Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Coles, Simon J.' 'Davies, D.' 'Eaton, Robert J.' 'Hursthouse, Michael B.' 'Kilic, Adam' 'Mayer, Thomas A.' 'Shaw, R.' 'Yenilmez, Gonul' _publ_contact_author_name 'Dr D Davies' _publ_contact_author_address ; Dr D Davies Department of Chemistry Birkbeck College Gordon House 29 Gordon Square LONDON WC1 0PP UK ; _publ_section_title ; Chiral configurations of spermine-bridged cyclo-triphosphazatrienes ; data_3ca _database_code_CSD 166075 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Cl4 N10 P6' _chemical_formula_weight 918.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 32.910(7) _cell_length_b 10.436(2) _cell_length_c 13.554(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4655.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23324 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.9428 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\\f and \\w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21779 _diffrn_reflns_av_R_equivalents 0.0921 _diffrn_reflns_av_sigmaI/netI 0.1624 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.52 _reflns_number_total 7869 _reflns_number_gt 3880 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Pearce 1995)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00106(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(7) _refine_ls_number_reflns 7869 _refine_ls_number_parameters 516 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1583 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.05787(19) 0.4802(5) 0.6541(5) 0.0561(16) Uani 1 1 d . . . C2 C 0.0180(2) 0.5002(6) 0.6797(6) 0.085(2) Uani 1 1 d . . . H2 H 0.0099 0.4884 0.7463 0.102 Uiso 1 1 calc R . . C3 C -0.0100(2) 0.5366(9) 0.6112(9) 0.123(3) Uani 1 1 d . . . H3 H -0.0374 0.5504 0.6300 0.148 Uiso 1 1 calc R . . C4 C 0.0016(3) 0.5530(8) 0.5159(8) 0.122(3) Uani 1 1 d . . . H4 H -0.0179 0.5784 0.4681 0.147 Uiso 1 1 calc R . . C5 C 0.0419(3) 0.5331(7) 0.4872(6) 0.110(3) Uani 1 1 d . . . H5 H 0.0500 0.5437 0.4204 0.132 Uiso 1 1 calc R . . C6 C 0.0694(2) 0.4980(6) 0.5581(6) 0.080(2) Uani 1 1 d . . . H6 H 0.0971 0.4858 0.5402 0.096 Uiso 1 1 calc R . . C7 C 0.10694(17) 0.5959(5) 0.8007(5) 0.0532(16) Uani 1 1 d . . . C8 C 0.11041(18) 0.6130(5) 0.8999(5) 0.0713(19) Uani 1 1 d . . . H8 H 0.1058 0.5418 0.9421 0.086 Uiso 1 1 calc R . . C9 C 0.12037(18) 0.7300(8) 0.9419(7) 0.090(2) Uani 1 1 d . . . H9 H 0.1228 0.7383 1.0114 0.108 Uiso 1 1 calc R . . C10 C 0.1265(2) 0.8318(8) 0.8824(9) 0.101(3) Uani 1 1 d . . . H10 H 0.1341 0.9120 0.9101 0.121 Uiso 1 1 calc R . . C11 C 0.1221(2) 0.8206(7) 0.7849(9) 0.100(3) Uani 1 1 d . . . H11 H 0.1252 0.8944 0.7446 0.120 Uiso 1 1 calc R . . C12 C 0.11297(17) 0.7022(6) 0.7403(6) 0.083(2) Uani 1 1 d . . . H12 H 0.1110 0.6950 0.6706 0.100 Uiso 1 1 calc R . . C13 C 0.19661(18) 0.0581(5) 0.6608(5) 0.0660(18) Uani 1 1 d . . . H13A H 0.1994 0.0086 0.5989 0.079 Uiso 1 1 calc R . . H13B H 0.1899 -0.0029 0.7143 0.079 Uiso 1 1 calc R . . C14 C 0.23619(18) 0.1221(5) 0.6839(4) 0.0674(19) Uani 1 1 d . . . H14A H 0.2437 0.1793 0.6286 0.081 Uiso 1 1 calc R . . H14B H 0.2576 0.0560 0.6901 0.081 Uiso 1 1 calc R . . C15 C 0.23446(17) 0.1990(5) 0.7776(5) 0.0662(18) Uani 1 1 d . . . H15A H 0.2305 0.1403 0.8341 0.079 Uiso 1 1 calc R . . H15B H 0.2607 0.2437 0.7870 0.079 Uiso 1 1 calc R . . C16 C 0.20431(16) 0.3848(5) 0.8599(4) 0.0580(16) Uani 1 1 d . . . H16A H 0.2189 0.3443 0.9157 0.070 Uiso 1 1 calc R . . H16B H 0.1767 0.4080 0.8825 0.070 Uiso 1 1 calc R . . C17 C 0.22701(17) 0.5056(5) 0.8270(5) 0.0694(18) Uani 1 1 d . . . H17A H 0.2536 0.4806 0.7988 0.083 Uiso 1 1 calc R . . H17B H 0.2112 0.5486 0.7744 0.083 Uiso 1 1 calc R . . C18 C 0.23395(17) 0.5994(5) 0.9112(4) 0.0671(18) Uani 1 1 d . . . H18A H 0.2508 0.5594 0.9632 0.080 Uiso 1 1 calc R . . H18B H 0.2077 0.6253 0.9406 0.080 Uiso 1 1 calc R . . C19 C 0.25588(16) 0.7166(5) 0.8671(4) 0.0632(17) Uani 1 1 d . . . H19A H 0.2802 0.6875 0.8304 0.076 Uiso 1 1 calc R . . H19B H 0.2375 0.7602 0.8199 0.076 Uiso 1 1 calc R . . C20 C 0.23504(16) 0.8939(5) 0.9742(4) 0.0587(17) Uani 1 1 d . . . H20A H 0.2114 0.8414 0.9945 0.070 Uiso 1 1 calc R . . H20B H 0.2267 0.9466 0.9169 0.070 Uiso 1 1 calc R . . C21 C 0.24714(18) 0.9819(5) 1.0590(5) 0.0650(18) Uani 1 1 d . . . H21A H 0.2243 1.0404 1.0744 0.078 Uiso 1 1 calc R . . H21B H 0.2528 0.9298 1.1185 0.078 Uiso 1 1 calc R . . C22 C 0.28437(17) 1.0599(5) 1.0333(4) 0.0567(16) Uani 1 1 d . . . H22A H 0.2786 1.1129 0.9744 0.068 Uiso 1 1 calc R . . H22B H 0.2908 1.1184 1.0886 0.068 Uiso 1 1 calc R . . C23 C 0.36341(16) 0.5334(5) 0.8457(5) 0.0554(16) Uani 1 1 d . . . C24 C 0.3543(2) 0.4806(6) 0.7561(6) 0.083(2) Uani 1 1 d . . . H24 H 0.3546 0.5321 0.6983 0.100 Uiso 1 1 calc R . . C25 C 0.3445(2) 0.3499(8) 0.7500(7) 0.103(2) Uani 1 1 d . . . H25 H 0.3373 0.3139 0.6881 0.123 Uiso 1 1 calc R . . C26 C 0.3452(2) 0.2746(6) 0.8310(8) 0.095(2) Uani 1 1 d . . . H26 H 0.3399 0.1854 0.8250 0.114 Uiso 1 1 calc R . . C27 C 0.3533(2) 0.3261(6) 0.9214(7) 0.103(3) Uani 1 1 d . . . H27 H 0.3527 0.2743 0.9790 0.124 Uiso 1 1 calc R . . C28 C 0.36258(18) 0.4564(6) 0.9274(6) 0.084(2) Uani 1 1 d . . . H28 H 0.3685 0.4928 0.9901 0.101 Uiso 1 1 calc R . . C29 C 0.42756(19) 0.7035(5) 0.8999(6) 0.0619(19) Uani 1 1 d . . . C30 C 0.4583(3) 0.7174(5) 0.8322(6) 0.091(2) Uani 1 1 d . . . H30 H 0.4517 0.7295 0.7646 0.110 Uiso 1 1 calc R . . C31 C 0.4987(3) 0.7141(9) 0.8605(11) 0.134(4) Uani 1 1 d . . . H31 H 0.5197 0.7258 0.8132 0.161 Uiso 1 1 calc R . . C32 C 0.5077(3) 0.6945(9) 0.9546(13) 0.133(5) Uani 1 1 d . . . H32 H 0.5355 0.6880 0.9733 0.159 Uiso 1 1 calc R . . C33 C 0.4779(3) 0.6830(7) 1.0273(8) 0.120(3) Uani 1 1 d . . . H33 H 0.4849 0.6734 1.0949 0.143 Uiso 1 1 calc R . . C34 C 0.4377(2) 0.6862(6) 0.9971(6) 0.083(2) Uani 1 1 d . . . H34 H 0.4167 0.6761 1.0447 0.100 Uiso 1 1 calc R . . N1 N 0.13286(12) 0.1818(3) 0.8277(3) 0.0505(12) Uani 1 1 d . . . N2 N 0.13340(12) 0.3787(3) 0.6975(3) 0.0445(12) Uani 1 1 d . . . N3 N 0.07292(12) 0.3610(3) 0.8341(3) 0.0547(12) Uani 1 1 d . . . N4 N 0.16303(14) 0.1512(4) 0.6499(4) 0.0505(13) Uani 1 1 d . . . N5 N 0.20159(13) 0.2938(4) 0.7768(3) 0.0464(12) Uani 1 1 d . . . N6 N 0.26846(12) 0.8089(3) 0.9447(3) 0.0490(11) Uani 1 1 d . . . N7 N 0.31949(14) 0.9782(4) 1.0134(3) 0.0463(13) Uani 1 1 d . . . N8 N 0.37220(14) 0.7649(4) 0.7530(3) 0.0647(14) Uani 1 1 d . . . N9 N 0.34761(11) 0.7599(3) 0.9447(3) 0.0469(11) Uani 1 1 d . . . N10 N 0.31659(12) 0.9374(3) 0.8203(3) 0.0483(12) Uani 1 1 d . . . P1 P 0.15580(4) 0.25419(12) 0.73958(12) 0.0434(4) Uani 1 1 d . . . P2 P 0.09415(4) 0.44213(11) 0.74837(12) 0.0474(4) Uani 1 1 d . . . P3 P 0.09024(5) 0.22655(13) 0.86552(12) 0.0540(5) Uani 1 1 d . . . P4 P 0.37568(5) 0.70039(12) 0.86074(13) 0.0539(4) Uani 1 1 d . . . P5 P 0.34233(6) 0.87839(13) 0.73493(13) 0.0674(5) Uani 1 1 d . . . P6 P 0.31445(4) 0.86877(12) 0.92719(12) 0.0455(4) Uani 1 1 d . . . Cl1 Cl 0.09037(6) 0.21651(18) 1.01332(14) 0.1017(7) Uani 1 1 d U . . Cl2 Cl 0.04788(5) 0.09380(14) 0.83642(19) 0.1114(7) Uani 1 1 d U . . Cl3 Cl 0.3010(3) 0.8103(9) 0.6294(8) 0.094(3) Uani 0.52(5) 1 d PU . . Cl3' Cl 0.3111(12) 0.849(4) 0.6167(14) 0.160(8) Uani 0.48(5) 1 d PU . . Cl4 Cl 0.3673(9) 1.0171(6) 0.6580(7) 0.101(5) Uani 0.71(5) 1 d PU . . Cl4' Cl 0.3884(16) 1.0226(19) 0.698(6) 0.129(14) Uani 0.29(5) 1 d PU . . H4N H 0.1641(15) 0.194(4) 0.596(4) 0.047(19) Uiso 1 1 d . . . H7N H 0.3324(12) 0.947(4) 1.066(3) 0.021(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(5) 0.060(4) 0.066(5) -0.003(3) -0.008(4) 0.012(3) C2 0.048(5) 0.115(5) 0.091(6) -0.015(4) -0.014(5) 0.015(4) C3 0.054(6) 0.195(9) 0.121(9) -0.036(8) -0.016(7) 0.041(5) C4 0.100(8) 0.137(7) 0.130(10) -0.029(7) -0.061(7) 0.054(6) C5 0.108(7) 0.140(6) 0.084(7) 0.005(5) -0.021(6) 0.042(6) C6 0.064(5) 0.110(5) 0.064(5) -0.001(4) -0.017(5) 0.032(4) C7 0.057(4) 0.050(4) 0.053(5) -0.007(3) 0.001(3) 0.004(3) C8 0.081(5) 0.049(4) 0.083(6) -0.014(4) -0.002(4) 0.003(3) C9 0.093(6) 0.082(5) 0.096(6) -0.026(5) -0.029(5) 0.019(4) C10 0.064(5) 0.080(6) 0.159(10) -0.040(7) -0.040(6) 0.012(4) C11 0.085(6) 0.049(5) 0.168(9) 0.021(5) -0.009(6) -0.009(4) C12 0.089(5) 0.061(4) 0.100(6) 0.016(5) -0.003(5) -0.009(4) C13 0.065(5) 0.054(3) 0.079(5) -0.007(3) -0.002(4) 0.013(4) C14 0.067(5) 0.061(4) 0.074(5) -0.001(4) -0.006(4) 0.028(4) C15 0.053(4) 0.063(4) 0.082(5) 0.013(4) -0.014(4) 0.016(3) C16 0.053(4) 0.063(4) 0.058(4) -0.006(3) -0.007(4) -0.009(3) C17 0.069(4) 0.071(4) 0.068(5) -0.011(4) 0.009(4) -0.009(3) C18 0.061(4) 0.071(4) 0.070(5) -0.010(4) 0.002(4) -0.015(3) C19 0.059(4) 0.069(4) 0.062(4) -0.010(4) -0.002(4) -0.017(3) C20 0.044(4) 0.063(3) 0.069(5) 0.008(3) 0.000(3) -0.001(3) C21 0.068(5) 0.063(4) 0.065(5) -0.008(3) 0.013(4) 0.016(3) C22 0.065(5) 0.049(3) 0.056(4) -0.008(3) -0.001(3) 0.006(3) C23 0.063(4) 0.047(3) 0.056(5) 0.002(4) 0.003(4) -0.002(3) C24 0.109(6) 0.064(5) 0.077(6) -0.008(4) 0.003(5) 0.003(4) C25 0.135(7) 0.080(6) 0.094(7) -0.025(5) -0.001(6) -0.011(5) C26 0.097(6) 0.056(4) 0.132(8) -0.026(6) 0.015(6) -0.004(4) C27 0.130(7) 0.061(5) 0.118(8) 0.007(5) -0.001(6) -0.010(4) C28 0.109(6) 0.050(4) 0.093(6) -0.020(4) 0.001(5) -0.013(3) C29 0.041(4) 0.053(3) 0.092(6) -0.002(4) 0.007(4) 0.003(3) C30 0.068(6) 0.084(5) 0.122(7) -0.007(5) 0.025(6) 0.010(4) C31 0.091(10) 0.109(6) 0.203(14) 0.013(9) 0.056(10) 0.008(6) C32 0.050(6) 0.103(6) 0.245(16) -0.012(9) 0.009(10) 0.008(5) C33 0.072(7) 0.127(7) 0.159(10) -0.035(6) -0.029(7) 0.014(5) C34 0.057(6) 0.095(5) 0.098(7) -0.016(5) -0.011(5) 0.010(4) N1 0.048(3) 0.050(2) 0.054(3) 0.010(2) 0.014(3) 0.011(2) N2 0.043(3) 0.050(2) 0.040(3) 0.006(2) 0.008(2) 0.010(2) N3 0.053(3) 0.046(2) 0.065(3) 0.005(3) 0.015(3) 0.001(2) N4 0.057(4) 0.052(3) 0.043(3) 0.001(3) -0.002(3) 0.009(3) N5 0.045(3) 0.047(2) 0.047(3) 0.000(2) -0.004(2) 0.000(2) N6 0.048(3) 0.049(2) 0.049(3) -0.012(2) 0.004(3) -0.005(2) N7 0.054(3) 0.051(3) 0.035(3) -0.004(3) -0.004(3) 0.009(2) N8 0.092(4) 0.057(3) 0.045(3) 0.004(2) 0.021(3) 0.021(3) N9 0.054(3) 0.048(2) 0.038(3) 0.005(2) 0.007(3) 0.008(2) N10 0.060(3) 0.048(2) 0.037(3) 0.002(2) 0.014(2) 0.004(2) P1 0.0435(9) 0.0459(7) 0.0407(9) 0.0029(8) 0.0010(9) 0.0026(7) P2 0.0444(9) 0.0461(8) 0.0518(10) 0.0018(8) 0.0025(9) 0.0028(7) P3 0.0557(11) 0.0509(9) 0.0554(11) 0.0027(8) 0.0090(10) -0.0067(8) P4 0.0586(11) 0.0475(8) 0.0557(12) -0.0020(8) 0.0071(10) 0.0040(8) P5 0.1017(14) 0.0542(9) 0.0462(11) 0.0048(9) 0.0167(11) 0.0099(9) P6 0.0501(10) 0.0435(8) 0.0429(10) -0.0015(8) 0.0008(9) -0.0029(7) Cl1 0.1213(17) 0.1231(15) 0.0607(13) 0.0165(11) 0.0289(12) 0.0261(12) Cl2 0.0757(13) 0.0678(10) 0.191(2) 0.0022(12) -0.0078(14) -0.0263(9) Cl3 0.150(5) 0.084(4) 0.047(4) -0.014(3) -0.032(3) -0.018(8) Cl3' 0.225(13) 0.189(13) 0.066(5) -0.029(8) -0.027(8) 0.139(10) Cl4 0.162(11) 0.060(2) 0.081(4) 0.019(2) 0.063(4) 0.010(3) Cl4' 0.126(19) 0.089(6) 0.17(3) 0.038(9) 0.09(2) 0.013(8) _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 C6 1.369(8) . ? C1 C2 1.372(7) . ? C1 P2 1.793(6) . ? C2 C3 1.363(10) . ? C3 C4 1.358(10) . ? C4 C5 1.396(10) . ? C5 C6 1.371(8) . ? C7 C8 1.360(7) . ? C7 C12 1.393(7) . ? C7 P2 1.804(6) . ? C8 C9 1.387(8) . ? C9 C10 1.349(10) . ? C10 C11 1.334(9) . ? C11 C12 1.408(9) . ? C13 N4 1.479(6) . ? C13 C14 1.497(7) . ? C14 C15 1.503(7) . ? C15 N5 1.466(6) . ? C16 N5 1.476(6) . ? C16 C17 1.531(6) . ? C17 C18 1.520(7) . ? C18 C19 1.541(7) . ? C19 N6 1.484(6) . ? C20 N6 1.469(6) . ? C20 C21 1.524(7) . ? C21 C22 1.512(7) . ? C22 N7 1.461(6) . ? C23 C24 1.366(8) . ? C23 C28 1.368(8) . ? C23 P4 1.801(5) . ? C24 C25 1.404(8) . ? C25 C26 1.350(9) . ? C26 C27 1.365(10) . ? C27 C28 1.397(8) . ? C29 C30 1.374(9) . ? C29 C34 1.371(8) . ? C29 P4 1.788(7) . ? C30 C31 1.386(11) . ? C31 C32 1.326(15) . ? C32 C33 1.397(13) . ? C33 C34 1.385(9) . ? N1 P3 1.565(4) . ? N1 P1 1.602(4) . ? N2 P1 1.599(4) . ? N2 P2 1.607(4) . ? N3 P3 1.573(4) . ? N3 P2 1.599(4) . ? N4 P1 1.640(5) . ? N5 P1 1.642(4) . ? N6 P6 1.655(4) . ? N7 P6 1.643(4) . ? N8 P5 1.559(4) . ? N8 P4 1.612(4) . ? N9 P4 1.592(4) . ? N9 P6 1.593(4) . ? N10 P5 1.561(4) . ? N10 P6 1.618(4) . ? P3 Cl2 2.005(2) . ? P3 Cl1 2.006(2) . ? P5 Cl3' 1.926(19) . ? P5 Cl4 1.965(10) . ? P5 Cl3 2.098(9) . ? P5 Cl4' 2.19(3) . ? Cl3 Cl3' 0.56(6) . ? Cl4 Cl4' 0.88(7) . ? 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 C6 C1 C2 119.0(6) . . ? C6 C1 P2 121.5(5) . . ? C2 C1 P2 119.3(6) . . ? C3 C2 C1 121.1(8) . . ? C4 C3 C2 119.6(8) . . ? C3 C4 C5 120.8(8) . . ? C6 C5 C4 118.2(8) . . ? C1 C6 C5 121.2(7) . . ? C8 C7 C12 117.7(6) . . ? C8 C7 P2 121.6(5) . . ? C12 C7 P2 120.7(5) . . ? C7 C8 C9 122.7(6) . . ? C10 C9 C8 118.9(8) . . ? C11 C10 C9 120.4(8) . . ? C10 C11 C12 121.7(8) . . ? C7 C12 C11 118.4(7) . . ? N4 C13 C14 112.2(4) . . ? C13 C14 C15 112.5(5) . . ? N5 C15 C14 112.5(5) . . ? N5 C16 C17 109.7(4) . . ? C18 C17 C16 112.6(5) . . ? C17 C18 C19 106.9(5) . . ? N6 C19 C18 111.8(5) . . ? N6 C20 C21 111.9(4) . . ? C22 C21 C20 111.3(5) . . ? N7 C22 C21 111.7(4) . . ? C24 C23 C28 118.6(5) . . ? C24 C23 P4 122.7(5) . . ? C28 C23 P4 118.7(5) . . ? C23 C24 C25 119.6(6) . . ? C26 C25 C24 121.0(7) . . ? C25 C26 C27 120.2(6) . . ? C26 C27 C28 118.6(7) . . ? C23 C28 C27 121.9(7) . . ? C30 C29 C34 118.5(7) . . ? C30 C29 P4 120.4(7) . . ? C34 C29 P4 121.0(6) . . ? C29 C30 C31 121.3(9) . . ? C32 C31 C30 119.0(12) . . ? C31 C32 C33 122.3(11) . . ? C34 C33 C32 117.5(9) . . ? C29 C34 C33 121.3(8) . . ? P3 N1 P1 121.8(2) . . ? P1 N2 P2 123.5(2) . . ? P3 N3 P2 120.7(3) . . ? C13 N4 P1 117.7(4) . . ? C15 N5 C16 112.6(4) . . ? C15 N5 P1 120.7(3) . . ? C16 N5 P1 116.9(4) . . ? C20 N6 C19 112.1(4) . . ? C20 N6 P6 119.7(3) . . ? C19 N6 P6 113.5(4) . . ? C22 N7 P6 117.2(4) . . ? P5 N8 P4 120.3(3) . . ? P4 N9 P6 124.7(3) . . ? P5 N10 P6 120.9(2) . . ? N2 P1 N1 115.6(2) . . ? N2 P1 N4 109.6(2) . . ? N1 P1 N4 108.2(2) . . ? N2 P1 N5 109.2(2) . . ? N1 P1 N5 108.8(2) . . ? N4 P1 N5 105.0(2) . . ? N3 P2 N2 116.4(2) . . ? N3 P2 C1 110.1(3) . . ? N2 P2 C1 108.7(3) . . ? N3 P2 C7 106.7(3) . . ? N2 P2 C7 110.4(2) . . ? C1 P2 C7 103.8(3) . . ? N1 P3 N3 120.1(2) . . ? N1 P3 Cl2 110.67(17) . . ? N3 P3 Cl2 108.12(18) . . ? N1 P3 Cl1 108.04(19) . . ? N3 P3 Cl1 108.54(19) . . ? Cl2 P3 Cl1 99.32(12) . . ? N9 P4 N8 116.3(2) . . ? N9 P4 C29 109.6(3) . . ? N8 P4 C29 109.2(3) . . ? N9 P4 C23 109.2(2) . . ? N8 P4 C23 106.6(3) . . ? C29 P4 C23 105.4(3) . . ? N8 P5 N10 121.7(2) . . ? N8 P5 Cl3' 110.3(6) . . ? N10 P5 Cl3' 112.9(7) . . ? N8 P5 Cl4 112.3(7) . . ? N10 P5 Cl4 109.3(3) . . ? Cl3' P5 Cl4 84.1(19) . . ? N8 P5 Cl3 105.0(3) . . ? N10 P5 Cl3 106.7(4) . . ? Cl3' P5 Cl3 15.1(16) . . ? Cl4 P5 Cl3 99.2(8) . . ? N8 P5 Cl4' 97.0(12) . . ? N10 P5 Cl4' 105.9(12) . . ? Cl3' P5 Cl4' 107(3) . . ? Cl4 P5 Cl4' 23.7(16) . . ? Cl3 P5 Cl4' 122(2) . . ? N9 P6 N10 114.8(2) . . ? N9 P6 N7 108.7(2) . . ? N10 P6 N7 109.0(2) . . ? N9 P6 N6 109.6(2) . . ? N10 P6 N6 109.6(2) . . ? N7 P6 N6 104.7(2) . . ? Cl3' Cl3 P5 65(2) . . ? Cl3 Cl3' P5 100(3) . . ? Cl4' Cl4 P5 92.9(17) . . ? Cl4 Cl4' P5 63.4(15) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 0.235 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.047 #===END data_3cb _database_code_CSD 166076 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Cl4 N10 P6' _chemical_formula_weight 918.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 28.970(6) _cell_length_b 13.965(3) _cell_length_c 10.247(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4145.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27502 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\\f and \\w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28171 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8200 _reflns_number_gt 5836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Pearce 1993)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00000(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(5) _refine_ls_number_reflns 8200 _refine_ls_number_parameters 620 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 1.977 _refine_ls_shift/su_mean 0.210 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 N9 N 0.44809(11) 0.0585(2) 0.1438(3) 0.0298(8) Uani 1 1 d . . . H12 H 0.1632(10) 0.116(2) 0.121(3) 0.011(8) Uiso 1 1 d . . . H2 H 0.0391(12) 0.049(2) 0.182(4) 0.016(11) Uiso 1 1 d . . . H10 H 0.1724(11) -0.010(2) -0.230(4) 0.020(9) Uiso 1 1 d . . . H28 H 0.4282(11) -0.133(2) -0.109(3) 0.008(9) Uiso 1 1 d . . . H6 H 0.0661(11) -0.145(2) 0.446(3) 0.010(9) Uiso 1 1 d . . . H27 H 0.4410(15) -0.303(3) -0.089(5) 0.061(14) Uiso 1 1 d . . . H5 H -0.0093(11) -0.166(2) 0.455(3) 0.013(10) Uiso 1 1 d . . . H3 H -0.0386(12) 0.029(2) 0.206(3) 0.019(10) Uiso 1 1 d . . . H14A H 0.2868(13) -0.237(2) 0.619(4) 0.022(10) Uiso 1 1 d . . . H9 H 0.1326(12) -0.133(3) -0.130(4) 0.027(11) Uiso 1 1 d . . . H17A H 0.2750(11) -0.154(2) 0.144(3) 0.023(10) Uiso 1 1 d . . . H18B H 0.2964(13) 0.041(3) 0.119(4) 0.041(13) Uiso 1 1 d . . . H16B H 0.2648(14) 0.014(3) 0.338(4) 0.061(14) Uiso 1 1 d . . . H19A H 0.3345(16) -0.101(3) -0.051(5) 0.062(15) Uiso 1 1 d . . . H16A H 0.2282(15) -0.033(3) 0.239(4) 0.049(14) Uiso 1 1 d . . . H13A H 0.2297(12) -0.144(2) 0.708(4) 0.021(10) Uiso 1 1 d . . . H18A H 0.2657(16) -0.020(3) 0.024(4) 0.052(14) Uiso 1 1 d . . . H32 H 0.6255(15) 0.245(3) -0.068(5) 0.058(14) Uiso 1 1 d . . . H33 H 0.5931(17) 0.232(3) 0.150(5) 0.073(16) Uiso 1 1 d . . . H4 H -0.0644(16) -0.081(3) 0.351(4) 0.054(15) Uiso 1 1 d . . . H11 H 0.1868(13) 0.123(2) -0.091(4) 0.033(11) Uiso 1 1 d . . . H22A H 0.3716(18) 0.118(4) -0.392(6) 0.078(19) Uiso 1 1 d . . . H13B H 0.2115(15) -0.248(3) 0.708(5) 0.053(14) Uiso 1 1 d . . . H25 H 0.5474(14) -0.239(3) 0.132(4) 0.034(13) Uiso 1 1 d . . . H26 H 0.5015(17) -0.352(4) 0.032(5) 0.059(15) Uiso 1 1 d . . . H14B H 0.2514(17) -0.283(3) 0.523(5) 0.058(16) Uiso 1 1 d . . . H34 H 0.5271(18) 0.127(3) 0.171(5) 0.072(17) Uiso 1 1 d . . . H17B H 0.3146(14) -0.094(3) 0.232(4) 0.039(12) Uiso 1 1 d . . . H30 H 0.5241(17) 0.085(3) -0.215(5) 0.063(17) Uiso 1 1 d . . . H22B H 0.3511(14) 0.213(3) -0.398(5) 0.055(13) Uiso 1 1 d . . . H8 H 0.1049(16) -0.132(3) 0.075(5) 0.061(16) Uiso 1 1 d . . . H24 H 0.5407(14) -0.087(3) 0.136(4) 0.051(13) Uiso 1 1 d . . . H19B H 0.3619(18) -0.039(3) 0.056(5) 0.066(16) Uiso 1 1 d . . . P2 P 0.16837(3) 0.10317(7) 0.46671(10) 0.0226(2) Uani 1 1 d . . . P3 P 0.18862(3) -0.09088(6) 0.45875(10) 0.0207(2) Uani 1 1 d . . . P1 P 0.12019(3) -0.01267(6) 0.29533(9) 0.0213(2) Uani 1 1 d . . . P4 P 0.38352(3) 0.10955(7) -0.09736(10) 0.0247(2) Uani 1 1 d . . . Cl1 Cl 0.13958(4) 0.17437(7) 0.61706(9) 0.0355(3) Uani 1 1 d . . . P5 P 0.46657(3) 0.03278(7) -0.00083(10) 0.0260(2) Uani 1 1 d . . . Cl2 Cl 0.21457(4) 0.20439(7) 0.41028(11) 0.0370(3) Uani 1 1 d . . . Cl3 Cl 0.44058(4) 0.26151(8) 0.22480(11) 0.0463(3) Uani 1 1 d . . . P6 P 0.41152(4) 0.13988(7) 0.15865(10) 0.0293(3) Uani 1 1 d . . . Cl4 Cl 0.37154(4) 0.10765(8) 0.31355(10) 0.0455(3) Uani 1 1 d . . . N3 N 0.14732(10) -0.10139(19) 0.3591(3) 0.0194(7) Uani 1 1 d . . . N2 N 0.19536(10) 0.0149(2) 0.5195(3) 0.0244(8) Uani 1 1 d . . . N1 N 0.13183(10) 0.09213(19) 0.3555(3) 0.0227(7) Uani 1 1 d . . . N10 N 0.37986(12) 0.1670(2) 0.0395(3) 0.0299(8) Uani 1 1 d . . . C13 C 0.22153(15) -0.1925(4) 0.6558(4) 0.0327(10) Uani 1 1 d . . . N6 N 0.33885(10) 0.0375(2) -0.1091(3) 0.0301(8) Uani 1 1 d . . . C29 C 0.51989(13) 0.0971(3) -0.0186(4) 0.0298(10) Uani 1 1 d . . . C2 C 0.02708(15) 0.0155(3) 0.2389(5) 0.0341(11) Uani 1 1 d . . . C24 C 0.51752(16) -0.1250(3) 0.0745(4) 0.0389(11) Uani 1 1 d . . . C7 C 0.13334(12) -0.0068(2) 0.1244(4) 0.0205(8) Uani 1 1 d . . . C6 C 0.04453(14) -0.1078(3) 0.3917(4) 0.0290(9) Uani 1 1 d . . . C10 C 0.16114(14) -0.0109(3) -0.1357(4) 0.0318(10) Uani 1 1 d . . . C16 C 0.25273(16) -0.0533(3) 0.2862(5) 0.0327(10) Uani 1 1 d . . . C23 C 0.48050(13) -0.0921(3) 0.0000(4) 0.0277(9) Uani 1 1 d . . . C26 C 0.49765(18) -0.2869(3) 0.0219(5) 0.0416(12) Uani 1 1 d . . . N8 N 0.43092(11) 0.0531(2) -0.1145(3) 0.0279(8) Uani 1 1 d . . . N5 N 0.23787(10) -0.1228(2) 0.3848(3) 0.0238(7) Uani 1 1 d . . . C8 C 0.12382(16) -0.0855(3) 0.0444(4) 0.0355(11) Uani 1 1 d . . . C28 C 0.45274(15) -0.1581(3) -0.0626(4) 0.0297(10) Uani 1 1 d . . . C1 C 0.05953(12) -0.0372(2) 0.3083(4) 0.0231(8) Uani 1 1 d . . . C27 C 0.46143(16) -0.2557(3) -0.0532(5) 0.0379(11) Uani 1 1 d . . . N7 N 0.37530(11) 0.1881(2) -0.2138(3) 0.0311(8) Uani 1 1 d . . . H7N H 0.3836 0.2466 -0.2028 0.037 Uiso 1 1 calc R . . N4 N 0.18161(11) -0.1661(2) 0.5771(3) 0.0265(8) Uani 1 1 d . . . H4N H 0.1549 -0.1901 0.5933 0.032 Uiso 1 1 calc R . . C5 C -0.00206(15) -0.1257(3) 0.4050(5) 0.0366(11) Uani 1 1 d . . . C30 C 0.53973(17) 0.1060(3) -0.1400(5) 0.0418(12) Uani 1 1 d . . . C19 C 0.33415(15) -0.0372(3) -0.0087(4) 0.0331(10) Uani 1 1 d . . . C12 C 0.15632(15) 0.0695(3) 0.0697(4) 0.0301(10) Uani 1 1 d . . . C3 C -0.01909(15) -0.0037(3) 0.2518(5) 0.0395(12) Uani 1 1 d . . . C18 C 0.29244(16) -0.0201(3) 0.0791(5) 0.0327(10) Uani 1 1 d . . . C11 C 0.17018(15) 0.0674(3) -0.0595(4) 0.0348(11) Uani 1 1 d . . . C17 C 0.28648(16) -0.0912(3) 0.1869(4) 0.0326(10) Uani 1 1 d . . . C15 C 0.27565(14) -0.1523(3) 0.4736(4) 0.0407(11) Uani 1 1 d . . . H15A H 0.2869 -0.0964 0.5200 0.049 Uiso 1 1 calc R . . H15B H 0.3010 -0.1776 0.4222 0.049 Uiso 1 1 calc R . . C25 C 0.52487(18) -0.2231(3) 0.0849(5) 0.0432(12) Uani 1 1 d . . . C22 C 0.3541(2) 0.1590(4) -0.3345(5) 0.0512(14) Uani 1 1 d . . . C9 C 0.13793(17) -0.0867(3) -0.0830(4) 0.0406(12) Uani 1 1 d . . . C20 C 0.31401(17) 0.0207(4) -0.2297(4) 0.0549(14) Uani 1 1 d . . . H20A H 0.2835 -0.0035 -0.2091 0.066 Uiso 1 1 calc R . . H20B H 0.3300 -0.0284 -0.2792 0.066 Uiso 1 1 calc R . . C14 C 0.26084(17) -0.2263(4) 0.5708(5) 0.0420(12) Uani 1 1 d . . . C4 C -0.03334(16) -0.0739(3) 0.3357(4) 0.0378(11) Uani 1 1 d . . . C21 C 0.30926(18) 0.1080(4) -0.3126(5) 0.0625(16) Uani 1 1 d . . . H21A H 0.2877 0.1517 -0.2713 0.075 Uiso 1 1 calc R . . H21B H 0.2964 0.0898 -0.3965 0.075 Uiso 1 1 calc R . . C34 C 0.54122(17) 0.1384(4) 0.0874(5) 0.0471(13) Uani 1 1 d . . . C32 C 0.59904(16) 0.2024(4) -0.0518(6) 0.0524(14) Uani 1 1 d . . . C31 C 0.57968(16) 0.1612(3) -0.1555(5) 0.0481(13) Uani 1 1 d . . . H31 H 0.5927 0.1690 -0.2378 0.058 Uiso 1 1 calc R . . C33 C 0.58127(18) 0.1919(4) 0.0711(6) 0.0551(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N9 0.034(2) 0.0282(17) 0.0267(18) 0.0023(16) -0.0030(15) 0.0074(15) P2 0.0274(6) 0.0192(5) 0.0214(5) -0.0006(4) 0.0017(5) -0.0004(4) P3 0.0195(5) 0.0217(5) 0.0208(5) 0.0021(4) 0.0010(4) 0.0004(4) P1 0.0232(5) 0.0202(5) 0.0206(5) 0.0009(4) -0.0011(4) 0.0010(4) P4 0.0271(6) 0.0255(5) 0.0217(5) 0.0012(5) -0.0016(5) -0.0006(5) Cl1 0.0452(7) 0.0370(6) 0.0242(5) -0.0055(5) 0.0036(5) 0.0091(5) P5 0.0266(6) 0.0266(5) 0.0247(5) 0.0000(5) 0.0014(5) 0.0002(5) Cl2 0.0426(6) 0.0280(5) 0.0404(6) 0.0044(5) 0.0039(5) -0.0103(5) Cl3 0.0573(8) 0.0352(6) 0.0464(7) -0.0133(5) -0.0128(6) 0.0000(6) P6 0.0355(6) 0.0309(6) 0.0216(5) -0.0012(5) -0.0013(5) 0.0024(5) Cl4 0.0507(7) 0.0601(7) 0.0258(6) 0.0000(6) 0.0087(5) 0.0066(6) N3 0.0175(17) 0.0176(16) 0.0232(17) 0.0021(13) -0.0002(13) 0.0008(13) N2 0.0228(18) 0.0230(17) 0.0275(18) -0.0018(14) -0.0009(14) -0.0015(14) N1 0.0274(18) 0.0204(16) 0.0205(16) 0.0013(14) -0.0026(13) 0.0023(14) N10 0.035(2) 0.0294(18) 0.0257(17) -0.0051(15) -0.0023(15) 0.0079(16) C13 0.032(3) 0.039(3) 0.027(2) 0.001(2) -0.007(2) 0.003(2) N6 0.0254(19) 0.0347(19) 0.0301(18) 0.0039(17) 0.0006(16) -0.0082(15) C29 0.026(2) 0.024(2) 0.040(3) 0.0021(19) -0.003(2) 0.0036(17) C2 0.030(3) 0.032(3) 0.040(3) 0.004(2) 0.001(2) 0.005(2) C24 0.037(3) 0.035(3) 0.045(3) -0.006(2) -0.004(2) 0.009(2) C7 0.020(2) 0.0200(18) 0.022(2) -0.0012(17) -0.0042(16) 0.0005(16) C6 0.022(2) 0.032(2) 0.033(2) 0.005(2) -0.001(2) 0.0030(19) C10 0.032(3) 0.039(3) 0.024(2) 0.001(2) -0.001(2) 0.010(2) C16 0.025(2) 0.034(3) 0.039(3) 0.008(2) 0.007(2) 0.004(2) C23 0.029(2) 0.028(2) 0.026(2) 0.0017(19) 0.0052(18) 0.0006(19) C26 0.050(3) 0.025(2) 0.050(3) 0.005(2) 0.017(2) 0.008(2) N8 0.029(2) 0.0303(18) 0.0248(17) 0.0025(15) -0.0002(15) 0.0059(15) N5 0.0192(18) 0.0282(17) 0.0239(17) 0.0039(15) 0.0025(14) 0.0025(14) C8 0.046(3) 0.030(2) 0.031(2) 0.000(2) 0.003(2) -0.004(2) C28 0.027(2) 0.030(2) 0.032(2) -0.001(2) 0.002(2) 0.002(2) C1 0.023(2) 0.023(2) 0.024(2) -0.0040(18) -0.0010(18) 0.0040(17) C27 0.042(3) 0.030(2) 0.042(3) -0.003(2) 0.017(2) -0.007(2) N7 0.045(2) 0.0221(18) 0.0268(19) 0.0037(15) -0.0075(16) -0.0057(15) N4 0.0189(18) 0.0338(19) 0.0267(19) 0.0099(16) 0.0007(14) -0.0017(15) C5 0.034(3) 0.042(3) 0.034(2) 0.005(2) 0.005(2) -0.005(2) C30 0.039(3) 0.036(3) 0.050(3) -0.009(2) 0.018(3) -0.001(2) C19 0.036(3) 0.028(2) 0.036(3) 0.004(2) 0.005(2) -0.001(2) C12 0.039(3) 0.025(2) 0.026(2) -0.007(2) 0.000(2) -0.004(2) C3 0.025(3) 0.033(3) 0.061(3) -0.005(2) -0.019(2) 0.010(2) C18 0.025(3) 0.036(3) 0.037(3) 0.000(2) 0.006(2) 0.002(2) C11 0.038(3) 0.040(3) 0.026(3) 0.006(2) 0.001(2) -0.006(2) C17 0.030(3) 0.035(3) 0.033(2) 0.001(2) 0.010(2) 0.002(2) C15 0.023(2) 0.053(3) 0.046(3) 0.006(2) 0.001(2) 0.012(2) C25 0.044(3) 0.039(3) 0.047(3) 0.003(2) -0.007(2) 0.018(3) C22 0.081(4) 0.045(3) 0.028(2) 0.007(3) -0.012(3) -0.011(3) C9 0.055(3) 0.039(3) 0.027(3) -0.012(2) -0.004(2) -0.004(2) C20 0.068(4) 0.061(3) 0.036(3) 0.002(3) -0.017(2) -0.034(3) C14 0.030(3) 0.057(3) 0.040(3) 0.012(3) -0.003(2) 0.020(3) C4 0.022(3) 0.039(3) 0.052(3) -0.007(2) 0.006(2) -0.002(2) C21 0.062(4) 0.078(4) 0.047(3) 0.011(3) -0.029(3) -0.022(3) C34 0.036(3) 0.061(3) 0.045(3) 0.002(3) -0.005(2) -0.010(3) C32 0.022(3) 0.042(3) 0.093(5) 0.000(3) 0.009(3) -0.003(2) C31 0.041(3) 0.042(3) 0.062(3) -0.011(3) 0.020(3) -0.010(2) C33 0.037(3) 0.063(3) 0.066(4) 0.004(3) -0.012(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N9 P6 1.561(3) . ? N9 P5 1.616(3) . ? P2 N2 1.557(3) . ? P2 N1 1.563(3) . ? P2 Cl1 2.0144(14) . ? P2 Cl2 2.0308(13) . ? P3 N3 1.580(3) . ? P3 N2 1.615(3) . ? P3 N4 1.618(3) . ? P3 N5 1.676(3) . ? P1 N3 1.606(3) . ? P1 N1 1.624(3) . ? P1 C7 1.795(4) . ? P1 C1 1.795(4) . ? P4 N8 1.593(3) . ? P4 N10 1.620(3) . ? P4 N7 1.638(3) . ? P4 N6 1.644(3) . ? P5 N8 1.582(3) . ? P5 C23 1.791(4) . ? P5 C29 1.796(4) . ? Cl3 P6 2.0133(15) . ? P6 N10 1.573(3) . ? P6 Cl4 2.0159(15) . ? C13 N4 1.457(5) . ? C13 C14 1.509(6) . ? N6 C20 1.450(5) . ? N6 C19 1.471(5) . ? C29 C34 1.376(6) . ? C29 C30 1.376(6) . ? C2 C3 1.370(6) . ? C2 C1 1.390(5) . ? C24 C25 1.391(6) . ? C24 C23 1.394(6) . ? C7 C12 1.376(5) . ? C7 C8 1.397(5) . ? C6 C1 1.376(5) . ? C6 C5 1.379(6) . ? C10 C9 1.365(6) . ? C10 C11 1.369(6) . ? C16 N5 1.465(5) . ? C16 C17 1.508(6) . ? C23 C28 1.381(5) . ? C26 C25 1.354(7) . ? C26 C27 1.372(7) . ? N5 C15 1.482(5) . ? C8 C9 1.369(6) . ? C28 C27 1.388(6) . ? N7 C22 1.440(6) . ? C5 C4 1.359(6) . ? C30 C31 1.399(6) . ? C19 C18 1.525(6) . ? C12 C11 1.384(5) . ? C3 C4 1.368(6) . ? C18 C17 1.496(6) . ? C15 C14 1.498(6) . ? C22 C21 1.498(7) . ? C20 C21 1.493(6) . ? C34 C33 1.390(7) . ? C32 C31 1.332(7) . ? C32 C33 1.369(7) . ? 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 P6 N9 P5 118.42(19) . . ? N2 P2 N1 121.03(16) . . ? N2 P2 Cl1 109.45(13) . . ? N1 P2 Cl1 109.02(12) . . ? N2 P2 Cl2 108.61(13) . . ? N1 P2 Cl2 107.91(12) . . ? Cl1 P2 Cl2 98.46(6) . . ? N3 P3 N2 115.19(15) . . ? N3 P3 N4 109.23(16) . . ? N2 P3 N4 108.69(16) . . ? N3 P3 N5 109.12(16) . . ? N2 P3 N5 108.35(16) . . ? N4 P3 N5 105.85(15) . . ? N3 P1 N1 116.06(15) . . ? N3 P1 C7 109.16(16) . . ? N1 P1 C7 106.61(16) . . ? N3 P1 C1 107.57(16) . . ? N1 P1 C1 110.30(16) . . ? C7 P1 C1 106.77(17) . . ? N8 P4 N10 113.41(17) . . ? N8 P4 N7 112.11(17) . . ? N10 P4 N7 106.84(16) . . ? N8 P4 N6 111.57(17) . . ? N10 P4 N6 108.35(17) . . ? N7 P4 N6 104.01(17) . . ? N8 P5 N9 114.78(17) . . ? N8 P5 C23 108.97(18) . . ? N9 P5 C23 106.67(17) . . ? N8 P5 C29 113.40(18) . . ? N9 P5 C29 105.46(18) . . ? C23 P5 C29 107.10(18) . . ? N9 P6 N10 119.70(17) . . ? N9 P6 Cl3 111.29(14) . . ? N10 P6 Cl3 107.58(13) . . ? N9 P6 Cl4 107.71(13) . . ? N10 P6 Cl4 109.25(14) . . ? Cl3 P6 Cl4 99.41(7) . . ? P3 N3 P1 124.18(18) . . ? P2 N2 P3 122.0(2) . . ? P2 N1 P1 120.44(18) . . ? P6 N10 P4 121.0(2) . . ? N4 C13 C14 111.0(4) . . ? C20 N6 C19 115.8(3) . . ? C20 N6 P4 123.5(3) . . ? C19 N6 P4 117.1(3) . . ? C34 C29 C30 119.2(4) . . ? C34 C29 P5 121.0(3) . . ? C30 C29 P5 119.7(3) . . ? C3 C2 C1 120.5(4) . . ? C25 C24 C23 119.0(5) . . ? C12 C7 C8 117.7(4) . . ? C12 C7 P1 122.4(3) . . ? C8 C7 P1 119.6(3) . . ? C1 C6 C5 120.0(4) . . ? C9 C10 C11 119.2(4) . . ? N5 C16 C17 115.1(3) . . ? C28 C23 C24 118.8(4) . . ? C28 C23 P5 121.1(3) . . ? C24 C23 P5 119.8(3) . . ? C25 C26 C27 120.2(4) . . ? P5 N8 P4 124.7(2) . . ? C16 N5 C15 113.0(3) . . ? C16 N5 P3 112.7(2) . . ? C15 N5 P3 115.1(3) . . ? C9 C8 C7 120.7(4) . . ? C23 C28 C27 121.1(4) . . ? C6 C1 C2 119.0(4) . . ? C6 C1 P1 119.5(3) . . ? C2 C1 P1 121.6(3) . . ? C26 C27 C28 119.3(4) . . ? C22 N7 P4 119.9(3) . . ? C13 N4 P3 118.7(3) . . ? C4 C5 C6 120.3(5) . . ? C29 C30 C31 119.8(5) . . ? N6 C19 C18 112.0(3) . . ? C7 C12 C11 120.9(4) . . ? C4 C3 C2 119.7(5) . . ? C17 C18 C19 115.0(4) . . ? C10 C11 C12 120.4(4) . . ? C18 C17 C16 109.9(4) . . ? N5 C15 C14 112.8(4) . . ? C26 C25 C24 121.5(5) . . ? N7 C22 C21 112.1(4) . . ? C10 C9 C8 121.0(4) . . ? N6 C20 C21 113.5(4) . . ? C15 C14 C13 112.6(4) . . ? C5 C4 C3 120.6(4) . . ? C20 C21 C22 113.2(4) . . ? C29 C34 C33 120.3(5) . . ? C31 C32 C33 121.9(5) . . ? C32 C31 C30 119.8(5) . . ? C32 C33 C34 118.8(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.345 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.079 #===END