# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Vojtech Kubicek' 'Luce Vander Elst' 'Petr Hermann' 'Jan Kotek' 'Ivan Lukes' 'Robert Muller' 'Joop A. Peters' 'Tomas Vitha' _publ_contact_author_name 'Vojtech Kubicek' _publ_contact_author_email VVVOJTA@VOLNY.CZ _publ_section_title ; A Gd(III) Complex of a Monophosphinate-bis(phosphonate) DOTA Analogue with a High 1H NMR Relaxivity; Lanthanide(III) Complexes for Imaging and Radiotherapy of Calcified Tissues. ; # Attachment 'do3apBP.cif' data_bpped _database_code_depnum_ccdc_archive 'CCDC 710108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H35 N4 O14 P3, 2.25(H2 O)' _chemical_formula_sum 'C17 H39.50 N4 O16.25 P3' _chemical_formula_weight 652.94 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _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 8.78940(10) _cell_length_b 24.6443(3) _cell_length_c 12.78370(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.0428(6) _cell_angle_gamma 90.00 _cell_volume 2758.34(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6414 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12357 _diffrn_reflns_av_R_equivalents 0.0141 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.44 _reflns_number_total 6277 _reflns_number_gt 5560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+1.8800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6277 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.73416(13) 0.23902(5) 0.22042(9) 0.0133(2) Uani 1 1 d . . . H11 H 0.8020 0.2321 0.2768 0.016 Uiso 1 1 calc R . . C2 C 0.58084(16) 0.21694(6) 0.24360(11) 0.0149(3) Uani 1 1 d . . . H21 H 0.5116 0.2187 0.1803 0.018 Uiso 1 1 calc R . . H22 H 0.5392 0.2396 0.2961 0.018 Uiso 1 1 calc R . . C3 C 0.58934(16) 0.15863(6) 0.28293(11) 0.0152(3) Uani 1 1 d . . . H31 H 0.4917 0.1488 0.3075 0.018 Uiso 1 1 calc R . . H32 H 0.6072 0.1349 0.2248 0.018 Uiso 1 1 calc R . . N4 N 0.70996(14) 0.14977(5) 0.36823(9) 0.0138(2) Uani 1 1 d . . . C5 C 0.73061(16) 0.09088(6) 0.38691(11) 0.0151(3) Uani 1 1 d . . . H51 H 0.6336 0.0725 0.3719 0.018 Uiso 1 1 calc R . . H52 H 0.7649 0.0847 0.4601 0.018 Uiso 1 1 calc R . . C6 C 0.84666(16) 0.06789(6) 0.31790(11) 0.0154(3) Uani 1 1 d . . . H61 H 0.8468 0.0286 0.3231 0.019 Uiso 1 1 calc R . . H62 H 0.8175 0.0775 0.2453 0.019 Uiso 1 1 calc R . . N7 N 1.00580(13) 0.08906(5) 0.34943(9) 0.0138(2) Uani 1 1 d . . . H71 H 0.9993 0.1247 0.3671 0.017 Uiso 1 1 calc R . . C8 C 1.10355(17) 0.08405(6) 0.25881(12) 0.0169(3) Uani 1 1 d . . . H81 H 1.0953 0.0475 0.2309 0.020 Uiso 1 1 calc R . . H82 H 1.2095 0.0903 0.2837 0.020 Uiso 1 1 calc R . . C9 C 1.05586(17) 0.12435(6) 0.17177(11) 0.0169(3) Uani 1 1 d . . . H91 H 1.1340 0.1257 0.1228 0.020 Uiso 1 1 calc R . . H92 H 0.9619 0.1120 0.1337 0.020 Uiso 1 1 calc R . . N10 N 1.03241(14) 0.17927(5) 0.21274(9) 0.0145(2) Uani 1 1 d . . . C11 C 0.96250(17) 0.21396(6) 0.12723(11) 0.0163(3) Uani 1 1 d . . . H111 H 0.9941 0.2016 0.0604 0.020 Uiso 1 1 calc R . . H112 H 0.9965 0.2511 0.1381 0.020 Uiso 1 1 calc R . . C12 C 0.79043(17) 0.21133(6) 0.12560(11) 0.0168(3) Uani 1 1 d . . . H121 H 0.7450 0.2287 0.0623 0.020 Uiso 1 1 calc R . . H122 H 0.7583 0.1737 0.1243 0.020 Uiso 1 1 calc R . . C20 C 0.72880(17) 0.29940(6) 0.20294(11) 0.0158(3) Uani 1 1 d . . . H201 H 0.6663 0.3067 0.1381 0.019 Uiso 1 1 calc R . . H202 H 0.8314 0.3120 0.1939 0.019 Uiso 1 1 calc R . . P1 P 0.65325(4) 0.339076(15) 0.30883(3) 0.01340(9) Uani 1 1 d . . . O11 O 0.48831(11) 0.35199(4) 0.27471(8) 0.0167(2) Uani 1 1 d . . . O12 O 0.68691(12) 0.30887(4) 0.41068(8) 0.0177(2) Uani 1 1 d . . . C21 C 0.75389(16) 0.40274(6) 0.30696(12) 0.0160(3) Uani 1 1 d . . . H211 H 0.7553 0.4137 0.2342 0.019 Uiso 1 1 calc R . . H212 H 0.6942 0.4296 0.3409 0.019 Uiso 1 1 calc R . . C22 C 0.92017(16) 0.40588(6) 0.35845(11) 0.0146(3) Uani 1 1 d . . . H221 H 0.9718 0.3721 0.3417 0.018 Uiso 1 1 calc R . . P2 P 0.92301(4) 0.410234(15) 0.50119(3) 0.01529(9) Uani 1 1 d . . . O21 O 0.88968(13) 0.35115(4) 0.53843(8) 0.0208(2) Uani 1 1 d . . . H21P H 0.8218 0.3354 0.4968 0.025 Uiso 1 1 d R . . O22 O 1.08147(12) 0.42506(4) 0.54903(8) 0.0188(2) Uani 1 1 d . . . O23 O 0.79886(12) 0.44923(4) 0.52758(8) 0.0197(2) Uani 1 1 d . . . P3 P 1.01219(4) 0.461219(15) 0.29340(3) 0.01399(9) Uani 1 1 d . . . O31 O 0.90814(12) 0.51133(4) 0.29978(8) 0.0175(2) Uani 1 1 d . . . H31P H 0.9108 0.5322 0.3607 0.021 Uiso 1 1 d R . . O32 O 1.17149(12) 0.47206(4) 0.34992(9) 0.0191(2) Uani 1 1 d . . . H32P H 1.1711 0.5006 0.3982 0.023 Uiso 1 1 d R . . O33 O 1.02440(12) 0.44417(4) 0.18156(8) 0.0190(2) Uani 1 1 d . . . C30 C 0.67889(17) 0.17734(6) 0.46541(11) 0.0164(3) Uani 1 1 d . . . H301 H 0.5963 0.1590 0.4966 0.020 Uiso 1 1 calc R . . H302 H 0.6475 0.2144 0.4500 0.020 Uiso 1 1 calc R . . C31 C 0.82051(17) 0.17723(6) 0.54185(11) 0.0164(3) Uani 1 1 d . . . O311 O 0.78734(13) 0.18951(5) 0.63832(8) 0.0212(2) Uani 1 1 d . . . H311 H 0.8666 0.1772 0.6839 0.025 Uiso 1 1 d R . . O312 O 0.94796(12) 0.16716(5) 0.51824(8) 0.0207(2) Uani 1 1 d . . . C40 C 1.07368(17) 0.05829(6) 0.44275(11) 0.0163(3) Uani 1 1 d . . . H401 H 1.0845 0.0206 0.4228 0.020 Uiso 1 1 calc R . . H402 H 1.0029 0.0595 0.4968 0.020 Uiso 1 1 calc R . . C41 C 1.22784(17) 0.07883(6) 0.48916(11) 0.0174(3) Uani 1 1 d . . . O411 O 1.28602(13) 0.04256(5) 0.55640(9) 0.0238(2) Uani 1 1 d . . . H411 H 1.3711 0.0532 0.5925 0.029 Uiso 1 1 d R . . O412 O 1.28458(13) 0.12172(5) 0.46831(10) 0.0268(3) Uani 1 1 d . . . C50 C 1.17421(16) 0.20226(6) 0.26088(12) 0.0168(3) Uani 1 1 d . . . H501 H 1.2401 0.2111 0.2063 0.020 Uiso 1 1 calc R . . H502 H 1.2261 0.1753 0.3063 0.020 Uiso 1 1 calc R . . C51 C 1.14873(17) 0.25253(6) 0.32409(11) 0.0169(3) Uani 1 1 d . . . O511 O 1.28090(12) 0.27110(5) 0.36753(8) 0.0203(2) Uani 1 1 d . . . H511 H 1.2715 0.3013 0.3950 0.024 Uiso 1 1 d R . . O512 O 1.02582(13) 0.27307(5) 0.33463(9) 0.0237(2) Uani 1 1 d . . . O1W O 1.30684(13) 0.36881(5) 0.44399(9) 0.0227(2) Uani 1 1 d . . . H11W H 1.3553 0.3789 0.4015 0.027 Uiso 1 1 d R . . H12W H 1.2461 0.3920 0.4635 0.027 Uiso 1 1 d R . . O2W O 0.85358(14) 0.05857(5) 0.64857(10) 0.0287(3) Uani 1 1 d . . . H21W H 0.8990 0.0802 0.6912 0.034 Uiso 1 1 d R . . H22W H 0.7559 0.0586 0.6609 0.034 Uiso 1 1 d R . . O3W O 0.9710(6) 0.0033(3) 0.0699(4) 0.0516(18) Uani 0.25 1 d P . . H31W H 1.0120 -0.0235 0.0392 0.062 Uiso 0.25 1 d PR . . H32W H 0.9667 0.0221 0.0265 0.062 Uiso 0.25 1 d PR . . 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 N1 0.0124(5) 0.0155(6) 0.0117(5) -0.0015(5) -0.0005(4) 0.0009(4) C2 0.0121(6) 0.0172(7) 0.0150(7) -0.0012(5) -0.0004(5) -0.0007(5) C3 0.0144(7) 0.0152(7) 0.0156(7) -0.0018(5) -0.0018(5) -0.0012(5) N4 0.0147(6) 0.0135(6) 0.0129(6) -0.0019(4) -0.0007(4) 0.0004(5) C5 0.0150(7) 0.0135(6) 0.0168(7) -0.0002(5) 0.0012(5) -0.0017(5) C6 0.0139(7) 0.0143(6) 0.0179(7) -0.0025(5) -0.0002(5) -0.0020(5) N7 0.0147(6) 0.0119(5) 0.0148(6) -0.0007(4) 0.0004(5) 0.0000(4) C8 0.0171(7) 0.0162(7) 0.0178(7) -0.0007(6) 0.0041(6) 0.0025(5) C9 0.0185(7) 0.0168(7) 0.0156(7) -0.0014(6) 0.0029(5) 0.0015(6) N10 0.0142(6) 0.0148(6) 0.0145(6) -0.0001(5) 0.0010(4) 0.0005(5) C11 0.0172(7) 0.0183(7) 0.0137(6) 0.0015(5) 0.0028(5) 0.0018(6) C12 0.0180(7) 0.0206(7) 0.0119(6) -0.0036(5) 0.0010(5) 0.0023(6) C20 0.0170(7) 0.0157(7) 0.0146(7) 0.0015(5) 0.0019(5) 0.0002(5) P1 0.01407(18) 0.01303(17) 0.01302(17) -0.00017(13) 0.00064(13) -0.00130(13) O11 0.0145(5) 0.0176(5) 0.0178(5) -0.0009(4) 0.0005(4) -0.0010(4) O12 0.0215(5) 0.0162(5) 0.0150(5) 0.0013(4) -0.0001(4) -0.0032(4) C21 0.0161(7) 0.0154(7) 0.0160(7) 0.0014(5) -0.0018(5) -0.0022(5) C22 0.0153(7) 0.0133(6) 0.0149(7) -0.0003(5) -0.0008(5) -0.0007(5) P2 0.01759(19) 0.01442(18) 0.01347(18) -0.00058(13) -0.00093(14) -0.00150(14) O21 0.0290(6) 0.0175(5) 0.0148(5) 0.0018(4) -0.0039(4) -0.0047(4) O22 0.0173(5) 0.0207(5) 0.0179(5) -0.0037(4) -0.0020(4) -0.0001(4) O23 0.0174(5) 0.0205(5) 0.0208(5) -0.0040(4) 0.0001(4) 0.0000(4) P3 0.01409(18) 0.01405(17) 0.01364(18) -0.00056(13) 0.00019(13) -0.00104(13) O31 0.0195(5) 0.0151(5) 0.0172(5) 0.0001(4) -0.0018(4) 0.0022(4) O32 0.0150(5) 0.0195(5) 0.0221(5) -0.0013(4) -0.0027(4) -0.0017(4) O33 0.0186(5) 0.0234(5) 0.0149(5) -0.0022(4) 0.0015(4) -0.0016(4) C30 0.0174(7) 0.0172(7) 0.0145(7) -0.0022(6) 0.0005(5) 0.0019(6) C31 0.0210(7) 0.0123(6) 0.0156(7) -0.0016(5) -0.0003(5) -0.0005(5) O311 0.0237(6) 0.0245(6) 0.0148(5) -0.0050(4) -0.0023(4) 0.0076(5) O312 0.0178(5) 0.0249(6) 0.0192(5) -0.0032(4) -0.0004(4) -0.0016(4) C40 0.0167(7) 0.0144(6) 0.0174(7) 0.0031(5) 0.0006(5) 0.0004(5) C41 0.0183(7) 0.0183(7) 0.0155(7) -0.0004(6) 0.0013(5) 0.0014(6) O411 0.0229(6) 0.0249(6) 0.0221(6) 0.0065(5) -0.0065(4) -0.0022(5) O412 0.0248(6) 0.0235(6) 0.0306(6) 0.0063(5) -0.0061(5) -0.0068(5) C50 0.0132(7) 0.0173(7) 0.0200(7) 0.0008(6) 0.0019(5) -0.0002(5) C51 0.0180(7) 0.0181(7) 0.0144(7) 0.0031(5) 0.0003(5) -0.0014(6) O511 0.0182(5) 0.0211(5) 0.0213(5) -0.0037(4) -0.0008(4) -0.0020(4) O512 0.0190(5) 0.0263(6) 0.0255(6) -0.0067(5) 0.0005(4) 0.0033(5) O1W 0.0225(6) 0.0225(6) 0.0237(6) -0.0003(5) 0.0041(4) 0.0035(4) O2W 0.0334(7) 0.0237(6) 0.0311(6) -0.0086(5) 0.0148(5) -0.0060(5) O3W 0.033(3) 0.089(5) 0.030(3) -0.014(3) -0.010(2) -0.040(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 N1 C20 1.5049(18) . ? N1 C2 1.5067(18) . ? N1 C12 1.5115(18) . ? N1 H11 0.9100 . ? C2 C3 1.522(2) . ? C2 H21 0.9700 . ? C2 H22 0.9700 . ? C3 N4 1.4688(18) . ? C3 H31 0.9700 . ? C3 H32 0.9700 . ? N4 C30 1.4626(18) . ? N4 C5 1.4792(18) . ? C5 C6 1.516(2) . ? C5 H51 0.9700 . ? C5 H52 0.9700 . ? C6 N7 1.5140(18) . ? C6 H61 0.9700 . ? C6 H62 0.9700 . ? N7 C40 1.4930(18) . ? N7 C8 1.5069(18) . ? N7 H71 0.9100 . ? C8 C9 1.523(2) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 N10 1.4721(18) . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? N10 C50 1.4555(18) . ? N10 C11 1.4783(18) . ? C11 C12 1.512(2) . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C12 H121 0.9700 . ? C12 H122 0.9700 . ? C20 P1 1.8405(15) . ? C20 H201 0.9700 . ? C20 H202 0.9700 . ? P1 O12 1.5064(11) . ? P1 O11 1.5106(11) . ? P1 C21 1.8024(15) . ? C21 C22 1.5511(19) . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C22 P3 1.8232(15) . ? C22 P2 1.8258(15) . ? C22 H221 0.9800 . ? P2 O23 1.5142(11) . ? P2 O22 1.5158(11) . ? P2 O21 1.5675(11) . ? O21 H21P 0.8569 . ? P3 O33 1.5030(11) . ? P3 O32 1.5414(11) . ? P3 O31 1.5432(11) . ? O31 H31P 0.9329 . ? O32 H32P 0.9367 . ? C30 C31 1.514(2) . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 O312 1.2112(19) . ? C31 O311 1.3268(18) . ? O311 H311 0.9194 . ? C40 C41 1.518(2) . ? C40 H401 0.9700 . ? C40 H402 0.9700 . ? C41 O412 1.2084(19) . ? C41 O411 1.3123(18) . ? O411 H411 0.8831 . ? C50 C51 1.506(2) . ? C50 H501 0.9700 . ? C50 H502 0.9700 . ? C51 O512 1.2112(19) . ? C51 O511 1.3244(18) . ? O511 H511 0.8298 . ? O1W H11W 0.7610 . ? O1W H12W 0.8352 . ? O2W H21W 0.8378 . ? O2W H22W 0.8866 . ? O3W H31W 0.8635 . ? O3W H32W 0.7210 . ? 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 C20 N1 C2 111.68(11) . . ? C20 N1 C12 109.60(11) . . ? C2 N1 C12 110.86(11) . . ? C20 N1 H11 108.2 . . ? C2 N1 H11 108.2 . . ? C12 N1 H11 108.2 . . ? N1 C2 C3 112.78(11) . . ? N1 C2 H21 109.0 . . ? C3 C2 H21 109.0 . . ? N1 C2 H22 109.0 . . ? C3 C2 H22 109.0 . . ? H21 C2 H22 107.8 . . ? N4 C3 C2 113.39(12) . . ? N4 C3 H31 108.9 . . ? C2 C3 H31 108.9 . . ? N4 C3 H32 108.9 . . ? C2 C3 H32 108.9 . . ? H31 C3 H32 107.7 . . ? C30 N4 C3 112.64(11) . . ? C30 N4 C5 110.36(11) . . ? C3 N4 C5 109.64(11) . . ? N4 C5 C6 110.61(12) . . ? N4 C5 H51 109.5 . . ? C6 C5 H51 109.5 . . ? N4 C5 H52 109.5 . . ? C6 C5 H52 109.5 . . ? H51 C5 H52 108.1 . . ? N7 C6 C5 111.68(11) . . ? N7 C6 H61 109.3 . . ? C5 C6 H61 109.3 . . ? N7 C6 H62 109.3 . . ? C5 C6 H62 109.3 . . ? H61 C6 H62 107.9 . . ? C40 N7 C8 110.97(11) . . ? C40 N7 C6 109.43(11) . . ? C8 N7 C6 110.06(11) . . ? C40 N7 H71 108.8 . . ? C8 N7 H71 108.8 . . ? C6 N7 H71 108.8 . . ? N7 C8 C9 111.68(11) . . ? N7 C8 H81 109.3 . . ? C9 C8 H81 109.3 . . ? N7 C8 H82 109.3 . . ? C9 C8 H82 109.3 . . ? H81 C8 H82 107.9 . . ? N10 C9 C8 112.20(12) . . ? N10 C9 H91 109.2 . . ? C8 C9 H91 109.2 . . ? N10 C9 H92 109.2 . . ? C8 C9 H92 109.2 . . ? H91 C9 H92 107.9 . . ? C50 N10 C9 111.52(11) . . ? C50 N10 C11 111.86(11) . . ? C9 N10 C11 109.31(11) . . ? N10 C11 C12 109.61(12) . . ? N10 C11 H111 109.7 . . ? C12 C11 H111 109.7 . . ? N10 C11 H112 109.7 . . ? C12 C11 H112 109.7 . . ? H111 C11 H112 108.2 . . ? N1 C12 C11 111.53(12) . . ? N1 C12 H121 109.3 . . ? C11 C12 H121 109.3 . . ? N1 C12 H122 109.3 . . ? C11 C12 H122 109.3 . . ? H121 C12 H122 108.0 . . ? N1 C20 P1 115.13(10) . . ? N1 C20 H201 108.5 . . ? P1 C20 H201 108.5 . . ? N1 C20 H202 108.5 . . ? P1 C20 H202 108.5 . . ? H201 C20 H202 107.5 . . ? O12 P1 O11 117.66(6) . . ? O12 P1 C21 112.47(6) . . ? O11 P1 C21 105.81(6) . . ? O12 P1 C20 108.49(6) . . ? O11 P1 C20 107.38(6) . . ? C21 P1 C20 104.09(7) . . ? C22 C21 P1 118.88(10) . . ? C22 C21 H211 107.6 . . ? P1 C21 H211 107.6 . . ? C22 C21 H212 107.6 . . ? P1 C21 H212 107.6 . . ? H211 C21 H212 107.0 . . ? C21 C22 P3 106.44(9) . . ? C21 C22 P2 110.89(10) . . ? P3 C22 P2 116.37(8) . . ? C21 C22 H221 107.6 . . ? P3 C22 H221 107.6 . . ? P2 C22 H221 107.6 . . ? O23 P2 O22 114.31(6) . . ? O23 P2 O21 111.37(6) . . ? O22 P2 O21 106.91(6) . . ? O23 P2 C22 108.25(6) . . ? O22 P2 C22 110.41(6) . . ? O21 P2 C22 105.21(6) . . ? P2 O21 H21P 111.8 . . ? O33 P3 O32 110.88(6) . . ? O33 P3 O31 111.48(6) . . ? O32 P3 O31 110.78(6) . . ? O33 P3 C22 107.24(6) . . ? O32 P3 C22 109.69(6) . . ? O31 P3 C22 106.61(6) . . ? P3 O31 H31P 121.0 . . ? P3 O32 H32P 112.6 . . ? N4 C30 C31 110.07(12) . . ? N4 C30 H301 109.6 . . ? C31 C30 H301 109.6 . . ? N4 C30 H302 109.6 . . ? C31 C30 H302 109.6 . . ? H301 C30 H302 108.2 . . ? O312 C31 O311 124.19(14) . . ? O312 C31 C30 124.45(13) . . ? O311 C31 C30 111.36(13) . . ? C31 O311 H311 107.3 . . ? N7 C40 C41 115.04(12) . . ? N7 C40 H401 108.5 . . ? C41 C40 H401 108.5 . . ? N7 C40 H402 108.5 . . ? C41 C40 H402 108.5 . . ? H401 C40 H402 107.5 . . ? O412 C41 O411 126.56(14) . . ? O412 C41 C40 125.25(14) . . ? O411 C41 C40 108.18(13) . . ? C41 O411 H411 113.8 . . ? N10 C50 C51 112.63(12) . . ? N10 C50 H501 109.1 . . ? C51 C50 H501 109.1 . . ? N10 C50 H502 109.1 . . ? C51 C50 H502 109.1 . . ? H501 C50 H502 107.8 . . ? O512 C51 O511 124.53(14) . . ? O512 C51 C50 125.42(14) . . ? O511 C51 C50 110.05(12) . . ? C51 O511 H511 111.8 . . ? H11W O1W H12W 113.6 . . ? H21W O2W H22W 107.3 . . ? H31W O3W H32W 97.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.495 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.057 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ;