# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1515542'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.1646(3)
_cell_length_b                   12.5454(5)
_cell_length_c                   17.8461(3)
_cell_angle_alpha                87.399(2)
_cell_angle_beta                 77.495(2)
_cell_angle_gamma                75.600(3)
_cell_volume                     1940.14(3)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn 0.0259 5.4591 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -5.4734 5.5774 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C40 H70 Br2 O4 P4 Sn2 W2 
# Dc =      2.57 Fooo =    904.00 Mu =    251.30 M =   1503.78
# Found Formula = C36 H66 O2 P2 Sn1 W1 
# Dc =      1.53 FOOO =    904.00 Mu =    114.99 M =    895.41

_chemical_formula_sum            'C36 H66 O2 P2 Sn1 W1'
_chemical_formula_moiety         'C36 H66 O2 P2 Sn1 W1'
_chemical_compound_source        ?
_chemical_formula_weight         895.41


_cell_measurement_reflns_used    17223
_cell_measurement_theta_min      4
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.032
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_max          0.172

_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    11.499

# Sheldrick geometric approximatio 0.54 0.69 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_T_max  0.69
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            36372
_reflns_number_total             7638
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7638 
# Theoretical number of reflections is about 15363 


_diffrn_reflns_theta_min         4.455
_diffrn_reflns_theta_max         72.407
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        69.642
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -10
_reflns_limit_h_max              11
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   1.98
_oxford_diffrn_Wilson_scale      0.16

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.73
_refine_diff_density_max         2.12


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7638
_refine_ls_number_restraints     0
_refine_ls_number_parameters     379
_oxford_refine_ls_R_factor_ref   0.0347
_refine_ls_wR_factor_ref         0.0838
_refine_ls_goodness_of_fit_ref   1.0077
_refine_ls_shift/su_max          0.0009902
_refine_ls_shift/su_mean         0.0000256


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7638
_refine_ls_R_factor_all          0.0347
_refine_ls_wR_factor_all         0.0838

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7119
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_gt          0.0808

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 2.15P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.827047(16) 0.192198(12) 0.233290(8) 0.0231 1.0000 Uani . . . . . .
Sn1 Sn 0.71559(3) 0.013428(19) 0.319899(13) 0.0270 1.0000 Uani . . . . . .
P2 P 1.10721(10) 0.08180(7) 0.20830(5) 0.0241 1.0000 Uani . . . . . .
P3 P 0.90974(10) 0.23985(7) 0.35173(5) 0.0242 1.0000 Uani . . . . . .
O1 O 0.7543(4) 0.0880(3) 0.09220(19) 0.0492 1.0000 Uani . . . . . .
O2 O 0.4685(3) 0.2916(3) 0.2820(2) 0.0452 1.0000 Uani . . . . . .
C1 C 0.8318(4) 0.3136(3) 0.1724(2) 0.0301 1.0000 Uani . . . . . .
C2 C 0.7942(5) 0.4082(3) 0.1207(2) 0.0356 1.0000 Uani . . . . . .
C3 C 0.9015(8) 0.4851(5) 0.1183(4) 0.0627 1.0000 Uani . . . . . .
C4 C 0.8149(7) 0.3641(4) 0.0389(3) 0.0546 1.0000 Uani . . . . . .
C5 C 0.6250(7) 0.4711(5) 0.1475(4) 0.0660 1.0000 Uani . . . . . .
C6 C 0.7825(4) 0.1226(3) 0.1446(2) 0.0321 1.0000 Uani . . . . . .
C7 C 0.5990(5) 0.2563(3) 0.2675(2) 0.0336 1.0000 Uani . . . . . .
C11 C 0.6592(5) -0.1015(4) 0.2494(2) 0.0413 1.0000 Uani . . . . . .
C12 C 0.4929(4) 0.0645(3) 0.4003(2) 0.0338 1.0000 Uani . . . . . .
C13 C 0.8427(5) -0.1034(3) 0.3927(2) 0.0342 1.0000 Uani . . . . . .
C201 C 1.1944(4) 0.0999(3) 0.2904(2) 0.0299 1.0000 Uani . . . . . .
C211 C 1.2476(4) 0.1187(3) 0.1254(2) 0.0320 1.0000 Uani . . . . . .
C212 C 1.2570(6) 0.2390(4) 0.1318(3) 0.0429 1.0000 Uani . . . . . .
C213 C 1.3694(6) 0.2713(5) 0.0622(3) 0.0554 1.0000 Uani . . . . . .
C214 C 1.3272(6) 0.2506(4) -0.0128(3) 0.0492 1.0000 Uani . . . . . .
C215 C 1.3187(8) 0.1329(5) -0.0191(3) 0.0628 1.0000 Uani . . . . . .
C216 C 1.2062(7) 0.0996(4) 0.0496(2) 0.0487 1.0000 Uani . . . . . .
C221 C 1.1439(4) -0.0709(3) 0.2042(2) 0.0269 1.0000 Uani . . . . . .
C222 C 1.0592(5) -0.1157(3) 0.1525(2) 0.0332 1.0000 Uani . . . . . .
C223 C 1.0786(5) -0.2403(3) 0.1651(3) 0.0399 1.0000 Uani . . . . . .
C224 C 1.2471(6) -0.3029(3) 0.1508(3) 0.0422 1.0000 Uani . . . . . .
C225 C 1.3342(5) -0.2556(3) 0.1997(2) 0.0402 1.0000 Uani . . . . . .
C226 C 1.3151(4) -0.1323(3) 0.1866(2) 0.0343 1.0000 Uani . . . . . .
C301 C 1.0722(4) 0.1252(3) 0.36537(19) 0.0279 1.0000 Uani . . . . . .
C311 C 0.9949(4) 0.3618(3) 0.3368(2) 0.0293 1.0000 Uani . . . . . .
C312 C 0.8675(5) 0.4680(3) 0.3378(2) 0.0333 1.0000 Uani . . . . . .
C313 C 0.9356(6) 0.5680(4) 0.3190(3) 0.0428 1.0000 Uani . . . . . .
C314 C 1.0354(6) 0.5790(4) 0.3741(3) 0.0445 1.0000 Uani . . . . . .
C315 C 1.1632(6) 0.4739(4) 0.3741(3) 0.0464 1.0000 Uani . . . . . .
C316 C 1.0994(5) 0.3717(4) 0.3908(3) 0.0393 1.0000 Uani . . . . . .
C321 C 0.7828(5) 0.2676(3) 0.4489(2) 0.0341 1.0000 Uani . . . . . .
C322 C 0.6152(5) 0.3212(3) 0.4457(2) 0.0358 1.0000 Uani . . . . . .
C323 C 0.5168(6) 0.3558(4) 0.5253(3) 0.0476 1.0000 Uani . . . . . .
C324 C 0.5270(6) 0.2611(4) 0.5813(3) 0.0482 1.0000 Uani . . . . . .
C325 C 0.6945(6) 0.2041(4) 0.5833(2) 0.0410 1.0000 Uani . . . . . .
C326 C 0.7910(5) 0.1690(4) 0.5026(2) 0.0372 1.0000 Uani . . . . . .
H31 H 0.8775 0.5452 0.0847 0.0734 1.0000 Uiso . . . . . .
H32 H 0.8935 0.5134 0.1681 0.0734 1.0000 Uiso . . . . . .
H33 H 1.0076 0.4461 0.0995 0.0734 1.0000 Uiso . . . . . .
H41 H 0.7906 0.4253 0.0059 0.0667 1.0000 Uiso . . . . . .
H42 H 0.9177 0.3243 0.0211 0.0667 1.0000 Uiso . . . . . .
H43 H 0.7465 0.3184 0.0392 0.0667 1.0000 Uiso . . . . . .
H51 H 0.5988 0.5315 0.1153 0.0790 1.0000 Uiso . . . . . .
H52 H 0.6062 0.4971 0.1993 0.0790 1.0000 Uiso . . . . . .
H53 H 0.5580 0.4228 0.1467 0.0790 1.0000 Uiso . . . . . .
H111 H 0.6238 -0.1580 0.2803 0.0522 1.0000 Uiso . . . . . .
H112 H 0.7482 -0.1357 0.2115 0.0522 1.0000 Uiso . . . . . .
H113 H 0.5802 -0.0642 0.2234 0.0522 1.0000 Uiso . . . . . .
H121 H 0.4653 0.0024 0.4260 0.0414 1.0000 Uiso . . . . . .
H122 H 0.4997 0.1149 0.4373 0.0414 1.0000 Uiso . . . . . .
H123 H 0.4157 0.1004 0.3732 0.0414 1.0000 Uiso . . . . . .
H131 H 0.7832 -0.1541 0.4152 0.0409 1.0000 Uiso . . . . . .
H132 H 0.8621 -0.0650 0.4330 0.0409 1.0000 Uiso . . . . . .
H133 H 0.9381 -0.1436 0.3631 0.0409 1.0000 Uiso . . . . . .
H2011 H 1.2441 0.1591 0.2799 0.0357 1.0000 Uiso . . . . . .
H2012 H 1.2704 0.0340 0.2965 0.0357 1.0000 Uiso . . . . . .
H2111 H 1.3481 0.0720 0.1259 0.0389 1.0000 Uiso . . . . . .
H2121 H 1.2895 0.2482 0.1782 0.0535 1.0000 Uiso . . . . . .
H2122 H 1.1568 0.2863 0.1345 0.0535 1.0000 Uiso . . . . . .
H2131 H 1.4723 0.2263 0.0620 0.0661 1.0000 Uiso . . . . . .
H2132 H 1.3710 0.3459 0.0664 0.0661 1.0000 Uiso . . . . . .
H2141 H 1.3999 0.2683 -0.0553 0.0583 1.0000 Uiso . . . . . .
H2142 H 1.2274 0.2987 -0.0142 0.0583 1.0000 Uiso . . . . . .
H2151 H 1.4191 0.0859 -0.0213 0.0763 1.0000 Uiso . . . . . .
H2152 H 1.2873 0.1231 -0.0657 0.0763 1.0000 Uiso . . . . . .
H2161 H 1.2062 0.0240 0.0451 0.0606 1.0000 Uiso . . . . . .
H2162 H 1.1032 0.1431 0.0498 0.0606 1.0000 Uiso . . . . . .
H2211 H 1.1044 -0.0930 0.2549 0.0322 1.0000 Uiso . . . . . .
H2221 H 1.1014 -0.1026 0.0999 0.0404 1.0000 Uiso . . . . . .
H2222 H 0.9526 -0.0784 0.1639 0.0404 1.0000 Uiso . . . . . .
H2231 H 1.0302 -0.2520 0.2168 0.0480 1.0000 Uiso . . . . . .
H2232 H 1.0281 -0.2679 0.1314 0.0480 1.0000 Uiso . . . . . .
H2241 H 1.2556 -0.3788 0.1620 0.0509 1.0000 Uiso . . . . . .
H2242 H 1.2943 -0.2964 0.0978 0.0509 1.0000 Uiso . . . . . .
H2251 H 1.4405 -0.2935 0.1882 0.0474 1.0000 Uiso . . . . . .
H2252 H 1.2929 -0.2680 0.2529 0.0474 1.0000 Uiso . . . . . .
H2261 H 1.3688 -0.1037 0.2179 0.0407 1.0000 Uiso . . . . . .
H2262 H 1.3594 -0.1205 0.1337 0.0407 1.0000 Uiso . . . . . .
H3011 H 1.1171 0.1441 0.4048 0.0338 1.0000 Uiso . . . . . .
H3012 H 1.0350 0.0611 0.3808 0.0338 1.0000 Uiso . . . . . .
H3111 H 1.0582 0.3550 0.2862 0.0361 1.0000 Uiso . . . . . .
H3121 H 0.8010 0.4788 0.3877 0.0415 1.0000 Uiso . . . . . .
H3122 H 0.8070 0.4620 0.3014 0.0415 1.0000 Uiso . . . . . .
H3131 H 0.8553 0.6329 0.3201 0.0513 1.0000 Uiso . . . . . .
H3132 H 0.9986 0.5585 0.2677 0.0513 1.0000 Uiso . . . . . .
H3141 H 1.0781 0.6404 0.3614 0.0540 1.0000 Uiso . . . . . .
H3142 H 0.9717 0.5900 0.4253 0.0540 1.0000 Uiso . . . . . .
H3151 H 1.2220 0.4814 0.4106 0.0560 1.0000 Uiso . . . . . .
H3152 H 1.2304 0.4659 0.3239 0.0560 1.0000 Uiso . . . . . .
H3161 H 1.1837 0.3074 0.3861 0.0481 1.0000 Uiso . . . . . .
H3162 H 1.0422 0.3761 0.4429 0.0481 1.0000 Uiso . . . . . .
H3211 H 0.8172 0.3210 0.4725 0.0416 1.0000 Uiso . . . . . .
H3221 H 0.6105 0.3841 0.4136 0.0432 1.0000 Uiso . . . . . .
H3222 H 0.5736 0.2695 0.4242 0.0432 1.0000 Uiso . . . . . .
H3231 H 0.5501 0.4130 0.5448 0.0587 1.0000 Uiso . . . . . .
H3232 H 0.4109 0.3831 0.5221 0.0587 1.0000 Uiso . . . . . .
H3241 H 0.4740 0.2892 0.6315 0.0613 1.0000 Uiso . . . . . .
H3242 H 0.4786 0.2096 0.5666 0.0613 1.0000 Uiso . . . . . .
H3251 H 0.7384 0.2534 0.6054 0.0497 1.0000 Uiso . . . . . .
H3252 H 0.6956 0.1407 0.6151 0.0497 1.0000 Uiso . . . . . .
H3261 H 0.8969 0.1389 0.5060 0.0461 1.0000 Uiso . . . . . .
H3262 H 0.7548 0.1144 0.4828 0.0461 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.89(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . Sn1 . 2.9332(3) yes
W1 . P2 . 2.5497(9) yes
W1 . P3 . 2.5363(8) yes
W1 . C1 . 1.834(4) yes
W1 . C6 . 2.003(4) yes
W1 . C7 . 2.011(4) yes
Sn1 . C11 . 2.178(4) yes
Sn1 . C12 . 2.191(4) yes
Sn1 . C13 . 2.197(4) yes
P2 . C201 . 1.862(4) yes
P2 . C211 . 1.863(4) yes
P2 . C221 . 1.863(4) yes
P3 . C301 . 1.845(4) yes
P3 . C311 . 1.868(4) yes
P3 . C321 . 1.861(4) yes
O1 . C6 . 1.153(5) yes
O2 . C7 . 1.143(5) yes
C1 . C2 . 1.488(5) yes
C2 . C3 . 1.532(7) yes
C2 . C4 . 1.540(6) yes
C2 . C5 . 1.536(7) yes
C3 . H31 . 0.954 no
C3 . H32 . 0.954 no
C3 . H33 . 0.967 no
C4 . H41 . 0.957 no
C4 . H42 . 0.942 no
C4 . H43 . 0.948 no
C5 . H51 . 0.944 no
C5 . H52 . 0.959 no
C5 . H53 . 0.967 no
C11 . H111 . 0.956 no
C11 . H112 . 0.959 no
C11 . H113 . 0.956 no
C12 . H121 . 0.947 no
C12 . H122 . 0.957 no
C12 . H123 . 0.952 no
C13 . H131 . 0.958 no
C13 . H132 . 0.954 no
C13 . H133 . 0.950 no
C201 . C301 . 1.535(5) yes
C201 . H2011 . 0.955 no
C201 . H2012 . 0.958 no
C211 . C212 . 1.544(6) yes
C211 . C216 . 1.525(6) yes
C211 . H2111 . 0.963 no
C212 . C213 . 1.542(6) yes
C212 . H2121 . 0.959 no
C212 . H2122 . 0.954 no
C213 . C214 . 1.521(8) yes
C213 . H2131 . 0.970 no
C213 . H2132 . 0.947 no
C214 . C215 . 1.509(7) yes
C214 . H2141 . 0.953 no
C214 . H2142 . 0.967 no
C215 . C216 . 1.537(6) yes
C215 . H2151 . 0.956 no
C215 . H2152 . 0.959 no
C216 . H2161 . 0.955 no
C216 . H2162 . 0.965 no
C221 . C222 . 1.531(5) yes
C221 . C226 . 1.537(5) yes
C221 . H2211 . 0.954 no
C222 . C223 . 1.540(5) yes
C222 . H2221 . 0.958 no
C222 . H2222 . 0.954 no
C223 . C224 . 1.521(6) yes
C223 . H2231 . 0.956 no
C223 . H2232 . 0.956 no
C224 . C225 . 1.528(7) yes
C224 . H2241 . 0.951 no
C224 . H2242 . 0.960 no
C225 . C226 . 1.526(6) yes
C225 . H2251 . 0.954 no
C225 . H2252 . 0.963 no
C226 . H2261 . 0.954 no
C226 . H2262 . 0.964 no
C301 . H3011 . 0.954 no
C301 . H3012 . 0.957 no
C311 . C312 . 1.535(5) yes
C311 . C316 . 1.526(5) yes
C311 . H3111 . 0.957 no
C312 . C313 . 1.529(6) yes
C312 . H3121 . 0.958 no
C312 . H3122 . 0.958 no
C313 . C314 . 1.512(7) yes
C313 . H3131 . 0.950 no
C313 . H3132 . 0.965 no
C314 . C315 . 1.530(7) yes
C314 . H3141 . 0.944 no
C314 . H3142 . 0.967 no
C315 . C316 . 1.528(6) yes
C315 . H3151 . 0.953 no
C315 . H3152 . 0.964 no
C316 . H3161 . 0.961 no
C316 . H3162 . 0.960 no
C321 . C322 . 1.528(6) yes
C321 . C326 . 1.527(6) yes
C321 . H3211 . 0.956 no
C322 . C323 . 1.526(5) yes
C322 . H3221 . 0.952 no
C322 . H3222 . 0.960 no
C323 . C324 . 1.515(7) yes
C323 . H3231 . 0.951 no
C323 . H3232 . 0.958 no
C324 . C325 . 1.531(7) yes
C324 . H3241 . 0.958 no
C324 . H3242 . 0.945 no
C325 . C326 . 1.536(5) yes
C325 . H3251 . 0.957 no
C325 . H3252 . 0.956 no
C326 . H3261 . 0.964 no
C326 . H3262 . 0.944 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Sn1 . W1 . P2 . 92.91(2) yes
Sn1 . W1 . P3 . 88.53(2) yes
P2 . W1 . P3 . 78.83(3) yes
Sn1 . W1 . C1 . 160.73(12) yes
P2 . W1 . C1 . 103.94(11) yes
P3 . W1 . C1 . 103.68(11) yes
Sn1 . W1 . C6 . 83.23(11) yes
P2 . W1 . C6 . 93.06(11) yes
P3 . W1 . C6 . 168.16(11) yes
C1 . W1 . C6 . 86.56(16) yes
Sn1 . W1 . C7 . 76.29(11) yes
P2 . W1 . C7 . 168.95(11) yes
P3 . W1 . C7 . 98.28(11) yes
C1 . W1 . C7 . 87.10(16) yes
C6 . W1 . C7 . 88.05(16) yes
W1 . Sn1 . C11 . 114.04(12) yes
W1 . Sn1 . C12 . 115.24(11) yes
C11 . Sn1 . C12 . 99.15(16) yes
W1 . Sn1 . C13 . 125.00(10) yes
C11 . Sn1 . C13 . 99.82(17) yes
C12 . Sn1 . C13 . 99.49(15) yes
W1 . P2 . C201 . 109.63(12) yes
W1 . P2 . C211 . 119.11(13) yes
C201 . P2 . C211 . 101.70(18) yes
W1 . P2 . C221 . 117.31(12) yes
C201 . P2 . C221 . 101.14(17) yes
C211 . P2 . C221 . 105.42(17) yes
W1 . P3 . C301 . 106.44(11) yes
W1 . P3 . C311 . 112.36(12) yes
C301 . P3 . C311 . 103.84(17) yes
W1 . P3 . C321 . 125.16(13) yes
C301 . P3 . C321 . 104.82(17) yes
C311 . P3 . C321 . 102.21(17) yes
W1 . C1 . C2 . 164.3(3) yes
C1 . C2 . C3 . 111.0(4) yes
C1 . C2 . C4 . 109.0(3) yes
C3 . C2 . C4 . 108.5(4) yes
C1 . C2 . C5 . 109.7(4) yes
C3 . C2 . C5 . 110.6(5) yes
C4 . C2 . C5 . 108.1(4) yes
C2 . C3 . H31 . 110.7 no
C2 . C3 . H32 . 111.3 no
H31 . C3 . H32 . 108.8 no
C2 . C3 . H33 . 110.4 no
H31 . C3 . H33 . 107.7 no
H32 . C3 . H33 . 107.8 no
C2 . C4 . H41 . 108.6 no
C2 . C4 . H42 . 110.0 no
H41 . C4 . H42 . 109.5 no
C2 . C4 . H43 . 109.5 no
H41 . C4 . H43 . 109.0 no
H42 . C4 . H43 . 110.3 no
C2 . C5 . H51 . 111.0 no
C2 . C5 . H52 . 110.6 no
H51 . C5 . H52 . 109.2 no
C2 . C5 . H53 . 110.0 no
H51 . C5 . H53 . 108.5 no
H52 . C5 . H53 . 107.3 no
W1 . C6 . O1 . 176.4(3) yes
W1 . C7 . O2 . 175.3(4) yes
Sn1 . C11 . H111 . 110.7 no
Sn1 . C11 . H112 . 110.5 no
H111 . C11 . H112 . 108.2 no
Sn1 . C11 . H113 . 110.7 no
H111 . C11 . H113 . 108.5 no
H112 . C11 . H113 . 108.2 no
Sn1 . C12 . H121 . 110.1 no
Sn1 . C12 . H122 . 109.6 no
H121 . C12 . H122 . 109.1 no
Sn1 . C12 . H123 . 109.8 no
H121 . C12 . H123 . 109.6 no
H122 . C12 . H123 . 108.7 no
Sn1 . C13 . H131 . 109.9 no
Sn1 . C13 . H132 . 110.1 no
H131 . C13 . H132 . 108.5 no
Sn1 . C13 . H133 . 110.3 no
H131 . C13 . H133 . 108.8 no
H132 . C13 . H133 . 109.1 no
P2 . C201 . C301 . 111.5(3) yes
P2 . C201 . H2011 . 109.4 no
C301 . C201 . H2011 . 109.0 no
P2 . C201 . H2012 . 109.2 no
C301 . C201 . H2012 . 109.3 no
H2011 . C201 . H2012 . 108.4 no
P2 . C211 . C212 . 111.1(3) yes
P2 . C211 . C216 . 110.9(3) yes
C212 . C211 . C216 . 110.6(3) yes
P2 . C211 . H2111 . 108.4 no
C212 . C211 . H2111 . 107.6 no
C216 . C211 . H2111 . 108.1 no
C211 . C212 . C213 . 111.5(4) yes
C211 . C212 . H2121 . 109.3 no
C213 . C212 . H2121 . 109.9 no
C211 . C212 . H2122 . 108.7 no
C213 . C212 . H2122 . 109.0 no
H2121 . C212 . H2122 . 108.3 no
C212 . C213 . C214 . 111.3(4) yes
C212 . C213 . H2131 . 108.5 no
C214 . C213 . H2131 . 108.1 no
C212 . C213 . H2132 . 110.2 no
C214 . C213 . H2132 . 110.6 no
H2131 . C213 . H2132 . 108.0 no
C213 . C214 . C215 . 111.3(4) yes
C213 . C214 . H2141 . 110.3 no
C215 . C214 . H2141 . 110.2 no
C213 . C214 . H2142 . 108.3 no
C215 . C214 . H2142 . 108.9 no
H2141 . C214 . H2142 . 107.8 no
C214 . C215 . C216 . 112.0(4) yes
C214 . C215 . H2151 . 108.6 no
C216 . C215 . H2151 . 108.8 no
C214 . C215 . H2152 . 109.5 no
C216 . C215 . H2152 . 109.5 no
H2151 . C215 . H2152 . 108.2 no
C215 . C216 . C211 . 111.3(4) yes
C215 . C216 . H2161 . 110.2 no
C211 . C216 . H2161 . 109.7 no
C215 . C216 . H2162 . 109.1 no
C211 . C216 . H2162 . 108.6 no
H2161 . C216 . H2162 . 107.8 no
P2 . C221 . C222 . 115.6(3) yes
P2 . C221 . C226 . 114.7(3) yes
C222 . C221 . C226 . 109.5(3) yes
P2 . C221 . H2211 . 105.9 no
C222 . C221 . H2211 . 105.3 no
C226 . C221 . H2211 . 104.8 no
C221 . C222 . C223 . 109.8(3) yes
C221 . C222 . H2221 . 109.3 no
C223 . C222 . H2221 . 109.5 no
C221 . C222 . H2222 . 109.5 no
C223 . C222 . H2222 . 110.3 no
H2221 . C222 . H2222 . 108.5 no
C222 . C223 . C224 . 112.2(3) yes
C222 . C223 . H2231 . 108.7 no
C224 . C223 . H2231 . 108.9 no
C222 . C223 . H2232 . 109.2 no
C224 . C223 . H2232 . 109.3 no
H2231 . C223 . H2232 . 108.4 no
C223 . C224 . C225 . 110.8(3) yes
C223 . C224 . H2241 . 110.3 no
C225 . C224 . H2241 . 109.7 no
C223 . C224 . H2242 . 109.4 no
C225 . C224 . H2242 . 108.1 no
H2241 . C224 . H2242 . 108.5 no
C224 . C225 . C226 . 111.0(3) yes
C224 . C225 . H2251 . 109.6 no
C226 . C225 . H2251 . 110.6 no
C224 . C225 . H2252 . 108.2 no
C226 . C225 . H2252 . 109.2 no
H2251 . C225 . H2252 . 108.1 no
C221 . C226 . C225 . 110.9(3) yes
C221 . C226 . H2261 . 109.8 no
C225 . C226 . H2261 . 110.1 no
C221 . C226 . H2262 . 109.0 no
C225 . C226 . H2262 . 108.9 no
H2261 . C226 . H2262 . 108.0 no
C201 . C301 . P3 . 110.5(2) yes
C201 . C301 . H3011 . 109.7 no
P3 . C301 . H3011 . 109.6 no
C201 . C301 . H3012 . 109.1 no
P3 . C301 . H3012 . 109.3 no
H3011 . C301 . H3012 . 108.5 no
P3 . C311 . C312 . 110.2(3) yes
P3 . C311 . C316 . 115.9(3) yes
C312 . C311 . C316 . 110.9(3) yes
P3 . C311 . H3111 . 106.9 no
C312 . C311 . H3111 . 106.4 no
C316 . C311 . H3111 . 106.0 no
C311 . C312 . C313 . 111.2(3) yes
C311 . C312 . H3121 . 109.6 no
C313 . C312 . H3121 . 108.5 no
C311 . C312 . H3122 . 109.8 no
C313 . C312 . H3122 . 109.5 no
H3121 . C312 . H3122 . 108.2 no
C312 . C313 . C314 . 111.3(4) yes
C312 . C313 . H3131 . 110.0 no
C314 . C313 . H3131 . 110.3 no
C312 . C313 . H3132 . 108.3 no
C314 . C313 . H3132 . 108.6 no
H3131 . C313 . H3132 . 108.3 no
C313 . C314 . C315 . 110.8(4) yes
C313 . C314 . H3141 . 110.6 no
C315 . C314 . H3141 . 110.4 no
C313 . C314 . H3142 . 108.5 no
C315 . C314 . H3142 . 108.0 no
H3141 . C314 . H3142 . 108.5 no
C314 . C315 . C316 . 112.2(4) yes
C314 . C315 . H3151 . 109.4 no
C316 . C315 . H3151 . 110.5 no
C314 . C315 . H3152 . 107.7 no
C316 . C315 . H3152 . 108.9 no
H3151 . C315 . H3152 . 108.1 no
C315 . C316 . C311 . 111.9(4) yes
C315 . C316 . H3161 . 109.3 no
C311 . C316 . H3161 . 109.8 no
C315 . C316 . H3162 . 108.6 no
C311 . C316 . H3162 . 109.5 no
H3161 . C316 . H3162 . 107.7 no
P3 . C321 . C322 . 112.4(3) yes
P3 . C321 . C326 . 115.3(3) yes
C322 . C321 . C326 . 110.1(3) yes
P3 . C321 . H3211 . 106.4 no
C322 . C321 . H3211 . 105.7 no
C326 . C321 . H3211 . 106.2 no
C321 . C322 . C323 . 111.7(4) yes
C321 . C322 . H3221 . 109.7 no
C323 . C322 . H3221 . 109.2 no
C321 . C322 . H3222 . 109.0 no
C323 . C322 . H3222 . 108.7 no
H3221 . C322 . H3222 . 108.4 no
C322 . C323 . C324 . 112.1(4) yes
C322 . C323 . H3231 . 109.3 no
C324 . C323 . H3231 . 108.7 no
C322 . C323 . H3232 . 109.7 no
C324 . C323 . H3232 . 108.2 no
H3231 . C323 . H3232 . 108.6 no
C323 . C324 . C325 . 111.7(4) yes
C323 . C324 . H3241 . 108.6 no
C325 . C324 . H3241 . 109.1 no
C323 . C324 . H3242 . 108.9 no
C325 . C324 . H3242 . 109.3 no
H3241 . C324 . H3242 . 109.2 no
C324 . C325 . C326 . 111.8(4) yes
C324 . C325 . H3251 . 109.0 no
C326 . C325 . H3251 . 109.5 no
C324 . C325 . H3252 . 108.7 no
C326 . C325 . H3252 . 109.4 no
H3251 . C325 . H3252 . 108.4 no
C325 . C326 . C321 . 110.6(4) yes
C325 . C326 . H3261 . 109.0 no
C321 . C326 . H3261 . 108.8 no
C325 . C326 . H3262 . 109.8 no
C321 . C326 . H3262 . 109.8 no
H3261 . C326 . H3262 . 108.8 no



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

data_Compound_3b
_database_code_depnum_ccdc_archive 'CCDC 1515557'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C39 H62 O2 P2 Se W'
_chemical_formula_sum            'C39 H62 O2 P2 Se W'
_chemical_formula_weight         887.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         C39H62O2P2SeW
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5933(3)
_cell_length_b                   15.6299(5)
_cell_length_c                   24.1696(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.630(3)
_cell_angle_gamma                90
_cell_volume                     3945.44(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12306
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1150
_cell_measurement_theta_min      3.7040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.473
_exptl_absorpt_correction_T_max  0.79291
_exptl_absorpt_correction_T_min  0.78344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -9 0 0.0272
-2 9 0 0.0272
-4 -8 5 0.0144
6 3 -6 0.0332
0 1 -16 0.0053
0 -1 16 0.0088

_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.014
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9984 -8.9851 -0.0021 0.0589 0.2861 0.8864
-1.9984 8.9851 0.0021 -0.0589 -0.2861 -0.8864
-4.0000 -7.9829 5.0196 0.2143 0.9371 0.2924
5.9988 2.9903 -6.0239 -0.2214 -0.8834 0.2765
-0.0064 0.9824 -15.9895 -1.0342 -0.0743 -0.0628
0.0064 -0.9824 15.9895 1.0342 0.0743 0.0628

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61798
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.836
_diffrn_reflns_theta_min         3.382
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00  32.00   1.00    6.25    --  -37.04  38.00-120.00   88
  2  ω    -30.00  54.00   1.00    6.25    --   37.04 -57.00-180.00   84
  3  ω    -32.00  56.00   1.00    6.25    --   37.04 -38.00 -60.00   88
  4  ω     64.00 104.00   1.00    6.25    --   37.04  57.00-150.00   40
  5  ω    -31.00   5.00   1.00    6.25    --   37.04 -38.00   0.00   36
  6  ω     42.00  69.00   1.00    6.25    --   37.04  77.00-180.00   27
  7  ω     23.00  57.00   1.00    6.25    --   37.04 -99.00 150.00   34
  8  ω    -30.00  18.00   1.00    6.25    --   37.04 -77.00   0.00   48
  9  ω     11.00  50.00   1.00    6.25    --   37.04  77.00-120.00   39
 10  ω     24.00  71.00   1.00    6.25    --   37.04-125.00 -30.00   47
 11  ω    -19.00  33.00   1.00    6.25    --   37.04 -57.00 -60.00   52
 12  ω     31.00  90.00   1.00    6.25    --   37.04-125.00  60.00   59
 13  ω     10.00  50.00   1.00    6.25    --   37.04 -38.00  60.00   40
 14  ω     19.00  55.00   1.00    6.25    --   37.04 -38.00   0.00   36
 15  ω    -34.00  63.00   1.00    6.25    --   37.04 -19.00  60.00   97
 16  ω     24.00  58.00   1.00    6.25    --   37.04  57.00-150.00   34
 17  ω     18.00  48.00   1.00    6.25    --   37.04 -38.00  90.00   30
 18  ω     31.00  96.00   1.00    6.25    --   37.04-136.00 149.00   65
 19  ω     30.00  60.00   1.00    6.25    --   37.04 -77.00   0.00   30
 20  ω     59.00  95.00   1.00    6.25    --   37.04  77.00-120.00   36
 21  ω    -19.00  22.00   1.00    6.25    --   37.04   0.00 150.00   41
 22  ω     60.00  87.00   1.00    6.25    --   37.04   0.00 150.00   27
 23  ω     61.00  95.00   1.00    6.25    --   37.04  57.00  60.00   34
 24  ω    -32.00  -4.00   1.00    6.25    --   37.04 -38.00  60.00   28
 25  ω     43.00  84.00   1.00    6.25    --   37.04-125.00 -60.00   41
 26  ω      3.00  30.00   1.00    6.25    --   37.04 -99.00 -30.00   27
 27  ω     73.00 113.00   1.00   25.00    --  111.00-111.00-180.00   40
 28  ω    104.00 136.00   1.00   25.00    --  111.00  12.00-120.00   32
 29  ω    123.00 173.00   1.00   25.00    --  111.00  25.00  90.00   50
 30  ω     96.00 128.00   1.00   25.00    --  111.00 -50.00 150.00   32
 31  ω     98.00 138.00   1.00   25.00    --  111.00  64.00-150.00   40
 32  ω     45.00  89.00   1.00   25.00    --  111.00 -50.00 150.00   44
 33  ω     41.00  81.00   1.00   25.00    --  111.00 -16.00-107.93   40
 34  ω     69.00 123.00   1.00   25.00    --  111.00 -50.00 -60.00   54
 35  ω     97.00 122.00   1.00   25.00    --  111.00  38.00 -30.00   25
 36  ω     94.00 127.00   1.00   25.00    --  111.00 -77.00 120.00   33
 37  ω    152.00 177.00   1.00   25.00    --  111.00  50.00 -60.00   25
 38  ω     95.00 122.00   1.00   25.00    --  111.00 -92.00  60.00   27
 39  ω     95.00 139.00   1.00   25.00    --  111.00  50.00 -60.00   44
 40  ω     73.00  98.00   1.00   25.00    --  111.00 -33.00  76.00   25
 41  ω     46.00 103.00   1.00   25.00    --  111.00 -70.00 -25.69   57
 42  ω     56.00  83.00   1.00   25.00    --  111.00 -92.00  60.00   27
 43  ω     55.00 102.00   1.00   25.00    --  111.00 -64.00-120.00   47
 44  ω    141.00 178.00   1.00   25.00    --  111.00  64.00 150.00   37
 45  ω    114.00 163.00   1.00   25.00    --  111.00  77.00 -90.00   49
 46  ω     44.00  92.00   1.00   25.00    --  111.00 -92.00  30.00   48
 47  ω     66.00  93.00   1.00   25.00    --  111.00 -77.00 -30.00   27
 48  ω    107.00 138.00   1.00   25.00    --  111.00 -77.00 150.00   31
 49  ω     53.00  78.00   1.00   25.00    --  111.00 -77.00 120.00   25
 50  ω     86.00 143.00   1.00   25.00    --  111.00  75.00  25.64   57
 51  ω     66.00 112.00   1.00   25.00    --  111.00-111.00  90.00   46
 52  ω    137.00 162.00   1.00   25.00    --  111.00  38.00 -30.00   25
 53  ω     95.00 153.00   1.00   25.00    --  111.00  50.00-120.00   58
 54  ω     86.00 113.00   1.00   25.00    --  111.00-111.00 -60.00   27
 55  ω     74.00 138.00   1.00   25.00    --  111.00  12.00-150.00   64
 56  ω    149.00 178.00   1.00   25.00    --  111.00  64.00-150.00   29
 57  ω    104.00 159.00   1.00   25.00    --  111.00  64.00   0.00   55
 58  ω     65.00  92.00   1.00   25.00    --  111.00 -38.00-150.00   27
 59  ω     94.00 122.00   1.00   25.00    --  111.00 -38.00-150.00   28
 60  ω     57.00  97.00   1.00   25.00    --  111.00 -77.00  60.00   40
 61  ω     41.00  81.00   1.00   25.00    --  111.00 -17.00  26.82   40
 62  ω     98.00 125.00   1.00   25.00    --  111.00 -92.00 150.00   27
 63  ω     44.00  91.00   1.00   25.00    --  111.00 -77.00 150.00   47
 64  ω     82.00 109.00   1.00   25.00    --  111.00 -55.00-149.56   27
 65  ω     62.00  89.00   1.00   25.00    --  111.00 -92.00 150.00   27
 66  ω     46.00  87.00   1.00   25.00    --  111.00 -64.00 -60.00   41
 67  ω     90.00 125.00   1.00   25.00    --  111.00-133.00 -33.00   35
 68  ω     98.00 158.00   1.00   25.00    --  111.00  50.00 -90.00   60
 69  ω     97.00 147.00   1.00   25.00    --  111.00  50.00-180.00   50
 70  ω     63.00 116.00   1.00   25.00    --  111.00-111.00 150.00   53
 71  ω     42.00 129.00   1.00   25.00    --  111.00 -42.00  18.58   87
 72  ω     88.00 115.00   1.00   25.00    --  111.00-111.00-150.00   27
 73  ω     95.00 161.00   1.00   25.00    --  111.00  50.00   0.00   66
 74  ω     92.00 134.00   1.00   25.00    --  111.00 -77.00  90.00   42
 75  ω     48.00  75.00   1.00   25.00    --  111.00 -77.00  90.00   27
 76  ω     76.00 103.00   1.00   25.00    --  111.00 -77.00 -90.00   27
 77  ω     46.00  72.00   1.00   25.00    --  111.00 -64.00-150.00   26
 78  ω    139.00 178.00   1.00   25.00    --  111.00  38.00  60.00   39
 79  ω    139.00 178.00   1.00   25.00    --  111.00  50.00 120.00   39
 80  ω    102.00 136.00   1.00   25.00    --  111.00  50.00 120.00   34
 81  ω     74.00 111.00   1.00   25.00    --  111.00-111.00  60.00   37
 82  ω     70.00 102.00   1.00   25.00    --  111.00-111.00 -30.00   32
 83  ω     96.00 121.00   1.00   25.00    --  111.00  38.00-150.00   25
 84  ω     71.00 116.00   1.00   25.00    --  111.00-111.00   0.00   45
 85  ω    113.00 138.00   1.00   25.00    --  111.00 -16.00-107.93   25
 86  ω     48.00  79.00   1.00   25.00    --  111.00 -55.00-149.56   31
 87  ω     82.00 109.00   1.00   25.00    --  111.00 -34.00 100.34   27
 88  ω    105.00 132.00   1.00   25.00    --  111.00 -92.00  30.00   27
 89  ω     46.00  73.00   1.00   25.00    --  111.00 -34.00 100.34   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0281629000
_diffrn_orient_matrix_UB_12      -0.0003018000
_diffrn_orient_matrix_UB_13      0.0646508000
_diffrn_orient_matrix_UB_21      -0.1172528000
_diffrn_orient_matrix_UB_22      -0.0579187000
_diffrn_orient_matrix_UB_23      0.0011341000
_diffrn_orient_matrix_UB_31      0.0848497000
_diffrn_orient_matrix_UB_32      -0.0797817000
_diffrn_orient_matrix_UB_33      -0.0010109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6591
_reflns_number_total             7980
_reflns_odcompleteness_completeness 98.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         3.192
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0473
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²+8.8272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1163
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28), C10(H10), C16(H16), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C21(H21A,H21B), C8(H8A,H8B), C23(H23A,H23B), C11(H11A,H11B),
 C13(H13A,H13B), C9(H9A,H9B), C17(H17A,H17B), C24(H24A,H24B), C20(H20A,H20B),
 C19(H19A,H19B), C12(H12A,H12B), C14(H14A,H14B), C18(H18A,H18B), C31(H31A,H31B),
  C32(H32A,H32B), C15(H15A,H15B), C26(H26A,H26B), C33(H33A,H33B), C27(H27A,
 H27B), C30(H30A,H30B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C39(H39), C37(H37), C36(H36), C38(H38)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.57612(2) 0.19614(2) 0.29640(2) 0.02670(8) Uani 1 1 d . . . . .
Se1 Se 0.33980(6) 0.12544(5) 0.29899(3) 0.03581(15) Uani 1 1 d . . . . .
P3 P 0.45738(12) 0.27329(10) 0.21024(5) 0.0270(3) Uani 1 1 d . . . . .
P4 P 0.51774(12) 0.33887(10) 0.33846(5) 0.0274(3) Uani 1 1 d . . . . .
C28 C 0.3531(5) 0.2194(4) 0.1512(2) 0.0333(12) Uani 1 1 d . . . . .
H28 H 0.3575 0.2534 0.1175 0.040 Uiso 1 1 calc R . . . .
C1 C 0.7429(6) 0.2199(4) 0.2921(2) 0.0349(13) Uani 1 1 d . . . . .
C2 C 0.8843(6) 0.2190(4) 0.2915(3) 0.0367(13) Uani 1 1 d . . . . .
C29 C 0.4017(6) 0.1295(4) 0.1401(2) 0.0354(13) Uani 1 1 d . . . . .
H29A H 0.4918 0.1323 0.1372 0.042 Uiso 1 1 calc R . . . .
H29B H 0.3926 0.0922 0.1713 0.042 Uiso 1 1 calc R . . . .
C10 C 0.6559(5) 0.4091(4) 0.3655(2) 0.0317(12) Uani 1 1 d . . . . .
H10 H 0.7063 0.4135 0.3351 0.038 Uiso 1 1 calc R . . . .
C16 C 0.4167(5) 0.3415(4) 0.3947(2) 0.0305(11) Uani 1 1 d . . . . .
H16 H 0.4351 0.3955 0.4151 0.037 Uiso 1 1 calc R . . . .
C35 C 0.2814(7) 0.0499(4) 0.4000(3) 0.0412(14) Uani 1 1 d . . . . .
H35 H 0.2217 0.0940 0.3980 0.049 Uiso 1 1 calc R . . . .
C34 C 0.3594(6) 0.0437(4) 0.3595(2) 0.0333(12) Uani 1 1 d . . . . .
C21 C 0.2718(5) 0.3395(4) 0.3724(2) 0.0331(12) Uani 1 1 d . . . . .
H21A H 0.2491 0.3861 0.3462 0.040 Uiso 1 1 calc R . . . .
H21B H 0.2495 0.2861 0.3528 0.040 Uiso 1 1 calc R . . . .
C8 C 0.4319(5) 0.4073(4) 0.2815(2) 0.0287(11) Uani 1 1 d . . . . .
H8A H 0.3757 0.4462 0.2969 0.034 Uiso 1 1 calc R . . . .
H8B H 0.4936 0.4412 0.2655 0.034 Uiso 1 1 calc R . . . .
C23 C 0.6431(6) 0.2785(4) 0.1415(2) 0.0367(13) Uani 1 1 d . . . . .
H23A H 0.5846 0.2503 0.1119 0.044 Uiso 1 1 calc R . . . .
H23B H 0.6855 0.2348 0.1664 0.044 Uiso 1 1 calc R . . . .
C11 C 0.7466(6) 0.3714(4) 0.4157(2) 0.0364(13) Uani 1 1 d . . . . .
H11A H 0.7029 0.3680 0.4479 0.044 Uiso 1 1 calc R . . . .
H11B H 0.7714 0.3139 0.4068 0.044 Uiso 1 1 calc R . . . .
C13 C 0.8312(6) 0.5190(5) 0.4427(3) 0.0422(15) Uani 1 1 d . . . . .
H13A H 0.9084 0.5535 0.4497 0.051 Uiso 1 1 calc R . . . .
H13B H 0.7922 0.5200 0.4762 0.051 Uiso 1 1 calc R . . . .
C22 C 0.5676(6) 0.3374(4) 0.1743(2) 0.0334(12) Uani 1 1 d . . . . .
H22 H 0.6299 0.3639 0.2039 0.040 Uiso 1 1 calc R . . . .
C9 C 0.3534(5) 0.3537(4) 0.2354(2) 0.0289(11) Uani 1 1 d . . . . .
H9A H 0.3162 0.3904 0.2045 0.035 Uiso 1 1 calc R . . . .
H9B H 0.2842 0.3255 0.2499 0.035 Uiso 1 1 calc R . . . .
C17 C 0.4527(5) 0.2687(5) 0.4370(2) 0.0351(13) Uani 1 1 d . . . . .
H17A H 0.5437 0.2709 0.4516 0.042 Uiso 1 1 calc R . . . .
H17B H 0.4342 0.2141 0.4184 0.042 Uiso 1 1 calc R . . . .
C24 C 0.7432(7) 0.3282(5) 0.1155(3) 0.0440(16) Uani 1 1 d . . . . .
H24A H 0.8063 0.3522 0.1452 0.053 Uiso 1 1 calc R . . . .
H24B H 0.7870 0.2894 0.0938 0.053 Uiso 1 1 calc R . . . .
C20 C 0.1979(6) 0.3478(4) 0.4210(3) 0.0370(13) Uani 1 1 d . . . . .
H20A H 0.2154 0.4034 0.4385 0.044 Uiso 1 1 calc R . . . .
H20B H 0.1069 0.3447 0.4066 0.044 Uiso 1 1 calc R . . . .
C19 C 0.2331(6) 0.2786(4) 0.4648(3) 0.0387(14) Uani 1 1 d . . . . .
H19A H 0.2057 0.2234 0.4488 0.046 Uiso 1 1 calc R . . . .
H19B H 0.1887 0.2890 0.4962 0.046 Uiso 1 1 calc R . . . .
C12 C 0.8661(6) 0.4274(5) 0.4302(3) 0.0454(17) Uani 1 1 d . . . . .
H12A H 0.9215 0.4038 0.4626 0.055 Uiso 1 1 calc R . . . .
H12B H 0.9129 0.4272 0.3989 0.055 Uiso 1 1 calc R . . . .
C14 C 0.7384(6) 0.5573(4) 0.3938(3) 0.0386(14) Uani 1 1 d . . . . .
H14A H 0.7125 0.6139 0.4040 0.046 Uiso 1 1 calc R . . . .
H14B H 0.7811 0.5631 0.3614 0.046 Uiso 1 1 calc R . . . .
C18 C 0.3767(6) 0.2767(5) 0.4858(3) 0.0408(15) Uani 1 1 d . . . . .
H18A H 0.3970 0.2286 0.5111 0.049 Uiso 1 1 calc R . . . .
H18B H 0.4020 0.3287 0.5067 0.049 Uiso 1 1 calc R . . . .
C4 C 0.9547(6) 0.1937(5) 0.3497(3) 0.0478(16) Uani 1 1 d . . . . .
H4A H 0.9339 0.2335 0.3770 0.072 Uiso 1 1 calc GR . . . .
H4B H 1.0453 0.1945 0.3498 0.072 Uiso 1 1 calc GR . . . .
H4C H 0.9289 0.1372 0.3587 0.072 Uiso 1 1 calc GR . . . .
C31 C 0.1843(6) 0.0885(5) 0.0897(3) 0.0443(15) Uani 1 1 d . . . . .
H31A H 0.1372 0.0687 0.0541 0.053 Uiso 1 1 calc R . . . .
H31B H 0.1714 0.0475 0.1183 0.053 Uiso 1 1 calc R . . . .
C32 C 0.1321(6) 0.1750(5) 0.1037(3) 0.0411(15) Uani 1 1 d . . . . .
H32A H 0.0440 0.1684 0.1091 0.049 Uiso 1 1 calc R . . . .
H32B H 0.1330 0.2137 0.0724 0.049 Uiso 1 1 calc R . . . .
C15 C 0.6201(5) 0.5009(4) 0.3784(3) 0.0349(13) Uani 1 1 d . . . . .
H15A H 0.5653 0.5248 0.3459 0.042 Uiso 1 1 calc R . . . .
H15B H 0.5723 0.5005 0.4094 0.042 Uiso 1 1 calc R . . . .
C26 C 0.6035(8) 0.4592(5) 0.1100(3) 0.0488(17) Uani 1 1 d . . . . .
H26A H 0.6612 0.4896 0.1388 0.059 Uiso 1 1 calc R . . . .
H26B H 0.5592 0.5013 0.0843 0.059 Uiso 1 1 calc R . . . .
C39 C 0.4433(7) -0.0248(5) 0.3624(3) 0.0509(18) Uani 1 1 d . . . . .
H39 H 0.4948 -0.0313 0.3350 0.061 Uiso 1 1 calc R . . . .
C33 C 0.2110(6) 0.2138(4) 0.1567(3) 0.0381(14) Uani 1 1 d . . . . .
H33A H 0.2017 0.1788 0.1889 0.046 Uiso 1 1 calc R . . . .
H33B H 0.1790 0.2706 0.1628 0.046 Uiso 1 1 calc R . . . .
C37 C 0.3775(8) -0.0750(5) 0.4475(3) 0.0527(18) Uani 1 1 d . . . . .
H37 H 0.3865 -0.1131 0.4774 0.063 Uiso 1 1 calc R . . . .
C3 C 0.9264(7) 0.3093(5) 0.2771(3) 0.0503(17) Uani 1 1 d . . . . .
H3A H 0.8827 0.3253 0.2406 0.075 Uiso 1 1 calc GR . . . .
H3B H 1.0172 0.3098 0.2774 0.075 Uiso 1 1 calc GR . . . .
H3C H 0.9058 0.3493 0.3044 0.075 Uiso 1 1 calc GR . . . .
C27 C 0.5058(7) 0.4095(4) 0.1373(3) 0.0418(14) Uani 1 1 d . . . . .
H27A H 0.4638 0.4484 0.1597 0.050 Uiso 1 1 calc R . . . .
H27B H 0.4410 0.3860 0.1081 0.050 Uiso 1 1 calc R . . . .
C30 C 0.3262(6) 0.0930(5) 0.0860(3) 0.0460(16) Uani 1 1 d . . . . .
H30A H 0.3385 0.1290 0.0546 0.055 Uiso 1 1 calc R . . . .
H30B H 0.3576 0.0362 0.0796 0.055 Uiso 1 1 calc R . . . .
C36 C 0.2916(8) -0.0090(5) 0.4437(3) 0.0519(18) Uani 1 1 d . . . . .
H36 H 0.2391 -0.0035 0.4707 0.062 Uiso 1 1 calc R . . . .
C5 C 0.9150(7) 0.1533(6) 0.2481(4) 0.058(2) Uani 1 1 d . . . . .
H5A H 0.8853 0.0978 0.2571 0.088 Uiso 1 1 calc GR . . . .
H5B H 1.0058 0.1513 0.2488 0.088 Uiso 1 1 calc GR . . . .
H5C H 0.8730 0.1698 0.2113 0.088 Uiso 1 1 calc GR . . . .
C25 C 0.6816(8) 0.3995(5) 0.0780(3) 0.0528(18) Uani 1 1 d . . . . .
H25A H 0.6257 0.3751 0.0460 0.063 Uiso 1 1 calc R . . . .
H25B H 0.7475 0.4322 0.0641 0.063 Uiso 1 1 calc R . . . .
C38 C 0.4509(8) -0.0831(5) 0.4053(4) 0.058(2) Uani 1 1 d . . . . .
H38 H 0.5066 -0.1292 0.4061 0.070 Uiso 1 1 calc R . . . .
O2 O 0.6311(5) 0.0200(3) 0.2398(2) 0.0521(12) Uani 1 1 d . . . . .
O1 O 0.6850(5) 0.1179(4) 0.41518(19) 0.0529(13) Uani 1 1 d . . . . .
C6 C 0.6425(5) 0.1450(4) 0.3719(2) 0.0343(13) Uani 1 1 d . . . . .
C7 C 0.6069(6) 0.0822(4) 0.2594(3) 0.0351(12) 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
W1 Se1 2.7467(7) . ?
W1 P3 2.5489(14) . ?
W1 P4 2.5696(15) . ?
W1 C1 1.826(7) . ?
W1 C6 2.009(6) . ?
W1 C7 2.044(6) . ?
Se1 C34 1.927(6) . ?
P3 C28 1.855(6) . ?
P3 C22 1.860(6) . ?
P3 C9 1.840(6) . ?
P4 C10 1.859(6) . ?
P4 C16 1.866(5) . ?
P4 C8 1.857(6) . ?
C28 C29 1.535(8) . ?
C28 C33 1.536(8) . ?
C1 C2 1.501(8) . ?
C2 C4 1.528(9) . ?
C2 C3 1.539(9) . ?
C2 C5 1.542(9) . ?
C29 C30 1.525(8) . ?
C10 C11 1.534(8) . ?
C10 C15 1.530(9) . ?
C16 C21 1.539(7) . ?
C16 C17 1.535(9) . ?
C35 C34 1.385(8) . ?
C35 C36 1.392(10) . ?
C34 C39 1.385(9) . ?
C21 C20 1.521(7) . ?
C8 C9 1.524(7) . ?
C23 C22 1.526(8) . ?
C23 C24 1.530(8) . ?
C11 C12 1.531(9) . ?
C13 C12 1.522(10) . ?
C13 C14 1.528(9) . ?
C22 C27 1.518(9) . ?
C17 C18 1.541(7) . ?
C24 C25 1.515(10) . ?
C20 C19 1.517(9) . ?
C19 C18 1.520(9) . ?
C14 C15 1.526(8) . ?
C31 C32 1.519(10) . ?
C31 C30 1.523(9) . ?
C32 C33 1.534(8) . ?
C26 C27 1.529(9) . ?
C26 C25 1.540(10) . ?
C39 C38 1.374(10) . ?
C37 C36 1.368(11) . ?
C37 C38 1.387(11) . ?
O2 C7 1.128(8) . ?
O1 C6 1.148(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
P3 W1 Se1 83.22(3) . . ?
P3 W1 P4 78.11(4) . . ?
P4 W1 Se1 93.42(3) . . ?
C1 W1 Se1 167.89(19) . . ?
C1 W1 P3 101.93(19) . . ?
C1 W1 P4 98.35(19) . . ?
C1 W1 C6 86.5(2) . . ?
C1 W1 C7 85.7(3) . . ?
C6 W1 Se1 90.06(18) . . ?
C6 W1 P3 168.67(16) . . ?
C6 W1 P4 93.26(18) . . ?
C6 W1 C7 89.6(3) . . ?
C7 W1 Se1 82.67(18) . . ?
C7 W1 P3 98.50(18) . . ?
C7 W1 P4 175.14(18) . . ?
C34 Se1 W1 107.53(18) . . ?
C28 P3 W1 124.2(2) . . ?
C28 P3 C22 103.0(3) . . ?
C22 P3 W1 111.94(19) . . ?
C9 P3 W1 107.12(18) . . ?
C9 P3 C28 104.6(3) . . ?
C9 P3 C22 104.1(3) . . ?
C10 P4 W1 115.11(19) . . ?
C10 P4 C16 104.2(2) . . ?
C16 P4 W1 120.9(2) . . ?
C8 P4 W1 109.06(18) . . ?
C8 P4 C10 100.4(3) . . ?
C8 P4 C16 105.0(3) . . ?
C29 C28 P3 112.0(4) . . ?
C33 C28 P3 115.1(4) . . ?
C33 C28 C29 109.0(5) . . ?
C2 C1 W1 167.4(5) . . ?
C1 C2 C4 109.2(5) . . ?
C1 C2 C3 108.7(5) . . ?
C1 C2 C5 109.7(5) . . ?
C4 C2 C3 109.3(6) . . ?
C4 C2 C5 109.2(6) . . ?
C3 C2 C5 110.8(6) . . ?
C30 C29 C28 110.4(5) . . ?
C11 C10 P4 113.8(4) . . ?
C15 C10 P4 114.7(4) . . ?
C15 C10 C11 110.0(5) . . ?
C21 C16 P4 113.9(4) . . ?
C17 C16 P4 111.1(4) . . ?
C17 C16 C21 109.8(5) . . ?
C34 C35 C36 120.6(7) . . ?
C35 C34 Se1 119.2(5) . . ?
C39 C34 Se1 122.4(5) . . ?
C39 C34 C35 118.2(6) . . ?
C20 C21 C16 109.9(5) . . ?
C9 C8 P4 111.4(4) . . ?
C22 C23 C24 111.5(5) . . ?
C12 C11 C10 110.1(5) . . ?
C12 C13 C14 111.2(5) . . ?
C23 C22 P3 110.1(4) . . ?
C27 C22 P3 115.6(4) . . ?
C27 C22 C23 110.7(5) . . ?
C8 C9 P3 109.4(4) . . ?
C16 C17 C18 110.3(5) . . ?
C25 C24 C23 111.1(6) . . ?
C19 C20 C21 112.3(5) . . ?
C20 C19 C18 111.3(5) . . ?
C13 C12 C11 111.4(5) . . ?
C15 C14 C13 110.9(5) . . ?
C19 C18 C17 111.6(5) . . ?
C32 C31 C30 111.8(6) . . ?
C31 C32 C33 111.8(5) . . ?
C14 C15 C10 111.7(5) . . ?
C27 C26 C25 111.6(6) . . ?
C38 C39 C34 120.4(7) . . ?
C32 C33 C28 110.7(5) . . ?
C36 C37 C38 117.9(7) . . ?
C22 C27 C26 112.0(6) . . ?
C31 C30 C29 110.5(5) . . ?
C37 C36 C35 121.1(7) . . ?
C24 C25 C26 111.0(5) . . ?
C39 C38 C37 121.7(7) . . ?
O1 C6 W1 177.1(6) . . ?
O2 C7 W1 176.2(6) . . ?



_ins_header                      
;
TITL RK09_scaled in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.593342  15.629852  24.169624  90.0000  99.6296  90.0000
ZERR    4.00   0.000284   0.000481   0.000625   0.0000   0.0026   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Se W
UNIT 156.00 248.00 8.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.668

####################################################################### 
# 
# 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_Compound_3c
_database_code_depnum_ccdc_archive 'CCDC 1515558'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C39 H62 O2 P2 Te W'
_chemical_formula_sum            'C39 H62 O2 P2 Te W'
_chemical_formula_weight         936.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C39 H62 O2 P2 Te W'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.62715(11)
_cell_length_b                   15.6401(2)
_cell_length_c                   24.3392(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.1600(11)
_cell_angle_gamma                90
_cell_volume                     3981.98(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19436
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6020
_cell_measurement_theta_min      3.3500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.026
_exptl_absorpt_correction_T_max  0.33411
_exptl_absorpt_correction_T_min  0.25367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 3 3 0.0969
-4 -8 0 0.1243
5 7 -1 0.1082
2 -10 -3 0.0869
0 10 2 0.1204
-1 -1 -15 0.0246
1 1 15 0.0246

_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.049
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.9969 2.9974 3.0061 0.3930 -0.0824 0.9769
-4.0001 -7.9924 -0.0006 0.9745 -0.1261 -0.0398
4.9996 6.9934 -1.0003 -0.9873 0.1031 -0.1374
1.9973 -9.9906 -3.0053 0.5927 -0.0847 -0.8449
0.0020 9.9906 2.0041 -0.7716 0.0964 0.6169
-1.0004 -0.9951 -14.9936 0.1411 -0.9952 -0.0300
1.0004 0.9951 14.9936 -0.1411 0.9952 0.0300

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.984
_diffrn_reflns_theta_min         3.375
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -20.00   1.00    1.04    --  -37.20 -57.00 120.00   84
  2  ω     23.00  91.00   1.00    1.04    --   37.20-125.00 120.00   68
  3  ω    -30.00  54.00   1.00    1.04    --   37.20 -57.00 -60.00   84
  4  ω      8.00 109.00   1.00    1.04    --   37.20  19.00 -90.00  101
  5  ω    -32.00 106.00   1.00    1.04    --   37.20   0.00-120.00  138
  6  ω     23.00  91.00   1.00    1.04    --   37.20-125.00  90.00   68
  7  ω    -34.00  67.00   1.00    1.04    --   37.20 -19.00  60.00  101
  8  ω      3.00  29.00   1.00    1.04    --   37.20  91.00-179.89   26
  9  ω    100.00 178.00   1.00    4.18    --  111.00 111.00-180.00   78
 10  ω     44.00 131.00   1.00    4.18    --  111.00 -64.00 -90.00   87
 11  ω     94.00 178.00   1.00    4.18    --  111.00  50.00  90.00   84
 12  ω     42.00 146.00   1.00    4.18    --  111.00 -92.00  30.00  104
 13  ω     94.00 178.00   1.00    4.18    --  111.00  50.00 120.00   84
 14  ω     94.00 178.00   1.00    4.18    --  111.00  50.00  60.00   84
 15  ω     65.00 178.00   1.00    4.18    --  111.00  12.00  30.00  113
 16  ω     86.00 178.00   1.00    4.18    --  111.00  25.00-180.00   92
 17  ω    100.00 178.00   1.00    4.18    --  111.00 111.00 -30.00   78
 18  ω     47.00 114.00   1.00    4.18    --  111.00-111.00 -30.00   67
 19  ω     42.00 136.00   1.00    4.18    --  111.00 -25.00 150.00   94
 20  ω     47.00  74.00   1.00    4.18    --  111.00 -77.00 -90.00   27
 21  ω     85.00 123.00   1.00    4.18    --  111.00 -77.00 -90.00   38
 22  ω     95.00 122.00   1.00    4.18    --  111.00  34.00-150.77   27
 23  ω    136.00 176.00   1.00    4.18    --  111.00  34.00-150.77   40
 24  ω     44.00 126.00   1.00    4.18    --  111.00 -64.00 120.00   82
 25  ω     54.00 125.00   1.00    4.18    --  111.00 -38.00-150.00   71
 26  ω    124.00 175.00   1.00    4.18    --  111.00  25.00 150.00   51
 27  ω     87.00 112.00   1.00    4.18    --  111.00  77.00  30.00   25
 28  ω    118.00 145.00   1.00    4.18    --  111.00  31.00 107.61   27
 29  ω     68.00  95.00   1.00    4.18    --  111.00 -77.00-180.00   27
 30  ω    100.00 125.00   1.00    4.18    --  111.00 -77.00-180.00   25
 31  ω     49.00  86.00   1.00    4.18    --  111.00 -77.00 -60.00   37
 32  ω    115.00 142.00   1.00    4.18    --  111.00 111.00-150.00   27
 33  ω     43.00 115.00   1.00    4.18    --  111.00 -25.00 -60.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0886764000
_diffrn_orient_matrix_UB_12      -0.0775459000
_diffrn_orient_matrix_UB_13      0.0016529000
_diffrn_orient_matrix_UB_21      0.0379222000
_diffrn_orient_matrix_UB_22      -0.0032055000
_diffrn_orient_matrix_UB_23      0.0640550000
_diffrn_orient_matrix_UB_31      -0.1113002000
_diffrn_orient_matrix_UB_32      0.0606892000
_diffrn_orient_matrix_UB_33      0.0054000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7401
_reflns_number_total             8049
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0356
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+8.3595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0975
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H10), C10(H18), C22(H4), C28(H0AA)
2.b Secondary CH2 refined with riding coordinates:
 C18(H7a,H7b), C15(H9a,H9b), C21(H12a,H12b), C20(H13a,H13b), C17(H32a,H32b),
 C19(H35a,H35b), C12(H37a,H37b), C11(H42a,H42b), C13(H45a,H45b), C14(H51a,H51b),
  C27(H5a,H5b), C8(H6a,H6b), C29(H1Ab,H1Aa), C9(H11a,H11b), C33(H2Aa,H2Ab),
 C23(H16a,H16b), C30(H17a,H17b), C24(H5Aa,H5Ab), C32(H19a,H19b), C31(H20a,H20b),
  C26(H21a,H21b), C25(H22a,H22b)
2.c Aromatic/amide H refined with riding coordinates:
 C38(H25), C39(H33), C35(H44), C37(H50), C36(H61)
2.d Idealised Me refined as rotating group:
 C5(H4Aa,H4Ab,H4Ac), C3(H15a,H15b,H15c), C4(H23a,H23b,H23c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.42819(2) 0.30106(2) 0.70609(2) 0.02758(7) Uani 1 1 d . . . . .
Te2 Te 0.67633(2) 0.38306(2) 0.70438(2) 0.03486(8) Uani 1 1 d . . . . .
P3 P 0.54593(9) 0.22328(7) 0.79189(4) 0.02778(19) Uani 1 1 d . . . . .
P4 P 0.48570(9) 0.15862(7) 0.66376(4) 0.0290(2) Uani 1 1 d . . . . .
C7 C 0.8056(4) 0.1486(3) 0.5831(2) 0.0391(10) Uani 1 1 d . . . . .
H7A H 0.8964 0.1510 0.5981 0.047 Uiso 1 1 calc R . . . .
H7B H 0.7879 0.0937 0.5649 0.047 Uiso 1 1 calc R . . . .
C9 C 0.2572(4) 0.1279(3) 0.58587(19) 0.0378(9) Uani 1 1 d . . . . .
H9A H 0.2332 0.1854 0.5949 0.045 Uiso 1 1 calc R . . . .
H9B H 0.3016 0.1314 0.5544 0.045 Uiso 1 1 calc R . . . .
C10 C 0.5867(4) 0.1548(3) 0.60843(16) 0.0312(8) Uani 1 1 d . . . . .
H10 H 0.5671 0.1013 0.5877 0.037 Uiso 1 1 calc R . . . .
C12 C 0.5541(4) 0.2287(3) 0.56690(17) 0.0358(9) Uani 1 1 d . . . . .
H12A H 0.4632 0.2279 0.5520 0.043 Uiso 1 1 calc R . . . .
H12B H 0.5740 0.2826 0.5862 0.043 Uiso 1 1 calc R . . . .
C13 C 0.6292(5) 0.2217(4) 0.51884(19) 0.0432(10) Uani 1 1 d . . . . .
H13A H 0.6036 0.1702 0.4976 0.052 Uiso 1 1 calc R . . . .
H13B H 0.6091 0.2703 0.4941 0.052 Uiso 1 1 calc R . . . .
C14 C 0.6433(4) 0.4659(3) 0.63377(18) 0.0345(9) Uani 1 1 d . . . . .
C18 C 0.3465(4) 0.0894(3) 0.63616(17) 0.0320(8) Uani 1 1 d . . . . .
H18 H 0.2960 0.0848 0.6661 0.038 Uiso 1 1 calc R . . . .
C25 C 0.7038(6) 0.5164(4) 0.5484(2) 0.0489(12) Uani 1 1 d . . . . .
H25 H 0.7558 0.5117 0.5215 0.059 Uiso 1 1 calc R . . . .
C32 C 0.7308(4) 0.1554(3) 0.63137(18) 0.0346(9) Uani 1 1 d . . . . .
H32A H 0.7537 0.2078 0.6520 0.042 Uiso 1 1 calc R . . . .
H32B H 0.7524 0.1076 0.6567 0.042 Uiso 1 1 calc R . . . .
C33 C 0.7195(5) 0.4597(3) 0.5932(2) 0.0408(10) Uani 1 1 d . . . . .
H33 H 0.7818 0.4174 0.5960 0.049 Uiso 1 1 calc R . . . .
C35 C 0.7722(4) 0.2192(3) 0.5402(2) 0.0407(10) Uani 1 1 d . . . . .
H35A H 0.8000 0.2738 0.5570 0.049 Uiso 1 1 calc R . . . .
H35B H 0.8168 0.2096 0.5093 0.049 Uiso 1 1 calc R . . . .
C37 C 0.2605(4) -0.0578(3) 0.6062(2) 0.0404(10) Uani 1 1 d . . . . .
H37A H 0.2848 -0.1146 0.5961 0.048 Uiso 1 1 calc R . . . .
H37B H 0.2174 -0.0630 0.6380 0.048 Uiso 1 1 calc R . . . .
C42 C 0.3810(4) -0.0026(3) 0.62233(19) 0.0365(9) Uani 1 1 d . . . . .
H42A H 0.4356 -0.0275 0.6545 0.044 Uiso 1 1 calc R . . . .
H42B H 0.4282 -0.0017 0.5917 0.044 Uiso 1 1 calc R . . . .
C44 C 0.5527(5) 0.5305(3) 0.6295(2) 0.0468(11) Uani 1 1 d . . . . .
H44 H 0.5027 0.5367 0.6570 0.056 Uiso 1 1 calc R . . . .
C45 C 0.1695(5) -0.0183(4) 0.5574(2) 0.0441(11) Uani 1 1 d . . . . .
H45A H 0.2089 -0.0194 0.5243 0.053 Uiso 1 1 calc R . . . .
H45B H 0.0917 -0.0519 0.5497 0.053 Uiso 1 1 calc R . . . .
C50 C 0.6118(6) 0.5792(4) 0.5435(2) 0.0510(12) Uani 1 1 d . . . . .
H50 H 0.6003 0.6166 0.5133 0.061 Uiso 1 1 calc R . . . .
C51 C 0.1370(4) 0.0732(4) 0.5701(2) 0.0461(11) Uani 1 1 d . . . . .
H51A H 0.0894 0.0735 0.6006 0.055 Uiso 1 1 calc R . . . .
H51B H 0.0830 0.0977 0.5377 0.055 Uiso 1 1 calc R . . . .
C61 C 0.5369(5) 0.5858(4) 0.5844(3) 0.0539(13) Uani 1 1 d . . . . .
H61 H 0.4746 0.6281 0.5815 0.065 Uiso 1 1 calc R . . . .
C3 C 0.2618(4) 0.2779(3) 0.70989(17) 0.0328(8) Uani 1 1 d . . . . .
C4 C 0.4336(4) 0.1601(3) 0.82718(17) 0.0331(8) Uani 1 1 d . . . . .
H4 H 0.3699 0.1348 0.7976 0.040 Uiso 1 1 calc R . . . .
C5 C 0.3613(4) 0.2204(3) 0.86043(19) 0.0367(9) Uani 1 1 d . . . . .
H5A H 0.4214 0.2476 0.8899 0.044 Uiso 1 1 calc R . . . .
H5B H 0.3196 0.2648 0.8359 0.044 Uiso 1 1 calc R . . . .
C6 C 0.5687(4) 0.0890(3) 0.72095(17) 0.0324(8) Uani 1 1 d . . . . .
H6A H 0.5058 0.0560 0.7363 0.039 Uiso 1 1 calc R . . . .
H6B H 0.6239 0.0492 0.7059 0.039 Uiso 1 1 calc R . . . .
C0AA C 0.6509(4) 0.2762(3) 0.85129(16) 0.0320(8) Uani 1 1 d . . . . .
H0AA H 0.6452 0.2419 0.8845 0.038 Uiso 1 1 calc R . . . .
C3AA C 0.1212(4) 0.2791(3) 0.71021(19) 0.0360(9) Uani 1 1 d . . . . .
C1AA C 0.6030(4) 0.3662(3) 0.86269(19) 0.0378(9) Uani 1 1 d . . . . .
H1AB H 0.6132 0.4040 0.8322 0.045 Uiso 1 1 calc R . . . .
H1AA H 0.5129 0.3638 0.8649 0.045 Uiso 1 1 calc R . . . .
C11 C 0.6484(4) 0.1418(3) 0.76734(17) 0.0317(8) Uani 1 1 d . . . . .
H11A H 0.7182 0.1693 0.7533 0.038 Uiso 1 1 calc R . . . .
H11B H 0.6845 0.1048 0.7981 0.038 Uiso 1 1 calc R . . . .
C2AA C 0.7924(4) 0.2800(3) 0.84709(19) 0.0395(10) Uani 1 1 d . . . . .
H2AA H 0.8031 0.3142 0.8149 0.047 Uiso 1 1 calc R . . . .
H2AB H 0.8233 0.2228 0.8418 0.047 Uiso 1 1 calc R . . . .
C4AA C 0.0505(5) 0.3057(4) 0.6525(2) 0.0473(12) Uani 1 1 d . . . . .
H4AA H 0.0795 0.3611 0.6434 0.071 Uiso 1 1 calc GR . . . .
H4AB H -0.0397 0.3077 0.6527 0.071 Uiso 1 1 calc GR . . . .
H4AC H 0.0673 0.2649 0.6252 0.071 Uiso 1 1 calc GR . . . .
C15 C 0.0760(5) 0.1891(4) 0.7240(2) 0.0488(12) Uani 1 1 d . . . . .
H15A H 0.0958 0.1490 0.6969 0.073 Uiso 1 1 calc GR . . . .
H15B H -0.0147 0.1899 0.7231 0.073 Uiso 1 1 calc GR . . . .
H15C H 0.1187 0.1725 0.7605 0.073 Uiso 1 1 calc GR . . . .
C16 C 0.4944(5) 0.0866(3) 0.8636(2) 0.0430(10) Uani 1 1 d . . . . .
H16A H 0.5607 0.1088 0.8926 0.052 Uiso 1 1 calc R . . . .
H16B H 0.5339 0.0471 0.8410 0.052 Uiso 1 1 calc R . . . .
C17 C 0.6777(5) 0.4014(3) 0.9170(2) 0.0434(10) Uani 1 1 d . . . . .
H17A H 0.6654 0.3646 0.9478 0.052 Uiso 1 1 calc R . . . .
H17B H 0.6463 0.4579 0.9239 0.052 Uiso 1 1 calc R . . . .
C5AA C 0.3943(6) 0.0387(4) 0.8905(2) 0.0518(12) Uani 1 1 d . . . . .
H5AA H 0.3345 0.0102 0.8616 0.062 Uiso 1 1 calc R . . . .
H5AB H 0.4368 -0.0048 0.9156 0.062 Uiso 1 1 calc R . . . .
C19 C 0.8713(5) 0.3193(4) 0.9001(2) 0.0445(11) Uani 1 1 d . . . . .
H19A H 0.8703 0.2807 0.9312 0.053 Uiso 1 1 calc R . . . .
H19B H 0.9593 0.3255 0.8949 0.053 Uiso 1 1 calc R . . . .
C20 C 0.8205(5) 0.4062(4) 0.9140(2) 0.0471(11) Uani 1 1 d . . . . .
H20A H 0.8334 0.4473 0.8856 0.057 Uiso 1 1 calc R . . . .
H20B H 0.8677 0.4258 0.9495 0.057 Uiso 1 1 calc R . . . .
C21 C 0.2608(5) 0.1714(4) 0.8861(2) 0.0458(11) Uani 1 1 d . . . . .
H21A H 0.2194 0.2102 0.9084 0.055 Uiso 1 1 calc R . . . .
H21B H 0.1960 0.1489 0.8566 0.055 Uiso 1 1 calc R . . . .
C22 C 0.3218(6) 0.0981(4) 0.9226(2) 0.0535(13) Uani 1 1 d . . . . .
H22A H 0.3798 0.1211 0.9544 0.064 Uiso 1 1 calc R . . . .
H22B H 0.2558 0.0662 0.9366 0.064 Uiso 1 1 calc R . . . .
C23 C 0.0915(5) 0.3439(4) 0.7542(3) 0.0604(16) Uani 1 1 d . . . . .
H23A H 0.1344 0.3268 0.7906 0.091 Uiso 1 1 calc GR . . . .
H23B H 0.0010 0.3456 0.7537 0.091 Uiso 1 1 calc GR . . . .
H23C H 0.1207 0.3997 0.7458 0.091 Uiso 1 1 calc GR . . . .
O1 O 0.3204(4) 0.3808(3) 0.58828(14) 0.0493(9) Uani 1 1 d . . . . .
O2 O 0.3749(4) 0.4774(2) 0.76243(17) 0.0522(9) Uani 1 1 d . . . . .
C6AA C 0.3631(4) 0.3520(3) 0.63060(18) 0.0340(9) Uani 1 1 d . . . . .
C7AA C 0.3989(4) 0.4137(3) 0.74305(19) 0.0373(9) 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
W1 Te2 2.9393(3) . ?
W1 P3 2.5464(10) . ?
W1 P4 2.5730(11) . ?
W1 C3 1.823(5) . ?
W1 C6AA 2.010(4) . ?
W1 C7AA 2.027(5) . ?
Te2 C14 2.131(4) . ?
P3 C4 1.871(4) . ?
P3 C0AA 1.857(4) . ?
P3 C11 1.843(4) . ?
P4 C10 1.866(4) . ?
P4 C18 1.860(4) . ?
P4 C6 1.863(4) . ?
C7 C32 1.534(6) . ?
C7 C35 1.518(7) . ?
C9 C18 1.534(6) . ?
C9 C51 1.530(6) . ?
C10 C12 1.534(6) . ?
C10 C32 1.534(5) . ?
C12 C13 1.532(6) . ?
C13 C35 1.518(7) . ?
C14 C33 1.385(6) . ?
C14 C44 1.387(7) . ?
C18 C42 1.536(6) . ?
C25 C33 1.393(7) . ?
C25 C50 1.377(8) . ?
C37 C42 1.537(6) . ?
C37 C45 1.524(7) . ?
C44 C61 1.384(7) . ?
C45 C51 1.517(7) . ?
C50 C61 1.384(8) . ?
C3 C3AA 1.496(6) . ?
C4 C5 1.535(6) . ?
C4 C16 1.524(6) . ?
C5 C21 1.534(6) . ?
C6 C11 1.529(6) . ?
C0AA C1AA 1.539(6) . ?
C0AA C2AA 1.527(6) . ?
C3AA C4AA 1.529(7) . ?
C3AA C15 1.543(7) . ?
C3AA C23 1.548(6) . ?
C1AA C17 1.520(6) . ?
C2AA C19 1.537(6) . ?
C16 C5AA 1.538(7) . ?
C17 C20 1.534(7) . ?
C5AA C22 1.510(8) . ?
C19 C20 1.523(8) . ?
C21 C22 1.524(8) . ?
O1 C6AA 1.142(6) . ?
O2 C7AA 1.149(6) . ?

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
P3 W1 Te2 84.71(2) . . ?
P3 W1 P4 78.33(3) . . ?
P4 W1 Te2 95.46(2) . . ?
C3 W1 Te2 165.47(14) . . ?
C3 W1 P3 101.78(13) . . ?
C3 W1 P4 98.58(14) . . ?
C3 W1 C6AA 86.82(18) . . ?
C3 W1 C7AA 85.66(19) . . ?
C6AA W1 Te2 88.81(13) . . ?
C6AA W1 P3 168.25(12) . . ?
C6AA W1 P4 92.58(13) . . ?
C6AA W1 C7AA 90.34(18) . . ?
C7AA W1 Te2 80.52(13) . . ?
C7AA W1 P3 98.22(13) . . ?
C7AA W1 P4 174.98(13) . . ?
C14 Te2 W1 104.84(12) . . ?
C4 P3 W1 111.58(14) . . ?
C0AA P3 W1 124.48(15) . . ?
C0AA P3 C4 102.83(19) . . ?
C11 P3 W1 107.31(13) . . ?
C11 P3 C4 104.2(2) . . ?
C11 P3 C0AA 104.63(19) . . ?
C10 P4 W1 121.63(15) . . ?
C18 P4 W1 114.76(14) . . ?
C18 P4 C10 104.06(18) . . ?
C18 P4 C6 99.83(19) . . ?
C6 P4 W1 108.77(14) . . ?
C6 P4 C10 105.30(19) . . ?
C35 C7 C32 112.7(4) . . ?
C51 C9 C18 110.6(4) . . ?
C12 C10 P4 111.1(3) . . ?
C32 C10 P4 113.7(3) . . ?
C32 C10 C12 109.3(4) . . ?
C13 C12 C10 111.2(4) . . ?
C35 C13 C12 111.4(4) . . ?
C33 C14 Te2 119.9(3) . . ?
C33 C14 C44 118.9(4) . . ?
C44 C14 Te2 121.1(3) . . ?
C9 C18 P4 113.6(3) . . ?
C9 C18 C42 109.3(3) . . ?
C42 C18 P4 114.8(3) . . ?
C50 C25 C33 120.4(5) . . ?
C7 C32 C10 109.9(3) . . ?
C14 C33 C25 120.6(5) . . ?
C13 C35 C7 110.7(4) . . ?
C45 C37 C42 110.9(4) . . ?
C18 C42 C37 111.2(4) . . ?
C61 C44 C14 120.0(5) . . ?
C51 C45 C37 111.0(4) . . ?
C25 C50 C61 118.8(5) . . ?
C45 C51 C9 111.7(4) . . ?
C50 C61 C44 121.3(5) . . ?
C3AA C3 W1 167.5(4) . . ?
C5 C4 P3 109.7(3) . . ?
C16 C4 P3 115.2(3) . . ?
C16 C4 C5 110.9(4) . . ?
C21 C5 C4 110.9(4) . . ?
C11 C6 P4 111.3(3) . . ?
C1AA C0AA P3 112.1(3) . . ?
C2AA C0AA P3 115.4(3) . . ?
C2AA C0AA C1AA 109.7(4) . . ?
C3 C3AA C4AA 109.2(4) . . ?
C3 C3AA C15 109.8(4) . . ?
C3 C3AA C23 109.7(4) . . ?
C4AA C3AA C15 109.0(4) . . ?
C4AA C3AA C23 109.3(4) . . ?
C15 C3AA C23 109.8(5) . . ?
C17 C1AA C0AA 110.4(4) . . ?
C6 C11 P3 109.3(3) . . ?
C0AA C2AA C19 111.0(4) . . ?
C4 C16 C5AA 111.2(4) . . ?
C1AA C17 C20 110.2(4) . . ?
C22 C5AA C16 112.0(5) . . ?
C20 C19 C2AA 112.4(4) . . ?
C19 C20 C17 111.1(4) . . ?
C22 C21 C5 111.0(4) . . ?
C5AA C22 C21 111.4(4) . . ?
O1 C6AA W1 176.8(4) . . ?
O2 C7AA W1 175.9(4) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.926
_oxdiff_exptl_absorpt_empirical_full_min 0.697

####################################################################### 
# 
# 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_Compound_5a
_database_code_depnum_ccdc_archive 'CCDC 1515559'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-06-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H57 Cl O2 P2 W'
_chemical_formula_sum            'C33 H57 Cl O2 P2 W'
_chemical_formula_weight         767.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.90249(14)
_cell_length_b                   14.24490(18)
_cell_length_c                   22.5025(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.8393(13)
_cell_angle_gamma                90
_cell_volume                     3462.09(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21562
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.2980
_cell_measurement_theta_min      3.6460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.1216
_exptl_crystal_size_mid          0.0731
_exptl_crystal_size_min          0.0175
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45483
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.434
_diffrn_reflns_theta_min         3.682
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   41.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000  -90.0000 56

#__ type_ start__ end____ width___ exp.time_
  2 omega   24.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   77.0000  150.0000 80

#__ type_ start__ end____ width___ exp.time_
  3 omega  -22.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -38.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
  5 omega    5.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
  6 omega  -30.00   53.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -38.0000    0.0000 83

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000   60.0000 31

#__ type_ start__ end____ width___ exp.time_
  8 omega   39.00  102.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000  120.0000 63

#__ type_ start__ end____ width___ exp.time_
  9 omega  -17.00   14.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000 -150.0000 31

#__ type_ start__ end____ width___ exp.time_
 10 omega   42.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000 -120.0000 47

#__ type_ start__ end____ width___ exp.time_
 11 omega   37.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 65

#__ type_ start__ end____ width___ exp.time_
 12 omega  120.00  165.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 45

#__ type_ start__ end____ width___ exp.time_
 13 omega   42.00   85.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
 14 omega   58.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 35

#__ type_ start__ end____ width___ exp.time_
 16 omega   45.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
 17 omega   42.00   80.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -82.0000  -14.3653 38

#__ type_ start__ end____ width___ exp.time_
 18 omega   70.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 44

#__ type_ start__ end____ width___ exp.time_
 19 omega   69.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 20 omega   90.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 31

#__ type_ start__ end____ width___ exp.time_
 21 omega   62.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -30.0000 43

#__ type_ start__ end____ width___ exp.time_
 22 omega   69.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
 23 omega  105.00  146.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
 24 omega  153.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 25 omega   60.00   85.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   60.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 27 omega   90.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 34

#__ type_ start__ end____ width___ exp.time_
 28 omega   53.00   78.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 29 omega   80.00  164.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
 30 omega   98.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 31 omega   82.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 32 omega   62.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -32.0000 -162.3212 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   44.00   80.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 36

#__ type_ start__ end____ width___ exp.time_
 34 omega  101.00  126.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 35 omega  143.00  168.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 36 omega   71.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   38.00   71.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 33

#__ type_ start__ end____ width___ exp.time_
 38 omega   76.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 38

#__ type_ start__ end____ width___ exp.time_
 39 omega   48.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 40 omega  147.00  172.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 41 omega   59.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 31

#__ type_ start__ end____ width___ exp.time_
 42 omega   45.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 41

#__ type_ start__ end____ width___ exp.time_
 43 omega   79.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
 44 omega  119.00  149.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
 45 omega  148.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 46 omega  116.00  145.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   30.0000 29

#__ type_ start__ end____ width___ exp.time_
 47 omega   54.00   91.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 37

#__ type_ start__ end____ width___ exp.time_
 48 omega   52.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
 49 omega  143.00  169.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 50 omega   65.00   91.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  129.5453 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   71.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 50

#__ type_ start__ end____ width___ exp.time_
 52 omega   46.00   76.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 30

#__ type_ start__ end____ width___ exp.time_
 53 omega  113.00  145.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 54 omega   49.00   78.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 55 omega  120.00  145.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 56 omega   69.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 57 omega  111.00  144.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
 58 omega   41.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 49

#__ type_ start__ end____ width___ exp.time_
 59 omega   68.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 45

#__ type_ start__ end____ width___ exp.time_
 60 omega   44.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 46

#__ type_ start__ end____ width___ exp.time_
 61 omega   71.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 62 omega  102.00  142.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
 63 omega  100.00  131.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
 64 omega  118.00  144.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   82.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 66 omega   41.00   66.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 67 omega   92.00  118.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 68 omega   86.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 69 omega   77.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 70 omega   49.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 71 omega  100.00  134.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -82.0000  -14.3653 34

#__ type_ start__ end____ width___ exp.time_
 72 omega   92.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -81.0000  137.7715 27

#__ type_ start__ end____ width___ exp.time_
 73 omega   73.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   -7.0000  -52.9283 34

#__ type_ start__ end____ width___ exp.time_
 74 omega   41.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -81.0000  137.7715 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_orient_matrix_UB_11      -0.0656321000
_diffrn_orient_matrix_UB_12      0.0006121000
_diffrn_orient_matrix_UB_13      -0.0651273000
_diffrn_orient_matrix_UB_21      0.0142948000
_diffrn_orient_matrix_UB_22      -0.1073961000
_diffrn_orient_matrix_UB_23      -0.0030221000
_diffrn_orient_matrix_UB_31      -0.1259205000
_diffrn_orient_matrix_UB_32      -0.0124880000
_diffrn_orient_matrix_UB_33      0.0228709000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6335
_reflns_number_total             6760
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         4.354
_refine_diff_density_min         -2.063
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     173
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²+52.3005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1507
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C43 = C44-C45
 1.53 with sigma of 0.01
 C46-C45
 1.53 with sigma of 0.01
 C24-H24A
 0.95 with sigma of 0.01
 C53-H53A
 0.95 with sigma of 0.01
3. Rigid bond restraints
 C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(W1) = Uanis(C1)
5. Others
 Fixed Sof: C31(0.5) H31(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) C41(0.5) H41(0.5) C42(0.5) H42A(0.5) H42B(0.5) C43(0.5)
 H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5) H45B(0.5)
 C46(0.5) H46A(0.5) H46B(0.5) C51(0.5) H51(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5)
 H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) C61(0.5) H61(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C65(0.5)
 H65A(0.5) H65B(0.5) C66(0.5) H66A(0.5) H66B(0.5)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C51(H51), C61(H61)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B),
  C26(H26A,H26B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B), C46(H46A,H46B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B),
  C56(H56A,H56B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C66(H66A,H66B)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.52082(4) 0.48614(2) 0.70958(2) 0.02911(13) Uani 1 1 d . . . . .
Cl1 Cl 0.7461(2) 0.42980(18) 0.71032(10) 0.0496(6) Uani 1 1 d . . . . .
P1 P 0.58741(18) 0.63023(13) 0.65425(8) 0.0247(4) Uani 1 1 d . . . . .
P2 P 0.5884(2) 0.59431(14) 0.79788(9) 0.0286(4) Uani 1 1 d . . . . .
O2 O 0.4451(8) 0.3701(6) 0.5908(3) 0.062(2) Uani 1 1 d . . . . .
O3 O 0.4964(9) 0.3046(5) 0.7872(4) 0.068(2) Uani 1 1 d . . . . .
C1 C 0.3624(8) 0.4995(5) 0.7084(3) 0.02911(13) Uani 1 1 d . . . . .
C2 C 0.4766(10) 0.4115(7) 0.6324(4) 0.045(2) Uani 1 1 d . . . . .
C3 C 0.5060(11) 0.3701(7) 0.7597(4) 0.048(2) Uani 1 1 d . . . . .
C4 C 0.6485(8) 0.7193(6) 0.7105(3) 0.0305(17) Uani 1 1 d . . . . .
H4A H 0.7369 0.7101 0.7211 0.037 Uiso 1 1 calc R . . . .
H4B H 0.6356 0.7813 0.6930 0.037 Uiso 1 1 calc R . . . .
C5 C 0.5865(8) 0.7140(5) 0.7672(3) 0.0292(16) Uani 1 1 d . . . . .
H5A H 0.5014 0.7352 0.7581 0.035 Uiso 1 1 calc R . . . .
H5B H 0.6289 0.7559 0.7972 0.035 Uiso 1 1 calc R . . . .
C6 C 0.2218(9) 0.4934(7) 0.7052(4) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.1533(12) 0.5829(10) 0.7231(7) 0.078(4) Uani 1 1 d . . . . .
H7A H 0.1856 0.6008 0.7633 0.117 Uiso 1 1 calc GR . . . .
H7B H 0.0664 0.5700 0.7208 0.117 Uiso 1 1 calc GR . . . .
H7C H 0.1658 0.6332 0.6961 0.117 Uiso 1 1 calc GR . . . .
C8 C 0.1840(13) 0.4164(10) 0.7479(7) 0.084(5) Uani 1 1 d . . . . .
H8A H 0.2104 0.3562 0.7353 0.126 Uiso 1 1 calc GR . . . .
H8B H 0.0956 0.4165 0.7467 0.126 Uiso 1 1 calc GR . . . .
H8C H 0.2224 0.4289 0.7881 0.126 Uiso 1 1 calc GR . . . .
C9 C 0.1606(12) 0.4669(11) 0.6407(5) 0.072(4) Uani 1 1 d . . . . .
H9A H 0.1627 0.5202 0.6147 0.108 Uiso 1 1 calc GR . . . .
H9B H 0.0762 0.4485 0.6417 0.108 Uiso 1 1 calc GR . . . .
H9C H 0.2051 0.4158 0.6259 0.108 Uiso 1 1 calc GR . . . .
C11 C 0.4738(7) 0.6979(6) 0.6024(4) 0.0299(16) Uani 1 1 d . . . . .
H11 H 0.5184 0.7502 0.5869 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3738(9) 0.7400(7) 0.6357(4) 0.039(2) Uani 1 1 d . . . . .
H12A H 0.4125 0.7797 0.6680 0.047 Uiso 1 1 calc R . . . .
H12B H 0.3307 0.6899 0.6534 0.047 Uiso 1 1 calc R . . . .
C13 C 0.2801(9) 0.7981(7) 0.5940(5) 0.047(2) Uani 1 1 d . . . . .
H13A H 0.2139 0.8181 0.6158 0.057 Uiso 1 1 calc R . . . .
H13B H 0.3207 0.8540 0.5815 0.057 Uiso 1 1 calc R . . . .
C14 C 0.2255(9) 0.7437(7) 0.5389(4) 0.043(2) Uani 1 1 d . . . . .
H14A H 0.1741 0.6932 0.5507 0.052 Uiso 1 1 calc R . . . .
H14B H 0.1736 0.7849 0.5119 0.052 Uiso 1 1 calc R . . . .
C15 C 0.3267(9) 0.7031(8) 0.5069(4) 0.044(2) Uani 1 1 d . . . . .
H15A H 0.3732 0.7539 0.4919 0.053 Uiso 1 1 calc R . . . .
H15B H 0.2897 0.6663 0.4728 0.053 Uiso 1 1 calc R . . . .
C16 C 0.4146(8) 0.6410(7) 0.5486(4) 0.038(2) Uani 1 1 d . . . . .
H16A H 0.3692 0.5885 0.5623 0.046 Uiso 1 1 calc R . . . .
H16B H 0.4787 0.6163 0.5270 0.046 Uiso 1 1 calc R . . . .
C21 C 0.7237(7) 0.6150(6) 0.6145(4) 0.0335(16) Uani 1 1 d . U . . .
H21 H 0.7902 0.5940 0.6454 0.040 Uiso 1 1 calc R . . . .
C22 C 0.7732(8) 0.7050(7) 0.5891(4) 0.0397(18) Uani 1 1 d . U . . .
H22A H 0.7159 0.7263 0.5549 0.048 Uiso 1 1 calc R . . . .
H22B H 0.7803 0.7538 0.6193 0.048 Uiso 1 1 calc R . . . .
C23 C 0.8994(9) 0.6865(9) 0.5696(5) 0.055(3) Uani 1 1 d . U . . .
H23A H 0.9287 0.7430 0.5521 0.066 Uiso 1 1 calc R . . . .
H23B H 0.9582 0.6702 0.6044 0.066 Uiso 1 1 calc R . . . .
C24 C 0.8922(11) 0.6073(12) 0.5243(6) 0.071(3) Uani 1 1 d D U . . .
H24A H 0.838(10) 0.621(10) 0.489(3) 0.085 Uiso 1 1 d DR . . . .
H24B H 0.980(13) 0.593(10) 0.518(6) 0.085 Uiso 1 1 d R . . . .
C25 C 0.8389(10) 0.5186(9) 0.5477(6) 0.064(3) Uani 1 1 d . U . . .
H25A H 0.8951 0.4948 0.5814 0.077 Uiso 1 1 calc R . . . .
H25B H 0.8308 0.4711 0.5164 0.077 Uiso 1 1 calc R . . . .
C26 C 0.7116(8) 0.5370(8) 0.5674(4) 0.046(2) Uani 1 1 d . U . . .
H26A H 0.6529 0.5556 0.5331 0.055 Uiso 1 1 calc R . . . .
H26B H 0.6811 0.4802 0.5841 0.055 Uiso 1 1 calc R . . . .
C31 C 0.516(2) 0.6000(14) 0.8660(8) 0.034(3) Uani 0.5 1 d . U P A 1
H31 H 0.5787 0.6233 0.8980 0.041 Uiso 0.5 1 calc R . P A 1
C32 C 0.473(2) 0.5089(17) 0.8857(11) 0.036(4) Uani 0.5 1 d . U P A 1
H32A H 0.5421 0.4657 0.8914 0.044 Uiso 0.5 1 calc R . P A 1
H32B H 0.4121 0.4837 0.8541 0.044 Uiso 0.5 1 calc R . P A 1
C33 C 0.415(2) 0.5140(15) 0.9436(9) 0.050(4) Uani 0.5 1 d . U P A 1
H33A H 0.3834 0.4528 0.9529 0.060 Uiso 0.5 1 calc R . P A 1
H33B H 0.4767 0.5329 0.9765 0.060 Uiso 0.5 1 calc R . P A 1
C34 C 0.313(2) 0.583(2) 0.9358(12) 0.054(4) Uani 0.5 1 d . U P A 1
H34A H 0.2811 0.5891 0.9738 0.064 Uiso 0.5 1 calc R . P A 1
H34B H 0.2470 0.5576 0.9070 0.064 Uiso 0.5 1 calc R . P A 1
C35 C 0.345(3) 0.6773(18) 0.9155(14) 0.050(5) Uani 0.5 1 d . U P A 1
H35A H 0.3989 0.7086 0.9474 0.060 Uiso 0.5 1 calc R . P A 1
H35B H 0.2706 0.7144 0.9063 0.060 Uiso 0.5 1 calc R . P A 1
C36 C 0.413(2) 0.6700(16) 0.8579(10) 0.047(4) Uani 0.5 1 d . U P A 1
H36A H 0.3538 0.6519 0.8237 0.056 Uiso 0.5 1 calc R . P A 1
H36B H 0.4462 0.7310 0.8494 0.056 Uiso 0.5 1 calc R . P A 1
C41 C 0.7614(18) 0.5739(12) 0.8278(9) 0.029(3) Uani 0.5 1 d . U P A 1
H41 H 0.8052 0.5637 0.7931 0.035 Uiso 0.5 1 calc R . P A 1
C42 C 0.7789(19) 0.483(3) 0.868(2) 0.033(5) Uani 0.5 1 d D U P A 1
H42A H 0.7346 0.4897 0.9026 0.040 Uiso 0.5 1 calc R . P A 1
H42B H 0.7452 0.4286 0.8454 0.040 Uiso 0.5 1 calc R . P A 1
C43 C 0.9166(19) 0.4671(14) 0.8898(10) 0.044(4) Uani 0.5 1 d D U P A 1
H43A H 0.9596 0.4548 0.8555 0.053 Uiso 0.5 1 calc R . P A 1
H43B H 0.9270 0.4129 0.9160 0.053 Uiso 0.5 1 calc R . P A 1
C44 C 0.973(2) 0.5546(14) 0.9238(10) 0.045(4) Uani 0.5 1 d D U P A 1
H44A H 0.9324 0.5655 0.9588 0.054 Uiso 0.5 1 calc R . P A 1
H44B H 1.0605 0.5436 0.9374 0.054 Uiso 0.5 1 calc R . P A 1
C45 C 0.9592(18) 0.6414(16) 0.8834(15) 0.041(5) Uani 0.5 1 d D U P A 1
H45A H 0.9966 0.6953 0.9051 0.049 Uiso 0.5 1 calc R . P A 1
H45B H 1.0013 0.6312 0.8486 0.049 Uiso 0.5 1 calc R . P A 1
C46 C 0.8218(15) 0.6604(12) 0.8630(9) 0.035(3) Uani 0.5 1 d D U P A 1
H46A H 0.8128 0.7156 0.8375 0.041 Uiso 0.5 1 calc R . P A 1
H46B H 0.7802 0.6724 0.8977 0.041 Uiso 0.5 1 calc R . P A 1
C51 C 0.458(2) 0.6097(12) 0.8469(9) 0.032(3) Uani 0.5 1 d . U P A 2
H51 H 0.3823 0.6135 0.8180 0.038 Uiso 0.5 1 calc R . P A 2
C52 C 0.459(2) 0.7020(12) 0.8833(9) 0.038(3) Uani 0.5 1 d . U P A 2
H52A H 0.5317 0.7030 0.9135 0.045 Uiso 0.5 1 calc R . P A 2
H52B H 0.4646 0.7550 0.8567 0.045 Uiso 0.5 1 calc R . P A 2
C53 C 0.346(3) 0.7120(17) 0.9132(14) 0.048(4) Uani 0.5 1 d D U P A 2
H53A H 0.281(14) 0.687(16) 0.885(8) 0.058 Uiso 0.5 1 d DR . P B 2
H53B H 0.33(2) 0.774(17) 0.923(10) 0.058 Uiso 0.5 1 d R . P C 2
C54 C 0.330(2) 0.6261(15) 0.9538(10) 0.045(4) Uani 0.5 1 d . U P A 2
H54A H 0.3974 0.6250 0.9867 0.054 Uiso 0.5 1 calc R . P A 2
H54B H 0.2532 0.6328 0.9707 0.054 Uiso 0.5 1 calc R . P A 2
C55 C 0.328(2) 0.5337(15) 0.9198(10) 0.045(4) Uani 0.5 1 d . U P A 2
H55A H 0.3300 0.4818 0.9479 0.054 Uiso 0.5 1 calc R . P A 2
H55B H 0.2517 0.5291 0.8921 0.054 Uiso 0.5 1 calc R . P A 2
C56 C 0.437(3) 0.5274(16) 0.8857(13) 0.037(4) Uani 0.5 1 d . U P A 2
H56A H 0.5111 0.5185 0.9144 0.044 Uiso 0.5 1 calc R . P A 2
H56B H 0.4272 0.4718 0.8606 0.044 Uiso 0.5 1 calc R . P A 2
C61 C 0.7261(18) 0.5861(13) 0.8503(10) 0.033(4) Uani 0.5 1 d . U P A 2
H61 H 0.7105 0.6223 0.8855 0.039 Uiso 0.5 1 calc R . P A 2
C62 C 0.8380(18) 0.6287(16) 0.8296(10) 0.046(4) Uani 0.5 1 d . U P A 2
H62A H 0.8234 0.6952 0.8225 0.055 Uiso 0.5 1 calc R . P A 2
H62B H 0.8511 0.6001 0.7919 0.055 Uiso 0.5 1 calc R . P A 2
C63 C 0.956(2) 0.6160(18) 0.8755(15) 0.045(7) Uani 0.5 1 d . U P A 2
H63A H 1.0275 0.6352 0.8570 0.054 Uiso 0.5 1 calc R . P A 2
H63B H 0.9511 0.6570 0.9095 0.054 Uiso 0.5 1 calc R . P A 2
C64 C 0.976(2) 0.516(2) 0.8979(13) 0.056(6) Uani 0.5 1 d . U P A 2
H64A H 0.9980 0.4769 0.8658 0.068 Uiso 0.5 1 calc R . P A 2
H64B H 1.0432 0.5145 0.9306 0.068 Uiso 0.5 1 calc R . P A 2
C65 C 0.8630(19) 0.4782(16) 0.9186(11) 0.049(5) Uani 0.5 1 d . U P A 2
H65A H 0.8482 0.5112 0.9546 0.059 Uiso 0.5 1 calc R . P A 2
H65B H 0.8758 0.4124 0.9287 0.059 Uiso 0.5 1 calc R . P A 2
C66 C 0.751(2) 0.488(3) 0.871(2) 0.040(6) Uani 0.5 1 d . U P A 2
H66A H 0.7620 0.4490 0.8373 0.047 Uiso 0.5 1 calc R . P A 2
H66B H 0.6785 0.4649 0.8878 0.047 Uiso 0.5 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 Cl1 2.582(2) . ?
W1 P1 2.557(2) . ?
W1 P2 2.5429(19) . ?
W1 C1 1.734(9) . ?
W1 C2 2.038(10) . ?
W1 C3 2.019(10) . ?
P1 C4 1.851(8) . ?
P1 C11 1.852(8) . ?
P1 C21 1.850(8) . ?
P2 C5 1.839(8) . ?
P2 C31 1.816(18) . ?
P2 C41 1.936(18) . ?
P2 C51 1.926(19) . ?
P2 C61 1.782(19) . ?
O2 C2 1.119(12) . ?
O3 C3 1.132(12) . ?
C1 C6 1.527(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.524(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.558(17) . ?
C6 C8 1.550(14) . ?
C6 C9 1.559(13) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 H11 0.9800 . ?
C11 C12 1.527(11) . ?
C11 C16 1.525(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.532(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.514(14) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.512(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.528(12) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C21 H21 0.9800 . ?
C21 C22 1.532(13) . ?
C21 C26 1.528(11) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.522(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.515(16) . ?
C24 H24A 0.949(10) . ?
C24 H24B 1.01(14) . ?
C24 C25 1.52(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.537(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C31 H31 0.9800 . ?
C31 C32 1.47(3) . ?
C31 C36 1.49(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.53(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.47(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.48(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.58(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C41 H41 0.9800 . ?
C41 C42 1.59(4) . ?
C41 C46 1.56(2) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.530(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.55(3) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.530(10) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.529(10) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C51 H51 0.9800 . ?
C51 C52 1.55(2) . ?
C51 C56 1.50(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.49(3) . ?
C53 H53A 0.950(11) . ?
C53 H53B 0.9(2) . ?
C53 C54 1.55(3) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.52(3) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55 C56 1.51(3) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C61 H61 0.9800 . ?
C61 C62 1.49(3) . ?
C61 C66 1.49(5) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 C63 1.55(3) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.52(3) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C64 C65 1.47(3) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C66 1.52(4) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?

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
P1 W1 Cl1 85.39(8) . . ?
P2 W1 Cl1 90.54(7) . . ?
P2 W1 P1 79.79(6) . . ?
C1 W1 Cl1 168.2(3) . . ?
C1 W1 P1 104.6(3) . . ?
C1 W1 P2 97.3(2) . . ?
C1 W1 C2 85.7(4) . . ?
C1 W1 C3 86.7(4) . . ?
C2 W1 Cl1 87.6(3) . . ?
C2 W1 P1 93.1(3) . . ?
C2 W1 P2 172.7(3) . . ?
C3 W1 Cl1 83.7(3) . . ?
C3 W1 P1 168.1(3) . . ?
C3 W1 P2 95.5(3) . . ?
C3 W1 C2 91.2(4) . . ?
C4 P1 W1 108.4(3) . . ?
C4 P1 C11 102.8(4) . . ?
C11 P1 W1 121.0(3) . . ?
C21 P1 W1 116.2(3) . . ?
C21 P1 C4 100.0(4) . . ?
C21 P1 C11 105.6(4) . . ?
C5 P2 W1 106.3(3) . . ?
C5 P2 C41 103.3(6) . . ?
C5 P2 C51 97.9(6) . . ?
C31 P2 W1 125.0(6) . . ?
C31 P2 C5 106.9(7) . . ?
C31 P2 C41 103.1(9) . . ?
C41 P2 W1 110.2(6) . . ?
C51 P2 W1 111.0(6) . . ?
C61 P2 W1 127.3(7) . . ?
C61 P2 C5 105.9(7) . . ?
C61 P2 C51 104.5(10) . . ?
C6 C1 W1 170.2(7) . . ?
O2 C2 W1 175.7(10) . . ?
O3 C3 W1 179.0(10) . . ?
P1 C4 H4A 109.1 . . ?
P1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 P1 112.3(6) . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
P2 C5 H5A 109.2 . . ?
P2 C5 H5B 109.2 . . ?
C4 C5 P2 112.1(5) . . ?
C4 C5 H5A 109.2 . . ?
C4 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C1 C6 C7 117.0(9) . . ?
C1 C6 C8 111.2(8) . . ?
C1 C6 C9 111.0(8) . . ?
C7 C6 C9 106.2(10) . . ?
C8 C6 C7 104.0(10) . . ?
C8 C6 C9 106.8(10) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C11 H11 107.3 . . ?
C12 C11 P1 110.9(6) . . ?
C12 C11 H11 107.3 . . ?
C16 C11 P1 113.5(6) . . ?
C16 C11 H11 107.3 . . ?
C16 C11 C12 110.2(7) . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
C11 C12 C13 111.8(8) . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C12 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 C12 112.3(8) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 C13 110.8(8) . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C14 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
C14 C15 C16 111.4(8) . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C11 C16 C15 110.0(8) . . ?
C11 C16 H16A 109.7 . . ?
C11 C16 H16B 109.7 . . ?
C15 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
P1 C21 H21 104.9 . . ?
C22 C21 P1 115.4(6) . . ?
C22 C21 H21 104.9 . . ?
C26 C21 P1 114.9(6) . . ?
C26 C21 H21 104.9 . . ?
C26 C21 C22 110.6(8) . . ?
C21 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C23 C22 C21 109.9(8) . . ?
C23 C22 H22A 109.7 . . ?
C23 C22 H22B 109.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 C22 110.9(9) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C23 C24 H24A 113(9) . . ?
C23 C24 H24B 107(8) . . ?
C23 C24 C25 112.0(10) . . ?
H24A C24 H24B 115(10) . . ?
C25 C24 H24A 104(9) . . ?
C25 C24 H24B 107(8) . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C24 C25 C26 111.2(10) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C21 C26 C25 109.2(8) . . ?
C21 C26 H26A 109.9 . . ?
C21 C26 H26B 109.9 . . ?
C25 C26 H26A 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
P2 C31 H31 107.4 . . ?
C32 C31 P2 114.2(15) . . ?
C32 C31 H31 107.4 . . ?
C32 C31 C36 110.9(18) . . ?
C36 C31 P2 109.4(14) . . ?
C36 C31 H31 107.4 . . ?
C31 C32 H32A 108.8 . . ?
C31 C32 H32B 108.8 . . ?
C31 C32 C33 113.8(19) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.8 . . ?
C33 C32 H32B 108.8 . . ?
C32 C33 H33A 109.9 . . ?
C32 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C34 C33 C32 108.9(19) . . ?
C34 C33 H33A 109.9 . . ?
C34 C33 H33B 109.9 . . ?
C33 C34 H34A 108.3 . . ?
C33 C34 H34B 108.3 . . ?
C33 C34 C35 116(2) . . ?
H34A C34 H34B 107.4 . . ?
C35 C34 H34A 108.3 . . ?
C35 C34 H34B 108.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 C36 111(2) . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C31 C36 C35 111.9(19) . . ?
C31 C36 H36A 109.2 . . ?
C31 C36 H36B 109.2 . . ?
C35 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
P2 C41 H41 107.7 . . ?
C42 C41 P2 111.0(13) . . ?
C42 C41 H41 107.7 . . ?
C46 C41 P2 112.4(12) . . ?
C46 C41 H41 107.7 . . ?
C46 C41 C42 110.2(19) . . ?
C41 C42 H42A 109.7 . . ?
C41 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
C43 C42 C41 110(2) . . ?
C43 C42 H42A 109.7 . . ?
C43 C42 H42B 109.7 . . ?
C42 C43 H43A 109.6 . . ?
C42 C43 H43B 109.6 . . ?
C42 C43 C44 110(2) . . ?
H43A C43 H43B 108.1 . . ?
C44 C43 H43A 109.6 . . ?
C44 C43 H43B 109.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
C45 C44 C43 110.8(19) . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
C44 C45 H45A 109.7 . . ?
C44 C45 H45B 109.7 . . ?
H45A C45 H45B 108.2 . . ?
C46 C45 C44 109.7(17) . . ?
C46 C45 H45A 109.7 . . ?
C46 C45 H45B 109.7 . . ?
C41 C46 H46A 109.7 . . ?
C41 C46 H46B 109.7 . . ?
C45 C46 C41 109.9(17) . . ?
C45 C46 H46A 109.7 . . ?
C45 C46 H46B 109.7 . . ?
H46A C46 H46B 108.2 . . ?
P2 C51 H51 104.4 . . ?
C52 C51 P2 116.5(13) . . ?
C52 C51 H51 104.4 . . ?
C56 C51 P2 115.3(13) . . ?
C56 C51 H51 104.4 . . ?
C56 C51 C52 110.2(16) . . ?
C51 C52 H52A 109.2 . . ?
C51 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
C53 C52 C51 111.9(18) . . ?
C53 C52 H52A 109.2 . . ?
C53 C52 H52B 109.2 . . ?
C52 C53 H53A 105(10) . . ?
C52 C53 H53B 114(10) . . ?
C52 C53 C54 111(2) . . ?
H53A C53 H53B 110(10) . . ?
C54 C53 H53A 88(10) . . ?
C54 C53 H53B 125(10) . . ?
C53 C54 H54A 109.1 . . ?
C53 C54 H54B 109.1 . . ?
H54A C54 H54B 107.8 . . ?
C55 C54 C53 112.5(18) . . ?
C55 C54 H54A 109.1 . . ?
C55 C54 H54B 109.1 . . ?
C54 C55 H55A 109.6 . . ?
C54 C55 H55B 109.6 . . ?
H55A C55 H55B 108.1 . . ?
C56 C55 C54 110.4(18) . . ?
C56 C55 H55A 109.6 . . ?
C56 C55 H55B 109.6 . . ?
C51 C56 C55 116.4(18) . . ?
C51 C56 H56A 108.2 . . ?
C51 C56 H56B 108.2 . . ?
C55 C56 H56A 108.2 . . ?
C55 C56 H56B 108.2 . . ?
H56A C56 H56B 107.3 . . ?
P2 C61 H61 106.1 . . ?
C62 C61 P2 114.7(15) . . ?
C62 C61 H61 106.1 . . ?
C66 C61 P2 111.8(17) . . ?
C66 C61 H61 106.1 . . ?
C66 C61 C62 111(2) . . ?
C61 C62 H62A 109.0 . . ?
C61 C62 H62B 109.0 . . ?
C61 C62 C63 112.7(19) . . ?
H62A C62 H62B 107.8 . . ?
C63 C62 H62A 109.0 . . ?
C63 C62 H62B 109.0 . . ?
C62 C63 H63A 108.9 . . ?
C62 C63 H63B 108.9 . . ?
H63A C63 H63B 107.7 . . ?
C64 C63 C62 113(2) . . ?
C64 C63 H63A 108.9 . . ?
C64 C63 H63B 108.9 . . ?
C63 C64 H64A 109.3 . . ?
C63 C64 H64B 109.3 . . ?
H64A C64 H64B 108.0 . . ?
C65 C64 C63 111(2) . . ?
C65 C64 H64A 109.3 . . ?
C65 C64 H64B 109.3 . . ?
C64 C65 H65A 109.2 . . ?
C64 C65 H65B 109.2 . . ?
C64 C65 C66 112(3) . . ?
H65A C65 H65B 107.9 . . ?
C66 C65 H65A 109.2 . . ?
C66 C65 H65B 109.2 . . ?
C61 C66 C65 114(3) . . ?
C61 C66 H66A 108.8 . . ?
C61 C66 H66B 108.8 . . ?
C65 C66 H66A 108.8 . . ?
C65 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 0 0.0088 0.0000 -1.0000 -0.0002 -0.0006 0.1074 0.0125
0 1 0 0.0088 -0.0000 1.0000 0.0002 0.0006 -0.1074 -0.0125
0 0 1 0.0365 -0.0000 -0.0000 1.0000 -0.0651 -0.0030 0.0229
0 0 -1 0.0365 0.0000 0.0000 -1.0000 0.0651 0.0030 -0.0229
1 0 0 0.0564 1.0000 0.0000 0.0000 -0.0656 0.0143 -0.1259
-1 0 0 0.0564 -1.0000 -0.0000 -0.0000 0.0656 -0.0143 0.1259
3 1 -5 0.0576 3.0000 1.0000 -4.9999 0.1293 -0.0494 -0.5046
-4 0 -5 0.0495 -4.0000 0.0000 -5.0001 0.5882 -0.0421 0.3893


_ins_header                      
;
TITL RK01_scaled in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.902495  14.244903  22.502518  90.0000  97.8393  90.0000
ZERR    4.00   0.000143   0.000180   0.000301   0.0000   0.0013   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Cl W
UNIT 132.00 228.00 8.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_Compound_5b
_database_code_depnum_ccdc_archive 'CCDC 1515560'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C33 H56.03 Br O2 P2 W'
_chemical_formula_sum            'C33 H55 Br O2 P2 W'
_chemical_formula_weight         809.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C37 H66 O2 P2 W'
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'
Br Br -0.2901 2.4595 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8206(5)
_cell_length_b                   14.4920(5)
_cell_length_c                   22.3551(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.561(4)
_cell_angle_gamma                90
_cell_volume                     3482.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      23.1600
_cell_measurement_theta_min      3.4550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -9 28 0.0515
1 -20 -2 0.0536
-1 20 2 0.0536
-15 -3 10 0.2362
15 3 -10 0.2362
0 9 -28 0.0515

_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.103
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0002 -9.0000 27.9995 -0.0771 -0.0618 0.9917
1.0002 -20.0000 -2.0003 0.5128 -0.7485 0.3760
-1.0002 20.0000 2.0003 -0.5128 0.7485 -0.3760
-15.0001 -2.9999 10.0001 -0.8217 -0.5775 0.1503
15.0001 2.9999 -10.0001 0.8217 0.5775 -0.1503
-0.0002 9.0000 -27.9995 0.0771 0.0618 -0.9917

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51350
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.357
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00 -34.00   1.00    1.35    --  -11.07 178.00-120.00   64
  2  ω    -61.00  39.00   1.00    1.35    --   11.30 -57.00   0.00  100
  3  ω    -21.00  87.00   1.00    1.35    --   11.30  77.00 -90.00  108
  4  ω    -17.00  84.00   1.00    1.35    --   11.30  57.00 150.00  101
  5  ω    -39.00  62.00   1.00    1.35    --  -11.07  57.00-150.00  101
  6  ω   -100.00 -35.00   1.00    1.35    --  -11.07-178.00  30.00   65
  7  ω    -17.00  53.00   1.00    1.35    --   11.30  57.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0526290000
_diffrn_orient_matrix_UB_12      -0.0220226000
_diffrn_orient_matrix_UB_13      -0.0098311000
_diffrn_orient_matrix_UB_21      0.0375771000
_diffrn_orient_matrix_UB_22      0.0382949000
_diffrn_orient_matrix_UB_23      0.0101016000
_diffrn_orient_matrix_UB_31      0.0132914000
_diffrn_orient_matrix_UB_32      -0.0210046000
_diffrn_orient_matrix_UB_33      0.0286653000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4465
_reflns_number_total             6134
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C128) = Uanis(C129) = Uanis(C132) = Uanis(C131) = Uanis(C130)
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32)
3. Others
 Sof(C30)=Sof(H24C)=Sof(C28)=Sof(H27A)=Sof(C32)=Sof(H30D)=Sof(H30C)=Sof(C29)=
 Sof(H31C)=Sof(H31D)=Sof(C31)=Sof(H32C)=Sof(H1BF)=Sof(H1BE)=1-FVAR(1)
 Sof(C130)=Sof(H24A)=Sof(H24B)=Sof(C128)=Sof(H27)=Sof(C132)=Sof(H30A)=
 Sof(H30B)=Sof(C129)=Sof(H31A)=Sof(H31B)=Sof(C131)=Sof(H32A)=Sof(H32B)=
 Sof(H1AC)=Sof(H1AD)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H5), C16(H0AA), C22(H17), C128(H27), C28(H27A)
4.b Secondary CH2 refined with riding coordinates:
 C8(H3B,H3A), C9(H6B,H6A), C27(H3AA,H3AB), C21(H8A,H8B), C12(H10A,H10B),
 C13(H11A,H11B), C14(H2AA,H2AB), C11(H13A,H13B), C17(H14A,H14B), C15(H15A,H15B),
  C20(H16A,H16B), C18(H1AA,H1AB), C24(H19A,H19B), C23(H20A,H20B), C130(H24A,
 H24B), C19(H25A,H25B), C25(H26A,H26B), C26(H28A,H28B), C132(H30A,H30B),
 C129(H31A,H31B), C131(H32A,H32B), C32(H30D,H30C), C29(H31C,H31D), C33(H1AC,
 H1AD), C33(H1BF,H1BE)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H24C), C31(H32C)
4.d Idealised Me refined as rotating group:
 C4(H21A,H21B,H21C), C5(H22A,H22B,H22C), C3(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.01467(3) 0.51511(2) 0.70787(2) 0.02918(12) Uani 1 1 d . . . . .
Br2 Br 0.25221(8) 0.57582(6) 0.70684(4) 0.0497(2) Uani 1 1 d . . . . .
P4 P 0.08412(16) 0.37201(12) 0.65326(8) 0.0259(4) Uani 1 1 d . . . . .
P5 P 0.08028(17) 0.41041(12) 0.79733(8) 0.0296(4) Uani 1 1 d . . . . .
C3 C 0.1424(6) 0.2861(4) 0.7114(3) 0.0300(16) Uani 1 1 d . . . . .
H3B H 0.1314 0.2246 0.6944 0.036 Uiso 1 1 calc R . . . .
H3A H 0.2308 0.2958 0.7223 0.036 Uiso 1 1 calc R . . . .
O4 O -0.0118(6) 0.6951(4) 0.7849(3) 0.0685(19) Uani 1 1 d . . . . .
O5 O -0.0535(5) 0.6295(4) 0.5883(2) 0.0552(16) Uani 1 1 d . . . . .
C6 C 0.0770(6) 0.2917(4) 0.7675(3) 0.0282(16) Uani 1 1 d . . . . .
H6B H 0.1172 0.2505 0.7979 0.034 Uiso 1 1 calc R . . . .
H6A H -0.0087 0.2719 0.7581 0.034 Uiso 1 1 calc R . . . .
C7 C -0.1521(7) 0.4983(4) 0.7073(3) 0.0309(17) Uani 1 1 d . . . . .
C9 C -0.2908(7) 0.5094(5) 0.7050(3) 0.0397(19) Uani 1 1 d . . . . .
C12 C -0.0259(7) 0.5893(5) 0.6304(4) 0.0372(18) Uani 1 1 d . . . . .
C18 C -0.0009(8) 0.6293(5) 0.7575(3) 0.044(2) Uani 1 1 d . . . . .
C5 C -0.0303(6) 0.3058(4) 0.6023(3) 0.0272(16) Uani 1 1 d . . . . .
H5 H 0.0158 0.2571 0.5840 0.033 Uiso 1 1 calc R . . . .
C0AA C 0.2227(6) 0.3834(5) 0.6125(3) 0.0316(17) Uani 1 1 d . . . . .
H0AA H 0.2890 0.4058 0.6425 0.038 Uiso 1 1 calc R . . . .
C3AA C 0.2571(7) 0.5156(5) 0.8687(4) 0.044(2) Uani 1 1 d . . . . .
H3AA H 0.2077 0.5150 0.9023 0.053 Uiso 1 1 calc R . . . .
H3AB H 0.2282 0.5663 0.8424 0.053 Uiso 1 1 calc R . . . .
C8 C 0.2112(6) 0.4562(5) 0.5624(3) 0.0392(19) Uani 1 1 d . . . . .
H8A H 0.1789 0.5132 0.5772 0.047 Uiso 1 1 calc R . . . .
H8B H 0.1538 0.4348 0.5287 0.047 Uiso 1 1 calc R . . . .
C10 C -0.2168(7) 0.2020(6) 0.5926(3) 0.047(2) Uani 1 1 d . . . . .
H10A H -0.1721 0.1505 0.5776 0.056 Uiso 1 1 calc R . . . .
H10B H -0.2815 0.1770 0.6146 0.056 Uiso 1 1 calc R . . . .
C11 C -0.2758(6) 0.2576(5) 0.5403(3) 0.042(2) Uani 1 1 d . . . . .
H11A H -0.3263 0.2176 0.5126 0.051 Uiso 1 1 calc R . . . .
H11B H -0.3297 0.3041 0.5547 0.051 Uiso 1 1 calc R . . . .
C2AA C -0.1785(7) 0.3035(5) 0.5081(3) 0.046(2) Uani 1 1 d . . . . .
H2AA H -0.2184 0.3409 0.4754 0.055 Uiso 1 1 calc R . . . .
H2AB H -0.1290 0.2568 0.4908 0.055 Uiso 1 1 calc R . . . .
C13 C -0.1281(7) 0.2586(5) 0.6350(3) 0.045(2) Uani 1 1 d . . . . .
H13A H -0.0874 0.2187 0.6661 0.054 Uiso 1 1 calc R . . . .
H13B H -0.1746 0.3048 0.6543 0.054 Uiso 1 1 calc R . . . .
C14 C 0.2718(6) 0.2943(5) 0.5888(3) 0.0387(19) Uani 1 1 d . . . . .
H14A H 0.2148 0.2721 0.5553 0.046 Uiso 1 1 calc R . . . .
H14B H 0.2776 0.2478 0.6202 0.046 Uiso 1 1 calc R . . . .
C15 C -0.0941(7) 0.3641(5) 0.5508(3) 0.0395(19) Uani 1 1 d . . . . .
H15A H -0.1428 0.4124 0.5669 0.047 Uiso 1 1 calc R . . . .
H15B H -0.0318 0.3930 0.5290 0.047 Uiso 1 1 calc R . . . .
C16 C 0.3412(8) 0.4736(7) 0.5413(4) 0.063(3) Uani 1 1 d . . . . .
H16A H 0.3339 0.5178 0.5085 0.075 Uiso 1 1 calc R . . . .
H16B H 0.3969 0.4991 0.5743 0.075 Uiso 1 1 calc R . . . .
C17 C 0.2392(8) 0.4238(5) 0.8339(4) 0.060(3) Uani 1 1 d . . . . .
H17 H 0.2847 0.4360 0.7993 0.072 Uiso 1 1 calc R . . . .
C1AA C 0.3991(7) 0.3101(6) 0.5684(4) 0.050(2) Uani 1 1 d . . . . .
H1AA H 0.4284 0.2534 0.5518 0.060 Uiso 1 1 calc R . . . .
H1AB H 0.4576 0.3276 0.6027 0.060 Uiso 1 1 calc R . . . .
C19 C 0.4430(8) 0.3662(7) 0.8842(5) 0.070(3) Uani 1 1 d . . . . .
H19A H 0.4772 0.3145 0.9083 0.083 Uiso 1 1 calc R . . . .
H19B H 0.4903 0.3724 0.8501 0.083 Uiso 1 1 calc R . . . .
C20 C 0.3072(9) 0.3455(7) 0.8612(6) 0.096(4) Uani 1 1 d . . . . .
H20A H 0.3051 0.2961 0.8318 0.115 Uiso 1 1 calc R . . . .
H20B H 0.2653 0.3236 0.8946 0.115 Uiso 1 1 calc R . . . .
C21 C -0.3434(8) 0.5420(8) 0.6416(4) 0.076(3) Uani 1 1 d . . . . .
H21A H -0.3011 0.5972 0.6317 0.113 Uiso 1 1 calc GR . . . .
H21B H -0.4307 0.5545 0.6408 0.113 Uiso 1 1 calc GR . . . .
H21C H -0.3312 0.4947 0.6128 0.113 Uiso 1 1 calc GR . . . .
C22 C -0.3224(8) 0.5804(7) 0.7515(4) 0.076(3) Uani 1 1 d . . . . .
H22A H -0.2891 0.5604 0.7910 0.114 Uiso 1 1 calc GR . . . .
H22B H -0.4110 0.5865 0.7497 0.114 Uiso 1 1 calc GR . . . .
H22C H -0.2867 0.6390 0.7430 0.114 Uiso 1 1 calc GR . . . .
C23 C -0.3554(8) 0.4187(6) 0.7181(5) 0.077(3) Uani 1 1 d . . . . .
H23A H -0.3394 0.3734 0.6886 0.115 Uiso 1 1 calc GR . . . .
H23B H -0.4434 0.4288 0.7164 0.115 Uiso 1 1 calc GR . . . .
H23C H -0.3238 0.3971 0.7575 0.115 Uiso 1 1 calc GR . . . .
C24 C -0.159(2) 0.3034(13) 0.9190(11) 0.055(3) Uani 0.514(18) 1 d . . P A 1
H24A H -0.0959 0.2778 0.9489 0.066 Uiso 0.514(18) 1 calc R . P A 1
H24B H -0.2285 0.2615 0.9113 0.066 Uiso 0.514(18) 1 calc R . P A 1
C25 C 0.3930(8) 0.3859(7) 0.5210(4) 0.063(3) Uani 1 1 d . . . . .
H25A H 0.4761 0.3971 0.5103 0.076 Uiso 1 1 calc R . . . .
H25B H 0.3420 0.3648 0.4851 0.076 Uiso 1 1 calc R . . . .
C26 C 0.4583(10) 0.4541(8) 0.9222(5) 0.089(4) Uani 1 1 d . . . . .
H26A H 0.4254 0.4437 0.9602 0.107 Uiso 1 1 calc R . . . .
H26B H 0.5462 0.4683 0.9309 0.107 Uiso 1 1 calc R . . . .
C27 C -0.0004(18) 0.4005(15) 0.8629(10) 0.055(3) Uani 0.514(18) 1 d . . P A 1
H27 H 0.0606 0.3768 0.8950 0.066 Uiso 0.514(18) 1 calc R . P A 1
C28 C 0.3961(11) 0.5308(7) 0.8925(5) 0.093(4) Uani 1 1 d . . . . .
H28A H 0.4403 0.5480 0.8588 0.112 Uiso 1 1 calc R . . . .
H28B H 0.4016 0.5825 0.9203 0.112 Uiso 1 1 calc R . . . .
C30 C -0.104(2) 0.4863(12) 0.9438(9) 0.055(3) Uani 0.514(18) 1 d . . P A 1
H30A H -0.0416 0.4661 0.9758 0.066 Uiso 0.514(18) 1 calc R . P A 1
H30B H -0.1337 0.5466 0.9544 0.066 Uiso 0.514(18) 1 calc R . P A 1
C31 C -0.1035(19) 0.3368(13) 0.8587(9) 0.055(3) Uani 0.514(18) 1 d . . P A 1
H31A H -0.0785 0.2820 0.8382 0.066 Uiso 0.514(18) 1 calc R . P A 1
H31B H -0.1713 0.3647 0.8327 0.066 Uiso 0.514(18) 1 calc R . P A 1
C32 C -0.2052(18) 0.4218(15) 0.9366(10) 0.055(3) Uani 0.514(18) 1 d . . P A 1
H32A H -0.2664 0.4433 0.9046 0.066 Uiso 0.514(18) 1 calc R . P A 1
H32B H -0.2446 0.4206 0.9735 0.066 Uiso 0.514(18) 1 calc R . P A 1
C24A C -0.182(2) 0.3317(14) 0.9135(11) 0.048(3) Uani 0.486(18) 1 d . . P A 2
H24C H -0.2564 0.3053 0.8972 0.057 Uiso 0.486(18) 1 calc R . P A 2
C27A C -0.0467(19) 0.4014(16) 0.8505(10) 0.048(3) Uani 0.486(18) 1 d . . P A 2
H27A H -0.1249 0.4017 0.8236 0.057 Uiso 0.486(18) 1 calc R . P A 2
C30A C -0.178(2) 0.4773(14) 0.9248(9) 0.048(3) Uani 0.486(18) 1 d . . P A 2
H30D H -0.1810 0.5270 0.9537 0.057 Uiso 0.486(18) 1 calc R . P A 2
H30C H -0.2528 0.4814 0.8963 0.057 Uiso 0.486(18) 1 calc R . P A 2
C31A C -0.0483(19) 0.3090(12) 0.8845(9) 0.048(3) Uani 0.486(18) 1 d . . P A 2
H31C H 0.0221 0.3019 0.9152 0.057 Uiso 0.486(18) 1 calc R . P A 2
H31D H -0.0548 0.2560 0.8578 0.057 Uiso 0.486(18) 1 calc R . P A 2
C32A C -0.1776(17) 0.3851(13) 0.9577(9) 0.048(3) Uani 0.486(18) 1 d . . P A 2
H32C H -0.1750 0.3724 0.9986 0.057 Uiso 0.486(18) 1 calc R . P A 2
C1 C -0.0500(7) 0.4913(5) 0.8869(3) 0.044(2) Uani 1 1 d . . . . .
H1AC H 0.0179 0.5354 0.8917 0.052 Uiso 0.514(18) 1 calc R . P A 1
H1AD H -0.1127 0.5157 0.8565 0.052 Uiso 0.514(18) 1 calc R . P A 1
H1BF H -0.0592 0.5447 0.8606 0.052 Uiso 0.486(18) 1 calc R . P A 2
H1BE H 0.0250 0.4984 0.9148 0.052 Uiso 0.486(18) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 Br2 2.7192(9) . ?
W1 P4 2.5624(18) . ?
W1 P5 2.5457(18) . ?
W1 C7 1.819(7) . ?
W1 C12 2.044(8) . ?
W1 C18 2.009(8) . ?
P4 C3 1.858(7) . ?
P4 C5 1.852(7) . ?
P4 C0AA 1.849(7) . ?
P5 C6 1.844(6) . ?
P5 C17 1.828(8) . ?
P5 C27 1.80(2) . ?
P5 C27A 1.92(2) . ?
C3 C6 1.511(9) . ?
O4 C18 1.147(9) . ?
O5 C12 1.118(8) . ?
C7 C9 1.505(10) . ?
C9 C21 1.540(11) . ?
C9 C22 1.529(11) . ?
C9 C23 1.532(12) . ?
C5 C13 1.516(9) . ?
C5 C15 1.528(9) . ?
C0AA C8 1.534(9) . ?
C0AA C14 1.515(10) . ?
C3AA C17 1.543(10) . ?
C3AA C28 1.554(13) . ?
C8 C16 1.554(10) . ?
C10 C11 1.502(10) . ?
C10 C13 1.511(10) . ?
C11 C2AA 1.498(10) . ?
C2AA C15 1.523(9) . ?
C14 C1AA 1.517(9) . ?
C16 C25 1.481(13) . ?
C17 C20 1.448(11) . ?
C1AA C25 1.522(11) . ?
C19 C20 1.530(12) . ?
C19 C26 1.529(13) . ?
C24 C31 1.61(3) . ?
C24 C32 1.84(3) . ?
C26 C28 1.423(14) . ?
C27 C31 1.44(3) . ?
C27 C1 1.54(2) . ?
C30 C32 1.43(3) . ?
C30 C1 1.461(18) . ?
C24A C31A 1.68(3) . ?
C24A C32A 1.25(3) . ?
C27A C31A 1.54(3) . ?
C27A C1 1.54(2) . ?
C30A C32A 1.53(3) . ?
C30A C1 1.72(2) . ?

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
P4 W1 Br2 85.92(4) . . ?
P5 W1 Br2 91.18(5) . . ?
P5 W1 P4 79.71(6) . . ?
C7 W1 Br2 168.8(2) . . ?
C7 W1 P4 103.5(2) . . ?
C7 W1 P5 96.5(2) . . ?
C7 W1 C12 87.0(3) . . ?
C7 W1 C18 88.2(3) . . ?
C12 W1 Br2 86.2(2) . . ?
C12 W1 P4 93.9(2) . . ?
C12 W1 P5 173.3(2) . . ?
C18 W1 Br2 83.0(2) . . ?
C18 W1 P4 167.7(2) . . ?
C18 W1 P5 95.2(2) . . ?
C18 W1 C12 90.7(3) . . ?
C3 P4 W1 107.7(2) . . ?
C5 P4 W1 120.0(2) . . ?
C5 P4 C3 103.5(3) . . ?
C0AA P4 W1 117.5(2) . . ?
C0AA P4 C3 100.1(3) . . ?
C0AA P4 C5 105.4(3) . . ?
C6 P5 W1 106.2(2) . . ?
C6 P5 C27A 100.1(7) . . ?
C17 P5 W1 116.9(3) . . ?
C17 P5 C6 103.8(3) . . ?
C17 P5 C27A 115.7(7) . . ?
C27 P5 W1 124.8(7) . . ?
C27 P5 C6 103.3(8) . . ?
C27 P5 C17 99.4(8) . . ?
C27A P5 W1 111.8(6) . . ?
C6 C3 P4 113.0(4) . . ?
C3 C6 P5 111.1(4) . . ?
C9 C7 W1 166.1(5) . . ?
C7 C9 C21 109.0(7) . . ?
C7 C9 C22 110.4(6) . . ?
C7 C9 C23 112.1(6) . . ?
C22 C9 C21 109.3(7) . . ?
C22 C9 C23 107.8(8) . . ?
C23 C9 C21 108.1(7) . . ?
O5 C12 W1 176.9(7) . . ?
O4 C18 W1 178.6(7) . . ?
C13 C5 P4 113.1(5) . . ?
C13 C5 C15 109.5(6) . . ?
C15 C5 P4 112.9(4) . . ?
C8 C0AA P4 114.8(5) . . ?
C14 C0AA P4 115.6(5) . . ?
C14 C0AA C8 109.4(6) . . ?
C17 C3AA C28 110.8(7) . . ?
C0AA C8 C16 109.4(6) . . ?
C11 C10 C13 112.3(6) . . ?
C2AA C11 C10 110.7(6) . . ?
C11 C2AA C15 111.0(6) . . ?
C10 C13 C5 111.8(6) . . ?
C0AA C14 C1AA 110.1(6) . . ?
C2AA C15 C5 109.9(6) . . ?
C25 C16 C8 109.9(7) . . ?
C3AA C17 P5 112.0(6) . . ?
C20 C17 P5 120.8(6) . . ?
C20 C17 C3AA 115.8(7) . . ?
C14 C1AA C25 110.5(6) . . ?
C26 C19 C20 112.9(8) . . ?
C17 C20 C19 114.3(9) . . ?
C31 C24 C32 92.1(15) . . ?
C16 C25 C1AA 113.1(7) . . ?
C28 C26 C19 112.1(9) . . ?
C31 C27 P5 116.2(16) . . ?
C31 C27 C1 105.8(15) . . ?
C1 C27 P5 115.9(14) . . ?
C26 C28 C3AA 115.9(8) . . ?
C32 C30 C1 108.1(17) . . ?
C27 C31 C24 119.6(19) . . ?
C30 C32 C24 114.0(17) . . ?
C32A C24A C31A 118(2) . . ?
C31A C27A P5 114.4(14) . . ?
C1 C27A P5 109.3(12) . . ?
C1 C27A C31A 118.2(16) . . ?
C32A C30A C1 112.4(14) . . ?
C27A C31A C24A 94.5(16) . . ?
C24A C32A C30A 99(2) . . ?
C30 C1 C27 116.8(12) . . ?
C27A C1 C30A 103.3(12) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.748
_oxdiff_exptl_absorpt_empirical_full_min 0.821

####################################################################### 
# 
# 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_rk05_scaled
_database_code_depnum_ccdc_archive 'CCDC 1515561'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_audit_creation_date             2016-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H62 O2 P2 S W'
_chemical_formula_sum            'C39 H62 O2 P2 S W'
_chemical_formula_weight         840.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C39 H62 O2 P2 S W'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.70419(20)
_cell_length_b                   20.77394(16)
_cell_length_c                   18.14956(16)
_cell_angle_alpha                90
_cell_angle_beta                 106.3363(10)
_cell_angle_gamma                90
_cell_volume                     7852.92(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    40607
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6350
_cell_measurement_theta_min      3.5180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.946
_exptl_absorpt_correction_T_max  0.61338
_exptl_absorpt_correction_T_min  0.58244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 8 -8 0.0204
-7 -8 9 0.0274
-12 4 -3 0.0728
-1 -9 9 0.0455
-7 10 7 0.0281
7 -10 -6 0.0141
12 -2 3 0.0832
-12 -6 6 0.0476

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Slow recrystallization from ether'
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.048
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.9906 7.9927 -7.9873 0.0709 0.4883 -0.8494
-6.9916 -7.9924 8.9873 -0.1118 -0.3902 0.9247
-11.9911 3.9934 -3.0047 -0.1970 -0.8908 -0.4949
-0.9963 -8.9903 8.9910 0.0104 0.0309 1.0240
-7.0008 9.9899 6.9939 -0.9894 -0.1872 -0.0740
7.0006 -9.9897 -5.9946 0.9373 0.2128 0.1407
11.9900 -1.9953 3.0053 0.0879 0.9191 0.3987
-11.9877 -5.9957 5.9866 -0.1208 -0.8015 0.5858

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            158756
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.098
_diffrn_reflns_theta_min         3.004
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -20.00   1.00    2.50    --  -37.04 -57.00   0.00   84
  2  ω     18.00 106.00   1.00    2.50    --   37.04  38.00  60.00   88
  3  ω     23.00  90.00   1.00    2.50    --   37.04-125.00 -90.00   67
  4  ω     20.00 104.00   1.00    2.50    --   37.04  57.00 120.00   84
  5  ω      1.00  76.00   1.00    2.50    --   37.04 -99.00 150.00   75
  6  ω    -30.00  54.00   1.00    2.50    --   37.04 -57.00-150.00   84
  7  ω     23.00  90.00   1.00    2.50    --   37.04-125.00 -30.00   67
  8  ω     10.00 105.00   1.00    2.50    --   37.04  77.00 150.00   95
  9  ω     18.00 106.00   1.00    2.50    --   37.04  38.00   0.00   88
 10  ω      1.00  76.00   1.00    2.50    --   37.04 -99.00  30.00   75
 11  ω    -29.00  58.00   1.00    2.50    --   37.04 -66.00  98.00   87
 12  ω    -32.00  56.00   1.00    2.50    --   37.04 -38.00   0.00   88
 13  ω      1.00  76.00   1.00    2.50    --   37.04 -99.00-120.00   75
 14  ω     10.00 105.00   1.00    2.50    --   37.04  77.00 -60.00   95
 15  ω     20.00 104.00   1.00    2.50    --   37.04  57.00 -90.00   84
 16  ω     41.00 157.00   1.00   10.00    --  111.00 -12.00 150.00  116
 17  ω     92.00 178.00   1.00   10.00    --  111.00  38.00 120.00   86
 18  ω     41.00 116.00   1.00   10.00    --  111.00-111.00-180.00   75
 19  ω     84.00 178.00   1.00   10.00    --  111.00  77.00 -60.00   94
 20  ω     86.00 178.00   1.00   10.00    --  111.00  25.00 150.00   92
 21  ω    100.00 178.00   1.00   10.00    --  111.00 111.00 150.00   78
 22  ω    100.00 178.00   1.00   10.00    --  111.00 111.00-180.00   78
 23  ω     44.00 131.00   1.00   10.00    --  111.00 -64.00  60.00   87
 24  ω     43.00 138.00   1.00   10.00    --  111.00 -77.00-180.00   95
 25  ω     42.00 146.00   1.00   10.00    --  111.00 -92.00 -60.00  104
 26  ω     94.00 178.00   1.00   10.00    --  111.00  50.00  90.00   84
 27  ω     42.00 146.00   1.00   10.00    --  111.00 -92.00 120.00  104
 28  ω     41.00 116.00   1.00   10.00    --  111.00-111.00  90.00   75
 29  ω     41.00 132.00   1.00   10.00    --  111.00 -32.00-157.63   91
 30  ω     41.00 116.00   1.00   10.00    --  111.00-111.00 120.00   75
 31  ω     41.00 116.00   1.00   10.00    --  111.00-111.00   0.00   75
 32  ω     42.00 146.00   1.00   10.00    --  111.00 -92.00   0.00  104
 33  ω    113.00 143.00   1.00   10.00    --  111.00 178.00 120.00   30
 34  ω     70.00 109.00   1.00   10.00    --  111.00 -38.00   0.00   39
 35  ω    107.00 133.00   1.00   10.00    --  111.00  64.00  30.00   26
 36  ω     67.00  94.00   1.00   10.00    --  111.00  11.00 -22.76   27
 37  ω    101.00 127.00   1.00   10.00    --  111.00 -50.00 -30.00   26
 38  ω     79.00 104.00   1.00   10.00    --  111.00-111.00 -90.00   25
 39  ω     67.00  93.00   1.00   10.00    --  111.00 -64.00-150.00   26
 40  ω    106.00 131.00   1.00   10.00    --  111.00 -64.00-150.00   25
 41  ω     78.00 116.00   1.00   10.00    --  111.00-111.00-120.00   38
 42  ω     52.00  79.00   1.00   10.00    --  111.00-111.00  30.00   27
 43  ω     85.00 111.00   1.00   10.00    --  111.00-111.00  30.00   26
 44  ω     42.00  74.00   1.00   10.00    --  111.00 -38.00  90.00   32
 45  ω     86.00 124.00   1.00   10.00    --  111.00 -38.00  90.00   38
 46  ω    100.00 125.00   1.00   10.00    --  111.00 -25.00  90.00   25
 47  ω     45.00  95.00   1.00   10.00    --  111.00 -25.00  90.00   50
 48  ω     43.00  68.00   1.00   10.00    --  111.00-111.00 -90.00   25
 49  ω     70.00 114.00   1.00   10.00    --  111.00-111.00-150.00   44
 50  ω     45.00  71.00   1.00   10.00    --  111.00 -77.00  30.00   26
 51  ω     89.00 115.00   1.00   10.00    --  111.00 -77.00  30.00   26
 52  ω     79.00 105.00   1.00   10.00    --  111.00-111.00 -30.00   26
 53  ω    111.00 136.00   1.00   10.00    --  111.00 -25.00 -60.00   25
 54  ω     96.00 122.00   1.00   10.00    --  111.00 -38.00 -60.00   26
 55  ω    130.00 164.00   1.00   10.00    --  111.00  50.00-180.00   34
 56  ω    132.00 157.00   1.00   10.00    --  111.00 -12.00 -90.00   25
 57  ω     57.00  82.00   1.00   10.00    --  111.00 -12.00 -90.00   25
 58  ω     42.00  89.00   1.00   10.00    --  111.00 -25.00 -60.00   47
 59  ω    106.00 132.00   1.00   10.00    --  111.00 -25.00   0.00   26
 60  ω     42.00  71.00   1.00   10.00    --  111.00 -25.00   0.00   29
 61  ω     73.00 125.00   1.00   10.00    --  111.00 -64.00 150.00   52
 62  ω     42.00  78.00   1.00   10.00    --  111.00 -38.00 -60.00   36
 63  ω    139.00 174.00   1.00   10.00    --  111.00  38.00  90.00   35
 64  ω     77.00 116.00   1.00   10.00    --  111.00-111.00 -60.00   39
 65  ω     86.00 112.00   1.00   10.00    --  111.00-111.00 150.00   26
 66  ω    101.00 178.00   1.00   10.00    --  111.00 111.00-120.00   77
 67  ω     94.00 121.00   1.00   10.00    --  111.00  50.00 -90.00   27
 68  ω    133.00 159.00   1.00   10.00    --  111.00  64.00 -30.00   26
 69  ω    143.00 169.00   1.00   10.00    --  111.00  12.00-150.00   26
 70  ω     71.00  97.00   1.00   10.00    --  111.00 -64.00-180.00   26
 71  ω     88.00 115.00   1.00   10.00    --  111.00  12.00-150.00   27
 72  ω    101.00 127.00   1.00   10.00    --  111.00 178.00-150.00   26
 73  ω     48.00 128.00   1.00   10.00    --  111.00 -50.00  90.00   80
 74  ω     92.00 118.00   1.00   10.00    --  111.00 -79.00 -96.86   26
 75  ω     50.00  76.00   1.00   10.00    --  111.00  -2.00 -40.17   26
 76  ω     44.00  74.00   1.00   10.00    --  111.00 -79.00 -96.86   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113222000
_diffrn_orient_matrix_UB_12      -0.0545833000
_diffrn_orient_matrix_UB_13      -0.0521686000
_diffrn_orient_matrix_UB_21      0.0725805000
_diffrn_orient_matrix_UB_22      0.0141691000
_diffrn_orient_matrix_UB_23      0.0256484000
_diffrn_orient_matrix_UB_31      0.0085247000
_diffrn_orient_matrix_UB_32      -0.0481385000
_diffrn_orient_matrix_UB_33      0.0667066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13238
_reflns_number_total             15875
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.222
_refine_diff_density_min         -3.803
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         15875
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0478
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0251P)²+39.1563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1094
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C128(H3AA), C10(H7AA), C16(H9AA), C122(H37), C110(H56), C28(H9), C116(H12),
 C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C109(H20a,H20b), C11(H6Aa,H6Ab), C21(H24a,H24b), C129(H8Aa,H8Ab), C115(H33a,
 H33b), C127(H34a,H34b), C12(H40a,H40b), C17(H0Ba,H0Bb), C126(H45a,H45b),
 C112(H46a,H46b), C108(H48a,H48b), C133(H54a,H54b), C131(H59a,H59b), C130(H61a,
 H61b), C114(H63a,H63b), C123(H66a,H66b), C14(H68a,H68b), C19(H70a,H70b),
 C125(H74a,H74b), C20(H75a,H75b), C15(H81a,H81b), C111(H83a,H83b), C18(H89a,
 H89b), C124(H90a,H90b), C132(H98a,H98b), C8(H2Ba,H2Bb), C9(H13a,H13b),
 C29(H14a,H14b), C23(H18a,H18b), C33(H21a,H21b), C117(H23a,H23b), C121(H25a,
 H25b), C120(H26a,H26b), C118(H28a,H28b), C30(H29a,H29b), C32(H31a,H31b),
 C13(H1Aa,H1Ab), C31(H35a,H35b), C26(H36a,H36b), C27(H38a,H38b), C119(H41a,
 H41b), C25(H43a,H43b), C24(H44a,H44b), C113(H4a,H4b)
2.c Aromatic/amide H refined with riding coordinates:
 C35(H2AA), C135(H5AA), C37(H49), C139(H55), C36(H76), C137(H80), C38(H84),
 C138(H86), C136(H95), C39(H0AA)
2.d Idealised Me refined as rotating group:
 C104(H67a,H67b,H67c), C105(H72a,H72b,H72c), C4(H8a,H8b,H8c), C103(H3Ba,H3Bb,
 H3Bc), C5(H10a,H10b,H10c), C3(H11a,H11b,H11c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.02495(2) 0.73483(2) -0.22824(2) 0.02402(6) Uani 1 1 d . . . . .
W2 W 0.52075(2) 0.75328(2) -0.23581(2) 0.02648(6) Uani 1 1 d . . . . .
P3 P 0.08001(6) 0.71094(6) -0.08647(7) 0.0278(2) Uani 1 1 d . . . . .
P4 P -0.07126(5) 0.72956(6) -0.17379(7) 0.0233(2) Uani 1 1 d . . . . .
P5 P 0.42450(6) 0.75582(6) -0.18140(7) 0.0278(2) Uani 1 1 d . . . . .
S6 S 0.50415(7) 0.87667(7) -0.25575(8) 0.0359(3) Uani 1 1 d . . . . .
S7 S 0.00784(6) 0.61184(6) -0.25218(7) 0.0306(2) Uani 1 1 d . . . . .
P8 P 0.57615(6) 0.77127(7) -0.09418(7) 0.0288(3) Uani 1 1 d . . . . .
C3AA C 0.6457(3) 0.7181(3) -0.0495(3) 0.0341(11) Uani 1 1 d . . . . .
H3AA H 0.6285 0.6731 -0.0558 0.041 Uiso 1 1 calc R . . . .
C20 C 0.5179(2) 0.7487(3) -0.0423(3) 0.0344(12) Uani 1 1 d . . . . .
H20A H 0.5120 0.7015 -0.0437 0.041 Uiso 1 1 calc R . . . .
H20B H 0.5338 0.7623 0.0121 0.041 Uiso 1 1 calc R . . . .
C4AA C 0.5334(2) 0.6659(3) -0.2354(3) 0.0337(11) Uani 1 1 d . . . . .
C6AA C -0.1403(2) 0.6109(2) -0.1855(3) 0.0316(11) Uani 1 1 d . . . . .
H6AA H -0.1034 0.5878 -0.1951 0.038 Uiso 1 1 calc R . . . .
H6AB H -0.1336 0.6130 -0.1293 0.038 Uiso 1 1 calc R . . . .
C24 C -0.1445(3) 0.8340(3) -0.2427(3) 0.0343(11) Uani 1 1 d . . . . .
H24A H -0.1802 0.8037 -0.2642 0.041 Uiso 1 1 calc R . . . .
H24B H -0.1168 0.8349 -0.2776 0.041 Uiso 1 1 calc R . . . .
C7AA C -0.1439(2) 0.6795(2) -0.2184(3) 0.0266(10) Uani 1 1 d . . . . .
H7AA H -0.1814 0.7012 -0.2073 0.032 Uiso 1 1 calc R . . . .
C8AA C 0.6981(3) 0.7199(3) -0.0902(3) 0.0388(12) Uani 1 1 d . . . . .
H8AA H 0.7168 0.7636 -0.0859 0.047 Uiso 1 1 calc R . . . .
H8AB H 0.6791 0.7103 -0.1454 0.047 Uiso 1 1 calc R . . . .
C9AA C -0.1053(2) 0.8102(3) -0.1633(3) 0.0291(10) Uani 1 1 d . . . . .
H9AA H -0.0682 0.8403 -0.1451 0.035 Uiso 1 1 calc R . . . .
C2AA C 0.0969(3) 0.5683(3) -0.3216(4) 0.0404(13) Uani 1 1 d . . . . .
H2AA H 0.1249 0.5649 -0.2710 0.049 Uiso 1 1 calc R . . . .
C33 C 0.3569(3) 0.8741(3) -0.1873(3) 0.0396(13) Uani 1 1 d . . . . .
H33A H 0.3638 0.8703 -0.1311 0.048 Uiso 1 1 calc R . . . .
H33B H 0.3939 0.8975 -0.1961 0.048 Uiso 1 1 calc R . . . .
C34 C 0.6518(3) 0.8824(3) -0.0891(3) 0.0344(11) Uani 1 1 d . . . . .
H34A H 0.6913 0.8645 -0.0534 0.041 Uiso 1 1 calc R . . . .
H34B H 0.6500 0.8680 -0.1417 0.041 Uiso 1 1 calc R . . . .
C37 C 0.5929(2) 0.8569(3) -0.0675(3) 0.0318(11) Uani 1 1 d . . . . .
H37 H 0.5559 0.8808 -0.1020 0.038 Uiso 1 1 calc R . . . .
C39 C 0.0354(3) 0.5921(2) -0.3328(3) 0.0312(11) Uani 1 1 d . . . . .
C40 C -0.2023(3) 0.5744(3) -0.2231(4) 0.0428(14) Uani 1 1 d . . . . .
H40A H -0.1983 0.5297 -0.2033 0.051 Uiso 1 1 calc R . . . .
H40B H -0.2383 0.5951 -0.2086 0.051 Uiso 1 1 calc R . . . .
C0BA C -0.1442(3) 0.8137(3) -0.1052(3) 0.0383(12) Uani 1 1 d . . . . .
H0BA H -0.1161 0.8029 -0.0535 0.046 Uiso 1 1 calc R . . . .
H0BB H -0.1793 0.7817 -0.1188 0.046 Uiso 1 1 calc R . . . .
C5AA C 0.5966(3) 0.9167(3) -0.3233(4) 0.0417(13) Uani 1 1 d . . . . .
H5AA H 0.6254 0.9155 -0.2730 0.050 Uiso 1 1 calc R . . . .
C45 C 0.6543(3) 0.9553(3) -0.0856(4) 0.0476(15) Uani 1 1 d . . . . .
H45A H 0.6170 0.9731 -0.1251 0.057 Uiso 1 1 calc R . . . .
H45B H 0.6938 0.9704 -0.0972 0.057 Uiso 1 1 calc R . . . .
C46 C 0.2766(3) 0.8500(3) -0.3451(4) 0.0467(15) Uani 1 1 d . . . . .
H46A H 0.2694 0.8541 -0.4012 0.056 Uiso 1 1 calc R . . . .
H46B H 0.2399 0.8259 -0.3362 0.056 Uiso 1 1 calc R . . . .
C48 C 0.4537(2) 0.7821(3) -0.0807(3) 0.0339(11) Uani 1 1 d . . . . .
H48A H 0.4595 0.8294 -0.0785 0.041 Uiso 1 1 calc R . . . .
H48B H 0.4218 0.7709 -0.0531 0.041 Uiso 1 1 calc R . . . .
C49 C 0.0779(4) 0.5543(3) -0.4576(4) 0.0507(16) Uani 1 1 d . . . . .
H49 H 0.0925 0.5413 -0.5000 0.061 Uiso 1 1 calc R . . . .
C50 C 0.5325(3) 0.8982(3) -0.3348(3) 0.0355(12) Uani 1 1 d . . . . .
C52 C 0.5462(3) 0.5971(3) -0.2479(3) 0.0351(11) Uani 1 1 d . . . . .
C54 C 0.6733(3) 0.7280(3) 0.0362(3) 0.0453(15) Uani 1 1 d . . . . .
H54A H 0.6386 0.7235 0.0616 0.054 Uiso 1 1 calc R . . . .
H54B H 0.6909 0.7722 0.0460 0.054 Uiso 1 1 calc R . . . .
C55 C 0.4918(3) 0.9001(3) -0.4093(3) 0.0412(13) Uani 1 1 d . . . . .
H55 H 0.4482 0.8876 -0.4187 0.049 Uiso 1 1 calc R . . . .
C56 C 0.3525(2) 0.8067(3) -0.2229(3) 0.0335(11) Uani 1 1 d . . . . .
H56 H 0.3149 0.7845 -0.2126 0.040 Uiso 1 1 calc R . . . .
C59 C 0.7790(3) 0.6824(3) 0.0299(4) 0.0496(16) Uani 1 1 d . . . . .
H59A H 0.7995 0.7254 0.0381 0.060 Uiso 1 1 calc R . . . .
H59B H 0.8122 0.6497 0.0520 0.060 Uiso 1 1 calc R . . . .
C61 C 0.7517(3) 0.6705(3) -0.0552(4) 0.0437(14) Uani 1 1 d . . . . .
H61A H 0.7339 0.6263 -0.0638 0.052 Uiso 1 1 calc R . . . .
H61B H 0.7862 0.6742 -0.0809 0.052 Uiso 1 1 calc R . . . .
C63 C 0.2951(3) 0.9120(3) -0.2227(4) 0.0536(17) Uani 1 1 d . . . . .
H63A H 0.2589 0.8909 -0.2091 0.064 Uiso 1 1 calc R . . . .
H63B H 0.2996 0.9560 -0.2010 0.064 Uiso 1 1 calc R . . . .
C66 C 0.5947(3) 0.8795(3) 0.0134(3) 0.0416(13) Uani 1 1 d . . . . .
H66A H 0.5562 0.8638 0.0268 0.050 Uiso 1 1 calc R . . . .
H66B H 0.6331 0.8616 0.0511 0.050 Uiso 1 1 calc R . . . .
C67 C 0.6136(3) 0.5907(3) -0.2582(4) 0.0515(16) Uani 1 1 d . . . . .
H67A H 0.6455 0.6045 -0.2111 0.077 Uiso 1 1 calc GR . . . .
H67B H 0.6169 0.6178 -0.3011 0.077 Uiso 1 1 calc GR . . . .
H67C H 0.6214 0.5457 -0.2691 0.077 Uiso 1 1 calc GR . . . .
C68 C -0.2202(3) 0.6409(3) -0.3426(3) 0.0413(13) Uani 1 1 d . . . . .
H68A H -0.2565 0.6646 -0.3324 0.050 Uiso 1 1 calc R . . . .
H68B H -0.2275 0.6388 -0.3989 0.050 Uiso 1 1 calc R . . . .
C70 C -0.2121(3) 0.9028(3) -0.1826(4) 0.0480(15) Uani 1 1 d . . . . .
H70A H -0.2496 0.8741 -0.2014 0.058 Uiso 1 1 calc R . . . .
H70B H -0.2282 0.9470 -0.1793 0.058 Uiso 1 1 calc R . . . .
C72 C 0.4973(3) 0.5716(3) -0.3197(4) 0.0569(18) Uani 1 1 d . . . . .
H72A H 0.4979 0.5985 -0.3638 0.085 Uiso 1 1 calc GR . . . .
H72B H 0.4543 0.5728 -0.3121 0.085 Uiso 1 1 calc GR . . . .
H72C H 0.5081 0.5272 -0.3293 0.085 Uiso 1 1 calc GR . . . .
C74 C 0.6535(4) 0.9800(3) -0.0072(4) 0.0524(16) Uani 1 1 d . . . . .
H74A H 0.6511 1.0276 -0.0085 0.063 Uiso 1 1 calc R . . . .
H74B H 0.6940 0.9675 0.0312 0.063 Uiso 1 1 calc R . . . .
C75 C -0.1719(3) 0.9017(3) -0.2382(4) 0.0415(13) Uani 1 1 d . . . . .
H75A H -0.1362 0.9329 -0.2214 0.050 Uiso 1 1 calc R . . . .
H75B H -0.1985 0.9148 -0.2898 0.050 Uiso 1 1 calc R . . . .
C76 C 0.1179(3) 0.5492(3) -0.3837(4) 0.0495(15) Uani 1 1 d . . . . .
H76 H 0.1600 0.5325 -0.3753 0.059 Uiso 1 1 calc R . . . .
C80 C 0.5774(4) 0.9389(3) -0.4580(4) 0.0541(17) Uani 1 1 d . . . . .
H80 H 0.5922 0.9531 -0.4997 0.065 Uiso 1 1 calc R . . . .
C81 C -0.1575(2) 0.6768(2) -0.3061(3) 0.0309(10) Uani 1 1 d . . . . .
H81A H -0.1604 0.7211 -0.3269 0.037 Uiso 1 1 calc R . . . .
H81B H -0.1216 0.6547 -0.3194 0.037 Uiso 1 1 calc R . . . .
C83 C 0.3387(3) 0.8127(3) -0.3103(3) 0.0354(12) Uani 1 1 d . . . . .
H83A H 0.3749 0.8352 -0.3224 0.042 Uiso 1 1 calc R . . . .
H83B H 0.3352 0.7692 -0.3334 0.042 Uiso 1 1 calc R . . . .
C84 C 0.0168(4) 0.5786(3) -0.4692(3) 0.0467(15) Uani 1 1 d . . . . .
H84 H -0.0109 0.5823 -0.5200 0.056 Uiso 1 1 calc R . . . .
C86 C 0.5144(4) 0.9200(3) -0.4697(3) 0.0500(16) Uani 1 1 d . . . . .
H86 H 0.4859 0.9206 -0.5202 0.060 Uiso 1 1 calc R . . . .
C89 C -0.1728(3) 0.8810(3) -0.1033(4) 0.0436(14) Uani 1 1 d . . . . .
H89A H -0.2005 0.8806 -0.0683 0.052 Uiso 1 1 calc R . . . .
H89B H -0.1376 0.9121 -0.0828 0.052 Uiso 1 1 calc R . . . .
C90 C 0.5968(3) 0.9531(3) 0.0170(4) 0.0499(15) Uani 1 1 d . . . . .
H90A H 0.5564 0.9706 -0.0171 0.060 Uiso 1 1 calc R . . . .
H90B H 0.6000 0.9672 0.0701 0.060 Uiso 1 1 calc R . . . .
C95 C 0.6186(4) 0.9369(3) -0.3843(4) 0.0523(16) Uani 1 1 d . . . . .
H95 H 0.6622 0.9493 -0.3755 0.063 Uiso 1 1 calc R . . . .
C98 C 0.7264(3) 0.6792(4) 0.0705(4) 0.0553(18) Uani 1 1 d . . . . .
H98A H 0.7451 0.6882 0.1259 0.066 Uiso 1 1 calc R . . . .
H98B H 0.7079 0.6353 0.0654 0.066 Uiso 1 1 calc R . . . .
O4 O 0.1502(2) 0.7241(2) -0.2833(3) 0.0488(11) Uani 1 1 d . . . . .
C9 C 0.0945(2) 0.6238(3) -0.0638(3) 0.0315(11) Uani 1 1 d . . . . .
H9 H 0.0565 0.6007 -0.0977 0.038 Uiso 1 1 calc R . . . .
C1BA C 0.1054(3) 0.7271(3) -0.2634(3) 0.0339(11) Uani 1 1 d . . . . .
C2BA C -0.0424(2) 0.7001(3) -0.0741(3) 0.0295(10) Uani 1 1 d . . . . .
H2BA H -0.0744 0.7099 -0.0463 0.035 Uiso 1 1 calc R . . . .
H2BB H -0.0365 0.6528 -0.0741 0.035 Uiso 1 1 calc R . . . .
C12 C 0.3900(2) 0.6745(3) -0.1748(3) 0.0327(11) Uani 1 1 d . . . . .
H12 H 0.4272 0.6444 -0.1570 0.039 Uiso 1 1 calc R . . . .
C13 C 0.0214(2) 0.7325(3) -0.0340(3) 0.0308(11) Uani 1 1 d . . . . .
H13A H 0.0369 0.7177 0.0199 0.037 Uiso 1 1 calc R . . . .
H13B H 0.0158 0.7798 -0.0339 0.037 Uiso 1 1 calc R . . . .
C14 C 0.1530(3) 0.5996(3) -0.0878(3) 0.0358(12) Uani 1 1 d . . . . .
H14A H 0.1490 0.6129 -0.1414 0.043 Uiso 1 1 calc R . . . .
H14B H 0.1926 0.6190 -0.0542 0.043 Uiso 1 1 calc R . . . .
C15 C 0.0471(3) 0.8913(2) -0.2419(3) 0.0313(11) Uani 1 1 d . . . . .
C16 C 0.0361(2) 0.8217(2) -0.2269(3) 0.0268(10) Uani 1 1 d . . . . .
C18 C 0.2005(3) 0.7630(3) -0.0830(3) 0.0415(13) Uani 1 1 d . . . . .
H18A H 0.2089 0.7225 -0.1073 0.050 Uiso 1 1 calc R . . . .
H18B H 0.1784 0.7930 -0.1243 0.050 Uiso 1 1 calc R . . . .
C21 C 0.0985(3) 0.6023(3) 0.0179(3) 0.0391(12) Uani 1 1 d . . . . .
H21A H 0.1365 0.6222 0.0543 0.047 Uiso 1 1 calc R . . . .
H21B H 0.0598 0.6169 0.0317 0.047 Uiso 1 1 calc R . . . .
C22 C 0.1566(3) 0.7488(4) -0.0308(4) 0.0529(18) Uani 1 1 d . . . . .
H22 H 0.1796 0.7156 0.0068 0.063 Uiso 1 1 calc R . . . .
C23 C 0.3515(3) 0.6513(3) -0.2544(3) 0.0402(13) Uani 1 1 d . . . . .
H23A H 0.3794 0.6520 -0.2892 0.048 Uiso 1 1 calc R . . . .
H23B H 0.3153 0.6812 -0.2753 0.048 Uiso 1 1 calc R . . . .
C0AA C -0.0046(3) 0.5975(3) -0.4077(3) 0.0394(12) Uani 1 1 d . . . . .
H0AA H -0.0467 0.6142 -0.4164 0.047 Uiso 1 1 calc R . . . .
C25 C 0.3508(3) 0.6688(3) -0.1171(4) 0.0453(14) Uani 1 1 d . . . . .
H25A H 0.3785 0.6794 -0.0651 0.054 Uiso 1 1 calc R . . . .
H25B H 0.3151 0.7002 -0.1304 0.054 Uiso 1 1 calc R . . . .
C26 C 0.3237(3) 0.6010(3) -0.1167(4) 0.0511(16) Uani 1 1 d . . . . .
H26A H 0.2957 0.6000 -0.0820 0.061 Uiso 1 1 calc R . . . .
H26B H 0.3594 0.5704 -0.0965 0.061 Uiso 1 1 calc R . . . .
C28 C 0.3253(3) 0.5830(3) -0.2521(4) 0.0493(15) Uani 1 1 d . . . . .
H28A H 0.2990 0.5706 -0.3041 0.059 Uiso 1 1 calc R . . . .
H28B H 0.3615 0.5523 -0.2359 0.059 Uiso 1 1 calc R . . . .
C29 C 0.1574(3) 0.5267(3) -0.0817(4) 0.0452(14) Uani 1 1 d . . . . .
H29A H 0.1963 0.5120 -0.0951 0.054 Uiso 1 1 calc R . . . .
H29B H 0.1195 0.5074 -0.1190 0.054 Uiso 1 1 calc R . . . .
C31 C 0.1038(3) 0.5293(3) 0.0246(4) 0.0492(15) Uani 1 1 d . . . . .
H31A H 0.0636 0.5097 -0.0074 0.059 Uiso 1 1 calc R . . . .
H31B H 0.1090 0.5166 0.0786 0.059 Uiso 1 1 calc R . . . .
C1AA C -0.2174(3) 0.5729(3) -0.3101(4) 0.0500(16) Uani 1 1 d . . . . .
H1AA H -0.2592 0.5512 -0.3321 0.060 Uiso 1 1 calc R . . . .
H1AB H -0.1840 0.5478 -0.3250 0.060 Uiso 1 1 calc R . . . .
C35 C 0.1603(3) 0.5036(3) -0.0009(4) 0.0509(16) Uani 1 1 d . . . . .
H35A H 0.1598 0.4560 0.0000 0.061 Uiso 1 1 calc R . . . .
H35B H 0.2009 0.5184 0.0355 0.061 Uiso 1 1 calc R . . . .
C36 C 0.2166(3) 0.8299(4) 0.0628(4) 0.0563(18) Uani 1 1 d . . . . .
H36A H 0.2110 0.8704 0.0889 0.068 Uiso 1 1 calc R . . . .
H36B H 0.2362 0.7977 0.1028 0.068 Uiso 1 1 calc R . . . .
C38 C 0.1498(4) 0.8052(4) 0.0146(5) 0.065(2) Uani 1 1 d . . . . .
H38A H 0.1236 0.7938 0.0493 0.078 Uiso 1 1 calc R . . . .
H38B H 0.1273 0.8398 -0.0201 0.078 Uiso 1 1 calc R . . . .
C41 C 0.2850(3) 0.5798(3) -0.1971(5) 0.0557(18) Uani 1 1 d . . . . .
H41A H 0.2696 0.5351 -0.1950 0.067 Uiso 1 1 calc R . . . .
H41B H 0.2470 0.6079 -0.2156 0.067 Uiso 1 1 calc R . . . .
C43 C 0.2610(4) 0.8417(5) 0.0140(6) 0.083(3) Uani 1 1 d . . . . .
H43A H 0.2472 0.8816 -0.0159 0.100 Uiso 1 1 calc R . . . .
H43B H 0.3047 0.8493 0.0484 0.100 Uiso 1 1 calc R . . . .
C44 C 0.2643(4) 0.7925(6) -0.0367(6) 0.097(4) Uani 1 1 d . . . . .
H44A H 0.2913 0.7577 -0.0071 0.117 Uiso 1 1 calc R . . . .
H44B H 0.2866 0.8094 -0.0733 0.117 Uiso 1 1 calc R . . . .
O0AA O 0.6472(2) 0.7651(2) -0.2888(3) 0.0477(11) Uani 1 1 d . . . . .
C6 C 0.6011(3) 0.7618(3) -0.2700(3) 0.0350(11) Uani 1 1 d . . . . .
C7 C -0.0277(3) 0.7460(3) -0.3374(3) 0.0347(11) Uani 1 1 d . . . . .
C8 C 0.1137(3) 0.8991(3) -0.2545(5) 0.0563(19) Uani 1 1 d . . . . .
H8A H 0.1165 0.8723 -0.2979 0.084 Uiso 1 1 calc GR . . . .
H8B H 0.1467 0.8856 -0.2082 0.084 Uiso 1 1 calc GR . . . .
H8C H 0.1205 0.9443 -0.2655 0.084 Uiso 1 1 calc GR . . . .
C3BA C 0.5425(4) 0.5574(3) -0.1779(4) 0.063(2) Uani 1 1 d . . . . .
H3BA H 0.4990 0.5601 -0.1722 0.094 Uiso 1 1 calc GR . . . .
H3BB H 0.5733 0.5744 -0.1316 0.094 Uiso 1 1 calc GR . . . .
H3BC H 0.5529 0.5123 -0.1852 0.094 Uiso 1 1 calc GR . . . .
C10 C -0.0032(4) 0.9144(3) -0.3143(4) 0.0589(19) Uani 1 1 d . . . . .
H10A H -0.0463 0.9074 -0.3085 0.088 Uiso 1 1 calc GR . . . .
H10B H 0.0014 0.8903 -0.3588 0.088 Uiso 1 1 calc GR . . . .
H10C H 0.0030 0.9604 -0.3218 0.088 Uiso 1 1 calc GR . . . .
C11 C 0.0424(5) 0.9319(3) -0.1743(4) 0.064(2) Uani 1 1 d . . . . .
H11A H 0.0760 0.9188 -0.1282 0.096 Uiso 1 1 calc GR . . . .
H11B H 0.0002 0.9258 -0.1658 0.096 Uiso 1 1 calc GR . . . .
H11C H 0.0481 0.9774 -0.1851 0.096 Uiso 1 1 calc GR . . . .
C4 C 0.2798(4) 0.9162(3) -0.3097(4) 0.062(2) Uani 1 1 d . . . . .
H4A H 0.2381 0.9384 -0.3305 0.074 Uiso 1 1 calc R . . . .
H4B H 0.3133 0.9419 -0.3235 0.074 Uiso 1 1 calc R . . . .
O1 O 0.4368(2) 0.7357(3) -0.4070(2) 0.0536(12) Uani 1 1 d . . . . .
C2 C 0.4655(3) 0.7429(3) -0.3467(3) 0.0369(12) Uani 1 1 d . . . . .
O5 O -0.0581(2) 0.7548(2) -0.3998(2) 0.0454(10) 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
W1 P3 2.5622(13) . ?
W1 P4 2.5515(12) . ?
W1 S7 2.6008(12) . ?
W1 C1BA 2.026(6) . ?
W1 C16 1.821(5) . ?
W1 C7 2.003(6) . ?
W2 P5 2.5498(12) . ?
W2 S6 2.5995(14) . ?
W2 P8 2.5405(13) . ?
W2 C4AA 1.836(6) . ?
W2 C6 2.017(6) . ?
W2 C2 2.045(5) . ?
P3 C9 1.864(6) . ?
P3 C13 1.846(5) . ?
P3 C22 1.860(6) . ?
P4 C7AA 1.872(5) . ?
P4 C9AA 1.861(5) . ?
P4 C2BA 1.844(5) . ?
P5 C48 1.841(5) . ?
P5 C56 1.862(5) . ?
P5 C12 1.865(6) . ?
S6 C50 1.771(6) . ?
S7 C39 1.777(5) . ?
P8 C3AA 1.863(5) . ?
P8 C20 1.837(5) . ?
P8 C37 1.853(6) . ?
C3AA C8AA 1.521(7) . ?
C3AA C54 1.515(7) . ?
C20 C48 1.538(7) . ?
C4AA C52 1.486(8) . ?
C6AA C7AA 1.538(7) . ?
C6AA C40 1.528(7) . ?
C24 C9AA 1.534(7) . ?
C24 C75 1.537(7) . ?
C7AA C81 1.537(7) . ?
C8AA C61 1.547(7) . ?
C9AA C0BA 1.528(7) . ?
C2AA C39 1.383(8) . ?
C2AA C76 1.387(9) . ?
C33 C56 1.534(8) . ?
C33 C63 1.532(8) . ?
C34 C37 1.534(7) . ?
C34 C45 1.516(8) . ?
C37 C66 1.531(7) . ?
C39 C0AA 1.397(7) . ?
C40 C1AA 1.521(9) . ?
C0BA C89 1.533(8) . ?
C5AA C50 1.401(8) . ?
C5AA C95 1.389(9) . ?
C45 C74 1.517(9) . ?
C46 C83 1.529(7) . ?
C46 C4 1.513(9) . ?
C49 C76 1.382(10) . ?
C49 C84 1.380(10) . ?
C50 C55 1.392(8) . ?
C52 C67 1.530(8) . ?
C52 C72 1.526(8) . ?
C52 C3BA 1.536(8) . ?
C54 C98 1.531(8) . ?
C55 C86 1.383(9) . ?
C56 C83 1.534(7) . ?
C59 C61 1.511(9) . ?
C59 C98 1.524(10) . ?
C63 C4 1.521(10) . ?
C66 C90 1.529(9) . ?
C68 C81 1.529(7) . ?
C68 C1AA 1.526(8) . ?
C70 C75 1.511(9) . ?
C70 C89 1.521(9) . ?
C74 C90 1.525(10) . ?
C80 C86 1.381(11) . ?
C80 C95 1.383(10) . ?
C84 C0AA 1.381(9) . ?
O4 C1BA 1.132(7) . ?
C9 C14 1.539(7) . ?
C9 C21 1.527(7) . ?
C2BA C13 1.528(7) . ?
C12 C23 1.529(8) . ?
C12 C25 1.527(7) . ?
C14 C29 1.519(8) . ?
C15 C16 1.502(7) . ?
C15 C8 1.536(8) . ?
C15 C10 1.530(8) . ?
C15 C11 1.515(8) . ?
C18 C22 1.548(8) . ?
C18 C44 1.533(8) . ?
C21 C31 1.523(9) . ?
C22 C38 1.464(9) . ?
C23 C28 1.533(8) . ?
C25 C26 1.527(9) . ?
C26 C41 1.531(10) . ?
C28 C41 1.503(10) . ?
C29 C35 1.528(9) . ?
C31 C35 1.523(9) . ?
C36 C38 1.554(9) . ?
C36 C43 1.500(11) . ?
C43 C44 1.390(12) . ?
O0AA C6 1.147(7) . ?
C7 O5 1.153(7) . ?
O1 C2 1.106(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
P3 W1 S7 88.96(4) . . ?
P4 W1 P3 78.70(4) . . ?
P4 W1 S7 85.90(4) . . ?
C1BA W1 P3 95.80(15) . . ?
C1BA W1 P4 171.83(16) . . ?
C1BA W1 S7 87.97(15) . . ?
C16 W1 P3 98.96(15) . . ?
C16 W1 P4 99.07(15) . . ?
C16 W1 S7 171.32(15) . . ?
C16 W1 C1BA 87.7(2) . . ?
C16 W1 C7 86.3(2) . . ?
C7 W1 P3 172.29(16) . . ?
C7 W1 P4 94.95(16) . . ?
C7 W1 S7 86.20(16) . . ?
C7 W1 C1BA 90.0(2) . . ?
P5 W2 S6 86.39(4) . . ?
P8 W2 P5 79.12(4) . . ?
P8 W2 S6 90.20(4) . . ?
C4AA W2 P5 99.00(15) . . ?
C4AA W2 S6 172.03(16) . . ?
C4AA W2 P8 96.55(16) . . ?
C4AA W2 C6 87.0(2) . . ?
C4AA W2 C2 86.8(2) . . ?
C6 W2 P5 172.28(17) . . ?
C6 W2 S6 88.21(16) . . ?
C6 W2 P8 95.40(16) . . ?
C6 W2 C2 91.4(2) . . ?
C2 W2 P5 93.77(16) . . ?
C2 W2 S6 86.95(18) . . ?
C2 W2 P8 172.51(16) . . ?
C9 P3 W1 114.34(16) . . ?
C13 P3 W1 106.07(17) . . ?
C13 P3 C9 102.7(2) . . ?
C13 P3 C22 104.9(3) . . ?
C22 P3 W1 123.8(2) . . ?
C22 P3 C9 102.8(3) . . ?
C7AA P4 W1 122.51(17) . . ?
C9AA P4 W1 113.10(16) . . ?
C9AA P4 C7AA 103.5(2) . . ?
C2BA P4 W1 107.72(16) . . ?
C2BA P4 C7AA 104.6(2) . . ?
C2BA P4 C9AA 103.5(2) . . ?
C48 P5 W2 107.47(17) . . ?
C48 P5 C56 104.4(2) . . ?
C48 P5 C12 103.7(3) . . ?
C56 P5 W2 122.75(18) . . ?
C56 P5 C12 103.5(2) . . ?
C12 P5 W2 113.18(17) . . ?
C50 S6 W2 107.23(18) . . ?
C39 S7 W1 107.36(17) . . ?
C3AA P8 W2 116.65(18) . . ?
C20 P8 W2 106.47(17) . . ?
C20 P8 C3AA 102.4(2) . . ?
C20 P8 C37 102.9(3) . . ?
C37 P8 W2 114.09(17) . . ?
C37 P8 C3AA 112.4(2) . . ?
C8AA C3AA P8 113.5(4) . . ?
C54 C3AA P8 113.8(4) . . ?
C54 C3AA C8AA 111.2(5) . . ?
C48 C20 P8 108.6(3) . . ?
C52 C4AA W2 170.1(4) . . ?
C40 C6AA C7AA 110.2(4) . . ?
C9AA C24 C75 111.5(5) . . ?
C6AA C7AA P4 113.7(3) . . ?
C81 C7AA P4 111.2(3) . . ?
C81 C7AA C6AA 110.0(4) . . ?
C3AA C8AA C61 111.3(5) . . ?
C24 C9AA P4 109.0(3) . . ?
C0BA C9AA P4 115.3(4) . . ?
C0BA C9AA C24 111.4(4) . . ?
C39 C2AA C76 120.5(6) . . ?
C63 C33 C56 110.4(5) . . ?
C45 C34 C37 110.9(5) . . ?
C34 C37 P8 112.4(4) . . ?
C66 C37 P8 119.7(4) . . ?
C66 C37 C34 109.9(5) . . ?
C2AA C39 S7 119.8(4) . . ?
C2AA C39 C0AA 118.7(5) . . ?
C0AA C39 S7 121.5(5) . . ?
C1AA C40 C6AA 112.2(5) . . ?
C9AA C0BA C89 111.5(5) . . ?
C95 C5AA C50 120.8(6) . . ?
C34 C45 C74 111.5(5) . . ?
C4 C46 C83 110.8(5) . . ?
C20 C48 P5 109.3(4) . . ?
C84 C49 C76 119.4(6) . . ?
C5AA C50 S6 120.3(4) . . ?
C55 C50 S6 121.6(5) . . ?
C55 C50 C5AA 118.0(6) . . ?
C4AA C52 C67 109.2(5) . . ?
C4AA C52 C72 110.4(5) . . ?
C4AA C52 C3BA 109.5(5) . . ?
C67 C52 C3BA 109.2(6) . . ?
C72 C52 C67 109.0(5) . . ?
C72 C52 C3BA 109.5(6) . . ?
C3AA C54 C98 111.2(5) . . ?
C86 C55 C50 120.6(6) . . ?
C33 C56 P5 113.7(4) . . ?
C33 C56 C83 109.4(5) . . ?
C83 C56 P5 111.2(4) . . ?
C61 C59 C98 110.8(5) . . ?
C59 C61 C8AA 110.1(5) . . ?
C4 C63 C33 112.1(5) . . ?
C90 C66 C37 109.9(5) . . ?
C1AA C68 C81 110.5(5) . . ?
C75 C70 C89 110.6(5) . . ?
C45 C74 C90 111.7(6) . . ?
C70 C75 C24 110.8(5) . . ?
C49 C76 C2AA 120.5(6) . . ?
C86 C80 C95 118.9(6) . . ?
C68 C81 C7AA 110.8(4) . . ?
C46 C83 C56 111.1(5) . . ?
C49 C84 C0AA 120.5(6) . . ?
C80 C86 C55 121.3(6) . . ?
C70 C89 C0BA 111.9(5) . . ?
C74 C90 C66 111.7(6) . . ?
C80 C95 C5AA 120.4(7) . . ?
C59 C98 C54 110.8(6) . . ?
C14 C9 P3 110.8(4) . . ?
C21 C9 P3 117.3(4) . . ?
C21 C9 C14 110.7(4) . . ?
O4 C1BA W1 178.6(5) . . ?
C13 C2BA P4 109.5(4) . . ?
C23 C12 P5 110.3(4) . . ?
C25 C12 P5 115.2(4) . . ?
C25 C12 C23 111.2(5) . . ?
C2BA C13 P3 108.0(3) . . ?
C29 C14 C9 110.2(5) . . ?
C16 C15 C8 109.4(4) . . ?
C16 C15 C10 110.3(5) . . ?
C16 C15 C11 109.8(5) . . ?
C10 C15 C8 108.2(5) . . ?
C11 C15 C8 110.0(6) . . ?
C11 C15 C10 109.1(6) . . ?
C15 C16 W1 168.2(4) . . ?
C44 C18 C22 110.9(5) . . ?
C31 C21 C9 110.6(5) . . ?
C18 C22 P3 111.0(4) . . ?
C38 C22 P3 115.3(5) . . ?
C38 C22 C18 111.7(6) . . ?
C12 C23 C28 112.0(5) . . ?
C84 C0AA C39 120.5(6) . . ?
C26 C25 C12 111.4(5) . . ?
C25 C26 C41 111.7(6) . . ?
C41 C28 C23 110.5(6) . . ?
C14 C29 C35 111.6(5) . . ?
C21 C31 C35 111.9(6) . . ?
C40 C1AA C68 110.9(5) . . ?
C31 C35 C29 111.3(5) . . ?
C43 C36 C38 111.9(6) . . ?
C22 C38 C36 110.8(6) . . ?
C28 C41 C26 110.8(5) . . ?
C44 C43 C36 115.6(7) . . ?
C43 C44 C18 116.8(8) . . ?
O0AA C6 W2 178.3(5) . . ?
O5 C7 W1 177.5(5) . . ?
C46 C4 C63 111.0(6) . . ?
O1 C2 W2 177.7(6) . . ?


