Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #============================================================================== _audit_creation_date 1-03-99 # 1. SUBMISSION DETAILS _publ_contact_author 'Dr Pierre Braunstein' _publ_contact_author_address ; Dr Pierre Braunstein Laboratoire de Chimie de Coordination, UMR 7513 CNRS Universite Louis Pasteur, 4 rue Blaise Pascal F-67070 Strasbourg Cedex France ; _publ_contact_author_phone '0033 388 416030' _publ_contact_author_email 'braunst@chimie.u-strasbg.fr' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A new chiral metalladiphosphine for early-late chemistry. Crystal structure of a D-Camphor-based zirconium enolato phosphine and rearrangement of heterobimetallic Zr/Pd complexes ; loop_ _publ_author_name _publ_author_address 'Braunstein, Pierre ' ; Laboratoire de Chimie de Coordination, UMR 7513 CNRS Universite Louis Pasteur, 4 rue Blaise Pascal F-67070 Strasbourg Cedex France ; 'Mattheis, Chris ' ; Laboratoire de Chimie de Coordination, UMR 7513 CNRS Universite Louis Pasteur, 4 rue Blaise Pascal F-67070 Strasbourg Cedex France ; 'Fischer, Axel ' ; Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 D-39106 Magdeburg Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st338 _database_code_CSD 158617 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C48 H58 O4 P2 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H58 O4 P2 Pd' _chemical_formula_weight 867.34 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall ' P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,-z _cell_length_a 10.4840(2) _cell_length_b 34.0610(7) _cell_length_c 12.9620(2) _cell_angle_alpha 90 _cell_angle_beta 112.670(3) _cell_angle_gamma 90 _cell_volume 4271.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.35 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 60 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 29 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18151 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 23.79 _reflns_number_total 5399 _reflns_number_gt 4817 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0009 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4817 _refine_ls_number_parameters 990 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39,876-881' _refine_ls_R_factor_all 0.037 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_all 0.222 _refine_ls_wR_factor_ref 0.035 _refine_ls_goodness_of_fit_all 6.686 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.362 _refine_diff_density_min -0.081 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol Pd1 -0.01093(4) 0.7100 0.19649(3) 0.0237(2) Uani ? ? Pd P1 0.1983(1) 0.72151(4) 0.3332(1) 0.0249(7) Uani ? ? P C1 0.3209(5) 0.6815(2) 0.3653(4) 0.024(3) Uani ? ? C C2 0.2922(5) 0.6484(2) 0.4143(4) 0.035(3) Uani ? ? C C3 0.3740(6) 0.6152(2) 0.4314(5) 0.042(3) Uani ? ? C C4 0.4866(6) 0.6153(2) 0.4026(5) 0.043(3) Uani ? ? C C5 0.5185(5) 0.6478(2) 0.3525(5) 0.043(3) Uani ? ? C C6 0.4352(5) 0.6812(2) 0.3331(4) 0.030(3) Uani ? ? C C7 0.2873(5) 0.7659(2) 0.3239(4) 0.030(3) Uani ? ? C C8 0.4258(6) 0.7728(2) 0.3928(4) 0.036(3) Uani ? ? C C9 0.4854(6) 0.8092(2) 0.3917(5) 0.048(4) Uani ? ? C C10 0.4104(6) 0.8386(2) 0.3232(5) 0.052(3) Uani ? ? C C11 0.2740(6) 0.8325(2) 0.2545(5) 0.041(3) Uani ? ? C C12 0.2126(6) 0.7963(2) 0.2550(4) 0.036(3) Uani ? ? C C13 0.1446(5) 0.7287(2) 0.4445(4) 0.029(3) Uani ? ? C C14 0.2073(5) 0.7470(2) 0.5583(4) 0.030(3) Uani ? ? C C15 0.1108(5) 0.7309(2) 0.6157(4) 0.031(3) Uani ? ? C C16 -0.0231(5) 0.7442(2) 0.5147(4) 0.032(3) Uani ? ? C C17 0.0061(5) 0.7278(2) 0.4168(4) 0.028(3) Uani ? ? C C18 0.1667(6) 0.7913(2) 0.5408(4) 0.040(3) Uani ? ? C C19 0.0092(6) 0.7892(2) 0.5089(5) 0.041(3) Uani ? ? C C20 0.1324(6) 0.7509(2) 0.7262(4) 0.050(3) Uani ? ? C C21 0.1223(6) 0.6872(2) 0.6344(4) 0.039(3) Uani ? ? C C22 -0.1622(6) 0.7355(2) 0.5181(4) 0.048(3) Uani ? ? C O1 -0.0915(3) 0.7187(1) 0.3199(3) 0.029(2) Uani ? ? O P2 0.0555(1) 0.70265(4) 0.0517(1) 0.0258(7) Uani ? ? P C23 0.1496(5) 0.7431(2) 0.0244(4) 0.028(3) Uani ? ? C C24 0.2931(5) 0.7443(2) 0.0645(4) 0.032(3) Uani ? ? C C25 0.3606(6) 0.7767(2) 0.0491(5) 0.044(3) Uani ? ? C C26 0.2873(7) 0.8089(2) -0.0066(5) 0.051(3) Uani ? ? C C27 0.1455(6) 0.8089(2) -0.0462(4) 0.036(3) Uani ? ? C C28 0.0762(5) 0.7759(2) -0.0309(4) 0.039(3) Uani ? ? C C29 0.1564(5) 0.6596(2) 0.0534(4) 0.030(3) Uani ? ? C C30 0.2200(6) 0.6554(2) -0.0235(5) 0.045(3) Uani ? ? C C31 0.2912(6) 0.6210(2) -0.0248(5) 0.063(4) Uani ? ? C C32 0.3025(6) 0.5917(2) 0.0498(6) 0.050(4) Uani ? ? C C33 0.2416(7) 0.5951(2) 0.1249(6) 0.046(4) Uani ? ? C C34 0.1681(6) 0.6290(2) 0.1279(5) 0.035(3) Uani ? ? C C35 -0.1093(5) 0.6987(2) -0.0558(4) 0.026(3) Uani ? ? C C36 -0.1646(5) 0.6863(2) -0.1774(4) 0.030(3) Uani ? ? C C37 -0.3128(5) 0.7044(2) -0.2186(4) 0.031(3) Uani ? ? C C38 -0.3447(5) 0.6846(2) -0.1219(4) 0.032(3) Uani ? ? C C39 -0.2153(5) 0.6965(2) -0.0207(4) 0.025(3) Uani ? ? C C40 -0.1958(7) 0.6420(2) -0.1787(5) 0.048(4) Uani ? ? C C41 -0.3201(7) 0.6407(2) -0.1404(5) 0.045(4) Uani ? ? C C42 -0.3167(6) 0.7484(2) -0.2164(5) 0.049(4) Uani ? ? C C43 -0.4086(6) 0.6904(2) -0.3368(5) 0.044(3) Uani ? ? C C44 -0.4817(6) 0.6940(3) -0.1122(5) 0.047(4) Uani ? ? C O2 -0.2121(3) 0.7007(1) 0.0796(2) 0.032(2) Uani ? ? O Pd2 0.13377(4) 0.49647(2) 0.32954(3) 0.0238(2) Uani ? ? Pd P3 0.0728(1) 0.49622(5) 0.4786(1) 0.0256(6) Uani ? ? P C45 -0.0338(4) 0.4578(2) 0.4983(4) 0.022(3) Uani ? ? C C46 0.0243(5) 0.4222(2) 0.5458(4) 0.030(3) Uani ? ? C C47 -0.0611(6) 0.3925(2) 0.5588(5) 0.039(3) Uani ? ? C C48 -0.2001(6) 0.3985(2) 0.5244(4) 0.045(3) Uani ? ? C C49 -0.2586(6) 0.4334(2) 0.4772(5) 0.044(3) Uani ? ? C C50 -0.1786(5) 0.4637(2) 0.4629(4) 0.034(3) Uani ? ? C C51 -0.0083(5) 0.5410(2) 0.4997(4) 0.030(3) Uani ? ? C C52 -0.0173(6) 0.5739(2) 0.4334(5) 0.033(3) Uani ? ? C C53 -0.0757(6) 0.6086(2) 0.4524(5) 0.043(4) Uani ? ? C C54 -0.1237(6) 0.6101(2) 0.5387(6) 0.054(4) Uani ? ? C C55 -0.1107(6) 0.5780(2) 0.6064(5) 0.067(4) Uani ? ? C C56 -0.0539(6) 0.5433(2) 0.5869(5) 0.052(3) Uani ? ? C C57 0.2391(5) 0.4939(2) 0.5820(4) 0.029(2) Uani ? ? C C58 0.3046(5) 0.4928(2) 0.7105(4) 0.031(3) Uani ? ? C C59 0.4120(5) 0.5265(2) 0.7341(4) 0.034(3) Uani ? ? C C60 0.4765(5) 0.5097(2) 0.6537(4) 0.026(3) Uani ? ? C C61 0.3420(5) 0.5043(2) 0.5492(4) 0.029(3) Uani ? ? C C62 0.3990(6) 0.4562(2) 0.7422(4) 0.040(3) Uani ? ? C C63 0.5143(6) 0.4674(2) 0.6994(4) 0.039(3) Uani ? ? C C64 0.5146(7) 0.5289(2) 0.8566(5) 0.049(4) Uani ? ? C C65 0.3454(6) 0.5672(2) 0.7019(5) 0.049(4) Uani ? ? C C66 0.5887(6) 0.5329(2) 0.6350(4) 0.038(3) Uani ? ? C O3 0.3345(3) 0.5075(1) 0.4455(3) 0.032(2) Uani ? ? O P4 -0.0760(1) 0.48771(4) 0.1935(1) 0.0264(7) Uani ? ? P C67 -0.1784(5) 0.5315(2) 0.1760(4) 0.027(3) Uani ? ? C C68 -0.2882(5) 0.5356(2) 0.2112(4) 0.028(3) Uani ? ? C C69 -0.3506(6) 0.5718(2) 0.2065(5) 0.047(3) Uani ? ? C C70 -0.3019(7) 0.6043(2) 0.1695(5) 0.048(4) Uani ? ? C C71 -0.1916(7) 0.6010(2) 0.1374(5) 0.046(4) Uani ? ? C C72 -0.1329(5) 0.5646(2) 0.1380(4) 0.033(3) Uani ? ? C C73 -0.1783(5) 0.4456(2) 0.1977(4) 0.026(3) Uani ? ? C C74 -0.1085(5) 0.4132(2) 0.2602(4) 0.033(3) Uani ? ? C C75 -0.1769(6) 0.3790(2) 0.2610(4) 0.043(3) Uani ? ? C C76 -0.3180(6) 0.3763(2) 0.1993(5) 0.044(3) Uani ? ? C C77 -0.3879(6) 0.4082(2) 0.1363(5) 0.046(3) Uani ? ? C C78 -0.3191(5) 0.4425(2) 0.1352(5) 0.036(3) Uani ? ? C C79 -0.0250(5) 0.4818(2) 0.0826(4) 0.032(3) Uani ? ? C C80 -0.0921(6) 0.4701(2) -0.0415(4) 0.035(3) Uani ? ? C C81 0.0250(6) 0.4455(2) -0.0558(4) 0.039(3) Uani ? ? C C82 0.1368(5) 0.4777(2) -0.0015(4) 0.036(3) Uani ? ? C C83 0.1125(5) 0.4851(2) 0.1070(4) 0.028(3) Uani ? ? C C84 -0.0867(6) 0.5076(2) -0.1071(4) 0.040(3) Uani ? ? C C85 0.0683(6) 0.5132(2) -0.0764(4) 0.041(3) Uani ? ? C C86 0.0531(7) 0.4065(2) 0.0101(5) 0.054(4) Uani ? ? C C87 -0.0001(7) 0.4353(2) -0.1765(5) 0.059(4) Uani ? ? C C88 0.2851(6) 0.4693(2) 0.0136(5) 0.051(3) Uani ? ? C O4 -0.3763(4) 0.7166(2) 0.2012(3) 0.055(3) Uani ? ? O O5 0.4977(4) 0.5034(2) 0.3199(3) 0.058(3) Uani ? ? O O6 -0.3594(6) 0.8422(2) 0.0295(5) 0.091(4) Uani ? ? O C89 -0.3586(7) 0.8587(2) 0.1285(6) 0.061(4) Uani ? ? C C90 -0.2806(7) 0.8337(3) 0.2218(6) 0.068(4) Uani ? ? C C91 -0.1762(8) 0.8163(3) 0.1862(6) 0.076(5) Uani ? ? C C92 -0.2534(8) 0.8125(3) 0.0622(6) 0.087(5) Uani ? ? C O7 0.2404(6) 0.3719(2) 0.4142(5) 0.106(4) Uani ? ? O C93 0.345(1) 0.4023(3) 0.4129(8) 0.089(6) Uani ? ? C C94 0.366(1) 0.3974(3) 0.3089(8) 0.098(6) Uani ? ? C C95 0.328(1) 0.3557(3) 0.2783(6) 0.085(5) Uani ? ? C C96 0.2238(9) 0.3467(3) 0.3239(7) 0.085(6) Uani ? ? C O8 0.2107(3) 0.4942(1) 0.2021(2) 0.028(2) Uani ? ? O H1 0.2157 0.6484 0.4364 0.0452 Uiso calc C2 H H2 0.3519 0.5924 0.4631 0.0562 Uiso calc C3 H H3 0.5440 0.5927 0.4172 0.0565 Uiso calc C4 H H4 0.5960 0.6474 0.3317 0.0550 Uiso calc C5 H H5 0.4552 0.7036 0.2983 0.0421 Uiso calc C6 H H6 0.4792 0.7526 0.4405 0.0495 Uiso calc C8 H H7 0.5793 0.8137 0.4389 0.0661 Uiso calc C9 H H8 0.4525 0.8632 0.3230 0.0663 Uiso calc C10 H H9 0.2220 0.8530 0.2071 0.0576 Uiso calc C11 H H10 0.1185 0.7922 0.2076 0.0472 Uiso calc C12 H H11 0.3037 0.7426 0.5959 0.0396 Uiso calc C14 H H12 0.1883 0.8024 0.4823 0.0493 Uiso calc C18 H H13 0.2109 0.8059 0.6075 0.0493 Uiso calc C18 H H14 -0.0165 0.8038 0.5603 0.0526 Uiso calc C19 H H15 -0.0388 0.7991 0.4355 0.0526 Uiso calc C19 H H16 0.0711 0.7398 0.7565 0.0627 Uiso calc C20 H H17 0.2251 0.7471 0.7771 0.0627 Uiso calc C20 H H18 0.1144 0.7782 0.7140 0.0627 Uiso calc C20 H H19 0.0618 0.6792 0.6693 0.0520 Uiso calc C21 H H20 0.0977 0.6741 0.5646 0.0520 Uiso calc C21 H H21 0.2147 0.6806 0.6811 0.0520 Uiso calc C21 H H22 -0.1678 0.7472 0.5827 0.0586 Uiso calc C22 H H23 -0.2328 0.7459 0.4531 0.0586 Uiso calc C22 H H24 -0.1739 0.7079 0.5206 0.0586 Uiso calc C22 H H25 0.3450 0.7222 0.1031 0.0419 Uiso calc C24 H H26 0.4587 0.7769 0.0770 0.0571 Uiso calc C25 H H27 0.3348 0.8312 -0.0178 0.0674 Uiso calc C26 H H28 0.0949 0.8313 -0.0837 0.0478 Uiso calc C27 H H29 -0.0219 0.7759 -0.0586 0.0496 Uiso calc C28 H H30 0.2144 0.6760 -0.0745 0.0552 Uiso calc C30 H H31 0.3322 0.6179 -0.0781 0.0777 Uiso calc C31 H H32 0.3535 0.5687 0.0494 0.0762 Uiso calc C32 H H33 0.2490 0.5743 0.1756 0.0736 Uiso calc C33 H H34 0.1261 0.6312 0.1807 0.0488 Uiso calc C34 H H35 -0.1070 0.6929 -0.2163 0.0430 Uiso calc C36 H H36 -0.1185 0.6280 -0.1280 0.0686 Uiso calc C40 H H37 -0.2209 0.6313 -0.2516 0.0686 Uiso calc C40 H H38 -0.3995 0.6295 -0.1966 0.0640 Uiso calc C41 H H39 -0.2971 0.6262 -0.0730 0.0640 Uiso calc C41 H H40 -0.2967 0.7586 -0.2767 0.0662 Uiso calc C42 H H41 -0.4061 0.7568 -0.2234 0.0662 Uiso calc C42 H H42 -0.2499 0.7576 -0.1477 0.0662 Uiso calc C42 H H43 -0.4968 0.7023 -0.3570 0.0645 Uiso calc C43 H H44 -0.3696 0.6976 -0.3891 0.0645 Uiso calc C43 H H45 -0.4183 0.6626 -0.3366 0.0645 Uiso calc C43 H H46 -0.5559 0.6857 -0.1781 0.0762 Uiso calc C44 H H47 -0.4865 0.6806 -0.0494 0.0762 Uiso calc C44 H H48 -0.4883 0.7215 -0.1029 0.0762 Uiso calc C44 H H49 0.1210 0.4180 0.5693 0.0424 Uiso calc C46 H H50 -0.0221 0.3682 0.5915 0.0538 Uiso calc C47 H H51 -0.2571 0.3782 0.5334 0.0544 Uiso calc C48 H H52 -0.3555 0.4370 0.4539 0.0550 Uiso calc C49 H H53 -0.2197 0.4878 0.4301 0.0427 Uiso calc C50 H H54 0.0164 0.5727 0.3752 0.0476 Uiso calc C52 H H55 -0.0826 0.6310 0.4068 0.0666 Uiso calc C53 H H56 -0.1655 0.6335 0.5510 0.0756 Uiso calc C54 H H57 -0.1407 0.5795 0.6666 0.0806 Uiso calc C55 H H58 -0.0462 0.5212 0.6334 0.0602 Uiso calc C56 H H59 0.2401 0.4938 0.7457 0.0457 Uiso calc C58 H H60 0.3504 0.4334 0.7055 0.0541 Uiso calc C62 H H61 0.4363 0.4520 0.8207 0.0541 Uiso calc C62 H H62 0.6027 0.4669 0.7588 0.0543 Uiso calc C63 H H63 0.5137 0.4501 0.6418 0.0543 Uiso calc C63 H H64 0.4691 0.5394 0.9012 0.0735 Uiso calc C64 H H65 0.5483 0.5034 0.8826 0.0735 Uiso calc C64 H H66 0.5897 0.5455 0.8615 0.0735 Uiso calc C64 H H67 0.3087 0.5753 0.7550 0.0670 Uiso calc C65 H H68 0.4131 0.5855 0.7008 0.0670 Uiso calc C65 H H69 0.2731 0.5659 0.6298 0.0670 Uiso calc C65 H H70 0.5545 0.5582 0.6070 0.0544 Uiso calc C66 H H71 0.6660 0.5355 0.7037 0.0544 Uiso calc C66 H H72 0.6159 0.5195 0.5824 0.0544 Uiso calc C66 H H73 -0.3202 0.5134 0.2386 0.0399 Uiso calc C68 H H74 -0.4267 0.5742 0.2286 0.0616 Uiso calc C69 H H75 -0.3447 0.6291 0.1662 0.0672 Uiso calc C70 H H76 -0.1560 0.6236 0.1149 0.0644 Uiso calc C71 H H77 -0.0601 0.5623 0.1120 0.0438 Uiso calc C72 H H78 -0.0120 0.4149 0.3028 0.0397 Uiso calc C74 H H79 -0.1278 0.3572 0.3037 0.0541 Uiso calc C75 H H80 -0.3663 0.3528 0.2001 0.0554 Uiso calc C76 H H81 -0.4844 0.4063 0.0935 0.0601 Uiso calc C77 H H82 -0.3681 0.4641 0.0916 0.0480 Uiso calc C78 H H83 -0.1809 0.4584 -0.0625 0.0510 Uiso calc C80 H H84 -0.1253 0.5294 -0.0837 0.0541 Uiso calc C84 H H85 -0.1341 0.5039 -0.1853 0.0541 Uiso calc C84 H H86 0.0889 0.5133 -0.1416 0.0539 Uiso calc C85 H H87 0.0991 0.5371 -0.0366 0.0539 Uiso calc C85 H H88 0.1252 0.3926 -0.0014 0.0737 Uiso calc C86 H H89 0.0799 0.4119 0.0876 0.0737 Uiso calc C86 H H90 -0.0284 0.3909 -0.0152 0.0737 Uiso calc C86 H H91 0.0754 0.4204 -0.1785 0.0774 Uiso calc C87 H H92 -0.0828 0.4204 -0.2083 0.0774 Uiso calc C87 H H93 -0.0086 0.4588 -0.2182 0.0774 Uiso calc C87 H H94 0.3414 0.4913 0.0474 0.0646 Uiso calc C88 H H95 0.3177 0.4469 0.0601 0.0646 Uiso calc C88 H H96 0.2891 0.4644 -0.0573 0.0646 Uiso calc C88 H H97 -0.4508 0.8611 0.1242 0.0838 Uiso calc C89 H H98 -0.3169 0.8840 0.1388 0.0838 Uiso calc C89 H H99 -0.3379 0.8141 0.2335 0.0876 Uiso calc C90 H H100 -0.2385 0.8486 0.2883 0.0876 Uiso calc C90 H H101 -0.1470 0.7914 0.2201 0.0976 Uiso calc C91 H H102 -0.0983 0.8331 0.2033 0.0976 Uiso calc C91 H H103 -0.1925 0.8165 0.0247 0.1058 Uiso calc C92 H H104 -0.2939 0.7872 0.0445 0.1058 Uiso calc C92 H H105 0.4299 0.3984 0.4749 0.1390 Uiso calc C93 H H106 0.3112 0.4279 0.4164 0.1390 Uiso calc C93 H H107 0.4597 0.4021 0.3199 0.1319 Uiso calc C94 H H108 0.3079 0.4146 0.2528 0.1319 Uiso calc C94 H H109 0.4059 0.3391 0.3104 0.1166 Uiso calc C95 H H110 0.2902 0.3525 0.1994 0.1166 Uiso calc C95 H H111 0.1342 0.3502 0.2674 0.1148 Uiso calc C96 H H112 0.2343 0.3202 0.3490 0.1148 Uiso calc C96 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pd1 0.0218(2) 0.0281(2) 0.0217(2) 0.0002(2) 0.0083(1) -0.0018(2) Pd P1 0.0245(6) 0.0275(8) 0.0228(6) 0.0008(6) 0.0084(5) -0.0017(6) P C1 0.020(2) 0.033(3) 0.021(2) 0.001(2) 0.004(2) -0.002(3) C C2 0.035(3) 0.040(3) 0.030(2) 0.010(3) 0.013(2) 0.000(3) C C3 0.052(3) 0.037(4) 0.040(3) 0.006(3) 0.016(2) 0.010(3) C C4 0.040(3) 0.044(4) 0.044(3) 0.020(3) 0.014(2) 0.011(3) C C5 0.035(3) 0.054(4) 0.042(3) 0.019(3) 0.019(2) 0.002(3) C C6 0.032(3) 0.038(3) 0.023(2) 0.002(3) 0.006(2) -0.003(3) C C7 0.033(3) 0.028(3) 0.030(2) 0.001(2) 0.014(2) 0.001(3) C C8 0.034(3) 0.042(4) 0.032(3) -0.003(3) 0.007(2) -0.005(3) C C9 0.038(3) 0.056(4) 0.051(3) -0.015(3) 0.010(3) -0.016(4) C C10 0.065(3) 0.035(4) 0.064(3) -0.004(3) 0.037(2) -0.006(3) C C11 0.067(4) 0.030(3) 0.035(3) 0.003(3) 0.018(2) 0.004(3) C C12 0.040(3) 0.041(4) 0.029(2) -0.003(3) 0.015(2) -0.006(3) C C13 0.027(2) 0.033(3) 0.028(2) 0.003(3) 0.013(2) -0.000(3) C C14 0.033(3) 0.037(3) 0.021(2) -0.004(3) 0.010(2) -0.007(3) C C15 0.040(3) 0.038(3) 0.021(2) -0.007(3) 0.010(2) -0.009(3) C C16 0.037(3) 0.038(3) 0.024(2) -0.003(3) 0.016(2) -0.005(3) C C17 0.039(3) 0.024(3) 0.025(2) 0.001(3) 0.012(2) 0.002(3) C C18 0.046(3) 0.038(3) 0.036(2) -0.012(3) 0.022(2) -0.015(3) C C19 0.049(3) 0.037(3) 0.036(3) 0.004(3) 0.018(2) -0.005(3) C C20 0.058(3) 0.062(4) 0.034(2) -0.002(3) 0.029(2) -0.005(3) C C21 0.046(3) 0.041(4) 0.031(3) -0.004(3) 0.013(2) 0.008(3) C C22 0.046(3) 0.057(4) 0.041(3) -0.004(3) 0.027(2) -0.013(3) C O1 0.026(2) 0.036(2) 0.026(2) -0.003(2) 0.006(1) -0.004(2) O P2 0.0249(6) 0.0301(8) 0.0229(6) 0.0000(6) 0.0094(4) -0.0013(7) P C23 0.026(2) 0.036(3) 0.024(2) -0.003(3) 0.011(2) -0.003(3) C C24 0.029(3) 0.034(3) 0.032(3) -0.001(3) 0.010(2) -0.006(3) C C25 0.039(3) 0.054(4) 0.039(3) -0.014(3) 0.016(2) 0.001(3) C C26 0.072(4) 0.050(4) 0.037(3) -0.013(3) 0.025(2) 0.005(3) C C27 0.051(3) 0.026(3) 0.037(3) -0.004(3) 0.020(2) -0.001(3) C C28 0.042(3) 0.042(4) 0.033(3) 0.000(3) 0.018(2) -0.007(3) C C29 0.026(3) 0.034(3) 0.029(2) 0.001(3) 0.010(2) -0.004(3) C C30 0.043(3) 0.046(4) 0.045(3) -0.009(3) 0.025(2) -0.011(3) C C31 0.049(3) 0.057(4) 0.088(4) -0.002(3) 0.043(2) -0.034(3) C C32 0.028(3) 0.050(4) 0.089(4) -0.003(3) 0.013(3) -0.030(4) C C33 0.051(4) 0.032(4) 0.059(4) 0.002(3) -0.010(3) -0.007(4) C C34 0.035(3) 0.035(3) 0.034(3) 0.002(3) 0.004(2) -0.009(3) C C35 0.024(2) 0.030(3) 0.025(2) 0.002(2) 0.008(2) -0.001(3) C C36 0.026(3) 0.046(4) 0.023(2) -0.004(3) 0.005(2) -0.000(3) C C37 0.031(3) 0.039(4) 0.024(2) -0.005(3) 0.008(2) -0.006(3) C C38 0.026(3) 0.053(4) 0.024(2) -0.004(3) 0.003(2) 0.007(3) C C39 0.026(3) 0.023(3) 0.025(2) -0.000(2) 0.006(2) -0.002(2) C C40 0.064(4) 0.044(4) 0.039(3) -0.001(4) 0.007(3) -0.013(3) C C41 0.059(4) 0.041(4) 0.038(3) -0.014(3) 0.008(3) -0.008(3) C C42 0.052(3) 0.056(4) 0.040(3) 0.004(4) 0.012(3) 0.017(3) C C43 0.038(3) 0.077(5) 0.029(3) -0.000(3) 0.007(2) 0.000(3) C C44 0.031(3) 0.107(6) 0.032(3) -0.010(4) 0.005(2) -0.003(4) C O2 0.031(2) 0.042(2) 0.025(2) -0.001(2) 0.013(1) -0.003(2) O Pd2 0.0219(2) 0.0286(2) 0.0215(2) 0.0008(2) 0.0079(1) 0.0004(2) Pd P3 0.0249(6) 0.0287(7) 0.0234(6) -0.0022(7) 0.0096(4) -0.0022(7) P C45 0.020(3) 0.028(3) 0.018(2) -0.001(2) 0.005(2) 0.000(2) C C46 0.032(3) 0.040(3) 0.022(2) -0.007(3) 0.006(2) -0.005(3) C C47 0.053(3) 0.029(3) 0.038(3) -0.005(3) 0.014(2) 0.005(3) C C48 0.046(3) 0.045(4) 0.043(3) -0.017(3) 0.028(2) -0.006(3) C C49 0.041(3) 0.043(4) 0.049(3) -0.006(3) 0.025(2) -0.007(3) C C50 0.034(3) 0.032(3) 0.035(3) -0.004(3) 0.016(2) -0.004(3) C C51 0.026(2) 0.032(3) 0.030(2) -0.003(3) 0.007(2) -0.003(3) C C52 0.039(3) 0.025(3) 0.037(3) 0.004(3) 0.005(2) -0.003(3) C C53 0.048(4) 0.031(3) 0.054(4) 0.002(3) -0.003(3) 0.001(3) C C54 0.043(3) 0.039(4) 0.093(4) -0.002(3) 0.027(3) -0.022(4) C C55 0.068(3) 0.046(4) 0.094(4) -0.019(3) 0.056(2) -0.025(3) C C56 0.061(3) 0.037(3) 0.061(3) -0.006(3) 0.046(2) -0.013(3) C C57 0.022(2) 0.036(3) 0.031(2) -0.003(3) 0.013(2) -0.004(3) C C58 0.029(2) 0.056(4) 0.019(2) -0.002(3) 0.008(2) -0.002(3) C C59 0.033(3) 0.047(4) 0.025(2) -0.010(3) 0.009(2) -0.003(3) C C60 0.024(3) 0.036(3) 0.021(2) -0.007(2) -0.002(2) 0.002(3) C C61 0.026(3) 0.036(4) 0.026(2) 0.002(3) 0.003(2) 0.004(3) C C62 0.048(3) 0.043(4) 0.032(3) -0.008(3) 0.013(2) 0.007(3) C C63 0.039(3) 0.049(4) 0.030(3) 0.007(3) 0.006(2) 0.011(3) C C64 0.053(4) 0.079(5) 0.028(3) -0.016(4) 0.005(3) 0.000(4) C C65 0.054(4) 0.048(4) 0.045(3) -0.006(3) 0.011(3) -0.009(4) C C66 0.031(3) 0.055(4) 0.032(3) -0.008(3) 0.004(2) 0.008(3) C O3 0.027(2) 0.045(2) 0.026(1) -0.001(2) 0.011(1) 0.004(2) O P4 0.0244(6) 0.0295(9) 0.0256(6) -0.0001(6) 0.0087(5) 0.0001(7) P C67 0.026(2) 0.034(3) 0.023(2) -0.001(3) 0.003(2) -0.005(3) C C68 0.025(3) 0.040(3) 0.023(2) 0.007(3) 0.004(2) 0.007(3) C C69 0.037(3) 0.056(4) 0.049(3) 0.010(3) 0.017(2) -0.006(3) C C70 0.064(4) 0.035(4) 0.049(3) 0.012(3) 0.014(3) 0.003(3) C C71 0.053(4) 0.044(4) 0.043(3) 0.001(3) 0.009(3) 0.011(3) C C72 0.035(3) 0.026(3) 0.039(3) 0.005(3) 0.012(2) 0.010(3) C C73 0.024(2) 0.027(3) 0.027(2) 0.004(2) 0.011(2) -0.000(3) C C74 0.037(3) 0.031(3) 0.031(2) -0.005(3) 0.020(2) -0.006(3) C C75 0.060(3) 0.032(3) 0.040(3) 0.000(3) 0.028(2) 0.001(3) C C76 0.044(3) 0.037(3) 0.053(3) -0.020(3) 0.026(2) -0.017(3) C C77 0.036(3) 0.044(4) 0.061(3) -0.004(3) 0.020(2) -0.013(3) C C78 0.033(3) 0.034(3) 0.041(3) -0.007(3) 0.012(2) -0.005(3) C C79 0.027(3) 0.042(3) 0.029(2) -0.006(3) 0.010(2) 0.000(3) C C80 0.030(3) 0.051(4) 0.028(3) -0.007(3) 0.003(2) 0.004(3) C C81 0.051(3) 0.043(4) 0.026(3) -0.001(3) 0.012(2) -0.006(3) C C82 0.041(3) 0.041(3) 0.028(2) 0.003(3) 0.018(2) 0.005(3) C C83 0.030(2) 0.026(3) 0.029(2) 0.002(2) 0.011(2) -0.001(3) C C84 0.038(3) 0.049(4) 0.034(3) 0.003(3) 0.009(2) 0.006(3) C C85 0.048(3) 0.047(4) 0.030(3) 0.007(3) 0.016(2) 0.008(3) C C86 0.083(4) 0.040(4) 0.048(3) -0.005(4) 0.026(3) -0.012(3) C C87 0.085(4) 0.055(5) 0.044(3) -0.005(4) 0.030(3) -0.010(3) C C88 0.049(3) 0.068(5) 0.039(3) 0.011(3) 0.025(2) 0.007(3) C O4 0.031(2) 0.109(4) 0.050(2) 0.006(3) 0.016(2) 0.003(3) O O5 0.034(2) 0.103(4) 0.057(2) -0.005(2) 0.022(1) -0.004(3) O O6 0.096(4) 0.095(4) 0.082(3) 0.034(3) 0.023(3) 0.012(3) O C89 0.047(4) 0.069(5) 0.070(4) 0.011(4) 0.014(3) -0.008(4) C C90 0.065(4) 0.080(5) 0.060(4) 0.006(4) 0.028(3) -0.015(4) C C91 0.077(4) 0.065(5) 0.086(4) 0.023(4) 0.035(3) 0.005(4) C C92 0.127(5) 0.059(5) 0.087(4) -0.013(4) 0.073(3) -0.012(4) C O7 0.092(4) 0.103(5) 0.125(4) 0.028(4) 0.036(3) -0.006(4) O C93 0.131(8) 0.056(5) 0.097(7) 0.009(6) 0.004(6) -0.006(6) C C94 0.098(6) 0.105(7) 0.091(6) -0.028(6) 0.025(4) -0.010(6) C C95 0.133(6) 0.066(5) 0.069(4) -0.006(5) 0.038(4) -0.012(5) C C96 0.098(6) 0.061(5) 0.102(6) -0.008(5) 0.034(4) 0.002(5) C O8 0.025(2) 0.043(2) 0.020(1) 0.002(2) 0.005(1) 0.002(2) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.260(2) . . ? Pd1 O1 2.097(4) . . ? Pd1 P2 2.254(2) . . ? Pd1 O2 2.093(4) . . ? P1 C1 1.808(6) . . ? P1 C7 1.804(7) . . ? P1 C13 1.757(7) . . ? C1 C2 1.38(1) . . ? C1 C6 1.412(9) . . ? C2 C3 1.38(1) . . ? C3 C4 1.37(1) . . ? C4 C5 1.39(1) . . ? C5 C6 1.40(1) . . ? C7 C8 1.401(9) . . ? C7 C12 1.39(1) . . ? C8 C9 1.39(1) . . ? C9 C10 1.37(1) . . ? C10 C11 1.38(1) . . ? C11 C12 1.39(1) . . ? C13 C14 1.501(9) . . ? C13 C17 1.355(9) . . ? C14 C15 1.568(9) . . ? C14 C18 1.56(1) . . ? C15 C16 1.57(1) . . ? C15 C20 1.52(1) . . ? C15 C21 1.51(1) . . ? C16 C17 1.521(9) . . ? C16 C19 1.58(1) . . ? C16 C22 1.51(1) . . ? C17 O1 1.316(8) . . ? C18 C19 1.54(1) . . ? P2 C23 1.806(7) . . ? P2 C29 1.804(7) . . ? P2 C35 1.758(6) . . ? C23 C24 1.390(9) . . ? C23 C28 1.39(1) . . ? C24 C25 1.37(1) . . ? C25 C26 1.37(1) . . ? C26 C27 1.37(1) . . ? C27 C28 1.39(1) . . ? C29 C30 1.404(9) . . ? C29 C34 1.39(1) . . ? C30 C31 1.39(1) . . ? C31 C32 1.36(1) . . ? C32 C33 1.36(1) . . ? C33 C34 1.40(1) . . ? C35 C36 1.514(9) . . ? C35 C39 1.356(9) . . ? C36 C37 1.561(9) . . ? C36 C40 1.54(1) . . ? C37 C38 1.569(9) . . ? C37 C42 1.50(1) . . ? C37 C43 1.547(9) . . ? C38 C39 1.535(9) . . ? C38 C41 1.55(1) . . ? C38 C44 1.52(1) . . ? C39 O2 1.295(7) . . ? C40 C41 1.56(1) . . ? Pd2 P3 2.257(2) . . ? Pd2 O3 2.096(4) . . ? Pd2 P4 2.246(2) . . ? Pd2 O8 2.100(4) . . ? P3 C45 1.801(7) . . ? P3 C51 1.818(7) . . ? P3 C57 1.744(6) . . ? C45 C46 1.39(1) . . ? C45 C50 1.421(9) . . ? C46 C47 1.40(1) . . ? C47 C48 1.37(1) . . ? C48 C49 1.37(1) . . ? C49 C50 1.38(1) . . ? C51 C52 1.39(1) . . ? C51 C56 1.39(1) . . ? C52 C53 1.40(1) . . ? C53 C54 1.39(1) . . ? C54 C55 1.38(1) . . ? C55 C56 1.39(1) . . ? C57 C58 1.538(8) . . ? C57 C61 1.351(9) . . ? C58 C59 1.55(1) . . ? C58 C62 1.55(1) . . ? C59 C60 1.55(1) . . ? C59 C64 1.54(1) . . ? C59 C65 1.54(1) . . ? C60 C61 1.544(9) . . ? C60 C63 1.55(1) . . ? C60 C66 1.51(1) . . ? C61 O3 1.320(7) . . ? C62 C63 1.56(1) . . ? P4 C67 1.801(7) . . ? P4 C73 1.805(7) . . ? P4 C79 1.728(7) . . ? C67 C68 1.400(9) . . ? C67 C72 1.39(1) . . ? C68 C69 1.39(1) . . ? C69 C70 1.38(1) . . ? C70 C71 1.38(1) . . ? C71 C72 1.38(1) . . ? C73 C74 1.40(1) . . ? C73 C78 1.387(9) . . ? C74 C75 1.37(1) . . ? C75 C76 1.39(1) . . ? C76 C77 1.39(1) . . ? C77 C78 1.38(1) . . ? C79 C80 1.54(1) . . ? C79 C83 1.355(9) . . ? C80 C81 1.56(1) . . ? C80 C84 1.55(1) . . ? C81 C82 1.56(1) . . ? C81 C86 1.55(1) . . ? C81 C87 1.52(1) . . ? C82 C83 1.544(9) . . ? C82 C85 1.54(1) . . ? C82 C88 1.52(1) . . ? C83 O8 1.304(7) . . ? C84 C85 1.53(1) . . ? O6 C89 1.40(1) . . ? O6 C92 1.44(1) . . ? C89 C90 1.45(1) . . ? C90 C91 1.47(1) . . ? C91 C92 1.50(1) . . ? O7 C93 1.51(2) . . ? O7 C96 1.41(1) . . ? C93 C94 1.46(2) . . ? C94 C95 1.49(2) . . ? C95 C96 1.46(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 O1 86.1(1) . . . ? P1 Pd1 P2 98.84(6) . . . ? P1 Pd1 O2 175.1(1) . . . ? O1 Pd1 P2 174.4(1) . . . ? O1 Pd1 O2 89.1(2) . . . ? P2 Pd1 O2 85.9(1) . . . ? C1 P1 C7 107.9(3) . . . ? C1 P1 C13 109.9(3) . . . ? C7 P1 C13 106.0(3) . . . ? P1 C1 C2 117.3(5) . . . ? P1 C1 C6 123.1(5) . . . ? C2 C1 C6 119.3(6) . . . ? C1 C2 C3 120.5(6) . . . ? C2 C3 C4 120.1(7) . . . ? C3 C4 C5 121.1(7) . . . ? C4 C5 C6 119.2(6) . . . ? C1 C6 C5 119.7(6) . . . ? P1 C7 C8 122.3(5) . . . ? P1 C7 C12 119.2(5) . . . ? C8 C7 C12 118.1(6) . . . ? C7 C8 C9 120.2(7) . . . ? C8 C9 C10 120.7(7) . . . ? C9 C10 C11 120.3(7) . . . ? C10 C11 C12 119.7(7) . . . ? C7 C12 C11 121.0(7) . . . ? P1 C13 C14 135.0(5) . . . ? P1 C13 C17 115.5(5) . . . ? C14 C13 C17 106.7(6) . . . ? C13 C14 C15 101.7(5) . . . ? C13 C14 C18 105.5(5) . . . ? C15 C14 C18 102.5(5) . . . ? C14 C15 C16 92.1(5) . . . ? C14 C15 C20 113.7(6) . . . ? C14 C15 C21 113.3(6) . . . ? C16 C15 C20 114.6(6) . . . ? C16 C15 C21 114.1(6) . . . ? C20 C15 C21 108.5(6) . . . ? C15 C16 C17 100.8(5) . . . ? C15 C16 C19 100.3(6) . . . ? C15 C16 C22 118.9(6) . . . ? C17 C16 C19 101.6(5) . . . ? C17 C16 C22 117.5(6) . . . ? C19 C16 C22 114.8(6) . . . ? C13 C17 C16 108.2(6) . . . ? C13 C17 O1 128.1(6) . . . ? C16 C17 O1 123.4(6) . . . ? C14 C18 C19 101.4(5) . . . ? C16 C19 C18 105.0(6) . . . ? C23 P2 C29 105.1(3) . . . ? C23 P2 C35 110.3(3) . . . ? C29 P2 C35 109.9(3) . . . ? P2 C23 C24 122.9(6) . . . ? P2 C23 C28 118.6(5) . . . ? C24 C23 C28 118.2(6) . . . ? C23 C24 C25 121.0(7) . . . ? C24 C25 C26 120.4(7) . . . ? C25 C26 C27 120.1(7) . . . ? C26 C27 C28 119.8(7) . . . ? C23 C28 C27 120.5(7) . . . ? P2 C29 C30 120.6(6) . . . ? P2 C29 C34 120.8(5) . . . ? C30 C29 C34 118.6(6) . . . ? C29 C30 C31 119.8(8) . . . ? C30 C31 C32 120.5(8) . . . ? C31 C32 C33 120.7(8) . . . ? C32 C33 C34 120.4(8) . . . ? C29 C34 C33 120.0(7) . . . ? P2 C35 C36 135.3(5) . . . ? P2 C35 C39 114.9(5) . . . ? C36 C35 C39 107.5(5) . . . ? C35 C36 C37 100.2(5) . . . ? C35 C36 C40 106.1(6) . . . ? C37 C36 C40 101.7(6) . . . ? C36 C37 C38 92.7(5) . . . ? C36 C37 C42 114.7(6) . . . ? C36 C37 C43 113.5(6) . . . ? C38 C37 C42 113.4(6) . . . ? C38 C37 C43 113.7(6) . . . ? C42 C37 C43 108.3(6) . . . ? C37 C38 C39 100.3(5) . . . ? C37 C38 C41 101.0(6) . . . ? C37 C38 C44 118.3(6) . . . ? C39 C38 C41 104.0(6) . . . ? C39 C38 C44 115.1(6) . . . ? C41 C38 C44 115.6(7) . . . ? C35 C39 C38 107.2(5) . . . ? C35 C39 O2 128.6(6) . . . ? C38 C39 O2 124.0(6) . . . ? C36 C40 C41 102.8(6) . . . ? C38 C41 C40 103.4(6) . . . ? P3 Pd2 O3 85.6(1) . . . ? P3 Pd2 P4 99.04(6) . . . ? P3 Pd2 O8 173.9(1) . . . ? O3 Pd2 P4 174.6(1) . . . ? O3 Pd2 O8 89.2(2) . . . ? P4 Pd2 O8 86.2(1) . . . ? C45 P3 C51 103.7(3) . . . ? C45 P3 C57 110.4(3) . . . ? C51 P3 C57 108.1(3) . . . ? P3 C45 C46 120.4(5) . . . ? P3 C45 C50 119.8(5) . . . ? C46 C45 C50 119.8(6) . . . ? C45 C46 C47 119.4(6) . . . ? C46 C47 C48 120.2(7) . . . ? C47 C48 C49 120.9(7) . . . ? C48 C49 C50 121.1(7) . . . ? C45 C50 C49 118.6(7) . . . ? P3 C51 C52 120.4(5) . . . ? P3 C51 C56 119.8(6) . . . ? C52 C51 C56 119.6(7) . . . ? C51 C52 C53 120.2(7) . . . ? C52 C53 C54 119.5(7) . . . ? C53 C54 C55 120.2(7) . . . ? C54 C55 C56 120.4(7) . . . ? C51 C56 C55 120.2(7) . . . ? P3 C57 C58 136.9(4) . . . ? P3 C57 C61 115.4(5) . . . ? C58 C57 C61 105.7(5) . . . ? C57 C58 C59 100.6(5) . . . ? C57 C58 C62 106.2(6) . . . ? C59 C58 C62 101.7(5) . . . ? C58 C59 C60 93.7(5) . . . ? C58 C59 C64 114.1(6) . . . ? C58 C59 C65 113.2(6) . . . ? C60 C59 C64 113.6(6) . . . ? C60 C59 C65 114.9(6) . . . ? C64 C59 C65 107.2(6) . . . ? C59 C60 C61 98.4(5) . . . ? C59 C60 C63 101.6(5) . . . ? C59 C60 C66 118.7(6) . . . ? C61 C60 C63 103.8(5) . . . ? C61 C60 C66 115.1(5) . . . ? C63 C60 C66 116.5(6) . . . ? C57 C61 C60 108.9(5) . . . ? C57 C61 O3 127.0(6) . . . ? C60 C61 O3 124.0(6) . . . ? C58 C62 C63 102.2(5) . . . ? C60 C63 C62 104.2(6) . . . ? C67 P4 C73 109.2(3) . . . ? C67 P4 C79 110.6(3) . . . ? C73 P4 C79 108.2(3) . . . ? P4 C67 C68 124.5(5) . . . ? P4 C67 C72 116.7(5) . . . ? C68 C67 C72 118.3(6) . . . ? C67 C68 C69 120.4(6) . . . ? C68 C69 C70 119.9(7) . . . ? C69 C70 C71 120.4(7) . . . ? C70 C71 C72 119.7(7) . . . ? C67 C72 C71 121.2(6) . . . ? P4 C73 C74 117.4(5) . . . ? P4 C73 C78 123.6(5) . . . ? C74 C73 C78 118.7(6) . . . ? C73 C74 C75 121.2(6) . . . ? C74 C75 C76 119.7(7) . . . ? C75 C76 C77 119.5(7) . . . ? C76 C77 C78 120.7(7) . . . ? C73 C78 C77 120.1(7) . . . ? P4 C79 C80 137.4(5) . . . ? P4 C79 C83 116.0(5) . . . ? C80 C79 C83 106.4(6) . . . ? C79 C80 C81 101.6(6) . . . ? C79 C80 C84 105.1(6) . . . ? C81 C80 C84 100.5(6) . . . ? C80 C81 C82 93.3(5) . . . ? C80 C81 C86 112.8(6) . . . ? C80 C81 C87 114.4(6) . . . ? C82 C81 C86 113.9(6) . . . ? C82 C81 C87 115.2(6) . . . ? C86 C81 C87 107.1(6) . . . ? C81 C82 C83 99.6(5) . . . ? C81 C82 C85 100.5(5) . . . ? C81 C82 C88 118.6(6) . . . ? C83 C82 C85 104.2(5) . . . ? C83 C82 C88 115.7(5) . . . ? C85 C82 C88 115.7(6) . . . ? C79 C83 C82 107.9(5) . . . ? C79 C83 O8 128.5(6) . . . ? C82 C83 O8 123.6(5) . . . ? C80 C84 C85 102.7(6) . . . ? C82 C85 C84 104.8(6) . . . ? C89 O6 C92 106.4(7) . . . ? O6 C89 C90 109.4(8) . . . ? C89 C90 C91 103.0(8) . . . ? C90 C91 C92 102.3(8) . . . ? O6 C92 C91 106.9(8) . . . ? C93 O7 C96 105.4(9) . . . ? O7 C93 C94 107.5(9) . . . ? C93 C94 C95 103(1) . . . ? C94 C95 C96 105(1) . . . ? O7 C96 C95 109.7(9) . . . ? data_stratos(6) _database_code_CSD 158618 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H36 N O P Pd' _chemical_formula_weight 575.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.9544(15) _cell_length_b 31.8046(15) _cell_length_c 11.0466(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.916(6) _cell_angle_gamma 90.00 _cell_volume 5575.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8006 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.2 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker AXS SMART CCD System' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18772 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.24 _reflns_number_total 10447 _reflns_number_gt 7555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART CCD System' _computing_cell_refinement 'Bruker AXS SMART CCD System' _computing_data_reduction 'Bruker AXS SMART CCD System' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP5' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(3) _refine_ls_number_reflns 10447 _refine_ls_number_parameters 641 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd' Pd 0.68665(3) 0.858538(11) 0.15121(5) 0.02231(17) Uani 1 d . . . P' P 0.67837(14) 0.91229(9) 0.28295(18) 0.0236(6) Uani 1 d . . . O' O 0.7689(3) 0.8979(2) 0.0625(5) 0.0324(17) Uani 1 d . . . N' N 0.7004(4) 0.8093(3) 0.0237(6) 0.0248(18) Uani 1 d . . . C1' C 0.7537(5) 0.9462(3) 0.2286(7) 0.025(2) Uani 1 d . . . C2' C 0.7824(5) 0.9333(3) 0.1225(7) 0.029(2) Uani 1 d . . . C3' C 0.8392(5) 0.9689(3) 0.0791(7) 0.033(2) Uani 1 d . . . C4' C 0.9185(4) 0.9665(2) 0.1804(6) 0.0533(19) Uani 1 d . . . H4'1 H 0.9385 0.9371 0.1918 0.064 Uiso 1 calc R . . H4'2 H 0.9655 0.9840 0.1570 0.064 Uiso 1 calc R . . C5' C 0.8858(4) 0.9832(2) 0.2962(6) 0.0537(17) Uani 1 d . . . H5'1 H 0.9127 1.0103 0.3216 0.064 Uiso 1 calc R . . H5'2 H 0.8953 0.9628 0.3639 0.064 Uiso 1 calc R . . C6' C 0.7913(5) 0.9889(3) 0.2561(7) 0.034(2) Uani 1 d . . . H6' H 0.7604 1.0065 0.3119 0.040 Uiso 1 calc R . . C7' C 0.7933(4) 1.00701(17) 0.1270(5) 0.0399(13) Uani 1 d . . . C8' C 0.8422(4) 1.04916(19) 0.1211(6) 0.0535(17) Uani 1 d . . . H8'1 H 0.8160 1.0706 0.1687 0.064 Uiso 1 calc R . . H8'2 H 0.8404 1.0584 0.0363 0.064 Uiso 1 calc R . . H8'3 H 0.9009 1.0451 0.1547 0.064 Uiso 1 calc R . . C9' C 0.7041(4) 1.0144(2) 0.0604(6) 0.0466(17) Uani 1 d . . . H9'1 H 0.6782 1.0388 0.0959 0.056 Uiso 1 calc R . . H9'2 H 0.6691 0.9895 0.0695 0.056 Uiso 1 calc R . . H9'3 H 0.7085 1.0195 -0.0262 0.056 Uiso 1 calc R . . C10' C 0.8569(5) 0.9672(4) -0.0507(8) 0.053(2) Uani 1 d . . . H10A H 0.8842 0.9404 -0.0663 0.063 Uiso 1 calc R . . H10B H 0.8943 0.9904 -0.0675 0.063 Uiso 1 calc R . . H10C H 0.8040 0.9695 -0.1037 0.063 Uiso 1 calc R . . C11' C 0.6084(5) 0.8167(3) 0.2196(7) 0.022(2) Uani 1 d . . . C12' C 0.5471(6) 0.8238(4) 0.2947(8) 0.036(3) Uani 1 d . . . H12' H 0.5377 0.8517 0.3203 0.043 Uiso 1 calc . . . C13' C 0.4982(6) 0.7919(4) 0.3351(7) 0.038(3) Uani 1 d . . . H13' H 0.4571 0.7977 0.3894 0.046 Uiso 1 calc . . . C14' C 0.5103(6) 0.7510(4) 0.2946(9) 0.048(3) Uani 1 d . . . H14' H 0.4789 0.7282 0.3225 0.057 Uiso 1 calc . . . C15' C 0.5699(7) 0.7442(4) 0.2119(10) 0.052(3) Uani 1 d . . . H15' H 0.5767 0.7167 0.1813 0.063 Uiso 1 calc . . . C16' C 0.6187(6) 0.7760(3) 0.1736(8) 0.030(2) Uani 1 d . . . C17' C 0.6851(5) 0.7700(3) 0.0907(8) 0.033(2) Uani 1 d . . . H17A H 0.7380 0.7612 0.1386 0.040 Uiso 1 calc R . . H17B H 0.6679 0.7474 0.0317 0.040 Uiso 1 calc R . . C18' C 0.7844(5) 0.8079(4) -0.0209(8) 0.038(3) Uani 1 d . . . H18A H 0.8272 0.8020 0.0472 0.045 Uiso 1 calc R . . H18B H 0.7964 0.8351 -0.0570 0.045 Uiso 1 calc R . . H18C H 0.7855 0.7858 -0.0825 0.045 Uiso 1 calc R . . C19' C 0.6338(5) 0.8154(4) -0.0783(7) 0.038(3) Uani 1 d . . . H19A H 0.6439 0.8417 -0.1203 0.046 Uiso 1 calc R . . H19B H 0.5787 0.8166 -0.0466 0.046 Uiso 1 calc R . . H19C H 0.6347 0.7918 -0.1354 0.046 Uiso 1 calc R . . C20' C 0.5762(6) 0.9378(3) 0.2684(7) 0.029(3) Uani 1 d . . . C21' C 0.5577(6) 0.9708(4) 0.3447(8) 0.041(3) Uani 1 d . . . H21' H 0.5975 0.9782 0.4112 0.049 Uiso 1 calc . . . C22' C 0.4801(6) 0.9936(4) 0.3254(8) 0.052(3) Uani 1 d . . . H22' H 0.4684 1.0162 0.3772 0.062 Uiso 1 calc . . . C23' C 0.4241(6) 0.9819(4) 0.2311(9) 0.053(3) Uani 1 d . . . H23' H 0.3710 0.9957 0.2196 0.063 Uiso 1 calc . . . C24' C 0.4418(6) 0.9507(5) 0.1515(8) 0.052(3) Uani 1 d . . . H24' H 0.4022 0.9443 0.0838 0.063 Uiso 1 calc . . . C25' C 0.5177(6) 0.9284(4) 0.1696(8) 0.040(3) Uani 1 d . . . H25' H 0.5294 0.9068 0.1144 0.048 Uiso 1 calc . . . C26' C 0.7021(5) 0.9060(3) 0.4483(7) 0.030(2) Uani 1 d . . . C27' C 0.7843(5) 0.9127(4) 0.5021(8) 0.040(3) Uani 1 d . . . H27' H 0.8276 0.9206 0.4536 0.048 Uiso 1 calc . . . C28' C 0.8020(5) 0.9077(4) 0.6268(8) 0.048(3) Uani 1 d . . . H28' H 0.8577 0.9127 0.6634 0.058 Uiso 1 calc . . . C29' C 0.7409(6) 0.8957(4) 0.6983(7) 0.039(2) Uani 1 d . . . H29' H 0.7540 0.8920 0.7835 0.046 Uiso 1 calc . . . C30' C 0.6610(6) 0.8892(4) 0.6451(8) 0.047(3) Uani 1 d . . . H30' H 0.6181 0.8811 0.6940 0.056 Uiso 1 calc . . . C31' C 0.6416(5) 0.8942(4) 0.5215(7) 0.038(3) Uani 1 d . . . H31' H 0.5856 0.8893 0.4864 0.045 Uiso 1 calc . . . Pd Pd 0.81635(3) 0.716832(11) 0.35335(5) 0.02347(18) Uani 1 d . . . P P 0.82429(14) 0.66254(10) 0.22394(19) 0.0254(6) Uani 1 d . . . O O 0.7378(4) 0.6772(2) 0.4472(5) 0.0320(17) Uani 1 d . . . N N 0.8029(4) 0.7673(3) 0.4749(6) 0.028(2) Uani 1 d . . . C1 C 0.7514(5) 0.6296(3) 0.2835(7) 0.026(2) Uani 1 d . . . C2 C 0.7241(5) 0.6421(3) 0.3909(7) 0.025(2) Uani 1 d . . . C3 C 0.6768(5) 0.6060(4) 0.4386(7) 0.035(2) Uani 1 d . . . C4 C 0.7476(4) 0.5727(2) 0.4804(5) 0.0481(16) Uani 1 d . . . H4A H 0.7938 0.5858 0.5340 0.058 Uiso 1 calc R . . H4B H 0.7241 0.5490 0.5243 0.058 Uiso 1 calc R . . C5 C 0.7789(4) 0.5577(2) 0.3618(7) 0.0555(18) Uani 1 d . . . H5A H 0.7697 0.5271 0.3502 0.067 Uiso 1 calc R . . H5B H 0.8394 0.5640 0.3598 0.067 Uiso 1 calc R . . C6 C 0.7240(4) 0.5832(3) 0.2649(7) 0.033(2) Uani 1 d . . . H6 H 0.7223 0.5725 0.1797 0.039 Uiso 1 calc R . . C7 C 0.6375(3) 0.58431(17) 0.3195(5) 0.0324(12) Uani 1 d . . . C8 C 0.5992(4) 0.5410(2) 0.3367(6) 0.0472(16) Uani 1 d . . . H8A H 0.5521 0.5436 0.3866 0.057 Uiso 1 calc R . . H8B H 0.6421 0.5223 0.3773 0.057 Uiso 1 calc R . . H8C H 0.5786 0.5293 0.2570 0.057 Uiso 1 calc R . . C9 C 0.5698(4) 0.6118(2) 0.2463(6) 0.0457(17) Uani 1 d . . . H9A H 0.5897 0.6409 0.2446 0.055 Uiso 1 calc R . . H9B H 0.5173 0.6107 0.2852 0.055 Uiso 1 calc R . . H9C H 0.5596 0.6010 0.1629 0.055 Uiso 1 calc R . . C10 C 0.6191(5) 0.6166(3) 0.5369(7) 0.051(3) Uani 1 d . . . H10D H 0.6528 0.6283 0.6081 0.061 Uiso 1 calc R . . H10E H 0.5908 0.5909 0.5605 0.061 Uiso 1 calc R . . H10F H 0.5768 0.6372 0.5049 0.061 Uiso 1 calc R . . C11 C 0.8922(5) 0.7565(3) 0.2834(7) 0.030(3) Uani 1 d . . . C12 C 0.9556(5) 0.7508(3) 0.2017(7) 0.028(2) Uani 1 d . . . H12 H 0.9666 0.7235 0.1726 0.034 Uiso 1 calc . . . C13 C 1.0020(5) 0.7855(4) 0.1642(8) 0.044(3) Uani 1 d . . . H13 H 1.0436 0.7810 0.1100 0.053 Uiso 1 calc . . . C14 C 0.9885(7) 0.8258(4) 0.2041(10) 0.049(3) Uani 1 d . . . H14 H 1.0199 0.8485 0.1763 0.059 Uiso 1 calc . . . C15 C 0.9299(6) 0.8329(3) 0.2834(8) 0.039(3) Uani 1 d . . . H15 H 0.9212 0.8605 0.3126 0.047 Uiso 1 calc . . . C16 C 0.8821(6) 0.7986(4) 0.3218(8) 0.035(3) Uani 1 d . . . C17 C 0.8153(6) 0.8069(3) 0.4074(8) 0.037(3) Uani 1 d . . . H17C H 0.8339 0.8297 0.4650 0.044 Uiso 1 calc R . . H17D H 0.7619 0.8155 0.3605 0.044 Uiso 1 calc R . . C18 C 0.8676(5) 0.7637(4) 0.5809(7) 0.036(2) Uani 1 d . . . H18D H 0.9233 0.7699 0.5551 0.044 Uiso 1 calc R . . H18E H 0.8673 0.7351 0.6137 0.044 Uiso 1 calc R . . H18F H 0.8550 0.7838 0.6438 0.044 Uiso 1 calc R . . C19 C 0.7185(5) 0.7683(4) 0.5226(7) 0.037(3) Uani 1 d . . . H19D H 0.7119 0.7433 0.5727 0.044 Uiso 1 calc R . . H19E H 0.6741 0.7687 0.4543 0.044 Uiso 1 calc R . . H19F H 0.7141 0.7936 0.5722 0.044 Uiso 1 calc R . . C20 C 0.7960(5) 0.6684(3) 0.0605(7) 0.027(2) Uani 1 d . . . C21 C 0.7128(6) 0.6613(3) 0.0134(8) 0.037(2) Uani 1 d . . . H21 H 0.6730 0.6523 0.0665 0.044 Uiso 1 calc . . . C22 C 0.6865(6) 0.6670(4) -0.1104(8) 0.047(2) Uani 1 d . . . H22 H 0.6297 0.6616 -0.1412 0.056 Uiso 1 calc . . . C23 C 0.7424(7) 0.6802(4) -0.1855(8) 0.059(3) Uani 1 d . . . H23 H 0.7245 0.6845 -0.2693 0.071 Uiso 1 calc . . . C24 C 0.8254(7) 0.6875(4) -0.1421(7) 0.063(4) Uani 1 d . . . H24 H 0.8641 0.6967 -0.1965 0.075 Uiso 1 calc . . . C25 C 0.8529(6) 0.6817(4) -0.0195(8) 0.047(3) Uani 1 d . . . H25 H 0.9101 0.6867 0.0096 0.057 Uiso 1 calc . . . C26 C 0.9272(5) 0.6361(3) 0.2323(8) 0.027(2) Uani 1 d . . . C27 C 0.9878(6) 0.6478(4) 0.3258(7) 0.037(3) Uani 1 d . . . H27 H 0.9763 0.6701 0.3786 0.044 Uiso 1 calc . . . C28 C 1.0635(7) 0.6276(5) 0.3428(9) 0.062(4) Uani 1 d . . . H28 H 1.1049 0.6363 0.4060 0.074 Uiso 1 calc . . . C29 C 1.0798(6) 0.5943(4) 0.2671(9) 0.060(4) Uani 1 d . . . H29 H 1.1307 0.5788 0.2806 0.072 Uiso 1 calc . . . C30 C 1.0190(6) 0.5843(3) 0.1701(8) 0.041(2) Uani 1 d . . . H30 H 1.0313 0.5628 0.1146 0.049 Uiso 1 calc . . . C31 C 0.9447(5) 0.6037(3) 0.1532(7) 0.031(2) Uani 1 d . . . H31 H 0.9042 0.5957 0.0882 0.037 Uiso 1 calc . . . 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 Pd' 0.0225(3) 0.0221(5) 0.0224(3) -0.0016(3) 0.0026(3) 0.0015(3) P' 0.0254(12) 0.0238(16) 0.0221(10) -0.0034(10) 0.0047(9) 0.0030(11) O' 0.034(3) 0.034(5) 0.032(3) -0.007(3) 0.020(3) -0.007(3) N' 0.032(4) 0.018(4) 0.023(4) -0.001(3) -0.004(3) -0.002(3) C1' 0.019(4) 0.035(6) 0.023(4) -0.007(4) 0.007(3) -0.002(4) C2' 0.021(4) 0.034(6) 0.031(4) -0.007(4) 0.004(3) -0.012(4) C3' 0.029(4) 0.026(4) 0.047(4) 0.003(4) 0.013(3) -0.014(3) C4' 0.023(3) 0.061(5) 0.076(5) 0.014(4) 0.002(3) -0.017(3) C5' 0.044(4) 0.056(5) 0.058(4) 0.004(3) -0.013(3) -0.023(3) C6' 0.044(4) 0.031(5) 0.025(3) -0.007(3) 0.000(3) -0.010(4) C7' 0.051(4) 0.029(3) 0.040(3) -0.005(3) 0.007(3) -0.019(3) C8' 0.072(5) 0.040(4) 0.049(4) 0.002(3) 0.007(3) -0.028(4) C9' 0.058(4) 0.041(4) 0.039(3) 0.005(3) 0.001(3) 0.000(3) C10' 0.057(5) 0.044(5) 0.062(5) -0.012(4) 0.028(4) -0.012(4) C11' 0.026(4) 0.022(5) 0.017(4) 0.011(4) -0.004(3) -0.013(4) C12' 0.039(6) 0.040(8) 0.026(5) 0.003(5) -0.005(4) -0.004(5) C13' 0.038(6) 0.049(7) 0.026(5) -0.004(5) -0.004(4) -0.003(5) C14' 0.042(6) 0.054(9) 0.047(6) 0.013(6) 0.003(5) -0.022(6) C15' 0.064(7) 0.038(7) 0.053(6) 0.000(6) 0.000(5) -0.001(6) C16' 0.040(5) 0.014(5) 0.033(5) 0.004(4) -0.014(4) -0.005(4) C17' 0.042(5) 0.025(6) 0.033(5) -0.007(5) 0.003(4) 0.005(5) C18' 0.030(5) 0.042(8) 0.043(6) -0.008(5) 0.016(4) 0.006(5) C19' 0.043(5) 0.043(6) 0.027(5) -0.002(4) -0.005(4) 0.002(5) C20' 0.042(5) 0.031(7) 0.015(4) 0.004(4) 0.012(4) 0.004(5) C21' 0.039(6) 0.044(8) 0.039(6) 0.007(5) 0.003(5) 0.010(6) C22' 0.058(6) 0.064(8) 0.036(5) 0.012(5) 0.019(5) 0.040(6) C23' 0.047(6) 0.057(8) 0.054(6) 0.004(6) 0.005(5) 0.047(6) C24' 0.049(6) 0.065(8) 0.041(5) 0.003(5) -0.006(5) 0.030(6) C25' 0.041(5) 0.048(7) 0.032(5) 0.006(5) 0.006(4) 0.018(5) C26' 0.035(5) 0.031(7) 0.022(4) -0.002(4) -0.003(3) 0.005(5) C27' 0.031(4) 0.053(7) 0.038(4) 0.001(4) 0.008(3) 0.000(5) C28' 0.037(4) 0.062(7) 0.041(5) 0.004(5) -0.015(4) -0.009(4) C29' 0.055(5) 0.043(5) 0.018(3) 0.005(3) 0.006(3) 0.000(4) C30' 0.041(4) 0.063(8) 0.037(5) 0.000(4) 0.008(3) -0.022(4) C31' 0.035(5) 0.054(7) 0.023(4) -0.004(4) -0.001(4) 0.003(5) Pd 0.0229(3) 0.0244(5) 0.0228(3) 0.0005(3) 0.0011(3) 0.0000(3) P 0.0246(12) 0.0272(17) 0.0249(11) 0.0020(11) 0.0050(9) -0.0030(12) O 0.033(3) 0.030(4) 0.033(3) -0.009(3) 0.006(3) -0.009(3) N 0.020(4) 0.039(6) 0.021(4) -0.002(4) -0.005(3) 0.006(4) C1 0.031(4) 0.018(5) 0.028(4) -0.004(3) 0.001(3) -0.007(4) C2 0.023(4) 0.032(6) 0.021(3) 0.003(3) 0.004(3) 0.003(4) C3 0.028(4) 0.051(6) 0.026(3) -0.007(3) 0.004(3) -0.012(4) C4 0.038(3) 0.056(4) 0.048(4) 0.022(3) -0.009(3) -0.021(3) C5 0.036(4) 0.032(4) 0.099(6) 0.010(4) 0.012(4) -0.002(3) C6 0.022(3) 0.033(5) 0.044(4) -0.004(4) 0.010(3) -0.002(3) C7 0.023(3) 0.034(3) 0.040(3) -0.002(3) 0.004(2) -0.009(2) C8 0.043(3) 0.047(4) 0.053(4) -0.009(3) 0.011(3) -0.028(3) C9 0.034(3) 0.063(5) 0.038(4) 0.003(4) -0.005(3) -0.001(3) C10 0.056(5) 0.062(6) 0.039(4) -0.014(4) 0.028(3) -0.035(5) C11 0.022(5) 0.039(7) 0.026(4) 0.002(4) -0.008(4) 0.011(4) C12 0.020(4) 0.035(7) 0.029(5) 0.003(4) 0.001(4) -0.002(4) C13 0.026(5) 0.075(9) 0.032(5) 0.024(5) 0.003(4) -0.022(5) C14 0.068(8) 0.032(7) 0.044(6) 0.016(5) -0.013(6) -0.018(6) C15 0.059(7) 0.022(6) 0.033(5) 0.008(4) -0.006(5) -0.018(5) C16 0.029(5) 0.051(8) 0.024(4) 0.006(5) 0.000(4) 0.001(5) C17 0.050(6) 0.023(6) 0.034(5) 0.007(4) -0.012(4) 0.004(5) C18 0.039(5) 0.044(6) 0.024(4) 0.000(4) -0.012(4) 0.004(5) C19 0.041(5) 0.041(8) 0.027(5) -0.008(5) -0.002(4) 0.009(5) C20 0.046(5) 0.012(5) 0.025(4) -0.001(3) 0.009(4) 0.000(4) C21 0.049(5) 0.027(5) 0.030(4) 0.000(4) -0.009(3) 0.001(4) C22 0.062(5) 0.037(6) 0.039(4) 0.003(4) -0.007(4) 0.008(4) C23 0.093(7) 0.045(6) 0.034(5) 0.007(4) -0.021(5) -0.020(6) C24 0.104(8) 0.064(8) 0.021(5) 0.009(5) 0.011(5) -0.005(6) C25 0.059(6) 0.046(7) 0.037(5) 0.011(5) 0.005(5) -0.023(5) C26 0.023(4) 0.023(6) 0.036(5) 0.009(4) 0.009(4) 0.009(4) C27 0.040(5) 0.046(7) 0.024(4) -0.007(4) 0.000(4) 0.008(5) C28 0.066(7) 0.081(10) 0.035(5) -0.007(6) -0.012(5) 0.032(7) C29 0.057(7) 0.081(11) 0.040(6) 0.009(6) -0.002(5) 0.022(7) C30 0.057(6) 0.027(5) 0.041(5) -0.008(4) 0.010(5) 0.005(5) C31 0.036(5) 0.029(7) 0.029(5) -0.010(5) 0.008(4) 0.004(5) _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 Pd' C11' 2.023(8) . ? Pd' O' 2.124(6) . ? Pd' N' 2.133(8) . ? Pd' P' 2.258(3) . ? P' C1' 1.765(9) . ? P' C20' 1.814(9) . ? P' C26' 1.838(8) . ? O' C2' 1.313(11) . ? N' C18' 1.476(9) . ? N' C19' 1.479(9) . ? N' C17' 1.483(12) . ? C1' C2' 1.364(11) . ? C1' C6' 1.503(13) . ? C2' C3' 1.557(12) . ? C3' C10' 1.492(10) . ? C3' C7' 1.537(11) . ? C3' C4' 1.603(10) . ? C4' C5' 1.527(9) . ? C5' C6' 1.538(9) . ? C6' C7' 1.541(9) . ? C7' C9' 1.552(8) . ? C7' C8' 1.555(7) . ? C11' C12' 1.365(11) . ? C11' C16' 1.408(13) . ? C12' C13' 1.381(14) . ? C13' C14' 1.397(16) . ? C14' C15' 1.401(14) . ? C15' C16' 1.367(14) . ? C16' C17' 1.482(12) . ? C20' C25' 1.393(11) . ? C20' C21' 1.396(14) . ? C21' C22' 1.431(12) . ? C22' C23' 1.353(13) . ? C23' C24' 1.374(15) . ? C24' C25' 1.402(13) . ? C26' C31' 1.374(12) . ? C26' C27' 1.400(10) . ? C27' C28' 1.386(11) . ? C28' C29' 1.371(12) . ? C29' C30' 1.364(11) . ? C30' C31' 1.377(10) . ? Pd C11 1.961(10) . ? Pd N 2.118(8) . ? Pd O 2.122(6) . ? Pd P 2.254(3) . ? P C1 1.744(9) . ? P C20 1.825(8) . ? P C26 1.838(9) . ? O C2 1.286(11) . ? N C18 1.484(8) . ? N C17 1.486(13) . ? N C19 1.496(9) . ? C1 C2 1.364(11) . ? C1 C6 1.545(13) . ? C2 C3 1.500(13) . ? C3 C10 1.532(10) . ? C3 C7 1.558(9) . ? C3 C4 1.582(11) . ? C4 C5 1.525(8) . ? C5 C6 1.542(10) . ? C6 C7 1.563(9) . ? C7 C8 1.527(7) . ? C7 C9 1.550(8) . ? C11 C16 1.418(14) . ? C11 C12 1.435(11) . ? C12 C13 1.415(13) . ? C13 C14 1.377(16) . ? C14 C15 1.364(14) . ? C15 C16 1.423(13) . ? C16 C17 1.518(13) . ? C20 C21 1.394(11) . ? C20 C25 1.396(11) . ? C21 C22 1.401(11) . ? C22 C23 1.345(13) . ? C23 C24 1.381(13) . ? C24 C25 1.393(11) . ? C26 C27 1.391(11) . ? C26 C31 1.398(13) . ? C27 C28 1.363(14) . ? C28 C29 1.390(17) . ? C29 C30 1.407(13) . ? C30 C31 1.333(12) . ? 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 C11' Pd' O' 173.6(3) . . ? C11' Pd' N' 82.7(3) . . ? O' Pd' N' 91.0(3) . . ? C11' Pd' P' 100.2(3) . . ? O' Pd' P' 86.06(18) . . ? N' Pd' P' 177.0(2) . . ? C1' P' C20' 109.5(4) . . ? C1' P' C26' 109.1(4) . . ? C20' P' C26' 103.2(4) . . ? C1' P' Pd' 99.0(3) . . ? C20' P' Pd' 113.2(3) . . ? C26' P' Pd' 122.6(4) . . ? C2' O' Pd' 110.5(5) . . ? C18' N' C19' 110.8(6) . . ? C18' N' C17' 110.1(7) . . ? C19' N' C17' 110.4(7) . . ? C18' N' Pd' 113.6(6) . . ? C19' N' Pd' 107.0(6) . . ? C17' N' Pd' 104.8(5) . . ? C2' C1' C6' 106.4(8) . . ? C2' C1' P' 114.2(7) . . ? C6' C1' P' 138.9(7) . . ? O' C2' C1' 129.7(9) . . ? O' C2' C3' 122.7(7) . . ? C1' C2' C3' 107.6(8) . . ? C10' C3' C7' 120.3(8) . . ? C10' C3' C2' 116.3(8) . . ? C7' C3' C2' 98.9(6) . . ? C10' C3' C4' 117.0(7) . . ? C7' C3' C4' 99.7(6) . . ? C2' C3' C4' 101.1(6) . . ? C5' C4' C3' 104.7(6) . . ? C4' C5' C6' 102.1(5) . . ? C1' C6' C5' 108.1(7) . . ? C1' C6' C7' 101.4(6) . . ? C5' C6' C7' 101.4(6) . . ? C3' C7' C6' 94.6(6) . . ? C3' C7' C9' 113.7(5) . . ? C6' C7' C9' 112.9(5) . . ? C3' C7' C8' 114.0(5) . . ? C6' C7' C8' 114.8(5) . . ? C9' C7' C8' 106.8(5) . . ? C12' C11' C16' 119.2(8) . . ? C12' C11' Pd' 128.9(8) . . ? C16' C11' Pd' 111.8(7) . . ? C11' C12' C13' 122.7(10) . . ? C12' C13' C14' 118.6(9) . . ? C13' C14' C15' 118.5(11) . . ? C16' C15' C14' 122.3(11) . . ? C15' C16' C11' 118.5(9) . . ? C15' C16' C17' 124.3(10) . . ? C11' C16' C17' 117.2(8) . . ? N' C17' C16' 111.5(8) . . ? C25' C20' C21' 118.0(9) . . ? C25' C20' P' 119.7(7) . . ? C21' C20' P' 121.8(7) . . ? C20' C21' C22' 121.6(9) . . ? C23' C22' C21' 118.0(9) . . ? C22' C23' C24' 121.8(8) . . ? C23' C24' C25' 120.5(9) . . ? C20' C25' C24' 120.1(9) . . ? C31' C26' C27' 118.4(7) . . ? C31' C26' P' 122.0(6) . . ? C27' C26' P' 119.6(7) . . ? C28' C27' C26' 119.4(8) . . ? C29' C28' C27' 121.4(8) . . ? C30' C29' C28' 118.8(8) . . ? C29' C30' C31' 121.0(9) . . ? C26' C31' C30' 121.0(8) . . ? C11 Pd N 82.5(4) . . ? C11 Pd O 173.8(3) . . ? N Pd O 92.1(3) . . ? C11 Pd P 99.6(3) . . ? N Pd P 177.36(18) . . ? O Pd P 85.93(19) . . ? C1 P C20 109.1(4) . . ? C1 P C26 109.4(4) . . ? C20 P C26 103.0(4) . . ? C1 P Pd 97.9(3) . . ? C20 P Pd 121.7(3) . . ? C26 P Pd 115.3(3) . . ? C2 O Pd 111.0(5) . . ? C18 N C17 110.0(8) . . ? C18 N C19 107.6(6) . . ? C17 N C19 109.3(8) . . ? C18 N Pd 109.5(6) . . ? C17 N Pd 107.2(5) . . ? C19 N Pd 113.2(6) . . ? C2 C1 C6 106.4(8) . . ? C2 C1 P 115.9(7) . . ? C6 C1 P 135.6(7) . . ? O C2 C1 128.4(9) . . ? O C2 C3 124.2(8) . . ? C1 C2 C3 107.4(9) . . ? C2 C3 C10 116.2(9) . . ? C2 C3 C7 102.5(6) . . ? C10 C3 C7 118.4(6) . . ? C2 C3 C4 104.2(6) . . ? C10 C3 C4 113.8(7) . . ? C7 C3 C4 99.4(7) . . ? C5 C4 C3 104.2(5) . . ? C4 C5 C6 102.6(5) . . ? C5 C6 C1 106.2(6) . . ? C5 C6 C7 101.8(6) . . ? C1 C6 C7 100.2(7) . . ? C8 C7 C9 107.9(5) . . ? C8 C7 C3 115.2(6) . . ? C9 C7 C3 112.9(6) . . ? C8 C7 C6 114.1(6) . . ? C9 C7 C6 114.0(5) . . ? C3 C7 C6 92.3(5) . . ? C16 C11 C12 114.6(9) . . ? C16 C11 Pd 113.3(7) . . ? C12 C11 Pd 132.1(8) . . ? C13 C12 C11 120.6(10) . . ? C14 C13 C12 121.8(9) . . ? C15 C14 C13 120.1(10) . . ? C14 C15 C16 119.1(10) . . ? C11 C16 C15 123.7(9) . . ? C11 C16 C17 117.3(9) . . ? C15 C16 C17 119.0(10) . . ? N C17 C16 107.7(8) . . ? C21 C20 C25 118.0(8) . . ? C21 C20 P 118.8(7) . . ? C25 C20 P 123.1(7) . . ? C20 C21 C22 121.4(9) . . ? C23 C22 C21 119.5(9) . . ? C22 C23 C24 120.8(9) . . ? C23 C24 C25 120.6(9) . . ? C24 C25 C20 119.8(9) . . ? C27 C26 C31 119.5(8) . . ? C27 C26 P 117.7(7) . . ? C31 C26 P 122.7(7) . . ? C28 C27 C26 121.0(9) . . ? C27 C28 C29 119.5(9) . . ? C28 C29 C30 118.4(9) . . ? C31 C30 C29 122.3(9) . . ? C30 C31 C26 119.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11' Pd' P' C1' 175.3(4) . . . . ? O' Pd' P' C1' -5.7(3) . . . . ? N' Pd' P' C1' 12(4) . . . . ? C11' Pd' P' C20' -68.9(4) . . . . ? O' Pd' P' C20' 110.0(4) . . . . ? N' Pd' P' C20' 128(3) . . . . ? C11' Pd' P' C26' 55.7(4) . . . . ? O' Pd' P' C26' -125.3(4) . . . . ? N' Pd' P' C26' -108(4) . . . . ? C11' Pd' O' C2' 174(2) . . . . ? N' Pd' O' C2' -175.7(6) . . . . ? P' Pd' O' C2' 3.3(5) . . . . ? C11' Pd' N' C18' -148.3(6) . . . . ? O' Pd' N' C18' 32.8(6) . . . . ? P' Pd' N' C18' 15(4) . . . . ? C11' Pd' N' C19' 89.1(6) . . . . ? O' Pd' N' C19' -89.7(6) . . . . ? P' Pd' N' C19' -107(3) . . . . ? C11' Pd' N' C17' -28.1(5) . . . . ? O' Pd' N' C17' 153.1(5) . . . . ? P' Pd' N' C17' 136(3) . . . . ? C20' P' C1' C2' -110.4(7) . . . . ? C26' P' C1' C2' 137.4(7) . . . . ? Pd' P' C1' C2' 8.2(7) . . . . ? C20' P' C1' C6' 60.7(10) . . . . ? C26' P' C1' C6' -51.5(10) . . . . ? Pd' P' C1' C6' 179.3(9) . . . . ? Pd' O' C2' C1' 1.8(12) . . . . ? Pd' O' C2' C3' -179.1(6) . . . . ? C6' C1' C2' O' 178.4(8) . . . . ? P' C1' C2' O' -7.7(13) . . . . ? C6' C1' C2' C3' -0.8(9) . . . . ? P' C1' C2' C3' 173.1(6) . . . . ? O' C2' C3' C10' 17.8(12) . . . . ? C1' C2' C3' C10' -163.0(8) . . . . ? O' C2' C3' C7' 148.2(8) . . . . ? C1' C2' C3' C7' -32.6(8) . . . . ? O' C2' C3' C4' -110.0(9) . . . . ? C1' C2' C3' C4' 69.2(9) . . . . ? C10' C3' C4' C5' 161.9(8) . . . . ? C7' C3' C4' C5' 30.4(7) . . . . ? C2' C3' C4' C5' -70.8(7) . . . . ? C3' C4' C5' C6' 5.9(8) . . . . ? C2' C1' C6' C5' -72.0(8) . . . . ? P' C1' C6' C5' 116.4(9) . . . . ? C2' C1' C6' C7' 34.1(9) . . . . ? P' C1' C6' C7' -137.5(8) . . . . ? C4' C5' C6' C1' 65.5(7) . . . . ? C4' C5' C6' C7' -40.6(7) . . . . ? C10' C3' C7' C6' 177.3(8) . . . . ? C2' C3' C7' C6' 49.7(6) . . . . ? C4' C3' C7' C6' -53.3(6) . . . . ? C10' C3' C7' C9' 59.8(9) . . . . ? C2' C3' C7' C9' -67.9(7) . . . . ? C4' C3' C7' C9' -170.8(5) . . . . ? C10' C3' C7' C8' -62.9(9) . . . . ? C2' C3' C7' C8' 169.4(5) . . . . ? C4' C3' C7' C8' 66.4(6) . . . . ? C1' C6' C7' C3' -51.9(7) . . . . ? C5' C6' C7' C3' 59.5(7) . . . . ? C1' C6' C7' C9' 66.3(8) . . . . ? C5' C6' C7' C9' 177.6(6) . . . . ? C1' C6' C7' C8' -170.9(6) . . . . ? C5' C6' C7' C8' -59.6(8) . . . . ? O' Pd' C11' C12' -151(2) . . . . ? N' Pd' C11' C12' -161.1(7) . . . . ? P' Pd' C11' C12' 19.7(7) . . . . ? O' Pd' C11' C16' 25(3) . . . . ? N' Pd' C11' C16' 14.7(5) . . . . ? P' Pd' C11' C16' -164.5(5) . . . . ? C16' C11' C12' C13' 4.8(12) . . . . ? Pd' C11' C12' C13' -179.7(6) . . . . ? C11' C12' C13' C14' -1.9(14) . . . . ? C12' C13' C14' C15' -1.9(14) . . . . ? C13' C14' C15' C16' 2.7(15) . . . . ? C14' C15' C16' C11' 0.1(14) . . . . ? C14' C15' C16' C17' 177.1(8) . . . . ? C12' C11' C16' C15' -3.8(12) . . . . ? Pd' C11' C16' C15' 179.9(7) . . . . ? C12' C11' C16' C17' 179.0(7) . . . . ? Pd' C11' C16' C17' 2.7(9) . . . . ? C18' N' C17' C16' 159.0(7) . . . . ? C19' N' C17' C16' -78.3(9) . . . . ? Pd' N' C17' C16' 36.5(7) . . . . ? C15' C16' C17' N' 154.9(8) . . . . ? C11' C16' C17' N' -28.1(10) . . . . ? C1' P' C20' C25' 98.7(9) . . . . ? C26' P' C20' C25' -145.2(8) . . . . ? Pd' P' C20' C25' -10.6(9) . . . . ? C1' P' C20' C21' -73.0(9) . . . . ? C26' P' C20' C21' 43.0(9) . . . . ? Pd' P' C20' C21' 177.6(7) . . . . ? C25' C20' C21' C22' 1.8(15) . . . . ? P' C20' C21' C22' 173.7(8) . . . . ? C20' C21' C22' C23' 0.9(17) . . . . ? C21' C22' C23' C24' -3.4(19) . . . . ? C22' C23' C24' C25' 3(2) . . . . ? C21' C20' C25' C24' -2.1(16) . . . . ? P' C20' C25' C24' -174.1(9) . . . . ? C23' C24' C25' C20' -0.3(18) . . . . ? C1' P' C26' C31' 157.2(9) . . . . ? C20' P' C26' C31' 40.8(10) . . . . ? Pd' P' C26' C31' -88.2(9) . . . . ? C1' P' C26' C27' -23.9(11) . . . . ? C20' P' C26' C27' -140.3(9) . . . . ? Pd' P' C26' C27' 90.7(10) . . . . ? C31' C26' C27' C28' -0.7(17) . . . . ? P' C26' C27' C28' -179.6(9) . . . . ? C26' C27' C28' C29' 0.9(19) . . . . ? C27' C28' C29' C30' -0.8(19) . . . . ? C28' C29' C30' C31' 0.5(19) . . . . ? C27' C26' C31' C30' 0.4(17) . . . . ? P' C26' C31' C30' 179.3(9) . . . . ? C29' C30' C31' C26' -0.3(19) . . . . ? C11 Pd P C1 -176.5(4) . . . . ? N Pd P C1 -37(5) . . . . ? O Pd P C1 6.3(3) . . . . ? C11 Pd P C20 -58.2(4) . . . . ? N Pd P C20 82(5) . . . . ? O Pd P C20 124.7(4) . . . . ? C11 Pd P C26 67.5(4) . . . . ? N Pd P C26 -153(5) . . . . ? O Pd P C26 -109.7(4) . . . . ? C11 Pd O C2 -157(3) . . . . ? N Pd O C2 174.5(6) . . . . ? P Pd O C2 -3.7(5) . . . . ? C11 Pd N C18 -89.8(6) . . . . ? O Pd N C18 87.3(6) . . . . ? P Pd N C18 130(4) . . . . ? C11 Pd N C17 29.6(5) . . . . ? O Pd N C17 -153.4(5) . . . . ? P Pd N C17 -111(5) . . . . ? C11 Pd N C19 150.2(6) . . . . ? O Pd N C19 -32.8(6) . . . . ? P Pd N C19 10(5) . . . . ? C20 P C1 C2 -136.7(7) . . . . ? C26 P C1 C2 111.3(7) . . . . ? Pd P C1 C2 -9.2(7) . . . . ? C20 P C1 C6 62.4(9) . . . . ? C26 P C1 C6 -49.6(9) . . . . ? Pd P C1 C6 -170.0(8) . . . . ? Pd O C2 C1 -1.9(11) . . . . ? Pd O C2 C3 174.9(6) . . . . ? C6 C1 C2 O 174.6(8) . . . . ? P C1 C2 O 8.5(13) . . . . ? C6 C1 C2 C3 -2.6(9) . . . . ? P C1 C2 C3 -168.7(6) . . . . ? O C2 C3 C10 20.0(12) . . . . ? C1 C2 C3 C10 -162.7(7) . . . . ? O C2 C3 C7 150.7(8) . . . . ? C1 C2 C3 C7 -32.0(9) . . . . ? O C2 C3 C4 -106.1(9) . . . . ? C1 C2 C3 C4 71.3(8) . . . . ? C2 C3 C4 C5 -68.6(7) . . . . ? C10 C3 C4 C5 163.9(7) . . . . ? C7 C3 C4 C5 37.0(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C4 C5 C6 C1 67.4(7) . . . . ? C4 C5 C6 C7 -37.0(7) . . . . ? C2 C1 C6 C5 -69.7(8) . . . . ? P C1 C6 C5 92.3(9) . . . . ? C2 C1 C6 C7 35.8(8) . . . . ? P C1 C6 C7 -162.1(7) . . . . ? C2 C3 C7 C8 168.4(6) . . . . ? C10 C3 C7 C8 -62.3(11) . . . . ? C4 C3 C7 C8 61.4(7) . . . . ? C2 C3 C7 C9 -67.1(7) . . . . ? C10 C3 C7 C9 62.2(10) . . . . ? C4 C3 C7 C9 -174.0(5) . . . . ? C2 C3 C7 C6 50.2(7) . . . . ? C10 C3 C7 C6 179.6(9) . . . . ? C4 C3 C7 C6 -56.7(6) . . . . ? C5 C6 C7 C8 -60.5(7) . . . . ? C1 C6 C7 C8 -169.6(5) . . . . ? C5 C6 C7 C9 174.9(6) . . . . ? C1 C6 C7 C9 65.8(7) . . . . ? C5 C6 C7 C3 58.5(7) . . . . ? C1 C6 C7 C3 -50.6(7) . . . . ? N Pd C11 C16 -16.0(6) . . . . ? O Pd C11 C16 -45(3) . . . . ? P Pd C11 C16 162.3(5) . . . . ? N Pd C11 C12 163.7(7) . . . . ? O Pd C11 C12 135(3) . . . . ? P Pd C11 C12 -18.0(7) . . . . ? C16 C11 C12 C13 -0.6(11) . . . . ? Pd C11 C12 C13 179.6(6) . . . . ? C11 C12 C13 C14 0.1(13) . . . . ? C12 C13 C14 C15 1.0(15) . . . . ? C13 C14 C15 C16 -1.4(14) . . . . ? C12 C11 C16 C15 0.2(12) . . . . ? Pd C11 C16 C15 -180.0(6) . . . . ? C12 C11 C16 C17 179.4(6) . . . . ? Pd C11 C16 C17 -0.8(9) . . . . ? C14 C15 C16 C11 0.8(14) . . . . ? C14 C15 C16 C17 -178.4(8) . . . . ? C18 N C17 C16 83.5(8) . . . . ? C19 N C17 C16 -158.6(6) . . . . ? Pd N C17 C16 -35.6(7) . . . . ? C11 C16 C17 N 25.6(10) . . . . ? C15 C16 C17 N -155.2(7) . . . . ? C1 P C20 C21 23.2(10) . . . . ? C26 P C20 C21 139.4(8) . . . . ? Pd P C20 C21 -89.6(8) . . . . ? C1 P C20 C25 -160.1(9) . . . . ? C26 P C20 C25 -43.9(10) . . . . ? Pd P C20 C25 87.2(9) . . . . ? C25 C20 C21 C22 0.3(16) . . . . ? P C20 C21 C22 177.2(8) . . . . ? C20 C21 C22 C23 -1.0(17) . . . . ? C21 C22 C23 C24 1.0(18) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C23 C24 C25 C20 -0.3(18) . . . . ? C21 C20 C25 C24 0.3(16) . . . . ? P C20 C25 C24 -176.5(9) . . . . ? C1 P C26 C27 -101.4(8) . . . . ? C20 P C26 C27 142.6(8) . . . . ? Pd P C26 C27 7.8(9) . . . . ? C1 P C26 C31 75.1(9) . . . . ? C20 P C26 C31 -40.8(9) . . . . ? Pd P C26 C31 -175.7(7) . . . . ? C31 C26 C27 C28 -1.2(16) . . . . ? P C26 C27 C28 175.5(9) . . . . ? C26 C27 C28 C29 -1.3(19) . . . . ? C27 C28 C29 C30 4(2) . . . . ? C28 C29 C30 C31 -4.3(19) . . . . ? C29 C30 C31 C26 1.9(17) . . . . ? C27 C26 C31 C30 0.9(15) . . . . ? P C26 C31 C30 -175.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.495 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.495 _refine_diff_density_max 0.346 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.080 data_stras _database_code_CSD 158619 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 O2 P2 Zr' _chemical_formula_weight 892.16 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.582(8) _cell_length_b 12.5470(10) _cell_length_c 18.959(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.67(1) _cell_angle_gamma 90.00 _cell_volume 2259(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 6641 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.2 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Bruker AXS SMART CCD System' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24146 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0987 _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 -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.28 _reflns_number_total 11141 _reflns_number_gt 8818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART CCD System' _computing_cell_refinement 'Bruker AXS SMART CCD System' _computing_data_reduction 'Bruker AXS SMART CCD System' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP5' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(2) _refine_ls_number_reflns 11141 _refine_ls_number_parameters 538 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.68640(2) 0.280100(18) 0.267813(11) 0.01553(5) Uani 1 d . . . P P 0.73037(7) 0.04458(5) 0.43426(3) 0.02022(15) Uani 1 d . . . O O 0.54885(16) 0.20967(13) 0.32301(8) 0.0199(4) Uani 1 d . . . C2 C 0.4906(2) 0.12715(19) 0.35165(12) 0.0181(5) Uani 1 d . . . C3 C 0.5495(3) 0.0481(2) 0.39539(12) 0.0195(6) Uani 1 d . . . C4 C 0.4229(3) -0.0171(2) 0.41358(12) 0.0232(6) Uani 1 d . . . H4 H 0.4454 -0.0913 0.4308 0.028 Uiso 1 calc R . . C5 C 0.3469(3) 0.0533(2) 0.46414(15) 0.0312(7) Uani 1 d . . . H5A H 0.2695 0.0137 0.4821 0.037 Uiso 1 calc R . . H5B H 0.4134 0.0790 0.5050 0.037 Uiso 1 calc R . . C6 C 0.2897(3) 0.1461(2) 0.41555(15) 0.0301(7) Uani 1 d . . . H6A H 0.3336 0.2144 0.4326 0.036 Uiso 1 calc R . . H6B H 0.1862 0.1523 0.4135 0.036 Uiso 1 calc R . . C7 C 0.3310(3) 0.1158(2) 0.34168(14) 0.0238(6) Uani 1 d . . . C8 C 0.3184(3) -0.0089(2) 0.34229(15) 0.0256(7) Uani 1 d . . . C9 C 0.3668(3) -0.0612(2) 0.27749(13) 0.0312(7) Uani 1 d . . . H9A H 0.3680 -0.1387 0.2836 0.047 Uiso 1 calc R . . H9B H 0.4617 -0.0362 0.2722 0.047 Uiso 1 calc R . . H9C H 0.3019 -0.0423 0.2349 0.047 Uiso 1 calc R . . C10 C 0.1701(3) -0.0496(2) 0.34901(15) 0.0389(8) Uani 1 d . . . H10A H 0.1090 -0.0386 0.3039 0.058 Uiso 1 calc R . . H10B H 0.1322 -0.0105 0.3870 0.058 Uiso 1 calc R . . H10C H 0.1743 -0.1258 0.3605 0.058 Uiso 1 calc R . . C11 C 0.2539(3) 0.1743(2) 0.27799(14) 0.0323(7) Uani 1 d . . . H11A H 0.2654 0.2513 0.2851 0.048 Uiso 1 calc R . . H11B H 0.1536 0.1561 0.2729 0.048 Uiso 1 calc R . . H11C H 0.2929 0.1532 0.2349 0.048 Uiso 1 calc R . . C21 C 0.7832(3) -0.0954(2) 0.42552(12) 0.0217(6) Uani 1 d . . . C22 C 0.7049(3) -0.1673(2) 0.38135(16) 0.0297(7) Uani 1 d . . . H22 H 0.6180 -0.1452 0.3554 0.036 Uiso 1 calc R . . C23 C 0.7509(3) -0.2711(3) 0.37423(17) 0.0363(8) Uani 1 d . . . H23 H 0.6948 -0.3196 0.3441 0.044 Uiso 1 calc R . . C24 C 0.8766(3) -0.3040(2) 0.41025(14) 0.0328(7) Uani 1 d . . . H24 H 0.9075 -0.3753 0.4055 0.039 Uiso 1 calc R . . C25 C 0.9586(3) -0.2331(3) 0.45371(12) 0.0321(7) Uani 1 d . . . H25 H 1.0461 -0.2554 0.4789 0.038 Uiso 1 calc R . . C26 C 0.9123(3) -0.1296(2) 0.46019(14) 0.0274(6) Uani 1 d . . . H26 H 0.9703 -0.0807 0.4890 0.033 Uiso 1 calc R . . C31 C 0.7099(3) 0.0506(2) 0.52969(13) 0.0222(6) Uani 1 d . . . C32 C 0.7229(4) -0.0334(3) 0.57571(16) 0.0526(11) Uani 1 d . . . H32 H 0.7469 -0.1018 0.5595 0.063 Uiso 1 calc R . . C33 C 0.7011(5) -0.0194(3) 0.64674(18) 0.0782(15) Uani 1 d . . . H33 H 0.7121 -0.0784 0.6785 0.094 Uiso 1 calc R . . C34 C 0.6644(4) 0.0772(3) 0.67090(17) 0.0484(10) Uani 1 d . . . H34 H 0.6478 0.0856 0.7189 0.058 Uiso 1 calc R . . C35 C 0.6516(3) 0.1615(3) 0.62556(16) 0.0451(8) Uani 1 d . . . H35 H 0.6264 0.2296 0.6419 0.054 Uiso 1 calc R . . C36 C 0.6750(3) 0.1486(2) 0.55613(15) 0.0399(8) Uani 1 d . . . H36 H 0.6671 0.2087 0.5253 0.048 Uiso 1 calc R . . P' P 0.79442(7) 0.48666(5) 0.11975(3) 0.02046(15) Uani 1 d . . . O' O 0.55316(17) 0.36457(13) 0.19839(8) 0.0226(4) Uani 1 d . . . C2' C 0.5212(3) 0.42416(19) 0.14028(12) 0.0207(6) Uani 1 d . . . C3' C 0.6053(2) 0.48224(19) 0.10290(12) 0.0188(5) Uani 1 d . . . C4' C 0.5063(3) 0.5244(2) 0.03853(12) 0.0245(6) Uani 1 d . . . H4' H 0.5415 0.5883 0.0147 0.029 Uiso 1 calc R . . C5' C 0.4720(3) 0.4262(2) -0.01037(14) 0.0338(7) Uani 1 d . . . H5'1 H 0.5587 0.3881 -0.0188 0.041 Uiso 1 calc R . . H5'2 H 0.4186 0.4469 -0.0567 0.041 Uiso 1 calc R . . C6' C 0.3800(3) 0.3569(2) 0.03439(14) 0.0359(7) Uani 1 d . . . H6'1 H 0.2853 0.3441 0.0079 0.043 Uiso 1 calc R . . H6'2 H 0.4255 0.2874 0.0471 0.043 Uiso 1 calc R . . C7' C 0.3709(3) 0.4251(2) 0.10157(13) 0.0251(6) Uani 1 d . . . C8' C 0.3671(3) 0.5414(2) 0.07025(14) 0.0269(6) Uani 1 d . . . C9' C 0.2375(3) 0.5644(3) 0.01467(15) 0.0429(9) Uani 1 d . . . H9'1 H 0.1520 0.5622 0.0378 0.064 Uiso 1 calc R . . H9'2 H 0.2312 0.5104 -0.0230 0.064 Uiso 1 calc R . . H9'3 H 0.2470 0.6351 -0.0061 0.064 Uiso 1 calc R . . C10' C 0.3715(3) 0.6281(2) 0.12664(15) 0.0356(7) Uani 1 d . . . H10D H 0.3844 0.6976 0.1048 0.053 Uiso 1 calc R . . H10E H 0.4500 0.6145 0.1642 0.053 Uiso 1 calc R . . H10F H 0.2829 0.6280 0.1472 0.053 Uiso 1 calc R . . C11' C 0.2548(3) 0.3934(2) 0.14447(14) 0.0334(7) Uani 1 d . . . H11D H 0.2655 0.3181 0.1579 0.050 Uiso 1 calc R . . H11E H 0.1631 0.4043 0.1157 0.050 Uiso 1 calc R . . H11F H 0.2608 0.4374 0.1875 0.050 Uiso 1 calc R . . C21' C 0.8435(3) 0.4942(2) 0.02917(13) 0.0233(6) Uani 1 d . . . C22' C 0.8843(3) 0.3990(2) -0.00116(14) 0.0322(7) Uani 1 d . . . H22' H 0.8846 0.3343 0.0250 0.039 Uiso 1 calc R . . C23' C 0.9242(3) 0.3983(3) -0.06873(15) 0.0386(8) Uani 1 d . . . H23' H 0.9512 0.3333 -0.0889 0.046 Uiso 1 calc R . . C24' C 0.9247(3) 0.4923(3) -0.10696(14) 0.0377(7) Uani 1 d . . . H24' H 0.9524 0.4920 -0.1532 0.045 Uiso 1 calc R . . C25' C 0.8852(3) 0.5855(3) -0.07796(14) 0.0350(7) Uani 1 d . . . H25' H 0.8852 0.6498 -0.1044 0.042 Uiso 1 calc R . . C26' C 0.8450(3) 0.5871(2) -0.01010(14) 0.0277(6) Uani 1 d . . . H26' H 0.8184 0.6526 0.0095 0.033 Uiso 1 calc R . . C31' C 0.8325(3) 0.6230(2) 0.15274(12) 0.0201(6) Uani 1 d . . . C32' C 0.9627(3) 0.6410(2) 0.19471(13) 0.0272(6) Uani 1 d . . . H32' H 1.0313 0.5859 0.2003 0.033 Uiso 1 calc R . . C33' C 0.9918(3) 0.7374(2) 0.22770(15) 0.0320(7) Uani 1 d . . . H33' H 1.0802 0.7482 0.2560 0.038 Uiso 1 calc R . . C34' C 0.8945(3) 0.8185(2) 0.22029(14) 0.0314(7) Uani 1 d . . . H34' H 0.9146 0.8845 0.2441 0.038 Uiso 1 calc R . . C35' C 0.7664(3) 0.80323(19) 0.17759(14) 0.0281(7) Uani 1 d . . . H35' H 0.6996 0.8595 0.1710 0.034 Uiso 1 calc R . . C36' C 0.7366(3) 0.7068(2) 0.14500(14) 0.0251(6) Uani 1 d . . . H36' H 0.6483 0.6970 0.1164 0.030 Uiso 1 calc R . . C41 C 0.8902(3) 0.4038(2) 0.30545(15) 0.0396(8) Uani 1 d . . . H41 H 0.9604 0.4104 0.2748 0.048 Uiso 1 calc R . . C42 C 0.7693(3) 0.4660(2) 0.30300(14) 0.0341(7) Uani 1 d . . . H42 H 0.7431 0.5227 0.2708 0.041 Uiso 1 calc R . . C43 C 0.6934(3) 0.4300(2) 0.35653(14) 0.0302(7) Uani 1 d . . . H43 H 0.6057 0.4574 0.3665 0.036 Uiso 1 calc R . . C44 C 0.7682(3) 0.3472(2) 0.39259(13) 0.0327(7) Uani 1 d . . . H44 H 0.7411 0.3092 0.4319 0.039 Uiso 1 calc R . . C45 C 0.8907(3) 0.3292(2) 0.36115(14) 0.0376(8) Uani 1 d . . . H45 H 0.9607 0.2768 0.3748 0.045 Uiso 1 calc R . . C46 C 0.8643(3) 0.2067(2) 0.19584(15) 0.0355(7) Uani 1 d . . . H46 H 0.9420 0.2513 0.1900 0.043 Uiso 1 calc R . . C47 C 0.7368(3) 0.2023(2) 0.15133(15) 0.0368(8) Uani 1 d . . . H47 H 0.7129 0.2429 0.1092 0.044 Uiso 1 calc R . . C48 C 0.6499(3) 0.1283(2) 0.17880(14) 0.0322(7) Uani 1 d . . . H48 H 0.5562 0.1110 0.1592 0.039 Uiso 1 calc R . . C49 C 0.7250(3) 0.0841(2) 0.24032(15) 0.0307(7) Uani 1 d . . . H49 H 0.6917 0.0304 0.2693 0.037 Uiso 1 calc R . . C50 C 0.8569(3) 0.1324(2) 0.25169(15) 0.0340(7) Uani 1 d . . . H50 H 0.9290 0.1182 0.2900 0.041 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01732(10) 0.01387(10) 0.01530(10) 0.00006(13) 0.00180(8) 0.00009(13) P 0.0215(4) 0.0190(4) 0.0193(4) 0.0019(3) -0.0002(3) -0.0010(3) O 0.0212(9) 0.0164(9) 0.0223(9) 0.0030(7) 0.0037(7) -0.0011(7) C2 0.0218(13) 0.0171(13) 0.0155(12) -0.0005(10) 0.0027(10) -0.0046(11) C3 0.0234(14) 0.0195(13) 0.0153(13) 0.0015(11) 0.0014(11) -0.0032(11) C4 0.0257(14) 0.0214(14) 0.0220(14) 0.0093(11) 0.0015(11) -0.0026(11) C5 0.0296(17) 0.0339(18) 0.0314(17) 0.0071(14) 0.0089(13) 0.0001(14) C6 0.0256(16) 0.0297(17) 0.0363(17) 0.0058(14) 0.0095(13) 0.0032(13) C7 0.0213(14) 0.0230(15) 0.0268(16) 0.0058(12) 0.0023(12) 0.0010(12) C8 0.0212(15) 0.0262(16) 0.0276(16) 0.0065(13) -0.0027(12) -0.0049(13) C9 0.0367(17) 0.0231(15) 0.0305(16) 0.0090(12) -0.0078(13) -0.0047(13) C10 0.0281(17) 0.0344(18) 0.052(2) 0.0130(14) -0.0040(15) -0.0088(13) C11 0.0236(15) 0.0310(17) 0.0395(18) 0.0130(13) -0.0060(13) -0.0017(13) C21 0.0232(14) 0.0252(15) 0.0171(13) 0.0010(11) 0.0047(11) 0.0000(12) C22 0.0333(17) 0.0287(17) 0.0262(16) -0.0043(13) 0.0002(13) 0.0030(14) C23 0.047(2) 0.0245(17) 0.0362(19) -0.0086(14) 0.0006(16) 0.0006(15) C24 0.045(2) 0.0233(16) 0.0311(17) -0.0009(13) 0.0092(15) 0.0113(14) C25 0.0284(13) 0.039(2) 0.0276(14) -0.0007(15) 0.0004(11) 0.0095(16) C26 0.0264(15) 0.0255(16) 0.0294(16) 0.0008(12) 0.0002(13) 0.0035(12) C31 0.0189(14) 0.0268(15) 0.0197(14) 0.0018(12) -0.0025(11) -0.0029(12) C32 0.094(3) 0.035(2) 0.0330(19) 0.0095(15) 0.0239(19) 0.032(2) C33 0.131(4) 0.074(3) 0.036(2) 0.033(2) 0.035(2) 0.059(3) C34 0.056(2) 0.067(3) 0.0235(18) -0.0055(18) 0.0080(16) 0.012(2) C35 0.060(2) 0.0340(19) 0.044(2) -0.0183(16) 0.0169(17) -0.0133(16) C36 0.067(2) 0.0206(16) 0.0356(18) -0.0015(13) 0.0201(16) -0.0073(15) P' 0.0222(4) 0.0192(4) 0.0198(4) 0.0009(3) 0.0022(3) -0.0018(3) O' 0.0226(10) 0.0241(10) 0.0208(9) 0.0090(8) 0.0021(8) -0.0003(8) C2' 0.0252(14) 0.0160(13) 0.0195(13) -0.0002(11) -0.0022(11) 0.0003(11) C3' 0.0221(14) 0.0173(13) 0.0162(13) 0.0011(11) -0.0012(11) -0.0020(11) C4' 0.0262(14) 0.0251(15) 0.0217(14) 0.0088(11) 0.0014(12) -0.0041(12) C5' 0.0376(17) 0.0397(18) 0.0220(15) -0.0012(13) -0.0029(13) -0.0119(14) C6' 0.0352(17) 0.0422(18) 0.0267(16) 0.0015(14) -0.0089(13) -0.0153(14) C7' 0.0208(14) 0.0284(15) 0.0245(14) 0.0065(12) -0.0028(12) -0.0034(12) C8' 0.0194(14) 0.0315(16) 0.0292(15) 0.0132(13) 0.0012(12) -0.0016(12) C9' 0.0255(16) 0.058(2) 0.0437(19) 0.0306(17) -0.0022(14) 0.0003(15) C10' 0.0309(17) 0.0330(17) 0.0455(18) 0.0165(14) 0.0146(14) 0.0053(14) C11' 0.0266(15) 0.0370(18) 0.0348(17) 0.0162(13) -0.0026(13) -0.0063(13) C21' 0.0197(14) 0.0285(15) 0.0214(14) -0.0013(12) 0.0017(11) -0.0022(12) C22' 0.0361(17) 0.0279(17) 0.0336(17) -0.0023(13) 0.0086(14) -0.0065(13) C23' 0.0459(19) 0.042(2) 0.0288(17) -0.0130(15) 0.0087(15) -0.0032(15) C24' 0.0320(17) 0.061(2) 0.0219(15) -0.0046(16) 0.0091(13) -0.0003(16) C25' 0.0335(18) 0.046(2) 0.0251(16) 0.0124(14) 0.0035(13) 0.0030(14) C26' 0.0250(15) 0.0311(16) 0.0279(16) 0.0026(13) 0.0072(12) 0.0027(12) C31' 0.0211(14) 0.0200(14) 0.0189(13) 0.0023(11) 0.0019(11) -0.0044(11) C32' 0.0221(15) 0.0284(16) 0.0310(15) 0.0000(12) 0.0034(12) -0.0030(12) C33' 0.0219(15) 0.0328(17) 0.0400(18) -0.0045(13) -0.0011(13) -0.0062(13) C34' 0.0363(17) 0.0260(16) 0.0324(16) -0.0064(12) 0.0065(14) -0.0108(13) C35' 0.0330(15) 0.0184(19) 0.0329(15) 0.0004(11) 0.0037(12) 0.0011(12) C36' 0.0255(15) 0.0228(15) 0.0264(16) 0.0016(12) 0.0017(12) -0.0016(13) C41 0.0351(18) 0.053(2) 0.0311(17) -0.0072(16) 0.0042(14) -0.0273(16) C42 0.056(2) 0.0254(16) 0.0196(15) -0.0044(12) 0.0002(14) -0.0188(14) C43 0.0451(18) 0.0230(15) 0.0234(15) -0.0102(12) 0.0074(14) -0.0071(14) C44 0.0442(18) 0.0390(18) 0.0141(14) -0.0034(12) 0.0005(13) -0.0179(14) C45 0.0276(16) 0.053(2) 0.0284(16) 0.0001(14) -0.0098(13) -0.0038(14) C46 0.0417(19) 0.0225(15) 0.0483(19) -0.0012(14) 0.0283(16) 0.0022(14) C47 0.064(2) 0.0264(17) 0.0237(16) -0.0059(13) 0.0180(16) 0.0062(16) C48 0.0455(19) 0.0238(16) 0.0274(16) -0.0090(13) 0.0053(14) -0.0015(14) C49 0.0411(18) 0.0135(14) 0.0408(18) -0.0019(12) 0.0173(14) 0.0037(12) C50 0.0358(17) 0.0253(16) 0.0424(18) 0.0036(14) 0.0109(14) 0.0127(13) _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 Zr O 1.9954(19) . ? Zr O' 2.0093(18) . ? Zr C46 2.497(3) . ? Zr C50 2.516(3) . ? Zr C43 2.518(3) . ? Zr C47 2.520(3) . ? Zr C41 2.522(3) . ? Zr C42 2.525(3) . ? Zr C45 2.534(3) . ? Zr C44 2.535(3) . ? Zr C48 2.537(3) . ? Zr C49 2.552(3) . ? P C3 1.791(3) . ? P C21 1.841(3) . ? P C31 1.847(3) . ? O C2 1.327(3) . ? C2 C3 1.366(3) . ? C2 C7 1.522(4) . ? C3 C4 1.540(3) . ? C4 C5 1.554(4) . ? C4 C8 1.575(4) . ? C5 C6 1.540(4) . ? C6 C7 1.553(4) . ? C7 C11 1.518(3) . ? C7 C8 1.569(4) . ? C8 C9 1.519(4) . ? C8 C10 1.531(4) . ? C21 C22 1.382(4) . ? C21 C26 1.390(3) . ? C22 C23 1.388(3) . ? C23 C24 1.366(4) . ? C24 C25 1.384(4) . ? C25 C26 1.383(4) . ? C31 C32 1.363(4) . ? C31 C36 1.386(4) . ? C32 C33 1.401(4) . ? C33 C34 1.359(5) . ? C34 C35 1.359(4) . ? C35 C36 1.374(4) . ? P' C3' 1.798(3) . ? P' C31' 1.841(3) . ? P' C21' 1.842(3) . ? O' C2' 1.333(3) . ? C2' C3' 1.355(3) . ? C2' C7' 1.526(3) . ? C3' C4' 1.537(3) . ? C4' C8' 1.549(4) . ? C4' C5' 1.551(3) . ? C5' C6' 1.566(4) . ? C6' C7' 1.547(4) . ? C7' C11' 1.516(3) . ? C7' C8' 1.574(3) . ? C8' C10' 1.522(4) . ? C8' C9' 1.545(4) . ? C21' C26' 1.384(4) . ? C21' C22' 1.404(4) . ? C22' C23' 1.385(4) . ? C23' C24' 1.385(4) . ? C24' C25' 1.367(4) . ? C25' C26' 1.392(4) . ? C31' C36' 1.392(3) . ? C31' C32' 1.406(3) . ? C32' C33' 1.373(3) . ? C33' C34' 1.375(3) . ? C34' C35' 1.390(4) . ? C35' C36' 1.371(3) . ? C41 C42 1.392(4) . ? C41 C45 1.410(4) . ? C42 C43 1.400(4) . ? C43 C44 1.389(4) . ? C44 C45 1.404(4) . ? C46 C47 1.390(4) . ? C46 C50 1.420(4) . ? C47 C48 1.393(4) . ? C48 C49 1.401(4) . ? C49 C50 1.393(4) . ? 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 O Zr O' 99.83(9) . . ? O Zr C46 132.07(8) . . ? O' Zr C46 104.89(10) . . ? O Zr C50 102.86(9) . . ? O' Zr C50 132.46(9) . . ? C46 Zr C50 32.90(9) . . ? O Zr C43 86.61(9) . . ? O' Zr C43 90.09(9) . . ? C46 Zr C43 132.95(10) . . ? C50 Zr C43 132.18(10) . . ? O Zr C47 120.36(9) . . ? O' Zr C47 79.02(10) . . ? C46 Zr C47 32.16(9) . . ? C50 Zr C47 53.45(10) . . ? C43 Zr C47 152.11(9) . . ? O Zr C41 131.68(9) . . ? O' Zr C41 105.13(9) . . ? C46 Zr C41 79.77(11) . . ? C50 Zr C41 89.82(11) . . ? C43 Zr C41 53.19(10) . . ? C47 Zr C41 104.76(11) . . ? O Zr C42 118.50(9) . . ? O' Zr C42 80.56(9) . . ? C46 Zr C42 105.75(10) . . ? C50 Zr C42 121.73(11) . . ? C43 Zr C42 32.25(8) . . ? C47 Zr C42 119.94(10) . . ? C41 Zr C42 32.02(9) . . ? O Zr C45 104.14(10) . . ? O' Zr C45 133.90(9) . . ? C46 Zr C45 87.21(12) . . ? C50 Zr C45 79.06(10) . . ? C43 Zr C45 53.32(10) . . ? C47 Zr C45 119.06(11) . . ? C41 Zr C45 32.40(9) . . ? C42 Zr C45 53.43(10) . . ? O Zr C44 78.54(9) . . ? O' Zr C44 121.77(9) . . ? C46 Zr C44 118.94(11) . . ? C50 Zr C44 103.48(10) . . ? C43 Zr C44 31.91(9) . . ? C47 Zr C44 151.06(11) . . ? C41 Zr C44 53.14(9) . . ? C42 Zr C44 53.08(9) . . ? C45 Zr C44 32.16(9) . . ? O Zr C48 88.53(9) . . ? O' Zr C48 86.62(9) . . ? C46 Zr C48 53.37(10) . . ? C50 Zr C48 53.16(10) . . ? C43 Zr C48 173.59(10) . . ? C47 Zr C48 31.98(9) . . ? C41 Zr C48 133.06(10) . . ? C42 Zr C48 151.59(9) . . ? C45 Zr C48 132.23(10) . . ? C44 Zr C48 150.23(9) . . ? O Zr C49 78.70(8) . . ? O' Zr C49 118.12(9) . . ? C46 Zr C49 53.47(9) . . ? C50 Zr C49 31.89(9) . . ? C43 Zr C49 149.86(9) . . ? C47 Zr C49 52.95(9) . . ? C41 Zr C49 121.56(11) . . ? C42 Zr C49 153.57(10) . . ? C45 Zr C49 104.93(10) . . ? C44 Zr C49 118.40(10) . . ? C48 Zr C49 31.96(8) . . ? C3 P C21 104.41(12) . . ? C3 P C31 100.30(12) . . ? C21 P C31 101.16(12) . . ? C2 O Zr 154.69(15) . . ? O C2 C3 130.7(2) . . ? O C2 C7 119.6(2) . . ? C3 C2 C7 109.5(2) . . ? C2 C3 C4 104.3(2) . . ? C2 C3 P 124.52(19) . . ? C4 C3 P 130.00(18) . . ? C3 C4 C5 106.5(2) . . ? C3 C4 C8 101.69(19) . . ? C5 C4 C8 101.3(2) . . ? C6 C5 C4 102.7(2) . . ? C5 C6 C7 103.9(2) . . ? C11 C7 C2 115.3(2) . . ? C11 C7 C6 116.3(2) . . ? C2 C7 C6 103.8(2) . . ? C11 C7 C8 117.3(2) . . ? C2 C7 C8 99.8(2) . . ? C6 C7 C8 102.0(2) . . ? C9 C8 C10 108.1(2) . . ? C9 C8 C7 113.1(2) . . ? C10 C8 C7 114.0(2) . . ? C9 C8 C4 116.0(2) . . ? C10 C8 C4 113.4(2) . . ? C7 C8 C4 91.8(2) . . ? C22 C21 C26 117.5(3) . . ? C22 C21 P 122.9(2) . . ? C26 C21 P 119.37(19) . . ? C21 C22 C23 121.2(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.7(3) . . ? C26 C25 C24 119.5(2) . . ? C25 C26 C21 121.6(3) . . ? C32 C31 C36 117.4(3) . . ? C32 C31 P 125.6(2) . . ? C36 C31 P 116.9(2) . . ? C31 C32 C33 120.4(3) . . ? C34 C33 C32 120.9(3) . . ? C33 C34 C35 119.2(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 122.0(3) . . ? C3' P' C31' 103.78(11) . . ? C3' P' C21' 102.26(11) . . ? C31' P' C21' 101.85(12) . . ? C2' O' Zr 153.28(16) . . ? O' C2' C3' 130.3(2) . . ? O' C2' C7' 120.0(2) . . ? C3' C2' C7' 109.5(2) . . ? C2' C3' C4' 104.7(2) . . ? C2' C3' P' 125.41(19) . . ? C4' C3' P' 129.14(18) . . ? C3' C4' C8' 102.2(2) . . ? C3' C4' C5' 105.1(2) . . ? C8' C4' C5' 102.5(2) . . ? C4' C5' C6' 102.0(2) . . ? C7' C6' C5' 103.7(2) . . ? C11' C7' C2' 116.9(2) . . ? C11' C7' C6' 115.0(2) . . ? C2' C7' C6' 103.8(2) . . ? C11' C7' C8' 117.6(2) . . ? C2' C7' C8' 99.29(19) . . ? C6' C7' C8' 101.7(2) . . ? C10' C8' C9' 106.9(2) . . ? C10' C8' C4' 115.2(2) . . ? C9' C8' C4' 114.6(2) . . ? C10' C8' C7' 113.6(2) . . ? C9' C8' C7' 114.0(2) . . ? C4' C8' C7' 92.4(2) . . ? C26' C21' C22' 118.2(2) . . ? C26' C21' P' 124.5(2) . . ? C22' C21' P' 117.2(2) . . ? C23' C22' C21' 120.7(3) . . ? C24' C23' C22' 120.0(3) . . ? C25' C24' C23' 119.9(3) . . ? C24' C25' C26' 120.7(3) . . ? C21' C26' C25' 120.6(3) . . ? C36' C31' C32' 117.5(2) . . ? C36' C31' P' 124.66(18) . . ? C32' C31' P' 117.55(19) . . ? C33' C32' C31' 120.7(2) . . ? C32' C33' C34' 120.8(2) . . ? C33' C34' C35' 119.4(2) . . ? C36' C35' C34' 119.9(2) . . ? C35' C36' C31' 121.6(2) . . ? C42 C41 C45 108.5(3) . . ? C42 C41 Zr 74.11(16) . . ? C45 C41 Zr 74.27(15) . . ? C41 C42 C43 107.8(3) . . ? C41 C42 Zr 73.87(16) . . ? C43 C42 Zr 73.60(15) . . ? C44 C43 C42 108.3(3) . . ? C44 C43 Zr 74.72(16) . . ? C42 C43 Zr 74.15(15) . . ? C43 C44 C45 108.5(3) . . ? C43 C44 Zr 73.37(15) . . ? C45 C44 Zr 73.88(15) . . ? C44 C45 C41 106.9(3) . . ? C44 C45 Zr 73.96(16) . . ? C41 C45 Zr 73.33(15) . . ? C47 C46 C50 107.4(3) . . ? C47 C46 Zr 74.81(17) . . ? C50 C46 Zr 74.29(15) . . ? C46 C47 C48 108.7(3) . . ? C46 C47 Zr 73.02(16) . . ? C48 C47 Zr 74.71(16) . . ? C47 C48 C49 108.0(3) . . ? C47 C48 Zr 73.30(16) . . ? C49 C48 Zr 74.58(15) . . ? C50 C49 C48 108.1(3) . . ? C50 C49 Zr 72.65(15) . . ? C48 C49 Zr 73.47(15) . . ? C49 C50 C46 107.8(3) . . ? C49 C50 Zr 75.46(16) . . ? C46 C50 Zr 72.82(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O' Zr O C2 128.1(3) . . . . ? C46 Zr O C2 7.6(4) . . . . ? C50 Zr O C2 -9.8(4) . . . . ? C43 Zr O C2 -142.4(4) . . . . ? C47 Zr O C2 45.2(4) . . . . ? C41 Zr O C2 -111.3(4) . . . . ? C42 Zr O C2 -147.4(3) . . . . ? C45 Zr O C2 -91.6(4) . . . . ? C44 Zr O C2 -111.2(4) . . . . ? C48 Zr O C2 41.8(4) . . . . ? C49 Zr O C2 11.2(3) . . . . ? Zr O C2 C3 52.2(5) . . . . ? Zr O C2 C7 -133.0(3) . . . . ? O C2 C3 C4 175.8(2) . . . . ? C7 C2 C3 C4 0.5(3) . . . . ? O C2 C3 P 7.1(4) . . . . ? C7 C2 C3 P -168.21(18) . . . . ? C21 P C3 C2 -138.0(2) . . . . ? C31 P C3 C2 117.5(2) . . . . ? C21 P C3 C4 56.2(2) . . . . ? C31 P C3 C4 -48.2(3) . . . . ? C2 C3 C4 C5 -71.3(2) . . . . ? P C3 C4 C5 96.6(3) . . . . ? C2 C3 C4 C8 34.4(3) . . . . ? P C3 C4 C8 -157.7(2) . . . . ? C3 C4 C5 C6 66.7(2) . . . . ? C8 C4 C5 C6 -39.2(3) . . . . ? C4 C5 C6 C7 3.3(3) . . . . ? O C2 C7 C11 22.4(3) . . . . ? C3 C2 C7 C11 -161.7(2) . . . . ? O C2 C7 C6 -106.0(2) . . . . ? C3 C2 C7 C6 69.9(3) . . . . ? O C2 C7 C8 149.0(2) . . . . ? C3 C2 C7 C8 -35.2(3) . . . . ? C5 C6 C7 C11 162.9(2) . . . . ? C5 C6 C7 C2 -69.4(3) . . . . ? C5 C6 C7 C8 34.0(3) . . . . ? C11 C7 C8 C9 57.0(3) . . . . ? C2 C7 C8 C9 -68.2(3) . . . . ? C6 C7 C8 C9 -174.7(2) . . . . ? C11 C7 C8 C10 -67.0(3) . . . . ? C2 C7 C8 C10 167.8(2) . . . . ? C6 C7 C8 C10 61.3(3) . . . . ? C11 C7 C8 C4 176.3(2) . . . . ? C2 C7 C8 C4 51.1(2) . . . . ? C6 C7 C8 C4 -55.4(2) . . . . ? C3 C4 C8 C9 64.8(3) . . . . ? C5 C4 C8 C9 174.5(2) . . . . ? C3 C4 C8 C10 -169.3(2) . . . . ? C5 C4 C8 C10 -59.6(3) . . . . ? C3 C4 C8 C7 -52.1(2) . . . . ? C5 C4 C8 C7 57.6(2) . . . . ? C3 P C21 C22 14.9(3) . . . . ? C31 P C21 C22 118.7(2) . . . . ? C3 P C21 C26 -170.3(2) . . . . ? C31 P C21 C26 -66.5(2) . . . . ? C26 C21 C22 C23 2.6(4) . . . . ? P C21 C22 C23 177.6(2) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C23 C24 C25 C26 0.0(4) . . . . ? C24 C25 C26 C21 1.7(4) . . . . ? C22 C21 C26 C25 -3.0(4) . . . . ? P C21 C26 C25 -178.2(2) . . . . ? C3 P C31 C32 102.9(3) . . . . ? C21 P C31 C32 -4.2(3) . . . . ? C3 P C31 C36 -75.4(2) . . . . ? C21 P C31 C36 177.5(2) . . . . ? C36 C31 C32 C33 0.1(5) . . . . ? P C31 C32 C33 -178.2(3) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? C32 C33 C34 C35 -1.4(6) . . . . ? C33 C34 C35 C36 0.3(6) . . . . ? C34 C35 C36 C31 0.9(5) . . . . ? C32 C31 C36 C35 -1.1(4) . . . . ? P C31 C36 C35 177.3(2) . . . . ? O Zr O' C2' -168.7(3) . . . . ? C46 Zr O' C2' -30.1(4) . . . . ? C50 Zr O' C2' -51.0(4) . . . . ? C43 Zr O' C2' 104.7(3) . . . . ? C47 Zr O' C2' -49.4(3) . . . . ? C41 Zr O' C2' 53.1(4) . . . . ? C42 Zr O' C2' 73.8(3) . . . . ? C45 Zr O' C2' 70.6(4) . . . . ? C44 Zr O' C2' 108.8(3) . . . . ? C48 Zr O' C2' -80.8(3) . . . . ? C49 Zr O' C2' -86.3(4) . . . . ? Zr O' C2' C3' -20.1(5) . . . . ? Zr O' C2' C7' 153.6(3) . . . . ? O' C2' C3' C4' 175.4(2) . . . . ? C7' C2' C3' C4' 1.2(3) . . . . ? O' C2' C3' P' 4.8(4) . . . . ? C7' C2' C3' P' -169.47(18) . . . . ? C31' P' C3' C2' -111.4(2) . . . . ? C21' P' C3' C2' 143.0(2) . . . . ? C31' P' C3' C4' 80.3(2) . . . . ? C21' P' C3' C4' -25.4(2) . . . . ? C2' C3' C4' C8' 33.8(3) . . . . ? P' C3' C4' C8' -156.04(19) . . . . ? C2' C3' C4' C5' -72.9(2) . . . . ? P' C3' C4' C5' 97.3(2) . . . . ? C3' C4' C5' C6' 68.7(2) . . . . ? C8' C4' C5' C6' -37.8(2) . . . . ? C4' C5' C6' C7' 1.2(3) . . . . ? O' C2' C7' C11' 22.7(3) . . . . ? C3' C2' C7' C11' -162.3(2) . . . . ? O' C2' C7' C6' -105.1(2) . . . . ? C3' C2' C7' C6' 69.8(3) . . . . ? O' C2' C7' C8' 150.3(2) . . . . ? C3' C2' C7' C8' -34.8(3) . . . . ? C5' C6' C7' C11' 163.1(2) . . . . ? C5' C6' C7' C2' -67.9(2) . . . . ? C5' C6' C7' C8' 34.9(2) . . . . ? C3' C4' C8' C10' 66.1(3) . . . . ? C5' C4' C8' C10' 174.8(2) . . . . ? C3' C4' C8' C9' -169.3(2) . . . . ? C5' C4' C8' C9' -60.6(3) . . . . ? C3' C4' C8' C7' -51.4(2) . . . . ? C5' C4' C8' C7' 57.2(2) . . . . ? C11' C7' C8' C10' 58.7(3) . . . . ? C2' C7' C8' C10' -68.4(2) . . . . ? C6' C7' C8' C10' -174.7(2) . . . . ? C11' C7' C8' C9' -64.1(3) . . . . ? C2' C7' C8' C9' 168.8(2) . . . . ? C6' C7' C8' C9' 62.5(3) . . . . ? C11' C7' C8' C4' 177.6(2) . . . . ? C2' C7' C8' C4' 50.5(2) . . . . ? C6' C7' C8' C4' -55.8(2) . . . . ? C3' P' C21' C26' 82.4(2) . . . . ? C31' P' C21' C26' -24.8(2) . . . . ? C3' P' C21' C22' -98.8(2) . . . . ? C31' P' C21' C22' 154.1(2) . . . . ? C26' C21' C22' C23' -0.4(4) . . . . ? P' C21' C22' C23' -179.3(2) . . . . ? C21' C22' C23' C24' 0.3(4) . . . . ? C22' C23' C24' C25' -0.3(4) . . . . ? C23' C24' C25' C26' 0.3(4) . . . . ? C22' C21' C26' C25' 0.4(4) . . . . ? P' C21' C26' C25' 179.2(2) . . . . ? C24' C25' C26' C21' -0.4(4) . . . . ? C3' P' C31' C36' -16.5(2) . . . . ? C21' P' C31' C36' 89.5(2) . . . . ? C3' P' C31' C32' 156.99(19) . . . . ? C21' P' C31' C32' -97.1(2) . . . . ? C36' C31' C32' C33' 1.3(4) . . . . ? P' C31' C32' C33' -172.6(2) . . . . ? C31' C32' C33' C34' -0.2(4) . . . . ? C32' C33' C34' C35' -1.4(4) . . . . ? C33' C34' C35' C36' 1.9(4) . . . . ? C34' C35' C36' C31' -0.8(4) . . . . ? C32' C31' C36' C35' -0.8(4) . . . . ? P' C31' C36' C35' 172.7(2) . . . . ? O Zr C41 C42 -77.4(2) . . . . ? O' Zr C41 C42 41.15(18) . . . . ? C46 Zr C41 C42 143.96(18) . . . . ? C50 Zr C41 C42 175.46(17) . . . . ? C43 Zr C41 C42 -37.29(16) . . . . ? C47 Zr C41 C42 123.53(17) . . . . ? C45 Zr C41 C42 -115.0(3) . . . . ? C44 Zr C41 C42 -77.46(18) . . . . ? C48 Zr C41 C42 140.89(17) . . . . ? C49 Zr C41 C42 178.81(16) . . . . ? O Zr C41 C45 37.6(2) . . . . ? O' Zr C41 C45 156.13(17) . . . . ? C46 Zr C41 C45 -101.06(19) . . . . ? C50 Zr C41 C45 -69.56(19) . . . . ? C43 Zr C41 C45 77.69(19) . . . . ? C47 Zr C41 C45 -121.50(19) . . . . ? C42 Zr C41 C45 115.0(3) . . . . ? C44 Zr C41 C45 37.52(17) . . . . ? C48 Zr C41 C45 -104.1(2) . . . . ? C49 Zr C41 C45 -66.2(2) . . . . ? C45 C41 C42 C43 -0.6(3) . . . . ? Zr C41 C42 C43 66.33(18) . . . . ? C45 C41 C42 Zr -66.91(19) . . . . ? O Zr C42 C41 123.97(17) . . . . ? O' Zr C42 C41 -139.91(18) . . . . ? C46 Zr C42 C41 -36.98(19) . . . . ? C50 Zr C42 C41 -5.3(2) . . . . ? C43 Zr C42 C41 114.6(3) . . . . ? C47 Zr C42 C41 -68.5(2) . . . . ? C45 Zr C42 C41 37.22(16) . . . . ? C44 Zr C42 C41 77.66(19) . . . . ? C48 Zr C42 C41 -75.6(3) . . . . ? C49 Zr C42 C41 -2.3(3) . . . . ? O Zr C42 C43 9.3(2) . . . . ? O' Zr C42 C43 105.47(19) . . . . ? C46 Zr C42 C43 -151.61(18) . . . . ? C50 Zr C42 C43 -119.97(19) . . . . ? C47 Zr C42 C43 176.89(17) . . . . ? C41 Zr C42 C43 -114.6(3) . . . . ? C45 Zr C42 C43 -77.41(19) . . . . ? C44 Zr C42 C43 -36.96(17) . . . . ? C48 Zr C42 C43 169.8(2) . . . . ? C49 Zr C42 C43 -116.9(2) . . . . ? C41 C42 C43 C44 1.0(3) . . . . ? Zr C42 C43 C44 67.52(19) . . . . ? C41 C42 C43 Zr -66.51(19) . . . . ? O Zr C43 C44 73.65(18) . . . . ? O' Zr C43 C44 173.50(17) . . . . ? C46 Zr C43 C44 -75.9(2) . . . . ? C50 Zr C43 C44 -30.7(2) . . . . ? C47 Zr C43 C44 -120.3(2) . . . . ? C41 Zr C43 C44 -77.55(19) . . . . ? C42 Zr C43 C44 -114.6(3) . . . . ? C45 Zr C43 C44 -36.79(16) . . . . ? C48 Zr C43 C44 114.4(9) . . . . ? C49 Zr C43 C44 13.2(3) . . . . ? O Zr C43 C42 -171.78(18) . . . . ? O' Zr C43 C42 -71.94(19) . . . . ? C46 Zr C43 C42 38.7(2) . . . . ? C50 Zr C43 C42 83.9(2) . . . . ? C47 Zr C43 C42 -5.8(3) . . . . ? C41 Zr C43 C42 37.02(17) . . . . ? C45 Zr C43 C42 77.8(2) . . . . ? C44 Zr C43 C42 114.6(3) . . . . ? C48 Zr C43 C42 -131.0(8) . . . . ? C49 Zr C43 C42 127.8(2) . . . . ? C42 C43 C44 C45 -1.1(3) . . . . ? Zr C43 C44 C45 66.07(19) . . . . ? C42 C43 C44 Zr -67.14(18) . . . . ? O Zr C44 C43 -102.21(18) . . . . ? O' Zr C44 C43 -7.7(2) . . . . ? C46 Zr C44 C43 125.80(18) . . . . ? C50 Zr C44 C43 157.14(17) . . . . ? C47 Zr C44 C43 123.4(2) . . . . ? C41 Zr C44 C43 77.72(19) . . . . ? C42 Zr C44 C43 37.38(17) . . . . ? C45 Zr C44 C43 115.5(3) . . . . ? C48 Zr C44 C43 -168.2(2) . . . . ? C49 Zr C44 C43 -172.51(16) . . . . ? O Zr C44 C45 142.26(18) . . . . ? O' Zr C44 C45 -123.19(17) . . . . ? C46 Zr C44 C45 10.3(2) . . . . ? C50 Zr C44 C45 41.61(19) . . . . ? C43 Zr C44 C45 -115.5(3) . . . . ? C47 Zr C44 C45 7.9(3) . . . . ? C41 Zr C44 C45 -37.81(17) . . . . ? C42 Zr C44 C45 -78.16(19) . . . . ? C48 Zr C44 C45 76.3(2) . . . . ? C49 Zr C44 C45 71.96(19) . . . . ? C43 C44 C45 C41 0.7(3) . . . . ? Zr C44 C45 C41 66.44(19) . . . . ? C43 C44 C45 Zr -65.74(19) . . . . ? C42 C41 C45 C44 -0.1(3) . . . . ? Zr C41 C45 C44 -66.87(19) . . . . ? C42 C41 C45 Zr 66.80(19) . . . . ? O Zr C45 C44 -38.22(18) . . . . ? O' Zr C45 C44 80.92(19) . . . . ? C46 Zr C45 C44 -171.02(18) . . . . ? C50 Zr C45 C44 -138.88(18) . . . . ? C43 Zr C45 C44 36.49(16) . . . . ? C47 Zr C45 C44 -175.63(17) . . . . ? C41 Zr C45 C44 113.7(3) . . . . ? C42 Zr C45 C44 76.99(19) . . . . ? C48 Zr C45 C44 -139.35(17) . . . . ? C49 Zr C45 C44 -120.05(17) . . . . ? O Zr C45 C41 -151.96(17) . . . . ? O' Zr C45 C41 -32.8(2) . . . . ? C46 Zr C45 C41 75.23(19) . . . . ? C50 Zr C45 C41 107.37(19) . . . . ? C43 Zr C45 C41 -77.26(19) . . . . ? C47 Zr C45 C41 70.6(2) . . . . ? C42 Zr C45 C41 -36.76(17) . . . . ? C44 Zr C45 C41 -113.7(3) . . . . ? C48 Zr C45 C41 106.9(2) . . . . ? C49 Zr C45 C41 126.20(19) . . . . ? O Zr C46 C47 81.00(19) . . . . ? O' Zr C46 C47 -37.55(18) . . . . ? C50 Zr C46 C47 113.5(3) . . . . ? C43 Zr C46 C47 -142.01(17) . . . . ? C41 Zr C46 C47 -140.64(18) . . . . ? C42 Zr C46 C47 -121.73(17) . . . . ? C45 Zr C46 C47 -172.41(18) . . . . ? C44 Zr C46 C47 -177.86(16) . . . . ? C48 Zr C46 C47 36.57(16) . . . . ? C49 Zr C46 C47 76.66(19) . . . . ? O Zr C46 C50 -32.5(2) . . . . ? O' Zr C46 C50 -151.05(17) . . . . ? C43 Zr C46 C50 104.49(19) . . . . ? C47 Zr C46 C50 -113.5(3) . . . . ? C41 Zr C46 C50 105.85(19) . . . . ? C42 Zr C46 C50 124.77(18) . . . . ? C45 Zr C46 C50 74.08(19) . . . . ? C44 Zr C46 C50 68.6(2) . . . . ? C48 Zr C46 C50 -76.94(19) . . . . ? C49 Zr C46 C50 -36.84(16) . . . . ? C50 C46 C47 C48 0.9(3) . . . . ? Zr C46 C47 C48 -66.8(2) . . . . ? C50 C46 C47 Zr 67.71(19) . . . . ? O Zr C47 C46 -121.82(17) . . . . ? O' Zr C47 C46 143.14(18) . . . . ? C50 Zr C47 C46 -38.31(16) . . . . ? C43 Zr C47 C46 74.4(3) . . . . ? C41 Zr C47 C46 40.20(19) . . . . ? C42 Zr C47 C46 70.9(2) . . . . ? C45 Zr C47 C46 8.7(2) . . . . ? C44 Zr C47 C46 3.9(3) . . . . ? C48 Zr C47 C46 -115.5(3) . . . . ? C49 Zr C47 C46 -78.44(18) . . . . ? O Zr C47 C48 -6.3(2) . . . . ? O' Zr C47 C48 -101.37(19) . . . . ? C46 Zr C47 C48 115.5(3) . . . . ? C50 Zr C47 C48 77.18(19) . . . . ? C43 Zr C47 C48 -170.1(2) . . . . ? C41 Zr C47 C48 155.69(18) . . . . ? C42 Zr C47 C48 -173.64(17) . . . . ? C45 Zr C47 C48 124.17(19) . . . . ? C44 Zr C47 C48 119.4(2) . . . . ? C49 Zr C47 C48 37.05(17) . . . . ? C46 C47 C48 C49 -1.4(3) . . . . ? Zr C47 C48 C49 -67.07(19) . . . . ? C46 C47 C48 Zr 65.68(19) . . . . ? O Zr C48 C47 174.54(19) . . . . ? O' Zr C48 C47 74.60(19) . . . . ? C46 Zr C48 C47 -36.78(17) . . . . ? C50 Zr C48 C47 -78.2(2) . . . . ? C43 Zr C48 C47 133.8(8) . . . . ? C41 Zr C48 C47 -33.0(2) . . . . ? C42 Zr C48 C47 11.6(3) . . . . ? C45 Zr C48 C47 -77.6(2) . . . . ? C44 Zr C48 C47 -121.9(2) . . . . ? C49 Zr C48 C47 -114.7(3) . . . . ? O Zr C48 C49 -70.77(18) . . . . ? O' Zr C48 C49 -170.71(18) . . . . ? C46 Zr C48 C49 77.91(19) . . . . ? C50 Zr C48 C49 36.53(16) . . . . ? C43 Zr C48 C49 -111.5(9) . . . . ? C47 Zr C48 C49 114.7(3) . . . . ? C41 Zr C48 C49 81.7(2) . . . . ? C42 Zr C48 C49 126.3(2) . . . . ? C45 Zr C48 C49 37.1(2) . . . . ? C44 Zr C48 C49 -7.2(3) . . . . ? C47 C48 C49 C50 1.3(3) . . . . ? Zr C48 C49 C50 -64.89(19) . . . . ? C47 C48 C49 Zr 66.23(19) . . . . ? O Zr C49 C50 -138.66(18) . . . . ? O' Zr C49 C50 126.14(17) . . . . ? C46 Zr C49 C50 38.06(17) . . . . ? C43 Zr C49 C50 -76.3(3) . . . . ? C47 Zr C49 C50 78.52(19) . . . . ? C41 Zr C49 C50 -6.4(2) . . . . ? C42 Zr C49 C50 -4.9(3) . . . . ? C45 Zr C49 C50 -36.86(19) . . . . ? C44 Zr C49 C50 -68.4(2) . . . . ? C48 Zr C49 C50 115.6(3) . . . . ? O Zr C49 C48 105.73(19) . . . . ? O' Zr C49 C48 10.5(2) . . . . ? C46 Zr C49 C48 -77.6(2) . . . . ? C50 Zr C49 C48 -115.6(3) . . . . ? C43 Zr C49 C48 168.1(2) . . . . ? C47 Zr C49 C48 -37.09(17) . . . . ? C41 Zr C49 C48 -121.97(18) . . . . ? C42 Zr C49 C48 -120.6(2) . . . . ? C45 Zr C49 C48 -152.46(18) . . . . ? C44 Zr C49 C48 175.95(17) . . . . ? C48 C49 C50 C46 -0.8(3) . . . . ? Zr C49 C50 C46 -66.20(19) . . . . ? C48 C49 C50 Zr 65.43(19) . . . . ? C47 C46 C50 C49 -0.1(3) . . . . ? Zr C46 C50 C49 67.97(19) . . . . ? C47 C46 C50 Zr -68.06(19) . . . . ? O Zr C50 C49 41.63(18) . . . . ? O' Zr C50 C49 -74.87(19) . . . . ? C46 Zr C50 C49 -114.2(3) . . . . ? C43 Zr C50 C49 138.81(17) . . . . ? C47 Zr C50 C49 -76.80(19) . . . . ? C41 Zr C50 C49 174.58(18) . . . . ? C42 Zr C50 C49 177.41(17) . . . . ? C45 Zr C50 C49 143.82(19) . . . . ? C44 Zr C50 C49 122.72(18) . . . . ? C48 Zr C50 C49 -36.61(17) . . . . ? O Zr C50 C46 155.85(17) . . . . ? O' Zr C50 C46 39.3(2) . . . . ? C43 Zr C50 C46 -106.97(19) . . . . ? C47 Zr C50 C46 37.42(17) . . . . ? C41 Zr C50 C46 -71.20(19) . . . . ? C42 Zr C50 C46 -68.4(2) . . . . ? C45 Zr C50 C46 -101.96(19) . . . . ? C44 Zr C50 C46 -123.06(18) . . . . ? C48 Zr C50 C46 77.61(19) . . . . ? C49 Zr C50 C46 114.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.419 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.055