data_2007src0927
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H15 Cl3 N5 O P3'
_chemical_formula_weight          420.53
 
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)
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    9.68270(10)
_cell_length_b                    22.3776(2)
_cell_length_c                    16.0124(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.8460(10)
_cell_angle_gamma                 90.00
_cell_volume                      3467.70(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     57249
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.611
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1712
_exptl_absorpt_coefficient_mu     0.812
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8545
_exptl_absorpt_correction_T_max   0.9683
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius APEX2 Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             35212
_diffrn_reflns_av_R_equivalents   0.0323
_diffrn_reflns_av_sigmaI/netI     0.0436
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -29
_diffrn_reflns_limit_k_max        28
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.01
_diffrn_reflns_theta_max          27.50
_reflns_number_total              15188
_reflns_number_gt                 14428
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 2003)'
_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)+(0.0197P)²+2.3106P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.44(3)
_refine_ls_number_reflns          15188
_refine_ls_number_parameters      814
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0345
_refine_ls_R_factor_gt            0.0316
_refine_ls_wR_factor_ref          0.0714
_refine_ls_wR_factor_gt           0.0696
_refine_ls_goodness_of_fit_ref    1.034
_refine_ls_restrained_S_all       1.034
_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 1.0396(4) 0.23800(13) 0.2323(2) 0.0339(7) Uani 1 1 d . . .
H1A H 0.9446 0.2528 0.2252 0.051 Uiso 1 1 calc R . .
H1B H 1.0827 0.2364 0.1778 0.051 Uiso 1 1 calc R . .
H1C H 1.0925 0.2650 0.2694 0.051 Uiso 1 1 calc R . .
C2 C 0.9763(3) 0.17593(14) 0.35196(18) 0.0277(6) Uani 1 1 d . . .
H2A H 0.8753 0.1821 0.3455 0.033 Uiso 1 1 calc R . .
H2B H 1.0146 0.2089 0.3868 0.033 Uiso 1 1 calc R . .
C3 C 1.0038(3) 0.11752(14) 0.39571(17) 0.0270(6) Uani 1 1 d . . .
H3A H 1.1046 0.1124 0.4050 0.032 Uiso 1 1 calc R . .
H3B H 0.9608 0.1182 0.4510 0.032 Uiso 1 1 calc R . .
C4 C 0.9475(3) 0.06555(14) 0.34605(18) 0.0275(6) Uani 1 1 d . . .
H4A H 0.9694 0.0278 0.3759 0.033 Uiso 1 1 calc R . .
H4B H 0.8457 0.0690 0.3398 0.033 Uiso 1 1 calc R . .
C5 C 0.6586(3) 0.12440(14) -0.06340(17) 0.0241(6) Uani 1 1 d . . .
C6 C 0.7269(3) 0.10612(14) -0.1320(2) 0.0299(7) Uani 1 1 d . . .
H6 H 0.8152 0.0877 -0.1264 0.036 Uiso 1 1 calc R . .
C7 C 0.6637(3) 0.11514(15) -0.2110(2) 0.0339(7) Uani 1 1 d . . .
H7 H 0.7100 0.1031 -0.2597 0.041 Uiso 1 1 calc R . .
C8 C 0.5362(3) 0.14098(15) -0.21865(19) 0.0306(7) Uani 1 1 d . . .
H8 H 0.4933 0.1463 -0.2723 0.037 Uiso 1 1 calc R . .
C9 C 0.4704(3) 0.1592(2) -0.1484(2) 0.0465(10) Uani 1 1 d . . .
H9 H 0.3821 0.1775 -0.1539 0.056 Uiso 1 1 calc R . .
C10 C 0.5310(3) 0.1512(2) -0.0688(2) 0.0473(10) Uani 1 1 d . . .
H10 H 0.4856 0.1638 -0.0202 0.057 Uiso 1 1 calc R . .
C11 C 0.5927(3) 0.28774(14) 0.3817(2) 0.0320(7) Uani 1 1 d . . .
H11A H 0.6854 0.2711 0.3919 0.048 Uiso 1 1 calc R . .
H11B H 0.5449 0.2902 0.4347 0.048 Uiso 1 1 calc R . .
H11C H 0.6001 0.3278 0.3576 0.048 Uiso 1 1 calc R . .
C12 C 0.5790(3) 0.24467(14) 0.24109(17) 0.0247(6) Uani 1 1 d . . .
H12A H 0.6704 0.2252 0.2482 0.030 Uiso 1 1 calc R . .
H12B H 0.5939 0.2854 0.2191 0.030 Uiso 1 1 calc R . .
C13 C 0.4907(3) 0.20945(13) 0.17855(17) 0.0238(6) Uani 1 1 d . . .
H13A H 0.4017 0.2304 0.1683 0.029 Uiso 1 1 calc R . .
H13B H 0.5384 0.2070 0.1249 0.029 Uiso 1 1 calc R . .
C14 C 0.4632(3) 0.14700(13) 0.21025(17) 0.0242(6) Uani 1 1 d . . .
H14A H 0.4098 0.1244 0.1670 0.029 Uiso 1 1 calc R . .
H14B H 0.5522 0.1261 0.2207 0.029 Uiso 1 1 calc R . .
C15 C 0.1578(3) 0.15689(13) 0.63225(16) 0.0196(5) Uani 1 1 d . . .
C16 C 0.1830(3) 0.10037(13) 0.66344(19) 0.0264(6) Uani 1 1 d . . .
H16 H 0.2268 0.0710 0.6306 0.032 Uiso 1 1 calc R . .
C17 C 0.1430(3) 0.08728(16) 0.7437(2) 0.0339(7) Uani 1 1 d . . .
H17 H 0.1606 0.0488 0.7667 0.041 Uiso 1 1 calc R . .
C18 C 0.0779(3) 0.13001(16) 0.7899(2) 0.0322(7) Uani 1 1 d . . .
H18 H 0.0503 0.1208 0.8448 0.039 Uiso 1 1 calc R . .
C19 C 0.0521(3) 0.18627(16) 0.75713(19) 0.0320(7) Uani 1 1 d . . .
H19 H 0.0062 0.2153 0.7895 0.038 Uiso 1 1 calc R . .
C20 C 0.0930(3) 0.20065(14) 0.67734(19) 0.0267(6) Uani 1 1 d . . .
H20 H 0.0769 0.2393 0.6545 0.032 Uiso 1 1 calc R . .
C21 C -0.2579(3) 0.27893(15) 0.7235(2) 0.0377(8) Uani 1 1 d . . .
H21A H -0.2682 0.2429 0.7575 0.057 Uiso 1 1 calc R . .
H21B H -0.2025 0.2696 0.6751 0.057 Uiso 1 1 calc R . .
H21C H -0.3493 0.2931 0.7044 0.057 Uiso 1 1 calc R . .
C22 C -0.2659(3) 0.34019(15) 0.84943(19) 0.0312(7) Uani 1 1 d . . .
H22A H -0.2839 0.3029 0.8805 0.037 Uiso 1 1 calc R . .
H22B H -0.3563 0.3578 0.8323 0.037 Uiso 1 1 calc R . .
C23 C -0.1885(3) 0.38359(17) 0.90667(19) 0.0350(7) Uani 1 1 d . . .
H23A H -0.2457 0.3926 0.9552 0.042 Uiso 1 1 calc R . .
H23B H -0.1020 0.3646 0.9279 0.042 Uiso 1 1 calc R . .
C24 C -0.1540(3) 0.44108(15) 0.86299(19) 0.0320(7) Uani 1 1 d . . .
H24A H -0.2406 0.4614 0.8447 0.038 Uiso 1 1 calc R . .
H24B H -0.1036 0.4678 0.9027 0.038 Uiso 1 1 calc R . .
C25 C 0.1501(3) 0.40836(14) 0.45109(17) 0.0234(6) Uani 1 1 d . . .
C26 C 0.2339(3) 0.36701(15) 0.4137(2) 0.0299(7) Uani 1 1 d . . .
H26 H 0.2645 0.3323 0.4431 0.036 Uiso 1 1 calc R . .
C27 C 0.2725(3) 0.37736(18) 0.3318(2) 0.0390(8) Uani 1 1 d . . .
H27 H 0.3298 0.3495 0.3046 0.047 Uiso 1 1 calc R . .
C28 C 0.2272(3) 0.42824(18) 0.2904(2) 0.0397(8) Uani 1 1 d . . .
H28 H 0.2547 0.4356 0.2350 0.048 Uiso 1 1 calc R . .
C29 C 0.1422(3) 0.46840(17) 0.3292(2) 0.0370(8) Uani 1 1 d . . .
H29 H 0.1108 0.5030 0.3000 0.044 Uiso 1 1 calc R . .
C30 C 0.1025(3) 0.45881(14) 0.4103(2) 0.0286(7) Uani 1 1 d . . .
H30 H 0.0438 0.4863 0.4371 0.034 Uiso 1 1 calc R . .
C31 C -0.7287(4) 0.32528(14) 0.8418(2) 0.0368(8) Uani 1 1 d . . .
H31A H -0.7692 0.2987 0.7990 0.055 Uiso 1 1 calc R . .
H31B H -0.7829 0.3230 0.8924 0.055 Uiso 1 1 calc R . .
H31C H -0.6333 0.3129 0.8550 0.055 Uiso 1 1 calc R . .
C32 C -0.6628(3) 0.39191(14) 0.72908(18) 0.0267(6) Uani 1 1 d . . .
H32A H -0.7039 0.3619 0.6902 0.032 Uiso 1 1 calc R . .
H32B H -0.5632 0.3828 0.7368 0.032 Uiso 1 1 calc R . .
C33 C -0.6796(3) 0.45382(13) 0.69081(18) 0.0274(6) Uani 1 1 d . . .
H33A H -0.6295 0.4555 0.6379 0.033 Uiso 1 1 calc R . .
H33B H -0.7786 0.4613 0.6775 0.033 Uiso 1 1 calc R . .
C34 C -0.6247(3) 0.50229(14) 0.74925(19) 0.0275(6) Uani 1 1 d . . .
H34A H -0.5253 0.4956 0.7624 0.033 Uiso 1 1 calc R . .
H34B H -0.6354 0.5419 0.7223 0.033 Uiso 1 1 calc R . .
C35 C -0.3684(3) 0.44544(12) 1.14951(18) 0.0209(6) Uani 1 1 d . . .
C36 C -0.4378(3) 0.47412(15) 1.21171(19) 0.0289(7) Uani 1 1 d . . .
H36 H -0.5183 0.4971 1.1995 0.035 Uiso 1 1 calc R . .
C37 C -0.3850(3) 0.46796(16) 1.2934(2) 0.0371(8) Uani 1 1 d . . .
H37 H -0.4318 0.4865 1.3377 0.045 Uiso 1 1 calc R . .
C38 C -0.2673(3) 0.43586(16) 1.3111(2) 0.0360(8) Uani 1 1 d . . .
H38 H -0.2326 0.4327 1.3671 0.043 Uiso 1 1 calc R . .
C39 C -0.1986(3) 0.40794(15) 1.2469(2) 0.0332(7) Uani 1 1 d . . .
H39 H -0.1167 0.3858 1.2592 0.040 Uiso 1 1 calc R . .
C40 C -0.2490(3) 0.41229(14) 1.16494(19) 0.0267(6) Uani 1 1 d . . .
H40 H -0.2032 0.3931 1.1207 0.032 Uiso 1 1 calc R . .
N1 N 1.1364(2) 0.11838(11) 0.14163(14) 0.0219(5) Uani 1 1 d . . .
N2 N 0.9772(2) 0.12917(11) -0.00058(14) 0.0225(5) Uani 1 1 d . . .
N3 N 0.8601(2) 0.13058(11) 0.15117(14) 0.0227(5) Uani 1 1 d . . .
N4 N 1.0380(3) 0.17802(10) 0.26885(15) 0.0229(5) Uani 1 1 d . . .
N5 N 1.0084(3) 0.06457(12) 0.26307(16) 0.0244(5) Uani 1 1 d . . .
N6 N 0.5810(2) 0.14959(11) 0.40766(14) 0.0217(5) Uani 1 1 d . . .
N7 N 0.4544(2) 0.14067(10) 0.55641(14) 0.0204(5) Uani 1 1 d . . .
N8 N 0.3345(2) 0.20439(10) 0.42885(14) 0.0204(5) Uani 1 1 d . . .
N9 N 0.5139(2) 0.24877(10) 0.32328(14) 0.0208(5) Uani 1 1 d . . .
N10 N 0.3855(3) 0.14838(10) 0.28790(15) 0.0207(5) Uani 1 1 d . . .
N11 N -0.2698(2) 0.41557(11) 0.67576(15) 0.0243(5) Uani 1 1 d . . .
N12 N -0.1439(2) 0.42245(12) 0.52784(15) 0.0291(6) Uani 1 1 d . . .
N13 N -0.0193(2) 0.36310(10) 0.65827(14) 0.0200(5) Uani 1 1 d . . .
N14 N -0.1886(2) 0.32561(10) 0.77379(15) 0.0232(5) Uani 1 1 d . . .
N15 N -0.0679(2) 0.43035(11) 0.78926(15) 0.0214(5) Uani 1 1 d . . .
N16 N -0.8340(2) 0.43962(11) 0.94062(15) 0.0236(5) Uani 1 1 d . . .
N17 N -0.6751(2) 0.42946(11) 1.08317(14) 0.0226(5) Uani 1 1 d . . .
N18 N -0.5563(2) 0.42949(11) 0.93206(14) 0.0205(5) Uani 1 1 d . . .
N19 N -0.7296(2) 0.38739(10) 0.81028(15) 0.0231(5) Uani 1 1 d . . .
N20 N -0.7029(3) 0.50043(11) 0.82617(16) 0.0235(5) Uani 1 1 d . . .
O1 O 0.7145(2) 0.11326(10) 0.01851(13) 0.0295(5) Uani 1 1 d . . .
O2 O 0.19384(19) 0.17000(9) 0.54927(11) 0.0205(4) Uani 1 1 d . . .
O3 O 0.11748(19) 0.39853(9) 0.53549(12) 0.0224(4) Uani 1 1 d . . .
O4 O -0.41460(18) 0.45181(9) 1.06468(12) 0.0218(4) Uani 1 1 d . . .
P1 P 1.00726(7) 0.12249(3) 0.20225(4) 0.01812(14) Uani 1 1 d . . .
P2 P 1.12401(7) 0.12747(3) 0.04479(4) 0.01924(14) Uani 1 1 d . . .
P3 P 0.84934(7) 0.14462(3) 0.05508(5) 0.02022(15) Uani 1 1 d . . .
P4 P 0.45333(7) 0.18707(3) 0.36544(4) 0.01698(13) Uani 1 1 d . . .
P5 P 0.58599(7) 0.13047(3) 0.50138(4) 0.01767(14) Uani 1 1 d . . .
P6 P 0.34394(7) 0.18836(3) 0.52376(4) 0.01728(13) Uani 1 1 d . . .
P7 P -0.13612(7) 0.38373(3) 0.71996(4) 0.01696(13) Uani 1 1 d . . .
P8 P -0.27171(7) 0.43653(3) 0.58336(5) 0.01992(14) Uani 1 1 d . . .
P9 P -0.02904(7) 0.37723(3) 0.56218(4) 0.01886(14) Uani 1 1 d . . .
P10 P -0.70224(7) 0.43953(3) 0.88157(4) 0.01854(14) Uani 1 1 d . . .
P11 P -0.82159(7) 0.42745(3) 1.03677(5) 0.02030(15) Uani 1 1 d . . .
P12 P -0.54455(7) 0.41725(3) 1.02761(4) 0.01813(14) Uani 1 1 d . . .
Cl1 Cl 1.22373(7) 0.20355(3) 0.01391(5) 0.02632(15) Uani 1 1 d . . .
Cl2 Cl 1.23951(8) 0.06612(3) -0.01038(5) 0.02872(15) Uani 1 1 d . . .
Cl3 Cl 0.80569(8) 0.23256(3) 0.03532(5) 0.03074(16) Uani 1 1 d . . .
Cl4 Cl 0.64096(7) 0.04458(3) 0.51352(5) 0.02806(15) Uani 1 1 d . . .
Cl5 Cl 0.75129(7) 0.16906(4) 0.56066(5) 0.03060(16) Uani 1 1 d . . .
Cl6 Cl 0.37763(8) 0.26384(3) 0.59191(5) 0.02859(15) Uani 1 1 d . . .
Cl7 Cl -0.30683(9) 0.52445(3) 0.57623(7) 0.0454(2) Uani 1 1 d . . .
Cl8 Cl -0.44344(7) 0.40523(3) 0.52401(4) 0.02570(15) Uani 1 1 d . . .
Cl9 Cl -0.05305(8) 0.30012(4) 0.49776(5) 0.03542(18) Uani 1 1 d . . .
Cl10 Cl -0.91046(7) 0.34795(3) 1.06391(5) 0.02924(16) Uani 1 1 d . . .
Cl11 Cl -0.94974(7) 0.48219(3) 1.09451(5) 0.02947(16) Uani 1 1 d . . .
Cl12 Cl -0.48901(7) 0.33057(3) 1.04687(5) 0.02810(15) Uani 1 1 d . . .
H20N H -0.729(4) 0.5292(17) 0.851(2) 0.035(10) Uiso 1 1 d . . .
H5N H 1.013(3) 0.0324(15) 0.245(2) 0.022(9) Uiso 1 1 d . . .
H15N H 0.010(3) 0.4177(14) 0.800(2) 0.025(9) Uiso 1 1 d . . .
H10N H 0.304(4) 0.1545(14) 0.281(2) 0.027(9) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N4 1.465(4) . ?
C2 N4 1.477(4) . ?
C2 C3 1.503(4) . ?
C3 C4 1.501(4) . ?
C4 N5 1.471(4) . ?
C5 C6 1.363(4) . ?
C5 C10 1.373(4) . ?
C5 O1 1.425(3) . ?
C6 C7 1.403(4) . ?
C7 C8 1.365(4) . ?
C8 C9 1.373(5) . ?
C9 C10 1.396(4) . ?
C11 N9 1.474(3) . ?
C12 N9 1.480(4) . ?
C12 C13 1.517(4) . ?
C13 C14 1.513(4) . ?
C14 N10 1.474(4) . ?
C15 C16 1.379(4) . ?
C15 C20 1.379(4) . ?
C15 O2 1.416(3) . ?
C16 C17 1.385(4) . ?
C17 C18 1.375(5) . ?
C18 C19 1.384(5) . ?
C19 C20 1.387(4) . ?
C21 N14 1.468(4) . ?
C22 N14 1.481(4) . ?
C22 C23 1.517(4) . ?
C23 C24 1.507(5) . ?
C24 N15 1.486(4) . ?
C25 C30 1.377(4) . ?
C25 C26 1.380(4) . ?
C25 O3 1.415(3) . ?
C26 C27 1.394(4) . ?
C27 C28 1.382(5) . ?
C28 C29 1.380(5) . ?
C29 C30 1.382(4) . ?
C31 N19 1.479(4) . ?
C32 N19 1.474(4) . ?
C32 C33 1.521(4) . ?
C33 C34 1.517(4) . ?
C34 N20 1.467(4) . ?
C35 C36 1.378(4) . ?
C35 C40 1.389(4) . ?
C35 O4 1.423(3) . ?
C36 C37 1.395(4) . ?
C37 C38 1.369(5) . ?
C38 C39 1.390(5) . ?
C39 C40 1.389(4) . ?
N1 P2 1.565(2) . ?
N1 P1 1.610(2) . ?
N2 P2 1.576(2) . ?
N2 P3 1.587(2) . ?
N3 P3 1.570(2) . ?
N3 P1 1.630(2) . ?
N4 P1 1.658(2) . ?
N5 P1 1.621(3) . ?
N6 P5 1.560(2) . ?
N6 P4 1.623(2) . ?
N7 P6 1.588(2) . ?
N7 P5 1.589(2) . ?
N8 P6 1.561(2) . ?
N8 P4 1.606(2) . ?
N9 P4 1.653(2) . ?
N10 P4 1.634(2) . ?
N11 P8 1.552(2) . ?
N11 P7 1.620(2) . ?
N12 P8 1.578(3) . ?
N12 P9 1.589(2) . ?
N13 P9 1.571(2) . ?
N13 P7 1.594(2) . ?
N14 P7 1.650(2) . ?
N15 P7 1.646(2) . ?
N16 P11 1.564(2) . ?
N16 P10 1.612(2) . ?
N17 P11 1.580(2) . ?
N17 P12 1.593(2) . ?
N18 P12 1.555(2) . ?
N18 P10 1.621(2) . ?
N19 P10 1.648(2) . ?
N20 P10 1.626(2) . ?
O1 P3 1.578(2) . ?
O2 P6 1.5768(19) . ?
O3 P9 1.569(2) . ?
O4 P12 1.5766(19) . ?
P2 Cl2 1.9950(10) . ?
P2 Cl1 2.0263(10) . ?
P2 P3 2.6974(10) . ?
P3 Cl3 2.0355(10) . ?
P5 Cl4 2.0021(10) . ?
P5 Cl5 2.0275(9) . ?
P6 Cl6 2.0315(10) . ?
P8 Cl7 1.9993(10) . ?
P8 Cl8 2.0142(9) . ?
P9 Cl9 2.0198(10) . ?
P11 Cl11 1.9922(10) . ?
P11 Cl10 2.0292(10) . ?
P12 Cl12 2.0336(10) . ?
 
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
N4 C2 C3 112.1(2) . . ?
C4 C3 C2 111.8(2) . . ?
N5 C4 C3 109.9(2) . . ?
C6 C5 C10 122.6(3) . . ?
C6 C5 O1 120.6(3) . . ?
C10 C5 O1 116.7(3) . . ?
C5 C6 C7 118.3(3) . . ?
C8 C7 C6 120.6(3) . . ?
C7 C8 C9 119.7(3) . . ?
C8 C9 C10 121.1(3) . . ?
C5 C10 C9 117.7(3) . . ?
N9 C12 C13 111.8(2) . . ?
C14 C13 C12 111.1(2) . . ?
N10 C14 C13 111.3(2) . . ?
C16 C15 C20 122.7(3) . . ?
C16 C15 O2 118.9(3) . . ?
C20 C15 O2 118.3(2) . . ?
C15 C16 C17 118.6(3) . . ?
C18 C17 C16 120.0(3) . . ?
C17 C18 C19 120.6(3) . . ?
C18 C19 C20 120.5(3) . . ?
C15 C20 C19 117.7(3) . . ?
N14 C22 C23 112.5(2) . . ?
C24 C23 C22 112.3(2) . . ?
N15 C24 C23 111.7(3) . . ?
C30 C25 C26 122.5(3) . . ?
C30 C25 O3 120.0(3) . . ?
C26 C25 O3 117.5(3) . . ?
C25 C26 C27 118.4(3) . . ?
C28 C27 C26 119.8(3) . . ?
C29 C28 C27 120.4(3) . . ?
C28 C29 C30 120.7(3) . . ?
C25 C30 C29 118.3(3) . . ?
N19 C32 C33 112.0(2) . . ?
C34 C33 C32 111.8(2) . . ?
N20 C34 C33 108.5(2) . . ?
C36 C35 C40 122.9(3) . . ?
C36 C35 O4 119.8(3) . . ?
C40 C35 O4 117.2(3) . . ?
C35 C36 C37 117.3(3) . . ?
C38 C37 C36 121.6(3) . . ?
C37 C38 C39 119.8(3) . . ?
C40 C39 C38 120.3(3) . . ?
C39 C40 C35 118.1(3) . . ?
P2 N1 P1 123.63(14) . . ?
P2 N2 P3 117.05(15) . . ?
P3 N3 P1 122.89(15) . . ?
C1 N4 C2 113.5(2) . . ?
C1 N4 P1 115.7(2) . . ?
C2 N4 P1 119.09(19) . . ?
C4 N5 P1 122.4(2) . . ?
P5 N6 P4 122.84(15) . . ?
P6 N7 P5 117.25(14) . . ?
P6 N8 P4 122.64(14) . . ?
C11 N9 C12 112.0(2) . . ?
C11 N9 P4 114.71(19) . . ?
C12 N9 P4 118.58(19) . . ?
C14 N10 P4 116.66(19) . . ?
P8 N11 P7 122.32(15) . . ?
P8 N12 P9 119.02(15) . . ?
P9 N13 P7 121.85(14) . . ?
C21 N14 C22 111.8(2) . . ?
C21 N14 P7 114.7(2) . . ?
C22 N14 P7 115.2(2) . . ?
C24 N15 P7 114.50(19) . . ?
P11 N16 P10 122.69(14) . . ?
P11 N17 P12 116.68(14) . . ?
P12 N18 P10 123.40(14) . . ?
C32 N19 C31 111.6(2) . . ?
C32 N19 P10 119.8(2) . . ?
C31 N19 P10 115.5(2) . . ?
C34 N20 P10 119.3(2) . . ?
C5 O1 P3 123.32(17) . . ?
C15 O2 P6 123.69(16) . . ?
C25 O3 P9 122.62(16) . . ?
C35 O4 P12 122.19(16) . . ?
N1 P1 N5 109.04(13) . . ?
N1 P1 N3 112.78(12) . . ?
N5 P1 N3 112.27(13) . . ?
N1 P1 N4 107.67(13) . . ?
N5 P1 N4 102.43(13) . . ?
N3 P1 N4 112.05(13) . . ?
N1 P2 N2 119.95(12) . . ?
N1 P2 Cl2 108.86(10) . . ?
N2 P2 Cl2 108.82(10) . . ?
N1 P2 Cl1 109.22(9) . . ?
N2 P2 Cl1 107.28(10) . . ?
Cl2 P2 Cl1 101.06(4) . . ?
N1 P2 P3 90.12(9) . . ?
N2 P2 P3 31.60(9) . . ?
Cl2 P2 P3 133.85(4) . . ?
Cl1 P2 P3 111.96(4) . . ?
N3 P3 O1 107.62(12) . . ?
N3 P3 N2 118.59(12) . . ?
O1 P3 N2 110.22(12) . . ?
N3 P3 Cl3 110.64(10) . . ?
O1 P3 Cl3 101.95(9) . . ?
N2 P3 Cl3 106.57(10) . . ?
N3 P3 P2 89.83(9) . . ?
O1 P3 P2 136.02(10) . . ?
N2 P3 P2 31.36(8) . . ?
Cl3 P3 P2 109.16(4) . . ?
N8 P4 N6 114.37(12) . . ?
N8 P4 N10 109.26(12) . . ?
N6 P4 N10 108.94(13) . . ?
N8 P4 N9 109.11(12) . . ?
N6 P4 N9 109.06(12) . . ?
N10 P4 N9 105.75(12) . . ?
N6 P5 N7 119.57(12) . . ?
N6 P5 Cl4 110.90(10) . . ?
N7 P5 Cl4 107.43(9) . . ?
N6 P5 Cl5 109.47(10) . . ?
N7 P5 Cl5 108.31(9) . . ?
Cl4 P5 Cl5 99.21(4) . . ?
N8 P6 O2 106.66(11) . . ?
N8 P6 N7 119.51(12) . . ?
O2 P6 N7 110.88(12) . . ?
N8 P6 Cl6 109.58(9) . . ?
O2 P6 Cl6 102.18(8) . . ?
N7 P6 Cl6 106.69(9) . . ?
N13 P7 N11 115.43(12) . . ?
N13 P7 N15 108.92(12) . . ?
N11 P7 N15 108.27(13) . . ?
N13 P7 N14 109.39(12) . . ?
N11 P7 N14 108.66(13) . . ?
N15 P7 N14 105.74(12) . . ?
N11 P8 N12 119.41(13) . . ?
N11 P8 Cl7 110.41(10) . . ?
N12 P8 Cl7 107.41(11) . . ?
N11 P8 Cl8 109.23(10) . . ?
N12 P8 Cl8 108.37(10) . . ?
Cl7 P8 Cl8 100.31(4) . . ?
O3 P9 N13 107.57(11) . . ?
O3 P9 N12 109.96(12) . . ?
N13 P9 N12 119.10(13) . . ?
O3 P9 Cl9 102.16(8) . . ?
N13 P9 Cl9 109.30(10) . . ?
N12 P9 Cl9 107.43(11) . . ?
N16 P10 N18 113.64(12) . . ?
N16 P10 N20 109.26(13) . . ?
N18 P10 N20 112.11(13) . . ?
N16 P10 N19 107.15(13) . . ?
N18 P10 N19 111.43(12) . . ?
N20 P10 N19 102.58(13) . . ?
N16 P11 N17 119.80(13) . . ?
N16 P11 Cl11 108.70(10) . . ?
N17 P11 Cl11 109.10(10) . . ?
N16 P11 Cl10 110.11(10) . . ?
N17 P11 Cl10 107.73(10) . . ?
Cl11 P11 Cl10 99.49(4) . . ?
N18 P12 O4 108.45(12) . . ?
N18 P12 N17 119.01(12) . . ?
O4 P12 N17 110.11(12) . . ?
N18 P12 Cl12 109.14(10) . . ?
O4 P12 Cl12 101.94(8) . . ?
N17 P12 Cl12 106.84(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.325
_refine_diff_density_min   -0.336
_refine_diff_density_rms    0.061
