# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'ProfD Annie-Claude Gaumont' _publ_contact_author_address ; ENSICAEN Laboratoire de chimie Molculaire et Thioorganique, UMR CNRS 6507 6 bd du Marchal Juin CAEN 14050 FRANCE ; _publ_contact_author_email GAUMONT@ENSICAEN.FR _publ_section_title ; Palladium catalysed enantioselective phosphination reactions using secondary phosphine-boranes and aryl iodide ; loop_ _publ_author_name 'Annie-Claude Gaumont' 'Stephanie Pican' data_sp844d1 _database_code_depnum_ccdc_archive 'CCDC 227137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H51 B F5 N O2 P2 Pd' _chemical_formula_weight 948.05 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Trigonal _symmetry_space_group_name_H-M P32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 11.9662(3) _cell_length_b 11.9662(3) _cell_length_c 26.4783(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3283.47(13) _cell_formula_units_Z 3 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method 'Area detector scans (see text)' _diffrn_detector_area_resol_mean 19.24 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6784 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6784 _reflns_number_gt 6578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1999)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+3.3111P] 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 -0.052(18) _refine_ls_number_reflns 6784 _refine_ls_number_parameters 541 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C53 C 0.3823(5) 0.7130(5) 0.4849(2) 0.0409(13) Uani 1 1 d . . . H53A H 0.3955 0.6673 0.4574 0.049 Uiso 1 1 calc R . . H53B H 0.3962 0.6788 0.5160 0.049 Uiso 1 1 calc R . . C51 C 0.6038(10) 0.8650(6) 0.4792(2) 0.101(4) Uani 1 1 d . . . H51A H 0.6593 0.9561 0.4745 0.152 Uiso 1 1 calc R . . H51B H 0.6138 0.8194 0.4514 0.152 Uiso 1 1 calc R . . H51C H 0.6264 0.8389 0.5101 0.152 Uiso 1 1 calc R . . C52 C 0.4762(13) 0.8368(12) 0.4818(4) 0.141(6) Uani 1 1 d . . . H52A H 0.4684 0.8817 0.5109 0.169 Uiso 1 1 calc R . . H52B H 0.4594 0.8736 0.4521 0.169 Uiso 1 1 calc R . . C54 C 0.2572(11) 0.6801(14) 0.4840(3) 0.135(5) Uani 1 1 d . . . H54A H 0.2421 0.7164 0.4538 0.162 Uiso 1 1 calc R . . H54B H 0.2406 0.7199 0.5128 0.162 Uiso 1 1 calc R . . C55 C 0.1667(10) 0.5460(14) 0.4850(7) 0.213(10) Uani 1 1 d . . . H55A H 0.0808 0.5329 0.4839 0.320 Uiso 1 1 calc R . . H55B H 0.1780 0.5089 0.5154 0.320 Uiso 1 1 calc R . . H55C H 0.1802 0.5053 0.4562 0.320 Uiso 1 1 calc R . . Pd1 Pd 0.61821(2) 0.36844(2) 0.304541(8) 0.01421(7) Uani 1 1 d . . . P1 P 0.40547(9) 0.31557(9) 0.31016(3) 0.01604(19) Uani 1 1 d . . . P2 P 0.83331(9) 0.41461(9) 0.29974(3) 0.01589(19) Uani 1 1 d . . . F1 F 0.6642(2) 0.5473(2) 0.20870(7) 0.0268(5) Uani 1 1 d . . . F2 F 0.7602(3) 0.8029(2) 0.19996(8) 0.0332(6) Uani 1 1 d . . . F3 F 0.8260(3) 0.9546(2) 0.28380(9) 0.0361(6) Uani 1 1 d . . . F4 F 0.7985(3) 0.8464(2) 0.37694(8) 0.0339(6) Uani 1 1 d . . . F5 F 0.7065(2) 0.5925(2) 0.38656(7) 0.0230(5) Uani 1 1 d . . . O1 O 0.4594(3) -0.0163(3) 0.35661(10) 0.0254(6) Uani 1 1 d . . . O2 O 0.7282(3) 0.3583(3) 0.40516(9) 0.0233(6) Uani 1 1 d . . . N1 N 0.5499(3) 0.1698(3) 0.31400(11) 0.0170(6) Uani 1 1 d . . . C1 C 0.3415(3) 0.2119(4) 0.36657(13) 0.0196(7) Uani 1 1 d . . . C2 C 0.2531(4) 0.2231(4) 0.39760(13) 0.0239(8) Uani 1 1 d . . . H2 H 0.2216 0.2769 0.3880 0.029 Uiso 1 1 calc R . . C3 C 0.2113(4) 0.1541(5) 0.44322(14) 0.0307(10) Uani 1 1 d . . . H3 H 0.1527 0.1622 0.4637 0.037 Uiso 1 1 calc R . . C4 C 0.2579(4) 0.0747(4) 0.45714(14) 0.0320(10) Uani 1 1 d . . . H4 H 0.2318 0.0302 0.4876 0.038 Uiso 1 1 calc R . . C5 C 0.3444(4) 0.0598(4) 0.42618(14) 0.0274(9) Uani 1 1 d . . . H5 H 0.3736 0.0041 0.4357 0.033 Uiso 1 1 calc R . . C6 C 0.3869(3) 0.1288(4) 0.38079(12) 0.0197(7) Uani 1 1 d . . . C7 C 0.4703(4) 0.1000(4) 0.34901(13) 0.0195(7) Uani 1 1 d . . . C8 C 0.5598(4) -0.0186(4) 0.32586(15) 0.0262(8) Uani 1 1 d . . . H8A H 0.5269 -0.1008 0.3087 0.031 Uiso 1 1 calc R . . H8B H 0.6333 -0.0031 0.3464 0.031 Uiso 1 1 calc R . . C9 C 0.5962(4) 0.0907(4) 0.28810(14) 0.0205(7) Uani 1 1 d . . . H9 H 0.6903 0.1409 0.2848 0.025 Uiso 1 1 calc R . . C10 C 0.5350(4) 0.0495(4) 0.23553(14) 0.0244(8) Uani 1 1 d . . . H10 H 0.5537 0.1280 0.2171 0.029 Uiso 1 1 calc R . . C11 C 0.5977(5) -0.0149(5) 0.20674(17) 0.0378(11) Uani 1 1 d . . . H11A H 0.5595 -0.0398 0.1738 0.057 Uiso 1 1 calc R . . H11B H 0.5847 -0.0900 0.2248 0.057 Uiso 1 1 calc R . . H11C H 0.6885 0.0446 0.2034 0.057 Uiso 1 1 calc R . . C12 C 0.3885(4) -0.0372(4) 0.23714(17) 0.0329(10) Uani 1 1 d . . . H12A H 0.3557 -0.0587 0.2033 0.049 Uiso 1 1 calc R . . H12B H 0.3509 0.0074 0.2537 0.049 Uiso 1 1 calc R . . H12C H 0.3670 -0.1148 0.2554 0.049 Uiso 1 1 calc R . . C13 C 0.3602(4) 0.4388(4) 0.31880(14) 0.0220(8) Uani 1 1 d . . . C14 C 0.4127(4) 0.5234(4) 0.35989(16) 0.0307(10) Uani 1 1 d . . . H14 H 0.4672 0.5142 0.3824 0.037 Uiso 1 1 calc R . . C15 C 0.3838(5) 0.6199(5) 0.3669(2) 0.0448(13) Uani 1 1 d . . . H15 H 0.4191 0.6758 0.3942 0.054 Uiso 1 1 calc R . . C16 C 0.3023(5) 0.6348(5) 0.3337(2) 0.0446(13) Uani 1 1 d . . . H16 H 0.2828 0.7001 0.3387 0.054 Uiso 1 1 calc R . . C17 C 0.2506(5) 0.5519(5) 0.2935(2) 0.0430(12) Uani 1 1 d . . . H17 H 0.1956 0.5611 0.2712 0.052 Uiso 1 1 calc R . . C18 C 0.2800(4) 0.4544(4) 0.28573(17) 0.0303(9) Uani 1 1 d . . . H18 H 0.2454 0.3995 0.2581 0.036 Uiso 1 1 calc R . . C19 C 0.3093(4) 0.2223(4) 0.25629(13) 0.0183(7) Uani 1 1 d . . . C20 C 0.1772(4) 0.1394(4) 0.25874(14) 0.0218(8) Uani 1 1 d . . . H20 H 0.1342 0.1252 0.2894 0.026 Uiso 1 1 calc R . . C21 C 0.1091(4) 0.0776(4) 0.21529(15) 0.0270(9) Uani 1 1 d . . . H21 H 0.0205 0.0215 0.2170 0.032 Uiso 1 1 calc R . . C22 C 0.1730(4) 0.0994(4) 0.16925(15) 0.0305(9) Uani 1 1 d . . . H22 H 0.1270 0.0584 0.1402 0.037 Uiso 1 1 calc R . . C23 C 0.3048(4) 0.1821(4) 0.16672(14) 0.0284(9) Uani 1 1 d . . . H23 H 0.3478 0.1958 0.1361 0.034 Uiso 1 1 calc R . . C24 C 0.3731(4) 0.2449(4) 0.21028(13) 0.0240(8) Uani 1 1 d . . . H24 H 0.4615 0.3020 0.2085 0.029 Uiso 1 1 calc R . . C25 C 0.6819(3) 0.5582(3) 0.29762(13) 0.0150(7) Uani 1 1 d . . . C26 C 0.6965(4) 0.6191(3) 0.25175(13) 0.0190(7) Uani 1 1 d . . . C27 C 0.7436(4) 0.7488(4) 0.24619(14) 0.0235(9) Uani 1 1 d . . . C28 C 0.7784(4) 0.8258(4) 0.28857(15) 0.0242(8) Uani 1 1 d . . . C29 C 0.7648(4) 0.7716(4) 0.33544(14) 0.0220(8) Uani 1 1 d . . . C30 C 0.7180(4) 0.6406(3) 0.33906(13) 0.0178(7) Uani 1 1 d . . . C31 C 0.9478(3) 0.5809(3) 0.31840(13) 0.0188(7) Uani 1 1 d . . . C32 C 0.9929(4) 0.6745(4) 0.28039(15) 0.0232(8) Uani 1 1 d . . . H32 H 0.9721 0.6497 0.2468 0.028 Uiso 1 1 calc R . . C33 C 1.0686(4) 0.8040(4) 0.29246(16) 0.0282(9) Uani 1 1 d . . . H33 H 1.0980 0.8658 0.2670 0.034 Uiso 1 1 calc R . . C34 C 1.1007(4) 0.8416(4) 0.34226(17) 0.0317(9) Uani 1 1 d . . . H34 H 1.1499 0.9287 0.3504 0.038 Uiso 1 1 calc R . . C35 C 1.0594(4) 0.7496(4) 0.37977(16) 0.0289(9) Uani 1 1 d . . . H35 H 1.0826 0.7745 0.4132 0.035 Uiso 1 1 calc R . . C36 C 0.9835(4) 0.6201(4) 0.36791(15) 0.0233(8) Uani 1 1 d . . . H36 H 0.9562 0.5586 0.3935 0.028 Uiso 1 1 calc R . . C37 C 0.8542(4) 0.3168(3) 0.34805(13) 0.0188(7) Uani 1 1 d . . . C38 C 0.9237(4) 0.2556(4) 0.33649(15) 0.0237(8) Uani 1 1 d . . . H38 H 0.9632 0.2691 0.3051 0.028 Uiso 1 1 calc R . . C39 C 0.9354(4) 0.1742(4) 0.37109(15) 0.0282(9) Uani 1 1 d . . . H39 H 0.9817 0.1334 0.3628 0.034 Uiso 1 1 calc R . . C40 C 0.8773(4) 0.1551(4) 0.41786(16) 0.0313(9) Uani 1 1 d . . . H40 H 0.8855 0.1015 0.4411 0.038 Uiso 1 1 calc R . . C41 C 0.8068(4) 0.2142(4) 0.43085(14) 0.0266(8) Uani 1 1 d . . . H41 H 0.7679 0.2002 0.4624 0.032 Uiso 1 1 calc R . . C42 C 0.7952(4) 0.2950(3) 0.39589(14) 0.0207(7) Uani 1 1 d . . . C43 C 0.6655(4) 0.3388(4) 0.45281(14) 0.0267(8) Uani 1 1 d . . . H43A H 0.6228 0.3886 0.4542 0.040 Uiso 1 1 calc R . . H43B H 0.7284 0.3659 0.4794 0.040 Uiso 1 1 calc R . . H43C H 0.6032 0.2490 0.4569 0.040 Uiso 1 1 calc R . . B1 B 0.8826(4) 0.3839(4) 0.23311(15) 0.0243(9) Uani 1 1 d . . . H1A H 0.8236 0.2969 0.2228 0.036 Uiso 1 1 calc R . . H1B H 0.9684 0.3967 0.2346 0.036 Uiso 1 1 calc R . . H1C H 0.8802 0.4429 0.2092 0.036 Uiso 1 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 C53 0.052(3) 0.044(3) 0.048(3) 0.030(2) 0.028(2) 0.040(3) C51 0.183(10) 0.032(3) 0.046(3) 0.009(3) 0.024(5) 0.022(5) C52 0.199(12) 0.176(11) 0.151(9) -0.121(9) -0.107(9) 0.171(11) C54 0.145(10) 0.274(16) 0.055(4) -0.068(7) -0.026(5) 0.156(11) C55 0.067(6) 0.210(14) 0.38(2) 0.226(16) 0.083(10) 0.079(8) Pd1 0.01280(13) 0.01294(13) 0.01490(11) -0.00041(10) 0.00057(10) 0.00494(11) P1 0.0137(4) 0.0166(4) 0.0160(4) -0.0018(4) 0.0007(3) 0.0062(4) P2 0.0144(4) 0.0158(4) 0.0155(4) 0.0004(3) 0.0014(3) 0.0061(4) F1 0.0399(14) 0.0243(12) 0.0162(10) -0.0038(9) -0.0019(9) 0.0160(11) F2 0.0499(16) 0.0250(12) 0.0235(11) 0.0087(10) 0.0058(11) 0.0177(12) F3 0.0503(17) 0.0164(12) 0.0389(13) 0.0016(10) 0.0022(12) 0.0147(12) F4 0.0487(16) 0.0228(12) 0.0249(11) -0.0105(10) -0.0041(11) 0.0138(12) F5 0.0287(12) 0.0239(11) 0.0147(9) -0.0003(8) -0.0011(9) 0.0118(10) O1 0.0257(15) 0.0184(14) 0.0310(14) 0.0071(11) 0.0052(12) 0.0101(12) O2 0.0314(15) 0.0248(14) 0.0167(12) 0.0042(10) 0.0052(11) 0.0161(12) N1 0.0153(15) 0.0191(16) 0.0181(14) 0.0035(13) 0.0028(12) 0.0098(13) C1 0.0134(17) 0.0215(19) 0.0182(17) -0.0032(14) -0.0002(14) 0.0044(15) C2 0.0178(18) 0.027(2) 0.0209(17) -0.0009(16) 0.0014(15) 0.0065(16) C3 0.020(2) 0.044(3) 0.0181(18) -0.0050(17) 0.0023(15) 0.0079(19) C4 0.028(2) 0.040(2) 0.0163(17) 0.0022(17) 0.0020(16) 0.008(2) C5 0.022(2) 0.028(2) 0.0207(18) 0.0037(16) -0.0014(15) 0.0035(17) C6 0.0157(17) 0.0217(19) 0.0136(15) 0.0001(14) 0.0014(13) 0.0032(15) C7 0.0185(18) 0.0164(18) 0.0190(16) -0.0021(14) -0.0042(14) 0.0052(15) C8 0.025(2) 0.0203(19) 0.034(2) 0.0030(16) -0.0005(17) 0.0115(17) C9 0.0145(17) 0.0194(18) 0.0268(18) -0.0026(15) -0.0005(14) 0.0078(15) C10 0.026(2) 0.025(2) 0.0241(18) -0.0049(16) -0.0004(16) 0.0140(17) C11 0.040(3) 0.041(3) 0.040(2) -0.015(2) -0.001(2) 0.025(2) C12 0.030(2) 0.033(2) 0.034(2) -0.0090(19) -0.0105(19) 0.014(2) C13 0.0182(18) 0.0198(18) 0.0283(19) -0.0038(15) 0.0019(15) 0.0097(16) C14 0.025(2) 0.031(2) 0.033(2) -0.0139(18) -0.0032(18) 0.0124(19) C15 0.030(2) 0.037(3) 0.070(3) -0.028(2) 0.001(2) 0.018(2) C16 0.029(2) 0.028(2) 0.083(4) -0.007(2) 0.009(2) 0.020(2) C17 0.033(2) 0.028(2) 0.075(3) -0.009(2) -0.009(2) 0.020(2) C18 0.028(2) 0.024(2) 0.042(2) -0.0072(18) -0.0073(19) 0.0149(19) C19 0.023(2) 0.0181(18) 0.0174(16) 0.0014(14) 0.0021(15) 0.0130(16) C20 0.022(2) 0.0195(19) 0.0207(17) 0.0002(15) -0.0008(15) 0.0082(16) C21 0.0205(19) 0.027(2) 0.027(2) 0.0002(17) -0.0051(16) 0.0068(17) C22 0.037(2) 0.029(2) 0.0249(19) -0.0052(17) -0.0122(18) 0.0156(19) C23 0.033(2) 0.037(2) 0.0168(17) -0.0014(16) 0.0010(16) 0.0179(19) C24 0.0227(19) 0.027(2) 0.0223(18) 0.0019(16) 0.0016(15) 0.0128(17) C25 0.0109(16) 0.0125(16) 0.0199(16) -0.0007(13) -0.0003(13) 0.0047(14) C26 0.0233(19) 0.0164(17) 0.0163(16) -0.0015(14) 0.0018(14) 0.0092(16) C27 0.028(2) 0.023(2) 0.0210(18) 0.0068(16) 0.0045(16) 0.0143(18) C28 0.026(2) 0.0140(18) 0.0317(19) -0.0006(15) 0.0003(17) 0.0094(16) C29 0.0237(19) 0.0191(18) 0.0222(18) -0.0071(15) -0.0011(15) 0.0098(16) C30 0.0189(18) 0.0175(18) 0.0158(15) 0.0006(14) 0.0004(13) 0.0082(15) C31 0.0144(17) 0.0173(18) 0.0224(17) -0.0025(14) -0.0024(14) 0.0063(14) C32 0.0176(19) 0.0190(19) 0.0261(19) 0.0021(16) 0.0004(15) 0.0040(16) C33 0.023(2) 0.021(2) 0.035(2) 0.0070(17) 0.0024(17) 0.0060(17) C34 0.023(2) 0.0171(19) 0.044(2) -0.0025(18) -0.0013(18) 0.0022(17) C35 0.022(2) 0.025(2) 0.032(2) -0.0096(17) -0.0073(17) 0.0068(17) C36 0.0197(19) 0.024(2) 0.0206(17) 0.0021(16) -0.0009(15) 0.0065(17) C37 0.0183(18) 0.0148(17) 0.0197(16) -0.0004(14) 0.0019(14) 0.0057(15) C38 0.0207(19) 0.023(2) 0.0278(19) -0.0055(16) -0.0054(16) 0.0110(16) C39 0.026(2) 0.029(2) 0.036(2) -0.0058(18) -0.0093(18) 0.0184(18) C40 0.037(2) 0.026(2) 0.035(2) -0.0021(18) -0.0146(19) 0.0193(19) C41 0.033(2) 0.024(2) 0.0223(18) 0.0001(16) -0.0046(16) 0.0143(18) C42 0.0222(19) 0.0156(18) 0.0233(17) -0.0005(14) -0.0019(15) 0.0086(15) C43 0.031(2) 0.033(2) 0.0164(16) 0.0003(16) 0.0009(15) 0.0167(19) B1 0.026(2) 0.024(2) 0.020(2) -0.0016(17) 0.0058(17) 0.0104(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C53 C54 1.344(10) . ? C53 C52 1.342(14) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C51 C52 1.392(13) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C54 C55 1.419(17) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? Pd1 C25 2.010(3) . ? Pd1 N1 2.107(3) . ? Pd1 P1 2.3005(10) . ? Pd1 P2 2.3504(10) . ? P1 C13 1.822(4) . ? P1 C19 1.822(4) . ? P1 C1 1.845(4) . ? P2 C31 1.832(4) . ? P2 C37 1.833(4) . ? P2 B1 1.953(4) . ? F1 C26 1.362(4) . ? F2 C27 1.352(4) . ? F3 C28 1.356(4) . ? F4 C29 1.345(4) . ? F5 C30 1.361(4) . ? O1 C7 1.346(5) . ? O1 C8 1.463(5) . ? O2 C42 1.373(5) . ? O2 C43 1.426(4) . ? N1 C7 1.292(5) . ? N1 C9 1.482(5) . ? C1 C2 1.397(5) . ? C1 C6 1.403(5) . ? C2 C3 1.407(5) . ? C2 H2 0.9300 . ? C3 C4 1.371(7) . ? C3 H3 0.9300 . ? C4 C5 1.399(6) . ? C4 H4 0.9300 . ? C5 C6 1.402(5) . ? C5 H5 0.9300 . ? C6 C7 1.472(5) . ? C8 C9 1.527(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.535(5) . ? C9 H9 0.9800 . ? C10 C11 1.522(6) . ? C10 C12 1.526(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.379(6) . ? C13 C14 1.403(5) . ? C14 C15 1.374(7) . ? C14 H14 0.9300 . ? C15 C16 1.388(8) . ? C15 H15 0.9300 . ? C16 C17 1.374(7) . ? C16 H16 0.9300 . ? C17 C18 1.392(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.386(5) . ? C19 C24 1.391(5) . ? C20 C21 1.390(5) . ? C20 H20 0.9300 . ? C21 C22 1.393(6) . ? C21 H21 0.9300 . ? C22 C23 1.382(6) . ? C22 H22 0.9300 . ? C23 C24 1.396(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.382(5) . ? C25 C30 1.391(5) . ? C26 C27 1.369(5) . ? C27 C28 1.378(6) . ? C28 C29 1.372(5) . ? C29 C30 1.380(5) . ? C31 C36 1.386(5) . ? C31 C32 1.398(5) . ? C32 C33 1.385(6) . ? C32 H32 0.9300 . ? C33 C34 1.384(6) . ? C33 H33 0.9300 . ? C34 C35 1.379(6) . ? C34 H34 0.9300 . ? C35 C36 1.385(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.390(5) . ? C37 C42 1.409(5) . ? C38 C39 1.394(6) . ? C38 H38 0.9300 . ? C39 C40 1.383(6) . ? C39 H39 0.9300 . ? C40 C41 1.387(6) . ? C40 H40 0.9300 . ? C41 C42 1.394(5) . ? C41 H41 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? B1 H1A 0.9600 . ? B1 H1B 0.9600 . ? B1 H1C 0.9600 . ? 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 C54 C53 C52 121.1(8) . . ? C54 C53 H53A 107.1 . . ? C52 C53 H53A 107.1 . . ? C54 C53 H53B 107.0 . . ? C52 C53 H53B 107.0 . . ? H53A C53 H53B 106.8 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.4 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C51 118.8(7) . . ? C53 C52 H52A 107.7 . . ? C51 C52 H52A 107.6 . . ? C53 C52 H52B 107.6 . . ? C51 C52 H52B 107.6 . . ? H52A C52 H52B 107.1 . . ? C53 C54 C55 116.0(10) . . ? C53 C54 H54A 108.3 . . ? C55 C54 H54A 108.3 . . ? C53 C54 H54B 108.3 . . ? C55 C54 H54B 108.3 . . ? H54A C54 H54B 107.4 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C25 Pd1 N1 178.32(13) . . ? C25 Pd1 P1 93.37(10) . . ? N1 Pd1 P1 86.02(9) . . ? C25 Pd1 P2 88.71(10) . . ? N1 Pd1 P2 91.88(9) . . ? P1 Pd1 P2 177.87(4) . . ? C13 P1 C19 103.99(17) . . ? C13 P1 C1 104.54(18) . . ? C19 P1 C1 107.41(17) . . ? C13 P1 Pd1 121.44(13) . . ? C19 P1 Pd1 113.00(13) . . ? C1 P1 Pd1 105.51(12) . . ? C31 P2 C37 103.82(16) . . ? C31 P2 B1 108.42(18) . . ? C37 P2 B1 111.07(18) . . ? C31 P2 Pd1 112.15(12) . . ? C37 P2 Pd1 107.16(12) . . ? B1 P2 Pd1 113.78(14) . . ? C7 O1 C8 106.3(3) . . ? C42 O2 C43 118.2(3) . . ? C7 N1 C9 108.1(3) . . ? C7 N1 Pd1 124.0(3) . . ? C9 N1 Pd1 127.4(2) . . ? C2 C1 C6 119.4(3) . . ? C2 C1 P1 119.4(3) . . ? C6 C1 P1 121.1(3) . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.5(4) . . ? C5 C6 C7 116.2(4) . . ? C1 C6 C7 124.1(3) . . ? N1 C7 O1 115.7(3) . . ? N1 C7 C6 128.8(3) . . ? O1 C7 C6 115.5(3) . . ? O1 C8 C9 103.5(3) . . ? O1 C8 H8A 111.1 . . ? C9 C8 H8A 111.1 . . ? O1 C8 H8B 111.1 . . ? C9 C8 H8B 111.1 . . ? H8A C8 H8B 109.0 . . ? N1 C9 C8 101.9(3) . . ? N1 C9 C10 110.7(3) . . ? C8 C9 C10 115.6(3) . . ? N1 C9 H9 109.4 . . ? C8 C9 H9 109.4 . . ? C10 C9 H9 109.4 . . ? C11 C10 C12 111.1(4) . . ? C11 C10 C9 109.9(3) . . ? C12 C10 C9 113.2(3) . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C9 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.0(4) . . ? C18 C13 P1 122.6(3) . . ? C14 C13 P1 118.3(3) . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.6(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 120.3(4) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C24 119.9(3) . . ? C20 C19 P1 123.2(3) . . ? C24 C19 P1 116.7(3) . . ? C19 C20 C21 119.9(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.8(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.1(4) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C30 114.0(3) . . ? C26 C25 Pd1 123.5(3) . . ? C30 C25 Pd1 122.4(3) . . ? F1 C26 C27 116.8(3) . . ? F1 C26 C25 118.8(3) . . ? C27 C26 C25 124.4(3) . . ? F2 C27 C26 121.2(3) . . ? F2 C27 C28 119.6(4) . . ? C26 C27 C28 119.1(4) . . ? F3 C28 C29 120.3(3) . . ? F3 C28 C27 119.9(3) . . ? C29 C28 C27 119.7(4) . . ? F4 C29 C28 119.9(3) . . ? F4 C29 C30 121.0(3) . . ? C28 C29 C30 119.0(3) . . ? F5 C30 C29 116.3(3) . . ? F5 C30 C25 119.9(3) . . ? C29 C30 C25 123.8(3) . . ? C36 C31 C32 118.7(3) . . ? C36 C31 P2 124.0(3) . . ? C32 C31 P2 117.1(3) . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.3(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.2(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.8(4) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C38 C37 C42 118.4(3) . . ? C38 C37 P2 119.4(3) . . ? C42 C37 P2 122.0(3) . . ? C37 C38 C39 121.3(4) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 119.1(4) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 121.5(4) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C40 C41 C42 119.0(4) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? O2 C42 C41 123.5(3) . . ? O2 C42 C37 115.8(3) . . ? C41 C42 C37 120.8(4) . . ? O2 C43 H43A 109.5 . . ? O2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P2 B1 H1A 109.5 . . ? P2 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? P2 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C54 C53 C52 C51 -175.4(7) . . . . ? C52 C53 C54 C55 176.8(11) . . . . ? C25 Pd1 P1 C13 -11.22(18) . . . . ? N1 Pd1 P1 C13 167.21(17) . . . . ? P2 Pd1 P1 C13 157.2(9) . . . . ? C25 Pd1 P1 C19 113.34(16) . . . . ? N1 Pd1 P1 C19 -68.22(15) . . . . ? P2 Pd1 P1 C19 -78.2(10) . . . . ? C25 Pd1 P1 C1 -129.59(16) . . . . ? N1 Pd1 P1 C1 48.85(14) . . . . ? P2 Pd1 P1 C1 38.8(10) . . . . ? C25 Pd1 P2 C31 23.45(16) . . . . ? N1 Pd1 P2 C31 -154.98(15) . . . . ? P1 Pd1 P2 C31 -145.0(9) . . . . ? C25 Pd1 P2 C37 136.75(15) . . . . ? N1 Pd1 P2 C37 -41.68(15) . . . . ? P1 Pd1 P2 C37 -31.7(10) . . . . ? C25 Pd1 P2 B1 -100.07(18) . . . . ? N1 Pd1 P2 B1 81.50(17) . . . . ? P1 Pd1 P2 B1 91.5(10) . . . . ? C25 Pd1 N1 C7 20(5) . . . . ? P1 Pd1 N1 C7 -49.0(3) . . . . ? P2 Pd1 N1 C7 130.6(3) . . . . ? C25 Pd1 N1 C9 -151(5) . . . . ? P1 Pd1 N1 C9 140.5(3) . . . . ? P2 Pd1 N1 C9 -39.8(3) . . . . ? C13 P1 C1 C2 13.4(3) . . . . ? C19 P1 C1 C2 -96.6(3) . . . . ? Pd1 P1 C1 C2 142.6(3) . . . . ? C13 P1 C1 C6 -162.0(3) . . . . ? C19 P1 C1 C6 88.0(3) . . . . ? Pd1 P1 C1 C6 -32.8(3) . . . . ? C6 C1 C2 C3 1.2(5) . . . . ? P1 C1 C2 C3 -174.3(3) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 -1.2(6) . . . . ? C3 C4 C5 C6 1.5(6) . . . . ? C4 C5 C6 C1 -0.4(5) . . . . ? C4 C5 C6 C7 -175.8(4) . . . . ? C2 C1 C6 C5 -0.9(5) . . . . ? P1 C1 C6 C5 174.5(3) . . . . ? C2 C1 C6 C7 174.1(3) . . . . ? P1 C1 C6 C7 -10.5(5) . . . . ? C9 N1 C7 O1 6.3(4) . . . . ? Pd1 N1 C7 O1 -165.7(2) . . . . ? C9 N1 C7 C6 -171.7(3) . . . . ? Pd1 N1 C7 C6 16.3(5) . . . . ? C8 O1 C7 N1 8.0(4) . . . . ? C8 O1 C7 C6 -173.7(3) . . . . ? C5 C6 C7 N1 -158.9(4) . . . . ? C1 C6 C7 N1 26.0(6) . . . . ? C5 C6 C7 O1 23.1(5) . . . . ? C1 C6 C7 O1 -152.1(3) . . . . ? C7 O1 C8 C9 -18.0(4) . . . . ? C7 N1 C9 C8 -16.9(4) . . . . ? Pd1 N1 C9 C8 154.7(2) . . . . ? C7 N1 C9 C10 106.6(4) . . . . ? Pd1 N1 C9 C10 -81.7(4) . . . . ? O1 C8 C9 N1 20.6(4) . . . . ? O1 C8 C9 C10 -99.5(4) . . . . ? N1 C9 C10 C11 172.0(3) . . . . ? C8 C9 C10 C11 -72.8(4) . . . . ? N1 C9 C10 C12 -63.2(4) . . . . ? C8 C9 C10 C12 52.0(5) . . . . ? C19 P1 C13 C18 -5.8(4) . . . . ? C1 P1 C13 C18 -118.3(4) . . . . ? Pd1 P1 C13 C18 122.8(3) . . . . ? C19 P1 C13 C14 176.3(3) . . . . ? C1 P1 C13 C14 63.8(4) . . . . ? Pd1 P1 C13 C14 -55.0(4) . . . . ? C18 C13 C14 C15 0.3(6) . . . . ? P1 C13 C14 C15 178.2(4) . . . . ? C13 C14 C15 C16 0.2(7) . . . . ? C14 C15 C16 C17 -0.1(8) . . . . ? C15 C16 C17 C18 -0.4(8) . . . . ? C14 C13 C18 C17 -0.8(7) . . . . ? P1 C13 C18 C17 -178.6(4) . . . . ? C16 C17 C18 C13 0.8(8) . . . . ? C13 P1 C19 C20 -71.8(4) . . . . ? C1 P1 C19 C20 38.6(4) . . . . ? Pd1 P1 C19 C20 154.6(3) . . . . ? C13 P1 C19 C24 103.4(3) . . . . ? C1 P1 C19 C24 -146.2(3) . . . . ? Pd1 P1 C19 C24 -30.2(3) . . . . ? C24 C19 C20 C21 0.9(6) . . . . ? P1 C19 C20 C21 176.0(3) . . . . ? C19 C20 C21 C22 -0.5(6) . . . . ? C20 C21 C22 C23 0.5(6) . . . . ? C21 C22 C23 C24 -0.9(7) . . . . ? C20 C19 C24 C23 -1.4(6) . . . . ? P1 C19 C24 C23 -176.8(3) . . . . ? C22 C23 C24 C19 1.4(6) . . . . ? N1 Pd1 C25 C26 -159(5) . . . . ? P1 Pd1 C25 C26 -90.0(3) . . . . ? P2 Pd1 C25 C26 90.4(3) . . . . ? N1 Pd1 C25 C30 23(5) . . . . ? P1 Pd1 C25 C30 91.5(3) . . . . ? P2 Pd1 C25 C30 -88.1(3) . . . . ? C30 C25 C26 F1 179.8(3) . . . . ? Pd1 C25 C26 F1 1.1(5) . . . . ? C30 C25 C26 C27 0.9(6) . . . . ? Pd1 C25 C26 C27 -177.7(3) . . . . ? F1 C26 C27 F2 -1.6(6) . . . . ? C25 C26 C27 F2 177.3(3) . . . . ? F1 C26 C27 C28 -179.6(3) . . . . ? C25 C26 C27 C28 -0.7(6) . . . . ? F2 C27 C28 F3 1.6(6) . . . . ? C26 C27 C28 F3 179.7(4) . . . . ? F2 C27 C28 C29 -178.4(4) . . . . ? C26 C27 C28 C29 -0.3(6) . . . . ? F3 C28 C29 F4 0.1(6) . . . . ? C27 C28 C29 F4 -179.9(4) . . . . ? F3 C28 C29 C30 -179.0(4) . . . . ? C27 C28 C29 C30 1.0(6) . . . . ? F4 C29 C30 F5 1.0(5) . . . . ? C28 C29 C30 F5 -179.9(3) . . . . ? F4 C29 C30 C25 -179.8(3) . . . . ? C28 C29 C30 C25 -0.8(6) . . . . ? C26 C25 C30 F5 179.0(3) . . . . ? Pd1 C25 C30 F5 -2.4(5) . . . . ? C26 C25 C30 C29 -0.2(5) . . . . ? Pd1 C25 C30 C29 178.5(3) . . . . ? C37 P2 C31 C36 -30.3(4) . . . . ? B1 P2 C31 C36 -148.5(3) . . . . ? Pd1 P2 C31 C36 85.1(3) . . . . ? C37 P2 C31 C32 155.0(3) . . . . ? B1 P2 C31 C32 36.8(4) . . . . ? Pd1 P2 C31 C32 -89.6(3) . . . . ? C36 C31 C32 C33 -1.9(6) . . . . ? P2 C31 C32 C33 173.1(3) . . . . ? C31 C32 C33 C34 0.3(6) . . . . ? C32 C33 C34 C35 1.5(6) . . . . ? C33 C34 C35 C36 -1.6(6) . . . . ? C34 C35 C36 C31 0.0(6) . . . . ? C32 C31 C36 C35 1.8(6) . . . . ? P2 C31 C36 C35 -172.8(3) . . . . ? C31 P2 C37 C38 -103.3(3) . . . . ? B1 P2 C37 C38 13.0(4) . . . . ? Pd1 P2 C37 C38 137.8(3) . . . . ? C31 P2 C37 C42 80.6(3) . . . . ? B1 P2 C37 C42 -163.1(3) . . . . ? Pd1 P2 C37 C42 -38.2(3) . . . . ? C42 C37 C38 C39 0.0(6) . . . . ? P2 C37 C38 C39 -176.2(3) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C38 C39 C40 C41 0.6(6) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C43 O2 C42 C41 -0.9(5) . . . . ? C43 O2 C42 C37 179.4(3) . . . . ? C40 C41 C42 O2 -179.7(4) . . . . ? C40 C41 C42 C37 -0.1(6) . . . . ? C38 C37 C42 O2 179.9(3) . . . . ? P2 C37 C42 O2 -4.0(5) . . . . ? C38 C37 C42 C41 0.2(6) . . . . ? P2 C37 C42 C41 176.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.002 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.073