# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_tm106_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H41 B F15 O P'
_chemical_formula_weight         912.55

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   11.5255(6)
_cell_length_b                   14.8611(8)
_cell_length_c                   11.8913(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.265(3)
_cell_angle_gamma                90.00
_cell_volume                     2035.17(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6637
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      26.34

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9763
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18720
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8663
_reflns_number_gt                6277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0493P)²+0.2380P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(11)
_refine_ls_number_reflns         8663
_refine_ls_number_parameters     559
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.14820(7) 0.35178(6) 0.39619(7) 0.02018(18) Uani 1 1 d . . .
F1 F 0.47387(16) 0.40894(16) -0.20754(16) 0.0377(5) Uani 1 1 d . . .
F2 F 0.58084(18) 0.49161(17) -0.37080(16) 0.0441(6) Uani 1 1 d . . .
F3 F 0.80675(19) 0.54422(16) -0.34300(18) 0.0451(6) Uani 1 1 d . . .
F4 F 0.92299(16) 0.51306(16) -0.14286(18) 0.0431(6) Uani 1 1 d . . .
F5 F 0.81743(15) 0.42911(14) 0.02389(15) 0.0315(5) Uani 1 1 d . . .
F6 F 0.78741(16) 0.25761(14) -0.07249(15) 0.0300(5) Uani 1 1 d . . .
F7 F 0.87557(17) 0.10553(15) 0.00582(19) 0.0418(5) Uani 1 1 d . . .
F8 F 0.79680(19) 0.02951(14) 0.19670(18) 0.0423(6) Uani 1 1 d . . .
F9 F 0.62107(19) 0.11061(15) 0.30534(17) 0.0432(6) Uani 1 1 d . . .
F10 F 0.53064(16) 0.26453(14) 0.22932(15) 0.0341(5) Uani 1 1 d . . .
F11 F 0.40532(15) 0.50381(13) 0.01908(15) 0.0270(4) Uani 1 1 d . . .
F12 F 0.36214(15) 0.62338(13) 0.17856(16) 0.0304(5) Uani 1 1 d . . .
F13 F 0.50670(18) 0.63944(15) 0.36294(17) 0.0419(6) Uani 1 1 d . . .
F14 F 0.69359(17) 0.52811(15) 0.38913(17) 0.0406(6) Uani 1 1 d . . .
F15 F 0.73177(15) 0.40024(14) 0.23931(15) 0.0289(4) Uani 1 1 d . . .
O1 O 0.46107(16) 0.33098(14) 0.00198(17) 0.0209(5) Uani 1 1 d . . .
C1 C 0.6407(3) 0.4119(2) -0.0825(2) 0.0202(7) Uani 1 1 d . . .
C2 C 0.5858(3) 0.4322(2) -0.1850(3) 0.0250(7) Uani 1 1 d . . .
C3 C 0.6387(3) 0.4765(3) -0.2722(3) 0.0296(8) Uani 1 1 d . . .
C4 C 0.7533(3) 0.5032(3) -0.2580(3) 0.0317(8) Uani 1 1 d . . .
C5 C 0.8112(3) 0.4868(2) -0.1576(3) 0.0286(8) Uani 1 1 d . . .
C6 C 0.7549(3) 0.4436(2) -0.0730(3) 0.0240(7) Uani 1 1 d . . .
C7 C 0.6553(2) 0.2725(2) 0.0752(2) 0.0179(6) Uani 1 1 d . . .
C8 C 0.7435(3) 0.2261(2) 0.0243(3) 0.0208(7) Uani 1 1 d . . .
C9 C 0.7914(3) 0.1468(2) 0.0622(3) 0.0260(8) Uani 1 1 d . . .
C10 C 0.7522(3) 0.1075(2) 0.1583(3) 0.0269(8) Uani 1 1 d . . .
C11 C 0.6634(3) 0.1495(2) 0.2126(3) 0.0286(8) Uani 1 1 d . . .
C12 C 0.6180(3) 0.2286(2) 0.1707(3) 0.0234(7) Uani 1 1 d . . .
C13 C 0.5676(2) 0.4417(2) 0.1225(2) 0.0189(7) Uani 1 1 d . . .
C14 C 0.4774(2) 0.5038(2) 0.1123(2) 0.0192(7) Uani 1 1 d . . .
C15 C 0.4550(3) 0.5681(2) 0.1918(3) 0.0211(7) Uani 1 1 d . . .
C16 C 0.5276(3) 0.5770(2) 0.2845(3) 0.0256(8) Uani 1 1 d . . .
C17 C 0.6211(3) 0.5198(2) 0.2981(3) 0.0250(7) Uani 1 1 d . . .
C18 C 0.6386(3) 0.4537(2) 0.2180(3) 0.0223(7) Uani 1 1 d . . .
C19 C 0.4404(3) 0.2526(2) -0.0619(3) 0.0233(7) Uani 1 1 d . . .
H19A H 0.4701 0.1995 -0.0197 0.028 Uiso 1 1 calc R . .
H19B H 0.4814 0.2565 -0.1334 0.028 Uiso 1 1 calc R . .
C20 C 0.3114(3) 0.2430(2) -0.0864(2) 0.0209(7) Uani 1 1 d . . .
C21 C 0.2427(3) 0.3177(2) -0.1101(3) 0.0239(7) Uani 1 1 d . . .
H21A H 0.2774 0.3755 -0.1136 0.029 Uiso 1 1 calc R . .
C22 C 0.1237(3) 0.3086(3) -0.1287(3) 0.0293(8) Uani 1 1 d . . .
H22A H 0.0772 0.3602 -0.1442 0.035 Uiso 1 1 calc R . .
C23 C 0.0725(3) 0.2240(3) -0.1245(3) 0.0322(9) Uani 1 1 d . . .
H23A H -0.0091 0.2178 -0.1356 0.039 Uiso 1 1 calc R . .
C24 C 0.1411(3) 0.1487(3) -0.1041(3) 0.0335(9) Uani 1 1 d . . .
H24A H 0.1071 0.0905 -0.1044 0.040 Uiso 1 1 calc R . .
C25 C 0.2589(3) 0.1586(3) -0.0833(3) 0.0275(8) Uani 1 1 d . . .
H25A H 0.3051 0.1070 -0.0665 0.033 Uiso 1 1 calc R . .
C26 C 0.2997(3) 0.3261(3) 0.4557(3) 0.0289(8) Uani 1 1 d . . .
C27 C 0.3075(3) 0.3414(4) 0.5831(3) 0.0551(13) Uani 1 1 d . . .
H27A H 0.3862 0.3275 0.6120 0.083 Uiso 1 1 calc R . .
H27B H 0.2518 0.3020 0.6194 0.083 Uiso 1 1 calc R . .
H27C H 0.2892 0.4043 0.5995 0.083 Uiso 1 1 calc R . .
C28 C 0.3927(3) 0.3856(3) 0.4014(4) 0.0457(11) Uani 1 1 d . . .
H28A H 0.4697 0.3703 0.4338 0.069 Uiso 1 1 calc R . .
H28B H 0.3762 0.4492 0.4159 0.069 Uiso 1 1 calc R . .
H28C H 0.3911 0.3750 0.3200 0.069 Uiso 1 1 calc R . .
C29 C 0.3336(3) 0.2271(3) 0.4331(3) 0.0361(9) Uani 1 1 d . . .
H29A H 0.4121 0.2157 0.4645 0.054 Uiso 1 1 calc R . .
H29B H 0.3315 0.2161 0.3518 0.054 Uiso 1 1 calc R . .
H29C H 0.2786 0.1868 0.4687 0.054 Uiso 1 1 calc R . .
C30 C 0.1397(3) 0.3454(3) 0.2378(3) 0.0264(7) Uani 1 1 d . . .
C31 C 0.2069(4) 0.2663(3) 0.1937(3) 0.0462(11) Uani 1 1 d . . .
H31A H 0.2002 0.2657 0.1113 0.069 Uiso 1 1 calc R . .
H31B H 0.1751 0.2103 0.2231 0.069 Uiso 1 1 calc R . .
H31C H 0.2888 0.2718 0.2181 0.069 Uiso 1 1 calc R . .
C32 C 0.1875(4) 0.4329(3) 0.1840(4) 0.0577(13) Uani 1 1 d . . .
H32A H 0.1823 0.4276 0.1018 0.087 Uiso 1 1 calc R . .
H32B H 0.2688 0.4415 0.2090 0.087 Uiso 1 1 calc R . .
H32C H 0.1415 0.4846 0.2073 0.087 Uiso 1 1 calc R . .
C33 C 0.0129(3) 0.3339(3) 0.1949(3) 0.0472(11) Uani 1 1 d . . .
H33A H 0.0098 0.3307 0.1125 0.071 Uiso 1 1 calc R . .
H33B H -0.0330 0.3854 0.2191 0.071 Uiso 1 1 calc R . .
H33C H -0.0189 0.2784 0.2258 0.071 Uiso 1 1 calc R . .
C34 C 0.0932(3) 0.4630(3) 0.4505(3) 0.0350(9) Uani 1 1 d . . .
C35 C 0.0662(4) 0.4567(3) 0.5763(4) 0.0566(13) Uani 1 1 d . . .
H35A H 0.0372 0.5149 0.6020 0.085 Uiso 1 1 calc R . .
H35B H 0.1372 0.4410 0.6200 0.085 Uiso 1 1 calc R . .
H35C H 0.0072 0.4103 0.5867 0.085 Uiso 1 1 calc R . .
C36 C -0.0185(3) 0.4921(3) 0.3896(4) 0.0518(11) Uani 1 1 d . . .
H36A H -0.0446 0.5493 0.4209 0.078 Uiso 1 1 calc R . .
H36B H -0.0783 0.4461 0.3992 0.078 Uiso 1 1 calc R . .
H36C H -0.0050 0.4996 0.3093 0.078 Uiso 1 1 calc R . .
C37 C 0.1871(4) 0.5367(3) 0.4387(5) 0.0654(15) Uani 1 1 d . . .
H37A H 0.1581 0.5940 0.4671 0.098 Uiso 1 1 calc R . .
H37B H 0.2051 0.5434 0.3593 0.098 Uiso 1 1 calc R . .
H37C H 0.2576 0.5194 0.4823 0.098 Uiso 1 1 calc R . .
C38 C 0.0626(3) 0.2553(2) 0.4473(3) 0.0278(8) Uani 1 1 d . . .
H38A H 0.0562 0.2115 0.3847 0.033 Uiso 1 1 calc R . .
H38B H 0.1105 0.2263 0.5080 0.033 Uiso 1 1 calc R . .
C39 C -0.0591(3) 0.2661(2) 0.4917(3) 0.0247(7) Uani 1 1 d . . .
C40 C -0.1578(3) 0.2714(3) 0.4230(3) 0.0311(8) Uani 1 1 d . . .
H40A H -0.1513 0.2700 0.3437 0.037 Uiso 1 1 calc R . .
C41 C -0.2673(3) 0.2789(3) 0.4683(3) 0.0408(10) Uani 1 1 d . . .
H41A H -0.3344 0.2833 0.4196 0.049 Uiso 1 1 calc R . .
C42 C -0.2787(3) 0.2800(3) 0.5813(3) 0.0405(10) Uani 1 1 d . . .
H42A H -0.3532 0.2857 0.6118 0.049 Uiso 1 1 calc R . .
C43 C -0.1803(4) 0.2727(3) 0.6521(3) 0.0507(12) Uani 1 1 d . . .
H43A H -0.1873 0.2727 0.7315 0.061 Uiso 1 1 calc R . .
C44 C -0.0723(3) 0.2653(3) 0.6068(3) 0.0434(10) Uani 1 1 d . . .
H44A H -0.0055 0.2596 0.6557 0.052 Uiso 1 1 calc R . .
B1 B 0.5797(3) 0.3611(3) 0.0263(3) 0.0189(7) 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
P1 C38 1.856(3) . ?
P1 C30 1.885(3) . ?
P1 C34 1.893(4) . ?
P1 C26 1.896(3) . ?
F1 C2 1.352(4) . ?
F2 C3 1.344(4) . ?
F3 C4 1.349(4) . ?
F4 C5 1.351(4) . ?
F5 C6 1.351(4) . ?
F6 C8 1.359(3) . ?
F7 C9 1.348(4) . ?
F8 C10 1.341(4) . ?
F9 C11 1.353(4) . ?
F10 C12 1.356(4) . ?
F11 C14 1.358(3) . ?
F12 C15 1.353(4) . ?
F13 C16 1.344(4) . ?
F14 C17 1.346(4) . ?
F15 C18 1.352(4) . ?
O1 C19 1.405(4) . ?
O1 B1 1.457(4) . ?
C1 C2 1.384(4) . ?
C1 C6 1.399(4) . ?
C1 B1 1.676(5) . ?
C2 C3 1.389(5) . ?
C3 C4 1.383(5) . ?
C4 C5 1.367(5) . ?
C5 C6 1.377(5) . ?
C7 C8 1.387(4) . ?
C7 C12 1.393(4) . ?
C7 B1 1.670(5) . ?
C8 C9 1.370(5) . ?
C9 C10 1.375(5) . ?
C10 C11 1.380(5) . ?
C11 C12 1.372(5) . ?
C13 C18 1.385(4) . ?
C13 C14 1.392(4) . ?
C13 B1 1.666(5) . ?
C14 C15 1.377(4) . ?
C15 C16 1.364(4) . ?
C16 C17 1.377(5) . ?
C17 C18 1.389(5) . ?
C19 C20 1.511(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.386(5) . ?
C20 C25 1.394(5) . ?
C21 C22 1.387(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.391(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.386(5) . ?
C23 H23A 0.9500 . ?
C24 C25 1.377(5) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 C27 1.532(5) . ?
C26 C29 1.549(5) . ?
C26 C28 1.550(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.512(5) . ?
C30 C33 1.538(5) . ?
C30 C32 1.561(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.515(5) . ?
C34 C35 1.543(6) . ?
C34 C37 1.550(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.526(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.376(5) . ?
C39 C44 1.383(5) . ?
C40 C41 1.396(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.355(5) . ?
C41 H41A 0.9500 . ?
C42 C43 1.390(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.380(5) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?

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
C38 P1 C30 106.31(16) . . ?
C38 P1 C34 111.92(16) . . ?
C30 P1 C34 112.33(17) . . ?
C38 P1 C26 102.50(16) . . ?
C30 P1 C26 111.93(14) . . ?
C34 P1 C26 111.34(16) . . ?
C19 O1 B1 120.0(2) . . ?
C2 C1 C6 113.2(3) . . ?
C2 C1 B1 126.0(3) . . ?
C6 C1 B1 120.7(3) . . ?
F1 C2 C1 121.1(3) . . ?
F1 C2 C3 114.6(3) . . ?
C1 C2 C3 124.2(3) . . ?
F2 C3 C4 119.8(3) . . ?
F2 C3 C2 120.8(3) . . ?
C4 C3 C2 119.3(3) . . ?
F3 C4 C5 120.9(3) . . ?
F3 C4 C3 120.0(3) . . ?
C5 C4 C3 119.1(3) . . ?
F4 C5 C4 119.5(3) . . ?
F4 C5 C6 120.9(3) . . ?
C4 C5 C6 119.6(3) . . ?
F5 C6 C5 116.5(3) . . ?
F5 C6 C1 118.9(3) . . ?
C5 C6 C1 124.5(3) . . ?
C8 C7 C12 112.2(3) . . ?
C8 C7 B1 128.4(3) . . ?
C12 C7 B1 118.7(3) . . ?
F6 C8 C9 114.6(3) . . ?
F6 C8 C7 120.1(3) . . ?
C9 C8 C7 125.3(3) . . ?
F7 C9 C8 121.1(3) . . ?
F7 C9 C10 119.1(3) . . ?
C8 C9 C10 119.8(3) . . ?
F8 C10 C9 121.0(3) . . ?
F8 C10 C11 120.8(3) . . ?
C9 C10 C11 118.1(3) . . ?
F9 C11 C12 121.1(3) . . ?
F9 C11 C10 119.1(3) . . ?
C12 C11 C10 119.8(3) . . ?
F10 C12 C11 115.6(3) . . ?
F10 C12 C7 119.6(3) . . ?
C11 C12 C7 124.9(3) . . ?
C18 C13 C14 113.7(3) . . ?
C18 C13 B1 126.4(3) . . ?
C14 C13 B1 119.9(3) . . ?
F11 C14 C15 115.8(3) . . ?
F11 C14 C13 120.2(3) . . ?
C15 C14 C13 124.1(3) . . ?
F12 C15 C16 119.5(3) . . ?
F12 C15 C14 120.7(3) . . ?
C16 C15 C14 119.8(3) . . ?
F13 C16 C15 120.4(3) . . ?
F13 C16 C17 120.4(3) . . ?
C15 C16 C17 119.2(3) . . ?
F14 C17 C16 119.7(3) . . ?
F14 C17 C18 120.9(3) . . ?
C16 C17 C18 119.3(3) . . ?
F15 C18 C13 121.2(3) . . ?
F15 C18 C17 115.0(3) . . ?
C13 C18 C17 123.8(3) . . ?
O1 C19 C20 109.1(2) . . ?
O1 C19 H19A 109.9 . . ?
C20 C19 H19A 109.9 . . ?
O1 C19 H19B 109.9 . . ?
C20 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C21 C20 C25 118.7(3) . . ?
C21 C20 C19 120.9(3) . . ?
C25 C20 C19 120.4(3) . . ?
C20 C21 C22 120.6(3) . . ?
C20 C21 H21A 119.7 . . ?
C22 C21 H21A 119.7 . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H23A 120.1 . . ?
C22 C23 H23A 120.1 . . ?
C25 C24 C23 119.8(3) . . ?
C25 C24 H24A 120.1 . . ?
C23 C24 H24A 120.1 . . ?
C24 C25 C20 121.1(3) . . ?
C24 C25 H25A 119.4 . . ?
C20 C25 H25A 119.4 . . ?
C27 C26 C29 107.9(3) . . ?
C27 C26 C28 108.3(3) . . ?
C29 C26 C28 106.6(3) . . ?
C27 C26 P1 110.9(2) . . ?
C29 C26 P1 111.1(2) . . ?
C28 C26 P1 111.8(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C33 107.0(3) . . ?
C31 C30 C32 108.1(3) . . ?
C33 C30 C32 107.6(3) . . ?
C31 C30 P1 112.2(2) . . ?
C33 C30 P1 110.4(2) . . ?
C32 C30 P1 111.3(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 106.3(3) . . ?
C36 C34 C37 109.8(4) . . ?
C35 C34 C37 107.4(4) . . ?
C36 C34 P1 112.1(3) . . ?
C35 C34 P1 111.2(3) . . ?
C37 C34 P1 110.0(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 P1 122.7(2) . . ?
C39 C38 H38A 106.7 . . ?
P1 C38 H38A 106.7 . . ?
C39 C38 H38B 106.7 . . ?
P1 C38 H38B 106.7 . . ?
H38A C38 H38B 106.6 . . ?
C40 C39 C44 117.9(3) . . ?
C40 C39 C38 123.4(3) . . ?
C44 C39 C38 118.6(3) . . ?
C39 C40 C41 121.0(3) . . ?
C39 C40 H40A 119.5 . . ?
C41 C40 H40A 119.5 . . ?
C42 C41 C40 120.5(4) . . ?
C42 C41 H41A 119.7 . . ?
C40 C41 H41A 119.7 . . ?
C41 C42 C43 119.4(3) . . ?
C41 C42 H42A 120.3 . . ?
C43 C42 H42A 120.3 . . ?
C44 C43 C42 119.7(3) . . ?
C44 C43 H43A 120.1 . . ?
C42 C43 H43A 120.1 . . ?
C43 C44 C39 121.5(4) . . ?
C43 C44 H44A 119.3 . . ?
C39 C44 H44A 119.3 . . ?
O1 B1 C13 104.7(2) . . ?
O1 B1 C7 107.4(3) . . ?
C13 B1 C7 112.6(2) . . ?
O1 B1 C1 113.8(2) . . ?
C13 B1 C1 104.8(3) . . ?
C7 B1 C1 113.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 F1 -178.1(3) . . . . ?
B1 C1 C2 F1 -2.1(5) . . . . ?
C6 C1 C2 C3 2.3(5) . . . . ?
B1 C1 C2 C3 178.3(3) . . . . ?
F1 C2 C3 F2 -1.6(5) . . . . ?
C1 C2 C3 F2 178.0(3) . . . . ?
F1 C2 C3 C4 -179.9(3) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
F2 C3 C4 F3 -0.1(5) . . . . ?
C2 C3 C4 F3 178.2(3) . . . . ?
F2 C3 C4 C5 -179.5(3) . . . . ?
C2 C3 C4 C5 -1.2(5) . . . . ?
F3 C4 C5 F4 0.8(5) . . . . ?
C3 C4 C5 F4 -179.7(3) . . . . ?
F3 C4 C5 C6 -179.0(3) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
F4 C5 C6 F5 -0.1(5) . . . . ?
C4 C5 C6 F5 179.7(3) . . . . ?
F4 C5 C6 C1 -178.0(3) . . . . ?
C4 C5 C6 C1 1.8(5) . . . . ?
C2 C1 C6 F5 179.1(3) . . . . ?
B1 C1 C6 F5 2.9(4) . . . . ?
C2 C1 C6 C5 -3.1(5) . . . . ?
B1 C1 C6 C5 -179.3(3) . . . . ?
C12 C7 C8 F6 177.6(3) . . . . ?
B1 C7 C8 F6 7.7(5) . . . . ?
C12 C7 C8 C9 -0.9(5) . . . . ?
B1 C7 C8 C9 -170.8(3) . . . . ?
F6 C8 C9 F7 0.2(4) . . . . ?
C7 C8 C9 F7 178.8(3) . . . . ?
F6 C8 C9 C10 -178.7(3) . . . . ?
C7 C8 C9 C10 -0.2(5) . . . . ?
F7 C9 C10 F8 0.4(5) . . . . ?
C8 C9 C10 F8 179.4(3) . . . . ?
F7 C9 C10 C11 -177.9(3) . . . . ?
C8 C9 C10 C11 1.0(5) . . . . ?
F8 C10 C11 F9 -0.3(5) . . . . ?
C9 C10 C11 F9 178.0(3) . . . . ?
F8 C10 C11 C12 -179.1(3) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
F9 C11 C12 F10 0.9(5) . . . . ?
C10 C11 C12 F10 179.6(3) . . . . ?
F9 C11 C12 C7 -179.2(3) . . . . ?
C10 C11 C12 C7 -0.4(5) . . . . ?
C8 C7 C12 F10 -178.9(3) . . . . ?
B1 C7 C12 F10 -7.8(4) . . . . ?
C8 C7 C12 C11 1.2(5) . . . . ?
B1 C7 C12 C11 172.2(3) . . . . ?
C18 C13 C14 F11 175.7(3) . . . . ?
B1 C13 C14 F11 -5.8(4) . . . . ?
C18 C13 C14 C15 -3.8(4) . . . . ?
B1 C13 C14 C15 174.7(3) . . . . ?
F11 C14 C15 F12 3.8(4) . . . . ?
C13 C14 C15 F12 -176.7(3) . . . . ?
F11 C14 C15 C16 -175.6(3) . . . . ?
C13 C14 C15 C16 3.9(5) . . . . ?
F12 C15 C16 F13 0.7(5) . . . . ?
C14 C15 C16 F13 -179.9(3) . . . . ?
F12 C15 C16 C17 179.2(3) . . . . ?
C14 C15 C16 C17 -1.4(5) . . . . ?
F13 C16 C17 F14 -1.7(5) . . . . ?
C15 C16 C17 F14 179.8(3) . . . . ?
F13 C16 C17 C18 177.7(3) . . . . ?
C15 C16 C17 C18 -0.9(5) . . . . ?
C14 C13 C18 F15 -178.5(3) . . . . ?
B1 C13 C18 F15 3.1(5) . . . . ?
C14 C13 C18 C17 1.4(4) . . . . ?
B1 C13 C18 C17 -177.0(3) . . . . ?
F14 C17 C18 F15 0.1(5) . . . . ?
C16 C17 C18 F15 -179.3(3) . . . . ?
F14 C17 C18 C13 -179.8(3) . . . . ?
C16 C17 C18 C13 0.8(5) . . . . ?
B1 O1 C19 C20 -173.2(3) . . . . ?
O1 C19 C20 C21 38.1(4) . . . . ?
O1 C19 C20 C25 -140.6(3) . . . . ?
C25 C20 C21 C22 0.9(5) . . . . ?
C19 C20 C21 C22 -177.7(3) . . . . ?
C20 C21 C22 C23 -0.5(5) . . . . ?
C21 C22 C23 C24 -1.3(5) . . . . ?
C22 C23 C24 C25 2.8(5) . . . . ?
C23 C24 C25 C20 -2.4(5) . . . . ?
C21 C20 C25 C24 0.5(5) . . . . ?
C19 C20 C25 C24 179.2(3) . . . . ?
C38 P1 C26 C27 -72.4(3) . . . . ?
C30 P1 C26 C27 174.1(3) . . . . ?
C34 P1 C26 C27 47.4(3) . . . . ?
C38 P1 C26 C29 47.6(3) . . . . ?
C30 P1 C26 C29 -66.0(3) . . . . ?
C34 P1 C26 C29 167.4(2) . . . . ?
C38 P1 C26 C28 166.7(3) . . . . ?
C30 P1 C26 C28 53.1(3) . . . . ?
C34 P1 C26 C28 -73.5(3) . . . . ?
C38 P1 C30 C31 -69.8(3) . . . . ?
C34 P1 C30 C31 167.5(3) . . . . ?
C26 P1 C30 C31 41.3(3) . . . . ?
C38 P1 C30 C33 49.4(3) . . . . ?
C34 P1 C30 C33 -73.3(3) . . . . ?
C26 P1 C30 C33 160.6(3) . . . . ?
C38 P1 C30 C32 168.9(3) . . . . ?
C34 P1 C30 C32 46.1(3) . . . . ?
C26 P1 C30 C32 -80.0(3) . . . . ?
C38 P1 C34 C36 -75.4(3) . . . . ?
C30 P1 C34 C36 44.1(3) . . . . ?
C26 P1 C34 C36 170.5(3) . . . . ?
C38 P1 C34 C35 43.3(3) . . . . ?
C30 P1 C34 C35 162.9(3) . . . . ?
C26 P1 C34 C35 -70.7(3) . . . . ?
C38 P1 C34 C37 162.1(3) . . . . ?
C30 P1 C34 C37 -78.4(3) . . . . ?
C26 P1 C34 C37 48.1(4) . . . . ?
C30 P1 C38 C39 -103.4(3) . . . . ?
C34 P1 C38 C39 19.6(3) . . . . ?
C26 P1 C38 C39 139.0(3) . . . . ?
P1 C38 C39 C40 81.9(4) . . . . ?
P1 C38 C39 C44 -101.9(4) . . . . ?
C44 C39 C40 C41 2.1(6) . . . . ?
C38 C39 C40 C41 178.3(3) . . . . ?
C39 C40 C41 C42 -0.7(6) . . . . ?
C40 C41 C42 C43 -0.7(6) . . . . ?
C41 C42 C43 C44 0.7(7) . . . . ?
C42 C43 C44 C39 0.8(7) . . . . ?
C40 C39 C44 C43 -2.1(6) . . . . ?
C38 C39 C44 C43 -178.5(4) . . . . ?
C19 O1 B1 C13 -169.2(2) . . . . ?
C19 O1 B1 C7 -49.3(3) . . . . ?
C19 O1 B1 C1 77.0(4) . . . . ?
C18 C13 B1 O1 137.2(3) . . . . ?
C14 C13 B1 O1 -41.1(4) . . . . ?
C18 C13 B1 C7 20.8(4) . . . . ?
C14 C13 B1 C7 -157.4(3) . . . . ?
C18 C13 B1 C1 -102.7(3) . . . . ?
C14 C13 B1 C1 79.0(3) . . . . ?
C8 C7 B1 O1 111.4(3) . . . . ?
C12 C7 B1 O1 -58.0(3) . . . . ?
C8 C7 B1 C13 -133.9(3) . . . . ?
C12 C7 B1 C13 56.7(4) . . . . ?
C8 C7 B1 C1 -15.2(4) . . . . ?
C12 C7 B1 C1 175.4(3) . . . . ?
C2 C1 B1 O1 5.2(5) . . . . ?
C6 C1 B1 O1 -179.1(3) . . . . ?
C2 C1 B1 C13 -108.6(3) . . . . ?
C6 C1 B1 C13 67.1(3) . . . . ?
C2 C1 B1 C7 128.3(3) . . . . ?
C6 C1 B1 C7 -56.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 991775'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[tBu2PH(C6H5)CPh2][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H34 P, C F3 O3 S'
_chemical_formula_sum            'C28 H34 F3 O3 P S'
_chemical_formula_weight         538.58

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/N'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   12.3858(12)
_cell_length_b                   10.4816(10)
_cell_length_c                   21.683(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.545(2)
_cell_angle_gamma                90.00
_cell_volume                     2809.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9806
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =   0.458473

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14348
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.87
_reflns_number_total             6584
_reflns_number_gt                4303
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0662P)²+1.5287P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6584
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1245
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H1 H 0.288(2) 0.558(2) 0.0347(11) 0.041(7) Uiso 1 1 d . . .
C1 C 0.41541(19) 0.8103(2) -0.22015(10) 0.0323(5) Uani 1 1 d . . .
C2 C 0.39066(18) 0.7823(2) -0.16122(10) 0.0299(5) Uani 1 1 d . . .
C3 C 0.37856(19) 0.8794(2) -0.11346(10) 0.0314(5) Uani 1 1 d . . .
H3 H 0.3757 0.9665 -0.1256 0.038 Uiso 1 1 calc R . .
C4 C 0.37137(19) 0.8519(2) -0.05401(10) 0.0316(5) Uani 1 1 d . . .
H4 H 0.3612 0.9194 -0.0257 0.038 Uiso 1 1 calc R . .
C5 C 0.37882(19) 0.7171(2) -0.03007(10) 0.0304(5) Uani 1 1 d . . .
H5 H 0.4541 0.7079 -0.0111 0.037 Uiso 1 1 calc R . .
C6 C 0.36894(19) 0.6197(2) -0.08097(10) 0.0325(5) Uani 1 1 d . . .
H6 H 0.3565 0.5331 -0.0706 0.039 Uiso 1 1 calc R . .
C7 C 0.37710(19) 0.6507(2) -0.14008(10) 0.0326(5) Uani 1 1 d . . .
H7 H 0.3740 0.5844 -0.1700 0.039 Uiso 1 1 calc R . .
C8 C 0.4409(2) 0.7097(2) -0.26575(11) 0.0357(5) Uani 1 1 d . . .
C9 C 0.5223(2) 0.6202(2) -0.25298(12) 0.0415(6) Uani 1 1 d . . .
H9 H 0.5626 0.6225 -0.2143 0.050 Uiso 1 1 calc R . .
C10 C 0.5454(2) 0.5274(3) -0.29607(13) 0.0470(7) Uani 1 1 d . . .
H10 H 0.6021 0.4679 -0.2871 0.056 Uiso 1 1 calc R . .
C11 C 0.4858(3) 0.5220(3) -0.35194(12) 0.0488(7) Uani 1 1 d . . .
H11 H 0.4997 0.4567 -0.3808 0.059 Uiso 1 1 calc R . .
C12 C 0.4064(3) 0.6107(3) -0.36588(12) 0.0492(7) Uani 1 1 d . . .
H12 H 0.3658 0.6070 -0.4045 0.059 Uiso 1 1 calc R . .
C13 C 0.3854(2) 0.7059(3) -0.32372(11) 0.0437(6) Uani 1 1 d . . .
H13 H 0.3326 0.7691 -0.3344 0.052 Uiso 1 1 calc R . .
C14 C 0.4261(2) 0.9436(2) -0.24292(10) 0.0350(5) Uani 1 1 d . . .
C15 C 0.5200(2) 0.9794(3) -0.27062(12) 0.0483(7) Uani 1 1 d . . .
H15 H 0.5758 0.9185 -0.2751 0.058 Uiso 1 1 calc R . .
C16 C 0.5328(3) 1.1027(3) -0.29170(13) 0.0596(9) Uani 1 1 d . . .
H16 H 0.5974 1.1262 -0.3103 0.072 Uiso 1 1 calc R . .
C17 C 0.4526(3) 1.1910(3) -0.28582(13) 0.0582(9) Uani 1 1 d . . .
H17 H 0.4619 1.2757 -0.3001 0.070 Uiso 1 1 calc R . .
C18 C 0.3596(3) 1.1581(3) -0.25964(13) 0.0533(8) Uani 1 1 d . . .
H18 H 0.3043 1.2198 -0.2559 0.064 Uiso 1 1 calc R . .
C19 C 0.3450(2) 1.0344(2) -0.23836(12) 0.0420(6) Uani 1 1 d . . .
H19 H 0.2794 1.0118 -0.2206 0.050 Uiso 1 1 calc R . .
C20 C 0.14599(19) 0.7201(2) 0.01375(11) 0.0339(5) Uani 1 1 d . . .
C21 C 0.1203(2) 0.6768(3) -0.05371(12) 0.0481(7) Uani 1 1 d . . .
H21A H 0.0431 0.6890 -0.0648 0.072 Uiso 1 1 calc R . .
H21B H 0.1387 0.5863 -0.0577 0.072 Uiso 1 1 calc R . .
H21C H 0.1629 0.7275 -0.0814 0.072 Uiso 1 1 calc R . .
C22 C 0.1255(2) 0.8636(3) 0.01969(13) 0.0462(7) Uani 1 1 d . . .
H22A H 0.1712 0.9102 -0.0079 0.069 Uiso 1 1 calc R . .
H22B H 0.1429 0.8904 0.0625 0.069 Uiso 1 1 calc R . .
H22C H 0.0492 0.8819 0.0084 0.069 Uiso 1 1 calc R . .
C23 C 0.0764(2) 0.6423(3) 0.05677(14) 0.0473(7) Uani 1 1 d . . .
H23A H 0.0877 0.6743 0.0991 0.071 Uiso 1 1 calc R . .
H23B H 0.0973 0.5522 0.0555 0.071 Uiso 1 1 calc R . .
H23C H -0.0001 0.6509 0.0430 0.071 Uiso 1 1 calc R . .
C24 C 0.35520(19) 0.7313(2) 0.10680(10) 0.0328(5) Uani 1 1 d . . .
C25 C 0.3928(3) 0.8702(3) 0.10421(13) 0.0505(7) Uani 1 1 d . . .
H25A H 0.3304 0.9256 0.0946 0.076 Uiso 1 1 calc R . .
H25B H 0.4446 0.8793 0.0721 0.076 Uiso 1 1 calc R . .
H25C H 0.4277 0.8945 0.1443 0.076 Uiso 1 1 calc R . .
C26 C 0.4538(2) 0.6429(3) 0.11863(12) 0.0471(7) Uani 1 1 d . . .
H26A H 0.4911 0.6644 0.1585 0.071 Uiso 1 1 calc R . .
H26B H 0.5036 0.6541 0.0856 0.071 Uiso 1 1 calc R . .
H26C H 0.4295 0.5540 0.1193 0.071 Uiso 1 1 calc R . .
C27 C 0.2795(2) 0.7123(3) 0.15947(11) 0.0451(6) Uani 1 1 d . . .
H27A H 0.3186 0.7315 0.1991 0.068 Uiso 1 1 calc R . .
H27B H 0.2543 0.6237 0.1596 0.068 Uiso 1 1 calc R . .
H27C H 0.2172 0.7696 0.1535 0.068 Uiso 1 1 calc R . .
C28 C 0.7712(3) 1.2556(3) -0.40561(17) 0.0575(8) Uani 1 1 d . . .
O1 O 0.8029(2) 1.3575(2) -0.50944(12) 0.0846(8) Uani 1 1 d . . .
O2 O 0.6850(2) 1.1709(3) -0.50682(14) 0.0906(9) Uani 1 1 d . . .
O3 O 0.87537(15) 1.14705(19) -0.48791(10) 0.0526(5) Uani 1 1 d . . .
F F 0.85760(18) 1.31286(19) -0.37798(9) 0.0762(6) Uani 1 1 d . . .
F1 F 0.75929(19) 1.14400(19) -0.37640(10) 0.0841(7) Uani 1 1 d . . .
F2 F 0.6876(2) 1.3276(2) -0.39328(14) 0.1093(9) Uani 1 1 d . . .
P1 P 0.28930(5) 0.67903(6) 0.03181(3) 0.02658(14) Uani 1 1 d . . .
S1 S 0.78419(6) 1.23211(7) -0.48738(4) 0.0477(2) 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
C1 C2 1.364(3) . ?
C1 C14 1.490(3) . ?
C1 C8 1.493(3) . ?
C2 C7 1.466(3) . ?
C2 C3 1.467(3) . ?
C3 C4 1.329(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.506(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.503(3) . ?
C5 P1 1.837(2) . ?
C5 H5 1.0000 . ?
C6 C7 1.332(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.392(4) . ?
C8 C13 1.396(3) . ?
C9 C10 1.391(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.391(4) . ?
C14 C15 1.393(4) . ?
C15 C16 1.384(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.369(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.360(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.532(4) . ?
C20 C23 1.542(4) . ?
C20 C21 1.546(3) . ?
C20 P1 1.845(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.530(4) . ?
C24 C27 1.535(3) . ?
C24 C26 1.543(3) . ?
C24 P1 1.857(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 F2 1.322(3) . ?
C28 F 1.336(4) . ?
C28 F1 1.343(3) . ?
C28 S1 1.807(4) . ?
O1 S1 1.422(2) . ?
O2 S1 1.426(2) . ?
O3 S1 1.440(2) . ?
P1 H1 1.27(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 122.8(2) . . ?
C2 C1 C8 122.5(2) . . ?
C14 C1 C8 114.61(19) . . ?
C1 C2 C7 122.2(2) . . ?
C1 C2 C3 123.4(2) . . ?
C7 C2 C3 114.43(19) . . ?
C4 C3 C2 123.4(2) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 122.1(2) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C6 C5 C4 112.55(19) . . ?
C6 C5 P1 111.32(16) . . ?
C4 C5 P1 115.39(16) . . ?
C6 C5 H5 105.5 . . ?
C4 C5 H5 105.5 . . ?
P1 C5 H5 105.5 . . ?
C7 C6 C5 122.2(2) . . ?
C7 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
C6 C7 C2 123.2(2) . . ?
C6 C7 H7 118.4 . . ?
C2 C7 H7 118.4 . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C1 121.7(2) . . ?
C13 C8 C1 120.2(2) . . ?
C10 C9 C8 121.0(2) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 120.8(3) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
C19 C14 C15 118.2(2) . . ?
C19 C14 C1 122.5(2) . . ?
C15 C14 C1 119.3(2) . . ?
C16 C15 C14 120.7(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C14 C19 C18 120.3(3) . . ?
C14 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C22 C20 C23 111.5(2) . . ?
C22 C20 C21 110.0(2) . . ?
C23 C20 C21 109.1(2) . . ?
C22 C20 P1 111.93(18) . . ?
C23 C20 P1 108.35(16) . . ?
C21 C20 P1 105.74(17) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C27 110.6(2) . . ?
C25 C24 C26 109.7(2) . . ?
C27 C24 C26 108.2(2) . . ?
C25 C24 P1 111.54(17) . . ?
C27 C24 P1 110.97(17) . . ?
C26 C24 P1 105.61(16) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
F2 C28 F 105.6(3) . . ?
F2 C28 F1 107.0(3) . . ?
F C28 F1 106.7(3) . . ?
F2 C28 S1 113.2(3) . . ?
F C28 S1 112.6(2) . . ?
F1 C28 S1 111.3(2) . . ?
C5 P1 C20 114.25(11) . . ?
C5 P1 C24 108.85(11) . . ?
C20 P1 C24 118.83(11) . . ?
C5 P1 H1 105.3(11) . . ?
C20 P1 H1 103.1(11) . . ?
C24 P1 H1 105.0(11) . . ?
O1 S1 O2 118.13(16) . . ?
O1 S1 O3 115.17(16) . . ?
O2 S1 O3 112.37(15) . . ?
O1 S1 C28 103.32(15) . . ?
O2 S1 C28 102.95(17) . . ?
O3 S1 C28 102.11(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C7 178.0(2) . . . . ?
C8 C1 C2 C7 -6.0(4) . . . . ?
C14 C1 C2 C3 -3.8(4) . . . . ?
C8 C1 C2 C3 172.2(2) . . . . ?
C1 C2 C3 C4 -169.1(2) . . . . ?
C7 C2 C3 C4 9.2(3) . . . . ?
C2 C3 C4 C5 2.1(4) . . . . ?
C3 C4 C5 C6 -13.3(3) . . . . ?
C3 C4 C5 P1 -142.5(2) . . . . ?
C4 C5 C6 C7 13.9(3) . . . . ?
P1 C5 C6 C7 145.2(2) . . . . ?
C5 C6 C7 C2 -3.3(4) . . . . ?
C1 C2 C7 C6 169.7(2) . . . . ?
C3 C2 C7 C6 -8.6(3) . . . . ?
C2 C1 C8 C9 -55.1(3) . . . . ?
C14 C1 C8 C9 121.2(3) . . . . ?
C2 C1 C8 C13 127.1(3) . . . . ?
C14 C1 C8 C13 -56.6(3) . . . . ?
C13 C8 C9 C10 -1.8(4) . . . . ?
C1 C8 C9 C10 -179.7(2) . . . . ?
C8 C9 C10 C11 -1.2(4) . . . . ?
C9 C10 C11 C12 2.3(4) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C11 C12 C13 C8 -2.8(4) . . . . ?
C9 C8 C13 C12 3.8(4) . . . . ?
C1 C8 C13 C12 -178.3(2) . . . . ?
C2 C1 C14 C19 -54.1(3) . . . . ?
C8 C1 C14 C19 129.7(2) . . . . ?
C2 C1 C14 C15 126.8(3) . . . . ?
C8 C1 C14 C15 -49.5(3) . . . . ?
C19 C14 C15 C16 1.4(4) . . . . ?
C1 C14 C15 C16 -179.4(2) . . . . ?
C14 C15 C16 C17 -0.4(4) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C15 C14 C19 C18 -1.6(4) . . . . ?
C1 C14 C19 C18 179.2(2) . . . . ?
C17 C18 C19 C14 0.9(4) . . . . ?
C6 C5 P1 C20 -77.74(19) . . . . ?
C4 C5 P1 C20 52.1(2) . . . . ?
C6 C5 P1 C24 146.81(16) . . . . ?
C4 C5 P1 C24 -83.32(19) . . . . ?
C22 C20 P1 C5 -76.7(2) . . . . ?
C23 C20 P1 C5 159.94(17) . . . . ?
C21 C20 P1 C5 43.1(2) . . . . ?
C22 C20 P1 C24 54.0(2) . . . . ?
C23 C20 P1 C24 -69.3(2) . . . . ?
C21 C20 P1 C24 173.83(17) . . . . ?
C25 C24 P1 C5 51.2(2) . . . . ?
C27 C24 P1 C5 175.07(17) . . . . ?
C26 C24 P1 C5 -67.92(19) . . . . ?
C25 C24 P1 C20 -81.9(2) . . . . ?
C27 C24 P1 C20 42.0(2) . . . . ?
C26 C24 P1 C20 158.98(17) . . . . ?
F2 C28 S1 O1 63.1(3) . . . . ?
F C28 S1 O1 -56.6(3) . . . . ?
F1 C28 S1 O1 -176.4(2) . . . . ?
F2 C28 S1 O2 -60.3(3) . . . . ?
F C28 S1 O2 180.0(2) . . . . ?
F1 C28 S1 O2 60.2(3) . . . . ?
F2 C28 S1 O3 -177.0(2) . . . . ?
F C28 S1 O3 63.3(2) . . . . ?
F1 C28 S1 O3 -56.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 991776'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[tBu2PH(C6H4)CHPh2][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H34 P, C F3 O3 S, C6 H4 F2'
_chemical_formula_sum            'C34 H38 F5 O3 P S'
_chemical_formula_weight         652.67

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.2485(2)
_cell_length_b                   9.5183(2)
_cell_length_c                   22.0780(6)
_cell_angle_alpha                88.3720(10)
_cell_angle_beta                 86.0270(10)
_cell_angle_gamma                73.0880(10)
_cell_volume                     1654.37(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9237
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_process_details   
;  
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.8662
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'HELIOS multilayer optics, Montel mirror'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25181
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         0.92
_diffrn_reflns_theta_max         27.87
_reflns_number_total             7868
_reflns_number_gt                6321
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 Software Suit (v2012.2-0)'
_computing_cell_refinement       'APEX2 Software Suit (v2012.2-0)'
_computing_data_reduction        'APEX2 Software Suit (v2012.2-0)'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0880P)²+1.0340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7868
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1594
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0528(3) 0.7960(2) 0.35803(9) 0.0364(4) Uani 1 1 d . . .
H1 H -0.1202 0.9013 0.3634 0.044 Uiso 1 1 calc R . .
C2 C 0.0661(3) 0.7898(2) 0.30178(9) 0.0329(4) Uani 1 1 d . . .
C3 C 0.2037(3) 0.6666(2) 0.28896(9) 0.0385(5) Uani 1 1 d . . .
H3 H 0.2232 0.5844 0.3158 0.046 Uiso 1 1 calc R . .
C4 C 0.3123(3) 0.6617(2) 0.23806(9) 0.0350(4) Uani 1 1 d . . .
H4 H 0.4050 0.5765 0.2299 0.042 Uiso 1 1 calc R . .
C5 C 0.2852(2) 0.7828(2) 0.19857(8) 0.0298(4) Uani 1 1 d . . .
C6 C 0.1470(2) 0.9064(2) 0.21074(9) 0.0324(4) Uani 1 1 d . . .
H6 H 0.1270 0.9886 0.1839 0.039 Uiso 1 1 calc R . .
C7 C 0.0394(2) 0.9091(2) 0.26169(9) 0.0319(4) Uani 1 1 d . . .
H7 H -0.0543 0.9936 0.2696 0.038 Uiso 1 1 calc R . .
C8 C -0.1799(3) 0.7097(3) 0.35251(9) 0.0384(5) Uani 1 1 d . . .
C9 C -0.1543(3) 0.5916(3) 0.31383(10) 0.0440(5) Uani 1 1 d . . .
H9 H -0.0557 0.5658 0.2868 0.053 Uiso 1 1 calc R . .
C10 C -0.2692(3) 0.5106(3) 0.31376(12) 0.0530(6) Uani 1 1 d . . .
H10 H -0.2484 0.4291 0.2875 0.064 Uiso 1 1 calc R . .
C11 C -0.4134(3) 0.5491(4) 0.35200(14) 0.0609(7) Uani 1 1 d . . .
H11 H -0.4921 0.4933 0.3526 0.073 Uiso 1 1 calc R . .
C12 C -0.4440(3) 0.6680(4) 0.38931(14) 0.0641(8) Uani 1 1 d . . .
H12 H -0.5453 0.6954 0.4149 0.077 Uiso 1 1 calc R . .
C13 C -0.3286(3) 0.7485(3) 0.38999(11) 0.0512(6) Uani 1 1 d . . .
H13 H -0.3511 0.8305 0.4161 0.061 Uiso 1 1 calc R . .
C14 C 0.0478(3) 0.7510(2) 0.41440(9) 0.0377(5) Uani 1 1 d . . .
C15 C 0.0948(3) 0.6081(3) 0.43646(10) 0.0439(5) Uani 1 1 d . . .
H15 H 0.0617 0.5344 0.4168 0.053 Uiso 1 1 calc R . .
C16 C 0.1901(3) 0.5717(3) 0.48718(11) 0.0517(6) Uani 1 1 d . . .
H16 H 0.2230 0.4731 0.5016 0.062 Uiso 1 1 calc R . .
C17 C 0.2372(3) 0.6781(3) 0.51666(11) 0.0550(7) Uani 1 1 d . . .
H17 H 0.3016 0.6533 0.5515 0.066 Uiso 1 1 calc R . .
C18 C 0.1901(4) 0.8203(3) 0.49522(12) 0.0599(7) Uani 1 1 d . . .
H18 H 0.2218 0.8942 0.5154 0.072 Uiso 1 1 calc R . .
C19 C 0.0970(3) 0.8562(3) 0.44458(11) 0.0502(6) Uani 1 1 d . . .
H19 H 0.0659 0.9547 0.4301 0.060 Uiso 1 1 calc R . .
C20 C 0.5571(3) 0.9044(2) 0.14339(11) 0.0405(5) Uani 1 1 d . . .
C21 C 0.6167(5) 0.8821(4) 0.20797(16) 0.0784(11) Uani 1 1 d . . .
H21A H 0.6862 0.7803 0.2132 0.118 Uiso 1 1 calc R . .
H21B H 0.5178 0.9030 0.2372 0.118 Uiso 1 1 calc R . .
H21C H 0.6843 0.9487 0.2149 0.118 Uiso 1 1 calc R . .
C22 C 0.7096(4) 0.8695(4) 0.0972(2) 0.0889(13) Uani 1 1 d . . .
H22A H 0.7773 0.7671 0.1022 0.133 Uiso 1 1 calc R . .
H22B H 0.7796 0.9345 0.1036 0.133 Uiso 1 1 calc R . .
H22C H 0.6698 0.8847 0.0560 0.133 Uiso 1 1 calc R . .
C23 C 0.4498(3) 1.0632(3) 0.13625(14) 0.0525(6) Uani 1 1 d . . .
H23A H 0.3523 1.0839 0.1660 0.079 Uiso 1 1 calc R . .
H23B H 0.4095 1.0789 0.0952 0.079 Uiso 1 1 calc R . .
H23C H 0.5187 1.1290 0.1430 0.079 Uiso 1 1 calc R . .
C24 C 0.3376(3) 0.7629(3) 0.06382(9) 0.0392(5) Uani 1 1 d . . .
C25 C 0.4765(4) 0.7200(4) 0.01260(12) 0.0716(9) Uani 1 1 d . . .
H25A H 0.5608 0.6282 0.0234 0.107 Uiso 1 1 calc R . .
H25B H 0.5318 0.7980 0.0064 0.107 Uiso 1 1 calc R . .
H25C H 0.4261 0.7063 -0.0249 0.107 Uiso 1 1 calc R . .
C26 C 0.2038(4) 0.9052(4) 0.04898(14) 0.0706(9) Uani 1 1 d . . .
H26A H 0.2579 0.9838 0.0420 0.106 Uiso 1 1 calc R . .
H26B H 0.1183 0.9314 0.0830 0.106 Uiso 1 1 calc R . .
H26C H 0.1492 0.8921 0.0124 0.106 Uiso 1 1 calc R . .
C27 C 0.2533(5) 0.6406(4) 0.07382(14) 0.0715(9) Uani 1 1 d . . .
H27A H 0.3391 0.5486 0.0832 0.107 Uiso 1 1 calc R . .
H27B H 0.1993 0.6284 0.0369 0.107 Uiso 1 1 calc R . .
H27C H 0.1671 0.6661 0.1077 0.107 Uiso 1 1 calc R . .
C28 C 0.9519(4) 0.4016(3) 0.12100(15) 0.0587(7) Uani 1 1 d . . .
C29 C -0.3816(4) 0.8277(3) 0.59635(19) 0.0722(9) Uani 1 1 d . . .
C30 C -0.4803(4) 0.8138(3) 0.64715(15) 0.0636(8) Uani 1 1 d . . .
C31 C -0.4144(7) 0.7705(4) 0.7025(2) 0.1052(16) Uani 1 1 d . . .
H31 H -0.4827 0.7571 0.7374 0.126 Uiso 1 1 calc R . .
C32 C -0.2281(9) 0.7462(4) 0.7035(3) 0.127(2) Uani 1 1 d . . .
H32 H -0.1705 0.7198 0.7398 0.152 Uiso 1 1 calc R . .
C33 C -0.1432(7) 0.7640(5) 0.6490(3) 0.116(2) Uani 1 1 d . . .
H33 H -0.0244 0.7498 0.6493 0.139 Uiso 1 1 calc R . .
C34 C -0.2133(5) 0.7992(4) 0.5962(3) 0.0967(14) Uani 1 1 d . . .
H34 H -0.1463 0.8039 0.5598 0.116 Uiso 1 1 calc R . .
F4 F -0.4584(4) 0.8687(3) 0.54455(11) 0.1062(8) Uani 1 1 d . . .
F5 F -0.6482(3) 0.8423(3) 0.64106(11) 0.0919(6) Uani 1 1 d . . .
O1 O 0.8772(4) 0.2364(2) 0.20332(11) 0.0858(8) Uani 1 1 d . . .
O2 O 0.8467(3) 0.1812(2) 0.10104(11) 0.0721(6) Uani 1 1 d . . .
O3 O 0.6505(3) 0.3938(2) 0.14860(13) 0.0775(7) Uani 1 1 d . . .
F1 F 1.1109(2) 0.3247(2) 0.11339(15) 0.1134(9) Uani 1 1 d . . .
F2 F 0.9416(3) 0.5081(2) 0.16025(10) 0.0861(6) Uani 1 1 d . . .
F3 F 0.9087(3) 0.4704(2) 0.06838(9) 0.0836(6) Uani 1 1 d . . .
P1 P 0.43502(6) 0.77231(5) 0.13545(2) 0.02956(14) Uani 1 1 d . . .
S1 S 0.81390(8) 0.29202(6) 0.14554(3) 0.04572(17) Uani 1 1 d . . .
H1A H 0.547(3) 0.649(2) 0.1414(10) 0.031(6) Uiso 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
C1 C2 1.520(3) . ?
C1 C8 1.521(3) . ?
C1 C14 1.525(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.394(3) . ?
C2 C7 1.395(3) . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(3) . ?
C5 P1 1.7825(19) . ?
C6 C7 1.379(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.389(3) . ?
C8 C13 1.393(3) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.374(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.385(3) . ?
C14 C19 1.386(3) . ?
C15 C16 1.390(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C23 1.523(3) . ?
C20 C22 1.527(4) . ?
C20 C21 1.529(4) . ?
C20 P1 1.843(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.522(3) . ?
C24 C27 1.524(4) . ?
C24 C25 1.527(3) . ?
C24 P1 1.839(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 F1 1.305(3) . ?
C28 F2 1.333(3) . ?
C28 F3 1.336(4) . ?
C28 S1 1.803(3) . ?
C29 C34 1.335(5) . ?
C29 F4 1.339(4) . ?
C29 C30 1.366(5) . ?
C30 F5 1.348(4) . ?
C30 C31 1.375(5) . ?
C31 C32 1.488(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.329(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
O1 S1 1.440(2) . ?
O2 S1 1.417(2) . ?
O3 S1 1.411(2) . ?
P1 H1A 1.27(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
C2 C1 C8 113.81(17) . . ?
C2 C1 C14 110.61(17) . . ?
C8 C1 C14 111.83(17) . . ?
C2 C1 H1 106.7 . . ?
C8 C1 H1 106.7 . . ?
C14 C1 H1 106.7 . . ?
C3 C2 C7 118.43(18) . . ?
C3 C2 C1 121.46(17) . . ?
C7 C2 C1 120.11(17) . . ?
C4 C3 C2 121.34(18) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.64(18) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 119.50(17) . . ?
C6 C5 P1 123.08(14) . . ?
C4 C5 P1 117.39(15) . . ?
C7 C6 C5 120.04(17) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 121.04(18) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C9 C8 C13 118.0(2) . . ?
C9 C8 C1 124.07(19) . . ?
C13 C8 C1 117.9(2) . . ?
C10 C9 C8 121.5(2) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C11 C10 C9 119.5(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 120.3(3) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C15 C14 C19 118.2(2) . . ?
C15 C14 C1 122.7(2) . . ?
C19 C14 C1 119.1(2) . . ?
C14 C15 C16 120.6(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 119.4(2) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 120.3(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 121.2(3) . . ?
C18 C19 H19 119.4 . . ?
C14 C19 H19 119.4 . . ?
C23 C20 C22 110.3(2) . . ?
C23 C20 C21 108.5(2) . . ?
C22 C20 C21 110.3(3) . . ?
C23 C20 P1 112.65(16) . . ?
C22 C20 P1 109.51(18) . . ?
C21 C20 P1 105.46(17) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C27 109.2(2) . . ?
C26 C24 C25 111.3(2) . . ?
C27 C24 C25 109.3(2) . . ?
C26 C24 P1 112.57(17) . . ?
C27 C24 P1 104.89(17) . . ?
C25 C24 P1 109.31(17) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
F1 C28 F2 108.0(3) . . ?
F1 C28 F3 106.9(3) . . ?
F2 C28 F3 105.1(2) . . ?
F1 C28 S1 113.1(2) . . ?
F2 C28 S1 111.5(2) . . ?
F3 C28 S1 111.8(2) . . ?
C34 C29 F4 119.3(4) . . ?
C34 C29 C30 122.8(4) . . ?
F4 C29 C30 117.9(3) . . ?
F5 C30 C29 117.1(3) . . ?
F5 C30 C31 120.2(4) . . ?
C29 C30 C31 122.7(4) . . ?
C30 C31 C32 114.9(5) . . ?
C30 C31 H31 122.6 . . ?
C32 C31 H31 122.6 . . ?
C33 C32 C31 116.6(4) . . ?
C33 C32 H32 121.7 . . ?
C31 C32 H32 121.7 . . ?
C34 C33 C32 125.6(5) . . ?
C34 C33 H33 117.2 . . ?
C32 C33 H33 117.2 . . ?
C33 C34 C29 117.2(5) . . ?
C33 C34 H34 121.4 . . ?
C29 C34 H34 121.4 . . ?
C5 P1 C24 110.74(9) . . ?
C5 P1 C20 110.78(10) . . ?
C24 P1 C20 120.03(11) . . ?
C5 P1 H1A 105.1(10) . . ?
C24 P1 H1A 106.0(10) . . ?
C20 P1 H1A 102.7(10) . . ?
O3 S1 O2 116.72(15) . . ?
O3 S1 O1 115.00(17) . . ?
O2 S1 O1 112.78(15) . . ?
O3 S1 C28 103.78(13) . . ?
O2 S1 C28 104.23(14) . . ?
O1 S1 C28 101.99(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C1 C2 C3 -77.4(3) . . . . ?
C14 C1 C2 C3 49.5(3) . . . . ?
C8 C1 C2 C7 102.9(2) . . . . ?
C14 C1 C2 C7 -130.2(2) . . . . ?
C7 C2 C3 C4 0.2(3) . . . . ?
C1 C2 C3 C4 -179.5(2) . . . . ?
C2 C3 C4 C5 0.5(3) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C3 C4 C5 P1 177.42(17) . . . . ?
C4 C5 C6 C7 0.7(3) . . . . ?
P1 C5 C6 C7 -177.57(15) . . . . ?
C5 C6 C7 C2 0.0(3) . . . . ?
C3 C2 C7 C6 -0.5(3) . . . . ?
C1 C2 C7 C6 179.26(19) . . . . ?
C2 C1 C8 C9 24.8(3) . . . . ?
C14 C1 C8 C9 -101.4(2) . . . . ?
C2 C1 C8 C13 -157.4(2) . . . . ?
C14 C1 C8 C13 76.4(2) . . . . ?
C13 C8 C9 C10 -2.4(3) . . . . ?
C1 C8 C9 C10 175.4(2) . . . . ?
C8 C9 C10 C11 1.1(4) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -1.5(4) . . . . ?
C11 C12 C13 C8 0.2(4) . . . . ?
C9 C8 C13 C12 1.7(4) . . . . ?
C1 C8 C13 C12 -176.2(2) . . . . ?
C2 C1 C14 C15 -93.2(2) . . . . ?
C8 C1 C14 C15 34.8(3) . . . . ?
C2 C1 C14 C19 85.9(2) . . . . ?
C8 C1 C14 C19 -146.1(2) . . . . ?
C19 C14 C15 C16 -0.6(3) . . . . ?
C1 C14 C15 C16 178.4(2) . . . . ?
C14 C15 C16 C17 0.9(4) . . . . ?
C15 C16 C17 C18 -0.5(4) . . . . ?
C16 C17 C18 C19 -0.2(4) . . . . ?
C17 C18 C19 C14 0.4(4) . . . . ?
C15 C14 C19 C18 0.0(4) . . . . ?
C1 C14 C19 C18 -179.1(2) . . . . ?
C34 C29 C30 F5 -178.3(3) . . . . ?
F4 C29 C30 F5 0.2(4) . . . . ?
C34 C29 C30 C31 0.6(5) . . . . ?
F4 C29 C30 C31 179.1(3) . . . . ?
F5 C30 C31 C32 -178.5(3) . . . . ?
C29 C30 C31 C32 2.6(5) . . . . ?
C30 C31 C32 C33 -2.5(5) . . . . ?
C31 C32 C33 C34 -0.7(7) . . . . ?
C32 C33 C34 C29 3.9(6) . . . . ?
F4 C29 C34 C33 177.6(3) . . . . ?
C30 C29 C34 C33 -3.9(5) . . . . ?
C6 C5 P1 C24 -69.9(2) . . . . ?
C4 C5 P1 C24 111.86(17) . . . . ?
C6 C5 P1 C20 65.87(19) . . . . ?
C4 C5 P1 C20 -112.40(17) . . . . ?
C26 C24 P1 C5 68.3(2) . . . . ?
C27 C24 P1 C5 -50.4(2) . . . . ?
C25 C24 P1 C5 -167.51(19) . . . . ?
C26 C24 P1 C20 -62.8(2) . . . . ?
C27 C24 P1 C20 178.55(18) . . . . ?
C25 C24 P1 C20 61.4(2) . . . . ?
C23 C20 P1 C5 -69.7(2) . . . . ?
C22 C20 P1 C5 167.1(2) . . . . ?
C21 C20 P1 C5 48.5(2) . . . . ?
C23 C20 P1 C24 61.4(2) . . . . ?
C22 C20 P1 C24 -61.8(3) . . . . ?
C21 C20 P1 C24 179.6(2) . . . . ?
F1 C28 S1 O3 -177.8(3) . . . . ?
F2 C28 S1 O3 60.2(2) . . . . ?
F3 C28 S1 O3 -57.1(3) . . . . ?
F1 C28 S1 O2 -55.1(3) . . . . ?
F2 C28 S1 O2 -177.1(2) . . . . ?
F3 C28 S1 O2 65.5(2) . . . . ?
F1 C28 S1 O1 62.4(3) . . . . ?
F2 C28 S1 O1 -59.6(2) . . . . ?
F3 C28 S1 O1 -176.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 991777'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[tBu2PH-Et2O][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H28 O P, C F3 O3 S'
_chemical_formula_sum            'C13 H28 F3 O4 P S'
_chemical_formula_weight         368.38

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'
F F 0.0727 0.0534 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.0615(3)
_cell_length_b                   15.5070(5)
_cell_length_c                   13.5090(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.580(2)
_cell_angle_gamma                90.00
_cell_volume                     1898.14(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      75

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    2.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3197
_exptl_absorpt_correction_T_max  0.6732
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.492374

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10730
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.34
_diffrn_reflns_theta_max         68.21
_reflns_number_total             3374
_reflns_number_gt                3009
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0659P)²+0.3161P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3374
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.1040
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1525(2) 0.19869(12) 0.28650(12) 0.0330(4) Uani 1 1 d . . .
C2 C 0.2763(2) 0.26552(13) 0.28876(16) 0.0458(5) Uani 1 1 d . . .
H2A H 0.2571 0.3079 0.3409 0.069 Uiso 1 1 calc R . .
H2B H 0.2806 0.2949 0.2246 0.069 Uiso 1 1 calc R . .
H2C H 0.3706 0.2367 0.3022 0.069 Uiso 1 1 calc R . .
C3 C 0.1480(3) 0.14645(15) 0.38319(14) 0.0510(5) Uani 1 1 d . . .
H3A H 0.2444 0.1196 0.3952 0.077 Uiso 1 1 calc R . .
H3B H 0.0722 0.1016 0.3776 0.077 Uiso 1 1 calc R . .
H3C H 0.1245 0.1849 0.4384 0.077 Uiso 1 1 calc R . .
C4 C 0.0029(2) 0.24353(13) 0.27276(14) 0.0414(4) Uani 1 1 d . . .
H4A H -0.0158 0.2810 0.3297 0.062 Uiso 1 1 calc R . .
H4B H -0.0752 0.2000 0.2676 0.062 Uiso 1 1 calc R . .
H4C H 0.0041 0.2783 0.2122 0.062 Uiso 1 1 calc R . .
C5 C 0.35473(18) 0.07190(11) 0.16520(13) 0.0315(4) Uani 1 1 d . . .
C6 C 0.4127(2) 0.03696(17) 0.26424(17) 0.0537(6) Uani 1 1 d . . .
H6A H 0.5014 0.0023 0.2530 0.081 Uiso 1 1 calc R . .
H6B H 0.3368 0.0010 0.2948 0.081 Uiso 1 1 calc R . .
H6C H 0.4371 0.0852 0.3083 0.081 Uiso 1 1 calc R . .
C7 C 0.4638(2) 0.13405(14) 0.11766(19) 0.0500(5) Uani 1 1 d . . .
H7A H 0.4799 0.1836 0.1615 0.075 Uiso 1 1 calc R . .
H7B H 0.4237 0.1541 0.0540 0.075 Uiso 1 1 calc R . .
H7C H 0.5578 0.1044 0.1069 0.075 Uiso 1 1 calc R . .
C8 C 0.3270(2) -0.00444(12) 0.09509(15) 0.0390(4) Uani 1 1 d . . .
H8A H 0.2958 0.0172 0.0300 0.058 Uiso 1 1 calc R . .
H8B H 0.2495 -0.0413 0.1222 0.058 Uiso 1 1 calc R . .
H8C H 0.4181 -0.0379 0.0883 0.058 Uiso 1 1 calc R . .
C9 C 0.11024(19) 0.16812(11) 0.06358(12) 0.0304(4) Uani 1 1 d . . .
H9 H 0.1642 0.1379 0.0094 0.037 Uiso 1 1 calc R . .
C10 C -0.0542(2) 0.15627(14) 0.04515(15) 0.0428(5) Uani 1 1 d . . .
H10A H -0.1095 0.1875 0.0958 0.064 Uiso 1 1 calc R . .
H10B H -0.0788 0.0948 0.0482 0.064 Uiso 1 1 calc R . .
H10C H -0.0804 0.1789 -0.0204 0.064 Uiso 1 1 calc R . .
C13 C 0.6785(2) 0.38680(14) 0.17799(16) 0.0467(5) Uani 1 1 d . . .
C11 C 0.1752(3) 0.29124(15) -0.03210(15) 0.0515(5) Uani 1 1 d . . .
H11A H 0.0826 0.2853 -0.0711 0.062 Uiso 1 1 calc R . .
H11B H 0.2544 0.2601 -0.0672 0.062 Uiso 1 1 calc R . .
C12 C 0.2145(3) 0.38360(16) -0.02175(19) 0.0630(7) Uani 1 1 d . . .
H12A H 0.1348 0.4142 0.0120 0.094 Uiso 1 1 calc R . .
H12B H 0.2288 0.4088 -0.0875 0.094 Uiso 1 1 calc R . .
H12C H 0.3060 0.3889 0.0171 0.094 Uiso 1 1 calc R . .
O1A O 0.15641(14) 0.25545(8) 0.06470(9) 0.0340(3) Uani 1 1 d . . .
O2 O 0.79737(14) 0.41446(9) 0.34791(10) 0.0412(3) Uani 1 1 d . . .
O3 O 0.53147(15) 0.42495(10) 0.33293(12) 0.0511(4) Uani 1 1 d . . .
O4 O 0.68556(15) 0.53474(8) 0.26076(11) 0.0420(3) Uani 1 1 d . . .
F1 F 0.56677(19) 0.40904(14) 0.11925(13) 0.0943(7) Uani 1 1 d . . .
F2 F 0.66921(16) 0.30259(9) 0.19435(14) 0.0774(5) Uani 1 1 d . . .
F3 F 0.80259(15) 0.40059(10) 0.12923(9) 0.0593(4) Uani 1 1 d . . .
P1 P 0.17354(4) 0.12266(2) 0.18267(3) 0.02348(14) Uani 1 1 d . . .
S1 S 0.67268(4) 0.44694(3) 0.29296(3) 0.02936(14) Uani 1 1 d . . .
H1 H 0.087(2) 0.0607(12) 0.1982(14) 0.029(5) Uiso 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
C1 C2 1.528(3) . ?
C1 C4 1.533(2) . ?
C1 C3 1.538(3) . ?
C1 P1 1.8438(17) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C7 1.527(3) . ?
C5 C6 1.531(3) . ?
C5 C8 1.535(2) . ?
C5 P1 1.8382(17) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O1A 1.417(2) . ?
C9 C10 1.519(2) . ?
C9 P1 1.8428(17) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C13 F1 1.326(2) . ?
C13 F3 1.326(3) . ?
C13 F2 1.327(3) . ?
C13 S1 1.813(2) . ?
C11 O1A 1.432(2) . ?
C11 C12 1.482(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O2 S1 1.4368(13) . ?
O3 S1 1.4349(14) . ?
O4 S1 1.4344(13) . ?
P1 H1 1.262(19) . ?

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
C2 C1 C4 110.07(16) . . ?
C2 C1 C3 111.47(17) . . ?
C4 C1 C3 108.12(16) . . ?
C2 C1 P1 111.54(13) . . ?
C4 C1 P1 107.23(12) . . ?
C3 C1 P1 108.24(13) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C5 C6 111.90(18) . . ?
C7 C5 C8 109.25(16) . . ?
C6 C5 C8 108.58(16) . . ?
C7 C5 P1 111.51(13) . . ?
C6 C5 P1 109.77(13) . . ?
C8 C5 P1 105.59(12) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1A C9 C10 113.97(15) . . ?
O1A C9 P1 105.48(11) . . ?
C10 C9 P1 113.13(13) . . ?
O1A C9 H9 108.0 . . ?
C10 C9 H9 108.0 . . ?
P1 C9 H9 108.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
F1 C13 F3 107.9(2) . . ?
F1 C13 F2 107.85(19) . . ?
F3 C13 F2 107.25(17) . . ?
F1 C13 S1 110.52(15) . . ?
F3 C13 S1 112.00(14) . . ?
F2 C13 S1 111.17(17) . . ?
O1A C11 C12 108.60(19) . . ?
O1A C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O1A C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 O1A C11 113.46(14) . . ?
C5 P1 C9 108.80(8) . . ?
C5 P1 C1 118.11(8) . . ?
C9 P1 C1 112.69(8) . . ?
C5 P1 H1 104.8(9) . . ?
C9 P1 H1 104.3(9) . . ?
C1 P1 H1 106.9(9) . . ?
O4 S1 O3 114.54(8) . . ?
O4 S1 O2 115.05(9) . . ?
O3 S1 O2 114.95(9) . . ?
O4 S1 C13 103.02(10) . . ?
O3 S1 C13 103.52(10) . . ?
O2 S1 C13 103.46(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C9 O1A C11 -80.4(2) . . . . ?
P1 C9 O1A C11 154.86(14) . . . . ?
C12 C11 O1A C9 176.65(18) . . . . ?
C7 C5 P1 C9 53.02(16) . . . . ?
C6 C5 P1 C9 177.61(14) . . . . ?
C8 C5 P1 C9 -65.53(14) . . . . ?
C7 C5 P1 C1 -77.06(16) . . . . ?
C6 C5 P1 C1 47.53(17) . . . . ?
C8 C5 P1 C1 164.39(12) . . . . ?
O1A C9 P1 C5 -93.81(12) . . . . ?
C10 C9 P1 C5 140.98(13) . . . . ?
O1A C9 P1 C1 39.18(14) . . . . ?
C10 C9 P1 C1 -86.04(15) . . . . ?
C2 C1 P1 C5 49.13(16) . . . . ?
C4 C1 P1 C5 169.71(12) . . . . ?
C3 C1 P1 C5 -73.86(16) . . . . ?
C2 C1 P1 C9 -79.14(15) . . . . ?
C4 C1 P1 C9 41.44(15) . . . . ?
C3 C1 P1 C9 157.87(13) . . . . ?
F1 C13 S1 O4 -60.92(19) . . . . ?
F3 C13 S1 O4 59.39(17) . . . . ?
F2 C13 S1 O4 179.35(13) . . . . ?
F1 C13 S1 O3 58.7(2) . . . . ?
F3 C13 S1 O3 178.99(15) . . . . ?
F2 C13 S1 O3 -61.04(15) . . . . ?
F1 C13 S1 O2 178.93(18) . . . . ?
F3 C13 S1 O2 -60.76(17) . . . . ?
F2 C13 S1 O2 59.20(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        68.21
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 991778'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[tBu2PH-benzylether][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C22 H32 O P, C F3 O3 S'
_chemical_formula_sum            'C23 H32 F3 O4 P S'
_chemical_formula_weight         492.52

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   8.9375(6)
_cell_length_b                   16.5265(9)
_cell_length_c                   16.7035(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2467.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22.5

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9235
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.9858

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'HELIOS multilayer optics, Montel mirror'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20122
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         27.88
_reflns_number_total             5874
_reflns_number_gt                5360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 Software Suit (v2012.2-0)'
_computing_cell_refinement       'APEX2 Software Suit (v2012.2-0)'
_computing_data_reduction        'APEX2 Software Suit (v2012.2-0)'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0361P)²+0.6370P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_number_reflns         5874
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0885
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1237(2) 0.30464(10) 0.80982(10) 0.0249(3) Uani 1 1 d . . .
H1 H 0.1651 0.2626 0.8468 0.030 Uiso 1 1 calc R . .
C2 C 0.2451(2) 0.22468(11) 0.71269(12) 0.0299(4) Uani 1 1 d . . .
H2A H 0.1493 0.1959 0.7040 0.036 Uiso 1 1 calc R . .
H2B H 0.3029 0.1947 0.7536 0.036 Uiso 1 1 calc R . .
C3 C -0.0374(2) 0.28241(11) 0.79373(10) 0.0256(4) Uani 1 1 d . . .
C4 C -0.1010(2) 0.29297(12) 0.71880(11) 0.0337(4) Uani 1 1 d . . .
H4 H -0.0442 0.3166 0.6768 0.040 Uiso 1 1 calc R . .
C5 C -0.2469(3) 0.26908(14) 0.70512(13) 0.0424(5) Uani 1 1 d . . .
H5 H -0.2898 0.2757 0.6535 0.051 Uiso 1 1 calc R . .
C6 C -0.3307(2) 0.23563(14) 0.76625(14) 0.0444(5) Uani 1 1 d . . .
H6 H -0.4313 0.2197 0.7567 0.053 Uiso 1 1 calc R . .
C7 C -0.2687(2) 0.22527(14) 0.84099(14) 0.0421(5) Uani 1 1 d . . .
H7 H -0.3266 0.2026 0.8831 0.051 Uiso 1 1 calc R . .
C8 C -0.1215(2) 0.24799(11) 0.85471(12) 0.0320(4) Uani 1 1 d . . .
H8 H -0.0781 0.2399 0.9060 0.038 Uiso 1 1 calc R . .
C9 C 0.3319(2) 0.22750(10) 0.63585(11) 0.0276(3) Uani 1 1 d . . .
C10 C 0.3463(3) 0.15725(12) 0.59100(12) 0.0391(5) Uani 1 1 d . . .
H10 H 0.2986 0.1090 0.6086 0.047 Uiso 1 1 calc R . .
C11 C 0.4292(3) 0.15649(15) 0.52113(13) 0.0480(6) Uani 1 1 d . . .
H11 H 0.4367 0.1083 0.4904 0.058 Uiso 1 1 calc R . .
C12 C 0.5009(3) 0.22584(16) 0.49603(13) 0.0472(6) Uani 1 1 d . . .
H12 H 0.5610 0.2249 0.4491 0.057 Uiso 1 1 calc R . .
C13 C 0.4855(3) 0.29625(14) 0.53893(12) 0.0405(5) Uani 1 1 d . . .
H13 H 0.5325 0.3444 0.5207 0.049 Uiso 1 1 calc R . .
C14 C 0.4013(2) 0.29742(12) 0.60904(11) 0.0334(4) Uani 1 1 d . . .
H14 H 0.3914 0.3463 0.6386 0.040 Uiso 1 1 calc R . .
C15 C 0.0807(3) 0.49143(12) 0.80078(13) 0.0375(5) Uani 1 1 d . . .
C16 C -0.0907(3) 0.48533(14) 0.79838(16) 0.0497(6) Uani 1 1 d . . .
H16A H -0.1300 0.4850 0.8532 0.075 Uiso 1 1 calc R . .
H16B H -0.1199 0.4352 0.7712 0.075 Uiso 1 1 calc R . .
H16C H -0.1316 0.5318 0.7693 0.075 Uiso 1 1 calc R . .
C17 C 0.1238(3) 0.56938(13) 0.84505(18) 0.0574(7) Uani 1 1 d . . .
H17A H 0.2330 0.5748 0.8458 0.086 Uiso 1 1 calc R . .
H17B H 0.0862 0.5671 0.9001 0.086 Uiso 1 1 calc R . .
H17C H 0.0798 0.6160 0.8175 0.086 Uiso 1 1 calc R . .
C18 C 0.1452(3) 0.49162(14) 0.71586(14) 0.0520(6) Uani 1 1 d . . .
H18A H 0.1062 0.5384 0.6864 0.078 Uiso 1 1 calc R . .
H18B H 0.1160 0.4417 0.6883 0.078 Uiso 1 1 calc R . .
H18C H 0.2545 0.4949 0.7185 0.078 Uiso 1 1 calc R . .
C19 C 0.3418(2) 0.40993(12) 0.90098(11) 0.0315(4) Uani 1 1 d . . .
C20 C 0.3372(3) 0.46348(15) 0.97650(13) 0.0491(6) Uani 1 1 d . . .
H20A H 0.4343 0.4613 1.0036 0.074 Uiso 1 1 calc R . .
H20B H 0.2591 0.4437 1.0127 0.074 Uiso 1 1 calc R . .
H20C H 0.3152 0.5195 0.9611 0.074 Uiso 1 1 calc R . .
C21 C 0.4554(2) 0.44123(14) 0.84033(13) 0.0409(5) Uani 1 1 d . . .
H21A H 0.5560 0.4387 0.8636 0.061 Uiso 1 1 calc R . .
H21B H 0.4316 0.4974 0.8265 0.061 Uiso 1 1 calc R . .
H21C H 0.4517 0.4077 0.7920 0.061 Uiso 1 1 calc R . .
C23 C 0.3861(2) 0.32449(13) 0.92708(13) 0.0402(5) Uani 1 1 d . . .
H23A H 0.3989 0.2902 0.8797 0.060 Uiso 1 1 calc R . .
H23B H 0.3075 0.3018 0.9613 0.060 Uiso 1 1 calc R . .
H23C H 0.4804 0.3267 0.9570 0.060 Uiso 1 1 calc R . .
C24 C 0.6089(3) 0.52237(14) 0.62115(14) 0.0508(6) Uani 1 1 d . . .
O1 O 0.21568(14) 0.30527(7) 0.74053(8) 0.0278(3) Uani 1 1 d . . .
O2 O 0.7350(3) 0.53843(13) 0.48525(12) 0.0776(7) Uani 1 1 d . . .
O3 O 0.8074(2) 0.63016(11) 0.59269(12) 0.0616(5) Uani 1 1 d . . .
O4 O 0.5630(2) 0.64211(9) 0.53074(10) 0.0512(4) Uani 1 1 d . . .
F2 F 0.7000(3) 0.46278(9) 0.64001(12) 0.0992(7) Uani 1 1 d . . .
F5 F 0.4848(2) 0.48925(10) 0.59273(11) 0.0780(5) Uani 1 1 d . . .
F6 F 0.5761(2) 0.56062(11) 0.68891(9) 0.0835(6) Uani 1 1 d . . .
P1 P 0.14959(5) 0.40389(3) 0.85933(3) 0.02651(10) Uani 1 1 d . . .
S1 S 0.68974(6) 0.59138(3) 0.54874(3) 0.03625(12) Uani 1 1 d . . .
H1A H 0.058(3) 0.3996(13) 0.9216(13) 0.042(6) Uiso 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
C1 O1 1.420(2) . ?
C1 C3 1.511(2) . ?
C1 P1 1.8514(18) . ?
C1 H1 1.0000 . ?
C2 O1 1.435(2) . ?
C2 C9 1.501(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.385(3) . ?
C3 C8 1.388(3) . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.386(3) . ?
C9 C10 1.388(3) . ?
C10 C11 1.382(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C18 1.531(3) . ?
C15 C17 1.535(3) . ?
C15 C16 1.536(3) . ?
C15 P1 1.852(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.525(3) . ?
C19 C23 1.530(3) . ?
C19 C20 1.542(3) . ?
C19 P1 1.856(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 F2 1.316(3) . ?
C24 F5 1.325(3) . ?
C24 F6 1.329(3) . ?
C24 S1 1.812(2) . ?
O2 S1 1.4332(17) . ?
O3 S1 1.4340(18) . ?
O4 S1 1.4414(18) . ?
P1 H1A 1.33(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
O1 C1 C3 114.12(15) . . ?
O1 C1 P1 106.58(11) . . ?
C3 C1 P1 114.46(12) . . ?
O1 C1 H1 107.1 . . ?
C3 C1 H1 107.1 . . ?
P1 C1 H1 107.1 . . ?
O1 C2 C9 110.06(14) . . ?
O1 C2 H2A 109.6 . . ?
C9 C2 H2A 109.6 . . ?
O1 C2 H2B 109.6 . . ?
C9 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C8 119.53(18) . . ?
C4 C3 C1 121.39(17) . . ?
C8 C3 C1 119.04(16) . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.2(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 119.9(2) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C3 120.22(19) . . ?
C7 C8 H8 119.9 . . ?
C3 C8 H8 119.9 . . ?
C14 C9 C10 118.79(17) . . ?
C14 C9 C2 122.27(16) . . ?
C10 C9 C2 118.93(17) . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 119.9(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.3(2) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C9 C14 C13 120.15(19) . . ?
C9 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C18 C15 C17 110.5(2) . . ?
C18 C15 C16 110.6(2) . . ?
C17 C15 C16 108.55(19) . . ?
C18 C15 P1 111.46(14) . . ?
C17 C15 P1 108.53(16) . . ?
C16 C15 P1 107.11(15) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C23 109.29(17) . . ?
C21 C19 C20 111.52(17) . . ?
C23 C19 C20 107.68(17) . . ?
C21 C19 P1 112.68(13) . . ?
C23 C19 P1 107.26(13) . . ?
C20 C19 P1 108.21(15) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F2 C24 F5 107.1(2) . . ?
F2 C24 F6 106.8(2) . . ?
F5 C24 F6 108.4(2) . . ?
F2 C24 S1 112.6(2) . . ?
F5 C24 S1 110.76(16) . . ?
F6 C24 S1 110.92(16) . . ?
C1 O1 C2 111.31(13) . . ?
C1 P1 C15 114.50(9) . . ?
C1 P1 C19 109.30(8) . . ?
C15 P1 C19 117.63(10) . . ?
C1 P1 H1A 103.0(9) . . ?
C15 P1 H1A 104.5(9) . . ?
C19 P1 H1A 106.3(10) . . ?
O2 S1 O3 116.40(13) . . ?
O2 S1 O4 115.00(13) . . ?
O3 S1 O4 115.05(10) . . ?
O2 S1 C24 102.84(12) . . ?
O3 S1 C24 103.41(12) . . ?
O4 S1 C24 101.07(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C3 C4 -23.7(2) . . . . ?
P1 C1 C3 C4 99.44(18) . . . . ?
O1 C1 C3 C8 153.89(16) . . . . ?
P1 C1 C3 C8 -82.93(19) . . . . ?
C8 C3 C4 C5 -0.2(3) . . . . ?
C1 C3 C4 C5 177.44(18) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
C5 C6 C7 C8 -0.4(3) . . . . ?
C6 C7 C8 C3 1.1(3) . . . . ?
C4 C3 C8 C7 -0.8(3) . . . . ?
C1 C3 C8 C7 -178.50(18) . . . . ?
O1 C2 C9 C14 14.1(2) . . . . ?
O1 C2 C9 C10 -167.47(18) . . . . ?
C14 C9 C10 C11 0.5(3) . . . . ?
C2 C9 C10 C11 -178.0(2) . . . . ?
C9 C10 C11 C12 1.2(4) . . . . ?
C10 C11 C12 C13 -2.4(4) . . . . ?
C11 C12 C13 C14 1.9(4) . . . . ?
C10 C9 C14 C13 -0.9(3) . . . . ?
C2 C9 C14 C13 177.51(19) . . . . ?
C12 C13 C14 C9 -0.3(3) . . . . ?
C3 C1 O1 C2 -72.37(18) . . . . ?
P1 C1 O1 C2 160.27(12) . . . . ?
C9 C2 O1 C1 175.46(15) . . . . ?
O1 C1 P1 C15 65.47(15) . . . . ?
C3 C1 P1 C15 -61.69(16) . . . . ?
O1 C1 P1 C19 -68.94(13) . . . . ?
C3 C1 P1 C19 163.91(13) . . . . ?
C18 C15 P1 C1 -52.4(2) . . . . ?
C17 C15 P1 C1 -174.32(15) . . . . ?
C16 C15 P1 C1 68.66(17) . . . . ?
C18 C15 P1 C19 78.03(19) . . . . ?
C17 C15 P1 C19 -43.88(19) . . . . ?
C16 C15 P1 C19 -160.90(15) . . . . ?
C21 C19 P1 C1 87.34(16) . . . . ?
C23 C19 P1 C1 -32.97(15) . . . . ?
C20 C19 P1 C1 -148.88(14) . . . . ?
C21 C19 P1 C15 -45.45(18) . . . . ?
C23 C19 P1 C15 -165.76(13) . . . . ?
C20 C19 P1 C15 78.33(16) . . . . ?
F2 C24 S1 O2 53.2(2) . . . . ?
F5 C24 S1 O2 -66.8(2) . . . . ?
F6 C24 S1 O2 172.8(2) . . . . ?
F2 C24 S1 O3 -68.38(19) . . . . ?
F5 C24 S1 O3 171.68(18) . . . . ?
F6 C24 S1 O3 51.2(2) . . . . ?
F2 C24 S1 O4 172.26(17) . . . . ?
F5 C24 S1 O4 52.3(2) . . . . ?
F6 C24 S1 O4 -68.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.039
_database_code_depnum_ccdc_archive 'CCDC 991779'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[tBu2PH-thf][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H26 O P, C F3 O3 S'
_chemical_formula_sum            'C13 H26 F3 O4 P S'
_chemical_formula_weight         366.37

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'
F F 0.0727 0.0534 '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'

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

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

_cell_length_a                   8.19840(10)
_cell_length_b                   14.7753(2)
_cell_length_c                   15.1140(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1830.82(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      75

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    2.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4338
_exptl_absorpt_correction_T_max  0.8507
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.694204


;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10580
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.18
_diffrn_reflns_theta_max         68.24
_reflns_number_total             3262
_reflns_number_gt                3077
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0972P)²+3.8311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_number_reflns         3262
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1822
_refine_ls_wR_factor_gt          0.1798
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.2188(5) 0.4890(3) 0.1260(3) 0.0323(10) Uani 1 1 d . . .
C2 C 1.2274(8) 0.5818(4) 0.0817(4) 0.0482(14) Uani 1 1 d . . .
H2A H 1.3299 0.6116 0.0979 0.072 Uiso 1 1 calc R . .
H2B H 1.1353 0.6189 0.1014 0.072 Uiso 1 1 calc R . .
H2C H 1.2225 0.5744 0.0173 0.072 Uiso 1 1 calc R . .
C3 C 1.2394(7) 0.5018(4) 0.2264(3) 0.0418(12) Uani 1 1 d . . .
H3A H 1.2355 0.4427 0.2557 0.063 Uiso 1 1 calc R . .
H3B H 1.1512 0.5401 0.2490 0.063 Uiso 1 1 calc R . .
H3C H 1.3447 0.5307 0.2384 0.063 Uiso 1 1 calc R . .
C4 C 1.3458(7) 0.4233(4) 0.0922(4) 0.0522(14) Uani 1 1 d . . .
H4A H 1.3391 0.4196 0.0275 0.078 Uiso 1 1 calc R . .
H4B H 1.3260 0.3633 0.1177 0.078 Uiso 1 1 calc R . .
H4C H 1.4547 0.4444 0.1094 0.078 Uiso 1 1 calc R . .
C5 C 0.9573(7) 0.4059(4) -0.0057(3) 0.0396(12) Uani 1 1 d . . .
C6 C 1.0119(9) 0.3090(4) -0.0190(4) 0.0605(17) Uani 1 1 d . . .
H6A H 0.9660 0.2709 0.0279 0.091 Uiso 1 1 calc R . .
H6B H 1.1312 0.3060 -0.0169 0.091 Uiso 1 1 calc R . .
H6C H 0.9737 0.2873 -0.0767 0.091 Uiso 1 1 calc R . .
C7 C 0.7685(7) 0.4110(5) -0.0126(4) 0.0558(15) Uani 1 1 d . . .
H7A H 0.7339 0.3902 -0.0712 0.084 Uiso 1 1 calc R . .
H7B H 0.7329 0.4737 -0.0038 0.084 Uiso 1 1 calc R . .
H7C H 0.7194 0.3724 0.0329 0.084 Uiso 1 1 calc R . .
C8 C 1.0265(8) 0.4705(5) -0.0748(4) 0.0596(16) Uani 1 1 d . . .
H8A H 1.1459 0.4694 -0.0723 0.089 Uiso 1 1 calc R . .
H8B H 0.9877 0.5321 -0.0629 0.089 Uiso 1 1 calc R . .
H8C H 0.9903 0.4517 -0.1338 0.089 Uiso 1 1 calc R . .
C9 C 0.9558(7) 0.3607(3) 0.1917(4) 0.0396(12) Uani 1 1 d . . .
H9 H 1.0529 0.3212 0.2023 0.048 Uiso 1 1 calc R . .
C10 C 0.9011(7) 0.4027(4) 0.2794(4) 0.0417(12) Uani 1 1 d . . .
H10A H 0.9815 0.3911 0.3269 0.050 Uiso 1 1 calc R . .
H10B H 0.8842 0.4687 0.2736 0.050 Uiso 1 1 calc R . .
C11 C 0.7440(11) 0.3547(6) 0.2970(6) 0.088(3) Uani 1 1 d . . .
H11A H 0.7438 0.3294 0.3576 0.106 Uiso 1 1 calc R . .
H11B H 0.6513 0.3972 0.2914 0.106 Uiso 1 1 calc R . .
C12 C 0.7291(8) 0.2824(5) 0.2325(4) 0.0600(16) Uani 1 1 d . . .
H12A H 0.7679 0.2245 0.2579 0.072 Uiso 1 1 calc R . .
H12B H 0.6139 0.2751 0.2143 0.072 Uiso 1 1 calc R . .
C13 C 1.2142(7) 0.7773(4) -0.1023(4) 0.0445(12) Uani 1 1 d . . .
O1 O 0.8254(5) 0.3071(3) 0.1598(3) 0.0543(11) Uani 1 1 d . . .
O2 O 1.4081(4) 0.8466(3) -0.2170(3) 0.0470(9) Uani 1 1 d . . .
O3 O 1.1374(6) 0.9078(3) -0.2051(3) 0.0694(14) Uani 1 1 d . . .
O4 O 1.1810(6) 0.7595(3) -0.2696(3) 0.0608(12) Uani 1 1 d . . .
F1 F 1.2608(7) 0.8342(4) -0.0396(2) 0.0923(15) Uani 1 1 d . . .
F2 F 1.3040(6) 0.7051(3) -0.0952(3) 0.0910(16) Uani 1 1 d . . .
F3 F 1.0616(5) 0.7549(3) -0.0850(3) 0.0741(12) Uani 1 1 d . . .
P1 P 1.00662(16) 0.44593(9) 0.10756(8) 0.0356(3) Uani 1 1 d . . .
S1 S 1.23633(14) 0.82830(8) -0.21117(8) 0.0342(3) Uani 1 1 d . . .
H1 H 0.917(7) 0.515(4) 0.140(4) 0.049(17) Uiso 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
C1 C4 1.513(7) . ?
C1 C2 1.527(7) . ?
C1 C3 1.539(6) . ?
C1 P1 1.873(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.513(8) . ?
C5 C8 1.526(8) . ?
C5 C7 1.553(8) . ?
C5 P1 1.855(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O1 1.415(6) . ?
C9 C10 1.531(7) . ?
C9 P1 1.838(5) . ?
C9 H9 1.0000 . ?
C10 C11 1.494(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.450(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O1 1.401(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 F2 1.301(7) . ?
C13 F3 1.320(7) . ?
C13 F1 1.323(7) . ?
C13 S1 1.819(5) . ?
O2 S1 1.437(4) . ?
O3 S1 1.431(4) . ?
O4 S1 1.421(4) . ?
P1 H1 1.35(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
C4 C1 C2 113.3(4) . . ?
C4 C1 C3 109.6(4) . . ?
C2 C1 C3 108.5(4) . . ?
C4 C1 P1 111.8(4) . . ?
C2 C1 P1 106.4(3) . . ?
C3 C1 P1 106.9(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C8 113.0(5) . . ?
C6 C5 C7 109.4(5) . . ?
C8 C5 C7 107.1(5) . . ?
C6 C5 P1 111.1(4) . . ?
C8 C5 P1 110.6(4) . . ?
C7 C5 P1 105.3(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 C10 107.5(4) . . ?
O1 C9 P1 108.6(4) . . ?
C10 C9 P1 112.8(4) . . ?
O1 C9 H9 109.3 . . ?
C10 C9 H9 109.3 . . ?
P1 C9 H9 109.3 . . ?
C11 C10 C9 102.4(5) . . ?
C11 C10 H10A 111.3 . . ?
C9 C10 H10A 111.3 . . ?
C11 C10 H10B 111.3 . . ?
C9 C10 H10B 111.3 . . ?
H10A C10 H10B 109.2 . . ?
C12 C11 C10 107.6(6) . . ?
C12 C11 H11A 110.2 . . ?
C10 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
C10 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O1 C12 C11 106.7(5) . . ?
O1 C12 H12A 110.4 . . ?
C11 C12 H12A 110.4 . . ?
O1 C12 H12B 110.4 . . ?
C11 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
F2 C13 F3 108.4(5) . . ?
F2 C13 F1 107.4(5) . . ?
F3 C13 F1 107.0(5) . . ?
F2 C13 S1 110.9(4) . . ?
F3 C13 S1 112.2(4) . . ?
F1 C13 S1 110.8(4) . . ?
C12 O1 C9 107.7(4) . . ?
C9 P1 C5 111.7(2) . . ?
C9 P1 C1 109.9(2) . . ?
C5 P1 C1 116.6(2) . . ?
C9 P1 H1 98(3) . . ?
C5 P1 H1 117(3) . . ?
C1 P1 H1 101(3) . . ?
O4 S1 O3 116.5(3) . . ?
O4 S1 O2 114.1(3) . . ?
O3 S1 O2 113.9(3) . . ?
O4 S1 C13 103.6(3) . . ?
O3 S1 C13 103.0(3) . . ?
O2 S1 C13 103.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        68.24
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.984
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 991780'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad[Ph2PH-Trt][OTf]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H26 P, C F3 O3 S'
_chemical_formula_sum            'C32 H26 F3 O3 P S'
_chemical_formula_weight         578.56

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  'C -2yc'

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

_cell_length_a                   10.6205(7)
_cell_length_b                   16.6690(11)
_cell_length_c                   15.7534(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.2710(10)
_cell_angle_gamma                90.00
_cell_volume                     2786.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      22.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9668
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =   0.820579

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10908
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         27.87
_reflns_number_total             5983
_reflns_number_gt                5407
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0427P)²+0.6205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_number_reflns         5983
_refine_ls_number_parameters     365
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C32 C -0.0456(2) 0.33538(14) 0.22761(16) 0.0327(5) Uani 1 1 d . . .
O1 O -0.09280(14) 0.45226(9) 0.12598(10) 0.0319(4) Uani 1 1 d . . .
O2 O 0.07834(16) 0.36432(10) 0.09406(11) 0.0379(4) Uani 1 1 d . . .
O3 O 0.10104(15) 0.45707(9) 0.21282(11) 0.0367(4) Uani 1 1 d . . .
F1 F -0.13612(13) 0.29203(8) 0.18728(9) 0.0414(4) Uani 1 1 d . . .
F2 F -0.09713(16) 0.36953(10) 0.29450(10) 0.0513(4) Uani 1 1 d . . .
F3 F 0.04265(14) 0.28414(9) 0.25578(11) 0.0506(4) Uani 1 1 d . . .
S1 S 0.01889(5) 0.41076(3) 0.15705(3) 0.02583(12) Uani 1 1 d . . .
C1 C 0.52964(19) 0.41556(12) 0.03844(13) 0.0226(4) Uani 1 1 d . . .
C2 C 0.42843(19) 0.39676(12) -0.03222(13) 0.0254(4) Uani 1 1 d . . .
C3 C 0.3780(2) 0.31969(13) -0.04186(15) 0.0298(5) Uani 1 1 d . . .
H3 H 0.4003 0.2793 -0.0015 0.036 Uiso 1 1 calc R . .
C4 C 0.2950(2) 0.30135(15) -0.11025(16) 0.0359(5) Uani 1 1 d . . .
H4 H 0.2614 0.2487 -0.1161 0.043 Uiso 1 1 calc R . .
C5 C 0.2620(2) 0.35972(17) -0.16933(16) 0.0425(6) Uani 1 1 d . . .
H5 H 0.2058 0.3473 -0.2159 0.051 Uiso 1 1 calc R . .
C6 C 0.3108(2) 0.43586(16) -0.16058(16) 0.0402(6) Uani 1 1 d . . .
H6 H 0.2875 0.4761 -0.2010 0.048 Uiso 1 1 calc R . .
C7 C 0.3941(2) 0.45444(14) -0.09276(14) 0.0328(5) Uani 1 1 d . . .
H7 H 0.4279 0.5071 -0.0878 0.039 Uiso 1 1 calc R . .
C8 C 0.5606(2) 0.50608(12) 0.04169(13) 0.0270(5) Uani 1 1 d . . .
C9 C 0.6730(2) 0.54028(12) 0.02085(14) 0.0304(5) Uani 1 1 d . . .
H9 H 0.7404 0.5068 0.0047 0.036 Uiso 1 1 calc R . .
C10 C 0.6901(3) 0.62387(14) 0.02308(16) 0.0406(6) Uani 1 1 d . . .
H10 H 0.7687 0.6467 0.0093 0.049 Uiso 1 1 calc R . .
C11 C 0.5919(3) 0.67247(15) 0.04546(18) 0.0473(7) Uani 1 1 d . . .
H11 H 0.6017 0.7291 0.0454 0.057 Uiso 1 1 calc R . .
C12 C 0.4795(3) 0.63883(15) 0.06787(19) 0.0500(8) Uani 1 1 d . . .
H12 H 0.4122 0.6725 0.0838 0.060 Uiso 1 1 calc R . .
C13 C 0.4636(2) 0.55626(15) 0.06740(17) 0.0391(6) Uani 1 1 d . . .
H13 H 0.3866 0.5337 0.0846 0.047 Uiso 1 1 calc R . .
C14 C 0.5004(2) 0.38819(13) 0.13021(14) 0.0249(4) Uani 1 1 d . . .
C15 C 0.5920(2) 0.40148(13) 0.19449(14) 0.0274(5) Uani 1 1 d . . .
H15 H 0.6688 0.4271 0.1815 0.033 Uiso 1 1 calc R . .
C16 C 0.5722(2) 0.37781(15) 0.27680(15) 0.0356(5) Uani 1 1 d . . .
H16 H 0.6357 0.3867 0.3200 0.043 Uiso 1 1 calc R . .
C17 C 0.4603(3) 0.34120(18) 0.29679(16) 0.0452(6) Uani 1 1 d . . .
H17 H 0.4478 0.3232 0.3530 0.054 Uiso 1 1 calc R . .
C18 C 0.3660(2) 0.33105(17) 0.23375(17) 0.0441(6) Uani 1 1 d . . .
H18 H 0.2877 0.3078 0.2474 0.053 Uiso 1 1 calc R . .
C19 C 0.3863(2) 0.35484(15) 0.15068(15) 0.0340(5) Uani 1 1 d . . .
H19 H 0.3215 0.3481 0.1079 0.041 Uiso 1 1 calc R . .
C20 C 0.64753(17) 0.24885(11) 0.01694(13) 0.0218(4) Uani 1 1 d . . .
C21 C 0.6229(2) 0.21088(13) 0.09314(14) 0.0269(5) Uani 1 1 d . . .
H21 H 0.6155 0.2415 0.1436 0.032 Uiso 1 1 calc R . .
C22 C 0.6094(2) 0.12863(14) 0.09526(16) 0.0330(5) Uani 1 1 d . . .
H22 H 0.5925 0.1027 0.1473 0.040 Uiso 1 1 calc R . .
C23 C 0.6201(2) 0.08350(13) 0.02201(17) 0.0365(6) Uani 1 1 d . . .
H23 H 0.6098 0.0269 0.0239 0.044 Uiso 1 1 calc R . .
C24 C 0.6457(2) 0.12039(13) -0.05314(16) 0.0356(5) Uani 1 1 d . . .
H24 H 0.6538 0.0892 -0.1031 0.043 Uiso 1 1 calc R . .
C25 C 0.6599(2) 0.20316(12) -0.05660(14) 0.0283(5) Uani 1 1 d . . .
H25 H 0.6779 0.2286 -0.1087 0.034 Uiso 1 1 calc R . .
C26 C 0.7318(2) 0.37849(12) -0.09087(13) 0.0231(4) Uani 1 1 d . . .
C27 C 0.6581(2) 0.37751(13) -0.16603(14) 0.0278(5) Uani 1 1 d . . .
H27 H 0.5708 0.3655 -0.1647 0.033 Uiso 1 1 calc R . .
C28 C 0.7119(3) 0.39388(15) -0.24247(15) 0.0380(6) Uani 1 1 d . . .
H28 H 0.6618 0.3926 -0.2938 0.046 Uiso 1 1 calc R . .
C29 C 0.8376(3) 0.41192(15) -0.24421(17) 0.0432(6) Uani 1 1 d . . .
H29 H 0.8737 0.4239 -0.2969 0.052 Uiso 1 1 calc R . .
C30 C 0.9125(3) 0.41292(17) -0.17058(18) 0.0438(6) Uani 1 1 d . . .
H30 H 0.9997 0.4252 -0.1731 0.053 Uiso 1 1 calc R . .
C31 C 0.8613(2) 0.39615(14) -0.09323(16) 0.0342(5) Uani 1 1 d . . .
H31 H 0.9126 0.3965 -0.0425 0.041 Uiso 1 1 calc R . .
P1 P 0.67128(4) 0.35574(3) 0.01052(3) 0.01978(11) Uani 1 1 d . . .
H1 H 0.757(2) 0.3746(13) 0.0617(14) 0.022(6) Uiso 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
C32 F3 1.331(3) . ?
C32 F2 1.334(3) . ?
C32 F1 1.342(3) . ?
C32 S1 1.829(2) . ?
O1 S1 1.4419(16) . ?
O2 S1 1.4255(18) . ?
O3 S1 1.4381(16) . ?
C1 C8 1.545(3) . ?
C1 C2 1.549(3) . ?
C1 C14 1.559(3) . ?
C1 P1 1.872(2) . ?
C2 C7 1.393(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.398(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.376(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 C13 1.399(3) . ?
C9 C10 1.405(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.383(3) . ?
C14 C15 1.394(3) . ?
C15 C16 1.380(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.391(3) . ?
C20 C25 1.397(3) . ?
C20 P1 1.8030(19) . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.393(3) . ?
C26 C31 1.409(3) . ?
C26 P1 1.786(2) . ?
C27 C28 1.380(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.369(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.381(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
P1 H1 1.23(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
F3 C32 F2 108.4(2) . . ?
F3 C32 F1 107.10(19) . . ?
F2 C32 F1 107.2(2) . . ?
F3 C32 S1 111.57(17) . . ?
F2 C32 S1 111.23(16) . . ?
F1 C32 S1 111.15(16) . . ?
O2 S1 O3 116.24(11) . . ?
O2 S1 O1 113.92(11) . . ?
O3 S1 O1 114.89(9) . . ?
O2 S1 C32 103.70(11) . . ?
O3 S1 C32 103.32(10) . . ?
O1 S1 C32 102.29(10) . . ?
C8 C1 C2 111.23(16) . . ?
C8 C1 C14 107.76(16) . . ?
C2 C1 C14 116.71(17) . . ?
C8 C1 P1 110.88(14) . . ?
C2 C1 P1 105.35(13) . . ?
C14 C1 P1 104.68(13) . . ?
C7 C2 C3 118.12(19) . . ?
C7 C2 C1 120.52(19) . . ?
C3 C2 C1 121.09(18) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.8(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.4(2) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C6 120.8(2) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C13 118.5(2) . . ?
C9 C8 C1 125.64(19) . . ?
C13 C8 C1 115.8(2) . . ?
C8 C9 C10 121.2(2) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 119.9(2) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.6(2) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 120.3(3) . . ?
C12 C13 H13 119.8 . . ?
C8 C13 H13 119.8 . . ?
C19 C14 C15 119.2(2) . . ?
C19 C14 C1 122.83(19) . . ?
C15 C14 C1 117.93(19) . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.3(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 119.4(2) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 120.2(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 120.2(2) . . ?
C14 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C25 119.65(18) . . ?
C21 C20 P1 121.97(16) . . ?
C25 C20 P1 118.31(15) . . ?
C22 C21 C20 119.8(2) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 120.5(2) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.3(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 119.7(2) . . ?
C24 C25 H25 120.2 . . ?
C20 C25 H25 120.2 . . ?
C27 C26 C31 119.7(2) . . ?
C27 C26 P1 123.24(17) . . ?
C31 C26 P1 117.01(17) . . ?
C28 C27 C26 120.1(2) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C29 C28 C27 119.9(2) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 121.0(2) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C31 120.3(2) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C26 119.0(2) . . ?
C30 C31 H31 120.5 . . ?
C26 C31 H31 120.5 . . ?
C26 P1 C20 108.43(10) . . ?
C26 P1 C1 114.71(9) . . ?
C20 P1 C1 113.44(9) . . ?
C26 P1 H1 104.5(10) . . ?
C20 P1 H1 108.5(10) . . ?
C1 P1 H1 106.7(10) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.043
_database_code_depnum_ccdc_archive 'CCDC 991781'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H38 P, C F3 O3 S'
_chemical_formula_sum            'C32 H38 F3 O3 P S'
_chemical_formula_weight         590.65

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'
F F 0.0727 0.0534 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.70330(10)
_cell_length_b                   17.8716(2)
_cell_length_c                   16.8564(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4360(10)
_cell_angle_gamma                90.00
_cell_volume                     2917.87(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    900
_cell_measurement_theta_min      1
_cell_measurement_theta_max      75

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_T_max  0.8924
_exptl_absorpt_process_details   
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.694747

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean 80
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16702
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         68.22
_reflns_number_total             5200
_reflns_number_gt                4373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_structure_solution    
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_refinement  
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_molecular_graphics    
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0669P)²+0.4977P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5200
_refine_ls_number_parameters     365
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1097
_refine_ls_wR_factor_gt          0.1061
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.33212(17) 0.10847(9) 0.87388(10) 0.0213(3) Uani 1 1 d . . .
C2 C 0.46523(17) 0.15288(9) 0.89775(10) 0.0227(4) Uani 1 1 d . . .
C3 C 0.50333(19) 0.22025(10) 0.86443(10) 0.0273(4) Uani 1 1 d . . .
H3 H 0.4458 0.2419 0.8230 0.033 Uiso 1 1 calc R . .
C4 C 0.62443(19) 0.25658(11) 0.89068(11) 0.0309(4) Uani 1 1 d . . .
H4 H 0.6492 0.3024 0.8669 0.037 Uiso 1 1 calc R . .
C5 C 0.70886(19) 0.22611(11) 0.95134(11) 0.0313(4) Uani 1 1 d . . .
H5 H 0.7927 0.2502 0.9685 0.038 Uiso 1 1 calc R . .
C6 C 0.67016(19) 0.16026(11) 0.98678(11) 0.0304(4) Uani 1 1 d . . .
H6 H 0.7269 0.1396 1.0291 0.036 Uiso 1 1 calc R . .
C7 C 0.54965(18) 0.12433(10) 0.96108(10) 0.0257(4) Uani 1 1 d . . .
H7 H 0.5236 0.0796 0.9867 0.031 Uiso 1 1 calc R . .
C8 C 0.23860(17) 0.11555(9) 0.94452(10) 0.0218(3) Uani 1 1 d . . .
C9 C 0.18023(18) 0.18446(10) 0.96110(10) 0.0248(4) Uani 1 1 d . . .
H9 H 0.1967 0.2263 0.9283 0.030 Uiso 1 1 calc R . .
C10 C 0.09806(18) 0.19255(11) 1.02525(11) 0.0292(4) Uani 1 1 d . . .
H10 H 0.0553 0.2393 1.0346 0.035 Uiso 1 1 calc R . .
C11 C 0.0781(2) 0.13299(12) 1.07565(11) 0.0341(4) Uani 1 1 d . . .
H11 H 0.0220 0.1386 1.1196 0.041 Uiso 1 1 calc R . .
C12 C 0.1404(2) 0.06513(12) 1.06150(11) 0.0351(4) Uani 1 1 d . . .
H12 H 0.1292 0.0244 1.0967 0.042 Uiso 1 1 calc R . .
C13 C 0.21969(19) 0.05606(10) 0.99594(11) 0.0288(4) Uani 1 1 d . . .
H13 H 0.2610 0.0090 0.9863 0.035 Uiso 1 1 calc R . .
C14 C 0.36199(17) 0.02732(9) 0.84852(10) 0.0227(4) Uani 1 1 d . . .
C15 C 0.25420(18) -0.02398(10) 0.83581(10) 0.0258(4) Uani 1 1 d . . .
H15 H 0.1632 -0.0100 0.8475 0.031 Uiso 1 1 calc R . .
C16 C 0.2780(2) -0.09478(10) 0.80646(11) 0.0316(4) Uani 1 1 d . . .
H16 H 0.2032 -0.1286 0.7975 0.038 Uiso 1 1 calc R . .
C17 C 0.4098(2) -0.11655(11) 0.79004(12) 0.0362(5) Uani 1 1 d . . .
H17 H 0.4263 -0.1656 0.7710 0.043 Uiso 1 1 calc R . .
C18 C 0.5179(2) -0.06628(12) 0.80150(12) 0.0373(5) Uani 1 1 d . . .
H18 H 0.6087 -0.0807 0.7898 0.045 Uiso 1 1 calc R . .
C19 C 0.49407(19) 0.00519(11) 0.83008(11) 0.0290(4) Uani 1 1 d . . .
H19 H 0.5687 0.0394 0.8371 0.035 Uiso 1 1 calc R . .
C20 C 0.06769(17) 0.11589(10) 0.75440(10) 0.0238(4) Uani 1 1 d . . .
H20 H 0.0716 0.0622 0.7380 0.029 Uiso 1 1 calc R . .
C21 C -0.03028(18) 0.12378(10) 0.82197(11) 0.0271(4) Uani 1 1 d . . .
H21A H -0.0007 0.0895 0.8659 0.033 Uiso 1 1 calc R . .
H21B H -0.0260 0.1756 0.8427 0.033 Uiso 1 1 calc R . .
C22 C -0.17831(19) 0.10546(12) 0.79282(12) 0.0328(4) Uani 1 1 d . . .
H22A H -0.1836 0.0525 0.7757 0.039 Uiso 1 1 calc R . .
H22B H -0.2398 0.1120 0.8371 0.039 Uiso 1 1 calc R . .
C23 C -0.2272(2) 0.15493(14) 0.72453(13) 0.0419(5) Uani 1 1 d . . .
H23A H -0.2267 0.2078 0.7421 0.050 Uiso 1 1 calc R . .
H23B H -0.3230 0.1414 0.7067 0.050 Uiso 1 1 calc R . .
C24 C -0.1332(2) 0.14588(13) 0.65570(12) 0.0402(5) Uani 1 1 d . . .
H24A H -0.1389 0.0938 0.6359 0.048 Uiso 1 1 calc R . .
H24B H -0.1649 0.1795 0.6116 0.048 Uiso 1 1 calc R . .
C25 C 0.01529(19) 0.16417(11) 0.68162(11) 0.0316(4) Uani 1 1 d . . .
H25A H 0.0225 0.2178 0.6958 0.038 Uiso 1 1 calc R . .
H25B H 0.0746 0.1550 0.6368 0.038 Uiso 1 1 calc R . .
C26 C 0.35639(18) 0.13752(10) 0.69935(10) 0.0250(4) Uani 1 1 d . . .
H26 H 0.4522 0.1314 0.7238 0.030 Uiso 1 1 calc R . .
C27 C 0.3253(2) 0.06748(11) 0.64875(11) 0.0306(4) Uani 1 1 d . . .
H27A H 0.3295 0.0225 0.6831 0.037 Uiso 1 1 calc R . .
H27B H 0.2311 0.0710 0.6230 0.037 Uiso 1 1 calc R . .
C28 C 0.4310(2) 0.06053(13) 0.58510(13) 0.0447(5) Uani 1 1 d . . .
H28A H 0.5242 0.0530 0.6111 0.054 Uiso 1 1 calc R . .
H28B H 0.4085 0.0163 0.5514 0.054 Uiso 1 1 calc R . .
C29 C 0.4313(3) 0.13054(14) 0.53322(13) 0.0502(6) Uani 1 1 d . . .
H29A H 0.5034 0.1255 0.4945 0.060 Uiso 1 1 calc R . .
H29B H 0.3409 0.1350 0.5030 0.060 Uiso 1 1 calc R . .
C30 C 0.4579(2) 0.20087(13) 0.58192(12) 0.0405(5) Uani 1 1 d . . .
H30A H 0.4495 0.2450 0.5465 0.049 Uiso 1 1 calc R . .
H30B H 0.5534 0.1996 0.6061 0.049 Uiso 1 1 calc R . .
C31 C 0.3570(2) 0.20888(11) 0.64756(11) 0.0313(4) Uani 1 1 d . . .
H31A H 0.2629 0.2180 0.6235 0.038 Uiso 1 1 calc R . .
H31B H 0.3837 0.2524 0.6814 0.038 Uiso 1 1 calc R . .
C32 C 0.0437(4) 0.41449(15) 0.90932(15) 0.0640(8) Uani 1 1 d . . .
O1 O 0.06607(19) 0.43580(8) 0.76136(9) 0.0512(4) Uani 1 1 d . . .
O2 O 0.22214(18) 0.34592(10) 0.82901(11) 0.0576(5) Uani 1 1 d . . .
O3 O -0.0168(2) 0.31623(9) 0.80390(12) 0.0670(5) Uani 1 1 d . . .
F1 F 0.1367(3) 0.46666(10) 0.93207(11) 0.1138(9) Uani 1 1 d . . .
F2 F 0.0474(2) 0.36425(10) 0.96748(9) 0.0839(6) Uani 1 1 d . . .
F3 F -0.0770(3) 0.44634(14) 0.90538(12) 0.1307(11) Uani 1 1 d . . .
P1 P 0.24246(4) 0.14890(2) 0.78175(2) 0.02042(12) Uani 1 1 d . . .
S1 S 0.08457(6) 0.37403(3) 0.81493(3) 0.03813(15) Uani 1 1 d . . .
H1 H 0.2295(18) 0.2200(10) 0.7923(11) 0.020(4) Uiso 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
C1 C14 1.544(2) . ?
C1 C8 1.545(2) . ?
C1 C2 1.548(2) . ?
C1 P1 1.8786(17) . ?
C2 C3 1.388(2) . ?
C2 C7 1.402(2) . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.391(2) . ?
C8 C9 1.391(2) . ?
C9 C10 1.389(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.394(2) . ?
C14 C15 1.398(2) . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.533(2) . ?
C20 C25 1.560(2) . ?
C20 P1 1.8284(17) . ?
C20 H20 1.0000 . ?
C21 C22 1.526(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.505(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.527(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.516(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.534(2) . ?
C26 C31 1.546(2) . ?
C26 P1 1.8376(17) . ?
C26 H26 1.0000 . ?
C27 C28 1.533(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.527(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.515(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.528(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 F3 1.300(3) . ?
C32 F2 1.328(3) . ?
C32 F1 1.338(4) . ?
C32 S1 1.813(3) . ?
O1 S1 1.4307(15) . ?
O2 S1 1.4326(18) . ?
O3 S1 1.4310(18) . ?
P1 H1 1.290(18) . ?

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
C14 C1 C8 114.76(13) . . ?
C14 C1 C2 112.69(13) . . ?
C8 C1 C2 106.09(13) . . ?
C14 C1 P1 102.57(11) . . ?
C8 C1 P1 109.96(11) . . ?
C2 C1 P1 110.82(11) . . ?
C3 C2 C7 117.77(16) . . ?
C3 C2 C1 125.29(15) . . ?
C7 C2 C1 116.84(15) . . ?
C2 C3 C4 121.10(17) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 120.19(17) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.38(17) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C7 C6 C5 120.49(17) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C2 120.98(17) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C13 C8 C9 118.77(15) . . ?
C13 C8 C1 121.55(15) . . ?
C9 C8 C1 119.50(15) . . ?
C10 C9 C8 120.55(16) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 120.42(17) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 119.37(17) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.47(17) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 120.33(17) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C19 C14 C15 117.99(16) . . ?
C19 C14 C1 121.23(15) . . ?
C15 C14 C1 120.48(15) . . ?
C16 C15 C14 121.04(16) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 120.38(18) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 119.48(18) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 120.24(18) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.84(18) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
C21 C20 C25 110.24(14) . . ?
C21 C20 P1 112.96(12) . . ?
C25 C20 P1 105.87(12) . . ?
C21 C20 H20 109.2 . . ?
C25 C20 H20 109.2 . . ?
P1 C20 H20 109.2 . . ?
C22 C21 C20 110.78(15) . . ?
C22 C21 H21A 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C21 111.56(16) . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 C24 110.11(17) . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.2 . . ?
C25 C24 C23 111.03(17) . . ?
C25 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C20 111.51(15) . . ?
C24 C25 H25A 109.3 . . ?
C20 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
C20 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C27 C26 C31 111.50(15) . . ?
C27 C26 P1 113.79(12) . . ?
C31 C26 P1 111.00(12) . . ?
C27 C26 H26 106.7 . . ?
C31 C26 H26 106.7 . . ?
P1 C26 H26 106.7 . . ?
C28 C27 C26 109.74(16) . . ?
C28 C27 H27A 109.7 . . ?
C26 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
C26 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
C29 C28 C27 111.02(18) . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28B 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C30 C29 C28 112.07(18) . . ?
C30 C29 H29A 109.2 . . ?
C28 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 C31 111.99(17) . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
C31 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C26 110.86(16) . . ?
C30 C31 H31A 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
F3 C32 F2 108.5(3) . . ?
F3 C32 F1 107.4(3) . . ?
F2 C32 F1 105.8(2) . . ?
F3 C32 S1 111.9(2) . . ?
F2 C32 S1 112.36(17) . . ?
F1 C32 S1 110.5(2) . . ?
C20 P1 C26 111.38(8) . . ?
C20 P1 C1 117.45(8) . . ?
C26 P1 C1 108.21(8) . . ?
C20 P1 H1 104.8(8) . . ?
C26 P1 H1 106.3(8) . . ?
C1 P1 H1 108.0(8) . . ?
O1 S1 O3 114.56(11) . . ?
O1 S1 O2 117.10(11) . . ?
O3 S1 O2 113.26(11) . . ?
O1 S1 C32 102.74(10) . . ?
O3 S1 C32 102.55(14) . . ?
O2 S1 C32 104.18(13) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        68.22
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.049

#===end



_database_code_depnum_ccdc_archive 'CCDC 991782'
