# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1575 data_jv30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H62.50 Cl4 N2 O10.25 P4' _chemical_formula_weight 856.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3054(4) _cell_length_b 11.5193(4) _cell_length_c 17.8036(7) _cell_angle_alpha 101.135(2) _cell_angle_beta 92.151(2) _cell_angle_gamma 113.594(2) _cell_volume 2067.68(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 909 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8275 _exptl_absorpt_correction_T_max 0.9758 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 17094 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8667 _reflns_number_gt 6824 _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^)+(0.0300P)^2^+1.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8667 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _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 Cl1 Cl 0.55218(5) 0.29409(5) 0.28762(3) 0.02947(12) Uani 1 d . . . Cl2 Cl 0.43386(6) 0.33290(6) 0.15146(3) 0.03923(15) Uani 1 d . . . Cl3 Cl 0.03933(5) -0.00572(5) 0.41734(3) 0.02485(11) Uani 1 d . . . Cl4 Cl 0.08618(5) -0.21762(5) 0.32548(3) 0.03031(13) Uani 1 d . . . P1 P 0.34565(5) 0.07096(5) 0.17974(3) 0.02245(12) Uani 1 d . . . P2 P 0.29009(5) 0.28984(5) 0.28511(3) 0.02126(12) Uani 1 d . . . P3 P 0.26524(5) 0.04961(5) 0.33685(3) 0.01683(11) Uani 1 d . . . P4 P -0.03161(5) -0.07737(5) 0.24969(3) 0.02335(12) Uani 1 d . . . O11 O 0.45232(15) 0.04208(16) 0.14982(9) 0.0326(4) Uani 1 d . . . O12 O 0.22046(14) 0.02800(15) 0.12957(8) 0.0287(3) Uani 1 d . . . O13 O 0.30873(13) 0.01008(13) 0.25684(8) 0.0210(3) Uani 1 d . . . O21 O 0.16495(14) 0.24332(14) 0.23396(9) 0.0273(3) Uani 1 d . . . O22 O 0.35285(15) 0.42218(14) 0.33255(9) 0.0313(4) Uani 1 d . . . O23 O 0.26660(13) 0.18763(12) 0.34227(8) 0.0197(3) Uani 1 d . . . O33 O 0.34119(14) 0.04169(14) 0.40203(8) 0.0254(3) Uani 1 d . . . O41 O -0.15858(14) -0.17349(15) 0.26007(9) 0.0300(3) Uani 1 d . . . O42 O -0.02671(15) 0.05993(15) 0.25737(10) 0.0321(4) Uani 1 d . . . O43 O 0.01967(16) -0.11911(17) 0.17463(9) 0.0360(4) Uani 1 d . . . C1 C 0.4041(2) 0.2459(2) 0.22643(12) 0.0231(4) Uani 1 d . . . C2 C 0.09128(19) -0.05972(18) 0.32885(11) 0.0192(4) Uani 1 d . . . N1 N 0.44674(15) 0.21010(15) 0.60700(9) 0.0188(3) Uani 1 d . . . N2 N 0.21576(16) -0.16781(16) -0.08794(9) 0.0190(3) Uani 1 d . . . C11 C 0.5477(2) 0.2653(2) 0.55560(12) 0.0238(4) Uani 1 d . . . H11A H 0.5784 0.3601 0.5669 0.036 Uiso 1 calc R . . H11B H 0.5093 0.2288 0.5015 0.036 Uiso 1 calc R . . H11C H 0.6211 0.2429 0.5650 0.036 Uiso 1 calc R . . C121 C 0.49525(19) 0.28317(19) 0.69037(11) 0.0206(4) Uani 1 d . . . H12A H 0.4236 0.2512 0.7218 0.025 Uiso 1 calc R . . H12B H 0.5175 0.3765 0.6937 0.025 Uiso 1 calc R . . C122 C 0.6131(2) 0.2705(2) 0.72521(12) 0.0267(5) Uani 1 d . . . H12C H 0.5863 0.1827 0.7356 0.032 Uiso 1 calc R . . H12D H 0.6778 0.2814 0.6881 0.032 Uiso 1 calc R . . C123 C 0.6746(2) 0.3727(2) 0.79994(12) 0.0268(5) Uani 1 d . . . H12E H 0.6055 0.3734 0.8323 0.032 Uiso 1 calc R . . H12F H 0.7161 0.4594 0.7878 0.032 Uiso 1 calc R . . C124 C 0.7760(3) 0.3491(3) 0.84548(15) 0.0424(6) Uani 1 d . . . H12G H 0.7358 0.2630 0.8573 0.064 Uiso 1 calc R . . H12H H 0.8103 0.4159 0.8937 0.064 Uiso 1 calc R . . H12I H 0.8471 0.3530 0.8148 0.064 Uiso 1 calc R . . C131 C 0.4181(2) 0.06658(18) 0.59583(12) 0.0209(4) Uani 1 d . . . H13A H 0.3821 0.0230 0.5413 0.025 Uiso 1 calc R . . H13B H 0.5012 0.0590 0.6056 0.025 Uiso 1 calc R . . C132 C 0.3240(2) -0.00547(19) 0.64693(12) 0.0250(4) Uani 1 d . . . H13C H 0.2508 0.0212 0.6496 0.030 Uiso 1 calc R . . H13D H 0.3690 0.0165 0.6999 0.030 Uiso 1 calc R . . C133 C 0.2716(2) -0.15292(19) 0.61349(13) 0.0264(5) Uani 1 d . . . H13E H 0.3452 -0.1750 0.5993 0.032 Uiso 1 calc R . . H13F H 0.2323 -0.1993 0.6538 0.032 Uiso 1 calc R . . C134 C 0.1704(2) -0.2003(2) 0.54279(15) 0.0360(6) Uani 1 d . . . H13A H 0.0941 -0.1852 0.5573 0.054 Uiso 1 calc R . . H13B H 0.1444 -0.2936 0.5223 0.054 Uiso 1 calc R . . H13C H 0.2076 -0.1527 0.5032 0.054 Uiso 1 calc R . . C141 C 0.32197(19) 0.22139(19) 0.58195(12) 0.0212(4) Uani 1 d . . . H14A H 0.2647 0.2042 0.6229 0.025 Uiso 1 calc R . . H14B H 0.2764 0.1526 0.5349 0.025 Uiso 1 calc R . . C142 C 0.3403(2) 0.35226(19) 0.56538(12) 0.0233(4) Uani 1 d . . . H14C H 0.3985 0.4238 0.6082 0.028 Uiso 1 calc R . . H14D H 0.3807 0.3629 0.5173 0.028 Uiso 1 calc R . . C143 C 0.2080(2) 0.3573(2) 0.55672(13) 0.0276(5) Uani 1 d . . . H14E H 0.1745 0.3599 0.6073 0.033 Uiso 1 calc R . . H14F H 0.1461 0.2772 0.5202 0.033 Uiso 1 calc R . . C144 C 0.2146(2) 0.4757(2) 0.52739(14) 0.0303(5) Uani 1 d . . . H14A H 0.2783 0.5552 0.5622 0.045 Uiso 1 calc R . . H14B H 0.1288 0.4780 0.5257 0.045 Uiso 1 calc R . . H14C H 0.2408 0.4699 0.4754 0.045 Uiso 1 calc R . . C21 C 0.3173(2) -0.1607(2) -0.02841(12) 0.0241(4) Uani 1 d . . . H21A H 0.3293 -0.0916 0.0169 0.036 Uiso 1 calc R . . H21B H 0.3997 -0.1418 -0.0500 0.036 Uiso 1 calc R . . H21C H 0.2893 -0.2441 -0.0132 0.036 Uiso 1 calc R . . C221 C 0.09266(19) -0.17695(19) -0.05265(12) 0.0212(4) Uani 1 d . . . H22A H 0.1134 -0.0958 -0.0132 0.025 Uiso 1 calc R . . H22B H 0.0276 -0.1825 -0.0935 0.025 Uiso 1 calc R . . C222 C 0.0320(2) -0.2917(2) -0.01544(13) 0.0255(4) Uani 1 d . . . H22C H 0.0887 -0.2781 0.0321 0.031 Uiso 1 calc R . . H22D H 0.0255 -0.3719 -0.0513 0.031 Uiso 1 calc R . . C223 C -0.1033(2) -0.3089(2) 0.00471(13) 0.0264(5) Uani 1 d . . . H22E H -0.0995 -0.2245 0.0333 0.032 Uiso 1 calc R . . H22F H -0.1641 -0.3373 -0.0434 0.032 Uiso 1 calc R . . C224 C -0.1540(2) -0.4091(2) 0.05380(14) 0.0349(5) Uani 1 d . . . H22G H -0.1622 -0.4938 0.0245 0.052 Uiso 1 calc R . . H22H H -0.2394 -0.4159 0.0675 0.052 Uiso 1 calc R . . H22I H -0.0931 -0.3819 0.1010 0.052 Uiso 1 calc R . . C231 C 0.19059(19) -0.28643(19) -0.15252(11) 0.0210(4) Uani 1 d . . . H23A H 0.2718 -0.2720 -0.1761 0.025 Uiso 1 calc R . . H23B H 0.1702 -0.3628 -0.1294 0.025 Uiso 1 calc R . . C232 C 0.0820(2) -0.31882(19) -0.21589(11) 0.0221(4) Uani 1 d . . . H23C H 0.1002 -0.2431 -0.2393 0.027 Uiso 1 calc R . . H23D H -0.0010 -0.3380 -0.1938 0.027 Uiso 1 calc R . . C233 C 0.0696(2) -0.43638(19) -0.27802(12) 0.0252(4) Uani 1 d . . . H23E H 0.1527 -0.4168 -0.3001 0.030 Uiso 1 calc R . . H23F H 0.0523 -0.5117 -0.2543 0.030 Uiso 1 calc R . . C234 C -0.0394(2) -0.4714(2) -0.34205(13) 0.0298(5) Uani 1 d . . . H23G H -0.1220 -0.4921 -0.3205 0.045 Uiso 1 calc R . . H23H H -0.0450 -0.5470 -0.3808 0.045 Uiso 1 calc R . . H23I H -0.0217 -0.3975 -0.3662 0.045 Uiso 1 calc R . . C241 C 0.2678(2) -0.04692(19) -0.12127(12) 0.0210(4) Uani 1 d . . . H24A H 0.3364 -0.0515 -0.1531 0.025 Uiso 1 calc R . . H24B H 0.1963 -0.0488 -0.1560 0.025 Uiso 1 calc R . . C242 C 0.3238(2) 0.0825(2) -0.06250(12) 0.0253(4) Uani 1 d . . . H24C H 0.2552 0.0917 -0.0322 0.030 Uiso 1 calc R . . H24D H 0.3946 0.0858 -0.0265 0.030 Uiso 1 calc R . . C243 C 0.3766(2) 0.1930(2) -0.10381(13) 0.0317(5) Uani 1 d . . . H24E H 0.3039 0.1927 -0.1368 0.038 Uiso 1 calc R . . H24F H 0.4391 0.1785 -0.1378 0.038 Uiso 1 calc R . . C244 C 0.4442(2) 0.3252(2) -0.04805(14) 0.0312(5) Uani 1 d . . . H24G H 0.3845 0.3377 -0.0121 0.047 Uiso 1 calc R . . H24H H 0.4698 0.3937 -0.0771 0.047 Uiso 1 calc R . . H24I H 0.5217 0.3294 -0.0191 0.047 Uiso 1 calc R . . H43 H 0.094(3) -0.060(3) 0.1597(16) 0.050 Uiso 1 d . . . H42 H 0.048(3) 0.124(3) 0.2479(17) 0.050 Uiso 1 d . . . O1 O 0.7281(7) 0.5593(6) 0.2158(5) 0.0433(18) Uani 0.25 d P . . 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 Cl1 0.0175(2) 0.0365(3) 0.0287(3) 0.0031(2) 0.0009(2) 0.0076(2) Cl2 0.0411(3) 0.0454(3) 0.0355(3) 0.0251(3) 0.0130(3) 0.0145(3) Cl3 0.0239(2) 0.0280(3) 0.0204(2) 0.0033(2) 0.0072(2) 0.0090(2) Cl4 0.0315(3) 0.0174(2) 0.0442(3) 0.0089(2) 0.0083(2) 0.0113(2) P1 0.0220(3) 0.0276(3) 0.0164(3) 0.0023(2) 0.0050(2) 0.0100(2) P2 0.0196(2) 0.0168(2) 0.0280(3) 0.0068(2) 0.0048(2) 0.0073(2) P3 0.0172(2) 0.0176(2) 0.0162(2) 0.00375(19) 0.00210(19) 0.0080(2) P4 0.0176(2) 0.0247(3) 0.0229(3) 0.0033(2) -0.0008(2) 0.0051(2) O11 0.0281(8) 0.0391(9) 0.0292(8) 0.0013(7) 0.0119(7) 0.0147(7) O12 0.0248(7) 0.0374(8) 0.0168(7) 0.0027(6) 0.0010(6) 0.0073(7) O13 0.0226(7) 0.0213(7) 0.0204(7) 0.0035(6) 0.0051(6) 0.0107(6) O21 0.0225(7) 0.0289(8) 0.0345(9) 0.0118(7) 0.0015(6) 0.0129(7) O22 0.0313(8) 0.0166(7) 0.0425(9) 0.0049(7) 0.0091(7) 0.0069(7) O23 0.0209(7) 0.0172(6) 0.0205(7) 0.0034(6) 0.0053(6) 0.0075(6) O33 0.0231(7) 0.0328(8) 0.0231(8) 0.0093(6) 0.0005(6) 0.0132(7) O41 0.0186(7) 0.0285(8) 0.0336(9) 0.0039(7) 0.0019(6) 0.0020(6) O42 0.0202(8) 0.0294(8) 0.0473(10) 0.0161(8) -0.0016(7) 0.0081(7) O43 0.0265(8) 0.0419(9) 0.0206(8) -0.0029(7) 0.0017(7) -0.0003(8) C1 0.0199(10) 0.0276(10) 0.0213(10) 0.0081(9) 0.0029(8) 0.0082(9) C2 0.0207(9) 0.0177(9) 0.0203(10) 0.0029(8) 0.0045(8) 0.0094(8) N1 0.0165(8) 0.0174(8) 0.0213(9) 0.0045(7) 0.0045(7) 0.0056(7) N2 0.0181(8) 0.0203(8) 0.0189(8) 0.0037(7) 0.0008(7) 0.0089(7) C11 0.0191(10) 0.0254(10) 0.0242(11) 0.0071(9) 0.0077(8) 0.0055(9) C121 0.0213(10) 0.0171(9) 0.0209(10) 0.0020(8) 0.0023(8) 0.0066(8) C122 0.0264(11) 0.0274(11) 0.0258(11) 0.0012(9) -0.0011(9) 0.0132(9) C123 0.0273(11) 0.0252(10) 0.0244(11) 0.0032(9) 0.0016(9) 0.0086(9) C124 0.0477(15) 0.0479(15) 0.0280(13) -0.0041(11) -0.0110(11) 0.0235(13) C131 0.0227(10) 0.0145(9) 0.0245(10) 0.0023(8) 0.0041(8) 0.0075(8) C132 0.0285(11) 0.0197(10) 0.0265(11) 0.0066(9) 0.0067(9) 0.0088(9) C133 0.0294(11) 0.0178(9) 0.0335(12) 0.0084(9) 0.0045(9) 0.0101(9) C134 0.0322(12) 0.0193(10) 0.0492(15) 0.0045(10) -0.0052(11) 0.0057(10) C141 0.0164(9) 0.0202(9) 0.0259(11) 0.0050(8) 0.0006(8) 0.0069(8) C142 0.0212(10) 0.0188(9) 0.0266(11) 0.0069(8) 0.0004(8) 0.0045(8) C143 0.0252(11) 0.0242(10) 0.0356(12) 0.0107(9) 0.0044(9) 0.0106(9) C144 0.0326(12) 0.0269(11) 0.0343(12) 0.0100(10) 0.0012(10) 0.0143(10) C21 0.0206(10) 0.0313(11) 0.0219(10) 0.0067(9) -0.0011(8) 0.0123(9) C221 0.0182(9) 0.0238(10) 0.0229(10) 0.0036(8) 0.0046(8) 0.0106(8) C222 0.0220(10) 0.0255(10) 0.0287(11) 0.0068(9) 0.0047(9) 0.0093(9) C223 0.0216(10) 0.0269(11) 0.0292(11) 0.0057(9) 0.0039(9) 0.0088(9) C224 0.0321(12) 0.0331(12) 0.0377(13) 0.0093(11) 0.0107(11) 0.0107(11) C231 0.0228(10) 0.0228(10) 0.0198(10) 0.0020(8) 0.0013(8) 0.0134(9) C232 0.0226(10) 0.0216(10) 0.0203(10) 0.0010(8) -0.0017(8) 0.0093(9) C233 0.0285(11) 0.0197(10) 0.0254(11) 0.0022(9) 0.0008(9) 0.0093(9) C234 0.0323(12) 0.0263(11) 0.0250(11) -0.0006(9) -0.0026(9) 0.0095(10) C241 0.0196(9) 0.0209(9) 0.0220(10) 0.0070(8) 0.0021(8) 0.0069(8) C242 0.0251(10) 0.0243(10) 0.0223(10) 0.0047(9) 0.0012(9) 0.0063(9) C243 0.0381(13) 0.0261(11) 0.0262(11) 0.0081(9) 0.0034(10) 0.0078(10) C244 0.0345(12) 0.0241(11) 0.0331(12) 0.0064(9) 0.0080(10) 0.0101(10) O1 0.038(4) 0.016(3) 0.066(5) 0.008(3) 0.017(4) 0.001(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 Cl1 C1 1.784(2) . ? Cl2 C1 1.783(2) . ? Cl3 C2 1.7881(19) . ? Cl4 C2 1.7858(19) . ? P1 O11 1.4661(15) . ? P1 O12 1.4898(16) . ? P1 O13 1.6525(14) . ? P1 C1 1.854(2) . ? P2 O22 1.4603(15) . ? P2 O21 1.4920(15) . ? P2 O23 1.6507(14) . ? P2 C1 1.852(2) . ? P3 O33 1.4564(15) . ? P3 O23 1.5679(14) . ? P3 O13 1.5683(14) . ? P3 C2 1.844(2) . ? P4 O41 1.4653(15) . ? P4 O42 1.5393(16) . ? P4 O43 1.5446(16) . ? P4 C2 1.864(2) . ? O42 H42 0.92(3) . ? O43 H43 0.94(3) . ? N1 C11 1.505(2) . ? N1 C121 1.516(2) . ? N1 C131 1.522(2) . ? N1 C141 1.526(2) . ? N2 C21 1.499(2) . ? N2 C221 1.522(2) . ? N2 C241 1.525(2) . ? N2 C231 1.526(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C121 C122 1.520(3) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C123 1.520(3) . ? C122 H12C 0.9900 . ? C122 H12D 0.9900 . ? C123 C124 1.520(3) . ? C123 H12E 0.9900 . ? C123 H12F 0.9900 . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C131 C132 1.518(3) . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C132 C133 1.539(3) . ? C132 H13C 0.9900 . ? C132 H13D 0.9900 . ? C133 C134 1.522(3) . ? C133 H13E 0.9900 . ? C133 H13F 0.9900 . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C141 C142 1.526(3) . ? C141 H14A 0.9900 . ? C141 H14B 0.9900 . ? C142 C143 1.524(3) . ? C142 H14C 0.9900 . ? C142 H14D 0.9900 . ? C143 C144 1.528(3) . ? C143 H14E 0.9900 . ? C143 H14F 0.9900 . ? C144 H14A 0.9800 . ? C144 H14B 0.9800 . ? C144 H14C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C221 C222 1.518(3) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 C223 1.528(3) . ? C222 H22C 0.9900 . ? C222 H22D 0.9900 . ? C223 C224 1.523(3) . ? C223 H22E 0.9900 . ? C223 H22F 0.9900 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C224 H22I 0.9800 . ? C231 C232 1.512(3) . ? C231 H23A 0.9900 . ? C231 H23B 0.9900 . ? C232 C233 1.528(3) . ? C232 H23C 0.9900 . ? C232 H23D 0.9900 . ? C233 C234 1.517(3) . ? C233 H23E 0.9900 . ? C233 H23F 0.9900 . ? C234 H23G 0.9800 . ? C234 H23H 0.9800 . ? C234 H23I 0.9800 . ? C241 C242 1.520(3) . ? C241 H24A 0.9900 . ? C241 H24B 0.9900 . ? C242 C243 1.517(3) . ? C242 H24C 0.9900 . ? C242 H24D 0.9900 . ? C243 C244 1.522(3) . ? C243 H24E 0.9900 . ? C243 H24F 0.9900 . ? C244 H24G 0.9800 . ? C244 H24H 0.9800 . ? C244 H24I 0.9800 . ? 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 O11 P1 O12 120.61(9) . . ? O11 P1 O13 108.60(9) . . ? O12 P1 O13 106.50(8) . . ? O11 P1 C1 110.79(9) . . ? O12 P1 C1 109.23(9) . . ? O13 P1 C1 98.81(8) . . ? O22 P2 O21 121.85(9) . . ? O22 P2 O23 108.22(9) . . ? O21 P2 O23 106.53(8) . . ? O22 P2 C1 111.81(10) . . ? O21 P2 C1 107.26(9) . . ? O23 P2 C1 98.54(8) . . ? O33 P3 O23 113.88(8) . . ? O33 P3 O13 113.57(8) . . ? O23 P3 O13 107.00(8) . . ? O33 P3 C2 112.05(9) . . ? O23 P3 C2 104.27(8) . . ? O13 P3 C2 105.29(8) . . ? O41 P4 O42 113.30(9) . . ? O41 P4 O43 113.72(9) . . ? O42 P4 O43 110.86(10) . . ? O41 P4 C2 108.49(9) . . ? O42 P4 C2 104.92(9) . . ? O43 P4 C2 104.75(9) . . ? P3 O13 P1 137.12(9) . . ? P3 O23 P2 136.97(9) . . ? P4 O42 H42 118.3(18) . . ? P4 O43 H43 119.9(17) . . ? Cl2 C1 Cl1 109.84(11) . . ? Cl2 C1 P2 108.03(11) . . ? Cl1 C1 P2 108.04(11) . . ? Cl2 C1 P1 107.20(11) . . ? Cl1 C1 P1 108.34(11) . . ? P2 C1 P1 115.32(11) . . ? Cl4 C2 Cl3 109.06(10) . . ? Cl4 C2 P3 105.54(10) . . ? Cl3 C2 P3 105.01(10) . . ? Cl4 C2 P4 107.22(10) . . ? Cl3 C2 P4 106.57(10) . . ? P3 C2 P4 122.94(11) . . ? C11 N1 C121 110.50(15) . . ? C11 N1 C131 107.05(14) . . ? C121 N1 C131 111.99(15) . . ? C11 N1 C141 109.62(15) . . ? C121 N1 C141 109.08(14) . . ? C131 N1 C141 108.55(15) . . ? C21 N2 C221 110.70(15) . . ? C21 N2 C241 109.72(15) . . ? C221 N2 C241 109.22(14) . . ? C21 N2 C231 106.79(14) . . ? C221 N2 C231 111.91(15) . . ? C241 N2 C231 108.43(14) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C121 C122 114.78(16) . . ? N1 C121 H12A 108.6 . . ? C122 C121 H12A 108.6 . . ? N1 C121 H12B 108.6 . . ? C122 C121 H12B 108.6 . . ? H12A C121 H12B 107.5 . . ? C123 C122 C121 110.45(17) . . ? C123 C122 H12C 109.6 . . ? C121 C122 H12C 109.6 . . ? C123 C122 H12D 109.6 . . ? C121 C122 H12D 109.6 . . ? H12C C122 H12D 108.1 . . ? C122 C123 C124 112.88(18) . . ? C122 C123 H12E 109.0 . . ? C124 C123 H12E 109.0 . . ? C122 C123 H12F 109.0 . . ? C124 C123 H12F 109.0 . . ? H12E C123 H12F 107.8 . . ? C123 C124 H12G 109.5 . . ? C123 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C123 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? C132 C131 N1 115.25(16) . . ? C132 C131 H13A 108.5 . . ? N1 C131 H13A 108.5 . . ? C132 C131 H13B 108.5 . . ? N1 C131 H13B 108.5 . . ? H13A C131 H13B 107.5 . . ? C131 C132 C133 109.44(17) . . ? C131 C132 H13C 109.8 . . ? C133 C132 H13C 109.8 . . ? C131 C132 H13D 109.8 . . ? C133 C132 H13D 109.8 . . ? H13C C132 H13D 108.2 . . ? C134 C133 C132 113.08(17) . . ? C134 C133 H13E 109.0 . . ? C132 C133 H13E 109.0 . . ? C134 C133 H13F 109.0 . . ? C132 C133 H13F 109.0 . . ? H13E C133 H13F 107.8 . . ? C133 C134 H13A 109.5 . . ? C133 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C133 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? N1 C141 C142 115.46(16) . . ? N1 C141 H14A 108.4 . . ? C142 C141 H14A 108.4 . . ? N1 C141 H14B 108.4 . . ? C142 C141 H14B 108.4 . . ? H14A C141 H14B 107.5 . . ? C143 C142 C141 108.92(16) . . ? C143 C142 H14C 109.9 . . ? C141 C142 H14C 109.9 . . ? C143 C142 H14D 109.9 . . ? C141 C142 H14D 109.9 . . ? H14C C142 H14D 108.3 . . ? C142 C143 C144 112.23(18) . . ? C142 C143 H14E 109.2 . . ? C144 C143 H14E 109.2 . . ? C142 C143 H14F 109.2 . . ? C144 C143 H14F 109.2 . . ? H14E C143 H14F 107.9 . . ? C143 C144 H14A 109.5 . . ? C143 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C143 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C222 C221 N2 114.81(16) . . ? C222 C221 H22A 108.6 . . ? N2 C221 H22A 108.6 . . ? C222 C221 H22B 108.6 . . ? N2 C221 H22B 108.6 . . ? H22A C221 H22B 107.5 . . ? C221 C222 C223 111.48(17) . . ? C221 C222 H22C 109.3 . . ? C223 C222 H22C 109.3 . . ? C221 C222 H22D 109.3 . . ? C223 C222 H22D 109.3 . . ? H22C C222 H22D 108.0 . . ? C224 C223 C222 111.11(18) . . ? C224 C223 H22E 109.4 . . ? C222 C223 H22E 109.4 . . ? C224 C223 H22F 109.4 . . ? C222 C223 H22F 109.4 . . ? H22E C223 H22F 108.0 . . ? C223 C224 H22G 109.5 . . ? C223 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C223 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? C232 C231 N2 115.61(15) . . ? C232 C231 H23A 108.4 . . ? N2 C231 H23A 108.4 . . ? C232 C231 H23B 108.4 . . ? N2 C231 H23B 108.4 . . ? H23A C231 H23B 107.4 . . ? C231 C232 C233 110.48(16) . . ? C231 C232 H23C 109.6 . . ? C233 C232 H23C 109.6 . . ? C231 C232 H23D 109.6 . . ? C233 C232 H23D 109.6 . . ? H23C C232 H23D 108.1 . . ? C234 C233 C232 111.47(17) . . ? C234 C233 H23E 109.3 . . ? C232 C233 H23E 109.3 . . ? C234 C233 H23F 109.3 . . ? C232 C233 H23F 109.3 . . ? H23E C233 H23F 108.0 . . ? C233 C234 H23G 109.5 . . ? C233 C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C242 C241 N2 115.67(16) . . ? C242 C241 H24A 108.4 . . ? N2 C241 H24A 108.4 . . ? C242 C241 H24B 108.4 . . ? N2 C241 H24B 108.4 . . ? H24A C241 H24B 107.4 . . ? C243 C242 C241 109.65(17) . . ? C243 C242 H24C 109.7 . . ? C241 C242 H24C 109.7 . . ? C243 C242 H24D 109.7 . . ? C241 C242 H24D 109.7 . . ? H24C C242 H24D 108.2 . . ? C242 C243 C244 112.46(18) . . ? C242 C243 H24E 109.1 . . ? C244 C243 H24E 109.1 . . ? C242 C243 H24F 109.1 . . ? C244 C243 H24F 109.1 . . ? H24E C243 H24F 107.8 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O33 P3 O13 P1 -130.48(13) . . . . ? O23 P3 O13 P1 -3.96(16) . . . . ? C2 P3 O13 P1 106.58(14) . . . . ? O11 P1 O13 P3 143.18(14) . . . . ? O12 P1 O13 P3 -85.52(15) . . . . ? C1 P1 O13 P3 27.64(15) . . . . ? O33 P3 O23 P2 132.03(13) . . . . ? O13 P3 O23 P2 5.69(16) . . . . ? C2 P3 O23 P2 -105.55(14) . . . . ? O22 P2 O23 P3 -146.74(13) . . . . ? O21 P2 O23 P3 80.63(14) . . . . ? C1 P2 O23 P3 -30.32(15) . . . . ? O22 P2 C1 Cl2 -72.20(13) . . . . ? O21 P2 C1 Cl2 63.82(12) . . . . ? O23 P2 C1 Cl2 174.18(10) . . . . ? O22 P2 C1 Cl1 46.57(14) . . . . ? O21 P2 C1 Cl1 -177.41(9) . . . . ? O23 P2 C1 Cl1 -67.05(11) . . . . ? O22 P2 C1 P1 167.93(11) . . . . ? O21 P2 C1 P1 -56.05(13) . . . . ? O23 P2 C1 P1 54.31(12) . . . . ? O11 P1 C1 Cl2 72.48(13) . . . . ? O12 P1 C1 Cl2 -62.70(12) . . . . ? O13 P1 C1 Cl2 -173.69(9) . . . . ? O11 P1 C1 Cl1 -46.00(13) . . . . ? O12 P1 C1 Cl1 178.82(9) . . . . ? O13 P1 C1 Cl1 67.83(11) . . . . ? O11 P1 C1 P2 -167.20(11) . . . . ? O12 P1 C1 P2 57.63(13) . . . . ? O13 P1 C1 P2 -53.37(12) . . . . ? O33 P3 C2 Cl4 -54.68(12) . . . . ? O23 P3 C2 Cl4 -178.30(9) . . . . ? O13 P3 C2 Cl4 69.23(11) . . . . ? O33 P3 C2 Cl3 60.50(12) . . . . ? O23 P3 C2 Cl3 -63.12(11) . . . . ? O13 P3 C2 Cl3 -175.59(8) . . . . ? O33 P3 C2 P4 -177.80(11) . . . . ? O23 P3 C2 P4 58.59(13) . . . . ? O13 P3 C2 P4 -53.88(13) . . . . ? O41 P4 C2 Cl4 56.46(12) . . . . ? O42 P4 C2 Cl4 177.84(10) . . . . ? O43 P4 C2 Cl4 -65.33(12) . . . . ? O41 P4 C2 Cl3 -60.21(12) . . . . ? O42 P4 C2 Cl3 61.18(12) . . . . ? O43 P4 C2 Cl3 178.00(10) . . . . ? O41 P4 C2 P3 178.80(11) . . . . ? O42 P4 C2 P3 -59.81(14) . . . . ? O43 P4 C2 P3 57.02(14) . . . . ? C11 N1 C121 C122 -64.4(2) . . . . ? C131 N1 C121 C122 54.9(2) . . . . ? C141 N1 C121 C122 175.04(16) . . . . ? N1 C121 C122 C123 165.40(17) . . . . ? C121 C122 C123 C124 168.78(19) . . . . ? C11 N1 C131 C132 176.27(17) . . . . ? C121 N1 C131 C132 55.0(2) . . . . ? C141 N1 C131 C132 -65.5(2) . . . . ? N1 C131 C132 C133 162.64(17) . . . . ? C131 C132 C133 C134 -75.4(2) . . . . ? C11 N1 C141 C142 -45.2(2) . . . . ? C121 N1 C141 C142 75.9(2) . . . . ? C131 N1 C141 C142 -161.78(16) . . . . ? N1 C141 C142 C143 -169.03(17) . . . . ? C141 C142 C143 C144 -170.85(18) . . . . ? C21 N2 C221 C222 -57.7(2) . . . . ? C241 N2 C221 C222 -178.60(16) . . . . ? C231 N2 C221 C222 61.3(2) . . . . ? N2 C221 C222 C223 -169.19(17) . . . . ? C221 C222 C223 C224 -170.50(18) . . . . ? C21 N2 C231 C232 174.89(16) . . . . ? C221 N2 C231 C232 53.6(2) . . . . ? C241 N2 C231 C232 -66.9(2) . . . . ? N2 C231 C232 C233 178.21(16) . . . . ? C231 C232 C233 C234 179.63(17) . . . . ? C21 N2 C241 C242 -51.9(2) . . . . ? C221 N2 C241 C242 69.6(2) . . . . ? C231 N2 C241 C242 -168.22(17) . . . . ? N2 C241 C242 C243 177.66(17) . . . . ? C241 C242 C243 C244 -175.33(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O42 H42 O21 0.92(3) 1.55(3) 2.465(2) 173(3) . O43 H43 O12 0.94(3) 1.57(3) 2.500(2) 174(3) . _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.336 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.057