 
data_2008src0009
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C5 H13 Cl3 N5 O P3'
_chemical_formula_weight          358.46
 
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            Monoclinic
_symmetry_space_group_name_H-M    P2(1)n
 
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                    18.3051(5)
_cell_length_b                    8.13900(10)
_cell_length_c                    39.2691(9)
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.6620(10)
_cell_angle_gamma                 90.00
_cell_volume                      5729.7(2)
_cell_formula_units_Z             16
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     14310
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.28
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.662
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2912
_exptl_absorpt_coefficient_mu     0.966
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7736
_exptl_absorpt_correction_T_max   0.9533
_exptl_absorpt_process_details    'SADABS (Sheldrick, 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_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             47265
_diffrn_reflns_av_R_equivalents   0.0757
_diffrn_reflns_av_sigmaI/netI     0.0922
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_h_max        23
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -50
_diffrn_reflns_limit_l_max        50
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          27.50
_reflns_number_total              11550
_reflns_number_gt                 7530
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction          'DENZO & COLLECT'
_computing_structure_solution     'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0522P)²+1.8622P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          11550
_refine_ls_number_parameters      649
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1003
_refine_ls_R_factor_gt            0.0542
_refine_ls_wR_factor_ref          0.1337
_refine_ls_wR_factor_gt           0.1145
_refine_ls_goodness_of_fit_ref    1.076
_refine_ls_restrained_S_all       1.076
_refine_ls_shift/su_max           0.026
_refine_ls_shift/su_mean          0.001
 
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
C20 C 0.1017(2) 0.4395(6) 0.04736(11) 0.0355(12) Uani 1 1 d . . .
H20A H 0.1005 0.5589 0.0440 0.053 Uiso 1 1 calc R . .
H20B H 0.1209 0.3870 0.0285 0.053 Uiso 1 1 calc R . .
H20C H 0.1342 0.4126 0.0697 0.053 Uiso 1 1 calc R . .
C1 C 0.7147(2) 0.4075(5) 0.12094(11) 0.0257(10) Uani 1 1 d . . .
H1A H 0.7672 0.3870 0.1193 0.031 Uiso 1 1 calc R . .
H1B H 0.7141 0.4976 0.1378 0.031 Uiso 1 1 calc R . .
C2 C 0.6696(2) 0.4564(5) 0.08559(10) 0.0233(10) Uani 1 1 d . . .
H2A H 0.6919 0.5555 0.0772 0.028 Uiso 1 1 calc R . .
H2B H 0.6712 0.3666 0.0688 0.028 Uiso 1 1 calc R . .
C3 C 0.5895(2) 0.4916(5) 0.08741(11) 0.0262(10) Uani 1 1 d . . .
H3A H 0.5873 0.5871 0.1028 0.031 Uiso 1 1 calc R . .
H3B H 0.5608 0.5190 0.0639 0.031 Uiso 1 1 calc R . .
C4 C 0.4335(2) -0.0985(6) 0.20208(11) 0.0322(12) Uani 1 1 d . . .
H4A H 0.4512 -0.0317 0.2232 0.039 Uiso 1 1 calc R . .
H4B H 0.4485 -0.2139 0.2076 0.039 Uiso 1 1 calc R . .
C5 C 0.3501(3) -0.0886(6) 0.19212(13) 0.0435(13) Uani 1 1 d . . .
H5A H 0.3349 0.0265 0.1882 0.065 Uiso 1 1 calc R . .
H5B H 0.3282 -0.1343 0.2109 0.065 Uiso 1 1 calc R . .
H5C H 0.3326 -0.1514 0.1707 0.065 Uiso 1 1 calc R . .
C6 C 0.2672(2) 0.4870(5) 0.12715(11) 0.0243(10) Uani 1 1 d . . .
H6A H 0.2642 0.3992 0.1095 0.029 Uiso 1 1 calc R . .
H6B H 0.2158 0.5156 0.1293 0.029 Uiso 1 1 calc R . .
C7 C 0.3112(2) 0.4254(5) 0.16202(11) 0.0237(10) Uani 1 1 d . . .
H7A H 0.3131 0.5125 0.1798 0.028 Uiso 1 1 calc R . .
H7B H 0.2857 0.3287 0.1695 0.028 Uiso 1 1 calc R . .
C8 C 0.3899(2) 0.3785(5) 0.15914(11) 0.0268(11) Uani 1 1 d . . .
H8A H 0.4185 0.3445 0.1822 0.032 Uiso 1 1 calc R . .
H8B H 0.3883 0.2844 0.1430 0.032 Uiso 1 1 calc R . .
C9 C 0.5486(2) 0.9865(5) 0.04554(10) 0.0231(10) Uani 1 1 d . . .
H9A H 0.5295 1.1004 0.0423 0.028 Uiso 1 1 calc R . .
H9B H 0.5292 0.9247 0.0239 0.028 Uiso 1 1 calc R . .
C10 C 0.6328(2) 0.9890(5) 0.05219(11) 0.0293(11) Uani 1 1 d . . .
H10A H 0.6522 1.0480 0.0739 0.044 Uiso 1 1 calc R . .
H10B H 0.6492 1.0445 0.0329 0.044 Uiso 1 1 calc R . .
H10C H 0.6518 0.8760 0.0541 0.044 Uiso 1 1 calc R . .
C11 C 0.1059(3) -0.1667(5) 0.10297(12) 0.0325(12) Uani 1 1 d . . .
H11A H 0.0718 -0.2449 0.0883 0.039 Uiso 1 1 calc R . .
H11B H 0.1368 -0.2298 0.1222 0.039 Uiso 1 1 calc R . .
C12 C 0.1564(2) -0.0876(5) 0.08122(11) 0.0302(11) Uani 1 1 d . . .
H12A H 0.1862 -0.1738 0.0725 0.036 Uiso 1 1 calc R . .
H12B H 0.1255 -0.0321 0.0609 0.036 Uiso 1 1 calc R . .
C13 C 0.2081(3) 0.0356(6) 0.10232(12) 0.0349(12) Uani 1 1 d . . .
H13A H 0.2422 -0.0219 0.1214 0.042 Uiso 1 1 calc R . .
H13B H 0.2388 0.0884 0.0873 0.042 Uiso 1 1 calc R . .
C14 C -0.0569(2) 0.4680(5) 0.20831(11) 0.0275(11) Uani 1 1 d . . .
H14A H -0.0367 0.5811 0.2112 0.033 Uiso 1 1 calc R . .
H14B H -0.0355 0.4050 0.2295 0.033 Uiso 1 1 calc R . .
C15 C -0.1401(2) 0.4735(6) 0.20387(11) 0.0327(12) Uani 1 1 d . . .
H15A H -0.1610 0.5413 0.1836 0.049 Uiso 1 1 calc R . .
H15B H -0.1534 0.5211 0.2247 0.049 Uiso 1 1 calc R . .
H15C H -0.1602 0.3619 0.2004 0.049 Uiso 1 1 calc R . .
C16 C -0.0979(2) 0.9744(5) 0.16451(11) 0.0284(11) Uani 1 1 d . . .
H16A H -0.0952 1.0653 0.1480 0.034 Uiso 1 1 calc R . .
H16B H -0.0643 1.0013 0.1869 0.034 Uiso 1 1 calc R . .
C17 C -0.1774(2) 0.9563(5) 0.16988(10) 0.0273(11) Uani 1 1 d . . .
H17A H -0.1792 0.8706 0.1876 0.033 Uiso 1 1 calc R . .
H17B H -0.1940 1.0612 0.1786 0.033 Uiso 1 1 calc R . .
C18 C -0.2297(2) 0.9098(5) 0.13617(11) 0.0291(11) Uani 1 1 d . . .
H18A H -0.2812 0.9001 0.1401 0.035 Uiso 1 1 calc R . .
H18B H -0.2289 0.9965 0.1185 0.035 Uiso 1 1 calc R . .
C19 C 0.0234(2) 0.3775(5) 0.04713(10) 0.0246(10) Uani 1 1 d . . .
H19A H -0.0101 0.4089 0.0250 0.030 Uiso 1 1 calc R . .
H19B H 0.0239 0.2562 0.0489 0.030 Uiso 1 1 calc R . .
N1 N 0.56932(18) 0.0926(4) 0.14341(8) 0.0200(8) Uani 1 1 d . . .
N2 N 0.5668(2) 0.1542(4) 0.21200(8) 0.0262(9) Uani 1 1 d . . .
N3 N 0.59757(18) 0.3964(4) 0.17013(8) 0.0181(8) Uani 1 1 d . . .
N4 N 0.5562(2) 0.3462(4) 0.10104(9) 0.0203(9) Uani 1 1 d . . .
N5 N 0.4686(2) -0.0387(5) 0.17376(9) 0.0242(9) Uani 1 1 d . . .
N6 N 0.42277(19) 0.7785(4) 0.10638(8) 0.0216(8) Uani 1 1 d . . .
N7 N 0.41701(19) 0.7293(4) 0.03654(8) 0.0226(8) Uani 1 1 d . . .
N8 N 0.38290(19) 0.4841(4) 0.07715(8) 0.0218(8) Uani 1 1 d . . .
N9 N 0.4272(2) 0.5187(4) 0.14622(9) 0.0213(8) Uani 1 1 d . . .
N10 N 0.5216(2) 0.9102(4) 0.07449(9) 0.0203(9) Uani 1 1 d . . .
N11 N 0.1552(2) 0.0344(4) 0.17547(9) 0.0325(10) Uani 1 1 d . . .
N12 N 0.07967(19) 0.2284(4) 0.21278(8) 0.0250(9) Uani 1 1 d . . .
N13 N 0.05525(18) 0.2569(4) 0.14201(8) 0.0204(8) Uani 1 1 d . . .
N14 N 0.0611(2) -0.0441(5) 0.11772(10) 0.0254(9) Uani 1 1 d . . .
N15 N -0.03521(19) 0.3905(4) 0.17792(9) 0.0206(8) Uani 1 1 d . . .
N16 N -0.10393(18) 0.5607(4) 0.11021(8) 0.0180(8) Uani 1 1 d . . .
N17 N -0.12062(18) 0.6034(4) 0.03977(8) 0.0186(8) Uani 1 1 d . . .
N18 N -0.1234(2) 0.8644(4) 0.08232(9) 0.0273(9) Uani 1 1 d . . .
N19 N -0.0735(2) 0.8203(5) 0.15066(9) 0.0237(9) Uani 1 1 d . . .
N20 N -0.0044(2) 0.4484(4) 0.07656(9) 0.0216(9) Uani 1 1 d . . .
O1 O 0.68238(14) 0.2575(3) 0.13293(7) 0.0194(6) Uani 1 1 d . . .
O2 O 0.30370(15) 0.6315(3) 0.11609(7) 0.0217(7) Uani 1 1 d . . .
O3 O 0.16661(15) 0.1623(3) 0.11706(8) 0.0279(7) Uani 1 1 d . . .
O4 O -0.20613(14) 0.7530(3) 0.12354(7) 0.0182(6) Uani 1 1 d . . .
P1 P 0.59957(6) 0.27127(13) 0.13830(3) 0.0165(2) Uani 1 1 d . . .
P2 P 0.55261(6) 0.03063(14) 0.17954(3) 0.0213(3) Uani 1 1 d . . .
P3 P 0.60125(6) 0.32772(13) 0.20777(3) 0.0196(3) Uani 1 1 d . . .
P4 P 0.38591(6) 0.60482(13) 0.10987(3) 0.0173(2) Uani 1 1 d . . .
P5 P 0.43671(6) 0.84575(13) 0.06994(3) 0.0194(3) Uani 1 1 d . . .
P6 P 0.37850(6) 0.55934(13) 0.03967(3) 0.0206(3) Uani 1 1 d . . .
P7 P 0.10855(6) 0.10557(13) 0.13946(3) 0.0185(3) Uani 1 1 d . . .
P8 P 0.04965(6) 0.33431(13) 0.17865(3) 0.0195(3) Uani 1 1 d . . .
P9 P 0.13805(6) 0.08743(14) 0.21131(3) 0.0235(3) Uani 1 1 d . . .
P10 P -0.12544(6) 0.74770(13) 0.11504(3) 0.0168(2) Uani 1 1 d . . .
P11 P -0.09198(6) 0.49317(13) 0.07353(3) 0.0180(3) Uani 1 1 d . . .
P12 P -0.12621(6) 0.79428(13) 0.04493(3) 0.0183(3) Uani 1 1 d . . .
Cl1 Cl 0.62325(7) -0.16210(14) 0.19459(3) 0.0374(3) Uani 1 1 d . . .
Cl2 Cl 0.55245(7) 0.48992(14) 0.23423(3) 0.0350(3) Uani 1 1 d . . .
Cl3 Cl 0.70627(6) 0.33342(15) 0.23578(3) 0.0366(3) Uani 1 1 d . . .
Cl4 Cl 0.37022(6) 1.04828(14) 0.05813(3) 0.0350(3) Uani 1 1 d . . .
Cl5 Cl 0.42122(7) 0.39563(13) 0.01106(3) 0.0334(3) Uani 1 1 d . . .
Cl6 Cl 0.27235(6) 0.56929(16) 0.01317(3) 0.0410(3) Uani 1 1 d . . .
Cl7 Cl 0.11300(7) 0.54499(14) 0.18382(3) 0.0379(3) Uani 1 1 d . . .
Cl8 Cl 0.23494(6) 0.14071(15) 0.24327(3) 0.0387(3) Uani 1 1 d . . .
Cl9 Cl 0.10595(7) -0.10719(14) 0.23603(3) 0.0399(3) Uani 1 1 d . . .
Cl10 Cl -0.15040(6) 0.28016(13) 0.06420(3) 0.0288(3) Uani 1 1 d . . .
Cl11 Cl -0.21474(6) 0.87564(14) 0.01080(3) 0.0345(3) Uani 1 1 d . . .
Cl12 Cl -0.04403(7) 0.90561(14) 0.02576(3) 0.0347(3) Uani 1 1 d . . .
H4N H 0.514(2) 0.343(5) 0.0990(11) 0.021(14) Uiso 1 1 d . . .
H5N H 0.460(2) -0.084(5) 0.1566(10) 0.022(13) Uiso 1 1 d . . .
H9N H 0.475(2) 0.515(4) 0.1498(10) 0.015(12) Uiso 1 1 d . . .
H10N H 0.533(2) 0.956(5) 0.0906(10) 0.021(13) Uiso 1 1 d . . .
H14N H 0.026(2) -0.016(4) 0.1048(10) 0.008(11) Uiso 1 1 d . . .
H15N H -0.049(2) 0.442(5) 0.1596(11) 0.034(14) Uiso 1 1 d . . .
H19N H -0.032(2) 0.822(4) 0.1499(10) 0.005(11) Uiso 1 1 d . . .
H20N H 0.010(2) 0.404(4) 0.0937(9) 0.006(11) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C20 C19 1.517(6) . ?
C1 O1 1.475(5) . ?
C1 C2 1.519(5) . ?
C2 C3 1.509(6) . ?
C3 N4 1.480(5) . ?
C4 N5 1.475(5) . ?
C4 C5 1.500(6) . ?
C6 O2 1.461(5) . ?
C6 C7 1.526(5) . ?
C7 C8 1.517(6) . ?
C8 N9 1.472(5) . ?
C9 N10 1.466(5) . ?
C9 C10 1.511(5) . ?
C11 N14 1.482(5) . ?
C11 C12 1.523(6) . ?
C12 C13 1.507(6) . ?
C13 O3 1.467(5) . ?
C14 N15 1.474(5) . ?
C14 C15 1.497(6) . ?
C16 N19 1.472(5) . ?
C16 C17 1.521(6) . ?
C17 C18 1.516(5) . ?
C18 O4 1.465(5) . ?
C19 N20 1.472(5) . ?
N1 P1 1.583(3) . ?
N1 P2 1.593(3) . ?
N2 P3 1.569(3) . ?
N2 P2 1.603(3) . ?
N3 P3 1.569(3) . ?
N3 P1 1.618(3) . ?
N4 P1 1.635(3) . ?
N5 P2 1.611(4) . ?
N6 P4 1.584(3) . ?
N6 P5 1.600(3) . ?
N7 P6 1.569(3) . ?
N7 P5 1.599(3) . ?
N8 P6 1.581(3) . ?
N8 P4 1.609(3) . ?
N9 P4 1.632(3) . ?
N10 P5 1.615(4) . ?
N11 P9 1.563(4) . ?
N11 P7 1.605(3) . ?
N12 P9 1.577(3) . ?
N12 P8 1.595(3) . ?
N13 P7 1.587(3) . ?
N13 P8 1.593(3) . ?
N14 P7 1.633(4) . ?
N15 P8 1.614(4) . ?
N16 P10 1.593(3) . ?
N16 P11 1.597(3) . ?
N17 P12 1.573(3) . ?
N17 P11 1.599(3) . ?
N18 P12 1.566(3) . ?
N18 P10 1.605(3) . ?
N19 P10 1.635(4) . ?
N20 P11 1.625(4) . ?
O1 P1 1.576(3) . ?
O2 P4 1.587(3) . ?
O3 P7 1.579(3) . ?
O4 P10 1.579(3) . ?
P2 Cl1 2.0427(16) . ?
P3 Cl2 1.9989(16) . ?
P3 Cl3 2.0132(15) . ?
P5 Cl4 2.0458(15) . ?
P6 Cl5 2.0012(16) . ?
P6 Cl6 2.0118(15) . ?
P8 Cl7 2.0568(16) . ?
P9 Cl8 2.0023(15) . ?
P9 Cl9 2.0070(17) . ?
P11 Cl10 2.0311(15) . ?
P12 Cl11 1.9959(15) . ?
P12 Cl12 2.0270(16) . ?
 
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 109.2(3) . . ?
C3 C2 C1 111.2(4) . . ?
N4 C3 C2 109.9(3) . . ?
N5 C4 C5 111.2(3) . . ?
O2 C6 C7 110.0(3) . . ?
C8 C7 C6 110.6(4) . . ?
N9 C8 C7 110.1(3) . . ?
N10 C9 C10 111.3(3) . . ?
N14 C11 C12 112.4(4) . . ?
C13 C12 C11 111.0(4) . . ?
O3 C13 C12 111.6(4) . . ?
N15 C14 C15 110.7(3) . . ?
N19 C16 C17 109.8(3) . . ?
C18 C17 C16 110.8(4) . . ?
O4 C18 C17 109.7(3) . . ?
N20 C19 C20 110.0(3) . . ?
P1 N1 P2 122.6(2) . . ?
P3 N2 P2 119.0(2) . . ?
P3 N3 P1 120.0(2) . . ?
C3 N4 P1 117.5(3) . . ?
C4 N5 P2 123.9(3) . . ?
P4 N6 P5 122.0(2) . . ?
P6 N7 P5 119.2(2) . . ?
P6 N8 P4 119.6(2) . . ?
C8 N9 P4 118.0(3) . . ?
C9 N10 P5 121.3(3) . . ?
P9 N11 P7 121.8(2) . . ?
P9 N12 P8 118.9(2) . . ?
P7 N13 P8 121.11(19) . . ?
C11 N14 P7 115.4(3) . . ?
C14 N15 P8 121.5(3) . . ?
P10 N16 P11 121.2(2) . . ?
P12 N17 P11 117.79(19) . . ?
P12 N18 P10 122.2(2) . . ?
C16 N19 P10 117.2(3) . . ?
C19 N20 P11 121.6(3) . . ?
C1 O1 P1 116.3(2) . . ?
C6 O2 P4 116.1(2) . . ?
C13 O3 P7 118.3(3) . . ?
C18 O4 P10 116.5(2) . . ?
O1 P1 N1 108.81(17) . . ?
O1 P1 N3 108.70(16) . . ?
N1 P1 N3 114.63(18) . . ?
O1 P1 N4 102.28(18) . . ?
N1 P1 N4 109.70(18) . . ?
N3 P1 N4 111.95(18) . . ?
N1 P2 N2 118.70(18) . . ?
N1 P2 N5 109.58(17) . . ?
N2 P2 N5 109.2(2) . . ?
N1 P2 Cl1 106.06(14) . . ?
N2 P2 Cl1 105.11(14) . . ?
N5 P2 Cl1 107.60(15) . . ?
N2 P3 N3 118.60(17) . . ?
N2 P3 Cl2 107.92(15) . . ?
N3 P3 Cl2 108.41(14) . . ?
N2 P3 Cl3 108.85(14) . . ?
N3 P3 Cl3 111.16(13) . . ?
Cl2 P3 Cl3 100.28(7) . . ?
N6 P4 O2 108.95(17) . . ?
N6 P4 N8 114.98(18) . . ?
O2 P4 N8 109.03(16) . . ?
N6 P4 N9 109.19(18) . . ?
O2 P4 N9 102.09(18) . . ?
N8 P4 N9 111.79(18) . . ?
N7 P5 N6 118.72(18) . . ?
N7 P5 N10 109.6(2) . . ?
N6 P5 N10 109.62(18) . . ?
N7 P5 Cl4 105.45(13) . . ?
N6 P5 Cl4 106.46(14) . . ?
N10 P5 Cl4 106.17(14) . . ?
N7 P6 N8 118.39(17) . . ?
N7 P6 Cl5 108.08(15) . . ?
N8 P6 Cl5 108.21(14) . . ?
N7 P6 Cl6 109.04(13) . . ?
N8 P6 Cl6 111.06(14) . . ?
Cl5 P6 Cl6 100.52(7) . . ?
O3 P7 N13 107.45(17) . . ?
O3 P7 N11 107.36(19) . . ?
N13 P7 N11 116.65(18) . . ?
O3 P7 N14 105.88(18) . . ?
N13 P7 N14 110.05(18) . . ?
N11 P7 N14 108.9(2) . . ?
N13 P8 N12 118.11(18) . . ?
N13 P8 N15 109.47(17) . . ?
N12 P8 N15 109.6(2) . . ?
N13 P8 Cl7 106.33(14) . . ?
N12 P8 Cl7 106.02(14) . . ?
N15 P8 Cl7 106.66(14) . . ?
N11 P9 N12 119.64(18) . . ?
N11 P9 Cl8 108.11(15) . . ?
N12 P9 Cl8 109.89(14) . . ?
N11 P9 Cl9 110.45(16) . . ?
N12 P9 Cl9 106.83(15) . . ?
Cl8 P9 Cl9 100.17(7) . . ?
O4 P10 N16 108.39(16) . . ?
O4 P10 N18 109.12(17) . . ?
N16 P10 N18 115.07(18) . . ?
O4 P10 N19 102.51(18) . . ?
N16 P10 N19 109.41(18) . . ?
N18 P10 N19 111.54(19) . . ?
N16 P11 N17 118.23(17) . . ?
N16 P11 N20 108.90(17) . . ?
N17 P11 N20 109.87(19) . . ?
N16 P11 Cl10 107.06(13) . . ?
N17 P11 Cl10 104.89(12) . . ?
N20 P11 Cl10 107.30(14) . . ?
N18 P12 N17 119.36(18) . . ?
N18 P12 Cl11 112.17(15) . . ?
N17 P12 Cl11 107.83(12) . . ?
N18 P12 Cl12 107.38(15) . . ?
N17 P12 Cl12 108.73(14) . . ?
Cl11 P12 Cl12 99.50(7) . . ?
 
_diffrn_measured_fraction_theta_max    0.877
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.877
_refine_diff_density_max    0.714
_refine_diff_density_min   -0.582
_refine_diff_density_rms    0.119
