# 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_apx012n
_database_code_depnum_ccdc_archive 'CCDC 1404547'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H48 O P4 S8 U'
_chemical_formula_weight         1307.29

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9621(7)
_cell_length_b                   13.3551(9)
_cell_length_c                   18.5207(12)
_cell_angle_alpha                94.845(1)
_cell_angle_beta                 95.092(1)
_cell_angle_gamma                96.650(1)
_cell_volume                     2670.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    3.510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4622
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30118
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         25.64
_reflns_number_total             10022
_reflns_number_gt                9010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0676P)²+0.0000P] 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_number_reflns         10022
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0913
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.734681(12) 0.742340(10) 0.741647(7) 0.01462(6) Uani 1 1 d . . .
S1 S 0.48409(9) 0.69727(7) 0.77430(6) 0.0187(2) Uani 1 1 d . . .
S2 S 0.65765(9) 0.91685(8) 0.81117(6) 0.0201(2) Uani 1 1 d . . .
S3 S 0.59706(9) 0.76994(8) 0.61137(6) 0.0211(2) Uani 1 1 d . . .
S4 S 0.86359(9) 0.90181(8) 0.67212(6) 0.0198(2) Uani 1 1 d . . .
S5 S 0.76862(9) 0.63977(8) 0.86908(5) 0.0188(2) Uani 1 1 d . . .
S6 S 0.96032(9) 0.82734(8) 0.82477(5) 0.0179(2) Uani 1 1 d . . .
S7 S 0.91114(10) 0.64186(8) 0.67350(6) 0.0237(2) Uani 1 1 d . . .
S8 S 0.62969(9) 0.53861(7) 0.69093(5) 0.0177(2) Uani 1 1 d . . .
P1 P 0.48565(9) 0.84322(8) 0.81184(6) 0.0164(2) Uani 1 1 d . . .
P2 P 0.73572(9) 0.86951(8) 0.58611(6) 0.0184(2) Uani 1 1 d . . .
P3 P 0.92440(9) 0.73453(8) 0.90202(6) 0.0162(2) Uani 1 1 d . . .
P4 P 0.79390(9) 0.51253(8) 0.65747(6) 0.0177(2) Uani 1 1 d . . .
O1 O 0.4134(3) 0.2789(3) 0.79979(19) 0.0398(9) Uani 1 1 d . . .
C1 C 0.4402(3) 0.8537(3) 0.9040(2) 0.0175(8) Uani 1 1 d . . .
C2 C 0.4904(4) 0.7935(3) 0.9537(2) 0.0246(9) Uani 1 1 d . . .
H2 H 0.5412 0.7462 0.9389 0.030 Uiso 1 1 calc R . .
C3 C 0.4643(4) 0.8046(4) 1.0255(2) 0.0289(10) Uani 1 1 d . . .
H3 H 0.4972 0.7641 1.0588 0.035 Uiso 1 1 calc R . .
C4 C 0.3896(4) 0.8756(3) 1.0482(2) 0.0255(10) Uani 1 1 d . . .
H4 H 0.3726 0.8823 1.0965 0.031 Uiso 1 1 calc R . .
C5 C 0.3399(4) 0.9367(3) 0.9990(2) 0.0242(9) Uani 1 1 d . . .
H5 H 0.2901 0.9846 1.0143 0.029 Uiso 1 1 calc R . .
C6 C 0.3655(4) 0.9255(3) 0.9263(2) 0.0209(9) Uani 1 1 d . . .
H6 H 0.3327 0.9660 0.8929 0.025 Uiso 1 1 calc R . .
C7 C 0.3740(4) 0.9028(3) 0.7578(2) 0.0177(8) Uani 1 1 d . . .
C8 C 0.2706(4) 0.8435(3) 0.7222(2) 0.0219(9) Uani 1 1 d . . .
H8 H 0.2618 0.7736 0.7238 0.026 Uiso 1 1 calc R . .
C9 C 0.1797(4) 0.8888(3) 0.6841(2) 0.0264(10) Uani 1 1 d . . .
H9 H 0.1105 0.8490 0.6600 0.032 Uiso 1 1 calc R . .
C10 C 0.1922(4) 0.9932(3) 0.6819(2) 0.0248(9) Uani 1 1 d . . .
H10 H 0.1310 1.0232 0.6569 0.030 Uiso 1 1 calc R . .
C11 C 0.2965(4) 1.0528(3) 0.7174(2) 0.0249(9) Uani 1 1 d . . .
H11 H 0.3051 1.1227 0.7158 0.030 Uiso 1 1 calc R . .
C12 C 0.3878(4) 1.0078(3) 0.7551(2) 0.0237(9) Uani 1 1 d . . .
H12 H 0.4578 1.0475 0.7785 0.028 Uiso 1 1 calc R . .
C13 C 0.6786(4) 0.9857(3) 0.5630(2) 0.0198(9) Uani 1 1 d . . .
C14 C 0.6008(5) 1.0301(4) 0.6079(3) 0.0340(11) Uani 1 1 d . . .
H14 H 0.5745 0.9972 0.6471 0.041 Uiso 1 1 calc R . .
C15 C 0.5621(5) 1.1222(4) 0.5950(3) 0.0356(12) Uani 1 1 d . . .
H15 H 0.5094 1.1509 0.6252 0.043 Uiso 1 1 calc R . .
C16 C 0.6015(4) 1.1716(3) 0.5374(2) 0.0255(10) Uani 1 1 d . . .
H16 H 0.5764 1.2342 0.5293 0.031 Uiso 1 1 calc R . .
C17 C 0.6774(5) 1.1293(4) 0.4918(3) 0.0322(11) Uani 1 1 d . . .
H17 H 0.7032 1.1628 0.4528 0.039 Uiso 1 1 calc R . .
C18 C 0.7160(4) 1.0355(3) 0.5041(2) 0.0272(10) Uani 1 1 d . . .
H18 H 0.7668 1.0063 0.4729 0.033 Uiso 1 1 calc R . .
C19 C 0.8013(4) 0.8192(3) 0.5061(2) 0.0208(9) Uani 1 1 d . . .
C20 C 0.7289(5) 0.7507(4) 0.4543(3) 0.0327(11) Uani 1 1 d . . .
H20 H 0.6478 0.7283 0.4618 0.039 Uiso 1 1 calc R . .
C21 C 0.7776(5) 0.7154(4) 0.3914(3) 0.0411(13) Uani 1 1 d . . .
H21 H 0.7287 0.6696 0.3570 0.049 Uiso 1 1 calc R . .
C22 C 0.8968(5) 0.7478(4) 0.3798(3) 0.0365(12) Uani 1 1 d . . .
H22 H 0.9285 0.7245 0.3374 0.044 Uiso 1 1 calc R . .
C23 C 0.9703(4) 0.8152(4) 0.4313(3) 0.0343(11) Uani 1 1 d . . .
H23 H 1.0514 0.8366 0.4234 0.041 Uiso 1 1 calc R . .
C24 C 0.9238(4) 0.8513(4) 0.4947(2) 0.0283(10) Uani 1 1 d . . .
H24 H 0.9737 0.8963 0.5291 0.034 Uiso 1 1 calc R . .
C25 C 0.9112(4) 0.8035(3) 0.9887(2) 0.0183(8) Uani 1 1 d . . .
C26 C 0.8078(4) 0.7881(4) 1.0271(2) 0.0254(10) Uani 1 1 d . . .
H26 H 0.7414 0.7407 1.0081 0.030 Uiso 1 1 calc R . .
C27 C 0.8043(4) 0.8433(4) 1.0932(2) 0.0281(10) Uani 1 1 d . . .
H27 H 0.7358 0.8323 1.1191 0.034 Uiso 1 1 calc R . .
C28 C 0.9018(4) 0.9147(3) 1.1212(2) 0.0258(10) Uani 1 1 d . . .
H28 H 0.8975 0.9531 1.1649 0.031 Uiso 1 1 calc R . .
C29 C 1.0063(4) 0.9295(3) 1.0843(2) 0.0244(9) Uani 1 1 d . . .
H29 H 1.0729 0.9763 1.1039 0.029 Uiso 1 1 calc R . .
C30 C 1.0104(4) 0.8739(3) 1.0181(2) 0.0226(9) Uani 1 1 d . . .
H30 H 1.0801 0.8837 0.9931 0.027 Uiso 1 1 calc R . .
C31 C 1.0555(4) 0.6657(3) 0.9221(2) 0.0176(8) Uani 1 1 d . . .
C32 C 1.0663(4) 0.6225(3) 0.9874(2) 0.0251(10) Uani 1 1 d . . .
H32 H 1.0086 0.6308 1.0206 0.030 Uiso 1 1 calc R . .
C33 C 1.1630(4) 0.5666(3) 1.0034(2) 0.0271(10) Uani 1 1 d . . .
H33 H 1.1704 0.5377 1.0473 0.033 Uiso 1 1 calc R . .
C34 C 1.2480(4) 0.5545(4) 0.9536(3) 0.0303(11) Uani 1 1 d . . .
H34 H 1.3124 0.5166 0.9640 0.036 Uiso 1 1 calc R . .
C35 C 1.2384(4) 0.5976(4) 0.8891(3) 0.0318(11) Uani 1 1 d . . .
H35 H 1.2968 0.5898 0.8563 0.038 Uiso 1 1 calc R . .
C36 C 1.1409(4) 0.6534(3) 0.8724(2) 0.0253(10) Uani 1 1 d . . .
H36 H 1.1336 0.6820 0.8284 0.030 Uiso 1 1 calc R . .
C37 C 0.8556(4) 0.4153(3) 0.7077(2) 0.0231(9) Uani 1 1 d . . .
C38 C 0.9463(4) 0.4414(4) 0.7659(2) 0.0322(11) Uani 1 1 d . . .
H38 H 0.9818 0.5083 0.7764 0.039 Uiso 1 1 calc R . .
C39 C 0.9833(5) 0.3682(5) 0.8081(3) 0.0477(15) Uani 1 1 d . . .
H39 H 1.0441 0.3855 0.8469 0.057 Uiso 1 1 calc R . .
C40 C 0.9298(5) 0.2686(5) 0.7925(3) 0.0544(18) Uani 1 1 d . . .
H40 H 0.9543 0.2195 0.8215 0.065 Uiso 1 1 calc R . .
C41 C 0.8408(5) 0.2414(4) 0.7346(3) 0.0472(15) Uani 1 1 d . . .
H41 H 0.8067 0.1741 0.7242 0.057 Uiso 1 1 calc R . .
C42 C 0.8020(4) 0.3150(3) 0.6917(3) 0.0306(11) Uani 1 1 d . . .
H42 H 0.7412 0.2975 0.6529 0.037 Uiso 1 1 calc R . .
C43 C 0.7770(4) 0.4640(3) 0.5624(2) 0.0203(9) Uani 1 1 d . . .
C44 C 0.8718(4) 0.4162(3) 0.5349(3) 0.0283(10) Uani 1 1 d . . .
H44 H 0.9404 0.4065 0.5656 0.034 Uiso 1 1 calc R . .
C45 C 0.8632(5) 0.3833(4) 0.4614(3) 0.0361(12) Uani 1 1 d . . .
H45 H 0.9256 0.3504 0.4429 0.043 Uiso 1 1 calc R . .
C46 C 0.7616(5) 0.3993(4) 0.4153(3) 0.0412(13) Uani 1 1 d . . .
H46 H 0.7572 0.3787 0.3658 0.049 Uiso 1 1 calc R . .
C47 C 0.6681(5) 0.4455(4) 0.4428(3) 0.0387(12) Uani 1 1 d . . .
H47 H 0.5994 0.4547 0.4120 0.046 Uiso 1 1 calc R . .
C48 C 0.6750(4) 0.4785(4) 0.5162(2) 0.0314(11) Uani 1 1 d . . .
H48 H 0.6116 0.5104 0.5344 0.038 Uiso 1 1 calc R . .
C49 C 0.5378(5) 0.2929(4) 0.7815(3) 0.0365(12) Uani 1 1 d . . .
H49A H 0.5407 0.3168 0.7336 0.044 Uiso 1 1 calc R . .
H49B H 0.5731 0.2296 0.7815 0.044 Uiso 1 1 calc R . .
C50 C 0.6080(4) 0.3707(3) 0.8389(3) 0.0295(10) Uani 1 1 d . . .
H50A H 0.6691 0.4149 0.8180 0.035 Uiso 1 1 calc R . .
H50B H 0.6490 0.3383 0.8776 0.035 Uiso 1 1 calc R . .
C51 C 0.5068(4) 0.4298(4) 0.8674(3) 0.0325(11) Uani 1 1 d . . .
H51A H 0.5026 0.4248 0.9191 0.039 Uiso 1 1 calc R . .
H51B H 0.5217 0.5006 0.8589 0.039 Uiso 1 1 calc R . .
C52 C 0.3889(5) 0.3783(4) 0.8235(3) 0.0425(13) Uani 1 1 d . . .
H52A H 0.3206 0.3751 0.8535 0.051 Uiso 1 1 calc R . .
H52B H 0.3683 0.4151 0.7821 0.051 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
U1 S3 2.8047(10) . ?
U1 S7 2.8078(10) . ?
U1 S2 2.8186(10) . ?
U1 S5 2.8449(10) . ?
U1 S6 2.8558(10) . ?
U1 S1 2.8719(10) . ?
U1 S8 2.8742(10) . ?
U1 S4 2.8775(10) . ?
S1 P1 2.0109(15) . ?
S2 P1 2.0245(14) . ?
S3 P2 2.0152(15) . ?
S4 P2 2.0089(15) . ?
S5 P3 2.0184(15) . ?
S6 P3 2.0063(15) . ?
S7 P4 2.0137(15) . ?
S8 P4 2.0131(14) . ?
P1 C7 1.810(4) . ?
P1 C1 1.818(4) . ?
P2 C13 1.809(4) . ?
P2 C19 1.816(4) . ?
P3 C25 1.808(4) . ?
P3 C31 1.821(4) . ?
P4 C43 1.810(4) . ?
P4 C37 1.817(4) . ?
O1 C52 1.424(6) . ?
O1 C49 1.429(6) . ?
C1 C2 1.391(6) . ?
C1 C6 1.392(6) . ?
C2 C3 1.384(6) . ?
C3 C4 1.385(6) . ?
C4 C5 1.391(6) . ?
C5 C6 1.399(6) . ?
C7 C8 1.384(6) . ?
C7 C12 1.399(6) . ?
C8 C9 1.395(6) . ?
C9 C10 1.389(6) . ?
C10 C11 1.393(6) . ?
C11 C12 1.392(6) . ?
C13 C14 1.389(6) . ?
C13 C18 1.392(6) . ?
C14 C15 1.380(6) . ?
C15 C16 1.378(6) . ?
C16 C17 1.369(7) . ?
C17 C18 1.397(6) . ?
C19 C20 1.392(7) . ?
C19 C24 1.402(6) . ?
C20 C21 1.393(7) . ?
C21 C22 1.370(7) . ?
C22 C23 1.385(7) . ?
C23 C24 1.391(6) . ?
C25 C30 1.390(6) . ?
C25 C26 1.394(6) . ?
C26 C27 1.382(6) . ?
C27 C28 1.379(7) . ?
C28 C29 1.387(6) . ?
C29 C30 1.387(6) . ?
C31 C36 1.383(6) . ?
C31 C32 1.386(6) . ?
C32 C33 1.390(6) . ?
C33 C34 1.380(7) . ?
C34 C35 1.372(7) . ?
C35 C36 1.399(6) . ?
C37 C38 1.393(6) . ?
C37 C42 1.395(6) . ?
C38 C39 1.376(7) . ?
C39 C40 1.387(9) . ?
C40 C41 1.378(9) . ?
C41 C42 1.397(7) . ?
C43 C48 1.389(6) . ?
C43 C44 1.393(6) . ?
C44 C45 1.385(6) . ?
C45 C46 1.390(7) . ?
C46 C47 1.370(7) . ?
C47 C48 1.385(6) . ?
C49 C50 1.512(7) . ?
C50 C51 1.539(6) . ?
C51 C52 1.522(7) . ?

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
S3 U1 S7 94.91(3) . . ?
S3 U1 S2 90.76(3) . . ?
S7 U1 S2 151.58(3) . . ?
S3 U1 S5 150.91(3) . . ?
S7 U1 S5 92.14(3) . . ?
S2 U1 S5 96.32(3) . . ?
S3 U1 S6 138.68(3) . . ?
S7 U1 S6 77.34(3) . . ?
S2 U1 S6 80.06(3) . . ?
S5 U1 S6 70.40(3) . . ?
S3 U1 S1 76.89(3) . . ?
S7 U1 S1 137.75(3) . . ?
S2 U1 S1 70.63(3) . . ?
S5 U1 S1 78.95(3) . . ?
S6 U1 S1 134.52(3) . . ?
S3 U1 S8 78.00(3) . . ?
S7 U1 S8 70.63(3) . . ?
S2 U1 S8 137.70(3) . . ?
S5 U1 S8 77.84(3) . . ?
S6 U1 S8 133.44(3) . . ?
S1 U1 S8 67.12(3) . . ?
S3 U1 S4 70.63(3) . . ?
S7 U1 S4 77.83(3) . . ?
S2 U1 S4 77.88(3) . . ?
S5 U1 S4 138.44(3) . . ?
S6 U1 S4 68.05(3) . . ?
S1 U1 S4 133.90(3) . . ?
S8 U1 S4 132.84(3) . . ?
P1 S1 U1 89.26(4) . . ?
P1 S2 U1 90.50(5) . . ?
P2 S3 U1 90.42(5) . . ?
P2 S4 U1 88.49(5) . . ?
P3 S5 U1 89.99(5) . . ?
P3 S6 U1 89.92(5) . . ?
P4 S7 U1 90.84(5) . . ?
P4 S8 U1 88.96(5) . . ?
C7 P1 C1 105.61(18) . . ?
C7 P1 S1 110.98(14) . . ?
C1 P1 S1 110.83(14) . . ?
C7 P1 S2 110.73(14) . . ?
C1 P1 S2 109.42(14) . . ?
S1 P1 S2 109.23(6) . . ?
C13 P2 C19 106.27(19) . . ?
C13 P2 S4 108.66(14) . . ?
C19 P2 S4 111.58(15) . . ?
C13 P2 S3 110.50(14) . . ?
C19 P2 S3 110.32(15) . . ?
S4 P2 S3 109.46(6) . . ?
C25 P3 C31 102.86(18) . . ?
C25 P3 S6 112.07(14) . . ?
C31 P3 S6 109.99(14) . . ?
C25 P3 S5 110.57(14) . . ?
C31 P3 S5 111.75(14) . . ?
S6 P3 S5 109.47(6) . . ?
C43 P4 C37 106.23(19) . . ?
C43 P4 S8 110.85(14) . . ?
C37 P4 S8 109.79(14) . . ?
C43 P4 S7 110.36(14) . . ?
C37 P4 S7 110.24(16) . . ?
S8 P4 S7 109.33(6) . . ?
C52 O1 C49 104.2(4) . . ?
C2 C1 C6 120.3(4) . . ?
C2 C1 P1 118.2(3) . . ?
C6 C1 P1 121.3(3) . . ?
C3 C2 C1 119.6(4) . . ?
C2 C3 C4 120.6(4) . . ?
C3 C4 C5 120.3(4) . . ?
C4 C5 C6 119.3(4) . . ?
C1 C6 C5 119.9(4) . . ?
C8 C7 C12 120.2(4) . . ?
C8 C7 P1 119.0(3) . . ?
C12 C7 P1 120.8(3) . . ?
C7 C8 C9 119.8(4) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C10 C11 119.9(4) . . ?
C12 C11 C10 120.0(4) . . ?
C11 C12 C7 119.8(4) . . ?
C14 C13 C18 118.7(4) . . ?
C14 C13 P2 119.0(3) . . ?
C18 C13 P2 122.1(3) . . ?
C15 C14 C13 120.9(4) . . ?
C16 C15 C14 119.8(4) . . ?
C17 C16 C15 120.6(4) . . ?
C16 C17 C18 119.9(4) . . ?
C13 C18 C17 120.1(4) . . ?
C20 C19 C24 119.3(4) . . ?
C20 C19 P2 120.1(3) . . ?
C24 C19 P2 120.6(3) . . ?
C19 C20 C21 120.1(5) . . ?
C22 C21 C20 120.5(5) . . ?
C21 C22 C23 119.9(4) . . ?
C22 C23 C24 120.7(5) . . ?
C23 C24 C19 119.5(5) . . ?
C30 C25 C26 119.3(4) . . ?
C30 C25 P3 117.6(3) . . ?
C26 C25 P3 123.1(3) . . ?
C27 C26 C25 120.0(4) . . ?
C28 C27 C26 120.3(4) . . ?
C27 C28 C29 120.4(4) . . ?
C30 C29 C28 119.4(4) . . ?
C29 C30 C25 120.6(4) . . ?
C36 C31 C32 120.1(4) . . ?
C36 C31 P3 121.1(3) . . ?
C32 C31 P3 118.7(3) . . ?
C31 C32 C33 120.2(4) . . ?
C34 C33 C32 119.5(4) . . ?
C35 C34 C33 120.6(4) . . ?
C34 C35 C36 120.3(4) . . ?
C31 C36 C35 119.3(4) . . ?
C38 C37 C42 120.3(4) . . ?
C38 C37 P4 120.6(4) . . ?
C42 C37 P4 118.8(3) . . ?
C39 C38 C37 120.0(5) . . ?
C38 C39 C40 119.8(5) . . ?
C41 C40 C39 120.8(5) . . ?
C40 C41 C42 119.9(6) . . ?
C37 C42 C41 119.2(5) . . ?
C48 C43 C44 119.9(4) . . ?
C48 C43 P4 121.2(3) . . ?
C44 C43 P4 118.8(3) . . ?
C45 C44 C43 119.5(4) . . ?
C44 C45 C46 120.3(5) . . ?
C47 C46 C45 119.9(4) . . ?
C46 C47 C48 120.5(5) . . ?
C47 C48 C43 119.8(4) . . ?
O1 C49 C50 106.4(4) . . ?
C49 C50 C51 103.4(4) . . ?
C52 C51 C50 103.8(4) . . ?
O1 C52 C51 106.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.587
_refine_diff_density_min         -1.760
_refine_diff_density_rms         0.146
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx1036
_database_code_depnum_ccdc_archive 'CCDC 1404548'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H48 N2 P3 Pu S6'
_chemical_formula_weight         1237.29

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'
P P 0.1023 0.0942 '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'
Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.770(2)
_cell_length_b                   14.808(3)
_cell_length_c                   16.972(3)
_cell_angle_alpha                79.148(2)
_cell_angle_beta                 70.433(2)
_cell_angle_gamma                69.036(2)
_cell_volume                     2594.8(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1230
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7565
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29476
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.83
_reflns_number_total             11790
_reflns_number_gt                9195
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0131P)²+0.0000P] 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_number_reflns         11790
_refine_ls_number_parameters     575
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.002
_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
Pu1 Pu 0.911705(16) 0.671305(12) 0.745461(10) 0.01575(5) Uani 1 1 d . . .
P1 P 0.76670(12) 0.92663(8) 0.73193(7) 0.0226(3) Uani 1 1 d . . .
P2 P 1.24439(11) 0.59168(8) 0.70084(7) 0.0196(3) Uani 1 1 d . . .
P3 P 0.80113(11) 0.46811(8) 0.79283(7) 0.0191(3) Uani 1 1 d . . .
S1 S 0.95268(11) 0.86068(8) 0.71623(7) 0.0270(3) Uani 1 1 d . . .
S2 S 0.67184(11) 0.83163(8) 0.76194(7) 0.0252(3) Uani 1 1 d . . .
S3 S 1.12448(11) 0.63312(8) 0.81259(7) 0.0232(3) Uani 1 1 d . . .
S4 S 1.15514(11) 0.61417(9) 0.61405(7) 0.0230(3) Uani 1 1 d . . .
S5 S 0.98518(11) 0.45722(8) 0.76344(7) 0.0239(3) Uani 1 1 d . . .
S6 S 0.69110(10) 0.60622(8) 0.79380(7) 0.0216(3) Uani 1 1 d . . .
N1 N 0.8854(3) 0.6874(3) 0.5954(2) 0.0198(8) Uani 1 1 d . . .
N2 N 0.8398(3) 0.6843(3) 0.9070(2) 0.0225(9) Uani 1 1 d . . .
C1 C 0.7001(5) 1.0124(3) 0.8125(3) 0.0311(12) Uani 1 1 d . . .
C2 C 0.5778(6) 1.0251(4) 0.8645(3) 0.0531(16) Uani 1 1 d . . .
H2 H 0.5294 0.9907 0.8582 0.064 Uiso 1 1 calc R . .
C3 C 0.5273(7) 1.0903(5) 0.9267(4) 0.066(2) Uani 1 1 d . . .
H3 H 0.4455 1.0982 0.9627 0.079 Uiso 1 1 calc R . .
C4 C 0.5957(8) 1.1416(4) 0.9351(4) 0.061(2) Uani 1 1 d . . .
H4 H 0.5606 1.1849 0.9766 0.073 Uiso 1 1 calc R . .
C5 C 0.7139(7) 1.1311(4) 0.8845(4) 0.065(2) Uani 1 1 d . . .
H5 H 0.7602 1.1675 0.8905 0.078 Uiso 1 1 calc R . .
C6 C 0.7675(7) 1.0652(4) 0.8224(3) 0.0579(18) Uani 1 1 d . . .
H6 H 0.8499 1.0575 0.7877 0.069 Uiso 1 1 calc R . .
C7 C 0.7430(4) 1.0001(3) 0.6362(3) 0.0229(10) Uani 1 1 d . . .
C8 C 0.8364(5) 1.0367(3) 0.5814(3) 0.0263(11) Uani 1 1 d . . .
H8 H 0.9117 1.0249 0.5940 0.032 Uiso 1 1 calc R . .
C9 C 0.8184(5) 1.0903(3) 0.5083(3) 0.0346(13) Uani 1 1 d . . .
H9 H 0.8816 1.1148 0.4720 0.041 Uiso 1 1 calc R . .
C10 C 0.7085(6) 1.1078(4) 0.4888(3) 0.0404(14) Uani 1 1 d . . .
H10 H 0.6975 1.1435 0.4391 0.049 Uiso 1 1 calc R . .
C11 C 0.6133(5) 1.0725(4) 0.5429(3) 0.0422(14) Uani 1 1 d . . .
H11 H 0.5380 1.0849 0.5300 0.051 Uiso 1 1 calc R . .
C12 C 0.6314(5) 1.0185(3) 0.6167(3) 0.0354(13) Uani 1 1 d . . .
H12 H 0.5679 0.9946 0.6532 0.043 Uiso 1 1 calc R . .
C13 C 1.3624(4) 0.6542(3) 0.6652(3) 0.0217(10) Uani 1 1 d . . .
C14 C 1.3685(4) 0.7136(3) 0.7159(3) 0.0292(12) Uani 1 1 d . . .
H14 H 1.3111 0.7228 0.7692 0.035 Uiso 1 1 calc R . .
C15 C 1.4606(5) 0.7598(4) 0.6872(3) 0.0368(13) Uani 1 1 d . . .
H15 H 1.4637 0.8006 0.7213 0.044 Uiso 1 1 calc R . .
C16 C 1.5473(4) 0.7458(3) 0.6088(3) 0.0321(12) Uani 1 1 d . . .
H16 H 1.6099 0.7757 0.5905 0.038 Uiso 1 1 calc R . .
C17 C 1.5403(4) 0.6874(3) 0.5582(3) 0.0311(12) Uani 1 1 d . . .
H17 H 1.5980 0.6781 0.5050 0.037 Uiso 1 1 calc R . .
C18 C 1.4482(4) 0.6419(3) 0.5856(3) 0.0257(11) Uani 1 1 d . . .
H18 H 1.4437 0.6029 0.5505 0.031 Uiso 1 1 calc R . .
C19 C 1.3379(4) 0.4656(3) 0.7125(3) 0.0240(11) Uani 1 1 d . . .
C20 C 1.4065(4) 0.4371(3) 0.7714(3) 0.0296(12) Uani 1 1 d . . .
H20 H 1.4046 0.4827 0.8031 0.036 Uiso 1 1 calc R . .
C21 C 1.4770(5) 0.3404(4) 0.7820(3) 0.0359(13) Uani 1 1 d . . .
H21 H 1.5221 0.3213 0.8213 0.043 Uiso 1 1 calc R . .
C22 C 1.4809(5) 0.2724(4) 0.7348(3) 0.0395(14) Uani 1 1 d . . .
H22 H 1.5287 0.2077 0.7421 0.047 Uiso 1 1 calc R . .
C23 C 1.4141(5) 0.3005(4) 0.6770(3) 0.0428(14) Uani 1 1 d . . .
H23 H 1.4171 0.2545 0.6451 0.051 Uiso 1 1 calc R . .
C24 C 1.3414(5) 0.3971(3) 0.6656(3) 0.0339(12) Uani 1 1 d . . .
H24 H 1.2957 0.4153 0.6267 0.041 Uiso 1 1 calc R . .
C25 C 0.7776(4) 0.4068(3) 0.7198(3) 0.0186(10) Uani 1 1 d . . .
C26 C 0.8333(4) 0.3072(3) 0.7164(3) 0.0276(11) Uani 1 1 d . . .
H26 H 0.8804 0.2723 0.7530 0.033 Uiso 1 1 calc R . .
C27 C 0.8202(5) 0.2596(3) 0.6600(3) 0.0323(12) Uani 1 1 d . . .
H27 H 0.8562 0.1926 0.6595 0.039 Uiso 1 1 calc R . .
C28 C 0.7536(4) 0.3110(4) 0.6040(3) 0.0298(12) Uani 1 1 d . . .
H28 H 0.7461 0.2788 0.5649 0.036 Uiso 1 1 calc R . .
C29 C 0.6983(5) 0.4097(3) 0.6060(3) 0.0297(12) Uani 1 1 d . . .
H29 H 0.6542 0.4445 0.5677 0.036 Uiso 1 1 calc R . .
C30 C 0.7081(4) 0.4572(3) 0.6648(3) 0.0249(11) Uani 1 1 d . . .
H30 H 0.6677 0.5237 0.6674 0.030 Uiso 1 1 calc R . .
C31 C 0.7484(4) 0.4047(3) 0.8939(3) 0.0235(11) Uani 1 1 d . . .
C32 C 0.8308(5) 0.3518(3) 0.9405(3) 0.0313(12) Uani 1 1 d . . .
H32 H 0.9164 0.3471 0.9202 0.038 Uiso 1 1 calc R . .
C33 C 0.7848(6) 0.3058(4) 1.0180(3) 0.0420(14) Uani 1 1 d . . .
H33 H 0.8398 0.2699 1.0494 0.050 Uiso 1 1 calc R . .
C34 C 0.6591(6) 0.3136(4) 1.0478(3) 0.0436(15) Uani 1 1 d . . .
H34 H 0.6293 0.2825 1.0997 0.052 Uiso 1 1 calc R . .
C35 C 0.5755(5) 0.3663(3) 1.0028(3) 0.0360(13) Uani 1 1 d . . .
H35 H 0.4898 0.3717 1.0241 0.043 Uiso 1 1 calc R . .
C36 C 0.6216(5) 0.4114(3) 0.9248(3) 0.0275(11) Uani 1 1 d . . .
H36 H 0.5663 0.4464 0.8933 0.033 Uiso 1 1 calc R . .
C37 C 0.8850(4) 0.6105(3) 0.5642(3) 0.0249(11) Uani 1 1 d . . .
H37 H 0.8902 0.5528 0.5981 0.030 Uiso 1 1 calc R . .
C38 C 0.8774(4) 0.6130(3) 0.4849(3) 0.0273(11) Uani 1 1 d . . .
H38 H 0.8767 0.5583 0.4659 0.033 Uiso 1 1 calc R . .
C39 C 0.8708(4) 0.6976(4) 0.4336(3) 0.0338(13) Uani 1 1 d . . .
H39 H 0.8661 0.7009 0.3794 0.041 Uiso 1 1 calc R . .
C40 C 0.8714(5) 0.7771(4) 0.4644(3) 0.0328(12) Uani 1 1 d . . .
H40 H 0.8668 0.8352 0.4312 0.039 Uiso 1 1 calc R . .
C41 C 0.8788(4) 0.7701(3) 0.5445(3) 0.0255(11) Uani 1 1 d . . .
H41 H 0.8794 0.8242 0.5645 0.031 Uiso 1 1 calc R . .
C42 C 0.8259(5) 0.7634(3) 0.9415(3) 0.0309(12) Uani 1 1 d . . .
H42 H 0.8254 0.8205 0.9073 0.037 Uiso 1 1 calc R . .
C43 C 0.8124(5) 0.7638(4) 1.0252(3) 0.0457(15) Uani 1 1 d . . .
H43 H 0.8027 0.8203 1.0468 0.055 Uiso 1 1 calc R . .
C44 C 0.8133(5) 0.6818(4) 1.0757(3) 0.0448(15) Uani 1 1 d . . .
H44 H 0.8021 0.6812 1.1327 0.054 Uiso 1 1 calc R . .
C45 C 0.8310(6) 0.6002(4) 1.0419(3) 0.0492(16) Uani 1 1 d . . .
H45 H 0.8353 0.5423 1.0752 0.059 Uiso 1 1 calc R . .
C46 C 0.8425(5) 0.6033(4) 0.9588(3) 0.0367(13) Uani 1 1 d . . .
H46 H 0.8527 0.5469 0.9370 0.044 Uiso 1 1 calc R . .
C47 C 0.0978(6) 0.0067(4) 0.8389(4) 0.096(3) Uani 1 1 d GU . .
C48 C 0.1857(7) -0.0373(3) 0.7676(5) 0.151(5) Uani 1 1 d GU . .
H48 H 0.1964 -0.1009 0.7607 0.182 Uiso 1 1 calc R . .
C49 C 0.2574(5) 0.0139(5) 0.7068(4) 0.126(4) Uani 1 1 d GU . .
H49 H 0.3162 -0.0156 0.6591 0.151 Uiso 1 1 calc R . .
C50 C 0.2414(6) 0.1090(5) 0.7172(4) 0.115(3) Uani 1 1 d GU . .
H50 H 0.2894 0.1432 0.6765 0.138 Uiso 1 1 calc R . .
C51 C 0.1536(7) 0.1530(3) 0.7884(4) 0.118(4) Uani 1 1 d GU . .
H51 H 0.1429 0.2166 0.7954 0.141 Uiso 1 1 calc R . .
C52 C 0.0818(6) 0.1019(5) 0.8493(3) 0.127(4) Uani 1 1 d GU . .
H52 H 0.0230 0.1313 0.8969 0.153 Uiso 1 1 calc R . .
C53 C 0.0242(10) -0.0524(6) 0.9046(5) 0.134(4) Uani 1 1 d U . .
H53A H -0.0017 -0.0899 0.8776 0.201 Uiso 1 1 calc R . .
H53B H -0.0496 -0.0097 0.9403 0.201 Uiso 1 1 calc R . .
H53C H 0.0773 -0.0952 0.9376 0.201 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
Pu1 N2 2.608(3) . ?
Pu1 N1 2.624(3) . ?
Pu1 S6 2.9000(12) . ?
Pu1 S3 2.9232(12) . ?
Pu1 S4 2.9317(12) . ?
Pu1 S2 2.9343(12) . ?
Pu1 S1 2.9370(13) . ?
Pu1 S5 2.9567(13) . ?
P1 C1 1.822(5) . ?
P1 C7 1.823(4) . ?
P1 S2 1.9895(17) . ?
P1 S1 1.9985(18) . ?
P2 C19 1.809(4) . ?
P2 C13 1.816(4) . ?
P2 S4 1.9965(16) . ?
P2 S3 1.9978(17) . ?
P3 C25 1.808(4) . ?
P3 C31 1.818(4) . ?
P3 S6 1.9908(16) . ?
P3 S5 2.0060(17) . ?
N1 C37 1.345(5) . ?
N1 C41 1.353(5) . ?
N2 C42 1.341(5) . ?
N2 C46 1.343(5) . ?
C1 C6 1.362(7) . ?
C1 C2 1.380(7) . ?
C2 C3 1.398(7) . ?
C3 C4 1.341(9) . ?
C4 C5 1.339(8) . ?
C5 C6 1.400(8) . ?
C7 C8 1.385(6) . ?
C7 C12 1.382(6) . ?
C8 C9 1.378(6) . ?
C9 C10 1.366(7) . ?
C10 C11 1.386(7) . ?
C11 C12 1.390(6) . ?
C13 C14 1.374(6) . ?
C13 C18 1.387(6) . ?
C14 C15 1.390(6) . ?
C15 C16 1.377(6) . ?
C16 C17 1.367(6) . ?
C17 C18 1.383(6) . ?
C19 C24 1.384(6) . ?
C19 C20 1.402(6) . ?
C20 C21 1.387(6) . ?
C21 C22 1.381(7) . ?
C22 C23 1.372(7) . ?
C23 C24 1.395(6) . ?
C25 C30 1.382(5) . ?
C25 C26 1.386(6) . ?
C26 C27 1.366(6) . ?
C27 C28 1.378(6) . ?
C28 C29 1.372(6) . ?
C29 C30 1.381(6) . ?
C31 C36 1.379(6) . ?
C31 C32 1.385(6) . ?
C32 C33 1.391(6) . ?
C33 C34 1.362(7) . ?
C34 C35 1.374(7) . ?
C35 C36 1.393(6) . ?
C37 C38 1.372(6) . ?
C38 C39 1.377(6) . ?
C39 C40 1.379(6) . ?
C40 C41 1.373(6) . ?
C42 C43 1.377(6) . ?
C43 C44 1.347(7) . ?
C44 C45 1.354(7) . ?
C45 C46 1.365(6) . ?
C47 C48 1.3900 . ?
C47 C52 1.3900 . ?
C47 C53 1.513(8) . ?
C48 C49 1.3900 . ?
C49 C50 1.3900 . ?
C50 C51 1.3900 . ?
C51 C52 1.3900 . ?

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
N2 Pu1 N1 157.04(11) . . ?
N2 Pu1 S6 80.18(8) . . ?
N1 Pu1 S6 82.46(8) . . ?
N2 Pu1 S3 67.10(8) . . ?
N1 Pu1 S3 135.46(8) . . ?
S6 Pu1 S3 134.65(3) . . ?
N2 Pu1 S4 136.05(8) . . ?
N1 Pu1 S4 66.87(8) . . ?
S6 Pu1 S4 131.69(3) . . ?
S3 Pu1 S4 69.13(3) . . ?
N2 Pu1 S2 80.50(8) . . ?
N1 Pu1 S2 78.94(8) . . ?
S6 Pu1 S2 66.91(3) . . ?
S3 Pu1 S2 132.18(3) . . ?
S4 Pu1 S2 135.14(3) . . ?
N2 Pu1 S1 90.24(8) . . ?
N1 Pu1 S1 91.59(8) . . ?
S6 Pu1 S1 135.23(3) . . ?
S3 Pu1 S1 77.25(3) . . ?
S4 Pu1 S1 83.94(3) . . ?
S2 Pu1 S1 68.39(3) . . ?
N2 Pu1 S5 93.00(8) . . ?
N1 Pu1 S5 94.52(8) . . ?
S6 Pu1 S5 68.56(3) . . ?
S3 Pu1 S5 82.26(3) . . ?
S4 Pu1 S5 77.36(3) . . ?
S2 Pu1 S5 135.46(3) . . ?
S1 Pu1 S5 156.13(3) . . ?
C1 P1 C7 105.1(2) . . ?
C1 P1 S2 109.54(18) . . ?
C7 P1 S2 110.07(16) . . ?
C1 P1 S1 110.84(18) . . ?
C7 P1 S1 109.46(16) . . ?
S2 P1 S1 111.66(7) . . ?
C19 P2 C13 103.5(2) . . ?
C19 P2 S4 111.40(16) . . ?
C13 P2 S4 109.48(14) . . ?
C19 P2 S3 109.02(15) . . ?
C13 P2 S3 110.55(16) . . ?
S4 P2 S3 112.53(7) . . ?
C25 P3 C31 103.7(2) . . ?
C25 P3 S6 110.22(15) . . ?
C31 P3 S6 109.34(16) . . ?
C25 P3 S5 110.22(15) . . ?
C31 P3 S5 111.83(16) . . ?
S6 P3 S5 111.26(7) . . ?
P1 S1 Pu1 89.80(5) . . ?
P1 S2 Pu1 90.05(6) . . ?
P2 S3 Pu1 89.05(5) . . ?
P2 S4 Pu1 88.83(5) . . ?
P3 S5 Pu1 89.12(5) . . ?
P3 S6 Pu1 91.05(5) . . ?
C37 N1 C41 117.1(4) . . ?
C37 N1 Pu1 120.4(3) . . ?
C41 N1 Pu1 122.4(3) . . ?
C42 N2 C46 116.1(4) . . ?
C42 N2 Pu1 123.1(3) . . ?
C46 N2 Pu1 119.2(3) . . ?
C6 C1 C2 118.8(5) . . ?
C6 C1 P1 121.7(4) . . ?
C2 C1 P1 119.5(4) . . ?
C1 C2 C3 119.4(6) . . ?
C4 C3 C2 120.6(7) . . ?
C3 C4 C5 120.9(6) . . ?
C4 C5 C6 119.7(6) . . ?
C1 C6 C5 120.7(6) . . ?
C8 C7 C12 119.0(4) . . ?
C8 C7 P1 121.0(3) . . ?
C12 C7 P1 120.0(4) . . ?
C9 C8 C7 120.5(5) . . ?
C10 C9 C8 120.4(5) . . ?
C9 C10 C11 120.2(5) . . ?
C10 C11 C12 119.3(5) . . ?
C7 C12 C11 120.6(5) . . ?
C14 C13 C18 119.2(4) . . ?
C14 C13 P2 121.1(4) . . ?
C18 C13 P2 119.7(3) . . ?
C13 C14 C15 119.8(5) . . ?
C16 C15 C14 120.8(5) . . ?
C17 C16 C15 119.3(5) . . ?
C16 C17 C18 120.5(5) . . ?
C17 C18 C13 120.4(5) . . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 P2 121.5(4) . . ?
C20 C19 P2 118.8(4) . . ?
C21 C20 C19 119.5(5) . . ?
C22 C21 C20 120.6(5) . . ?
C23 C22 C21 119.7(5) . . ?
C22 C23 C24 120.8(5) . . ?
C19 C24 C23 119.6(5) . . ?
C30 C25 C26 118.5(4) . . ?
C30 C25 P3 121.6(3) . . ?
C26 C25 P3 119.9(3) . . ?
C27 C26 C25 121.0(4) . . ?
C26 C27 C28 119.9(5) . . ?
C29 C28 C27 120.0(5) . . ?
C28 C29 C30 120.0(4) . . ?
C29 C30 C25 120.5(4) . . ?
C36 C31 C32 119.6(4) . . ?
C36 C31 P3 118.2(3) . . ?
C32 C31 P3 122.1(4) . . ?
C31 C32 C33 119.7(5) . . ?
C34 C33 C32 120.0(5) . . ?
C33 C34 C35 121.3(5) . . ?
C34 C35 C36 118.8(5) . . ?
C31 C36 C35 120.5(5) . . ?
N1 C37 C38 123.2(4) . . ?
C37 C38 C39 119.2(5) . . ?
C38 C39 C40 118.4(4) . . ?
C41 C40 C39 119.6(4) . . ?
N1 C41 C40 122.5(4) . . ?
N2 C42 C43 122.8(5) . . ?
C44 C43 C42 119.6(5) . . ?
C43 C44 C45 118.7(5) . . ?
C44 C45 C46 119.9(5) . . ?
N2 C46 C45 122.9(5) . . ?
C48 C47 C52 120.0 . . ?
C48 C47 C53 118.3(6) . . ?
C52 C47 C53 121.7(6) . . ?
C47 C48 C49 120.0 . . ?
C48 C49 C50 120.0 . . ?
C51 C50 C49 120.0 . . ?
C50 C51 C52 120.0 . . ?
C51 C52 C47 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.132
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx1863
_database_code_depnum_ccdc_archive 'CCDC 1404549'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H28 P2 S2'
_chemical_formula_weight         586.64

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   11.616(4)
_cell_length_b                   16.103(5)
_cell_length_c                   16.319(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.164(4)
_cell_angle_gamma                90.00
_cell_volume                     2883.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28472
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.84
_reflns_number_total             5494
_reflns_number_gt                4194
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0334P)²+0.0000P] 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_number_reflns         5494
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_refine_ls_shift/su_max          0.000
_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
P1 P 0.27571(5) 0.03398(3) 0.05233(4) 0.01441(14) Uani 1 1 d . . .
P2 P 0.78601(5) 0.59744(3) 0.03859(3) 0.01360(14) Uani 1 1 d . . .
S1 S 0.30754(5) -0.08138(3) 0.09487(4) 0.02150(15) Uani 1 1 d . . .
S2 S 0.20335(5) 0.05289(4) -0.07402(4) 0.02056(15) Uani 1 1 d . . .
C1 C 0.1918(2) 0.09195(13) 0.11001(13) 0.0147(5) Uani 1 1 d . . .
C2 C 0.0737(2) 0.07906(14) 0.10934(13) 0.0188(5) Uani 1 1 d . . .
H2 H 0.0276 0.0356 0.0774 0.023 Uiso 1 1 calc R . .
C3 C 0.0246(2) 0.13160(14) 0.15672(14) 0.0236(6) Uani 1 1 d . . .
H3 H -0.0547 0.1234 0.1567 0.028 Uiso 1 1 calc R . .
C4 C 0.0941(2) 0.19653(14) 0.20426(14) 0.0237(6) Uani 1 1 d . . .
H4 H 0.0611 0.2315 0.2361 0.028 Uiso 1 1 calc R . .
C5 C 0.2115(2) 0.20955(13) 0.20457(14) 0.0215(5) Uani 1 1 d . . .
H5 H 0.2572 0.2531 0.2366 0.026 Uiso 1 1 calc R . .
C6 C 0.2619(2) 0.15774(13) 0.15716(13) 0.0167(5) Uani 1 1 d . . .
C7 C 0.3833(2) 0.16383(12) 0.14828(13) 0.0161(5) Uani 1 1 d . . .
C8 C 0.4700(2) 0.22503(14) 0.18255(14) 0.0226(5) Uani 1 1 d . . .
H8 H 0.4542 0.2675 0.2160 0.027 Uiso 1 1 calc R . .
C9 C 0.5795(2) 0.22257(14) 0.16675(14) 0.0258(6) Uani 1 1 d . . .
H9 H 0.6370 0.2640 0.1890 0.031 Uiso 1 1 calc R . .
C10 C 0.6046(2) 0.15896(14) 0.11808(15) 0.0248(6) Uani 1 1 d . . .
H10 H 0.6792 0.1575 0.1085 0.030 Uiso 1 1 calc R . .
C11 C 0.5193(2) 0.09783(14) 0.08378(14) 0.0195(5) Uani 1 1 d . . .
H11 H 0.5364 0.0548 0.0515 0.023 Uiso 1 1 calc R . .
C12 C 0.40806(19) 0.10080(12) 0.09758(13) 0.0148(5) Uani 1 1 d . . .
C13 C 0.80702(19) 0.49788(13) 0.09023(13) 0.0142(5) Uani 1 1 d . . .
C14 C 0.8119(2) 0.49239(13) 0.17658(14) 0.0182(5) Uani 1 1 d . . .
H14 H 0.8012 0.5397 0.2059 0.022 Uiso 1 1 calc R . .
C15 C 0.8325(2) 0.41672(13) 0.21853(14) 0.0209(5) Uani 1 1 d . . .
H15 H 0.8362 0.4130 0.2762 0.025 Uiso 1 1 calc R . .
C16 C 0.8477(2) 0.34637(13) 0.17440(14) 0.0208(5) Uani 1 1 d . . .
H16 H 0.8614 0.2953 0.2026 0.025 Uiso 1 1 calc R . .
C17 C 0.8425(2) 0.35146(13) 0.08884(15) 0.0221(5) Uani 1 1 d . . .
H17 H 0.8527 0.3039 0.0597 0.026 Uiso 1 1 calc R . .
C18 C 0.8222(2) 0.42700(13) 0.04636(14) 0.0179(5) Uani 1 1 d . . .
H18 H 0.8188 0.4304 -0.0113 0.021 Uiso 1 1 calc R . .
C19 C 0.7409(2) 0.58325(12) -0.07663(13) 0.0149(5) Uani 1 1 d . . .
C20 C 0.6191(2) 0.56876(13) -0.12339(14) 0.0217(5) Uani 1 1 d . . .
H20 H 0.5607 0.5710 -0.0958 0.026 Uiso 1 1 calc R . .
C21 C 0.5848(2) 0.55103(14) -0.21097(15) 0.0268(6) Uani 1 1 d . . .
H21 H 0.5036 0.5403 -0.2422 0.032 Uiso 1 1 calc R . .
C22 C 0.6715(2) 0.54924(13) -0.25214(15) 0.0259(6) Uani 1 1 d . . .
H22 H 0.6482 0.5374 -0.3111 0.031 Uiso 1 1 calc R . .
C23 C 0.7918(2) 0.56486(13) -0.20664(14) 0.0239(6) Uani 1 1 d . . .
H23 H 0.8493 0.5644 -0.2350 0.029 Uiso 1 1 calc R . .
C24 C 0.8277(2) 0.58136(13) -0.11842(14) 0.0194(5) Uani 1 1 d . . .
H24 H 0.9093 0.5911 -0.0874 0.023 Uiso 1 1 calc R . .
C25 C 0.92787(19) 0.65218(12) 0.07390(13) 0.0133(5) Uani 1 1 d . . .
C26 C 0.9397(2) 0.72957(13) 0.03815(13) 0.0170(5) Uani 1 1 d . . .
H26 H 0.8741 0.7526 -0.0052 0.020 Uiso 1 1 calc R . .
C27 C 1.0491(2) 0.77132(13) 0.06769(14) 0.0191(5) Uani 1 1 d . . .
H27 H 1.0567 0.8233 0.0451 0.023 Uiso 1 1 calc R . .
C28 C 1.1475(2) 0.73657(13) 0.13051(14) 0.0182(5) Uani 1 1 d . . .
H28 H 1.2212 0.7651 0.1497 0.022 Uiso 1 1 calc R . .
C29 C 1.1373(2) 0.65944(13) 0.16518(14) 0.0181(5) Uani 1 1 d . . .
H29 H 1.2042 0.6358 0.2069 0.022 Uiso 1 1 calc R . .
C30 C 1.02744(19) 0.61785(13) 0.13764(13) 0.0160(5) Uani 1 1 d . . .
H30 H 1.0199 0.5667 0.1618 0.019 Uiso 1 1 calc R . .
C31 C 0.66780(19) 0.65014(12) 0.06518(13) 0.0150(5) Uani 1 1 d . . .
C32 C 0.5741(2) 0.60406(14) 0.07829(14) 0.0222(5) Uani 1 1 d . . .
H32 H 0.5765 0.5464 0.0769 0.027 Uiso 1 1 calc R . .
C33 C 0.4775(2) 0.64357(14) 0.09343(15) 0.0261(6) Uani 1 1 d . . .
H33 H 0.4155 0.6125 0.1028 0.031 Uiso 1 1 calc R . .
C34 C 0.4732(2) 0.72937(14) 0.09463(14) 0.0243(6) Uani 1 1 d . . .
H34 H 0.4073 0.7561 0.1034 0.029 Uiso 1 1 calc R . .
C35 C 0.5664(2) 0.77522(14) 0.08285(13) 0.0211(5) Uani 1 1 d . . .
H35 H 0.5639 0.8329 0.0849 0.025 Uiso 1 1 calc R . .
C36 C 0.6637(2) 0.73641(13) 0.06801(13) 0.0177(5) Uani 1 1 d . . .
H36 H 0.7263 0.7678 0.0599 0.021 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
P1 C1 1.820(2) . ?
P1 C12 1.822(2) . ?
P1 S1 1.9751(10) . ?
P1 S2 1.9781(10) . ?
P2 C31 1.785(2) . ?
P2 C25 1.789(2) . ?
P2 C13 1.790(2) . ?
P2 C19 1.793(2) . ?
C1 C2 1.384(3) . ?
C1 C6 1.402(3) . ?
C2 C3 1.389(3) . ?
C3 C4 1.391(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.468(3) . ?
C7 C8 1.388(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.379(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.383(3) . ?
C13 C18 1.389(3) . ?
C13 C14 1.395(3) . ?
C14 C15 1.379(3) . ?
C15 C16 1.384(3) . ?
C16 C17 1.380(3) . ?
C17 C18 1.382(3) . ?
C19 C20 1.389(3) . ?
C19 C24 1.391(3) . ?
C20 C21 1.382(3) . ?
C21 C22 1.382(3) . ?
C22 C23 1.373(3) . ?
C23 C24 1.387(3) . ?
C25 C30 1.391(3) . ?
C25 C26 1.402(3) . ?
C26 C27 1.378(3) . ?
C27 C28 1.379(3) . ?
C28 C29 1.386(3) . ?
C29 C30 1.379(3) . ?
C31 C32 1.391(3) . ?
C31 C36 1.391(3) . ?
C32 C33 1.381(3) . ?
C33 C34 1.383(3) . ?
C34 C35 1.375(3) . ?
C35 C36 1.380(3) . ?

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
C1 P1 C12 90.65(10) . . ?
C1 P1 S1 111.77(7) . . ?
C12 P1 S1 112.16(7) . . ?
C1 P1 S2 110.11(7) . . ?
C12 P1 S2 110.17(7) . . ?
S1 P1 S2 118.53(4) . . ?
C31 P2 C25 112.84(10) . . ?
C31 P2 C13 107.96(10) . . ?
C25 P2 C13 108.71(10) . . ?
C31 P2 C19 109.39(10) . . ?
C25 P2 C19 108.78(10) . . ?
C13 P2 C19 109.10(10) . . ?
C2 C1 C6 120.9(2) . . ?
C2 C1 P1 128.10(17) . . ?
C6 C1 P1 111.00(16) . . ?
C1 C2 C3 119.4(2) . . ?
C2 C3 C4 119.9(2) . . ?
C5 C4 C3 120.6(2) . . ?
C4 C5 C6 120.2(2) . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 127.5(2) . . ?
C1 C6 C7 113.58(18) . . ?
C8 C7 C12 119.4(2) . . ?
C8 C7 C6 126.9(2) . . ?
C12 C7 C6 113.62(18) . . ?
C9 C8 C7 119.7(2) . . ?
C8 C9 C10 120.6(2) . . ?
C11 C10 C9 120.1(2) . . ?
C10 C11 C12 119.7(2) . . ?
C11 C12 C7 120.4(2) . . ?
C11 C12 P1 128.49(17) . . ?
C7 C12 P1 111.03(16) . . ?
C18 C13 C14 119.93(19) . . ?
C18 C13 P2 120.93(16) . . ?
C14 C13 P2 119.11(16) . . ?
C15 C14 C13 120.0(2) . . ?
C14 C15 C16 119.7(2) . . ?
C17 C16 C15 120.5(2) . . ?
C16 C17 C18 120.2(2) . . ?
C17 C18 C13 119.6(2) . . ?
C20 C19 C24 119.9(2) . . ?
C20 C19 P2 119.48(17) . . ?
C24 C19 P2 120.49(17) . . ?
C21 C20 C19 119.9(2) . . ?
C22 C21 C20 119.9(2) . . ?
C23 C22 C21 120.5(2) . . ?
C22 C23 C24 120.1(2) . . ?
C23 C24 C19 119.6(2) . . ?
C30 C25 C26 119.58(19) . . ?
C30 C25 P2 119.79(16) . . ?
C26 C25 P2 120.63(16) . . ?
C27 C26 C25 119.6(2) . . ?
C26 C27 C28 120.4(2) . . ?
C27 C28 C29 120.4(2) . . ?
C30 C29 C28 119.7(2) . . ?
C29 C30 C25 120.3(2) . . ?
C32 C31 C36 119.4(2) . . ?
C32 C31 P2 119.16(16) . . ?
C36 C31 P2 121.37(16) . . ?
C33 C32 C31 120.3(2) . . ?
C32 C33 C34 119.9(2) . . ?
C35 C34 C33 120.1(2) . . ?
C34 C35 C36 120.6(2) . . ?
C35 C36 C31 119.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.060
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx2033s
_database_code_depnum_ccdc_archive 'CCDC 1404550'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45.50 H47 As O0.50 P S2'
_chemical_formula_weight         771.84

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'
P P 0.1023 0.0942 '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'
As As 0.0499 2.0058 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5652(13)
_cell_length_b                   13.0602(14)
_cell_length_c                   14.2301(15)
_cell_angle_alpha                110.587(1)
_cell_angle_beta                 91.766(1)
_cell_angle_gamma                114.432(1)
_cell_volume                     1947.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8169
_exptl_absorpt_correction_T_max  0.8839
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22934
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         28.66
_reflns_number_total             9192
_reflns_number_gt                7779
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 134 27 acetone
_platon_squeeze_details          
;
;


_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)+(0.0036P)²+0.0000P] 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_number_reflns         9192
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_restrained_S_all      1.410
_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
As1 As 0.629914(15) 0.533565(15) 0.200254(13) 0.01293(5) Uani 1 1 d . . .
P1 P 0.91342(4) 0.21573(4) 0.18845(3) 0.01404(10) Uani 1 1 d . . .
S1 S 0.95910(4) 0.09056(4) 0.19653(4) 0.02206(11) Uani 1 1 d . . .
S2 S 1.03461(4) 0.39004(4) 0.24526(3) 0.02046(11) Uani 1 1 d . . .
C1 C 0.78006(14) 0.20601(14) 0.23898(13) 0.0134(4) Uani 1 1 d . . .
C2 C 0.76838(15) 0.23359(15) 0.33998(13) 0.0155(4) Uani 1 1 d . . .
H2 H 0.8323 0.2547 0.3896 0.019 Uiso 1 1 calc R . .
C3 C 0.66187(15) 0.23023(14) 0.36858(13) 0.0153(4) Uani 1 1 d . . .
C4 C 0.56924(15) 0.19921(15) 0.29074(13) 0.0169(4) Uani 1 1 d . . .
H4 H 0.4979 0.1976 0.3080 0.020 Uiso 1 1 calc R . .
C5 C 0.57948(15) 0.17083(15) 0.18936(13) 0.0156(4) Uani 1 1 d . . .
H5 H 0.5161 0.1509 0.1398 0.019 Uiso 1 1 calc R . .
C6 C 0.68529(14) 0.17222(14) 0.16194(13) 0.0128(4) Uani 1 1 d . . .
C7 C 0.71497(15) 0.14745(14) 0.05926(13) 0.0134(4) Uani 1 1 d . . .
C8 C 0.64045(15) 0.10869(14) -0.03326(13) 0.0153(4) Uani 1 1 d . . .
H8 H 0.5608 0.0925 -0.0355 0.018 Uiso 1 1 calc R . .
C9 C 0.68518(15) 0.09439(15) -0.12188(13) 0.0156(4) Uani 1 1 d . . .
H9 H 0.6339 0.0669 -0.1835 0.019 Uiso 1 1 calc R . .
C10 C 0.80538(15) 0.11978(14) -0.12250(13) 0.0137(4) Uani 1 1 d . . .
C11 C 0.87825(15) 0.15458(14) -0.02953(13) 0.0145(4) Uani 1 1 d . . .
H11 H 0.9573 0.1686 -0.0275 0.017 Uiso 1 1 calc R . .
C12 C 0.83385(14) 0.16835(14) 0.05966(12) 0.0126(4) Uani 1 1 d . . .
C13 C 0.64388(16) 0.25554(16) 0.47873(13) 0.0200(4) Uani 1 1 d . . .
C14 C 0.76102(17) 0.31586(17) 0.55578(14) 0.0277(5) Uani 1 1 d . . .
H14A H 0.7978 0.2621 0.5402 0.042 Uiso 1 1 calc R . .
H14B H 0.7454 0.3317 0.6238 0.042 Uiso 1 1 calc R . .
H14C H 0.8136 0.3918 0.5519 0.042 Uiso 1 1 calc R . .
C15 C 0.5631(2) 0.13317(18) 0.48401(15) 0.0446(6) Uani 1 1 d . . .
H15A H 0.4879 0.0952 0.4373 0.067 Uiso 1 1 calc R . .
H15B H 0.5498 0.1473 0.5525 0.067 Uiso 1 1 calc R . .
H15C H 0.6007 0.0802 0.4655 0.067 Uiso 1 1 calc R . .
C16 C 0.58463(19) 0.3410(2) 0.51075(15) 0.0398(6) Uani 1 1 d . . .
H16A H 0.6332 0.4163 0.5041 0.060 Uiso 1 1 calc R . .
H16B H 0.5767 0.3582 0.5808 0.060 Uiso 1 1 calc R . .
H16C H 0.5071 0.3019 0.4674 0.060 Uiso 1 1 calc R . .
C17 C 0.85007(15) 0.10907(16) -0.22274(13) 0.0163(4) Uani 1 1 d . . .
C18 C 0.80089(16) -0.02701(16) -0.29424(14) 0.0237(4) Uani 1 1 d . . .
H18A H 0.8258 -0.0339 -0.3583 0.036 Uiso 1 1 calc R . .
H18B H 0.7152 -0.0657 -0.3062 0.036 Uiso 1 1 calc R . .
H18C H 0.8309 -0.0666 -0.2629 0.036 Uiso 1 1 calc R . .
C19 C 0.98646(16) 0.16927(17) -0.20414(14) 0.0260(4) Uani 1 1 d . . .
H19A H 1.0181 0.2538 -0.1576 0.039 Uiso 1 1 calc R . .
H19B H 1.0112 0.1644 -0.2681 0.039 Uiso 1 1 calc R . .
H19C H 1.0157 0.1274 -0.1750 0.039 Uiso 1 1 calc R . .
C20 C 0.80785(18) 0.17295(18) -0.27665(14) 0.0272(5) Uani 1 1 d . . .
H20A H 0.8346 0.2571 -0.2311 0.041 Uiso 1 1 calc R . .
H20B H 0.7222 0.1323 -0.2953 0.041 Uiso 1 1 calc R . .
H20C H 0.8403 0.1694 -0.3373 0.041 Uiso 1 1 calc R . .
C21 C 0.48083(14) 0.38792(15) 0.15816(13) 0.0137(4) Uani 1 1 d . . .
C22 C 0.44902(15) 0.29781(15) 0.05972(13) 0.0168(4) Uani 1 1 d . . .
H22 H 0.5017 0.3057 0.0152 0.020 Uiso 1 1 calc R . .
C23 C 0.33755(15) 0.19531(16) 0.02795(14) 0.0200(4) Uani 1 1 d . . .
H23 H 0.3159 0.1338 -0.0375 0.024 Uiso 1 1 calc R . .
C24 C 0.25910(16) 0.18553(16) 0.09436(14) 0.0217(4) Uani 1 1 d . . .
H24 H 0.1845 0.1174 0.0730 0.026 Uiso 1 1 calc R . .
C25 C 0.29075(16) 0.27621(16) 0.19230(14) 0.0231(4) Uani 1 1 d . . .
H25 H 0.2371 0.2695 0.2360 0.028 Uiso 1 1 calc R . .
C26 C 0.40242(15) 0.37690(16) 0.22507(14) 0.0200(4) Uani 1 1 d . . .
H26 H 0.4249 0.4368 0.2914 0.024 Uiso 1 1 calc R . .
C27 C 0.59805(15) 0.66930(15) 0.21667(13) 0.0138(4) Uani 1 1 d . . .
C28 C 0.48282(15) 0.65317(16) 0.19409(13) 0.0160(4) Uani 1 1 d . . .
H28 H 0.4182 0.5757 0.1731 0.019 Uiso 1 1 calc R . .
C29 C 0.46457(16) 0.75356(16) 0.20309(13) 0.0196(4) Uani 1 1 d . . .
H29 H 0.3874 0.7434 0.1880 0.024 Uiso 1 1 calc R . .
C30 C 0.56006(16) 0.86814(16) 0.23417(13) 0.0205(4) Uani 1 1 d . . .
H30 H 0.5470 0.9351 0.2402 0.025 Uiso 1 1 calc R . .
C31 C 0.67550(16) 0.88452(16) 0.25660(15) 0.0245(4) Uani 1 1 d . . .
H31 H 0.7398 0.9621 0.2773 0.029 Uiso 1 1 calc R . .
C32 C 0.69466(16) 0.78516(16) 0.24817(14) 0.0231(4) Uani 1 1 d . . .
H32 H 0.7719 0.7957 0.2635 0.028 Uiso 1 1 calc R . .
C33 C 0.72010(14) 0.51772(15) 0.09547(12) 0.0132(4) Uani 1 1 d . . .
C34 C 0.76747(15) 0.43489(15) 0.07599(13) 0.0175(4) Uani 1 1 d . . .
H34 H 0.7537 0.3859 0.1129 0.021 Uiso 1 1 calc R . .
C35 C 0.83508(16) 0.42565(16) 0.00153(13) 0.0211(4) Uani 1 1 d . . .
H35 H 0.8677 0.3710 -0.0113 0.025 Uiso 1 1 calc R . .
C36 C 0.85426(15) 0.49781(15) -0.05395(13) 0.0191(4) Uani 1 1 d . . .
H36 H 0.9001 0.4918 -0.1038 0.023 Uiso 1 1 calc R . .
C37 C 0.80577(15) 0.57857(15) -0.03580(13) 0.0175(4) Uani 1 1 d . . .
H37 H 0.8183 0.6261 -0.0739 0.021 Uiso 1 1 calc R . .
C38 C 0.73851(14) 0.58917(15) 0.03894(13) 0.0157(4) Uani 1 1 d . . .
H38 H 0.7058 0.6437 0.0513 0.019 Uiso 1 1 calc R . .
C39 C 0.71879(15) 0.57133(15) 0.32970(13) 0.0162(4) Uani 1 1 d . . .
C40 C 0.80873(16) 0.53702(16) 0.33779(14) 0.0218(4) Uani 1 1 d . . .
H40 H 0.8270 0.4928 0.2792 0.026 Uiso 1 1 calc R . .
C41 C 0.87047(17) 0.56941(17) 0.43397(15) 0.0291(5) Uani 1 1 d . . .
H41 H 0.9309 0.5471 0.4400 0.035 Uiso 1 1 calc R . .
C42 C 0.84333(19) 0.63454(18) 0.52106(16) 0.0354(5) Uani 1 1 d . . .
H42 H 0.8852 0.6559 0.5855 0.042 Uiso 1 1 calc R . .
C43 C 0.7540(2) 0.66796(19) 0.51256(15) 0.0370(5) Uani 1 1 d . . .
H43 H 0.7356 0.7116 0.5714 0.044 Uiso 1 1 calc R . .
C44 C 0.69175(18) 0.63717(17) 0.41730(14) 0.0275(5) Uani 1 1 d . . .
H44 H 0.6319 0.6604 0.4119 0.033 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
As1 C33 1.9057(16) . ?
As1 C21 1.9152(16) . ?
As1 C39 1.9136(17) . ?
As1 C27 1.9129(16) . ?
P1 C1 1.8177(17) . ?
P1 C12 1.8218(17) . ?
P1 S1 1.9797(6) . ?
P1 S2 1.9792(7) . ?
C1 C2 1.382(2) . ?
C1 C6 1.400(2) . ?
C2 C3 1.399(2) . ?
C3 C4 1.400(2) . ?
C3 C13 1.529(2) . ?
C4 C5 1.382(2) . ?
C5 C6 1.392(2) . ?
C6 C7 1.476(2) . ?
C7 C8 1.389(2) . ?
C7 C12 1.402(2) . ?
C8 C9 1.381(2) . ?
C9 C10 1.407(2) . ?
C10 C11 1.398(2) . ?
C10 C17 1.531(2) . ?
C11 C12 1.386(2) . ?
C13 C14 1.524(2) . ?
C13 C16 1.536(2) . ?
C13 C15 1.529(2) . ?
C17 C19 1.529(2) . ?
C17 C20 1.535(2) . ?
C17 C18 1.535(2) . ?
C21 C22 1.387(2) . ?
C21 C26 1.391(2) . ?
C22 C23 1.394(2) . ?
C23 C24 1.385(2) . ?
C24 C25 1.385(2) . ?
C25 C26 1.385(2) . ?
C27 C32 1.391(2) . ?
C27 C28 1.384(2) . ?
C28 C29 1.386(2) . ?
C29 C30 1.375(2) . ?
C30 C31 1.385(2) . ?
C31 C32 1.381(2) . ?
C33 C38 1.390(2) . ?
C33 C34 1.390(2) . ?
C34 C35 1.382(2) . ?
C35 C36 1.384(2) . ?
C36 C37 1.378(2) . ?
C37 C38 1.383(2) . ?
C39 C44 1.387(2) . ?
C39 C40 1.392(2) . ?
C40 C41 1.382(2) . ?
C41 C42 1.379(3) . ?
C42 C43 1.378(3) . ?
C43 C44 1.379(3) . ?

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
C33 As1 C21 109.38(7) . . ?
C33 As1 C39 111.54(7) . . ?
C21 As1 C39 112.62(7) . . ?
C33 As1 C27 107.80(7) . . ?
C21 As1 C27 108.59(7) . . ?
C39 As1 C27 106.73(7) . . ?
C1 P1 C12 90.74(8) . . ?
C1 P1 S1 112.26(6) . . ?
C12 P1 S1 111.04(6) . . ?
C1 P1 S2 108.36(6) . . ?
C12 P1 S2 111.60(5) . . ?
S1 P1 S2 119.22(3) . . ?
C2 C1 C6 121.12(15) . . ?
C2 C1 P1 127.41(13) . . ?
C6 C1 P1 111.37(12) . . ?
C1 C2 C3 120.95(16) . . ?
C2 C3 C4 117.00(15) . . ?
C2 C3 C13 122.52(15) . . ?
C4 C3 C13 120.47(15) . . ?
C5 C4 C3 122.66(16) . . ?
C4 C5 C6 119.57(16) . . ?
C5 C6 C1 118.67(15) . . ?
C5 C6 C7 127.98(15) . . ?
C1 C6 C7 113.28(14) . . ?
C8 C7 C12 118.77(15) . . ?
C8 C7 C6 127.71(15) . . ?
C12 C7 C6 113.52(14) . . ?
C9 C8 C7 119.68(16) . . ?
C8 C9 C10 122.47(16) . . ?
C11 C10 C9 117.19(15) . . ?
C11 C10 C17 123.42(15) . . ?
C9 C10 C17 119.39(15) . . ?
C12 C11 C10 120.64(15) . . ?
C11 C12 C7 121.16(15) . . ?
C11 C12 P1 127.82(13) . . ?
C7 C12 P1 111.01(12) . . ?
C14 C13 C3 112.55(15) . . ?
C14 C13 C16 107.55(15) . . ?
C3 C13 C16 110.67(15) . . ?
C14 C13 C15 108.55(16) . . ?
C3 C13 C15 108.21(14) . . ?
C16 C13 C15 109.25(17) . . ?
C19 C17 C20 107.25(15) . . ?
C19 C17 C18 108.89(14) . . ?
C20 C17 C18 108.90(15) . . ?
C19 C17 C10 111.81(14) . . ?
C20 C17 C10 110.56(14) . . ?
C18 C17 C10 109.36(14) . . ?
C22 C21 C26 120.58(16) . . ?
C22 C21 As1 119.97(12) . . ?
C26 C21 As1 119.35(13) . . ?
C21 C22 C23 119.54(16) . . ?
C24 C23 C22 119.68(17) . . ?
C25 C24 C23 120.62(17) . . ?
C24 C25 C26 119.94(17) . . ?
C25 C26 C21 119.61(17) . . ?
C32 C27 C28 120.34(15) . . ?
C32 C27 As1 118.14(12) . . ?
C28 C27 As1 121.47(12) . . ?
C29 C28 C27 119.38(16) . . ?
C30 C29 C28 120.31(16) . . ?
C29 C30 C31 120.44(16) . . ?
C32 C31 C30 119.72(17) . . ?
C31 C32 C27 119.80(16) . . ?
C38 C33 C34 120.24(15) . . ?
C38 C33 As1 119.90(12) . . ?
C34 C33 As1 119.86(13) . . ?
C35 C34 C33 119.69(16) . . ?
C34 C35 C36 119.93(16) . . ?
C37 C36 C35 120.42(16) . . ?
C36 C37 C38 120.19(16) . . ?
C37 C38 C33 119.52(15) . . ?
C44 C39 C40 120.21(16) . . ?
C44 C39 As1 117.28(13) . . ?
C40 C39 As1 122.51(13) . . ?
C41 C40 C39 119.21(17) . . ?
C42 C41 C40 120.58(18) . . ?
C41 C42 C43 119.94(18) . . ?
C44 C43 C42 120.43(19) . . ?
C43 C44 C39 119.64(18) . . ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.064
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx2085
_database_code_depnum_ccdc_archive 'CCDC 1404551'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H48 Np O P4 S8'
_chemical_formula_weight         1306.26

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'
P P 0.1023 0.0942 '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'
Np Np -11.4937 4.1493 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9835(9)
_cell_length_b                   13.3013(10)
_cell_length_c                   18.4912(14)
_cell_angle_alpha                94.945(1)
_cell_angle_beta                 95.113(1)
_cell_angle_gamma                96.364(1)
_cell_volume                     2661.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1298
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5939
_exptl_absorpt_correction_T_max  0.6695
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31406
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         28.66
_reflns_number_total             12585
_reflns_number_gt                11294
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0219P)²+0.0000P] 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_number_reflns         12585
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0480
_refine_ls_wR_factor_gt          0.0465
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.002
_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
Np1 Np 0.734464(7) 0.742185(6) 0.741672(4) 0.01075(3) Uani 1 1 d . . .
P1 P 0.48624(5) 0.84293(4) 0.81139(3) 0.01372(11) Uani 1 1 d . . .
P2 P 0.73595(5) 0.86951(4) 0.58685(3) 0.01555(12) Uani 1 1 d . . .
P3 P 0.79323(5) 0.51253(4) 0.65717(3) 0.01475(11) Uani 1 1 d . . .
P4 P 0.92346(5) 0.73434(4) 0.90135(3) 0.01338(11) Uani 1 1 d . . .
S1 S 0.65694(5) 0.91619(4) 0.81093(3) 0.01768(11) Uani 1 1 d . . .
S2 S 0.48646(5) 0.69670(4) 0.77364(3) 0.01582(11) Uani 1 1 d . . .
S3 S 0.59830(5) 0.77019(4) 0.61199(3) 0.01920(12) Uani 1 1 d . . .
S4 S 0.86264(5) 0.90125(4) 0.67334(3) 0.01757(11) Uani 1 1 d . . .
S5 S 0.63036(5) 0.53961(4) 0.69105(3) 0.01526(11) Uani 1 1 d . . .
S6 S 0.90941(5) 0.64201(4) 0.67368(3) 0.02165(12) Uani 1 1 d . . .
S7 S 0.95752(5) 0.82752(4) 0.82399(3) 0.01515(11) Uani 1 1 d . . .
S8 S 0.76885(5) 0.63999(4) 0.86830(3) 0.01645(11) Uani 1 1 d . . .
C1 C 0.37474(19) 0.90214(16) 0.75720(11) 0.0147(4) Uani 1 1 d . . .
C2 C 0.3876(2) 1.00719(17) 0.75379(13) 0.0210(5) Uani 1 1 d . . .
H2 H 0.4575 1.0472 0.7767 0.025 Uiso 1 1 calc R . .
C3 C 0.2962(2) 1.05191(18) 0.71638(13) 0.0249(5) Uani 1 1 d . . .
H3 H 0.3047 1.1219 0.7143 0.030 Uiso 1 1 calc R . .
C4 C 0.1923(2) 0.99250(19) 0.68211(13) 0.0246(5) Uani 1 1 d . . .
H4 H 0.1309 1.0227 0.6572 0.030 Uiso 1 1 calc R . .
C5 C 0.1795(2) 0.88809(19) 0.68470(13) 0.0245(5) Uani 1 1 d . . .
H5 H 0.1100 0.8482 0.6612 0.029 Uiso 1 1 calc R . .
C6 C 0.2703(2) 0.84342(17) 0.72240(12) 0.0193(5) Uani 1 1 d . . .
H6 H 0.2613 0.7734 0.7244 0.023 Uiso 1 1 calc R . .
C7 C 0.44038(19) 0.85329(16) 0.90310(12) 0.0156(4) Uani 1 1 d . . .
C8 C 0.4902(2) 0.79274(18) 0.95291(13) 0.0231(5) Uani 1 1 d . . .
H8 H 0.5402 0.7445 0.9379 0.028 Uiso 1 1 calc R . .
C9 C 0.4649(2) 0.80471(19) 1.02499(13) 0.0270(5) Uani 1 1 d . . .
H9 H 0.4991 0.7650 1.0586 0.032 Uiso 1 1 calc R . .
C10 C 0.3895(2) 0.87504(19) 1.04719(13) 0.0257(5) Uani 1 1 d . . .
H10 H 0.3717 0.8817 1.0955 0.031 Uiso 1 1 calc R . .
C11 C 0.3405(2) 0.93553(18) 0.99812(13) 0.0242(5) Uani 1 1 d . . .
H11 H 0.2910 0.9839 1.0135 0.029 Uiso 1 1 calc R . .
C12 C 0.3649(2) 0.92432(17) 0.92581(13) 0.0208(5) Uani 1 1 d . . .
H12 H 0.3307 0.9644 0.8925 0.025 Uiso 1 1 calc R . .
C13 C 0.67907(19) 0.98618(16) 0.56305(12) 0.0165(4) Uani 1 1 d . . .
C14 C 0.6006(2) 1.0298(2) 0.60795(14) 0.0316(6) Uani 1 1 d . . .
H14 H 0.5744 0.9970 0.6472 0.038 Uiso 1 1 calc R . .
C15 C 0.5614(3) 1.1220(2) 0.59417(15) 0.0344(6) Uani 1 1 d . . .
H15 H 0.5083 1.1508 0.6241 0.041 Uiso 1 1 calc R . .
C16 C 0.6000(2) 1.17159(18) 0.53655(13) 0.0248(5) Uani 1 1 d . . .
H16 H 0.5742 1.2341 0.5280 0.030 Uiso 1 1 calc R . .
C17 C 0.6768(3) 1.1285(2) 0.49176(14) 0.0324(6) Uani 1 1 d . . .
H17 H 0.7028 1.1617 0.4526 0.039 Uiso 1 1 calc R . .
C18 C 0.7160(2) 1.03528(19) 0.50461(13) 0.0272(6) Uani 1 1 d . . .
H18 H 0.7673 1.0059 0.4737 0.033 Uiso 1 1 calc R . .
C19 C 0.8025(2) 0.81908(17) 0.50741(12) 0.0195(5) Uani 1 1 d . . .
C20 C 0.9234(2) 0.85120(19) 0.49575(13) 0.0268(5) Uani 1 1 d . . .
H20 H 0.9726 0.8968 0.5302 0.032 Uiso 1 1 calc R . .
C21 C 0.9704(2) 0.8151(2) 0.43269(15) 0.0344(6) Uani 1 1 d . . .
H21 H 1.0511 0.8370 0.4249 0.041 Uiso 1 1 calc R . .
C22 C 0.8988(3) 0.7472(2) 0.38166(15) 0.0367(7) Uani 1 1 d . . .
H22 H 0.9310 0.7234 0.3395 0.044 Uiso 1 1 calc R . .
C23 C 0.7797(3) 0.7146(2) 0.39297(15) 0.0409(7) Uani 1 1 d . . .
H23 H 0.7313 0.6687 0.3584 0.049 Uiso 1 1 calc R . .
C24 C 0.7309(2) 0.7499(2) 0.45584(14) 0.0326(6) Uani 1 1 d . . .
H24 H 0.6502 0.7272 0.4634 0.039 Uiso 1 1 calc R . .
C25 C 0.8542(2) 0.41442(18) 0.70673(12) 0.0208(5) Uani 1 1 d . . .
C26 C 0.9447(2) 0.4401(2) 0.76484(13) 0.0333(6) Uani 1 1 d . . .
H26 H 0.9804 0.5070 0.7756 0.040 Uiso 1 1 calc R . .
C27 C 0.9812(3) 0.3655(3) 0.80632(16) 0.0510(9) Uani 1 1 d . . .
H27 H 1.0419 0.3822 0.8452 0.061 Uiso 1 1 calc R . .
C28 C 0.9284(3) 0.2666(3) 0.79047(19) 0.0597(11) Uani 1 1 d . . .
H28 H 0.9524 0.2169 0.8193 0.072 Uiso 1 1 calc R . .
C29 C 0.8405(3) 0.2405(2) 0.73234(19) 0.0484(9) Uani 1 1 d . . .
H29 H 0.8063 0.1731 0.7214 0.058 Uiso 1 1 calc R . .
C30 C 0.8027(2) 0.31427(19) 0.68999(15) 0.0314(6) Uani 1 1 d . . .
H30 H 0.7431 0.2968 0.6506 0.038 Uiso 1 1 calc R . .
C31 C 0.7762(2) 0.46431(16) 0.56211(12) 0.0166(4) Uani 1 1 d . . .
C32 C 0.8713(2) 0.41737(19) 0.53402(14) 0.0278(6) Uani 1 1 d . . .
H32 H 0.9402 0.4078 0.5645 0.033 Uiso 1 1 calc R . .
C33 C 0.8626(3) 0.3848(2) 0.46005(14) 0.0367(7) Uani 1 1 d . . .
H33 H 0.9257 0.3533 0.4409 0.044 Uiso 1 1 calc R . .
C34 C 0.7607(3) 0.3994(2) 0.41543(14) 0.0376(7) Uani 1 1 d . . .
H34 H 0.7555 0.3781 0.3659 0.045 Uiso 1 1 calc R . .
C35 C 0.6665(3) 0.4451(2) 0.44293(14) 0.0399(7) Uani 1 1 d . . .
H35 H 0.5976 0.4540 0.4121 0.048 Uiso 1 1 calc R . .
C36 C 0.6736(2) 0.4780(2) 0.51654(13) 0.0298(6) Uani 1 1 d . . .
H36 H 0.6097 0.5091 0.5352 0.036 Uiso 1 1 calc R . .
C37 C 0.9105(2) 0.80391(16) 0.98821(11) 0.0159(4) Uani 1 1 d . . .
C38 C 0.8074(2) 0.78887(19) 1.02599(13) 0.0253(5) Uani 1 1 d . . .
H38 H 0.7407 0.7422 1.0065 0.030 Uiso 1 1 calc R . .
C39 C 0.8041(2) 0.8440(2) 1.09324(13) 0.0278(6) Uani 1 1 d . . .
H39 H 0.7357 0.8332 1.1190 0.033 Uiso 1 1 calc R . .
C40 C 0.9015(2) 0.91423(18) 1.12156(13) 0.0248(5) Uani 1 1 d . . .
H40 H 0.8980 0.9522 1.1658 0.030 Uiso 1 1 calc R . .
C41 C 1.0047(2) 0.92853(17) 1.08436(12) 0.0237(5) Uani 1 1 d . . .
H41 H 1.0711 0.9754 1.1040 0.028 Uiso 1 1 calc R . .
C42 C 1.0097(2) 0.87331(17) 1.01799(12) 0.0209(5) Uani 1 1 d . . .
H42 H 1.0796 0.8827 0.9933 0.025 Uiso 1 1 calc R . .
C43 C 1.05414(19) 0.66535(16) 0.92055(12) 0.0153(4) Uani 1 1 d . . .
C44 C 1.0662(2) 0.62186(18) 0.98612(13) 0.0240(5) Uani 1 1 d . . .
H44 H 1.0090 0.6299 1.0197 0.029 Uiso 1 1 calc R . .
C45 C 1.1635(2) 0.56648(19) 1.00160(14) 0.0292(6) Uani 1 1 d . . .
H45 H 1.1715 0.5373 1.0454 0.035 Uiso 1 1 calc R . .
C46 C 1.2482(2) 0.55490(19) 0.95182(15) 0.0314(6) Uani 1 1 d . . .
H46 H 1.3132 0.5175 0.9621 0.038 Uiso 1 1 calc R . .
C47 C 1.2372(2) 0.5982(2) 0.88710(16) 0.0337(6) Uani 1 1 d . . .
H47 H 1.2951 0.5903 0.8539 0.040 Uiso 1 1 calc R . .
C48 C 1.1401(2) 0.65378(18) 0.87099(13) 0.0242(5) Uani 1 1 d . . .
H48 H 1.1328 0.6830 0.8271 0.029 Uiso 1 1 calc R . .
C49 C 0.5380(3) 0.2918(2) 0.78085(16) 0.0371(7) Uani 1 1 d . . .
H49A H 0.5406 0.3158 0.7329 0.044 Uiso 1 1 calc R . .
H49B H 0.5734 0.2281 0.7807 0.044 Uiso 1 1 calc R . .
C50 C 0.6081(2) 0.36978(19) 0.83839(14) 0.0316(6) Uani 1 1 d . . .
H50A H 0.6692 0.4138 0.8175 0.038 Uiso 1 1 calc R . .
H50B H 0.6486 0.3373 0.8773 0.038 Uiso 1 1 calc R . .
C51 C 0.5071(2) 0.4296(2) 0.86649(16) 0.0364(7) Uani 1 1 d . . .
H51A H 0.5029 0.4253 0.9183 0.044 Uiso 1 1 calc R . .
H51B H 0.5217 0.5005 0.8576 0.044 Uiso 1 1 calc R . .
C52 C 0.3901(3) 0.3776(2) 0.82268(19) 0.0479(8) Uani 1 1 d . . .
H52A H 0.3219 0.3747 0.8527 0.057 Uiso 1 1 calc R . .
H52B H 0.3692 0.4142 0.7810 0.057 Uiso 1 1 calc R . .
O1 O 0.41495(18) 0.27841(15) 0.79943(11) 0.0438(5) Uani 1 1 d . . .


_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
Np1 S6 2.7853(6) . ?
Np1 S3 2.7863(6) . ?
Np1 S1 2.8004(5) . ?
Np1 S8 2.8245(6) . ?
Np1 S7 2.8334(6) . ?
Np1 S2 2.8493(6) . ?
Np1 S5 2.8523(6) . ?
Np1 S4 2.8587(6) . ?
P1 C1 1.804(2) . ?
P1 C7 1.810(2) . ?
P1 S2 2.0094(8) . ?
P1 S1 2.0160(8) . ?
P2 C19 1.809(2) . ?
P2 C13 1.810(2) . ?
P2 S4 2.0072(8) . ?
P2 S3 2.0089(8) . ?
P3 C31 1.805(2) . ?
P3 C25 1.811(2) . ?
P3 S5 2.0065(8) . ?
P3 S6 2.0101(8) . ?
P4 C37 1.808(2) . ?
P4 C43 1.813(2) . ?
P4 S7 2.0052(8) . ?
P4 S8 2.0106(8) . ?
C1 C6 1.387(3) . ?
C1 C2 1.396(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.383(3) . ?
C4 C5 1.386(3) . ?
C5 C6 1.383(3) . ?
C7 C12 1.387(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.385(3) . ?
C9 C10 1.377(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.386(3) . ?
C13 C18 1.378(3) . ?
C13 C14 1.388(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.375(3) . ?
C16 C17 1.369(3) . ?
C17 C18 1.389(3) . ?
C19 C24 1.389(3) . ?
C19 C20 1.390(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.374(4) . ?
C22 C23 1.372(4) . ?
C23 C24 1.390(3) . ?
C25 C30 1.386(3) . ?
C25 C26 1.390(3) . ?
C26 C27 1.377(4) . ?
C27 C28 1.374(5) . ?
C28 C29 1.373(5) . ?
C29 C30 1.384(4) . ?
C31 C36 1.384(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.390(3) . ?
C33 C34 1.372(4) . ?
C34 C35 1.371(4) . ?
C35 C36 1.386(3) . ?
C37 C42 1.387(3) . ?
C37 C38 1.388(3) . ?
C38 C39 1.394(3) . ?
C39 C40 1.374(3) . ?
C40 C41 1.381(3) . ?
C41 C42 1.384(3) . ?
C43 C48 1.384(3) . ?
C43 C44 1.390(3) . ?
C44 C45 1.386(3) . ?
C45 C46 1.377(4) . ?
C46 C47 1.374(4) . ?
C47 C48 1.389(3) . ?
C49 O1 1.420(3) . ?
C49 C50 1.512(4) . ?
C50 C51 1.536(4) . ?
C51 C52 1.519(4) . ?
C52 O1 1.415(3) . ?

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
S6 Np1 S3 94.785(18) . . ?
S6 Np1 S1 151.670(17) . . ?
S3 Np1 S1 90.666(17) . . ?
S6 Np1 S8 92.175(18) . . ?
S3 Np1 S8 151.104(16) . . ?
S1 Np1 S8 96.364(17) . . ?
S6 Np1 S7 77.460(17) . . ?
S3 Np1 S7 138.270(16) . . ?
S1 Np1 S7 80.015(16) . . ?
S8 Np1 S7 70.626(16) . . ?
S6 Np1 S2 137.474(17) . . ?
S3 Np1 S2 76.928(17) . . ?
S1 Np1 S2 70.813(16) . . ?
S8 Np1 S2 79.022(16) . . ?
S7 Np1 S2 134.827(16) . . ?
S6 Np1 S5 70.839(17) . . ?
S3 Np1 S5 77.975(16) . . ?
S1 Np1 S5 137.392(16) . . ?
S8 Np1 S5 77.937(16) . . ?
S7 Np1 S5 133.906(15) . . ?
S2 Np1 S5 66.636(15) . . ?
S6 Np1 S4 77.746(18) . . ?
S3 Np1 S4 70.833(16) . . ?
S1 Np1 S4 77.882(17) . . ?
S8 Np1 S4 138.052(16) . . ?
S7 Np1 S4 67.447(16) . . ?
S2 Np1 S4 134.243(15) . . ?
S5 Np1 S4 133.120(16) . . ?
C1 P1 C7 105.53(10) . . ?
C1 P1 S2 110.95(7) . . ?
C7 P1 S2 110.96(7) . . ?
C1 P1 S1 110.95(7) . . ?
C7 P1 S1 109.61(7) . . ?
S2 P1 S1 108.82(3) . . ?
C19 P2 C13 106.05(10) . . ?
C19 P2 S4 111.35(8) . . ?
C13 P2 S4 108.99(8) . . ?
C19 P2 S3 110.56(8) . . ?
C13 P2 S3 110.74(8) . . ?
S4 P2 S3 109.11(3) . . ?
C31 P3 C25 106.08(10) . . ?
C31 P3 S5 111.00(8) . . ?
C25 P3 S5 109.75(8) . . ?
C31 P3 S6 110.50(8) . . ?
C25 P3 S6 110.60(8) . . ?
S5 P3 S6 108.89(3) . . ?
C37 P4 C43 103.17(10) . . ?
C37 P4 S7 111.89(7) . . ?
C43 P4 S7 110.07(7) . . ?
C37 P4 S8 110.78(8) . . ?
C43 P4 S8 111.81(7) . . ?
S7 P4 S8 109.06(3) . . ?
P1 S1 Np1 90.62(2) . . ?
P1 S2 Np1 89.36(2) . . ?
P2 S3 Np1 90.53(2) . . ?
P2 S4 Np1 88.51(2) . . ?
P3 S5 Np1 89.11(2) . . ?
P3 S6 Np1 90.95(3) . . ?
P4 S7 Np1 89.99(2) . . ?
P4 S8 Np1 90.13(2) . . ?
C6 C1 C2 119.3(2) . . ?
C6 C1 P1 119.50(17) . . ?
C2 C1 P1 121.04(17) . . ?
C3 C2 C1 120.1(2) . . ?
C4 C3 C2 120.0(2) . . ?
C3 C4 C5 120.2(2) . . ?
C6 C5 C4 119.8(2) . . ?
C5 C6 C1 120.6(2) . . ?
C12 C7 C8 119.8(2) . . ?
C12 C7 P1 121.90(17) . . ?
C8 C7 P1 118.16(16) . . ?
C9 C8 C7 119.6(2) . . ?
C10 C9 C8 120.4(2) . . ?
C11 C10 C9 120.2(2) . . ?
C10 C11 C12 120.0(2) . . ?
C11 C12 C7 120.0(2) . . ?
C18 C13 C14 119.3(2) . . ?
C18 C13 P2 122.38(18) . . ?
C14 C13 P2 118.18(17) . . ?
C15 C14 C13 119.9(2) . . ?
C16 C15 C14 120.7(2) . . ?
C17 C16 C15 119.7(2) . . ?
C16 C17 C18 120.2(2) . . ?
C13 C18 C17 120.2(2) . . ?
C24 C19 C20 119.3(2) . . ?
C24 C19 P2 119.72(18) . . ?
C20 C19 P2 120.98(18) . . ?
C21 C20 C19 119.9(2) . . ?
C22 C21 C20 120.6(3) . . ?
C23 C22 C21 119.9(2) . . ?
C22 C23 C24 120.3(3) . . ?
C19 C24 C23 120.0(3) . . ?
C30 C25 C26 120.2(2) . . ?
C30 C25 P3 119.29(18) . . ?
C26 C25 P3 120.35(19) . . ?
C27 C26 C25 119.5(3) . . ?
C28 C27 C26 120.3(3) . . ?
C29 C28 C27 120.5(3) . . ?
C28 C29 C30 120.1(3) . . ?
C29 C30 C25 119.5(3) . . ?
C36 C31 C32 120.0(2) . . ?
C36 C31 P3 121.07(17) . . ?
C32 C31 P3 118.84(18) . . ?
C33 C32 C31 119.6(2) . . ?
C34 C33 C32 119.8(2) . . ?
C35 C34 C33 120.8(2) . . ?
C34 C35 C36 120.1(3) . . ?
C31 C36 C35 119.6(2) . . ?
C42 C37 C38 119.6(2) . . ?
C42 C37 P4 117.72(17) . . ?
C38 C37 P4 122.64(17) . . ?
C37 C38 C39 119.7(2) . . ?
C40 C39 C38 120.2(2) . . ?
C39 C40 C41 120.1(2) . . ?
C40 C41 C42 120.2(2) . . ?
C41 C42 C37 120.1(2) . . ?
C48 C43 C44 119.8(2) . . ?
C48 C43 P4 121.48(17) . . ?
C44 C43 P4 118.75(17) . . ?
C45 C44 C43 120.1(2) . . ?
C46 C45 C44 119.7(2) . . ?
C47 C46 C45 120.4(2) . . ?
C46 C47 C48 120.3(2) . . ?
C43 C48 C47 119.6(2) . . ?
O1 C49 C50 106.2(2) . . ?
C49 C50 C51 103.3(2) . . ?
C52 C51 C50 103.6(2) . . ?
O1 C52 C51 106.1(2) . . ?
C52 O1 C49 104.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.087
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_dq0029s
_database_code_depnum_ccdc_archive 'CCDC 1404552'
_audit_update_record             
;
2015-08-12 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_dq0029s             
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Platon/Squeeze used to treat disordered solvent molecules.
;
_vrf_PLAT412_dq0029s             
;
PROBLEM: Short Intra XH3 .. XHn     H11    ..  H18B    ..       1.77 Ang.  
RESPONSE: Caused by disorder in methyl groups
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H128 Np P4 S8'
_chemical_formula_weight         2043.46

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'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   22.8029(17)
_cell_length_b                   20.2642(15)
_cell_length_c                   23.9268(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.0200(10)
_cell_angle_gamma                90.00
_cell_volume                     10388.1(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4228
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7507
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_process_details   'SADABS v. 2014/3 (Bruker AXS, 2013)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            117259
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         35.36
_reflns_number_total             22227
_reflns_number_gt                19663
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 Disordered tetrabutyl group refined with methyl groups in two positions,
 with site occupancy factors tied to 1.0 and 6 C-C distance restraints.
 Hydrogen atom positions were not refined on the disordered methyl groups. 
;

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.153 0.199 0.191 1781 768 '8 toluene'
2 0.131 -0.222 0.691 1781 765 '8 toluene'
_platon_squeeze_details          
;
;
_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)+(0.0509P)²+12.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         22227
_refine_ls_number_parameters     463
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1365
_refine_ls_wR_factor_gt          0.1331
_refine_ls_goodness_of_fit_ref   1.467
_refine_ls_restrained_S_all      1.472
_refine_ls_shift/su_max          0.004
_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
Np1 Np 0.0000 0.171275(6) 0.2500 0.01309(4) Uani 1 2 d S . .
S1 S 0.06377(3) 0.22293(3) 0.36485(3) 0.01868(10) Uani 1 1 d . . .
S2 S 0.08629(3) 0.26772(3) 0.24204(3) 0.02016(11) Uani 1 1 d . . .
S5 S -0.03677(3) 0.11911(3) 0.34296(3) 0.01779(10) Uani 1 1 d . . .
S6 S -0.09426(3) 0.07639(3) 0.20270(3) 0.01990(11) Uani 1 1 d . . .
P1 P 0.11234(3) 0.28256(3) 0.33011(3) 0.01668(11) Uani 1 1 d . . .
P3 P -0.09698(3) 0.05962(3) 0.28453(3) 0.01593(10) Uani 1 1 d . . .
C1 C 0.10851(12) 0.36700(12) 0.35110(11) 0.0197(4) Uani 1 1 d . . .
C2 C 0.05552(13) 0.40540(13) 0.34130(12) 0.0224(4) Uani 1 1 d . . .
H2 H 0.0167 0.3892 0.3179 0.027 Uiso 1 1 calc R . .
C3 C 0.06025(14) 0.46833(13) 0.36641(13) 0.0244(5) Uani 1 1 d . . .
C4 C 0.12013(16) 0.49129(14) 0.39949(14) 0.0296(6) Uani 1 1 d . . .
H4 H 0.1243 0.5338 0.4151 0.035 Uiso 1 1 calc R . .
C5 C 0.17349(15) 0.45307(14) 0.40996(14) 0.0281(5) Uani 1 1 d . . .
H5 H 0.2125 0.4697 0.4324 0.034 Uiso 1 1 calc R . .
C6 C 0.16787(13) 0.38924(13) 0.38635(12) 0.0226(5) Uani 1 1 d . . .
C7 C 0.21693(13) 0.33806(14) 0.39737(13) 0.0233(5) Uani 1 1 d . . .
C8 C 0.27891(14) 0.34236(19) 0.43483(17) 0.0342(7) Uani 1 1 d . . .
H8 H 0.2952 0.3820 0.4531 0.041 Uiso 1 1 calc R . .
C9 C 0.31642(14) 0.2852(2) 0.44440(16) 0.0365(7) Uani 1 1 d . . .
H9 H 0.3574 0.2877 0.4703 0.044 Uiso 1 1 calc R . .
C10 C 0.29447(13) 0.22539(18) 0.41660(14) 0.0299(6) Uani 1 1 d . A .
C11 C 0.23232(13) 0.22226(14) 0.37811(12) 0.0231(5) Uani 1 1 d . . .
H11 H 0.2164 0.1831 0.3584 0.028 Uiso 1 1 calc R . .
C12 C 0.19468(11) 0.27768(13) 0.36951(12) 0.0204(4) Uani 1 1 d . . .
C13 C 0.00211(16) 0.50916(14) 0.36199(14) 0.0299(6) Uani 1 1 d . . .
C14 C -0.05642(17) 0.48468(19) 0.3136(2) 0.0419(8) Uani 1 1 d . . .
H14A H -0.0504 0.4866 0.2758 0.063 Uiso 1 1 calc R . .
H14B H -0.0912 0.5121 0.3125 0.063 Uiso 1 1 calc R . .
H14C H -0.0647 0.4400 0.3219 0.063 Uiso 1 1 calc R . .
C15 C 0.0118(2) 0.58214(17) 0.3502(2) 0.0445(9) Uani 1 1 d . . .
H15A H 0.0187 0.5862 0.3129 0.067 Uiso 1 1 calc R . .
H15B H 0.0474 0.5989 0.3815 0.067 Uiso 1 1 calc R . .
H15C H -0.0246 0.6069 0.3486 0.067 Uiso 1 1 calc R . .
C16 C -0.0063(2) 0.5034(2) 0.42306(18) 0.0515(11) Uani 1 1 d . . .
H16A H -0.0420 0.5288 0.4228 0.077 Uiso 1 1 calc R . .
H16B H 0.0303 0.5199 0.4534 0.077 Uiso 1 1 calc R . .
H16C H -0.0125 0.4580 0.4310 0.077 Uiso 1 1 calc R . .
C17 C 0.33517(16) 0.16366(19) 0.42904(14) 0.0364(8) Uani 1 1 d D . .
C18 C 0.3093(7) 0.1084(6) 0.3899(6) 0.051(4) Uani 0.319(8) 1 d PD A 1
H18A H 0.3391 0.0932 0.3726 0.077 Uiso 0.319(8) 1 calc PR A 1
H18B H 0.2718 0.1220 0.3589 0.077 Uiso 0.319(8) 1 calc PR A 1
H18C H 0.2997 0.0732 0.4123 0.077 Uiso 0.319(8) 1 calc PR A 1
C19 C 0.4002(6) 0.1861(8) 0.4227(9) 0.056(4) Uani 0.319(8) 1 d PD A 1
H19A H 0.4270 0.1484 0.4275 0.085 Uiso 0.319(8) 1 calc PR A 1
H19B H 0.4200 0.2182 0.4528 0.085 Uiso 0.319(8) 1 calc PR A 1
H19C H 0.3926 0.2052 0.3841 0.085 Uiso 0.319(8) 1 calc PR A 1
C20 C 0.3501(8) 0.1555(8) 0.4934(5) 0.053(4) Uani 0.319(8) 1 d PD A 1
H20A H 0.3233 0.1226 0.5007 0.079 Uiso 0.319(8) 1 calc PR A 1
H20B H 0.3440 0.1967 0.5105 0.079 Uiso 0.319(8) 1 calc PR A 1
H20C H 0.3928 0.1419 0.5112 0.079 Uiso 0.319(8) 1 calc PR A 1
C18' C 0.3469(2) 0.1442(3) 0.3726(2) 0.0359(12) Uani 0.681(8) 1 d PD A 2
H18D H 0.3753 0.1075 0.3807 0.054 Uiso 0.681(8) 1 calc PR A 2
H18E H 0.3648 0.1809 0.3586 0.054 Uiso 0.681(8) 1 calc PR A 2
H18F H 0.3082 0.1319 0.3426 0.054 Uiso 0.681(8) 1 calc PR A 2
C19' C 0.2951(3) 0.1025(3) 0.4428(3) 0.0480(17) Uani 0.681(8) 1 d PD A 2
H19D H 0.2610 0.0918 0.4073 0.072 Uiso 0.681(8) 1 calc PR A 2
H19E H 0.2793 0.1153 0.4735 0.072 Uiso 0.681(8) 1 calc PR A 2
H19F H 0.3217 0.0647 0.4556 0.072 Uiso 0.681(8) 1 calc PR A 2
C20' C 0.3931(3) 0.1659(4) 0.4821(3) 0.058(2) Uani 0.681(8) 1 d PD A 2
H20D H 0.3826 0.1743 0.5170 0.088 Uiso 0.681(8) 1 calc PR A 2
H20E H 0.4197 0.2005 0.4773 0.088 Uiso 0.681(8) 1 calc PR A 2
H20F H 0.4145 0.1244 0.4863 0.088 Uiso 0.681(8) 1 calc PR A 2
C41 C -0.17407(11) 0.06283(13) 0.28882(11) 0.0190(4) Uani 1 1 d . . .
C42 C -0.20959(12) 0.11937(14) 0.28703(12) 0.0226(5) Uani 1 1 d . . .
H42 H -0.1955 0.1604 0.2796 0.027 Uiso 1 1 calc R . .
C43 C -0.26681(13) 0.11364(17) 0.29659(13) 0.0282(6) Uani 1 1 d . . .
C44 C -0.28650(14) 0.04975(19) 0.30475(15) 0.0332(6) Uani 1 1 d . . .
H44 H -0.3254 0.0448 0.3088 0.040 Uiso 1 1 calc R . .
C45 C -0.25081(13) -0.00610(17) 0.30698(14) 0.0296(6) Uani 1 1 d . . .
H45 H -0.2656 -0.0474 0.3128 0.035 Uiso 1 1 calc R . .
C46 C -0.19232(11) -0.00013(14) 0.30035(11) 0.0214(4) Uani 1 1 d . . .
C47 C -0.14350(12) -0.05084(13) 0.30922(12) 0.0213(4) Uani 1 1 d . . .
C48 C -0.14503(15) -0.11698(15) 0.32527(14) 0.0288(5) Uani 1 1 d . . .
H48 H -0.1818 -0.1357 0.3267 0.035 Uiso 1 1 calc R . .
C49 C -0.09058(16) -0.15454(15) 0.33916(15) 0.0303(6) Uani 1 1 d . . .
H49 H -0.0918 -0.1985 0.3498 0.036 Uiso 1 1 calc R . .
C50 C -0.03397(14) -0.12871(14) 0.33776(12) 0.0246(5) Uani 1 1 d . . .
C51 C -0.03384(13) -0.06346(13) 0.31934(12) 0.0228(4) Uani 1 1 d . . .
H51 H 0.0024 -0.0451 0.3165 0.027 Uiso 1 1 calc R . .
C52 C -0.08799(12) -0.02582(12) 0.30521(11) 0.0191(4) Uani 1 1 d . . .
C53 C -0.30392(16) 0.17436(19) 0.30251(17) 0.0368(8) Uani 1 1 d . . .
C54 C -0.2934(3) 0.1836(3) 0.3691(2) 0.0641(16) Uani 1 1 d . . .
H54A H -0.3204 0.2178 0.3740 0.096 Uiso 1 1 calc R . .
H54B H -0.2508 0.1957 0.3898 0.096 Uiso 1 1 calc R . .
H54C H -0.3026 0.1431 0.3853 0.096 Uiso 1 1 calc R . .
C55 C -0.37389(18) 0.1638(3) 0.2701(2) 0.0520(12) Uani 1 1 d . . .
H55A H -0.3809 0.1505 0.2298 0.078 Uiso 1 1 calc R . .
H55B H -0.3958 0.2043 0.2701 0.078 Uiso 1 1 calc R . .
H55C H -0.3889 0.1301 0.2900 0.078 Uiso 1 1 calc R . .
C56 C -0.28351(19) 0.2368(2) 0.2779(2) 0.0457(9) Uani 1 1 d . . .
H56A H -0.2887 0.2303 0.2367 0.069 Uiso 1 1 calc R . .
H56B H -0.2404 0.2457 0.2999 0.069 Uiso 1 1 calc R . .
H56C H -0.3086 0.2734 0.2816 0.069 Uiso 1 1 calc R . .
C57 C 0.02686(17) -0.16927(14) 0.36036(15) 0.0302(6) Uani 1 1 d . . .
C58 C 0.0145(2) -0.24256(16) 0.3454(2) 0.0450(9) Uani 1 1 d . . .
H58A H 0.0533 -0.2662 0.3580 0.067 Uiso 1 1 calc R . .
H58B H -0.0055 -0.2476 0.3032 0.067 Uiso 1 1 calc R . .
H58C H -0.0121 -0.2598 0.3655 0.067 Uiso 1 1 calc R . .
C59 C 0.0533(2) -0.1618(2) 0.42826(19) 0.0498(11) Uani 1 1 d . . .
H59A H 0.0260 -0.1831 0.4455 0.075 Uiso 1 1 calc R . .
H59B H 0.0567 -0.1158 0.4385 0.075 Uiso 1 1 calc R . .
H59C H 0.0938 -0.1819 0.4433 0.075 Uiso 1 1 calc R . .
C60 C 0.07575(17) -0.14451(19) 0.3350(2) 0.0410(8) Uani 1 1 d . . .
H60A H 0.1117 -0.1728 0.3480 0.061 Uiso 1 1 calc R . .
H60B H 0.0878 -0.1003 0.3487 0.061 Uiso 1 1 calc R . .
H60C H 0.0586 -0.1448 0.2923 0.061 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
Np1 S6 2.8165(6) . ?
Np1 S6 2.8165(6) 2 ?
Np1 S2 2.8257(6) . ?
Np1 S2 2.8258(6) 2 ?
Np1 S1 2.8329(6) . ?
Np1 S1 2.8329(6) 2 ?
Np1 S5 2.8363(6) . ?
Np1 S5 2.8363(6) 2 ?
S1 P1 2.0019(9) . ?
S2 P1 2.0067(9) . ?
S5 P3 1.9946(9) . ?
S6 P3 2.0089(9) . ?
P1 C12 1.792(3) . ?
P1 C1 1.794(3) . ?
P3 C52 1.793(2) . ?
P3 C41 1.797(2) . ?
C1 C2 1.388(4) . ?
C1 C6 1.402(4) . ?
C2 C3 1.398(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.403(5) . ?
C3 C13 1.535(4) . ?
C4 C5 1.391(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.400(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.482(4) . ?
C7 C8 1.393(4) . ?
C7 C12 1.402(4) . ?
C8 C9 1.411(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.391(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.402(4) . ?
C10 C17 1.525(5) . ?
C11 C12 1.386(4) . ?
C11 H11 0.9300 . ?
C13 C14 1.520(5) . ?
C13 C15 1.536(5) . ?
C13 C16 1.542(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.450(12) . ?
C17 C20 1.469(12) . ?
C17 C20' 1.487(6) . ?
C17 C18' 1.517(5) . ?
C17 C19 1.608(12) . ?
C17 C19' 1.637(7) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
C19' H19D 0.9600 . ?
C19' H19E 0.9600 . ?
C19' H19F 0.9600 . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C41 C46 1.398(4) . ?
C41 C42 1.395(4) . ?
C42 C43 1.404(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.406(5) . ?
C43 C53 1.527(4) . ?
C44 C45 1.384(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.401(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.476(4) . ?
C47 C48 1.398(4) . ?
C47 C52 1.397(4) . ?
C48 C49 1.396(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.404(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.394(4) . ?
C50 C57 1.542(4) . ?
C51 C52 1.391(4) . ?
C51 H51 0.9300 . ?
C53 C55 1.531(6) . ?
C53 C54 1.541(6) . ?
C53 C56 1.533(6) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 C60 1.525(6) . ?
C57 C58 1.531(4) . ?
C57 C59 1.535(5) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?

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
S6 Np1 S6 93.89(3) . 2 ?
S6 Np1 S2 153.944(18) . . ?
S6 Np1 S2 92.64(2) 2 . ?
S6 Np1 S2 92.64(2) . 2 ?
S6 Np1 S2 153.941(18) 2 2 ?
S2 Np1 S2 92.48(3) . 2 ?
S6 Np1 S1 135.211(17) . . ?
S6 Np1 S1 78.157(19) 2 . ?
S2 Np1 S1 70.841(18) . . ?
S2 Np1 S1 79.460(19) 2 . ?
S6 Np1 S1 78.158(19) . 2 ?
S6 Np1 S1 135.214(17) 2 2 ?
S2 Np1 S1 79.460(19) . 2 ?
S2 Np1 S1 70.841(18) 2 2 ?
S1 Np1 S1 136.63(3) . 2 ?
S6 Np1 S5 70.781(18) . . ?
S6 Np1 S5 79.646(18) 2 . ?
S2 Np1 S5 135.259(18) . . ?
S2 Np1 S5 78.769(18) 2 . ?
S1 Np1 S5 64.432(18) . . ?
S1 Np1 S5 134.990(18) 2 . ?
S6 Np1 S5 79.648(18) . 2 ?
S6 Np1 S5 70.782(18) 2 2 ?
S2 Np1 S5 78.771(18) . 2 ?
S2 Np1 S5 135.261(18) 2 2 ?
S1 Np1 S5 134.990(18) . 2 ?
S1 Np1 S5 64.433(18) 2 2 ?
S5 Np1 S5 136.24(3) . 2 ?
P1 S1 Np1 89.63(3) . . ?
P1 S2 Np1 89.74(3) . . ?
P3 S5 Np1 89.60(3) . . ?
P3 S6 Np1 89.87(3) . . ?
C12 P1 C1 92.75(12) . . ?
C12 P1 S1 112.15(10) . . ?
C1 P1 S1 111.88(9) . . ?
C12 P1 S2 115.11(9) . . ?
C1 P1 S2 114.31(9) . . ?
S1 P1 S2 109.79(4) . . ?
C52 P3 C41 92.34(12) . . ?
C52 P3 S5 113.83(9) . . ?
C41 P3 S5 112.96(9) . . ?
C52 P3 S6 113.17(9) . . ?
C41 P3 S6 114.00(9) . . ?
S5 P3 S6 109.72(4) . . ?
C2 C1 C6 121.8(2) . . ?
C2 C1 P1 127.6(2) . . ?
C6 C1 P1 110.22(19) . . ?
C1 C2 C3 120.3(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 117.5(3) . . ?
C2 C3 C13 121.6(3) . . ?
C4 C3 C13 120.7(3) . . ?
C5 C4 C3 122.6(3) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 118.4(3) . . ?
C5 C6 C7 128.0(3) . . ?
C1 C6 C7 113.4(2) . . ?
C8 C7 C12 118.9(3) . . ?
C8 C7 C6 127.5(3) . . ?
C12 C7 C6 113.4(2) . . ?
C7 C8 C9 118.6(3) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C10 C9 C8 122.6(3) . . ?
C10 C9 H9 118.7 . . ?
C8 C9 H9 118.7 . . ?
C9 C10 C11 118.1(3) . . ?
C9 C10 C17 121.8(3) . . ?
C11 C10 C17 120.1(3) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C7 122.1(2) . . ?
C11 C12 P1 127.4(2) . . ?
C7 C12 P1 110.2(2) . . ?
C14 C13 C3 112.9(2) . . ?
C14 C13 C15 108.5(3) . . ?
C3 C13 C15 110.9(3) . . ?
C14 C13 C16 109.6(3) . . ?
C3 C13 C16 106.2(3) . . ?
C15 C13 C16 108.7(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C20 119.2(10) . . ?
C18 C17 C20' 128.4(6) . . ?
C20 C17 C20' 44.7(8) . . ?
C18 C17 C18' 51.8(7) . . ?
C20 C17 C18' 149.0(7) . . ?
C20' C17 C18' 113.1(4) . . ?
C18 C17 C10 114.9(5) . . ?
C20 C17 C10 101.8(7) . . ?
C20' C17 C10 116.4(4) . . ?
C18' C17 C10 108.7(3) . . ?
C18 C17 C19 110.1(9) . . ?
C20 C17 C19 103.9(10) . . ?
C20' C17 C19 59.5(8) . . ?
C18' C17 C19 62.6(7) . . ?
C10 C17 C19 105.6(6) . . ?
C18 C17 C19' 54.1(7) . . ?
C20 C17 C19' 69.5(8) . . ?
C20' C17 C19' 104.2(5) . . ?
C18' C17 C19' 105.3(4) . . ?
C10 C17 C19' 108.4(3) . . ?
C19 C17 C19' 146.0(6) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
C17 C18' H18D 109.5 . . ?
C17 C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
C17 C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
C17 C19' H19D 109.5 . . ?
C17 C19' H19E 109.5 . . ?
H19D C19' H19E 109.5 . . ?
C17 C19' H19F 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C17 C20' H20D 109.5 . . ?
C17 C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C17 C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C46 C41 C42 123.1(2) . . ?
C46 C41 P3 109.95(19) . . ?
C42 C41 P3 126.7(2) . . ?
C41 C42 C43 119.3(3) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C42 C43 C44 117.2(3) . . ?
C42 C43 C53 121.6(3) . . ?
C44 C43 C53 121.0(3) . . ?
C45 C44 C43 123.1(3) . . ?
C45 C44 H44 118.4 . . ?
C43 C44 H44 118.4 . . ?
C44 C45 C46 119.7(3) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C41 C46 C45 117.4(3) . . ?
C41 C46 C47 113.8(2) . . ?
C45 C46 C47 128.6(3) . . ?
C48 C47 C52 118.4(3) . . ?
C48 C47 C46 128.2(3) . . ?
C52 C47 C46 113.2(2) . . ?
C47 C48 C49 119.0(3) . . ?
C47 C48 H48 120.5 . . ?
C49 C48 H48 120.5 . . ?
C48 C49 C50 122.8(3) . . ?
C48 C49 H49 118.6 . . ?
C50 C49 H49 118.6 . . ?
C51 C50 C49 117.6(3) . . ?
C51 C50 C57 121.2(3) . . ?
C49 C50 C57 121.1(3) . . ?
C50 C51 C52 119.9(3) . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C51 C52 C47 122.3(2) . . ?
C51 C52 P3 127.2(2) . . ?
C47 C52 P3 110.41(19) . . ?
C43 C53 C55 110.8(3) . . ?
C43 C53 C54 107.4(3) . . ?
C55 C53 C54 107.9(4) . . ?
C43 C53 C56 112.2(3) . . ?
C55 C53 C56 108.7(3) . . ?
C54 C53 C56 109.7(4) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C60 C57 C58 109.1(3) . . ?
C60 C57 C59 108.2(3) . . ?
C58 C57 C59 108.5(3) . . ?
C60 C57 C50 112.2(3) . . ?
C58 C57 C50 111.3(3) . . ?
C59 C57 C50 107.4(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         3.837
_refine_diff_density_min         -3.013
_refine_diff_density_rms         0.179
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# 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_apx2068
_database_code_depnum_ccdc_archive 'CCDC 1404568'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-08-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C87 H104 P4 S8 U'
_chemical_formula_weight         1768.09

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'
P P 0.1023 0.0942 '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'
U U -9.6767 9.6646 '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'

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

_cell_length_a                   17.760(3)
_cell_length_b                   19.279(4)
_cell_length_c                   25.446(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8713(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3624
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5622
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            96181
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.83
_reflns_number_total             18631
_reflns_number_gt                15063
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0115P)²+0.0000P] 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'
_refine_ls_abs_structure_Flack   -0.009(2)
_refine_ls_number_reflns         18631
_refine_ls_number_parameters     926
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0451
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_restrained_S_all      0.831
_refine_ls_shift/su_max          0.004
_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
U1 U 0.757694(6) 0.749413(9) 0.808875(4) 0.01156(3) Uani 1 1 d . . .
S1 S 0.71992(5) 0.83074(5) 0.89872(4) 0.0174(2) Uani 1 1 d . . .
S2 S 0.88551(5) 0.82135(5) 0.84616(4) 0.0192(2) Uani 1 1 d . . .
S3 S 0.63721(5) 0.67302(5) 0.85518(4) 0.0147(2) Uani 1 1 d . . .
S4 S 0.81733(5) 0.64466(5) 0.87387(4) 0.0164(2) Uani 1 1 d . . .
S5 S 0.73603(5) 0.64151(5) 0.73496(4) 0.0160(2) Uani 1 1 d . . .
S6 S 0.89869(5) 0.71431(5) 0.76163(4) 0.0195(2) Uani 1 1 d . . .
S7 S 0.60933(5) 0.78795(5) 0.77591(4) 0.0165(2) Uani 1 1 d . . .
S8 S 0.76416(5) 0.84749(5) 0.72403(4) 0.0151(2) Uani 1 1 d . . .
P1 P 0.82869(5) 0.85445(5) 0.90888(4) 0.0154(2) Uani 1 1 d . . .
P2 P 0.71253(5) 0.61485(5) 0.89308(4) 0.0145(2) Uani 1 1 d . . .
P3 P 0.84492(5) 0.64840(5) 0.71447(4) 0.0161(2) Uani 1 1 d . . .
P4 P 0.65245(5) 0.83784(5) 0.71398(4) 0.0132(2) Uani 1 1 d . . .
C1 C 0.8470(2) 0.94440(18) 0.92380(15) 0.0182(9) Uani 1 1 d . . .
C2 C 0.83596(19) 1.00124(18) 0.89195(15) 0.0191(9) Uani 1 1 d . . .
H2 H 0.8169 0.9951 0.8582 0.023 Uiso 1 1 calc R . .
C3 C 0.8531(2) 1.06833(19) 0.90980(16) 0.0204(9) Uani 1 1 d . . .
C4 C 0.8804(2) 1.0736(2) 0.96093(16) 0.0271(10) Uani 1 1 d . . .
H4 H 0.8904 1.1176 0.9743 0.033 Uiso 1 1 calc R . .
C5 C 0.8933(2) 1.01691(19) 0.99267(16) 0.0272(10) Uani 1 1 d . . .
H5 H 0.9126 1.0229 1.0263 0.033 Uiso 1 1 calc R . .
C6 C 0.8773(2) 0.9507(2) 0.97405(15) 0.0225(10) Uani 1 1 d . . .
C7 C 0.8906(2) 0.8835(2) 1.00013(16) 0.0234(10) Uani 1 1 d . . .
C8 C 0.9269(3) 0.8722(2) 1.04702(18) 0.0396(13) Uani 1 1 d . . .
H8 H 0.9420 0.9095 1.0676 0.048 Uiso 1 1 calc R . .
C9 C 0.9409(3) 0.8047(2) 1.06356(18) 0.0343(13) Uani 1 1 d . . .
H9 H 0.9654 0.7979 1.0954 0.041 Uiso 1 1 calc R . .
C10 C 0.91959(17) 0.7464(3) 1.03423(13) 0.0232(8) Uani 1 1 d . . .
C11 C 0.88266(17) 0.7585(2) 0.98712(13) 0.0193(9) Uani 1 1 d . . .
H11 H 0.8666 0.7212 0.9668 0.023 Uiso 1 1 calc R . .
C12 C 0.86948(19) 0.8258(2) 0.96998(14) 0.0186(9) Uani 1 1 d . . .
C13 C 0.8424(2) 1.13096(19) 0.87335(16) 0.0236(10) Uani 1 1 d . . .
C14 C 0.8977(2) 1.1270(2) 0.82770(15) 0.0340(12) Uani 1 1 d . . .
H14A H 0.9482 1.1312 0.8408 0.051 Uiso 1 1 calc R . .
H14B H 0.8877 1.1639 0.8034 0.051 Uiso 1 1 calc R . .
H14C H 0.8921 1.0832 0.8101 0.051 Uiso 1 1 calc R . .
C15 C 0.7625(2) 1.12973(19) 0.85113(16) 0.0399(12) Uani 1 1 d . . .
H15A H 0.7557 1.1683 0.8277 0.060 Uiso 1 1 calc R . .
H15B H 0.7269 1.1329 0.8794 0.060 Uiso 1 1 calc R . .
H15C H 0.7546 1.0872 0.8323 0.060 Uiso 1 1 calc R . .
C16 C 0.8549(2) 1.19987(19) 0.90172(17) 0.0379(12) Uani 1 1 d . . .
H16A H 0.9055 1.2017 0.9149 0.057 Uiso 1 1 calc R . .
H16B H 0.8202 1.2037 0.9305 0.057 Uiso 1 1 calc R . .
H16C H 0.8469 1.2375 0.8776 0.057 Uiso 1 1 calc R . .
C17 C 0.9411(2) 0.6733(2) 1.05354(17) 0.0229(11) Uani 1 1 d . . .
C18 C 0.8995(3) 0.6182(2) 1.0225(2) 0.0602(19) Uani 1 1 d . . .
H18A H 0.9112 0.5732 1.0365 0.090 Uiso 1 1 calc R . .
H18B H 0.9146 0.6203 0.9863 0.090 Uiso 1 1 calc R . .
H18C H 0.8462 0.6261 1.0250 0.090 Uiso 1 1 calc R . .
C19 C 0.9205(3) 0.6650(3) 1.11120(18) 0.077(2) Uani 1 1 d . . .
H19A H 0.8681 0.6755 1.1160 0.116 Uiso 1 1 calc R . .
H19B H 0.9503 0.6962 1.1320 0.116 Uiso 1 1 calc R . .
H19C H 0.9300 0.6182 1.1220 0.116 Uiso 1 1 calc R . .
C20 C 1.0242(2) 0.6635(2) 1.0468(2) 0.0605(17) Uani 1 1 d . . .
H20A H 1.0380 0.6177 1.0582 0.091 Uiso 1 1 calc R . .
H20B H 1.0506 0.6972 1.0676 0.091 Uiso 1 1 calc R . .
H20C H 1.0373 0.6692 1.0105 0.091 Uiso 1 1 calc R . .
C21 C 0.69637(19) 0.61051(19) 0.96240(14) 0.0156(9) Uani 1 1 d . . .
C22 C 0.69159(18) 0.66557(19) 0.99706(14) 0.0183(9) Uani 1 1 d . . .
H22 H 0.6984 0.7107 0.9850 0.022 Uiso 1 1 calc R . .
C23 C 0.6764(2) 0.6535(2) 1.05022(15) 0.0205(9) Uani 1 1 d . . .
C24 C 0.6718(2) 0.5842(2) 1.06582(16) 0.0281(10) Uani 1 1 d . . .
H24 H 0.6654 0.5746 1.1014 0.034 Uiso 1 1 calc R . .
C25 C 0.6761(2) 0.5295(2) 1.03132(15) 0.0247(10) Uani 1 1 d . . .
H25 H 0.6716 0.4842 1.0436 0.030 Uiso 1 1 calc R . .
C26 C 0.6870(2) 0.54180(19) 0.97808(15) 0.0186(9) Uani 1 1 d . . .
C27 C 0.6859(2) 0.49176(18) 0.93381(15) 0.0193(9) Uani 1 1 d . . .
C28 C 0.6723(2) 0.42100(19) 0.93410(16) 0.0240(10) Uani 1 1 d . . .
H28 H 0.6659 0.3978 0.9658 0.029 Uiso 1 1 calc R . .
C29 C 0.6683(2) 0.3848(2) 0.88716(16) 0.0272(10) Uani 1 1 d . . .
H29 H 0.6582 0.3375 0.8884 0.033 Uiso 1 1 calc R . .
C30 C 0.67873(19) 0.41579(19) 0.83809(16) 0.0182(9) Uani 1 1 d . . .
C31 C 0.69444(18) 0.48674(18) 0.83848(15) 0.0178(9) Uani 1 1 d . . .
H31 H 0.7028 0.5097 0.8069 0.021 Uiso 1 1 calc R . .
C32 C 0.69778(19) 0.52317(18) 0.88479(15) 0.0163(9) Uani 1 1 d . . .
C33 C 0.6607(2) 0.7136(2) 1.08766(15) 0.0243(10) Uani 1 1 d . . .
C34 C 0.6937(2) 0.7819(2) 1.06797(16) 0.0362(12) Uani 1 1 d . . .
H34A H 0.6688 0.7952 1.0360 0.054 Uiso 1 1 calc R . .
H34B H 0.7465 0.7761 1.0614 0.054 Uiso 1 1 calc R . .
H34C H 0.6864 0.8172 1.0941 0.054 Uiso 1 1 calc R . .
C35 C 0.6919(2) 0.6999(2) 1.14267(15) 0.0451(13) Uani 1 1 d . . .
H35A H 0.6802 0.7385 1.1651 0.068 Uiso 1 1 calc R . .
H35B H 0.7455 0.6942 1.1407 0.068 Uiso 1 1 calc R . .
H35C H 0.6696 0.6585 1.1567 0.068 Uiso 1 1 calc R . .
C36 C 0.5747(2) 0.7206(2) 1.09175(18) 0.0428(13) Uani 1 1 d . . .
H36A H 0.5540 0.6790 1.1067 0.064 Uiso 1 1 calc R . .
H36B H 0.5539 0.7278 1.0574 0.064 Uiso 1 1 calc R . .
H36C H 0.5625 0.7594 1.1138 0.064 Uiso 1 1 calc R . .
C37 C 0.6711(2) 0.37517(18) 0.78683(16) 0.0201(9) Uani 1 1 d . . .
C38 C 0.5870(2) 0.3616(2) 0.77544(16) 0.0298(11) Uani 1 1 d . . .
H38A H 0.5649 0.3375 0.8046 0.045 Uiso 1 1 calc R . .
H38B H 0.5823 0.3339 0.7443 0.045 Uiso 1 1 calc R . .
H38C H 0.5615 0.4050 0.7704 0.045 Uiso 1 1 calc R . .
C39 C 0.7108(2) 0.30431(18) 0.79192(16) 0.0347(12) Uani 1 1 d . . .
H39A H 0.7624 0.3113 0.8018 0.052 Uiso 1 1 calc R . .
H39B H 0.7087 0.2804 0.7588 0.052 Uiso 1 1 calc R . .
H39C H 0.6859 0.2771 0.8183 0.052 Uiso 1 1 calc R . .
C40 C 0.7046(2) 0.41365(19) 0.73966(15) 0.0297(11) Uani 1 1 d . . .
H40A H 0.6779 0.4564 0.7344 0.045 Uiso 1 1 calc R . .
H40B H 0.7001 0.3853 0.7088 0.045 Uiso 1 1 calc R . .
H40C H 0.7568 0.4233 0.7462 0.045 Uiso 1 1 calc R . .
C41 C 0.89033(19) 0.56555(18) 0.70941(15) 0.0158(9) Uani 1 1 d . . .
C42 C 0.90134(19) 0.51769(19) 0.74945(15) 0.0188(9) Uani 1 1 d . . .
H42 H 0.8816 0.5260 0.7827 0.023 Uiso 1 1 calc R . .
C43 C 0.94178(19) 0.45737(19) 0.73984(16) 0.0177(9) Uani 1 1 d . . .
C44 C 0.96969(19) 0.44820(19) 0.68889(17) 0.0235(9) Uani 1 1 d . . .
H44 H 0.9970 0.4082 0.6816 0.028 Uiso 1 1 calc R . .
C45 C 0.9587(2) 0.4956(2) 0.64893(16) 0.0226(10) Uani 1 1 d . . .
H45 H 0.9782 0.4872 0.6156 0.027 Uiso 1 1 calc R . .
C46 C 0.9183(2) 0.55590(19) 0.65883(15) 0.0185(9) Uani 1 1 d . . .
C47 C 0.90279(19) 0.6140(2) 0.62287(15) 0.0190(9) Uani 1 1 d . . .
C48 C 0.9255(2) 0.6225(2) 0.57124(17) 0.0248(11) Uani 1 1 d . . .
H48 H 0.9526 0.5877 0.5544 0.030 Uiso 1 1 calc R . .
C49 C 0.9076(2) 0.6829(2) 0.54477(16) 0.0232(10) Uani 1 1 d . . .
H49 H 0.9230 0.6873 0.5100 0.028 Uiso 1 1 calc R . .
C50 C 0.86805(18) 0.73706(19) 0.56732(14) 0.0170(9) Uani 1 1 d . . .
C51 C 0.84576(18) 0.72822(19) 0.61964(14) 0.0177(9) Uani 1 1 d . . .
H51 H 0.8190 0.7633 0.6364 0.021 Uiso 1 1 calc R . .
C52 C 0.86268(19) 0.66861(19) 0.64660(14) 0.0153(8) Uani 1 1 d . . .
C53 C 0.9583(2) 0.4027(2) 0.78205(16) 0.0240(10) Uani 1 1 d . . .
C54 C 0.9178(2) 0.4177(2) 0.83364(15) 0.0293(11) Uani 1 1 d . . .
H54A H 0.9343 0.4616 0.8472 0.044 Uiso 1 1 calc R . .
H54B H 0.9291 0.3818 0.8586 0.044 Uiso 1 1 calc R . .
H54C H 0.8645 0.4191 0.8276 0.044 Uiso 1 1 calc R . .
C55 C 1.0441(2) 0.4017(2) 0.79215(16) 0.0333(12) Uani 1 1 d . . .
H55A H 1.0703 0.3972 0.7593 0.050 Uiso 1 1 calc R . .
H55B H 1.0565 0.3632 0.8144 0.050 Uiso 1 1 calc R . .
H55C H 1.0589 0.4441 0.8090 0.050 Uiso 1 1 calc R . .
C56 C 0.9330(2) 0.33114(19) 0.76261(16) 0.0289(11) Uani 1 1 d . . .
H56A H 0.8800 0.3321 0.7552 0.043 Uiso 1 1 calc R . .
H56B H 0.9430 0.2971 0.7892 0.043 Uiso 1 1 calc R . .
H56C H 0.9602 0.3194 0.7312 0.043 Uiso 1 1 calc R . .
C57 C 0.8533(2) 0.8052(2) 0.53820(15) 0.0214(9) Uani 1 1 d . . .
C58 C 0.8540(2) 0.7955(2) 0.47829(14) 0.0304(11) Uani 1 1 d . . .
H58A H 0.9022 0.7782 0.4675 0.046 Uiso 1 1 calc R . .
H58B H 0.8446 0.8392 0.4615 0.046 Uiso 1 1 calc R . .
H58C H 0.8155 0.7630 0.4684 0.046 Uiso 1 1 calc R . .
C59 C 0.9163(2) 0.8564(2) 0.55358(17) 0.0324(12) Uani 1 1 d . . .
H59A H 0.9125 0.8671 0.5903 0.049 Uiso 1 1 calc R . .
H59B H 0.9112 0.8982 0.5334 0.049 Uiso 1 1 calc R . .
H59C H 0.9644 0.8357 0.5466 0.049 Uiso 1 1 calc R . .
C60 C 0.7770(2) 0.8371(2) 0.55334(15) 0.0356(11) Uani 1 1 d . . .
H60A H 0.7375 0.8044 0.5462 0.053 Uiso 1 1 calc R . .
H60B H 0.7687 0.8785 0.5332 0.053 Uiso 1 1 calc R . .
H60C H 0.7770 0.8483 0.5901 0.053 Uiso 1 1 calc R . .
C61 C 0.60358(18) 0.91766(17) 0.70063(14) 0.0130(8) Uani 1 1 d . . .
C62 C 0.59504(19) 0.97405(18) 0.73359(15) 0.0175(9) Uani 1 1 d . . .
H62 H 0.6201 0.9750 0.7657 0.021 Uiso 1 1 calc R . .
C63 C 0.54964(19) 1.02900(18) 0.71940(15) 0.0139(8) Uani 1 1 d . . .
C64 C 0.51264(19) 1.02523(19) 0.67103(14) 0.0173(9) Uani 1 1 d . . .
H64 H 0.4817 1.0618 0.6610 0.021 Uiso 1 1 calc R . .
C65 C 0.52020(19) 0.96932(18) 0.63760(15) 0.0158(9) Uani 1 1 d . . .
H65 H 0.4950 0.9686 0.6056 0.019 Uiso 1 1 calc R . .
C66 C 0.56611(18) 0.91377(18) 0.65228(14) 0.0131(8) Uani 1 1 d . . .
C67 C 0.57853(18) 0.84772(18) 0.62415(14) 0.0130(8) Uani 1 1 d . . .
C68 C 0.54938(19) 0.82737(19) 0.57620(14) 0.0170(9) Uani 1 1 d . . .
H68 H 0.5187 0.8575 0.5574 0.020 Uiso 1 1 calc R . .
C69 C 0.56552(18) 0.76255(19) 0.55601(14) 0.0177(9) Uani 1 1 d . . .
H69 H 0.5458 0.7503 0.5235 0.021 Uiso 1 1 calc R . .
C70 C 0.61036(19) 0.71486(18) 0.58268(15) 0.0171(9) Uani 1 1 d . . .
C71 C 0.63999(18) 0.73556(19) 0.63149(14) 0.0157(9) Uani 1 1 d . . .
H71 H 0.6704 0.7053 0.6504 0.019 Uiso 1 1 calc R . .
C72 C 0.62410(19) 0.80075(18) 0.65153(14) 0.0134(8) Uani 1 1 d . . .
C73 C 0.5373(2) 1.0922(2) 0.75454(16) 0.0230(10) Uani 1 1 d . . .
C74 C 0.5838(2) 1.0894(2) 0.80469(18) 0.0469(14) Uani 1 1 d . . .
H74A H 0.5705 1.0487 0.8244 0.070 Uiso 1 1 calc R . .
H74B H 0.5741 1.1300 0.8254 0.070 Uiso 1 1 calc R . .
H74C H 0.6364 1.0876 0.7959 0.070 Uiso 1 1 calc R . .
C75 C 0.4537(2) 1.0955(2) 0.77037(15) 0.0261(10) Uani 1 1 d . . .
H75A H 0.4419 1.0570 0.7928 0.039 Uiso 1 1 calc R . .
H75B H 0.4229 1.0936 0.7394 0.039 Uiso 1 1 calc R . .
H75C H 0.4442 1.1381 0.7888 0.039 Uiso 1 1 calc R . .
C76 C 0.5584(2) 1.15837(19) 0.72423(17) 0.0371(12) Uani 1 1 d . . .
H76A H 0.5508 1.1981 0.7464 0.056 Uiso 1 1 calc R . .
H76B H 0.5273 1.1623 0.6935 0.056 Uiso 1 1 calc R . .
H76C H 0.6103 1.1560 0.7139 0.056 Uiso 1 1 calc R . .
C77 C 0.6233(2) 0.64231(19) 0.55999(15) 0.0191(9) Uani 1 1 d . . .
C78 C 0.6830(2) 0.6013(2) 0.59071(17) 0.0380(12) Uani 1 1 d . . .
H78A H 0.6658 0.5939 0.6260 0.057 Uiso 1 1 calc R . .
H78B H 0.7293 0.6271 0.5913 0.057 Uiso 1 1 calc R . .
H78C H 0.6913 0.5574 0.5739 0.057 Uiso 1 1 calc R . .
C79 C 0.6507(2) 0.6478(2) 0.50248(16) 0.0362(12) Uani 1 1 d . . .
H79A H 0.6959 0.6750 0.5012 0.054 Uiso 1 1 calc R . .
H79B H 0.6125 0.6696 0.4815 0.054 Uiso 1 1 calc R . .
H79C H 0.6606 0.6022 0.4890 0.054 Uiso 1 1 calc R . .
C80 C 0.5500(2) 0.60186(19) 0.56161(16) 0.0269(11) Uani 1 1 d . . .
H80A H 0.5573 0.5571 0.5460 0.040 Uiso 1 1 calc R . .
H80B H 0.5120 0.6266 0.5424 0.040 Uiso 1 1 calc R . .
H80C H 0.5342 0.5963 0.5975 0.040 Uiso 1 1 calc R . .
C81 C 0.6810(3) 0.9515(3) 0.1361(2) 0.0507(15) Uani 1 1 d . . .
C82 C 0.6509(3) 0.9188(3) 0.1800(2) 0.0599(16) Uani 1 1 d . . .
H82 H 0.6811 0.9116 0.2094 0.072 Uiso 1 1 calc R . .
C83 C 0.5773(3) 0.8972(3) 0.1807(2) 0.0693(18) Uani 1 1 d . . .
H83 H 0.5586 0.8741 0.2100 0.083 Uiso 1 1 calc R . .
C84 C 0.5310(3) 0.9094(3) 0.1382(3) 0.0679(19) Uani 1 1 d . . .
H84 H 0.4809 0.8953 0.1386 0.082 Uiso 1 1 calc R . .
C85 C 0.5609(4) 0.9436(3) 0.0941(3) 0.0671(18) Uani 1 1 d . . .
H85 H 0.5304 0.9533 0.0653 0.080 Uiso 1 1 calc R . .
C86 C 0.6343(3) 0.9624(3) 0.0936(2) 0.0607(16) Uani 1 1 d . . .
H86 H 0.6539 0.9833 0.0636 0.073 Uiso 1 1 calc R . .
C87 C 0.7600(3) 0.9724(3) 0.1338(2) 0.093(2) Uani 1 1 d . . .
H87A H 0.7652 1.0188 0.1469 0.140 Uiso 1 1 calc R . .
H87B H 0.7772 0.9705 0.0980 0.140 Uiso 1 1 calc R . .
H87C H 0.7897 0.9414 0.1549 0.140 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
U1 S4 2.8170(10) . ?
U1 S2 2.8243(10) . ?
U1 S5 2.8307(10) . ?
U1 S1 2.8522(10) . ?
U1 S3 2.8524(10) . ?
U1 S6 2.8589(10) . ?
U1 S7 2.8634(10) . ?
U1 S8 2.8722(10) . ?
S1 P1 2.0019(14) . ?
S2 P1 1.9931(14) . ?
S3 P2 1.9943(13) . ?
S4 P2 2.0083(13) . ?
S5 P3 2.0072(14) . ?
S6 P3 1.9916(14) . ?
S7 P4 1.9987(14) . ?
S8 P4 2.0089(14) . ?
P1 C12 1.802(4) . ?
P1 C1 1.805(4) . ?
P2 C21 1.789(4) . ?
P2 C32 1.799(4) . ?
P3 C41 1.794(4) . ?
P3 C52 1.798(4) . ?
P4 C61 1.799(3) . ?
P4 C72 1.814(4) . ?
C1 C2 1.377(5) . ?
C1 C6 1.393(5) . ?
C2 C3 1.404(5) . ?
C3 C4 1.392(5) . ?
C3 C13 1.534(5) . ?
C4 C5 1.379(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.474(5) . ?
C7 C8 1.373(5) . ?
C7 C12 1.402(5) . ?
C8 C9 1.390(6) . ?
C9 C10 1.400(6) . ?
C10 C11 1.386(4) . ?
C10 C17 1.541(6) . ?
C11 C12 1.390(5) . ?
C13 C14 1.523(5) . ?
C13 C15 1.527(5) . ?
C13 C16 1.528(5) . ?
C17 C20 1.498(5) . ?
C17 C18 1.517(6) . ?
C17 C19 1.521(6) . ?
C21 C22 1.383(5) . ?
C21 C26 1.393(5) . ?
C22 C23 1.399(5) . ?
C23 C24 1.396(5) . ?
C23 C33 1.526(5) . ?
C24 C25 1.375(5) . ?
C25 C26 1.389(5) . ?
C26 C27 1.483(5) . ?
C27 C28 1.385(5) . ?
C27 C32 1.403(5) . ?
C28 C29 1.385(5) . ?
C29 C30 1.396(5) . ?
C30 C31 1.396(5) . ?
C30 C37 1.528(5) . ?
C31 C32 1.373(5) . ?
C33 C34 1.525(5) . ?
C33 C35 1.529(5) . ?
C33 C36 1.536(5) . ?
C37 C40 1.532(5) . ?
C37 C38 1.543(5) . ?
C37 C39 1.543(5) . ?
C41 C42 1.388(5) . ?
C41 C46 1.392(5) . ?
C42 C43 1.388(5) . ?
C43 C44 1.399(5) . ?
C43 C53 1.534(5) . ?
C44 C45 1.381(5) . ?
C45 C46 1.390(5) . ?
C46 C47 1.472(5) . ?
C47 C48 1.384(5) . ?
C47 C52 1.407(5) . ?
C48 C49 1.382(5) . ?
C49 C50 1.383(5) . ?
C50 C51 1.399(5) . ?
C50 C57 1.532(5) . ?
C51 C52 1.372(5) . ?
C53 C54 1.525(5) . ?
C53 C56 1.532(5) . ?
C53 C55 1.545(5) . ?
C57 C58 1.536(5) . ?
C57 C60 1.537(5) . ?
C57 C59 1.542(5) . ?
C61 C62 1.381(5) . ?
C61 C66 1.401(5) . ?
C62 C63 1.379(5) . ?
C63 C64 1.397(5) . ?
C63 C73 1.527(5) . ?
C64 C65 1.380(5) . ?
C65 C66 1.397(4) . ?
C66 C67 1.477(5) . ?
C67 C68 1.382(5) . ?
C67 C72 1.400(4) . ?
C68 C69 1.381(5) . ?
C69 C70 1.393(5) . ?
C70 C71 1.407(5) . ?
C70 C77 1.531(5) . ?
C71 C72 1.385(5) . ?
C73 C74 1.522(5) . ?
C73 C76 1.537(5) . ?
C73 C75 1.539(5) . ?
C77 C80 1.519(5) . ?
C77 C78 1.536(5) . ?
C77 C79 1.545(5) . ?
C81 C86 1.379(7) . ?
C81 C82 1.389(7) . ?
C81 C87 1.462(6) . ?
C82 C83 1.372(6) . ?
C83 C84 1.380(7) . ?
C84 C85 1.405(7) . ?
C85 C86 1.352(7) . ?

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
S4 U1 S2 81.52(3) . . ?
S4 U1 S5 85.09(3) . . ?
S2 U1 S5 133.89(3) . . ?
S4 U1 S1 90.68(3) . . ?
S2 U1 S1 69.51(3) . . ?
S5 U1 S1 154.77(3) . . ?
S4 U1 S3 70.70(3) . . ?
S2 U1 S3 135.87(3) . . ?
S5 U1 S3 78.06(3) . . ?
S1 U1 S3 77.07(3) . . ?
S4 U1 S6 75.39(3) . . ?
S2 U1 S6 63.48(3) . . ?
S5 U1 S6 70.47(3) . . ?
S1 U1 S6 132.31(3) . . ?
S3 U1 S6 135.12(3) . . ?
S4 U1 S7 134.75(3) . . ?
S2 U1 S7 135.29(3) . . ?
S5 U1 S7 82.58(3) . . ?
S1 U1 S7 82.86(3) . . ?
S3 U1 S7 64.19(3) . . ?
S6 U1 S7 138.09(3) . . ?
S4 U1 S8 153.93(3) . . ?
S2 U1 S8 84.10(3) . . ?
S5 U1 S8 89.41(3) . . ?
S1 U1 S8 104.48(3) . . ?
S3 U1 S8 132.87(3) . . ?
S6 U1 S8 78.74(3) . . ?
S7 U1 S8 69.25(3) . . ?
P1 S1 U1 90.11(4) . . ?
P1 S2 U1 91.10(4) . . ?
P2 S3 U1 89.25(4) . . ?
P2 S4 U1 89.97(4) . . ?
P3 S5 U1 89.60(4) . . ?
P3 S6 U1 89.11(4) . . ?
P4 S7 U1 90.18(4) . . ?
P4 S8 U1 89.73(4) . . ?
C12 P1 C1 92.30(18) . . ?
C12 P1 S2 112.91(13) . . ?
C1 P1 S2 112.62(13) . . ?
C12 P1 S1 115.43(13) . . ?
C1 P1 S1 114.89(13) . . ?
S2 P1 S1 108.19(6) . . ?
C21 P2 C32 92.65(18) . . ?
C21 P2 S3 113.30(12) . . ?
C32 P2 S3 113.45(12) . . ?
C21 P2 S4 113.70(12) . . ?
C32 P2 S4 112.80(12) . . ?
S3 P2 S4 110.07(6) . . ?
C41 P3 C52 92.58(17) . . ?
C41 P3 S6 113.31(13) . . ?
C52 P3 S6 110.88(13) . . ?
C41 P3 S5 113.13(12) . . ?
C52 P3 S5 115.64(12) . . ?
S6 P3 S5 110.35(6) . . ?
C61 P4 C72 92.17(16) . . ?
C61 P4 S7 112.07(12) . . ?
C72 P4 S7 113.24(12) . . ?
C61 P4 S8 114.92(12) . . ?
C72 P4 S8 114.96(12) . . ?
S7 P4 S8 108.82(6) . . ?
C2 C1 C6 121.7(4) . . ?
C2 C1 P1 128.0(3) . . ?
C6 C1 P1 110.3(3) . . ?
C1 C2 C3 120.8(4) . . ?
C4 C3 C2 116.4(4) . . ?
C4 C3 C13 123.4(3) . . ?
C2 C3 C13 120.2(3) . . ?
C5 C4 C3 123.2(4) . . ?
C4 C5 C6 119.6(4) . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C7 128.3(4) . . ?
C1 C6 C7 113.5(3) . . ?
C8 C7 C12 118.3(4) . . ?
C8 C7 C6 127.3(4) . . ?
C12 C7 C6 114.1(3) . . ?
C7 C8 C9 119.7(4) . . ?
C8 C9 C10 122.7(4) . . ?
C11 C10 C9 117.0(4) . . ?
C11 C10 C17 123.1(4) . . ?
C9 C10 C17 119.8(3) . . ?
C10 C11 C12 120.5(4) . . ?
C11 C12 C7 121.6(3) . . ?
C11 C12 P1 128.7(3) . . ?
C7 C12 P1 109.7(3) . . ?
C14 C13 C15 108.4(3) . . ?
C14 C13 C16 108.1(3) . . ?
C15 C13 C16 108.9(3) . . ?
C14 C13 C3 109.9(3) . . ?
C15 C13 C3 109.1(3) . . ?
C16 C13 C3 112.4(3) . . ?
C20 C17 C18 109.4(4) . . ?
C20 C17 C19 109.5(4) . . ?
C18 C17 C19 108.2(4) . . ?
C20 C17 C10 108.9(3) . . ?
C18 C17 C10 110.7(3) . . ?
C19 C17 C10 110.1(4) . . ?
C22 C21 C26 122.7(3) . . ?
C22 C21 P2 127.1(3) . . ?
C26 C21 P2 110.2(3) . . ?
C21 C22 C23 120.0(4) . . ?
C24 C23 C22 116.5(4) . . ?
C24 C23 C33 122.6(4) . . ?
C22 C23 C33 120.8(4) . . ?
C25 C24 C23 123.3(4) . . ?
C24 C25 C26 120.0(4) . . ?
C25 C26 C21 117.3(4) . . ?
C25 C26 C27 128.9(4) . . ?
C21 C26 C27 113.7(3) . . ?
C28 C27 C32 117.1(4) . . ?
C28 C27 C26 129.7(4) . . ?
C32 C27 C26 113.1(3) . . ?
C29 C28 C27 120.0(4) . . ?
C28 C29 C30 123.3(4) . . ?
C31 C30 C29 116.1(4) . . ?
C31 C30 C37 121.8(3) . . ?
C29 C30 C37 122.2(3) . . ?
C32 C31 C30 121.1(4) . . ?
C31 C32 C27 122.4(3) . . ?
C31 C32 P2 127.5(3) . . ?
C27 C32 P2 110.0(3) . . ?
C34 C33 C23 112.3(3) . . ?
C34 C33 C35 108.1(4) . . ?
C23 C33 C35 112.0(3) . . ?
C34 C33 C36 109.1(3) . . ?
C23 C33 C36 107.0(3) . . ?
C35 C33 C36 108.3(3) . . ?
C30 C37 C40 112.7(3) . . ?
C30 C37 C38 109.5(3) . . ?
C40 C37 C38 108.1(3) . . ?
C30 C37 C39 110.0(3) . . ?
C40 C37 C39 108.5(3) . . ?
C38 C37 C39 107.9(3) . . ?
C42 C41 C46 122.6(3) . . ?
C42 C41 P3 127.0(3) . . ?
C46 C41 P3 110.2(3) . . ?
C43 C42 C41 120.0(4) . . ?
C42 C43 C44 116.9(4) . . ?
C42 C43 C53 123.5(4) . . ?
C44 C43 C53 119.6(3) . . ?
C45 C44 C43 123.3(4) . . ?
C44 C45 C46 119.5(4) . . ?
C45 C46 C41 117.6(4) . . ?
C45 C46 C47 128.4(4) . . ?
C41 C46 C47 114.0(3) . . ?
C48 C47 C52 117.8(4) . . ?
C48 C47 C46 128.7(4) . . ?
C52 C47 C46 113.4(3) . . ?
C49 C48 C47 119.7(4) . . ?
C48 C49 C50 123.4(4) . . ?
C49 C50 C51 116.5(4) . . ?
C49 C50 C57 122.3(3) . . ?
C51 C50 C57 121.1(3) . . ?
C52 C51 C50 121.0(3) . . ?
C51 C52 C47 121.5(3) . . ?
C51 C52 P3 128.6(3) . . ?
C47 C52 P3 109.8(3) . . ?
C54 C53 C56 108.1(3) . . ?
C54 C53 C43 112.4(3) . . ?
C56 C53 C43 109.7(3) . . ?
C54 C53 C55 108.9(3) . . ?
C56 C53 C55 109.4(3) . . ?
C43 C53 C55 108.3(3) . . ?
C50 C57 C58 111.9(3) . . ?
C50 C57 C60 111.9(3) . . ?
C58 C57 C60 107.7(3) . . ?
C50 C57 C59 107.6(3) . . ?
C58 C57 C59 108.9(3) . . ?
C60 C57 C59 108.7(3) . . ?
C62 C61 C66 121.6(3) . . ?
C62 C61 P4 127.7(3) . . ?
C66 C61 P4 110.4(3) . . ?
C63 C62 C61 120.6(3) . . ?
C62 C63 C64 117.7(3) . . ?
C62 C63 C73 122.9(3) . . ?
C64 C63 C73 119.3(3) . . ?
C65 C64 C63 122.6(3) . . ?
C64 C65 C66 119.4(3) . . ?
C65 C66 C61 118.1(3) . . ?
C65 C66 C67 128.2(3) . . ?
C61 C66 C67 113.6(3) . . ?
C68 C67 C72 118.2(3) . . ?
C68 C67 C66 128.1(3) . . ?
C72 C67 C66 113.7(3) . . ?
C69 C68 C67 120.5(4) . . ?
C68 C69 C70 122.3(3) . . ?
C69 C70 C71 117.2(3) . . ?
C69 C70 C77 120.4(3) . . ?
C71 C70 C77 122.4(3) . . ?
C72 C71 C70 120.4(3) . . ?
C71 C72 C67 121.4(3) . . ?
C71 C72 P4 128.6(3) . . ?
C67 C72 P4 110.0(3) . . ?
C74 C73 C63 112.6(3) . . ?
C74 C73 C76 108.5(3) . . ?
C63 C73 C76 109.5(3) . . ?
C74 C73 C75 107.8(3) . . ?
C63 C73 C75 109.0(3) . . ?
C76 C73 C75 109.4(3) . . ?
C80 C77 C70 109.3(3) . . ?
C80 C77 C78 108.3(3) . . ?
C70 C77 C78 112.4(3) . . ?
C80 C77 C79 109.3(3) . . ?
C70 C77 C79 110.0(3) . . ?
C78 C77 C79 107.5(3) . . ?
C86 C81 C82 117.9(5) . . ?
C86 C81 C87 120.2(6) . . ?
C82 C81 C87 121.8(6) . . ?
C83 C82 C81 121.0(6) . . ?
C82 C83 C84 120.4(6) . . ?
C83 C84 C85 118.7(6) . . ?
C86 C85 C84 119.8(6) . . ?
C85 C86 C81 122.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.078
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

