Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name N.Norman 'Christopher J. Adams' 'R. Angharad Baber' A.Batsanov 'George Bramham' 'Jonathan Charmant' 'Mairi F. Haddow' J.Howard 'Wai Han Lam.' 'Zhenyang Lin.' 'Todd Marder' A.Orpen _publ_contact_author_name N.Norman _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email N.C.NORMAN@BRISTOL.AC.UK _publ_section_title ; Synthesis and Reactivity of Cobalt Boryl Complexes ; data_2 _database_code_depnum_ccdc_archive 'CCDC 290418' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C23 H39 B2 Co O4 P3' _chemical_formula_sum 'C23 H39 B2 Co O4 P3' _chemical_formula_weight 553.00 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3126(12) _cell_length_b 16.2340(16) _cell_length_c 16.3156(16) _cell_angle_alpha 110.985(2) _cell_angle_beta 91.761(2) _cell_angle_gamma 108.279(2) _cell_volume 2853.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.42 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method none _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30455 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12934 _reflns_number_gt 6776 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The methyl substituent (C37A/C37B) on one of the catecholate rings is disordered over two positions. Using a free variable to evaluate the relative occupancies at these positions, an approximate 1:1 occupancy ratio was found. ; _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^)+(0.0509P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 12934 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1217 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0757(3) 0.5236(3) 0.1906(2) 0.0446(10) Uani 1 1 d . . . C2 C 0.0920(3) 0.4972(3) 0.1027(2) 0.0605(12) Uani 1 1 d . . . H2A H 0.0907 0.5349 0.0699 0.073 Uiso 1 1 calc R . . C3 C 0.1109(3) 0.4104(3) 0.0645(3) 0.0650(14) Uani 1 1 d . . . C4 C 0.1101(4) 0.3555(3) 0.1110(3) 0.0721(13) Uani 1 1 d . . . H4A H 0.1214 0.2972 0.0829 0.087 Uiso 1 1 calc R . . C5 C 0.0929(4) 0.3835(3) 0.1988(3) 0.0644(12) Uani 1 1 d . . . H5A H 0.0929 0.3456 0.2316 0.077 Uiso 1 1 calc R . . C6 C 0.0758(3) 0.4684(3) 0.2373(2) 0.0468(10) Uani 1 1 d . . . C7 C 0.1359(4) 0.3763(4) -0.0281(3) 0.0970(18) Uani 1 1 d . . . H7A H 0.1376 0.3124 -0.0449 0.146 Uiso 1 1 calc R . . H7B H 0.2112 0.4183 -0.0314 0.146 Uiso 1 1 calc R . . H7C H 0.0752 0.3757 -0.0688 0.146 Uiso 1 1 calc R . . C8 C 0.3492(3) 0.7447(2) 0.5036(2) 0.0339(8) Uani 1 1 d . . . C9 C 0.4438(3) 0.7439(2) 0.5481(2) 0.0439(9) Uani 1 1 d . . . H9A H 0.4374 0.7008 0.5762 0.053 Uiso 1 1 calc R . . C10 C 0.5507(3) 0.8091(2) 0.5509(2) 0.0428(9) Uani 1 1 d . . . H10A H 0.6181 0.8100 0.5816 0.051 Uiso 1 1 calc R . . C11 C 0.5623(3) 0.8725(2) 0.5105(2) 0.0365(8) Uani 1 1 d . . . C12 C 0.4639(3) 0.8709(2) 0.4647(2) 0.0354(8) Uani 1 1 d . . . H12A H 0.4697 0.9133 0.4359 0.043 Uiso 1 1 calc R . . C13 C 0.3588(3) 0.8073(2) 0.4619(2) 0.0299(7) Uani 1 1 d . . . C14 C 0.6790(3) 0.9439(3) 0.5168(3) 0.0544(11) Uani 1 1 d . . . H14A H 0.7383 0.9361 0.5520 0.082 Uiso 1 1 calc R . . H14B H 0.6766 1.0075 0.5456 0.082 Uiso 1 1 calc R . . H14C H 0.6979 0.9343 0.4570 0.082 Uiso 1 1 calc R . . C15 C -0.1073(4) 0.8522(3) 0.4112(3) 0.0917(17) Uani 1 1 d . . . H15A H -0.1295 0.8757 0.3681 0.138 Uiso 1 1 calc R . . H15B H -0.0514 0.9046 0.4610 0.138 Uiso 1 1 calc R . . H15C H -0.1763 0.8235 0.4334 0.138 Uiso 1 1 calc R . . C16 C -0.1470(3) 0.6980(3) 0.2547(2) 0.0623(12) Uani 1 1 d . . . H16A H -0.1564 0.7414 0.2284 0.093 Uiso 1 1 calc R . . H16B H -0.2216 0.6658 0.2683 0.093 Uiso 1 1 calc R . . H16C H -0.1196 0.6514 0.2126 0.093 Uiso 1 1 calc R . . C17 C 0.0767(3) 0.8322(3) 0.3168(3) 0.0766(15) Uani 1 1 d . . . H17A H 0.0466 0.8648 0.2865 0.115 Uiso 1 1 calc R . . H17B H 0.1098 0.7898 0.2751 0.115 Uiso 1 1 calc R . . H17C H 0.1369 0.8785 0.3672 0.115 Uiso 1 1 calc R . . C18 C -0.1721(4) 0.5059(3) 0.4755(3) 0.0835(16) Uani 1 1 d . . . H18A H -0.2455 0.4529 0.4586 0.125 Uiso 1 1 calc R . . H18B H -0.1636 0.5466 0.5382 0.125 Uiso 1 1 calc R . . H18C H -0.1077 0.4820 0.4668 0.125 Uiso 1 1 calc R . . C19 C -0.3014(3) 0.6022(3) 0.4285(3) 0.0643(12) Uani 1 1 d . . . H19A H -0.3673 0.5449 0.4184 0.096 Uiso 1 1 calc R . . H19B H -0.3170 0.6314 0.3884 0.096 Uiso 1 1 calc R . . H19C H -0.2899 0.6463 0.4903 0.096 Uiso 1 1 calc R . . C20 C -0.2276(3) 0.4772(3) 0.2973(3) 0.0702(13) Uani 1 1 d . . . H20A H -0.3038 0.4348 0.2985 0.105 Uiso 1 1 calc R . . H20B H -0.1743 0.4422 0.2819 0.105 Uiso 1 1 calc R . . H20C H -0.2350 0.5037 0.2529 0.105 Uiso 1 1 calc R . . C21 C 0.1183(3) 0.8970(3) 0.6052(3) 0.0632(12) Uani 1 1 d . . . H21A H 0.1192 0.9311 0.6686 0.095 Uiso 1 1 calc R . . H21B H 0.0928 0.9279 0.5706 0.095 Uiso 1 1 calc R . . H21C H 0.1964 0.8970 0.5955 0.095 Uiso 1 1 calc R . . C22 C 0.0788(4) 0.7391(3) 0.6493(2) 0.0644(12) Uani 1 1 d . . . H22A H 0.0835 0.7833 0.7100 0.097 Uiso 1 1 calc R . . H22B H 0.1565 0.7388 0.6386 0.097 Uiso 1 1 calc R . . H22C H 0.0287 0.6758 0.6419 0.097 Uiso 1 1 calc R . . C23 C -0.1059(4) 0.7977(3) 0.6211(3) 0.0756(14) Uani 1 1 d . . . H23A H -0.0781 0.8479 0.6805 0.113 Uiso 1 1 calc R . . H23B H -0.1568 0.7401 0.6259 0.113 Uiso 1 1 calc R . . H23C H -0.1491 0.8168 0.5842 0.113 Uiso 1 1 calc R . . B1 B 0.0471(3) 0.5995(3) 0.3299(3) 0.0363(10) Uani 1 1 d . . . B2 B 0.1688(3) 0.7210(3) 0.4423(2) 0.0333(9) Uani 1 1 d . . . Co1 Co -0.00062(4) 0.68231(3) 0.42954(3) 0.03069(12) Uani 1 1 d . . . O1 O 0.05860(19) 0.60545(16) 0.24443(14) 0.0432(6) Uani 1 1 d . . . O2 O 0.0603(2) 0.51286(17) 0.32267(15) 0.0454(6) Uani 1 1 d . . . O3 O 0.23440(18) 0.69006(15) 0.49124(15) 0.0402(6) Uani 1 1 d . . . O4 O 0.25053(17) 0.79332(15) 0.42237(14) 0.0345(5) Uani 1 1 d . . . P1 P -0.04116(8) 0.76396(7) 0.35721(7) 0.0445(3) Uani 1 1 d . . . P2 P -0.17120(8) 0.57260(7) 0.40693(6) 0.0402(2) Uani 1 1 d . . . P3 P 0.01839(8) 0.77558(7) 0.56982(6) 0.0429(2) Uani 1 1 d . . . C24 C 0.4205(3) 0.3558(2) 1.1490(2) 0.0369(8) Uani 1 1 d . . . C25 C 0.4016(3) 0.4345(3) 1.2037(2) 0.0440(9) Uani 1 1 d . . . H25A H 0.3922 0.4792 1.1818 0.053 Uiso 1 1 calc R . . C26 C 0.3963(3) 0.4476(3) 1.2928(2) 0.0472(10) Uani 1 1 d . . . C27 C 0.4098(3) 0.3809(3) 1.3216(2) 0.0512(10) Uani 1 1 d . . . H27A H 0.4061 0.3902 1.3822 0.061 Uiso 1 1 calc R . . C28 C 0.4285(3) 0.3007(3) 1.2661(2) 0.0508(10) Uani 1 1 d . . . H28A H 0.4365 0.2551 1.2872 0.061 Uiso 1 1 calc R . . C29 C 0.4349(3) 0.2901(2) 1.1790(2) 0.0375(8) Uani 1 1 d . . . C30 C 0.3765(4) 0.5332(3) 1.3560(3) 0.0706(13) Uani 1 1 d . . . H30A H 0.3818 0.5335 1.4162 0.106 Uiso 1 1 calc R . . H30B H 0.2994 0.5320 1.3375 0.106 Uiso 1 1 calc R . . H30C H 0.4355 0.5900 1.3556 0.106 Uiso 1 1 calc R . . C31 C 0.1470(3) 0.0799(3) 0.8834(2) 0.0615(13) Uani 1 1 d . B . C32 C 0.0367(4) 0.0743(4) 0.8576(3) 0.0830(16) Uani 1 1 d . . . H32 H 0.0234 0.1214 0.8413 0.100 Uiso 1 1 calc R A 1 C33A C -0.0537(4) -0.0023(5) 0.8562(3) 0.104(2) Uani 0.489(6) 1 d P B 1 C34A C -0.0351(5) -0.0693(4) 0.8793(4) 0.106(3) Uani 0.489(6) 1 d P B 1 H34A H -0.0996 -0.1211 0.8777 0.128 Uiso 0.489(6) 1 calc PR B 1 C33B C -0.0537(4) -0.0023(5) 0.8562(3) 0.104(2) Uani 0.511(6) 1 d P B 2 H33B H -0.1310 -0.0081 0.8387 0.125 Uiso 0.511(6) 1 calc PR B 2 C34B C -0.0351(5) -0.0693(4) 0.8793(4) 0.106(3) Uani 0.511(6) 1 d P B 2 C35 C 0.0773(4) -0.0643(3) 0.9057(3) 0.0802(16) Uani 1 1 d . . . H35 H 0.0903 -0.1119 0.9213 0.096 Uiso 1 1 calc R B 1 C36 C 0.1672(3) 0.0124(3) 0.9078(3) 0.0584(12) Uani 1 1 d . B . C37A C -0.1757(7) -0.0366(7) 0.8322(6) 0.070(3) Uani 0.489(6) 1 d P B 1 H37A H -0.2025 -0.1042 0.7956 0.106 Uiso 0.489(6) 1 calc PR B 1 H37B H -0.1973 -0.0035 0.7982 0.106 Uiso 0.489(6) 1 calc PR B 1 H37C H -0.2116 -0.0258 0.8860 0.106 Uiso 0.489(6) 1 calc PR B 1 C37B C -0.1479(6) -0.1387(5) 0.8699(5) 0.052(2) Uani 0.511(6) 1 d P B 2 H37D H -0.1480 -0.1626 0.9172 0.078 Uiso 0.511(6) 1 calc PR B 2 H37E H -0.1647 -0.1909 0.8119 0.078 Uiso 0.511(6) 1 calc PR B 2 H37F H -0.2073 -0.1095 0.8743 0.078 Uiso 0.511(6) 1 calc PR B 2 C38 C 0.6270(3) 0.3055(3) 0.7966(3) 0.0591(11) Uani 1 1 d . . . H38A H 0.6062 0.3298 0.7537 0.089 Uiso 1 1 calc R . . H38B H 0.6586 0.2560 0.7670 0.089 Uiso 1 1 calc R . . H38C H 0.6853 0.3568 0.8456 0.089 Uiso 1 1 calc R . . C39 C 0.4514(3) 0.3587(3) 0.8854(3) 0.0602(11) Uani 1 1 d . . . H39A H 0.4444 0.3829 0.8392 0.090 Uiso 1 1 calc R . . H39B H 0.5090 0.4078 0.9362 0.090 Uiso 1 1 calc R . . H39C H 0.3762 0.3401 0.9050 0.090 Uiso 1 1 calc R . . C40 C 0.3956(3) 0.1903(3) 0.7357(2) 0.0680(13) Uani 1 1 d . . . H40A H 0.3952 0.2323 0.7050 0.102 Uiso 1 1 calc R . . H40B H 0.3175 0.1640 0.7478 0.102 Uiso 1 1 calc R . . H40C H 0.4198 0.1390 0.6979 0.102 Uiso 1 1 calc R . . C41 C 0.7218(3) 0.2264(3) 1.0916(3) 0.0576(11) Uani 1 1 d . . . H41A H 0.8021 0.2647 1.1202 0.086 Uiso 1 1 calc R . . H41B H 0.7125 0.1595 1.0702 0.086 Uiso 1 1 calc R . . H41C H 0.6695 0.2396 1.1347 0.086 Uiso 1 1 calc R . . C42 C 0.8131(3) 0.2462(3) 0.9420(3) 0.0595(11) Uani 1 1 d . . . H42A H 0.8844 0.2877 0.9843 0.089 Uiso 1 1 calc R . . H42B H 0.8107 0.2652 0.8915 0.089 Uiso 1 1 calc R . . H42C H 0.8113 0.1811 0.9206 0.089 Uiso 1 1 calc R . . C43 C 0.7293(3) 0.3825(2) 1.0513(2) 0.0509(10) Uani 1 1 d . . . H43A H 0.8093 0.4090 1.0823 0.076 Uiso 1 1 calc R . . H43B H 0.6777 0.3986 1.0942 0.076 Uiso 1 1 calc R . . H43C H 0.7236 0.4085 1.0062 0.076 Uiso 1 1 calc R . . C44 C 0.5616(5) -0.0215(3) 0.8775(3) 0.0906(18) Uani 1 1 d . . . H44A H 0.5644 -0.0789 0.8311 0.136 Uiso 1 1 calc R . . H44B H 0.5048 -0.0383 0.9149 0.136 Uiso 1 1 calc R . . H44C H 0.6383 0.0148 0.9143 0.136 Uiso 1 1 calc R . . C45 C 0.3917(4) -0.0409(3) 0.7492(3) 0.109(2) Uani 1 1 d . . . H45A H 0.4124 -0.0936 0.7101 0.164 Uiso 1 1 calc R . . H45B H 0.3611 -0.0136 0.7132 0.164 Uiso 1 1 calc R . . H45C H 0.3325 -0.0635 0.7825 0.164 Uiso 1 1 calc R . . C46 C 0.6219(3) 0.0530(3) 0.7479(2) 0.0561(11) Uani 1 1 d . . . H46A H 0.6179 -0.0110 0.7113 0.084 Uiso 1 1 calc R . . H46B H 0.7007 0.0901 0.7806 0.084 Uiso 1 1 calc R . . H46C H 0.6017 0.0824 0.7095 0.084 Uiso 1 1 calc R . . B3 B 0.4543(3) 0.2427(3) 1.0341(3) 0.0371(10) Uani 1 1 d . . . B4 B 0.3406(4) 0.1221(3) 0.9195(3) 0.0456(11) Uani 1 1 d . B . Co2 Co 0.50811(4) 0.17825(3) 0.92598(3) 0.03738(13) Uani 1 1 d . . . O5 O 0.4306(2) 0.32834(16) 1.06015(14) 0.0420(6) Uani 1 1 d . . . O6 O 0.4532(2) 0.21934(16) 1.11044(15) 0.0432(6) Uani 1 1 d . . . O7 O 0.2514(2) 0.14952(19) 0.89075(16) 0.0536(7) Uani 1 1 d . . . O8 O 0.2849(2) 0.03731(17) 0.93229(16) 0.0534(7) Uani 1 1 d . . . P4 P 0.49696(8) 0.25670(8) 0.84075(6) 0.0469(3) Uani 1 1 d . . . P5 P 0.68665(8) 0.25493(7) 0.99754(6) 0.0405(2) Uani 1 1 d . . . P6 P 0.52007(9) 0.04848(7) 0.82671(7) 0.0522(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0252(19) 0.047(2) 0.033(2) -0.0062(19) 0.0057(16) 0.0007(17) C2 0.042(2) 0.067(3) 0.037(2) 0.002(2) 0.0121(19) -0.006(2) C3 0.039(2) 0.068(3) 0.034(2) -0.022(2) 0.0172(19) -0.006(2) C4 0.052(3) 0.070(3) 0.066(3) 0.003(3) 0.013(2) 0.012(2) C5 0.062(3) 0.050(3) 0.064(3) -0.002(2) 0.010(2) 0.026(2) C6 0.034(2) 0.048(2) 0.044(2) 0.004(2) 0.0082(18) 0.0114(18) C7 0.093(4) 0.097(4) 0.071(3) 0.018(3) 0.026(3) 0.010(3) C8 0.032(2) 0.0301(19) 0.0322(19) 0.0054(16) -0.0018(15) 0.0089(16) C9 0.046(2) 0.034(2) 0.047(2) 0.0132(19) -0.0082(18) 0.0127(18) C10 0.033(2) 0.041(2) 0.045(2) 0.0020(19) -0.0071(17) 0.0173(17) C11 0.0284(19) 0.041(2) 0.0301(19) 0.0025(17) 0.0069(15) 0.0119(16) C12 0.032(2) 0.042(2) 0.0318(19) 0.0148(17) 0.0076(15) 0.0112(16) C13 0.0273(18) 0.0338(19) 0.0243(17) 0.0055(15) 0.0023(14) 0.0119(15) C14 0.038(2) 0.062(3) 0.052(2) 0.013(2) 0.0072(19) 0.013(2) C15 0.113(4) 0.082(4) 0.090(4) 0.018(3) -0.006(3) 0.068(3) C16 0.048(3) 0.080(3) 0.051(3) 0.027(2) -0.009(2) 0.012(2) C17 0.054(3) 0.080(3) 0.106(4) 0.068(3) -0.014(3) 0.001(2) C18 0.074(3) 0.067(3) 0.103(4) 0.055(3) 0.002(3) -0.008(3) C19 0.033(2) 0.069(3) 0.065(3) 0.006(2) 0.013(2) 0.008(2) C20 0.047(3) 0.060(3) 0.055(3) -0.012(2) 0.001(2) -0.003(2) C21 0.064(3) 0.043(2) 0.051(3) -0.004(2) -0.009(2) 0.005(2) C22 0.074(3) 0.073(3) 0.032(2) 0.014(2) 0.002(2) 0.015(2) C23 0.061(3) 0.091(4) 0.046(3) -0.006(2) 0.017(2) 0.024(3) B1 0.026(2) 0.040(2) 0.031(2) 0.0075(19) 0.0037(17) 0.0042(18) B2 0.039(2) 0.031(2) 0.026(2) 0.0074(18) 0.0026(17) 0.0114(18) Co1 0.0281(2) 0.0311(3) 0.0252(2) 0.0060(2) 0.00267(19) 0.0060(2) O1 0.0425(15) 0.0481(16) 0.0296(13) 0.0110(12) 0.0073(11) 0.0078(12) O2 0.0493(16) 0.0447(16) 0.0370(14) 0.0054(13) 0.0069(12) 0.0220(12) O3 0.0333(14) 0.0347(14) 0.0475(15) 0.0188(12) -0.0056(11) 0.0029(11) O4 0.0261(12) 0.0427(14) 0.0356(13) 0.0190(12) 0.0035(10) 0.0086(11) P1 0.0398(6) 0.0466(6) 0.0458(6) 0.0179(5) -0.0027(5) 0.0142(5) P2 0.0322(5) 0.0377(6) 0.0357(5) 0.0054(5) 0.0055(4) 0.0028(4) P3 0.0422(6) 0.0405(6) 0.0305(5) 0.0009(4) 0.0036(4) 0.0090(5) C24 0.032(2) 0.041(2) 0.0293(19) 0.0092(18) 0.0047(15) 0.0071(16) C25 0.045(2) 0.044(2) 0.041(2) 0.0119(19) 0.0097(18) 0.0175(18) C26 0.035(2) 0.048(2) 0.041(2) 0.004(2) 0.0067(17) 0.0083(18) C27 0.048(2) 0.060(3) 0.0254(19) 0.008(2) 0.0076(17) 0.003(2) C28 0.064(3) 0.049(3) 0.030(2) 0.0138(19) 0.0052(19) 0.010(2) C29 0.035(2) 0.039(2) 0.0295(19) 0.0080(17) 0.0039(15) 0.0066(16) C30 0.067(3) 0.074(3) 0.054(3) 0.002(2) 0.015(2) 0.031(3) C31 0.031(2) 0.088(3) 0.029(2) 0.000(2) 0.0046(17) -0.003(2) C32 0.037(3) 0.143(5) 0.042(3) 0.020(3) 0.004(2) 0.014(3) C33A 0.033(3) 0.161(7) 0.044(3) -0.008(4) 0.008(2) -0.008(4) C34A 0.056(4) 0.109(5) 0.053(3) -0.027(3) 0.032(3) -0.037(3) C33B 0.033(3) 0.161(7) 0.044(3) -0.008(4) 0.008(2) -0.008(4) C34B 0.056(4) 0.109(5) 0.053(3) -0.027(3) 0.032(3) -0.037(3) C35 0.055(3) 0.066(3) 0.059(3) -0.010(2) 0.024(2) -0.020(2) C36 0.039(3) 0.061(3) 0.038(2) -0.003(2) 0.0112(19) -0.006(2) C37A 0.041(5) 0.088(7) 0.083(7) 0.023(6) 0.006(5) 0.036(5) C37B 0.049(5) 0.031(4) 0.056(5) 0.010(4) 0.016(4) -0.002(3) C38 0.044(2) 0.087(3) 0.049(2) 0.037(2) 0.013(2) 0.013(2) C39 0.065(3) 0.077(3) 0.055(3) 0.036(2) 0.017(2) 0.033(2) C40 0.048(3) 0.107(4) 0.037(2) 0.018(2) 0.002(2) 0.023(2) C41 0.044(2) 0.064(3) 0.056(3) 0.022(2) -0.009(2) 0.011(2) C42 0.040(2) 0.063(3) 0.052(3) 0.005(2) 0.005(2) 0.009(2) C43 0.044(2) 0.042(2) 0.042(2) 0.0033(19) 0.0014(18) -0.0012(18) C44 0.160(5) 0.046(3) 0.074(3) 0.028(3) 0.052(4) 0.037(3) C45 0.062(3) 0.083(4) 0.081(4) -0.044(3) 0.010(3) -0.019(3) C46 0.064(3) 0.053(3) 0.038(2) 0.004(2) 0.011(2) 0.018(2) B3 0.034(2) 0.042(3) 0.028(2) 0.0092(19) 0.0016(17) 0.0085(19) B4 0.037(2) 0.051(3) 0.030(2) 0.004(2) 0.0050(19) 0.004(2) Co2 0.0302(3) 0.0397(3) 0.0275(2) 0.0038(2) 0.0026(2) 0.0038(2) O5 0.0513(15) 0.0452(15) 0.0305(13) 0.0147(12) 0.0106(11) 0.0179(12) O6 0.0550(16) 0.0411(15) 0.0312(13) 0.0109(12) 0.0050(12) 0.0173(12) O7 0.0313(15) 0.078(2) 0.0413(15) 0.0211(15) 0.0029(12) 0.0087(14) O8 0.0430(16) 0.0489(16) 0.0467(16) 0.0064(13) 0.0098(13) 0.0014(13) P4 0.0358(6) 0.0675(7) 0.0312(5) 0.0165(5) 0.0053(4) 0.0129(5) P5 0.0330(5) 0.0418(6) 0.0324(5) 0.0065(4) 0.0007(4) 0.0039(4) P6 0.0472(6) 0.0422(6) 0.0384(6) -0.0039(5) 0.0105(5) 0.0002(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 C1 C6 1.368(5) . ? C1 C2 1.383(5) . ? C1 O1 1.390(4) . ? C2 C3 1.420(6) . ? C2 H2A 0.9500 . ? C3 C4 1.359(6) . ? C3 C7 1.490(5) . ? C4 C5 1.384(6) . ? C4 H4A 0.9500 . ? C5 C6 1.381(5) . ? C5 H5A 0.9500 . ? C6 O2 1.372(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.360(4) . ? C8 O3 1.376(4) . ? C8 C13 1.391(4) . ? C9 C10 1.393(5) . ? C9 H9A 0.9500 . ? C10 C11 1.383(5) . ? C10 H10A 0.9500 . ? C11 C12 1.393(4) . ? C11 C14 1.509(5) . ? C12 C13 1.366(4) . ? C12 H12A 0.9500 . ? C13 O4 1.377(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 P1 1.834(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 P1 1.830(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 P1 1.827(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 P2 1.813(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 P2 1.823(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 P2 1.828(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 P3 1.831(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 P3 1.831(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 P3 1.838(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? B1 O2 1.430(5) . ? B1 O1 1.440(4) . ? B1 Co1 1.945(4) . ? B2 O3 1.431(4) . ? B2 O4 1.431(4) . ? B2 Co1 1.961(4) . ? Co1 P3 2.2019(10) . ? Co1 P2 2.2034(10) . ? Co1 P1 2.2131(10) . ? C24 C25 1.366(5) . ? C24 O5 1.377(4) . ? C24 C29 1.378(4) . ? C25 C26 1.398(5) . ? C25 H25A 0.9500 . ? C26 C27 1.375(5) . ? C26 C30 1.503(5) . ? C27 C28 1.388(5) . ? C27 H27A 0.9500 . ? C28 C29 1.376(4) . ? C28 H28A 0.9500 . ? C29 O6 1.371(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.375(6) . ? C31 C36 1.379(6) . ? C31 O7 1.388(4) . ? C32 C33A 1.378(7) . ? C32 H32 0.9500 . ? C33A C34A 1.349(8) . ? C33A C37A 1.415(9) . ? C34A C35 1.405(8) . ? C34A H34A 0.9500 . ? C35 C36 1.371(5) . ? C35 H35 0.9500 . ? C36 O8 1.380(4) . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38 P4 1.842(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 P4 1.825(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 P4 1.834(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 P5 1.831(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 P5 1.843(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 P5 1.823(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 P6 1.803(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 P6 1.825(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 P6 1.828(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? B3 O6 1.425(4) . ? B3 O5 1.428(5) . ? B3 Co2 1.958(4) . ? B4 O8 1.424(5) . ? B4 O7 1.432(5) . ? B4 Co2 1.958(4) . ? Co2 P5 2.1977(10) . ? Co2 P6 2.2019(11) . ? Co2 P4 2.2227(11) . ? 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 C6 C1 C2 121.9(4) . . ? C6 C1 O1 110.2(3) . . ? C2 C1 O1 127.9(4) . . ? C1 C2 C3 115.9(4) . . ? C1 C2 H2A 122.0 . . ? C3 C2 H2A 122.0 . . ? C4 C3 C2 121.9(4) . . ? C4 C3 C7 116.8(4) . . ? C2 C3 C7 121.3(5) . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 117.9(4) . . ? C6 C5 H5A 121.0 . . ? C4 C5 H5A 121.0 . . ? C1 C6 O2 109.1(3) . . ? C1 C6 C5 121.5(4) . . ? O2 C6 C5 129.4(4) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 O3 129.7(3) . . ? C9 C8 C13 121.4(3) . . ? O3 C8 C13 108.9(3) . . ? C8 C9 C10 117.1(3) . . ? C8 C9 H9A 121.4 . . ? C10 C9 H9A 121.4 . . ? C11 C10 C9 122.5(3) . . ? C11 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C10 C11 C12 119.0(3) . . ? C10 C11 C14 121.1(3) . . ? C12 C11 C14 119.9(3) . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C12 C13 O4 129.5(3) . . ? C12 C13 C8 121.1(3) . . ? O4 C13 C8 109.4(3) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P1 C17 H17A 109.5 . . ? P1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P2 C19 H19A 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P2 C20 H20A 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P3 C22 H22A 109.5 . . ? P3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P3 C23 H23A 109.5 . . ? P3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 B1 O1 106.4(3) . . ? O2 B1 Co1 126.1(3) . . ? O1 B1 Co1 126.8(3) . . ? O3 B2 O4 106.6(3) . . ? O3 B2 Co1 122.5(2) . . ? O4 B2 Co1 130.0(3) . . ? B1 Co1 B2 68.90(16) . . ? B1 Co1 P3 153.86(12) . . ? B2 Co1 P3 88.63(11) . . ? B1 Co1 P2 91.49(11) . . ? B2 Co1 P2 150.08(12) . . ? P3 Co1 P2 103.03(4) . . ? B1 Co1 P1 95.47(13) . . ? B2 Co1 P1 102.99(11) . . ? P3 Co1 P1 102.73(4) . . ? P2 Co1 P1 101.14(4) . . ? C1 O1 B1 106.2(3) . . ? C6 O2 B1 108.0(3) . . ? C8 O3 B2 107.7(2) . . ? C13 O4 B2 107.3(2) . . ? C17 P1 C16 99.92(19) . . ? C17 P1 C15 100.5(2) . . ? C16 P1 C15 97.6(2) . . ? C17 P1 Co1 118.26(13) . . ? C16 P1 Co1 117.12(14) . . ? C15 P1 Co1 119.51(16) . . ? C18 P2 C19 101.4(2) . . ? C18 P2 C20 100.6(2) . . ? C19 P2 C20 98.82(19) . . ? C18 P2 Co1 111.49(14) . . ? C19 P2 Co1 121.43(14) . . ? C20 P2 Co1 119.76(13) . . ? C21 P3 C22 100.10(19) . . ? C21 P3 C23 99.5(2) . . ? C22 P3 C23 99.9(2) . . ? C21 P3 Co1 117.27(14) . . ? C22 P3 Co1 114.28(14) . . ? C23 P3 Co1 122.15(14) . . ? C25 C24 O5 128.9(3) . . ? C25 C24 C29 122.1(3) . . ? O5 C24 C29 109.0(3) . . ? C24 C25 C26 118.2(3) . . ? C24 C25 H25A 120.9 . . ? C26 C25 H25A 120.9 . . ? C27 C26 C25 119.0(4) . . ? C27 C26 C30 120.5(3) . . ? C25 C26 C30 120.5(4) . . ? C26 C27 C28 122.9(3) . . ? C26 C27 H27A 118.6 . . ? C28 C27 H27A 118.6 . . ? C29 C28 C27 117.1(4) . . ? C29 C28 H28A 121.5 . . ? C27 C28 H28A 121.5 . . ? O6 C29 C28 129.7(3) . . ? O6 C29 C24 109.5(3) . . ? C28 C29 C24 120.7(3) . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 121.8(4) . . ? C32 C31 O7 128.4(5) . . ? C36 C31 O7 109.8(4) . . ? C31 C32 C33A 117.3(6) . . ? C31 C32 H32 121.4 . . ? C33A C32 H32 121.4 . . ? C34A C33A C32 121.5(6) . . ? C34A C33A C37A 102.6(7) . . ? C32 C33A C37A 135.8(8) . . ? C33A C34A C35 121.7(5) . . ? C33A C34A H34A 119.2 . . ? C35 C34A H34A 119.2 . . ? C36 C35 C34A 116.9(5) . . ? C36 C35 H35 121.6 . . ? C34A C35 H35 121.6 . . ? C35 C36 C31 120.9(4) . . ? C35 C36 O8 130.1(5) . . ? C31 C36 O8 109.1(3) . . ? H37D C37B H37E 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? P4 C38 H38A 109.5 . . ? P4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P4 C39 H39A 109.5 . . ? P4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P4 C40 H40A 109.5 . . ? P4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P5 C41 H41A 109.5 . . ? P5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P5 C42 H42A 109.5 . . ? P5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P5 C43 H43A 109.5 . . ? P5 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? P5 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P6 C44 H44A 109.5 . . ? P6 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? P6 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? P6 C45 H45A 109.5 . . ? P6 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? P6 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? P6 C46 H46A 109.5 . . ? P6 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? P6 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O6 B3 O5 106.4(3) . . ? O6 B3 Co2 123.4(3) . . ? O5 B3 Co2 129.3(3) . . ? O8 B4 O7 107.2(3) . . ? O8 B4 Co2 124.7(3) . . ? O7 B4 Co2 127.6(3) . . ? B3 Co2 B4 67.95(17) . . ? B3 Co2 P5 88.34(12) . . ? B4 Co2 P5 153.40(12) . . ? B3 Co2 P6 150.43(12) . . ? B4 Co2 P6 93.23(13) . . ? P5 Co2 P6 102.99(4) . . ? B3 Co2 P4 103.63(12) . . ? B4 Co2 P4 95.85(14) . . ? P5 Co2 P4 101.55(4) . . ? P6 Co2 P4 100.73(4) . . ? C24 O5 B3 107.5(3) . . ? C29 O6 B3 107.5(3) . . ? C31 O7 B4 106.4(3) . . ? C36 O8 B4 107.4(3) . . ? C39 P4 C40 100.0(2) . . ? C39 P4 C38 100.82(19) . . ? C40 P4 C38 98.53(18) . . ? C39 P4 Co2 118.54(12) . . ? C40 P4 Co2 116.51(15) . . ? C38 P4 Co2 118.84(13) . . ? C43 P5 C41 100.75(18) . . ? C43 P5 C42 99.75(17) . . ? C41 P5 C42 99.24(18) . . ? C43 P5 Co2 116.49(13) . . ? C41 P5 Co2 115.10(13) . . ? C42 P5 Co2 121.98(13) . . ? C44 P6 C45 99.9(3) . . ? C44 P6 C46 101.0(2) . . ? C45 P6 C46 98.7(2) . . ? C44 P6 Co2 112.26(15) . . ? C45 P6 Co2 120.29(17) . . ? C46 P6 Co2 121.08(13) . . ? 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 C6 C1 C2 C3 -1.0(5) . . . . ? O1 C1 C2 C3 178.2(3) . . . . ? C1 C2 C3 C4 1.6(6) . . . . ? C1 C2 C3 C7 -176.7(4) . . . . ? C2 C3 C4 C5 -1.3(6) . . . . ? C7 C3 C4 C5 177.1(4) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C2 C1 C6 O2 178.7(3) . . . . ? O1 C1 C6 O2 -0.7(4) . . . . ? C2 C1 C6 C5 0.3(6) . . . . ? O1 C1 C6 C5 -179.1(3) . . . . ? C4 C5 C6 C1 0.0(6) . . . . ? C4 C5 C6 O2 -178.0(4) . . . . ? O3 C8 C9 C10 -179.1(3) . . . . ? C13 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C9 C10 C11 C14 178.4(3) . . . . ? C10 C11 C12 C13 0.7(5) . . . . ? C14 C11 C12 C13 -178.3(3) . . . . ? C11 C12 C13 O4 179.0(3) . . . . ? C11 C12 C13 C8 -0.2(5) . . . . ? C9 C8 C13 C12 -0.4(5) . . . . ? O3 C8 C13 C12 179.3(3) . . . . ? C9 C8 C13 O4 -179.8(3) . . . . ? O3 C8 C13 O4 -0.1(3) . . . . ? O2 B1 Co1 B2 93.8(3) . . . . ? O1 B1 Co1 B2 -96.5(3) . . . . ? O2 B1 Co1 P3 61.4(4) . . . . ? O1 B1 Co1 P3 -129.0(3) . . . . ? O2 B1 Co1 P2 -63.0(3) . . . . ? O1 B1 Co1 P2 106.6(3) . . . . ? O2 B1 Co1 P1 -164.4(3) . . . . ? O1 B1 Co1 P1 5.3(3) . . . . ? O3 B2 Co1 B1 -93.5(3) . . . . ? O4 B2 Co1 B1 99.0(3) . . . . ? O3 B2 Co1 P3 72.8(3) . . . . ? O4 B2 Co1 P3 -94.7(3) . . . . ? O3 B2 Co1 P2 -41.4(4) . . . . ? O4 B2 Co1 P2 151.0(2) . . . . ? O3 B2 Co1 P1 175.6(3) . . . . ? O4 B2 Co1 P1 8.0(3) . . . . ? C6 C1 O1 B1 -0.2(4) . . . . ? C2 C1 O1 B1 -179.5(3) . . . . ? O2 B1 O1 C1 1.0(3) . . . . ? Co1 B1 O1 C1 -170.3(3) . . . . ? C1 C6 O2 B1 1.3(4) . . . . ? C5 C6 O2 B1 179.5(4) . . . . ? O1 B1 O2 C6 -1.4(3) . . . . ? Co1 B1 O2 C6 170.0(3) . . . . ? C9 C8 O3 B2 177.9(4) . . . . ? C13 C8 O3 B2 -1.7(3) . . . . ? O4 B2 O3 C8 2.8(3) . . . . ? Co1 B2 O3 C8 -167.2(2) . . . . ? C12 C13 O4 B2 -177.4(3) . . . . ? C8 C13 O4 B2 1.9(3) . . . . ? O3 B2 O4 C13 -2.9(3) . . . . ? Co1 B2 O4 C13 166.1(3) . . . . ? B1 Co1 P1 C17 -63.0(2) . . . . ? B2 Co1 P1 C17 6.6(2) . . . . ? P3 Co1 P1 C17 98.15(19) . . . . ? P2 Co1 P1 C17 -155.59(19) . . . . ? B1 Co1 P1 C16 56.70(19) . . . . ? B2 Co1 P1 C16 126.27(19) . . . . ? P3 Co1 P1 C16 -142.18(16) . . . . ? P2 Co1 P1 C16 -35.91(16) . . . . ? B1 Co1 P1 C15 174.2(2) . . . . ? B2 Co1 P1 C15 -116.3(2) . . . . ? P3 Co1 P1 C15 -24.7(2) . . . . ? P2 Co1 P1 C15 81.6(2) . . . . ? B1 Co1 P2 C18 94.4(2) . . . . ? B2 Co1 P2 C18 47.0(3) . . . . ? P3 Co1 P2 C18 -63.65(19) . . . . ? P1 Co1 P2 C18 -169.68(18) . . . . ? B1 Co1 P2 C19 -146.2(2) . . . . ? B2 Co1 P2 C19 166.3(3) . . . . ? P3 Co1 P2 C19 55.66(17) . . . . ? P1 Co1 P2 C19 -50.37(17) . . . . ? B1 Co1 P2 C20 -22.4(2) . . . . ? B2 Co1 P2 C20 -69.8(3) . . . . ? P3 Co1 P2 C20 179.48(18) . . . . ? P1 Co1 P2 C20 73.45(18) . . . . ? B1 Co1 P3 C21 80.4(3) . . . . ? B2 Co1 P3 C21 50.43(19) . . . . ? P2 Co1 P3 C21 -157.39(16) . . . . ? P1 Co1 P3 C21 -52.58(16) . . . . ? B1 Co1 P3 C22 -36.2(3) . . . . ? B2 Co1 P3 C22 -66.24(19) . . . . ? P2 Co1 P3 C22 85.94(16) . . . . ? P1 Co1 P3 C22 -169.25(15) . . . . ? B1 Co1 P3 C23 -156.7(3) . . . . ? B2 Co1 P3 C23 173.3(2) . . . . ? P2 Co1 P3 C23 -34.54(19) . . . . ? P1 Co1 P3 C23 70.27(19) . . . . ? O5 C24 C25 C26 -179.1(3) . . . . ? C29 C24 C25 C26 -0.3(5) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C24 C25 C26 C30 179.6(3) . . . . ? C25 C26 C27 C28 0.0(5) . . . . ? C30 C26 C27 C28 -179.9(4) . . . . ? C26 C27 C28 C29 0.9(6) . . . . ? C27 C28 C29 O6 179.5(3) . . . . ? C27 C28 C29 C24 -1.5(5) . . . . ? C25 C24 C29 O6 -179.6(3) . . . . ? O5 C24 C29 O6 -0.6(4) . . . . ? C25 C24 C29 C28 1.2(5) . . . . ? O5 C24 C29 C28 -179.8(3) . . . . ? C36 C31 C32 C33A -0.5(6) . . . . ? O7 C31 C32 C33A -179.6(4) . . . . ? C31 C32 C33A C34A 0.0(8) . . . . ? C31 C32 C33A C37A -177.4(7) . . . . ? C32 C33A C34A C35 -0.1(9) . . . . ? C37A C33A C34A C35 178.1(5) . . . . ? C33A C34A C35 C36 0.7(8) . . . . ? C34A C35 C36 C31 -1.2(6) . . . . ? C34A C35 C36 O8 178.6(4) . . . . ? C32 C31 C36 C35 1.2(6) . . . . ? O7 C31 C36 C35 -179.6(3) . . . . ? C32 C31 C36 O8 -178.6(3) . . . . ? O7 C31 C36 O8 0.6(4) . . . . ? O6 B3 Co2 B4 92.9(3) . . . . ? O5 B3 Co2 B4 -99.8(4) . . . . ? O6 B3 Co2 P5 -74.7(3) . . . . ? O5 B3 Co2 P5 92.5(3) . . . . ? O6 B3 Co2 P6 39.1(5) . . . . ? O5 B3 Co2 P6 -153.6(2) . . . . ? O6 B3 Co2 P4 -176.2(3) . . . . ? O5 B3 Co2 P4 -8.9(3) . . . . ? O8 B4 Co2 B3 -102.0(3) . . . . ? O7 B4 Co2 B3 86.7(4) . . . . ? O8 B4 Co2 P5 -73.5(5) . . . . ? O7 B4 Co2 P5 115.2(3) . . . . ? O8 B4 Co2 P6 54.5(3) . . . . ? O7 B4 Co2 P6 -116.8(3) . . . . ? O8 B4 Co2 P4 155.6(3) . . . . ? O7 B4 Co2 P4 -15.7(3) . . . . ? C25 C24 O5 B3 177.8(3) . . . . ? C29 C24 O5 B3 -1.1(4) . . . . ? O6 B3 O5 C24 2.2(4) . . . . ? Co2 B3 O5 C24 -166.7(3) . . . . ? C28 C29 O6 B3 -178.9(4) . . . . ? C24 C29 O6 B3 2.0(4) . . . . ? O5 B3 O6 C29 -2.6(4) . . . . ? Co2 B3 O6 C29 167.2(3) . . . . ? C32 C31 O7 B4 -179.6(4) . . . . ? C36 C31 O7 B4 1.2(4) . . . . ? O8 B4 O7 C31 -2.5(4) . . . . ? Co2 B4 O7 C31 170.1(3) . . . . ? C35 C36 O8 B4 178.1(4) . . . . ? C31 C36 O8 B4 -2.1(4) . . . . ? O7 B4 O8 C36 2.8(4) . . . . ? Co2 B4 O8 C36 -170.0(3) . . . . ? B3 Co2 P4 C39 2.6(2) . . . . ? B4 Co2 P4 C39 71.3(2) . . . . ? P5 Co2 P4 C39 -88.45(16) . . . . ? P6 Co2 P4 C39 165.75(16) . . . . ? B3 Co2 P4 C40 -116.81(19) . . . . ? B4 Co2 P4 C40 -48.1(2) . . . . ? P5 Co2 P4 C40 152.10(15) . . . . ? P6 Co2 P4 C40 46.30(15) . . . . ? B3 Co2 P4 C38 125.6(2) . . . . ? B4 Co2 P4 C38 -165.8(2) . . . . ? P5 Co2 P4 C38 34.47(17) . . . . ? P6 Co2 P4 C38 -71.34(16) . . . . ? B3 Co2 P5 C43 -52.79(18) . . . . ? B4 Co2 P5 C43 -79.0(4) . . . . ? P6 Co2 P5 C43 154.80(14) . . . . ? P4 Co2 P5 C43 50.78(14) . . . . ? B3 Co2 P5 C41 64.8(2) . . . . ? B4 Co2 P5 C41 38.6(4) . . . . ? P6 Co2 P5 C41 -87.58(16) . . . . ? P4 Co2 P5 C41 168.40(15) . . . . ? B3 Co2 P5 C42 -175.1(2) . . . . ? B4 Co2 P5 C42 158.7(4) . . . . ? P6 Co2 P5 C42 32.52(17) . . . . ? P4 Co2 P5 C42 -71.50(16) . . . . ? B3 Co2 P6 C44 -47.4(3) . . . . ? B4 Co2 P6 C44 -95.9(2) . . . . ? P5 Co2 P6 C44 62.86(18) . . . . ? P4 Co2 P6 C44 167.51(18) . . . . ? B3 Co2 P6 C45 69.6(3) . . . . ? B4 Co2 P6 C45 21.0(3) . . . . ? P5 Co2 P6 C45 179.8(2) . . . . ? P4 Co2 P6 C45 -75.5(2) . . . . ? B3 Co2 P6 C46 -166.6(3) . . . . ? B4 Co2 P6 C46 144.9(2) . . . . ? P5 Co2 P6 C46 -56.36(16) . . . . ? P4 Co2 P6 C46 48.29(16) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.888 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.065 data_3 _database_code_depnum_ccdc_archive 'CCDC 290419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cobalt tris-dimethylphenylphosphine-bisboryl ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H41 B2 Co O4 P3' _chemical_formula_sum 'C36 H41 B2 Co O4 P3' _chemical_formula_weight 711.15 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.2266(6) _cell_length_b 16.0716(7) _cell_length_c 33.7307(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.30(1) _cell_angle_gamma 90.00 _cell_volume 7126.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5561 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.32 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f angles and each scan (35 sec exposure) covering 0.3\% in \w. Crystal to detector distance 5.93 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '60W microfocus Bede Microsource with glass polycapillary optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ProteumM APEX CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 33424 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7749 _reflns_number_gt 6062 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.28A (Bruker, 2002)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. Methyl groups were refined as rigid (rotating) bodies with a common refined U for three H atoms, other H atoms were treated as riding. ; _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^)+(0.0406P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7749 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.54565(2) 0.30086(2) 0.116396(9) 0.01342(9) Uani 1 1 d . . . P1 P 0.58292(5) 0.36877(4) 0.173571(18) 0.01537(15) Uani 1 1 d . . . P2 P 0.52514(5) 0.39052(4) 0.064868(19) 0.01706(15) Uani 1 1 d . . . P3 P 0.69709(5) 0.24891(4) 0.109381(19) 0.01577(15) Uani 1 1 d . . . O1 O 0.42948(13) 0.21223(10) 0.04605(5) 0.0219(4) Uani 1 1 d . . . O2 O 0.47441(13) 0.12541(10) 0.09902(5) 0.0205(4) Uani 1 1 d . . . O3 O 0.32465(13) 0.35294(10) 0.11513(5) 0.0225(4) Uani 1 1 d . . . O4 O 0.36817(12) 0.24848(10) 0.16011(5) 0.0207(4) Uani 1 1 d . . . C1 C 0.70266(18) 0.42596(15) 0.18590(7) 0.0171(5) Uani 1 1 d . . . C2 C 0.77748(19) 0.40016(17) 0.21571(8) 0.0242(6) Uani 1 1 d . . . H2 H 0.7664 0.3522 0.2311 0.029 Uiso 1 1 d R . . C3 C 0.8678(2) 0.44383(19) 0.22299(9) 0.0331(7) Uani 1 1 d . . . H3 H 0.9180 0.4258 0.2435 0.040 Uiso 1 1 d R . . C4 C 0.8857(2) 0.51340(19) 0.20080(9) 0.0329(7) Uani 1 1 d . . . H4 H 0.9483 0.5426 0.2056 0.040 Uiso 1 1 d R . . C5 C 0.8117(2) 0.54024(17) 0.17149(8) 0.0284(7) Uani 1 1 d . . . H5 H 0.8231 0.5883 0.1562 0.034 Uiso 1 1 d R . . C6 C 0.7210(2) 0.49708(16) 0.16448(8) 0.0243(6) Uani 1 1 d . . . H6 H 0.6702 0.5166 0.1445 0.029 Uiso 1 1 d R . . C7 C 0.49331(19) 0.44583(16) 0.18944(8) 0.0220(6) Uani 1 1 d . . . H71 H 0.5168 0.4648 0.2165 0.023(4) Uiso 1 1 d R . . H72 H 0.4258 0.4205 0.1892 0.023(4) Uiso 1 1 d R . . H73 H 0.4894 0.4933 0.1711 0.023(4) Uiso 1 1 d R . . C8 C 0.58696(19) 0.29308(16) 0.21428(7) 0.0199(6) Uani 1 1 d . . . H81 H 0.6429 0.2539 0.2122 0.026(4) Uiso 1 1 d R . . H82 H 0.5225 0.2626 0.2125 0.026(4) Uiso 1 1 d R . . H83 H 0.5977 0.3222 0.2399 0.026(4) Uiso 1 1 d R . . C11 C 0.55416(18) 0.50065(15) 0.07439(7) 0.0162(5) Uani 1 1 d . . . C12 C 0.64159(19) 0.53959(16) 0.06437(7) 0.0204(6) Uani 1 1 d . . . H12 H 0.6892 0.5090 0.0510 0.025 Uiso 1 1 d R . . C13 C 0.6603(2) 0.62300(16) 0.07371(8) 0.0257(6) Uani 1 1 d . . . H13 H 0.7201 0.6490 0.0664 0.031 Uiso 1 1 d R . . C14 C 0.5924(2) 0.66835(17) 0.09354(8) 0.0275(6) Uani 1 1 d . . . H14 H 0.6053 0.7252 0.1000 0.033 Uiso 1 1 d R . . C15 C 0.5056(2) 0.62981(17) 0.10383(8) 0.0266(6) Uani 1 1 d . . . H15 H 0.4589 0.6605 0.1176 0.032 Uiso 1 1 d R . . C16 C 0.48586(19) 0.54746(16) 0.09447(8) 0.0223(6) Uani 1 1 d . . . H16 H 0.4255 0.5222 0.1016 0.027 Uiso 1 1 d R . . C17 C 0.3975(2) 0.40282(17) 0.03804(8) 0.0275(7) Uani 1 1 d . . . H171 H 0.3518 0.4265 0.0560 0.031(4) Uiso 1 1 d R . . H172 H 0.3717 0.3484 0.0285 0.031(4) Uiso 1 1 d R . . H173 H 0.4009 0.4402 0.0153 0.031(4) Uiso 1 1 d R . . C18 C 0.5929(2) 0.36784(16) 0.02142(7) 0.0270(6) Uani 1 1 d . . . H181 H 0.5765 0.4104 0.0009 0.034(5) Uiso 1 1 d R . . H182 H 0.5721 0.3131 0.0106 0.034(5) Uiso 1 1 d R . . H183 H 0.6664 0.3678 0.0295 0.034(5) Uiso 1 1 d R . . C21 C 0.74386(18) 0.18324(15) 0.15212(7) 0.0178(5) Uani 1 1 d . . . C22 C 0.83028(19) 0.20206(17) 0.17816(8) 0.0242(6) Uani 1 1 d . . . H22 H 0.8708 0.2488 0.1730 0.029 Uiso 1 1 d R . . C23 C 0.8576(2) 0.15324(18) 0.21158(8) 0.0293(7) Uani 1 1 d . . . H23 H 0.9168 0.1670 0.2289 0.035 Uiso 1 1 d R . . C24 C 0.8002(2) 0.08510(18) 0.22002(8) 0.0305(7) Uani 1 1 d . . . H24 H 0.8186 0.0525 0.2432 0.037 Uiso 1 1 d R . . C25 C 0.7149(2) 0.06529(17) 0.19396(8) 0.0311(7) Uani 1 1 d . . . H25 H 0.6752 0.0180 0.1991 0.037 Uiso 1 1 d R . . C26 C 0.6871(2) 0.11366(16) 0.16069(8) 0.0276(6) Uani 1 1 d . . . H26 H 0.6283 0.0993 0.1433 0.033 Uiso 1 1 d R . . C27 C 0.80335(18) 0.32027(15) 0.10542(8) 0.0216(6) Uani 1 1 d . . . H271 H 0.8656 0.2882 0.1034 0.028(4) Uiso 1 1 d R . . H272 H 0.8125 0.3559 0.1291 0.028(4) Uiso 1 1 d R . . H273 H 0.7889 0.3549 0.0816 0.028(4) Uiso 1 1 d R . . C28 C 0.7115(2) 0.17764(16) 0.06776(8) 0.0239(6) Uani 1 1 d . . . H281 H 0.6943 0.2069 0.0424 0.036(5) Uiso 1 1 d R . . H282 H 0.6660 0.1299 0.0692 0.036(5) Uiso 1 1 d R . . H283 H 0.7821 0.1581 0.0694 0.036(5) Uiso 1 1 d R . . C31 C 0.40905(19) 0.13093(16) 0.03454(8) 0.0213(6) Uani 1 1 d . . . C32 C 0.43588(18) 0.07882(16) 0.06618(8) 0.0198(6) Uani 1 1 d . . . C33 C 0.42573(19) -0.00621(16) 0.06300(9) 0.0248(6) Uani 1 1 d . . . H33 H 0.4450 -0.0422 0.0849 0.030 Uiso 1 1 d R . . C34 C 0.3853(2) -0.03645(17) 0.02571(9) 0.0294(7) Uani 1 1 d . . . H34 H 0.3773 -0.0948 0.0220 0.035 Uiso 1 1 d R . . C35 C 0.3567(2) 0.01627(18) -0.00593(9) 0.0297(7) Uani 1 1 d . . . H35 H 0.3288 -0.0065 -0.0308 0.036 Uiso 1 1 d R . . C36 C 0.3680(2) 0.10203(18) -0.00210(8) 0.0285(7) Uani 1 1 d . . . H36 H 0.3484 0.1387 -0.0237 0.034 Uiso 1 1 d R . . C41 C 0.24624(19) 0.33997(16) 0.13801(8) 0.0217(6) Uani 1 1 d . . . C42 C 0.27185(19) 0.27703(16) 0.16493(8) 0.0211(6) Uani 1 1 d . . . C43 C 0.2068(2) 0.25072(18) 0.19140(8) 0.0286(7) Uani 1 1 d . . . H43 H 0.2246 0.2073 0.2100 0.034 Uiso 1 1 d R . . C44 C 0.1128(2) 0.2914(2) 0.18948(9) 0.0346(7) Uani 1 1 d . . . H44 H 0.0654 0.2752 0.2072 0.041 Uiso 1 1 d R . . C45 C 0.0875(2) 0.35446(19) 0.16246(9) 0.0346(7) Uani 1 1 d . . . H45 H 0.0231 0.3807 0.1621 0.041 Uiso 1 1 d R . . C46 C 0.1539(2) 0.38043(17) 0.13588(9) 0.0305(7) Uani 1 1 d . . . H46 H 0.1367 0.4238 0.1172 0.037 Uiso 1 1 d R . . B1 B 0.4748(2) 0.21050(18) 0.08651(9) 0.0187(6) Uani 1 1 d . . . B2 B 0.4050(2) 0.29745(18) 0.12911(8) 0.0183(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.01421(17) 0.01379(17) 0.01193(17) -0.00036(14) -0.00004(13) -0.00149(14) P1 0.0158(3) 0.0180(3) 0.0122(3) -0.0010(3) 0.0008(3) -0.0004(3) P2 0.0213(4) 0.0162(3) 0.0130(3) 0.0002(3) -0.0009(3) -0.0011(3) P3 0.0166(3) 0.0143(3) 0.0164(3) -0.0013(3) 0.0018(3) -0.0009(3) O1 0.0288(10) 0.0166(10) 0.0192(10) -0.0038(7) -0.0027(8) -0.0029(8) O2 0.0216(10) 0.0192(10) 0.0197(10) -0.0018(7) -0.0022(8) -0.0063(8) O3 0.0187(9) 0.0218(10) 0.0272(11) 0.0016(8) 0.0027(8) 0.0004(8) O4 0.0170(9) 0.0225(10) 0.0228(10) -0.0003(8) 0.0022(8) -0.0024(8) C1 0.0200(13) 0.0190(13) 0.0124(13) -0.0082(10) 0.0027(10) -0.0028(11) C2 0.0222(14) 0.0250(15) 0.0249(15) 0.0033(12) 0.0003(12) 0.0005(12) C3 0.0201(15) 0.0409(19) 0.0360(18) 0.0027(14) -0.0070(13) 0.0020(13) C4 0.0187(15) 0.0384(18) 0.0411(19) -0.0084(15) 0.0009(13) -0.0088(13) C5 0.0333(16) 0.0248(15) 0.0280(16) -0.0026(12) 0.0066(13) -0.0071(13) C6 0.0261(15) 0.0260(15) 0.0196(14) -0.0002(11) -0.0026(11) -0.0055(12) C7 0.0213(14) 0.0262(15) 0.0190(14) -0.0052(11) 0.0043(11) 0.0041(11) C8 0.0209(13) 0.0258(14) 0.0127(13) 0.0008(11) 0.0006(10) -0.0018(11) C11 0.0215(14) 0.0146(13) 0.0114(12) 0.0039(10) -0.0033(10) -0.0004(10) C12 0.0210(14) 0.0228(14) 0.0176(14) 0.0010(11) 0.0020(11) 0.0017(11) C13 0.0242(15) 0.0250(15) 0.0273(16) 0.0031(12) -0.0003(12) -0.0068(12) C14 0.0328(16) 0.0187(14) 0.0293(16) -0.0033(12) -0.0049(13) -0.0014(12) C15 0.0261(15) 0.0274(16) 0.0258(16) -0.0064(12) 0.0002(12) 0.0076(12) C16 0.0185(14) 0.0265(15) 0.0217(14) 0.0003(12) 0.0012(11) 0.0003(11) C17 0.0328(16) 0.0243(16) 0.0226(15) 0.0055(12) -0.0096(12) -0.0021(12) C18 0.0422(18) 0.0227(15) 0.0166(14) 0.0016(11) 0.0063(13) 0.0000(13) C21 0.0180(13) 0.0169(13) 0.0188(14) -0.0029(10) 0.0031(10) 0.0031(10) C22 0.0205(14) 0.0259(15) 0.0261(15) -0.0022(12) 0.0018(11) 0.0001(12) C23 0.0215(15) 0.0389(18) 0.0257(16) -0.0016(13) -0.0050(12) 0.0034(13) C24 0.0368(17) 0.0296(16) 0.0242(16) 0.0045(12) -0.0017(13) 0.0107(14) C25 0.0401(18) 0.0211(15) 0.0311(17) 0.0043(12) -0.0005(14) -0.0039(13) C26 0.0308(16) 0.0208(15) 0.0289(16) 0.0018(12) -0.0065(13) -0.0045(12) C27 0.0169(13) 0.0213(14) 0.0270(15) 0.0008(11) 0.0047(11) -0.0021(11) C28 0.0278(15) 0.0207(14) 0.0239(15) -0.0061(11) 0.0054(12) 0.0016(11) C31 0.0182(14) 0.0211(14) 0.0245(15) -0.0074(11) 0.0019(11) -0.0026(11) C32 0.0130(13) 0.0212(14) 0.0254(15) -0.0057(11) 0.0025(11) -0.0038(11) C33 0.0200(14) 0.0192(14) 0.0359(17) -0.0027(12) 0.0056(12) -0.0030(11) C34 0.0205(15) 0.0228(15) 0.0466(19) -0.0191(14) 0.0116(14) -0.0094(12) C35 0.0237(15) 0.0366(17) 0.0291(16) -0.0190(14) 0.0039(12) -0.0060(13) C36 0.0255(15) 0.0341(17) 0.0254(16) -0.0089(13) 0.0007(12) -0.0031(13) C41 0.0171(13) 0.0230(15) 0.0248(15) -0.0078(12) 0.0015(11) -0.0073(11) C42 0.0168(13) 0.0233(14) 0.0231(14) -0.0095(11) 0.0010(11) -0.0048(11) C43 0.0255(15) 0.0366(17) 0.0243(15) -0.0050(13) 0.0050(12) -0.0090(13) C44 0.0225(16) 0.049(2) 0.0339(17) -0.0181(15) 0.0112(13) -0.0136(14) C45 0.0186(15) 0.0377(18) 0.048(2) -0.0193(15) 0.0045(14) -0.0018(13) C46 0.0227(15) 0.0265(16) 0.0415(19) -0.0075(13) 0.0003(13) 0.0001(12) B1 0.0152(14) 0.0209(16) 0.0201(16) -0.0017(12) 0.0021(12) -0.0023(12) B2 0.0183(15) 0.0190(15) 0.0170(15) -0.0044(12) -0.0008(12) -0.0023(12) _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 Co B1 1.948(3) . ? Co B2 1.955(3) . ? Co P3 2.2067(7) . ? Co P1 2.2237(7) . ? Co P2 2.2510(7) . ? P1 C8 1.831(2) . ? P1 C7 1.834(2) . ? P1 C1 1.839(2) . ? P2 C11 1.832(2) . ? P2 C18 1.836(3) . ? P2 C17 1.837(3) . ? P3 C27 1.830(2) . ? P3 C28 1.838(2) . ? P3 C21 1.838(3) . ? O1 C31 1.381(3) . ? O1 B1 1.429(3) . ? O2 C32 1.387(3) . ? O2 B1 1.431(3) . ? O3 C41 1.375(3) . ? O3 B2 1.427(3) . ? O4 C42 1.380(3) . ? O4 B2 1.436(3) . ? C1 C6 1.388(3) . ? C1 C2 1.394(3) . ? C2 C3 1.384(4) . ? C3 C4 1.380(4) . ? C4 C5 1.381(4) . ? C5 C6 1.383(4) . ? C11 C12 1.389(3) . ? C11 C16 1.405(3) . ? C12 C13 1.393(3) . ? C13 C14 1.385(4) . ? C14 C15 1.382(4) . ? C15 C16 1.379(4) . ? C21 C26 1.395(3) . ? C21 C22 1.396(3) . ? C22 C23 1.388(4) . ? C23 C24 1.380(4) . ? C24 C25 1.389(4) . ? C25 C26 1.381(4) . ? C31 C32 1.372(4) . ? C31 C36 1.375(4) . ? C32 C33 1.376(3) . ? C33 C34 1.399(4) . ? C34 C35 1.382(4) . ? C35 C36 1.391(4) . ? C41 C42 1.377(4) . ? C41 C46 1.378(4) . ? C42 C43 1.373(3) . ? C43 C44 1.400(4) . ? C44 C45 1.379(4) . ? C45 C46 1.386(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 B1 Co B2 71.19(12) . . ? B1 Co P3 93.04(9) . . ? B2 Co P3 155.46(9) . . ? B1 Co P1 149.64(9) . . ? B2 Co P1 87.09(8) . . ? P3 Co P1 99.28(3) . . ? B1 Co P2 93.86(9) . . ? B2 Co P2 98.65(9) . . ? P3 Co P2 101.14(3) . . ? P1 Co P2 110.61(3) . . ? C8 P1 C7 101.32(12) . . ? C8 P1 C1 102.07(11) . . ? C7 P1 C1 99.47(12) . . ? C8 P1 Co 108.04(8) . . ? C7 P1 Co 119.72(9) . . ? C1 P1 Co 123.01(8) . . ? C11 P2 C18 102.74(12) . . ? C11 P2 C17 98.39(12) . . ? C18 P2 C17 97.52(13) . . ? C11 P2 Co 118.55(8) . . ? C18 P2 Co 117.46(9) . . ? C17 P2 Co 118.41(9) . . ? C27 P3 C28 100.93(12) . . ? C27 P3 C21 102.83(12) . . ? C28 P3 C21 100.78(12) . . ? C27 P3 Co 118.96(9) . . ? C28 P3 Co 119.30(9) . . ? C21 P3 Co 111.37(8) . . ? C31 O1 B1 107.4(2) . . ? C32 O2 B1 107.05(19) . . ? C41 O3 B2 107.4(2) . . ? C42 O4 B2 107.1(2) . . ? C6 C1 C2 118.0(2) . . ? C6 C1 P1 119.32(19) . . ? C2 C1 P1 122.67(19) . . ? C3 C2 C1 120.5(3) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 119.4(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C1 121.5(3) . . ? C12 C11 C16 118.2(2) . . ? C12 C11 P2 123.83(19) . . ? C16 C11 P2 117.93(18) . . ? C11 C12 C13 120.7(2) . . ? C14 C13 C12 120.5(2) . . ? C15 C14 C13 119.1(3) . . ? C16 C15 C14 121.0(2) . . ? C15 C16 C11 120.6(2) . . ? C26 C21 C22 117.7(2) . . ? C26 C21 P3 118.73(19) . . ? C22 C21 P3 123.42(19) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 121.1(3) . . ? C23 C24 C25 118.6(3) . . ? C26 C25 C24 120.7(3) . . ? C25 C26 C21 121.3(3) . . ? C32 C31 C36 122.4(2) . . ? C32 C31 O1 109.4(2) . . ? C36 C31 O1 128.2(2) . . ? C31 C32 C33 122.0(2) . . ? C31 C32 O2 109.4(2) . . ? C33 C32 O2 128.5(2) . . ? C32 C33 C34 116.1(3) . . ? C35 C34 C33 121.8(3) . . ? C34 C35 C36 121.2(3) . . ? C31 C36 C35 116.5(3) . . ? O3 C41 C42 109.6(2) . . ? O3 C41 C46 128.2(3) . . ? C42 C41 C46 122.2(3) . . ? C43 C42 C41 121.9(2) . . ? C43 C42 O4 128.8(3) . . ? C41 C42 O4 109.3(2) . . ? C42 C43 C44 116.3(3) . . ? C45 C44 C43 121.6(3) . . ? C44 C45 C46 121.6(3) . . ? C41 C46 C45 116.4(3) . . ? O1 B1 O2 106.6(2) . . ? O1 B1 Co 127.4(2) . . ? O2 B1 Co 125.23(19) . . ? O3 B2 O4 106.5(2) . . ? O3 B2 Co 127.00(19) . . ? O4 B2 Co 125.59(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.569 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.078 data_4 _database_code_depnum_ccdc_archive 'CCDC 290420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H40 B Co O2 P4' _chemical_formula_sum 'C18 H40 B Co O2 P4' _chemical_formula_weight 482.12 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6032(12) _cell_length_b 9.7012(7) _cell_length_c 16.1590(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.3940(10) _cell_angle_gamma 90.00 _cell_volume 2521.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 153 _cell_measurement_theta_min 2.452 _cell_measurement_theta_max 27.518 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.730238 _exptl_absorpt_correction_T_max 0.910000 _exptl_absorpt_process_details 'SADABS V2.1 (Bruker AXS, 2001)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15951 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5793 _reflns_number_gt 4639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _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^)+(0.0336P)^2^+0.3803P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5793 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.275953(14) 0.05888(2) 0.068348(14) 0.01816(7) Uani 1 1 d . . . B1 B 0.18937(12) 0.1705(2) -0.00510(12) 0.0221(4) Uani 1 1 d . . . O1 O 0.17010(7) 0.31121(13) 0.01090(7) 0.0257(3) Uani 1 1 d . . . O2 O 0.13095(7) 0.13322(13) -0.08258(7) 0.0257(3) Uani 1 1 d . . . P1 P 0.35312(3) 0.23065(5) 0.05318(3) 0.02392(11) Uani 1 1 d . . . P2 P 0.19136(3) 0.08215(5) 0.15031(3) 0.02292(11) Uani 1 1 d . . . P3 P 0.25082(3) -0.09873(5) -0.02990(3) 0.02343(11) Uani 1 1 d . . . P4 P 0.37041(3) -0.05454(5) 0.16194(3) 0.02383(11) Uani 1 1 d . . . C1 C 0.10336(11) 0.35165(19) -0.05358(11) 0.0243(4) Uani 1 1 d . . . C2 C 0.07972(11) 0.24404(19) -0.10940(11) 0.0245(4) Uani 1 1 d . . . C3 C 0.01345(12) 0.2549(2) -0.17979(12) 0.0329(5) Uani 1 1 d . . . H3 H -0.0031 0.1804 -0.2184 0.039 Uiso 1 1 calc R . . C4 C -0.02805(12) 0.3810(2) -0.19150(13) 0.0368(5) Uani 1 1 d . . . H4 H -0.0742 0.3928 -0.2393 0.044 Uiso 1 1 calc R . . C5 C -0.00376(13) 0.4889(2) -0.13543(13) 0.0365(5) Uani 1 1 d . . . H5 H -0.0332 0.5737 -0.1455 0.044 Uiso 1 1 calc R . . C6 C 0.06289(12) 0.4760(2) -0.06445(13) 0.0320(4) Uani 1 1 d . . . H6 H 0.0797 0.5497 -0.0253 0.038 Uiso 1 1 calc R . . C7 C 0.46748(11) 0.2181(2) 0.07474(13) 0.0367(5) Uani 1 1 d . . . H7A H 0.4902 0.3067 0.0620 0.055 Uiso 1 1 calc R . . H7B H 0.4823 0.1462 0.0386 0.055 Uiso 1 1 calc R . . H7C H 0.4906 0.1949 0.1350 0.055 Uiso 1 1 calc R . . C8 C 0.35040(12) 0.3888(2) 0.11518(13) 0.0337(5) Uani 1 1 d . . . H8A H 0.3682 0.3678 0.1763 0.051 Uiso 1 1 calc R . . H8B H 0.2936 0.4255 0.1016 0.051 Uiso 1 1 calc R . . H8C H 0.3879 0.4575 0.1006 0.051 Uiso 1 1 calc R . . C9 C 0.33850(14) 0.3088(2) -0.05345(12) 0.0406(5) Uani 1 1 d . . . H9A H 0.3751 0.3890 -0.0497 0.061 Uiso 1 1 calc R . . H9B H 0.2805 0.3381 -0.0745 0.061 Uiso 1 1 calc R . . H9C H 0.3521 0.2411 -0.0929 0.061 Uiso 1 1 calc R . . C10 C 0.07862(11) 0.0785(2) 0.10365(13) 0.0342(5) Uani 1 1 d . . . H10A H 0.0495 0.0899 0.1490 0.051 Uiso 1 1 calc R . . H10B H 0.0631 -0.0099 0.0748 0.051 Uiso 1 1 calc R . . H10C H 0.0632 0.1537 0.0622 0.051 Uiso 1 1 calc R . . C11 C 0.19866(12) 0.2440(2) 0.21028(12) 0.0321(4) Uani 1 1 d . . . H11A H 0.1577 0.2437 0.2447 0.048 Uiso 1 1 calc R . . H11B H 0.1875 0.3217 0.1703 0.048 Uiso 1 1 calc R . . H11C H 0.2546 0.2532 0.2479 0.048 Uiso 1 1 calc R . . C12 C 0.18896(13) -0.0358(2) 0.23908(12) 0.0365(5) Uani 1 1 d . . . H12A H 0.2439 -0.0382 0.2792 0.055 Uiso 1 1 calc R . . H12B H 0.1740 -0.1286 0.2165 0.055 Uiso 1 1 calc R . . H12C H 0.1477 -0.0034 0.2687 0.055 Uiso 1 1 calc R . . C13 C 0.25976(14) -0.0530(2) -0.13766(12) 0.0366(5) Uani 1 1 d . . . H13A H 0.2418 -0.1311 -0.1763 0.055 Uiso 1 1 calc R . . H13B H 0.3178 -0.0306 -0.1357 0.055 Uiso 1 1 calc R . . H13C H 0.2245 0.0270 -0.1584 0.055 Uiso 1 1 calc R . . C14 C 0.14731(12) -0.1779(2) -0.05500(13) 0.0380(5) Uani 1 1 d . . . H14A H 0.1049 -0.1062 -0.0728 0.057 Uiso 1 1 calc R . . H14B H 0.1388 -0.2250 -0.0042 0.057 Uiso 1 1 calc R . . H14C H 0.1429 -0.2446 -0.1014 0.057 Uiso 1 1 calc R . . C15 C 0.31027(15) -0.2609(2) -0.02190(14) 0.0447(6) Uani 1 1 d . . . H15A H 0.3050 -0.3121 0.0288 0.067 Uiso 1 1 calc R . . H15B H 0.3690 -0.2399 -0.0171 0.067 Uiso 1 1 calc R . . H15C H 0.2884 -0.3168 -0.0731 0.067 Uiso 1 1 calc R . . C16 C 0.46920(12) -0.1106(2) 0.13892(14) 0.0395(5) Uani 1 1 d . . . H16A H 0.4978 -0.0304 0.1227 0.059 Uiso 1 1 calc R . . H16B H 0.4574 -0.1772 0.0919 0.059 Uiso 1 1 calc R . . H16C H 0.5047 -0.1537 0.1899 0.059 Uiso 1 1 calc R . . C17 C 0.34352(14) -0.2215(2) 0.20306(13) 0.0380(5) Uani 1 1 d . . . H17A H 0.2982 -0.2647 0.1603 0.057 Uiso 0.50 1 calc PR . . H17B H 0.3258 -0.2064 0.2559 0.057 Uiso 0.50 1 calc PR . . H17C H 0.3923 -0.2821 0.2148 0.057 Uiso 0.50 1 calc PR . . H17D H 0.3794 -0.2374 0.2603 0.057 Uiso 0.50 1 calc PR . . H17E H 0.3517 -0.2957 0.1648 0.057 Uiso 0.50 1 calc PR . . H17F H 0.2852 -0.2200 0.2059 0.057 Uiso 0.50 1 calc PR . . C18 C 0.41436(12) 0.0348(2) 0.26333(12) 0.0349(5) Uani 1 1 d . . . H18A H 0.4551 -0.0251 0.3010 0.052 Uiso 1 1 calc R . . H18B H 0.3697 0.0574 0.2909 0.052 Uiso 1 1 calc R . . H18C H 0.4417 0.1199 0.2522 0.052 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 Co1 0.01916(12) 0.01853(13) 0.01582(11) 0.00029(9) 0.00249(9) 0.00093(9) B1 0.0228(10) 0.0230(11) 0.0200(9) 0.0012(8) 0.0044(8) -0.0005(8) O1 0.0280(7) 0.0211(7) 0.0236(6) -0.0002(5) -0.0020(5) 0.0031(5) O2 0.0282(7) 0.0235(7) 0.0217(6) -0.0019(5) -0.0009(5) 0.0050(5) P1 0.0255(2) 0.0248(3) 0.0204(2) 0.00047(18) 0.00364(18) -0.0043(2) P2 0.0214(2) 0.0285(3) 0.0189(2) 0.00053(18) 0.00490(18) 0.00147(19) P3 0.0264(2) 0.0200(2) 0.0224(2) -0.00308(18) 0.00310(19) 0.00171(19) P4 0.0241(2) 0.0261(3) 0.0199(2) 0.00187(19) 0.00264(18) 0.0052(2) C1 0.0234(9) 0.0250(9) 0.0235(9) 0.0050(7) 0.0039(7) 0.0019(8) C2 0.0238(9) 0.0274(10) 0.0220(8) 0.0043(7) 0.0051(7) 0.0034(8) C3 0.0305(10) 0.0426(12) 0.0230(9) -0.0008(8) 0.0017(8) 0.0029(9) C4 0.0270(10) 0.0510(14) 0.0289(10) 0.0125(10) 0.0005(8) 0.0085(10) C5 0.0355(11) 0.0351(12) 0.0381(11) 0.0135(10) 0.0080(9) 0.0140(10) C6 0.0355(11) 0.0261(10) 0.0331(10) 0.0029(8) 0.0059(9) 0.0039(9) C7 0.0273(10) 0.0427(13) 0.0407(11) -0.0016(10) 0.0099(9) -0.0071(9) C8 0.0344(11) 0.0258(10) 0.0378(11) -0.0052(9) 0.0029(9) -0.0065(9) C9 0.0478(13) 0.0431(13) 0.0292(10) 0.0099(9) 0.0063(9) -0.0126(11) C10 0.0218(9) 0.0503(13) 0.0303(10) 0.0010(9) 0.0061(8) -0.0002(9) C11 0.0334(10) 0.0369(11) 0.0262(9) -0.0079(8) 0.0076(8) 0.0049(9) C12 0.0343(11) 0.0476(13) 0.0299(10) 0.0098(9) 0.0123(9) 0.0011(10) C13 0.0486(13) 0.0375(12) 0.0253(10) -0.0075(9) 0.0123(9) 0.0010(10) C14 0.0368(11) 0.0312(11) 0.0426(12) -0.0077(9) 0.0036(9) -0.0113(9) C15 0.0551(14) 0.0310(12) 0.0405(12) -0.0117(9) -0.0022(11) 0.0144(11) C16 0.0285(11) 0.0479(14) 0.0418(12) 0.0030(10) 0.0085(9) 0.0140(10) C17 0.0475(13) 0.0297(11) 0.0356(11) 0.0099(9) 0.0080(10) 0.0088(10) C18 0.0347(11) 0.0420(13) 0.0229(9) -0.0013(9) -0.0025(8) 0.0050(9) _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 Co1 B1 1.949(2) . ? Co1 P1 2.1527(5) . ? Co1 P2 2.1686(5) . ? Co1 P3 2.1687(5) . ? Co1 P4 2.1859(5) . ? B1 O2 1.427(2) . ? B1 O1 1.440(2) . ? O1 C1 1.376(2) . ? O2 C2 1.373(2) . ? P1 C8 1.839(2) . ? P1 C9 1.8427(19) . ? P1 C7 1.8473(19) . ? P2 C11 1.8334(19) . ? P2 C10 1.8362(19) . ? P2 C12 1.8433(19) . ? P3 C14 1.833(2) . ? P3 C13 1.8383(19) . ? P3 C15 1.844(2) . ? P4 C18 1.8370(19) . ? P4 C17 1.847(2) . ? P4 C16 1.8514(19) . ? C1 C6 1.370(3) . ? C1 C2 1.372(3) . ? C2 C3 1.376(2) . ? C3 C4 1.393(3) . ? C3 H3 0.9500 . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Co1 P1 82.56(6) . . ? B1 Co1 P2 79.77(6) . . ? P1 Co1 P2 118.89(2) . . ? B1 Co1 P3 88.12(6) . . ? P1 Co1 P3 118.30(2) . . ? P2 Co1 P3 118.98(2) . . ? B1 Co1 P4 174.04(6) . . ? P1 Co1 P4 97.09(2) . . ? P2 Co1 P4 95.28(2) . . ? P3 Co1 P4 97.24(2) . . ? O2 B1 O1 105.35(14) . . ? O2 B1 Co1 129.16(14) . . ? O1 B1 Co1 125.47(13) . . ? C1 O1 B1 107.90(13) . . ? C2 O2 B1 108.16(14) . . ? C8 P1 C9 98.65(10) . . ? C8 P1 C7 96.62(10) . . ? C9 P1 C7 95.37(10) . . ? C8 P1 Co1 119.21(7) . . ? C9 P1 Co1 118.77(7) . . ? C7 P1 Co1 122.73(7) . . ? C11 P2 C10 99.22(9) . . ? C11 P2 C12 97.58(9) . . ? C10 P2 C12 95.20(9) . . ? C11 P2 Co1 116.37(7) . . ? C10 P2 Co1 119.74(7) . . ? C12 P2 Co1 123.59(7) . . ? C14 P3 C13 100.57(10) . . ? C14 P3 C15 96.57(11) . . ? C13 P3 C15 95.99(10) . . ? C14 P3 Co1 117.16(7) . . ? C13 P3 Co1 118.50(7) . . ? C15 P3 Co1 123.21(7) . . ? C18 P4 C17 99.85(10) . . ? C18 P4 C16 98.19(10) . . ? C17 P4 C16 96.90(10) . . ? C18 P4 Co1 115.92(7) . . ? C17 P4 Co1 119.62(7) . . ? C16 P4 Co1 121.86(7) . . ? C6 C1 C2 122.30(17) . . ? C6 C1 O1 128.68(17) . . ? C2 C1 O1 109.02(15) . . ? C1 C2 O2 109.56(15) . . ? C1 C2 C3 121.64(18) . . ? O2 C2 C3 128.80(18) . . ? C2 C3 C4 116.52(19) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? C5 C4 C3 121.58(18) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 121.17(19) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 116.79(19) . . ? C1 C6 H6 121.6 . . ? C5 C6 H6 121.6 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P3 C13 H13A 109.5 . . ? P3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P3 C14 H14A 109.5 . . ? P3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P3 C15 H15A 109.5 . . ? P3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P4 C16 H16A 109.5 . . ? P4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P4 C17 H17A 109.5 . . ? P4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P4 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? P4 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? P4 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? P4 C18 H18A 109.5 . . ? P4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 P1 Co1 B1 O2 127.86(17) . . . . ? P2 Co1 B1 O2 -110.90(17) . . . . ? P3 Co1 B1 O2 9.00(16) . . . . ? P1 Co1 B1 O1 -54.12(15) . . . . ? P2 Co1 B1 O1 67.12(15) . . . . ? P3 Co1 B1 O1 -172.98(15) . . . . ? O2 B1 O1 C1 0.75(18) . . . . ? Co1 B1 O1 C1 -177.65(13) . . . . ? O1 B1 O2 C2 -1.08(18) . . . . ? Co1 B1 O2 C2 177.24(14) . . . . ? B1 Co1 P1 C8 77.81(10) . . . . ? P2 Co1 P1 C8 3.86(8) . . . . ? P3 Co1 P1 C8 161.62(8) . . . . ? P4 Co1 P1 C8 -96.19(8) . . . . ? B1 Co1 P1 C9 -42.43(11) . . . . ? P2 Co1 P1 C9 -116.38(9) . . . . ? P3 Co1 P1 C9 41.38(9) . . . . ? P4 Co1 P1 C9 143.57(9) . . . . ? B1 Co1 P1 C7 -161.11(10) . . . . ? P2 Co1 P1 C7 124.95(8) . . . . ? P3 Co1 P1 C7 -77.30(8) . . . . ? P4 Co1 P1 C7 24.89(8) . . . . ? B1 Co1 P2 C11 -81.32(10) . . . . ? P1 Co1 P2 C11 -5.78(8) . . . . ? P3 Co1 P2 C11 -163.38(7) . . . . ? P4 Co1 P2 C11 95.33(7) . . . . ? B1 Co1 P2 C10 37.97(10) . . . . ? P1 Co1 P2 C10 113.50(8) . . . . ? P3 Co1 P2 C10 -44.10(9) . . . . ? P4 Co1 P2 C10 -145.39(8) . . . . ? B1 Co1 P2 C12 158.28(11) . . . . ? P1 Co1 P2 C12 -126.18(9) . . . . ? P3 Co1 P2 C12 76.22(9) . . . . ? P4 Co1 P2 C12 -25.08(9) . . . . ? B1 Co1 P3 C14 -63.54(10) . . . . ? P1 Co1 P3 C14 -144.06(8) . . . . ? P2 Co1 P3 C14 13.67(9) . . . . ? P4 Co1 P3 C14 113.83(8) . . . . ? B1 Co1 P3 C13 57.33(10) . . . . ? P1 Co1 P3 C13 -23.18(9) . . . . ? P2 Co1 P3 C13 134.55(8) . . . . ? P4 Co1 P3 C13 -125.29(8) . . . . ? B1 Co1 P3 C15 177.15(12) . . . . ? P1 Co1 P3 C15 96.64(10) . . . . ? P2 Co1 P3 C15 -105.63(10) . . . . ? P4 Co1 P3 C15 -5.47(10) . . . . ? P1 Co1 P4 C18 60.94(8) . . . . ? P2 Co1 P4 C18 -59.09(8) . . . . ? P3 Co1 P4 C18 -179.24(8) . . . . ? P1 Co1 P4 C17 -179.38(8) . . . . ? P2 Co1 P4 C17 60.59(8) . . . . ? P3 Co1 P4 C17 -59.56(8) . . . . ? P1 Co1 P4 C16 -58.31(9) . . . . ? P2 Co1 P4 C16 -178.33(9) . . . . ? P3 Co1 P4 C16 61.52(9) . . . . ? B1 O1 C1 C6 179.10(19) . . . . ? B1 O1 C1 C2 -0.15(19) . . . . ? C6 C1 C2 O2 -179.86(16) . . . . ? O1 C1 C2 O2 -0.6(2) . . . . ? C6 C1 C2 C3 -0.2(3) . . . . ? O1 C1 C2 C3 179.13(16) . . . . ? B1 O2 C2 C1 1.03(19) . . . . ? B1 O2 C2 C3 -178.62(18) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? O2 C2 C3 C4 179.87(17) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C2 C1 C6 C5 -0.2(3) . . . . ? O1 C1 C6 C5 -179.38(18) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.369 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.056 data_6 _database_code_depnum_ccdc_archive 'CCDC 290421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 B2 F6 O4' _chemical_formula_sum 'C28 H24 B2 F6 O4' _chemical_formula_weight 560.09 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.588(1) _cell_length_b 13.554(1) _cell_length_c 26.571(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.58(1) _cell_angle_gamma 90.00 _cell_volume 4088.4(7) _cell_formula_units_Z 6 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5145 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of 600 \w-scans each (scan width 0.3\% \w, 20s exposure); every run at a different \f angle. Crystal to detector distance 4.87 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 45186 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9403 _reflns_number_gt 6654 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 6.02A (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXTL version 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL version 6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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. Group C(14)F~3~ is disordered by rotation around the C(11)---C(14) bond and a tilt of this bond, atoms C(14), F(1), F(2) and F(3) were refined in positions A (anisotropic, occupancy 75%) and B (isotropic, occupancy 25%). Group C(35)F~3~ is disordered by rotation around the C(32)---C(35) bond. Atoms F(4), F(5) and F(6) were refined in positions A (anisotropic, occupancy 50%), B and C (isotropic, rigid-body, occupancy 25% each). One molecule is in general position, another lies on a twofold axis and hence has its Bpin and Bcat groups symmetrically superimposed (with occupancies 50%). Bcat group: O(2A), C(1A) to C(6A), Bpin group: O(2B), C(2B) to C(6B) with the attached hydrogens. The C(1), B(1) and O(1) are ordered. ; _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^)+(0.0376P)^2^+9.5145P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9403 _refine_ls_number_parameters 580 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2090 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.7249(2) 0.84127(19) 0.28223(12) 0.0539(7) Uani 1 1 d . A . O2A O 0.6411(6) 0.8588(5) 0.2048(2) 0.0580(16) Uani 0.50 1 d P A 1 O2B O 0.5508(5) 0.8967(4) 0.2256(2) 0.0555(16) Uani 0.50 1 d P A 2 C1 C 0.7630(4) 0.9316(3) 0.2628(2) 0.0618(13) Uani 1 1 d . . . C2A C 0.7240(7) 0.9341(6) 0.2168(3) 0.0463(18) Uiso 0.50 1 d P A 1 C3A C 0.7492(10) 1.0056(8) 0.1877(4) 0.074(3) Uiso 0.50 1 d P A 1 H3A H 0.7102 1.0134 0.1530 0.089 Uiso 0.50 1 d PR A 1 C4A C 0.8363(11) 1.0732(9) 0.2117(5) 0.086(3) Uiso 0.50 1 d P A 1 H4A H 0.8629 1.1229 0.1915 0.103 Uiso 0.50 1 d PR A 1 C5A C 0.8889(10) 1.0649(8) 0.2637(4) 0.073(3) Uiso 0.50 1 d P A 1 H5A H 0.9445 1.1120 0.2802 0.088 Uiso 0.50 1 d PR A 1 C6A C 0.8567(9) 0.9881(8) 0.2934(4) 0.052(3) Uiso 0.50 1 d P A 1 H6A H 0.8932 0.9728 0.3278 0.063 Uiso 0.50 1 d PR A 1 C2B C 0.6251(7) 0.9827(6) 0.2385(3) 0.0505(19) Uiso 0.50 1 d P A 2 C3B C 0.8159(10) 0.9140(9) 0.2127(4) 0.078(3) Uiso 0.50 1 d P A 2 H31B H 0.7633 0.8715 0.1884 0.117 Uiso 0.50 1 d PR A 2 H32B H 0.8932 0.8824 0.2226 0.117 Uiso 0.50 1 d PR A 2 H33B H 0.8246 0.9777 0.1964 0.117 Uiso 0.50 1 d PR A 2 C4B C 0.8248(10) 0.9913(8) 0.3019(4) 0.059(3) Uiso 0.50 1 d P A 2 H41B H 0.7821 0.9961 0.3301 0.088 Uiso 0.50 1 d PR A 2 H42B H 0.8344 1.0573 0.2883 0.088 Uiso 0.50 1 d PR A 2 H43B H 0.9025 0.9620 0.3146 0.088 Uiso 0.50 1 d PR A 2 C5B C 0.6181(11) 1.0481(9) 0.1909(5) 0.086(3) Uiso 0.50 1 d P A 2 H51B H 0.6451 1.0089 0.1645 0.129 Uiso 0.50 1 d PR A 2 H52B H 0.6690 1.1060 0.1993 0.129 Uiso 0.50 1 d PR A 2 H53B H 0.5368 1.0697 0.1779 0.129 Uiso 0.50 1 d PR A 2 C6B C 0.5775(9) 1.0386(7) 0.2801(4) 0.065(2) Uiso 0.50 1 d P A 2 H61B H 0.5842 0.9955 0.3102 0.098 Uiso 0.50 1 d PR A 2 H62B H 0.4951 1.0586 0.2685 0.098 Uiso 0.50 1 d PR A 2 H63B H 0.6265 1.0973 0.2894 0.098 Uiso 0.50 1 d PR A 2 C7 C 0.5595(3) 0.7137(3) 0.25165(13) 0.0400(8) Uani 1 1 d . . . C8 C 0.6288(3) 0.6207(3) 0.25646(13) 0.0366(8) Uani 1 1 d . B . C9 C 0.7079(3) 0.6021(3) 0.22411(13) 0.0417(8) Uani 1 1 d . . . H9 H 0.7209 0.6511 0.2003 0.050 Uiso 1 1 d R . . C10 C 0.7678(3) 0.5138(3) 0.22690(14) 0.0473(10) Uani 1 1 d . B . H10 H 0.8189 0.5012 0.2038 0.057 Uiso 1 1 d R . . C11 C 0.7515(3) 0.4429(3) 0.26261(14) 0.0475(10) Uani 1 1 d D . . C12 C 0.6790(3) 0.4632(3) 0.29697(14) 0.0411(8) Uani 1 1 d . B . H12 H 0.6705 0.4165 0.3226 0.049 Uiso 1 1 d R . . C13 C 0.6182(3) 0.5513(3) 0.29365(13) 0.0367(7) Uani 1 1 d . . . H13 H 0.5681 0.5646 0.3171 0.044 Uiso 1 1 d R B . C14A C 0.8034(5) 0.3396(4) 0.2649(2) 0.0487(14) Uiso 0.75 1 d PD B 1 F1A F 0.8456(9) 0.3195(7) 0.2247(2) 0.157(4) Uani 0.75 1 d PD B 1 F2A F 0.8953(5) 0.3326(3) 0.30438(16) 0.0901(16) Uani 0.75 1 d PD B 1 F3A F 0.7335(4) 0.2683(3) 0.2718(3) 0.123(2) Uani 0.75 1 d PD B 1 C14B C 0.8396(11) 0.3660(9) 0.2649(5) 0.037(3) Uiso 0.25 1 d PD B 2 F1B F 0.8279(11) 0.3108(11) 0.2219(4) 0.041(3) Uiso 0.25 1 d PD B 2 F2B F 0.8289(15) 0.3045(12) 0.3022(5) 0.096(5) Uiso 0.25 1 d PD B 2 F3B F 0.9504(12) 0.3926(13) 0.2741(6) 0.123(5) Uiso 0.25 1 d PD B 2 B1 B 0.6277(6) 0.8138(4) 0.25005(18) 0.0599(14) Uani 1 1 d . . . O3 O 0.8918(2) 0.5653(2) 0.04687(9) 0.0459(6) Uani 1 1 d . . . O4 O 0.8701(2) 0.60780(19) 0.12744(9) 0.0407(6) Uani 1 1 d . . . O6 O 0.4804(2) 0.64527(18) 0.10476(9) 0.0381(6) Uani 1 1 d . . . O5 O 0.6275(2) 0.68918(18) 0.06342(9) 0.0387(6) Uani 1 1 d . . . C15 C 1.0008(3) 0.6181(3) 0.07008(15) 0.0486(10) Uani 1 1 d . . . C16 C 0.9642(3) 0.6722(3) 0.11602(15) 0.0459(9) Uani 1 1 d . . . C17 C 1.0939(4) 0.5397(4) 0.0860(2) 0.0671(13) Uani 1 1 d . . . H171 H 1.0713 0.4988 0.1129 0.101 Uiso 1 1 d R . . H172 H 1.1703 0.5708 0.0993 0.101 Uiso 1 1 d R . . H173 H 1.0999 0.4982 0.0564 0.101 Uiso 1 1 d R . . C18 C 1.0346(4) 0.6856(5) 0.02992(18) 0.0818(18) Uani 1 1 d . . . H181 H 1.0512 0.6474 0.0008 0.123 Uiso 1 1 d R . . H182 H 1.1048 0.7234 0.0456 0.123 Uiso 1 1 d R . . H183 H 0.9692 0.7311 0.0176 0.123 Uiso 1 1 d R . . C19 C 1.0600(4) 0.6790(4) 0.16402(18) 0.0635(12) Uani 1 1 d . . . H191 H 1.0289 0.7142 0.1907 0.095 Uiso 1 1 d R . . H192 H 1.1276 0.7153 0.1563 0.095 Uiso 1 1 d R . . H193 H 1.0854 0.6128 0.1765 0.095 Uiso 1 1 d R . . C20 C 0.9072(4) 0.7721(3) 0.1025(2) 0.0780(16) Uani 1 1 d . . . H201 H 0.8451 0.7657 0.0716 0.117 Uiso 1 1 d R . . H202 H 0.9670 0.8189 0.0958 0.117 Uiso 1 1 d R . . H203 H 0.8727 0.7966 0.1309 0.117 Uiso 1 1 d R . . C22 C 0.4734(3) 0.7461(3) 0.09482(13) 0.0364(7) Uani 1 1 d . . . C21 C 0.5622(3) 0.7731(3) 0.07005(13) 0.0380(8) Uani 1 1 d . . . C26 C 0.5754(4) 0.8672(3) 0.05416(16) 0.0477(9) Uani 1 1 d . . . H26 H 0.6359 0.8844 0.0363 0.057 Uiso 1 1 d R . . C25 C 0.4937(4) 0.9362(3) 0.06501(16) 0.0538(10) Uani 1 1 d . . . H25 H 0.5003 1.0030 0.0551 0.065 Uiso 1 1 d R . . C24 C 0.4058(4) 0.9092(3) 0.09046(16) 0.0527(10) Uani 1 1 d . . . H24 H 0.3517 0.9576 0.0973 0.063 Uiso 1 1 d R . . C23 C 0.3936(4) 0.8128(3) 0.10627(15) 0.0481(9) Uani 1 1 d . . . H23 H 0.3335 0.7936 0.1239 0.058 Uiso 1 1 d R . . C27 C 0.7250(3) 0.4775(2) 0.08131(12) 0.0304(7) Uani 1 1 d . . . C28 C 0.6136(3) 0.5035(2) 0.08533(12) 0.0312(7) Uani 1 1 d . . . C29 C 0.7610(3) 0.3733(2) 0.07535(12) 0.0316(7) Uani 1 1 d . . . C30 C 0.6966(3) 0.3112(3) 0.03808(13) 0.0363(7) Uani 1 1 d . . . H30 H 0.6279 0.3355 0.0159 0.044 Uiso 1 1 d R . . C31 C 0.7329(3) 0.2147(3) 0.03287(14) 0.0398(8) Uani 1 1 d . . . H31 H 0.6883 0.1723 0.0078 0.048 Uiso 1 1 d R . . C32 C 0.8342(3) 0.1800(3) 0.06452(14) 0.0398(8) Uani 1 1 d . C . C33 C 0.8996(3) 0.2401(3) 0.10169(14) 0.0383(8) Uani 1 1 d . . . H33 H 0.9685 0.2154 0.1236 0.046 Uiso 1 1 d R . . C34 C 0.8633(3) 0.3368(3) 0.10663(13) 0.0354(7) Uani 1 1 d . . . H34 H 0.9090 0.3786 0.1316 0.043 Uiso 1 1 d R . . C35 C 0.8735(3) 0.0766(2) 0.05809(15) 0.0565(11) Uani 1 1 d D . . F4B F 0.8095(3) 0.0234(2) 0.02100(15) 0.057(3) Uiso 0.25 1 d PRD C 2 F5B F 0.8608(3) 0.0202(2) 0.10199(15) 0.086(4) Uiso 0.25 1 d PRD C 2 F6B F 0.9849(3) 0.0629(2) 0.05740(15) 0.066(3) Uiso 0.25 1 d PRD C 2 F4C F 0.9439(3) 0.0761(2) 0.02376(15) 0.060(3) Uiso 0.25 1 d PRD C 3 F5C F 0.7893(3) 0.0134(2) 0.04462(15) 0.064(4) Uiso 0.25 1 d PRD C 3 F6C F 0.9408(3) 0.0437(2) 0.10216(15) 0.064(4) Uiso 0.25 1 d PRD C 3 C36 C 0.5208(3) 0.4281(2) 0.08859(12) 0.0305(7) Uani 1 1 d . . . C37 C 0.4112(3) 0.4337(3) 0.05548(13) 0.0356(7) Uani 1 1 d . . . H37 H 0.3942 0.4885 0.0329 0.043 Uiso 1 1 d R . . C38 C 0.3273(3) 0.3618(3) 0.05514(13) 0.0377(8) Uani 1 1 d . . . H38 H 0.2534 0.3661 0.0320 0.045 Uiso 1 1 d R . . C39 C 0.3511(3) 0.2831(3) 0.08867(14) 0.0380(8) Uani 1 1 d . D . C40 C 0.4575(3) 0.2782(3) 0.12346(15) 0.0409(8) Uani 1 1 d . . . H40 H 0.4724 0.2253 0.1473 0.049 Uiso 1 1 d R . . C41 C 0.5421(3) 0.3507(3) 0.12335(14) 0.0381(8) Uani 1 1 d . . . H41 H 0.6148 0.3474 0.1473 0.046 Uiso 1 1 d R . . C42 C 0.2611(3) 0.2044(3) 0.08588(18) 0.0500(10) Uani 1 1 d . . . F4A F 0.8858(7) 0.0626(5) 0.0071(2) 0.106(3) Uani 0.50 1 d PD C 1 F5A F 0.7979(5) 0.0121(4) 0.0659(5) 0.121(3) Uani 0.50 1 d PD C 1 F6A F 0.9780(4) 0.0536(3) 0.0852(2) 0.0550(12) Uani 0.50 1 d PD C 1 F7A F 0.1546(2) 0.2386(2) 0.0855(2) 0.0796(12) Uani 0.85 1 d P D 1 F8A F 0.2842(3) 0.1410(3) 0.12566(16) 0.0809(11) Uani 0.85 1 d P D 1 F9A F 0.2532(4) 0.1475(3) 0.04460(18) 0.0965(15) Uani 0.85 1 d P D 1 F7B F 0.302(2) 0.122(2) 0.0789(12) 0.091(7) Uiso 0.15 1 d P D 2 F8B F 0.164(2) 0.2192(19) 0.0517(9) 0.084(7) Uiso 0.15 1 d P D 2 F9B F 0.226(2) 0.1981(19) 0.1299(9) 0.086(6) Uiso 0.15 1 d P D 2 B2 B 0.8287(3) 0.5542(3) 0.08455(15) 0.0337(8) Uani 1 1 d . . . B3 B 0.5764(3) 0.6134(3) 0.08531(14) 0.0331(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0449(15) 0.0327(14) 0.084(2) 0.0090(14) 0.0124(14) -0.0012(12) O2A 0.068(4) 0.057(4) 0.044(3) 0.011(3) 0.002(3) -0.024(3) O2B 0.067(4) 0.025(2) 0.059(3) -0.001(2) -0.025(3) 0.005(2) C1 0.075(3) 0.042(2) 0.080(3) -0.019(2) 0.044(3) -0.017(2) C7 0.056(2) 0.0335(18) 0.0286(16) 0.0002(14) 0.0049(16) -0.0047(16) C8 0.0392(18) 0.0380(19) 0.0320(17) -0.0032(14) 0.0056(14) -0.0094(15) C9 0.0401(19) 0.052(2) 0.0333(18) 0.0028(16) 0.0091(15) -0.0120(17) C10 0.0331(18) 0.077(3) 0.0325(18) -0.0077(19) 0.0095(15) 0.0010(19) C11 0.041(2) 0.069(3) 0.0309(18) -0.0025(18) 0.0039(15) 0.0147(19) C12 0.0418(19) 0.047(2) 0.0346(18) 0.0008(16) 0.0083(15) 0.0047(16) C13 0.0378(18) 0.0423(19) 0.0313(16) -0.0018(14) 0.0102(14) -0.0011(15) F1A 0.260(10) 0.149(6) 0.068(3) 0.005(3) 0.051(4) 0.136(6) F2A 0.094(3) 0.077(3) 0.074(3) -0.010(2) -0.043(2) 0.039(3) F3A 0.093(3) 0.040(2) 0.244(7) -0.009(3) 0.055(4) 0.012(2) B1 0.096(4) 0.044(3) 0.033(2) 0.0017(19) -0.003(2) -0.017(3) O3 0.0356(13) 0.0653(18) 0.0372(13) 0.0011(12) 0.0082(10) -0.0173(12) O4 0.0364(13) 0.0444(14) 0.0417(13) -0.0040(11) 0.0087(10) -0.0111(11) O6 0.0384(13) 0.0390(13) 0.0390(13) 0.0048(11) 0.0124(10) 0.0006(10) O5 0.0356(12) 0.0362(13) 0.0463(14) 0.0039(11) 0.0128(11) -0.0017(10) C15 0.0343(18) 0.066(3) 0.045(2) 0.0024(19) 0.0083(16) -0.0175(18) C16 0.0386(19) 0.045(2) 0.052(2) 0.0019(18) 0.0046(17) -0.0141(17) C17 0.034(2) 0.079(3) 0.088(3) -0.014(3) 0.012(2) -0.003(2) C18 0.063(3) 0.125(5) 0.058(3) 0.018(3) 0.013(2) -0.051(3) C19 0.049(2) 0.076(3) 0.061(3) -0.014(2) 0.001(2) -0.022(2) C20 0.055(3) 0.043(3) 0.132(5) 0.011(3) 0.009(3) -0.014(2) C22 0.0409(18) 0.0346(18) 0.0334(17) 0.0003(14) 0.0063(14) -0.0021(15) C21 0.0388(18) 0.0371(19) 0.0366(18) -0.0011(15) 0.0039(14) -0.0018(15) C26 0.053(2) 0.037(2) 0.054(2) 0.0007(17) 0.0108(18) -0.0071(17) C25 0.070(3) 0.034(2) 0.053(2) -0.0035(18) 0.000(2) -0.0014(19) C24 0.064(3) 0.045(2) 0.048(2) -0.0095(18) 0.005(2) 0.011(2) C23 0.054(2) 0.050(2) 0.041(2) -0.0055(18) 0.0128(18) 0.0076(19) C27 0.0319(16) 0.0315(16) 0.0270(15) 0.0041(13) 0.0038(12) -0.0052(13) C28 0.0304(15) 0.0366(17) 0.0257(15) 0.0037(13) 0.0034(12) -0.0038(13) C29 0.0299(16) 0.0325(17) 0.0334(16) 0.0024(13) 0.0088(13) -0.0031(13) C30 0.0319(16) 0.0407(19) 0.0353(17) 0.0006(15) 0.0041(14) -0.0054(14) C31 0.0394(19) 0.0390(19) 0.0401(19) -0.0045(15) 0.0059(15) -0.0095(15) C32 0.0355(18) 0.0383(19) 0.046(2) 0.0007(16) 0.0104(15) -0.0013(15) C33 0.0293(16) 0.043(2) 0.0414(19) 0.0028(16) 0.0050(14) -0.0008(15) C34 0.0302(16) 0.0410(19) 0.0346(17) 0.0002(15) 0.0054(13) -0.0048(14) C35 0.046(2) 0.048(2) 0.073(3) -0.009(2) 0.006(2) 0.0002(19) C36 0.0271(15) 0.0318(16) 0.0328(16) -0.0002(13) 0.0066(12) -0.0023(13) C37 0.0338(17) 0.0395(18) 0.0322(16) 0.0023(14) 0.0033(13) -0.0014(14) C38 0.0289(16) 0.044(2) 0.0380(18) -0.0029(15) 0.0026(14) -0.0005(14) C39 0.0331(17) 0.0341(18) 0.049(2) -0.0032(15) 0.0133(15) -0.0005(14) C40 0.0326(17) 0.0378(19) 0.054(2) 0.0118(17) 0.0123(16) 0.0026(15) C41 0.0265(15) 0.046(2) 0.0410(19) 0.0085(16) 0.0044(14) -0.0012(14) C42 0.040(2) 0.041(2) 0.071(3) -0.005(2) 0.018(2) -0.0042(17) F4A 0.141(7) 0.100(5) 0.070(4) -0.028(4) 0.004(5) 0.076(5) F5A 0.066(4) 0.027(3) 0.275(12) -0.032(4) 0.047(6) -0.022(3) F6A 0.053(3) 0.033(2) 0.075(4) 0.004(2) 0.003(3) 0.011(2) F7A 0.0324(15) 0.061(2) 0.154(4) -0.009(2) 0.037(2) -0.0090(14) F8A 0.072(2) 0.057(2) 0.113(3) 0.020(2) 0.017(2) -0.0270(18) F9A 0.108(3) 0.087(3) 0.110(3) -0.059(3) 0.059(3) -0.067(2) B2 0.0291(18) 0.037(2) 0.0339(19) 0.0055(16) 0.0032(15) -0.0019(15) B3 0.0315(18) 0.039(2) 0.0277(17) 0.0026(15) 0.0039(14) -0.0021(16) _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 O1 B1 1.323(6) . ? O1 C1 1.433(5) . ? O2A B1 1.384(7) . ? O2A C2A 1.394(9) . ? O2B C2B 1.448(10) . ? O2B B1 1.499(7) . ? C1 C2A 1.215(9) . ? C1 C4B 1.395(12) . ? C1 C6A 1.439(11) . ? C1 C3B 1.592(12) . ? C1 C2B 1.742(10) . ? C2A C3A 1.308(13) . ? C3A C4A 1.415(15) . ? C4A C5A 1.400(15) . ? C5A C6A 1.400(14) . ? C2B C6B 1.532(12) . ? C2B C5B 1.534(14) . ? C7 C7 1.364(8) 2_655 ? C7 C8 1.487(5) . ? C7 B1 1.575(6) . ? C8 C13 1.388(5) . ? C8 C9 1.399(5) . ? C9 C10 1.378(6) . ? C10 C11 1.390(6) . ? C11 C12 1.387(5) . ? C11 C14B 1.452(12) . ? C11 C14A 1.520(7) . ? C12 C13 1.379(5) . ? C14A F1A 1.288(7) . ? C14A F3A 1.298(7) . ? C14A F2A 1.340(6) . ? C14B F3B 1.308(12) . ? C14B F2B 1.321(12) . ? C14B F1B 1.349(12) . ? O3 B2 1.362(4) . ? O3 C15 1.475(4) . ? O4 B2 1.355(5) . ? O4 C16 1.475(4) . ? O6 B3 1.387(4) . ? O6 C22 1.392(4) . ? O5 B3 1.373(4) . ? O5 C21 1.397(4) . ? C15 C17 1.513(6) . ? C15 C18 1.516(6) . ? C15 C16 1.554(6) . ? C16 C19 1.516(5) . ? C16 C20 1.518(6) . ? C22 C23 1.370(5) . ? C22 C21 1.378(5) . ? C21 C26 1.363(5) . ? C26 C25 1.401(6) . ? C25 C24 1.380(6) . ? C24 C23 1.388(6) . ? C27 C28 1.363(4) . ? C27 C29 1.491(5) . ? C27 B2 1.578(5) . ? C28 C36 1.498(4) . ? C28 B3 1.549(5) . ? C29 C34 1.395(5) . ? C29 C30 1.396(5) . ? C30 C31 1.389(5) . ? C31 C32 1.382(5) . ? C32 C33 1.384(5) . ? C32 C35 1.494(5) . ? C33 C34 1.390(5) . ? C35 F5A 1.284(6) . ? C35 F5C 1.2936 . ? C35 F6B 1.3084 . ? C35 F6A 1.317(6) . ? C35 F4B 1.3224 . ? C35 F4C 1.3406 . ? C35 F6C 1.3456 . ? C35 F4A 1.403(6) . ? C35 F5B 1.4267 . ? C36 C41 1.387(5) . ? C36 C37 1.394(4) . ? C37 C38 1.376(5) . ? C38 C39 1.382(5) . ? C39 C40 1.386(5) . ? C39 C42 1.483(5) . ? C40 C41 1.389(5) . ? C42 F7B 1.24(3) . ? C42 F8B 1.31(2) . ? C42 F7A 1.317(5) . ? C42 F9B 1.32(2) . ? C42 F9A 1.329(5) . ? C42 F8A 1.347(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 O1 C1 107.0(4) . . ? B1 O2A C2A 108.4(5) . . ? C2B O2B B1 103.1(5) . . ? C2A C1 O1 107.8(5) . . ? C4B C1 O1 112.1(6) . . ? C2A C1 C6A 129.7(7) . . ? O1 C1 C6A 120.2(6) . . ? C4B C1 C3B 118.9(7) . . ? O1 C1 C3B 111.8(5) . . ? C4B C1 C2B 110.0(6) . . ? O1 C1 C2B 98.4(4) . . ? C3B C1 C2B 103.2(6) . . ? C1 C2A C3A 122.1(9) . . ? C1 C2A O2A 108.1(7) . . ? C3A C2A O2A 129.2(8) . . ? C2A C3A C4A 116.0(11) . . ? C5A C4A C3A 121.4(12) . . ? C6A C5A C4A 120.3(11) . . ? C5A C6A C1 109.5(9) . . ? O2B C2B C6B 106.6(7) . . ? O2B C2B C5B 109.7(7) . . ? C6B C2B C5B 110.0(8) . . ? O2B C2B C1 103.1(6) . . ? C6B C2B C1 111.5(6) . . ? C5B C2B C1 115.4(7) . . ? C7 C7 C8 121.82(19) 2_655 . ? C7 C7 B1 120.3(3) 2_655 . ? C8 C7 B1 117.9(4) . . ? C13 C8 C9 118.5(3) . . ? C13 C8 C7 120.9(3) . . ? C9 C8 C7 120.6(3) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C11 120.1(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 C14B 129.0(6) . . ? C10 C11 C14B 109.5(6) . . ? C12 C11 C14A 116.4(4) . . ? C10 C11 C14A 123.8(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C8 121.0(3) . . ? F1A C14A F3A 108.1(6) . . ? F1A C14A F2A 105.1(6) . . ? F3A C14A F2A 104.9(5) . . ? F1A C14A C11 112.0(6) . . ? F3A C14A C11 116.0(5) . . ? F2A C14A C11 110.0(4) . . ? F3B C14B F2B 105.6(11) . . ? F3B C14B F1B 103.9(10) . . ? F2B C14B F1B 106.1(11) . . ? F3B C14B C11 117.8(13) . . ? F2B C14B C11 108.3(11) . . ? F1B C14B C11 114.3(11) . . ? O1 B1 O2A 102.0(5) . . ? O1 B1 O2B 115.1(4) . . ? O1 B1 C7 126.3(4) . . ? O2A B1 C7 123.2(4) . . ? O2B B1 C7 113.6(5) . . ? B2 O3 C15 106.7(3) . . ? B2 O4 C16 107.2(3) . . ? B3 O6 C22 104.8(3) . . ? B3 O5 C21 105.4(3) . . ? O3 C15 C17 106.2(3) . . ? O3 C15 C18 108.6(3) . . ? C17 C15 C18 110.5(4) . . ? O3 C15 C16 102.2(3) . . ? C17 C15 C16 113.8(4) . . ? C18 C15 C16 114.7(4) . . ? O4 C16 C19 108.0(3) . . ? O4 C16 C20 105.8(3) . . ? C19 C16 C20 110.8(4) . . ? O4 C16 C15 102.2(3) . . ? C19 C16 C15 114.8(3) . . ? C20 C16 C15 114.2(4) . . ? C23 C22 C21 122.2(3) . . ? C23 C22 O6 128.5(3) . . ? C21 C22 O6 109.3(3) . . ? C26 C21 C22 122.5(4) . . ? C26 C21 O5 128.7(3) . . ? C22 C21 O5 108.7(3) . . ? C21 C26 C25 116.0(4) . . ? C24 C25 C26 121.3(4) . . ? C25 C24 C23 121.9(4) . . ? C22 C23 C24 116.1(4) . . ? C28 C27 C29 122.9(3) . . ? C28 C27 B2 123.2(3) . . ? C29 C27 B2 113.8(3) . . ? C27 C28 C36 122.0(3) . . ? C27 C28 B3 121.1(3) . . ? C36 C28 B3 116.9(3) . . ? C34 C29 C30 118.6(3) . . ? C34 C29 C27 119.7(3) . . ? C30 C29 C27 121.7(3) . . ? C31 C30 C29 120.6(3) . . ? C32 C31 C30 119.8(3) . . ? C31 C32 C33 120.7(3) . . ? C31 C32 C35 119.4(3) . . ? C33 C32 C35 119.9(3) . . ? C32 C33 C34 119.3(3) . . ? C33 C34 C29 121.0(3) . . ? F5A C35 F6A 109.5(5) . . ? F6B C35 F4B 108.6 . . ? F5C C35 F4C 109.7 . . ? F5C C35 F6C 107.2 . . ? F4C C35 F6C 105.3 . . ? F5A C35 F4A 105.6(6) . . ? F6A C35 F4A 103.7(4) . . ? F6B C35 F5B 101.5 . . ? F4B C35 F5B 100.5 . . ? F5A C35 C32 112.7(4) . . ? F5C C35 C32 114.94(19) . . ? F6B C35 C32 117.36(19) . . ? F6A C35 C32 115.3(4) . . ? F4B C35 C32 117.3(2) . . ? F4C C35 C32 108.9(2) . . ? F6C C35 C32 110.3(2) . . ? F4A C35 C32 109.3(4) . . ? F5B C35 C32 109.0(2) . . ? C41 C36 C37 118.7(3) . . ? C41 C36 C28 121.4(3) . . ? C37 C36 C28 120.0(3) . . ? C38 C37 C36 121.3(3) . . ? C37 C38 C39 119.5(3) . . ? C38 C39 C40 120.2(3) . . ? C38 C39 C42 118.4(3) . . ? C40 C39 C42 121.4(3) . . ? C39 C40 C41 119.9(3) . . ? C36 C41 C40 120.3(3) . . ? F7B C42 F8B 109.4(17) . . ? F7B C42 F9B 105.5(17) . . ? F8B C42 F9B 104.6(15) . . ? F7A C42 F9A 106.8(4) . . ? F7A C42 F8A 105.6(4) . . ? F9A C42 F8A 104.3(4) . . ? F7B C42 C39 111.8(12) . . ? F8B C42 C39 114.9(11) . . ? F7A C42 C39 113.3(3) . . ? F9B C42 C39 110.0(11) . . ? F9A C42 C39 113.0(3) . . ? F8A C42 C39 113.2(4) . . ? O4 B2 O3 114.0(3) . . ? O4 B2 C27 122.4(3) . . ? O3 B2 C27 123.2(3) . . ? O5 B3 O6 111.8(3) . . ? O5 B3 C28 125.2(3) . . ? O6 B3 C28 122.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.675 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.060