 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 2,2-trimethylenedioxy-4,4,6,6-tetrachlorocyclotriphosphazene
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C3 H6 Cl4 N3 O2 P3'
_chemical_formula_weight          350.82
 
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'
 'P'  'P'   0.1023   0.0942
 '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    Pna2(1)
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z+1/2'
 
_cell_length_a                    13.3686(5)
_cell_length_b                    10.4704(4)
_cell_length_c                    8.7799(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1228.96(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        needle
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.896
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              696
_exptl_absorpt_coefficient_mu     1.336
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6900
_exptl_absorpt_correction_T_max   0.9485
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type    'Nonius KappaCCD'
_diffrn_measurement_method        'φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             5145
_diffrn_reflns_av_R_equivalents   0.0369
_diffrn_reflns_av_sigmaI/netI     0.0483
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.03
_diffrn_reflns_theta_max          27.47
_reflns_number_total              2403
_reflns_number_gt                 2284
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+0.2979P] 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      SHELXL
_refine_ls_extinction_coef        0.0020(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.00(7)
_refine_ls_number_reflns          2403
_refine_ls_number_parameters      137
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0286
_refine_ls_R_factor_gt            0.0253
_refine_ls_wR_factor_ref          0.0579
_refine_ls_wR_factor_gt           0.0567
_refine_ls_goodness_of_fit_ref    1.057
_refine_ls_restrained_S_all       1.057
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.5365(2) 0.0919(3) 0.2152(3) 0.0344(6) Uani 1 1 d . . .
H1A H 0.5801 0.1620 0.2513 0.041 Uiso 1 1 calc R . .
H1B H 0.5251 0.1038 0.1047 0.041 Uiso 1 1 calc R . .
C2 C 0.5874(2) -0.0351(2) 0.2426(3) 0.0342(6) Uani 1 1 d . . .
H2A H 0.6037 -0.0436 0.3521 0.041 Uiso 1 1 calc R . .
H2B H 0.6508 -0.0383 0.1845 0.041 Uiso 1 1 calc R . .
C3 C 0.52151(19) -0.1439(3) 0.1948(3) 0.0328(6) Uani 1 1 d . . .
H3A H 0.5061 -0.1370 0.0848 0.039 Uiso 1 1 calc R . .
H3B H 0.5565 -0.2260 0.2123 0.039 Uiso 1 1 calc R . .
N1 N 0.31282(15) -0.0045(2) 0.1101(3) 0.0284(5) Uani 1 1 d . . .
N2 N 0.12854(16) -0.0369(2) 0.2326(3) 0.0314(5) Uani 1 1 d . . .
N3 N 0.29117(17) -0.0152(2) 0.4155(3) 0.0318(5) Uani 1 1 d . . .
O1 O 0.44048(13) 0.09638(16) 0.2961(2) 0.0307(4) Uani 1 1 d . . .
O2 O 0.42886(13) -0.14056(15) 0.2831(2) 0.0293(4) Uani 1 1 d . . .
P1 P 0.36404(5) -0.01592(6) 0.27410(8) 0.02445(15) Uani 1 1 d . . .
P2 P 0.19796(5) -0.01989(6) 0.08679(8) 0.02560(16) Uani 1 1 d . . .
P3 P 0.17444(5) -0.02806(6) 0.39714(8) 0.02745(16) Uani 1 1 d . . .
Cl1 Cl 0.17081(5) -0.16570(6) -0.05393(8) 0.03755(17) Uani 1 1 d . . .
Cl2 Cl 0.14660(5) 0.12595(6) -0.03624(8) 0.03721(17) Uani 1 1 d . . .
Cl3 Cl 0.10916(5) 0.11455(7) 0.51041(9) 0.04301(19) Uani 1 1 d . . .
Cl4 Cl 0.12756(5) -0.17805(7) 0.51805(8) 0.03705(17) Uani 1 1 d . . .
 
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
C1 0.0294(15) 0.0405(14) 0.0334(14) -0.0007(12) 0.0052(11) -0.0103(12)
C2 0.0244(13) 0.0548(16) 0.0234(14) 0.0011(12) 0.0008(11) 0.0010(12)
C3 0.0323(14) 0.0405(14) 0.0255(14) 0.0012(11) 0.0038(11) 0.0105(12)
N1 0.0239(11) 0.0367(11) 0.0247(14) 0.0039(10) -0.0010(9) -0.0004(8)
N2 0.0248(11) 0.0397(12) 0.0297(13) 0.0015(10) -0.0014(9) -0.0024(9)
N3 0.0251(11) 0.0459(13) 0.0244(13) -0.0042(10) -0.0018(9) -0.0021(9)
O1 0.0256(10) 0.0307(9) 0.0360(11) -0.0063(8) 0.0019(8) -0.0039(7)
O2 0.0291(10) 0.0280(8) 0.0307(10) 0.0017(8) 0.0013(8) 0.0033(7)
P1 0.0235(3) 0.0269(3) 0.0230(4) -0.0005(3) -0.0002(3) -0.0001(2)
P2 0.0252(3) 0.0276(3) 0.0240(3) 0.0021(3) -0.0015(3) 0.0001(2)
P3 0.0252(3) 0.0316(4) 0.0255(4) -0.0010(3) 0.0028(3) -0.0003(3)
Cl1 0.0406(4) 0.0361(3) 0.0360(4) -0.0079(3) -0.0004(3) -0.0048(3)
Cl2 0.0347(3) 0.0354(3) 0.0416(4) 0.0118(3) -0.0044(3) 0.0031(3)
Cl3 0.0409(4) 0.0414(4) 0.0468(4) -0.0104(3) 0.0106(3) 0.0052(3)
Cl4 0.0378(4) 0.0400(4) 0.0334(4) 0.0075(3) 0.0014(3) -0.0051(3)
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.468(3) . ?
C1 C2 1.513(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.500(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.461(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N1 P2 1.557(2) . ?
N1 P1 1.599(2) . ?
N2 P3 1.572(3) . ?
N2 P2 1.591(3) . ?
N3 P1 1.578(2) . ?
N3 P3 1.575(2) . ?
O1 P1 1.5697(18) . ?
O2 P1 1.5685(17) . ?
P2 Cl2 1.9925(9) . ?
P2 Cl1 1.9973(9) . ?
P3 Cl3 1.9950(9) . ?
P3 Cl4 1.9964(9) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 C2 110.2(2) . . ?
O1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
O1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 111.0(2) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C2 109.3(2) . . ?
O2 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
P2 N1 P1 122.17(14) . . ?
P3 N2 P2 120.33(14) . . ?
P1 N3 P3 122.06(15) . . ?
C1 O1 P1 119.06(16) . . ?
C3 O2 P1 117.51(16) . . ?
O1 P1 O2 104.92(10) . . ?
O1 P1 N3 107.56(11) . . ?
O2 P1 N3 107.78(11) . . ?
O1 P1 N1 109.47(10) . . ?
O2 P1 N1 110.12(11) . . ?
N3 P1 N1 116.36(12) . . ?
N1 P2 N2 118.76(12) . . ?
N1 P2 Cl2 109.36(8) . . ?
N2 P2 Cl2 108.73(9) . . ?
N1 P2 Cl1 109.85(9) . . ?
N2 P2 Cl1 107.82(9) . . ?
Cl2 P2 Cl1 100.83(4) . . ?
N2 P3 N3 119.07(13) . . ?
N2 P3 Cl3 109.36(9) . . ?
N3 P3 Cl3 108.58(9) . . ?
N2 P3 Cl4 108.64(9) . . ?
N3 P3 Cl4 108.89(9) . . ?
Cl3 P3 Cl4 100.74(4) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
O1 C1 C2 C3 57.0(3) . . . . ?
C1 C2 C3 O2 -60.3(3) . . . . ?
C2 C1 O1 P1 -51.3(3) . . . . ?
C2 C3 O2 P1 57.8(2) . . . . ?
C1 O1 P1 O2 43.7(2) . . . . ?
C1 O1 P1 N3 158.27(19) . . . . ?
C1 O1 P1 N1 -74.4(2) . . . . ?
C3 O2 P1 O1 -46.7(2) . . . . ?
C3 O2 P1 N3 -161.15(18) . . . . ?
C3 O2 P1 N1 71.0(2) . . . . ?
P3 N3 P1 O1 134.03(15) . . . . ?
P3 N3 P1 O2 -113.32(16) . . . . ?
P3 N3 P1 N1 10.9(2) . . . . ?
P2 N1 P1 O1 -134.37(14) . . . . ?
P2 N1 P1 O2 110.78(15) . . . . ?
P2 N1 P1 N3 -12.21(19) . . . . ?
P1 N1 P2 N2 4.8(2) . . . . ?
P1 N1 P2 Cl2 130.31(13) . . . . ?
P1 N1 P2 Cl1 -119.90(14) . . . . ?
P3 N2 P2 N1 4.5(2) . . . . ?
P3 N2 P2 Cl2 -121.34(13) . . . . ?
P3 N2 P2 Cl1 130.16(13) . . . . ?
P2 N2 P3 N3 -5.8(2) . . . . ?
P2 N2 P3 Cl3 119.81(13) . . . . ?
P2 N2 P3 Cl4 -131.10(12) . . . . ?
P1 N3 P3 N2 -2.2(2) . . . . ?
P1 N3 P3 Cl3 -128.18(14) . . . . ?
P1 N3 P3 Cl4 122.99(14) . . . . ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    0.302
_refine_diff_density_min   -0.338
_refine_diff_density_rms    0.062
