# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Bis(phosphanylamino)benzene ligands: a zinc(II) complex and an unusual nickel(I) complex with a Dewar-benzene-type Ni2P2N2 backbone ; loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Olaf Kuhl' 'Peter Lonnecke' 'Felicite Majoumo-Mbe' ; I.Silaghi-Dumitrescu ; data_c876_fin _database_code_depnum_ccdc_archive 'CCDC 671845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 N2 P2' _chemical_formula_weight 644.78 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6118(12) _cell_length_b 12.6111(14) _cell_length_c 14.9209(17) _cell_angle_alpha 83.586(2) _cell_angle_beta 83.405(2) _cell_angle_gamma 70.247(2) _cell_volume 1861.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'ccd diffractometer (AXS Bruker)' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19834 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.93 _reflns_number_total 8817 _reflns_number_gt 5553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0675P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8817 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.34999(17) 0.10542(14) 0.28619(13) 0.0415(4) Uani 1 1 d . . . C2 C 0.27182(18) 0.13225(15) 0.36832(13) 0.0458(4) Uani 1 1 d . . . C3 C 0.2135(2) 0.05612(19) 0.41398(17) 0.0593(6) Uani 1 1 d . . . C4 C 0.2322(2) -0.04745(19) 0.3836(2) 0.0702(7) Uani 1 1 d . . . C5 C 0.3097(2) -0.07408(17) 0.3040(2) 0.0689(7) Uani 1 1 d . . . C6 C 0.36586(19) 0.00101(15) 0.25208(15) 0.0528(5) Uani 1 1 d . . . C7 C 0.60426(17) 0.13035(13) 0.20517(12) 0.0391(4) Uani 1 1 d . . . C8 C 0.67614(18) 0.07773(14) 0.28047(12) 0.0437(4) Uani 1 1 d . . . C9 C 0.8157(2) 0.03197(16) 0.26789(16) 0.0520(5) Uani 1 1 d . . . C10 C 0.88623(19) 0.03574(16) 0.18528(16) 0.0561(5) Uani 1 1 d . . . C11 C 0.8148(2) 0.08978(18) 0.11235(16) 0.0582(5) Uani 1 1 d . . . C12 C 0.67560(19) 0.13695(16) 0.12059(13) 0.0499(5) Uani 1 1 d . . . C13 C 0.67046(17) 0.52221(13) 0.36484(11) 0.0373(4) Uani 1 1 d . . . C14 C 0.63448(18) 0.56024(14) 0.45219(12) 0.0423(4) Uani 1 1 d . . . C15 C 0.7202(2) 0.51164(16) 0.52004(13) 0.0450(4) Uani 1 1 d . . . C16 C 0.84037(19) 0.42615(15) 0.50561(12) 0.0449(4) Uani 1 1 d . . . C17 C 0.87136(19) 0.38514(16) 0.42062(13) 0.0447(4) Uani 1 1 d . . . C18 C 0.78970(17) 0.43045(14) 0.34992(11) 0.0400(4) Uani 1 1 d . . . C19 C 0.66941(17) 0.63351(14) 0.18349(12) 0.0398(4) Uani 1 1 d . . . C20 C 0.69017(19) 0.59902(16) 0.09443(12) 0.0475(4) Uani 1 1 d . . . C21 C 0.7644(2) 0.6455(2) 0.02947(15) 0.0595(5) Uani 1 1 d . . . C22 C 0.8186(2) 0.72570(19) 0.04675(15) 0.0607(6) Uani 1 1 d . . . C23 C 0.79752(19) 0.75936(17) 0.13270(16) 0.0536(5) Uani 1 1 d . . . C24 C 0.72480(17) 0.71593(14) 0.20141(13) 0.0435(4) Uani 1 1 d . . . C25 C 0.32466(16) 0.42398(13) 0.22954(11) 0.0342(4) Uani 1 1 d . . . C26 C 0.37258(16) 0.51550(13) 0.22429(11) 0.0347(4) Uani 1 1 d . . . C27 C 0.2901(2) 0.62136(15) 0.19287(13) 0.0462(4) Uani 1 1 d . . . C28 C 0.1633(2) 0.63674(17) 0.16861(14) 0.0525(5) Uani 1 1 d . . . C29 C 0.1153(2) 0.54768(16) 0.17409(14) 0.0507(5) Uani 1 1 d . . . C30 C 0.19662(17) 0.44140(15) 0.20540(12) 0.0416(4) Uani 1 1 d . . . C31 C 0.2493(3) 0.2389(2) 0.41372(17) 0.0568(5) Uani 1 1 d . . . C32 C 0.1695(3) -0.1299(2) 0.4359(2) 0.1124(12) Uani 1 1 d . . . H32A H 0.1832 -0.1926 0.4006 0.169 Uiso 1 1 calc R . . H32B H 0.0749 -0.0925 0.4484 0.169 Uiso 1 1 calc R . . H32C H 0.2105 -0.1568 0.4918 0.169 Uiso 1 1 calc R . . C33 C 0.4399(3) -0.0312(2) 0.1626(2) 0.0705(7) Uani 1 1 d . . . C34 C 0.6112(3) 0.0683(2) 0.37436(15) 0.0609(6) Uani 1 1 d . . . C35 C 1.0373(3) -0.0160(3) 0.1747(3) 0.0865(9) Uani 1 1 d . . . C36 C 0.6063(3) 0.1969(3) 0.03679(18) 0.0800(8) Uani 1 1 d . . . C37 C 0.5052(2) 0.6526(2) 0.47633(16) 0.0526(5) Uani 1 1 d . . . C38 C 0.9350(3) 0.3805(2) 0.57939(17) 0.0597(6) Uani 1 1 d . . . C39 C 0.8337(3) 0.3774(2) 0.26122(15) 0.0546(5) Uani 1 1 d . . . C40 C 0.6366(3) 0.5135(2) 0.06374(16) 0.0633(6) Uani 1 1 d . . . C41 C 0.8986(3) 0.7739(3) -0.02675(18) 0.1026(10) Uani 1 1 d . . . H41A H 0.9132 0.8380 -0.0062 0.154 Uiso 1 1 calc R . . H41B H 0.8499 0.7970 -0.0799 0.154 Uiso 1 1 calc R . . H41C H 0.9836 0.7174 -0.0409 0.154 Uiso 1 1 calc R . . C42 C 0.7060(3) 0.76016(19) 0.29331(17) 0.0564(5) Uani 1 1 d . . . N1 N 0.40800(15) 0.31543(11) 0.25823(10) 0.0388(3) Uani 1 1 d . . . N2 N 0.50189(15) 0.49678(13) 0.25019(10) 0.0390(3) Uani 1 1 d . . . P1 P 0.42026(4) 0.19840(4) 0.20739(3) 0.03842(13) Uani 1 1 d . . . P2 P 0.55657(5) 0.59998(4) 0.27763(3) 0.03850(13) Uani 1 1 d . . . H1N H 0.4561(18) 0.3165(15) 0.2970(12) 0.043(5) Uiso 1 1 d . . . H2N H 0.5514(19) 0.4379(16) 0.2401(13) 0.046(6) Uiso 1 1 d . . . H3 H 0.161(2) 0.0774(18) 0.4716(16) 0.074(7) Uiso 1 1 d . . . H5 H 0.327(2) -0.1433(19) 0.2729(14) 0.074(7) Uiso 1 1 d . . . H9 H 0.863(2) -0.0044(17) 0.3159(14) 0.061(6) Uiso 1 1 d . . . H11 H 0.860(2) 0.0958(17) 0.0543(15) 0.064(6) Uiso 1 1 d . . . H15 H 0.6944(17) 0.5335(14) 0.5800(13) 0.046(5) Uiso 1 1 d . . . H17 H 0.9505(19) 0.3215(15) 0.4106(12) 0.046(5) Uiso 1 1 d . . . H21 H 0.776(2) 0.6178(16) -0.0276(14) 0.061(6) Uiso 1 1 d . . . H23 H 0.8301(19) 0.8145(16) 0.1447(12) 0.052(5) Uiso 1 1 d . . . H27 H 0.327(2) 0.6833(17) 0.1837(13) 0.064(6) Uiso 1 1 d . . . H28 H 0.110(2) 0.7065(19) 0.1440(15) 0.070(6) Uiso 1 1 d . . . H29 H 0.026(2) 0.5568(17) 0.1526(14) 0.070(6) Uiso 1 1 d . . . H30 H 0.1636(17) 0.3791(15) 0.2092(11) 0.045(5) Uiso 1 1 d . . . H31A H 0.197(2) 0.2360(16) 0.4686(15) 0.060(6) Uiso 1 1 d . . . H31B H 0.333(2) 0.2451(18) 0.4286(15) 0.077(7) Uiso 1 1 d . . . H31C H 0.207(2) 0.308(2) 0.3748(16) 0.084(8) Uiso 1 1 d . . . H33A H 0.538(2) -0.0415(18) 0.1587(14) 0.074(7) Uiso 1 1 d . . . H33B H 0.412(2) 0.0242(19) 0.1084(15) 0.072(7) Uiso 1 1 d . . . H33C H 0.432(2) -0.106(2) 0.1457(17) 0.102(8) Uiso 1 1 d . . . H34A H 0.670(3) 0.047(2) 0.4117(18) 0.092(9) Uiso 1 1 d . . . H34B H 0.536(3) 0.132(2) 0.3915(17) 0.099(9) Uiso 1 1 d . . . H34C H 0.565(3) 0.011(2) 0.3817(18) 0.106(10) Uiso 1 1 d . . . H35A H 1.068(3) -0.084(3) 0.2045(19) 0.100(10) Uiso 1 1 d . . . H35B H 1.073(3) -0.014(2) 0.108(2) 0.117(11) Uiso 1 1 d . . . H35C H 1.077(3) 0.036(2) 0.192(2) 0.116(11) Uiso 1 1 d . . . H36A H 0.546(3) 0.165(2) 0.0233(19) 0.102(11) Uiso 1 1 d . . . H36B H 0.667(3) 0.198(2) -0.010(2) 0.114(11) Uiso 1 1 d . . . H36C H 0.549(3) 0.282(3) 0.044(2) 0.132(12) Uiso 1 1 d . . . H37A H 0.509(2) 0.722(2) 0.4508(15) 0.073(7) Uiso 1 1 d . . . H37B H 0.427(2) 0.6396(17) 0.4549(14) 0.067(6) Uiso 1 1 d . . . H37C H 0.485(2) 0.6493(17) 0.5389(16) 0.069(7) Uiso 1 1 d . . . H38A H 0.986(3) 0.296(2) 0.5780(17) 0.098(9) Uiso 1 1 d . . . H38B H 0.900(3) 0.374(3) 0.637(2) 0.132(12) Uiso 1 1 d . . . H38C H 1.003(3) 0.410(2) 0.5795(18) 0.100(9) Uiso 1 1 d . . . H39A H 0.824(2) 0.431(2) 0.2069(19) 0.094(8) Uiso 1 1 d . . . H39B H 0.924(3) 0.326(2) 0.2597(16) 0.085(8) Uiso 1 1 d . . . H39C H 0.781(3) 0.335(2) 0.2485(18) 0.099(9) Uiso 1 1 d . . . H40A H 0.665(2) 0.5060(19) -0.0006(17) 0.080(7) Uiso 1 1 d . . . H40B H 0.541(2) 0.5363(18) 0.0750(15) 0.072(7) Uiso 1 1 d . . . H40C H 0.676(2) 0.437(2) 0.0920(15) 0.076(7) Uiso 1 1 d . . . H42A H 0.751(2) 0.7073(17) 0.3343(14) 0.057(6) Uiso 1 1 d . . . H42B H 0.608(2) 0.7851(18) 0.3180(15) 0.074(7) Uiso 1 1 d . . . H42C H 0.739(2) 0.8237(18) 0.2895(14) 0.069(6) 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 0.0362(9) 0.0331(9) 0.0576(11) -0.0017(8) -0.0159(8) -0.0113(7) C2 0.0381(10) 0.0420(10) 0.0583(12) 0.0045(8) -0.0116(9) -0.0146(8) C3 0.0436(12) 0.0584(13) 0.0763(16) 0.0143(11) -0.0151(11) -0.0200(10) C4 0.0487(13) 0.0540(13) 0.112(2) 0.0215(13) -0.0248(14) -0.0253(10) C5 0.0577(14) 0.0338(11) 0.123(2) -0.0012(12) -0.0352(15) -0.0178(10) C6 0.0428(11) 0.0369(10) 0.0817(15) -0.0100(9) -0.0227(10) -0.0097(8) C7 0.0408(9) 0.0344(9) 0.0438(10) -0.0061(7) -0.0079(8) -0.0123(7) C8 0.0430(10) 0.0382(9) 0.0510(11) -0.0050(8) -0.0104(9) -0.0124(8) C9 0.0448(11) 0.0452(11) 0.0655(14) 0.0027(10) -0.0168(11) -0.0124(9) C10 0.0402(11) 0.0480(11) 0.0801(15) -0.0029(10) -0.0046(11) -0.0150(9) C11 0.0511(12) 0.0626(13) 0.0602(14) -0.0030(11) 0.0049(11) -0.0215(10) C12 0.0500(11) 0.0491(11) 0.0500(11) -0.0039(9) -0.0048(9) -0.0154(9) C13 0.0410(9) 0.0371(9) 0.0385(9) -0.0058(7) -0.0024(8) -0.0185(7) C14 0.0486(10) 0.0411(9) 0.0433(10) -0.0081(8) -0.0009(8) -0.0223(8) C15 0.0557(12) 0.0511(11) 0.0356(10) -0.0101(8) -0.0003(9) -0.0262(9) C16 0.0520(11) 0.0500(10) 0.0407(10) 0.0005(8) -0.0083(8) -0.0271(9) C17 0.0430(11) 0.0455(10) 0.0458(11) -0.0031(8) -0.0047(9) -0.0146(9) C18 0.0441(10) 0.0405(9) 0.0390(10) -0.0051(7) -0.0022(8) -0.0182(8) C19 0.0391(9) 0.0381(9) 0.0434(10) 0.0041(7) -0.0095(8) -0.0147(7) C20 0.0481(11) 0.0575(11) 0.0400(10) 0.0022(8) -0.0099(9) -0.0214(9) C21 0.0611(14) 0.0807(15) 0.0402(12) 0.0065(11) -0.0080(10) -0.0300(12) C22 0.0538(13) 0.0762(14) 0.0559(13) 0.0207(11) -0.0119(10) -0.0321(11) C23 0.0452(11) 0.0456(11) 0.0740(15) 0.0139(10) -0.0156(10) -0.0223(9) C24 0.0417(10) 0.0347(9) 0.0552(11) 0.0031(8) -0.0127(9) -0.0134(8) C25 0.0357(9) 0.0322(8) 0.0337(9) -0.0021(7) -0.0037(7) -0.0098(7) C26 0.0351(9) 0.0358(9) 0.0333(9) -0.0038(7) -0.0030(7) -0.0112(7) C27 0.0540(12) 0.0329(9) 0.0522(11) 0.0010(8) -0.0119(9) -0.0138(8) C28 0.0529(12) 0.0387(10) 0.0575(12) 0.0006(9) -0.0175(10) -0.0012(9) C29 0.0413(11) 0.0499(11) 0.0588(12) -0.0042(9) -0.0162(9) -0.0083(9) C30 0.0378(10) 0.0411(10) 0.0477(11) -0.0044(8) -0.0069(8) -0.0140(8) C31 0.0542(13) 0.0617(14) 0.0542(14) -0.0100(11) 0.0084(11) -0.0212(11) C32 0.0819(19) 0.0730(17) 0.192(3) 0.0474(19) -0.032(2) -0.0497(15) C33 0.0706(17) 0.0520(14) 0.093(2) -0.0315(14) -0.0201(15) -0.0140(12) C34 0.0531(14) 0.0737(16) 0.0462(13) 0.0008(11) -0.0142(11) -0.0069(13) C35 0.0428(14) 0.085(2) 0.120(3) 0.0130(19) 0.0010(15) -0.0139(14) C36 0.0712(18) 0.114(3) 0.0467(14) 0.0102(14) -0.0049(14) -0.0245(18) C37 0.0531(13) 0.0570(13) 0.0483(13) -0.0170(10) 0.0025(10) -0.0172(10) C38 0.0658(15) 0.0706(16) 0.0482(13) 0.0017(11) -0.0184(12) -0.0270(13) C39 0.0542(13) 0.0572(13) 0.0449(12) -0.0139(10) -0.0038(10) -0.0057(11) C40 0.0788(18) 0.0873(18) 0.0402(12) -0.0140(12) -0.0016(12) -0.0470(15) C41 0.107(2) 0.141(3) 0.0796(18) 0.0323(18) -0.0045(16) -0.080(2) C42 0.0681(16) 0.0442(12) 0.0685(15) -0.0064(11) -0.0111(12) -0.0311(11) N1 0.0446(9) 0.0309(7) 0.0431(9) -0.0014(6) -0.0174(7) -0.0116(6) N2 0.0365(8) 0.0320(8) 0.0498(9) -0.0067(7) -0.0062(7) -0.0111(7) P1 0.0396(3) 0.0345(2) 0.0418(3) -0.00555(18) -0.0108(2) -0.00992(19) P2 0.0424(3) 0.0349(2) 0.0415(3) -0.00548(18) -0.0046(2) -0.01594(19) _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 C2 1.405(3) . ? C1 C6 1.415(2) . ? C1 P1 1.8425(18) . ? C2 C3 1.388(3) . ? C2 C31 1.508(3) . ? C3 C4 1.374(3) . ? C4 C5 1.370(4) . ? C4 C32 1.517(3) . ? C5 C6 1.401(3) . ? C6 C33 1.493(3) . ? C7 C12 1.404(3) . ? C7 C8 1.404(2) . ? C7 P1 1.8463(18) . ? C8 C9 1.394(3) . ? C8 C34 1.499(3) . ? C9 C10 1.372(3) . ? C10 C11 1.378(3) . ? C10 C35 1.509(3) . ? C11 C12 1.390(3) . ? C12 C36 1.516(3) . ? C13 C14 1.406(2) . ? C13 C18 1.412(2) . ? C13 P2 1.8414(17) . ? C14 C15 1.387(3) . ? C14 C37 1.506(3) . ? C15 C16 1.377(3) . ? C16 C17 1.385(3) . ? C16 C38 1.508(3) . ? C17 C18 1.390(2) . ? C18 C39 1.504(3) . ? C19 C20 1.414(2) . ? C19 C24 1.417(2) . ? C19 P2 1.8463(18) . ? C20 C21 1.383(3) . ? C20 C40 1.510(3) . ? C21 C22 1.380(3) . ? C22 C23 1.366(3) . ? C22 C41 1.510(3) . ? C23 C24 1.387(3) . ? C24 C42 1.505(3) . ? C25 C30 1.385(2) . ? C25 C26 1.402(2) . ? C25 N1 1.406(2) . ? C26 C27 1.390(2) . ? C26 N2 1.404(2) . ? C27 C28 1.378(3) . ? C28 C29 1.373(3) . ? C29 C30 1.389(3) . ? N1 P1 1.6937(14) . ? N2 P2 1.6978(15) . ? 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 C2 C1 C6 118.48(17) . . ? C2 C1 P1 127.43(13) . . ? C6 C1 P1 113.63(15) . . ? C3 C2 C1 119.62(19) . . ? C3 C2 C31 116.2(2) . . ? C1 C2 C31 124.19(17) . . ? C4 C3 C2 122.6(2) . . ? C5 C4 C3 117.7(2) . . ? C5 C4 C32 120.8(2) . . ? C3 C4 C32 121.4(3) . . ? C4 C5 C6 122.7(2) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C33 119.2(2) . . ? C1 C6 C33 122.07(19) . . ? C12 C7 C8 118.88(16) . . ? C12 C7 P1 115.56(13) . . ? C8 C7 P1 125.51(14) . . ? C9 C8 C7 118.59(18) . . ? C9 C8 C34 117.78(18) . . ? C7 C8 C34 123.63(17) . . ? C10 C9 C8 123.05(19) . . ? C9 C10 C11 117.77(19) . . ? C9 C10 C35 121.2(2) . . ? C11 C10 C35 121.0(2) . . ? C10 C11 C12 121.8(2) . . ? C11 C12 C7 119.84(18) . . ? C11 C12 C36 117.9(2) . . ? C7 C12 C36 122.26(19) . . ? C14 C13 C18 118.77(16) . . ? C14 C13 P2 116.07(13) . . ? C18 C13 P2 125.16(13) . . ? C15 C14 C13 119.56(17) . . ? C15 C14 C37 117.64(17) . . ? C13 C14 C37 122.81(17) . . ? C16 C15 C14 122.49(17) . . ? C15 C16 C17 117.43(17) . . ? C15 C16 C38 120.97(18) . . ? C17 C16 C38 121.59(19) . . ? C16 C17 C18 122.65(18) . . ? C17 C18 C13 118.92(16) . . ? C17 C18 C39 117.50(17) . . ? C13 C18 C39 123.58(17) . . ? C20 C19 C24 117.87(16) . . ? C20 C19 P2 127.48(13) . . ? C24 C19 P2 113.99(13) . . ? C21 C20 C19 119.03(18) . . ? C21 C20 C40 116.35(18) . . ? C19 C20 C40 124.61(18) . . ? C22 C21 C20 123.2(2) . . ? C23 C22 C21 117.55(19) . . ? C23 C22 C41 121.4(2) . . ? C21 C22 C41 121.1(2) . . ? C22 C23 C24 122.41(19) . . ? C23 C24 C19 119.91(18) . . ? C23 C24 C42 118.03(17) . . ? C19 C24 C42 122.06(17) . . ? C30 C25 C26 119.61(15) . . ? C30 C25 N1 120.91(15) . . ? C26 C25 N1 119.48(14) . . ? C27 C26 C25 118.48(15) . . ? C27 C26 N2 122.58(15) . . ? C25 C26 N2 118.94(14) . . ? C28 C27 C26 120.98(17) . . ? C29 C28 C27 120.89(18) . . ? C28 C29 C30 118.74(18) . . ? C25 C30 C29 121.28(17) . . ? C25 N1 P1 122.63(12) . . ? C26 N2 P2 124.22(12) . . ? N1 P1 C1 109.66(8) . . ? N1 P1 C7 98.12(7) . . ? C1 P1 C7 105.13(8) . . ? N2 P2 C13 100.78(7) . . ? N2 P2 C19 109.72(8) . . ? C13 P2 C19 103.96(8) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.217 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.041 # Attachment 'ccdc_671846_new.cif' data_c888_fin _database_code_depnum_ccdc_archive 'CCDC 671846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H104 N4 O7 P4 Zn2' _chemical_formula_weight 1584.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 22.577(2) _cell_length_b 15.4672(17) _cell_length_c 24.523(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.566(2) _cell_angle_gamma 90.00 _cell_volume 8249.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.27 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'ccd diffractometer (AXS Bruker)' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48341 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.37 _reflns_number_total 16860 _reflns_number_gt 10051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 858.2 265.7 2 0.000 0.500 1.000 858.3 265.7 _platon_squeeze_details ; Three solvent molecules (thf) had been removed by using the program SQUEEZE ; _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^)+(0.0881P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16860 _refine_ls_number_parameters 943 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.005 _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 Zn1 Zn 0.903306(16) 0.01244(2) 0.207243(15) 0.04045(11) Uani 1 1 d . . . Zn2 Zn 0.785837(16) 0.06785(2) 0.089762(15) 0.03990(11) Uani 1 1 d . . . P1 P 1.02034(4) -0.04162(6) 0.29948(4) 0.0485(2) Uani 1 1 d . . . P2 P 0.78116(4) -0.06969(5) 0.12736(4) 0.0417(2) Uani 1 1 d . . . P3 P 0.68757(4) 0.07987(6) -0.02612(4) 0.0466(2) Uani 1 1 d . . . P4 P 0.92780(4) 0.10851(5) 0.14356(4) 0.0404(2) Uani 1 1 d . . . N1 N 0.95144(12) -0.07129(17) 0.25881(11) 0.0454(6) Uani 1 1 d . . . N2 N 0.84293(11) -0.08081(16) 0.18027(11) 0.0422(6) Uani 1 1 d . . . N3 N 0.75678(12) 0.11032(17) 0.01332(11) 0.0446(6) Uani 1 1 d . . . N4 N 0.86494(11) 0.12470(16) 0.09317(11) 0.0416(6) Uani 1 1 d . . . C1 C 1.07949(17) -0.1127(3) 0.28435(19) 0.0660(11) Uani 1 1 d . . . C2 C 1.0950(2) -0.0951(4) 0.2344(2) 0.0963(16) Uani 1 1 d . . . H2 H 1.0728 -0.0525 0.2099 0.116 Uiso 1 1 calc R . . C3 C 1.1419(3) -0.1380(5) 0.2195(3) 0.134(2) Uani 1 1 d . . . H3 H 1.1518 -0.1243 0.1856 0.161 Uiso 1 1 calc R . . C4 C 1.1734(3) -0.1998(6) 0.2540(4) 0.146(3) Uani 1 1 d . . . H4 H 1.2052 -0.2298 0.2441 0.175 Uiso 1 1 calc R . . C5 C 1.1594(3) -0.2188(4) 0.3032(4) 0.129(2) Uani 1 1 d . . . H5 H 1.1819 -0.2617 0.3271 0.155 Uiso 1 1 calc R . . C6 C 1.1123(2) -0.1757(3) 0.3184(2) 0.0877(14) Uani 1 1 d . . . H6 H 1.1029 -0.1901 0.3524 0.105 Uiso 1 1 calc R . . C7 C 1.02309(16) -0.0715(2) 0.37264(15) 0.0503(8) Uani 1 1 d . . . C8 C 1.07789(19) -0.0627(3) 0.41520(18) 0.0639(10) Uani 1 1 d . . . C9 C 1.0802(2) -0.0754(3) 0.47165(19) 0.0797(14) Uani 1 1 d . . . C10 C 1.0269(3) -0.0977(3) 0.4861(2) 0.0893(15) Uani 1 1 d . . . C11 C 0.9725(2) -0.1051(3) 0.44537(19) 0.0825(13) Uani 1 1 d . . . C12 C 0.97050(19) -0.0919(3) 0.38879(17) 0.0611(10) Uani 1 1 d . . . C13 C 0.92369(14) -0.1525(2) 0.25042(14) 0.0440(8) Uani 1 1 d . . . C14 C 0.94719(18) -0.2278(2) 0.27896(16) 0.0545(9) Uani 1 1 d . . . C15 C 0.91641(19) -0.3052(2) 0.26905(18) 0.0588(10) Uani 1 1 d . . . C16 C 0.86050(18) -0.3115(2) 0.22974(16) 0.0563(9) Uani 1 1 d . . . C17 C 0.83508(17) -0.2373(2) 0.20007(16) 0.0508(8) Uani 1 1 d . . . C18 C 0.86516(14) -0.1580(2) 0.20903(14) 0.0428(7) Uani 1 1 d . . . C19 C 0.77797(17) -0.1522(2) 0.07324(15) 0.0528(9) Uani 1 1 d . . . C20 C 0.8257(2) -0.1552(3) 0.0492(2) 0.1010(18) Uani 1 1 d . . . H20 H 0.8587 -0.1168 0.0623 0.121 Uiso 1 1 calc R . . C21 C 0.8276(3) -0.2127(4) 0.0062(3) 0.121(2) Uani 1 1 d . . . H21 H 0.8615 -0.2136 -0.0092 0.145 Uiso 1 1 calc R . . C22 C 0.7796(4) -0.2674(4) -0.0132(3) 0.114(2) Uani 1 1 d . . . H22 H 0.7800 -0.3072 -0.0420 0.137 Uiso 1 1 calc R . . C23 C 0.7311(3) -0.2642(4) 0.0092(3) 0.114(2) Uani 1 1 d . . . H23 H 0.6974 -0.3012 -0.0051 0.137 Uiso 1 1 calc R . . C24 C 0.7298(2) -0.2081(3) 0.0527(2) 0.0883(15) Uani 1 1 d . . . H24 H 0.6960 -0.2081 0.0682 0.106 Uiso 1 1 calc R . . C25 C 0.71117(15) -0.0854(2) 0.14964(15) 0.0468(8) Uani 1 1 d . . . C26 C 0.71314(18) -0.1017(2) 0.20546(17) 0.0551(9) Uani 1 1 d . . . C27 C 0.6596(2) -0.1038(3) 0.2230(2) 0.0744(12) Uani 1 1 d . . . C28 C 0.6043(2) -0.0908(3) 0.1842(3) 0.0862(16) Uani 1 1 d . . . C29 C 0.6012(2) -0.0737(3) 0.1284(2) 0.0822(14) Uani 1 1 d . . . C30 C 0.65466(19) -0.0714(3) 0.1113(2) 0.0670(12) Uani 1 1 d . . . C31 C 0.69821(17) 0.0392(2) -0.09347(16) 0.0544(9) Uani 1 1 d . . . C32 C 0.7344(2) -0.0338(3) -0.0897(2) 0.0795(14) Uani 1 1 d . . . C33 C 0.7421(2) -0.0735(4) -0.1382(3) 0.1038(19) Uani 1 1 d . . . C34 C 0.7129(3) -0.0403(5) -0.1908(3) 0.111(2) Uani 1 1 d . . . C35 C 0.6788(3) 0.0297(5) -0.1947(2) 0.1118(19) Uani 1 1 d . . . C36 C 0.6708(3) 0.0713(3) -0.14637(19) 0.0883(15) Uani 1 1 d . . . C37 C 0.64161(15) 0.1771(2) -0.04946(14) 0.0489(8) Uani 1 1 d . . . C38 C 0.58007(19) 0.1677(3) -0.0793(2) 0.0725(12) Uani 1 1 d . . . C39 C 0.5422(2) 0.2396(4) -0.0946(2) 0.0841(14) Uani 1 1 d . . . C40 C 0.5645(2) 0.3201(4) -0.0813(2) 0.0831(15) Uani 1 1 d . . . C41 C 0.6248(2) 0.3317(3) -0.0508(2) 0.0776(13) Uani 1 1 d . . . C42 C 0.66322(19) 0.2601(3) -0.03491(17) 0.0607(10) Uani 1 1 d . . . C43 C 0.80366(14) 0.15644(19) -0.00194(13) 0.0415(7) Uani 1 1 d . . . C44 C 0.79804(17) 0.1939(2) -0.05471(15) 0.0505(8) Uani 1 1 d . . . C45 C 0.84616(19) 0.2391(3) -0.06684(16) 0.0596(10) Uani 1 1 d . . . C46 C 0.90167(19) 0.2481(2) -0.02571(16) 0.0580(9) Uani 1 1 d . . . C47 C 0.90806(17) 0.2107(2) 0.02748(16) 0.0504(8) Uani 1 1 d . . . C48 C 0.86068(15) 0.16451(19) 0.03988(13) 0.0411(7) Uani 1 1 d . . . C49 C 0.96095(14) 0.2091(2) 0.17754(14) 0.0445(8) Uani 1 1 d . . . C50 C 0.93446(18) 0.2885(2) 0.16102(16) 0.0521(9) Uani 1 1 d . . . C51 C 0.9593(2) 0.3634(3) 0.18974(19) 0.0658(11) Uani 1 1 d . . . C52 C 1.0104(2) 0.3582(3) 0.2352(2) 0.0754(13) Uani 1 1 d . . . C53 C 1.0361(2) 0.2783(3) 0.2530(2) 0.0790(14) Uani 1 1 d . . . C54 C 1.01153(18) 0.2042(3) 0.22512(18) 0.0646(11) Uani 1 1 d . . . C55 C 0.98828(15) 0.0621(2) 0.11548(15) 0.0491(8) Uani 1 1 d . . . C56 C 1.0424(2) 0.1005(3) 0.1157(2) 0.0945(17) Uani 1 1 d . . . H56 H 1.0512 0.1564 0.1308 0.113 Uiso 1 1 calc R . . C57 C 1.0848(2) 0.0575(4) 0.0937(3) 0.1074(19) Uani 1 1 d . . . H57 H 1.1221 0.0850 0.0945 0.129 Uiso 1 1 calc R . . C58 C 1.0741(2) -0.0221(4) 0.0715(2) 0.0849(14) Uani 1 1 d . . . H58 H 1.1035 -0.0504 0.0571 0.102 Uiso 1 1 calc R . . C59 C 1.0212(3) -0.0594(4) 0.0705(3) 0.112(2) Uani 1 1 d . . . H59 H 1.0123 -0.1144 0.0539 0.135 Uiso 1 1 calc R . . C60 C 0.9788(2) -0.0189(3) 0.0934(2) 0.0972(17) Uani 1 1 d . . . H60 H 0.9424 -0.0482 0.0937 0.117 Uiso 1 1 calc R . . O1 O 0.86578(10) 0.09660(15) 0.25908(10) 0.0519(6) Uani 1 1 d D . . C61 C 0.90481(18) 0.1512(3) 0.30161(18) 0.0735(12) Uani 1 1 d D . . H61A H 0.9457 0.1252 0.3155 0.088 Uiso 1 1 calc R . . H61B H 0.9094 0.2082 0.2857 0.088 Uiso 1 1 calc R . . C62 C 0.8758(2) 0.1592(4) 0.3470(2) 0.1075(19) Uani 1 1 d D . . H62A H 0.8995 0.1280 0.3805 0.129 Uiso 1 1 calc R . . H62B H 0.8733 0.2202 0.3570 0.129 Uiso 1 1 calc R . . C63 C 0.8168(3) 0.1240(5) 0.3279(3) 0.167(4) Uani 1 1 d D . . H63A H 0.7863 0.1701 0.3158 0.200 Uiso 1 1 calc R . . H63B H 0.8066 0.0912 0.3584 0.200 Uiso 1 1 calc R . . C64 C 0.8165(2) 0.0670(3) 0.2804(2) 0.0858(15) Uani 1 1 d D . . H64A H 0.8231 0.0068 0.2930 0.103 Uiso 1 1 calc R . . H64B H 0.7773 0.0711 0.2512 0.103 Uiso 1 1 calc R . . O2 O 0.74177(10) 0.14584(15) 0.13880(10) 0.0543(6) Uani 1 1 d . . . C65 C 0.67549(17) 0.1487(3) 0.12353(19) 0.0717(12) Uani 1 1 d . . . H65A H 0.6597 0.1202 0.1524 0.086 Uiso 1 1 calc R . . H65B H 0.6583 0.1199 0.0871 0.086 Uiso 1 1 calc R . . C66 C 0.6591(2) 0.2424(3) 0.1196(2) 0.0915(15) Uani 1 1 d . . . H66A H 0.6522 0.2635 0.0807 0.110 Uiso 1 1 calc R . . H66B H 0.6222 0.2531 0.1323 0.110 Uiso 1 1 calc R . . C67 C 0.7127(3) 0.2837(3) 0.1571(3) 0.1041(17) Uani 1 1 d . . . H67A H 0.7166 0.3437 0.1457 0.125 Uiso 1 1 calc R . . H67B H 0.7100 0.2831 0.1963 0.125 Uiso 1 1 calc R . . C68 C 0.7642(2) 0.2325(3) 0.1513(2) 0.0895(15) Uani 1 1 d . . . H68A H 0.7801 0.2551 0.1207 0.107 Uiso 1 1 calc R . . H68B H 0.7974 0.2337 0.1865 0.107 Uiso 1 1 calc R . . O3 O 0.2456(3) 0.6515(5) 0.1945(3) 0.210(3) Uani 1 1 d D . . C69 C 0.3081(3) 0.6743(5) 0.2148(5) 0.224(6) Uani 1 1 d D . . H69A H 0.3174 0.7271 0.1967 0.269 Uiso 1 1 calc R . . H69B H 0.3197 0.6825 0.2560 0.269 Uiso 1 1 calc R . . C70 C 0.3363(4) 0.6055(9) 0.2002(8) 0.380(13) Uani 1 1 d D . . H70A H 0.3582 0.5744 0.2345 0.456 Uiso 1 1 calc R . . H70B H 0.3667 0.6252 0.1810 0.456 Uiso 1 1 calc R . . C71 C 0.2942(4) 0.5476(7) 0.1636(6) 0.249(7) Uani 1 1 d D . . H71A H 0.3039 0.5415 0.1272 0.298 Uiso 1 1 calc R . . H71B H 0.2954 0.4903 0.1810 0.298 Uiso 1 1 calc R . . C72 C 0.2408(5) 0.5837(7) 0.1572(5) 0.232(6) Uani 1 1 d D . . H72A H 0.2115 0.5410 0.1640 0.279 Uiso 1 1 calc R . . H72B H 0.2255 0.6049 0.1183 0.279 Uiso 1 1 calc R . . O4 O 0.4935(4) 0.0714(5) 0.1028(4) 0.237(4) Uani 1 1 d D . . C73 C 0.4972(7) 0.1009(13) 0.0493(7) 0.387(14) Uani 1 1 d D . . H73A H 0.5379 0.1255 0.0521 0.464 Uiso 1 1 calc R . . H73B H 0.4902 0.0530 0.0222 0.464 Uiso 1 1 calc R . . C74 C 0.4517(6) 0.1640(8) 0.0317(5) 0.222(6) Uani 1 1 d D . . H74A H 0.4702 0.2216 0.0340 0.267 Uiso 1 1 calc R . . H74B H 0.4279 0.1535 -0.0074 0.267 Uiso 1 1 calc R . . C75 C 0.4139(6) 0.1582(9) 0.0680(4) 0.237(7) Uani 1 1 d D . . H75A H 0.4064 0.2161 0.0811 0.285 Uiso 1 1 calc R . . H75B H 0.3742 0.1330 0.0480 0.285 Uiso 1 1 calc R . . C76 C 0.4422(4) 0.1068(6) 0.1142(4) 0.162(3) Uani 1 1 d D . . H76A H 0.4539 0.1417 0.1487 0.195 Uiso 1 1 calc R . . H76B H 0.4142 0.0611 0.1194 0.195 Uiso 1 1 calc R . . H8 H 1.1169(17) -0.055(2) 0.4045(16) 0.062(11) Uiso 1 1 d . . . H9 H 1.1243(19) -0.069(2) 0.5031(18) 0.083(13) Uiso 1 1 d . . . H10 H 1.019(3) -0.099(4) 0.526(3) 0.14(2) Uiso 1 1 d . . . H11 H 0.925(2) -0.110(3) 0.4566(19) 0.104(15) Uiso 1 1 d . . . H12 H 0.9306(18) -0.091(2) 0.3614(17) 0.070(12) Uiso 1 1 d . . . H14 H 0.9840(16) -0.223(2) 0.3065(15) 0.056(10) Uiso 1 1 d . . . H15 H 0.9338(16) -0.349(2) 0.2861(15) 0.057(11) Uiso 1 1 d . . . H16 H 0.8366(15) -0.370(2) 0.2208(14) 0.060(10) Uiso 1 1 d . . . H17 H 0.7959(17) -0.241(2) 0.1710(16) 0.068(11) Uiso 1 1 d . . . H19 H 0.721(2) -0.066(3) -0.221(2) 0.099(16) Uiso 1 1 d . . . H26 H 0.7531(18) -0.115(2) 0.2312(17) 0.073(12) Uiso 1 1 d . . . H27 H 0.665(2) -0.109(3) 0.262(2) 0.090(15) Uiso 1 1 d . . . H28 H 0.572(2) -0.087(3) 0.197(2) 0.114(19) Uiso 1 1 d . . . H29 H 0.562(2) -0.056(3) 0.1020(18) 0.081(13) Uiso 1 1 d . . . H30 H 0.6538(17) -0.059(2) 0.0790(16) 0.053(12) Uiso 1 1 d . . . H32 H 0.753(2) -0.057(3) -0.053(2) 0.086(15) Uiso 1 1 d . . . H33 H 0.771(2) -0.145(4) -0.120(2) 0.126(18) Uiso 1 1 d . . . H35 H 0.649(3) 0.066(5) -0.234(3) 0.19(3) Uiso 1 1 d . . . H36 H 0.633(3) 0.116(4) -0.153(3) 0.17(3) Uiso 1 1 d . . . H38 H 0.5637(19) 0.111(3) -0.0866(18) 0.086(14) Uiso 1 1 d . . . H39 H 0.497(2) 0.230(3) -0.107(2) 0.109(16) Uiso 1 1 d . . . H40 H 0.540(2) 0.360(3) -0.084(2) 0.098(17) Uiso 1 1 d . . . H41 H 0.646(2) 0.384(3) -0.041(2) 0.094(16) Uiso 1 1 d . . . H42 H 0.7071(15) 0.269(2) -0.0135(14) 0.051(9) Uiso 1 1 d . . . H44 H 0.7592(15) 0.1904(19) -0.0880(14) 0.047(9) Uiso 1 1 d . . . H45 H 0.8391(17) 0.270(3) -0.1103(18) 0.081(12) Uiso 1 1 d . . . H46 H 0.9384(14) 0.2842(19) -0.0342(13) 0.043(8) Uiso 1 1 d . . . H47 H 0.9446(15) 0.217(2) 0.0543(14) 0.046(9) Uiso 1 1 d . . . H50 H 0.8994(17) 0.291(2) 0.1316(16) 0.063(11) Uiso 1 1 d . . . H51 H 0.9433(19) 0.417(3) 0.1797(18) 0.079(14) Uiso 1 1 d . . . H52 H 1.0268(19) 0.410(3) 0.2536(18) 0.084(13) Uiso 1 1 d . . . H53 H 1.065(2) 0.273(3) 0.2831(19) 0.081(14) Uiso 1 1 d . . . H54 H 1.0265(15) 0.153(2) 0.2398(14) 0.049(10) 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 Zn1 0.0376(2) 0.0387(2) 0.0397(2) 0.00315(15) 0.00101(15) -0.00037(16) Zn2 0.0360(2) 0.0411(2) 0.0377(2) 0.00380(15) 0.00143(15) -0.00122(16) P1 0.0379(5) 0.0474(5) 0.0529(6) 0.0060(4) -0.0004(4) 0.0007(4) P2 0.0390(4) 0.0405(4) 0.0404(5) 0.0022(4) 0.0015(4) -0.0034(4) P3 0.0432(5) 0.0480(5) 0.0406(5) 0.0029(4) -0.0028(4) -0.0024(4) P4 0.0354(4) 0.0415(4) 0.0399(5) 0.0014(4) 0.0028(3) -0.0024(4) N1 0.0395(15) 0.0440(15) 0.0456(16) 0.0061(12) -0.0006(12) 0.0007(12) N2 0.0357(14) 0.0390(14) 0.0463(16) 0.0040(11) 0.0014(12) -0.0041(11) N3 0.0435(15) 0.0487(16) 0.0344(15) 0.0032(12) -0.0019(12) -0.0007(13) N4 0.0366(14) 0.0446(15) 0.0389(15) 0.0033(11) 0.0023(11) -0.0023(12) C1 0.048(2) 0.068(3) 0.076(3) -0.004(2) 0.007(2) 0.0097(19) C2 0.088(3) 0.124(4) 0.080(4) -0.001(3) 0.026(3) 0.034(3) C3 0.108(5) 0.183(7) 0.119(5) -0.017(5) 0.044(4) 0.051(5) C4 0.097(5) 0.183(8) 0.162(8) -0.038(6) 0.039(5) 0.062(5) C5 0.091(4) 0.129(5) 0.160(7) -0.001(5) 0.019(4) 0.059(4) C6 0.070(3) 0.082(3) 0.108(4) 0.009(3) 0.018(3) 0.031(3) C7 0.049(2) 0.0419(18) 0.051(2) 0.0028(15) -0.0024(16) 0.0001(16) C8 0.054(2) 0.062(2) 0.064(3) 0.0053(19) -0.004(2) -0.002(2) C9 0.086(3) 0.076(3) 0.056(3) 0.009(2) -0.017(2) -0.007(3) C10 0.106(4) 0.102(4) 0.050(3) 0.006(2) 0.004(3) -0.020(3) C11 0.091(3) 0.097(3) 0.056(3) -0.004(2) 0.015(3) -0.020(3) C12 0.053(2) 0.069(3) 0.054(2) 0.0016(19) 0.0017(19) -0.005(2) C13 0.0422(18) 0.0412(18) 0.0439(19) 0.0037(14) 0.0032(14) 0.0015(15) C14 0.053(2) 0.047(2) 0.056(2) 0.0076(17) 0.0007(18) 0.0064(17) C15 0.063(3) 0.040(2) 0.069(3) 0.0113(18) 0.009(2) 0.0141(19) C16 0.066(2) 0.0377(19) 0.062(2) 0.0035(16) 0.011(2) -0.0038(18) C17 0.048(2) 0.046(2) 0.051(2) 0.0026(16) 0.0009(17) -0.0001(16) C18 0.0429(18) 0.0401(17) 0.0421(19) 0.0034(14) 0.0059(14) 0.0023(14) C19 0.060(2) 0.0448(19) 0.048(2) -0.0016(15) 0.0037(17) 0.0006(17) C20 0.094(4) 0.102(4) 0.121(5) -0.054(3) 0.053(3) -0.031(3) C21 0.128(5) 0.122(5) 0.127(5) -0.054(4) 0.058(4) -0.005(4) C22 0.169(6) 0.076(4) 0.091(4) -0.031(3) 0.023(4) 0.007(4) C23 0.116(5) 0.104(4) 0.114(5) -0.055(4) 0.015(4) -0.028(4) C24 0.088(3) 0.081(3) 0.095(4) -0.037(3) 0.022(3) -0.027(3) C25 0.0418(18) 0.0407(18) 0.054(2) 0.0071(15) 0.0056(16) -0.0056(14) C26 0.050(2) 0.053(2) 0.061(3) 0.0058(18) 0.0119(19) -0.0074(18) C27 0.070(3) 0.084(3) 0.075(3) 0.011(3) 0.031(3) -0.001(2) C28 0.055(3) 0.094(4) 0.117(5) 0.021(3) 0.037(3) -0.001(3) C29 0.043(2) 0.095(3) 0.102(4) 0.032(3) 0.007(2) -0.002(2) C30 0.053(2) 0.078(3) 0.064(3) 0.019(2) 0.005(2) -0.006(2) C31 0.052(2) 0.052(2) 0.052(2) -0.0096(16) 0.0021(17) -0.0055(17) C32 0.061(3) 0.079(3) 0.083(4) -0.026(3) -0.007(2) 0.008(2) C33 0.067(3) 0.108(4) 0.130(5) -0.056(4) 0.015(3) -0.002(3) C34 0.103(5) 0.138(6) 0.096(5) -0.064(4) 0.035(4) -0.015(4) C35 0.151(6) 0.121(5) 0.063(4) -0.021(3) 0.027(4) 0.013(4) C36 0.107(4) 0.099(4) 0.051(3) -0.010(2) 0.006(3) 0.017(3) C37 0.048(2) 0.057(2) 0.0364(19) 0.0021(15) 0.0027(15) 0.0084(17) C38 0.056(3) 0.068(3) 0.079(3) 0.005(2) -0.007(2) 0.004(2) C39 0.055(3) 0.090(4) 0.091(4) 0.010(3) -0.006(2) 0.015(3) C40 0.072(3) 0.080(3) 0.089(4) 0.013(3) 0.008(3) 0.034(3) C41 0.082(3) 0.056(3) 0.086(3) 0.002(2) 0.007(3) 0.017(3) C42 0.054(2) 0.061(2) 0.061(3) -0.0036(19) 0.0042(19) 0.007(2) C43 0.0425(18) 0.0387(17) 0.0399(18) 0.0038(14) 0.0055(14) 0.0040(14) C44 0.058(2) 0.051(2) 0.039(2) 0.0030(15) 0.0064(17) 0.0008(17) C45 0.072(3) 0.062(2) 0.044(2) 0.0078(18) 0.0142(19) 0.000(2) C46 0.063(2) 0.059(2) 0.055(2) 0.0048(18) 0.020(2) -0.0069(19) C47 0.047(2) 0.054(2) 0.048(2) 0.0009(16) 0.0087(17) -0.0027(17) C48 0.0467(18) 0.0396(17) 0.0368(18) -0.0012(13) 0.0110(14) -0.0004(14) C49 0.0406(18) 0.0484(19) 0.0425(19) -0.0005(15) 0.0075(15) -0.0088(15) C50 0.052(2) 0.051(2) 0.052(2) -0.0026(17) 0.0117(19) -0.0027(18) C51 0.078(3) 0.049(2) 0.070(3) -0.010(2) 0.020(2) -0.003(2) C52 0.075(3) 0.067(3) 0.083(3) -0.029(3) 0.020(3) -0.026(3) C53 0.068(3) 0.088(4) 0.067(3) -0.017(3) -0.007(2) -0.022(3) C54 0.055(2) 0.061(3) 0.065(3) 0.002(2) -0.0043(19) -0.007(2) C55 0.0430(19) 0.052(2) 0.050(2) 0.0035(16) 0.0082(15) 0.0020(16) C56 0.062(3) 0.080(3) 0.153(5) -0.033(3) 0.049(3) -0.009(2) C57 0.065(3) 0.120(5) 0.153(6) -0.015(4) 0.057(4) 0.001(3) C58 0.080(3) 0.094(4) 0.092(4) -0.001(3) 0.041(3) 0.027(3) C59 0.102(4) 0.097(4) 0.152(6) -0.049(4) 0.058(4) -0.002(3) C60 0.079(3) 0.084(3) 0.142(5) -0.053(3) 0.052(3) -0.019(3) O1 0.0465(13) 0.0535(14) 0.0529(15) -0.0101(11) 0.0085(11) -0.0002(11) C61 0.060(2) 0.084(3) 0.076(3) -0.034(2) 0.018(2) -0.014(2) C62 0.098(4) 0.147(5) 0.074(4) -0.047(3) 0.017(3) -0.023(4) C63 0.151(6) 0.216(8) 0.174(7) -0.114(6) 0.113(6) -0.087(6) C64 0.064(3) 0.105(4) 0.093(4) -0.043(3) 0.030(3) -0.022(3) O2 0.0470(14) 0.0519(14) 0.0626(16) -0.0081(11) 0.0121(12) 0.0031(11) C65 0.053(2) 0.086(3) 0.078(3) -0.017(2) 0.021(2) 0.003(2) C66 0.083(3) 0.107(4) 0.088(4) 0.006(3) 0.030(3) 0.036(3) C67 0.125(5) 0.074(3) 0.111(4) -0.023(3) 0.027(4) 0.015(3) C68 0.072(3) 0.067(3) 0.127(4) -0.036(3) 0.021(3) -0.003(2) O3 0.213(7) 0.223(7) 0.221(7) -0.016(6) 0.107(6) 0.056(6) C69 0.078(5) 0.149(7) 0.474(18) -0.120(9) 0.124(8) -0.026(5) C70 0.081(6) 0.317(16) 0.69(3) -0.31(2) 0.008(11) -0.003(8) C71 0.114(7) 0.234(12) 0.387(18) -0.109(12) 0.047(9) 0.057(8) C72 0.259(14) 0.198(10) 0.211(11) -0.076(9) 0.014(10) 0.081(10) O4 0.201(7) 0.234(8) 0.235(9) -0.008(6) -0.010(7) 0.125(6) C73 0.246(15) 0.67(4) 0.237(18) 0.09(2) 0.062(14) 0.26(2) C74 0.232(13) 0.205(11) 0.187(12) 0.050(10) -0.019(10) -0.027(10) C75 0.338(18) 0.238(12) 0.117(8) 0.017(8) 0.027(9) 0.152(13) C76 0.147(7) 0.117(6) 0.188(9) -0.026(6) -0.014(6) -0.034(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 Zn1 N1 1.929(3) . ? Zn1 N2 1.973(2) . ? Zn1 O1 2.146(2) . ? Zn1 P4 2.3272(9) . ? Zn2 N3 1.928(3) . ? Zn2 N4 1.972(2) . ? Zn2 O2 2.129(2) . ? Zn2 P2 2.3321(9) . ? P1 N1 1.671(3) . ? P1 C7 1.837(4) . ? P1 C1 1.843(4) . ? P2 N2 1.639(3) . ? P2 C25 1.822(3) . ? P2 C19 1.829(4) . ? P3 N3 1.670(3) . ? P3 C37 1.830(3) . ? P3 C31 1.842(4) . ? P4 N4 1.632(3) . ? P4 C49 1.827(3) . ? P4 C55 1.833(4) . ? N1 C13 1.394(4) . ? N2 C18 1.408(4) . ? N3 C43 1.408(4) . ? N4 C48 1.424(4) . ? C1 C6 1.366(6) . ? C1 C2 1.389(6) . ? C2 C3 1.380(7) . ? C3 C4 1.345(10) . ? C4 C5 1.358(9) . ? C5 C6 1.389(7) . ? C7 C12 1.385(5) . ? C7 C8 1.395(5) . ? C8 C9 1.385(6) . ? C9 C10 1.385(7) . ? C10 C11 1.365(6) . ? C11 C12 1.391(6) . ? C13 C14 1.388(4) . ? C13 C18 1.437(4) . ? C14 C15 1.373(5) . ? C15 C16 1.371(5) . ? C16 C17 1.397(5) . ? C17 C18 1.391(5) . ? C19 C20 1.360(6) . ? C19 C24 1.374(5) . ? C20 C21 1.389(7) . ? C21 C22 1.356(8) . ? C22 C23 1.352(8) . ? C23 C24 1.380(7) . ? C25 C26 1.380(5) . ? C25 C30 1.384(5) . ? C26 C27 1.387(6) . ? C27 C28 1.366(7) . ? C28 C29 1.378(7) . ? C29 C30 1.381(6) . ? C31 C36 1.372(6) . ? C31 C32 1.382(6) . ? C32 C33 1.389(7) . ? C33 C34 1.380(9) . ? C34 C35 1.316(9) . ? C35 C36 1.402(7) . ? C37 C42 1.385(5) . ? C37 C38 1.393(5) . ? C38 C39 1.392(6) . ? C39 C40 1.350(7) . ? C40 C41 1.376(7) . ? C41 C42 1.397(5) . ? C43 C44 1.392(5) . ? C43 C48 1.420(4) . ? C44 C45 1.389(5) . ? C45 C46 1.389(5) . ? C46 C47 1.399(5) . ? C47 C48 1.386(5) . ? C49 C50 1.378(5) . ? C49 C54 1.398(5) . ? C50 C51 1.394(5) . ? C51 C52 1.373(6) . ? C52 C53 1.386(7) . ? C53 C54 1.374(6) . ? C55 C56 1.357(5) . ? C55 C60 1.359(5) . ? C56 C57 1.387(6) . ? C57 C58 1.341(7) . ? C58 C59 1.320(7) . ? C59 C60 1.385(6) . ? O1 C64 1.425(4) . ? O1 C61 1.443(4) . ? C61 C62 1.440(6) . ? C62 C63 1.398(7) . ? C63 C64 1.460(6) . ? O2 C68 1.437(5) . ? O2 C65 1.442(4) . ? C65 C66 1.493(6) . ? C66 C67 1.457(7) . ? C67 C68 1.445(6) . ? O3 C72 1.377(8) . ? O3 C69 1.408(8) . ? C69 C70 1.338(9) . ? C70 C71 1.433(10) . ? C71 C72 1.299(9) . ? O4 C76 1.376(9) . ? O4 C73 1.412(12) . ? C73 C74 1.400(12) . ? C74 C75 1.390(11) . ? C75 C76 1.390(9) . ? 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 Zn1 N2 86.90(11) . . ? N1 Zn1 O1 105.16(11) . . ? N2 Zn1 O1 107.16(10) . . ? N1 Zn1 P4 132.47(8) . . ? N2 Zn1 P4 120.60(8) . . ? O1 Zn1 P4 102.29(7) . . ? N3 Zn2 N4 87.55(11) . . ? N3 Zn2 O2 105.51(11) . . ? N4 Zn2 O2 106.17(10) . . ? N3 Zn2 P2 130.96(8) . . ? N4 Zn2 P2 121.77(8) . . ? O2 Zn2 P2 102.48(7) . . ? N1 P1 C7 107.22(15) . . ? N1 P1 C1 108.95(17) . . ? C7 P1 C1 102.14(18) . . ? N2 P2 C25 111.75(15) . . ? N2 P2 C19 111.14(15) . . ? C25 P2 C19 104.82(16) . . ? N2 P2 Zn2 106.83(9) . . ? C25 P2 Zn2 112.06(11) . . ? C19 P2 Zn2 110.31(12) . . ? N3 P3 C37 108.27(15) . . ? N3 P3 C31 106.79(15) . . ? C37 P3 C31 101.53(16) . . ? N4 P4 C49 112.41(14) . . ? N4 P4 C55 111.10(15) . . ? C49 P4 C55 104.44(15) . . ? N4 P4 Zn1 106.93(10) . . ? C49 P4 Zn1 112.30(11) . . ? C55 P4 Zn1 109.71(11) . . ? C13 N1 P1 130.2(2) . . ? C13 N1 Zn1 110.9(2) . . ? P1 N1 Zn1 118.52(14) . . ? C18 N2 P2 126.8(2) . . ? C18 N2 Zn1 109.28(19) . . ? P2 N2 Zn1 123.59(14) . . ? C43 N3 P3 130.0(2) . . ? C43 N3 Zn2 110.32(19) . . ? P3 N3 Zn2 119.25(15) . . ? C48 N4 P4 126.3(2) . . ? C48 N4 Zn2 108.45(19) . . ? P4 N4 Zn2 123.87(14) . . ? C6 C1 C2 117.1(4) . . ? C6 C1 P1 127.3(4) . . ? C2 C1 P1 115.4(3) . . ? C3 C2 C1 122.1(5) . . ? C4 C3 C2 119.3(7) . . ? C3 C4 C5 120.2(6) . . ? C4 C5 C6 120.8(6) . . ? C1 C6 C5 120.5(6) . . ? C12 C7 C8 117.7(4) . . ? C12 C7 P1 122.0(3) . . ? C8 C7 P1 119.8(3) . . ? C9 C8 C7 121.5(4) . . ? C8 C9 C10 119.3(4) . . ? C11 C10 C9 120.4(5) . . ? C10 C11 C12 120.0(5) . . ? C7 C12 C11 121.2(4) . . ? C14 C13 N1 125.8(3) . . ? C14 C13 C18 117.5(3) . . ? N1 C13 C18 116.7(3) . . ? C15 C14 C13 122.4(4) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C17 118.7(3) . . ? C18 C17 C16 121.8(3) . . ? C17 C18 N2 125.1(3) . . ? C17 C18 C13 118.8(3) . . ? N2 C18 C13 116.2(3) . . ? C20 C19 C24 117.4(4) . . ? C20 C19 P2 117.1(3) . . ? C24 C19 P2 125.4(3) . . ? C19 C20 C21 122.7(5) . . ? C22 C21 C20 118.7(6) . . ? C23 C22 C21 119.6(5) . . ? C22 C23 C24 121.5(5) . . ? C19 C24 C23 120.1(5) . . ? C26 C25 C30 118.7(4) . . ? C26 C25 P2 121.5(3) . . ? C30 C25 P2 119.4(3) . . ? C25 C26 C27 120.8(4) . . ? C28 C27 C26 119.4(5) . . ? C27 C28 C29 120.9(5) . . ? C28 C29 C30 119.4(5) . . ? C29 C30 C25 120.8(4) . . ? C36 C31 C32 117.9(4) . . ? C36 C31 P3 126.1(3) . . ? C32 C31 P3 115.9(3) . . ? C31 C32 C33 120.8(5) . . ? C34 C33 C32 119.8(6) . . ? C35 C34 C33 119.9(6) . . ? C34 C35 C36 121.4(6) . . ? C31 C36 C35 120.4(5) . . ? C42 C37 C38 117.7(4) . . ? C42 C37 P3 123.4(3) . . ? C38 C37 P3 118.7(3) . . ? C39 C38 C37 120.9(4) . . ? C40 C39 C38 120.5(5) . . ? C39 C40 C41 120.2(5) . . ? C40 C41 C42 119.9(5) . . ? C37 C42 C41 120.9(4) . . ? C44 C43 N3 124.8(3) . . ? C44 C43 C48 118.3(3) . . ? N3 C43 C48 116.9(3) . . ? C45 C44 C43 121.8(3) . . ? C46 C45 C44 120.0(3) . . ? C45 C46 C47 118.8(4) . . ? C48 C47 C46 121.7(4) . . ? C47 C48 C43 119.4(3) . . ? C47 C48 N4 123.9(3) . . ? C43 C48 N4 116.7(3) . . ? C50 C49 C54 119.1(3) . . ? C50 C49 P4 122.1(3) . . ? C54 C49 P4 118.5(3) . . ? C49 C50 C51 120.5(4) . . ? C52 C51 C50 119.8(4) . . ? C51 C52 C53 120.0(4) . . ? C54 C53 C52 120.4(4) . . ? C53 C54 C49 120.1(4) . . ? C56 C55 C60 116.8(4) . . ? C56 C55 P4 126.0(3) . . ? C60 C55 P4 117.2(3) . . ? C55 C56 C57 120.1(5) . . ? C58 C57 C56 122.1(5) . . ? C59 C58 C57 118.2(4) . . ? C58 C59 C60 121.0(5) . . ? C55 C60 C59 121.8(4) . . ? C64 O1 C61 108.0(3) . . ? C64 O1 Zn1 119.6(2) . . ? C61 O1 Zn1 121.4(2) . . ? C62 C61 O1 107.0(3) . . ? C63 C62 C61 107.4(4) . . ? C62 C63 C64 107.6(4) . . ? O1 C64 C63 105.2(4) . . ? C68 O2 C65 108.0(3) . . ? C68 O2 Zn2 117.2(2) . . ? C65 O2 Zn2 118.7(2) . . ? O2 C65 C66 105.6(4) . . ? C67 C66 C65 103.6(4) . . ? C68 C67 C66 104.6(4) . . ? O2 C68 C67 106.6(4) . . ? C72 O3 C69 108.6(7) . . ? C70 C69 O3 102.1(7) . . ? C69 C70 C71 112.5(7) . . ? C72 C71 C70 104.2(8) . . ? C71 C72 O3 110.0(9) . . ? C76 O4 C73 108.8(8) . . ? C74 C73 O4 106.8(10) . . ? C75 C74 C73 106.5(10) . . ? C76 C75 C74 109.3(10) . . ? O4 C76 C75 106.9(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.456 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.090 data_c891_fin _database_code_depnum_ccdc_archive 'CCDC 671847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 N2 P2' _chemical_formula_weight 476.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 9.6450(11) _cell_length_b 10.4268(12) _cell_length_c 24.624(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.407(2) _cell_angle_gamma 90.00 _cell_volume 2469.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 955 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 27.22 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector (AXS Bruker)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15718 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.79 _reflns_number_total 5889 _reflns_number_gt 4537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0567P)^2^+0.2844P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5889 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.32963(4) 0.03485(3) 0.117345(14) 0.02848(10) Uani 1 1 d . . . P2 P 0.59996(4) -0.34730(4) 0.063309(15) 0.03076(10) Uani 1 1 d . . . N1 N 0.37869(13) 0.02441(12) 0.05267(5) 0.0312(3) Uani 1 1 d . . . N2 N 0.51631(13) -0.20557(12) 0.04812(5) 0.0305(3) Uani 1 1 d . . . C1 C 0.24095(14) 0.18992(13) 0.12002(6) 0.0292(3) Uani 1 1 d . . . C2 C 0.14589(17) 0.20416(16) 0.15957(6) 0.0378(3) Uani 1 1 d . . . C3 C 0.07619(18) 0.31894(17) 0.16540(8) 0.0455(4) Uani 1 1 d . . . C4 C 0.09726(18) 0.41936(17) 0.13112(8) 0.0462(4) Uani 1 1 d . . . C5 C 0.1890(2) 0.40670(17) 0.09127(8) 0.0458(4) Uani 1 1 d . . . C6 C 0.26132(17) 0.29266(15) 0.08605(7) 0.0383(3) Uani 1 1 d . . . C7 C 0.49171(15) 0.07293(13) 0.15768(6) 0.0304(3) Uani 1 1 d . . . C8 C 0.49475(18) 0.05121(17) 0.21379(7) 0.0426(4) Uani 1 1 d . . . C9 C 0.6124(2) 0.07808(19) 0.24738(7) 0.0509(4) Uani 1 1 d . . . C10 C 0.72989(19) 0.12406(18) 0.22572(8) 0.0470(4) Uani 1 1 d . . . C11 C 0.72893(18) 0.14446(18) 0.17032(7) 0.0456(4) Uani 1 1 d . . . C12 C 0.61104(16) 0.11872(16) 0.13648(7) 0.0375(3) Uani 1 1 d . . . C13 C 0.52024(15) -0.40245(14) 0.12434(6) 0.0306(3) Uani 1 1 d . . . C14 C 0.55707(18) -0.52400(15) 0.14436(6) 0.0373(3) Uani 1 1 d . . . C15 C 0.49725(19) -0.57358(16) 0.18905(7) 0.0422(4) Uani 1 1 d . . . C16 C 0.39904(18) -0.50376(17) 0.21416(7) 0.0425(4) Uani 1 1 d . . . C17 C 0.36035(18) -0.38407(18) 0.19460(7) 0.0432(4) Uani 1 1 d . . . C18 C 0.42034(17) -0.33346(16) 0.14987(6) 0.0384(3) Uani 1 1 d . . . C19 C 0.76262(15) -0.27919(14) 0.09348(6) 0.0311(3) Uani 1 1 d . . . C20 C 0.76949(17) -0.20491(17) 0.14036(7) 0.0403(4) Uani 1 1 d . . . C21 C 0.89453(19) -0.15401(18) 0.16123(8) 0.0487(4) Uani 1 1 d . . . C22 C 1.01425(18) -0.17692(18) 0.13570(8) 0.0487(4) Uani 1 1 d . . . C23 C 1.00910(18) -0.24890(19) 0.08894(8) 0.0495(4) Uani 1 1 d . . . C24 C 0.88411(17) -0.30021(17) 0.06769(7) 0.0411(4) Uani 1 1 d . . . C25 C 0.31591(15) -0.07691(14) 0.01978(5) 0.0292(3) Uani 1 1 d . . . C26 C 0.38478(14) -0.19511(14) 0.02015(5) 0.0280(3) Uani 1 1 d . . . C27 C 0.32193(16) -0.29803(16) -0.00847(6) 0.0349(3) Uani 1 1 d . . . C28 C 0.19492(17) -0.28140(18) -0.03803(7) 0.0417(4) Uani 1 1 d . . . C29 C 0.12958(17) -0.16425(19) -0.03994(7) 0.0447(4) Uani 1 1 d . . . C30 C 0.19020(16) -0.06178(18) -0.01076(6) 0.0392(4) Uani 1 1 d . . . H1N H 0.3917(19) 0.0902(19) 0.0352(7) 0.044(5) Uiso 1 1 d . . . H2N H 0.5374(17) -0.1416(16) 0.0664(6) 0.029(4) Uiso 1 1 d . . . H2 H 0.131(2) 0.1307(18) 0.1839(8) 0.051(5) Uiso 1 1 d . . . H3 H 0.012(2) 0.3280(19) 0.1941(8) 0.056(5) Uiso 1 1 d . . . H4 H 0.049(2) 0.496(2) 0.1360(8) 0.053(5) Uiso 1 1 d . . . H5 H 0.207(2) 0.4741(19) 0.0692(8) 0.054(5) Uiso 1 1 d . . . H6 H 0.327(2) 0.2852(18) 0.0578(8) 0.051(5) Uiso 1 1 d . . . H8 H 0.413(2) 0.0161(19) 0.2292(8) 0.060(6) Uiso 1 1 d . . . H9 H 0.613(2) 0.0633(18) 0.2873(8) 0.055(5) Uiso 1 1 d . . . H10 H 0.810(2) 0.1414(18) 0.2474(8) 0.056(6) Uiso 1 1 d . . . H11 H 0.808(2) 0.1766(18) 0.1552(8) 0.053(5) Uiso 1 1 d . . . H12 H 0.6098(18) 0.1324(16) 0.0978(7) 0.043(5) Uiso 1 1 d . . . H14 H 0.6236(19) -0.5733(18) 0.1272(7) 0.048(5) Uiso 1 1 d . . . H15 H 0.524(2) -0.653(2) 0.2013(8) 0.054(5) Uiso 1 1 d . . . H16 H 0.3549(19) -0.5366(17) 0.2441(8) 0.050(5) Uiso 1 1 d . . . H17 H 0.299(2) -0.3346(19) 0.2126(8) 0.054(5) Uiso 1 1 d . . . H18 H 0.3917(17) -0.2537(17) 0.1359(7) 0.039(4) Uiso 1 1 d . . . H20 H 0.690(2) -0.1928(18) 0.1600(8) 0.051(5) Uiso 1 1 d . . . H21 H 0.896(2) -0.1028(19) 0.1932(8) 0.058(6) Uiso 1 1 d . . . H22 H 1.098(2) -0.1414(18) 0.1512(8) 0.057(6) Uiso 1 1 d . . . H23 H 1.090(2) -0.264(2) 0.0719(8) 0.063(6) Uiso 1 1 d . . . H24 H 0.8783(19) -0.3530(17) 0.0358(8) 0.046(5) Uiso 1 1 d . . . H27 H 0.3660(18) -0.3807(17) -0.0077(7) 0.040(5) Uiso 1 1 d . . . H28 H 0.1548(19) -0.3531(17) -0.0570(7) 0.043(5) Uiso 1 1 d . . . H29 H 0.044(2) -0.1512(18) -0.0619(8) 0.053(5) Uiso 1 1 d . . . H30 H 0.1452(18) 0.0163(17) -0.0099(7) 0.040(5) 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 P1 0.03009(19) 0.02669(18) 0.02895(18) 0.00089(14) 0.00427(14) -0.00257(14) P2 0.0336(2) 0.02886(19) 0.02970(19) -0.00047(14) 0.00140(14) 0.00154(15) N1 0.0368(7) 0.0278(6) 0.0296(6) -0.0012(5) 0.0065(5) -0.0037(5) N2 0.0308(6) 0.0271(6) 0.0326(6) -0.0009(5) -0.0044(5) -0.0018(5) C1 0.0264(7) 0.0306(7) 0.0301(7) -0.0022(6) -0.0012(5) -0.0004(5) C2 0.0383(8) 0.0396(8) 0.0363(8) -0.0034(7) 0.0069(6) -0.0022(7) C3 0.0376(9) 0.0481(10) 0.0516(10) -0.0145(8) 0.0079(8) 0.0007(7) C4 0.0417(9) 0.0394(9) 0.0560(11) -0.0118(8) -0.0067(8) 0.0087(7) C5 0.0555(11) 0.0332(8) 0.0476(10) 0.0056(8) -0.0041(8) 0.0024(8) C6 0.0412(9) 0.0370(8) 0.0371(8) 0.0029(7) 0.0056(7) 0.0006(7) C7 0.0329(7) 0.0263(7) 0.0318(7) 0.0004(6) 0.0012(6) 0.0021(6) C8 0.0432(9) 0.0504(10) 0.0341(8) 0.0082(7) 0.0013(7) -0.0065(8) C9 0.0564(11) 0.0620(11) 0.0328(9) 0.0090(8) -0.0052(7) -0.0047(9) C10 0.0406(9) 0.0521(10) 0.0461(10) -0.0013(8) -0.0112(8) 0.0012(8) C11 0.0339(8) 0.0558(11) 0.0470(10) -0.0034(8) 0.0024(7) -0.0048(8) C12 0.0343(8) 0.0439(9) 0.0344(8) 0.0000(7) 0.0035(6) -0.0028(7) C13 0.0312(7) 0.0284(7) 0.0317(7) 0.0006(6) -0.0015(6) -0.0035(6) C14 0.0438(9) 0.0301(8) 0.0376(8) 0.0004(6) 0.0014(7) 0.0017(7) C15 0.0565(10) 0.0312(8) 0.0379(8) 0.0060(7) -0.0027(7) -0.0030(7) C16 0.0489(10) 0.0450(9) 0.0338(8) 0.0053(7) 0.0041(7) -0.0095(8) C17 0.0408(9) 0.0493(10) 0.0403(9) 0.0021(7) 0.0083(7) 0.0038(8) C18 0.0402(9) 0.0353(8) 0.0398(8) 0.0049(7) 0.0041(7) 0.0034(7) C19 0.0294(7) 0.0313(7) 0.0323(7) 0.0049(6) 0.0015(6) 0.0038(6) C20 0.0324(8) 0.0481(9) 0.0404(9) -0.0043(7) 0.0019(7) 0.0010(7) C21 0.0425(9) 0.0508(10) 0.0515(10) -0.0077(9) -0.0043(8) -0.0044(8) C22 0.0322(9) 0.0511(10) 0.0618(11) 0.0102(9) -0.0037(8) -0.0082(8) C23 0.0327(9) 0.0598(11) 0.0571(11) 0.0129(9) 0.0111(8) 0.0020(8) C24 0.0369(9) 0.0479(9) 0.0394(9) 0.0037(7) 0.0081(7) 0.0057(7) C25 0.0294(7) 0.0333(7) 0.0252(6) -0.0012(6) 0.0038(5) -0.0026(6) C26 0.0273(7) 0.0344(7) 0.0224(6) 0.0012(5) 0.0024(5) -0.0039(6) C27 0.0371(8) 0.0365(8) 0.0312(7) -0.0052(6) 0.0035(6) -0.0053(7) C28 0.0372(8) 0.0541(10) 0.0335(8) -0.0117(7) 0.0010(6) -0.0126(8) C29 0.0299(8) 0.0672(12) 0.0358(8) -0.0060(8) -0.0045(6) -0.0022(8) C30 0.0304(8) 0.0492(10) 0.0378(8) -0.0001(7) 0.0013(6) 0.0074(7) _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 N1 1.6994(12) . ? P1 C7 1.8300(15) . ? P1 C1 1.8327(15) . ? P2 N2 1.7112(13) . ? P2 C19 1.8271(15) . ? P2 C13 1.8325(15) . ? N1 C25 1.4364(18) . ? N2 C26 1.4005(18) . ? C1 C6 1.382(2) . ? C1 C2 1.396(2) . ? C2 C3 1.386(2) . ? C3 C4 1.370(3) . ? C4 C5 1.377(3) . ? C5 C6 1.390(2) . ? C7 C12 1.385(2) . ? C7 C8 1.398(2) . ? C8 C9 1.381(2) . ? C9 C10 1.375(3) . ? C10 C11 1.380(3) . ? C11 C12 1.383(2) . ? C13 C18 1.391(2) . ? C13 C14 1.396(2) . ? C14 C15 1.381(2) . ? C15 C16 1.378(3) . ? C16 C17 1.379(2) . ? C17 C18 1.387(2) . ? C19 C20 1.387(2) . ? C19 C24 1.393(2) . ? C20 C21 1.380(2) . ? C21 C22 1.377(3) . ? C22 C23 1.372(3) . ? C23 C24 1.384(3) . ? C25 C30 1.386(2) . ? C25 C26 1.400(2) . ? C26 C27 1.396(2) . ? C27 C28 1.387(2) . ? C28 C29 1.374(3) . ? C29 C30 1.391(2) . ? 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 P1 C7 103.58(6) . . ? N1 P1 C1 104.74(6) . . ? C7 P1 C1 99.83(6) . . ? N2 P2 C19 97.41(6) . . ? N2 P2 C13 103.28(6) . . ? C19 P2 C13 100.94(6) . . ? C25 N1 P1 116.09(10) . . ? C26 N2 P2 124.67(10) . . ? C6 C1 C2 118.12(14) . . ? C6 C1 P1 124.99(11) . . ? C2 C1 P1 116.89(11) . . ? C3 C2 C1 120.93(16) . . ? C4 C3 C2 120.02(16) . . ? C3 C4 C5 119.98(16) . . ? C4 C5 C6 120.18(17) . . ? C1 C6 C5 120.75(15) . . ? C12 C7 C8 118.25(14) . . ? C12 C7 P1 124.77(11) . . ? C8 C7 P1 116.96(12) . . ? C9 C8 C7 120.86(16) . . ? C10 C9 C8 120.14(16) . . ? C9 C10 C11 119.61(17) . . ? C10 C11 C12 120.56(17) . . ? C11 C12 C7 120.55(15) . . ? C18 C13 C14 118.44(14) . . ? C18 C13 P2 123.87(11) . . ? C14 C13 P2 117.59(11) . . ? C15 C14 C13 120.70(15) . . ? C16 C15 C14 120.21(16) . . ? C15 C16 C17 119.89(16) . . ? C16 C17 C18 120.22(16) . . ? C17 C18 C13 120.53(15) . . ? C20 C19 C24 118.64(15) . . ? C20 C19 P2 122.68(11) . . ? C24 C19 P2 118.66(12) . . ? C21 C20 C19 120.59(16) . . ? C22 C21 C20 120.18(18) . . ? C23 C22 C21 120.02(17) . . ? C22 C23 C24 120.19(17) . . ? C23 C24 C19 120.37(17) . . ? C30 C25 C26 119.92(13) . . ? C30 C25 N1 122.39(14) . . ? C26 C25 N1 117.68(12) . . ? C27 C26 C25 119.07(13) . . ? C27 C26 N2 122.00(14) . . ? C25 C26 N2 118.90(12) . . ? C28 C27 C26 120.03(15) . . ? C29 C28 C27 120.90(15) . . ? C28 C29 C30 119.46(15) . . ? C25 C30 C29 120.56(16) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.79 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.289 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.044 data_c936_fin _database_code_depnum_ccdc_archive 'CCDC 671848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H60 N6 Ni2 P4' _chemical_formula_weight 1178.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5087(9) _cell_length_b 12.1620(12) _cell_length_c 13.8429(13) _cell_angle_alpha 101.889(2) _cell_angle_beta 100.363(2) _cell_angle_gamma 107.307(2) _cell_volume 1444.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.36 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'ccd diffractometer (AXS Bruker)' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15714 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 29.02 _reflns_number_total 6949 _reflns_number_gt 4687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0540P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6949 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.08808(4) 0.02608(3) 0.08263(2) 0.02636(10) Uani 1 1 d . . . P1 P 0.23212(7) 0.06633(5) 0.23325(5) 0.02691(15) Uani 1 1 d . . . P2 P 0.00639(7) 0.16181(5) -0.01843(5) 0.02657(15) Uani 1 1 d . . . N1 N 0.3749(2) 0.19723(18) 0.25159(17) 0.0301(5) Uani 1 1 d . . . N2 N 0.1405(2) 0.19006(17) 0.08556(16) 0.0304(5) Uani 1 1 d . . . N3 N 0.7091(4) 0.2780(3) 0.3876(3) 0.0826(11) Uani 1 1 d . . . C1 C 0.3451(3) -0.0219(2) 0.2717(2) 0.0316(6) Uani 1 1 d . . . C2 C 0.3483(3) -0.0598(2) 0.3597(2) 0.0436(7) Uani 1 1 d . . . H2 H 0.2928 -0.0372 0.4051 0.052 Uiso 1 1 calc R . . C3 C 0.4339(4) -0.1315(3) 0.3810(3) 0.0591(10) Uani 1 1 d . . . H3 H 0.4350 -0.1579 0.4403 0.071 Uiso 1 1 calc R . . C4 C 0.5163(4) -0.1633(3) 0.3155(3) 0.0624(10) Uani 1 1 d . . . H4 H 0.5743 -0.2110 0.3304 0.075 Uiso 1 1 calc R . . C5 C 0.5150(3) -0.1261(3) 0.2281(3) 0.0553(9) Uani 1 1 d . . . H5 H 0.5724 -0.1480 0.1838 0.066 Uiso 1 1 calc R . . C6 C 0.4289(3) -0.0565(2) 0.2058(2) 0.0420(7) Uani 1 1 d . . . H6 H 0.4267 -0.0322 0.1455 0.050 Uiso 1 1 calc R . . C7 C 0.1397(3) 0.0931(2) 0.33615(19) 0.0312(6) Uani 1 1 d . . . C8 C 0.2201(3) 0.1768(3) 0.4300(2) 0.0414(7) Uani 1 1 d . . . H8 H 0.3255 0.2171 0.4427 0.050 Uiso 1 1 calc R . . C9 C 0.1459(4) 0.2009(3) 0.5045(2) 0.0501(8) Uani 1 1 d . . . H9 H 0.2012 0.2563 0.5681 0.060 Uiso 1 1 calc R . . C10 C -0.0084(4) 0.1440(3) 0.4862(2) 0.0552(9) Uani 1 1 d . . . H10 H -0.0585 0.1614 0.5369 0.066 Uiso 1 1 calc R . . C11 C -0.0895(4) 0.0622(3) 0.3941(3) 0.0544(8) Uani 1 1 d . . . H11 H -0.1951 0.0234 0.3818 0.065 Uiso 1 1 calc R . . C12 C -0.0160(3) 0.0366(2) 0.3191(2) 0.0419(7) Uani 1 1 d . . . H12 H -0.0722 -0.0197 0.2561 0.050 Uiso 1 1 calc R . . C13 C 0.3467(3) 0.3022(2) 0.23934(19) 0.0287(5) Uani 1 1 d . . . C14 C 0.2332(3) 0.2993(2) 0.15726(19) 0.0286(5) Uani 1 1 d . . . C15 C 0.2199(3) 0.4092(2) 0.1492(2) 0.0330(6) Uani 1 1 d . . . H15 H 0.1453 0.4098 0.0947 0.040 Uiso 1 1 calc R . . C16 C 0.3142(3) 0.5174(2) 0.2197(2) 0.0381(6) Uani 1 1 d . . . H16 H 0.3034 0.5899 0.2123 0.046 Uiso 1 1 calc R . . C17 C 0.4230(3) 0.5178(2) 0.2999(2) 0.0400(7) Uani 1 1 d . . . H17 H 0.4861 0.5904 0.3480 0.048 Uiso 1 1 calc R . . C18 C 0.4394(3) 0.4115(2) 0.3097(2) 0.0362(6) Uani 1 1 d . . . H18 H 0.5143 0.4124 0.3648 0.043 Uiso 1 1 calc R . . C19 C -0.1397(3) 0.2216(2) 0.01518(19) 0.0300(6) Uani 1 1 d . . . C20 C -0.2428(3) 0.1546(3) 0.0595(2) 0.0437(7) Uani 1 1 d . . . H20 H -0.2361 0.0818 0.0690 0.052 Uiso 1 1 calc R . . C21 C -0.3551(4) 0.1941(3) 0.0897(3) 0.0570(9) Uani 1 1 d . . . H21 H -0.4235 0.1482 0.1197 0.068 Uiso 1 1 calc R . . C22 C -0.3668(4) 0.3005(3) 0.0759(2) 0.0530(8) Uani 1 1 d . . . H22 H -0.4427 0.3271 0.0967 0.064 Uiso 1 1 calc R . . C23 C -0.2681(3) 0.3670(3) 0.0321(2) 0.0463(7) Uani 1 1 d . . . H23 H -0.2765 0.4393 0.0225 0.056 Uiso 1 1 calc R . . C24 C -0.1553(3) 0.3286(2) 0.0017(2) 0.0348(6) Uani 1 1 d . . . H24 H -0.0881 0.3753 -0.0285 0.042 Uiso 1 1 calc R . . C25 C 0.0883(3) 0.2497(2) -0.10094(19) 0.0290(5) Uani 1 1 d . . . C26 C 0.2455(3) 0.2907(2) -0.0875(2) 0.0379(6) Uani 1 1 d . . . H26 H 0.3086 0.2752 -0.0354 0.045 Uiso 1 1 calc R . . C27 C 0.3096(4) 0.3541(3) -0.1506(2) 0.0488(8) Uani 1 1 d . . . H27 H 0.4159 0.3813 -0.1411 0.059 Uiso 1 1 calc R . . C28 C 0.2191(4) 0.3775(3) -0.2269(2) 0.0512(8) Uani 1 1 d . . . H28 H 0.2634 0.4221 -0.2685 0.061 Uiso 1 1 calc R . . C29 C 0.0634(4) 0.3354(2) -0.2425(2) 0.0469(8) Uani 1 1 d . . . H29 H 0.0011 0.3502 -0.2955 0.056 Uiso 1 1 calc R . . C30 C -0.0020(3) 0.2711(2) -0.17995(19) 0.0356(6) Uani 1 1 d . . . H30 H -0.1086 0.2419 -0.1915 0.043 Uiso 1 1 calc R . . C31 C 1.0790(5) 0.4450(4) 0.3963(3) 0.0851(13) Uani 1 1 d . . . H31A H 1.0511 0.5160 0.4112 0.128 Uiso 1 1 calc R . . H31B H 1.1680 0.4621 0.3693 0.128 Uiso 1 1 calc R . . H31C H 1.1019 0.4215 0.4585 0.128 Uiso 1 1 calc R . . C32 C 0.9491(4) 0.3451(4) 0.3191(3) 0.0760(11) Uani 1 1 d . . . H32A H 0.9230 0.3713 0.2580 0.091 Uiso 1 1 calc R . . H32B H 0.9820 0.2766 0.2991 0.091 Uiso 1 1 calc R . . C33 C 0.8128(5) 0.3062(3) 0.3559(3) 0.0697(11) Uani 1 1 d . . . H1N H 0.451(3) 0.212(2) 0.297(2) 0.041(9) 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 Ni1 0.03067(19) 0.02207(16) 0.02496(18) 0.00645(12) 0.00364(13) 0.00933(13) P1 0.0265(3) 0.0266(3) 0.0269(4) 0.0079(3) 0.0044(3) 0.0092(3) P2 0.0301(4) 0.0231(3) 0.0265(3) 0.0072(2) 0.0059(3) 0.0097(3) N1 0.0235(12) 0.0310(11) 0.0321(12) 0.0087(9) 0.0015(10) 0.0075(9) N2 0.0346(12) 0.0212(10) 0.0314(12) 0.0061(8) 0.0014(9) 0.0091(9) N3 0.0430(19) 0.087(2) 0.101(3) 0.011(2) -0.0028(19) 0.0217(17) C1 0.0268(14) 0.0273(13) 0.0341(15) 0.0064(11) -0.0018(11) 0.0072(10) C2 0.0470(18) 0.0380(16) 0.0430(18) 0.0153(13) 0.0018(14) 0.0140(13) C3 0.066(2) 0.0424(18) 0.055(2) 0.0173(16) -0.0161(18) 0.0149(16) C4 0.053(2) 0.0343(17) 0.086(3) 0.0104(17) -0.0158(19) 0.0184(15) C5 0.0422(18) 0.0376(16) 0.076(2) 0.0004(16) 0.0007(17) 0.0188(14) C6 0.0378(16) 0.0357(15) 0.0483(18) 0.0061(13) 0.0040(14) 0.0149(12) C7 0.0331(14) 0.0326(13) 0.0284(14) 0.0093(11) 0.0070(11) 0.0119(11) C8 0.0338(16) 0.0501(17) 0.0336(16) 0.0063(13) 0.0057(12) 0.0104(13) C9 0.053(2) 0.060(2) 0.0321(17) 0.0040(14) 0.0116(14) 0.0187(16) C10 0.064(2) 0.064(2) 0.047(2) 0.0147(16) 0.0315(17) 0.0257(18) C11 0.0384(18) 0.058(2) 0.062(2) 0.0109(16) 0.0248(16) 0.0073(15) C12 0.0348(16) 0.0391(16) 0.0438(17) 0.0063(13) 0.0090(13) 0.0055(12) C13 0.0267(13) 0.0283(13) 0.0320(14) 0.0083(10) 0.0114(11) 0.0084(10) C14 0.0275(13) 0.0272(13) 0.0306(14) 0.0076(10) 0.0111(11) 0.0070(10) C15 0.0348(15) 0.0269(13) 0.0339(15) 0.0072(11) 0.0057(12) 0.0083(11) C16 0.0403(16) 0.0237(13) 0.0474(17) 0.0095(12) 0.0104(13) 0.0077(11) C17 0.0361(16) 0.0269(14) 0.0437(17) 0.0018(12) 0.0064(13) -0.0004(11) C18 0.0310(15) 0.0320(14) 0.0375(16) 0.0056(11) 0.0044(12) 0.0048(11) C19 0.0314(14) 0.0289(13) 0.0270(14) 0.0043(10) 0.0066(11) 0.0097(11) C20 0.0467(18) 0.0391(16) 0.0454(18) 0.0119(13) 0.0185(14) 0.0111(13) C21 0.0442(19) 0.066(2) 0.057(2) 0.0101(17) 0.0295(17) 0.0087(16) C22 0.0398(18) 0.066(2) 0.051(2) 0.0003(16) 0.0154(15) 0.0238(16) C23 0.0476(18) 0.0491(18) 0.0452(18) 0.0048(14) 0.0106(15) 0.0277(15) C24 0.0374(15) 0.0327(14) 0.0344(15) 0.0067(11) 0.0101(12) 0.0137(11) C25 0.0369(15) 0.0229(12) 0.0280(14) 0.0043(10) 0.0124(11) 0.0110(10) C26 0.0392(16) 0.0375(15) 0.0431(17) 0.0103(12) 0.0170(13) 0.0187(12) C27 0.0474(19) 0.0420(17) 0.059(2) 0.0064(15) 0.0319(17) 0.0123(14) C28 0.074(2) 0.0389(17) 0.0449(19) 0.0126(14) 0.0364(18) 0.0134(16) C29 0.071(2) 0.0373(16) 0.0313(16) 0.0125(12) 0.0144(15) 0.0152(15) C30 0.0431(16) 0.0287(13) 0.0315(15) 0.0068(11) 0.0094(12) 0.0086(12) C31 0.072(3) 0.098(3) 0.088(3) 0.029(3) 0.039(2) 0.020(2) C32 0.072(3) 0.085(3) 0.067(3) 0.010(2) 0.016(2) 0.030(2) C33 0.049(2) 0.071(3) 0.075(3) 0.005(2) -0.006(2) 0.022(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 Ni1 N2 1.8961(19) . ? Ni1 P2 2.1150(7) 2 ? Ni1 P1 2.1485(7) . ? Ni1 Ni1 2.4152(6) 2 ? Ni1 P2 2.5708(7) . ? P1 N1 1.693(2) . ? P1 C1 1.818(2) . ? P1 C7 1.827(3) . ? P2 N2 1.640(2) . ? P2 C19 1.835(3) . ? P2 C25 1.839(3) . ? P2 Ni1 2.1150(7) 2 ? N1 C13 1.417(3) . ? N2 C14 1.404(3) . ? N3 C33 1.141(5) . ? C1 C2 1.387(4) . ? C1 C6 1.396(4) . ? C2 C3 1.397(4) . ? C3 C4 1.370(5) . ? C4 C5 1.374(5) . ? C5 C6 1.383(4) . ? C7 C12 1.386(4) . ? C7 C8 1.394(4) . ? C8 C9 1.381(4) . ? C9 C10 1.373(4) . ? C10 C11 1.370(4) . ? C11 C12 1.386(4) . ? C13 C18 1.397(3) . ? C13 C14 1.406(3) . ? C14 C15 1.405(3) . ? C15 C16 1.394(3) . ? C16 C17 1.373(4) . ? C17 C18 1.379(4) . ? C19 C20 1.396(4) . ? C19 C24 1.398(3) . ? C20 C21 1.390(4) . ? C21 C22 1.379(5) . ? C22 C23 1.363(4) . ? C23 C24 1.388(4) . ? C25 C30 1.383(4) . ? C25 C26 1.392(4) . ? C26 C27 1.385(4) . ? C27 C28 1.371(4) . ? C28 C29 1.374(4) . ? C29 C30 1.389(4) . ? C31 C32 1.497(5) . ? C32 C33 1.460(6) . ? 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 N2 Ni1 P2 157.26(7) . 2 ? N2 Ni1 P1 92.81(7) . . ? P2 Ni1 P1 109.45(3) 2 . ? N2 Ni1 Ni1 89.27(6) . 2 ? P2 Ni1 Ni1 68.78(2) 2 2 ? P1 Ni1 Ni1 176.14(3) . 2 ? N2 Ni1 P2 39.59(6) . . ? P2 Ni1 P2 118.86(2) 2 . ? P1 Ni1 P2 131.56(3) . . ? Ni1 Ni1 P2 50.078(18) 2 . ? N1 P1 C1 99.11(11) . . ? N1 P1 C7 105.38(11) . . ? C1 P1 C7 104.53(12) . . ? N1 P1 Ni1 106.62(8) . . ? C1 P1 Ni1 124.46(9) . . ? C7 P1 Ni1 114.30(9) . . ? N2 P2 C19 109.01(11) . . ? N2 P2 C25 108.26(11) . . ? C19 P2 C25 104.48(11) . . ? N2 P2 Ni1 108.03(7) . 2 ? C19 P2 Ni1 110.69(8) . 2 ? C25 P2 Ni1 116.16(8) . 2 ? N2 P2 Ni1 47.44(7) . . ? C19 P2 Ni1 118.41(9) . . ? C25 P2 Ni1 135.23(8) . . ? Ni1 P2 Ni1 61.14(2) 2 . ? C13 N1 P1 122.23(18) . . ? C14 N2 P2 130.47(17) . . ? C14 N2 Ni1 135.35(18) . . ? P2 N2 Ni1 92.97(9) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 P1 124.1(2) . . ? C6 C1 P1 117.1(2) . . ? C1 C2 C3 120.1(3) . . ? C4 C3 C2 119.9(3) . . ? C3 C4 C5 120.8(3) . . ? C4 C5 C6 119.6(3) . . ? C5 C6 C1 120.8(3) . . ? C12 C7 C8 118.5(2) . . ? C12 C7 P1 120.0(2) . . ? C8 C7 P1 121.4(2) . . ? C9 C8 C7 120.4(3) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 120.0(3) . . ? C7 C12 C11 120.7(3) . . ? C18 C13 C14 120.1(2) . . ? C18 C13 N1 118.0(2) . . ? C14 C13 N1 121.9(2) . . ? N2 C14 C15 122.2(2) . . ? N2 C14 C13 120.4(2) . . ? C15 C14 C13 117.4(2) . . ? C16 C15 C14 121.8(3) . . ? C17 C16 C15 119.7(2) . . ? C16 C17 C18 119.9(2) . . ? C17 C18 C13 121.1(3) . . ? C20 C19 C24 117.4(2) . . ? C20 C19 P2 116.7(2) . . ? C24 C19 P2 125.9(2) . . ? C21 C20 C19 120.8(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 120.4(3) . . ? C23 C24 C19 121.2(3) . . ? C30 C25 C26 118.6(2) . . ? C30 C25 P2 122.1(2) . . ? C26 C25 P2 119.3(2) . . ? C27 C26 C25 120.3(3) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 119.8(3) . . ? C28 C29 C30 120.2(3) . . ? C25 C30 C29 120.6(3) . . ? C33 C32 C31 113.6(3) . . ? N3 C33 C32 177.8(4) . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.429 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.147 # Attachment 'ccdc_671849_new.cif' data_c1075fin _database_code_depnum_ccdc_archive 'CCDC 671849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H66 N2 O2 P2' _chemical_formula_weight 788.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.740(2) _cell_length_b 13.040(3) _cell_length_c 16.010(3) _cell_angle_alpha 113.30(3) _cell_angle_beta 91.60(3) _cell_angle_gamma 92.20(3) _cell_volume 2246.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 217(2) _cell_measurement_reflns_used 956 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 217(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 'CCD area detector (AXS Bruker)' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11481 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.68 _reflns_number_total 9257 _reflns_number_gt 6832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.1025P)^2^+0.0824P] 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 9257 _refine_ls_number_parameters 725 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 P1 P 1.23459(4) 0.81208(4) 0.37397(3) 0.02906(14) Uani 1 1 d . . . P2 P 0.82915(4) 0.45295(4) 0.29579(3) 0.02978(14) Uani 1 1 d . . . O1 O 0.8647(6) 0.8348(7) 0.0928(3) 0.284(4) Uani 1 1 d . . . O2 O 0.16921(14) 0.46884(13) 0.23147(11) 0.0477(4) Uani 1 1 d . . . N1 N 1.12348(13) 0.71443(13) 0.34311(11) 0.0307(4) Uani 1 1 d . . . N2 N 0.93617(15) 0.54837(13) 0.30252(12) 0.0336(4) Uani 1 1 d . . . C1 C 1.27934(16) 0.84101(16) 0.27546(13) 0.0319(4) Uani 1 1 d . . . C2 C 1.22393(17) 0.80294(17) 0.18801(14) 0.0357(4) Uani 1 1 d . . . C3 C 1.2575(2) 0.8512(2) 0.12804(16) 0.0461(5) Uani 1 1 d . . . C4 C 1.3440(2) 0.9332(2) 0.14881(17) 0.0507(6) Uani 1 1 d . . . C5 C 1.3991(2) 0.96833(19) 0.23421(17) 0.0461(5) Uani 1 1 d . . . C6 C 1.36808(18) 0.92549(17) 0.29762(15) 0.0378(5) Uani 1 1 d . . . C7 C 1.1297(2) 0.7117(2) 0.15455(17) 0.0478(6) Uani 1 1 d . . . C8 C 1.3779(3) 0.9836(3) 0.0823(2) 0.0794(9) Uani 1 1 d . . . H8A H 1.3714 0.9263 0.0209 0.119 Uiso 1 1 calc R . . H8B H 1.4561 1.0139 0.0965 0.119 Uiso 1 1 calc R . . H8C H 1.3279 1.0430 0.0870 0.119 Uiso 1 1 calc R . . C9 C 1.4305(3) 0.9719(2) 0.3901(2) 0.0524(7) Uani 1 1 d . . . C10 C 1.34886(15) 0.73652(15) 0.40221(13) 0.0284(4) Uani 1 1 d . . . C11 C 1.36435(16) 0.76160(15) 0.49625(13) 0.0308(4) Uani 1 1 d . . . C12 C 1.45320(18) 0.71658(17) 0.52741(14) 0.0353(4) Uani 1 1 d . . . C13 C 1.52771(16) 0.64534(17) 0.46876(14) 0.0352(4) Uani 1 1 d . . . C14 C 1.51028(17) 0.61913(17) 0.37652(14) 0.0340(4) Uani 1 1 d . . . C15 C 1.42395(16) 0.66432(16) 0.34196(13) 0.0316(4) Uani 1 1 d . . . C16 C 1.2888(2) 0.8388(2) 0.56602(15) 0.0416(5) Uani 1 1 d . . . C17 C 1.6238(2) 0.5985(3) 0.5049(2) 0.0545(7) Uani 1 1 d . . . C18 C 1.4182(2) 0.6338(2) 0.24085(15) 0.0466(6) Uani 1 1 d . . . C19 C 1.00961(15) 0.74502(15) 0.35854(12) 0.0285(4) Uani 1 1 d . . . C20 C 0.98395(18) 0.85774(17) 0.39565(16) 0.0396(5) Uani 1 1 d . . . C21 C 0.8740(2) 0.89159(18) 0.41481(17) 0.0455(5) Uani 1 1 d . . . C22 C 0.7852(2) 0.81261(19) 0.39431(17) 0.0465(6) Uani 1 1 d . . . C23 C 0.80778(18) 0.70011(18) 0.35432(16) 0.0422(5) Uani 1 1 d . . . C24 C 0.91853(16) 0.66374(15) 0.33794(13) 0.0305(4) Uani 1 1 d . . . C25 C 0.74919(16) 0.40676(16) 0.18491(13) 0.0317(4) Uani 1 1 d . . . C26 C 0.76197(19) 0.44933(17) 0.11687(14) 0.0375(5) Uani 1 1 d . . . C27 C 0.6772(2) 0.4214(2) 0.04727(15) 0.0452(5) Uani 1 1 d . . . C28 C 0.5822(2) 0.3514(2) 0.04026(15) 0.0461(6) Uani 1 1 d . . . C29 C 0.57342(19) 0.3073(2) 0.10548(15) 0.0409(5) Uani 1 1 d . . . C30 C 0.65358(17) 0.33490(17) 0.17800(13) 0.0342(4) Uani 1 1 d . . . C31 C 0.8641(3) 0.5207(2) 0.11198(19) 0.0532(6) Uani 1 1 d . . . C32 C 0.4932(3) 0.3226(4) -0.0367(2) 0.0688(9) Uani 1 1 d . . . C33 C 0.6341(2) 0.2847(2) 0.24726(17) 0.0446(5) Uani 1 1 d . . . C34 C 0.91369(16) 0.33699(15) 0.29583(13) 0.0306(4) Uani 1 1 d . . . C35 C 0.95801(18) 0.25149(17) 0.22013(14) 0.0361(4) Uani 1 1 d . . . C36 C 1.0261(2) 0.17437(18) 0.23499(16) 0.0426(5) Uani 1 1 d . . . C37 C 1.05268(19) 0.17848(18) 0.32149(16) 0.0429(5) Uani 1 1 d . . . C38 C 1.00542(18) 0.25992(18) 0.39457(15) 0.0386(5) Uani 1 1 d . . . C39 C 0.93431(16) 0.33767(16) 0.38383(13) 0.0327(4) Uani 1 1 d . . . C40 C 0.9348(2) 0.2374(2) 0.12295(16) 0.0491(6) Uani 1 1 d . . . C41 C 1.1315(3) 0.0965(3) 0.3348(3) 0.0676(8) Uani 1 1 d . . . C42 C 0.8796(2) 0.4179(2) 0.46728(15) 0.0409(5) Uani 1 1 d . . . C43 C 0.8209(7) 0.9148(6) 0.0686(4) 0.162(3) Uani 1 1 d . . . H43A H 0.7834 0.8804 0.0077 0.195 Uiso 1 1 calc R . . H43B H 0.8820 0.9677 0.0677 0.195 Uiso 1 1 calc R . . C44 C 0.7429(6) 0.9696(5) 0.1320(5) 0.163(2) Uani 1 1 d . . . H44A H 0.6665 0.9586 0.1026 0.195 Uiso 1 1 calc R . . H44B H 0.7635 1.0500 0.1595 0.195 Uiso 1 1 calc R . . C45 C 0.7436(6) 0.9250(6) 0.2008(3) 0.176(3) Uani 1 1 d . . . H45A H 0.7732 0.9817 0.2594 0.211 Uiso 1 1 calc R . . H45B H 0.6664 0.8995 0.2082 0.211 Uiso 1 1 calc R . . C46 C 0.8160(6) 0.8339(7) 0.1697(4) 0.212(4) Uani 1 1 d . . . H46A H 0.8751 0.8421 0.2166 0.255 Uiso 1 1 calc R . . H46B H 0.7717 0.7632 0.1554 0.255 Uiso 1 1 calc R . . C47 C 0.2018(3) 0.4019(2) 0.14038(18) 0.0520(6) Uani 1 1 d . . . C48 C 0.2520(3) 0.2993(2) 0.14511(19) 0.0556(6) Uani 1 1 d . . . C49 C 0.3042(2) 0.3435(2) 0.24165(19) 0.0547(6) Uani 1 1 d . . . C50 C 0.2218(2) 0.4288(2) 0.29503(17) 0.0456(5) Uani 1 1 d . . . H1N1 H 1.1335(19) 0.643(2) 0.3089(15) 0.040(6) Uiso 1 1 d . . . H1N2 H 0.995(2) 0.524(2) 0.2756(16) 0.043(7) Uiso 1 1 d . . . H3 H 1.218(2) 0.824(2) 0.0687(18) 0.057(7) Uiso 1 1 d . . . H5 H 1.459(2) 1.027(2) 0.2509(18) 0.064(8) Uiso 1 1 d . . . H7A H 1.110(2) 0.692(2) 0.0899(17) 0.047(6) Uiso 1 1 d . . . H7B H 1.061(2) 0.730(2) 0.1876(17) 0.047(7) Uiso 1 1 d . . . H7C H 1.155(2) 0.638(2) 0.1557(17) 0.054(7) Uiso 1 1 d . . . H9A H 1.481(2) 1.038(2) 0.3975(17) 0.058(7) Uiso 1 1 d . . . H9B H 1.481(3) 0.924(3) 0.398(2) 0.076(9) Uiso 1 1 d . . . H9C H 1.375(3) 0.991(3) 0.437(3) 0.103(13) Uiso 1 1 d . . . H12 H 1.459(2) 0.733(2) 0.5887(17) 0.047(7) Uiso 1 1 d . . . H14 H 1.5616(18) 0.5634(18) 0.3327(14) 0.034(5) Uiso 1 1 d . . . H16A H 1.209(2) 0.818(2) 0.5551(17) 0.054(7) Uiso 1 1 d . . . H16B H 1.302(2) 0.915(2) 0.5697(17) 0.056(7) Uiso 1 1 d . . . H16C H 1.299(2) 0.836(2) 0.629(2) 0.070(8) Uiso 1 1 d . . . H17A H 1.684(4) 0.645(4) 0.520(3) 0.110(14) Uiso 1 1 d . . . H17B H 1.600(2) 0.569(3) 0.551(2) 0.072(9) Uiso 1 1 d . . . H17C H 1.657(4) 0.540(4) 0.460(3) 0.123(15) Uiso 1 1 d . . . H18A H 1.343(3) 0.624(2) 0.2163(19) 0.063(8) Uiso 1 1 d . . . H18B H 1.463(2) 0.566(2) 0.2095(16) 0.046(6) Uiso 1 1 d . . . H18C H 1.455(2) 0.688(3) 0.2260(19) 0.064(9) Uiso 1 1 d . . . H20 H 1.043(2) 0.914(3) 0.408(2) 0.070(8) Uiso 1 1 d . . . H21 H 0.863(2) 0.976(2) 0.4486(18) 0.062(8) Uiso 1 1 d . . . H22 H 0.709(2) 0.833(2) 0.4098(16) 0.052(7) Uiso 1 1 d . . . H23 H 0.741(2) 0.646(2) 0.3420(18) 0.061(8) Uiso 1 1 d . . . H27 H 0.691(2) 0.445(2) 0.0019(18) 0.051(7) Uiso 1 1 d . . . H29 H 0.509(2) 0.262(2) 0.1003(16) 0.044(6) Uiso 1 1 d . . . H31A H 0.867(2) 0.593(2) 0.1626(18) 0.053(7) Uiso 1 1 d . . . H31B H 0.858(2) 0.535(3) 0.059(2) 0.073(9) Uiso 1 1 d . . . H31C H 0.939(3) 0.482(3) 0.113(2) 0.085(10) Uiso 1 1 d . . . H32A H 0.518(3) 0.267(3) -0.096(3) 0.094(11) Uiso 1 1 d . . . H32B H 0.431(4) 0.292(4) -0.022(3) 0.127(17) Uiso 1 1 d . . . H32C H 0.484(3) 0.386(3) -0.052(3) 0.099(12) Uiso 1 1 d . . . H33A H 0.632(2) 0.343(2) 0.308(2) 0.063(8) Uiso 1 1 d . . . H33B H 0.695(3) 0.230(3) 0.245(2) 0.085(10) Uiso 1 1 d . . . H33C H 0.560(2) 0.234(2) 0.2352(19) 0.066(8) Uiso 1 1 d . . . H36 H 1.055(2) 0.119(2) 0.1812(17) 0.046(6) Uiso 1 1 d . . . H38 H 1.023(2) 0.263(2) 0.4531(17) 0.049(7) Uiso 1 1 d . . . H40A H 0.945(2) 0.304(2) 0.1179(17) 0.049(7) Uiso 1 1 d . . . H40B H 0.853(2) 0.210(2) 0.1055(16) 0.046(6) Uiso 1 1 d . . . H40C H 0.984(2) 0.181(2) 0.084(2) 0.066(8) Uiso 1 1 d . . . H41A H 1.140(3) 0.106(3) 0.393(3) 0.102(13) Uiso 1 1 d . . . H41B H 1.098(4) 0.019(4) 0.301(3) 0.126(15) Uiso 1 1 d . . . H41C H 1.199(4) 0.088(4) 0.307(3) 0.130(17) Uiso 1 1 d . . . H42A H 0.800(2) 0.400(2) 0.4610(16) 0.046(6) Uiso 1 1 d . . . H42B H 0.912(2) 0.413(2) 0.5208(16) 0.044(6) Uiso 1 1 d . . . H42C H 0.892(2) 0.496(3) 0.4755(18) 0.063(8) Uiso 1 1 d . . . H47A H 0.274(3) 0.446(3) 0.125(2) 0.076(9) Uiso 1 1 d . . . H47B H 0.142(2) 0.385(2) 0.0992(18) 0.053(7) Uiso 1 1 d . . . H48A H 0.305(2) 0.266(2) 0.0972(19) 0.061(8) Uiso 1 1 d . . . H48B H 0.196(3) 0.239(3) 0.138(2) 0.071(9) Uiso 1 1 d . . . H49A H 0.390(3) 0.379(2) 0.2443(19) 0.067(8) Uiso 1 1 d . . . H49B H 0.305(3) 0.284(3) 0.264(2) 0.080(10) Uiso 1 1 d . . . H50A H 0.256(2) 0.490(2) 0.3455(18) 0.054(7) Uiso 1 1 d . . . H50B H 0.162(2) 0.396(2) 0.3221(19) 0.063(8) 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 P1 0.0257(3) 0.0264(2) 0.0353(3) 0.0127(2) -0.0013(2) 0.00044(17) P2 0.0271(3) 0.0281(2) 0.0348(3) 0.0132(2) 0.0023(2) 0.00096(18) O1 0.366(8) 0.414(10) 0.135(4) 0.149(5) 0.103(4) 0.266(8) O2 0.0476(9) 0.0447(9) 0.0545(9) 0.0217(7) 0.0138(7) 0.0175(7) N1 0.0253(8) 0.0238(8) 0.0412(9) 0.0109(7) 0.0018(7) 0.0013(6) N2 0.0258(9) 0.0257(8) 0.0478(10) 0.0126(7) 0.0059(8) 0.0026(6) C1 0.0291(10) 0.0294(9) 0.0401(10) 0.0165(8) 0.0007(8) 0.0044(7) C2 0.0344(11) 0.0366(10) 0.0381(10) 0.0166(9) 0.0009(9) 0.0053(8) C3 0.0555(15) 0.0485(13) 0.0399(12) 0.0226(10) 0.0041(11) 0.0120(11) C4 0.0619(16) 0.0465(13) 0.0541(14) 0.0292(11) 0.0163(12) 0.0122(11) C5 0.0433(13) 0.0397(12) 0.0621(15) 0.0270(11) 0.0103(11) -0.0005(10) C6 0.0338(11) 0.0332(10) 0.0497(12) 0.0200(9) 0.0003(9) 0.0008(8) C7 0.0454(14) 0.0554(15) 0.0392(12) 0.0170(11) -0.0105(11) -0.0082(11) C8 0.110(3) 0.075(2) 0.074(2) 0.0516(17) 0.0205(19) 0.0013(19) C9 0.0477(15) 0.0476(14) 0.0628(17) 0.0262(12) -0.0160(13) -0.0192(12) C10 0.0243(9) 0.0266(9) 0.0357(10) 0.0143(7) 0.0002(8) -0.0009(7) C11 0.0287(10) 0.0309(9) 0.0359(10) 0.0164(8) 0.0050(8) 0.0014(7) C12 0.0363(11) 0.0404(11) 0.0350(10) 0.0212(9) 0.0009(9) 0.0018(8) C13 0.0267(10) 0.0398(11) 0.0453(11) 0.0231(9) 0.0021(9) 0.0038(8) C14 0.0260(10) 0.0353(10) 0.0420(11) 0.0161(9) 0.0060(8) 0.0045(8) C15 0.0294(10) 0.0307(9) 0.0348(10) 0.0132(8) 0.0023(8) 0.0007(7) C16 0.0440(14) 0.0454(13) 0.0380(11) 0.0182(10) 0.0089(10) 0.0103(10) C17 0.0431(15) 0.0731(18) 0.0581(16) 0.0363(15) 0.0001(13) 0.0206(13) C18 0.0535(15) 0.0507(14) 0.0343(11) 0.0139(10) 0.0052(10) 0.0179(12) C19 0.0261(9) 0.0285(9) 0.0317(9) 0.0125(7) 0.0015(7) 0.0054(7) C20 0.0337(11) 0.0273(10) 0.0549(13) 0.0135(9) -0.0022(10) 0.0027(8) C21 0.0406(12) 0.0320(11) 0.0579(14) 0.0108(10) 0.0004(10) 0.0125(9) C22 0.0311(12) 0.0421(12) 0.0634(15) 0.0165(11) 0.0076(11) 0.0134(9) C23 0.0274(11) 0.0350(11) 0.0615(14) 0.0161(10) 0.0042(10) 0.0025(8) C24 0.0281(10) 0.0276(9) 0.0355(10) 0.0119(8) 0.0024(8) 0.0045(7) C25 0.0299(10) 0.0322(10) 0.0351(10) 0.0151(8) 0.0036(8) 0.0054(7) C26 0.0432(12) 0.0351(10) 0.0384(11) 0.0182(9) 0.0098(9) 0.0054(9) C27 0.0520(14) 0.0549(14) 0.0381(11) 0.0267(11) 0.0093(10) 0.0151(11) C28 0.0384(12) 0.0623(15) 0.0369(11) 0.0180(10) 0.0026(10) 0.0133(10) C29 0.0296(11) 0.0497(13) 0.0400(11) 0.0146(10) 0.0007(9) -0.0003(9) C30 0.0311(10) 0.0365(10) 0.0366(10) 0.0158(8) 0.0023(8) 0.0024(8) C31 0.0686(19) 0.0514(15) 0.0476(14) 0.0291(13) 0.0080(13) -0.0102(13) C32 0.0522(18) 0.114(3) 0.0433(15) 0.0355(18) -0.0084(13) 0.0064(17) C33 0.0411(13) 0.0495(13) 0.0491(14) 0.0275(11) -0.0043(11) -0.0125(10) C34 0.0278(10) 0.0284(9) 0.0366(10) 0.0138(8) 0.0022(8) 0.0010(7) C35 0.0363(11) 0.0325(10) 0.0379(10) 0.0118(8) 0.0056(9) 0.0037(8) C36 0.0474(13) 0.0327(10) 0.0462(12) 0.0125(10) 0.0121(10) 0.0110(9) C37 0.0431(12) 0.0356(11) 0.0567(13) 0.0245(10) 0.0081(10) 0.0090(9) C38 0.0401(12) 0.0405(11) 0.0430(12) 0.0242(9) 0.0041(9) 0.0054(9) C39 0.0295(10) 0.0302(9) 0.0390(10) 0.0143(8) 0.0041(8) 0.0008(7) C40 0.0565(16) 0.0507(15) 0.0359(12) 0.0111(11) 0.0075(11) 0.0156(12) C41 0.082(2) 0.0585(18) 0.077(2) 0.0395(17) 0.0179(18) 0.0375(16) C42 0.0429(13) 0.0450(13) 0.0352(11) 0.0158(10) 0.0038(10) 0.0085(10) C43 0.266(8) 0.148(5) 0.090(3) 0.060(3) 0.018(4) 0.062(5) C44 0.210(7) 0.121(4) 0.171(6) 0.066(4) 0.016(5) 0.076(5) C45 0.224(6) 0.207(6) 0.086(3) 0.032(4) 0.016(3) 0.153(6) C46 0.280(8) 0.296(9) 0.111(4) 0.112(5) 0.072(5) 0.223(8) C47 0.0537(16) 0.0531(14) 0.0479(13) 0.0178(11) 0.0063(12) 0.0114(12) C48 0.0532(16) 0.0511(15) 0.0596(16) 0.0170(12) 0.0155(13) 0.0171(12) C49 0.0499(15) 0.0549(15) 0.0619(16) 0.0241(13) 0.0094(12) 0.0198(12) C50 0.0456(14) 0.0442(13) 0.0474(13) 0.0178(11) 0.0063(11) 0.0076(10) _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 N1 1.7047(17) . ? P1 C10 1.8425(19) . ? P1 C1 1.846(2) . ? P2 N2 1.7043(18) . ? P2 C34 1.841(2) . ? P2 C25 1.847(2) . ? O1 C43 1.362(7) . ? O1 C46 1.375(7) . ? O2 C47 1.444(3) . ? O2 C50 1.449(3) . ? N1 C19 1.410(2) . ? N2 C24 1.408(2) . ? C1 C2 1.416(3) . ? C1 C6 1.417(3) . ? C2 C3 1.397(3) . ? C2 C7 1.513(3) . ? C3 C4 1.379(4) . ? C4 C5 1.389(4) . ? C4 C8 1.510(4) . ? C5 C6 1.389(3) . ? C6 C9 1.514(3) . ? C10 C15 1.410(3) . ? C10 C11 1.413(3) . ? C11 C12 1.390(3) . ? C11 C16 1.511(3) . ? C12 C13 1.389(3) . ? C13 C14 1.385(3) . ? C13 C17 1.509(3) . ? C14 C15 1.398(3) . ? C15 C18 1.505(3) . ? C19 C20 1.399(3) . ? C19 C24 1.411(3) . ? C20 C21 1.384(3) . ? C21 C22 1.373(3) . ? C22 C23 1.389(3) . ? C23 C24 1.397(3) . ? C25 C30 1.407(3) . ? C25 C26 1.414(3) . ? C26 C27 1.398(3) . ? C26 C31 1.512(3) . ? C27 C28 1.387(3) . ? C28 C29 1.381(3) . ? C28 C32 1.511(3) . ? C29 C30 1.395(3) . ? C30 C33 1.512(3) . ? C34 C35 1.412(3) . ? C34 C39 1.419(3) . ? C35 C36 1.395(3) . ? C35 C40 1.509(3) . ? C36 C37 1.391(3) . ? C37 C38 1.380(3) . ? C37 C41 1.513(3) . ? C38 C39 1.396(3) . ? C39 C42 1.512(3) . ? C43 C44 1.382(8) . ? C44 C45 1.434(8) . ? C45 C46 1.420(6) . ? C47 C48 1.509(4) . ? C48 C49 1.521(4) . ? C49 C50 1.510(3) . ? 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 P1 C10 101.61(8) . . ? N1 P1 C1 110.71(9) . . ? C10 P1 C1 107.26(9) . . ? N2 P2 C34 100.06(8) . . ? N2 P2 C25 110.10(9) . . ? C34 P2 C25 108.27(9) . . ? C43 O1 C46 111.0(5) . . ? C47 O2 C50 109.49(17) . . ? C19 N1 P1 121.65(13) . . ? C24 N2 P2 121.32(15) . . ? C2 C1 C6 118.17(18) . . ? C2 C1 P1 127.46(15) . . ? C6 C1 P1 113.46(15) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C7 117.26(19) . . ? C1 C2 C7 123.82(19) . . ? C4 C3 C2 123.4(2) . . ? C3 C4 C5 117.1(2) . . ? C3 C4 C8 121.9(3) . . ? C5 C4 C8 120.9(3) . . ? C6 C5 C4 122.3(2) . . ? C5 C6 C1 120.1(2) . . ? C5 C6 C9 118.5(2) . . ? C1 C6 C9 121.44(19) . . ? C15 C10 C11 118.52(17) . . ? C15 C10 P1 127.28(15) . . ? C11 C10 P1 114.07(14) . . ? C12 C11 C10 119.88(18) . . ? C12 C11 C16 117.79(18) . . ? C10 C11 C16 122.32(17) . . ? C13 C12 C11 122.15(19) . . ? C14 C13 C12 117.58(18) . . ? C14 C13 C17 121.6(2) . . ? C12 C13 C17 120.8(2) . . ? C13 C14 C15 122.46(19) . . ? C14 C15 C10 119.36(18) . . ? C14 C15 C18 117.13(19) . . ? C10 C15 C18 123.50(18) . . ? C20 C19 N1 120.54(18) . . ? C20 C19 C24 118.03(17) . . ? N1 C19 C24 121.43(16) . . ? C21 C20 C19 122.5(2) . . ? C22 C21 C20 119.5(2) . . ? C21 C22 C23 119.2(2) . . ? C22 C23 C24 122.4(2) . . ? C23 C24 N2 119.54(18) . . ? C23 C24 C19 118.31(17) . . ? N2 C24 C19 122.15(17) . . ? C30 C25 C26 118.58(17) . . ? C30 C25 P2 112.91(14) . . ? C26 C25 P2 127.54(16) . . ? C27 C26 C25 118.7(2) . . ? C27 C26 C31 117.0(2) . . ? C25 C26 C31 124.3(2) . . ? C28 C27 C26 123.2(2) . . ? C29 C28 C27 117.3(2) . . ? C29 C28 C32 121.3(3) . . ? C27 C28 C32 121.4(2) . . ? C28 C29 C30 122.0(2) . . ? C29 C30 C25 120.18(19) . . ? C29 C30 C33 117.84(19) . . ? C25 C30 C33 121.97(17) . . ? C35 C34 C39 118.89(18) . . ? C35 C34 P2 127.53(15) . . ? C39 C34 P2 113.58(14) . . ? C36 C35 C34 118.81(19) . . ? C36 C35 C40 117.6(2) . . ? C34 C35 C40 123.63(19) . . ? C37 C36 C35 122.7(2) . . ? C38 C37 C36 117.88(19) . . ? C38 C37 C41 121.2(2) . . ? C36 C37 C41 120.9(2) . . ? C37 C38 C39 122.0(2) . . ? C38 C39 C34 119.47(19) . . ? C38 C39 C42 117.94(19) . . ? C34 C39 C42 122.58(18) . . ? O1 C43 C44 107.6(5) . . ? C43 C44 C45 108.4(5) . . ? C46 C45 C44 105.5(5) . . ? O1 C46 C45 107.0(5) . . ? O2 C47 C48 106.0(2) . . ? C47 C48 C49 102.6(2) . . ? C50 C49 C48 103.0(2) . . ? O2 C50 C49 106.3(2) . . ? _diffrn_measured_fraction_theta_max 0.798 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.798 _refine_diff_density_max 0.559 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.054