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

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

data_dal08c4
_database_code_depnum_ccdc_archive 'CCDC 1418255'
_audit_update_record             
;
2015-08-12 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C10 H27 P3, 2(C F3 O3 S)'

_chemical_formula_sum            'C12 H27 F6 O6 P3 S2'

_chemical_formula_weight         538.37



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source












C C 0.0033 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/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                   6.581(4)

_cell_length_b                   21.895(12)

_cell_length_c                   16.904(9)

_cell_angle_alpha                90.00

_cell_angle_beta                 91.650(8)

_cell_angle_gamma                90.00

_cell_volume                     2435(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    7293

_cell_measurement_theta_min      3.04

_cell_measurement_theta_max      26.58



_exptl_crystal_description       plate

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.78

_exptl_crystal_size_mid          0.31

_exptl_crystal_size_min          0.08

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.469

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1112

_exptl_absorpt_coefficient_mu    0.485

_exptl_absorpt_correction_type   integration

_exptl_absorpt_correction_T_min  0.7040

_exptl_absorpt_correction_T_max  0.9604

_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      173(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       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            18399

_diffrn_reflns_av_R_equivalents  0.0779

_diffrn_reflns_av_sigmaI/netI    0.0599

_diffrn_reflns_limit_h_min       -8

_diffrn_reflns_limit_h_max       8

_diffrn_reflns_limit_k_min       -27

_diffrn_reflns_limit_k_max       27

_diffrn_reflns_limit_l_min       -21

_diffrn_reflns_limit_l_max       21

_diffrn_reflns_theta_min         1.52

_diffrn_reflns_theta_max         26.60

_reflns_number_total             5045

_reflns_number_gt                3463

_reflns_threshold_expression     I>2σ(I)



_computing_data_collection       'Bruker APEX2'

_computing_cell_refinement       'Bruker SAINT'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 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)+(0.0224P)²+4.2157P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         5045

_refine_ls_number_parameters     262

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0914

_refine_ls_R_factor_gt           0.0524

_refine_ls_wR_factor_ref         0.1061

_refine_ls_wR_factor_gt          0.0924

_refine_ls_goodness_of_fit_ref   1.093

_refine_ls_restrained_S_all      1.093

_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 0.00357(13) 0.14205(4) 0.25533(5) 0.0227(2) Uani 1 1 d . . .
P2 P 0.15872(13) 0.23067(4) 0.28403(5) 0.0230(2) Uani 1 1 d . . .
P3 P 0.13527(13) 0.12032(4) 0.13820(5) 0.0230(2) Uani 1 1 d . . .
C1 C 0.1039(6) 0.28146(15) 0.2022(2) 0.0307(8) Uani 1 1 d . . .
H1A H -0.0429 0.2820 0.1907 0.037 Uiso 1 1 calc R . .
H1B H 0.1747 0.2672 0.1554 0.037 Uiso 1 1 calc R . .
H1C H 0.1501 0.3228 0.2159 0.037 Uiso 1 1 calc R . .
C2 C 0.0348(6) 0.26175(16) 0.3693(2) 0.0339(9) Uani 1 1 d . . .
H2A H -0.1125 0.2627 0.3591 0.041 Uiso 1 1 calc R . .
H2B H 0.0843 0.3033 0.3795 0.041 Uiso 1 1 calc R . .
H2C H 0.0655 0.2361 0.4156 0.041 Uiso 1 1 calc R . .
C3 C 0.4303(5) 0.22967(17) 0.3050(2) 0.0331(8) Uani 1 1 d . . .
H3A H 0.4602 0.2023 0.3497 0.040 Uiso 1 1 calc R . .
H3B H 0.4767 0.2710 0.3184 0.040 Uiso 1 1 calc R . .
H3C H 0.5008 0.2152 0.2583 0.040 Uiso 1 1 calc R . .
C4 C 0.0127(6) 0.16930(16) 0.0647(2) 0.0316(8) Uani 1 1 d . . .
H4A H -0.1352 0.1664 0.0691 0.038 Uiso 1 1 calc R . .
H4B H 0.0511 0.1563 0.0117 0.038 Uiso 1 1 calc R . .
H4C H 0.0558 0.2116 0.0736 0.038 Uiso 1 1 calc R . .
C5 C 0.4073(5) 0.12648(16) 0.1284(2) 0.0316(8) Uani 1 1 d . . .
H5A H 0.4509 0.1682 0.1411 0.038 Uiso 1 1 calc R . .
H5B H 0.4428 0.1168 0.0739 0.038 Uiso 1 1 calc R . .
H5C H 0.4758 0.0978 0.1647 0.038 Uiso 1 1 calc R . .
C6 C 0.0572(6) 0.04290(15) 0.1152(2) 0.0333(9) Uani 1 1 d . . .
H6A H -0.0902 0.0392 0.1204 0.040 Uiso 1 1 calc R . .
H6B H 0.1263 0.0146 0.1519 0.040 Uiso 1 1 calc R . .
H6C H 0.0934 0.0330 0.0609 0.040 Uiso 1 1 calc R . .
C7 C 0.0990(5) 0.08064(15) 0.3290(2) 0.0284(8) Uani 1 1 d . . .
C8 C 0.0717(6) 0.10821(17) 0.4121(2) 0.0397(9) Uani 1 1 d . . .
H8A H 0.1668 0.1422 0.4203 0.048 Uiso 1 1 calc R . .
H8B H 0.0988 0.0768 0.4524 0.048 Uiso 1 1 calc R . .
H8C H -0.0680 0.1231 0.4166 0.048 Uiso 1 1 calc R . .
C9 C 0.3199(5) 0.05887(17) 0.3197(2) 0.0367(9) Uani 1 1 d . . .
H9A H 0.4127 0.0936 0.3270 0.044 Uiso 1 1 calc R . .
H9B H 0.3351 0.0417 0.2666 0.044 Uiso 1 1 calc R . .
H9C H 0.3522 0.0275 0.3595 0.044 Uiso 1 1 calc R . .
C10 C -0.0531(6) 0.02634(17) 0.3180(2) 0.0398(10) Uani 1 1 d . . .
H10A H -0.0386 0.0084 0.2654 0.048 Uiso 1 1 calc R . .
H10B H -0.1924 0.0413 0.3234 0.048 Uiso 1 1 calc R . .
H10C H -0.0237 -0.0047 0.3585 0.048 Uiso 1 1 calc R . .
S1 S 0.37323(13) 0.42750(4) 0.37188(5) 0.0264(2) Uani 1 1 d . . .
F1 F 0.7024(3) 0.43105(10) 0.46583(14) 0.0507(6) Uani 1 1 d . . .
F2 F 0.6033(3) 0.33933(9) 0.43356(14) 0.0492(6) Uani 1 1 d . . .
F3 F 0.7562(4) 0.39640(12) 0.34824(16) 0.0598(7) Uani 1 1 d . . .
O1 O 0.3113(4) 0.38432(12) 0.31077(16) 0.0490(7) Uani 1 1 d . . .
O2 O 0.4219(4) 0.48845(11) 0.34459(15) 0.0383(6) Uani 1 1 d . . .
O3 O 0.2539(4) 0.42493(13) 0.44257(16) 0.0440(7) Uani 1 1 d . . .
C11 C 0.6214(6) 0.39679(16) 0.4061(2) 0.0351(9) Uani 1 1 d . . .
S2 S 0.56760(14) 0.29790(4) 0.05026(5) 0.0295(2) Uani 1 1 d . . .
F4 F 0.5474(5) 0.41570(11) 0.01617(19) 0.0793(9) Uani 1 1 d . . .
F5 F 0.7592(5) 0.39411(12) 0.1091(2) 0.0910(11) Uani 1 1 d . . .
F6 F 0.4358(6) 0.39302(13) 0.1300(2) 0.1065(13) Uani 1 1 d . . .
O4 O 0.6163(4) 0.26619(12) 0.12427(16) 0.0461(7) Uani 1 1 d . . .
O5 O 0.3584(4) 0.28840(13) 0.02315(17) 0.0497(8) Uani 1 1 d . . .
O6 O 0.7175(5) 0.29338(14) -0.0094(2) 0.0646(9) Uani 1 1 d . . .
C12 C 0.5759(7) 0.37901(18) 0.0791(3) 0.0465(10) Uani 1 1 d . . .






_geom_special_details            
; 

 All esds (except the esd in the dihedral angle between two l.s. planes) 

 are estimated using the full covariance matrix.  The cell esds are taken 

 into account individually in the estimation of esds in distances, angles 

 and torsion angles; correlations between esds in cell parameters are only 

 used when they are defined by crystal symmetry.  An approximate (isotropic) 

 treatment of cell esds is used for estimating esds involving l.s. planes. 

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag


























P1 C7 1.925(3) . ?
P1 P3 2.2354(16) . ?
P1 P2 2.2391(15) . ?
P2 C1 1.804(3) . ?
P2 C2 1.810(3) . ?
P2 C3 1.812(4) . ?
P3 C5 1.808(4) . ?
P3 C6 1.810(3) . ?
P3 C4 1.813(3) . ?
C7 C9 1.542(5) . ?
C7 C8 1.545(5) . ?
C7 C10 1.562(5) . ?
S1 O3 1.450(3) . ?
S1 O1 1.450(3) . ?
S1 O2 1.451(3) . ?
S1 C11 1.844(4) . ?
F1 C11 1.355(4) . ?
F2 C11 1.347(4) . ?
F3 C11 1.339(4) . ?
S2 O6 1.434(3) . ?
S2 O5 1.453(3) . ?
S2 O4 1.458(3) . ?
S2 C12 1.842(4) . ?
F4 C12 1.342(5) . ?
F5 C12 1.336(5) . ?
F6 C12 1.315(5) . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag













































C7 P1 P3 107.25(12) . . ?
C7 P1 P2 109.08(12) . . ?
P3 P1 P2 100.97(5) . . ?
C1 P2 C2 107.13(18) . . ?
C1 P2 C3 109.39(18) . . ?
C2 P2 C3 108.24(17) . . ?
C1 P2 P1 106.75(12) . . ?
C2 P2 P1 106.58(13) . . ?
C3 P2 P1 118.23(12) . . ?
C5 P3 C6 109.01(17) . . ?
C5 P3 C4 108.37(17) . . ?
C6 P3 C4 106.80(17) . . ?
C5 P3 P1 118.42(12) . . ?
C6 P3 P1 105.94(13) . . ?
C4 P3 P1 107.75(13) . . ?
C9 C7 C8 110.4(3) . . ?
C9 C7 C10 110.8(3) . . ?
C8 C7 C10 108.3(3) . . ?
C9 C7 P1 116.2(2) . . ?
C8 C7 P1 105.7(2) . . ?
C10 C7 P1 105.0(2) . . ?
O3 S1 O1 114.46(18) . . ?
O3 S1 O2 115.31(16) . . ?
O1 S1 O2 115.68(17) . . ?
O3 S1 C11 102.89(17) . . ?
O1 S1 C11 102.36(17) . . ?
O2 S1 C11 103.51(16) . . ?
F3 C11 F2 108.2(3) . . ?
F3 C11 F1 107.0(3) . . ?
F2 C11 F1 107.3(3) . . ?
F3 C11 S1 111.9(3) . . ?
F2 C11 S1 111.3(3) . . ?
F1 C11 S1 111.0(2) . . ?
O6 S2 O5 115.7(2) . . ?
O6 S2 O4 115.6(2) . . ?
O5 S2 O4 112.65(17) . . ?
O6 S2 C12 103.71(19) . . ?
O5 S2 C12 104.01(19) . . ?
O4 S2 C12 103.15(18) . . ?
F6 C12 F5 109.7(4) . . ?
F6 C12 F4 107.1(4) . . ?
F5 C12 F4 104.8(3) . . ?
F6 C12 S2 112.5(3) . . ?
F5 C12 S2 111.0(3) . . ?
F4 C12 S2 111.4(3) . . ?



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




































C7 P1 P2 C1 168.50(17) . . . . ?
P3 P1 P2 C1 55.75(14) . . . . ?
C7 P1 P2 C2 -77.26(18) . . . . ?
P3 P1 P2 C2 169.99(13) . . . . ?
C7 P1 P2 C3 44.78(19) . . . . ?
P3 P1 P2 C3 -67.96(15) . . . . ?
C7 P1 P3 C5 -66.51(18) . . . . ?
P2 P1 P3 C5 47.63(14) . . . . ?
C7 P1 P3 C6 56.16(18) . . . . ?
P2 P1 P3 C6 170.29(13) . . . . ?
C7 P1 P3 C4 170.17(17) . . . . ?
P2 P1 P3 C4 -75.69(14) . . . . ?
P3 P1 C7 C9 37.8(3) . . . . ?
P2 P1 C7 C9 -70.8(3) . . . . ?
P3 P1 C7 C8 160.6(2) . . . . ?
P2 P1 C7 C8 52.0(3) . . . . ?
P3 P1 C7 C10 -85.0(2) . . . . ?
P2 P1 C7 C10 166.4(2) . . . . ?
O3 S1 C11 F3 -179.0(3) . . . . ?
O1 S1 C11 F3 62.0(3) . . . . ?
O2 S1 C11 F3 -58.6(3) . . . . ?
O3 S1 C11 F2 59.9(3) . . . . ?
O1 S1 C11 F2 -59.2(3) . . . . ?
O2 S1 C11 F2 -179.7(3) . . . . ?
O3 S1 C11 F1 -59.5(3) . . . . ?
O1 S1 C11 F1 -178.5(3) . . . . ?
O2 S1 C11 F1 60.9(3) . . . . ?
O6 S2 C12 F6 175.2(3) . . . . ?
O5 S2 C12 F6 53.9(4) . . . . ?
O4 S2 C12 F6 -63.9(4) . . . . ?
O6 S2 C12 F5 -61.5(4) . . . . ?
O5 S2 C12 F5 177.2(3) . . . . ?
O4 S2 C12 F5 59.4(3) . . . . ?
O6 S2 C12 F4 54.9(4) . . . . ?
O5 S2 C12 F4 -66.4(3) . . . . ?
O4 S2 C12 F4 175.8(3) . . . . ?



_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        26.60

_diffrn_measured_fraction_theta_full 0.988

_refine_diff_density_max         0.471

_refine_diff_density_min         -0.424

_refine_diff_density_rms         0.080

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

data_dal1078
_database_code_depnum_ccdc_archive 'CCDC 1418256'
_audit_update_record             
;
2015-08-12 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 N P3, 2(C F3 O3 S)'
_chemical_formula_sum            'C14 H32 F6 N O6 P3 S2'
_chemical_formula_weight         581.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   11.9037(6)
_cell_length_b                   13.9854(7)
_cell_length_c                   24.2752(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1515(5)
_cell_angle_gamma                90.00
_cell_volume                     3918.6(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1812
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35259
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.87
_diffrn_reflns_theta_max         27.51
_reflns_number_total             17964
_reflns_number_gt                17489
_reflns_threshold_expression     I>2σ(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)+(0.0565P)²+0.6512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_number_reflns         17964
_refine_ls_number_parameters     884
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
P11 P 0.23183(5) 0.53885(5) 0.41007(2) 0.02143(12) Uani 1 1 d . . .
P12 P 0.38364(6) 0.44699(5) 0.40814(3) 0.02700(13) Uani 1 1 d . . .
P13 P 0.08450(6) 0.43859(5) 0.40428(3) 0.02356(12) Uani 1 1 d . . .
N1 N 0.2601(2) 0.58840(14) 0.47398(8) 0.0245(4) Uani 1 1 d . . .
C11 C 0.4535(3) 0.3825(3) 0.47121(14) 0.0451(8) Uani 1 1 d . . .
H11A H 0.5221 0.3497 0.4650 0.054 Uiso 1 1 calc R . .
H11B H 0.3997 0.3354 0.4801 0.054 Uiso 1 1 calc R . .
H11C H 0.4769 0.4274 0.5030 0.054 Uiso 1 1 calc R . .
C12 C 0.4846(3) 0.5325(2) 0.39395(16) 0.0448(7) Uani 1 1 d . . .
H12A H 0.5523 0.4991 0.3872 0.054 Uiso 1 1 calc R . .
H12B H 0.5091 0.5753 0.4267 0.054 Uiso 1 1 calc R . .
H12C H 0.4477 0.5700 0.3603 0.054 Uiso 1 1 calc R . .
C13 C 0.3503(3) 0.3628(2) 0.35098(14) 0.0405(7) Uani 1 1 d . . .
H13A H 0.4222 0.3353 0.3452 0.049 Uiso 1 1 calc R . .
H13B H 0.3087 0.3953 0.3162 0.049 Uiso 1 1 calc R . .
H13C H 0.3016 0.3117 0.3602 0.049 Uiso 1 1 calc R . .
C14 C 0.0870(3) 0.3558(2) 0.46115(12) 0.0344(6) Uani 1 1 d . . .
H14A H 0.0150 0.3186 0.4528 0.041 Uiso 1 1 calc R . .
H14B H 0.0942 0.3911 0.4967 0.041 Uiso 1 1 calc R . .
H14C H 0.1532 0.3124 0.4650 0.041 Uiso 1 1 calc R . .
C15 C -0.0330(2) 0.5213(2) 0.39788(14) 0.0358(6) Uani 1 1 d . . .
H15A H -0.1060 0.4860 0.3925 0.043 Uiso 1 1 calc R . .
H15B H -0.0365 0.5632 0.3651 0.043 Uiso 1 1 calc R . .
H15C H -0.0208 0.5600 0.4325 0.043 Uiso 1 1 calc R . .
C16 C 0.0576(3) 0.3705(2) 0.33972(12) 0.0355(6) Uani 1 1 d . . .
H16A H -0.0200 0.3423 0.3323 0.043 Uiso 1 1 calc R . .
H16B H 0.1154 0.3195 0.3435 0.043 Uiso 1 1 calc R . .
H16C H 0.0627 0.4126 0.3081 0.043 Uiso 1 1 calc R . .
C17 C 0.2793(2) 0.5370(2) 0.52924(10) 0.0274(5) Uani 1 1 d . . .
H17 H 0.2794 0.4669 0.5209 0.033 Uiso 1 1 calc R . .
C18 C 0.2545(3) 0.69509(18) 0.47600(11) 0.0297(6) Uani 1 1 d . . .
H18 H 0.2835 0.7144 0.5167 0.036 Uiso 1 1 calc R . .
C171 C 0.3956(3) 0.5609(2) 0.56932(13) 0.0410(7) Uani 1 1 d . . .
H17A H 0.4578 0.5488 0.5502 0.049 Uiso 1 1 calc R . .
H17B H 0.4073 0.5209 0.6034 0.049 Uiso 1 1 calc R . .
H17C H 0.3965 0.6284 0.5802 0.049 Uiso 1 1 calc R . .
C172 C 0.1813(3) 0.5556(2) 0.55868(12) 0.0360(6) Uani 1 1 d . . .
H17D H 0.1068 0.5400 0.5326 0.043 Uiso 1 1 calc R . .
H17E H 0.1818 0.6231 0.5695 0.043 Uiso 1 1 calc R . .
H17F H 0.1926 0.5155 0.5927 0.043 Uiso 1 1 calc R . .
C181 C 0.3342(3) 0.7411(2) 0.44316(14) 0.0423(7) Uani 1 1 d . . .
H18A H 0.4127 0.7156 0.4569 0.051 Uiso 1 1 calc R . .
H18B H 0.3353 0.8105 0.4489 0.051 Uiso 1 1 calc R . .
H18C H 0.3057 0.7268 0.4026 0.051 Uiso 1 1 calc R . .
C182 C 0.1307(3) 0.7327(2) 0.45602(14) 0.0378(7) Uani 1 1 d . . .
H18D H 0.0816 0.7019 0.4779 0.045 Uiso 1 1 calc R . .
H18E H 0.1008 0.7183 0.4156 0.045 Uiso 1 1 calc R . .
H18F H 0.1303 0.8021 0.4618 0.045 Uiso 1 1 calc R . .
P21 P 0.19616(6) 0.04229(5) 0.25656(3) 0.02227(12) Uani 1 1 d . . .
P22 P 0.34312(6) -0.05542(5) 0.25694(3) 0.02524(12) Uani 1 1 d . . .
P23 P 0.05049(5) -0.05184(5) 0.26524(3) 0.02538(13) Uani 1 1 d . . .
N2 N 0.1595(2) 0.08977(15) 0.19199(8) 0.0255(4) Uani 1 1 d . . .
C21 C 0.3347(3) -0.1365(2) 0.19905(13) 0.0432(8) Uani 1 1 d . . .
H21A H 0.4074 -0.1723 0.2048 0.052 Uiso 1 1 calc R . .
H21B H 0.3216 -0.1004 0.1634 0.052 Uiso 1 1 calc R . .
H21C H 0.2704 -0.1811 0.1972 0.052 Uiso 1 1 calc R . .
C22 C 0.4572(2) 0.0280(2) 0.25811(15) 0.0424(7) Uani 1 1 d . . .
H22A H 0.5315 -0.0060 0.2660 0.051 Uiso 1 1 calc R . .
H22B H 0.4587 0.0757 0.2878 0.051 Uiso 1 1 calc R . .
H22C H 0.4441 0.0599 0.2212 0.051 Uiso 1 1 calc R . .
C23 C 0.3781(3) -0.1233(2) 0.32146(11) 0.0307(6) Uani 1 1 d . . .
H23A H 0.4604 -0.1407 0.3305 0.037 Uiso 1 1 calc R . .
H23B H 0.3309 -0.1815 0.3167 0.037 Uiso 1 1 calc R . .
H23C H 0.3624 -0.0849 0.3525 0.037 Uiso 1 1 calc R . .
C24 C -0.0127(3) -0.1318(2) 0.20852(12) 0.0376(6) Uani 1 1 d . . .
H24A H -0.0805 -0.1631 0.2168 0.045 Uiso 1 1 calc R . .
H24B H 0.0443 -0.1803 0.2048 0.045 Uiso 1 1 calc R . .
H24C H -0.0366 -0.0958 0.1729 0.045 Uiso 1 1 calc R . .
C25 C -0.0557(3) 0.0344(2) 0.27438(14) 0.0402(7) Uani 1 1 d . . .
H25A H -0.1242 0.0010 0.2802 0.048 Uiso 1 1 calc R . .
H25B H -0.0778 0.0746 0.2404 0.048 Uiso 1 1 calc R . .
H25C H -0.0228 0.0745 0.3075 0.048 Uiso 1 1 calc R . .
C26 C 0.0906(3) -0.1211(2) 0.32884(12) 0.0331(6) Uani 1 1 d . . .
H26A H 0.0206 -0.1428 0.3396 0.040 Uiso 1 1 calc R . .
H26B H 0.1373 -0.0818 0.3594 0.040 Uiso 1 1 calc R . .
H26C H 0.1359 -0.1766 0.3224 0.040 Uiso 1 1 calc R . .
C27 C 0.1202(2) 0.03703(18) 0.13742(9) 0.0242(5) Uani 1 1 d . . .
H27 H 0.1239 -0.0328 0.1465 0.029 Uiso 1 1 calc R . .
C28 C 0.1582(3) 0.19764(18) 0.18865(11) 0.0304(6) Uani 1 1 d . . .
H28 H 0.1402 0.2152 0.1475 0.036 Uiso 1 1 calc R . .
C271 C 0.1992(3) 0.0552(2) 0.09773(12) 0.0341(6) Uani 1 1 d . . .
H27A H 0.2793 0.0396 0.1173 0.041 Uiso 1 1 calc R . .
H27B H 0.1944 0.1227 0.0865 0.041 Uiso 1 1 calc R . .
H27C H 0.1748 0.0150 0.0638 0.041 Uiso 1 1 calc R . .
C272 C -0.0045(3) 0.0608(2) 0.10821(12) 0.0318(6) Uani 1 1 d . . .
H27D H -0.0539 0.0487 0.1344 0.038 Uiso 1 1 calc R . .
H27E H -0.0300 0.0207 0.0743 0.038 Uiso 1 1 calc R . .
H27F H -0.0102 0.1283 0.0971 0.038 Uiso 1 1 calc R . .
C281 C 0.2758(3) 0.2379(2) 0.21580(15) 0.0448(8) Uani 1 1 d . . .
H28A H 0.3338 0.2084 0.1986 0.054 Uiso 1 1 calc R . .
H28B H 0.2951 0.2243 0.2566 0.054 Uiso 1 1 calc R . .
H28C H 0.2752 0.3072 0.2098 0.054 Uiso 1 1 calc R . .
C282 C 0.0633(3) 0.2404(2) 0.21312(14) 0.0430(7) Uani 1 1 d . . .
H28D H 0.0650 0.3102 0.2103 0.052 Uiso 1 1 calc R . .
H28E H 0.0760 0.2218 0.2531 0.052 Uiso 1 1 calc R . .
H28F H -0.0123 0.2166 0.1918 0.052 Uiso 1 1 calc R . .
P31 P 0.57847(6) 0.53772(4) 0.07710(2) 0.02205(12) Uani 1 1 d . . .
P32 P 0.42140(6) 0.44741(5) 0.06878(3) 0.02536(13) Uani 1 1 d . . .
P33 P 0.71943(6) 0.43373(5) 0.07733(3) 0.02507(13) Uani 1 1 d . . .
N3 N 0.6060(2) 0.58621(14) 0.14118(8) 0.0252(4) Uani 1 1 d . . .
C31 C 0.4058(3) 0.3810(2) 0.12959(12) 0.0366(7) Uani 1 1 d . . .
H31A H 0.3284 0.3523 0.1217 0.044 Uiso 1 1 calc R . .
H31B H 0.4161 0.4239 0.1623 0.044 Uiso 1 1 calc R . .
H31C H 0.4645 0.3304 0.1380 0.044 Uiso 1 1 calc R . .
C32 C 0.3086(3) 0.5347(2) 0.05049(15) 0.0410(7) Uani 1 1 d . . .
H32A H 0.2331 0.5026 0.0427 0.049 Uiso 1 1 calc R . .
H32B H 0.3160 0.5697 0.0166 0.049 Uiso 1 1 calc R . .
H32C H 0.3147 0.5794 0.0821 0.049 Uiso 1 1 calc R . .
C33 C 0.4035(3) 0.3650(2) 0.01037(12) 0.0343(6) Uani 1 1 d . . .
H33A H 0.3239 0.3407 0.0006 0.041 Uiso 1 1 calc R . .
H33B H 0.4575 0.3115 0.0213 0.041 Uiso 1 1 calc R . .
H33C H 0.4194 0.3978 -0.0226 0.041 Uiso 1 1 calc R . .
C34 C 0.7575(3) 0.3456(2) 0.13259(13) 0.0380(7) Uani 1 1 d . . .
H34A H 0.8180 0.3037 0.1250 0.046 Uiso 1 1 calc R . .
H34B H 0.6890 0.3074 0.1336 0.046 Uiso 1 1 calc R . .
H34C H 0.7862 0.3776 0.1693 0.046 Uiso 1 1 calc R . .
C35 C 0.8385(3) 0.5127(2) 0.08094(18) 0.0482(9) Uani 1 1 d . . .
H35A H 0.9066 0.4758 0.0776 0.058 Uiso 1 1 calc R . .
H35B H 0.8558 0.5466 0.1174 0.058 Uiso 1 1 calc R . .
H35C H 0.8187 0.5590 0.0498 0.058 Uiso 1 1 calc R . .
C36 C 0.6917(3) 0.3714(2) 0.01118(12) 0.0327(6) Uani 1 1 d . . .
H36A H 0.7651 0.3490 0.0043 0.039 Uiso 1 1 calc R . .
H36B H 0.6535 0.4145 -0.0195 0.039 Uiso 1 1 calc R . .
H36C H 0.6413 0.3164 0.0125 0.039 Uiso 1 1 calc R . .
C37 C 0.6294(2) 0.53415(18) 0.19678(10) 0.0254(5) Uani 1 1 d . . .
H37 H 0.6201 0.4642 0.1883 0.031 Uiso 1 1 calc R . .
C38 C 0.6135(3) 0.69398(18) 0.14359(11) 0.0299(5) Uani 1 1 d . . .
H38 H 0.6246 0.7128 0.1843 0.036 Uiso 1 1 calc R . .
C371 C 0.5418(3) 0.5620(2) 0.23123(12) 0.0329(6) Uani 1 1 d . . .
H37A H 0.4629 0.5505 0.2083 0.039 Uiso 1 1 calc R . .
H37B H 0.5509 0.6299 0.2414 0.039 Uiso 1 1 calc R . .
H37C H 0.5557 0.5233 0.2659 0.039 Uiso 1 1 calc R . .
C372 C 0.7535(3) 0.5506(2) 0.23085(12) 0.0336(6) Uani 1 1 d . . .
H37D H 0.8073 0.5323 0.2079 0.040 Uiso 1 1 calc R . .
H37E H 0.7687 0.5118 0.2655 0.040 Uiso 1 1 calc R . .
H37F H 0.7643 0.6184 0.2411 0.040 Uiso 1 1 calc R . .
C381 C 0.5011(3) 0.7394(2) 0.11086(14) 0.0379(7) Uani 1 1 d . . .
H38A H 0.5084 0.8092 0.1131 0.045 Uiso 1 1 calc R . .
H38B H 0.4376 0.7191 0.1274 0.045 Uiso 1 1 calc R . .
H38C H 0.4847 0.7193 0.0710 0.045 Uiso 1 1 calc R . .
C382 C 0.7168(3) 0.7313(2) 0.12446(14) 0.0364(6) Uani 1 1 d . . .
H38D H 0.7874 0.7004 0.1466 0.044 Uiso 1 1 calc R . .
H38E H 0.7228 0.8006 0.1303 0.044 Uiso 1 1 calc R . .
H38F H 0.7072 0.7170 0.0840 0.044 Uiso 1 1 calc R . .
S1 S 0.71237(6) 0.32708(5) 0.36219(3) 0.02965(14) Uani 1 1 d . . .
F11 F 0.7616(3) 0.2846(2) 0.26647(11) 0.0802(9) Uani 1 1 d . . .
F12 F 0.6896(3) 0.16822(16) 0.30354(11) 0.0700(7) Uani 1 1 d . . .
F13 F 0.5800(3) 0.2834(3) 0.26317(12) 0.0919(10) Uani 1 1 d . . .
O11 O 0.6229(2) 0.29517(18) 0.38840(11) 0.0478(6) Uani 1 1 d . . .
O12 O 0.7031(2) 0.42531(16) 0.34459(10) 0.0458(5) Uani 1 1 d . . .
O13 O 0.8265(2) 0.29690(17) 0.39078(11) 0.0441(5) Uani 1 1 d . . .
C1 C 0.6838(4) 0.2616(3) 0.29525(14) 0.0486(8) Uani 1 1 d . . .
S2 S 0.04736(6) 0.33357(5) 0.03153(3) 0.02934(14) Uani 1 1 d . . .
F21 F 0.0028(3) 0.17697(16) -0.02855(10) 0.0674(7) Uani 1 1 d . . .
F22 F -0.1067(2) 0.2962(2) -0.06313(9) 0.0649(7) Uani 1 1 d . . .
F23 F 0.0679(2) 0.2905(2) -0.07032(10) 0.0696(7) Uani 1 1 d . . .
O21 O 0.0366(2) 0.43246(16) 0.01535(10) 0.0484(6) Uani 1 1 d . . .
O22 O 0.1639(2) 0.30001(18) 0.05274(11) 0.0453(5) Uani 1 1 d . . .
O23 O -0.0333(2) 0.30199(16) 0.06328(9) 0.0373(5) Uani 1 1 d . . .
C2 C 0.0005(3) 0.2697(2) -0.03594(14) 0.0411(7) Uani 1 1 d . . .
S3 S 0.28593(6) 0.33043(5) 0.69795(3) 0.02900(13) Uani 1 1 d . . .
F31 F 0.2708(3) 0.17326(15) 0.63822(10) 0.0668(7) Uani 1 1 d . . .
F32 F 0.1550(2) 0.2844(2) 0.59861(10) 0.0747(8) Uani 1 1 d . . .
F33 F 0.3345(3) 0.2949(2) 0.60069(10) 0.0754(8) Uani 1 1 d . . .
O31 O 0.2764(2) 0.42972(16) 0.68146(9) 0.0479(6) Uani 1 1 d . . .
O32 O 0.4010(2) 0.30180(16) 0.72727(9) 0.0394(5) Uani 1 1 d . . .
O33 O 0.1964(2) 0.29588(19) 0.72290(11) 0.0476(6) Uani 1 1 d . . .
C3 C 0.2601(3) 0.2660(2) 0.63062(13) 0.0433(7) Uani 1 1 d . . .
S4 S 0.16909(8) 0.60311(7) 0.25516(4) 0.04509(18) Uani 1 1 d . . .
F41 F 0.0485(3) 0.6410(2) 0.15421(12) 0.0925(11) Uani 1 1 d . . .
F42 F 0.2364(3) 0.6286(3) 0.16293(13) 0.1030(11) Uani 1 1 d . . .
F43 F 0.1245(5) 0.5032(2) 0.16168(14) 0.1261(17) Uani 1 1 d . . .
O41 O 0.2681(3) 0.5415(3) 0.27443(13) 0.0860(11) Uani 1 1 d . . .
O42 O 0.0637(4) 0.5675(3) 0.26618(18) 0.0995(13) Uani 1 1 d . . .
O43 O 0.1936(3) 0.7014(2) 0.26436(12) 0.0687(8) Uani 1 1 d . . .
C4 C 0.1452(5) 0.5921(3) 0.17907(17) 0.0665(12) Uani 1 1 d . . .
S5 S 0.53872(6) 0.10446(5) 0.09395(3) 0.03218(14) Uani 1 1 d . . .
F51 F 0.6465(3) -0.00600(19) 0.17705(11) 0.0754(7) Uani 1 1 d . . .
F52 F 0.7423(2) 0.11991(16) 0.16496(11) 0.0665(7) Uani 1 1 d . . .
F53 F 0.72597(19) 0.00076(17) 0.10773(11) 0.0645(6) Uani 1 1 d . . .
O51 O 0.5813(3) 0.16399(19) 0.05606(11) 0.0571(7) Uani 1 1 d . . .
O52 O 0.4751(2) 0.02255(17) 0.06821(11) 0.0478(6) Uani 1 1 d . . .
O53 O 0.4890(3) 0.1544(2) 0.13428(12) 0.0617(8) Uani 1 1 d . . .
C5 C 0.6701(3) 0.0528(2) 0.13928(14) 0.0414(7) Uani 1 1 d . . .
S6 S 0.26380(10) 0.10844(6) 0.42975(4) 0.0516(2) Uani 1 1 d . . .
F61 F 0.1336(3) 0.13128(16) 0.50130(10) 0.0668(7) Uani 1 1 d . . .
F62 F 0.2470(4) 0.0111(3) 0.51813(16) 0.1274(16) Uani 1 1 d . . .
F63 F 0.1012(3) 0.0047(2) 0.45239(18) 0.1137(14) Uani 1 1 d . . .
O61 O 0.3051(2) 0.02656(18) 0.40704(12) 0.0530(6) Uani 1 1 d . . .
O62 O 0.1805(6) 0.1594(4) 0.38973(18) 0.164(3) Uani 1 1 d . . .
O63 O 0.3485(5) 0.1648(4) 0.4669(3) 0.156(3) Uani 1 1 d . . .
C6 C 0.1840(3) 0.0631(2) 0.47845(16) 0.0469(8) 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
P11 N1 1.657(2) . ?
P11 P13 2.2229(9) . ?
P11 P12 2.2271(9) . ?
P12 C12 1.787(3) . ?
P12 C13 1.789(3) . ?
P12 C11 1.796(3) . ?
P13 C15 1.792(3) . ?
P13 C16 1.794(3) . ?
P13 C14 1.797(3) . ?
N1 C17 1.490(3) . ?
N1 C18 1.495(3) . ?
C17 C171 1.521(4) . ?
C17 C172 1.533(4) . ?
C18 C181 1.523(4) . ?
C18 C182 1.528(4) . ?
P21 N2 1.660(2) . ?
P21 P22 2.2181(9) . ?
P21 P23 2.2277(9) . ?
P22 C22 1.785(3) . ?
P22 C21 1.789(3) . ?
P22 C23 1.791(3) . ?
P23 C26 1.786(3) . ?
P23 C24 1.791(3) . ?
P23 C25 1.799(3) . ?
N2 C27 1.488(3) . ?
N2 C28 1.511(3) . ?
C27 C272 1.518(4) . ?
C27 C271 1.523(4) . ?
C28 C281 1.503(5) . ?
C28 C282 1.522(4) . ?
P31 N3 1.655(2) . ?
P31 P33 2.2196(9) . ?
P31 P32 2.2242(9) . ?
P32 C32 1.788(3) . ?
P32 C31 1.792(3) . ?
P32 C33 1.799(3) . ?
P33 C35 1.782(3) . ?
P33 C36 1.786(3) . ?
P33 C34 1.796(3) . ?
N3 C37 1.499(3) . ?
N3 C38 1.510(3) . ?
C37 C372 1.524(4) . ?
C37 C371 1.538(4) . ?
C38 C382 1.509(4) . ?
C38 C381 1.519(4) . ?
S1 O13 1.429(2) . ?
S1 O12 1.435(2) . ?
S1 O11 1.439(2) . ?
S1 C1 1.823(4) . ?
F11 C1 1.329(5) . ?
F12 C1 1.321(4) . ?
F13 C1 1.325(5) . ?
S2 O21 1.435(2) . ?
S2 O22 1.435(2) . ?
S2 O23 1.439(2) . ?
S2 C2 1.829(3) . ?
F21 C2 1.309(4) . ?
F22 C2 1.338(4) . ?
F23 C2 1.323(4) . ?
S3 O33 1.432(2) . ?
S3 O32 1.437(2) . ?
S3 O31 1.442(2) . ?
S3 C3 1.826(3) . ?
F31 C3 1.311(4) . ?
F32 C3 1.327(4) . ?
F33 C3 1.337(4) . ?
S4 O43 1.412(3) . ?
S4 O42 1.434(4) . ?
S4 O41 1.443(3) . ?
S4 C4 1.805(4) . ?
F41 C4 1.348(6) . ?
F42 C4 1.342(7) . ?
F43 C4 1.318(5) . ?
S5 O51 1.423(3) . ?
S5 O52 1.430(2) . ?
S5 O53 1.442(3) . ?
S5 C5 1.827(3) . ?
F51 C5 1.312(4) . ?
F52 C5 1.321(4) . ?
F53 C5 1.344(4) . ?
S6 O62 1.401(4) . ?
S6 O61 1.410(2) . ?
S6 O63 1.416(4) . ?
S6 C6 1.803(4) . ?
F61 C6 1.319(4) . ?
F62 C6 1.291(5) . ?
F63 C6 1.317(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P11 P13 107.42(9) . . ?
N1 P11 P12 106.31(9) . . ?
P13 P11 P12 105.46(3) . . ?
C12 P12 C13 108.85(17) . . ?
C12 P12 C11 107.88(18) . . ?
C13 P12 C11 107.44(17) . . ?
C12 P12 P11 101.85(11) . . ?
C13 P12 P11 111.62(11) . . ?
C11 P12 P11 118.73(11) . . ?
C15 P13 C16 107.34(15) . . ?
C15 P13 C14 110.42(16) . . ?
C16 P13 C14 107.16(14) . . ?
C15 P13 P11 100.67(10) . . ?
C16 P13 P11 111.07(11) . . ?
C14 P13 P11 119.56(10) . . ?
C17 N1 C18 116.8(2) . . ?
C17 N1 P11 126.34(17) . . ?
C18 N1 P11 116.59(16) . . ?
N1 C17 C171 112.7(2) . . ?
N1 C17 C172 111.8(2) . . ?
C171 C17 C172 110.0(2) . . ?
N1 C18 C181 111.5(2) . . ?
N1 C18 C182 112.4(2) . . ?
C181 C18 C182 111.3(2) . . ?
N2 P21 P22 105.97(9) . . ?
N2 P21 P23 107.15(9) . . ?
P22 P21 P23 105.48(3) . . ?
C22 P22 C21 108.85(18) . . ?
C22 P22 C23 108.60(15) . . ?
C21 P22 C23 107.89(15) . . ?
C22 P22 P21 101.17(11) . . ?
C21 P22 P21 119.62(12) . . ?
C23 P22 P21 110.17(10) . . ?
C26 P23 C24 107.44(15) . . ?
C26 P23 C25 107.70(15) . . ?
C24 P23 C25 109.74(16) . . ?
C26 P23 P21 110.63(11) . . ?
C24 P23 P21 119.13(11) . . ?
C25 P23 P21 101.65(11) . . ?
C27 N2 C28 116.8(2) . . ?
C27 N2 P21 126.54(17) . . ?
C28 N2 P21 116.56(16) . . ?
N2 C27 C272 111.5(2) . . ?
N2 C27 C271 111.9(2) . . ?
C272 C27 C271 110.7(2) . . ?
C281 C28 N2 110.7(2) . . ?
C281 C28 C282 112.5(2) . . ?
N2 C28 C282 111.7(2) . . ?
N3 P31 P33 106.87(9) . . ?
N3 P31 P32 106.68(9) . . ?
P33 P31 P32 104.26(3) . . ?
C32 P32 C31 109.61(16) . . ?
C32 P32 C33 107.73(15) . . ?
C31 P32 C33 107.50(15) . . ?
C32 P32 P31 101.46(11) . . ?
C31 P32 P31 118.27(10) . . ?
C33 P32 P31 111.73(10) . . ?
C35 P33 C36 108.46(16) . . ?
C35 P33 C34 109.63(18) . . ?
C36 P33 C34 107.09(14) . . ?
C35 P33 P31 100.72(11) . . ?
C36 P33 P31 110.14(10) . . ?
C34 P33 P31 120.27(11) . . ?
C37 N3 C38 116.99(19) . . ?
C37 N3 P31 126.74(17) . . ?
C38 N3 P31 116.21(16) . . ?
N3 C37 C372 111.0(2) . . ?
N3 C37 C371 111.4(2) . . ?
C372 C37 C371 111.3(2) . . ?
C382 C38 N3 112.2(2) . . ?
C382 C38 C381 112.0(2) . . ?
N3 C38 C381 111.2(2) . . ?
O13 S1 O12 114.98(15) . . ?
O13 S1 O11 114.33(14) . . ?
O12 S1 O11 114.65(15) . . ?
O13 S1 C1 103.44(18) . . ?
O12 S1 C1 103.36(15) . . ?
O11 S1 C1 103.98(18) . . ?
F12 C1 F13 108.8(3) . . ?
F12 C1 F11 107.6(4) . . ?
F13 C1 F11 107.8(3) . . ?
F12 C1 S1 111.7(2) . . ?
F13 C1 S1 110.6(3) . . ?
F11 C1 S1 110.2(3) . . ?
O21 S2 O22 115.29(16) . . ?
O21 S2 O23 114.57(14) . . ?
O22 S2 O23 114.83(13) . . ?
O21 S2 C2 103.78(15) . . ?
O22 S2 C2 102.57(15) . . ?
O23 S2 C2 103.45(15) . . ?
F21 C2 F23 108.0(3) . . ?
F21 C2 F22 109.1(3) . . ?
F23 C2 F22 106.3(3) . . ?
F21 C2 S2 111.7(2) . . ?
F23 C2 S2 111.0(3) . . ?
F22 C2 S2 110.6(2) . . ?
O33 S3 O32 114.46(14) . . ?
O33 S3 O31 115.23(16) . . ?
O32 S3 O31 113.98(15) . . ?
O33 S3 C3 103.43(17) . . ?
O32 S3 C3 103.71(15) . . ?
O31 S3 C3 104.03(15) . . ?
F31 C3 F32 108.6(3) . . ?
F31 C3 F33 108.7(3) . . ?
F32 C3 F33 106.1(3) . . ?
F31 C3 S3 111.9(2) . . ?
F32 C3 S3 110.9(3) . . ?
F33 C3 S3 110.4(2) . . ?
O43 S4 O42 117.7(3) . . ?
O43 S4 O41 114.2(2) . . ?
O42 S4 O41 114.5(3) . . ?
O43 S4 C4 102.7(2) . . ?
O42 S4 C4 103.6(3) . . ?
O41 S4 C4 101.1(2) . . ?
F43 C4 F42 111.5(5) . . ?
F43 C4 F41 105.3(4) . . ?
F42 C4 F41 109.9(4) . . ?
F43 C4 S4 112.2(3) . . ?
F42 C4 S4 109.3(3) . . ?
F41 C4 S4 108.6(4) . . ?
O51 S5 O52 114.87(16) . . ?
O51 S5 O53 115.2(2) . . ?
O52 S5 O53 115.03(18) . . ?
O51 S5 C5 103.48(17) . . ?
O52 S5 C5 103.31(15) . . ?
O53 S5 C5 102.46(16) . . ?
F51 C5 F52 109.9(3) . . ?
F51 C5 F53 106.2(3) . . ?
F52 C5 F53 107.4(3) . . ?
F51 C5 S5 111.7(3) . . ?
F52 C5 S5 111.4(2) . . ?
F53 C5 S5 109.9(2) . . ?
O62 S6 O61 113.4(2) . . ?
O62 S6 O63 115.6(4) . . ?
O61 S6 O63 116.0(3) . . ?
O62 S6 C6 103.7(3) . . ?
O61 S6 C6 105.11(17) . . ?
O63 S6 C6 100.7(2) . . ?
F62 C6 F63 103.8(4) . . ?
F62 C6 F61 109.6(4) . . ?
F63 C6 F61 106.7(3) . . ?
F62 C6 S6 112.6(3) . . ?
F63 C6 S6 110.8(3) . . ?
F61 C6 S6 112.9(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
N1 P11 P12 C12 -80.86(15) . . . . ?
P13 P11 P12 C12 165.27(13) . . . . ?
N1 P11 P12 C13 163.14(15) . . . . ?
P13 P11 P12 C13 49.28(13) . . . . ?
N1 P11 P12 C11 37.34(18) . . . . ?
P13 P11 P12 C11 -76.53(16) . . . . ?
N1 P11 P13 C15 73.34(14) . . . . ?
P12 P11 P13 C15 -173.56(11) . . . . ?
N1 P11 P13 C16 -173.24(14) . . . . ?
P12 P11 P13 C16 -60.14(12) . . . . ?
N1 P11 P13 C14 -47.65(15) . . . . ?
P12 P11 P13 C14 65.44(13) . . . . ?
P13 P11 N1 C17 51.4(2) . . . . ?
P12 P11 N1 C17 -61.1(2) . . . . ?
P13 P11 N1 C18 -122.4(2) . . . . ?
P12 P11 N1 C18 125.1(2) . . . . ?
C18 N1 C17 C171 -63.0(3) . . . . ?
P11 N1 C17 C171 123.2(2) . . . . ?
C18 N1 C17 C172 61.4(3) . . . . ?
P11 N1 C17 C172 -112.4(2) . . . . ?
C17 N1 C18 C181 129.8(3) . . . . ?
P11 N1 C18 C181 -55.8(3) . . . . ?
C17 N1 C18 C182 -104.4(3) . . . . ?
P11 N1 C18 C182 70.0(3) . . . . ?
N2 P21 P22 C22 72.95(15) . . . . ?
P23 P21 P22 C22 -173.62(12) . . . . ?
N2 P21 P22 C21 -46.46(17) . . . . ?
P23 P21 P22 C21 66.97(15) . . . . ?
N2 P21 P22 C23 -172.29(13) . . . . ?
P23 P21 P22 C23 -58.86(11) . . . . ?
N2 P21 P23 C26 170.79(14) . . . . ?
P22 P21 P23 C26 58.19(12) . . . . ?
N2 P21 P23 C24 45.60(16) . . . . ?
P22 P21 P23 C24 -67.01(13) . . . . ?
N2 P21 P23 C25 -75.05(14) . . . . ?
P22 P21 P23 C25 172.35(11) . . . . ?
P22 P21 N2 C27 59.7(2) . . . . ?
P23 P21 N2 C27 -52.6(2) . . . . ?
P22 P21 N2 C28 -124.7(2) . . . . ?
P23 P21 N2 C28 123.0(2) . . . . ?
C28 N2 C27 C272 -60.9(3) . . . . ?
P21 N2 C27 C272 114.7(2) . . . . ?
C28 N2 C27 C271 63.6(3) . . . . ?
P21 N2 C27 C271 -120.9(2) . . . . ?
C27 N2 C28 C281 -124.5(3) . . . . ?
P21 N2 C28 C281 59.5(3) . . . . ?
C27 N2 C28 C282 109.3(3) . . . . ?
P21 N2 C28 C282 -66.7(3) . . . . ?
N3 P31 P32 C32 81.49(14) . . . . ?
P33 P31 P32 C32 -165.64(12) . . . . ?
N3 P31 P32 C31 -38.38(16) . . . . ?
P33 P31 P32 C31 74.50(13) . . . . ?
N3 P31 P32 C33 -163.97(14) . . . . ?
P33 P31 P32 C33 -51.10(12) . . . . ?
N3 P31 P33 C35 -69.68(16) . . . . ?
P32 P31 P33 C35 177.58(14) . . . . ?
N3 P31 P33 C36 175.94(14) . . . . ?
P32 P31 P33 C36 63.21(12) . . . . ?
N3 P31 P33 C34 50.74(16) . . . . ?
P32 P31 P33 C34 -61.99(13) . . . . ?
P33 P31 N3 C37 -52.4(2) . . . . ?
P32 P31 N3 C37 58.7(2) . . . . ?
P33 P31 N3 C38 124.6(2) . . . . ?
P32 P31 N3 C38 -124.3(2) . . . . ?
C38 N3 C37 C372 -63.2(3) . . . . ?
P31 N3 C37 C372 113.7(2) . . . . ?
C38 N3 C37 C371 61.4(3) . . . . ?
P31 N3 C37 C371 -121.7(2) . . . . ?
C37 N3 C38 C382 110.4(3) . . . . ?
P31 N3 C38 C382 -66.9(3) . . . . ?
C37 N3 C38 C381 -123.3(3) . . . . ?
P31 N3 C38 C381 59.3(3) . . . . ?
O13 S1 C1 F12 59.4(3) . . . . ?
O12 S1 C1 F12 179.7(3) . . . . ?
O11 S1 C1 F12 -60.3(3) . . . . ?
O13 S1 C1 F13 -179.2(3) . . . . ?
O12 S1 C1 F13 -59.0(3) . . . . ?
O11 S1 C1 F13 61.1(3) . . . . ?
O13 S1 C1 F11 -60.0(3) . . . . ?
O12 S1 C1 F11 60.2(3) . . . . ?
O11 S1 C1 F11 -179.8(3) . . . . ?
O21 S2 C2 F21 -178.6(3) . . . . ?
O22 S2 C2 F21 61.0(3) . . . . ?
O23 S2 C2 F21 -58.7(3) . . . . ?
O21 S2 C2 F23 60.8(3) . . . . ?
O22 S2 C2 F23 -59.6(3) . . . . ?
O23 S2 C2 F23 -179.3(2) . . . . ?
O21 S2 C2 F22 -56.9(3) . . . . ?
O22 S2 C2 F22 -177.3(3) . . . . ?
O23 S2 C2 F22 63.0(3) . . . . ?
O33 S3 C3 F31 -62.0(3) . . . . ?
O32 S3 C3 F31 57.8(3) . . . . ?
O31 S3 C3 F31 177.2(3) . . . . ?
O33 S3 C3 F32 59.4(3) . . . . ?
O32 S3 C3 F32 179.2(3) . . . . ?
O31 S3 C3 F32 -61.3(3) . . . . ?
O33 S3 C3 F33 176.7(3) . . . . ?
O32 S3 C3 F33 -63.5(3) . . . . ?
O31 S3 C3 F33 56.0(3) . . . . ?
O43 S4 C4 F43 177.8(5) . . . . ?
O42 S4 C4 F43 -59.2(5) . . . . ?
O41 S4 C4 F43 59.6(5) . . . . ?
O43 S4 C4 F42 53.6(4) . . . . ?
O42 S4 C4 F42 176.6(4) . . . . ?
O41 S4 C4 F42 -64.6(4) . . . . ?
O43 S4 C4 F41 -66.2(4) . . . . ?
O42 S4 C4 F41 56.7(4) . . . . ?
O41 S4 C4 F41 175.6(4) . . . . ?
O51 S5 C5 F51 -179.3(3) . . . . ?
O52 S5 C5 F51 -59.2(3) . . . . ?
O53 S5 C5 F51 60.6(3) . . . . ?
O51 S5 C5 F52 57.3(3) . . . . ?
O52 S5 C5 F52 177.4(3) . . . . ?
O53 S5 C5 F52 -62.8(3) . . . . ?
O51 S5 C5 F53 -61.6(3) . . . . ?
O52 S5 C5 F53 58.5(3) . . . . ?
O53 S5 C5 F53 178.3(2) . . . . ?
O62 S6 C6 F62 178.2(4) . . . . ?
O61 S6 C6 F62 58.9(4) . . . . ?
O63 S6 C6 F62 -62.0(4) . . . . ?
O62 S6 C6 F63 62.4(4) . . . . ?
O61 S6 C6 F63 -56.9(3) . . . . ?
O63 S6 C6 F63 -177.7(4) . . . . ?
O62 S6 C6 F61 -57.2(4) . . . . ?
O61 S6 C6 F61 -176.4(3) . . . . ?
O63 S6 C6 F61 62.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.052

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

data_dal1079
_database_code_depnum_ccdc_archive 'CCDC 1418257'
_audit_update_record             
;
2015-08-12 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H29 F6 O6 P3 S2'
_chemical_formula_weight         564.40

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   Pba2

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

_cell_length_a                   16.7757(19)
_cell_length_b                   22.426(3)
_cell_length_c                   6.3922(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2404.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9733
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_T_max  0.8787
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47736
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5523
_reflns_number_gt                5472
_reflns_threshold_expression     I>2σ(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)+(0.0344P)²+0.8012P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881. 2511 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_number_reflns         5523
_refine_ls_number_parameters     286
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
P1 P 0.38865(2) 0.372459(16) 0.00523(6) 0.02126(8) Uani 1 1 d . . .
P2 P 0.28243(2) 0.339455(17) 0.16986(6) 0.02141(8) Uani 1 1 d . . .
P3 P 0.25229(2) 0.257760(16) -0.00274(7) 0.02188(8) Uani 1 1 d . . .
C1 C 0.41200(11) 0.44268(7) 0.1223(3) 0.0310(3) Uani 1 1 d . . .
H1A H 0.4659 0.4548 0.0809 0.037 Uiso 1 1 calc R . .
H1B H 0.4094 0.4390 0.2749 0.037 Uiso 1 1 calc R . .
H1C H 0.3736 0.4727 0.0752 0.037 Uiso 1 1 calc R . .
C2 C 0.46614(9) 0.32101(8) 0.0689(3) 0.0348(4) Uani 1 1 d . . .
H2A H 0.5179 0.3383 0.0317 0.042 Uiso 1 1 calc R . .
H2B H 0.4582 0.2839 -0.0093 0.042 Uiso 1 1 calc R . .
H2C H 0.4649 0.3126 0.2193 0.042 Uiso 1 1 calc R . .
C3 C 0.38782(10) 0.38221(8) -0.2731(3) 0.0305(3) Uani 1 1 d . . .
H3A H 0.4365 0.4030 -0.3166 0.037 Uiso 1 1 calc R . .
H3B H 0.3412 0.4059 -0.3134 0.037 Uiso 1 1 calc R . .
H3C H 0.3853 0.3431 -0.3413 0.037 Uiso 1 1 calc R . .
C4 C 0.19819(9) 0.39180(7) 0.1253(3) 0.0263(3) Uani 1 1 d . . .
H4 H 0.1485 0.3697 0.1639 0.032 Uiso 1 1 calc R . .
C5 C 0.18512(11) 0.41581(8) -0.0949(3) 0.0302(3) Uani 1 1 d . . .
H5A H 0.1743 0.3823 -0.1915 0.036 Uiso 1 1 calc R . .
H5B H 0.2340 0.4364 -0.1434 0.036 Uiso 1 1 calc R . .
C6 C 0.11451(12) 0.45971(9) -0.0984(3) 0.0416(4) Uani 1 1 d . . .
H6A H 0.1082 0.4761 -0.2413 0.050 Uiso 1 1 calc R . .
H6B H 0.0649 0.4382 -0.0617 0.050 Uiso 1 1 calc R . .
C7 C 0.12747(13) 0.51041(9) 0.0546(3) 0.0435(5) Uani 1 1 d . . .
H7A H 0.0812 0.5378 0.0504 0.052 Uiso 1 1 calc R . .
H7B H 0.1755 0.5333 0.0138 0.052 Uiso 1 1 calc R . .
C8 C 0.13787(12) 0.48630(10) 0.2755(3) 0.0447(5) Uani 1 1 d . . .
H8A H 0.0882 0.4660 0.3197 0.054 Uiso 1 1 calc R . .
H8B H 0.1476 0.5199 0.3728 0.054 Uiso 1 1 calc R . .
C9 C 0.20755(12) 0.44233(9) 0.2876(3) 0.0404(4) Uani 1 1 d . . .
H9A H 0.2100 0.4249 0.4298 0.048 Uiso 1 1 calc R . .
H9B H 0.2581 0.4638 0.2617 0.048 Uiso 1 1 calc R . .
C10 C 0.31719(11) 0.20081(7) 0.0953(3) 0.0340(4) Uani 1 1 d . . .
H10A H 0.2988 0.1618 0.0462 0.041 Uiso 1 1 calc R . .
H10B H 0.3168 0.2016 0.2486 0.041 Uiso 1 1 calc R . .
H10C H 0.3715 0.2080 0.0447 0.041 Uiso 1 1 calc R . .
C11 C 0.25753(11) 0.25726(8) -0.2825(3) 0.0317(4) Uani 1 1 d . . .
H11A H 0.2359 0.2196 -0.3356 0.038 Uiso 1 1 calc R . .
H11B H 0.3132 0.2613 -0.3266 0.038 Uiso 1 1 calc R . .
H11C H 0.2264 0.2906 -0.3384 0.038 Uiso 1 1 calc R . .
C12 C 0.15190(10) 0.24237(8) 0.0746(3) 0.0347(4) Uani 1 1 d . . .
H12A H 0.1385 0.2011 0.0383 0.042 Uiso 1 1 calc R . .
H12B H 0.1156 0.2696 0.0018 0.042 Uiso 1 1 calc R . .
H12C H 0.1466 0.2479 0.2260 0.042 Uiso 1 1 calc R . .
S1 S 0.14932(2) 0.074388(17) 0.74112(7) 0.02934(9) Uani 1 1 d . . .
S2 S 0.50372(2) 0.200524(19) 0.60525(7) 0.03000(9) Uani 1 1 d . . .
F1 F 0.19481(14) 0.09908(14) 0.3638(3) 0.1242(10) Uani 1 1 d . . .
F2 F 0.07908(16) 0.06279(10) 0.3811(4) 0.1139(8) Uani 1 1 d . . .
F3 F 0.09771(13) 0.15094(7) 0.4688(3) 0.0882(6) Uani 1 1 d . . .
F4 F 0.48498(9) 0.08454(5) 0.5824(3) 0.0561(4) Uani 1 1 d . . .
F5 F 0.37659(7) 0.13492(6) 0.5578(3) 0.0618(4) Uani 1 1 d . . .
F6 F 0.45722(10) 0.13177(7) 0.3003(2) 0.0626(4) Uani 1 1 d . . .
O1 O 0.07241(11) 0.07537(11) 0.8364(4) 0.0809(7) Uani 1 1 d . . .
O2 O 0.20307(14) 0.11883(9) 0.8137(4) 0.0789(7) Uani 1 1 d . . .
O3 O 0.18358(10) 0.01674(6) 0.7176(3) 0.0603(5) Uani 1 1 d . . .
O4 O 0.45525(9) 0.24844(6) 0.5255(3) 0.0502(4) Uani 1 1 d . . .
O5 O 0.58248(8) 0.19581(7) 0.5206(3) 0.0528(4) Uani 1 1 d . . .
O6 O 0.49932(11) 0.19297(8) 0.8287(2) 0.0533(4) Uani 1 1 d . . .
C13 C 0.13071(14) 0.09821(10) 0.4748(3) 0.0462(5) Uani 1 1 d . . .
C14 C 0.45329(11) 0.13426(8) 0.5075(4) 0.0369(4) 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 C2 1.7851(17) . ?
P1 C1 1.7869(16) . ?
P1 C3 1.7923(17) . ?
P1 P2 2.1979(5) . ?
P2 C4 1.8589(16) . ?
P2 P3 2.1976(6) . ?
P3 C12 1.7889(16) . ?
P3 C11 1.7905(17) . ?
P3 C10 1.7914(17) . ?
C4 C5 1.523(2) . ?
C4 C9 1.544(2) . ?
C5 C6 1.540(2) . ?
C6 C7 1.516(3) . ?
C7 C8 1.522(3) . ?
C8 C9 1.531(3) . ?
S1 O2 1.4217(18) . ?
S1 O3 1.4229(14) . ?
S1 O1 1.4270(17) . ?
S1 C13 1.812(2) . ?
S2 O5 1.4316(15) . ?
S2 O6 1.4403(16) . ?
S2 O4 1.4408(15) . ?
S2 C14 1.8206(18) . ?
F1 C13 1.288(3) . ?
F2 C13 1.319(3) . ?
F3 C13 1.306(3) . ?
F4 C14 1.325(2) . ?
F5 C14 1.326(2) . ?
F6 C14 1.328(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 P1 C1 108.33(9) . . ?
C2 P1 C3 108.11(9) . . ?
C1 P1 C3 108.04(8) . . ?
C2 P1 P2 105.28(6) . . ?
C1 P1 P2 105.91(6) . . ?
C3 P1 P2 120.66(6) . . ?
C4 P2 P3 105.95(5) . . ?
C4 P2 P1 109.29(5) . . ?
P3 P2 P1 103.11(2) . . ?
C12 P3 C11 108.72(9) . . ?
C12 P3 C10 109.75(9) . . ?
C11 P3 C10 108.37(9) . . ?
C12 P3 P2 103.81(7) . . ?
C11 P3 P2 119.69(6) . . ?
C10 P3 P2 106.19(6) . . ?
C5 C4 C9 112.10(14) . . ?
C5 C4 P2 118.30(11) . . ?
C9 C4 P2 106.46(11) . . ?
C4 C5 C6 110.49(14) . . ?
C7 C6 C5 111.09(16) . . ?
C6 C7 C8 110.40(17) . . ?
C7 C8 C9 111.30(16) . . ?
C8 C9 C4 111.16(16) . . ?
O2 S1 O3 114.53(12) . . ?
O2 S1 O1 115.05(16) . . ?
O3 S1 O1 115.11(12) . . ?
O2 S1 C13 102.07(12) . . ?
O3 S1 C13 103.79(11) . . ?
O1 S1 C13 103.94(12) . . ?
O5 S2 O6 114.41(11) . . ?
O5 S2 O4 116.24(10) . . ?
O6 S2 O4 114.20(11) . . ?
O5 S2 C14 103.82(10) . . ?
O6 S2 C14 102.74(10) . . ?
O4 S2 C14 103.00(9) . . ?
F1 C13 F3 108.9(2) . . ?
F1 C13 F2 107.9(3) . . ?
F3 C13 F2 104.7(2) . . ?
F1 C13 S1 112.23(17) . . ?
F3 C13 S1 111.55(16) . . ?
F2 C13 S1 111.23(18) . . ?
F4 C14 F5 108.12(18) . . ?
F4 C14 F6 107.78(16) . . ?
F5 C14 F6 106.89(17) . . ?
F4 C14 S2 112.11(13) . . ?
F5 C14 S2 111.01(13) . . ?
F6 C14 S2 110.72(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
C2 P1 P2 C4 177.34(9) . . . . ?
C1 P1 P2 C4 62.70(8) . . . . ?
C3 P1 P2 C4 -60.22(9) . . . . ?
C2 P1 P2 P3 -70.30(7) . . . . ?
C1 P1 P2 P3 175.06(6) . . . . ?
C3 P1 P2 P3 52.14(7) . . . . ?
C4 P2 P3 C12 -48.63(9) . . . . ?
P1 P2 P3 C12 -163.42(7) . . . . ?
C4 P2 P3 C11 72.75(9) . . . . ?
P1 P2 P3 C11 -42.05(8) . . . . ?
C4 P2 P3 C10 -164.34(9) . . . . ?
P1 P2 P3 C10 80.86(7) . . . . ?
P3 P2 C4 C5 -66.86(13) . . . . ?
P1 P2 C4 C5 43.63(14) . . . . ?
P3 P2 C4 C9 165.95(11) . . . . ?
P1 P2 C4 C9 -83.57(12) . . . . ?
C9 C4 C5 C6 -53.8(2) . . . . ?
P2 C4 C5 C6 -178.25(13) . . . . ?
C4 C5 C6 C7 56.8(2) . . . . ?
C5 C6 C7 C8 -58.7(2) . . . . ?
C6 C7 C8 C9 57.6(2) . . . . ?
C7 C8 C9 C4 -54.4(2) . . . . ?
C5 C4 C9 C8 53.0(2) . . . . ?
P2 C4 C9 C8 -176.20(14) . . . . ?
O2 S1 C13 F1 61.0(3) . . . . ?
O3 S1 C13 F1 -58.4(2) . . . . ?
O1 S1 C13 F1 -179.1(2) . . . . ?
O2 S1 C13 F3 -61.6(2) . . . . ?
O3 S1 C13 F3 179.12(18) . . . . ?
O1 S1 C13 F3 58.4(2) . . . . ?
O2 S1 C13 F2 -178.1(2) . . . . ?
O3 S1 C13 F2 62.6(2) . . . . ?
O1 S1 C13 F2 -58.1(2) . . . . ?
O5 S2 C14 F4 64.61(19) . . . . ?
O6 S2 C14 F4 -54.86(18) . . . . ?
O4 S2 C14 F4 -173.78(16) . . . . ?
O5 S2 C14 F5 -174.35(16) . . . . ?
O6 S2 C14 F5 66.18(18) . . . . ?
O4 S2 C14 F5 -52.74(19) . . . . ?
O5 S2 C14 F6 -55.80(15) . . . . ?
O6 S2 C14 F6 -175.27(14) . . . . ?
O4 S2 C14 F6 65.82(15) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.042
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dal1091
_database_code_depnum_ccdc_archive 'CCDC 1418258'
_audit_update_record             
;
2015-08-12 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H21 P3, 2(C F3 O3 S)'
_chemical_formula_sum            'C9 H21 F6 O6 P3 S2'
_chemical_formula_weight         496.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   13.2969(19)
_cell_length_b                   11.4350(17)
_cell_length_c                   13.956(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.8691(16)
_cell_angle_gamma                90.00
_cell_volume                     2008.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6665
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      24.96

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7814
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17498
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         27.59
_reflns_number_total             4636
_reflns_number_gt                4323
_reflns_threshold_expression     I>2σ(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)+(0.0365P)²+0.9698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4636
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0699
_refine_ls_wR_factor_gt          0.0684
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
P1 P 0.13481(2) 0.46958(3) 0.38399(2) 0.01838(8) Uani 1 1 d . . .
P2 P 0.27719(3) 0.35509(3) 0.41499(2) 0.01910(8) Uani 1 1 d . . .
P3 P -0.01135(2) 0.36438(3) 0.31295(2) 0.01860(8) Uani 1 1 d . . .
C1 C 0.14422(11) 0.55082(12) 0.27321(10) 0.0247(3) Uani 1 1 d . . .
H1A H 0.0849 0.6061 0.2503 0.030 Uiso 1 1 calc R . .
H1B H 0.1412 0.4958 0.2185 0.030 Uiso 1 1 calc R . .
H1C H 0.2116 0.5938 0.2919 0.030 Uiso 1 1 calc R . .
C2 C -0.07771(10) 0.42269(13) 0.18909(10) 0.0253(3) Uani 1 1 d . . .
H2A H -0.0837 0.5078 0.1935 0.030 Uiso 1 1 calc R . .
H2B H -0.1489 0.3884 0.1622 0.030 Uiso 1 1 calc R . .
H2C H -0.0368 0.4036 0.1440 0.030 Uiso 1 1 calc R . .
C3 C -0.09359(11) 0.39191(13) 0.38992(10) 0.0255(3) Uani 1 1 d . . .
H3A H -0.0594 0.3602 0.4579 0.031 Uiso 1 1 calc R . .
H3B H -0.1628 0.3542 0.3595 0.031 Uiso 1 1 calc R . .
H3C H -0.1036 0.4764 0.3944 0.031 Uiso 1 1 calc R . .
C4 C -0.00197(11) 0.20861(12) 0.30295(11) 0.0247(3) Uani 1 1 d . . .
H4A H 0.0344 0.1756 0.3701 0.030 Uiso 1 1 calc R . .
H4B H 0.0384 0.1899 0.2573 0.030 Uiso 1 1 calc R . .
H4C H -0.0735 0.1752 0.2760 0.030 Uiso 1 1 calc R . .
C5 C 0.35000(11) 0.38798(13) 0.54433(10) 0.0253(3) Uani 1 1 d . . .
H5A H 0.3607 0.4727 0.5523 0.030 Uiso 1 1 calc R . .
H5B H 0.4192 0.3487 0.5636 0.030 Uiso 1 1 calc R . .
H5C H 0.3100 0.3606 0.5879 0.030 Uiso 1 1 calc R . .
C6 C 0.26066(11) 0.19956(12) 0.40364(11) 0.0271(3) Uani 1 1 d . . .
H6A H 0.2216 0.1793 0.3332 0.032 Uiso 1 1 calc R . .
H6B H 0.2208 0.1725 0.4474 0.032 Uiso 1 1 calc R . .
H6C H 0.3306 0.1618 0.4241 0.032 Uiso 1 1 calc R . .
C7 C 0.35739(11) 0.39767(14) 0.33911(11) 0.0278(3) Uani 1 1 d . . .
H7A H 0.3683 0.4825 0.3437 0.033 Uiso 1 1 calc R . .
H7B H 0.3213 0.3757 0.2684 0.033 Uiso 1 1 calc R . .
H7C H 0.4263 0.3580 0.3638 0.033 Uiso 1 1 calc R . .
S1 S 0.38384(3) 0.76454(3) 0.44530(3) 0.02425(8) Uani 1 1 d . . .
F1 F 0.26280(10) 0.93880(9) 0.45845(11) 0.0601(3) Uani 1 1 d . . .
F2 F 0.18485(8) 0.77223(10) 0.43349(10) 0.0528(3) Uani 1 1 d . . .
F3 F 0.29208(11) 0.81650(12) 0.57950(9) 0.0610(3) Uani 1 1 d . . .
O1 O 0.38153(11) 0.64280(10) 0.46971(11) 0.0471(3) Uani 1 1 d . . .
O2 O 0.47625(9) 0.82723(12) 0.50523(10) 0.0455(3) Uani 1 1 d . . .
O3 O 0.35275(10) 0.78722(12) 0.33803(9) 0.0400(3) Uani 1 1 d . . .
C8 C 0.27544(12) 0.82634(14) 0.48181(12) 0.0314(3) Uani 1 1 d . . .
S2 S 0.12552(3) 0.25972(3) 0.64313(3) 0.02231(8) Uani 1 1 d . . .
F4 F -0.00477(9) 0.08129(11) 0.59812(14) 0.0785(5) Uani 1 1 d . . .
F5 F 0.15774(10) 0.03460(10) 0.64293(15) 0.0808(5) Uani 1 1 d . . .
F6 F 0.08914(16) 0.09149(15) 0.75370(14) 0.0976(6) Uani 1 1 d . . .
O4 O 0.23256(8) 0.26946(10) 0.71098(8) 0.0339(2) Uani 1 1 d . . .
O5 O 0.04740(9) 0.32842(10) 0.66823(10) 0.0379(3) Uani 1 1 d . . .
O6 O 0.11767(10) 0.26417(12) 0.53747(8) 0.0405(3) Uani 1 1 d . . .
C9 C 0.08962(14) 0.10910(15) 0.66034(17) 0.0459(4) 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 C1 1.8423(14) . ?
P1 P2 2.2262(5) . ?
P1 P3 2.2273(5) . ?
P2 C5 1.7907(14) . ?
P2 C6 1.7927(15) . ?
P2 C7 1.7961(14) . ?
P3 C3 1.7913(13) . ?
P3 C4 1.7943(14) . ?
P3 C2 1.7957(14) . ?
S1 O2 1.4347(12) . ?
S1 O1 1.4359(12) . ?
S1 O3 1.4418(12) . ?
S1 C8 1.8198(15) . ?
F1 C8 1.3239(19) . ?
F2 C8 1.3279(18) . ?
F3 C8 1.3135(19) . ?
S2 O5 1.4333(11) . ?
S2 O4 1.4364(11) . ?
S2 O6 1.4451(12) . ?
S2 C9 1.8238(18) . ?
F4 C9 1.314(2) . ?
F5 C9 1.322(2) . ?
F6 C9 1.320(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 100.10(5) . . ?
C1 P1 P3 100.67(5) . . ?
P2 P1 P3 109.49(2) . . ?
C5 P2 C6 107.96(7) . . ?
C5 P2 C7 107.87(7) . . ?
C6 P2 C7 107.22(7) . . ?
C5 P2 P1 102.76(5) . . ?
C6 P2 P1 119.60(5) . . ?
C7 P2 P1 110.84(5) . . ?
C3 P3 C4 107.00(7) . . ?
C3 P3 C2 107.87(7) . . ?
C4 P3 C2 108.58(7) . . ?
C3 P3 P1 104.61(5) . . ?
C4 P3 P1 119.88(5) . . ?
C2 P3 P1 108.32(5) . . ?
O2 S1 O1 115.22(8) . . ?
O2 S1 O3 114.79(8) . . ?
O1 S1 O3 113.56(8) . . ?
O2 S1 C8 104.44(8) . . ?
O1 S1 C8 103.32(8) . . ?
O3 S1 C8 103.52(7) . . ?
F3 C8 F1 107.70(14) . . ?
F3 C8 F2 107.93(13) . . ?
F1 C8 F2 107.78(14) . . ?
F3 C8 S1 112.00(12) . . ?
F1 C8 S1 110.93(11) . . ?
F2 C8 S1 110.33(10) . . ?
O5 S2 O4 116.00(7) . . ?
O5 S2 O6 114.28(7) . . ?
O4 S2 O6 113.52(7) . . ?
O5 S2 C9 104.13(8) . . ?
O4 S2 C9 103.42(8) . . ?
O6 S2 C9 103.42(9) . . ?
F4 C9 F6 107.87(17) . . ?
F4 C9 F5 106.71(17) . . ?
F6 C9 F5 107.79(18) . . ?
F4 C9 S2 112.10(14) . . ?
F6 C9 S2 111.04(15) . . ?
F5 C9 S2 111.12(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
C1 P1 P2 C5 124.22(7) . . . . ?
P3 P1 P2 C5 -130.56(5) . . . . ?
C1 P1 P2 C6 -116.29(7) . . . . ?
P3 P1 P2 C6 -11.07(6) . . . . ?
C1 P1 P2 C7 9.20(7) . . . . ?
P3 P1 P2 C7 114.42(6) . . . . ?
C1 P1 P3 C3 -128.22(7) . . . . ?
P2 P1 P3 C3 126.95(5) . . . . ?
C1 P1 P3 C4 111.90(7) . . . . ?
P2 P1 P3 C4 7.07(6) . . . . ?
C1 P1 P3 C2 -13.36(7) . . . . ?
P2 P1 P3 C2 -118.19(5) . . . . ?
O2 S1 C8 F3 -57.63(13) . . . . ?
O1 S1 C8 F3 63.24(13) . . . . ?
O3 S1 C8 F3 -178.11(12) . . . . ?
O2 S1 C8 F1 62.75(14) . . . . ?
O1 S1 C8 F1 -176.38(12) . . . . ?
O3 S1 C8 F1 -57.73(13) . . . . ?
O2 S1 C8 F2 -177.89(12) . . . . ?
O1 S1 C8 F2 -57.02(13) . . . . ?
O3 S1 C8 F2 61.63(13) . . . . ?
O5 S2 C9 F4 62.80(17) . . . . ?
O4 S2 C9 F4 -175.55(14) . . . . ?
O6 S2 C9 F4 -56.94(16) . . . . ?
O5 S2 C9 F6 -57.94(16) . . . . ?
O4 S2 C9 F6 63.72(15) . . . . ?
O6 S2 C9 F6 -177.68(14) . . . . ?
O5 S2 C9 F5 -177.90(15) . . . . ?
O4 S2 C9 F5 -56.24(18) . . . . ?
O6 S2 C9 F5 62.36(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.050
