# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1280 data_Compound4 _audit_creation_method SHELXL _chemical_name_systematic ; 4,4,6,6,8,8-Hexachloro-1,3,5,7-tetraaza-2\l^5,4\l^5,6\l^5,8\l^5- tetraphospha-cyclooctatetraen-2-spiro-11'-(1',3',7',9'-tetra(tert- butyl)- dibenzo[d',g']-[1',3']-dioxa-[2'\l^5]-phospha-[4',7']-cyclooctadiene) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H42 Cl6 N4 O2 P8 + 1/2(C4 H8 Cl2)' _chemical_formula_weight '815.29 + 65.51' _chemical_melting_point 451 _chemical_compound_source 'K.C. Kumara Swamy' 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1(bar) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x,-y,-z' _cell_length_a 11.154(14) _cell_length_b 11.703(2) _cell_length_c 17.428(5) _cell_angle_alpha 106.34(2) _cell_angle_beta 104.25(5) _cell_angle_gamma 89.85(4) _cell_volume 2110(9.7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method ? _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 0.59 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710690 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'enraf-nonius CAD4' _diffrn_measurement_method 'omega scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.5 _diffrn_reflns_number 7632 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25 _reflns_number_total 7367 _reflns_number_observed 3850 _reflns_observed_criterion >4sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_refinement 'Xtal3.0 (Hall & Stewart, 1990)' _computing_molecular_graphics 'SCHAKAL-88 (univ.Freiburg, 1988)' _computing_publication_material xtal_BONDLA_CIFIO _refine_special_details ; Refinement on F ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'not refined, U set to 0.035' _refine_ls_extinction_method 'isotropic (Zachariasen)' _refine_ls_extinction_coef 0 _refine_ls_extinction_expression ? _refine_ls_number_reflns 3850 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.192 _refine_ls_R_factor_obs 0.106 _refine_ls_wR_factor_all 0.066 _refine_ls_wR_factor_obs 0.062 _refine_ls_goodness_of_fit_all 2.27 _refine_ls_goodness_of_fit_obs 3.11 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.03 _refine_ls_shift/esd_mean 0.006 _refine_diff_density_max 1.3 _refine_diff_density_min -1.6 _refine_diff_density_rms 0.08 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P2 P 1.18448(23) 0.47540(24) 0.63626(18) 0.0472(23) Uani 1 d . . P4 P 1.37297(25) 0.63027(28) 0.76714(21) 0.0614(27) Uani 1 d . . P6 P 1.24294(23) 0.61037(23) 0.88432(17) 0.0401(21) Uani 1 d . . P8 P 1.03960(23) 0.46323(22) 0.75249(17) 0.0343(19) Uani 1 d . . CL21 CL 1.20207(25) 0.31808(27) 0.56203(22) 0.0812(28) Uani 1 d . . CL22 CL 1.14312(26) 0.57431(32) 0.56037(21) 0.1056(32) Uani 1 d . . CL41 CL 1.39292(35) 0.76760(29) 0.72723(24) 0.1270(39) Uani 1 d . . CL42 CL 1.54747(25) 0.59559(33) 0.80850(23) 0.1121(38) Uani 1 d . . CL61 CL 1.17667(25) 0.73804(24) 0.96096(18) 0.0684(25) Uani 1 d . . CL62 CL 1.36217(23) 0.54689(26) 0.96304(19) 0.0728(26) Uani 1 d . . CL01 CL 0.51089(34) 0.24826(38) 0.49107(27) 0.1345(44) Uani 1 d . . O1 O 0.91913(48) 0.53408(49) 0.75301(36) 0.0346(46) Uani 1 d . . O2 O 0.99830(46) 0.33256(47) 0.74456(37) 0.0396(47) Uani 1 d . . N1 N 1.07223(60) 0.46638(64) 0.67093(44) 0.0467(63) Uani 1 d . . N3 N 1.31706(61) 0.51752(67) 0.69548(48) 0.0501(70) Uani 1 d . . N5 N 1.31291(66) 0.67710(65) 0.84090(46) 0.0516(66) Uani 1 d . . N7 N 1.14180(62) 0.50629(61) 0.83582(43) 0.0384(58) Uani 1 d . . C1 C 0.88588(73) 0.61007(81) 0.82264(55) 0.0285(69) Uani 1 d . . C2 C 0.85957(74) 0.72259(84) 0.82034(65) 0.0370(79) Uani 1 d . . C3 C 0.82571(82) 0.79671(78) 0.88858(71) 0.0446(81) Uani 1 d . . C4 C 0.81876(76) 0.75443(82) 0.95444(65) 0.0377(78) Uani 1 d . . C5 C 0.84221(73) 0.63858(82) 0.95171(55) 0.0318(69) Uani 1 d . . C6 C 0.87519(70) 0.56210(76) 0.88525(56) 0.0268(71) Uani 1 d . . C7 C 0.90150(72) 0.43790(76) 0.88491(54) 0.0320(69) Uani 1 d . . C8 C 0.87866(77) 0.28827(75) 0.74377(62) 0.0401(74) Uani 1 d . . C9 C 0.81848(79) 0.19259(77) 0.67727(55) 0.0352(73) Uani 1 d . . C10 C 0.70177(80) 0.15392(77) 0.68057(58) 0.0402(74) Uani 1 d . . C11 C 0.64926(81) 0.20416(81) 0.74384(63) 0.0443(78) Uani 1 d . . C12 C 0.71483(79) 0.29610(77) 0.81107(56) 0.0412(78) Uani 1 d . . C13 C 0.83202(82) 0.34192(73) 0.81126(57) 0.0376(73) Uani 1 d . . C211 C 0.86253(100) 0.77155(97) 0.74999(76) 0.0625(97) Uani 1 d . . C41 C 0.78498(128) 0.83936(109) 1.02754(88) 0.0737(102) Uani 1 d . . C91 C 0.87112(86) 0.13001(78) 0.60410(61) 0.0414(79) Uani 1 d . . C111 C 0.52179(89) 0.15251(93) 0.74693(73) 0.0579(87) Uani 1 d . . C14 C 0.99067(102) 0.77798(93) 0.73623(75) 0.0909(112) Uani 1 d . . C15 C 0.78275(103) 0.69568(114) 0.66927(78) 0.0942(121) Uani 1 d . . C16 C 0.81964(114) 0.89465(111) 0.75826(81) 0.1217(146) Uani 1 d . . C17 C 0.99954(99) 0.09051(83) 0.63696(67) 0.0715(96) Uani 1 d . . C18 C 0.87856(89) 0.21367(85) 0.55242(61) 0.0598(90) Uani 1 d . . C19 C 0.78880(94) 0.01881(87) 0.54620(64) 0.0742(93) Uani 1 d . . C20 C 0.67243(236) 0.87405(323) 1.01186(125) 0.3329(421) Uani 1 d . . C21 C 0.80164(262) 0.80094(153) 1.09811(117) 0.2560(299) Uani 1 d . . C22 C 0.84204(396) 0.94874(241) 1.05635(214) 0.5100(598) Uani 1 d . . C23 C 0.44494(91) 0.25618(120) 0.76221(91) 0.1264(145) Uani 1 d . . C24 C 0.53761(92) 0.10082(99) 0.81469(85) 0.1039((121) Uani 1 d . . C25 C 0.46096(96) 0.05891(122) 0.66839(82) 0.1176(137) Uani 1 d . . C026 C 0.48190(134) 0.48438(136) 0.53358(99) 0.1210(181) Uani 1 d . . C027 C 0.54727(119) 0.38501(108) 0.57007(97) 0.1094(162) Uani 1 d . . H3 H .81670 .88532 .88726 .02891 Uiso 1 calc R . H5 H .85192 .59895 1.00175 .01545 Uiso 1 calc R . H10 H .64534 .08911 .62655 .04106 Uiso 1 calc R . H12 H .67801 .33233 .87293 .03500 Uiso 1 calc R . H71 H .88216 .42667 .93806 .00018 Uiso 1 calc R . H72 H .99068 .41762 .89684 .03678 Uiso 1 calc R . H141 H 1.03485 .70256 .73675 .03500 Uiso 1 calc R . H142 H .99375 .79478 .68152 .03500 Uiso 1 calc R . H143 H 1.04617 .84606 .78174 .03500 Uiso 1 calc R . H151 H .69537 .66967 .67379 .03500 Uiso 1 calc R . H152 H .76649 .72543 .61958 .03500 Uiso 1 calc R . H153 H .81732 .60937 .64844 .03500 Uiso 1 calc R . H161 H .85000 .94272 .78765 .03500 Uiso 1 calc R . H162 H .80704 .91470 .70220 .03500 Uiso 1 calc R . H163 H .72939 .89202 .76534 .03500 Uiso 1 calc R . H171 H .99786 .04303 .67733 .03500 Uiso 1 calc R . H172 H 1.03463 .03430 .59088 .03500 Uiso 1 calc R . H173 H 1.06254 .16002 .66542 .03500 Uiso 1 calc R . H181 H .91639 .29448 .58583 .03500 Uiso 1 calc R . H182 H .92673 .18180 .50787 .03500 Uiso 1 calc R . H183 H .79062 .22331 .51922 .03500 Uiso 1 calc R . H191 H .70107 .04088 .53228 .03500 Uiso 1 calc R . H192 H .81749 -.00934 .49441 .03500 Uiso 1 calc R . H193 H .79244 -.04758 .57222 .03500 Uiso 1 calc R . H201 H .60937 .78323 .98300 .03500 Uiso 1 calc R . H202 H .63344 .90455 1.06082 .03500 Uiso 1 calc R . H203 H .64613 .91067 .97070 .03500 Uiso 1 calc R . H211 H .89748 .77302 1.11147 .03500 Uiso 1 calc R . H212 H .80152 .86218 1.15121 .03500 Uiso 1 calc R . H213 H .75325 .72664 1.09420 .03500 Uiso 1 calc R . H221 H .83373 .98147 1.00826 .03500 Uiso 1 calc R . H222 H .79789 .99862 1.09601 .03500 Uiso 1 calc R . H223 H .93213 .95616 1.08554 .03500 Uiso 1 calc R . H231 H .49272 .32508 .75429 .03500 Uiso 1 calc R . H232 H .36630 .23718 .71020 .03500 Uiso 1 calc R . H233 H .42477 .27027 .80550 .03500 Uiso 1 calc R . H241 H .59417 .15404 .87073 .03500 Uiso 1 calc R . H242 H .46334 .07234 .82886 .03500 Uiso 1 calc R . H243 H .58982 .02381 .80225 .03500 Uiso 1 calc R . H251 H .51866 .00042 .64997 .03500 Uiso 1 calc R . H252 H .38441 .01832 .67186 .03500 Uiso 1 calc R . H253 H .42751 .09471 .61738 .03500 Uiso 1 calc R . H261 H .39111 .46020 .51280 .03500 Uiso 1 calc R . H262 H .49573 .56069 .57951 .03500 Uiso 1 calc R . H271 H .51620 .38021 .61830 .03500 Uiso 1 calc R . H272 H .63909 .40382 .58825 .03500 Uiso 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 P2 .0326(19) .0575(24) .0517(24) -.0091(17) .0196(18) .0108(20) P4 .0375(22) .0724(27) .0735(30) -.0222(19) .0178(21) .0169(23) P6 .0292(18) .0446(22) .0469(23) -.0059(16) .0065(17) .0058(18) P8 .0281(18) .0331(19) .0431(23) -.0028(15) .0116(17) .0063(17) CL21 .0545(23) .0940(28) .0961(31) -.0164(19) .0433(22) -.0239(24) CL22 .0581(24) .1526(39) .1062(35) -.0107(24) .0143(23) .0800(31) CL41 .1598(42) .0839(30) .1373(41) -.0400(28) .0696(34) .0309(29) CL42 .0301(21) .1707(42) .1355(42) -.0270(23) .0122(24) -.0043(34) CL61 .0674(24) .0593(23) .0785(28) -.0056(18) .0258(21) -.0089(20) CL62 .0448(21) .0890(27) .0844(29) .0020(18) -.0060(20) .0315(23) CL01 .0997(36) .1476(45) .1562(50) .0112(31) .0206(34) .0231(39) O1 .0256(43) .0417(48) .0365(48) -.0009(36) .0038(37) .0005(40) O2 .0200(40) .0378(46) .0610(55) -.0066(34) .0167(38) .0074(41) N1 .0363(58) .0650(67) .0388(64) -.0102(48) .0241(49) .0106(53) N3 .0236(55) .0676(71) .0592(76) -.0056(49) .0122(53) .0038(60) N5 .0506(64) .0608(67) .0433(68) -.0252(51) .0175(54) -.0039(54) N7 .0355(53) .0503(63) .0294(58) .0061(46) .0077(46) .0054(48) C1 .0258(62) .0363(78) .0235(67) -.0066(55) .0067(52) -.0069(59) C2 .0192(64) .0329(64) .0589(104) .0026(53) .0098(64) .0207(72) C3 .0366(78) .0242(72) .0730(106) -.0049(57) .0070(74) .0095(72) C4 .0242(66) .0294(70) .0593(98) .0061(53) .0159(65) .0045(68) C5 .0237(62) .0395(72) .0322(73) -.0096(53) .0077(54) .0045(59) C6 .0162(57) .0329(70) .0313(73) -.0040(50) .0068(52) -.0002(58) C7 .0217(62) .0336(69) .0407(77) -.0009(53) .0108(55) .0012(59) C8 .0290(68) .0282(66) .0631(91) -.0056(53) .0239(66) .0081(64) C9 .0377(75) .0383(70) .0295(74) -.0060(59) .0154(61) -.0004(58) C10 .0382(67) .0406(78) .0416(78) -.0201(57) .0152(60) -.0069(62) C11 .0303(68) .0443(77) .0584(89) -.0061(59) .0218(64) -.0010(68) C12 .0381(75) .0434(78) .0420(82) -.0074(61) .0283(66) .0028(65) C13 .0444(73) .0236(64) .0447(83) -.0028(54) .0230(64) .0027(59) C211 .0550(97) .0550(92) .0775(118) .0183(75) .0203(87) .0324(87) C41 .0794(115) .0524(95) .0892(152) .0076(83) .0522((111) -.0070(97) C91 .0453(80) .0310(73) .0479(84) -.0116(62) .0170(67) -.0072(64) C111 .0333(73) .0530(88) .0874(109) -.0022(65) .0456(76) .0142(81) C14 .0788(108) .0754(99) .1184(131) .0170(81) .0484(98) .0568(93) C15 .0640(100) .1330(142) .0856(119) .0280(94) .0248(88) .0565(108) C16 .1274(143) .1090(135) .1288(159) .0513(110) .0650(123) .0802(124) C17 .0786(98) .0517(81) .0843(109) .0137(70) .0548(86) -.0037(74) C18 .0748(96) .0539(84) .0506(93) -.0189(70) .0335(77) .0021(71) C19 .0884(91) .0639(93) .0704(93) -.0110(73) .0698(77) -.0115(70) C20 .2948(439) .6021(656) .1018(184) .2761(458) .0513(250) -.1178(274) C21 .5107(470) .1229(190) .1344(224) .1795(243) .1950(282) .0493(168) C22 .8695(740) .2122(282) .4483(464) -.3288(392) .5586(512) -.2670(301) C23 .0225(83) .1472(150) .2094(204) -.0306(87) .0375(107) .0632(143) C24 .0580(92) .0873(113) .1663(159) .0036(77) .0739(101) .0618(112) C25 .0483(99) .1920(169) .1125(143) -.0829(107) .0441(97) -.0381(126) C026 .0896(146) .1174(145) .1559(253) -.0428(109) .0949(147) -.0471(152) C027 .09439164) .0596(141) .1743(180) -.0077(118) .0236(141) -.0222(128) _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 P2 CL21 1.970(4) . yes P2 CL22 1.962(6) . yes P2 N1 1.53(1) . yes P2 N3 1.565(8) . yes P4 CL41 1.952(6) . yes P4 CL42 1.982(5) . yes P4 N3 1.552(8) . yes P4 N5 1.56(1) . yes P6 CL61 1.982(4) . yes P6 CL62 1.970(5) . yes P6 N5 1.55(1) . yes P6 N7 1.569(8) . yes P8 O1 1.579(7) . yes P8 O2 1.555(7) . yes P8 N1 1.55(1) . yes P8 N7 1.550(7) . yes O1 C1 1.43(1) . yes O2 C8 1.43(1) . yes C1 C2 1.35(2) . no C1 C6 1.40(2) . no C2 C3 1.39(2) . no C2 C211 1.51(2) . no C3 C4 1.38(2) . no C3 H3 1.03(1) . no C4 C5 1.36(2) . no C4 C41 1.50(2) . no C5 C6 1.39(1) . no C5 H5 1.08(1) . no C6 C7 1.49(1) . no C7 C13 1.50(1) . no C7 H71 1.05(1) . no C7 H72 1.002(9) . no C8 C9 1.40(1) . no C8 C13 1.38(2) . no C9 C10 1.39(2) . no C9 C91 1.54(2) . no C10 C11 1.36(2) . no C10 H10 1.065(9) . no C11 C12 1.39(1) . no C11 C111 1.56(2) . no C12 C13 1.43(2) . no C12 H12 1.01(1) . no C211 C14 1.54(2) . no C211 C15 1.49(2) . no C211 C16 1.49(2) . no C41 C20 1.35(4) . no C41 C21 1.41(3) . no C41 C22 1.35(4) . no C91 C17 1.55(2) . no C91 C18 1.51(2) . no C91 C19 1.53(1) . no C111 C23 1.50(2) . no C111 C24 1.45(2) . no C111 C25 1.49(2) . no C14 H141 1.01(1) . no C14 H142 1.05(2) . no C14 H143 1.00(1) . no C15 H151 1.03(1) . no C15 H152 .99(2) . no C15 H153 1.09(1) . no C16 H161 .69(1) . no C16 H162 1.03(2) . no C16 H163 1.02(2) . no C17 H171 1.00(1) . no C17 H172 1.03(1) . no C17 H173 .99(1) . no C18 H181 1.01(1) . no C18 H182 1.05(1) . no C18 H183 1.03(1) . no C19 H191 1.03(1) . no C19 H192 1.01(1) . no C19 H193 .97(1) . no C20 H201 .91(3) . no C20 H202 1.00(3) . no C20 H203 1.13(4) . no C21 H211 .97(3) . no C21 H212 1.00(2) . no C21 H213 1.00(3) . no C22 H221 1.02(4) . no C22 H222 1.07(4) . no C22 H223 .92(4) . no C23 H231 1.01(2) . no C23 H232 1.09(1) . no C23 H233 .78(2) . no C24 H241 1.02(1) . no C24 H242 1.00(1) . no C24 H243 1.08(1) . no C25 H251 1.00(1) . no C25 H252 1.01(2) . no C25 H253 1.08(2) . no CL01 C027 1.77(1) . yes C026 C027 1.57(3) . yes C026 H261 1.00(2) . no C026 H262 1.00(2) . no C026 C026 1.41(3) . yes C027 H271 .99(2) . no C027 H272 1.01(2) . no 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 CL21 P2 CL22 102.8(2) . . yes CL21 P2 N1 109.1(3) . . yes CL21 P2 N3 105.2(4) . . yes CL22 P2 N1 108.4(4) . . yes CL22 P2 N3 109.3(4) . . yes N1 P2 N3 120.5(5) . . yes CL41 P4 CL42 102.1(3) . . yes CL41 P4 N3 111.8(5) . . yes CL41 P4 N5 105.7(4) . . yes CL42 P4 N3 104.1(4) . . yes CL42 P4 N5 110.2(4) . . yes N3 P4 N5 121.2(5) . . yes CL61 P6 CL62 101.0(2) . . yes CL61 P6 N5 104.8(4) . . yes CL61 P6 N7 110.3(4) . . yes CL62 P6 N5 110.1(4) . . yes CL62 P6 N7 105.3(4) . . yes N5 P6 N7 123.2(5) . . yes O1 P8 O2 105.3(4) . . yes O1 P8 N1 104.7(5) . . yes O1 P8 N7 112.9(4) . . yes O2 P8 N1 108.8(4) . . yes O2 P8 N7 105.5(5) . . yes N1 P8 N7 118.9(5) . . yes P8 O1 C1 127.7(6) . . yes P8 O2 C8 127.5(6) . . yes P2 N1 P8 141.9(5) . . yes P2 N3 P4 134.4(6) . . yes P4 N5 P6 131.4(6) . . yes P6 N7 P8 140.0(7) . . yes O1 C1 C2 118(1) . . no O1 C1 C6 116.8(9) . . no C2 C1 C6 125(1) . . no C1 C2 C3 117(1) . . no C1 C2 C211 124(1) . . no C3 C2 C211 119(1) . . no C2 C3 C4 120(1) . . no C2 C3 H3 113(1) . . no C4 C3 H3 126(1) . . no C3 C4 C5 122(1) . . no C3 C4 C41 118(1) . . no C5 C4 C41 120(1) . . no C4 C5 C6 121(1) . . no C4 C5 H5 129(1) . . no C6 C5 H5 110(1) . . no C1 C6 C5 116(1) . . no C1 C6 C7 123.8(9) . . no C5 C6 C7 120(1) . . no C6 C7 C13 116.4(8) . . no C6 C7 H71 106.3(9) . . no C6 C7 H72 118.9(9) . . no C13 C7 H71 109.2(9) . . no C13 C7 H72 106.5(8) . . no H71 C7 H72 97.5(9) . . no O2 C8 C9 119(1) . . no O2 C8 C13 116.6(8) . . no C9 C8 C13 124(1) . . no C8 C9 C10 116(1) . . no C8 C9 C91 124(1) . . no C10 C9 C91 120.1(8) . . no C9 C10 C11 123.2(8) . . no C9 C10 H10 119(1) . . no C11 C10 H10 117(1) . . no C10 C11 C12 120(1) . . no C10 C11 C111 122.7(9) . . no C12 C11 C111 117(1) . . no C11 C12 C13 121(1) . . no C11 C12 H12 120(1) . . no C13 C12 H12 119.5(8) . . no C7 C13 C8 124(1) . . no C7 C13 C12 119(1) . . no C8 C13 C12 116.3(8) . . no C2 C211 C14 111(1) . . no C2 C211 C15 113(1) . . no C2 C211 C16 115(1) . . no C14 C211 C15 107(1) . . no C14 C211 C16 105(1) . . no C15 C211 C16 105(1) . . no C4 C41 C20 112(1) . . no C4 C41 C21 118(1) . . no C4 C41 C22 115(2) . . no C20 C41 C21 105(2) . . no C20 C41 C22 102(3) . . no C21 C41 C22 103(2) . . no C9 C91 C17 109.7(9) . . no C9 C91 C18 109.3(9) . . no C9 C91 C19 112(1) . . no C17 C91 C18 111(1) . . no C17 C91 C19 107.9(8) . . no C18 C91 C19 107.6(9) . . no C11 C111 C23 106(1) . . no C11 C111 C24 111.2(9) . . no C11 C111 C25 111(1) . . no C23 C111 C24 108(1) . . no C23 C111 C25 112(1) . . no C24 C111 C25 109(1) . . no C211 C14 H141 112(1) . . no C211 C14 H142 113(1) . . no C211 C14 H143 112(1) . . no H141 C14 H142 105(1) . . no H141 C14 H143 108(1) . . no H142 C14 H143 106(1) . . no C211 C15 H151 112(1) . . no C211 C15 H152 118(1) . . no C211 C15 H153 112(1) . . no H151 C15 H152 108(1) . . no H151 C15 H153 101(1) . . no H152 C15 H153 103(1) . . no C211 C16 H161 121(2) . . no C211 C16 H162 110(1) . . no C211 C16 H163 107(1) . . no H161 C16 H162 105(2) . . no H161 C16 H163 106(2) . . no H162 C16 H163 105(1) . . no C91 C17 H171 109(1) . . no C91 C17 H172 112(1) . . no C91 C17 H173 111(1) . . no H171 C17 H172 107(1) . . no H171 C17 H173 110(1) . . no H172 C17 H173 108(1) . . no C91 C18 H181 114(1) . . no C91 C18 H182 114(1) . . no C91 C18 H183 112(1) . . no H181 C18 H182 105(1) . . no H181 C18 H183 107(1) . . no H182 C18 H183 104(1) . . no C91 C19 H191 107.8(9) . . no C91 C19 H192 108(1) . . no C91 C19 H193 114(1) . . no H191 C19 H192 106(1) . . no H191 C19 H193 109(1) . . no H192 C19 H193 111(1) . . no C41 C20 H201 117(4) . . no C41 C20 H202 110(2) . . no C41 C20 H203 106(3) . . no H201 C20 H202 118(4) . . no H201 C20 H203 105(2) . . no H202 C20 H203 99(3) . . no C41 C21 H211 107(3) . . no C41 C21 H212 106(2) . . no C41 C21 H213 115(2) . . no H211 C21 H212 112(2) . . no H211 C21 H213 110(2) . . no H212 C21 H213 108(3) . . no C41 C22 H221 107(3) . . no C41 C22 H222 104(4) . . no C41 C22 H223 121(3) . . no H221 C22 H222 103(3) . . no H221 C22 H223 113(5) . . no H222 C22 H223 108(3) . . no C111 C23 H231 104(1) . . no C111 C23 H232 103(1) . . no C111 C23 H233 114(2) . . no H231 C23 H232 102(2) . . no H231 C23 H233 120(2) . . no H232 C23 H233 112(1) . . no C111 C24 H241 114(1) . . no C111 C24 H242 120(1) . . no C111 C24 H243 108(1) . . no H241 C24 H242 107(2) . . no H241 C24 H243 102(1) . . no H242 C24 H243 104(1) . . no C111 C25 H251 113(1) . . no C111 C25 H252 114(1) . . no C111 C25 H253 115(1) . . no H251 C25 H252 109(1) . . no H251 C25 H253 103(1) . . no H252 C25 H253 102(1) . . no C027 C026 H261 108(2) . . no C027 C026 H262 108(2) . . no C027 C026 C026 112(2) . . no H261 C026 H262 109(2) . . no H261 C026 C026 109(2) . . no H262 C026 C026 110(2) . . no CL01 C027 C026 111(1) . . no CL01 C027 H271 109(1) . . no CL01 C027 H272 108(1) . . no C026 C027 H271 110(2) . . no C026 C027 H272 109(2) . . no H271 C027 H272 110(2) . . no 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_publ_flag N1 P2 N3 P4 -57(1) yes P2 N3 P4 N5 52(1) yes N3 P4 N5 P6 34(1) yes P4 N5 P6 N7 -45.1(9) yes N5 P6 N7 P8 -30(1) yes P6 N7 P8 N1 45(1) yes N7 P8 N1 P2 17(1) yes P8 N1 P2 N3 -15(1) yes #=END data_compound5 _audit_creation_date 98-07-20 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 21.08.98 _chemical_compound_source synthesis #ActaC _chemical_name_systematic ;4',4',6',6',8',8'-hexachloro-1,3- diisopropyl- 1,3-diaza-2-phosphorinane-2-spiro-2'-1',3',5',7'-tetraaza-2'\l^5,4'\l^5, 6'\l^5,8'\l^5-tetraphosphacyclooctatetraene ; _chemical_name_common ? #ActaC _chemical_formula_analytical C9H20Cl6N6P4 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C9H20Cl6N6P4 #ActaC _chemical_formula_weight 548.91 #ActaC _chemical_melting_point 363 #ActaC _computing_data_collection CAD-4 #ActaC _computing_cell_refinement CAD-4 #ActaC _computing_data_reduction xtal_ADDREF_SORTRF #ActaC _computing_structure_solution MULTAN_Shelx93 #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal_ORTEP #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 11.373(3) #ActaC _cell_length_b 16.955(6) #ActaC _cell_length_c 12.570(4) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 111.28(2) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 2258.6(13) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 173 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 7 #ActaC _cell_measurement_theta_max 14 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/n_1 #ActaC _symmetry_space_group_name_Hall -p_2yn #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description prism #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max 0.8 #ActaC _exptl_crystal_size_mid 0.4 #ActaC _exptl_crystal_size_min 0.3 #ActaC _exptl_crystal_density_diffrn 1.614 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1112 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 1.06 #ActaC _exptl_absorpt_correction_type none #ActaC _exptl_absorpt_correction_T_min ? #ActaC _exptl_absorpt_correction_T_max ? #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 #ActaC _diffrn_radiation_wavelength 0.71069 #ActaC _diffrn_radiation_type MoK-alpha #ActaC _diffrn_radiation_source xray_tube #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector ? #ActaC _diffrn_measurement_device Enraf-Nonius_CAD-4 #ActaC _diffrn_measurement_method 'omega scan' #ActaC _diffrn_standards_number 2 #ActaC _diffrn_standards_interval_count 100 #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% 14.7 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 4144 #ActaC _diffrn_reflns_av_R_equivalents 0.022 #ActaC _diffrn_reflns_av_sigmaI/netI 0.034 #ActaC _diffrn_reflns_limit_h_min -12 #ActaC _diffrn_reflns_limit_h_max 13 #ActaC _diffrn_reflns_limit_k_min -20 #ActaC _diffrn_reflns_limit_k_max 0 #ActaC _diffrn_reflns_limit_l_min -14 #ActaC _diffrn_reflns_limit_l_max 0 #ActaC _diffrn_reflns_theta_min 2.97 #ActaC _diffrn_reflns_theta_max 24.98 #ActaC _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 36 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 80 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 CL ? 0 24 .132 .159 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 24 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 16 .09 .095 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC P2 .26499(10) .44075(6) .88566(9) .0336(5) Uani ? ? P4 .32877(10) .36564(7) .70762(10) .0366(6) Uani ? ? P6 .06750(10) .34139(7) .59290(9) .0331(5) Uani ? ? P8 .01191(10) .37299(6) .80759(9) .0317(5) Uani ? ? CL21 .38039(10) .45198(8) 1.04724(10) .0560(7) Uani ? ? CL22 .26345(12) .55158(7) .82794(13) .0694(8) Uani ? ? CL41 .44836(12) .43188(10) .66362(12) .0776(9) Uani ? ? CL42 .40741(15) .25963(8) .71981(12) .0822(9) Uani ? ? CL61 .04748(14) .22912(7) .54217(12) .0726(8) Uani ? ? CL62 -.04738(12) .39520(8) .45261(10) .0629(7) Uani ? ? N1 .1339(3) .4191(2) .8838(3) .042(2) Uani ? ? N3 .3391(3) .3863(2) .8310(3) .048(2) Uani ? ? N5 .2029(3) .3689(2) .6050(3) .046(2) Uani ? ? N7 .0183(3) .3509(2) .6885(3) .054(2) Uani ? ? N11 -.0060(3) .2933(2) .8725(3) .047(2) Uani ? ? N31 -.1138(3) .4253(2) .7872(3) .0384(19) Uani ? ? C41 -.1983(7) .4115(5) .8464(8) .090(5) Uani ? ? C51 -.2083(6) .3332(4) .8820(7) .088(5) Uani ? ? C61 -.1030(5) .2833(4) .9169(5) .088(4) Uani ? ? C1 .0992(5) .2361(3) .9038(5) .059(3) Uani ? ? C2 .0577(9) .1556(4) .8554(7) .087(5) Uani ? ? C3 .1708(8) .2332(5) 1.0320(7) .084(5) Uani ? ? C4 -.1242(4) .5014(3) .7268(5) .049(3) Uani ? ? C5 -.2453(7) .5076(5) .6286(7) .078(4) Uani ? ? C6 -.0999(8) .5714(4) .8082(8) .088(5) Uani ? ? H1 .166(4) .252(2) .872(4) .062(15) Uiso ? ? H4 -.052(4) .503(2) .707(4) .061(15) Uiso ? ? H411 -.290(4) .440(3) .803(4) .072(15) Uiso ? ? H412 -.160(7) .437(4) .911(6) .14(4) Uiso ? ? H511 -.263(4) .322(3) .902(4) .058(16) Uiso ? ? H512 -.268(8) .331(6) .772(8) .25(5) Uiso ? ? H611 -.13877 .22725 .88440 .03500 Uiso ? ? H612 -.06496 .28033 .99740 .03500 Uiso ? ? H21 .137(5) .118(4) .880(5) .12(2) Uiso ? ? H22 -.009(6) .138(3) .882(5) .11(3) Uiso ? ? H23 -.019(5) .158(3) .787(4) .09(2) Uiso ? ? H31 .250(6) .194(4) 1.042(5) .14(3) Uiso ? ? H32 .212(5) .286(3) 1.061(5) .11(2) Uiso ? ? H33 .120(5) .209(3) 1.053(5) .08(2) Uiso ? ? H51 -.318(5) .508(3) .646(4) .08(2) Uiso ? ? H52 -.242(5) .554(3) .594(4) .09(2) Uiso ? ? H53 -.253(6) .460(4) .582(5) .13(3) Uiso ? ? H61 -.125(5) .619(3) .766(5) .11(2) Uiso ? ? H62 -.168(4) .575(3) .824(4) .051(17) Uiso ? ? H63 -.009(5) .564(3) .860(5) .11(2) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC P2 .0342(6) .0351(6) .0307(6) .0022(5) .0109(5) -.0047(5) P4 .0354(6) .0469(7) .0328(7) .0029(6) .0187(5) .0002(6) P6 .0390(6) .0365(6) .0267(6) -.0052(5) .0153(5) -.0042(5) P8 .0325(6) .0358(6) .0316(6) -.0031(5) .0172(5) -.0021(5) CL21 .0437(7) .0835(9) .0354(7) .0059(7) .0077(5) -.0179(7) CL22 .0692(9) .0452(8) .0952(11) -.0002(7) .0314(8) .0197(8) CL41 .0483(8) .1201(13) .0678(10) -.0231(8) .0250(7) .0210(9) CL42 .1215(13) .0706(10) .0595(9) .0456(9) .0390(9) .0019(8) CL61 .1013(11) .0442(8) .0778(10) -.0112(8) .0389(9) -.0234(7) CL62 .0568(8) .0785(10) .0444(7) -.0027(7) .0077(6) .0177(7) N1 .033(2) .044(2) .048(2) -.0064(17) .0141(18) -.012(2) N3 .051(2) .064(3) .030(2) .019(2) .0163(18) -.005(2) N5 .035(2) .068(3) .035(2) -.0122(19) .0126(17) .004(2) N7 .061(3) .078(3) .036(2) .004(2) .031(2) -.009(2) N11 .053(2) .044(2) .060(3) .005(2) .040(2) .014(2) N31 .038(2) .043(2) .043(2) .0027(17) .0251(18) .0074(19) C41 .070(5) .106(6) .127(7) .038(5) .074(5) .058(6) C51 .064(4) .100(5) .137(7) .015(4) .082(5) .049(5) C61 .073(4) .093(5) .121(6) .013(4) .061(4) .053(4) C1 .070(4) .047(3) .077(4) .012(3) .048(3) .017(3) C2 .113(7) .062(5) .088(6) .007(5) .040(6) -.008(4) C3 .074(5) .071(5) .095(6) .008(5) .016(5) .009(5) C4 .040(3) .048(3) .067(4) .001(2) .029(3) .001(3) C5 .081(5) .068(5) .072(5) .007(4) .011(4) .022(4) C6 .084(6) .057(5) .116(7) -.000(4) .028(5) -.017(4) _atom_sites_solution_primary 'direct methods ' _atom_sites_solution_secondary 'difference fourier maps ' _atom_sites_solution_hydrogens 'calculated geometrically' _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment isotropic #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 3807 #ActaC _refine_ls_number_parameters 298 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .072 #ActaC _refine_ls_R_factor_obs .049 #ActaC _refine_ls_wR_factor_all .038 #ActaC _refine_ls_wR_factor_obs .037 #ActaC _refine_ls_goodness_of_fit_all 2.334 #ActaC _refine_ls_goodness_of_fit_obs 2.643 #ActaC _refine_ls_shift/esd_max .097 #ActaC _refine_ls_shift/esd_mean .006 #ActaC _refine_diff_density_min -.695 #ActaC _refine_diff_density_max .553 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC P2 CL21 1.9872(15) . . yes P2 CL22 2.0122(18) . . yes P2 N1 1.527(4) . . yes P2 N3 1.566(4) . . yes P4 CL41 1.991(2) . . yes P4 CL42 1.988(2) . . yes P4 N3 1.553(4) . . yes P4 N5 1.542(3) . . yes P6 CL61 1.9940(18) . . yes P6 CL62 1.9942(16) . . yes P6 N5 1.562(4) . . yes P6 N7 1.507(5) . . yes P8 N1 1.577(3) . . yes P8 N7 1.570(4) . . yes P8 N11 1.630(4) . . yes P8 N31 1.621(4) . . yes N11 C61 1.415(8) . . no N11 C1 1.477(6) . . no N31 C41 1.433(12) . . no N31 C4 1.480(6) . . no C41 C51 1.419(12) . . no C41 H411 1.10(4) . . no C41 H412 .89(7) . . no C51 C61 1.400(9) . . no C51 H511 .77(5) . . no C51 H512 1.31(9) . . no C61 H611 1.056(6) . . no C61 H612 .947(6) . . no C1 C2 1.500(9) . . no C1 C3 1.520(9) . . no C1 H1 1.01(5) . . no C2 H21 1.06(6) . . no C2 H22 .98(7) . . no C2 H23 .98(5) . . no C3 H31 1.09(6) . . no C3 H32 1.02(5) . . no C3 H33 .83(6) . . no C4 C5 1.482(8) . . no C4 C6 1.525(10) . . no C4 H4 .94(5) . . no C5 H51 .93(6) . . no C5 H52 .90(5) . . no C5 H53 .98(6) . . no C6 H61 .96(6) . . no C6 H62 .87(5) . . no C6 H63 1.01(5) . . no loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC CL21 P2 CL22 101.26(7) . . . no CL21 P2 N1 108.54(15) . . . no CL21 P2 N3 104.12(12) . . . no CL22 P2 N1 109.76(14) . . . no CL22 P2 N3 109.14(17) . . . no N1 P2 N3 121.9(2) . . . yes CL41 P4 CL42 101.41(9) . . . no CL41 P4 N3 109.81(16) . . . no CL41 P4 N5 105.54(16) . . . no CL42 P4 N3 104.97(15) . . . no CL42 P4 N5 110.63(16) . . . no N3 P4 N5 122.6(2) . . . yes CL61 P6 CL62 101.06(7) . . . no CL61 P6 N5 108.08(16) . . . no CL61 P6 N7 108.97(17) . . . no CL62 P6 N5 104.80(14) . . . no CL62 P6 N7 110.00(15) . . . no N5 P6 N7 121.9(2) . . . yes N1 P8 N7 111.2(2) . . . yes N1 P8 N11 110.44(18) . . . yes N1 P8 N31 110.82(18) . . . yes N7 P8 N11 109.7(2) . . . yes N7 P8 N31 108.82(19) . . . yes N11 P8 N31 105.7(2) . . . yes P2 N1 P8 140.1(3) . . . yes P2 N3 P4 135.5(2) . . . yes P4 N5 P6 130.8(3) . . . yes P6 N7 P8 160.9(3) . . . yes P8 N11 C61 123.6(3) . . . no P8 N11 C1 116.2(4) . . . no C61 N11 C1 119.3(4) . . . no P8 N31 C41 123.2(4) . . . no P8 N31 C4 117.4(3) . . . no C41 N31 C4 117.7(5) . . . no N31 C41 C51 117.6(8) . . . no N31 C41 H411 112(3) . . . no N31 C41 H412 101(5) . . . no C51 C41 H411 113(3) . . . no C51 C41 H412 104(5) . . . no H411 C41 H412 108(5) . . . no C41 C51 C61 120.4(7) . . . no C41 C51 H511 120(3) . . . no C41 C51 H512 76(4) . . . no C61 C51 H511 116(3) . . . no C61 C51 H512 112(4) . . . no H511 C51 H512 99(6) . . . no N11 C61 C51 120.4(6) . . . no N11 C61 H611 101.6(5) . . . no N11 C61 H612 108.0(5) . . . no C51 C61 H611 104.9(5) . . . no C51 C61 H612 112.0(7) . . . no H611 C61 H612 109.1(6) . . . no N11 C1 C2 112.6(5) . . . no N11 C1 C3 112.0(6) . . . no N11 C1 H1 112(2) . . . no C2 C1 C3 111.7(5) . . . no C2 C1 H1 105(2) . . . no C3 C1 H1 104(2) . . . no C1 C2 H21 109(3) . . . no C1 C2 H22 108(4) . . . no C1 C2 H23 112(3) . . . no H21 C2 H22 114(5) . . . no H21 C2 H23 132(5) . . . no H22 C2 H23 76(5) . . . no C1 C3 H31 104(3) . . . no C1 C3 H32 111(3) . . . no C1 C3 H33 101(4) . . . no H31 C3 H32 104(4) . . . no H31 C3 H33 108(5) . . . no H32 C3 H33 127(6) . . . no N31 C4 C5 111.5(5) . . . no N31 C4 C6 111.9(5) . . . no N31 C4 H4 105(3) . . . no C5 C4 C6 113.0(5) . . . no C5 C4 H4 114(2) . . . no C6 C4 H4 101(3) . . . no C4 C5 H51 116(3) . . . no C4 C5 H52 106(3) . . . no C4 C5 H53 107(3) . . . no H51 C5 H52 107(5) . . . no H51 C5 H53 105(5) . . . no H52 C5 H53 116(5) . . . no C4 C6 H61 111(4) . . . no C4 C6 H62 104(3) . . . no C4 C6 H63 103(3) . . . no H61 C6 H62 87(5) . . . no H61 C6 H63 120(5) . . . no H62 C6 H63 130(5) . . . no loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -12 _reflns_limit_h_max 13 _reflns_limit_k_min -20 _reflns_limit_k_max 0 _reflns_limit_l_min -14 _reflns_limit_l_max 0 _reflns_number_total 4144 #ActaC _reflns_number_observed 3210 #ActaC _reflns_observed_criterion refl_observed_if_F____>_2.00_sigma(F___) _reflns_d_resolution_high .841 _reflns_d_resolution_low 6.858 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.6439 #=END data_compound6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 Cl4 N8 P4' _chemical_formula_weight 634.26 _chemical_melting_point 473 _chemical_compound_source 'K.C. Kumara Swamy' 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.058(11) _cell_length_b 16.7959(14) _cell_length_c 18.0196(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3044(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 15 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3051 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.23 _reflns_number_total 3051 _reflns_number_gt 2655 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+2.2190P] 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 0.34(16) _refine_ls_number_reflns 3051 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P2 P -0.00814(12) 0.57230(8) 0.19644(7) 0.0372(3) Uani 1 d . . . P4 P 0.24897(12) 0.63162(8) 0.16096(7) 0.0336(3) Uani 1 d . . . P6 P 0.20863(13) 0.52684(8) 0.03284(7) 0.0365(3) Uani 1 d . . . P8 P 0.02027(12) 0.42468(7) 0.10424(7) 0.0337(3) Uani 1 d . . . Cl21 Cl -0.13838(19) 0.64105(11) 0.13864(17) 0.1029(9) Uani 1 d . . . Cl22 Cl -0.0984(3) 0.56936(14) 0.29529(13) 0.1102(10) Uani 1 d . . . Cl61 Cl 0.1329(3) 0.61132(12) -0.03409(12) 0.1005(8) Uani 1 d . . . Cl62 Cl 0.35230(18) 0.48662(15) -0.03415(12) 0.0889(7) Uani 1 d . . . N3 N 0.1171(4) 0.6223(3) 0.2088(2) 0.0393(10) Uani 1 d . . . N5 N 0.2789(4) 0.5631(3) 0.1013(2) 0.0444(10) Uani 1 d . . . N7 N 0.1058(6) 0.4597(4) 0.0392(3) 0.0709(17) Uani 1 d . . . N1 N -0.0122(5) 0.4880(3) 0.1663(3) 0.0519(12) Uani 1 d . . . N11 N 0.2532(5) 0.7182(3) 0.1187(3) 0.0491(11) Uani 1 d . . . N31 N 0.3747(4) 0.6342(3) 0.2190(2) 0.0465(11) Uani 1 d . . . N12 N -0.1165(5) 0.3873(3) 0.0714(3) 0.0515(12) Uani 1 d . . . N32 N 0.0928(5) 0.3482(3) 0.1426(3) 0.0539(13) Uani 1 d . . . C61 C 0.3834(6) 0.7351(4) 0.0854(4) 0.0598(17) Uani 1 d . . . H61A H 0.3814 0.7873 0.0625 0.072 Uiso 1 calc R . . H61B H 0.4013 0.6963 0.0468 0.072 Uiso 1 calc R . . C51 C 0.4942(7) 0.7325(5) 0.1422(4) 0.071(2) Uani 1 d . . . H51A H 0.4814 0.7756 0.1773 0.086 Uiso 1 calc R . . H51B H 0.5783 0.7415 0.1171 0.086 Uiso 1 calc R . . C41 C 0.5021(6) 0.6546(5) 0.1844(4) 0.0637(19) Uani 1 d . . . H41A H 0.5279 0.6123 0.1507 0.076 Uiso 1 calc R . . H41B H 0.5699 0.6587 0.2225 0.076 Uiso 1 calc R . . C1 C 0.1680(7) 0.7855(3) 0.1409(4) 0.0605(17) Uani 1 d . . . H1 H 0.0904 0.7631 0.1663 0.073 Uiso 1 calc R . . C2 C 0.1182(12) 0.8250(5) 0.0705(6) 0.112(4) Uani 1 d . . . H2A H 0.1926 0.8430 0.0417 0.168 Uiso 1 calc R . . H2B H 0.0632 0.8697 0.0833 0.168 Uiso 1 calc R . . H2C H 0.0674 0.7874 0.0422 0.168 Uiso 1 calc R . . C3 C 0.2307(11) 0.8438(5) 0.1925(6) 0.102(3) Uani 1 d . . . H3A H 0.2574 0.8170 0.2372 0.153 Uiso 1 calc R . . H3B H 0.1678 0.8848 0.2045 0.153 Uiso 1 calc R . . H3C H 0.3071 0.8671 0.1692 0.153 Uiso 1 calc R . . C4 C 0.3821(6) 0.5815(4) 0.2845(3) 0.0574(16) Uani 1 d . . . H4 H 0.2922 0.5611 0.2934 0.069 Uiso 1 calc R . . C5 C 0.4710(8) 0.5106(5) 0.2737(5) 0.088(3) Uani 1 d . . . H5A H 0.4514 0.4859 0.2269 0.132 Uiso 1 calc R . . H5B H 0.4562 0.4730 0.3130 0.132 Uiso 1 calc R . . H5C H 0.5622 0.5274 0.2743 0.132 Uiso 1 calc R . . C6 C 0.4201(9) 0.6299(5) 0.3511(4) 0.083(2) Uani 1 d . . . H6A H 0.5073 0.6519 0.3439 0.125 Uiso 1 calc R . . H6B H 0.4202 0.5965 0.3943 0.125 Uiso 1 calc R . . H6C H 0.3572 0.6723 0.3577 0.125 Uiso 1 calc R . . C42 C 0.0427(15) 0.2710(5) 0.1380(9) 0.178(8) Uani 1 d . . . H42A H 0.1175 0.2367 0.1267 0.214 Uiso 1 calc R . . H42B H 0.0134 0.2568 0.1876 0.214 Uiso 1 calc R . . C52 C -0.0556(12) 0.2500(4) 0.0917(7) 0.126(4) Uani 1 d . . . H52A H -0.1210 0.2218 0.1213 0.151 Uiso 1 calc R . . H52B H -0.0183 0.2113 0.0576 0.151 Uiso 1 calc R . . C62 C -0.1267(11) 0.3055(4) 0.0481(6) 0.113(4) Uani 1 d . . . H62A H -0.2198 0.2905 0.0482 0.136 Uiso 1 calc R . . H62B H -0.0952 0.3017 -0.0027 0.136 Uiso 1 calc R . . C10 C 0.2140(6) 0.3620(4) 0.1847(4) 0.0598(17) Uani 1 d . . . H10 H 0.2364 0.4184 0.1784 0.072 Uiso 1 calc R . . C11 C 0.1967(10) 0.3488(7) 0.2655(5) 0.102(3) Uani 1 d . . . H11A H 0.1257 0.3818 0.2835 0.152 Uiso 1 calc R . . H11B H 0.2775 0.3623 0.2909 0.152 Uiso 1 calc R . . H11C H 0.1756 0.2939 0.2744 0.152 Uiso 1 calc R . . C12 C 0.3275(9) 0.3156(7) 0.1536(7) 0.117(4) Uani 1 d . . . H12A H 0.3171 0.2603 0.1661 0.175 Uiso 1 calc R . . H12B H 0.4094 0.3351 0.1741 0.175 Uiso 1 calc R . . H12C H 0.3292 0.3214 0.1006 0.175 Uiso 1 calc R . . C7 C -0.2220(6) 0.4414(4) 0.0481(4) 0.069(2) Uani 1 d . . . H7 H -0.1960 0.4954 0.0626 0.083 Uiso 1 calc R . . C8 C -0.2478(9) 0.4419(6) -0.0326(5) 0.093(3) Uani 1 d . . . H8A H -0.1672 0.4545 -0.0586 0.140 Uiso 1 calc R . . H8B H -0.3142 0.4811 -0.0438 0.140 Uiso 1 calc R . . H8C H -0.2788 0.3903 -0.0478 0.140 Uiso 1 calc R . . C9 C -0.3497(10) 0.4206(12) 0.0895(6) 0.187(8) Uani 1 d . . . H9A H -0.3584 0.3638 0.0927 0.280 Uiso 1 calc R . . H9B H -0.4246 0.4422 0.0633 0.280 Uiso 1 calc R . . H9C H -0.3464 0.4428 0.1386 0.280 Uiso 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 P2 0.0285(6) 0.0349(6) 0.0481(7) -0.0107(6) 0.0091(6) -0.0048(6) P4 0.0277(6) 0.0361(6) 0.0370(6) 0.0001(5) -0.0031(5) -0.0061(5) P6 0.0361(6) 0.0404(7) 0.0329(6) -0.0014(6) 0.0039(5) -0.0026(5) P8 0.0319(6) 0.0298(6) 0.0395(6) -0.0027(5) -0.0032(5) -0.0028(5) Cl21 0.0541(10) 0.0591(10) 0.195(3) -0.0084(14) -0.0488(14) 0.0125(9) Cl22 0.141(2) 0.0983(15) 0.0910(13) -0.0462(12) 0.0785(15) -0.0706(16) Cl61 0.150(2) 0.0722(12) 0.0792(13) 0.0093(10) -0.0514(15) 0.0232(14) Cl62 0.0555(10) 0.1254(17) 0.0857(13) -0.0445(13) 0.0231(10) 0.0024(11) N3 0.027(2) 0.046(2) 0.045(2) -0.007(2) 0.0013(18) -0.0056(19) N5 0.042(2) 0.048(2) 0.043(2) 0.001(2) 0.000(2) -0.004(2) N7 0.082(4) 0.087(4) 0.044(3) -0.005(3) 0.003(3) -0.044(4) N1 0.037(2) 0.044(3) 0.075(3) -0.020(2) 0.004(2) -0.005(2) N11 0.042(2) 0.044(2) 0.061(3) 0.008(2) -0.001(2) -0.008(2) N31 0.035(2) 0.061(3) 0.044(2) 0.011(2) -0.006(2) -0.014(2) N12 0.044(3) 0.041(2) 0.070(3) -0.011(2) -0.017(3) -0.007(2) N32 0.048(3) 0.031(2) 0.082(3) 0.001(2) -0.014(3) 0.000(2) C61 0.053(4) 0.062(4) 0.065(4) 0.021(3) 0.007(3) -0.014(3) C51 0.049(3) 0.088(5) 0.077(4) 0.016(4) 0.000(3) -0.034(4) C41 0.034(3) 0.099(5) 0.058(4) 0.012(4) -0.005(3) -0.017(3) C1 0.058(4) 0.035(3) 0.088(5) 0.000(3) -0.008(4) 0.005(3) C2 0.124(9) 0.075(5) 0.136(8) 0.028(6) -0.052(8) 0.011(6) C3 0.116(7) 0.066(5) 0.123(7) -0.025(5) -0.016(7) -0.010(5) C4 0.045(3) 0.069(4) 0.058(3) 0.022(3) -0.012(3) -0.020(3) C5 0.070(5) 0.073(5) 0.121(7) 0.027(5) -0.018(5) 0.000(4) C6 0.093(6) 0.106(6) 0.051(4) 0.007(4) -0.017(4) -0.029(5) C42 0.204(14) 0.037(4) 0.293(18) 0.027(7) -0.164(14) -0.030(6) C52 0.140(9) 0.039(4) 0.198(11) -0.012(5) -0.076(9) -0.008(5) C62 0.133(9) 0.053(4) 0.153(9) -0.014(5) -0.074(8) -0.021(5) C10 0.050(3) 0.048(3) 0.082(4) 0.015(3) -0.020(3) 0.001(3) C11 0.090(6) 0.128(8) 0.087(6) 0.028(6) -0.025(5) 0.000(6) C12 0.061(5) 0.138(9) 0.150(9) -0.010(8) -0.012(6) 0.039(6) C7 0.048(3) 0.071(4) 0.089(5) -0.026(4) -0.030(3) 0.013(3) C8 0.085(5) 0.102(6) 0.093(6) 0.019(5) -0.022(5) 0.006(6) C9 0.065(6) 0.38(3) 0.111(8) 0.014(13) 0.007(6) 0.081(11) _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 P2 N1 1.517(5) . ? P2 N3 1.530(4) . ? P2 Cl22 2.000(2) . ? P2 Cl21 2.033(3) . ? P4 N3 1.590(4) . ? P4 N5 1.603(5) . ? P4 N11 1.642(5) . ? P4 N31 1.642(4) . ? P6 N7 1.534(5) . ? P6 N5 1.547(5) . ? P6 Cl62 2.000(2) . ? P6 Cl61 2.012(2) . ? P8 N7 1.569(5) . ? P8 N1 1.578(5) . ? P8 N12 1.624(5) . ? P8 N32 1.631(5) . ? N11 C61 1.469(8) . ? N11 C1 1.473(8) . ? N31 C41 1.466(7) . ? N31 C4 1.477(7) . ? N12 C62 1.440(9) . ? N12 C7 1.459(8) . ? N32 C42 1.393(9) . ? N32 C10 1.455(8) . ? C61 C51 1.513(9) . ? C51 C41 1.517(10) . ? C1 C3 1.491(10) . ? C1 C2 1.516(11) . ? C4 C6 1.499(9) . ? C4 C5 1.502(10) . ? C42 C52 1.342(14) . ? C52 C62 1.413(12) . ? C10 C11 1.482(10) . ? C10 C12 1.492(11) . ? C7 C8 1.477(11) . ? C7 C9 1.526(13) . ? 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 P2 N3 125.9(3) . . ? N1 P2 Cl22 106.5(2) . . ? N3 P2 Cl22 104.95(19) . . ? N1 P2 Cl21 109.2(2) . . ? N3 P2 Cl21 107.1(2) . . ? Cl22 P2 Cl21 100.23(14) . . ? N3 P4 N5 116.7(2) . . ? N3 P4 N11 111.1(3) . . ? N5 P4 N11 108.7(2) . . ? N3 P4 N31 107.4(2) . . ? N5 P4 N31 107.6(3) . . ? N11 P4 N31 104.6(2) . . ? N7 P6 N5 122.6(3) . . ? N7 P6 Cl62 106.5(3) . . ? N5 P6 Cl62 106.5(2) . . ? N7 P6 Cl61 107.9(3) . . ? N5 P6 Cl61 111.9(2) . . ? Cl62 P6 Cl61 98.61(13) . . ? N7 P8 N1 113.0(3) . . ? N7 P8 N12 109.7(3) . . ? N1 P8 N12 110.1(3) . . ? N7 P8 N32 111.5(3) . . ? N1 P8 N32 108.9(3) . . ? N12 P8 N32 103.2(3) . . ? P2 N3 P4 131.5(3) . . ? P6 N5 P4 137.0(3) . . ? P6 N7 P8 134.5(4) . . ? P2 N1 P8 151.3(4) . . ? C61 N11 C1 118.8(5) . . ? C61 N11 P4 112.5(4) . . ? C1 N11 P4 122.6(4) . . ? C41 N31 C4 115.8(5) . . ? C41 N31 P4 114.1(4) . . ? C4 N31 P4 122.2(4) . . ? C62 N12 C7 117.3(6) . . ? C62 N12 P8 122.4(5) . . ? C7 N12 P8 118.7(4) . . ? C42 N32 C10 118.8(6) . . ? C42 N32 P8 123.1(6) . . ? C10 N32 P8 118.1(4) . . ? N11 C61 C51 112.0(5) . . ? C61 C51 C41 113.7(5) . . ? N31 C41 C51 111.6(6) . . ? N11 C1 C3 115.3(6) . . ? N11 C1 C2 107.5(7) . . ? C3 C1 C2 111.9(6) . . ? N31 C4 C6 109.1(5) . . ? N31 C4 C5 113.7(6) . . ? C6 C4 C5 112.5(6) . . ? C52 C42 N32 123.2(9) . . ? C42 C52 C62 123.0(7) . . ? C52 C62 N12 115.5(7) . . ? N32 C10 C11 113.0(6) . . ? N32 C10 C12 111.2(6) . . ? C11 C10 C12 112.4(8) . . ? N12 C7 C8 114.5(6) . . ? N12 C7 C9 109.2(8) . . ? C8 C7 C9 109.6(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.567 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.065 #=END data_compound7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H20 Cl4 N5 P3' _chemical_formula_weight 433.01 _chemical_melting_point 423 _chemical_compound_source 'K.C. Kumara Swamy' 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.449(3) _cell_length_b 11.725(3) _cell_length_c 13.366(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.67(2) _cell_angle_gamma 90.00 _cell_volume 1950.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13 _cell_measurement_theta_max 15 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3576 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3418 _reflns_number_gt 2228 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+2.1060P] 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_number_reflns 3418 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 1.507 _refine_ls_shift/su_mean 0.294 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P6 P 0.32660(9) 0.15735(10) 0.58040(8) 0.0452(3) Uani 1 d . . . P4 P 0.17221(10) 0.30348(11) 0.49417(9) 0.0525(4) Uani 1 d . . . P2 P 0.25447(10) 0.13540(12) 0.38100(9) 0.0559(4) Uani 1 d . . . Cl41 Cl 0.02135(11) 0.31007(17) 0.54426(12) 0.0896(5) Uani 1 d . . . Cl21 Cl 0.17977(16) -0.00083(16) 0.32427(15) 0.1065(7) Uani 1 d . . . Cl22 Cl 0.34708(15) 0.17683(18) 0.26375(11) 0.1020(6) Uani 1 d . . . Cl42 Cl 0.19383(15) 0.46827(14) 0.46075(13) 0.0932(5) Uani 1 d . . . N5 N 0.2512(3) 0.2697(3) 0.5796(3) 0.0522(9) Uani 1 d . . . N3 N 0.1683(3) 0.2325(4) 0.3933(3) 0.0715(13) Uani 1 d . . . N1 N 0.3255(3) 0.0973(3) 0.4705(3) 0.0534(10) Uani 1 d . . . N11 N 0.2857(3) 0.0706(4) 0.6664(3) 0.0614(11) Uani 1 d . . . N31 N 0.4493(3) 0.1899(3) 0.6115(3) 0.0516(9) Uani 1 d . . . C61 C 0.3574(5) 0.0152(6) 0.7385(5) 0.088(2) Uani 1 d . . . H61A H 0.3165 -0.0055 0.7971 0.106 Uiso 1 calc R . . H61B H 0.3844 -0.0547 0.7091 0.106 Uiso 1 calc R . . C51 C 0.4461(6) 0.0834(7) 0.7691(5) 0.099(2) Uani 1 d . . . H51A H 0.4948 0.0352 0.8072 0.119 Uiso 1 calc R . . H51B H 0.4194 0.1410 0.8146 0.119 Uiso 1 calc R . . C41 C 0.5074(5) 0.1403(7) 0.6947(5) 0.096(2) Uani 1 d . . . H41A H 0.5587 0.0863 0.6683 0.115 Uiso 1 calc R . . H41B H 0.5481 0.2006 0.7273 0.115 Uiso 1 calc R . . C1 C 0.1709(4) 0.0405(5) 0.6676(4) 0.0664(14) Uani 1 d . . . H1 H 0.1377 0.0752 0.6081 0.080 Uiso 1 calc R . . C2 C 0.1524(5) -0.0871(6) 0.6598(5) 0.093(2) Uani 1 d . . . H2A H 0.1916 -0.1169 0.6042 0.139 Uiso 1 calc R . . H2B H 0.0771 -0.1018 0.6500 0.139 Uiso 1 calc R . . H2C H 0.1766 -0.1235 0.7204 0.139 Uiso 1 calc R . . C3 C 0.1166(6) 0.0933(7) 0.7586(6) 0.111(2) Uani 1 d . . . H3A H 0.1498 0.0646 0.8187 0.166 Uiso 1 calc R . . H3B H 0.0417 0.0739 0.7578 0.166 Uiso 1 calc R . . H3C H 0.1243 0.1747 0.7563 0.166 Uiso 1 calc R . . C4 C 0.5105(4) 0.2603(5) 0.5413(4) 0.0643(13) Uani 1 d . . . H4 H 0.4617 0.2778 0.4853 0.077 Uiso 1 calc R . . C5 C 0.5425(8) 0.3718(6) 0.5859(7) 0.131(3) Uani 1 d . . . H5A H 0.4804 0.4088 0.6126 0.196 Uiso 1 calc R . . H5B H 0.5735 0.4191 0.5353 0.196 Uiso 1 calc R . . H5C H 0.5943 0.3592 0.6385 0.196 Uiso 1 calc R . . C6 C 0.6043(7) 0.2007(7) 0.4981(7) 0.140(4) Uani 1 d . . . H6A H 0.6557 0.1842 0.5502 0.210 Uiso 1 calc R . . H6B H 0.6369 0.2486 0.4487 0.210 Uiso 1 calc R . . H6C H 0.5809 0.1308 0.4673 0.210 Uiso 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 P6 0.0487(6) 0.0497(7) 0.0368(6) 0.0034(5) -0.0103(5) 0.0033(5) P4 0.0534(7) 0.0611(8) 0.0429(6) 0.0006(5) -0.0063(5) 0.0172(6) P2 0.0607(8) 0.0672(8) 0.0394(6) -0.0092(6) -0.0126(5) 0.0124(6) Cl41 0.0560(8) 0.1305(15) 0.0823(10) -0.0047(10) 0.0041(7) 0.0260(9) Cl21 0.1157(14) 0.0933(12) 0.1093(13) -0.0279(10) -0.0551(11) -0.0038(10) Cl22 0.1166(14) 0.1344(16) 0.0553(8) 0.0095(9) 0.0212(8) 0.0278(12) Cl42 0.1146(13) 0.0663(9) 0.0983(12) 0.0225(8) -0.0211(10) 0.0128(9) N5 0.060(2) 0.059(2) 0.0373(18) -0.0046(17) -0.0078(16) 0.0168(19) N3 0.075(3) 0.094(3) 0.044(2) -0.009(2) -0.020(2) 0.037(3) N1 0.059(2) 0.054(2) 0.047(2) -0.0094(18) -0.0138(17) 0.0150(19) N11 0.059(2) 0.070(3) 0.055(2) 0.021(2) -0.0103(19) -0.003(2) N31 0.050(2) 0.058(2) 0.046(2) 0.0056(18) -0.0126(17) -0.0012(18) C61 0.095(4) 0.097(5) 0.071(4) 0.041(4) -0.023(3) -0.009(4) C51 0.106(5) 0.119(6) 0.072(4) 0.044(4) -0.041(4) -0.015(4) C41 0.070(4) 0.139(6) 0.078(4) 0.040(4) -0.034(3) -0.012(4) C1 0.062(3) 0.078(4) 0.059(3) 0.014(3) -0.002(2) -0.008(3) C2 0.084(4) 0.084(5) 0.110(5) -0.004(4) 0.006(4) -0.021(4) C3 0.103(5) 0.121(6) 0.108(6) -0.006(5) 0.029(4) -0.013(5) C4 0.062(3) 0.066(3) 0.064(3) 0.005(3) -0.012(2) -0.003(3) C5 0.167(8) 0.074(5) 0.153(8) -0.021(5) 0.047(6) -0.035(5) C6 0.170(8) 0.101(6) 0.152(8) 0.025(5) 0.106(7) 0.033(6) _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 P6 N5 1.617(4) . ? P6 N11 1.622(4) . ? P6 N31 1.623(4) . ? P6 N1 1.629(4) . ? P4 N5 1.550(4) . ? P4 N3 1.585(4) . ? P4 Cl42 2.002(2) . ? P4 Cl41 2.0027(19) . ? P4 P2 2.6938(18) . ? P2 N1 1.545(4) . ? P2 N3 1.574(4) . ? P2 Cl21 1.994(2) . ? P2 Cl22 2.016(2) . ? N11 C61 1.458(6) . ? N11 C1 1.472(6) . ? N31 C41 1.443(6) . ? N31 C4 1.470(6) . ? C61 C51 1.419(9) . ? C51 C41 1.426(8) . ? C1 C2 1.517(8) . ? C1 C3 1.528(9) . ? C4 C5 1.488(9) . ? C4 C6 1.484(8) . ? 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 N5 P6 N11 109.2(2) . . ? N5 P6 N31 110.7(2) . . ? N11 P6 N31 105.6(2) . . ? N5 P6 N1 110.35(18) . . ? N11 P6 N1 111.6(2) . . ? N31 P6 N1 109.3(2) . . ? N5 P4 N3 120.4(2) . . ? N5 P4 Cl42 108.97(18) . . ? N3 P4 Cl42 108.7(2) . . ? N5 P4 Cl41 110.66(16) . . ? N3 P4 Cl41 106.58(19) . . ? Cl42 P4 Cl41 99.58(10) . . ? N5 P4 P2 89.14(14) . . ? N3 P4 P2 31.35(14) . . ? Cl42 P4 P2 121.86(8) . . ? Cl41 P4 P2 125.46(9) . . ? N1 P2 N3 120.9(2) . . ? N1 P2 Cl21 108.84(17) . . ? N3 P2 Cl21 107.7(2) . . ? N1 P2 Cl22 110.13(17) . . ? N3 P2 Cl22 107.67(19) . . ? Cl21 P2 Cl22 99.54(10) . . ? N1 P2 P4 89.70(15) . . ? N3 P2 P4 31.60(14) . . ? Cl21 P2 P4 128.39(9) . . ? Cl22 P2 P4 119.01(9) . . ? P4 N5 P6 125.1(2) . . ? P2 N3 P4 117.1(2) . . ? P2 N1 P6 124.9(2) . . ? C61 N11 C1 118.2(4) . . ? C61 N11 P6 123.5(4) . . ? C1 N11 P6 118.1(3) . . ? C41 N31 C4 117.4(4) . . ? C41 N31 P6 124.4(4) . . ? C4 N31 P6 117.5(3) . . ? C51 C61 N11 114.0(5) . . ? C61 C51 C41 118.9(6) . . ? C51 C41 N31 117.3(5) . . ? N11 C1 C2 112.5(5) . . ? N11 C1 C3 110.5(5) . . ? C2 C1 C3 112.7(5) . . ? N31 C4 C5 112.1(5) . . ? N31 C4 C6 113.6(5) . . ? C5 C4 C6 111.2(6) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.535 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.075 #=END data_Compound8 _audit_creation_method SHELXL _chemical_name_systematic ; 1,9-Di(tert-butyl)-11-chloro-11-(N-dichlorphosphoryl)imino-3,7-dimethyl- dibenzo[d,g]-[1,3]-dioxa-[2\l^5]-phospha-[4,7]-cyclooctadien ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H30 Cl3 N O3 P2' _chemical_formula_weight 536.77 _chemical_melting_point 461 _chemical_compound_source K.C. Kumara Swamy 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.188(2) _cell_length_b 17.743(2) _cell_length_c 26.405(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5241.6(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method ? _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.9903 _exptl_absorpt_correction_T_max 0.9998 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710690 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'enraf-nonius CAD4' _diffrn_measurement_method 'omega scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 4539 _diffrn_reflns_av_R_equivalents 0.0065 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.91 _reflns_number_total 4536 _reflns_number_observed 3059 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL-88 (univ.Freiburg, 1988)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+1.2610P] 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 'isotropic U only' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4536 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_obs 0.0562 _refine_ls_wR_factor_all 0.1496 _refine_ls_wR_factor_obs 0.1311 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.172 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 1.172 _refine_ls_shift/esd_max -0.041 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.02876(10) 0.24851(6) 0.15890(4) 0.0464(3) Uani 1 d . . P2 P 0.05240(8) 0.10393(5) 0.10824(3) 0.0347(3) Uani 1 d . . Cl1 Cl 0.15665(13) 0.21548(8) 0.20813(5) 0.0810(4) Uani 1 d . . Cl2 Cl -0.11510(13) 0.25223(9) 0.20396(5) 0.0872(5) Uani 1 d . . Cl3 Cl -0.05165(9) 0.05134(6) 0.05915(4) 0.0482(3) Uani 1 d . . O1 O 0.0545(3) 0.3222(2) 0.1392(2) 0.0873(12) Uani 1 d . . O2 O 0.0582(2) 0.05247(13) 0.15609(9) 0.0396(6) Uani 1 d . . O3 O 0.1779(2) 0.11036(12) 0.08307(9) 0.0354(6) Uani 1 d . . N1 N 0.0055(3) 0.1823(2) 0.12124(12) 0.0442(8) Uani 1 d . . C1 C 0.0486(3) -0.0280(2) 0.15734(13) 0.0390(9) Uani 1 d . . C2 C -0.0509(4) -0.0595(2) 0.18158(14) 0.0429(9) Uani 1 d . . C3 C -0.0544(4) -0.1378(2) 0.17921(15) 0.0497(10) Uani 1 d . . H3 H -0.1191(4) -0.1621(2) 0.19404(15) 0.038(5) Uiso 1 calc R . C4 C 0.0320(4) -0.1818(2) 0.15626(14) 0.0474(10) Uani 1 d . . C5 C 0.1319(4) -0.1464(2) 0.13636(14) 0.0468(10) Uani 1 d . . H5 H 0.1928(4) -0.1755(2) 0.12250(14) 0.038(5) Uiso 1 calc R . C6 C 0.1431(3) -0.0682(2) 0.13667(13) 0.0399(9) Uani 1 d . . C7 C -0.1440(4) -0.0134(2) 0.2108(2) 0.0513(11) Uani 1 d . . C8 C -0.2150(4) 0.0388(3) 0.1762(2) 0.0679(13) Uani 1 d . . H8A H -0.2793(17) 0.0612(13) 0.1950(3) 0.091(4) Uiso 1 calc R . H8B H -0.2469(23) 0.0104(4) 0.1484(6) 0.091(4) Uiso 1 calc R . H8C H -0.1634(8) 0.0777(10) 0.1635(9) 0.091(4) Uiso 1 calc R . C9 C -0.0823(5) 0.0324(3) 0.2524(2) 0.0678(13) Uani 1 d . . H9A H -0.1406(6) 0.0620(13) 0.2701(8) 0.091(4) Uiso 1 calc R . H9B H -0.0238(19) 0.0651(13) 0.2374(2) 0.091(4) Uiso 1 calc R . H9C H -0.0436(23) -0.0012(3) 0.2757(7) 0.091(4) Uiso 1 calc R . C10 C -0.2355(5) -0.0652(3) 0.2366(2) 0.078(2) Uani 1 d . . H10A H -0.2951(16) -0.0351(3) 0.2532(10) 0.091(4) Uiso 1 calc R . H10B H -0.1956(6) -0.0963(12) 0.2612(8) 0.091(4) Uiso 1 calc R . H10C H -0.2730(20) -0.0966(12) 0.2116(2) 0.091(4) Uiso 1 calc R . C11 C 0.2350(3) 0.0608(2) 0.04774(13) 0.0330(8) Uani 1 d . . C12 C 0.2594(3) 0.0886(2) -0.00052(13) 0.0354(8) Uani 1 d . . C13 C 0.3184(3) 0.0373(2) -0.03199(14) 0.0397(9) Uani 1 d . . H13 H 0.3363(3) 0.0522(2) -0.06488(14) 0.038(5) Uiso 1 calc R . C14 C 0.3518(3) -0.0346(2) -0.01706(15) 0.0408(9) Uani 1 d . . C15 C 0.3293(3) -0.0568(2) 0.03211(14) 0.0407(9) Uani 1 d . . H15 H 0.3535(3) -0.1043(2) 0.04286(14) 0.038(5) Uiso 1 calc R . C16 C 0.2711(3) -0.0092(2) 0.06568(13) 0.0348(8) Uani 1 d . . C17 C 0.2312(3) 0.1688(2) -0.01836(14) 0.0426(9) Uani 1 d . . C18 C 0.2787(5) 0.1839(3) -0.0717(2) 0.0715(15) Uani 1 d . . H18A H 0.2614(25) 0.2350(6) -0.0811(5) 0.091(4) Uiso 1 calc R . H18B H 0.2410(20) 0.1502(12) -0.0952(2) 0.091(4) Uiso 1 calc R . H18C H 0.3636(6) 0.1760(17) -0.0723(3) 0.091(4) Uiso 1 calc R . C19 C 0.2872(5) 0.2271(2) 0.0171(2) 0.0670(14) Uani 1 d . . H19A H 0.2527(20) 0.2222(12) 0.0502(4) 0.091(4) Uiso 1 calc R . H19B H 0.2720(25) 0.2768(2) 0.0043(7) 0.091(4) Uiso 1 calc R . H19C H 0.3718(6) 0.2188(11) 0.0190(9) 0.091(4) Uiso 1 calc R . C20 C 0.0953(4) 0.1822(3) -0.0211(2) 0.0615(12) Uani 1 d . . H20A H 0.0799(4) 0.2305(8) -0.0360(11) 0.091(4) Uiso 1 calc R . H20B H 0.0622(6) 0.1808(17) 0.0124(2) 0.091(4) Uiso 1 calc R . H20C H 0.0590(5) 0.1435(10) -0.0414(10) 0.091(4) Uiso 1 calc R . C21 C 0.2583(3) -0.0304(2) 0.12087(14) 0.0415(9) Uani 1 d . . H21A H 0.3239(3) -0.0638(2) 0.12959(14) 0.054(8) Uiso 1 calc R . H21B H 0.2675(3) 0.0150(2) 0.14092(14) 0.054(8) Uiso 1 calc R . C22 C 0.0205(5) -0.2670(2) 0.1541(2) 0.0659(13) Uani 1 d . . H22A H 0.0751(20) -0.2866(3) 0.1293(9) 0.091(4) Uiso 1 calc R . H22B H -0.0597(8) -0.2803(2) 0.1449(11) 0.091(4) Uiso 1 calc R . H22C H 0.0390(28) -0.2880(3) 0.1867(4) 0.091(4) Uiso 1 calc R . C23 C 0.4154(4) -0.0862(2) -0.0542(2) 0.0570(11) Uani 1 d . . H23A H 0.4669(21) -0.0569(3) -0.0756(8) 0.091(4) Uiso 1 calc R . H23B H 0.3573(4) -0.1120(13) -0.0746(8) 0.091(4) Uiso 1 calc R . H23C H 0.4621(22) -0.1225(11) -0.0359(2) 0.091(4) Uiso 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 0.0453(6) 0.0391(6) 0.0548(7) -0.0021(5) -0.0037(5) -0.0007(5) P2 0.0326(5) 0.0382(5) 0.0332(5) -0.0029(4) 0.0010(4) 0.0002(4) Cl1 0.0751(9) 0.0822(9) 0.0856(9) -0.0110(7) -0.0368(7) 0.0059(7) Cl2 0.0822(10) 0.1058(11) 0.0736(9) -0.0146(8) 0.0252(7) 0.0335(9) Cl3 0.0443(6) 0.0580(6) 0.0421(5) -0.0071(4) -0.0043(4) -0.0115(5) O1 0.088(3) 0.049(2) 0.125(3) 0.021(2) -0.023(2) -0.024(2) O2 0.044(2) 0.0387(14) 0.0361(14) -0.0005(11) 0.0048(12) -0.0021(12) O3 0.0328(13) 0.0329(13) 0.0404(14) -0.0023(11) 0.0041(11) 0.0020(11) N1 0.045(2) 0.044(2) 0.044(2) -0.004(2) 0.0021(15) 0.0096(15) C1 0.043(2) 0.041(2) 0.033(2) 0.002(2) -0.004(2) -0.001(2) C2 0.046(2) 0.050(2) 0.032(2) 0.003(2) 0.002(2) -0.007(2) C3 0.054(3) 0.050(2) 0.045(2) 0.005(2) 0.007(2) -0.012(2) C4 0.063(3) 0.045(2) 0.035(2) 0.003(2) -0.003(2) -0.010(2) C5 0.063(3) 0.042(2) 0.035(2) -0.001(2) -0.005(2) 0.006(2) C6 0.046(2) 0.042(2) 0.031(2) 0.005(2) -0.005(2) 0.000(2) C7 0.052(3) 0.055(3) 0.047(2) 0.002(2) 0.015(2) -0.009(2) C8 0.049(3) 0.080(3) 0.074(3) 0.005(3) 0.017(2) 0.007(3) C9 0.070(3) 0.082(3) 0.051(3) -0.009(3) 0.018(2) -0.005(3) C10 0.073(3) 0.075(3) 0.086(4) 0.007(3) 0.040(3) -0.004(3) C11 0.027(2) 0.035(2) 0.037(2) -0.008(2) 0.0009(15) -0.001(2) C12 0.030(2) 0.039(2) 0.038(2) 0.001(2) -0.004(2) -0.004(2) C13 0.034(2) 0.047(2) 0.038(2) -0.004(2) 0.001(2) -0.003(2) C14 0.031(2) 0.042(2) 0.048(2) -0.009(2) 0.000(2) 0.000(2) C15 0.036(2) 0.033(2) 0.053(2) 0.000(2) 0.000(2) 0.004(2) C16 0.027(2) 0.035(2) 0.042(2) 0.003(2) -0.0011(15) -0.003(2) C17 0.040(2) 0.041(2) 0.046(2) 0.006(2) 0.002(2) 0.003(2) C18 0.085(4) 0.067(3) 0.063(3) 0.024(3) 0.030(3) 0.016(3) C19 0.072(3) 0.045(2) 0.085(3) 0.006(2) -0.010(3) -0.012(2) C20 0.047(3) 0.061(3) 0.077(3) 0.021(2) -0.002(2) 0.008(2) C21 0.043(2) 0.040(2) 0.042(2) 0.004(2) -0.002(2) 0.007(2) C22 0.093(4) 0.048(3) 0.057(3) 0.001(2) 0.000(3) -0.015(2) C23 0.055(3) 0.054(3) 0.062(3) -0.018(2) 0.013(2) 0.008(2) _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 O1 1.437(3) . yes P1 N1 1.560(3) . yes P1 Cl2 2.003(2) . yes P1 Cl1 2.020(2) . yes P2 N1 1.526(3) . yes P2 O3 1.558(2) . yes P2 O2 1.560(2) . yes P2 Cl3 1.9764(13) . yes O2 C1 1.432(4) . yes O3 C11 1.432(4) . yes C1 C6 1.388(5) . no C1 C2 1.400(5) . no C2 C3 1.391(5) . no C2 C7 1.533(6) . no C3 C4 1.382(6) . no C4 C5 1.385(6) . no C4 C22 1.518(5) . no C5 C6 1.393(5) . no C6 C21 1.512(5) . no C7 C8 1.525(6) . no C7 C9 1.531(6) . no C7 C10 1.535(6) . no C11 C16 1.390(5) . no C11 C12 1.393(5) . no C12 C13 1.399(5) . no C12 C17 1.532(5) . no C13 C14 1.385(5) . no C14 C15 1.380(5) . no C14 C23 1.519(5) . no C15 C16 1.387(5) . no C16 C21 1.512(5) . no C17 C19 1.529(6) . no C17 C18 1.530(5) . no C17 C20 1.541(6) . no 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 P1 N1 119.2(2) . . yes O1 P1 Cl2 110.3(2) . . yes N1 P1 Cl2 105.62(14) . . yes O1 P1 Cl1 110.8(2) . . yes N1 P1 Cl1 108.07(14) . . yes Cl2 P1 Cl1 101.34(8) . . yes N1 P2 O3 109.8(2) . . yes N1 P2 O2 111.5(2) . . yes O3 P2 O2 110.55(13) . . yes N1 P2 Cl3 112.04(14) . . yes O3 P2 Cl3 106.60(10) . . yes O2 P2 Cl3 106.21(10) . . yes C1 O2 P2 126.8(2) . . yes C11 O3 P2 129.4(2) . . yes P2 N1 P1 140.5(2) . . yes C6 C1 C2 125.5(3) . . ? C6 C1 O2 116.5(3) . . ? C2 C1 O2 117.9(3) . . ? C3 C2 C1 113.6(4) . . ? C3 C2 C7 122.4(4) . . ? C1 C2 C7 123.9(3) . . ? C4 C3 C2 124.4(4) . . ? C3 C4 C5 118.3(4) . . ? C3 C4 C22 121.3(4) . . ? C5 C4 C22 120.3(4) . . ? C4 C5 C6 121.5(4) . . ? C1 C6 C5 116.5(4) . . ? C1 C6 C21 122.0(3) . . ? C5 C6 C21 121.1(4) . . ? C8 C7 C9 110.0(4) . . ? C8 C7 C2 112.1(3) . . ? C9 C7 C2 109.7(4) . . ? C8 C7 C10 106.4(4) . . ? C9 C7 C10 107.5(4) . . ? C2 C7 C10 111.0(4) . . ? C16 C11 C12 124.8(3) . . ? C16 C11 O3 117.1(3) . . ? C12 C11 O3 117.8(3) . . ? C11 C12 C13 113.9(3) . . ? C11 C12 C17 124.7(3) . . ? C13 C12 C17 121.3(3) . . ? C14 C13 C12 123.9(3) . . ? C15 C14 C13 118.8(3) . . ? C15 C14 C23 121.3(4) . . ? C13 C14 C23 119.9(4) . . ? C14 C15 C16 120.9(3) . . ? C15 C16 C11 117.6(3) . . ? C15 C16 C21 120.6(3) . . ? C11 C16 C21 121.6(3) . . ? C19 C17 C18 107.7(4) . . ? C19 C17 C12 110.8(3) . . ? C18 C17 C12 112.0(3) . . ? C19 C17 C20 109.2(4) . . ? C18 C17 C20 105.8(4) . . ? C12 C17 C20 111.2(3) . . ? C6 C21 C16 117.2(3) . . yes _refine_diff_density_max 0.414 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.084 #=======================================================================