# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name C.Richards _publ_contact_author_email Chris.Richards@uea.ac.uk _publ_author_name C.Richards data_04src0348 _database_code_depnum_ccdc_archive 'CCDC 889207' #TrackingRef '- Compound 8a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H50 Co O5 P' _chemical_formula_weight 868.84 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4703(6) _cell_length_b 13.2242(7) _cell_length_c 14.7781(7) _cell_angle_alpha 98.752(2) _cell_angle_beta 110.602(3) _cell_angle_gamma 97.307(3) _cell_volume 2211.20(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22469 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8788 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44729 _diffrn_reflns_av_R_equivalents 0.1552 _diffrn_reflns_av_sigmaI/netI 0.1763 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10080 _reflns_number_gt 5211 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. In the asymmetric unit all the solvent molecules (ethyl acetate) are disordered, one over the iversion centre. As a result of this various geometrical (SAME) and thermal (DELU, SIMU) restraints have been used on these disordered atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0057(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10080 _refine_ls_number_parameters 634 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.1706 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.026 _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 Co1 Co 0.00935(4) 0.76788(4) 0.84034(4) 0.02250(17) Uani 1 1 d . . . C1 C -0.2620(3) 0.3696(3) 0.7147(3) 0.0274(9) Uani 1 1 d . . . C2 C -0.2940(3) 0.4251(3) 0.7944(3) 0.0272(9) Uani 1 1 d . . . C3 C -0.2433(3) 0.5268(3) 0.8490(3) 0.0235(8) Uani 1 1 d . . . C4 C -0.1469(3) 0.5956(3) 0.8375(3) 0.0221(8) Uani 1 1 d . . . C5 C -0.0490(3) 0.5538(3) 0.8228(3) 0.0219(8) Uani 1 1 d . . . C6 C -0.0492(3) 0.4390(3) 0.8110(3) 0.0298(9) Uani 1 1 d . . . H6 H 0.0213 0.4297 0.7956 0.036 Uiso 1 1 calc R . . C7 C -0.1407(3) 0.6991(3) 0.8385(3) 0.0224(8) Uani 1 1 d . . . C8 C 0.0332(3) 0.6249(3) 0.8151(3) 0.0209(8) Uani 1 1 d . . . C9 C -0.0375(4) 0.3905(4) 0.8961(3) 0.0487(12) Uani 1 1 d . . . H9A H -0.0948 0.4091 0.9240 0.073 Uiso 1 1 calc R . . H9B H 0.0415 0.4154 0.9466 0.073 Uiso 1 1 calc R . . H9C H -0.0514 0.3145 0.8747 0.073 Uiso 1 1 calc R . . C10 C -0.3864(3) 0.3673(3) 0.8092(3) 0.0356(10) Uani 1 1 d . . . H10 H -0.4210 0.2988 0.7705 0.043 Uiso 1 1 calc R . . C11 C -0.4279(4) 0.4082(3) 0.8790(3) 0.0393(11) Uani 1 1 d . . . H11 H -0.4906 0.3683 0.8885 0.047 Uiso 1 1 calc R . . C12 C -0.3771(3) 0.5079(3) 0.9352(3) 0.0347(10) Uani 1 1 d . . . H12 H -0.4040 0.5366 0.9843 0.042 Uiso 1 1 calc R . . C13 C -0.2874(3) 0.5655(3) 0.9198(3) 0.0287(9) Uani 1 1 d . . . H13 H -0.2541 0.6341 0.9586 0.034 Uiso 1 1 calc R . . C14 C -0.2406(3) 0.7518(3) 0.8335(3) 0.0229(8) Uani 1 1 d . . . C15 C -0.3465(3) 0.7162(3) 0.7519(3) 0.0284(9) Uani 1 1 d . . . H15 H -0.3525 0.6595 0.7013 0.034 Uiso 1 1 calc R . . C16 C -0.4422(3) 0.7618(3) 0.7436(3) 0.0385(11) Uani 1 1 d . . . H16 H -0.5134 0.7351 0.6884 0.046 Uiso 1 1 calc R . . C17 C -0.4352(4) 0.8459(3) 0.8148(3) 0.0423(11) Uani 1 1 d . . . H17 H -0.5007 0.8781 0.8082 0.051 Uiso 1 1 calc R . . C18 C -0.3320(3) 0.8826(3) 0.8957(3) 0.0375(11) Uani 1 1 d . . . H18 H -0.3266 0.9398 0.9455 0.045 Uiso 1 1 calc R . . C19 C -0.2363(3) 0.8366(3) 0.9047(3) 0.0294(9) Uani 1 1 d . . . H19 H -0.1658 0.8632 0.9607 0.035 Uiso 1 1 calc R . . C20 C 0.1344(3) 0.5973(3) 0.7921(3) 0.0220(8) Uani 1 1 d . . . C21 C 0.1207(3) 0.5562(3) 0.6950(3) 0.0257(9) Uani 1 1 d . . . H21 H 0.0455 0.5435 0.6438 0.031 Uiso 1 1 calc R . . C22 C 0.2147(3) 0.5335(3) 0.6720(3) 0.0308(10) Uani 1 1 d . . . H22 H 0.2033 0.5061 0.6053 0.037 Uiso 1 1 calc R . . C23 C 0.3250(3) 0.5504(3) 0.7452(3) 0.0343(10) Uani 1 1 d . . . H23 H 0.3895 0.5350 0.7293 0.041 Uiso 1 1 calc R . . C24 C 0.3396(3) 0.5897(3) 0.8411(3) 0.0377(11) Uani 1 1 d . . . H24 H 0.4149 0.6012 0.8920 0.045 Uiso 1 1 calc R . . C25 C 0.2462(3) 0.6130(3) 0.8650(3) 0.0316(10) Uani 1 1 d . . . H25 H 0.2585 0.6401 0.9319 0.038 Uiso 1 1 calc R . . O1 O -0.1491(2) 0.38141(19) 0.72230(19) 0.0314(7) Uani 1 1 d . . . O2 O -0.3338(2) 0.3112(2) 0.6414(2) 0.0361(7) Uani 1 1 d . . . C26 C 0.0528(3) 0.8443(3) 0.9867(3) 0.0270(9) Uani 1 1 d . . . H26 H 0.0097 0.8293 1.0264 0.032 Uiso 1 1 calc R . . C27 C 0.0344(3) 0.9174(3) 0.9250(3) 0.0276(9) Uani 1 1 d . . . H27 H -0.0236 0.9592 0.9149 0.033 Uiso 1 1 calc R . . C28 C 0.1186(3) 0.9165(3) 0.8812(3) 0.0269(9) Uani 1 1 d . . . H28 H 0.1276 0.9587 0.8367 0.032 Uiso 1 1 calc R . . C29 C 0.1864(3) 0.8430(3) 0.9142(3) 0.0269(9) Uani 1 1 d . . . H29 H 0.2490 0.8267 0.8958 0.032 Uiso 1 1 calc R . . C30 C 0.1458(3) 0.7974(3) 0.9796(3) 0.0289(9) Uani 1 1 d . . . H30 H 0.1756 0.7448 1.0127 0.035 Uiso 1 1 calc R . . C31 C 0.0387(3) 0.7628(3) 0.6194(3) 0.0234(8) Uani 1 1 d . . . C32 C 0.1567(3) 0.8092(3) 0.6658(3) 0.0286(9) Uani 1 1 d . . . H32 H 0.1853 0.8497 0.7313 0.034 Uiso 1 1 calc R . . C33 C 0.2322(3) 0.7972(3) 0.6178(3) 0.0309(10) Uani 1 1 d . . . H33 H 0.3120 0.8306 0.6499 0.037 Uiso 1 1 calc R . . C34 C 0.1930(3) 0.7372(3) 0.5236(3) 0.0319(10) Uani 1 1 d . . . H34 H 0.2458 0.7276 0.4912 0.038 Uiso 1 1 calc R . . C35 C 0.0765(3) 0.6910(3) 0.4765(3) 0.0291(9) Uani 1 1 d . . . H35 H 0.0492 0.6499 0.4113 0.035 Uiso 1 1 calc R . . C36 C -0.0005(3) 0.7038(3) 0.5229(3) 0.0280(9) Uani 1 1 d . . . H36 H -0.0807 0.6724 0.4893 0.034 Uiso 1 1 calc R . . C37 C -0.0892(3) 0.9111(3) 0.6737(3) 0.0257(9) Uani 1 1 d . . . C38 C -0.1606(3) 0.9524(3) 0.7188(3) 0.0332(10) Uani 1 1 d . . . H38 H -0.1943 0.9117 0.7533 0.040 Uiso 1 1 calc R . . C39 C -0.1823(4) 1.0516(3) 0.7137(3) 0.0411(11) Uani 1 1 d . . . H39 H -0.2299 1.0791 0.7454 0.049 Uiso 1 1 calc R . . C40 C -0.1349(4) 1.1108(4) 0.6628(3) 0.0478(12) Uani 1 1 d . . . H40 H -0.1497 1.1792 0.6596 0.057 Uiso 1 1 calc R . . C41 C -0.0662(4) 1.0711(3) 0.6166(3) 0.0447(12) Uani 1 1 d . . . H41 H -0.0344 1.1118 0.5810 0.054 Uiso 1 1 calc R . . C42 C -0.0434(3) 0.9722(3) 0.6217(3) 0.0333(10) Uani 1 1 d . . . H42 H 0.0040 0.9454 0.5894 0.040 Uiso 1 1 calc R . . C43 C -0.1964(3) 0.6966(3) 0.5996(3) 0.0254(9) Uani 1 1 d . . . C44 C -0.2847(3) 0.7363(3) 0.5364(3) 0.0346(10) Uani 1 1 d . . . H44 H -0.2747 0.8094 0.5394 0.041 Uiso 1 1 calc R . . C45 C -0.3865(3) 0.6719(4) 0.4694(3) 0.0402(11) Uani 1 1 d . . . H45 H -0.4458 0.7007 0.4271 0.048 Uiso 1 1 calc R . . C46 C -0.4024(3) 0.5654(4) 0.4638(3) 0.0365(11) Uani 1 1 d . . . H46 H -0.4721 0.5208 0.4172 0.044 Uiso 1 1 calc R . . C47 C -0.3159(3) 0.5241(3) 0.5265(3) 0.0304(10) Uani 1 1 d . . . H47 H -0.3266 0.4511 0.5234 0.036 Uiso 1 1 calc R . . C48 C -0.2140(3) 0.5891(3) 0.5936(3) 0.0280(9) Uani 1 1 d . . . H48 H -0.1551 0.5601 0.6362 0.034 Uiso 1 1 calc R . . P1 P -0.06002(8) 0.78009(8) 0.68559(7) 0.0231(2) Uani 1 1 d . . . C51 C 0.5201(9) 0.1286(13) 0.9412(11) 0.059(4) Uani 0.67(2) 1 d PDU A 1 H51A H 0.5336 0.0808 0.9868 0.089 Uiso 0.67(2) 1 calc PR A 1 H51B H 0.5435 0.2008 0.9790 0.089 Uiso 0.67(2) 1 calc PR A 1 H51C H 0.5663 0.1180 0.9001 0.089 Uiso 0.67(2) 1 calc PR A 1 C52 C 0.3957(8) 0.1079(8) 0.8775(9) 0.046(3) Uani 0.67(2) 1 d PDU A 1 C53 C 0.2311(11) 0.1858(9) 0.8057(15) 0.100(6) Uani 0.67(2) 1 d PDU A 1 H53A H 0.1855 0.1632 0.8446 0.120 Uiso 0.67(2) 1 calc PR A 1 H53B H 0.2074 0.1320 0.7442 0.120 Uiso 0.67(2) 1 calc PR A 1 C54 C 0.2066(10) 0.2852(7) 0.7812(12) 0.084(5) Uani 0.67(2) 1 d PDU A 1 H54A H 0.2299 0.3382 0.8422 0.126 Uiso 0.67(2) 1 calc PR A 1 H54B H 0.1228 0.2777 0.7432 0.126 Uiso 0.67(2) 1 calc PR A 1 H54C H 0.2506 0.3066 0.7416 0.126 Uiso 0.67(2) 1 calc PR A 1 O51 O 0.3387(6) 0.0225(6) 0.8477(5) 0.044(2) Uani 0.67(2) 1 d PDU A 1 O52 O 0.3542(10) 0.1962(7) 0.8624(10) 0.072(3) Uani 0.67(2) 1 d PDU A 1 C151 C 0.527(2) 0.146(3) 0.947(3) 0.097(12) Uani 0.33(2) 1 d PDU A 2 H15A H 0.5200 0.1908 1.0032 0.146 Uiso 0.33(2) 1 calc PR A 2 H15B H 0.5783 0.1869 0.9224 0.146 Uiso 0.33(2) 1 calc PR A 2 H15C H 0.5608 0.0868 0.9683 0.146 Uiso 0.33(2) 1 calc PR A 2 C152 C 0.413(3) 0.109(2) 0.869(3) 0.111(11) Uani 0.33(2) 1 d PDU A 2 C153 C 0.248(2) 0.162(2) 0.757(3) 0.109(11) Uani 0.33(2) 1 d PDU A 2 H15D H 0.1911 0.1442 0.7876 0.130 Uiso 0.33(2) 1 calc PR A 2 H15E H 0.2387 0.1036 0.7031 0.130 Uiso 0.33(2) 1 calc PR A 2 C154 C 0.234(2) 0.259(3) 0.721(3) 0.112(12) Uani 0.33(2) 1 d PDU A 2 H15F H 0.2220 0.3101 0.7701 0.167 Uiso 0.33(2) 1 calc PR A 2 H15G H 0.1656 0.2440 0.6587 0.167 Uiso 0.33(2) 1 calc PR A 2 H15H H 0.3037 0.2863 0.7099 0.167 Uiso 0.33(2) 1 calc PR A 2 O151 O 0.353(3) 0.027(2) 0.842(3) 0.204(16) Uani 0.33(2) 1 d PDU A 2 O152 O 0.366(2) 0.187(2) 0.830(3) 0.112(9) Uani 0.33(2) 1 d PDU A 2 C61 C 0.304(2) 0.075(3) 0.617(2) 0.335(16) Uani 0.50 1 d PDU B -1 H61A H 0.2988 0.0607 0.6782 0.502 Uiso 0.50 1 calc PR B -1 H61B H 0.2441 0.0244 0.5602 0.502 Uiso 0.50 1 calc PR B -1 H61C H 0.2917 0.1456 0.6109 0.502 Uiso 0.50 1 calc PR B -1 C62 C 0.4178(16) 0.0650(11) 0.6168(13) 0.117(6) Uani 0.50 1 d PDU B -1 C63 C 0.502(2) -0.048(2) 0.519(2) 0.215(12) Uani 0.50 1 d PDU B -1 H63A H 0.4620 -0.1184 0.5162 0.258 Uiso 0.50 1 calc PR B -1 H63B H 0.5813 -0.0321 0.5713 0.258 Uiso 0.50 1 calc PR B -1 C64 C 0.506(2) -0.038(3) 0.4216(17) 0.261(16) Uani 0.50 1 d PDU B -1 H64A H 0.5548 -0.0840 0.4046 0.391 Uiso 0.50 1 calc PR B -1 H64B H 0.5401 0.0348 0.4251 0.391 Uiso 0.50 1 calc PR B -1 H64C H 0.4271 -0.0564 0.3709 0.391 Uiso 0.50 1 calc PR B -1 O61 O 0.4955(15) 0.0692(16) 0.6783(12) 0.230(8) Uani 0.50 1 d PDU B -1 O62 O 0.4362(16) 0.029(2) 0.5326(12) 0.232(9) Uani 0.50 1 d PDU B -1 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 0.0211(3) 0.0216(3) 0.0240(3) 0.0036(2) 0.0083(2) 0.0037(2) C1 0.028(2) 0.024(2) 0.031(2) 0.0078(19) 0.011(2) 0.0028(18) C2 0.021(2) 0.030(2) 0.027(2) 0.0038(18) 0.0055(18) 0.0028(18) C3 0.0205(19) 0.025(2) 0.025(2) 0.0068(17) 0.0069(17) 0.0069(17) C4 0.0199(19) 0.024(2) 0.023(2) 0.0062(17) 0.0074(17) 0.0063(16) C5 0.0192(19) 0.023(2) 0.020(2) 0.0029(16) 0.0026(16) 0.0070(16) C6 0.020(2) 0.025(2) 0.036(2) 0.0044(19) 0.0037(19) -0.0001(17) C7 0.0197(19) 0.026(2) 0.019(2) 0.0044(17) 0.0048(16) 0.0061(17) C8 0.0200(19) 0.022(2) 0.018(2) 0.0060(16) 0.0025(16) 0.0056(16) C9 0.051(3) 0.046(3) 0.046(3) 0.013(2) 0.012(2) 0.012(2) C10 0.029(2) 0.034(3) 0.038(3) 0.007(2) 0.009(2) 0.0015(19) C11 0.031(2) 0.042(3) 0.048(3) 0.015(2) 0.018(2) 0.003(2) C12 0.033(2) 0.040(3) 0.038(3) 0.015(2) 0.017(2) 0.012(2) C13 0.031(2) 0.029(2) 0.029(2) 0.0103(18) 0.0131(19) 0.0078(19) C14 0.025(2) 0.019(2) 0.027(2) 0.0089(17) 0.0118(18) 0.0050(17) C15 0.026(2) 0.030(2) 0.033(2) 0.0047(19) 0.0162(19) 0.0054(18) C16 0.019(2) 0.048(3) 0.044(3) 0.009(2) 0.007(2) 0.007(2) C17 0.032(2) 0.044(3) 0.051(3) 0.002(2) 0.016(2) 0.017(2) C18 0.036(2) 0.033(3) 0.045(3) 0.000(2) 0.019(2) 0.012(2) C19 0.024(2) 0.031(2) 0.034(2) 0.0037(19) 0.0132(19) 0.0064(18) C20 0.0183(19) 0.019(2) 0.027(2) 0.0050(17) 0.0076(17) 0.0018(16) C21 0.028(2) 0.023(2) 0.026(2) 0.0046(17) 0.0101(18) 0.0053(17) C22 0.037(2) 0.025(2) 0.037(3) 0.0068(19) 0.020(2) 0.0070(19) C23 0.032(2) 0.034(3) 0.045(3) 0.008(2) 0.023(2) 0.009(2) C24 0.025(2) 0.043(3) 0.042(3) 0.006(2) 0.010(2) 0.008(2) C25 0.024(2) 0.040(3) 0.028(2) 0.0046(19) 0.0076(19) 0.0079(19) O1 0.0253(15) 0.0270(16) 0.0367(17) -0.0005(13) 0.0090(13) 0.0037(12) O2 0.0245(15) 0.0401(18) 0.0319(17) -0.0066(14) 0.0054(14) -0.0026(13) C26 0.027(2) 0.026(2) 0.024(2) -0.0013(18) 0.0097(18) -0.0007(18) C27 0.028(2) 0.024(2) 0.028(2) 0.0003(18) 0.0101(19) 0.0045(18) C28 0.027(2) 0.021(2) 0.025(2) -0.0018(17) 0.0063(18) -0.0032(17) C29 0.024(2) 0.025(2) 0.026(2) -0.0015(18) 0.0075(18) 0.0006(17) C30 0.027(2) 0.028(2) 0.024(2) 0.0023(18) 0.0018(18) 0.0021(18) C31 0.025(2) 0.019(2) 0.029(2) 0.0099(17) 0.0109(18) 0.0084(17) C32 0.027(2) 0.030(2) 0.024(2) 0.0024(18) 0.0064(19) 0.0031(18) C33 0.023(2) 0.036(2) 0.038(3) 0.012(2) 0.014(2) 0.0074(18) C34 0.035(2) 0.034(2) 0.038(3) 0.013(2) 0.022(2) 0.014(2) C35 0.042(3) 0.024(2) 0.024(2) 0.0047(18) 0.015(2) 0.0070(19) C36 0.026(2) 0.024(2) 0.032(2) 0.0072(18) 0.0092(19) 0.0014(17) C37 0.023(2) 0.024(2) 0.030(2) 0.0088(18) 0.0085(18) 0.0055(17) C38 0.039(2) 0.031(2) 0.039(3) 0.017(2) 0.019(2) 0.014(2) C39 0.046(3) 0.039(3) 0.049(3) 0.013(2) 0.025(2) 0.021(2) C40 0.070(3) 0.034(3) 0.051(3) 0.020(2) 0.029(3) 0.023(2) C41 0.060(3) 0.035(3) 0.055(3) 0.021(2) 0.034(3) 0.014(2) C42 0.038(2) 0.030(2) 0.035(3) 0.009(2) 0.015(2) 0.012(2) C43 0.020(2) 0.034(2) 0.022(2) 0.0061(18) 0.0076(17) 0.0034(17) C44 0.027(2) 0.038(3) 0.037(3) 0.013(2) 0.010(2) 0.005(2) C45 0.026(2) 0.057(3) 0.033(3) 0.017(2) 0.002(2) 0.008(2) C46 0.028(2) 0.049(3) 0.026(2) 0.003(2) 0.009(2) -0.003(2) C47 0.029(2) 0.037(3) 0.025(2) 0.0029(19) 0.014(2) -0.0016(19) C48 0.023(2) 0.032(2) 0.029(2) 0.0071(19) 0.0101(19) 0.0038(18) P1 0.0218(5) 0.0225(6) 0.0254(6) 0.0063(4) 0.0089(5) 0.0048(4) C51 0.036(5) 0.058(8) 0.073(8) 0.026(6) 0.010(5) -0.013(5) C52 0.030(4) 0.045(5) 0.063(6) 0.030(5) 0.014(4) -0.002(4) C53 0.044(5) 0.065(7) 0.151(14) 0.042(8) -0.017(7) 0.002(5) C54 0.055(6) 0.053(6) 0.112(10) 0.028(6) -0.010(7) 0.009(5) O51 0.025(3) 0.048(4) 0.057(4) 0.021(3) 0.011(3) -0.002(3) O52 0.044(4) 0.050(4) 0.103(7) 0.040(4) 0.000(4) -0.008(3) C151 0.067(16) 0.050(16) 0.14(3) 0.023(15) -0.009(13) 0.039(12) C152 0.082(15) 0.059(12) 0.141(18) 0.018(13) -0.014(13) 0.007(11) C153 0.063(12) 0.093(15) 0.118(19) 0.060(13) -0.029(13) -0.026(11) C154 0.064(13) 0.13(2) 0.14(2) 0.11(2) 0.010(15) 0.001(13) O151 0.17(2) 0.085(13) 0.25(3) -0.005(17) -0.01(2) -0.039(14) O152 0.051(10) 0.117(11) 0.133(16) 0.059(11) -0.016(10) 0.006(8) C61 0.22(2) 0.43(4) 0.38(4) 0.13(3) 0.13(2) 0.08(3) C62 0.156(14) 0.037(8) 0.130(14) 0.028(9) 0.018(11) 0.018(9) C63 0.082(12) 0.31(3) 0.20(2) -0.08(2) 0.041(15) 0.026(19) C64 0.17(3) 0.38(4) 0.15(2) 0.02(3) -0.046(18) 0.14(3) O61 0.199(15) 0.28(2) 0.172(12) 0.100(15) 0.019(12) -0.011(15) O62 0.193(16) 0.249(17) 0.159(13) -0.029(14) -0.033(11) 0.090(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C8 1.952(4) . ? Co1 C7 1.963(4) . ? Co1 C26 2.089(4) . ? Co1 C27 2.095(4) . ? Co1 C30 2.099(4) . ? Co1 C28 2.112(4) . ? Co1 C29 2.114(4) . ? Co1 P1 2.1818(11) . ? C1 O2 1.207(4) . ? C1 O1 1.358(4) . ? C1 C2 1.492(5) . ? C2 C3 1.398(5) . ? C2 C10 1.402(5) . ? C3 C13 1.404(5) . ? C3 C4 1.489(5) . ? C4 C7 1.358(5) . ? C4 C5 1.471(5) . ? C5 C8 1.347(5) . ? C5 C6 1.502(5) . ? C6 C9 1.468(6) . ? C6 O1 1.468(4) . ? C6 H6 1.0000 . ? C7 C14 1.489(5) . ? C8 C20 1.492(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.380(5) . ? C10 H10 0.9500 . ? C11 C12 1.384(6) . ? C11 H11 0.9500 . ? C12 C13 1.377(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.397(5) . ? C14 C15 1.403(5) . ? C15 C16 1.379(5) . ? C15 H15 0.9500 . ? C16 C17 1.381(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.382(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.396(5) . ? C20 C25 1.396(5) . ? C21 C22 1.385(5) . ? C21 H21 0.9500 . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(5) . ? C23 H23 0.9500 . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C30 1.410(5) . ? C26 C27 1.412(5) . ? C26 H26 0.9500 . ? C27 C28 1.415(5) . ? C27 H27 0.9500 . ? C28 C29 1.400(5) . ? C28 H28 0.9500 . ? C29 C30 1.414(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.395(5) . ? C31 C36 1.398(5) . ? C31 P1 1.837(3) . ? C32 C33 1.373(5) . ? C32 H32 0.9500 . ? C33 C34 1.377(5) . ? C33 H33 0.9500 . ? C34 C35 1.378(5) . ? C34 H34 0.9500 . ? C35 C36 1.376(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.396(5) . ? C37 C38 1.403(5) . ? C37 P1 1.836(4) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.381(6) . ? C39 H39 0.9500 . ? C40 C41 1.376(6) . ? C40 H40 0.9500 . ? C41 C42 1.381(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.391(5) . ? C43 C48 1.394(5) . ? C43 P1 1.817(4) . ? C44 C45 1.379(6) . ? C44 H44 0.9500 . ? C45 C46 1.382(6) . ? C45 H45 0.9500 . ? C46 C47 1.386(6) . ? C46 H46 0.9500 . ? C47 C48 1.383(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C51 C52 1.467(9) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O51 1.183(8) . ? C52 O52 1.353(9) . ? C53 O52 1.444(9) . ? C53 C54 1.458(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C151 C152 1.452(16) . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C152 O151 1.155(15) . ? C152 O152 1.358(15) . ? C153 O152 1.437(15) . ? C153 C154 1.462(16) . ? C153 H15D 0.9900 . ? C153 H15E 0.9900 . ? C154 H15F 0.9800 . ? C154 H15G 0.9800 . ? C154 H15H 0.9800 . ? C61 C62 1.440(16) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 O61 1.057(14) . ? C62 O62 1.369(16) . ? C63 O62 1.424(17) . ? C63 C64 1.481(18) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 C8 Co1 C7 83.13(15) . . ? C8 Co1 C26 118.41(15) . . ? C7 Co1 C26 89.40(14) . . ? C8 Co1 C27 155.82(15) . . ? C7 Co1 C27 102.68(14) . . ? C26 Co1 C27 39.45(14) . . ? C8 Co1 C30 89.75(15) . . ? C7 Co1 C30 113.56(15) . . ? C26 Co1 C30 39.37(14) . . ? C27 Co1 C30 66.32(15) . . ? C8 Co1 C28 134.37(14) . . ? C7 Co1 C28 141.09(14) . . ? C26 Co1 C28 65.52(14) . . ? C27 Co1 C28 39.31(13) . . ? C30 Co1 C28 65.56(15) . . ? C8 Co1 C29 98.23(15) . . ? C7 Co1 C29 152.42(15) . . ? C26 Co1 C29 65.58(14) . . ? C27 Co1 C29 65.81(14) . . ? C30 Co1 C29 39.22(14) . . ? C28 Co1 C29 38.70(14) . . ? C8 Co1 P1 96.04(11) . . ? C7 Co1 P1 94.80(11) . . ? C26 Co1 P1 145.55(11) . . ? C27 Co1 P1 106.69(11) . . ? C30 Co1 P1 151.56(11) . . ? C28 Co1 P1 91.29(11) . . ? C29 Co1 P1 112.34(11) . . ? O2 C1 O1 116.7(3) . . ? O2 C1 C2 122.2(3) . . ? O1 C1 C2 121.1(3) . . ? C3 C2 C10 120.4(3) . . ? C3 C2 C1 125.7(3) . . ? C10 C2 C1 113.8(4) . . ? C2 C3 C13 116.8(3) . . ? C2 C3 C4 124.7(3) . . ? C13 C3 C4 118.5(3) . . ? C7 C4 C5 114.4(3) . . ? C7 C4 C3 124.6(3) . . ? C5 C4 C3 121.0(3) . . ? C8 C5 C4 114.8(3) . . ? C8 C5 C6 124.7(3) . . ? C4 C5 C6 120.5(3) . . ? C9 C6 O1 111.6(3) . . ? C9 C6 C5 118.9(3) . . ? O1 C6 C5 109.8(3) . . ? C9 C6 H6 105.1 . . ? O1 C6 H6 105.1 . . ? C5 C6 H6 105.1 . . ? C4 C7 C14 122.6(3) . . ? C4 C7 Co1 112.9(2) . . ? C14 C7 Co1 124.4(3) . . ? C5 C8 C20 123.2(3) . . ? C5 C8 Co1 113.6(2) . . ? C20 C8 Co1 123.1(3) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C2 121.1(4) . . ? C11 C10 H10 119.5 . . ? C2 C10 H10 119.5 . . ? C10 C11 C12 119.2(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C3 122.6(4) . . ? C12 C13 H13 118.7 . . ? C3 C13 H13 118.7 . . ? C19 C14 C15 116.8(3) . . ? C19 C14 C7 124.4(3) . . ? C15 C14 C7 118.9(3) . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 119.2(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 120.4(4) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 121.6(4) . . ? C18 C19 H19 119.2 . . ? C14 C19 H19 119.2 . . ? C21 C20 C25 117.2(3) . . ? C21 C20 C8 120.6(3) . . ? C25 C20 C8 122.1(3) . . ? C22 C21 C20 121.2(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 118.8(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.1(4) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C20 121.0(4) . . ? C24 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? C1 O1 C6 124.0(3) . . ? C30 C26 C27 108.7(3) . . ? C30 C26 Co1 70.7(2) . . ? C27 C26 Co1 70.5(2) . . ? C30 C26 H26 125.6 . . ? C27 C26 H26 125.6 . . ? Co1 C26 H26 124.8 . . ? C26 C27 C28 107.1(3) . . ? C26 C27 Co1 70.1(2) . . ? C28 C27 Co1 71.0(2) . . ? C26 C27 H27 126.5 . . ? C28 C27 H27 126.5 . . ? Co1 C27 H27 124.1 . . ? C29 C28 C27 108.6(3) . . ? C29 C28 Co1 70.7(2) . . ? C27 C28 Co1 69.7(2) . . ? C29 C28 H28 125.7 . . ? C27 C28 H28 125.7 . . ? Co1 C28 H28 125.5 . . ? C28 C29 C30 108.2(3) . . ? C28 C29 Co1 70.6(2) . . ? C30 C29 Co1 69.8(2) . . ? C28 C29 H29 125.9 . . ? C30 C29 H29 125.9 . . ? Co1 C29 H29 125.3 . . ? C26 C30 C29 107.4(3) . . ? C26 C30 Co1 69.9(2) . . ? C29 C30 Co1 71.0(2) . . ? C26 C30 H30 126.3 . . ? C29 C30 H30 126.3 . . ? Co1 C30 H30 124.4 . . ? C32 C31 C36 118.2(3) . . ? C32 C31 P1 119.8(3) . . ? C36 C31 P1 122.0(3) . . ? C33 C32 C31 120.8(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.5(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 120.7(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 120.3(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C37 C38 118.1(3) . . ? C42 C37 P1 123.1(3) . . ? C38 C37 P1 118.8(3) . . ? C39 C38 C37 120.7(4) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 120.1(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.2(4) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.8(4) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C44 C43 C48 117.9(4) . . ? C44 C43 P1 121.8(3) . . ? C48 C43 P1 120.3(3) . . ? C45 C44 C43 121.3(4) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C44 C45 C46 120.1(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 119.6(4) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C48 C47 C46 120.1(4) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C43 121.0(4) . . ? C47 C48 H48 119.5 . . ? C43 C48 H48 119.5 . . ? C43 P1 C37 102.31(17) . . ? C43 P1 C31 102.42(16) . . ? C37 P1 C31 102.83(16) . . ? C43 P1 Co1 120.37(13) . . ? C37 P1 Co1 111.30(12) . . ? C31 P1 Co1 115.45(12) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O51 C52 O52 125.0(8) . . ? O51 C52 C51 122.1(9) . . ? O52 C52 C51 112.8(8) . . ? O52 C53 C54 109.9(9) . . ? O52 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? O52 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 O52 C53 117.8(8) . . ? C152 C151 H15A 109.5 . . ? C152 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C152 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? O151 C152 O152 117(2) . . ? O151 C152 C151 130(2) . . ? O152 C152 C151 112.5(18) . . ? O152 C153 C154 103.5(17) . . ? O152 C153 H15D 111.1 . . ? C154 C153 H15D 111.1 . . ? O152 C153 H15E 111.1 . . ? C154 C153 H15E 111.1 . . ? H15D C153 H15E 109.0 . . ? C153 C154 H15F 109.5 . . ? C153 C154 H15G 109.5 . . ? H15F C154 H15G 109.5 . . ? C153 C154 H15H 109.5 . . ? H15F C154 H15H 109.5 . . ? H15G C154 H15H 109.5 . . ? C152 O152 C153 118.4(19) . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O61 C62 O62 108.2(18) . . ? O61 C62 C61 128(2) . . ? O62 C62 C61 122.7(19) . . ? O62 C63 C64 100.7(18) . . ? O62 C63 H63A 111.6 . . ? C64 C63 H63A 111.6 . . ? O62 C63 H63B 111.6 . . ? C64 C63 H63B 111.6 . . ? H63A C63 H63B 109.4 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 O62 C63 127.0(19) . . ? 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 O2 C1 C2 C3 -143.0(4) . . . . ? O1 C1 C2 C3 38.0(6) . . . . ? O2 C1 C2 C10 34.5(5) . . . . ? O1 C1 C2 C10 -144.5(4) . . . . ? C10 C2 C3 C13 1.7(5) . . . . ? C1 C2 C3 C13 179.0(3) . . . . ? C10 C2 C3 C4 -178.6(3) . . . . ? C1 C2 C3 C4 -1.3(6) . . . . ? C2 C3 C4 C7 138.9(4) . . . . ? C13 C3 C4 C7 -41.4(5) . . . . ? C2 C3 C4 C5 -40.5(5) . . . . ? C13 C3 C4 C5 139.2(4) . . . . ? C7 C4 C5 C8 1.6(5) . . . . ? C3 C4 C5 C8 -178.9(3) . . . . ? C7 C4 C5 C6 -174.5(3) . . . . ? C3 C4 C5 C6 4.9(5) . . . . ? C8 C5 C6 C9 116.0(4) . . . . ? C4 C5 C6 C9 -68.2(5) . . . . ? C8 C5 C6 O1 -113.8(4) . . . . ? C4 C5 C6 O1 62.0(4) . . . . ? C5 C4 C7 C14 168.3(3) . . . . ? C3 C4 C7 C14 -11.1(6) . . . . ? C5 C4 C7 Co1 -8.8(4) . . . . ? C3 C4 C7 Co1 171.8(3) . . . . ? C8 Co1 C7 C4 9.7(3) . . . . ? C26 Co1 C7 C4 -109.0(3) . . . . ? C27 Co1 C7 C4 -146.4(3) . . . . ? C30 Co1 C7 C4 -77.0(3) . . . . ? C28 Co1 C7 C4 -156.7(3) . . . . ? C29 Co1 C7 C4 -84.9(4) . . . . ? P1 Co1 C7 C4 105.2(3) . . . . ? C8 Co1 C7 C14 -167.3(3) . . . . ? C26 Co1 C7 C14 74.0(3) . . . . ? C27 Co1 C7 C14 36.5(3) . . . . ? C30 Co1 C7 C14 106.0(3) . . . . ? C28 Co1 C7 C14 26.2(4) . . . . ? C29 Co1 C7 C14 98.1(4) . . . . ? P1 Co1 C7 C14 -71.8(3) . . . . ? C4 C5 C8 C20 -175.0(3) . . . . ? C6 C5 C8 C20 1.0(6) . . . . ? C4 C5 C8 Co1 6.5(4) . . . . ? C6 C5 C8 Co1 -177.5(3) . . . . ? C7 Co1 C8 C5 -8.9(3) . . . . ? C26 Co1 C8 C5 76.7(3) . . . . ? C27 Co1 C8 C5 96.9(4) . . . . ? C30 Co1 C8 C5 104.9(3) . . . . ? C28 Co1 C8 C5 159.2(3) . . . . ? C29 Co1 C8 C5 143.3(3) . . . . ? P1 Co1 C8 C5 -103.0(3) . . . . ? C7 Co1 C8 C20 172.6(3) . . . . ? C26 Co1 C8 C20 -101.9(3) . . . . ? C27 Co1 C8 C20 -81.7(4) . . . . ? C30 Co1 C8 C20 -73.7(3) . . . . ? C28 Co1 C8 C20 -19.3(4) . . . . ? C29 Co1 C8 C20 -35.2(3) . . . . ? P1 Co1 C8 C20 78.4(3) . . . . ? C3 C2 C10 C11 -1.3(6) . . . . ? C1 C2 C10 C11 -178.9(4) . . . . ? C2 C10 C11 C12 -0.1(6) . . . . ? C10 C11 C12 C13 1.0(6) . . . . ? C11 C12 C13 C3 -0.6(6) . . . . ? C2 C3 C13 C12 -0.8(5) . . . . ? C4 C3 C13 C12 179.5(3) . . . . ? C4 C7 C14 C19 122.3(4) . . . . ? Co1 C7 C14 C19 -60.9(5) . . . . ? C4 C7 C14 C15 -58.6(5) . . . . ? Co1 C7 C14 C15 118.2(3) . . . . ? C19 C14 C15 C16 -1.1(5) . . . . ? C7 C14 C15 C16 179.7(3) . . . . ? C14 C15 C16 C17 1.5(6) . . . . ? C15 C16 C17 C18 -1.3(7) . . . . ? C16 C17 C18 C19 0.8(7) . . . . ? C17 C18 C19 C14 -0.4(6) . . . . ? C15 C14 C19 C18 0.6(5) . . . . ? C7 C14 C19 C18 179.7(4) . . . . ? C5 C8 C20 C21 79.3(5) . . . . ? Co1 C8 C20 C21 -102.3(4) . . . . ? C5 C8 C20 C25 -102.0(5) . . . . ? Co1 C8 C20 C25 76.4(4) . . . . ? C25 C20 C21 C22 -1.0(5) . . . . ? C8 C20 C21 C22 177.8(3) . . . . ? C20 C21 C22 C23 0.5(6) . . . . ? C21 C22 C23 C24 0.2(6) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C20 -0.1(6) . . . . ? C21 C20 C25 C24 0.8(6) . . . . ? C8 C20 C25 C24 -178.0(4) . . . . ? O2 C1 O1 C6 -172.4(3) . . . . ? C2 C1 O1 C6 6.7(5) . . . . ? C9 C6 O1 C1 62.9(4) . . . . ? C5 C6 O1 C1 -71.2(4) . . . . ? C8 Co1 C26 C30 48.2(3) . . . . ? C7 Co1 C26 C30 130.0(2) . . . . ? C27 Co1 C26 C30 -119.0(3) . . . . ? C28 Co1 C26 C30 -80.7(2) . . . . ? C29 Co1 C26 C30 -38.0(2) . . . . ? P1 Co1 C26 C30 -132.4(2) . . . . ? C8 Co1 C26 C27 167.2(2) . . . . ? C7 Co1 C26 C27 -111.0(2) . . . . ? C30 Co1 C26 C27 119.0(3) . . . . ? C28 Co1 C26 C27 38.3(2) . . . . ? C29 Co1 C26 C27 81.0(2) . . . . ? P1 Co1 C26 C27 -13.4(3) . . . . ? C30 C26 C27 C28 -1.1(4) . . . . ? Co1 C26 C27 C28 -61.7(2) . . . . ? C30 C26 C27 Co1 60.6(3) . . . . ? C8 Co1 C27 C26 -28.5(4) . . . . ? C7 Co1 C27 C26 73.1(2) . . . . ? C30 Co1 C27 C26 -37.3(2) . . . . ? C28 Co1 C27 C26 -117.1(3) . . . . ? C29 Co1 C27 C26 -80.4(2) . . . . ? P1 Co1 C27 C26 172.15(18) . . . . ? C8 Co1 C27 C28 88.5(4) . . . . ? C7 Co1 C27 C28 -169.8(2) . . . . ? C26 Co1 C27 C28 117.1(3) . . . . ? C30 Co1 C27 C28 79.8(2) . . . . ? C29 Co1 C27 C28 36.7(2) . . . . ? P1 Co1 C27 C28 -70.8(2) . . . . ? C26 C27 C28 C29 0.8(4) . . . . ? Co1 C27 C28 C29 -60.3(3) . . . . ? C26 C27 C28 Co1 61.1(3) . . . . ? C8 Co1 C28 C29 -25.7(3) . . . . ? C7 Co1 C28 C29 135.3(2) . . . . ? C26 Co1 C28 C29 80.9(2) . . . . ? C27 Co1 C28 C29 119.3(3) . . . . ? C30 Co1 C28 C29 37.5(2) . . . . ? P1 Co1 C28 C29 -125.5(2) . . . . ? C8 Co1 C28 C27 -145.1(2) . . . . ? C7 Co1 C28 C27 15.9(3) . . . . ? C26 Co1 C28 C27 -38.4(2) . . . . ? C30 Co1 C28 C27 -81.9(2) . . . . ? C29 Co1 C28 C27 -119.3(3) . . . . ? P1 Co1 C28 C27 115.2(2) . . . . ? C27 C28 C29 C30 -0.3(4) . . . . ? Co1 C28 C29 C30 -59.9(3) . . . . ? C27 C28 C29 Co1 59.6(3) . . . . ? C8 Co1 C29 C28 161.7(2) . . . . ? C7 Co1 C29 C28 -107.4(3) . . . . ? C26 Co1 C29 C28 -80.7(2) . . . . ? C27 Co1 C29 C28 -37.3(2) . . . . ? C30 Co1 C29 C28 -118.9(3) . . . . ? P1 Co1 C29 C28 61.7(2) . . . . ? C8 Co1 C29 C30 -79.4(2) . . . . ? C7 Co1 C29 C30 11.5(4) . . . . ? C26 Co1 C29 C30 38.1(2) . . . . ? C27 Co1 C29 C30 81.6(2) . . . . ? C28 Co1 C29 C30 118.9(3) . . . . ? P1 Co1 C29 C30 -179.44(19) . . . . ? C27 C26 C30 C29 0.9(4) . . . . ? Co1 C26 C30 C29 61.5(3) . . . . ? C27 C26 C30 Co1 -60.5(3) . . . . ? C28 C29 C30 C26 -0.4(4) . . . . ? Co1 C29 C30 C26 -60.8(3) . . . . ? C28 C29 C30 Co1 60.4(3) . . . . ? C8 Co1 C30 C26 -139.1(2) . . . . ? C7 Co1 C30 C26 -56.7(3) . . . . ? C27 Co1 C30 C26 37.4(2) . . . . ? C28 Co1 C30 C26 80.6(2) . . . . ? C29 Co1 C30 C26 117.6(3) . . . . ? P1 Co1 C30 C26 118.6(2) . . . . ? C8 Co1 C30 C29 103.4(2) . . . . ? C7 Co1 C30 C29 -174.2(2) . . . . ? C26 Co1 C30 C29 -117.6(3) . . . . ? C27 Co1 C30 C29 -80.2(2) . . . . ? C28 Co1 C30 C29 -37.0(2) . . . . ? P1 Co1 C30 C29 1.1(4) . . . . ? C36 C31 C32 C33 0.0(6) . . . . ? P1 C31 C32 C33 179.8(3) . . . . ? C31 C32 C33 C34 -1.4(6) . . . . ? C32 C33 C34 C35 1.5(6) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C34 C35 C36 C31 -0.9(6) . . . . ? C32 C31 C36 C35 1.1(5) . . . . ? P1 C31 C36 C35 -178.7(3) . . . . ? C42 C37 C38 C39 -1.5(6) . . . . ? P1 C37 C38 C39 178.4(3) . . . . ? C37 C38 C39 C40 0.8(7) . . . . ? C38 C39 C40 C41 0.3(7) . . . . ? C39 C40 C41 C42 -0.6(7) . . . . ? C40 C41 C42 C37 -0.1(7) . . . . ? C38 C37 C42 C41 1.2(6) . . . . ? P1 C37 C42 C41 -178.7(3) . . . . ? C48 C43 C44 C45 -0.2(6) . . . . ? P1 C43 C44 C45 178.1(3) . . . . ? C43 C44 C45 C46 -0.2(6) . . . . ? C44 C45 C46 C47 0.6(6) . . . . ? C45 C46 C47 C48 -0.6(6) . . . . ? C46 C47 C48 C43 0.1(5) . . . . ? C44 C43 C48 C47 0.3(5) . . . . ? P1 C43 C48 C47 -178.1(3) . . . . ? C44 C43 P1 C37 7.8(3) . . . . ? C48 C43 P1 C37 -173.9(3) . . . . ? C44 C43 P1 C31 -98.5(3) . . . . ? C48 C43 P1 C31 79.8(3) . . . . ? C44 C43 P1 Co1 131.7(3) . . . . ? C48 C43 P1 Co1 -49.9(3) . . . . ? C42 C37 P1 C43 -104.3(3) . . . . ? C38 C37 P1 C43 75.8(3) . . . . ? C42 C37 P1 C31 1.7(4) . . . . ? C38 C37 P1 C31 -178.3(3) . . . . ? C42 C37 P1 Co1 125.9(3) . . . . ? C38 C37 P1 Co1 -54.1(3) . . . . ? C32 C31 P1 C43 -175.0(3) . . . . ? C36 C31 P1 C43 4.8(3) . . . . ? C32 C31 P1 C37 79.1(3) . . . . ? C36 C31 P1 C37 -101.1(3) . . . . ? C32 C31 P1 Co1 -42.3(3) . . . . ? C36 C31 P1 Co1 137.5(3) . . . . ? C8 Co1 P1 C43 63.44(17) . . . . ? C7 Co1 P1 C43 -20.14(17) . . . . ? C26 Co1 P1 C43 -116.1(2) . . . . ? C27 Co1 P1 C43 -124.92(17) . . . . ? C30 Co1 P1 C43 164.2(3) . . . . ? C28 Co1 P1 C43 -161.67(17) . . . . ? C29 Co1 P1 C43 164.92(17) . . . . ? C8 Co1 P1 C37 -176.98(16) . . . . ? C7 Co1 P1 C37 99.44(16) . . . . ? C26 Co1 P1 C37 3.5(2) . . . . ? C27 Co1 P1 C37 -5.34(16) . . . . ? C30 Co1 P1 C37 -76.2(3) . . . . ? C28 Co1 P1 C37 -42.09(16) . . . . ? C29 Co1 P1 C37 -75.50(17) . . . . ? C8 Co1 P1 C31 -60.26(17) . . . . ? C7 Co1 P1 C31 -143.84(17) . . . . ? C26 Co1 P1 C31 120.2(2) . . . . ? C27 Co1 P1 C31 111.38(17) . . . . ? C30 Co1 P1 C31 40.5(3) . . . . ? C28 Co1 P1 C31 74.63(16) . . . . ? C29 Co1 P1 C31 41.22(17) . . . . ? O51 C52 O52 C53 0(2) . . . . ? C51 C52 O52 C53 -176.4(13) . . . . ? C54 C53 O52 C52 -169.2(13) . . . . ? O151 C152 O152 C153 -2(7) . . . . ? C151 C152 O152 C153 -175(4) . . . . ? C154 C153 O152 C152 -171(4) . . . . ? O61 C62 O62 C63 37(3) . . . . ? C61 C62 O62 C63 -132(3) . . . . ? C64 C63 O62 C62 -170(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.052 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.083 # Attachment '- Compound 8c.cif' data_ja388 _database_code_depnum_ccdc_archive 'CCDC 889208' #TrackingRef '- Compound 8c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H37 Co F3 O2 P' _chemical_formula_weight 804.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9334(3) _cell_length_b 13.7437(4) _cell_length_c 21.5542(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.477(2) _cell_angle_gamma 90.00 _cell_volume 3725.82(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 46002 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8235 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 44424 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8518 _reflns_number_gt 6047 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'DIRDIF08 (Beurskens et al, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0581P)^2^+4.3629P] 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 8518 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C -0.1038(3) 0.7388(2) 0.22861(16) 0.0319(7) Uani 1 1 d . . . H1 H -0.1591 0.7409 0.2509 0.038 Uiso 1 1 calc R . . C2 C -0.0005(2) 0.7789(2) 0.24893(16) 0.0295(7) Uani 1 1 d . . . H2 H 0.0254 0.8139 0.2875 0.035 Uiso 1 1 calc R . . C3 C 0.0570(3) 0.7586(2) 0.20288(15) 0.0298(7) Uani 1 1 d . . . H3 H 0.1289 0.7761 0.2053 0.036 Uiso 1 1 calc R . . C4 C -0.0101(3) 0.7075(2) 0.15205(16) 0.0339(7) Uani 1 1 d . . . H4 H 0.0078 0.6857 0.1141 0.041 Uiso 1 1 calc R . . C5 C -0.1085(3) 0.6950(2) 0.16842(15) 0.0337(7) Uani 1 1 d . . . H5 H -0.1685 0.6624 0.1432 0.040 Uiso 1 1 calc R . . C6 C 0.1502(2) 0.5697(2) 0.24018(14) 0.0219(6) Uani 1 1 d . . . C7 C 0.2131(2) 0.5625(2) 0.29953(14) 0.0227(6) Uani 1 1 d . . . C8 C 0.1632(2) 0.5885(2) 0.35200(13) 0.0211(6) Uani 1 1 d . . . C9 C 0.0594(2) 0.61673(19) 0.33242(13) 0.0201(6) Uani 1 1 d . . . C10 C 0.2255(2) 0.5846(2) 0.41953(13) 0.0217(6) Uani 1 1 d . . . C11 C 0.3002(2) 0.5113(2) 0.44411(14) 0.0241(6) Uani 1 1 d . . . C12 C 0.3239(2) 0.4247(2) 0.40770(15) 0.0276(7) Uani 1 1 d . . . C13 C 0.3267(2) 0.5280(2) 0.31384(15) 0.0320(7) Uani 1 1 d . . . H13 H 0.3413 0.5126 0.2713 0.038 Uiso 1 1 calc R . . C14 C 0.4100(3) 0.5988(3) 0.34373(18) 0.0437(9) Uani 1 1 d . . . H14A H 0.3897 0.6303 0.3799 0.066 Uiso 1 1 calc R . . H14B H 0.4175 0.6482 0.3123 0.066 Uiso 1 1 calc R . . H14C H 0.4778 0.5648 0.3587 0.066 Uiso 1 1 calc R . . C15 C 0.3603(2) 0.5150(2) 0.50703(15) 0.0303(7) Uani 1 1 d . . . H15 H 0.4088 0.4639 0.5229 0.036 Uiso 1 1 calc R . . C16 C 0.3501(3) 0.5919(3) 0.54648(16) 0.0356(8) Uani 1 1 d . . . H16 H 0.3917 0.5948 0.5890 0.043 Uiso 1 1 calc R . . C17 C 0.2775(2) 0.6651(2) 0.52244(15) 0.0327(7) Uani 1 1 d . . . H17 H 0.2709 0.7193 0.5486 0.039 Uiso 1 1 calc R . . C18 C 0.2150(2) 0.6603(2) 0.46114(14) 0.0256(6) Uani 1 1 d . . . H18 H 0.1635 0.7096 0.4468 0.031 Uiso 1 1 calc R . . C19 C -0.01305(13) 0.63065(12) 0.37775(8) 0.0214(6) Uani 1 1 d G . . C20 C -0.06064(15) 0.71957(10) 0.38425(9) 0.0278(7) Uani 1 1 d G . . H20 H -0.0455 0.7748 0.3613 0.033 Uiso 1 1 calc R . . C21 C -0.13031(15) 0.72775(11) 0.42430(10) 0.0338(7) Uani 1 1 d G . . H21 H -0.1628 0.7885 0.4287 0.041 Uiso 1 1 calc R . . C22 C -0.15239(15) 0.64700(14) 0.45784(9) 0.0328(7) Uani 1 1 d G . . H22 H -0.2000 0.6526 0.4852 0.039 Uiso 1 1 calc R . . C23 C -0.10480(15) 0.55808(11) 0.45134(9) 0.0291(7) Uani 1 1 d G . . H23 H -0.1199 0.5029 0.4743 0.035 Uiso 1 1 calc R . . C24 C -0.03513(14) 0.54991(10) 0.41129(9) 0.0239(6) Uani 1 1 d G . . H24 H -0.0026 0.4891 0.4069 0.029 Uiso 1 1 calc R . . C25 C 0.18958(16) 0.53967(12) 0.18206(8) 0.0230(6) Uani 1 1 d G . . C26 C 0.21551(16) 0.60927(9) 0.14141(9) 0.0298(7) Uani 1 1 d G . . H26 H 0.2050 0.6763 0.1486 0.036 Uiso 1 1 calc R . . C27 C 0.25684(17) 0.58071(11) 0.09022(8) 0.0288(7) Uani 1 1 d G . . H27 H 0.2746 0.6283 0.0624 0.035 Uiso 1 1 calc R . . C28 C 0.27225(16) 0.48256(13) 0.07968(8) 0.0269(7) Uani 1 1 d G . . C29 C 0.24632(17) 0.41296(9) 0.12034(9) 0.0322(7) Uani 1 1 d G . . H29 H 0.2568 0.3459 0.1131 0.039 Uiso 1 1 calc R . . C30 C 0.20498(17) 0.44152(11) 0.17153(8) 0.0301(7) Uani 1 1 d G . . H30 H 0.1873 0.3939 0.1993 0.036 Uiso 1 1 calc R . . C31 C 0.3160(3) 0.4515(2) 0.02356(15) 0.0319(7) Uani 1 1 d . . . C32 C -0.07130(18) 0.41551(13) 0.15754(8) 0.0289(7) Uani 1 1 d G . . C33 C -0.04724(19) 0.45857(11) 0.10426(9) 0.0368(8) Uani 1 1 d G . . H33 H -0.0302 0.5258 0.1048 0.044 Uiso 1 1 calc R . . C34 C -0.0481(2) 0.40318(16) 0.05019(8) 0.0498(10) Uani 1 1 d G . . H34 H -0.0316 0.4326 0.0138 0.060 Uiso 1 1 calc R . . C35 C -0.0730(2) 0.30474(15) 0.04938(9) 0.0455(9) Uani 1 1 d G . . H35 H -0.0736 0.2669 0.0124 0.055 Uiso 1 1 calc R . . C36 C -0.0971(2) 0.26168(11) 0.10265(10) 0.0437(9) Uani 1 1 d G . . H36 H -0.1141 0.1944 0.1021 0.052 Uiso 1 1 calc R . . C37 C -0.09622(19) 0.31706(13) 0.15673(8) 0.0395(8) Uani 1 1 d G . . H37 H -0.1127 0.2876 0.1931 0.047 Uiso 1 1 calc R . . C38 C -0.22120(10) 0.51012(14) 0.21802(9) 0.0255(6) Uani 1 1 d G . . C39 C -0.29402(14) 0.48140(14) 0.16291(8) 0.0283(7) Uani 1 1 d G . . H39 H -0.2700 0.4503 0.1295 0.034 Uiso 1 1 calc R . . C40 C -0.40194(13) 0.49812(16) 0.15675(8) 0.0345(8) Uani 1 1 d G . . H40 H -0.4517 0.4785 0.1191 0.041 Uiso 1 1 calc R . . C41 C -0.43704(10) 0.54356(16) 0.20569(10) 0.0386(8) Uani 1 1 d G . . H41 H -0.5108 0.5550 0.2015 0.046 Uiso 1 1 calc R . . C42 C -0.36422(14) 0.57227(15) 0.26080(9) 0.0369(8) Uani 1 1 d G . . H42 H -0.3882 0.6033 0.2942 0.044 Uiso 1 1 calc R . . C43 C -0.25631(13) 0.55555(15) 0.26696(8) 0.0311(7) Uani 1 1 d G . . H43 H -0.2065 0.5752 0.3046 0.037 Uiso 1 1 calc R . . C44 C -0.04782(14) 0.39736(12) 0.29140(8) 0.0239(6) Uani 1 1 d G . . C45 C 0.05738(12) 0.36897(13) 0.31401(9) 0.0284(7) Uani 1 1 d G . . H45 H 0.1117 0.3977 0.2971 0.034 Uiso 1 1 calc R . . C46 C 0.08309(11) 0.29860(14) 0.36142(10) 0.0317(7) Uani 1 1 d G . . H46 H 0.1550 0.2792 0.3769 0.038 Uiso 1 1 calc R . . C47 C 0.00359(15) 0.25662(13) 0.38623(9) 0.0368(8) Uani 1 1 d G . . H47 H 0.0212 0.2085 0.4186 0.044 Uiso 1 1 calc R . . C48 C -0.10161(13) 0.28502(14) 0.36362(10) 0.0361(8) Uani 1 1 d G . . H48 H -0.1559 0.2563 0.3806 0.043 Uiso 1 1 calc R . . C49 C -0.12732(11) 0.35538(14) 0.31620(10) 0.0286(7) Uani 1 1 d G . . H49 H -0.1992 0.3748 0.3008 0.034 Uiso 1 1 calc R . . O1 O 0.33479(17) 0.43433(16) 0.34769(10) 0.0327(5) Uani 1 1 d . . . O2 O 0.33631(18) 0.34432(16) 0.43123(11) 0.0358(5) Uani 1 1 d . . . F1 F 0.24134(17) 0.40968(16) -0.02274(9) 0.0495(5) Uani 1 1 d . . . F2 F 0.39335(16) 0.38553(14) 0.03977(9) 0.0422(5) Uani 1 1 d . . . F3 F 0.35659(18) 0.52578(15) -0.00283(10) 0.0488(5) Uani 1 1 d . . . P1 P -0.07644(6) 0.49015(5) 0.22808(4) 0.02239(17) Uani 1 1 d . . . Co1 Co 0.01098(3) 0.62770(3) 0.238769(18) 0.02099(12) 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 0.0299(17) 0.0272(16) 0.0372(19) 0.0109(14) 0.0048(15) 0.0100(13) C2 0.0331(17) 0.0165(14) 0.0386(19) 0.0038(12) 0.0076(15) 0.0028(12) C3 0.0313(17) 0.0200(14) 0.0376(19) 0.0093(13) 0.0071(15) 0.0020(13) C4 0.0401(19) 0.0327(17) 0.0278(17) 0.0148(14) 0.0056(15) 0.0075(14) C5 0.0325(18) 0.0331(17) 0.0289(17) 0.0113(14) -0.0060(14) 0.0040(14) C6 0.0207(14) 0.0203(14) 0.0244(15) 0.0022(11) 0.0047(12) -0.0012(11) C7 0.0218(14) 0.0209(14) 0.0256(16) 0.0012(11) 0.0058(12) -0.0021(11) C8 0.0211(14) 0.0185(13) 0.0228(15) 0.0006(11) 0.0036(12) -0.0018(11) C9 0.0235(14) 0.0140(13) 0.0210(14) -0.0006(10) 0.0019(12) -0.0007(11) C10 0.0200(14) 0.0227(14) 0.0228(15) 0.0008(12) 0.0057(12) -0.0034(11) C11 0.0208(14) 0.0272(15) 0.0233(15) 0.0012(12) 0.0035(12) 0.0017(12) C12 0.0202(15) 0.0341(17) 0.0266(16) -0.0017(13) 0.0015(13) 0.0052(13) C13 0.0257(16) 0.0437(19) 0.0277(17) 0.0073(14) 0.0088(14) 0.0041(14) C14 0.0289(18) 0.063(2) 0.039(2) 0.0042(18) 0.0066(16) -0.0017(17) C15 0.0263(16) 0.0347(17) 0.0271(17) 0.0048(13) 0.0009(14) -0.0002(13) C16 0.0315(18) 0.0452(19) 0.0255(17) -0.0059(15) -0.0029(14) -0.0013(15) C17 0.0293(17) 0.0343(17) 0.0308(18) -0.0124(14) -0.0004(14) -0.0014(14) C18 0.0237(15) 0.0233(14) 0.0292(16) -0.0018(12) 0.0052(13) -0.0023(12) C19 0.0178(13) 0.0243(14) 0.0188(14) -0.0031(11) -0.0019(11) -0.0016(11) C20 0.0262(16) 0.0251(15) 0.0312(17) 0.0008(13) 0.0050(13) -0.0015(12) C21 0.0311(17) 0.0333(17) 0.0370(19) -0.0017(14) 0.0081(15) 0.0120(14) C22 0.0280(16) 0.0409(19) 0.0323(18) 0.0005(14) 0.0124(14) 0.0037(14) C23 0.0259(16) 0.0344(17) 0.0268(17) 0.0003(13) 0.0061(13) -0.0061(13) C24 0.0212(15) 0.0226(14) 0.0260(16) -0.0020(12) 0.0020(12) 0.0031(12) C25 0.0203(14) 0.0267(15) 0.0203(15) 0.0007(12) 0.0011(12) 0.0000(12) C26 0.0368(18) 0.0262(16) 0.0272(17) -0.0028(12) 0.0088(14) -0.0052(13) C27 0.0380(18) 0.0245(15) 0.0251(16) 0.0003(12) 0.0098(14) -0.0061(13) C28 0.0254(16) 0.0328(16) 0.0203(15) -0.0027(12) 0.0008(13) -0.0010(13) C29 0.0448(19) 0.0247(15) 0.0284(17) -0.0034(13) 0.0111(15) 0.0001(14) C30 0.0365(18) 0.0254(15) 0.0292(17) 0.0052(13) 0.0090(14) -0.0010(13) C31 0.0383(18) 0.0297(17) 0.0250(17) 0.0010(13) 0.0020(14) -0.0022(14) C32 0.0234(15) 0.0305(16) 0.0297(17) -0.0050(13) 0.0000(13) -0.0009(13) C33 0.044(2) 0.0385(19) 0.0272(18) -0.0052(14) 0.0065(15) -0.0065(16) C34 0.060(3) 0.059(2) 0.0306(19) -0.0108(18) 0.0112(18) -0.012(2) C35 0.048(2) 0.050(2) 0.034(2) -0.0204(17) 0.0026(17) -0.0011(18) C36 0.049(2) 0.0344(19) 0.043(2) -0.0115(16) 0.0031(18) -0.0003(16) C37 0.049(2) 0.0306(18) 0.037(2) -0.0072(15) 0.0058(17) -0.0023(16) C38 0.0190(14) 0.0242(15) 0.0305(17) 0.0002(12) 0.0001(13) -0.0014(12) C39 0.0234(15) 0.0303(16) 0.0287(17) -0.0007(13) 0.0013(13) -0.0025(13) C40 0.0243(16) 0.0342(17) 0.0375(19) 0.0027(14) -0.0079(14) -0.0043(13) C41 0.0280(17) 0.0351(18) 0.053(2) 0.0041(16) 0.0099(17) 0.0022(14) C42 0.0301(18) 0.0359(18) 0.046(2) -0.0048(16) 0.0116(16) 0.0002(14) C43 0.0257(16) 0.0328(17) 0.0330(18) -0.0045(14) 0.0029(14) -0.0016(13) C44 0.0282(16) 0.0181(13) 0.0239(15) -0.0035(11) 0.0032(13) -0.0022(12) C45 0.0269(16) 0.0232(15) 0.0353(18) 0.0008(13) 0.0076(14) -0.0009(12) C46 0.0278(17) 0.0246(15) 0.0395(19) 0.0055(14) 0.0017(14) 0.0008(13) C47 0.046(2) 0.0247(16) 0.037(2) 0.0066(14) 0.0050(16) -0.0033(15) C48 0.0350(18) 0.0347(18) 0.040(2) 0.0054(15) 0.0121(16) -0.0086(14) C49 0.0233(15) 0.0283(16) 0.0331(17) -0.0012(13) 0.0044(13) -0.0041(12) O1 0.0344(12) 0.0364(12) 0.0261(12) -0.0001(9) 0.0049(10) 0.0142(10) O2 0.0402(13) 0.0309(12) 0.0338(13) 0.0042(10) 0.0038(10) 0.0113(10) F1 0.0521(13) 0.0628(14) 0.0308(11) -0.0182(10) 0.0041(10) -0.0023(11) F2 0.0452(12) 0.0447(12) 0.0398(11) -0.0037(9) 0.0165(10) 0.0081(9) F3 0.0768(15) 0.0398(11) 0.0390(12) 0.0001(9) 0.0323(11) -0.0044(10) P1 0.0212(4) 0.0216(4) 0.0225(4) -0.0014(3) 0.0014(3) -0.0013(3) Co1 0.0211(2) 0.0185(2) 0.0218(2) 0.00269(15) 0.00187(16) -0.00013(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.417(4) . ? C1 C5 1.419(5) . ? C1 Co1 2.106(3) . ? C1 H1 0.9500 . ? C2 C3 1.401(4) . ? C2 Co1 2.099(3) . ? C2 H2 0.9500 . ? C3 C4 1.416(5) . ? C3 Co1 2.099(3) . ? C3 H3 0.9500 . ? C4 C5 1.408(5) . ? C4 Co1 2.129(3) . ? C4 H4 0.9500 . ? C5 Co1 2.110(3) . ? C5 H5 0.9500 . ? C6 C7 1.350(4) . ? C6 C25 1.515(3) . ? C6 Co1 1.963(3) . ? C7 C8 1.471(4) . ? C7 C13 1.506(4) . ? C8 C9 1.367(4) . ? C8 C10 1.491(4) . ? C9 C19 1.515(3) . ? C9 Co1 1.975(3) . ? C10 C18 1.401(4) . ? C10 C11 1.410(4) . ? C11 C15 1.398(4) . ? C11 C12 1.496(4) . ? C12 O2 1.211(4) . ? C12 O1 1.340(4) . ? C13 O1 1.471(4) . ? C13 C14 1.483(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 C17 1.391(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 C31 1.512(3) . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 F3 1.334(4) . ? C31 F2 1.335(4) . ? C31 F1 1.345(4) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C32 P1 1.8482(16) . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C38 P1 1.8544(15) . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C44 P1 1.8413(15) . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? P1 Co1 2.1871(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 106.5(3) . . ? C2 C1 Co1 70.05(17) . . ? C5 C1 Co1 70.49(17) . . ? C2 C1 H1 126.7 . . ? C5 C1 H1 126.7 . . ? Co1 C1 H1 124.4 . . ? C3 C2 C1 108.8(3) . . ? C3 C2 Co1 70.50(17) . . ? C1 C2 Co1 70.56(17) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Co1 C2 H2 124.9 . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Co1 70.51(17) . . ? C4 C3 Co1 71.58(17) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Co1 C3 H3 123.7 . . ? C5 C4 C3 107.1(3) . . ? C5 C4 Co1 69.87(17) . . ? C3 C4 Co1 69.29(17) . . ? C5 C4 H4 126.4 . . ? C3 C4 H4 126.4 . . ? Co1 C4 H4 126.0 . . ? C4 C5 C1 109.2(3) . . ? C4 C5 Co1 71.34(18) . . ? C1 C5 Co1 70.18(17) . . ? C4 C5 H5 125.4 . . ? C1 C5 H5 125.4 . . ? Co1 C5 H5 124.7 . . ? C7 C6 C25 121.3(2) . . ? C7 C6 Co1 113.1(2) . . ? C25 C6 Co1 125.55(19) . . ? C6 C7 C8 115.8(3) . . ? C6 C7 C13 124.1(3) . . ? C8 C7 C13 120.1(3) . . ? C9 C8 C7 114.0(3) . . ? C9 C8 C10 125.5(3) . . ? C7 C8 C10 120.5(2) . . ? C8 C9 C19 123.2(2) . . ? C8 C9 Co1 113.1(2) . . ? C19 C9 Co1 123.59(18) . . ? C18 C10 C11 116.7(3) . . ? C18 C10 C8 119.1(3) . . ? C11 C10 C8 124.0(3) . . ? C15 C11 C10 121.1(3) . . ? C15 C11 C12 113.7(3) . . ? C10 C11 C12 125.2(3) . . ? O2 C12 O1 117.5(3) . . ? O2 C12 C11 122.0(3) . . ? O1 C12 C11 120.5(3) . . ? O1 C13 C14 113.5(3) . . ? O1 C13 C7 109.3(2) . . ? C14 C13 C7 117.2(3) . . ? O1 C13 H13 105.2 . . ? C14 C13 H13 105.2 . . ? C7 C13 H13 105.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 120.8(3) . . ? C16 C15 H15 119.6 . . ? C11 C15 H15 119.6 . . ? C15 C16 C17 118.5(3) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C10 121.7(3) . . ? C17 C18 H18 119.1 . . ? C10 C18 H18 119.1 . . ? C20 C19 C24 120.0 . . ? C20 C19 C9 122.07(14) . . ? C24 C19 C9 117.87(14) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 C6 120.70(15) . . ? C30 C25 C6 119.21(15) . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 C31 119.98(16) . . ? C29 C28 C31 120.02(16) . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? F3 C31 F2 106.6(3) . . ? F3 C31 F1 107.2(3) . . ? F2 C31 F1 105.6(3) . . ? F3 C31 C28 112.5(2) . . ? F2 C31 C28 112.3(2) . . ? F1 C31 C28 112.1(3) . . ? C33 C32 C37 120.0 . . ? C33 C32 P1 120.08(11) . . ? C37 C32 P1 119.86(11) . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C43 120.0 . . ? C39 C38 P1 121.50(10) . . ? C43 C38 P1 118.50(10) . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 H43 120.0 . . ? C38 C43 H43 120.0 . . ? C45 C44 C49 120.0 . . ? C45 C44 P1 117.74(10) . . ? C49 C44 P1 122.25(10) . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 H49 120.0 . . ? C44 C49 H49 120.0 . . ? C12 O1 C13 123.6(2) . . ? C44 P1 C32 100.71(10) . . ? C44 P1 C38 102.25(9) . . ? C32 P1 C38 102.40(10) . . ? C44 P1 Co1 120.72(7) . . ? C32 P1 Co1 116.72(7) . . ? C38 P1 Co1 111.56(7) . . ? C6 Co1 C9 83.23(12) . . ? C6 Co1 C3 90.89(12) . . ? C9 Co1 C3 113.11(12) . . ? C6 Co1 C2 119.17(12) . . ? C9 Co1 C2 88.98(12) . . ? C3 Co1 C2 38.98(12) . . ? C6 Co1 C1 156.66(12) . . ? C9 Co1 C1 102.09(12) . . ? C3 Co1 C1 66.02(12) . . ? C2 Co1 C1 39.39(12) . . ? C6 Co1 C5 134.82(12) . . ? C9 Co1 C5 140.59(12) . . ? C3 Co1 C5 65.33(13) . . ? C2 Co1 C5 65.36(13) . . ? C1 Co1 C5 39.34(13) . . ? C6 Co1 C4 98.76(12) . . ? C9 Co1 C4 151.88(12) . . ? C3 Co1 C4 39.13(13) . . ? C2 Co1 C4 65.41(13) . . ? C1 Co1 C4 65.92(13) . . ? C5 Co1 C4 38.80(12) . . ? C6 Co1 P1 95.77(8) . . ? C9 Co1 P1 94.28(8) . . ? C3 Co1 P1 152.41(9) . . ? C2 Co1 P1 145.03(9) . . ? C1 Co1 P1 106.34(9) . . ? C5 Co1 P1 91.66(9) . . ? C4 Co1 P1 113.28(10) . . ? 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 C5 C1 C2 C3 -1.0(3) . . . . ? Co1 C1 C2 C3 60.4(2) . . . . ? C5 C1 C2 Co1 -61.4(2) . . . . ? C1 C2 C3 C4 1.5(3) . . . . ? Co1 C2 C3 C4 61.9(2) . . . . ? C1 C2 C3 Co1 -60.4(2) . . . . ? C2 C3 C4 C5 -1.3(3) . . . . ? Co1 C3 C4 C5 59.9(2) . . . . ? C2 C3 C4 Co1 -61.2(2) . . . . ? C3 C4 C5 C1 0.7(3) . . . . ? Co1 C4 C5 C1 60.2(2) . . . . ? C3 C4 C5 Co1 -59.5(2) . . . . ? C2 C1 C5 C4 0.2(3) . . . . ? Co1 C1 C5 C4 -61.0(2) . . . . ? C2 C1 C5 Co1 61.1(2) . . . . ? C25 C6 C7 C8 -176.5(2) . . . . ? Co1 C6 C7 C8 6.5(3) . . . . ? C25 C6 C7 C13 1.9(4) . . . . ? Co1 C6 C7 C13 -175.1(2) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C13 C7 C8 C9 -178.7(3) . . . . ? C6 C7 C8 C10 -179.2(3) . . . . ? C13 C7 C8 C10 2.3(4) . . . . ? C7 C8 C9 C19 169.6(2) . . . . ? C10 C8 C9 C19 -11.5(4) . . . . ? C7 C8 C9 Co1 -6.1(3) . . . . ? C10 C8 C9 Co1 172.8(2) . . . . ? C9 C8 C10 C18 -41.8(4) . . . . ? C7 C8 C10 C18 137.1(3) . . . . ? C9 C8 C10 C11 142.0(3) . . . . ? C7 C8 C10 C11 -39.2(4) . . . . ? C18 C10 C11 C15 0.0(4) . . . . ? C8 C10 C11 C15 176.4(3) . . . . ? C18 C10 C11 C12 -179.7(3) . . . . ? C8 C10 C11 C12 -3.4(4) . . . . ? C15 C11 C12 O2 42.2(4) . . . . ? C10 C11 C12 O2 -138.0(3) . . . . ? C15 C11 C12 O1 -136.2(3) . . . . ? C10 C11 C12 O1 43.6(4) . . . . ? C6 C7 C13 O1 -113.0(3) . . . . ? C8 C7 C13 O1 65.3(3) . . . . ? C6 C7 C13 C14 116.1(3) . . . . ? C8 C7 C13 C14 -65.6(4) . . . . ? C10 C11 C15 C16 -1.7(5) . . . . ? C12 C11 C15 C16 178.1(3) . . . . ? C11 C15 C16 C17 0.9(5) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? C16 C17 C18 C10 -3.3(5) . . . . ? C11 C10 C18 C17 2.4(4) . . . . ? C8 C10 C18 C17 -174.1(3) . . . . ? C8 C9 C19 C20 119.9(2) . . . . ? Co1 C9 C19 C20 -64.9(2) . . . . ? C8 C9 C19 C24 -62.9(3) . . . . ? Co1 C9 C19 C24 112.30(17) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C9 C19 C20 C21 177.1(2) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? C9 C19 C24 C23 -177.21(19) . . . . ? C7 C6 C25 C26 -105.9(3) . . . . ? Co1 C6 C25 C26 70.7(2) . . . . ? C7 C6 C25 C30 70.7(3) . . . . ? Co1 C6 C25 C30 -112.67(19) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C6 C25 C26 C27 176.6(2) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C31 179.3(2) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C31 C28 C29 C30 -179.3(2) . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? C6 C25 C30 C29 -176.6(2) . . . . ? C27 C28 C31 F3 13.4(3) . . . . ? C29 C28 C31 F3 -167.3(2) . . . . ? C27 C28 C31 F2 133.7(2) . . . . ? C29 C28 C31 F2 -47.0(3) . . . . ? C27 C28 C31 F1 -107.6(2) . . . . ? C29 C28 C31 F1 71.7(3) . . . . ? C37 C32 C33 C34 0.0 . . . . ? P1 C32 C33 C34 -177.11(17) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C32 0.0 . . . . ? C33 C32 C37 C36 0.0 . . . . ? P1 C32 C37 C36 177.12(17) . . . . ? C43 C38 C39 C40 0.0 . . . . ? P1 C38 C39 C40 -179.53(16) . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C38 0.0 . . . . ? C39 C38 C43 C42 0.0 . . . . ? P1 C38 C43 C42 179.54(15) . . . . ? C49 C44 C45 C46 0.0 . . . . ? P1 C44 C45 C46 -179.49(15) . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C44 0.0 . . . . ? C45 C44 C49 C48 0.0 . . . . ? P1 C44 C49 C48 179.46(16) . . . . ? O2 C12 O1 C13 -177.3(3) . . . . ? C11 C12 O1 C13 1.2(4) . . . . ? C14 C13 O1 C12 63.0(4) . . . . ? C7 C13 O1 C12 -69.8(3) . . . . ? C45 C44 P1 C32 78.47(13) . . . . ? C49 C44 P1 C32 -101.00(13) . . . . ? C45 C44 P1 C38 -176.17(11) . . . . ? C49 C44 P1 C38 4.35(14) . . . . ? C45 C44 P1 Co1 -51.67(13) . . . . ? C49 C44 P1 Co1 128.86(10) . . . . ? C33 C32 P1 C44 -154.75(13) . . . . ? C37 C32 P1 C44 28.13(14) . . . . ? C33 C32 P1 C38 100.02(14) . . . . ? C37 C32 P1 C38 -77.09(14) . . . . ? C33 C32 P1 Co1 -22.11(15) . . . . ? C37 C32 P1 Co1 160.77(10) . . . . ? C39 C38 P1 C44 -111.47(13) . . . . ? C43 C38 P1 C44 69.00(13) . . . . ? C39 C38 P1 C32 -7.44(14) . . . . ? C43 C38 P1 C32 173.02(11) . . . . ? C39 C38 P1 Co1 118.15(11) . . . . ? C43 C38 P1 Co1 -61.39(12) . . . . ? C7 C6 Co1 C9 -7.7(2) . . . . ? C25 C6 Co1 C9 175.4(2) . . . . ? C7 C6 Co1 C3 105.5(2) . . . . ? C25 C6 Co1 C3 -71.4(2) . . . . ? C7 C6 Co1 C2 77.3(2) . . . . ? C25 C6 Co1 C2 -99.6(2) . . . . ? C7 C6 Co1 C1 97.2(4) . . . . ? C25 C6 Co1 C1 -79.7(4) . . . . ? C7 C6 Co1 C5 160.5(2) . . . . ? C25 C6 Co1 C5 -16.4(3) . . . . ? C7 C6 Co1 C4 144.0(2) . . . . ? C25 C6 Co1 C4 -32.9(2) . . . . ? C7 C6 Co1 P1 -101.3(2) . . . . ? C25 C6 Co1 P1 81.8(2) . . . . ? C8 C9 Co1 C6 7.6(2) . . . . ? C19 C9 Co1 C6 -168.1(2) . . . . ? C8 C9 Co1 C3 -80.5(2) . . . . ? C19 C9 Co1 C3 103.9(2) . . . . ? C8 C9 Co1 C2 -112.0(2) . . . . ? C19 C9 Co1 C2 72.4(2) . . . . ? C8 C9 Co1 C1 -149.4(2) . . . . ? C19 C9 Co1 C1 35.0(2) . . . . ? C8 C9 Co1 C5 -159.2(2) . . . . ? C19 C9 Co1 C5 25.1(3) . . . . ? C8 C9 Co1 C4 -88.3(3) . . . . ? C19 C9 Co1 C4 96.0(3) . . . . ? C8 C9 Co1 P1 102.90(19) . . . . ? C19 C9 Co1 P1 -72.75(19) . . . . ? C2 C3 Co1 C6 -139.1(2) . . . . ? C4 C3 Co1 C6 102.8(2) . . . . ? C2 C3 Co1 C9 -56.1(2) . . . . ? C4 C3 Co1 C9 -174.14(18) . . . . ? C4 C3 Co1 C2 -118.1(3) . . . . ? C2 C3 Co1 C1 37.34(19) . . . . ? C4 C3 Co1 C1 -80.7(2) . . . . ? C2 C3 Co1 C5 80.7(2) . . . . ? C4 C3 Co1 C5 -37.39(19) . . . . ? C2 C3 Co1 C4 118.1(3) . . . . ? C2 C3 Co1 P1 116.6(2) . . . . ? C4 C3 Co1 P1 -1.5(3) . . . . ? C3 C2 Co1 C6 48.6(2) . . . . ? C1 C2 Co1 C6 167.73(18) . . . . ? C3 C2 Co1 C9 130.3(2) . . . . ? C1 C2 Co1 C9 -110.6(2) . . . . ? C1 C2 Co1 C3 119.1(3) . . . . ? C3 C2 Co1 C1 -119.1(3) . . . . ? C3 C2 Co1 C5 -80.6(2) . . . . ? C1 C2 Co1 C5 38.53(19) . . . . ? C3 C2 Co1 C4 -37.76(19) . . . . ? C1 C2 Co1 C4 81.4(2) . . . . ? C3 C2 Co1 P1 -133.74(17) . . . . ? C1 C2 Co1 P1 -14.6(3) . . . . ? C2 C1 Co1 C6 -27.9(4) . . . . ? C5 C1 Co1 C6 88.8(4) . . . . ? C2 C1 Co1 C9 73.2(2) . . . . ? C5 C1 Co1 C9 -170.12(19) . . . . ? C2 C1 Co1 C3 -36.97(19) . . . . ? C5 C1 Co1 C3 79.8(2) . . . . ? C5 C1 Co1 C2 116.7(3) . . . . ? C2 C1 Co1 C5 -116.7(3) . . . . ? C2 C1 Co1 C4 -80.0(2) . . . . ? C5 C1 Co1 C4 36.73(19) . . . . ? C2 C1 Co1 P1 171.35(17) . . . . ? C5 C1 Co1 P1 -71.93(19) . . . . ? C4 C5 Co1 C6 -26.7(3) . . . . ? C1 C5 Co1 C6 -146.05(19) . . . . ? C4 C5 Co1 C9 134.7(2) . . . . ? C1 C5 Co1 C9 15.3(3) . . . . ? C4 C5 Co1 C3 37.7(2) . . . . ? C1 C5 Co1 C3 -81.7(2) . . . . ? C4 C5 Co1 C2 80.8(2) . . . . ? C1 C5 Co1 C2 -38.58(19) . . . . ? C4 C5 Co1 C1 119.4(3) . . . . ? C1 C5 Co1 C4 -119.4(3) . . . . ? C4 C5 Co1 P1 -126.51(19) . . . . ? C1 C5 Co1 P1 114.12(18) . . . . ? C5 C4 Co1 C6 161.2(2) . . . . ? C3 C4 Co1 C6 -80.54(19) . . . . ? C5 C4 Co1 C9 -106.8(3) . . . . ? C3 C4 Co1 C9 11.5(4) . . . . ? C5 C4 Co1 C3 -118.3(3) . . . . ? C5 C4 Co1 C2 -80.6(2) . . . . ? C3 C4 Co1 C2 37.62(18) . . . . ? C5 C4 Co1 C1 -37.2(2) . . . . ? C3 C4 Co1 C1 81.0(2) . . . . ? C3 C4 Co1 C5 118.3(3) . . . . ? C5 C4 Co1 P1 61.0(2) . . . . ? C3 C4 Co1 P1 179.27(15) . . . . ? C44 P1 Co1 C6 64.43(12) . . . . ? C32 P1 Co1 C6 -58.33(12) . . . . ? C38 P1 Co1 C6 -175.56(11) . . . . ? C44 P1 Co1 C9 -19.19(11) . . . . ? C32 P1 Co1 C9 -141.95(12) . . . . ? C38 P1 Co1 C9 100.83(11) . . . . ? C44 P1 Co1 C3 167.6(2) . . . . ? C32 P1 Co1 C3 44.8(2) . . . . ? C38 P1 Co1 C3 -72.4(2) . . . . ? C44 P1 Co1 C2 -113.53(18) . . . . ? C32 P1 Co1 C2 123.71(18) . . . . ? C38 P1 Co1 C2 6.48(18) . . . . ? C44 P1 Co1 C1 -123.12(12) . . . . ? C32 P1 Co1 C1 114.12(13) . . . . ? C38 P1 Co1 C1 -3.11(12) . . . . ? C44 P1 Co1 C5 -160.20(12) . . . . ? C32 P1 Co1 C5 77.04(13) . . . . ? C38 P1 Co1 C5 -40.19(12) . . . . ? C44 P1 Co1 C4 166.55(12) . . . . ? C32 P1 Co1 C4 43.79(13) . . . . ? C38 P1 Co1 C4 -73.43(12) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.736 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.077