# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2004



data_global

_publ_contact_author_email       TAILLEFE@CIT.ENSCM.FR

_publ_contact_author_name        'Dr Marc Taillefer'
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'

_journal_coden_Cambridge         0440
_publ_contact_author_address     
;
Chimie
CNRS / ENSCM
ENSCM 8 rue de l'Ecole Normale 3429
Montpellier
France
;

_publ_section_title              
;
Synthesis and structural studies (1H, 13C, 31P NMR and
X-ray) of new  C-bonded cyclotriphosphazenes with heterocyclic substituents
from novel phosphinic acid derivatives
;

loop_
_publ_author_name
'Marc Taillefer'
'Corinne Combes-Chamalet'
'Henri-Jean Cristau'
'Alain Fruchier'
;
F.Plenat
;
'Ian J. Scowen'
'Virginie Vicente'

#----------------------------------------------------------------------#
#----------------------------------------------------------------------#
data_taille31
_database_code_depnum_ccdc_archive 'CCDC 184574'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Hexa(3-thienyl)cyclotriphosphazene
;

_chemical_formula_moiety         'C12 H12 Cl1 N1 P1'
_chemical_formula_structural     'C12.5 H9.5 CL1.5 N1.5 P1.5 S3'
_chemical_formula_sum            'C25 H19 Cl3 N3 P3 S6'
_chemical_compound_source        'synthesis as described'
_chemical_formula_weight         376.52

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_Int_Tables_number      62

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

_cell_length_a                   9.828(2)
_cell_length_b                   15.632(3)
_cell_length_c                   20.084(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3085.5(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      24.13

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(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  'Stoe IPDS'
_diffrn_measurement_method       '\f scan'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        <0.1
_diffrn_reflns_number            14257
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         24.13
_reflns_number_total             2472
_reflns_number_gt                2108
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'IPDS software (Stoe, 1996)'
_computing_cell_refinement       'IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_structure_solution    'SIR97 (Altomare, et al.,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_molecular_graphics    'ORTEP-III( Burnett and Johnson,1996)'
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0485P)^2^+4.0609P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2472
_refine_ls_number_parameters     304
_refine_ls_number_restraints     375
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.1031
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002

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 0.83206(6) 0.16076(4) 0.55327(3) 0.0271(2) Uani 1 1 d U A .
P2 P 1.07391(9) 0.2500 0.53031(5) 0.0301(3) Uani 1 2 d SU . .
N1 N 0.9897(2) 0.16278(15) 0.53358(11) 0.0340(5) Uani 1 1 d U . .
N2 N 0.7542(3) 0.2500 0.56121(15) 0.0303(7) Uani 1 2 d SU . .
C11 C 0.8160(2) 0.09969(18) 0.62842(12) 0.0296(6) Uani 1 1 d DU . .
C12 C 0.6916(6) 0.0807(4) 0.6608(3) 0.0431(14) Uani 0.63 1 d PDU A 1
H12 H 0.6056 0.1006 0.6458 0.052 Uiso 0.63 1 calc PR A 1
C13 C 0.7088(7) 0.0288(5) 0.7178(3) 0.0458(18) Uani 0.63 1 d PDU A 1
H13 H 0.6375 0.0076 0.7452 0.055 Uiso 0.63 1 calc PR A 1
S14 S 0.8750(2) 0.01062(15) 0.72939(9) 0.0689(6) Uani 0.63 1 d PDU A 1
C15 C 0.9231(6) 0.0677(5) 0.6626(2) 0.0481(13) Uani 0.63 1 d PDU A 1
H15 H 1.0153 0.0765 0.6501 0.058 Uiso 0.63 1 calc PR A 1
C12A C 0.8829(10) 0.0196(7) 0.6416(5) 0.049(2) Uani 0.37 1 d PDU A 2
H12A H 0.9445 -0.0061 0.6112 0.058 Uiso 0.37 1 calc PR A 2
C13A C 0.8504(12) -0.0160(7) 0.7011(5) 0.053(3) Uani 0.37 1 d PDU A 2
H13A H 0.8835 -0.0692 0.7172 0.064 Uiso 0.37 1 calc PR A 2
S14A S 0.7416(4) 0.0494(3) 0.74225(16) 0.0729(13) Uani 0.37 1 d PDU A 2
C15A C 0.7359(12) 0.1207(8) 0.6781(5) 0.058(3) Uani 0.37 1 d PDU A 2
H15A H 0.6805 0.1705 0.6783 0.070 Uiso 0.37 1 calc PR A 2
C16 C 0.7429(2) 0.09816(17) 0.49296(12) 0.0292(6) Uani 1 1 d DU . .
C17 C 0.7868(8) 0.0171(6) 0.4673(5) 0.0334(19) Uani 0.76 1 d PDU A 1
H17A H 0.8689 -0.0099 0.4808 0.040 Uiso 0.76 1 calc PR A 1
C18 C 0.7020(14) -0.0167(9) 0.4231(8) 0.051(3) Uani 0.76 1 d PDU A 1
H18A H 0.7170 -0.0698 0.4013 0.061 Uiso 0.76 1 calc PR A 1
S19 S 0.56295(19) 0.04634(12) 0.40999(8) 0.0577(5) Uani 0.76 1 d PDU A 1
C20 C 0.6225(7) 0.1224(5) 0.4649(3) 0.0397(15) Uani 0.76 1 d PDU A 1
H20A H 0.5771 0.1746 0.4745 0.048 Uiso 0.76 1 calc PR A 1
C20A C 0.5987(19) 0.1028(14) 0.4805(10) 0.050(6) Uani 0.24 1 d PDU A 2
H20B H 0.5410 0.1439 0.5008 0.060 Uiso 0.24 1 calc PR A 2
C19A C 0.5535(19) 0.0431(14) 0.4371(7) 0.049(4) Uani 0.24 1 d PDU A 2
H19A H 0.4620 0.0366 0.4227 0.059 Uiso 0.24 1 calc PR A 2
S18A S 0.6842(15) -0.0174(9) 0.4131(8) 0.067(3) Uani 0.24 1 d PDU A 2
C17A C 0.802(2) 0.0322(17) 0.4608(16) 0.033(5) Uani 0.24 1 d PDU A 2
H17B H 0.8954 0.0162 0.4643 0.039 Uiso 0.24 1 calc PR A 2
C21 C 1.1973(4) 0.2500 0.5968(2) 0.0402(10) Uani 1 2 d SU . .
C22 C 1.1610(7) 0.2247(4) 0.6639(3) 0.052(3) Uani 0.50 1 d PU . .
C23 C 1.2705(8) 0.2242(5) 0.7056(3) 0.066(3) Uani 0.50 1 d PU . .
S24 S 1.41477(14) 0.2500 0.66501(8) 0.0702(4) Uani 1 2 d SU . .
C25 C 1.3330(4) 0.2500 0.5900(2) 0.0433(10) Uani 1 2 d SU . .
H25 H 1.3784 0.2500 0.5482 0.052 Uiso 1 2 calc SR . .
C26 C 1.1750(4) 0.2500 0.45663(19) 0.0325(9) Uani 1 2 d SU . .
C27 C 1.2195(4) 0.1782(3) 0.42424(18) 0.0618(11) Uani 1 1 d U . .
C28 C 1.310(2) 0.2006(15) 0.3730(7) 0.055(4) Uani 0.50 1 d PU . .
S29 S 1.3009(6) 0.1925(4) 0.35433(19) 0.0517(9) Uani 0.50 1 d PU . .
C1 C 0.8178(5) 0.2500 0.3472(2) 0.0584(14) Uani 1 2 d SU . .
Cl12 Cl 0.90350(14) 0.15921(8) 0.32363(6) 0.0909(4) Uani 1 1 d U . .
Cl1A Cl 0.65702(17) 0.2342(4) 0.31178(11) 0.097(2) Uani 0.50 1 d PU . .
H22 H 1.067(7) 0.2500 0.686(3) 0.11(2) Uiso 1 2 d S . .
H27 H 1.212(4) 0.129(3) 0.436(2) 0.077(15) Uiso 1 1 d . . .
H1 H 0.811(7) 0.2500 0.394(3) 0.10(2) Uiso 1 2 d S . .
H28 H 1.359(8) 0.166(5) 0.333(4) 0.06(2) Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0236(3) 0.0256(4) 0.0322(4) 0.0013(3) 0.0036(3) 0.0003(3)
P2 0.0217(5) 0.0333(6) 0.0353(5) 0.000 0.0043(4) 0.000
N1 0.0253(11) 0.0291(14) 0.0477(13) 0.0012(10) 0.0069(9) 0.0030(9)
N2 0.0239(15) 0.0248(18) 0.0421(18) 0.000 0.0074(13) 0.000
C11 0.0312(13) 0.0266(16) 0.0309(13) -0.0022(11) 0.0004(10) -0.0034(11)
C12 0.039(3) 0.045(4) 0.045(3) 0.001(2) 0.005(2) -0.012(2)
C13 0.056(3) 0.041(4) 0.040(4) -0.003(3) 0.007(3) -0.022(3)
S14 0.0946(14) 0.0640(14) 0.0479(11) 0.0181(9) 0.0091(9) 0.0216(11)
C15 0.045(3) 0.062(4) 0.037(3) 0.008(3) 0.004(2) 0.014(3)
C12A 0.052(5) 0.043(6) 0.051(5) 0.012(4) 0.020(4) 0.017(4)
C13A 0.074(7) 0.035(6) 0.050(6) 0.007(4) 0.008(5) 0.002(4)
S14A 0.089(3) 0.089(3) 0.0410(19) 0.0321(18) 0.0277(17) 0.045(2)
C15A 0.069(7) 0.063(8) 0.043(5) 0.018(5) 0.013(5) 0.034(6)
C16 0.0286(13) 0.0290(16) 0.0301(13) 0.0023(11) 0.0026(10) -0.0002(11)
C17 0.036(3) 0.026(4) 0.038(3) 0.000(3) 0.005(2) 0.000(2)
C18 0.067(5) 0.033(5) 0.053(7) -0.006(3) 0.000(4) 0.017(4)
S19 0.0620(8) 0.0529(9) 0.0581(11) -0.0210(8) -0.0296(9) 0.0104(6)
C20 0.039(3) 0.031(3) 0.049(3) -0.009(2) -0.005(2) 0.002(2)
C20A 0.028(6) 0.042(11) 0.080(14) 0.000(8) -0.006(8) -0.010(7)
C19A 0.033(6) 0.089(10) 0.026(9) 0.004(7) -0.016(7) -0.015(6)
S18A 0.090(5) 0.062(5) 0.049(3) -0.006(3) -0.011(3) -0.017(4)
C17A 0.034(6) 0.020(9) 0.045(9) 0.010(6) 0.002(7) -0.010(6)
C21 0.031(2) 0.050(3) 0.040(2) 0.000 -0.0013(16) 0.000
C22 0.048(3) 0.064(8) 0.044(3) 0.020(3) -0.003(2) -0.003(3)
C23 0.082(4) 0.064(8) 0.053(3) 0.023(3) -0.020(3) -0.011(3)
S24 0.0514(8) 0.0763(11) 0.0827(10) 0.000 -0.0296(7) 0.000
C25 0.034(2) 0.039(3) 0.056(3) 0.000 -0.0052(18) 0.000
C26 0.0222(17) 0.040(3) 0.0350(19) 0.000 0.0021(15) 0.000
C27 0.093(3) 0.044(2) 0.049(2) 0.0052(17) 0.0273(19) 0.014(2)
C28 0.048(5) 0.085(9) 0.032(7) -0.006(6) 0.005(5) 0.023(5)
S29 0.0595(17) 0.0597(17) 0.036(2) -0.0057(16) 0.0176(17) 0.0028(11)
C1 0.058(3) 0.082(4) 0.036(2) 0.000 0.007(2) 0.000
Cl12 0.1145(10) 0.0664(8) 0.0919(8) 0.0110(6) -0.0126(7) 0.0223(7)
Cl1A 0.0441(8) 0.141(5) 0.1075(14) -0.059(3) 0.0134(9) -0.0291(18)

_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 N1 1.599(2) . ?
P1 N2 1.5991(15) . ?
P1 C16 1.787(3) . ?
P1 C11 1.793(3) . ?
P2 N1 1.596(2) . ?
P2 N1 1.596(2) 7_565 ?
P2 C26 1.782(4) . ?
P2 C21 1.804(4) . ?
N2 P1 1.5991(15) 7_565 ?
C11 C15A 1.313(9) . ?
C11 C15 1.353(6) . ?
C11 C12 1.416(6) . ?
C11 C12A 1.438(9) . ?
C12 C13 1.413(9) . ?
C13 S14 1.674(8) . ?
S14 C15 1.680(6) . ?
C12A C13A 1.357(13) . ?
C13A S14A 1.694(10) . ?
S14A C15A 1.704(9) . ?
C16 C17A 1.35(2) . ?
C16 C20 1.365(7) . ?
C16 C17 1.434(8) . ?
C16 C20A 1.441(18) . ?
C17 C18 1.328(14) . ?
C18 S19 1.705(11) . ?
S19 C20 1.724(7) . ?
C20A C19A 1.35(2) . ?
C19A S18A 1.667(16) . ?
S18A C17A 1.69(2) . ?
C21 C25 1.341(6) . ?
C21 C22 1.450(7) 7_565 ?
C21 C22 1.450(7) . ?
C22 C22 0.790(13) 7_565 ?
C22 C23 1.364(9) . ?
C22 C23 1.580(9) 7_565 ?
C23 C23 0.805(14) 7_565 ?
C23 C22 1.580(9) 7_565 ?
C23 S24 1.684(8) . ?
S24 C23 1.684(8) 7_565 ?
S24 C25 1.708(5) . ?
C26 C27 1.370(4) . ?
C26 C27 1.370(4) 7_565 ?
C27 C28 1.41(2) . ?
C27 S29 1.631(5) . ?
C28 C28 1.54(5) 7_565 ?
C28 S29 1.71(2) 7_565 ?
S29 C28 1.71(2) 7_565 ?
S29 S29 1.798(12) 7_565 ?
C1 Cl12 1.717(3) 7_565 ?
C1 Cl12 1.717(3) . ?
C1 Cl1A 1.751(5) . ?
C1 Cl1A 1.751(5) 7_565 ?
Cl1A Cl1A 0.493(13) 7_565 ?

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 P1 N2 118.11(13) . . ?
N1 P1 C16 108.55(12) . . ?
N2 P1 C16 108.10(14) . . ?
N1 P1 C11 107.71(12) . . ?
N2 P1 C11 109.77(14) . . ?
C16 P1 C11 103.64(12) . . ?
N1 P2 N1 117.32(16) . 7_565 ?
N1 P2 C26 108.86(10) . . ?
N1 P2 C26 108.86(10) 7_565 . ?
N1 P2 C21 108.55(11) . . ?
N1 P2 C21 108.55(11) 7_565 . ?
C26 P2 C21 103.88(18) . . ?
P2 N1 P1 121.96(14) . . ?
P1 N2 P1 121.46(18) . 7_565 ?
C15A C11 C15 100.0(5) . . ?
C15A C11 C12 35.5(6) . . ?
C15 C11 C12 111.2(4) . . ?
C15A C11 C12A 110.6(5) . . ?
C15 C11 C12A 39.6(4) . . ?
C12 C11 C12A 97.3(5) . . ?
C15A C11 P1 124.1(5) . . ?
C15 C11 P1 123.7(3) . . ?
C12 C11 P1 125.1(3) . . ?
C12A C11 P1 125.3(4) . . ?
C13 C12 C11 112.9(5) . . ?
C12 C13 S14 109.1(5) . . ?
C13 S14 C15 94.2(3) . . ?
C11 C15 S14 112.5(4) . . ?
C13A C12A C11 114.3(8) . . ?
C12A C13A S14A 109.3(8) . . ?
C13A S14A C15A 92.6(5) . . ?
C11 C15A S14A 113.1(6) . . ?
C17A C16 C20 113.0(12) . . ?
C17A C16 C17 12.3(19) . . ?
C20 C16 C17 111.0(4) . . ?
C17A C16 C20A 112.4(11) . . ?
C20 C16 C20A 20.1(8) . . ?
C17 C16 C20A 106.1(11) . . ?
C17A C16 P1 122.0(9) . . ?
C20 C16 P1 123.6(3) . . ?
C17 C16 P1 125.4(4) . . ?
C20A C16 P1 124.9(9) . . ?
C18 C17 C16 113.8(7) . . ?
C17 C18 S19 112.1(8) . . ?
C18 S19 C20 91.6(5) . . ?
C16 C20 S19 111.5(5) . . ?
C19A C20A C16 113.7(17) . . ?
C20A C19A S18A 109.0(14) . . ?
C19A S18A C17A 96.0(11) . . ?
C16 C17A S18A 108.8(14) . . ?
C25 C21 C22 109.9(4) . 7_565 ?
C25 C21 C22 109.9(4) . . ?
C22 C21 C22 31.6(6) 7_565 . ?
C25 C21 P2 126.4(3) . . ?
C22 C21 P2 121.5(3) 7_565 . ?
C22 C21 P2 121.5(3) . . ?
C22 C22 C23 90.3(4) 7_565 . ?
C22 C22 C21 74.2(3) 7_565 . ?
C23 C22 C21 112.2(6) . . ?
C22 C22 C23 59.7(4) 7_565 7_565 ?
C23 C22 C23 30.6(6) . 7_565 ?
C21 C22 C23 100.8(5) . 7_565 ?
C23 C23 C22 89.7(4) 7_565 . ?
C23 C23 C22 59.7(4) 7_565 7_565 ?
C22 C23 C22 30.0(5) . 7_565 ?
C23 C23 S24 76.2(3) 7_565 . ?
C22 C23 S24 111.4(5) . . ?
C22 C23 S24 101.3(4) 7_565 . ?
C23 S24 C23 27.7(5) . 7_565 ?
C23 S24 C25 91.8(3) . . ?
C23 S24 C25 91.8(3) 7_565 . ?
C21 C25 S24 112.2(4) . . ?
C27 C26 C27 110.2(4) . 7_565 ?
C27 C26 P2 124.9(2) . . ?
C27 C26 P2 124.9(2) 7_565 . ?
C26 C27 C28 110.2(10) . . ?
C26 C27 S29 116.9(4) . . ?
C28 C27 S29 12.9(9) . . ?
C27 C28 C28 104.5(10) . 7_565 ?
C27 C28 S29 111.7(14) . 7_565 ?
C28 C28 S29 13.0(6) 7_565 7_565 ?
C27 S29 C28 88.4(7) . 7_565 ?
C27 S29 S29 97.9(3) . 7_565 ?
C28 S29 S29 13.0(6) 7_565 7_565 ?
Cl12 C1 Cl12 111.5(3) 7_565 . ?
Cl12 C1 Cl1A 116.5(3) 7_565 . ?
Cl12 C1 Cl1A 102.4(3) . . ?
Cl12 C1 Cl1A 102.4(3) 7_565 7_565 ?
Cl12 C1 Cl1A 116.5(3) . 7_565 ?
Cl1A C1 Cl1A 16.2(4) . 7_565 ?
Cl1A Cl1A C1 81.9(2) 7_565 . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        24.13
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.059

#====END

#****************************************************************************   
data_taille2
_database_code_depnum_ccdc_archive 'CCDC 184619'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Hexa-2-thienylcyclotrphosphazene
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 N3 P3 S6'
_chemical_formula_weight         633.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'

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

_cell_length_a                   11.2770(16)
_cell_length_b                   9.1335(10)
_cell_length_c                   13.561(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.044(17)
_cell_angle_gamma                90.00
_cell_volume                     1370.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;

;

_diffrn_ambient_temperature      160(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  'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         200
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_decay_%        negligible
_diffrn_reflns_number            13519
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         25.99
_reflns_number_total             5198
_reflns_number_gt                4995
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS software (Stoe, 1996)'
_computing_cell_refinement       'IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_structure_solution    'SIR97 (Altomare, et al.,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_molecular_graphics    'ORTEP-III( Burnett and Johnson,1996)'
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0467P)^2^+0.4685P] where P=(Fo^2^+2Fc^2^)/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   -0.01(6)
_refine_ls_number_reflns         5198
_refine_ls_number_parameters     346
_refine_ls_number_restraints     433
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.010
_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 0.30963(5) 0.25126(6) 0.71822(4) 0.01468(11) Uani 1 1 d U C .
P2 P 0.21671(4) 0.30261(6) 0.89126(4) 0.01541(12) Uani 1 1 d U . .
P3 P 0.06979(5) 0.17682(6) 0.72365(4) 0.01554(12) Uani 1 1 d U G .
N1 N 0.09236(16) 0.2283(2) 0.83835(13) 0.0210(4) Uani 1 1 d U . .
N2 N 0.18461(16) 0.1731(2) 0.67057(13) 0.0195(4) Uani 1 1 d U . .
N3 N 0.31548(15) 0.3322(2) 0.82323(13) 0.0172(4) Uani 1 1 d U . .
C11 C 0.35058(19) 0.3858(2) 0.63502(15) 0.0173(4) Uani 1 1 d DU . .
C13 C 0.4131(3) 0.5019(4) 0.4991(2) 0.0377(6) Uani 1 1 d DU . .
H13 H 0.4478 0.5132 0.4410 0.045 Uiso 1 1 calc R A 1
C14 C 0.3640(3) 0.6114(3) 0.5441(2) 0.0388(6) Uani 1 1 d DU C .
H14 H 0.3621 0.7096 0.5207 0.047 Uiso 1 1 calc R B 1
S11 S 0.30709(10) 0.56295(11) 0.64309(8) 0.0370(2) Uani 0.80 1 d PDU C 1
C12 C 0.4060(7) 0.3643(11) 0.5511(6) 0.043(2) Uiso 0.80 1 d PDU C 1
H12 H 0.4345 0.2729 0.5315 0.052 Uiso 0.80 1 calc PR C 1
S11A S 0.4067(6) 0.3450(9) 0.5357(6) 0.0352(15) Uani 0.20 1 d PDU C 2
C12A C 0.3263(12) 0.5357(18) 0.6307(12) 0.043(2) Uiso 0.20 1 d PDU C 2
H12A H 0.2892 0.5851 0.6785 0.052 Uiso 0.20 1 calc PR C 2
C15 C 0.42508(19) 0.1148(3) 0.72932(16) 0.0181(4) Uani 1 1 d DU . .
C17 C 0.5238(3) -0.1137(3) 0.7579(2) 0.0408(7) Uani 1 1 d DU . .
H17 H 0.5333 -0.2170 0.7599 0.049 Uiso 1 1 calc R C 1
C18 C 0.6125(2) -0.0158(4) 0.78347(19) 0.0347(6) Uani 1 1 d DU C .
H18 H 0.6938 -0.0446 0.8079 0.042 Uiso 1 1 calc R D 1
S15 S 0.57297(9) 0.15588(13) 0.77020(8) 0.0291(2) Uani 0.73 1 d PDU C 1
C16 C 0.4075(7) -0.0340(9) 0.7260(5) 0.034(2) Uiso 0.73 1 d PDU C 1
H16 H 0.3311 -0.0801 0.7060 0.040 Uiso 0.73 1 calc PR C 1
S15A S 0.3946(4) -0.0625(5) 0.7204(3) 0.0301(10) Uani 0.27 1 d PDU C 2
C16A C 0.5472(12) 0.1321(18) 0.7648(8) 0.034(2) Uiso 0.27 1 d PDU C 2
H16A H 0.5862 0.2244 0.7763 0.040 Uiso 0.27 1 calc PR C 2
S21 S 0.42356(6) 0.11679(9) 0.99703(5) 0.03593(17) Uani 1 1 d U . .
C21 C 0.28411(19) 0.1906(3) 0.99485(16) 0.0188(4) Uani 1 1 d U . .
C22 C 0.2352(2) 0.1464(3) 1.08115(17) 0.0226(5) Uani 1 1 d U . .
H22 H 0.1594 0.1758 1.0953 0.027 Uiso 1 1 calc R . .
C23 C 0.3203(2) 0.0504(3) 1.14210(19) 0.0291(5) Uani 1 1 d U . .
H23 H 0.3061 0.0072 1.2025 0.035 Uiso 1 1 calc R . .
C24 C 0.4228(2) 0.0269(3) 1.1057(2) 0.0311(6) Uani 1 1 d U . .
H24 H 0.4871 -0.0337 1.1379 0.037 Uiso 1 1 calc R . .
S25 S 0.08314(6) 0.50193(8) 1.01838(5) 0.03041(15) Uani 1 1 d U . .
C25 C 0.18933(19) 0.4751(3) 0.94431(16) 0.0184(4) Uani 1 1 d U . .
C26 C 0.25593(19) 0.6027(3) 0.93650(16) 0.0187(4) Uani 1 1 d U . .
H26 H 0.3183 0.6111 0.8986 0.022 Uiso 1 1 calc R . .
C27 C 0.2165(2) 0.7188(3) 0.99391(18) 0.0280(5) Uani 1 1 d U . .
H27 H 0.2512 0.8140 0.9990 0.034 Uiso 1 1 calc R . .
C28 C 0.1253(2) 0.6796(3) 1.03990(17) 0.0294(5) Uani 1 1 d U . .
H28 H 0.0885 0.7443 1.0800 0.035 Uiso 1 1 calc R . .
C31 C -0.04406(19) 0.2898(3) 0.65150(15) 0.0181(4) Uani 1 1 d DU . .
C33 C -0.2202(2) 0.4291(3) 0.6006(2) 0.0307(6) Uani 1 1 d DU . .
H33 H -0.2968 0.4702 0.6039 0.037 Uiso 1 1 calc R E 1
C34 C -0.1605(3) 0.4489(3) 0.5250(2) 0.0388(7) Uani 1 1 d DU G .
H34 H -0.1912 0.5075 0.4679 0.047 Uiso 1 1 calc R F 1
S31 S -0.02756(9) 0.36186(12) 0.53952(7) 0.0347(2) Uani 0.84 1 d PDU G 1
C32 C -0.1507(6) 0.3364(8) 0.6759(5) 0.0264(14) Uiso 0.84 1 d PDU G 1
H32 H -0.1759 0.3100 0.7364 0.032 Uiso 0.84 1 calc PR G 1
C32A C -0.0461(17) 0.358(2) 0.5556(13) 0.0264(14) Uiso 0.16 1 d PDU G 2
H32A H 0.0151 0.3475 0.5168 0.032 Uiso 0.16 1 calc PR G 2
S31A S -0.1654(8) 0.3370(11) 0.6903(6) 0.039(2) Uani 0.16 1 d PDU G 2
S35 S 0.08790(7) -0.14968(9) 0.76371(7) 0.0474(2) Uani 1 1 d U G .
C35 C 0.0041(2) -0.0016(3) 0.71374(16) 0.0195(4) Uani 1 1 d U . .
C36 C -0.1104(2) -0.0445(3) 0.6695(2) 0.0304(5) Uani 1 1 d U G .
H36 H -0.1708 0.0212 0.6371 0.037 Uiso 1 1 calc R . .
C37 C -0.1292(3) -0.1994(3) 0.6777(2) 0.0385(6) Uani 1 1 d U . .
H37 H -0.2029 -0.2483 0.6516 0.046 Uiso 1 1 calc R G .
C38 C -0.0285(3) -0.2664(3) 0.7272(3) 0.0438(7) Uani 1 1 d U G .
H38 H -0.0236 -0.3687 0.7401 0.053 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0152(2) 0.0151(3) 0.0142(2) -0.00263(19) 0.00376(18) -0.00061(19)
P2 0.0150(2) 0.0182(3) 0.0127(2) -0.0024(2) 0.00171(18) 0.0006(2)
P3 0.0152(2) 0.0174(3) 0.0135(2) -0.0009(2) 0.00142(18) -0.0018(2)
N1 0.0158(8) 0.0322(12) 0.0154(8) -0.0031(8) 0.0041(7) -0.0038(7)
N2 0.0181(8) 0.0243(11) 0.0162(8) -0.0056(8) 0.0034(7) -0.0042(8)
N3 0.0168(8) 0.0182(10) 0.0167(8) -0.0041(7) 0.0034(7) -0.0032(7)
C11 0.0193(10) 0.0151(11) 0.0175(10) -0.0012(8) 0.0033(8) -0.0002(8)
C13 0.0435(15) 0.0466(18) 0.0251(13) 0.0048(12) 0.0124(11) -0.0077(13)
C14 0.0470(16) 0.0229(15) 0.0467(16) 0.0110(12) 0.0095(13) 0.0008(12)
S11 0.0544(6) 0.0174(5) 0.0453(5) 0.0024(4) 0.0243(4) 0.0045(4)
S11A 0.043(3) 0.027(3) 0.042(3) 0.019(2) 0.026(2) 0.0037(17)
C15 0.0200(10) 0.0180(12) 0.0178(10) -0.0017(8) 0.0072(8) -0.0002(8)
C17 0.0514(17) 0.0236(16) 0.0479(17) 0.0095(12) 0.0105(14) 0.0106(12)
C18 0.0255(12) 0.0487(18) 0.0287(13) 0.0024(12) 0.0023(10) 0.0132(11)
S15 0.0185(4) 0.0278(6) 0.0397(5) -0.0067(4) 0.0024(4) 0.0005(4)
S15A 0.0232(16) 0.0092(17) 0.056(2) -0.0006(12) 0.0025(11) 0.0021(12)
S21 0.0300(3) 0.0447(5) 0.0332(3) 0.0102(3) 0.0061(3) 0.0133(3)
C21 0.0200(10) 0.0185(12) 0.0177(9) -0.0018(8) 0.0029(8) 0.0001(8)
C22 0.0210(10) 0.0201(13) 0.0229(11) 0.0010(9) -0.0056(8) 0.0005(9)
C23 0.0381(13) 0.0227(14) 0.0244(12) 0.0047(9) 0.0007(10) -0.0070(10)
C24 0.0336(13) 0.0260(14) 0.0302(13) 0.0082(10) -0.0025(10) 0.0057(10)
S25 0.0285(3) 0.0338(4) 0.0318(3) -0.0038(3) 0.0130(2) 0.0038(3)
C25 0.0180(10) 0.0235(12) 0.0132(9) -0.0019(8) 0.0020(7) 0.0039(8)
C26 0.0200(10) 0.0166(11) 0.0185(10) -0.0058(8) 0.0012(8) 0.0050(8)
C27 0.0327(12) 0.0221(13) 0.0272(12) -0.0046(10) 0.0005(9) 0.0036(9)
C28 0.0302(12) 0.0359(15) 0.0213(10) -0.0072(10) 0.0029(9) 0.0127(11)
C31 0.0210(10) 0.0157(11) 0.0166(10) 0.0009(8) 0.0013(8) -0.0031(8)
C33 0.0310(13) 0.0225(14) 0.0347(14) -0.0011(10) -0.0030(10) 0.0057(10)
C34 0.0466(16) 0.0314(16) 0.0321(14) 0.0126(11) -0.0084(12) -0.0013(12)
S31 0.0354(5) 0.0474(5) 0.0232(4) 0.0161(3) 0.0101(3) 0.0054(4)
S31A 0.035(3) 0.050(4) 0.033(3) 0.015(3) 0.008(3) 0.022(3)
S35 0.0357(4) 0.0280(4) 0.0739(5) 0.0212(4) -0.0009(3) 0.0008(3)
C35 0.0216(10) 0.0179(11) 0.0196(10) 0.0021(9) 0.0051(8) -0.0002(9)
C36 0.0295(12) 0.0192(13) 0.0408(15) -0.0027(10) 0.0021(11) -0.0060(9)
C37 0.0361(14) 0.0225(14) 0.0584(18) -0.0046(13) 0.0131(12) -0.0105(11)
C38 0.0503(17) 0.0192(15) 0.067(2) 0.0072(13) 0.0245(15) -0.0038(12)

_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 N3 1.5948(18) . ?
P1 N2 1.6016(18) . ?
P1 C15 1.788(2) . ?
P1 C11 1.788(2) . ?
P2 N1 1.5989(19) . ?
P2 N3 1.5996(18) . ?
P2 C25 1.783(2) . ?
P2 C21 1.786(2) . ?
P3 N2 1.5978(18) . ?
P3 N1 1.5980(18) . ?
P3 C35 1.785(3) . ?
P3 C31 1.786(2) . ?
C11 C12A 1.395(17) . ?
C11 C12 1.413(9) . ?
C11 S11A 1.637(8) . ?
C11 S11 1.700(2) . ?
C13 C14 1.345(4) . ?
C13 C12 1.451(11) . ?
C13 S11A 1.523(8) . ?
C14 C12A 1.493(17) . ?
C14 S11 1.656(3) . ?
C15 C16 1.373(8) . ?
C15 C16A 1.378(14) . ?
C15 S15A 1.655(5) . ?
C15 S15 1.696(2) . ?
C17 C18 1.336(5) . ?
C17 C16 1.490(9) . ?
C17 S15A 1.522(5) . ?
C18 C16A 1.537(16) . ?
C18 S15 1.631(3) . ?
S21 C24 1.688(3) . ?
S21 C21 1.706(2) . ?
C21 C22 1.444(3) . ?
C22 C23 1.439(3) . ?
C23 C24 1.358(4) . ?
S25 C28 1.700(3) . ?
S25 C25 1.722(2) . ?
C25 C26 1.401(3) . ?
C26 C27 1.436(3) . ?
C27 C28 1.349(4) . ?
C31 C32 1.374(7) . ?
C31 C32A 1.438(17) . ?
C31 S31A 1.616(9) . ?
C31 S31 1.698(2) . ?
C33 C34 1.342(4) . ?
C33 C32 1.438(8) . ?
C33 S31A 1.511(8) . ?
C34 C32A 1.524(18) . ?
C34 S31 1.675(3) . ?
S35 C38 1.690(3) . ?
S35 C35 1.714(2) . ?
C35 C36 1.372(3) . ?
C36 C37 1.438(4) . ?
C37 C38 1.350(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
N3 P1 N2 116.72(9) . . ?
N3 P1 C15 110.08(10) . . ?
N2 P1 C15 107.09(11) . . ?
N3 P1 C11 105.85(10) . . ?
N2 P1 C11 111.43(10) . . ?
C15 P1 C11 105.10(10) . . ?
N1 P2 N3 117.43(9) . . ?
N1 P2 C25 110.56(10) . . ?
N3 P2 C25 106.06(10) . . ?
N1 P2 C21 108.32(11) . . ?
N3 P2 C21 108.19(10) . . ?
C25 P2 C21 105.63(10) . . ?
N2 P3 N1 116.94(10) . . ?
N2 P3 C35 107.91(11) . . ?
N1 P3 C35 109.17(10) . . ?
N2 P3 C31 108.96(10) . . ?
N1 P3 C31 109.08(11) . . ?
C35 P3 C31 104.00(10) . . ?
P3 N1 P2 121.62(11) . . ?
P3 N2 P1 122.38(11) . . ?
P1 N3 P2 121.48(11) . . ?
C12A C11 C12 102.5(10) . . ?
C12A C11 S11A 107.0(7) . . ?
C12 C11 S11A 6.0(6) . . ?
C12A C11 S11 9.0(8) . . ?
C12 C11 S11 111.2(4) . . ?
S11A C11 S11 115.6(3) . . ?
C12A C11 P1 129.0(8) . . ?
C12 C11 P1 128.3(4) . . ?
S11A C11 P1 123.4(3) . . ?
S11 C11 P1 120.06(12) . . ?
C14 C13 C12 111.0(4) . . ?
C14 C13 S11A 120.2(4) . . ?
C12 C13 S11A 10.2(6) . . ?
C13 C14 C12A 102.5(7) . . ?
C13 C14 S11 115.2(2) . . ?
C12A C14 S11 12.9(7) . . ?
C14 S11 C11 92.33(14) . . ?
C11 C12 C13 110.2(7) . . ?
C13 S11A C11 95.9(5) . . ?
C11 C12A C14 113.8(13) . . ?
C16 C15 C16A 104.7(9) . . ?
C16 C15 S15A 4.0(5) . . ?
C16A C15 S15A 108.5(7) . . ?
C16 C15 S15 110.9(4) . . ?
C16A C15 S15 6.3(7) . . ?
S15A C15 S15 114.7(2) . . ?
C16 C15 P1 126.1(4) . . ?
C16A C15 P1 127.7(7) . . ?
S15A C15 P1 122.56(19) . . ?
S15 C15 P1 121.86(14) . . ?
C18 C17 C16 108.8(4) . . ?
C18 C17 S15A 120.2(3) . . ?
C16 C17 S15A 11.4(4) . . ?
C17 C18 C16A 103.5(6) . . ?
C17 C18 S15 116.0(2) . . ?
C16A C18 S15 12.6(5) . . ?
C18 S15 C15 93.10(14) . . ?
C15 C16 C17 111.1(5) . . ?
C17 S15A C15 95.9(3) . . ?
C15 C16A C18 111.8(10) . . ?
C24 S21 C21 92.77(12) . . ?
C22 C21 S21 111.70(17) . . ?
C22 C21 P2 128.80(17) . . ?
S21 C21 P2 119.47(12) . . ?
C23 C22 C21 108.6(2) . . ?
C24 C23 C22 114.1(2) . . ?
C23 C24 S21 112.8(2) . . ?
C28 S25 C25 91.91(12) . . ?
C26 C25 S25 111.64(16) . . ?
C26 C25 P2 124.56(16) . . ?
S25 C25 P2 123.68(14) . . ?
C25 C26 C27 110.3(2) . . ?
C28 C27 C26 113.4(2) . . ?
C27 C28 S25 112.74(19) . . ?
C32 C31 C32A 102.7(9) . . ?
C32 C31 S31A 5.4(5) . . ?
C32A C31 S31A 108.2(8) . . ?
C32 C31 S31 110.2(3) . . ?
C32A C31 S31 7.6(8) . . ?
S31A C31 S31 115.7(3) . . ?
C32 C31 P3 128.1(3) . . ?
C32A C31 P3 129.1(8) . . ?
S31A C31 P3 122.7(3) . . ?
S31 C31 P3 121.57(13) . . ?
C34 C33 C32 109.7(3) . . ?
C34 C33 S31A 120.2(4) . . ?
C32 C33 S31A 10.5(5) . . ?
C33 C34 C32A 103.9(7) . . ?
C33 C34 S31 114.5(2) . . ?
C32A C34 S31 10.6(7) . . ?
C34 S31 C31 92.30(13) . . ?
C31 C32 C33 113.3(5) . . ?
C31 C32A C34 110.4(12) . . ?
C33 S31A C31 97.3(5) . . ?
C38 S35 C35 92.49(14) . . ?
C36 C35 S35 110.4(2) . . ?
C36 C35 P3 129.5(2) . . ?
S35 C35 P3 120.09(13) . . ?
C35 C36 C37 112.8(3) . . ?
C38 C37 C36 111.2(3) . . ?
C37 C38 S35 113.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.055


data_sx019
_database_code_depnum_ccdc_archive 'CCDC 204454'

_audit_creation_date             2003-02-20T08:16:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C25 H13 Cl3 N3 P3 S6'
_chemical_formula_weight         747

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monclinic
_symmetry_space_group_name_H-M   I2/a
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   19.420(2)
_cell_length_b                   15.7094(16)
_cell_length_c                   20.428(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.673(7)
_cell_angle_gamma                90
_cell_volume                     6190.0(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    48
_cell_measurement_theta_min      4.89
_cell_measurement_theta_max      12.49

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.88
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_number            6293
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             5446
_reflns_number_gt                3187
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0421P)^2^+13.1621P] where P=(Fo^2^+2Fc^2^)/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_number_reflns         5446
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.122
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.074

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
S11 S 0.13462(8) 0.28062(12) 0.07110(8) 0.0596(5) Uani 1 1 d . . .
S12 S 0.20264(9) 0.64898(11) 0.08487(9) 0.0645(5) Uani 1 1 d . . .
S21 S 0.22930(9) 0.64413(10) 0.31657(8) 0.0572(5) Uani 1 1 d . . .
S22 S 0.21723(7) 0.26660(9) 0.32727(7) 0.0390(4) Uani 1 1 d . . .
S31 S 0.45782(8) 0.28913(10) 0.18796(8) 0.0523(4) Uani 1 1 d . . .
S32 S 0.38094(8) 0.65513(10) 0.17625(8) 0.0529(4) Uani 1 1 d . . .
P1 P 0.21836(7) 0.45039(9) 0.12570(6) 0.0323(3) Uani 1 1 d . . .
P2 P 0.24500(7) 0.45089(9) 0.26377(6) 0.0301(3) Uani 1 1 d . . .
P3 P 0.35401(6) 0.45167(9) 0.18565(6) 0.0307(3) Uani 1 1 d . . .
N1 N 0.19313(19) 0.4524(3) 0.19727(19) 0.0356(10) Uani 1 1 d . . .
N2 N 0.32523(19) 0.4451(3) 0.25614(19) 0.0375(11) Uani 1 1 d . . .
N3 N 0.29878(19) 0.4326(3) 0.12316(19) 0.0327(10) Uani 1 1 d . . .
C111 C 0.0697(3) 0.3002(6) 0.0097(3) 0.075(2) Uani 1 1 d . . .
H111 H 0.0394 0.2585 -0.0086 0.09 Uiso 1 1 calc R . .
C112 C 0.0666(3) 0.3830(6) -0.0100(3) 0.073(2) Uani 1 1 d . . .
H112 H 0.0341 0.4044 -0.0429 0.088 Uiso 1 1 calc R . .
C113 C 0.1189(3) 0.4323(5) 0.0256(3) 0.0497(17) Uani 1 1 d . . .
C114 C 0.1611(3) 0.3851(4) 0.0712(3) 0.0427(14) Uani 1 1 d . . .
C121 C 0.1388(4) 0.6674(6) 0.0204(4) 0.081(3) Uani 1 1 d . . .
H121 H 0.1268 0.7215 0.0043 0.097 Uiso 1 1 calc R . .
C122 C 0.1084(4) 0.5968(6) -0.0039(3) 0.073(2) Uani 1 1 d . . .
H122 H 0.0731 0.5957 -0.0388 0.087 Uiso 1 1 calc R . .
C123 C 0.1363(3) 0.5227(5) 0.0297(3) 0.0519(18) Uani 1 1 d . . .
C124 C 0.1877(3) 0.5425(4) 0.0791(3) 0.0447(15) Uani 1 1 d . . .
C211 C 0.2035(3) 0.6496(4) 0.3941(3) 0.0614(18) Uani 1 1 d . . .
H211 H 0.1975 0.7006 0.4159 0.074 Uiso 1 1 calc R . .
C212 C 0.1931(3) 0.5727(4) 0.4200(3) 0.0532(17) Uani 1 1 d . . .
H212 H 0.1786 0.5644 0.4613 0.064 Uiso 1 1 calc R . .
C213 C 0.2068(3) 0.5059(3) 0.3767(3) 0.0342(12) Uani 1 1 d . . .
C214 C 0.2269(3) 0.5357(3) 0.3187(3) 0.0377(13) Uani 1 1 d . . .
C221 C 0.1923(3) 0.2717(4) 0.4048(3) 0.0434(15) Uani 1 1 d . . .
H221 H 0.1829 0.224 0.4292 0.052 Uiso 1 1 calc R . .
C222 C 0.1875(3) 0.3528(4) 0.4270(3) 0.0425(14) Uani 1 1 d . . .
H222 H 0.1752 0.367 0.4682 0.051 Uiso 1 1 calc R . .
C223 C 0.2037(3) 0.4130(3) 0.3794(2) 0.0344(13) Uani 1 1 d . . .
C224 C 0.2212(2) 0.3749(3) 0.3230(2) 0.0320(12) Uani 1 1 d . . .
C311 C 0.5432(3) 0.3170(5) 0.1865(3) 0.0642(19) Uani 1 1 d . . .
H311 H 0.5792 0.2778 0.1877 0.077 Uiso 1 1 calc R . .
C312 C 0.5524(3) 0.4021(4) 0.1835(3) 0.0531(17) Uani 1 1 d . . .
H312 H 0.5953 0.4282 0.1825 0.064 Uiso 1 1 calc R . .
C313 C 0.4895(3) 0.4464(4) 0.1820(2) 0.0370(13) Uani 1 1 d . . .
C314 C 0.4336(2) 0.3938(3) 0.1843(2) 0.0346(13) Uani 1 1 d . . .
C321 C 0.4661(3) 0.6816(4) 0.1720(3) 0.0584(18) Uani 1 1 d . . .
H321 H 0.4818 0.7372 0.1686 0.07 Uiso 1 1 calc R . .
C322 C 0.5074(3) 0.6133(4) 0.1741(3) 0.0526(16) Uani 1 1 d . . .
H322 H 0.5551 0.6161 0.1727 0.063 Uiso 1 1 calc R . .
C323 C 0.4707(3) 0.5370(4) 0.1787(2) 0.0393(14) Uani 1 1 d . . .
C324 C 0.4013(3) 0.5494(3) 0.1791(2) 0.0369(12) Uani 1 1 d . . .
C1SA C 0.44072(13) 0.5017(2) 0.37575(11) 0.102(3) Uani 1 1 d . . .
H1SA H 0.4078 0.4883 0.3371 0.122 Uiso 1 1 calc R A 1
Cl1C Cl 0.44108(13) 0.6062(2) 0.38772(11) 0.255(5) Uani 0.6 1 d PR A 1
Cl2C Cl 0.51884(13) 0.4670(2) 0.36271(11) 0.218(4) Uani 0.6 1 d PR A 1
Cl3C Cl 0.41298(13) 0.4551(2) 0.44332(11) 0.139(2) Uani 0.6 1 d PR A 1
Cl1D Cl 0.40006(13) 0.5638(2) 0.42335(11) 0.331(12) Uani 0.4 1 d PR A 2
Cl2D Cl 0.51288(13) 0.5600(2) 0.35929(11) 0.137(3) Uani 0.4 1 d PR A 2
Cl3D Cl 0.47612(13) 0.4071(2) 0.40616(11) 0.284(8) Uani 0.4 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S11 0.0443(9) 0.0692(12) 0.0666(11) -0.0311(9) 0.0116(8) -0.0114(8)
S12 0.0546(10) 0.0548(11) 0.0864(13) 0.0297(10) 0.0178(9) 0.0075(9)
S21 0.0846(13) 0.0348(9) 0.0557(10) 0.0003(8) 0.0231(9) -0.0001(9)
S22 0.0482(8) 0.0320(8) 0.0396(8) 0.0019(6) 0.0169(7) -0.0019(7)
S31 0.0418(9) 0.0474(10) 0.0685(11) 0.0128(8) 0.0094(8) 0.0108(7)
S32 0.0645(11) 0.0381(9) 0.0568(10) -0.0030(8) 0.0098(8) -0.0033(8)
P1 0.0282(7) 0.0408(8) 0.0282(7) 0.0016(7) 0.0037(5) 0.0008(7)
P2 0.0319(7) 0.0330(8) 0.0263(7) 0.0005(7) 0.0079(5) -0.0009(6)
P3 0.0262(7) 0.0359(8) 0.0305(7) 0.0029(7) 0.0057(5) 0.0002(6)
N1 0.026(2) 0.048(3) 0.034(2) 0.000(2) 0.0068(18) 0.005(2)
N2 0.028(2) 0.055(3) 0.029(2) 0.002(2) 0.0040(18) -0.005(2)
N3 0.029(2) 0.042(3) 0.028(2) -0.001(2) 0.0090(18) 0.001(2)
C111 0.040(4) 0.118(7) 0.069(5) -0.053(5) 0.012(3) -0.012(5)
C112 0.034(4) 0.145(8) 0.040(4) -0.022(5) 0.001(3) 0.003(5)
C113 0.027(3) 0.095(6) 0.028(3) -0.006(3) 0.006(2) 0.002(3)
C114 0.028(3) 0.065(4) 0.036(3) -0.011(3) 0.006(2) 0.004(3)
C121 0.064(5) 0.093(6) 0.090(6) 0.054(5) 0.027(4) 0.026(5)
C122 0.048(4) 0.121(7) 0.053(4) 0.044(5) 0.017(3) 0.029(5)
C123 0.033(3) 0.089(5) 0.034(3) 0.019(3) 0.009(3) 0.017(3)
C124 0.035(3) 0.059(4) 0.040(3) 0.016(3) 0.008(3) 0.006(3)
C211 0.087(5) 0.040(4) 0.062(4) -0.014(3) 0.028(4) 0.001(4)
C212 0.073(4) 0.047(4) 0.044(4) -0.006(3) 0.023(3) 0.003(3)
C213 0.040(3) 0.033(3) 0.032(3) -0.002(3) 0.011(2) 0.003(3)
C214 0.045(3) 0.033(3) 0.036(3) 0.003(3) 0.006(2) -0.001(3)
C221 0.047(3) 0.047(4) 0.040(3) 0.012(3) 0.020(3) 0.000(3)
C222 0.051(4) 0.046(4) 0.034(3) 0.001(3) 0.019(3) 0.000(3)
C223 0.033(3) 0.041(3) 0.031(3) -0.002(3) 0.011(2) 0.001(3)
C224 0.034(3) 0.032(3) 0.031(3) 0.001(2) 0.010(2) -0.003(2)
C311 0.035(3) 0.082(6) 0.076(5) 0.014(4) 0.010(3) 0.021(4)
C312 0.027(3) 0.077(5) 0.055(4) 0.010(4) 0.008(3) 0.004(3)
C313 0.031(3) 0.050(4) 0.030(3) 0.002(3) 0.006(2) -0.002(3)
C314 0.030(3) 0.044(3) 0.030(3) 0.005(3) 0.006(2) 0.004(3)
C321 0.078(5) 0.043(4) 0.053(4) -0.007(3) 0.007(3) -0.031(4)
C322 0.049(4) 0.060(4) 0.050(4) 0.000(3) 0.012(3) -0.020(3)
C323 0.032(3) 0.059(4) 0.027(3) -0.001(3) 0.006(2) -0.011(3)
C324 0.038(3) 0.035(3) 0.039(3) 0.006(3) 0.011(2) -0.002(3)
C1SA 0.092(6) 0.141(8) 0.064(5) -0.005(5) -0.025(5) -0.037(6)
Cl1C 0.351(13) 0.109(5) 0.269(10) 0.061(6) -0.114(9) -0.046(7)
Cl2C 0.089(4) 0.454(14) 0.113(4) -0.042(7) 0.019(3) 0.038(6)
Cl3C 0.186(6) 0.133(4) 0.107(3) 0.011(4) 0.061(4) -0.048(4)
Cl1D 0.111(7) 0.71(4) 0.179(11) -0.204(17) 0.041(7) 0.041(14)
Cl2D 0.126(6) 0.152(8) 0.132(6) 0.029(6) 0.010(5) -0.048(6)
Cl3D 0.41(2) 0.105(7) 0.295(17) 0.062(9) -0.128(15) -0.059(10)

#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
S11 C111 1.699(7) . ?
S11 C114 1.720(6) . ?
S12 C124 1.700(6) . ?
S12 C121 1.726(8) . ?
S21 C214 1.704(5) . ?
S21 C211 1.717(6) . ?
S22 C224 1.706(5) . ?
S22 C221 1.711(5) . ?
S31 C314 1.710(5) . ?
S31 C311 1.718(6) . ?
S32 C324 1.707(5) . ?
S32 C321 1.718(6) . ?
P1 N3 1.593(4) . ?
P1 N1 1.595(4) . ?
P1 C124 1.795(6) . ?
P1 C114 1.801(6) . ?
P2 N2 1.586(4) . ?
P2 N1 1.595(4) . ?
P2 C224 1.798(5) . ?
P2 C214 1.803(5) . ?
P3 N3 1.597(4) . ?
P3 N2 1.608(4) . ?
P3 C314 1.795(5) . ?
P3 C324 1.802(5) . ?
C111 C112 1.361(10) . ?
C112 C113 1.410(9) . ?
C113 C114 1.382(8) . ?
C113 C123 1.459(9) . ?
C121 C122 1.325(10) . ?
C122 C123 1.427(9) . ?
C123 C124 1.370(8) . ?
C211 C212 1.344(8) . ?
C212 C213 1.417(7) . ?
C213 C214 1.373(7) . ?
C213 C223 1.461(7) . ?
C221 C222 1.358(7) . ?
C222 C223 1.417(7) . ?
C223 C224 1.377(6) . ?
C311 C312 1.351(8) . ?
C312 C313 1.404(7) . ?
C313 C314 1.369(7) . ?
C313 C323 1.468(8) . ?
C321 C322 1.337(8) . ?
C322 C323 1.404(7) . ?
C323 C324 1.363(7) . ?
C1SA Cl1D 1.6427 . ?
C1SA Cl1C 1.6596 . ?
C1SA Cl2C 1.6624 . ?
C1SA Cl3C 1.704 . ?
C1SA Cl3D 1.7223 . ?
C1SA Cl2D 1.7395 . ?

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
C111 S11 C114 91.4(4) . . ?
C124 S12 C121 90.6(4) . . ?
C214 S21 C211 90.9(3) . . ?
C224 S22 C221 91.1(3) . . ?
C314 S31 C311 90.9(3) . . ?
C324 S32 C321 91.0(3) . . ?
N3 P1 N1 116.1(2) . . ?
N3 P1 C124 113.0(2) . . ?
N1 P1 C124 110.6(2) . . ?
N3 P1 C114 114.7(2) . . ?
N1 P1 C114 110.2(2) . . ?
C124 P1 C114 89.3(3) . . ?
N2 P2 N1 116.6(2) . . ?
N2 P2 C224 111.1(2) . . ?
N1 P2 C224 113.4(2) . . ?
N2 P2 C214 111.6(2) . . ?
N1 P2 C214 111.7(2) . . ?
C224 P2 C214 89.3(2) . . ?
N3 P3 N2 115.6(2) . . ?
N3 P3 C314 113.1(2) . . ?
N2 P3 C314 111.7(2) . . ?
N3 P3 C324 113.7(2) . . ?
N2 P3 C324 110.8(2) . . ?
C314 P3 C324 89.0(2) . . ?
P2 N1 P1 123.3(2) . . ?
P2 N2 P3 122.1(3) . . ?
P1 N3 P3 120.7(2) . . ?
C112 C111 S11 113.3(6) . . ?
C111 C112 C113 111.6(7) . . ?
C114 C113 C112 112.8(7) . . ?
C114 C113 C123 111.6(5) . . ?
C112 C113 C123 135.4(6) . . ?
C113 C114 S11 111.0(4) . . ?
C113 C114 P1 112.7(5) . . ?
S11 C114 P1 135.0(4) . . ?
C122 C121 S12 113.2(6) . . ?
C121 C122 C123 112.1(7) . . ?
C124 C123 C122 111.9(7) . . ?
C124 C123 C113 114.0(5) . . ?
C122 C123 C113 134.0(6) . . ?
C123 C124 S12 112.2(5) . . ?
C123 C124 P1 112.1(5) . . ?
S12 C124 P1 135.5(4) . . ?
C212 C211 S21 113.1(5) . . ?
C211 C212 C213 111.9(5) . . ?
C214 C213 C212 112.2(5) . . ?
C214 C213 C223 113.0(5) . . ?
C212 C213 C223 134.8(5) . . ?
C213 C214 S21 112.0(4) . . ?
C213 C214 P2 112.4(4) . . ?
S21 C214 P2 135.6(3) . . ?
C222 C221 S22 113.0(4) . . ?
C221 C222 C223 111.6(5) . . ?
C224 C223 C222 112.3(5) . . ?
C224 C223 C213 112.8(5) . . ?
C222 C223 C213 134.9(5) . . ?
C223 C224 S22 112.0(4) . . ?
C223 C224 P2 112.5(4) . . ?
S22 C224 P2 135.5(3) . . ?
C312 C311 S31 112.7(5) . . ?
C311 C312 C313 111.8(6) . . ?
C314 C313 C312 113.1(5) . . ?
C314 C313 C323 113.1(5) . . ?
C312 C313 C323 133.8(5) . . ?
C313 C314 S31 111.5(4) . . ?
C313 C314 P3 112.5(4) . . ?
S31 C314 P3 136.0(3) . . ?
C322 C321 S32 112.5(5) . . ?
C321 C322 C323 112.3(5) . . ?
C324 C323 C322 112.9(6) . . ?
C324 C323 C313 112.2(5) . . ?
C322 C323 C313 134.9(5) . . ?
C323 C324 S32 111.4(4) . . ?
C323 C324 P3 113.0(4) . . ?
S32 C324 P3 135.5(3) . . ?
Cl1D C1SA Cl1C 47.1 . . ?
Cl1D C1SA Cl2C 143.1 . . ?
Cl1C C1SA Cl2C 111.1 . . ?
Cl1D C1SA Cl3C 63.7 . . ?
Cl1C C1SA Cl3C 107.6 . . ?
Cl2C C1SA Cl3C 111.7 . . ?
Cl1D C1SA Cl3D 119.9 . . ?
Cl1C C1SA Cl3D 143.6 . . ?
Cl2C C1SA Cl3D 56.1 . . ?
Cl3C C1SA Cl3D 59.2 . . ?
Cl1D C1SA Cl2D 104.8 . . ?
Cl1C C1SA Cl2D 61.2 . . ?
Cl2C C1SA Cl2D 51 . . ?
Cl3C C1SA Cl2D 136.1 . . ?
Cl3D C1SA Cl2D 103.1 . . ?

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
N2 P2 N1 P1 -1.4(4) . . . . ?
C224 P2 N1 P1 -132.3(3) . . . . ?
C214 P2 N1 P1 128.6(3) . . . . ?
N3 P1 N1 P2 9.0(4) . . . . ?
C124 P1 N1 P2 -121.5(3) . . . . ?
C114 P1 N1 P2 141.4(3) . . . . ?
N1 P2 N2 P3 7.2(4) . . . . ?
C224 P2 N2 P3 139.2(3) . . . . ?
C214 P2 N2 P3 -122.9(3) . . . . ?
N3 P3 N2 P2 -20.1(4) . . . . ?
C314 P3 N2 P2 -151.4(3) . . . . ?
C324 P3 N2 P2 111.0(3) . . . . ?
N1 P1 N3 P3 -22.9(4) . . . . ?
C124 P1 N3 P3 106.4(3) . . . . ?
C114 P1 N3 P3 -153.2(3) . . . . ?
N2 P3 N3 P1 28.2(4) . . . . ?
C314 P3 N3 P1 158.8(3) . . . . ?
C324 P3 N3 P1 -101.6(3) . . . . ?
C114 S11 C111 C112 -1.0(5) . . . . ?
S11 C111 C112 C113 0.4(8) . . . . ?
C111 C112 C113 C114 0.6(8) . . . . ?
C111 C112 C113 C123 -173.5(6) . . . . ?
C112 C113 C114 S11 -1.4(6) . . . . ?
C123 C113 C114 S11 174.2(4) . . . . ?
C112 C113 C114 P1 -170.4(4) . . . . ?
C123 C113 C114 P1 5.2(6) . . . . ?
C111 S11 C114 C113 1.3(4) . . . . ?
C111 S11 C114 P1 166.9(4) . . . . ?
N3 P1 C114 C113 -119.8(4) . . . . ?
N1 P1 C114 C113 107.0(4) . . . . ?
C124 P1 C114 C113 -4.7(4) . . . . ?
N3 P1 C114 S11 74.8(5) . . . . ?
N1 P1 C114 S11 -58.4(5) . . . . ?
C124 P1 C114 S11 -170.1(4) . . . . ?
C124 S12 C121 C122 -0.3(6) . . . . ?
S12 C121 C122 C123 0.2(8) . . . . ?
C121 C122 C123 C124 0.1(8) . . . . ?
C121 C122 C123 C113 175.3(6) . . . . ?
C114 C113 C123 C124 -2.9(7) . . . . ?
C112 C113 C123 C124 171.3(6) . . . . ?
C114 C113 C123 C122 -178.1(6) . . . . ?
C112 C113 C123 C122 -3.9(11) . . . . ?
C122 C123 C124 S12 -0.3(6) . . . . ?
C113 C123 C124 S12 -176.5(4) . . . . ?
C122 C123 C124 P1 175.5(4) . . . . ?
C113 C123 C124 P1 -0.7(6) . . . . ?
C121 S12 C124 C123 0.3(5) . . . . ?
C121 S12 C124 P1 -174.1(5) . . . . ?
N3 P1 C124 C123 119.6(4) . . . . ?
N1 P1 C124 C123 -108.3(4) . . . . ?
C114 P1 C124 C123 3.0(4) . . . . ?
N3 P1 C124 S12 -65.9(5) . . . . ?
N1 P1 C124 S12 66.1(5) . . . . ?
C114 P1 C124 S12 177.5(4) . . . . ?
C214 S21 C211 C212 -0.5(6) . . . . ?
S21 C211 C212 C213 0.6(7) . . . . ?
C211 C212 C213 C214 -0.4(8) . . . . ?
C211 C212 C213 C223 -179.6(6) . . . . ?
C212 C213 C214 S21 0.1(6) . . . . ?
C223 C213 C214 S21 179.4(4) . . . . ?
C212 C213 C214 P2 179.6(4) . . . . ?
C223 C213 C214 P2 -1.1(6) . . . . ?
C211 S21 C214 C213 0.2(5) . . . . ?
C211 S21 C214 P2 -179.1(5) . . . . ?
N2 P2 C214 C213 -110.9(4) . . . . ?
N1 P2 C214 C213 116.6(4) . . . . ?
C224 P2 C214 C213 1.6(4) . . . . ?
N2 P2 C214 S21 68.5(5) . . . . ?
N1 P2 C214 S21 -64.0(5) . . . . ?
C224 P2 C214 S21 -179.0(5) . . . . ?
C224 S22 C221 C222 -0.4(5) . . . . ?
S22 C221 C222 C223 0.8(6) . . . . ?
C221 C222 C223 C224 -0.9(7) . . . . ?
C221 C222 C223 C213 179.9(6) . . . . ?
C214 C213 C223 C224 -0.4(7) . . . . ?
C212 C213 C223 C224 178.8(6) . . . . ?
C214 C213 C223 C222 178.8(6) . . . . ?
C212 C213 C223 C222 -2.0(12) . . . . ?
C222 C223 C224 S22 0.6(6) . . . . ?
C213 C223 C224 S22 180.0(4) . . . . ?
C222 C223 C224 P2 -177.7(4) . . . . ?
C213 C223 C224 P2 1.6(6) . . . . ?
C221 S22 C224 C223 -0.1(4) . . . . ?
C221 S22 C224 P2 177.7(4) . . . . ?
N2 P2 C224 C223 111.1(4) . . . . ?
N1 P2 C224 C223 -115.3(4) . . . . ?
C214 P2 C224 C223 -1.8(4) . . . . ?
N2 P2 C224 S22 -66.7(5) . . . . ?
N1 P2 C224 S22 66.9(5) . . . . ?
C214 P2 C224 S22 -179.6(5) . . . . ?
C314 S31 C311 C312 0.1(5) . . . . ?
S31 C311 C312 C313 -0.3(7) . . . . ?
C311 C312 C313 C314 0.4(7) . . . . ?
C311 C312 C313 C323 -179.8(6) . . . . ?
C312 C313 C314 S31 -0.3(6) . . . . ?
C323 C313 C314 S31 179.8(4) . . . . ?
C312 C313 C314 P3 177.7(4) . . . . ?
C323 C313 C314 P3 -2.2(6) . . . . ?
C311 S31 C314 C313 0.1(4) . . . . ?
C311 S31 C314 P3 -177.2(5) . . . . ?
N3 P3 C314 C313 117.9(4) . . . . ?
N2 P3 C314 C313 -109.6(4) . . . . ?
C324 P3 C314 C313 2.4(4) . . . . ?
N3 P3 C314 S31 -64.8(5) . . . . ?
N2 P3 C314 S31 67.7(5) . . . . ?
C324 P3 C314 S31 179.8(4) . . . . ?
C324 S32 C321 C322 -1.3(5) . . . . ?
S32 C321 C322 C323 0.5(7) . . . . ?
C321 C322 C323 C324 0.8(7) . . . . ?
C321 C322 C323 C313 179.6(6) . . . . ?
C314 C313 C323 C324 0.5(7) . . . . ?
C312 C313 C323 C324 -179.4(6) . . . . ?
C314 C313 C323 C322 -178.3(6) . . . . ?
C312 C313 C323 C322 1.8(11) . . . . ?
C322 C323 C324 S32 -1.7(6) . . . . ?
C313 C323 C324 S32 179.2(4) . . . . ?
C322 C323 C324 P3 -179.5(4) . . . . ?
C313 C323 C324 P3 1.4(6) . . . . ?
C321 S32 C324 C323 1.7(4) . . . . ?
C321 S32 C324 P3 178.8(4) . . . . ?
N3 P3 C324 C323 -117.1(4) . . . . ?
N2 P3 C324 C323 110.7(4) . . . . ?
C314 P3 C324 C323 -2.2(4) . . . . ?
N3 P3 C324 S32 65.9(5) . . . . ?
N2 P3 C324 S32 -66.3(5) . . . . ?
C314 P3 C324 S32 -179.2(4) . . . . ?