 N3 C31 C32 -60(2) . . . . ?
C31 N3 C33 C34 55(2) . . . . ?
C35 N3 C33 C34 -63(2) . . . . ?
C37 N3 C33 C34 175.5(18) . . . . ?
C31 N3 C35 C36 -175.5(16) . . . . ?
C33 N3 C35 C36 -55(2) . . . . ?
C37 N3 C35 C36 64.3(19) . . . . ?
C31 N3 C37 C38 -58.7(18) . . . . ?
C33 N3 C37 C38 -178.9(17) . . . . ?
C35 N3 C37 C38 59.0(18) . . . . ?
C45 N4 C41 C42 176.3(19) . . . . ?
C47 N4 C41 C42 53(2) . . . . ?
C43 N4 C41 C42 -62(2) . . . . ?
C45 N4 C43 C44 62(3) . . . . ?
C47 N4 C43 C44 -177(2) . . . . ?
C41 N4 C43 C44 -59(3) . . . . ?
C47 N4 C45 C46 -60(2) . . . . ?
C41 N4 C45 C46 178.9(18) . . . . ?
C43 N4 C45 C46 57(2) . . . . ?
C45 N4 C47 C48 -60(3) . . . . ?
C41 N4 C47 C48 61(2) . . . . ?
C43 N4 C47 C48 179(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.983
_refine_diff_density_min         -2.664
_refine_diff_density_rms         0.180
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-H2O
_database_code_depnum_ccdc_archive 'CCDC 1413125'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_audit_creation_date             2015-07-11
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
(NEt4)2[W(S2C6H3CONH-t-Bu)3]-H2O
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H81 N5 O4 S6 W'
_chemical_formula_sum            'C49 H81 N5 O4 S6 W'
_chemical_formula_weight         1180.39

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
'-x, -y, z+1/2'

_cell_length_a                   21.3866(5)
_cell_length_b                   18.6641(4)
_cell_length_c                   29.515(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11781.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    200
_cell_measurement_reflns_used    65074
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.50

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             4896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.216
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            85613
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.018
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             20684
_reflns_number_gt                15384
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR2008 (Burla et al., 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_refine_special_details          'Twin, SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+130.5720P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.318(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         20684
_refine_ls_number_parameters     1172
_refine_ls_number_restraints     579
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0781
_refine_ls_wR_factor_ref         0.1503
_refine_ls_wR_factor_gt          0.1415
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000

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 0.65677(4) 0.00415(5) 0.11244(2) 0.0400(3) Uani 1 1 d . U . . .
W2 W 0.65294(4) 0.50680(5) 0.29094(2) 0.0371(3) Uani 1 1 d . U . . .
S11 S 0.7325(3) -0.0036(3) 0.1712(2) 0.0405(13) Uani 1 1 d . U . . .
S12 S 0.5895(3) 0.0110(5) 0.1771(2) 0.065(2) Uani 1 1 d . U . . .
S21 S 0.7225(3) -0.0733(4) 0.0717(2) 0.0525(16) Uani 1 1 d . U . . .
S22 S 0.5799(3) -0.0822(3) 0.0897(2) 0.0433(14) Uani 1 1 d . U . . .
S31 S 0.7252(3) 0.0942(4) 0.0823(2) 0.0569(17) Uani 1 1 d . U . . .
S32 S 0.5813(3) 0.0838(3) 0.0844(2) 0.0460(15) Uani 1 1 d . U . . .
S41 S 0.7290(2) 0.5304(3) 0.2345(2) 0.0433(14) Uani 1 1 d . U . . .
S42 S 0.5863(3) 0.5126(3) 0.2263(2) 0.0395(14) Uani 1 1 d . U . . .
S51 S 0.7202(3) 0.5766(3) 0.3373(2) 0.0441(14) Uani 1 1 d . U . . .
S52 S 0.5779(3) 0.5920(4) 0.3200(2) 0.0471(16) Uani 1 1 d . U . . .
S61 S 0.7169(3) 0.4108(3) 0.3147(2) 0.0438(14) Uani 1 1 d . U . . .
S62 S 0.5741(3) 0.4250(4) 0.3132(2) 0.0474(15) Uani 1 1 d . U . . .
O1 O 0.5148(9) 0.0331(13) 0.3210(7) 0.093(7) Uani 1 1 d . U . . .
O2 O 0.4865(10) -0.2747(12) 0.0459(8) 0.091(7) Uani 1 1 d . U . . .
O3 O 0.4854(13) 0.2821(16) 0.0257(10) 0.126(10) Uani 1 1 d . U . . .
O4 O 0.5159(8) 0.5192(8) 0.0836(5) 0.047(4) Uani 1 1 d . U . . .
O5 O 0.4909(10) 0.7837(12) 0.3851(8) 0.093(7) Uani 1 1 d . U . . .
O6 O 0.4743(11) 0.2234(13) 0.3631(8) 0.107(8) Uani 1 1 d . U . . .
O7 O 0.182(2) 0.551(3) 0.4324(16) 0.28(2) Uani 1 1 d . U . . .
O8 O 0.268(3) 0.494(3) 0.463(2) 0.31(3) Uani 1 1 d . U . . .
N1 N 0.4949(8) 0.0027(12) 0.2491(6) 0.070(5) Uani 1 1 d . U . . .
H1 H 0.5114 0.0029 0.2218 0.085 Uiso 1 1 calc R U . . .
N2 N 0.4702(10) -0.1618(12) 0.0472(8) 0.069(5) Uani 1 1 d . U . . .
H2 H 0.4900 -0.1205 0.0460 0.082 Uiso 1 1 calc R U . . .
N3 N 0.4768(10) 0.1892(13) 0.0708(8) 0.081(6) Uani 1 1 d . U . . .
H3 H 0.4954 0.1526 0.0838 0.098 Uiso 1 1 calc R U . . .
N4 N 0.4907(8) 0.5533(10) 0.1546(5) 0.050(4) Uani 1 1 d . U . . .
H4 H 0.5077 0.5716 0.1792 0.059 Uiso 1 1 calc R U . . .
N5 N 0.4715(9) 0.6685(12) 0.3665(8) 0.068(5) Uani 1 1 d . U . . .
H5 H 0.4886 0.6256 0.3666 0.082 Uiso 1 1 calc R U . . .
N6 N 0.4695(10) 0.3150(12) 0.3117(9) 0.082(6) Uani 1 1 d . U . . .
H6 H 0.4920 0.3411 0.2930 0.098 Uiso 1 1 calc R U . . .
N7 N 0.4146(10) 0.0095(11) 0.4351(8) 0.053(5) Uani 1 1 d . U . . .
N8 N 0.5841(9) 0.4784(12) 0.4669(7) 0.049(4) Uani 1 1 d . U . . .
N9 N 0.1411(12) 0.2253(15) 0.1862(8) 0.083(6) Uani 1 1 d . U . . .
N10 N 0.1394(12) 0.7311(14) 0.2184(9) 0.083(6) Uani 1 1 d . U . . .
C11 C 0.6980(9) -0.0013(10) 0.2247(6) 0.036(4) Uani 1 1 d . U . . .
C12 C 0.6325(11) 0.0087(16) 0.2288(8) 0.061(8) Uani 1 1 d . U . . .
C13 C 0.6034(11) 0.0122(13) 0.2713(8) 0.054(6) Uani 1 1 d . U . . .
C14 C 0.6424(11) 0.0067(14) 0.3091(7) 0.064(6) Uani 1 1 d . U . . .
H7 H 0.6241 0.0058 0.3384 0.077 Uiso 1 1 calc R U . . .
C15 C 0.7065(10) 0.0026(18) 0.3054(7) 0.081(9) Uani 1 1 d . U . . .
H8 H 0.7317 0.0026 0.3319 0.097 Uiso 1 1 calc R U . . .
C16 C 0.7342(11) -0.0016(17) 0.2634(8) 0.073(8) Uani 1 1 d . U . . .
H9 H 0.7784 -0.0048 0.2610 0.088 Uiso 1 1 calc R U . . .
C17 C 0.5352(8) 0.0185(6) 0.2833(6) 0.029(4) Uani 1 1 d . U . . .
C18 C 0.4244(10) -0.0158(15) 0.2510(9) 0.060(5) Uani 1 1 d . U . . .
C21 C 0.6774(11) -0.1463(13) 0.0504(8) 0.050(5) Uani 1 1 d . U . . .
C22 C 0.6111(11) -0.1496(13) 0.0563(8) 0.053(6) Uani 1 1 d . U . . .
C23 C 0.5767(14) -0.2107(15) 0.0396(11) 0.073(8) Uani 1 1 d . U . . .
C24 C 0.6116(14) -0.2574(14) 0.0161(11) 0.079(8) Uani 1 1 d . U . . .
H10 H 0.5895 -0.2967 0.0034 0.094 Uiso 1 1 calc R U . . .
C25 C 0.6718(14) -0.2564(17) 0.0083(11) 0.093(9) Uani 1 1 d . U . . .
H11 H 0.6913 -0.2931 -0.0090 0.112 Uiso 1 1 calc R U . . .
C26 C 0.7055(12) -0.2012(13) 0.0257(9) 0.067(7) Uani 1 1 d . U . . .
H12 H 0.7494 -0.1999 0.0209 0.080 Uiso 1 1 calc R U . . .
C27 C 0.5055(15) -0.219(2) 0.0436(11) 0.080(8) Uani 1 1 d . U . . .
C28 C 0.4056(13) -0.1577(18) 0.0526(11) 0.080(7) Uani 1 1 d . U . . .
C31 C 0.6812(12) 0.1663(15) 0.0582(8) 0.060(6) Uani 1 1 d . U . . .
C32 C 0.6149(11) 0.1591(13) 0.0602(7) 0.047(5) Uani 1 1 d . U . . .
C33 C 0.5847(14) 0.2200(17) 0.0381(12) 0.087(9) Uani 1 1 d . U . . .
C34 C 0.6146(15) 0.2778(16) 0.0204(11) 0.084(8) Uani 1 1 d . U . . .
H13 H 0.5917 0.3188 0.0109 0.101 Uiso 1 1 calc R U . . .
C35 C 0.6790(16) 0.276(2) 0.0164(13) 0.124(15) Uani 1 1 d . U . . .
H14 H 0.7004 0.3101 -0.0017 0.149 Uiso 1 1 calc R U . . .
C36 C 0.7121(14) 0.2227(15) 0.0394(11) 0.086(9) Uani 1 1 d . U . . .
H15 H 0.7563 0.2259 0.0419 0.104 Uiso 1 1 calc R U . . .
C37 C 0.5159(15) 0.2295(14) 0.0473(11) 0.074(8) Uani 1 1 d . U . . .
C38 C 0.4083(15) 0.1915(17) 0.0804(13) 0.099(9) Uani 1 1 d D U . . .
C41 C 0.6927(10) 0.5413(14) 0.1807(7) 0.055(6) Uani 1 1 d . U . . .
C42 C 0.6265(11) 0.5305(17) 0.1766(8) 0.060(6) Uani 1 1 d . U . . .
C43 C 0.5984(10) 0.5437(19) 0.1329(8) 0.080(8) Uani 1 1 d D U . . .
C44 C 0.6391(10) 0.5563(16) 0.0959(8) 0.077(8) Uani 1 1 d . U . . .
H16 H 0.6227 0.5542 0.0660 0.092 Uiso 1 1 calc R U . . .
C45 C 0.7021(11) 0.5715(16) 0.1017(8) 0.077(7) Uani 1 1 d . U . . .
H17 H 0.7259 0.5927 0.0780 0.092 Uiso 1 1 calc R U . . .
C46 C 0.7295(12) 0.5546(18) 0.1434(8) 0.087(8) Uani 1 1 d . U . . .
H18 H 0.7737 0.5524 0.1460 0.104 Uiso 1 1 calc R U . . .
C47 C 0.5319(7) 0.5336(7) 0.1162(6) 0.014(3) Uani 1 1 d D U . . .
C48 C 0.4244(10) 0.5438(14) 0.1533(8) 0.057(5) Uani 1 1 d D U . . .
C51 C 0.6772(9) 0.6409(10) 0.3674(7) 0.040(5) Uani 1 1 d . U . . .
C52 C 0.6125(11) 0.6536(14) 0.3599(8) 0.055(6) Uani 1 1 d . U . . .
C53 C 0.5761(12) 0.7020(16) 0.3806(13) 0.089(11) Uani 1 1 d D U . . .
C54 C 0.6072(13) 0.7404(17) 0.4162(10) 0.091(10) Uani 1 1 d . U . . .
H19 H 0.5833 0.7711 0.4352 0.109 Uiso 1 1 calc R U . . .
C55 C 0.6727(13) 0.7342(15) 0.4240(10) 0.085(8) Uani 1 1 d . U . . .
H20 H 0.6926 0.7633 0.4461 0.102 Uiso 1 1 calc R U . . .
C56 C 0.7073(11) 0.6848(12) 0.3986(9) 0.062(7) Uani 1 1 d . U . . .
H21 H 0.7513 0.6813 0.4027 0.074 Uiso 1 1 calc R U . . .
C57 C 0.5089(13) 0.724(2) 0.3776(12) 0.088(9) Uani 1 1 d D U . . .
C58 C 0.4030(13) 0.6733(19) 0.3540(10) 0.084(8) Uani 1 1 d D U . . .
C61 C 0.6713(11) 0.3382(13) 0.3307(8) 0.056(6) Uani 1 1 d . U . . .
C62 C 0.6057(10) 0.3409(13) 0.3286(7) 0.049(6) Uani 1 1 d . U . . .
C63 C 0.5702(10) 0.2835(14) 0.3413(10) 0.067(7) Uani 1 1 d D U . . .
C64 C 0.5998(13) 0.2125(16) 0.3516(11) 0.084(9) Uani 1 1 d . U . . .
H22 H 0.5767 0.1694 0.3553 0.101 Uiso 1 1 calc R U . . .
C65 C 0.6662(13) 0.2164(15) 0.3552(11) 0.088(8) Uani 1 1 d . U . . .
H23 H 0.6868 0.1763 0.3682 0.105 Uiso 1 1 calc R U . . .
C66 C 0.7039(13) 0.2737(14) 0.3414(12) 0.084(9) Uani 1 1 d . U . . .
H24 H 0.7481 0.2699 0.3392 0.101 Uiso 1 1 calc R U . . .
C67 C 0.4993(11) 0.2763(16) 0.3400(12) 0.079(9) Uani 1 1 d D U . . .
C68 C 0.4017(13) 0.3201(16) 0.3074(14) 0.096(9) Uani 1 1 d . U . . .
C71 C 0.3649(11) -0.0106(13) 0.4703(9) 0.054(5) Uani 1 1 d . U . . .
H26 H 0.3865 -0.0322 0.4967 0.065 Uiso 1 1 calc R U . . .
H25 H 0.3448 0.0341 0.4810 0.065 Uiso 1 1 calc R U . . .
C72 C 0.3160(13) -0.0595(13) 0.4559(10) 0.074(8) Uani 1 1 d . U . . .
H28 H 0.2872 -0.0683 0.4812 0.088 Uiso 1 1 calc R U . . .
H27 H 0.2929 -0.0384 0.4305 0.088 Uiso 1 1 calc R U . . .
H29 H 0.3348 -0.1049 0.4463 0.088 Uiso 1 1 calc R U . . .
C73 C 0.4487(16) -0.0543(16) 0.4194(9) 0.094(9) Uani 1 1 d . U . . .
H31 H 0.4804 -0.0391 0.3970 0.113 Uiso 1 1 calc R U . . .
H30 H 0.4189 -0.0864 0.4037 0.113 Uiso 1 1 calc R U . . .
C74 C 0.4823(18) -0.0979(18) 0.4582(11) 0.112(13) Uani 1 1 d . U . . .
H33 H 0.5038 -0.1393 0.4450 0.134 Uiso 1 1 calc R U . . .
H34 H 0.5128 -0.0670 0.4734 0.134 Uiso 1 1 calc R U . . .
H32 H 0.4511 -0.1144 0.4802 0.134 Uiso 1 1 calc R U . . .
C75 C 0.4593(11) 0.0628(16) 0.4590(8) 0.067(6) Uani 1 1 d . U . . .
H36 H 0.4349 0.1047 0.4696 0.080 Uiso 1 1 calc R U . . .
H35 H 0.4776 0.0393 0.4860 0.080 Uiso 1 1 calc R U . . .
C76 C 0.5102(12) 0.0880(17) 0.4297(9) 0.081(9) Uani 1 1 d . U . . .
H38 H 0.5367 0.1214 0.4466 0.098 Uiso 1 1 calc R U . . .
H37 H 0.5352 0.0470 0.4197 0.098 Uiso 1 1 calc R U . . .
H39 H 0.4925 0.1124 0.4033 0.098 Uiso 1 1 calc R U . . .
C77 C 0.3867(11) 0.0470(14) 0.3934(8) 0.062(6) Uani 1 1 d . U . . .
H40 H 0.4207 0.0538 0.3710 0.074 Uiso 1 1 calc R U . . .
H41 H 0.3556 0.0143 0.3796 0.074 Uiso 1 1 calc R U . . .
C78 C 0.3565(12) 0.1164(13) 0.4008(10) 0.076(8) Uani 1 1 d . U . . .
H43 H 0.3407 0.1348 0.3719 0.091 Uiso 1 1 calc R U . . .
H44 H 0.3216 0.1106 0.4220 0.091 Uiso 1 1 calc R U . . .
H42 H 0.3869 0.1502 0.4134 0.091 Uiso 1 1 calc R U . . .
C81 C 0.6342(12) 0.4723(17) 0.4325(8) 0.069(8) Uani 1 1 d . U . . .
H46 H 0.6542 0.5196 0.4284 0.083 Uiso 1 1 calc R U . . .
H45 H 0.6156 0.4580 0.4032 0.083 Uiso 1 1 calc R U . . .
C82 C 0.6851(14) 0.416(2) 0.4462(10) 0.110(13) Uani 1 1 d . U . . .
H48 H 0.7173 0.4139 0.4226 0.132 Uiso 1 1 calc R U . . .
H49 H 0.7044 0.4306 0.4750 0.132 Uiso 1 1 calc R U . . .
H47 H 0.6657 0.3690 0.4497 0.132 Uiso 1 1 calc R U . . .
C83 C 0.6083(12) 0.5160(15) 0.5092(7) 0.067(6) Uani 1 1 d . U . . .
H51 H 0.6434 0.4876 0.5218 0.080 Uiso 1 1 calc R U . . .
H50 H 0.5746 0.5168 0.5321 0.080 Uiso 1 1 calc R U . . .
C84 C 0.6309(14) 0.5927(15) 0.5013(10) 0.083(8) Uani 1 1 d . U . . .
H53 H 0.6457 0.6131 0.5300 0.099 Uiso 1 1 calc R U . . .
H52 H 0.6652 0.5925 0.4793 0.099 Uiso 1 1 calc R U . . .
H54 H 0.5963 0.6217 0.4896 0.099 Uiso 1 1 calc R U . . .
C85 C 0.5341(13) 0.527(2) 0.4461(9) 0.099(10) Uani 1 1 d . U . . .
H55 H 0.5550 0.5720 0.4361 0.119 Uiso 1 1 calc R U . . .
H56 H 0.5177 0.5035 0.4186 0.119 Uiso 1 1 calc R U . . .
C86 C 0.4785(13) 0.549(2) 0.4755(12) 0.114(13) Uani 1 1 d . U . . .
H58 H 0.4504 0.5797 0.4581 0.137 Uiso 1 1 calc R U . . .
H59 H 0.4559 0.5054 0.4849 0.137 Uiso 1 1 calc R U . . .
H57 H 0.4934 0.5742 0.5024 0.137 Uiso 1 1 calc R U . . .
C87 C 0.5541(12) 0.4079(16) 0.4811(9) 0.074(6) Uani 1 1 d . U . . .
H61 H 0.5859 0.3792 0.4973 0.089 Uiso 1 1 calc R U . . .
H60 H 0.5203 0.4188 0.5030 0.089 Uiso 1 1 calc R U . . .
C88 C 0.5277(18) 0.363(2) 0.4452(11) 0.130(16) Uani 1 1 d . U . . .
H63 H 0.5098 0.3198 0.4584 0.156 Uiso 1 1 calc R U . . .
H62 H 0.4949 0.3902 0.4293 0.156 Uiso 1 1 calc R U . . .
H64 H 0.5607 0.3504 0.4237 0.156 Uiso 1 1 calc R U . . .
C91 C 0.0993(17) 0.221(2) 0.1469(12) 0.140(16) Uani 1 1 d . U . . .
H66 H 0.1247 0.2197 0.1189 0.168 Uiso 1 1 calc R U . . .
H65 H 0.0728 0.2643 0.1459 0.168 Uiso 1 1 calc R U . . .
C92 C 0.055(2) 0.152(2) 0.1481(18) 0.20(3) Uani 1 1 d . U . . .
H68 H 0.0284 0.1515 0.1212 0.241 Uiso 1 1 calc R U . . .
H69 H 0.0811 0.1085 0.1484 0.241 Uiso 1 1 calc R U . . .
H67 H 0.0292 0.1531 0.1754 0.241 Uiso 1 1 calc R U . . .
C93 C 0.1791(13) 0.1652(19) 0.1994(12) 0.110(12) Uani 1 1 d . U . . .
H70 H 0.1518 0.1242 0.2072 0.132 Uiso 1 1 calc R U . . .
H71 H 0.2036 0.1780 0.2267 0.132 Uiso 1 1 calc R U . . .
C94 C 0.2264(17) 0.142(2) 0.1591(14) 0.156(18) Uani 1 1 d . U . . .
H73 H 0.2517 0.1012 0.1690 0.187 Uiso 1 1 calc R U . . .
H72 H 0.2022 0.1287 0.1322 0.187 Uiso 1 1 calc R U . . .
H74 H 0.2539 0.1825 0.1517 0.187 Uiso 1 1 calc R U . . .
C95 C 0.1744(16) 0.2889(19) 0.1774(12) 0.104(10) Uani 1 1 d . U . . .
H76 H 0.1438 0.3276 0.1716 0.125 Uiso 1 1 calc R U . . .
H75 H 0.1988 0.2820 0.1492 0.125 Uiso 1 1 calc R U . . .
C96 C 0.2215(19) 0.3155(19) 0.2165(14) 0.146(17) Uani 1 1 d . U . . .
H78 H 0.2420 0.3599 0.2068 0.175 Uiso 1 1 calc R U . . .
H79 H 0.1979 0.3242 0.2444 0.175 Uiso 1 1 calc R U . . .
H77 H 0.2531 0.2785 0.2219 0.175 Uiso 1 1 calc R U . . .
C97 C 0.0996(17) 0.239(2) 0.2259(13) 0.132(14) Uani 1 1 d . U . . .
H81 H 0.1271 0.2461 0.2525 0.158 Uiso 1 1 calc R U . . .
H80 H 0.0752 0.1952 0.2314 0.158 Uiso 1 1 calc R U . . .
C98 C 0.0516(19) 0.304(2) 0.2257(17) 0.17(2) Uani 1 1 d . U . . .
H83 H 0.0286 0.3048 0.2544 0.209 Uiso 1 1 calc R U . . .
H82 H 0.0743 0.3492 0.2219 0.209 Uiso 1 1 calc R U . . .
H84 H 0.0220 0.2979 0.2006 0.209 Uiso 1 1 calc R U . . .
C101 C 0.1041(15) 0.675(2) 0.2438(12) 0.121(11) Uani 1 1 d D U . . .
H85 H 0.0786 0.6481 0.2218 0.145 Uiso 1 1 calc R U . . .
H86 H 0.1347 0.6416 0.2570 0.145 Uiso 1 1 calc R U . . .
C102 C 0.063(2) 0.700(2) 0.2802(15) 0.171(19) Uani 1 1 d D U . . .
H88 H 0.0422 0.6585 0.2943 0.205 Uiso 1 1 calc R U . . .
H89 H 0.0872 0.7255 0.3031 0.205 Uiso 1 1 calc R U . . .
H87 H 0.0309 0.7321 0.2677 0.205 Uiso 1 1 calc R U . . .
C103 C 0.1833(15) 0.7748(17) 0.2492(13) 0.107(12) Uani 1 1 d . U . . .
H91 H 0.2065 0.8092 0.2300 0.128 Uiso 1 1 calc R U . . .
H90 H 0.1573 0.8029 0.2705 0.128 Uiso 1 1 calc R U . . .
C104 C 0.231(2) 0.732(3) 0.2768(19) 0.24(3) Uani 1 1 d . U . . .
H93 H 0.2561 0.7644 0.2951 0.283 Uiso 1 1 calc R U . . .
H92 H 0.2085 0.6984 0.2968 0.283 Uiso 1 1 calc R U . . .
H94 H 0.2578 0.7047 0.2562 0.283 Uiso 1 1 calc R U . . .
C105 C 0.1814(16) 0.686(2) 0.1852(13) 0.121(12) Uani 1 1 d . U . . .
H96 H 0.1555 0.6518 0.1675 0.146 Uiso 1 1 calc R U . . .
H95 H 0.2131 0.6581 0.2024 0.146 Uiso 1 1 calc R U . . .
C106 C 0.215(2) 0.744(2) 0.1519(15) 0.177(19) Uani 1 1 d . U . . .
H98 H 0.2420 0.7194 0.1302 0.213 Uiso 1 1 calc R U . . .
H99 H 0.1829 0.7712 0.1354 0.213 Uiso 1 1 calc R U . . .
H97 H 0.2401 0.7775 0.1701 0.213 Uiso 1 1 calc R U . . .
C107 C 0.0969(19) 0.786(2) 0.1970(15) 0.144(15) Uani 1 1 d . U . . .
H100 H 0.1222 0.8189 0.1781 0.172 Uiso 1 1 calc R U . . .
H101 H 0.0768 0.8149 0.2211 0.172 Uiso 1 1 calc R U . . .
C108 C 0.046(2) 0.752(3) 0.1676(16) 0.22(3) Uani 1 1 d . U . . .
H103 H 0.0199 0.7891 0.1544 0.262 Uiso 1 1 calc R U . . .
H102 H 0.0660 0.7239 0.1433 0.262 Uiso 1 1 calc R U . . .
H104 H 0.0206 0.7198 0.1863 0.262 Uiso 1 1 calc R U . . .
C111 C 0.4047(12) -0.0341(18) 0.2004(10) 0.094(9) Uani 1 1 d . U . . .
H105 H 0.4196 0.0037 0.1801 0.113 Uiso 1 1 calc R U . . .
H107 H 0.4234 -0.0800 0.1915 0.113 Uiso 1 1 calc R U . . .
H106 H 0.3591 -0.0375 0.1984 0.113 Uiso 1 1 calc R U . . .
C112 C 0.4026(14) 0.0629(14) 0.2624(11) 0.084(8) Uani 1 1 d . U . . .
H108 H 0.4182 0.0959 0.2392 0.101 Uiso 1 1 calc R U . . .
H109 H 0.3568 0.0648 0.2631 0.101 Uiso 1 1 calc R U . . .
H110 H 0.4192 0.0770 0.2921 0.101 Uiso 1 1 calc R U . . .
C113 C 0.4040(11) -0.0693(13) 0.2831(11) 0.077(7) Uani 1 1 d . U . . .
H113 H 0.3586 -0.0755 0.2807 0.093 Uiso 1 1 calc R U . . .
H112 H 0.4249 -0.1148 0.2766 0.093 Uiso 1 1 calc R U . . .
H111 H 0.4147 -0.0537 0.3139 0.093 Uiso 1 1 calc R U . . .
C121 C 0.3856(12) -0.0814(17) 0.0594(15) 0.112(12) Uani 1 1 d . U . . .
H115 H 0.3401 -0.0794 0.0632 0.134 Uiso 1 1 calc R U . . .
H116 H 0.4059 -0.0620 0.0865 0.134 Uiso 1 1 calc R U . . .
H114 H 0.3978 -0.0529 0.0329 0.134 Uiso 1 1 calc R U . . .
C122 C 0.381(2) -0.196(2) 0.0987(15) 0.148(15) Uani 1 1 d . U . . .
H117 H 0.3358 -0.1920 0.1009 0.178 Uiso 1 1 calc R U . . .
H119 H 0.3929 -0.2472 0.0980 0.178 Uiso 1 1 calc R U . . .
H118 H 0.4008 -0.1734 0.1250 0.178 Uiso 1 1 calc R U . . .
C123 C 0.3645(14) -0.190(2) 0.0187(13) 0.120(12) Uani 1 1 d . U . . .
H122 H 0.3208 -0.1823 0.0275 0.144 Uiso 1 1 calc R U . . .
H121 H 0.3721 -0.1675 -0.0108 0.144 Uiso 1 1 calc R U . . .
H120 H 0.3729 -0.2414 0.0167 0.144 Uiso 1 1 calc R U . . .
C131 C 0.3952(13) 0.1379(18) 0.1160(14) 0.121(11) Uani 1 1 d D U . . .
H125 H 0.4075 0.0903 0.1053 0.145 Uiso 1 1 calc R U . . .
H124 H 0.4192 0.1499 0.1433 0.145 Uiso 1 1 calc R U . . .
H123 H 0.3505 0.1381 0.1231 0.145 Uiso 1 1 calc R U . . .
C132 C 0.3779(14) 0.188(2) 0.0344(13) 0.123(12) Uani 1 1 d . U . . .
H127 H 0.3909 0.1443 0.0189 0.147 Uiso 1 1 calc R U . . .
H126 H 0.3323 0.1882 0.0380 0.147 Uiso 1 1 calc R U . . .
H128 H 0.3906 0.2299 0.0166 0.147 Uiso 1 1 calc R U . . .
C133 C 0.3875(17) 0.2573(18) 0.1021(13) 0.119(12) Uani 1 1 d . U . . .
H129 H 0.3939 0.2977 0.0814 0.143 Uiso 1 1 calc R U . . .
H130 H 0.3430 0.2534 0.1097 0.143 Uiso 1 1 calc R U . . .
H131 H 0.4117 0.2651 0.1299 0.143 Uiso 1 1 calc R U . . .
C141 C 0.4014(12) 0.5638(15) 0.1985(8) 0.073(7) Uani 1 1 d . U . . .
H132 H 0.3558 0.5583 0.1994 0.088 Uiso 1 1 calc R U . . .
H134 H 0.4205 0.5327 0.2213 0.088 Uiso 1 1 calc R U . . .
H133 H 0.4123 0.6138 0.2048 0.088 Uiso 1 1 calc R U . . .
C142 C 0.4019(10) 0.4667(13) 0.1397(10) 0.061(6) Uani 1 1 d . U . . .
H137 H 0.3561 0.4652 0.1397 0.074 Uiso 1 1 calc R U . . .
H136 H 0.4175 0.4550 0.1094 0.074 Uiso 1 1 calc R U . . .
H135 H 0.4180 0.4318 0.1616 0.074 Uiso 1 1 calc R U . . .
C143 C 0.3969(12) 0.6015(13) 0.1210(9) 0.075(7) Uani 1 1 d D U . . .
H139 H 0.3514 0.5962 0.1195 0.090 Uiso 1 1 calc R U . . .
H140 H 0.4073 0.6493 0.1325 0.090 Uiso 1 1 calc R U . . .
H138 H 0.4148 0.5954 0.0906 0.090 Uiso 1 1 calc R U . . .
C151 C 0.3834(15) 0.595(2) 0.3422(14) 0.122(12) Uani 1 1 d . U . . .
H141 H 0.3864 0.5651 0.3694 0.146 Uiso 1 1 calc R U . . .
H143 H 0.3402 0.5948 0.3311 0.146 Uiso 1 1 calc R U . . .
H142 H 0.4111 0.5761 0.3187 0.146 Uiso 1 1 calc R U . . .
C152 C 0.3986(14) 0.719(2) 0.3133(12) 0.142(16) Uani 1 1 d D U . . .
H145 H 0.4229 0.6976 0.2887 0.170 Uiso 1 1 calc R U . . .
H146 H 0.3547 0.7232 0.3041 0.170 Uiso 1 1 calc R U . . .
H144 H 0.4152 0.7668 0.3202 0.170 Uiso 1 1 calc R U . . .
C153 C 0.3689(16) 0.697(2) 0.3961(13) 0.122(13) Uani 1 1 d . U . . .
H149 H 0.3759 0.6614 0.4202 0.147 Uiso 1 1 calc R U . . .
H148 H 0.3845 0.7435 0.4058 0.147 Uiso 1 1 calc R U . . .
H147 H 0.3241 0.6999 0.3896 0.147 Uiso 1 1 calc R U . . .
C161 C 0.3884(17) 0.380(2) 0.2716(17) 0.164(17) Uani 1 1 d . U . . .
H152 H 0.3431 0.3854 0.2676 0.197 Uiso 1 1 calc R U . . .
H150 H 0.4062 0.4255 0.2822 0.197 Uiso 1 1 calc R U . . .
H151 H 0.4076 0.3668 0.2426 0.197 Uiso 1 1 calc R U . . .
C162 C 0.3708(14) 0.346(2) 0.3502(14) 0.127(13) Uani 1 1 d . U . . .
H154 H 0.3255 0.3486 0.3456 0.153 Uiso 1 1 calc R U . . .
H153 H 0.3801 0.3127 0.3749 0.153 Uiso 1 1 calc R U . . .
H155 H 0.3868 0.3937 0.3579 0.153 Uiso 1 1 calc R U . . .
C163 C 0.3764(13) 0.2501(16) 0.2900(13) 0.101(9) Uani 1 1 d . U . . .
H157 H 0.3308 0.2534 0.2871 0.122 Uiso 1 1 calc R U . . .
H156 H 0.3948 0.2396 0.2604 0.122 Uiso 1 1 calc R U . . .
H158 H 0.3870 0.2117 0.3113 0.122 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 S32 2.345(6) . ?
W1 S21 2.347(7) . ?
W1 S11 2.376(6) . ?
W1 S12 2.393(7) . ?
W1 S22 2.399(6) . ?
W1 S31 2.400(7) . ?
W2 S61 2.362(6) . ?
W2 S62 2.366(7) . ?
W2 S41 2.371(6) . ?
W2 S51 2.374(6) . ?
W2 S42 2.384(7) . ?
W2 S52 2.416(6) . ?
S11 C11 1.74(2) . ?
S12 C12 1.78(2) . ?
S21 C21 1.78(2) . ?
S22 C22 1.73(2) . ?
S31 C31 1.79(3) . ?
S32 C32 1.73(2) . ?
S41 C41 1.78(2) . ?
S42 C42 1.73(3) . ?
S51 C51 1.75(2) . ?
S52 C52 1.80(2) . ?
S61 C61 1.73(2) . ?
S62 C62 1.77(2) . ?
O1 C17 1.22(3) . ?
O2 C27 1.11(4) . ?
O3 C37 1.34(3) . ?
O4 C47 1.06(2) . ?
O5 C57 1.19(4) . ?
O6 C67 1.31(3) . ?
N1 C17 1.36(2) . ?
N1 C18 1.55(3) . ?
N2 C27 1.32(4) . ?
N2 C28 1.39(3) . ?
N3 C37 1.32(3) . ?
N3 C38 1.49(3) . ?
N4 C48 1.43(3) . ?
N4 C47 1.48(2) . ?
N5 C57 1.35(4) . ?
N5 C58 1.51(3) . ?
N6 C67 1.27(3) . ?
N6 C68 1.46(3) . ?
N7 C73 1.47(3) . ?
N7 C71 1.53(3) . ?
N7 C77 1.53(3) . ?
N7 C75 1.55(3) . ?
N8 C81 1.48(3) . ?
N8 C83 1.52(3) . ?
N8 C87 1.52(3) . ?
N8 C85 1.54(3) . ?
N9 C95 1.41(4) . ?
N9 C93 1.44(4) . ?
N9 C91 1.47(4) . ?
N9 C97 1.49(4) . ?
N10 C101 1.49(4) . ?
N10 C107 1.51(4) . ?
N10 C103 1.54(4) . ?
N10 C105 1.58(4) . ?
C11 C16 1.38(3) . ?
C11 C12 1.42(3) . ?
C12 C13 1.40(3) . ?
C13 C14 1.40(3) . ?
C13 C17 1.51(3) . ?
C14 C15 1.38(3) . ?
C15 C16 1.38(3) . ?
C18 C113 1.44(3) . ?
C18 C112 1.58(4) . ?
C18 C111 1.59(4) . ?
C21 C26 1.39(3) . ?
C21 C22 1.43(3) . ?
C22 C23 1.44(3) . ?
C23 C24 1.34(4) . ?
C23 C27 1.53(4) . ?
C24 C25 1.31(4) . ?
C25 C26 1.36(4) . ?
C28 C123 1.46(4) . ?
C28 C121 1.50(4) . ?
C28 C122 1.63(4) . ?
C31 C36 1.36(3) . ?
C31 C32 1.42(3) . ?
C32 C33 1.46(4) . ?
C33 C34 1.36(4) . ?
C33 C37 1.51(4) . ?
C34 C35 1.38(4) . ?
C35 C36 1.39(4) . ?
C38 C133 1.45(4) . ?
C38 C131 1.48(2) . ?
C38 C132 1.51(5) . ?
C41 C46 1.37(3) . ?
C41 C42 1.43(3) . ?
C42 C43 1.44(3) . ?
C43 C44 1.42(3) . ?
C43 C47 1.52(2) . ?
C44 C45 1.39(3) . ?
C45 C46 1.40(3) . ?
C48 C141 1.47(3) . ?
C48 C143 1.55(2) . ?
C48 C142 1.57(3) . ?
C51 C56 1.39(3) . ?
C51 C52 1.42(3) . ?
C52 C53 1.34(3) . ?
C53 C54 1.43(4) . ?
C53 C57 1.50(2) . ?
C54 C55 1.42(4) . ?
C55 C56 1.40(3) . ?
C58 C152 1.48(2) . ?
C58 C153 1.50(4) . ?
C58 C151 1.56(4) . ?
C61 C62 1.41(3) . ?
C61 C66 1.43(3) . ?
C62 C63 1.37(3) . ?
C63 C64 1.50(4) . ?
C63 C67 1.52(2) . ?
C64 C65 1.43(4) . ?
C65 C66 1.40(4) . ?
C68 C163 1.50(4) . ?
C68 C162 1.50(5) . ?
C68 C161 1.56(5) . ?
C71 C72 1.45(3) . ?
C73 C74 1.58(4) . ?
C75 C76 1.47(3) . ?
C77 C78 1.46(3) . ?
C81 C82 1.56(3) . ?
C83 C84 1.53(4) . ?
C85 C86 1.52(4) . ?
C87 C88 1.46(4) . ?
C91 C92 1.60(5) . ?
C93 C94 1.62(4) . ?
C95 C96 1.61(4) . ?
C97 C98 1.58(5) . ?
C101 C102 1.47(2) . ?
C103 C104 1.53(5) . ?
C105 C106 1.64(5) . ?
C107 C108 1.53(5) . ?

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
S32 W1 S21 128.4(2) . . ?
S32 W1 S11 139.9(2) . . ?
S21 W1 S11 85.9(2) . . ?
S32 W1 S12 80.4(3) . . ?
S21 W1 S12 143.3(3) . . ?
S11 W1 S12 80.3(2) . . ?
S32 W1 S22 81.7(2) . . ?
S21 W1 S22 81.5(2) . . ?
S11 W1 S22 129.1(2) . . ?
S12 W1 S22 81.2(2) . . ?
S32 W1 S31 81.1(2) . . ?
S21 W1 S31 82.9(2) . . ?
S11 W1 S31 84.1(2) . . ?
S12 W1 S31 128.6(3) . . ?
S22 W1 S31 141.7(3) . . ?
S61 W2 S62 80.9(2) . . ?
S61 W2 S41 87.2(2) . . ?
S62 W2 S41 143.5(2) . . ?
S61 W2 S51 83.9(2) . . ?
S62 W2 S51 128.7(2) . . ?
S41 W2 S51 83.6(2) . . ?
S61 W2 S42 128.2(2) . . ?
S62 W2 S42 80.0(2) . . ?
S41 W2 S42 80.7(2) . . ?
S51 W2 S42 143.0(2) . . ?
S61 W2 S52 141.1(3) . . ?
S62 W2 S52 81.6(2) . . ?
S41 W2 S52 125.7(2) . . ?
S51 W2 S52 80.6(2) . . ?
S42 W2 S52 81.9(2) . . ?
C11 S11 W1 111.8(7) . . ?
C12 S12 W1 111.8(9) . . ?
C21 S21 W1 109.1(8) . . ?
C22 S22 W1 112.5(9) . . ?
C31 S31 W1 110.6(9) . . ?
C32 S32 W1 112.0(8) . . ?
C41 S41 W2 110.4(7) . . ?
C42 S42 W2 113.0(8) . . ?
C51 S51 W2 110.5(7) . . ?
C52 S52 W2 112.3(8) . . ?
C61 S61 W2 110.3(8) . . ?
C62 S62 W2 111.9(8) . . ?
C17 N1 C18 129.6(17) . . ?
C27 N2 C28 129(3) . . ?
C37 N3 C38 135(3) . . ?
C48 N4 C47 122.6(17) . . ?
C57 N5 C58 126(2) . . ?
C67 N6 C68 126(2) . . ?
C73 N7 C71 111(2) . . ?
C73 N7 C77 108(2) . . ?
C71 N7 C77 112.7(19) . . ?
C73 N7 C75 111(2) . . ?
C71 N7 C75 106.0(19) . . ?
C77 N7 C75 108.2(19) . . ?
C81 N8 C83 111(2) . . ?
C81 N8 C87 115(2) . . ?
C83 N8 C87 108.4(19) . . ?
C81 N8 C85 106.1(19) . . ?
C83 N8 C85 107(2) . . ?
C87 N8 C85 109(2) . . ?
C95 N9 C93 115(3) . . ?
C95 N9 C91 102(3) . . ?
C93 N9 C91 121(3) . . ?
C95 N9 C97 107(3) . . ?
C93 N9 C97 105(2) . . ?
C91 N9 C97 106(3) . . ?
C101 N10 C107 112(3) . . ?
C101 N10 C103 112(3) . . ?
C107 N10 C103 105(2) . . ?
C101 N10 C105 103(2) . . ?
C107 N10 C105 117(3) . . ?
C103 N10 C105 108(2) . . ?
C16 C11 C12 119.0(19) . . ?
C16 C11 S11 120.8(16) . . ?
C12 C11 S11 119.8(15) . . ?
C13 C12 C11 121(2) . . ?
C13 C12 S12 122.4(18) . . ?
C11 C12 S12 116.1(17) . . ?
C14 C13 C12 117(2) . . ?
C14 C13 C17 113.2(19) . . ?
C12 C13 C17 130(2) . . ?
C15 C14 C13 122(2) . . ?
C16 C15 C14 120(2) . . ?
C15 C16 C11 120(2) . . ?
O1 C17 N1 119.8(18) . . ?
O1 C17 C13 125.2(19) . . ?
N1 C17 C13 114.9(17) . . ?
C113 C18 N1 118(2) . . ?
C113 C18 C112 114(2) . . ?
N1 C18 C112 95(2) . . ?
C113 C18 C111 113(2) . . ?
N1 C18 C111 105.7(17) . . ?
C112 C18 C111 109(2) . . ?
C26 C21 C22 117(2) . . ?
C26 C21 S21 120.9(19) . . ?
C22 C21 S21 121.7(18) . . ?
C21 C22 C23 120(2) . . ?
C21 C22 S22 114.9(18) . . ?
C23 C22 S22 125(2) . . ?
C24 C23 C22 114(3) . . ?
C24 C23 C27 122(3) . . ?
C22 C23 C27 124(3) . . ?
C25 C24 C23 129(3) . . ?
C24 C25 C26 118(3) . . ?
C25 C26 C21 122(3) . . ?
O2 C27 N2 123(3) . . ?
O2 C27 C23 118(3) . . ?
N2 C27 C23 119(3) . . ?
N2 C28 C123 120(3) . . ?
N2 C28 C121 111(2) . . ?
C123 C28 C121 108(3) . . ?
N2 C28 C122 113(3) . . ?
C123 C28 C122 101(3) . . ?
C121 C28 C122 103(3) . . ?
C36 C31 C32 125(3) . . ?
C36 C31 S31 119(2) . . ?
C32 C31 S31 115.9(19) . . ?
C31 C32 C33 110(2) . . ?
C31 C32 S32 120.4(19) . . ?
C33 C32 S32 129(2) . . ?
C34 C33 C32 126(3) . . ?
C34 C33 C37 116(3) . . ?
C32 C33 C37 116(3) . . ?
C33 C34 C35 119(3) . . ?
C34 C35 C36 119(3) . . ?
C31 C36 C35 120(3) . . ?
N3 C37 O3 111(3) . . ?
N3 C37 C33 130(3) . . ?
O3 C37 C33 118(3) . . ?
C133 C38 C131 102(3) . . ?
C133 C38 N3 114(3) . . ?
C131 C38 N3 108(2) . . ?
C133 C38 C132 107(3) . . ?
C131 C38 C132 122(4) . . ?
N3 C38 C132 105(3) . . ?
C46 C41 C42 121(2) . . ?
C46 C41 S41 119.0(17) . . ?
C42 C41 S41 119.3(16) . . ?
C41 C42 C43 118(2) . . ?
C41 C42 S42 116.4(17) . . ?
C43 C42 S42 125.6(18) . . ?
C44 C43 C42 117(2) . . ?
C44 C43 C47 110.3(19) . . ?
C42 C43 C47 131(2) . . ?
C45 C44 C43 122(2) . . ?
C44 C45 C46 118(2) . . ?
C41 C46 C45 120(2) . . ?
O4 C47 N4 124.6(16) . . ?
O4 C47 C43 129.1(19) . . ?
N4 C47 C43 106.1(16) . . ?
N4 C48 C141 106(2) . . ?
N4 C48 C143 107.8(19) . . ?
C141 C48 C143 105(2) . . ?
N4 C48 C142 115(2) . . ?
C141 C48 C142 111(2) . . ?
C143 C48 C142 111(2) . . ?
C56 C51 C52 117(2) . . ?
C56 C51 S51 119.8(16) . . ?
C52 C51 S51 123.0(16) . . ?
C53 C52 C51 127(2) . . ?
C53 C52 S52 119(2) . . ?
C51 C52 S52 113.2(17) . . ?
C52 C53 C54 114(2) . . ?
C52 C53 C57 136(3) . . ?
C54 C53 C57 111(3) . . ?
C55 C54 C53 122(2) . . ?
C56 C55 C54 119(2) . . ?
C51 C56 C55 120(2) . . ?
O5 C57 N5 125(3) . . ?
O5 C57 C53 124(3) . . ?
N5 C57 C53 112(3) . . ?
C152 C58 C153 118(3) . . ?
C152 C58 N5 107(2) . . ?
C153 C58 N5 107(3) . . ?
C152 C58 C151 110(3) . . ?
C153 C58 C151 109(3) . . ?
N5 C58 C151 105(2) . . ?
C62 C61 C66 122(2) . . ?
C62 C61 S61 121.5(18) . . ?
C66 C61 S61 116.4(18) . . ?
C63 C62 C61 121(2) . . ?
C63 C62 S62 123.7(18) . . ?
C61 C62 S62 115.1(18) . . ?
C62 C63 C64 121(2) . . ?
C62 C63 C67 128(2) . . ?
C64 C63 C67 110(2) . . ?
C65 C64 C63 113(2) . . ?
C66 C65 C64 126(3) . . ?
C65 C66 C61 115(2) . . ?
N6 C67 O6 124(2) . . ?
N6 C67 C63 118(2) . . ?
O6 C67 C63 117(3) . . ?
N6 C68 C163 109(2) . . ?
N6 C68 C162 113(3) . . ?
C163 C68 C162 114(3) . . ?
N6 C68 C161 107(3) . . ?
C163 C68 C161 109(3) . . ?
C162 C68 C161 105(3) . . ?
C72 C71 N7 117(2) . . ?
N7 C73 C74 115(2) . . ?
C76 C75 N7 113(2) . . ?
C78 C77 N7 117(2) . . ?
N8 C81 C82 112(2) . . ?
N8 C83 C84 114(2) . . ?
C86 C85 N8 118(2) . . ?
C88 C87 N8 117(2) . . ?
N9 C91 C92 113(3) . . ?
N9 C93 C94 111(3) . . ?
N9 C95 C96 116(3) . . ?
N9 C97 C98 121(3) . . ?
C102 C101 N10 117(3) . . ?
C104 C103 N10 116(3) . . ?
N10 C105 C106 105(3) . . ?
N10 C107 C108 112(4) . . ?

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
N1 H1 S12 0.88 2.13 2.938(18) 151.7 .
N2 H2 S22 0.88 2.42 3.05(2) 128.3 .
N3 H3 S32 0.88 2.24 3.01(2) 145.1 .
N4 H4 S42 0.88 2.44 3.040(16) 125.4 .
N5 H5 S52 0.88 2.44 3.02(2) 124.0 .
N6 H6 S62 0.88 2.43 3.04(2) 126.8 .
C71 H26 S32 0.99 2.85 3.81(3) 164.8 4_655
C74 H33 O5 0.98 2.29 3.09(4) 138.0 1_545
C76 H39 O6 0.98 2.42 3.29(4) 148.4 .
C77 H40 O1 0.99 2.53 3.49(3) 162.7 .
C81 H45 S62 0.99 2.87 3.85(3) 173.1 .
C83 H50 O4 0.99 2.55 3.51(3) 163.1 4_665
C93 H70 S42 0.99 2.97 3.95(3) 171.3 3_455
C96 H78 S11 0.98 2.89 3.76(3) 149.2 3_455
C98 H82 S12 0.98 2.94 3.83(4) 150.4 3_455
C103 H90 S52 0.99 2.98 3.95(3) 169.0 3_465
C111 H106 S41 0.98 2.98 3.89(3) 154.9 3_455
C112 H110 O1 0.98 2.36 3.01(4) 122.9 .
C122 H119 O2 0.98 2.58 3.10(5) 113.6 .
C123 H120 O2 0.98 2.65 3.16(4) 112.3 .
C132 H128 O3 0.98 2.26 2.90(5) 121.7 .
C133 H129 O3 0.98 2.57 3.11(5) 114.6 .
C141 H132 S11 0.98 2.95 3.87(3) 156.5 3_455
C142 H137 S11 0.98 2.89 3.80(2) 155.0 3_455
C142 H136 O4 0.98 2.54 3.11(3) 116.8 .
C143 H138 O4 0.98 2.60 3.17(3) 117.4 .
C152 H144 O5 0.98 2.53 3.14(4) 120.2 .
C153 H148 O5 0.98 2.47 3.09(4) 120.9 .
C162 H153 O6 0.98 2.64 3.21(4) 117.2 .
C163 H158 O6 0.98 2.42 3.05(4) 121.2 .
N1 H1 S12 0.88 2.13 2.938(18) 151.7 .
N2 H2 S22 0.88 2.42 3.05(2) 128.3 .
N3 H3 S32 0.88 2.24 3.01(2) 145.1 .
N4 H4 S42 0.88 2.44 3.040(16) 125.4 .
N5 H5 S52 0.88 2.44 3.02(2) 124.0 .
N6 H6 S62 0.88 2.43 3.04(2) 126.8 .
C71 H26 S32 0.99 2.85 3.81(3) 164.8 4_655
C74 H33 O5 0.98 2.29 3.09(4) 138.0 1_545
C76 H39 O6 0.98 2.42 3.29(4) 148.4 .
C77 H40 O1 0.99 2.53 3.49(3) 162.7 .
C81 H45 S62 0.99 2.87 3.85(3) 173.1 .
C83 H50 O4 0.99 2.55 3.51(3) 163.1 4_665
C93 H70 S42 0.99 2.97 3.95(3) 171.3 3_455
C96 H78 S11 0.98 2.89 3.76(3) 149.2 3_455
C98 H82 S12 0.98 2.94 3.83(4) 150.4 3_455
C103 H90 S52 0.99 2.98 3.95(3) 169.0 3_465
C111 H106 S41 0.98 2.98 3.89(3) 154.9 3_455
C112 H110 O1 0.98 2.36 3.01(4) 122.9 .
C122 H119 O2 0.98 2.58 3.10(5) 113.6 .
C123 H120 O2 0.98 2.65 3.16(4) 112.3 .
C132 H128 O3 0.98 2.26 2.90(5) 121.7 .
C133 H129 O3 0.98 2.57 3.11(5) 114.6 .
C141 H132 S11 0.98 2.95 3.87(3) 156.5 3_455
C142 H137 S11 0.98 2.89 3.80(2) 155.0 3_455
C142 H136 O4 0.98 2.54 3.11(3) 116.8 .
C143 H138 O4 0.98 2.60 3.17(3) 117.4 .
C152 H144 O5 0.98 2.53 3.14(4) 120.2 .
C153 H148 O5 0.98 2.47 3.09(4) 120.9 .
C162 H153 O6 0.98 2.64 3.21(4) 117.2 .
C163 H158 O6 0.98 2.42 3.05(4) 121.2 .

_refine_diff_density_max         2.777
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.132


# start Validation Reply Form
_vrf_PLAT430_3-H2O               
;
PROBLEM: Short Inter D...A Contact  O7     ..  O8      ..       2.33 Ang.  
RESPONSE: Theese are water molecules of crystallization. They should form 
an intermolecular hydrogen bond although H atoms could not be found in the 
differential Fourier map because of the poor qualiy of the data.
;
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-2Et2O
_database_code_depnum_ccdc_archive 'CCDC 1413126'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
;
(NEt4)2[W2O5(1,2-S2-3-t-BuNHCOC6H3)2]-2Et2O
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H86 N4 O9 S4 W2'
_chemical_formula_sum            'C46 H86 N4 O9 S4 W2'
_chemical_formula_weight         1335.12

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.9606(14)
_cell_length_b                   8.7047(8)
_cell_length_c                   18.3212(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.438(5)
_cell_angle_gamma                90
_cell_volume                     2863.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    19911
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      'not measured'

_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.210
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26944
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.138
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6532
_reflns_number_gt                4605
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6532
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0437
_refine_ls_wR_factor_gt          0.0424
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_restrained_S_all      0.858
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.92187(2) 0.54858(2) 0.43202(2) 0.02396(5) Uani 1 1 d . . . . .
S11 S 0.90475(5) 0.27121(10) 0.45271(5) 0.0312(2) Uani 1 1 d . . . . .
S12 S 0.79316(5) 0.51808(10) 0.38780(5) 0.0302(2) Uani 1 1 d . . . . .
O1 O 0.64842(15) 0.3706(3) 0.22640(14) 0.0451(7) Uani 1 1 d . . . . .
O2 O 0.89228(14) 0.7237(3) 0.46463(13) 0.0408(7) Uani 1 1 d . . . . .
O3 O 0.96636(13) 0.5811(3) 0.35140(12) 0.0370(7) Uani 1 1 d . . . . .
O4 O 1.0000 0.5000 0.5000 0.0342(10) Uani 1 2 d S . P . .
O5 O 0.60938(16) 0.3483(3) 0.49681(14) 0.0535(8) Uani 1 1 d . . . . .
N1 N 0.62596(16) 0.4785(3) 0.33693(16) 0.0339(8) Uani 1 1 d . . . . .
H1 H 0.6324 0.4642 0.3842 0.041 Uiso 1 1 calc R U . . .
N2 N 1.12788(17) 0.0104(3) 0.35015(14) 0.0290(7) Uani 1 1 d . . . . .
C11 C 0.82522(19) 0.2108(4) 0.40273(17) 0.0254(8) Uani 1 1 d . . . . .
C12 C 0.77551(19) 0.3203(4) 0.37237(17) 0.0257(9) Uani 1 1 d . . . . .
C13 C 0.71384(19) 0.2691(4) 0.33088(17) 0.0271(9) Uani 1 1 d . . . . .
C14 C 0.7030(2) 0.1140(4) 0.3198(2) 0.0389(10) Uani 1 1 d . . . . .
H2 H 0.6622 0.0804 0.2899 0.047 Uiso 1 1 calc R U . . .
C15 C 0.7507(2) 0.0059(4) 0.3514(2) 0.0375(10) Uani 1 1 d . . . . .
H3 H 0.7421 -0.1008 0.3444 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8106(2) 0.0559(4) 0.39295(17) 0.0324(9) Uani 1 1 d . . . . .
H4 H 0.8428 -0.0176 0.4155 0.039 Uiso 1 1 calc R U . . .
C17 C 0.6591(2) 0.3780(4) 0.2932(2) 0.0311(9) Uani 1 1 d . . . . .
C18 C 0.5798(2) 0.6108(4) 0.3143(2) 0.0399(11) Uani 1 1 d . . . . .
C21 C 1.0495(2) -0.0216(4) 0.37436(18) 0.0347(9) Uani 1 1 d . . . . .
H5 H 1.0346 0.0617 0.4077 0.042 Uiso 1 1 calc R U . . .
H6 H 1.0500 -0.1185 0.4027 0.042 Uiso 1 1 calc R U . . .
C22 C 0.9910(2) -0.0350(5) 0.3138(2) 0.0504(11) Uani 1 1 d . . . . .
H7 H 0.9424 -0.0557 0.3349 0.061 Uiso 1 1 calc R U . . .
H8 H 0.9886 0.0613 0.2862 0.061 Uiso 1 1 calc R U . . .
H9 H 1.0040 -0.1194 0.2811 0.061 Uiso 1 1 calc R U . . .
C23 C 1.1763(2) 0.0191(4) 0.41954(18) 0.0363(10) Uani 1 1 d . . . . .
H10 H 1.1547 0.0971 0.4522 0.044 Uiso 1 1 calc R U . . .
H11 H 1.1737 -0.0812 0.4448 0.044 Uiso 1 1 calc R U . . .
C24 C 1.2575(2) 0.0584(5) 0.4091(2) 0.0500(11) Uani 1 1 d . . . . .
H12 H 1.2836 0.0611 0.4567 0.060 Uiso 1 1 calc R U . . .
H13 H 1.2803 -0.0197 0.3782 0.060 Uiso 1 1 calc R U . . .
H14 H 1.2612 0.1591 0.3856 0.060 Uiso 1 1 calc R U . . .
C25 C 1.1552(2) -0.1137(4) 0.29999(19) 0.0338(9) Uani 1 1 d . . . . .
H15 H 1.2079 -0.0918 0.2890 0.041 Uiso 1 1 calc R U . . .
H16 H 1.1262 -0.1075 0.2534 0.041 Uiso 1 1 calc R U . . .
C26 C 1.1504(2) -0.2763(4) 0.3282(2) 0.0452(11) Uani 1 1 d . . . . .
H17 H 1.1695 -0.3473 0.2916 0.054 Uiso 1 1 calc R U . . .
H18 H 1.1803 -0.2857 0.3734 0.054 Uiso 1 1 calc R U . . .
H19 H 1.0984 -0.3014 0.3378 0.054 Uiso 1 1 calc R U . . .
C27 C 1.1320(2) 0.1599(4) 0.30726(18) 0.0353(10) Uani 1 1 d . . . . .
H20 H 1.1837 0.1744 0.2913 0.042 Uiso 1 1 calc R U . . .
H21 H 1.0997 0.1506 0.2629 0.042 Uiso 1 1 calc R U . . .
C28 C 1.1088(2) 0.3007(4) 0.3489(2) 0.0476(12) Uani 1 1 d . . . . .
H22 H 1.1130 0.3915 0.3176 0.057 Uiso 1 1 calc R U . . .
H23 H 1.0571 0.2892 0.3638 0.057 Uiso 1 1 calc R U . . .
H24 H 1.1413 0.3131 0.3923 0.057 Uiso 1 1 calc R U . . .
C51 C 0.6671(3) 0.3627(5) 0.5509(2) 0.0657(14) Uani 1 1 d . . . . .
H25 H 0.7139 0.3190 0.5324 0.079 Uiso 1 1 calc R U . . .
H26 H 0.6536 0.3051 0.5952 0.079 Uiso 1 1 calc R U . . .
C52 C 0.6781(3) 0.5270(5) 0.5691(3) 0.0744(16) Uani 1 1 d . . . . .
H27 H 0.7179 0.5369 0.6064 0.089 Uiso 1 1 calc R U . . .
H28 H 0.6919 0.5833 0.5251 0.089 Uiso 1 1 calc R U . . .
H29 H 0.6318 0.5695 0.5878 0.089 Uiso 1 1 calc R U . . .
C53 C 0.5892(3) 0.1924(5) 0.4848(2) 0.0592(13) Uani 1 1 d . . . . .
H30 H 0.5771 0.1432 0.5318 0.071 Uiso 1 1 calc R U . . .
H31 H 0.6315 0.1361 0.4637 0.071 Uiso 1 1 calc R U . . .
C54 C 0.5230(3) 0.1853(5) 0.4335(2) 0.0712(15) Uani 1 1 d . . . . .
H32 H 0.5090 0.0778 0.4252 0.085 Uiso 1 1 calc R U . . .
H33 H 0.4812 0.2403 0.4549 0.085 Uiso 1 1 calc R U . . .
H34 H 0.5355 0.2332 0.3870 0.085 Uiso 1 1 calc R U . . .
C101 C 0.6211(2) 0.7029(4) 0.2570(2) 0.0518(13) Uani 1 1 d . . . . .
H35 H 0.5908 0.7913 0.2416 0.062 Uiso 1 1 calc R U . . .
H36 H 0.6687 0.7391 0.2781 0.062 Uiso 1 1 calc R U . . .
H37 H 0.6305 0.6374 0.2147 0.062 Uiso 1 1 calc R U . . .
C102 C 0.5677(3) 0.7069(5) 0.3816(2) 0.0683(15) Uani 1 1 d . . . . .
H38 H 0.5370 0.7964 0.3686 0.082 Uiso 1 1 calc R U . . .
H39 H 0.5423 0.6451 0.4182 0.082 Uiso 1 1 calc R U . . .
H40 H 0.6159 0.7414 0.4017 0.082 Uiso 1 1 calc R U . . .
C103 C 0.5052(2) 0.5566(5) 0.2818(2) 0.0582(13) Uani 1 1 d . . . . .
H41 H 0.4752 0.6459 0.2670 0.070 Uiso 1 1 calc R U . . .
H42 H 0.5139 0.4918 0.2391 0.070 Uiso 1 1 calc R U . . .
H43 H 0.4787 0.4972 0.3184 0.070 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O3 1.720(2) . ?
W1 O2 1.726(2) . ?
W1 O4 1.90035(18) . ?
W1 S12 2.4449(9) . ?
W1 S11 2.4645(9) . ?
S11 C11 1.758(3) . ?
S12 C12 1.772(3) . ?
O1 C17 1.236(4) . ?
O4 W1 1.90038(18) 3_766 ?
O5 C53 1.421(4) . ?
O5 C51 1.421(4) . ?
N1 C17 1.336(4) . ?
N1 C18 1.473(4) . ?
N1 H1 0.8800 . ?
N2 C25 1.509(4) . ?
N2 C21 1.512(4) . ?
N2 C27 1.523(4) . ?
N2 C23 1.524(4) . ?
C11 C16 1.385(4) . ?
C11 C12 1.411(4) . ?
C12 C13 1.400(4) . ?
C13 C14 1.378(4) . ?
C13 C17 1.518(4) . ?
C14 C15 1.390(5) . ?
C14 H2 0.9500 . ?
C15 C16 1.373(4) . ?
C15 H3 0.9500 . ?
C16 H4 0.9500 . ?
C18 C102 1.510(5) . ?
C18 C103 1.526(5) . ?
C18 C101 1.527(5) . ?
C21 C22 1.514(4) . ?
C21 H5 0.9900 . ?
C21 H6 0.9900 . ?
C22 H7 0.9800 . ?
C22 H8 0.9800 . ?
C22 H9 0.9800 . ?
C23 C24 1.516(5) . ?
C23 H10 0.9900 . ?
C23 H11 0.9900 . ?
C24 H12 0.9800 . ?
C24 H13 0.9800 . ?
C24 H14 0.9800 . ?
C25 C26 1.509(4) . ?
C25 H15 0.9900 . ?
C25 H16 0.9900 . ?
C26 H17 0.9800 . ?
C26 H18 0.9800 . ?
C26 H19 0.9800 . ?
C27 C28 1.507(5) . ?
C27 H20 0.9900 . ?
C27 H21 0.9900 . ?
C28 H22 0.9800 . ?
C28 H23 0.9800 . ?
C28 H24 0.9800 . ?
C51 C52 1.480(5) . ?
C51 H25 0.9900 . ?
C51 H26 0.9900 . ?
C52 H27 0.9800 . ?
C52 H28 0.9800 . ?
C52 H29 0.9800 . ?
C53 C54 1.498(5) . ?
C53 H30 0.9900 . ?
C53 H31 0.9900 . ?
C54 H32 0.9800 . ?
C54 H33 0.9800 . ?
C54 H34 0.9800 . ?
C101 H35 0.9800 . ?
C101 H36 0.9800 . ?
C101 H37 0.9800 . ?
C102 H38 0.9800 . ?
C102 H39 0.9800 . ?
C102 H40 0.9800 . ?
C103 H41 0.9800 . ?
C103 H42 0.9800 . ?
C103 H43 0.9800 . ?

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
O3 W1 O2 107.78(12) . . ?
O3 W1 O4 104.37(7) . . ?
O2 W1 O4 101.45(7) . . ?
O3 W1 S12 100.90(7) . . ?
O2 W1 S12 85.05(8) . . ?
O4 W1 S12 150.40(2) . . ?
O3 W1 S11 110.85(8) . . ?
O2 W1 S11 140.47(9) . . ?
O4 W1 S11 76.95(2) . . ?
S12 W1 S11 79.86(3) . . ?
C11 S11 W1 108.40(11) . . ?
C12 S12 W1 108.80(11) . . ?
W1 O4 W1 180.0 . 3_766 ?
C53 O5 C51 111.8(3) . . ?
C17 N1 C18 126.9(3) . . ?
C17 N1 H1 116.6 . . ?
C18 N1 H1 116.6 . . ?
C25 N2 C21 111.5(3) . . ?
C25 N2 C27 106.1(3) . . ?
C21 N2 C27 111.5(3) . . ?
C25 N2 C23 110.9(3) . . ?
C21 N2 C23 106.2(3) . . ?
C27 N2 C23 110.7(3) . . ?
C16 C11 C12 119.4(3) . . ?
C16 C11 S11 120.5(2) . . ?
C12 C11 S11 120.1(3) . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 S12 122.1(3) . . ?
C11 C12 S12 119.0(2) . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 C17 117.2(3) . . ?
C12 C13 C17 122.8(3) . . ?
C13 C14 C15 121.3(3) . . ?
C13 C14 H2 119.4 . . ?
C15 C14 H2 119.4 . . ?
C16 C15 C14 118.9(3) . . ?
C16 C15 H3 120.6 . . ?
C14 C15 H3 120.6 . . ?
C15 C16 C11 121.6(3) . . ?
C15 C16 H4 119.2 . . ?
C11 C16 H4 119.2 . . ?
O1 C17 N1 124.5(3) . . ?
O1 C17 C13 120.0(3) . . ?
N1 C17 C13 115.5(3) . . ?
N1 C18 C102 107.1(3) . . ?
N1 C18 C103 110.5(3) . . ?
C102 C18 C103 110.3(4) . . ?
N1 C18 C101 108.9(3) . . ?
C102 C18 C101 110.7(3) . . ?
C103 C18 C101 109.4(3) . . ?
N2 C21 C22 115.7(3) . . ?
N2 C21 H5 108.4 . . ?
C22 C21 H5 108.4 . . ?
N2 C21 H6 108.4 . . ?
C22 C21 H6 108.4 . . ?
H5 C21 H6 107.4 . . ?
C21 C22 H7 109.5 . . ?
C21 C22 H8 109.5 . . ?
H7 C22 H8 109.5 . . ?
C21 C22 H9 109.5 . . ?
H7 C22 H9 109.5 . . ?
H8 C22 H9 109.5 . . ?
C24 C23 N2 115.9(3) . . ?
C24 C23 H10 108.3 . . ?
N2 C23 H10 108.3 . . ?
C24 C23 H11 108.3 . . ?
N2 C23 H11 108.3 . . ?
H10 C23 H11 107.4 . . ?
C23 C24 H12 109.5 . . ?
C23 C24 H13 109.5 . . ?
H12 C24 H13 109.5 . . ?
C23 C24 H14 109.5 . . ?
H12 C24 H14 109.5 . . ?
H13 C24 H14 109.5 . . ?
N2 C25 C26 116.2(3) . . ?
N2 C25 H15 108.2 . . ?
C26 C25 H15 108.2 . . ?
N2 C25 H16 108.2 . . ?
C26 C25 H16 108.2 . . ?
H15 C25 H16 107.4 . . ?
C25 C26 H17 109.5 . . ?
C25 C26 H18 109.5 . . ?
H17 C26 H18 109.5 . . ?
C25 C26 H19 109.5 . . ?
H17 C26 H19 109.5 . . ?
H18 C26 H19 109.5 . . ?
C28 C27 N2 114.6(3) . . ?
C28 C27 H20 108.6 . . ?
N2 C27 H20 108.6 . . ?
C28 C27 H21 108.6 . . ?
N2 C27 H21 108.6 . . ?
H20 C27 H21 107.6 . . ?
C27 C28 H22 109.5 . . ?
C27 C28 H23 109.5 . . ?
H22 C28 H23 109.5 . . ?
C27 C28 H24 109.5 . . ?
H22 C28 H24 109.5 . . ?
H23 C28 H24 109.5 . . ?
O5 C51 C52 109.5(3) . . ?
O5 C51 H25 109.8 . . ?
C52 C51 H25 109.8 . . ?
O5 C51 H26 109.8 . . ?
C52 C51 H26 109.8 . . ?
H25 C51 H26 108.2 . . ?
C51 C52 H27 109.5 . . ?
C51 C52 H28 109.5 . . ?
H27 C52 H28 109.5 . . ?
C51 C52 H29 109.5 . . ?
H27 C52 H29 109.5 . . ?
H28 C52 H29 109.5 . . ?
O5 C53 C54 109.4(3) . . ?
O5 C53 H30 109.8 . . ?
C54 C53 H30 109.8 . . ?
O5 C53 H31 109.8 . . ?
C54 C53 H31 109.8 . . ?
H30 C53 H31 108.3 . . ?
C53 C54 H32 109.5 . . ?
C53 C54 H33 109.5 . . ?
H32 C54 H33 109.5 . . ?
C53 C54 H34 109.5 . . ?
H32 C54 H34 109.5 . . ?
H33 C54 H34 109.5 . . ?
C18 C101 H35 109.5 . . ?
C18 C101 H36 109.5 . . ?
H35 C101 H36 109.5 . . ?
C18 C101 H37 109.5 . . ?
H35 C101 H37 109.5 . . ?
H36 C101 H37 109.5 . . ?
C18 C102 H38 109.5 . . ?
C18 C102 H39 109.5 . . ?
H38 C102 H39 109.5 . . ?
C18 C102 H40 109.5 . . ?
H38 C102 H40 109.5 . . ?
H39 C102 H40 109.5 . . ?
C18 C103 H41 109.5 . . ?
C18 C103 H42 109.5 . . ?
H41 C103 H42 109.5 . . ?
C18 C103 H43 109.5 . . ?
H41 C103 H43 109.5 . . ?
H42 C103 H43 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 S11 C11 C16 167.4(3) . . . . ?
W1 S11 C11 C12 -12.8(3) . . . . ?
C16 C11 C12 C13 -2.2(5) . . . . ?
S11 C11 C12 C13 178.0(3) . . . . ?
C16 C11 C12 S12 177.9(3) . . . . ?
S11 C11 C12 S12 -1.9(4) . . . . ?
W1 S12 C12 C13 -164.2(3) . . . . ?
W1 S12 C12 C11 15.7(3) . . . . ?
C11 C12 C13 C14 -0.6(5) . . . . ?
S12 C12 C13 C14 179.3(3) . . . . ?
C11 C12 C13 C17 -177.2(3) . . . . ?
S12 C12 C13 C17 2.6(5) . . . . ?
C12 C13 C14 C15 2.6(6) . . . . ?
C17 C13 C14 C15 179.4(4) . . . . ?
C13 C14 C15 C16 -1.6(6) . . . . ?
C14 C15 C16 C11 -1.3(6) . . . . ?
C12 C11 C16 C15 3.2(6) . . . . ?
S11 C11 C16 C15 -177.0(3) . . . . ?
C18 N1 C17 O1 -9.1(6) . . . . ?
C18 N1 C17 C13 170.1(3) . . . . ?
C14 C13 C17 O1 -54.9(5) . . . . ?
C12 C13 C17 O1 121.8(4) . . . . ?
C14 C13 C17 N1 125.9(4) . . . . ?
C12 C13 C17 N1 -57.4(5) . . . . ?
C17 N1 C18 C102 -169.0(4) . . . . ?
C17 N1 C18 C103 70.8(5) . . . . ?
C17 N1 C18 C101 -49.4(5) . . . . ?
C25 N2 C21 C22 -59.2(4) . . . . ?
C27 N2 C21 C22 59.2(4) . . . . ?
C23 N2 C21 C22 179.9(3) . . . . ?
C25 N2 C23 C24 61.6(4) . . . . ?
C21 N2 C23 C24 -177.1(3) . . . . ?
C27 N2 C23 C24 -55.9(4) . . . . ?
C21 N2 C25 C26 -53.5(4) . . . . ?
C27 N2 C25 C26 -175.1(3) . . . . ?
C23 N2 C25 C26 64.6(4) . . . . ?
C25 N2 C27 C28 -178.3(3) . . . . ?
C21 N2 C27 C28 60.1(4) . . . . ?
C23 N2 C27 C28 -57.9(4) . . . . ?
C53 O5 C51 C52 -171.7(4) . . . . ?
C51 O5 C53 C54 173.9(4) . . . . ?

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
N1 H1 O5 0.88 2.34 3.162(4) 155.0 .

_refine_diff_density_max         0.829
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.125

_shelxl_version_number           2014/6

#===END



_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
